# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 877931' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 Ni O8' _chemical_formula_sum 'C17 H18 Ni O8' _chemical_formula_weight 409.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.6619(4) _cell_length_b 5.8283(3) _cell_length_c 19.2568(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.833(4) _cell_angle_gamma 90.00 _cell_volume 844.60(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2423 _cell_measurement_theta_min 3.1204 _cell_measurement_theta_max 29.0659 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7087 _exptl_absorpt_correction_T_max 0.7964 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5276 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2622 _reflns_number_gt 2421 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0351P)^2^+0.0000P] 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' _refine_ls_abs_structure_Flack -0.006(18) _refine_ls_number_reflns 2622 _refine_ls_number_parameters 247 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _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 Ni1 Ni 0.66450(6) 0.44080(10) 0.61611(2) 0.02340(15) Uani 1 1 d . . . C1 C 1.1344(6) 0.1152(9) 1.2845(2) 0.0278(10) Uani 1 1 d . . . C2 C 1.0280(5) 0.1988(8) 1.21691(19) 0.0240(9) Uani 1 1 d . . . C3 C 1.0016(6) 0.0526(8) 1.1593(2) 0.0343(11) Uani 1 1 d . . . H3 H 1.0493 -0.0946 1.1640 0.041 Uiso 1 1 calc R . . C4 C 0.9050(6) 0.1229(8) 1.0947(2) 0.0344(11) Uani 1 1 d . . . H4 H 0.8931 0.0253 1.0559 0.041 Uiso 1 1 calc R . . C5 C 0.8261(5) 0.3365(8) 1.0873(2) 0.0297(10) Uani 1 1 d . . . C6 C 0.8510(5) 0.4808(9) 1.14536(19) 0.0311(11) Uani 1 1 d . . . H6 H 0.7963 0.6239 1.1415 0.037 Uiso 1 1 calc R . . C7 C 0.9557(5) 0.4165(9) 1.20908(18) 0.0281(10) Uani 1 1 d . . . H7 H 0.9772 0.5198 1.2465 0.034 Uiso 1 1 calc R . . C8 C 0.7158(6) 0.4201(10) 1.01857(18) 0.0383(11) Uani 1 1 d . . . H8A H 0.6031 0.4796 1.0267 0.046 Uiso 1 1 calc R . . H8B H 0.7778 0.5425 0.9991 0.046 Uiso 1 1 calc R . . C9 C 0.6216(5) 0.2836(8) 0.89989(19) 0.0277(10) Uani 1 1 d . . . C10 C 0.6486(6) 0.1159(8) 0.85247(19) 0.0324(10) Uani 1 1 d . . . H10 H 0.7021 -0.0221 0.8687 0.039 Uiso 1 1 calc R . . C11 C 0.5957(6) 0.1541(8) 0.7808(2) 0.0328(11) Uani 1 1 d . . . H11 H 0.6138 0.0427 0.7483 0.039 Uiso 1 1 calc R . . C12 C 0.5157(5) 0.3598(7) 0.7581(2) 0.0264(10) Uani 1 1 d . . . C13 C 0.4817(5) 0.5245(8) 0.8051(2) 0.0331(11) Uani 1 1 d . . . H13 H 0.4243 0.6602 0.7889 0.040 Uiso 1 1 calc R . . C14 C 0.5355(5) 0.4832(9) 0.87756(19) 0.0335(12) Uani 1 1 d . . . H14 H 0.5128 0.5910 0.9103 0.040 Uiso 1 1 calc R . . C15 C 0.2954(5) 0.4207(10) 0.64963(17) 0.0276(9) Uani 1 1 d . . . H15 H 0.2268 0.5077 0.6788 0.033 Uiso 1 1 calc R . . C16 C 0.2173(6) 0.1837(9) 0.6362(2) 0.0423(12) Uani 1 1 d . . . H16A H 0.2197 0.1071 0.6805 0.064 Uiso 1 1 calc R . . H16B H 0.2858 0.0976 0.6083 0.064 Uiso 1 1 calc R . . H16C H 0.0968 0.1955 0.6113 0.064 Uiso 1 1 calc R . . C17 C 0.2954(5) 0.5486(7) 0.5809(2) 0.0257(9) Uani 1 1 d . . . O1 O 1.1301(3) -0.0957(6) 1.29937(13) 0.0295(8) Uani 1 1 d . . . O2 O 1.2322(4) 0.2492(5) 1.32675(13) 0.0304(7) Uani 1 1 d . . . O3 O 0.6864(4) 0.2335(6) 0.97059(14) 0.0408(8) Uani 1 1 d . . . O4 O 0.4807(3) 0.4091(6) 0.68524(11) 0.0304(8) Uani 1 1 d . . . O5 O 0.1541(4) 0.6380(6) 0.55096(14) 0.0368(8) Uani 1 1 d . . . O6 O 0.4379(3) 0.5561(5) 0.55693(13) 0.0278(7) Uani 1 1 d . . . O1W O 0.8090(4) 0.4951(5) 0.53992(14) 0.0309(8) Uani 1 1 d D . . H1A H 0.918(3) 0.558(8) 0.552(2) 0.046 Uiso 1 1 d D . . H1B H 0.832(6) 0.371(5) 0.516(2) 0.046 Uiso 1 1 d D . . O2W O 0.6185(4) 0.1093(5) 0.58720(15) 0.0368(8) Uani 1 1 d D . . H2A H 0.582(6) 0.085(9) 0.5409(8) 0.055 Uiso 1 1 d D . . H2B H 0.709(4) 0.031(8) 0.613(2) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0256(3) 0.0260(3) 0.0170(2) -0.0008(2) -0.00040(16) 0.0013(3) C1 0.032(3) 0.029(3) 0.021(2) 0.003(2) 0.0038(17) -0.002(2) C2 0.024(2) 0.027(2) 0.020(2) 0.0007(18) 0.0001(15) -0.0032(19) C3 0.040(3) 0.029(3) 0.029(2) 0.0014(19) -0.0047(19) 0.006(2) C4 0.047(3) 0.033(3) 0.019(2) -0.008(2) -0.0040(18) 0.005(2) C5 0.031(2) 0.033(3) 0.023(2) 0.0010(19) 0.0009(17) -0.001(2) C6 0.033(2) 0.028(3) 0.029(2) 0.0005(19) 0.0006(16) 0.009(2) C7 0.038(2) 0.025(3) 0.0199(18) 0.000(2) 0.0025(15) -0.004(2) C8 0.050(2) 0.043(3) 0.0190(19) 0.001(3) -0.0018(16) 0.009(3) C9 0.031(2) 0.035(3) 0.015(2) 0.0026(19) -0.0015(16) 0.000(2) C10 0.046(3) 0.023(2) 0.025(2) 0.0034(19) -0.0023(18) 0.007(2) C11 0.041(3) 0.031(3) 0.025(2) -0.0049(19) 0.0037(18) 0.000(2) C12 0.027(2) 0.031(3) 0.020(2) 0.0031(17) 0.0021(16) 0.0010(18) C13 0.037(2) 0.036(3) 0.025(2) 0.0041(18) 0.0018(18) 0.009(2) C14 0.042(2) 0.038(4) 0.0188(19) -0.0041(19) 0.0002(16) 0.009(2) C15 0.0243(19) 0.038(3) 0.0199(17) 0.001(2) 0.0035(13) 0.005(3) C16 0.046(3) 0.039(3) 0.041(3) 0.011(2) 0.006(2) -0.005(3) C17 0.027(2) 0.024(2) 0.025(2) -0.0022(17) 0.0026(18) -0.0033(19) O1 0.0271(14) 0.034(2) 0.0235(14) 0.0025(14) -0.0047(10) -0.0042(15) O2 0.0337(17) 0.0311(19) 0.0215(14) -0.0020(13) -0.0075(12) -0.0061(15) O3 0.067(2) 0.032(2) 0.0174(15) 0.0054(14) -0.0078(13) 0.0009(17) O4 0.0264(13) 0.052(2) 0.0128(12) 0.0037(14) 0.0028(9) 0.0015(17) O5 0.0241(16) 0.048(2) 0.0362(16) 0.0185(15) -0.0001(12) 0.0047(16) O6 0.0267(16) 0.0373(18) 0.0177(13) 0.0082(12) 0.0001(11) 0.0050(13) O1W 0.0294(15) 0.039(3) 0.0245(14) -0.0080(13) 0.0062(11) -0.0070(15) O2W 0.057(2) 0.0269(19) 0.0231(16) -0.0041(14) -0.0004(14) -0.0001(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni1 O6 2.005(3) . ? Ni1 O1W 2.022(2) . ? Ni1 O2W 2.023(3) . ? Ni1 O1 2.051(3) 2_757 ? Ni1 O4 2.120(2) . ? Ni1 O2 2.177(3) 2_757 ? Ni1 C1 2.442(4) 2_757 ? C1 O1 1.264(6) . ? C1 O2 1.266(5) . ? C1 C2 1.482(6) . ? C1 Ni1 2.442(4) 2_747 ? C2 C7 1.382(6) . ? C2 C3 1.383(6) . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.379(6) . ? C4 H4 0.9300 . ? C5 C6 1.383(6) . ? C5 C8 1.511(5) . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.418(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.366(6) . ? C9 C10 1.379(6) . ? C9 O3 1.390(4) . ? C10 C11 1.382(5) . ? C10 H10 0.9300 . ? C11 C12 1.379(6) . ? C11 H11 0.9300 . ? C12 C13 1.376(6) . ? C12 O4 1.408(4) . ? C13 C14 1.400(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.458(4) . ? C15 C16 1.508(7) . ? C15 C17 1.520(5) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.241(5) . ? C17 O6 1.263(4) . ? O1 Ni1 2.051(3) 2_747 ? O2 Ni1 2.177(3) 2_747 ? O1W H1A 0.898(10) . ? O1W H1B 0.897(10) . ? O2W H2A 0.895(10) . ? O2W H2B 0.895(10) . ? 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 O6 Ni1 O1W 93.95(11) . . ? O6 Ni1 O2W 94.37(13) . . ? O1W Ni1 O2W 92.33(12) . . ? O6 Ni1 O1 159.86(11) . 2_757 ? O1W Ni1 O1 98.56(11) . 2_757 ? O2W Ni1 O1 100.79(13) . 2_757 ? O6 Ni1 O4 77.27(10) . . ? O1W Ni1 O4 171.18(12) . . ? O2W Ni1 O4 89.30(14) . . ? O1 Ni1 O4 89.64(10) 2_757 . ? O6 Ni1 O2 101.78(11) . 2_757 ? O1W Ni1 O2 92.34(11) . 2_757 ? O2W Ni1 O2 162.82(11) . 2_757 ? O1 Ni1 O2 62.16(12) 2_757 2_757 ? O4 Ni1 O2 88.60(11) . 2_757 ? O6 Ni1 C1 131.09(14) . 2_757 ? O1W Ni1 C1 98.78(12) . 2_757 ? O2W Ni1 C1 131.68(14) . 2_757 ? O1 Ni1 C1 31.17(15) 2_757 2_757 ? O4 Ni1 C1 86.54(12) . 2_757 ? O2 Ni1 C1 31.15(13) 2_757 2_757 ? O1 C1 O2 119.4(4) . . ? O1 C1 C2 119.0(4) . . ? O2 C1 C2 121.5(4) . . ? O1 C1 Ni1 57.1(2) . 2_747 ? O2 C1 Ni1 62.8(2) . 2_747 ? C2 C1 Ni1 170.7(3) . 2_747 ? C7 C2 C3 118.9(4) . . ? C7 C2 C1 122.7(4) . . ? C3 C2 C1 118.4(4) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.3(4) . . ? C4 C5 C8 122.9(4) . . ? C6 C5 C8 118.8(4) . . ? C5 C6 C7 121.4(4) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C2 C7 C6 119.9(4) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O3 C8 C5 108.5(4) . . ? O3 C8 H8A 110.0 . . ? C5 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C5 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C14 C9 C10 121.2(4) . . ? C14 C9 O3 123.3(4) . . ? C10 C9 O3 115.4(4) . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.0(4) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 121.8(4) . . ? C13 C12 O4 119.2(4) . . ? C11 C12 O4 118.9(4) . . ? C12 C13 C14 118.6(4) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C9 C14 C13 119.6(4) . . ? C9 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? O4 C15 C16 111.0(4) . . ? O4 C15 C17 105.8(3) . . ? C16 C15 C17 111.4(3) . . ? O4 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? C17 C15 H15 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 123.7(4) . . ? O5 C17 C15 117.9(3) . . ? O6 C17 C15 118.5(3) . . ? C1 O1 Ni1 91.7(3) . 2_747 ? C1 O2 Ni1 86.0(3) . 2_747 ? C9 O3 C8 117.5(3) . . ? C12 O4 C15 117.7(2) . . ? C12 O4 Ni1 128.3(2) . . ? C15 O4 Ni1 113.82(17) . . ? C17 O6 Ni1 119.8(2) . . ? Ni1 O1W H1A 119(3) . . ? Ni1 O1W H1B 116(3) . . ? H1A O1W H1B 101(4) . . ? Ni1 O2W H2A 115(4) . . ? Ni1 O2W H2B 105(3) . . ? H2A O2W H2B 122(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 148.7(4) . . . . ? O2 C1 C2 C7 -32.9(6) . . . . ? Ni1 C1 C2 C7 -148.6(19) 2_747 . . . ? O1 C1 C2 C3 -31.8(6) . . . . ? O2 C1 C2 C3 146.6(4) . . . . ? Ni1 C1 C2 C3 31(2) 2_747 . . . ? C7 C2 C3 C4 0.2(6) . . . . ? C1 C2 C3 C4 -179.3(4) . . . . ? C2 C3 C4 C5 -3.0(7) . . . . ? C3 C4 C5 C6 2.1(6) . . . . ? C3 C4 C5 C8 -178.6(4) . . . . ? C4 C5 C6 C7 1.5(6) . . . . ? C8 C5 C6 C7 -177.8(4) . . . . ? C3 C2 C7 C6 3.3(6) . . . . ? C1 C2 C7 C6 -177.2(4) . . . . ? C5 C6 C7 C2 -4.3(6) . . . . ? C4 C5 C8 O3 9.5(6) . . . . ? C6 C5 C8 O3 -171.2(4) . . . . ? C14 C9 C10 C11 3.2(7) . . . . ? O3 C9 C10 C11 -177.2(4) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C10 C11 C12 C13 -2.3(7) . . . . ? C10 C11 C12 O4 172.7(4) . . . . ? C11 C12 C13 C14 2.1(6) . . . . ? O4 C12 C13 C14 -172.9(4) . . . . ? C10 C9 C14 C13 -3.4(7) . . . . ? O3 C9 C14 C13 177.0(4) . . . . ? C12 C13 C14 C9 0.8(6) . . . . ? O4 C15 C17 O5 -159.7(4) . . . . ? C16 C15 C17 O5 79.6(5) . . . . ? O4 C15 C17 O6 21.1(6) . . . . ? C16 C15 C17 O6 -99.7(4) . . . . ? O2 C1 O1 Ni1 -8.2(4) . . . 2_747 ? C2 C1 O1 Ni1 170.2(3) . . . 2_747 ? O1 C1 O2 Ni1 7.8(4) . . . 2_747 ? C2 C1 O2 Ni1 -170.6(4) . . . 2_747 ? C14 C9 O3 C8 -20.7(6) . . . . ? C10 C9 O3 C8 159.7(4) . . . . ? C5 C8 O3 C9 -166.3(3) . . . . ? C13 C12 O4 C15 -72.1(6) . . . . ? C11 C12 O4 C15 112.8(5) . . . . ? C13 C12 O4 Ni1 114.1(4) . . . . ? C11 C12 O4 Ni1 -61.1(5) . . . . ? C16 C15 O4 C12 -76.9(4) . . . . ? C17 C15 O4 C12 162.1(4) . . . . ? C16 C15 O4 Ni1 97.8(3) . . . . ? C17 C15 O4 Ni1 -23.2(5) . . . . ? O6 Ni1 O4 C12 -169.7(4) . . . . ? O1W Ni1 O4 C12 -163.6(8) . . . . ? O2W Ni1 O4 C12 95.7(4) . . . . ? O1 Ni1 O4 C12 -5.1(4) 2_757 . . . ? O2 Ni1 O4 C12 -67.3(4) 2_757 . . . ? C1 Ni1 O4 C12 -36.2(4) 2_757 . . . ? O6 Ni1 O4 C15 16.3(3) . . . . ? O1W Ni1 O4 C15 22.4(11) . . . . ? O2W Ni1 O4 C15 -78.4(3) . . . . ? O1 Ni1 O4 C15 -179.2(3) 2_757 . . . ? O2 Ni1 O4 C15 118.7(3) 2_757 . . . ? C1 Ni1 O4 C15 149.8(4) 2_757 . . . ? O5 C17 O6 Ni1 172.1(3) . . . . ? C15 C17 O6 Ni1 -8.7(5) . . . . ? O1W Ni1 O6 C17 176.8(3) . . . . ? O2W Ni1 O6 C17 84.1(3) . . . . ? O1 Ni1 O6 C17 -54.8(5) 2_757 . . . ? O4 Ni1 O6 C17 -4.1(3) . . . . ? O2 Ni1 O6 C17 -90.0(3) 2_757 . . . ? C1 Ni1 O6 C17 -77.9(3) 2_757 . . . ? 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 O1W H1A O5 0.898(10) 1.874(17) 2.742(4) 162(4) 1_655 O1W H1B O5 0.897(10) 1.885(15) 2.768(4) 167(5) 2_646 O2W H2A O6 0.895(10) 1.869(16) 2.745(4) 166(4) 2_646 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.394 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.062 #=========================END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 877932' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 Co O8' _chemical_formula_sum 'C17 H18 Co O8' _chemical_formula_weight 409.24 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.6746(5) _cell_length_b 5.8610(3) _cell_length_c 19.3632(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.186(6) _cell_angle_gamma 90.00 _cell_volume 854.43(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3389 _cell_measurement_theta_min 3.1033 _cell_measurement_theta_max 29.1454 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7371 _exptl_absorpt_correction_T_max 0.8338 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5381 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2869 _reflns_number_gt 2665 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0170P)^2^+0.0000P] 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' _refine_ls_abs_structure_Flack -0.004(13) _refine_ls_number_reflns 2869 _refine_ls_number_parameters 247 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _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 Co1 Co 0.33165(5) 0.84615(6) 0.385566(15) 0.02413(11) Uani 1 1 d U . . C1 C 0.1343(4) 1.0321(6) 0.28448(14) 0.0266(7) Uani 1 1 d . . . C2 C 0.0276(4) 1.1140(5) 0.21596(13) 0.0248(7) Uani 1 1 d . . . C3 C 0.0018(4) 0.9690(5) 0.15855(14) 0.0323(7) Uani 1 1 d . . . H3 H 0.0504 0.8232 0.1633 0.039 Uiso 1 1 calc R . . C4 C -0.0943(4) 1.0373(5) 0.09480(14) 0.0342(8) Uani 1 1 d . . . H4 H -0.1063 0.9396 0.0563 0.041 Uiso 1 1 calc R . . C5 C -0.1740(4) 1.2507(5) 0.08696(14) 0.0287(7) Uani 1 1 d . . . C6 C -0.1486(4) 1.3942(5) 0.14461(13) 0.0304(7) Uani 1 1 d . . . H6 H -0.2030 1.5367 0.1406 0.036 Uiso 1 1 calc R . . C7 C -0.0446(4) 1.3311(6) 0.20798(12) 0.0294(6) Uani 1 1 d . . . H7 H -0.0229 1.4340 0.2452 0.035 Uiso 1 1 calc R . . C8 C -0.2852(4) 1.3320(7) 0.01812(12) 0.0372(7) Uani 1 1 d . . . H8A H -0.3983 1.3899 0.0259 0.045 Uiso 1 1 calc R . . H8B H -0.2243 1.4541 -0.0013 0.045 Uiso 1 1 calc R . . C9 C -0.3794(4) 1.1944(5) -0.09960(13) 0.0289(7) Uani 1 1 d . . . C10 C -0.3519(4) 1.0285(5) -0.14652(13) 0.0338(8) Uani 1 1 d . . . H10 H -0.2967 0.8922 -0.1302 0.041 Uiso 1 1 calc R . . C11 C -0.4071(4) 1.0652(5) -0.21866(14) 0.0335(8) Uani 1 1 d . . . H11 H -0.3904 0.9534 -0.2508 0.040 Uiso 1 1 calc R . . C12 C -0.4859(4) 1.2676(5) -0.24124(13) 0.0274(7) Uani 1 1 d . . . C13 C -0.5191(4) 1.4312(5) -0.19499(14) 0.0343(8) Uani 1 1 d . . . H13 H -0.5764 1.5661 -0.2113 0.041 Uiso 1 1 calc R . . C14 C -0.4651(4) 1.3921(5) -0.12273(13) 0.0337(8) Uani 1 1 d . . . H14 H -0.4877 1.5006 -0.0905 0.040 Uiso 1 1 calc R . . C15 C -0.7054(3) 1.3324(7) -0.34865(12) 0.0278(6) Uani 1 1 d . . . H15 H -0.7714 1.4180 -0.3187 0.033 Uiso 1 1 calc R . . C16 C -0.7870(5) 1.0992(6) -0.36353(16) 0.0428(9) Uani 1 1 d . . . H16A H -0.7848 1.0201 -0.3199 0.064 Uiso 1 1 calc R . . H16B H -0.7207 1.0141 -0.3920 0.064 Uiso 1 1 calc R . . H16C H -0.9077 1.1149 -0.3881 0.064 Uiso 1 1 calc R . . C17 C -0.7069(4) 1.4643(5) -0.41677(14) 0.0272(7) Uani 1 1 d . . . O1 O 0.1380(3) 0.8228(4) 0.29701(8) 0.0317(5) Uani 1 1 d . . . O2 O 0.2219(3) 1.1694(4) 0.32802(9) 0.0361(5) Uani 1 1 d U . . O3 O -0.3135(3) 1.1448(3) -0.02948(9) 0.0404(6) Uani 1 1 d . . . O4 O -0.5218(3) 1.3139(4) -0.31402(8) 0.0325(5) Uani 1 1 d . . . O5 O -0.8477(3) 1.5526(4) -0.44648(10) 0.0381(5) Uani 1 1 d . . . O6 O -0.5627(3) 1.4747(3) -0.43974(9) 0.0298(5) Uani 1 1 d . . . O1W O 0.1884(3) 0.9040(3) 0.46204(10) 0.0350(6) Uani 1 1 d D . . H1A H 0.182(5) 0.787(4) 0.4916(13) 0.053 Uiso 1 1 d D . . H1B H 0.080(2) 0.966(6) 0.4521(16) 0.053 Uiso 1 1 d D . . O2W O 0.3776(4) 0.5140(3) 0.41474(10) 0.0407(6) Uani 1 1 d D . . H2A H 0.397(5) 0.477(6) 0.4606(7) 0.061 Uiso 1 1 d D . . H2B H 0.309(4) 0.401(4) 0.3947(15) 0.061 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0246(2) 0.02896(19) 0.01698(16) 0.00022(19) -0.00055(13) -0.0007(2) C1 0.0220(18) 0.0370(18) 0.0200(13) 0.0016(14) 0.0023(12) -0.0018(14) C2 0.0239(18) 0.0302(16) 0.0181(13) 0.0015(12) -0.0012(12) 0.0004(13) C3 0.036(2) 0.0265(16) 0.0311(16) -0.0017(13) -0.0012(14) 0.0064(15) C4 0.042(2) 0.0375(19) 0.0192(14) -0.0064(14) -0.0029(14) 0.0068(17) C5 0.0279(19) 0.0373(17) 0.0196(14) 0.0054(12) 0.0016(12) -0.0019(14) C6 0.0328(19) 0.027(2) 0.0291(14) -0.0005(12) 0.0011(12) 0.0056(14) C7 0.0368(17) 0.0303(14) 0.0197(12) -0.0013(16) 0.0023(11) -0.002(2) C8 0.0438(19) 0.0453(17) 0.0193(12) 0.0023(18) -0.0015(11) 0.014(2) C9 0.036(2) 0.0345(18) 0.0149(14) 0.0039(13) 0.0017(13) -0.0027(15) C10 0.044(2) 0.0297(17) 0.0248(15) 0.0075(13) -0.0018(14) 0.0038(16) C11 0.043(2) 0.0343(18) 0.0206(14) -0.0042(13) 0.0010(13) -0.0003(16) C12 0.0260(18) 0.0393(18) 0.0166(13) 0.0050(12) 0.0032(12) 0.0020(13) C13 0.038(2) 0.0389(18) 0.0238(15) 0.0049(13) 0.0006(13) 0.0124(15) C14 0.043(2) 0.036(2) 0.0198(13) -0.0020(13) 0.0001(12) 0.0100(16) C15 0.0233(15) 0.0406(16) 0.0190(11) 0.0024(17) 0.0025(10) -0.0013(19) C16 0.037(2) 0.052(2) 0.0382(17) 0.0169(16) 0.0027(15) -0.0077(17) C17 0.027(2) 0.0296(15) 0.0235(14) 0.0004(12) 0.0018(14) -0.0027(14) O1 0.0362(12) 0.0318(13) 0.0229(9) 0.0034(10) -0.0045(8) -0.0002(12) O2 0.0462(16) 0.0326(11) 0.0228(10) 0.0022(8) -0.0102(10) -0.0043(10) O3 0.0615(18) 0.0354(13) 0.0178(10) 0.0040(9) -0.0082(10) -0.0013(12) O4 0.0259(11) 0.0569(15) 0.0133(8) 0.0032(10) 0.0006(7) 0.0056(12) O5 0.0226(13) 0.0522(14) 0.0374(11) 0.0178(11) 0.0004(10) 0.0022(11) O6 0.0234(13) 0.0453(12) 0.0196(9) 0.0090(9) 0.0018(9) 0.0035(10) O1W 0.0289(13) 0.0486(17) 0.0287(10) 0.0083(9) 0.0085(9) 0.0092(11) O2W 0.0646(18) 0.0301(13) 0.0237(10) 0.0018(10) -0.0005(11) -0.0024(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co1 O6 2.023(2) 2_545 ? Co1 O1W 2.0366(17) . ? Co1 O2W 2.039(2) . ? Co1 O1 2.0441(18) . ? Co1 O4 2.2066(16) 2_545 ? Co1 O2 2.275(2) . ? Co1 C1 2.482(3) . ? C1 O1 1.250(4) . ? C1 O2 1.261(3) . ? C1 C2 1.497(4) . ? C2 C3 1.382(4) . ? C2 C7 1.385(4) . ? C3 C4 1.369(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.381(4) . ? C5 C8 1.514(4) . ? C6 C7 1.378(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.422(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.365(4) . ? C9 C10 1.375(4) . ? C9 O3 1.385(3) . ? C10 C11 1.395(4) . ? C10 H10 0.9300 . ? C11 C12 1.365(4) . ? C11 H11 0.9300 . ? C12 C13 1.369(4) . ? C12 O4 1.409(3) . ? C13 C14 1.399(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.442(3) . ? C15 C16 1.508(5) . ? C15 C17 1.527(4) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.235(4) . ? C17 O6 1.271(3) . ? O4 Co1 2.2066(16) 2 ? O6 Co1 2.023(2) 2 ? O1W H1A 0.901(10) . ? O1W H1B 0.893(10) . ? O2W H2A 0.897(10) . ? O2W H2B 0.887(10) . ? 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 O6 Co1 O1W 95.94(8) 2_545 . ? O6 Co1 O2W 97.16(9) 2_545 . ? O1W Co1 O2W 92.66(8) . . ? O6 Co1 O1 151.83(8) 2_545 . ? O1W Co1 O1 102.36(8) . . ? O2W Co1 O1 103.12(10) . . ? O6 Co1 O4 74.77(7) 2_545 2_545 ? O1W Co1 O4 170.66(9) . 2_545 ? O2W Co1 O4 89.56(9) . 2_545 ? O1 Co1 O4 85.95(7) . 2_545 ? O6 Co1 O2 98.50(8) 2_545 . ? O1W Co1 O2 90.96(8) . . ? O2W Co1 O2 163.46(8) . . ? O1 Co1 O2 60.34(8) . . ? O4 Co1 O2 89.47(8) 2_545 . ? O6 Co1 C1 125.79(10) 2_545 . ? O1W Co1 C1 99.64(9) . . ? O2W Co1 C1 133.16(10) . . ? O1 Co1 C1 30.11(9) . . ? O4 Co1 C1 85.36(8) 2_545 . ? O2 Co1 C1 30.35(8) . . ? O1 C1 O2 120.5(3) . . ? O1 C1 C2 118.4(3) . . ? O2 C1 C2 121.1(3) . . ? O1 C1 Co1 55.15(15) . . ? O2 C1 Co1 65.70(15) . . ? C2 C1 Co1 170.1(2) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 C1 119.0(3) . . ? C7 C2 C1 122.1(2) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C8 119.1(3) . . ? C4 C5 C8 122.8(3) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C2 119.7(3) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? O3 C8 C5 108.5(3) . . ? O3 C8 H8A 110.0 . . ? C5 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C5 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C14 C9 C10 120.6(2) . . ? C14 C9 O3 124.1(2) . . ? C10 C9 O3 115.2(3) . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 121.8(2) . . ? C11 C12 O4 118.5(2) . . ? C13 C12 O4 119.6(2) . . ? C12 C13 C14 118.9(3) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C9 C14 C13 119.8(3) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? O4 C15 C16 110.7(3) . . ? O4 C15 C17 106.4(2) . . ? C16 C15 C17 111.1(2) . . ? O4 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? C17 C15 H15 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 124.0(2) . . ? O5 C17 C15 118.3(2) . . ? O6 C17 C15 117.7(3) . . ? C1 O1 Co1 94.74(18) . . ? C1 O2 Co1 83.95(17) . . ? C9 O3 C8 117.0(2) . . ? C12 O4 C15 117.60(18) . . ? C12 O4 Co1 128.29(16) . 2 ? C15 O4 Co1 114.02(12) . 2 ? C17 O6 Co1 122.39(17) . 2 ? Co1 O1W H1A 116(2) . . ? Co1 O1W H1B 121(2) . . ? H1A O1W H1B 106(3) . . ? Co1 O2W H2A 119(2) . . ? Co1 O2W H2B 122(2) . . ? H2A O2W H2B 103(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Co1 C1 O1 157.37(14) 2_545 . . . ? O1W Co1 C1 O1 -98.04(17) . . . . ? O2W Co1 C1 O1 4.9(2) . . . . ? O4 Co1 C1 O1 89.91(17) 2_545 . . . ? O2 Co1 C1 O1 -173.2(3) . . . . ? O6 Co1 C1 O2 -29.4(2) 2_545 . . . ? O1W Co1 C1 O2 75.15(17) . . . . ? O2W Co1 C1 O2 178.07(15) . . . . ? O1 Co1 C1 O2 173.2(3) . . . . ? O4 Co1 C1 O2 -96.90(17) 2_545 . . . ? O6 Co1 C1 C2 105.8(13) 2_545 . . . ? O1W Co1 C1 C2 -149.6(13) . . . . ? O2W Co1 C1 C2 -46.6(13) . . . . ? O1 Co1 C1 C2 -51.5(12) . . . . ? O4 Co1 C1 C2 38.4(13) 2_545 . . . ? O2 Co1 C1 C2 135.3(14) . . . . ? O1 C1 C2 C3 -27.6(4) . . . . ? O2 C1 C2 C3 150.8(3) . . . . ? Co1 C1 C2 C3 19.3(14) . . . . ? O1 C1 C2 C7 153.2(3) . . . . ? O2 C1 C2 C7 -28.5(4) . . . . ? Co1 C1 C2 C7 -160.0(11) . . . . ? C7 C2 C3 C4 -0.4(5) . . . . ? C1 C2 C3 C4 -179.7(3) . . . . ? C2 C3 C4 C5 -2.5(5) . . . . ? C3 C4 C5 C6 2.1(5) . . . . ? C3 C4 C5 C8 -178.5(3) . . . . ? C4 C5 C6 C7 1.3(4) . . . . ? C8 C5 C6 C7 -178.2(3) . . . . ? C5 C6 C7 C2 -4.2(4) . . . . ? C3 C2 C7 C6 3.7(4) . . . . ? C1 C2 C7 C6 -177.0(3) . . . . ? C6 C5 C8 O3 -171.5(3) . . . . ? C4 C5 C8 O3 9.1(4) . . . . ? C14 C9 C10 C11 2.0(5) . . . . ? O3 C9 C10 C11 -177.6(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C10 C11 C12 C13 -2.9(5) . . . . ? C10 C11 C12 O4 172.5(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? O4 C12 C13 C14 -173.2(3) . . . . ? C10 C9 C14 C13 -2.8(5) . . . . ? O3 C9 C14 C13 176.8(3) . . . . ? C12 C13 C14 C9 0.7(5) . . . . ? O4 C15 C17 O5 -161.6(3) . . . . ? C16 C15 C17 O5 77.8(4) . . . . ? O4 C15 C17 O6 19.0(4) . . . . ? C16 C15 C17 O6 -101.6(3) . . . . ? O2 C1 O1 Co1 -7.2(3) . . . . ? C2 C1 O1 Co1 171.2(2) . . . . ? O6 Co1 O1 C1 -41.4(3) 2_545 . . . ? O1W Co1 O1 C1 87.93(17) . . . . ? O2W Co1 O1 C1 -176.34(17) . . . . ? O4 Co1 O1 C1 -87.75(18) 2_545 . . . ? O2 Co1 O1 C1 3.96(16) . . . . ? O1 C1 O2 Co1 6.5(3) . . . . ? C2 C1 O2 Co1 -171.9(2) . . . . ? O6 Co1 O2 C1 156.22(17) 2_545 . . . ? O1W Co1 O2 C1 -107.62(17) . . . . ? O2W Co1 O2 C1 -4.9(4) . . . . ? O1 Co1 O2 C1 -3.93(16) . . . . ? O4 Co1 O2 C1 81.71(17) 2_545 . . . ? C14 C9 O3 C8 -19.7(4) . . . . ? C10 C9 O3 C8 159.9(3) . . . . ? C5 C8 O3 C9 -166.6(2) . . . . ? C11 C12 O4 C15 114.7(3) . . . . ? C13 C12 O4 C15 -69.8(4) . . . . ? C11 C12 O4 Co1 -61.8(4) . . . 2 ? C13 C12 O4 Co1 113.7(3) . . . 2 ? C16 C15 O4 C12 -79.3(3) . . . . ? C17 C15 O4 C12 159.8(2) . . . . ? C16 C15 O4 Co1 97.7(2) . . . 2 ? C17 C15 O4 Co1 -23.2(3) . . . 2 ? O5 C17 O6 Co1 175.6(2) . . . 2 ? C15 C17 O6 Co1 -5.0(3) . . . 