# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_general _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'JPLang.cif' _audit_creation_date 2011-12-02 _audit_creation_method 'SHELXL 97' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email jplang@suda.edu.cn _publ_contact_author_fax 86-512-65880089 _publ_contact_author_phone 86-512-65882865 _publ_contact_author_address ; College of Chemistry and Chemical Engineering, Materials Science Soochow University, Suzhou 215123, Jiangsu, P. R. China ; _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_footnote _publ_author_address ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; loop_ _publ_author_name 'Xiaoyan Tang' 'Rongxin Yuan' 'Jin-Xiang Chen' 'Ai-Xia Zheng' 'Miao Yu' ; Hong-Xi Li ; 'Zhi-Gang Ren' 'Jian-Ping Lang' #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 294977' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(4-(trimethylammonio)benzenethiolate)-cadmium(II) dihexafluorophosphate hydrate ; _chemical_name_common ; Tetrakis(4-(trimethylammonio)benzenethiolate)-cadmium(ii) dihexafluorophosphate hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Cd N4 S4, 2(F6 P), H2 O' _chemical_formula_sum 'C36 H54 Cd F12 N4 O P2 S4' _chemical_formula_weight 1089.46 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' P P 0.1023 0.0942 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 13.984(3) _cell_length_b 34.339(7) _cell_length_c 10.048(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4825.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 15754 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6632 _exptl_absorpt_correction_T_max 0.9131 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Rigaku Mercury' _diffrn_measurement_method \w _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 41607 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8681 _reflns_number_gt 8142 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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. The distance between H atom and O atom of the water molecule was fixed to be 0.82 \%A. The U~ij~ values of all H atoms of water molecules were restrained to be equal. The U~ij~ values of Zn1 and S1 atoms, N1 and C4 atoms, N4, C34, C35 and C36 atoms were restrained by the EADP instruction. ; _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^)+(0.0501P)^2^+12.5961P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3912, Friedel pairs' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 8681 _refine_ls_number_parameters 574 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.111 _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 0.50633(3) 0.109105(13) 0.34179(6) 0.03256(12) Uani 1 1 d . . . S1 S 0.57108(12) 0.04264(5) 0.2889(2) 0.0482(5) Uani 1 1 d . . . S2 S 0.60051(12) 0.14866(6) 0.51115(18) 0.0427(4) Uani 1 1 d . . . S3 S 0.51818(11) 0.14248(4) 0.11376(16) 0.0301(3) Uani 1 1 d . . . S4 S 0.33631(12) 0.12099(8) 0.4188(2) 0.0560(6) Uani 1 1 d . . . P1 P 0.98349(12) 0.00187(6) 0.13706(18) 0.0367(4) Uani 1 1 d . . . P2 P 0.51138(14) 0.33163(6) -0.0532(2) 0.0438(5) Uani 1 1 d . . . O1 O 0.4260(16) 0.7529(4) 0.0423(12) 0.117(8) Uani 0.50 1 d PD . . H37 H 0.381(5) 0.748(4) 0.092(11) 0.025 Uiso 0.50 1 d PD . . H38 H 0.410(8) 0.771(3) -0.006(11) 0.050 Uiso 0.50 1 d PD . . O2 O 0.2165(13) 0.7168(4) 0.0617(18) 0.097(5) Uani 0.50 1 d PD . . H39 H 0.170(7) 0.725(5) 0.103(10) 0.045 Uiso 0.50 1 d PD . . H40 H 0.247(7) 0.703(3) 0.113(9) 0.028 Uiso 0.50 1 d PD . . F1 F 0.9095(3) 0.02461(15) 0.2307(5) 0.0597(12) Uani 1 1 d . . . F2 F 0.9984(3) 0.03985(14) 0.0479(5) 0.0577(12) Uani 1 1 d . . . F3 F 1.0560(3) -0.02232(14) 0.0464(5) 0.0531(11) Uani 1 1 d . . . F4 F 0.8954(3) -0.01035(12) 0.0447(4) 0.0461(10) Uani 1 1 d . . . F5 F 1.0714(3) 0.01464(13) 0.2301(4) 0.0477(10) Uani 1 1 d . . . F6 F 0.9674(3) -0.03601(13) 0.2264(5) 0.0548(12) Uani 1 1 d . . . F7 F 0.6073(3) 0.33358(16) 0.0296(6) 0.0720(15) Uani 1 1 d . . . F8 F 0.5366(5) 0.37039(14) -0.1282(5) 0.0778(16) Uani 1 1 d . . . F9 F 0.4846(3) 0.29323(14) 0.0233(6) 0.0711(15) Uani 1 1 d . . . F10 F 0.4580(4) 0.35614(14) 0.0596(5) 0.0631(13) Uani 1 1 d . . . F11 F 0.5637(4) 0.30706(15) -0.1647(7) 0.0843(16) Uani 1 1 d . . . F12 F 0.4140(4) 0.32881(17) -0.1333(6) 0.0917(19) Uani 1 1 d . . . N1 N 0.2608(3) -0.07819(15) 0.3775(5) 0.0317(13) Uani 1 1 d . . . N2 N 1.0276(4) 0.13127(19) 0.4300(5) 0.0382(14) Uani 1 1 d . . . N3 N 0.2214(4) 0.27064(16) 0.1210(6) 0.0392(14) Uani 1 1 d . . . N4 N 0.2872(3) 0.05783(15) 0.9766(5) 0.0274(11) Uani 1 1 d . . . C1 C 0.4786(4) 0.00840(17) 0.3107(6) 0.0326(16) Uani 1 1 d . . . C2 C 0.4053(6) 0.0145(2) 0.3997(7) 0.051(2) Uani 1 1 d . . . H2 H 0.4023 0.0384 0.4474 0.061 Uiso 1 1 calc R . . C3 C 0.3355(6) -0.0138(2) 0.4210(8) 0.055(2) Uani 1 1 d . . . H3 H 0.2859 -0.0092 0.4837 0.067 Uiso 1 1 calc R . . C4 C 0.3380(4) -0.04815(17) 0.3520(7) 0.0297(12) Uani 1 1 d . . . C5 C 0.4071(5) -0.0540(2) 0.2595(8) 0.0446(18) Uani 1 1 d . . . H5 H 0.4077 -0.0770 0.2069 0.053 Uiso 1 1 calc R . . C6 C 0.4775(5) -0.0254(2) 0.2429(9) 0.0477(19) Uani 1 1 d . . . H6 H 0.5272 -0.0302 0.1805 0.057 Uiso 1 1 calc R . . C7 C 0.1726(5) -0.0670(3) 0.3019(10) 0.070(3) Uani 1 1 d U . . H7A H 0.1189 -0.0832 0.3309 0.105 Uiso 1 1 calc R . . H7B H 0.1835 -0.0708 0.2065 0.105 Uiso 1 1 calc R . . H7C H 0.1577 -0.0395 0.3190 0.105 Uiso 1 1 calc R . . C8 C 0.2914(5) -0.11727(18) 0.3362(9) 0.0456(16) Uani 1 1 d . . . H8A H 0.2405 -0.1360 0.3554 0.068 Uiso 1 1 calc R . . H8B H 0.3493 -0.1246 0.3852 0.068 Uiso 1 1 calc R . . H8C H 0.3049 -0.1173 0.2405 0.068 Uiso 1 1 calc R . . C9 C 0.2367(6) -0.0806(2) 0.5218(8) 0.049(2) Uani 1 1 d . . . H9A H 0.2955 -0.0842 0.5735 0.074 Uiso 1 1 calc R . . H9B H 0.1938 -0.1027 0.5371 0.074 Uiso 1 1 calc R . . H9C H 0.2051 -0.0564 0.5496 0.074 Uiso 1 1 calc R . . C10 C 0.7232(4) 0.1425(2) 0.4809(6) 0.0340(15) Uani 1 1 d . . . C11 C 0.7874(5) 0.1711(3) 0.5310(8) 0.0477(19) Uani 1 1 d . . . H11 H 0.7632 0.1932 0.5764 0.057 Uiso 1 1 calc R . . C12 C 0.8853(5) 0.1666(2) 0.5139(8) 0.0481(19) Uani 1 1 d . . . H12 H 0.9278 0.1855 0.5497 0.058 Uiso 1 1 calc R . . C13 C 0.9211(4) 0.1351(2) 0.4455(6) 0.0368(16) Uani 1 1 d . . . C14 C 0.8600(5) 0.1067(2) 0.3948(7) 0.0375(16) Uani 1 1 d . . . H14 H 0.8848 0.0845 0.3499 0.045 Uiso 1 1 calc R . . C15 C 0.7622(5) 0.1114(2) 0.4115(7) 0.0368(15) Uani 1 1 d . . . H15 H 0.7203 0.0926 0.3738 0.044 Uiso 1 1 calc R . . C16 C 1.0670(5) 0.1664(2) 0.3639(8) 0.0456(18) Uani 1 1 d . . . H16A H 1.0444 0.1674 0.2716 0.068 Uiso 1 1 calc R . . H16B H 1.1370 0.1652 0.3649 0.068 Uiso 1 1 calc R . . H16C H 1.0457 0.1897 0.4114 0.068 Uiso 1 1 calc R . . C17 C 1.0569(4) 0.0960(2) 0.3547(8) 0.0418(16) Uani 1 1 d . . . H17A H 1.0318 0.0974 0.2638 0.063 Uiso 1 1 calc R . . H17B H 1.0313 0.0727 0.3989 0.063 Uiso 1 1 calc R . . H17C H 1.1268 0.0944 0.3520 0.063 Uiso 1 1 calc R . . C18 C 1.0715(5) 0.1287(3) 0.5677(7) 0.054(2) Uani 1 1 d . . . H18A H 1.1413 0.1294 0.5604 0.081 Uiso 1 1 calc R . . H18B H 1.0518 0.1043 0.6102 0.081 Uiso 1 1 calc R . . H18C H 1.0496 0.1508 0.6216 0.081 Uiso 1 1 calc R . . C19 C 0.4332(5) 0.18024(16) 0.1180(6) 0.0300(14) Uani 1 1 d . . . C20 C 0.3906(6) 0.1921(2) 0.0004(8) 0.0498(19) Uani 1 1 d . . . H20 H 0.4095 0.1805 -0.0812 0.060 Uiso 1 1 calc R . . C21 C 0.3203(6) 0.2211(2) 0.0000(8) 0.054(2) Uani 1 1 d . . . H21 H 0.2896 0.2282 -0.0808 0.065 Uiso 1 1 calc R . . C22 C 0.2955(5) 0.23925(19) 0.1179(7) 0.0332(14) Uani 1 1 d . . . C23 C 0.3388(5) 0.2291(2) 0.2307(7) 0.0418(17) Uani 1 1 d . . . H23 H 0.3230 0.2422 0.3109 0.050 Uiso 1 1 calc R . . C24 C 0.4068(5) 0.1995(2) 0.2328(7) 0.0418(16) Uani 1 1 d . . . H24 H 0.4356 0.1924 0.3149 0.050 Uiso 1 1 calc R . . C25 C 0.1764(6) 0.2788(2) -0.0128(8) 0.0506(19) Uani 1 1 d . . . H25A H 0.1479 0.2548 -0.0478 0.076 Uiso 1 1 calc R . . H25B H 0.2255 0.2881 -0.0747 0.076 Uiso 1 1 calc R . . H25C H 0.1267 0.2987 -0.0028 0.076 Uiso 1 1 calc R . . C26 C 0.1414(5) 0.2599(2) 0.2131(9) 0.054(2) Uani 1 1 d . . . H26A H 0.1674 0.2464 0.2911 0.081 Uiso 1 1 calc R . . H26B H 0.0965 0.2427 0.1668 0.081 Uiso 1 1 calc R . . H26C H 0.1081 0.2836 0.2418 0.081 Uiso 1 1 calc R . . C27 C 0.2649(5) 0.3083(2) 0.1665(9) 0.048(2) Uani 1 1 d . . . H27A H 0.3209 0.3144 0.1116 0.072 Uiso 1 1 calc R . . H27B H 0.2845 0.3060 0.2598 0.072 Uiso 1 1 calc R . . H27C H 0.2178 0.3293 0.1579 0.072 Uiso 1 1 calc R . . C28 C 0.3307(4) 0.1002(2) 0.5793(7) 0.0380(17) Uani 1 1 d . . . C29 C 0.2692(4) 0.0699(2) 0.6073(7) 0.0425(18) Uani 1 1 d . . . H29 H 0.2337 0.0588 0.5361 0.051 Uiso 1 1 calc R . . C30 C 0.2565(5) 0.0548(2) 0.7325(7) 0.0356(15) Uani 1 1 d . . . H30 H 0.2146 0.0335 0.7467 0.043 Uiso 1 1 calc R . . C31 C 0.3048(3) 0.07104(16) 0.8362(7) 0.0245(11) Uani 1 1 d . . . C32 C 0.3684(4) 0.10128(18) 0.8135(7) 0.0335(15) Uani 1 1 d . . . H32 H 0.4035 0.1122 0.8853 0.040 Uiso 1 1 calc R . . C33 C 0.3805(5) 0.1156(2) 0.6857(6) 0.0355(15) Uani 1 1 d . . . H33 H 0.4239 0.1364 0.6709 0.043 Uiso 1 1 calc R . . C34 C 0.3791(5) 0.0507(2) 1.0457(8) 0.0490(19) Uani 1 1 d . . . H34A H 0.4179 0.0745 1.0438 0.074 Uiso 1 1 calc R . . H34B H 0.4136 0.0296 1.0006 0.074 Uiso 1 1 calc R . . H34C H 0.3666 0.0433 1.1382 0.074 Uiso 1 1 calc R . . C35 C 0.2339(8) 0.0888(3) 1.0503(9) 0.080(3) Uani 1 1 d . . . H35A H 0.1733 0.0941 1.0049 0.119 Uiso 1 1 calc R . . H35B H 0.2725 0.1126 1.0530 0.119 Uiso 1 1 calc R . . H35C H 0.2211 0.0800 1.1413 0.119 Uiso 1 1 calc R . . C36 C 0.2305(6) 0.0209(3) 0.9813(8) 0.062(2) Uani 1 1 d . . . H36A H 0.2599 0.0016 0.9225 0.092 Uiso 1 1 calc R . . H36B H 0.1649 0.0261 0.9518 0.092 Uiso 1 1 calc R . . H36C H 0.2295 0.0109 1.0727 0.092 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 0.01823(18) 0.0445(2) 0.0349(2) 0.0130(2) -0.0009(2) -0.00197(18) S1 0.0216(8) 0.0379(9) 0.0852(14) 0.0200(9) -0.0007(8) -0.0005(7) S2 0.0226(8) 0.0680(12) 0.0375(9) -0.0050(9) -0.0010(7) 0.0071(8) S3 0.0304(8) 0.0279(7) 0.0321(8) 0.0048(6) 0.0037(7) 0.0009(6) S4 0.0224(8) 0.1032(17) 0.0425(10) 0.0360(11) 0.0047(8) 0.0063(9) P1 0.0255(9) 0.0462(10) 0.0385(10) 0.0005(9) 0.0013(7) -0.0023(7) P2 0.0440(11) 0.0431(10) 0.0444(11) 0.0076(9) -0.0022(9) 0.0069(8) O1 0.27(2) 0.046(7) 0.034(7) 0.006(6) 0.014(10) 0.070(12) O2 0.122(15) 0.061(9) 0.108(13) 0.035(9) 0.001(11) 0.012(9) F1 0.037(2) 0.080(3) 0.063(3) -0.013(3) 0.001(2) 0.008(2) F2 0.049(3) 0.058(3) 0.066(3) 0.020(2) -0.008(2) -0.015(2) F3 0.029(2) 0.067(3) 0.063(3) -0.011(2) 0.010(2) -0.006(2) F4 0.0298(19) 0.061(3) 0.048(2) 0.004(2) -0.0033(18) -0.0072(18) F5 0.035(2) 0.058(3) 0.050(2) -0.006(2) -0.0094(19) -0.0064(19) F6 0.037(2) 0.060(3) 0.067(3) 0.020(2) -0.001(2) -0.006(2) F7 0.047(3) 0.085(4) 0.085(4) 0.025(3) -0.011(3) -0.008(3) F8 0.124(5) 0.055(3) 0.055(3) 0.021(2) 0.011(3) 0.004(3) F9 0.052(3) 0.048(3) 0.113(5) 0.023(3) 0.014(3) 0.001(2) F10 0.072(3) 0.063(3) 0.055(3) 0.000(2) 0.003(3) 0.013(3) F11 0.103(4) 0.069(3) 0.080(4) -0.010(3) 0.030(4) 0.023(3) F12 0.082(4) 0.099(4) 0.094(5) -0.021(4) -0.047(3) 0.026(3) N1 0.025(3) 0.032(3) 0.037(3) 0.006(2) -0.004(2) -0.008(2) N2 0.021(3) 0.066(4) 0.027(3) -0.001(3) 0.001(2) -0.004(3) N3 0.028(3) 0.033(3) 0.057(4) 0.007(3) -0.001(3) 0.002(2) N4 0.024(3) 0.033(3) 0.024(3) 0.001(2) 0.005(2) 0.003(2) C1 0.024(3) 0.029(3) 0.044(4) 0.018(3) -0.010(3) 0.005(2) C2 0.069(5) 0.053(5) 0.030(4) -0.013(3) 0.011(3) -0.030(4) C3 0.069(5) 0.054(5) 0.043(4) -0.016(4) 0.022(4) -0.040(4) C4 0.023(3) 0.034(3) 0.032(3) 0.010(3) 0.000(3) -0.004(2) C5 0.041(4) 0.034(3) 0.059(5) -0.010(3) 0.016(4) -0.004(3) C6 0.036(4) 0.030(3) 0.078(6) 0.004(4) 0.019(4) 0.003(3) C7 0.037(4) 0.062(5) 0.111(8) 0.034(5) -0.038(4) -0.018(4) C8 0.046(4) 0.035(4) 0.056(4) -0.004(4) 0.009(4) -0.010(3) C9 0.053(5) 0.048(4) 0.047(4) 0.000(4) 0.029(4) -0.013(4) C10 0.019(3) 0.055(4) 0.028(3) 0.005(3) 0.001(2) 0.001(3) C11 0.031(4) 0.071(5) 0.041(4) -0.014(4) 0.002(3) 0.005(4) C12 0.023(3) 0.069(5) 0.052(5) -0.013(4) -0.002(3) -0.007(3) C13 0.022(3) 0.061(5) 0.027(3) 0.000(3) 0.000(3) 0.002(3) C14 0.025(3) 0.052(4) 0.036(4) -0.006(3) -0.002(3) 0.003(3) C15 0.027(3) 0.049(4) 0.034(4) 0.001(3) -0.005(3) 0.008(3) C16 0.033(3) 0.056(4) 0.047(5) 0.006(4) 0.010(3) -0.011(3) C17 0.025(3) 0.064(4) 0.036(4) -0.003(4) 0.000(3) 0.005(3) C18 0.023(3) 0.108(7) 0.032(4) 0.008(4) -0.010(3) 0.002(4) C19 0.038(3) 0.019(3) 0.033(3) 0.002(3) -0.001(3) -0.002(2) C20 0.075(5) 0.036(4) 0.038(4) -0.002(3) -0.013(4) 0.019(4) C21 0.075(6) 0.040(4) 0.048(5) -0.017(4) -0.022(4) 0.021(4) C22 0.035(3) 0.029(3) 0.036(4) -0.001(3) -0.001(3) -0.001(3) C23 0.047(4) 0.044(4) 0.035(4) 0.003(3) 0.007(3) 0.010(3) C24 0.036(4) 0.055(4) 0.034(4) 0.006(3) -0.005(3) 0.007(3) C25 0.048(4) 0.049(5) 0.055(5) -0.010(4) -0.010(4) 0.006(4) C26 0.038(4) 0.046(4) 0.078(6) 0.019(4) 0.013(4) 0.008(3) C27 0.039(4) 0.033(4) 0.073(5) -0.017(4) -0.003(4) -0.005(3) C28 0.015(3) 0.058(4) 0.041(4) 0.018(3) 0.011(3) 0.008(3) C29 0.022(3) 0.078(5) 0.027(3) 0.011(4) -0.005(3) -0.010(3) C30 0.021(3) 0.050(4) 0.036(4) 0.006(3) 0.000(3) -0.009(3) C31 0.020(2) 0.033(3) 0.020(3) -0.002(3) 0.002(3) 0.005(2) C32 0.030(3) 0.032(3) 0.038(4) -0.003(3) 0.006(3) -0.010(2) C33 0.032(3) 0.044(4) 0.031(3) 0.018(3) 0.005(3) -0.009(3) C34 0.038(4) 0.068(5) 0.041(4) 0.019(4) -0.003(3) -0.011(4) C35 0.105(8) 0.089(7) 0.044(5) 0.009(5) 0.031(5) 0.059(6) C36 0.068(6) 0.072(6) 0.044(5) 0.022(4) 0.002(4) -0.030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 S1 2.512(2) . yes Cd1 S4 2.5335(18) . yes Cd1 S2 2.5446(19) . yes Cd1 S3 2.5671(17) . yes S1 C1 1.761(6) . no S2 C10 1.755(6) . no S3 C19 1.759(6) . no S4 C28 1.765(7) . no P1 F6 1.596(5) . no P1 F3 1.597(5) . no P1 F2 1.596(5) . no P1 F4 1.598(4) . no P1 F1 1.601(5) . no P1 F5 1.605(4) . no P2 F8 1.570(5) . no P2 F9 1.572(5) . no P2 F7 1.579(5) . no P2 F11 1.582(6) . no P2 F12 1.585(5) . no P2 F10 1.596(5) . no O1 H37 0.816(12) . no O1 H38 0.817(12) . no O2 H39 0.819(12) . no O2 H40 0.818(12) . no N1 C8 1.468(8) . no N1 C9 1.491(9) . no N1 C7 1.499(8) . no N1 C4 1.514(7) . no N2 C16 1.482(9) . no N2 C17 1.486(9) . no N2 C13 1.503(8) . no N2 C18 1.516(9) . no N3 C22 1.495(9) . no N3 C26 1.498(9) . no N3 C27 1.502(9) . no N3 C25 1.511(9) . no N4 C34 1.481(8) . no N4 C35 1.495(9) . no N4 C36 1.496(9) . no N4 C31 1.503(8) . no C1 C6 1.347(10) . no C1 C2 1.377(10) . no C2 C3 1.395(10) . no C2 H2 0.9500 . no C3 C4 1.369(10) . no C3 H3 0.9500 . no C4 C5 1.356(9) . no C5 C6 1.400(9) . no C5 H5 0.9500 . no C6 H6 0.9500 . no C7 H7A 0.9800 . no C7 H7B 0.9800 . no C7 H7C 0.9800 . no C8 H8A 0.9800 . no C8 H8B 0.9800 . no C8 H8C 0.9800 . no C9 H9A 0.9800 . no C9 H9B 0.9800 . no C9 H9C 0.9800 . no C10 C15 1.387(9) . no C10 C11 1.421(10) . no C11 C12 1.388(9) . no C11 H11 0.9500 . no C12 C13 1.376(10) . no C12 H12 0.9500 . no C13 C14 1.394(10) . no C14 C15 1.388(9) . no C14 H14 0.9500 . no C15 H15 0.9500 . no C16 H16A 0.9800 . no C16 H16B 0.9800 . no C16 H16C 0.9800 . no C17 H17A 0.9800 . no C17 H17B 0.9800 . no C17 H17C 0.9800 . no C18 H18A 0.9800 . no C18 H18B 0.9800 . no C18 H18C 0.9800 . no C19 C24 1.380(10) . no C19 C20 1.384(9) . no C20 C21 1.399(10) . no C20 H20 0.9500 . no C21 C22 1.384(10) . no C21 H21 0.9500 . no C22 C23 1.331(10) . no C23 C24 1.391(10) . no C23 H23 0.9500 . no C24 H24 0.9500 . no C25 H25A 0.9800 . no C25 H25B 0.9800 . no C25 H25C 0.9800 . no C26 H26A 0.9800 . no C26 H26B 0.9800 . no C26 H26C 0.9800 . no C27 H27A 0.9800 . no C27 H27B 0.9800 . no C27 H27C 0.9800 . no C28 C29 1.379(10) . no C28 C33 1.381(10) . no C29 C30 1.372(9) . no C29 H29 0.9500 . no C30 C31 1.361(9) . no C30 H30 0.9500 . no C31 C32 1.386(8) . no C32 C33 1.385(9) . no C32 H32 0.9500 . no C33 H33 0.9500 . no C34 H34A 0.9800 . no C34 H34B 0.9800 . no C34 H34C 0.9800 . no C35 H35A 0.9800 . no C35 H35B 0.9800 . no C35 H35C 0.9800 . no C36 H36A 0.9800 . no C36 H36B 0.9800 . no C36 H36C 0.9800 . no 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 S1 Cd1 S4 123.31(7) . . yes S1 Cd1 S2 116.10(6) . . yes S4 Cd1 S2 101.26(7) . . yes S1 Cd1 S3 101.17(6) . . yes S4 Cd1 S3 105.15(6) . . yes S2 Cd1 S3 108.98(6) . . yes C1 S1 Cd1 108.4(2) . . no C10 S2 Cd1 109.0(2) . . no C19 S3 Cd1 105.3(2) . . no C28 S4 Cd1 104.8(2) . . no F6 P1 F3 89.2(3) . . no F6 P1 F2 179.4(3) . . no F3 P1 F2 91.2(3) . . no F6 P1 F4 90.2(2) . . no F3 P1 F4 91.2(2) . . no F2 P1 F4 89.4(2) . . no F6 P1 F1 88.6(3) . . no F3 P1 F1 177.8(3) . . no F2 P1 F1 90.9(3) . . no F4 P1 F1 88.4(2) . . no F6 P1 F5 90.2(2) . . no F3 P1 F5 89.3(2) . . no F2 P1 F5 90.2(2) . . no F4 P1 F5 179.3(3) . . no F1 P1 F5 91.1(2) . . no F8 P2 F9 179.0(3) . . no F8 P2 F7 91.5(3) . . no F9 P2 F7 88.8(3) . . no F8 P2 F11 90.4(3) . . no F9 P2 F11 90.5(3) . . no F7 P2 F11 90.2(3) . . no F8 P2 F12 90.1(3) . . no F9 P2 F12 89.6(3) . . no F7 P2 F12 178.4(4) . . no F11 P2 F12 90.3(4) . . no F8 P2 F10 90.0(3) . . no F9 P2 F10 89.1(3) . . no F7 P2 F10 90.0(3) . . no F11 P2 F10 179.5(3) . . no F12 P2 F10 89.5(3) . . no H37 O1 H38 107(4) . . no H39 O2 H40 107(4) . . no C8 N1 C9 106.9(6) . . no C8 N1 C7 109.4(6) . . no C9 N1 C7 108.7(6) . . no C8 N1 C4 111.6(5) . . no C9 N1 C4 111.3(5) . . no C7 N1 C4 109.0(5) . . no C16 N2 C17 109.4(5) . . no C16 N2 C13 110.1(6) . . no C17 N2 C13 113.4(5) . . no C16 N2 C18 107.8(6) . . no C17 N2 C18 107.8(6) . . no C13 N2 C18 108.2(5) . . no C22 N3 C26 110.7(5) . . no C22 N3 C27 110.3(5) . . no C26 N3 C27 109.0(6) . . no C22 N3 C25 113.8(5) . . no C26 N3 C25 106.5(6) . . no C27 N3 C25 106.3(6) . . no C34 N4 C35 108.6(6) . . no C34 N4 C36 107.8(6) . . no C35 N4 C36 108.9(7) . . no C34 N4 C31 110.3(5) . . no C35 N4 C31 109.4(5) . . no C36 N4 C31 111.9(5) . . no C6 C1 C2 116.9(6) . . no C6 C1 S1 121.4(5) . . no C2 C1 S1 121.7(5) . . no C1 C2 C3 120.9(7) . . no C1 C2 H2 119.5 . . no C3 C2 H2 119.5 . . no C4 C3 C2 120.4(7) . . no C4 C3 H3 119.8 . . no C2 C3 H3 119.8 . . no C5 C4 C3 119.5(6) . . no C5 C4 N1 121.5(6) . . no C3 C4 N1 118.9(6) . . no C4 C5 C6 118.6(7) . . no C4 C5 H5 120.7 . . no C6 C5 H5 120.7 . . no C1 C6 C5 123.6(7) . . no C1 C6 H6 118.2 . . no C5 C6 H6 118.2 . . no N1 C7 H7A 109.5 . . no N1 C7 H7B 109.5 . . no H7A C7 H7B 109.5 . . no N1 C7 H7C 109.5 . . no H7A C7 H7C 109.5 . . no H7B C7 H7C 109.5 . . no N1 C8 H8A 109.5 . . no N1 C8 H8B 109.5 . . no H8A C8 H8B 109.5 . . no N1 C8 H8C 109.5 . . no H8A C8 H8C 109.5 . . no H8B C8 H8C 109.5 . . no N1 C9 H9A 109.5 . . no N1 C9 H9B 109.5 . . no H9A C9 H9B 109.5 . . no N1 C9 H9C 109.5 . . no H9A C9 H9C 109.5 . . no H9B C9 H9C 109.5 . . no C15 C10 C11 117.5(6) . . no C15 C10 S2 124.3(5) . . no C11 C10 S2 118.2(5) . . no C12 C11 C10 120.2(7) . . no C12 C11 H11 119.9 . . no C10 C11 H11 119.9 . . no C13 C12 C11 120.5(7) . . no C13 C12 H12 119.8 . . no C11 C12 H12 119.8 . . no C12 C13 C14 120.7(6) . . no C12 C13 N2 118.8(6) . . no C14 C13 N2 120.5(6) . . no C15 C14 C13 118.5(7) . . no C15 C14 H14 120.7 . . no C13 C14 H14 120.7 . . no C14 C15 C10 122.6(7) . . no C14 C15 H15 118.7 . . no C10 C15 H15 118.7 . . no N2 C16 H16A 109.5 . . no N2 C16 H16B 109.5 . . no H16A C16 H16B 109.5 . . no N2 C16 H16C 109.5 . . no H16A C16 H16C 109.5 . . no H16B C16 H16C 109.5 . . no N2 C17 H17A 109.5 . . no N2 C17 H17B 109.5 . . no H17A C17 H17B 109.5 . . no N2 C17 H17C 109.5 . . no H17A C17 H17C 109.5 . . no H17B C17 H17C 109.5 . . no N2 C18 H18A 109.5 . . no N2 C18 H18B 109.5 . . no H18A C18 H18B 109.5 . . no N2 C18 H18C 109.5 . . no H18A C18 H18C 109.5 . . no H18B C18 H18C 109.5 . . no C24 C19 C20 117.2(6) . . no C24 C19 S3 123.6(5) . . no C20 C19 S3 119.2(5) . . no C19 C20 C21 121.0(7) . . no C19 C20 H20 119.5 . . no C21 C20 H20 119.5 . . no C22 C21 C20 119.6(7) . . no C22 C21 H21 120.2 . . no C20 C21 H21 120.2 . . no C23 C22 C21 119.8(6) . . no C23 C22 N3 119.1(6) . . no C21 C22 N3 121.1(6) . . no C22 C23 C24 121.0(7) . . no C22 C23 H23 119.5 . . no C24 C23 H23 119.5 . . no C19 C24 C23 121.3(6) . . no C19 C24 H24 119.3 . . no C23 C24 H24 119.3 . . no N3 C25 H25A 109.5 . . no N3 C25 H25B 109.5 . . no H25A C25 H25B 109.5 . . no N3 C25 H25C 109.5 . . no H25A C25 H25C 109.5 . . no H25B C25 H25C 109.5 . . no N3 C26 H26A 109.5 . . no N3 C26 H26B 109.5 . . no H26A C26 H26B 109.5 . . no N3 C26 H26C 109.5 . . no H26A C26 H26C 109.5 . . no H26B C26 H26C 109.5 . . no N3 C27 H27A 109.5 . . no N3 C27 H27B 109.5 . . no H27A C27 H27B 109.5 . . no N3 C27 H27C 109.5 . . no H27A C27 H27C 109.5 . . no H27B C27 H27C 109.5 . . no C29 C28 C33 116.5(6) . . no C29 C28 S4 121.3(6) . . no C33 C28 S4 121.9(5) . . no C30 C29 C28 123.5(7) . . no C30 C29 H29 118.3 . . no C28 C29 H29 118.3 . . no C31 C30 C29 119.0(6) . . no C31 C30 H30 120.5 . . no C29 C30 H30 120.5 . . no C30 C31 C32 120.0(6) . . no C30 C31 N4 120.9(5) . . no C32 C31 N4 119.1(5) . . no C33 C32 C31 119.8(6) . . no C33 C32 H32 120.1 . . no C31 C32 H32 120.1 . . no C28 C33 C32 121.3(6) . . no C28 C33 H33 119.3 . . no C32 C33 H33 119.3 . . no N4 C34 H34A 109.5 . . no N4 C34 H34B 109.5 . . no H34A C34 H34B 109.5 . . no N4 C34 H34C 109.5 . . no H34A C34 H34C 109.5 . . no H34B C34 H34C 109.5 . . no N4 C35 H35A 109.5 . . no N4 C35 H35B 109.5 . . no H35A C35 H35B 109.5 . . no N4 C35 H35C 109.5 . . no H35A C35 H35C 109.5 . . no H35B C35 H35C 109.5 . . no N4 C36 H36A 109.5 . . no N4 C36 H36B 109.5 . . no H36A C36 H36B 109.5 . . no N4 C36 H36C 109.5 . . no H36A C36 H36C 109.5 . . no H36B C36 H36C 109.5 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C8 H8A F12 0.98 2.48 3.431(8) 164.5 4_545 yes C8 H8C S2 0.98 2.87 3.757(9) 151.4 2_654 yes C14 H14 F1 0.95 2.41 3.338(9) 166.9 . yes C15 H15 S1 0.95 2.83 3.773(7) 170.2 . yes C16 H16C O1 0.98 2.57 3.472(15) 153.4 4_645 yes C25 H25C S3 0.98 2.79 3.718(8) 159.3 3_455 yes C26 H26B F9 0.98 2.46 3.431(11) 171.5 3_455 yes C34 H34A S3 0.98 2.81 3.767(8) 164.2 1_556 yes _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.259 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.085 # Attachment '- JPLang (revsied).cif' #TrackingRef '- JPLang (revsied).cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 865705' #TrackingRef '- JPLang (revsied).cif' _audit_creation_date 2011-12-02 _audit_creation_method 'SHELXL 97' _audit_update_record ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C90 H130 N10 S10 Zn4, C3 H7 N O, 8(F6 P), 0.5(H1.20 O0.60), 3.7(H2 O) ; _chemical_formula_sum 'C93 H145 F48 N11 O5 P8 S10 Zn4' _chemical_formula_weight 3239.23 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.7099(11) _cell_length_b 21.1388(14) _cell_length_c 21.3929(19) _cell_angle_alpha 104.421(3) _cell_angle_beta 116.145(3) _cell_angle_gamma 92.600(2) _cell_volume 7624.