# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Fei-Yan Yi' _publ_contact_author_email fyyi@ciac.jl.cn loop_ _publ_author_name 'Zhongming Sun' 'Fei-Yan Yi' 'Weiting Yang' data_1 _database_code_depnum_ccdc_archive 'CCDC 893227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H79 Cd3 N5 O26' _chemical_formula_weight 1755.59 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.373(6) _cell_length_b 11.367(3) _cell_length_c 36.596(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.685(4) _cell_angle_gamma 90.00 _cell_volume 10048(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5551 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53896 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.09 _reflns_number_total 19841 _reflns_number_gt 14244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1343P)^2^+31.8335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19841 _refine_ls_number_parameters 860 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2469 _refine_ls_wR_factor_gt 0.2250 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.069 _refine_ls_shift/su_mean 0.002 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 0.327551(19) 0.64314(4) 1.157921(13) 0.03624(15) Uani 1 1 d . . . Cd2 Cd 0.28370(2) 0.36729(4) 1.118633(13) 0.03764(15) Uani 1 1 d . . . Cd3 Cd 0.29894(3) 0.08209(5) 1.091422(16) 0.05145(18) Uani 1 1 d . . . N1 N 0.4968(3) 0.7790(8) 1.1547(3) 0.092(3) Uani 1 1 d . . . N2 N 0.1756(6) -0.2075(14) 1.0509(5) 0.151(5) Uani 1 1 d . . . N3 N 0.5018(4) 0.4906(9) 0.2556(3) 0.090(3) Uani 1 1 d . . . N4 N 0.2760(8) 0.8194(16) 0.7826(5) 0.166(6) Uiso 1 1 d . . . N5 N 0.321(3) 0.095(5) 0.9179(19) 0.50(4) Uiso 1 1 d . . . O1 O 0.21010(19) 0.4741(5) 0.85189(16) 0.0563(14) Uani 1 1 d . . . O1W O 0.3507(4) -0.0578(7) 1.0705(3) 0.114(3) Uani 1 1 d . . . O2W O 0.3264(2) 0.8281(5) 1.18143(17) 0.0593(15) Uani 1 1 d . . . O2 O 0.2987(3) 0.5763(5) 0.92644(14) 0.0669(17) Uani 1 1 d . . . O3 O 0.40532(19) 0.5341(5) 0.87620(16) 0.0525(13) Uani 1 1 d . . . O4 O 0.3199(2) 0.4158(4) 0.80996(13) 0.0539(13) Uani 1 1 d . . . O5 O 0.1182(3) 0.3962(6) 0.90041(15) 0.0745(19) Uani 1 1 d . . . O6 O 0.0184(2) 0.3774(5) 0.82430(18) 0.0643(16) Uani 1 1 d . . . O7 O 0.1196(3) 0.4360(6) 0.77091(16) 0.075(2) Uani 1 1 d . . . O8 O 0.3231(3) 0.7297(5) 1.09430(14) 0.0573(14) Uani 1 1 d . . . O9 O 0.3239(2) 0.5405(4) 1.10207(12) 0.0440(11) Uani 1 1 d . . . O10 O 0.6471(2) 0.7476(6) 0.90124(16) 0.0619(16) Uani 1 1 d . . . O11 O 0.6030(3) 0.8930(7) 0.8693(2) 0.093(2) Uani 1 1 d . . . O12 O 0.3337(2) -0.0358(5) 0.70987(14) 0.0565(14) Uani 1 1 d . . . O13 O 0.3446(2) 0.1062(5) 0.66968(13) 0.0543(14) Uani 1 1 d . . . O14 O 0.2330(3) 0.3466(6) 1.06427(15) 0.0637(16) Uani 1 1 d . . . O15 O 0.2561(4) 0.1740(7) 1.04263(19) 0.092(2) Uani 1 1 d . . . O16 O -0.2197(2) 0.5459(5) 0.85295(17) 0.0604(15) Uani 1 1 d . . . O17 O -0.2347(2) 0.3526(5) 0.84563(17) 0.0582(14) Uani 1 1 d . . . O18 O 0.2477(3) 0.3111(5) 0.63578(16) 0.0620(15) Uani 1 1 d . . . O19 O 0.2675(3) 0.4970(5) 0.64273(15) 0.0591(15) Uani 1 1 d . . . O20 O 0.4220(2) 0.6686(6) 1.16325(18) 0.0630(15) Uani 1 1 d . . . O21 O 0.2301(6) -0.0538(12) 1.0618(3) 0.162(5) Uani 1 1 d . . . O22 O 0.5830(3) 0.3968(8) 0.2728(3) 0.107(3) Uani 1 1 d . . . O23 O 0.3255(9) 0.8724(17) 0.8312(6) 0.246(8) Uiso 1 1 d . . . O24 O 0.3548(14) -0.002(3) 0.9901(11) 0.404(18) Uiso 1 1 d . . . C1 C 0.2527(3) 0.5569(6) 0.8513(2) 0.0418(16) Uani 1 1 d . . . H1A H 0.2455 0.6253 0.8658 0.050 Uiso 1 1 calc R . . H1B H 0.2546 0.5823 0.8262 0.050 Uiso 1 1 calc R . . C2 C 0.3073(3) 0.5000(6) 0.86739(18) 0.0367(14) Uani 1 1 d . . . C3 C 0.3074(3) 0.4695(6) 0.90796(18) 0.0441(16) Uani 1 1 d . . . H3A H 0.2782 0.4138 0.9108 0.053 Uiso 1 1 calc R . . H3B H 0.3426 0.4348 0.9180 0.053 Uiso 1 1 calc R . . C4 C 0.3539(3) 0.5864(6) 0.8628(2) 0.0415(15) Uani 1 1 d . . . H4A H 0.3530 0.6066 0.8370 0.050 Uiso 1 1 calc R . . H4B H 0.3489 0.6579 0.8765 0.050 Uiso 1 1 calc R . . C5 C 0.3155(3) 0.3852(6) 0.84720(19) 0.0420(16) Uani 1 1 d . . . H5A H 0.3490 0.3458 0.8583 0.050 Uiso 1 1 calc R . . H5B H 0.2843 0.3329 0.8483 0.050 Uiso 1 1 calc R . . C6 C 0.1565(3) 0.5214(8) 0.8429(2) 0.056(2) Uani 1 1 d . . . H6A H 0.1551 0.5712 0.8213 0.067 Uiso 1 1 calc R . . H6B H 0.1469 0.5686 0.8632 0.067 Uiso 1 1 calc R . . C7 C 0.1159(3) 0.4191(7) 0.8353(2) 0.0453(17) Uani 1 1 d . . . C8 C 0.1237(3) 0.3317(8) 0.8675(2) 0.055(2) Uani 1 1 d . . . H8A H 0.0960 0.2701 0.8638 0.066 Uiso 1 1 calc R . . H8B H 0.1601 0.2957 0.8694 0.066 Uiso 1 1 calc R . . C9 C 0.0573(3) 0.4712(8) 0.8311(2) 0.0508(18) Uani 1 1 d . . . H9A H 0.0515 0.5127 0.8534 0.061 Uiso 1 1 calc R . . H9B H 0.0525 0.5265 0.8107 0.061 Uiso 1 1 calc R . . C10 C 0.1256(3) 0.3531(7) 0.8005(2) 0.0521(19) Uani 1 1 d . . . H10A H 0.1624 0.3193 0.8035 0.063 Uiso 1 1 calc R . . H10B H 0.0988 0.2900 0.7955 0.063 Uiso 1 1 calc R . . C11 C 0.3053(3) 0.5802(7) 0.96410(19) 0.0495(18) Uani 1 1 d . . . C12 C 0.2944(5) 0.6877(8) 0.9788(2) 0.080(3) Uani 1 1 d . . . H12A H 0.2828 0.7502 0.9632 0.095 Uiso 1 1 calc R . . C13 C 0.3006(5) 0.7033(7) 1.0167(2) 0.074(3) Uani 1 1 d . . . H13A H 0.2942 0.7771 1.0263 0.089 Uiso 1 1 calc R . . C14 C 0.3161(3) 0.6112(6) 1.04055(19) 0.0458(17) Uani 1 1 d . . . C15 C 0.3251(3) 0.5020(6) 1.02511(19) 0.0459(17) Uani 1 1 d . . . H15A H 0.3350 0.4383 1.0406 0.055 Uiso 1 1 calc R . . C16 C 0.3199(3) 0.4862(7) 0.9875(2) 0.0475(17) Uani 1 1 d . . . H16A H 0.3261 0.4125 0.9778 0.057 Uiso 1 1 calc R . . C17 C 