####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_cr4dy4s _audit_block_doi 10.5517/cct4pvg _database_code_depnum_ccdc_archive 'CCDC 749296' loop_ _citation_id _citation_doi _citation_year 1 10.1002/anie.201002690 2010 _audit_update_record ; 2009-09-28 deposited with the CCDC. 2018-08-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H120 Cr4 Dy4 N16 O28, 3(C H2 Cl2)' _chemical_formula_sum 'C63 H126 Cl6 Cr4 Dy4 N16 O28' _chemical_formula_weight 2626.50 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' Cr Cr 0.3209 0.6236 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 2 m' _symmetry_space_group_name_Hall 'I -4 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 19.3300(8) _cell_length_b 19.3300(8) _cell_length_c 13.6488(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5099.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16820 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.10 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2604 _exptl_absorpt_coefficient_mu 3.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.443 _exptl_absorpt_correction_T_max 0.513 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17801 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0107 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 28.15 _reflns_number_total 3088 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The methylene groups of the Me-dea ligands are disordered by a 27 degree rotation about the Dy-N bond, with the two components related by the crystallographic mirror plane, and the atoms were refined with half-occupancy. The t-butyl group of the pivalate ligand was two-fold disordered, with relative occupancies 55:45. The partial carbon atoms could be refined anisotropically with appropriate (DELU) restraints. The lattice dichloromethane molecules were badly disordered, and the data were treated using the SQUEEZE option within PLATON. Electron density corresponding to 276 e was corrected for - calculated for six CH2Cl2 molecules (three per aggregate) = 288 e. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 148 60 ' ' 2 0.000 0.500 0.000 90 39 ' ' 3 0.500 0.000 0.000 90 39 ' ' 4 0.500 0.500 0.500 148 59 ' ' 5 0.000 0.500 0.500 90 39 ' ' 6 0.500 0.000 0.500 90 39 ' ' _platon_squeeze_details ; Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; _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^)+(0.0279P)^2^+8.5180P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1290 Friedel pairs' _refine_ls_abs_structure_Flack -0.027(11) _refine_ls_number_reflns 3088 _refine_ls_number_parameters 194 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0179 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0457 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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 0.5000 0.352436(6) 1.0000 0.01423(5) Uani 1 2 d S . . Cr1 Cr 0.343745(19) 0.343745(19) 1.10256(4) 0.01627(11) Uani 1 2 d S A . O1 O 0.41569(11) 0.41569(11) 1.0939(2) 0.0160(5) Uani 1 2 d SD . . H1 H 0.4335(16) 0.4335(16) 1.136(3) 0.019 Uiso 1 2 d SD . . N1 N 0.26861(11) 0.26861(11) 1.0745(3) 0.0257(7) Uani 1 2 d S . . C1 C 0.3146(3) 0.2065(3) 1.0363(6) 0.0271(14) Uani 0.50 1 d P A -1 H1A H 0.3367 0.1831 1.0928 0.033 Uiso 0.50 1 calc PR A -1 H1B H 0.2849 0.1724 1.0024 0.033 Uiso 0.50 1 calc PR A -1 C2 C 0.3692(4) 0.2315(4) 0.9678(6) 0.0272(15) Uani 0.50 1 d P A -1 H2A H 0.4063 0.1965 0.9618 0.033 Uiso 0.50 1 calc PR A -1 H2B H 0.3490 0.2393 0.9020 0.033 Uiso 0.50 1 calc PR A -1 O2 O 0.39650(8) 0.29356(8) 1.00445(17) 0.0190(3) Uani 1 1 d . . . C3 C 0.2239(3) 0.2934(3) 0.9997(9) 0.0367(15) Uani 0.50 1 d P A -1 H3A H 0.1806 0.3106 1.0297 0.044 Uiso 0.50 1 calc PR A -1 H3B H 0.2118 0.2548 0.9551 0.044 Uiso 0.50 1 calc PR A -1 C4 C 0.2578(4) 0.3523(4) 0.9399(6) 0.0312(15) Uani 0.50 1 d P A -1 H4A H 0.2904 0.3326 0.8913 0.037 Uiso 0.50 1 calc PR A -1 H4B H 0.2218 0.3786 0.9042 0.037 Uiso 0.50 1 calc PR A -1 C5 C 0.23667(17) 0.23667(17) 1.1609(4) 0.0416(11) Uani 1 2 d S A . H5A H 0.2026 0.2022 1.1398 0.062 Uiso 1 2 calc SR . . H5B H 0.2136 0.2724 1.2000 0.062 Uiso 0.50 1 calc PR . . H5C H 0.2725 0.2141 1.2005 0.062 Uiso 0.50 1 calc PR . . N2 N 0.43002(11) 0.43002(11) 0.8940(3) 0.0186(7) Uani 1 2 d S . . N3 N 0.4153(3) 0.4153(3) 0.8112(3) 0.0652(18) Uani 1 2 d S A . N4 N 0.3966(4) 0.3966(4) 0.7332(5) 0.115(4) Uani 1 2 d S . . O3 O 0.39029(10) 0.28889(10) 1.20642(14) 0.0231(4) Uani 1 1 d . . . O4 O 0.49866(13) 0.29033(8) 1.14926(11) 0.0221(3) Uani 1 1 d . . . C6 C 0.45314(15) 0.27130(15) 1.2084(2) 0.0256(5) Uani 1 1 d U A . C7A C 0.4754(3) 0.2111(4) 1.2771(5) 0.0265(13) Uani 0.55 1 d PU A 2 C8A C 0.5479(9) 0.2242(10) 1.3199(10) 0.028(2) Uani 0.55 1 d PU A 2 H8A1 H 0.5813 0.2288 1.2664 0.042 Uiso 0.55 1 calc PR A 2 H8A2 H 0.5611 0.1853 1.3619 0.042 Uiso 0.55 1 calc PR A 2 H8A3 H 0.5473 0.2669 1.3586 0.042 Uiso 0.55 1 calc PR A 2 C9A C 0.4236(5) 0.2042(5) 1.3587(6) 0.045(2) Uani 0.55 1 d PU A 2 H9A1 H 0.3780 0.1937 1.3311 0.068 Uiso 0.55 1 calc PR A 2 H9A2 H 0.4214 0.2477 1.3954 0.068 Uiso 0.55 1 calc PR A 2 H9A3 H 0.4378 0.1667 1.4026 0.068 Uiso 0.55 1 calc PR A 2 C10A C 0.4774(3) 0.1427(3) 1.2141(6) 0.0421(14) Uani 0.55 1 d PU A 2 H10A H 0.5106 0.1481 1.1604 0.063 Uiso 0.55 1 calc PR A 2 H10B H 0.4313 0.1336 1.1871 0.063 Uiso 0.55 1 calc PR A 2 H10C H 0.4915 0.1038 1.2557 0.063 Uiso 0.55 1 calc PR A 2 C7B C 0.4726(5) 0.2388(6) 1.3108(7) 0.037(2) Uani 0.45 1 d PU A 3 C8B C 0.4256(6) 0.1749(6) 1.3235(8) 0.045(2) Uani 0.45 1 d PU A 3 H8B1 H 0.4337 0.1425 1.2694 0.067 Uiso 0.45 1 calc PR A 3 H8B2 H 0.3770 0.1895 1.3233 0.067 Uiso 0.45 1 calc PR A 3 H8B3 H 0.4363 0.1522 1.3858 0.067 Uiso 0.45 1 calc PR A 3 C9B C 0.4620(5) 0.2885(6) 1.3941(6) 0.056(2) Uani 0.45 1 d PU A 3 H9B1 H 0.4923 0.3286 1.3854 0.084 Uiso 0.45 1 calc PR A 3 H9B2 H 0.4732 0.2654 1.4560 0.084 Uiso 0.45 1 calc PR A 3 H9B3 H 0.4137 0.3037 1.3952 0.084 Uiso 0.45 1 calc PR A 3 C10B C 0.5475(13) 0.2120(16) 1.2960(15) 0.054(5) Uani 0.45 1 d PU A 3 H10D H 0.5486 0.1799 1.2405 0.081 Uiso 