# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 899841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H30 Cl4 Dy0.87 N2 O7 Yb1.13' _chemical_formula_weight 841.13 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' Cl Cl 0.1484 0.1585 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.469(4) _cell_length_b 9.292(2) _cell_length_c 8.889(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.463(3) _cell_angle_gamma 90.00 _cell_volume 1266.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 801 _exptl_absorpt_coefficient_mu 7.150 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4567 _exptl_absorpt_correction_T_max 0.6345 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3640 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.49 _reflns_number_total 1354 _reflns_number_gt 1283 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0200P)^2^+1.5604P] 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 1354 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0499 _refine_ls_wR_factor_gt 0.0490 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.43 2 d SP . 1 Yb1 Yb 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.57 2 d SP . 2 Cl1 Cl 0.37090(7) 0.23233(14) 1.19536(13) 0.0431(3) Uani 1 1 d . . . O1 O 0.4783(2) 0.0000 0.8583(3) 0.0147(7) Uani 1 2 d S . . O2 O 0.31898(16) 0.1562(3) 0.8356(3) 0.0199(5) Uani 1 1 d . . . H2O H 0.2669 0.1860 0.8269 0.024 Uiso 1 1 d R . . C1 C 0.4615(3) 0.0000 0.6957(5) 0.0181(11) Uani 1 2 d S . . H1 H 0.5188 0.0000 0.6552 0.022 Uiso 1 2 calc SR . . C2 C 0.4122(2) 0.1359(4) 0.6390(4) 0.0206(8) Uani 1 1 d . . . H2A H 0.4429 0.2208 0.6876 0.025 Uiso 1 1 calc R . . H2B H 0.4128 0.1443 0.5281 0.025 Uiso 1 1 calc R . . C3 C 0.3183(2) 0.1372(4) 0.6721(4) 0.0198(8) Uani 1 1 d . . . H3 H 0.2877 0.2212 0.6187 0.024 Uiso 1 1 calc R . . C4 C 0.2700(3) 0.0000 0.6178(6) 0.0229(12) Uani 1 2 d S . . H4A H 0.2603 0.0000 0.5055 0.027 Uiso 1 2 calc SR . . H4B H 0.2121 0.0000 0.6541 0.027 Uiso 1 2 calc SR . . N1 N 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP A 1 C5 C 0.1528(6) 0.0000 1.0575(11) 0.016(2) Uani 0.50 2 d SP A 1 C6 C 0.0576(7) 0.0000 1.0419(15) 0.038(3) Uani 0.50 2 d SP . 1 H6A H 0.0386 0.0000 1.1405 0.057 Uiso 0.50 2 d SPR . 1 H6B H 0.0360 0.0844 0.9873 0.057 Uiso 0.50 1 d PR . 1 O1W O 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP B 2 H1WA H 0.2032 -0.0719 1.0043 0.041 Uiso 0.25 1 d PR B 2 H1WB H 0.2214 0.0000 1.1446 0.041 Uiso 0.50 2 d SPR B 2 N2 N 0.1207(7) 0.0000 1.2855(12) 0.036(2) Uani 0.50 2 d SP . . C7 C 0.0712(8) 0.0000 1.3658(12) 0.025(2) Uani 0.50 2 d SP . . C8 C 0.007(2) 0.0000 1.476(3) 0.042(5) Uani 0.50 2 d SP . . H8A H -0.0254 -0.0813 1.4338 0.063 Uiso 0.50 1 d PR . . H8B H 0.0266 0.0000 1.5831 0.063 Uiso 0.50 2 d SPR . . 