0.3214(3) 0.6289(6) 1.08100(19) 0.0377(15) Uani 1 1 d . . . C18 C 0.4512(3) 0.6012(7) 0.8757(2) 0.0479(17) Uani 1 1 d . . . C19 C 0.4515(3) 0.7158(7) 0.8637(2) 0.059(2) Uani 1 1 d . . . H19A H 0.4185 0.7523 0.8543 0.070 Uiso 1 1 calc R . . C20 C 0.5012(3) 0.7769(8) 0.8658(3) 0.060(2) Uani 1 1 d . . . H20A H 0.5008 0.8554 0.8585 0.071 Uiso 1 1 calc R . . C21 C 0.5517(3) 0.7232(7) 0.8785(2) 0.0505(18) Uani 1 1 d . . . C22 C 0.5511(3) 0.6054(8) 0.8889(3) 0.060(2) Uani 1 1 d . . . H22A H 0.5842 0.5672 0.8970 0.072 Uiso 1 1 calc R . . C23 C 0.5018(3) 0.5450(7) 0.8875(3) 0.059(2) Uani 1 1 d . . . H23A H 0.5021 0.4663 0.8945 0.070 Uiso 1 1 calc R . . C24 C 0.6036(3) 0.7903(9) 0.8820(3) 0.062(2) Uani 1 1 d . . . C25 C 0.3243(3) 0.3267(6) 0.78498(19) 0.0431(16) Uani 1 1 d . . . C26 C 0.3188(4) 0.2085(7) 0.79268(19) 0.0524(19) Uani 1 1 d . . . H26A H 0.3123 0.1843 0.8160 0.063 Uiso 1 1 calc R . . C27 C 0.3231(4) 0.1266(7) 0.7653(2) 0.0516(19) Uani 1 1 d . . . H27A H 0.3180 0.0473 0.7700 0.062 Uiso 1 1 calc R . . C28 C 0.3348(3) 0.1607(7) 0.73100(19) 0.0426(16) Uani 1 1 d . . . C29 C 0.3415(3) 0.2789(7) 0.72422(18) 0.0463(17) Uani 1 1 d . . . H29A H 0.3499 0.3027 0.7013 0.056 Uiso 1 1 calc R . . C30 C 0.3360(3) 0.3618(7) 0.75064(19) 0.0481(17) Uani 1 1 d . . . H30A H 0.3401 0.4412 0.7455 0.058 Uiso 1 1 calc R . . C31 C 0.3373(3) 0.0708(7) 0.70137(19) 0.0409(16) Uani 1 1 d . . . C32 C 0.1463(4) 0.3599(9) 0.9328(2) 0.060(2) Uani 1 1 d . . . C33 C 0.1526(5) 0.4418(9) 0.9612(3) 0.080(3) Uani 1 1 d . . . H33A H 0.1377 0.5168 0.9572 0.096 Uiso 1 1 calc R . . C34 C 0.1808(5) 0.4129(9) 0.9950(2) 0.075(3) Uani 1 1 d . . . H34A H 0.1858 0.4700 1.0134 0.090 Uiso 1 1 calc R . . C35 C 0.2020(4) 0.3020(9) 1.0026(2) 0.059(2) Uani 1 1 d . . . C36 C 0.1956(5) 0.2198(9) 0.9746(3) 0.079(3) Uani 1 1 d . . . H36A H 0.2099 0.1445 0.9789 0.095 Uiso 1 1 calc R . . C37 C 0.1669(5) 0.2495(10) 0.9387(3) 0.084(3) Uani 1 1 d . . . H37A H 0.1625 0.1939 0.9199 0.101 Uiso 1 1 calc R . . C38 C 0.2331(4) 0.2727(8) 1.0396(2) 0.059(2) Uani 1 1 d . . . C39 C -0.0364(3) 0.4008(8) 0.8283(2) 0.053(2) Uani 1 1 d . . . C40 C -0.0700(3) 0.3048(8) 0.8278(3) 0.066(3) Uani 1 1 d . . . H40A H -0.0560 0.2304 0.8237 0.079 Uiso 1 1 calc R . . C41 C -0.1239(3) 0.3174(8) 0.8333(3) 0.067(3) Uani 1 1 d . . . H41A H -0.1462 0.2510 0.8331 0.081 Uiso 1 1 calc R . . C42 C -0.1462(3) 0.4272(7) 0.8390(2) 0.0453(17) Uani 1 1 d . . . C43 C -0.1113(3) 0.5233(8) 0.8385(3) 0.062(2) Uani 1 1 d . . . H43A H -0.1249 0.5980 0.8424 0.075 Uiso 1 1 calc R . . C44 C -0.0574(3) 0.5115(8) 0.8324(3) 0.063(2) Uani 1 1 d . . . H44A H -0.0352 0.5776 0.8311 0.075 Uiso 1 1 calc R . . C45 C -0.2048(3) 0.4438(7) 0.8463(2) 0.0467(17) Uani 1 1 d . . . C46 C 0.1509(3) 0.4206(8) 0.7426(2) 0.055(2) Uani 1 1 d . . . C47 C 0.1653(4) 0.5253(8) 0.7259(2) 0.067(2) Uani 1 1 d . . . H47A H 0.1541 0.5979 0.7340 0.080 Uiso 1 1 calc R . . C48 C 0.1966(4) 0.5177(7) 0.6971(2) 0.060(2) Uani 1 1 d . . . H48A H 0.2073 0.5863 0.6861 0.072 Uiso 1 1 calc R . . C49 C 0.2122(3) 0.4109(7) 0.68442(19) 0.0426(16) Uani 1 1 d . . . C50 C 0.1968(3) 0.3072(7) 0.7005(2) 0.0497(18) Uani 1 1 d . . . H50A H 0.2065 0.2346 0.6916 0.060 Uiso 1 1 calc R . . C51 C 0.1662(3) 0.3140(8) 0.7303(2) 0.056(2) Uani 1 1 d . . . H51A H 0.1564 0.2455 0.7417 0.068 Uiso 1 1 calc R . . C52 C 0.2456(3) 0.4047(7) 0.65228(19) 0.0437(16) Uani 1 1 d . . . C53 C 0.4431(4) 0.7500(10) 1.1492(3) 0.075(3) Uani 1 1 d . . . H53A H 0.4199 0.7969 1.1331 0.090 Uiso 1 1 calc R . . C54 C 0.5352(5) 0.7068(15) 1.1814(5) 0.153(7) Uani 1 1 d . . . H54A H 0.5148 0.6442 1.1910 0.230 Uiso 1 1 calc R . . H54B H 0.5513 0.7559 1.2014 0.230 Uiso 1 1 calc R . . H54C H 0.5640 0.6743 1.1690 0.230 Uiso 1 1 calc R . . C55 C 0.5158(7) 0.8804(15) 1.1360(5) 0.161(8) Uani 1 1 d . . . H55A H 0.4852 0.9151 1.1205 0.241 Uiso 1 1 calc R . . H55B H 0.5435 0.8563 1.1212 0.241 Uiso 1 1 calc R . . H55C H 0.5314 0.9371 1.1539 0.241 Uiso 1 1 calc R . . C56 C 0.2092(8) -0.1432(15) 1.0729(6) 0.142(7) Uani 1 1 d . . . H56A H 0.2175 -0.1649 1.0975 0.170 Uiso 1 1 calc R . . C57 C 0.1609(12) -0.185(3) 1.0112(7) 0.289(19) Uani 1 1 d . . . H57A H 0.1715 -0.1067 1.0056 0.434 Uiso 1 1 calc R . . H57B H 0.1217 -0.1944 1.0046 0.434 Uiso 1 1 calc R . . H57C H 0.1800 -0.2404 0.9975 0.434 Uiso 1 1 calc R . . C58 C 0.1634(10) -0.316(2) 1.0633(7) 0.210(11) Uani 1 1 d . . . H58A H 0.1759 -0.3209 1.0892 0.315 Uiso 1 1 calc R . . H58B H 0.1815 -0.3746 1.0505 0.315 Uiso 1 1 calc R . . H58C H 0.1241 -0.3277 1.0589 0.315 Uiso 1 1 calc R . . C59 C 0.5495(5) 0.4748(12) 0.2783(3) 0.095(4) Uani 1 1 d . . . C60 C 0.4596(6) 0.5779(15) 0.2644(5) 0.133(6) Uani 1 1 d . . . C61 C 0.4848(5) 0.4153(13) 0.2231(4) 0.110(4) Uani 1 1 d . . . C62 C 0.2657(14) 0.882(3) 0.8146(9) 0.235(12) Uiso 1 1 d . . . C63 C 0.3191(15) 0.765(3) 0.7719(9) 0.263(14) Uiso 1 1 d . . . C64 C 0.2275(15) 0.850(3) 0.7569(10) 0.264(14) Uiso 1 1 d . . . C65 C 0.3766(19) -0.038(4) 0.9272(13) 0.34(2) Uiso 1 1 d . . . C66 C 0.336(2) 0.056(5) 0.951(2) 0.38(3) Uiso 1 1 d . . . C67 C 0.4326(19) 0.291(4) 0.9518(12) 0.35(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0340(3) 0.0406(3) 0.0343(3) 0.0014(2) 0.00515(19) -0.0008(2) Cd2 0.0396(3) 0.0383(3) 0.0356(3) 0.0002(2) 0.0069(2) 0.0001(2) Cd3 0.0639(4) 0.0423(3) 0.0523(3) 0.0041(2) 0.0232(3) 0.0052(3) N1 0.051(5) 0.087(6) 0.145(9) -0.029(6) 0.040(5) -0.027(4) N2 0.151(12) 0.132(11) 0.161(13) 0.000(10) -0.015(10) -0.074(10) N3 0.083(6) 0.097(7) 0.086(6) 0.022(5) -0.004(5) 