# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_g #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cd N2 O6' _chemical_formula_weight 392.65 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' Cd Cd -0.8075 1.2024 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_HALL '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.860(2) _cell_length_b 13.113(3) _cell_length_c 11.650(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.99(3) _cell_angle_gamma 90.00 _cell_volume 1473.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3383 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14099 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3383 _reflns_number_gt 3076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^2^+115.8665P] 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_number_reflns 3365 _refine_ls_number_parameters 190 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.1022 _refine_ls_wR_factor_ref 0.2771 _refine_ls_wR_factor_gt 0.2763 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _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 Cd1 Cd 0.74328(10) 0.49531(7) 0.50598(8) 0.0221(3) Uani 1 1 d . . . O1 O 0.5837(11) 0.3795(8) 0.4126(10) 0.035(2) Uani 1 1 d . . . O2 O 0.3808(12) 0.4562(8) 0.3527(10) 0.034(2) Uani 1 1 d . . . O3 O 0.9036(11) 0.6078(8) 0.6058(10) 0.035(2) Uani 1 1 d . . . O4 O 0.8821(11) 0.4536(8) 0.3728(9) 0.031(2) Uani 1 1 d . . . N1 N 0.3317(12) 0.1324(9) 0.1216(10) 0.026(2) Uani 1 1 d U . . N2 N 0.8254(12) 0.3577(9) 0.6213(10) 0.026(2) Uani 1 1 d U . . C1 C 0.4184(13) 0.2960(11) 0.2712(12) 0.023(3) Uani 1 1 d . . . C2 C 0.3537(18) 0.3117(12) 0.1538(14) 0.035(3) Uani 1 1 d . . . H2 H 0.3368 0.3775 0.1245 0.042 Uiso 1 1 calc R . . C3 C 0.3152(18) 0.2284(13) 0.0815(14) 0.037(4) Uani 1 1 d . . . H3 H 0.2766 0.2394 0.0026 0.045 Uiso 1 1 calc R . . C4 C 0.3934(18) 0.1163(12) 0.2323(14) 0.036(3) Uani 1 1 d . . . H4 H 0.4055 0.0495 0.2592 0.044 Uiso 1 1 calc R . . C5 C 0.4412(18) 0.1963(12) 0.3107(14) 0.037(4) Uani 1 1 d . . . H5 H 0.4872 0.1827 0.3873 0.045 Uiso 1 1 calc R . . C6 C 0.4633(13) 0.3848(10) 0.3537(11) 0.021(2) Uani 1 1 d U . . C7 C 0.9193(14) 0.1953(10) 0.7688(12) 0.023(3) Uani 1 1 d . . . C8 C 0.7790(17) 0.2155(15) 0.737(2) 0.055(6) Uani 1 1 d . . . H8 H 0.7142 0.1754 0.7638 0.066 Uiso 1 1 calc R . . C9 C 0.7390(17) 0.2984(16) 0.664(2) 0.056(6) Uani 1 1 d . . . H9 H 0.6448 0.3133 0.6431 0.067 Uiso 1 1 calc R . . C10 C 0.9603(16) 0.3317(12) 0.6454(15) 0.035(3) Uani 1 1 d . . . H10 H 1.0211 0.3672 0.6088 0.041 Uiso 1 1 calc R . . C11 C 1.0117(15) 0.2541(12) 0.7226(14) 0.033(3) Uani 1 1 d . . . H11 H 1.1065 0.2416 0.7430 0.039 Uiso 1 1 calc R . . C12 C 1.0304(14) 0.6092(10) 0.6471(11) 0.022(3) Uani 1 1 d U . . O1W O 0.915(7) 0.034(4) 0.471(8) 0.41(5) Uani 1 1 d . . . H12A H 0.8596 -0.0160 0.4676 0.613 Uiso 1 1 d R . . H12B H 0.8869 0.0734 0.4127 0.613 Uiso 1 1 d R . . O2W O 0.296(14) 0.993(6) 0.454(5) 0.58(9) Uani 1 1 d . . . H13A H 0.3373 1.0275 0.4102 0.868 Uiso 1 1 d R . . H13B H 0.3311 1.0064 0.5258 0.868 Uiso 1 1 d 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 Cd1 0.0241(5) 0.0173(5) 0.0230(5) -0.0019(4) 0.0006(3) 0.0034(4) O1 0.031(6) 0.031(6) 0.041(6) -0.010(5) -0.002(5) -0.003(4) O2 0.039(6) 0.029(5) 0.035(6) -0.009(4) 0.011(5) 0.003(5) O3 0.027(5) 0.032(6) 0.043(6) -0.011(5) 0.002(5) -0.006(4) O4 0.041(6) 0.025(5) 0.029(5) -0.007(4) 0.012(5) -0.002(4) N1 0.026(3) 0.026(3) 0.026(3) -0.0007(19) 0.0040(19) -0.0003(19) N2 0.026(3) 0.026(3) 0.027(3) 0.0019(19) 0.0046(19) -0.0005(19) C1 0.019(6) 0.026(7) 0.026(7) -0.005(5) 0.008(5) -0.004(5) C2 0.051(10) 0.021(7) 0.031(8) -0.003(6) 0.001(7) -0.004(7) C3 0.044(9) 0.035(8) 0.028(7) -0.002(6) -0.004(7) -0.005(7) C4 0.048(9) 0.025(7) 0.036(8) -0.003(6) 0.010(7) -0.006(7) C5 0.044(9) 0.028(8) 0.033(8) -0.003(6) -0.008(7) 0.002(7) C6 0.022(3) 0.021(3) 0.021(3) -0.0013(19) 0.0044(19) -0.0001(19) C7 0.023(6) 0.025(6) 0.024(6) 0.008(5) 0.009(5) 0.006(5) C8 0.024(8) 0.053(11) 0.084(15) 0.049(11) 0.004(8) 0.002(7) C9 0.020(7) 0.062(12) 0.082(14) 0.043(11) 0.002(8) 0.011(8) C10 0.026(7) 0.031(8) 0.048(9) 0.020(7) 0.009(6) 0.004(6) C11 0.020(6) 0.038(8) 0.042(9) 0.024(7) 0.011(6) 0.003(6) C12 0.022(3) 0.022(3) 0.021(3) -0.0011(19) 0.0043(19) -0.0004(19) O1W 0.41(11) 0.19(6) 0.54(13) -0.21(8) -0.10(9) 0.00(6) O2W 1.3(3) 0.30(7) 0.18(5) -0.07(5) 0.13(9) 