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 O1W H1A O5 0.901(10) 1.866(11) 2.765(3) 176(3) 1_646 O1W H1B O5 0.893(10) 1.838(12) 2.717(3) 168(3) 2_445 O2W H2A O6 0.897(10) 1.895(13) 2.775(3) 166(3) 1_646 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.281 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.044 #=========================END data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 877933' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H16 Cd O7' _chemical_formula_sum 'C17 H16 Cd O7' _chemical_formula_weight 444.70 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' 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_hall C2y 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' _cell_length_a 18.3690(12) _cell_length_b 6.1110(3) _cell_length_c 15.1160(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.078(6) _cell_angle_gamma 90.00 _cell_volume 1675.56(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1399 _cell_measurement_theta_min 3.2433 _cell_measurement_theta_max 29.1028 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9360 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3250 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2458 _reflns_number_gt 2187 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0153P)^2^+0.0000P] 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' _refine_ls_abs_structure_Flack -0.11(5) _refine_ls_number_reflns 2458 _refine_ls_number_parameters 232 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.22864(3) 0.27088(15) 0.06601(3) 0.03367(17) Uani 1 1 d . . . C1 C 0.6400(4) 0.242(3) 0.8152(5) 0.039(3) Uani 1 1 d . . . C2 C 0.5738(4) 0.2324(19) 0.7446(5) 0.038(3) Uani 1 1 d . . . C3 C 0.5294(5) 0.4079(15) 0.7259(6) 0.051(3) Uani 1 1 d . . . H3 H 0.5402 0.5374 0.7576 0.061 Uiso 1 1 calc R . . C4 C 0.4676(5) 0.3966(14) 0.6594(6) 0.042(2) Uani 1 1 d . . . H4 H 0.4375 0.5188 0.6470 0.050 Uiso 1 1 calc R . . C5 C 0.4506(5) 0.2054(14) 0.6120(6) 0.041(3) Uani 1 1 d . . . C6 C 0.4957(5) 0.0259(14) 0.6313(6) 0.043(2) Uani 1 1 d . . . H6 H 0.4845 -0.1036 0.5998 0.051 Uiso 1 1 calc R . . C7 C 0.5575(5) 0.0352(14) 0.6970(6) 0.044(2) Uani 1 1 d . . . H7 H 0.5877 -0.0866 0.7095 0.052 Uiso 1 1 calc R . . C8 C 0.3817(6) 0.1872(16) 0.5412(6) 0.048(3) Uani 1 1 d . . . H8A H 0.3904 0.0847 0.4950 0.058 Uiso 1 1 calc R . . H8B H 0.3408 0.1334 0.5685 0.058 Uiso 1 1 calc R . . C9 C 0.3110(4) 0.3988(14) 0.4268(5) 0.037(2) Uani 1 1 d . . . C10 C 0.3094(5) 0.5882(12) 0.3782(6) 0.040(2) Uani 1 1 d . . . H10 H 0.3406 0.7031 0.3991 0.048 Uiso 1 1 calc R . . C11 C 0.2613(5) 0.6105(13) 0.2979(5) 0.041(2) Uani 1 1 d . . . H11 H 0.2601 0.7389 0.2647 0.050 Uiso 1 1 calc R . . C12 C 0.2151(4) 0.4356(12) 0.2683(5) 0.0278(17) Uani 1 1 d . . . C13 C 0.2156(4) 0.247(2) 0.3186(5) 0.039(2) Uani 1 1 d . . . H13 H 0.1829 0.1347 0.2995 0.047 Uiso 1 1 calc R . . C14 C 0.2654(4) 0.2253(12) 0.3983(5) 0.037(2) Uani 1 1 d . . . H14 H 0.2677 0.0963 0.4313 0.044 Uiso 1 1 calc R . . C15 C 0.1322(4) 0.6378(13) 0.1563(6) 0.038(2) Uani 1 1 d . . . H15 H 0.1285 0.7296 0.2085 0.045 Uiso 1 1 calc R . . C16 C 0.0559(4) 0.5802(14) 0.1098(6) 0.053(3) Uani 1 1 d . . . H16A H 0.0303 0.5012 0.1504 0.079 Uiso 1 1 calc R . . H16B H 0.0594 0.4909 0.0584 0.079 Uiso 1 1 calc R . . H16C H 0.0293 0.7119 0.0911 0.079 Uiso 1 1 calc R . . C17 C 0.1740(3) 0.760(2) 0.0936(4) 0.0285(15) Uani 1 1 d . . . O1 O 0.6552(4) 0.4142(13) 0.8589(5) 0.055(2) Uani 1 1 d . . . O2 O 0.6815(4) 0.0775(11) 0.8307(5) 0.048(2) Uani 1 1 d . . . O3 O 0.3646(4) 0.3922(11) 0.5036(4) 0.056(2) Uani 1 1 d . . . O4 O 0.1680(3) 0.4335(8) 0.1859(3) 0.0375(13) Uani 1 1 d . . . O5 O 0.1656(3) 0.9613(10) 0.0894(4) 0.0427(14) Uani 1 1 d . . . O6 O 0.2110(3) 0.6465(8) 0.0462(3) 0.0341(13) Uani 1 1 d . . . O1W O 0.1298(3) 0.2894(18) -0.0512(4) 0.0446(14) Uani 1 1 d D . . H1A H 0.132(5) 0.367(11) -0.101(3) 0.067 Uiso 1 1 d D . . H1B H 0.128(6) 0.151(6) -0.071(6) 0.067 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0394(3) 0.0300(3) 0.0311(3) 0.0003(4) 0.0037(2) 0.0028(5) C1 0.035(4) 0.049(8) 0.035(4) -0.004(6) 0.008(3) 0.001(7) C2 0.037(4) 0.053(9) 0.026(4) 0.013(5) 0.011(3) -0.009(5) C3 0.067(7) 0.037(6) 0.044(6) 0.003(5) -0.006(5) 0.006(5) C4 0.039(5) 0.025(5) 0.056(7) 0.001(5) -0.007(5) 0.008(4) C5 0.030(4) 0.059(8) 0.032(5) 0.009(4) -0.005(4) -0.007(4) C6 0.046(6) 0.028(5) 0.051(6) -0.004(4) -0.001(5) 0.001(4) C7 0.041(5) 0.041(5) 0.045(6) 0.008(5) -0.003(5) 0.021(4) C8 0.051(6) 0.051(7) 0.040(6) 0.007(5) 0.001(5) -0.004(5) C9 0.038(5) 0.053(6) 0.018(4) -0.001(4) -0.001(4) -0.003(4) C10 0.048(5) 0.028(5) 0.043(5) -0.003(4) 0.008(4) -0.012(4) C11 0.049(5) 0.042(5) 0.029(5) 0.005(4) -0.004(4) -0.006(4) C12 0.030(4) 0.025(4) 0.028(4) -0.004(4) 0.005(4) -0.003(4) C13 0.032(4) 0.045(7) 0.036(4) 0.000(6) -0.002(3) 0.010(6) C14 0.050(5) 0.019(7) 0.040(5) 0.003(4) 0.000(4) -0.008(4) C15 0.041(5) 0.045(5) 0.029(5) 0.013(4) 0.009(4) 0.002(4) C16 0.044(6) 0.061(6) 0.056(6) 0.007(5) 0.016(5) 0.011(5) C17 0.021(3) 0.033(4) 0.028(3) -0.007(7) -0.008(3) -0.006(7) O1 0.060(5) 0.052(5) 0.048(5) -0.009(4) -0.007(4) 0.002(4) O2 0.044(4) 0.050(5) 0.047(4) 0.002(3) -0.003(3) -0.002(4) O3 0.076(5) 0.043(4) 0.041(4) 0.008(3) -0.016(4) 0.003(4) O4 0.049(3) 0.025(3) 0.036(3) 0.001(2) -0.002(3) 0.002(3) O5 0.053(4) 0.029(3) 0.044(4) 0.000(3) 0.003(3) 0.003(3) O6 0.042(3) 0.038(3) 0.026(3) 0.007(3) 0.015(3) 0.014(3) O1W 0.050(3) 0.037(4) 0.043(3) 0.000(5) -0.005(2) -0.003(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.275(6) 1_545 ? Cd1 O6 2.297(5) 4_545 ? Cd1 O6 2.331(5) . ? Cd1 O1W 2.332(5) . ? Cd1 O2 2.397(7) 2_656 ? Cd1 O1 2.417(7) 2_656 ? Cd1 O4 2.480(5) . ? C1 O1 1.251(15) . ? C1 O2 1.262(14) . ? C1 C2 1.486(10) . ? C2 C3 1.350(13) . ? C2 C7 1.411(14) . ? C3 C4 1.394(12) . ? C3 H3 0.9300 . ? C4 C5 1.381(11) . ? C4 H4 0.9300 . ? C5 C6 1.378(12) . ? C5 C8 1.526(11) . ? C6 C7 1.387(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.391(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.369(11) . ? C9 C14 1.377(10) . ? C9 O3 1.399(9) . ? C10 C11 1.390(10) . ? C10 H10 0.9300 . ? C11 C12 1.395(10) . ? C11 H11 0.9300 . ? C12 C13 1.377(15) . ? C12 O4 1.400(8) . ? C13 C14 1.400(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.449(9) . ? C15 C17 1.507(12) . ? C15 C16 1.508(11) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.241(15) . ? C17 O6 1.269(10) . ? O1 Cd1 2.417(7) 2_656 ? O2 Cd1 2.397(7) 2_656 ? O5 Cd1 2.275(6) 1_565 ? O6 Cd1 2.297(5) 4 ? O1W H1A 0.897(10) . ? O1W H1B 0.897(10) . ? 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 O6 99.0(2) 1_545 4_545 ? O5 Cd1 O6 140.8(2) 1_545 . ? O6 Cd1 O6 107.73(15) 4_545 . ? O5 Cd1 O1W 78.7(3) 1_545 . ? O6 Cd1 O1W 82.2(2) 4_545 . ? O6 Cd1 O1W 77.2(3) . . ? O5 Cd1 O2 78.7(2) 1_545 2_656 ? O6 Cd1 O2 87.4(2) 4_545 2_656 ? O6 Cd1 O2 129.6(2) . 2_656 ? O1W Cd1 O2 153.2(3) . 2_656 ? O5 Cd1 O1 131.4(2) 1_545 2_656 ? O6 Cd1 O1 88.5(2) 4_545 2_656 ? O6 Cd1 O1 78.4(2) . 2_656 ? O1W Cd1 O1 149.7(3) . 2_656 ? O2 Cd1 O1 53.6(2) 2_656 2_656 ? O5 Cd1 O4 85.47(19) 1_545 . ? O6 Cd1 O4 175.51(18) 4_545 . ? O6 Cd1 O4 68.28(18) . . ? O1W Cd1 O4 98.6(2) . . ? O2 Cd1 O4 93.7(2) 2_656 . ? O1 Cd1 O4 88.7(2) 2_656 . ? O1 C1 O2 119.5(7) . . ? O1 C1 C2 120.2(11) . . ? O2 C1 C2 120.2(11) . . ? C3 C2 C7 119.9(8) . . ? C3 C2 C1 121.1(10) . . ? C7 C2 C1 118.9(10) . . ? C2 C3 C4 120.5(9) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.5(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 119.0(8) . . ? C6 C5 C8 119.7(8) . . ? C4 C5 C8 121.3(8) . . ? C5 C6 C7 121.1(8) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.0(8) . . ? C6 C7 H7 120.5 . . ? C2 C7 H7 120.5 . . ? O3 C8 C5 109.2(7) . . ? O3 C8 H8A 109.8 . . ? C5 C8 H8A 109.8 . . ? O3 C8 H8B 109.8 . . ? C5 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C14 121.5(7) . . ? C10 C9 O3 115.0(7) . . ? C14 C9 O3 123.4(8) . . ? C9 C10 C11 120.6(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 118.4(7) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C13 C12 C11 120.8(7) . . ? C13 C12 O4 115.7(7) . . ? C11 C12 O4 123.5(7) . . ? C12 C13 C14 120.2(10) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 118.5(9) . . ? C9 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? O4 C15 C17 111.7(7) . . ? O4 C15 C16 106.6(7) . . ? C17 C15 C16 110.5(6) . . ? O4 C15 H15 109.3 . . ? C17 C15 H15 109.3 . . ? C16 C15 H15 109.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 125.9(9) . . ? O5 C17 C15 116.9(8) . . ? O6 C17 C15 117.1(11) . . ? C1 O1 Cd1 92.9(6) . 2_656 ? C1 O2 Cd1 93.6(6) . 2_656 ? C8 O3 C9 116.7(7) . . ? C12 O4 C15 116.9(6) . . ? C12 O4 Cd1 111.6(4) . . ? C15 O4 Cd1 110.7(4) . . ? C17 O5 Cd1 140.4(5) . 1_565 ? C17 O6 Cd1 126.9(7) . 4 ? C17 O6 Cd1 122.8(7) . . ? Cd1 O6 Cd1 110.3(2) 4 . ? Cd1 O1W H1A 122(6) . . ? Cd1 O1W H1B 101(7) . . ? H1A O1W H1B 103(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 0.5(14) . . . . ? O2 C1 C2 C3 -178.8(9) . . . . ? O1 C1 C2 C7 -179.3(9) . . . . ? O2 C1 C2 C7 1.4(13) . . . . ? C7 C2 C3 C4 -0.3(15) . . . . ? C1 C2 C3 C4 179.9(8) . . . . ? C2 C3 C4 C5 0.3(16) . . . . ? C3 C4 C5 C6 0.0(16) . . . . ? C3 C4 C5 C8 177.9(9) . . . . ? C4 C5 C6 C7 -0.2(15) . . . . ? C8 C5 C6 C7 -178.1(9) . . . . ? C5 C6 C7 C2 0.2(14) . . . . ? C3 C2 C7 C6 0.1(14) . . . . ? C1 C2 C7 C6 179.9(8) . . . . ? C6 C5 C8 O3 -152.8(9) . . . . ? C4 C5 C8 O3 29.3(14) . . . . ? C14 C9 C10 C11 -0.2(14) . . . . ? O3 C9 C10 C11 176.5(8) . . . . ? C9 C10 C11 C12 0.1(13) . . . . ? C10 C11 C12 C13 1.6(13) . . . . ? C10 C11 C12 O4 -175.7(8) . . . . ? C11 C12 C13 C14 -3.0(13) . . . . ? O4 C12 C13 C14 174.4(7) . . . . ? C10 C9 C14 C13 -1.2(13) . . . . ? O3 C9 C14 C13 -177.6(8) . . . . ? C12 C13 C14 C9 2.8(12) . . . . ? O4 C15 C17 O5 -154.8(6) . . . . ? C16 C15 C17 O5 86.6(9) . . . . ? O4 C15 C17 O6 29.1(9) . . . . ? C16 C15 C17 O6 -89.4(8) . . . . ? O2 C1 O1 Cd1 5.7(10) . . . 2_656 ? C2 C1 O1 Cd1 -173.6(7) . . . 2_656 ? O1 C1 O2 Cd1 -5.7(10) . . . 2_656 ? C2 C1 O2 Cd1 173.6(7) . . . 2_656 ? C5 C8 O3 C9 169.0(7) . . . . ? C10 C9 O3 C8 -163.4(10) . . . . ? C14 C9 O3 C8 13.2(14) . . . . ? C13 C12 O4 C15 144.9(7) . . . . ? C11 C12 O4 C15 -37.7(10) . . . . ? C13 C12 O4 Cd1 -86.1(7) . . . . ? C11 C12 O4 Cd1 91.2(8) . . . . ? C17 C15 O4 C12 95.8(8) . . . . ? C16 C15 O4 C12 -143.4(7) . . . . ? C17 C15 O4 Cd1 -33.6(7) . . . . ? C16 C15 O4 Cd1 87.3(6) . . . . ? O5 Cd1 O4 C12 99.7(4) 1_545 . . . ? O6 Cd1 O4 C12 -82(2) 4_545 . . . ? O6 Cd1 O4 C12 -110.0(5) . . . . ? O1W Cd1 O4 C12 177.5(5) . . . . ? O2 Cd1 O4 C12 21.4(5) 2_656 . . . ? O1 Cd1 O4 C12 -32.0(5) 2_656 . . . ? O5 Cd1 O4 C15 -128.1(5) 1_545 . . . ? O6 Cd1 O4 C15 50(2) 4_545 . . . ? O6 Cd1 O4 C15 22.1(4) . . . . ? O1W Cd1 O4 C15 -50.3(5) . . . . ? O2 Cd1 O4 C15 153.5(5) 2_656 . . . ? O1 Cd1 O4 C15 100.1(5) 2_656 . . . ? O6 C17 O5 Cd1 -36.1(11) . . . 1_565 ? C15 C17 O5 Cd1 148.2(6) . . . 1_565 ? O5 C17 O6 Cd1 -2.3(9) . . . 4 ? C15 C17 O6 Cd1 173.4(4) . . . 4 ? O5 C17 O6 Cd1 176.2(5) . . . . ? C15 C17 O6 Cd1 -8.2(8) . . . . ? O5 Cd1 O6 C17 43.6(6) 1_545 . . . ? O6 Cd1 O6 C17 174.4(6) 4_545 . . . ? O1W Cd1 O6 C17 97.0(5) . . . . ? O2 Cd1 O6 C17 -84.0(6) 2_656 . . . ? O1 Cd1 O6 C17 -101.1(5) 2_656 . . . ? O4 Cd1 O6 C17 -7.8(5) . . . . ? O5 Cd1 O6 Cd1 -137.6(3) 1_545 . . 4 ? O6 Cd1 O6 Cd1 -6.93(11) 4_545 . . 4 ? O1W Cd1 O6 Cd1 -84.3(2) . . . 4 ? O2 Cd1 O6 Cd1 94.7(3) 2_656 . . 4 ? O1 Cd1 O6 Cd1 77.6(2) 2_656 . . 4 ? O4 Cd1 O6 Cd1 170.9(3) . . . 4 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.850 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.096 #=========================END data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 877934' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H22 Cd N2 O6' _chemical_formula_sum 'C29 H22 Cd N2 O6' _chemical_formula_weight 606.89 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'p 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.2904(3) _cell_length_b 16.5876(5) _cell_length_c 18.3294(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2520.62(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4373 _cell_measurement_theta_min 2.7411 _cell_measurement_theta_max 29.1964 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7647 _exptl_absorpt_correction_T_max 0.8455 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9865 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4428 _reflns_number_gt 3927 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0358P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 4428 _refine_ls_number_parameters 343 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.032 _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 Cd1 Cd 0.08066(4) 0.738136(17) 0.469909(17) 0.03951(11) Uani 1 1 d U . . C1 C 0.0839(7) 0.5756(3) 0.5084(3) 0.0509(12) Uani 1 1 d U . . C2 C 0.0694(6) 0.4848(2) 0.5149(3) 0.0464(12) Uani 1 1 d . . . C3 C 0.1047(8) 0.4464(3) 0.5789(3) 0.0608(15) Uani 1 1 d . . . H3 H 0.1409 0.4762 0.6187 0.073 Uiso 1 1 calc R . . C4 C 0.0871(9) 0.3639(3) 0.5853(3) 0.0676(15) Uani 1 1 d . . . H4 H 0.1118 0.3388 0.6293 0.081 Uiso 1 1 calc R . . C5 C 0.0336(6) 0.3185(2) 0.5275(3) 0.0511(13) Uani 1 1 d . . . C6 C -0.0022(6) 0.3573(3) 0.4630(3) 0.0552(13) Uani 1 1 d . . . H6 H -0.0380 0.3276 0.4232 0.066 Uiso 1 1 calc R . . C7 C 0.0143(6) 0.4397(3) 0.4569(3) 0.0545(14) Uani 1 1 d . . . H7 H -0.0120 0.4650 0.4132 0.065 Uiso 1 1 calc R . . C8 C 0.0036(7) 0.2291(3) 0.5328(3) 0.0613(13) Uani 1 1 d . . . H8A H -0.1110 0.2192 0.5389 0.074 Uiso 1 1 calc R . . H8B H 0.0383 0.2030 0.4882 0.074 Uiso 1 1 calc R . . C9 C 0.0542(6) 0.1181(2) 0.6127(3) 0.0462(13) Uani 1 1 d . . . C10 C 0.1296(7) 0.0908(3) 0.6742(3) 0.0588(15) Uani 1 1 d . . . H10 H 0.2031 0.1240 0.6981 0.071 Uiso 1 1 calc R . . C11 C 0.0986(8) 0.0151(3) 0.7013(3) 0.0541(14) Uani 1 1 d . . . H11 H 0.1487 -0.0023 0.7439 0.065 Uiso 1 1 calc R . . C12 C -0.0081(6) -0.0351(2) 0.6647(3) 0.0407(11) Uani 1 1 d . . . C13 C -0.0782(6) -0.0095(2) 0.6019(2) 0.0430(11) Uani 1 1 d . . . H13 H -0.1463 -0.0439 0.5762 0.052 Uiso 1 1 calc R . . C14 C -0.0484(6) 0.0682(3) 0.5756(3) 0.0481(13) Uani 1 1 d . . . H14 H -0.0983 0.0859 0.5331 0.058 Uiso 1 1 calc R . . C15 C -0.1355(6) -0.1647(3) 0.6597(2) 0.0404(12) Uani 1 1 d . . . H15 H -0.2380 -0.1388 0.6470 0.048 Uiso 1 1 calc R . . C16 C -0.1665(7) -0.2335(3) 0.7123(3) 0.0554(13) Uani 1 1 d . . . H16A H -0.2166 -0.2131 0.7557 0.083 Uiso 1 1 calc R . . H16B H -0.0660 -0.2588 0.7247 0.083 Uiso 1 1 calc R . . H16C H -0.2363 -0.2724 0.6897 0.083 Uiso 1 1 calc R . . C17 C -0.0574(6) -0.1975(2) 0.5918(2) 0.0359(10) Uani 1 1 d . . . C18 C -0.1293(6) 0.6898(3) 0.3213(3) 0.0534(15) Uani 1 1 d . . . H18 H -0.1233 0.6384 0.3413 0.064 Uiso 1 1 calc R . . C19 C -0.2131(7) 0.7001(4) 0.2564(3) 0.0638(16) Uani 1 1 d . . . H19 H -0.2616 0.6562 0.2337 0.077 Uiso 1 1 calc R . . C20 C -0.2237(7) 0.7740(4) 0.2268(3) 0.0701(17) Uani 1 1 d . . . H20 H -0.2785 0.7813 0.1830 0.084 Uiso 1 1 calc R . . C21 C -0.1520(7) 0.8405(4) 0.2618(3) 0.0572(15) Uani 1 1 d . . . C22 C -0.1594(8) 0.9209(4) 0.2342(3) 0.0754(19) Uani 1 1 d . . . H22 H -0.2153 0.9310 0.1911 0.091 Uiso 1 1 calc R . . C23 C -0.0874(9) 0.9820(4) 0.2691(3) 0.0746(17) Uani 1 1 d . . . H23 H -0.0970 1.0340 0.2505 0.089 Uiso 1 1 calc R . . C24 C 0.0025(7) 0.9695(3) 0.3334(3) 0.0575(14) Uani 1 1 d . . . C25 C 0.0831(8) 1.0297(3) 0.3711(3) 0.0643(15) Uani 1 1 d . . . H25 H 0.0778 1.0825 0.3543 0.077 Uiso 1 1 calc R . . C26 C 0.1686(7) 1.0132(3) 0.4316(3) 0.0621(16) Uani 1 1 d . . . H26 H 0.2249 1.0537 0.4558 0.074 Uiso 1 1 calc R . . C27 C 0.1712(6) 0.9333(3) 0.4575(3) 0.0556(14) Uani 1 1 d . . . H27 H 0.2293 0.9218 0.4996 0.067 Uiso 1 1 calc R . . C28 C 0.0120(6) 0.8907(3) 0.3630(3) 0.0453(12) Uani 1 1 d . . . C29 C -0.0677(6) 0.8257(3) 0.3262(2) 0.0438(11) Uani 1 1 d . . . N1 N -0.0567(4) 0.7505(2) 0.35613(19) 0.0441(9) Uani 1 1 d . . . N2 N 0.0953(5) 0.8746(2) 0.4247(2) 0.0447(9) Uani 1 1 d . . . O1 O 0.1346(5) 0.6153(2) 0.5595(2) 0.0758(12) Uani 1 1 d U . . O2 O 0.0429(4) 0.60580(18) 0.4477(2) 0.0608(10) Uani 1 1 d U . . O3 O 0.0886(5) 0.19686(17) 0.5925(2) 0.0657(10) Uani 1 1 d . . . O4 O -0.0352(4) -0.10829(17) 0.69806(16) 0.0480(9) Uani 1 1 d . . . O5 O -0.1482(3) -0.23357(17) 0.54647(16) 0.0417(7) Uani 1 1 d . . . O6 O 0.0893(4) -0.19088(16) 0.58203(16) 0.0418(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04406(18) 0.03063(16) 0.04385(18) 0.00182(14) 0.00174(17) 0.00265(15) C1 0.054(3) 0.030(2) 0.069(3) 0.005(2) 0.003(3) -0.004(3) C2 0.052(3) 0.029(2) 0.059(3) 0.004(2) 0.000(3) -0.002(2) C3 0.083(4) 0.035(2) 0.064(4) 0.001(2) -0.018(4) -0.005(3) C4 0.099(4) 0.039(3) 0.065(3) 0.013(3) -0.022(4) -0.005(4) C5 0.063(3) 0.030(2) 0.061(3) 0.001(3) 0.005(3) -0.001(2) C6 0.076(3) 0.035(2) 0.055(3) -0.003(3) -0.001(3) -0.005(2) C7 0.067(3) 0.039(3) 0.057(3) 0.009(2) -0.002(3) -0.002(2) C8 0.081(3) 0.036(2) 0.067(3) 0.010(3) -0.007(3) -0.007(2) C9 0.055(3) 0.021(2) 0.063(3) 0.000(2) 0.003(3) 0.004(2) C10 0.073(4) 0.030(2) 0.073(4) -0.007(3) -0.018(3) -0.005(3) C11 0.073(4) 0.034(2) 0.056(3) -0.001(2) -0.022(3) -0.001(3) C12 0.053(3) 0.026(2) 0.043(3) -0.004(2) -0.003(2) 0.000(2) C13 0.053(3) 0.029(2) 0.047(3) -0.0066(19) -0.001(3) -0.005(3) C14 0.065(3) 0.029(2) 0.050(3) -0.002(2) -0.002(3) 0.004(2) C15 0.048(3) 0.032(2) 0.042(3) 0.003(2) -0.006(2) -0.006(2) C16 0.076(3) 0.046(3) 0.044(3) 0.005(3) 0.003(3) -0.013(3) C17 0.043(3) 0.0220(19) 0.043(3) 0.0100(19) -0.007(2) 0.003(2) C18 0.054(4) 0.054(3) 0.052(3) 0.001(3) 0.007(3) -0.003(3) C19 0.066(4) 0.074(4) 0.051(4) -0.006(3) -0.003(3) -0.005(3) C20 0.057(3) 0.105(5) 0.048(3) 0.000(4) -0.009(3) 0.010(4) C21 0.058(3) 0.072(4) 0.042(3) 0.009(3) 0.001(3) 0.020(3) C22 0.084(4) 0.087(5) 0.055(4) 0.025(4) -0.014(4) 0.017(4) C23 0.083(4) 0.070(4) 0.070(4) 0.033(3) 0.000(4) 0.020(4) C24 0.059(3) 0.046(3) 0.067(4) 0.017(3) 0.015(3) 0.007(3) C25 0.072(4) 0.039(3) 0.082(4) 0.021(3) 0.014(4) 0.003(4) C26 0.067(4) 0.041(3) 0.078(4) -0.003(3) 0.015(3) -0.005(3) C27 0.057(3) 0.043(3) 0.067(4) 0.004(3) 0.003(3) -0.002(2) C28 0.045(3) 0.042(3) 0.049(3) 0.012(2) 0.009(3) 0.007(2) C29 0.036(3) 0.051(3) 0.045(3) 0.003(2) 0.004(3) 0.010(3) N1 0.046(2) 0.040(2) 0.046(2) 0.0042(19) 0.0067(18) 0.003(2) N2 0.041(2) 0.040(2) 0.053(2) 0.0033(18) 0.001(2) 0.003(2) O1 0.107(3) 0.0337(18) 0.086(3) -0.0008(19) -0.010(2) -0.006(2) O2 0.074(3) 0.0314(16) 0.077(3) 0.0144(17) -0.002(2) -0.0006(17) O3 0.079(2) 0.0265(15) 0.092(3) 0.0081(17) -0.016(3) -0.010(2) O4 0.074(2) 0.0275(16) 0.0420(18) -0.0006(14) -0.0092(17) -0.0050(16) O5 0.0446(16) 0.0346(15) 0.0459(18) -0.0074(15) -0.0071(15) -0.0022(14) O6 0.0433(19) 0.0389(16) 0.0432(18) -0.0034(13) -0.0095(18) -0.0019(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 2.254(3) . ? Cd1 O5 2.269(3) 3_556 ? Cd1 O6 2.370(3) 1_565 ? Cd1 N1 2.385(4) . ? Cd1 O5 2.406(3) 1_565 ? Cd1 N2 2.414(4) . ? Cd1 C17 2.728(5) 1_565 ? C1 O1 1.219(6) . ? C1 O2 1.267(6) . ? C1 C2 1.515(6) . ? C2 C3 1.368(7) . ? C2 C7 1.378(7) . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C5 1.373(7) . ? C4 H4 0.9300 . ? C5 C6 1.379(8) . ? C5 C8 1.506(6) . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.406(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.367(7) . ? C9 C14 1.368(7) . ? C9 O3 1.387(5) . ? C10 C11 1.375(7) . ? C10 H10 0.9300 . ? C11 C12 1.389(7) . ? C11 H11 0.9300 . ? C12 C13 1.357(6) . ? C12 O4 1.378(5) . ? C13 C14 1.398(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.435(5) . ? C15 C17 1.505(7) . ? C15 C16 1.516(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.234(6) . ? C17 O5 1.271(5) . ? C17 Cd1 2.728(5) 1_545 ? C18 N1 1.336(6) . ? C18 C19 1.387(7) . ? C18 H18 0.9300 . ? C19 C20 1.345(8) . ? C19 H19 0.9300 . ? C20 C21 1.407(8) . ? C20 H20 0.9300 . ? C21 C29 1.394(7) . ? C21 C22 1.428(8) . ? C22 C23 1.339(9) . ? C22 H22 0.9300 . ? C23 C24 1.410(8) . ? C23 H23 0.9300 . ? C24 C25 1.386(8) . ? C24 C28 1.419(7) . ? C25 C26 1.344(8) . ? C25 H25 0.9300 . ? C26 C27 1.408(7) . ? C26 H26 0.9300 . ? C27 N2 1.306(6) . ? C27 H27 0.9300 . ? C28 N2 1.351(6) . ? C28 C29 1.433(7) . ? C29 N1 1.364(6) . ? O5 Cd1 2.269(3) 3_456 ? O5 Cd1 2.406(3) 1_545 ? O6 Cd1 2.370(3) 1_545 ? 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 Cd1 O5 94.66(12) . 3_556 ? O2 Cd1 O6 130.13(12) . 1_565 ? O5 Cd1 O6 95.82(11) 3_556 1_565 ? O2 Cd1 N1 81.95(13) . . ? O5 Cd1 N1 111.11(11) 3_556 . ? O6 Cd1 N1 136.88(11) 1_565 . ? O2 Cd1 O5 100.70(12) . 1_565 ? O5 Cd1 O5 149.87(6) 3_556 1_565 ? O6 Cd1 O5 54.63(10) 1_565 1_565 ? N1 Cd1 O5 96.70(11) . 1_565 ? O2 Cd1 N2 149.11(14) . . ? O5 Cd1 N2 86.34(13) 3_556 . ? O6 Cd1 N2 80.24(11) 1_565 . ? N1 Cd1 N2 69.06(13) . . ? O5 Cd1 N2 93.27(12) 1_565 . ? O2 Cd1 C17 118.09(13) . 1_565 ? O5 Cd1 C17 122.48(12) 3_556 1_565 ? O6 Cd1 C17 26.85(12) 1_565 1_565 ? N1 Cd1 C17 118.82(14) . 1_565 ? O5 Cd1 C17 27.77(11) 1_565 1_565 ? N2 Cd1 C17 86.28(12) . 1_565 ? O1 C1 O2 123.6(4) . . ? O1 C1 C2 120.3(5) . . ? O2 C1 C2 116.1(4) . . ? C3 C2 C7 118.7(4) . . ? C3 C2 C1 120.9(4) . . ? C7 C2 C1 120.4(4) . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 118.3(4) . . ? C4 C5 C8 123.0(5) . . ? C6 C5 C8 118.7(5) . . ? C7 C6 C5 120.8(5) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 120.6(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O3 C8 C5 110.0(4) . . ? O3 C8 H8A 109.7 . . ? C5 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C5 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C14 119.6(4) . . ? C10 C9 O3 116.0(4) . . ? C14 C9 O3 124.4(5) . . ? C9 C10 C11 121.0(5) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 119.5(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 O4 125.6(4) . . ? C13 C12 C11 119.7(4) . . ? O4 C12 C11 114.7(4) . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 119.8(5) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? O4 C15 C17 113.0(4) . . ? O4 C15 C16 106.1(4) . . ? C17 C15 C16 109.0(4) . . ? O4 C15 H15 109.5 . . ? C17 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 122.1(4) . . ? O6 C17 C15 120.8(4) . . ? O5 C17 C15 117.1(4) . . ? O6 C17 Cd1 60.2(2) . 1_545 ? O5 C17 Cd1 61.9(2) . 1_545 ? C15 C17 Cd1 178.1(3) . 1_545 ? N1 C18 C19 122.9(5) . . ? N1 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C20 C19 C18 119.4(6) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.2(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C29 C21 C20 117.4(5) . . ? C29 C21 C22 119.2(6) . . ? C20 C21 C22 123.5(6) . . ? C23 C22 C21 121.2(6) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 121.6(5) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 124.5(5) . . ? C25 C24 C28 116.5(5) . . ? C23 C24 C28 119.0(6) . . ? C26 C25 C24 121.3(5) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 118.5(5) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? N2 C27 C26 122.6(5) . . ? N2 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? N2 C28 C24 122.0(5) . . ? N2 C28 C29 118.7(4) . . ? C24 C28 C29 119.2(5) . . ? N1 C29 C21 122.3(5) . . ? N1 C29 C28 117.9(4) . . ? C21 C29 C28 119.8(5) . . ? C18 N1 C29 117.8(4) . . ? C18 N1 Cd1 124.6(3) . . ? C29 N1 Cd1 117.5(3) . . ? C27 N2 C28 119.0(4) . . ? C27 N2 Cd1 124.4(3) . . ? C28 N2 Cd1 116.5(3) . . ? C1 O2 Cd1 100.9(3) . . ? C9 O3 C8 117.6(4) . . ? C12 O4 C15 116.8(3) . . ? C17 O5 Cd1 133.6(3) . 3_456 ? C17 O5 Cd1 90.3(3) . 1_545 ? Cd1 O5 Cd1 134.23(13) 3_456 1_545 ? C17 O6 Cd1 93.0(3) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 3.5(9) . . . . ? O2 C1 C2 C3 -177.5(6) . . . . ? O1 C1 C2 C7 -179.0(5) . . . . ? O2 C1 C2 C7 0.0(8) . . . . ? C7 C2 C3 C4 0.7(9) . . . . ? C1 C2 C3 C4 178.2(6) . . . . ? C2 C3 C4 C5 -0.1(11) . . . . ? C3 C4 C5 C6 0.0(10) . . . . ? C3 C4 C5 C8 -176.5(6) . . . . ? C4 C5 C6 C7 -0.4(8) . . . . ? C8 C5 C6 C7 176.2(5) . . . . ? C5 C6 C7 C2 1.0(8) . . . . ? C3 C2 C7 C6 -1.1(8) . . . . ? C1 C2 C7 C6 -178.6(5) . . . . ? C4 C5 C8 O3 -20.6(8) . . . . ? C6 C5 C8 O3 162.9(5) . . . . ? C14 C9 C10 C11 -2.9(8) . . . . ? O3 C9 C10 C11 176.8(5) . . . . ? C9 C10 C11 C12 1.6(9) . . . . ? C10 C11 C12 C13 1.2(8) . . . . ? C10 C11 C12 O4 -177.6(5) . . . . ? O4 C12 C13 C14 176.0(4) . . . . ? C11 C12 C13 C14 -2.6(8) . . . . ? C10 C9 C14 C13 1.5(8) . . . . ? O3 C9 C14 C13 -178.2(5) . . . . ? C12 C13 C14 C9 1.2(8) . . . . ? O4 C15 C17 O6 16.5(6) . . . . ? C16 C15 C17 O6 -101.3(5) . . . . ? O4 C15 C17 O5 -165.2(3) . . . . ? C16 C15 C17 O5 77.1(5) . . . . ? O4 C15 C17 Cd1 137(10) . . . 1_545 ? C16 C15 C17 Cd1 19(10) . . . 1_545 ? N1 C18 C19 C20 -0.3(9) . . . . ? C18 C19 C20 C21 -0.8(9) . . . . ? C19 C20 C21 C29 1.7(8) . . . . ? C19 C20 C21 C22 -179.3(6) . . . . ? C29 C21 C22 C23 -0.2(9) . . . . ? C20 C21 C22 C23 -179.1(6) . . . . ? C21 C22 C23 C24 1.8(11) . . . . ? C22 C23 C24 C25 178.4(6) . . . . ? C22 C23 C24 C28 -2.2(9) . . . . ? C23 C24 C25 C26 -179.0(6) . . . . ? C28 C24 C25 C26 1.6(9) . . . . ? C24 C25 C26 C27 -1.9(9) . . . . ? C25 C26 C27 N2 0.7(8) . . . . ? C25 C24 C28 N2 -0.2(8) . . . . ? C23 C24 C28 N2 -179.6(5) . . . . ? C25 C24 C28 C29 -179.6(5) . . . . ? C23 C24 C28 C29 1.0(8) . . . . ? C20 C21 C29 N1 -1.5(8) . . . . ? C22 C21 C29 N1 179.5(5) . . . . ? C20 C21 C29 C28 178.0(5) . . . . ? C22 C21 C29 C28 -1.0(8) . . . . ? N2 C28 C29 N1 0.7(7) . . . . ? C24 C28 C29 N1 -179.9(4) . . . . ? N2 C28 C29 C21 -178.9(5) . . . . ? C24 C28 C29 C21 0.6(7) . . . . ? C19 C18 N1 C29 0.5(7) . . . . ? C19 C18 N1 Cd1 177.5(4) . . . . ? C21 C29 N1 C18 0.4(7) . . . . ? C28 C29 N1 C18 -179.1(4) . . . . ? C21 C29 N1 Cd1 -176.8(4) . . . . ? C28 C29 N1 Cd1 3.7(6) . . . . ? O2 Cd1 N1 C18 9.6(4) . . . . ? O5 Cd1 N1 C18 101.5(4) 3_556 . . . ? O6 Cd1 N1 C18 -133.7(3) 1_565 . . . ? O5 Cd1 N1 C18 -90.3(4) 1_565 . . . ? N2 Cd1 N1 C18 178.7(4) . . . . ? C17 Cd1 N1 C18 -108.1(4) 1_565 . . . ? O2 Cd1 N1 C29 -173.4(3) . . . . ? O5 Cd1 N1 C29 -81.5(3) 3_556 . . . ? O6 Cd1 N1 C29 43.3(4) 1_565 . . . ? O5 Cd1 N1 C29 86.7(3) 1_565 . . . ? N2 Cd1 N1 C29 -4.3(3) . . . . ? C17 Cd1 N1 C29 68.9(4) 1_565 . . . ? C26 C27 N2 C28 0.7(8) . . . . ? C26 C27 N2 Cd1 -176.0(4) . . . . ? C24 C28 N2 C27 -0.9(7) . . . . ? C29 C28 N2 C27 178.5(5) . . . . ? C24 C28 N2 Cd1 176.0(4) . . . . ? C29 C28 N2 Cd1 -4.6(6) . . . . ? O2 Cd1 N2 C27 -157.4(4) . . . . ? O5 Cd1 N2 C27 -64.4(4) 3_556 . . . ? O6 Cd1 N2 C27 32.1(4) 1_565 . . . ? N1 Cd1 N2 C27 -178.7(4) . . . . ? O5 Cd1 N2 C27 85.4(4) 1_565 . . . ? C17 Cd1 N2 C27 58.5(4) 1_565 . . . ? O2 Cd1 N2 C28 25.9(5) . . . . ? O5 Cd1 N2 C28 118.8(3) 3_556 . . . ? O6 Cd1 N2 C28 -144.6(3) 1_565 . . . ? N1 Cd1 N2 C28 4.6(3) . . . . ? O5 Cd1 N2 C28 -91.4(3) 1_565 . . . ? C17 Cd1 N2 C28 -118.2(3) 1_565 . . . ? O1 C1 O2 Cd1 -2.6(7) . . . . ? C2 C1 O2 Cd1 178.4(4) . . . . ? O5 Cd1 O2 C1 79.5(4) 3_556 . . . ? O6 Cd1 O2 C1 -22.1(4) 1_565 . . . ? N1 Cd1 O2 C1 -169.8(4) . . . . ? O5 Cd1 O2 C1 -74.4(4) 1_565 . . . ? N2 Cd1 O2 C1 170.2(4) . . . . ? C17 Cd1 O2 C1 -51.3(4) 1_565 . . . ? C10 C9 O3 C8 -175.1(5) . . . . ? C14 C9 O3 C8 4.7(7) . . . . ? C5 C8 O3 C9 169.6(4) . . . . ? C13 C12 O4 C15 5.7(7) . . . . ? C11 C12 O4 C15 -175.7(4) . . . . ? C17 C15 O4 C12 68.9(5) . . . . ? C16 C15 O4 C12 -171.7(4) . . . . ? O6 C17 O5 Cd1 -165.4(3) . . . 