# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jyunwu@ncnu.edu.tw _publ_contact_author_name 'Jing-Yun Wu' loop_ _publ_author_name 'Jing-Yun Wu' 'Sheng-Ming Huang' data_cpd1 _database_code_depnum_ccdc_archive 'CCDC 790237' #TrackingRef '- SI_cpd 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H47 Co2 N4 O9.50' _chemical_formula_weight 781.62 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' Co Co 0.3494 0.9721 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.568(2) _cell_length_b 13.363(3) _cell_length_c 13.111(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.40(3) _cell_angle_gamma 90.00 _cell_volume 1711.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4857 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 25.05 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6685 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 '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 11006 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5105 _reflns_number_gt 4456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.5477P] 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 0.02(2) _refine_ls_number_reflns 5105 _refine_ls_number_parameters 457 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Co1 Co 0.35946(6) 0.09851(4) 0.19068(5) 0.0193(2) Uani 1 1 d . . . Co2 Co 0.64647(6) 0.05874(4) 0.31701(5) 0.0199(2) Uani 1 1 d . . . O1 O 0.7410(4) 0.4754(3) -0.1015(3) 0.0244(9) Uani 1 1 d . . . O2 O 0.5220(3) 0.4543(3) -0.1983(3) 0.0206(9) Uani 1 1 d . . . O3 O 0.4291(3) 0.1493(3) 0.0767(3) 0.0222(9) Uani 1 1 d . . . O4 O 0.6487(3) 0.1090(3) 0.1734(2) 0.0218(9) Uani 1 1 d . . . O5 O 0.3563(3) 0.0459(3) 0.3347(3) 0.0215(9) Uani 1 1 d . . . O6 O 0.5760(4) 0.0106(3) 0.4299(3) 0.0229(9) Uani 1 1 d . . . O7 O 0.2559(4) -0.3120(3) 0.6022(3) 0.0253(9) Uani 1 1 d . . . O8 O 0.4772(4) -0.3011(3) 0.6933(3) 0.0227(9) Uani 1 1 d . . . N1 N 0.0444(5) 0.4813(4) 0.2312(3) 0.0240(11) Uani 1 1 d . . . N2 N -0.0540(5) 0.6695(4) 0.2757(3) 0.0230(11) Uani 1 1 d . . . N3 N 0.2229(4) 0.2139(4) 0.1802(3) 0.0217(11) Uani 1 1 d . . . N4 N -0.2226(4) 0.9417(4) 0.3247(3) 0.0205(11) Uani 1 1 d . . . C1 C 0.6509(5) 0.3084(5) -0.1047(4) 0.0208(12) Uani 1 1 d . . . C2 C 0.6310(6) 0.2926(5) 0.0072(4) 0.0260(13) Uani 1 1 d . . . C3 C 0.5957(5) 0.1793(5) -0.0025(4) 0.0224(13) Uani 1 1 d . . . H3 H 0.6769 0.1416 0.0012 0.027 Uiso 1 1 calc R . . C4 C 0.4873(6) 0.1698(5) -0.1187(4) 0.0350(15) Uani 1 1 d . . . H4A H 0.3975 0.1875 -0.1203 0.042 Uiso 1 1 calc R . . H4B H 0.4841 0.1022 -0.1465 0.042 Uiso 1 1 calc R . . C5 C 0.5346(6) 0.2448(5) -0.1869(5) 0.0345(15) Uani 1 1 d . . . H5A H 0.5674 0.2091 -0.2364 0.041 Uiso 1 1 calc R . . H5B H 0.4590 0.2873 -0.2305 0.041 Uiso 1 1 calc R . . C6 C 0.6364(6) 0.4189(5) -0.1370(4) 0.0218(13) Uani 1 1 d . . . C7 C 0.5544(6) 0.1443(5) 0.0886(4) 0.0218(13) Uani 1 1 d . . . C8 C 0.7906(5) 0.2722(4) -0.0988(5) 0.0417(14) Uani 1 1 d . . . H8A H 0.7945 0.2765 -0.1706 0.062 Uiso 1 1 calc R . . H8B H 0.8040 0.2040 -0.0740 0.062 Uiso 1 1 calc R . . H8C H 0.8611 0.3133 -0.0481 0.062 Uiso 1 1 calc R . . C9 C 0.7622(5) 0.3122(5) 0.1084(4) 0.0424(16) Uani 1 1 d . . . H9A H 0.7948 0.3785 0.1041 0.064 Uiso 1 1 calc R . . H9B H 0.8308 0.2642 0.1103 0.064 Uiso 1 1 calc R . . H9C H 0.7433 0.3061 0.1741 0.064 Uiso 1 1 calc R . . C10 C 0.5201(6) 0.3565(5) 0.0131(5) 0.0319(14) Uani 1 1 d . . . H10A H 0.5004 0.3380 0.0763 0.048 Uiso 1 1 calc R . . H10B H 0.4395 0.3479 -0.0526 0.048 Uiso 1 1 calc R . . H10C H 0.5482 0.4253 0.0196 0.048 Uiso 1 1 calc R . . C11 C 0.4175(5) -0.0155(5) 0.5177(4) 0.0209(13) Uani 1 1 d . . . C12 C 0.3536(5) -0.1225(5) 0.4998(4) 0.0224(13) Uani 1 1 d . . . C13 C 0.3604(5) -0.1495(5) 0.6183(4) 0.0211(13) Uani 1 1 d . . . H13 H 0.2782 -0.1226 0.6259 0.025 Uiso 1 1 calc R . . C14 C 0.4866(6) -0.0910(5) 0.6990(4) 0.0262(14) Uani 1 1 d . . . H14A H 0.4600 -0.0494 0.7481 0.031 Uiso 1 1 calc R . . H14B H 0.5569 -0.1373 0.7431 0.031 Uiso 1 1 calc R . . C15 C 0.5399(6) -0.0262(5) 0.6277(4) 0.0288(14) Uani 1 1 d . . . H15A H 0.6161 -0.0585 0.6170 0.035 Uiso 1 1 calc R . . H15B H 0.5695 0.0387 0.6615 0.035 Uiso 1 1 calc R . . C16 C 0.4539(5) 0.0167(5) 0.4193(4) 0.0203(12) Uani 1 1 d . . . C17 C 0.3645(6) -0.2605(5) 0.6391(4) 0.0208(13) Uani 1 1 d . . . C18 C 0.3219(5) 0.0654(4) 0.5339(4) 0.0337(12) Uani 1 1 d . . . H18A H 0.3012 0.0489 0.5971 0.051 Uiso 1 1 calc R . . H18B H 0.2386 0.0681 0.4695 0.051 Uiso 1 1 calc R . . H18C H 0.3665 0.1294 0.5450 0.051 Uiso 1 1 calc R . . C19 C 0.2048(5) -0.1278(5) 0.4160(4) 0.0414(16) Uani 1 1 d . . . H19A H 0.2006 -0.1052 0.3453 0.062 Uiso 1 1 calc R . . H19B H 0.1480 -0.0859 0.4404 0.062 Uiso 1 1 calc R . . H19C H 0.1728 -0.1956 0.4100 0.062 Uiso 1 1 calc R . . C20 C 0.4399(6) -0.1968(5) 0.4631(4) 0.0294(14) Uani 1 1 d . . . H20A H 0.4011 -0.2626 0.4566 0.044 Uiso 1 1 calc R . . H20B H 0.5320 -0.1977 0.5168 0.044 Uiso 1 1 calc R . . H20C H 0.4402 -0.1764 0.3930 0.044 Uiso 1 1 calc R . . C21 C 0.0479(7) 0.5044(5) 0.3402(5) 0.0393(17) Uani 1 1 d . . . H21A H 0.1381 0.5292 0.3856 0.047 Uiso 1 1 calc R . . H21B H 0.0321 0.4436 0.3740 0.047 Uiso 1 1 calc R . . C22 C -0.0563(6) 0.5802(5) 0.3373(5) 0.0376(17) Uani 1 1 d . . . H22A H -0.1463 0.5500 0.3049 0.045 Uiso 1 1 calc R . . H22B H -0.0416 0.5991 0.4123 0.045 Uiso 1 1 calc R . . C23 C -0.0587(6) 0.6434(5) 0.1657(4) 0.0313(14) Uani 1 1 d . . . H23A H -0.0481 0.7037 0.1286 0.038 Uiso 1 1 calc R . . H23B H -0.1475 0.6148 0.1226 0.038 Uiso 1 1 calc R . . C24 C 0.0515(6) 0.5699(6) 0.1706(5) 0.0402(18) Uani 1 1 d . . . H24A H 0.0410 0.5513 0.0962 0.048 Uiso 1 1 calc R . . H24B H 0.1405 0.6010 0.2059 0.048 Uiso 1 1 calc R . . C25 C 0.1766(5) 0.2257(5) 0.2623(4) 0.0255(14) Uani 1 1 d . . . H25 H 0.1844 0.1713 0.3086 0.031 Uiso 1 1 calc R . . C26 C 0.1193(5) 0.3110(5) 0.2831(5) 0.0249(13) Uani 1 1 d . . . H26 H 0.0928 0.3142 0.3430 0.030 Uiso 1 1 calc R . . C27 C 0.1012(5) 0.3934(5) 0.2130(4) 0.0215(13) Uani 1 1 d . . . C28 C 0.1458(5) 0.3810(5) 0.1265(4) 0.0221(13) Uani 1 1 d . . . H28 H 0.1364 0.4333 0.0774 0.026 Uiso 1 1 calc R . . C29 C 0.2032(5) 0.2930(5) 0.1132(4) 0.0245(14) Uani 1 1 d . . . H29 H 0.2304 0.2876 0.0538 0.029 Uiso 1 1 calc R . . C30 C -0.1754(5) 0.9294(5) 0.2441(4) 0.0257(14) Uani 1 1 d . . . H30 H -0.1813 0.9833 0.1976 0.031 Uiso 1 1 calc R . . C31 C -0.1196(6) 0.8431(5) 0.2266(4) 0.0272(14) Uani 1 1 d . . . H31 H -0.0873 0.8402 0.1699 0.033 Uiso 1 1 calc R . . C32 C -0.1091(5) 0.7575(5) 0.2921(4) 0.0197(13) Uani 1 1 d . . . C33 C -0.1541(5) 0.7716(5) 0.3793(4) 0.0221(13) Uani 1 1 d . . . H33 H -0.1458 0.7202 0.4292 0.027 Uiso 1 1 calc R . . C34 C -0.2104(5) 0.8617(4) 0.3903(4) 0.0196(13) Uani 1 1 d . . . H34 H -0.2423 0.8678 0.4470 0.023 Uiso 1 1 calc R . . O9 O -0.0037(5) 0.0202(5) 0.0997(4) 0.0706(18) Uani 1 1 d . . . H101 H -0.0448 0.0485 0.1411 0.106 Uiso 1 1 d R . . H102 H 0.0709 0.0474 0.1021 0.106 Uiso 1 1 d R . . O10 O 0.9885(7) 0.1418(7) 0.3914(6) 0.0303(19) Uani 0.50 1 d P . . H103 H 0.9272 0.1726 0.4066 0.045 Uiso 0.50 1 d PR . . H104 H 0.9515 0.0913 0.3476 0.045 Uiso 0.50 1 d PR . . 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 0.0270(4) 0.0118(5) 0.0213(3) 0.0013(3) 0.0117(3) 0.0034(3) Co2 0.0274(4) 0.0143(5) 0.0219(3) 0.0019(3) 0.0138(3) 0.0048(3) O1 0.026(2) 0.019(2) 0.0284(19) 0.0011(18) 0.0112(16) -0.0016(18) O2 0.024(2) 0.014(2) 0.0239(19) 0.0051(17) 0.0099(16) 0.0034(17) O3 0.029(2) 0.016(2) 0.0251(18) 0.0000(17) 0.0142(15) 0.0024(19) O4 0.0282(18) 0.014(2) 0.0267(16) 0.0042(19) 0.0146(15) 0.005(2) O5 0.0295(19) 0.017(2) 0.0223(16) 0.0045(18) 0.0149(15) 0.003(2) O6 0.029(2) 0.018(2) 0.0270(18) 0.0040(17) 0.0166(16) 0.0050(19) O7 0.028(2) 0.020(2) 0.0280(19) 0.0029(18) 0.0105(16) -0.0021(19) O8 0.031(2) 0.016(2) 0.0234(19) 0.0000(18) 0.0137(17) -0.0059(19) N1 0.028(2) 0.020(3) 0.029(2) 0.005(2) 0.016(2) 0.005(2) N2 0.035(3) 0.014(3) 0.025(2) 0.0025(19) 0.0172(19) 0.007(2) N3 0.023(2) 0.018(3) 0.022(2) 0.000(2) 0.0073(19) 0.003(2) N4 0.022(2) 0.016(3) 0.024(2) 0.002(2) 0.0099(18) 0.002(2) C1 0.028(3) 0.016(3) 0.021(2) 0.002(2) 0.012(2) 0.003(2) C2 0.036(3) 0.017(3) 0.028(3) 0.003(2) 0.016(2) -0.005(2) C3 0.033(3) 0.014(3) 0.027(3) 0.002(2) 0.019(2) 0.002(2) C4 0.055(4) 0.021(4) 0.032(3) -0.003(3) 0.021(3) -0.011(3) C5 0.055(4) 0.024(4) 0.029(3) 0.007(3) 0.021(3) 0.003(3) C6 0.030(3) 0.019(4) 0.022(3) 0.000(3) 0.016(2) -0.003(3) C7 0.042(3) 0.005(3) 0.024(3) 0.002(2) 0.018(2) 0.004(3) C8 0.042(3) 0.026(3) 0.066(4) 0.011(3) 0.030(3) 0.009(2) C9 0.041(3) 0.045(4) 0.032(3) 0.005(3) 0.004(2) -0.014(3) C10 0.049(3) 0.021(3) 0.036(3) -0.004(3) 0.028(3) -0.004(3) C11 0.027(3) 0.017(3) 0.021(2) 0.006(2) 0.011(2) 0.005(2) C12 0.028(3) 0.022(3) 0.019(2) 0.002(2) 0.011(2) 0.002(2) C13 0.029(3) 0.018(3) 0.023(3) 0.003(2) 0.016(2) 0.001(2) C14 0.043(3) 0.019(3) 0.015(2) -0.006(2) 0.009(2) -0.002(3) C15 0.039(3) 0.025(4) 0.019(2) -0.004(2) 0.008(2) -0.005(3) C16 0.030(3) 0.010(3) 0.023(3) -0.004(2) 0.012(2) 0.000(3) C17 0.031(3) 0.017(3) 0.016(2) 0.001(3) 0.010(2) 0.003(3) C18 0.058(3) 0.021(3) 0.036(3) 0.007(2) 0.034(2) 0.009(2) C19 0.035(3) 0.046(4) 0.031(3) 0.009(3) -0.001(2) -0.013(3) C20 0.056(4) 0.015(3) 0.023(3) 0.001(2) 0.022(2) -0.002(3) C21 0.070(4) 0.024(4) 0.032(3) 0.004(3) 0.029(3) 0.018(3) C22 0.065(4) 0.019(5) 0.048(3) 0.009(3) 0.044(3) 0.014(3) C23 0.047(3) 0.020(3) 0.032(3) 0.008(3) 0.021(3) 0.010(3) C24 0.063(4) 0.028(5) 0.041(3) 0.008(3) 0.032(3) 0.015(3) C25 0.034(3) 0.018(4) 0.028(3) 0.004(3) 0.015(2) 0.005(3) C26 0.033(3) 0.015(3) 0.032(3) 0.003(3) 0.018(2) 0.007(3) C27 0.020(3) 0.018(4) 0.026(3) -0.003(2) 0.008(2) 0.002(2) C28 0.025(3) 0.017(3) 0.024(3) 0.008(2) 0.009(2) 0.005(3) C29 0.026(3) 0.028(4) 0.018(3) -0.003(3) 0.007(2) 0.002(3) C30 0.028(3) 0.021(4) 0.033(3) 0.006(3) 0.016(2) 0.006(3) C31 0.032(3) 0.028(4) 0.028(3) 0.004(3) 0.018(2) 0.005(3) C32 0.017(3) 0.015(3) 0.025(3) 0.002(2) 0.005(2) 0.005(2) C33 0.026(3) 0.016(3) 0.024(3) 0.000(2) 0.010(2) 0.000(3) C34 0.018(3) 0.017(4) 0.024(3) -0.001(3) 0.007(2) 0.004(3) O9 0.050(3) 0.094(5) 0.073(3) -0.014(3) 0.028(3) -0.015(3) O10 0.023(4) 0.027(5) 0.047(4) -0.021(4) 0.021(3) -0.014(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 Co1 O3 2.019(4) . ? Co1 O5 2.027(3) . ? Co1 O1 2.063(4) 2_645 ? Co1 N3 2.080(5) . ? Co1 O8 2.257(4) 2_656 ? Co1 O2 2.280(4) 2_645 ? Co1 C6 2.506(6) 2_645 ? Co1 Co2 2.8976(12) . ? Co2 O6 2.000(3) . ? Co2 O4 2.007(3) . ? Co2 N4 2.065(5) 1_645 ? Co2 O7 2.082(4) 2_656 ? Co2 O8 2.259(4) 2_656 ? Co2 O2 2.330(4) 2_645 ? Co2 C17 2.496(6) 2_656 ? O1 C6 1.271(7) . ? O1 Co1 2.063(4) 2_655 ? O2 C6 1.261(6) . ? O2 Co1 2.280(4) 2_655 ? O2 Co2 2.330(4) 2_655 ? O3 C7 1.274(6) . ? O4 C7 1.268(6) . ? O5 C16 1.254(6) . ? O6 C16 1.247(6) . ? O7 C17 1.266(7) . ? O7 Co2 2.082(4) 2_646 ? O8 C17 1.253(6) . ? O8 Co1 2.257(4) 2_646 ? O8 Co2 2.259(4) 2_646 ? N1 C27 1.381(8) . ? N1 C24 1.445(8) . ? N1 C21 1.448(7) . ? N2 C32 1.366(7) . ? N2 C22 1.446(8) . ? N2 C23 1.467(7) . ? N3 C29 1.339(7) . ? N3 C25 1.351(7) . ? N4 C30 1.339(7) . ? N4 C34 1.347(7) . ? N4 Co2 2.065(5) 1_465 ? C1 C8 1.528(7) . ? C1 C6 1.528(8) . ? C1 C5 1.544(9) . ? C1 C2 1.573(7) . ? C2 C10 1.477(9) . ? C2 C9 1.533(7) . ? C2 C3 1.553(8) . ? C3 C7 1.494(7) . ? C3 C4 1.523(7) . ? C4 C5 1.547(8) . ? C6 Co1 2.506(6) 2_655 ? C11 C15 1.533(7) . ? C11 C16 1.542(7) . ? C11 C18 1.549(7) . ? C11 C12 1.560(9) . ? C12 C19 1.540(7) . ? C12 C20 1.544(8) . ? C12 C13 1.569(7) . ? C13 C17 1.507(8) . ? C13 C14 1.560(7) . ? C14 C15 1.531(8) . ? C17 Co2 2.496(6) 2_646 ? C21 C22 1.485(8) . ? C23 C24 1.506(8) . ? C25 C26 1.365(8) . ? C26 C27 1.400(8) . ? C27 C28 1.394(7) . ? C28 C29 1.365(9) . ? C30 C31 1.355(9) . ? C31 C32 1.409(8) . ? C32 C33 1.407(7) . ? C33 C34 1.375(8) . ? 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 O3 Co1 O5 161.16(14) . . ? O3 Co1 O1 95.89(15) . 2_645 ? O5 Co1 O1 93.64(15) . 2_645 ? O3 Co1 N3 98.14(18) . . ? O5 Co1 N3 93.51(16) . . ? O1 Co1 N3 111.07(17) 2_645 . ? O3 Co1 O8 84.16(14) . 2_656 ? O5 Co1 O8 81.85(14) . 2_656 ? O1 Co1 O8 162.28(15) 2_645 2_656 ? N3 Co1 O8 86.38(16) . 2_656 ? O3 Co1 O2 88.12(15) . 2_645 ? O5 Co1 O2 82.52(15) . 2_645 ? O1 Co1 O2 60.40(14) 2_645 2_645 ? N3 Co1 O2 170.10(16) . 2_645 ? O8 Co1 O2 101.94(13) 2_656 2_645 ? O3 Co1 C6 93.64(17) . 2_645 ? O5 Co1 C6 86.43(17) . 2_645 ? O1 Co1 C6 30.37(16) 2_645 2_645 ? N3 Co1 C6 140.99(18) . 2_645 ? O8 Co1 C6 131.92(16) 2_656 2_645 ? O2 Co1 C6 30.08(15) 2_645 2_645 ? O3 Co1 Co2 83.53(10) . . ? O5 Co1 Co2 77.83(10) . . ? O1 Co1 Co2 112.23(11) 2_645 . ? N3 Co1 Co2 136.25(12) . . ? O8 Co1 Co2 50.10(10) 2_656 . ? O2 Co1 Co2 51.84(9) 2_645 . ? C6 Co1 Co2 81.87(13) 2_645 . ? O6 Co2 O4 160.48(14) . . ? O6 Co2 N4 98.74(18) . 1_645 ? O4 Co2 N4 92.98(16) . 1_645 ? O6 Co2 O7 98.17(16) . 2_656 ? O4 Co2 O7 91.09(16) . 2_656 ? N4 Co2 O7 114.24(17) 1_645 2_656 ? O6 Co2 O8 86.60(15) . 2_656 ? O4 Co2 O8 83.10(15) . 2_656 ? N4 Co2 O8 173.11(16) 1_645 2_656 ? O7 Co2 O8 60.38(14) 2_656 2_656 ? O6 Co2 O2 84.06(14) . 2_645 ? O4 Co2 O2 81.55(14) . 2_645 ? N4 Co2 O2 84.60(15) 1_645 2_645 ? O7 Co2 O2 160.23(15) 2_656 2_645 ? O8 Co2 O2 100.35(13) 2_656 2_645 ? O6 Co2 C17 94.43(17) . 