# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chun-Sen Liu' _publ_contact_author_email chunsenliu@yahoo.com.cn loop_ _publ_author_name 'Chun-Sen Liu' 'Jun-Jie Wang' 'Ze Chang' 'Li-Fen Yan' 'Xian-He Bu' data_1 _database_code_depnum_ccdc_archive 'CCDC 749744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35.50 Cd2 N2 O12.75' _chemical_formula_weight 1009.03 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.3784(4) _cell_length_b 21.2929(6) _cell_length_c 21.9656(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8128.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4236 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 20.12 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4044 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35156 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7159 _reflns_number_gt 5090 _reflns_threshold_expression i>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+27.9390P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7159 _refine_ls_number_parameters 572 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 2.366 _refine_ls_shift/su_mean 0.004 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 0.36145(3) 0.282602(17) 1.211159(17) 0.03741(15) Uani 1 1 d . . . Cd2 Cd 0.60211(3) 0.26706(3) 0.79937(2) 0.06052(19) Uani 1 1 d D . . C1 C 0.2222(4) 0.6688(3) 1.2185(2) 0.0396(13) Uani 1 1 d . . . C2 C 0.2513(3) 0.6021(2) 1.2146(2) 0.0364(12) Uani 1 1 d . . . C3 C 0.2411(3) 0.5692(2) 1.1592(2) 0.0377(13) Uani 1 1 d . . . C4 C 0.2100(4) 0.5979(3) 1.1064(3) 0.0499(15) Uani 1 1 d . . . H4A H 0.1967 0.6402 1.1076 0.060 Uiso 1 1 calc R . . C5 C 0.1994(4) 0.5652(3) 1.0543(3) 0.0589(18) Uani 1 1 d . . . H5A H 0.1781 0.5850 1.0205 0.071 Uiso 1 1 calc R . . C6 C 0.2202(4) 0.5017(3) 1.0510(3) 0.0583(18) Uani 1 1 d . . . H6A H 0.2126 0.4796 1.0150 0.070 Uiso 1 1 calc R . . C7 C 0.2510(4) 0.4725(3) 1.0991(3) 0.0485(15) Uani 1 1 d . . . H7A H 0.2646 0.4304 1.0958 0.058 Uiso 1 1 calc R . . C8 C 0.2633(3) 0.5042(2) 1.1554(3) 0.0394(13) Uani 1 1 d . . . C9 C 0.2965(3) 0.4749(2) 1.2068(2) 0.0358(12) Uani 1 1 d . . . C10 C 0.3221(4) 0.4067(2) 1.2033(2) 0.0410(14) Uani 1 1 d . . . C11 C 0.3059(3) 0.5074(2) 1.2618(3) 0.0387(13) Uani 1 1 d . . . C12 C 0.3373(4) 0.4782(3) 1.3151(3) 0.0488(15) Uani 1 1 d . . . H12A H 0.3522 0.4362 1.3135 0.059 Uiso 1 1 calc R . . C13 C 0.3456(4) 0.5107(3) 1.3674(3) 0.0593(18) Uani 1 1 d . . . H13A H 0.3657 0.4907 1.4016 0.071 Uiso 1 1 calc R . . C14 C 0.3242(4) 0.5747(3) 1.3709(3) 0.0586(17) Uani 1 1 d . . . H14A H 0.3306 0.5964 1.4073 0.070 Uiso 1 1 calc R . . C15 C 0.2946(3) 0.6045(3) 1.3222(3) 0.0436(14) Uani 1 1 d . . . H15A H 0.2812 0.6467 1.3254 0.052 Uiso 1 1 calc R . . C16 C 0.2833(3) 0.5723(2) 1.2656(2) 0.0367(12) Uani 1 1 d . . . C17 C 0.4217(5) 0.2636(3) 1.0933(3) 0.0593(19) Uani 1 1 d . . . C18 C 0.4347(4) 0.2554(3) 1.0247(3) 0.0464(14) Uani 1 1 d . . . C19 C 0.4610(4) 0.1976(3) 1.0008(3) 0.0445(14) Uani 1 1 d . . . C20 C 0.4874(4) 0.1480(3) 1.0382(3) 0.0577(18) Uani 1 1 d . . . H20A H 0.4880 0.1530 1.0803 0.069 Uiso 1 1 calc R . . C21 C 0.5116(4) 0.0937(3) 1.0137(3) 0.0613(18) Uani 1 1 d . . . H21A H 0.5290 0.0620 1.0394 0.074 Uiso 1 1 calc R . . C22 C 0.5116(4) 0.0832(3) 0.9503(3) 0.0624(18) Uani 1 1 d . . . H22A H 0.5295 0.0455 0.9344 0.075 Uiso 1 1 calc R . . C23 C 0.4848(4) 0.1294(3) 0.9126(3) 0.0517(16) Uani 1 1 d . . . H23A H 0.4834 0.1224 0.8708 0.062 Uiso 1 1 calc R . . C24 C 0.4589(3) 0.1878(3) 0.9362(2) 0.0405(13) Uani 1 1 d . . . C25 C 0.4327(3) 0.2364(3) 0.8980(2) 0.0383(13) Uani 1 1 d . . . C26 C 0.4214(4) 0.2248(3) 0.8303(2) 0.0412(14) Uani 1 1 d . . . C27 C 0.4111(3) 0.2949(3) 0.9217(2) 0.0388(13) Uani 1 1 d . . . C28 C 0.3885(3) 0.3448(3) 0.8843(3) 0.0473(15) Uani 1 1 d . . . H28A H 0.3875 0.3389 0.8424 0.057 Uiso 1 1 calc R . . C29 C 0.3680(4) 0.4017(3) 0.9075(3) 0.0553(16) Uani 1 1 d . . . H29A H 0.3527 0.4339 0.8815 0.066 Uiso 1 1 calc R . . C30 C 0.3701(4) 0.4119(3) 0.9713(3) 0.0603(18) Uani 1 1 d . . . H30A H 0.3569 0.4509 0.9871 0.072 Uiso 1 1 calc R . . C31 C 0.3911(4) 0.3651(3) 1.0088(3) 0.0523(16) Uani 1 1 d . . . H31A H 0.3917 0.3724 1.0506 0.063 Uiso 1 1 calc R . . C32 C 0.4126(3) 0.3045(3) 0.9864(2) 0.0424(14) Uani 1 1 d . . . C33 C 0.6684(6) 0.1948(5) 0.9215(5) 0.100(3) Uani 1 1 d . . . H33A H 0.6720 0.1614 0.8943 0.120 Uiso 1 1 calc R . . C34 C 0.6940(7) 0.1867(6) 0.9787(6) 0.119(4) Uani 1 1 d . . . H34A H 0.7180 0.1495 0.9900 0.143 Uiso 1 1 calc R . . C35 C 0.6841(10) 0.2346(7) 1.0204(7) 0.156(6) Uani 1 1 d . . . H35A H 0.6980 0.2295 1.0610 0.188 Uiso 1 1 calc R . . C36 C 0.6511(8) 0.2934(6) 0.9985(5) 0.141(5) Uani 1 1 d . . . H36A H 0.6452 0.3272 1.0250 0.169 Uiso 1 1 calc R . . C37 C 0.6287(5) 0.2990(4) 0.9384(3) 0.069(2) Uani 1 1 d . . . C38 C 0.5981(4) 0.3554(4) 0.9132(4) 0.071(2) Uani 1 1 d . . . C39 C 0.5847(5) 0.4096(4) 0.9510(5) 0.092(3) Uani 1 1 d . . . H39A H 0.5942 0.4088 0.9926 0.111 Uiso 1 1 calc R . . C40 C 0.5583(6) 0.4604(5) 0.9238(5) 0.098(3) Uani 1 1 d . . . H40A H 0.5488 0.4957 0.9474 0.118 Uiso 1 1 calc R . . C41 C 0.5438(6) 0.4640(4) 0.8608(6) 0.108(3) Uani 1 1 d . . . H41A H 0.5276 0.5012 0.8427 0.129 Uiso 1 1 calc R . . C42 C 0.5546(5) 0.4104(3) 0.8272(4) 0.080(2) Uani 1 1 d . . . H42A H 0.5427 0.4098 0.7859 0.095 Uiso 1 1 calc R . . C43 C 0.4645(12) 0.5636(14) 0.7383(11) 0.140(10) Uani 0.50 1 d P A 2 H43A H 0.4272 0.5838 0.7639 0.210 Uiso 0.50 1 calc PR A 2 H43B H 0.4711 0.5876 0.7017 0.210 Uiso 0.50 1 calc PR A 2 H43C H 0.5127 0.5608 0.7595 0.210 Uiso 0.50 1 calc PR A 2 C44 C 0.4380(16) 0.5014(12) 0.7230(12) 0.133(9) Uani 0.50 1 d P A 2 H44A H 0.3932 0.4914 0.7440 0.160 Uiso 0.50 1 calc PR A 2 N1 N 0.6375(4) 0.2494(3) 0.9016(3) 0.0771(18) Uani 1 1 d . . . N2 N 0.5835(3) 0.3568(3) 0.8556(3) 0.0711(17) Uani 1 1 d . . . O1W O 0.5829(5) 0.2887(5) 0.7014(3) 0.182(5) Uani 1 1 d D . . H1WA H 0.5481 0.2666 0.6882 0.273 Uiso 1 1 calc RD . . H1WB H 0.6273 0.2783 0.6883 0.273 Uiso 1 1 d RD . . O1 O 0.2711(2) 0.36503(17) 1.20563(19) 0.0513(11) Uani 1 1 d . . . O2W O 0.6248(4) 0.1649(3) 0.7802(4) 0.140(3) Uani 1 1 d D . . H2WA H 0.6708 0.1576 0.7845 0.209 Uiso 1 1 calc RD . . O2 O 0.3911(3) 0.39455(19) 1.2010(2) 0.0608(13) Uani 1 1 d . . . O3 O 0.1502(2) 0.67530(18) 1.22253(19) 0.0488(10) Uani 1 1 d . . . O3W O 0.2076(6) 0.3061(10) 0.3558(5) 0.317(10) Uani 1 1 d . . . O4 O 0.2672(2) 0.71406(17) 1.21785(19) 0.0491(10) Uani 1 1 d . . . O4W O 0.4453(10) 0.6194(6) 0.8355(10) 0.154(8) Uani 0.50 1 d P . . O5 O 0.3566(3) 0.2060(2) 0.81411(18) 0.0529(11) Uani 1 1 d . . . O5W O 0.359(4) 0.5836(19) 0.8843(16) 0.24(3) Uani 0.25 1 d P . . O6 O 0.4744(2) 0.2351(2) 0.79348(17) 0.0484(10) Uani 1 1 d . . . O6W O 0.4766(8) 0.3968(7) 0.7002(6) 0.102(5) Uani 0.50 1 d P B 1 O7 O 0.4751(4) 0.2690(3) 1.1286(2) 0.0944(19) Uani 1 1 d . . . O8 O 0.3523(4) 0.2645(3) 1.1100(2) 0.0869(18) Uani 1 1 d . . . O9 O 0.4611(9) 0.4518(10) 0.6854(8) 0.139(6) Uani 0.50 1 d P A 2 H9A H 0.4290 0.4237 0.6868 0.208 Uiso 0.50 1 calc PR A 2 H2WB H 0.6115(15) 0.1706(8) 0.7434(8) 2.0(16) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0559(3) 0.0266(2) 0.0297(2) -0.00042(16) 0.00171(19) 0.00082(18) Cd2 0.0595(3) 0.0635(3) 0.0585(3) -0.0127(2) 0.0048(3) -0.0047(2) C1 0.055(4) 0.034(3) 0.029(3) 0.000(2) 0.002(3) 0.007(3) C2 0.043(3) 0.029(3) 0.038(3) -0.001(2) 0.006(3) 0.005(2) C3 0.041(3) 0.034(3) 0.038(3) 0.002(2) 0.003(3) 0.005(2) C4 0.058(4) 0.046(3) 0.045(4) 0.001(3) -0.001(3) 0.014(3) C5 0.080(5) 0.066(4) 0.031(3) 0.000(3) -0.009(3) 0.022(4) C6 0.071(5) 0.060(4) 0.043(4) -0.017(3) -0.010(3) 0.007(4) C7 0.062(4) 0.036(3) 0.047(4) -0.010(3) -0.002(3) 0.006(3) C8 0.044(4) 0.033(3) 0.041(3) -0.005(2) 0.002(3) 0.001(2) C9 0.039(3) 0.025(3) 0.043(3) 0.002(2) 0.005(3) -0.002(2) C10 0.055(4) 0.029(3) 0.039(3) 0.000(2) 0.003(3) 0.000(3) C11 0.043(3) 0.032(3) 0.041(3) -0.001(2) 0.004(3) 0.002(2) C12 0.059(4) 0.038(3) 0.050(4) 0.006(3) -0.007(3) 0.012(3) C13 0.079(5) 0.057(4) 0.041(4) 0.005(3) -0.016(3) 0.015(4) C14 0.070(5) 0.063(4) 0.043(4) -0.010(3) -0.009(3) 0.007(4) C15 0.053(4) 0.039(3) 0.039(3) -0.007(3) -0.001(3) 0.006(3) C16 0.041(3) 0.029(3) 0.040(3) -0.001(2) 0.003(3) 0.000(2) C17 0.101(6) 0.040(4) 0.037(4) -0.001(3) -0.008(4) -0.005(4) C18 0.058(4) 0.051(4) 0.030(3) 0.000(3) 0.000(3) -0.011(3) C19 0.051(4) 0.048(3) 0.034(3) 0.007(3) -0.006(3) -0.009(3) C20 0.079(5) 0.056(4) 0.038(3) 0.010(3) -0.012(3) -0.010(4) C21 0.069(5) 0.049(4) 0.065(5) 0.017(3) -0.017(4) -0.003(3) C22 0.073(5) 0.046(4) 0.068(5) -0.001(3) -0.004(4) 0.010(3) C23 0.066(4) 0.045(3) 0.044(3) 0.003(3) -0.001(3) 0.001(3) C24 0.047(3) 0.043(3) 0.032(3) -0.001(2) 0.001(3) -0.006(3) C25 0.041(3) 0.043(3) 0.031(3) 0.003(2) -0.001(2) -0.003(3) C26 0.057(4) 0.037(3) 0.030(3) 0.006(2) 0.003(3) 0.007(3) C27 0.043(3) 0.040(3) 0.033(3) -0.002(2) 0.004(3) -0.001(3) C28 0.053(4) 0.049(4) 0.039(3) -0.001(3) 0.000(3) 0.001(3) C29 0.061(4) 0.047(4) 0.058(4) 0.003(3) -0.003(3) 0.004(3) C30 0.069(5) 0.049(4) 0.063(4) -0.007(3) 0.014(4) 0.001(3) C31 0.066(4) 0.057(4) 0.034(3) -0.013(3) 0.007(3) -0.004(3) C32 0.049(4) 0.045(3) 0.034(3) -0.003(3) 0.003(3) -0.002(3) C33 0.114(8) 0.084(6) 0.102(8) 0.023(6) 0.029(6) 0.029(6) C34 0.130(10) 0.106(9) 0.122(10) 0.043(8) 0.004(8) 0.035(7) C35 0.223(17) 0.140(12) 0.106(10) 0.040(9) -0.044(11) 0.022(11) C36 0.209(14) 0.140(11) 0.073(7) 0.008(7) -0.023(8) -0.003(10) C37 0.074(5) 0.080(5) 0.053(4) 0.003(4) -0.005(4) -0.011(4) C38 0.065(5) 0.079(5) 0.069(5) -0.004(4) 0.006(4) -0.013(4) C39 0.084(6) 0.070(6) 0.123(8) -0.020(6) 0.009(6) -0.008(5) C40 0.091(7) 0.102(8) 0.102(8) -0.013(6) 0.009(6) -0.002(6) C41 0.101(7) 0.060(5) 0.163(11) 0.016(6) 0.032(7) -0.002(5) C42 0.082(6) 0.049(4) 0.107(7) 0.009(4) 0.027(5) 0.001(4) C43 0.068(13) 0.23(3) 0.125(18) 0.04(2) -0.034(13) -0.018(16) C44 0.15(2) 0.109(18) 0.14(2) -0.023(16) 0.004(17) -0.062(17) N1 0.078(5) 0.076(4) 0.078(5) 0.009(4) 0.004(4) 0.013(4) N2 0.057(4) 0.077(4) 0.079(4) -0.005(4) -0.001(3) -0.005(3) O1W 0.148(7) 0.336(14) 0.063(4) 0.064(6) -0.035(4) -0.156(8) O1 0.051(3) 0.029(2) 0.074(3) 0.0020(19) -0.006(2) -0.0054(19) O2W 0.068(4) 0.081(5) 0.270(10) -0.018(5) -0.020(5) 0.011(3) O2 0.048(3) 0.033(2) 0.102(4) 0.001(2) 0.018(3) 0.0073(19) O3 0.049(3) 0.035(2) 0.063(3) -0.0039(19) 0.010(2) 0.0109(18) O3W 0.125(8) 0.69(3) 0.140(9) -0.058(14) 0.042(7) -0.028(13) O4 0.055(3) 0.028(2) 0.064(3) 0.0003(18) 0.002(2) 0.0008(19) O4W 0.134(13) 0.065(8) 0.26(2) -0.022(11) -0.102(14) 0.013(8) O5 0.057(3) 0.066(3) 0.036(2) 0.000(2) -0.006(2) -0.016(2) O5W 0.45(8) 0.15(3) 0.11(3) -0.08(2) -0.02(4) 0.13(4) O6 0.050(3) 0.062(3) 0.034(2) -0.0022(19) 0.0050(19) 0.002(2) O6W 0.122(11) 0.083(9) 0.101(9) -0.027(7) 0.038(8) -0.052(8) O7 0.134(5) 0.088(4) 0.061(3) -0.004(3) -0.040(4) 0.010(4) O8 0.126(5) 0.091(4) 0.043(3) -0.014(3) 0.033(3) -0.024(4) O9 0.089(10) 0.140(15) 0.188(17) -0.034(14) 0.005(10) -0.054(11) _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 O8 2.262(5) . ? Cd1 O5 2.276(4) 7_566 ? Cd1 O3 2.307(4) 8_655 ? Cd1 O1 2.358(4) . ? Cd1 O2 2.449(4) . ? Cd1 C10 2.735(5) . ? Cd2 O1W 2.227(6) . ? Cd2 O2W 2.250(7) . ? Cd2 N2 2.298(7) . ? Cd2 O6 2.326(4) . ? Cd2 O4 2.338(4) 5_667 ? Cd2 N1 2.359(7) . ? C1 O4 1.241(7) . ? C1 O3 1.262(7) . ? C1 C2 1.509(7) . ? C2 C16 1.402(7) . ? C2 C3 1.416(7) . ? C3 C4 1.418(8) . ? C3 C8 1.440(7) . ? C4 C5 1.352(8) . ? C4 H4A 0.9300 . ? C5 C6 1.403(9) . ? C5 H5A 0.9300 . ? C6 C7 1.338(8) . ? C6 H6A 0.9300 . ? C7 C8 1.424(8) . ? C7 H7A 0.9300 . ? C8 C9 1.413(8) . ? C9 C11 1.401(7) . ? C9 C10 1.521(7) . ? C10 O2 1.229(7) . ? C10 O1 1.255(7) . ? C11 C12 1.433(8) . ? C11 C16 1.441(7) . ? C12 C13 1.350(9) . ? C12 H12A 0.9300 . ? C13 C14 1.416(9) . ? C13 H13A 0.9300 . ? C14 C15 1.346(8) . ? C14 H14A 0.9300 . ? C15 C16 1.434(7) . ? C15 H15A 0.9300 . ? C17 O7 1.215(9) . ? C17 O8 1.260(9) . ? C17 C18 1.533(9) . ? C18 C32 1.396(8) . ? C18 C19 1.413(9) . ? C19 C20 1.415(8) . ? C19 C24 1.436(7) . ? C20 C21 1.343(9) . ? C20 H20A 0.9300 . ? C21 C22 1.412(9) . ? C21 H21A 0.9300 . ? C22 C23 1.366(9) . ? C22 H22A 0.9300 . ? C23 C24 1.420(8) . ? C23 H23A 0.9300 . ? C24 C25 1.408(8) . ? C25 C27 1.401(8) . ? C25 C26 1.521(8) . ? C26 O6 1.245(7) . ? C26 O5 1.246(7) . ? C27 C28 1.400(8) . ? C27 C32 1.436(7) . ? C28 C29 1.361(8) . ? C28 H28A 0.9300 . ? C29 C30 1.418(9) . ? C29 H29A 0.9300 . ? C30 C31 1.344(9) . ? C30 H30A 0.9300 . ? C31 C32 1.430(8) . ? C31 H31A 0.9300 . ? C33 C34 1.345(14) . ? C33 N1 1.352(11) . ? C33 H33A 0.9300 . ? C34 C35 1.382(16) . ? C34 H34A 0.9300 . ? C35 C36 1.459(16) . ? C35 H35A 0.9300 . ? C36 C37 1.382(12) . ? C36 H36A 0.9300 . ? C37 N1 1.337(10) . ? C37 C38 1.426(11) . ? C38 N2 1.290(9) . ? C38 C39 1.441(11) . ? C39 C40 1.317(13) . ? C39 H39A 0.9300 . ? C40 C41 1.408(13) . ? C40 H40A 0.9300 . ? C41 C42 1.372(12) . ? C41 H41A 0.9300 . ? C42 N2 1.394(10) . ? C42 H42A 0.9300 . ? C43 C44 1.44(3) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 O9 1.40(3) . ? C44 H44A 0.9300 . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8537 . ? O2W H2WA 0.8200 . ? O2W H2WB 0.851(10) . ? O3 Cd1 2.307(4) 8_665 ? O4 Cd2 2.338(4) 5_667 ? O5 Cd1 2.276(4) 7_565 ? O9 H9A 0.8200 . ? 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 O8 Cd1 O5 172.8(2) . 7_566 ? O8 Cd1 O3 86.07(18) . 