Electronic Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Miao Du' _publ_contact_author_address ; College of Chemistry and Life Science Tianjin Normal University Tianjin 300074 CHINA ; _publ_contact_author_email DUMIAO@PUBLIC.TPT.TJ.CN _publ_section_title ; Direction of unusual mixed-ligand metal-organic frameworks: a new type of 3-D polythreading involving 1-D and 2-D structural motifs and a 2-fold interpenetrating porous network ; loop_ _publ_author_name 'Miao Du' 'Xiu-Juan Jiang' 'Xiao-Jun Zhao' data_1 _database_code_depnum_ccdc_archive 'CCDC 277592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Cu3 N24 O16' _chemical_formula_weight 1708.06 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8387(11) _cell_length_b 11.6113(12) _cell_length_c 28.883(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.010(2) _cell_angle_gamma 90.00 _cell_volume 3590.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2637 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.18 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1750 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.887032 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20237 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6308 _reflns_number_gt 4370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.5094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6308 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.0000 0.03226(16) Uani 1 2 d S . . Cu2 Cu 1.06031(3) 0.74888(3) 0.212591(13) 0.02479(11) Uani 1 1 d . . . O1 O 0.87344(17) 0.73918(18) 0.20265(7) 0.0277(5) Uani 1 1 d . . . O2 O 0.89657(19) 0.9150(2) 0.23160(9) 0.0416(6) Uani 1 1 d . . . O3 O 0.2451(2) 0.9528(2) 0.20765(11) 0.0615(8) Uani 1 1 d . . . O4 O 0.24044(18) 0.7659(2) 0.22470(8) 0.0350(6) Uani 1 1 d . . . O5 O 0.33883(19) 0.47960(19) 0.01990(8) 0.0381(6) Uani 1 1 d . . . O6 O 0.2828(2) 0.5355(2) -0.05340(9) 0.0480(7) Uani 1 1 d . . . O7 O 1.0711(2) 0.5561(2) 0.19138(9) 0.0532(7) Uani 1 1 d . . . H7A H 0.9946 0.5529 0.1791 0.080 Uiso 1 1 d R . . H7B H 1.0825 0.5077 0.2137 0.080 Uiso 1 1 d R . . N1 N 1.0517(2) 0.7102(2) 0.64412(9) 0.0284(6) Uani 1 1 d . . . N2 N 0.8829(3) 0.6334(3) 0.47600(10) 0.0441(8) Uani 1 1 d . . . N3 N 0.8833(3) 0.6374(3) 0.42840(9) 0.0438(8) Uani 1 1 d . . . N4 N 1.0681(2) 0.6886(2) 0.46360(9) 0.0281(6) Uani 1 1 d . . . N5 N 1.1976(2) 0.7113(2) 0.47369(9) 0.0367(7) Uani 1 1 d . . . H5A H 1.2128 0.7782 0.4568 0.044 Uiso 1 1 d R . . H5B H 1.2375 0.6599 0.4557 0.044 Uiso 1 1 d R . . N6 N 1.0568(2) 0.7152(2) 0.28095(9) 0.0268(6) Uani 1 1 d . . . N7 N 0.5106(2) 0.6610(2) 0.02610(10) 0.0349(7) Uani 1 1 d . . . N8 N 0.4599(2) 1.0580(2) 0.10483(9) 0.0326(6) Uani 1 1 d . . . N9 N 0.3462(2) 1.0105(2) 0.11284(11) 0.0410(7) Uani 1 1 d . . . H9A H 0.2841 1.0639 0.1016 0.049 Uiso 1 1 d R . . H9B H 0.3348 1.0112 0.1443 0.049 Uiso 1 1 d R . . N10 N 0.6169(3) 1.1702(3) 0.09761(12) 0.0555(9) Uani 1 1 d . . . N11 N 0.6384(3) 1.0648(3) 0.07910(12) 0.0535(9) Uani 1 1 d . . . N12 N 0.3632(4) 1.4767(3) 0.16075(14) 0.0753(12) Uani 1 1 d . . . C1 C 0.9421(3) 0.6269(3) 0.57424(11) 0.0371(8) Uani 1 1 d . . . H1 H 0.8759 0.5818 0.5601 0.044 Uiso 1 1 calc R . . C2 C 0.9596(3) 0.6455(3) 0.62163(11) 0.0331(8) Uani 1 1 d . . . H2 H 0.9044 0.6112 0.6391 0.040 Uiso 1 1 calc R . . C3 C 1.1315(3) 0.7550(3) 0.61861(11) 0.0371(8) Uani 1 1 d . . . H3 H 1.1973 0.7992 0.6338 0.045 Uiso 1 1 calc R . . C4 C 1.1223(3) 0.7397(3) 0.57120(11) 0.0384(8) Uani 1 1 d . . . H4 H 1.1815 0.7717 0.5550 0.046 Uiso 1 1 calc R . . C5 C 1.0243(3) 0.6762(3) 0.54761(10) 0.0281(7) Uani 1 1 d . . . C6 C 0.9948(3) 0.6647(3) 0.49697(11) 0.0323(8) Uani 1 1 d . . . C7 C 0.9949(3) 0.6700(3) 0.42135(11) 0.0314(8) Uani 1 1 d . . . C8 C 1.0255(3) 0.6856(3) 0.37390(10) 0.0279(7) Uani 1 1 d . . . C9 C 1.1091(3) 0.7657(3) 0.36143(11) 0.0331(8) Uani 1 1 d . . . H9 H 1.1563 0.8110 0.3842 0.040 Uiso 1 1 calc R . . C10 C 1.1213(3) 0.7775(3) 0.31511(11) 0.0334(8) Uani 1 1 d . . . H10 H 1.1776 0.8317 0.3072 0.040 Uiso 1 1 calc R . . C11 C 0.9778(3) 0.6364(3) 0.29287(11) 0.0299(8) Uani 1 1 d . . . H11 H 0.9327 0.5916 0.2694 0.036 Uiso 1 1 calc R . . C12 C 0.9606(3) 0.6189(3) 0.33836(11) 0.0313(8) Uani 1 1 d . . . H12 H 0.9055 0.5625 0.3454 0.038 Uiso 1 1 calc R . . C13 C 0.8295(3) 0.8315(3) 0.21765(11) 0.0274(7) Uani 1 1 d . . . C14 C 0.6916(3) 0.8365(3) 0.21808(11) 0.0275(7) Uani 1 1 d . . . C15 C 0.6336(3) 0.9429(3) 0.21950(12) 0.0358(8) Uani 1 1 d . . . H15 H 0.6803 1.0103 0.2202 0.043 Uiso 1 1 calc R . . C16 C 0.5069(3) 0.9485(3) 0.21980(12) 0.0356(8) Uani 1 1 d . . . H16 H 0.4687 1.0200 0.2206 0.043 Uiso 1 1 calc R . . C17 C 0.4356(3) 0.8498(3) 0.21898(11) 0.0284(7) Uani 1 1 d . . . C18 C 0.2957(3) 0.8591(3) 0.21731(11) 0.0342(8) Uani 1 1 d . . . C19 C 0.4939(3) 0.7438(3) 0.21838(12) 0.0326(8) Uani 1 1 d . . . H19 H 0.4473 0.6766 0.2187 0.039 Uiso 1 1 calc R . . C20 C 0.6206(3) 0.7373(3) 0.21739(12) 0.0334(8) Uani 1 1 d . . . H20 H 0.6586 0.6657 0.2162 0.040 Uiso 1 1 calc R . . C21 C 0.3403(4) 1.2744(4) 0.14556(16) 0.0639(12) Uani 1 1 d . . . H21 H 0.2912 1.2089 0.1460 0.077 Uiso 1 1 calc R . . C22 C 0.2987(4) 1.3814(5) 0.15901(16) 0.0726(14) Uani 1 1 d . . . H22 H 0.2193 1.3850 0.1673 0.087 Uiso 1 1 calc R . . C23 C 0.4767(5) 1.4670(4) 0.14986(18) 0.0763(14) Uani 1 1 d . . . H23 H 0.5271 1.5322 0.1529 0.092 Uiso 1 1 calc R . . C24 C 0.5252(4) 1.3686(3) 0.13458(15) 0.0597(12) Uani 1 1 d . . . H24 H 0.6046 1.3685 0.1262 0.072 Uiso 1 1 calc R . . C25 C 0.4551(3) 1.2685(3) 0.13168(12) 0.0404(9) Uani 1 1 d . . . C26 C 0.5091(3) 1.1664(3) 0.11274(12) 0.0378(8) Uani 1 1 d . . . C27 C 0.5438(3) 0.9983(3) 0.08347(12) 0.0369(8) Uani 1 1 d . . . C28 C 0.5295(3) 0.8806(3) 0.06487(12) 0.0336(8) Uani 1 1 d . . . C29 C 0.5863(3) 0.8532(3) 0.02640(13) 0.0423(9) Uani 1 1 d . . . H29 H 0.6318 0.9086 0.0131 0.051 Uiso 1 1 calc R . . C30 C 0.5750(3) 0.7441(3) 0.00825(13) 0.0398(9) Uani 1 1 d . . . H30 H 0.6136 0.7269 -0.0175 0.048 Uiso 1 1 calc R . . C31 C 0.4585(3) 0.6875(3) 0.06355(13) 0.0413(9) Uani 1 1 d . . . H31 H 0.4144 0.6304 0.0765 0.050 Uiso 1 1 calc R . . C32 C 0.4663(3) 0.7947(3) 0.08399(13) 0.0425(9) Uani 1 1 d . . . H32 H 0.4293 0.8089 0.1104 0.051 Uiso 1 1 calc R . . C33 C 0.2565(3) 0.5047(3) -0.01543(13) 0.0339(8) Uani 1 1 d . . . C34 C 0.1234(3) 