0.32(14) _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 Cd1 O1 2.292(10) . ? Cd1 O3 2.294(10) . ? Cd1 N2 2.295(12) . ? Cd1 O2 2.334(10) 3_666 ? Cd1 O4 2.337(10) . ? Cd1 N1 2.352(12) 2_655 ? O1 C6 1.244(16) . ? O2 C6 1.239(17) . ? O2 Cd1 2.334(10) 3_666 ? O3 C12 1.242(17) . ? O4 C12 1.249(17) 3_766 ? N1 C4 1.32(2) . ? N1 C3 1.34(2) . ? N1 Cd1 2.352(12) 2_645 ? N2 C9 1.32(2) . ? N2 C10 1.344(18) . ? C1 C5 1.39(2) . ? C1 C2 1.40(2) . ? C1 C6 1.516(18) . ? C2 C3 1.38(2) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.41(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.38(2) . ? C7 C11 1.385(18) . ? C7 C12 1.510(18) 2_746 ? C8 C9 1.39(2) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.382(19) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O4 1.249(17) 3_766 ? C12 C7 1.510(18) 2_756 ? O1W H12A 0.8500 . ? O1W H12B 0.8500 . ? O2W H13A 0.8500 . ? O2W H13B 0.8500 . ? 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 Cd1 O3 177.9(4) . . ? O1 Cd1 N2 83.2(4) . . ? O3 Cd1 N2 95.0(4) . . ? O1 Cd1 O2 96.1(4) . 3_666 ? O3 Cd1 O2 82.8(4) . 3_666 ? N2 Cd1 O2 88.5(4) . 3_666 ? O1 Cd1 O4 88.2(4) . . ? O3 Cd1 O4 92.9(4) . . ? N2 Cd1 O4 91.2(4) . . ? O2 Cd1 O4 175.6(4) 3_666 . ? O1 Cd1 N1 96.4(4) . 2_655 ? O3 Cd1 N1 85.5(4) . 2_655 ? N2 Cd1 N1 176.0(4) . 2_655 ? O2 Cd1 N1 95.5(4) 3_666 2_655 ? O4 Cd1 N1 84.8(4) . 2_655 ? C6 O1 Cd1 135.0(10) . . ? C6 O2 Cd1 129.7(10) . 3_666 ? C12 O3 Cd1 137.5(10) . . ? C12 O4 Cd1 143.1(9) 3_766 . ? C4 N1 C3 119.1(13) . . ? C4 N1 Cd1 121.0(10) . 2_645 ? C3 N1 Cd1 119.9(10) . 2_645 ? C9 N2 C10 117.3(13) . . ? C9 N2 Cd1 120.3(10) . . ? C10 N2 Cd1 122.4(10) . . ? C5 C1 C2 118.1(13) . . ? C5 C1 C6 120.5(12) . . ? C2 C1 C6 121.4(13) . . ? C3 C2 C1 119.4(14) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? N1 C3 C2 122.1(14) . . ? N1 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? N1 C4 C5 122.6(15) . . ? N1 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C1 C5 C4 118.5(14) . . ? C1 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? O2 C6 O1 126.7(13) . . ? O2 C6 C1 118.0(12) . . ? O1 C6 C1 115.2(12) . . ? C8 C7 C11 119.5(13) . . ? C8 C7 C12 119.5(12) . 2_746 ? C11 C7 C12 121.0(12) . 2_746 ? C7 C8 C9 117.1(15) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? N2 C9 C8 124.5(15) . . ? N2 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? N2 C10 C11 122.4(14) . . ? N2 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C7 118.7(13) . . ? C10 C11 H11 120.6 . . ? C7 C11 H11 120.6 . . ? O3 C12 O4 126.6(13) . 3_766 ? O3 C12 C7 115.5(12) . 2_756 ? O4 C12 C7 117.8(12) 3_766 2_756 ? H12A O1W H12B 109.5 . . ? H13A O2W H13B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.668 _refine_diff_density_min -2.170 _refine_diff_density_rms 0.302 _database_code_depnum_ccdc_archive 'CCDC 923079' ####################################################################### # # 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_g _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Cd2 N4 O10 S' _chemical_formula_weight 711.29 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.390(2) _cell_length_b 12.295(3) _cell_length_c 12.497(3) _cell_angle_alpha 79.31(3) _cell_angle_beta 68.20(3) _cell_angle_gamma 69.58(3) _cell_volume 1386.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6360 _cell_measurement_theta_min 0.734 _cell_measurement_theta_max 0.847 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6360 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6360 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0640P)^2^+7.8705P] 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_number_reflns 6177 _refine_ls_number_parameters 320 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _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 Cd1 Cd 0.40038(6) 0.69632(5) 0.02158(5) 0.04101(18) Uani 1 1 d . . . Cd2 Cd 0.04869(6) 0.52707(5) 0.81438(5) 0.04087(18) Uani 1 1 d . . . S1 S 0.7352(2) 0.51493(18) 0.00492(18) 0.0423(4) Uani 1 1 d . . . O1 O 0.3835(7) 0.8766(5) 0.0645(7) 0.0628(17) Uani 1 1 d U . . O2 O 0.1907(7) 0.8679(6) 0.0407(7) 0.0634(17) Uani 1 1 d U . . O3 O 0.4960(11) 0.7465(9) -0.1730(7) 0.094(3) Uani 1 1 d U . . O4 O 0.8266(14) 0.5043(9) 0.0690(13) 0.157(6) Uani 1 1 d . . . O5 O 0.6687(10) 0.4221(7) 0.0423(6) 0.086(3) Uani 1 1 d . . . O6 O 0.8211(9) 0.5085(8) -0.1155(7) 0.107(4) Uani 1 1 d . . . O7 O 0.6297(7) 