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3817 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 24.55 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8077 _exptl_absorpt_correction_T_max 0.8490 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _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 77173 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 29989 _reflns_number_gt 19152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.08P)^2^+1.99P] 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 29989 _refine_ls_number_parameters 1722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0057(2) 0.8041(2) 0.5285(2) 0.0315(9) Uani 1 1 d . . . C2 C 1.0209(3) 0.8039(3) 0.4737(3) 0.0445(12) Uani 1 1 d . . . H2 H 0.9822 0.7913 0.4256 0.053 Uiso 1 1 calc R . . C3 C 1.0977(3) 0.8237(2) 0.4915(3) 0.0357(10) Uani 1 1 d . . . H3 H 1.1119 0.8181 0.4546 0.043 Uiso 1 1 calc R . . C4 C 1.1537(3) 0.8520(3) 0.5649(3) 0.0488(13) Uani 1 1 d . . . C5 C 1.1390(3) 0.8513(2) 0.6202(3) 0.0376(10) Uani 1 1 d . . . H5 H 1.1769 0.8666 0.6686 0.045 Uiso 1 1 calc R . . C6 C 1.0637(3) 0.8262(2) 0.6008(3) 0.0407(11) Uani 1 1 d . . . H6 H 1.0514 0.8242 0.6376 0.049 Uiso 1 1 calc R . . C7 C 0.7085(3) 0.8598(2) 0.4939(2) 0.0342(10) Uani 1 1 d . . . C8 C 0.7438(3) 0.8392(3) 0.5569(2) 0.0423(11) Uani 1 1 d . . . H8 H 0.7534 0.7961 0.5529 0.051 Uiso 1 1 calc R . . C9 C 0.7644(3) 0.8836(3) 0.6252(3) 0.0460(12) Uani 1 1 d . . . H9 H 0.7891 0.8704 0.6670 0.055 Uiso 1 1 calc R . . C10 C 0.7478(3) 0.9486(3) 0.6315(3) 0.0517(13) Uani 1 1 d . . . C11 C 0.7137(3) 0.9686(2) 0.5684(3) 0.0376(10) Uani 1 1 d . . . H11 H 0.7052 1.0120 0.5720 0.045 Uiso 1 1 calc R . . C12 C 0.6929(3) 0.9244(2) 0.5013(3) 0.0416(11) Uani 1 1 d . . . H12 H 0.6679 0.9377 0.4596 0.050 Uiso 1 1 calc R . . C13 C 0.7979(2) 0.6480(2) 0.5617(2) 0.0317(9) Uani 1 1 d . . . C14 C 0.7672(3) 0.6042(3) 0.5861(3) 0.0401(11) Uani 1 1 d . . . H14 H 0.7374 0.5635 0.5535 0.048 Uiso 1 1 calc R . . C15 C 0.7802(3) 0.6203(3) 0.6575(3) 0.0439(12) Uani 1 1 d . . . H15 H 0.7601 0.5903 0.6730 0.053 Uiso 1 1 calc R . . C16 C 0.8234(3) 0.6811(3) 0.7060(3) 0.0426(11) Uani 1 1 d . . . C17 C 0.8547(3) 0.7260(3) 0.6837(3) 0.0476(13) Uani 1 1 d . . . H17 H 0.8842 0.7667 0.7166 0.057 Uiso 1 1 calc R . . C18 C 0.8410(3) 0.7089(3) 0.6096(3) 0.0462(12) Uani 1 1 d . . . H18 H 0.8610 0.7386 0.5938 0.055 Uiso 1 1 calc R . . C19 C 0.5888(3) 0.5676(2) 0.2495(3) 0.0456(12) Uani 1 1 d . . . C20 C 0.6144(3) 0.5133(2) 0.2214(3) 0.0491(13) Uani 1 1 d . . . H20 H 0.6610 0.5192 0.2207 0.059 Uiso 1 1 calc R . . C21 C 0.5711(3) 0.4500(3) 0.1942(3) 0.0522(13) Uani 1 1 d . . . H21 H 0.5884 0.4133 0.1755 0.063 Uiso 1 1 calc R . . C22 C 0.5010(3) 0.4426(3) 0.1955(3) 0.0524(14) Uani 1 1 d . . . C23 C 0.4765(3) 0.4987(2) 0.2242(3) 0.0440(12) Uani 1 1 d . . . H23 H 0.4296 0.4934 0.2245 0.053 Uiso 1 1 calc R . . C24 C 0.5187(3) 0.5602(3) 0.2514(3) 0.0474(13) Uani 1 1 d . . . H24 H 0.5017 0.5967 0.2708 0.057 Uiso 1 1 calc R . . C25 C 0.7188(3) 0.7948(2) 0.2249(2) 0.0366(10) Uani 1 1 d . . . C26 C 0.6816(3) 0.8467(3) 0.2471(3) 0.0507(13) Uani 1 1 d . . . H26 H 0.6967 0.8661 0.2963 0.061 Uiso 1 1 calc R . . C27 C 0.6233(3) 0.8677(3) 0.1946(3) 0.0469(12) Uani 1 1 d . . . H27 H 0.5992 0.9005 0.2097 0.056 Uiso 1 1 calc R . . C28 C 0.5997(3) 0.8413(3) 0.1207(3) 0.0468(12) Uani 1 1 d . . . C29 C 0.6378(3) 0.7899(3) 0.1008(3) 0.0413(11) Uani 1 1 d . . . H29 H 0.6236 0.7704 0.0517 0.050 Uiso 1 1 calc R . . C30 C 0.6950(3) 0.7688(2) 0.1529(2) 0.0412(11) Uani 1 1 d . . . H30 H 0.7182 0.7352 0.1376 0.049 Uiso 1 1 calc R . . C31 C 0.8416(3) 0.5247(2) 0.3077(3) 0.0423(11) Uani 1 1 d . . . C32 C 0.8369(3) 0.4887(2) 0.2407(3) 0.0409(11) Uani 1 1 d . . . H32 H 0.8490 0.5105 0.2131 0.049 Uiso 1 1 calc R . . C33 C 0.8142(3) 0.4205(2) 0.2163(3) 0.0472(13) Uani 1 1 d . . . H33 H 0.8093 0.3964 0.1713 0.057 Uiso 1 1 calc R . . C34 C 0.7984(3) 0.3875(3) 0.2591(3) 0.0511(14) Uani 1 1 d . . . C35 C 0.8018(3) 0.4232(3) 0.3241(3) 0.0449(12) Uani 1 1 d . . . H35 H 0.7901 0.4011 0.3516 0.054 Uiso 1 1 calc R . . C36 C 0.8226(3) 0.4924(2) 0.3489(3) 0.0456(12) Uani 1 1 d . . . H36 H 0.8237 0.5165 0.3923 0.055 Uiso 1 1 calc R . . C37 C 0.9199(3) 0.9778(2) 0.5406(3) 0.0413(11) Uani 1 1 d . . . C38 C 0.9242(3) 0.9514(3) 0.5958(2) 0.0417(11) Uani 1 1 d . . . H38 H 0.8913 0.9123 0.5836 0.050 Uiso 1 1 calc R . . C39 C 0.9755(3) 0.9819(3) 0.6669(3) 0.0539(15) Uani 1 1 d . . . H39 H 0.9778 0.9635 0.7029 0.065 Uiso 1 1 calc R . . C40 C 1.0257(3) 1.0416(2) 0.6861(3) 0.0478(13) Uani 1 1 d . . . C41 C 1.0239(3) 1.0672(3) 0.6325(3) 0.0459(12) Uani 1 1 d . . . H41 H 1.0589 1.1046 0.6440 0.055 Uiso 1 1 calc R . . C42 C 0.9688(3) 1.0363(2) 0.5609(3) 0.0450(12) Uani 1 1 d . . . H42 H 0.9646 1.0559 0.5252 0.054 Uiso 1 1 calc R . . C43 C 0.9755(3) 0.5769(2) 0.5944(3) 0.0336(9) Uani 1 1 d . . . C44 C 0.9428(3) 0.5162(2) 0.5429(3) 0.0465(12) Uani 1 1 d . . . H44 H 0.9354 0.5117 0.4959 0.056 Uiso 1 1 calc R . . C45 C 0.9202(3) 0.4610(3) 0.5577(3) 0.0527(14) Uani 1 1 d . . . H45 H 0.9004 0.4197 0.5224 0.063 Uiso 1 1 calc R . . C46 C 0.9285(3) 0.4701(3) 0.6277(3) 0.0443(12) Uani 1 1 d . . . C47 C 0.9617(3) 0.5319(2) 0.6816(3) 0.0401(11) Uani 1 1 d . . . H47 H 0.9686 0.5372 0.7286 0.048 Uiso 1 1 calc R . . C48 C 0.9837(3) 0.5846(3) 0.6636(3) 0.0451(12) Uani 1 1 d . . . H48 H 1.0043 0.6261 0.6985 0.054 Uiso 1 1 calc R . . C49 C 0.4848(3) 0.7153(3) 0.3710(3) 0.0382(10) Uani 1 1 d . . . C50 C 0.4125(3) 0.7071(3) 0.3668(3) 0.0419(11) Uani 1 1 d . . . H50 H 0.4054 0.6922 0.4012 0.050 Uiso 1 1 calc R . . C51 C 0.3504(3) 0.7213(2) 0.3102(3) 0.0432(11) Uani 1 1 d . . . H51 H 0.3018 0.7160 0.3071 0.052 Uiso 1 1 calc R . . C52 C 0.3614(3) 0.7435(3) 0.2588(3) 0.0460(12) Uani 1 1 d . . . C53 C 0.4336(3) 0.7504(2) 0.2633(3) 0.0429(12) Uani 1 1 d . . . H53 H 0.4407 0.7642 0.2283 0.052 Uiso 1 1 calc R . . C54 C 0.4953(3) 0.7369(3) 0.3192(3) 0.0441(12) Uani 1 1 d . . . H54 H 0.5438 0.7424 0.3221 0.053 Uiso 1 1 calc R . . C55 C 0.7656(3) 0.5943(3) 0.1045(3) 0.0445(12) Uani 1 1 d . . . C56 C 0.8328(3) 0.6380(2) 0.1520(3) 0.0390(11) Uani 1 1 d . . . H56 H 0.8399 0.6634 0.1974 0.047 Uiso 1 1 calc R . . C57 C 0.8893(3) 0.6440(3) 0.1322(3) 0.0425(11) Uani 1 1 d . . . H57 H 0.9364 0.6717 0.1644 0.051 Uiso 1 1 calc R . . C58 C 0.8744(3) 0.6076(3) 0.0624(3) 0.0491(13) Uani 1 1 d . . . C59 C 0.8041(3) 0.5650(3) 0.0120(3) 0.0468(12) Uani 1 1 d . . . H59 H 0.7954 0.5410 -0.0344 0.056 Uiso 1 1 calc R . . C60 C 0.7505(3) 0.5604(3) 0.0335(3) 0.0499(13) Uani 1 1 d . . . H60 H 0.7025 0.5342 0.0009 0.060 Uiso 1 1 calc R . . C61 C 1.2352(3) 0.8948(3) 0.5241(3) 0.0477(12) Uani 1 1 d . . . H61A H 1.2822 0.9241 0.5401 0.072 Uiso 1 1 calc R . . H61B H 1.1926 0.9171 0.5051 0.072 Uiso 1 1 calc R . . H61C H 1.2298 0.8559 0.4865 0.072 Uiso 1 1 calc R . . C62 C 1.2638(3) 0.9368(3) 0.6528(3) 0.0464(12) Uani 1 1 d . . . H62A H 1.2929 0.9242 0.6959 0.070 Uiso 1 1 calc R . . H62B H 1.2200 0.9535 0.6547 0.070 Uiso 1 1 calc R . . H62C H 1.2955 0.9708 0.6500 0.070 Uiso 1 1 calc R . . C63 C 1.2934(3) 0.8287(3) 0.6097(3) 0.0433(12) Uani 1 1 d . . . H63A H 1.2658 0.7874 0.6042 0.065 Uiso 1 1 calc R . . H63B H 1.3303 0.8485 0.6601 0.065 Uiso 1 1 calc R . . H63C H 1.3194 0.8208 0.5805 0.065 Uiso 1 1 calc R . . C64 C 0.8153(3) 1.0612(3) 0.7120(3) 0.0445(12) Uani 1 1 d . . . H64A H 0.8325 1.0918 0.7597 0.067 Uiso 1 1 calc R . . H64B H 0.7805 1.0794 0.6759 0.067 Uiso 1 1 calc R . . H64C H 0.8586 1.0534 0.7037 0.067 Uiso 1 1 calc R . . C65 C 0.7042(3) 1.0080(3) 0.7128(3) 0.0499(13) Uani 1 1 d . . . H65A H 0.6778 1.0347 0.6824 0.075 Uiso 1 1 calc R . . H65B H 0.7174 1.0307 0.7626 0.075 Uiso 1 1 calc R . . H65C H 0.6714 0.9662 0.6972 0.075 Uiso 1 1 calc R . . C66 C 0.8356(3) 0.9691(3) 0.7669(3) 0.0579(15) Uani 1 1 d . . . H66A H 0.8134 0.9260 0.7631 0.087 Uiso 1 1 calc R . . H66B H 0.8503 0.9988 0.8145 0.087 Uiso 1 1 calc R . . H66C H 0.8801 0.9657 0.7595 0.087 Uiso 1 1 calc R . . C67 C 0.8311(3) 0.7736(3) 0.8074(3) 0.0479(12) Uani 1 1 d . . . H67A H 0.7790 0.7804 0.7839 0.072 Uiso 1 1 calc R . . H67B H 0.8624 0.7997 0.7957 0.072 Uiso 1 1 calc R . . H67C H 0.8499 0.7869 0.8593 0.072 Uiso 1 1 calc R . . C68 C 0.7948(3) 0.6581(3) 0.7959(3) 0.0469(12) Uani 1 1 d . . . H68A H 0.8016 0.6756 0.8446 0.070 Uiso 1 1 calc R . . H68B H 0.8141 0.6172 0.7913 0.070 Uiso 1 1 calc R . . H68C H 0.7412 0.6501 0.7617 0.070 Uiso 1 1 calc R . . C69 C 0.9211(3) 0.7080(3) 0.8301(3) 0.0489(13) Uani 1 1 d . . . H69A H 0.9493 0.7388 0.8200 0.073 Uiso 1 1 calc R . . H69B H 0.9351 0.6651 0.8197 0.073 Uiso 1 1 calc R . . H69C H 0.9331 0.7233 0.8805 0.073 Uiso 1 1 calc R . . C70 C 0.3899(3) 0.3748(3) 0.0930(3) 0.0512(13) Uani 1 1 d . . . H70A H 0.3575 0.4056 0.0997 0.077 Uiso 1 1 calc R . . H70B H 0.3606 0.3306 0.0706 0.077 Uiso 1 1 calc R . . H70C H 0.4094 0.3855 0.0623 0.077 Uiso 1 1 calc R . . C71 C 0.4284(3) 0.3718(3) 0.2192(3) 0.0446(12) Uani 1 1 d . . . H71A H 0.4485 0.4112 0.2603 0.067 Uiso 1 1 calc R . . H71B H 0.4450 0.3342 0.2357 0.067 Uiso 1 1 calc R . . H71C H 0.3733 0.3651 0.1952 0.067 Uiso 1 1 calc R . . C72 C 0.5035(3) 0.3225(3) 0.1609(3) 0.0483(13) Uani 1 1 d . . . H72A H 0.5479 0.3290 0.2072 0.072 Uiso 1 1 calc R . . H72B H 0.5194 0.3230 0.1246 0.072 Uiso 1 1 calc R . . H72C H 0.4718 0.2805 0.1471 0.072 Uiso 1 1 calc R . . C73 C 0.5755(3) 0.8939(3) 0.0268(3) 0.0451(12) Uani 1 1 d . . . H73A H 0.5805 0.8585 -0.0081 0.068 Uiso 1 1 calc R . . H73B H 0.6254 0.9195 0.0619 0.068 Uiso 1 1 calc R . . H73C H 0.5438 0.9220 0.0021 0.068 Uiso 1 1 calc R . . C74 C 0.4722(3) 0.8166(3) 0.0096(3) 0.0501(13) Uani 1 1 d . . . H74A H 0.4500 0.7978 0.0342 0.075 Uiso 1 1 calc R . . H74B H 0.4866 0.7822 -0.0185 0.075 Uiso 1 1 calc R . . H74C H 0.4354 0.8372 -0.0223 0.075 Uiso 1 1 calc R . . C75 C 0.5102(3) 0.9284(3) 0.0948(3) 0.0475(13) Uani 1 1 d . . . H75A H 0.4760 0.9435 0.0554 0.071 Uiso 1 1 calc R . . H75B H 0.5529 0.9635 0.1289 0.071 Uiso 1 1 calc R . . H75C H 0.4833 0.9157 0.1191 0.071 Uiso 1 1 calc R . . C76 C 0.6921(3) 0.3014(3) 0.1688(3) 0.0453(12) Uani 1 1 d . . . H76A H 0.6689 0.3366 0.1847 0.068 Uiso 1 1 calc R . . H76B H 0.6684 0.2600 0.1674 0.068 Uiso 1 1 calc R . . H76C H 0.6852 0.2992 0.1210 0.068 Uiso 1 1 calc R . . C77 C 0.7865(3) 0.2862(3) 0.2794(3) 0.0476(13) Uani 1 1 d . . . H77A H 0.8372 0.3025 0.3198 0.071 Uiso 1 1 calc R . . H77B H 0.7787 0.2388 0.2611 0.071 Uiso 1 1 calc R . . H77C H 0.7491 0.2986 0.2953 0.071 Uiso 1 1 calc R . . C78 C 0.8416(3) 0.2819(3) 0.2069(3) 0.0537(14) Uani 1 1 d . . . H78A H 0.8461 0.2956 0.1691 0.081 Uiso 1 1 calc R . . H78B H 0.8274 0.2344 0.1914 0.081 Uiso 1 1 calc R . . H78C H 0.8900 0.2955 0.2506 0.081 Uiso 1 1 calc R . . C79 C 1.1507(3) 1.0252(3) 0.7920(3) 0.0488(13) Uani 1 1 d . . . H79A H 1.1291 0.9861 0.7968 0.073 Uiso 1 1 calc R . . H79B H 1.1940 1.0492 0.8378 0.073 Uiso 1 1 calc R . . H79C H 1.1672 1.0125 0.7553 0.073 Uiso 1 1 calc R . . C80 C 1.0462(3) 1.0844(3) 0.8146(3) 0.0479(13) Uani 1 1 d . . . H80A H 0.9937 1.0868 0.7844 0.072 Uiso 1 1 calc R . . H80B H 1.0710 1.1256 0.8528 0.072 Uiso 1 1 calc R . . H80C H 1.0476 1.0490 0.8357 0.072 Uiso 1 1 calc R . . C81 C 1.1228(3) 1.1374(3) 0.7812(3) 0.0449(12) Uani 1 1 d . . . H81A H 1.1613 1.1552 0.8313 0.067 Uiso 1 1 calc R . . H81B H 1.0846 1.1652 0.7704 0.067 Uiso 1 1 calc R . . H81C H 1.1463 1.1359 0.7501 0.067 Uiso 1 1 calc R . . C82 C 0.8319(3) 0.4302(3) 0.6438(3) 0.0434(12) Uani 1 1 d . . . H82A H 0.8390 0.4535 0.6916 0.065 Uiso 1 1 calc R . . H82B H 0.7994 0.3879 0.6264 0.065 Uiso 1 1 calc R . . H82C H 0.8083 0.4557 0.6111 0.065 Uiso 1 1 calc R . . C83 C 0.9733(3) 0.4172(3) 0.7221(3) 0.0449(12) Uani 1 1 d . . . H83A H 1.0131 0.4555 0.7435 0.067 Uiso 1 1 calc R . . H83B H 0.9948 0.3777 0.7152 0.067 Uiso 1 1 calc R . . H83C H 0.9512 0.4166 0.7540 0.067 Uiso 1 1 calc R . . C84 C 0.9038(3) 0.3514(3) 0.5932(3) 0.0564(15) Uani 1 1 d . . . H84A H 0.9484 0.3516 0.5858 0.085 Uiso 1 1 calc R . . H84B H 0.8587 0.3446 0.5474 0.085 Uiso 1 1 calc R . . H84C H 0.8999 0.3162 0.6131 0.085 Uiso 1 1 calc R . . C85 C 0.2249(3) 0.7148(3) 0.1727(3) 0.0484(13) Uani 1 1 d . . . H85A H 0.1831 0.7299 0.1387 0.073 Uiso 1 1 calc R . . H85B H 0.2175 0.7159 0.2144 0.073 Uiso 1 1 calc R . . H85C H 0.2268 0.6702 0.1497 0.073 Uiso 1 1 calc R . . C86 C 0.2868(3) 0.8268(2) 0.2141(3) 0.0466(12) Uani 1 1 d . . . H86A H 0.2478 0.8354 0.1719 0.070 Uiso 1 1 calc R . . H86B H 0.3348 0.8545 0.2299 0.070 Uiso 1 1 calc R . . H86C H 0.2727 0.8362 0.2526 0.070 Uiso 1 1 calc R . . C87 C 0.3083(3) 0.7355(2) 0.1308(3) 0.0431(12) Uani 1 1 d . . . H87A H 0.2625 0.7082 0.0897 0.065 Uiso 1 1 calc R . . H87B H 0.3495 0.7106 0.1414 0.065 Uiso 1 1 calc R . . H87C H 0.3219 0.7739 0.1197 0.065 Uiso 1 1 calc R . . C88 C 1.0174(3) 0.6130(3) 0.0991(3) 0.0458(12) Uani 1 1 d . . . H88A H 1.0228 0.5673 0.0924 0.069 Uiso 1 1 calc R . . H88B H 1.0245 0.6328 0.1476 0.069 Uiso 1 1 calc R . . H88C H 1.0552 0.6362 0.0920 0.069 Uiso 1 1 calc R . . C89 C 0.9154(3) 0.5665(2) -0.0318(3) 0.0407(11) Uani 1 1 d . . . H89A H 0.9567 0.5709 -0.0436 0.061 Uiso 1 1 calc R . . H89B H 0.8698 0.5748 -0.0687 0.061 Uiso 1 1 calc R . . H89C H 0.9064 0.5223 -0.0296 0.061 Uiso 1 1 calc R . . C90 C 0.9350(3) 0.6845(3) 0.0302(3) 0.0495(13) Uani 1 1 d . . . H90A H 0.9507 0.6841 -0.0064 0.074 Uiso 1 1 calc R . . H90B H 0.9692 0.7182 0.0746 0.074 Uiso 1 1 calc R . . H90C H 0.8837 0.6935 0.0137 0.074 Uiso 1 1 calc R . . C91 C 0.4830(3) 0.6319(3) 0.0067(3) 0.0423(11) Uani 1 1 d . . . H91 H 0.5349 0.6297 0.0300 0.051 Uiso 1 1 calc R . . C92 C 0.3521(3) 0.5987(2) -0.0201(3) 0.0433(11) Uani 1 1 d . . . H92A H 0.3418 0.6409 -0.0275 0.065 Uiso 1 1 calc R . . H92B H 0.3297 0.5884 0.0087 0.065 Uiso 1 1 calc R . . H92C H 0.3303 0.5650 -0.0665 0.065 Uiso 1 1 calc R . . C93 C 0.4645(3) 0.5556(3) 0.0637(3) 0.0452(12) Uani 1 1 d . . . H93A H 0.5133 0.5471 0.0674 0.068 Uiso 1 1 calc R . . H93B H 0.4286 0.5145 0.0415 0.068 Uiso 1 1 calc R . . H93C H 0.4702 0.5759 0.1116 0.068 Uiso 1 1 calc R . . P1 P 0.09147(11) 0.59592(10) 0.92181(11) 0.0728(5) Uani 1 1 d . . . F1 F 0.1775(2) 0.6255(2) 0.9724(2) 0.0772(11) Uani 1 1 d . . . F2 F 0.1182(2) 0.53725(19) 0.8823(2) 0.0739(11) Uani 1 1 d . . . F3 F 0.0002(2) 0.5659(2) 0.8671(2) 0.0738(11) Uani 1 1 d . . . F4 F 0.0601(2) 0.6549(2) 0.9619(2) 0.0776(11) Uani 1 1 d . . . F5 F 0.0971(2) 0.5595(2) 0.9768(2) 0.0737(10) Uani 1 1 d . . . F6 F 0.0801(2) 0.63194(19) 0.8634(2) 0.0703(10) Uani 1 1 d . . . P2 P 0.75251(12) 0.79660(10) 0.97584(11) 0.0726(5) Uani 1 1 d . . . F7 F 0.7468(2) 0.8333(2) 0.9225(2) 0.0754(11) Uani 1 1 d . . . F8 F 0.6577(2) 0.78326(19) 0.9348(2) 0.0744(11) Uani 1 1 d . . . F9 F 0.7585(2) 0.76063(19) 1.03006(19) 0.0725(10) Uani 1 1 d . . . F10 F 0.8426(2) 0.8097(2) 1.0152(2) 0.0791(11) Uani 1 1 d . . . F11 F 0.7508(2) 0.8629(2) 1.0311(2) 0.0759(11) Uani 1 1 d . . . F12 F 0.7552(2) 0.7282(2) 0.9249(2) 0.0722(10) Uani 1 1 d . . . P3 P 0.32270(12) 0.91350(10) 0.85562(11) 0.0738(5) Uani 1 1 d . . . F13 F 0.3103(2) 0.96452(18) 0.8222(2) 0.0729(10) Uani 1 1 d . . . F14 F 0.3297(2) 0.86377(19) 0.7982(2) 0.0768(11) Uani 1 1 d . . . F15 F 0.3122(2) 0.86439(19) 0.8883(2) 0.0772(11) Uani 1 1 d . . . F16 F 0.2925(3) 0.97021(19) 0.9074(2) 0.0773(11) Uani 1 1 d . . . F17 F 0.4048(2) 0.9405(2) 0.9217(2) 0.0813(12) Uani 1 1 d . . . F18 F 0.2321(3) 0.8913(2) 0.8043(2) 0.0862(12) Uani 1 1 d . . . P4 P 0.10848(11) 0.77482(10) 0.29704(11) 0.0732(5) Uani 1 1 d . . . F19 F 0.0505(2) 0.7688(2) 0.2164(2) 0.0792(11) Uani 1 1 d . . . F20 F 0.0939(3) 0.8474(2) 0.3225(2) 0.0862(12) Uani 1 1 d . . . F21 F 0.1679(3) 0.7821(2) 0.3802(2) 0.0843(12) Uani 1 1 d . . . F22 F 0.1104(2) 0.7021(2) 0.2629(2) 0.0867(13) Uani 1 1 d . . . F23 F 0.1777(2) 0.7930(2) 0.2846(2) 0.0756(11) Uani 1 1 d . . . F24 F 0.0373(2) 0.7551(2) 0.3057(2) 0.0832(12) Uani 1 1 d . . . P5 P 0.66368(12) 0.35529(10) 0.39799(10) 0.0750(5) Uani 1 1 d . . . F25 F 0.6337(2) 0.2879(2) 0.3338(2) 0.0751(11) Uani 1 1 d . . . F26 F 0.7498(2) 0.3449(2) 0.4196(2) 0.0761(11) Uani 1 1 d . . . F27 F 0.6906(2) 0.4221(2) 0.4625(2) 0.0782(11) Uani 1 1 d . . . F28 F 0.5742(2) 0.3626(2) 0.3754(2) 0.0786(11) Uani 1 1 d . . . F29 F 0.6707(3) 0.3201(2) 0.4524(2) 0.0806(11) Uani 1 1 d . . . F30 F 0.6539(2) 0.38955(19) 0.3406(2) 0.0731(11) Uani 1 1 d . . . P6 P 0.06020(12) 0.85883(10) 0.05598(11) 0.0735(5) Uani 1 1 d . . . F31 F -0.0002(2) 0.91233(18) 0.0664(2) 0.0715(10) Uani 1 1 d . . . F32 F 0.0753(2) 0.83503(19) 0.1182(2) 0.0760(11) Uani 1 1 d . . . F33 F 0.1134(2) 0.81149(19) 0.0370(2) 0.0752(11) Uani 1 1 d . . . F34 F 0.0446(2) 0.88064(19) -0.0108(2) 0.0756(11) Uani 1 1 d . . . F35 F -0.0101(2) 0.8035(2) 0.0010(2) 0.0794(11) Uani 1 1 d . . . F36 F 0.1465(3) 0.9041(2) 0.1120(2) 0.0863(13) Uani 1 1 d . . . P7 P 0.51351(12) 0.98507(10) 0.30219(11) 0.0739(5) Uani 1 1 d . . . F37 F 0.5362(2) 1.00447(19) 0.2507(2) 0.0755(11) Uani 1 1 d . . . F38 F 0.4643(3) 0.9223(2) 0.2377(2) 0.0817(12) Uani 1 1 d . . . F39 F 0.4893(2) 0.95728(19) 0.3469(2) 0.0776(11) Uani 1 1 d . . . F40 F 0.5659(2) 1.05068(18) 0.3669(2) 0.0698(10) Uani 1 1 d . . . F41 F 0.4453(2) 1.0289(2) 0.2844(2) 0.0756(11) Uani 1 1 d . . . F42 F 0.5887(3) 0.9502(2) 0.3267(2) 0.0822(12) Uani 1 1 d . . . P8 P 0.25494(12) 0.52055(10) 0.22733(11) 0.0753(5) Uani 1 1 d . . . F43 F 0.2146(2) 0.58202(19) 0.2424(2) 0.0743(11) Uani 1 1 d . . . F44 F 0.2653(3) 0.5023(2) 0.2907(2) 0.0816(12) Uani 1 1 d . . . F45 F 0.2919(2) 0.4614(2) 0.2013(2) 0.0743(11) Uani 1 1 d . . . F46 F 0.2482(3) 0.5569(2) 0.1659(2) 0.0791(11) Uani 1 1 d . . . F47 F 0.1762(2) 0.4801(2) 0.1943(2) 0.0812(12) Uani 1 1 d . . . F48 F 0.3378(2) 0.56284(19) 0.2760(2) 0.0779(11) Uani 1 1 d . . . N1 N 1.2365(2) 0.8759(2) 0.5847(2) 0.0445(10) Uani 1 1 d . . . N2 N 0.7747(2) 0.9966(2) 0.7070(2) 0.0440(10) Uani 1 1 d . . . N3 N 0.8341(2) 0.7029(2) 0.7816(2) 0.0408(9) Uani 1 1 d . . . N4 N 0.4569(3) 0.3792(2) 0.1672(2) 0.0492(11) Uani 1 1 d . . . N5 N 0.5407(2) 0.8665(2) 0.0636(2) 0.0444(10) Uani 1 1 d . . . N6 N 0.7783(3) 0.3146(2) 0.2223(2) 0.0506(11) Uani 1 1 d . . . N7 N 1.0872(3) 1.0713(2) 0.7689(2) 0.0474(11) Uani 1 1 d . . . N8 N 0.9107(2) 0.4198(2) 0.6478(2) 0.0421(10) Uani 1 1 d . . . N9 N 0.2946(2) 0.7567(2) 0.1953(2) 0.0413(9) Uani 1 1 d . . . N10 N 0.9372(3) 0.6175(2) 0.0437(2) 0.0503(11) Uani 1 1 d . . . N11 N 0.4351(2) 0.6014(2) 0.0179(2) 0.0401(9) Uani 1 1 d . . . O1 O 0.45766(18) 0.66590(16) -0.03781(17) 0.0354(7) Uani 1 1 d . . . O1W O 0.0244(6) 0.9258(8) 0.8236(6) 0.062(4) Uani 0.30 1 d P . . H1X H 0.0218 0.9084 0.7825 0.074 Uiso 0.30 1 d PR . . H1Y H 0.0168 0.8962 0.8385 0.074 Uiso 0.30 1 d PR . . O2W O 0.5529(8) 0.5572(6) 0.4308(8) 0.064(4) Uani 0.30 1 d P . . H2X H 0.5680 0.5213 0.4186 0.076 Uiso 0.30 1 d PR . . H2Y H 0.5285 0.5692 0.3929 0.076 Uiso 0.30 1 d PR . . O3W O 0.3009(7) -0.0082(7) 0.1391(7) 0.057(3) Uani 0.30 1 d P . . H3X H 0.3020 0.0281 0.1680 0.068 Uiso 0.30 1 d PR . . H3Y H 0.3052 -0.0005 0.1037 0.068 Uiso 0.30 1 d PR . . O4W O 0.1159(7) 0.8582(6) 0.8745(7) 0.047(3) Uani 0.30 1 d P . . H4X H 0.1492 0.8923 0.8982 0.057 Uiso 0.30 1 d PR . . H4Y H 0.1022 0.8496 0.9024 0.057 Uiso 0.30 1 d PR . . O5W O 0.5722(8) 0.1389(9) 0.5239(9) 0.074(4) Uani 0.30 1 d P . . H5X H 0.5971 0.1147 0.5499 0.089 Uiso 0.30 1 d PR . . H5Y H 0.5630 0.1209 0.4803 0.089 Uiso 0.30 1 d PR . . O6W O 0.5510(7) 0.3586(6) 0.5120(6) 0.048(3) Uani 0.30 1 d P . . H6X H 0.5328 0.3749 0.5406 0.058 Uiso 0.30 1 d PR . . H6Y H 0.5145 0.3427 0.4687 0.058 Uiso 0.30 1 d PR . . O7W O 0.4425(9) 0.1614(7) 0.2444(7) 0.068(4) Uani 0.30 1 d P . . H7X H 0.4174 0.1338 0.2017 0.081 Uiso 0.30 1 d PR . . H7Y H 0.4173 0.1628 0.2668 0.081 Uiso 0.30 1 d PR . . O8W O 0.6344(7) 0.8190(6) 0.7017(6) 0.046(3) Uani 0.30 1 d P . . H8X H 0.5918 0.7953 0.6854 0.055 Uiso 0.30 1 d PR . . H8Y H 0.6354 0.8260 0.6663 0.055 Uiso 0.30 1 d PR . . O9W O 0.4202(7) 0.4200(7) 0.4324(6) 0.054(3) Uani 0.30 1 d P . . H9X H 0.4116 0.4010 0.4570 0.065 Uiso 0.30 1 d PR . . H9Y H 0.3769 0.4200 0.3944 0.065 Uiso 0.30 1 d PR . . O10W O 0.8360(8) 0.8993(6) 0.9316(6) 0.052(3) Uani 0.30 1 d P . . H10X H 0.8088 0.9246 0.9459 0.062 Uiso 0.30 1 d PR . . H10Y H 0.8713 0.8876 0.9669 0.062 Uiso 0.30 1 d PR . . O11W O 0.5000 0.0000 0.5000 0.0432(19) Uani 0.60 2 d SP . . H11X H 0.5153 0.0407 0.5195 0.052 Uiso 0.30 1 d PR . . H11Y H 0.5283 -0.0196 0.5304 0.052 Uiso 0.30 1 d PR . . O12W O 0.5427(6) 0.8946(5) 0.8686(5) 0.061(3) Uani 0.40 1 d P . . H12X H 0.5134 0.8583 0.8474 0.074 Uiso 0.40 1 d PR . . H12Y H 0.5853 0.8909 0.9050 0.074 Uiso 0.40 1 d PR . . O13W O 0.3214(8) 0.7988(6) 0.0202(7) 0.058(3) Uani 0.30 1 d P . . H13X H 0.3253 0.8155 -0.0106 0.069 Uiso 0.30 1 d PR . . H13Y H 0.2972 0.7590 -0.0013 0.069 Uiso 0.30 1 d PR . . S1 S 0.91167(5) 0.77754(5) 0.50896(5) 0.0252(2) Uani 1 1 d . . . S2 S 0.68688(5) 0.80606(5) 0.41036(5) 0.02425(19) Uani 1 1 d . . . S3 S 0.77029(5) 0.62172(5) 0.47088(5) 0.0243(2) Uani 1 1 d . . . S4 S 0.62975(5) 0.64700(5) 0.27818(5) 0.02243(19) Uani 1 1 d . . . S5 S 0.79851(6) 0.76540(5) 0.29242(5) 0.0253(2) Uani 1 1 d . . . S6 S 0.86813(5) 0.60819(5) 0.34266(5) 0.02387(19) Uani 1 1 d . . . S7 S 0.85012(6) 0.94651(5) 0.44381(5) 0.0254(2) Uani 1 1 d . . . S8 S 1.01332(5) 0.63569(5) 0.57821(5) 0.02239(19) Uani 1 1 d . . . S9 S 0.56202(5) 0.69756(5) 0.44482(5) 0.02322(19) Uani 1 1 d . . . S10 S 0.69160(6) 0.58416(5) 0.12482(5) 0.0280(2) Uani 1 1 d . . . Zn1 Zn 0.81720(3) 0.83009(2) 0.41770(2) 0.02419(10) Uani 1 1 d . . . Zn2 Zn 0.89556(3) 0.65294(2) 0.47383(2) 0.02485(10) Uani 1 1 d . . . Zn3 Zn 0.66691(3) 0.69216(2) 0.41424(2) 0.02359(10) Uani 1 1 d . . . Zn4 Zn 0.74313(2) 0.64679(2) 0.25494(2) 0.02246(10) 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 C1 0.027(2) 0.030(2) 0.036(2) 0.0136(18) 0.0119(18) 0.0031(17) C2 0.032(2) 0.065(3) 0.046(3) 0.030(3) 0.019(2) 0.009(2) C3 0.031(2) 0.046(3) 0.040(2) 0.023(2) 0.019(2) 0.019(2) C4 0.039(3) 0.054(3) 0.043(3) 0.012(2) 0.012(2) 0.001(2) C5 0.028(2) 0.038(2) 0.039(3) 0.006(2) 0.013(2) 0.0078(18) C6 0.035(2) 0.042(3) 0.036(2) 0.018(2) 0.005(2) 0.000(2) C7 0.044(3) 0.029(2) 0.029(2) 0.0046(18) 0.020(2) -0.0012(18) C8 0.051(3) 0.044(3) 0.028(2) 0.012(2) 0.016(2) -0.002(2) C9 0.053(3) 0.050(3) 0.027(2) 0.011(2) 0.012(2) 0.008(2) C10 0.059(3) 0.038(3) 0.044(3) 0.010(2) 0.014(3) -0.003(2) C11 0.037(2) 0.028(2) 0.040(3) 0.0020(19) 0.016(2) 0.0020(18) C12 0.029(2) 0.043(3) 0.038(3) 0.004(2) 0.007(2) 0.013(2) C13 0.028(2) 0.041(2) 0.030(2) 0.0155(19) 0.0132(18) 0.0074(18) C14 0.053(3) 0.041(3) 0.039(3) 0.024(2) 0.026(2) 0.018(2) C15 0.046(3) 0.049(3) 0.030(2) 0.025(2) 0.006(2) 0.000(2) C16 0.050(3) 0.042(3) 0.040(3) 0.021(2) 0.019(2) 0.013(2) C17 0.051(3) 0.047(3) 0.029(2) 0.008(2) 0.009(2) -0.011(2) C18 0.057(3) 0.042(3) 0.037(3) 0.006(2) 0.022(2) 0.006(2) C19 0.041(3) 0.033(2) 0.049(3) -0.001(2) 0.017(2) -0.016(2) C20 0.056(3) 0.029(2) 0.054(3) 0.005(2) 0.024(3) -0.008(2) C21 0.054(3) 0.032(3) 0.061(3) 0.011(2) 0.022(3) -0.004(2) C22 0.054(3) 0.042(3) 0.047(3) 0.000(2) 0.020(3) -0.011(2) C23 0.031(2) 0.040(3) 0.047(3) 0.007(2) 0.011(2) -0.011(2) C24 0.038(3) 0.043(3) 0.039(3) -0.006(2) 0.011(2) -0.023(2) C25 0.038(2) 0.035(2) 0.030(2) 0.0107(19) 0.0099(19) 0.0087(19) C26 0.051(3) 0.041(3) 0.042(3) 0.009(2) 0.008(2) 0.015(2) C27 0.050(3) 0.056(3) 0.041(3) 0.023(2) 0.020(2) 0.025(2) C28 0.051(3) 0.046(3) 0.038(3) 0.016(2) 0.015(2) 0.005(2) C29 0.029(2) 0.051(3) 0.031(2) 0.005(2) 0.0080(19) -0.006(2) C30 0.045(3) 0.040(3) 0.026(2) 0.0099(19) 0.008(2) -0.007(2) C31 0.049(3) 0.030(2) 0.044(3) 0.013(2) 0.017(2) 0.012(2) C32 0.044(3) 0.027(2) 0.049(3) 0.007(2) 0.022(2) 0.013(2) C33 0.054(3) 0.034(3) 0.037(3) 0.004(2) 0.012(2) -0.005(2) C34 0.062(3) 0.043(3) 0.028(2) 0.015(2) 0.003(2) 0.005(2) C35 0.050(3) 0.039(3) 0.036(3) 0.018(2) 0.009(2) 0.001(2) C36 0.048(3) 0.033(3) 0.050(3) 0.014(2) 0.017(2) 0.001(2) C37 0.053(3) 0.033(2) 0.030(2) 0.005(2) 0.016(2) -0.005(2) C38 0.055(3) 0.045(3) 0.022(2) 0.004(2) 0.020(2) 0.006(2) C39 0.056(3) 0.054(3) 0.036(3) 0.012(2) 0.011(2) -0.017(3) C40 0.055(3) 0.029(2) 0.049(3) 0.018(2) 0.012(2) 0.006(2) C41 0.038(3) 0.050(3) 0.039(3) 0.014(2) 0.010(2) -0.007(2) C42 0.047(3) 0.029(2) 0.041(3) 0.005(2) 0.008(2) -0.001(2) C43 0.038(2) 0.028(2) 0.037(2) 0.0173(19) 0.015(2) 0.0048(18) C44 0.047(3) 0.036(3) 0.042(3) 0.015(2) 0.009(2) -0.007(2) C45 0.064(4) 0.038(3) 0.049(3) 0.006(2) 0.026(3) -0.014(3) C46 0.043(3) 0.046(3) 0.039(3) 0.020(2) 0.012(2) 0.000(2) C47 0.045(3) 0.043(3) 0.033(2) 0.018(2) 0.015(2) 0.005(2) C48 0.075(4) 0.033(3) 0.048(3) 0.027(2) 0.038(3) 0.026(2) C49 0.039(2) 0.053(3) 0.033(2) 0.021(2) 0.021(2) 0.021(2) C50 0.033(2) 0.054(3) 0.037(3) 0.015(2) 0.015(2) 0.004(2) C51 0.031(2) 0.041(3) 0.051(3) 0.020(2) 0.011(2) 0.006(2) C52 0.039(3) 0.046(3) 0.036(3) 0.007(2) 0.007(2) -0.013(2) C53 0.033(2) 0.043(3) 0.035(2) 0.022(2) -0.0035(19) -0.013(2) C54 0.047(3) 0.053(3) 0.034(3) 0.025(2) 0.014(2) 0.011(2) C55 0.038(3) 0.056(3) 0.029(2) 0.007(2) 0.011(2) -0.010(2) C56 0.039(2) 0.021(2) 0.045(3) 0.0046(19) 0.013(2) -0.0019(18) C57 0.036(3) 0.045(3) 0.041(3) 0.020(2) 0.010(2) 0.002(2) C58 0.045(3) 0.053(3) 0.041(3) 0.013(2) 0.015(2) 0.002(2) C59 0.051(3) 0.049(3) 0.035(3) 0.006(2) 0.020(2) 0.001(2) C60 0.054(3) 0.045(3) 0.039(3) -0.002(2) 0.020(2) -0.006(2) C61 0.052(3) 0.050(3) 0.035(3) 0.019(2) 0.013(2) 0.009(2) C62 0.046(3) 0.044(3) 0.039(3) 0.019(2) 0.009(2) 0.004(2) C63 0.042(3) 0.047(3) 0.029(2) 0.013(2) 0.007(2) -0.002(2) C64 0.035(3) 0.044(3) 0.040(3) 0.010(2) 0.007(2) -0.004(2) C65 0.054(3) 0.038(3) 0.059(3) 0.020(2) 0.025(3) 0.004(2) C66 0.049(3) 0.053(3) 0.047(3) 0.014(3) 0.003(3) -0.001(3) C67 0.057(3) 0.043(3) 0.039(3) 0.016(2) 0.015(2) 0.017(2) C68 0.053(3) 0.052(3) 0.026(2) 0.014(2) 0.009(2) 0.004(2) C69 0.044(3) 0.042(3) 0.047(3) 0.011(2) 0.012(2) 0.006(2) C70 0.052(3) 0.047(3) 0.041(3) 0.009(2) 0.012(2) -0.001(2) C71 0.036(3) 0.040(3) 0.042(3) 0.009(2) 0.008(2) -0.009(2) C72 0.050(3) 0.039(3) 0.035(3) 0.000(2) 0.008(2) -0.004(2) C73 0.044(3) 0.048(3) 0.038(3) 0.013(2) 0.015(2) 0.004(2) C74 0.059(3) 0.040(3) 0.037(3) 0.009(2) 0.013(2) -0.004(2) C75 0.046(3) 0.052(3) 0.024(2) 0.000(2) 0.006(2) 0.003(2) C76 0.045(3) 0.049(3) 0.040(3) 0.019(2) 0.016(2) -0.001(2) C77 0.043(3) 0.037(3) 0.039(3) 0.005(2) 0.003(2) -0.008(2) C78 0.045(3) 0.043(3) 0.051(3) 0.004(2) 0.010(3) -0.010(2) C79 0.048(3) 0.046(3) 0.041(3) 0.017(2) 0.011(2) -0.004(2) C80 0.042(3) 0.043(3) 0.044(3) 0.011(2) 0.010(2) -0.013(2) C81 0.054(3) 0.047(3) 0.028(2) 0.016(2) 0.013(2) -0.003(2) C82 0.034(2) 0.061(3) 0.034(2) 0.025(2) 0.010(2) 0.004(2) C83 0.036(2) 0.043(3) 0.047(3) 0.020(2) 0.009(2) -0.005(2) C84 0.046(3) 0.048(3) 0.060(3) 0.000(3) 0.023(3) -0.018(2) C85 0.042(3) 0.045(3) 0.044(3) 0.012(2) 0.009(2) -0.005(2) C86 0.038(3) 0.039(3) 0.038(3) -0.006(2) 0.007(2) -0.005(2) C87 0.051(3) 0.031(2) 0.032(2) -0.0001(19) 0.013(2) -0.010(2) C88 0.034(2) 0.039(3) 0.048(3) 0.010(2) 0.009(2) -0.016(2) C89 0.039(3) 0.042(3) 0.041(3) 0.021(2) 0.014(2) 0.013(2) C90 0.052(3) 0.046(3) 0.040(3) 0.004(2) 0.017(2) -0.001(2) C91 0.046(3) 0.044(3) 0.041(3) 0.012(2) 0.025(2) 0.008(2) C92 0.044(3) 0.033(2) 0.052(3) 0.020(2) 0.018(2) 0.005(2) C93 0.054(3) 0.038(3) 0.039(3) 0.011(2) 0.018(2) 0.011(2) P1 0.0648(11) 0.0677(11) 0.0628(11) 0.0121(9) 0.0148(9) 0.0016(9) F1 0.073(2) 0.082(3) 0.052(2) 0.0103(19) 0.0152(19) -0.013(2) F2 0.072(2) 0.067(2) 0.058(2) 0.0138(19) 0.0114(19) 0.0080(19) F3 0.068(2) 0.071(2) 0.053(2) 0.0078(18) 0.0108(18) -0.0021(19) F4 0.083(3) 0.067(2) 0.060(2) 0.0175(19) 0.015(2) 0.011(2) F5 0.070(2) 0.070(2) 0.057(2) 0.0152(19) 0.0120(19) 0.0029(19) F6 0.071(2) 0.064(2) 0.059(2) 0.0151(18) 0.0180(19) 0.0073(18) P2 0.0677(11) 0.0649(11) 0.0617(11) 0.0094(9) 0.0169(9) -0.0075(9) F7 0.071(2) 0.075(3) 0.064(2) 0.015(2) 0.022(2) -0.004(2) F8 0.076(3) 0.065(2) 0.061(2) 0.0147(19) 0.017(2) 0.0075(19) F9 0.076(2) 0.060(2) 0.050(2) 0.0088(17) 0.0089(18) -0.0020(19) F10 0.075(3) 0.066(2) 0.069(2) 0.012(2) 0.016(2) 0.005(2) F11 0.077(3) 0.069(2) 0.061(2) 0.0147(19) 0.018(2) 0.006(2) F12 0.072(2) 0.069(2) 0.058(2) 0.0179(18) 0.0167(19) 0.0041(19) P3 0.0729(12) 0.0625(11) 0.0606(11) 0.0127(9) 0.0129(9) 0.0048(9) F13 0.078(3) 0.056(2) 0.062(2) 0.0123(18) 0.017(2) 0.0047(19) F14 0.078(3) 0.059(2) 0.069(2) 0.0148(19) 0.017(2) 0.0073(19) F15 0.083(3) 0.060(2) 0.065(2) 0.0174(19) 0.015(2) 0.013(2) F16 0.088(3) 0.062(2) 0.056(2) 0.0089(18) 0.017(2) 0.012(2) F17 0.078(3) 0.062(2) 0.066(2) -0.0006(19) 0.013(2) -0.005(2) F18 0.079(3) 0.076(3) 0.080(3) 0.009(2) 0.025(2) 0.003(2) P4 0.0666(11) 0.0677(11) 0.0629(11) 0.0157(9) 0.0144(9) -0.0012(9) F19 0.072(2) 0.079(3) 0.062(2) 0.016(2) 0.015(2) -0.012(2) F20 0.078(3) 0.076(3) 0.081(3) 0.010(2) 0.025(2) 0.004(2) F21 0.082(3) 0.080(3) 0.062(2) 0.014(2) 0.015(2) -0.007(2) F22 0.070(3) 0.070(3) 0.079(3) 0.002(2) 0.013(2) -0.011(2) F23 0.071(2) 0.067(2) 0.069(2) 0.0176(19) 0.018(2) 