CMM-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H98 Cd8 F14 N8 O12 S14' _chemical_formula_weight 3241.92 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 14.8591(2) _cell_length_b 15.0112(2) _cell_length_c 15.6142(2) _cell_angle_alpha 93.269(2) _cell_angle_beta 114.292(2) _cell_angle_gamma 103.701(2) _cell_volume 3036.82(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.692 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.849613 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS(SCHLDRICK, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD dector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38561 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10670 _reflns_number_gt 9948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _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^)+(0.0550P)^2^+12.7061P] 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 10670 _refine_ls_number_parameters 603 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.80496(2) 0.40619(2) 0.28799(2) 0.02623(9) Uani 1 1 d . . . Cd2 Cd 0.94368(2) 0.65996(2) 0.36665(2) 0.02541(9) Uani 1 1 d . . . Cd3 Cd 0.79554(2) 0.37564(2) 0.51837(2) 0.02867(9) Uani 1 1 d . . . Cd4 Cd 0.90728(2) 0.67166(2) 0.62388(2) 0.02667(9) Uani 1 1 d . . . S1 S 0.89639(8) 0.27930(8) 0.32668(8) 0.0273(2) Uani 1 1 d . . . S2 S 0.86959(9) 0.53735(8) 0.21482(8) 0.0292(2) Uani 1 1 d . . . S3 S 1.12922(9) 0.76445(9) 0.45243(8) 0.0335(3) Uani 1 1 d . . . S4 S 0.67474(10) 0.40144(9) 0.35603(9) 0.0342(3) Uani 1 1 d . . . S5 S 0.85022(10) 0.79538(9) 0.68069(9) 0.0352(3) Uani 1 1 d . . . S6 S 0.82039(8) 0.66463(8) 0.44109(7) 0.0274(2) Uani 1 1 d . . . S7 S 0.85613(12) 0.50741(9) 0.65895(9) 0.0417(3) Uani 1 1 d . . . F1 F 0.6241(3) 0.0126(3) 0.0675(4) 0.0921(16) Uani 1 1 d . . . F2 F 0.5302(3) 0.6189(3) 0.1295(3) 0.0717(11) Uani 1 1 d . . . F3' F 1.3060(9) 1.0139(6) 0.3253(8) 0.099(3) Uani 0.50 1 d P . . F3 F 1.1287(10) 0.7451(7) 0.1246(6) 0.102(4) Uani 0.50 1 d P . . F4 F 0.5401(5) 0.0462(3) 0.2831(5) 0.123(2) Uani 1 1 d . . . F5 F 0.8940(4) 0.9578(3) 0.9934(3) 0.0859(14) Uani 1 1 d . . . F6 F 0.6184(4) 0.8792(4) 0.2628(3) 0.0939(16) Uani 1 1 d . . . O1 O 0.6657(3) 0.2871(3) 0.5496(3) 0.0544(11) Uani 1 1 d . . . O2 O 0.8854(3) 0.7616(2) 0.2654(2) 0.0342(7) Uani 1 1 d . . . O3 O 0.6720(2) 0.3263(2) 0.1423(2) 0.0344(7) Uani 1 1 d . . . N1 N 0.5029(4) 0.2229(5) 0.5267(5) 0.0739(19) Uani 1 1 d . . . N2 N 0.8827(3) 0.9023(3) 0.2223(3) 0.0319(9) Uani 1 1 d . . . N3 N 0.6097(4) 0.2505(3) -0.0085(3) 0.0525(13) Uani 1 1 d . . . C1 C 0.5752(4) 0.2789(4) 0.5116(4) 