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 0.01065(14) 0.02274(14) 0.01275(13) 0.000 0.00207(8) 0.000 Yb1 0.01065(14) 0.02274(14) 0.01275(13) 0.000 0.00207(8) 0.000 Cl1 0.0278(6) 0.0620(8) 0.0357(6) -0.0273(5) -0.0108(5) 0.0252(5) O1 0.0111(17) 0.0227(18) 0.0097(15) 0.000 -0.0004(13) 0.000 O2 0.0155(13) 0.0253(14) 0.0188(12) -0.0008(11) 0.0017(10) 0.0074(10) C1 0.012(2) 0.032(3) 0.012(2) 0.000 0.0064(19) 0.000 C2 0.021(2) 0.028(2) 0.0125(16) 0.0036(15) 0.0014(14) -0.0026(15) C3 0.0194(19) 0.026(2) 0.0129(16) 0.0042(15) -0.0014(14) 0.0027(15) C4 0.012(3) 0.039(3) 0.017(3) 0.000 -0.002(2) 0.000 N1 0.019(2) 0.060(3) 0.024(2) 0.000 0.0029(18) 0.000 C5 0.005(5) 0.018(5) 0.025(5) 0.000 0.003(4) 0.000 C6 0.019(7) 0.049(8) 0.045(8) 0.000 0.004(5) 0.000 O1W 0.019(2) 0.060(3) 0.024(2) 0.000 0.0029(18) 0.000 N2 0.034(6) 0.038(6) 0.038(6) 0.000 0.019(5) 0.000 C7 0.033(6) 0.019(5) 0.023(5) 0.000 0.005(5) 0.000 C8 0.047(13) 0.054(7) 0.030(17) 0.000 0.024(10) 0.000 _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 O1 2.205(3) . ? Dy1 O1 2.236(3) 5_657 ? Dy1 O2 2.352(2) 6 ? Dy1 O2 2.352(2) . ? Dy1 N1 2.459(4) . ? Dy1 Cl1 2.6604(12) . ? Dy1 Cl1 2.6604(12) 6 ? Dy1 Dy1 3.6556(9) 5_657 ? O1 C1 1.435(5) . ? O1 Yb1 2.236(3) 5_657 ? O1 Dy1 2.236(3) 5_657 ? O2 C3 1.463(4) . ? O2 H2O 0.8461 . ? C1 C2 1.527(4) 6 ? C1 C2 1.527(4) . ? C1 Yb1 3.208(5) 5_657 ? C1 H1 1.0000 . ? C2 C3 1.520(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.524(5) . ? C3 H3 1.0000 . ? C4 C3 1.524(5) 6 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N1 C5 1.176(10) . ? N1 H1WA 0.8573 . ? N1 H1WB 0.8440 . ? C5 C6 1.461(14) . ? C5 H1WA 1.1716 . ? C5 H1WB 1.2292 . ? C6 C6 1.84(2) 5_557 ? C6 H6A 0.9603 . ? C6 H6B 0.9596 . ? N2 C7 1.112(14) . ? C7 C8 1.481(19) . ? C7 C8 1.97(2) 5_558 ? C8 C8 0.50(3) 5_558 ? C8 C7 1.97(2) 5_558 ? C8 H8A 0.9587 . ? C8 H8B 0.9587 . ? 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 Dy1 O1 69.19(13) . 5_657 ? O1 Dy1 O2 77.19(9) . 6 ? O1 Dy1 O2 128.83(8) 5_657 6 ? O1 Dy1 O2 77.19(9) . . ? O1 Dy1 O2 128.83(8) 5_657 . ? O2 Dy1 O2 76.20(12) 6 . ? O1 Dy1 N1 143.70(13) . . ? O1 Dy1 N1 147.11(13) 5_657 . ? O2 Dy1 N1 74.43(10) 6 . ? O2 Dy1 N1 74.43(10) . . ? O1 Dy1 Cl1 119.37(4) . . ? O1 Dy1 Cl1 82.94(5) 5_657 . ? O2 Dy1 Cl1 148.14(7) 6 . ? O2 Dy1 Cl1 81.25(7) . . ? N1 Dy1 Cl1 78.05(6) . . ? O1 Dy1 Cl1 119.37(4) . 6 ? O1 Dy1 Cl1 82.94(5) 5_657 6 ? O2 Dy1 Cl1 81.25(7) 6 6 ? O2 Dy1 Cl1 148.14(7) . 6 ? N1 Dy1 Cl1 78.05(6) . 6 ? Cl1 Dy1 Cl1 108.48(6) . 6 ? O1 Dy1 Dy1 34.87(8) . 5_657 ? O1 Dy1 Dy1 34.32(8) 5_657 5_657 ? O2 Dy1 Dy1 104.46(6) 6 5_657 ? O2 Dy1 Dy1 104.46(6) . 5_657 ? N1 Dy1 Dy1 178.57(10) . 5_657 ? Cl1 Dy1 Dy1 102.75(3) . 