0.4995(3) -0.00727(12) 0.0335(8) Uani 1 1 d . . . C35 C 0.0278(3) 0.5209(3) -0.04436(13) 0.0393(9) Uani 1 1 d . . . H35 H 0.0465 0.5340 -0.0743 0.047 Uiso 1 1 calc R . . C36 C 0.0944(3) 0.4771(3) 0.03682(13) 0.0403(9) Uani 1 1 d . . . H36 H 0.1579 0.4606 0.0615 0.048 Uiso 1 1 calc R . . O8 O 0.8001(3) 0.5423(3) 0.14822(12) 0.0940(11) Uani 1 1 d . . . H8A H 0.7546 0.5440 0.1207 0.113 Uiso 1 1 d R . . H8B H 0.8036 0.6091 0.1618 0.113 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0159(3) 0.0375(3) 0.0440(4) -0.0063(3) 0.0067(2) 0.0006(2) Cu2 0.01646(18) 0.0392(2) 0.0193(2) 0.00113(18) 0.00477(14) 0.00038(17) O1 0.0187(10) 0.0375(13) 0.0271(12) -0.0029(10) 0.0045(9) 0.0010(9) O2 0.0240(12) 0.0452(15) 0.0560(17) -0.0136(12) 0.0077(11) -0.0099(11) O3 0.0268(13) 0.0460(17) 0.110(3) 0.0033(16) 0.0058(14) 0.0101(12) O4 0.0194(11) 0.0523(15) 0.0342(13) 0.0091(11) 0.0071(10) -0.0003(11) O5 0.0198(11) 0.0470(15) 0.0476(15) -0.0066(12) 0.0052(11) 0.0003(10) O6 0.0270(12) 0.0697(18) 0.0502(17) 0.0084(14) 0.0154(12) -0.0014(12) O7 0.0713(18) 0.0447(15) 0.0464(16) 0.0059(13) 0.0178(14) 0.0146(13) N1 0.0252(14) 0.0403(16) 0.0201(15) -0.0008(12) 0.0050(12) -0.0001(12) N2 0.0360(17) 0.075(2) 0.0222(16) -0.0013(15) 0.0077(13) -0.0106(15) N3 0.0357(17) 0.075(2) 0.0200(16) -0.0021(15) 0.0034(13) -0.0119(15) N4 0.0277(14) 0.0388(16) 0.0188(14) -0.0014(12) 0.0069(12) -0.0017(12) N5 0.0264(14) 0.0569(19) 0.0284(16) 0.0000(14) 0.0093(12) -0.0034(13) N6 0.0244(13) 0.0369(16) 0.0195(14) 0.0005(12) 0.0050(12) -0.0025(11) N7 0.0215(14) 0.0400(17) 0.0434(18) -0.0012(14) 0.0057(13) 0.0040(12) N8 0.0266(14) 0.0363(16) 0.0357(17) 0.0016(13) 0.0076(13) -0.0027(12) N9 0.0285(14) 0.0417(17) 0.056(2) 0.0013(15) 0.0159(14) 0.0016(13) N10 0.050(2) 0.042(2) 0.081(3) -0.0164(18) 0.0308(18) -0.0153(15) N11 0.0465(19) 0.045(2) 0.077(2) -0.0182(18) 0.0327(18) -0.0120(15) N12 0.094(3) 0.058(3) 0.069(3) -0.022(2) -0.003(2) 0.014(2) C1 0.0374(19) 0.046(2) 0.028(2) -0.0042(17) 0.0068(16) -0.0115(16) C2 0.0363(19) 0.043(2) 0.0208(18) -0.0014(16) 0.0079(15) -0.0094(16) C3 0.0294(17) 0.055(2) 0.0284(19) -0.0057(18) 0.0086(15) -0.0095(17) C4 0.0301(18) 0.061(2) 0.0269(19) 0.0010(18) 0.0126(15) -0.0072(17) C5 0.0298(18) 0.0374(19) 0.0185(17) -0.0003(15) 0.0084(14) 0.0031(15) C6 0.0310(17) 0.042(2) 0.0261(18) 0.0017(16) 0.0096(15) -0.0038(16) C7 0.0328(18) 0.041(2) 0.0198(18) -0.0036(15) 0.0028(15) -0.0030(15) C8 0.0292(17) 0.0370(19) 0.0175(17) 0.0002(15) 0.0037(14) 0.0040(15) C9 0.0318(17) 0.045(2) 0.0218(17) -0.0040(16) 0.0035(14) -0.0101(16) C10 0.0316(18) 0.041(2) 0.0283(19) 0.0022(16) 0.0053(15) -0.0093(15) C11 0.0278(17) 0.0367(19) 0.0262(19) -0.0030(15) 0.0071(14) -0.0024(14) C12 0.0334(18) 0.0364(19) 0.0265(19) 0.0052(15) 0.0119(15) -0.0003(15) C13 0.0230(16) 0.037(2) 0.0224(18) 0.0012(15) 0.0040(14) -0.0025(15) C14 0.0192(16) 0.0353(19) 0.0283(19) 0.0006(15) 0.0048(14) 0.0000(14) C15 0.0255(18) 0.0337(19) 0.048(2) -0.0055(17) 0.0052(16) -0.0050(15) C16 0.0254(17) 0.0300(19) 0.051(2) -0.0025(17) 0.0032(16) 0.0047(15) C17 0.0216(16) 0.037(2) 0.0266(18) 0.0021(15) 0.0051(14) 0.0022(14) C18 0.0218(17) 0.051(2) 0.030(2) 0.0005(17) 0.0053(15) 0.0053(17) C19 0.0233(16) 0.0323(19) 0.043(2) 0.0024(16) 0.0075(15) -0.0046(15) C20 0.0235(16) 0.0334(19) 0.045(2) 0.0004(16) 0.0105(15) 0.0040(14) C21 0.055(3) 0.059(3) 0.081(3) -0.027(2) 0.021(2) -0.002(2) C22 0.056(3) 0.093(4) 0.069(3) -0.033(3) 0.009(2) 0.016(3) C23 0.096(4) 0.047(3) 0.085(4) -0.018(3) 0.012(3) -0.007(3) C24 0.068(3) 0.045(3) 0.069(3) -0.011(2) 0.018(2) -0.010(2) C25 0.042(2) 0.045(2) 0.034(2) -0.0060(17) 0.0048(17) -0.0003(17) C26 0.037(2) 0.038(2) 0.039(2) -0.0062(17) 0.0098(17) -0.0079(16) C27 0.0339(18) 0.040(2) 0.039(2) -0.0037(17) 0.0136(16) -0.0017(16) C28 0.0257(17) 0.0321(19) 0.043(2) 0.0000(16) 0.0055(16) 0.0039(14) C29 0.043(2) 0.039(2) 0.049(2) 0.0009(18) 0.0196(18) -0.0033(17) C30 0.0378(19) 0.040(2) 0.045(2) -0.0002(19) 0.0167(17) 0.0011(17) C31 0.037(2) 0.039(2) 0.052(2) 0.0009(19) 0.0194(18) -0.0027(16) C32 0.042(2) 0.044(2) 0.045(2) -0.0061(18) 0.0216(19) -0.0018(17) C33 0.0222(17) 0.0345(19) 0.047(2) -0.0070(17) 0.0114(17) -0.0020(15) C34 0.0212(16) 0.0340(19) 0.046(2) 0.0011(17) 0.0080(16) -0.0020(14) C35 0.0277(18) 0.051(2) 0.041(2) 0.0065(17) 0.0098(16) -0.0012(16) C36 0.0213(17) 0.054(2) 0.044(2) 0.0061(18) 0.0006(16) -0.0002(16) O8 0.122(3) 0.068(2) 0.085(3) -0.0260(19) -0.007(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.937(2) 3_665 ? Cu1 O5 1.9371(19) . ? Cu1 N7 2.013(3) . ? Cu1 N7 2.013(3) 3_665 ? Cu2 O4 1.939(2) 1_655 ? Cu2 O1 2.0039(19) . ? Cu2 N6 2.019(2) . ? Cu2 N1 2.022(2) 4_575 ? Cu2 O7 2.328(2) . ? O1 C13 1.275(4) . ? O2 C13 1.241(4) . ? O3 C18 1.231(4) . ? O4 C18 1.271(4) . ? O4 Cu2 1.939(2) 1_455 ? O5 C33 1.280(4) . ? O6 C33 1.229(4) . ? O7 H7A 0.8500 . ? O7 H7B 0.8499 . ? N1 C3 1.327(4) . ? N1 C2 1.334(4) . ? N1 Cu2 2.022(2) 4_576 ? N2 C6 1.319(4) . ? N2 N3 1.376(4) . ? N3 C7 1.313(4) . ? N4 C7 1.365(4) . ? N4 C6 1.370(4) . ? N4 N5 1.413(3) . ? N5 H5A 0.9462 . ? N5 H5B 0.9397 . ? N6 C10 1.330(4) . ? N6 C11 1.335(4) . ? N7 C31 1.332(4) . ? N7 C30 1.340(4) . ? N8 C27 1.366(4) . ? N8 C26 1.372(4) . ? N8 N9 1.402(3) . ? N9 H9A 0.9359 . ? N9 H9B 0.9362 . ? N10 C26 1.310(4) . ? N10 N11 1.370(4) . ? N11 C27 1.306(4) . ? N12 C22 1.306(6) . ? N12 C23 1.321(6) . ? C1 C2 1.369(4) . ? C1 C5 1.389(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.369(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 H4 0.9300 . ? C5 C6 1.453(4) . ? C7 C8 1.471(4) . ? C8 C9 1.385(4) . ? C8 C12 1.387(4) . ? C9 C10 1.372(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.371(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.498(4) . ? C14 C20 1.384(4) . ? C14 C15 1.390(4) . ? C15 C16 1.375(4) . ? C15 H15 0.9300 . ? C16 C17 1.380(4) . ? C16 H16 0.9300 . ? C17 C19 1.384(4) . ? C17 C18 1.514(4) . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C25 1.367(5) . ? C21 C22 1.397(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.360(6) . ? C23 H23 0.9300 . ? C24 C25 1.384(5) . ? C24 H24 0.9300 . ? C25 C26 1.466(5) . ? C27 C28 1.468(5) . ? C28 C32 1.374(4) . ? C28 C29 1.389(4) . ? C29 C30 1.369(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.375(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.499(4) . ? C34 C36 1.383(5) . ? C34 C35 1.391(5) . ? C35 C36 1.376(4) 3_565 ? C35 H35 0.9300 . ? C36 C35 1.376(4) 3_565 ? C36 H36 0.9300 . ? O8 H8A 0.8678 . ? O8 H8B 0.8669 . ? 