0.0017(19) F24 0.077(3) 0.081(3) 0.077(3) 0.020(2) 0.026(2) 0.000(2) P5 0.0739(12) 0.0710(12) 0.0538(10) 0.0112(9) 0.0121(9) 0.0033(9) F25 0.071(2) 0.070(2) 0.062(2) 0.0146(19) 0.0133(19) 0.018(2) F26 0.073(3) 0.076(3) 0.052(2) 0.0086(19) 0.0120(19) 0.006(2) F27 0.083(3) 0.074(3) 0.057(2) 0.0081(19) 0.022(2) 0.010(2) F28 0.075(3) 0.070(3) 0.076(3) 0.020(2) 0.024(2) 0.013(2) F29 0.087(3) 0.074(3) 0.067(2) 0.019(2) 0.026(2) 0.014(2) F30 0.073(2) 0.064(2) 0.053(2) 0.0106(18) 0.0091(18) 0.0021(19) P6 0.0717(12) 0.0611(11) 0.0622(11) 0.0124(9) 0.0131(9) 0.0061(9) F31 0.080(3) 0.055(2) 0.060(2) 0.0134(18) 0.0182(19) 0.0082(18) F32 0.079(3) 0.056(2) 0.070(2) 0.0173(19) 0.015(2) 0.0104(19) F33 0.081(3) 0.057(2) 0.067(2) 0.0154(18) 0.017(2) 0.0134(19) F34 0.085(3) 0.064(2) 0.058(2) 0.0113(18) 0.020(2) 0.018(2) F35 0.076(3) 0.066(2) 0.070(3) 0.012(2) 0.016(2) 0.005(2) F36 0.084(3) 0.081(3) 0.057(2) 0.001(2) 0.015(2) -0.008(2) P7 0.0697(11) 0.0647(11) 0.0606(11) 0.0090(9) 0.0136(9) 0.0009(9) F37 0.084(3) 0.057(2) 0.061(2) 0.0087(18) 0.018(2) 0.0051(19) F38 0.089(3) 0.064(2) 0.060(2) 0.0068(19) 0.016(2) -0.011(2) F39 0.087(3) 0.056(2) 0.067(2) 0.0122(19) 0.020(2) 0.006(2) F40 0.068(2) 0.060(2) 0.061(2) 0.0096(18) 0.0177(19) 0.0006(18) F41 0.075(3) 0.073(2) 0.056(2) 0.0186(19) 0.0120(19) 0.005(2) F42 0.091(3) 0.068(2) 0.060(2) 0.0109(19) 0.016(2) 0.013(2) P8 0.0795(13) 0.0568(10) 0.0573(10) 0.0068(8) 0.0112(9) -0.0037(9) F43 0.077(3) 0.066(2) 0.058(2) 0.0154(19) 0.0143(19) 0.009(2) F44 0.086(3) 0.069(3) 0.061(2) 0.014(2) 0.015(2) -0.002(2) F45 0.072(2) 0.069(2) 0.058(2) 0.0175(19) 0.0113(19) 0.0031(19) F46 0.085(3) 0.069(3) 0.068(2) 0.020(2) 0.023(2) 0.011(2) F47 0.074(3) 0.081(3) 0.062(2) 0.010(2) 0.015(2) 0.000(2) F48 0.071(2) 0.061(2) 0.069(2) 0.0101(19) 0.010(2) 0.0025(19) N1 0.048(2) 0.043(2) 0.044(2) 0.0195(19) 0.020(2) -0.0012(19) N2 0.044(2) 0.042(2) 0.038(2) 0.0099(18) 0.0143(19) -0.0105(18) N3 0.043(2) 0.038(2) 0.042(2) 0.0184(18) 0.0171(19) 0.0132(18) N4 0.046(2) 0.043(2) 0.041(2) 0.0075(19) 0.010(2) -0.0052(19) N5 0.037(2) 0.051(3) 0.036(2) 0.0135(19) 0.0097(18) 0.0041(19) N6 0.043(2) 0.043(2) 0.049(3) 0.007(2) 0.014(2) -0.0191(19) N7 0.051(3) 0.041(2) 0.043(2) 0.0176(19) 0.013(2) -0.0027(19) N8 0.033(2) 0.043(2) 0.045(2) 0.0209(19) 0.0096(18) 0.0002(17) N9 0.035(2) 0.048(2) 0.044(2) 0.0139(19) 0.0216(19) 0.0061(18) N10 0.044(2) 0.050(3) 0.039(2) 0.007(2) 0.009(2) -0.007(2) N11 0.041(2) 0.034(2) 0.046(2) 0.0119(18) 0.0210(19) 0.0042(17) O1 0.0419(17) 0.0418(17) 0.0408(17) 0.0115(14) 0.0358(15) 0.0033(14) O1W 0.028(6) 0.098(11) 0.023(6) 0.001(6) -0.008(5) -0.014(6) O2W 0.073(9) 0.032(6) 0.062(8) 0.024(6) 0.006(7) 0.008(6) O3W 0.052(7) 0.062(8) 0.037(7) -0.002(6) 0.015(6) -0.016(6) O4W 0.051(7) 0.038(6) 0.049(7) 0.014(5) 0.020(6) 0.010(5) O5W 0.043(7) 0.105(13) 0.072(10) 0.041(9) 0.015(7) 0.034(8) O6W 0.047(7) 0.058(7) 0.029(6) 0.017(5) 0.007(5) -0.009(6) O7W 0.072(9) 0.059(9) 0.044(7) 0.014(6) 0.006(7) -0.014(7) O8W 0.064(8) 0.048(7) 0.045(6) 0.014(5) 0.040(6) 0.030(6) O9W 0.050(7) 0.065(8) 0.031(6) 0.004(6) 0.009(5) 0.018(6) O10W 0.063(8) 0.042(7) 0.027(6) -0.009(5) 0.012(6) -0.006(6) O11W 0.051(5) 0.035(4) 0.052(5) 0.028(4) 0.021(4) 0.030(4) O12W 0.059(6) 0.038(5) 0.052(6) -0.021(4) 0.016(5) -0.028(4) O13W 0.065(8) 0.045(7) 0.048(7) 0.002(6) 0.023(6) -0.020(6) S1 0.0240(5) 0.0287(5) 0.0251(5) 0.0131(4) 0.0111(4) 0.0014(4) S2 0.0251(5) 0.0242(5) 0.0255(5) 0.0131(4) 0.0109(4) 0.0013(4) S3 0.0240(5) 0.0276(5) 0.0251(5) 0.0134(4) 0.0122(4) 0.0011(4) S4 0.0222(4) 0.0226(5) 0.0267(5) 0.0131(4) 0.0123(4) 0.0007(3) S5 0.0292(5) 0.0228(5) 0.0245(5) 0.0131(4) 0.0103(4) -0.0004(4) S6 0.0264(5) 0.0251(5) 0.0252(5) 0.0135(4) 0.0133(4) 0.0037(4) S7 0.0291(5) 0.0259(5) 0.0252(5) 0.0137(4) 0.0130(4) 0.0038(4) S8 0.0212(4) 0.0283(5) 0.0255(5) 0.0140(4) 0.0146(4) 0.0032(4) S9 0.0276(5) 0.0216(4) 0.0254(5) 0.0137(4) 0.0133(4) 0.0023(4) S10 0.0271(5) 0.0293(5) 0.0235(5) 0.0115(4) 0.0072(4) -0.0039(4) Zn1 0.0251(2) 0.0247(2) 0.0252(2) 0.01303(18) 0.01116(18) 0.00138(17) Zn2 0.0238(2) 0.0281(2) 0.0262(2) 0.01320(19) 0.01225(19) 0.00224(18) Zn3 0.0260(2) 0.0234(2) 0.0248(2) 0.01323(18) 0.01196(19) 0.00150(17) Zn4 0.0222(2) 0.0226(2) 0.0267(2) 0.01305(18) 0.01230(18) 0.00071(16) _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 C1 C2 1.332(7) . ? C1 C6 1.396(6) . ? C1 S1 1.740(4) . ? C2 C3 1.403(6) . ? C2 H2 0.9300 . ? C3 C4 1.409(7) . ? C3 H3 0.9300 . ? C4 C5 1.339(7) . ? C4 N1 1.520(5) . ? C5 C6 1.390(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.399(7) . ? C7 C8 1.407(6) . ? C7 S2 1.714(4) . ? C8 C9 1.394(7) . ? C8 H8 0.9300 . ? C9 C10 1.414(8) . ? C9 H9 0.9300 . ? C10 C11 1.401(7) . ? C10 N2 1.516(6) . ? C11 C12 1.371(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.381(7) . ? C13 C14 1.401(6) . ? C13 S3 1.699(4) . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C15 C16 1.382(7) . ? C15 H15 0.9300 . ? C16 C17 1.394(7) . ? C16 N3 1.482(5) . ? C17 C18 1.428(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.381(8) . ? C19 C24 1.403(7) . ? C19 S4 1.666(4) . ? C20 C21 1.389(7) . ? C20 H20 0.9300 . ? C21 C22 1.398(8) . ? C21 H21 0.9300 . ? C22 N4 1.394(5) . ? C22 C23 1.403(8) . ? C23 C24 1.347(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.347(7) . ? C25 C26 1.445(7) . ? C25 S5 1.865(5) . ? C26 C27 1.391(7) . ? C26 H26 0.9300 . ? C27 C28 1.384(7) . ? C27 H27 0.9300 . ? C28 C29 1.432(8) . ? C28 N5 1.502(5) . ? C29 C30 1.378(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.398(7) . ? C31 C32 1.406(7) . ? C31 S6 1.692(5) . ? C32 C33 1.383(7) . ? C32 H32 0.9300 . ? C33 C34 1.406(8) . ? C33 H33 0.9300 . ? C34 C35 1.376(8) . ? C34 N6 1.488(5) . ? C35 C36 1.399(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.379(7) . ? C37 C38 1.400(7) . ? C37 S7 1.828(5) . ? C38 C39 1.361(7) . ? C38 H38 0.9300 . ? C39 C40 1.418(7) . ? C39 H39 0.9300 . ? C40 C41 1.372(7) . ? C40 N7 1.577(5) . ? C41 C42 1.388(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.368(7) . ? C43 C48 1.382(7) . ? C43 S8 1.606(4) . ? C44 C45 1.385(7) . ? C44 H44 0.9300 . ? C45 C46 1.394(8) . ? C45 H45 0.9300 . ? C46 N8 1.329(5) . ? C46 C47 1.405(7) . ? C47 C48 1.377(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.386(7) . ? C49 C54 1.388(7) . ? C49 S9 1.783(5) . ? C50 C51 1.401(7) . ? C50 H50 0.9300 . ? C51 C52 1.390(7) . ? C51 H51 0.9300 . ? C52 C53 1.382(7) . ? C52 N9 1.517(5) . ? C53 C54 1.382(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.368(6) . ? C55 C60 1.396(7) . ? C55 S10 1.715(5) . ? C56 C57 1.368(7) . ? C56 H56 0.9300 . ? C57 C58 1.387(8) . ? C57 H57 0.9300 . ? C58 C59 1.407(7) . ? C58 N10 1.481(6) . ? C59 C60 1.334(8) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 N1 1.439(5) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 N1 1.543(5) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 N1 1.541(5) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 N2 1.506(5) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 N2 1.475(6) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 N2 1.581(6) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 N3 1.473(5) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 N3 1.368(5) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N3 1.546(5) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 N4 1.530(5) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 N4 1.485(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N4 1.557(6) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 N5 1.448(5) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 N5 1.470(5) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 N5 1.583(5) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 N6 1.535(5) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 N6 1.441(5) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 N6 1.573(6) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 N7 1.603(6) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 N7 1.507(6) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 N7 1.443(5) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 N8 1.546(5) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 N8 1.541(5) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 N8 1.574(6) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 N9 1.412(5) . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 N9 1.470(5) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 N9 1.486(5) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 N10 1.526(5) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 N10 1.561(5) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 N10 1.512(6) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 N11 1.259(5) . ? C91 O1 1.275(5) . ? C91 H91 0.9300 . ? C92 N11 1.462(5) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 N11 1.503(5) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? P1 F5 1.528(5) . ? P1 F1 1.545(4) . ? P1 F6 1.561(4) . ? P1 F2 1.569(5) . ? P1 F4 1.636(5) . ? P1 F3 1.637(4) . ? P2 F7 1.502(5) . ? P2 F9 1.505(4) . ? P2 F10 1.569(5) . ? P2 F12 1.599(5) . ? P2 F11 1.604(5) . ? P2 F8 1.652(5) . ? P3 F13 1.410(4) . ? P3 F15 1.441(5) . ? P3 F14 1.468(5) . ? P3 F17 1.563(4) . ? P3 F18 1.598(5) . ? P3 F16 1.734(5) . ? P4 F22 1.539(5) . ? P4 F24 1.546(5) . ? P4 F23 1.549(5) . ? P4 F19 1.561(4) . ? P4 F20 1.579(5) . ? P4 F21 1.603(4) . ? P5 F29 1.492(5) . ? P5 F30 1.522(4) . ? P5 F27 1.580(4) . ? P5 F25 1.580(4) . ? P5 F26 1.592(5) . ? P5 F28 1.637(5) . ? P6 F32 1.452(5) . ? P6 F34 1.517(5) . ? P6 F35 1.550(4) . ? P6 F33 1.593(5) . ? P6 F36 1.652(4) . ? P6 F31 1.725(5) . ? P7 F39 1.465(5) . ? P7 F37 1.492(5) . ? P7 F38 1.548(4) . ? P7 F40 1.600(4) . ? P7 F42 1.619(5) . ? P7 F41 1.627(5) . ? P8 F44 1.432(5) . ? P8 F47 1.501(5) . ? P8 F48 1.567(4) . ? P8 F45 1.580(5) . ? P8 F43 1.593(5) . ? P8 F46 1.641(5) . ? O1W H1X 0.8417 . ? O1W H1Y 0.8053 . ? O2W H2X 0.8502 . ? O2W H2Y 0.8502 . ? O3W H3X 0.8496 . ? O3W H3Y 0.8508 . ? O4W H4X 0.8302 . ? O4W H4Y 0.8086 . ? O5W H5X 0.8578 . ? O5W H5Y 0.8459 . ? O6W H6X 0.8494 . ? O6W H6Y 0.8510 . ? O7W H7X 0.8542 . ? O7W H7Y 0.8254 . ? O8W H8X 0.8333 . ? O8W H8Y 0.8152 . ? O9W H9X 0.8029 . ? O9W H9Y 0.8819 . ? O10W H10X 0.8695 . ? O10W H10Y 0.8724 . ? O11W H11X 0.8319 . ? O11W H11Y 0.8609 . ? O12W H12X 0.8268 . ? O12W H12Y 0.8818 . ? O13W H13X 0.8499 . ? O13W H13Y 0.8500 . ? S1 Zn2 2.5161(11) . ? S1 Zn1 2.5645(11) . ? S2 Zn3 2.4496(10) . ? S2 Zn1 2.5231(10) . ? S3 Zn2 2.4960(10) . ? S3 Zn3 2.6145(11) . ? S4 Zn4 2.4940(10) . ? S4 Zn3 2.5677(11) . ? S5 Zn4 2.4698(10) . ? S5 Zn1 2.5392(11) . ? S6 Zn2 2.5210(11) . ? S6 Zn4 2.6699(11) . ? S7 Zn1 2.3750(11) . ? S8 Zn2 2.5340(11) . ? S9 Zn3 2.4271(11) . ? S10 Zn4 2.4664(11) . ? 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 C2 C1 C6 120.8(4) . . ? C2 C1 S1 119.0(4) . . ? C6 C1 S1 120.2(4) . . ? C1 C2 C3 117.2(5) . . ? C1 C2 H2 121.4 . . ? C3 C2 H2 121.4 . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 121.7(5) . . ? C5 C4 N1 116.7(4) . . ? C3 C4 N1 121.0(4) . . ? C4 C5 C6 115.9(5) . . ? C4 C5 H5 122.0 . . ? C6 C5 H5 122.0 . . ? C5 C6 C1 122.9(5) . . ? C5 C6 H6 118.5 . . ? C1 C6 H6 118.5 . . ? C12 C7 C8 118.9(4) . . ? C12 C7 S2 121.4(4) . . ? C8 C7 S2 119.7(4) . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.3(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.0(5) . . ? C11 C10 N2 121.9(4) . . ? C9 C10 N2 118.8(4) . . ? C12 C11 C10 120.2(5) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 121.6(5) . . ? C11 C12 H12 119.2 . . ? C7 C12 H12 119.2 . . ? C18 C13 C14 119.5(4) . . ? C18 C13 S3 126.0(4) . . ? C14 C13 S3 114.3(4) . . ? C15 C14 C13 121.2(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 120.7(5) . . ? C15 C16 N3 121.8(4) . . ? C17 C16 N3 117.3(4) . . ? C16 C17 C18 119.2(5) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C13 C18 C17 119.6(5) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C24 120.9(4) . . ? C20 C19 S4 126.9(4) . . ? C24 C19 S4 112.0(4) . . ? C19 C20 C21 120.7(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 118.4(6) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N4 C22 C21 118.5(5) . . ? N4 C22 C23 122.0(5) . . ? C21 C22 C23 119.5(5) . . ? C24 C23 C22 122.3(5) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C19 118.2(5) . . ? C23 C24 H24 120.9 . . ? C19 C24 H24 120.9 . . ? C30 C25 C26 117.5(5) . . ? C30 C25 S5 120.4(4) . . ? C26 C25 S5 122.0(4) . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 122.4(5) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.2(5) . . ? C27 C28 N5 123.1(5) . . ? C29 C28 N5 120.7(4) . . ? C30 C29 C28 121.3(5) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C25 C30 C29 122.7(5) . . ? C25 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C36 C31 C32 120.8(5) . . ? C36 C31 S6 116.0(4) . . ? C32 C31 S6 123.2(4) . . ? C33 C32 C31 119.1(5) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.3(5) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 120.1(5) . . ? C35 C34 N6 130.1(5) . . ? C33 C34 N6 109.8(4) . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C31 C36 C35 119.0(5) . . ? C31 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C42 C37 C38 117.7(5) . . ? C42 C37 S7 115.5(4) . . ? C38 C37 S7 126.6(4) . . ? C39 C38 C37 121.2(5) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 119.8(5) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 119.8(5) . . ? C41 C40 N7 123.1(4) . . ? C39 C40 N7 116.8(4) . . ? C40 C41 C42 118.7(5) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? C37 C42 C41 122.5(5) . . ? C37 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? C44 C43 C48 118.9(4) . . ? C44 C43 S8 120.6(4) . . ? C48 C43 S8 120.0(4) . . ? C43 C44 C45 122.9(5) . . ? C43 C44 H44 118.6 . . ? C45 C44 H44 118.6 . . ? C44 C45 C46 117.1(5) . . ? C44 C45 H45 121.4 . . ? C46 C45 H45 121.4 . . ? N8 C46 C45 121.6(5) . . ? N8 C46 C47 117.0(4) . . ? C45 C46 C47 121.1(5) . . ? C48 C47 C46 118.8(5) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 C43 121.0(5) . . ? C47 C48 H48 119.5 . . ? C43 C48 H48 119.5 . . ? C50 C49 C54 120.2(5) . . ? C50 C49 S9 117.6(4) . . ? C54 C49 S9 122.2(4) . . ? C49 C50 C51 119.5(5) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120.0(5) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C53 C52 C51 119.7(5) . . ? C53 C52 N9 119.1(4) . . ? C51 C52 N9 121.1(4) . . ? C52 C53 C54 120.7(5) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C49 119.9(5) . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? C56 C55 C60 121.4(5) . . ? C56 C55 S10 122.5(4) . . ? C60 C55 S10 115.8(4) . . ? C57 C56 C55 119.5(5) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 118.0(5) . . ? C56 C57 H57 121.0 . . ? C58 C57 H57 121.0 . . ? C57 C58 C59 122.8(5) . . ? C57 C58 N10 115.4(4) . . ? C59 C58 N10 121.8(4) . . ? C60 C59 C58 117.4(5) . . ? C60 C59 H59 121.3 . . ? C58 C59 H59 121.3 . . ? C59 C60 C55 120.7(5) . . ? C59 C60 H60 119.7 . . ? C55 C60 H60 119.7 . . ? N1 C61 H61A 109.5 . . ? N1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N1 C62 H62A 109.5 . . ? N1 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N1 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N1 C63 H63A 109.5 . . ? N1 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N1 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N2 C64 H64A 109.5 . . ? N2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N2 C65 H65A 109.5 . . ? N2 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N2 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N2 C66 H66A 109.5 . . ? N2 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N2 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N3 C67 H67A 109.5 . . ? N3 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N3 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N3 C68 H68A 109.5 . . ? N3 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N3 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N3 C69 H69A 109.5 . . ? N3 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N3 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N4 C70 H70A 109.5 . . ? N4 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N4 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N4 C71 H71A 109.5 . . ? N4 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N4 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N4 C72 H72A 109.5 . . ? N4 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N4 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N5 C73 H73A 109.5 . . ? N5 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N5 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 H74A 109.5 . . ? N5 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N5 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N5 C75 H75A 109.5 . . ? N5 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N5 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N6 C76 H76A 109.5 . . ? N6 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N6 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N6 C77 H77A 109.5 . . ? N6 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N6 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N6 C78 H78A 109.5 . . ? N6 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N6 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N7 C79 H79A 109.5 . . ? N7 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N7 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N7 C80 H80A 109.5 . . ? N7 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N7 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N7 C81 H81A 109.5 . . ? N7 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N7 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N8 C82 H82A 109.5 . . ? N8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N8 C83 H83A 109.5 . . ? N8 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N8 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N8 C84 H84A 109.5 . . ? N8 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N8 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N9 C85 H85A 109.5 . . ? N9 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? N9 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N9 C86 H86A 109.5 . . ? N9 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N9 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N9 C87 H87A 109.5 . . ? N9 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N9 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N10 C88 H88A 109.5 . . ? N10 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N10 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N10 C89 H89A 109.5 . . ? N10 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N10 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N10 C90 H90A 109.5 . . ? N10 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N10 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N11 C91 O1 117.6(4) . . ? N11 C91 H91 121.2 . . ? O1 C91 H91 121.2 . . ? N11 C92 H92A 109.5 . . ? N11 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N11 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N11 C93 H93A 109.5 . . ? N11 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N11 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? F5 P1 F1 86.8(2) . . ? F5 P1 F6 176.4(3) . . ? F1 P1 F6 96.6(2) . . ? F5 P1 F2 89.7(2) . . ? F1 P1 F2 86.9(2) . . ? F6 P1 F2 91.3(2) . . ? F5 P1 F4 89.4(2) . . ? F1 P1 F4 95.3(2) . . ? F6 P1 F4 89.5(2) . . ? F2 P1 F4 177.5(3) . . ? F5 P1 F3 94.5(2) . . ? F1 P1 F3 178.6(3) . . ? F6 P1 F3 82.0(2) . . ? F2 P1 F3 93.4(2) . . ? F4 P1 F3 84.4(2) . . ? F7 P2 F9 179.3(3) . . ? F7 P2 F10 93.8(3) . . ? F9 P2 F10 86.1(2) . . ? F7 P2 F12 92.9(2) . . ? F9 P2 F12 87.8(2) . . ? F10 P2 F12 87.6(2) . . ? F7 P2 F11 90.9(2) . . ? F9 P2 F11 88.4(2) . . ? F10 P2 F11 91.7(2) . . ? F12 P2 F11 176.2(3) . . ? F7 P2 F8 86.2(2) . . ? F9 P2 F8 94.0(2) . . ? F10 P2 F8 179.6(3) . . ? F12 P2 F8 92.7(2) . . ? F11 P2 F8 87.9(2) . . ? F13 P3 F15 162.0(3) . . ? F13 P3 F14 97.0(3) . . ? F15 P3 F14 92.4(3) . . ? F13 P3 F17 102.5(3) . . ? F15 P3 F17 89.1(3) . . ? F14 P3 F17 107.9(3) . . ? F13 P3 F18 81.7(3) . . ? F15 P3 F18 83.8(3) . . ? F14 P3 F18 85.5(3) . . ? F17 P3 F18 165.1(3) . . ? F13 P3 F16 77.3(2) . . ? F15 P3 F16 90.1(3) . . ? F14 P3 F16 166.5(2) . . ? F17 P3 F16 85.5(2) . . ? F18 P3 F16 81.5(2) . . ? F22 P4 F24 92.5(3) . . ? F22 P4 F23 86.1(3) . . ? F24 P4 F23 177.4(3) . . ? F22 P4 F19 82.6(3) . . ? F24 P4 F19 86.2(2) . . ? F23 P4 F19 91.5(2) . . ? F22 P4 F20 171.4(3) . . ? F24 P4 F20 82.9(3) . . ? F23 P4 F20 98.2(3) . . ? F19 P4 F20 89.9(3) . . ? F22 P4 F21 98.3(3) . . ? F24 P4 F21 93.8(3) . . ? F23 P4 F21 88.6(2) . . ? F19 P4 F21 179.1(3) . . ? F20 P4 F21 89.3(3) . . ? F29 P5 F30 178.0(3) . . ? F29 P5 F27 86.9(2) . . ? F30 P5 F27 94.6(2) . . ? F29 P5 F25 92.0(2) . . ? F30 P5 F25 86.4(2) . . ? F27 P5 F25 177.6(3) . . ? F29 P5 F26 84.0(3) . . ? F30 P5 F26 97.2(3) . . ? F27 P5 F26 92.3(2) . . ? F25 P5 F26 89.6(2) . . ? F29 P5 F28 94.3(3) . . ? F30 P5 F28 84.4(2) . . ? F27 P5 F28 89.4(2) . . ? F25 P5 F28 88.6(2) . . ? F26 P5 F28 177.5(3) . . ? F32 P6 F34 177.5(3) . . ? F32 P6 F35 95.0(3) . . ? F34 P6 F35 83.5(2) . . ? F32 P6 F33 89.2(3) . . ? F34 P6 F33 88.7(2) . . ? F35 P6 F33 88.3(2) . . ? F32 P6 F36 82.2(2) . . ? F34 P6 F36 98.8(3) . . ? F35 P6 F36 166.7(3) . . ? F33 P6 F36 78.7(2) . . ? F32 P6 F31 98.0(3) . . ? F34 P6 F31 84.1(2) . . ? F35 P6 F31 90.3(2) . . ? F33 P6 F31 172.8(2) . . ? F36 P6 F31 103.0(2) . . ? F39 P7 F37 172.7(3) . . ? F39 P7 F38 87.4(2) . . ? F37 P7 F38 85.9(2) . . ? F39 P7 F40 94.9(2) . . ? F37 P7 F40 91.8(2) . . ? F38 P7 F40 177.7(3) . . ? F39 P7 F42 90.3(3) . . ? F37 P7 F42 86.9(3) . . ? F38 P7 F42 91.8(3) . . ? F40 P7 F42 87.7(2) . . ? F39 P7 F41 91.8(3) . . ? F37 P7 F41 91.9(3) . . ? F38 P7 F41 95.2(2) . . ? F40 P7 F41 85.2(2) . . ? F42 P7 F41 172.8(2) . . ? F44 P8 F47 83.4(3) . . ? F44 P8 F48 86.2(3) . . ? F47 P8 F48 169.1(3) . . ? F44 P8 F45 92.9(3) . . ? F47 P8 F45 95.3(2) . . ? F48 P8 F45 88.4(2) . . ? F44 P8 F43 95.4(3) . . ? F47 P8 F43 84.5(3) . . ? F48 P8 F43 93.3(2) . . ? F45 P8 F43 171.6(3) . . ? F44 P8 F46 168.4(3) . . ? F47 P8 F46 103.1(3) . . ? F48 P8 F46 86.7(2) . . ? F45 P8 F46 96.0(2) . . ? F43 P8 F46 75.9(2) . . ? C61 N1 C4 106.9(3) . . ? C61 N1 C63 113.2(3) . . ? C4 N1 C63 116.5(3) . . ? C61 N1 C62 111.1(3) . . ? C4 N1 C62 104.1(3) . . ? C63 N1 C62 104.6(3) . . ? C65 N2 C64 108.8(3) . . ? C65 N2 C10 105.6(2) . . ? C64 N2 C10 109.0(3) . . ? C65 N2 C66 116.5(3) . . ? C64 N2 C66 106.5(3) . . ? C10 N2 C66 110.3(3) . . ? C68 N3 C67 117.8(3) . . ? C68 N3 C16 112.9(3) . . ? C67 N3 C16 113.8(3) . . ? C68 N3 C69 108.7(3) . . ? C67 N3 C69 96.9(3) . . ? C16 N3 C69 104.4(3) . . ? C22 N4 C71 107.1(3) . . ? C22 N4 C70 107.6(3) . . ? C71 N4 C70 110.6(3) . . ? C22 N4 C72 113.6(3) . . ? C71 N4 C72 106.5(3) . . ? C70 N4 C72 111.4(3) . . ? C73 N5 C74 109.7(3) . . ? C73 N5 C28 109.7(3) . . ? C74 N5 C28 114.3(3) . . ? C73 N5 C75 101.5(3) . . ? C74 N5 C75 106.2(3) . . ? C28 N5 C75 114.7(3) . . ? C77 N6 C34 104.0(3) . . ? C77 N6 C76 106.8(3) . . ? C34 N6 C76 105.2(3) . . ? C77 N6 C78 95.9(3) . . ? C34 N6 C78 115.8(3) . . ? C76 N6 C78 126.1(3) . . ? C81 N7 C80 101.9(3) . . ? C81 N7 C40 109.3(3) . . ? C80 N7 C40 108.8(3) . . ? C81 N7 C79 110.5(3) . . ? C80 N7 C79 114.7(3) . . ? C40 N7 C79 111.1(3) . . ? C46 N8 C83 113.2(3) . . ? C46 N8 C82 102.4(3) . . ? C83 N8 C82 115.8(3) . . ? C46 N8 C84 110.8(3) . . ? C83 N8 C84 103.7(3) . . ? C82 N8 C84 111.2(3) . . ? C85 N9 C86 110.6(3) . . ? C85 N9 C87 102.6(3) . . ? C86 N9 C87 113.4(3) . . ? C85 N9 C52 112.4(3) . . ? C86 N9 C52 110.4(3) . . ? C87 N9 C52 107.3(3) . . ? C58 N10 C90 105.2(3) . . ? C58 N10 C88 116.6(3) . . ? C90 N10 C88 111.6(3) . . ? C58 N10 C89 108.6(3) . . ? C90 N10 C89 105.0(3) . . ? C88 N10 C89 109.3(3) . . ? C91 N11 C92 124.5(3) . . ? C91 N11 C93 116.7(3) . . ? C92 N11 C93 117.8(3) . . ? H1X O1W H1Y 107.6 . . ? H2X O2W H2Y 108.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 106.3 . . ? H5X O5W H5Y 108.4 . . ? H6X O6W H6Y 109.4 . . ? H7X O7W H7Y 110.0 . . ? H8X O8W H8Y 105.3 . . ? H9X O9W H9Y 110.1 . . ? H10X O10W H10Y 112.8 . . ? H11X O11W H11Y 107.7 . . ? H12X O12W H12Y 109.6 . . ? H13X O13W H13Y 109.5 . . ? C1 S1 Zn2 104.53(14) . . ? C1 S1 Zn1 110.95(14) . . ? Zn2 S1 Zn1 118.07(4) . . ? C7 S2 Zn3 108.67(15) . . ? C7 S2 Zn1 96.80(15) . . ? Zn3 S2 Zn1 108.05(4) . . ? C13 S3 Zn2 99.57(14) . . ? C13 S3 Zn3 104.88(15) . . ? Zn2 S3 Zn3 114.25(4) . . ? C19 S4 Zn4 105.38(19) . . ? C19 S4 Zn3 107.59(19) . . ? Zn4 S4 Zn3 112.94(4) . . ? C25 S5 Zn4 100.76(14) . . ? C25 S5 Zn1 106.54(15) . . ? Zn4 S5 Zn1 113.53(4) . . ? C31 S6 Zn2 114.23(18) . . ? C31 S6 Zn4 100.76(17) . . ? Zn2 S6 Zn4 110.66(4) . . ? C37 S7 Zn1 106.23(15) . . ? C43 S8 Zn2 100.13(16) . . ? C49 S9 Zn3 105.89(15) . . ? C55 S10 Zn4 105.66(16) . . ? S7 Zn1 S2 108.08(4) . . ? S7 Zn1 S5 112.72(3) . . ? S2 Zn1 S5 104.07(4) . . ? S7 Zn1 S1 115.99(4) . . ? S2 Zn1 S1 108.66(3) . . ? S5 Zn1 S1 106.62(4) . . ? S3 Zn2 S1 101.70(4) . . ? S3 Zn2 S6 104.07(3) . . ? S1 Zn2 S6 109.37(3) . . ? S3 Zn2 S8 115.74(3) . . ? S1 Zn2 S8 101.72(4) . . ? S6 Zn2 S8 122.29(4) . . ? S9 Zn3 S2 99.18(4) . . ? S9 Zn3 S4 116.56(4) . . ? S2 Zn3 S4 90.41(3) . . ? S9 Zn3 S3 118.37(3) . . ? S2 Zn3 S3 128.33(4) . . ? S4 Zn3 S3 101.56(3) . . ? S10 Zn4 S5 117.14(4) . . ? S10 Zn4 S4 105.13(4) . . ? S5 Zn4 S4 104.45(4) . . ? S10 Zn4 S6 113.45(4) . . ? S5 Zn4 S6 97.61(3) . . ? S4 Zn4 S6 119.23(3) . . ? 