2_656 ? O4 Co2 C17 84.87(17) . 2_656 ? N4 Co2 C17 144.20(18) 1_645 2_656 ? O7 Co2 C17 30.44(15) 2_656 2_656 ? O8 Co2 C17 30.03(15) 2_656 2_656 ? O2 Co2 C17 130.00(16) 2_645 2_656 ? O6 Co2 Co1 83.00(10) . . ? O4 Co2 Co1 77.67(9) . . ? N4 Co2 Co1 134.63(12) 1_645 . ? O7 Co2 Co1 110.28(11) 2_656 . ? O8 Co2 Co1 50.06(10) 2_656 . ? O2 Co2 Co1 50.28(10) 2_645 . ? C17 Co2 Co1 79.84(13) 2_656 . ? C6 O1 Co1 94.5(3) . 2_655 ? C6 O2 Co1 84.9(3) . 2_655 ? C6 O2 Co2 162.4(4) . 2_655 ? Co1 O2 Co2 77.88(13) 2_655 2_655 ? C7 O3 Co1 123.1(3) . . ? C7 O4 Co2 131.4(3) . . ? C16 O5 Co1 129.2(3) . . ? C16 O6 Co2 123.9(4) . . ? C17 O7 Co2 93.1(3) . 2_646 ? C17 O8 Co1 163.0(4) . 2_646 ? C17 O8 Co2 85.5(3) . 2_646 ? Co1 O8 Co2 79.83(14) 2_646 2_646 ? C27 N1 C24 119.0(4) . . ? C27 N1 C21 120.2(5) . . ? C24 N1 C21 112.4(5) . . ? C32 N2 C22 121.6(4) . . ? C32 N2 C23 120.2(5) . . ? C22 N2 C23 110.6(5) . . ? C29 N3 C25 114.7(5) . . ? C29 N3 Co1 124.0(4) . . ? C25 N3 Co1 119.2(4) . . ? C30 N4 C34 115.6(5) . . ? C30 N4 Co2 119.9(4) . 1_465 ? C34 N4 Co2 122.1(4) . 1_465 ? C8 C1 C6 108.2(5) . . ? C8 C1 C5 110.9(5) . . ? C6 C1 C5 111.7(5) . . ? C8 C1 C2 112.3(4) . . ? C6 C1 C2 110.7(5) . . ? C5 C1 C2 102.9(5) . . ? C10 C2 C9 109.2(5) . . ? C10 C2 C3 113.4(5) . . ? C9 C2 C3 110.3(5) . . ? C10 C2 C1 111.2(5) . . ? C9 C2 C1 112.7(4) . . ? C3 C2 C1 99.7(5) . . ? C7 C3 C4 115.9(5) . . ? C7 C3 C2 112.0(5) . . ? C4 C3 C2 103.2(5) . . ? C3 C4 C5 103.8(5) . . ? C1 C5 C4 107.4(4) . . ? O2 C6 O1 120.0(6) . . ? O2 C6 C1 120.6(5) . . ? O1 C6 C1 119.4(5) . . ? O2 C6 Co1 65.0(3) . 2_655 ? O1 C6 Co1 55.2(3) . 2_655 ? C1 C6 Co1 173.2(4) . 2_655 ? O4 C7 O3 124.0(5) . . ? O4 C7 C3 116.5(5) . . ? O3 C7 C3 119.4(5) . . ? C15 C11 C16 115.0(4) . . ? C15 C11 C18 107.3(4) . . ? C16 C11 C18 107.7(4) . . ? C15 C11 C12 102.5(4) . . ? C16 C11 C12 111.2(4) . . ? C18 C11 C12 113.1(4) . . ? C19 C12 C20 108.2(5) . . ? C19 C12 C11 114.5(5) . . ? C20 C12 C11 111.3(4) . . ? C19 C12 C13 110.2(4) . . ? C20 C12 C13 110.6(5) . . ? C11 C12 C13 102.0(4) . . ? C17 C13 C14 114.3(5) . . ? C17 C13 C12 113.2(5) . . ? C14 C13 C12 105.1(4) . . ? C15 C14 C13 106.7(4) . . ? C14 C15 C11 104.6(4) . . ? O6 C16 O5 125.9(5) . . ? O6 C16 C11 117.7(5) . . ? O5 C16 C11 116.4(4) . . ? O8 C17 O7 120.6(6) . . ? O8 C17 C13 119.0(5) . . ? O7 C17 C13 120.4(5) . . ? O8 C17 Co2 64.5(3) . 2_646 ? O7 C17 Co2 56.4(3) . 2_646 ? C13 C17 Co2 173.9(4) . 2_646 ? N1 C21 C22 112.3(5) . . ? N2 C22 C21 114.0(5) . . ? N2 C23 C24 112.2(5) . . ? N1 C24 C23 110.9(5) . . ? N3 C25 C26 125.5(6) . . ? C25 C26 C27 119.0(5) . . ? N1 C27 C28 123.1(5) . . ? N1 C27 C26 121.0(5) . . ? C28 C27 C26 115.9(6) . . ? C29 C28 C27 120.7(6) . . ? N3 C29 C28 124.2(5) . . ? N4 C30 C31 123.7(6) . . ? C30 C31 C32 121.7(5) . . ? N2 C32 C33 122.6(5) . . ? N2 C32 C31 122.8(5) . . ? C33 C32 C31 114.5(5) . . ? C34 C33 C32 119.7(5) . . ? N4 C34 C33 124.6(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.451 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.146 # Attachment '- cpd 2.cif' data_cpd2 _database_code_depnum_ccdc_archive 'CCDC 790238' #TrackingRef '- cpd 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Cd N4 O8' _chemical_formula_weight 751.15 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.4338(6) _cell_length_b 20.8333(16) _cell_length_c 22.0157(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.7680(10) _cell_angle_gamma 90.00 _cell_volume 3409.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3663 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 24.81 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6846 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 '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 13636 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.08 _reflns_number_total 10505 _reflns_number_gt 9133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+1.8426P] 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 -0.02(3) _refine_ls_number_reflns 10505 _refine_ls_number_parameters 861 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1690 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 -0.55118(8) 0.85999(2) 0.37008(3) 0.03254(18) Uani 1 1 d . . . Cd2 Cd 0.97713(8) 0.84570(2) 0.87751(3) 0.03217(18) Uani 1 1 d . . . O1 O -1.0941(13) 0.5199(4) 0.2913(4) 0.070(2) Uani 1 1 d . . . O2 O -0.8802(13) 0.5231(4) 0.2195(4) 0.067(2) Uani 1 1 d . . . H101 H -0.9590 0.5075 0.1976 0.101 Uiso 1 1 calc R . . O3 O -0.7053(11) 0.7774(3) 0.3189(4) 0.056(2) Uani 1 1 d . . . O4 O -0.6134(12) 0.7593(3) 0.4110(3) 0.059(2) Uani 1 1 d . . . O5 O -0.6815(10) 0.9610(3) 0.3425(3) 0.0467(18) Uani 1 1 d . . . O6 O -0.7211(9) 0.9228(3) 0.4330(3) 0.0365(15) Uani 1 1 d . . . O7 O -0.6064(17) 1.2229(4) 0.4540(5) 0.107(4) Uani 1 1 d . . . O8 O -0.6475(14) 1.1821(4) 0.5445(4) 0.081(3) Uani 1 1 d . . . H102 H -0.5389 1.1864 0.5502 0.121 Uiso 1 1 d R . . O9 O 1.1301(12) 1.2081(4) 0.9482(4) 0.066(2) Uani 1 1 d . . . O10 O 1.2075(11) 1.1639(3) 1.0336(3) 0.0503(18) Uani 1 1 d . . . H103 H 1.1064 1.1731 1.0452 0.075 Uiso 1 1 calc R . . O11 O 1.1872(8) 0.9037(3) 0.9330(3) 0.0387(15) Uani 1 1 d . . . O12 O 1.0989(10) 0.9452(3) 0.8462(3) 0.0458(18) Uani 1 1 d . . . O13 O 1.0234(11) 0.7381(3) 0.9066(3) 0.0539(19) Uani 1 1 d . . . O14 O 1.1341(9) 0.7695(3) 0.8204(3) 0.0467(19) Uani 1 1 d . . . O15 O 1.5979(15) 0.5233(4) 0.8024(5) 0.087(3) Uani 1 1 d . . . O16 O 1.431(3) 0.5345(5) 0.7114(5) 0.184(9) Uani 1 1 d . . . H104 H 1.5262 0.5215 0.6969 0.277 Uiso 1 1 d R . . N1 N 0.0685(10) 0.8447(4) 0.5797(3) 0.0369(17) Uani 1 1 d . . . N2 N 0.3544(9) 0.8489(4) 0.6680(3) 0.0371(17) Uani 1 1 d . . . N3 N -0.3206(9) 0.8610(4) 0.4403(3) 0.0332(16) Uani 1 1 d . . . N4 N 0.7608(9) 0.8473(4) 0.8032(3) 0.0344(16) Uani 1 1 d . . . N5 N 0.0778(9) 0.8518(4) 0.1700(3) 0.0352(16) Uani 1 1 d . . . N6 N 0.3754(9) 0.8399(3) 0.0885(3) 0.0344(17) Uani 1 1 d . . . N7 N -0.3435(10) 0.8595(4) 0.2946(3) 0.0402(17) Uani 1 1 d . . . N8 N 0.7620(9) 0.8510(4) -0.0485(3) 0.0339(15) Uani 1 1 d . . . C1 C -0.8093(16) 0.5699(4) 0.3139(4) 0.050(3) Uani 1 1 d . . . C2 C -0.7784(15) 0.6409(4) 0.2970(4) 0.046(3) Uani 1 1 d . . . C3 C -0.7018(16) 0.6673(4) 0.3550(4) 0.048(3) Uani 1 1 d . . . H3 H -0.5806 0.6489 0.3578 0.058 Uiso 1 1 calc R . . C4 C -0.7995(18) 0.6385(5) 0.4075(5) 0.055(3) Uani 1 1 d . . . H4A H -0.8989 0.6655 0.4197 0.066 Uiso 1 1 calc R . . H4B H -0.7191 0.6321 0.4420 0.066 Uiso 1 1 calc R . . C5 C -0.8682(19) 0.5734(5) 0.3819(5) 0.058(3) Uani 1 1 d . . . H5A H -0.9981 0.5709 0.3846 0.070 Uiso 1 1 calc R . . H5B H -0.8161 0.5380 0.4048 0.070 Uiso 1 1 calc R . . C6 C -0.9470(19) 0.5351(4) 0.2741(5) 0.057(3) Uani 1 1 d . . . C7 C -0.6728(15) 0.7400(4) 0.3611(4) 0.037(2) Uani 1 1 d . . . C8 C -0.6293(17) 0.5307(5) 0.3161(5) 0.065(3) Uani 1 1 d . . . H8A H -0.6503 0.4897 0.3347 0.097 Uiso 1 1 calc R . . H8B H -0.5406 0.5538 0.3394 0.097 Uiso 1 1 calc R . . H8C H -0.5868 0.5244 0.2755 0.097 Uiso 1 1 calc R . . C9 C -0.6677(19) 0.6514(6) 0.2412(5) 0.067(4) Uani 1 1 d . . . H9A H -0.6780 0.6954 0.2286 0.100 Uiso 1 1 calc R . . H9B H -0.7104 0.6239 0.2092 0.100 Uiso 1 1 calc R . . H9C H -0.5440 0.6417 0.2503 0.100 Uiso 1 1 calc R . . C10 C -0.9704(17) 0.6707(5) 0.2838(6) 0.064(3) Uani 1 1 d . . . H10A H -1.0423 0.6674 0.3196 0.095 Uiso 1 1 calc R . . H10B H -1.0279 0.6478 0.2511 0.095 Uiso 1 1 calc R . . H10C H -0.9577 0.7150 0.2728 0.095 Uiso 1 1 calc R . . C11 C -0.8314(16) 1.0298(5) 0.4175(5) 0.054(3) Uani 1 1 d . . . C12 C -0.7013(15) 1.0670(5) 0.4641(5) 0.051(3) Uani 1 1 d . . . C13 C -0.7962(15) 1.1331(4) 0.4638(5) 0.046(2) Uani 1 1 d . . . H13 H -0.8995 1.1309 0.4909 0.055 Uiso 1 1 calc R . . C14 C -0.858(3) 1.1476(7) 0.4060(6) 0.104(6) Uani 1 1 d . . . H14A H -0.7746 1.1759 0.3857 0.125 Uiso 1 1 calc R . . H14B H -0.9743 1.1688 0.4077 0.125 Uiso 1 1 calc R . . C15 C -0.877(2) 1.0778(6) 0.3686(7) 0.096(5) Uani 1 1 d . . . H15A H -0.9976 1.0714 0.3527 0.115 Uiso 1 1 calc R . . H15B H -0.7921 1.0754 0.3355 0.115 Uiso 1 1 calc R . . C16 C -0.7393(12) 0.9681(4) 0.3955(4) 0.034(2) Uani 1 1 d . . . C17 C -0.6683(19) 1.1854(5) 0.4875(5) 0.061(3) Uani 1 1 d . . . C18 C -1.0052(16) 1.0131(6) 0.4489(6) 0.076(4) Uani 1 1 d . . . H18A H -1.0438 1.0491 0.4727 0.114 Uiso 1 1 calc R . . H18B H -0.9862 0.9767 0.4749 0.114 Uiso 1 1 calc R . . H18C H -1.0960 1.0030 0.4190 0.114 Uiso 1 1 calc R . . C19 C -0.690(2) 1.0374(6) 0.5277(5) 0.067(4) Uani 1 1 d . . . H19A H -0.6438 0.9945 0.5250 0.101 Uiso 1 1 calc R . . H19B H -0.8083 1.0363 0.5449 0.101 Uiso 1 1 calc R . . H19C H -0.6122 1.0628 0.5531 0.101 Uiso 1 1 calc R . . C20 C -0.5265(14) 1.0708(5) 0.4377(5) 0.051(3) Uani 1 1 d . . . H20A H -0.4434 1.0894 0.4665 0.076 Uiso 1 1 calc R . . H20B H -0.5323 1.0972 0.4020 0.076 Uiso 1 1 calc R . . H20C H -0.4867 1.0285 0.4270 0.076 Uiso 1 1 calc R . . C21 C 1.3174(13) 1.1137(4) 0.9477(4) 0.035(2) Uani 1 1 d . . . C22 C 1.2236(13) 1.0481(4) 0.9583(4) 0.036(2) Uani 1 1 d . . . C23 C 1.3129(13) 1.0049(4) 0.9080(5) 0.042(2) Uani 1 1 d . . . H23 H 1.4269 0.9886 0.9246 0.051 Uiso 1 1 calc R . . C24 C 1.3563(16) 1.0495(5) 0.8558(4) 0.050(3) Uani 1 1 d . . . H24A H 1.2812 1.0397 0.8206 0.060 Uiso 1 1 calc R . . H24B H 1.4813 1.0450 0.8445 0.060 Uiso 1 1 calc R . . C25 C 1.3193(16) 1.1182(5) 0.8780(4) 0.051(3) Uani 1 1 d . . . H25A H 1.2043 1.1334 0.8625 0.061 Uiso 1 1 calc R . . H25B H 1.4129 1.1472 0.8648 0.061 Uiso 1 1 calc R . . C26 C 1.2114(13) 1.1669(4) 0.9759(4) 0.037(2) Uani 1 1 d . . . C27 C 1.1944(12) 0.9480(4) 0.8939(4) 0.0302(19) Uani 1 1 d . . . C28 C 1.5033(14) 1.1159(5) 0.9694(6) 0.062(3) Uani 1 1 d . . . H28A H 1.5572 1.1557 0.9574 0.094 Uiso 1 1 calc R . . H28B H 1.5692 1.0808 0.9523 0.094 Uiso 1 1 calc R . . H28C H 1.5062 1.1125 1.0129 0.094 Uiso 1 1 calc R . . C29 C 1.2537(16) 1.0176(4) 1.0207(4) 0.046(3) Uani 1 1 d . . . H29A H 1.3802 1.0165 1.0300 0.069 Uiso 1 1 calc R . . H29B H 1.2070 0.9746 1.0204 0.069 Uiso 1 1 calc R . . H29C H 1.1929 1.0425 1.0508 0.069 Uiso 1 1 calc R . . C30 C 1.0210(12) 1.0536(4) 0.9464(5) 0.041(2) Uani 1 1 d . . . H30A H 0.9709 1.0115 0.9408 0.061 Uiso 1 1 calc R . . H30B H 0.9996 1.0788 0.9105 0.061 Uiso 1 1 calc R . . H30C H 0.9654 1.0739 0.9805 0.061 Uiso 1 1 calc R . . C31 C 1.1265(13) 0.6539(4) 0.8400(4) 0.042(2) Uani 1 1 d . . . C32 C 1.2867(13) 0.6413(5) 0.7963(5) 0.047(2) Uani 1 1 d . . . C33 C 1.2910(16) 0.5671(4) 0.7988(4) 0.046(3) Uani 1 1 d . . . H33 H 1.1831 0.5500 0.7784 0.055 Uiso 1 1 calc R . . C34 C 1.288(2) 0.5489(7) 0.8661(5) 0.089(5) Uani 1 1 d . . . H34A H 1.4080 0.5459 0.8836 0.107 Uiso 1 1 calc R . . H34B H 1.2238 0.5090 0.8728 0.107 Uiso 1 1 calc R . . C35 C 1.177(2) 0.6113(7) 0.8927(6) 0.090(5) Uani 1 1 d . . . H35A H 1.0694 0.5971 0.9133 0.107 Uiso 1 1 calc R . . H35B H 1.2516 0.6347 0.9216 0.107 Uiso 1 1 calc R . . C36 C 1.0954(12) 0.7252(4) 0.8542(4) 0.034(2) Uani 1 1 d . . . C37 C 1.4709(18) 0.5361(5) 0.7674(6) 0.062(3) Uani 1 1 d . . . C38 C 0.9433(16) 0.6324(6) 0.8101(8) 0.102(6) Uani 1 1 d . . . H38A H 0.9470 0.5872 0.8018 0.153 Uiso 1 1 calc R . . H38B H 0.9242 0.6554 0.7728 0.153 Uiso 1 1 calc R . . H38C H 0.8468 0.6414 0.8373 0.153 Uiso 1 1 calc R . . C39 C 1.2527(18) 0.6661(6) 0.7300(5) 0.067(3) Uani 1 1 d . . . H39A H 1.2238 0.7110 0.7309 0.101 Uiso 1 1 calc R . . H39B H 1.1544 0.6427 0.7118 0.101 Uiso 1 1 calc R . . H39C H 1.3591 0.6597 0.7065 0.101 Uiso 1 1 calc R . . C40 C 1.4619(15) 0.6699(6) 0.8220(8) 0.090(5) Uani 1 1 d . . . H40A H 1.4458 0.7150 0.8292 0.135 Uiso 1 1 calc R . . H40B H 1.5567 0.6637 0.7934 0.135 Uiso 1 1 calc R . . H40C H 1.4928 0.6489 0.8595 0.135 Uiso 1 1 calc R . . C41 C 0.2503(14) 0.8241(5) 0.5651(5) 0.050(3) Uani 1 1 d . . . H41A H 0.3121 0.8593 0.5455 0.060 Uiso 1 1 calc R . . H41B H 0.2428 0.7889 0.5362 0.060 Uiso 1 1 calc R . . C42 C 0.3607(16) 0.8026(5) 0.6196(5) 0.056(3) Uani 1 1 d . . . H42A H 0.3152 0.7618 0.6339 0.067 Uiso 1 1 calc R . . H42B H 0.4846 0.7964 0.6076 0.067 Uiso 1 1 calc R . . C43 C 0.1724(12) 0.8697(5) 0.6831(4) 0.043(2) Uani 1 1 d . . . H43A H 0.1097 0.8343 0.7020 0.051 Uiso 1 1 calc R . . H43B H 0.1803 0.9043 0.7125 0.051 Uiso 1 1 calc R . . C44 C 0.0712(14) 0.8909(5) 0.6323(5) 0.053(3) Uani 1 1 d . . . H44A H 0.1201 0.9315 0.6186 0.063 Uiso 1 1 calc R . . H44B H -0.0516 0.8986 0.6447 0.063 Uiso 1 1 calc R . . C45 C -0.1679(14) 0.8285(4) 0.4346(4) 0.040(2) Uani 1 1 d . . . H45 H -0.1488 0.8086 0.3974 0.048 Uiso 1 1 calc R . . C46 C -0.0367(13) 0.8215(4) 0.4778(4) 0.034(2) Uani 1 1 d . . . H46 H 0.0659 0.7977 0.4694 0.041 Uiso 1 1 calc R . . C47 C -0.0566(12) 0.8503(6) 0.5354(4) 0.035(2) Uani 1 1 d . . . C48 C -0.2191(12) 0.8850(4) 0.5413(4) 0.037(2) Uani 1 1 d . . . H48 H -0.2430 0.9057 0.5777 0.045 Uiso 1 1 calc R . . C49 C -0.3363(14) 0.8887(4) 0.4966(5) 0.042(2) Uani 1 1 d . . . H49 H -0.4402 0.9122 0.5037 0.051 Uiso 1 1 calc R . . C50 C 0.7678(12) 0.8100(4) 0.7544(4) 0.033(2) Uani 1 1 d . . . H50 H 0.8665 0.7829 0.7508 0.039 Uiso 1 1 calc R . . C51 C 0.6382(13) 0.8085(4) 0.7082(4) 0.038(2) Uani 1 1 d . . . H51 H 0.6536 0.7819 0.6747 0.045 Uiso 1 1 calc R . . C52 C 0.4844(10) 0.8470(6) 0.7125(3) 0.0271(17) Uani 1 1 d . . . C53 C 0.4827(14) 