data_mm109_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Dy2 N8 O14' _chemical_formula_weight 1187.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4807(5) _cell_length_b 10.5015(5) _cell_length_c 11.4678(5) _cell_angle_alpha 64.937(2) _cell_angle_beta 66.519(2) _cell_angle_gamma 79.936(2) _cell_volume 1048.63(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9309 _cell_measurement_theta_min 2.341 _cell_measurement_theta_max 36.318 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 3.614 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5318 _exptl_absorpt_correction_T_max 0.6709 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method ' \f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56987 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 36.43 _reflns_number_total 10134 _reflns_number_gt 9729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.1937P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10134 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0155 _refine_ls_R_factor_gt 0.0145 _refine_ls_wR_factor_ref 0.0358 _refine_ls_wR_factor_gt 0.0354 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.145947(4) 0.087075(4) -0.005196(4) 0.00785(1) Uani 1 1 d . . . O1 O 0.07517(9) -0.30517(8) 0.43055(8) 0.01599(13) Uani 1 1 d . . . O2 O 0.18126(8) -0.08860(8) 0.16995(8) 0.01373(13) Uani 1 1 d . . . O3 O -0.09153(7) 0.03782(7) 0.10408(7) 0.00976(11) Uani 1 1 d . . . O4 O -0.21883(9) -0.07842(8) 0.37896(8) 0.01409(13) Uani 1 1 d . . . O5 O 0.27249(9) 0.25123(9) 0.00672(8) 0.01580(13) Uani 1 1 d . . . O6 O 0.07485(9) 0.18648(9) 0.17558(9) 0.01669(14) Uani 1 1 d . . . O7 O 0.21749(11) 0.30838(10) 0.18311(10) 0.02343(17) Uani 1 1 d . . . N1 N 0.38414(9) -0.00947(9) -0.09671(9) 0.01195(13) Uani 1 1 d . . . N2 N 0.28585(9) 0.24159(9) -0.25218(9) 0.01159(13) Uani 1 1 d . . . N3 N 0.01218(9) 0.29968(9) -0.11161(9) 0.01160(13) Uani 1 1 d . . . N4 N 0.18806(10) 0.25018(9) 0.12463(9) 0.01302(14) Uani 1 1 d . . . C1 C 0.09827(15) -0.20467(15) 0.47412(13) 0.0234(2) Uani 1 1 d . . . C2 C 0.18724(11) -0.32528(10) 0.32441(10) 0.01263(15) Uani 1 1 d . . . C3 C 0.23938(12) -0.46059(11) 0.34542(11) 0.01552(17) Uani 1 1 d . . . C4 C 0.35208(12) -0.48931(11) 0.24157(12) 0.01590(17) Uani 1 1 d . . . C5 C 0.41309(11) -0.38019(11) 0.11705(11) 0.01425(16) Uani 1 1 d . . . C6 C 0.35845(10) -0.24241(10) 0.09112(10) 0.01183(15) Uani 1 1 d . . . C7 C 0.24046(10) -0.21261(10) 0.19317(10) 0.01138(15) Uani 1 1 d . . . C8 C 0.42793(10) -0.13535(11) -0.04344(10) 0.01269(15) Uani 1 1 d . . . C9 C 0.47722(11) 0.07457(11) -0.23768(11) 0.01501(17) Uani 1 1 d . . . C10 C 0.43566(11) 0.22859(11) -0.27754(10) 0.01371(16) Uani 1 1 d . . . C11 C 0.23571(11) 0.38837(10) -0.28997(10) 0.01333(16) Uani 1 1 d . . . C12 C 0.08114(11) 0.38819(11) -0.25868(10) 0.01483(16) Uani 1 1 d . . . C13 C -0.10886(11) 0.33936(10) -0.04888(10) 0.01197(15) Uani 1 1 d . . . C14 C -0.19146(10) 0.26445(10) 0.09721(10) 0.01062(14) Uani 1 1 d . . . C15 C -0.28677(11) 0.34444(10) 0.16639(11) 0.01360(16) Uani 1 1 d . . . C16 C -0.35840(12) 0.28458(11) 0.30716(11) 0.01558(17) Uani 1 1 d . . . C17 C -0.33650(11) 0.14264(11) 0.38118(11) 0.01431(16) Uani 1 1 d . . . C18 C -0.24584(10) 0.06117(10) 0.31341(10) 0.01089(14) Uani 1 1 d . . . C19 C -0.17436(10) 0.11928(9) 0.16867(9) 0.00938(13) Uani 1 1 d . . . C20 C -0.25494(13) -0.13110(12) 0.52508(11) 0.01762(18) Uani 1 1 d . . . H1 H -0.422(2) 0.3410(19) 0.3547(19) 0.021(4) Uiso 1 1 d . . . H2 H -0.383(2) 0.1024(19) 0.477(2) 0.024(4) Uiso 1 1 d . . . H3 H -0.2942(18) 0.4374(18) 0.1161(18) 0.018(4) Uiso 1 1 d . . . H4 H -0.221(2) -0.076(2) 0.547(2) 0.024(4) Uiso 1 1 d . . . H5 H -0.2162(19) -0.2229(19) 0.5522(19) 0.022(4) Uiso 1 1 d . . . H6 H -0.356(2) -0.140(2) 0.574(2) 0.028(5) Uiso 1 1 d . . . H7 H -0.1481(19) 0.4251(18) -0.1002(18) 0.020(4) Uiso 1 1 d . . . H8 H 0.042(2) 0.485(2) -0.283(2) 0.023(4) Uiso 1 1 d . . . H9 H 0.0645(18) 0.3455(17) -0.3146(18) 0.016(4) Uiso 1 1 d . . . H10 H 0.2844(19) 0.4433(18) -0.3831(19) 0.019(4) Uiso 1 1 d . . . H11 H 0.2568(17) 0.4265(17) -0.2392(17) 0.013(4) Uiso 1 1 d . . . H12 H 0.2679(18) 0.2070(17) -0.3027(17) 0.015(4) Uiso 1 1 d . . . H13 H 0.4562(17) 0.2661(16) -0.2238(17) 0.012(3) Uiso 1 1 d . . . H14 H 0.490(2) 0.287(2) -0.379(2) 0.029(5) Uiso 1 1 d . . . H15 H 0.5778(19) 0.0617(19) -0.2430(19) 0.021(4) Uiso 1 1 d . . . H16 H 0.4629(18) 0.0404(17) -0.3007(17) 0.014(4) Uiso 1 1 d . . . H17 H 0.516(2) -0.176(2) -0.087(2) 0.028(5) Uiso 1 1 d . . . H18 H 0.4932(18) -0.3946(18) 0.0455(18) 0.017(4) Uiso 1 1 d . . . H19 H 0.3864(18) -0.5815(18) 0.2555(18) 0.016(4) Uiso 1 1 d . . . H20 H 0.025(2) -0.215(2) 0.558(2) 0.024(4) Uiso 1 1 d . . . H21 H 0.100(2) -0.112(2) 0.408(2) 0.030(5) Uiso 1 1 d . . . H22 H 0.1913(19) -0.5303(19) 0.4292(19) 0.020(4) Uiso 1 1 d . . . H23 H 0.183(3) -0.221(2) 0.481(2) 0.044(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.00833(2) 0.00797(2) 0.00697(2) -0.00289(1) -0.00220(1) -0.00090(1) O1 0.0168(3) 0.0174(3) 0.0119(3) -0.0053(3) -0.0029(3) -0.0025(3) O2 0.0148(3) 0.0127(3) 0.0106(3) -0.0033(2) -0.0044(2) 0.0030(2) O3 0.0097(3) 0.0100(3) 0.0098(3) -0.0056(2) -0.0018(2) -0.0004(2) O4 0.0205(4) 0.0107(3) 0.0092(3) -0.0033(2) -0.0040(3) -0.0006(2) O5 0.0156(3) 0.0199(3) 0.0126(3) -0.0080(3) -0.0019(3) -0.0053(3) O6 0.0135(3) 0.0216(3) 0.0164(3) -0.0107(3) -0.0017(3) -0.0043(3) O7 0.0315(5) 0.0267(4) 0.0220(4) -0.0145(3) -0.0113(4) -0.0066(3) N1 0.0106(3) 0.0134(3) 0.0101(3) -0.0042(3) -0.0018(3) -0.0016(3) N2 0.0119(3) 0.0125(3) 0.0102(3) -0.0038(3) -0.0034(3) -0.0029(3) N3 0.0132(3) 0.0109(3) 0.0090(3) -0.0023(2) -0.0036(3) -0.0014(3) N4 0.0166(4) 0.0123(3) 0.0130(3) -0.0057(3) -0.0071(3) -0.0005(3) C1 0.0264(6) 0.0286(6) 0.0175(5) -0.0136(4) -0.0032(4) -0.0054(5) C2 0.0133(4) 0.0138(4) 0.0107(4) -0.0037(3) -0.0050(3) -0.0011(3) C3 0.0191(5) 0.0122(4) 0.0148(4) -0.0026(3) -0.0081(4) -0.0011(3) C4 0.0176(4) 0.0126(4) 0.0194(4) -0.0060(3) -0.0096(4) 0.0015(3) C5 0.0136(4) 0.0138(4) 0.0175(4) -0.0071(3) -0.0077(3) 0.0022(3) C6 0.0108(4) 0.0128(4) 0.0125(4) -0.0051(3) -0.0050(3) 0.0006(3) C7 0.0118(4) 0.0120(3) 0.0106(4) -0.0038(3) -0.0052(3) 0.0002(3) C8 0.0101(4) 0.0157(4) 0.0131(4) -0.0067(3) -0.0043(3) 0.0007(3) C9 0.0119(4) 0.0171(4) 0.0116(4) -0.0046(3) -0.0004(3) -0.0019(3) C10 0.0114(4) 0.0153(4) 0.0118(4) -0.0042(3) -0.0016(3) -0.0034(3) C11 0.0150(4) 0.0117(4) 0.0108(4) -0.0015(3) -0.0041(3) -0.0035(3) C12 0.0152(4) 0.0154(4) 0.0096(4) -0.0006(3) -0.0045(3) -0.0011(3) C13 0.0143(4) 0.0102(3) 0.0115(4) -0.0036(3) -0.0057(3) 0.0004(3) C14 0.0111(4) 0.0102(3) 0.0111(3) -0.0048(3) -0.0042(3) 0.0007(3) C15 0.0143(4) 0.0123(4) 0.0149(4) -0.0071(3) -0.0056(3) 0.0033(3) C16 0.0154(4) 0.0166(4) 0.0147(4) -0.0094(3) -0.0034(3) 0.0037(3) C17 0.0143(4) 0.0159(4) 0.0121(4) -0.0079(3) -0.0021(3) 0.0011(3) C18 0.0112(4) 0.0115(3) 0.0098(3) -0.0049(3) -0.0027(3) -0.0007(3) C19 0.0089(3) 0.0104(3) 0.0098(3) -0.0051(3) -0.0029(3) -0.0002(3) C20 0.0235(5) 0.0161(4) 0.0103(4) -0.0033(3) -0.0045(4) -0.0021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.1884(7) . ? Dy1 O3 2.3169(7) 2 ? Dy1 O3 2.3341(7) . ? Dy1 O5 2.4275(8) . ? Dy1 O6 2.5046(8) . ? Dy1 N1 2.5081(9) . ? Dy1 N3 2.5300(8) . ? Dy1 N2 2.5365(8) . ? Dy1 N4 2.8799(8) . ? Dy1 Dy1 3.76804(17) 2 ? O1 C2 1.3775(13) . ? O1 C1 1.4333(15) . ? O2 C7 1.3066(12) . ? O3 C19 1.3413(11) . ? O3 Dy1 2.3169(7) 2 ? O4 C18 1.3730(12) . ? O4 C20 1.4282(13) . ? O5 N4 1.2841(12) . ? O6 N4 1.2611(12) . ? O7 N4 1.2232(11) . ? N1 C8 1.2878(13) . ? N1 C9 1.4763(13) . ? N2 C10 1.4708(14) . ? N2 C11 1.4738(13) . ? N2 H12 0.890(17) . ? N3 C13 1.2815(13) . ? N3 C12 1.4718(13) . ? C1 H20 0.932(19) . ? C1 H21 0.94(2) . ? C1 H23 0.90(2) . ? C2 C3 1.3854(14) . ? C2 C7 1.4245(14) . ? C3 C4 1.4012(16) . ? C3 H22 0.927(19) . ? C4 C5 1.3796(16) . ? C4 H19 0.941(17) . ? C5 C6 1.4112(14) . ? C5 H18 0.955(17) . ? C6 C7 1.4208(14) . ? C6 C8 1.4479(14) . ? C8 H17 0.98(2) . ? C9 C10 1.5169(15) . ? C9 H15 1.019(18) . ? C9 H16 0.999(17) . ? C10 H13 0.960(16) . ? C10 H14 1.02(2) . ? C11 C12 1.5135(15) . ? C11 H10 0.938(18) . ? C11 H11 0.938(16) . ? C12 H8 0.988(18) . ? C12 H9 1.001(17) . ? C13 C14 1.4631(14) . ? C13 H7 0.970(17) . ? C14 C15 1.4045(13) . ? C14 C19 1.4111(13) . ? C15 C16 1.3800(15) . ? C15 H3 0.907(17) . ? C16 C17 1.3996(15) . ? C16 H1 0.968(18) . ? C17 C18 1.3891(13) . ? C17 H2 0.933(19) . ? C18 C19 1.4140(13) . ? C20 H4 0.890(19) . ? C20 H5 0.949(18) . ? C20 H6 0.98(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O3 99.35(3) . 2 ? O2 Dy1 O3 88.96(3) . . ? O3 Dy1 O3 71.78(3) 2 . ? O2 Dy1 O5 93.12(3) . . ? O3 Dy1 O5 157.14(3) 2 . ? O3 Dy1 O5 127.88(3) . . ? O2 Dy1 O6 76.84(3) . . ? O3 Dy1 O6 149.81(3) 2 . ? O3 Dy1 O6 78.18(2) . . ? O5 Dy1 O6 52.02(3) . . ? O2 Dy1 N1 72.87(3) . . ? O3 Dy1 N1 82.03(3) 2 . ? O3 Dy1 N1 145.25(3) . . ? O5 Dy1 N1 83.46(3) . . ? O6 Dy1 N1 123.72(3) . . ? O2 Dy1 N3 153.18(3) . . ? O3 Dy1 N3 91.27(3) 2 . ? O3 Dy1 N3 70.99(3) . . ? O5 Dy1 N3 85.94(3) . . ? O6 Dy1 N3 81.61(3) . . ? N1 Dy1 N3 133.36(3) . . ? O2 Dy1 N2 138.51(3) . . ? O3 Dy1 N2 84.87(3) 2 . ? O3 Dy1 N2 130.61(3) . . ? O5 Dy1 N2 73.18(3) . . ? O6 Dy1 N2 118.07(3) . . ? N1 Dy1 N2 66.86(3) . . ? N3 Dy1 N2 66.59(3) . . ? O2 Dy1 N4 82.44(3) . . ? O3 Dy1 N4 174.90(3) 2 . ? O3 Dy1 N4 103.57(2) . . ? O5 Dy1 N4 26.27(3) . . ? O6 Dy1 N4 25.91(3) . . ? N1 Dy1 N4 103.07(3) . . ? N3 Dy1 N4 85.14(3) . . ? N2 Dy1 N4 96.97(3) . . ? O2 Dy1 Dy1 95.09(2) . 2 ? O3 Dy1 Dy1 36.042(18) 2 2 ? O3 Dy1 Dy1 35.737(16) . 2 ? O5 Dy1 Dy1 161.26(2) . 2 ? O6 Dy1 Dy1 113.865(19) . 2 ? N1 Dy1 Dy1 115.07(2) . 2 ? N3 Dy1 Dy1 79.15(2) . 2 ? N2 Dy1 Dy1 110.38(2) . 2 ? N4 Dy1 Dy1 139.267(19) . 2 ? C2 O1 C1 114.27(9) . . ? C7 O2 Dy1 137.33(6) . . ? C19 O3 Dy1 128.90(6) . 2 ? C19 O3 Dy1 118.14(6) . . ? Dy1 O3 Dy1 108.22(3) 2 . ? C18 O4 C20 117.06(8) . . ? N4 O5 Dy1 96.93(6) . . ? N4 O6 Dy1 93.91(6) . . ? C8 N1 C9 114.40(9) . . ? C8 N1 Dy1 126.65(7) . . ? C9 N1 Dy1 117.95(6) . . ? C10 N2 C11 113.06(8) . . ? C10 N2 Dy1 110.99(6) . . ? C11 N2 Dy1 111.94(6) . . ? C10 N2 H12 109.4(11) . . ? C11 N2 H12 107.1(11) . . ? Dy1 N2 H12 103.8(11) . . ? C13 N3 C12 116.83(8) . . ? C13 N3 Dy1 126.17(7) . . ? C12 N3 Dy1 116.98(6) . . ? O7 N4 O6 122.54(9) . . ? O7 N4 O5 120.99(9) . . ? O6 N4 O5 116.47(8) . . ? O7 N4 Dy1 172.64(8) . . ? O6 N4 Dy1 60.19(5) . . ? O5 N4 Dy1 56.80(5) . . ? O1 C1 H20 106.2(12) . . ? O1 C1 H21 111.0(12) . . ? H20 C1 H21 111.1(17) . . ? O1 C1 H23 108.5(15) . . ? H20 C1 H23 113.5(19) . . ? H21 C1 H23 106.5(19) . . ? O1 C2 C3 117.99(9) . . ? O1 C2 C7 120.95(9) . . ? C3 C2 C7 120.85(9) . . ? C2 C3 C4 121.19(10) . . ? C2 C3 H22 115.8(11) . . ? C4 C3 H22 122.9(11) . . ? C5 C4 C3 119.16(9) . . ? C5 C4 H19 119.8(11) . . ? C3 C4 H19 121.1(11) . . ? C4 C5 C6 120.70(10) . . ? C4 C5 H18 121.7(10) . . ? C6 C5 H18 117.6(10) . . ? C5 C6 C7 120.79(9) . . ? C5 C6 C8 116.72(9) . . ? C7 C6 C8 122.49(9) . . ? O2 C7 C6 122.59(9) . . ? O2 C7 C2 120.45(9) . . ? C6 C7 C2 116.95(9) . . ? N1 C8 C6 127.02(9) . . ? N1 C8 H17 126.0(11) . . ? C6 C8 H17 106.9(11) . . ? N1 C9 C10 110.23(8) . . ? N1 C9 H15 110.0(10) . . ? C10 C9 H15 110.4(10) . . ? N1 C9 H16 106.3(10) . . ? C10 C9 H16 108.2(9) . . ? H15 C9 H16 111.7(14) . . ? N2 C10 C9 108.99(8) . . ? N2 C10 H13 110.0(10) . . ? C9 C10 H13 109.8(9) . . ? N2 C10 H14 109.7(12) . . ? C9 C10 H14 111.5(11) . . ? H13 C10 H14 106.8(15) . . ? N2 C11 C12 108.18(8) . . ? N2 C11 H10 111.2(11) . . ? C12 C11 H10 111.6(11) . . ? N2 C11 H11 107.6(10) . . ? C12 C11 H11 112.6(10) . . ? H10 C11 H11 105.5(15) . . ? N3 C12 C11 108.49(8) . . ? N3 C12 H8 111.9(11) . . ? C11 C12 H8 111.6(11) . . ? N3 C12 H9 108.0(10) . . ? C11 C12 H9 109.3(10) . . ? H8 C12 H9 107.5(14) . . ? N3 C13 C14 123.99(9) . . ? N3 C13 H7 118.5(11) . . ? C14 C13 H7 117.5(11) . . ? C15 C14 C19 120.55(9) . . ? C15 C14 C13 117.05(8) . . ? C19 C14 C13 122.36(8) . . ? C16 C15 C14 120.56(9) . . ? C16 C15 H3 121.9(11) . . ? C14 C15 H3 117.4(11) . . ? C15 C16 C17 119.59(9) . . ? C15 C16 H1 120.1(11) . . ? C17 C16 H1 120.3(11) . . ? C18 C17 C16 120.45(9) . . ? C18 C17 H2 119.8(11) . . ? C16 C17 H2 119.8(11) . . ? O4 C18 C17 123.78(9) . . ? O4 C18 C19 115.30(8) . . ? C17 C18 C19 120.92(9) . . ? O3 C19 C14 122.13(8) . . ? O3 C19 C18 120.17(8) . . ? C14 C19 C18 117.68(8) . . ? O4 C20 H4 110.3(12) . . ? O4 C20 H5 106.8(11) . . ? H4 C20 H5 110.8(16) . . ? O4 C20 H6 111.1(12) . . ? H4 C20 H6 110.3(17) . . ? H5 C20 H6 107.4(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 36.43 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.117 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.093 data_mm008a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Eu2 N8 O14' _chemical_formula_weight 1166.