0.45 1 calc PR A 3 H10E H 0.5628 0.1880 1.3554 0.081 Uiso 0.45 1 calc PR A 3 H10F H 0.5783 0.2512 1.2829 0.081 Uiso 0.45 1 calc PR A 3 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 0.01080(7) 0.01208(7) 0.01982(7) 0.000 0.00036(8) 0.000 Cr1 0.01206(14) 0.01206(14) 0.0247(2) 0.00193(15) 0.00193(15) -0.0003(2) O1 0.0140(7) 0.0140(7) 0.0200(13) -0.0008(8) -0.0008(8) -0.0012(10) N1 0.0161(9) 0.0161(9) 0.045(2) 0.0039(9) 0.0039(9) -0.0045(12) C1 0.019(3) 0.016(3) 0.046(4) -0.008(2) -0.005(3) -0.001(3) C2 0.017(3) 0.025(3) 0.040(4) -0.014(3) -0.006(2) 0.002(3) O2 0.0147(7) 0.0146(7) 0.0277(8) -0.0035(10) -0.0014(9) -0.0006(5) C3 0.025(3) 0.013(3) 0.072(5) 0.010(5) -0.019(5) -0.007(2) C4 0.035(4) 0.015(3) 0.043(4) 0.007(3) -0.021(3) -0.008(3) C5 0.0309(15) 0.0309(15) 0.063(3) 0.0113(15) 0.0113(15) -0.0102(19) N2 0.0176(11) 0.0176(11) 0.0205(16) 0.0008(9) 0.0008(9) 0.0015(13) N3 0.084(3) 0.084(3) 0.028(2) -0.011(2) -0.011(2) 0.068(3) N4 0.138(5) 0.138(5) 0.069(4) -0.060(4) -0.060(4) 0.092(6) O3 0.0189(9) 0.0224(9) 0.0280(9) 0.0086(8) 0.0023(7) 0.0015(7) O4 0.0161(7) 0.0235(8) 0.0266(7) 0.0079(6) 0.0002(10) 0.0002(10) C6 0.0225(13) 0.0243(13) 0.0300(14) 0.0098(11) 0.0000(11) -0.0041(11) C7A 0.020(2) 0.031(3) 0.029(3) 0.018(2) 0.000(2) 0.000(2) C8A 0.020(3) 0.051(5) 0.013(5) 0.013(3) -0.003(3) 0.008(3) C9A 0.030(3) 0.065(6) 0.040(4) 0.029(4) 0.009(3) 0.010(4) C10A 0.043(3) 0.022(3) 0.062(4) 0.010(2) -0.001(3) 0.006(2) C7B 0.030(4) 0.051(6) 0.029(4) 0.018(4) -0.002(3) -0.007(4) C8B 0.037(4) 0.046(6) 0.051(6) 0.033(4) 0.003(4) -0.001(4) C9B 0.063(5) 0.073(6) 0.032(4) 0.006(4) -0.007(4) -0.010(5) C10B 0.036(5) 0.095(17) 0.031(11) 0.032(8) 0.000(7) -0.002(7) _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 2.3024(15) 5_657 ? Dy1 O2 2.3025(15) . ? Dy1 O4 2.3648(15) . ? Dy1 O4 2.3648(15) 5_657 ? Dy1 O1 2.4072(17) 4_657 ? Dy1 O1 2.4072(17) . ? Dy1 N2 2.484(2) 4_657 ? Dy1 N2 2.484(2) . ? Cr1 O2 1.943(2) 8 ? Cr1 O2 1.943(2) . ? Cr1 O1 1.970(3) . ? Cr1 O3 1.9858(19) . ? Cr1 O3 1.9858(19) 8 ? Cr1 N1 2.089(3) . ? O1 Dy1 2.4071(17) 3_567 ? O1 H1 0.75(3) . ? N1 C3 1.421(9) . ? N1 C3 1.421(9) 8 ? N1 C5 1.468(6) . ? N1 C1 1.582(6) 8 ? N1 C1 1.582(6) . ? C1 C2 1.490(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.403(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O2 C4 1.409(7) 8 ? C3 C4 1.546(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O2 1.409(7) 8 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N2 N3 1.200(6) . ? N2 Dy1 2.484(2) 3_567 ? N3 N4 1.181(8) . ? O3 C6 1.262(4) . ? O4 C6 1.250(3) . ? C6 C7A 1.555(7) . ? C6 C7B 1.577(9) . ? C7A C9A 1.503(10) . ? C7A C8A 1.539(18) . ? C7A C10A 1.577(10) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C7B C9B 1.502(15) . ? C7B C8B 1.543(15) . ? C7B C10B 1.55(2) . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? 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 O2 120.75(8) 5_657 . ? O2 Dy1 O4 77.36(8) 5_657 . ? O2 Dy1 O4 73.55(8) . . ? O2 Dy1 O4 73.55(8) 5_657 5_657 ? O2 Dy1 O4 77.36(8) . 