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 C6 C1 C2 C3 3.1(7) . . . . ? S1 C1 C2 C3 -178.1(4) . . . . ? C1 C2 C3 C4 -9.5(8) . . . . ? C2 C3 C4 C5 11.0(8) . . . . ? C2 C3 C4 N1 -177.8(4) . . . . ? C3 C4 C5 C6 -5.4(8) . . . . ? N1 C4 C5 C6 -177.0(4) . . . . ? C4 C5 C6 C1 -1.1(8) . . . . ? C2 C1 C6 C5 2.2(8) . . . . ? S1 C1 C6 C5 -176.6(4) . . . . ? C12 C7 C8 C9 -1.7(7) . . . . ? S2 C7 C8 C9 177.3(4) . . . . ? C7 C8 C9 C10 2.0(8) . . . . ? C8 C9 C10 C11 -2.9(8) . . . . ? C8 C9 C10 N2 -176.9(4) . . . . ? C9 C10 C11 C12 3.6(8) . . . . ? N2 C10 C11 C12 177.4(4) . . . . ? C10 C11 C12 C7 -3.4(8) . . . . ? C8 C7 C12 C11 2.4(7) . . . . ? S2 C7 C12 C11 -176.6(4) . . . . ? C18 C13 C14 C15 -1.1(7) . . . . ? S3 C13 C14 C15 -175.9(4) . . . . ? C13 C14 C15 C16 1.0(8) . . . . ? C14 C15 C16 C17 -0.8(8) . . . . ? C14 C15 C16 N3 175.2(4) . . . . ? C15 C16 C17 C18 0.7(8) . . . . ? N3 C16 C17 C18 -175.5(4) . . . . ? C14 C13 C18 C17 1.0(8) . . . . ? S3 C13 C18 C17 175.1(4) . . . . ? C16 C17 C18 C13 -0.8(8) . . . . ? C24 C19 C20 C21 0.0(9) . . . . ? S4 C19 C20 C21 -174.9(5) . . . . ? C19 C20 C21 C22 0.4(9) . . . . ? C20 C21 C22 N4 179.0(5) . . . . ? C20 C21 C22 C23 -0.2(9) . . . . ? N4 C22 C23 C24 -179.7(5) . . . . ? C21 C22 C23 C24 -0.5(9) . . . . ? C22 C23 C24 C19 0.9(8) . . . . ? C20 C19 C24 C23 -0.7(8) . . . . ? S4 C19 C24 C23 174.9(4) . . . . ? C30 C25 C26 C27 0.4(8) . . . . ? S5 C25 C26 C27 178.9(4) . . . . ? C25 C26 C27 C28 -1.2(9) . . . . ? C26 C27 C28 C29 1.3(8) . . . . ? C26 C27 C28 N5 -175.6(5) . . . . ? C27 C28 C29 C30 -0.6(7) . . . . ? N5 C28 C29 C30 176.4(4) . . . . ? C26 C25 C30 C29 0.2(7) . . . . ? S5 C25 C30 C29 -178.3(4) . . . . ? C28 C29 C30 C25 -0.2(8) . . . . ? C36 C31 C32 C33 -0.8(8) . . . . ? S6 C31 C32 C33 -179.6(4) . . . . ? C31 C32 C33 C34 -2.1(8) . . . . ? C32 C33 C34 C35 3.3(9) . . . . ? C32 C33 C34 N6 -177.7(4) . . . . ? C33 C34 C35 C36 -1.5(9) . . . . ? N6 C34 C35 C36 179.7(5) . . . . ? C32 C31 C36 C35 2.6(8) . . . . ? S6 C31 C36 C35 -178.6(4) . . . . ? C34 C35 C36 C31 -1.4(8) . . . . ? C42 C37 C38 C39 -0.9(9) . . . . ? S7 C37 C38 C39 -175.4(5) . . . . ? C37 C38 C39 C40 0.2(9) . . . . ? C38 C39 C40 C41 -2.1(9) . . . . ? C38 C39 C40 N7 -176.0(5) . . . . ? C39 C40 C41 C42 4.6(9) . . . . ? N7 C40 C41 C42 178.1(5) . . . . ? C38 C37 C42 C41 3.6(9) . . . . ? S7 C37 C42 C41 178.7(5) . . . . ? C40 C41 C42 C37 -5.5(9) . . . . ? C48 C43 C44 C45 -2.7(9) . . . . ? S8 C43 C44 C45 169.7(5) . . . . ? C43 C44 C45 C46 3.1(9) . . . . ? C44 C45 C46 N8 -177.9(5) . . . . ? C44 C45 C46 C47 -2.8(9) . . . . ? N8 C46 C47 C48 177.5(4) . . . . ? C45 C46 C47 C48 2.3(8) . . . . ? C46 C47 C48 C43 -1.8(8) . . . . ? C44 C43 C48 C47 2.0(8) . . . . ? S8 C43 C48 C47 -170.4(4) . . . . ? C54 C49 C50 C51 -0.6(8) . . . . ? S9 C49 C50 C51 179.1(4) . . . . ? C49 C50 C51 C52 0.1(8) . . . . ? C50 C51 C52 C53 0.9(8) . . . . ? C50 C51 C52 N9 177.6(4) . . . . ? C51 C52 C53 C54 -1.4(8) . . . . ? N9 C52 C53 C54 -178.2(4) . . . . ? C52 C53 C54 C49 0.9(8) . . . . ? C50 C49 C54 C53 0.1(8) . . . . ? S9 C49 C54 C53 -179.6(4) . . . . ? C60 C55 C56 C57 -6.2(8) . . . . ? S10 C55 C56 C57 -179.5(4) . . . . ? C55 C56 C57 C58 3.2(8) . . . . ? C56 C57 C58 C59 -0.2(8) . . . . ? C56 C57 C58 N10 178.6(4) . . . . ? C57 C58 C59 C60 0.1(9) . . . . ? N10 C58 C59 C60 -178.6(5) . . . . ? C58 C59 C60 C55 -2.9(9) . . . . ? C56 C55 C60 C59 6.1(9) . . . . ? S10 C55 C60 C59 179.9(5) . . . . ? C5 C4 N1 C61 -160.1(4) . . . . ? C3 C4 N1 C61 28.2(5) . . . . ? C5 C4 N1 C63 72.1(5) . . . . ? C3 C4 N1 C63 -99.5(5) . . . . ? C5 C4 N1 C62 -42.5(5) . . . . ? C3 C4 N1 C62 145.9(4) . . . . ? C11 C10 N2 C65 73.7(5) . . . . ? C9 C10 N2 C65 -112.5(5) . . . . ? C11 C10 N2 C64 -43.0(6) . . . . ? C9 C10 N2 C64 130.8(4) . . . . ? C11 C10 N2 C66 -159.6(4) . . . . ? C9 C10 N2 C66 14.2(6) . . . . ? C15 C16 N3 C68 -2.4(5) . . . . ? C17 C16 N3 C68 173.7(4) . . . . ? C15 C16 N3 C67 -140.1(4) . . . . ? C17 C16 N3 C67 36.1(5) . . . . ? C15 C16 N3 C69 115.5(4) . . . . ? C17 C16 N3 C69 -68.4(5) . . . . ? C21 C22 N4 C71 136.1(5) . . . . ? C23 C22 N4 C71 -44.7(6) . . . . ? C21 C22 N4 C70 -104.9(5) . . . . ? C23 C22 N4 C70 74.3(5) . . . . ? C21 C22 N4 C72 18.9(6) . . . . ? C23 C22 N4 C72 -161.9(4) . . . . ? C27 C28 N5 C73 116.3(5) . . . . ? C29 C28 N5 C73 -60.4(5) . . . . ? C27 C28 N5 C74 -120.0(5) . . . . ? C29 C28 N5 C74 63.2(5) . . . . ? C27 C28 N5 C75 2.9(6) . . . . ? C29 C28 N5 C75 -173.8(4) . . . . ? C35 C34 N6 C77 -17.9(7) . . . . ? C33 C34 N6 C77 163.2(4) . . . . ? C35 C34 N6 C76 94.2(6) . . . . ? C33 C34 N6 C76 -84.7(5) . . . . ? C35 C34 N6 C78 -121.7(6) . . . . ? C33 C34 N6 C78 59.4(5) . . . . ? C41 C40 N7 C81 17.2(6) . . . . ? C39 C40 N7 C81 -169.1(5) . . . . ? C41 C40 N7 C80 127.7(5) . . . . ? C39 C40 N7 C80 -58.5(6) . . . . ? C41 C40 N7 C79 -105.0(5) . . . . ? C39 C40 N7 C79 68.7(6) . . . . ? C45 C46 N8 C83 132.3(5) . . . . ? C47 C46 N8 C83 -43.0(6) . . . . ? C45 C46 N8 C82 -102.3(6) . . . . ? C47 C46 N8 C82 82.4(5) . . . . ? C45 C46 N8 C84 16.3(6) . . . . ? C47 C46 N8 C84 -159.0(4) . . . . ? C53 C52 N9 C85 145.7(5) . . . . ? C51 C52 N9 C85 -30.9(6) . . . . ? C53 C52 N9 C86 -90.3(5) . . . . ? C51 C52 N9 C86 93.0(5) . . . . ? C53 C52 N9 C87 33.7(5) . . . . ? C51 C52 N9 C87 -143.0(5) . . . . ? C57 C58 N10 C90 -75.4(5) . . . . ? C59 C58 N10 C90 103.4(6) . . . . ? C57 C58 N10 C88 48.8(6) . . . . ? C59 C58 N10 C88 -132.4(5) . . . . ? C57 C58 N10 C89 172.7(4) . . . . ? C59 C58 N10 C89 -8.6(6) . . . . ? O1 C91 N11 C92 4.2(6) . . . . ? O1 C91 N11 C93 173.3(3) . . . . ? C2 C1 S1 Zn2 81.9(4) . . . . ? C6 C1 S1 Zn2 -99.3(4) . . . . ? C2 C1 S1 Zn1 -46.4(4) . . . . ? C6 C1 S1 Zn1 132.4(4) . . . . ? C12 C7 S2 Zn3 -153.8(4) . . . . ? C8 C7 S2 Zn3 27.2(4) . . . . ? C12 C7 S2 Zn1 94.5(4) . . . . ? C8 C7 S2 Zn1 -84.5(4) . . . . ? C18 C13 S3 Zn2 47.7(5) . . . . ? C14 C13 S3 Zn2 -137.9(3) . . . . ? C18 C13 S3 Zn3 -70.7(4) . . . . ? C14 C13 S3 Zn3 103.7(3) . . . . ? C20 C19 S4 Zn4 2.1(6) . . . . ? C24 C19 S4 Zn4 -173.1(4) . . . . ? C20 C19 S4 Zn3 -118.6(5) . . . . ? C24 C19 S4 Zn3 66.1(4) . . . . ? C30 C25 S5 Zn4 -60.7(4) . . . . ? C26 C25 S5 Zn4 120.9(4) . . . . ? C30 C25 S5 Zn1 -179.4(4) . . . . ? C26 C25 S5 Zn1 2.2(5) . . . . ? C36 C31 S6 Zn2 12.8(5) . . . . ? C32 C31 S6 Zn2 -168.4(4) . . . . ? C36 C31 S6 Zn4 -105.8(4) . . . . ? C32 C31 S6 Zn4 73.0(5) . . . . ? C42 C37 S7 Zn1 155.1(4) . . . . ? C38 C37 S7 Zn1 -30.4(5) . . . . ? C44 C43 S8 Zn2 63.7(4) . . . . ? C48 C43 S8 Zn2 -124.0(4) . . . . ? C50 C49 S9 Zn3 166.4(4) . . . . ? C54 C49 S9 Zn3 -13.8(5) . . . . ? C56 C55 S10 Zn4 -9.0(5) . . . . ? C60 C55 S10 Zn4 177.3(4) . . . . ? C37 S7 Zn1 S2 103.18(18) . . . . ? C37 S7 Zn1 S5 -142.36(18) . . . . ? C37 S7 Zn1 S1 -19.06(18) . . . . ? C7 S2 Zn1 S7 -53.82(16) . . . . ? Zn3 S2 Zn1 S7 -166.03(4) . . . . ? C7 S2 Zn1 S5 -173.87(16) . . . . ? Zn3 S2 Zn1 S5 73.93(4) . . . . ? C7 S2 Zn1 S1 72.81(16) . . . . ? Zn3 S2 Zn1 S1 -39.39(5) . . . . ? C25 S5 Zn1 S7 -60.21(15) . . . . ? Zn4 S5 Zn1 S7 -170.20(4) . . . . ? C25 S5 Zn1 S2 56.65(15) . . . . ? Zn4 S5 Zn1 S2 -53.34(5) . . . . ? C25 S5 Zn1 S1 171.42(15) . . . . ? Zn4 S5 Zn1 S1 61.43(5) . . . . ? C1 S1 Zn1 S7 -47.82(16) . . . . ? Zn2 S1 Zn1 S7 -168.38(4) . . . . ? C1 S1 Zn1 S2 -169.75(16) . . . . ? Zn2 S1 Zn1 S2 69.69(5) . . . . ? C1 S1 Zn1 S5 78.62(16) . . . . ? Zn2 S1 Zn1 S5 -41.94(5) . . . . ? C13 S3 Zn2 S1 -71.13(15) . . . . ? Zn3 S3 Zn2 S1 40.07(5) . . . . ? C13 S3 Zn2 S6 175.22(15) . . . . ? Zn3 S3 Zn2 S6 -73.59(5) . . . . ? C13 S3 Zn2 S8 38.15(15) . . . . ? Zn3 S3 Zn2 S8 149.34(4) . . . . ? C1 S1 Zn2 S3 169.48(15) . . . . ? Zn1 S1 Zn2 S3 -66.69(5) . . . . ? C1 S1 Zn2 S6 -80.89(15) . . . . ? Zn1 S1 Zn2 S6 42.94(5) . . . . ? C1 S1 Zn2 S8 49.75(15) . . . . ? Zn1 S1 Zn2 S8 173.58(4) . . . . ? C31 S6 Zn2 S3 -62.4(2) . . . . ? Zn4 S6 Zn2 S3 50.50(4) . . . . ? C31 S6 Zn2 S1 -170.4(2) . . . . ? Zn4 S6 Zn2 S1 -57.54(4) . . . . ? C31 S6 Zn2 S8 71.1(2) . . . . ? Zn4 S6 Zn2 S8 -176.02(3) . . . . ? C43 S8 Zn2 S3 26.59(18) . . . . ? C43 S8 Zn2 S1 135.86(18) . . . . ? C43 S8 Zn2 S6 -102.01(18) . . . . ? C49 S9 Zn3 S2 61.83(18) . . . . ? C49 S9 Zn3 S4 -33.27(18) . . . . ? C49 S9 Zn3 S3 -154.91(18) . . . . ? C7 S2 Zn3 S9 59.01(17) . . . . ? Zn1 S2 Zn3 S9 162.99(4) . . . . ? C7 S2 Zn3 S4 176.02(17) . . . . ? Zn1 S2 Zn3 S4 -80.00(4) . . . . ? C7 S2 Zn3 S3 -78.84(17) . . . . ? Zn1 S2 Zn3 S3 25.14(6) . . . . ? C19 S4 Zn3 S9 -65.4(2) . . . . ? Zn4 S4 Zn3 S9 178.69(4) . . . . ? C19 S4 Zn3 S2 -165.9(2) . . . . ? Zn4 S4 Zn3 S2 78.21(4) . . . . ? C19 S4 Zn3 S3 64.7(2) . . . . ? Zn4 S4 Zn3 S3 -51.18(4) . . . . ? C13 S3 Zn3 S9 -50.48(15) . . . . ? Zn2 S3 Zn3 S9 -158.44(4) . . . . ? C13 S3 Zn3 S2 80.69(15) . . . . ? Zn2 S3 Zn3 S2 -27.28(6) . . . . ? C13 S3 Zn3 S4 -179.47(15) . . . . ? Zn2 S3 Zn3 S4 72.57(4) . . . . ? C55 S10 Zn4 S5 55.6(2) . . . . ? C55 S10 Zn4 S4 171.0(2) . . . . ? C55 S10 Zn4 S6 -57.0(2) . . . . ? C25 S5 Zn4 S10 51.51(15) . . . . ? Zn1 S5 Zn4 S10 165.02(4) . . . . ? C25 S5 Zn4 S4 -64.28(15) . . . . ? Zn1 S5 Zn4 S4 49.23(5) . . . . ? C25 S5 Zn4 S6 172.82(15) . . . . ? Zn1 S5 Zn4 S6 -73.67(5) . . . . ? C19 S4 Zn4 S10 53.4(2) . . . . ? Zn3 S4 Zn4 S10 170.62(4) . . . . ? C19 S4 Zn4 S5 177.3(2) . . . . ? Zn3 S4 Zn4 S5 -65.49(4) . . . . ? C19 S4 Zn4 S6 -75.2(2) . . . . ? Zn3 S4 Zn4 S6 42.03(5) . . . . ? C31 S6 Zn4 S10 -44.11(19) . . . . ? Zn2 S6 Zn4 S10 -165.32(4) . . . . ? C31 S6 Zn4 S5 -168.15(19) . . . . ? Zn2 S6 Zn4 S5 70.65(4) . . . . ? C31 S6 Zn4 S4 80.56(19) . . . . ? Zn2 S6 Zn4 S4 -40.65(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.716 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.091 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 865706' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C90 H130 Cd4 N10 S10, C3 H7 N O, 8(F6 P), 0.5(H1.20 O0.60), 4.7(H2 O) ; _chemical_formula_sum 'C93 H147 Cd4 F48 N11 O6 P8 S10' _chemical_formula_weight 3445.32 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.6626(19) _cell_length_b 21.1266(12) _cell_length_c 21.6391(13) _cell_angle_alpha 105.636(3) _cell_angle_beta 92.555(3) _cell_angle_gamma 114.528(2) _cell_volume 7748.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3755 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 23.55 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3468 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.8332 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Corp.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _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 65464 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 30451 _reflns_number_gt 24782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^+1.99P] 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 30451 _refine_ls_number_parameters 1749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.600499(13) 0.417683(12) 0.830198(11) 0.03021(5) Uani 1 1 d . . . Cd2 Cd 0.578242(13) 0.473812(12) 0.652923(11) 0.03056(5) Uani 1 1 d . . . Cd3 Cd 0.747297(13) 0.414230(12) 0.692158(11) 0.03034(5) Uani 1 1 d . . . Cd4 Cd 0.511829(12) 0.254962(12) 0.646816(11) 0.02850(5) Uani 1 1 d . . . S1 S 0.59753(4) 0.50914(4) 0.77756(4) 0.03030(16) Uani 1 1 d . . . S2 S 0.72302(4) 0.41010(4) 0.80608(4) 0.02984(16) Uani 1 1 d . . . S3 S 0.70069(4) 0.47109(4) 0.62181(4) 0.03064(16) Uani 1 1 d . . . S4 S 0.64845(4) 0.27820(4) 0.64702(4) 0.02934(15) Uani 1 1 d . . . S5 S 0.49390(4) 0.29215(4) 0.76537(4) 0.02674(15) Uani 1 1 d . . . S6 S 0.47457(4) 0.34247(4) 0.60810(4) 0.02858(15) Uani 1 1 d . . . S7 S 0.59396(4) 0.44403(4) 0.94653(4) 0.03038(16) Uani 1 1 d . . . S8 S 0.56489(5) 0.57812(4) 0.63555(4) 0.03176(16) Uani 1 1 d . . . S9 S 0.88279(4) 0.44472(4) 0.69738(4) 0.02912(15) Uani 1 1 d . . . S10 S 0.43297(4) 0.12464(4) 0.58431(4) 0.02774(15) Uani 1 1 d . . . C1 C 0.52244(19) 0.52824(18) 0.80372(15) 0.0337(7) Uani 1 1 d . . . C2 C 0.45187(19) 0.47295(19) 0.80346(16) 0.0347(7) Uani 1 1 d . . . H2 H 0.4428 0.4241 0.7887 0.042 Uiso 1 1 calc R . . C3 C 0.39361(19) 0.49173(18) 0.82597(15) 0.0336(7) Uani 1 1 d . . . H3 H 0.3454 0.4552 0.8238 0.040 Uiso 1 1 calc R . . C4 C 0.4093(2) 0.5634(2) 0.85060(17) 0.0414(8) Uani 1 1 d . . . C5 C 0.48047(19) 0.6210(2) 0.85166(17) 0.0414(8) Uani 1 1 d . . . H5 H 0.4897 0.6699 0.8677 0.050 Uiso 1 1 calc R . . C6 C 0.5372(2) 0.60129(19) 0.82725(18) 0.0423(8) Uani 1 1 d . . . H6 H 0.5845 0.6377 0.8271 0.051 Uiso 1 1 calc R . . C7 C 0.7866(2) 0.49489(19) 0.86017(17) 0.0393(8) Uani 1 1 d . . . C8 C 0.8140(2) 0.55786(19) 0.83993(16) 0.0412(8) Uani 1 1 d . . . H8 H 0.8005 0.5536 0.7967 0.049 Uiso 1 1 calc R . . C9 C 0.8578(2) 0.6216(2) 0.88141(19) 0.0450(8) Uani 1 1 d . . . H9 H 0.8745 0.6627 0.8675 0.054 Uiso 1 1 calc R . . C10 C 0.8815(2) 0.6306(2) 0.94853(18) 0.0458(9) Uani 1 1 d . . . C11 C 0.8556(2) 0.5702(2) 0.96957(19) 0.0471(9) Uani 1 1 d . . . H11 H 0.8698 0.5747 1.0127 0.057 Uiso 1 1 calc R . . C12 C 0.8077(2) 0.50192(19) 0.92485(17) 0.0411(8) Uani 1 1 d . . . H12 H 0.7897 0.4605 0.9384 0.049 Uiso 1 1 calc R . . C13 C 0.7664(2) 0.5623(2) 0.64675(18) 0.0418(8) Uani 1 1 d . . . C14 C 0.81761(17) 0.5842(2) 0.60512(18) 0.0384(8) Uani 1 1 d . . . H14 H 0.8132 0.5513 0.5649 0.046 Uiso 1 1 calc R . . C15 C 0.8750(2) 0.6555(2) 0.62438(19) 0.0512(10) Uani 1 1 d . . . H15 H 0.9103 0.6695 0.5975 0.061 Uiso 1 1 calc R . . C16 C 0.88084(19) 0.70614(19) 0.68297(18) 0.0395(8) Uani 1 1 d . . . C17 C 0.8311(2) 0.6841(2) 0.72324(19) 0.0475(9) Uani 1 1 d . . . H17 H 0.8362 0.7174 0.7634 0.057 Uiso 1 1 calc R . . C18 C 0.77170(19) 0.6116(2) 0.70568(18) 0.0415(8) Uani 1 1 d . . . H18 H 0.7372 0.5978 0.7332 0.050 Uiso 1 1 calc R . . C19 C 0.6615(2) 0.2491(2) 0.56609(18) 0.0432(8) Uani 1 1 d . . . C20 C 0.6068(2) 0.22081(18) 0.51035(16) 0.0386(8) Uani 1 1 d . . . H20 H 0.5593 0.2194 0.5137 0.046 Uiso 1 1 calc R . . C21 C 0.6231(2) 0.1946(2) 0.44958(17) 0.0408(8) Uani 1 1 d . . . H21 H 0.5865 0.1757 0.4123 0.049 Uiso 1 1 calc R . . C22 C 0.6942(2) 0.1967(2) 0.44455(17) 0.0427(8) Uani 1 1 d . . . C23 C 0.7490(2) 0.2250(2) 0.50029(17) 0.0446(9) Uani 1 1 d . . . H23 H 0.7965 0.2263 0.4969 0.054 Uiso 1 1 calc R . . C24 C 0.7326(2) 0.2512(2) 0.5611(2) 0.0489(9) Uani 1 1 d . . . H24 H 0.7692 0.2701 0.5984 0.059 Uiso 1 1 calc R . . C25 C 0.50791(19) 0.22594(17) 0.79422(17) 0.0345(7) Uani 1 1 d . . . C26 C 0.56580(19) 0.2474(2) 0.84606(19) 0.0426(8) Uani 1 1 d . . . H26 H 0.6002 0.2965 0.8649 0.051 Uiso 1 1 calc R . . C27 C 0.5711(2) 0.1940(2) 0.86890(19) 0.0469(9) Uani 1 1 d . . . H27 H 0.6097 0.2077 0.9033 0.056 Uiso 1 1 calc R . . C28 C 0.5202(2) 0.1208(2) 0.84153(16) 0.0404(8) Uani 1 1 d . . . C29 C 0.4614(2) 0.10077(19) 0.78972(16) 0.0376(7) Uani 1 1 d . . . H29 H 0.4264 0.0519 0.7707 0.045 Uiso 1 1 calc R . . C30 C 0.4565(2) 0.15282(17) 0.76821(14) 0.0354(7) Uani 1 1 d . . . H30 H 0.4172 0.1392 0.7346 0.042 Uiso 1 1 calc R . . C31 C 0.46831(18) 0.3084(2) 0.52290(17) 0.0399(8) Uani 1 1 d . . . C32 C 0.40732(18) 0.24280(17) 0.48610(16) 0.0341(7) Uani 1 1 d . . . H32 H 0.3700 0.2163 0.5064 0.041 Uiso 1 1 calc R . . C33 C 0.40205(19) 0.21689(18) 0.41895(16) 0.0341(7) Uani 1 1 d . . . H33 H 0.3612 0.1730 0.3943 0.041 Uiso 1 1 calc R . . C34 C 0.4578(2) 0.2565(2) 0.38861(18) 0.0432(8) Uani 1 1 d . . . C35 C 0.5188(2) 0.32210(19) 0.42541(18) 0.0416(8) Uani 1 1 d . . . H35 H 0.5561 0.3486 0.4051 0.050 Uiso 1 1 calc R . . C36 C 0.52404(19) 0.34801(18) 0.49255(17) 0.0379(8) Uani 1 1 d . . . H36 H 0.5649 0.3919 0.5172 0.046 Uiso 1 1 calc R . . C37 C 0.62041(19) 0.53971(19) 0.97816(17) 0.0373(7) Uani 1 1 d . . . C38 C 0.6689(2) 0.5934(2) 0.95485(17) 0.0401(8) Uani 1 1 d . . . H38 H 0.6886 0.5805 0.9178 0.048 Uiso 1 1 calc R . . C39 C 0.6876(2) 0.6642(2) 0.98559(18) 0.0451(9) Uani 1 1 d . . . H39 H 0.7207 0.6991 0.9688 0.054 Uiso 1 1 calc R . . C40 C 0.6610(2) 0.6883(2) 1.04030(17) 0.0414(8) Uani 1 1 d . . . C41 C 0.6109(2) 0.6338(2) 1.06518(17) 0.0385(8) Uani 1 1 d . . . H41 H 0.5905 0.6468 1.1017 0.046 Uiso 1 1 calc R . . C42 C 0.59278(19) 0.56016(18) 1.03374(16) 0.0358(7) Uani 1 1 d . . . H42 H 0.5616 0.5244 1.0506 0.043 Uiso 1 1 calc R . . C43 C 0.62299(19) 0.59703(19) 0.57416(17) 0.0358(7) Uani 1 1 d . . . C44 C 0.5997(2) 0.5434(2) 0.51479(19) 0.0483(9) Uani 1 1 d . . . H44 H 0.5594 0.4978 0.5092 0.058 Uiso 1 1 calc R . . C45 C 0.6366(2) 0.5572(2) 0.4622(2) 0.0492(10) Uani 1 1 d . . . H45 H 0.6218 0.5210 0.4219 0.059 Uiso 1 1 calc R . . C46 C 0.6964(2) 0.6273(2) 0.47257(17) 0.0415(8) Uani 1 1 d . . . C47 C 0.7191(2) 0.68091(19) 0.53360(18) 0.0411(8) Uani 1 1 d . . . H47 H 0.7598 0.7267 0.5408 0.049 Uiso 1 1 calc R . . C48 C 0.67911(19) 0.6642(2) 0.58449(17) 0.0384(8) Uani 1 1 d . . . H48 H 0.6918 0.6999 0.6249 0.046 Uiso 1 1 calc R . . C49 C 0.88490(19) 0.37288(17) 0.71630(19) 0.0388(8) Uani 1 1 d . . . C50 C 0.9210(2) 0.3378(2) 0.6769(2) 0.0487(9) Uani 1 1 d . . . H50 H 0.9416 0.3543 0.6431 0.058 Uiso 1 1 calc R . . C51 C 0.9263(3) 0.2780(2) 0.6879(2) 0.0535(10) Uani 1 1 d . . . H51 H 0.9505 0.2545 0.6615 0.064 Uiso 1 1 calc R . . C52 C 0.8956(3) 0.2533(2) 0.7383(2) 0.0546(10) Uani 1 1 d . . . C53 C 0.8594(3) 0.2885(2) 0.7777(2) 0.0562(11) Uani 1 1 d . . . H53 H 0.8389 0.2720 0.8115 0.067 Uiso 1 1 calc R . . C54 C 0.8541(2) 0.3482(2) 0.76673(19) 0.0493(9) Uani 1 1 d . . . H54 H 0.8300 0.3717 0.7931 0.059 Uiso 1 1 calc R . . C55 C 0.33779(19) 0.10344(18) 0.59427(19) 0.0394(8) Uani 1 1 d . . . C56 C 0.3181(2) 0.15163(19) 0.63735(17) 0.0391(8) Uani 1 1 d . . . H56 H 0.3556 0.1976 0.6622 0.047 Uiso 1 1 calc R . . C57 C 0.24188(19) 0.13191(19) 0.64398(16) 0.0364(7) Uani 1 1 d . . . H57 H 0.2285 0.1650 0.6721 0.044 Uiso 1 1 calc R . . C58 C 0.1862(2) 0.06146(19) 0.60754(17) 0.0385(7) Uani 1 1 d . . . C59 C 0.20733(19) 0.0116(2) 0.56442(17) 0.0384(8) Uani 1 1 d . . . H59 H 0.1711 -0.0353 0.5404 0.046 Uiso 1 1 calc R . . C60 C 0.28291(19) 0.0347(2) 0.55909(16) 0.0407(8) Uani 1 1 d . . . H60 H 0.2971 0.0026 0.5307 0.049 Uiso 1 1 calc R . . C61 C 0.2882(2) 0.5240(2) 0.89549(18) 0.0419(8) Uani 1 1 d . . . H61A H 0.2619 0.5439 0.9252 0.063 Uiso 1 1 calc R . . H61B H 0.3114 0.5011 0.9159 0.063 Uiso 1 1 calc R . . H61C H 0.2528 0.4884 0.8569 0.063 Uiso 1 1 calc R . . C62 C 0.3890(2) 0.65251(19) 0.93800(18) 0.0435(8) Uani 1 1 d . . . H62A H 0.4160 0.6950 0.9250 0.065 Uiso 1 1 calc R . . H62B H 0.4241 0.6452 0.9641 0.065 Uiso 1 1 calc R . . H62C H 0.3520 0.6595 0.9629 0.065 Uiso 1 1 calc R . . C63 C 0.3172(2) 0.6102(2) 0.82865(19) 0.0467(9) Uani 1 1 d . . . H63A H 0.3432 0.6088 0.7922 0.070 Uiso 1 1 calc R . . H63B H 0.3245 0.6595 0.8492 0.070 Uiso 1 1 calc R . . H63C H 0.2639 0.5784 0.8138 0.070 Uiso 1 1 calc R . . C64 C 0.8959(2) 0.7117(2) 1.06028(17) 0.0429(8) Uani 1 1 d . . . H64A H 0.9249 0.7595 1.0914 0.064 Uiso 1 1 calc R . . H64B H 0.8968 0.6752 1.0785 0.064 Uiso 1 1 calc R . . H64C H 0.8444 0.7035 1.0499 0.064 Uiso 1 1 calc R . . C65 C 1.0098(2) 0.7131(2) 1.00848(18) 0.0449(8) Uani 1 1 d . . . H65A H 1.0105 0.6816 1.0330 0.067 Uiso 1 1 calc R . . H65B H 1.0442 0.7630 1.0327 0.067 Uiso 1 1 calc R . . H65C H 1.0251 0.6991 0.9675 0.067 Uiso 1 1 calc R . . C66 C 0.9309(2) 0.7663(2) 0.96937(18) 0.0469(9) Uani 1 1 d . . . H66A H 0.9542 0.7650 0.9313 0.070 Uiso 1 1 calc R . . H66B H 0.9586 0.8135 1.0019 0.070 Uiso 1 1 calc R . . H66C H 0.8794 0.7579 0.9580 0.070 Uiso 1 1 calc R . . C67 C 0.9768(2) 0.8078(2) 0.77332(18) 0.0461(9) Uani 1 1 d . . . H67A H 1.0002 0.7789 0.7831 0.069 Uiso 1 1 calc R . . H67B H 0.9358 0.8034 0.7969 0.069 Uiso 1 1 calc R . . H67C H 1.0137 0.8583 0.7859 0.069 Uiso 1 1 calc R . . C68 C 1.0016(2) 0.7958(2) 0.6581(2) 0.0501(9) Uani 1 1 d . . . H68A H 0.9752 0.7726 0.6137 0.075 Uiso 1 1 calc R . . H68B H 1.0368 0.7767 0.6652 0.075 Uiso 1 1 calc R . . H68C H 1.0287 0.8478 0.6664 0.075 Uiso 1 1 calc R . . C69 C 0.9089(2) 0.8287(2) 0.70688(19) 0.0451(8) Uani 1 1 d . . . H69A H 0.8713 0.8171 0.7342 0.068 Uiso 1 1 calc R . . H69B H 0.8848 0.8211 0.6642 0.068 Uiso 1 1 calc R . . H69C H 0.9457 0.8791 0.7255 0.068 Uiso 1 1 calc R . . C70 C 0.7035(2) 0.0929(2) 0.37466(19) 0.0467(9) Uani 1 1 d . . . H70A H 0.7438 0.0981 0.4054 0.070 Uiso 1 1 calc R . . H70B H 0.7075 0.0691 0.3314 0.070 Uiso 1 1 calc R . . H70C H 0.6554 0.0639 0.3844 0.070 Uiso 1 1 calc R . . C71 C 0.7905(2) 0.2186(2) 0.37199(19) 0.0503(9) Uani 1 1 d . . . H71A H 0.8164 0.2560 0.4131 0.075 Uiso 1 1 calc R . . H71B H 0.7865 0.2410 0.3397 0.075 Uiso 1 1 calc R . . H71C H 0.8185 0.1908 0.3588 0.075 Uiso 1 1 calc R . . C72 C 0.6565(2) 0.1613(2) 0.32332(18) 0.0509(9) Uani 1 1 d . . . H72A H 0.6581 0.2085 0.3286 0.076 Uiso 1 1 calc R . . H72B H 0.6057 0.1268 0.3230 0.076 Uiso 1 1 calc R . . H72C H 0.6718 0.1450 0.2829 0.076 Uiso 1 1 calc R . . C73 C 0.4509(2) 0.02721(19) 0.89364(16) 0.0389(8) Uani 1 1 d . . . H73A H 0.4094 -0.0041 0.8579 0.058 Uiso 1 1 calc R . . H73B H 0.4398 0.0647 0.9207 0.058 Uiso 1 1 calc R . . H73C H 0.4580 -0.0013 0.9189 0.058 Uiso 1 1 calc R . . C74 C 0.5362(2) 0.0092(2) 0.81619(19) 0.0507(9) Uani 1 1 d . . . H74A H 0.5391 0.0222 0.7768 0.076 Uiso 1 1 calc R . . H74B H 0.4947 -0.0385 0.8082 0.076 Uiso 1 1 calc R . . H74C H 0.5828 0.0085 0.8302 0.076 Uiso 1 1 calc R . . C75 C 0.5848(2) 0.0949(2) 0.9280(2) 0.0503(9) Uani 1 1 d . . . H75A H 0.5821 0.0562 0.9445 0.075 Uiso 1 1 calc R . . H75B H 0.5764 0.1306 0.9607 0.075 Uiso 1 1 calc R . . H75C H 0.6342 0.1179 0.9172 0.075 Uiso 1 1 calc R . . C76 C 0.4769(2) 0.1688(2) 0.3010(2) 0.0508(9) Uani 1 1 d . . . H76A H 0.5189 0.1846 0.3350 0.076 Uiso 1 1 calc R . . H76B H 0.4940 0.1659 0.2599 0.076 Uiso 1 1 calc R . . H76C H 0.4387 0.1214 0.2993 0.076 Uiso 1 1 calc R . . C77 C 0.4928(2) 0.2799(2) 0.28531(17) 0.0443(8) Uani 1 1 d . . . H77A H 0.4767 0.3180 0.2929 0.066 Uiso 1 1 calc R . . H77B H 0.4873 0.2578 0.2392 0.066 Uiso 1 1 calc R . . H77C H 0.5451 0.3005 0.3053 0.066 Uiso 1 1 calc R . . C78 C 0.3665(2) 0.2081(2) 0.28292(18) 0.0459(9) Uani 1 1 d . . . H78A H 0.3570 0.2495 0.3024 0.069 Uiso 1 1 calc R . . H78B H 0.3281 0.1651 0.2893 0.069 Uiso 1 1 calc R . . H78C H 0.3652 0.2009 0.2371 0.069 Uiso 1 1 calc R . . C79 C 0.6416(2) 0.79205(18) 1.02548(18) 0.0439(8) Uani 1 1 d . . . H79A H 0.6609 0.7880 0.9854 0.066 Uiso 1 1 calc R . . H79B H 0.6511 0.8420 1.0460 0.066 Uiso 1 1 calc R . . H79C H 0.5879 0.7609 1.0166 0.066 Uiso 1 1 calc R . . C80 C 0.7688(2) 0.8141(2) 1.08381(19) 0.0476(9) Uani 1 1 d . . . H80A H 0.7926 0.7836 1.0880 0.071 Uiso 1 1 calc R . . H80B H 0.7842 0.8545 1.1233 0.071 Uiso 1 1 calc R . . H80C H 0.7837 0.8324 1.0481 0.071 Uiso 1 1 calc R . . C81 C 0.6591(2) 0.78049(19) 1.13870(18) 0.0444(8) Uani 1 1 d . . . H81A H 0.6737 0.8317 1.1590 0.067 Uiso 1 1 calc R . . H81B H 0.6846 0.7640 1.1650 0.067 Uiso 1 1 calc R . . H81C H 0.6051 0.7532 1.1345 0.067 Uiso 1 1 calc R . . C82 C 0.81209(19) 0.6435(2) 0.43062(19) 0.0410(8) Uani 1 1 d . . . H82A H 0.8502 0.6899 0.4588 0.062 Uiso 1 1 calc R . . H82B H 0.8280 0.6315 0.3896 0.062 Uiso 1 1 calc R . . H82C H 0.8050 0.6062 0.4504 0.062 Uiso 1 1 calc R . . C83 C 0.7503(2) 0.72208(19) 0.41698(17) 0.0431(8) Uani 1 1 d . . . H83A H 0.7412 0.7486 0.4567 0.065 Uiso 1 1 calc R . . H83B H 0.7159 0.7163 0.3807 0.065 Uiso 1 1 calc R . . H83C H 0.8017 0.7488 0.4118 0.065 Uiso 1 1 calc R . . C84 C 0.6896(2) 0.5928(2) 0.35242(18) 0.0482(9) Uani 1 1 d . . . H84A H 0.7172 0.6044 0.3183 0.072 Uiso 1 1 calc R . . H84B H 0.6427 0.5961 0.3460 0.072 Uiso 1 1 calc R . . H84C H 0.6790 0.5439 0.3515 0.072 Uiso 1 1 calc R . . C85 C 0.9524(2) 0.1683(2) 0.71872(19) 0.0481(9) Uani 1 1 d . . . H85A H 1.0020 0.2092 0.7310 0.072 Uiso 1 1 calc R . . H85B H 0.9340 0.1563 0.6732 0.072 Uiso 1 1 calc R . . H85C H 0.9554 0.1268 0.7265 0.072 Uiso 1 1 calc R . . C86 C 0.9267(2) 0.2053(2) 0.82881(18) 0.0537(10) Uani 1 1 d . . . H86A H 0.8912 0.2162 0.8532 0.080 Uiso 1 1 calc R . . H86B H 0.9757 0.2471 0.8424 0.080 Uiso 1 1 calc R . . H86C H 0.9305 0.1640 0.8364 0.080 Uiso 1 1 calc R . . C87 C 0.8234(2) 0.1240(2) 0.73768(17) 0.0443(8) Uani 1 1 d . . . H87A H 0.8184 0.0940 0.6940 0.066 Uiso 1 1 calc R . . H87B H 0.7854 0.1415 0.7393 0.066 Uiso 1 1 calc R . . H87C H 0.8169 0.0956 0.7668 0.066 Uiso 1 1 calc R . . C88 C 0.0818(2) 0.0993(2) 0.6133(2) 0.0492(9) Uani 1 1 d . . . H88A H 0.0637 0.0911 0.5685 0.074 Uiso 1 1 calc R . . H88B H 0.1246 0.1467 0.6307 0.074 Uiso 1 1 calc R . . H88C H 0.0420 0.0971 0.6380 0.074 Uiso 1 1 calc R . . C89 C 0.0528(2) -0.03149(19) 0.56658(17) 0.0394(8) Uani 1 1 d . . . H89A H 0.0013 -0.0447 0.5729 0.059 Uiso 1 1 calc R . . H89B H 0.0670 -0.0685 0.5714 0.059 Uiso 1 1 calc R . . H89C H 0.0572 -0.0275 0.5236 0.059 Uiso 1 1 calc R . . C90 C 0.0955(2) 0.0303(2) 0.68429(17) 0.0460(9) Uani 1 1 d . . . H90A H 0.0474 -0.0105 0.6803 0.069 Uiso 1 1 calc R . . H90B H 0.0975 0.0737 0.7149 0.069 Uiso 1 1 calc R . . H90C H 0.1357 0.0205 0.6994 0.069 Uiso 1 1 calc R . . C91 C 0.52377(18) 0.00611(18) 0.63166(16) 0.0348(7) Uani 1 1 d . . . H91 H 0.4950 0.0310 0.6281 0.042 Uiso 1 1 calc R . . C92 C 0.6284(2) -0.0196(2) 0.59896(18) 0.0423(8) Uani 1 1 d . . . H92A H 0.6412 -0.0210 0.6417 0.063 Uiso 1 1 calc R . . H92B H 0.6740 0.0053 0.5836 0.063 Uiso 1 1 calc R . . H92C H 0.6006 -0.0688 0.5697 0.063 Uiso 1 1 calc R . . C93 C 0.59986(19) 0.06345(19) 0.55478(17) 0.0406(8) Uani 1 1 d . . . H93A H 0.5589 0.0758 0.5482 0.061 Uiso 1 1 calc R . . H93B H 0.6049 0.0355 0.5138 0.061 Uiso 1 1 calc R . . H93C H 0.6463 0.1076 0.5731 0.061 Uiso 1 1 calc R . . F1 F 0.79479(15) 0.97242(14) 0.62533(14) 0.0696(7) Uani 1 1 d . . . F2 F 0.76348(15) 0.88220(14) 0.53709(12) 0.0671(7) Uani 1 1 d . . . F3 F 0.86687(14) 0.86778(14) 0.56545(12) 0.0640(7) Uani 1 1 d . . . F4 F 0.90199(14) 0.96206(15) 0.65485(12) 0.0685(7) Uani 1 1 d . . . F5 F 0.87934(15) 0.97730(14) 0.55962(13) 0.0644(6) Uani 1 1 d . . . F6 F 0.78317(14) 0.86346(14) 0.63207(12) 0.0663(7) Uani 1 1 d . . . F7 F 0.17570(15) 0.92284(15) 0.83278(14) 0.0744(8) Uani 1 1 d . . . F8 F 0.27757(17) 0.93571(16) 0.78327(13) 0.0732(7) Uani 1 1 d . . . F9 F 0.27090(15) 1.02985(14) 0.76008(13) 0.0669(7) Uani 1 1 d . . . F10 F 0.17184(16) 1.01478(16) 0.80981(13) 0.0713(7) Uani 1 1 d . . . F11 F 0.28034(15) 1.03056(14) 0.86224(12) 0.0680(7) Uani 1 1 d . . . F12 F 0.17001(16) 0.92477(15) 0.72754(13) 0.0752(8) Uani 1 1 d . . . F13 F 0.51124(16) 0.82181(14) 0.96396(12) 0.0658(7) Uani 1 1 d . . . F14 F 0.46852(16) 0.79825(16) 0.86371(13) 0.0755(8) Uani 1 1 d . . . F15 F 0.57549(16) 0.88775(15) 0.86447(12) 0.0708(7) Uani 1 1 d . . . F16 F 0.61504(16) 0.90743(15) 0.97052(13) 0.0724(7) Uani 1 1 d . . . F17 F 0.51768(17) 0.92164(14) 0.94038(13) 0.0703(7) Uani 1 1 d . . . F18 F 0.57244(17) 0.80499(15) 0.89111(14) 0.0734(8) Uani 1 1 d . . . F19 F 0.16501(15) 0.21506(13) 0.76466(15) 0.0713(7) Uani 1 1 d . . . F20 F 0.21933(16) 0.31943(16) 0.84741(13) 0.0719(7) Uani 1 1 d . . . F21 F 0.21259(15) 0.38013(13) 0.78324(14) 0.0667(7) Uani 1 1 d . . . F22 F 0.15464(16) 0.27451(16) 0.70155(12) 0.0725(8) Uani 1 1 d . . . F23 F 0.10565(14) 0.28411(15) 0.79322(13) 0.0658(7) Uani 1 1 d . . . F24 F 0.26860(14) 0.30604(15) 0.75524(13) 0.0679(7) Uani 1 1 d . . . F25 F 0.70017(16) 0.33418(14) 0.28784(12) 0.0659(7) Uani 1 1 d . . . F26 F 0.66891(15) 0.41984(15) 0.34506(14) 0.0709(7) Uani 1 1 d . . . F27 F 0.77143(16) 0.46306(14) 0.42211(13) 0.0685(7) Uani 1 1 d . . . F28 F 0.80151(14) 0.37517(15) 0.36279(14) 0.0698(7) Uani 1 1 d . . . F29 F 0.78091(16) 0.45248(15) 0.31902(13) 0.0726(7) Uani 1 1 d . . . F30 F 0.68661(15) 0.34069(14) 0.39017(13) 0.0635(6) Uani 1 1 d . . . F31 F 1.06731(16) 0.06753(16) 0.91220(13) 0.0751(8) Uani 1 1 d . . . F32 F 1.04301(17) 0.11886(15) 0.83431(13) 0.0732(7) Uani 1 1 d . . . F33 F 0.92416(16) 0.03886(15) 0.81261(13) 0.0713(7) Uani 1 1 d . . . F34 F 0.94425(16) -0.00973(15) 0.88130(13) 0.0707(7) Uani 1 1 d . . . F35 F 1.01617(17) 0.00434(15) 0.80355(14) 0.0772(8) Uani 1 1 d . . . F36 F 0.96568(16) 0.11252(15) 0.90450(14) 0.0735(8) Uani 1 1 d . . . F37 F 0.71470(14) 0.25096(14) 1.00426(13) 0.0649(7) Uani 1 1 d . . . F38 F 0.77360(16) 0.23775(15) 0.92185(13) 0.0721(7) Uani 1 1 d . . . F39 F 0.85971(14) 0.34736(15) 0.95756(12) 0.0658(7) Uani 1 1 d . . . F40 F 0.80174(15) 0.36760(15) 1.05078(12) 0.0687(7) Uani 1 1 d . . . F41 F 0.83934(15) 0.28464(15) 1.02904(13) 0.0663(7) Uani 1 1 d . . . F42 F 0.73720(15) 0.32676(14) 0.95097(13) 0.0684(7) Uani 1 1 d . . . F43 F -0.01953(16) 0.72004(16) 0.41842(13) 0.0749(8) Uani 1 1 d . . . F44 F -0.00083(16) 0.72121(14) 0.51631(13) 0.0692(7) Uani 1 1 d . . . F45 F 0.08752(14) 0.82081(14) 0.54461(12) 0.0609(6) Uani 1 1 d . . . F46 F 0.08236(16) 0.83871(15) 0.44741(13) 0.0747(8) Uani 1 1 d . . . F47 F -0.02718(15) 0.80038(15) 0.50859(15) 0.0738(8) Uani 1 1 d . . . F48 F 0.07999(17) 0.72571(16) 0.46982(14) 0.0747(8) Uani 1 1 d . . . N1 N 0.34871(18) 0.58503(17) 0.87722(15) 0.0442(7) Uani 1 1 d . . . N2 N 0.93149(18) 0.70624(17) 0.99660(15) 0.0437(7) Uani 1 1 d . . . N3 N 0.94696(17) 0.78103(17) 0.70206(14) 0.0413(7) Uani 1 1 d . . . N4 N 0.70972(17) 0.16679(17) 0.37898(14) 0.0413(7) Uani 1 1 d . . . N5 N 0.52409(17) 0.06314(17) 0.86696(15) 0.0434(7) Uani 1 1 d . . . N6 N 0.44433(16) 0.22214(15) 0.31462(15) 0.0424(7) Uani 1 1 d . . . N7 N 0.68123(17) 0.76853(17) 1.07088(15) 0.0437(7) Uani 1 1 d . . . N8 N 0.73804(17) 0.64816(16) 0.41967(14) 0.0385(6) Uani 1 1 d . . . N9 N 0.89999(18) 0.18744(17) 0.75767(15) 0.0434(7) Uani 1 1 d . . . N10 N 0.10523(17) 0.04186(17) 0.61715(15) 0.0424(7) Uani 1 1 d . . . N11 N 0.58313(18) 0.01796(16) 0.60156(14) 0.0399(7) Uani 1 1 d . . . O1 O 0.50427(15) -0.03795(15) 0.66535(12) 0.0483(6) Uani 1 1 d . . . O1W O 0.7968(4) 0.8228(5) 0.9279(4) 0.0417(19) Uani 0.30 1 d P . . H1X H 0.7583 0.7816 0.9105 0.050 Uiso 0.30 1 d PR . . H1Y H 0.8193 0.8376 0.8983 0.050 Uiso 0.30 1 d PR . . O2W O 0.8764(5) 0.4301(5) 0.5564(5) 0.057(3) Uani 0.30 1 d P . . H2X H 0.8698 0.4616 0.5861 0.069 Uiso 0.30 1 d PR . . H2Y H 0.9223 0.4482 0.5508 0.069 Uiso 0.30 1 d PR . . O3W O 0.8371(8) 0.1367(8) 0.9909(7) 0.096(4) Uani 0.30 1 d P . . H3X H 0.8401 0.1565 0.9611 0.115 Uiso 0.30 1 d PR . . H3Y H 0.7942 0.1266 1.0027 0.115 Uiso 0.30 1 d PR . . O4W O 0.7598(4) 0.8751(4) 0.8579(4) 0.0333(16) Uani 0.30 1 d P . . H4X H 0.7502 0.8989 0.8920 0.040 Uiso 0.30 1 d PR . . H4Y H 0.8014 0.9030 0.8494 0.040 Uiso 0.30 1 d PR . . O5W O 0.9528(5) 0.5231(5) 0.1378(4) 0.043(2) Uani 0.30 1 d P . . H5X H 0.9540 0.5491 0.1136 0.051 Uiso 0.30 1 d PR . . H5Y H 0.9184 0.4796 0.1198 0.051 Uiso 0.30 1 d PR . . O6W O 0.6829(9) 0.1983(9) 0.6919(6) 0.116(6) Uani 0.30 1 d P . . H6X H 0.6977 0.2163 0.6615 0.139 Uiso 0.30 1 d PR . . H6Y H 0.6778 0.1546 0.6813 0.139 Uiso 0.30 1 d PR . . O7W O 0.7999(7) 0.2440(5) 0.1628(5) 0.062(3) Uani 0.30 1 d P . . H7X H 0.7823 0.2013 0.1352 0.075 Uiso 0.30 1 d PR . . H7Y H 0.8475 0.2664 0.1642 0.075 Uiso 0.30 1 d PR . . O8W O 0.0681(9) 0.6975(8) 0.8191(6) 0.099(5) Uani 0.30 1 d P . . H8X H 0.0943 0.6812 0.7955 0.119 Uiso 0.30 1 d PR . . H8Y H 0.0316 0.6620 0.8262 0.119 Uiso 0.30 1 d PR . . O9W O 0.0145(6) 0.4308(6) 0.4215(5) 0.068(3) Uani 0.30 1 d P . . H9X H 0.0477 0.4554 0.4025 0.082 Uiso 0.30 1 d PR . . H9Y H 0.0198 0.3929 0.4215 0.082 Uiso 0.30 1 d PR . . O10W O 0.0950(5) 0.9332(4) 0.9005(4) 0.050(2) Uani 0.30 1 d P . . H10X H 0.1366 0.9475 0.9257 0.060 Uiso 0.30 1 d PR . . H10Y H 0.0951 0.9685 0.8888 0.060 Uiso 0.30 1 d PR . . O11W O 0.0000 0.5000 0.0000 0.0603(18) Uani 0.60 2 d SP . . H11X H 0.0042 0.5195 0.0407 0.072 Uiso 0.30 1 d PR . . H11Y H 0.0021 0.5304 -0.0196 0.072 Uiso 0.30 1 d PR . . O12W O 0.0843(5) 0.4909(5) 0.6905(4) 0.048(2) Uani 0.30 1 d P . . H12X H 0.0864 0.4516 0.6909 0.058 Uiso 0.30 1 d PR . . H12Y H 0.0465 0.4929 0.7070 0.058 Uiso 0.30 1 d PR . . O13W O 0.2004(5) 0.0288(4) 1.0011(4) 0.054(2) Uani 0.30 1 d P . . H13X H 0.2146 -0.0022 1.0075 0.065 Uiso 0.30 1 d PR . . H13Y H 0.1587 0.0064 0.9742 0.065 Uiso 0.30 1 d PR . . O14W O 0.6970(4) 0.0205(4) 0.8002(4) 0.0392(18) Uani 0.30 1 d P . . H14X H 0.6756 0.0210 0.7655 0.047 Uiso 0.30 1 d PR . . H14Y H 0.7281 0.0641 0.8227 0.047 Uiso 0.30 1 d PR . . O15W O 0.2903(4) 0.3089(4) 0.1881(4) 0.0570(19) Uani 0.40 1 d P . . H15D H 0.3055 0.3235 0.2291 0.068 Uiso 0.40 1 d PR . . H15C H 0.2839 0.2650 0.1721 0.068 Uiso 0.40 1 d PR . . O16W O 0.3258(4) 0.8690(4) 0.8925(3) 0.060(2) Uani 0.40 1 d P . . H16X H 0.3339 0.8477 0.8562 0.073 Uiso 0.40 1 d PR . . H16Y H 0.3196 0.9053 0.8888 0.073 Uiso 0.40 1 d PR . . P1 P 0.83038(7) 0.92208(7) 0.59596(5) 0.0578(3) Uani 1 1 d . . . P2 P 0.22329(7) 0.97540(7) 0.79643(6) 0.0589(3) Uani 1 1 d . . . P3 P 0.53279(7) 0.85562(7) 0.91338(6) 0.0577(3) Uani 1 1 d . . . P4 P 0.18888(7) 0.29731(6) 0.77513(5) 0.0542(3) Uani 1 1 d . . . P5 P 0.73449(7) 0.39793(6) 0.35476(5) 0.0541(3) Uani 1 1 d . . . P6 P 0.99560(7) 0.05581(7) 0.85880(6) 0.0598(3) Uani 1 1 d . . . P7 P 0.78863(7) 0.30183(6) 0.98519(5) 0.0552(3) Uani 1 1 d . . . P8 P 0.02756(7) 0.77220(6) 0.47966(6) 0.0582(3) 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 0.03339(12) 0.02906(12) 0.03083(12) 0.01340(9) 0.01094(9) 0.01342(10) Cd2 0.03306(12) 0.02968(12) 0.03156(12) 0.01385(9) 0.01105(9) 0.01330(10) Cd3 0.03112(12) 0.03190(12) 0.03036(11) 0.01405(9) 0.01195(9) 0.01300(10) Cd4 0.02937(11) 0.02834(11) 0.03120(11) 0.01317(9) 0.01196(9) 0.01306(9) S1 0.0316(4) 0.0289(4) 0.0317(4) 0.0132(3) 0.0097(3) 0.0121(3) S2 0.0348(4) 0.0282(4) 0.0320(4) 0.0147(3) 0.0120(3) 0.0154(3) S3 0.0328(4) 0.0302(4) 0.0311(4) 0.0133(3) 0.0114(3) 0.0133(3) S4 0.0314(4) 0.0319(4) 0.0300(4) 0.0127(3) 0.0121(3) 0.0166(3) S5 0.0293(4) 0.0288(4) 0.0306(4) 0.0164(3) 0.0137(3) 0.0157(3) S6 0.0292(4) 0.0305(4) 0.0304(4) 0.0147(3) 0.0105(3) 0.0137(3) S7 0.0318(4) 0.0294(4) 0.0326(4) 0.0138(3) 0.0109(3) 0.0130(3) S8 0.0373(4) 0.0342(4) 0.0336(4) 0.0181(3) 0.0164(3) 0.0195(3) S9 0.0328(4) 0.0316(4) 0.0310(4) 0.0184(3) 0.0131(3) 0.0158(3) S10 0.0296(4) 0.0287(4) 0.0321(4) 0.0132(3) 0.0146(3) 0.0166(3) C1 0.0363(17) 0.0397(18) 0.0290(16) 0.0177(14) 0.0136(13) 0.0156(15) C2 0.0423(18) 0.0455(19) 0.0375(17) 0.0320(15) 0.0244(15) 0.0260(16) C3 0.0351(17) 0.0368(17) 0.0306(16) 0.0157(14) 0.0087(13) 0.0140(14) C4 0.0388(19) 0.042(2) 0.0350(18) 0.0107(15) 0.0058(15) 0.0113(16) C5 0.0316(17) 0.045(2) 0.0421(19) 0.0145(16) -0.0055(14) 0.0131(16) C6 0.050(2) 0.0336(18) 0.046(2) 0.0176(16) 0.0197(17) 0.0167(16) C7 0.046(2) 0.0322(17) 0.0348(18) 0.0074(14) 0.0063(15) 0.0154(15) C8 0.051(2) 0.0371(19) 0.0268(16) 0.0066(14) 0.0131(15) 0.0129(16) C9 0.041(2) 0.0388(19) 0.049(2) 0.0148(17) 0.0142(17) 0.0111(16) C10 0.045(2) 0.047(2) 0.0352(18) 0.0093(16) 0.0169(16) 0.0117(17) C11 0.060(2) 0.0371(19) 0.0388(19) 0.0045(15) 0.0154(17) 0.0201(18) C12 0.050(2) 0.0347(18) 0.0364(18) 0.0092(15) 0.0058(15) 0.0183(16) C13 0.0385(19) 0.0372(19) 0.043(2) 0.0163(16) 0.0117(15) 0.0084(15) C14 0.0151(14) 0.046(2) 0.047(2) 0.0151(16) 0.0122(13) 0.0059(13) C15 0.053(2) 0.047(2) 0.042(2) 0.0138(18) 0.0128(18) 0.0116(19) C16 0.0291(16) 0.0370(18) 0.051(2) 0.0198(16) 0.0056(15) 0.0096(14) C17 0.043(2) 0.0363(19) 0.046(2) 0.0060(16) 0.0106(17) 0.0059(16) C18 0.0292(17) 0.045(2) 0.0421(19) 0.0151(16) 0.0108(14) 0.0081(15) C19 0.0355(18) 0.050(2) 0.0396(19) 0.0139(16) 0.0181(15) 0.0137(16) C20 0.0369(18) 0.0318(17) 0.0361(18) 0.0006(14) 0.0111(14) 0.0107(14) C21 0.0421(19) 0.045(2) 0.0322(17) 0.0156(15) 0.0191(15) 0.0136(16) C22 0.0335(18) 0.048(2) 0.0378(19) 0.0088(16) 0.0169(15) 0.0117(16) C23 0.044(2) 0.051(2) 0.0370(19) 0.0025(16) 0.0117(16) 0.0267(18) C24 0.045(2) 0.039(2) 0.046(2) -0.0016(16) 0.0097(17) 0.0123(17) C25 0.0402(18) 0.0268(16) 0.0409(18) 0.0143(14) 0.0111(14) 0.0163(14) C26 0.0292(17) 0.0346(18) 0.054(2) 0.0122(16) 0.0019(15) 0.0063(14) C27 0.0391(19) 0.051(2) 0.042(2) 0.0238(17) 0.0147(16) 0.0056(17) C28 0.0442(19) 0.051(2) 0.0278(16) 0.0179(15) 0.0139(14) 0.0182(17) C29 0.0454(19) 0.0325(17) 0.0320(17) 0.0027(14) 0.0091(14) 0.0189(15) C30 0.051(2) 0.0288(16) 0.0163(13) 0.0076(12) 0.0090(13) 0.0075(15) C31 0.0261(16) 0.045(2) 0.0344(17) 0.0123(15) 0.0084(13) 0.0030(15) C32 0.0335(17) 0.0285(16) 0.0382(17) 0.0188(14) 0.0094(14) 0.0065(13) C33 0.0339(17) 0.0317(17) 0.0340(17) 0.0120(14) 0.0090(13) 0.0106(14) C34 0.041(2) 0.042(2) 0.0392(19) 0.0129(16) 0.0091(15) 0.0110(16) C35 0.0367(18) 0.0316(17) 0.049(2) 0.0142(15) 0.0174(16) 0.0060(15) C36 0.0346(17) 0.0261(16) 0.0391(18) 0.0139(14) 0.0079(14) -0.0018(13) C37 0.0339(17) 0.0345(17) 0.0428(19) 0.0091(15) 0.0045(14) 0.0167(15) C38 0.0404(19) 0.0423(19) 0.0351(18) 0.0109(15) 0.0121(15) 0.0165(16) C39 0.0389(19) 0.043(2) 0.044(2) 0.0117(16) 0.0238(16) 0.0096(16) C40 0.045(2) 0.051(2) 0.0393(19) 0.0267(17) 0.0203(16) 0.0233(17) C41 0.0386(18) 0.0447(19) 0.0368(18) 0.0153(15) 0.0194(15) 0.0200(16) C42 0.0327(17) 0.0357(18) 0.0296(16) 0.0067(14) 0.0032(13) 0.0089(14) C43 0.0366(18) 0.0373(18) 0.0420(18) 0.0200(15) 0.0154(15) 0.0189(15) C44 0.0381(19) 0.043(2) 0.052(2) 0.0112(18) 0.0174(17) 0.0085(16) C45 0.050(2) 0.0314(18) 0.052(2) 0.0122(17) 0.0240(18) 0.0048(16) C46 0.0405(19) 0.0373(19) 0.0396(19) 0.0126(15) 0.0090(15) 0.0102(16) C47 0.0338(18) 0.0356(18) 0.049(2) 0.0107(16) 0.0234(16) 0.0113(15) C48 0.0354(18) 0.046(2) 0.0390(18) 0.0227(16) 0.0085(14) 0.0171(16) C49 0.0318(17) 0.0244(16) 0.062(2) 0.0219(15) 0.0149(16) 0.0082(13) C50 0.043(2) 0.041(2) 0.051(2) 0.0094(17) 0.0076(17) 0.0120(17) C51 0.066(3) 0.056(2) 0.042(2) 0.0146(18) 0.0168(19) 0.031(2) C52 0.069(3) 0.036(2) 0.063(3) 0.0141(18) 0.031(2) 0.026(2) C53 0.075(3) 0.039(2) 0.065(3) 0.0181(19) 0.030(2) 0.031(2) C54 0.059(2) 0.051(2) 0.045(2) 0.0194(18) 0.0124(18) 0.028(2) C55 0.0324(17) 0.0260(16) 0.060(2) 0.0197(16) 0.0218(16) 0.0081(14) C56 0.0339(17) 0.0329(17) 0.0425(19) 0.0048(15) 0.0062(14) 0.0120(15) C57 0.0387(18) 0.0432(19) 0.0315(17) 0.0164(14) 0.0194(14) 0.0182(15) C58 0.0351(17) 0.0401(19) 0.0348(17) 0.0095(15) 0.0102(14) 0.0127(15) C59 0.0298(17) 0.045(2) 0.0352(17) 0.0053(15) 0.0050(14) 0.0160(15) C60 0.0365(18) 0.044(2) 0.0265(16) 0.0031(14) 0.0076(14) 0.0091(16) C61 0.0341(18) 0.045(2) 0.0415(19) 0.0147(16) 0.0037(15) 0.0129(16) C62 0.058(2) 0.0329(18) 0.043(2) 0.0191(15) 0.0199(17) 0.0186(17) C63 0.043(2) 0.0375(19) 0.054(2) 0.0127(17) 0.0148(17) 0.0139(16) C64 0.0400(19) 0.044(2) 0.0362(18) 0.0139(15) 0.0138(15) 0.0099(16) C65 0.045(2) 0.056(2) 0.0364(18) 0.0206(17) 0.0199(16) 0.0200(18) C66 0.057(2) 0.055(2) 0.0348(18) 0.0177(17) 0.0166(17) 0.028(2) C67 0.0384(19) 0.0391(19) 0.043(2) 0.0167(16) -0.0103(15) 0.0001(16) C68 0.041(2) 0.0355(19) 0.063(2) 0.0149(18) 0.0166(18) 0.0073(16) C69 0.0403(19) 0.042(2) 0.044(2) 0.0087(16) 0.0056(16) 0.0142(16) C70 0.047(2) 0.043(2) 0.042(2) 0.0071(16) 0.0082(16) 0.0163(17) C71 0.052(2) 0.046(2) 0.046(2) 0.0104(17) 0.0196(18) 0.0156(18) C72 0.053(2) 0.053(2) 0.0340(19) 0.0101(17) 0.0018(16) 0.0152(19) C73 0.0431(19) 0.0415(19) 0.0252(16) 0.0104(14) 0.0101(14) 0.0122(16) C74 0.045(2) 0.055(2) 0.048(2) 0.0164(19) 0.0118(17) 0.0185(19) C75 0.051(2) 0.0328(19) 0.053(2) 0.0046(16) -0.0057(18) 0.0131(17) C76 0.056(2) 0.041(2) 0.054(2) 0.0156(18) 0.0122(19) 0.0201(19) C77 0.043(2) 0.0409(19) 0.0351(18) 0.0059(15) 0.0120(15) 0.0090(16) C78 0.046(2) 0.044(2) 0.0382(19) 0.0065(16) 0.0136(16) 0.0141(17) C79 0.049(2) 0.0262(16) 0.047(2) 0.0119(15) 0.0148(17) 0.0072(15) C80 0.052(2) 0.040(2) 0.046(2) 0.0144(17) 0.0248(18) 0.0156(17) C81 0.050(2) 0.0304(17) 0.048(2) 0.0091(15) 0.0207(17) 0.0137(16) C82 0.0317(17) 0.0396(19) 0.053(2) 0.0178(16) 0.0064(15) 0.0152(15) C83 0.069(2) 0.0425(19) 0.0297(17) 0.0174(15) 0.0184(16) 0.0314(19) C84 0.043(2) 0.057(2) 0.042(2) 0.0063(17) 0.0094(16) 0.0253(18) C85 0.055(2) 0.046(2) 0.044(2) 0.0149(17) 0.0080(17) 0.0220(19) C86 0.063(3) 0.039(2) 0.036(2) -0.0107(16) 0.0034(18) 0.0153(19) C87 0.051(2) 0.0397(19) 0.0363(18) 0.0042(15) 0.0131(16) 0.0184(17) C88 0.039(2) 0.049(2) 0.064(2) 0.0154(19) 0.0205(18) 0.0229(17) C89 0.0426(19) 0.0393(18) 0.0389(18) 0.0219(15) 0.0152(15) 0.0140(16) C90 0.0368(19) 0.046(2) 0.0374(19) -0.0013(16) 0.0104(15) 0.0107(16) C91 0.0296(16) 0.0325(17) 0.0376(17) 0.0114(14) -0.0048(13) 0.0103(13) C92 0.0431(19) 0.048(2) 0.0409(19) 0.0200(16) 0.0227(16) 0.0196(17) C93 0.0308(17) 0.0407(19) 0.0408(19) 0.0143(15) 0.0043(14) 0.0066(15) F1 0.0576(15) 0.0597(15) 0.0746(17) 0.0115(13) 0.0214(13) 0.0154(13) F2 0.0616(16) 0.0628(16) 0.0569(15) 0.0203(12) 0.0045(12) 0.0089(13) F3 0.0592(15) 0.0532(14) 0.0613(15) 0.0101(12) 0.0135(12) 0.0127(12) F4 0.0549(15) 0.0657(16) 0.0567(15) 0.0141(13) -0.0010(12) 0.0049(13) F5 0.0612(15) 0.0587(15) 0.0644(16) 0.0235(12) 0.0185(12) 0.0154(12) F6 0.0583(15) 0.0606(15) 0.0496(14) 0.0161(12) 0.0094(11) -0.0013(12) F7 0.0517(15) 0.0700(17) 0.0764(18) 0.0225(14) 0.0200(13) 0.0032(13) F8 0.0809(19) 0.0722(18) 0.0643(16) 0.0133(14) 0.0244(14) 0.0361(15) F9 0.0695(17) 0.0525(14) 0.0628(15) 0.0177(12) 0.0230(13) 0.0115(13) F10 0.0700(17) 0.0746(18) 0.0626(16) 0.0124(14) 0.0212(13) 0.0305(15) F11 0.0668(16) 0.0515(14) 0.0566(15) 0.0026(12) 0.0016(12) 0.0092(13) F12 0.0655(17) 0.0675(17) 0.0550(15) -0.0014(13) 0.0046(13) 0.0079(14) F13 0.0821(18) 0.0616(15) 0.0543(14) 0.0211(12) 0.0194(13) 0.0302(14) F14 0.0692(17) 0.0738(18) 0.0573(15) 0.0142(14) 0.0076(13) 0.0118(14) F15 0.0810(18) 0.0605(16) 0.0506(14) 0.0150(12) 0.0180(13) 0.0136(14) F16 0.0689(17) 0.0619(16) 0.0536(15) 0.0029(12) 0.0028(13) 0.0087(13) F17 0.0866(19) 0.0501(14) 0.0674(17) 0.0128(12) 0.0222(14) 0.0266(14) F18 0.0837(19) 0.0571(16) 0.0691(17) 0.0071(13) 0.0213(15) 0.0289(14) F19 0.0602(16) 0.0450(14) 0.090(2) 0.0119(13) 0.0217(14) 0.0113(12) F20 0.0668(17) 0.0770(18) 0.0534(15) 0.0087(13) 0.0041(13) 0.0227(14) F21 0.0602(15) 0.0485(14) 0.0804(18) 0.0179(13) 0.0170(13) 0.0151(12) F22 0.0722(18) 0.0816(19) 0.0447(13) 0.0010(13) 0.0093(12) 0.0282(15) F23 0.0559(15) 0.0715(17) 0.0663(16) 0.0243(13) 0.0201(12) 0.0225(13) F24 0.0536(15) 0.0696(17) 0.0711(17) 0.0194(14) 0.0217(13) 0.0193(13) F25 0.0736(17) 0.0639(16) 0.0483(14) 0.0087(12) -0.0092(12) 0.0270(14) F26 0.0617(16) 0.0641(16) 0.0789(18) 0.0208(14) 0.0104(14) 0.0220(13) F27 0.0743(18) 0.0565(15) 0.0567(15) 0.0069(12) -0.0041(13) 0.0206(13) F28 0.0495(14) 0.0707(17) 0.0711(17) 0.0179(14) 0.0018(12) 0.0134(13) F29 0.0649(17) 0.0723(18) 0.0655(16) 0.0285(14) 0.0174(13) 0.0116(14) F30 0.0621(15) 0.0531(14) 0.0651(15) 0.0244(12) 0.0215(12) 0.0115(12) F31 0.0643(17) 0.0799(19) 0.0610(16) 0.0223(14) 0.0034(13) 0.0140(14) F32 0.0776(18) 0.0708(17) 0.0617(16) 0.0289(14) 0.0211(14) 0.0185(15) F33 0.0683(17) 0.0627(16) 0.0665(16) 0.0159(13) -0.0074(13) 0.0185(14) F34 0.0736(18) 0.0634(16) 0.0619(16) 0.0227(13) 0.0151(13) 0.0162(14) F35 0.0805(19) 0.0639(17) 0.0704(18) 0.0087(14) 0.0179(15) 0.0237(15) F36 0.0724(18) 0.0562(15) 0.0740(18) 0.0063(13) 0.0168(14) 0.0202(14) F37 0.0522(14) 0.0619(15) 0.0637(16) 0.0136(13) 0.0126(12) 0.0131(12) F38 0.0746(18) 0.0596(16) 0.0620(16) 0.0082(13) 0.0208(14) 0.0169(14) F39 0.0514(14) 0.0670(16) 0.0564(15) 0.0176(12) 0.0101(11) 0.0064(12) F40 0.0633(16) 0.0729(17) 0.0552(15) 0.0076(13) 0.0115(12) 0.0243(14) F41 0.0580(15) 0.0634(16) 0.0669(16) 0.0169(13) 0.0094(12) 0.0195(13) F42 0.0569(15) 0.0546(15) 0.0706(17) 0.0121(13) -0.0019(13) 0.0093(12) F43 0.0592(16) 0.0711(18) 0.0648(17) 0.0036(14) 0.0085(13) 0.0126(14) F44 0.0745(17) 0.0548(15) 0.0610(16) 0.0118(12) 0.0215(13) 0.0158(13) F45 0.0544(14) 0.0593(15) 0.0518(14) 0.0134(11) 0.0069(11) 0.0121(12) F46 0.0709(18) 0.0634(16) 0.0638(16) 0.0201(13) 0.0133(14) 0.0055(14) F47 0.0599(16) 0.0637(16) 0.0855(19) 0.0154(14) 0.0219(14) 0.0203(13) F48 0.0724(18) 0.0696(17) 0.0734(18) 0.0083(14) 0.0169(14) 0.0318(15) N1 0.0466(17) 0.0449(17) 0.0423(17) 0.0140(14) 0.0158(14) 0.0206(15) N2 0.0427(17) 0.0470(18) 0.0411(16) 0.0132(14) 0.0177(13) 0.0191(14) N3 0.0387(16) 0.0467(17) 0.0332(15) 0.0163(13) 0.0036(12) 0.0120(14) N4 0.0416(16) 0.0429(17) 0.0363(15) 0.0070(13) 0.0150(13) 0.0184(14) N5 0.0414(17) 0.0436(17) 0.0400(16) 0.0103(13) 0.0085(13) 0.0157(14) N6 0.0306(15) 0.0279(14) 0.0512(18) 0.0050(13) 0.0195(13) 0.0002(12) N7 0.0385(16) 0.0402(16) 0.0451(17) 0.0157(14) 0.0125(13) 0.0088(13) N8 0.0392(16) 0.0416(16) 0.0406(16) 0.0180(13) 0.0141(13) 0.0197(13) N9 0.0481(18) 0.0444(17) 0.0380(16) 0.0100(13) 0.0066(13) 0.0228(15) N10 0.0393(16) 0.0424(17) 0.0432(17) 0.0102(14) 0.0110(13) 0.0179(14) N11 0.0535(18) 0.0352(15) 0.0399(16) 0.0146(13) 0.0175(14) 0.0254(14) O1 0.0458(15) 0.0477(15) 0.0404(14) 0.0133(12) 0.0108(11) 0.0106(12) O1W 0.028(4) 0.055(5) 0.050(5) 0.007(4) 0.023(3) 0.030(4) O2W 0.046(5) 0.045(5) 0.085(7) 0.010(5) -0.023(5) 0.034(4) O3W 0.101(10) 0.115(11) 0.108(10) 0.075(9) 0.042(8) 0.055(9) O4W 0.038(4) 0.016(3) 0.046(4) 0.003(3) 0.009(3) 0.015(3) O5W 0.044(5) 0.047(5) 0.024(4) 0.009(3) -0.016(3) 0.012(4) O6W 0.125(12) 0.111(11) 0.066(8) 0.019(8) -0.049(8) 0.024(10) O7W 0.091(8) 0.049(5) 0.057(6) 0.018(5) 0.016(5) 0.040(6) O8W 0.135(12) 0.105(10) 0.089(9) 0.035(8) -0.018(8) 0.084(10) O9W 0.069(7) 0.056(6) 0.056(6) 0.022(5) 0.025(5) 0.002(5) O10W 0.049(5) 0.028(4) 0.056(5) -0.001(4) 0.016(4) 0.008(4) O11W 0.037(3) 0.056(4) 0.069(5) 0.017(4) -0.002(3) 0.006(3) O12W 0.038(4) 0.047(5) 0.040(5) 0.026(4) 0.006(4) -0.007(4) O13W 0.052(5) 0.029(4) 0.038(5) -0.002(3) -0.017(4) -0.014(4) O14W 0.036(4) 0.023(4) 0.055(5) 0.010(3) 0.024(4) 0.011(3) O15W 0.060(4) 0.033(3) 0.069(5) 0.025(3) 0.026(4) 0.006(3) O16W 0.051(4) 0.051(4) 0.029(3) -0.020(3) -0.010(3) -0.004(3) P1 0.0536(6) 0.0580(7) 0.0445(6) 0.0121(5) 0.0083(5) 0.0113(5) P2 0.0500(6) 0.0562(7) 0.0495(6) 0.0095(5) 0.0159(5) 0.0077(5) P3 0.0548(6) 0.0522(6) 0.0555(6) 0.0130(5) 0.0096(5) 0.0162(5) P4 0.0553(6) 0.0559(6) 0.0466(6) 0.0173(5) 0.0192(5) 0.0188(5) P5 0.0539(6) 0.0523(6) 0.0448(6) 0.0141(5) 0.0114(5) 0.0136(5) P6 0.0543(6) 0.0560(7) 0.0588(7) 0.0153(5) 0.0109(5) 0.0168(5) P7 0.0534(6) 0.0536(6) 0.0472(6) 0.0118(5) 0.0120(5) 0.0155(5) P8 0.0590(7) 0.0496(6) 0.0508(6) 0.0105(5) 0.0116(5) 0.0130(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 S7 2.4488(8) . ? Cd1 S1 2.5116(8) . ? Cd1 S2 2.5475(8) . ? Cd1 S5 2.5518(8) . ? Cd2 S8 2.4463(8) . ? Cd2 S6 2.5441(8) . ? Cd2 S3 2.5479(8) . ? Cd2 S1 2.5619(8) . ? Cd3 S9 2.4566(8) . ? Cd3 S3 2.5251(8) . ? Cd3 S2 2.5492(8) . ? Cd3 S4 2.5828(8) . ? Cd4 S10 2.4649(8) . ? Cd4 S4 2.5220(8) . ? Cd4 S5 2.5588(8) . ? Cd4 S6 2.5614(8) . ? S1 C1 1.763(3) . ? S2 C7 1.738(4) . ? S3 C13 1.727(4) . ? S4 C19 1.761(4) . ? S5 C25 1.788(3) . ? S6 C31 1.767(3) . ? S7 C37 1.782(3) . ? S8 C43 1.809(3) . ? S9 C49 1.691(3) . ? S10 C55 1.772(3) . ? C1 C6 1.385(5) . ? C1 C2 1.393(5) . ? C2 C3 1.425(5) . ? C2 H2 0.9300 . ? C3 C4 1.354(5) . ? C3 H3 0.9300 . ? C4 C5 1.418(5) . ? C4 N1 1.527(4) . ? C5 C6 1.420(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.392(5) . ? C7 C8 1.411(5) . ? C8 C9 1.295(5) . ? C8 H8 0.9300 . ? C9 C10 1.442(5) . ? C9 H9 0.9300 . ? C10 C11 1.375(5) . ? C10 N2 1.520(4) . ? C11 C12 1.393(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.380(5) . ? C13 C14 1.399(5) . ? C14 C15 1.387(5) . ? C14 H14 0.9300 . ? C15 C16 1.386(5) . ? C15 H15 0.9300 . ? C16 C17 1.360(5) . ? C16 N3 1.502(3) . ? C17 C18 1.419(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.390(5) . ? C19 C24 1.390(5) . ? C20 C21 1.390(5) . ? C20 H20 0.9300 . ? C21 C22 1.390(5) . ? C21 H21 0.9300 . ? C22 C23 1.390(5) . ? C22 N4 1.490(3) . ? C23 C24 1.390(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.381(5) . ? C25 C26 1.394(5) . ? C26 C27 1.386(5) . ? C26 H26 0.9300 . ? C27 C28 1.384(5) . ? C27 H27 0.9300 . ? C28 C29 1.413(5) . ? C28 N5 1.492(4) . ? C29 C30 1.340(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.390(5) . ? C31 C36 1.390(4) . ? C32 C33 1.390(5) . ? C32 H32 0.9300 . ? C33 C34 1.390(5) . ? C33 H33 0.9300 . ? C34 C35 1.390(5) . ? C34 N6 1.529(4) . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.379(5) . ? C37 C38 1.380(5) . ? C38 C39 1.342(5) . ? C38 H38 0.9300 . ? C39 C40 1.374(5) . ? C39 H39 0.9300 . ? C40 C41 1.424(5) . ? C40 N7 1.510(4) . ? C41 C42 1.398(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.338(5) . ? C43 C44 1.370(5) . ? C44 C45 1.408(5) . ? C44 H44 0.9300 . ? C45 C46 1.406(5) . ? C45 H45 0.9300 . ? C46 C47 1.396(5) . ? C46 N8 1.494(4) . ? C47 C48 1.419(5) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.390(5) . ? C49 C54 1.390(5) . ? C50 C51 1.390(6) . ? C50 H50 0.9300 . ? C51 C52 1.390(6) . ? C51 H51 0.9300 . ? C52 C53 1.390(5) . ? C52 N9 1.591(4) . ? C53 C54 1.390(6) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.372(5) . ? C55 C56 1.380(5) . ? C56 C57 1.404(5) . ? C56 H56 0.9300 . ? C57 C58 1.405(5) . ? C57 H57 0.9300 . ? C58 C59 1.421(5) . ? C58 N10 1.509(3) . ? C59 C60 1.380(5) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 N1 1.508(3) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 N1 1.532(4) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 N1 1.513(4) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 N2 1.571(3) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 N2 1.489(4) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 N2 1.541(4) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 N3 1.489(3) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 N3 1.459(4) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N3 1.471(4) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 N4 1.491(4) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 N4 1.553(4) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N4 1.506(4) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 N5 1.544(3) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 N5 1.461(4) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 N5 1.529(4) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 N6 1.484(4) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 N6 1.519(4) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 N6 1.524(4) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 N7 1.528(4) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 N7 1.550(4) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 N7 1.535(3) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 N8 1.512(3) . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 N8 1.496(3) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 N8 1.558(4) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 N9 1.476(4) . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C86 N9 1.496(4) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 N9 1.485(4) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 N10 1.485(4) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 N10 1.523(4) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 N10 1.544(4) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 O1 1.280(3) . ? C91 N11 1.327(3) . ? C91 H91 0.9300 . ? C92 N11 1.411(4) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 N11 1.532(3) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? F1 P1 1.522(3) . ? F2 P1 1.554(3) . ? F3 P1 1.608(3) . ? F4 P1 1.610(3) . ? F5 P1 1.592(3) . ? F6 P1 1.624(3) . ? F7 P2 1.550(3) . ? F8 P2 1.601(3) . ? F9 P2 1.574(3) . ? F10 P2 1.547(3) . ? F11 P2 1.588(3) . ? F12 P2 1.592(3) . ? F13 P3 1.449(3) . ? F14 P3 1.458(3) . ? F15 P3 1.510(3) . ? F16 P3 1.722(3) . ? F17 P3 1.515(3) . ? F18 P3 1.560(3) . ? F19 P4 1.547(3) . ? F20 P4 1.521(3) . ? F21 P4 1.568(3) . ? F22 P4 1.563(3) . ? F23 P4 1.627(3) . ? F24 P4 1.593(3) . ? F25 P5 1.573(3) . ? F26 P5 1.564(3) . ? F27 P5 1.594(3) . ? F28 P5 1.597(3) . ? F29 P5 1.559(3) . ? F30 P5 1.598(3) . ? F31 P6 1.672(3) . ? F32 P6 1.522(3) . ? F33 P6 1.538(3) . ? F34 P6 1.556(3) . ? F35 P6 1.576(3) . ? F36 P6 1.661(3) . ? F37 P7 1.560(3) . ? F38 P7 1.559(3) . ? F39 P7 1.582(3) . ? F40 P7 1.618(3) . ? F41 P7 1.558(3) . ? F42 P7 1.560(3) . ? F43 P8 1.444(3) . ? F44 P8 1.450(3) . ? F45 P8 1.578(3) . ? F46 P8 1.721(3) . ? F47 P8 1.515(3) . ? F48 P8 1.679(3) . ? O1W H1X 0.8501 . ? O1W H1Y 0.8501 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8500 . ? O3W H3X 0.8500 . ? O3W H3Y 0.8499 . ? O4W H4X 0.8500 . ? O4W H4Y 0.8501 . ? O5W H5X 0.8500 . ? O5W H5Y 0.8500 . ? O6W H6X 0.8499 . ? O6W H6Y 0.8499 . ? O7W H7X 0.8500 . ? O7W H7Y 0.8499 . ? O8W H8X 0.8500 . ? O8W H8Y 0.8500 . ? O9W H9X 0.8500 . ? O9W H9Y 0.8499 . ? O10W H10X 0.8501 . ? O10W H10Y 0.8499 . ? O11W H11X 0.8499 . ? O11W H11Y 0.8500 . ? O12W H12X 0.8499 . ? O12W H12Y 0.8500 . ? O13W H13X 0.8500 . ? O13W H13Y 0.8501 . ? O14W H14X 0.8501 . ? O14W H14Y 0.8499 . ? O15W H15D 0.8499 . ? O15W H15C 0.8500 . ? O16W H16X 0.8500 . ? O16W H16Y 0.8499 . ? 