8_655 ? O5 Cd1 O3 89.72(16) 7_566 8_655 ? O8 Cd1 O1 91.7(2) . . ? O5 Cd1 O1 86.96(15) 7_566 . ? O3 Cd1 O1 133.16(14) 8_655 . ? O8 Cd1 O2 95.24(19) . . ? O5 Cd1 O2 89.65(17) 7_566 . ? O3 Cd1 O2 172.83(15) 8_655 . ? O1 Cd1 O2 53.92(14) . . ? O8 Cd1 C10 94.9(2) . . ? O5 Cd1 C10 87.15(16) 7_566 . ? O3 Cd1 C10 160.31(18) 8_655 . ? O1 Cd1 C10 27.26(16) . . ? O2 Cd1 C10 26.69(16) . . ? O1W Cd2 O2W 92.6(4) . . ? O1W Cd2 N2 109.0(4) . . ? O2W Cd2 N2 158.2(3) . . ? O1W Cd2 O6 82.2(2) . . ? O2W Cd2 O6 82.8(2) . . ? N2 Cd2 O6 98.00(18) . . ? O1W Cd2 O4 87.3(2) . 5_667 ? O2W Cd2 O4 88.03(19) . 5_667 ? N2 Cd2 O4 94.62(17) . 5_667 ? O6 Cd2 O4 165.67(14) . 5_667 ? O1W Cd2 N1 173.0(2) . . ? O2W Cd2 N1 88.7(3) . . ? N2 Cd2 N1 70.0(2) . . ? O6 Cd2 N1 104.77(19) . . ? O4 Cd2 N1 85.89(19) 5_667 . ? O4 C1 O3 122.7(5) . . ? O4 C1 C2 121.2(5) . . ? O3 C1 C2 116.0(5) . . ? C16 C2 C3 120.8(5) . . ? C16 C2 C1 120.9(5) . . ? C3 C2 C1 118.2(5) . . ? C2 C3 C4 122.6(5) . . ? C2 C3 C8 119.5(5) . . ? C4 C3 C8 118.0(5) . . ? C5 C4 C3 121.5(6) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 120.7(6) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C6 C7 C8 121.7(6) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 123.1(5) . . ? C9 C8 C3 119.2(5) . . ? C7 C8 C3 117.8(5) . . ? C11 C9 C8 121.3(5) . . ? C11 C9 C10 118.7(5) . . ? C8 C9 C10 120.0(5) . . ? O2 C10 O1 122.9(5) . . ? O2 C10 C9 119.2(5) . . ? O1 C10 C9 117.9(5) . . ? O2 C10 Cd1 63.6(3) . . ? O1 C10 Cd1 59.4(3) . . ? C9 C10 Cd1 173.0(4) . . ? C9 C11 C12 122.3(5) . . ? C9 C11 C16 119.5(5) . . ? C12 C11 C16 118.2(5) . . ? C13 C12 C11 120.9(5) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 120.8(6) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 120.8(6) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 121.1(5) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C2 C16 C15 122.1(5) . . ? C2 C16 C11 119.7(5) . . ? C15 C16 C11 118.2(5) . . ? O7 C17 O8 122.9(7) . . ? O7 C17 C18 121.7(8) . . ? O8 C17 C18 115.3(6) . . ? C32 C18 C19 121.2(5) . . ? C32 C18 C17 117.8(6) . . ? C19 C18 C17 120.7(5) . . ? C18 C19 C20 122.7(5) . . ? C18 C19 C24 119.1(5) . . ? C20 C19 C24 118.2(6) . . ? C21 C20 C19 120.9(6) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 122.1(6) . . ? C20 C21 H21A 119.0 . . ? C22 C21 H21A 119.0 . . ? C23 C22 C21 119.0(6) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 121.1(6) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C25 C24 C23 122.0(5) . . ? C25 C24 C19 119.3(5) . . ? C23 C24 C19 118.7(5) . . ? C27 C25 C24 121.3(5) . . ? C27 C25 C26 118.3(5) . . ? C24 C25 C26 120.3(5) . . ? O6 C26 O5 122.6(5) . . ? O6 C26 C25 120.8(6) . . ? O5 C26 C25 116.6(5) . . ? C28 C27 C25 122.1(5) . . ? C28 C27 C32 118.5(5) . . ? C25 C27 C32 119.4(5) . . ? C29 C28 C27 122.0(6) . . ? C29 C28 H28A 119.0 . . ? C27 C28 H28A 119.0 . . ? C28 C29 C30 119.9(6) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0(6) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 121.9(6) . . ? C30 C31 H31A 119.1 . . ? C32 C31 H31A 119.1 . . ? C18 C32 C31 122.7(5) . . ? C18 C32 C27 119.6(5) . . ? C31 C32 C27 117.7(5) . . ? C34 C33 N1 122.9(10) . . ? C34 C33 H33A 118.6 . . ? N1 C33 H33A 118.6 . . ? C33 C34 C35 119.0(10) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C34 C35 C36 117.6(11) . . ? C34 C35 H35A 121.2 . . ? C36 C35 H35A 121.2 . . ? C37 C36 C35 120.0(12) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? N1 C37 C36 118.5(9) . . ? N1 C37 C38 118.3(7) . . ? C36 C37 C38 123.2(9) . . ? N2 C38 C37 118.2(8) . . ? N2 C38 C39 121.0(9) . . ? C37 C38 C39 120.8(8) . . ? C40 C39 C38 116.9(10) . . ? C40 C39 H39A 121.6 . . ? C38 C39 H39A 121.6 . . ? C39 C40 C41 123.6(10) . . ? C39 C40 H40A 118.2 . . ? C41 C40 H40A 118.2 . . ? C42 C41 C40 117.3(9) . . ? C42 C41 H41A 121.4 . . ? C40 C41 H41A 121.4 . . ? C41 C42 N2 119.3(9) . . ? C41 C42 H42A 120.3 . . ? N2 C42 H42A 120.3 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O9 C44 C43 138(2) . . ? O9 C44 H44A 111.2 . . ? C43 C44 H44A 111.2 . . ? C37 N1 C33 122.0(8) . . ? C37 N1 Cd2 114.8(5) . . ? C33 N1 Cd2 123.2(7) . . ? C38 N2 C42 121.9(7) . . ? C38 N2 Cd2 118.7(6) . . ? C42 N2 Cd2 119.4(6) . . ? Cd2 O1W H1WA 109.5 . . ? Cd2 O1W H1WB 97.8 . . ? H1WA O1W H1WB 113.5 . . ? C10 O1 Cd1 93.3(3) . . ? Cd2 O2W H2WA 109.5 . . ? Cd2 O2W H2WB 89.6(9) . . ? H2WA O2W H2WB 113.7 . . ? C10 O2 Cd1 89.7(3) . . ? C1 O3 Cd1 100.8(3) . 8_665 ? C1 O4 Cd2 138.4(4) . 5_667 ? C26 O5 Cd1 102.5(4) . 7_565 ? C26 O6 Cd2 136.2(4) . . ? C17 O8 Cd1 102.8(5) . . ? C44 O9 H9A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 C1 C2 C16 77.8(7) . . . . ? O3 C1 C2 C16 -102.1(6) . . . . ? O4 C1 C2 C3 -106.0(6) . . . . ? O3 C1 C2 C3 74.1(7) . . . . ? C16 C2 C3 C4 -179.1(6) . . . . ? C1 C2 C3 C4 4.7(8) . . . . ? C16 C2 C3 C8 0.6(8) . . . . ? C1 C2 C3 C8 -175.6(5) . . . . ? C2 C3 C4 C5 -178.6(6) . . . . ? C8 C3 C4 C5 1.7(9) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? C4 C5 C6 C7 -0.1(11) . . . . ? C5 C6 C7 C8 0.4(11) . . . . ? C6 C7 C8 C9 -179.2(6) . . . . ? C6 C7 C8 C3 0.3(9) . . . . ? C2 C3 C8 C9 -1.5(8) . . . . ? C4 C3 C8 C9 178.1(5) . . . . ? C2 C3 C8 C7 179.0(5) . . . . ? C4 C3 C8 C7 -1.3(8) . . . . ? C7 C8 C9 C11 -178.4(6) . . . . ? C3 C8 C9 C11 2.2(8) . . . . ? C7 C8 C9 C10 0.9(9) . . . . ? C3 C8 C9 C10 -178.6(5) . . . . ? C11 C9 C10 O2 -74.1(7) . . . . ? C8 C9 C10 O2 106.6(7) . . . . ? C11 C9 C10 O1 102.7(6) . . . . ? C8 C9 C10 O1 -76.6(7) . . . . ? C11 C9 C10 Cd1 38(4) . . . . ? C8 C9 C10 Cd1 -142(3) . . . . ? O8 Cd1 C10 O2 -92.0(4) . . . . ? O5 Cd1 C10 O2 94.9(4) 7_566 . . . ? O3 Cd1 C10 O2 176.1(4) 8_655 . . . ? O1 Cd1 C10 O2 -176.2(6) . . . . ? O8 Cd1 C10 O1 84.2(4) . . . . ? O5 Cd1 C10 O1 -88.9(3) 7_566 . . . ? O3 Cd1 C10 O1 -7.7(7) 8_655 . . . ? O2 Cd1 C10 O1 176.2(6) . . . . ? O8 Cd1 C10 C9 153(4) . . . . ? O5 Cd1 C10 C9 -20(4) 7_566 . . . ? O3 Cd1 C10 C9 61(4) 8_655 . . . ? O1 Cd1 C10 C9 69(4) . . . . ? O2 Cd1 C10 C9 -115(4) . . . . ? C8 C9 C11 C12 178.1(5) . . . . ? C10 C9 C11 C12 -1.2(9) . . . . ? C8 C9 C11 C16 -1.8(8) . . . . ? C10 C9 C11 C16 178.9(5) . . . . ? C9 C11 C12 C13 180.0(6) . . . . ? C16 C11 C12 C13 -0.1(9) . . . . ? C11 C12 C13 C14 -0.6(11) . . . . ? C12 C13 C14 C15 0.4(11) . . . . ? C13 C14 C15 C16 0.5(10) . . . . ? C3 C2 C16 C15 179.7(5) . . . . ? C1 C2 C16 C15 -4.2(9) . . . . ? C3 C2 C16 C11 -0.2(8) . . . . ? C1 C2 C16 C11 175.9(5) . . . . ? C14 C15 C16 C2 178.9(6) . . . . ? C14 C15 C16 C11 -1.1(9) . . . . ? C9 C11 C16 C2 0.9(8) . . . . ? C12 C11 C16 C2 -179.1(5) . . . . ? C9 C11 C16 C15 -179.1(5) . . . . ? C12 C11 C16 C15 0.9(8) . . . . ? O7 C17 C18 C32 -111.7(8) . . . . ? O8 C17 C18 C32 67.9(8) . . . . ? O7 C17 C18 C19 74.6(9) . . . . ? O8 C17 C18 C19 -105.8(7) . . . . ? C32 C18 C19 C20 176.8(6) . . . . ? C17 C18 C19 C20 -9.6(10) . . . . ? C32 C18 C19 C24 -4.9(9) . . . . ? C17 C18 C19 C24 168.6(6) . . . . ? C18 C19 C20 C21 179.8(6) . . . . ? C24 C19 C20 C21 1.6(10) . . . . ? C19 C20 C21 C22 -0.4(11) . . . . ? C20 C21 C22 C23 -1.1(11) . . . . ? C21 C22 C23 C24 1.5(10) . . . . ? C22 C23 C24 C25 178.6(6) . . . . ? C22 C23 C24 C19 -0.4(9) . . . . ? C18 C19 C24 C25 1.6(9) . . . . ? C20 C19 C24 C25 179.8(6) . . . . ? C18 C19 C24 C23 -179.4(6) . . . . ? C20 C19 C24 C23 -1.2(9) . . . . ? C23 C24 C25 C27 -176.7(6) . . . . ? C19 C24 C25 C27 2.3(9) . . . . ? C23 C24 C25 C26 8.0(9) . . . . ? C19 C24 C25 C26 -173.1(5) . . . . ? C27 C25 C26 O6 93.1(7) . . . . ? C24 C25 C26 O6 -91.4(7) . . . . ? C27 C25 C26 O5 -85.5(7) . . . . ? C24 C25 C26 O5 90.0(7) . . . . ? C24 C25 C27 C28 176.8(6) . . . . ? C26 C25 C27 C28 -7.8(8) . . . . ? C24 C25 C27 C32 -2.7(8) . . . . ? C26 C25 C27 C32 172.7(5) . . . . ? C25 C27 C28 C29 -179.6(6) . . . . ? C32 C27 C28 C29 -0.1(9) . . . . ? C27 C28 C29 C30 0.7(10) . . . . ? C28 C29 C30 C31 -1.0(10) . . . . ? C29 C30 C31 C32 0.6(10) . . . . ? C19 C18 C32 C31 -175.3(6) . . . . ? C17 C18 C32 C31 11.0(9) . . . . ? C19 C18 C32 C27 4.5(9) . . . . ? C17 C18 C32 C27 -169.2(6) . . . . ? C30 C31 C32 C18 179.9(6) . . . . ? C30 C31 C32 C27 0.1(10) . . . . ? C28 C27 C32 C18 179.9(6) . . . . ? C25 C27 C32 C18 -0.6(8) . . . . ? C28 C27 C32 C31 -0.3(8) . . . . ? C25 C27 C32 C31 179.2(5) . . . . ? N1 C33 C34 C35 4.3(19) . . . . ? C33 C34 C35 C36 -4(2) . . . . ? C34 C35 C36 C37 2(2) . . . . ? C35 C36 C37 N1 0.5(18) . . . . ? C35 C36 C37 C38 -178.1(11) . . . . ? N1 C37 C38 N2 -3.0(11) . . . . ? C36 C37 C38 N2 175.6(9) . . . . ? N1 C37 C38 C39 177.7(7) . . . . ? C36 C37 C38 C39 -3.6(14) . . . . ? N2 C38 C39 C40 -1.1(13) . . . . ? C37 C38 C39 C40 178.1(8) . . . . ? C38 C39 C40 C41 -0.6(15) . . . . ? C39 C40 C41 C42 3.1(15) . . . . ? C40 C41 C42 N2 -4.0(13) . . . . ? C36 C37 N1 C33 -0.9(13) . . . . ? C38 C37 N1 C33 177.9(8) . . . . ? C36 C37 N1 Cd2 -177.3(8) . . . . ? C38 C37 N1 Cd2 1.4(9) . . . . ? C34 C33 N1 C37 -1.6(15) . . . . ? C34 C33 N1 Cd2 174.6(8) . . . . ? O1W Cd2 N1 C37 83(3) . . . . ? O2W Cd2 N1 C37 -175.4(6) . . . . ? N2 Cd2 N1 C37 0.1(5) . . . . ? O6 Cd2 N1 C37 -93.2(6) . . . . ? O4 Cd2 N1 C37 96.5(6) 5_667 . . . ? O1W Cd2 N1 C33 -93(3) . . . . ? O2W Cd2 N1 C33 8.2(7) . . . . ? N2 Cd2 N1 C33 -176.3(8) . . . . ? O6 Cd2 N1 C33 90.4(7) . . . . ? O4 Cd2 N1 C33 -79.9(7) 5_667 . . . ? C37 C38 N2 C42 -179.1(7) . . . . ? C39 C38 N2 C42 0.2(12) . . . . ? C37 C38 N2 Cd2 3.1(9) . . . . ? C39 C38 N2 Cd2 -177.6(6) . . . . ? C41 C42 N2 C38 2.4(12) . . . . ? C41 C42 N2 Cd2 -179.7(6) . . . . ? O1W Cd2 N2 C38 -174.4(6) . . . . ? O2W Cd2 N2 C38 10.7(10) . . . . ? O6 Cd2 N2 C38 101.2(6) . . . . ? O4 Cd2 N2 C38 -85.6(6) 5_667 . . . ? N1 Cd2 N2 C38 -1.7(5) . . . . ? O1W Cd2 N2 C42 7.7(6) . . . . ? O2W Cd2 N2 C42 -167.2(6) . . . . ? O6 Cd2 N2 C42 -76.7(5) . . . . ? O4 Cd2 N2 C42 96.5(5) 5_667 . . . ? N1 Cd2 N2 C42 -179.6(6) . . . . ? O2 C10 O1 Cd1 4.1(6) . . . . ? C9 C10 O1 Cd1 -172.7(4) . . . . ? O8 Cd1 O1 C10 -97.4(4) . . . . ? O5 Cd1 O1 C10 89.7(3) 7_566 . . . ? O3 Cd1 O1 C10 176.4(3) 8_655 . . . ? O2 Cd1 O1 C10 -2.1(3) . . . . ? O1 C10 O2 Cd1 -3.9(6) . . . . ? C9 C10 O2 Cd1 172.8(4) . . . . ? O8 Cd1 O2 C10 90.4(4) . . . . ? O5 Cd1 O2 C10 -84.3(4) 7_566 . . . ? O3 Cd1 O2 C10 -169.3(11) 8_655 . . . ? O1 Cd1 O2 C10 2.2(3) . . . . ? O4 C1 O3 Cd1 8.9(6) . . . 8_665 ? C2 C1 O3 Cd1 -171.2(4) . . . 8_665 ? O3 C1 O4 Cd2 -171.0(4) . . . 5_667 ? C2 C1 O4 Cd2 9.1(9) . . . 5_667 ? O6 C26 O5 Cd1 -10.8(6) . . . 7_565 ? C25 C26 O5 Cd1 167.8(4) . . . 7_565 ? O5 C26 O6 Cd2 -178.2(4) . . . . ? C25 C26 O6 Cd2 3.2(8) . . . . ? O1W Cd2 O6 C26 -161.8(6) . . . . ? O2W Cd2 O6 C26 104.5(6) . . . . ? N2 Cd2 O6 C26 -53.5(6) . . . . ? O4 Cd2 O6 C26 154.9(6) 5_667 . . . ? N1 Cd2 O6 C26 17.8(6) . . . . ? O7 C17 O8 Cd1 2.7(8) . . . . ? C18 C17 O8 Cd1 -176.9(4) . . . . ? O5 Cd1 O8 C17 -150.9(14) 7_566 . . . ? O3 Cd1 O8 C17 -96.8(5) 8_655 . . . ? O1 Cd1 O8 C17 130.1(4) . . . . ? O2 Cd1 O8 C17 76.2(5) . . . . ? C10 Cd1 O8 C17 103.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.125 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.100 data_2 _database_code_depnum_ccdc_archive 'CCDC 749745' #TrackingRef 'revised CCDC data for 749745 and 749747.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H58 Cd2 N8 O12' _chemical_formula_weight 1740.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7828(9) _cell_length_b 12.1306(12) _cell_length_c 17.092(2) _cell_angle_alpha 105.588(2) _cell_angle_beta 99.624(2) _cell_angle_gamma 100.178(2) _cell_volume 1873.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2129 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.11 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method none _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8930 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12678 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.83 _reflns_number_total 8598 _reflns_number_gt 5209 _reflns_threshold_expression i>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^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 8598 _refine_ls_number_parameters 533 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.40925(3) 1.15300(2) 1.258549(14) 0.04531(10) Uani 1 1 d . . . N1 N 0.4303(3) 1.1556(2) 1.12235(15) 0.0472(7) Uani 1 1 d . . . N2 N 0.2183(3) 1.0062(2) 1.15348(16) 0.0505(7) Uani 1 1 d . . . N3 N 0.2466(3) 1.2784(2) 1.26329(16) 0.0495(7) Uani 1 1 d . . . N4 N 0.3346(3) 1.1791(2) 1.38283(14) 0.0412(6) Uani 1 1 d . . . O1 O 0.6874(3) 1.5152(2) 1.33393(14) 0.0574(6) Uani 1 1 d . . . O2 O 0.5840(2) 1.3275(2) 1.30572(13) 0.0527(6) Uani 1 1 d . . . O3 O 0.7727(2) 0.4728(2) 1.20172(14) 0.0519(6) Uani 1 1 d D . . H3 H 0.7395 0.4926 1.2429 0.078 Uiso 1 1 calc RD . . O4 O 0.8562(3) 0.5582(2) 1.11629(16) 0.0760(8) Uani 1 1 d . . . O5 O 0.5520(3) 1.0292(2) 1.24995(15) 0.0665(7) Uani 1 1 d . . . O6 O 0.4122(4) 0.9324(3) 1.3110(2) 0.1042(11) Uani 1 1 d . . . C1 C 0.7882(3) 0.5573(3) 1.16875(19) 0.0438(8) Uani 1 1 d . . . C2 C 0.7164(4) 0.6564(3) 1.19913(18) 0.0421(8) Uani 1 1 d . . . C3 C 0.7974(4) 0.7617(3) 1.25716(19) 0.0465(8) Uani 1 1 d . . . C4 C 0.9457(4) 0.7771(4) 1.2929(2) 0.0585(10) Uani 1 1 d . . . H4A H 0.9905 0.7159 1.2769 0.070 Uiso 1 1 calc R . . C5 C 1.0208(5) 0.8805(4) 1.3501(3) 0.0791(13) Uani 1 1 d . . . H5A H 1.1162 0.8891 1.3742 0.095 Uiso 1 1 calc R . . C6 C 0.9551(6) 0.9746(4) 1.3729(3) 0.0795(13) Uani 1 1 d . . . H6A H 1.0084 1.0455 1.4113 0.095 Uiso 1 1 calc R . . C7 C 0.8164(5) 0.9644(3) 1.3404(2) 0.0705(12) Uani 1 1 d . . . H7A H 0.7763 1.0286 1.3565 0.085 Uiso 1 1 calc R . . C8 C 0.7304(4) 0.8584(3) 