0.8869(4) 0.7662(5) 0.041(2) Uani 1 1 d . . . H53 H 0.3852 0.9141 0.7723 0.049 Uiso 1 1 calc R . . C54 C 0.6147(13) 0.8861(4) 0.8067(5) 0.040(2) Uani 1 1 d . . . H54 H 0.6072 0.9138 0.8397 0.048 Uiso 1 1 calc R . . C55 C 0.0885(15) 0.7983(5) 0.1277(5) 0.051(3) Uani 1 1 d . . . H55A H -0.0321 0.7860 0.1149 0.062 Uiso 1 1 calc R . . H55B H 0.1433 0.7618 0.1481 0.062 Uiso 1 1 calc R . . C56 C 0.1969(13) 0.8151(5) 0.0725(5) 0.053(3) Uani 1 1 d . . . H56A H 0.2099 0.7771 0.0475 0.064 Uiso 1 1 calc R . . H56B H 0.1324 0.8471 0.0487 0.064 Uiso 1 1 calc R . . C57 C 0.3732(12) 0.8899(4) 0.1345(4) 0.033(2) Uani 1 1 d . . . H57A H 0.3296 0.9294 0.1161 0.040 Uiso 1 1 calc R . . H57B H 0.4953 0.8975 0.1488 0.040 Uiso 1 1 calc R . . C58 C 0.2588(12) 0.8743(5) 0.1876(4) 0.040(2) Uani 1 1 d . . . H58A H 0.3179 0.8413 0.2118 0.048 Uiso 1 1 calc R . . H58B H 0.2475 0.9122 0.2129 0.048 Uiso 1 1 calc R . . C59 C -0.3345(12) 0.8149(4) 0.2521(4) 0.038(2) Uani 1 1 d . . . H59 H -0.4257 0.7843 0.2508 0.045 Uiso 1 1 calc R . . C60 C -0.2004(12) 0.8099(4) 0.2094(4) 0.035(2) Uani 1 1 d . . . H60 H -0.2048 0.7778 0.1800 0.042 Uiso 1 1 calc R . . C61 C -0.0590(11) 0.8537(6) 0.2110(4) 0.0325(19) Uani 1 1 d . . . C62 C -0.0631(13) 0.8996(5) 0.2562(4) 0.042(2) Uani 1 1 d . . . H62 H 0.0300 0.9292 0.2602 0.050 Uiso 1 1 calc R . . C63 C -0.2073(14) 0.9014(5) 0.2958(4) 0.050(3) Uani 1 1 d . . . H63 H -0.2092 0.9337 0.3249 0.060 Uiso 1 1 calc R . . C64 C 0.6127(13) 0.8132(4) -0.0546(4) 0.040(2) Uani 1 1 d . . . H64 H 0.5967 0.7899 -0.0903 0.048 Uiso 1 1 calc R . . C65 C 0.4871(14) 0.8082(4) -0.0110(4) 0.040(2) Uani 1 1 d . . . H65 H 0.3893 0.7810 -0.0169 0.048 Uiso 1 1 calc R . . C66 C 0.5025(11) 0.8436(5) 0.0435(4) 0.0310(19) Uani 1 1 d . . . C67 C 0.6560(13) 0.8824(4) 0.0485(4) 0.039(2) Uani 1 1 d . . . H67 H 0.6740 0.9074 0.0831 0.047 Uiso 1 1 calc R . . C68 C 0.7783(13) 0.8839(4) 0.0036(4) 0.039(2) Uani 1 1 d . . . H68 H 0.8799 0.9094 0.0092 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0386(4) 0.0294(4) 0.0297(3) -0.0010(2) 0.0027(3) -0.0058(2) Cd2 0.0341(3) 0.0258(4) 0.0366(3) 0.0027(2) 0.0041(3) 0.0035(2) O1 0.076(6) 0.067(5) 0.067(6) -0.002(4) 0.006(5) -0.031(5) O2 0.099(7) 0.049(5) 0.053(5) -0.021(4) -0.004(5) -0.009(4) O3 0.076(6) 0.031(4) 0.061(5) 0.002(3) -0.004(4) -0.011(3) O4 0.090(6) 0.034(4) 0.051(5) 0.000(3) -0.012(4) -0.001(4) O5 0.062(5) 0.029(3) 0.048(5) 0.007(3) -0.024(4) -0.012(3) O6 0.046(4) 0.028(3) 0.036(4) -0.001(3) 0.000(3) -0.003(3) O7 0.156(11) 0.051(5) 0.116(8) -0.016(5) 0.046(8) -0.029(6) O8 0.110(8) 0.048(5) 0.084(7) -0.017(4) -0.018(6) 0.023(5) O9 0.087(6) 0.050(4) 0.060(5) -0.003(4) -0.011(5) 0.020(4) O10 0.071(5) 0.038(4) 0.042(4) 0.003(3) 0.009(4) -0.006(4) O11 0.042(4) 0.030(3) 0.044(4) 0.006(3) -0.012(3) 0.000(3) O12 0.060(5) 0.025(3) 0.052(5) 0.003(3) 0.008(4) -0.005(3) O13 0.081(5) 0.030(3) 0.052(4) 0.006(3) 0.017(4) 0.003(3) O14 0.045(4) 0.025(3) 0.071(5) 0.013(3) 0.027(4) 0.013(3) O15 0.106(8) 0.066(6) 0.088(7) -0.003(5) 0.023(6) 0.032(5) O16 0.43(3) 0.041(6) 0.088(9) -0.024(5) 0.089(13) -0.005(10) N1 0.037(4) 0.049(4) 0.025(3) -0.003(3) -0.009(3) 0.011(4) N2 0.037(4) 0.031(4) 0.044(4) 0.000(3) 0.009(4) 0.011(3) N3 0.031(4) 0.039(4) 0.029(3) -0.003(3) -0.003(3) -0.002(3) N4 0.040(4) 0.031(4) 0.033(4) 0.000(3) 0.010(3) 0.004(4) N5 0.033(4) 0.046(4) 0.027(3) -0.006(3) -0.004(3) -0.012(3) N6 0.033(4) 0.032(4) 0.038(4) -0.010(3) 0.007(3) -0.006(3) N7 0.040(4) 0.046(5) 0.034(4) -0.003(4) 0.003(3) -0.004(4) N8 0.030(4) 0.030(4) 0.041(4) 0.003(3) 0.001(3) 0.004(3) C1 0.085(8) 0.028(5) 0.039(5) -0.008(4) 0.018(5) -0.019(5) C2 0.069(7) 0.029(5) 0.038(5) -0.006(4) 0.007(5) -0.005(5) C3 0.072(8) 0.041(5) 0.032(5) 0.000(4) 0.012(5) -0.004(5) C4 0.085(9) 0.047(6) 0.035(6) -0.006(4) 0.007(6) -0.016(5) C5 0.084(9) 0.054(6) 0.036(6) 0.002(5) -0.004(6) -0.014(6) C6 0.091(10) 0.025(5) 0.056(7) 0.000(4) -0.006(7) -0.010(5) C7 0.058(7) 0.030(5) 0.022(4) -0.004(4) 0.005(5) -0.008(4) C8 0.080(9) 0.055(7) 0.059(7) -0.007(5) -0.008(7) 0.000(6) C9 0.106(10) 0.055(7) 0.039(6) 0.000(5) 0.023(6) -0.028(6) C10 0.074(9) 0.052(7) 0.064(8) -0.012(5) -0.009(7) -0.009(6) C11 0.055(7) 0.038(5) 0.069(7) 0.002(5) -0.013(6) 0.003(5) C12 0.054(7) 0.054(7) 0.046(6) 0.007(5) 0.005(5) -0.001(5) C13 0.056(7) 0.040(5) 0.041(6) 0.006(4) 0.003(5) 0.015(4) C14 0.173(18) 0.071(9) 0.069(10) -0.003(7) -0.045(11) 0.033(10) C15 0.126(14) 0.059(8) 0.104(12) 0.014(8) 0.026(11) 0.025(8) C16 0.029(5) 0.040(5) 0.033(5) -0.005(4) -0.018(5) -0.006(4) C17 0.104(10) 0.037(6) 0.043(6) -0.005(5) 0.023(7) 0.032(6) C18 0.042(7) 0.095(10) 0.091(10) -0.038(8) -0.017(7) 0.023(6) C19 0.088(10) 0.064(9) 0.049(7) 0.008(6) -0.005(7) 0.005(7) C20 0.050(7) 0.052(6) 0.050(6) -0.006(5) 0.002(5) -0.013(5) C21 0.045(6) 0.031(5) 0.028(5) 0.004(3) -0.002(4) 0.004(4) C22 0.040(6) 0.028(5) 0.038(5) -0.003(4) -0.007(5) 0.005(4) C23 0.038(5) 0.033(5) 0.056(6) -0.010(4) 0.015(5) -0.004(4) C24 0.065(7) 0.045(6) 0.041(6) -0.001(4) 0.014(5) -0.018(5) C25 0.072(8) 0.047(6) 0.034(6) 0.010(4) 0.013(5) -0.012(5) C26 0.050(6) 0.019(5) 0.042(6) 0.004(4) -0.001(5) 0.000(4) C27 0.031(5) 0.034(5) 0.025(4) -0.002(3) -0.005(4) 0.003(3) C28 0.036(6) 0.040(5) 0.112(10) -0.017(6) 0.015(7) 0.001(4) C29 0.070(7) 0.029(5) 0.038(5) 0.006(4) -0.004(5) 0.009(5) C30 0.031(5) 0.040(5) 0.051(6) -0.009(4) 0.006(5) 0.004(4) C31 0.042(6) 0.035(5) 0.050(6) 0.012(4) 0.012(5) 0.004(4) C32 0.035(5) 0.043(6) 0.063(7) -0.004(5) -0.003(5) 0.000(4) C33 0.078(8) 0.023(5) 0.036(5) -0.001(4) -0.018(5) 0.009(4) C34 0.142(15) 0.079(9) 0.047(7) 0.013(6) 0.028(9) 0.000(9) C35 0.120(13) 0.077(9) 0.073(9) 0.023(7) 0.039(9) 0.032(8) C36 0.022(5) 0.038(5) 0.043(5) 0.002(4) 0.001(4) 0.006(3) C37 0.074(9) 0.056(7) 0.054(7) 0.036(6) -0.029(7) -0.013(6) C38 0.043(7) 0.064(8) 0.202(18) -0.072(10) 0.054(9) -0.023(6) C39 0.084(9) 0.051(7) 0.067(8) 0.014(6) 0.008(7) 0.004(6) C40 0.031(6) 0.065(8) 0.173(16) -0.054(9) 0.012(8) 0.000(5) C41 0.041(6) 0.068(7) 0.042(6) -0.002(5) 0.002(5) 0.022(5) C42 0.063(7) 0.064(7) 0.039(6) -0.010(5) -0.011(6) 0.025(6) C43 0.035(5) 0.068(7) 0.026(4) -0.009(4) -0.009(4) 0.015(5) C44 0.032(5) 0.062(7) 0.065(7) -0.019(5) 0.006(6) 0.018(5) C45 0.050(6) 0.034(5) 0.037(5) -0.012(4) 0.006(5) -0.009(4) C46 0.039(6) 0.033(5) 0.031(5) -0.002(4) -0.006(5) 0.003(4) C47 0.032(4) 0.038(6) 0.035(4) 0.000(5) 0.002(4) -0.002(5) C48 0.030(5) 0.048(6) 0.034(5) -0.010(4) -0.013(5) 0.010(4) C49 0.043(6) 0.039(5) 0.045(6) -0.003(4) 0.012(5) 0.002(4) C50 0.024(5) 0.039(5) 0.034(5) 0.009(4) -0.004(4) 0.013(4) C51 0.047(6) 0.033(5) 0.034(5) -0.004(4) 0.016(5) 0.008(4) C52 0.028(4) 0.030(4) 0.024(4) 0.004(4) -0.004(3) 0.007(4) C53 0.035(5) 0.034(5) 0.055(6) -0.009(4) 0.000(5) 0.012(4) C54 0.035(5) 0.038(5) 0.047(6) -0.012(4) -0.011(5) 0.015(4) C55 0.055(6) 0.052(6) 0.048(6) -0.018(5) 0.017(5) -0.017(5) C56 0.040(6) 0.061(7) 0.058(7) -0.023(5) 0.018(6) -0.016(5) C57 0.026(5) 0.041(5) 0.032(5) 0.000(4) 0.003(4) -0.010(3) C58 0.036(5) 0.054(6) 0.030(5) -0.004(4) -0.006(4) -0.013(4) C59 0.029(5) 0.045(5) 0.039(5) 0.002(4) -0.005(4) -0.003(4) C60 0.030(5) 0.041(5) 0.034(5) -0.002(4) 0.001(4) -0.012(4) C61 0.032(4) 0.039(5) 0.026(4) -0.002(5) -0.003(4) -0.001(5) C62 0.037(6) 0.052(6) 0.037(5) -0.010(4) 0.009(5) -0.017(5) C63 0.052(7) 0.059(6) 0.038(6) -0.015(5) 0.012(5) -0.025(5) C64 0.044(6) 0.042(5) 0.034(5) 0.000(4) 0.005(5) 0.004(4) C65 0.042(6) 0.030(5) 0.048(6) -0.003(4) 0.007(5) -0.002(4) C66 0.030(4) 0.028(5) 0.034(4) 0.000(4) -0.003(4) 0.002(4) C67 0.040(5) 0.044(5) 0.033(5) -0.003(4) 0.004(5) -0.005(4) C68 0.041(6) 0.032(5) 0.046(6) -0.001(4) 0.009(5) -0.004(4) _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 N7 2.283(7) . ? Cd1 N3 2.292(7) . ? Cd1 O6 2.296(6) . ? Cd1 O4 2.332(7) . ? Cd1 O3 2.347(7) . ? Cd1 O5 2.392(7) . ? Cd1 C7 2.665(8) . ? Cd1 C16 2.713(9) . ? Cd2 N4 2.279(7) . ? Cd2 N8 2.300(6) 1_556 ? Cd2 O11 2.311(6) . ? Cd2 O14 2.345(6) . ? Cd2 O13 2.354(6) . ? Cd2 O12 2.368(6) . ? Cd2 C27 2.696(9) . ? Cd2 C36 2.711(8) . ? O1 C6 1.204(14) . ? O2 C6 1.332(13) . ? O3 C7 1.234(11) . ? O4 C7 1.244(11) . ? O5 C16 1.257(12) . ? O6 C16 1.261(11) . ? O7 C17 1.172(14) . ? O8 C17 1.265(13) . ? O9 C26 1.209(11) . ? O10 C26 1.272(11) . ? O11 C27 1.265(10) . ? O12 C27 1.261(11) . ? O13 C36 1.305(11) . ? O14 C36 1.223(10) . ? O15 C37 1.241(15) . ? O16 C37 1.263(17) . ? N1 C47 1.344(11) . ? N1 C41 1.459(11) . ? N1 C44 1.505(12) . ? N2 C52 1.367(11) . ? N2 C42 1.440(12) . ? N2 C43 1.463(11) . ? N3 C45 1.330(12) . ? N3 C49 1.375(11) . ? N4 C50 1.328(11) . ? N4 C54 1.357(11) . ? N5 C61 1.370(10) . ? N5 C55 1.454(11) . ? N5 C58 1.472(11) . ? N6 C66 1.380(10) . ? N6 C57 1.454(10) . ? N6 C56 1.463(12) . ? N7 C59 1.321(11) . ? N7 C63 1.337(12) . ? N8 C68 1.341(11) . ? N8 C64 1.366(12) . ? N8 Cd2 2.300(6) 1_554 ? C1 C6 1.523(15) . ? C1 C2 1.542(12) . ? C1 C5 1.567(13) . ? C1 C8 1.569(16) . ? C2 C3 1.496(14) . ? C2 C9 1.503(14) . ? C2 C10 1.580(17) . ? C3 C4 1.499(13) . ? C3 C7 1.536(12) . ? C4 C5 1.553(14) . ? C11 C15 1.504(17) . ? C11 C18 1.514(17) . ? C11 C16 1.537(14) . ? C11 C12 1.602(16) . ? C12 C20 1.432(14) . ? C12 C19 1.531(15) . ? C12 C13 1.547(14) . ? C13 C14 1.383(16) . ? C13 C17 1.533(17) . ? C14 C15 1.68(2) . ? C21 C28 1.457(15) . ? C21 C26 1.500(12) . ? C21 C25 1.537(12) . ? C21 C22 1.553(12) . ? C22 C29 1.528(13) . ? C22 C30 1.529(13) . ? C22 C23 1.580(12) . ? C23 C27 1.506(12) . ? C23 C24 1.516(13) . ? C24 C25 1.537(14) . ? C31 C35 1.505(15) . ? C31 C36 1.536(12) . ? C31 C32 1.562(13) . ? C31 C38 1.570(17) . ? C32 C40 1.533(15) . ? C32 C33 1.548(13) . ? C32 C39 1.567(15) . ? C33 C34 1.531(14) . ? C33 C37 1.645(18) . ? C34 C35 1.651(18) . ? C41 C42 1.512(14) . ? C43 C44 1.412(14) . ? C45 C46 1.361(14) . ? C46 C47 1.413(12) . ? C47 C48 1.415(13) . ? C48 C49 1.307(14) . ? C50 C51 1.391(13) . ? C51 C52 1.402(12) . ? C52 C53 1.445(13) . ? C53 C54 1.317(14) . ? C55 C56 1.508(13) . ? C57 C58 1.491(11) . ? C59 C60 1.383(12) . ? C60 C61 1.392(14) . ? C61 C62 1.381(14) . ? C62 C63 1.391(13) . ? C64 C65 1.353(12) . ? C65 C66 1.412(13) . ? C66 C67 1.401(13) . ? C67 C68 1.352(12) . ? 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 N7 Cd1 N3 89.1(2) . . ? N7 Cd1 O6 145.5(3) . . ? N3 Cd1 O6 90.0(2) . . ? N7 Cd1 O4 114.6(3) . . ? N3 Cd1 O4 84.2(3) . . ? O6 Cd1 O4 99.6(3) . . ? N7 Cd1 O3 88.7(3) . . ? N3 Cd1 O3 133.3(3) . . ? O6 Cd1 O3 116.0(3) . . ? O4 Cd1 O3 55.1(3) . . ? N7 Cd1 O5 95.5(3) . . ? N3 Cd1 O5 117.3(2) . . ? O6 Cd1 O5 55.1(2) . . ? O4 Cd1 O5 143.9(3) . . ? O3 Cd1 O5 109.3(3) . . ? N7 Cd1 C7 100.0(3) . . ? N3 Cd1 C7 108.0(3) . . ? O6 Cd1 C7 113.0(3) . . ? O4 Cd1 C7 27.8(3) . . ? O3 Cd1 C7 27.6(3) . . ? O5 Cd1 C7 132.1(3) . . ? N7 Cd1 C16 120.6(3) . . ? N3 Cd1 C16 103.7(3) . . ? O6 Cd1 C16 27.6(3) . . ? O4 Cd1 C16 124.2(3) . . ? O3 Cd1 C16 117.3(3) . . ? O5 Cd1 C16 27.6(3) . . ? C7 Cd1 C16 128.2(3) . . ? N4 Cd2 N8 91.0(2) . 1_556 ? N4 Cd2 O11 146.8(2) . . ? N8 Cd2 O11 94.1(2) 1_556 . ? N4 Cd2 O14 88.7(3) . . ? N8 Cd2 O14 140.2(2) 1_556 . ? O11 Cd2 O14 107.4(2) . . ? N4 Cd2 O13 108.0(3) . . ? N8 Cd2 O13 87.4(2) 1_556 . ? O11 Cd2 O13 105.0(2) . . ? O14 Cd2 O13 55.2(2) . . ? N4 Cd2 O12 92.7(3) . . ? N8 Cd2 O12 115.8(2) 1_556 . ? O11 Cd2 O12 55.8(2) . . ? O14 Cd2 O12 104.0(2) . . ? O13 Cd2 O12 149.0(3) . . ? N4 Cd2 C27 120.0(3) . . ? N8 Cd2 C27 106.7(3) 1_556 . ? O11 Cd2 C27 27.9(2) . . ? O14 Cd2 C27 107.8(2) . . ? O13 Cd2 C27 129.1(3) . . ? O12 Cd2 C27 27.9(2) . . ? N4 Cd2 C36 96.1(3) . . ? N8 Cd2 C36 114.1(3) 1_556 . ? O11 Cd2 C36 111.4(2) . . ? O14 Cd2 C36 26.8(2) . . ? O13 Cd2 C36 28.8(2) . . ? O12 Cd2 C36 129.0(2) . . ? C27 Cd2 C36 124.2(3) . . ? C7 O3 Cd1 90.7(6) . . ? C7 O4 Cd1 91.1(5) . . ? C16 O5 Cd1 90.6(5) . . ? C16 O6 Cd1 95.0(5) . . ? C27 O11 Cd2 93.2(6) . . ? C27 O12 Cd2 90.7(5) . . ? C36 O13 Cd2 91.0(5) . . ? C36 O14 Cd2 93.6(5) . . ? C47 N1 C41 120.0(7) . . ? C47 N1 C44 120.3(8) . . ? C41 N1 C44 110.8(8) . . ? C52 N2 C42 118.8(8) . . ? C52 N2 C43 119.5(7) . . ? C42 N2 C43 114.0(8) . . ? C45 N3 C49 112.4(8) . . ? C45 N3 Cd1 124.3(6) . . ? C49 N3 Cd1 122.8(6) . . ? C50 N4 C54 115.8(8) . . ? C50 N4 Cd2 122.5(6) . . ? C54 N4 Cd2 121.7(6) . . ? C61 N5 C55 119.4(8) . . ? C61 N5 C58 120.0(7) . . ? C55 N5 C58 110.8(8) . . ? C66 N6 C57 118.3(7) . . ? C66 N6 C56 118.3(7) . . ? C57 N6 C56 113.7(7) . . ? C59 N7 C63 115.3(8) . . ? C59 N7 Cd1 124.1(6) . . ? C63 N7 Cd1 120.2(6) . . ? C68 N8 C64 116.3(7) . . ? C68 N8 Cd2 125.1(6) . 1_554 ? C64 N8 Cd2 118.3(6) . 