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5977(5) _cell_length_b 10.6420(5) _cell_length_c 11.5192(6) _cell_angle_alpha 65.341(2) _cell_angle_beta 64.813(2) _cell_angle_gamma 80.419(2) _cell_volume 1068.32(9) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 2.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5467 _exptl_absorpt_correction_T_max 0.7158 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19057 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.54 _reflns_number_total 6170 _reflns_number_gt 5886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.3377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6170 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.649559(7) 0.580112(8) -0.000901(7) 0.01666(3) Uani 1 1 d . . . N1 N 0.89291(15) 0.48538(17) -0.09391(15) 0.0227(3) Uani 1 1 d . . . N2 N 0.80461(15) 0.73081(16) -0.25225(15) 0.0229(3) Uani 1 1 d . . . H2A H 0.7969 0.6938 -0.3092 0.027 Uiso 1 1 calc R . . N3 N 0.52630(16) 0.79232(16) -0.11721(15) 0.0232(3) Uani 1 1 d . . . N4 N 0.68304(17) 0.74551(18) 0.13189(17) 0.0286(3) Uani 1 1 d . . . O1 O 0.67795(13) 0.40070(14) 0.17497(13) 0.0257(3) Uani 1 1 d . . . O2 O 0.57164(14) 0.18759(15) 0.43591(14) 0.0310(3) Uani 1 1 d . . . O3 O 0.40355(12) 0.54210(13) 0.10649(12) 0.0198(2) Uani 1 1 d . . . O4 O 0.22808(19) 0.43701(16) 0.38501(15) 0.0388(4) Uani 1 1 d . . . O5 O 0.77071(15) 0.74877(17) 0.01321(14) 0.0338(3) Uani 1 1 d . . . O6 O 0.57223(14) 0.67716(17) 0.18418(15) 0.0335(3) Uani 1 1 d . . . O7 O 0.7060(2) 0.8054(2) 0.1904(2) 0.0585(6) Uani 1 1 d . . . C1 C 0.73615(18) 0.27979(19) 0.19440(18) 0.0219(3) Uani 1 1 d . . . C2 C 0.68219(19) 0.1674(2) 0.32538(18) 0.0249(3) Uani 1 1 d . . . C3 C 0.7316(2) 0.0358(2) 0.3426(2) 0.0311(4) Uani 1 1 d . . . H3A H 0.6888 -0.0386 0.4292 0.037 Uiso 1 1 calc R . . C4 C 0.8439(2) 0.0094(2) 0.2350(2) 0.0322(4) Uani 1 1 d . . . H4A H 0.8758 -0.0823 0.2474 0.039 Uiso 1 1 calc R . . C5 C 0.9074(2) 0.1177(2) 0.1112(2) 0.0281(4) Uani 1 1 d . . . H5A H 0.9877 0.1015 0.0399 0.034 Uiso 1 1 calc R . . C6 C 0.85501(18) 0.2523(2) 0.08867(18) 0.0230(3) Uani 1 1 d . . . C7 C 0.6091(3) 0.2714(3) 0.4871(2) 0.0414(5) Uani 1 1 d . . . H7A H 0.5275 0.2825 0.5650 0.062 Uiso 1 1 calc R . . H7B H 0.6417 0.3624 0.4125 0.062 Uiso 1 1 calc R . . H7C H 0.6836 0.2266 0.5189 0.062 Uiso 1 1 calc R . . C8 C 0.92959(17) 0.3601(2) -0.04458(18) 0.0242(3) Uani 1 1 d . . . H8A H 1.0161 0.3348 -0.1022 0.029 Uiso 1 1 calc R . . C9 C 0.99429(19) 0.5710(2) -0.23240(19) 0.0291(4) Uani 1 1 d . . . H9A H 0.9991 0.5376 -0.3025 0.035 Uiso 1 1 calc R . . H9B H 1.0880 0.5622 -0.2307 0.035 Uiso 1 1 calc R . . C10 C 0.95242(18) 0.7203(2) -0.27266(18) 0.0265(4) Uani 1 1 d . . . H10A H 0.9665 0.7596 -0.2148 0.032 Uiso 1 1 calc R . . H10B H 1.0112 0.7736 -0.3714 0.032 Uiso 1 1 calc R . . C11 C 0.7573(2) 0.8738(2) -0.29628(19) 0.0283(4) Uani 1 1 d . . . H11A H 0.8110 0.9243 -0.3971 0.034 Uiso 1 1 calc R . . H11B H 0.7724 0.9212 -0.2452 0.034 Uiso 1 1 calc R . . C12 C 0.6033(2) 0.8730(2) -0.26609(19) 0.0290(4) Uani 1 1 d . . . H12A H 0.5686 0.9689 -0.2914 0.035 Uiso 1 1 calc R . . H12B H 0.5891 0.8314 -0.3222 0.035 Uiso 1 1 calc R . . C13 C 0.40814(19) 0.83875(19) -0.05692(19) 0.0242(3) Uani 1 1 d . . . H13A H 0.3782 0.9233 -0.1109 0.029 Uiso 1 1 calc R . . C14 C 0.31945(16) 0.62749(18) 0.16505(17) 0.0198(3) Uani 1 1 d . . . C15 C 0.31589(17) 0.77044(19) 0.08952(18) 0.0218(3) Uani 1 1 d . . . C16 C 0.2205(2) 0.8545(2) 0.1527(2) 0.0296(4) Uani 1 1 d . . . H16A H 0.2168 0.9501 0.0990 0.035 Uiso 1 1 calc R . . C17 C 0.1319(2) 0.8005(3) 0.2917(2) 0.0374(5) Uani 1 1 d . . . H17A H 0.0688 0.8585 0.3341 0.045 Uiso 1 1 calc R . . C18 C 0.1364(2) 0.6616(2) 0.3676(2) 0.0354(4) Uani 1 1 d . . . H18A H 0.0753 0.6236 0.4631 0.042 Uiso 1 1 calc R . . C19 C 0.2288(2) 0.5759(2) 0.30729(18) 0.0266(4) Uani 1 1 d . . . C20 C 0.3032(5) 0.3992(4) 0.4659(5) 0.0883(14) Uani 1 1 d . . . H20A H 0.2953 0.2989 0.5185 0.132 Uiso 1 1 calc R . . H20B H 0.2666 0.4463 0.5307 0.132 Uiso 1 1 calc R . . H20C H 0.4014 0.4254 0.4063 0.132 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01737(4) 0.01616(5) 0.01563(4) -0.00511(3) -0.00593(3) -0.00243(3) N1 0.0196(6) 0.0260(8) 0.0198(6) -0.0073(6) -0.0057(5) -0.0031(5) N2 0.0238(6) 0.0246(8) 0.0202(6) -0.0070(6) -0.0078(5) -0.0063(5) N3 0.0258(7) 0.0208(7) 0.0194(6) -0.0035(6) -0.0091(5) -0.0023(5) N4 0.0321(8) 0.0298(9) 0.0290(7) -0.0148(7) -0.0122(6) -0.0033(6) O1 0.0267(6) 0.0245(7) 0.0206(6) -0.0062(5) -0.0085(5) 0.0044(5) O2 0.0306(7) 0.0317(8) 0.0234(6) -0.0063(6) -0.0067(5) -0.0049(5) O3 0.0197(5) 0.0190(6) 0.0210(5) -0.0098(5) -0.0057(4) -0.0013(4) O4 0.0643(10) 0.0251(8) 0.0249(6) -0.0046(6) -0.0158(7) -0.0130(7) O5 0.0319(7) 0.0414(9) 0.0291(7) -0.0176(6) -0.0041(5) -0.0137(6) O6 0.0292(6) 0.0426(9) 0.0316(7) -0.0218(6) -0.0037(5) -0.0096(6) O7 0.0627(11) 0.0781(15) 0.0535(10) -0.0443(11) -0.0119(9) -0.0257(10) C1 0.0237(7) 0.0220(8) 0.0217(7) -0.0066(7) -0.0122(6) 0.0001(6) C2 0.0268(8) 0.0250(9) 0.0227(8) -0.0061(7) -0.0117(6) -0.0023(7) C3 0.0376(10) 0.0252(10) 0.0302(9) -0.0037(8) -0.0192(8) -0.0028(8) C4 0.0393(10) 0.0222(9) 0.0408(11) -0.0118(8) -0.0230(9) 0.0048(8) C5 0.0295(8) 0.0277(10) 0.0345(9) -0.0158(8) -0.0173(7) 0.0051(7) C6 0.0230(7) 0.0245(9) 0.0249(8) -0.0104(7) -0.0120(6) 0.0016(6) C7 0.0427(11) 0.0525(15) 0.0302(10) -0.0201(10) -0.0096(9) -0.0049(10) C8 0.0196(7) 0.0314(10) 0.0237(8) -0.0127(7) -0.0088(6) 0.0015(6) C9 0.0217(8) 0.0346(11) 0.0219(8) -0.0074(8) -0.0024(6) -0.0041(7) C10 0.0219(7) 0.0307(10) 0.0211(7) -0.0059(7) -0.0040(6) -0.0091(7) C11 0.0319(9) 0.0233(9) 0.0223(8) -0.0009(7) -0.0089(7) -0.0082(7) C12 0.0317(9) 0.0267(10) 0.0195(8) -0.0003(7) -0.0099(7) -0.0017(7) C13 0.0307(8) 0.0187(8) 0.0249(8) -0.0063(7) -0.0149(7) 0.0010(6) C14 0.0182(7) 0.0222(8) 0.0214(7) -0.0106(6) -0.0073(6) -0.0012(6) C15 0.0227(7) 0.0219(8) 0.0236(7) -0.0102(7) -0.0111(6) 0.0021(6) C16 0.0310(9) 0.0267(10) 0.0353(9) -0.0169(8) -0.0148(8) 0.0076(7) C17 0.0347(10) 0.0411(13) 0.0374(10) -0.0264(10) -0.0060(8) 0.0048(9) C18 0.0382(10) 0.0384(12) 0.0268(9) -0.0195(9) -0.0019(8) -0.0044(9) C19 0.0314(9) 0.0260(9) 0.0218(8) -0.0104(7) -0.0066(7) -0.0064(7) C20 0.150(4) 0.0436(18) 0.137(4) -0.036(2) -0.125(3) 0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.2226(13) . ? Eu1 O3 2.3736(11) 2_665 ? Eu1 O3 2.3832(11) . ? Eu1 O5 2.4668(13) . ? Eu1 O6 2.5204(13) . ? Eu1 N1 2.5493(15) . ? Eu1 N3 2.5660(16) . ? Eu1 N2 2.5706(14) . ? Eu1 N4 2.9121(15) . ? Eu1 C14 3.2668(16) . ? Eu1 Eu1 3.8301(2) 2_665 ? N1 C8 1.278(3) . ? N1 C9 1.478(2) . ? N2 C11 1.464(3) . ? N2 C10 1.474(2) . ? N3 C13 1.279(2) . ? N3 C12 1.469(2) . ? N4 O7 1.212(2) . ? N4 O6 1.260(2) . ? N4 O5 1.274(2) . ? O1 C1 1.304(2) . ? O2 C2 1.384(2) . ? O2 C7 1.434(3) . ? O3 C14 1.3437(19) . ? O3 Eu1 2.3735(11) 2_665 ? O4 C19 1.371(2) . ? O4 C20 1.369(3) . ? C1 C6 1.423(2) . ? C1 C2 1.422(3) . ? C2 C3 1.374(3) . ? C3 C4 1.398(3) . ? C4 C5 1.373(3) . ? C5 C6 1.405(3) . ? C6 C8 1.448(3) . ? C9 C10 1.504(3) . ? C11 C12 1.517(3) . ? C13 C15 1.463(2) . ? C14 C15 1.406(3) . ? C14 C19 1.412(2) . ? C15 C16 1.403(2) . ? C16 C17 1.381(3) . ? C17 C18 1.373(3) . ? C18 C19 1.388(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O3 98.81(5) . 2_665 ? O1 Eu1 O3 91.24(5) . . ? O3 Eu1 O3 72.74(4) 2_665 . ? O1 Eu1 O5 95.38(5) . . ? O3 Eu1 O5 157.35(4) 2_665 . ? O3 Eu1 O5 124.66(4) . . ? O1 Eu1 O6 78.11(5) . . ? O3 Eu1 O6 149.64(4) 2_665 . ? O3 Eu1 O6 77.11(4) . . ? O5 Eu1 O6 51.16(4) . . ? O1 Eu1 N1 72.03(5) . . ? O3 Eu1 N1 83.23(4) 2_665 . ? O3 Eu1 N1 148.32(4) . . ? O5 Eu1 N1 84.48(5) . . ? O6 Eu1 N1 123.04(5) . . ? O1 Eu1 N3 156.06(5) . . ? O3 Eu1 N3 89.27(5) 2_665 . ? O3 Eu1 N3 69.58(4) . . ? O5 Eu1 N3 84.76(5) . . ? O6 Eu1 N3 83.54(5) . . ? N1 Eu1 N3 131.59(5) . . ? O1 Eu1 N2 136.83(5) . . ? O3 Eu1 N2 84.31(4) 2_665 . ? O3 Eu1 N2 129.87(5) . . ? O5 Eu1 N2 73.29(4) . . ? O6 Eu1 N2 118.78(5) . . ? N1 Eu1 N2 65.58(5) . . ? N3 Eu1 N2 66.11(5) . . ? O1 Eu1 N4 84.76(5) . . ? O3 Eu1 N4 173.26(4) 2_665 . ? O3 Eu1 N4 101.58(4) . . ? O5 Eu1 N4 25.74(4) . . ? O6 Eu1 N4 25.54(4) . . ? N1 Eu1 N4 103.36(5) . . ? N3 Eu1 N4 85.26(5) . . ? N2 Eu1 N4 97.04(5) . . ? O1 Eu1 C14 96.91(5) . . ? O3 Eu1 C14 91.79(4) 2_665 . ? O3 Eu1 C14 20.90(4) . . ? O5 Eu1 C14 103.97(4) . . ? O6 Eu1 C14 59.13(4) . . ? N1 Eu1 C14 166.89(5) . . ? N3 Eu1 C14 60.14(5) . . ? N2 Eu1 C14 126.14(5) . . ? N4 Eu1 C14 82.07(4) . . ? O1 Eu1 Eu1 96.22(4) . 2_665 ? O3 Eu1 Eu1 36.46(3) 2_665 2_665 ? O3 Eu1 Eu1 36.28(3) . 2_665 ? O5 Eu1 Eu1 157.78(4) . 2_665 ? O6 Eu1 Eu1 113.33(3) . 2_665 ? N1 Eu1 Eu1 117.16(3) . 2_665 ? N3 Eu1 Eu1 77.00(3) . 2_665 ? N2 Eu1 Eu1 109.72(3) . 2_665 ? N4 Eu1 Eu1 137.75(3) . 2_665 ? C14 Eu1 Eu1 55.81(3) . 2_665 ? C8 N1 C9 114.51(15) . . ? C8 N1 Eu1 125.74(11) . . ? C9 N1 Eu1 118.46(12) . . ? C11 N2 C10 113.05(14) . . ? C11 N2 Eu1 112.71(10) . . ? C10 N2 Eu1 110.81(11) . . ? C13 N3 C12 116.93(16) . . ? C13 N3 Eu1 126.44(12) . . ? C12 N3 Eu1 116.51(12) . . ? O7 N4 O6 122.29(17) . . ? O7 N4 O5 121.30(17) . . ? O6 N4 O5 116.41(14) . . ? O7 N4 Eu1 173.91(17) . . ? O6 N4 Eu1 59.58(8) . . ? O5 N4 Eu1 57.21(8) . . ? C1 O1 Eu1 137.32(11) . . ? C2 O2 C7 112.71(15) . . ? C14 O3 Eu1 127.02(10) . 2_665 ? C14 O3 Eu1 119.85(9) . . ? Eu1 O3 Eu1 107.26(4) 2_665 . ? C19 O4 C20 115.3(2) . . ? N4 O5 Eu1 97.05(10) . . ? N4 O6 Eu1 94.88(10) . . ? O1 C1 C6 122.93(16) . . ? O1 C1 C2 120.61(16) . . ? C6 C1 C2 116.46(17) . . ? C3 C2 O2 118.66(17) . . ? C3 C2 C1 121.19(17) . . ? O2 C2 C1 120.01(17) . . ? C2 C3 C4 121.15(19) . . ? C5 C4 C3 119.19(19) . . ? C4 C5 C6 120.74(18) . . ? C5 C6 C1 120.78(17) . . ? C5 C6 C8 116.86(16) . . ? C1 C6 C8 122.34(17) . . ? N1 C8 C6 127.73(16) . . ? N1 C9 C10 110.63(15) . . ? N2 C10 C9 109.53(15) . . ? N2 C11 C12 108.82(15) . . ? N3 C12 C11 109.05(15) . . ? N3 C13 C15 124.42(17) . . ? O3 C14 C15 122.51(15) . . ? O3 C14 C19 120.67(16) . . ? C15 C14 C19 116.82(15) . . ? O3 C14 Eu1 39.25(7) . . ? C15 C14 Eu1 98.03(10) . . ? C19 C14 Eu1 132.92(13) . . ? C14 C15 C16 120.58(16) . . ? C14 C15 C13 122.67(15) . . ? C16 C15 C13 116.74(17) . . ? C17 C16 C15 121.1(2) . . ? C18 C17 C16 118.89(18) . . ? C17 C18 C19 121.17(18) . . ? O4 C19 C18 119.69(17) . . ? O4 C19 C14 118.91(16) . . ? C18 C19 C14 121.32(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 N1 C8 27.87(13) . . . . ? O3 Eu1 N1 C8 -73.71(14) 2_665 . . . ? O3 Eu1 N1 C8 -33.30(18) . . . . ? O5 Eu1 N1 C8 125.36(14) . . . . ? O6 Eu1 N1 C8 89.89(14) . . . . ? N3 Eu1 N1 C8 -156.67(13) . . . . ? N2 Eu1 N1 C8 -160.51(15) . . . . ? N4 Eu1 N1 C8 107.75(14) . . . . ? C14 Eu1 N1 C8 -5.5(3) . . . . ? Eu1 Eu1 N1 C8 -59.93(14) 2_665 . . . ? O1 Eu1 N1 C9 -165.89(13) . . . . ? O3 Eu1 N1 C9 92.54(12) 2_665 . . . ? O3 Eu1 N1 C9 132.95(12) . . . . ? O5 Eu1 N1 C9 -68.40(12) . . . . ? O6 Eu1 N1 C9 -103.87(13) . . . . ? N3 Eu1 N1 C9 9.57(15) . . . . ? N2 Eu1 N1 C9 5.73(12) . . . . ? N4 Eu1 N1 C9 -86.01(13) . . . . ? C14 Eu1 N1 C9 160.73(16) . . . . ? Eu1 Eu1 N1 C9 106.31(12) 2_665 . . . ? O1 Eu1 N2 C11 -147.89(11) . . . . ? O3 Eu1 N2 C11 115.29(11) 2_665 . . . ? O3 Eu1 N2 C11 53.44(12) . . . . ? O5 Eu1 N2 C11 -68.08(11) . . . . ? O6 Eu1 N2 C11 -43.87(12) . . . . ? N1 Eu1 N2 C11 -159.58(12) . . . . ? N3 Eu1 N2 C11 23.56(11) . . . . ? N4 Eu1 N2 C11 -58.06(11) . . . . ? C14 Eu1 N2 C11 27.24(13) . . . . ? Eu1 Eu1 N2 C11 88.72(11) 2_665 . . . ? O1 Eu1 N2 C10 -20.07(14) . . . . ? O3 Eu1 N2 C10 -116.89(11) 2_665 . . . ? O3 Eu1 N2 C10 -178.74(10) . . . . ? O5 Eu1 N2 C10 59.73(11) . . . . ? O6 Eu1 N2 C10 83.94(12) . . . . ? N1 Eu1 N2 C10 -31.76(11) . . . . ? N3 Eu1 N2 C10 151.38(12) . . . . ? N4 Eu1 N2 C10 69.76(12) . . . . ? C14 Eu1 N2 C10 155.05(10) . . . . ? Eu1 Eu1 N2 C10 -143.46(10) 2_665 . . . ? O1 Eu1 N3 C13 -3.1(2) . . . . ? O3 Eu1 N3 C13 107.31(14) 2_665 . . . ? O3 Eu1 