1.28243(19) 0.0513(9) Uani 1 1 d . . . C9 C 0.5835(4) 0.8420(3) 1.25076(19) 0.0497(9) Uani 1 1 d . . . C10 C 0.5017(4) 0.7344(3) 1.19654(19) 0.0470(8) Uani 1 1 d . . . C11 C 0.3507(4) 0.7125(4) 1.1621(2) 0.0609(10) Uani 1 1 d . . . H11A H 0.3029 0.7714 1.1791 0.073 Uiso 1 1 calc R . . C12 C 0.2778(4) 0.6099(4) 1.1062(3) 0.0695(11) Uani 1 1 d . . . H12A H 0.1806 0.5992 1.0855 0.083 Uiso 1 1 calc R . . C13 C 0.3439(4) 0.5182(4) 1.0783(2) 0.0651(10) Uani 1 1 d . . . H13A H 0.2916 0.4477 1.0390 0.078 Uiso 1 1 calc R . . C14 C 0.4858(4) 0.5332(3) 1.1092(2) 0.0534(9) Uani 1 1 d . . . H14A H 0.5292 0.4717 1.0908 0.064 Uiso 1 1 calc R . . C15 C 0.5702(4) 0.6402(3) 1.16875(19) 0.0431(8) Uani 1 1 d . . . C16 C 0.5141(5) 0.9438(3) 1.2749(2) 0.0649(11) Uani 1 1 d . . . C17 C 0.1154(4) 0.9327(4) 1.1675(2) 0.0650(11) Uani 1 1 d . . . H17A H 0.1089 0.9420 1.2225 0.078 Uiso 1 1 calc R . . C18 C 0.0164(4) 0.8423(4) 1.1051(3) 0.0811(13) Uani 1 1 d . . . H18A H -0.0527 0.7914 1.1182 0.097 Uiso 1 1 calc R . . C19 C 0.0223(4) 0.8296(4) 1.0248(3) 0.0831(13) Uani 1 1 d . . . H19A H -0.0430 0.7697 0.9820 0.100 Uiso 1 1 calc R . . C20 C 0.1271(4) 0.9070(4) 1.0060(2) 0.0630(10) Uani 1 1 d . . . C21 C 0.1412(5) 0.8993(4) 0.9234(2) 0.0798(13) Uani 1 1 d . . . H21A H 0.0762 0.8420 0.8788 0.096 Uiso 1 1 calc R . . C22 C 0.2453(5) 0.9725(4) 0.9081(2) 0.0762(13) Uani 1 1 d . . . H22A H 0.2518 0.9650 0.8534 0.091 Uiso 1 1 calc R . . C23 C 0.3465(4) 1.0617(3) 0.9746(2) 0.0519(9) Uani 1 1 d . . . C24 C 0.4598(4) 1.1378(3) 0.9619(2) 0.0642(11) Uani 1 1 d . . . H24A H 0.4713 1.1314 0.9080 0.077 Uiso 1 1 calc R . . C25 C 0.5525(5) 1.2204(3) 1.0275(2) 0.0674(11) Uani 1 1 d . . . H25A H 0.6269 1.2725 1.0194 0.081 Uiso 1 1 calc R . . C26 C 0.5346(4) 1.2261(3) 1.1074(2) 0.0572(10) Uani 1 1 d . . . H26A H 0.5995 1.2825 1.1525 0.069 Uiso 1 1 calc R . . C27 C 0.3364(4) 1.0729(3) 1.05697(19) 0.0434(8) Uani 1 1 d . . . C28 C 0.2239(4) 0.9943(3) 1.07282(19) 0.0463(8) Uani 1 1 d . . . C29 C 0.2044(4) 1.3278(3) 1.2063(2) 0.0650(10) Uani 1 1 d . . . H29A H 0.2451 1.3180 1.1602 0.078 Uiso 1 1 calc R . . C30 C 0.1020(5) 1.3935(4) 1.2122(3) 0.0844(14) Uani 1 1 d . . . H30A H 0.0733 1.4256 1.1703 0.101 Uiso 1 1 calc R . . C31 C 0.0445(5) 1.4102(4) 1.2801(3) 0.0854(14) Uani 1 1 d . . . H31A H -0.0245 1.4538 1.2846 0.102 Uiso 1 1 calc R . . C32 C 0.0873(4) 1.3631(3) 1.3429(3) 0.0623(10) Uani 1 1 d . . . C33 C 0.0345(4) 1.3797(4) 1.4167(3) 0.0762(13) Uani 1 1 d . . . H33A H -0.0367 1.4209 1.4229 0.091 Uiso 1 1 calc R . . C34 C 0.0846(4) 1.3377(4) 1.4773(3) 0.0746(13) Uani 1 1 d . . . H34A H 0.0500 1.3525 1.5257 0.090 Uiso 1 1 calc R . . C35 C 0.1907(4) 1.2701(3) 1.4696(2) 0.0533(9) Uani 1 1 d . . . C36 C 0.2472(4) 1.2260(3) 1.5316(2) 0.0664(11) Uani 1 1 d . . . H36A H 0.2187 1.2419 1.5819 0.080 Uiso 1 1 calc R . . C37 C 0.3427(5) 1.1605(3) 1.5187(2) 0.0663(11) Uani 1 1 d . . . H37A H 0.3809 1.1306 1.5600 0.080 Uiso 1 1 calc R . . C38 C 0.3845(4) 1.1374(3) 1.44311(19) 0.0540(9) Uani 1 1 d . . . H38A H 0.4499 1.0909 1.4346 0.065 Uiso 1 1 calc R . . C39 C 0.2400(3) 1.2469(3) 1.39519(18) 0.0408(8) Uani 1 1 d . . . C40 C 0.1896(3) 1.2960(3) 1.3318(2) 0.0455(8) Uani 1 1 d . . . C41 C 0.6110(3) 1.4323(3) 1.34900(18) 0.0393(7) Uani 1 1 d . . . C42 C 0.5518(3) 1.4666(3) 1.42701(17) 0.0372(7) Uani 1 1 d . . . C43 C 0.5936(3) 1.4228(3) 1.49347(18) 0.0371(7) Uani 1 1 d . . . C44 C 0.6873(3) 1.3452(3) 1.4898(2) 0.0473(8) Uani 1 1 d . . . H44A H 0.7216 1.3215 1.4419 0.057 Uiso 1 1 calc R . . C45 C 0.7277(4) 1.3051(3) 1.5546(2) 0.0589(10) Uani 1 1 d . . . H45A H 0.7905 1.2556 1.5513 0.071 Uiso 1 1 calc R . . C46 C 0.6747(4) 1.3383(3) 1.6271(2) 0.0612(10) Uani 1 1 d . . . H46A H 0.7013 1.3091 1.6710 0.073 Uiso 1 1 calc R . . C47 C 0.5868(4) 1.4111(3) 1.63361(19) 0.0488(8) Uani 1 1 d . . . H47A H 0.5548 1.4325 1.6826 0.059 Uiso 1 1 calc R . . C48 C 0.4600(3) 1.5426(3) 1.43224(17) 0.0368(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.06491(18) 0.04221(15) 0.03743(14) 0.01422(11) 0.02359(11) 0.01999(12) N1 0.0712(19) 0.0374(16) 0.0408(15) 0.0152(13) 0.0266(15) 0.0144(15) N2 0.0612(18) 0.0509(18) 0.0481(16) 0.0197(14) 0.0261(14) 0.0152(15) N3 0.0547(18) 0.0496(18) 0.0407(15) 0.0111(14) 0.0041(14) 0.0138(15) N4 0.0512(16) 0.0401(16) 0.0369(14) 0.0122(12) 0.0170(13) 0.0146(14) O1 0.0778(17) 0.0438(15) 0.0550(14) 0.0172(12) 0.0311(13) 0.0067(13) O2 0.0667(16) 0.0421(15) 0.0506(14) 0.0099(12) 0.0231(12) 0.0137(12) O3 0.0645(16) 0.0473(14) 0.0557(15) 0.0219(12) 0.0232(12) 0.0251(12) O4 0.102(2) 0.079(2) 0.0711(17) 0.0328(15) 0.0523(17) 0.0389(17) O5 0.098(2) 0.0482(16) 0.0704(17) 0.0291(14) 0.0308(15) 0.0332(15) O6 0.162(3) 0.082(2) 0.107(2) 0.0358(19) 0.087(2) 0.063(2) C1 0.048(2) 0.047(2) 0.0404(18) 0.0186(16) 0.0108(16) 0.0118(17) C2 0.057(2) 0.040(2) 0.0396(17) 0.0205(16) 0.0190(16) 0.0174(17) C3 0.064(2) 0.042(2) 0.0391(18) 0.0197(16) 0.0145(17) 0.0110(18) C4 0.064(3) 0.059(3) 0.053(2) 0.025(2) 0.0104(19) 0.005(2) C5 0.081(3) 0.080(3) 0.069(3) 0.034(3) 0.006(2) -0.008(3) C6 0.115(4) 0.046(3) 0.058(3) 0.014(2) 0.008(3) -0.017(3) C7 0.114(4) 0.038(2) 0.053(2) 0.0106(19) 0.018(2) 0.006(2) C8 0.087(3) 0.035(2) 0.0356(18) 0.0157(16) 0.0196(19) 0.010(2) C9 0.081(3) 0.047(2) 0.0381(18) 0.0235(17) 0.0260(18) 0.030(2) C10 0.070(2) 0.044(2) 0.0411(18) 0.0245(17) 0.0204(18) 0.0228(19) C11 0.077(3) 0.069(3) 0.060(2) 0.035(2) 0.027(2) 0.042(2) C12 0.061(3) 0.074(3) 0.079(3) 0.034(3) 0.012(2) 0.018(2) C13 0.066(3) 0.062(3) 0.061(2) 0.018(2) 0.005(2) 0.010(2) C14 0.065(2) 0.045(2) 0.051(2) 0.0130(18) 0.0158(18) 0.0155(19) C15 0.059(2) 0.042(2) 0.0390(18) 0.0196(16) 0.0199(16) 0.0188(18) C16 0.110(3) 0.055(3) 0.049(2) 0.0230(19) 0.034(2) 0.042(2) C17 0.068(3) 0.068(3) 0.067(2) 0.029(2) 0.029(2) 0.009(2) C18 0.065(3) 0.084(3) 0.087(3) 0.029(3) 0.022(2) -0.007(3) C19 0.066(3) 0.089(4) 0.078(3) 0.020(3) 0.010(2) -0.007(3) C20 0.063(2) 0.065(3) 0.054(2) 0.012(2) 0.008(2) 0.012(2) C21 0.084(3) 0.095(4) 0.041(2) 0.010(2) -0.003(2) 0.004(3) C22 0.096(3) 0.096(4) 0.035(2) 0.018(2) 0.012(2) 0.025(3) C23 0.073(2) 0.055(2) 0.0373(19) 0.0202(17) 0.0184(18) 0.022(2) C24 0.104(3) 0.062(3) 0.044(2) 0.027(2) 0.034(2) 0.029(2) C25 0.103(3) 0.054(2) 0.063(2) 0.028(2) 0.049(2) 0.017(2) C26 0.081(3) 0.046(2) 0.049(2) 0.0151(17) 0.0286(19) 0.011(2) C27 0.059(2) 0.0401(19) 0.0379(18) 0.0151(16) 0.0149(16) 0.0202(18) C28 0.054(2) 0.048(2) 0.0434(19) 0.0165(17) 0.0168(17) 0.0187(18) C29 0.079(3) 0.054(2) 0.055(2) 0.014(2) -0.003(2) 0.020(2) C30 0.100(4) 0.069(3) 0.072(3) 0.018(3) -0.024(3) 0.034(3) C31 0.066(3) 0.074(3) 0.096(4) 0.004(3) -0.016(3) 0.033(3) C32 0.042(2) 0.053(2) 0.076(3) -0.001(2) 0.0013(19) 0.0144(19) C33 0.048(2) 0.069(3) 0.102(3) -0.001(3) 0.031(2) 0.022(2) C34 0.064(3) 0.065(3) 0.086(3) -0.003(2) 0.044(2) 0.007(2) C35 0.056(2) 0.038(2) 0.058(2) -0.0015(17) 0.0317(18) -0.0019(17) C36 0.099(3) 0.052(2) 0.044(2) 0.0081(19) 0.036(2) -0.003(2) C37 0.106(3) 0.050(2) 0.043(2) 0.0174(18) 0.023(2) 0.010(2) C38 0.079(3) 0.047(2) 0.0391(19) 0.0154(17) 0.0148(18) 0.016(2) C39 0.0431(19) 0.0309(17) 0.0406(17) -0.0005(14) 0.0151(15) 0.0015(15) C40 0.0364(18) 0.042(2) 0.0477(19) -0.0012(16) 0.0043(15) 0.0097(16) C41 0.0462(19) 0.0364(19) 0.0357(17) 0.0108(15) 0.0096(15) 0.0113(16) C42 0.0405(18) 0.0332(17) 0.0371(16) 0.0119(14) 0.0088(14) 0.0051(15) C43 0.0400(18) 0.0331(17) 0.0396(17) 0.0133(14) 0.0099(14) 0.0078(15) C44 0.048(2) 0.053(2) 0.0493(19) 0.0222(17) 0.0162(16) 0.0204(18) C45 0.064(2) 0.065(3) 0.067(2) 0.036(2) 0.022(2) 0.032(2) C46 0.073(3) 0.069(3) 0.057(2) 0.038(2) 0.013(2) 0.030(2) C47 0.060(2) 0.053(2) 0.0385(18) 0.0184(17) 0.0121(16) 0.0176(19) C48 0.0405(18) 0.0329(17) 0.0362(16) 0.0128(14) 0.0075(14) 0.0039(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O5 2.217(2) . ? Cd1 N4 2.320(2) . ? Cd1 O2 2.323(2) . ? Cd1 N1 2.379(2) . ? Cd1 N3 2.384(3) . ? Cd1 N2 2.422(3) . ? N1 C26 1.317(4) . ? N1 C27 1.351(4) . ? N2 C17 1.322(4) . ? N2 C28 1.358(4) . ? N3 C29 1.320(4) . ? N3 C40 1.361(4) . ? N4 C38 1.325(4) . ? N4 C39 1.348(4) . ? O1 C41 1.255(4) . ? O2 C41 1.243(4) . ? O3 C1 1.294(4) . ? O3 H3 0.8200 . ? O4 C1 1.203(3) . ? O5 C16 1.244(4) . ? O6 C16 1.264(4) . ? C1 C2 1.514(4) . ? C2 C3 1.394(4) . ? C2 C15 1.397(4) . ? C3 C4 1.435(5) . ? C3 C8 1.445(5) . ? C4 C5 1.358(5) . ? C4 H4A 0.9300 . ? C5 C6 1.405(6) . ? C5 H5A 0.9300 . ? C6 C7 1.348(6) . ? C6 H6A 0.9300 . ? C7 C8 1.413(5) . ? C7 H7A 0.9300 . ? C8 C9 1.406(5) . ? C9 C10 1.391(5) . ? C9 C16 1.508(5) . ? C10 C15 1.437(4) . ? C10 C11 1.445(5) . ? C11 C12 1.338(5) . ? C11 H11A 0.9300 . ? C12 C13 1.399(5) . ? C12 H12A 0.9300 . ? C13 C14 1.361(5) . ? C13 H13A 0.9300 . ? C14 C15 1.426(5) . ? C14 H14A 0.9300 . ? C17 C18 1.389(5) . ? C17 H17A 0.9300 . ? C18 C19 1.352(5) . ? C18 H18A 0.9300 . ? C19 C20 1.402(5) . ? C19 H19A 0.9300 . ? C20 C28 1.398(5) . ? C20 C21 1.422(5) . ? C21 C22 1.337(5) . ? C21 H21A 0.9300 . ? C22 C23 1.423(5) . ? C22 H22A 0.9300 . ? C23 C24 1.399(5) . ? C23 C27 1.399(4) . ? C24 C25 1.349(5) . ? C24 H24A 0.9300 . ? C25 C26 1.391(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.436(4) . ? C29 C30 1.386(5) . ? C29 H29A 0.9300 . ? C30 C31 1.355(6) . ? C30 H30A 0.9300 . ? C31 C32 1.385(6) . ? C31 H31A 0.9300 . ? C32 C40 1.403(4) . ? C32 C33 1.420(5) . ? C33 C34 1.333(6) . ? C33 H33A 0.9300 . ? C34 C35 1.434(5) . ? C34 H34A 0.9300 . ? C35 C36 1.389(5) . ? C35 C39 1.410(4) . ? C36 C37 1.338(5) . ? C36 H36A 0.9300 . ? C37 C38 1.392(5) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.430(4) . ? C41 C42 1.527(4) . ? C42 C48 1.392(4) . ? C42 C43 1.409(4) . ? C43 C44 1.422(4) . ? C43 C48 1.441(4) 2_688 ? C44 C45 1.353(4) . ? C44 H44A 0.9300 . ? C45 C46 1.410(5) . ? C45 H45A 0.9300 . ? C46 C47 1.334(5) . ? C46 H46A 0.9300 . ? C47 C48 1.432(4) 2_688 ? C47 H47A 0.9300 . ? C48 C47 1.432(4) 2_688 ? C48 C43 1.441(4) 2_688 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 N4 109.57(9) . . ? O5 Cd1 O2 97.99(9) . . ? N4 Cd1 O2 95.04(8) . . ? O5 Cd1 N1 87.39(9) . . ? N4 Cd1 N1 162.68(9) . . ? O2 Cd1 N1 85.75(9) . . ? O5 Cd1 N3 177.19(10) . . ? N4 Cd1 N3 71.00(9) . . ? O2 Cd1 N3 84.66(9) . . ? N1 Cd1 N3 91.89(9) . . ? O5 Cd1 N2 91.57(10) . . ? N4 Cd1 N2 105.77(9) . . ? O2 Cd1 N2 152.71(8) . . ? N1 Cd1 N2 69.14(9) . . ? N3 Cd1 N2 85.63(9) . . ? C26 N1 C27 118.5(3) . . ? C26 N1 Cd1 123.7(2) . . ? C27 N1 Cd1 117.5(2) . . ? C17 N2 C28 117.5(3) . . ? C17 N2 Cd1 126.0(2) . . ? C28 N2 Cd1 116.3(2) . . ? C29 N3 C40 118.2(3) . . ? C29 N3 Cd1 127.1(2) . . ? C40 N3 Cd1 114.6(2) . . ? C38 N4 C39 118.8(3) . . ? C38 N4 Cd1 124.3(2) . . ? C39 N4 Cd1 116.80(19) . . ? C41 O2 Cd1 143.3(2) . . ? C1 O3 H3 109.5 . . ? C16 O5 Cd1 114.8(2) . . ? O4 C1 O3 122.2(3) . . ? O4 C1 C2 120.9(3) . . ? O3 C1 C2 116.9(3) . . ? C3 C2 C15 121.3(3) . . ? C3 C2 C1 119.3(3) . . ? C15 C2 C1 119.3(3) . . ? C2 C3 C4 122.0(3) . . ? C2 C3 C8 119.2(3) . . ? C4 C3 C8 118.8(3) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 121.4(4) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 121.6(4) . . ? C6 C7 H7A 119.2 . . ? C8 C7 H7A 119.2 . . ? C9 C8 C7 123.3(4) . . ? C9 C8 C3 119.1(3) . . ? C7 C8 C3 117.6(4) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 C16 119.4(4) . . ? C8 C9 C16 119.2(4) . . ? C9 C10 C15 119.3(3) . . ? C9 C10 C11 123.7(3) . . ? C15 C10 C11 116.9(3) . . ? C12 C11 C10 121.8(3) . . ? C12 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C11 C12 C13 121.7(4) . . ? C11 C12 H12A 119.2 . . ? C13 C12 H12A 119.2 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 122.1(3) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C2 C15 C14 122.0(3) . . ? C2 C15 C10 119.6(3) . . ? C14 C15 C10 118.3(3) . . ? O5 C16 O6 124.1(4) . . ? O5 C16 C9 116.9(3) . . ? O6 C16 C9 118.6(3) . . ? N2 C17 C18 123.9(4) . . ? N2 C17 H17A 118.1 . . ? C18 C17 H17A 118.1 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C28 C20 C19 117.6(3) . . ? C28 C20 C21 119.0(4) . . ? C19 C20 C21 123.4(4) . . ? C22 C21 C20 121.6(4) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C27 117.6(3) . . ? C24 C23 C22 122.9(3) . . ? C27 C23 C22 119.5(3) . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 118.6(4) . . ? C24 C25 H25A 120.7 . . ? C26 C25 H25A 120.7 . . ? N1 C26 C25 123.3(4) . . ? N1 C26 H26A 118.4 . . ? C25 C26 H26A 118.4 . . ? N1 C27 C23 121.8(3) . . ? N1 C27 C28 118.9(3) . . ? C23 C27 C28 119.3(3) . . ? N2 C28 C20 122.4(3) . . ? N2 C28 C27 117.9(3) . . ? C20 C28 C27 119.7(3) . . ? N3 C29 C30 122.9(4) . . ? N3 C29 H29A 118.6 . . ? C30 C29 H29A 118.6 . . ? C31 C30 C29 118.8(4) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? C30 C31 C32 120.9(4) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C31 C32 C40 116.9(4) . . ? C31 C32 C33 123.9(4) . . ? C40 C32 C33 119.2(4) . . ? C34 C33 C32 121.6(4) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 121.4(4) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C36 C35 C39 118.2(3) . . ? C36 C35 C34 123.3(3) . . ? C39 C35 C34 118.5(4) . . ? C37 C36 C35 119.9(3) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C38 119.4(4) . . ? C36 C37 H37A 120.3 . . ? C38 C37 H37A 120.3 . . ? N4 C38 C37 122.6(3) . . ? N4 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? N4 C39 C35 121.0(3) . . ? N4 C39 C40 119.2(3) . . ? C35 C39 C40 119.7(3) . . ? N3 C40 C32 122.3(3) . . ? N3 C40 C39 118.2(3) . . ? C32 C40 C39 119.5(3) . . ? O2 C41 O1 124.3(3) . . ? O2 C41 C42 120.0(3) . . ? O1 C41 C42 115.8(3) . . ? C48 C42 C43 121.0(3) . . ? C48 C42 C41 119.6(3) . . ? C43 C42 C41 119.4(3) . . ? C42 C43 C44 122.1(3) . . ? C42 C43 C48 119.2(3) . 