5_657 ? Cl1 Dy1 Dy1 102.75(3) 6 5_657 ? C1 O1 Dy1 128.9(3) . . ? C1 O1 Yb1 120.3(3) . 5_657 ? Dy1 O1 Yb1 110.81(13) . 5_657 ? C1 O1 Dy1 120.3(3) . 5_657 ? Dy1 O1 Dy1 110.81(13) . 5_657 ? Yb1 O1 Dy1 0.000(11) 5_657 5_657 ? C3 O2 Dy1 125.8(2) . . ? C3 O2 H2O 93.7 . . ? Dy1 O2 H2O 125.8 . . ? O1 C1 C2 110.5(2) . 6 ? O1 C1 C2 110.5(2) . . ? C2 C1 C2 111.7(4) 6 . ? O1 C1 Yb1 37.00(18) . 5_657 ? C2 C1 Yb1 122.9(2) 6 5_657 ? C2 C1 Yb1 122.9(2) . 5_657 ? O1 C1 H1 108.0 . . ? C2 C1 H1 108.0 6 . ? C2 C1 H1 108.0 . . ? Yb1 C1 H1 71.0 5_657 . ? C3 C2 C1 113.0(3) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O2 C3 C2 108.0(3) . . ? O2 C3 C4 110.8(3) . . ? C2 C3 C4 112.0(3) . . ? O2 C3 H3 108.7 . . ? C2 C3 H3 108.7 . . ? C4 C3 H3 108.7 . . ? C3 C4 C3 113.5(4) . 6 ? C3 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 6 . ? C3 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 6 . ? H4A C4 H4B 107.7 . . ? C5 N1 Dy1 176.8(6) . . ? C5 N1 H1WA 68.3 . . ? Dy1 N1 H1WA 109.9 . . ? C5 N1 H1WB 72.9 . . ? Dy1 N1 H1WB 110.3 . . ? H1WA N1 H1WB 112.1 . . ? N1 C5 C6 172.3(11) . . ? N1 C5 H1WA 42.8 . . ? C6 C5 H1WA 132.6 . . ? N1 C5 H1WB 41.0 . . ? C6 C5 H1WB 146.7 . . ? H1WA C5 H1WB 71.9 . . ? C5 C6 C6 161.7(14) . 5_557 ? C5 C6 H6A 109.8 . . ? C6 C6 H6A 88.5 5_557 . ? C5 C6 H6B 109.1 . . ? C6 C6 H6B 62.6 5_557 . ? H6A C6 H6B 109.5 . . ? N2 C7 C8 178.5(19) . . ? N2 C7 C8 174.6(16) . 5_558 ? C8 C7 C8 4(3) . 5_558 ? C8 C8 C7 165(10) 5_558 . ? C8 C8 C7 11(8) 5_558 5_558 ? C7 C8 C7 176(3) . 5_558 ? C8 C8 H8A 93.4 5_558 . ? C7 C8 H8A 95.9 . . ? C7 C8 H8A 86.4 5_558 . ? C8 C8 H8B 44.3 5_558 . ? C7 C8 H8B 120.6 . . ? C7 C8 H8B 55.6 5_558 . ? H8A C8 H8B 118.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O Cl1 0.85 2.25 3.093(3) 179.3 7_557 O1W H1WB N2 0.84 2.12 2.825(11) 140.6 . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.909 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.134 data_2 _database_code_depnum_ccdc_archive 'CCDC 899842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H30 Cl4 Dy2 N2 O7' _chemical_formula_weight 829.22 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.546(2) _cell_length_b 9.2831(14) _cell_length_c 8.8893(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.267(2) _cell_angle_gamma 90.00 _cell_volume 1272.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 6.