0.6289(6) 0.0268(6) 0.073(2) Uani 1 1 d U . . O8 O 0.0295(8) 0.5785(7) 0.6302(5) 0.0683(19) Uani 1 1 d U . . O9 O 0.2470(8) 0.5415(8) 0.6381(6) 0.079(2) Uani 1 1 d U . . O10 O 0.1225(8) 0.3320(6) 0.7950(7) 0.072(2) Uani 1 1 d . . . N1 N 0.3173(7) 0.6415(6) 0.2167(5) 0.0438(15) Uani 1 1 d . . . N2 N -0.0492(7) 0.7197(5) 0.8574(6) 0.0408(14) Uani 1 1 d . . . N3 N 0.5471(12) 0.7353(9) -0.3618(7) 0.077(3) Uani 1 1 d . . . N4 N 0.2845(8) 0.1524(7) 0.7843(7) 0.0545(18) Uani 1 1 d . . . C1 C 0.1595(11) 0.5689(9) 0.5841(7) 0.058(2) Uani 1 1 d . . . C2 C 0.2168(9) 0.5938(8) 0.4538(7) 0.049(2) Uani 1 1 d . . . C3 C 0.1221(10) 0.6251(9) 0.3900(7) 0.058(2) Uani 1 1 d . . . H3 H 0.0246 0.6293 0.4253 0.070 Uiso 1 1 calc R . . C4 C 0.1788(10) 0.6495(9) 0.2730(8) 0.055(2) Uani 1 1 d . . . H4 H 0.1155 0.6732 0.2307 0.066 Uiso 1 1 calc R . . C5 C 0.4074(10) 0.6106(9) 0.2796(8) 0.058(2) Uani 1 1 d . . . H5 H 0.5050 0.6052 0.2418 0.069 Uiso 1 1 calc R . . C6 C 0.3611(10) 0.5867(10) 0.3968(8) 0.063(3) Uani 1 1 d . . . H6 H 0.4261 0.5660 0.4374 0.075 Uiso 1 1 calc R . . C7 C 0.2585(9) 0.9220(7) 0.0632(8) 0.049(2) Uani 1 1 d . . . C8 C 0.1834(9) 1.0474(7) 0.0896(7) 0.0437(18) Uani 1 1 d . . . C9 C 0.0457(9) 1.1075(7) 0.0825(8) 0.051(2) Uani 1 1 d . . . H9 H -0.0044 1.0704 0.0611 0.061 Uiso 1 1 calc R . . C10 C 0.2503(10) 1.1086(8) 0.1236(9) 0.056(2) Uani 1 1 d . . . H10 H 0.3426 1.0718 0.1293 0.068 Uiso 1 1 calc R . . C11 C 0.0157(9) 0.7769(7) 0.8924(8) 0.0474(19) Uani 1 1 d . . . H11 H 0.1063 0.7367 0.9000 0.057 Uiso 1 1 calc R . . C12 C -0.1807(10) 0.7767(7) 0.8512(9) 0.055(2) Uani 1 1 d . . . H12 H -0.2280 0.7376 0.8288 0.066 Uiso 1 1 calc R . . C13 C 0.4843(19) 0.7256(13) -0.2484(13) 0.106(5) Uani 1 1 d U . . H13 H 0.4105 0.6918 -0.2283 0.127 Uiso 1 1 calc R . . C14 C 0.481(3) 0.730(3) -0.444(2) 0.235(15) Uani 1 1 d . . . H14A H 0.4735 0.6530 -0.4383 0.352 Uiso 1 1 calc R . . H14B H 0.5398 0.7470 -0.5206 0.352 Uiso 1 1 calc R . . H14C H 0.3853 0.7853 -0.4266 0.352 Uiso 1 1 calc R . . C15 C 0.693(2) 0.741(3) -0.416(2) 0.269(19) Uani 1 1 d . . . H15A H 0.6904 0.8159 -0.4561 0.404 Uiso 1 1 calc R . . H15B H 0.7475 0.6815 -0.4699 0.404 Uiso 1 1 calc R . . H15C H 0.7373 0.7295 -0.3583 0.404 Uiso 1 1 calc R . . C16 C 0.2359(10) 0.2631(9) 0.8054(9) 0.058(2) Uani 1 1 d . . . H16 H 0.2918 0.2911 0.8302 0.070 Uiso 1 1 calc R . . C17 C 0.1979(15) 0.1034(11) 0.7505(13) 0.096(4) Uani 1 1 d . . . H17A H 0.0983 0.1519 0.7739 0.144 Uiso 1 1 calc R . . H17B H 0.2037 0.0268 0.7871 0.144 Uiso 1 1 calc R . . H17C H 0.2345 0.0991 0.6682 0.144 Uiso 1 1 calc R . . C18 C 0.4239(13) 0.0778(11) 0.7930(12) 0.093(4) Uani 1 1 d . . . H18A H 0.4912 0.0575 0.7173 0.139 Uiso 1 1 calc R . . H18B H 0.4117 0.0084 0.8398 0.139 Uiso 1 1 calc R . . H18C H 0.4611 0.1182 0.8277 0.139 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 Cd1 0.0468(3) 0.0349(3) 0.0378(3) -0.0013(2) -0.0136(2) -0.0094(2) Cd2 0.0425(3) 0.0379(3) 0.0354(3) -0.0062(2) -0.0073(2) -0.0085(2) S1 0.0345(9) 0.0398(10) 0.0535(11) -0.0081(8) -0.0175(8) -0.0070(8) O1 0.042(3) 0.043(3) 0.103(5) -0.010(3) -0.033(3) 0.000(3) O2 0.059(4) 0.046(3) 0.099(5) -0.011(3) -0.044(3) -0.010(3) O3 0.132(7) 0.103(6) 0.058(4) 0.004(4) -0.027(4) -0.058(5) O4 0.194(12) 0.083(7) 0.285(16) -0.028(8) -0.209(13) -0.003(7) O5 0.132(7) 0.085(6) 0.064(4) -0.005(4) -0.022(5) -0.071(6) O6 0.085(6) 0.118(7) 0.103(6) -0.074(5) 0.054(5) -0.072(5) O7 0.050(4) 0.059(4) 0.080(4) -0.006(3) -0.011(3) 0.008(3) O8 0.062(4) 0.100(5) 0.042(3) -0.007(3) -0.001(3) -0.039(4) O9 0.068(4) 0.116(6) 0.044(3) 0.007(4) -0.015(3) -0.027(4) O10 0.070(5) 0.050(4) 0.103(6) -0.013(4) -0.047(4) -0.004(3) N1 0.042(4) 0.054(4) 0.037(3) -0.005(3) -0.014(3) -0.014(3) N2 0.035(3) 0.033(3) 0.054(4) -0.005(3) -0.017(3) -0.007(3) N3 0.096(7) 0.087(7) 0.045(4) -0.005(4) -0.019(5) -0.030(6) N4 0.045(4) 0.054(5) 0.066(5) -0.009(4) -0.025(4) -0.007(3) C1 0.066(6) 0.066(6) 0.035(4) -0.010(4) -0.004(4) -0.020(5) C2 0.047(5) 0.058(5) 0.039(4) -0.007(4) -0.008(4) -0.017(4) C3 0.041(5) 0.087(7) 0.044(5) -0.018(4) -0.006(4) -0.020(5) C4 0.047(5) 0.073(6) 0.049(5) -0.013(4) -0.020(4) -0.012(4) C5 0.038(4) 0.089(7) 0.047(5) -0.004(5) -0.009(4) -0.028(5) C6 0.052(5) 0.088(8) 0.042(5) -0.005(5) -0.018(4) -0.014(5) C7 0.048(5) 0.034(4) 0.065(5) -0.004(4) -0.027(4) -0.004(4) C8 0.044(4) 0.036(4) 0.052(5) -0.001(3) -0.025(4) -0.006(3) C9 