3_456 ? C15 C17 O5 Cd1 16.3(5) . . . 3_456 ? Cd1 C17 O5 Cd1 -165.5(3) 1_545 . . 3_456 ? O6 C17 O5 Cd1 0.1(4) . . . 1_545 ? C15 C17 O5 Cd1 -178.2(3) . . . 1_545 ? O5 C17 O6 Cd1 -0.1(4) . . . 1_545 ? C15 C17 O6 Cd1 178.1(3) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.559 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.062 #=========================END data_Compound-5 _database_code_depnum_ccdc_archive 'CCDC 877935' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H46 Mn2 N4 O13' _chemical_formula_sum 'C58 H46 Mn2 N4 O13' _chemical_formula_weight 1116.87 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2 _symmetry_space_group_name_hall P2y loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' _cell_length_a 12.6724(6) _cell_length_b 9.9767(3) _cell_length_c 20.6665(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.217(4) _cell_angle_gamma 90.00 _cell_volume 2597.47(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9412 _exptl_absorpt_correction_T_max 0.9568 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16879 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8373 _reflns_number_gt 6175 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0367P)^2^+0.0162P] 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' _refine_ls_abs_structure_Flack -0.015(18) _refine_ls_number_reflns 8373 _refine_ls_number_parameters 712 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.006 _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 Mn1 Mn 0.35549(5) 0.01638(5) 0.95080(3) 0.0439(2) Uani 1 1 d . . . Mn2 Mn 0.64496(6) 1.29174(5) 0.55149(3) 0.0478(2) Uani 1 1 d . . . C1 C 0.5522(5) 0.1439(4) 0.9088(2) 0.0474(13) Uani 1 1 d . . . C2 C 0.6106(4) 0.2280(4) 0.8640(2) 0.0437(12) Uani 1 1 d . . . C3 C 0.5589(4) 0.2746(5) 0.8065(2) 0.0503(13) Uani 1 1 d . . . H3 H 0.4885 0.2508 0.7948 0.060 Uiso 1 1 calc R . . C4 C 0.6100(5) 0.3563(5) 0.7656(2) 0.0636(15) Uani 1 1 d . . . H4 H 0.5751 0.3845 0.7260 0.076 Uiso 1 1 calc R . . C5 C 0.7138(5) 0.3954(5) 0.7844(3) 0.0610(16) Uani 1 1 d . . . C6 C 0.7661(4) 0.3445(5) 0.8410(3) 0.0655(16) Uani 1 1 d . . . H6 H 0.8369 0.3664 0.8527 0.079 Uiso 1 1 calc R . . C7 C 0.7142(4) 0.2615(5) 0.8804(2) 0.0585(14) Uani 1 1 d . . . H7 H 0.7502 0.2280 0.9186 0.070 Uiso 1 1 calc R . . C8 C 0.7700(5) 0.4940(6) 0.7441(3) 0.0712(18) Uani 1 1 d . . . H8A H 0.8449 0.4985 0.7598 0.085 Uiso 1 1 calc R . . H8B H 0.7630 0.4667 0.6988 0.085 Uiso 1 1 calc R . . C9 C 0.7724(5) 0.7350(6) 0.7330(3) 0.0759(18) Uani 1 1 d . . . C10 C 0.7233(5) 0.8542(6) 0.7481(3) 0.098(2) Uani 1 1 d . . . H10 H 0.6597 0.8519 0.7667 0.118 Uiso 1 1 calc R . . C11 C 0.7682(5) 0.9740(6) 0.7356(3) 0.0920(17) Uani 1 1 d . . . H11 H 0.7350 1.0536 0.7452 0.110 Uiso 1 1 calc R . . C12 C 0.8618(4) 0.9769(5) 0.7090(3) 0.0694(15) Uani 1 1 d . . . C13 C 0.9090(4) 0.8603(7) 0.6912(3) 0.103(2) Uani 1 1 d . . . H13 H 0.9718 0.8633 0.6718 0.124 Uiso 1 1 calc R . . C14 C 0.8607(5) 0.7350(6) 0.7027(3) 0.092(2) Uani 1 1 d . . . H14 H 0.8897 0.6552 0.6896 0.110 Uiso 1 1 calc R . . C15 C 0.9374(4) 1.1403(6) 0.6430(3) 0.0630(16) Uani 1 1 d . . . H15 H 0.9712 1.0649 0.6229 0.076 Uiso 1 1 calc R . . C16 C 1.0123(4) 1.2576(7) 0.6493(3) 0.101(2) Uani 1 1 d . . . H16A H 1.0757 1.2331 0.6764 0.152 Uiso 1 1 calc R . . H16B H 0.9789 1.3318 0.6686 0.152 Uiso 1 1 calc R . . H16C H 1.0302 1.2829 0.6070 0.152 Uiso 1 1 calc R . . C17 C 0.8372(5) 1.1820(6) 0.5995(4) 0.0694(17) Uani 1 1 d . . . C18 C 0.4417(4) 1.1627(4) 0.5871(3) 0.0518(14) Uani 1 1 d . . . C19 C 0.3852(4) 1.0808(4) 0.6326(2) 0.0451(12) Uani 1 1 d . . . C20 C 0.4352(4) 1.0371(5) 0.6916(2) 0.0580(14) Uani 1 1 d . . . H20 H 0.5046 1.0631 0.7050 0.070 Uiso 1 1 calc R . . C21 C 0.3815(5) 0.9545(6) 0.7304(3) 0.0656(16) Uani 1 1 d . . . H21 H 0.4161 0.9259 0.7699 0.079 Uiso 1 1 calc R . . C22 C 0.2802(5) 0.9132(5) 0.7133(3) 0.0578(16) Uani 1 1 d . . . C23 C 0.2295(5) 0.9576(6) 0.6547(3) 0.0720(17) Uani 1 1 d . . . H23 H 0.1602 0.9304 0.6418 0.086 Uiso 1 1 calc R . . C24 C 0.2802(4) 1.0420(5) 0.6150(3) 0.0611(14) Uani 1 1 d . . . H24 H 0.2442 1.0731 0.5763 0.073 Uiso 1 1 calc R . . C25 C 0.2241(6) 0.8216(6) 0.7561(3) 0.089(2) Uani 1 1 d . . . H25A H 0.2466 0.8408 0.8015 0.106 Uiso 1 1 calc R . . H25B H 0.1480 0.8353 0.7484 0.106 Uiso 1 1 calc R . . C26 C 0.1992(5) 0.5912(5) 0.7754(3) 0.0653(15) Uani 1 1 d . . . C27 C 0.2333(4) 0.4620(5) 0.7687(3) 0.0679(14) Uani 1 1 d . . . H27 H 0.2899 0.4459 0.7446 0.081 Uiso 1 1 calc R . . C28 C 0.1862(4) 0.3555(5) 0.7968(2) 0.0622(14) Uani 1 1 d . . . H28 H 0.2100 0.2685 0.7912 0.075 Uiso 1 1 calc R . . C29 C 0.1031(3) 0.3797(4) 0.8334(2) 0.0527(11) Uani 1 1 d . . . C30 C 0.0694(3) 0.5093(4) 0.8424(2) 0.0658(12) Uani 1 1 d . . . H30 H 0.0143 0.5255 0.8677 0.079 Uiso 1 1 calc R . . C31 C 0.1182(4) 0.6164(5) 0.8136(3) 0.0738(16) Uani 1 1 d . . . H31 H 0.0964 0.7039 0.8201 0.089 Uiso 1 1 calc R . . C32 C 0.0730(4) 0.1460(4) 0.8523(3) 0.0520(13) Uani 1 1 d . . . H32 H 0.0787 0.1306 0.8060 0.062 Uiso 1 1 calc R . . C33 C -0.0186(4) 0.0629(5) 0.8739(3) 0.0807(17) Uani 1 1 d . . . H33A H -0.0836 0.0876 0.8484 0.121 Uiso 1 1 calc R . . H33B H -0.0248 0.0795 0.9190 0.121 Uiso 1 1 calc R . . H33C H -0.0049 -0.0306 0.8676 0.121 Uiso 1 1 calc R . . C34 C 0.1754(4) 0.1065(5) 0.8919(3) 0.0548(13) Uani 1 1 d . . . C35 C 0.5147(4) -0.1988(6) 0.8907(2) 0.0584(14) Uani 1 1 d . . . H35 H 0.5505 -0.1227 0.8790 0.070 Uiso 1 1 calc R . . C36 C 0.5518(5) -0.3205(6) 0.8724(3) 0.0686(17) Uani 1 1 d . . . H36 H 0.6094 -0.3262 0.8482 0.082 Uiso 1 1 calc R . . C37 C 0.5018(5) -0.4329(5) 0.8906(3) 0.076(2) Uani 1 1 d . . . H37 H 0.5266 -0.5169 0.8799 0.091 Uiso 1 1 calc R . . C38 C 0.4135(5) -0.4229(5) 0.9251(3) 0.0551(16) Uani 1 1 d . . . C39 C 0.3532(5) -0.5360(6) 0.9436(3) 0.076(2) Uani 1 1 d . . . H39 H 0.3728 -0.6217 0.9318 0.091 Uiso 1 1 calc R . . C40 C 0.2702(5) -0.5216(5) 0.9772(3) 0.0730(18) Uani 1 1 d . . . H40 H 0.2334 -0.5973 0.9885 0.088 Uiso 1 1 calc R . . C41 C 0.2364(5) -0.3928(5) 0.9963(3) 0.0651(17) Uani 1 1 d . . . C42 C 0.1540(6) -0.3721(7) 1.0332(4) 0.100(2) Uani 1 1 d . . . H42 H 0.1144 -0.4443 1.0456 0.120 Uiso 1 1 calc R . . C43 C 0.1311(5) -0.2470(7) 1.0513(4) 0.107(3) Uani 1 1 d . . . H43 H 0.0762 -0.2326 1.0769 0.128 Uiso 1 1 calc R . . C44 C 0.1895(5) -0.1385(7) 1.0316(3) 0.088(2) Uani 1 1 d . . . H44 H 0.1725 -0.0528 1.0448 0.105 Uiso 1 1 calc R . . C45 C 0.2933(4) -0.2784(5) 0.9790(3) 0.0461(13) Uani 1 1 d . . . C46 C 0.3822(5) -0.2935(5) 0.9417(3) 0.0507(15) Uani 1 1 d . . . C47 C 0.4811(4) 1.4974(6) 0.6109(3) 0.0584(15) Uani 1 1 d . . . H47 H 0.4484 1.4191 0.6229 0.070 Uiso 1 1 calc R . . C48 C 0.4392(6) 1.6204(8) 0.6279(3) 0.086(2) Uani 1 1 d . . . H48 H 0.3778 1.6248 0.6486 0.103 Uiso 1 1 calc R . . C49 C 0.4909(6) 1.7323(8) 0.6131(3) 0.088(2) Uani 1 1 d . . . H49 H 0.4655 1.8151 0.6252 0.105 Uiso 1 1 calc R . . C50 C 0.5805(6) 1.7280(6) 0.5804(3) 0.0695(18) Uani 1 1 d . . . C51 C 0.6377(7) 1.8437(7) 0.5638(4) 0.094(2) Uani 1 1 d . . . H51 H 0.6150 1.9280 0.5756 0.113 Uiso 1 1 calc R . . C52 C 0.7224(7) 1.8337(6) 0.5318(4) 0.092(2) Uani 1 1 d . . . H52 H 0.7593 1.9104 0.5222 0.110 Uiso 1 1 calc R . . C53 C 0.7579(5) 1.7032(6) 0.5117(3) 0.0721(18) Uani 1 1 d . . . C54 C 0.8437(6) 1.6860(8) 0.4746(4) 0.101(2) Uani 1 1 d . . . H54 H 0.8817 1.7604 0.4629 0.121 Uiso 1 1 calc R . . C55 C 0.8719(6) 1.5602(9) 0.4554(4) 0.120(3) Uani 1 1 d . . . H55 H 0.9276 1.5483 0.4302 0.144 Uiso 1 1 calc R . . C56 C 0.8148(5) 1.4515(7) 0.4747(3) 0.083(2) Uani 1 1 d . . . H56 H 0.8344 1.3663 0.4622 0.100 Uiso 1 1 calc R . . C57 C 0.7054(5) 1.5883(5) 0.5286(3) 0.0574(16) Uani 1 1 d . . . C58 C 0.6162(4) 1.6002(5) 0.5634(3) 0.0490(14) Uani 1 1 d . . . N1 N 0.4313(3) -0.1807(4) 0.92414(19) 0.0468(11) Uani 1 1 d . . . N2 N 0.2669(4) -0.1529(4) 0.9954(2) 0.0575(13) Uani 1 1 d . . . N3 N 0.5645(4) 1.4878(4) 0.5789(2) 0.0507(12) Uani 1 1 d . . . N4 N 0.7337(4) 1.4622(4) 0.5101(2) 0.0580(13) Uani 1 1 d . . . O1 O 0.4530(3) 0.1330(4) 0.8969(2) 0.0650(11) Uani 1 1 d . . . O2 O 0.6057(3) 0.0899(3) 0.95591(17) 0.0670(10) Uani 1 1 d . . . O3 O 0.7217(4) 0.6195(4) 0.7507(2) 0.0903(14) Uani 1 1 d . . . O4 O 0.9129(3) 1.1026(3) 0.70534(16) 0.0851(10) Uani 1 1 d . . . O5 O 0.8086(9) 1.1552(12) 0.5468(9) 0.077(4) Uani 0.50 1 d P . . O5' O 0.8557(8) 1.1482(14) 0.5371(8) 0.071(3) Uani 0.50 1 d P . . O6 O 0.7683(3) 1.2473(4) 0.6240(2) 0.0982(15) Uani 1 1 d . . . O7 O 0.5400(3) 1.1772(4) 0.6013(2) 0.0676(11) Uani 1 1 d . . . O8 O 0.3894(3) 1.2158(4) 0.54029(18) 0.0758(12) Uani 1 1 d . . . O9 O 0.2490(4) 0.6886(4) 0.7419(2) 0.0906(15) Uani 1 1 d . . . O10 O 0.04583(19) 0.2836(2) 0.86253(14) 0.0631(8) Uani 1 1 d . . . O11 O 0.2284(3) 0.0168(4) 0.86937(17) 0.0766(10) Uani 1 1 d . . . O12 O 0.2023(3) 0.1589(4) 0.9454(2) 0.0759(11) Uani 1 1 d . . . O1W O 0.0000 -0.6461(7) 1.0000 0.125(3) Uani 1 2 d SD . . H1A H 0.038(6) -0.696(6) 0.975(3) 0.188 Uiso 1 1 d D . . O2W O 0.9780(15) 1.9833(7) 0.4906(11) 0.093(4) Uani 0.50 1 d PD . . H2A H 1.0000 2.0667(14) 0.5000 0.140 Uiso 1 2 d SD . . 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 Mn1 0.0474(5) 0.0323(4) 0.0525(5) -0.0039(4) 0.0082(4) 0.0001(3) Mn2 0.0548(5) 0.0358(4) 0.0537(5) -0.0030(4) 0.0106(4) -0.0049(3) C1 0.064(4) 0.039(3) 0.041(3) -0.002(2) 0.012(3) 0.011(2) C2 0.049(3) 0.032(3) 0.053(3) -0.002(2) 0.015(3) -0.001(2) C3 0.057(3) 0.043(3) 0.049(3) -0.001(3) -0.002(3) -0.009(2) C4 0.091(4) 0.063(3) 0.038(3) 0.006(3) 0.009(3) -0.012(3) C5 0.075(4) 0.049(3) 0.064(4) -0.002(3) 0.031(3) 0.002(3) C6 0.046(3) 0.058(4) 0.093(5) 0.017(3) 0.013(3) -0.001(2) C7 0.053(3) 0.055(3) 0.067(4) 0.016(3) 0.005(3) 0.006(3) C8 0.082(4) 0.058(4) 0.078(4) 0.008(3) 0.031(3) -0.006(3) C9 0.077(4) 0.067(4) 0.087(4) 0.024(3) 0.026(3) -0.003(3) C10 0.104(5) 0.060(4) 0.139(6) 0.030(3) 0.054(4) 0.003(3) C11 0.090(4) 0.075(4) 0.115(5) 0.021(3) 0.031(4) 0.003(3) C12 0.069(3) 0.065(3) 0.074(4) 0.026(2) 0.007(3) -0.006(3) C13 0.056(3) 0.101(5) 0.157(6) 0.027(4) 0.033(4) -0.001(3) C14 0.086(4) 0.068(4) 0.128(6) 0.028(3) 0.038(4) -0.005(3) C15 0.044(3) 0.080(4) 0.067(4) 0.018(3) 0.015(3) -0.002(3) C16 0.067(4) 0.114(5) 0.120(5) 0.035(4) -0.004(3) -0.030(3) C17 0.062(4) 0.048(3) 0.096(5) 0.018(3) -0.005(4) -0.008(3) C18 0.055(4) 0.030(3) 0.073(4) 0.004(2) 0.018(3) -0.003(2) C19 0.056(3) 0.034(3) 0.045(3) 0.003(2) 0.008(3) 0.006(2) C20 0.063(3) 0.053(3) 0.058(4) 0.002(3) 0.006(3) -0.009(3) C21 0.081(4) 0.065(4) 0.050(3) 0.014(3) 0.002(3) 0.000(3) C22 0.080(4) 0.035(3) 0.062(4) 0.004(2) 0.025(3) -0.007(3) C23 0.068(4) 0.071(4) 0.079(4) 0.001(3) 0.020(3) -0.022(3) C24 0.055(3) 0.067(4) 0.060(3) 0.014(3) 0.003(3) 0.000(3) C25 0.130(6) 0.052(4) 0.094(5) 0.006(3) 0.060(5) -0.009(4) C26 0.085(4) 0.050(3) 0.065(3) 0.008(2) 0.027(3) -0.010(3) C27 0.083(4) 0.048(3) 0.079(4) 0.003(2) 0.037(3) -0.002(2) C28 0.061(3) 0.048(3) 0.082(4) 0.006(2) 0.030(3) 0.001(2) C29 0.049(3) 0.043(2) 0.068(3) 0.008(2) 0.013(2) 0.004(2) C30 0.069(3) 0.054(3) 0.081(3) 0.018(2) 0.039(2) 0.006(2) C31 0.087(4) 0.051(3) 0.090(4) 0.012(3) 0.039(3) 0.006(3) C32 0.054(3) 0.040(2) 0.062(3) 0.012(2) 0.007(3) -0.004(2) C33 0.057(3) 0.063(3) 0.122(5) 0.010(3) 0.010(3) -0.020(2) C34 0.070(4) 0.041(3) 0.053(3) 0.009(2) 0.002(3) -0.024(3) C35 0.064(4) 0.059(3) 0.055(3) 0.002(3) 0.019(3) 0.011(3) C36 0.080(4) 0.062(4) 0.068(4) -0.005(3) 0.025(3) 0.025(3) C37 0.108(6) 0.034(3) 0.085(5) -0.013(3) 0.010(4) 0.025(3) C38 0.079(4) 0.032(3) 0.053(3) -0.011(2) 0.001(3) 0.016(3) C39 0.104(6) 0.031(4) 0.091(5) -0.015(3) -0.001(4) 0.007(3) C40 0.085(4) 0.041(3) 0.094(5) -0.002(3) 0.014(4) -0.011(3) C41 0.082(4) 0.034(3) 0.080(4) 0.002(3) 0.013(3) -0.008(3) C42 0.099(5) 0.068(5) 0.143(7) 0.003(4) 0.060(5) -0.018(4) C43 0.115(6) 0.064(5) 0.160(7) -0.004(4) 0.098(5) -0.001(4) C44 0.084(5) 0.056(4) 0.132(6) -0.015(4) 0.053(5) -0.001(3) C45 0.049(3) 0.041(3) 0.049(3) -0.003(2) 0.010(2) 0.002(2) C46 0.066(4) 0.036(3) 0.046(3) -0.004(2) -0.012(3) 0.002(3) C47 0.069(4) 0.047(3) 0.060(4) -0.009(3) 0.009(3) 0.009(3) C48 0.095(5) 0.082(5) 0.083(5) -0.012(4) 0.020(4) 0.019(4) C49 0.110(6) 0.074(5) 0.080(5) -0.018(4) 0.017(4) 0.032(4) C50 0.098(5) 0.044(4) 0.065(4) -0.007(3) 0.002(4) 0.004(3) C51 0.142(7) 0.050(5) 0.089(5) -0.005(3) 0.006(5) 0.006(4) C52 0.144(7) 0.033(4) 0.094(5) 0.009(3) -0.006(5) -0.022(4) C53 0.080(5) 0.064(4) 0.073(4) 0.005(3) 0.012(4) -0.014(3) C54 0.117(6) 0.062(5) 0.125(6) 0.023(4) 0.016(5) -0.039(4) C55 0.108(6) 0.096(7) 0.163(8) 0.021(5) 0.049(5) -0.025(5) C56 0.100(5) 0.056(4) 0.100(5) 0.008(3) 0.043(4) -0.005(4) C57 0.078(4) 0.032(3) 0.060(4) 0.001(2) -0.005(3) -0.015(3) C58 0.065(4) 0.035(3) 0.046(3) -0.003(2) 0.002(3) 0.006(3) N1 0.056(3) 0.042(3) 0.042(3) 0.000(2) 0.004(2) 0.001(2) N2 0.063(3) 0.040(3) 0.071(3) -0.005(2) 0.018(3) -0.001(2) N3 0.058(3) 0.041(3) 0.053(3) -0.007(2) 0.007(2) 0.008(2) N4 0.063(3) 0.046(3) 0.068(3) -0.003(2) 0.022(3) -0.005(2) O1 0.063(3) 0.056(2) 0.078(3) 0.016(2) 0.014(2) -0.0065(19) O2 0.077(2) 0.064(2) 0.060(2) 0.0213(19) 0.009(2) 0.0036(19) O3 0.093(3) 0.055(2) 0.133(4) 0.037(2) 0.057(2) 0.0066(19) O4 0.092(2) 0.086(2) 0.076(2) 0.0123(17) 0.0063(19) -0.0238(19) O5 0.083(10) 0.042(5) 0.100(10) -0.018(5) -0.026(9) 0.009(6) O5' 0.062(7) 0.084(6) 0.064(6) 0.005(4) -0.003(6) 0.013(5) O6 0.057(2) 0.121(4) 0.117(3) 0.046(3) 0.013(2) 0.010(2) O7 0.053(2) 0.065(3) 0.087(3) 0.024(2) 0.014(2) -0.0101(19) O8 0.074(3) 0.080(3) 0.074(3) 0.042(2) 0.014(2) 0.014(2) O9 0.131(4) 0.046(2) 0.108(3) 0.003(2) 0.072(3) -0.013(2) O10 0.0519(16) 0.0405(15) 0.102(2) 0.0182(14) 0.0317(15) 0.0029(12) O11 0.068(2) 0.082(2) 0.079(2) -0.0138(19) 0.0014(18) 0.0182(19) O12 0.098(3) 0.057(2) 0.070(3) -0.003(2) -0.002(2) -0.004(2) O1W 0.165(7) 0.083(4) 0.142(7) 0.000 0.090(5) 0.000 O2W 0.120(15) 0.077(4) 0.083(12) 0.001(5) 0.008(9) -0.028(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mn1 O2 2.071(3) 2_657 ? Mn1 O1 2.103(4) . ? Mn1 O11 2.200(3) . ? Mn1 N2 2.278(4) . ? Mn1 N1 2.282(4) . ? Mn1 O12 2.399(4) . ? Mn1 C34 2.626(5) . ? Mn2 O8 2.045(4) 2_656 ? Mn2 O6 2.093(4) . ? Mn2 O7 2.105(4) . ? Mn2 N4 2.258(5) . ? Mn2 N3 2.305(4) . ? Mn2 O5 2.492(11) . ? C1 O2 1.248(5) . ? C1 O1 1.259(6) . ? C1 C2 1.503(7) . ? C2 C7 1.361(6) . ? C2 C3 1.375(6) . ? C3 C4 1.384(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 C6 1.378(7) . ? C5 C8 1.516(7) . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.407(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.339(7) . ? C9 O3 1.388(7) . ? C9 C10 1.394(8) . ? C10 C11 1.359(7) . ? C10 H10 0.9300 . ? C11 C12 1.361(7) . ? C11 H11 0.9300 . ? C12 C13 1.377(8) . ? C12 O4 1.418(6) . ? C13 C14 1.423(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.409(6) . ? C15 C16 1.504(8) . ? C15 C17 1.531(8) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.142(17) . ? C17 O6 1.240(7) . ? C17 O5' 1.377(18) . ? C18 O8 1.231(6) . ? C18 O7 1.257(6) . ? C18 C19 1.488(7) . ? C19 C20 1.382(6) . ? C19 C24 1.395(7) . ? C20 C21 1.380(7) . ? C20 H20 0.9300 . ? C21 C22 1.358(7) . ? C21 H21 0.9300 . ? C22 C23 1.381(7) . ? C22 C25 1.503(7) . ? C23 C24 1.382(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.403(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.372(7) . ? C26 C31 1.384(7) . ? C26 O9 1.384(6) . ? C27 C28 1.377(7) . ? C27 H27 0.9300 . ? C28 C29 1.384(6) . ? C28 H28 0.9300 . ? C29 O10 1.380(5) . ? C29 C30 1.381(6) . ? C30 C31 1.399(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O10 1.436(5) . ? C32 C34 1.510(7) . ? C32 C33 1.531(6) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O12 1.237(5) . ? C34 O11 1.239(6) . ? C35 N1 1.337(6) . ? C35 C36 1.370(8) . ? C35 H35 0.9300 . ? C36 C37 1.361(8) . ? C36 H36 0.9300 . ? C37 C38 1.394(8) . ? C37 H37 0.9300 . ? C38 C46 1.403(7) . ? C38 C39 1.439(8) . ? C39 C40 1.329(8) . ? C39 H39 0.9300 . ? C40 C41 1.424(8) . ? C40 H40 0.9300 . ? C41 C42 1.372(8) . ? C41 C45 1.417(8) . ? C42 C43 1.344(10) . ? C42 H42 0.9300 . ? C43 C44 1.396(9) . ? C43 H43 0.9300 . ? C44 N2 1.305(7) . ? C44 H44 0.9300 . ? C45 N2 1.348(6) . ? C45 C46 1.440(7) . ? C46 N1 1.354(7) . ? C47 N3 1.310(6) . ? C47 C48 1.397(8) . ? C47 H47 0.9300 . ? C48 C49 1.346(10) . ? C48 H48 0.9300 . ? C49 C50 1.384(8) . ? C49 H49 0.9300 . ? C50 C58 1.411(8) . ? C50 C51 1.424(10) . ? C51 C52 1.324(10) . ? C51 H51 0.9300 . ? C52 C53 1.452(10) . ? C52 H52 0.9300 . ? C53 C57 1.389(8) . ? C53 C54 1.408(9) . ? C54 C55 1.376(11) . ? C54 H54 0.9300 . ? C55 C56 1.386(9) . ? C55 H55 0.9300 . ? C56 N4 1.329(7) . ? C56 H56 0.9300 . ? C57 N4 1.374(7) . ? C57 C58 1.409(8) . ? C58 N3 1.354(7) . ? O2 Mn1 2.071(3) 2_657 ? O5 O5' 0.654(17) . ? O8 Mn2 2.045(4) 2_656 ? O1W H1A 0.898(10) . ? O2W O2W 0.65(3) 2_756 ? O2W H2A 0.893(10) . ? 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 Mn1 O1 101.75(15) 2_657 . ? O2 Mn1 O11 142.34(14) 2_657 . ? O1 Mn1 O11 90.99(15) . . ? O2 Mn1 N2 87.90(16) 2_657 . ? O1 Mn1 N2 165.61(16) . . ? O11 Mn1 N2 87.64(16) . . ? O2 Mn1 N1 117.78(14) 2_657 . ? O1 Mn1 N1 93.55(16) . . ? O11 Mn1 N1 96.28(14) . . ? N2 Mn1 N1 72.38(16) . . ? O2 Mn1 O12 86.71(14) 2_657 . ? O1 Mn1 O12 99.59(15) . . ? O11 Mn1 O12 56.06(13) . . ? N2 Mn1 O12 91.52(15) . . ? N1 Mn1 O12 149.22(15) . . ? O2 Mn1 C34 114.64(16) 2_657 . ? O1 Mn1 C34 95.51(15) . . ? O11 Mn1 C34 28.02(14) . . ? N2 Mn1 C34 90.00(16) . . ? N1 Mn1 C34 123.40(16) . . ? O12 Mn1 C34 28.04(13) . . ? O8 Mn2 O6 130.80(17) 2_656 . ? O8 Mn2 O7 99.80(16) 2_656 . ? O6 Mn2 O7 89.86(15) . . ? O8 Mn2 N4 89.58(17) 2_656 . ? O6 Mn2 N4 93.82(16) . . ? O7 Mn2 N4 163.98(17) . . ? O8 Mn2 N3 119.12(16) 2_656 . ? O6 Mn2 N3 108.66(17) . . ? O7 Mn2 N3 91.18(17) . . ? N4 Mn2 N3 72.87(17) . . ? O8 Mn2 O5 81.7(4) 2_656 . ? O6 Mn2 O5 49.6(4) . . ? O7 Mn2 O5 107.2(4) . . ? N4 Mn2 O5 86.9(4) . . ? N3 Mn2 O5 150.0(3) . . ? O2 C1 O1 124.2(5) . . ? O2 C1 C2 117.3(5) . . ? O1 C1 C2 118.4(5) . . ? C7 C2 C3 119.3(5) . . ? C7 C2 C1 120.6(5) . . ? C3 C2 C1 120.0(5) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 119.3(5) . . ? C6 C5 C8 119.6(6) . . ? C4 C5 C8 121.1(6) . . ? C5 C6 C7 120.5(5) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.6(5) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? O3 C8 C5 106.8(4) . . ? O3 C8 H8A 110.4 . . ? C5 C8 H8A 110.4 . . ? O3 C8 H8B 110.4 . . ? C5 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C14 C9 O3 123.9(6) . . ? C14 C9 C10 121.3(6) . . ? O3 C9 C10 114.7(5) . . ? C11 C10 C9 120.1(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 120.8(5) . . ? C11 C12 O4 117.7(5) . . ? C13 C12 O4 121.3(5) . . ? C12 C13 C14 119.4(5) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C9 C14 C13 118.3(6) . . ? C9 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? O4 C15 C16 109.1(5) . . ? O4 C15 C17 111.0(4) . . ? C16 C15 C17 108.4(5) . . ? O4 C15 H15 109.4 . . ? C16 C15 H15 109.4 . . ? C17 C15 H15 109.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 110.4(9) . . ? O5 C17 O5' 28.2(8) . . ? O6 C17 O5' 135.2(8) . . ? O5 C17 C15 130.8(9) . . ? O6 C17 C15 118.6(6) . . ? O5' C17 C15 105.5(7) . . ? O8 C18 O7 124.7(5) . . ? O8 C18 C19 118.6(5) . . ? O7 C18 C19 116.6(5) . . ? C20 C19 C24 118.4(5) . . ? C20 C19 C18 121.7(5) . . ? C24 C19 C18 119.9(4) . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 122.9(5) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C21 C22 C23 117.9(5) . . ? C21 C22 C25 121.7(6) . . ? C23 C22 C25 120.4(6) . . ? C22 C23 C24 120.9(5) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 120.4(5) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? O9 C25 C22 108.7(5) . . ? O9 C25 H25A 110.0 . . ? C22 C25 H25A 110.0 . . ? O9 C25 H25B 110.0 . . ? C22 C25 H25B 110.0 . . ? H25A C25 H25B 108.3 . . ? C27 C26 C31 119.3(5) . . ? C27 C26 O9 116.3(5) . . ? C31 C26 O9 124.4(5) . . ? C26 C27 C28 121.8(5) . . ? C26 C27 H27 119.1 . . ? C28 C27 H27 119.1 . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? O10 C29 C30 114.0(4) . . ? O10 C29 C28 125.8(4) . . ? C30 C29 C28 120.2(4) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C26 C31 C30 119.6(5) . . ? C26 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? O10 C32 C34 112.0(4) . . ? O10 C32 C33 105.9(4) . . ? C34 C32 C33 109.6(4) . . ? O10 C32 H32 109.8 . . ? C34 C32 H32 109.8 . . ? C33 C32 H32 109.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O12 C34 O11 122.2(5) . . ? O12 C34 C32 120.8(5) . . ? O11 C34 C32 117.0(5) . . ? O12 C34 Mn1 65.7(3) . . ? O11 C34 Mn1 56.5(3) . . ? C32 C34 Mn1 173.5(4) . . ? N1 C35 C36 125.2(6) . . ? N1 C35 H35 117.4 . . ? C36 C35 H35 117.4 . . ? C37 C36 C35 118.1(5) . . ? C37 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C36 C37 C38 120.4(5) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C46 117.1(5) . . ? C37 C38 C39 124.0(5) . . ? C46 C38 C39 118.9(5) . . ? C40 C39 C38 121.8(5) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C39 C40 C41 121.4(5) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C45 117.3(6) . . ? C42 C41 C40 124.0(6) . . ? C45 C41 C40 118.7(6) . . ? C43 C42 C41 119.6(6) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.1(6) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? N2 C44 C43 122.5(6) . . ? N2 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? N2 C45 C41 122.5(5) . . ? N2 C45 C46 117.5(5) . . ? C41 C45 C46 120.0(5) . . ? N1 C46 C38 123.2(5) . . ? N1 C46 C45 117.7(5) . . ? C38 C46 C45 119.1(5) . . ? N3 C47 C48 122.7(6) . . ? N3 C47 H47 118.6 . . ? C48 C47 H47 118.6 . . ? C49 C48 C47 117.7(6) . . ? C49 C48 H48 121.2 . . ? C47 C48 H48 121.2 . . ? C48 C49 C50 122.0(6) . . ? C48 C49 H49 119.0 . . ? C50 C49 H49 119.0 . . ? C49 C50 C58 116.9(6) . . ? C49 C50 C51 124.0(7) . . ? C58 C50 C51 119.2(6) . . ? C52 C51 C50 121.4(6) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C53 120.2(6) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C57 C53 C54 117.1(6) . . ? C57 C53 C52 119.7(6) . . ? C54 C53 C52 123.1(7) . . ? C55 C54 C53 120.5(6) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 118.1(7) . . ? C54 C55 H55 120.9 . . ? C56 C55 H55 120.9 . . ? N4 C56 C55 123.7(7) . . ? N4 C56 H56 118.2 . . ? C55 C56 H56 118.2 . . ? N4 C57 C53 122.6(6) . . ? N4 C57 C58 117.9(5) . . ? C53 C57 C58 119.5(5) . . ? N3 C58 C57 119.1(4) . . ? N3 C58 C50 120.9(5) . . ? C57 C58 C50 120.0(5) . . ? C35 N1 C46 116.0(5) . . ? C35 N1 Mn1 128.2(4) . . ? C46 N1 Mn1 115.7(3) . . ? C44 N2 C45 118.0(5) . . ? C44 N2 Mn1 125.8(4) . . ? C45 N2 Mn1 116.1(4) . . ? C47 N3 C58 119.8(5) . . ? C47 N3 Mn2 126.1(4) . . ? C58 N3 Mn2 114.0(3) . . ? C56 N4 C57 117.9(5) . . ? C56 N4 Mn2 126.5(4) . . ? C57 N4 Mn2 115.4(4) . . ? C1 O1 Mn1 125.2(3) . . ? C1 O2 Mn1 159.0(4) . 2_657 ? C9 O3 C8 119.6(4) . . ? C15 O4 C12 115.6(4) . . ? O5' O5 C17 96(3) . . ? O5' O5 Mn2 150(3) . . ? C17 O5 Mn2 90.8(8) . . ? O5 O5' C17 56(3) . . ? C17 O6 Mn2 108.8(4) . . ? C18 O7 Mn2 127.7(4) . . ? C18 O8 Mn2 158.5(4) . 