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 S7 Cd1 S1 117.16(3) . . ? S7 Cd1 S2 112.28(3) . . ? S1 Cd1 S2 103.08(3) . . ? S7 Cd1 S5 110.20(3) . . ? S1 Cd1 S5 108.00(3) . . ? S2 Cd1 S5 105.26(3) . . ? S8 Cd2 S6 123.15(3) . . ? S8 Cd2 S3 111.54(3) . . ? S6 Cd2 S3 106.55(3) . . ? S8 Cd2 S1 101.25(3) . . ? S6 Cd2 S1 107.11(3) . . ? S3 Cd2 S1 105.86(3) . . ? S9 Cd3 S3 113.87(3) . . ? S9 Cd3 S2 104.24(3) . . ? S3 Cd3 S2 128.20(3) . . ? S9 Cd3 S4 118.82(3) . . ? S3 Cd3 S4 101.89(3) . . ? S2 Cd3 S4 88.17(3) . . ? S10 Cd4 S4 106.76(3) . . ? S10 Cd4 S5 114.72(3) . . ? S4 Cd4 S5 108.07(3) . . ? S10 Cd4 S6 113.50(3) . . ? S4 Cd4 S6 115.37(3) . . ? S5 Cd4 S6 98.41(2) . . ? C1 S1 Cd1 105.32(11) . . ? C1 S1 Cd2 108.36(11) . . ? Cd1 S1 Cd2 118.67(3) . . ? C7 S2 Cd1 97.90(13) . . ? C7 S2 Cd3 106.50(12) . . ? Cd1 S2 Cd3 113.11(3) . . ? C13 S3 Cd3 104.92(13) . . ? C13 S3 Cd2 104.22(13) . . ? Cd3 S3 Cd2 109.45(3) . . ? C19 S4 Cd4 109.15(13) . . ? C19 S4 Cd3 104.37(13) . . ? Cd4 S4 Cd3 115.31(3) . . ? C25 S5 Cd1 107.02(12) . . ? C25 S5 Cd4 101.65(11) . . ? Cd1 S5 Cd4 110.62(3) . . ? C31 S6 Cd2 110.12(11) . . ? C31 S6 Cd4 101.07(13) . . ? Cd2 S6 Cd4 111.18(3) . . ? C37 S7 Cd1 106.51(12) . . ? C43 S8 Cd2 101.89(11) . . ? C49 S9 Cd3 100.73(12) . . ? C55 S10 Cd4 107.51(12) . . ? C6 C1 C2 120.7(3) . . ? C6 C1 S1 117.2(3) . . ? C2 C1 S1 122.1(3) . . ? C1 C2 C3 119.6(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 122.6(3) . . ? C3 C4 N1 120.2(3) . . ? C5 C4 N1 117.1(3) . . ? C4 C5 C6 117.4(3) . . ? C4 C5 H5 121.3 . . ? C6 C5 H5 121.3 . . ? C1 C6 C5 120.4(3) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C12 C7 C8 119.4(3) . . ? C12 C7 S2 120.1(3) . . ? C8 C7 S2 120.4(3) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.9(4) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 119.2(3) . . ? C11 C10 N2 119.9(3) . . ? C9 C10 N2 120.8(3) . . ? C10 C11 C12 118.6(4) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 120.8(3) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C18 C13 C14 120.4(3) . . ? C18 C13 S3 123.0(3) . . ? C14 C13 S3 116.6(3) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 121.2(4) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 118.8(3) . . ? C17 C16 N3 122.8(3) . . ? C15 C16 N3 118.0(3) . . ? C16 C17 C18 121.8(4) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C13 C18 C17 118.3(3) . . ? C13 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C24 120.0(3) . . ? C20 C19 S4 126.0(3) . . ? C24 C19 S4 113.8(3) . . ? C21 C20 C19 120.0(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 N4 121.1(3) . . ? C21 C22 N4 118.9(3) . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 120.0(4) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C30 C25 C26 119.4(3) . . ? C30 C25 S5 119.2(3) . . ? C26 C25 S5 121.2(3) . . ? C27 C26 C25 118.6(3) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C28 C27 C26 121.4(4) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 118.8(3) . . ? C27 C28 N5 121.8(3) . . ? C29 C28 N5 119.4(3) . . ? C30 C29 C28 119.4(3) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C25 122.4(3) . . ? C29 C30 H30 118.8 . . ? C25 C30 H30 118.8 . . ? C32 C31 C36 120.0(3) . . ? C32 C31 S6 120.3(2) . . ? C36 C31 S6 119.7(3) . . ? C31 C32 C33 120.0(3) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 N6 114.4(3) . . ? C35 C34 N6 125.6(3) . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0(3) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C42 C37 C38 119.0(3) . . ? C42 C37 S7 114.8(3) . . ? C38 C37 S7 126.1(3) . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 124.0(3) . . ? C38 C39 H39 118.0 . . ? C40 C39 H39 118.0 . . ? C39 C40 C41 116.8(3) . . ? C39 C40 N7 121.5(3) . . ? C41 C40 N7 121.6(3) . . ? C42 C41 C40 118.9(3) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C37 C42 C41 121.1(3) . . ? C37 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C48 C43 C44 122.5(3) . . ? C48 C43 S8 120.1(3) . . ? C44 C43 S8 116.7(3) . . ? C43 C44 C45 120.1(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 118.1(4) . . ? C46 C45 H45 121.0 . . ? C44 C45 H45 121.0 . . ? C47 C46 C45 120.7(3) . . ? C47 C46 N8 117.0(3) . . ? C45 C46 N8 122.3(3) . . ? C46 C47 C48 118.7(3) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C43 C48 C47 119.8(3) . . ? C43 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C54 120.0(3) . . ? C50 C49 S9 114.9(3) . . ? C54 C49 S9 125.2(3) . . ? C51 C50 C49 120.0(4) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 120.0(4) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.0(4) . . ? C51 C52 N9 125.1(3) . . ? C53 C52 N9 114.8(3) . . ? C54 C53 C52 120.0(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C49 120.0(4) . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? C60 C55 C56 119.8(3) . . ? C60 C55 S10 117.3(3) . . ? C56 C55 S10 122.8(3) . . ? C55 C56 C57 120.6(3) . . ? C55 C56 H56 119.7 . . ? C57 C56 H56 119.7 . . ? C56 C57 C58 119.0(3) . . ? C56 C57 H57 120.5 . . ? C58 C57 H57 120.5 . . ? C57 C58 C59 119.9(3) . . ? C57 C58 N10 117.4(3) . . ? C59 C58 N10 122.7(3) . . ? C60 C59 C58 118.4(3) . . ? C60 C59 H59 120.8 . . ? C58 C59 H59 120.8 . . ? C55 C60 C59 122.2(3) . . ? C55 C60 H60 118.9 . . ? C59 C60 H60 118.9 . . ? N1 C61 H61A 109.5 . . ? N1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N1 C62 H62A 109.5 . . ? N1 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N1 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N1 C63 H63A 109.5 . . ? N1 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N1 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N2 C64 H64A 109.5 . . ? N2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N2 C65 H65A 109.5 . . ? N2 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N2 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N2 C66 H66A 109.5 . . ? N2 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N2 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N3 C67 H67A 109.5 . . ? N3 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N3 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N3 C68 H68A 109.5 . . ? N3 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N3 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N3 C69 H69A 109.5 . . ? N3 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N3 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N4 C70 H70A 109.5 . . ? N4 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N4 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N4 C71 H71A 109.5 . . ? N4 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N4 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N4 C72 H72A 109.5 . . ? N4 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N4 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N5 C73 H73A 109.5 . . ? N5 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N5 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N5 C74 H74A 109.5 . . ? N5 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N5 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N5 C75 H75A 109.5 . . ? N5 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N5 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N6 C76 H76A 109.5 . . ? N6 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N6 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N6 C77 H77A 109.5 . . ? N6 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N6 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N6 C78 H78A 109.5 . . ? N6 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N6 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N7 C79 H79A 109.5 . . ? N7 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N7 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N7 C80 H80A 109.5 . . ? N7 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N7 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N7 C81 H81A 109.5 . . ? N7 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N7 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N8 C82 H82A 109.5 . . ? N8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N8 C83 H83A 109.5 . . ? N8 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N8 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N8 C84 H84A 109.5 . . ? N8 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N8 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N9 C85 H85A 109.5 . . ? N9 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? N9 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N9 C86 H86A 109.5 . . ? N9 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N9 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N9 C87 H87A 109.5 . . ? N9 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N9 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N10 C88 H88A 109.5 . . ? N10 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N10 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N10 C89 H89A 109.5 . . ? N10 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N10 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N10 C90 H90A 109.5 . . ? N10 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N10 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O1 C91 N11 123.0(3) . . ? O1 C91 H91 118.5 . . ? N11 C91 H91 118.5 . . ? N11 C92 H92A 109.5 . . ? N11 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N11 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N11 C93 H93A 109.5 . . ? N11 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N11 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C61 N1 C63 113.2(2) . . ? C61 N1 C4 111.6(2) . . ? C63 N1 C4 109.30(18) . . ? C61 N1 C62 109.48(19) . . ? C63 N1 C62 105.9(2) . . ? C4 N1 C62 107.07(19) . . ? C65 N2 C10 107.91(19) . . ? C65 N2 C66 111.0(2) . . ? C10 N2 C66 110.5(2) . . ? C65 N2 C64 112.2(2) . . ? C10 N2 C64 106.88(18) . . ? C66 N2 C64 108.3(2) . . ? C68 N3 C69 109.9(2) . . ? C68 N3 C67 118.1(2) . . ? C69 N3 C67 94.3(2) . . ? C68 N3 C16 118.0(2) . . ? C69 N3 C16 102.10(18) . . ? C67 N3 C16 110.51(18) . . ? C22 N4 C70 106.40(19) . . ? C22 N4 C72 113.78(19) . . ? C70 N4 C72 110.4(2) . . ? C22 N4 C71 109.72(18) . . ? C70 N4 C71 111.1(2) . . ? C72 N4 C71 105.5(2) . . ? C74 N5 C28 110.5(2) . . ? C74 N5 C75 110.6(2) . . ? C28 N5 C75 112.78(19) . . ? C74 N5 C73 111.9(2) . . ? C28 N5 C73 109.38(19) . . ? C75 N5 C73 101.4(2) . . ? C76 N6 C77 103.4(2) . . ? C76 N6 C78 125.5(2) . . ? C77 N6 C78 98.3(2) . . ? C76 N6 C34 107.7(2) . . ? C77 N6 C34 109.13(17) . . ? C78 N6 C34 111.26(17) . . ? C40 N7 C79 108.92(19) . . ? C40 N7 C81 109.19(18) . . ? C79 N7 C81 112.7(2) . . ? C40 N7 C80 109.4(2) . . ? C79 N7 C80 111.8(2) . . ? C81 N7 C80 104.8(2) . . ? C46 N8 C83 113.22(18) . . ? C46 N8 C82 106.75(18) . . ? C83 N8 C82 112.1(2) . . ? C46 N8 C84 109.03(18) . . ? C83 N8 C84 105.6(2) . . ? C82 N8 C84 110.1(2) . . ? C85 N9 C87 109.0(2) . . ? C85 N9 C86 110.6(2) . . ? C87 N9 C86 108.9(2) . . ? C85 N9 C52 105.45(19) . . ? C87 N9 C52 108.48(19) . . ? C86 N9 C52 114.17(19) . . ? C88 N10 C58 112.5(2) . . ? C88 N10 C89 110.6(2) . . ? C58 N10 C89 109.03(18) . . ? C88 N10 C90 108.6(2) . . ? C58 N10 C90 109.90(19) . . ? C89 N10 C90 106.05(18) . . ? C91 N11 C92 124.5(2) . . ? C91 N11 C93 122.2(2) . . ? C92 N11 C93 112.3(2) . . ? H1X O1W H1Y 109.5 . . ? H2X O2W H2Y 109.5 . . ? H3X O3W H3Y 109.5 . . ? H4X O4W H4Y 109.5 . . ? H5X O5W H5Y 109.5 . . ? H6X O6W H6Y 109.5 . . ? H7X O7W H7Y 109.5 . . ? H8X O8W H8Y 109.5 . . ? H9X O9W H9Y 109.5 . . ? H10X O10W H10Y 109.8 . . ? H11X O11W H11Y 109.5 . . ? H12X O12W H12Y 109.5 . . ? H13X O13W H13Y 109.5 . . ? H14X O14W H14Y 109.5 . . ? H15D O15W H15C 109.5 . . ? H16X O16W H16Y 108.3 . . ? F1 P1 F2 88.60(17) . . ? F1 P1 F5 91.07(16) . . ? F2 P1 F5 91.00(15) . . ? F1 P1 F3 178.93(16) . . ? F2 P1 F3 91.22(16) . . ? F5 P1 F3 89.99(15) . . ? F1 P1 F4 93.83(16) . . ? F2 P1 F4 177.36(18) . . ? F5 P1 F4 87.94(15) . . ? F3 P1 F4 86.37(16) . . ? F1 P1 F6 91.90(16) . . ? F2 P1 F6 89.69(14) . . ? F5 P1 F6 176.97(18) . . ? F3 P1 F6 87.05(15) . . ? F4 P1 F6 91.25(14) . . ? F10 P2 F7 88.44(17) . . ? F10 P2 F9 90.44(17) . . ? F7 P2 F9 178.85(19) . . ? F10 P2 F11 90.27(16) . . ? F7 P2 F11 91.27(16) . . ? F9 P2 F11 88.46(15) . . ? F10 P2 F12 89.65(17) . . ? F7 P2 F12 93.44(16) . . ? F9 P2 F12 86.83(16) . . ? F11 P2 F12 175.29(17) . . ? F10 P2 F8 179.16(19) . . ? F7 P2 F8 91.90(17) . . ? F9 P2 F8 89.21(16) . . ? F11 P2 F8 88.96(16) . . ? F12 P2 F8 91.09(17) . . ? F13 P3 F14 94.64(17) . . ? F13 P3 F15 163.3(2) . . ? F14 P3 F15 93.55(16) . . ? F13 P3 F17 99.10(16) . . ? F14 P3 F17 109.77(19) . . ? F15 P3 F17 91.71(17) . . ? F13 P3 F18 86.83(17) . . ? F14 P3 F18 84.87(18) . . ? F15 P3 F18 79.49(17) . . ? F17 P3 F18 163.51(18) . . ? F13 P3 F16 80.36(16) . . ? F14 P3 F16 166.69(19) . . ? F15 P3 F16 88.44(16) . . ? F17 P3 F16 83.30(16) . . ? F18 P3 F16 82.55(16) . . ? F20 P4 F19 93.04(18) . . ? F20 P4 F22 177.79(17) . . ? F19 P4 F22 87.18(17) . . ? F20 P4 F21 88.82(17) . . ? F19 P4 F21 178.11(18) . . ? F22 P4 F21 90.98(17) . . ? F20 P4 F24 92.84(16) . . ? F19 P4 F24 89.44(15) . . ? F22 P4 F24 89.36(15) . . ? F21 P4 F24 90.13(15) . . ? F20 P4 F23 88.59(15) . . ? F19 P4 F23 88.02(15) . . ? F22 P4 F23 89.22(15) . . ? F21 P4 F23 92.37(15) . . ? F24 P4 F23 177.15(16) . . ? F29 P5 F26 87.98(16) . . ? F29 P5 F25 90.24(16) . . ? F26 P5 F25 90.60(15) . . ? F29 P5 F27 88.79(16) . . ? F26 P5 F27 90.51(16) . . ? F25 P5 F27 178.49(17) . . ? F29 P5 F28 91.14(16) . . ? F26 P5 F28 178.59(17) . . ? F25 P5 F28 88.30(15) . . ? F27 P5 F28 90.58(15) . . ? F29 P5 F30 178.88(17) . . ? F26 P5 F30 92.34(16) . . ? F25 P5 F30 88.69(15) . . ? F27 P5 F30 92.28(15) . . ? F28 P5 F30 88.52(16) . . ? F32 P6 F33 90.62(17) . . ? F32 P6 F34 177.47(18) . . ? F33 P6 F34 86.90(16) . . ? F32 P6 F35 87.79(17) . . ? F33 P6 F35 90.54(17) . . ? F34 P6 F35 91.73(17) . . ? F32 P6 F36 86.69(16) . . ? F33 P6 F36 79.30(16) . . ? F34 P6 F36 93.34(16) . . ? F35 P6 F36 168.37(19) . . ? F32 P6 F31 95.36(17) . . ? F33 P6 F31 173.99(17) . . ? F34 P6 F31 87.12(16) . . ? F35 P6 F31 90.27(17) . . ? F36 P6 F31 100.42(16) . . ? F41 P7 F38 97.15(17) . . ? F41 P7 F37 91.98(16) . . ? F38 P7 F37 89.05(15) . . ? F41 P7 F42 171.44(17) . . ? F38 P7 F42 91.18(17) . . ? F37 P7 F42 86.16(16) . . ? F41 P7 F39 91.11(16) . . ? F38 P7 F39 84.83(15) . . ? F37 P7 F39 173.45(16) . . ? F42 P7 F39 91.61(16) . . ? F41 P7 F40 83.80(15) . . ? F38 P7 F40 178.43(16) . . ? F37 P7 F40 89.66(15) . . ? F42 P7 F40 87.83(16) . . ? F39 P7 F40 96.42(15) . . ? F43 P8 F44 94.54(17) . . ? F43 P8 F47 100.32(18) . . ? F44 P8 F47 84.23(17) . . ? F43 P8 F45 169.56(19) . . ? F44 P8 F45 82.53(15) . . ? F47 P8 F45 89.39(16) . . ? F43 P8 F48 86.63(17) . . ? F44 P8 F48 74.43(16) . . ? F47 P8 F48 158.05(18) . . ? F45 P8 F48 82.92(15) . . ? F43 P8 F46 95.98(16) . . ? F44 P8 F46 165.90(18) . . ? F47 P8 F46 103.02(17) . . ? F45 P8 F46 85.45(14) . . ? F48 P8 F46 96.84(16) . . ? 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 S7 Cd1 S1 C1 -46.86(12) . . . . ? S2 Cd1 S1 C1 -170.68(12) . . . . ? S5 Cd1 S1 C1 78.24(12) . . . . ? S7 Cd1 S1 Cd2 -168.33(3) . . . . ? S2 Cd1 S1 Cd2 67.85(4) . . . . ? S5 Cd1 S1 Cd2 -43.23(4) . . . . ? S8 Cd2 S1 C1 53.11(12) . . . . ? S6 Cd2 S1 C1 -77.02(12) . . . . ? S3 Cd2 S1 C1 169.57(12) . . . . ? S8 Cd2 S1 Cd1 173.04(3) . . . . ? S6 Cd2 S1 Cd1 42.90(4) . . . . ? S3 Cd2 S1 Cd1 -70.50(4) . . . . ? S7 Cd1 S2 C7 -54.10(12) . . . . ? S1 Cd1 S2 C7 72.89(12) . . . . ? S5 Cd1 S2 C7 -174.01(12) . . . . ? S7 Cd1 S2 Cd3 -165.87(3) . . . . ? S1 Cd1 S2 Cd3 -38.88(4) . . . . ? S5 Cd1 S2 Cd3 74.22(3) . . . . ? S9 Cd3 S2 C7 56.43(13) . . . . ? S3 Cd3 S2 C7 -80.55(13) . . . . ? S4 Cd3 S2 C7 175.73(13) . . . . ? S9 Cd3 S2 Cd1 162.83(3) . . . . ? S3 Cd3 S2 Cd1 25.85(5) . . . . ? S4 Cd3 S2 Cd1 -77.87(3) . . . . ? S9 Cd3 S3 C13 -48.44(13) . . . . ? S2 Cd3 S3 C13 85.24(13) . . . . ? S4 Cd3 S3 C13 -177.63(13) . . . . ? S9 Cd3 S3 Cd2 -159.77(3) . . . . ? S2 Cd3 S3 Cd2 -26.08(5) . . . . ? S4 Cd3 S3 Cd2 71.05(3) . . . . ? S8 Cd2 S3 C13 37.69(13) . . . . ? S6 Cd2 S3 C13 174.62(13) . . . . ? S1 Cd2 S3 C13 -71.59(13) . . . . ? S8 Cd2 S3 Cd3 149.47(3) . . . . ? S6 Cd2 S3 Cd3 -73.60(3) . . . . ? S1 Cd2 S3 Cd3 40.20(4) . . . . ? S10 Cd4 S4 C19 53.39(14) . . . . ? S5 Cd4 S4 C19 177.28(14) . . . . ? S6 Cd4 S4 C19 -73.75(14) . . . . ? S10 Cd4 S4 Cd3 170.45(3) . . . . ? S5 Cd4 S4 Cd3 -65.66(3) . . . . ? S6 Cd4 S4 Cd3 43.31(4) . . . . ? S9 Cd3 S4 C19 -61.54(14) . . . . ? S3 Cd3 S4 C19 64.46(14) . . . . ? S2 Cd3 S4 C19 -166.81(14) . . . . ? S9 Cd3 S4 Cd4 178.74(3) . . . . ? S3 Cd3 S4 Cd4 -55.26(4) . . . . ? S2 Cd3 S4 Cd4 73.47(3) . . . . ? S7 Cd1 S5 C25 -61.25(12) . . . . ? S1 Cd1 S5 C25 169.62(12) . . . . ? S2 Cd1 S5 C25 60.02(12) . . . . ? S7 Cd1 S5 Cd4 -171.18(3) . . . . ? S1 Cd1 S5 Cd4 59.69(3) . . . . ? S2 Cd1 S5 Cd4 -49.91(3) . . . . ? S10 Cd4 S5 C25 52.64(12) . . . . ? S4 Cd4 S5 C25 -66.31(12) . . . . ? S6 Cd4 S5 C25 173.43(12) . . . . ? S10 Cd4 S5 Cd1 166.02(3) . . . . ? S4 Cd4 S5 Cd1 47.07(3) . . . . ? S6 Cd4 S5 Cd1 -73.19(3) . . . . ? S8 Cd2 S6 C31 73.19(14) . . . . ? S3 Cd2 S6 C31 -57.46(14) . . . . ? S1 Cd2 S6 C31 -170.40(14) . . . . ? S8 Cd2 S6 Cd4 -175.64(3) . . . . ? S3 Cd2 S6 Cd4 53.71(3) . . . . ? S1 Cd2 S6 Cd4 -59.22(3) . . . . ? S10 Cd4 S6 C31 -47.84(11) . . . . ? S4 Cd4 S6 C31 75.82(11) . . . . ? S5 Cd4 S6 C31 -169.53(11) . . . . ? S10 Cd4 S6 Cd2 -164.69(3) . . . . ? S4 Cd4 S6 Cd2 -41.04(4) . . . . ? S5 Cd4 S6 Cd2 73.62(3) . . . . ? S1 Cd1 S7 C37 -19.39(12) . . . . ? S2 Cd1 S7 C37 99.63(12) . . . . ? S5 Cd1 S7 C37 -143.38(12) . . . . ? S6 Cd2 S8 C43 -104.39(12) . . . . ? S3 Cd2 S8 C43 24.18(13) . . . . ? S1 Cd2 S8 C43 136.38(12) . . . . ? S3 Cd3 S9 C49 -155.74(14) . . . . ? S2 Cd3 S9 C49 60.16(14) . . . . ? S4 Cd3 S9 C49 -35.70(14) . . . . ? S4 Cd4 S10 C55 170.95(13) . . . . ? S5 Cd4 S10 C55 51.27(13) . . . . ? S6 Cd4 S10 C55 -60.81(13) . . . . ? Cd1 S1 C1 C6 132.0(2) . . . . ? Cd2 S1 C1 C6 -100.1(3) . . . . ? Cd1 S1 C1 C2 -45.6(3) . . . . ? Cd2 S1 C1 C2 82.4(3) . . . . ? C6 C1 C2 C3 1.7(5) . . . . ? S1 C1 C2 C3 179.2(2) . . . . ? C1 C2 C3 C4 -3.6(5) . . . . ? C2 C3 C4 C5 3.7(5) . . . . ? C2 C3 C4 N1 -177.9(3) . . . . ? C3 C4 C5 C6 -1.8(5) . . . . ? N1 C4 C5 C6 179.7(3) . . . . ? C2 C1 C6 C5 0.1(5) . . . . ? S1 C1 C6 C5 -177.4(3) . . . . ? C4 C5 C6 C1 -0.2(5) . . . . ? Cd1 S2 C7 C12 86.7(3) . . . . ? Cd3 S2 C7 C12 -156.3(3) . . . . ? Cd1 S2 C7 C8 -89.9(3) . . . . ? Cd3 S2 C7 C8 27.1(3) . . . . ? C12 C7 C8 C9 -0.6(6) . . . . ? S2 C7 C8 C9 176.0(3) . . . . ? C7 C8 C9 C10 1.4(6) . . . . ? C8 C9 C10 C11 -1.4(6) . . . . ? C8 C9 C10 N2 -178.5(3) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? N2 C10 C11 C12 177.7(3) . . . . ? C8 C7 C12 C11 -0.1(6) . . . . ? S2 C7 C12 C11 -176.8(3) . . . . ? C10 C11 C12 C7 0.1(6) . . . . ? Cd3 S3 C13 C18 -72.4(3) . . . . ? Cd2 S3 C13 C18 42.6(4) . . . . ? Cd3 S3 C13 C14 104.9(3) . . . . ? Cd2 S3 C13 C14 -140.1(3) . . . . ? C18 C13 C14 C15 1.7(6) . . . . ? S3 C13 C14 C15 -175.6(3) . . . . ? C13 C14 C15 C16 -2.5(6) . . . . ? C14 C15 C16 C17 3.0(6) . . . . ? C14 C15 C16 N3 176.8(3) . . . . ? C15 C16 C17 C18 -2.7(6) . . . . ? N3 C16 C17 C18 -176.2(3) . . . . ? C14 C13 C18 C17 -1.4(6) . . . . ? S3 C13 C18 C17 175.8(3) . . . . ? C16 C17 C18 C13 1.9(6) . . . . ? Cd4 S4 C19 C20 2.7(4) . . . . ? Cd3 S4 C19 C20 -121.1(3) . . . . ? Cd4 S4 C19 C24 -172.6(3) . . . . ? Cd3 S4 C19 C24 63.6(3) . . . . ? C24 C19 C20 C21 0.0(6) . . . . ? S4 C19 C20 C21 -175.0(3) . . . . ? C19 C20 C21 C22 0.0(5) . . . . ? C20 C21 C22 C23 0.0(6) . . . . ? C20 C21 C22 N4 178.7(3) . . . . ? C21 C22 C23 C24 0.0(6) . . . . ? N4 C22 C23 C24 -178.7(3) . . . . ? C22 C23 C24 C19 0.0(6) . . . . ? C20 C19 C24 C23 0.0(6) . . . . ? S4 C19 C24 C23 175.6(3) . . . . ? Cd1 S5 C25 C30 178.4(2) . . . . ? Cd4 S5 C25 C30 -65.5(3) . . . . ? Cd1 S5 C25 C26 3.9(3) . . . . ? Cd4 S5 C25 C26 119.9(3) . . . . ? C30 C25 C26 C27 1.6(5) . . . . ? S5 C25 C26 C27 176.1(3) . . . . ? C25 C26 C27 C28 -0.3(6) . . . . ? C26 C27 C28 C29 -0.7(5) . . . . ? C26 C27 C28 N5 -178.2(3) . . . . ? C27 C28 C29 C30 0.3(5) . . . . ? N5 C28 C29 C30 178.0(3) . . . . ? C28 C29 C30 C25 1.0(5) . . . . ? C26 C25 C30 C29 -2.0(5) . . . . ? S5 C25 C30 C29 -176.7(3) . . . . ? Cd2 S6 C31 C32 -168.7(3) . . . . ? Cd4 S6 C31 C32 73.7(3) . . . . ? Cd2 S6 C31 C36 10.2(4) . . . . ? Cd4 S6 C31 C36 -107.4(3) . . . . ? C36 C31 C32 C33 0.0(5) . . . . ? S6 C31 C32 C33 178.9(3) . . . . ? C31 C32 C33 C34 0.0(5) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C32 C33 C34 N6 -179.3(3) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? N6 C34 C35 C36 179.2(3) . . . . ? C34 C35 C36 C31 0.0(6) . . . . ? C32 C31 C36 C35 0.0(6) . . . . ? S6 C31 C36 C35 -178.9(3) . . . . ? Cd1 S7 C37 C42 155.7(2) . . . . ? Cd1 S7 C37 C38 -29.0(3) . . . . ? C42 C37 C38 C39 -1.0(6) . . . . ? S7 C37 C38 C39 -176.1(3) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C38 C39 C40 C41 0.4(6) . . . . ? C38 C39 C40 N7 -177.1(3) . . . . ? C39 C40 C41 C42 0.9(5) . . . . ? N7 C40 C41 C42 178.4(3) . . . . ? C38 C37 C42 C41 2.3(5) . . . . ? S7 C37 C42 C41 178.0(3) . . . . ? C40 C41 C42 C37 -2.3(5) . . . . ? Cd2 S8 C43 C48 -125.1(3) . . . . ? Cd2 S8 C43 C44 64.0(3) . . . . ? C48 C43 C44 C45 2.0(6) . . . . ? S8 C43 C44 C45 172.6(3) . . . . ? C43 C44 C45 C46 -1.0(6) . . . . ? C44 C45 C46 C47 1.1(6) . . . . ? C44 C45 C46 N8 -178.5(3) . . . . ? C45 C46 C47 C48 -2.1(6) . . . . ? N8 C46 C47 C48 177.6(3) . . . . ? C44 C43 C48 C47 -3.0(5) . . . . ? S8 C43 C48 C47 -173.2(3) . . . . ? C46 C47 C48 C43 3.0(5) . . . . ? Cd3 S9 C49 C50 129.8(3) . . . . ? Cd3 S9 C49 C54 -50.3(4) . . . . ? C54 C49 C50 C51 0.0(6) . . . . ? S9 C49 C50 C51 179.9(3) . . . . ? C49 C50 C51 C52 0.0(6) . . . . ? C50 C51 C52 C53 0.0(7) . . . . ? C50 C51 C52 N9 -177.9(4) . . . . ? C51 C52 C53 C54 0.0(7) . . . . ? N9 C52 C53 C54 178.1(4) . . . . ? C52 C53 C54 C49 0.0(7) . . . . ? C50 C49 C54 C53 0.0(6) . . . . ? S9 C49 C54 C53 -179.9(3) . . . . ? Cd4 S10 C55 C60 174.9(3) . . . . ? Cd4 S10 C55 C56 -7.9(3) . . . . ? C60 C55 C56 C57 -2.1(6) . . . . ? S10 C55 C56 C57 -179.3(3) . . . . ? C55 C56 C57 C58 1.9(5) . . . . ? C56 C57 C58 C59 -0.5(5) . . . . ? C56 C57 C58 N10 178.7(3) . . . . ? C57 C58 C59 C60 -0.7(5) . . . . ? N10 C58 C59 C60 -179.9(3) . . . . ? C56 C55 C60 C59 0.9(6) . . . . ? S10 C55 C60 C59 178.2(3) . . . . ? C58 C59 C60 C55 0.6(6) . . . . ? C3 C4 N1 C61 21.6(3) . . . . ? C5 C4 N1 C61 -159.9(2) . . . . ? C3 C4 N1 C63 -104.4(3) . . . . ? C5 C4 N1 C63 74.1(3) . . . . ? C3 C4 N1 C62 141.4(3) . . . . ? C5 C4 N1 C62 -40.1(3) . . . . ? C11 C10 N2 C65 77.9(3) . . . . ? C9 C10 N2 C65 -105.1(3) . . . . ? C11 C10 N2 C66 -160.6(3) . . . . ? C9 C10 N2 C66 16.4(4) . . . . ? C11 C10 N2 C64 -43.0(4) . . . . ? C9 C10 N2 C64 134.0(3) . . . . ? C17 C16 N3 C68 173.0(3) . . . . ? C15 C16 N3 C68 -0.6(4) . . . . ? C17 C16 N3 C69 -66.5(4) . . . . ? C15 C16 N3 C69 119.9(3) . . . . ? C17 C16 N3 C67 32.8(4) . . . . ? C15 C16 N3 C67 -140.8(3) . . . . ? C23 C22 N4 C70 76.9(3) . . . . ? C21 C22 N4 C70 -101.9(3) . . . . ? C23 C22 N4 C72 -161.4(3) . . . . ? C21 C22 N4 C72 19.9(4) . . . . ? C23 C22 N4 C71 -43.4(4) . . . . ? C21 C22 N4 C71 137.9(3) . . . . ? C27 C28 N5 C74 -119.8(3) . . . . ? C29 C28 N5 C74 62.7(3) . . . . ? C27 C28 N5 C75 4.5(4) . . . . ? C29 C28 N5 C75 -173.0(2) . . . . ? C27 C28 N5 C73 116.6(3) . . . . ? C29 C28 N5 C73 -61.0(3) . . . . ? C33 C34 N6 C76 -86.2(3) . . . . ? C35 C34 N6 C76 94.5(4) . . . . ? C33 C34 N6 C77 162.2(3) . . . . ? C35 C34 N6 C77 -17.1(4) . . . . ? C33 C34 N6 C78 54.9(3) . . . . ? C35 C34 N6 C78 -124.4(3) . . . . ? C39 C40 N7 C79 69.6(4) . . . . ? C41 C40 N7 C79 -107.8(3) . . . . ? C39 C40 N7 C81 -167.0(3) . . . . ? C41 C40 N7 C81 15.6(4) . . . . ? C39 C40 N7 C80 -52.8(4) . . . . ? C41 C40 N7 C80 129.8(3) . . . . ? C47 C46 N8 C83 -44.5(3) . . . . ? C45 C46 N8 C83 135.1(3) . . . . ? C47 C46 N8 C82 79.3(3) . . . . ? C45 C46 N8 C82 -101.1(3) . . . . ? C47 C46 N8 C84 -161.8(3) . . . . ? C45 C46 N8 C84 17.9(4) . . . . ? C51 C52 N9 C85 8.7(5) . . . . ? C53 C52 N9 C85 -169.3(3) . . . . ? C51 C52 N9 C87 -108.0(4) . . . . ? C53 C52 N9 C87 74.0(4) . . . . ? C51 C52 N9 C86 130.4(4) . . . . ? C53 C52 N9 C86 -47.7(4) . . . . ? C57 C58 N10 C88 48.7(3) . . . . ? C59 C58 N10 C88 -132.1(3) . . . . ? C57 C58 N10 C89 171.7(2) . . . . ? C59 C58 N10 C89 -9.1(4) . . . . ? C57 C58 N10 C90 -72.5(3) . . . . ? C59 C58 N10 C90 106.7(3) . . . . ? O1 C91 N11 C92 4.7(4) . . . . ? O1 C91 N11 C93 172.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.053 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.080 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 865707' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 N4 S4 Zn, 2(F6 P), H2 O' _chemical_formula_sum 'C36 H54 F12 N4 O P2 S4 Zn' _chemical_formula_weight 1042.44 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' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 13.866(3) _cell_length_b 35.254(3) _cell_length_c 10.231(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5001.