0.007(5) O1 0.026(2) 0.065(3) 0.077(4) 0.004(3) 0.004(2) -0.004(2) O1W 0.141(8) 0.083(5) 0.125(7) -0.015(5) 0.045(6) 0.014(5) O2W 0.060(3) 0.041(3) 0.073(4) -0.012(3) -0.003(3) 0.007(3) O2 0.112(5) 0.057(4) 0.032(3) -0.005(2) 0.012(3) 0.025(3) O3 0.028(2) 0.054(3) 0.074(4) 0.008(3) 0.004(2) -0.002(2) O4 0.082(4) 0.046(3) 0.037(3) -0.006(2) 0.021(3) -0.001(3) O5 0.074(4) 0.109(5) 0.039(3) -0.002(3) 0.001(3) 0.026(4) O6 0.030(3) 0.074(4) 0.091(4) -0.027(3) 0.015(3) -0.001(3) O7 0.073(4) 0.106(5) 0.053(3) 0.021(3) 0.033(3) 0.042(4) O8 0.087(4) 0.046(3) 0.038(3) -0.005(2) 0.007(3) 0.004(3) O9 0.052(3) 0.046(3) 0.034(2) 0.002(2) 0.007(2) -0.006(2) O10 0.030(3) 0.090(4) 0.068(4) -0.027(3) 0.012(2) -0.001(3) O11 0.067(4) 0.074(5) 0.135(7) -0.002(5) 0.012(4) -0.031(4) O12 0.071(4) 0.051(3) 0.047(3) -0.014(3) 0.004(3) 0.004(3) O13 0.049(3) 0.081(4) 0.033(3) -0.012(3) 0.003(2) 0.005(3) O14 0.069(4) 0.075(4) 0.043(3) -0.004(3) -0.008(3) -0.010(3) O15 0.122(6) 0.085(5) 0.060(4) -0.004(4) -0.026(4) 0.005(5) O16 0.040(3) 0.060(4) 0.085(4) -0.010(3) 0.024(3) 0.009(3) O17 0.034(3) 0.061(4) 0.081(4) 0.000(3) 0.012(3) 0.001(3) O18 0.076(4) 0.049(3) 0.067(4) -0.015(3) 0.033(3) -0.003(3) O19 0.082(4) 0.045(3) 0.057(3) -0.001(3) 0.033(3) -0.003(3) O20 0.038(3) 0.068(4) 0.083(4) -0.001(3) 0.003(3) -0.003(3) O21 0.199(13) 0.145(10) 0.143(10) -0.010(8) 0.033(9) -0.066(9) O22 0.072(5) 0.106(6) 0.133(8) 0.035(5) -0.021(5) 0.011(5) C1 0.029(3) 0.052(4) 0.045(4) -0.002(3) 0.007(3) -0.003(3) C2 0.027(3) 0.047(4) 0.037(3) -0.003(3) 0.006(3) -0.002(3) C3 0.049(4) 0.048(4) 0.036(4) -0.009(3) 0.009(3) 0.004(3) C4 0.034(3) 0.048(4) 0.043(4) -0.003(3) 0.004(3) -0.001(3) C5 0.045(4) 0.045(4) 0.037(4) -0.009(3) 0.010(3) -0.005(3) C6 0.029(4) 0.069(5) 0.069(5) -0.006(4) 0.003(3) 0.001(4) C7 0.025(3) 0.063(5) 0.049(4) 0.002(4) 0.007(3) -0.002(3) C8 0.051(4) 0.072(5) 0.042(4) -0.002(4) 0.007(3) 0.008(4) C9 0.036(4) 0.070(5) 0.048(4) -0.003(4) 0.009(3) -0.002(4) C10 0.041(4) 0.067(5) 0.051(4) 0.005(4) 0.015(3) 0.011(4) C11 0.064(5) 0.056(5) 0.028(3) -0.005(3) 0.009(3) 0.001(4) C12 0.155(10) 0.051(5) 0.034(4) 0.008(4) 0.014(5) 0.024(6) C13 0.141(9) 0.041(5) 0.041(5) -0.002(4) 0.010(5) 0.026(5) C14 0.061(5) 0.042(4) 0.035(4) 0.004(3) 0.008(3) -0.003(3) C15 0.063(5) 0.038(4) 0.038(4) 0.002(3) 0.013(3) 0.004(3) C16 0.059(5) 0.041(4) 0.045(4) -0.008(3) 0.014(3) 0.000(3) C17 0.034(3) 0.042(4) 0.039(4) 0.006(3) 0.011(3) 0.000(3) C18 0.038(4) 0.054(5) 0.052(4) -0.003(4) 0.008(3) 0.001(3) C19 0.040(4) 0.057(5) 0.076(6) 0.012(4) -0.006(4) -0.005(4) C20 0.044(4) 0.050(5) 0.083(6) 0.010(4) 0.002(4) 0.002(4) C21 0.030(4) 0.060(5) 0.061(5) -0.007(4) 0.005(3) -0.001(3) C22 0.037(4) 0.063(5) 0.081(6) -0.003(4) 0.007(4) 0.012(4) C23 0.034(4) 0.048(5) 0.095(7) 0.004(4) 0.013(4) 0.005(3) C24 0.031(4) 0.068(6) 0.089(6) -0.022(5) 0.018(4) -0.004(4) C25 0.050(4) 0.045(4) 0.035(4) -0.007(3) 0.010(3) 0.002(3) C26 0.077(5) 0.053(5) 0.030(4) -0.002(3) 0.017(3) -0.004(4) C27 0.070(5) 0.043(4) 0.044(4) -0.002(3) 0.016(4) 0.000(4) C28 0.042(4) 0.051(4) 0.035(4) -0.004(3) 0.003(3) 0.004(3) C29 0.056(4) 0.055(5) 0.028(3) -0.002(3) 0.010(3) 0.002(4) C30 0.062(5) 0.047(4) 0.035(4) 0.001(3) 0.008(3) -0.002(4) C31 0.035(4) 0.050(4) 0.037(4) -0.008(3) -0.001(3) 0.003(3) C32 0.058(5) 0.084(6) 0.037(4) -0.005(4) 0.000(3) 0.004(5) C33 0.108(8) 0.072(6) 0.055(5) -0.001(5) -0.004(5) 0.025(6) C34 0.103(8) 0.074(6) 0.044(5) -0.010(4) -0.008(5) 0.018(6) C35 0.059(5) 0.078(6) 0.038(4) -0.004(4) -0.003(3) -0.016(5) C36 0.107(8) 0.070(6) 0.055(5) 0.002(5) -0.012(5) -0.007(6) C37 0.111(9) 0.082(7) 0.053(6) -0.009(5) -0.016(5) 0.003(6) C38 0.062(5) 0.061(5) 0.051(5) -0.002(4) 0.002(4) -0.017(4) C39 0.031(4) 0.072(5) 0.057(5) -0.014(4) 0.010(3) 0.003(4) C40 0.035(4) 0.059(5) 0.103(7) -0.030(5) 0.009(4) 0.001(4) C41 0.032(4) 0.059(5) 0.111(8) -0.022(5) 0.014(4) -0.008(4) C42 0.027(3) 0.057(5) 0.052(4) -0.003(3) 0.007(3) -0.001(3) C43 0.045(4) 0.053(5) 0.089(7) -0.001(4) 0.011(4) 0.008(4) C44 0.032(4) 0.056(5) 0.102(7) -0.001(5) 0.016(4) -0.005(4) C45 0.039(4) 0.056(5) 0.044(4) 0.000(3) 0.004(3) 0.000(4) C46 0.051(4) 0.075(6) 0.042(4) 0.006(4) 0.017(3) 0.020(4) C47 0.081(6) 0.063(5) 0.064(5) -0.001(4) 0.035(5) 0.021(5) C48 0.079(6) 0.045(4) 0.061(5) 0.006(4) 0.029(4) 0.016(4) C49 0.039(4) 0.051(4) 0.039(4) -0.002(3) 0.009(3) 0.005(3) C50 0.051(4) 0.047(4) 0.055(5) -0.002(4) 0.019(4) -0.001(4) C51 0.064(5) 0.058(5) 0.052(5) 0.006(4) 0.023(4) -0.004(4) C52 0.052(4) 0.044(4) 0.035(4) -0.002(3) 0.004(3) 0.009(3) C53 0.051(5) 0.084(7) 0.090(7) -0.012(6) 0.012(5) 0.000(5) C54 0.048(7) 0.141(13) 0.26(2) -0.020(14) -0.023(9) 0.000(8) C55 0.161(16) 0.141(14) 0.200(19) -0.024(13) 0.097(15) -0.084(12) C56 0.136(14) 0.121(13) 0.159(16) 0.017(11) -0.016(12) -0.047(11) C57 0.23(3) 0.49(6) 0.14(2) 0.10(3) -0.011(18) 0.07(3) C58 0.18(2) 0.17(2) 0.27(3) 0.01(2) 0.00(2) -0.051(18) C59 0.061(6) 0.113(9) 0.105(9) 0.053(8) -0.015(6) -0.003(7) C60 0.104(10) 0.151(14) 0.139(13) -0.019(10) 0.002(9) 0.060(10) C61 0.093(9) 0.128(11) 0.101(10) -0.019(8) -0.023(7) 0.003(8) _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 O12 2.247(5) 4_566 ? Cd1 O17 2.250(5) 3_567 ? Cd1 O2W 2.274(5) . ? Cd1 O20 2.303(6) . ? Cd1 O9 2.345(5) . ? Cd1 O8 2.517(5) . ? Cd2 O14 2.210(5) . ? Cd2 O16 2.220(5) 3_567 ? Cd2 O13 2.245(5) 4_566 ? Cd2 O9 2.315(5) . ? Cd2 O10 2.325(5) 3_667 ? Cd2 O18 2.329(6) 4_566 ? Cd2 Cd3 3.4261(11) . ? Cd3 O15 2.207(7) . ? Cd3 O1W 2.228(8) . ? Cd3 O19 2.303(5) 4_566 ? Cd3 O10 2.336(6) 3_667 ? Cd3 O21 2.427(12) . ? Cd3 O18 2.492(6) 4_566 ? Cd3 O11 2.634(7) 3_667 ? Cd3 C52 2.729(7) 4_566 ? N1 C53 1.339(12) . ? N1 C55 1.448(17) . ? N1 C54 1.503(18) . ? N2 C56 1.295(19) . ? N2 C58 1.36(2) . ? N2 C57 1.47(2) . ? N3 C59 1.349(13) . ? N3 C61 1.478(16) . ? N3 C60 1.495(16) . ? N4 C63 1.33(3) . ? N4 C62 1.42(3) . ? N4 C64 1.45(4) . ? N5 C66 1.31(8) . ? O1 C1 1.404(8) . ? O1 C6 1.410(9) . ? O2 C11 1.367(8) . ? O2 C3 1.420(9) . ? O3 C18 1.357(9) . ? O3 C4 1.415(8) . ? O4 C25 1.379(8) . ? O4 C5 1.424(8) . ? O5 C32 1.353(10) . ? O5 C8 1.431(10) . ? O6 C39 1.388(9) . ? O6 C9 1.426(9) . ? O7 C46 1.377(9) . ? O7 C10 1.428(10) . ? O8 C17 1.244(8) . ? O9 C17 1.263(8) . ? O10 C24 1.286(11) . ? O10 Cd2 2.325(5) 3_667 ? O10 Cd3 2.336(6) 3_667 ? O11 C24 1.255(12) . ? O11 Cd3 2.634(7) 3_667 ? O12 C31 1.258(9) . ? O12 Cd1 2.247(5) 4_565 ? O13 C31 1.262(9) . ? O13 Cd2 2.245(5) 4_565 ? O14 C38 1.232(10) . ? O15 C38 1.252(11) . ? O16 C45 1.248(9) . ? O16 Cd2 2.220(5) 3_567 ? O17 C45 1.265(9) . ? O17 Cd1 2.250(5) 3_567 ? O18 C52 1.227(9) . ? O18 Cd2 2.329(5) 4_565 ? O18 Cd3 2.492(6) 4_565 ? O19 C52 1.249(9) . ? O19 Cd3 2.303(5) 4_565 ? O20 C53 1.206(12) . ? O21 C56 1.231(18) . ? O22 C59 1.239(15) . ? O23 C62 1.51(3) . ? O24 C66 1.57(7) . ? C1 C2 1.526(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.524(9) . ? C2 C5 1.526(9) . ? C2 C4 1.526(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.529(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C10 1.524(11) . ? C7 C8 1.534(11) . ? C7 C9 1.535(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.375(11) . ? C11 C16 1.386(11) . ? C12 C13 1.388(11) . ? C12 H12A 0.9300 . ? C13 C14 1.382(11) . ? C13 H13A 0.9300 . ? C14 C15 1.393(10) . ? C14 C17 1.482(10) . ? C15 C16 1.376(10) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C19 1.374(11) . ? C18 C23 1.405(11) . ? C19 C20 1.389(11) . ? C19 H19A 0.9300 . ? C20 C21 1.398(11) . ? C20 H20A 0.9300 . ? C21 C22 1.393(12) . ? C21 C24 1.469(11) . ? C22 C23 1.377(11) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C26 1.383(11) . ? C25 C30 1.384(10) . ? C26 C27 1.382(10) . ? C26 H26A 0.9300 . ? C27 C28 1.379(10) . ? C27 H27A 0.9300 . ? C28 C29 1.380(11) . ? C28 C31 1.497(10) . ? C29 C30 1.369(10) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C32 C37 1.358(14) . ? C32 C33 1.386(13) . ? C33 C34 1.375(13) . ? C33 H33A 0.9300 . ? C34 C35 1.376(13) . ? C34 H34A 0.9300 . ? C35 C36 1.380(13) . ? C35 C38 1.500(11) . ? C36 C37 1.442(13) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C39 C40 1.363(12) . ? C39 C44 1.375(12) . ? C40 C41 1.364(11) . ? C40 H40A 0.9300 . ? C41 C42 1.389(11) . ? C41 H41A 0.9300 . ? C42 C43 1.387(11) . ? C42 C45 1.500(10) . ? C43 C44 1.367(11) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C46 C51 1.363(12) . ? C46 C47 1.404(12) . ? C47 C48 1.385(11) . ? C47 H47A 0.9300 . ? C48 C49 1.371(10) . ? C48 H48A 0.9300 . ? C49 C50 1.391(11) . ? C49 C52 1.518(10) . ? C50 C51 1.403(10) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 Cd3 2.729(7) 4_565 ? C53 H53A 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C65 C66 1.76(6) . ? 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 O12 Cd1 O17 90.7(2) 4_566 3_567 ? O12 Cd1 O2W 100.6(2) 4_566 . ? O17 Cd1 O2W 86.5(2) 3_567 . ? O12 Cd1 O20 92.5(2) 4_566 . ? O17 Cd1 O20 171.4(2) 3_567 . ? O2W Cd1 O20 85.1(2) . . ? O12 Cd1 O9 117.24(19) 4_566 . ? O17 Cd1 O9 92.3(2) 3_567 . ? O2W Cd1 O9 142.1(2) . . ? O20 Cd1 O9 93.3(2) . . ? O12 Cd1 O8 170.01(19) 4_566 . ? O17 Cd1 O8 91.1(2) 3_567 . ? O2W Cd1 O8 89.3(2) . . ? O20 Cd1 O8 87.0(2) . . ? O9 Cd1 O8 52.87(17) . . ? O14 Cd2 O16 97.2(2) . 3_567 ? O14 Cd2 O13 172.4(2) . 4_566 ? O16 Cd2 O13 88.8(2) 3_567 4_566 ? O14 Cd2 O9 93.5(2) . . ? O16 Cd2 O9 95.4(2) 3_567 . ? O13 Cd2 O9 81.25(19) 4_566 . ? O14 Cd2 O10 90.0(2) . 3_667 ? O16 Cd2 O10 168.9(2) 3_567 3_667 ? O13 Cd2 O10 84.8(2) 4_566 3_667 ? O9 Cd2 O10 92.6(2) . 3_667 ? O14 Cd2 O18 87.9(2) . 4_566 ? O16 Cd2 O18 87.0(2) 3_567 4_566 ? O13 Cd2 O18 97.1(2) 4_566 4_566 ? O9 Cd2 O18 177.1(2) . 4_566 ? O10 Cd2 O18 84.9(2) 3_667 4_566 ? O14 Cd2 Cd3 72.95(17) . . ? O16 Cd2 Cd3 131.87(16) 3_567 . ? O13 Cd2 Cd3 106.47(16) 4_566 . ? O9 Cd2 Cd3 131.46(12) . . ? O10 Cd2 Cd3 42.81(15) 3_667 . ? O18 Cd2 Cd3 46.67(14) 4_566 . ? O15 Cd3 O1W 106.7(3) . . ? O15 Cd3 O19 132.2(3) . 4_566 ? O1W Cd3 O19 105.5(3) . 4_566 ? O15 Cd3 O10 84.2(3) . 3_667 ? O1W Cd3 O10 107.2(3) . 3_667 ? O19 Cd3 O10 118.2(2) 4_566 3_667 ? O15 Cd3 O21 73.5(4) . . ? O1W Cd3 O21 77.3(4) . . ? O19 Cd3 O21 80.3(3) 4_566 . ? O10 Cd3 O21 157.5(4) 3_667 . ? O15 Cd3 O18 94.2(3) . 4_566 ? O1W Cd3 O18 158.1(3) . 4_566 ? O19 Cd3 O18 53.76(18) 4_566 4_566 ? O10 Cd3 O18 81.07(18) 3_667 4_566 ? O21 Cd3 O18 103.0(4) . 4_566 ? O15 Cd3 O11 133.4(3) . 3_667 ? O1W Cd3 O11 75.6(3) . 3_667 ? O19 Cd3 O11 88.5(2) 4_566 3_667 ? O10 Cd3 O11 52.6(2) 3_667 3_667 ? O21 Cd3 O11 146.6(4) . 3_667 ? O18 Cd3 O11 95.1(2) 4_566 3_667 ? O15 Cd3 C52 114.1(3) . 4_566 ? O1W Cd3 C52 132.4(3) . 4_566 ? O19 Cd3 C52 27.08(19) 4_566 4_566 ? O10 Cd3 C52 100.5(2) 3_667 4_566 ? O21 Cd3 C52 91.4(3) . 