2_656 ? C26 O9 C25 115.7(4) . . ? C29 O10 C32 117.0(3) . . ? C34 O11 Mn1 95.5(3) . . ? C34 O12 Mn1 86.2(3) . . ? O2W O2W H2A 68.8(9) 2_756 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -10.6(6) . . . . ? O1 C1 C2 C7 168.9(5) . . . . ? O2 C1 C2 C3 170.9(4) . . . . ? O1 C1 C2 C3 -9.6(6) . . . . ? C7 C2 C3 C4 -0.9(7) . . . . ? C1 C2 C3 C4 177.6(4) . . . . ? C2 C3 C4 C5 -2.4(7) . . . . ? C3 C4 C5 C6 4.6(8) . . . . ? C3 C4 C5 C8 -174.8(5) . . . . ? C4 C5 C6 C7 -3.5(8) . . . . ? C8 C5 C6 C7 175.8(5) . . . . ? C3 C2 C7 C6 2.0(7) . . . . ? C1 C2 C7 C6 -176.5(4) . . . . ? C5 C6 C7 C2 0.2(7) . . . . ? C6 C5 C8 O3 -109.5(6) . . . . ? C4 C5 C8 O3 69.9(7) . . . . ? C14 C9 C10 C11 -4.0(11) . . . . ? O3 C9 C10 C11 177.2(6) . . . . ? C9 C10 C11 C12 -0.7(10) . . . . ? C10 C11 C12 C13 3.6(9) . . . . ? C10 C11 C12 O4 -171.4(5) . . . . ? C11 C12 C13 C14 -2.0(10) . . . . ? O4 C12 C13 C14 172.8(6) . . . . ? O3 C9 C14 C13 -175.8(6) . . . . ? C10 C9 C14 C13 5.5(11) . . . . ? C12 C13 C14 C9 -2.5(10) . . . . ? O4 C15 C17 O5 -134.8(12) . . . . ? C16 C15 C17 O5 105.4(13) . . . . ? O4 C15 C17 O6 38.8(7) . . . . ? C16 C15 C17 O6 -81.0(6) . . . . ? O4 C15 C17 O5' -149.1(7) . . . . ? C16 C15 C17 O5' 91.1(8) . . . . ? O8 C18 C19 C20 -169.0(5) . . . . ? O7 C18 C19 C20 7.9(7) . . . . ? O8 C18 C19 C24 13.5(7) . . . . ? O7 C18 C19 C24 -169.6(5) . . . . ? C24 C19 C20 C21 1.5(7) . . . . ? C18 C19 C20 C21 -176.0(4) . . . . ? C19 C20 C21 C22 0.0(8) . . . . ? C20 C21 C22 C23 -0.6(8) . . . . ? C20 C21 C22 C25 179.1(5) . . . . ? C21 C22 C23 C24 -0.3(8) . . . . ? C25 C22 C23 C24 179.9(5) . . . . ? C22 C23 C24 C19 1.9(8) . . . . ? C20 C19 C24 C23 -2.5(8) . . . . ? C18 C19 C24 C23 175.1(5) . . . . ? C21 C22 C25 O9 -86.2(7) . . . . ? C23 C22 C25 O9 93.6(7) . . . . ? C31 C26 C27 C28 2.8(9) . . . . ? O9 C26 C27 C28 -176.4(5) . . . . ? C26 C27 C28 C29 -0.8(8) . . . . ? C27 C28 C29 O10 177.7(4) . . . . ? C27 C28 C29 C30 -1.1(7) . . . . ? O10 C29 C30 C31 -177.8(4) . . . . ? C28 C29 C30 C31 1.1(7) . . . . ? C27 C26 C31 C30 -2.8(9) . . . . ? O9 C26 C31 C30 176.4(5) . . . . ? C29 C30 C31 C26 0.9(8) . . . . ? O10 C32 C34 O12 31.4(6) . . . . ? C33 C32 C34 O12 -85.8(6) . . . . ? O10 C32 C34 O11 -151.1(4) . . . . ? C33 C32 C34 O11 91.7(6) . . . . ? O10 C32 C34 Mn1 -156(3) . . . . ? C33 C32 C34 Mn1 87(3) . . . . ? O2 Mn1 C34 O12 5.6(3) 2_657 . . . ? O1 Mn1 C34 O12 -100.1(3) . . . . ? O11 Mn1 C34 O12 178.2(5) . . . . ? N2 Mn1 C34 O12 93.2(3) . . . . ? N1 Mn1 C34 O12 162.0(3) . . . . ? O2 Mn1 C34 O11 -172.7(3) 2_657 . . . ? O1 Mn1 C34 O11 81.7(3) . . . . ? N2 Mn1 C34 O11 -85.0(3) . . . . ? N1 Mn1 C34 O11 -16.2(4) . . . . ? O12 Mn1 C34 O11 -178.2(5) . . . . ? O2 Mn1 C34 C32 -168(3) 2_657 . . . ? O1 Mn1 C34 C32 87(3) . . . . ? O11 Mn1 C34 C32 5(3) . . . . ? N2 Mn1 C34 C32 -80(3) . . . . ? N1 Mn1 C34 C32 -11(3) . . . . ? O12 Mn1 C34 C32 -173(3) . . . . ? N1 C35 C36 C37 -1.5(9) . . . . ? C35 C36 C37 C38 1.9(9) . . . . ? C36 C37 C38 C46 -2.1(9) . . . . ? C36 C37 C38 C39 177.1(6) . . . . ? C37 C38 C39 C40 179.3(6) . . . . ? C46 C38 C39 C40 -1.5(9) . . . . ? C38 C39 C40 C41 0.3(10) . . . . ? C39 C40 C41 C42 -177.3(6) . . . . ? C39 C40 C41 C45 -0.1(10) . . . . ? C45 C41 C42 C43 -0.2(11) . . . . ? C40 C41 C42 C43 177.0(7) . . . . ? C41 C42 C43 C44 1.2(12) . . . . ? C42 C43 C44 N2 0.3(12) . . . . ? C42 C41 C45 N2 -2.3(9) . . . . ? C40 C41 C45 N2 -179.6(6) . . . . ? C42 C41 C45 C46 178.5(6) . . . . ? C40 C41 C45 C46 1.1(8) . . . . ? C37 C38 C46 N1 2.0(8) . . . . ? C39 C38 C46 N1 -177.3(5) . . . . ? C37 C38 C46 C45 -178.3(5) . . . . ? C39 C38 C46 C45 2.5(8) . . . . ? N2 C45 C46 N1 -1.8(8) . . . . ? C41 C45 C46 N1 177.5(5) . . . . ? N2 C45 C46 C38 178.4(5) . . . . ? C41 C45 C46 C38 -2.3(8) . . . . ? N3 C47 C48 C49 -3.4(10) . . . . ? C47 C48 C49 C50 2.0(10) . . . . ? C48 C49 C50 C58 -0.3(10) . . . . ? C48 C49 C50 C51 180.0(7) . . . . ? C49 C50 C51 C52 -179.2(7) . . . . ? C58 C50 C51 C52 1.1(11) . . . . ? C50 C51 C52 C53 1.2(12) . . . . ? C51 C52 C53 C57 -2.8(11) . . . . ? C51 C52 C53 C54 176.4(7) . . . . ? C57 C53 C54 C55 1.1(11) . . . . ? C52 C53 C54 C55 -178.1(7) . . . . ? C53 C54 C55 C56 -1.2(12) . . . . ? C54 C55 C56 N4 0.8(12) . . . . ? C54 C53 C57 N4 -0.5(9) . . . . ? C52 C53 C57 N4 178.8(6) . . . . ? C54 C53 C57 C58 -177.4(6) . . . . ? C52 C53 C57 C58 1.9(9) . . . . ? N4 C57 C58 N3 2.0(9) . . . . ? C53 C57 C58 N3 179.1(5) . . . . ? N4 C57 C58 C50 -176.6(5) . . . . ? C53 C57 C58 C50 0.4(9) . . . . ? C49 C50 C58 N3 -0.3(9) . . . . ? C51 C50 C58 N3 179.4(6) . . . . ? C49 C50 C58 C57 178.4(5) . . . . ? C51 C50 C58 C57 -1.9(9) . . . . ? C36 C35 N1 C46 1.3(8) . . . . ? C36 C35 N1 Mn1 -175.1(4) . . . . ? C38 C46 N1 C35 -1.5(7) . . . . ? C45 C46 N1 C35 178.7(4) . . . . ? C38 C46 N1 Mn1 175.3(4) . . . . ? C45 C46 N1 Mn1 -4.4(6) . . . . ? O2 Mn1 N1 C35 -99.9(4) 2_657 . . . ? O1 Mn1 N1 C35 5.4(4) . . . . ? O11 Mn1 N1 C35 96.8(4) . . . . ? N2 Mn1 N1 C35 -177.7(5) . . . . ? O12 Mn1 N1 C35 120.9(4) . . . . ? C34 Mn1 N1 C35 104.4(4) . . . . ? O2 Mn1 N1 C46 83.7(4) 2_657 . . . ? O1 Mn1 N1 C46 -171.0(4) . . . . ? O11 Mn1 N1 C46 -79.7(4) . . . . ? N2 Mn1 N1 C46 5.9(3) . . . . ? O12 Mn1 N1 C46 -55.6(5) . . . . ? C34 Mn1 N1 C46 -72.1(4) . . . . ? C43 C44 N2 C45 -2.7(11) . . . . ? C43 C44 N2 Mn1 172.7(5) . . . . ? C41 C45 N2 C44 3.7(9) . . . . ? C46 C45 N2 C44 -177.0(5) . . . . ? C41 C45 N2 Mn1 -172.1(4) . . . . ? C46 C45 N2 Mn1 7.2(7) . . . . ? O2 Mn1 N2 C44 57.6(6) 2_657 . . . ? O1 Mn1 N2 C44 -169.7(6) . . . . ? O11 Mn1 N2 C44 -85.0(6) . . . . ? N1 Mn1 N2 C44 177.7(6) . . . . ? O12 Mn1 N2 C44 -29.0(6) . . . . ? C34 Mn1 N2 C44 -57.0(6) . . . . ? O2 Mn1 N2 C45 -126.9(4) 2_657 . . . ? O1 Mn1 N2 C45 5.7(10) . . . . ? O11 Mn1 N2 C45 90.5(4) . . . . ? N1 Mn1 N2 C45 -6.9(4) . . . . ? O12 Mn1 N2 C45 146.4(4) . . . . ? C34 Mn1 N2 C45 118.4(4) . . . . ? C48 C47 N3 C58 2.8(9) . . . . ? C48 C47 N3 Mn2 177.5(4) . . . . ? C57 C58 N3 C47 -179.6(5) . . . . ? C50 C58 N3 C47 -1.0(8) . . . . ? C57 C58 N3 Mn2 5.1(7) . . . . ? C50 C58 N3 Mn2 -176.3(4) . . . . ? O8 Mn2 N3 C47 98.7(4) 2_656 . . . ? O6 Mn2 N3 C47 -93.5(4) . . . . ? O7 Mn2 N3 C47 -3.2(4) . . . . ? N4 Mn2 N3 C47 178.3(5) . . . . ? O5 Mn2 N3 C47 -132.0(10) . . . . ? O8 Mn2 N3 C58 -86.4(4) 2_656 . . . ? O6 Mn2 N3 C58 81.5(4) . . . . ? O7 Mn2 N3 C58 171.7(4) . . . . ? N4 Mn2 N3 C58 -6.8(3) . . . . ? O5 Mn2 N3 C58 43.0(10) . . . . ? C55 C56 N4 C57 -0.2(11) . . . . ? C55 C56 N4 Mn2 -174.3(5) . . . . ? C53 C57 N4 C56 0.0(9) . . . . ? C58 C57 N4 C56 177.0(5) . . . . ? C53 C57 N4 Mn2 174.8(4) . . . . ? C58 C57 N4 Mn2 -8.3(7) . . . . ? O8 Mn2 N4 C56 -57.1(6) 2_656 . . . ? O6 Mn2 N4 C56 73.7(6) . . . . ? O7 Mn2 N4 C56 176.7(6) . . . . ? N3 Mn2 N4 C56 -177.9(6) . . . . ? O5 Mn2 N4 C56 24.6(7) . . . . ? O8 Mn2 N4 C57 128.7(4) 2_656 . . . ? O6 Mn2 N4 C57 -100.5(4) . . . . ? O7 Mn2 N4 C57 2.4(9) . . . . ? N3 Mn2 N4 C57 7.9(4) . . . . ? O5 Mn2 N4 C57 -149.6(6) . . . . ? O2 C1 O1 Mn1 -2.5(7) . . . . ? C2 C1 O1 Mn1 178.0(3) . . . . ? O2 Mn1 O1 C1 54.9(4) 2_657 . . . ? O11 Mn1 O1 C1 -160.8(4) . . . . ? N2 Mn1 O1 C1 -76.5(8) . . . . ? N1 Mn1 O1 C1 -64.5(4) . . . . ? O12 Mn1 O1 C1 143.5(4) . . . . ? C34 Mn1 O1 C1 171.5(4) . . . . ? O1 C1 O2 Mn1 -35.0(12) . . . 2_657 ? C2 C1 O2 Mn1 144.5(8) . . . 2_657 ? C14 C9 O3 C8 7.8(10) . . . . ? C10 C9 O3 C8 -173.4(6) . . . . ? C5 C8 O3 C9 164.0(6) . . . . ? C16 C15 O4 C12 -167.0(4) . . . . ? C17 C15 O4 C12 73.6(6) . . . . ? C11 C12 O4 C15 -125.3(5) . . . . ? C13 C12 O4 C15 59.7(7) . . . . ? O6 C17 O5 O5' 156(2) . . . . ? C15 C17 O5 O5' -30(3) . . . . ? O6 C17 O5 Mn2 5.3(8) . . . . ? O5' C17 O5 Mn2 -150(3) . . . . ? C15 C17 O5 Mn2 179.2(7) . . . . ? O8 Mn2 O5 O5' 80(6) 2_656 . . . ? O6 Mn2 O5 O5' -108(6) . . . . ? O7 Mn2 O5 O5' 178(6) . . . . ? N4 Mn2 O5 O5' -10(6) . . . . ? N3 Mn2 O5 O5' -57(7) . . . . ? O8 Mn2 O5 C17 -176.2(9) 2_656 . . . ? O6 Mn2 O5 C17 -3.8(6) . . . . ? O7 Mn2 O5 C17 -78.4(8) . . . . ? N4 Mn2 O5 C17 93.8(8) . . . . ? N3 Mn2 O5 C17 46.9(15) . . . . ? Mn2 O5 O5' C17 102(5) . . . . ? O6 C17 O5' O5 -33(3) . . . . ? C15 C17 O5' O5 157(2) . . . . ? O5 C17 O6 Mn2 -6.6(10) . . . . ? O5' C17 O6 Mn2 9.4(12) . . . . ? C15 C17 O6 Mn2 178.6(4) . . . . ? O8 Mn2 O6 C17 13.8(5) 2_656 . . . ? O7 Mn2 O6 C17 116.7(4) . . . . ? N4 Mn2 O6 C17 -78.9(4) . . . . ? N3 Mn2 O6 C17 -152.1(4) . . . . ? O5 Mn2 O6 C17 3.7(6) . . . . ? O8 C18 O7 Mn2 -0.5(8) . . . . ? C19 C18 O7 Mn2 -177.2(3) . . . . ? O8 Mn2 O7 C18 -53.0(5) 2_656 . . . ? O6 Mn2 O7 C18 175.5(5) . . . . ? N4 Mn2 O7 C18 72.1(8) . . . . ? N3 Mn2 O7 C18 66.9(4) . . . . ? O5 Mn2 O7 C18 -137.2(6) . . . . ? O7 C18 O8 Mn2 34.2(13) . . . 2_656 ? C19 C18 O8 Mn2 -149.1(8) . . . 2_656 ? C27 C26 O9 C25 -171.4(6) . . . . ? C31 C26 O9 C25 9.4(9) . . . . ? C22 C25 O9 C26 -177.1(6) . . . . ? C30 C29 O10 C32 176.9(4) . . . . ? C28 C29 O10 C32 -2.0(6) . . . . ? C34 C32 O10 C29 75.0(5) . . . . ? C33 C32 O10 C29 -165.6(4) . . . . ? O12 C34 O11 Mn1 -1.9(5) . . . . ? C32 C34 O11 Mn1 -179.4(3) . . . . ? O2 Mn1 O11 C34 10.9(4) 2_657 . . . ? O1 Mn1 O11 C34 -99.9(3) . . . . ? N2 Mn1 O11 C34 94.4(3) . . . . ? N1 Mn1 O11 C34 166.4(3) . . . . ? O12 Mn1 O11 C34 1.0(3) . . . . ? O11 C34 O12 Mn1 1.7(5) . . . . ? C32 C34 O12 Mn1 179.1(4) . . . . ? O2 Mn1 O12 C34 -174.9(3) 2_657 . . . ? O1 Mn1 O12 C34 83.7(3) . . . . ? O11 Mn1 O12 C34 -1.0(3) . . . . ? N2 Mn1 O12 C34 -87.1(3) . . . . ? N1 Mn1 O12 C34 -30.3(4) . . . . ? 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 O1W H1A O10 0.898(10) 2.34(6) 3.043(3) 135(7) 1_545 C42 H42 O1W 0.93 2.60 3.385(9) 142.9 . C25 H25A O11 0.97 2.27 3.041(7) 135.3 1_565 C52 H52 O5 0.93 2.56 3.392(14) 149.5 1_565 C54 H54 O2W 0.93 2.57 3.417(12) 151.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.265 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.037 #=========================END data_Compound-6 _database_code_depnum_ccdc_archive 'CCDC 877936' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H56 Cd2 N8 O12' _chemical_formula_sum 'C54 H56 Cd2 N8 O12' _chemical_formula_weight 1233.87 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.8443(3) _cell_length_b 16.4131(9) _cell_length_c 23.3284(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.720(4) _cell_angle_gamma 90.00 _cell_volume 2615.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9740 _exptl_absorpt_correction_T_max 0.9825 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16529 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7512 _reflns_number_gt 5392 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0198P)^2^+0.2371P] 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' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 7512 _refine_ls_number_parameters 685 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Cd1 Cd -0.77680(7) 0.20901(4) -0.07893(2) 0.04351(17) Uani 1 1 d . . . Cd2 Cd 0.71738(10) 0.56813(5) 0.43745(3) 0.0625(2) Uani 1 1 d . . . C1 C 1.9155(13) 0.2739(8) 0.8585(4) 0.051(3) Uani 1 1 d . . . C2 C 1.7310(12) 0.3095(7) 0.8325(3) 0.044(2) Uani 1 1 d . . . C3 C 1.6038(12) 0.2626(7) 0.7970(3) 0.064(3) Uani 1 1 d . . . H3 H 1.6379 0.2098 0.7872 0.077 Uiso 1 1 calc R . . C4 C 1.4287(13) 0.2948(7) 0.7766(4) 0.063(3) Uani 1 1 d . . . H4 H 1.3485 0.2642 0.7511 0.076 Uiso 1 1 calc R . . C5 C 1.3668(13) 0.3707(7) 0.7924(4) 0.052(3) Uani 1 1 d . . . C6 C 1.4889(14) 0.4166(8) 0.8271(4) 0.064(3) Uani 1 1 d . . . H6 H 1.4520 0.4691 0.8368 0.076 Uiso 1 1 calc R . . C7 C 1.6702(15) 0.3859(7) 0.8486(4) 0.057(3) Uani 1 1 d . . . H7 H 1.7499 0.4172 0.8738 0.068 Uiso 1 1 calc R . . C8 C 1.1694(12) 0.4041(7) 0.7714(4) 0.071(3) Uani 1 1 d . . . H8A H 1.0850 0.3599 0.7575 0.085 Uiso 1 1 calc R . . H8B H 1.1084 0.4307 0.8027 0.085 Uiso 1 1 calc R . . C9 C 1.0265(13) 0.4989(6) 0.7042(4) 0.048(3) Uani 1 1 d . . . C10 C 1.0540(13) 0.5627(8) 0.6679(4) 0.066(3) Uani 1 1 d . . . H10 H 1.1807 0.5779 0.6603 0.079 Uiso 1 1 calc R . . C11 C 0.8954(14) 0.6057(8) 0.6420(4) 0.079(4) Uani 1 1 d . . . H11 H 0.9154 0.6492 0.6175 0.094 Uiso 1 1 calc R . . C12 C 0.7069(11) 0.5817(7) 0.6536(3) 0.053(3) Uani 1 1 d . . . C13 C 0.6792(12) 0.5180(6) 0.6902(3) 0.046(2) Uani 1 1 d . . . H13 H 0.5530 0.5029 0.6984 0.055 Uiso 1 1 calc R . . C14 C 0.8392(13) 0.4757(6) 0.7152(3) 0.058(3) Uani 1 1 d . . . H14 H 0.8196 0.4318 0.7394 0.070 Uiso 1 1 calc R . . C15 C 0.5526(13) 0.6806(6) 0.5899(3) 0.059(3) Uani 1 1 d . . . H15 H 0.6480 0.7218 0.6038 0.070 Uiso 1 1 calc R . . C16 C 0.3527(15) 0.7209(10) 0.5829(4) 0.087(4) Uani 1 1 d . . . H16A H 0.3166 0.7406 0.6195 0.131 Uiso 1 1 calc R . . H16B H 0.2576 0.6818 0.5683 0.131 Uiso 1 1 calc R . . H16C H 0.3575 0.7656 0.5565 0.131 Uiso 1 1 calc R . . C17 C 0.6178(16) 0.6465(8) 0.5348(4) 0.060(3) Uani 1 1 d . . . C18 C 0.4634(16) 0.4920(8) 0.3605(4) 0.066(3) Uani 1 1 d . . . C19 C 0.3201(14) 0.4374(7) 0.3265(3) 0.056(3) Uani 1 1 d . . . C20 C 0.3811(16) 0.3655(7) 0.3058(5) 0.088(4) Uani 1 1 d . . . H20 H 0.5121 0.3506 0.3113 0.106 Uiso 1 1 calc R . . C21 C 0.2513(15) 0.3148(7) 0.2770(4) 0.081(3) Uani 1 1 d . . . H21 H 0.2966 0.2670 0.2611 0.097 Uiso 1 1 calc R . . C22 C 0.0603(15) 0.3323(8) 0.2711(4) 0.067(3) Uani 1 1 d . . . C23 C -0.0013(18) 0.4049(10) 0.2897(6) 0.101(5) Uani 1 1 d . . . H23 H -0.1336 0.4179 0.2852 0.121 Uiso 1 1 calc R . . C24 C 0.1309(17) 0.4615(9) 0.3159(5) 0.094(4) Uani 1 1 d . . . H24 H 0.0904 0.5134 0.3256 0.113 Uiso 1 1 calc R . . C25 C -0.0895(16) 0.2683(8) 0.2484(5) 0.096(4) Uani 1 1 d . . . H25A H -0.0212 0.2223 0.2330 0.115 Uiso 1 1 calc R . . H25B H -0.1634 0.2489 0.2797 0.115 Uiso 1 1 calc R . . C26 C -0.3713(18) 0.2501(9) 0.1866(4) 0.072(4) Uani 1 1 d . . . C27 C -0.4902(13) 0.2804(6) 0.1414(4) 0.060(3) Uani 1 1 d . . . H27 H -0.4635 0.3310 0.1257 0.072 Uiso 1 1 calc R . . C28 C -0.6486(15) 0.2355(6) 0.1198(4) 0.067(3) Uani 1 1 d . . . H28 H -0.7275 0.2555 0.0890 0.081 Uiso 1 1 calc R . . C29 C -0.6904(15) 0.1621(7) 0.1432(4) 0.056(3) Uani 1 1 d . . . C30 C -0.5708(14) 0.1319(7) 0.1871(4) 0.072(3) Uani 1 1 d . . . H30 H -0.5964 0.0811 0.2025 0.087 Uiso 1 1 calc R . . C31 C -0.4085(17) 0.1774(8) 0.2092(4) 0.077(4) Uani 1 1 d . . . H31 H -0.3277 0.1569 0.2393 0.092 Uiso 1 1 calc R . . C32 C -0.9794(13) 0.1391(6) 0.0824(4) 0.058(3) Uani 1 1 d . . . H32 H -1.0230 0.1935 0.0932 0.070 Uiso 1 1 calc R . . C33 C -1.1528(15) 0.0813(9) 0.0818(3) 0.080(4) Uani 1 1 d . . . H33A H -1.2031 0.0798 0.1192 0.121 Uiso 1 1 calc R . . H33B H -1.1116 0.0277 0.0714 0.121 Uiso 1 1 calc R . . H33C H -1.2532 0.1000 0.0542 0.121 Uiso 1 1 calc R . . C34 C -0.8973(14) 0.1439(7) 0.0231(4) 0.047(2) Uani 1 1 d . . . C35 C -0.4177(13) 0.0972(7) -0.1071(4) 0.057(3) Uani 1 1 d . . . H35 H -0.3487 0.1155 -0.0739 0.069 Uiso 1 1 calc R . . C36 C -0.4902(16) 0.0304(7) -0.1862(4) 0.069(4) Uani 1 1 d . . . H36 H -0.4850 -0.0045 -0.2175 0.083 Uiso 1 1 calc R . . C37 C -0.6434(12) 0.0783(7) -0.1735(3) 0.055(3) Uani 1 1 d . . . H37 H -0.7612 0.0815 -0.1956 0.066 Uiso 1 1 calc R . . C38 C -0.1541(15) 0.0057(8) -0.1391(4) 0.080(4) Uani 1 1 d . . . H38A H -0.1410 -0.0312 -0.1711 0.096 Uiso 1 1 calc R . . H38B H -0.0558 0.0479 -0.1414 0.096 Uiso 1 1 calc R . . C39 C -0.1169(13) -0.0378(8) -0.0874(4) 0.072(3) Uani 1 1 d . . . H39A H -0.2076 -0.0832 -0.0873 0.087 Uiso 1 1 calc R . . H39B H -0.1457 -0.0022 -0.0558 0.087 Uiso 1 1 calc R . . C40 C 0.0886(13) -0.0707(8) -0.0759(4) 0.059(3) Uani 1 1 d . . . H40A H 0.1148 -0.1106 -0.1051 0.071 Uiso 1 1 calc R . . H40B H 0.1818 -0.0265 -0.0786 0.071 Uiso 1 1 calc R . . C41 C 0.1161(12) -0.1086(8) -0.0190(4) 0.068(3) Uani 1 1 d . . . H41A H 0.0642 -0.0720 0.0088 0.082 Uiso 1 1 calc R . . H41B H 0.0383 -0.1580 -0.0193 0.082 Uiso 1 1 calc R . . C42 C 0.3859(12) -0.2023(7) 0.0157(3) 0.052(3) Uani 1 1 d . . . H42 H 0.3131 -0.2500 0.0115 0.062 Uiso 1 1 calc R . . C43 C 0.4630(14) -0.0757(7) 0.0132(4) 0.058(3) Uani 1 1 d . . . H43 H 0.4589 -0.0196 0.0077 0.069 Uiso 1 1 calc R . . C44 C 0.6138(13) -0.1195(7) 0.0350(3) 0.051(2) Uani 1 1 d . . . H44 H 0.7346 -0.0973 0.0471 0.061 Uiso 1 1 calc R . . C45 C 1.097(3) 0.4888(11) 0.5086(7) 0.151(7) Uani 1 1 d . . . H45 H 1.1344 0.5383 0.5253 0.181 Uiso 1 1 calc R . . C46 C 1.100(2) 0.3636(10) 0.4833(6) 0.124(6) Uani 1 1 d . . . H46 H 1.1299 0.3086 0.4799 0.149 Uiso 1 1 calc R . . C47 C 0.954(2) 0.4030(10) 0.4567(5) 0.104(5) Uani 1 1 d . . . H47 H 0.8689 0.3804 0.4283 0.125 Uiso 1 1 calc R . . C48 C 1.415(2) 0.4079(15) 0.5429(11) 0.204(11) Uani 1 1 d . . . H48A H 1.4971 0.3894 0.5131 0.245 Uiso 1 1 calc R . . H48B H 1.4671 0.4595 0.5575 0.245 Uiso 1 1 calc R . . C49 C 1.421(3) 0.3520(14) 0.5864(8) 0.179(9) Uani 1 1 d . . . H49A H 1.3405 0.3051 0.5753 0.215 Uiso 1 1 calc R . . H49B H 1.3714 0.3758 0.6207 0.215 Uiso 1 1 calc R . . C50 C 1.646(3) 0.3252(12) 0.5982(7) 0.146(7) Uani 1 1 d . . . H50A H 1.7056 0.3160 0.5622 0.176 Uiso 1 1 calc R . . H50B H 1.7190 0.3678 0.6190 0.176 Uiso 1 1 calc R . . C51 C 1.650(2) 0.2525(13) 0.6312(7) 0.150(7) Uani 1 1 d . . . H51A H 1.5611 0.2130 0.6130 0.180 Uiso 1 1 calc R . . H51B H 1.6076 0.2640 0.6692 0.180 Uiso 1 1 calc R . . C52 C 1.9422(19) 0.1824(9) 0.5951(5) 0.105(5) Uani 1 1 d . . . H52 H 1.8969 0.1813 0.5566 0.127 Uiso 1 1 calc R . . C53 C 1.959(2) 0.2102(15) 0.6844(7) 0.161(9) Uani 1 1 d . . . H53 H 1.9375 0.2317 0.7203 0.193 Uiso 1 1 calc R . . C54 C 2.1070(19) 0.1642(8) 0.6702(5) 0.092(4) Uani 1 1 d . . . H54 H 2.2041 0.1447 0.6964 0.110 Uiso 1 1 calc R . . N1 N -0.6019(10) 0.1207(5) -0.1243(3) 0.048(2) Uani 1 1 d . . . N2 N -0.3476(12) 0.0433(6) -0.1448(3) 0.056(3) Uani 1 1 d . . . N3 N 0.3173(10) -0.1294(6) 0.0008(3) 0.050(2) Uani 1 1 d . . . N4 N 0.5719(10) -0.1997(5) 0.0375(3) 0.046(2) Uani 1 1 d . . . N5 N 0.9426(14) 0.4802(7) 0.4757(4) 0.074(3) Uani 1 1 d . . . N6 N 1.2001(19) 0.4202(9) 0.5171(6) 0.126(5) Uani 1 1 d . . . N7 N 1.8494(15) 0.2187(9) 0.6361(5) 0.114(4) Uani 1 1 d . . . N8 N 2.1007(13) 0.1493(6) 0.6146(3) 0.070(3) Uani 1 1 d . . . O1 O 1.9664(8) 0.2042(6) 0.8447(2) 0.0642(17) Uani 1 1 d . . . O2 O 2.0233(9) 0.3179(4) 0.8921(3) 0.0577(18) Uani 1 1 d . . . O3 O 1.1925(8) 0.4597(4) 0.7273(2) 0.066(2) Uani 1 1 d . . . O4 O 0.5391(8) 0.6213(4) 0.6330(2) 0.0651(19) Uani 1 1 d . . . O5 O 0.7494(14) 0.6785(5) 0.5095(3) 0.103(3) Uani 1 1 d . . . O6 O 0.5368(12) 0.5870(7) 0.5148(3) 0.112(3) Uani 1 1 d . . . O7 O 0.6144(14) 0.4616(8) 0.3789(5) 0.182(6) Uani 1 1 d . . . O8 O 0.4288(13) 0.5587(8) 0.3738(4) 0.144(4) Uani 1 1 d . . . O9 O -0.2168(10) 0.3014(5) 0.2059(3) 0.081(2) Uani 1 1 d . . . O10 O -0.8424(10) 0.1108(4) 0.1250(2) 0.0687(19) Uani 1 1 d . . . O11 O -0.7400(10) 0.1154(5) 0.0126(2) 0.070(2) Uani 1 1 d . . . O12 O -1.0011(9) 0.1835(5) -0.0141(3) 0.077(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0335(3) 0.0423(5) 0.0540(3) -0.0014(3) -0.0031(2) 0.0035(4) Cd2 0.0584(5) 0.0573(6) 0.0703(4) -0.0030(4) -0.0061(3) -0.0046(4) C1 0.031(5) 0.060(9) 0.062(6) 0.016(5) 0.006(4) -0.002(6) C2 0.030(5) 0.065(8) 0.038(4) 0.014(4) 0.002(3) -0.003(5) C3 0.046(6) 0.072(9) 0.072(6) 0.011(5) -0.002(4) 0.004(5) C4 0.044(6) 0.077(9) 0.066(6) 0.009(6) -0.011(4) 0.002(6) C5 0.038(6) 0.065(9) 0.052(6) 0.020(5) 0.005(4) -0.004(6) C6 0.048(7) 0.066(9) 0.078(7) 0.018(6) 0.010(5) 0.019(6) C7 0.044(6) 0.062(9) 0.064(6) 0.013(6) -0.001(5) -0.009(6) C8 0.047(6) 0.091(10) 0.074(6) 0.037(6) -0.004(4) 0.005(6) C9 0.043(6) 0.048(7) 0.053(5) 0.015(5) -0.005(4) 0.013(5) C10 0.039(5) 0.091(10) 0.068(6) 0.024(7) -0.004(4) -0.010(6) C11 0.055(7) 0.099(11) 0.082(7) 0.045(6) 0.005(5) 0.001(7) C12 0.037(5) 0.076(9) 0.045(5) 0.003(5) 0.003(3) -0.005(6) C13 0.039(5) 0.060(7) 0.039(5) 0.009(4) 0.004(4) -0.005(5) C14 0.050(6) 0.058(8) 0.067(6) 0.023(5) 0.011(4) 0.003(5) C15 0.067(6) 0.063(9) 0.045(5) 0.013(4) -0.003(4) 0.015(5) C16 0.077(7) 0.098(13) 0.089(6) 0.032(8) 0.011(5) 0.035(9) C17 0.062(7) 0.056(9) 0.061(7) -0.001(6) 0.001(5) 0.016(6) C18 0.045(7) 0.056(9) 0.096(8) -0.016(6) -0.006(5) 0.009(6) C19 0.056(6) 0.064(9) 0.048(5) -0.007(5) -0.006(4) -0.005(6) C20 0.075(8) 0.068(10) 0.117(9) -0.027(7) -0.027(6) 0.008(7) C21 0.064(8) 0.080(10) 0.099(8) -0.016(7) -0.001(5) 0.009(7) C22 0.060(7) 0.096(11) 0.044(5) -0.003(5) -0.005(4) -0.001(7) C23 0.049(8) 0.110(14) 0.142(11) -0.049(10) -0.014(7) 0.016(9) C24 0.064(8) 0.093(12) 0.123(9) -0.046(8) -0.007(6) 0.008(8) C25 0.080(8) 0.095(11) 0.109(9) -0.006(7) -0.032(6) -0.006(7) C26 0.078(8) 0.066(10) 0.070(7) -0.006(6) -0.012(6) -0.018(7) C27 0.061(6) 0.058(8) 0.059(6) 0.010(5) -0.012(5) -0.021(6) C28 0.081(7) 0.056(9) 0.061(6) 0.001(5) -0.020(5) -0.018(6) C29 0.074(8) 0.035(7) 0.057(6) 0.009(5) -0.010(5) -0.019(6) C30 0.094(8) 0.053(8) 0.069(7) 0.016(5) -0.005(5) -0.016(6) C31 0.095(9) 0.064(9) 0.067(7) 0.004(6) -0.025(6) -0.019(7) C32 0.054(6) 0.058(8) 0.063(6) -0.001(5) 0.003(4) -0.016(6) C33 0.081(7) 0.089(11) 0.073(6) -0.005(6) 0.017(5) -0.038(8) C34 0.045(6) 0.037(7) 0.059(6) -0.006(5) -0.001(4) -0.010(5) C35 0.051(6) 0.059(9) 0.060(6) 0.005(5) -0.011(4) 0.016(6) C36 0.062(8) 0.086(11) 0.060(6) -0.018(5) 0.010(5) 0.013(7) C37 0.048(6) 0.066(8) 0.051(5) -0.002(5) -0.003(4) 0.003(6) C38 0.058(7) 0.091(11) 0.092(8) 0.007(7) 0.020(5) 0.034(7) C39 0.038(6) 0.083(10) 0.094(7) 0.034(6) -0.015(4) 0.015(6) C40 0.036(5) 0.071(9) 0.072(6) 0.019(5) 0.015(4) 0.020(6) C41 0.036(6) 0.072(9) 0.097(7) 0.026(6) -0.003(5) 0.001(5) C42 0.038(6) 0.049(8) 0.067(6) 0.016(5) -0.012(4) -0.019(5) C43 0.054(6) 0.041(8) 0.079(6) 0.014(5) 0.004(4) 0.007(6) C44 0.040(6) 0.041(7) 0.070(5) 0.013(5) -0.002(4) -0.005(5) C45 0.178(17) 0.077(13) 0.185(15) -0.045(11) -0.075(13) 0.069(13) C46 0.152(15) 0.058(12) 0.158(12) -0.016(9) -0.034(10) 0.041(11) C47 0.107(11) 0.081(13) 0.119(10) -0.015(9) -0.039(7) 0.007(9) C48 0.095(13) 0.15(2) 0.36(3) 0.08(2) -0.031(16) -0.005(14) C49 0.26(3) 0.12(2) 0.152(15) -0.009(13) -0.033(15) -0.02(2) C50 0.166(17) 0.112(17) 0.150(13) -0.002(10) -0.074(11) 0.058(13) C51 0.127(15) 0.138(19) 0.187(16) -0.021(13) 0.019(11) 0.058(13) C52 0.102(10) 0.133(17) 0.080(7) -0.018(7) -0.004(6) 0.045(10) C53 0.080(10) 0.24(3) 0.166(15) -0.139(18) 0.021(10) -0.031(15) C54 0.100(10) 0.105(12) 0.070(8) -0.024(6) 0.002(6) -0.007(8) N1 0.041(5) 0.052(6) 0.051(4) 0.004(4) 0.000(3) 0.003(4) N2 0.041(5) 0.061(8) 0.066(5) 0.000(5) 0.007(4) 0.016(5) N3 0.035(5) 0.045(7) 0.068(5) 0.014(4) -0.001(3) 0.004(4) N4 0.038(5) 0.035(6) 0.065(4) 0.004(4) 0.002(3) -0.002(4) N5 0.067(7) 0.044(8) 0.108(7) -0.012(6) -0.026(5) 0.013(6) N6 0.117(10) 0.073(11) 0.180(11) -0.010(9) -0.051(8) 0.022(9) N7 0.078(7) 0.127(12) 0.139(9) -0.065(9) 0.012(6) 0.047(9) N8 0.071(6) 0.082(8) 0.057(5) -0.004(4) 0.006(4) 0.017(6) O1 0.051(4) 0.060(6) 0.079(4) -0.008(4) -0.011(3) 0.016(5) O2 0.046(4) 0.049(5) 0.076(4) 0.007(3) -0.014(3) -0.003(4) O3 0.045(4) 0.084(6) 0.068(4) 0.036(4) -0.004(3) 0.008(4) O4 0.048(4) 0.083(6) 0.065(4) 0.035(3) 0.002(3) 0.004(4) O5 0.157(8) 0.065(7) 0.095(5) -0.003(4) 0.065(5) -0.031(6) O6 0.098(6) 0.119(10) 0.120(6) -0.060(6) 0.022(4) -0.037(6) O7 0.092(7) 0.147(12) 0.291(13) -0.108(10) -0.099(8) 0.029(7) O8 0.097(7) 0.112(10) 0.213(9) -0.077(9) -0.061(6) 0.017(8) O9 0.086(5) 0.077(6) 0.077(4) 0.009(4) -0.026(4) -0.027(5) O10 0.092(5) 0.052(5) 0.060(4) 0.011(3) -0.010(3) -0.028(4) O11 0.065(5) 0.071(6) 0.074(4) -0.002(3) 0.008(3) 0.013(4) O12 0.052(4) 0.108(8) 0.071(4) 0.023(4) -0.001(3) 0.014(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 2.196(8) . ? Cd1 N4 2.229(8) 2 ? Cd1 O12 2.263(6) . ? Cd1 O2 2.324(6) 1_254 ? Cd1 O1 2.421(5) 1_254 ? Cd1 O11 2.629(6) . ? Cd1 C1 2.703(9) 1_254 ? Cd2 N8 2.235(9) 2_856 ? Cd2 N5 2.253(10) . ? Cd2 O6 2.274(7) . ? Cd2 O7 2.300(10) . ? Cd2 O8 2.397(8) . ? Cd2 O5 2.471(8) . ? Cd2 C18 2.721(11) . ? Cd2 C17 2.735(10) . ? C1 O1 1.244(13) . ? C1 O2 1.266(11) . ? C1 C2 1.484(12) . ? C1 Cd1 2.703(9) 1_856 ? C2 C7 1.382(14) . ? C2 C3 1.394(12) . ? C3 C4 1.366(12) . ? C3 H3 0.9300 . ? C4 C5 1.373(13) . ? C4 H4 0.9300 . ? C5 C6 1.355(14) . ? C5 C8 1.510(12) . ? C6 C7 1.401(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.391(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.367(14) . ? C9 C14 1.378(11) . ? C9 O3 1.385(10) . ? C10 C11 1.399(13) . ? C10 H10 0.9300 . ? C11 C12 1.392(12) . ? C11 H11 0.9300 . ? C12 C13 1.372(12) . ? C12 O4 1.379(9) . ? C13 C14 1.392(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.407(10) . ? C15 C17 1.496(13) . ? C15 C16 1.518(13) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.203(14) . ? C17 O5 1.227(12) . ? C18 O8 1.168(15) . ? C18 O7 1.202(12) . ? C18 C19 1.514(14) . ? C19 C20 1.350(14) . ? C19 C24 1.360(13) . ? C20 C21 1.362(13) . ? C20 H20 0.9300 . ? C21 C22 1.337(12) . ? C21 H21 0.9300 . ? C22 C23 1.344(17) . ? C22 C25 1.538(14) . ? C23 C24 1.408(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.388(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C31 1.337(14) . ? C26 C27 1.381(14) . ? C26 O9 1.402(13) . ? C27 C28 1.380(12) . ? C27 H27 0.9300 . ? C28 C29 1.361(13) . ? C28 H28 0.9300 . ? C29 C30 1.362(12) . ? C29 O10 1.382(10) . ? C30 C31 1.408(13) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O10 1.400(10) . ? C32 C33 1.518(13) . ? C32 C34 1.530(12) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O11 1.213(11) . ? C34 O12 1.264(11) . ? C35 N1 1.354(10) . ? C35 N2 1.358(12) . ? C35 H35 0.9300 . ? C36 N2 1.344(12) . ? C36 C37 1.359(13) . ? C36 H36 0.9300 . ? C37 N1 1.355(11) . ? C37 H37 0.9300 . ? C38 C39 1.410(12) . ? C38 N2 1.459(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.515(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.467(12) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N3 1.464(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N3 1.322(12) . ? C42 N4 1.340(10) . ? C42 H42 0.9300 . ? C43 C44 1.332(13) . ? C43 N3 1.349(12) . ? C43 H43 0.9300 . ? C44 N4 1.350(12) . ? C44 H44 0.9300 . ? C45 N5 1.272(15) . ? C45 N6 1.337(18) . ? C45 H45 0.9300 . ? C46 C47 1.312(17) . ? C46 N6 1.372(17) . ? C46 H46 0.9300 . ? C47 N5 1.347(16) . ? C47 H47 0.9300 . ? C48 C49 1.37(2) . ? C48 N6 1.569(19) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.61(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.42(2) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 N7 1.469(17) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 N8 1.271(13) . ? C52 N7 1.324(13) . ? C52 H52 0.9300 . ? C53 C54 1.321(19) . ? C53 N7 1.322(17) . ? C53 H53 0.9300 . ? C54 N8 1.319(11) . ? C54 H54 0.9300 . ? N4 Cd1 2.229(8) 2_545 ? N8 Cd2 2.235(8) 2_846 ? O1 Cd1 2.421(5) 1_856 ? O2 Cd1 2.324(6) 1_856 ? 