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4725 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.12 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan' _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rikagu Mercury' _diffrn_measurement_method \w _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 47895 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9492 _reflns_number_gt 8021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The U~ij~ values of Zn1 and S1 atoms were restrained by 'DELU' instruction. The sum of the occupancies of the multi-component disordered water molecule was restrained by the use of free variables. Linear combinations of these free variables were restrained by 'SUMP' instruction. ; _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^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.079(12) _refine_ls_number_reflns 9492 _refine_ls_number_parameters 551 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1655(3) 0.09749(14) 0.0164(5) 0.0379(11) Uani 1 1 d . . . C2 C 0.2253(4) 0.06698(15) -0.0074(5) 0.0413(12) Uani 1 1 d . . . H2 H 0.2548 0.0548 0.0626 0.050 Uiso 1 1 calc R . . C3 C 0.2422(4) 0.05416(15) -0.1324(5) 0.0401(11) Uani 1 1 d . . . H3 H 0.2858 0.0346 -0.1469 0.048 Uiso 1 1 calc R . . C4 C 0.1946(3) 0.07033(14) -0.2351(5) 0.0387(11) Uani 1 1 d . . . C5 C 0.1278(3) 0.10043(14) -0.2152(5) 0.0396(12) Uani 1 1 d . . . H5 H 0.0933 0.1114 -0.2834 0.047 Uiso 1 1 calc R . . C6 C 0.1176(4) 0.11241(14) -0.0832(5) 0.0442(12) Uani 1 1 d . . . H6 H 0.0746 0.1320 -0.0656 0.053 Uiso 1 1 calc R . . C7 C 0.2869(4) 0.07667(15) -0.4553(5) 0.0467(13) Uani 1 1 d . . . H7A H 0.3350 0.0586 -0.4813 0.070 Uiso 1 1 calc R . . H7B H 0.3169 0.0968 -0.4069 0.070 Uiso 1 1 calc R . . H7C H 0.2562 0.0869 -0.5316 0.070 Uiso 1 1 calc R . . C8 C 0.2344(3) 0.01630(13) -0.3719(5) 0.0363(11) Uani 1 1 d . . . H8A H 0.3029 0.0124 -0.3752 0.055 Uiso 1 1 calc R . . H8B H 0.2049 0.0048 -0.4469 0.055 Uiso 1 1 calc R . . H8C H 0.2090 0.0050 -0.2938 0.055 Uiso 1 1 calc R . . C9 C 0.1226(3) 0.06199(13) -0.4502(5) 0.0392(11) Uani 1 1 d . . . H9B H 0.1176 0.0877 -0.4807 0.047 Uiso 1 1 calc R . . H9C H 0.0679 0.0561 -0.3965 0.047 Uiso 1 1 calc R . . H9A H 0.1244 0.0451 -0.5237 0.047 Uiso 1 1 calc R . . C10 C 0.0701(2) 0.17953(7) 0.4495(3) 0.0342(10) Uani 1 1 d G . . C11 C 0.0909(2) 0.19847(9) 0.3338(2) 0.0418(12) Uani 1 1 d G . . H11 H 0.0601 0.1915 0.2567 0.050 Uiso 1 1 calc R . . C12 C 0.1578(2) 0.22785(8) 0.3332(2) 0.0402(11) Uani 1 1 d G . . H12 H 0.1717 0.2405 0.2558 0.048 Uiso 1 1 calc R . . C13 C 0.2038(2) 0.23829(7) 0.4484(3) 0.0373(11) Uani 1 1 d G . . C14 C 0.1830(2) 0.21935(9) 0.5642(3) 0.0412(12) Uani 1 1 d G . . H14 H 0.2138 0.2263 0.6413 0.049 Uiso 1 1 calc R . . C15 C 0.1161(2) 0.18997(8) 0.5647(2) 0.0456(13) Uani 1 1 d G . . H15 H 0.1022 0.1773 0.6422 0.055 Uiso 1 1 calc R . . C16 C 0.3662(4) 0.25449(15) 0.3778(5) 0.0437(12) Uani 1 1 d . . . H16A H 0.4217 0.2675 0.4113 0.066 Uiso 1 1 calc R . . H16B H 0.3615 0.2586 0.2853 0.066 Uiso 1 1 calc R . . H16C H 0.3723 0.2278 0.3947 0.066 Uiso 1 1 calc R . . C17 C 0.2418(4) 0.30079(16) 0.3639(5) 0.0467(13) Uani 1 1 d . . . H17A H 0.1727 0.3015 0.3691 0.070 Uiso 1 1 calc R . . H17B H 0.2610 0.2974 0.2745 0.070 Uiso 1 1 calc R . . H17C H 0.2678 0.3242 0.3966 0.070 Uiso 1 1 calc R . . C18 C 0.3024(3) 0.28260(14) 0.5761(5) 0.0378(11) Uani 1 1 d . . . H18A H 0.3428 0.2642 0.6187 0.057 Uiso 1 1 calc R . . H18B H 0.2442 0.2859 0.6256 0.057 Uiso 1 1 calc R . . H18C H 0.3359 0.3064 0.5705 0.057 Uiso 1 1 calc R . . C19 C 0.0224(2) 0.01249(7) 0.2892(3) 0.0320(10) Uani 1 1 d G . . C20 C 0.0873(2) 0.01545(7) 0.1862(3) 0.0425(12) Uani 1 1 d G . . H20 H 0.0865 0.0367 0.1325 0.051 Uiso 1 1 calc R . . C21 C 0.1535(2) -0.01342(8) 0.1633(3) 0.0441(12) Uani 1 1 d G . . H21 H 0.1969 -0.0114 0.0943 0.053 Uiso 1 1 calc R . . C22 C 0.1547(2) -0.04525(7) 0.2434(3) 0.0390(11) Uani 1 1 d G . . C23 C 0.0899(2) -0.04820(7) 0.3465(3) 0.0370(11) Uani 1 1 d G . . H23 H 0.0907 -0.0695 0.4001 0.044 Uiso 1 1 calc R . . C24 C 0.0237(2) -0.01933(8) 0.3694(3) 0.0431(12) Uani 1 1 d G . . H24 H -0.0197 -0.0213 0.4384 0.052 Uiso 1 1 calc R . . C25 C 0.2651(4) -0.07283(14) 0.0890(5) 0.0422(12) Uani 1 1 d . . . H25A H 0.3029 -0.0502 0.0796 0.063 Uiso 1 1 calc R . . H25B H 0.2111 -0.0718 0.0305 0.063 Uiso 1 1 calc R . . H25C H 0.3041 -0.0945 0.0686 0.063 Uiso 1 1 calc R . . C26 C 0.1888(3) -0.11478(12) 0.2463(5) 0.0396(10) Uani 1 1 d . . . H26A H 0.2169 -0.1318 0.1836 0.059 Uiso 1 1 calc R . . H26B H 0.1202 -0.1141 0.2343 0.059 Uiso 1 1 calc R . . H26C H 0.2032 -0.1235 0.3330 0.059 Uiso 1 1 calc R . . C27 C 0.3109(4) -0.07051(14) 0.3154(6) 0.0468(13) Uani 1 1 d . . . H27A H 0.3587 -0.0896 0.2984 0.070 Uiso 1 1 calc R . . H27B H 0.2893 -0.0726 0.4042 0.070 Uiso 1 1 calc R . . H27C H 0.3384 -0.0459 0.3014 0.070 Uiso 1 1 calc R . . C28 C -0.2216(3) 0.13585(12) 0.1221(5) 0.0327(10) Uani 1 1 d . . . C29 C -0.2609(3) 0.10711(13) 0.2012(5) 0.0357(10) Uani 1 1 d . . . H29 H -0.2205 0.0900 0.2433 0.043 Uiso 1 1 calc R . . C30 C -0.3608(3) 0.10440(14) 0.2161(5) 0.0394(12) Uani 1 1 d . . . H30 H -0.3872 0.0851 0.2669 0.047 Uiso 1 1 calc R . . C31 C -0.4206(3) 0.13052(13) 0.1551(5) 0.0362(11) Uani 1 1 d . . . C32 C -0.3809(3) 0.15672(14) 0.0755(5) 0.0392(11) Uani 1 1 d . . . H32 H -0.4214 0.1728 0.0287 0.047 Uiso 1 1 calc R . . C33 C -0.2822(3) 0.16066(14) 0.0605(5) 0.0370(11) Uani 1 1 d . . . H33 H -0.2573 0.1800 0.0090 0.044 Uiso 1 1 calc R . . C34 C -0.5574(4) 0.09449(14) 0.2530(6) 0.0458(11) Uani 1 1 d . . . H34A H -0.6254 0.0901 0.2431 0.069 Uiso 1 1 calc R . . H34B H -0.5434 0.1002 0.3428 0.069 Uiso 1 1 calc R . . H34C H -0.5226 0.0722 0.2273 0.069 Uiso 1 1 calc R . . C35 C -0.5719(4) 0.12502(14) 0.0391(5) 0.0425(12) Uani 1 1 d . . . H35A H -0.5289 0.1122 -0.0198 0.064 Uiso 1 1 calc R . . H35B H -0.5840 0.1502 0.0078 0.064 Uiso 1 1 calc R . . H35C H -0.6316 0.1113 0.0442 0.064 Uiso 1 1 calc R . . C36 C -0.5620(4) 0.16240(14) 0.2361(5) 0.0436(12) Uani 1 1 d . . . H36A H -0.5514 0.1838 0.1799 0.065 Uiso 1 1 calc R . . H36B H -0.5269 0.1658 0.3161 0.065 Uiso 1 1 calc R . . H36C H -0.6296 0.1602 0.2550 0.065 Uiso 1 1 calc R . . F1 F 0.4739(2) 1.03653(10) 0.8739(3) 0.0572(8) Uani 1 1 d . . . F2 F 0.5587(2) 1.02150(9) 1.0484(3) 0.0590(9) Uani 1 1 d . . . F3 F 0.4988(2) 0.96203(9) 1.0415(3) 0.0577(9) Uani 1 1 d . . . F4 F 0.3985(2) 1.01077(9) 1.0476(3) 0.0526(8) Uani 1 1 d . . . F5 F 0.4116(2) 0.97864(10) 0.8676(3) 0.0594(9) Uani 1 1 d . . . F6 F 0.5761(2) 0.98643(10) 0.8696(3) 0.0569(8) Uani 1 1 d . . . F7 F 0.5483(2) 0.80721(9) 0.2633(4) 0.0610(8) Uani 1 1 d . . . F8 F 0.5966(2) 0.83484(10) 0.0846(4) 0.0625(9) Uani 1 1 d . . . F9 F 0.4462(2) 0.85429(10) 0.0537(3) 0.0604(9) Uani 1 1 d . . . F10 F 0.4793(2) 0.79542(9) 0.0783(4) 0.0597(9) Uani 1 1 d . . . F11 F 0.4004(2) 0.82813(9) 0.2234(3) 0.0593(9) Uani 1 1 d . . . F12 F 0.5213(2) 0.86719(9) 0.2366(4) 0.0590(8) Uani 1 1 d . . . O1A O 0.4641(6) 0.2626(2) 0.9719(8) 0.036(3) Uani 0.360(9) 1 d P . . H1A H 0.5139 0.2517 1.0021 0.043 Uiso 0.360(9) 1 d PR . . H1B H 0.4772 0.2857 0.9553 0.043 Uiso 0.360(9) 1 d PR . . O1B O 0.2362(11) 0.2118(3) 0.9631(13) 0.068(5) Uani 0.331(9) 1 d P . . H1C H 0.2455 0.1888 0.9856 0.081 Uiso 0.331(9) 1 d PR . . H1D H 0.1957 0.2219 1.0147 0.081 Uiso 0.331(9) 1 d PR . . O1C O 0.3331(8) 0.2637(4) 0.8676(11) 0.051(4) Uani 0.309(9) 1 d P . . H1E H 0.3822 0.2774 0.8518 0.061 Uiso 0.309(9) 1 d PR . . H1F H 0.3449 0.2492 0.9318 0.061 Uiso 0.309(9) 1 d PR . . N1 N 0.2134(3) 0.05755(11) -0.3716(4) 0.0349(9) Uani 1 1 d . . . N2 N 0.2782(3) 0.26913(12) 0.4427(4) 0.0399(9) Uani 1 1 d . . . N3 N 0.2295(3) -0.07587(11) 0.2275(4) 0.0339(9) Uani 1 1 d . . . N4 N -0.5278(3) 0.12692(11) 0.1693(4) 0.0350(9) Uani 1 1 d . . . P1 P 0.48631(10) 0.99930(4) 0.95788(14) 0.0434(3) Uani 1 1 d . . . P2 P 0.50004(10) 0.83067(4) 0.15687(14) 0.0390(3) Uani 1 1 d . . . S1 S 0.15369(7) 0.11511(3) 0.17867(11) 0.0286(2) Uani 1 1 d U . . S2 S -0.01515(7) 0.14116(3) 0.45183(10) 0.0234(2) Uani 1 1 d . . . S3 S -0.06373(7) 0.04799(3) 0.31579(10) 0.0235(2) Uani 1 1 d . . . S4 S -0.09669(7) 0.13896(3) 0.09056(10) 0.0229(2) Uani 1 1 d . . . Zn1 Zn -0.00495(3) 0.107941(12) 0.25040(5) 0.02296(11) Uani 1 1 d U . . 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 C1 0.035(2) 0.040(3) 0.039(3) -0.015(2) 0.008(2) 0.010(2) C2 0.039(3) 0.046(3) 0.039(3) -0.021(2) 0.003(2) 0.013(2) C3 0.047(3) 0.046(3) 0.028(2) -0.016(2) 0.000(2) 0.004(2) C4 0.041(2) 0.041(3) 0.035(3) -0.004(2) 0.010(2) -0.002(2) C5 0.036(2) 0.046(3) 0.036(3) 0.006(2) 0.020(2) 0.007(2) C6 0.063(3) 0.034(3) 0.036(3) -0.006(2) 0.003(2) 0.007(2) C7 0.046(3) 0.045(3) 0.049(3) -0.009(2) 0.015(3) -0.021(2) C8 0.034(2) 0.034(2) 0.040(3) -0.005(2) 0.000(2) -0.001(2) C9 0.033(2) 0.033(2) 0.052(3) -0.020(2) 0.001(2) 0.005(2) C10 0.032(2) 0.035(2) 0.035(2) -0.018(2) 0.007(2) -0.0070(19) C11 0.047(3) 0.036(2) 0.043(3) -0.011(2) 0.005(2) -0.003(2) C12 0.039(3) 0.046(3) 0.036(3) -0.004(2) 0.002(2) -0.008(2) C13 0.037(2) 0.034(2) 0.041(3) -0.008(2) -0.006(2) 0.0090(19) C14 0.028(2) 0.043(3) 0.053(3) 0.004(2) -0.023(2) -0.008(2) C15 0.042(3) 0.049(3) 0.047(3) -0.002(2) -0.010(2) -0.018(2) C16 0.045(3) 0.045(3) 0.040(3) -0.008(2) -0.007(2) -0.009(2) C17 0.047(3) 0.058(3) 0.036(3) 0.013(2) 0.011(2) 0.001(3) C18 0.027(2) 0.042(3) 0.044(3) -0.005(2) -0.001(2) -0.0058(19) C19 0.030(2) 0.028(2) 0.038(3) -0.0126(18) -0.0038(18) 0.0006(18) C20 0.036(3) 0.047(3) 0.044(3) 0.008(2) 0.007(2) 0.018(2) C21 0.036(3) 0.047(3) 0.049(3) 0.015(2) 0.021(2) 0.019(2) C22 0.034(2) 0.039(2) 0.044(3) 0.009(2) 0.006(2) 0.0170(19) C23 0.030(2) 0.035(2) 0.045(3) 0.008(2) 0.013(2) -0.0030(19) C24 0.059(3) 0.037(3) 0.033(3) -0.011(2) 0.012(2) 0.013(2) C25 0.042(3) 0.048(3) 0.036(3) 0.002(2) 0.008(2) 0.024(2) C26 0.042(2) 0.039(3) 0.038(2) -0.015(2) 0.008(2) 0.008(2) C27 0.051(3) 0.036(3) 0.053(3) -0.025(2) -0.015(3) 0.022(2) C28 0.024(2) 0.027(2) 0.047(3) 0.0023(19) -0.005(2) -0.0078(18) C29 0.039(3) 0.035(2) 0.033(2) 0.0058(19) 0.011(2) -0.001(2) C30 0.032(2) 0.043(3) 0.044(3) 0.011(2) -0.004(2) -0.009(2) C31 0.035(2) 0.032(2) 0.042(3) -0.003(2) -0.001(2) -0.0083(19) C32 0.032(2) 0.041(3) 0.045(3) 0.012(2) 0.001(2) 0.003(2) C33 0.036(2) 0.043(3) 0.032(3) 0.007(2) 0.006(2) 0.014(2) C34 0.043(3) 0.044(3) 0.050(3) 0.004(3) 0.011(3) -0.004(2) C35 0.043(3) 0.037(2) 0.047(3) -0.020(2) -0.013(2) 0.012(2) C36 0.045(3) 0.041(3) 0.045(3) -0.016(2) 0.002(3) 0.002(2) F1 0.057(2) 0.0581(19) 0.057(2) 0.0114(17) -0.0020(16) 0.0036(16) F2 0.059(2) 0.0538(19) 0.064(2) -0.0089(16) -0.0193(17) 0.0127(16) F3 0.069(2) 0.0494(18) 0.054(2) 0.0064(16) 0.0178(17) 0.0126(15) F4 0.0571(19) 0.0569(18) 0.0438(17) -0.0077(14) 0.0007(15) 0.0099(15) F5 0.055(2) 0.063(2) 0.060(2) -0.0174(17) 0.0022(17) -0.0034(16) F6 0.0551(19) 0.059(2) 0.056(2) 0.0042(16) 0.0145(16) 0.0039(16) F7 0.0578(18) 0.0570(18) 0.068(2) 0.0109(18) -0.0164(18) -0.0003(15) F8 0.0481(18) 0.065(2) 0.074(2) -0.0035(19) 0.0126(17) -0.0047(16) F9 0.065(2) 0.065(2) 0.052(2) 0.0045(16) -0.0117(17) 0.0070(17) F10 0.063(2) 0.0486(18) 0.068(2) -0.0232(17) -0.0035(17) -0.0041(15) F11 0.0495(17) 0.063(2) 0.065(2) -0.0035(17) 0.0123(16) 0.0076(15) F12 0.070(2) 0.0495(17) 0.057(2) -0.0180(17) -0.0020(18) -0.0032(15) O1A 0.036(5) 0.038(5) 0.033(5) 0.011(4) 0.004(4) 0.019(4) O1B 0.101(11) 0.033(6) 0.068(9) -0.002(6) -0.021(8) -0.019(6) O1C 0.025(6) 0.082(9) 0.045(7) -0.016(6) -0.001(5) 0.006(6) N1 0.032(2) 0.041(2) 0.033(2) 0.0083(17) 0.0106(17) 0.0023(17) N2 0.041(2) 0.042(2) 0.037(2) -0.0082(19) -0.0091(19) -0.0031(18) N3 0.0353(19) 0.035(2) 0.031(2) 0.0025(16) -0.0006(17) 0.0131(16) N4 0.032(2) 0.040(2) 0.033(2) -0.0046(18) 0.0097(17) -0.0044(16) P1 0.0479(8) 0.0428(7) 0.0396(7) -0.0062(6) -0.0038(6) 0.0123(6) P2 0.0431(7) 0.0340(6) 0.0401(7) -0.0111(5) -0.0005(6) 0.0078(5) S1 0.0240(5) 0.0293(5) 0.0324(5) -0.0150(5) 0.0063(4) -0.0043(4) S2 0.0223(5) 0.0234(5) 0.0244(5) -0.0098(4) 0.0008(4) -0.0003(4) S3 0.0250(5) 0.0228(5) 0.0226(5) -0.0105(4) 0.0008(4) -0.0003(4) S4 0.0245(5) 0.0216(4) 0.0227(5) -0.0097(4) 0.0010(4) -0.0013(4) Zn1 0.0235(2) 0.0221(2) 0.0232(2) -0.0104(2) 0.0010(2) -0.00018(18) _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 C1 C6 1.325(7) . ? C1 C2 1.379(7) . ? C1 S1 1.780(5) . ? C2 C3 1.377(7) . ? C2 H2 0.9300 . ? C3 C4 1.365(7) . ? C3 H3 0.9300 . ? C4 C5 1.423(7) . ? C4 N1 1.490(6) . ? C5 C6 1.422(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.492(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.483(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N1 1.502(6) . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C9 H9A 0.9600 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C10 S2 1.796(2) . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 N2 1.500(4) . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N2 1.481(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N2 1.467(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N2 1.484(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 S3 1.752(2) . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 N3 1.506(4) . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N3 1.504(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N3 1.496(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N3 1.455(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C33 1.366(6) . ? C28 C29 1.406(6) . ? C28 S4 1.766(4) . ? C29 C30 1.398(6) . ? C29 H29 0.9300 . ? C30 C31 1.388(7) . ? C30 H30 0.9300 . ? C31 C32 1.350(7) . ? C31 N4 1.498(6) . ? C32 C33 1.384(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N4 1.487(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N4 1.467(6) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 N4 1.502(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? F1 P1 1.578(4) . ? F2 P1 1.575(4) . ? F3 P1 1.578(4) . ? F4 P1 1.578(3) . ? F5 P1 1.567(4) . ? F6 P1 1.603(3) . ? F7 P2 1.523(4) . ? F8 P2 1.536(4) . ? F9 P2 1.538(3) . ? F10 P2 1.508(3) . ? F11 P2 1.543(3) . ? F12 P2 1.553(3) . ? O1A H1A 0.8499 . ? O1A H1B 0.8500 . ? O1B H1C 0.8498 . ? O1B H1D 0.8500 . ? O1C H1E 0.8501 . ? O1C H1F 0.8500 . ? S1 Zn1 2.3326(12) . ? S2 Zn1 2.3746(11) . ? S3 Zn1 2.3618(11) . ? S4 Zn1 2.3428(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.4(4) . . ? C6 C1 S1 122.2(4) . . ? C2 C1 S1 119.5(4) . . ? C3 C2 C1 121.5(5) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.1(4) . . ? C3 C4 N1 120.7(4) . . ? C5 C4 N1 118.3(4) . . ? C6 C5 C4 114.9(5) . . ? C6 C5 H5 122.5 . . ? C4 C5 H5 122.5 . . ? C1 C6 C5 124.3(5) . . ? C1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? C11 C10 C15 120.0 . . ? C11 C10 S2 120.64(17) . . ? C15 C10 S2 119.36(17) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 N2 118.3(2) . . ? C14 C13 N2 121.6(2) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.0 . . ? C20 C19 S3 120.37(16) . . ? C24 C19 S3 119.60(16) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 N3 118.3(2) . . ? C21 C22 N3 121.6(2) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 119.2(4) . . ? C33 C28 S4 118.6(4) . . ? C29 C28 S4 122.0(4) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 119.8(4) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 118.8(4) . . ? C32 C31 N4 121.4(4) . . ? C30 C31 N4 119.5(4) . . ? C31 C32 C33 122.6(5) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C28 C33 C32 119.5(4) . . ? C28 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? N4 C34 H34A 109.5 . . ? N4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? H1A O1A H1B 109.5 . . ? H1C O1B H1D 109.5 . . ? H1E O1C H1F 109.5 . . ? C8 N1 C4 109.4(4) . . ? C8 N1 C7 107.9(4) . . ? C4 N1 C7 121.4(4) . . ? C8 N1 C9 105.4(4) . . ? C4 N1 C9 108.9(4) . . ? C7 N1 C9 102.6(4) . . ? C17 N2 C16 107.6(4) . . ? C17 N2 C18 109.9(4) . . ? C16 N2 C18 109.8(4) . . ? C17 N2 C13 109.6(4) . . ? C16 N2 C13 109.3(3) . . ? C18 N2 C13 110.6(4) . . ? C27 N3 C26 109.4(4) . . ? C27 N3 C25 108.5(4) . . ? C26 N3 C25 108.1(4) . . ? C27 N3 C22 112.0(3) . . ? C26 N3 C22 112.6(3) . . ? C25 N3 C22 106.1(3) . . ? C35 N4 C34 111.9(4) . . ? C35 N4 C31 109.2(4) . . ? C34 N4 C31 113.3(4) . . ? C35 N4 C36 108.7(4) . . ? C34 N4 C36 106.9(4) . . ? C31 N4 C36 106.6(3) . . ? F5 P1 F2 177.7(2) . . ? F5 P1 F3 90.3(2) . . ? F2 P1 F3 91.40(19) . . ? F5 P1 F4 87.21(19) . . ? F2 P1 F4 91.30(18) . . ? F3 P1 F4 89.01(18) . . ? F5 P1 F1 89.6(2) . . ? F2 P1 F1 88.65(19) . . ? F3 P1 F1 179.8(2) . . ? F4 P1 F1 91.14(19) . . ? F5 P1 F6 92.87(19) . . ? F2 P1 F6 88.67(19) . . ? F3 P1 F6 89.12(18) . . ? F4 P1 F6 178.1(2) . . ? F1 P1 F6 90.74(19) . . ? F10 P2 F7 91.0(2) . . ? F10 P2 F8 89.3(2) . . ? F7 P2 F8 90.7(2) . . ? F10 P2 F9 89.3(2) . . ? F7 P2 F9 176.9(2) . . ? F8 P2 F9 92.3(2) . . ? F10 P2 F11 90.9(2) . . ? F7 P2 F11 92.7(2) . . ? F8 P2 F11 176.6(2) . . ? F9 P2 F11 84.2(2) . . ? F10 P2 F12 179.5(2) . . ? F7 P2 F12 89.5(2) . . ? F8 P2 F12 90.45(19) . . ? F9 P2 F12 90.2(2) . . ? F11 P2 F12 89.22(19) . . ? C1 S1 Zn1 110.03(17) . . ? C10 S2 Zn1 108.70(11) . . ? C19 S3 Zn1 111.10(11) . . ? C28 S4 Zn1 112.11(16) . . ? S1 Zn1 S4 104.00(4) . . ? S1 Zn1 S3 120.77(4) . . ? S4 Zn1 S3 115.34(4) . . ? S1 Zn1 S2 106.01(4) . . ? S4 Zn1 S2 110.08(4) . . ? S3 Zn1 S2 100.07(4) . . ? 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 C6 C1 C2 C3 5.7(8) . . . . ? S1 C1 C2 C3 -175.2(4) . . . . ? C1 C2 C3 C4 -4.0(8) . . . . ? C2 C3 C4 C5 0.2(8) . . . . ? C2 C3 C4 N1 178.6(5) . . . . ? C3 C4 C5 C6 1.7(7) . . . . ? N1 C4 C5 C6 -176.7(4) . . . . ? C2 C1 C6 C5 -3.7(9) . . . . ? S1 C1 C6 C5 177.2(4) . . . . ? C4 C5 C6 C1 0.1(8) . . . . ? C15 C10 C11 C12 0.0 . . . . ? S2 C10 C11 C12 -179.4(2) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C11 C12 C13 N2 177.7(3) . . . . ? C12 C13 C14 C15 0.0 . . . . ? N2 C13 C14 C15 -177.6(3) . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? S2 C10 C15 C14 179.4(2) . . . . ? C24 C19 C20 C21 0.0 . . . . ? S3 C19 C20 C21 -178.0(3) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C20 C21 C22 N3 -175.8(3) . . . . ? C21 C22 C23 C24 0.0 . . . . ? N3 C22 C23 C24 175.9(3) . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 C23 0.0 . . . . ? S3 C19 C24 C23 178.0(2) . . . . ? C33 C28 C29 C30 -0.3(7) . . . . ? S4 C28 C29 C30 -175.8(4) . . . . ? C28 C29 C30 C31 -1.3(7) . . . . ? C29 C30 C31 C32 4.1(7) . . . . ? C29 C30 C31 N4 178.7(4) . . . . ? C30 C31 C32 C33 -5.5(8) . . . . ? N4 C31 C32 C33 -180.0(4) . . . . ? C29 C28 C33 C32 -1.0(7) . . . . ? S4 C28 C33 C32 174.7(4) . . . . ? C31 C32 C33 C28 4.0(8) . . . . ? C3 C4 N1 C8 34.0(6) . . . . ? C5 C4 N1 C8 -147.6(4) . . . . ? C3 C4 N1 C7 -92.7(6) . . . . ? C5 C4 N1 C7 85.7(6) . . . . ? C3 C4 N1 C9 148.7(5) . . . . ? C5 C4 N1 C9 -32.9(6) . . . . ? C12 C13 N2 C17 45.4(4) . . . . ? C14 C13 N2 C17 -137.0(3) . . . . ? C12 C13 N2 C16 -72.3(4) . . . . ? C14 C13 N2 C16 105.3(4) . . . . ? C12 C13 N2 C18 166.7(3) . . . . ? C14 C13 N2 C18 -15.7(4) . . . . ? C23 C22 N3 C27 -80.5(4) . . . . ? C21 C22 N3 C27 95.4(4) . . . . ? C23 C22 N3 C26 43.2(4) . . . . ? C21 C22 N3 C26 -140.9(3) . . . . ? C23 C22 N3 C25 161.2(3) . . . . ? C21 C22 N3 C25 -22.9(4) . . . . ? C32 C31 N4 C35 49.9(6) . . . . ? C30 C31 N4 C35 -124.4(5) . . . . ? C32 C31 N4 C34 175.4(5) . . . . ? C30 C31 N4 C34 1.0(6) . . . . ? C32 C31 N4 C36 -67.3(6) . . . . ? C30 C31 N4 C36 118.3(5) . . . . ? C6 C1 S1 Zn1 62.3(5) . . . . ? C2 C1 S1 Zn1 -116.8(4) . . . . ? C11 C10 S2 Zn1 33.7(2) . . . . ? C15 C10 S2 Zn1 -145.70(15) . . . . ? C20 C19 S3 Zn1 -31.4(2) . . . . ? C24 C19 S3 Zn1 150.68(15) . . . . ? C33 C28 S4 Zn1 162.1(3) . . . . ? C29 C28 S4 Zn1 -22.3(4) . . . . ? C1 S1 Zn1 S4 -55.15(18) . . . . ? C1 S1 Zn1 S3 76.28(18) . . . . ? C1 S1 Zn1 S2 -171.23(18) . . . . ? C28 S4 Zn1 S1 178.07(16) . . . . ? C28 S4 Zn1 S3 43.53(17) . . . . ? C28 S4 Zn1 S2 -68.74(17) . . . . ? C19 S3 Zn1 S1 -4.81(13) . . . . ? C19 S3 Zn1 S4 121.58(12) . . . . ? C19 S3 Zn1 S2 -120.39(12) . . . . ? C10 S2 Zn1 S1 29.21(12) . . . . ? C10 S2 Zn1 S4 -82.68(12) . . . . ? C10 S2 Zn1 S3 155.47(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.276 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.066 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 865708' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 Hg N4 S4, 2(C3 H7 N O), 2(F6 P)' _chemical_formula_sum 'C42 H66 F12 Hg N6 O2 P2 S4' _chemical_formula_weight 1305.82 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.796(2) _cell_length_b 19.459(4) _cell_length_c 28.684(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.96(3) _cell_angle_gamma 90.00 _cell_volume 5438(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19465 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 3.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3080 _exptl_absorpt_correction_T_max 0.3942 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku Mercury' _diffrn_measurement_method \w _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 52088 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9938 _reflns_number_gt 9133 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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^)+(0.0242P)^2^+10.4890P] 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 9938 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Hg1 Hg 0.833864(14) 0.266326(7) 0.266429(5) 0.02442(5) Uani 1 1 d . . . P1 P 0.20760(10) 0.54895(5) 0.07515(4) 0.0289(2) Uani 1 1 d . . . P2 P 0.17168(14) 0.57090(6) 0.42454(4) 0.0449(3) Uani 1 1 d . . . S1 S 0.81052(9) 0.29856(5) 0.35189(3) 0.0294(2) Uani 1 1 d . . . S2 S 0.86279(11) 0.13563(5) 0.27393(3) 0.0312(2) Uani 1 1 d . . . S3 S 1.07344(9) 0.30039(5) 0.24730(3) 0.0255(2) Uani 1 1 d . . . S4 S 0.63091(10) 0.29546(5) 0.21036(3) 0.0301(2) Uani 1 1 d . . . F1 F 0.1112(3) 0.52950(16) 0.02934(10) 0.0581(8) Uani 1 1 d . . . F2 F 0.3043(2) 0.56923(12) 0.12166(8) 0.0382(6) Uani 1 1 d . . . F3 F 0.2982(3) 0.59688(15) 0.04508(9) 0.0522(7) Uani 1 1 d . . . F4 F 0.1123(2) 0.61370(12) 0.08339(9) 0.0402(6) Uani 1 1 d . . . F5 F 0.1174(2) 0.50230(12) 0.10592(10) 0.0462(6) Uani 1 1 d . . . F6 F 0.3048(3) 0.48582(14) 0.06725(10) 0.0532(7) Uani 1 1 d . . . F7 F 0.2634(5) 0.5406(2) 0.38808(13) 0.1230(19) Uani 1 1 d . . . F8 F 0.2985(4) 0.5809(2) 0.46214(12) 0.0960(13) Uani 1 1 d . . . F9 F 0.0738(4) 0.59679(16) 0.46067(12) 0.0786(10) Uani 1 1 d . . . F10 F 0.1864(3) 0.64572(15) 0.40463(11) 0.0667(9) Uani 1 1 d . . . F11 F 0.1505(4) 0.49488(15) 0.44445(10) 0.0816(11) Uani 1 1 d . . . F12 F 0.0437(4) 0.5597(2) 0.38708(12) 0.0998(14) Uani 1 1 d . . . O1 O 0.6810(4) 0.69536(18) 1.00881(11) 0.0557(9) Uani 1 1 d . . . O2 O -0.0698(4) 0.21363(17) 0.04285(13) 0.0565(9) Uani 1 1 d . . . N1 N 0.2236(3) 0.29399(18) 0.40008(11) 0.0305(7) Uani 1 1 d . . . N2 N 0.8198(3) 0.00302(16) 0.08199(11) 0.0307(7) Uani 1 1 d . . . N3 N 1.1665(3) 0.60830(15) 0.25969(11) 0.0255(7) Uani 1 1 d . . . N4 N 0.7346(3) 0.55558(15) 0.10362(11) 0.0252(7) Uani 1 1 d . . . N5 N 0.4948(4) 0.70745(18) 0.95540(12) 0.0361(8) Uani 1 1 d . . . N6 N 0.0679(4) 0.29919(19) 0.07446(13) 0.0401(9) Uani 1 1 d . . . C1 C 0.6378(3) 0.29433(17) 0.36414(12) 0.0205(7) Uani 1 1 d . . . C2 C 0.5272(4) 0.30817(19) 0.33071(13) 0.0252(8) Uani 1 1 d . . . H2 H 0.5435 0.3179 0.2993 0.030 Uiso 1 1 calc R . . C3 C 0.3939(4) 0.3079(2) 0.34276(13) 0.0278(8) Uani 1 1 d . . . H3 H 0.3194 0.3170 0.3197 0.033 Uiso 1 1 calc R . . C4 C 0.3695(3) 0.29430(19) 0.38861(13) 0.0243(8) Uani 1 1 d . . . C5 C 0.4771(4) 0.28011(19) 0.42231(13) 0.0270(8) Uani 1 1 d . . . H5 H 0.4603 0.2706 0.4537 0.032 Uiso 1 1 calc R . . C6 C 0.6102(4) 0.27990(18) 0.40966(13) 0.0244(8) Uani 1 1 d . . . H6 H 0.6841 0.2696 0.4327 0.029 Uiso 1 1 calc R . . C7 C 0.1474(4) 0.2356(2) 0.37413(17) 0.0367(10) Uani 1 1 d . . . H7A H 0.1432 0.2438 0.3403 0.055 Uiso 1 1 calc R . . H7B H 0.0540 0.2329 0.3834 0.055 Uiso 1 1 calc R . . H7C H 0.1955 0.1923 0.3819 0.055 Uiso 1 1 calc R . . C8 C 0.1550(4) 0.3602(2) 0.3847(2) 0.0495(13) Uani 1 1 d . . . H8A H 0.2076 0.3988 0.3993 0.074 Uiso 1 1 calc R . . H8B H 0.0618 0.3610 0.3942 0.074 Uiso 1 1 calc R . . H8C H 0.1506 0.3642 0.3505 0.074 Uiso 1 1 calc R . . C9 C 0.2123(5) 0.2828(4) 0.45099(17) 0.0714(19) Uani 1 1 d . . . H9A H 0.2541 0.2386 0.4606 0.107 Uiso 1 1 calc R . . H9B H 0.1154 0.2826 0.4566 0.107 Uiso 1 1 calc R . . H9C H 0.2602 0.3199 0.4691 0.107 Uiso 1 1 calc R . . C10 C 0.8462(4) 0.09959(18) 0.21737(13) 0.0229(8) Uani 1 1 d . . . C11 C 0.8415(4) 0.13871(19) 0.17644(13) 0.0283(8) Uani 1 1 d . . . H11 H 0.8445 0.1874 0.1787 0.034 Uiso 1 1 calc R . . C12 C 0.8326(4) 0.1083(2) 0.13273(13) 0.0301(9) Uani 1 1 d . . . H12 H 0.8298 0.1360 0.1054 0.036 Uiso 1 1 calc R . . C13 C 0.8277(4) 0.03765(19) 0.12889(13) 0.0266(8) Uani 1 1 d . . . C14 C 0.8314(4) -0.00267(19) 0.16891(13) 0.0283(8) Uani 1 1 d . . . H14 H 0.8276 -0.0513 0.1663 0.034 Uiso 1 1 calc R . . C15 C 0.8405(4) 0.02791(18) 0.21245(13) 0.0259(8) Uani 1 1 d . . . H15 H 0.8430 -0.0001 0.2397 0.031 Uiso 1 1 calc R . . C16 C 0.6959(5) -0.0430(2) 0.07541(16) 0.0433(11) Uani 1 1 d . . . H16A H 0.7033 -0.0787 0.0996 0.065 Uiso 1 1 calc R . . H16B H 0.6908 -0.0646 0.0444 0.065 Uiso 1 1 calc R . . H16C H 0.6129 -0.0157 0.0779 0.065 Uiso 1 1 calc R . . C17 C 0.9457(5) -0.0397(2) 0.07854(16) 0.0439(11) Uani 1 1 d . . . H17A H 1.0269 -0.0099 0.0815 0.066 Uiso 1 1 calc R . . H17B H 0.9386 -0.0631 0.0481 0.066 Uiso 1 1 calc R . . H17C H 0.9540 -0.0739 0.1037 0.066 Uiso 1 1 calc R . . C18 C 0.8095(6) 0.0540(2) 0.04252(15) 0.0565(15) Uani 1 1 d . . . H18A H 0.7246 0.0806 0.0428 0.085 Uiso 1 1 calc R . . H18B H 0.8087 0.0296 0.0126 0.085 Uiso 1 1 calc R . . H18C H 0.8885 0.0851 0.0464 0.085 Uiso 1 1 calc R . . C19 C 1.0931(4) 0.39000(18) 0.25108(13) 0.0239(8) Uani 1 1 d . . . C20 C 1.2127(4) 0.4197(2) 0.23766(16) 0.0390(11) Uani 1 1 d . . . H20 H 1.2802 0.3910 0.2262 0.047 Uiso 1 1 calc R . . C21 C 1.2359(4) 0.4896(2) 0.24057(16) 0.0388(11) Uani 1 1 d . . . H21 H 1.3184 