2_688 ? C44 C43 C48 118.7(3) . 2_688 ? C45 C44 C43 121.3(3) . . ? C45 C44 H44A 119.3 . . ? C43 C44 H44A 119.3 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C47 C46 C45 120.8(3) . . ? C47 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C46 C47 C48 122.2(3) . 2_688 ? C46 C47 H47A 118.9 . . ? C48 C47 H47A 118.9 2_688 . ? C42 C48 C47 123.3(3) . 2_688 ? C42 C48 C43 119.8(3) . 2_688 ? C47 C48 C43 116.9(3) 2_688 2_688 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cd1 N1 C26 -85.8(3) . . . . ? N4 Cd1 N1 C26 105.7(4) . . . . ? O2 Cd1 N1 C26 12.4(3) . . . . ? N3 Cd1 N1 C26 96.9(3) . . . . ? N2 Cd1 N1 C26 -178.5(3) . . . . ? O5 Cd1 N1 C27 88.3(2) . . . . ? N4 Cd1 N1 C27 -80.1(4) . . . . ? O2 Cd1 N1 C27 -173.4(2) . . . . ? N3 Cd1 N1 C27 -88.9(2) . . . . ? N2 Cd1 N1 C27 -4.3(2) . . . . ? O5 Cd1 N2 C17 92.9(3) . . . . ? N4 Cd1 N2 C17 -17.9(3) . . . . ? O2 Cd1 N2 C17 -156.2(3) . . . . ? N1 Cd1 N2 C17 179.5(3) . . . . ? N3 Cd1 N2 C17 -86.8(3) . . . . ? O5 Cd1 N2 C28 -82.7(2) . . . . ? N4 Cd1 N2 C28 166.5(2) . . . . ? O2 Cd1 N2 C28 28.2(3) . . . . ? N1 Cd1 N2 C28 3.9(2) . . . . ? N3 Cd1 N2 C28 97.6(2) . . . . ? O5 Cd1 N3 C29 -78.6(19) . . . . ? N4 Cd1 N3 C29 179.3(3) . . . . ? O2 Cd1 N3 C29 82.1(3) . . . . ? N1 Cd1 N3 C29 -3.5(3) . . . . ? N2 Cd1 N3 C29 -72.4(3) . . . . ? O5 Cd1 N3 C40 99.1(18) . . . . ? N4 Cd1 N3 C40 -3.0(2) . . . . ? O2 Cd1 N3 C40 -100.2(2) . . . . ? N1 Cd1 N3 C40 174.2(2) . . . . ? N2 Cd1 N3 C40 105.3(2) . . . . ? O5 Cd1 N4 C38 7.6(3) . . . . ? O2 Cd1 N4 C38 -92.7(3) . . . . ? N1 Cd1 N4 C38 175.4(3) . . . . ? N3 Cd1 N4 C38 -175.3(3) . . . . ? N2 Cd1 N4 C38 105.1(3) . . . . ? O5 Cd1 N4 C39 -176.2(2) . . . . ? O2 Cd1 N4 C39 83.5(2) . . . . ? N1 Cd1 N4 C39 -8.4(4) . . . . ? N3 Cd1 N4 C39 0.9(2) . . . . ? N2 Cd1 N4 C39 -78.7(2) . . . . ? O5 Cd1 O2 C41 -149.3(3) . . . . ? N4 Cd1 O2 C41 -38.7(3) . . . . ? N1 Cd1 O2 C41 124.0(3) . . . . ? N3 Cd1 O2 C41 31.7(3) . . . . ? N2 Cd1 O2 C41 101.3(4) . . . . ? N4 Cd1 O5 C16 40.5(3) . . . . ? O2 Cd1 O5 C16 138.8(3) . . . . ? N1 Cd1 O5 C16 -135.9(3) . . . . ? N3 Cd1 O5 C16 -60.7(19) . . . . ? N2 Cd1 O5 C16 -66.9(3) . . . . ? O4 C1 C2 C3 -79.2(4) . . . . ? O3 C1 C2 C3 100.8(3) . . . . ? O4 C1 C2 C15 101.1(4) . . . . ? O3 C1 C2 C15 -78.9(4) . . . . ? C15 C2 C3 C4 175.9(3) . . . . ? C1 C2 C3 C4 -3.7(4) . . . . ? C15 C2 C3 C8 -3.8(4) . . . . ? C1 C2 C3 C8 176.5(3) . . . . ? C2 C3 C4 C5 -179.2(3) . . . . ? C8 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C6 -1.8(5) . . . . ? C4 C5 C6 C7 1.4(6) . . . . ? C5 C6 C7 C8 0.5(6) . . . . ? C6 C7 C8 C9 176.2(3) . . . . ? C6 C7 C8 C3 -1.7(5) . . . . ? C2 C3 C8 C9 2.9(4) . . . . ? C4 C3 C8 C9 -176.8(3) . . . . ? C2 C3 C8 C7 -179.1(3) . . . . ? C4 C3 C8 C7 1.2(4) . . . . ? C7 C8 C9 C10 -177.2(3) . . . . ? C3 C8 C9 C10 0.7(4) . . . . ? C7 C8 C9 C16 4.0(5) . . . . ? C3 C8 C9 C16 -178.1(3) . . . . ? C8 C9 C10 C15 -3.5(4) . . . . ? C16 C9 C10 C15 175.4(3) . . . . ? C8 C9 C10 C11 -179.9(3) . . . . ? C16 C9 C10 C11 -1.1(4) . . . . ? C9 C10 C11 C12 176.0(3) . . . . ? C15 C10 C11 C12 -0.6(5) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C14 0.6(6) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C3 C2 C15 C14 179.8(3) . . . . ? C1 C2 C15 C14 -0.5(4) . . . . ? C3 C2 C15 C10 1.1(4) . . . . ? C1 C2 C15 C10 -179.2(3) . . . . ? C13 C14 C15 C2 -178.7(3) . . . . ? C13 C14 C15 C10 0.0(5) . . . . ? C9 C10 C15 C2 2.6(4) . . . . ? C11 C10 C15 C2 179.3(3) . . . . ? C9 C10 C15 C14 -176.1(3) . . . . ? C11 C10 C15 C14 0.6(4) . . . . ? Cd1 O5 C16 O6 -7.6(5) . . . . ? Cd1 O5 C16 C9 164.8(3) . . . . ? C10 C9 C16 O5 -113.1(4) . . . . ? C8 C9 C16 O5 65.7(4) . . . . ? C10 C9 C16 O6 59.7(5) . . . . ? C8 C9 C16 O6 -121.5(4) . . . . ? C28 N2 C17 C18 2.2(6) . . . . ? Cd1 N2 C17 C18 -173.4(3) . . . . ? N2 C17 C18 C19 -1.7(7) . . . . ? C17 C18 C19 C20 0.0(7) . . . . ? C18 C19 C20 C28 1.0(6) . . . . ? C18 C19 C20 C21 179.6(4) . . . . ? C28 C20 C21 C22 0.8(6) . . . . ? C19 C20 C21 C22 -177.8(4) . . . . ? C20 C21 C22 C23 -0.2(7) . . . . ? C21 C22 C23 C24 178.0(4) . . . . ? C21 C22 C23 C27 -0.1(6) . . . . ? C27 C23 C24 C25 -1.7(5) . . . . ? C22 C23 C24 C25 -179.8(4) . . . . ? C23 C24 C25 C26 1.5(6) . . . . ? C27 N1 C26 C25 0.5(5) . . . . ? Cd1 N1 C26 C25 174.6(3) . . . . ? C24 C25 C26 N1 -0.8(6) . . . . ? C26 N1 C27 C23 -0.8(5) . . . . ? Cd1 N1 C27 C23 -175.2(2) . . . . ? C26 N1 C27 C28 178.9(3) . . . . ? Cd1 N1 C27 C28 4.5(4) . . . . ? C24 C23 C27 N1 1.4(5) . . . . ? C22 C23 C27 N1 179.6(3) . . . . ? C24 C23 C27 C28 -178.3(3) . . . . ? C22 C23 C27 C28 -0.1(5) . . . . ? C17 N2 C28 C20 -1.0(5) . . . . ? Cd1 N2 C28 C20 175.0(3) . . . . ? C17 N2 C28 C27 -179.3(3) . . . . ? Cd1 N2 C28 C27 -3.3(4) . . . . ? C19 C20 C28 N2 -0.5(5) . . . . ? C21 C20 C28 N2 -179.2(3) . . . . ? C19 C20 C28 C27 177.7(3) . . . . ? C21 C20 C28 C27 -1.0(5) . . . . ? N1 C27 C28 N2 -0.7(4) . . . . ? C23 C27 C28 N2 179.0(3) . . . . ? N1 C27 C28 C20 -179.0(3) . . . . ? C23 C27 C28 C20 0.7(5) . . . . ? C40 N3 C29 C30 -1.9(6) . . . . ? Cd1 N3 C29 C30 175.7(3) . . . . ? N3 C29 C30 C31 1.4(6) . . . . ? C29 C30 C31 C32 0.3(7) . . . . ? C30 C31 C32 C40 -1.4(6) . . . . ? C30 C31 C32 C33 178.2(4) . . . . ? C31 C32 C33 C34 -176.4(4) . . . . ? C40 C32 C33 C34 3.2(6) . . . . ? C32 C33 C34 C35 -2.2(7) . . . . ? C33 C34 C35 C36 179.1(4) . . . . ? C33 C34 C35 C39 -1.1(6) . . . . ? C39 C35 C36 C37 -1.9(5) . . . . ? C34 C35 C36 C37 177.9(4) . . . . ? C35 C36 C37 C38 0.1(6) . . . . ? C39 N4 C38 C37 0.2(5) . . . . ? Cd1 N4 C38 C37 176.3(3) . . . . ? C36 C37 C38 N4 0.9(6) . . . . ? C38 N4 C39 C35 -2.1(4) . . . . ? Cd1 N4 C39 C35 -178.6(2) . . . . ? C38 N4 C39 C40 177.7(3) . . . . ? Cd1 N4 C39 C40 1.3(4) . . . . ? C36 C35 C39 N4 3.0(5) . . . . ? C34 C35 C39 N4 -176.8(3) . . . . ? C36 C35 C39 C40 -176.8(3) . . . . ? C34 C35 C39 C40 3.4(5) . . . . ? C29 N3 C40 C32 0.7(5) . . . . ? Cd1 N3 C40 C32 -177.2(2) . . . . ? C29 N3 C40 C39 -177.2(3) . . . . ? Cd1 N3 C40 C39 4.8(4) . . . . ? C31 C32 C40 N3 0.8(5) . . . . ? C33 C32 C40 N3 -178.8(3) . . . . ? C31 C32 C40 C39 178.8(3) . . . . ? C33 C32 C40 C39 -0.8(5) . . . . ? N4 C39 C40 N3 -4.2(4) . . . . ? C35 C39 C40 N3 175.6(3) . . . . ? N4 C39 C40 C32 177.7(3) . . . . ? C35 C39 C40 C32 -2.4(5) . . . . ? Cd1 O2 C41 O1 -146.5(3) . . . . ? Cd1 O2 C41 C42 34.5(5) . . . . ? O2 C41 C42 C48 -118.7(3) . . . . ? O1 C41 C42 C48 62.3(4) . . . . ? O2 C41 C42 C43 62.7(4) . . . . ? O1 C41 C42 C43 -116.4(3) . . . . ? C48 C42 C43 C44 -179.9(3) . . . . ? C41 C42 C43 C44 -1.3(5) . . . . ? C48 C42 C43 C48 0.0(5) . . . 2_688 ? C41 C42 C43 C48 178.6(3) . . . 2_688 ? C42 C43 C44 C45 179.2(3) . . . . ? C48 C43 C44 C45 -0.8(5) 2_688 . . . ? C43 C44 C45 C46 1.2(6) . . . . ? C44 C45 C46 C47 -1.4(6) . . . . ? C45 C46 C47 C48 1.1(6) . . . 2_688 ? C43 C42 C48 C47 -179.4(3) . . . 2_688 ? C41 C42 C48 C47 2.0(5) . . . 2_688 ? C43 C42 C48 C43 0.0(5) . . . 2_688 ? C41 C42 C48 C43 -178.6(3) . . . 2_688 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.499 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.067 data_3 _database_code_depnum_ccdc_archive 'CCDC 749746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H44 Cd2 N12 O8' _chemical_formula_weight 1333.91 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 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 20.542(5) _cell_length_b 28.488(7) _cell_length_c 20.519(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.776(5) _cell_angle_gamma 90.00 _cell_volume 11833(5) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 9715 _cell_measurement_theta_min 1.4295 _cell_measurement_theta_max 27.8565 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5376 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7338 _exptl_absorpt_correction_T_max 0.8587 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47578 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10422 _reflns_number_gt 7735 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1398P)^2^+39.2002P] 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 SHELXL _refine_ls_extinction_coef 0.00032(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10422 _refine_ls_number_parameters 757 _refine_ls_number_restraints 299 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.2555 _refine_ls_wR_factor_gt 0.2326 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.69783(3) 0.881904(18) 0.41284(3) 0.0546(2) Uani 1 1 d . . . Cd2 Cd 0.81652(4) 0.91770(2) 0.65610(3) 0.0798(3) Uani 1 1 d . . . N1 N 0.7655(4) 0.8283(2) 0.3703(3) 0.0660(17) Uani 1 1 d . . . N2 N 0.6337(3) 0.8209(2) 0.3643(3) 0.0604(16) Uani 1 1 d . . . N4 N 0.6621(3) 0.9272(2) 0.3144(3) 0.0574(15) Uani 1 1 d . . . N5 N 0.7624(3) 0.9491(2) 0.4135(3) 0.0509(14) Uani 1 1 d . . . N8 N 0.7410(4) 0.9746(2) 0.6099(3) 0.0663(18) Uani 1 1 d . . . N7 N 0.8415(5) 0.9906(3) 0.7117(4) 0.083(2) Uani 1 1 d . . . C1 C 0.8303(5) 0.8327(4) 0.3746(5) 0.079(3) Uani 1 1 d . . . H1 H 0.8506 0.8596 0.3942 0.095 Uiso 1 1 calc R . . C2 C 0.8688(6) 0.7993(4) 0.3511(6) 0.098(3) Uani 1 1 d . . . H2 H 0.9142 0.8034 0.3544 0.118 Uiso 1 1 calc R . . C3 C 0.8373(8) 0.7586(5) 0.3219(6) 0.116(4) Uani 1 1 d . . . H3 H 0.8621 0.7349 0.3070 0.139 Uiso 1 1 calc R . . C4 C 0.7716(6) 0.7542(3) 0.3156(5) 0.090(3) Uani 1 1 d . . . H4 H 0.7503 0.7282 0.2946 0.108 Uiso 1 1 calc R . . C5 C 0.7354(5) 0.7891(3) 0.3410(4) 0.074(2) Uani 1 1 d . . . C6 C 0.6640(5) 0.7863(3) 0.3381(4) 0.071(2) Uani 1 1 d . . . C7 C 0.6172(6) 0.7522(3) 0.3125(4) 0.088(3) Uani 1 1 d . . . H7 H 0.6251 0.7245 0.2912 0.105 Uiso 1 1 calc R . . C8 C 0.5573(6) 0.7679(3) 0.3251(4) 0.084(3) Uani 1 1 d . . . H8 H 0.5166 0.7530 0.3147 0.101 Uiso 1 1 calc R . . N3 N 0.5705(4) 0.8098(2) 0.3559(3) 0.0707(18) Uani 1 1 d . . . H3A H 0.5408 0.8273 0.3685 0.085 Uiso 1 1 calc R . . C10 C 0.6129(4) 0.9166(3) 0.2662(4) 0.067(2) Uani 1 1 d . . . H10 H 0.5930 0.8874 0.2676 0.080 Uiso 1 1 calc R . . C11 C 0.5891(5) 0.9455(3) 0.2143(4) 0.074(2) Uani 1 1 d . . . H11 H 0.5531 0.9368 0.1827 0.089 Uiso 1 1 calc R . . C12 C 0.6197(4) 0.9873(3) 0.2104(4) 0.073(2) Uani 1 1 d . . . H12 H 0.6062 1.0072 0.1748 0.087 Uiso 1 1 calc R . . C13 C 0.6707(4) 1.0001(3) 0.2591(3) 0.0584(18) Uani 1 1 d . . . H13 H 0.6911 1.0292 0.2578 0.070 Uiso 1 1 calc R . . C14 C 0.6911(4) 0.9694(3) 0.3098(3) 0.0520(17) Uani 1 1 d . . . C15 C 0.7458(4) 0.9808(3) 0.3647(3) 0.0543(17) Uani 1 1 d . . . C16 C 0.7848(5) 1.0201(3) 0.3758(4) 0.076(2) Uani 1 1 d . . . H16 H 0.7832 1.0470 0.3499 0.091 Uiso 1 1 calc R . . C17 C 0.8258(5) 1.0110(3) 0.4327(4) 0.082(3) Uani 1 1 d . . . H17 H 0.8588 1.0310 0.4531 0.099 Uiso 1 1 calc R . . N6 N 0.8123(3) 0.9694(2) 0.4553(3) 0.0571(15) Uani 1 1 d . . . H6A H 0.8323 0.9571 0.4915 0.069 Uiso 1 1 calc R . . C19 C 0.7686(4) 0.8441(3) 0.5565(4) 0.0566(18) Uani 1 1 d . . . C20 C 0.7590(4) 0.7953(2) 0.5272(4) 0.0588(19) Uani 1 1 d . . . C21 C 0.6949(4) 0.7759(2) 0.5153(4) 0.0553(18) Uani 1 1 d . . . C22 C 0.6383(4) 0.7998(3) 0.5304(4) 0.064(2) Uani 1 1 d . . . H22 H 0.6432 0.8296 0.5493 0.077 Uiso 1 1 calc R . . C23 C 0.5766(4) 0.7795(3) 0.5174(4) 0.071(2) Uani 1 1 d . . . H23 H 0.5403 0.7957 0.5275 0.085 Uiso 1 1 calc R . . C24 C 0.9319(4) 0.7642(3) 0.5103(5) 0.077(2) Uani 1 1 d . . . H24 H 0.9740 0.7773 0.5188 0.093 Uiso 1 1 calc R . . C25 C 0.8794(4) 0.7889(3) 0.5256(4) 0.064(2) Uani 1 1 d . . . H25 H 0.8866 0.8186 0.5445 0.077 Uiso 1 1 calc R . . C26 C 0.8142(4) 0.7705(2) 0.5135(4) 0.0571(18) Uani 1 1 d . . . C27 C 0.5594(4) 0.9205(3) 0.4424(4) 0.0560(18) Uani 1 1 d . . . C28 C 0.5275(3) 0.9618(2) 0.4722(4) 0.0508(16) Uani 1 1 d . . . C29 C 0.5221(3) 1.0046(3) 0.4391(4) 0.0535(17) Uani 1 1 d . . . C30 C 0.5461(4) 1.0119(3) 0.3773(4) 0.071(2) Uani 1 1 d . . . H30 H 0.5643 0.9868 0.3577 0.085 Uiso 1 1 calc R . . C31 C 0.5424(5) 1.0547(4) 0.3475(5) 0.086(3) Uani 1 1 d . . . H31 H 0.5583 1.0589 0.3081 0.103 Uiso 1 1 calc R . . C32 C 0.4857(5) 0.9076(3) 0.6229(5) 0.085(3) Uani 1 1 d . . . H32 H 0.4886 0.8784 0.6435 0.102 Uiso 1 1 calc R . . C33 C 0.5086(4) 0.9125(3) 0.5655(5) 0.070(2) Uani 1 1 d . . . H33 H 0.5268 0.8866 0.5474 0.084 Uiso 1 1 calc R . . C34 C 0.5056(4) 0.9556(2) 0.5325(4) 0.0535(17) Uani 1 1 d . . . C35 C 0.9374(4) 0.9493(3) 0.5966(5) 0.070(2) Uani 1 1 d . . . C36 C 0.9702(4) 0.9747(3) 0.5464(4) 0.068(2) Uani 1 1 d . . . C37 C 0.9734(4) 1.0248(3) 0.5493(4) 0.070(2) Uani 1 1 d . . . C38 C 0.9457(5) 1.0517(4) 0.5966(5) 0.083(3) Uani 1 1 d . . . H38 H 0.9248 1.0361 0.6271 0.100 Uiso 1 1 calc R . . C39 C 0.9489(5) 1.0992(4) 0.5983(6) 0.091(3) Uani 1 1 d . . . H39 H 0.9303 1.1159 0.6295 0.109 Uiso 1 1 calc R . . C40 C 1.0195(6) 0.8772(4) 0.4472(6) 0.105(4) Uani 1 1 d . . . H40 H 1.0155 0.8447 0.4445 0.126 Uiso 1 1 calc R . . C41 C 0.9946(5) 0.9001(4) 0.4949(6) 0.093(3) Uani 1 1 d . . . H41 H 0.9762 0.8829 0.5258 0.112 Uiso 1 1 calc R . . C42 C 0.9958(4) 0.9505(3) 0.4991(5) 0.073(2) Uani 1 1 d . . . N9 N 0.6914(4) 0.9779(3) 0.5575(4) 0.076(2) Uani 1 1 d . . . H9A H 0.6738 0.9543 0.5348 0.091 Uiso 1 1 calc R . . C44 C 0.6738(5) 1.0213(4) 0.5458(6) 0.101(4) Uani 1 1 d . . . H44 H 0.6404 1.0315 0.5124 0.121 Uiso 1 1 calc R . . C45 C 0.7115(6) 1.0493(4) 0.5898(6) 0.099(3) Uani 1 1 d . . . H45 H 0.7099 1.0818 0.5929 0.119 Uiso 1 1 calc R . . C46 C 