N3 C13 35.48(14) . . . . ? O5 Eu1 N3 C13 -94.57(14) . . . . ? O6 Eu1 N3 C13 -43.14(14) . . . . ? N1 Eu1 N3 C13 -172.41(13) . . . . ? N2 Eu1 N3 C13 -168.60(16) . . . . ? N4 Eu1 N3 C13 -68.74(14) . . . . ? C14 Eu1 N3 C13 14.83(13) . . . . ? Eu1 Eu1 N3 C13 72.66(14) 2_665 . . . ? O1 Eu1 N3 C12 172.87(12) . . . . ? O3 Eu1 N3 C12 -76.71(12) 2_665 . . . ? O3 Eu1 N3 C12 -148.54(13) . . . . ? O5 Eu1 N3 C12 81.41(12) . . . . ? O6 Eu1 N3 C12 132.84(12) . . . . ? N1 Eu1 N3 C12 3.56(15) . . . . ? N2 Eu1 N3 C12 7.38(12) . . . . ? N4 Eu1 N3 C12 107.24(12) . . . . ? C14 Eu1 N3 C12 -169.19(14) . . . . ? Eu1 Eu1 N3 C12 -111.36(12) 2_665 . . . ? O1 Eu1 N4 O7 36.3(14) . . . . ? O3 Eu1 N4 O7 158.6(12) 2_665 . . . ? O3 Eu1 N4 O7 126.5(14) . . . . ? O5 Eu1 N4 O7 -77.7(14) . . . . ? O6 Eu1 N4 O7 109.6(14) . . . . ? N1 Eu1 N4 O7 -33.8(14) . . . . ? N3 Eu1 N4 O7 -165.5(14) . . . . ? N2 Eu1 N4 O7 -100.3(14) . . . . ? C14 Eu1 N4 O7 134.1(14) . . . . ? Eu1 Eu1 N4 O7 129.8(14) 2_665 . . . ? O1 Eu1 N4 O6 -73.27(12) . . . . ? O3 Eu1 N4 O6 49.0(4) 2_665 . . . ? O3 Eu1 N4 O6 16.92(13) . . . . ? O5 Eu1 N4 O6 172.7(2) . . . . ? N1 Eu1 N4 O6 -143.39(12) . . . . ? N3 Eu1 N4 O6 84.94(12) . . . . ? N2 Eu1 N4 O6 150.12(12) . . . . ? C14 Eu1 N4 O6 24.47(12) . . . . ? Eu1 Eu1 N4 O6 20.21(14) 2_665 . . . ? O1 Eu1 N4 O5 114.03(12) . . . . ? O3 Eu1 N4 O5 -123.7(4) 2_665 . . . ? O3 Eu1 N4 O5 -155.78(12) . . . . ? O6 Eu1 N4 O5 -172.7(2) . . . . ? N1 Eu1 N4 O5 43.91(13) . . . . ? N3 Eu1 N4 O5 -87.76(12) . . . . ? N2 Eu1 N4 O5 -22.58(13) . . . . ? C14 Eu1 N4 O5 -148.23(12) . . . . ? Eu1 Eu1 N4 O5 -152.49(10) 2_665 . . . ? O3 Eu1 O1 C1 41.68(17) 2_665 . . . ? O3 Eu1 O1 C1 114.41(16) . . . . ? O5 Eu1 O1 C1 -120.61(16) . . . . ? O6 Eu1 O1 C1 -169.04(17) . . . . ? N1 Eu1 O1 C1 -38.20(16) . . . . ? N3 Eu1 O1 C1 150.19(15) . . . . ? N2 Eu1 O1 C1 -49.38(19) . . . . ? N4 Eu1 O1 C1 -144.08(17) . . . . ? C14 Eu1 O1 C1 134.58(16) . . . . ? Eu1 Eu1 O1 C1 78.37(16) 2_665 . . . ? O1 Eu1 O3 C14 106.31(12) . . . . ? O3 Eu1 O3 C14 -154.85(15) 2_665 . . . ? O5 Eu1 O3 C14 8.90(14) . . . . ? O6 Eu1 O3 C14 28.80(12) . . . . ? N1 Eu1 O3 C14 162.76(11) . . . . ? N3 Eu1 O3 C14 -59.03(12) . . . . ? N2 Eu1 O3 C14 -88.11(12) . . . . ? N4 Eu1 O3 C14 21.40(13) . . . . ? Eu1 Eu1 O3 C14 -154.85(15) 2_665 . . . ? O1 Eu1 O3 Eu1 -98.84(5) . . . 2_665 ? O3 Eu1 O3 Eu1 0.0 2_665 . . 2_665 ? O5 Eu1 O3 Eu1 163.75(5) . . . 2_665 ? O6 Eu1 O3 Eu1 -176.35(6) . . . 2_665 ? N1 Eu1 O3 Eu1 -42.38(10) . . . 2_665 ? N3 Eu1 O3 Eu1 95.83(6) . . . 2_665 ? N2 Eu1 O3 Eu1 66.75(7) . . . 2_665 ? N4 Eu1 O3 Eu1 176.26(5) . . . 2_665 ? C14 Eu1 O3 Eu1 154.85(15) . . . 2_665 ? O7 N4 O5 Eu1 173.0(2) . . . . ? O6 N4 O5 Eu1 -7.03(19) . . . . ? O1 Eu1 O5 N4 -66.00(12) . . . . ? O3 Eu1 O5 N4 165.31(11) 2_665 . . . ? O3 Eu1 O5 N4 29.25(14) . . . . ? O6 Eu1 O5 N4 4.03(11) . . . . ? N1 Eu1 O5 N4 -137.32(12) . . . . ? N3 Eu1 O5 N4 89.95(12) . . . . ? N2 Eu1 O5 N4 156.56(13) . . . . ? C14 Eu1 O5 N4 32.51(13) . . . . ? Eu1 Eu1 O5 N4 55.22(17) 2_665 . . . ? O7 N4 O6 Eu1 -173.2(2) . . . . ? O5 N4 O6 Eu1 6.85(18) . . . . ? O1 Eu1 O6 N4 102.94(12) . . . . ? O3 Eu1 O6 N4 -169.90(10) 2_665 . . . ? O3 Eu1 O6 N4 -163.00(13) . . . . ? O5 Eu1 O6 N4 -4.06(11) . . . . ? N1 Eu1 O6 N4 43.80(14) . . . . ? N3 Eu1 O6 N4 -92.52(12) . . . . ? N2 Eu1 O6 N4 -34.34(13) . . . . ? C14 Eu1 O6 N4 -151.45(14) . . . . ? Eu1 Eu1 O6 N4 -165.35(11) 2_665 . . . ? Eu1 O1 C1 C6 30.2(3) . . . . ? Eu1 O1 C1 C2 -149.85(13) . . . . ? C7 O2 C2 C3 115.2(2) . . . . ? C7 O2 C2 C1 -69.0(2) . . . . ? O1 C1 C2 C3 172.11(16) . . . . ? C6 C1 C2 C3 -8.0(2) . . . . ? O1 C1 C2 O2 -3.5(2) . . . . ? C6 C1 C2 O2 176.39(15) . . . . ? O2 C2 C3 C4 -179.40(17) . . . . ? C1 C2 C3 C4 4.9(3) . . . . ? C2 C3 C4 C5 1.4(3) . . . . ? C3 C4 C5 C6 -4.3(3) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C4 C5 C6 C8 179.41(16) . . . . ? O1 C1 C6 C5 -174.98(16) . . . . ? C2 C1 C6 C5 5.1(2) . . . . ? O1 C1 C6 C8 6.6(3) . . . . ? C2 C1 C6 C8 -173.33(15) . . . . ? C9 N1 C8 C6 178.61(16) . . . . ? Eu1 N1 C8 C6 -14.7(2) . . . . ? C5 C6 C8 N1 171.36(17) . . . . ? C1 C6 C8 N1 -10.2(3) . . . . ? C8 N1 C9 C10 -171.94(15) . . . . ? Eu1 N1 C9 C10 20.31(19) . . . . ? C11 N2 C10 C9 -176.89(14) . . . . ? Eu1 N2 C10 C9 55.48(15) . . . . ? N1 C9 C10 N2 -49.62(19) . . . . ? C10 N2 C11 C12 -177.94(14) . . . . ? Eu1 N2 C11 C12 -51.31(16) . . . . ? C13 N3 C12 C11 140.56(17) . . . . ? Eu1 N3 C12 C11 -35.82(19) . . . . ? N2 C11 C12 N3 57.02(19) . . . . ? C12 N3 C13 C15 178.44(16) . . . . ? Eu1 N3 C13 C15 -5.6(2) . . . . ? Eu1 O3 C14 C15 -90.65(17) 2_665 . . . ? Eu1 O3 C14 C15 58.80(18) . . . . ? Eu1 O3 C14 C19 88.86(18) 2_665 . . . ? Eu1 O3 C14 C19 -121.69(14) . . . . ? Eu1 O3 C14 Eu1 -149.45(17) 2_665 . . . ? O1 Eu1 C14 O3 -75.14(12) . . . . ? O3 Eu1 C14 O3 23.96(14) 2_665 . . . ? O5 Eu1 C14 O3 -172.47(12) . . . . ? O6 Eu1 C14 O3 -146.83(14) . . . . ? N1 Eu1 C14 O3 -43.3(2) . . . . ? N3 Eu1 C14 O3 112.09(13) . . . . ? N2 Eu1 C14 O3 108.21(12) . . . . ? N4 Eu1 C14 O3 -158.84(12) . . . . ? Eu1 Eu1 C14 O3 17.70(10) 2_665 . . . ? O1 Eu1 C14 C15 151.62(10) . . . . ? O3 Eu1 C14 C15 -109.28(10) 2_665 . . . ? O3 Eu1 C14 C15 -133.24(17) . . . . ? O5 Eu1 C14 C15 54.30(10) . . . . ? O6 Eu1 C14 C15 79.93(10) . . . . ? N1 Eu1 C14 C15 -176.57(16) . . . . ? N3 Eu1 C14 C15 -21.14(9) . . . . ? N2 Eu1 C14 C15 -25.02(11) . . . . ? N4 Eu1 C14 C15 67.92(10) . . . . ? Eu1 Eu1 C14 C15 -115.54(10) 2_665 . . . ? O1 Eu1 C14 C19 12.73(16) . . . . ? O3 Eu1 C14 C19 111.83(15) 2_665 . . . ? O3 Eu1 C14 C19 87.88(19) . . . . ? O5 Eu1 C14 C19 -84.59(15) . . . . ? O6 Eu1 C14 C19 -58.96(15) . . . . ? N1 Eu1 C14 C19 44.5(3) . . . . ? N3 Eu1 C14 C19 -160.03(16) . . . . ? N2 Eu1 C14 C19 -163.91(14) . . . . ? N4 Eu1 C14 C19 -70.96(15) . . . . ? Eu1 Eu1 C14 C19 105.58(16) 2_665 . . . ? O3 C14 C15 C16 176.10(15) . . . . ? C19 C14 C15 C16 -3.4(2) . . . . ? Eu1 C14 C15 C16 -150.76(14) . . . . ? O3 C14 C15 C13 -3.1(2) . . . . ? C19 C14 C15 C13 177.38(15) . . . . ? Eu1 C14 C15 C13 30.03(17) . . . . ? N3 C13 C15 C14 -24.4(3) . . . . ? N3 C13 C15 C16 156.35(17) . . . . ? C14 C15 C16 C17 2.7(3) . . . . ? C13 C15 C16 C17 -178.01(18) . . . . ? C15 C16 C17 C18 -1.2(3) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C20 O4 C19 C18 -83.3(3) . . . . ? C20 O4 C19 C14 99.8(3) . . . . ? C17 C18 C19 O4 -178.24(19) . . . . ? C17 C18 C19 C14 -1.3(3) . . . . ? O3 C14 C19 O4 0.1(2) . . . . ? C15 C14 C19 O4 179.68(16) . . . . ? Eu1 C14 C19 O4 -47.2(2) . . . . ? O3 C14 C19 C18 -176.77(17) . . . . ? C15 C14 C19 C18 2.8(3) . . . . ? Eu1 C14 C19 C18 135.90(17) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.954 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.090 data_mm013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H23 Gd N4 O7' _chemical_formula_weight 588.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Gd' 'Gd' -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5766(5) _cell_length_b 10.5991(5) _cell_length_c 11.5192(5) _cell_angle_alpha 65.1840(10) _cell_angle_beta 65.4820(10) _cell_angle_gamma 80.2930(10) _cell_volume 1066.38(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9916 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.40 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 582 _exptl_absorpt_coefficient_mu 3.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5566 _exptl_absorpt_correction_T_max 0.7029 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10345 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3531 _reflns_number_gt 3445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3531 _refine_ls_number_parameters 307 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.147938(11) 0.082463(10) 0.498185(11) 0.01723(7) Uani 1 1 d . . . N1 N 0.3890(2) -0.0129(2) 0.4060(2) 0.0225(5) Uani 1 1 d . . . N2 N 0.2962(2) 0.2346(2) 0.2492(2) 0.0239(5) Uani 1 1 d . . . H2A H 0.2862 0.1986 0.1924 0.029 Uiso 1 1 calc R . . N3 N 0.0203(2) 0.2955(2) 0.3853(2) 0.0237(5) Uani 1 1 d . . . N4 N 0.1839(3) 0.2465(2) 0.6303(3) 0.0285(6) Uani 1 1 d . . . O1 O 0.17899(19) -0.09699(18) 0.67432(19) 0.0255(4) Uani 1 1 d . . . O2 O 0.0749(2) -0.31217(19) 0.9344(2) 0.0314(4) Uani 1 1 d . . . O3 O -0.09507(19) 0.04026(17) 0.60496(19) 0.0203(4) Uani 1 1 d . . . O5 O 0.2710(2) 0.2494(2) 0.5123(2) 0.0332(5) Uani 1 1 d . . . O6 O 0.0728(2) 0.1788(2) 0.6824(2) 0.0341(5) Uani 1 1 d . . . O7 O 0.2085(3) 0.3058(3) 0.6883(3) 0.0539(7) Uani 1 1 d . . . C1 C 0.2377(3) -0.2193(3) 0.6957(3) 0.0225(6) Uani 1 1 d . . . C2 C 0.1854(3) -0.3308(3) 0.8252(3) 0.0256(6) Uani 1 1 d . . . C3 C 0.2364(3) -0.4640(3) 0.8431(3) 0.0326(7) Uani 1 1 d . . . H3A H 0.1945 -0.5390 0.9290 0.039 Uiso 1 1 calc R . . C4 C 0.3483(3) -0.4895(3) 0.7367(3) 0.0323(7) Uani 1 1 d . . . H4A H 0.3820 -0.5814 0.7497 0.039 Uiso 1 1 calc R . . C5 C 0.4090(3) -0.3817(3) 0.6137(3) 0.0297(6) Uani 1 1 d . . . H5A H 0.4883 -0.3985 0.5430 0.036 Uiso 1 1 calc R . . C6 C 0.3563(3) -0.2460(3) 0.5896(3) 0.0241(6) Uani 1 1 d . . . C7 C 0.1099(4) -0.2235(4) 0.9835(4) 0.0470(8) Uani 1 1 d . . . H7A H 0.0286 -0.2136 1.0612 0.071 Uiso 1 1 calc R . . H7B H 0.1385 -0.1319 0.9084 0.071 Uiso 1 1 calc R . . H7C H 0.1863 -0.2648 1.0144 0.071 Uiso 1 1 calc R . . C8 C 0.4278(3) -0.1383(3) 0.4565(3) 0.0262(6) Uani 1 1 d . . . H8A H 0.5139 -0.1636 0.3994 0.031 Uiso 1 1 calc R . . C9 C 0.4863(3) 0.0721(3) 0.2674(3) 0.0313(7) Uani 1 1 d . . . H9A H 0.4873 0.0384 0.1989 0.038 Uiso 1 1 calc R . . H9B H 0.5813 0.0627 0.2668 0.038 Uiso 1 1 calc R . . C10 C 0.4445(3) 0.2232(3) 0.2271(3) 0.0275(6) Uani 1 1 d . . . H10A H 0.4611 0.2625 0.2838 0.033 Uiso 1 1 calc R . . H10B H 0.5013 0.2765 0.1284 0.033 Uiso 1 1 calc R . . C11 C 0.2480(3) 0.3792(3) 0.2070(3) 0.0295(6) Uani 1 1 d . . . H11A H 0.2999 0.4312 0.1068 0.035 Uiso 1 1 calc R . . H11B H 0.2642 0.4253 0.2588 0.035 Uiso 1 1 calc R . . C12 C 0.0944(3) 0.3781(3) 0.2378(3) 0.0297(6) Uani 1 1 d . . . H12A H 0.0587 0.4744 0.2140 0.036 Uiso 1 1 calc R . . H12B H 0.0792 0.3376 0.1813 0.036 Uiso 1 1 calc R . . C13 C -0.0994(3) 0.3377(3) 0.4465(3) 0.0246(6) Uani 1 1 d . . . H13A H -0.1336 0.4205 0.3932 0.030 Uiso 1 1 calc R . . C14 C -0.1788(3) 0.1233(3) 0.6670(3) 0.0218(6) Uani 1 1 d . A . C15 C -0.1870(3) 0.2680(3) 0.5921(3) 0.0229(6) Uani 1 1 d . . . C16 C -0.2820(3) 0.3495(3) 0.6580(3) 0.0309(6) Uani 1 1 d . . . H16A H -0.2908 0.4453 0.6060 0.037 Uiso 1 1 calc R . . C17 C -0.3630(3) 0.2922(3) 0.7976(3) 0.0382(7) Uani 1 1 d . . . H17A H -0.4266 0.3484 0.8419 0.046 Uiso 1 1 calc R . . C18 C -0.3509(4) 0.1522(3) 0.8729(3) 0.0406(8) Uani 1 1 d . A . H18A H -0.4058 0.1130 0.9694 0.049 Uiso 1 1 calc R . . C19 C -0.2603(3) 0.0690(3) 0.8097(3) 0.0293(6) Uani 1 1 d . . . O4' O -0.2762(18) -0.059(3) 0.888(2) 0.027(3) Uani 0.35 1 d PD A 1 C20' C -0.1729(12) -0.0973(11) 0.9470(12) 0.042(2) Uani 0.35 1 d PD A 1 H20A H -0.0808 -0.0693 0.8728 0.063 Uiso 0.35 1 calc PR A 1 H20B H -0.1754 -0.1982 0.9985 0.063 Uiso 0.35 1 calc PR A 1 H20C H -0.1919 -0.0506 1.0100 0.063 Uiso 0.35 1 calc PR A 1 O4 O -0.2342(11) -0.0762(14) 0.8782(12) 0.0334(19) Uani 0.65 1 d PD A 2 C20 C -0.2491(8) -0.1222(6) 1.0165(6) 0.0432(14) Uani 0.65 1 d PD A 2 H20D H -0.2414 -0.2237 1.0552 0.065 Uiso 0.65 1 calc PR A 2 H20E H -0.3402 -0.0947 1.0703 0.065 Uiso 0.65 1 calc PR A 2 H20F H -0.1759 -0.0804 1.0206 0.065 Uiso 0.65 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01858(9) 0.01774(10) 0.01311(9) -0.00428(7) -0.00434(6) -0.00373(6) N1 0.0201(12) 0.0261(12) 0.0176(12) -0.0066(11) -0.0043(9) -0.0039(9) N2 0.0259(12) 0.0265(11) 0.0184(12) -0.0073(10) -0.0056(9) -0.0088(9) N3 0.0288(13) 0.0212(11) 0.0167(12) -0.0011(10) -0.0090(10) -0.0056(9) N4 0.0358(15) 0.0299(13) 0.0262(14) -0.0148(12) -0.0133(11) -0.0010(11) O1 0.0261(10) 0.0261(10) 0.0169(10) -0.0039(9) -0.0072(8) 0.0034(8) O2 0.0327(11) 0.0332(11) 0.0213(11) -0.0060(10) -0.0057(9) -0.0076(9) O3 0.0202(10) 0.0189(9) 0.0191(10) -0.0076(8) -0.0037(8) -0.0033(7) O5 0.0333(12) 0.0392(11) 0.0256(12) -0.0125(10) -0.0040(9) -0.0156(9) O6 0.0286(11) 0.0451(12) 0.0307(12) -0.0208(10) -0.0030(9) -0.0112(9) O7 0.0636(17) 0.0673(16) 0.0461(16) -0.0353(14) -0.0130(13) -0.0228(13) C1 0.0237(14) 0.0250(14) 0.0196(16) -0.0055(13) -0.0110(12) -0.0029(11) C2 0.0248(14) 0.0289(14) 0.0200(15) -0.0044(13) -0.0086(11) -0.0062(11) C3 0.0403(17) 