0.0471(13) Uani 1 1 d . . . H1A H 0.5537 0.3165 0.4664 0.056 Uiso 1 1 calc R . . C2 C 0.5299(15) 0.1642(14) 0.5953(14) 0.211(8) Uiso 1 1 d . . . H2A H 0.6032 0.1745 0.6241 0.316 Uiso 1 1 calc R . . H2B H 0.4962 0.1003 0.5648 0.316 Uiso 1 1 calc R . . H2C H 0.5085 0.1780 0.6436 0.316 Uiso 1 1 calc R . . C3 C 0.3950(6) 0.2187(7) 0.4744(7) 0.090(3) Uani 1 1 d . . . H3A H 0.3881 0.2608 0.4296 0.135 Uiso 1 1 calc R . . H3B H 0.3694 0.2359 0.5182 0.135 Uiso 1 1 calc R . . H3C H 0.3562 0.1564 0.4407 0.135 Uiso 1 1 calc R . . C4 C 0.9256(4) 0.8458(3) 0.2762(3) 0.0288(9) Uani 1 1 d . . . H4A H 0.9910 0.8713 0.3261 0.035 Uiso 1 1 calc R . . C5 C 0.9353(4) 1.0019(4) 0.2411(5) 0.0482(14) Uani 1 1 d . . . H5A H 1.0030 1.0147 0.2927 0.072 Uiso 1 1 calc R . . H5B H 0.8967 1.0366 0.2580 0.072 Uiso 1 1 calc R . . H5C H 0.9407 1.0196 0.1849 0.072 Uiso 1 1 calc R . . C6 C 0.7785(4) 0.8690(4) 0.1462(4) 0.0416(12) Uani 1 1 d . . . H6A H 0.7529 0.8030 0.1412 0.062 Uiso 1 1 calc R . . H6B H 0.7789 0.8825 0.0869 0.062 Uiso 1 1 calc R . . H6C H 0.7349 0.8995 0.1601 0.062 Uiso 1 1 calc R . . C7 C 0.6776(4) 0.3120(3) 0.0664(4) 0.0366(11) Uani 1 1 d . . . H7A H 0.7353 0.3482 0.0621 0.044 Uiso 1 1 calc R . . C8 C 0.6216(8) 0.2396(7) -0.0962(5) 0.092(3) Uani 1 1 d . . . H8A H 0.6847 0.2829 -0.0881 0.138 Uiso 1 1 calc R . . H8B H 0.5646 0.2515 -0.1476 0.138 Uiso 1 1 calc R . . H8C H 0.6235 0.1773 -0.1107 0.138 Uiso 1 1 calc R . . C9 C 0.5193(5) 0.1911(5) -0.0061(6) 0.079(3) Uani 1 1 d . . . H9A H 0.5213 0.2053 0.0555 0.118 Uiso 1 1 calc R . . H9B H 0.5178 0.1272 -0.0178 0.118 Uiso 1 1 calc R . . H9C H 0.4587 0.2013 -0.0543 0.118 Uiso 1 1 calc R . . C11 C 0.8415(2) 0.2083(2) 0.21172(18) 0.0307(10) Uani 1 1 d G . . C12 C 0.7512(2) 0.1365(2) 0.1839(3) 0.0455(13) Uani 1 1 d G . . H12A H 0.7191 0.1274 0.2241 0.055 Uiso 1 1 calc R . . C13 C 0.7089(2) 0.0784(2) 0.0961(3) 0.062(2) Uani 1 1 d G . . C14 C 0.7569(3) 0.0920(3) 0.0361(2) 0.067(2) Uani 1 1 d G . . H14A H 0.7286 0.0531 -0.0227 0.081 Uiso 1 1 calc R . . C15 C 0.8472(3) 0.1638(3) 0.0639(2) 0.0591(17) Uani 1 1 d G . . H15A H 0.8793 0.1729 0.0237 0.071 Uiso 1 1 calc R . . C16 C 0.8895(2) 0.2219(2) 0.1517(2) 0.0407(12) Uani 1 1 d G . . H16A H 0.9499 0.2700 0.1703 0.049 Uiso 1 1 calc R . . C21 C 0.7552(2) 0.5627(2) 0.1359(2) 0.0300(10) Uani 1 1 d G . . C22 C 0.6834(2) 0.5796(2) 0.16535(17) 0.0352(11) Uani 1 1 d G . . H22A H 0.6930 0.5761 0.2277 0.042 Uiso 1 1 calc R . . C23 C 0.5971(2) 0.6017(3) 0.1016(2) 0.0441(13) Uani 1 1 d G . . C24 C 0.5827(2) 0.6069(3) 0.0084(2) 0.0530(15) Uani 1 1 d G . . H24A H 0.5250 0.6216 -0.0342 0.064 