0.7531(4) 1.0188(3) 0.6293(5) 0.074(2) Uani 1 1 d . . . C47 C 0.8069(5) 1.0275(3) 0.6868(5) 0.074(2) Uani 1 1 d . . . C48 C 0.8197(6) 1.0726(4) 0.7091(6) 0.103(4) Uani 1 1 d . . . H48 H 0.7948 1.0978 0.6898 0.124 Uiso 1 1 calc R . . C49 C 0.8700(8) 1.0790(6) 0.7605(6) 0.125(5) Uani 1 1 d . . . H49 H 0.8809 1.1091 0.7763 0.151 Uiso 1 1 calc R . . C50 C 0.9059(8) 1.0402(6) 0.7899(6) 0.127(5) Uani 1 1 d . . . H50 H 0.9390 1.0436 0.8266 0.153 Uiso 1 1 calc R . . C51 C 0.8898(6) 0.9970(4) 0.7620(5) 0.099(3) Uani 1 1 d . . . H51 H 0.9141 0.9711 0.7795 0.118 Uiso 1 1 calc R . . O1 O 0.7510(2) 0.87884(14) 0.5204(2) 0.0506(11) Uani 1 1 d . . . O2 O 0.7962(3) 0.84620(19) 0.6153(3) 0.0778(17) Uani 1 1 d . . . O3 O 0.6213(2) 0.91632(17) 0.4633(2) 0.0565(12) Uani 1 1 d . . . O4 O 0.5268(3) 0.8948(2) 0.4019(3) 0.0835(19) Uani 1 1 d . . . O5 O 0.8770(2) 0.93859(19) 0.5779(3) 0.0609(13) Uani 1 1 d . . . O6 O 0.9697(3) 0.9420(3) 0.6536(3) 0.109(3) Uani 1 1 d . . . N11 N 0.8836(5) 0.8796(3) 0.7461(4) 0.141(3) Uani 1 1 d GDU . . N12 N 0.9504(5) 0.8710(3) 0.7666(5) 0.167(4) Uani 1 1 d GDU . . H12A H 0.9819 0.8809 0.7475 0.200 Uiso 1 1 calc R . . C53 C 0.9573(5) 0.8436(4) 0.8232(6) 0.161(4) Uani 1 1 d GDU . . H53A H 0.9969 0.8328 0.8472 0.193 Uiso 1 1 calc R . . C54 C 0.8948(6) 0.8353(4) 0.8377(5) 0.154(4) Uani 1 1 d GDU . . H54A H 0.8852 0.8179 0.8732 0.185 Uiso 1 1 calc R . . C55 C 0.8493(4) 0.8575(3) 0.7901(5) 0.147(3) Uani 1 1 d GDU . . N10 N 0.7452(4) 0.8865(3) 0.7285(4) 0.113(3) Uani 1 1 d GDU . . C56 C 0.7773(3) 0.8603(3) 0.7816(5) 0.140(3) Uani 1 1 d GDU . . C57 C 0.7410(5) 0.8322(3) 0.8176(4) 0.157(4) Uani 1 1 d GDU . . H57A H 0.7625 0.8147 0.8531 0.188 Uiso 1 1 calc R . . C58 C 0.6726(5) 0.8303(3) 0.8006(5) 0.163(4) Uani 1 1 d GDU . . H58A H 0.6483 0.8115 0.8248 0.196 Uiso 1 1 calc R . . C59 C 0.6405(3) 0.8565(4) 0.7476(5) 0.139(4) Uani 1 1 d GDU . . H59A H 0.5947 0.8552 0.7362 0.166 Uiso 1 1 calc R . . C60 C 0.6768(4) 0.8846(3) 0.7115(4) 0.121(3) Uani 1 1 d GDU . . H60A H 0.6553 0.9021 0.6760 0.146 Uiso 1 1 calc R . . O7 O 0.5785(7) 0.7440(8) 0.9104(9) 0.350(9) Uani 1 1 d DU . . O8 O 0.5773(7) 0.7431(9) 1.0157(11) 0.385(10) Uani 1 1 d DU . . C61 C 0.6079(4) 0.7443(4) 0.9686(9) 0.321(7) Uani 1 1 d DU . . C62 C 0.6820(3) 0.7462(3) 0.9828(5) 0.291(6) Uani 1 1 d DU . . C63 C 0.7195(4) 0.7061(2) 0.9976(6) 0.271(6) Uani 1 1 d DU . . C64 C 0.6892(7) 0.6626(3) 0.9996(7) 0.264(7) Uani 1 1 d DU . . H64A H 0.6434 0.6602 0.9910 0.316 Uiso 1 1 calc R . . C65 C 0.7275(9) 0.6230(5) 1.0144(9) 0.258(8) Uani 1 1 d DU . . H65A H 0.7077 0.5935 1.0098 0.309 Uiso 1 1 calc R . . C66 C 0.7047(9) 0.8735(4) 0.9637(9) 0.294(9) Uani 1 1 d DU . . H66A H 0.6801 0.8998 0.9479 0.353 Uiso 1 1 calc R . . C67 C 0.6739(6) 0.8298(4) 0.9659(7) 0.296(7) Uani 1 1 d DU . . H67A H 0.6281 0.8275 0.9575 0.355 Uiso 1 1 calc R . . C68 C 0.7125(4) 0.7899(2) 0.9808(7) 0.292(7) Uani 1 1 d DU . . 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 0.0668(4) 0.0405(3) 0.0576(4) 0.0020(2) 0.0133(3) 0.0100(2) Cd2 0.1318(7) 0.0506(4) 0.0630(4) 0.0024(3) 0.0342(4) -0.0088(4) N1 0.085(5) 0.058(4) 0.058(4) 0.013(3) 0.023(3) 0.020(4) N2 0.077(5) 0.041(3) 0.064(4) -0.006(3) 0.013(3) 0.000(3) N4 0.067(4) 0.056(4) 0.048(3) -0.003(3) 0.009(3) 0.011(3) N5 0.054(3) 0.051(4) 0.048(3) 0.007(3) 0.010(3) 0.006(3) N8 0.079(5) 0.052(4) 0.074(4) -0.017(3) 0.032(4) -0.013(3) N7 0.121(7) 0.075(6) 0.058(4) -0.005(4) 0.028(4) -0.027(5) C1 0.090(7) 0.075(6) 0.079(6) 0.006(5) 0.031(5) 0.020(5) C2 0.103(8) 0.092(8) 0.108(8) 0.016(7) 0.043(7) 0.024(7) C3 0.142(12) 0.098(9) 0.124(9) 0.003(7) 0.065(9) 0.050(8) C4 0.122(9) 0.059(6) 0.100(7) -0.007(5) 0.048(6) 0.019(6) C5 0.116(8) 0.046(5) 0.067(5) 0.015(4) 0.037(5) 0.022(5) C6 0.119(8) 0.038(4) 0.056(4) 0.001(3) 0.016(5) 0.014(4) C7 0.150(10) 0.046(5) 0.074(6) -0.008(4) 0.036(6) 0.012(6) C8 0.126(9) 0.052(5) 0.074(6) -0.004(4) 0.018(6) -0.007(5) N3 0.088(5) 0.051(4) 0.072(4) -0.004(3) 0.012(4) 0.009(4) C10 0.084(6) 0.063(5) 0.053(4) 0.003(4) 0.010(4) -0.008(4) C11 0.078(6) 0.075(6) 0.064(5) 0.010(4) 0.000(4) -0.008(5) C12 0.079(6) 0.084(6) 0.056(5) 0.015(4) 0.009(4) 0.004(5) C13 0.073(5) 0.055(5) 0.047(4) 0.011(3) 0.012(4) 0.000(4) C14 0.059(4) 0.050(4) 0.052(4) 0.003(3) 0.024(3) 0.009(3) C15 0.061(4) 0.052(4) 0.052(4) 0.005(3) 0.015(3) 0.009(3) C16 0.094(6) 0.059(5) 0.066(5) 0.013(4) -0.009(4) -0.023(5) C17 0.099(7) 0.063(6) 0.075(6) 0.013(4) -0.010(5) -0.021(5) N6 0.065(4) 0.054(4) 0.052(3) 0.010(3) 0.009(3) -0.002(3) C19 0.063(5) 0.047(4) 0.063(5) 0.007(3) 0.023(4) -0.004(3) C20 0.082(5) 0.031(4) 0.067(5) 0.007(3) 0.022(4) 0.002(4) C21 0.063(5) 0.039(4) 0.065(4) 0.018(3) 0.015(3) -0.001(3) C22 0.074(5) 0.046(4) 0.072(5) 0.019(4) 0.015(4) 0.010(4) C23 0.065(5) 0.058(5) 0.094(6) 0.021(4) 0.025(4) 0.002(4) C24 0.066(5) 0.057(5) 0.108(7) 0.025(5) 0.013(5) -0.007(4) C25 0.071(5) 0.039(4) 0.083(5) 0.017(4) 0.013(4) -0.009(4) C26 0.076(5) 0.035(4) 0.064(4) 0.014(3) 0.024(4) -0.004(3) C27 0.058(5) 0.049(4) 0.059(4) -0.005(3) 0.003(3) 0.005(3) C28 0.045(4) 0.046(4) 0.061(4) -0.003(3) 0.007(3) 0.004(3) C29 0.047(4) 0.053(4) 0.060(4) -0.001(3) 0.010(3) -0.001(3) C30 0.082(6) 0.073(6) 0.060(5) -0.004(4) 0.022(4) 0.007(4) C31 0.112(8) 0.086(7) 0.067(5) 0.011(5) 0.036(5) 0.021(6) C32 0.109(7) 0.066(6) 0.088(6) 0.025(5) 0.039(6) 0.019(5) C33 0.080(6) 0.043(4) 0.094(6) 0.008(4) 0.030(5) 0.011(4) C34 0.056(4) 0.044(4) 0.061(4) 0.000(3) 0.012(3) 0.016(3) C35 0.064(5) 0.064(5) 0.085(6) 0.008(4) 0.018(4) -0.010(4) C36 0.061(5) 0.074(6) 0.065(5) 0.002(4) 0.004(4) -0.008(4) C37 0.061(5) 0.082(6) 0.065(5) 0.005(4) 0.008(4) -0.011(4) C38 0.076(6) 0.097(8) 0.079(6) 0.007(5) 0.021(5) -0.005(5) C39 0.099(7) 0.071(7) 0.112(8) 0.001(6) 0.049(6) -0.005(6) C40 0.112(9) 0.094(8) 0.123(9) -0.007(7) 0.059(8) -0.004(6) C41 0.085(7) 0.083(7) 0.118(8) 0.009(6) 0.032(6) -0.016(6) C42 0.066(5) 0.075(6) 0.077(5) 0.006(5) 0.010(4) -0.013(4) N9 0.065(4) 0.072(5) 0.095(5) -0.027(4) 0.027(4) -0.007(4) C44 0.074(6) 0.076(7) 0.142(10) -0.030(7) -0.009(6) 0.006(5) C45 0.104(8) 0.051(6) 0.135(9) -0.022(6) -0.002(7) -0.004(5) C46 0.071(5) 0.062(6) 0.092(6) -0.009(5) 0.027(5) -0.003(4) C47 0.090(6) 0.058(5) 0.084(6) -0.014(5) 0.040(5) -0.015(5) C48 0.108(8) 0.092(8) 0.111(8) -0.045(7) 0.023(7) -0.014(6) C49 0.152(12) 0.132(12) 0.087(8) -0.047(8) 0.005(8) -0.029(10) C50 0.148(12) 0.151(13) 0.070(7) -0.014(8) -0.020(7) -0.046(10) C51 0.140(10) 0.084(7) 0.072(6) -0.004(5) 0.017(6) -0.022(7) O1 0.060(3) 0.029(2) 0.063(3) 0.005(2) 0.010(2) 0.002(2) O2 0.121(5) 0.046(3) 0.065(4) 0.014(3) 0.012(3) 0.004(3) O3 0.059(3) 0.048(3) 0.062(3) -0.006(2) 0.009(2) 0.011(2) O4 0.074(4) 0.072(4) 0.095(4) -0.033(3) -0.013(3) 0.025(3) O5 0.050(3) 0.065(3) 0.067(3) 0.011(3) 0.007(2) -0.015(2) O6 0.074(4) 0.175(8) 0.072(4) 0.031(5) -0.003(3) -0.021(5) N11 0.156(6) 0.130(6) 0.134(6) 0.007(5) 0.012(5) 0.005(5) N12 0.178(6) 0.158(6) 0.161(6) 0.010(5) 0.019(6) -0.002(6) C53 0.175(7) 0.153(7) 0.149(6) 0.007(6) 0.011(6) 0.005(6) C54 0.175(7) 0.148(6) 0.136(6) 0.006(6) 0.015(6) 0.008(6) C55 0.164(6) 0.142(6) 0.132(5) -0.004(5) 0.020(5) 0.006(5) N10 0.132(5) 0.109(5) 0.108(5) 0.008(4) 0.048(4) 0.010(4) C56 0.157(6) 0.141(6) 0.127(5) -0.005(5) 0.042(5) -0.010(5) C57 0.175(7) 0.155(6) 0.145(6) 0.000(6) 0.037(6) -0.020(6) C58 0.171(7) 0.160(7) 0.162(6) -0.014(6) 0.037(6) -0.015(6) C59 0.151(6) 0.125(6) 0.146(6) -0.016(5) 0.043(5) -0.009(5) C60 0.138(6) 0.106(6) 0.127(6) -0.010(5) 0.044(5) -0.001(5) O7 0.341(12) 0.354(12) 0.352(12) -0.003(9) 0.051(9) -0.007(9) O8 0.378(12) 0.390(12) 0.390(12) -0.005(9) 0.070(9) 0.002(9) C61 0.318(9) 0.326(9) 0.321(9) 0.002(7) 0.059(7) -0.011(7) C62 0.287(8) 0.293(8) 0.295(8) 0.003(6) 0.052(6) -0.005(6) C63 0.270(8) 0.269(9) 0.275(8) 0.002(7) 0.051(7) -0.012(7) C64 0.258(9) 0.266(9) 0.268(9) 0.003(7) 0.050(7) -0.014(7) C65 0.254(10) 0.261(10) 0.262(10) 0.001(8) 0.053(8) -0.013(8) C66 0.300(11) 0.291(11) 0.292(11) 0.000(8) 0.049(8) -0.001(8) C67 0.300(9) 0.289(10) 0.296(9) -0.001(7) 0.045(7) 0.003(7) C68 0.293(9) 0.288(9) 0.294(8) 0.001(7) 0.048(7) 0.002(7) _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 O3 2.249(5) . ? Cd1 O1 2.292(5) . ? Cd1 N2 2.303(6) . ? Cd1 N5 2.326(6) . ? Cd1 N1 2.333(7) . ? Cd1 N4 2.404(6) . ? Cd2 O2 2.215(6) . ? Cd2 O5 2.270(5) . ? Cd2 N8 2.330(8) . ? Cd2 N11 2.372(8) . ? Cd2 N7 2.383(8) . ? Cd2 N10 2.425(6) . ? N1 C1 1.325(11) . ? N1 C5 1.365(11) . ? N2 N3 1.319(9) . ? N2 C6 1.329(10) . ? N4 C10 1.325(10) . ? N4 C14 1.352(9) . ? N5 C15 1.348(9) . ? N5 N6 1.352(8) . ? N8 C46 1.331(10) . ? N8 N9 1.355(10) . ? N7 C51 1.317(13) . ? N7 C47 1.322(12) . ? C1 C2 1.376(14) . ? C1 H1 0.9300 . ? C2 C3 1.411(17) . ? C2 H2 0.9300 . ? C3 C4 1.339(16) . ? C3 H3 0.9300 . ? C4 C5 1.393(12) . ? C4 H4 0.9300 . ? C5 C6 1.460(13) . ? C6 C7 1.403(13) . ? C7 C8 1.373(15) . ? C7 H7 0.9300 . ? C8 N3 1.357(11) . ? C8 H8 0.9300 . ? N3 H3A 0.8600 . ? C10 C11 1.369(11) . ? C10 H10 0.9300 . ? C11 C12 1.355(12) . ? C11 H11 0.9300 . ? C12 C13 1.368(11) . ? C12 H12 0.9300 . ? C13 C14 1.371(10) . ? C13 H13 0.9300 . ? C14 C15 1.485(11) . ? C15 C16 1.375(11) . ? C16 C17 1.343(12) . ? C16 H16 0.9300 . ? C17 N6 1.318(10) . ? C17 H17 0.9300 . ? N6 H6A 0.8600 . ? C19 O2 1.246(9) . ? C19 O1 1.252(8) . ? C19 C20 1.513(10) . ? C20 C26 1.404(11) . ? C20 C21 1.411(10) . ? C21 C22 1.425(11) . ? C21 C26 1.446(10) 7_666 ? C22 C23 1.379(11) . ? C22 H22 0.9300 . ? C23 C24 1.367(12) 7_666 ? C23 H23 0.9300 . ? C24 C23 1.367(12) 7_666 ? C24 C25 1.370(12) . ? C24 H24 0.9300 . ? C25 C26 1.421(11) . ? C25 H25 0.9300 . ? C26 C21 1.446(10) 7_666 ? C27 O4 1.217(9) . ? C27 O3 1.276(8) . ? C27 C28 1.525(10) . ? C28 C29 1.393(10) . ? C28 C34 1.398(10) . ? C29 C34 1.436(10) 5_676 ? C29 C30 1.451(11) . ? C30 C31 1.359(12) . ? C30 H30 0.9300 . ? C31 C32 1.406(13) 5_676 ? C31 H31 0.9300 . ? C32 C33 1.347(12) . ? C32 C31 1.406(13) 5_676 ? C32 H32 0.9300 . ? C33 C34 1.398(10) . ? C33 H33 0.9300 . ? C34 C29 1.436(10) 5_676 ? C35 O6 1.259(11) . ? C35 O5 1.271(9) . ? C35 C36 1.509(12) . ? C36 C42 1.366(13) . ? C36 C37 1.431(12) . ? C37 C38 1.426(13) . ? C37 C42 1.447(12) 5_776 ? C38 C39 1.356(14) . ? C38 H38 0.9300 . ? C39 C40 1.398(14) 5_776 ? C39 H39 0.9300 . ? C40 C41 1.346(15) . ? C40 C39 1.398(14) 5_776 ? C40 H40 0.9300 . ? C41 C42 1.440(14) . ? C41 H41 0.9300 . ? C42 C37 1.447(12) 5_776 ? N9 C44 1.299(13) . ? N9 H9A 0.8600 . ? C44 C45 1.346(14) . ? C44 H44 0.9300 . ? C45 C46 1.381(14) . ? C45 H45 0.9300 . ? C46 C47 1.495(14) . ? C47 C48 1.375(13) . ? C48 C49 1.358(17) . ? C48 H48 0.9300 . ? C49 C50 1.405(19) . ? C49 H49 0.9300 . ? C50 C51 1.374(17) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? N11 C55 1.386(6) . ? N11 N12 1.386(6) . ? N12 C53 1.386(6) . ? N12 H12A 0.8600 . ? C53 C54 1.386(6) . ? C53 H53A 0.9300 . ? C54 C55 1.386(6) . ? C54 H54A 0.9300 . ? C55 C56 1.462(8) . ? N10 C56 1.3900 . ? N10 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C57 H57A 0.9300 . ? C58 C59 1.3900 . ? C58 H58A 0.9300 . ? C59 C60 1.3900 . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? O7 C61 1.244(9) . ? O8 C61 1.241(9) . ? C61 C62 1.501(7) . ? C62 C63 1.381(7) . ? C62 C68 1.398(7) . ? C63 C64 1.391(8) . ? C63 C68 1.397(8) 7_667 ? C64 C65 1.380(10) . ? C64 H64A 0.9300 . ? C65 C66 1.394(10) 7_667 ? C65 H65A 0.9300 . ? C66 C65 1.394(10) 7_667 ? C66 C67 1.399(8) . ? C66 H66A 0.9300 . ? C67 C68 1.391(7) . ? C67 H67A 0.9300 . ? C68 C63 1.397(8) 7_667 ? 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 Cd1 O1 80.16(17) . . ? O3 Cd1 N2 97.7(2) . . ? O1 Cd1 N2 122.10(19) . . ? O3 Cd1 N5 94.66(19) . . ? O1 Cd1 N5 81.27(18) . . ? N2 Cd1 N5 155.1(2) . . ? O3 Cd1 N1 164.9(2) . . ? O1 Cd1 N1 96.8(2) . . ? N2 Cd1 N1 71.2(3) . . ? N5 Cd1 N1 99.5(2) . . ? O3 Cd1 N4 90.88(19) . . ? O1 Cd1 N4 148.97(19) . . ? N2 Cd1 N4 88.4(2) . . ? N5 Cd1 N4 69.8(2) . . ? N1 Cd1 N4 98.8(2) . . ? O2 Cd2 O5 93.7(2) . . ? O2 Cd2 N8 114.6(2) . . ? O5 Cd2 N8 86.4(2) . . ? O2 Cd2 N11 85.4(3) . . ? O5 Cd2 N11 110.8(3) . . ? N8 Cd2 N11 153.3(3) . . ? O2 Cd2 N7 173.6(2) . . ? O5 Cd2 N7 90.6(2) . . ? N8 Cd2 N7 70.3(3) . . ? N11 Cd2 N7 88.7(3) . . ? O2 Cd2 N10 78.4(2) . . ? O5 Cd2 N10 171.6(2) . . ? N8 Cd2 N10 94.3(3) . . ? N11 Cd2 N10 71.7(4) . . ? N7 Cd2 N10 97.4(3) . . ? C1 N1 C5 118.8(8) . . ? C1 N1 Cd1 124.6(6) . . ? C5 N1 Cd1 116.5(6) . . ? N3 N2 C6 106.8(7) . . ? N3 N2 Cd1 135.7(5) . . ? C6 N2 Cd1 117.5(6) . . ? C10 N4 C14 116.1(7) . . ? C10 N4 Cd1 126.2(5) . . ? C14 N4 Cd1 117.4(5) . . ? C15 N5 N6 104.6(6) . . ? C15 N5 Cd1 118.4(5) . . ? N6 N5 Cd1 136.6(4) . . ? C46 N8 N9 104.4(7) . . ? C46 N8 Cd2 117.3(6) . . ? N9 N8 Cd2 137.0(5) . . ? C51 N7 C47 118.4(9) . . ? C51 N7 Cd2 124.7(8) . . ? C47 N7 Cd2 116.8(6) . . ? N1 C1 C2 122.8(11) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 117.9(11) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 120.0(10) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.3(11) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.1(10) . . ? N1 C5 C6 116.1(7) . . ? C4 C5 C6 122.8(10) . . ? N2 C6 C7 109.0(9) . . ? N2 C6 C5 118.7(8) . . ? C7 C6 C5 132.3(8) . . ? C8 C7 C6 106.5(8) . . ? C8 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N3 C8 C7 105.1(9) . . ? N3 C8 H8 127.5 . . ? C7 C8 H8 127.5 . . ? N2 N3 C8 112.6(8) . . ? N2 N3 H3A 123.7 . . ? C8 N3 H3A 123.7 . . ? N4 C10 C11 124.8(8) . . ? N4 C10 H10 117.6 . . ? C11 C10 H10 117.6 . . ? C12 C11 C10 117.8(8) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C13 119.8(8) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 118.8(8) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N4 C14 C13 122.6(7) . . ? N4 C14 C15 115.3(6) . . ? C13 C14 C15 122.1(7) . . ? N5 C15 C16 110.9(7) . . ? N5 C15 C14 118.6(7) . . ? C16 C15 C14 130.4(7) . . ? C17 C16 C15 104.3(7) . . ? C17 C16 H16 127.9 . . ? C15 C16 H16 127.9 . . ? N6 C17 C16 110.1(8) . . ? N6 C17 H17 125.0 . . ? C16 C17 H17 125.0 . . ? C17 N6 N5 110.1(6) . . ? C17 N6 H6A 125.0 . . ? N5 N6 H6A 125.0 . . ? O2 C19 O1 125.0(7) . . ? O2 C19 C20 115.9(7) . . ? O1 C19 C20 119.1(7) . . ? C26 C20 C21 122.0(7) . . ? C26 C20 C19 119.2(7) . . ? C21 C20 C19 118.9(7) . . ? C20 C21 C22 123.1(7) . . ? C20 C21 C26 118.7(7) . 