1_554 ? C6 C1 C2 114.7(9) . . ? C6 C1 C5 112.2(9) . . ? C2 C1 C5 103.4(7) . . ? C6 C1 C8 109.6(8) . . ? C2 C1 C8 112.2(9) . . ? C5 C1 C8 104.1(10) . . ? C3 C2 C9 115.9(9) . . ? C3 C2 C1 101.6(8) . . ? C9 C2 C1 115.0(8) . . ? C3 C2 C10 110.1(8) . . ? C9 C2 C10 107.2(10) . . ? C1 C2 C10 106.5(9) . . ? C2 C3 C4 109.2(9) . . ? C2 C3 C7 119.3(8) . . ? C4 C3 C7 113.3(8) . . ? C3 C4 C5 103.3(8) . . ? C4 C5 C1 107.0(8) . . ? O1 C6 O2 125.9(11) . . ? O1 C6 C1 123.4(10) . . ? O2 C6 C1 110.7(10) . . ? O3 C7 O4 121.6(8) . . ? O3 C7 C3 122.0(9) . . ? O4 C7 C3 116.4(8) . . ? O3 C7 Cd1 61.7(5) . . ? O4 C7 Cd1 61.0(5) . . ? C3 C7 Cd1 168.2(8) . . ? C15 C11 C18 107.2(11) . . ? C15 C11 C16 115.2(10) . . ? C18 C11 C16 109.8(9) . . ? C15 C11 C12 105.3(10) . . ? C18 C11 C12 109.3(10) . . ? C16 C11 C12 109.9(9) . . ? C20 C12 C19 110.9(10) . . ? C20 C12 C13 111.4(9) . . ? C19 C12 C13 112.4(9) . . ? C20 C12 C11 108.1(9) . . ? C19 C12 C11 114.5(10) . . ? C13 C12 C11 99.1(9) . . ? C14 C13 C17 110.8(11) . . ? C14 C13 C12 110.2(10) . . ? C17 C13 C12 110.5(9) . . ? C13 C14 C15 106.6(11) . . ? C11 C15 C14 102.1(11) . . ? O5 C16 O6 119.0(8) . . ? O5 C16 C11 123.3(9) . . ? O6 C16 C11 117.6(9) . . ? O5 C16 Cd1 61.8(5) . . ? O6 C16 Cd1 57.5(5) . . ? C11 C16 Cd1 172.6(7) . . ? O7 C17 O8 128.1(14) . . ? O7 C17 C13 120.5(12) . . ? O8 C17 C13 111.4(11) . . ? C28 C21 C26 110.0(8) . . ? C28 C21 C25 107.7(9) . . ? C26 C21 C25 112.3(8) . . ? C28 C21 C22 113.8(8) . . ? C26 C21 C22 110.4(7) . . ? C25 C21 C22 102.3(7) . . ? C29 C22 C30 108.5(8) . . ? C29 C22 C21 116.1(8) . . ? C30 C22 C21 110.6(7) . . ? C29 C22 C23 109.6(8) . . ? C30 C22 C23 110.2(8) . . ? C21 C22 C23 101.7(7) . . ? C27 C23 C24 117.2(9) . . ? C27 C23 C22 110.0(7) . . ? C24 C23 C22 106.1(7) . . ? C23 C24 C25 106.7(7) . . ? C24 C25 C21 105.4(8) . . ? O9 C26 O10 121.4(9) . . ? O9 C26 C21 125.3(9) . . ? O10 C26 C21 113.3(8) . . ? O12 C27 O11 120.3(8) . . ? O12 C27 C23 121.9(8) . . ? O11 C27 C23 117.7(8) . . ? O12 C27 Cd2 61.4(4) . . ? O11 C27 Cd2 58.9(5) . . ? C23 C27 Cd2 175.8(6) . . ? C35 C31 C36 116.7(9) . . ? C35 C31 C32 101.1(8) . . ? C36 C31 C32 113.9(7) . . ? C35 C31 C38 111.1(11) . . ? C36 C31 C38 103.3(8) . . ? C32 C31 C38 111.0(9) . . ? C40 C32 C33 111.0(9) . . ? C40 C32 C31 111.0(9) . . ? C33 C32 C31 99.3(8) . . ? C40 C32 C39 110.0(11) . . ? C33 C32 C39 111.4(8) . . ? C31 C32 C39 113.8(9) . . ? C34 C33 C32 106.3(9) . . ? C34 C33 C37 109.5(9) . . ? C32 C33 C37 113.2(9) . . ? C33 C34 C35 99.4(10) . . ? C31 C35 C34 108.1(9) . . ? O14 C36 O13 119.0(8) . . ? O14 C36 C31 124.7(8) . . ? O13 C36 C31 116.4(7) . . ? O14 C36 Cd2 59.7(4) . . ? O13 C36 Cd2 60.3(4) . . ? C31 C36 Cd2 169.7(6) . . ? O15 C37 O16 140.0(17) . . ? O15 C37 C33 116.1(11) . . ? O16 C37 C33 103.9(13) . . ? N1 C41 C42 114.0(8) . . ? N2 C42 C41 111.5(8) . . ? C44 C43 N2 113.4(7) . . ? C43 C44 N1 114.3(8) . . ? N3 C45 C46 126.5(8) . . ? C45 C46 C47 119.9(9) . . ? N1 C47 C46 122.3(9) . . ? N1 C47 C48 124.1(8) . . ? C46 C47 C48 113.6(9) . . ? C49 C48 C47 121.4(9) . . ? C48 C49 N3 126.2(9) . . ? N4 C50 C51 124.8(8) . . ? C50 C51 C52 119.7(8) . . ? N2 C52 C51 122.6(8) . . ? N2 C52 C53 123.7(8) . . ? C51 C52 C53 113.6(8) . . ? C54 C53 C52 122.1(8) . . ? C53 C54 N4 124.0(8) . . ? N5 C55 C56 111.9(8) . . ? N6 C56 C55 112.3(9) . . ? N6 C57 C58 113.6(7) . . ? N5 C58 C57 113.0(7) . . ? N7 C59 C60 125.3(8) . . ? C59 C60 C61 119.0(8) . . ? N5 C61 C62 121.3(9) . . ? N5 C61 C60 122.1(9) . . ? C62 C61 C60 116.6(8) . . ? C61 C62 C63 119.6(9) . . ? N7 C63 C62 124.1(9) . . ? C65 C64 N8 122.8(9) . . ? C64 C65 C66 120.9(9) . . ? N6 C66 C67 122.8(9) . . ? N6 C66 C65 122.1(9) . . ? C67 C66 C65 115.1(8) . . ? C68 C67 C66 120.8(9) . . ? N8 C68 C67 124.0(9) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.193 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.194 data_cpd3 _database_code_depnum_ccdc_archive 'CCDC 790239' #TrackingRef '- SI_cpd 3_R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 N4 O8 Zn' _chemical_formula_weight 704.12 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.1460(4) _cell_length_b 20.3903(11) _cell_length_c 22.8153(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.790(4) _cell_angle_gamma 90.00 _cell_volume 3322.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5168 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 21.22 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6613 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 '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 22012 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 25.12 _reflns_number_total 11406 _reflns_number_gt 7317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+1.2458P] 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 0.010(17) _refine_ls_number_reflns 11406 _refine_ls_number_parameters 894 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Zn1 Zn -0.48771(11) 0.85005(4) 0.36833(3) 0.0681(2) Uani 1 1 d . . . Zn2 Zn 0.93448(11) 0.85312(4) 0.88490(4) 0.0689(2) Uani 1 1 d . . . O1 O -1.0801(13) 0.5149(4) 0.2901(3) 0.131(3) Uani 1 1 d . . . O2 O -0.8602(11) 0.5280(4) 0.2258(3) 0.105(2) Uani 1 1 d . . . H101 H -0.8554 0.4895 0.2157 0.157 Uiso 1 1 calc R . . O3 O -0.606(2) 0.7720(5) 0.3422(4) 0.087(3) Uani 0.65 1 d PD A 1 O4 O -0.5920(12) 0.7496(4) 0.4338(5) 0.087(3) Uani 0.65 1 d P A 1 O3' O -0.703(2) 0.7743(11) 0.3543(15) 0.138(14) Uani 0.35 1 d PD A 2 O4' O -0.437(2) 0.7152(7) 0.3789(6) 0.068(4) Uani 0.35 1 d P A 2 O5 O -0.7398(9) 1.1420(4) 0.5461(3) 0.0987(19) Uani 1 1 d . . . O6 O -0.6237(9) 1.1998(3) 0.4768(3) 0.0941(18) Uani 1 1 d . . . H102 H -0.6855 1.2232 0.4543 0.141 Uiso 1 1 calc R . . O7 O -0.6163(11) 0.9575(3) 0.3171(4) 0.119(3) Uani 1 1 d . A . O8 O -0.6670(8) 0.9145(3) 0.4037(3) 0.0892(19) Uani 1 1 d . A . O9 O 1.1558(9) 1.2167(3) 0.9464(3) 0.102(2) Uani 1 1 d . . . O10 O 1.2375(8) 1.1708(3) 1.0315(3) 0.0772(15) Uani 1 1 d . . . H103 H 1.1831 1.2024 1.0452 0.116 Uiso 1 1 calc R . . O11 O 1.1339(8) 0.9071(3) 0.9281(3) 0.0792(15) Uani 1 1 d . . . O12 O 1.0673(11) 0.9516(3) 0.8447(3) 0.105(2) Uani 1 1 d . . . O13 O 1.4715(9) 0.5233(4) 0.7652(3) 0.107(2) Uani 1 1 d . . . H104 H 1.5130 0.5094 0.7344 0.160 Uiso 1 1 calc R . . O14 O 1.2211(9) 0.5437(3) 0.7080(3) 0.0885(16) Uani 1 1 d . . . O15 O 0.9665(9) 0.7535(3) 0.9070(3) 0.0902(17) Uani 1 1 d . . . O16 O 1.1506(9) 0.7866(3) 0.8438(3) 0.0874(17) Uani 1 1 d . . . N1 N 0.0965(7) 0.8429(3) 0.5774(2) 0.0570(13) Uani 1 1 d . A . N2 N 0.3681(7) 0.8473(4) 0.6712(2) 0.0597(13) Uani 1 1 d . . . N3 N -0.2883(7) 0.8525(3) 0.4343(2) 0.0576(12) Uani 1 1 d . A . N4 N 0.7586(7) 0.8536(3) 0.8128(2) 0.0606(12) Uani 1 1 d . . . N5 N 0.0993(9) 0.8446(4) 0.1746(3) 0.0834(19) Uani 1 1 d D . . N6 N 0.3692(9) 0.8437(4) 0.0856(3) 0.0796(18) Uani 1 1 d D . . N7 N -0.3105(9) 0.8491(4) 0.3004(2) 0.0763(16) Uani 1 1 d . A . N8 N 0.7352(8) 0.8602(3) -0.0523(2) 0.0664(15) Uani 1 1 d . . . C1 C -0.7868(13) 0.5660(4) 0.3215(4) 0.084(2) Uani 1 1 d . . . C2 C -0.7563(16) 0.6379(4) 0.3097(4) 0.093(3) Uani 1 1 d . . . C3 C -0.6729(16) 0.6603(4) 0.3681(4) 0.095(3) Uani 1 1 d . A . H3 H -0.5526 0.6372 0.3697 0.114 Uiso 1 1 calc R . . C4 C -0.7690(16) 0.6303(6) 0.4140(5) 0.110(4) Uani 1 1 d . . . H4A H -0.8664 0.6589 0.4281 0.132 Uiso 1 1 calc R . . H4B H -0.6837 0.6195 0.4465 0.132 Uiso 1 1 calc R . . C5 C -0.8570(16) 0.5654(5) 0.3851(4) 0.103(3) Uani 1 1 d . . . H5A H -0.8133 0.5266 0.4059 0.124 Uiso 1 1 calc R . . H5B H -0.9927 0.5666 0.3853 0.124 Uiso 1 1 calc R . . C6 C -0.9242(15) 0.5317(5) 0.2781(4) 0.088(3) Uani 1 1 d . . . C7 C -0.6152(17) 0.7291(5) 0.3775(5) 0.089(3) Uani 1 1 d D . . C8 C -0.6048(14) 0.5300(7) 0.3218(6) 0.136(5) Uani 1 1 d . . . H8A H -0.5519 0.5329 0.2837 0.203 Uiso 1 1 calc R . . H8B H -0.6253 0.4848 0.3314 0.203 Uiso 1 1 calc R . . H8C H -0.5201 0.5492 0.3504 0.203 Uiso 1 1 calc R . . C9 C -0.644(3) 0.6530(8) 0.2557(5) 0.200(9) Uani 1 1 d . . . H9A H -0.6703 0.6971 0.2429 0.300 Uiso 1 1 calc R . . H9B H -0.6790 0.6230 0.2248 0.300 Uiso 1 1 calc R . . H9C H -0.5131 0.6487 0.2651 0.300 Uiso 1 1 calc R . . C10 C -0.944(3) 0.6704(7) 0.2980(8) 0.185(7) Uani 1 1 d . . . H10A H -0.9305 0.7171 0.3013 0.277 Uiso 1 1 calc R . . H10B H -1.0314 0.6552 0.3262 0.277 Uiso 1 1 calc R . . H10C H -0.9896 0.6594 0.2592 0.277 Uiso 1 1 calc R . . C11 C -0.8214(10) 1.1132(3) 0.4477(3) 0.0572(17) Uani 1 1 d . . . C12 C -0.6890(12) 1.0774(4) 0.4068(4) 0.076(2) Uani 1 1 d . . . C13 C -0.8054(9) 1.0188(3) 0.3818(3) 0.0568(16) Uani 1 1 d . A . H13 H -0.8660 1.0334 0.3449 0.068 Uiso 1 1 calc R . . C14 C -0.9612(11) 1.0042(4) 0.4250(3) 0.071(2) Uani 1 1 d . . . H14A H -1.0840 1.0101 0.4064 0.085 Uiso 1 1 calc R . . H14B H -0.9512 0.9597 0.4399 0.085 Uiso 1 1 calc R . . C15 C -0.9274(11) 1.0534(4) 0.4732(3) 0.081(2) Uani 1 1 d . . . H15A H -0.8532 1.0337 0.5049 0.097 Uiso 1 1 calc R . . H15B H -1.0457 1.0676 0.4886 0.097 Uiso 1 1 calc R . . C16 C -0.7256(12) 1.1523(5) 0.4944(5) 0.084(2) Uani 1 1 d . . . C17 C -0.6892(11) 0.9593(4) 0.3682(5) 0.077(3) Uani 1 1 d . . . C18 C -0.9667(14) 1.1558(5) 0.4135(5) 0.102(3) Uani 1 1 d . . . H18A H -1.0590 1.1713 0.4398 0.153 Uiso 1 1 calc R . . H18B H -1.0265 1.1300 0.3831 0.153 Uiso 1 1 calc R . . H18C H -0.9046 1.1925 0.3963 0.153 Uiso 1 1 calc R . . C19 C -0.622(2) 1.1195(5) 0.3552(5) 0.136(5) Uani 1 1 d . . . H19A H -0.7233 1.1260 0.3273 0.204 Uiso 1 1 calc R . . H19B H -0.5207 1.0975 0.3365 0.204 Uiso 1 1 calc R . . H19C H -0.5789 1.1613 0.3697 0.204 Uiso 1 1 calc R . . C20 C -0.5130(11) 1.0559(4) 0.4393(5) 0.092(3) Uani 1 1 d . . . H20A H -0.4391 1.0937 0.4498 0.139 Uiso 1 1 calc R . . H20B H -0.4423 1.0276 0.4147 0.139 Uiso 1 1 calc R . . H20C H -0.5452 1.0327 0.4742 0.139 Uiso 1 1 calc R . . C21 C 1.3298(9) 1.1169(3) 0.9442(3) 0.0534(16) Uani 1 1 d . . . C22 C 1.2231(9) 1.0506(3) 0.9558(3) 0.0551(16) Uani 1 1 d . . . C23 C 1.2950(10) 1.0058(3) 0.9064(3) 0.0626(17) Uani 1 1 d . . . H23 H 1.4096 0.9847 0.9218 0.075 Uiso 1 1 calc R . . C24 C 1.3510(13) 1.0493(4) 0.8558(4) 0.083(2) Uani 1 1 d . . . H24A H 1.2736 1.0402 0.8210 0.099 Uiso 1 1 calc R . . H24B H 1.4811 1.0422 0.8467 0.099 Uiso 1 1 calc R . . C25 C 1.3201(13) 1.1218(4) 0.8772(4) 0.083(2) Uani 1 1 d . . . H25A H 1.4172 1.1506 0.8632 0.100 Uiso 1 1 calc R . . H25B H 1.1991 1.1383 0.8635 0.100 Uiso 1 1 calc R . . C26 C 1.2276(10) 1.1736(3) 0.9737(4) 0.067(2) Uani 1 1 d . . . C27 C 1.1589(11) 0.9517(4) 0.8908(3) 0.0622(18) Uani 1 1 d . . . C28 C 1.5301(10) 1.1172(5) 0.9665(5) 0.091(3) Uani 1 1 d . . . H28A H 1.5852 1.1591 0.9588 0.136 Uiso 1 1 calc R . . H28B H 1.5985 1.0836 0.9469 0.136 Uiso 1 1 calc R . . H28C H 1.5345 1.1090 1.0079 0.136 Uiso 1 1 calc R . . C29 C 1.2565(13) 1.0218(4) 1.0154(4) 0.079(2) Uani 1 1 d . . . H29A H 1.1893 0.9812 1.0182 0.119 Uiso 1 1 calc R . . H29B H 1.2137 1.0518 1.0445 0.119 Uiso 1 1 calc R . . H29C H 1.3880 1.0138 1.0218 0.119 Uiso 1 1 calc R . . C30 C 1.0113(9) 1.0625(4) 0.9471(4) 0.073(2) Uani 1 1 d . . . H30A H 0.9467 1.0212 0.9469 0.110 Uiso 1 1 calc R . . H30B H 0.9874 1.0845 0.9105 0.110 Uiso 1 1 calc R . . H30C H 0.9677 1.0891 0.9786 0.110 Uiso 1 1 calc R . . C31 C 1.2113(13) 0.5722(4) 0.8093(4) 0.082(2) Uani 1 1 d . . . C32 C 1.2629(10) 0.6483(4) 0.8150(4) 0.073(2) Uani 1 1 d . . . C33 C 1.1162(11) 0.6684(4) 0.8602(4) 0.076(2) Uani 1 1 d . . . H33 H 1.1504 0.6477 0.8978 0.091 Uiso 1 1 calc R . . C34 C 0.9311(11) 0.6371(4) 0.8366(4) 0.085(2) Uani 1 1 d . . . H34A H 0.8634 0.6670 0.8105 0.102 Uiso 1 1 calc R . . H34B H 0.8514 0.6251 0.8685 0.102 Uiso 1 1 calc R . . C35 C 0.9964(14) 0.5746(5) 0.8025(5) 0.112(3) Uani 1 1 d . . . H35A H 0.9415 0.5354 0.8188 0.134 Uiso 1 1 calc R . . H35B H 0.9584 0.5776 0.7614 0.134 Uiso 1 1 calc R . . C36 C 1.3018(12) 0.5447(4) 0.7557(4) 0.076(2) Uani 1 1 d . . . C37 C 1.0853(11) 0.7420(4) 0.8710(4) 0.067(2) Uani 1 1 d . . . C38 C 1.268(2) 0.5340(6) 0.8639(5) 0.143(5) Uani 1 1 d . . . H38A H 1.2251 0.4896 0.8600 0.215 Uiso 1 1 calc R . . H38B H 1.2129 0.5538 0.8974 0.215 Uiso 1 1 calc R . . H38C H 1.4019 0.5344 0.8688 0.215 Uiso 1 1 calc R . . C39 C 1.4618(13) 0.6645(7) 0.8351(6) 0.128(4) Uani 1 1 d . . . H39A H 1.4770 0.7112 0.8370 0.192 Uiso 1 1 calc R . . H39B H 1.5478 0.6465 0.8079 0.192 Uiso 1 1 calc R . . H39C H 1.4865 0.6460 0.8733 0.192 Uiso 1 1 calc R . . C40 C 1.2274(13) 0.6824(4) 0.7547(3) 0.078(2) Uani 1 1 d . . . H40A H 1.1093 0.6682 0.7380 0.117 Uiso 1 1 calc R . . H40B H 1.3257 0.6710 0.7289 0.117 Uiso 1 1 calc R . . H40C H 1.2254 0.7291 0.7601 0.117 Uiso 1 1 calc R . . C41 C 0.2884(10) 0.8216(4) 0.5702(3) 0.076(2) Uani 1 1 d . . . H41A H 0.2883 0.7853 0.5427 0.091 Uiso 1 1 calc R . . H41B H 0.3581 0.8572 0.5531 0.091 Uiso 1 1 calc R . . C42 C 0.3828(12) 0.8015(4) 0.6230(3) 0.077(2) Uani 1 1 d . . . H42A H 0.5143 0.7951 0.6152 0.092 Uiso 1 1 calc R . . H42B H 0.3325 0.7596 0.6349 0.092 Uiso 1 1 calc R . . C43 C 0.1733(10) 0.8633(5) 0.6800(3) 0.079(3) Uani 1 1 d . . . H43A H 0.1665 0.8961 0.7107 0.094 Uiso 1 1 calc R . . H43B H 0.1091 0.8244 0.6933 0.094 Uiso 1 1 calc R . . C44 C 0.0759(11) 0.8883(4) 0.6264(3) 0.076(2) Uani 1 1 d . . . H44A H -0.0560 0.8942 0.6338 0.091 Uiso 1 1 calc R . . H44B H 0.1274 0.9307 0.6162 0.091 Uiso 1 1 calc R . . C45 C -0.1267(11) 0.8184(3) 0.4322(3) 0.0622(18) Uani 1 1 d . . . H45 H -0.1030 0.7955 0.3979 0.075 Uiso 1 1 calc R A . C46 C 0.0040(10) 0.8151(3) 0.4768(3) 0.0544(16) Uani 1 1 d . A . H46 H 0.1140 0.7916 0.4719 0.065 Uiso 1 1 calc R . . C47 C -0.0267(9) 0.8471(4) 0.5303(2) 0.0534(14) Uani 1 1 d . . . C48 C -0.1979(10) 0.8812(3) 0.5324(3) 0.0609(18) Uani 1 1 d . A . H48 H -0.2297 0.9027 0.5667 0.073 Uiso 1 1 calc R . . C49 C -0.3152(10) 0.8830(3) 0.4854(3) 0.0596(18) Uani 1 1 d . . . H49 H -0.4244 0.9074 0.4885 0.071 Uiso 1 1 calc R A . C50 C 0.7804(10) 0.8147(4) 0.7660(3) 0.066(2) Uani 1 1 d . . . H50 H 0.8885 0.7893 