0.0258(15) 0.0287(17) -0.0017(14) -0.0172(14) -0.0066(13) C4 0.0412(18) 0.0240(14) 0.0375(19) -0.0115(15) -0.0217(15) 0.0022(13) C5 0.0291(15) 0.0303(15) 0.0348(18) -0.0153(14) -0.0159(13) 0.0039(12) C6 0.0251(14) 0.0255(14) 0.0231(15) -0.0089(13) -0.0110(12) -0.0003(11) C7 0.052(2) 0.061(2) 0.0293(18) -0.0225(18) -0.0061(15) -0.0132(17) C8 0.0208(14) 0.0389(16) 0.0228(16) -0.0162(14) -0.0072(12) -0.0014(12) C9 0.0262(16) 0.0365(17) 0.0195(17) -0.0060(15) -0.0011(12) -0.0046(13) C10 0.0246(15) 0.0326(15) 0.0166(14) -0.0043(13) -0.0015(11) -0.0096(12) C11 0.0331(16) 0.0283(14) 0.0202(15) -0.0027(13) -0.0070(12) -0.0096(12) C12 0.0365(17) 0.0257(15) 0.0156(15) 0.0037(13) -0.0098(12) -0.0051(12) C13 0.0308(15) 0.0193(13) 0.0254(16) -0.0065(13) -0.0141(13) -0.0008(11) C14 0.0219(14) 0.0235(14) 0.0202(15) -0.0087(13) -0.0067(12) -0.0040(11) C15 0.0254(14) 0.0246(14) 0.0220(15) -0.0083(13) -0.0128(12) 0.0000(11) C16 0.0338(16) 0.0296(15) 0.0347(17) -0.0175(14) -0.0151(13) 0.0053(13) C17 0.0363(17) 0.0419(18) 0.0371(19) -0.0253(16) -0.0048(14) 0.0009(14) C18 0.051(2) 0.0432(18) 0.0219(16) -0.0192(15) 0.0011(14) -0.0088(15) C19 0.0356(17) 0.0278(16) 0.0250(16) -0.0129(14) -0.0063(13) -0.0081(12) O4' 0.044(9) 0.018(6) 0.020(5) -0.011(4) -0.011(6) 0.007(6) C20' 0.048(7) 0.046(6) 0.019(5) -0.004(5) -0.008(5) -0.005(5) O4 0.059(6) 0.019(4) 0.018(3) -0.007(2) -0.011(4) 0.002(4) C20 0.077(5) 0.032(3) 0.029(3) -0.012(3) -0.032(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.2237(17) . ? Gd1 O3 2.3474(17) 2_556 ? Gd1 O3 2.3708(18) . ? Gd1 O5 2.4587(19) . ? Gd1 O6 2.5149(18) . ? Gd1 N1 2.537(2) . ? Gd1 N2 2.554(2) . ? Gd1 N3 2.564(2) . ? Gd1 N4 2.900(2) . ? Gd1 Gd1 3.8112(2) 2_556 ? N1 C8 1.280(4) . ? N1 C9 1.470(4) . ? N2 C11 1.470(3) . ? N2 C10 1.473(4) . ? N3 C13 1.278(4) . ? N3 C12 1.464(4) . ? N4 O7 1.209(3) . ? N4 O6 1.262(3) . ? N4 O5 1.278(3) . ? O1 C1 1.310(3) . ? O2 C2 1.378(4) . ? O2 C7 1.441(4) . ? O3 C14 1.345(3) . ? O3 Gd1 2.3474(17) 2_556 ? C1 C2 1.408(4) . ? C1 C6 1.430(4) . ? C2 C3 1.385(4) . ? C3 C4 1.394(4) . ? C4 C5 1.363(4) . ? C5 C6 1.407(4) . ? C6 C8 1.444(4) . ? C9 C10 1.511(4) . ? C11 C12 1.513(4) . ? C13 C15 1.456(4) . ? C14 C19 1.405(4) . ? C14 C15 1.418(4) . ? C15 C16 1.398(4) . ? C16 C17 1.379(5) . ? C17 C18 1.385(5) . ? C18 C19 1.379(4) . ? C19 O4 1.444(12) . ? C19 O4' 1.27(3) . ? O4' C20' 1.433(16) . ? O4 C20 1.403(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O3 98.87(6) . 2_556 ? O1 Gd1 O3 90.62(7) . . ? O3 Gd1 O3 72.25(7) 2_556 . ? O1 Gd1 O5 94.53(7) . . ? O3 Gd1 O5 157.32(7) 2_556 . ? O3 Gd1 O5 126.03(6) . . ? O1 Gd1 O6 77.51(7) . . ? O3 Gd1 O6 149.69(7) 2_556 . ? O3 Gd1 O6 77.68(6) . . ? O5 Gd1 O6 51.57(7) . . ? O1 Gd1 N1 72.24(7) . . ? O3 Gd1 N1 82.69(6) 2_556 . ? O3 Gd1 N1 147.12(6) . . ? O5 Gd1 N1 84.11(7) . . ? O6 Gd1 N1 123.22(7) . . ? O1 Gd1 N2 137.58(7) . . ? O3 Gd1 N2 84.34(6) 2_556 . ? O3 Gd1 N2 129.68(7) . . ? O5 Gd1 N2 73.46(7) . . ? O6 Gd1 N2 118.83(6) . . ? N1 Gd1 N2 66.22(7) . . ? O1 Gd1 N3 155.08(7) . . ? O3 Gd1 N3 90.02(6) 2_556 . ? O3 Gd1 N3 69.88(7) . . ? O5 Gd1 N3 85.34(7) . . ? O6 Gd1 N3 83.09(7) . . ? N1 Gd1 N3 132.30(7) . . ? N2 Gd1 N3 66.16(7) . . ? O1 Gd1 N4 84.01(7) . . ? O3 Gd1 N4 173.91(6) 2_556 . ? O3 Gd1 N4 102.45(6) . . ? O5 Gd1 N4 25.96(8) . . ? O6 Gd1 N4 25.71(7) . . ? N1 Gd1 N4 103.34(7) . . ? N2 Gd1 N4 97.18(7) . . ? N3 Gd1 N4 85.24(7) . . ? O1 Gd1 Gd1 95.84(5) . 2_556 ? O3 Gd1 Gd1 36.33(4) 2_556 2_556 ? O3 Gd1 Gd1 35.92(4) . 2_556 ? O5 Gd1 Gd1 159.10(5) . 2_556 ? O6 Gd1 Gd1 113.52(5) . 2_556 ? N1 Gd1 Gd1 116.36(5) . 2_556 ? N2 Gd1 Gd1 109.66(5) . 2_556 ? N3 Gd1 Gd1 77.66(5) . 2_556 ? N4 Gd1 Gd1 138.30(5) . 2_556 ? C8 N1 C9 114.6(2) . . ? C8 N1 Gd1 126.05(19) . . ? C9 N1 Gd1 118.04(17) . . ? C11 N2 C10 113.1(2) . . ? C11 N2 Gd1 112.68(16) . . ? C10 N2 Gd1 110.70(16) . . ? C13 N3 C12 117.5(2) . . ? C13 N3 Gd1 126.09(19) . . ? C12 N3 Gd1 116.38(16) . . ? O7 N4 O6 122.3(3) . . ? O7 N4 O5 120.8(3) . . ? O6 N4 O5 116.9(2) . . ? O7 N4 Gd1 173.7(2) . . ? O6 N4 Gd1 59.85(12) . . ? O5 N4 Gd1 57.37(12) . . ? C1 O1 Gd1 137.70(17) . . ? C2 O2 C7 112.3(2) . . ? C14 O3 Gd1 128.04(16) . 2_556 ? C14 O3 Gd1 119.12(15) . . ? Gd1 O3 Gd1 107.75(7) 2_556 . ? N4 O5 Gd1 96.67(16) . . ? N4 O6 Gd1 94.44(15) . . ? O1 C1 C2 120.9(3) . . ? O1 C1 C6 121.9(3) . . ? C2 C1 C6 117.2(2) . . ? O2 C2 C3 118.1(3) . . ? O2 C2 C1 120.8(2) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 120.9(3) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 121.2(3) . . ? C5 C6 C1 119.9(3) . . ? C5 C6 C8 117.3(3) . . ? C1 C6 C8 122.9(2) . . ? N1 C8 C6 127.8(2) . . ? N1 C9 C10 110.7(2) . . ? N2 C10 C9 109.4(2) . . ? N2 C11 C12 108.4(2) . . ? N3 C12 C11 109.2(2) . . ? N3 C13 C15 124.6(2) . . ? O3 C14 C19 120.7(2) . . ? O3 C14 C15 121.7(3) . . ? C19 C14 C15 117.6(2) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 C13 117.4(2) . . ? C14 C15 C13 122.5(2) . . ? C17 C16 C15 120.7(3) . . ? C18 C17 C16 119.5(3) . . ? C17 C18 C19 120.8(3) . . ? O4 C19 O4' 17.0(11) . . ? O4 C19 C18 125.9(5) . . ? O4' C19 C18 112.7(8) . . ? O4 C19 C14 113.1(5) . . ? O4' C19 C14 125.4(8) . . ? C18 C19 C14 121.0(3) . . ? C20' O4' C19 108.0(18) . . ? C19 O4 C20 117.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Gd1 N1 C8 26.9(2) . . . . ? O3 Gd1 N1 C8 -74.9(2) 2_556 . . . ? O3 Gd1 N1 C8 -34.8(3) . . . . ? O5 Gd1 N1 C8 123.6(2) . . . . ? O6 Gd1 N1 C8 88.1(2) . . . . ? N2 Gd1 N1 C8 -161.9(2) . . . . ? N3 Gd1 N1 C8 -158.2(2) . . . . ? N4 Gd1 N1 C8 106.1(2) . . . . ? Gd1 Gd1 N1 C8 -60.8(2) 2_556 . . . ? O1 Gd1 N1 C9 -166.7(2) . . . . ? O3 Gd1 N1 C9 91.5(2) 2_556 . . . ? O3 Gd1 N1 C9 131.7(2) . . . . ? O5 Gd1 N1 C9 -70.0(2) . . . . ? O6 Gd1 N1 C9 -105.4(2) . . . . ? N2 Gd1 N1 C9 4.53(19) . . . . ? N3 Gd1 N1 C9 8.2(2) . . . . ? N4 Gd1 N1 C9 -87.5(2) . . . . ? Gd1 Gd1 N1 C9 105.6(2) 2_556 . . . ? O1 Gd1 N2 C11 -146.21(16) . . . . ? O3 Gd1 N2 C11 116.82(17) 2_556 . . . ? O3 Gd1 N2 C11 55.53(18) . . . . ? O5 Gd1 N2 C11 -67.91(17) . . . . ? O6 Gd1 N2 C11 -42.54(19) . . . . ? N1 Gd1 N2 C11 -158.70(18) . . . . ? N3 Gd1 N2 C11 24.30(16) . . . . ? N4 Gd1 N2 C11 -57.24(17) . . . . ? Gd1 Gd1 N2 C11 90.34(16) 2_556 . . . ? O1 Gd1 N2 C10 -18.5(2) . . . . ? O3 Gd1 N2 C10 -115.47(16) 2_556 . . . ? O3 Gd1 N2 C10 -176.76(14) . . . . ? O5 Gd1 N2 C10 59.81(16) . . . . ? O6 Gd1 N2 C10 85.18(16) . . . . ? N1 Gd1 N2 C10 -30.98(15) . . . . ? N3 Gd1 N2 C10 152.01(17) . . . . ? N4 Gd1 N2 C10 70.47(16) . . . . ? Gd1 Gd1 N2 C10 -141.95(15) 2_556 . . . ? O1 Gd1 N3 C13 -6.6(3) . . . . ? O3 Gd1 N3 C13 104.9(2) 2_556 . . . ? O3 Gd1 N3 C13 33.9(2) . . . . ? O5 Gd1 N3 C13 -97.3(2) . . . . ? O6 Gd1 N3 C13 -45.5(2) . . . . ? N1 Gd1 N3 C13 -175.0(2) . . . . ? N2 Gd1 N3 C13 -171.3(2) . . . . ? N4 Gd1 N3 C13 -71.2(2) . . . . ? Gd1 Gd1 N3 C13 70.5(2) 2_556 . . . ? O1 Gd1 N3 C12 171.34(18) . . . . ? O3 Gd1 N3 C12 -77.16(18) 2_556 . . . ? O3 Gd1 N3 C12 -148.21(19) . . . . ? O5 Gd1 N3 C12 80.61(18) . . . . ? O6 Gd1 N3 C12 132.42(19) . . . . ? N1 Gd1 N3 C12 2.9(2) . . . . ? N2 Gd1 N3 C12 6.64(17) . . . . ? N4 Gd1 N3 C12 106.66(19) . . . . ? Gd1 Gd1 N3 C12 -111.60(18) 2_556 . . . ? O1 Gd1 N4 O7 38(2) . . . . ? O3 Gd1 N4 O7 156.7(19) 2_556 . . . ? O3 Gd1 N4 O7 127(2) . . . . ? O5 Gd1 N4 O7 -75(2) . . . . ? O6 Gd1 N4 O7 112(2) . . . . ? N1 Gd1 N4 O7 -32(2) . . . . ? N2 Gd1 N4 O7 -99(2) . . . . ? N3 Gd1 N4 O7 -164(2) . . . . ? Gd1 Gd1 N4 O7 130(2) 2_556 . . . ? O1 Gd1 N4 O6 -73.53(16) . . . . ? O3 Gd1 N4 O6 45.0(7) 2_556 . . . ? O3 Gd1 N4 O6 15.78(17) . . . . ? O5 Gd1 N4 O6 173.1(3) . . . . ? N1 Gd1 N4 O6 -143.65(16) . . . . ? N2 Gd1 N4 O6 149.17(16) . . . . ? N3 Gd1 N4 O6 83.95(17) . . . . ? Gd1 Gd1 N4 O6 18.5(2) 2_556 . . . ? O1 Gd1 N4 O5 113.39(16) . . . . ? O3 Gd1 N4 O5 -128.1(6) 2_556 . . . ? O3 Gd1 N4 O5 -157.30(15) . . . . ? O6 Gd1 N4 O5 -173.1(3) . . . . ? N1 Gd1 N4 O5 43.28(17) . . . . ? N2 Gd1 N4 O5 -23.91(16) . . . . ? N3 Gd1 N4 O5 -89.12(16) . . . . ? Gd1 Gd1 N4 O5 -154.55(13) 2_556 . . . ? O3 Gd1 O1 C1 41.4(3) 2_556 . . . ? O3 Gd1 O1 C1 113.6(3) . . . . ? O5 Gd1 O1 C1 -120.2(3) . . . . ? O6 Gd1 O1 C1 -169.2(3) . . . . ? N1 Gd1 O1 C1 -37.9(3) . . . . ? N2 Gd1 O1 C1 -49.9(3) . . . . ? N3 Gd1 O1 C1 151.1(3) . . . . ? N4 Gd1 O1 C1 -144.0(3) . . . . ? Gd1 Gd1 O1 C1 78.0(3) 2_556 . . . ? O1 Gd1 O3 C14 104.10(18) . . . . ? O3 Gd1 O3 C14 -156.8(2) 2_556 . . . ? O5 Gd1 O3 C14 8.0(2) . . . . ? O6 Gd1 O3 C14 27.03(18) . . . . ? N1 Gd1 O3 C14 161.06(17) . . . . ? N2 Gd1 O3 C14 -90.37(19) . . . . ? N3 Gd1 O3 C14 -60.04(18) . . . . ? N4 Gd1 O3 C14 20.09(19) . . . . ? Gd1 Gd1 O3 C14 -156.8(2) 2_556 . . . ? O1 Gd1 O3 Gd1 -99.11(7) . . . 2_556 ? O3 Gd1 O3 Gd1 0.0 2_556 . . 2_556 ? O5 Gd1 O3 Gd1 164.82(7) . . . 2_556 ? O6 Gd1 O3 Gd1 -176.18(8) . . . 2_556 ? N1 Gd1 O3 Gd1 -42.15(15) . . . 2_556 ? N2 Gd1 O3 Gd1 66.42(9) . . . 2_556 ? N3 Gd1 O3 Gd1 96.75(8) . . . 2_556 ? N4 Gd1 O3 Gd1 176.88(6) . . . 2_556 ? O7 N4 O5 Gd1 172.9(2) . . . . ? O6 N4 O5 Gd1 -6.7(3) . . . . ? O1 Gd1 O5 N4 -66.30(16) . . . . ? O3 Gd1 O5 N4 167.48(14) 2_556 . . . ? O3 Gd1 O5 N4 27.78(18) . . . . ? O6 Gd1 O5 N4 3.83(15) . . . . ? N1 Gd1 O5 N4 -137.89(16) . . . . ? N2 Gd1 O5 N4 155.20(17) . . . . ? N3 Gd1 O5 N4 88.70(16) . . . . ? Gd1 Gd1 O5 N4 53.3(2) 2_556 . . . ? O7 N4 O6 Gd1 -173.1(3) . . . . ? O5 N4 O6 Gd1 6.5(2) . . . . ? O1 Gd1 O6 N4 102.34(17) . . . . ? O3 Gd1 O6 N4 -171.45(13) 2_556 . . . ? O3 Gd1 O6 N4 -164.23(17) . . . . ? O5 Gd1 O6 N4 -3.86(15) . . . . ? N1 Gd1 O6 N4 43.59(19) . . . . ? N2 Gd1 O6 N4 -35.48(18) . . . . ? N3 Gd1 O6 N4 -93.38(17) . . . . ? Gd1 Gd1 O6 N4 -166.67(14) 2_556 . . . ? Gd1 O1 C1 C2 -149.3(2) . . . . ? Gd1 O1 C1 C6 30.4(4) . . . . ? C7 O2 C2 C3 117.5(3) . . . . ? C7 O2 C2 C1 -67.4(3) . . . . ? O1 C1 C2 O2 -2.9(4) . . . . ? C6 C1 C2 O2 177.3(2) . . . . ? O1 C1 C2 C3 172.1(3) . . . . ? C6 C1 C2 C3 -7.7(4) . . . . ? O2 C2 C3 C4 -179.7(3) . . . . ? C1 C2 C3 C4 5.1(4) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 -3.3(4) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C4 C5 C6 C8 179.8(3) . . . . ? O1 C1 C6 C5 -174.8(2) . . . . ? C2 C1 C6 C5 4.9(4) . . . . ? O1 C1 C6 C8 5.9(4) . . . . ? C2 C1 C6 C8 -174.3(2) . . . . ? C9 N1 C8 C6 179.4(3) . . . . ? Gd1 N1 C8 C6 -13.8(4) . . . . ? C5 C6 C8 N1 170.6(3) . . . . ? C1 C6 C8 N1 -10.1(4) . . . . ? C8 N1 C9 C10 -170.3(2) . . . . ? Gd1 N1 C9 C10 21.7(3) . . . . ? C11 N2 C10 C9 -177.7(2) . . . . ? Gd1 N2 C10 C9 54.8(2) . . . . ? N1 C9 C10 N2 -50.3(3) . . . . ? C10 N2 C11 C12 -178.5(2) . . . . ? Gd1 N2 C11 C12 -52.0(2) . . . . ? C13 N3 C12 C11 142.7(2) . . . . ? Gd1 N3 C12 C11 -35.4(3) . . . . ? N2 C11 C12 N3 57.1(3) . . . . ? C12 N3 C13 C15 179.8(2) . . . . ? Gd1 N3 C13 C15 -2.3(4) . . . . ? Gd1 O3 C14 C19 90.2(3) 2_556 . . . ? Gd1 O3 C14 C19 -118.3(2) . . . . ? Gd1 O3 C14 C15 -90.5(3) 2_556 . . . ? Gd1 O3 C14 C15 61.0(3) . . . . ? O3 C14 C15 C16 175.7(2) . . . . ? C19 C14 C15 C16 -5.0(4) . . . . ? O3 C14 C15 C13 -4.3(4) . . . . ? C19 C14 C15 C13 175.0(3) . . . . ? N3 C13 C15 C16 153.8(3) . . . . ? N3 C13 C15 C14 -26.2(4) . . . . ? C14 C15 C16 C17 3.7(4) . . . . ? C13 C15 C16 C17 -176.4(3) . . . . ? C15 C16 C17 C18 -0.7(5) . . . . ? C16 C17 C18 C19 -0.9(5) . . . . ? C17 C18 C19 O4 177.0(7) . . . . ? C17 C18 C19 O4' -170.5(10) . . . . ? C17 C18 C19 C14 -0.7(5) . . . . ? O3 C14 C19 O4 4.9(7) . . . . ? C15 C14 C19 O4 -174.4(6) . . . . ? O3 C14 C19 O4' -8.6(11) . . . . ? C15 C14 C19 O4' 172.1(11) . . . . ? O3 C14 C19 C18 -177.1(3) . . . . ? C15 C14 C19 C18 3.6(4) . . . . ? O4 C19 O4' C20' 45(4) . . . . ? C18 C19 O4' C20' -98.5(11) . . . . ? C14 C19 O4' C20' 92.1(14) . . . . ? O4' C19 O4 C20 -73(4) . . . . ? C18 C19 O4 C20 -29.7(13) . . . . ? C14 C19 O4 C20 148.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.208 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.099 data_mm002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Ho2 N8 O14' _chemical_formula_weight 1192.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ho' 'Ho' -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5330(7) _cell_length_b 10.5394(9) _cell_length_c 11.5002(9) _cell_angle_alpha 66.484(4) _cell_angle_beta 65.036(4) _cell_angle_gamma 79.837(4) _cell_volume 1061.21(14) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4262 _cell_measurement_theta_min 4.68 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 3.