Uiso 1 1 calc R . . C25 C 0.6545(3) 0.5900(3) -0.02096(19) 0.0667(19) Uani 1 1 d G . . H25A H 0.6448 0.5935 -0.0833 0.080 Uiso 1 1 calc R . . C26 C 0.7408(3) 0.5679(3) 0.0428(2) 0.0541(15) Uani 1 1 d G . . H26A H 0.7888 0.5566 0.0231 0.065 Uiso 1 1 calc R . . C31 C 1.1597(3) 0.8074(2) 0.3605(2) 0.0364(11) Uani 1 1 d G . . C32 C 1.1260(3) 0.7525(2) 0.2724(2) 0.0463(13) Uani 1 1 d G . . H32A H 1.0873 0.6906 0.2602 0.056 Uiso 1 1 calc R . . C33 C 1.1500(4) 0.7899(3) 0.2024(2) 0.0648(18) Uani 1 1 d G . . C34 C 1.2077(4) 0.8823(3) 0.2206(3) 0.074(2) Uani 1 1 d G . . H34A H 1.2238 0.9074 0.1738 0.089 Uiso 1 1 calc R . . C35 C 1.2415(4) 0.9373(2) 0.3087(3) 0.081(2) Uani 1 1 d G . . C36 C 1.2175(3) 0.8998(2) 0.3787(2) 0.0601(17) Uani 1 1 d G . . H36A H 1.2401 0.9366 0.4376 0.072 Uiso 1 1 calc R . . C41 C 0.5798(2) 0.2940(2) 0.2985(3) 0.0351(11) Uani 1 1 d G . . C42 C 0.5993(2) 0.2086(2) 0.3125(3) 0.0494(14) Uani 1 1 d G . . H42A H 0.6655 0.2063 0.3514 0.059 Uiso 1 1 calc R . . C43 C 0.5198(4) 0.1265(2) 0.2682(4) 0.072(2) Uani 1 1 d G . . C44 C 0.4208(3) 0.1299(3) 0.2100(4) 0.084(3) Uani 1 1 d G . . H44A H 0.3676 0.0750 0.1804 0.101 Uiso 1 1 calc R . . C45 C 0.4013(2) 0.2153(4) 0.1960(3) 0.088(3) Uani 1 1 d G . . H45A H 0.3351 0.2176 0.1571 0.105 Uiso 1 1 calc R . . C46 C 0.4808(3) 0.2974(3) 0.2402(3) 0.0627(18) Uani 1 1 d G . . H46A H 0.4678 0.3545 0.2309 0.075 Uiso 1 1 calc R . . C51 C 0.8667(3) 0.7931(2) 0.79991(18) 0.0324(10) Uani 1 1 d G . . C52 C 0.8751(3) 0.87593(19) 0.8512(2) 0.0432(12) Uani 1 1 d G . . H52A H 0.8714 0.9285 0.8226 0.052 Uiso 1 1 calc R . . C53 C 0.8890(3) 0.8802(2) 0.9451(2) 0.0533(15) Uani 1 1 d G . . C54 C 0.8946(4) 0.8016(3) 0.98781(19) 0.0612(18) Uani 1 1 d G . . H54A H 0.9039 0.8045 1.0507 0.073 Uiso 1 1 calc R . . C55 C 0.8862(4) 0.7188(2) 0.9366(3) 0.0638(18) Uani 1 1 d G . . H55A H 0.8899 0.6663 0.9651 0.077 Uiso 1 1 calc R . . C56 C 0.8723(3) 0.71458(19) 0.8426(2) 0.0481(14) Uani 1 1 d G . . H56A H 0.8667 0.6592 0.8083 0.058 Uiso 1 1 calc R . . C61 C 0.8053(2) 0.77872(17) 0.4251(2) 0.0317(10) Uani 1 1 d G . . C62 C 0.7153(2) 0.7846(2) 0.3509(2) 0.0437(13) Uani 1 1 d G . . H62A H 0.6655 0.7307 0.3117 0.052 Uiso 1 1 calc R . . C63 C 0.6999(3) 0.8712(3) 0.3351(2) 0.0564(17) Uani 1 1 d G . . C64 C 0.7744(3) 0.9518(2) 0.3936(3) 0.0578(17) Uani 1 1 d G . . H64A H 0.7640 1.0097 0.3830 0.069 Uiso 1 1 calc R . . C65 C 0.8643(3) 0.94589(18) 0.4679(2) 0.0526(15) Uani 1 1 d G . . H65A H 0.9142 0.9998 0.5070 0.063 Uiso 1 1 calc R . . C66 C 0.8798(2) 0.8594(2) 0.4836(2) 0.0388(11) Uani 1 1 d G . . H66A H 0.9400 0.8554 0.5333 