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.568 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3062 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.00 _reflns_number_total 1436 _reflns_number_gt 1360 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0226P)^2^+0.1132P] 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 1436 _refine_ls_number_parameters 97 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.061 _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 0.384300(11) 0.0000 1.02738(2) 0.01432(8) Uani 1 2 d S . . Cl1 Cl 0.37112(6) 0.23553(12) 1.19782(10) 0.0384(3) Uani 1 1 d . A . O1 O 0.47780(17) 0.0000 0.8575(3) 0.0134(6) Uani 1 2 d S . . O2 O 0.31843(13) 0.1567(2) 0.8344(2) 0.0177(5) Uani 1 1 d . A . H2O H 0.2663 0.1865 0.8257 0.021 Uiso 1 1 d R . . C1 C 0.4611(3) 0.0000 0.6948(5) 0.0174(10) Uani 1 2 d S . . H1 H 0.5182 0.0000 0.6543 0.021 Uiso 1 2 calc SR A . C2 C 0.4126(2) 0.1361(4) 0.6382(3) 0.0195(7) Uani 1 1 d . A . H2A H 0.4430 0.2210 0.6869 0.023 Uiso 1 1 calc R . . H2B H 0.4134 0.1446 0.5274 0.023 Uiso 1 1 calc R . . C3 C 0.3191(2) 0.1372(4) 0.6714(3) 0.0178(7) Uani 1 1 d . . . H3 H 0.2889 0.2212 0.6176 0.021 Uiso 1 1 calc R A . C4 C 0.2707(3) 0.0000 0.6165(5) 0.0199(10) Uani 1 2 d S . . H4A H 0.2614 0.0000 0.5043 0.024 Uiso 1 2 calc SR . . H4B H 0.2131 0.0000 0.6528 0.024 Uiso 1 2 calc SR . . N1 N 0.2270(2) 0.0000 1.0553(4) 0.0315(10) Uani 0.50 2 d SP A 1 C5 C 0.1524(5) 0.0000 1.0612(8) 0.0076(15) Uani 0.50 2 d SPU A 1 C6 C 0.0564(6) 0.0000 1.0462(13) 0.038(3) Uani 0.50 2 d SP . 1 H6A H 0.0373 0.0000 1.1448 0.056 Uiso 0.50 2 d SPR . 1 H6B H 0.0348 0.0844 0.9916 0.056 Uiso 0.50 1 d PR . 1 O1W O 0.2270(2) 0.0000 1.0553(4) 0.0315(10) Uani 0.50 2 d SP A 2 H1WA H 0.2020 -0.0719 1.0086 0.038 Uiso 0.25 1 d PR A 2 H1WB H 0.2201 0.0000 1.1490 0.038 Uiso 0.50 2 d SPR A 2 N2 N 0.1215(6) 0.0000 1.2872(10) 0.032(2) Uani 0.50 2 d SP . . C7 C 0.0709(6) 0.0000 1.3712(11) 0.025(2) Uani 0.50 2 d SP . . C8 C 0.0077(19) 0.0000 1.480(3) 0.046(5) Uani 0.50 2 d SPU . . H8A H -0.0251 -0.0813 1.4372 0.069 Uiso 0.50 1 d PR . . H8B H 0.0269 0.0000 1.5866 0.069 Uiso 0.50 2 d SPR . . 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 0.00962(12) 0.02047(14) 0.01289(12) 0.000 0.00145(7) 0.000 Cl1 0.0246(4) 0.0557(7) 0.0315(5) -0.0245(4) -0.0101(4) 0.0225(4) O1 0.0118(14) 0.0169(17) 0.0115(13) 0.000 0.0012(11) 0.000 O2 0.0147(10) 0.0236(13) 0.0146(10) -0.0014(9) 0.0016(8) 0.0052(9) C1 0.013(2) 0.026(3) 0.013(2) 0.000 0.0009(16) 0.000 C2 0.0219(17) 0.0231(19) 0.0132(14) 0.0045(13) 0.0009(12) -0.0036(14) C3 0.0189(16) 0.0213(18) 0.0127(14) 0.0036(12) 0.0000(11) 0.0016(13) C4 0.012(2) 0.031(3) 0.016(2) 0.000 0.0003(16) 0.000 N1 0.0178(19) 0.052(3) 0.0238(19) 0.000 -0.0001(15) 0.000 C5 0.0071(17) 0.0078(17) 0.0080(17) 0.000 0.0017(10) 0.000 C6 0.015(5) 0.050(8) 0.048(7) 0.000 0.007(4) 0.000 O1W 0.0178(19) 0.052(3) 0.0238(19) 0.000 -0.0001(15) 0.000 N2 0.030(5) 0.029(5) 0.036(5) 0.000 0.004(4) 0.000 C7 0.025(5) 0.021(6) 0.029(5) 0.000 0.001(4) 0.000 C8 0.042(8) 0.047(6) 0.051(10) 0.000 0.010(7) 0.000 _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 