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3514 _exptl_absorpt_correction_T_max 0.5187 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5037 _diffrn_reflns_av_R_equivalents 0.0096 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4449 _reflns_number_gt 4323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.4814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4449 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.414586(9) 0.854412(10) 0.505068(10) 0.01560(5) Uani 1 1 d . . . N1 N 0.2023(2) 0.9866(2) 0.6104(2) 0.0217(4) Uani 1 1 d . . . N2 N 0.2616(2) 0.7142(2) 0.7495(2) 0.0227(4) Uani 1 1 d . . . H2A H 0.2954 0.7276 0.8065 0.027 Uiso 1 1 calc R . . N3 N 0.5111(2) 0.6173(2) 0.5959(2) 0.0219(4) Uani 1 1 d . . . N4 N 0.2530(2) 0.8129(3) 0.3744(2) 0.0253(5) Uani 1 1 d . . . O1 O 0.46255(17) 1.09025(18) 0.39631(18) 0.0179(3) Uani 1 1 d . . . O2 O 0.57804(19) 1.2204(2) 0.1218(2) 0.0289(4) Uani 1 1 d . . . O3 O 0.59012(19) 0.8213(2) 0.33051(19) 0.0255(4) Uani 1 1 d . . . O4 O 0.8043(2) 0.9242(2) 0.0697(2) 0.0312(4) Uani 1 1 d . . . O5 O 0.3153(2) 0.9255(2) 0.3256(2) 0.0308(4) Uani 1 1 d . . . O6 O 0.2542(2) 0.7276(2) 0.4912(2) 0.0311(4) Uani 1 1 d . . . O7 O 0.1944(3) 0.7837(3) 0.3173(3) 0.0460(6) Uani 1 1 d . . . C1 C 0.3808(2) 1.1736(2) 0.3313(3) 0.0166(4) Uani 1 1 d . . . C2 C 0.4387(3) 1.2452(3) 0.1877(3) 0.0218(5) Uani 1 1 d . . . C3 C 0.3567(3) 1.3358(3) 0.1208(3) 0.0285(6) Uani 1 1 d . . . H3A H 0.3972 1.3839 0.0240 0.034 Uiso 1 1 calc R . . C4 C 0.2157(3) 1.3569(3) 0.1940(3) 0.0301(6) Uani 1 1 d . . . H4A H 0.1610 1.4208 0.1478 0.036 Uiso 1 1 calc R . . C5 C 0.1560(3) 1.2844(3) 0.3340(3) 0.0269(6) Uani 1 1 d . . . H5A H 0.0600 1.2989 0.3844 0.032 Uiso 1 1 calc R . . C6 C 0.2361(2) 1.1896(3) 0.4024(3) 0.0201(5) Uani 1 1 d . . . C7 C 0.6314(3) 1.2542(4) -0.0226(3) 0.0369(7) Uani 1 1 d . . . H7A H 0.7315 1.2314 -0.0561 0.055 Uiso 1 1 calc R . . H7B H 0.6178 1.3534 -0.0679 0.055 Uiso 1 1 calc R . . H7C H 0.5816 1.2012 -0.0435 0.055 Uiso 1 1 calc R . . C8 C 0.1624(3) 1.1066(3) 0.5479(3) 0.0231(5) Uani 1 1 d . . . H8A H 0.0794 1.1444 0.5994 0.028 Uiso 1 1 calc R . . C9 C 0.1152(3) 0.9175(3) 0.7567(3) 0.0284(6) Uani 1 1 d . . . H9A H 0.0183 0.9547 0.7774 0.034 Uiso 1 1 calc R . . H9B H 0.1530 0.9345 0.8147 0.034 Uiso 1 1 calc R . . C10 C 0.1154(3) 0.7634(3) 0.7877(3) 0.0252(5) Uani 1 1 d . . . H10A H 0.0609 0.7140 0.8868 0.030 Uiso 1 1 calc R . . H10B H 0.0721 0.7457 0.7341 0.030 Uiso 1 1 calc R . . C11 C 0.2743(3) 0.5648(3) 0.7746(3) 0.0260(5) Uani 1 1 d . . . H11A H 0.2357 0.5443 0.7191 0.031 Uiso 1 1 calc R . . H11B H 0.2210 0.5115 0.8731 0.031 Uiso 1 1 calc R . . C12 C 0.4272(3) 0.5244(3) 0.7350(3) 0.0290(6) Uani 1 1 d . . . H12A H 0.4606 0.5289 0.8019 0.035 Uiso 1 1 calc R . . H12B H 0.4391 0.4280 0.7380 0.035 Uiso 1 1 calc R . . C13 C 0.6359(3) 0.5748(3) 0.5427(3) 0.0242(5) Uani 1 1 d . . . H13A H 0.6614 0.4879 0.5973 0.029 Uiso 1 1 calc R . . C14 C 0.7132(3) 0.7618(3) 0.3071(3) 0.0218(5) Uani 1 1 d . . . C15 C 0.7428(3) 0.6435(3) 0.4091(3) 0.0227(5) Uani 1 1 d . . . C16 C 0.8802(3) 0.5896(3) 0.3824(3) 0.0280(6) Uani 1 1 d . . . H16A H 0.8983 0.5108 0.4514 0.034 Uiso 1 1 calc R . . C17 C 0.9882(3) 0.6484(3) 0.2591(3) 0.0318(6) Uani 1 1 d . . . H17A H 1.0812 0.6139 0.2442 0.038 Uiso 1 1 calc R . . C18 C 0.9597(3) 0.7603(3) 0.1552(3) 0.0309(6) Uani 1 1 d . . . H18A H 1.0339 0.8007 0.0689 0.037 Uiso 1 1 calc R . . C19 C 0.8248(3) 0.8131(3) 0.1764(3) 0.0248(5) Uani 1 1 d . . . C20 C 0.7054(4) 0.8995(4) 0.0259(4) 0.0460(8) Uani 1 1 d . . . H20A H 0.6968 0.9822 -0.0498 0.069 Uiso 1 1 calc R . . H20B H 0.6141 0.8779 0.1031 0.069 Uiso 1 1 calc R . . H20C H 0.7378 0.8212 -0.0055 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01591(6) 0.01708(7) 0.01282(7) -0.00377(5) -0.00555(4) -0.00202(4) N1 0.0191(9) 0.0253(11) 0.0179(11) -0.0078(10) -0.0043(8) -0.0017(8) N2 0.0248(10) 0.0252(11) 0.0180(11) -0.0063(10) -0.0073(8) -0.0061(8) N3 0.0269(10) 0.0176(11) 0.0185(11) -0.0014(10) -0.0094(8) -0.0051(8) N4 0.0246(10) 0.0327(13) 0.0238(12) -0.0123(11) -0.0123(9) -0.0002(9) O1 0.0196(8) 0.0185(8) 0.0137(9) -0.0003(7) -0.0090(6) -0.0026(6) O2 0.0220(9) 0.0440(12) 0.0176(10) -0.0079(9) -0.0073(7) -0.0022(8) O3 0.0255(9) 0.0280(10) 0.0183(10) -0.0081(8) -0.0068(7) 0.0055(7) O4 0.0328(10) 0.0353(12) 0.0210(10) -0.0065(9) -0.0082(8) -0.0045(8) O5 0.0411(11) 0.0241(10) 0.0289(11) -0.0021(9) -0.0198(9) -0.0070(8) O6 0.0384(11) 0.0314(11) 0.0252(11) -0.0041(9) -0.0155(8) -0.0113(8) O7 0.0542(14) 0.0605(16) 0.0401(14) -0.0176(13) -0.0289(11) -0.0146(12) C1 0.0181(10) 0.0158(11) 0.0159(12) -0.0031(10) -0.0087(9) -0.0010(8) C2 0.0227(11) 0.0234(13) 0.0190(13) -0.0051(11) -0.0095(9) -0.0022(9) C3 0.0343(14) 0.0287(14) 0.0196(14) -0.0006(12) -0.0150(11) -0.0016(11) C4 0.0338(14) 0.0300(15) 0.0297(16) -0.0068(13) -0.0214(12) 0.0056(11) C5 0.0245(12) 0.0297(14) 0.0311(15) -0.0134(13) -0.0160(11) 0.0078(10) C6 0.0189(11) 0.0223(12) 0.0206(13) -0.0087(11) -0.0087(9) 0.0009(9) C7 0.0310(14) 0.052(2) 0.0228(15) -0.0125(15) -0.0075(11) -0.0005(13) C8 0.0183(11) 0.0298(14) 0.0243(14) -0.0149(12) -0.0072(9) 0.0020(9) C9 0.0277(13) 0.0312(15) 0.0158(13) -0.0073(12) 0.0010(10) -0.0037(10) C10 0.0224(12) 0.0301(14) 0.0169(13) -0.0066(12) -0.0013(9) -0.0069(10) C11 0.0311(13) 0.0199(13) 0.0196(14) 0.0001(12) -0.0066(10) -0.0088(10) C12 0.0367(15) 0.0213(14) 0.0195(15) 0.0009(12) -0.0082(11) -0.0050(11) C13 0.0334(13) 0.0183(12) 0.0234(14) -0.0068(12) -0.0145(11) 0.0006(10) C14 0.0234(12) 0.0239(13) 0.0209(14) -0.0117(12) -0.0079(10) 0.0002(10) C15 0.0236(12) 0.0217(13) 0.0252(14) -0.0113(12) -0.0100(10) 0.0021(9) C16 0.0276(13) 0.0269(14) 0.0349(16) -0.0160(13) -0.0148(11) 0.0051(10) C17 0.0255(13) 0.0370(16) 0.0393(17) -0.0224(15) -0.0120(11) 0.0036(11) C18 0.0248(13) 0.0402(17) 0.0283(15) -0.0186(14) -0.0037(10) -0.0037(11) C19 0.0283(13) 0.0265(14) 0.0200(14) -0.0100(12) -0.0067(10) -0.0041(10) C20 0.055(2) 0.056(2) 0.0318(19) -0.0073(17) -0.0249(15) -0.0100(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O3 2.1837(18) . ? Ho1 O1 2.3096(16) 2_676 ? Ho1 O1 2.3295(18) . ? Ho1 O6 2.4212(19) . ? Ho1 O5 2.4953(19) . ? Ho1 N3 2.507(2) . ? Ho1 N1 2.523(2) . ? Ho1 N2 2.526(2) . ? Ho1 N4 2.879(2) . ? Ho1 Ho1 3.7623(3) 2_676 ? N1 C8 1.279(3) . ? N1 C9 1.469(3) . ? N2 C11 1.475(3) . ? N2 C10 1.471(3) . ? N3 C13 1.279(3) . ? N3 C12 1.469(4) . ? N4 O5 1.259(3) . ? N4 O7 1.216(3) . ? N4 O6 1.287(3) . ? O1 C1 1.351(3) . ? O1 Ho1 2.3096(16) 2_676 ? O2 C2 1.372(3) . ? O2 C7 1.418(3) . ? O3 C14 1.303(3) . ? O4 C19 1.383(4) . ? O4 C20 1.431(4) . ? C1 C6 1.409(3) . ? C1 C2 1.409(4) . ? C2 C3 1.391(3) . ? C3 C4 1.393(4) . ? C4 C5 1.381(4) . ? C5 C6 1.402(3) . ? C6 C8 1.464(4) . ? C9 C10 1.518(4) . ? C11 C12 1.509(4) . ? C13 C15 1.447(4) . ? C14 C19 1.421(4) . ? C14 C15 1.425(4) . ? C15 C16 1.409(4) . ? C16 C17 1.369(4) . ? C17 C18 1.400(4) . ? C18 C19 1.387(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ho1 O1 99.28(7) . 2_676 ? O3 Ho1 O1 88.46(7) . . ? O1 Ho1 O1 71.62(7) 2_676 . ? O3 Ho1 O6 92.92(7) . . ? O1 Ho1 O6 157.45(7) 2_676 . ? O1 Ho1 O6 127.97(6) . . ? O3 Ho1 O5 77.07(7) . . ? O1 Ho1 O5 149.46(6) 2_676 . ? O1 Ho1 O5 77.95(6) . . ? O6 Ho1 O5 52.06(7) . . ? O3 Ho1 N3 73.16(7) . . ? O1 Ho1 N3 82.59(6) 2_676 . ? O1 Ho1 N3 145.48(6) . . ? O6 Ho1 N3 82.91(7) . . ? O5 Ho1 N3 123.71(7) . . ? O3 Ho1 N1 152.87(7) . . ? O1 Ho1 N1 91.14(6) 2_676 . ? O1 Ho1 N1 71.08(7) . . ? O6 Ho1 N1 86.37(7) . . ? O5 Ho1 N1 81.26(7) . . ? N3 Ho1 N1 133.38(7) . . ? O3 Ho1 N2 138.60(7) . . ? O1 Ho1 N2 85.21(6) 2_676 . ? O1 Ho1 N2 131.06(6) . . ? O6 Ho1 N2 73.20(7) . . ? O5 Ho1 N2 117.83(7) . . ? N3 Ho1 N2 66.62(7) . . ? N1 Ho1 N2 66.83(7) . . ? O3 Ho1 N4 82.57(7) . . ? O1 Ho1 N4 174.49(6) 2_676 . ? O1 Ho1 N4 103.34(6) . . ? O6 Ho1 N4 26.34(7) . . ? O5 Ho1 N4 25.85(7) . . ? N3 Ho1 N4 102.92(7) . . ? N1 Ho1 N4 85.01(7) . . ? N2 Ho1 N4 96.85(7) . . ? O3 Ho1 Ho1 94.73(5) . 2_676 ? O1 Ho1 Ho1 35.99(4) 2_676 2_676 ? O1 Ho1 Ho1 35.63(4) . 2_676 ? O6 Ho1 Ho1 161.42(5) . 2_676 ? O5 Ho1 Ho1 113.54(5) . 2_676 ? N3 Ho1 Ho1 115.53(5) . 2_676 ? N1 Ho1 Ho1 79.13(5) . 2_676 ? N2 Ho1 Ho1 110.82(5) . 2_676 ? N4 Ho1 Ho1 138.93(5) . 2_676 ? C8 N1 C9 117.1(2) . . ? C8 N1 Ho1 126.19(17) . . ? C9 N1 Ho1 116.68(16) . . ? C11 N2 C10 112.6(2) . . ? C11 N2 Ho1 111.45(15) . . ? C10 N2 Ho1 112.16(16) . . ? C13 N3 C12 114.9(2) . . ? C13 N3 Ho1 126.26(19) . . ? C12 N3 Ho1 117.95(16) . . ? O5 N4 O7 123.4(2) . . ? O5 N4 O6 115.9(2) . . ? O7 N4 O6 120.7(2) . . ? O5 N4 Ho1 59.79(12) . . ? O7 N4 Ho1 173.1(2) . . ? O6 N4 Ho1 56.56(11) . . ? C1 O1 Ho1 128.32(14) . 2_676 ? C1 O1 Ho1 118.48(14) . . ? Ho1 O1 Ho1 108.38(7) 2_676 . ? C2 O2 C7 118.0(2) . . ? C14 O3 Ho1 137.63(17) . . ? C19 O4 C20 114.1(2) . . ? N4 O5 Ho1 94.36(15) . . ? N4 O6 Ho1 97.10(14) . . ? O1 C1 C6 121.9(2) . . ? O1 C1 C2 120.1(2) . . ? C6 C1 C2 117.9(2) . . ? O2 C2 C3 123.6(2) . . ? O2 C2 C1 115.9(2) . . ? C3 C2 C1 120.5(2) . . ? C4 C3 C2 120.8(3) . . ? C5 C4 C3 119.6(2) . . ? C4 C5 C6 120.4(2) . . ? C1 C6 C5 120.6(2) . . ? C1 C6 C8 122.2(2) . . ? C5 C6 C8 117.2(2) . . ? N1 C8 C6 124.4(2) . . ? N1 C9 C10 108.6(2) . . ? N2 C10 C9 108.0(2) . . ? N2 C11 C12 108.4(2) . . ? N3 C12 C11 110.7(2) . . ? N3 C13 C15 127.6(2) . . ? O3 C14 C19 120.7(2) . . ? O3 C14 C15 122.5(2) . . ? C19 C14 C15 116.8(2) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 C13 117.4(2) . . ? C14 C15 C13 122.3(2) . . ? C17 C16 C15 121.4(3) . . ? C16 C17 C18 119.0(3) . . ? C19 C18 C17 121.0(3) . . ? O4 C19 C18 118.0(3) . . ? O4 C19 C14 120.8(2) . . ? C18 C19 C14 121.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ho1 N1 C8 -10.3(3) . . . . ? O1 Ho1 N1 C8 102.8(2) 2_676 . . . ? O1 Ho1 N1 C8 32.7(2) . . . . ? O6 Ho1 N1 C8 -99.6(2) . . . . ? O5 Ho1 N1 C8 -47.5(2) . . . . ? N3 Ho1 N1 C8 -176.31(18) . . . . ? N2 Ho1 N1 C8 -172.9(2) . . . . ? N4 Ho1 N1 C8 -73.2(2) . . . . ? Ho1 Ho1 N1 C8 68.7(2) 2_676 . . . ? O3 Ho1 N1 C9 168.44(18) . . . . ? O1 Ho1 N1 C9 -78.44(18) 2_676 . . . ? O1 Ho1 N1 C9 -148.54(19) . . . . ? O6 Ho1 N1 C9 79.13(18) . . . . ? O5 Ho1 N1 C9 131.28(18) . . . . ? N3 Ho1 N1 C9 2.4(2) . . . . ? N2 Ho1 N1 C9 5.86(17) . . . . ? N4 Ho1 N1 C9 105.51(18) . . . . ? Ho1 Ho1 N1 C9 -112.55(18) 2_676 . . . ? O3 Ho1 N2 C11 -15.5(2) . . . . ? O1 Ho1 N2 C11 -114.12(16) 2_676 . . . ? O1 Ho1 N2 C11 -174.60(14) . . . . ? O6 Ho1 N2 C11 59.30(16) . . . . ? O5 Ho1 N2 C11 86.97(17) . . . . ? N3 Ho1 N2 C11 -30.13(16) . . . . ? N1 Ho1 N2 C11 152.58(18) . . . . ? N4 Ho1 N2 C11 71.01(17) . . . . ? Ho1 Ho1 N2 C11 -139.88(15) 2_676 . . . ? O3 Ho1 N2 C10 -142.77(15) . . . . ? O1 Ho1 N2 C10 118.62(16) 2_676 . . . ? O1 Ho1 N2 C10 58.14(18) . . . . ? O6 Ho1 N2 C10 -67.96(16) . . . . ? O5 Ho1 N2 C10 -40.29(18) . . . . ? N3 Ho1 N2 C10 -157.39(17) . . . . ? N1 Ho1 N2 C10 25.32(15) . . . . ? N4 Ho1 N2 C10 -56.24(16) . . . . ? Ho1 Ho1 N2 C10 92.86(15) 2_676 . . . ? O3 Ho1 N3 C13 24.4(2) . . . . ? O1 Ho1 N3 C13 -77.7(2) 2_676 . . . ? O1 Ho1 N3 C13 -36.3(3) . . . . ? O6 Ho1 N3 C13 119.6(2) . . . . ? O5 Ho1 N3 C13 85.5(2) . . . . ? N1 Ho1 N3 C13 -162.23(19) . . . . ? N2 Ho1 N3 C13 -165.7(2) . . . . ? N4 Ho1 N3 C13 102.4(2) . . . . ? Ho1 Ho1 N3 C13 -62.8(2) 2_676 . . . ? O3 Ho1 N3 C12 -167.1(2) . . . . ? O1 Ho1 N3 C12 90.79(19) 2_676 . . . ? O1 Ho1 N3 C12 132.17(18) . . . . ? O6 Ho1 N3 C12 -71.90(19) . . . . ? O5 Ho1 N3 C12 -106.02(19) . . . . ? N1 Ho1 N3 C12 6.3(2) . . . . ? N2 Ho1 N3 C12 2.82(17) . . . . ? N4 Ho1 N3 C12 -89.14(19) . . . . ? Ho1 Ho1 N3 C12 105.68(18) 2_676 . . . ? O3 Ho1 N4 O5 -75.61(16) . . . . ? O1 Ho1 N4 O5 34.4(7) 2_676 . . . ? O1 Ho1 N4 O5 11.02(16) . . . . ? O6 Ho1 N4 O5 172.1(2) . . . . ? N3 Ho1 N4 O5 -146.36(15) . . . . ? N1 Ho1 N4 O5 80.22(16) . . . . ? N2 Ho1 N4 O5 146.13(15) . . . . ? Ho1 Ho1 N4 O5 13.06(19) 2_676 . . . ? O3 Ho1 N4 O7 43.6(17) . . . . ? O1 Ho1 N4 O7 153.7(15) 2_676 . . . ? O1 Ho1 N4 O7 130.3(17) . . . . ? O6 Ho1 N4 O7 -68.6(17) . . . . ? O5 Ho1 N4 O7 119.3(18) . . . . ? N3 Ho1 N4 O7 -27.1(17) . . . . ? N1 Ho1 N4 O7 -160.5(17) . . . . ? N2 Ho1 N4 O7 -94.6(17) . . . . ? Ho1 Ho1 N4 O7 132.3(17) 2_676 . . . ? O3 Ho1 N4 O6 112.29(16) . . . . ? O1 Ho1 N4 O6 -137.7(6) 2_676 . . . ? O1 Ho1 N4 O6 -161.08(15) . . . . ? O5 Ho1 N4 O6 -172.1(2) . . . . ? N3 Ho1 N4 O6 41.53(16) . . . . ? N1 Ho1 N4 O6 -91.89(16) . . . . ? N2 Ho1 N4 O6 -25.98(16) . . . . ? Ho1 Ho1 N4 O6 -159.04(13) 2_676 . . . ? O3 Ho1 O1 C1 102.24(16) . . . . ? O1 Ho1 O1 C1 -157.45(19) 2_676 . . . ? O6 Ho1 O1 C1 9.74(19) . . . . ? O5 Ho1 O1 C1 25.14(16) . . . . ? N3 Ho1 O1 C1 158.85(15) . . . . ? N1 Ho1 O1 C1 -59.63(16) . . . . ? N2 Ho1 O1 C1 -91.41(17) . . . . ? N4 Ho1 O1 C1 20.25(17) . . . . ? Ho1 Ho1 O1 C1 -157.45(19) 2_676 . . . ? O3 Ho1 O1 Ho1 -100.31(8) . . . 