0.7656 0.079 Uiso 1 1 calc R . . C51 C 0.6595(10) 0.8091(4) 0.7192(3) 0.0622(18) Uani 1 1 d . . . H51 H 0.6831 0.7799 0.6890 0.075 Uiso 1 1 calc R . . C52 C 0.4957(8) 0.8489(4) 0.7174(2) 0.0532(14) Uani 1 1 d . . . C53 C 0.4743(11) 0.8897(3) 0.7656(3) 0.067(2) Uani 1 1 d . . . H53 H 0.3698 0.9168 0.7671 0.080 Uiso 1 1 calc R . . C54 C 0.6009(11) 0.8907(3) 0.8098(3) 0.067(2) Uani 1 1 d . . . H54 H 0.5794 0.9188 0.8410 0.080 Uiso 1 1 calc R . . C55 C 0.116(2) 0.7877(5) 0.1379(5) 0.081(4) Uani 0.65 1 d PD B 1 H55A H -0.0050 0.7671 0.1313 0.097 Uiso 0.65 1 calc PR B 1 H55B H 0.2007 0.7560 0.1562 0.097 Uiso 0.65 1 calc PR B 1 C56 C 0.190(2) 0.8102(10) 0.0826(8) 0.130(12) Uani 0.65 1 d PD B 1 H56A H 0.2011 0.7725 0.0570 0.155 Uiso 0.65 1 calc PR B 1 H56B H 0.0984 0.8395 0.0643 0.155 Uiso 0.65 1 calc PR B 1 C57 C 0.3682(19) 0.8918(6) 0.1331(4) 0.063(3) Uani 0.65 1 d PD B 1 H57A H 0.4964 0.9050 0.1420 0.076 Uiso 0.65 1 calc PR B 1 H57B H 0.3008 0.9303 0.1192 0.076 Uiso 0.65 1 calc PR B 1 C58 C 0.2860(18) 0.8704(7) 0.1870(5) 0.087(4) Uani 0.65 1 d PD B 1 H58A H 0.2792 0.9070 0.2140 0.104 Uiso 0.65 1 calc PR B 1 H58B H 0.3638 0.8367 0.2053 0.104 Uiso 0.65 1 calc PR B 1 C55' C 0.066(5) 0.8315(19) 0.1110(9) 0.124(11) Uiso 0.35 1 d PD B 2 H55C H -0.0439 0.8036 0.1079 0.148 Uiso 0.35 1 calc PR B 2 H55D H 0.0305 0.8731 0.0933 0.148 Uiso 0.35 1 calc PR B 2 C56' C 0.204(3) 0.8026(14) 0.0734(13) 0.069(10) Uiso 0.35 1 d PD B 2 H56C H 0.1637 0.8051 0.0324 0.083 Uiso 0.35 1 calc PR B 2 H56D H 0.2278 0.7571 0.0837 0.083 Uiso 0.35 1 calc PR B 2 C57' C 0.432(3) 0.8614(19) 0.1459(9) 0.106(11) Uiso 0.35 1 d PD B 2 H57C H 0.5337 0.8928 0.1465 0.127 Uiso 0.35 1 calc PR B 2 H57D H 0.4674 0.8232 0.1691 0.127 Uiso 0.35 1 calc PR B 2 C58' C 0.2514(12) 0.8912(5) 0.1651(4) 0.118(15) Uiso 0.35 1 d PD B 2 H58C H 0.2761 0.9152 0.2012 0.141 Uiso 0.35 1 calc PR B 2 H58D H 0.2093 0.9227 0.1356 0.141 Uiso 0.35 1 calc PR B 2 C59 C -0.3019(12) 0.8031(5) 0.2591(4) 0.094(3) Uani 1 1 d R . . H59 H -0.3909 0.7698 0.2596 0.113 Uiso 1 1 calc R . . C60 C -0.1779(14) 0.8006(5) 0.2174(4) 0.104(3) Uani 1 1 d . A . H60 H -0.1872 0.7679 0.1891 0.124 Uiso 1 1 calc R . . C61 C -0.0350(11) 0.8458(5) 0.2152(3) 0.075(2) Uani 1 1 d . A . C62 C -0.0387(18) 0.8938(4) 0.2579(4) 0.109(4) Uani 1 1 d . . . H62 H 0.0518 0.9266 0.2592 0.131 Uiso 1 1 calc R B . C63 C -0.176(2) 0.8929(5) 0.2981(4) 0.117(4) Uani 1 1 d . A . H63 H -0.1739 0.9260 0.3262 0.141 Uiso 1 1 calc R . . C64 C 0.5756(11) 0.8256(4) -0.0556(4) 0.074(2) Uani 1 1 d . B . H64 H 0.5470 0.8046 -0.0910 0.088 Uiso 1 1 calc R . . C65 C 0.4529(11) 0.8184(4) -0.0123(4) 0.069(2) Uani 1 1 d . . . H65 H 0.3457 0.7931 -0.0183 0.083 Uiso 1 1 calc R B . C66 C 0.4879(10) 0.8489(5) 0.0410(3) 0.0701(18) Uani 1 1 d . B . C67 C 0.6507(14) 0.8851(4) 0.0456(4) 0.088(3) Uani 1 1 d . . . H67 H 0.6819 0.9067 0.0804 0.106 Uiso 1 1 calc R B . C68 C 0.7648(12) 0.8891(4) -0.0004(4) 0.081(2) Uani 1 1 d . B . H68 H 0.8730 0.9141 0.0046 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0834(5) 0.0516(4) 0.0687(4) 0.0020(5) -0.0081(4) 0.0117(5) Zn2 0.0616(5) 0.0558(5) 0.0885(5) -0.0100(6) -0.0088(4) 0.0022(5) O1 0.137(7) 0.131(6) 0.124(6) -0.007(5) -0.005(5) -0.058(6) O2 0.110(5) 0.114(5) 0.091(4) -0.026(4) 0.001(4) -0.001(4) O3 0.111(10) 0.063(6) 0.087(7) -0.015(5) 0.014(7) -0.012(7) O4 0.080(6) 0.050(5) 0.131(8) -0.017(5) -0.025(5) 0.003(4) O3' 0.045(12) 0.092(17) 0.28(4) -0.01(2) 0.077(18) -0.025(11) O4' 0.073(10) 0.067(9) 0.064(8) 0.022(7) 0.002(7) 0.002(7) O5 0.098(5) 0.127(5) 0.071(4) -0.015(4) 0.004(3) 0.006(4) O6 0.090(4) 0.094(5) 0.098(5) -0.038(4) 0.016(3) 0.010(4) O7 0.127(6) 0.069(4) 0.165(7) -0.038(4) 0.079(5) -0.035(4) O8 0.060(3) 0.045(3) 0.162(6) 0.013(4) -0.006(3) 0.001(2) O9 0.105(5) 0.066(4) 0.136(5) -0.002(4) -0.003(4) 0.031(3) O10 0.087(4) 0.059(3) 0.086(4) -0.011(3) 0.017(3) 0.001(3) O11 0.078(4) 0.058(3) 0.102(4) 0.010(3) 0.000(3) 0.000(3) O12 0.127(6) 0.075(4) 0.110(5) 0.011(4) -0.045(4) 0.002(4) O13 0.085(4) 0.116(5) 0.120(5) 0.025(4) 0.015(4) 0.040(4) O14 0.095(4) 0.073(4) 0.098(4) 0.002(3) 0.009(4) 0.010(3) O15 0.105(5) 0.066(3) 0.101(4) 0.012(3) 0.037(4) 0.001(3) O16 0.109(5) 0.063(4) 0.090(4) 0.003(3) 0.008(3) -0.009(3) N1 0.054(3) 0.059(4) 0.059(3) -0.006(3) 0.010(2) 0.005(3) N2 0.056(3) 0.063(3) 0.060(3) -0.003(3) 0.008(2) 0.015(3) N3 0.060(3) 0.047(3) 0.066(3) 0.004(4) 0.004(2) 0.007(4) N4 0.059(3) 0.047(3) 0.076(3) -0.012(4) 0.009(2) 0.006(4) N5 0.099(5) 0.084(5) 0.067(3) -0.017(4) -0.010(3) -0.035(4) N6 0.082(4) 0.086(5) 0.071(3) -0.012(4) 0.000(3) -0.021(4) N7 0.106(5) 0.053(3) 0.070(3) -0.001(4) -0.003(3) 0.019(5) N8 0.069(4) 0.054(4) 0.075(3) -0.001(3) -0.022(3) 0.009(3) C1 0.108(7) 0.063(5) 0.083(5) -0.019(4) 0.010(5) -0.003(5) C2 0.138(8) 0.058(5) 0.083(6) -0.008(4) 0.016(5) -0.006(5) C3 0.117(8) 0.061(5) 0.109(7) -0.010(5) 0.020(6) -0.023(5) C4 0.110(8) 0.121(9) 0.099(7) -0.004(6) 0.005(6) -0.049(7) C5 0.117(8) 0.098(7) 0.097(7) -0.014(5) 0.023(6) -0.031(6) C6 0.091(7) 0.101(7) 0.074(6) 0.004(5) 0.001(5) -0.008(6) C7 0.100(9) 0.079(7) 0.089(7) 0.011(6) 0.019(6) -0.002(6) C8 0.089(7) 0.159(11) 0.158(10) -0.067(9) -0.011(7) 0.036(7) C9 0.32(2) 0.196(15) 0.085(8) -0.033(8) 0.073(11) -0.135(16) C10 0.241(19) 0.083(9) 0.228(18) 0.007(10) -0.029(15) 0.023(11) C11 0.060(4) 0.054(4) 0.058(4) 0.009(3) 0.009(3) 0.011(3) C12 0.069(5) 0.051(4) 0.110(6) -0.007(4) 0.024(5) -0.009(4) C13 0.051(4) 0.044(4) 0.076(4) 0.008(3) 0.013(3) 0.000(3) C14 0.065(5) 0.067(5) 0.082(5) 0.011(4) 0.018(4) 0.003(4) C15 0.070(5) 0.096(6) 0.078(5) -0.003(5) 0.014(4) 0.008(5) C16 0.060(5) 0.100(7) 0.093(7) -0.023(5) 0.017(4) 0.000(5) C17 0.050(5) 0.047(5) 0.133(8) -0.019(5) 0.019(5) -0.009(4) C18 0.102(7) 0.079(6) 0.123(8) -0.007(6) -0.022(6) 0.018(5) C19 0.221(14) 0.067(6) 0.126(8) -0.023(6) 0.098(9) -0.055(8) C20 0.055(5) 0.080(6) 0.143(8) -0.043(6) 0.015(5) -0.007(4) C21 0.048(4) 0.045(4) 0.068(4) -0.001(3) 0.011(3) 0.005(3) C22 0.044(4) 0.042(3) 0.079(4) -0.006(3) -0.001(3) 0.005(3) C23 0.049(4) 0.053(4) 0.086(5) 0.000(4) 0.005(3) 0.005(3) C24 0.084(6) 0.066(5) 0.099(6) -0.008(5) 0.016(5) 0.004(4) C25 0.089(6) 0.066(5) 0.096(6) 0.016(4) 0.026(5) 0.009(4) C26 0.063(5) 0.037(4) 0.101(6) 0.000(4) -0.009(4) 0.002(3) C27 0.061(5) 0.059(4) 0.067(5) 0.004(4) -0.006(4) 0.012(4) C28 0.039(4) 0.085(6) 0.149(8) -0.031(6) 0.011(4) 0.004(4) C29 0.094(6) 0.055(4) 0.087(5) 0.006(4) -0.003(4) 0.008(4) C30 0.046(4) 0.068(5) 0.105(6) -0.003(4) 0.005(4) 0.007(4) C31 0.099(6) 0.070(5) 0.080(5) 0.023(4) 0.014(5) 0.031(5) C32 0.051(4) 0.075(5) 0.092(5) -0.006(4) -0.010(4) 0.011(4) C33 0.071(5) 0.062(5) 0.094(5) 0.010(4) 0.008(4) 0.005(4) C34 0.067(5) 0.078(6) 0.110(6) -0.003(5) 0.003(5) -0.005(4) C35 0.093(7) 0.106(8) 0.139(9) -0.031(7) 0.044(6) -0.028(6) C36 0.074(6) 0.073(5) 0.081(6) 0.018(4) 0.003(4) 0.015(4) C37 0.049(4) 0.069(5) 0.082(5) -0.008(4) 0.011(4) -0.002(4) C38 0.210(14) 0.118(9) 0.102(7) 0.048(7) 0.024(8) 0.060(9) C39 0.052(5) 0.170(12) 0.162(11) -0.029(9) -0.011(6) -0.011(6) C40 0.100(6) 0.059(5) 0.075(5) 0.016(4) 0.004(4) 0.004(4) C41 0.063(5) 0.094(6) 0.071(5) -0.025(4) 0.004(4) 0.006(4) C42 0.070(5) 0.088(6) 0.072(5) -0.013(4) 0.002(4) 0.031(4) C43 0.076(5) 0.102(7) 0.057(4) -0.006(4) 0.004(3) 0.048(5) C44 0.060(5) 0.089(6) 0.079(5) -0.011(4) 0.007(4) 0.031(4) C45 0.075(5) 0.051(4) 0.061(4) 0.004(3) 0.011(4) 0.005(4) C46 0.060(4) 0.038(3) 0.066(4) 0.004(3) 0.009(3) 0.010(3) C47 0.061(4) 0.045(3) 0.054(3) -0.002(4) 0.012(3) -0.009(4) C48 0.066(5) 0.058(4) 0.061(4) -0.003(3) 0.019(4) 0.010(3) C49 0.062(4) 0.052(4) 0.066(4) 0.006(3) 0.016(4) 0.005(3) C50 0.058(4) 0.062(4) 0.077(5) 0.011(4) 0.005(4) 0.022(4) C51 0.064(4) 0.059(4) 0.064(4) -0.008(3) 0.007(4) 0.018(4) C52 0.053(3) 0.048(3) 0.059(3) 0.002(4) 0.007(3) 0.007(4) C53 0.071(5) 0.047(4) 0.082(5) -0.004(4) -0.007(4) 0.016(3) C54 0.083(5) 0.043(4) 0.074(5) -0.008(3) -0.001(4) 0.015(4) C55 0.129(12) 0.052(7) 0.065(7) -0.010(6) 0.038(7) -0.025(7) C56 0.095(13) 0.130(16) 0.17(2) -0.119(16) 0.051(11) -0.078(11) C57 0.077(8) 0.051(7) 0.062(7) -0.010(5) 0.003(6) -0.021(6) C58 0.125(12) 0.073(9) 0.060(7) -0.013(7) -0.030(8) -0.001(8) C59 0.081(6) 0.104(7) 0.097(6) -0.041(6) 0.005(5) -0.001(5) C60 0.094(7) 0.116(8) 0.101(7) -0.059(6) 0.007(6) -0.037(6) C61 0.093(5) 0.070(5) 0.061(4) -0.005(5) -0.001(4) -0.010(5) C62 0.180(11) 0.054(5) 0.095(6) -0.021(5) 0.031(7) -0.042(6) C63 0.228(13) 0.058(5) 0.069(5) -0.014(4) 0.049(7) -0.022(7) C64 0.062(5) 0.066(5) 0.092(6) -0.022(4) -0.014(4) 0.001(4) C65 0.059(5) 0.062(4) 0.087(5) -0.021(4) -0.007(4) -0.004(4) C66 0.073(4) 0.059(4) 0.077(4) -0.008(5) -0.015(4) 0.004(5) C67 0.115(7) 0.075(5) 0.074(5) -0.005(4) 0.004(5) -0.028(5) C68 0.077(6) 0.070(5) 0.096(6) -0.009(5) -0.018(5) -0.023(4) _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 Zn1 O3 1.889(10) . ? Zn1 O8 2.021(6) . ? Zn1 N7 2.031(6) . ? Zn1 N3 2.040(5) . ? Zn1 O3' 2.20(2) . ? Zn2 O11 2.031(6) . ? Zn2 N4 2.039(5) . ? Zn2 N8 2.057(6) 1_556 ? Zn2 O15 2.103(5) . ? Zn2 O16 2.280(6) . ? Zn2 O12 2.415(7) . ? Zn2 C37 2.534(8) . ? Zn2 C27 2.572(8) . ? O1 C6 1.204(11) . ? O2 C6 1.294(10) . ? O3 C7 1.191(12) . ? O4 C7 1.357(13) . ? O3' C7 1.225(18) . ? O4' C7 1.306(18) . ? O5 C16 1.206(11) . ? O6 C16 1.284(11) . ? O7 C17 1.290(11) . ? O8 C17 1.228(11) . ? O9 C26 1.186(9) . ? O10 C26 1.320(10) . ? O11 C27 1.262(9) . ? O12 C27 1.222(9) . ? O13 C36 1.301(10) . ? O14 C36 1.215(10) . ? O15 C37 1.223(9) . ? O16 C37 1.204(10) . ? N1 C47 1.370(8) . ? N1 C41 1.453(9) . ? N1 C44 1.462(9) . ? N2 C52 1.372(8) . ? N2 C42 1.448(9) . ? N2 C43 1.450(8) . ? N3 C49 1.341(9) . ? N3 C45 1.350(9) . ? N4 C50 1.343(9) . ? N4 C54 1.357(9) . ? N5 C61 1.354(9) . ? N5 C55 1.440(11) . ? N5 C58 1.453(12) . ? N5 C58' 1.465(11) . ? N5 C55' 1.488(18) . ? N6 C66 1.350(9) . ? N6 C56 1.454(13) . ? N6 C57 1.461(10) . ? N6 C56' 1.470(18) . ? N6 C57' 1.477(17) . ? N7 C63 1.315(13) . ? N7 C59 1.335(11) . ? N8 C68 1.334(10) . ? N8 C64 1.341(9) . ? N8 Zn2 2.057(6) 1_554 ? C1 C8 1.493(13) . ? C1 C2 1.507(12) . ? C1 C6 1.540(13) . ? C1 C5 1.550(13) . ? C2 C10 1.512(18) . ? C2 C3 1.513(13) . ? C2 C9 1.522(14) . ? C3 C4 1.410(13) . ? C3 C7 1.477(13) . ? C4 C5 1.599(14) . ? C11 C16 1.480(12) . ? C11 C12 1.535(10) . ? C11 C18 1.546(11) . ? C11 C15 1.557(11) . ? C12 C20 1.506(13) . ? C12 C19 1.547(13) . ? C12 C13 1.555(11) . ? C13 C17 1.508(11) . ? C13 C14 1.539(10) . ? C14 C15 1.504(11) . ? C21 C28 1.504(10) . ? C21 C25 1.532(11) . ? C21 C26 1.533(10) . ? C21 C22 1.578(9) . ? C22 C29 1.494(10) . ? C22 C30 1.540(9) . ? C22 C23 1.551(9) . ? C23 C27 1.506(11) . ? C23 C24 1.520(11) . ? C24 C25 1.576(12) . ? C31 C36 1.510(12) . ? C31 C38 1.512(12) . ? C31 C35 1.539(13) . ? C31 C32 1.600(12) . ? C32 C39 1.516(12) . ? C32 C33 1.549(11) . ? C32 C40 1.554(11) . ? C33 C37 1.537(11) . ? C33 C34 1.551(12) . ? C34 C35 1.571(13) . ? C41 C42 1.422(11) . ? C43 C44 1.480(10) . ? C45 C46 1.361(10) . ? C46 C47 1.408(9) . ? C47 C48 1.410(10) . ? C48 C49 1.341(10) . ? C50 C51 1.356(10) . ? C51 C52 1.424(10) . ? C52 C53 1.391(10) . ? C53 C54 1.333(10) . ? C55 C56 1.455(16) . ? C57 C58 1.446(13) . ? C55' C56' 1.451(19) . ? C57' C58' 1.503(18) . ? C59 C60 1.320(12) . ? C60 C61 1.377(12) . ? C61 C62 1.383(12) . ? C62 C63 1.363(14) . ? C64 C65 1.349(11) . ? C65 C66 1.381(10) . ? C66 C67 1.378(12) . ? C67 C68 1.351(12) . ? 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 O3 Zn1 O8 113.0(5) . . ? O3 Zn1 N7 92.0(4) . . ? O8 Zn1 N7 136.7(3) . . ? O3 Zn1 N3 123.2(4) . . ? O8 Zn1 N3 97.3(3) . . ? N7 Zn1 N3 97.2(2) . . ? O3 Zn1 O3' 19.5(7) . . ? O8 Zn1 O3' 93.8(7) . . ? N7 Zn1 O3' 109.4(9) . . ? N3 Zn1 O3' 126.5(7) . . ? O11 Zn2 N4 142.6(3) . . ? O11 Zn2 N8 96.6(2) . 1_556 ? N4 Zn2 N8 98.0(2) . 1_556 ? O11 Zn2 O15 109.7(2) . . ? N4 Zn2 O15 105.0(3) . . ? N8 Zn2 O15 88.4(3) 1_556 . ? O11 Zn2 O16 92.7(2) . . ? N4 Zn2 O16 94.6(2) . . ? N8 Zn2 O16 145.2(2) 1_556 . ? O15 Zn2 O16 56.9(2) . . ? O11 Zn2 O12 57.0(2) . . ? N4 Zn2 O12 85.9(2) . . ? N8 Zn2 O12 119.7(3) 1_556 . ? O15 Zn2 O12 148.5(3) . . ? O16 Zn2 O12 93.4(3) . . ? O11 Zn2 C37 104.5(2) . . ? N4 Zn2 C37 99.1(3) . . ? N8 Zn2 C37 117.1(3) 1_556 . ? O15 Zn2 C37 28.7(2) . . ? O16 Zn2 C37 28.3(2) . . ? O12 Zn2 C37 121.5(3) . . ? O11 Zn2 C27 28.9(2) . . ? N4 Zn2 C27 113.9(3) . . ? N8 Zn2 C27 110.7(3) 1_556 . ? O15 Zn2 C27 132.8(3) . . ? O16 Zn2 C27 93.3(2) . . ? O12 Zn2 C27 28.1(2) . . ? C37 Zn2 C27 116.0(3) . . ? C7 O3 Zn1 116.1(9) . . ? C7 O3' Zn1 96.7(14) . . ? C17 O8 Zn1 106.9(6) . . ? C27 O11 Zn2 100.1(5) . . ? C27 O12 Zn2 83.1(5) . . ? C37 O15 Zn2 95.6(5) . . ? C37 O16 Zn2 87.6(5) . . ? C47 N1 C41 121.1(5) . . ? C47 N1 C44 118.8(6) . . ? C41 N1 C44 113.2(6) . . ? C52 N2 C42 122.5(6) . . ? C52 N2 C43 120.3(5) . . ? C42 N2 C43 110.1(6) . . ? C49 N3 C45 114.5(6) . . ? C49 N3 Zn1 122.5(5) . . ? C45 N3 Zn1 122.7(5) . . ? C50 N4 C54 113.9(6) . . ? C50 N4 Zn2 123.7(5) . . ? C54 N4 Zn2 122.2(5) . . ? C61 N5 C55 119.1(8) . . ? C61 N5 C58 121.8(7) . . ? C55 N5 C58 108.1(10) . . ? C61 N5 C58' 129.5(7) . . ? C55 N5 C58' 111.1(8) . . ? C58 N5 C58' 27.6(7) . . ? C61 N5 C55' 125.0(14) . . ? C55 N5 C55' 45.6(15) . . ? C58 N5 C55' 111.9(15) . . ? C58' N5 C55' 94.0(16) . . ? C66 N6 C56 125.1(9) . . ? C66 N6 C57 121.7(8) . . ? C56 N6 C57 109.0(9) . . ? C66 N6 C56' 115.0(13) . . ? C56 N6 C56' 11.0(15) . . ? C57 N6 C56' 120.1(14) . . ? C66 N6 C57' 120.3(12) . . ? C56 N6 C57' 113.6(15) . . ? C57 N6 C57' 32.3(11) . . ? C56' N6 C57' 122.3(19) . . ? C63 N7 C59 113.5(7) . . ? C63 N7 Zn1 120.0(6) . . ? C59 N7 Zn1 126.1(7) . . ? C68 N8 C64 113.2(7) . . ? C68 N8 Zn2 123.7(6) . 