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 Cu1 O5 180.0 3_665 . ? O5 Cu1 N7 89.78(10) 3_665 . ? O5 Cu1 N7 90.22(10) . . ? O5 Cu1 N7 90.22(10) 3_665 3_665 ? O5 Cu1 N7 89.78(10) . 3_665 ? N7 Cu1 N7 180.0 . 3_665 ? O4 Cu2 O1 176.59(9) 1_655 . ? O4 Cu2 N6 90.91(9) 1_655 . ? O1 Cu2 N6 87.47(9) . . ? O4 Cu2 N1 92.48(9) 1_655 4_575 ? O1 Cu2 N1 89.00(9) . 4_575 ? N6 Cu2 N1 175.59(10) . 4_575 ? O4 Cu2 O7 93.15(9) 1_655 . ? O1 Cu2 O7 89.97(9) . . ? N6 Cu2 O7 94.64(9) . . ? N1 Cu2 O7 88.00(10) 4_575 . ? C13 O1 Cu2 109.07(18) . . ? C18 O4 Cu2 123.0(2) . 1_455 ? C33 O5 Cu1 106.5(2) . . ? Cu2 O7 H7A 93.8 . . ? Cu2 O7 H7B 116.4 . . ? H7B O7 H7A 107.7 . . ? C3 N1 C2 117.0(3) . . ? C3 N1 Cu2 121.1(2) . 4_576 ? C2 N1 Cu2 121.7(2) . 4_576 ? C6 N2 N3 107.6(3) . . ? C7 N3 N2 108.2(3) . . ? C7 N4 C6 106.1(3) . . ? C7 N4 N5 129.3(2) . . ? C6 N4 N5 124.0(3) . . ? N4 N5 H5A 107.1 . . ? N4 N5 H5B 107.2 . . ? H5A N5 H5B 95.9 . . ? C10 N6 C11 117.7(3) . . ? C10 N6 Cu2 122.2(2) . . ? C11 N6 Cu2 119.7(2) . . ? C31 N7 C30 117.3(3) . . ? C31 N7 Cu1 120.8(2) . . ? C30 N7 Cu1 121.8(2) . . ? C27 N8 C26 105.8(3) . . ? C27 N8 N9 122.6(3) . . ? C26 N8 N9 131.5(3) . . ? N8 N9 H9A 106.6 . . ? N8 N9 H9B 114.2 . . ? H9A N9 H9B 97.7 . . ? C26 N10 N11 108.4(3) . . ? C27 N11 N10 107.8(3) . . ? C22 N12 C23 115.5(4) . . ? C2 C1 C5 119.2(3) . . ? C2 C1 H1 120.4 . . ? C5 C1 H1 120.4 . . ? N1 C2 C1 123.5(3) . . ? N1 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? N1 C3 C4 123.5(3) . . ? N1 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C1 117.2(3) . . ? C4 C5 C6 125.2(3) . . ? C1 C5 C6 117.4(3) . . ? N2 C6 N4 109.0(3) . . ? N2 C6 C5 121.9(3) . . ? N4 C6 C5 129.0(3) . . ? N3 C7 N4 109.1(3) . . ? N3 C7 C8 121.8(3) . . ? N4 C7 C8 129.0(3) . . ? C9 C8 C12 117.4(3) . . ? C9 C8 C7 125.3(3) . . ? C12 C8 C7 117.3(3) . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N6 C10 C9 123.3(3) . . ? N6 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N6 C11 C12 122.6(3) . . ? N6 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C8 119.8(3) . . ? C11 C12 H12 120.1 . . ? C8 C12 H12 120.1 . . ? O2 C13 O1 122.4(3) . . ? O2 C13 C14 120.1(3) . . ? O1 C13 C14 117.5(3) . . ? C20 C14 C15 119.2(3) . . ? C20 C14 C13 121.3(3) . . ? C15 C14 C13 119.5(3) . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C19 118.9(3) . . ? C16 C17 C18 119.8(3) . . ? C19 C17 C18 121.3(3) . . ? O3 C18 O4 125.8(3) . . ? O3 C18 C17 118.6(3) . . ? O4 C18 C17 115.5(3) . . ? C20 C19 C17 120.4(3) . . ? C20 C19 H19 119.8 . . ? C17 C19 H19 119.8 . . ? C19 C20 C14 120.4(3) . . ? C19 C20 H20 119.8 . . ? C14 C20 H20 119.8 . . ? C25 C21 C22 118.3(4) . . ? C25 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? N12 C22 C21 124.8(4) . . ? N12 C22 H22 117.6 . . ? C21 C22 H22 117.6 . . ? N12 C23 C24 124.8(4) . . ? N12 C23 H23 117.6 . . ? C24 C23 H23 117.6 . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C21 C25 C24 117.2(4) . . ? C21 C25 C26 125.8(3) . . ? C24 C25 C26 117.0(3) . . ? N10 C26 N8 108.6(3) . . ? N10 C26 C25 121.8(3) . . ? N8 C26 C25 129.5(3) . . ? N11 C27 N8 109.4(3) . . ? N11 C27 C28 123.7(3) . . ? N8 C27 C28 126.8(3) . . ? C32 C28 C29 117.8(3) . . ? C32 C28 C27 124.0(3) . . ? C29 C28 C27 118.1(3) . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N7 C30 C29 122.6(3) . . ? N7 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? N7 C31 C32 123.5(3) . . ? N7 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C28 C32 C31 119.1(3) . . ? C28 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? O6 C33 O5 123.2(3) . . ? O6 C33 C34 121.1(3) . . ? O5 C33 C34 115.7(3) . . ? C36 C34 C35 119.6(3) . . ? C36 C34 C33 121.0(3) . . ? C35 C34 C33 119.4(3) . . ? C36 C35 C34 120.0(3) 3_565 . ? C36 C35 H35 120.0 3_565 . ? C34 C35 H35 120.0 . . ? C35 C36 C34 120.4(3) 3_565 . ? C35 C36 H36 119.8 3_565 . ? C34 C36 H36 119.8 . . ? H8A O8 H8B 112.0 . . ? 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 N6 Cu2 O1 C13 76.5(2) . . . . ? N1 Cu2 O1 C13 -100.9(2) 4_575 . . . ? O7 Cu2 O1 C13 171.13(19) . . . . ? N7 Cu1 O5 C33 94.6(2) . . . . ? N7 Cu1 O5 C33 -85.4(2) 3_665 . . . ? C6 N2 N3 C7 0.5(4) . . . . ? O4 Cu2 N6 C10 45.3(2) 1_655 . . . ? O1 Cu2 N6 C10 -131.7(2) . . . . ? O7 Cu2 N6 C10 138.5(2) . . . . ? O4 Cu2 N6 C11 -142.0(2) 1_655 . . . ? O1 Cu2 N6 C11 41.0(2) . . . . ? O7 Cu2 N6 C11 -48.8(2) . . . . ? O5 Cu1 N7 C31 -148.4(3) 3_665 . . . ? O5 Cu1 N7 C31 31.6(3) . . . . ? O5 Cu1 N7 C30 28.3(3) 3_665 . . . ? O5 Cu1 N7 C30 -151.7(3) . . . . ? C26 N10 N11 C27 -0.3(4) . . . . ? C3 N1 C2 C1 -2.1(5) . . . . ? Cu2 N1 C2 C1 172.1(3) 4_576 . . . ? C5 C1 C2 N1 0.8(5) . . . . ? C2 N1 C3 C4 1.2(5) . . . . ? Cu2 N1 C3 C4 -173.1(3) 4_576 . . . ? N1 C3 C4 C5 1.2(5) . . . . ? C3 C4 C5 C1 -2.5(5) . . . . ? C3 C4 C5 C6 172.2(3) . . . . ? C2 C1 C5 C4 1.6(5) . . . . ? C2 C1 C5 C6 -173.6(3) . . . . ? N3 N2 C6 N4 -0.2(4) . . . . ? N3 N2 C6 C5 176.4(3) . . . . ? C7 N4 C6 N2 -0.1(4) . . . . ? N5 N4 C6 N2 -172.1(3) . . . . ? C7 N4 C6 C5 -176.4(3) . . . . ? N5 N4 C6 C5 11.5(5) . . . . ? C4 C5 C6 N2 -159.4(3) . . . . ? C1 C5 C6 N2 15.4(5) . . . . ? C4 C5 C6 N4 16.5(5) . . . . ? C1 C5 C6 N4 -168.7(3) . . . . ? N2 N3 C7 N4 -0.5(4) . . . . ? N2 N3 C7 C8 -178.5(3) . . . . ? C6 N4 C7 N3 0.3(4) . . . . ? N5 N4 C7 N3 171.8(3) . . . . ? C6 N4 C7 C8 178.2(3) . . . . ? N5 N4 C7 C8 -10.3(5) . . . . ? N3 C7 C8 C9 147.5(3) . . . . ? N4 C7 C8 C9 -30.1(5) . . . . ? N3 C7 C8 C12 -28.9(5) . . . . ? N4 C7 C8 C12 153.5(3) . . . . ? C12 C8 C9 C10 1.7(5) . . . . ? C7 C8 C9 C10 -174.7(3) . . . . ? C11 N6 C10 C9 -1.0(5) . . . . ? Cu2 N6 C10 C9 171.8(2) . . . . ? C8 C9 C10 N6 -0.2(5) . . . . ? C10 N6 C11 C12 0.7(4) . . . . ? Cu2 N6 C11 C12 -172.3(2) . . . . ? N6 C11 C12 C8 0.9(5) . . . . ? C9 C8 C12 C11 -2.0(5) . . . . ? C7 C8 C12 C11 174.7(3) . . . . ? Cu2 O1 C13 O2 6.2(4) . . . . ? Cu2 O1 C13 C14 -173.7(2) . . . . ? O2 C13 C14 C20 -159.2(3) . . . . ? O1 C13 C14 C20 20.7(4) . . . . ? O2 C13 C14 C15 20.4(5) . . . . ? O1 C13 C14 C15 -159.7(3) . . . . ? C20 C14 C15 C16 -0.5(5) . . . . ? C13 C14 C15 C16 179.9(3) . . . . ? C14 C15 C16 C17 0.4(5) . . . . ? C15 C16 C17 C19 0.7(5) . . . . ? C15 C16 C17 C18 -177.5(3) . . . . ? Cu2 O4 C18 O3 9.8(5) 1_455 . . . ? Cu2 O4 C18 C17 -167.7(2) 1_455 . . . ? C16 C17 C18 O3 13.8(5) . . . . ? C19 C17 C18 O3 -164.3(3) . . . . ? C16 C17 C18 O4 -168.5(3) . . . . ? C19 C17 C18 O4 13.4(5) . . . . ? C16 C17 C19 C20 -1.7(5) . . . . ? C18 C17 C19 C20 176.5(3) . . . . ? C17 C19 C20 C14 1.5(5) . . . . ? C15 C14 C20 C19 -0.4(5) . . . . ? C13 C14 C20 C19 179.2(3) . . . . ? C23 N12 C22 C21 -1.7(7) . . . . ? C25 C21 C22 N12 -2.2(8) . . . . ? C22 N12 C23 C24 4.3(8) . . . . ? N12 C23 C24 C25 -2.9(8) . . . . ? C22 C21 C25 C24 3.7(6) . . . . ? C22 C21 C25 C26 -174.5(4) . . . . ? C23 C24 C25 C21 -1.4(6) . . . . ? C23 C24 C25 C26 177.0(4) . . . . ? N11 N10 C26 N8 0.8(4) . . . . ? N11 N10 C26 C25 -175.7(3) . . . . ? C27 N8 C26 N10 -0.9(4) . . . . ? N9 N8 C26 N10 -177.5(3) . . . . ? C27 N8 C26 C25 175.3(4) . . . . ? N9 N8 C26 C25 -1.3(6) . . . . ? C21 C25 C26 N10 175.8(4) . . . . ? C24 C25 C26 N10 -2.4(6) . . . . ? C21 C25 C26 N8 0.0(6) . . . . ? C24 C25 C26 N8 -178.1(4) . . . . ? N10 N11 C27 N8 -0.3(4) . . . . ? N10 N11 C27 C28 175.9(3) . . . . ? C26 N8 C27 N11 0.7(4) . . . . ? N9 N8 C27 N11 177.7(3) . . . . ? C26 N8 C27 C28 -175.3(3) . . . . ? N9 N8 C27 C28 1.7(5) . . . . ? N11 C27 C28 C32 151.6(4) . . . . ? N8 C27 C28 C32 -32.9(6) . . . . ? N11 C27 C28 C29 -26.5(5) . . . . ? N8 C27 C28 C29 149.0(3) . . . . ? C32 C28 C29 C30 1.7(5) . . . . ? C27 C28 C29 C30 179.9(3) . . . . ? C31 N7 C30 C29 -1.3(5) . . . . ? Cu1 N7 C30 C29 -178.0(3) . . . . ? C28 C29 C30 N7 0.0(5) . . . . ? C30 N7 C31 C32 0.8(5) . . . . ? Cu1 N7 C31 C32 177.6(3) . . . . ? C29 C28 C32 C31 -2.1(5) . . . . ? C27 C28 C32 C31 179.8(3) . . . . ? N7 C31 C32 C28 0.9(6) . . . . ? Cu1 O5 C33 O6 -0.2(4) . . . . ? Cu1 O5 C33 C34 -177.6(2) . . . . ? O6 C33 C34 C36 -172.9(3) . . . . ? O5 C33 C34 C36 4.6(5) . . . . ? O6 C33 C34 C35 5.2(5) . . . . ? O5 C33 C34 C35 -177.4(3) . . . . ? C36 C34 C35 C36 1.8(6) . . . 3_565 ? C33 C34 C35 C36 -176.3(3) . . . 3_565 ? C35 C34 C36 C35 -1.8(6) . . . 3_565 ? C33 C34 C36 C35 176.2(3) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.362 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.062 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 277593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.50 H44.50 Cd2 N13.50 O12.50' _chemical_formula_weight 1193.24 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1571(16) _cell_length_b 20.483(2) _cell_length_c 16.9026(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.1070(10) _cell_angle_gamma 90.00 _cell_volume 5217.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7928 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.85 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas None _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.857226 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'Apex II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27878 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9139 _reflns_number_gt 7506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.6793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9139 _refine_ls_number_parameters 679 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.003 _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 1.201706(15) 0.125347(12) 0.620515(15) 0.02457(9) Uani 1 1 d . . . Cd2 Cd 0.307391(15) 0.324586(12) 0.389553(15) 0.02727(9) Uani 1 1 d . . . O1 O 1.20024(19) 0.20381(12) 0.72782(16) 0.0434(7) Uani 1 1 d . . . O2 O 1.22097(18) 0.23903(12) 0.60930(15) 0.0388(6) Uani 1 1 d . . . O3 O 1.2942(2) 0.55242(13) 0.76771(16) 0.0474(7) Uani 1 1 d . . . O4 O 1.31141(16) 0.51023(13) 0.88766(14) 0.0362(6) Uani 1 1 d . . . O5 O 1.20441(17) 0.10788(13) 0.48011(15) 0.0370(6) Uani 1 1 d . . . H5C H 1.2322 0.1341 0.4479 0.044 Uiso 1 1 d R . . H5D H 1.2143 0.0655 0.4715 0.044 Uiso 1 1 d R . . O6 O 0.3216(3) 0.45265(17) 0.4185(2) 0.0694(10) Uani 1 1 d . . . O7 O 0.2844(2) 0.40845(14) 0.30268(19) 0.0539(8) Uani 1 1 d . . . O8 O 0.20328(17) 0.70014(14) 0.11176(15) 0.0401(7) Uani 1 1 d . . . O9 O 0.2101(2) 0.75586(12) 0.22304(17) 0.0452(7) Uani 1 1 d . . . O10 O 0.33414(19) 0.30764(15) 0.52304(16) 0.0532(8) Uani 1 1 d . . . H10A H 0.3832 0.3216 0.5527 0.064 Uiso 1 1 d R . . H10B H 0.2930 0.2920 0.5527 0.064 Uiso 1 1 d R . . N1 N 1.04733(18) 0.12507(14) 0.60141(18) 0.0290(7) Uani 1 1 d . . . N2 N 0.73969(18) 0.02789(15) 0.55583(19) 0.0358(7) Uani 1 1 d . . . N3 N 0.64971(18) 0.02813(15) 0.55806(19) 0.0361(7) Uani 1 1 d . . . N4 N 0.70259(17) 0.12054(14) 0.60719(16) 0.0259(6) Uani 1 1 d . . . N5 N 0.70329(19) 0.18508(15) 0.6353(2) 0.0368(7) Uani 1 1 d . . . H5A H 0.7242 0.1858 0.6872 0.044 Uiso 1 1 d R . . H5B H 0.7316 0.2133 0.6060 0.044 Uiso 1 1 d R . . N6 N 0.35739(19) 0.11719(15) 0.6241(2) 0.0367(8) Uani 1 1 d . . . N7 N 0.4624(2) 0.31875(15) 0.3993(2) 0.0387(8) Uani 1 1 d . . . N8 N 0.7750(2) 0.25469(18) 0.4992(2) 0.0491(9) Uani 1 1 d . . . N9 N 0.8658(2) 0.25434(18) 0.4985(2) 0.0516(10) Uani 1 1 d . . . N10 N 0.80981(18) 0.32820(15) 0.41360(19) 0.0312(7) Uani 1 1 d . . . N11 N 0.8080(2) 0.37586(17) 0.3547(2) 0.0428(8) Uani 1 1 d . . . H11A H 0.7776 0.3621 0.3093 0.051 Uiso 1 1 d R . . H11B H 0.7882 0.4138 0.3727 0.051 Uiso 1 1 d R . . N12 N 1.1555(2) 0.32174(16) 0.4040(2) 0.0412(8) Uani 1 1 d . . . C1 C 0.9161(2) 0.07662(17) 0.5351(2) 0.0305(8) Uani 1 1 d . . . H1 H 0.8898 0.0522 0.4926 0.037 Uiso 1 1 calc R . . C2 C 1.0060(2) 0.08985(18) 0.5422(2) 0.0322(8) Uani 1 1 d . . . H2 H 1.0394 0.0733 0.5037 0.039 Uiso 1 1 calc R . . C3 C 0.9976(2) 0.14779(19) 0.6562(2) 0.0346(8) Uani 1 1 d . . . H3 H 1.0254 0.1720 0.6982 0.042 Uiso 1 1 calc R . . C4 C 0.9079(2) 0.13732(19) 0.6539(2) 0.0354(9) Uani 1 1 d . . . H4 H 0.8759 0.1547 0.6930 0.042 Uiso 1 1 calc R . . C5 C 0.8659(2) 0.10053(17) 0.5927(2) 0.0274(7) Uani 1 1 d . . . C6 C 0.7708(2) 0.08351(17) 0.5854(2) 0.0281(7) Uani 1 1 d . . . C7 C 0.6283(2) 0.08412(17) 0.5887(2) 0.0292(8) Uani 1 1 d . . . C8 C 0.5366(2) 0.09940(18) 0.6033(2) 0.0319(8) Uani 1 1 d . . . C9 C 0.5053(3) 0.1581(2) 0.6292(3) 0.0498(11) Uani 1 1 d . . . H9 H 0.5439 0.1930 0.6405 0.060 Uiso 1 1 calc R . . C10 C 0.4168(3) 0.1644(2) 0.6382(3) 0.0500(12) Uani 1 1 d . . . H10 H 0.3972 0.2045 0.6553 0.060 Uiso 1 1 calc R . . C11 C 0.3880(3) 0.0604(2) 0.6006(3) 0.0474(11) Uani 1 1 d . . . H11 H 