2_676 ? O1 Ho1 O1 Ho1 0.0 2_676 . . 2_676 ? O6 Ho1 O1 Ho1 167.19(7) . . . 2_676 ? O5 Ho1 O1 Ho1 -177.41(8) . . . 2_676 ? N3 Ho1 O1 Ho1 -43.70(14) . . . 2_676 ? N1 Ho1 O1 Ho1 97.82(8) . . . 2_676 ? N2 Ho1 O1 Ho1 66.04(10) . . . 2_676 ? N4 Ho1 O1 Ho1 177.70(6) . . . 2_676 ? O1 Ho1 O3 C14 42.2(3) 2_676 . . . ? O1 Ho1 O3 C14 113.3(3) . . . . ? O6 Ho1 O3 C14 -118.7(3) . . . . ? O5 Ho1 O3 C14 -168.7(3) . . . . ? N3 Ho1 O3 C14 -37.0(2) . . . . ? N1 Ho1 O3 C14 153.5(2) . . . . ? N2 Ho1 O3 C14 -51.1(3) . . . . ? N4 Ho1 O3 C14 -143.0(3) . . . . ? Ho1 Ho1 O3 C14 78.2(3) 2_676 . . . ? O7 N4 O5 Ho1 -172.8(2) . . . . ? O6 N4 O5 Ho1 7.3(2) . . . . ? O3 Ho1 O5 N4 99.77(16) . . . . ? O1 Ho1 O5 N4 -173.88(13) 2_676 . . . ? O1 Ho1 O5 N4 -169.03(16) . . . . ? O6 Ho1 O5 N4 -4.43(14) . . . . ? N3 Ho1 O5 N4 40.47(18) . . . . ? N1 Ho1 O5 N4 -96.65(16) . . . . ? N2 Ho1 O5 N4 -38.74(17) . . . . ? Ho1 Ho1 O5 N4 -170.68(13) 2_676 . . . ? O5 N4 O6 Ho1 -7.6(2) . . . . ? O7 N4 O6 Ho1 172.5(2) . . . . ? O3 Ho1 O6 N4 -66.74(15) . . . . ? O1 Ho1 O6 N4 170.31(14) 2_676 . . . ? O1 Ho1 O6 N4 23.59(18) . . . . ? O5 Ho1 O6 N4 4.36(14) . . . . ? N3 Ho1 O6 N4 -139.37(16) . . . . ? N1 Ho1 O6 N4 86.09(15) . . . . ? N2 Ho1 O6 N4 152.98(17) . . . . ? Ho1 Ho1 O6 N4 47.5(3) 2_676 . . . ? Ho1 O1 C1 C6 -90.4(3) 2_676 . . . ? Ho1 O1 C1 C6 62.0(3) . . . . ? Ho1 O1 C1 C2 91.3(2) 2_676 . . . ? Ho1 O1 C1 C2 -116.4(2) . . . . ? C7 O2 C2 C3 -19.5(4) . . . . ? C7 O2 C2 C1 161.3(3) . . . . ? O1 C1 C2 O2 2.0(3) . . . . ? C6 C1 C2 O2 -176.4(2) . . . . ? O1 C1 C2 C3 -177.2(2) . . . . ? C6 C1 C2 C3 4.3(4) . . . . ? O2 C2 C3 C4 -179.7(3) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? C2 C3 C4 C5 -1.6(4) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? O1 C1 C6 C5 175.4(2) . . . . ? C2 C1 C6 C5 -6.2(3) . . . . ? O1 C1 C6 C8 -6.4(4) . . . . ? C2 C1 C6 C8 172.0(2) . . . . ? C4 C5 C6 C1 4.3(4) . . . . ? C4 C5 C6 C8 -174.0(2) . . . . ? C9 N1 C8 C6 -179.7(2) . . . . ? Ho1 N1 C8 C6 -1.0(3) . . . . ? C1 C6 C8 N1 -25.4(4) . . . . ? C5 C6 C8 N1 152.8(2) . . . . ? C8 N1 C9 C10 144.1(2) . . . . ? Ho1 N1 C9 C10 -34.7(3) . . . . ? C11 N2 C10 C9 -179.6(2) . . . . ? Ho1 N2 C10 C9 -53.0(2) . . . . ? N1 C9 C10 N2 57.1(3) . . . . ? C10 N2 C11 C12 -178.9(2) . . . . ? Ho1 N2 C11 C12 54.1(2) . . . . ? C13 N3 C12 C11 -166.3(2) . . . . ? Ho1 N3 C12 C11 24.0(3) . . . . ? N2 C11 C12 N3 -50.8(3) . . . . ? C12 N3 C13 C15 -179.3(2) . . . . ? Ho1 N3 C13 C15 -10.6(4) . . . . ? Ho1 O3 C14 C19 -149.2(2) . . . . ? Ho1 O3 C14 C15 31.0(4) . . . . ? O3 C14 C15 C16 -174.9(2) . . . . ? C19 C14 C15 C16 5.3(4) . . . . ? O3 C14 C15 C13 4.6(4) . . . . ? C19 C14 C15 C13 -175.2(2) . . . . ? N3 C13 C15 C16 168.6(3) . . . . ? N3 C13 C15 C14 -10.9(4) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C13 C15 C16 C17 -179.6(2) . . . . ? C15 C16 C17 C18 -3.2(4) . . . . ? C16 C17 C18 C19 1.0(4) . . . . ? C20 O4 C19 C18 122.2(3) . . . . ? C20 O4 C19 C14 -62.8(3) . . . . ? C17 C18 C19 O4 179.6(2) . . . . ? C17 C18 C19 C14 4.6(4) . . . . ? O3 C14 C19 O4 -2.2(4) . . . . ? C15 C14 C19 O4 177.6(2) . . . . ? O3 C14 C19 C18 172.7(2) . . . . ? C15 C14 C19 C18 -7.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.778 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.091 data_mm001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 N8 O14 Tb2' _chemical_formula_weight 1180.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5536(3) _cell_length_b 10.5537(3) _cell_length_c 11.4994(3) _cell_angle_alpha 66.1710(10) _cell_angle_beta 65.0160(10) _cell_angle_gamma 80.0090(10) _cell_volume 1061.98(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7473 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 3.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4304 _exptl_absorpt_correction_T_max 0.4853 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 8893 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4922 _reflns_number_gt 4752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.3331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4922 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.415538(10) 0.353711(10) 1.002997(10) 0.01628(5) Uani 1 1 d . . . N1 N 0.5113(2) 0.1147(2) 1.0952(2) 0.0218(4) Uani 1 1 d . . . N2 N 0.2617(2) 0.2110(2) 1.2501(2) 0.0223(4) Uani 1 1 d . . . H2A H 0.2966 0.2231 1.3069 0.027 Uiso 1 1 calc R . . N3 N 0.2030(2) 0.4855(2) 1.1119(2) 0.0227(4) Uani 1 1 d . . . N4 N 0.2523(2) 0.3143(2) 0.8718(2) 0.0262(4) Uani 1 1 d . . . O1 O 0.59246(19) 0.31954(19) 0.82826(19) 0.0266(4) Uani 1 1 d . . . O2 O 0.8084(2) 0.4231(2) 0.5684(2) 0.0314(4) Uani 1 1 d . . . O3 O 0.46195(17) 0.59274(17) 0.89521(17) 0.0187(3) Uani 1 1 d . . . O4 O 0.5761(2) 0.7269(2) 0.6212(2) 0.0347(4) Uani 1 1 d . . . O5 O 0.2516(2) 0.2292(2) 0.9888(2) 0.0321(4) Uani 1 1 d . . . O6 O 0.3175(2) 0.42578(19) 0.8212(2) 0.0323(4) Uani 1 1 d . . . O7 O 0.1937(3) 0.2871(3) 0.8140(3) 0.0483(6) Uani 1 1 d . . . C1 C 0.7149(3) 0.2601(3) 0.8067(3) 0.0225(5) Uani 1 1 d . . . C2 C 0.8279(3) 0.3122(3) 0.6759(3) 0.0251(5) Uani 1 1 d . . . C3 C 0.9615(3) 0.2603(3) 0.6567(3) 0.0309(6) Uani 1 1 d . . . H3A H 1.0364 0.3016 0.5707 0.037 Uiso 1 1 calc R . . C4 C 0.9888(3) 0.1486(3) 0.7609(3) 0.0321(6) Uani 1 1 d . . . H4A H 1.0815 0.1146 0.7466 0.039 Uiso 1 1 calc R . . C5 C 0.8803(3) 0.0885(3) 0.8843(3) 0.0290(5) Uani 1 1 d . . . H5A H 0.8975 0.0090 0.9538 0.035 Uiso 1 1 calc R . . C6 C 0.7439(3) 0.1427(2) 0.9094(3) 0.0231(5) Uani 1 1 d . . . C7 C 0.7138(4) 0.3959(4) 0.5219(4) 0.0489(8) Uani 1 1 d . . . H7A H 0.7053 0.4785 0.4455 0.073 Uiso 1 1 calc R . . H7B H 0.6218 0.3722 0.5981 0.073 Uiso 1 1 calc R . . H7C H 0.7492 0.3184 0.4903 0.073 Uiso 1 1 calc R . . C8 C 0.6361(3) 0.0731(3) 1.0432(3) 0.0241(5) Uani 1 1 d . . . H8A H 0.6613 -0.0135 1.0988 0.029 Uiso 1 1 calc R . . C9 C 0.4260(3) 0.0207(3) 1.2349(3) 0.0293(6) Uani 1 1 d . . . H9A H 0.4593 0.0236 1.3024 0.035 Uiso 1 1 calc R . . H9B H 0.4367 -0.0754 1.2377 0.035 Uiso 1 1 calc R . . C10 C 0.2738(3) 0.0623(3) 1.2741(3) 0.0269(5) Uani 1 1 d . . . H10A H 0.2353 0.0434 1.2178 0.032 Uiso 1 1 calc R . . H10B H 0.2199 0.0079 1.3727 0.032 Uiso 1 1 calc R . . C11 C 0.1163(3) 0.2606(3) 1.2897(3) 0.0271(5) Uani 1 1 d . . . H11A H 0.0626 0.2105 1.3894 0.033 Uiso 1 1 calc R . . H11B H 0.0718 0.2437 1.2369 0.033 Uiso 1 1 calc R . . C12 C 0.1166(3) 0.4143(3) 1.2590(3) 0.0286(5) Uani 1 1 d . . . H12A H 0.0199 0.4510 1.2806 0.034 Uiso 1 1 calc R . . H12B H 0.1549 0.4305 1.3169 0.034 Uiso 1 1 calc R . . C13 C 0.1617(2) 0.6048(3) 1.0508(3) 0.0234(5) Uani 1 1 d . . . H13A H 0.0785 0.6412 1.1030 0.028 Uiso 1 1 calc R . . C14 C 0.2350(3) 0.6892(2) 0.9045(3) 0.0213(5) Uani 1 1 d . . . C15 C 0.1546(3) 0.7835(3) 0.8365(3) 0.0272(5) Uani 1 1 d . . . H15A H 0.0585 0.7958 0.8874 0.033 Uiso 1 1 calc R . . C16 C 0.2133(3) 0.8585(3) 0.6969(3) 0.0334(6) Uani 1 1 d . . . H16A H 0.1582 0.9224 0.6514 0.040 Uiso 1 1 calc R . . C17 C 0.3541(3) 0.8400(3) 0.6229(3) 0.0325(6) Uani 1 1 d . . . H17A H 0.3944 0.8898 0.5260 0.039 Uiso 1 1 calc R . . C18 C 0.4364(3) 0.7500(3) 0.6887(3) 0.0239(5) Uani 1 1 d . . . C19 C 0.3796(2) 0.6750(2) 0.8321(3) 0.0188(4) Uani 1 1 d . . . C20 C 0.6285(3) 0.7524(4) 0.4788(3) 0.0445(7) Uani 1 1 d . . . H20A H 0.7288 0.7316 0.4457 0.067 Uiso 1 1 calc R . . H20B H 0.6134 0.8499 0.4284 0.067 Uiso 1 1 calc R . . H20C H 0.5798 0.6934 0.4635 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01576(6) 0.01890(6) 0.01398(7) -0.00524(4) -0.00571(5) -0.00200(4) N1 0.0244(10) 0.0206(9) 0.0188(10) -0.0041(8) -0.0090(8) -0.0025(8) N2 0.0235(10) 0.0256(10) 0.0179(10) -0.0065(8) -0.0070(8) -0.0074(8) N3 0.0199(10) 0.0280(10) 0.0183(10) -0.0091(8) -0.0042(8) -0.0025(8) N4 0.0249(11) 0.0335(11) 0.0258(12) -0.0142(9) -0.0118(9) -0.0001(9) O1 0.0262(9) 0.0294(9) 0.0196(9) -0.0086(7) -0.0070(7) 0.0050(7) O2 0.0325(10) 0.0349(10) 0.0219(10) -0.0062(8) -0.0076(8) -0.0072(8) O3 0.0187(8) 0.0199(7) 0.0170(8) -0.0033(6) -0.0094(6) -0.0017(6) O4 0.0219(9) 0.0606(13) 0.0202(10) -0.0132(9) -0.0070(7) -0.0045(9) O5 0.0402(11) 0.0333(10) 0.0254(10) -0.0044(8) -0.0161(9) -0.0137(8) O6 0.0401(11) 0.0293(9) 0.0304(11) -0.0042(8) -0.0203(9) -0.0073(8) O7 0.0550(14) 0.0642(15) 0.0446(14) -0.0197(12) -0.0311(12) -0.0155(12) C1 0.0224(12) 0.0255(11) 0.0226(13) -0.0130(10) -0.0076(10) -0.0002(9) C2 0.0265(12) 0.0276(12) 0.0231(13) -0.0128(10) -0.0075(10) -0.0021(9) C3 0.0230(13) 0.0420(15) 0.0292(14) -0.0191(12) -0.0047(11) -0.0032(11) C4 0.0231(13) 0.0408(15) 0.0395(16) -0.0243(13) -0.0112(11) 0.0039(11) C5 0.0293(13) 0.0281(12) 0.0364(15) -0.0150(11) -0.0171(12) 0.0028(10) C6 0.0255(12) 0.0230(11) 0.0257(13) -0.0121(10) -0.0125(10) 0.0021(9) C7 0.058(2) 0.058(2) 0.0337(18) -0.0058(15) -0.0261(16) -0.0143(17) C8 0.0313(13) 0.0212(11) 0.0236(13) -0.0078(10) -0.0147(11) 0.0006(9) C9 0.0332(14) 0.0248(12) 0.0199(13) 0.0001(10) -0.0080(11) -0.0037(10) C10 0.0308(13) 0.0234(11) 0.0214(13) -0.0033(10) -0.0072(10) -0.0083(10) C11 0.0230(12) 0.0336(13) 0.0181(12) -0.0077(10) -0.0006(9) -0.0084(10) C12 0.0260(13) 0.0318(13) 0.0184(13) -0.0090(10) 0.0003(10) -0.0013(10) C13 0.0177(11) 0.0308(12) 0.0229(13) -0.0132(10) -0.0059(9) -0.0003(9) C14 0.0211(11) 0.0237(11) 0.0220(12) -0.0104(9) -0.0096(9) 0.0011(9) C15 0.0239(12) 0.0304(12) 0.0310(14) -0.0139(11) -0.0141(11) 0.0067(10) C16 0.0376(15) 0.0320(13) 0.0329(15) -0.0063(12) -0.0236(13) 0.0062(11) C17 0.0385(15) 0.0355(14) 0.0226(13) -0.0017(11) -0.0178(12) -0.0048(11) C18 0.0222(11) 0.0297(12) 0.0204(12) -0.0062(10) -0.0105(10) -0.0036(9) C19 0.0212(11) 0.0195(10) 0.0202(12) -0.0075(9) -0.0121(9) -0.0004(8) C20 0.0363(16) 0.064(2) 0.0326(17) -0.0210(16) -0.0115(13) 0.0035(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.1992(18) . ? Tb1 O3 2.3297(16) 2_667 ? Tb1 O3 2.3515(16) . ? Tb1 O5 2.4383(18) . ? Tb1 O6 2.5080(19) . ? Tb1 N1 2.523(2) . ? Tb1 N3 2.547(2) . ? Tb1 N2 2.544(2) . ? Tb1 N4 2.893(2) . ? Tb1 Tb1 3.7883(2) 2_667 ? N1 C8 1.278(3) . ? N1 C9 1.475(3) . ? N2 C10 1.472(3) . ? N2 C11 1.470(3) . ? N3 C13 1.274(3) . ? N3 C12 1.471(3) . ? N4 O7 1.213(3) . ? N4 O6 1.259(3) . ? N4 O5 1.278(3) . ? O1 C1 1.303(3) . ? O2 C2 1.380(3) . ? O2 C7 1.428(4) . ? O3 C19 1.341(3) . ? O3 Tb1 2.3297(16) 2_667 ? O4 C18 1.378(3) . ? O4 C20 1.411(4) . ? C1 C2 1.425(4) . ? C1 C6 1.420(4) . ? C2 C3 1.380(4) . ? C3 C4 1.393(4) . ? C4 C5 1.371(4) . ? C5 C6 1.407(4) . ? C6 C8 1.449(4) . ? C9 C10 1.510(4) . ? C11 C12 1.514(4) . ? C13 C14 1.467(4) . ? C14 C15 1.399(3) . ? C14 C19 1.412(3) . ? C15 C16 1.376(4) . ? C16 C17 1.391(4) . ? C17 C18 1.385(4) . ? C18 C19 1.407(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 99.47(7) . 2_667 ? O1 Tb1 O3 89.76(6) . . ? O3 Tb1 O3 71.95(6) 2_667 . ? O1 Tb1 O5 93.37(7) . . ? O3 Tb1 O5 157.21(6) 2_667 . ? O3 Tb1 O5 127.18(6) . . ? O1 Tb1 O6 77.20(7) . . ? O3 Tb1 O6 149.95(6) 2_667 . ? O3 Tb1 O6 78.14(6) . . ? O5 Tb1 O6 51.60(6) . . ? O1 Tb1 N1 72.62(7) . . ? O3 Tb1 N1 82.34(6) 2_667 . ? O3 Tb1 N1 146.02(6) . . ? O5 Tb1 N1 83.67(7) . . ? O6 Tb1 N1 123.51(6) . . ? O1 Tb1 N3 154.04(7) . . ? O3 Tb1 N3 90.35(6) 2_667 . ? O3 Tb1 N3 70.41(6) . . ? O5 Tb1 N3 86.09(7) . . ? O6 Tb1 N3 82.28(7) . . ? N1 Tb1 N3 132.87(7) . . ? O1 Tb1 N2 137.99(7) . . ? O3 Tb1 N2 84.52(6) 2_667 . ? O3 Tb1 N2 130.27(6) . . ? O5 Tb1 N2 73.41(6) . . ? O6 Tb1 N2 118.19(7) . . ? N1 Tb1 N2 66.47(7) . . ? N3 Tb1 N2 66.49(7) . . ? O1 Tb1 N4 83.07(7) . . ? O3 Tb1 N4 174.41(6) 2_667 . ? O3 Tb1 N4 103.19(6) . . ? O5 Tb1 N4 26.00(6) . . ? O6 Tb1 N4 25.72(6) . . ? N1 Tb1 N4 103.20(6) . . ? N3 Tb1 N4 85.33(6) . . ? N2 Tb1 N4 96.95(7) . . ? O1 Tb1 Tb1 95.66(5) . 2_667 ? O3 Tb1 Tb1 36.17(4) 2_667 2_667 ? O3 Tb1 Tb1 35.78(4) . 2_667 ? O5 Tb1 Tb1 160.40(5) . 2_667 ? O6 Tb1 Tb1 113.87(4) . 2_667 ? N1 Tb1 Tb1 115.64(5) . 2_667 ? N3 Tb1 Tb1 78.21(5) . 2_667 ? N2 Tb1 Tb1 110.03(4) . 2_667 ? N4 Tb1 Tb1 138.91(5) . 