7_666 ? C22 C21 C26 118.2(7) . 7_666 ? C23 C22 C21 120.9(8) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.8(8) 7_666 . ? C24 C23 H23 119.6 7_666 . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.9(8) 7_666 . ? C23 C24 H24 119.5 7_666 . ? C25 C24 H24 119.5 . . ? C24 C25 C26 121.7(8) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C20 C26 C25 123.2(7) . . ? C20 C26 C21 119.3(7) . 7_666 ? C25 C26 C21 117.5(7) . 7_666 ? O4 C27 O3 125.1(7) . . ? O4 C27 C28 120.9(7) . . ? O3 C27 C28 114.0(6) . . ? C29 C28 C34 122.2(6) . . ? C29 C28 C27 119.0(6) . . ? C34 C28 C27 118.8(6) . . ? C28 C29 C34 119.9(6) . 5_676 ? C28 C29 C30 122.8(7) . . ? C34 C29 C30 117.3(7) 5_676 . ? C31 C30 C29 121.3(8) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.1(8) . 5_676 ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 5_676 . ? C33 C32 C31 121.9(8) . 5_676 ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 5_676 . ? C32 C33 C34 121.3(8) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C28 123.0(7) . . ? C33 C34 C29 119.0(7) . 5_676 ? C28 C34 C29 117.9(6) . 5_676 ? O6 C35 O5 125.1(8) . . ? O6 C35 C36 119.1(8) . . ? O5 C35 C36 115.7(8) . . ? C42 C36 C37 120.8(8) . . ? C42 C36 C35 121.0(8) . . ? C37 C36 C35 118.1(8) . . ? C38 C37 C36 122.9(8) . . ? C38 C37 C42 118.6(9) . 5_776 ? C36 C37 C42 118.5(8) . 5_776 ? C39 C38 C37 122.0(9) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 119.3(10) . 5_776 ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 5_776 . ? C41 C40 C39 122.0(11) . 5_776 ? C41 C40 H40 119.0 . . ? C39 C40 H40 119.0 5_776 . ? C40 C41 C42 121.5(10) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C36 C42 C41 122.7(9) . . ? C36 C42 C37 120.6(9) . 5_776 ? C41 C42 C37 116.6(9) . 5_776 ? C44 N9 N8 111.2(8) . . ? C44 N9 H9A 124.4 . . ? N8 N9 H9A 124.4 . . ? N9 C44 C45 109.2(10) . . ? N9 C44 H44 125.4 . . ? C45 C44 H44 125.4 . . ? C44 C45 C46 104.4(9) . . ? C44 C45 H45 127.8 . . ? C46 C45 H45 127.8 . . ? N8 C46 C45 110.8(9) . . ? N8 C46 C47 118.0(9) . . ? C45 C46 C47 131.3(9) . . ? N7 C47 C48 123.8(10) . . ? N7 C47 C46 116.7(8) . . ? C48 C47 C46 119.5(10) . . ? C49 C48 C47 117.4(13) . . ? C49 C48 H48 121.3 . . ? C47 C48 H48 121.3 . . ? C48 C49 C50 120.3(12) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 116.9(11) . . ? C51 C50 H50 121.6 . . ? C49 C50 H50 121.6 . . ? N7 C51 C50 123.2(12) . . ? N7 C51 H51 118.4 . . ? C50 C51 H51 118.4 . . ? C19 O1 Cd1 129.9(5) . . ? C19 O2 Cd2 115.9(5) . . ? C27 O3 Cd1 128.3(5) . . ? C35 O5 Cd2 118.1(5) . . ? C55 N11 N12 108.0 . . ? C55 N11 Cd2 115.0(7) . . ? N12 N11 Cd2 137.0(7) . . ? C53 N12 N11 108.0 . . ? C53 N12 H12A 126.0 . . ? N11 N12 H12A 126.0 . . ? C54 C53 N12 108.0 . . ? C54 C53 H53A 126.0 . . ? N12 C53 H53A 126.0 . . ? C55 C54 C53 108.0 . . ? C55 C54 H54A 126.0 . . ? C53 C54 H54A 126.0 . . ? N11 C55 C54 108.0 . . ? N11 C55 C56 120.9(10) . . ? C54 C55 C56 131.1(10) . . ? C56 N10 C60 120.0 . . ? C56 N10 Cd2 114.9(5) . . ? C60 N10 Cd2 123.4(5) . . ? N10 C56 C57 120.0 . . ? N10 C56 C55 117.3(8) . . ? C57 C56 C55 121.9(8) . . ? C58 C57 C56 120.0 . . ? C58 C57 H57A 120.0 . . ? C56 C57 H57A 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C59 C60 N10 120.0 . . ? C59 C60 H60A 120.0 . . ? N10 C60 H60A 120.0 . . ? O8 C61 O7 121.4(9) . . ? O8 C61 C62 118.7(9) . . ? O7 C61 C62 119.9(9) . . ? C63 C62 C68 120.5(7) . . ? C63 C62 C61 121.4(7) . . ? C68 C62 C61 118.1(6) . . ? C62 C63 C64 120.5(7) . . ? C62 C63 C68 119.5(6) . 7_667 ? C64 C63 C68 119.4(6) . 7_667 ? C65 C64 C63 119.7(8) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C64 C65 C66 120.8(8) . 7_667 ? C64 C65 H65A 119.6 . . ? C66 C65 H65A 119.6 7_667 . ? C65 C66 C67 119.1(7) 7_667 . ? C65 C66 H66A 120.4 7_667 . ? C67 C66 H66A 120.4 . . ? C68 C67 C66 119.4(7) . . ? C68 C67 H67A 120.3 . . ? C66 C67 H67A 120.3 . . ? C67 C68 C63 120.3(6) . 7_667 ? C67 C68 C62 119.6(7) . . ? C63 C68 C62 119.5(6) 7_667 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cd1 N1 C1 -135.2(8) . . . . ? O1 Cd1 N1 C1 -57.7(7) . . . . ? N2 Cd1 N1 C1 -179.3(7) . . . . ? N5 Cd1 N1 C1 24.6(7) . . . . ? N4 Cd1 N1 C1 95.5(7) . . . . ? O3 Cd1 N1 C5 42.5(11) . . . . ? O1 Cd1 N1 C5 120.0(5) . . . . ? N2 Cd1 N1 C5 -1.6(5) . . . . ? N5 Cd1 N1 C5 -157.7(5) . . . . ? N4 Cd1 N1 C5 -86.8(5) . . . . ? O3 Cd1 N2 N3 10.2(7) . . . . ? O1 Cd1 N2 N3 93.4(7) . . . . ? N5 Cd1 N2 N3 -109.0(8) . . . . ? N1 Cd1 N2 N3 179.6(8) . . . . ? N4 Cd1 N2 N3 -80.5(7) . . . . ? O3 Cd1 N2 C6 -168.4(5) . . . . ? O1 Cd1 N2 C6 -85.2(6) . . . . ? N5 Cd1 N2 C6 72.5(8) . . . . ? N1 Cd1 N2 C6 1.1(5) . . . . ? N4 Cd1 N2 C6 100.9(6) . . . . ? O3 Cd1 N4 C10 -85.0(6) . . . . ? O1 Cd1 N4 C10 -157.2(6) . . . . ? N2 Cd1 N4 C10 12.7(6) . . . . ? N5 Cd1 N4 C10 -179.7(7) . . . . ? N1 Cd1 N4 C10 83.4(7) . . . . ? O3 Cd1 N4 C14 89.2(5) . . . . ? O1 Cd1 N4 C14 17.1(7) . . . . ? N2 Cd1 N4 C14 -173.1(5) . . . . ? N5 Cd1 N4 C14 -5.4(5) . . . . ? N1 Cd1 N4 C14 -102.4(5) . . . . ? O3 Cd1 N5 C15 -83.6(5) . . . . ? O1 Cd1 N5 C15 -162.9(5) . . . . ? N2 Cd1 N5 C15 36.1(8) . . . . ? N1 Cd1 N5 C15 101.6(5) . . . . ? N4 Cd1 N5 C15 5.6(5) . . . . ? O3 Cd1 N5 N6 88.0(6) . . . . ? O1 Cd1 N5 N6 8.7(6) . . . . ? N2 Cd1 N5 N6 -152.3(6) . . . . ? N1 Cd1 N5 N6 -86.9(6) . . . . ? N4 Cd1 N5 N6 177.2(7) . . . . ? O2 Cd2 N8 C46 -175.7(6) . . . . ? O5 Cd2 N8 C46 -83.2(6) . . . . ? N11 Cd2 N8 C46 48.6(10) . . . . ? N7 Cd2 N8 C46 8.7(6) . . . . ? N10 Cd2 N8 C46 105.1(6) . . . . ? O2 Cd2 N8 N9 -11.4(8) . . . . ? O5 Cd2 N8 N9 81.0(7) . . . . ? N11 Cd2 N8 N9 -147.1(8) . . . . ? N7 Cd2 N8 N9 173.0(8) . . . . ? N10 Cd2 N8 N9 -90.6(7) . . . . ? O2 Cd2 N7 C51 37(3) . . . . ? O5 Cd2 N7 C51 -95.7(8) . . . . ? N8 Cd2 N7 C51 178.3(8) . . . . ? N11 Cd2 N7 C51 15.1(8) . . . . ? N10 Cd2 N7 C51 86.5(8) . . . . ? O2 Cd2 N7 C47 -148(2) . . . . ? O5 Cd2 N7 C47 79.4(6) . . . . ? N8 Cd2 N7 C47 -6.5(6) . . . . ? N11 Cd2 N7 C47 -169.8(7) . . . . ? N10 Cd2 N7 C47 -98.4(6) . . . . ? C5 N1 C1 C2 -0.4(13) . . . . ? Cd1 N1 C1 C2 177.3(7) . . . . ? N1 C1 C2 C3 -0.5(15) . . . . ? C1 C2 C3 C4 2.3(17) . . . . ? C2 C3 C4 C5 -3.0(17) . . . . ? C1 N1 C5 C4 -0.4(12) . . . . ? Cd1 N1 C5 C4 -178.2(6) . . . . ? C1 N1 C5 C6 179.8(7) . . . . ? Cd1 N1 C5 C6 2.0(9) . . . . ? C3 C4 C5 N1 2.1(14) . . . . ? C3 C4 C5 C6 -178.1(9) . . . . ? N3 N2 C6 C7 -0.3(9) . . . . ? Cd1 N2 C6 C7 178.7(5) . . . . ? N3 N2 C6 C5 -179.4(7) . . . . ? Cd1 N2 C6 C5 -0.4(9) . . . . ? N1 C5 C6 N2 -1.0(11) . . . . ? C4 C5 C6 N2 179.1(8) . . . . ? N1 C5 C6 C7 -179.9(8) . . . . ? C4 C5 C6 C7 0.2(14) . . . . ? N2 C6 C7 C8 -0.4(10) . . . . ? C5 C6 C7 C8 178.6(9) . . . . ? C6 C7 C8 N3 0.8(10) . . . . ? C6 N2 N3 C8 0.8(9) . . . . ? Cd1 N2 N3 C8 -177.8(6) . . . . ? C7 C8 N3 N2 -1.1(10) . . . . ? C14 N4 C10 C11 -1.8(12) . . . . ? Cd1 N4 C10 C11 172.5(7) . . . . ? N4 C10 C11 C12 2.8(14) . . . . ? C10 C11 C12 C13 -2.9(14) . . . . ? C11 C12 C13 C14 2.2(13) . . . . ? C10 N4 C14 C13 1.0(10) . . . . ? Cd1 N4 C14 C13 -173.8(5) . . . . ? C10 N4 C14 C15 179.5(6) . . . . ? Cd1 N4 C14 C15 4.7(7) . . . . ? C12 C13 C14 N4 -1.3(11) . . . . ? C12 C13 C14 C15 -179.7(7) . . . . ? N6 N5 C15 C16 0.2(8) . . . . ? Cd1 N5 C15 C16 174.2(6) . . . . ? N6 N5 C15 C14 -179.5(6) . . . . ? Cd1 N5 C15 C14 -5.5(8) . . . . ? N4 C14 C15 N5 0.4(9) . . . . ? C13 C14 C15 N5 178.9(6) . . . . ? N4 C14 C15 C16 -179.2(8) . . . . ? C13 C14 C15 C16 -0.7(13) . . . . ? N5 C15 C16 C17 0.4(11) . . . . ? C14 C15 C16 C17 -179.9(8) . . . . ? C15 C16 C17 N6 -0.9(12) . . . . ? C16 C17 N6 N5 1.1(11) . . . . ? C15 N5 N6 C17 -0.8(8) . . . . ? Cd1 N5 N6 C17 -173.1(6) . . . . ? O2 C19 C20 C26 -71.8(9) . . . . ? O1 C19 C20 C26 105.6(8) . . . . ? O2 C19 C20 C21 107.2(8) . . . . ? O1 C19 C20 C21 -75.3(9) . . . . ? C26 C20 C21 C22 178.2(7) . . . . ? C19 C20 C21 C22 -0.9(11) . . . . ? C26 C20 C21 C26 -1.8(11) . . . 7_666 ? C19 C20 C21 C26 179.2(6) . . . 7_666 ? C20 C21 C22 C23 179.5(7) . . . . ? C26 C21 C22 C23 -0.6(11) 7_666 . . . ? C21 C22 C23 C24 0.2(12) . . . 7_666 ? C23 C24 C25 C26 -0.1(13) 7_666 . . . ? C21 C20 C26 C25 -179.3(7) . . . . ? C19 C20 C26 C25 -0.3(11) . . . . ? C21 C20 C26 C21 1.8(12) . . . 7_666 ? C19 C20 C26 C21 -179.2(6) . . . 7_666 ? C24 C25 C26 C20 -178.4(8) . . . . ? C24 C25 C26 C21 0.5(11) . . . 7_666 ? O4 C27 C28 C29 -86.6(10) . . . . ? O3 C27 C28 C29 92.9(8) . . . . ? O4 C27 C28 C34 94.4(9) . . . . ? O3 C27 C28 C34 -86.1(9) . . . . ? C34 C28 C29 C34 1.3(12) . . . 5_676 ? C27 C28 C29 C34 -177.8(6) . . . 5_676 ? C34 C28 C29 C30 178.4(7) . . . . ? C27 C28 C29 C30 -0.6(11) . . . . ? C28 C29 C30 C31 -177.3(9) . . . . ? C34 C29 C30 C31 -0.1(12) 5_676 . . . ? C29 C30 C31 C32 -0.5(15) . . . 5_676 ? C31 C32 C33 C34 0.2(16) 5_676 . . . ? C32 C33 C34 C28 -178.6(9) . . . . ? C32 C33 C34 C29 0.4(13) . . . 5_676 ? C29 C28 C34 C33 177.8(8) . . . . ? C27 C28 C34 C33 -3.2(11) . . . . ? C29 C28 C34 C29 -1.2(11) . . . 5_676 ? C27 C28 C34 C29 177.8(6) . . . 5_676 ? O6 C35 C36 C42 99.1(11) . . . . ? O5 C35 C36 C42 -83.6(11) . . . . ? O6 C35 C36 C37 -81.3(12) . . . . ? O5 C35 C36 C37 96.1(10) . . . . ? C42 C36 C37 C38 178.2(8) . . . . ? C35 C36 C37 C38 -1.5(12) . . . . ? C42 C36 C37 C42 0.3(14) . . . 5_776 ? C35 C36 C37 C42 -179.3(7) . . . 5_776 ? C36 C37 C38 C39 -179.6(9) . . . . ? C42 C37 C38 C39 -1.8(14) 5_776 . . . ? C37 C38 C39 C40 -0.3(16) . . . 5_776 ? C39 C40 C41 C42 3.7(19) 5_776 . . . ? C37 C36 C42 C41 179.1(8) . . . . ? C35 C36 C42 C41 -1.3(13) . . . . ? C37 C36 C42 C37 -0.3(14) . . . 5_776 ? C35 C36 C42 C37 179.3(8) . . . 5_776 ? C40 C41 C42 C36 179.1(11) . . . . ? C40 C41 C42 C37 -1.5(15) . . . 5_776 ? C46 N8 N9 C44 -0.6(10) . . . . ? Cd2 N8 N9 C44 -166.2(7) . . . . ? N8 N9 C44 C45 0.7(13) . . . . ? N9 C44 C45 C46 -0.5(14) . . . . ? N9 N8 C46 C45 0.3(10) . . . . ? Cd2 N8 C46 C45 169.3(7) . . . . ? N9 N8 C46 C47 -179.2(7) . . . . ? Cd2 N8 C46 C47 -10.2(10) . . . . ? C44 C45 C46 N8 0.1(13) . . . . ? C44 C45 C46 C47 179.5(10) . . . . ? C51 N7 C47 C48 2.0(14) . . . . ? Cd2 N7 C47 C48 -173.4(8) . . . . ? C51 N7 C47 C46 179.3(8) . . . . ? Cd2 N7 C47 C46 3.9(10) . . . . ? N8 C46 C47 N7 4.1(12) . . . . ? C45 C46 C47 N7 -175.2(10) . . . . ? N8 C46 C47 C48 -178.4(9) . . . . ? C45 C46 C47 C48 2.2(16) . . . . ? N7 C47 C48 C49 -1.2(16) . . . . ? C46 C47 C48 C49 -178.5(10) . . . . ? C47 C48 C49 C50 -2(2) . . . . ? C48 C49 C50 C51 3(2) . . . . ? C47 N7 C51 C50 0.1(16) . . . . ? Cd2 N7 C51 C50 175.1(9) . . . . ? C49 C50 C51 N7 -3(2) . . . . ? O2 C19 O1 Cd1 -178.3(5) . . . . ? C20 C19 O1 Cd1 4.5(10) . . . . ? O3 Cd1 O1 C19 116.4(6) . . . . ? N2 Cd1 O1 C19 23.4(7) . . . . ? N5 Cd1 O1 C19 -147.3(6) . . . . ? N1 Cd1 O1 C19 -48.6(6) . . . . ? N4 Cd1 O1 C19 -168.5(5) . . . . ? O1 C19 O2 Cd2 -1.4(10) . . . . ? C20 C19 O2 Cd2 175.8(5) . . . . ? O5 Cd2 O2 C19 -57.1(6) . . . . ? N8 Cd2 O2 C19 30.6(6) . . . . ? N11 Cd2 O2 C19 -167.7(6) . . . . ? N7 Cd2 O2 C19 170(2) . . . . ? N10 Cd2 O2 C19 120.0(6) . . . . ? O4 C27 O3 Cd1 24.3(12) . . . . ? C28 C27 O3 Cd1 -155.1(5) . . . . ? O1 Cd1 O3 C27 -158.1(6) . . . . ? N2 Cd1 O3 C27 -36.8(6) . . . . ? N5 Cd1 O3 C27 121.6(6) . . . . ? N1 Cd1 O3 C27 -78.5(10) . . . . ? N4 Cd1 O3 C27 51.7(6) . . . . ? O6 C35 O5 Cd2 12.5(13) . . . . ? C36 C35 O5 Cd2 -164.7(6) . . . . ? O2 Cd2 O5 C35 -118.3(6) . . . . ? N8 Cd2 O5 C35 127.3(6) . . . . ? N11 Cd2 O5 C35 -31.8(7) . . . . ? N7 Cd2 O5 C35 57.0(6) . . . . ? N10 Cd2 O5 C35 -138.1(17) . . . . ? O2 Cd2 N11 C55 -75.8(5) . . . . ? O5 Cd2 N11 C55 -168.1(5) . . . . ? N8 Cd2 N11 C55 64.6(9) . . . . ? N7 Cd2 N11 C55 101.8(5) . . . . ? N10 Cd2 N11 C55 3.5(5) . . . . ? O2 Cd2 N11 N12 100.5(5) . . . . ? O5 Cd2 N11 N12 8.2(6) . . . . ? N8 Cd2 N11 N12 -119.1(7) . . . . ? N7 Cd2 N11 N12 -81.9(6) . . . . ? N10 Cd2 N11 N12 179.8(6) . . . . ? C55 N11 N12 C53 0.0 . . . . ? Cd2 N11 N12 C53 -176.5(9) . . . . ? N11 N12 C53 C54 0.0 . . . . ? N12 C53 C54 C55 0.0 . . . . ? N12 N11 C55 C54 0.0 . . . . ? Cd2 N11 C55 C54 177.3(6) . . . . ? N12 N11 C55 C56 179.9(3) . . . . ? Cd2 N11 C55 C56 -2.7(7) . . . . ? C53 C54 C55 N11 0.0 . . . . ? C53 C54 C55 C56 -179.9(3) . . . . ? O2 Cd2 N10 C56 84.9(4) . . . . ? O5 Cd2 N10 C56 105.0(18) . . . . ? N8 Cd2 N10 C56 -160.9(4) . . . . ? N11 Cd2 N10 C56 -4.1(4) . . . . ? N7 Cd2 N10 C56 -90.2(5) . . . . ? O2 Cd2 N10 C60 -80.3(5) . . . . ? O5 Cd2 N10 C60 -60.1(19) . . . . ? N8 Cd2 N10 C60 34.0(5) . . . . ? N11 Cd2 N10 C60 -169.2(5) . . . . ? N7 Cd2 N10 C60 104.6(5) . . . . ? C60 N10 C56 C57 0.0 . . . . ? Cd2 N10 C56 C57 -165.7(5) . . . . ? C60 N10 C56 C55 169.9(6) . . . . ? Cd2 N10 C56 C55 4.3(6) . . . . ? N11 C55 C56 N10 -1.1(7) . . . . ? C54 C55 C56 N10 178.8(6) . . . . ? N11 C55 C56 C57 168.6(6) . . . . ? C54 C55 C56 C57 -11.5(6) . . . . ? N10 C56 C57 C58 0.0 . . . . ? C55 C56 C57 C58 -169.5(6) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 N10 0.0 . . . . ? C56 N10 C60 C59 0.0 . . . . ? Cd2 N10 C60 C59 164.4(5) . . . . ? O8 C61 C62 C63 81.8(11) . . . . ? O7 C61 C62 C63 -98.3(11) . . . . ? O8 C61 C62 C68 -98.2(11) . . . . ? O7 C61 C62 C68 81.7(11) . . . . ? C68 C62 C63 C64 180.0(4) . . . . ? C61 C62 C63 C64 0.0(3) . . . . ? C68 C62 C63 C68 8.6(16) . . . 