0.047 Uiso 1 1 calc R . . C71 C 0.7351(4) 0.4966(4) 0.6665(5) 0.0619(17) Uiso 1 1 d G . . C72 C 0.6622(6) 0.5376(5) 0.6093(5) 0.106(3) Uiso 1 1 d G . . C73 C 0.5697(5) 0.5255(7) 0.6159(7) 0.171(6) Uiso 1 1 d G . . C74 C 0.5502(6) 0.4724(8) 0.6797(8) 0.149(5) Uiso 1 1 d G . . C75 C 0.6231(8) 0.4314(8) 0.7369(7) 0.223(9) Uiso 1 1 d G . . C76 C 0.7156(7) 0.4436(6) 0.7303(6) 0.160(6) Uiso 1 1 d G . . N4 N 1.0000 0.5000 0.5000 0.0386(14) Uani 1 2 d SD . . O4 O 0.9011(4) 0.4627(4) 0.4562(4) 0.0280(13) Uani 0.50 1 d PD . . O5 O 1.0550(5) 0.4843(4) 0.5805(4) 0.0314(15) Uani 0.50 1 d PD . . O6 O 1.0367(4) 0.5726(4) 0.4675(4) 0.0290(14) Uani 0.50 1 d PD . . N5 N 1.0000 0.5000 1.0000 0.214(9) Uiso 1 2 d SDU . . O7 O 0.8958(18) 0.457(3) 0.938(3) 0.38(2) Uiso 0.50 1 d PDU . . O8 O 1.0532(13) 0.5647(12) 0.9643(13) 0.131(5) Uiso 0.50 1 d PDU . . O9 O 1.014(4) 0.531(3) 1.0886(17) 0.315(18) Uiso 0.50 1 d PDU . . 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 0.02640(17) 0.02151(16) 0.02446(16) 0.00340(12) 0.00580(13) 0.00571(13) Cd2 0.02545(17) 0.02386(17) 0.02885(17) 0.00984(13) 0.01182(13) 0.00938(13) Cd3 0.02192(17) 0.03417(19) 0.02719(17) 0.00285(13) 0.01156(13) 0.00231(13) Cd4 0.02731(17) 0.02726(18) 0.02431(16) 0.00321(13) 0.01084(13) 0.00698(13) S1 0.0264(5) 0.0303(6) 0.0264(5) 0.0067(4) 0.0106(4) 0.0114(4) S2 0.0285(6) 0.0238(5) 0.0364(6) 0.0058(4) 0.0150(5) 0.0080(4) S3 0.0272(6) 0.0467(7) 0.0265(5) 0.0031(5) 0.0118(5) 0.0107(5) S4 0.0402(7) 0.0321(6) 0.0331(6) 0.0066(5) 0.0164(5) 0.0145(5) S5 0.0403(7) 0.0331(6) 0.0338(6) 0.0030(5) 0.0164(5) 0.0135(5) S6 0.0270(5) 0.0301(6) 0.0229(5) 0.0024(4) 0.0096(4) 0.0073(4) S7 0.0641(9) 0.0272(6) 0.0322(6) 0.0049(5) 0.0219(6) 0.0089(6) F1 0.055(2) 0.042(2) 0.120(4) -0.002(2) -0.007(2) -0.0042(18) F2 0.048(2) 0.093(3) 0.072(3) 0.003(2) 0.0157(19) 0.040(2) F3' 0.141(9) 0.050(5) 0.121(8) 0.016(5) 0.094(7) -0.012(5) F3 0.167(11) 0.085(7) 0.052(5) 0.007(4) 0.062(6) 0.010(7) F4 0.130(5) 0.034(2) 0.178(6) -0.009(3) 0.060(4) -0.004(3) F5 0.107(4) 0.077(3) 0.080(3) -0.028(2) 0.058(3) 0.014(3) F6 0.093(3) 0.119(4) 0.074(3) 0.022(3) 0.016(3) 0.076(3) O1 0.032(2) 0.072(3) 0.064(3) 0.025(2) 0.0265(19) 0.0084(19) O2 0.0380(18) 0.0246(17) 0.0372(18) 0.0105(14) 0.0125(15) 0.0100(14) O3 0.0289(17) 0.0324(18) 0.0310(18) 0.0017(14) 0.0053(14) 0.0046(14) N1 0.037(3) 0.087(4) 0.113(5) 0.051(4) 0.043(3) 0.017(3) N2 0.031(2) 0.0223(19) 0.039(2) 0.0106(16) 0.0112(17) 0.0079(16) N3 0.052(3) 0.046(3) 0.036(2) -0.006(2) -0.006(2) 0.023(2) C1 0.043(3) 0.059(4) 0.051(3) 0.021(3) 0.027(3) 0.021(3) C3 0.041(4) 0.116(7) 0.110(7) 