1_554 ? C64 N8 Zn2 121.9(5) . 1_554 ? C8 C1 C2 110.4(9) . . ? C8 C1 C6 108.5(8) . . ? C2 C1 C6 114.8(8) . . ? C8 C1 C5 107.4(9) . . ? C2 C1 C5 103.2(7) . . ? C6 C1 C5 112.3(8) . . ? C1 C2 C10 108.9(10) . . ? C1 C2 C3 101.0(7) . . ? C10 C2 C3 110.2(10) . . ? C1 C2 C9 115.1(10) . . ? C10 C2 C9 104.8(12) . . ? C3 C2 C9 116.7(10) . . ? C4 C3 C7 116.4(9) . . ? C4 C3 C2 109.6(8) . . ? C7 C3 C2 121.0(9) . . ? C3 C4 C5 104.3(8) . . ? C1 C5 C4 104.2(7) . . ? O1 C6 O2 123.2(9) . . ? O1 C6 C1 124.0(9) . . ? O2 C6 C1 112.5(9) . . ? O3 C7 O3' 36.5(9) . . ? O3 C7 O4' 95.8(13) . . ? O3' C7 O4' 131.5(15) . . ? O3 C7 O4 114.0(10) . . ? O3' C7 O4 103.0(19) . . ? O4' C7 O4 87.3(10) . . ? O3 C7 C3 128.4(11) . . ? O3' C7 C3 120.9(17) . . ? O4' C7 C3 93.7(11) . . ? O4 C7 C3 117.1(9) . . ? C16 C11 C12 114.4(6) . . ? C16 C11 C18 110.4(7) . . ? C12 C11 C18 112.1(7) . . ? C16 C11 C15 111.9(7) . . ? C12 C11 C15 99.8(6) . . ? C18 C11 C15 107.6(7) . . ? C20 C12 C11 111.1(7) . . ? C20 C12 C19 105.2(8) . . ? C11 C12 C19 114.3(7) . . ? C20 C12 C13 112.8(7) . . ? C11 C12 C13 104.9(6) . . ? C19 C12 C13 108.9(8) . . ? C17 C13 C14 113.0(6) . . ? C17 C13 C12 113.7(6) . . ? C14 C13 C12 107.6(6) . . ? C15 C14 C13 103.7(6) . . ? C14 C15 C11 108.5(6) . . ? O5 C16 O6 120.1(9) . . ? O5 C16 C11 124.0(9) . . ? O6 C16 C11 115.9(8) . . ? O8 C17 O7 121.8(8) . . ? O8 C17 C13 121.5(9) . . ? O7 C17 C13 116.7(9) . . ? C28 C21 C25 110.5(7) . . ? C28 C21 C26 108.1(6) . . ? C25 C21 C26 112.4(6) . . ? C28 C21 C22 114.0(6) . . ? C25 C21 C22 102.5(6) . . ? C26 C21 C22 109.4(5) . . ? C29 C22 C30 107.9(6) . . ? C29 C22 C23 112.5(6) . . ? C30 C22 C23 110.2(6) . . ? C29 C22 C21 115.2(6) . . ? C30 C22 C21 108.8(5) . . ? C23 C22 C21 102.2(5) . . ? C27 C23 C24 115.5(7) . . ? C27 C23 C22 112.2(6) . . ? C24 C23 C22 108.0(6) . . ? C23 C24 C25 105.7(6) . . ? C21 C25 C24 104.2(6) . . ? O9 C26 O10 124.5(8) . . ? O9 C26 C21 122.1(8) . . ? O10 C26 C21 113.2(6) . . ? O12 C27 O11 119.8(8) . . ? O12 C27 C23 122.0(7) . . ? O11 C27 C23 118.2(7) . . ? O12 C27 Zn2 68.7(5) . . ? O11 C27 Zn2 51.0(4) . . ? C23 C27 Zn2 169.0(6) . . ? C36 C31 C38 111.5(8) . . ? C36 C31 C35 112.4(8) . . ? C38 C31 C35 109.9(9) . . ? C36 C31 C32 108.8(7) . . ? C38 C31 C32 112.2(9) . . ? C35 C31 C32 101.7(7) . . ? C39 C32 C33 112.8(8) . . ? C39 C32 C40 107.2(8) . . ? C33 C32 C40 112.1(6) . . ? C39 C32 C31 116.6(8) . . ? C33 C32 C31 98.8(6) . . ? C40 C32 C31 109.4(6) . . ? C37 C33 C32 118.0(7) . . ? C37 C33 C34 109.4(7) . . ? C32 C33 C34 104.3(7) . . ? C33 C34 C35 104.1(7) . . ? C31 C35 C34 106.7(8) . . ? O14 C36 O13 123.9(8) . . ? O14 C36 C31 121.9(7) . . ? O13 C36 C31 114.2(8) . . ? O16 C37 O15 119.3(8) . . ? O16 C37 C33 126.5(7) . . ? O15 C37 C33 113.7(7) . . ? O16 C37 Zn2 64.0(5) . . ? O15 C37 Zn2 55.7(4) . . ? C33 C37 Zn2 163.1(6) . . ? C42 C41 N1 114.5(7) . . ? C41 C42 N2 114.5(7) . . ? N2 C43 C44 113.0(6) . . ? N1 C44 C43 111.0(6) . . ? N3 C45 C46 124.6(7) . . ? C45 C46 C47 120.2(6) . . ? N1 C47 C46 122.5(6) . . ? N1 C47 C48 122.8(6) . . ? C46 C47 C48 114.7(6) . . ? C49 C48 C47 120.5(6) . . ? N3 C49 C48 125.5(6) . . ? N4 C50 C51 126.0(6) . . ? C50 C51 C52 118.6(6) . . ? N2 C52 C53 122.4(6) . . ? N2 C52 C51 122.3(6) . . ? C53 C52 C51 115.3(6) . . ? C54 C53 C52 121.2(7) . . ? C53 C54 N4 124.9(7) . . ? N5 C55 C56 106.9(10) . . ? N6 C56 C55 116.7(14) . . ? C58 C57 N6 116.1(9) . . ? C57 C58 N5 109.8(9) . . ? C56' C55' N5 124(2) . . ? C55' C56' N6 102(2) . . ? N6 C57' C58' 97.6(12) . . ? N5 C58' C57' 115.4(17) . . ? C60 C59 N7 125.6(9) . . ? C59 C60 C61 121.1(8) . . ? N5 C61 C60 123.8(8) . . ? N5 C61 C62 121.6(9) . . ? C60 C61 C62 114.7(8) . . ? C63 C62 C61 119.6(9) . . ? N7 C63 C62 125.4(8) . . ? N8 C64 C65 125.9(7) . . ? C64 C65 C66 119.5(7) . . ? N6 C66 C67 122.2(7) . . ? N6 C66 C65 121.9(8) . . ? C67 C66 C65 115.9(7) . . ? C68 C67 C66 120.1(8) . . ? N8 C68 C67 125.4(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.589 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.114 # Attachment '- SI_cpd 4.cif' data_cpd4 _database_code_depnum_ccdc_archive 'CCDC 790240' #TrackingRef '- SI_cpd 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Co2 N4 O7' _chemical_formula_weight 632.43 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 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 21.088(4) _cell_length_b 12.195(2) _cell_length_c 12.630(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.74(3) _cell_angle_gamma 90.00 _cell_volume 2791.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3374 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 24.78 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7002 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '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 8990 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4429 _reflns_number_gt 3543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+9.4461P] 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 0.05(4) _refine_ls_number_reflns 4429 _refine_ls_number_parameters 353 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.28887(6) 0.71291(7) 0.29561(10) 0.0408(3) Uani 1 1 d . . . Co2 Co 0.29087(7) 0.97983(8) 0.30108(12) 0.0502(4) Uani 1 1 d . . . O1 O 0.3764(4) 0.6053(6) 0.2722(6) 0.0436(17) Uani 1 1 d . . . O2 O 0.2572(4) 0.5780(6) 0.1945(6) 0.0459(18) Uani 1 1 d . . . O3 O 0.2583(4) 0.1151(6) 0.1961(7) 0.0498(19) Uani 1 1 d . . . O4 O 0.3761(4) 0.0828(6) 0.2778(7) 0.0465(18) Uani 1 1 d . . . O5 O 0.32217(15) 0.8462(7) 0.2594(3) 0.0370(8) Uani 1 1 d . . . H101 H 0.3699 0.8480 0.2627 0.055 Uiso 1 1 d R . . O6 O 0.1873(3) 0.7573(5) 0.2592(6) 0.0495(17) Uani 1 1 d . . . O7 O 0.1916(4) 0.9371(6) 0.2731(8) 0.071(2) Uani 1 1 d . . . N1 N 0.4615(4) 1.0491(7) 0.8692(8) 0.0436(19) Uani 1 1 d . . . N2 N 0.4602(4) 0.6822(6) 0.8680(7) 0.044(2) Uani 1 1 d . . . N3 N 0.3438(5) 1.0080(7) 0.4847(8) 0.053(3) Uani 1 1 d . . . N4 N 0.3451(4) 0.6909(7) 0.4821(7) 0.046(2) Uani 1 1 d . . . C1 C 0.3212(5) 0.4421(9) 0.1460(8) 0.045(3) Uani 1 1 d . . . C2 C 0.3510(3) 0.3435(11) 0.2378(5) 0.0546(19) Uani 1 1 d . . . C3 C 0.3291(5) 0.2438(8) 0.1548(7) 0.041(2) Uani 1 1 d . . . H3 H 0.3668 0.2314 0.1329 0.049 Uiso 1 1 calc R . . C4 C 0.2545(7) 0.2751(12) 0.0340(10) 0.085(4) Uani 1 1 d . . . H4A H 0.2584 0.2640 -0.0385 0.102 Uiso 1 1 calc R . . H4B H 0.2139 0.2313 0.0263 0.102 Uiso 1 1 calc R . . C5 C 0.2430(6) 0.3967(10) 0.0500(9) 0.080(4) Uani 1 1 d . . . H5A H 0.2092 0.4052 0.0801 0.096 Uiso 1 1 calc R . . H5B H 0.2231 0.4354 -0.0278 0.096 Uiso 1 1 calc R . . C6 C 0.3195(6) 0.5460(9) 0.2081(9) 0.044(3) Uani 1 1 d . . . C7 C 0.3218(5) 0.1411(9) 0.2140(9) 0.042(2) Uani 1 1 d . . . C8 C 0.3636(4) 0.4574(8) 0.0806(7) 0.071(2) Uani 1 1 d . . . H8A H 0.3403 0.5132 0.0187 0.107 Uiso 1 1 calc R . . H8B H 0.3643 0.3897 0.0424 0.107 Uiso 1 1 calc R . . H8C H 0.4133 0.4791 0.1389 0.107 Uiso 1 1 calc R . . C9 C 0.4355(3) 0.3438(11) 0.3207(6) 0.064(2) Uani 1 1 d . . . H9A H 0.4575 0.3347 0.2709 0.096 Uiso 1 1 calc R . . H9B H 0.4505 0.2847 0.3789 0.096 Uiso 1 1 calc R . . H9C H 0.4512 0.4123 0.3642 0.096 Uiso 1 1 calc R . . C10 C 0.3180(2) 0.3420(11) 0.3226(4) 0.0353(12) Uani 1 1 d . . . H10A H 0.3422 0.3964 0.3858 0.053 Uiso 1 1 calc R . . H10B H 0.3253 0.2709 0.3597 0.053 Uiso 1 1 calc R . . H10C H 0.2662 0.3577 0.2748 0.053 Uiso 1 1 calc R . . C11 C 0.1597(2) 0.8495(10) 0.2553(4) 0.0345(11) Uani 1 1 d . . . C12 C 0.0810(2) 0.8531(11) 0.2261(6) 0.0535(15) Uani 1 1 d . . . H12A H 0.0784 0.8940 0.2888 0.080 Uiso 1 1 calc R . . H12B H 0.0636 0.7798 0.2233 0.080 Uiso 1 1 calc R . . H12C H 0.0507 0.8879 0.1477 0.080 Uiso 1 1 calc R . . C13 C 0.5410(6) 1.0816(10) 0.9525(11) 0.023(3) Uiso 0.50 1 d P . 1 H13A H 0.5688 1.0387 0.9254 0.028 Uiso 0.50 1 calc PR . 1 H13B H 0.5443 1.1572 0.9319 0.028 Uiso 0.50 1 calc PR . 1 C14 C 0.4286(7) 1.0778(11) 0.9501(12) 0.031(3) Uiso 0.50 1 d P . 1 H14A H 0.4052 1.1488 0.9221 0.038 Uiso 0.50 1 calc PR . 1 H14B H 0.3892 1.0255 0.9286 0.038 Uiso 0.50 1 calc PR . 1 C13' C 0.5346(8) 1.0197(14) 0.9261(13) 0.037(4) Uiso 0.50 1 d P . 2 H13C H 0.5582 1.0657 0.8935 0.044 Uiso 0.50 1 calc PR . 2 H13D H 0.5372 0.9448 0.9029 0.044 Uiso 0.50 1 calc PR . 2 C14' C 0.4168(9) 1.0278(14) 0.9223(13) 0.025(3) Uiso 0.50 1 d P . 2 H14C H 0.3904 0.9594 0.8894 0.030 Uiso 0.50 1 calc PR . 2 H14D H 0.3805 1.0858 0.8986 0.030 Uiso 0.50 1 calc PR . 2 C15 C 0.4183(5) 1.0340(8) 0.5486(9) 0.043(2) Uani 1 1 d . . . H15 H 0.4422 1.0418 0.5043 0.051 Uiso 1 1 calc R . . C16 C 0.4574(5) 1.0483(8) 0.6705(9) 0.039(2) Uani 1 1 d . . . H16 H 0.5072 1.0664 0.7086 0.047 Uiso 1 1 calc R . . C17 C 0.4235(5) 1.0360(7) 0.7424(10) 0.040(2) Uani 1 1 d . . . C18 C 0.3466(6) 1.0098(10) 0.6768(10) 0.061(4) Uani 1 1 d . . . H18 H 0.3203 1.0018 0.7172 0.073 Uiso 1 1 calc R . . C19 C 0.3135(5) 0.9971(12) 0.5527(10) 0.068(4) Uani 1 1 d . . . H19 H 0.2637 0.9785 0.5113 0.081 Uiso 1 1 calc R . . C20 C 0.5414(7) 0.6537(12) 0.9470(12) 0.020(3) Uiso 0.50 1 d P . 1 H20A H 0.5463 0.5748 0.9451 0.024 Uiso 0.50 1 calc PR . 1 H20B H 0.5670 0.6859 0.9091 0.024 Uiso 0.50 1 calc PR . 1 C20' C 0.5333(6) 0.7164(13) 0.9242(10) 0.033(3) Uiso 0.50 1 d P . 2 H20C H 0.5350 0.7952 0.9156 0.039 Uiso 0.50 1 calc PR . 2 H20D H 0.5569 0.6821 0.8839 0.039 Uiso 0.50 1 calc PR . 2 C21 C 0.4243(4) 0.6851(9) 0.9362(8) 0.054(3) Uani 1 1 d . . . H21A H 0.4080 0.7599 0.9334 0.064 Uiso 1 1 calc R . . H21B H 0.3802 0.6405 0.8922 0.064 Uiso 1 1 calc R . . C22 C 0.4152(5) 0.6743(8) 0.5480(8) 0.044(3) Uani 1 1 d . . . H22 H 0.4401 0.6634 0.5058 0.053 Uiso 1 1 calc R . . C23 C 0.4567(5) 0.6711(7) 0.6744(8) 0.038(2) Uani 1 1 d . . . H23 H 0.5074 0.6600 0.7142 0.046 Uiso 1 1 calc R . . C24 C 0.4223(5) 0.6846(7) 0.7422(8) 0.037(2) Uani 1 1 d . . . C25 C 0.3464(5) 0.6971(11) 0.6720(8) 0.053(3) Uani 1 1 d . . . H25 H 0.3197 0.7010 0.7119 0.063 Uiso 1 1 calc R . . C26 C 0.3095(5) 0.7037(12) 0.5472(8) 0.056(3) Uani 1 1 d . . . H26 H 0.2590 0.7173 0.5047 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0245(6) 0.0596(9) 0.0401(6) 0.0217(7) 0.0179(5) 0.0169(6) Co2 0.0326(7) 0.0650(10) 0.0638(9) -0.0325(8) 0.0325(7) -0.0232(7) O1 0.021(4) 0.066(5) 0.041(4) 0.014(3) 0.014(3) 0.010(3) O2 0.025(4) 0.064(5) 0.054(4) 0.016(3) 0.024(3) 0.016(3) O3 0.023(4) 0.065(5) 0.061(5) -0.024(4) 0.021(3) -0.012(3) O4 0.029(4) 0.055(4) 0.063(5) -0.016(3) 0.029(4) -0.008(3) O5 0.0259(15) 0.057(2) 0.0313(16) 0.010(4) 0.0170(13) 0.005(4) O6 0.031(3) 0.049(4) 0.068(4) 0.019(3) 0.025(3) 0.008(3) O7 0.050(4) 0.071(5) 0.120(6) -0.067(4) 0.064(4) -0.046(4) N1 0.023(3) 0.057(5) 0.056(4) -0.005(3) 0.024(3) -0.008(3) N2 0.023(3) 0.068(5) 0.045(3) 0.025(3) 0.020(3) 0.012(3) N3 0.031(5) 0.074(7) 0.060(5) -0.041(5) 0.026(4) -0.032(4) N4 0.036(5) 0.062(6) 0.055(4) 0.024(4) 0.034(4) 0.015(4) C1 0.035(5) 0.077(7) 0.035(4) 0.011(4) 0.025(4) 0.019(4) C2 0.052(3) 0.077(5) 0.045(3) 0.039(6) 0.032(3) 0.033(6) C3 0.027(4) 0.064(6) 0.029(4) -0.009(4) 0.012(3) 0.008(4) C4 0.070(7) 0.119(10) 0.054(6) -0.001(6) 0.023(5) 0.016(6) C5 0.049(5) 0.119(10) 0.038(5) -0.009(4) -0.003(4) 0.033(5) C6 0.034(6) 0.068(7) 0.038(5) 0.017(5) 0.025(5) 0.005(5) C7 0.031(6) 0.053(6) 0.042(5) -0.027(4) 0.018(5) -0.016(5) C8 0.080(5) 0.091(7) 0.062(5) 0.034(5) 0.051(5) 0.029(5) C9 0.036(3) 0.084(5) 0.070(4) 0.053(6) 0.025(3) 0.022(6) C10 0.033(2) 0.046(3) 0.029(2) -0.002(4) 0.0171(19) 0.010(5) C11 0.025(2) 0.048(3) 0.028(2) -0.009(5) 0.0116(18) 0.009(5) C12 0.030(3) 0.036(4) 0.098(4) 0.004(7) 0.036(3) -0.003(5) C15 0.024(5) 0.049(5) 0.059(6) -0.014(4) 0.024(5) -0.013(4) C16 0.023(4) 0.046(5) 0.055(6) -0.006(4) 0.026(4) -0.011(3) C17 0.029(4) 0.039(5) 0.060(6) -0.015(4) 0.028(4) -0.012(3) C18 0.046(6) 0.087(9) 0.065(7) -0.042(6) 0.040(5) -0.037(6) C19 0.033(6) 0.107(10) 0.084(8) -0.053(8) 0.046(6) -0.044(6) C21 0.024(3) 0.087(7) 0.054(4) -0.035(5) 0.023(3) -0.014(4) C22 0.033(5) 0.065(7) 0.046(5) 0.030(4) 0.029(4) 0.019(4) C23 0.025(4) 0.039(5) 0.050(5) 0.014(4) 0.019(4) 0.006(3) C24 0.032(4) 0.041(5) 0.044(4) 0.014(4) 0.024(4) 0.009(3) C25 0.025(5) 0.092(8) 0.049(5) 0.026(6) 0.025(4) 0.021(5) C26 0.039(6) 0.092(8) 0.044(5) 0.032(7) 0.025(4) 0.034(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 1.916(8) . ? Co1 O2 1.978(7) . ? Co1 O6 2.021(7) . ? Co1 N4 2.042(7) . ? Co1 O1 2.403(7) . ? Co2 O5 1.930(8) . ? Co2 O7 2.005(6) . ? Co2 O3 2.006(8) 1_565 ? Co2 N3 2.024(8) . ? Co2 O4 2.331(7) 1_565 ? Co2 C7 2.497(12) 1_565 ? O1 C6 1.275(13) . ? O2 C6 1.296(11) . ? O3 C7 1.278(11) . ? O3 Co2 2.006(8) 1_545 ? O4 C7 1.234(13) . ? O4 Co2 2.331(7) 1_545 ? O6 C11 1.256(12) . ? O7 C11 1.221(13) . ? N1 C13' 1.375(17) . ? N1 C17 1.386(13) . ? N1 C14' 1.432(17) . ? N1 C13 1.507(14) . ? N1 C14 1.540(15) . ? N2 C24 1.366(11) . ? N2 C20' 1.390(14) . ? N2 C21 1.408(11) . ? N2 C20 1.516(14) . ? N3 C19 1.314(12) . ? N3 C15 1.387(12) . ? N4 C22 1.288(12) . ? N4 C26 1.377(11) . ? C1 C6 1.500(15) . ? C1 C8 1.509(10) . ? C1 C2 1.562(14) . ? C1 C5 1.566(14) . ? C2 C3 1.514(15) . ? C2 C9 1.538(7) . ? C2 C10 1.545(6) . ? C3 C7 1.506(15) . ? C3 C4 1.579(13) . ? C4 C5 1.533(11) . ? C7 Co2 2.497(12) 1_545 ? C11 C12 1.505(6) . ? C13 C14 1.058(16) 2_657 ? C14 C13 1.058(16) 2_657 ? C13' C14' 1.65(2) 2_657 ? C14' C13' 1.65(2) 2_657 ? C15 C16 1.336(13) . ? C16 C17 1.423(13) . ? C17 C18 1.430(14) . ? C18 C19 1.359(14) . ? C20 C21 1.325(15) 2_657 ? C20' C21 1.563(14) 2_657 ? C21 C20 1.325(15) 2_657 ? C21 C20' 1.563(14) 2_657 ? C22 C23 1.375(13) . ? C23 C24 1.386(13) . ? C24 C25 1.385(13) . ? C25 C26 1.357(12) . ? 