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 N1 Cd1 N4 107.8(3) . 2 ? N1 Cd1 O12 128.0(3) . . ? N4 Cd1 O12 105.6(3) 2 . ? N1 Cd1 O2 134.1(2) . 1_254 ? N4 Cd1 O2 87.2(3) 2 1_254 ? O12 Cd1 O2 85.7(2) . 1_254 ? N1 Cd1 O1 90.9(2) . 1_254 ? N4 Cd1 O1 138.3(3) 2 1_254 ? O12 Cd1 O1 89.7(2) . 1_254 ? O2 Cd1 O1 54.9(3) 1_254 1_254 ? N1 Cd1 O11 88.8(2) . . ? N4 Cd1 O11 90.9(2) 2 . ? O12 Cd1 O11 51.9(2) . . ? O2 Cd1 O11 135.2(2) 1_254 . ? O1 Cd1 O11 127.2(3) 1_254 . ? N1 Cd1 C1 115.4(3) . 1_254 ? N4 Cd1 C1 114.6(3) 2 1_254 ? O12 Cd1 C1 84.0(2) . 1_254 ? O2 Cd1 C1 27.9(3) 1_254 1_254 ? O1 Cd1 C1 27.4(3) 1_254 1_254 ? O11 Cd1 C1 134.4(2) . 1_254 ? N8 Cd2 N5 101.9(4) 2_856 . ? N8 Cd2 O6 134.5(4) 2_856 . ? N5 Cd2 O6 99.5(4) . . ? N8 Cd2 O7 106.9(4) 2_856 . ? N5 Cd2 O7 85.6(4) . . ? O6 Cd2 O7 114.4(4) . . ? N8 Cd2 O8 99.7(4) 2_856 . ? N5 Cd2 O8 136.0(4) . . ? O6 Cd2 O8 91.8(3) . . ? O7 Cd2 O8 51.3(4) . . ? N8 Cd2 O5 84.5(3) 2_856 . ? N5 Cd2 O5 99.9(3) . . ? O6 Cd2 O5 52.4(3) . . ? O7 Cd2 O5 166.2(4) . . ? O8 Cd2 O5 120.1(4) . . ? N8 Cd2 C18 105.7(3) 2_856 . ? N5 Cd2 C18 111.0(4) . . ? O6 Cd2 C18 103.3(3) . . ? O7 Cd2 C18 26.0(3) . . ? O8 Cd2 C18 25.4(3) . . ? O5 Cd2 C18 144.1(3) . . ? N8 Cd2 C17 110.4(4) 2_856 . ? N5 Cd2 C17 100.0(3) . . ? O6 Cd2 C17 25.7(3) . . ? O7 Cd2 C17 140.1(4) . . ? O8 Cd2 C17 107.7(3) . . ? O5 Cd2 C17 26.7(3) . . ? C18 Cd2 C17 125.5(3) . . ? O1 C1 O2 121.5(9) . . ? O1 C1 C2 120.1(9) . . ? O2 C1 C2 118.4(10) . . ? O1 C1 Cd1 63.6(5) . 1_856 ? O2 C1 Cd1 59.2(5) . 1_856 ? C2 C1 Cd1 171.1(6) . 1_856 ? C7 C2 C3 118.4(9) . . ? C7 C2 C1 120.6(9) . . ? C3 C2 C1 120.6(10) . . ? C4 C3 C2 119.6(10) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 122.4(10) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 118.4(9) . . ? C6 C5 C8 119.8(11) . . ? C4 C5 C8 121.8(9) . . ? C5 C6 C7 120.7(11) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 120.3(10) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? O3 C8 C5 109.7(7) . . ? O3 C8 H8A 109.7 . . ? C5 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C5 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C14 119.7(8) . . ? C10 C9 O3 117.0(8) . . ? C14 C9 O3 123.2(8) . . ? C9 C10 C11 121.3(9) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C12 C11 C10 118.5(10) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C13 C12 O4 115.5(7) . . ? C13 C12 C11 120.3(8) . . ? O4 C12 C11 124.1(9) . . ? C12 C13 C14 120.3(8) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 C13 120.0(8) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O4 C15 C17 113.1(9) . . ? O4 C15 C16 106.1(7) . . ? C17 C15 C16 112.8(7) . . ? O4 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C16 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 119.7(10) . . ? O6 C17 C15 118.8(11) . . ? O5 C17 C15 121.5(11) . . ? O6 C17 Cd2 55.2(6) . . ? O5 C17 Cd2 64.6(6) . . ? C15 C17 Cd2 173.6(9) . . ? O8 C18 O7 118.5(12) . . ? O8 C18 C19 124.0(11) . . ? O7 C18 C19 117.1(12) . . ? O8 C18 Cd2 61.6(6) . . ? O7 C18 Cd2 57.0(7) . . ? C19 C18 Cd2 169.1(8) . . ? C20 C19 C24 120.1(10) . . ? C20 C19 C18 119.9(10) . . ? C24 C19 C18 120.0(11) . . ? C19 C20 C21 120.2(10) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 121.4(11) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 118.9(11) . . ? C21 C22 C25 120.9(12) . . ? C23 C22 C25 120.0(11) . . ? C22 C23 C24 121.2(12) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C19 C24 C23 117.7(12) . . ? C19 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? O9 C25 C22 110.7(10) . . ? O9 C25 H25A 109.5 . . ? C22 C25 H25A 109.5 . . ? O9 C25 H25B 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C31 C26 C27 120.3(11) . . ? C31 C26 O9 124.7(11) . . ? C27 C26 O9 115.0(11) . . ? C28 C27 C26 119.8(10) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.5(10) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 119.4(10) . . ? C28 C29 O10 126.1(9) . . ? C30 C29 O10 114.4(9) . . ? C29 C30 C31 120.3(10) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C26 C31 C30 119.7(11) . . ? C26 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? O10 C32 C33 106.7(8) . . ? O10 C32 C34 113.0(8) . . ? C33 C32 C34 110.8(7) . . ? O10 C32 H32 108.7 . . ? C33 C32 H32 108.7 . . ? C34 C32 H32 108.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O11 C34 O12 121.8(8) . . ? O11 C34 C32 123.1(8) . . ? O12 C34 C32 115.1(9) . . ? N1 C35 N2 110.7(8) . . ? N1 C35 H35 124.6 . . ? N2 C35 H35 124.6 . . ? N2 C36 C37 106.6(9) . . ? N2 C36 H36 126.7 . . ? C37 C36 H36 126.7 . . ? N1 C37 C36 111.1(8) . . ? N1 C37 H37 124.5 . . ? C36 C37 H37 124.5 . . ? C39 C38 N2 113.9(8) . . ? C39 C38 H38A 108.8 . . ? N2 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? N2 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C38 C39 C40 116.5(8) . . ? C38 C39 H39A 108.2 . . ? C40 C39 H39A 108.2 . . ? C38 C39 H39B 108.2 . . ? C40 C39 H39B 108.2 . . ? H39A C39 H39B 107.3 . . ? C41 C40 C39 112.0(7) . . ? C41 C40 H40A 109.2 . . ? C39 C40 H40A 109.2 . . ? C41 C40 H40B 109.2 . . ? C39 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? N3 C41 C40 116.6(7) . . ? N3 C41 H41A 108.1 . . ? C40 C41 H41A 108.1 . . ? N3 C41 H41B 108.1 . . ? C40 C41 H41B 108.1 . . ? H41A C41 H41B 107.3 . . ? N3 C42 N4 112.6(8) . . ? N3 C42 H42 123.7 . . ? N4 C42 H42 123.7 . . ? C44 C43 N3 105.8(10) . . ? C44 C43 H43 127.1 . . ? N3 C43 H43 127.1 . . ? C43 C44 N4 112.4(9) . . ? C43 C44 H44 123.8 . . ? N4 C44 H44 123.8 . . ? N5 C45 N6 114.0(15) . . ? N5 C45 H45 123.0 . . ? N6 C45 H45 123.0 . . ? C47 C46 N6 106.0(14) . . ? C47 C46 H46 127.0 . . ? N6 C46 H46 127.0 . . ? C46 C47 N5 111.5(12) . . ? C46 C47 H47 124.3 . . ? N5 C47 H47 124.3 . . ? C49 C48 N6 110.5(18) . . ? C49 C48 H48A 109.6 . . ? N6 C48 H48A 109.6 . . ? C49 C48 H48B 109.6 . . ? N6 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? C48 C49 C50 106.8(18) . . ? C48 C49 H49A 110.4 . . ? C50 C49 H49A 110.4 . . ? C48 C49 H49B 110.4 . . ? C50 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? C51 C50 C49 107.9(18) . . ? C51 C50 H50A 110.1 . . ? C49 C50 H50A 110.1 . . ? C51 C50 H50B 110.1 . . ? C49 C50 H50B 110.1 . . ? H50A C50 H50B 108.4 . . ? C50 C51 N7 110.2(16) . . ? C50 C51 H51A 109.6 . . ? N7 C51 H51A 109.6 . . ? C50 C51 H51B 109.6 . . ? N7 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? N8 C52 N7 111.8(10) . . ? N8 C52 H52 124.1 . . ? N7 C52 H52 124.1 . . ? C54 C53 N7 104.4(12) . . ? C54 C53 H53 127.8 . . ? N7 C53 H53 127.8 . . ? N8 C54 C53 112.1(12) . . ? N8 C54 H54 124.0 . . ? C53 C54 H54 124.0 . . ? C35 N1 C37 104.2(8) . . ? C35 N1 Cd1 124.8(6) . . ? C37 N1 Cd1 131.0(6) . . ? C36 N2 C35 107.3(8) . . ? C36 N2 C38 127.7(9) . . ? C35 N2 C38 125.0(9) . . ? C42 N3 C43 106.8(8) . . ? C42 N3 C41 127.2(8) . . ? C43 N3 C41 125.6(9) . . ? C42 N4 C44 102.3(8) . . ? C42 N4 Cd1 134.4(7) . 2_545 ? C44 N4 Cd1 123.0(6) . 2_545 ? C45 N5 C47 103.8(12) . . ? C45 N5 Cd2 133.5(11) . . ? C47 N5 Cd2 121.7(8) . . ? C45 N6 C46 104.2(13) . . ? C45 N6 C48 129.8(17) . . ? C46 N6 C48 123.7(16) . . ? C53 N7 C52 107.2(12) . . ? C53 N7 C51 125.4(12) . . ? C52 N7 C51 126.8(12) . . ? C52 N8 C54 104.3(10) . . ? C52 N8 Cd2 123.6(8) . 2_846 ? C54 N8 Cd2 131.4(9) . 2_846 ? C1 O1 Cd1 89.0(5) . 1_856 ? C1 O2 Cd1 92.9(6) . 1_856 ? C9 O3 C8 117.6(6) . . ? C12 O4 C15 118.9(6) . . ? C17 O5 Cd2 88.8(7) . . ? C17 O6 Cd2 99.1(8) . . ? C18 O7 Cd2 97.0(9) . . ? C18 O8 Cd2 93.0(8) . . ? C25 O9 C26 114.9(9) . . ? C29 O10 C32 118.2(7) . . ? C34 O11 Cd1 84.2(6) . . ? C34 O12 Cd1 100.3(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 178.2(9) . . . . ? O2 C1 C2 C7 -5.6(13) . . . . ? Cd1 C1 C2 C7 66(6) 1_856 . . . ? O1 C1 C2 C3 6.3(13) . . . . ? O2 C1 C2 C3 -177.6(8) . . . . ? Cd1 C1 C2 C3 -106(5) 1_856 . . . ? C7 C2 C3 C4 3.6(13) . . . . ? C1 C2 C3 C4 175.7(8) . . . . ? C2 C3 C4 C5 -3.8(14) . . . . ? C3 C4 C5 C6 3.5(15) . . . . ? C3 C4 C5 C8 -177.5(8) . . . . ? C4 C5 C6 C7 -3.0(16) . . . . ? C8 C5 C6 C7 178.0(8) . . . . ? C3 C2 C7 C6 -3.2(13) . . . . ? C1 C2 C7 C6 -175.3(8) . . . . ? C5 C6 C7 C2 3.0(15) . . . . ? C6 C5 C8 O3 76.9(12) . . . . ? C4 C5 C8 O3 -102.0(11) . . . . ? C14 C9 C10 C11 0.5(17) . . . . ? O3 C9 C10 C11 179.4(10) . . . . ? C9 C10 C11 C12 -0.4(18) . . . . ? C10 C11 C12 C13 0.7(16) . . . . ? C10 C11 C12 O4 176.8(10) . . . . ? O4 C12 C13 C14 -177.6(8) . . . . ? C11 C12 C13 C14 -1.2(14) . . . . ? C10 C9 C14 C13 -1.0(15) . . . . ? O3 C9 C14 C13 -179.8(9) . . . . ? C12 C13 C14 C9 1.3(14) . . . . ? O4 C15 C17 O6 49.5(13) . . . . ? C16 C15 C17 O6 -70.9(14) . . . . ? O4 C15 C17 O5 -131.5(10) . . . . ? C16 C15 C17 O5 108.1(12) . . . . ? O4 C15 C17 Cd2 29(6) . . . . ? C16 C15 C17 Cd2 -91(6) . . . . ? N8 Cd2 C17 O6 162.0(8) 2_856 . . . ? N5 Cd2 C17 O6 -91.3(8) . . . . ? O7 Cd2 C17 O6 3.9(11) . . . . ? O8 Cd2 C17 O6 54.1(9) . . . . ? O5 Cd2 C17 O6 176.5(12) . . . . ? C18 Cd2 C17 O6 33.7(10) . . . . ? N8 Cd2 C17 O5 -14.5(7) 2_856 . . . ? N5 Cd2 C17 O5 92.2(7) . . . . ? O6 Cd2 C17 O5 -176.5(12) . . . . ? O7 Cd2 C17 O5 -172.6(7) . . . . ? O8 Cd2 C17 O5 -122.4(7) . . . . ? C18 Cd2 C17 O5 -142.8(7) . . . . ? N8 Cd2 C17 C15 -177(6) 2_856 . . . ? N5 Cd2 C17 C15 -70(6) . . . . ? O6 Cd2 C17 C15 21(6) . . . . ? O7 Cd2 C17 C15 25(6) . . . . ? O8 Cd2 C17 C15 76(6) . . . . ? O5 Cd2 C17 C15 -162(6) . . . . ? C18 Cd2 C17 C15 55(6) . . . . ? N8 Cd2 C18 O8 -79.3(10) 2_856 . . . ? N5 Cd2 C18 O8 171.0(9) . . . . ? O6 Cd2 C18 O8 65.1(10) . . . . ? O7 Cd2 C18 O8 -175.9(16) . . . . ? O5 Cd2 C18 O8 23.2(13) . . . . ? C17 Cd2 C18 O8 50.8(11) . . . . ? N8 Cd2 C18 O7 96.5(10) 2_856 . . . ? N5 Cd2 C18 O7 -13.1(11) . . . . ? O6 Cd2 C18 O7 -119.0(10) . . . . ? O8 Cd2 C18 O7 175.9(16) . . . . ? O5 Cd2 C18 O7 -160.9(9) . . . . ? C17 Cd2 C18 O7 -133.3(10) . . . . ? N8 Cd2 C18 C19 157(4) 2_856 . . . ? N5 Cd2 C18 C19 47(4) . . . . ? O6 Cd2 C18 C19 -59(4) . . . . ? O7 Cd2 C18 C19 60(4) . . . . ? O8 Cd2 C18 C19 -124(4) . . . . ? O5 Cd2 C18 C19 -101(4) . . . . ? C17 Cd2 C18 C19 -73(4) . . . . ? O8 C18 C19 C20 170.5(14) . . . . ? O7 C18 C19 C20 -16.4(17) . . . . ? Cd2 C18 C19 C20 -71(4) . . . . ? O8 C18 C19 C24 -8.4(19) . . . . ? O7 C18 C19 C24 164.7(13) . . . . ? Cd2 C18 C19 C24 110(4) . . . . ? C24 C19 C20 C21 -3.5(18) . . . . ? C18 C19 C20 C21 177.5(10) . . . . ? C19 C20 C21 C22 -3.7(18) . . . . ? C20 C21 C22 C23 5.9(18) . . . . ? C20 C21 C22 C25 -168.9(10) . . . . ? C21 C22 C23 C24 -1(2) . . . . ? C25 C22 C23 C24 173.7(12) . . . . ? C20 C19 C24 C23 8.0(19) . . . . ? C18 C19 C24 C23 -173.1(11) . . . . ? C22 C23 C24 C19 -6(2) . . . . ? C21 C22 C25 O9 -132.3(10) . . . . ? C23 C22 C25 O9 53.0(15) . . . . ? C31 C26 C27 C28 0.3(18) . . . . ? O9 C26 C27 C28 -178.9(9) . . . . ? C26 C27 C28 C29 1.0(16) . . . . ? C27 C28 C29 C30 -2.1(16) . . . . ? C27 C28 C29 O10 -179.0(10) . . . . ? C28 C29 C30 C31 1.8(17) . . . . ? O10 C29 C30 C31 179.1(9) . . . . ? C27 C26 C31 C30 -0.5(18) . . . . ? O9 C26 C31 C30 178.6(10) . . . . ? C29 C30 C31 C26 -0.6(17) . . . . ? O10 C32 C34 O11 9.9(13) . . . . ? C33 C32 C34 O11 -109.8(11) . . . . ? O10 C32 C34 O12 -166.8(8) . . . . ? C33 C32 C34 O12 73.4(12) . . . . ? N2 C36 C37 N1 -0.8(12) . . . . ? N2 C38 C39 C40 -173.7(10) . . . . ? C38 C39 C40 C41 175.1(11) . . . . ? C39 C40 C41 N3 -169.5(10) . . . . ? N3 C43 C44 N4 -0.3(10) . . . . ? N6 C46 C47 N5 -6(2) . . . . ? N6 C48 C49 C50 164.8(15) . . . . ? C48 C49 C50 C51 -164(2) . . . . ? C49 C50 C51 N7 171.7(12) . . . . ? N7 C53 C54 N8 5(2) . . . . ? N2 C35 N1 C37 1.0(11) . . . . ? N2 C35 N1 Cd1 -178.7(6) . . . . ? C36 C37 N1 C35 -0.1(11) . . . . ? C36 C37 N1 Cd1 179.5(7) . . . . ? N4 Cd1 N1 C35 32.5(8) 2 . . . ? O12 Cd1 N1 C35 -95.0(8) . . . . ? O2 Cd1 N1 C35 136.4(7) 1_254 . . . ? O1 Cd1 N1 C35 174.7(7) 1_254 . . . ? O11 Cd1 N1 C35 -58.1(7) . . . . ? C1 Cd1 N1 C35 162.0(7) 1_254 . . . ? N4 Cd1 N1 C37 -147.1(8) 2 . . . ? O12 Cd1 N1 C37 85.4(8) . . . . ? O2 Cd1 N1 C37 -43.1(10) 1_254 . . . ? O1 Cd1 N1 C37 -4.9(8) 1_254 . . . ? O11 Cd1 N1 C37 122.3(8) . . . . ? C1 Cd1 N1 C37 -17.6(9) 1_254 . . . ? C37 C36 N2 C35 1.3(12) . . . . ? C37 C36 N2 C38 179.6(10) . . . . ? N1 C35 N2 C36 -1.5(11) . . . . ? N1 C35 N2 C38 -179.8(9) . . . . ? C39 C38 N2 C36 -120.7(12) . . . . ? C39 C38 N2 C35 57.3(16) . . . . ? N4 C42 N3 C43 -0.2(10) . . . . ? N4 C42 N3 C41 -173.5(7) . . . . ? C44 C43 N3 C42 0.3(10) . . . . ? C44 C43 N3 C41 173.8(8) . . . . ? C40 C41 N3 C42 -121.6(11) . . . . ? C40 C41 N3 C43 66.1(13) . . . . ? N3 C42 N4 C44 0.0(9) . . . . ? N3 C42 N4 Cd1 173.2(6) . . . 2_545 ? C43 C44 N4 C42 0.2(9) . . . . ? C43 C44 N4 Cd1 -174.0(6) . . . 2_545 ? N6 C45 N5 C47 -6(2) . . . . ? N6 C45 N5 Cd2 -174.2(11) . . . . ? C46 C47 N5 C45 7.5(19) . . . . ? C46 C47 N5 Cd2 177.4(10) . . . . ? N8 Cd2 N5 C45 60.5(15) 2_856 . . . ? O6 Cd2 N5 C45 -79.1(15) . . . . ? O7 Cd2 N5 C45 166.9(15) . . . . ? O8 Cd2 N5 C45 178.2(14) . . . . ? O5 Cd2 N5 C45 -25.9(15) . . . . ? C18 Cd2 N5 C45 172.6(14) . . . . ? C17 Cd2 N5 C45 -53.0(15) . . . . ? N8 Cd2 N5 C47 -105.9(11) 2_856 . . . ? O6 Cd2 N5 C47 114.5(11) . . . . ? O7 Cd2 N5 C47 0.5(11) . . . . ? O8 Cd2 N5 C47 11.8(13) . . . . ? O5 Cd2 N5 C47 167.7(10) . . . . ? C18 Cd2 N5 C47 6.2(11) . . . . ? C17 Cd2 N5 C47 140.6(11) . . . . ? N5 C45 N6 C46 3(2) . . . . ? N5 C45 N6 C48 165.5(17) . . . . ? C47 C46 N6 C45 2(2) . . . . ? C47 C46 N6 C48 -162.0(15) . . . . ? C49 C48 N6 C45 128(2) . . . . ? C49 C48 N6 C46 -72(3) . . . . ? C54 C53 N7 C52 -4(2) . . . . ? C54 C53 N7 C51 168.5(16) . . . . ? N8 C52 N7 C53 2(2) . . . . ? N8 C52 N7 C51 -170.4(16) . . . . ? C50 C51 N7 C53 116(2) . . . . ? C50 C51 N7 C52 -72(2) . . . . ? N7 C52 N8 C54 0.9(16) . . . . ? N7 C52 N8 Cd2 171.8(10) . . . 2_846 ? C53 C54 N8 C52 -3.6(17) . . . . ? C53 C54 N8 Cd2 -173.5(12) . . . 2_846 ? O2 C1 O1 Cd1 13.1(9) . . . 1_856 ? C2 C1 O1 Cd1 -170.8(7) . . . 1_856 ? O1 C1 O2 Cd1 -13.7(10) . . . 1_856 ? C2 C1 O2 Cd1 170.2(7) . . . 1_856 ? C10 C9 O3 C8 169.5(10) . . . . ? C14 C9 O3 C8 -11.8(14) . . . . ? C5 C8 O3 C9 -177.6(9) . . . . ? C13 C12 O4 C15 -172.2(8) . . . . ? C11 C12 O4 C15 11.5(14) . . . . ? C17 C15 O4 C12 63.9(11) . . . . ? C16 C15 O4 C12 -172.0(9) . . . . ? O6 C17 O5 Cd2 -3.3(12) . . . . ? C15 C17 O5 Cd2 177.7(8) . . . . ? N8 Cd2 O5 C17 166.3(7) 2_856 . . . ? N5 Cd2 O5 C17 -92.5(7) . . . . ? O6 Cd2 O5 C17 1.9(7) . . . . ? O7 Cd2 O5 C17 20.2(19) . . . . ? O8 Cd2 O5 C17 68.3(8) . . . . ? C18 Cd2 O5 C17 57.1(9) . . . . ? O5 C17 O6 Cd2 3.7(13) . . . . ? C15 C17 O6 Cd2 -177.3(7) . . . . ? N8 Cd2 O6 C17 -24.0(10) 2_856 . . . ? N5 Cd2 O6 C17 93.2(8) . . . . ? O7 Cd2 O6 C17 -177.3(8) . . . . ? O8 Cd2 O6 C17 -129.5(8) . . . . ? O5 Cd2 O6 C17 -2.0(7) . . . . ? C18 Cd2 O6 C17 -152.4(8) . . . . ? O8 C18 O7 Cd2 4.1(16) . . . . ? C19 C18 O7 Cd2 -169.4(8) . . . . ? N8 Cd2 O7 C18 -91.2(10) 2_856 . . . ? N5 Cd2 O7 C18 167.7(10) . . . . ? O6 Cd2 O7 C18 69.2(11) . . . . ? O8 Cd2 O7 C18 -2.3(9) . . . . ? O5 Cd2 O7 C18 53(2) . . . . ? C17 Cd2 O7 C18 67.4(12) . . . . ? O7 C18 O8 Cd2 -3.9(15) . . . . ? C19 C18 O8 Cd2 169.1(10) . . . . ? N8 Cd2 O8 C18 106.3(10) 2_856 . . . ? N5 Cd2 O8 C18 -12.2(12) . . . . ? O6 Cd2 O8 C18 -117.9(10) . . . . ? O7 Cd2 O8 C18 2.3(9) . . . . ? O5 Cd2 O8 C18 -164.5(8) . . . . ? C17 Cd2 O8 C18 -138.5(9) . . . . ? C22 C25 O9 C26 -173.7(9) . . . . ? C31 C26 O9 C25 5.3(17) . . . . ? C27 C26 O9 C25 -175.6(10) . . . . ? C28 C29 O10 C32 -6.8(15) . . . . ? C30 C29 O10 C32 176.2(9) . . . . ? C33 C32 O10 C29 -166.0(8) . . . . ? C34 C32 O10 C29 71.9(11) . . . . ? O12 C34 O11 Cd1 13.1(10) . . . . ? C32 C34 O11 Cd1 -163.4(9) . . . . ? N1 Cd1 O11 C34 -150.9(6) . . . . ? N4 Cd1 O11 C34 101.4(6) 2 . . . ? O12 Cd1 O11 C34 -7.9(6) . . . . ? O2 Cd1 O11 C34 14.4(7) 1_254 . . . ? O1 Cd1 O11 C34 -60.6(6) 1_254 . . . ? C1 Cd1 O11 C34 -25.3(8) 1_254 . . . ? O11 C34 O12 Cd1 -15.5(11) . . . . ? C32 C34 O12 Cd1 161.3(7) . . . . ? N1 Cd1 O12 C34 57.4(7) . . . . ? N4 Cd1 O12 C34 -70.9(7) 2 . . . ? O2 Cd1 O12 C34 -156.8(6) 1_254 . . . ? O1 Cd1 O12 C34 148.3(7) 1_254 . . . ? O11 Cd1 O12 C34 7.6(6) . . . . ? C1 Cd1 O12 C34 175.2(7) 1_254 . . . ? 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 C38 H38B O1 0.97 2.59 3.388(17) 139.5 1_354 C46 H46 O5 0.93 2.30 3.209(18) 166.5 2_746 C48 H48B O6 0.97 2.38 3.14(3) 134.4 1_655 C51 H51A O8 0.97 2.55 3.23(2) 126.9 2_746 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.572 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.075 #=========================END data_Compound-7 _database_code_depnum_ccdc_archive 'CCDC 877937' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H56 N8 O12 Zn2' _chemical_formula_sum 'C54 H56 N8 O12 Zn2' _chemical_formula_weight 1139.81 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.5495(5) _cell_length_b 16.5696(13) _cell_length_c 23.432(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.632(8) _cell_angle_gamma 90.00 _cell_volume 2541.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1468 _cell_measurement_theta_min 2.8783 _cell_measurement_theta_max 29.2220 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9701 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10074 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.1304 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7420 _reflns_number_gt 4718 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0423P)^2^+0.4120P] 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' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 7420 _refine_ls_number_parameters 685 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.100 _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 Zn1 Zn 0.7644(2) 0.56030(6) 0.57202(6) 0.0393(4) Uani 1 1 d . . . Zn2 Zn -0.7296(2) 0.19554(6) 0.07373(6) 0.0391(4) Uani 1 1 d . . . C1 C -1.938(2) 0.5082(8) -0.3515(6) 0.045(3) Uani 1 1 d . . . C2 C -1.8025(17) 0.4439(7) -0.3231(5) 0.036(3) Uani 1 1 d . . . C3 C -1.617(2) 0.4663(9) -0.3006(6) 0.060(4) Uani 1 1 d . . . H3 H -1.5796 0.5205 -0.3007 0.072 Uiso 1 1 calc R . . C4 C -1.481(2) 0.4094(9) -0.2774(6) 0.070(4) Uani 1 1 d . . . H4 H -1.3541 0.4249 -0.2622 0.084 Uiso 1 1 calc R . . C5 C -1.5414(19) 0.3281(7) -0.2775(5) 0.056(3) Uani 1 1 d . . . C6 C -1.729(2) 0.3091(7) -0.2967(6) 0.074(4) Uani 1 1 d . . . H6 H -1.7744 0.2563 -0.2930 0.089 Uiso 1 1 calc R . . C7 C -1.858(2) 0.3662(8) -0.3222(6) 0.071(4) Uani 1 1 d . . . H7 H -1.9822 0.3504 -0.3386 0.085 Uiso 1 1 calc R . . C8 C -1.394(2) 0.2632(8) -0.2569(6) 0.083(5) Uani 1 1 d . . . H8A H -1.4701 0.2162 -0.2452 0.099 Uiso 1 1 calc R . . H8B H -1.3080 0.2474 -0.2881 0.099 Uiso 1 1 calc R . . C9 C -1.110(2) 0.2423(9) -0.1947(6) 0.066(4) Uani 1 1 d . . . C10 C -1.001(2) 0.2659(8) -0.1478(6) 0.068(4) Uani 1 1 d . . . H10 H -1.0397 0.3132 -0.1297 0.081 Uiso 1 1 calc R . . C11 C -0.8344(19) 0.2232(6) -0.1252(6) 0.051(3) Uani 1 1 d . . . H11 H -0.7586 0.2427 -0.0940 0.061 Uiso 1 1 calc R . . C12 C -0.785(2) 0.1497(7) -0.1510(5) 0.050(3) Uani 1 1 d . . . C13 C -0.9012(19) 0.1255(7) -0.1969(5) 0.063(4) Uani 1 1 d . . . H13 H -0.8664 0.0775 -0.2147 0.076 Uiso 1 1 calc R . . C14 C -1.066(2) 0.1671(7) -0.2183(6) 0.077(5) Uani 1 1 d . . . H14 H -1.1468 0.1459 -0.2480 0.093 Uiso 1 1 calc R . . C15 C -0.5112(19) 0.1220(8) -0.0837(5) 0.047(3) Uani 1 1 d . . . H15 H -0.4596 0.1769 -0.0893 0.056 Uiso 1 1 calc R . . C16 C -0.334(2) 0.0633(11) -0.0798(5) 0.075(5) Uani 1 1 d . . . H16A H -0.2562 0.0671 -0.1137 0.112 Uiso 1 1 calc R . . H16B H -0.3860 0.0094 -0.0761 0.112 Uiso 1 1 calc R . . H16C H -0.2489 0.0762 -0.0471 0.112 Uiso 1 1 calc R . . C17 C -0.631(2) 0.1182(7) -0.0295(6) 0.040(3) Uani 1 1 d . . . C18 C -0.428(3) 0.2452(12) 0.1438(9) 0.081(2) Uani 1 1 d U . . C19 C -0.2472(17) 0.2933(7) 0.1653(5) 0.034(3) Uani 1 1 d . . . C20 C -0.2112(17) 0.3699(7) 0.1471(5) 0.048(3) Uani 1 1 d . . . H20 H -0.3043 0.3949 0.1221 0.058 Uiso 1 1 calc R . . C21 C -0.036(2) 0.4114(8) 0.1655(5) 0.059(4) Uani 1 1 d . . . H21 H -0.0128 0.4630 0.1516 0.071 Uiso 1 1 calc R . . C22 C 0.098(2) 0.3787(10) 0.2025(6) 0.061(4) Uani 1 1 d . . . C23 C 0.069(2) 0.2989(10) 0.2204(6) 0.074(4) Uani 1 1 d . . . H23 H 0.1655 0.2738 0.2442 0.089 Uiso 1 1 calc R . . C24 C -0.106(2) 0.2579(9) 0.2023(6) 0.060(4) Uani 1 1 d . . . H24 H -0.1276 0.2056 0.2152 0.072 Uiso 1 1 calc R . . C25 C 0.299(2) 0.4183(10) 0.2206(6) 0.087(5) Uani 1 1 d . . . H25A H 0.4116 0.3817 0.2143 0.104 Uiso 1 1 calc R . . H25B H 0.3199 0.4668 0.1984 0.104 Uiso 1 1 calc R . . C26 C 0.4609(17) 0.4738(7) 0.3014(5) 0.040(3) Uani 1 1 d . . . C27 C 0.4183(18) 0.5377(8) 0.3375(6) 0.064(4) Uani 1 1 d . . . H27 H 0.2841 0.5542 0.3422 0.077 Uiso 1 1 calc R . . C28 C 0.5801(16) 0.5774(8) 0.3670(5) 0.050(3) Uani 1 1 d . . . H28 H 0.5513 0.6177 0.3932 0.060 Uiso 1 1 calc R . . C29 C 0.7810(14) 0.5570(7) 0.3574(4) 0.035(2) Uani 1 1 d . . . C30 C 0.8163(17) 0.4959(6) 0.3186(4) 0.039(3) Uani 1 1 d . . . H30 H 0.9500 0.4815 0.3110 0.047 Uiso 1 1 calc R . . C31 C 0.6591(16) 0.4564(7) 0.2914(5) 0.047(3) Uani 1 1 d . . . H31 H 0.6886 0.4162 0.2651 0.056 Uiso 1 1 calc R . . C32 C 0.9151(18) 0.6636(7) 0.4168(5) 0.044(3) Uani 1 1 d . . . H32 H 0.8225 0.7000 0.3956 0.052 Uiso 1 1 calc R . . C33 C 1.123(2) 0.7036(8) 0.4234(6) 0.060(4) Uani 1 1 d . . . H33A H 1.1743 0.7156 0.3863 0.090 Uiso 1 1 calc R . . H33B H 1.2162 0.6677 0.4431 0.090 Uiso 1 1 calc R . . H33C H 1.1110 0.7526 0.4448 0.090 Uiso 1 1 calc R . . C34 C 0.8212(19) 0.6424(8) 0.4736(5) 0.034(3) Uani 1 1 d . . . C35 C 0.443(2) 0.6757(8) 0.5999(6) 0.054(4) Uani 1 1 d . . . H35 H 0.3838 0.6663 0.5639 0.064 Uiso 1 1 calc R . . C36 C 0.482(2) 0.7163(10) 0.6853(7) 0.071(5) Uani 1 1 d . . . H36 H 0.4619 0.7393 0.7209 0.086 Uiso 1 1 calc R . . C37 C 0.640(2) 0.6701(8) 0.6696(6) 0.045(4) Uani 1 1 d . . . H37 H 0.7537 0.6577 0.6927 0.054 Uiso 1 1 calc R . . C38 C 0.159(2) 0.7606(9) 0.6316(6) 0.059(4) Uani 1 1 d . . . H38A H 0.1306 0.7886 0.6669 0.071 Uiso 1 1 calc R . . H38B H 0.0550 0.7192 0.6261 0.071 Uiso 1 1 calc R . . C39 C 0.142(2) 0.8200(7) 0.5825(6) 0.049(4) Uani 1 1 d . . . H39A H 0.2240 0.8674 0.5915 0.059 Uiso 1 1 calc R . . H39B H 0.1943 0.7955 0.5483 0.059 Uiso 1 1 calc R . . C40 C -0.078(2) 0.8446(9) 0.5720(6) 0.051(4) Uani 1 1 d . . . H40A H -0.1328 0.8673 0.6065 0.062 Uiso 1 1 calc R . . H40B H -0.1593 0.7981 0.5609 0.062 Uiso 1 1 calc R . . C41 C -0.083(2) 0.9096(8) 0.5227(7) 0.067(5) Uani 1 1 d . . . H41A H -0.0348 0.9610 0.5377 0.080 Uiso 1 1 calc R . . H41B H 0.0087 0.8931 0.4930 0.080 Uiso 1 1 calc R . . C42 C -0.400(2) 0.8631(8) 0.4708(6) 0.063(4) Uani 1 1 d . . . H42 H -0.3685 0.8084 0.4682 0.075 Uiso 1 1 calc R . . C43 C -0.559(2) 0.8980(8) 0.4482(6) 0.056(4) Uani 1 1 d . . . H43 H -0.6617 0.8722 0.4270 0.067 Uiso 1 1 calc R . . C44 C -0.385(2) 0.9910(8) 0.4898(7) 0.060(4) Uani 1 1 d . . . H44 H -0.3353 1.0401 0.5036 0.071 Uiso 1 1 calc R . . C45 C -1.068(2) 0.0847(9) 0.0985(7) 0.062(4) Uani 1 1 d . . . H45 H -1.1317 0.0978 0.0638 0.074 Uiso 1 1 calc R . . C46 C -1.006(3) 0.0317(10) 0.1805(7) 0.074(5) Uani 1 1 d . . . H46 H -1.0150 0.0004 0.2132 0.088 Uiso 1 1 calc R . . C47 C -0.854(3) 0.0806(11) 0.1684(7) 0.080(6) Uani 1 1 d . . . H47 H -0.7415 0.0911 0.1922 0.096 Uiso 1 1 calc R . . C48 C -1.348(3) -0.0044(11) 0.1324(8) 0.083(6) Uani 1 1 d U . . H48A H -1.3711 -0.0329 0.1679 0.100 Uiso 1 1 calc R . . H48B H -1.4514 0.0375 0.1290 0.100 Uiso 1 1 calc R . . C49 C -1.379(2) -0.0568(12) 0.0889(9) 0.104(7) Uani 1 1 d . . . H49A H -1.2905 -0.1029 0.0963 0.125 Uiso 1 1 calc R . . H49B H -1.3304 -0.0310 0.0547 0.125 Uiso 1 1 calc R . . C50 C -1.593(2) -0.0896(9) 0.0748(7) 0.069(5) Uani 1 1 d . . . H50A H -1.6349 -0.1240 0.1059 0.083 Uiso 1 1 calc R . . H50B H -1.6881 -0.0447 0.0722 0.083 