0.3481 0.0261 0.5908 0.057 Uiso 1 1 calc R . . C12 C 0.4745(2) 0.0497(2) 0.5902(3) 0.0457(10) Uani 1 1 d . . . H12 H 0.4922 0.0087 0.5742 0.055 Uiso 1 1 calc R . . C13 C 1.2177(2) 0.24885(17) 0.6823(2) 0.0302(8) Uani 1 1 d . . . C14 C 1.2374(2) 0.31526(17) 0.7154(2) 0.0313(8) Uani 1 1 d . . . C15 C 1.2315(3) 0.36976(18) 0.6672(2) 0.0431(10) Uani 1 1 d . . . H15 H 1.2136 0.3654 0.6131 0.052 Uiso 1 1 calc R . . C16 C 1.2521(3) 0.43091(18) 0.6987(2) 0.0441(10) Uani 1 1 d . . . H16 H 1.2488 0.4673 0.6656 0.053 Uiso 1 1 calc R . . C17 C 1.2774(2) 0.43824(17) 0.7795(2) 0.0307(8) Uani 1 1 d . . . C18 C 1.2966(2) 0.50442(17) 0.8131(2) 0.0309(8) Uani 1 1 d . . . C19 C 1.2809(3) 0.38406(19) 0.8274(2) 0.0440(10) Uani 1 1 d . . . H19 H 1.2967 0.3884 0.8818 0.053 Uiso 1 1 calc R . . C20 C 1.2610(3) 0.32335(19) 0.7956(2) 0.0454(11) Uani 1 1 d . . . H20 H 1.2637 0.2871 0.8289 0.054 Uiso 1 1 calc R . . C21 C 0.5916(3) 0.2575(2) 0.4447(3) 0.0613(14) Uani 1 1 d . . . H21 H 0.6156 0.2184 0.4649 0.074 Uiso 1 1 calc R . . C22 C 0.5010(3) 0.2646(2) 0.4300(3) 0.0618(14) Uani 1 1 d . . . H22 H 0.4651 0.2300 0.4421 0.074 Uiso 1 1 calc R . . C23 C 0.5152(3) 0.3664(2) 0.3836(3) 0.0584(14) Uani 1 1 d . . . H23 H 0.4895 0.4043 0.3613 0.070 Uiso 1 1 calc R . . C24 C 0.6067(3) 0.3643(2) 0.3977(3) 0.0594(14) Uani 1 1 d . . . H24 H 0.6407 0.4001 0.3859 0.071 Uiso 1 1 calc R . . C25 C 0.6466(2) 0.30865(19) 0.4294(2) 0.0357(9) Uani 1 1 d . . . C26 C 0.7421(2) 0.29895(19) 0.4482(2) 0.0346(8) Uani 1 1 d . . . C27 C 0.8861(2) 0.29844(19) 0.4470(2) 0.0378(9) Uani 1 1 d . . . C28 C 0.9763(2) 0.3101(2) 0.4293(2) 0.0376(9) Uani 1 1 d . . . C29 C 1.0071(3) 0.3612(3) 0.3885(4) 0.086(2) Uani 1 1 d . . . H29 H 0.9681 0.3935 0.3681 0.104 Uiso 1 1 calc R . . C30 C 1.0948(3) 0.3652(3) 0.3772(4) 0.087(2) Uani 1 1 d . . . H30 H 1.1132 0.4007 0.3489 0.105 Uiso 1 1 calc R . . C31 C 1.1264(3) 0.2720(2) 0.4434(3) 0.0523(12) Uani 1 1 d . . . H31 H 1.1670 0.2400 0.4622 0.063 Uiso 1 1 calc R . . C32 C 1.0392(3) 0.2646(2) 0.4583(3) 0.0540(12) Uani 1 1 d . . . H32 H 1.0227 0.2291 0.4877 0.065 Uiso 1 1 calc R . . C33 C 0.2942(3) 0.4572(2) 0.3474(3) 0.0439(10) Uani 1 1 d . . . C34 C 0.2704(3) 0.52255(19) 0.3106(2) 0.0373(9) Uani 1 1 d . . . C35 C 0.2207(3) 0.52450(19) 0.2374(2) 0.0409(9) Uani 1 1 d . . . H35 H 0.1997 0.4856 0.2139 0.049 Uiso 1 1 calc R . . C36 C 0.2013(3) 0.58230(18) 0.1981(2) 0.0373(9) Uani 1 1 d . . . H36 H 0.1682 0.5821 0.1485 0.045 Uiso 1 1 calc R . . C37 C 0.2312(2) 0.64115(18) 0.2324(2) 0.0340(8) Uani 1 1 d . . . C38 C 0.2138(2) 0.70302(18) 0.1864(2) 0.0331(8) Uani 1 1 d . . . C39 C 0.2780(3) 0.6400(2) 0.3075(3) 0.0456(10) Uani 1 1 d . . . H39 H 0.2964 0.6792 0.3318 0.055 Uiso 1 1 calc R . . C40 C 0.2981(3) 0.5814(2) 0.3470(3) 0.0472(10) Uani 1 1 d . . . H40 H 0.3296 0.5814 0.3973 0.057 Uiso 1 1 calc R . . C41 C 0.4811(5) 0.5400(4) 0.2183(6) 0.161(4) Uani 1 1 d D . . H41A H 0.4975 0.5060 0.2561 0.242 Uiso 1 1 calc R . . H41B H 0.5157 0.5361 0.1741 0.242 Uiso 1 1 calc R . . H41C H 0.4193 0.5362 0.1997 0.242 Uiso 1 1 calc R . . C42 C 0.4783(8) 0.6617(6) 0.2080(8) 0.217(6) Uani 1 1 d D . . H42A H 0.4774 0.6987 0.2429 0.325 Uiso 1 1 calc R . . H42B H 0.4216 0.6575 0.1773 0.325 Uiso 1 1 calc R . . H42C H 0.5234 0.6679 0.1730 0.325 Uiso 1 1 calc R . . C43 C 0.5253(5) 0.6169(5) 0.3325(6) 0.158(4) Uani 1 1 d D . . H43 H 0.5373 0.5825 0.3679 0.190 Uiso 1 1 calc R . . N13 N 0.4975(3) 0.6023(3) 0.2555(4) 0.0968(18) Uani 1 1 d D . . O11 O 0.5354(4) 0.6718(3) 0.3580(4) 0.127(2) Uani 1 1 d D . . C44 C 0.9947(12) 0.3342(7) 0.7379(11) 0.186(9) Uani 0.50 1 d PDU A 1 H44A H 1.0090 0.2972 0.7068 0.279 Uiso 0.50 1 d PR A 1 H44B H 0.9399 0.3263 0.7598 0.279 Uiso 0.50 1 d PR A 1 H44C H 1.0412 0.3411 0.7802 0.279 Uiso 0.50 1 d PR A 1 C45 C 0.9325(11) 0.3951(8) 0.6217(8) 0.138(7) Uani 0.50 1 d PDU A 1 H45 H 0.9031 0.3601 0.5956 0.166 Uiso 0.50 1 calc PR A 1 C46 C 1.0228(8) 0.4518(6) 0.7247(9) 0.117(5) Uani 0.50 1 d PDU A 1 H46A H 0.9879 0.4677 0.7647 0.176 Uiso 0.50 1 calc PR A 1 H46B H 1.0214 0.4829 0.6821 0.176 Uiso 0.50 1 calc PR A 1 H46C H 1.0829 0.4455 0.7475 0.176 Uiso 0.50 1 calc PR A 1 N14 N 0.9878(5) 0.3918(4) 0.6950(6) 0.059(2) Uani 0.50 1 d PD A 1 O12 O 0.9304(11) 0.4507(9) 0.5994(11) 0.246(11) Uani 0.50 1 d PD A 1 O13 O 0.7754(4) 0.4768(2) 0.4722(2) 0.1072(15) Uani 1 1 d . B 1 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 0.01901(14) 0.02022(15) 0.03450(16) -0.00052(10) 0.00296(10) -0.00090(9) Cd2 0.02145(14) 0.02602(16) 0.03441(16) 0.00153(10) 0.00339(10) -0.00044(9) O1 0.0610(18) 0.0259(14) 0.0434(16) 0.0002(12) 0.0058(13) -0.0091(13) O2 0.0512(16) 0.0264(14) 0.0394(16) -0.0050(11) 0.0083(12) -0.0047(12) O3 0.076(2) 0.0219(14) 0.0422(16) -0.0008(12) -0.0035(14) -0.0006(13) O4 0.0436(15) 0.0281(15) 0.0371(15) -0.0028(11) 0.0049(12) 0.0001(11) O5 0.0429(15) 0.0316(14) 0.0384(14) 0.0011(11) 0.0127(12) 0.0022(11) O6 0.092(3) 0.052(2) 0.063(2) 0.0208(18) 0.0012(19) 0.0209(18) O7 0.069(2) 0.0272(16) 0.069(2) 0.0087(15) 0.0229(17) 0.0076(14) O8 0.0488(17) 0.0337(15) 0.0379(16) 0.0051(11) 0.0048(13) 0.0037(12) O9 0.0630(18) 0.0235(14) 0.0476(16) -0.0005(12) -0.0009(14) 0.0053(13) O10 0.0486(18) 0.074(2) 0.0367(15) 0.0031(15) 0.0025(13) -0.0202(15) N1 0.0185(14) 0.0311(17) 0.0374(17) -0.0010(13) 0.0027(12) 0.0002(12) N2 0.0213(15) 0.0382(18) 0.0486(19) -0.0088(15) 0.0075(13) -0.0027(13) N3 0.0228(15) 0.0382(18) 0.0480(19) -0.0105(15) 0.0071(13) -0.0030(13) N4 0.0191(14) 0.0267(16) 0.0319(16) -0.0021(12) 0.0032(12) -0.0006(11) N5 0.0274(16) 0.0314(18) 0.0521(19) -0.0084(15) 0.0062(14) -0.0032(13) N6 0.0213(15) 0.0362(19) 0.053(2) -0.0046(15) 0.0039(14) -0.0010(13) N7 0.0251(16) 0.0380(19) 0.053(2) 0.0048(15) 0.0051(14) 0.0000(13) N8 0.0231(16) 0.062(2) 0.063(2) 0.0239(19) 0.0079(15) 0.0006(16) N9 0.0260(17) 0.058(2) 0.070(2) 0.029(2) 0.0051(16) 0.0018(16) N10 0.0198(15) 0.0353(18) 0.0384(17) 0.0057(14) 0.0023(12) 0.0006(12) N11 0.0328(18) 0.051(2) 0.0445(19) 0.0170(17) 0.0022(15) 0.0023(15) N12 0.0224(16) 0.044(2) 0.058(2) 0.0108(16) 0.0079(15) 0.0027(14) C1 0.0236(17) 0.034(2) 0.0341(19) -0.0049(16) 0.0031(14) 0.0006(15) C2 0.0241(18) 0.037(2) 0.037(2) -0.0071(16) 0.0075(15) 0.0004(15) C3 0.0252(18) 0.040(2) 0.039(2) -0.0110(17) 0.0040(16) -0.0019(16) C4 0.0254(18) 0.047(2) 0.035(2) -0.0132(17) 