O1 2.225(3) . ? Dy1 O1 2.256(3) 5_657 ? Dy1 O2 2.380(2) 6 ? Dy1 O2 2.380(2) . ? Dy1 N1 2.489(4) . ? Dy1 Cl1 2.6826(10) . ? Dy1 Cl1 2.6826(10) 6 ? Dy1 Dy1 3.6907(7) 5_657 ? O1 C1 1.436(5) . ? O1 Dy1 2.256(3) 5_657 ? O2 C3 1.462(4) . ? O2 H2O 0.8501 . ? C1 C2 1.524(4) 6 ? C1 C2 1.524(4) . ? C1 H1 1.0000 . ? C2 C3 1.519(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.527(4) . ? C3 H3 1.0000 . ? C4 C3 1.527(4) 6 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N1 C5 1.168(8) . ? N1 H1WA 0.8534 . ? N1 H1WB 0.8526 . ? C5 C6 1.482(12) . ? C5 H1WA 1.1615 . ? C5 H1WB 1.2286 . ? C6 C6 1.839(18) 5_557 ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? N2 C7 1.150(13) . ? C7 C8 1.46(3) . ? C7 C8 1.91(3) 5_558 ? C8 C8 0.46(4) 5_558 ? C8 C7 1.91(3) 5_558 ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? 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 Dy1 O1 69.08(11) . 5_657 ? O1 Dy1 O2 76.65(7) . 6 ? O1 Dy1 O2 128.65(7) 5_657 6 ? O1 Dy1 O2 76.65(7) . . ? O1 Dy1 O2 128.65(7) 5_657 . ? O2 Dy1 O2 75.38(10) 6 . ? O1 Dy1 N1 143.36(11) . . ? O1 Dy1 N1 147.57(11) 5_657 . ? O2 Dy1 N1 74.54(8) 6 . ? O2 Dy1 N1 74.54(8) . . ? O1 Dy1 Cl1 119.12(3) . . ? O1 Dy1 Cl1 83.10(4) 5_657 . ? O2 Dy1 Cl1 148.07(5) 6 . ? O2 Dy1 Cl1 81.50(6) . . ? N1 Dy1 Cl1 78.31(5) . . ? O1 Dy1 Cl1 119.12(3) . 6 ? O1 Dy1 Cl1 83.10(4) 5_657 6 ? O2 Dy1 Cl1 81.50(6) 6 6 ? O2 Dy1 Cl1 148.07(5) . 6 ? N1 Dy1 Cl1 78.31(5) . 6 ? Cl1 Dy1 Cl1 109.18(5) . 6 ? O1 Dy1 Dy1 34.81(6) . 5_657 ? O1 Dy1 Dy1 34.27(7) 5_657 5_657 ? O2 Dy1 Dy1 104.04(5) 6 5_657 ? O2 Dy1 Dy1 104.04(5) . 5_657 ? N1 Dy1 Dy1 178.17(8) . 5_657 ? Cl1 Dy1 Dy1 102.70(2) . 5_657 ? Cl1 Dy1 Dy1 102.70(2) 6 5_657 ? C1 O1 Dy1 129.3(2) . . ? C1 O1 Dy1 119.8(2) . 5_657 ? Dy1 O1 Dy1 110.92(11) . 5_657 ? C3 O2 Dy1 125.63(18) . . ? C3 O2 H2O 94.4 . . ? Dy1 O2 H2O 125.6 . . ? O1 C1 C2 110.6(2) . 6 ? O1 C1 C2 110.6(2) . . ? C2 C1 C2 112.0(3) 6 . ? O1 C1 H1 107.8 . . ? C2 C1 H1 107.8 6 . ? C2 C1 H1 107.8 . . ? C3 C2 C1 112.8(3) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O2 C3 C2 108.7(2) . . ? O2 C3 C4 110.8(3) . . ? C2 C3 C4 112.1(3) . . ? O2 C3 H3 108.4 . . ? C2 C3 H3 108.4 . . ? C4 C3 H3 108.4 . . ? C3 C4 C3 113.0(3) . 6 ? C3 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 6 . ? C3 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 6 . ? H4A C4 H4B 107.8 . . ? C5 N1 Dy1 176.8(4) . . ? C5 N1 H1WA 68.1 . . ? Dy1 N1 H1WA 110.2 . . ? C5 N1 H1WB 73.0 . . ? Dy1 N1 H1WB 110.1 . . ? H1WA N1 H1WB 111.7 . . ? N1 C5 C6 172.4(8) . . ? N1 C5 H1WA 43.0 . . ? C6 C5 H1WA 132.6 . . ? N1 C5 H1WB 41.6 . . ? C6 C5 H1WB 146.1 . . ? H1WA C5 H1WB 72.3 . . ? C5 C6 C6 158.8(13) . 