Uiso 1 1 calc R . . C51 C -1.607(2) -0.1357(10) 0.0214(7) 0.073(5) Uani 1 1 d . . . H51A H -1.5405 -0.1050 -0.0081 0.088 Uiso 1 1 calc R . . H51B H -1.5309 -0.1856 0.0267 0.088 Uiso 1 1 calc R . . C52 C -1.9576(19) -0.1015(8) -0.0139(6) 0.050(4) Uani 1 1 d . . . H52 H -1.9514 -0.0458 -0.0093 0.060 Uiso 1 1 calc R . . C53 C -2.1142(19) -0.1450(8) -0.0375(7) 0.056(4) Uani 1 1 d . . . H53 H -2.2338 -0.1225 -0.0528 0.068 Uiso 1 1 calc R . . C54 C -1.887(2) -0.2255(9) -0.0141(6) 0.051(4) Uani 1 1 d . . . H54 H -1.8152 -0.2736 -0.0101 0.061 Uiso 1 1 calc R . . N1 N 0.6099(17) 0.6444(6) 0.6156(5) 0.047(3) Uani 1 1 d . . . N2 N 0.3578(17) 0.7221(7) 0.6372(5) 0.054(3) Uani 1 1 d . . . N3 N -0.2879(15) 0.9191(6) 0.4985(5) 0.043(3) Uani 1 1 d . . . N4 N -0.5517(16) 0.9835(6) 0.4607(5) 0.045(3) Uani 1 1 d . . . N5 N -0.8874(15) 0.1131(6) 0.1159(4) 0.037(3) Uani 1 1 d . . . N6 N -1.1460(18) 0.0350(6) 0.1371(5) 0.052(3) Uani 1 1 d . . . N7 N -1.8145(19) -0.1554(7) 0.0014(5) 0.059(4) Uani 1 1 d . . . N8 N -2.0769(16) -0.2203(6) -0.0362(5) 0.042(3) Uani 1 1 d . . . O1 O -1.9175(17) 0.5801(6) -0.3385(6) 0.106(4) Uani 1 1 d . . . O2 O -2.0686(14) 0.4810(6) -0.3877(4) 0.055(2) Uani 1 1 d . . . O3 O -1.2720(18) 0.2895(6) -0.2117(4) 0.087(4) Uani 1 1 d . . . O4 O -0.6340(13) 0.0986(5) -0.1318(3) 0.059(2) Uani 1 1 d . . . O5 O -0.5513(13) 0.1601(6) 0.0119(4) 0.055(3) Uani 1 1 d . . . O6 O -0.7949(14) 0.0864(6) -0.0269(4) 0.060(3) Uani 1 1 d . . . O7 O -0.5480(17) 0.2804(7) 0.1080(5) 0.081(2) Uani 1 1 d U . . O8 O -0.4583(16) 0.1775(7) 0.1608(5) 0.082(2) Uani 1 1 d U . . O9 O 0.2893(13) 0.4368(6) 0.2765(4) 0.065(3) Uani 1 1 d . . . O10 O 0.9498(10) 0.5918(4) 0.3823(3) 0.0449(19) Uani 1 1 d . . . O11 O 0.6498(13) 0.6659(5) 0.4849(4) 0.051(2) Uani 1 1 d . . . O12 O 0.9332(14) 0.5967(6) 0.5064(4) 0.055(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0399(9) 0.0363(8) 0.0412(9) -0.0010(7) -0.0066(8) 0.0040(7) Zn2 0.0321(8) 0.0419(9) 0.0429(10) -0.0004(7) -0.0043(8) -0.0053(7) C1 0.031(7) 0.052(8) 0.051(8) 0.004(6) -0.001(6) 0.004(5) C2 0.028(6) 0.037(7) 0.044(7) 0.015(6) 0.004(6) 0.002(5) C3 0.060(10) 0.061(9) 0.059(9) 0.003(7) -0.007(8) -0.002(7) C4 0.049(9) 0.079(11) 0.080(11) 0.004(9) -0.033(8) 0.002(8) C5 0.050(8) 0.058(8) 0.060(9) -0.010(7) -0.017(7) 0.009(6) C6 0.097(12) 0.038(7) 0.086(10) 0.006(7) -0.042(9) 0.001(7) C7 0.063(9) 0.066(9) 0.083(10) -0.009(8) -0.032(8) 0.011(7) C8 0.109(13) 0.066(9) 0.071(10) 0.007(7) -0.045(9) 0.032(8) C9 0.073(11) 0.060(9) 0.062(10) -0.009(8) -0.032(9) 0.011(8) C10 0.068(10) 0.058(8) 0.076(10) -0.018(8) -0.006(8) 0.030(7) C11 0.042(8) 0.041(7) 0.067(9) -0.008(6) -0.027(7) 0.004(6) C12 0.057(9) 0.058(8) 0.034(7) -0.011(6) -0.012(6) 0.004(7) C13 0.074(10) 0.056(8) 0.059(8) -0.005(7) -0.015(8) 0.020(7) C14 0.106(12) 0.047(7) 0.076(10) -0.013(7) -0.046(9) 0.033(7) C15 0.053(9) 0.063(8) 0.025(6) -0.004(6) 0.005(6) 0.018(7) C16 0.071(10) 0.114(13) 0.039(8) -0.024(9) -0.021(7) 0.049(10) C17 0.040(8) 0.021(6) 0.057(9) 0.007(6) -0.014(7) -0.005(5) C18 0.058(4) 0.084(6) 0.102(6) -0.010(5) -0.013(4) -0.008(4) C19 0.028(7) 0.041(7) 0.033(6) -0.015(5) 0.004(5) 0.001(5) C20 0.030(7) 0.075(9) 0.039(7) -0.008(6) 0.004(6) -0.011(6) C21 0.062(9) 0.063(8) 0.053(8) -0.013(7) 0.026(8) -0.029(7) C22 0.043(9) 0.085(11) 0.054(9) -0.028(8) -0.003(7) -0.019(7) C23 0.053(9) 0.108(12) 0.060(9) -0.004(9) -0.024(8) 0.001(9) C24 0.041(8) 0.080(10) 0.059(9) 0.000(7) -0.022(7) 0.005(7) C25 0.044(8) 0.165(16) 0.051(9) -0.021(9) 0.000(7) -0.046(9) C26 0.026(6) 0.056(8) 0.038(7) -0.010(6) -0.001(5) -0.001(5) C27 0.018(6) 0.100(12) 0.075(10) -0.019(9) 0.002(7) -0.004(6) C28 0.029(6) 0.069(9) 0.052(7) -0.038(7) 0.005(6) 0.008(6) C29 0.023(6) 0.047(6) 0.034(6) 0.009(6) 0.001(5) -0.009(6) C30 0.047(7) 0.047(6) 0.024(6) -0.003(5) 0.003(5) -0.007(5) C31 0.039(7) 0.053(7) 0.048(7) -0.008(6) 0.009(6) -0.015(5) C32 0.046(8) 0.039(7) 0.045(7) -0.005(6) -0.010(6) -0.003(6) C33 0.068(9) 0.038(7) 0.074(10) -0.017(7) 0.009(8) -0.023(7) C34 0.028(7) 0.043(8) 0.032(7) -0.001(6) 0.011(6) -0.012(6) C35 0.056(9) 0.057(9) 0.046(9) -0.015(7) -0.016(7) 0.038(8) C36 0.031(8) 0.128(15) 0.055(10) -0.020(9) -0.003(8) 0.045(9) C37 0.032(7) 0.060(10) 0.044(9) -0.005(7) 0.003(7) 0.000(7) C38 0.053(9) 0.059(8) 0.064(10) 0.010(7) -0.015(8) 0.024(7) C39 0.040(8) 0.040(7) 0.067(9) -0.005(7) 0.000(7) -0.002(6) C40 0.030(7) 0.068(10) 0.057(10) 0.003(8) 0.009(7) -0.003(7) C41 0.047(9) 0.037(7) 0.113(13) 0.006(8) -0.032(9) -0.002(6) C42 0.065(10) 0.040(8) 0.082(11) 0.005(7) -0.011(9) 0.016(7) C43 0.065(10) 0.042(7) 0.060(8) -0.013(6) -0.021(8) 0.001(7) C44 0.068(10) 0.031(7) 0.078(11) 0.004(7) -0.036(9) 0.007(7) C45 0.046(9) 0.081(12) 0.058(10) 0.011(9) -0.008(8) -0.001(8) C46 0.082(13) 0.083(12) 0.056(10) 0.021(9) -0.019(10) 0.006(10) C47 0.082(12) 0.098(15) 0.060(11) 0.032(10) -0.014(10) -0.045(11) C48 0.071(9) 0.096(9) 0.084(9) -0.001(8) 0.018(8) -0.030(8) C49 0.039(10) 0.139(16) 0.133(17) -0.056(14) -0.035(11) -0.012(10) C50 0.057(10) 0.055(10) 0.095(13) -0.008(9) -0.007(10) -0.029(8) C51 0.045(9) 0.071(10) 0.103(13) -0.040(10) -0.002(9) -0.006(8) C52 0.035(7) 0.039(7) 0.077(10) 0.008(7) 0.001(7) 0.011(6) C53 0.027(7) 0.044(8) 0.097(12) 0.011(8) -0.007(7) -0.001(6) C54 0.031(8) 0.059(10) 0.062(10) -0.016(8) -0.002(7) 0.013(7) N1 0.044(7) 0.046(7) 0.052(8) 0.000(6) -0.003(6) 0.017(6) N2 0.038(7) 0.074(10) 0.050(8) -0.004(7) 0.016(6) 0.018(6) N3 0.020(5) 0.031(6) 0.078(8) 0.000(6) -0.017(6) 0.008(4) N4 0.028(6) 0.038(6) 0.068(8) -0.003(6) -0.008(6) -0.003(5) N5 0.032(6) 0.042(7) 0.038(7) -0.002(5) 0.004(6) -0.005(5) N6 0.045(8) 0.051(8) 0.060(9) -0.001(7) 0.003(7) -0.026(6) N7 0.059(8) 0.060(8) 0.058(8) -0.022(7) -0.007(7) -0.002(7) N8 0.034(6) 0.039(7) 0.051(7) 0.004(6) -0.019(6) -0.004(5) O1 0.081(8) 0.041(6) 0.192(13) -0.001(7) -0.044(8) 0.008(5) O2 0.055(6) 0.070(6) 0.037(5) 0.001(4) -0.028(4) 0.015(5) O3 0.114(9) 0.072(6) 0.073(7) -0.007(5) -0.043(7) 0.046(6) O4 0.073(6) 0.053(5) 0.050(5) -0.016(4) -0.029(5) 0.038(4) O5 0.036(5) 0.064(6) 0.064(7) -0.023(5) -0.003(5) 0.001(5) O6 0.045(6) 0.079(7) 0.058(6) 0.000(5) 0.011(5) -0.028(5) O7 0.057(4) 0.084(6) 0.101(6) -0.010(5) -0.014(4) -0.008(4) O8 0.058(4) 0.084(6) 0.102(6) -0.010(5) -0.013(4) -0.008(4) O9 0.029(5) 0.106(8) 0.061(6) -0.028(5) -0.005(5) -0.025(5) O10 0.025(4) 0.060(5) 0.050(5) -0.018(4) -0.003(4) -0.005(3) O11 0.044(5) 0.073(6) 0.039(5) -0.001(4) 0.023(4) 0.012(4) O12 0.054(6) 0.063(6) 0.049(6) -0.003(5) 0.005(5) 0.009(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zn1 O2 1.938(9) 1_856 ? Zn1 O12 2.011(9) . ? Zn1 N1 2.016(11) . ? Zn1 N4 2.021(11) 2_546 ? Zn2 O5 1.975(9) . ? Zn2 N5 1.992(10) . ? Zn2 O7 1.996(11) . ? Zn2 N8 2.064(10) 2_255 ? C1 O1 1.235(16) . ? C1 O2 1.271(15) . ? C1 C2 1.527(16) . ? C2 C7 1.336(16) . ? C2 C3 1.365(17) . ? C3 C4 1.395(18) . ? C3 H3 0.9300 . ? C4 C5 1.405(18) . ? C4 H4 0.9300 . ? C5 C6 1.332(16) . ? C5 C8 1.516(15) . ? C6 C7 1.392(16) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.377(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.350(17) . ? C9 O3 1.366(16) . ? C9 C14 1.399(17) . ? C10 C11 1.395(16) . ? C10 H10 0.9300 . ? C11 C12 1.401(15) . ? C11 H11 0.9300 . ? C12 C13 1.360(16) . ? C12 O4 1.367(13) . ? C13 C14 1.364(15) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.418(13) . ? C15 C17 1.511(18) . ? C15 C16 1.513(17) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.202(14) . ? C17 O5 1.291(14) . ? C18 O8 1.21(2) . ? C18 O7 1.28(2) . ? C18 C19 1.50(2) . ? C19 C20 1.363(15) . ? C19 C24 1.381(16) . ? C20 C21 1.393(15) . ? C20 H20 0.9300 . ? C21 C22 1.334(18) . ? C21 H21 0.9300 . ? C22 C23 1.402(19) . ? C22 C25 1.518(16) . ? C23 C24 1.386(18) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 O9 1.349(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C31 1.357(14) . ? C26 C27 1.388(16) . ? C26 O9 1.394(13) . ? C27 C28 1.412(15) . ? C27 H27 0.9300 . ? C28 C29 1.384(13) . ? C28 H28 0.9300 . ? C29 O10 1.363(11) . ? C29 C30 1.384(14) . ? C30 C31 1.363(14) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 O10 1.460(12) . ? C32 C33 1.520(16) . ? C32 C34 1.523(17) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O11 1.224(14) . ? C34 O12 1.294(14) . ? C35 N1 1.256(15) . ? C35 N2 1.301(15) . ? C35 H35 0.9300 . ? C36 C37 1.347(18) . ? C36 N2 1.377(17) . ? C36 H36 0.9300 . ? C37 N1 1.344(15) . ? C37 H37 0.9300 . ? C38 N2 1.455(17) . ? C38 C39 1.515(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.509(17) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.580(18) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N3 1.453(16) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.291(18) . ? C42 N3 1.338(17) . ? C42 H42 0.9300 . ? C43 N4 1.446(16) . ? C43 H43 0.9300 . ? C44 N4 1.278(16) . ? C44 N3 1.363(15) . ? C44 H44 0.9300 . ? C45 N5 1.324(16) . ? C45 N6 1.337(17) . ? C45 H45 0.9300 . ? C46 C47 1.32(2) . ? C46 N6 1.350(18) . ? C46 H46 0.9300 . ? C47 N5 1.355(17) . ? C47 H47 0.9300 . ? C48 C49 1.35(2) . ? C48 N6 1.479(19) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.534(19) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.466(19) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 N7 1.465(17) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 N7 1.336(16) . ? C52 C53 1.359(18) . ? C52 H52 0.9300 . ? C53 N8 1.271(16) . ? C53 H53 0.9300 . ? C54 N7 1.302(17) . ? C54 N8 1.336(15) . ? C54 H54 0.9300 . ? N4 Zn1 2.021(11) 2_556 ? N8 Zn2 2.064(10) 2_245 ? O2 Zn1 1.938(9) 1_254 ? 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 Zn1 O12 105.1(4) 1_856 . ? O2 Zn1 N1 120.4(4) 1_856 . ? O12 Zn1 N1 118.3(4) . . ? O2 Zn1 N4 97.5(4) 1_856 2_546 ? O12 Zn1 N4 106.7(4) . 2_546 ? N1 Zn1 N4 106.1(4) . 2_546 ? O5 Zn2 N5 119.1(4) . . ? O5 Zn2 O7 98.4(4) . . ? N5 Zn2 O7 126.5(5) . . ? O5 Zn2 N8 104.9(4) . 2_255 ? N5 Zn2 N8 110.7(4) . 2_255 ? O7 Zn2 N8 92.7(5) . 2_255 ? O1 C1 O2 124.9(13) . . ? O1 C1 C2 120.6(13) . . ? O2 C1 C2 114.6(11) . . ? C7 C2 C3 119.6(11) . . ? C7 C2 C1 121.6(11) . . ? C3 C2 C1 118.7(11) . . ? C2 C3 C4 121.2(13) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 118.1(13) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 118.9(11) . . ? C6 C5 C8 120.9(12) . . ? C4 C5 C8 120.1(12) . . ? C5 C6 C7 121.8(12) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 120.0(12) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O3 C8 C5 111.8(11) . . ? O3 C8 H8A 109.3 . . ? C5 C8 H8A 109.3 . . ? O3 C8 H8B 109.3 . . ? C5 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C10 C9 O3 117.3(12) . . ? C10 C9 C14 118.0(13) . . ? O3 C9 C14 124.2(12) . . ? C9 C10 C11 123.6(12) . . ? C9 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 117.7(11) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C13 C12 O4 117.4(11) . . ? C13 C12 C11 117.8(12) . . ? O4 C12 C11 124.7(10) . . ? C12 C13 C14 124.2(12) . . ? C12 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C13 C14 C9 118.4(13) . . ? C13 C14 H14 120.8 . . ? C9 C14 H14 120.8 . . ? O4 C15 C17 111.1(10) . . ? O4 C15 C16 106.8(9) . . ? C17 C15 C16 109.6(10) . . ? O4 C15 H15 109.8 . . ? C17 C15 H15 109.8 . . ? C16 C15 H15 109.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 122.6(13) . . ? O6 C17 C15 123.1(12) . . ? O5 C17 C15 113.8(11) . . ? O8 C18 O7 122.4(18) . . ? O8 C18 C19 121.3(17) . . ? O7 C18 C19 116.3(16) . . ? C20 C19 C24 118.2(12) . . ? C20 C19 C18 122.1(13) . . ? C24 C19 C18 119.6(13) . . ? C19 C20 C21 120.7(12) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 121.6(12) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 118.9(12) . . ? C21 C22 C25 123.8(15) . . ? C23 C22 C25 116.7(14) . . ? C24 C23 C22 119.4(13) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C19 C24 C23 121.1(14) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? O9 C25 C22 107.8(11) . . ? O9 C25 H25A 110.2 . . ? C22 C25 H25A 110.2 . . ? O9 C25 H25B 110.2 . . ? C22 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C31 C26 C27 118.5(10) . . ? C31 C26 O9 126.7(10) . . ? C27 C26 O9 114.6(10) . . ? C26 C27 C28 119.6(11) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 120.6(10) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? O10 C29 C30 116.2(9) . . ? O10 C29 C28 126.1(10) . . ? C30 C29 C28 117.6(10) . . ? C31 C30 C29 121.4(10) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C26 C31 C30 122.0(11) . . ? C26 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? O10 C32 C33 105.0(10) . . ? O10 C32 C34 111.7(9) . . ? C33 C32 C34 113.3(11) . . ? O10 C32 H32 108.9 . . ? C33 C32 H32 108.9 . . ? C34 C32 H32 108.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O11 C34 O12 124.4(12) . . ? O11 C34 C32 120.8(12) . . ? O12 C34 C32 114.7(11) . . ? N1 C35 N2 115.7(13) . . ? N1 C35 H35 122.1 . . ? N2 C35 H35 122.1 . . ? C37 C36 N2 104.8(13) . . ? C37 C36 H36 127.6 . . ? N2 C36 H36 127.6 . . ? N1 C37 C36 110.1(13) . . ? N1 C37 H37 124.9 . . ? C36 C37 H37 124.9 . . ? N2 C38 C39 113.4(13) . . ? N2 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? N2 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 110.2(12) . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? C38 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C39 C40 C41 107.6(11) . . ? C39 C40 H40A 110.2 . . ? C41 C40 H40A 110.2 . . ? C39 C40 H40B 110.2 . . ? C41 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? N3 C41 C40 111.0(12) . . ? N3 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? N3 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C43 C42 N3 108.1(12) . . ? C43 C42 H42 125.9 . . ? N3 C42 H42 125.9 . . ? C42 C43 N4 109.7(13) . . ? C42 C43 H43 125.2 . . ? N4 C43 H43 125.2 . . ? N4 C44 N3 112.4(12) . . ? N4 C44 H44 123.8 . . ? N3 C44 H44 123.8 . . ? N5 C45 N6 111.5(13) . . ? N5 C45 H45 124.2 . . ? N6 C45 H45 124.2 . . ? C47 C46 N6 108.3(15) . . ? C47 C46 H46 125.8 . . ? N6 C46 H46 125.8 . . ? C46 C47 N5 109.7(15) . . ? C46 C47 H47 125.2 . . ? N5 C47 H47 125.2 . . ? C49 C48 N6 116.8(15) . . ? C49 C48 H48A 108.1 . . ? N6 C48 H48A 108.1 . . ? C49 C48 H48B 108.1 . . ? N6 C48 H48B 108.1 . . ? H48A C48 H48B 107.3 . . ? C48 C49 C50 120.3(17) . . ? C48 C49 H49A 107.3 . . ? C50 C49 H49A 107.3 . . ? C48 C49 H49B 107.3 . . ? C50 C49 H49B 107.3 . . ? H49A C49 H49B 106.9 . . ? C51 C50 C49 113.6(15) . . ? C51 C50 H50A 108.8 . . ? C49 C50 H50A 108.8 . . ? C51 C50 H50B 108.8 . . ? C49 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? N7 C51 C50 114.9(13) . . ? N7 C51 H51A 108.5 . . ? C50 C51 H51A 108.5 . . ? N7 C51 H51B 108.5 . . ? C50 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? N7 C52 C53 105.6(12) . . ? N7 C52 H52 127.2 . . ? C53 C52 H52 127.2 . . ? N8 C53 C52 111.6(12) . . ? N8 C53 H53 124.2 . . ? C52 C53 H53 124.2 . . ? N7 C54 N8 112.3(12) . . ? N7 C54 H54 123.9 . . ? N8 C54 H54 123.9 . . ? C35 N1 C37 104.4(12) . . ? C35 N1 Zn1 125.6(10) . . ? C37 N1 Zn1 129.2(9) . . ? C35 N2 C36 104.7(11) . . ? C35 N2 C38 126.8(13) . . ? C36 N2 C38 127.8(12) . . ? C42 N3 C44 106.8(11) . . ? C42 N3 C41 127.0(11) . . ? C44 N3 C41 125.0(11) . . ? C44 N4 C43 103.0(11) . . ? C44 N4 Zn1 135.3(9) . 2_556 ? C43 N4 Zn1 121.5(9) . 2_556 ? C45 N5 C47 104.9(13) . . ? C45 N5 Zn2 124.2(10) . . ? C47 N5 Zn2 130.6(10) . . ? C45 N6 C46 105.5(13) . . ? C45 N6 C48 125.6(14) . . ? C46 N6 C48 128.8(14) . . ? C54 N7 C52 105.9(12) . . ? C54 N7 C51 128.1(13) . . ? C52 N7 C51 125.2(13) . . ? C53 N8 C54 104.4(11) . . ? C53 N8 Zn2 122.5(9) . 2_245 ? C54 N8 Zn2 132.5(10) . 2_245 ? C1 O2 Zn1 116.4(9) . 1_254 ? C9 O3 C8 118.1(11) . . ? C12 O4 C15 118.7(8) . . ? C17 O5 Zn2 118.6(8) . . ? C18 O7 Zn2 107.0(12) . . ? C25 O9 C26 116.6(10) . . ? C29 O10 C32 116.4(8) . . ? C34 O12 Zn1 108.4(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 159.1(15) . . . . ? O2 C1 C2 C7 -20.4(19) . . . . ? O1 C1 C2 C3 -24(2) . . . . ? O2 C1 C2 C3 156.5(13) . . . . ? C7 C2 C3 C4 1(2) . . . . ? C1 C2 C3 C4 -175.9(13) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 -4(2) . . . . ? C3 C4 C5 C8 175.4(13) . . . . ? C4 C5 C6 C7 7(2) . . . . ? C8 C5 C6 C7 -172.1(14) . . . . ? C3 C2 C7 C6 2(2) . . . . ? C1 C2 C7 C6 179.0(13) . . . . ? C5 C6 C7 C2 -6(2) . . . . ? C6 C5 C8 O3 -144.7(14) . . . . ? C4 C5 C8 O3 36(2) . . . . ? O3 C9 C10 C11 179.1(13) . . . . ? C14 C9 C10 C11 7(3) . . . . ? C9 C10 C11 C12 -3(2) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C10 C11 C12 O4 -175.8(13) . . . . ? O4 C12 C13 C14 175.1(13) . . . . ? C11 C12 C13 C14 -2(2) . . . . ? C12 C13 C14 C9 5(2) . . . . ? C10 C9 C14 C13 -7(2) . . . . ? O3 C9 C14 C13 -179.1(14) . . . . ? O4 C15 C17 O6 11.9(17) . . . . ? C16 C15 C17 O6 -105.9(15) . . . . ? O4 C15 C17 O5 -160.7(10) . . . . ? C16 C15 C17 O5 81.6(14) . . . . ? O8 C18 C19 C20 -179.3(16) . . . . ? O7 C18 C19 C20 -1(2) . . . . ? O8 C18 C19 C24 4(3) . . . . ? O7 C18 C19 C24 -177.2(14) . . . . ? C24 C19 C20 C21 -0.2(17) . . . . ? C18 C19 C20 C21 -176.5(13) . . . . ? C19 C20 C21 C22 -1.9(19) . . . . ? C20 C21 C22 C23 4(2) . . . . ? C20 C21 C22 C25 175.2(11) . . . . ? C21 C22 C23 C24 -4(2) . . . . ? C25 C22 C23 C24 -176.0(13) . . . . ? C20 C19 C24 C23 -0.1(19) . . . . ? C18 C19 C24 C23 176.3(14) . . . . ? C22 C23 C24 C19 2(2) . . . . ? C21 C22 C25 O9 114.0(16) . . . . ? C23 C22 C25 O9 -74.7(17) . . . . ? C31 C26 C27 C28 -6(2) . . . . ? O9 C26 C27 C28 177.2(12) . . . . ? C26 C27 C28 C29 4(2) . . . . ? C27 C28 C29 O10 178.7(12) . . . . ? C27 C28 C29 C30 -0.9(19) . . . . ? O10 C29 C30 C31 179.5(10) . . . . ? C28 C29 C30 C31 -0.9(17) . . . . ? C27 C26 C31 C30 4.6(18) . . . . ? O9 C26 C31 C30 -179.3(12) . . . . ? C29 C30 C31 C26 -1.0(17) . . . . ? O10 C32 C34 O11 -115.8(13) . . . . ? C33 C32 C34 O11 125.9(13) . . . . ? O10 C32 C34 O12 61.9(13) . . . . ? C33 C32 C34 O12 -56.3(15) . . . . ? N2 C36 C37 N1 -3.5(18) . . . . ? N2 C38 C39 C40 168.7(12) . . . . ? C38 C39 C40 C41 177.2(11) . . . . ? C39 C40 C41 N3 163.2(12) . . . . ? N3 C42 C43 N4 1.0(18) . . . . ? N6 C46 C47 N5 -3(2) . . . . ? N6 C48 C49 C50 -169.9(17) . . . . ? C48 C49 C50 C51 171.1(18) . . . . ? C49 C50 C51 N7 -169.4(15) . . . . ? N7 C52 C53 N8 1.5(18) . . . . ? N2 C35 N1 C37 1.8(18) . . . . ? N2 C35 N1 Zn1 172.6(9) . . . . ? C36 C37 N1 C35 1.2(17) . . . . ? C36 C37 N1 Zn1 -169.1(11) . . . . ? O2 Zn1 N1 C35 -149.2(12) 1_856 . . . ? O12 Zn1 N1 C35 79.5(13) . . . . ? N4 Zn1 N1 C35 -40.1(13) 2_546 . . . ? O2 Zn1 N1 C37 19.3(13) 1_856 . . . ? O12 Zn1 N1 C37 -112.0(11) . . . . ? N4 Zn1 N1 C37 128.4(12) 2_546 . . . ? N1 C35 N2 C36 -3.9(18) . . . . ? N1 C35 N2 C38 -175.1(14) . . . . ? C37 C36 N2 C35 4.3(17) . . . . ? C37 C36 N2 C38 175.3(13) . . . . ? C39 C38 N2 C35 -62.4(19) . . . . ? C39 C38 N2 C36 128.5(16) . . . . ? C43 C42 N3 C44 -1.9(18) . . . . ? C43 C42 N3 C41 -169.9(14) . . . . ? N4 C44 N3 C42 2.3(18) . . . . ? N4 C44 N3 C41 170.6(15) . . . . ? C40 C41 N3 C42 -63(2) . . . . ? C40 C41 N3 C44 130.7(15) . . . . ? N3 C44 N4 C43 -1.6(17) . . . . ? N3 C44 N4 Zn1 -176.0(10) . . . 2_556 ? C42 C43 N4 C44 0.4(17) . . . . ? C42 C43 N4 Zn1 175.7(10) . . . 2_556 ? N6 C45 N5 C47 -1.2(17) . . . . ? N6 C45 N5 Zn2 -175.1(8) . . . . ? C46 C47 N5 C45 2.7(19) . . . . ? C46 C47 N5 Zn2 176.0(11) . . . . ? O5 Zn2 N5 C45 -85.0(11) . . . . ? O7 Zn2 N5 C45 146.7(11) . . . . ? N8 Zn2 N5 C45 36.7(12) 2_255 . . . ? O5 Zn2 N5 C47 102.9(13) . . . . ? O7 Zn2 N5 C47 -25.5(15) . . . . ? N8 Zn2 N5 C47 -135.5(13) 2_255 . . . ? N5 C45 N6 C46 -0.6(17) . . . . ? N5 C45 N6 C48 177.2(13) . . . . ? C47 C46 N6 C45 2.3(19) . . . . ? C47 C46 N6 C48 -175.4(16) . . . . ? C49 C48 N6 C45 63(2) . . . . ? C49 C48 N6 C46 -120(2) . . . . ? N8 C54 N7 C52 -3.2(17) . . . . ? N8 C54 N7 C51 -172.8(15) . . . . ? C53 C52 N7 C54 1.1(17) . . . . ? C53 C52 N7 C51 171.0(15) . . . . ? C50 C51 N7 C54 -129.5(16) . . . . ? C50 C51 N7 C52 63(2) . . . . ? C52 C53 N8 C54 -3.3(17) . . . . ? C52 C53 N8 Zn2 -175.3(10) . . . 2_245 ? N7 C54 N8 C53 4.1(16) . . . . ? N7 C54 N8 Zn2 174.9(10) . . . 2_245 ? O1 C1 O2 Zn1 4(2) . . . 1_254 ? C2 C1 O2 Zn1 -177.0(8) . . . 1_254 ? C10 C9 O3 C8 -175.3(15) . . . . ? C14 C9 O3 C8 -3(2) . . . . ? C5 C8 O3 C9 -169.7(13) . . . . ? C13 C12 O4 C15 -179.5(12) . . . . ? C11 C12 O4 C15 -3.0(19) . . . . ? C17 C15 O4 C12 71.8(14) . . . . ? C16 C15 O4 C12 -168.7(11) . . . . ? O6 C17 O5 Zn2 -15.2(17) . . . . ? C15 C17 O5 Zn2 157.3(8) . . . . ? N5 Zn2 O5 C17 55.9(10) . . . . ? O7 Zn2 O5 C17 -163.7(9) . . . . ? N8 Zn2 O5 C17 -68.7(10) 2_255 . . . ? O8 C18 O7 Zn2 -15(2) . . . . ? C19 C18 O7 Zn2 166.8(11) . . . . ? O5 Zn2 O7 C18 -86.1(13) . . . . ? N5 Zn2 O7 C18 50.0(14) . . . . ? N8 Zn2 O7 C18 168.4(13) 2_255 . . . ? C22 C25 O9 C26 179.8(12) . . . . ? C31 C26 O9 C25 -39(2) . . . . ? C27 C26 O9 C25 137.0(14) . . . . ? C30 C29 O10 C32 171.5(10) . . . . ? C28 C29 O10 C32 -8.1(16) . . . . ? C33 C32 O10 C29 -162.9(10) . . . . ? C34 C32 O10 C29 73.9(12) . . . . ? O11 C34 O12 Zn1 7.4(16) . . . . ? C32 C34 O12 Zn1 -170.2(7) . . . . ? O2 Zn1 O12 C34 172.3(8) 1_856 . . . ? N1 Zn1 O12 C34 -49.9(10) . . . . ? N4 Zn1 O12 C34 69.4(9) 2_546 . . . ? 