0.020(6) 0.034(4) 0.015(4) C4 0.029(2) 0.027(2) 0.029(2) 0.0048(18) 0.0100(19) 0.0098(19) C5 0.043(3) 0.028(3) 0.064(4) 0.014(3) 0.014(3) 0.009(2) C6 0.035(3) 0.037(3) 0.044(3) 0.015(2) 0.008(2) 0.011(2) C7 0.033(3) 0.033(3) 0.035(3) 0.007(2) 0.004(2) 0.014(2) C8 0.118(7) 0.116(7) 0.034(3) 0.000(4) 0.007(4) 0.072(6) C9 0.047(4) 0.041(4) 0.093(6) -0.003(3) -0.016(4) 0.006(3) C11 0.029(2) 0.023(2) 0.033(2) 0.0040(18) 0.0038(19) 0.0131(19) C12 0.034(3) 0.029(3) 0.061(4) 0.010(2) 0.008(3) 0.012(2) C13 0.043(3) 0.028(3) 0.076(4) -0.001(3) -0.012(3) 0.012(3) C14 0.075(5) 0.050(4) 0.048(4) -0.008(3) -0.007(3) 0.034(4) C15 0.072(4) 0.067(4) 0.033(3) 0.002(3) 0.010(3) 0.036(4) C16 0.046(3) 0.047(3) 0.029(2) 0.007(2) 0.011(2) 0.022(3) C21 0.031(2) 0.023(2) 0.033(2) 0.0073(18) 0.010(2) 0.0075(18) C22 0.033(2) 0.034(3) 0.032(2) 0.002(2) 0.008(2) 0.011(2) C23 0.033(3) 0.035(3) 0.052(3) 0.000(2) 0.008(2) 0.011(2) C24 0.047(3) 0.046(3) 0.047(3) 0.014(3) -0.001(3) 0.017(3) C25 0.073(5) 0.093(5) 0.042(3) 0.036(4) 0.023(3) 0.036(4) C26 0.057(4) 0.075(4) 0.044(3) 0.029(3) 0.027(3) 0.027(3) C31 0.031(2) 0.047(3) 0.034(3) 0.011(2) 0.015(2) 0.013(2) C32 0.055(3) 0.051(3) 0.035(3) 0.010(2) 0.023(3) 0.014(3) C33 0.078(5) 0.083(5) 0.044(3) 0.019(3) 0.034(3) 0.024(4) C34 0.082(5) 0.086(6) 0.068(5) 0.036(4) 0.047(4) 0.014(4) C35 0.089(6) 0.075(5) 0.073(5) 0.022(4) 0.043(5) -0.002(4) C36 0.062(4) 0.055(4) 0.058(4) 0.003(3) 0.032(3) -0.001(3) C41 0.031(2) 0.044(3) 0.028(2) 0.004(2) 0.014(2) 0.005(2) C42 0.038(3) 0.040(3) 0.057(3) -0.008(3) 0.016(3) 0.000(2) C43 0.074(5) 0.044(4) 0.085(5) -0.013(3) 0.039(4) -0.010(3) C44 0.049(4) 0.087(6) 0.078(5) -0.020(4) 0.024(4) -0.032(4) C45 0.037(4) 0.122(8) 0.069(5) 0.004(5) 0.005(3) -0.003(4) C46 0.041(3) 0.082(5) 0.052(4) 0.013(3) 0.008(3) 0.016(3) C51 0.024(2) 0.036(3) 0.035(2) -0.001(2) 0.014(2) 0.0034(19) C52 0.038(3) 0.042(3) 0.050(3) -0.005(2) 0.023(2) 0.007(2) C53 0.049(3) 0.057(4) 0.051(3) -0.017(3) 0.027(3) 0.007(3) C54 0.064(4) 0.087(5) 0.041(3) 0.000(3) 0.032(3) 0.022(4) C55 0.086(5) 0.072(5) 0.059(4) 0.025(3) 0.051(4) 0.031(4) C56 0.067(4) 0.042(3) 0.048(3) 0.004(2) 0.038(3) 0.015(3) C61 0.036(3) 0.039(3) 0.027(2) 0.0078(19) 0.016(2) 0.018(2) C62 0.043(3) 0.056(3) 0.033(3) 0.002(2) 0.012(2) 0.025(3) C63 0.066(4) 0.077(5) 0.040(3) 0.018(3) 0.019(3) 0.052(4) C64 0.093(5) 0.059(4) 0.048(3) 0.023(3) 0.038(4) 0.053(4) C65 0.080(4) 0.041(3) 0.047(3) 0.013(3) 0.032(3) 0.026(3) C66 0.050(3) 0.035(3) 0.032(2) 0.009(2) 0.016(2) 0.016(2) N4 0.038(3) 0.039(3) 0.034(3) 0.002(3) 0.015(3) 0.007(3) O4 0.015(3) 0.035(3) 0.023(3) 0.004(3) 