4_566 ? O18 Cd3 C52 26.7(2) 4_566 4_566 ? O11 Cd3 C52 92.6(2) 3_667 4_566 ? O15 Cd3 Cd2 74.3(2) . . ? O1W Cd3 Cd2 149.7(3) . . ? O19 Cd3 Cd2 94.09(14) 4_566 . ? O10 Cd3 Cd2 42.56(12) 3_667 . ? O21 Cd3 Cd2 129.6(4) . . ? O18 Cd3 Cd2 42.82(13) 4_566 . ? O11 Cd3 Cd2 82.26(18) 3_667 . ? C52 Cd3 Cd2 68.20(16) 4_566 . ? C53 N1 C55 119.6(13) . . ? C53 N1 C54 118.3(10) . . ? C55 N1 C54 122.1(12) . . ? C56 N2 C58 116.8(19) . . ? C56 N2 C57 125(2) . . ? C58 N2 C57 117(2) . . ? C59 N3 C61 123.0(11) . . ? C59 N3 C60 121.0(12) . . ? C61 N3 C60 115.6(10) . . ? C63 N4 C62 136(3) . . ? C63 N4 C64 122(3) . . ? C62 N4 C64 101(2) . . ? C1 O1 C6 113.8(6) . . ? C11 O2 C3 120.2(6) . . ? C18 O3 C4 117.0(6) . . ? C25 O4 C5 118.5(6) . . ? C32 O5 C8 119.2(7) . . ? C39 O6 C9 117.7(6) . . ? C46 O7 C10 118.4(6) . . ? C17 O8 Cd1 89.8(4) . . ? C17 O9 Cd2 148.0(5) . . ? C17 O9 Cd1 97.4(4) . . ? Cd2 O9 Cd1 99.38(17) . . ? C24 O10 Cd2 128.4(5) . 3_667 ? C24 O10 Cd3 99.2(6) . 3_667 ? Cd2 O10 Cd3 94.62(18) 3_667 3_667 ? C24 O11 Cd3 86.1(6) . 3_667 ? C31 O12 Cd1 108.2(4) . 4_565 ? C31 O13 Cd2 130.5(5) . 4_565 ? C38 O14 Cd2 132.5(6) . . ? C38 O15 Cd3 130.7(6) . . ? C45 O16 Cd2 138.1(5) . 3_567 ? C45 O17 Cd1 123.7(5) . 3_567 ? C52 O18 Cd2 158.3(6) . 4_565 ? C52 O18 Cd3 87.5(5) . 4_565 ? Cd2 O18 Cd3 90.51(18) 4_565 4_565 ? C52 O19 Cd3 95.9(4) . 4_565 ? C53 O20 Cd1 122.6(6) . . ? C56 O21 Cd3 132.0(12) . . ? O1 C1 C2 108.6(6) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C3 C2 C5 107.1(6) . . ? C3 C2 C1 111.1(5) . . ? C5 C2 C1 109.9(6) . . ? C3 C2 C4 110.3(6) . . ? C5 C2 C4 110.5(5) . . ? C1 C2 C4 107.9(6) . . ? O2 C3 C2 106.8(6) . . ? O2 C3 H3A 110.4 . . ? C2 C3 H3A 110.4 . . ? O2 C3 H3B 110.4 . . ? C2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? O3 C4 C2 109.2(6) . . ? O3 C4 H4A 109.8 . . ? C2 C4 H4A 109.8 . . ? O3 C4 H4B 109.8 . . ? C2 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? O4 C5 C2 106.6(6) . . ? O4 C5 H5A 110.4 . . ? C2 C5 H5A 110.4 . . ? O4 C5 H5B 110.4 . . ? C2 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O1 C6 C7 108.0(7) . . ? O1 C6 H6A 110.1 . . ? C7 C6 H6A 110.1 . . ? O1 C6 H6B 110.1 . . ? C7 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C10 C7 C6 110.9(6) . . ? C10 C7 C8 107.9(6) . . ? C6 C7 C8 109.9(6) . . ? C10 C7 C9 110.6(6) . . ? C6 C7 C9 107.2(6) . . ? C8 C7 C9 110.3(6) . . ? O5 C8 C7 107.4(7) . . ? O5 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O5 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O6 C9 C7 108.4(6) . . ? O6 C9 H9A 110.0 . . ? C7 C9 H9A 110.0 . . ? O6 C9 H9B 110.0 . . ? C7 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O7 C10 C7 107.3(7) . . ? O7 C10 H10A 110.2 . . ? C7 C10 H10A 110.2 . . ? O7 C10 H10B 110.2 . . ? C7 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O2 C11 C12 114.9(7) . . ? O2 C11 C16 125.8(7) . . ? C12 C11 C16 119.3(7) . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 121.2(8) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 117.6(7) . . ? C13 C14 C17 120.4(7) . . ? C15 C14 C17 121.9(6) . . ? C16 C15 C14 121.5(7) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 C11 120.0(7) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? O8 C17 O9 119.9(6) . . ? O8 C17 C14 120.6(6) . . ? O9 C17 C14 119.5(6) . . ? O3 C18 C19 125.3(7) . . ? O3 C18 C23 115.5(7) . . ? C19 C18 C23 119.2(7) . . ? C18 C19 C20 119.9(8) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C21 121.4(8) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C22 C21 C20 118.0(7) . . ? C22 C21 C24 121.1(7) . . ? C20 C21 C24 120.8(8) . . ? C23 C22 C21 120.7(7) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C18 120.6(8) . . ? C22 C23 H23A 119.7 . . ? C18 C23 H23A 119.7 . . ? O11 C24 O10 121.5(8) . . ? O11 C24 C21 118.9(8) . . ? O10 C24 C21 119.3(9) . . ? O4 C25 C26 124.1(6) . . ? O4 C25 C30 115.7(7) . . ? C26 C25 C30 120.2(6) . . ? C27 C26 C25 119.2(7) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C28 C27 C26 121.1(7) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C27 C28 C29 118.7(7) . . ? C27 C28 C31 120.0(7) . . ? C29 C28 C31 121.1(6) . . ? C30 C29 C28 121.2(7) . . ? C30 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C29 C30 C25 119.6(7) . . ? C29 C30 H30A 120.2 . . ? C25 C30 H30A 120.2 . . ? O12 C31 O13 123.9(7) . . ? O12 C31 C28 117.9(6) . . ? O13 C31 C28 118.2(7) . . ? O5 C32 C37 123.6(8) . . ? O5 C32 C33 116.3(9) . . ? C37 C32 C33 120.0(8) . . ? C34 C33 C32 120.4(9) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 121.9(9) . . ? C33 C34 H34A 119.0 . . ? C35 C34 H34A 119.0 . . ? C34 C35 C36 118.0(8) . . ? C34 C35 C38 121.0(8) . . ? C36 C35 C38 121.0(9) . . ? C35 C36 C37 120.7(10) . . ? C35 C36 H36A 119.6 . . ? C37 C36 H36A 119.6 . . ? C32 C37 C36 118.9(9) . . ? C32 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? O14 C38 O15 126.3(8) . . ? O14 C38 C35 117.4(9) . . ? O15 C38 C35 116.4(8) . . ? C40 C39 C44 120.1(7) . . ? C40 C39 O6 115.5(7) . . ? C44 C39 O6 124.4(7) . . ? C39 C40 C41 120.3(8) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C42 121.4(8) . . ? C40 C41 H41A 119.3 . . ? C42 C41 H41A 119.3 . . ? C43 C42 C41 116.9(7) . . ? C43 C42 C45 120.3(7) . . ? C41 C42 C45 122.8(7) . . ? C44 C43 C42 122.0(8) . . ? C44 C43 H43A 119.0 . . ? C42 C43 H43A 119.0 . . ? C43 C44 C39 119.2(8) . . ? C43 C44 H44A 120.4 . . ? C39 C44 H44A 120.4 . . ? O16 C45 O17 125.8(7) . . ? O16 C45 C42 117.3(7) . . ? O17 C45 C42 116.9(7) . . ? C51 C46 O7 124.4(8) . . ? C51 C46 C47 121.0(7) . . ? O7 C46 C47 114.6(7) . . ? C48 C47 C46 118.3(8) . . ? C48 C47 H47A 120.8 . . ? C46 C47 H47A 120.8 . . ? C49 C48 C47 121.2(8) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? C48 C49 C50 120.3(7) . . ? C48 C49 C52 120.3(7) . . ? C50 C49 C52 119.4(6) . . ? C49 C50 C51 119.0(7) . . ? C49 C50 H50A 120.5 . . ? C51 C50 H50A 120.5 . . ? C46 C51 C50 120.2(8) . . ? C46 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? O18 C52 O19 122.8(7) . . ? O18 C52 C49 118.9(7) . . ? O19 C52 C49 118.1(6) . . ? O18 C52 Cd3 65.8(4) . 