5_557 ? C5 C6 H6A 110.0 . . ? C6 C6 H6A 91.2 5_557 . ? C5 C6 H6B 109.2 . . ? C6 C6 H6B 61.4 5_557 . ? H6A C6 H6B 109.5 . . ? N2 C7 C8 179.2(14) . . ? N2 C7 C8 176.7(12) . 5_558 ? C8 C7 C8 3(2) . 5_558 ? C8 C8 C7 169(9) 5_558 . ? C8 C8 C7 8(7) 5_558 5_558 ? C7 C8 C7 177(2) . 5_558 ? C8 C8 H8A 90.4 5_558 . ? C7 C8 H8A 96.2 . . ? C7 C8 H8A 85.4 5_558 . ? C8 C8 H8B 49.1 5_558 . ? C7 C8 H8B 120.1 . . ? C7 C8 H8B 57.3 5_558 . ? H8A C8 H8B 118.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O Cl1 0.85 2.24 3.091(2) 179.8 7_557 O1W H1WB N2 0.85 2.08 2.792(11) 140.3 . _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.919 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.124 data_3 _database_code_depnum_ccdc_archive 'CCDC 899843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H30 Cl4 N2 O7 Yb2' _chemical_formula_weight 850.30 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 15.378(3) _cell_length_b 9.2501(16) _cell_length_c 8.8674(16) _cell_angle_alpha 90.00 _cell_angle_beta 97.534(2) _cell_angle_gamma 90.00 _cell_volume 1250.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 7.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2878 _exptl_absorpt_correction_T_max 0.5056 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3500 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1301 _reflns_number_gt 1271 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0291P)^2^+2.2487P] 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 1301 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0196 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Yb1 Yb 0.384843(12) 0.0000 1.02364(2) 0.01431(9) Uani 1 2 d S . . Cl1 Cl 0.37122(7) 0.23132(13) 1.19367(12) 0.0403(3) Uani 1 1 d . A . O1 O 0.4784(2) 0.0000 0.8592(4) 0.0147(7) Uani 1 2 d S . . O2 O 0.31937(15) 0.1566(3) 0.8370(3) 0.0191(5) Uani 1 1 d . A . H2O H 0.2671 0.1864 0.8283 0.023 Uiso 1 1 d R . . C1 C 0.4617(3) 0.0000 0.6957(5) 0.0177(10) Uani 1 2 d S . . H1 H 0.5194 0.0000 0.6554 0.021 Uiso 1 2 calc SR A . C2 C 0.4124(2) 0.1357(4) 0.6391(4) 0.0203(7) Uani 1 1 d . A . H2A H 0.4434 0.2210 0.6874 0.024 Uiso 1 1 calc R . . H2B H 0.4128 0.1439 0.5278 0.024 Uiso 1 1 calc R . . C3 C 0.3181(2) 0.1376(4) 0.6725(4) 0.0191(7) Uani 1 1 d . . . H3 H 0.2873 0.2220 0.6191 0.023 Uiso 1 1 calc R A . C4 C 0.2694(3) 0.0000 0.6182(6) 0.0201(10) Uani 1 2 d S . . H4A H 0.2595 0.0000 0.5056 0.024 Uiso 1 2 calc SR . . H4B H 0.2113 0.0000 0.6549 0.024 Uiso 1 2 calc SR . . N1 N 0.2297(3) 0.0000 1.0508(5) 0.0310(10) Uani 0.50 2 d SP A 1 C5 C 0.1540(6) 0.0000 1.0526(12) 0.019(2) Uani 0.50 2 d SP A 1 C6 C 0.0576(7) 0.0000 1.0445(15) 0.035(3) Uani 0.50 2 d SP . 1 H6A H 0.0385 0.0000 1.1431 0.053 Uiso 0.50 2 d SPR . 1 H6B H 0.0360 0.0844 0.9898 0.053 Uiso 0.50 1 d PR . 