2_667 ? C8 N1 C9 114.9(2) . . ? C8 N1 Tb1 126.28(17) . . ? C9 N1 Tb1 117.81(16) . . ? C10 N2 C11 113.05(19) . . ? C10 N2 Tb1 111.04(15) . . ? C11 N2 Tb1 112.32(15) . . ? C13 N3 C12 116.9(2) . . ? C13 N3 Tb1 126.52(18) . . ? C12 N3 Tb1 116.58(16) . . ? O7 N4 O6 122.8(2) . . ? O7 N4 O5 121.1(2) . . ? O6 N4 O5 116.2(2) . . ? O7 N4 Tb1 173.2(2) . . ? O6 N4 Tb1 59.81(12) . . ? O5 N4 Tb1 56.73(11) . . ? C1 O1 Tb1 137.30(16) . . ? C2 O2 C7 113.8(2) . . ? C19 O3 Tb1 128.72(13) . 2_667 ? C19 O3 Tb1 118.16(13) . . ? Tb1 O3 Tb1 108.05(6) 2_667 . ? C18 O4 C20 119.0(2) . . ? N4 O5 Tb1 97.27(13) . . ? N4 O6 Tb1 94.47(14) . . ? O1 C1 C2 120.5(2) . . ? O1 C1 C6 122.9(2) . . ? C2 C1 C6 116.5(2) . . ? O2 C2 C3 118.2(2) . . ? O2 C2 C1 120.6(2) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 121.3(3) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 120.9(3) . . ? C5 C6 C1 120.8(2) . . ? C5 C6 C8 117.1(2) . . ? C1 C6 C8 122.2(2) . . ? N1 C8 C6 127.6(2) . . ? N1 C9 C10 110.6(2) . . ? N2 C10 C9 109.0(2) . . ? N2 C11 C12 108.5(2) . . ? N3 C12 C11 108.9(2) . . ? N3 C13 C14 123.8(2) . . ? C15 C14 C19 120.4(2) . . ? C15 C14 C13 117.2(2) . . ? C19 C14 C13 122.4(2) . . ? C16 C15 C14 120.7(2) . . ? C17 C16 C15 119.4(2) . . ? C16 C17 C18 120.8(3) . . ? C17 C18 O4 123.6(2) . . ? C17 C18 C19 120.8(2) . . ? O4 C18 C19 115.6(2) . . ? O3 C19 C18 120.0(2) . . ? O3 C19 C14 122.3(2) . . ? C18 C19 C14 117.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 N1 C8 25.4(2) . . . . ? O3 Tb1 N1 C8 -77.0(2) 2_667 . . . ? O3 Tb1 N1 C8 -36.4(3) . . . . ? O5 Tb1 N1 C8 121.0(2) . . . . ? O6 Tb1 N1 C8 86.4(2) . . . . ? N3 Tb1 N1 C8 -160.35(18) . . . . ? N2 Tb1 N1 C8 -164.4(2) . . . . ? N4 Tb1 N1 C8 103.7(2) . . . . ? Tb1 Tb1 N1 C8 -62.5(2) 2_667 . . . ? O1 Tb1 N1 C9 -166.82(19) . . . . ? O3 Tb1 N1 C9 90.70(18) 2_667 . . . ? O3 Tb1 N1 C9 131.35(17) . . . . ? O5 Tb1 N1 C9 -71.27(18) . . . . ? O6 Tb1 N1 C9 -105.88(18) . . . . ? N3 Tb1 N1 C9 7.4(2) . . . . ? N2 Tb1 N1 C9 3.37(17) . . . . ? N4 Tb1 N1 C9 -88.55(18) . . . . ? Tb1 Tb1 N1 C9 105.22(17) 2_667 . . . ? O1 Tb1 N2 C10 -16.4(2) . . . . ? O3 Tb1 N2 C10 -114.50(16) 2_667 . . . ? O3 Tb1 N2 C10 -175.22(14) . . . . ? O5 Tb1 N2 C10 59.75(16) . . . . ? O6 Tb1 N2 C10 86.25(17) . . . . ? N1 Tb1 N2 C10 -30.49(15) . . . . ? N3 Tb1 N2 C10 152.72(17) . . . . ? N4 Tb1 N2 C10 70.92(16) . . . . ? Tb1 Tb1 N2 C10 -140.59(14) 2_667 . . . ? O1 Tb1 N2 C11 -144.12(15) . . . . ? O3 Tb1 N2 C11 117.80(16) 2_667 . . . ? O3 Tb1 N2 C11 57.09(18) . . . . ? O5 Tb1 N2 C11 -67.94(16) . . . . ? O6 Tb1 N2 C11 -41.44(17) . . . . ? N1 Tb1 N2 C11 -158.18(17) . . . . ? N3 Tb1 N2 C11 25.03(15) . . . . ? N4 Tb1 N2 C11 -56.78(16) . . . . ? Tb1 Tb1 N2 C11 91.72(15) 2_667 . . . ? O1 Tb1 N3 C13 -8.5(3) . . . . ? O3 Tb1 N3 C13 104.4(2) 2_667 . . . ? O3 Tb1 N3 C13 33.69(19) . . . . ? O5 Tb1 N3 C13 -98.2(2) . . . . ? O6 Tb1 N3 C13 -46.4(2) . . . . ? N1 Tb1 N3 C13 -175.79(18) . . . . ? N2 Tb1 N3 C13 -171.8(2) . . . . ? N4 Tb1 N3 C13 -72.1(2) . . . . ? Tb1 Tb1 N3 C13 70.0(2) 2_667 . . . ? O1 Tb1 N3 C12 169.00(17) . . . . ? O3 Tb1 N3 C12 -78.14(17) 2_667 . . . ? O3 Tb1 N3 C12 -148.82(18) . . . . ? O5 Tb1 N3 C12 79.33(17) . . . . ? O6 Tb1 N3 C12 131.09(17) . . . . ? N1 Tb1 N3 C12 1.7(2) . . . . ? N2 Tb1 N3 C12 5.73(16) . . . . ? N4 Tb1 N3 C12 105.39(17) . . . . ? Tb1 Tb1 N3 C12 -112.46(17) 2_667 . . . ? O1 Tb1 N4 O7 39.4(17) . . . . ? O3 Tb1 N4 O7 156.7(15) 2_667 . . . ? O3 Tb1 N4 O7 127.5(17) . . . . ? O5 Tb1 N4 O7 -73.3(17) . . . . ? O6 Tb1 N4 O7 114.2(18) . . . . ? N1 Tb1 N4 O7 -30.9(17) . . . . ? N3 Tb1 N4 O7 -163.9(17) . . . . ? N2 Tb1 N4 O7 -98.3(17) . . . . ? Tb1 Tb1 N4 O7 130.0(17) 2_667 . . . ? O1 Tb1 N4 O6 -74.82(15) . . . . ? O3 Tb1 N4 O6 42.6(7) 2_667 . . . ? O3 Tb1 N4 O6 13.30(16) . . . . ? O5 Tb1 N4 O6 172.6(2) . . . . ? N1 Tb1 N4 O6 -145.10(15) . . . . ? N3 Tb1 N4 O6 81.91(15) . . . . ? N2 Tb1 N4 O6 147.51(15) . . . . ? Tb1 Tb1 N4 O6 15.85(18) 2_667 . . . ? O1 Tb1 N4 O5 112.61(16) . . . . ? O3 Tb1 N4 O5 -130.0(6) 2_667 . . . ? O3 Tb1 N4 O5 -159.27(15) . . . . ? O6 Tb1 N4 O5 -172.6(2) . . . . ? N1 Tb1 N4 O5 42.34(16) . . . . ? N3 Tb1 N4 O5 -90.65(15) . . . . ? N2 Tb1 N4 O5 -25.05(16) . . . . ? Tb1 Tb1 N4 O5 -156.71(13) 2_667 . . . ? O3 Tb1 O1 C1 41.1(2) 2_667 . . . ? O3 Tb1 O1 C1 112.8(2) . . . . ? O5 Tb1 O1 C1 -120.0(2) . . . . ? O6 Tb1 O1 C1 -169.3(2) . . . . ? N1 Tb1 O1 C1 -37.7(2) . . . . ? N3 Tb1 O1 C1 152.0(2) . . . . ? N2 Tb1 O1 C1 -51.2(3) . . . . ? N4 Tb1 O1 C1 -143.9(2) . . . . ? Tb1 Tb1 O1 C1 77.4(2) 2_667 . . . ? O1 Tb1 O3 C19 102.94(17) . . . . ? O3 Tb1 O3 C19 -157.0(2) 2_667 . . . ? O5 Tb1 O3 C19 8.88(19) . . . . ? O6 Tb1 O3 C19 25.97(16) . . . . ? N1 Tb1 O3 C19 160.22(16) . . . . ? N3 Tb1 O3 C19 -59.97(16) . . . . ? N2 Tb1 O3 C19 -91.07(17) . . . . ? N4 Tb1 O3 C19 20.11(18) . . . . ? Tb1 Tb1 O3 C19 -157.0(2) 2_667 . . . ? O1 Tb1 O3 Tb1 -100.05(8) . . . 2_667 ? O3 Tb1 O3 Tb1 0.0 2_667 . . 2_667 ? O5 Tb1 O3 Tb1 165.90(7) . . . 2_667 ? O6 Tb1 O3 Tb1 -177.01(8) . . . 2_667 ? N1 Tb1 O3 Tb1 -42.76(14) . . . 2_667 ? N3 Tb1 O3 Tb1 97.05(8) . . . 2_667 ? N2 Tb1 O3 Tb1 65.94(10) . . . 2_667 ? N4 Tb1 O3 Tb1 177.13(6) . . . 2_667 ? O7 N4 O5 Tb1 172.4(2) . . . . ? O6 N4 O5 Tb1 -7.2(2) . . . . ? O1 Tb1 O5 N4 -66.63(15) . . . . ? O3 Tb1 O5 N4 168.90(14) 2_667 . . . ? O3 Tb1 O5 N4 25.63(18) . . . . ? O6 Tb1 O5 N4 4.11(13) . . . . ? N1 Tb1 O5 N4 -138.72(16) . . . . ? N3 Tb1 O5 N4 87.36(15) . . . . ? N2 Tb1 O5 N4 153.99(16) . . . . ? Tb1 Tb1 O5 N4 50.8(2) 2_667 . . . ? O7 N4 O6 Tb1 -172.7(2) . . . . ? O5 N4 O6 Tb1 6.9(2) . . . . ? O1 Tb1 O6 N4 100.74(15) . . . . ? O3 Tb1 O6 N4 -172.45(13) 2_667 . . . ? O3 Tb1 O6 N4 -166.77(16) . . . . ? O5 Tb1 O6 N4 -4.15(14) . . . . ? N1 Tb1 O6 N4 41.92(18) . . . . ? N3 Tb1 O6 N4 -95.27(15) . . . . ? N2 Tb1 O6 N4 -37.22(17) . . . . ? Tb1 Tb1 O6 N4 -168.68(13) 2_667 . . . ? Tb1 O1 C1 C2 -148.41(19) . . . . ? Tb1 O1 C1 C6 31.4(4) . . . . ? C7 O2 C2 C3 120.8(3) . . . . ? C7 O2 C2 C1 -64.2(3) . . . . ? O1 C1 C2 O2 -2.4(4) . . . . ? C6 C1 C2 O2 177.9(2) . . . . ? O1 C1 C2 C3 172.5(2) . . . . ? C6 C1 C2 C3 -7.3(3) . . . . ? O2 C2 C3 C4 179.9(2) . . . . ? C1 C2 C3 C4 4.9(4) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C3 C4 C5 C6 -3.5(4) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C4 C5 C6 C8 -179.4(2) . . . . ? O1 C1 C6 C5 -175.3(2) . . . . ? C2 C1 C6 C5 4.4(3) . . . . ? O1 C1 C6 C8 5.0(4) . . . . ? C2 C1 C6 C8 -175.3(2) . . . . ? C9 N1 C8 C6 -179.6(2) . . . . ? Tb1 N1 C8 C6 -11.5(4) . . . . ? C5 C6 C8 N1 169.4(2) . . . . ? C1 C6 C8 N1 -10.9(4) . . . . ? C8 N1 C9 C10 -167.6(2) . . . . ? Tb1 N1 C9 C10 23.3(3) . . . . ? C11 N2 C10 C9 -178.1(2) . . . . ? Tb1 N2 C10 C9 54.6(2) . . . . ? N1 C9 C10 N2 -51.0(3) . . . . ? C10 N2 C11 C12 -179.3(2) . . . . ? Tb1 N2 C11 C12 -52.7(2) . . . . ? C13 N3 C12 C11 143.4(2) . . . . ? Tb1 N3 C12 C11 -34.3(3) . . . . ? N2 C11 C12 N3 56.7(3) . . . . ? C12 N3 C13 C14 -179.6(2) . . . . ? Tb1 N3 C13 C14 -2.1(3) . . . . ? N3 C13 C14 C15 153.1(2) . . . . ? N3 C13 C14 C19 -25.3(4) . . . . ? C19 C14 C15 C16 3.5(4) . . . . ? C13 C14 C15 C16 -174.8(2) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? C15 C16 C17 C18 -1.7(4) . . . . ? C16 C17 C18 O4 179.8(3) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C20 O4 C18 C17 -23.9(4) . . . . ? C20 O4 C18 C19 156.0(3) . . . . ? Tb1 O3 C19 C18 91.3(2) 2_667 . . . ? Tb1 O3 C19 C18 -117.1(2) . . . . ? Tb1 O3 C19 C14 -89.3(2) 2_667 . . . ? Tb1 O3 C19 C14 62.3(3) . . . . ? C17 C18 C19 O3 -177.1(2) . . . . ? O4 C18 C19 O3 3.0(3) . . . . ? C17 C18 C19 C14 3.5(4) . . . . ? O4 C18 C19 C14 -176.4(2) . . . . ? C15 C14 C19 O3 175.5(2) . . . . ? C13 C14 C19 O3 -6.3(3) . . . . ? C15 C14 C19 C18 -5.2(3) . . . . ? C13 C14 C19 C18 173.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.702 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.116 data_mm002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Ho2 N8 O14' _chemical_formula_weight 1192.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ho' 'Ho' -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5104(4) _cell_length_b 10.5297(4) _cell_length_c 11.4828(4) _cell_angle_alpha 66.414(2) _cell_angle_beta 65.1260(10) _cell_angle_gamma 79.981(2) _cell_volume 1056.59(7) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 3.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5029 _exptl_absorpt_correction_T_max 0.5174 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16595 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5157 _reflns_number_gt 5109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.3973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5157 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0131 _refine_ls_R_factor_gt 0.0130 _refine_ls_wR_factor_ref 0.0347 _refine_ls_wR_factor_gt 0.0346 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.414833(6) 0.854317(6) 0.504937(5) 0.01624(3) Uani 1 1 d . . . N1 N 0.20284(13) 0.98648(14) 0.61018(13) 0.0224(2) Uani 1 1 d . . . N2 N 0.26166(14) 0.71379(14) 0.74905(13) 0.0222(2) Uani 1 1 d . . . H2A H 0.2958 0.7271 0.8060 0.027 Uiso 1 1 calc R . . N3 N 0.51119(14) 0.61757(14) 0.59559(13) 0.0228(2) Uani 1 1 d . . . N4 N 0.25357(15) 0.81236(16) 0.37453(14) 0.0256(3) Uani 1 1 d . . . O1 O 0.46244(11) 1.09058(11) 0.39589(10) 0.01839(19) Uani 1 1 d . . . O2 O 0.57789(12) 1.22029(14) 0.12191(12) 0.0301(3) Uani 1 1 d . . . O3 O 0.59087(12) 0.82174(12) 0.33048(11) 0.0262(2) Uani 1 1 d . . . O4 O 0.80483(14) 0.92459(14) 0.06964(12) 0.0320(3) Uani 1 1 d . . . O5 O 0.31606(14) 0.92485(13) 0.32516(13) 0.0324(3) Uani 1 1 d . . . O6 O 0.25489(14) 0.72743(13) 0.49090(13) 0.0315(3) Uani 1 1 d . . . O7 O 0.19471(18) 0.78403(18) 0.31705(16) 0.0479(4) Uani 1 1 d . . . C1 C 0.38063(15) 1.17336(15) 0.33159(15) 0.0180(3) Uani 1 1 d . . . C2 C 0.43826(16) 1.24592(17) 0.18767(15) 0.0226(3) Uani 1 1 d . . . C3 C 0.35660(19) 1.33648(19) 0.12063(17) 0.0296(3) Uani 1 1 d . . . H3A H 0.3973 1.3848 0.0237 0.035 Uiso 1 1 calc R . . C4 C 0.21560(19) 1.35743(19) 0.19384(19) 0.0320(4) Uani 1 1 d . . . H4A H 0.1608 1.4215 0.1477 0.038 Uiso 1 1 calc R . . C5 C 0.15628(17) 1.28435(18) 0.33388(18) 0.0273(3) Uani 1 1 d . . . H5A H 0.0602 1.2986 0.3844 0.033 Uiso 1 1 calc R . . C6 C 0.23618(15) 1.18940(16) 0.40231(15) 0.0207(3) Uani 1 1 d . . . C7 C 0.6305(2) 1.2542(2) -0.02251(18) 0.0384(4) Uani 1 1 d . . . H7A H 0.7307 1.2315 -0.0564 0.058 Uiso 1 1 calc R . . H7B H 0.6169 1.3536 -0.0680 0.058 Uiso 1 1 calc R . . H7C H 0.5802 1.2011 -0.0430 0.058 Uiso 1 1 calc R . . C8 C 0.16223(16) 1.10602(17) 0.54790(16) 0.0232(3) Uani 1 1 d . . . H8A H 0.0787 1.1432 0.5993 0.028 Uiso 1 1 calc R . . C9 C 0.11532(18) 0.91680(18) 0.75683(16) 0.0290(3) Uani 1 1 d . . . H9A H 0.0183 0.9537 0.7774 0.035 Uiso 1 1 calc R . . H9B H 0.1530 0.9338 0.8151 0.035 Uiso 1 1 calc R . . C10 C 0.11571(17) 0.76301(18) 0.78755(16) 0.0265(3) Uani 1 1 d . . . H10A H 0.0615 0.7132 0.8869 0.032 Uiso 1 1 calc R . . H10B H 0.0719 0.7454 0.7342 0.032 Uiso 1 1 calc R . . C11 C 0.27467(18) 0.56442(17) 0.77440(16) 0.0269(3) Uani 1 1 d . . . H11A H 0.2361 0.5438 0.7187 0.032 Uiso 1 1 calc R . . H11B H 0.2210 0.5110 0.8730 0.032 Uiso 1 1 calc R . . C12 C 0.4276(2) 0.52361(18) 0.73536(17) 0.0303(3) Uani 1 1 d . . . H12A H 0.4612 0.5280 0.8023 0.036 Uiso 1 1 calc R . . H12B H 0.4394 0.4272 0.7383 0.036 Uiso 1 1 calc R . . C13 C 0.63662(18) 0.57503(16) 0.54271(17) 0.0248(3) Uani 1 1 d . . . H13A H 0.6623 0.4883 0.5978 0.030 Uiso 1 1 calc R . . C14 C 0.71351(17) 0.76177(17) 0.30732(16) 0.0225(3) Uani 1 1 d . . . C15 C 0.74336(17) 0.64405(16) 0.40878(16) 0.0231(3) Uani 1 1 d . . . C16 C 0.88053(18) 0.58886(18) 0.38287(19) 0.0289(3) Uani 1 1 d . . . H16A H 0.8985 0.5095 0.4518 0.035 Uiso 1 1 calc R . . C17 C 0.98809(18) 0.6490(2) 0.2589(2) 0.0331(4) Uani 1 1 d . . . H17A H 1.0813 0.6150 0.2437 0.040 Uiso 1 1 calc R . . C18 C 0.95948(18) 0.7605(2) 0.15542(19) 0.0324(4) Uani 1 1 d . . . H18A H 1.0338 0.8010 0.0689 0.039 Uiso 1 1 calc R . . C19 C 0.82524(17) 0.81315(18) 0.17623(16) 0.0257(3) Uani 1 1 d . . . C20 C 0.7062(3) 0.8996(3) 0.0260(2) 0.0483(5) Uani 1 1 d . . . H20A H 0.6975 0.9825 -0.0500 0.072 Uiso 1 1 calc R . . H20B H 0.6148 0.8778 0.1032 0.072 Uiso 1 1 calc R . . H20C H 0.7386 0.8214 -0.0055 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01622(4) 