4_565 ? O19 C52 Cd3 57.1(4) . 4_565 ? C49 C52 Cd3 173.0(5) . 4_565 ? O20 C53 N1 126.1(11) . . ? O20 C53 H53A 117.0 . . ? N1 C53 H53A 117.0 . . ? N1 C54 H54A 109.5 . . ? N1 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N1 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N1 C55 H55A 109.5 . . ? N1 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N1 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O21 C56 N2 120.9(19) . . ? O21 C56 H56A 119.5 . . ? N2 C56 H56A 119.5 . . ? N2 C57 H57A 109.5 . . ? N2 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N2 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N2 C58 H58A 109.5 . . ? N2 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N2 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O22 C59 N3 121.8(13) . . ? N4 C62 O23 92(2) . . ? N5 C66 O24 175(7) . . ? N5 C66 C65 81(5) . . ? O24 C66 C65 95(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.375 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.153 #===end data_2 _database_code_depnum_ccdc_archive 'CCDC 893228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H50 Cd3 N4 O19' _chemical_formula_weight 1516.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.766(6) _cell_length_b 20.293(5) _cell_length_c 16.483(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.107(4) _cell_angle_gamma 90.00 _cell_volume 9288(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6599 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24231 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8570 _reflns_number_gt 4496 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1461P)^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_number_reflns 8570 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2603 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.7500 0.2500 0.5000 0.0508(3) Uani 1 2 d S . . Cd2 Cd 0.77216(3) 0.41563(3) 0.54923(4) 0.0640(3) Uani 1 1 d . . . N1 N 0.7665(3) 0.5188(3) 0.5865(5) 0.069(2) Uani 1 1 d . . . N2 N 0.7584(3) 0.6253(3) 0.5736(5) 0.0641(19) Uani 1 1 d . . . O1 O 0.5000 0.3243(4) 0.7500 0.079(3) Uani 1 2 d S . . O2 O 0.6223(2) 0.3297(3) 0.8745(4) 0.0733(18) Uani 1 1 d . . . O3 O 0.5952(2) 0.3086(3) 1.0485(4) 0.0726(16) Uani 1 1 d . . . O4 O 0.4815(2) 0.2926(4) 0.9384(5) 0.089(2) Uani 1 1 d . . . O5 O 0.7482(2) 0.3788(3) 0.6496(4) 0.0787(19) Uani 1 1 d . . . O6 O 0.7281(2) 0.2739(3) 0.6119(4) 0.0671(16) Uani 1 1 d . . . O7 O 0.7233(3) 0.4494(4) 1.3965(4) 0.089(2) Uani 1 1 d . . . O8 O 0.7194(2) 0.3497(3) 1.4436(4) 0.0775(19) Uani 1 1 d . . . O9 O 0.3189(2) 0.1880(3) 1.0613(4) 0.0682(16) Uani 1 1 d . . . O10 O 0.3397(3) 0.0940(4) 1.0177(6) 0.093(2) Uani 1 1 d . . . C1 C 0.5493(3) 0.3146(4) 0.8985(5) 0.055(2) Uani 1 1 d . . . C2 C 0.5216(3) 0.3621(5) 0.8263(5) 0.077(3) Uani 1 1 d . . . H2A H 0.4971 0.3850 0.8415 0.092 Uiso 1 1 calc R . . H2B H 0.5433 0.3946 0.8173 0.092 Uiso 1 1 calc R . . C3 C 0.5887(3) 0.2797(5) 0.8758(6) 0.067(2) Uani 1 1 d . . . H3A H 0.6044 0.2465 0.9190 0.080 Uiso 1 1 calc R . . H3B H 0.5753 0.2586 0.8194 0.080 Uiso 1 1 calc R . . C4 C 0.5719(3) 0.3519(5) 0.9812(5) 0.062(2) Uani 1 1 d . . . H4A H 0.5949 0.3834 0.9746 0.074 Uiso 1 1 calc R . . H4B H 0.5474 0.3761 0.9947 0.074 Uiso 1 1 calc R . . C5 C 0.5154(3) 0.2597(5) 0.9092(6) 0.071(3) Uani 1 1 d . . . H5A H 0.4990 0.2377 0.8543 0.085 Uiso 1 1 calc R . . H5B H 0.5336 0.2273 0.9516 0.085 Uiso 1 1 calc R . . C6 C 0.6486(3) 0.3230(4) 0.8217(5) 0.060(2) Uani 1 1 d . . . C7 C 0.6499(3) 0.2674(5) 0.7760(6) 0.066(2) Uani 1 1 d . . . H7A H 0.6327 0.2301 0.7802 0.080 Uiso 1 1 calc R . . C8 C 0.6774(3) 0.2671(4) 0.7231(5) 0.060(2) Uani 1 1 d . . . H8A H 0.6787 0.2295 0.6918 0.072 Uiso 1 1 calc R . . C9 C 0.7026(3) 0.3231(4) 0.7174(5) 0.057(2) Uani 1 1 d . . . C10 C 0.7019(3) 0.3763(5) 0.7658(6) 0.063(2) Uani 1 1 d . . . H10A H 0.7195 0.4136 0.7631 0.076 Uiso 1 1 calc R . . C11 C 0.6758(3) 0.3760(5) 0.8186(6) 0.067(2) Uani 1 1 d . . . H11A H 0.6766 0.4126 0.8530 0.080 Uiso 1 1 calc R . . C12 C 0.7282(3) 0.3249(5) 0.6545(5) 0.058(2) Uani 1 1 d . . . C13 C 0.6212(3) 0.3323(5) 1.1284(6) 0.068(2) Uani 1 1 d . . . C14 C 0.6292(4) 0.3970(6) 1.1493(7) 0.088(3) Uani 1 1 d . . . H14A H 0.6156 0.4285 1.1064 0.106 Uiso 1 1 calc R . . C15 C 0.6568(4) 0.4176(5) 1.2323(6) 0.085(3) Uani 1 1 d . . . H15A H 0.6611 0.4622 1.2455 0.102 Uiso 1 1 calc R . . C16 C 0.6778(3) 0.3711(5) 1.2944(6) 0.065(2) Uiso 1 1 d . . . C17 C 0.6686(4) 0.3065(5) 1.2729(6) 0.078(3) Uani 1 1 d . . . H17A H 0.6810 0.2749 1.3161 0.094 Uiso 1 1 calc R . . C18 C 0.6421(4) 0.2859(5) 1.1913(6) 0.078(3) Uani 1 1 d . . . H18A H 0.6382 0.2412 1.1783 0.094 Uiso 1 1 calc R . . C19 C 0.7090(4) 0.3916(5) 1.3826(6) 0.071(3) Uani 1 1 d . . . C20 C 0.4509(3) 0.2557(5) 0.9609(7) 0.072(3) Uani 1 1 d . . . C21 C 0.4233(4) 0.2869(5) 0.9964(8) 0.093(4) Uani 1 1 d . . . H21A H 0.4271 0.3321 1.0054 0.112 Uiso 1 1 calc R . . C22 C 0.3894(4) 0.2550(5) 1.0204(7) 0.084(3) Uani 1 1 d . . . H22A H 0.3708 0.2786 1.0452 0.101 Uiso 1 1 calc R . . C23 C 0.3828(3) 0.1889(5) 1.0082(6) 0.071(2) Uani 1 1 d . . . C24 C 0.4107(4) 0.1562(5) 0.9731(8) 0.096(4) Uani 1 1 d . . . H24A H 0.4077 0.1108 0.9658 0.115 Uiso 1 1 calc R . . C25 C 0.4446(4) 0.1907(6) 0.9472(7) 0.089(3) Uani 1 1 d . . . H25A H 0.4627 0.1681 0.9205 0.106 Uiso 1 1 calc R . . C26 C 0.3447(3) 0.1541(5) 1.0303(6) 0.068(2) Uani 1 1 d . . . C27 C 0.7646(3) 0.5681(4) 0.5363(7) 0.069(3) Uani 1 1 d . . . H27A H 0.7671 0.5650 0.4819 0.083 Uiso 1 1 calc R . . C28 C 0.7556(4) 0.6083(6) 0.6520(7) 0.092(3) Uani 1 1 d . . . H28A H 0.7510 0.6370 0.6922 0.111 Uiso 1 1 calc R . . C29 C 0.7608(5) 0.5427(5) 0.6602(8) 0.098(4) Uani 1 1 d . . . H29A H 0.7606 0.5178 0.7075 0.118 Uiso 1 1 calc R . . C30 C 0.7549(3) 0.6899(4) 0.5372(6) 0.058(2) Uani 1 1 d . . . C31 C 0.7805(3) 0.7049(4) 0.4877(7) 0.073(3) Uani 1 1 d . . . H31A H 0.8013 0.6737 0.4792 0.088 Uiso 1 1 calc R . . C32 C 0.7235(4) 0.7340(4) 0.5507(6) 0.071(3) Uani 1 1 d . . . H32A H 0.7055 0.7231 0.5846 0.085 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 0.0629(6) 0.0432(5) 0.0575(5) 0.0025(4) 0.0351(4) 0.0043(4) Cd2 0.0880(5) 0.0432(4) 0.0774(5) -0.0008(3) 0.0499(4) 0.0003(3) N1 0.099(6) 0.040(4) 0.079(5) 0.003(4) 0.045(4) 0.005(4) N2 0.090(5) 0.039(4) 0.074(5) -0.001(3) 0.043(4) -0.002(4) O1 0.093(6) 0.065(6) 0.065(6) 0.000 0.013(5) 0.000 O2 0.070(4) 0.091(5) 0.077(4) -0.013(3) 0.048(3) -0.012(3) O3 0.085(4) 0.074(4) 0.054(4) 0.003(3) 0.020(3) 0.001(3) O4 0.070(4) 0.087(5) 0.139(6) -0.005(4) 0.073(4) -0.007(4) O5 0.110(5) 0.062(4) 0.093(5) -0.004(4) 0.071(4) -0.017(4) O6 0.080(4) 0.064(4) 0.078(4) 0.003(3) 0.053(3) 0.003(3) O7 0.127(6) 0.069(5) 0.062(4) 0.007(4) 0.022(4) 0.000(4) O8 0.104(5) 0.065(4) 0.058(4) 0.018(3) 0.022(3) 0.025(4) O9 0.061(4) 0.082(4) 0.074(4) 0.007(3) 0.038(3) 0.003(3) O10 0.089(5) 0.071(5) 0.145(7) 0.002(4) 0.073(5) -0.002(4) C1 0.053(5) 0.067(5) 0.056(5) 0.003(4) 0.033(4) 0.005(4) C2 0.079(6) 0.098(8) 0.052(5) -0.002(5) 0.024(5) -0.004(6) C3 0.056(5) 0.085(7) 0.071(6) -0.003(5) 0.035(4) -0.011(5) C4 0.072(6) 0.065(6) 0.057(5) 0.005(4) 0.034(4) 0.002(4) C5 0.071(6) 0.077(7) 0.076(6) -0.003(5) 0.041(5) 0.003(5) C6 0.063(5) 0.066(6) 0.065(5) 0.001(4) 0.041(4) 0.001(4) C7 0.074(6) 0.070(6) 0.071(6) 0.004(5) 0.045(5) -0.005(5) C8 0.075(6) 0.054(5) 0.063(5) -0.005(4) 0.040(5) 0.002(4) C9 0.053(5) 0.068(6) 0.057(5) 0.005(4) 0.028(4) -0.002(4) C10 0.066(6) 0.069(6) 0.071(6) -0.010(5) 0.044(5) -0.012(4) C11 0.077(6) 0.068(6) 0.063(5) -0.017(5) 0.036(5) -0.010(5) C12 0.058(5) 0.069(6) 0.059(5) 0.006(4) 0.036(4) 0.015(4) C13 0.079(6) 0.065(7) 0.067(6) 0.008(5) 0.035(5) 0.012(5) C14 0.105(8) 0.088(9) 0.061(6) 0.018(6) 0.017(6) 0.015(6) C15 0.118(9) 0.064(6) 0.063(6) 0.012(5) 0.019(6) 0.015(6) C17 0.115(8) 0.065(6) 0.053(5) 0.010(5) 0.028(5) 0.011(6) C18 0.110(8) 0.055(6) 0.067(6) 0.010(5) 0.028(6) 0.006(5) C19 0.083(7) 0.060(6) 0.068(6) -0.007(5) 0.026(5) 0.015(5) C20 0.068(6) 0.061(6) 0.103(7) 0.006(5) 0.050(6) 0.001(5) C21 0.091(7) 0.068(7) 0.152(10) -0.035(7) 0.082(8) -0.022(6) C22 0.089(7) 0.069(7) 0.114(9) -0.018(6) 0.061(7) 0.003(5) C23 0.068(6) 0.067(6) 0.088(7) -0.007(5) 0.041(5) -0.003(5) C24 0.098(8) 0.059(6) 0.168(11) -0.023(7) 0.093(8) -0.010(6) C25 0.100(8) 0.075(7) 0.121(9) -0.015(6) 0.074(7) -0.004(6) C26 0.070(6) 0.071(7) 0.073(6) 0.009(5) 0.039(5) 0.005(5) C27 0.090(7) 0.042(5) 0.085(6) -0.012(5) 0.043(5) 0.008(4) C28 0.150(10) 0.074(7) 0.083(7) -0.009(6) 0.077(7) 0.003(7) C29 0.178(12) 0.043(6) 0.105(8) 0.005(6) 0.088(9) 0.003(6) C30 0.075(6) 0.043(5) 0.066(5) -0.002(4) 0.038(4) -0.005(4) C31 0.091(7) 0.038(5) 0.110(8) 0.006(5) 0.060(6) 0.012(4) C32 0.092(7) 0.053(6) 0.089(7) -0.008(5) 0.058(6) -0.003(5) _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 O6 2.219(5) 7_656 ? Cd1 O6 2.219(5) . ? Cd1 O8 2.274(6) 1_554 ? Cd1 O8 2.274(6) 7_657 ? Cd1 O9 2.307(6) 8 ? Cd1 O9 2.307(6) 2_656 ? Cd1 Cd2 3.4648(10) . ? Cd1 Cd2 3.4648(10) 7_656 ? Cd2 O5 2.158(6) . ? Cd2 N1 2.205(7) . ? Cd2 O10 2.259(6) 8 ? Cd2 O8 2.307(7) 1_554 ? Cd2 O9 2.490(6) 8 ? Cd2 O7 2.508(6) 1_554 ? Cd2 C26 2.693(9) 8 ? Cd2 C19 2.757(10) 1_554 ? N1 C27 1.287(11) . ? N1 C29 1.373(12) . ? N2 C27 1.356(10) . ? N2 C28 1.367(11) . ? N2 C30 1.431(11) . ? O1 C2 1.414(10) 2_656 ? O1 C2 1.414(10) . ? O2 C6 1.369(9) . ? O2 C3 1.430(10) . ? O3 C13 1.352(11) . ? O3 C4 1.389(10) . ? O4 C20 1.332(10) . ? O4 C5 1.429(10) . ? O5 C12 1.260(10) . ? O6 C12 1.251(10) . ? O7 C19 1.241(11) . ? O7 Cd2 2.508(6) 1_556 ? O8 C19 1.267(11) . ? O8 Cd1 2.274(6) 1_556 ? O8 Cd2 2.307(7) 1_556 ? O9 C26 1.267(10) . ? O9 Cd1 2.307(6) 2_656 ? O9 Cd2 2.490(6) 8_456 ? O10 C26 1.238(11) . ? O10 Cd2 2.259(6) 8_456 ? C1 C4 1.492(11) . ? C1 C2 1.523(12) . ? C1 C3 1.529(11) . ? C1 C5 1.554(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C11 1.360(12) . ? C6 C7 1.365(12) . ? C7 C8 1.394(10) . ? C7 H7A 0.9300 . ? C8 C9 1.384(11) . ? C8 H8A 0.9300 . ? C9 C10 1.346(12) . ? C9 C12 1.493(10) . ? C10 C11 1.359(11) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.357(14) . ? C13 C18 1.372(12) . ? C14 C15 1.383(14) . ? C14 H14A 0.9300 . ? C15 C16 1.367(13) . ? C15 H15A 0.9300 . ? C16 C17 1.361(13) . ? C16 C19 1.474(13) . ? C17 C18 1.356(13) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 Cd2 2.757(10) 1_556 ? C20 C21 1.328(12) . ? C20 C25 1.340(13) . ? C21 C22 1.372(13) . ? C21 H21A 0.9300 . ? C22 C23 1.359(13) . ? C22 H22A 0.9300 . ? C23 C24 1.346(12) . ? C23 C26 1.487(13) . ? C24 C25 1.415(13) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 Cd2 2.693(9) 8_456 ? C27 H27A 0.9300 . ? C28 C29 1.342(14) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.337(11) . ? C30 C32 1.369(11) . ? C31 C32 1.377(12) 7_666 ? C31 H31A 0.9300 . ? C32 C31 1.377(12) 7_666 ? C32 H32A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cd1 O6 180.0(3) 7_656 . ? O6 Cd1 O8 92.8(2) 7_656 1_554 ? O6 Cd1 O8 87.2(2) . 