7_667 ? C61 C62 C63 C68 -171.4(16) . . . 7_667 ? C62 C63 C64 C65 180.0(4) . . . . ? C68 C63 C64 C65 -8.6(17) 7_667 . . . ? C63 C64 C65 C66 8.9(18) . . . 7_667 ? C65 C66 C67 C68 -9.1(18) 7_667 . . . ? C66 C67 C68 C63 9.0(18) . . . 7_667 ? C66 C67 C68 C62 -179.8(5) . . . . ? C63 C62 C68 C67 -179.9(4) . . . . ? C61 C62 C68 C67 0.0(6) . . . . ? C63 C62 C68 C63 -8.6(16) . . . 7_667 ? C61 C62 C68 C63 171.4(16) . . . 7_667 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.279 _refine_diff_density_min -1.525 _refine_diff_density_rms 0.116 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 749747' #TrackingRef 'revised CCDC data for 749745 and 749747.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H46 Cd N2 O11' _chemical_formula_weight 867.21 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 Orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 18.560(2) _cell_length_b 20.499(2) _cell_length_c 20.761(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7899.0(16) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 12968 _cell_measurement_theta_min 1.7755 _cell_measurement_theta_max 27.8844 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9639 _exptl_absorpt_correction_T_max 0.9817 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn70 (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28290 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6927 _reflns_number_gt 5590 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+32.6614P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6927 _refine_ls_number_parameters 537 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.056 _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 0.619518(18) 0.029885(17) 0.750063(16) 0.01923(14) Uani 1 1 d . . . O1 O 0.72243(19) 0.09773(16) 0.75424(17) 0.0286(8) Uani 1 1 d . . . O2 O 0.61723(18) 0.1471(2) 0.74819(18) 0.0340(9) Uani 1 1 d . . . O3 O 0.8976(2) 0.40035(19) 0.7374(2) 0.0416(10) Uani 1 1 d . . . O4 O 0.7962(2) 0.44921(18) 0.76030(19) 0.0365(9) Uani 1 1 d . . . O5 O 0.6239(2) 0.0309(2) 0.86632(19) 0.0424(11) Uani 1 1 d . . . O6 O 0.5207(2) 0.0086(2) 0.82206(17) 0.0417(10) Uani 1 1 d . . . O7 O 0.53356(19) 0.02455(17) 0.67139(16) 0.0292(8) Uani 1 1 d . . . O8 O 0.6402(2) 0.0268(2) 0.62649(19) 0.0434(11) Uani 1 1 d . . . O9 O 0.7359(3) 0.0565(3) 0.9463(2) 0.0530(12) Uani 1 1 d D . . H9WA H 0.746(5) 0.031(3) 0.978(3) 0.079 Uiso 1 1 d D . . H9WB H 0.6929(19) 0.056(4) 0.931(4) 0.079 Uiso 1 1 d D . . O10 O 0.7520(3) 0.0260(4) 0.5438(3) 0.097(2) Uani 1 1 d D . . H10 H 0.712(3) 0.025(6) 0.565(5) 0.146 Uiso 1 1 d D . . O11 O 0.5406(3) 0.2656(2) 0.7369(3) 0.0633(14) Uani 1 1 d . . . H11B H 0.5700 0.2341 0.7410 0.095 Uiso 1 1 d R A . C1 C 0.6853(3) 0.1481(2) 0.7518(2) 0.0246(11) Uani 1 1 d . . . C2 C 0.7222(3) 0.2135(2) 0.7509(2) 0.0238(11) Uani 1 1 d . . . C3 C 0.7239(3) 0.2505(2) 0.6940(2) 0.0244(11) Uani 1 1 d . . . C4 C 0.6938(3) 0.2263(3) 0.6349(3) 0.0324(12) Uani 1 1 d . . . H4 H 0.6742 0.1846 0.6333 0.039 Uiso 1 1 calc R . . C5 C 0.6939(3) 0.2645(3) 0.5812(3) 0.0379(14) Uani 1 1 d . . . H5 H 0.6748 0.2482 0.5430 0.046 Uiso 1 1 calc R . . C6 C 0.7229(3) 0.3288(3) 0.5826(3) 0.0379(14) Uani 1 1 d . . . H6 H 0.7199 0.3551 0.5463 0.046 Uiso 1 1 calc R . . C7 C 0.7545(3) 0.3515(3) 0.6367(2) 0.0310(12) Uani 1 1 d . . . H7 H 0.7740 0.3933 0.6368 0.037 Uiso 1 1 calc R . . C8 C 0.7586(3) 0.3126(2) 0.6938(2) 0.0254(11) Uani 1 1 d . . . C9 C 0.7935(3) 0.3347(2) 0.7500(2) 0.0252(11) Uani 1 1 d . . . C10 C 0.7906(3) 0.2980(2) 0.8071(2) 0.0250(11) Uani 1 1 d . . . C11 C 0.8227(3) 0.3215(3) 0.8657(2) 0.0300(12) Uani 1 1 d . . . H11A H 0.8469 0.3613 0.8659 0.036 Uiso 1 1 calc R . . C12 C 0.8180(3) 0.2861(3) 0.9205(3) 0.0383(14) Uani 1 1 d . . . H12 H 0.8379 0.3020 0.9585 0.046 Uiso 1 1 calc R . . C13 C 0.7826(3) 0.2247(3) 0.9202(3) 0.0390(14) Uani 1 1 d . . . H13 H 0.7809 0.2002 0.9578 0.047 Uiso 1 1 calc R . . C14 C 0.7516(3) 0.2012(3) 0.8665(2) 0.0325(12) Uani 1 1 d . . . H14 H 0.7280 0.1611 0.8678 0.039 Uiso 1 1 calc R . . C15 C 0.7542(3) 0.2366(2) 0.8081(2) 0.0250(11) Uani 1 1 d . . . C16 C 0.8326(3) 0.3993(3) 0.7489(2) 0.0271(11) Uani 1 1 d . . . C17 C 0.5588(3) 0.0168(3) 0.8701(2) 0.0295(12) Uani 1 1 d . . . C18 C 0.5266(3) 0.0080(3) 0.9369(2) 0.0291(12) Uani 1 1 d . . . C19 C 0.5011(3) -0.0534(3) 0.9562(2) 0.0287(12) Uani 1 1 d . . . C20 C 0.5011(3) -0.1088(3) 0.9146(3) 0.0336(13) Uani 1 1 d . . . H20 H 0.5179 -0.1041 0.8727 0.040 Uiso 1 1 calc R . . C21 C 0.4776(3) -0.1676(3) 0.9339(3) 0.0404(14) Uani 1 1 d . . . H21 H 0.4767 -0.2024 0.9052 0.048 Uiso 1 1 calc R . . C22 C 0.4542(3) -0.1764(3) 0.9984(3) 0.0422(15) Uani 1 1 d . . . H22 H 0.4400 -0.2176 1.0122 0.051 Uiso 1 1 calc R . . C23 C 0.4521(3) -0.1254(3) 1.0405(3) 0.0364(13) Uani 1 1 d . . . H23 H 0.4359 -0.1320 1.0824 0.044 Uiso 1 1 calc R . . C24 C 0.4746(3) -0.0621(3) 1.0209(2) 0.0294(12) Uani 1 1 d . . . C25 C 0.5739(3) 0.0220(2) 0.6232(2) 0.0268(11) Uani 1 1 d . . . C26 C 0.5368(3) 0.0111(3) 0.5588(2) 0.0258(11) Uani 1 1 d . . . C27 C 0.5409(3) -0.0506(2) 0.5289(2) 0.0230(10) Uani 1 1 d . . . C28 C 0.5801(3) -0.1033(3) 0.5569(2) 0.0315(12) Uani 1 1 d . . . H28 H 0.6041 -0.0970 0.5958 0.038 Uiso 1 1 calc R . . C29 C 0.5828(3) -0.1624(3) 0.5275(3) 0.0361(13) Uani 1 1 d . . . H29 H 0.6080 -0.1964 0.5468 0.043 Uiso 1 1 calc R . . C30 C 0.5476(3) -0.1730(3) 0.4678(3) 0.0388(14) Uani 1 1 d . . . H30 H 0.5514 -0.2134 0.4477 0.047 Uiso 1 1 calc R . . C31 C 0.5087(3) -0.1250(3) 0.4399(2) 0.0309(12) Uani 1 1 d . . . H31 H 0.4848 -0.1331 0.4013 0.037 Uiso 1 1 calc R . . C32 C 0.5035(3) -0.0617(2) 0.4689(2) 0.0231(11) Uani 1 1 d . . . C33 C 0.8143(6) 0.0346(6) 0.5804(5) 0.107(4) Uani 1 1 d . . . H33A H 0.8053 0.0175 0.6233 0.128 Uiso 1 1 calc R . . H33B H 0.8524 0.0085 0.5615 0.128 Uiso 1 1 calc R . . C34 C 0.8391(7) 0.0982(5) 0.5865(9) 0.167(7) Uani 1 1 d . . . H34A H 0.8407 0.1183 0.5448 0.251 Uiso 1 1 calc R . . H34B H 0.8865 0.0978 0.6049 0.251 Uiso 1 1 calc R . . H34C H 0.8072 0.1223 0.6140 0.251 Uiso 1 1 calc R . . C35 C 0.4724(6) 0.2414(6) 0.7316(10) 0.062(6) Uani 0.540(19) 1 d P A 1 H35A H 0.4720 0.2128 0.6944 0.075 Uiso 0.540(19) 1 calc PR A 1 H35B H 0.4411 0.2779 0.7215 0.075 Uiso 0.540(19) 1 calc PR A 1 C36 C 0.4353(11) 0.2022(13) 0.7897(14) 0.116(11) Uani 0.540(19) 1 d P A 1 H36A H 0.4695 0.1724 0.8081 0.174 Uiso 0.540(19) 1 calc PR A 1 H36B H 0.3946 0.1783 0.7737 0.174 Uiso 0.540(19) 1 calc PR A 1 H36C H 0.4196 0.2324 0.8221 0.174 Uiso 0.540(19) 1 calc PR A 1 C35' C 0.4627(15) 0.2316(14) 0.7801(16) 0.091(8) Uani 0.460(19) 1 d PU A 2 H35C H 0.4764 0.2090 0.8193 0.109 Uiso 0.460(19) 1 calc PR A 2 H35D H 0.4262 0.2641 0.7894 0.109 Uiso 0.460(19) 1 calc PR A 2 C36' C 0.4403(8) 0.1853(8) 0.7272(8) 0.052(5) Uani 0.460(19) 1 d P A 2 H36D H 0.4808 0.1593 0.7144 0.078 Uiso 0.460(19) 1 calc PR A 2 H36E H 0.4233 0.2099 0.6908 0.078 Uiso 0.460(19) 1 calc PR A 2 H36F H 0.4025 0.1575 0.7426 0.078 Uiso 0.460(19) 1 calc PR A 2 N1 N 0.8051(3) 0.9824(3) 0.8571(2) 0.0556(16) Uani 1 1 d . . . H1A H 0.7763 0.9649 0.8268 0.067 Uiso 1 1 calc R . . H1B H 0.7774 1.0077 0.8825 0.067 Uiso 1 1 calc R . . N2 N 0.9446(3) 0.9002(3) 0.7630(2) 0.0463(13) Uani 1 1 d . . . H2A H 0.9464 0.8606 0.7444 0.056 Uiso 1 1 calc R . . H2B H 0.9848 0.9218 0.7514 0.056 Uiso 1 1 calc R . . C37 C 0.8364(4) 0.9269(3) 0.8981(3) 0.0516(17) Uani 1 1 d . . . H37A H 0.8695 0.9460 0.9290 0.062 Uiso 1 1 calc R . . H37B H 0.7972 0.9076 0.9224 0.062 Uiso 1 1 calc R . . C38 C 0.8754(4) 0.8727(4) 0.8637(4) 0.0532(18) Uani 1 1 d . . . H38A H 0.8838 0.8376 0.8941 0.064 Uiso 1 1 calc R . . H38B H 0.8442 0.8559 0.8301 0.064 Uiso 1 1 calc R . . C39 C 0.9460(4) 0.8912(3) 0.8338(3) 0.0483(16) Uani 1 1 d . . . H39A H 0.9625 0.9315 0.8534 0.058 Uiso 1 1 calc R . . H39B H 0.9811 0.8577 0.8440 0.058 Uiso 1 1 calc R . . C41 C 0.8738(3) 1.0075(4) 0.7544(3) 0.0495(18) Uani 1 1 d . . . H41A H 0.8344 1.0255 0.7293 0.059 Uiso 1 1 calc R . . H41B H 0.9173 1.0297 0.7407 0.059 Uiso 1 1 calc R . . C40 C 0.8814(3) 0.9359(4) 0.7361(3) 0.0444(16) Uani 1 1 d . . . H40A H 0.8381 0.9133 0.7497 0.053 Uiso 1 1 calc R . . H40B H 0.8836 0.9330 0.6895 0.053 Uiso 1 1 calc R . . C42 C 0.8606(3) 1.0252(4) 0.8242(3) 0.0507(18) Uani 1 1 d . . . H42A H 0.9057 1.0220 0.8475 0.061 Uiso 1 1 calc R . . H42B H 0.8447 1.0702 0.8264 0.061 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 0.0237(2) 0.0180(2) 0.0160(2) -0.00003(14) -0.00042(14) -0.00037(14) O1 0.0293(19) 0.0176(18) 0.039(2) -0.0008(16) 0.0020(16) -0.0039(15) O2 0.0225(19) 0.028(2) 0.051(3) -0.0058(18) -0.0025(17) -0.0037(15) O3 0.033(2) 0.026(2) 0.066(3) 0.004(2) 0.007(2) -0.0097(18) O4 0.035(2) 0.0221(19) 0.052(3) -0.0019(18) 0.0030(18) -0.0026(17) O5 0.037(2) 0.067(3) 0.024(2) 0.004(2) 0.0079(16) -0.002(2) O6 0.040(2) 0.067(3) 0.0176(19) 0.0034(19) -0.0003(17) 0.003(2) O7 0.0330(19) 0.036(2) 0.0191(18) -0.0020(16) -0.0039(16) 0.0007(16) O8 0.031(2) 0.069(3) 0.030(2) -0.009(2) -0.0069(17) -0.002(2) O9 0.045(3) 0.064(3) 0.050(3) 0.004(2) -0.005(2) 0.000(3) O10 0.065(4) 0.159(7) 0.067(4) -0.042(4) 0.012(3) 0.000(4) O11 0.049(3) 0.049(3) 0.091(4) -0.005(3) 0.002(3) 0.008(2) C1 0.035(3) 0.019(2) 0.020(2) 0.001(2) 0.002(2) 0.005(2) C2 0.021(2) 0.022(3) 0.029(3) -0.004(2) 0.002(2) 0.000(2) C3 0.027(2) 0.019(2) 0.027(3) 0.002(2) 0.003(2) 0.003(2) C4 0.036(3) 0.029(3) 0.031(3) -0.007(2) 0.001(2) 0.000(2) C5 0.047(3) 0.041(3) 0.026(3) -0.001(3) -0.006(3) 0.000(3) C6 0.048(3) 0.038(3) 0.027(3) 0.007(3) 0.001(3) 0.003(3) C7 0.040(3) 0.026(3) 0.027(3) 0.002(2) 0.008(2) -0.002(2) C8 0.030(3) 0.022(3) 0.024(3) 0.000(2) 0.006(2) 0.000(2) C9 0.028(3) 0.019(2) 0.028(3) -0.001(2) 0.005(2) -0.002(2) C10 0.025(2) 0.020(3) 0.030(3) 0.000(2) 0.001(2) 0.001(2) C11 0.034(3) 0.025(3) 0.031(3) -0.005(2) -0.002(2) 0.000(2) C12 0.047(3) 0.037(3) 0.031(3) -0.002(3) -0.006(3) 0.002(3) C13 0.051(4) 0.039(3) 0.027(3) 0.008(3) 0.005(3) 0.000(3) C14 0.038(3) 0.028(3) 0.032(3) 0.004(2) 0.001(2) 0.000(2) C15 0.029(3) 0.017(2) 0.029(3) 0.003(2) 0.000(2) 0.004(2) C16 0.035(3) 0.026(3) 0.021(3) 0.001(2) 0.001(2) -0.002(2) C17 0.032(3) 0.034(3) 0.022(3) 0.001(2) 0.006(2) 0.011(2) C18 0.028(3) 0.044(3) 0.016(2) 0.006(2) 0.006(2) 0.007(2) C19 0.027(3) 0.043(3) 0.016(2) 0.000(2) -0.001(2) 0.006(2) C20 0.034(3) 0.044(3) 0.023(3) 0.004(3) 0.002(2) 0.010(3) C21 0.046(3) 0.043(4) 0.031(3) -0.002(3) 0.002(3) 0.010(3) C22 0.051(4) 0.036(3) 0.040(3) 0.006(3) 0.005(3) 0.004(3) C23 0.040(3) 0.047(3) 0.022(3) 0.007(3) 0.002(2) 0.001(3) C24 0.029(3) 0.038(3) 0.020(2) 0.006(2) 0.000(2) 0.010(2) C25 0.034(3) 0.023(3) 0.023(3) -0.001(2) -0.005(2) 0.002(2) C26 0.029(3) 0.029(3) 0.020(2) -0.001(2) 0.000(2) -0.001(2) C27 0.028(3) 0.022(2) 0.019(2) 0.001(2) 0.003(2) 0.003(2) C28 0.037(3) 0.037(3) 0.021(3) -0.002(2) -0.002(2) 0.007(3) C29 0.043(3) 0.033(3) 0.033(3) -0.001(3) -0.005(3) 0.011(3) C30 0.054(4) 0.026(3) 0.036(3) -0.006(3) -0.002(3) 0.003(3) C31 0.040(3) 0.031(3) 0.021(3) -0.004(2) -0.007(2) 0.001(3) C32 0.029(3) 0.026(3) 0.015(2) -0.005(2) 0.0013(19) 0.003(2) C33 0.096(8) 0.145(11) 0.079(7) -0.009(7) -0.027(6) 0.018(7) C34 0.089(9) 0.068(7) 0.34(2) 0.032(11) -0.004(11) -0.002(7) C35 0.017(5) 0.035(7) 0.135(17) 0.022(8) -0.002(7) -0.006(5) C36 0.076(13) 0.12(2) 0.15(2) 0.092(18) 0.047(13) 0.029(13) C35' 0.092(11) 0.091(11) 0.091(11) 0.002(9) -0.006(9) 0.029(8) C36' 0.038(8) 0.063(11) 0.056(11) 0.003(8) 0.000(7) 0.003(8) N1 0.033(3) 0.097(5) 0.037(3) -0.016(3) -0.001(2) -0.006(3) N2 0.034(3) 0.053(3) 0.052(3) 0.006(3) 0.000(2) -0.013(2) C37 0.064(4) 0.053(4) 0.038(3) -0.002(3) 0.006(3) -0.009(4) C38 0.052(4) 0.052(4) 0.056(4) -0.002(4) -0.004(3) -0.003(3) C39 0.051(4) 0.048(4) 0.046(4) -0.014(3) -0.011(3) 0.000(3) C41 0.038(4) 0.070(5) 0.040(4) 0.008(3) 0.009(3) 0.003(3) C40 0.031(3) 0.062(5) 0.040(3) 0.004(3) 0.004(3) 0.004(3) C42 0.033(3) 0.081(5) 0.038(4) 0.013(3) -0.005(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O7 2.286(3) . ? Cd1 O4 2.286(4) 2_645 ? Cd1 O1 2.364(3) . ? Cd1 O2 2.403(4) . ? Cd1 O6 2.406(4) . ? Cd1 O5 2.415(4) . ? Cd1 O8 2.595(4) . ? Cd1 C1 2.713(5) . ? Cd1 C17 2.748(5) . ? O1 C1 1.242(6) . ? O2 C1 1.265(6) . ? O3 C16 1.229(7) . ? O4 C16 1.249(6) . ? O4 Cd1 2.286(4) 2_655 ? O5 C17 1.245(6) . ? O6 C17 1.234(6) . ? O7 C25 1.250(6) . ? O8 C25 1.236(6) . ? O9 H9WA 0.86(2) . ? O9 H9WB 0.86(2) . ? O10 C33 1.394(11) . ? O10 H10 0.86(2) . ? O11 C35 1.364(12) . ? O11 C35' 1.84(3) . ? O11 H11B 0.8500 . ? C1 C2 1.507(7) . ? C2 C3 1.405(7) . ? C2 C15 1.410(7) . ? C3 C8 1.426(7) . ? C3 C4 1.436(7) . ? C4 C5 1.362(8) . ? C4 H4 0.9300 . ? C5 C6 1.424(8) . ? C5 H5 0.9300 . ? C6 C7 1.350(8) . ? C6 H6 0.9300 . ? C7 C8 1.432(7) . ? C7 H7 0.9300 . ? C8 C9 1.409(7) . ? C9 C10 1.406(7) . ? C9 C16 1.510(7) . ? C10 C15 1.428(7) . ? C10 C11 1.438(7) . ? C11 C12 1.353(7) . ? C11 H11A 0.9300 . ? C12 C13 1.420(8) . ? C12 H12 0.9300 . ? C13 C14 1.344(8) . ? C13 H13 0.9300 . ? C14 C15 1.414(7) . ? C14 H14 0.9300 . ? C17 C18 1.520(7) . ? C18 C19 1.404(8) . ? C18 C24 1.413(8) 5_657 ? C19 C20 1.427(8) . ? C19 C24 1.442(7) . ? C20 C21 1.343(8) . ? C20 H20 0.9300 . ? C21 C22 1.420(8) . ? C21 H21 0.9300 . ? C22 C23 1.364(8) . ? C22 H22 0.9300 . ? C23 C24 1.423(8) . ? C23 H23 0.9300 . ? C24 C18 1.413(8) 5_657 ? C25 C26 1.520(7) . ? C26 C32 1.401(7) 5_656 ? C26 C27 1.411(7) . ? C27 C28 1.426(7) . ? C27 C32 1.443(7) . ? C28 C29 1.359(7) . ? C28 H28 0.9300 . ? C29 C30 1.417(8) . ? C29 H29 0.9300 . ? C30 C31 1.353(8) . ? C30 H30 0.9300 . ? C31 C32 1.434(7) . ? C31 H31 0.9300 . ? C32 C26 1.401(7) 5_656 ? C33 C34 1.388(14) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.61(3) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C35' C36' 1.51(3) . ? C35' H35C 0.9700 . ? C35' H35D 0.9700 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? N1 C42 1.517(8) . ? N1 C37 1.534(9) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C39 1.483(8) . ? N2 C40 1.490(8) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C37 C38 1.506(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.498(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C40 1.524(12) . ? C41 C42 1.514(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? 