0.01736(4) 0.01434(4) -0.00422(3) -0.00569(3) -0.00270(2) N1 0.0195(6) 0.0258(6) 0.0179(6) -0.0069(5) -0.0033(5) -0.0041(5) N2 0.0243(6) 0.0235(6) 0.0180(6) -0.0055(5) -0.0066(5) -0.0072(5) N3 0.0264(6) 0.0198(6) 0.0198(6) -0.0032(5) -0.0089(5) -0.0042(5) N4 0.0251(6) 0.0318(7) 0.0254(6) -0.0129(6) -0.0117(5) -0.0018(5) O1 0.0176(5) 0.0193(5) 0.0177(5) -0.0033(4) -0.0089(4) -0.0021(4) O2 0.0221(5) 0.0460(7) 0.0191(5) -0.0087(5) -0.0071(4) -0.0029(5) O3 0.0254(5) 0.0277(6) 0.0198(5) -0.0079(4) -0.0060(4) 0.0044(4) O4 0.0337(6) 0.0348(7) 0.0226(5) -0.0066(5) -0.0077(5) -0.0064(5) O5 0.0419(7) 0.0278(6) 0.0312(6) -0.0042(5) -0.0211(5) -0.0073(5) O6 0.0389(7) 0.0317(6) 0.0259(6) -0.0043(5) -0.0157(5) -0.0123(5) O7 0.0552(9) 0.0626(10) 0.0434(8) -0.0193(7) -0.0295(7) -0.0154(8) C1 0.0202(6) 0.0168(6) 0.0188(6) -0.0054(5) -0.0100(5) -0.0007(5) C2 0.0221(7) 0.0254(7) 0.0202(7) -0.0054(6) -0.0092(6) -0.0040(6) C3 0.0335(8) 0.0307(8) 0.0225(7) -0.0029(6) -0.0153(7) -0.0007(7) C4 0.0340(9) 0.0311(9) 0.0326(8) -0.0068(7) -0.0218(7) 0.0074(7) C5 0.0239(7) 0.0297(8) 0.0317(8) -0.0131(7) -0.0147(6) 0.0067(6) C6 0.0202(7) 0.0220(7) 0.0220(7) -0.0092(6) -0.0094(6) 0.0010(5) C7 0.0332(9) 0.0526(12) 0.0236(8) -0.0106(8) -0.0082(7) -0.0019(8) C8 0.0180(7) 0.0292(8) 0.0234(7) -0.0129(6) -0.0057(6) -0.0005(6) C9 0.0277(8) 0.0313(8) 0.0181(7) -0.0087(6) 0.0013(6) -0.0038(6) C10 0.0220(7) 0.0319(8) 0.0191(7) -0.0071(6) -0.0005(5) -0.0092(6) C11 0.0315(8) 0.0220(7) 0.0215(7) -0.0021(6) -0.0072(6) -0.0091(6) C12 0.0355(9) 0.0227(8) 0.0225(8) 0.0015(6) -0.0092(7) -0.0054(7) C13 0.0329(8) 0.0185(7) 0.0251(7) -0.0071(6) -0.0142(6) 0.0005(6) C14 0.0239(7) 0.0233(7) 0.0219(7) -0.0113(6) -0.0074(6) -0.0006(6) C15 0.0244(7) 0.0221(7) 0.0248(7) -0.0111(6) -0.0095(6) 0.0010(6) C16 0.0274(8) 0.0285(8) 0.0364(9) -0.0162(7) -0.0151(7) 0.0043(6) C17 0.0232(8) 0.0395(10) 0.0420(10) -0.0234(8) -0.0111(7) 0.0039(7) C18 0.0245(8) 0.0418(10) 0.0314(8) -0.0200(8) -0.0037(6) -0.0039(7) C19 0.0281(8) 0.0277(8) 0.0222(7) -0.0114(6) -0.0073(6) -0.0033(6) C20 0.0590(14) 0.0549(13) 0.0345(10) -0.0052(9) -0.0270(10) -0.0131(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O3 2.1829(11) . ? Ho1 O1 2.3070(10) 2_676 ? Ho1 O1 2.3282(11) . ? Ho1 O6 2.4123(12) . ? Ho1 O5 2.4897(12) . ? Ho1 N3 2.5011(13) . ? Ho1 N2 2.5203(13) . ? Ho1 N1 2.5225(13) . ? Ho1 N4 2.8697(13) . ? Ho1 Ho1 3.75402(17) 2_676 ? N1 C8 1.276(2) . ? N1 C9 1.4708(19) . ? N2 C10 1.467(2) . ? N2 C11 1.473(2) . ? N3 C13 1.283(2) . ? N3 C12 1.474(2) . ? N4 O7 1.2135(18) . ? N4 O5 1.2553(19) . ? N4 O6 1.2808(19) . ? O1 C1 1.3426(17) . ? O1 Ho1 2.3070(10) 2_676 ? O2 C2 1.3747(19) . ? O2 C7 1.416(2) . ? O3 C14 1.3015(19) . ? O4 C19 1.380(2) . ? O4 C20 1.426(2) . ? C1 C2 1.411(2) . ? C1 C6 1.406(2) . ? C2 C3 1.386(2) . ? C3 C4 1.392(3) . ? C4 C5 1.378(2) . ? C5 C6 1.399(2) . ? C6 C8 1.463(2) . ? C9 C10 1.513(2) . ? C11 C12 1.509(3) . ? C13 C15 1.446(2) . ? C14 C15 1.417(2) . ? C14 C19 1.421(2) . ? C15 C16 1.411(2) . ? C16 C17 1.371(3) . ? C17 C18 1.393(3) . ? C18 C19 1.380(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ho1 O1 99.21(4) . 2_676 ? O3 Ho1 O1 88.50(4) . . ? O1 Ho1 O1 71.83(4) 2_676 . ? O3 Ho1 O6 92.99(5) . . ? O1 Ho1 O6 157.35(4) 2_676 . ? O1 Ho1 O6 127.86(4) . . ? O3 Ho1 O5 77.06(4) . . ? O1 Ho1 O5 149.62(4) 2_676 . ? O1 Ho1 O5 77.91(4) . . ? O6 Ho1 O5 52.02(4) . . ? O3 Ho1 N3 73.04(4) . . ? O1 Ho1 N3 82.59(4) 2_676 . ? O1 Ho1 N3 145.63(4) . . ? O6 Ho1 N3 82.82(4) . . ? O5 Ho1 N3 123.49(4) . . ? O3 Ho1 N2 138.61(4) . . ? O1 Ho1 N2 85.18(4) 2_676 . ? O1 Ho1 N2 131.04(4) . . ? O6 Ho1 N2 73.15(4) . . ? O5 Ho1 N2 117.79(4) . . ? N3 Ho1 N2 66.73(4) . . ? O3 Ho1 N1 152.93(4) . . ? O1 Ho1 N1 90.98(4) 2_676 . ? O1 Ho1 N1 70.87(4) . . ? O6 Ho1 N1 86.58(5) . . ? O5 Ho1 N1 81.49(4) . . ? N3 Ho1 N1 133.50(4) . . ? N2 Ho1 N1 66.85(4) . . ? O3 Ho1 N4 82.69(4) . . ? O1 Ho1 N4 174.63(4) 2_676 . ? O1 Ho1 N4 103.29(4) . . ? O6 Ho1 N4 26.28(4) . . ? O5 Ho1 N4 25.86(4) . . ? N3 Ho1 N4 102.78(4) . . ? N2 Ho1 N4 96.73(4) . . ? N1 Ho1 N4 85.19(4) . . ? O3 Ho1 Ho1 94.71(3) . 2_676 ? O1 Ho1 Ho1 36.10(3) 2_676 2_676 ? O1 Ho1 Ho1 35.73(2) . 2_676 ? O6 Ho1 Ho1 161.39(3) . 2_676 ? O5 Ho1 Ho1 113.60(3) . 2_676 ? N3 Ho1 Ho1 115.64(3) . 2_676 ? N2 Ho1 Ho1 110.83(3) . 2_676 ? N1 Ho1 Ho1 78.89(3) . 2_676 ? N4 Ho1 Ho1 138.97(3) . 2_676 ? C8 N1 C9 116.92(13) . . ? C8 N1 Ho1 126.43(10) . . ? C9 N1 Ho1 116.62(10) . . ? C10 N2 C11 113.00(13) . . ? C10 N2 Ho1 112.30(9) . . ? C11 N2 Ho1 111.43(9) . . ? C13 N3 C12 114.38(14) . . ? C13 N3 Ho1 126.46(11) . . ? C12 N3 Ho1 118.18(10) . . ? O7 N4 O5 122.88(15) . . ? O7 N4 O6 121.11(15) . . ? O5 N4 O6 116.01(13) . . ? O7 N4 Ho1 173.46(13) . . ? O5 N4 Ho1 59.91(8) . . ? O6 N4 Ho1 56.51(7) . . ? C1 O1 Ho1 128.36(9) . 2_676 ? C1 O1 Ho1 118.52(9) . . ? Ho1 O1 Ho1 108.17(4) 2_676 . ? C2 O2 C7 117.66(13) . . ? C14 O3 Ho1 137.77(10) . . ? C19 O4 C20 113.93(15) . . ? N4 O5 Ho1 94.23(9) . . ? N4 O6 Ho1 97.21(9) . . ? O1 C1 C2 120.12(13) . . ? O1 C1 C6 122.31(13) . . ? C2 C1 C6 117.56(13) . . ? O2 C2 C3 123.77(14) . . ? O2 C2 C1 115.41(13) . . ? C3 C2 C1 120.82(15) . . ? C2 C3 C4 120.70(15) . . ? C5 C4 C3 119.36(15) . . ? C4 C5 C6 120.62(15) . . ? C5 C6 C1 120.70(14) . . ? C5 C6 C8 117.18(14) . . ? C1 C6 C8 122.10(13) . . ? N1 C8 C6 124.13(14) . . ? N1 C9 C10 108.57(13) . . ? N2 C10 C9 108.31(13) . . ? N2 C11 C12 108.85(13) . . ? N3 C12 C11 110.11(13) . . ? N3 C13 C15 127.39(15) . . ? O3 C14 C15 122.80(14) . . ? O3 C14 C19 120.54(15) . . ? C15 C14 C19 116.66(14) . . ? C16 C15 C14 120.91(15) . . ? C16 C15 C13 116.80(15) . . ? C14 C15 C13 122.29(14) . . ? C17 C16 C15 120.46(16) . . ? C16 C17 C18 119.41(16) . . ? C19 C18 C17 121.24(17) . . ? O4 C19 C18 118.11(15) . . ? O4 C19 C14 120.80(15) . . ? C18 C19 C14 120.88(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ho1 N1 C8 -9.23(19) . . . . ? O1 Ho1 N1 C8 103.43(13) 2_676 . . . ? O1 Ho1 N1 C8 33.07(13) . . . . ? O6 Ho1 N1 C8 -99.11(13) . . . . ? O5 Ho1 N1 C8 -47.01(13) . . . . ? N3 Ho1 N1 C8 -175.85(12) . . . . ? N2 Ho1 N1 C8 -172.23(14) . . . . ? N4 Ho1 N1 C8 -72.79(13) . . . . ? Ho1 Ho1 N1 C8 69.21(13) 2_676 . . . ? O3 Ho1 N1 C9 168.82(11) . . . . ? O1 Ho1 N1 C9 -78.52(11) 2_676 . . . ? O1 Ho1 N1 C9 -148.88(12) . . . . ? O6 Ho1 N1 C9 78.94(11) . . . . ? O5 Ho1 N1 C9 131.03(12) . . . . ? N3 Ho1 N1 C9 2.19(14) . . . . ? N2 Ho1 N1 C9 5.81(11) . . . . ? N4 Ho1 N1 C9 105.25(11) . . . . ? Ho1 Ho1 N1 C9 -112.74(11) 2_676 . . . ? O3 Ho1 N2 C10 -143.29(10) . . . . ? O1 Ho1 N2 C10 118.24(10) 2_676 . . . ? O1 Ho1 N2 C10 57.48(11) . . . . ? O6 Ho1 N2 C10 -68.43(10) . . . . ? O5 Ho1 N2 C10 -40.86(11) . . . . ? N3 Ho1 N2 C10 -157.76(11) . . . . ? N1 Ho1 N2 C10 25.10(10) . . . . ? N4 Ho1 N2 C10 -56.71(10) . . . . ? Ho1 Ho1 N2 C10 92.35(10) 2_676 . . . ? O3 Ho1 N2 C11 -15.37(13) . . . . ? O1 Ho1 N2 C11 -113.84(10) 2_676 . . . ? O1 Ho1 N2 C11 -174.61(9) . . . . ? O6 Ho1 N2 C11 59.49(10) . . . . ? O5 Ho1 N2 C11 87.06(11) . . . . ? N3 Ho1 N2 C11 -29.84(10) . . . . ? N1 Ho1 N2 C11 153.02(11) . . . . ? N4 Ho1 N2 C11 71.21(10) . . . . ? Ho1 Ho1 N2 C11 -139.73(9) 2_676 . . . ? O3 Ho1 N3 C13 24.55(13) . . . . ? O1 Ho1 N3 C13 -77.48(13) 2_676 . . . ? O1 Ho1 N3 C13 -35.81(16) . . . . ? O6 Ho1 N3 C13 119.90(13) . . . . ? O5 Ho1 N3 C13 85.69(14) . . . . ? N2 Ho1 N3 C13 -165.40(14) . . . . ? N1 Ho1 N3 C13 -161.77(12) . . . . ? N4 Ho1 N3 C13 102.69(13) . . . . ? Ho1 Ho1 N3 C13 -62.52(13) 2_676 . . . ? O3 Ho1 N3 C12 -167.50(12) . . . . ? O1 Ho1 N3 C12 90.48(12) 2_676 . . . ? O1 Ho1 N3 C12 132.14(11) . . . . ? O6 Ho1 N3 C12 -72.14(12) . . . . ? O5 Ho1 N3 C12 -106.35(12) . . . . ? N2 Ho1 N3 C12 2.56(11) . . . . ? N1 Ho1 N3 C12 6.18(14) . . . . ? N4 Ho1 N3 C12 -89.35(12) . . . . ? Ho1 Ho1 N3 C12 105.44(11) 2_676 . . . ? O3 Ho1 N4 O7 41.7(11) . . . . ? O1 Ho1 N4 O7 152.8(10) 2_676 . . . ? O1 Ho1 N4 O7 128.4(11) . . . . ? O6 Ho1 N4 O7 -70.6(11) . . . . ? O5 Ho1 N4 O7 117.0(12) . . . . ? N3 Ho1 N4 O7 -29.0(11) . . . . ? N2 Ho1 N4 O7 -96.6(11) . . . . ? N1 Ho1 N4 O7 -162.6(11) . . . . ? Ho1 Ho1 N4 O7 130.5(11) 2_676 . . . ? O3 Ho1 N4 O5 -75.34(10) . . . . ? O1 Ho1 N4 O5 35.8(4) 2_676 . . . ? O1 Ho1 N4 O5 11.37(10) . . . . ? O6 Ho1 N4 O5 172.42(16) . . . . ? N3 Ho1 N4 O5 -146.03(10) . . . . ? N2 Ho1 N4 O5 146.38(10) . . . . ? N1 Ho1 N4 O5 80.40(10) . . . . ? Ho1 Ho1 N4 O5 13.44(12) 2_676 . . . ? O3 Ho1 N4 O6 112.24(10) . . . . ? O1 Ho1 N4 O6 -136.7(4) 2_676 . . . ? O1 Ho1 N4 O6 -161.06(9) . . . . ? O5 Ho1 N4 O6 -172.42(15) . . . . ? N3 Ho1 N4 O6 41.55(10) . . . . ? N2 Ho1 N4 O6 -26.05(10) . . . . ? N1 Ho1 N4 O6 -92.02(10) . . . . ? Ho1 Ho1 N4 O6 -158.98(8) 2_676 . . . ? O3 Ho1 O1 C1 102.64(10) . . . . ? O1 Ho1 O1 C1 -157.16(12) 2_676 . . . ? O6 Ho1 O1 C1 10.02(12) . . . . ? O5 Ho1 O1 C1 25.55(10) . . . . ? N3 Ho1 O1 C1 158.90(9) . . . . ? N2 Ho1 O1 C1 -90.93(10) . . . . ? N1 Ho1 O1 C1 -59.52(10) . . . . ? N4 Ho1 O1 C1 20.50(10) . . . . ? Ho1 Ho1 O1 C1 -157.16(12) 2_676 . . . ? O3 Ho1 O1 Ho1 -100.20(5) . . . 2_676 ? O1 Ho1 O1 Ho1 0.0 2_676 . . 2_676 ? O6 Ho1 O1 Ho1 167.18(4) . . . 2_676 ? O5 Ho1 O1 Ho1 -177.29(5) . . . 2_676 ? N3 Ho1 O1 Ho1 -43.93(9) . . . 2_676 ? N2 Ho1 O1 Ho1 66.24(6) . . . 2_676 ? N1 Ho1 O1 Ho1 97.64(5) . . . 2_676 ? N4 Ho1 O1 Ho1 177.67(4) . . . 2_676 ? O1 Ho1 O3 C14 42.81(16) 2_676 . . . ? O1 Ho1 O3 C14 114.13(16) . . . . ? O6 Ho1 O3 C14 -118.04(16) . . . . ? O5 Ho1 O3 C14 -167.93(17) . . . . ? N3 Ho1 O3 C14 -36.47(16) . . . . ? N2 Ho1 O3 C14 -50.35(19) . . . . ? N1 Ho1 O3 C14 153.63(14) . . . . ? N4 Ho1 O3 C14 -142.27(16) . . . . ? Ho1 Ho1 O3 C14 78.92(16) 2_676 . . . ? O7 N4 O5 Ho1 -173.06(15) . . . . ? O6 N4 O5 Ho1 7.03(14) . . . . ? O3 Ho1 O5 N4 100.07(10) . . . . ? O1 Ho1 O5 N4 -173.79(8) 2_676 . . . ? O1 Ho1 O5 N4 -168.69(10) . . . . ? O6 Ho1 O5 N4 -4.25(9) . . . . ? N3 Ho1 O5 N4 40.80(11) . . . . ? N2 Ho1 O5 N4 -38.43(11) . . . . ? N1 Ho1 O5 N4 -96.55(10) . . . . ? Ho1 Ho1 O5 N4 -170.42(8) 2_676 . . . ? O7 N4 O6 Ho1 172.79(15) . . . . ? O5 N4 O6 Ho1 -7.29(15) . . . . ? O3 Ho1 O6 N4 -66.83(10) . . . . ? O1 Ho1 O6 N4 170.40(9) 2_676 . . . ? O1 Ho1 O6 N4 23.59(11) . . . . ? O5 Ho1 O6 N4 4.18(9) . . . . ? N3 Ho1 O6 N4 -139.31(10) . . . . ? N2 Ho1 O6 N4 152.89(10) . . . . ? N1 Ho1 O6 N4 86.06(10) . . . . ? Ho1 Ho1 O6 N4 47.54(16) 2_676 . . . ? Ho1 O1 C1 C2 91.39(15) 2_676 . . . ? Ho1 O1 C1 C2 -116.66(13) . . . . ? Ho1 O1 C1 C6 -89.91(16) 2_676 . . . ? Ho1 O1 C1 C6 62.04(16) . . . . ? C7 O2 C2 C3 -19.3(2) . . . . ? C7 O2 C2 C1 160.98(16) . . . . ? O1 C1 C2 O2 2.6(2) . . . . ? C6 C1 C2 O2 -176.12(13) . . . . ? O1 C1 C2 C3 -177.14(15) . . . . ? C6 C1 C2 C3 4.1(2) . . . . ? O2 C2 C3 C4 179.97(16) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -1.7(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C4 C5 C6 C1 4.3(2) . . . . ? C4 C5 C6 C8 -173.97(16) . . . . ? O1 C1 C6 C5 175.18(14) . . . . ? C2 C1 C6 C5 -6.1(2) . . . . ? O1 C1 C6 C8 -6.6(2) . . . . ? C2 C1 C6 C8 172.10(14) . . . . ? C9 N1 C8 C6 -179.74(14) . . . . ? Ho1 N1 C8 C6 -1.7(2) . . . . ? C5 C6 C8 N1 153.43(16) . . . . ? C1 C6 C8 N1 -24.8(2) . . . . ? C8 N1 C9 C10 143.81(15) . . . . ? Ho1 N1 C9 C10 -34.42(17) . . . . ? C11 N2 C10 C9 -179.86(13) . . . . ? Ho1 N2 C10 C9 -52.77(14) . . . . ? N1 C9 C10 N2 56.71(17) . . . . ? C10 N2 C11 C12 -178.44(13) . . . . ? Ho1 N2 C11 C12 54.02(14) . . . . ? C13 N3 C12 C11 -166.59(14) . . . . ? Ho1 N3 C12 C11 24.03(18) . . . . ? N2 C11 C12 N3 -50.74(18) . . . . ? C12 N3 C13 C15 -179.52(16) . . . . ? Ho1 N3 C13 C15 -11.2(2) . . . . ? Ho1 O3 C14 C15 30.2(2) . . . . ? Ho1 O3 C14 C19 -149.75(13) . . . . ? O3 C14 C15 C16 -174.96(15) . . . . ? C19 C14 C15 C16 5.0(2) . . . . ? O3 C14 C15 C13 4.9(2) . . . . ? C19 C14 C15 C13 -175.14(14) . . . . ? N3 C13 C15 C16 169.35(16) . . . . ? N3 C13 C15 C14 -10.5(3) . . . . ? C14 C15 C16 C17 0.5(2) . . . . ? C13 C15 C16 C17 -179.38(15) . . . . ? C15 C16 C17 C18 -3.7(3) . . . . ? C16 C17 C18 C19 1.2(3) . . . . ? C20 O4 C19 C18 122.06(19) . . . . ? C20 O4 C19 C14 -63.2(2) . . . . ? C17 C18 C19 O4 179.36(16) . . . . ? C17 C18 C19 C14 4.6(3) . . . . ? O3 C14 C19 O4 -2.2(2) . . . . ? C15 C14 C19 O4 177.88(14) . . . . ? O3 C14 C19 C18 172.46(15) . . . . ? C15 C14 C19 C18 -7.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.395 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.090