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 Co1 O2 126.6(3) . . ? O5 Co1 O6 101.2(2) . . ? O2 Co1 O6 96.1(3) . . ? O5 Co1 N4 108.6(3) . . ? O2 Co1 N4 116.1(3) . . ? O6 Co1 N4 102.8(3) . . ? O5 Co1 O1 92.0(2) . . ? O2 Co1 O1 59.6(2) . . ? O6 Co1 O1 155.4(3) . . ? N4 Co1 O1 92.3(3) . . ? O5 Co2 O7 101.8(2) . . ? O5 Co2 O3 124.3(3) . 1_565 ? O7 Co2 O3 97.1(3) . 1_565 ? O5 Co2 N3 113.0(3) . . ? O7 Co2 N3 99.3(3) . . ? O3 Co2 N3 114.8(3) 1_565 . ? O5 Co2 O4 91.6(2) . 1_565 ? O7 Co2 O4 157.0(3) . 1_565 ? O3 Co2 O4 59.9(3) 1_565 1_565 ? N3 Co2 O4 92.5(3) . 1_565 ? O5 Co2 C7 110.0(3) . 1_565 ? O7 Co2 C7 127.7(4) . 1_565 ? O3 Co2 C7 30.6(3) 1_565 1_565 ? N3 Co2 C7 104.8(3) . 1_565 ? O4 Co2 C7 29.4(3) 1_565 1_565 ? C6 O1 Co1 81.7(6) . . ? C6 O2 Co1 100.4(7) . . ? C7 O3 Co2 96.5(7) . 1_545 ? C7 O4 Co2 82.8(6) . 1_545 ? Co1 O5 Co2 115.64(14) . . ? C11 O6 Co1 131.7(6) . . ? C11 O7 Co2 133.5(6) . . ? C13' N1 C17 113.9(9) . . ? C13' N1 C14' 122.6(11) . . ? C17 N1 C14' 112.9(9) . . ? C13' N1 C13 32.2(8) . . ? C17 N1 C13 128.1(8) . . ? C14' N1 C13 118.9(9) . . ? C13' N1 C14 118.5(10) . . ? C17 N1 C14 127.1(8) . . ? C14' N1 C14 26.3(7) . . ? C13 N1 C14 101.2(8) . . ? C24 N2 C20' 115.2(8) . . ? C24 N2 C21 122.2(7) . . ? C20' N2 C21 118.8(8) . . ? C24 N2 C20 124.3(8) . . ? C20' N2 C20 31.7(7) . . ? C21 N2 C20 112.5(8) . . ? C19 N3 C15 115.3(8) . . ? C19 N3 Co2 124.3(7) . . ? C15 N3 Co2 120.2(7) . . ? C22 N4 C26 115.3(8) . . ? C22 N4 Co1 124.3(7) . . ? C26 N4 Co1 120.1(6) . . ? C6 C1 C8 111.2(8) . . ? C6 C1 C2 111.7(8) . . ? C8 C1 C2 112.1(6) . . ? C6 C1 C5 114.0(8) . . ? C8 C1 C5 107.7(8) . . ? C2 C1 C5 99.7(9) . . ? C3 C2 C9 108.1(8) . . ? C3 C2 C10 112.6(9) . . ? C9 C2 C10 107.7(4) . . ? C3 C2 C1 103.9(5) . . ? C9 C2 C1 112.9(9) . . ? C10 C2 C1 111.7(8) . . ? C7 C3 C2 113.3(7) . . ? C7 C3 C4 112.1(9) . . ? C2 C3 C4 106.0(8) . . ? C5 C4 C3 104.7(10) . . ? C4 C5 C1 105.6(10) . . ? O1 C6 O2 118.4(10) . . ? O1 C6 C1 123.0(9) . . ? O2 C6 C1 118.6(9) . . ? O4 C7 O3 120.7(11) . . ? O4 C7 C3 120.5(9) . . ? O3 C7 C3 118.8(10) . . ? O4 C7 Co2 67.8(6) . 1_545 ? O3 C7 Co2 52.9(5) . 1_545 ? C3 C7 Co2 171.6(8) . 1_545 ? O7 C11 O6 125.1(4) . . ? O7 C11 C12 117.1(9) . . ? O6 C11 C12 117.9(10) . . ? C14 C13 N1 126.7(12) 2_657 . ? C13 C14 N1 124.8(12) 2_657 . ? N1 C13' C14' 117.2(13) . 2_657 ? N1 C14' C13' 112.8(12) . 2_657 ? C16 C15 N3 123.3(10) . . ? C15 C16 C17 120.4(9) . . ? N1 C17 C16 122.9(8) . . ? N1 C17 C18 120.7(9) . . ? C16 C17 C18 116.4(9) . . ? C19 C18 C17 117.1(10) . . ? N3 C19 C18 127.4(9) . . ? C21 C20 N2 117.2(10) 2_657 . ? N2 C20' C21 110.4(9) . 2_657 ? C20 C21 N2 121.1(9) 2_657 . ? C20 C21 C20' 30.9(8) 2_657 2_657 ? N2 C21 C20' 121.3(8) . 2_657 ? N4 C22 C23 126.4(9) . . ? C22 C23 C24 119.4(9) . . ? N2 C24 C25 123.1(8) . . ? N2 C24 C23 122.4(8) . . ? C25 C24 C23 114.6(8) . . ? C26 C25 C24 122.6(9) . . ? C25 C26 N4 121.5(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.951 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.073 # Attachment '- SI_cpd 5.cif' data_cpd5 _database_code_depnum_ccdc_archive 'CCDC 800211' #TrackingRef '- SI_cpd 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 N4 O7 Zn2' _chemical_formula_weight 645.31 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.623(3) _cell_length_b 12.253(3) _cell_length_c 18.244(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.69(3) _cell_angle_gamma 90.00 _cell_volume 2808.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7327 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.02 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6633 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 '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 18430 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.18 _reflns_number_total 8598 _reflns_number_gt 6773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^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 0.09(2) _refine_ls_number_reflns 8598 _refine_ls_number_parameters 702 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _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 Zn1 Zn 1.23702(8) 0.71149(9) 0.54199(6) 0.0324(4) Uani 1 1 d . . . Zn2 Zn 1.24130(9) 0.97584(10) 0.53269(6) 0.0389(4) Uani 1 1 d . . . Zn3 Zn 0.25676(7) 0.67890(6) 0.96784(5) 0.0190(3) Uani 1 1 d . . . Zn4 Zn 0.26803(8) 0.94218(7) 0.95545(6) 0.0244(3) Uani 1 1 d . . . O1 O 1.3577(5) 0.6000(6) 0.6334(4) 0.0398(19) Uani 1 1 d . . . O2 O 1.3056(5) 0.5752(6) 0.5145(3) 0.0352(18) Uani 1 1 d . . . O3 O 1.3123(5) 0.1117(6) 0.5095(3) 0.0357(17) Uani 1 1 d . . . O4 O 1.3593(5) 0.0805(6) 0.6271(4) 0.0401(19) Uani 1 1 d . . . O5 O 0.1322(5) 0.5666(5) 0.8732(4) 0.0285(16) Uani 1 1 d . . . O6 O 0.1843(5) 0.5428(5) 0.9912(3) 0.0270(16) Uani 1 1 d . . . O7 O 0.1465(5) 0.0504(5) 0.8701(3) 0.0293(16) Uani 1 1 d . . . O8 O 0.1978(5) 0.0758(5) 0.9866(3) 0.0255(15) Uani 1 1 d . . . O9 O 1.3107(5) 0.8444(6) 0.5702(4) 0.0402(19) Uani 1 1 d . . . H101 H 1.3401 0.8438 0.6108 0.060 Uiso 1 1 d R . . O10 O 1.1695(5) 0.7528(6) 0.4418(4) 0.0458(19) Uani 1 1 d . . . O11 O 1.1765(6) 0.9335(6) 0.4316(3) 0.047(2) Uani 1 1 d . . . O12 O 0.1881(4) 0.8098(5) 0.9333(3) 0.0208(14) Uani 1 1 d . . . H102 H 0.1609 0.8143 0.8929 0.031 Uiso 1 1 d R . . O13 O 0.3167(5) 0.7243(5) 1.0691(4) 0.0302(16) Uani 1 1 d . . . O14 O 0.3422(5) 0.9010(5) 1.0551(3) 0.0352(17) Uani 1 1 d . . . N1 N 0.8385(6) 0.6627(8) 0.7143(4) 0.043(2) Uani 1 1 d . . . N2 N 0.6545(5) 0.6422(7) 0.7936(4) 0.0269(18) Uani 1 1 d . . . N3 N 1.1072(6) 0.6889(7) 0.5973(4) 0.035(2) Uani 1 1 d . . . N4 N 0.3879(5) 0.6582(6) 0.9128(4) 0.0273(19) Uani 1 1 d . . . N5 N 0.8473(6) 1.0342(8) 0.7056(4) 0.048(3) Uani 1 1 d D . . N6 N 0.6638(6) 1.0252(7) 0.7845(4) 0.035(2) Uani 1 1 d D . . N7 N 1.1114(6) 1.0007(7) 0.5848(4) 0.031(2) Uani 1 1 d . . . N8 N 0.3967(6) 0.9678(6) 0.9013(4) 0.0249(18) Uani 1 1 d . . . C1 C 1.4220(7) 0.4431(10) 0.5711(5) 0.039(3) Uani 1 1 d . . . C2 C 1.3589(10) 0.3411(10) 0.5922(11) 0.097(6) Uani 1 1 d . . . C3 C 1.4222(7) 0.2486(10) 0.5762(6) 0.044(3) Uani 1 1 d . . . H3 H 1.4836 0.2442 0.6134 0.052 Uiso 1 1 calc R . . C4 C 1.4633(9) 0.2796(11) 0.4988(8) 0.075(4) Uani 1 1 d . . . H4A H 1.5398 0.2701 0.5001 0.090 Uiso 1 1 calc R . . H4B H 1.4285 0.2356 0.4594 0.090 Uiso 1 1 calc R . . C5 C 1.4330(9) 0.3979(10) 0.4895(7) 0.064(3) Uani 1 1 d . . . H5A H 1.3660 0.4052 0.4589 0.077 Uiso 1 1 calc R . . H5B H 1.4874 0.4379 0.4668 0.077 Uiso 1 1 calc R . . C6 C 1.3582(8) 0.5460(9) 0.5729(6) 0.039(3) Uani 1 1 d . . . C7 C 1.3627(8) 0.1368(9) 0.5730(6) 0.040(3) Uani 1 1 d . . . C8 C 1.5311(6) 0.4558(8) 0.6118(5) 0.064(3) Uani 1 1 d . . . H8A H 1.5667 0.5167 0.5920 0.096 Uiso 1 1 calc R . . H8B H 1.5717 0.3906 0.6063 0.096 Uiso 1 1 calc R . . H8C H 1.5245 0.4681 0.6631 0.096 Uiso 1 1 calc R . . C9 C 1.3737(9) 0.3323(9) 0.6822(6) 0.070(4) Uani 1 1 d . . . H9A H 1.3287 0.2755 0.6979 0.105 Uiso 1 1 calc R . . H9B H 1.3546 0.4006 0.7031 0.105 Uiso 1 1 calc R . . H9C H 1.4466 0.3158 0.6984 0.105 Uiso 1 1 calc R . . C10 C 1.2440(6) 0.3395(9) 0.5712(5) 0.033(3) Uani 1 1 d . . . H10A H 1.2301 0.3569 0.5199 0.049 Uiso 1 1 calc R . . H10B H 1.2100 0.3923 0.5999 0.049 Uiso 1 1 calc R . . H10C H 1.2165 0.2682 0.5801 0.049 Uiso 1 1 calc R . . C11 C 0.0713(7) 0.4072(7) 0.9327(5) 0.022(2) Uani 1 1 d . . . C12 C 0.1367(6) 0.3086(8) 0.8995(4) 0.0214(17) Uiso 1 1 d . . . C13 C 0.0777(7) 0.2094(8) 0.9234(5) 0.030(2) Uani 1 1 d . . . H13 H 0.0136 0.1989 0.8892 0.036 Uiso 1 1 calc R . . C14 C 0.0428(7) 0.2401(8) 1.0022(6) 0.037(2) Uani 1 1 d . . . H14A H -0.0324 0.2257 1.0041 0.044 Uiso 1 1 calc R . . H14B H 0.0828 0.1974 1.0402 0.044 Uiso 1 1 calc R . . C15 C 0.0657(8) 0.3589(8) 1.0134(5) 0.039(2) Uani 1 1 d . . . H15A H 0.1327 0.3695 1.0433 0.047 Uiso 1 1 calc R . . H15B H 0.0095 0.3940 1.0373 0.047 Uiso 1 1 calc R . . C16 C 0.1337(7) 0.5112(7) 0.9321(5) 0.0180(19) Uani 1 1 d . . . C17 C 0.1444(7) 0.1056(6) 0.9248(5) 0.018(2) Uani 1 1 d . . . C18 C -0.0370(6) 0.4182(7) 0.8969(5) 0.047(2) Uani 1 1 d . . . H18A H -0.0835 0.4410 0.9325 0.071 Uiso 1 1 calc R . . H18B H -0.0606 0.3493 0.8763 0.071 Uiso 1 1 calc R . . H18C H -0.0379 0.4717 0.8584 0.071 Uiso 1 1 calc R . . C19 C 0.1288(8) 0.3073(9) 0.8159(5) 0.051(3) Uani 1 1 d . . . H19A H 0.1812 0.2584 0.7999 0.076 Uiso 1 1 calc R . . H19B H 0.1410 0.3795 0.7981 0.076 Uiso 1 1 calc R . . H19C H 0.0590 0.2833 0.7969 0.076 Uiso 1 1 calc R . . C20 C 0.2518(6) 0.3096(8) 0.9315(5) 0.034(3) Uani 1 1 d . . . H20A H 0.2552 0.3172 0.9840 0.051 Uiso 1 1 calc R . . H20B H 0.2879 0.3698 0.9113 0.051 Uiso 1 1 calc R . . H20C H 0.2853 0.2425 0.9195 0.051 Uiso 1 1 calc R . . C21 C 1.1565(9) 0.8405(10) 0.4083(6) 0.041(3) Uani 1 1 d . . . C22 C 1.1087(10) 0.8354(10) 0.3282(6) 0.062(4) Uani 1 1 d . . . H22A H 1.1621 0.8541 0.2965 0.093 Uiso 1 1 calc R . . H22B H 1.0506 0.8861 0.3208 0.093 Uiso 1 1 calc R . . H22C H 1.0832 0.7629 0.3171 0.093 Uiso 1 1 calc R . . C23 C 0.3465(7) 0.8142(8) 1.0921(5) 0.019(2) Uani 1 1 d . . . C24 C 0.3959(9) 0.8252(9) 1.1712(6) 0.054(4) Uani 1 1 d . . . H24A H 0.3453 0.8577 1.2005 0.082 Uiso 1 1 calc R . . H24B H 0.4581 0.8706 1.1725 0.082 Uiso 1 1 calc R . . H24C H 0.4156 0.7544 1.1904 0.082 Uiso 1 1 calc R . . C25 C 0.8463(6) 0.6303(11) 0.7902(4) 0.048(3) Uani 1 1 d . . . H25A H 0.8570 0.5519 0.7923 0.057 Uiso 1 1 calc R . . H25B H 0.9095 0.6638 0.8151 0.057 Uiso 1 1 calc R . . C26 C 0.7601(7) 0.6553(11) 0.8302(5) 0.055(4) Uani 1 1 d . . . H26A H 0.7678 0.7305 0.8464 0.066 Uiso 1 1 calc R . . H26B H 0.7657 0.6100 0.8740 0.066 Uiso 1 1 calc R . . C27 C 0.6422(7) 0.6826(11) 0.7183(4) 0.057(3) Uani 1 1 d . . . H27A H 0.5771 0.6532 0.6933 0.068 Uiso 1 1 calc R . . H27B H 0.6354 0.7614 0.7192 0.068 Uiso 1 1 calc R . . C28 C 0.7291(7) 0.6543(10) 0.6777(5) 0.052(3) Uani 1 1 d . . . H28A H 0.7249 0.7001 0.6342 0.063 Uiso 1 1 calc R . . H28B H 0.7184 0.5797 0.6610 0.063 Uiso 1 1 calc R . . C29 C 1.1148(8) 0.6581(8) 0.6672(5) 0.034(2) Uani 1 1 d . . . H29 H 1.1820 0.6412 0.6900 0.040 Uiso 1 1 calc R . . C30 C 1.0297(7) 0.6496(7) 0.7080(5) 0.029(2) Uani 1 1 d . . . H30 H 1.0409 0.6315 0.7576 0.035 Uiso 1 1 calc R . . C31 C 0.9271(7) 0.6677(9) 0.6761(5) 0.035(2) Uani 1 1 d . . . C32 C 0.9176(7) 0.6944(10) 0.6020(5) 0.041(3) Uani 1 1 d . . . H32 H 0.8503 0.7062 0.5776 0.049 Uiso 1 1 calc R . . C33 C 1.0086(7) 0.7042(9) 0.5622(5) 0.034(3) Uani 1 1 d . . . H33 H 1.0004 0.7210 0.5122 0.041 Uiso 1 1 calc R . . C34 C 0.4889(6) 0.6625(7) 0.9479(4) 0.0178(19) Uani 1 1 d . . . H34 H 0.4975 0.6703 0.9988 0.021 Uiso 1 1 calc R . . C35 C 0.5764(7) 0.6558(7) 0.9110(5) 0.024(2) Uani 1 1 d . . . H35 H 0.6439 0.6555 0.9366 0.028 Uiso 1 1 calc R . . C36 C 0.5648(6) 0.6492(6) 0.8335(5) 0.0178(19) Uani 1 1 d . . . C37 C 0.4633(7) 0.6446(8) 0.7983(6) 0.035(3) Uani 1 1 d . . . H37 H 0.4511 0.6398 0.7473 0.042 Uiso 1 1 calc R . . C38 C 0.3800(8) 0.6473(8) 0.8424(5) 0.033(2) Uani 1 1 d . . . H38 H 0.3116 0.6407 0.8187 0.040 Uiso 1 1 calc R . . C39 C 0.8472(12) 1.0593(15) 0.7846(7) 0.049(5) Uiso 0.50 1 d PD A 1 H39A H 0.8408 1.1377 0.7898 0.059 Uiso 0.50 1 calc PR A 1 H39B H 0.9159 1.0383 0.8092 0.059 Uiso 0.50 1 calc PR A 1 C40 C 0.7638(10) 1.0074(16) 0.8239(8) 0.021(4) Uiso 0.50 1 d PD A 1 H40A H 0.7773 0.9297 0.8286 0.025 Uiso 0.50 1 calc PR A 1 H40B H 0.7646 1.0381 0.8730 0.025 Uiso 0.50 1 calc PR A 1 C41 C 0.6534(19) 1.016(2) 0.7046(9) 0.077(10) Uiso 0.50 1 d PD A 1 H41A H 0.5849 1.0443 0.6849 0.093 Uiso 0.50 1 calc PR A 1 H41B H 0.6561 0.9391 0.6912 0.093 Uiso 0.50 1 calc PR A 1 C42 C 0.7389(10) 1.0753(14) 0.6720(9) 0.044(4) Uiso 0.50 1 d PD A 1 H42A H 0.7326 1.1528 0.6814 0.053 Uiso 0.50 1 calc PR A 1 H42B H 0.7324 1.0642 0.6191 0.053 Uiso 0.50 1 calc PR A 1 C39' C 0.8543(14) 0.9877(16) 0.7823(8) 0.034(5) Uiso 0.50 1 d PD A 2 H39C H 0.9247 0.9992 0.8076 0.041 Uiso 0.50 1 calc PR A 2 H39D H 0.8393 0.9101 0.7809 0.041 Uiso 0.50 1 calc PR A 2 C40' C 0.7711(9) 1.0488(12) 0.8206(7) 0.009(3) Uiso 0.50 1 d PD A 2 H40C H 0.7752 1.0269 0.8719 0.010 Uiso 0.50 1 calc PR A 2 H40D H 0.7848 1.1266 0.8188 0.010 Uiso 0.50 1 calc PR A 2 C41' C 0.6590(13) 1.0559(15) 0.7077(8) 0.021(4) Uiso 0.50 1 d PD A 2 H41C H 0.6635 1.1348 0.7046 0.026 Uiso 0.50 1 calc PR A 2 H41D H 0.5903 1.0343 0.6836 0.026 Uiso 0.50 1 calc PR A 2 C42' C 0.7465(9) 1.0060(12) 0.6655(7) 0.010(3) Uiso 0.50 1 d PD A 2 H42C H 0.7384 0.9274 0.6625 0.012 Uiso 0.50 1 calc PR A 2 H42D H 