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 O7 Cd1 O4 120.62(13) . 2_645 ? O7 Cd1 O1 128.19(12) . . ? O4 Cd1 O1 82.50(13) 2_645 . ? O7 Cd1 O2 91.37(12) . . ? O4 Cd1 O2 137.46(13) 2_645 . ? O1 Cd1 O2 55.03(12) . . ? O7 Cd1 O6 84.44(13) . . ? O4 Cd1 O6 109.42(14) 2_645 . ? O1 Cd1 O6 134.41(13) . . ? O2 Cd1 O6 100.25(14) . . ? O7 Cd1 O5 137.56(13) . . ? O4 Cd1 O5 83.70(14) 2_645 . ? O1 Cd1 O5 86.05(13) . . ? O2 Cd1 O5 90.47(14) . . ? O6 Cd1 O5 53.59(13) . . ? O7 Cd1 O8 52.80(12) . . ? O4 Cd1 O8 88.46(14) 2_645 . ? O1 Cd1 O8 86.07(12) . . ? O2 Cd1 O8 90.65(14) . . ? O6 Cd1 O8 136.25(12) . . ? O5 Cd1 O8 169.53(13) . . ? O7 Cd1 C1 111.49(14) . . ? O4 Cd1 C1 109.70(14) 2_645 . ? O1 Cd1 C1 27.23(13) . . ? O2 Cd1 C1 27.80(13) . . ? O6 Cd1 C1 119.78(15) . . ? O5 Cd1 C1 87.92(14) . . ? O8 Cd1 C1 88.21(14) . . ? O7 Cd1 C17 110.91(14) . . ? O4 Cd1 C17 97.21(15) 2_645 . ? O1 Cd1 C17 110.83(15) . . ? O2 Cd1 C17 96.04(14) . . ? O6 Cd1 C17 26.66(14) . . ? O5 Cd1 C17 26.93(14) . . ? O8 Cd1 C17 162.69(15) . . ? C1 Cd1 C17 105.06(15) . . ? C1 O1 Cd1 92.2(3) . . ? C1 O2 Cd1 89.9(3) . . ? C16 O4 Cd1 101.8(3) . 2_655 ? C17 O5 Cd1 91.6(3) . . ? C17 O6 Cd1 92.3(3) . . ? C25 O7 Cd1 99.0(3) . . ? C25 O8 Cd1 84.8(3) . . ? H9WA O9 H9WB 118(8) . . ? C33 O10 H10 116(8) . . ? C35 O11 C35' 34.0(11) . . ? C35 O11 H11B 109.1 . . ? C35' O11 H11B 99.6 . . ? O1 C1 O2 122.9(5) . . ? O1 C1 C2 119.2(5) . . ? O2 C1 C2 117.9(4) . . ? O1 C1 Cd1 60.6(3) . . ? O2 C1 Cd1 62.3(3) . . ? C2 C1 Cd1 178.5(3) . . ? C3 C2 C15 121.2(5) . . ? C3 C2 C1 120.1(4) . . ? C15 C2 C1 118.7(4) . . ? C2 C3 C8 119.6(4) . . ? C2 C3 C4 121.5(5) . . ? C8 C3 C4 118.8(5) . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 120.1(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 121.3(5) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C3 119.6(4) . . ? C9 C8 C7 122.1(5) . . ? C3 C8 C7 118.3(5) . . ? C10 C9 C8 120.5(4) . . ? C10 C9 C16 120.0(4) . . ? C8 C9 C16 119.4(4) . . ? C9 C10 C15 120.1(5) . . ? C9 C10 C11 121.2(5) . . ? C15 C10 C11 118.7(5) . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.8(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C2 C15 C14 122.4(5) . . ? C2 C15 C10 118.9(4) . . ? C14 C15 C10 118.7(5) . . ? O3 C16 O4 123.6(5) . . ? O3 C16 C9 119.3(5) . . ? O4 C16 C9 117.1(5) . . ? O6 C17 O5 122.5(5) . . ? O6 C17 C18 119.7(5) . . ? O5 C17 C18 117.8(5) . . ? O6 C17 Cd1 61.0(3) . . ? O5 C17 Cd1 61.4(3) . . ? C18 C17 Cd1 178.4(4) . . ? C19 C18 C24 121.4(4) . 5_657 ? C19 C18 C17 119.9(5) . . ? C24 C18 C17 118.7(5) 5_657 . ? C18 C19 C20 122.8(5) . . ? C18 C19 C24 119.4(5) . . ? C20 C19 C24 117.8(5) . . ? C21 C20 C19 122.3(5) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 119.7(6) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C18 C24 C23 122.2(5) 5_657 . ? C18 C24 C19 119.2(5) 5_657 . ? C23 C24 C19 118.6(5) . . ? O8 C25 O7 123.3(5) . . ? O8 C25 C26 120.7(5) . . ? O7 C25 C26 116.0(5) . . ? C32 C26 C27 120.6(4) 5_656 . ? C32 C26 C25 119.7(4) 5_656 . ? C27 C26 C25 119.6(4) . . ? C26 C27 C28 121.8(5) . . ? C26 C27 C32 119.7(4) . . ? C28 C27 C32 118.5(4) . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.8(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.6(5) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 121.0(5) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C26 C32 C31 122.1(4) 5_656 . ? C26 C32 C27 119.6(4) 5_656 . ? C31 C32 C27 118.2(4) . . ? C34 C33 O10 116.3(11) . . ? C34 C33 H33A 108.2 . . ? O10 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? O10 C33 H33B 108.2 . . ? H33A C33 H33B 107.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O11 C35 C36 121.4(18) . . ? O11 C35 H35A 107.0 . . ? C36 C35 H35A 106.9 . . ? O11 C35 H35B 107.0 . . ? C36 C35 H35B 107.0 . . ? H35A C35 H35B 106.7 . . ? C36' C35' O11 95.8(19) . . ? C36' C35' H35C 112.6 . . ? O11 C35' H35C 112.6 . . ? C36' C35' H35D 112.6 . . ? O11 C35' H35D 112.6 . . ? H35C C35' H35D 110.1 . . ? C35' C36' H36D 109.5 . . ? C35' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35' C36' H36F 109.4 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C42 N1 C37 114.9(5) . . ? C42 N1 H1A 108.5 . . ? C37 N1 H1A 108.5 . . ? C42 N1 H1B 108.5 . . ? C37 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? C39 N2 C40 116.5(5) . . ? C39 N2 H2A 108.2 . . ? C40 N2 H2A 108.2 . . ? C39 N2 H2B 108.2 . . ? C40 N2 H2B 108.2 . . ? H2A N2 H2B 107.3 . . ? C38 C37 N1 117.7(5) . . ? C38 C37 H37A 107.9 . . ? N1 C37 H37A 107.9 . . ? C38 C37 H37B 107.9 . . ? N1 C37 H37B 107.9 . . ? H37A C37 H37B 107.2 . . ? C39 C38 C37 115.5(6) . . ? C39 C38 H38A 108.4 . . ? C37 C38 H38A 108.4 . . ? C39 C38 H38B 108.4 . . ? C37 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? N2 C39 C38 115.2(5) . . ? N2 C39 H39A 108.5 . . ? C38 C39 H39A 108.5 . . ? N2 C39 H39B 108.5 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C40 C41 C42 119.0(6) . . ? C40 C41 H41A 107.6 . . ? C42 C41 H41A 107.6 . . ? C40 C41 H41B 107.6 . . ? C42 C41 H41B 107.6 . . ? H41A C41 H41B 107.0 . . ? N2 C40 C41 116.9(5) . . ? N2 C40 H40A 108.1 . . ? C41 C40 H40A 108.1 . . ? N2 C40 H40B 108.1 . . ? C41 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? N1 C42 C41 113.7(6) . . ? N1 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? N1 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cd1 O1 C1 59.3(3) . . . . ? O4 Cd1 O1 C1 -177.3(3) 2_645 . . . ? O2 Cd1 O1 C1 0.2(3) . . . . ? O6 Cd1 O1 C1 -67.4(3) . . . . ? O5 Cd1 O1 C1 -93.1(3) . . . . ? O8 Cd1 O1 C1 93.7(3) . . . . ? C17 Cd1 O1 C1 -82.4(3) . . . . ? O7 Cd1 O2 C1 -137.7(3) . . . . ? O4 Cd1 O2 C1 3.5(4) 2_645 . . . ? O1 Cd1 O2 C1 -0.2(3) . . . . ? O6 Cd1 O2 C1 137.7(3) . . . . ? O5 Cd1 O2 C1 84.7(3) . . . . ? O8 Cd1 O2 C1 -84.9(3) . . . . ? C17 Cd1 O2 C1 111.1(3) . . . . ? O7 Cd1 O5 C17 10.0(4) . . . . ? O4 Cd1 O5 C17 -119.7(3) 2_645 . . . ? O1 Cd1 O5 C17 157.4(3) . . . . ? O2 Cd1 O5 C17 102.5(3) . . . . ? O6 Cd1 O5 C17 0.1(3) . . . . ? O8 Cd1 O5 C17 -161.4(7) . . . . ? C1 Cd1 O5 C17 130.2(3) . . . . ? O7 Cd1 O6 C17 -173.4(3) . . . . ? O4 Cd1 O6 C17 66.1(4) 2_645 . . . ? O1 Cd1 O6 C17 -32.7(4) . . . . ? O2 Cd1 O6 C17 -83.0(3) . . . . ? O5 Cd1 O6 C17 -0.1(3) . . . . ? O8 Cd1 O6 C17 175.1(3) . . . . ? C1 Cd1 O6 C17 -61.8(4) . . . . ? O4 Cd1 O7 C25 -58.5(3) 2_645 . . . ? O1 Cd1 O7 C25 47.4(4) . . . . ? O2 Cd1 O7 C25 92.1(3) . . . . ? O6 Cd1 O7 C25 -167.8(3) . . . . ? O5 Cd1 O7 C25 -175.7(3) . . . . ? O8 Cd1 O7 C25 2.3(3) . . . . ? C1 Cd1 O7 C25 72.4(3) . . . . ? C17 Cd1 O7 C25 -170.9(3) . . . . ? O7 Cd1 O8 C25 -2.3(3) . . . . ? O4 Cd1 O8 C25 129.0(3) 2_645 . . . ? O1 Cd1 O8 C25 -148.4(3) . . . . ? O2 Cd1 O8 C25 -93.5(3) . . . . ? O6 Cd1 O8 C25 12.1(4) . . . . ? O5 Cd1 O8 C25 170.4(7) . . . . ? C1 Cd1 O8 C25 -121.2(3) . . . . ? C17 Cd1 O8 C25 19.4(7) . . . . ? Cd1 O1 C1 O2 -0.4(5) . . . . ? Cd1 O1 C1 C2 -178.3(4) . . . . ? Cd1 O2 C1 O1 0.4(5) . . . . ? Cd1 O2 C1 C2 178.3(4) . . . . ? O7 Cd1 C1 O1 -133.4(3) . . . . ? O4 Cd1 C1 O1 2.8(3) 2_645 . . . ? O2 Cd1 C1 O1 -179.7(5) . . . . ? O6 Cd1 C1 O1 130.6(3) . . . . ? O5 Cd1 C1 O1 85.4(3) . . . . ? O8 Cd1 C1 O1 -84.9(3) . . . . ? C17 Cd1 C1 O1 106.4(3) . . . . ? O7 Cd1 C1 O2 46.3(3) . . . . ? O4 Cd1 C1 O2 -177.5(3) 2_645 . . . ? O1 Cd1 C1 O2 179.7(5) . . . . ? O6 Cd1 C1 O2 -49.8(3) . . . . ? O5 Cd1 C1 O2 -94.9(3) . . . . ? O8 Cd1 C1 O2 94.8(3) . . . . ? C17 Cd1 C1 O2 -74.0(3) . . . . ? O7 Cd1 C1 C2 -53(14) . . . . ? O4 Cd1 C1 C2 83(13) 2_645 . . . ? O1 Cd1 C1 C2 80(13) . . . . ? O2 Cd1 C1 C2 -100(14) . . . . ? O6 Cd1 C1 C2 -149(13) . . . . ? O5 Cd1 C1 C2 165(13) . . . . ? O8 Cd1 C1 C2 -5(13) . . . . ? C17 Cd1 C1 C2 -174(100) . . . . ? O1 C1 C2 C3 107.4(6) . . . . ? O2 C1 C2 C3 -70.6(6) . . . . ? Cd1 C1 C2 C3 28(14) . . . . ? O1 C1 C2 C15 -73.1(6) . . . . ? O2 C1 C2 C15 108.9(5) . . . . ? Cd1 C1 C2 C15 -152(13) . . . . ? C15 C2 C3 C8 0.1(7) . . . . ? C1 C2 C3 C8 179.5(4) . . . . ? C15 C2 C3 C4 177.7(5) . . . . ? C1 C2 C3 C4 -2.8(7) . . . . ? C2 C3 C4 C5 177.5(5) . . . . ? C8 C3 C4 C5 -4.8(8) . . . . ? C3 C4 C5 C6 -0.8(9) . . . . ? C4 C5 C6 C7 3.8(9) . . . . ? C5 C6 C7 C8 -1.2(9) . . . . ? C2 C3 C8 C9 2.8(7) . . . . ? C4 C3 C8 C9 -174.9(5) . . . . ? C2 C3 C8 C7 -175.0(5) . . . . ? C4 C3 C8 C7 7.2(7) . . . . ? C6 C7 C8 C9 177.8(5) . . . . ? C6 C7 C8 C3 -4.3(8) . . . . ? C3 C8 C9 C10 -4.0(7) . . . . ? C7 C8 C9 C10 173.8(5) . . . . ? C3 C8 C9 C16 177.7(5) . . . . ? C7 C8 C9 C16 -4.5(7) . . . . ? C8 C9 C10 C15 2.3(7) . . . . ? C16 C9 C10 C15 -179.4(5) . . . . ? C8 C9 C10 C11 -176.7(5) . . . . ? C16 C9 C10 C11 1.5(7) . . . . ? C9 C10 C11 C12 178.6(5) . . . . ? C15 C10 C11 C12 -0.4(8) . . . . ? C10 C11 C12 C13 1.5(9) . . . . ? C11 C12 C13 C14 -1.9(9) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C3 C2 C15 C14 178.2(5) . . . . ? C1 C2 C15 C14 -1.2(7) . . . . ? C3 C2 C15 C10 -1.8(7) . . . . ? C1 C2 C15 C10 178.7(4) . . . . ? C13 C14 C15 C2 180.0(5) . . . . ? C13 C14 C15 C10 0.0(8) . . . . ? C9 C10 C15 C2 0.6(7) . . . . ? C11 C10 C15 C2 179.7(5) . . . . ? C9 C10 C15 C14 -179.4(5) . . . . ? C11 C10 C15 C14 -0.4(7) . . . . ? Cd1 O4 C16 O3 1.5(6) 2_655 . . . ? Cd1 O4 C16 C9 -178.7(4) 2_655 . . . ? C10 C9 C16 O3 87.6(6) . . . . ? C8 C9 C16 O3 -94.2(6) . . . . ? C10 C9 C16 O4 -92.2(6) . . . . ? C8 C9 C16 O4 86.1(6) . . . . ? Cd1 O6 C17 O5 0.1(6) . . . . ? Cd1 O6 C17 C18 -178.4(4) . . . . ? Cd1 O5 C17 O6 -0.1(6) . . . . ? Cd1 O5 C17 C18 178.5(4) . . . . ? O7 Cd1 C17 O6 7.0(4) . . . . ? O4 Cd1 C17 O6 -119.7(3) 2_645 . . . ? O1 Cd1 C17 O6 155.6(3) . . . . ? O2 Cd1 C17 O6 100.8(3) . . . . ? O5 Cd1 C17 O6 179.9(6) . . . . ? O8 Cd1 C17 O6 -11.4(7) . . . . ? C1 Cd1 C17 O6 127.6(3) . . . . ? O7 Cd1 C17 O5 -172.8(3) . . . . ? O4 Cd1 C17 O5 60.5(3) 2_645 . . . ? O1 Cd1 C17 O5 -24.2(4) . . . . ? O2 Cd1 C17 O5 -79.0(3) . . . . ? O6 Cd1 C17 O5 -179.9(6) . . . . ? O8 Cd1 C17 O5 168.8(4) . . . . ? C1 Cd1 C17 O5 -52.2(4) . . . . ? O7 Cd1 C17 C18 127(16) . . . . ? O4 Cd1 C17 C18 0(16) 2_645 . . . ? O1 Cd1 C17 C18 -84(16) . . . . ? O2 Cd1 C17 C18 -139(16) . . . . ? O6 Cd1 C17 C18 120(16) . . . . ? O5 Cd1 C17 C18 -60(16) . . . . ? O8 Cd1 C17 C18 109(16) . . . . ? C1 Cd1 C17 C18 -113(16) . . . . ? O6 C17 C18 C19 63.9(7) . . . . ? O5 C17 C18 C19 -114.8(6) . . . . ? Cd1 C17 C18 C19 -55(16) . . . . ? O6 C17 C18 C24 -118.3(6) . . . 5_657 ? O5 C17 C18 C24 63.1(7) . . . 5_657 ? Cd1 C17 C18 C24 123(16) . . . 5_657 ? C24 C18 C19 C20 179.5(5) 5_657 . . . ? C17 C18 C19 C20 -2.7(8) . . . . ? C24 C18 C19 C24 -1.4(8) 5_657 . . . ? C17 C18 C19 C24 176.4(5) . . . . ? C18 C19 C20 C21 178.9(5) . . . . ? C24 C19 C20 C21 -0.2(8) . . . . ? C19 C20 C21 C22 -2.3(9) . . . . ? C20 C21 C22 C23 2.9(9) . . . . ? C21 C22 C23 C24 -1.0(9) . . . . ? C22 C23 C24 C18 -179.9(5) . . . 5_657 ? C22 C23 C24 C19 -1.5(8) . . . . ? C18 C19 C24 C18 1.3(8) . . . 5_657 ? C20 C19 C24 C18 -179.5(5) . . . 5_657 ? C18 C19 C24 C23 -177.1(5) . . . . ? C20 C19 C24 C23 2.1(7) . . . . ? Cd1 O8 C25 O7 4.0(5) . . . . ? Cd1 O8 C25 C26 -174.7(4) . . . . ? Cd1 O7 C25 O8 -4.6(6) . . . . ? Cd1 O7 C25 C26 174.2(4) . . . . ? O8 C25 C26 C32 -108.9(6) . . . 5_656 ? O7 C25 C26 C32 72.2(6) . . . 5_656 ? O8 C25 C26 C27 73.6(7) . . . . ? O7 C25 C26 C27 -105.3(6) . . . . ? C32 C26 C27 C28 -178.5(5) 5_656 . . . ? C25 C26 C27 C28 -1.0(7) . . . . ? C32 C26 C27 C32 0.3(8) 5_656 . . . ? C25 C26 C27 C32 177.8(4) . . . . ? C26 C27 C28 C29 179.4(5) . . . . ? C32 C27 C28 C29 0.6(8) . . . . ? C27 C28 C29 C30 0.9(9) . . . . ? C28 C29 C30 C31 -2.2(9) . . . . ? C29 C30 C31 C32 1.7(9) . . . . ? C30 C31 C32 C26 -179.7(5) . . . 5_656 ? C30 C31 C32 C27 -0.2(8) . . . . ? C26 C27 C32 C26 -0.3(8) . . . 5_656 ? C28 C27 C32 C26 178.5(5) . . . 5_656 ? C26 C27 C32 C31 -179.8(5) . . . . ? C28 C27 C32 C31 -1.0(7) . . . . ? C35' O11 C35 C36 -14(2) . . . . ? C35 O11 C35' C36' 34.3(15) . . . . ? C42 N1 C37 C38 -67.3(8) . . . . ? N1 C37 C38 C39 69.1(8) . . . . ? C40 N2 C39 C38 42.2(8) . . . . ? C37 C38 C39 N2 -103.2(7) . . . . ? C39 N2 C40 C41 65.8(7) . . . . ? C42 C41 C40 N2 -64.8(7) . . . . ? C37 N1 C42 C41 98.5(6) . . . . ? C40 C41 C42 N1 -43.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.135 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.098