0.046(5) 0.034(4) 0.081(6) -0.004(4) -0.031(4) -0.010(4) C10 0.046(5) 0.042(5) 0.090(7) -0.002(4) -0.041(5) -0.005(4) C11 0.038(4) 0.038(4) 0.069(5) -0.007(4) -0.027(4) -0.004(3) C12 0.058(5) 0.033(4) 0.087(7) -0.004(4) -0.043(5) -0.008(4) C13 0.138(9) 0.088(8) 0.089(7) 0.009(6) -0.026(7) -0.053(7) C14 0.28(3) 0.32(4) 0.20(2) 0.14(2) -0.19(3) -0.18(3) C15 0.139(19) 0.43(5) 0.24(3) 0.16(3) -0.056(19) -0.20(3) C16 0.054(5) 0.058(6) 0.072(6) -0.005(5) -0.026(5) -0.022(5) C17 0.091(9) 0.070(8) 0.149(13) -0.036(8) -0.053(9) -0.023(7) C18 0.064(7) 0.073(8) 0.120(11) -0.014(7) -0.036(7) 0.014(6) _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 Cd1 O5 2.204(7) 2_665 ? Cd1 O7 2.256(7) . ? Cd1 O1 2.309(7) . ? Cd1 O3 2.315(8) . ? Cd1 N1 2.319(6) . ? Cd1 O2 2.419(6) . ? Cd2 O4 2.190(8) 2_666 ? Cd2 O6 2.275(8) 1_456 ? Cd2 O10 2.279(7) . ? Cd2 N2 2.307(6) . ? Cd2 O8 2.334(7) . ? Cd2 O9 2.423(7) . ? S1 O4 1.414(8) . ? S1 O6 1.437(8) . ? S1 O7 1.445(7) . ? S1 O5 1.453(7) . ? O1 C7 1.226(10) . ? O2 C7 1.250(10) . ? O3 C13 1.080(16) . ? O4 Cd2 2.190(8) 2_666 ? O5 Cd1 2.204(7) 2_665 ? O6 Cd2 2.275(8) 1_654 ? O8 C1 1.227(12) . ? O9 C1 1.247(12) . ? O10 C16 1.224(11) . ? N1 C4 1.323(11) . ? N1 C5 1.352(11) . ? N2 C12 1.325(10) . ? N2 C11 1.342(10) . ? N3 C13 1.324(16) . ? N3 C15 1.43(2) . ? N3 C14 1.45(2) . ? N4 C16 1.317(12) . ? N4 C18 1.450(12) . ? N4 C17 1.450(13) . ? C1 C2 1.524(11) . ? C2 C6 1.379(13) . ? C2 C3 1.398(12) . ? C3 C4 1.377(12) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.371(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.501(11) . ? C8 C9 1.390(11) . ? C8 C10 1.391(12) . ? C9 C11 1.382(11) 2_576 ? C9 H9 0.9300 . ? C10 C12 1.377(12) 2_576 ? C10 H10 0.9300 . ? C11 C9 1.382(11) 2_576 ? C11 H11 0.9300 . ? C12 C10 1.377(12) 2_576 ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 O5 Cd1 O7 116.0(3) 2_665 . ? O5 Cd1 O1 153.6(3) 2_665 . ? O7 Cd1 O1 89.0(2) . . ? O5 Cd1 O3 83.4(3) 2_665 . ? O7 Cd1 O3 88.1(3) . . ? O1 Cd1 O3 89.6(3) . . ? O5 Cd1 N1 97.8(3) 2_665 . ? O7 Cd1 N1 88.9(3) . . ? O1 Cd1 N1 90.6(3) . . ? O3 Cd1 N1 176.9(3) . . ? O5 Cd1 O2 99.9(3) 2_665 . ? O7 Cd1 O2 143.6(3) . . ? O1 Cd1 O2 54.6(2) . . ? O3 Cd1 O2 90.5(3) . . ? N1 Cd1 O2 92.1(3) . . ? O4 Cd2 O6 119.7(5) 2_666 1_456 ? O4 Cd2 O10 89.5(3) 2_666 . ? O6 Cd2 O10 84.2(3) 1_456 . ? O4 Cd2 N2 89.2(3) 2_666 . ? O6 Cd2 N2 89.8(3) 1_456 . ? O10 Cd2 N2 172.2(3) . . ? O4 Cd2 O8 149.9(5) 2_666 . ? O6 Cd2 O8 90.4(3) 1_456 . ? O10 Cd2 O8 94.5(3) . . ? N2 Cd2 O8 90.5(3) . . ? O4 Cd2 O9 95.9(5) 2_666 . ? O6 Cd2 O9 143.4(3) 1_456 . ? O10 Cd2 O9 88.2(3) . . ? N2 Cd2 O9 99.5(3) . . ? O8 Cd2 O9 54.5(2) . . ? O4 S1 O6 108.8(8) . . ? O4 S1 O7 104.7(6) . . ? O6 S1 O7 110.5(6) . . ? O4 S1 O5 110.0(7) . . ? O6 S1 O5 109.9(4) . . ? O7 S1 O5 112.8(5) . . ? C7 O1 Cd1 94.3(6) . . ? C7 O2 Cd1 88.5(5) . . ? C13 O3 Cd1 131.8(11) . . ? S1 O4 Cd2 172.1(10) . 2_666 ? S1 O5 Cd1 142.7(5) . 2_665 ? S1 O6 Cd2 122.4(6) . 1_654 ? S1 O7 Cd1 129.7(5) . . ? C1 O8 Cd2 93.2(6) . . ? C1 O9 Cd2 88.6(6) . . ? C16 O10 Cd2 125.0(7) . . ? C4 N1 C5 117.2(7) . . ? C4 N1 Cd1 122.1(5) . . ? C5 N1 Cd1 120.4(5) . . ? C12 N2 C11 117.8(7) . . ? C12 N2 Cd2 117.7(5) . . ? C11 N2 Cd2 124.5(5) . . ? C13 N3 C15 123.3(16) . . ? C13 N3 C14 123.4(16) . . ? C15 N3 C14 113.0(17) . . ? C16 N4 C18 121.5(9) . . ? C16 N4 C17 119.6(8) . . ? C18 N4 C17 118.9(10) . . ? O8 C1 O9 123.6(8) . . ? O8 C1 C2 118.2(9) . . ? O9 C1 C2 118.1(9) . . ? C6 C2 C3 118.9(8) . . ? C6 C2 C1 121.2(8) . . ? C3 C2 C1 119.9(8) . . ? C4 C3 C2 117.5(8) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? N1 C4 C3 124.4(8) . . ? N1 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? N1 C5 C6 122.8(8) . . ? N1 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C2 119.1(8) . . ? C5 C6 H6 120.4 . . ? C2 C6 H6 120.4 . . ? O1 C7 O2 122.6(8) . . ? O1 C7 C8 119.1(8) . . ? O2 C7 C8 118.3(7) . . ? C9 C8 C10 116.9(8) . . ? C9 C8 C7 122.7(8) . . ? C10 C8 C7 120.4(7) . . ? C11 C9 C8 119.2(8) 2_576 . ? C11 C9 H9 120.4 2_576 . ? C8 C9 H9 120.4 . . ? C12 C10 C8 120.3(7) 2_576 . ? C12 C10 H10 119.8 2_576 . ? C8 C10 H10 119.8 . . ? N2 C11 C9 123.2(7) . 2_576 ? N2 C11 H11 118.4 . . ? C9 C11 H11 118.4 2_576 . ? N2 C12 C10 122.6(8) . 2_576 ? N2 C12 H12 118.7 . . ? C10 C12 H12 118.7 2_576 . ? O3 C13 N3 136.9(17) . . ? O3 C13 H13 111.6 . . ? N3 C13 H13 111.6 . . ? N3 C14 H14A 109.5 . . ? N3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O10 C16 N4 124.9(9) . . ? O10 C16 H16 117.5 . . ? N4 C16 H16 117.5 . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.974 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.163 _database_code_depnum_ccdc_archive 'CCDC 951152' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 Cd3 N5.50 O11.50' _chemical_formula_weight 1017.77 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' Cd Cd -0.8075 1.2024 '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 12.048(2) _cell_length_b 12.280(3) _cell_length_c 19.092(4) _cell_angle_alpha 91.92(3) _cell_angle_beta 98.10(3) _cell_angle_gamma 117.88(3) _cell_volume 2455.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9146 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 987 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 0.661 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9146 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9146 _reflns_number_gt 8170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0824P)^2^+7.9633P] 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_number_reflns 9070 _refine_ls_number_parameters 496 _refine_ls_number_restraints 654 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.005 _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 O1W O 0.8866(8) 0.0811(7) 0.4347(4) 0.078(2) Uani 0.50 1 d PU . . H1WB H 0.9656 0.1121 0.4331 0.116 Uiso 0.50 1 d PR . . H1WC H 0.8774 0.0951 0.4768 0.116 Uiso 0.50 1 d PR . . Cd1 Cd 0.76625(2) 0.50709(2) 0.279208(13) 0.02521(6) Uani 1 1 d U . . Cd2 Cd 0.57876(2) 0.670864(19) 0.200255(11) 0.02094(6) Uani 1 1 d U . . Cd3 Cd 0.42096(2) 0.325409(19) 0.299186(11) 0.02134(6) Uani 1 1 d U . . O8 O 0.4308(2) 0.3148(2) 0.18133(12) 0.0358(7) Uani 1 1 d U A . O6 O 0.6158(2) 0.5139(2) 0.34142(12) 0.0264(6) Uani 1 1 d U A . O7 O 0.6103(2) 0.4937(2) 0.18108(12) 0.0281(6) Uani 1 1 d U A . O3 O 0.5228(2) 0.2124(2) 0.31614(14) 0.0361(6) Uani 1 1 d U A . O5 O 0.6070(3) 0.6882(2) 0.32093(13) 0.0371(7) Uani 1 1 d U A . O1 O 0.3192(2) 0.4374(2) 0.27918(14) 0.0402(7) Uani 1 1 d U A . O2 O 0.3652(2) 0.5647(2) 0.19356(14) 0.0377(7) Uani 1 1 d U A . O10 O 0.7860(3) 0.7917(3) 0.19730(15) 0.0444(8) Uani 1 1 d U A . N4 N 0.4590(3) 0.3303(3) -0.07613(15) 0.0317(7) Uani 1 1 d U . . O4 O 0.6700(2) 0.2997(2) 0.24790(16) 0.0405(7) Uani 1 1 d U A . N5 N 1.2301(3) 1.1356(3) 0.27249(17) 0.0357(8) Uani 1 1 d U . . N3 N 0.6098(3) 0.6741(3) 0.58267(15) 0.0304(7) Uani 1 1 d U . . N2 N 0.5699(3) -0.1432(3) 0.21874(18) 0.0403(8) Uani 1 1 d U . . N1 N -0.0623(3) 0.4962(3) 0.2373(2) 0.0471(9) Uani 1 1 d U . . O9 O 0.8742(3) 0.7104(2) 0.27574(19) 0.0527(9) Uani 1 1 d U A . C13 C 0.6132(3) 0.6122(3) 0.36056(17) 0.0267(8) Uani 1 1 d U . . C14 C 0.6141(3) 0.6377(3) 0.43889(17) 0.0276(8) Uani 1 1 d U A . C20 C 0.4965(3) 0.3673(3) 0.07200(17) 0.0270(8) Uani 1 1 d U A . C19 C 0.5124(3) 0.3927(3) 0.15116(17) 0.0251(7) Uani 1 1 d U . . C1 C 0.2943(3) 0.4998(3) 0.23509(18) 0.0282(8) Uani 1 1 d U . . C16 C 0.6681(3) 0.5887(3) 0.48934(18) 0.0330(9) Uani 1 1 d U . . H16A H 0.7046 0.5413 0.4754 0.040 Uiso 1 1 calc R A . C2 C 0.1697(3) 0.4982(3) 0.2331(2) 0.0323(8) Uani 1 1 d U A . C18 C 0.5583(4) 0.7209(3) 0.5339(2) 0.0373(9) Uani 1 1 d U A . H18 H 0.5196 0.7654 0.5490 0.045 Uiso 1 1 calc R . . C15 C 0.5600(4) 0.7063(3) 0.46236(19) 0.0352(9) Uani 1 1 d U . . H15 H 0.5251 0.7421 0.4302 0.042 Uiso 1 1 calc R A . C7 C 0.5925(3) 0.2102(3) 0.2750(2) 0.0328(8) Uani 1 1 d U . . C21 C 0.5972(3) 0.4238(3) 0.03596(18) 0.0355(10) Uani 1 1 d U . . H21 H 0.6791 0.4759 0.0609 0.043 Uiso 1 1 calc R A . C23 C 0.3615(4) 0.2738(4) -0.0409(2) 0.0412(11) Uani 1 1 d U A . H23 H 0.2801 0.2232 -0.0668 0.049 Uiso 1 1 calc R . . C25 C 0.8764(3) 0.7946(3) 0.2392(2) 0.0361(9) Uani 1 1 d U . . C22 C 0.3783(4) 0.2885(4) 0.0325(2) 0.0408(11) Uani 1 1 d U . . H22 H 0.3095 0.2450 0.0553 0.049 Uiso 1 1 calc R A . O11 O 0.8573(4) 0.4906(4) 0.3897(2) 0.0658(10) Uani 0.50 1 d PU A 1 N1A N 0.8573(4) 0.4906(4) 0.3897(2) 0.0658(10) Uani 0.50 1 d PU A 2 C26 C 1.0022(3) 0.9134(3) 0.2498(2) 0.0337(9) Uani 1 1 d U A . C17 C 0.6667(3) 0.6117(3) 0.56033(19) 0.0335(9) Uani 1 1 d U A . H17 H 0.7069 0.5826 0.5940 0.040 Uiso 1 1 calc R . . C30 C 1.1038(4) 0.9289(4) 0.3004(2) 0.0419(10) Uani 1 1 d U . . H30 H 1.0972 0.8655 0.3278 0.050 Uiso 1 1 calc R A . C24 C 0.5753(3) 0.4024(4) -0.03734(19) 