0.0071(15) -0.0007(16) C5 0.0217(17) 0.0290(19) 0.0321(18) 0.0030(15) 0.0053(14) -0.0004(14) C6 0.0206(17) 0.033(2) 0.0303(18) -0.0019(15) 0.0031(14) -0.0010(14) C7 0.0210(17) 0.032(2) 0.0345(19) 0.0012(16) 0.0024(14) -0.0015(14) C8 0.0218(18) 0.035(2) 0.039(2) -0.0014(16) 0.0027(15) 0.0005(15) C9 0.028(2) 0.032(2) 0.089(3) -0.011(2) 0.008(2) -0.0048(17) C10 0.027(2) 0.035(2) 0.088(3) -0.012(2) 0.011(2) -0.0002(17) C11 0.026(2) 0.042(2) 0.076(3) -0.015(2) 0.0138(19) -0.0054(17) C12 0.026(2) 0.041(2) 0.071(3) -0.016(2) 0.0093(19) -0.0021(17) C13 0.0288(18) 0.0214(18) 0.041(2) -0.0031(16) 0.0043(16) -0.0002(14) C14 0.035(2) 0.0222(19) 0.038(2) -0.0019(15) 0.0078(16) -0.0012(15) C15 0.069(3) 0.029(2) 0.031(2) -0.0012(16) 0.0020(19) 0.0000(19) C16 0.073(3) 0.021(2) 0.038(2) 0.0031(16) 0.006(2) -0.0017(18) C17 0.0353(19) 0.0239(19) 0.0332(19) -0.0010(15) 0.0054(15) 0.0005(15) C18 0.0293(18) 0.0253(19) 0.038(2) -0.0015(16) 0.0024(15) 0.0034(14) C19 0.068(3) 0.028(2) 0.034(2) 0.0004(17) -0.002(2) -0.0024(19) C20 0.071(3) 0.024(2) 0.039(2) 0.0050(17) -0.002(2) -0.0044(18) C21 0.032(2) 0.046(3) 0.105(4) 0.029(3) 0.004(2) 0.0010(19) C22 0.026(2) 0.050(3) 0.109(4) 0.026(3) 0.005(2) -0.0033(19) C23 0.028(2) 0.047(3) 0.102(4) 0.028(3) 0.012(2) 0.0077(19) C24 0.030(2) 0.043(3) 0.106(4) 0.024(3) 0.009(2) -0.0021(19) C25 0.0242(18) 0.042(2) 0.041(2) -0.0006(18) 0.0057(16) 0.0004(16) C26 0.0246(18) 0.037(2) 0.043(2) 0.0022(17) 0.0063(16) -0.0011(15) C27 0.0227(18) 0.040(2) 0.051(2) 0.0104(19) 0.0020(16) 0.0023(16) C28 0.0233(18) 0.042(2) 0.046(2) 0.0073(18) 0.0008(16) 0.0035(16) C29 0.029(2) 0.063(3) 0.169(6) 0.068(4) 0.022(3) 0.012(2) C30 0.031(2) 0.068(4) 0.166(6) 0.070(4) 0.024(3) 0.010(2) C31 0.027(2) 0.059(3) 0.071(3) 0.027(2) 0.007(2) 0.0108(19) C32 0.032(2) 0.057(3) 0.074(3) 0.035(2) 0.012(2) 0.0068(19) C33 0.039(2) 0.040(3) 0.055(3) 0.013(2) 0.017(2) 0.0067(18) C34 0.040(2) 0.029(2) 0.045(2) 0.0049(17) 0.0138(17) 0.0050(16) C35 0.052(2) 0.026(2) 0.046(2) 0.0019(17) 0.0112(19) -0.0032(17) C36 0.043(2) 0.029(2) 0.040(2) 0.0013(17) 0.0042(17) 0.0007(16) C37 0.037(2) 0.028(2) 0.037(2) 0.0026(16) 0.0055(16) 0.0044(16) C38 0.0310(19) 0.025(2) 0.043(2) 0.0006(17) 0.0059(16) 0.0014(15) C39 0.059(3) 0.027(2) 0.050(2) -0.0011(18) -0.001(2) 0.0015(18) C40 0.060(3) 0.036(2) 0.044(2) 0.0072(19) -0.002(2) 0.005(2) C41 0.096(6) 0.176(9) 0.221(11) -0.114(8) 0.054(6) -0.039(6) C42 0.177(12) 0.196(13) 0.282(17) 0.100(12) 0.049(11) 0.043(10) C43 0.065(5) 0.214(13) 0.198(12) -0.041(10) 0.025(6) -0.026(6) N13 0.059(3) 0.130(5) 0.101(4) -0.031(4) 0.004(3) -0.016(3) O11 0.118(4) 0.127(5) 0.122(4) -0.022(4) -0.043(3) -0.019(3) C44 0.146(12) 0.197(12) 0.225(13) 0.022(9) 0.060(9) 0.032(9) C45 0.128(10) 0.154(10) 0.143(10) -0.037(8) 0.058(8) -0.017(8) C46 0.066(6) 0.153(9) 0.138(9) -0.045(8) 0.029(7) 0.000(7) N14 0.031(4) 0.054(5) 0.099(7) -0.021(5) 0.042(4) -0.003(3) O12 0.168(14) 0.33(2) 0.27(2) 0.134(19) 0.155(15) 0.081(15) O13 0.161(5) 0.097(3) 0.066(3) -0.007(2) 0.024(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.328(3) . ? Cd1 O2 2.357(3) . ? Cd1 N6 2.360(3) 1_655 ? Cd1 O4 2.369(3) 2_746 ? Cd1 O3 2.404(3) 2_746 ? Cd1 O5 2.405(3) . ? Cd1 O1 2.425(3) . ? Cd1 C18 2.718(4) 2_746 ? Cd1 C13 2.738(3) . ? Cd2 O7 2.263(3) . ? Cd2 O10 2.276(3) . ? Cd2 N7 2.341(3) . ? Cd2 N12 2.341(3) 1_455 ? Cd2 O9 2.359(3) 2_545 ? Cd2 O8 2.554(3) 2_545 ? O1 C13 1.248(4) . ? O2 C13 1.256(4) . ? O3 C18 1.246(4) . ? O3 Cd1 2.404(3) 2_756 ? O4 C18 1.261(4) . ? O4 Cd1 2.369(3) 2_756 ? O5 H5C 0.9001 . ? O5 H5D 0.8951 . ? O6 C33 1.232(6) . ? O7 C33 1.251(5) . ? O8 C38 1.256(4) . ? O8 Cd2 2.554(3) 2 ? O9 C38 1.251(4) . ? O9 Cd2 2.359(3) 2 ? O10 H10A 0.8980 . ? O10 H10B 0.9003 . ? N1 C2 1.335(4) . ? N1 C3 1.338(5) . ? N2 C6 1.312(4) . ? N2 N3 1.368(4) . ? N3 C7 1.314(5) . ? N4 C7 1.360(4) . ? N4 C6 1.364(4) . ? N4 N5 1.404(4) . ? N5 H5A 0.9005 . ? N5 H5B 0.8987 . ? N6 C10 1.326(5) . ? N6 C11 1.329(5) . ? N6 Cd1 2.360(3) 1_455 ? N7 C23 1.307(5) . ? N7 C22 1.333(5) . ? N8 C26 1.312(5) . ? N8 N9 1.378(4) . ? N9 C27 1.314(5) . ? N10 C26 1.372(5) . ? N10 C27 1.374(4) . ? N10 N11 1.393(4) . ? N11 H11A 0.8972 . ? N11 H11B 0.8982 . ? N12 C31 1.319(5) . ? N12 C30 1.324(5) . ? N12 Cd2 2.341(3) 1_655 ? C1 C2 1.381(5) . ? C1 C5 1.387(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C3 H3 0.9300 . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 C6 1.475(4) . ? C7 C8 1.471(5) . ? C8 C9 1.380(5) . ? C8 C12 1.388(5) . ? C9 C10 1.373(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.359(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.489(5) . ? C14 C20 1.374(5) . ? C14 C15 1.380(5) . ? C15 C16 1.384(5) . ? C15 H15 0.9300 . ? C16 C17 1.386(5) . ? C16 H16 0.9300 . ? C17 C19 1.371(5) . ? C17 C18 1.487(5) . ? C18 Cd1 2.718(4) 2_756 ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.376(6) . ? C21 C25 1.382(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.382(6) . ? C23 H23 0.9300 . ? C24 C25 1.372(6) . ? C24 H24 0.9300 . ? C25 C26 1.462(5) . ? C27 C28 1.449(5) . ? C28 C29 1.363(6) . ? C28 C32 1.385(5) . ? C29 C30 1.365(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.380(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.505(5) . ? C34 C35 1.379(6) . ? C34 C40 1.398(6) . ? C35 C36 1.374(5) . ? C35 H35 0.9300 . ? C36 C37 1.392(5) . ? C36 H36 0.9300 . ? C37 C39 1.387(6) . ? C37 C38 1.495(5) . ? C39 C40 1.392(6) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 N13 1.431(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N13 1.470(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O11 1.209(8) . ? C43 N13 1.359(8) . ? C43 H43 0.9300 . ? C44 N14 1.383(9) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O12 1.198(10) . ? C45 N14 1.420(9) . ? C45 H45 0.9300 . ? C46 N14 1.409(8) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O2 97.04(10) . . ? N1 Cd1 N6 172.31(10) . 1_655 ? O2 Cd1 N6 86.55(10) . 1_655 ? N1 Cd1 O4 84.99(9) . 2_746 ? O2 Cd1 O4 171.48(9) . 2_746 ? N6 Cd1 O4 90.49(10) 1_655 2_746 ? N1 Cd1 O3 92.82(10) . 2_746 ? O2 Cd1 O3 133.16(9) . 2_746 ? N6 Cd1 O3 89.62(11) 1_655 2_746 ? O4 Cd1 O3 54.72(9) 2_746 2_746 ? N1 Cd1 O5 89.15(10) . . ? O2 Cd1 O5 93.00(9) . . ? N6 Cd1 O5 83.86(10) 1_655 . ? O4 Cd1 O5 78.73(9) 2_746 . ? O3 Cd1 O5 132.96(9) 2_746 . ? N1 Cd1 O1 90.93(10) . . ? O2 Cd1 O1 54.31(9) . . ? N6 Cd1 O1 96.67(10) 1_655 . ? O4 Cd1 O1 134.09(9) 2_746 . ? O3 Cd1 O1 79.95(9) 2_746 . ? O5 Cd1 O1 147.05(9) . . ? N1 Cd1 C18 91.16(10) . 