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 C27 H27 O10 0.93 2.49 3.392(14) 164.6 1_455 C30 H30 O9 0.93 2.50 3.421(14) 171.7 1_655 C38 H38B O1 0.97 2.46 3.115(17) 125.0 1_756 C41 H41A O12 0.97 2.57 3.326(16) 134.9 2_656 C42 H42 O11 0.93 2.40 3.299(16) 163.5 1_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.921 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.082 #=========================END data_Compound-8 _database_code_depnum_ccdc_archive 'CCDC 877938' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H28 Cd N4 O6' _chemical_formula_sum 'C31 H28 Cd N4 O6' _chemical_formula_weight 664.97 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'p 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2789(2) _cell_length_b 16.8823(5) _cell_length_c 23.5500(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2893.93(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5798 _cell_measurement_theta_min 3.0415 _cell_measurement_theta_max 29.1403 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7883 _exptl_absorpt_correction_T_max 0.8555 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11898 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5097 _reflns_number_gt 4702 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0289P)^2^+1.6679P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 5097 _refine_ls_number_parameters 379 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.004 _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 0.19358(4) 0.39688(2) 0.827971(14) 0.04811(10) Uani 1 1 d U . . C1 C 0.4689(6) 0.3771(3) 0.7509(2) 0.0549(7) Uani 1 1 d U . . C2 C 0.6306(5) 0.3716(2) 0.71198(17) 0.0407(10) Uani 1 1 d . . . C3 C 0.6330(6) 0.3194(3) 0.6666(2) 0.0501(11) Uani 1 1 d . . . H3 H 0.5302 0.2885 0.6590 0.060 Uiso 1 1 calc R . . C4 C 0.7864(7) 0.3130(3) 0.6326(2) 0.0561(12) Uani 1 1 d . . . H4 H 0.7862 0.2778 0.6023 0.067 Uiso 1 1 calc R . . C5 C 0.9403(6) 0.3583(3) 0.64328(18) 0.0460(11) Uani 1 1 d . . . C6 C 0.9369(6) 0.4109(3) 0.68743(17) 0.0530(12) Uani 1 1 d . . . H6 H 1.0391 0.4425 0.6946 0.064 Uiso 1 1 calc R . . C7 C 0.7838(6) 0.4176(3) 0.72120(18) 0.0548(12) Uani 1 1 d . . . H7 H 0.7837 0.4540 0.7509 0.066 Uiso 1 1 calc R . . C8 C 1.1104(6) 0.3479(3) 0.60877(18) 0.0534(12) Uani 1 1 d . . . H8A H 1.2030 0.3857 0.6207 0.064 Uiso 1 1 calc R . . H8B H 1.1591 0.2949 0.6142 0.064 Uiso 1 1 calc R . . C9 C 1.2123(7) 0.3581(2) 0.51268(18) 0.0448(10) Uani 1 1 d . . . C10 C 1.1710(7) 0.3751(2) 0.45756(17) 0.0481(11) Uani 1 1 d . . . H10 H 1.0498 0.3843 0.4470 0.058 Uiso 1 1 calc R . . C11 C 1.3094(7) 0.3786(2) 0.41721(18) 0.0503(11) Uani 1 1 d . . . H11 H 1.2812 0.3905 0.3797 0.060 Uiso 1 1 calc R . . C12 C 1.4895(6) 0.3643(3) 0.43290(19) 0.0461(11) Uani 1 1 d . . . C13 C 1.5290(7) 0.3435(3) 0.48751(19) 0.0516(11) Uani 1 1 d . . . H13 H 1.6491 0.3311 0.4976 0.062 Uiso 1 1 calc R . . C14 C 1.3922(7) 0.3407(3) 0.5278(2) 0.0549(13) Uani 1 1 d . . . H14 H 1.4202 0.3272 0.5651 0.066 Uiso 1 1 calc R . . C15 C 1.6046(7) 0.3886(3) 0.33891(18) 0.0540(12) Uani 1 1 d . . . H15 H 1.5192 0.3505 0.3219 0.065 Uiso 1 1 calc R . . C16 C 1.7886(8) 0.3845(3) 0.3085(2) 0.0751(16) Uani 1 1 d . . . H16A H 1.8370 0.3317 0.3113 0.113 Uiso 1 1 calc R . . H16B H 1.8727 0.4210 0.3258 0.113 Uiso 1 1 calc R . . H16C H 1.7722 0.3980 0.2692 0.113 Uiso 1 1 calc R . . C17 C 1.5238(6) 0.4723(3) 0.3347(2) 0.0479(11) Uani 1 1 d . . . C18 C 0.5049(6) 0.4358(3) 0.92110(18) 0.0458(10) Uani 1 1 d . . . H18 H 0.5849 0.4483 0.8917 0.055 Uiso 1 1 calc R . . C19 C 0.3931(7) 0.4212(4) 1.0054(2) 0.0709(16) Uani 1 1 d . . . H19 H 0.3790 0.4211 1.0446 0.085 Uiso 1 1 calc R . . C20 C 0.2674(6) 0.3991(4) 0.9674(2) 0.0688(14) Uani 1 1 d . . . H20 H 0.1503 0.3806 0.9760 0.083 Uiso 1 1 calc R . . C21 C 0.7126(7) 0.4802(3) 0.99906(19) 0.0549(12) Uani 1 1 d . . . H21A H 0.6816 0.5316 1.0149 0.066 Uiso 1 1 calc R . . H21B H 0.7979 0.4890 0.9680 0.066 Uiso 1 1 calc R . . C22 C 0.8069(7) 0.4319(3) 1.04394(18) 0.0480(10) Uani 1 1 d . . . C23 C 0.8776(7) 0.4690(3) 1.0912(2) 0.0596(13) Uani 1 1 d . . . H23 H 0.8656 0.5236 1.0949 0.072 Uiso 1 1 calc R . . C24 C 0.9660(7) 0.4265(3) 1.1331(2) 0.0675(15) Uani 1 1 d . . . H24 H 1.0101 0.4526 1.1651 0.081 Uiso 1 1 calc R . . C25 C 0.9896(6) 0.3467(3) 1.1282(2) 0.0601(14) Uani 1 1 d U . . C26 C 0.9228(8) 0.3104(3) 1.0803(3) 0.0747(16) Uani 1 1 d . . . H26 H 0.9389 0.2560 1.0761 0.090 Uiso 1 1 calc R . . C27 C 0.8332(9) 0.3514(3) 1.0386(2) 0.0615(14) Uani 1 1 d . . . H27 H 0.7901 0.3250 1.0066 0.074 Uiso 1 1 calc R . . C28 C 1.0653(7) 0.2988(4) 1.1767(3) 0.090(2) Uani 1 1 d U . . H28A H 1.0418 0.3272 1.2117 0.108 Uiso 1 1 calc R . . H28B H 0.9984 0.2491 1.1786 0.108 Uiso 1 1 calc R . . C29 C 1.4012(9) 0.3281(4) 1.1889(3) 0.099(2) Uani 1 1 d . . . H29 H 1.3927 0.3809 1.2000 0.119 Uiso 1 1 calc R . . C30 C 1.5540(8) 0.2850(4) 1.1852(3) 0.097(2) Uani 1 1 d . . . H30 H 1.6712 0.3034 1.1938 0.116 Uiso 1 1 calc R . . C31 C 1.3361(6) 0.2113(3) 1.1619(2) 0.0567(12) Uani 1 1 d . . . H31 H 1.2678 0.1674 1.1509 0.068 Uiso 1 1 calc R . . N1 N 0.3371(5) 0.4076(2) 0.91371(15) 0.0537(7) Uani 1 1 d U . . N2 N 0.5453(5) 0.4439(2) 0.97638(16) 0.0518(9) Uani 1 1 d . . . N3 N 1.2626(5) 0.2809(2) 1.1736(2) 0.0592(10) Uani 1 1 d U . . N4 N 1.5146(5) 0.2107(2) 1.16726(19) 0.0534(9) Uani 1 1 d . . . O1 O 0.3297(5) 0.33882(19) 0.74212(13) 0.0607(6) Uani 1 1 d U . . O2 O 0.4836(4) 0.4207(2) 0.79358(14) 0.0628(6) Uani 1 1 d U . . O3 O 1.0666(4) 0.3600(2) 0.55048(13) 0.0572(9) Uani 1 1 d . . . O4 O 1.6388(4) 0.36733(18) 0.39661(12) 0.0564(9) Uani 1 1 d . . . O5 O 1.4047(5) 0.48355(19) 0.29671(14) 0.0601(8) Uani 1 1 d . . . O6 O 1.5733(5) 0.52510(19) 0.36806(14) 0.0575(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03534(15) 0.05358(17) 0.05540(18) -0.00887(17) 0.00487(17) -0.00384(16) C1 0.0411(12) 0.0662(13) 0.0574(12) -0.0082(12) 0.0039(12) -0.0013(12) C2 0.037(2) 0.050(3) 0.035(2) 0.0053(19) -0.0035(17) 0.0017(18) C3 0.043(2) 0.053(3) 0.054(3) 0.004(2) 0.000(2) -0.0123(19) C4 0.061(3) 0.052(3) 0.055(3) -0.005(2) 0.012(3) 0.001(3) C5 0.044(2) 0.058(3) 0.036(2) 0.003(2) 0.006(2) 0.002(2) C6 0.037(2) 0.075(3) 0.047(3) -0.009(2) 0.0017(19) -0.010(2) C7 0.047(3) 0.074(3) 0.044(2) -0.019(2) 0.000(2) -0.002(3) C8 0.048(3) 0.068(3) 0.044(3) 0.002(2) 0.009(2) 0.009(2) C9 0.043(2) 0.044(2) 0.047(2) 0.000(2) 0.016(2) 0.001(2) C10 0.045(3) 0.051(3) 0.048(2) 0.002(2) 0.003(2) -0.001(2) C11 0.059(3) 0.046(3) 0.046(2) 0.0017(19) 0.009(2) -0.002(3) C12 0.049(3) 0.037(2) 0.052(3) 0.003(2) 0.015(2) 0.000(2) C13 0.046(3) 0.055(3) 0.054(3) 0.008(2) 0.004(2) 0.005(2) C14 0.054(3) 0.069(3) 0.042(2) 0.012(2) 0.009(2) 0.004(2) C15 0.063(3) 0.048(3) 0.051(3) 0.001(2) 0.016(2) 0.004(2) C16 0.081(4) 0.067(3) 0.077(3) 0.006(3) 0.040(3) 0.023(3) C17 0.043(2) 0.054(3) 0.046(3) 0.005(2) 0.016(2) -0.002(2) C18 0.038(2) 0.051(3) 0.048(3) 0.000(2) 0.008(2) 0.000(2) C19 0.059(3) 0.102(5) 0.052(3) 0.006(3) 0.014(3) -0.007(3) C20 0.042(2) 0.104(4) 0.060(3) 0.005(3) 0.011(2) -0.009(3) C21 0.059(3) 0.053(3) 0.052(3) 0.003(2) -0.013(3) -0.009(3) C22 0.040(2) 0.051(2) 0.054(3) 0.004(2) 0.001(2) 0.001(2) C23 0.070(3) 0.048(3) 0.061(3) 0.001(2) -0.013(3) 0.008(2) C24 0.064(3) 0.075(4) 0.064(3) 0.006(3) -0.015(3) 0.007(3) C25 0.034(2) 0.069(3) 0.078(4) 0.030(3) 0.006(3) 0.015(2) C26 0.070(4) 0.042(3) 0.112(5) 0.010(3) 0.012(4) 0.012(3) C27 0.068(4) 0.045(3) 0.071(3) -0.006(2) 0.000(3) 0.005(3) C28 0.049(3) 0.113(5) 0.108(4) 0.058(4) 0.016(3) 0.027(3) C29 0.071(4) 0.062(4) 0.163(8) -0.032(4) -0.006(4) 0.020(3) C30 0.043(3) 0.073(4) 0.174(8) -0.044(5) -0.013(4) -0.001(3) C31 0.044(3) 0.053(3) 0.073(3) 0.007(2) -0.014(2) 0.000(2) N1 0.0386(12) 0.0649(14) 0.0575(13) -0.0095(13) 0.0053(12) -0.0035(13) N2 0.048(2) 0.061(2) 0.047(2) 0.0030(19) 0.0007(18) -0.0005(19) N3 0.039(2) 0.065(2) 0.074(2) 0.023(2) 0.004(2) 0.0102(18) N4 0.0368(19) 0.055(2) 0.069(2) -0.008(2) -0.007(2) 0.0041(17) O1 0.0449(11) 0.0709(12) 0.0664(11) -0.0063(11) 0.0090(11) -0.0048(11) O2 0.0465(10) 0.0775(11) 0.0643(10) -0.0130(10) 0.0081(10) -0.0042(10) O3 0.0447(18) 0.081(2) 0.0456(17) 0.0051(16) 0.0129(15) 0.0033(17) O4 0.054(2) 0.062(2) 0.0529(18) 0.0114(16) 0.0179(15) 0.0103(15) O5 0.065(2) 0.063(2) 0.0526(18) 0.0063(16) 0.0029(17) -0.0013(18) O6 0.0573(19) 0.056(2) 0.059(2) -0.0011(17) 0.0036(17) 0.0028(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N4 2.237(4) 3_357 ? Cd1 O5 2.265(3) 2_665 ? Cd1 N1 2.281(4) . ? Cd1 O2 2.297(3) . ? Cd1 O1 2.456(3) . ? Cd1 O6 2.530(3) 2_665 ? Cd1 C17 2.722(5) 2_665 ? Cd1 C1 2.724(5) . ? C1 O1 1.220(5) . ? C1 O2 1.250(5) . ? C1 C2 1.495(6) . ? C2 C7 1.377(6) . ? C2 C3 1.384(6) . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.379(7) . ? C4 H4 0.9300 . ? C5 C6 1.368(6) . ? C5 C8 1.492(6) . ? C6 C7 1.373(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.424(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.363(6) . ? C9 O3 1.385(5) . ? C9 C14 1.388(6) . ? C10 C11 1.386(6) . ? C10 H10 0.9300 . ? C11 C12 1.383(7) . ? C11 H11 0.9300 . ? C12 C13 1.364(6) . ? C12 O4 1.383(5) . ? C13 C14 1.376(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.427(5) . ? C15 C16 1.520(6) . ? C15 C17 1.533(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.242(5) . ? C17 O5 1.261(6) . ? C17 Cd1 2.722(4) 2_664 ? C18 N1 1.322(5) . ? C18 N2 1.342(5) . ? C18 H18 0.9300 . ? C19 C20 1.333(7) . ? C19 N2 1.356(6) . ? C19 H19 0.9300 . ? C20 N1 1.369(6) . ? C20 H20 0.9300 . ? C21 N2 1.465(6) . ? C21 C22 1.501(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.377(6) . ? C22 C27 1.377(6) . ? C23 C24 1.380(7) . ? C23 H23 0.9300 . ? C24 C25 1.363(7) . ? C24 H24 0.9300 . ? C25 C26 1.373(8) . ? C25 C28 1.503(7) . ? C26 C27 1.368(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 N3 1.469(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.332(8) . ? C29 N3 1.335(7) . ? C29 H29 0.9300 . ? C30 N4 1.355(7) . ? C30 H30 0.9300 . ? C31 N4 1.306(5) . ? C31 N3 1.320(6) . ? C31 H31 0.9300 . ? N4 Cd1 2.237(4) 3_657 ? O5 Cd1 2.265(3) 2_664 ? O6 Cd1 2.530(3) 2_664 ? 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 N4 Cd1 O5 123.76(13) 3_357 2_665 ? N4 Cd1 N1 106.66(15) 3_357 . ? O5 Cd1 N1 111.21(13) 2_665 . ? N4 Cd1 O2 134.03(13) 3_357 . ? O5 Cd1 O2 91.12(13) 2_665 . ? N1 Cd1 O2 82.95(12) . . ? N4 Cd1 O1 87.26(13) 3_357 . ? O5 Cd1 O1 102.45(12) 2_665 . ? N1 Cd1 O1 125.16(12) . . ? O2 Cd1 O1 53.76(11) . . ? N4 Cd1 O6 87.53(12) 3_357 2_665 ? O5 Cd1 O6 54.17(11) 2_665 2_665 ? N1 Cd1 O6 88.85(12) . 2_665 ? O2 Cd1 O6 138.26(11) . 2_665 ? O1 Cd1 O6 145.58(11) . 2_665 ? N4 Cd1 C17 108.49(13) 3_357 2_665 ? O5 Cd1 C17 27.37(13) 2_665 2_665 ? N1 Cd1 C17 98.64(13) . 2_665 ? O2 Cd1 C17 114.38(14) . 2_665 ? O1 Cd1 C17 127.34(13) . 2_665 ? O6 Cd1 C17 27.03(12) 2_665 2_665 ? N4 Cd1 C1 111.26(15) 3_357 . ? O5 Cd1 C1 97.17(14) 2_665 . ? N1 Cd1 C1 105.21(13) . . ? O2 Cd1 C1 27.15(12) . . ? O1 Cd1 C1 26.61(12) . . ? O6 Cd1 C1 151.31(13) 2_665 . ? C17 Cd1 C1 124.46(15) 2_665 . ? O1 C1 O2 121.3(4) . . ? O1 C1 C2 121.1(4) . . ? O2 C1 C2 117.6(4) . . ? O1 C1 Cd1 64.3(2) . . ? O2 C1 Cd1 57.0(2) . . ? C2 C1 Cd1 174.6(3) . . ? C7 C2 C3 118.1(4) . . ? C7 C2 C1 120.4(4) . . ? C3 C2 C1 121.6(4) . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.0(4) . . ? C6 C5 C8 120.4(4) . . ? C4 C5 C8 120.6(4) . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 121.3(4) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? O3 C8 C5 108.8(4) . . ? O3 C8 H8A 109.9 . . ? C5 C8 H8A 109.9 . . ? O3 C8 H8B 109.9 . . ? C5 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 O3 116.0(4) . . ? C10 C9 C14 119.7(4) . . ? O3 C9 C14 124.3(4) . . ? C9 C10 C11 120.1(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 119.8(4) . . ? C13 C12 O4 115.2(4) . . ? C11 C12 O4 125.0(4) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 120.0(4) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? O4 C15 C16 106.4(4) . . ? O4 C15 C17 111.1(4) . . ? C16 C15 C17 110.5(4) . . ? O4 C15 H15 109.6 . . ? C16 C15 H15 109.6 . . ? C17 C15 H15 109.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 122.7(4) . . ? O6 C17 C15 120.7(4) . . ? O5 C17 C15 116.7(4) . . ? O6 C17 Cd1 67.8(2) . 2_664 ? O5 C17 Cd1 55.7(2) . 2_664 ? C15 C17 Cd1 167.0(3) . 2_664 ? N1 C18 N2 111.5(4) . . ? N1 C18 H18 124.2 . . ? N2 C18 H18 124.2 . . ? C20 C19 N2 107.6(4) . . ? C20 C19 H19 126.2 . . ? N2 C19 H19 126.2 . . ? C19 C20 N1 109.6(4) . . ? C19 C20 H20 125.2 . . ? N1 C20 H20 125.2 . . ? N2 C21 C22 114.2(4) . . ? N2 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N2 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C27 118.1(5) . . ? C23 C22 C21 119.5(4) . . ? C27 C22 C21 122.4(5) . . ? C22 C23 C24 121.1(5) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 120.8(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 117.8(5) . . ? C24 C25 C28 120.9(6) . . ? C26 C25 C28 120.9(5) . . ? C27 C26 C25 122.2(5) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C22 120.0(5) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? N3 C28 C25 115.5(5) . . ? N3 C28 H28A 108.4 . . ? C25 C28 H28A 108.4 . . ? N3 C28 H28B 108.4 . . ? C25 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C30 C29 N3 106.7(5) . . ? C30 C29 H29 126.7 . . ? N3 C29 H29 126.7 . . ? C29 C30 N4 110.5(5) . . ? C29 C30 H30 124.8 . . ? N4 C30 H30 124.8 . . ? N4 C31 N3 113.0(4) . . ? N4 C31 H31 123.5 . . ? N3 C31 H31 123.5 . . ? C18 N1 C20 105.0(4) . . ? C18 N1 Cd1 124.6(3) . . ? C20 N1 Cd1 129.7(3) . . ? C18 N2 C19 106.3(4) . . ? C18 N2 C21 125.4(4) . . ? C19 N2 C21 127.9(4) . . ? C31 N3 C29 106.4(4) . . ? C31 N3 C28 126.1(5) . . ? C29 N3 C28 127.1(5) . . ? C31 N4 C30 103.4(4) . . ? C31 N4 Cd1 126.3(3) . 3_657 ? C30 N4 Cd1 127.8(3) . 3_657 ? C1 O1 Cd1 89.1(3) . . ? C1 O2 Cd1 95.8(3) . . ? C9 O3 C8 116.4(3) . . ? C12 O4 C15 117.4(4) . . ? C17 O5 Cd1 97.0(3) . 2_664 ? C17 O6 Cd1 85.2(3) . 2_664 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd1 C1 O1 27.0(3) 3_357 . . . ? O5 Cd1 C1 O1 -103.5(3) 2_665 . . . ? N1 Cd1 C1 O1 142.1(3) . . . . ? O2 Cd1 C1 O1 178.2(5) . . . . ? O6 Cd1 C1 O1 -100.9(4) 2_665 . . . ? C17 Cd1 C1 O1 -105.8(3) 2_665 . . . ? N4 Cd1 C1 O2 -151.1(3) 3_357 . . . ? O5 Cd1 C1 O2 78.3(3) 2_665 . . . ? N1 Cd1 C1 O2 -36.0(3) . . . . ? O1 Cd1 C1 O2 -178.2(5) . . . . ? O6 Cd1 C1 O2 81.0(4) 2_665 . . . ? C17 Cd1 C1 O2 76.0(3) 2_665 . . . ? N4 Cd1 C1 C2 -151(4) 3_357 . . . ? O5 Cd1 C1 C2 78(4) 2_665 . . . ? N1 Cd1 C1 C2 -36(4) . . . . ? O2 Cd1 C1 C2 0(3) . . . . ? O1 Cd1 C1 C2 -178(100) . . . . ? O6 Cd1 C1 C2 81(4) 2_665 . . . ? C17 Cd1 C1 C2 76(4) 2_665 . . . ? O1 C1 C2 C7 177.3(5) . . . . ? O2 C1 C2 C7 -4.6(7) . . . . ? Cd1 C1 C2 C7 -5(4) . . . . ? O1 C1 C2 C3 -4.0(7) . . . . ? O2 C1 C2 C3 174.1(4) . . . . ? Cd1 C1 C2 C3 174(3) . . . . ? C7 C2 C3 C4 1.3(7) . . . . ? C1 C2 C3 C4 -177.4(4) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? C3 C4 C5 C8 176.2(4) . . . . ? C4 C5 C6 C7 1.1(7) . . . . ? C8 C5 C6 C7 -176.5(4) . . . . ? C5 C6 C7 C2 0.4(7) . . . . ? C3 C2 C7 C6 -1.6(7) . . . . ? C1 C2 C7 C6 177.1(4) . . . . ? C6 C5 C8 O3 -125.3(5) . . . . ? C4 C5 C8 O3 57.2(6) . . . . ? O3 C9 C10 C11 176.7(4) . . . . ? C14 C9 C10 C11 -3.0(7) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? C10 C11 C12 C13 2.8(6) . . . . ? C10 C11 C12 O4 -179.0(4) . . . . ? C11 C12 C13 C14 -3.5(7) . . . . ? O4 C12 C13 C14 178.1(4) . . . . ? C12 C13 C14 C9 0.9(8) . . . . ? C10 C9 C14 C13 2.4(8) . . . . ? O3 C9 C14 C13 -177.3(4) . . . . ? O4 C15 C17 O6 35.2(6) . . . . ? C16 C15 C17 O6 -82.7(5) . . . . ? O4 C15 C17 O5 -143.8(4) . . . . ? C16 C15 C17 O5 98.4(5) . . . . ? O4 C15 C17 Cd1 -92.9(15) . . . 2_664 ? C16 C15 C17 Cd1 149.2(13) . . . 2_664 ? N2 C19 C20 N1 -0.2(7) . . . . ? N2 C21 C22 C23 -138.5(5) . . . . ? N2 C21 C22 C27 44.5(8) . . . . ? C27 C22 C23 C24 -2.5(9) . . . . ? C21 C22 C23 C24 -179.6(5) . . . . ? C22 C23 C24 C25 1.6(9) . . . . ? C23 C24 C25 C26 0.1(8) . . . . ? C23 C24 C25 C28 -172.6(5) . . . . ? C24 C25 C26 C27 -0.7(9) . . . . ? C28 C25 C26 C27 172.0(5) . . . . ? C25 C26 C27 C22 -0.3(10) . . . . ? C23 C22 C27 C26 1.9(9) . . . . ? C21 C22 C27 C26 178.9(5) . . . . ? C24 C25 C28 N3 -98.1(7) . . . . ? C26 C25 C28 N3 89.5(7) . . . . ? N3 C29 C30 N4 0.4(9) . . . . ? N2 C18 N1 C20 1.2(5) . . . . ? N2 C18 N1 Cd1 172.6(3) . . . . ? C19 C20 N1 C18 -0.6(6) . . . . ? C19 C20 N1 Cd1 -171.3(4) . . . . ? N4 Cd1 N1 C18 146.9(4) 3_357 . . . ? O5 Cd1 N1 C18 -75.5(4) 2_665 . . . ? O2 Cd1 N1 C18 12.9(4) . . . . ? O1 Cd1 N1 C18 48.3(4) . . . . ? O6 Cd1 N1 C18 -126.1(4) 2_665 . . . ? C17 Cd1 N1 C18 -100.8(4) 2_665 . . . ? C1 Cd1 N1 C18 28.6(4) . . . . ? N4 Cd1 N1 C20 -44.0(5) 3_357 . . . ? O5 Cd1 N1 C20 93.6(5) 2_665 . . . ? O2 Cd1 N1 C20 -177.9(5) . . . . ? O1 Cd1 N1 C20 -142.6(4) . . . . ? O6 Cd1 N1 C20 43.1(5) 2_665 . . . ? C17 Cd1 N1 C20 68.4(5) 2_665 . . . ? C1 Cd1 N1 C20 -162.2(5) . . . . ? N1 C18 N2 C19 -1.3(6) . . . . ? N1 C18 N2 C21 -174.1(4) . . . . ? C20 C19 N2 C18 0.9(6) . . . . ? C20 C19 N2 C21 173.4(5) . . . . ? C22 C21 N2 C18 -131.2(5) . . . . ? C22 C21 N2 C19 57.6(7) . . . . ? N4 C31 N3 C29 -1.6(7) . . . . ? N4 C31 N3 C28 -173.9(6) . . . . ? C30 C29 N3 C31 0.6(8) . . . . ? C30 C29 N3 C28 172.9(6) . . . . ? C25 C28 N3 C31 -107.1(7) . . . . ? C25 C28 N3 C29 82.1(9) . . . . ? N3 C31 N4 C30 1.8(7) . . . . ? N3 C31 N4 Cd1 164.9(3) . . . 3_657 ? C29 C30 N4 C31 -1.3(8) . . . . ? C29 C30 N4 Cd1 -164.1(5) . . . 3_657 ? O2 C1 O1 Cd1 1.8(5) . . . . ? C2 C1 O1 Cd1 179.8(4) . . . . ? N4 Cd1 O1 C1 -154.9(3) 3_357 . . . ? O5 Cd1 O1 C1 81.1(3) 2_665 . . . ? N1 Cd1 O1 C1 -46.4(3) . . . . ? O2 Cd1 O1 C1 -1.0(3) . . . . ? O6 Cd1 O1 C1 123.5(3) 2_665 . . . ? C17 Cd1 O1 C1 93.8(3) 2_665 . . . ? O1 C1 O2 Cd1 -1.9(5) . . . . ? C2 C1 O2 Cd1 180.0(4) . . . . ? N4 Cd1 O2 C1 38.7(4) 3_357 . . . ? O5 Cd1 O2 C1 -103.6(3) 2_665 . . . ? N1 Cd1 O2 C1 145.1(3) . . . . ? O1 Cd1 O2 C1 1.0(3) . . . . ? O6 Cd1 O2 C1 -134.6(3) 2_665 . . . ? C17 Cd1 O2 C1 -118.5(3) 2_665 . . . ? C10 C9 O3 C8 -175.8(4) . . . . ? C14 C9 O3 C8 3.9(7) . . . . ? C5 C8 O3 C9 175.6(4) . . . . ? C13 C12 O4 C15 179.8(4) . . . . ? C11 C12 O4 C15 1.5(6) . . . . ? C16 C15 O4 C12 -178.0(4) . . . . ? C17 C15 O4 C12 61.7(5) . . . . ? O6 C17 O5 Cd1 -11.2(5) . . . 2_664 ? C15 C17 O5 Cd1 167.8(3) . . . 2_664 ? O5 C17 O6 Cd1 10.0(4) . . . 2_664 ? C15 C17 O6 Cd1 -169.0(4) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.486 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.052 #=========================END data_Compound-9 _database_code_depnum_ccdc_archive 'CCDC 877939' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 Cd N6 O6' _chemical_formula_sum 'C29 H26 Cd N6 O6' _chemical_formula_weight 666.96 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'p 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2883(3) _cell_length_b 16.8613(8) _cell_length_c 23.5290(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2891.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5203 _cell_measurement_theta_min 2.8586 _cell_measurement_theta_max 29.1070 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7877 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11352 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4865 _reflns_number_gt 4317 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0523P)^2^+4.0670P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_number_reflns 4865 _refine_ls_number_parameters 379 _refine_ls_number_restraints 133 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.099 _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 0.19385(6) 0.89664(3) 0.32797(2) 0.04709(16) Uani 1 1 d U . . C1 C 0.4701(9) 0.8774(4) 0.2509(3) 0.0532(7) Uani 1 1 d U . . C2 C 0.6303(8) 0.8716(4) 0.2122(3) 0.0397(15) Uani 1 1 d . . . C3 C 0.6316(8) 0.8196(4) 0.1664(3) 0.0496(16) Uani 1 1 d . . . H3 H 0.5284 0.7891 0.1585 0.060 Uiso 1 1 calc R . . C4 C 0.7862(11) 0.8130(4) 0.1326(3) 0.0537(17) Uani 1 1 d . . . H4 H 0.7861 0.7776 0.1023 0.064 Uiso 1 1 calc R . . C5 C 0.9395(9) 0.8578(4) 0.1430(3) 0.0441(15) Uani 1 1 d . . . C6 C 0.9377(9) 0.9107(4) 0.1875(3) 0.0515(17) Uani 1 1 d . . . H6 H 1.0401 0.9421 0.1947 0.062 Uiso 1 1 calc R . . C7 C 0.7841(9) 0.9174(4) 0.2215(3) 0.0521(17) Uani 1 1 d . . . H7 H 0.7844 0.9535 0.2513 0.062 Uiso 1 1 calc R . . C8 C 1.1107(10) 0.8471(5) 0.1085(3) 0.0533(18) Uani 1 1 d . . . H8A H 1.2036 0.8846 0.1206 0.064 Uiso 1 1 calc R . . H8B H 1.1584 0.7939 0.1136 0.064 Uiso 1 1 calc R . . C9 C 1.2129(10) 0.8584(4) 0.0120(3) 0.0442(15) Uani 1 1 d . . . C10 C 1.1715(10) 0.8751(4) -0.0424(3) 0.0461(16) Uani 1 1 d . . . H10 H 1.0503 0.8842 -0.0528 0.055 Uiso 1 1 calc R . . C11 C 1.3090(10) 0.8789(3) -0.0829(3) 0.0464(15) Uani 1 1 d . . . H11 H 1.2806 0.8913 -0.1204 0.056 Uiso 1 1 calc R . . C12 C 1.4898(9) 0.8640(4) -0.0673(3) 0.0454(16) Uani 1 1 d . . . C13 C 1.5282(10) 0.8433(4) -0.0124(3) 0.0500(17) Uani 1 1 d . . . H13 H 1.6480 0.8309 -0.0021 0.060 Uiso 1 1 calc R . . C14 C 1.3926(10) 0.8408(5) 0.0274(3) 0.0559(19) Uani 1 1 d . . . H14 H 1.4201 0.8273 0.0648 0.067 Uiso 1 1 calc R . . C15 C 1.6036(10) 0.8893(4) -0.1603(3) 0.0530(17) Uani 1 1 d . . . H15 H 1.5185 0.8511 -0.1773 0.064 Uiso 1 1 calc R . . C16 C 1.7879(11) 0.8846(5) -0.1909(3) 0.069(2) Uani 1 1 d . . . H16A H 1.8355 0.8316 -0.1881 0.103 Uiso 1 1 calc R . . H16B H 1.8726 0.9210 -0.1738 0.103 Uiso 1 1 calc R . . H16C H 1.7716 0.8981 -0.2303 0.103 Uiso 1 1 calc R . . C17 C 1.5228(9) 0.9729(4) -0.1656(3) 0.0468(16) Uani 1 1 d . . . C18 C 0.0572(10) 0.7148(4) 0.3143(3) 0.0588(7) Uani 1 1 d U . . H18 H 0.1748 0.6976 0.3052 0.071 Uiso 1 1 calc R . . C19 C -0.1634(9) 0.7890(4) 0.3383(3) 0.0570(19) Uani 1 1 d . . . H19 H -0.2312 0.8336 0.3484 0.068 Uiso 1 1 calc R . . C20 C -0.4317(10) 0.7012(5) 0.3241(4) 0.0666(9) Uani 1 1 d U . . H20A H -0.4533 0.6736 0.2886 0.080 Uiso 1 1 calc R . . H20B H -0.4985 0.7509 0.3223 0.080 Uiso 1 1 calc R . . C21 C -0.5112(10) 0.6529(5) 0.3708(4) 0.0643(9) Uani 1 1 d U . . C22 C -0.5332(11) 0.5726(5) 0.3669(3) 0.066(2) Uani 1 1 d . . . H22 H -0.4872 0.5457 0.3355 0.079 Uiso 1 1 calc R . . C23 C -0.6226(10) 0.5312(4) 0.4090(3) 0.060(2) Uani 1 1 d . . . H23 H -0.6359 0.4766 0.4052 0.072 Uiso 1 1 calc R . . C24 C -0.6923(11) 0.5676(4) 0.4559(3) 0.0447(14) Uani 1 1 d . . . C25 C -0.6660(13) 0.6488(4) 0.4615(4) 0.063(2) Uani 1 1 d . . . H25 H -0.7091 0.6756 0.4934 0.076 Uiso 1 1 calc R . . C26 C -0.5740(12) 0.6896(5) 0.4185(4) 0.075(3) Uani 1 1 d . . . H26 H -0.5548 0.7439 0.4226 0.090 Uiso 1 1 calc R . . C27 C -0.7871(10) 0.5197(4) 0.5013(3) 0.0521(17) Uani 1 1 d . . . H27A H -0.8182 0.4681 0.4857 0.062 Uiso 1 1 calc R . . H27B H -0.7018 0.5111 0.5324 0.062 Uiso 1 1 calc R . . C28 C -0.9936(9) 0.5644(4) 0.5791(3) 0.0428(15) Uani 1 1 d . . . H28 H -0.9135 0.5521 0.6086 0.051 Uiso 1 1 calc R . . C29 C -1.2312(10) 0.6012(5) 0.5328(3) 0.0656(12) Uani 1 1 d U . . H29 H -1.3477 0.6204 0.5244 0.079 Uiso 1 1 calc R . . N1 N 0.0143(7) 0.7890(3) 0.3334(3) 0.0562(7) Uani 1 1 d U . . N2 N -0.0996(9) 0.6692(4) 0.3106(3) 0.0657(8) Uani 1 1 d U . . N3 N -0.2371(8) 0.7195(4) 0.3276(3) 0.0644(9) Uani 1 1 d U . . N4 N -0.9545(8) 0.5563(4) 0.5240(3) 0.0635(12) Uani 1 1 d U . . N5 N -1.1619(7) 0.5924(3) 0.5862(2) 0.0489(13) Uani 1 1 d . . . N6 N -1.1068(9) 0.5780(4) 0.4939(3) 0.0691(12) Uani 1 1 d U . . O1 O 0.3293(7) 0.8382(3) 0.2421(2) 0.0571(6) Uani 1 1 d U . . O2 O 0.4838(6) 0.9201(3) 0.2941(2) 0.0583(7) Uani 1 1 d U . . O3 O 1.0666(7) 0.8600(3) 0.05059(19) 0.0576(13) Uani 1 1 d . . . O4 O 1.6384(6) 0.8676(3) -0.1037(2) 0.0563(13) Uani 1 1 d . . . O5 O 1.4044(7) 0.9838(3) -0.2035(2) 0.0576(12) Uani 1 1 d . . . O6 O 1.5741(7) 1.0252(3) -0.1322(2) 0.0575(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0341(2) 0.0530(3) 0.0542(3) -0.0084(3) 0.0043(2) -0.0035(2) C1 0.0398(13) 0.0621(14) 0.0578(13) -0.0078(13) 0.0043(13) -0.0016(13) C2 0.037(3) 0.046(4) 0.037(3) 0.006(3) -0.001(3) 0.003(3) C3 0.038(3) 0.054(4) 0.056(4) 0.003(4) 0.000(3) -0.008(3) C4 0.062(4) 0.051(4) 0.048(4) -0.007(3) 0.012(4) -0.001(4) C5 0.039(3) 0.058(4) 0.035(3) 0.000(3) 0.003(3) 0.003(3) C6 0.040(3) 0.065(5) 0.049(4) -0.006(3) 0.004(3) -0.007(3) C7 0.042(4) 0.068(5) 0.046(4) -0.019(3) 0.007(3) 0.000(3) C8 0.045(4) 0.064(5) 0.050(4) 0.000(4) 0.010(3) 0.010(3) C9 0.036(3) 0.047(3) 0.050(4) 0.004(3) 0.011(3) -0.002(3) C10 0.045(4) 0.048(4) 0.046(4) -0.001(3) 0.007(3) -0.003(3) C11 0.053(4) 0.041(3) 0.046(3) 0.000(3) 0.008(4) -0.003(3) C12 0.051(4) 0.032(3) 0.053(4) 0.005(3) 0.016(3) 0.002(3) C13 0.045(4) 0.052(4) 0.052(4) 0.010(3) 0.005(3) 0.005(3) C14 0.058(4) 0.069(5) 0.040(4) 0.011(4) 0.004(4) 0.006(4) C15 0.064(4) 0.055(4) 0.040(4) -0.003(3) 0.017(3) 0.006(4) C16 0.068(5) 0.073(5) 0.065(5) 0.007(4) 0.029(4) 0.015(5) C17 0.042(4) 0.054(4) 0.044(4) 0.001(4) 0.014(3) -0.008(3) C18 0.0432(12) 0.0644(13) 0.0689(13) -0.0072(12) 0.0045(12) -0.0044(12) C19 0.044(4) 0.056(4) 0.071(5) 0.004(4) 0.017(4) -0.003(3) C20 0.0476(17) 0.0722(19) 0.0801(19) 0.0043(18) -0.0019(18) -0.0110(16) C21 0.0458(17) 0.0694(19) 0.0776(19) 0.0037(18) -0.0014(18) -0.0110(16) C22 0.063(5) 0.073(5) 0.062(5) 0.001(4) 0.013(4) -0.013(4) C23 0.072(5) 0.041(4) 0.067(5) 0.003(4) 0.019(4) -0.008(3) C24 0.041(3) 0.051(3) 0.042(3) 0.000(3) -0.001(4) 0.002(3) C25 0.062(5) 0.043(4) 0.085(6) -0.004(4) 0.006(5) -0.002(4) C26 0.073(5) 0.038(4) 0.115(7) 0.011(5) -0.020(6) -0.010(4) C27 0.054(4) 0.047(4) 0.056(4) 0.007(3) 0.010(4) 0.008(3) C28 0.039(3) 0.049(4) 0.041(4) 0.000(3) -0.006(3) -0.002(3) C29 0.048(2) 0.086(3) 0.062(3) 0.006(3) -0.007(2) 0.006(2) N1 0.0410(12) 0.0623(12) 0.0654(13) -0.0067(12) 0.0043(12) -0.0055(11) N2 0.0493(14) 0.0703(15) 0.0776(15) -0.0018(14) 0.0012(14) -0.0088(13) N3 0.0457(17) 0.0697(18) 0.0778(18) 0.0035(18) -0.0006(17) -0.0107(15) N4 0.047(2) 0.084(3) 0.060(3) 0.006(2) -0.005(2) 0.006(2) N5 0.034(3) 0.059(3) 0.053(3) -0.005(3) -0.003(2) 0.003(3) N6 0.053(2) 0.089(3) 0.066(3) 0.005(2) -0.006(2) 0.006(2) O1 0.0426(11) 0.0650(11) 0.0636(11) -0.0068(11) 0.0064(11) -0.0039(10) O2 0.0439(12) 0.0690(13) 0.0620(13) -0.0106(12) 0.0062(12) -0.0034(12) O3 0.046(3) 0.084(4) 0.043(3) 0.007(2) 0.016(2) 0.005(2) O4 0.051(3) 0.063(3) 0.055(3) 0.012(2) 0.017(2) 0.011(2) O5 0.062(3) 0.057(3) 0.054(3) 0.001(2) 0.002(3) -0.004(2) O6 0.055(3) 0.058(3) 0.059(3) -0.003(3) 0.008(3) 0.005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 2.242(6) . ? Cd1 O5 2.263(5) 2_675 ? Cd1 N5 2.284(5) 3_666 ? Cd1 O2 2.293(5) . ? Cd1 O1 2.456(5) . ? Cd1 O6 2.535(5) 2_675 ? Cd1 C17 2.712(7) 2_675 ? Cd1 C1 2.728(7) . ? C1 O1 1.238(8) . ? C1 O2 1.248(8) . ? C1 C2 1.485(9) . ? C2 C7 1.379(9) . ? C2 C3 1.388(9) . ? C3 C4 1.384(9) . ? C3 H3 0.9300 . ? C4 C5 1.371(10) . ? C4 H4 0.9300 . ? C5 C6 1.375(9) . ? C5 C8 1.500(9) . ? C6 C7 1.380(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.416(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.345(9) . ? C9 C14 1.391(10) . ? C9 O3 1.401(8) . ? C10 C11 1.384(9) . ? C10 H10 0.9300 . ? C11 C12 1.391(10) . ? C11 H11 0.9300 . ? C12 C13 1.367(9) . ? C12 O4 1.382(7) . ? C13 C14 1.362(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.406(8) . ? C15 C16 1.527(9) . ? C15 C17 1.532(10) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.240(8) . ? C17 O5 1.254(8) . ? C17 Cd1 2.712(7) 2_674 ? C18 N1 1.364(9) . ? C18 N2 1.381(9) . ? C18 H18 0.9300 . ? C19 N1 1.300(8) . ? C19 N3 1.315(9) . ? C19 H19 0.9300 . ? C20 N3 1.454(9) . ? C20 C21 1.486(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.361(12) . ? C21 C22 1.366(11) . ? C22 C23 1.376(10) . ? C22 H22 0.9300 . ? C23 C24 1.362(9) . ? C23 H23 0.9300 . ? C24 C25 1.389(9) . ? C24 C27 1.507(9) . ? C25 C26 1.395(12) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N4 1.468(9) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N5 1.325(8) . ? C28 N4 1.334(8) . ? C28 H28 0.9300 . ? C29 N6 1.347(9) . ? C29 N5 1.363(9) . ? C29 H29 0.9300 . ? N2 N3 1.372(9) . ? N4 N6 1.368(8) . ? N5 Cd1 2.284(5) 3_366 ? O5 Cd1 2.263(5) 2_674 ? O6 Cd1 2.535(5) 2_674 ? 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 N1 Cd1 O5 123.7(2) . 2_675 ? N1 Cd1 N5 106.5(2) . 3_666 ? O5 Cd1 N5 111.29(19) 2_675 3_666 ? N1 Cd1 O2 134.22(19) . . ? O5 Cd1 O2 91.40(19) 2_675 . ? N5 Cd1 O2 82.49(18) 3_666 . ? N1 Cd1 O1 87.5(2) . . ? O5 Cd1 O1 102.45(18) 2_675 . ? N5 Cd1 O1 125.08(17) 3_666 . ? O2 Cd1 O1 54.02(16) . . ? N1 Cd1 O6 87.16(19) . 