0.0367(9) Uani 1 1 d U A . H24 H 0.6442 0.4395 -0.0609 0.044 Uiso 1 1 calc R . . C8 C 0.5839(3) 0.0855(3) 0.2546(2) 0.0361(9) Uani 1 1 d U A . C27 C 1.1315(4) 1.1180(4) 0.2230(2) 0.0434(11) Uani 1 1 d U A . H27 H 1.1403 1.1825 0.1962 0.052 Uiso 1 1 calc R . . C29 C 1.2163(4) 1.0413(4) 0.3098(2) 0.0417(10) Uani 1 1 d U A . H29 H 1.2850 1.0511 0.3435 0.050 Uiso 1 1 calc R . . C10 C 0.5080(4) -0.0177(3) 0.2856(2) 0.0410(9) Uani 1 1 d U . . H10 H 0.4607 -0.0121 0.3187 0.049 Uiso 1 1 calc R A . C9 C 0.6504(4) 0.0718(4) 0.2044(2) 0.0457(10) Uani 1 1 d U . . H9 H 0.6999 0.1389 0.1814 0.055 Uiso 1 1 calc R A . C11 C 0.5038(4) -0.1296(3) 0.2665(2) 0.0428(10) Uani 1 1 d U A . H11 H 0.4529 -0.1987 0.2877 0.051 Uiso 1 1 calc R . . C28 C 1.0173(4) 1.0095(4) 0.2097(2) 0.0450(11) Uani 1 1 d U . . H28 H 0.9514 1.0011 0.1742 0.054 Uiso 1 1 calc R A . C12 C 0.6421(4) -0.0426(3) 0.1889(2) 0.0450(10) Uani 1 1 d U A . H12 H 0.6890 -0.0502 0.1561 0.054 Uiso 1 1 calc R . . C3 C 0.1456(4) 0.5904(4) 0.2080(3) 0.0526(11) Uani 1 1 d U . . H3 H 0.2070 0.6551 0.1886 0.063 Uiso 1 1 calc R A . C5 C 0.0301(4) 0.5867(4) 0.2117(3) 0.0525(11) Uani 1 1 d U A . H5 H 0.0169 0.6510 0.1955 0.063 Uiso 1 1 calc R . . C4 C 0.0721(4) 0.4025(4) 0.2608(3) 0.0519(11) Uani 1 1 d U . . H4 H 0.0836 0.3387 0.2793 0.062 Uiso 1 1 calc R A . C6 C -0.0409(4) 0.4049(4) 0.2601(3) 0.0559(12) Uani 1 1 d U A . H6 H -0.1065 0.3390 0.2764 0.067 Uiso 1 1 calc R . . C1A C 0.9759(6) 0.5680(6) 0.4130(3) 0.0763(16) Uani 1 1 d U . . C3A C 1.0340(6) 0.5483(5) 0.4826(3) 0.0765(17) Uani 1 1 d U . . O12 O 1.0327(10) 0.6525(9) 0.3846(5) 0.105(3) Uani 0.50 1 d PU A . C4A C 0.8007(9) 0.3982(9) 0.4208(5) 0.0541(19) Uani 0.50 1 d PU . . C2A C 0.8566(9) 0.3800(9) 0.4871(5) 0.054(2) Uani 0.50 1 d PU . . 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 O1W 0.075(4) 0.076(4) 0.080(4) 0.006(3) 0.027(3) 0.032(3) Cd1 0.02035(9) 0.02135(9) 0.03540(12) 0.00723(8) 0.00879(9) 0.00986(7) Cd2 0.02368(9) 0.02043(9) 0.01800(10) 0.00240(8) 0.00492(8) 0.00959(8) Cd3 0.02192(9) 0.02116(10) 0.01842(10) 0.00183(8) 0.00591(8) 0.00762(8) O8 0.0399(12) 0.0347(12) 0.0204(11) 0.0018(9) 0.0068(10) 0.0075(10) O6 0.0255(9) 0.0264(10) 0.0248(10) -0.0033(8) 0.0076(8) 0.0100(8) O7 0.0354(10) 0.0229(9) 0.0212(10) -0.0012(8) -0.0002(9) 0.0117(8) O3 0.0443(11) 0.0311(10) 0.0441(13) 0.0038(10) 0.0143(10) 0.0255(8) O5 0.0568(13) 0.0320(11) 0.0206(11) 0.0049(9) 0.0087(10) 0.0189(10) O1 0.0420(11) 0.0541(12) 0.0414(13) 0.0193(10) 0.0175(10) 0.0330(9) O2 0.0247(10) 0.0496(13) 0.0383(12) 0.0176(10) 0.0151(9) 0.0139(9) O10 0.0275(12) 0.0432(14) 0.0426(14) 0.0063(12) 0.0029(11) 0.0015(11) N4 0.0355(13) 0.0361(13) 0.0213(12) 0.0033(11) 0.0077(11) 0.0146(11) O4 0.0335(11) 0.0249(10) 0.0641(16) 0.0046(11) 0.0143(11) 0.0133(9) N5 0.0270(13) 0.0275(13) 0.0398(15) 0.0059(12) 0.0029(12) 0.0033(11) N3 0.0367(12) 0.0328(12) 0.0214(12) 0.0028(10) 0.0099(11) 0.0150(10) N2 0.0580(15) 0.0300(12) 0.0429(16) 0.0075(12) 0.0175(13) 0.0266(11) N1 0.0360(13) 0.0468(15) 0.069(2) 0.0169(14) 0.0168(14) 0.0258(11) O9 0.0395(14) 0.0258(12) 0.0771(19) 0.0114(13) 0.0060(14) 0.0037(11) C13 0.0283(13) 0.0262(13) 0.0179(13) 0.0004(11) 0.0050(11) 0.0066(11) C14 0.0291(13) 0.0280(13) 0.0225(14) 0.0032(12) 0.0069(11) 0.0103(11) C20 0.0337(14) 0.0255(13) 0.0191(13) 0.0015(11) 0.0038(11) 0.0122(11) C19 0.0318(13) 0.0253(12) 0.0199(13) 0.0015(11) 0.0052(11) 0.0150(10) C1 0.0227(12) 0.0361(14) 0.0306(15) 0.0063(12) 0.0094(11) 0.0167(10) C16 0.0384(15) 0.0381(15) 0.0244(15) 0.0031(13) 0.0076(13) 0.0192(13) C2 0.0270(13) 0.0352(14) 0.0401(16) 0.0151(13) 0.0146(12) 0.0162(11) C18 0.0529(16) 0.0387(15) 0.0299(16) 0.0027(13) 0.0102(14) 0.0292(13) C15 0.0529(16) 0.0366(14) 0.0255(15) 0.0072(12) 0.0108(13) 0.0277(12) C7 0.0321(14) 0.0254(13) 0.0436(17) 0.0044(13) 0.0067(13) 0.0158(11) C21 0.0293(15) 0.0434(17) 0.0251(15) 0.0024(14) 0.0019(13) 0.0111(13) C23 0.0348(17) 0.0416(18) 0.0268(16) 0.0022(14) 0.0059(14) 0.0015(15) C25 0.0279(14) 0.0264(14) 0.0448(18) -0.0007(14) 0.0103(14) 0.0047(12) C22 0.0337(16) 0.0430(18) 0.0266(16) 0.0038(14) 0.0107(14) 0.0012(15) O11 0.0604(15) 0.0836(18) 0.0557(17) 0.0143(15) -0.0001(14) 0.0385(13) N1A 0.0604(15) 0.0836(18) 0.0557(17) 0.0143(15) -0.0001(14) 0.0385(13) C26 0.0264(14) 0.0248(14) 0.0419(17) 0.0043(13) 0.0079(13) 0.0052(12) C17 0.0334(14) 0.0447(16) 0.0265(15) 0.0054(13) 0.0073(12) 0.0215(12) C30 