2_746 ? O2 Cd1 C18 159.67(10) . 2_746 ? N6 Cd1 C18 87.67(11) 1_655 2_746 ? O4 Cd1 C18 27.64(9) 2_746 2_746 ? O3 Cd1 C18 27.27(10) 2_746 2_746 ? O5 Cd1 C18 105.74(10) . 2_746 ? O1 Cd1 C18 107.20(10) . 2_746 ? N1 Cd1 C13 95.85(10) . . ? O2 Cd1 C13 27.25(10) . . ? N6 Cd1 C13 90.45(10) 1_655 . ? O4 Cd1 C13 160.99(10) 2_746 . ? O3 Cd1 C13 106.30(10) 2_746 . ? O5 Cd1 C13 120.24(10) . . ? O1 Cd1 C13 27.12(10) . . ? C18 Cd1 C13 133.49(11) 2_746 . ? O7 Cd2 O10 139.28(11) . . ? O7 Cd2 N7 99.69(11) . . ? O10 Cd2 N7 81.44(11) . . ? O7 Cd2 N12 90.09(11) . 1_455 ? O10 Cd2 N12 88.06(11) . 1_455 ? N7 Cd2 N12 169.13(12) . 1_455 ? O7 Cd2 O9 86.17(11) . 2_545 ? O10 Cd2 O9 134.55(10) . 2_545 ? N7 Cd2 O9 92.99(11) . 2_545 ? N12 Cd2 O9 92.39(11) 1_455 2_545 ? O7 Cd2 O8 138.31(10) . 2_545 ? O10 Cd2 O8 82.00(10) . 2_545 ? N7 Cd2 O8 90.68(10) . 2_545 ? N12 Cd2 O8 85.07(10) 1_455 2_545 ? O9 Cd2 O8 52.84(9) 2_545 2_545 ? C13 O1 Cd1 90.5(2) . . ? C13 O2 Cd1 93.5(2) . . ? C18 O3 Cd1 90.5(2) . 2_756 ? C18 O4 Cd1 91.8(2) . 2_756 ? Cd1 O5 H5C 124.5 . . ? Cd1 O5 H5D 108.9 . . ? H5C O5 H5D 112.6 . . ? C33 O7 Cd2 102.3(3) . . ? C38 O8 Cd2 87.9(2) . 2 ? C38 O9 Cd2 97.1(2) . 2 ? Cd2 O10 H10A 123.7 . . ? Cd2 O10 H10B 123.1 . . ? H10A O10 H10B 112.5 . . ? C2 N1 C3 116.9(3) . . ? C2 N1 Cd1 119.4(2) . . ? C3 N1 Cd1 122.3(2) . . ? C6 N2 N3 107.8(3) . . ? C7 N3 N2 107.7(3) . . ? C7 N4 C6 105.5(3) . . ? C7 N4 N5 124.8(3) . . ? C6 N4 N5 129.5(3) . . ? N4 N5 H5A 109.5 . . ? N4 N5 H5B 113.9 . . ? H5A N5 H5B 112.8 . . ? C10 N6 C11 116.1(3) . . ? C10 N6 Cd1 127.7(3) . 1_455 ? C11 N6 Cd1 115.7(2) . 1_455 ? C23 N7 C22 116.5(3) . . ? C23 N7 Cd2 125.4(3) . . ? C22 N7 Cd2 117.8(3) . . ? C26 N8 N9 107.9(3) . . ? C27 N9 N8 107.9(3) . . ? C26 N10 C27 105.4(3) . . ? C26 N10 N11 130.8(3) . . ? C27 N10 N11 123.8(3) . . ? N10 N11 H11A 111.2 . . ? N10 N11 H11B 110.2 . . ? H11A N11 H11B 113.7 . . ? C31 N12 C30 115.8(4) . . ? C31 N12 Cd2 117.2(2) . 1_655 ? C30 N12 Cd2 127.0(3) . 1_655 ? C2 C1 C5 118.7(3) . . ? C2 C1 H1 120.7 . . ? C5 C1 H1 120.7 . . ? N1 C2 C1 123.4(3) . . ? N1 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? N1 C3 C4 123.7(3) . . ? N1 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C1 118.4(3) . . ? C4 C5 C6 124.0(3) . . ? C1 C5 C6 117.5(3) . . ? N2 C6 N4 109.5(3) . . ? N2 C6 C5 123.1(3) . . ? N4 C6 C5 127.4(3) . . ? N3 C7 N4 109.6(3) . . ? N3 C7 C8 122.0(3) . . ? N4 C7 C8 128.3(3) . . ? C9 C8 C12 116.1(3) . . ? C9 C8 C7 126.9(3) . . ? C12 C8 C7 117.0(3) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N6 C10 C9 124.4(4) . . ? N6 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N6 C11 C12 123.5(4) . . ? N6 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C8 120.6(4) . . ? C11 C12 H12 119.7 . . ? C8 C12 H12 119.7 . . ? O1 C13 O2 121.4(3) . . ? O1 C13 C14 119.4(3) . . ? O2 C13 C14 119.2(3) . . ? O1 C13 Cd1 62.36(19) . . ? O2 C13 Cd1 59.25(18) . . ? C14 C13 Cd1 173.5(2) . . ? C20 C14 C15 118.6(3) . . ? C20 C14 C13 120.1(3) . . ? C15 C14 C13 121.2(3) . . ? C14 C15 C16 120.4(4) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C19 C17 C16 118.9(3) . . ? C19 C17 C18 121.2(3) . . ? C16 C17 C18 119.8(3) . . ? O3 C18 O4 122.1(3) . . ? O3 C18 C17 119.5(3) . . ? O4 C18 C17 118.3(3) . . ? O3 C18 Cd1 62.19(19) . 2_756 ? O4 C18 Cd1 60.60(18) . 2_756 ? C17 C18 Cd1 169.0(3) . 2_756 ? C17 C19 C20 120.5(4) . . ? C17 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C14 C20 C19 121.2(4) . . ? C14 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C25 119.7(4) . . ? C22 C21 H21 120.1 . . ? C25 C21 H21 120.1 . . ? N7 C22 C21 123.2(4) . . ? N7 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N7 C23 C24 124.5(4) . . ? N7 C23 H23 117.7 . . ? C24 C23 H23 117.7 . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C21 116.9(4) . . ? C24 C25 C26 125.7(4) . . ? C21 C25 C26 117.4(4) . . ? N8 C26 N10 109.5(3) . . ? N8 C26 C25 122.3(3) . . ? N10 C26 C25 128.0(3) . . ? N9 C27 N10 109.3(3) . . ? N9 C27 C28 122.8(3) . . ? N10 C27 C28 127.8(3) . . ? C29 C28 C32 115.8(4) . . ? C29 C28 C27 127.8(4) . . ? C32 C28 C27 116.5(4) . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? N12 C30 C29 124.3(4) . . ? N12 C30 H30 117.9 . . ? C29 C30 H30 117.9 . . ? N12 C31 C32 123.6(4) . . ? N12 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C31 C32 C28 120.0(4) . . ? C31 C32 H32 120.0 . . ? C28 C32 H32 120.0 . . ? O6 C33 O7 122.4(4) . . ? O6 C33 C34 120.8(4) . . ? O7 C33 C34 116.9(4) . . ? C35 C34 C40 118.7(4) . . ? C35 C34 C33 118.8(4) . . ? C40 C34 C33 122.5(4) . . ? C36 C35 C34 121.8(4) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C35 C36 C37 120.1(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C39 C37 C36 118.6(3) . . ? C39 C37 C38 122.3(3) . . ? C36 C37 C38 119.1(3) . . ? O9 C38 O8 122.0(3) . . ? O9 C38 C37 119.3(3) . . ? O8 C38 C37 118.6(3) . . ? C37 C39 C40 121.2(4) . . ? C37 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C34 119.5(4) . . ? C39 C40 H40 120.2 . . ? C34 C40 H40 120.2 . . ? N13 C41 H41A 109.5 . . ? N13 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N13 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N13 C42 H42A 109.5 . . ? N13 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N13 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O11 C43 N13 124.2(10) . . ? O11 C43 H43 117.9 . . ? N13 C43 H43 117.9 . . ? C43 N13 C41 129.7(8) . . ? C43 N13 C42 111.3(9) . . ? C41 N13 C42 118.9(9) . . ? N14 C44 H44A 113.3 . . ? N14 C44 H44B 109.1 . . ? H44A C44 H44B 109.5 . . ? N14 C44 H44C 106.0 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O12 C45 N14 108.3(15) . . ? O12 C45 H45 125.9 . . ? N14 C45 H45 125.9 . . ? C44 N14 C46 123.5(11) . . ? C44 N14 C45 120.2(10) . . ? C46 N14 C45 115.7(9) . . ? 