1 O1W O 0.2297(3) 0.0000 1.0508(5) 0.0310(10) Uani 0.50 2 d SP A 2 H1WA H 0.2204 0.0000 1.1477 0.037 Uiso 0.50 2 d SPR A 2 H1WB H 0.2131 -0.0732 1.0042 0.037 Uiso 0.25 1 d PR A 2 N2 N 0.1223(7) 0.0000 1.2848(11) 0.029(2) Uani 0.50 2 d SP . . C7 C 0.0708(7) 0.0000 1.3666(12) 0.024(2) Uani 0.50 2 d SP . . C8 C 0.004(2) 0.0000 1.4718(19) 0.039(5) Uani 0.50 2 d SP . . H8A H -0.0284 -0.0813 1.4294 0.059 Uiso 0.50 1 d PR . . H8B H 0.0236 0.0000 1.5788 0.059 Uiso 0.50 2 d SPR . . 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 Yb1 0.01056(13) 0.02084(14) 0.01143(13) 0.000 0.00112(8) 0.000 Cl1 0.0262(5) 0.0588(7) 0.0320(5) -0.0260(5) -0.0104(4) 0.0231(5) O1 0.0126(16) 0.0186(16) 0.0120(16) 0.000 -0.0011(12) 0.000 O2 0.0143(11) 0.0251(13) 0.0176(12) -0.0021(10) 0.0004(9) 0.0058(10) C1 0.013(2) 0.031(3) 0.010(2) 0.000 0.0031(17) 0.000 C2 0.0187(17) 0.0282(19) 0.0137(17) 0.0036(14) 0.0010(13) -0.0032(15) C3 0.0182(17) 0.0236(18) 0.0142(17) 0.0051(14) -0.0027(13) 0.0008(14) C4 0.015(2) 0.030(3) 0.015(2) 0.000 -0.0003(18) 0.000 N1 0.014(2) 0.060(3) 0.018(2) 0.000 0.0013(16) 0.000 C5 0.013(5) 0.024(5) 0.022(5) 0.000 0.007(4) 0.000 C6 0.014(5) 0.046(7) 0.045(8) 0.000 0.003(5) 0.000 O1W 0.014(2) 0.060(3) 0.018(2) 0.000 0.0013(16) 0.000 N2 0.036(5) 0.026(5) 0.028(5) 0.000 0.006(4) 0.000 C7 0.028(6) 0.017(5) 0.026(6) 0.000 0.001(5) 0.000 C8 0.050(10) 0.048(7) 0.021(15) 0.000 0.005(12) 0.000 _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 Yb1 O1 2.178(3) . ? Yb1 O1 2.220(3) 5_657 ? Yb1 O2 2.327(2) 6 ? Yb1 O2 2.327(2) . ? Yb1 N1 2.429(4) . ? Yb1 Cl1 2.6416(11) . ? Yb1 Cl1 2.6416(11) 6 ? Yb1 C1 3.198(5) 5_657 ? Yb1 Yb1 3.6207(7) 5_657 ? Yb1 H1WB 2.7100 . ? O1 C1 1.439(5) . ? O1 Yb1 2.220(3) 5_657 ? O2 C3 1.466(4) . ? O2 H2O 0.8433 . ? C1 C2 1.518(4) 6 ? C1 C2 1.518(4) . ? C1 Yb1 3.198(5) 5_657 ? C1 H1 1.0000 . ? C2 C3 1.518(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(4) . ? C3 H3 1.0000 . ? C4 C3 1.522(4) 6 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N1 C5 1.167(11) . ? N1 H1WA 0.8896 . ? N1 H1WB 0.8163 . ? C5 C6 1.475(14) . ? C5 H1WA 1.2370 . ? C5 H1WB 1.2539 . ? C6 C6 1.84(2) 5_557 ? C6 H6A 0.9578 . ? C6 H6B 0.9554 . ? N2 C7 1.143(15) . ? C7 C8 1.47(2) . ? C7 C8 1.95(2) 5_558 ? C8 C8 0.53(3) 5_558 ? C8 C7 1.95(2) 5_558 ? C8 H8A 0.9541 . ? C8 H8B 0.9558 . ? 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 Yb1 O1 69.19(13) . 5_657 ? O1 Yb1 O2 77.64(9) . 6 ? O1 Yb1 O2 128.89(8) 5_657 6 ? O1 Yb1 O2 77.64(9) . . ? O1 Yb1 O2 128.89(8) 5_657 . ? O2 Yb1 O2 76.98(12) 6 . ? O1 Yb1 N1 144.07(13) . . ? O1 Yb1 N1 146.74(12) 5_657 . ? O2 Yb1 N1 74.43(9) 6 . ? O2 Yb1 N1 74.43(9) . . ? O1 Yb1 Cl1 119.39(4) . . ? O1 Yb1 Cl1 82.77(5) 5_657 . ? O2 Yb1 Cl1 148.31(6) 6 . ? O2 Yb1 Cl1 80.94(6) . . ? N1 Yb1 Cl1 77.94(6) . . ? O1 Yb1 Cl1 119.39(4) . 