0.7424 1.0352 0.6159 0.012 Uiso 0.50 1 calc PR A 2 C43 C 1.1221(7) 1.0160(10) 0.6613(5) 0.041(3) Uani 1 1 d . A . H43 H 1.1902 1.0193 0.6858 0.049 Uiso 1 1 calc R . . C44 C 1.0396(7) 1.0259(9) 0.7003(5) 0.036(3) Uani 1 1 d . . . H44 H 1.0521 1.0334 0.7512 0.043 Uiso 1 1 calc R A . C45 C 0.9321(8) 1.0257(9) 0.6672(5) 0.041(3) Uani 1 1 d . A . C46 C 0.9237(8) 1.0050(9) 0.5900(5) 0.033(2) Uani 1 1 d . . . H46 H 0.8571 0.9970 0.5638 0.040 Uiso 1 1 calc R A . C47 C 1.0121(8) 0.9972(9) 0.5553(5) 0.041(3) Uani 1 1 d . A . H47 H 1.0021 0.9882 0.5045 0.049 Uiso 1 1 calc R . . C48 C 0.4978(7) 0.9537(8) 0.9297(4) 0.024(2) Uani 1 1 d . A . H48 H 0.5072 0.9288 0.9781 0.029 Uiso 1 1 calc R . . C49 C 0.5839(7) 0.9703(7) 0.8985(5) 0.027(2) Uani 1 1 d . . . H49 H 0.6501 0.9586 0.9244 0.032 Uiso 1 1 calc R A . C50 C 0.5765(7) 1.0074(8) 0.8226(5) 0.028(2) Uani 1 1 d . A . C51 C 0.4707(7) 1.0248(8) 0.7892(5) 0.033(2) Uani 1 1 d . . . H51 H 0.4591 1.0511 0.7413 0.040 Uiso 1 1 calc R A . C52 C 0.3878(7) 1.0028(8) 0.8281(5) 0.030(2) Uani 1 1 d . A . H52 H 0.3197 1.0116 0.8044 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0276(7) 0.0458(8) 0.0237(7) 0.0123(5) 0.0015(5) -0.0067(5) Zn2 0.0384(8) 0.0512(9) 0.0261(7) -0.0095(6) -0.0014(6) 0.0057(6) Zn3 0.0263(6) 0.0118(5) 0.0194(6) -0.0010(4) 0.0043(4) -0.0002(4) Zn4 0.0299(6) 0.0184(6) 0.0244(6) 0.0010(5) -0.0006(5) -0.0018(4) O1 0.043(4) 0.059(5) 0.017(4) 0.012(4) -0.002(3) -0.014(4) O2 0.043(4) 0.043(4) 0.019(4) 0.012(3) -0.003(3) 0.004(4) O3 0.044(4) 0.047(4) 0.015(4) -0.002(3) -0.005(3) 0.009(3) O4 0.051(5) 0.045(5) 0.021(4) 0.011(4) -0.010(3) -0.001(4) O5 0.032(4) 0.027(4) 0.026(4) -0.005(3) -0.001(3) -0.002(3) O6 0.033(4) 0.023(3) 0.024(4) -0.001(3) 0.000(3) -0.009(3) O7 0.043(4) 0.022(3) 0.021(4) -0.011(3) -0.008(3) 0.010(3) O8 0.028(4) 0.029(4) 0.018(4) -0.009(3) -0.005(3) -0.003(3) O9 0.023(4) 0.068(5) 0.031(4) 0.015(4) 0.005(3) -0.003(3) O10 0.045(4) 0.050(5) 0.041(5) 0.018(4) -0.005(3) -0.017(4) O11 0.060(5) 0.059(5) 0.018(4) -0.018(4) -0.007(3) 0.007(4) O12 0.027(3) 0.014(3) 0.021(4) -0.007(3) -0.004(3) -0.001(3) O13 0.042(4) 0.013(3) 0.032(4) 0.007(3) -0.010(3) -0.002(3) O14 0.053(4) 0.023(4) 0.024(4) 0.006(3) -0.020(3) -0.005(3) N1 0.023(4) 0.091(7) 0.013(4) 0.017(4) -0.007(3) -0.012(4) N2 0.018(4) 0.050(5) 0.011(4) 0.009(3) -0.004(3) 0.010(3) N3 0.027(4) 0.050(5) 0.026(5) 0.006(4) -0.005(4) -0.005(4) N4 0.028(4) 0.030(5) 0.022(5) 0.006(4) -0.002(3) 0.008(4) N5 0.036(5) 0.094(7) 0.014(4) 0.000(4) 0.001(4) -0.023(4) N6 0.037(4) 0.051(5) 0.017(4) -0.002(3) 0.001(3) -0.007(3) N7 0.033(5) 0.043(5) 0.016(4) -0.013(4) 0.001(4) -0.001(4) N8 0.030(4) 0.021(4) 0.024(4) 0.009(3) -0.001(3) -0.008(3) C1 0.030(5) 0.054(7) 0.032(6) 0.013(5) -0.008(4) 0.004(5) C2 0.041(6) 0.036(6) 0.218(19) 0.004(7) 0.028(9) 0.005(4) C3 0.023(5) 0.060(7) 0.045(6) 0.002(5) -0.013(4) 0.005(5) C4 0.056(7) 0.081(10) 0.093(10) -0.014(8) 0.033(7) -0.004(6) C5 0.071(8) 0.071(8) 0.055(7) -0.003(6) 0.024(6) 0.005(7) C6 0.018(5) 0.056(7) 0.044(8) 0.001(6) 0.007(5) -0.006(5) C7 0.033(6) 0.040(6) 0.045(7) -0.017(5) 0.000(5) 0.009(5) C8 0.048(5) 0.067(7) 0.077(7) 0.014(5) 0.000(5) -0.015(5) C9 0.089(9) 0.069(8) 0.052(8) 0.026(6) 0.008(7) -0.055(7) C10 0.026(5) 0.059(7) 0.015(5) 0.017(5) 0.006(4) 0.010(4) C11 0.032(5) 0.014(4) 0.023(4) -0.005(3) 0.007(4) -0.001(4) C13 0.026(5) 0.026(5) 0.036(6) -0.007(4) 0.002(4) -0.007(4) C14 0.034(5) 0.034(5) 0.045(6) 0.010(4) 0.011(4) 0.000(4) C15 0.061(6) 0.028(4) 0.031(5) -0.009(4) 0.024(4) -0.023(5) C16 0.021(5) 0.018(5) 0.016(5) 0.007(4) 0.002(4) 0.005(4) C17 0.030(5) 0.006(4) 0.015(5) 0.004(4) -0.001(4) -0.006(4) C18 0.042(5) 0.036(5) 0.064(6) -0.004(4) 0.004(4) 0.009(4) C19 0.082(8) 0.045(5) 0.024(5) -0.015(5) 0.000(5) 0.045(6) C20 0.026(5) 0.020(4) 0.055(7) -0.016(5) -0.003(5) -0.014(4) C21 0.042(7) 0.056(8) 0.021(7) -0.004(5) -0.010(5) 0.003(5) C22 0.105(11) 0.054(9) 0.023(7) 0.002(5) -0.020(7) -0.008(7) C23 0.020(5) 0.025(5) 0.013(5) 0.002(4) 0.005(4) 0.000(4) C24 0.094(10) 0.034(7) 0.029(7) 0.000(5) -0.023(7) -0.013(6) C25 0.019(4) 0.111(10) 0.013(4) 0.018(5) 0.006(3) 0.027(5) C26 0.033(5) 0.114(10) 0.017(4) 0.019(5) -0.004(3) -0.033(5) C27 0.025(4) 0.125(10) 0.019(4) 0.030(5) -0.001(3) -0.010(5) C28 0.053(6) 0.075(8) 0.027(5) 0.001(5) -0.004(4) 0.026(5) C29 0.035(6) 0.043(6) 0.024(5) 0.014(5) 0.005(4) -0.011(5) C30 0.026(5) 0.034(5) 0.026(5) 0.008(4) -0.001(4) -0.008(4) C31 0.030(5) 0.058(6) 0.017(5) -0.005(4) 0.006(4) -0.011(5) C32 0.024(5) 0.072(8) 0.028(6) 0.014(5) 0.006(4) 0.005(5) C33 0.029(5) 0.051(6) 0.024(5) 0.019(4) 0.005(4) 0.002(5) C34 0.027(5) 0.013(4) 0.014(4) -0.007(4) 0.005(4) -0.001(4) C35 0.019(5) 0.017(5) 0.035(6) -0.006(4) -0.001(4) -0.001(4) C36 0.021(4) 0.007(4) 0.025(5) 0.001(3) 0.002(4) -0.001(3) C37 0.035(6) 0.042(6) 0.028(6) 0.003(4) -0.001(5) 0.007(4) C38 0.040(6) 0.031(5) 0.030(6) 0.005(4) 0.005(5) -0.005(4) C43 0.018(5) 0.084(8) 0.019(5) -0.025(5) -0.011(4) 0.009(5) C44 0.030(5) 0.064(7) 0.012(5) -0.001(4) -0.002(4) -0.012(4) C45 0.046(6) 0.058(7) 0.017(5) -0.007(5) 0.004(5) -0.003(5) C46 0.038(6) 0.048(6) 0.012(5) -0.004(4) -0.003(4) -0.006(5) C47 0.048(7) 0.049(6) 0.022(6) -0.006(5) -0.009(5) 0.003(5) C48 0.033(5) 0.030(5) 0.009(4) -0.001(4) -0.004(4) 0.001(4) C49 0.033(5) 0.028(5) 0.018(5) -0.006(4) -0.008(4) -0.010(4) C50 0.033(5) 0.024(5) 0.026(5) 0.008(4) -0.005(4) -0.007(4) C51 0.041(6) 0.050(6) 0.008(4) 0.002(4) 0.001(4) -0.004(4) C52 0.019(5) 0.045(6) 0.025(5) 0.004(4) -0.010(4) -0.005(4) _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 Zn1 O9 1.920(7) . ? Zn1 O2 1.969(7) . ? Zn1 O10 2.004(7) . ? Zn1 N3 2.027(7) . ? Zn1 C6 2.569(11) . ? Zn2 O9 1.926(7) . ? Zn2 O3 1.957(7) 1_565 ? Zn2 N7 1.999(7) . ? Zn2 O11 2.010(6) . ? Zn2 C7 2.561(11) 1_565 ? Zn3 O12 1.901(6) . ? Zn3 O6 1.969(6) . ? Zn3 O13 2.004(6) . ? Zn3 N4 2.035(7) . ? Zn4 O12 1.931(6) . ? Zn4 O8 1.972(6) 1_565 ? Zn4 N8 2.007(7) . ? Zn4 O14 2.025(6) . ? Zn4 O7 2.462(6) 1_565 ? Zn4 C17 2.567(8) 1_565 ? O1 C6 1.286(12) . ? O2 C6 1.251(12) . ? O3 C7 1.302(12) . ? O3 Zn2 1.957(7) 1_545 ? O4 C7 1.209(13) . ? O5 C16 1.269(11) . ? O6 C16 1.258(10) . ? O7 C17 1.208(10) . ? O7 Zn4 2.462(6) 1_545 ? O8 C17 1.308(9) . ? O8 Zn4 1.972(6) 1_545 ? O10 C21 1.239(13) . ? O11 C21 1.233(13) . ? O13 C23 1.225(11) . ? O14 C23 1.258(11) . ? N1 C31 1.376(11) . ? N1 C25 1.435(10) . ? N1 C28 1.477(11) . ? N2 C36 1.409(10) . ? N2 C26 1.440(10) . ? N2 C27 1.453(10) . ? N3 C29 1.326(12) . ? N3 C33 1.355(11) . ? N4 C38 1.286(12) . ? N4 C34 1.369(10) . ? N5 C45 1.340(12) . ? N5 C42' 1.446(13) . ? N5 C39 1.474(13) . ? N5 C39' 1.504(14) . ? N5 C42 1.529(13) . ? N6 C50 1.378(11) . ? N6 C40 1.407(14) . ? N6 C41' 1.446(14) . ? N6 C41 1.454(17) . ? N6 C40' 1.475(12) . ? N7 C47 1.315(12) . ? N7 C43 1.401(11) . ? N8 C48 1.340(10) . ? N8 C52 1.396(11) . ? C1 C6 1.499(15) . ? C1 C8 1.507(12) . ? C1 C2 1.551(17) . ? C1 C5 1.607(15) . ? C2 C3 1.433(16) . ? C2 C10 1.463(14) . ? C2 C9 1.64(2) . ? C3 C7 1.560(15) . ? C3 C4 1.597(15) . ? C4 C5 1.504(18) . ? C7 Zn2 2.561(11) 1_545 ? C11 C18 1.462(11) . ? C11 C16 1.498(12) . ? C11 C15 1.595(12) . ? C11 C12 1.614(12) . ? C12 C20 1.511(10) . ? C12 C13 1.512(13) . ? C12 C19 1.518(11) . ? C13 C17 1.524(12) . ? C13 C14 1.590(13) . ? C14 C15 1.494(12) . ? C17 Zn4 2.567(8) 1_545 ? C21 C22 1.526(13) . ? C23 C24 1.519(12) . ? C25 C26 1.402(12) . ? C27 C28 1.426(12) . ? C29 C30 1.370(12) . ? C30 C31 1.383(12) . ? C31 C32 1.386(13) . ? C32 C33 1.422(12) . ? C34 C35 1.353(11) . ? C35 C36 1.409(12) . ? C36 C37 1.375(12) . ? C37 C38 1.386(12) . ? C39 C40 1.475(15) . ? C41 C42 1.477(17) . ? C39' C40' 1.516(15) . ? C41' C42' 1.535(15) . ? C43 C44 1.324(12) . ? C44 C45 1.429(13) . ? C45 C46 1.426(12) . ? C46 C47 1.340(13) . ? C48 C49 1.293(11) . ? C49 C50 1.450(12) . ? C50 C51 1.428(12) . ? C51 C52 1.349(12) . ? 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 O9 Zn1 O2 125.1(3) . . ? O9 Zn1 O10 100.5(3) . . ? O2 Zn1 O10 98.0(3) . . ? O9 Zn1 N3 112.1(3) . . ? O2 Zn1 N3 114.1(3) . . ? O10 Zn1 N3 101.3(3) . . ? O9 Zn1 C6 110.4(3) . . ? O2 Zn1 C6 28.3(3) . . ? O10 Zn1 C6 126.1(4) . . ? N3 Zn1 C6 106.0(3) . . ? O9 Zn2 O3 125.9(3) . 1_565 ? O9 Zn2 N7 108.9(3) . . ? O3 Zn2 N7 112.8(3) 1_565 . ? O9 Zn2 O11 103.8(3) . . ? O3 Zn2 O11 100.1(3) 1_565 . ? N7 Zn2 O11 101.4(3) . . ? O9 Zn2 C7 107.7(3) . 1_565 ? O3 Zn2 C7 29.9(3) 1_565 1_565 ? N7 Zn2 C7 104.0(3) . 1_565 ? O11 Zn2 C7 129.8(4) . 1_565 ? O12 Zn3 O6 125.5(3) . . ? O12 Zn3 O13 100.9(2) . . ? O6 Zn3 O13 100.2(2) . . ? O12 Zn3 N4 107.9(3) . . ? O6 Zn3 N4 114.8(3) . . ? O13 Zn3 N4 103.8(3) . . ? O12 Zn4 O8 121.1(2) . 1_565 ? O12 Zn4 N8 117.4(3) . . ? O8 Zn4 N8 114.9(3) 1_565 . ? O12 Zn4 O14 99.5(3) . . ? O8 Zn4 O14 97.4(3) 1_565 . ? N8 Zn4 O14 99.0(3) . . ? O12 Zn4 O7 92.3(2) . 1_565 ? O8 Zn4 O7 57.7(2) 1_565 1_565 ? N8 Zn4 O7 95.1(3) . 1_565 ? O14 Zn4 O7 154.9(2) . 1_565 ? O12 Zn4 C17 108.4(2) . 1_565 ? O8 Zn4 C17 30.0(2) 1_565 1_565 ? N8 Zn4 C17 105.9(3) . 1_565 ? O14 Zn4 C17 127.4(3) . 1_565 ? O7 Zn4 C17 27.7(2) 1_565 1_565 ? C6 O2 Zn1 103.6(7) . . ? C7 O3 Zn2 101.7(7) . 1_545 ? C16 O6 Zn3 106.4(5) . . ? C17 O7 Zn4 81.0(5) . 1_545 ? C17 O8 Zn4 101.0(5) . 1_545 ? Zn1 O9 Zn2 115.0(3) . . ? C21 O10 Zn1 133.7(7) . . ? C21 O11 Zn2 127.3(7) . . ? Zn3 O12 Zn4 115.3(3) . . ? C23 O13 Zn3 129.8(6) . . ? C23 O14 Zn4 133.1(6) . . ? C31 N1 C25 121.3(7) . . ? C31 N1 C28 123.1(7) . . ? C25 N1 C28 112.8(7) . . ? C36 N2 C26 120.6(7) . . ? C36 N2 C27 116.8(7) . . ? C26 N2 C27 114.0(7) . . ? C29 N3 C33 118.0(8) . . ? C29 N3 Zn1 122.2(7) . . ? C33 N3 Zn1 119.8(6) . . ? C38 N4 C34 116.5(8) . . ? C38 N4 Zn3 121.3(7) . . ? C34 N4 Zn3 122.0(6) . . ? C45 N5 C42' 115.2(9) . . ? C45 N5 C39 127.3(10) . . ? C42' N5 C39 117.3(10) . . ? C45 N5 C39' 118.7(10) . . ? C42' N5 C39' 110.4(11) . . ? C39 N5 C39' 34.5(9) . . ? C45 N5 C42 123.0(9) . . ? C42' N5 C42 33.6(8) . . ? C39 N5 C42 103.7(11) . . ? C39' N5 C42 117.8(10) . . ? C50 N6 C40 116.0(9) . . ? C50 N6 C41' 124.9(9) . . ? C40 N6 C41' 119.0(10) . . ? C50 N6 C41 119.8(11) . . ? C40 N6 C41 119.1(14) . . ? C41' N6 C41 19.9(13) . . ? C50 N6 C40' 123.4(8) . . ? C40 N6 C40' 20.6(7) . . ? C41' N6 C40' 109.3(10) . . ? C41 N6 C40' 116.8(11) . . ? C47 N7 C43 113.9(7) . . ? C47 N7 Zn2 126.4(6) . . ? C43 N7 Zn2 119.5(6) . . ? C48 N8 C52 113.1(7) . . ? C48 N8 Zn4 125.1(6) . . ? C52 N8 Zn4 121.8(6) . . ? C6 C1 C8 111.7(10) . . ? C6 C1 C2 112.5(8) . . ? C8 C1 C2 115.3(10) . . ? C6 C1 C5 114.0(9) . . ? C8 C1 C5 109.5(8) . . ? C2 C1 C5 92.6(11) . . ? C3 C2 C10 119.6(12) . . ? C3 C2 C1 106.0(11) . . ? C10 C2 C1 117.8(11) . . ? C3 C2 C9 98.2(11) . . ? C10 C2 C9 105.9(12) . . ? C1 C2 C9 106.9(11) . . ? C2 C3 C7 115.2(9) . . ? C2 C3 C4 103.2(11) . . ? C7 C3 C4 111.9(10) . . ? C5 C4 C3 103.2(9) . . ? C4 C5 C1 105.7(10) . . ? O2 C6 O1 122.5(10) . . ? O2 C6 C1 117.5(10) . . ? O1 C6 C1 120.0(10) . . ? O2 C6 Zn1 48.2(5) . . ? O1 C6 Zn1 74.3(6) . . ? C1 C6 Zn1 165.7(8) . . ? O4 C7 O3 122.5(10) . . ? O4 C7 C3 121.8(10) . . ? O3 C7 C3 115.6(10) . . ? O4 C7 Zn2 74.1(6) . 1_545 ? O3 C7 Zn2 48.4(5) . 1_545 ? C3 C7 Zn2 163.6(8) . 1_545 ? C18 C11 C16 112.8(7) . . ? C18 C11 C15 108.7(7) . . ? C16 C11 C15 113.2(7) . . ? C18 C11 C12 113.1(7) . . ? C16 C11 C12 110.3(6) . . ? C15 C11 C12 98.0(7) . . ? C20 C12 C13 112.2(8) . . ? C20 C12 C19 110.7(8) . . ? C13 C12 C19 107.2(8) . . ? C20 C12 C11 110.9(7) . . ? C13 C12 C11 102.1(6) . . ? C19 C12 C11 113.5(7) . . ? C12 C13 C17 112.9(7) . . ? C12 C13 C14 105.0(7) . . ? C17 C13 C14 112.6(8) . . ? C15 C14 C13 106.6(7) . . ? C14 C15 C11 105.2(8) . . ? O6 C16 O5 121.6(8) . . ? O6 C16 C11 118.6(8) . . ? O5 C16 C11 119.8(8) . . ? O7 C17 O8 120.3(8) . . ? O7 C17 C13 120.8(8) . . ? O8 C17 C13 118.9(8) . . ? O7 C17 Zn4 71.3(5) . 1_545 ? O8 C17 Zn4 49.0(4) . 1_545 ? C13 C17 Zn4 167.9(6) . 1_545 ? O11 C21 O10 128.3(10) . . ? O11 C21 C22 114.6(10) . . ? O10 C21 C22 117.1(10) . . ? O13 C23 O14 125.6(8) . . ? O13 C23 C24 119.2(8) . . ? O14 C23 C24 115.2(8) . . ? C26 C25 N1 117.3(8) . . ? C25 C26 N2 117.7(8) . . ? C28 C27 N2 113.1(8) . . ? C27 C28 N1 118.8(9) . . ? N3 C29 C30 123.9(10) . . ? C29 C30 C31 120.8(9) . . ? N1 C31 C30 123.6(8) . . ? N1 C31 C32 120.6(8) . . ? C30 C31 C32 115.7(8) . . ? C31 C32 C33 121.5(9) . . ? N3 C33 C32 119.8(8) . . ? C35 C34 N4 122.3(8) . . ? C34 C35 C36 119.6(8) . . ? C37 C36 N2 121.1(8) . . ? C37 C36 C35 118.0(8) . . ? N2 C36 C35 120.8(7) . . ? C36 C37 C38 117.0(9) . . ? N4 C38 C37 126.5(10) . . ? N5 C39 C40 117.1(12) . . ? N6 C40 C39 109.4(13) . . ? N6 C41 C42 111.5(16) . . ? C41 C42 N5 109.6(15) . . ? N5 C39' C40' 105.2(12) . . ? N6 C40' C39' 110.2(11) . . ? N6 C41' C42' 114.8(12) . . ? N5 C42' C41' 107.0(11) . . ? C44 C43 N7 123.0(9) . . ? C43 C44 C45 122.5(9) . . ? N5 C45 C46 123.1(9) . . ? N5 C45 C44 123.6(9) . . ? C46 C45 C44 113.1(9) . . ? C47 C46 C45 119.7(10) . . ? N7 C47 C46 127.5(9) . . ? C49 C48 N8 128.3(8) . . ? C48 C49 C50 119.5(9) . . ? N6 C50 C51 121.4(8) . . ? N6 C50 C49 123.6(8) . . ? C51 C50 C49 115.0(8) . . ? C52 C51 C50 119.1(9) . . ? C51 C52 N8 124.9(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.238 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.097