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 O1 C13 -101.1(2) . . . . ? O2 Cd1 O1 C13 -3.1(2) . . . . ? N6 Cd1 O1 C13 77.8(2) 1_655 . . . ? O4 Cd1 O1 C13 175.01(19) 2_746 . . . ? O3 Cd1 O1 C13 166.2(2) 2_746 . . . ? O5 Cd1 O1 C13 -11.2(3) . . . . ? C18 Cd1 O1 C13 167.4(2) 2_746 . . . ? N1 Cd1 O2 C13 89.1(2) . . . . ? N6 Cd1 O2 C13 -97.7(2) 1_655 . . . ? O3 Cd1 O2 C13 -11.5(3) 2_746 . . . ? O5 Cd1 O2 C13 178.6(2) . . . . ? O1 Cd1 O2 C13 3.1(2) . . . . ? C18 Cd1 O2 C13 -23.9(4) 2_746 . . . ? O10 Cd2 O7 C33 3.5(3) . . . . ? N7 Cd2 O7 C33 -84.6(3) . . . . ? N12 Cd2 O7 C33 90.7(3) 1_455 . . . ? O9 Cd2 O7 C33 -177.0(3) 2_545 . . . ? O8 Cd2 O7 C33 173.3(2) 2_545 . . . ? O2 Cd1 N1 C2 122.6(3) . . . . ? O4 Cd1 N1 C2 -49.1(3) 2_746 . . . ? O3 Cd1 N1 C2 -103.3(3) 2_746 . . . ? O5 Cd1 N1 C2 29.7(3) . . . . ? O1 Cd1 N1 C2 176.7(3) . . . . ? C18 Cd1 N1 C2 -76.1(3) 2_746 . . . ? C13 Cd1 N1 C2 150.0(3) . . . . ? O2 Cd1 N1 C3 -71.2(3) . . . . ? O4 Cd1 N1 C3 117.1(3) 2_746 . . . ? O3 Cd1 N1 C3 62.9(3) 2_746 . . . ? O5 Cd1 N1 C3 -164.2(3) . . . . ? O1 Cd1 N1 C3 -17.1(3) . . . . ? C18 Cd1 N1 C3 90.1(3) 2_746 . . . ? C13 Cd1 N1 C3 -43.8(3) . . . . ? C6 N2 N3 C7 0.3(4) . . . . ? O7 Cd2 N7 C23 22.8(4) . . . . ? O10 Cd2 N7 C23 -116.0(4) . . . . ? N12 Cd2 N7 C23 -131.0(6) 1_455 . . . ? O9 Cd2 N7 C23 109.4(4) 2_545 . . . ? O8 Cd2 N7 C23 162.2(4) 2_545 . . . ? O7 Cd2 N7 C22 -163.6(4) . . . . ? O10 Cd2 N7 C22 57.6(4) . . . . ? N12 Cd2 N7 C22 42.6(8) 1_455 . . . ? O9 Cd2 N7 C22 -77.0(4) 2_545 . . . ? O8 Cd2 N7 C22 -24.2(4) 2_545 . . . ? C26 N8 N9 C27 -0.1(5) . . . . ? C3 N1 C2 C1 0.4(5) . . . . ? Cd1 N1 C2 C1 167.3(3) . . . . ? C5 C1 C2 N1 -0.6(6) . . . . ? C2 N1 C3 C4 -0.7(6) . . . . ? Cd1 N1 C3 C4 -167.2(3) . . . . ? N1 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 C1 -1.1(6) . . . . ? C3 C4 C5 C6 177.3(3) . . . . ? C2 C1 C5 C4 0.9(5) . . . . ? C2 C1 C5 C6 -177.6(3) . . . . ? N3 N2 C6 N4 0.0(4) . . . . ? N3 N2 C6 C5 179.9(3) . . . . ? C7 N4 C6 N2 -0.2(4) . . . . ? N5 N4 C6 N2 -174.3(3) . . . . ? C7 N4 C6 C5 179.9(3) . . . . ? N5 N4 C6 C5 5.9(6) . . . . ? C4 C5 C6 N2 -145.7(4) . . . . ? C1 C5 C6 N2 32.8(5) . . . . ? C4 C5 C6 N4 34.2(6) . . . . ? C1 C5 C6 N4 -147.3(3) . . . . ? N2 N3 C7 N4 -0.4(4) . . . . ? N2 N3 C7 C8 -177.1(3) . . . . ? C6 N4 C7 N3 0.4(4) . . . . ? N5 N4 C7 N3 174.8(3) . . . . ? C6 N4 C7 C8 176.8(3) . . . . ? N5 N4 C7 C8 -8.8(6) . . . . ? N3 C7 C8 C9 -174.6(4) . . . . ? N4 C7 C8 C9 9.4(6) . . . . ? N3 C7 C8 C12 5.9(5) . . . . ? N4 C7 C8 C12 -170.1(4) . . . . ? C12 C8 C9 C10 -1.8(7) . . . . ? C7 C8 C9 C10 178.6(4) . . . . ? C11 N6 C10 C9 0.7(7) . . . . ? Cd1 N6 C10 C9 -171.1(4) 1_455 . . . ? C8 C9 C10 N6 0.6(8) . . . . ? C10 N6 C11 C12 -0.6(7) . . . . ? Cd1 N6 C11 C12 172.2(4) 1_455 . . . ? N6 C11 C12 C8 -0.7(7) . . . . ? C9 C8 C12 C11 1.9(6) . . . . ? C7 C8 C12 C11 -178.5(4) . . . . ? Cd1 O1 C13 O2 5.5(4) . . . . ? Cd1 O1 C13 C14 -172.9(3) . . . . ? Cd1 O2 C13 O1 -5.6(4) . . . . ? Cd1 O2 C13 C14 172.7(3) . . . . ? N1 Cd1 C13 O1 80.5(2) . . . . ? O2 Cd1 C13 O1 174.6(4) . . . . ? N6 Cd1 C13 O1 -103.9(2) 1_655 . . . ? O4 Cd1 C13 O1 -11.1(4) 2_746 . . . ? O3 Cd1 C13 O1 -14.1(2) 2_746 . . . ? O5 Cd1 C13 O1 173.0(2) . . . . ? C18 Cd1 C13 O1 -16.7(3) 2_746 . . . ? N1 Cd1 C13 O2 -94.0(2) . . . . ? N6 Cd1 C13 O2 81.6(2) 1_655 . . . ? O4 Cd1 C13 O2 174.4(2) 2_746 . . . ? O3 Cd1 C13 O2 171.3(2) 2_746 . . . ? O5 Cd1 C13 O2 -1.6(2) . . . . ? O1 Cd1 C13 O2 -174.6(4) . . . . ? C18 Cd1 C13 O2 168.79(19) 2_746 . . . ? O1 C13 C14 C20 18.4(6) . . . . ? O2 C13 C14 C20 -160.0(4) . . . . ? O1 C13 C14 C15 -160.9(4) . . . . ? O2 C13 C14 C15 20.8(5) . . . . ? C20 C14 C15 C16 2.2(6) . . . . ? C13 C14 C15 C16 -178.5(4) . . . . ? C14 C15 C16 C17 -1.0(7) . . . . ? C15 C16 C17 C19 -0.7(6) . . . . ? C15 C16 C17 C18 -178.1(4) . . . . ? Cd1 O3 C18 O4 -9.5(4) 2_756 . . . ? Cd1 O3 C18 C17 167.6(3) 2_756 . . . ? Cd1 O4 C18 O3 9.6(4) 2_756 . . . ? Cd1 O4 C18 C17 -167.5(3) 2_756 . . . ? C19 C17 C18 O3 178.9(4) . . . . ? C16 C17 C18 O3 -3.7(6) . . . . ? C19 C17 C18 O4 -3.9(5) . . . . ? C16 C17 C18 O4 173.5(4) . . . . ? C19 C17 C18 Cd1 -85.4(14) . . . 2_756 ? C16 C17 C18 Cd1 92.0(14) . . . 2_756 ? C16 C17 C19 C20 1.2(6) . . . . ? C18 C17 C19 C20 178.6(4) . . . . ? C15 C14 C20 C19 -1.7(7) . . . . ? C13 C14 C20 C19 179.0(4) . . . . ? C17 C19 C20 C14 0.0(7) . . . . ? C23 N7 C22 C21 -0.4(8) . . . . ? Cd2 N7 C22 C21 -174.6(4) . . . . ? C25 C21 C22 N7 1.7(9) . . . . ? C22 N7 C23 C24 -0.9(8) . . . . ? Cd2 N7 C23 C24 172.8(4) . . . . ? N7 C23 C24 C25 0.9(9) . . . . ? C23 C24 C25 C21 0.4(7) . . . . ? C23 C24 C25 C26 -179.6(5) . . . . ? C22 C21 C25 C24 -1.6(8) . . . . ? C22 C21 C25 C26 178.3(5) . . . . ? N9 N8 C26 N10 -0.1(5) . . . . ? N9 N8 C26 C25 175.1(4) . . . . ? C27 N10 C26 N8 0.2(4) . . . . ? N11 N10 C26 N8 177.6(4) . . . . ? C27 N10 C26 C25 -174.6(4) . . . . ? N11 N10 C26 C25 2.8(7) . . . . ? C24 C25 C26 N8 158.6(5) . . . . ? C21 C25 C26 N8 -21.3(6) . . . . ? C24 C25 C26 N10 -27.2(7) . . . . ? C21 C25 C26 N10 152.8(4) . . . . ? N8 N9 C27 N10 0.2(5) . . . . ? N8 N9 C27 C28 -178.3(4) . . . . ? C26 N10 C27 N9 -0.2(5) . . . . ? N11 N10 C27 N9 -177.8(4) . . . . ? C26 N10 C27 C28 178.1(4) . . . . ? N11 N10 C27 C28 0.5(7) . . . . ? N9 C27 C28 C29 -167.5(6) . . . . ? N10 C27 C28 C29 14.4(8) . . . . ? N9 C27 C28 C32 11.4(6) . . . . ? N10 C27 C28 C32 -166.7(4) . . . . ? C32 C28 C29 C30 0.7(9) . . . . ? C27 C28 C29 C30 179.6(6) . . . . ? C31 N12 C30 C29 0.4(10) . . . . ? Cd2 N12 C30 C29 -179.2(5) 1_655 . . . ? C28 C29 C30 N12 -0.2(12) . . . . ? C30 N12 C31 C32 -1.2(8) . . . . ? Cd2 N12 C31 C32 178.4(4) 1_655 . . . ? N12 C31 C32 C28 1.8(8) . . . . ? C29 C28 C32 C31 -1.5(8) . . . . ? C27 C28 C32 C31 179.5(4) . . . . ? Cd2 O7 C33 O6 8.3(5) . . . . ? Cd2 O7 C33 C34 -171.4(3) . . . . ? O6 C33 C34 C35 -164.6(4) . . . . ? O7 C33 C34 C35 15.1(6) . . . . ? O6 C33 C34 C40 16.6(6) . . . . ? O7 C33 C34 C40 -163.7(4) . . . . ? C33 C34 C35 C36 -175.9(4) . . . . ? C34 C35 C36 C37 -0.7(6) . . . . ? C35 C36 C37 C39 -2.0(6) . . . . ? C35 C36 C37 C38 176.4(4) . . . . ? Cd2 O9 C38 O8 -4.0(4) 2 . . . ? Cd2 O9 C38 C37 176.0(3) 2 . . . ? Cd2 O8 C38 O9 3.7(4) 2 . . . ? Cd2 O8 C38 C37 -176.3(3) 2 . . . ? C39 C37 C38 O9 -27.1(6) . . . . ? C36 C37 C38 O9 154.5(4) . . . . ? C39 C37 C38 O8 152.9(4) . . . . ? C36 C37 C38 O8 -25.5(5) . . . . ? C36 C37 C39 C40 2.4(6) . . . . ? C38 C37 C39 C40 -176.0(4) . . . . ? C37 C39 C40 C34 -0.1(7) . . . . ? C35 C34 C40 C39 -2.6(6) . . . . ? C33 C34 C40 C39 176.3(4) . . . . ? O11 C43 N13 C41 -178.5(8) . . . . ? O11 C43 N13 C42 -2.1(12) . . . . ? O12 C45 N14 C44 173.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.126 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.092 #===END