6 ? O1 Yb1 Cl1 82.77(5) 5_657 6 ? O2 Yb1 Cl1 80.94(6) 6 6 ? O2 Yb1 Cl1 148.31(6) . 6 ? N1 Yb1 Cl1 77.94(6) . 6 ? Cl1 Yb1 Cl1 108.19(6) . 6 ? O1 Yb1 C1 92.06(12) . 5_657 ? O1 Yb1 C1 22.87(12) 5_657 5_657 ? O2 Yb1 C1 139.47(7) 6 5_657 ? O2 Yb1 C1 139.47(7) . 5_657 ? N1 Yb1 C1 123.87(13) . 5_657 ? Cl1 Yb1 C1 70.21(5) . 5_657 ? Cl1 Yb1 C1 70.21(5) 6 5_657 ? O1 Yb1 Yb1 34.97(8) . 5_657 ? O1 Yb1 Yb1 34.22(8) 5_657 5_657 ? O2 Yb1 Yb1 104.84(6) 6 5_657 ? O2 Yb1 Yb1 104.84(6) . 5_657 ? N1 Yb1 Yb1 179.04(10) . 5_657 ? Cl1 Yb1 Yb1 102.60(2) . 5_657 ? Cl1 Yb1 Yb1 102.60(2) 6 5_657 ? C1 Yb1 Yb1 57.09(8) 5_657 5_657 ? O1 Yb1 H1WB 132.9 . . ? O1 Yb1 H1WB 152.3 5_657 . ? O2 Yb1 H1WB 58.1 6 . ? O2 Yb1 H1WB 77.5 . . ? N1 Yb1 H1WB 17.2 . . ? Cl1 Yb1 H1WB 95.1 . . ? Cl1 Yb1 H1WB 71.6 6 . ? C1 Yb1 H1WB 131.6 5_657 . ? Yb1 Yb1 H1WB 162.3 5_657 . ? C1 O1 Yb1 128.9(3) . . ? C1 O1 Yb1 120.3(3) . 5_657 ? Yb1 O1 Yb1 110.81(13) . 5_657 ? C3 O2 Yb1 125.5(2) . . ? C3 O2 H2O 93.4 . . ? Yb1 O2 H2O 125.9 . . ? O1 C1 C2 110.4(2) . 6 ? O1 C1 C2 110.4(2) . . ? C2 C1 C2 111.6(4) 6 . ? O1 C1 Yb1 36.83(18) . 5_657 ? C2 C1 Yb1 122.9(2) 6 5_657 ? C2 C1 Yb1 122.9(2) . 5_657 ? O1 C1 H1 108.1 . . ? C2 C1 H1 108.1 6 . ? C2 C1 H1 108.1 . . ? Yb1 C1 H1 71.2 5_657 . ? C3 C2 C1 113.2(3) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.8 . . ? O2 C3 C2 107.9(3) . . ? O2 C3 C4 110.9(3) . . ? C2 C3 C4 111.8(3) . . ? O2 C3 H3 108.7 . . ? C2 C3 H3 108.7 . . ? C4 C3 H3 108.7 . . ? C3 C4 C3 113.5(4) . 6 ? C3 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 6 . ? C3 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 6 . ? H4A C4 H4B 107.7 . . ? C5 N1 Yb1 175.2(6) . . ? C5 N1 H1WA 72.5 . . ? Yb1 N1 H1WA 112.3 . . ? C5 N1 H1WB 76.1 . . ? Yb1 N1 H1WB 101.3 . . ? H1WA N1 H1WB 114.2 . . ? N1 C5 C6 176.4(11) . . ? N1 C5 H1WA 43.3 . . ? C6 C5 H1WA 140.3 . . ? N1 C5 H1WB 39.2 . . ? C6 C5 H1WB 138.8 . . ? H1WA C5 H1WB 70.2 . . ? C5 C6 C6 157.6(14) . 5_557 ? C5 C6 H6A 112.4 . . ? C6 C6 H6A 89.9 5_557 . ? C5 C6 H6B 107.8 . . ? C6 C6 H6B 62.1 5_557 . ? H6A C6 H6B 109.6 . . ? N2 C7 C8 179.9(16) . . ? N2 C7 C8 172.4(14) . 5_558 ? C8 C7 C8 8(2) . 5_558 ? C8 C8 C7 151(9) 5_558 . ? C8 C8 C7 22(7) 5_558 5_558 ? C7 C8 C7 172(2) . 5_558 ? C8 C8 H8A 100.8 5_558 . ? C7 C8 H8A 97.2 . . ? C7 C8 H8A 87.5 5_558 . ? C8 C8 H8B 32.1 5_558 . ? C7 C8 H8B 118.6 . . ? C7 C8 H8B 53.7 5_558 . ? H8A C8 H8B 118.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O Cl1 0.84 2.24 3.087(3) 179.3 7_557 O1W H1WA N2 0.89 2.06 2.817(11) 142.5 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.748 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.129 #_eof #End of Crystallographic Information File