0.0322(16) 0.0308(16) 0.053(2) 0.0140(15) 0.0034(15) 0.0072(13) C24 0.0287(14) 0.0497(18) 0.0274(15) 0.0062(14) 0.0107(13) 0.0136(13) C8 0.0424(15) 0.0277(13) 0.0450(18) 0.0051(13) 0.0117(14) 0.0212(11) C27 0.0346(17) 0.0312(16) 0.050(2) 0.0145(15) 0.0025(16) 0.0042(14) C29 0.0304(16) 0.0340(16) 0.0465(19) 0.0101(15) -0.0007(15) 0.0055(14) C10 0.0488(16) 0.0318(14) 0.0528(19) 0.0068(14) 0.0266(15) 0.0230(12) C9 0.0611(18) 0.0302(15) 0.055(2) 0.0123(14) 0.0300(16) 0.0234(13) C11 0.0553(17) 0.0289(14) 0.0528(19) 0.0125(14) 0.0278(16) 0.0217(13) C28 0.0319(16) 0.0361(17) 0.051(2) 0.0114(16) -0.0037(16) 0.0055(14) C12 0.0635(17) 0.0365(15) 0.0502(19) 0.0091(14) 0.0317(15) 0.0301(13) C3 0.0455(17) 0.0552(18) 0.071(2) 0.0315(17) 0.0248(17) 0.0300(14) C5 0.0447(16) 0.0551(18) 0.074(2) 0.0324(17) 0.0290(17) 0.0308(14) C4 0.0420(16) 0.0465(17) 0.081(2) 0.0219(17) 0.0277(17) 0.0268(14) C6 0.0440(17) 0.0443(18) 0.088(3) 0.0229(18) 0.0286(18) 0.0224(15) C1A 0.075(2) 0.080(2) 0.060(2) 0.011(2) -0.004(2) 0.031(2) C3A 0.081(3) 0.081(3) 0.066(3) 0.002(2) -0.013(2) 0.045(2) O12 0.119(5) 0.096(4) 0.077(4) 0.030(4) -0.007(4) 0.039(4) C4A 0.054(3) 0.065(3) 0.049(3) 0.012(3) 0.008(3) 0.033(2) C2A 0.060(3) 0.061(3) 0.046(4) 0.009(3) 0.006(3) 0.034(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. ; # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.010 0.000 0.000 552.5 1.7 2 0.041 0.329 0.409 11.9 0.2 3 -0.041 0.670 0.591 11.9 0.2 4 0.096 0.165 0.575 25.8 -3.4 5 0.108 0.883 0.708 8.6 0.9 6 0.165 0.094 0.458 10.6 -1.7 7 0.500 1.000 0.500 162.6 4.6 8 0.837 0.897 0.532 13.0 -2.4 9 0.908 0.832 0.419 22.9 -2.6 10 0.892 0.117 0.292 8.6 1.2 _platon_squeeze_details ; ? ; 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 O1W H1WB 0.8500 . ? O1W H1WC 0.8500 . ? Cd1 O9 2.220(3) . ? Cd1 O4 2.265(3) . ? Cd1 O11 2.298(4) . ? Cd1 O6 2.334(3) . ? Cd1 N1 2.376(4) 1_655 ? Cd1 O7 2.401(2) . ? Cd2 O10 2.240(3) . ? Cd2 O2 2.257(2) . ? Cd2 O5 2.269(2) . ? Cd2 N4 2.347(3) 2_665 ? Cd2 N2 2.353(3) 1_565 ? Cd2 O7 2.402(3) . ? Cd3 O1 2.241(3) . ? Cd3 O3 2.246(3) . ? Cd3 O8 2.272(2) . ? Cd3 N3 2.337(3) 2_666 ? Cd3 N5 2.357(3) 1_445 ? Cd3 O6 2.404(2) . ? O8 C19 1.237(4) . ? O6 C13 1.264(5) . ? O7 C19 1.284(4) . ? O3 C7 1.236(5) . ? O5 C13 1.243(5) . ? O1 C1 1.254(5) . ? O2 C1 1.261(4) . ? O10 C25 1.243(5) . ? N4 C24 1.341(4) . ? N4 C23 1.344(5) . ? N4 Cd2 2.347(3) 2_665 ? O4 C7 1.250(4) . ? N5 C27 1.334(5) . ? N5 C29 1.337(5) . ? N5 Cd3 2.357(3) 1_665 ? N3 C18 1.338(5) . ? N3 C17 1.339(5) . ? N3 Cd3 2.337(3) 2_666 ? N2 C12 1.337(5) . ? N2 C11 1.345(6) . ? N2 Cd2 2.353(3) 1_545 ? N1 C5 1.321(5) . ? N1 C6 1.336(7) . ? N1 Cd1 2.376(4) 1_455 ? O9 C25 1.258(5) . ? C13 C14 1.515(5) . ? C14 C15 1.380(6) . ? C14 C16 1.394(5) . ? C20 C22 1.376(5) . ? C20 C21 1.381(5) . ? C20 C19 1.500(4) . ? C1 C2 1.487(5) . ? C16 C17 1.379(5) . ? C16 H16A 0.9300 . ? C2 C3 1.379(6) . ? C2 C4 1.403(5) . ? C18 C15 1.375(5) . ? C18 H18 0.9300 . ? C15 H15 0.9300 . ? C7 C8 1.520(5) . ? C21 C24 1.380(5) . ? C21 H21 0.9300 . ? C23 C22 1.381(5) . ? C23 H23 0.9300 . ? C25 C26 1.514(4) . ? C22 H22 0.9300 . ? O11 C4A 1.241(10) . ? O11 C1A 1.290(7) . ? C26 C30 1.381(6) . ? C26 C28 1.383(6) . ? C17 H17 0.9300 . ? C30 C29 1.393(5) . ? C30 H30 0.9300 . ? C24 H24 0.9300 . ? C8 C10 1.382(5) . ? C8 C9 1.387(6) . ? C27 C28 1.378(5) . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C10 C11 1.387(6) . ? C10 H10 0.9300 . ? C9 C12 1.380(6) . ? C9 H9 0.9300 . ? C11 H11 0.9300 . ? C28 H28 0.9300 . ? C12 H12 0.9300 . ? C3 C5 1.382(7) . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? C4 C6 1.373(7) . ? C4 H4 0.9300 . ? C6 H6 0.9300 . ? C1A O12 1.148(11) . ? C1A C3A 1.494(8) . ? C3A C2A 1.230(10) 2_766 ? C3A C3A 1.347(12) 2_766 ? C4A C2A 1.423(14) . ? C2A C3A 1.230(10) 2_766 ? 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 H1WB O1W H1WC 109.5 . . ? O9 Cd1 O4 162.00(12) . . ? O9 Cd1 O11 100.50(14) . . ? O4 Cd1 O11 92.29(14) . . ? O9 Cd1 O6 95.47(12) . . ? O4 Cd1 O6 98.62(10) . . ? O11 Cd1 O6 83.11(13) . . ? O9 Cd1 N1 86.65(13) . 1_655 ? O4 Cd1 N1 81.62(11) . 1_655 ? O11 Cd1 N1 86.00(15) . 1_655 ? O6 Cd1 N1 169.11(11) . 1_655 ? O9 Cd1 O7 89.50(11) . . ? O4 Cd1 O7 81.94(10) . . ? O11 Cd1 O7 161.32(12) . . ? O6 Cd1 O7 80.24(9) . . ? N1 Cd1 O7 110.50(11) 1_655 . ? O10 Cd2 O2 172.66(11) . . ? O10 Cd2 O5 94.20(11) . . ? O2 Cd2 O5 90.45(10) . . ? O10 Cd2 N4 87.20(11) . 