1_554 ? O6 Cd1 O8 87.2(2) 7_656 7_657 ? O6 Cd1 O8 92.8(2) . 7_657 ? O8 Cd1 O8 180.0(3) 1_554 7_657 ? O6 Cd1 O9 90.1(2) 7_656 8 ? O6 Cd1 O9 89.9(2) . 8 ? O8 Cd1 O9 81.7(2) 1_554 8 ? O8 Cd1 O9 98.3(2) 7_657 8 ? O6 Cd1 O9 89.9(2) 7_656 2_656 ? O6 Cd1 O9 90.1(2) . 2_656 ? O8 Cd1 O9 98.3(2) 1_554 2_656 ? O8 Cd1 O9 81.7(2) 7_657 2_656 ? O9 Cd1 O9 180.0(4) 8 2_656 ? O6 Cd1 Cd2 108.55(16) 7_656 . ? O6 Cd1 Cd2 71.45(16) . . ? O8 Cd1 Cd2 41.20(17) 1_554 . ? O8 Cd1 Cd2 138.80(17) 7_657 . ? O9 Cd1 Cd2 45.89(15) 8 . ? O9 Cd1 Cd2 134.11(15) 2_656 . ? O6 Cd1 Cd2 71.45(16) 7_656 7_656 ? O6 Cd1 Cd2 108.55(16) . 7_656 ? O8 Cd1 Cd2 138.80(17) 1_554 7_656 ? O8 Cd1 Cd2 41.20(17) 7_657 7_656 ? O9 Cd1 Cd2 134.11(15) 8 7_656 ? O9 Cd1 Cd2 45.89(15) 2_656 7_656 ? Cd2 Cd1 Cd2 180.0 . 7_656 ? O5 Cd2 N1 92.0(3) . . ? O5 Cd2 O10 135.6(3) . 8 ? N1 Cd2 O10 108.1(3) . 8 ? O5 Cd2 O8 93.1(2) . 1_554 ? N1 Cd2 O8 131.4(3) . 1_554 ? O10 Cd2 O8 101.3(3) 8 1_554 ? O5 Cd2 O9 88.6(2) . 8 ? N1 Cd2 O9 151.2(3) . 8 ? O10 Cd2 O9 55.0(2) 8 8 ? O8 Cd2 O9 77.2(2) 1_554 8 ? O5 Cd2 O7 129.2(3) . 1_554 ? N1 Cd2 O7 86.9(3) . 1_554 ? O10 Cd2 O7 92.0(3) 8 1_554 ? O8 Cd2 O7 53.8(2) 1_554 1_554 ? O9 Cd2 O7 114.6(2) 8 1_554 ? O5 Cd2 C26 114.1(3) . 8 ? N1 Cd2 C26 132.6(3) . 8 ? O10 Cd2 C26 27.2(2) 8 8 ? O8 Cd2 C26 87.9(3) 1_554 8 ? O9 Cd2 C26 28.0(2) 8 8 ? O7 Cd2 C26 103.1(3) 1_554 8 ? O5 Cd2 C19 114.0(3) . 1_554 ? N1 Cd2 C19 110.6(3) . 1_554 ? O10 Cd2 C19 95.7(3) 8 1_554 ? O8 Cd2 C19 27.2(3) 1_554 1_554 ? O9 Cd2 C19 95.3(2) 8 1_554 ? O7 Cd2 C19 26.7(2) 1_554 1_554 ? C26 Cd2 C19 94.5(3) 8 1_554 ? O5 Cd2 Cd1 75.86(17) . . ? N1 Cd2 Cd1 163.5(2) . . ? O10 Cd2 Cd1 88.42(19) 8 . ? O8 Cd2 Cd1 40.51(15) 1_554 . ? O9 Cd2 Cd1 41.70(14) 8 . ? O7 Cd2 Cd1 92.14(17) 1_554 . ? C26 Cd2 Cd1 63.6(2) 8 . ? C19 Cd2 Cd1 65.9(2) 1_554 . ? C27 N1 C29 107.7(8) . . ? C27 N1 Cd2 123.3(6) . . ? C29 N1 Cd2 128.9(6) . . ? C27 N2 C28 106.1(8) . . ? C27 N2 C30 126.5(7) . . ? C28 N2 C30 127.4(8) . . ? C2 O1 C2 114.3(11) 2_656 . ? C6 O2 C3 120.0(7) . . ? C13 O3 C4 120.0(8) . . ? C20 O4 C5 118.0(8) . . ? C12 O5 Cd2 130.0(6) . . ? C12 O6 Cd1 134.8(5) . . ? C19 O7 Cd2 87.9(6) . 1_556 ? C19 O8 Cd1 150.4(6) . 1_556 ? C19 O8 Cd2 96.6(6) . 1_556 ? Cd1 O8 Cd2 98.3(2) 1_556 1_556 ? C26 O9 Cd1 133.7(6) . 2_656 ? C26 O9 Cd2 85.0(6) . 8_456 ? Cd1 O9 Cd2 92.4(2) 2_656 8_456 ? C26 O10 Cd2 96.3(6) . 8_456 ? C4 C1 C2 109.3(8) . . ? C4 C1 C3 108.9(7) . . ? C2 C1 C3 110.5(7) . . ? C4 C1 C5 110.9(6) . . ? C2 C1 C5 110.6(7) . . ? C3 C1 C5 106.5(7) . . ? O1 C2 C1 107.2(8) . . ? O1 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O1 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C1 106.2(7) . . ? O2 C3 H3A 110.5 . . ? C1 C3 H3A 110.5 . . ? O2 C3 H3B 110.5 . . ? C1 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? O3 C4 C1 109.9(8) . . ? O3 C4 H4A 109.7 . . ? C1 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C1 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? O4 C5 C1 105.7(7) . . ? O4 C5 H5A 110.6 . . ? C1 C5 H5A 110.6 . . ? O4 C5 H5B 110.6 . . ? C1 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C11 C6 C7 119.8(8) . . ? C11 C6 O2 115.4(8) . . ? C7 C6 O2 124.7(8) . . ? C6 C7 C8 119.3(8) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C9 C8 C7 119.6(8) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C10 C9 C8 119.6(8) . . ? C10 C9 C12 120.9(8) . . ? C8 C9 C12 119.4(8) . . ? C9 C10 C11 120.7(9) . . ? C9 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 . . ? C10 C11 C6 120.9(9) . . ? C10 C11 H11A 119.6 . . ? C6 C11 H11A 119.6 . . ? O6 C12 O5 126.1(7) . . ? O6 C12 C9 118.1(8) . . ? O5 C12 C9 115.8(8) . . ? O3 C13 C14 125.2(9) . . ? O3 C13 C18 116.0(9) . . ? C14 C13 C18 118.8(10) . . ? C13 C14 C15 122.1(10) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C16 C15 C14 118.8(10) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C17 C16 C15 118.3(9) . . ? C17 C16 C19 121.7(9) . . ? C15 C16 C19 120.0(9) . . ? C18 C17 C16 123.1(9) . . ? C18 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? C17 C18 C13 118.8(10) . . ? C17 C18 H18A 120.6 . . ? C13 C18 H18A 120.6 . . ? O7 C19 O8 121.2(9) . . ? O7 C19 C16 120.0(9) . . ? O8 C19 C16 118.7(9) . . ? O7 C19 Cd2 65.4(5) . 1_556 ? O8 C19 Cd2 56.2(5) . 1_556 ? C16 C19 Cd2 173.3(7) . 1_556 ? C21 C20 O4 116.7(9) . . ? C21 C20 C25 118.3(9) . . ? O4 C20 C25 125.0(9) . . ? C20 C21 C22 122.5(10) . . ? C20 C21 H21A 118.7 . . ? C22 C21 H21A 118.7 . . ? C23 C22 C21 120.4(9) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 118.1(9) . . ? C24 C23 C26 120.9(10) . . ? C22 C23 C26 121.0(9) . . ? C23 C24 C25 120.3(10) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C20 C25 C24 120.4(9) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? O10 C26 O9 123.2(9) . . ? O10 C26 C23 118.9(9) . . ? O9 C26 C23 117.8(9) . . ? O10 C26 Cd2 56.5(5) . 8_456 ? O9 C26 Cd2 67.1(5) . 8_456 ? C23 C26 Cd2 172.5(7) . 8_456 ? N1 C27 N2 110.8(8) . . ? N1 C27 H27A 124.6 . . ? N2 C27 H27A 124.6 . . ? C29 C28 N2 107.5(9) . . ? C29 C28 H28A 126.2 . . ? N2 C28 H28A 126.2 . . ? C28 C29 N1 107.9(9) . . ? C28 C29 H29A 126.0 . . ? N1 C29 H29A 126.0 . . ? C31 C30 C32 121.6(8) . . ? C31 C30 N2 119.5(8) . . ? C32 C30 N2 118.8(7) . . ? C30 C31 C32 120.7(8) . 7_666 ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 7_666 . ? C30 C32 C31 117.8(8) . 7_666 ? C30 C32 H32A 121.1 . . ? C31 C32 H32A 121.1 7_666 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.735 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.169