5_657 ? O4 Dy1 O4 118.98(8) . 5_657 ? O2 Dy1 O1 69.44(8) 5_657 4_657 ? O2 Dy1 O1 148.58(9) . 4_657 ? O4 Dy1 O1 136.39(9) . 4_657 ? O4 Dy1 O1 77.97(8) 5_657 4_657 ? O2 Dy1 O1 148.58(9) 5_657 . ? O2 Dy1 O1 69.44(8) . . ? O4 Dy1 O1 77.97(8) . . ? O4 Dy1 O1 136.39(9) 5_657 . ? O1 Dy1 O1 118.95(14) 4_657 . ? O2 Dy1 N2 80.83(8) 5_657 4_657 ? O2 Dy1 N2 139.13(9) . 4_657 ? O4 Dy1 N2 79.10(9) . 4_657 ? O4 Dy1 N2 143.33(9) 5_657 4_657 ? O1 Dy1 N2 68.58(8) 4_657 4_657 ? O1 Dy1 N2 75.64(11) . 4_657 ? O2 Dy1 N2 139.13(9) 5_657 . ? O2 Dy1 N2 80.83(8) . . ? O4 Dy1 N2 143.33(9) . . ? O4 Dy1 N2 79.10(9) 5_657 . ? O1 Dy1 N2 75.64(11) 4_657 . ? O1 Dy1 N2 68.58(8) . . ? N2 Dy1 N2 105.73(15) 4_657 . ? O2 Cr1 O2 92.82(12) 8 . ? O2 Cr1 O1 86.60(8) 8 . ? O2 Cr1 O1 86.60(8) . . ? O2 Cr1 O3 176.95(8) 8 . ? O2 Cr1 O3 89.29(8) . . ? O1 Cr1 O3 95.73(9) . . ? O2 Cr1 O3 89.29(8) 8 8 ? O2 Cr1 O3 176.95(8) . 8 ? O1 Cr1 O3 95.73(9) . 8 ? O3 Cr1 O3 88.52(11) . 8 ? O2 Cr1 N1 83.76(8) 8 . ? O2 Cr1 N1 83.76(8) . . ? O1 Cr1 N1 166.00(14) . . ? O3 Cr1 N1 94.29(9) . . ? O3 Cr1 N1 94.29(9) 8 . ? Cr1 O1 Dy1 98.70(8) . 3_567 ? Cr1 O1 Dy1 98.70(8) . . ? Dy1 O1 Dy1 113.83(12) 3_567 . ? Cr1 O1 H1 127(4) . . ? Dy1 O1 H1 109.2(19) 3_567 . ? Dy1 O1 H1 109.2(19) . . ? C3 N1 C5 117.6(4) . . ? C3 N1 C5 117.6(4) 8 . ? C3 N1 C1 111.2(6) 8 8 ? C5 N1 C1 100.5(3) . 8 ? C3 N1 C1 111.2(6) . . ? C5 N1 C1 100.5(3) . . ? C3 N1 Cr1 108.7(3) . . ? C3 N1 Cr1 108.7(3) 8 . ? C5 N1 Cr1 115.9(3) . . ? C1 N1 Cr1 101.4(3) 8 . ? C1 N1 Cr1 101.4(3) . . ? C2 C1 N1 111.0(5) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? O2 C2 C1 108.6(5) . . ? O2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C2 O2 Cr1 118.4(3) . . ? C4 O2 Cr1 110.9(3) 8 . ? C2 O2 Dy1 137.8(3) . . ? C4 O2 Dy1 138.9(3) 8 . ? Cr1 O2 Dy1 103.15(7) . . ? N1 C3 C4 111.7(5) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? O2 C4 C3 108.9(6) 8 . ? O2 C4 H4A 109.9 8 . ? C3 C4 H4A 109.9 . . ? O2 C4 H4B 109.9 8 . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 N2 Dy1 122.32(13) . 3_567 ? N3 N2 Dy1 122.32(13) . . ? Dy1 N2 Dy1 108.57(16) 3_567 . ? N4 N3 N2 173.8(9) . . ? C6 O3 Cr1 126.55(17) . . ? C6 O4 Dy1 135.5(2) . . ? O4 C6 O3 125.8(3) . . ? O4 C6 C7A 114.5(3) . . ? O3 C6 C7A 118.7(3) . . ? O4 C6 C7B 121.5(4) . . ? O3 C6 C7B 110.8(4) . . ? C9A C7A C8A 109.8(8) . . ? C9A C7A C6 109.2(6) . . ? C8A C7A C6 110.9(9) . . ? C9A C7A C10A 110.2(7) . . ? C8A C7A C10A 108.9(7) . . ? C6 C7A C10A 107.8(5) . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C7A C10A H10A 109.5 . . ? C7A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C7A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C9B C7B C8B 110.3(8) . . ? C9B C7B C10B 116.0(11) . . ? C8B C7B C10B 107.3(15) . . ? C9B C7B C6 112.6(8) . . ? C8B C7B C6 106.2(7) . . ? C10B C7B C6 103.9(11) . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7B C9B H9B1 109.5 . . ? C7B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.739 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.076