2_665 ? O2 Cd2 N4 87.55(10) . 2_665 ? O5 Cd2 N4 173.41(12) . 2_665 ? O10 Cd2 N2 85.97(12) . 1_565 ? O2 Cd2 N2 89.07(12) . 1_565 ? O5 Cd2 N2 81.94(12) . 1_565 ? N4 Cd2 N2 91.74(12) 2_665 1_565 ? O10 Cd2 O7 88.26(11) . . ? O2 Cd2 O7 96.68(10) . . ? O5 Cd2 O7 98.48(10) . . ? N4 Cd2 O7 88.00(10) 2_665 . ? N2 Cd2 O7 174.23(10) 1_565 . ? O1 Cd3 O3 178.50(10) . . ? O1 Cd3 O8 88.83(11) . . ? O3 Cd3 O8 89.67(11) . . ? O1 Cd3 N3 88.81(11) . 2_666 ? O3 Cd3 N3 92.67(11) . 2_666 ? O8 Cd3 N3 174.68(9) . 2_666 ? O1 Cd3 N5 92.89(11) . 1_445 ? O3 Cd3 N5 86.89(11) . 1_445 ? O8 Cd3 N5 87.14(11) . 1_445 ? N3 Cd3 N5 88.21(11) 2_666 1_445 ? O1 Cd3 O6 89.20(9) . . ? O3 Cd3 O6 91.19(9) . . ? O8 Cd3 O6 99.63(9) . . ? N3 Cd3 O6 85.11(9) 2_666 . ? N5 Cd3 O6 172.96(10) 1_445 . ? C19 O8 Cd3 126.9(2) . . ? C13 O6 Cd1 124.3(2) . . ? C13 O6 Cd3 120.6(2) . . ? Cd1 O6 Cd3 105.64(9) . . ? C19 O7 Cd2 116.9(2) . . ? C19 O7 Cd1 124.9(2) . . ? Cd2 O7 Cd1 107.01(9) . . ? C7 O3 Cd3 121.1(3) . . ? C13 O5 Cd2 127.5(2) . . ? C1 O1 Cd3 143.6(3) . . ? C1 O2 Cd2 133.5(2) . . ? C25 O10 Cd2 125.5(3) . . ? C24 N4 C23 117.5(3) . . ? C24 N4 Cd2 121.0(2) . 2_665 ? C23 N4 Cd2 120.7(2) . 2_665 ? C7 O4 Cd1 131.9(3) . . ? C27 N5 C29 117.4(3) . . ? C27 N5 Cd3 123.2(3) . 1_665 ? C29 N5 Cd3 119.4(2) . 1_665 ? C18 N3 C17 117.9(3) . . ? C18 N3 Cd3 122.1(3) . 2_666 ? C17 N3 Cd3 119.4(2) . 2_666 ? C12 N2 C11 117.3(3) . . ? C12 N2 Cd2 121.3(3) . 1_545 ? C11 N2 Cd2 120.9(3) . 1_545 ? C5 N1 C6 117.2(4) . . ? C5 N1 Cd1 125.7(3) . 1_455 ? C6 N1 Cd1 114.3(3) . 1_455 ? C25 O9 Cd1 141.7(3) . . ? O5 C13 O6 126.2(3) . . ? O5 C13 C14 117.0(3) . . ? O6 C13 C14 116.8(3) . . ? C15 C14 C16 118.2(3) . . ? C15 C14 C13 122.0(3) . . ? C16 C14 C13 119.7(4) . . ? C22 C20 C21 117.7(3) . . ? C22 C20 C19 120.2(3) . . ? C21 C20 C19 122.0(3) . . ? O8 C19 O7 126.3(3) . . ? O8 C19 C20 117.3(3) . . ? O7 C19 C20 116.4(3) . . ? O1 C1 O2 126.4(3) . . ? O1 C1 C2 116.2(3) . . ? O2 C1 C2 117.4(3) . . ? C17 C16 C14 119.0(4) . . ? C17 C16 H16A 120.5 . . ? C14 C16 H16A 120.5 . . ? C3 C2 C4 116.9(4) . . ? C3 C2 C1 123.2(3) . . ? C4 C2 C1 119.9(4) . . ? N3 C18 C15 123.0(4) . . ? N3 C18 H18 118.5 . . ? C15 C18 H18 118.5 . . ? C18 C15 C14 119.2(4) . . ? C18 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? O3 C7 O4 127.3(4) . . ? O3 C7 C8 117.1(3) . . ? O4 C7 C8 115.7(4) . . ? C24 C21 C20 119.4(3) . . ? C24 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? N4 C23 C22 122.1(3) . . ? N4 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? O10 C25 O9 127.0(3) . . ? O10 C25 C26 117.0(4) . . ? O9 C25 C26 116.0(3) . . ? C20 C22 C23 120.1(4) . . ? C20 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C4A O11 C1A 120.2(6) . . ? C4A O11 Cd1 120.5(5) . . ? C1A O11 Cd1 118.3(4) . . ? C30 C26 C28 118.5(3) . . ? C30 C26 C25 120.7(4) . . ? C28 C26 C25 120.8(3) . . ? N3 C17 C16 122.6(4) . . ? N3 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C26 C30 C29 118.7(4) . . ? C26 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? N4 C24 C21 122.9(3) . . ? N4 C24 H24 118.5 . . ? C21 C24 H24 118.5 . . ? C10 C8 C9 118.4(4) . . ? C10 C8 C7 120.3(4) . . ? C9 C8 C7 121.2(3) . . ? N5 C27 C28 123.5(4) . . ? N5 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? N5 C29 C30 123.0(4) . . ? N5 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C8 C10 C11 118.8(4) . . ? C8 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C9 C8 119.1(4) . . ? C12 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C11 C10 123.1(4) . . ? N2 C11 H11 118.4 . . ? C10 C11 H11 118.4 . . ? C27 C28 C26 118.9(4) . . ? C27 C28 H28 120.5 . . ? C26 C28 H28 120.5 . . ? N2 C12 C9 123.2(4) . . ? N2 C12 H12 118.4 . . ? C9 C12 H12 118.4 . . ? C2 C3 C5 120.1(4) . . ? C2 C3 H3 120.0 . . ? C5 C3 H3 120.0 . . ? N1 C5 C3 123.1(5) . . ? N1 C5 H5 118.5 . . ? C3 C5 H5 118.5 . . ? C6 C4 C2 118.8(4) . . ? C6 C4 H4 120.6 . . ? C2 C4 H4 120.6 . . ? N1 C6 C4 123.9(4) . . ? N1 C6 H6 118.1 . . ? C4 C6 H6 118.1 . . ? O12 C1A O11 122.4(7) . . ? O12 C1A C3A 120.9(7) . . ? O11 C1A C3A 116.6(5) . . ? C2A C3A C3A 115.9(8) 2_766 2_766 ? C2A C3A C1A 123.0(7) 2_766 . ? C3A C3A C1A 121.0(7) 2_766 . ? O11 C4A C2A 122.5(8) . . ? C3A C2A C4A 123.3(9) 2_766 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.525 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.174 _database_code_depnum_ccdc_archive 'CCDC 951153'