0.005(2) -0.004(3) O5 0.030(3) 0.024(3) 0.023(3) 0.008(3) -0.004(3) 0.006(3) O6 0.020(3) 0.027(3) 0.038(3) 0.019(3) 0.011(3) 0.003(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 O3 2.320(3) . ? Cd1 O5 2.393(6) 2_766 ? Cd1 O4 2.397(6) . ? Cd1 S2 2.5234(12) . ? Cd1 S4 2.5520(13) . ? Cd1 S1 2.5535(11) . ? Cd2 O2 2.314(3) . ? Cd2 O6 2.327(6) . ? Cd2 O5 2.362(6) 2_766 ? Cd2 S6 2.5526(11) . ? Cd2 S3 2.5551(12) . ? Cd2 S2 2.5719(12) . ? Cd3 O1 2.315(4) . ? Cd3 O6 2.340(6) 2_766 ? Cd3 O4 2.353(6) . ? Cd3 S4 2.5484(12) . ? Cd3 S7 2.5645(13) . ? Cd3 S3 2.5854(13) 2_766 ? Cd4 S5 2.4763(12) . ? Cd4 S7 2.5622(13) . ? Cd4 S6 2.5871(11) . ? Cd4 S1 2.5909(11) 2_766 ? S1 C11 1.786(3) . ? S1 Cd4 2.5909(11) 2_766 ? S2 C21 1.786(2) . ? S3 C31 1.785(3) . ? S3 Cd3 2.5854(13) 2_766 ? S4 C41 1.764(3) . ? S5 C51 1.778(3) . ? S6 C61 1.797(3) . ? S7 C71 1.820(6) . ? F1 C13 1.289(5) . ? F2 C23 1.308(5) . ? F3' C35 1.244(9) . ? F3 C33 1.233(9) . ? F4 C43 1.320(6) . ? F5 C53 1.321(5) . ? F6 C63 1.310(5) . ? O1 C1 1.197(7) . ? O2 C4 1.232(6) . ? O3 C7 1.232(6) . ? N1 C1 1.311(8) . ? N1 C2 1.417(19) . ? N1 C3 1.453(9) . ? N2 C4 1.316(6) . ? N2 C6 1.452(6) . ? N2 C5 1.462(6) . ? N3 C7 1.305(7) . ? N3 C9 1.442(10) . ? N3 C8 1.456(9) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C75 C76 1.3900 . ? N4 O5 1.258(5) . ? N4 O5 1.258(5) 2_766 ? N4 O4 1.297(5) 2_766 ? N4 O4 1.297(5) . ? N4 O6 1.324(5) . ? N4 O6 1.324(5) 2_766 ? O4 O5 1.225(9) 2_766 ? O4 O6 1.397(8) 2_766 ? O5 O4 1.225(9) 2_766 ? O5 O6 1.298(8) 2_766 ? O5 Cd2 2.362(6) 2_766 ? O5 Cd1 2.393(6) 2_766 ? O6 O5 1.298(8) 2_766 ? O6 O4 1.397(8) 2_766 ? O6 Cd3 2.340(6) 2_766 ? N5 O9 1.347(18) 2_767 ? N5 O9 1.347(18) . ? N5 O8 1.392(13) . ? N5 O8 1.392(13) 2_767 ? N5 O7 1.405(19) 2_767 ? N5 O7 1.405(18) . ? O7 O8 1.50(4) 2_767 ? O7 O9 1.53(4) 2_767 ? O8 O9 1.50(4) 2_767 ? O8 O7 1.50(4) 2_767 ? O9 O8 1.50(4) 2_767 ? O9 O7 1.53(4) 2_767 ? 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 O5 167.55(16) . 2_766 ? O3 Cd1 O4 160.76(16) . . ? O5 Cd1 O4 29.6(2) 2_766 . ? O3 Cd1 S2 93.11(9) . . ? O5 Cd1 S2 74.75(15) 2_766 . ? O4 Cd1 S2 103.61(15) . . ? O3 Cd1 S4 89.77(9) . . ? O5 Cd1 S4 95.07(17) 2_766 . ? O4 Cd1 S4 72.83(14) . . ? S2 Cd1 S4 125.58(4) . . ? O3 Cd1 S1 97.01(9) . . ? O5 Cd1 S1 91.43(15) 2_766 . ? O4 Cd1 S1 83.30(16) . . ? S2 Cd1 S1 119.04(4) . . ? S4 Cd1 S1 114.44(4) . . ? O2 Cd2 O6 167.32(17) . . ? O2 Cd2 O5 157.17(16) . 2_766 ? O6 Cd2 O5 32.1(2) . 