2_675 ? O5 Cd1 O6 54.16(17) 2_675 2_675 ? N5 Cd1 O6 89.17(17) 3_666 2_675 ? O2 Cd1 O6 138.48(17) . 2_675 ? O1 Cd1 O6 145.36(16) . 2_675 ? N1 Cd1 C17 108.3(2) . 2_675 ? O5 Cd1 C17 27.34(19) 2_675 2_675 ? N5 Cd1 C17 98.83(19) 3_666 2_675 ? O2 Cd1 C17 114.59(19) . 2_675 ? O1 Cd1 C17 127.27(19) . 2_675 ? O6 Cd1 C17 27.06(18) 2_675 2_675 ? N1 Cd1 C1 111.8(2) . . ? O5 Cd1 C1 97.0(2) 2_675 . ? N5 Cd1 C1 104.9(2) 3_666 . ? O2 Cd1 C1 27.05(18) . . ? O1 Cd1 C1 26.98(18) . . ? O6 Cd1 C1 151.14(19) 2_675 . ? C17 Cd1 C1 124.3(2) 2_675 . ? O1 C1 O2 120.7(6) . . ? O1 C1 C2 120.9(6) . . ? O2 C1 C2 118.3(6) . . ? O1 C1 Cd1 64.1(4) . . ? O2 C1 Cd1 56.7(3) . . ? C2 C1 Cd1 175.0(5) . . ? C7 C2 C3 118.1(6) . . ? C7 C2 C1 120.3(6) . . ? C3 C2 C1 121.6(6) . . ? C4 C3 C2 120.1(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.1(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.1(6) . . ? C4 C5 C8 120.9(6) . . ? C6 C5 C8 119.9(6) . . ? C5 C6 C7 120.1(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 121.5(6) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O3 C8 C5 108.3(6) . . ? O3 C8 H8A 110.0 . . ? C5 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C5 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 C14 120.2(6) . . ? C10 C9 O3 116.2(6) . . ? C14 C9 O3 123.5(6) . . ? C9 C10 C11 120.2(7) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 119.7(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 O4 115.9(6) . . ? C13 C12 C11 119.3(6) . . ? O4 C12 C11 124.8(6) . . ? C14 C13 C12 120.6(7) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C9 119.9(7) . . ? C13 C14 H14 120.1 . . ? C9 C14 H14 120.1 . . ? O4 C15 C16 105.9(6) . . ? O4 C15 C17 112.8(5) . . ? C16 C15 C17 110.4(6) . . ? O4 C15 H15 109.2 . . ? C16 C15 H15 109.2 . . ? C17 C15 H15 109.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 123.6(6) . . ? O6 C17 C15 119.1(7) . . ? O5 C17 C15 117.2(6) . . ? O6 C17 Cd1 68.5(4) . 2_674 ? O5 C17 Cd1 56.0(3) . 2_674 ? C15 C17 Cd1 166.9(5) . 2_674 ? N1 C18 N2 110.0(6) . . ? N1 C18 H18 125.0 . . ? N2 C18 H18 125.0 . . ? N1 C19 N3 112.9(7) . . ? N1 C19 H19 123.6 . . ? N3 C19 H19 123.6 . . ? N3 C20 C21 117.0(8) . . ? N3 C20 H20A 108.0 . . ? C21 C20 H20A 108.0 . . ? N3 C20 H20B 108.0 . . ? C21 C20 H20B 108.0 . . ? H20A C20 H20B 107.3 . . ? C26 C21 C22 117.8(8) . . ? C26 C21 C20 119.5(8) . . ? C22 C21 C20 122.6(8) . . ? C21 C22 C23 120.7(8) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 122.1(7) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.0(7) . . ? C23 C24 C27 120.2(6) . . ? C25 C24 C27 121.7(7) . . ? C24 C25 C26 119.0(8) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 122.3(7) . . ? C21 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N4 C27 C24 114.4(6) . . ? N4 C27 H27A 108.7 . . ? C24 C27 H27A 108.7 . . ? N4 C27 H27B 108.7 . . ? C24 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? N5 C28 N4 110.9(6) . . ? N5 C28 H28 124.5 . . ? N4 C28 H28 124.5 . . ? N6 C29 N5 110.3(6) . . ? N6 C29 H29 124.8 . . ? N5 C29 H29 124.8 . . ? C19 N1 C18 105.0(6) . . ? C19 N1 Cd1 125.9(5) . . ? C18 N1 Cd1 126.1(5) . . ? N3 N2 C18 104.0(6) . . ? C19 N3 N2 108.0(6) . . ? C19 N3 C20 126.7(7) . . ? N2 N3 C20 124.4(7) . . ? C28 N4 N6 107.7(6) . . ? C28 N4 C27 125.1(6) . . ? N6 N4 C27 126.7(6) . . ? C28 N5 C29 105.4(6) . . ? C28 N5 Cd1 124.5(4) . 3_366 ? C29 N5 Cd1 129.5(4) . 3_366 ? C29 N6 N4 105.7(6) . . ? C1 O1 Cd1 88.9(4) . . ? C1 O2 Cd1 96.3(4) . . ? C9 O3 C8 116.6(5) . . ? C12 O4 C15 117.2(5) . . ? C17 O5 Cd1 96.7(4) . 2_674 ? C17 O6 Cd1 84.4(4) . 2_674 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 C1 O1 27.0(5) . . . . ? O5 Cd1 C1 O1 -103.7(4) 2_675 . . . ? N5 Cd1 C1 O1 142.0(4) 3_666 . . . ? O2 Cd1 C1 O1 177.1(7) . . . . ? O6 Cd1 C1 O1 -101.1(5) 2_675 . . . ? C17 Cd1 C1 O1 -106.1(4) 2_675 . . . ? N1 Cd1 C1 O2 -150.1(4) . . . . ? O5 Cd1 C1 O2 79.2(4) 2_675 . . . ? N5 Cd1 C1 O2 -35.1(5) 3_666 . . . ? O1 Cd1 C1 O2 -177.1(7) . . . . ? O6 Cd1 C1 O2 81.8(6) 2_675 . . . ? C17 Cd1 C1 O2 76.9(5) 2_675 . . . ? N1 Cd1 C1 C2 -149(6) . . . . ? O5 Cd1 C1 C2 80(6) 2_675 . . . ? N5 Cd1 C1 C2 -34(6) 3_666 . . . ? O2 Cd1 C1 C2 1(6) . . . . ? O1 Cd1 C1 C2 -176(6) . . . . ? O6 Cd1 C1 C2 83(6) 2_675 . . . ? C17 Cd1 C1 C2 78(6) 2_675 . . . ? O1 C1 C2 C7 178.0(7) . . . . ? O2 C1 C2 C7 -5.2(10) . . . . ? Cd1 C1 C2 C7 -6(6) . . . . ? O1 C1 C2 C3 -3.1(10) . . . . ? O2 C1 C2 C3 173.8(6) . . . . ? Cd1 C1 C2 C3 173(5) . . . . ? C7 C2 C3 C4 1.9(10) . . . . ? C1 C2 C3 C4 -177.1(6) . . . . ? C2 C3 C4 C5 -0.7(11) . . . . ? C3 C4 C5 C6 -0.8(11) . . . . ? C3 C4 C5 C8 176.3(6) . . . . ? C4 C5 C6 C7 1.0(11) . . . . ? C8 C5 C6 C7 -176.2(6) . . . . ? C3 C2 C7 C6 -1.7(10) . . . . ? C1 C2 C7 C6 177.3(6) . . . . ? C5 C6 C7 C2 0.3(11) . . . . ? C4 C5 C8 O3 57.8(9) . . . . ? C6 C5 C8 O3 -125.1(7) . . . . ? C14 C9 C10 C11 -3.2(10) . . . . ? O3 C9 C10 C11 176.7(5) . . . . ? C9 C10 C11 C12 1.1(9) . . . . ? C10 C11 C12 C13 2.0(9) . . . . ? C10 C11 C12 O4 -178.6(6) . . . . ? O4 C12 C13 C14 177.7(6) . . . . ? C11 C12 C13 C14 -2.9(10) . . . . ? C12 C13 C14 C9 0.8(11) . . . . ? C10 C9 C14 C13 2.3(11) . . . . ? O3 C9 C14 C13 -177.5(6) . . . . ? O4 C15 C17 O6 35.1(9) . . . . ? C16 C15 C17 O6 -83.2(8) . . . . ? O4 C15 C17 O5 -143.5(6) . . . . ? C16 C15 C17 O5 98.2(7) . . . . ? O4 C15 C17 Cd1 -88(2) . . . 2_674 ? C16 C15 C17 Cd1 154(2) . . . 2_674 ? N3 C20 C21 C26 87.1(10) . . . . ? N3 C20 C21 C22 -96.3(10) . . . . ? C26 C21 C22 C23 2.6(13) . . . . ? C20 C21 C22 C23 -174.0(7) . . . . ? C21 C22 C23 C24 -0.1(13) . . . . ? C22 C23 C24 C25 -1.9(13) . . . . ? C22 C23 C24 C27 -179.2(7) . . . . ? C23 C24 C25 C26 1.5(13) . . . . ? C27 C24 C25 C26 178.7(7) . . . . ? C22 C21 C26 C25 -3.0(13) . . . . ? C20 C21 C26 C25 173.7(8) . . . . ? C24 C25 C26 C21 1.0(14) . . . . ? C23 C24 C27 N4 -138.2(7) . . . . ? C25 C24 C27 N4 44.6(11) . . . . ? N3 C19 N1 C18 4.2(10) . . . . ? N3 C19 N1 Cd1 165.4(5) . . . . ? N2 C18 N1 C19 -2.8(9) . . . . ? N2 C18 N1 Cd1 -164.0(5) . . . . ? O5 Cd1 N1 C19 -24.9(8) 2_675 . . . ? N5 Cd1 N1 C19 105.9(7) 3_666 . . . ? O2 Cd1 N1 C19 -158.5(6) . . . . ? O1 Cd1 N1 C19 -128.2(7) . . . . ? O6 Cd1 N1 C19 17.6(7) 2_675 . . . ? C17 Cd1 N1 C19 0.4(8) 2_675 . . . ? C1 Cd1 N1 C19 -140.1(7) . . . . ? O5 Cd1 N1 C18 132.4(6) 2_675 . . . ? N5 Cd1 N1 C18 -96.8(6) 3_666 . . . ? O2 Cd1 N1 C18 -1.2(8) . . . . ? O1 Cd1 N1 C18 29.1(6) . . . . ? O6 Cd1 N1 C18 174.9(6) 2_675 . . . ? C17 Cd1 N1 C18 157.7(6) 2_675 . . . ? C1 Cd1 N1 C18 17.3(7) . . . . ? N1 C18 N2 N3 0.6(9) . . . . ? N1 C19 N3 N2 -4.0(10) . . . . ? N1 C19 N3 C20 -173.7(9) . . . . ? C18 N2 N3 C19 1.9(9) . . . . ? C18 N2 N3 C20 172.0(8) . . . . ? C21 C20 N3 C19 -109.2(10) . . . . ? C21 C20 N3 N2 82.6(12) . . . . ? N5 C28 N4 N6 -1.8(8) . . . . ? N5 C28 N4 C27 -173.8(6) . . . . ? C24 C27 N4 C28 -131.5(7) . . . . ? C24 C27 N4 N6 58.0(10) . . . . ? N4 C28 N5 C29 0.8(8) . . . . ? N4 C28 N5 Cd1 172.6(5) . . . 3_366 ? N6 C29 N5 C28 0.6(9) . . . . ? N6 C29 N5 Cd1 -170.7(5) . . . 3_366 ? N5 C29 N6 N4 -1.6(9) . . . . ? C28 N4 N6 C29 2.0(9) . . . . ? C27 N4 N6 C29 173.9(7) . . . . ? O2 C1 O1 Cd1 2.9(7) . . . . ? C2 C1 O1 Cd1 179.6(6) . . . . ? N1 Cd1 O1 C1 -155.1(5) . . . . ? O5 Cd1 O1 C1 80.9(5) 2_675 . . . ? N5 Cd1 O1 C1 -46.6(5) 3_666 . . . ? O2 Cd1 O1 C1 -1.7(4) . . . . ? O6 Cd1 O1 C1 123.6(5) 2_675 . . . ? C17 Cd1 O1 C1 93.7(5) 2_675 . . . ? O1 C1 O2 Cd1 -3.1(8) . . . . ? C2 C1 O2 Cd1 -179.9(5) . . . . ? N1 Cd1 O2 C1 40.2(5) . . . . ? O5 Cd1 O2 C1 -102.8(4) 2_675 . . . ? N5 Cd1 O2 C1 146.0(4) 3_666 . . . ? O1 Cd1 O2 C1 1.6(4) . . . . ? O6 Cd1 O2 C1 -133.9(4) 2_675 . . . ? C17 Cd1 O2 C1 -117.7(4) 2_675 . . . ? C10 C9 O3 C8 -176.3(6) . . . . ? C14 C9 O3 C8 3.5(10) . . . . ? C5 C8 O3 C9 175.4(5) . . . . ? C13 C12 O4 C15 -179.4(6) . . . . ? C11 C12 O4 C15 1.2(9) . . . . ? C16 C15 O4 C12 -177.3(6) . . . . ? C17 C15 O4 C12 61.8(8) . . . . ? O6 C17 O5 Cd1 -11.6(7) . . . 2_674 ? C15 C17 O5 Cd1 167.0(5) . . . 2_674 ? O5 C17 O6 Cd1 10.3(6) . . . 2_674 ? C15 C17 O6 Cd1 -168.3(5) . . . 2_674 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.548 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.075 #=========================END data_Compound-10 _database_code_depnum_ccdc_archive 'CCDC 877940' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 Cd N4 O6' _chemical_formula_sum 'C29 H32 Cd N4 O6' _chemical_formula_weight 644.99 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' _check for _chemical_absolute_configuration rm _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_hall 'p 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.2266(2) _cell_length_b 15.4580(4) _cell_length_c 24.9598(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2788.23(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4393 _cell_measurement_theta_min 2.8130 _cell_measurement_theta_max 29.1682 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8188 _exptl_absorpt_correction_T_max 0.8578 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10637 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4839 _reflns_number_gt 4229 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0350P)^2^+0.0621P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 4839 _refine_ls_number_parameters 361 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.062 _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 Cd1 Cd 0.14581(4) 0.95616(2) 0.309811(11) 0.04340(10) Uani 1 1 d . . . C1 C 1.0454(6) 1.0404(4) 0.74728(14) 0.0443(10) Uani 1 1 d . . . C2 C 0.8691(5) 1.0473(3) 0.71522(12) 0.0356(8) Uani 1 1 d . . . C3 C 0.8365(6) 1.1210(3) 0.68454(14) 0.0419(9) Uani 1 1 d . . . H3 H 0.9237 1.1652 0.6840 0.050 Uiso 1 1 calc R . . C4 C 0.6772(6) 1.1289(3) 0.65500(15) 0.0455(11) Uani 1 1 d . . . H4 H 0.6606 1.1776 0.6336 0.055 Uiso 1 1 calc R . . C5 C 0.5418(6) 1.0667(3) 0.65627(15) 0.0390(11) Uani 1 1 d . . . C6 C 0.5728(6) 0.9930(3) 0.68743(17) 0.0476(10) Uani 1 1 d . . . H6 H 0.4841 0.9495 0.6888 0.057 Uiso 1 1 calc R . . C7 C 0.7355(6) 0.9847(3) 0.71639(16) 0.0465(12) Uani 1 1 d . . . H7 H 0.7542 0.9354 0.7371 0.056 Uiso 1 1 calc R . . C8 C 0.3617(7) 1.0767(3) 0.62746(15) 0.0526(12) Uani 1 1 d . . . H8A H 0.2963 1.0219 0.6270 0.063 Uiso 1 1 calc R . . H8B H 0.2851 1.1188 0.6458 0.063 Uiso 1 1 calc R . . C9 C 0.2433(6) 1.1168(3) 0.54163(16) 0.0441(11) Uani 1 1 d . . . C10 C 0.2794(6) 1.1366(3) 0.48877(16) 0.0469(12) Uani 1 1 d . . . H10 H 0.4008 1.1429 0.4770 0.056 Uiso 1 1 calc R . . C11 C 0.1326(7) 1.1473(3) 0.45300(15) 0.0462(11) Uani 1 1 d . . . H11 H 0.1570 1.1595 0.4172 0.055 Uiso 1 1 calc R . . C12 C -0.0473(6) 1.1400(3) 0.47009(16) 0.0431(11) Uani 1 1 d . . . C13 C -0.0824(7) 1.1225(3) 0.52350(16) 0.0505(12) Uani 1 1 d . . . H13 H -0.2038 1.1191 0.5358 0.061 Uiso 1 1 calc R . . C14 C 0.0626(7) 1.1102(3) 0.55848(17) 0.0508(12) Uani 1 1 d . . . H14 H 0.0379 1.0972 0.5941 0.061 Uiso 1 1 calc R . . C15 C -0.1793(6) 1.1567(3) 0.38225(14) 0.0402(11) Uani 1 1 d . . . H15 H -0.0972 1.2057 0.3748 0.048 Uiso 1 1 calc R . . C16 C -0.3679(7) 1.1753(3) 0.35930(16) 0.0561(12) Uani 1 1 d . . . H16A H -0.4164 1.2271 0.3751 0.084 Uiso 1 1 calc R . . H16B H -0.4493 1.1278 0.3669 0.084 Uiso 1 1 calc R . . H16C H -0.3581 1.1828 0.3212 0.084 Uiso 1 1 calc R . . C17 C -0.0962(6) 1.0746(3) 0.35783(15) 0.0360(10) Uani 1 1 d . . . C18 C -0.1978(6) 0.8291(3) 0.31611(18) 0.0469(11) Uani 1 1 d . . . H18 H -0.2550 0.8683 0.3391 0.056 Uiso 1 1 calc R . . C19 C -0.1506(8) 0.7172(3) 0.26628(16) 0.0499(11) Uani 1 1 d . . . H19 H -0.1658 0.6651 0.2482 0.060 Uiso 1 1 calc R . . C20 C -0.0017(7) 0.7684(3) 0.26508(16) 0.0486(12) Uani 1 1 d . . . H20 H 0.1056 0.7575 0.2457 0.058 Uiso 1 1 calc R . . C21 C -0.4602(7) 0.7265(3) 0.3138(2) 0.0606(13) Uani 1 1 d . . . H21A H -0.5067 0.6889 0.2858 0.073 Uiso 1 1 calc R . . H21B H -0.5425 0.7759 0.3163 0.073 Uiso 1 1 calc R . . C22 C -0.4628(8) 0.6785(4) 0.3660(2) 0.0775(17) Uani 1 1 d . . . H22A H -0.4175 0.6202 0.3602 0.093 Uiso 1 1 calc R . . H22B H -0.3793 0.7068 0.3909 0.093 Uiso 1 1 calc R . . C23 C -0.6514(9) 0.6740(4) 0.3906(2) 0.0739(14) Uani 1 1 d U . . H23A H -0.6888 0.7322 0.4003 0.089 Uiso 1 1 calc R . . H23B H -0.7373 0.6535 0.3636 0.089 Uiso 1 1 calc R . . C24 C -0.6700(9) 0.6198(5) 0.4372(2) 0.1018(18) Uani 1 1 d U . . H24A H -0.5719 0.6343 0.4622 0.122 Uiso 1 1 calc R . . H24B H -0.6519 0.5601 0.4264 0.122 Uiso 1 1 calc R . . C25 C -0.8540(10) 0.6263(5) 0.4665(2) 0.0954(17) Uani 1 1 d U . . H25A H -0.8600 0.6816 0.4848 0.114 Uiso 1 1 calc R . . H25B H -0.9534 0.6247 0.4404 0.114 Uiso 1 1 calc R . . C26 C -0.8833(8) 0.5577(4) 0.5055(2) 0.0850(16) Uani 1 1 d U . . H26A H -0.7762 0.5542 0.5288 0.102 Uiso 1 1 calc R . . H26B H -0.8944 0.5030 0.4867 0.102 Uiso 1 1 calc R . . C27 C -1.0655(7) 0.5539(3) 0.59109(16) 0.0479(11) Uani 1 1 d . . . H27 H -0.9687 0.5344 0.6124 0.057 Uiso 1 1 calc R . . C28 C -1.3291(7) 0.5952(3) 0.56488(17) 0.0584(13) Uani 1 1 d . . . H28 H -1.4537 0.6102 0.5651 0.070 Uiso 1 1 calc R . . C29 C -1.2203(8) 0.5974(4) 0.5221(2) 0.0667(16) Uani 1 1 d . . . H29 H -1.2542 0.6136 0.4876 0.080 Uiso 1 1 calc R . . N1 N -0.0315(5) 0.8395(2) 0.29693(12) 0.0423(9) Uani 1 1 d . . . N2 N -0.2763(5) 0.7564(2) 0.29916(14) 0.0476(10) Uani 1 1 d . . . N3 N -1.0500(6) 0.5714(3) 0.53831(14) 0.0569(12) Uani 1 1 d . . . N4 N -1.2324(5) 0.5678(3) 0.60838(13) 0.0469(10) Uani 1 1 d . . . O1 O 1.1494(5) 1.1036(2) 0.74938(13) 0.0683(9) Uani 1 1 d . . . O2 O 1.0823(5) 0.9723(3) 0.77080(15) 0.0810(12) Uani 1 1 d . . . O3 O 0.3958(4) 1.1045(2) 0.57414(10) 0.0561(9) Uani 1 1 d . . . O4 O -0.2030(4) 1.1486(2) 0.43887(10) 0.0495(8) Uani 1 1 d . . . O5 O 0.0202(4) 1.0849(2) 0.32112(11) 0.0525(8) Uani 1 1 d . . . O6 O -0.1475(5) 1.0036(2) 0.37475(11) 0.0507(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.04210(17) 0.04518(18) 0.04291(15) -0.00008(16) 0.00565(15) -0.00120(18) C1 0.041(3) 0.060(3) 0.0319(19) -0.004(3) 0.0023(18) 0.003(3) C2 0.032(2) 0.046(2) 0.0297(16) -0.0035(19) 0.0044(17) 0.000(3) C3 0.036(2) 0.045(2) 0.044(2) -0.001(2) 0.004(2) -0.009(2) C4 0.045(3) 0.049(3) 0.042(2) 0.010(2) 0.004(2) 0.005(2) C5 0.030(2) 0.050(3) 0.036(2) 0.001(2) 0.0026(18) 0.005(2) C6 0.044(2) 0.048(3) 0.051(2) -0.004(2) -0.005(2) -0.005(2) C7 0.047(3) 0.047(3) 0.045(2) 0.007(2) 0.001(2) 0.004(2) C8 0.043(3) 0.070(3) 0.045(2) 0.002(2) -0.003(2) 0.003(3) C9 0.041(3) 0.053(3) 0.038(2) -0.008(2) -0.001(2) 0.007(2) C10 0.041(3) 0.058(3) 0.042(2) 0.000(2) -0.001(2) -0.005(2) C11 0.054(3) 0.049(3) 0.035(2) -0.0009(19) -0.002(2) 0.000(3) C12 0.047(3) 0.041(3) 0.041(2) -0.011(2) -0.007(2) 0.005(2) C13 0.042(3) 0.067(3) 0.043(2) -0.008(2) 0.002(2) 0.005(3) C14 0.046(3) 0.067(4) 0.039(2) -0.005(2) 0.000(2) 0.001(3) C15 0.043(3) 0.038(3) 0.039(2) 0.0001(18) -0.003(2) 0.000(2) C16 0.060(3) 0.052(3) 0.057(3) -0.001(2) -0.014(3) 0.021(3) C17 0.034(3) 0.041(3) 0.033(2) 0.0021(18) -0.0050(18) -0.0028(19) C18 0.051(3) 0.041(3) 0.050(2) -0.008(2) 0.007(2) -0.005(2) C19 0.069(3) 0.037(3) 0.045(2) -0.0024(19) 0.002(3) 0.001(3) C20 0.054(3) 0.046(3) 0.045(2) -0.004(2) 0.011(2) 0.014(3) C21 0.051(3) 0.062(3) 0.069(3) 0.006(3) 0.000(3) -0.014(3) C22 0.066(4) 0.085(4) 0.081(4) 0.018(3) 0.020(3) -0.011(3) C23 0.063(3) 0.087(3) 0.072(3) 0.009(3) 0.025(3) -0.010(3) C24 0.074(4) 0.131(4) 0.100(3) 0.045(3) 0.025(3) 0.008(4) C25 0.071(3) 0.121(4) 0.094(3) 0.033(3) 0.034(3) 0.005(4) C26 0.066(3) 0.109(4) 0.080(3) 0.022(3) 0.021(3) 0.012(4) C27 0.049(3) 0.048(3) 0.047(2) 0.001(2) -0.008(2) -0.012(3) C28 0.040(3) 0.083(4) 0.052(2) 0.018(2) 0.002(2) 0.006(3) C29 0.050(3) 0.095(5) 0.054(3) 0.022(3) -0.003(3) 0.007(3) N1 0.038(2) 0.042(2) 0.047(2) -0.0022(16) 0.0053(16) -0.0004(17) N2 0.054(2) 0.042(2) 0.047(2) 0.0027(18) 0.0030(18) -0.0110(19) N3 0.042(2) 0.073(3) 0.056(2) 0.012(2) 0.0071(19) 0.004(2) N4 0.039(2) 0.057(3) 0.045(2) 0.0072(17) 0.0012(17) 0.001(2) O1 0.047(2) 0.079(3) 0.079(2) 0.0074(19) -0.018(2) -0.006(2) O2 0.068(3) 0.080(3) 0.095(3) 0.016(2) -0.035(2) 0.004(2) O3 0.041(2) 0.090(3) 0.0372(15) 0.0067(16) -0.0049(13) 0.0045(17) O4 0.0424(19) 0.064(2) 0.0422(16) -0.0083(15) -0.0045(13) 0.0131(16) O5 0.056(2) 0.057(2) 0.0447(17) 0.0090(14) 0.0101(15) 0.0028(16) O6 0.0478(18) 0.0422(18) 0.0622(17) -0.0019(15) 0.0083(19) 0.0024(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.205(3) . ? Cd1 N1 2.235(4) . ? Cd1 N4 2.254(3) 3_666 ? Cd1 O1 2.306(3) 2_674 ? Cd1 O2 2.456(4) 2_674 ? Cd1 C1 2.724(4) 2_674 ? C1 O1 1.233(6) . ? C1 O2 1.235(6) . ? C1 C2 1.508(6) . ? C1 Cd1 2.724(4) 2_675 ? C2 C7 1.368(6) . ? C2 C3 1.392(6) . ? C3 C4 1.373(6) . ? C3 H3 0.9300 . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.397(6) . ? C5 C8 1.495(6) . ? C6 C7 1.386(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.420(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.376(6) . ? C9 C10 1.379(6) . ? C9 O3 1.382(5) . ? C10 C11 1.396(6) . ? C10 H10 0.9300 . ? C11 C12 1.373(7) . ? C11 H11 0.9300 . ? C12 O4 1.375(5) . ? C12 C13 1.384(6) . ? C13 C14 1.377(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O4 1.429(4) . ? C15 C16 1.506(6) . ? C15 C17 1.530(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O6 1.233(5) . ? C17 O5 1.254(5) . ? C18 N1 1.304(5) . ? C18 N2 1.328(5) . ? C18 H18 0.9300 . ? C19 C20 1.336(7) . ? C19 N2 1.366(6) . ? C19 H19 0.9300 . ? C20 N1 1.374(5) . ? C20 H20 0.9300 . ? C21 N2 1.454(6) . ? C21 C22 1.499(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.497(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.440(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.520(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.453(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N3 1.473(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N4 1.299(5) . ? C27 N3 1.349(5) . ? C27 H27 0.9300 . ? C28 C29 1.327(7) . ? C28 N4 1.359(5) . ? C28 H28 0.9300 . ? C29 N3 1.357(6) . ? C29 H29 0.9300 . ? N4 Cd1 2.254(3) 3_366 ? O1 Cd1 2.306(3) 2_675 ? O2 Cd1 2.456(4) 2_675 ? 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 N1 120.69(13) . . ? O5 Cd1 N4 101.15(12) . 3_666 ? N1 Cd1 N4 102.78(13) . 3_666 ? O5 Cd1 O1 135.17(12) . 2_674 ? N1 Cd1 O1 87.17(13) . 2_674 ? N4 Cd1 O1 106.02(15) 3_666 2_674 ? O5 Cd1 O2 88.49(13) . 2_674 ? N1 Cd1 O2 139.90(12) . 2_674 ? N4 Cd1 O2 96.94(14) 3_666 2_674 ? O1 Cd1 O2 53.69(12) 2_674 2_674 ? O5 Cd1 C1 113.15(15) . 2_674 ? N1 Cd1 C1 113.75(15) . 2_674 ? N4 Cd1 C1 101.68(12) 3_666 2_674 ? O1 Cd1 C1 26.78(13) 2_674 2_674 ? O2 Cd1 C1 26.96(14) 2_674 2_674 ? O1 C1 O2 121.6(4) . . ? O1 C1 C2 118.8(5) . . ? O2 C1 C2 119.7(5) . . ? O1 C1 Cd1 57.4(2) . 2_675 ? O2 C1 Cd1 64.4(3) . 2_675 ? C2 C1 Cd1 174.1(4) . 2_675 ? C7 C2 C3 118.1(4) . . ? C7 C2 C1 122.3(4) . . ? C3 C2 C1 119.5(4) . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 121.5(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 118.0(4) . . ? C4 C5 C8 122.5(4) . . ? C6 C5 C8 119.5(4) . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C2 C7 C6 121.4(4) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O3 C8 C5 109.3(4) . . ? O3 C8 H8A 109.8 . . ? C5 C8 H8A 109.8 . . ? O3 C8 H8B 109.8 . . ? C5 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C14 C9 C10 119.2(4) . . ? C14 C9 O3 124.6(4) . . ? C10 C9 O3 116.2(4) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.7(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 O4 126.2(4) . . ? C11 C12 C13 119.3(4) . . ? O4 C12 C13 114.5(4) . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C9 C14 C13 121.2(4) . . ? C9 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? O4 C15 C16 106.5(3) . . ? O4 C15 C17 111.7(3) . . ? C16 C15 C17 111.2(3) . . ? O4 C15 H15 109.1 . . ? C16 C15 H15 109.1 . . ? C17 C15 H15 109.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 124.4(4) . . ? O6 C17 C15 118.9(4) . . ? O5 C17 C15 116.7(4) . . ? N1 C18 N2 112.4(4) . . ? N1 C18 H18 123.8 . . ? N2 C18 H18 123.8 . . ? C20 C19 N2 106.7(4) . . ? C20 C19 H19 126.7 . . ? N2 C19 H19 126.7 . . ? C19 C20 N1 109.6(4) . . ? C19 C20 H20 125.2 . . ? N1 C20 H20 125.2 . . ? N2 C21 C22 112.8(4) . . ? N2 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N2 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 113.0(5) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 116.3(6) . . ? C24 C23 H23A 108.2 . . ? C22 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? C22 C23 H23B 108.2 . . ? H23A C23 H23B 107.4 . . ? C23 C24 C25 115.6(6) . . ? C23 C24 H24A 108.4 . . ? C25 C24 H24A 108.4 . . ? C23 C24 H24B 108.4 . . ? C25 C24 H24B 108.4 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C24 113.6(6) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 N3 112.7(5) . . ? C25 C26 H26A 109.0 . . ? N3 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? N3 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N4 C27 N3 111.6(4) . . ? N4 C27 H27 124.2 . . ? N3 C27 H27 124.2 . . ? C29 C28 N4 110.3(4) . . ? C29 C28 H28 124.9 . . ? N4 C28 H28 124.9 . . ? C28 C29 N3 106.8(4) . . ? C28 C29 H29 126.6 . . ? N3 C29 H29 126.6 . . ? C18 N1 C20 105.0(4) . . ? C18 N1 Cd1 125.1(3) . . ? C20 N1 Cd1 129.7(3) . . ? C18 N2 C19 106.4(4) . . ? C18 N2 C21 125.4(4) . . ? C19 N2 C21 128.1(4) . . ? C27 N3 C29 106.0(4) . . ? C27 N3 C26 125.7(4) . . ? C29 N3 C26 128.2(4) . . ? C27 N4 C28 105.3(4) . . ? C27 N4 Cd1 129.5(3) . 3_366 ? C28 N4 Cd1 125.0(3) . 3_366 ? C1 O1 Cd1 95.8(3) . 2_675 ? C1 O2 Cd1 88.7(3) . 2_675 ? C9 O3 C8 117.0(3) . . ? C12 O4 C15 118.1(3) . . ? C17 O5 Cd1 104.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 -171.4(4) . . . . ? O2 C1 C2 C7 8.4(6) . . . . ? Cd1 C1 C2 C7 -123(3) 2_675 . . . ? O1 C1 C2 C3 6.4(6) . . . . ? O2 C1 C2 C3 -173.7(4) . . . . ? Cd1 C1 C2 C3 54(3) 2_675 . . . ? C7 C2 C3 C4 -2.0(6) . . . . ? C1 C2 C3 C4 -180.0(4) . . . . ? C2 C3 C4 C5 2.6(6) . . . . ? C3 C4 C5 C6 -1.9(6) . . . . ? C3 C4 C5 C8 175.7(4) . . . . ? C4 C5 C6 C7 0.7(6) . . . . ? C8 C5 C6 C7 -177.0(4) . . . . ? C3 C2 C7 C6 0.8(6) . . . . ? C1 C2 C7 C6 178.7(4) . . . . ? C5 C6 C7 C2 -0.2(6) . . . . ? C4 C5 C8 O3 47.8(5) . . . . ? C6 C5 C8 O3 -134.7(4) . . . . ? C14 C9 C10 C11 -1.7(7) . . . . ? O3 C9 C10 C11 178.0(4) . . . . ? C9 C10 C11 C12 1.3(7) . . . . ? C10 C11 C12 O4 -179.7(4) . . . . ? C10 C11 C12 C13 0.5(7) . . . . ? C11 C12 C13 C14 -1.9(7) . . . . ? O4 C12 C13 C14 178.3(4) . . . . ? C10 C9 C14 C13 0.4(8) . . . . ? O3 C9 C14 C13 -179.3(5) . . . . ? C12 C13 C14 C9 1.5(8) . . . . ? O4 C15 C17 O6 39.2(5) . . . . ? C16 C15 C17 O6 -79.7(5) . . . . ? O4 C15 C17 O5 -141.3(3) . . . . ? C16 C15 C17 O5 99.8(4) . . . . ? N2 C19 C20 N1 0.1(5) . . . . ? N2 C21 C22 C23 160.3(5) . . . . ? C21 C22 C23 C24 172.4(6) . . . . ? C22 C23 C24 C25 171.2(6) . . . . ? C23 C24 C25 C26 167.0(6) . . . . ? C24 C25 C26 N3 172.4(6) . . . . ? N4 C28 C29 N3 -0.3(6) . . . . ? N2 C18 N1 C20 0.4(5) . . . . ? N2 C18 N1 Cd1 175.6(3) . . . . ? C19 C20 N1 C18 -0.3(5) . . . . ? C19 C20 N1 Cd1 -175.2(3) . . . . ? O5 Cd1 N1 C18 -30.1(4) . . . . ? N4 Cd1 N1 C18 81.4(4) 3_666 . . . ? O1 Cd1 N1 C18 -172.9(4) 2_674 . . . ? O2 Cd1 N1 C18 -161.2(3) 2_674 . . . ? C1 Cd1 N1 C18 -169.6(3) 2_674 . . . ? O5 Cd1 N1 C20 143.9(3) . . . . ? N4 Cd1 N1 C20 -104.7(3) 3_666 . . . ? O1 Cd1 N1 C20 1.1(4) 2_674 . . . ? O2 Cd1 N1 C20 12.8(4) 2_674 . . . ? C1 Cd1 N1 C20 4.4(4) 2_674 . . . ? N1 C18 N2 C19 -0.3(5) . . . . ? N1 C18 N2 C21 179.5(4) . . . . ? C20 C19 N2 C18 0.1(5) . . . . ? C20 C19 N2 C21 -179.7(4) . . . . ? C22 C21 N2 C18 -84.1(6) . . . . ? C22 C21 N2 C19 95.7(6) . . . . ? N4 C27 N3 C29 -0.4(6) . . . . ? N4 C27 N3 C26 -176.1(5) . . . . ? C28 C29 N3 C27 0.4(6) . . . . ? C28 C29 N3 C26 176.0(5) . . . . ? C25 C26 N3 C27 -141.4(6) . . . . ? C25 C26 N3 C29 43.9(9) . . . . ? N3 C27 N4 C28 0.2(6) . . . . ? N3 C27 N4 Cd1 175.8(3) . . . 3_366 ? C29 C28 N4 C27 0.1(6) . . . . ? C29 C28 N4 Cd1 -175.8(4) . . . 3_366 ? O2 C1 O1 Cd1 -5.0(5) . . . 2_675 ? C2 C1 O1 Cd1 174.8(3) . . . 2_675 ? O1 C1 O2 Cd1 4.7(4) . . . 2_675 ? C2 C1 O2 Cd1 -175.1(3) . . . 2_675 ? C14 C9 O3 C8 5.0(7) . . . . ? C10 C9 O3 C8 -174.7(4) . . . . ? C5 C8 O3 C9 179.8(4) . . . . ? C11 C12 O4 C15 7.4(7) . . . . ? C13 C12 O4 C15 -172.8(4) . . . . ? C16 C15 O4 C12 -173.6(4) . . . . ? C17 C15 O4 C12 64.8(5) . . . . ? O6 C17 O5 Cd1 -12.2(5) . . . . ? C15 C17 O5 Cd1 168.3(3) . . . . ? N1 Cd1 O5 C17 52.0(3) . . . . ? N4 Cd1 O5 C17 -60.3(3) 3_666 . . . ? O1 Cd1 O5 C17 173.0(2) 2_674 . . . ? O2 Cd1 O5 C17 -157.1(3) 2_674 . . . ? C1 Cd1 O5 C17 -168.3(2) 2_674 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.393 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.054 #=========================END