2_766 ? O2 Cd2 S6 93.30(9) . . ? O6 Cd2 S6 97.53(16) . . ? O5 Cd2 S6 84.44(18) 2_766 . ? O2 Cd2 S3 94.77(9) . . ? O6 Cd2 S3 74.21(14) . . ? O5 Cd2 S3 106.21(15) 2_766 . ? S6 Cd2 S3 119.05(4) . . ? O2 Cd2 S2 86.21(9) . . ? O6 Cd2 S2 95.10(17) . . ? O5 Cd2 S2 74.36(15) 2_766 . ? S6 Cd2 S2 115.02(4) . . ? S3 Cd2 S2 125.74(4) . . ? O1 Cd3 O6 155.36(17) . 2_766 ? O1 Cd3 O4 168.61(17) . . ? O6 Cd3 O4 34.6(2) 2_766 . ? O1 Cd3 S4 95.15(11) . . ? O6 Cd3 S4 107.17(15) 2_766 . ? O4 Cd3 S4 73.60(14) . . ? O1 Cd3 S7 94.22(12) . . ? O6 Cd3 S7 85.45(17) 2_766 . ? O4 Cd3 S7 92.44(15) . . ? S4 Cd3 S7 115.94(4) . . ? O1 Cd3 S3 85.37(11) . 2_766 ? O6 Cd3 S3 73.42(15) 2_766 2_766 ? O4 Cd3 S3 99.48(16) . 2_766 ? S4 Cd3 S3 125.06(4) . 2_766 ? S7 Cd3 S3 118.80(4) . 2_766 ? S5 Cd4 S7 118.98(5) . . ? S5 Cd4 S6 101.74(4) . . ? S7 Cd4 S6 108.42(4) . . ? S5 Cd4 S1 112.65(4) . 2_766 ? S7 Cd4 S1 108.47(4) . 2_766 ? S6 Cd4 S1 105.49(4) . 2_766 ? C11 S1 Cd1 100.87(11) . . ? C11 S1 Cd4 104.21(11) . 2_766 ? Cd1 S1 Cd4 117.05(4) . 2_766 ? C21 S2 Cd1 103.89(12) . . ? C21 S2 Cd2 104.56(12) . . ? Cd1 S2 Cd2 94.20(4) . . ? C31 S3 Cd2 105.35(13) . . ? C31 S3 Cd3 103.33(13) . 2_766 ? Cd2 S3 Cd3 92.94(4) . 2_766 ? C41 S4 Cd3 106.57(13) . . ? C41 S4 Cd1 104.44(13) . . ? Cd3 S4 Cd1 93.23(4) . . ? C51 S5 Cd4 111.74(12) . . ? C61 S6 Cd2 99.98(12) . . ? C61 S6 Cd4 105.21(11) . . ? Cd2 S6 Cd4 112.24(4) . . ? C71 S7 Cd4 105.1(2) . . ? C71 S7 Cd3 99.7(2) . . ? Cd4 S7 Cd3 114.71(5) . . ? C1 O1 Cd3 129.1(4) . . ? C4 O2 Cd2 127.5(3) . . ? C7 O3 Cd1 126.9(3) . . ? C1 N1 C2 119.6(10) . . ? C1 N1 C3 121.8(6) . . ? C2 N1 C3 118.6(10) . . ? C4 N2 C6 121.0(4) . . ? C4 N2 C5 121.1(4) . . ? C6 N2 C5 117.7(4) . . ? C7 N3 C9 119.9(6) . . ? C7 N3 C8 122.0(7) . . ? C9 N3 C8 118.1(6) . . ? O1 C1 N1 127.3(6) . . ? O2 C4 N2 124.7(4) . . ? O3 C7 N3 125.7(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 S1 118.95(19) . . ? C16 C11 S1 121.01(19) . . ? C13 C12 C11 120.0 . . ? F1 C13 C12 121.4(4) . . ? F1 C13 C14 118.6(4) . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 S2 122.45(18) . . ? C26 C21 S2 117.53(18) . . ? C23 C22 C21 120.0 . . ? F2 C23 C22 120.1(3) . . ? F2 C23 C24 119.9(3) . . ? C22 C23 C24 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 S3 122.3(2) . . ? C36 C31 S3 117.7(2) . . ? C33 C32 C31 120.0 . . ? F3 C33 C32 124.4(5) . . ? F3 C33 C34 115.4(5) . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? F3' C35 C34 116.2(6) . . ? F3' C35 C36 122.8(6) . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 S4 122.9(2) . . ? C46 C41 S4 117.0(2) . . ? C41 C42 C43 120.0 . . ? F4 C43 C44 121.1(4) . . ? F4 C43 C42 118.9(4) . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 S5 116.45(19) . . ? C56 C51 S5 123.55(19) . . ? C53 C52 C51 120.0 . . ? F5 C53 C52 120.4(3) . . ? F5 C53 C54 119.6(3) . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 S6 117.63(18) . . ? C66 C61 S6 122.37(18) . . ? C63 C62 C61 120.0 . . ? F6 C63 C64 118.5(4) . . ? F6 C63 C62 121.4(4) . . ? C64 C63 C62 120.0 . . ? C63 C64 C65 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 S7 122.1(5) . . ? C76 C71 S7 117.9(5) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C75 C74 C73 120.0 . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? O5 N4 O5 180.000(2) . 2_766 ? O5 N4 O4 57.3(4) . 2_766 ? O5 N4 O4 122.7(4) 2_766 2_766 ? O5 N4 O4 122.7(4) . . ? O5 N4 O4 57.3(4) 2_766 . ? O4 N4 O4 180.000(1) 2_766 . ? O5 N4 O6 119.7(4) . . ? O5 N4 O6 60.3(4) 2_766 . ? O4 N4 O6 64.5(4) 2_766 . ? O4 N4 O6 115.5(4) . . ? O5 N4 O6 60.3(4) . 2_766 ? O5 N4 O6 119.7(4) 2_766 2_766 ? O4 N4 O6 115.5(4) 2_766 2_766 ? O4 N4 O6 64.5(4) . 2_766 ? O6 N4 O6 180.0(4) . 2_766 ? O5 O4 N4 59.8(4) 2_766 . ? O5 O4 O6 116.6(5) 2_766 2_766 ? N4 O4 O6 58.7(3) . 2_766 ? O5 O4 Cd3 170.1(5) 2_766 . ? N4 O4 Cd3 127.0(4) . . ? O6 O4 Cd3 72.2(3) 2_766 . ? O5 O4 Cd1 75.0(4) 2_766 . ? N4 O4 Cd1 124.9(4) . . ? O6 O4 Cd1 133.7(5) 2_766 . ? Cd3 O4 Cd1 102.6(2) . . ? O4 O5 N4 62.9(4) 2_766 . ? O4 O5 O6 122.9(6) 2_766 2_766 ? N4 O5 O6 62.4(4) . 2_766 ? O4 O5 Cd2 138.8(5) 2_766 2_766 ? N4 O5 Cd2 128.8(4) . 2_766 ? O6 O5 Cd2 72.4(4) 2_766 2_766 ? O4 O5 Cd1 75.3(4) 2_766 2_766 ? N4 O5 Cd1 127.5(4) . 2_766 ? O6 O5 Cd1 157.3(6) 2_766 2_766 ? Cd2 O5 Cd1 103.4(2) 2_766 2_766 ? O5 O6 N4 57.4(3) 2_766 . ? O5 O6 O4 112.6(5) 2_766 2_766 ? N4 O6 O4 56.8(3) . 2_766 ? O5 O6 Cd2 75.4(4) 2_766 . ? N4 O6 Cd2 127.2(4) . . ? O4 O6 Cd2 167.2(5) 2_766 . ? O5 O6 Cd3 146.6(5) 2_766 2_766 ? N4 O6 Cd3 126.2(4) . 2_766 ? O4 O6 Cd3 73.2(3) 2_766 2_766 ? Cd2 O6 Cd3 106.0(2) . 2_766 ? O9 N5 O9 180.00(2) 2_767 . ? O9 N5 O8 66.2(17) 2_767 . ? O9 N5 O8 113.8(17) . . ? O9 N5 O8 113.8(17) 2_767 2_767 ? O9 N5 O8 66.2(17) . 2_767 ? O8 N5 O8 180.000(7) . 2_767 ? O9 N5 O7 112.5(19) 2_767 2_767 ? O9 N5 O7 67.5(19) . 2_767 ? O8 N5 O7 64.9(18) . 2_767 ? O8 N5 O7 115.1(18) 2_767 2_767 ? O9 N5 O7 67.5(19) 2_767 . ? O9 N5 O7 112.5(19) . . ? O8 N5 O7 115.1(18) . . ? O8 N5 O7 64.9(18) 2_767 . ? O7 N5 O7 180.0(15) 2_767 . ? N5 O7 O8 57.2(12) . 2_767 ? N5 O7 O9 54.5(12) . 2_767 ? O8 O7 O9 98(2) 2_767 2_767 ? N5 O8 O9 55.4(11) . 2_767 ? N5 O8 O7 58.0(12) . 2_767 ? O9 O8 O7 100(2) 2_767 2_767 ? N5 O9 O8 58.3(12) . 2_767 ? N5 O9 O7 58.1(13) . 2_767 ? O8 O9 O7 103(2) 2_767 2_767 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.212 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.115