0.5083 0.2313 0.047 Uiso 1 1 calc R . . C22 C 1.1386(4) 0.53248(18) 0.25702(13) 0.0245(8) Uani 1 1 d . . . C23 C 1.0197(4) 0.5047(2) 0.27039(14) 0.0306(9) Uani 1 1 d . . . H23 H 0.9524 0.5338 0.2816 0.037 Uiso 1 1 calc R . . C24 C 0.9978(4) 0.43444(19) 0.26747(14) 0.0302(9) Uani 1 1 d . . . H24 H 0.9152 0.4161 0.2769 0.036 Uiso 1 1 calc R . . C25 C 1.1789(6) 0.6365(2) 0.21178(15) 0.0488(12) Uani 1 1 d . . . H25A H 1.2558 0.6141 0.1985 0.073 Uiso 1 1 calc R . . H25B H 1.1953 0.6861 0.2139 0.073 Uiso 1 1 calc R . . H25C H 1.0938 0.6276 0.1916 0.073 Uiso 1 1 calc R . . C26 C 1.2995(4) 0.6215(2) 0.28958(16) 0.0373(10) Uani 1 1 d . . . H26A H 1.2958 0.6004 0.3205 0.056 Uiso 1 1 calc R . . H26B H 1.3137 0.6711 0.2932 0.056 Uiso 1 1 calc R . . H26C H 1.3755 0.6014 0.2745 0.056 Uiso 1 1 calc R . . C27 C 1.0573(4) 0.6476(2) 0.28110(18) 0.0427(11) Uani 1 1 d . . . H27A H 0.9692 0.6414 0.2620 0.064 Uiso 1 1 calc R . . H27B H 1.0812 0.6965 0.2824 0.064 Uiso 1 1 calc R . . H27C H 1.0500 0.6306 0.3129 0.064 Uiso 1 1 calc R . . C28 C 0.6686(4) 0.37215(19) 0.18158(12) 0.0235(8) Uani 1 1 d . . . C29 C 0.7947(4) 0.3859(2) 0.16505(14) 0.0297(9) Uani 1 1 d . . . H29 H 0.8675 0.3538 0.1709 0.036 Uiso 1 1 calc R . . C30 C 0.8161(4) 0.4452(2) 0.14028(14) 0.0284(9) Uani 1 1 d . . . H30 H 0.9029 0.4538 0.1295 0.034 Uiso 1 1 calc R . . C31 C 0.7095(4) 0.49225(18) 0.13133(12) 0.0212(7) Uani 1 1 d . . . C32 C 0.5847(4) 0.48032(19) 0.14765(13) 0.0272(8) Uani 1 1 d . . . H32 H 0.5123 0.5127 0.1419 0.033 Uiso 1 1 calc R . . C33 C 0.5649(4) 0.42070(19) 0.17260(13) 0.0262(8) Uani 1 1 d . . . H33 H 0.4784 0.4128 0.1838 0.031 Uiso 1 1 calc R . . C34 C 0.7754(4) 0.5358(2) 0.05636(13) 0.0342(9) Uani 1 1 d . . . H34A H 0.8617 0.5100 0.0603 0.051 Uiso 1 1 calc R . . H34B H 0.7877 0.5773 0.0379 0.051 Uiso 1 1 calc R . . H34C H 0.7034 0.5071 0.0400 0.051 Uiso 1 1 calc R . . C35 C 0.6096(4) 0.6004(2) 0.09571(16) 0.0368(10) Uani 1 1 d . . . H35A H 0.5345 0.5744 0.0786 0.055 Uiso 1 1 calc R . . H35B H 0.6306 0.6408 0.0773 0.055 Uiso 1 1 calc R . . H35C H 0.5819 0.6153 0.1260 0.055 Uiso 1 1 calc R . . C36 C 0.8469(4) 0.5976(2) 0.12954(15) 0.0329(9) Uani 1 1 d . . . H36A H 0.8190 0.6115 0.1600 0.049 Uiso 1 1 calc R . . H36B H 0.8639 0.6386 0.1112 0.049 Uiso 1 1 calc R . . H36C H 0.9310 0.5700 0.1343 0.049 Uiso 1 1 calc R . . C37 C 0.4075(6) 0.7522(3) 0.9244(2) 0.0620(15) Uani 1 1 d . . . H37A H 0.4367 0.8001 0.9295 0.093 Uiso 1 1 calc R . . H37B H 0.3120 0.7473 0.9312 0.093 Uiso 1 1 calc R . . H37C H 0.4152 0.7395 0.8917 0.093 Uiso 1 1 calc R . . C38 C 0.4598(5) 0.6355(2) 0.95488(17) 0.0514(13) Uani 1 1 d . . . H38A H 0.5293 0.6101 0.9750 0.077 Uiso 1 1 calc R . . H38B H 0.4562 0.6180 0.9228 0.077 Uiso 1 1 calc R . . H38C H 0.3699 0.6296 0.9665 0.077 Uiso 1 1 calc R . . C39 C 0.6031(5) 0.7306(2) 0.98237(16) 0.0425(11) Uani 1 1 d . . . H39 H 0.6220 0.7784 0.9812 0.051 Uiso 1 1 calc R . . C40 C 0.0168(6) 0.3491(3) 0.03950(19) 0.0600(14) Uani 1 1 d . . . H40A H -0.0789 0.3384 0.0284 0.090 Uiso 1 1 calc R . . H40B H 0.0726 0.3475 0.0131 0.090 Uiso 1 1 calc R . . H40C H 0.0219 0.3952 0.0534 0.090 Uiso 1 1 calc R . . C41 C 0.1753(6) 0.3200(3) 0.11027(19) 0.0620(15) Uani 1 1 d . . . H41A H 0.2010 0.2810 0.1309 0.093 Uiso 1 1 calc R . . H41B H 0.1420 0.3578 0.1287 0.093 Uiso 1 1 calc R . . H41C H 0.2556 0.3354 0.0954 0.093 Uiso 1 1 calc R . . C42 C 0.0197(5) 0.2361(2) 0.07254(18) 0.0480(12) Uani 1 1 d . . . H42 H 0.0568 0.2050 0.0961 0.058 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 Hg1 0.02476(8) 0.02155(8) 0.02746(8) 0.00139(6) 0.00516(6) -0.00164(6) P1 0.0204(5) 0.0331(6) 0.0335(6) -0.0061(4) 0.0045(4) -0.0010(4) P2 0.0626(8) 0.0408(7) 0.0312(6) 0.0051(5) 0.0046(6) 0.0151(6) S1 0.0163(4) 0.0416(6) 0.0307(5) -0.0108(4) 0.0039(4) -0.0002(4) S2 0.0516(6) 0.0197(5) 0.0233(5) 0.0022(4) 0.0090(4) 0.0008(4) S3 0.0240(5) 0.0181(4) 0.0356(5) -0.0002(4) 0.0096(4) -0.0003(4) S4 0.0273(5) 0.0307(5) 0.0315(5) 0.0104(4) -0.0004(4) -0.0081(4) F1 0.0422(15) 0.079(2) 0.0500(17) -0.0181(15) -0.0118(13) -0.0022(14) F2 0.0320(12) 0.0471(15) 0.0348(13) -0.0093(11) -0.0001(10) 0.0019(11) F3 0.0380(14) 0.074(2) 0.0471(16) 0.0109(14) 0.0178(12) -0.0065(13) F4 0.0276(12) 0.0342(13) 0.0601(16) 0.0036(12) 0.0104(11) 0.0061(10) F5 0.0334(13) 0.0353(14) 0.0722(19) 0.0106(13) 0.0171(12) -0.0023(11) F6 0.0388(15) 0.0504(16) 0.0706(19) -0.0255(14) 0.0069(13) 0.0114(12) F7 0.166(4) 0.152(4) 0.059(2) 0.035(2) 0.054(3) 0.103(3) F8 0.076(2) 0.147(4) 0.060(2) 0.042(2) -0.0198(18) -0.038(2) F9 0.105(3) 0.059(2) 0.079(2) 0.0210(17) 0.049(2) 0.0272(19) F10 0.091(2) 0.0515(18) 0.0580(19) 0.0209(15) 0.0102(17) -0.0117(16) F11 0.157(3) 0.0369(16) 0.0468(18) 0.0075(14) -0.0098(19) 0.0183(19) F12 0.132(3) 0.091(3) 0.065(2) 0.034(2) -0.042(2) -0.033(2) O1 0.068(2) 0.053(2) 0.0412(19) 0.0142(16) -0.0193(17) -0.0143(18) O2 0.057(2) 0.046(2) 0.063(2) 0.0130(17) -0.0100(18) -0.0151(17) N1 0.0193(16) 0.041(2) 0.0319(18) -0.0021(15) 0.0058(13) 0.0011(14) N2 0.044(2) 0.0218(17) 0.0263(17) -0.0010(14) 0.0024(15) -0.0065(15) N3 0.0299(17) 0.0174(16) 0.0297(18) 0.0005(13) 0.0048(14) -0.0021(13) N4 0.0250(16) 0.0239(16) 0.0280(17) 0.0055(13) 0.0083(13) 0.0020(13) N5 0.043(2) 0.0333(19) 0.0314(19) -0.0012(15) 0.0008(16) -0.0046(16) N6 0.045(2) 0.037(2) 0.038(2) 0.0049(17) 0.0043(17) -0.0063(17) C1 0.0170(17) 0.0166(17) 0.0284(19) -0.0052(15) 0.0050(14) 0.0004(14) C2 0.0227(19) 0.030(2) 0.0232(19) -0.0017(16) 0.0034(15) -0.0001(16) C3 0.0209(19) 0.035(2) 0.026(2) -0.0029(17) -0.0014(15) 0.0035(16) C4 0.0156(17) 0.0262(19) 0.032(2) -0.0042(16) 0.0059(15) -0.0014(15) C5 0.026(2) 0.029(2) 0.027(2) 0.0009(16) 0.0084(16) -0.0026(16) C6 0.0222(18) 0.0214(19) 0.029(2) -0.0005(15) -0.0008(15) 0.0015(15) C7 0.021(2) 0.028(2) 0.061(3) -0.001(2) 0.0049(19) -0.0011(17) C8 0.028(2) 0.026(2) 0.098(4) -0.013(2) 0.021(2) 0.0006(18) C9 0.031(3) 0.149(6) 0.037(3) -0.007(3) 0.016(2) -0.005(3) C10 0.0228(18) 0.0221(19) 0.0246(19) 0.0002(15) 0.0064(15) 0.0012(15) C11 0.036(2) 0.0185(19) 0.031(2) -0.0001(16) 0.0047(17) 0.0016(16) C12 0.042(2) 0.026(2) 0.023(2) 0.0043(16) 0.0022(17) 0.0015(17) C13 0.031(2) 0.025(2) 0.024(2) -0.0020(16) 0.0024(16) -0.0022(16) C14 0.035(2) 0.0176(19) 0.033(2) 0.0031(16) 0.0079(17) -0.0034(16) C15 0.029(2) 0.0206(19) 0.028(2) 0.0039(16) 0.0064(16) -0.0016(15) C16 0.048(3) 0.043(3) 0.037(3) -0.008(2) -0.003(2) -0.013(2) C17 0.048(3) 0.043(3) 0.043(3) -0.015(2) 0.015(2) -0.001(2) C18 0.111(5) 0.034(3) 0.024(2) 0.0021(19) 0.000(3) -0.012(3) C19 0.0240(19) 0.0219(19) 0.026(2) -0.0008(15) 0.0056(15) -0.0012(15) C20 0.035(2) 0.023(2) 0.064(3) -0.005(2) 0.029(2) -0.0016(18) C21 0.035(2) 0.025(2) 0.061(3) -0.002(2) 0.026(2) -0.0077(18) C22 0.0261(19) 0.0183(18) 0.030(2) -0.0010(15) 0.0054(16) -0.0022(15) C23 0.024(2) 0.025(2) 0.044(2) -0.0032(18) 0.0119(17) 0.0014(16) C24 0.0232(19) 0.025(2) 0.044(2) -0.0011(18) 0.0127(17) -0.0025(16) C25 0.081(4) 0.033(2) 0.033(2) 0.006(2) 0.007(2) -0.014(2) C26 0.034(2) 0.029(2) 0.048(3) -0.0012(19) -0.0003(19) -0.0059(18) C27 0.037(2) 0.026(2) 0.067(3) -0.009(2) 0.011(2) 0.0051(19) C28 0.0254(19) 0.026(2) 0.0190(18) 0.0015(15) 0.0010(15) -0.0038(15) C29 0.024(2) 0.030(2) 0.035(2) 0.0070(17) 0.0043(17) 0.0037(16) C30 0.0188(18) 0.033(2) 0.035(2) 0.0095(17) 0.0072(16) -0.0012(16) C31 0.0209(18) 0.0235(19) 0.0196(18) 0.0030(15) 0.0032(14) -0.0005(15) C32 0.0229(19) 0.027(2) 0.032(2) 0.0038(16) 0.0064(16) 0.0023(16) C33 0.0208(18) 0.029(2) 0.030(2) 0.0015(16) 0.0082(15) -0.0030(16) C34 0.042(2) 0.037(2) 0.026(2) 0.0076(18) 0.0105(18) 0.0006(19) C35 0.036(2) 0.031(2) 0.045(3) 0.0167(19) 0.0104(19) 0.0110(18) C36 0.031(2) 0.027(2) 0.042(2) -0.0054(18) 0.0114(18) -0.0072(17) C37 0.062(3) 0.047(3) 0.072(4) 0.005(3) -0.022(3) 0.000(3) C38 0.064(3) 0.043(3) 0.046(3) -0.004(2) -0.001(2) -0.015(2) C39 0.054(3) 0.033(2) 0.038(2) 0.005(2) -0.007(2) -0.014(2) C40 0.081(4) 0.039(3) 0.058(3) 0.012(2) 0.000(3) -0.006(3) C41 0.064(3) 0.063(4) 0.057(3) -0.005(3) -0.005(3) -0.013(3) C42 0.050(3) 0.042(3) 0.051(3) 0.020(2) -0.002(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S4 2.4892(12) . ? Hg1 S3 2.5525(10) . ? Hg1 S1 2.5634(11) . ? Hg1 S2 2.5655(11) . ? P1 F1 1.582(3) . ? P1 F6 1.585(3) . ? P1 F5 1.596(3) . ? P1 F3 1.600(3) . ? P1 F4 1.600(2) . ? P1 F2 1.603(2) . ? P2 F7 1.563(4) . ? P2 F9 1.566(3) . ? P2 F8 1.570(3) . ? P2 F10 1.576(3) . ? P2 F12 1.579(4) . ? P2 F11 1.607(3) . ? S1 C1 1.765(3) . ? S2 C10 1.760(4) . ? S3 C19 1.756(4) . ? S4 C28 1.763(4) . ? O1 C39 1.228(5) . ? O2 C42 1.237(6) . ? N1 C9 1.492(6) . ? N1 C8 1.499(5) . ? N1 C4 1.500(4) . ? N1 C7 1.512(5) . ? N2 C17 1.499(5) . ? N2 C13 1.499(5) . ? N2 C18 1.501(5) . ? N2 C16 1.504(5) . ? N3 C25 1.496(5) . ? N3 C27 1.498(5) . ? N3 C22 1.501(5) . ? N3 C26 1.505(5) . ? N4 C31 1.500(4) . ? N4 C35 1.501(5) . ? N4 C34 1.503(5) . ? N4 C36 1.504(5) . ? N5 C39 1.325(5) . ? N5 C38 1.441(6) . ? N5 C37 1.457(6) . ? N6 C42 1.315(6) . ? N6 C40 1.448(6) . ? N6 C41 1.450(6) . ? C1 C6 1.390(5) . ? C1 C2 1.397(5) . ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.386(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C5 C6 1.389(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.396(5) . ? C10 C15 1.403(5) . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 C13 1.380(5) . ? C12 H12 0.9500 . ? C13 C14 1.388(5) . ? C14 C15 1.378(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.390(5) . ? C19 C20 1.396(5) . ? C20 C21 1.380(6) . ? C20 H20 0.9500 . ? C21 C22 1.385(5) . ? C21 H21 0.9500 . ? C22 C23 1.374(5) . ? C23 C24 1.386(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.392(5) . ? C28 C29 1.393(5) . ? C29 C30 1.383(5) . ? C29 H29 0.9500 . ? C30 C31 1.392(5) . ? C30 H30 0.9500 . ? C31 C32 1.374(5) . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42 0.9500 . ? 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 S4 Hg1 S3 119.50(3) . . ? S4 Hg1 S1 114.68(4) . . ? S3 Hg1 S1 108.50(4) . . ? S4 Hg1 S2 110.72(3) . . ? S3 Hg1 S2 100.34(3) . . ? S1 Hg1 S2 100.51(3) . . ? F1 P1 F6 90.67(15) . . ? F1 P1 F5 90.36(16) . . ? F6 P1 F5 90.77(15) . . ? F1 P1 F3 90.48(16) . . ? F6 P1 F3 89.99(16) . . ? F5 P1 F3 178.86(16) . . ? F1 P1 F4 90.23(15) . . ? F6 P1 F4 178.76(15) . . ? F5 P1 F4 90.08(13) . . ? F3 P1 F4 89.15(14) . . ? F1 P1 F2 179.45(16) . . ? F6 P1 F2 89.88(14) . . ? F5 P1 F2 89.60(14) . . ? F3 P1 F2 89.56(14) . . ? F4 P1 F2 89.23(13) . . ? F7 P2 F9 176.2(3) . . ? F7 P2 F8 92.2(3) . . ? F9 P2 F8 90.0(2) . . ? F7 P2 F10 91.4(2) . . ? F9 P2 F10 91.60(18) . . ? F8 P2 F10 92.2(2) . . ? F7 P2 F12 87.9(3) . . ? F9 P2 F12 89.9(2) . . ? F8 P2 F12 179.1(2) . . ? F10 P2 F12 88.68(18) . . ? F7 P2 F11 89.7(2) . . ? F9 P2 F11 87.16(19) . . ? F8 P2 F11 89.5(2) . . ? F10 P2 F11 177.8(2) . . ? F12 P2 F11 89.53(19) . . ? C1 S1 Hg1 111.19(12) . . ? C10 S2 Hg1 108.60(12) . . ? C19 S3 Hg1 110.00(12) . . ? C28 S4 Hg1 107.65(12) . . ? C9 N1 C8 109.7(4) . . ? C9 N1 C4 112.6(3) . . ? C8 N1 C4 109.9(3) . . ? C9 N1 C7 106.8(4) . . ? C8 N1 C7 108.5(3) . . ? C4 N1 C7 109.2(3) . . ? C17 N2 C13 110.0(3) . . ? C17 N2 C18 107.9(4) . . ? C13 N2 C18 111.9(3) . . ? C17 N2 C16 108.7(3) . . ? C13 N2 C16 110.3(3) . . ? C18 N2 C16 108.0(3) . . ? C25 N3 C27 108.6(3) . . ? C25 N3 C22 110.2(3) . . ? C27 N3 C22 112.9(3) . . ? C25 N3 C26 108.2(3) . . ? C27 N3 C26 107.0(3) . . ? C22 N3 C26 109.8(3) . . ? C31 N4 C35 112.4(3) . . ? C31 N4 C34 109.9(3) . . ? C35 N4 C34 107.6(3) . . ? C31 N4 C36 109.6(3) . . ? C35 N4 C36 107.6(3) . . ? C34 N4 C36 109.6(3) . . ? C39 N5 C38 120.8(4) . . ? C39 N5 C37 122.4(4) . . ? C38 N5 C37 116.8(4) . . ? C42 N6 C40 120.0(4) . . ? C42 N6 C41 121.5(4) . . ? C40 N6 C41 118.5(4) . . ? C6 C1 C2 118.1(3) . . ? C6 C1 S1 118.8(3) . . ? C2 C1 S1 123.1(3) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 N1 121.4(3) . . ? C3 C4 N1 118.1(3) . . ? C4 C5 C6 119.1(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.4(3) . . ? C11 C10 S2 123.4(3) . . ? C15 C10 S2 119.2(3) . . ? C12 C11 C10 121.5(3) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 N2 121.2(3) . . ? C14 C13 N2 118.9(3) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C10 121.3(3) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 116.6(3) . . ? C24 C19 S3 124.4(3) . . ? C20 C19 S3 119.0(3) . . ? C21 C20 C19 121.9(4) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 120.0(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.4(3) . . ? C23 C22 N3 121.8(3) . . ? C21 C22 N3 118.8(3) . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 122.0(3) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 117.5(3) . . ? C33 C28 S4 118.5(3) . . ? C29 C28 S4 123.9(3) . . ? C30 C29 C28 121.5(4) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 119.5(3) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 N4 121.3(3) . . ? C30 C31 N4 118.5(3) . . ? C31 C32 C33 119.6(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C28 121.6(3) . . ? C32 C33 H33 119.2 . . ? C28 C33 H33 119.2 . . ? N4 C34 H34A 109.5 . . ? N4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 N5 125.4(4) . . ? O1 C39 H39 117.3 . . ? N5 C39 H39 117.3 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 H41A 109.5 . . ? N6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O2 C42 N6 125.8(4) . . ? O2 C42 H42 117.1 . . ? N6 C42 H42 117.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.103 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.081 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 865709' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H78 N6 S6 Zn2, 2(C3 H7 N O), 4(F6 P), 2(H2 O)' _chemical_formula_sum 'C60 H96 F24 N8 O4 P4 S6 Zn2' _chemical_formula_weight 1896.53 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 38.959(8) _cell_length_b 9.5325(19) _cell_length_c 28.966(6) _cell_angle_alpha 90.00 _cell_angle_beta 131.23(3) _cell_angle_gamma 90.00 _cell_volume 8090(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 10892 _cell_measurement_theta_min 3.0132 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8290 _exptl_absorpt_correction_T_max 0.9127 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Rigaku Mercury' _diffrn_measurement_method \w _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 38726 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7402 _reflns_number_gt 5609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The U~ij~ values of N2 and C16 atoms were restrained by the EADP instruction. ; _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^)+(0.0672P)^2^+39.1098P] 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 7402 _refine_ls_number_parameters 501 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1710 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.05136(2) 0.60362(7) 0.28942(3) 0.0267(2) Uani 1 1 d . . . P1 P 0.22530(6) 0.97421(18) 0.35307(8) 0.0368(4) Uani 1 1 d . . . P2 P 0.13367(5) 0.99141(18) 0.59326(8) 0.0362(4) Uani 1 1 d . . . S1 S 0.05988(5) 0.84427(16) 0.29445(7) 0.0317(4) Uani 1 1 d . . . S2 S 0.10487(5) 0.43152(16) 0.32912(7) 0.0316(4) Uani 1 1 d . . . S3 S 0.00815(5) 0.58071(15) 0.32092(6) 0.0265(3) Uani 1 1 d . . . O1 O 0.06415(18) 0.4628(6) 0.5275(3) 0.0575(14) Uani 1 1 d . . . O2 O 0.0082(3) 0.3283(7) 0.5419(4) 0.077(2) Uani 1 1 d D . . H32 H -0.011(3) 0.378(9) 0.528(4) 0.08(4) Uiso 1 1 d D . . H31 H 0.028(2) 0.369(7) 0.550(3) 0.04(2) Uiso 1 1 d D . . F1 F 0.17924(19) 1.0145(6) 0.2878(2) 0.109(2) Uani 1 1 d . . . F2 F 0.27064(17) 0.9331(6) 0.4185(2) 0.104(2) Uani 1 1 d . . . F3 F 0.2515(2) 1.0862(5) 0.3464(3) 0.0878(18) Uani 1 1 d . . . F4 F 0.19898(19) 0.8621(5) 0.3591(3) 0.0825(16) Uani 1 1 d . . . F5 F 0.23453(18) 0.8571(5) 0.3237(3) 0.0752(15) Uani 1 1 d . . . F6 F 0.21574(18) 1.0926(5) 0.3815(2) 0.0703(14) Uani 1 1 d . . . F7 F 0.10972(15) 1.0067(6) 0.52304(19) 0.0701(14) Uani 1 1 d . . . F8 F 0.15775(14) 0.9770(6) 0.66336(19) 0.0697(14) Uani 1 1 d . . . F9 F 0.09874(14) 0.8721(4) 0.5762(2) 0.0644(13) Uani 1 1 d . . . F10 F 0.16888(14) 1.1119(4) 0.6102(2) 0.0612(12) Uani 1 1 d . . . F11 F 0.16799(13) 0.8776(4) 0.6030(2) 0.0539(11) Uani 1 1 d . . . F12 F 0.09976(13) 1.1066(4) 0.5839(2) 0.0519(10) Uani 1 1 d . . . N1 N 0.23587(19) 1.0068(6) 0.5442(2) 0.0451(15) Uani 1 1 d . . . N2 N 0.18491(17) 0.5048(6) 0.2089(2) 0.0398(10) Uani 1 1 d . . . N3 N -0.02074(16) 0.0040(5) 0.3770(2) 0.0264(11) Uani 1 1 d . . . N4 N 0.10373(18) 0.4634(6) 0.4957(2) 0.0431(14) Uani 1 1 d . . . C1 C 0.11084(19) 0.8876(6) 0.3678(3) 0.0271(13) Uani 1 1 d . . . C2 C 0.1376(2) 0.7914(6) 0.4150(3) 0.0362(15) Uani 1 1 d . A . H2 H 0.1284 0.6959 0.4076 0.043 Uiso 1 1 calc R . . C3 C 0.1775(2) 0.8301(7) 0.4725(3) 0.0407(16) Uani 1 1 d . . . H3 H 0.1951 0.7624 0.5043 0.049 Uiso 1 1 calc R A . C4 C 0.1912(2) 0.9674(7) 0.4830(3) 0.0372(15) Uani 1 1 d . A . C5 C 0.1649(2) 1.0653(7) 0.4370(3) 0.0370(15) Uani 1 1 d . . . H5 H 0.1746 1.1603 0.4443 0.044 Uiso 1 1 calc R A . C6 C 0.12512(19) 1.0262(6) 0.3808(3) 0.0304(14) Uani 1 1 d . A . H6 H 0.1068 1.0955 0.3501 0.037 Uiso 1 1 calc R . . C7A C 0.2541(8) 0.898(3) 0.5908(10) 0.0556(18) Uani 0.389(8) 1 d P A 1 H7A1 H 0.2649 0.8190 0.5817 0.083 Uiso 0.389(8) 1 calc PR A 1 H7A2 H 0.2301 0.8664 0.5906 0.083 Uiso 0.389(8) 1 calc PR A 1 H7A3 H 0.2796 0.9367 0.6312 0.083 Uiso 0.389(8) 1 calc PR A 1 C7 C 0.2436(5) 0.9428(17) 0.5958(6) 0.0556(18) Uani 0.611(8) 1 d P A 2 H7A H 0.2750 0.9617 0.6336 0.083 Uiso 0.611(8) 1 calc PR A 2 H7B H 0.2389 0.8412 0.5893 0.083 Uiso 0.611(8) 1 calc PR A 2 H7C H 0.2222 0.9822 0.5993 0.083 Uiso 0.611(8) 1 calc PR A 2 C8 C 0.2670(4) 1.0410(16) 0.5371(5) 0.0556(18) Uani 0.611(8) 1 d P A 1 H8A H 0.2533 1.1100 0.5040 0.083 Uiso 0.611(8) 1 calc PR A 1 H8B H 0.2750 0.9563 0.5267 0.083 Uiso 0.611(8) 1 calc PR A 1 H8C H 0.2946 1.0807 0.5754 0.083 Uiso 0.611(8) 1 calc PR A 1 C8A C 0.2753(6) 0.904(2) 0.5500(8) 0.0556(18) Uani 0.389(8) 1 d P A 2 H8A1 H 0.2733 0.9226 0.5150 0.083 Uiso 0.389(8) 1 calc PR A 2 H8A2 H 0.2687 0.8044 0.5499 0.083 Uiso 0.389(8) 1 calc PR A 2 H8A3 H 0.3061 0.9257 0.5882 0.083 Uiso 0.389(8) 1 calc PR A 2 C9 C 0.2265(4) 1.1491(14) 0.5654(5) 0.0556(18) Uani 0.611(8) 1 d P A 1 H9A H 0.2544 1.1764 0.6065 0.083 Uiso 0.611(8) 1 calc PR A 1 H9B H 0.2021 1.1320 0.5662 0.083 Uiso 0.611(8) 1 calc PR A 1 H9C H 0.2173 1.2247 0.5363 0.083 Uiso 0.611(8) 1 calc PR A 1 C9A C 0.2540(6) 1.144(2) 0.5489(8) 0.0556(18) Uani 0.389(8) 1 d P A 2 H9A1 H 0.2859 1.1497 0.5872 0.083 Uiso 0.389(8) 1 calc PR A 2 H9A2 H 0.2361 1.2162 0.5488 0.083 Uiso 0.389(8) 1 calc PR A 2 H9A3 H 0.2522 1.1585 0.5139 0.083 Uiso 0.389(8) 1 calc PR A 2 C10 C 0.12489(18) 0.4573(6) 0.2905(2) 0.0253(12) Uani 1 1 d . . . C11 C 0.14253(19) 0.3435(6) 0.2818(3) 0.0304(13) Uani 1 1 d . . . H11 H 0.1421 0.2530 0.2952 0.036 Uiso 1 1 calc R . . C12 C 0.16066(19) 0.3601(6) 0.2541(3) 0.0307(14) Uani 1 1 d . . . H12 H 0.1720 0.2807 0.2480 0.037 Uiso 1 1 calc R . . C13 C 0.16241(19) 0.4897(6) 0.2354(3) 0.0279(13) Uani 1 1 d . . . C14 C 0.14537(18) 0.6053(6) 0.2433(3) 0.0278(13) Uani 1 1 d . . . H14 H 0.1460 0.6952 0.2298 0.033 Uiso 1 1 calc R . . C15 C 0.12735(19) 0.5887(6) 0.2711(3) 0.0298(13) Uani 1 1 d . . . H15 H 0.1163 0.6689 0.2772 0.036 Uiso 1 1 calc R . . C16 C 0.2352(2) 0.4894(8) 0.2596(3) 0.0398(10) Uani 1 1 d . . . H16A H 0.2463 0.5609 0.2909 0.060 Uiso 1 1 calc R . . H16B H 0.2504 0.5011 0.2431 0.060 Uiso 1 1 calc R . . H16C H 0.2421 0.3959 0.2779 0.060 Uiso 1 1 calc R . . C17 C 0.1761(3) 0.6467(8) 0.1801(4) 0.0521(19) Uani 1 1 d . . . H17A H 0.1431 0.6632 0.1492 0.078 Uiso 1 1 calc R . . H17B H 0.1891 0.6499 0.1605 0.078 Uiso 1 1 calc R . . H17C H 0.1903 0.7194 0.2118 0.078 Uiso 1 1 calc R . . C18 C 0.1680(3) 0.3960(8) 0.1613(3) 0.0519(19) Uani 1 1 d . . . H18A H 0.1764 0.3027 0.1802 0.078 Uiso 1 1 calc R . . H18B H 0.1819 0.4108 0.1432 0.078 Uiso 1 1 calc R . . H18C H 0.1348 0.4027 0.1292 0.078 Uiso 1 1 calc R . . C19 C -0.00014(17) 0.4084(6) 0.3347(2) 0.0235(12) Uani 1 1 d . . . C20 C 0.0144(2) 0.2872(6) 0.3245(3) 0.0313(14) Uani 1 1 d . . . H20 H 0.0289 0.2957 0.3082 0.038 Uiso 1 1 calc R . . C21 C 0.0079(2) 0.1565(6) 0.3375(3) 0.0314(14) Uani 1 1 d . . . H21 H 0.0177 0.0751 0.3300 0.038 Uiso 1 1 calc R . . C22 C -0.01309(18) 0.1443(6) 0.3618(2) 0.0255(12) Uani 1 1 d . . . C23 C -0.0282(2) 0.2624(6) 0.3712(3) 0.0325(14) Uani 1 1 d . . . H23 H -0.0434 0.2535 0.3865 0.039 Uiso 1 1 calc R . . C24 C -0.0213(2) 0.3941(6) 0.3584(3) 0.0295(13) Uani 1 1 d . . . H24 H -0.0312 0.4752 0.3658 0.035 Uiso 1 1 calc R . . C25 C -0.0702(2) -0.0368(8) 0.3286(3) 0.0453(17) Uani 1 1 d . . . H25A H -0.0894 0.0348 0.3262 0.068 Uiso 1 1 calc R . . H25B H -0.0752 -0.1274 0.3393 0.068 Uiso 1 1 calc R . . H25C H -0.0781 -0.0445 0.2887 0.068 Uiso 1 1 calc R . . C26 C -0.0083(2) 0.0071(6) 0.4383(3) 0.0348(14) Uani 1 1 d . . . H26A H 0.0224 0.0464 0.4691 0.052 Uiso 1 1 calc R . . H26B H -0.0089 -0.0886 0.4502 0.052 Uiso 1 1 calc R . . H26C H -0.0303 0.0653 0.4356 0.052 Uiso 1 1 calc R . . C27 C 0.0081(3) -0.1083(7) 0.3801(3) 0.0427(17) Uani 1 1 d . . . H27A H -0.0016 -0.1210 0.3394 0.064 Uiso 1 1 calc R . . H27B H 0.0044 -0.1968 0.3936 0.064 Uiso 1 1 calc R . . H27C H 0.0403 -0.0800 0.4093 0.064 Uiso 1 1 calc R . . C28 C 0.1236(3) 0.3820(10) 0.4759(4) 0.064(2) Uani 1 1 d . . . H28A H 0.1170 0.2823 0.4749 0.097 Uiso 1 1 calc R . . H28B H 0.1567 0.3965 0.5047 0.097 Uiso 1 1 calc R . . H28C H 0.1104 0.4125 0.4348 0.097 Uiso 1 1 calc R . . C29 C 0.1073(2) 0.6148(8) 0.4962(3) 0.0503(19) Uani 1 1 d . . . H29A H 0.0897 0.6487 0.4540 0.075 Uiso 1 1 calc R . . H29B H 0.1394 0.6414 0.5209 0.075 Uiso 1 1 calc R . . H29C H 0.0952 0.6566 0.5139 0.075 Uiso 1 1 calc R . . C30 C 0.0817(2) 0.4011(8) 0.5106(3) 0.0488(18) Uani 1 1 d . . . H30 H 0.0794 0.3017 0.5078 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0261(3) 0.0247(4) 0.0281(4) -0.0019(3) 0.0174(3) -0.0024(3) P1 0.0410(9) 0.0335(9) 0.0406(10) 0.0040(8) 0.0289(8) 0.0037(7) P2 0.0306(8) 0.0379(10) 0.0374(10) 0.0000(8) 0.0213(8) -0.0004(7) S1 0.0306(8) 0.0262(8) 0.0279(8) -0.0003(6) 0.0148(7) -0.0044(6) S2 0.0305(8) 0.0315(8) 0.0354(9) 0.0058(7) 0.0228(7) 0.0025(6) S3 0.0321(7) 0.0229(7) 0.0262(8) 0.0015(6) 0.0199(7) 0.0005(6) O1 0.056(3) 0.055(3) 0.071(4) 0.011(3) 0.046(3) 0.002(3) O2 0.086(5) 0.046(4) 0.137(7) 0.031(4) 0.091(5) 0.016(4) F1 0.087(4) 0.085(4) 0.063(3) 0.005(3) 0.010(3) 0.018(3) F2 0.060(3) 0.090(4) 0.062(3) 0.016(3) -0.002(3) 0.011(3) F3 0.135(5) 0.050(3) 0.167(6) -0.011(3) 0.137(5) -0.020(3) F4 0.107(4) 0.054(3) 0.147(5) -0.009(3) 0.109(4) -0.018(3) F5 0.112(4) 0.050(3) 0.118(4) -0.011(3) 0.099(4) -0.001(3) F6 0.100(4) 0.052(3) 0.099(4) -0.017(3) 0.082(3) -0.009(3) F7 0.065(3) 0.100(4) 0.041(2) 0.004(2) 0.033(2) 0.014(3) F8 0.054(3) 0.110(4) 0.045(3) 0.015(3) 0.032(2) 0.016(3) F9 0.046(2) 0.041(2) 0.103(4) -0.002(2) 0.048(3) -0.0041(19) F10 0.054(2) 0.045(2) 0.097(4) -0.010(2) 0.055(3) -0.013(2) F11 0.044(2) 0.045(2) 0.076(3) -0.001(2) 0.041(2) 0.0054(18) F12 0.048(2) 0.039(2) 0.072(3) 0.002(2) 0.042(2) 0.0031(18) N1 0.045(3) 0.045(3) 0.027(3) -0.001(3) 0.016(3) -0.022(3) N2 0.031(2) 0.055(3) 0.033(2) 0.001(2) 0.021(2) 0.003(2) N3 0.035(3) 0.023(3) 0.028(3) -0.001(2) 0.023(2) -0.005(2) N4 0.036(3) 0.060(4) 0.031(3) 0.001(3) 0.021(3) -0.003(3) C1 0.027(3) 0.025(3) 0.028(3) -0.001(3) 0.017(3) -0.003(2) C2 0.038(3) 0.027(3) 0.032(4) -0.001(3) 0.018(3) -0.012(3) C3 0.043(4) 0.033(3) 0.029(3) 0.009(3) 0.016(3) -0.007(3) C4 0.037(3) 0.040(4) 0.027(3) -0.007(3) 0.018(3) -0.015(3) C5 0.041(4) 0.025(3) 0.034(4) 0.000(3) 0.020(3) -0.004(3) C6 0.031(3) 0.024(3) 0.034(3) 0.002(3) 0.020(3) -0.002(2) C7A 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C7 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C8 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C8A 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C9 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C9A 0.045(4) 0.070(5) 0.034(3) -0.007(3) 0.019(3) -0.008(3) C10 0.023(3) 0.029(3) 0.024(3) -0.001(2) 0.015(3) -0.002(2) C11 0.029(3) 0.025(3) 0.036(3) 0.002(3) 0.021(3) 0.000(2) C12 0.027(3) 0.026(3) 0.034(3) -0.008(3) 0.018(3) -0.003(2) C13 0.031(3) 0.024(3) 0.025(3) 0.001(2) 0.017(3) 0.002(2) C14 0.027(3) 0.022(3) 0.031(3) 0.006(3) 0.018(3) 0.003(2) C15 0.030(3) 0.021(3) 0.036(3) 0.002(3) 0.020(3) 0.003(2) C16 0.031(2) 0.055(3) 0.033(2) 0.001(2) 0.021(2) 0.003(2) C17 0.061(5) 0.049(4) 0.072(5) 0.019(4) 0.055(5) 0.008(4) C18 0.058(5) 0.060(5) 0.052(4) -0.017(4) 0.042(4) -0.012(4) C19 0.019(3) 0.025(3) 0.022(3) 0.005(2) 0.011(2) 0.000(2) C20 0.037(3) 0.033(3) 0.036(3) 0.001(3) 0.030(3) 0.003(3) C21 0.044(4) 0.025(3) 0.036(3) 0.001(3) 0.031(3) 0.001(3) C22 0.024(3) 0.029(3) 0.019(3) 0.003(2) 0.012(2) -0.001(2) C23 0.040(3) 0.030(3) 0.045(4) 0.007(3) 0.035(3) 0.007(3) C24 0.035(3) 0.024(3) 0.040(4) -0.001(3) 0.030(3) 0.003(3) C25 0.045(4) 0.046(4) 0.033(4) -0.005(3) 0.021(3) -0.018(3) C26 0.047(4) 0.030(3) 0.034(3) 0.008(3) 0.029(3) 0.003(3) C27 0.074(5) 0.029(3) 0.050(4) 0.005(3) 0.052(4) 0.007(3) C28 0.050(4) 0.089(7) 0.046(5) -0.014(4) 0.029(4) -0.001(4) C29 0.050(4) 0.058(5) 0.038(4) 0.004(3) 0.027(4) -0.018(4) C30 0.041(4) 0.048(4) 0.051(4) 0.007(4) 0.028(4) 0.001(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 Zn1 S2 2.2804(17) . ? Zn1 S1 2.3087(17) . ? Zn1 S3 2.3957(16) . ? Zn1 S3 2.423(2) 2 ? Zn1 Zn1 3.0307(19) 2 ? P1 F4 1.568(5) . ? P1 F6 1.579(5) . ? P1 F2 1.566(5) . ? P1 F3 1.576(5) . ? P1 F5 1.582(5) . ? P1 F1 1.571(5) . ? P2 F8 1.585(5) . ? P2 F9 1.582(4) . ? P2 F7 1.590(4) . ? P2 F11 1.596(4) . ? P2 F12 1.598(4) . ? P2 F10 1.598(4) . ? S1 C1 1.751(6) . ? S2 C10 1.752(6) . ? S3 C19 1.770(6) . ? S3 Zn1 2.423(2) 2 ? O1 C30 1.223(9) . ? O2 H32 0.74(11) . ? O2 H31 0.75(5) . ? N1 C8 1.397(14) . ? N1 C9A 1.45(2) . ? N1 C7A 1.46(2) . ? N1 C7 1.450(15) . ? N1 C4 1.499(8) . ? N1 C9 1.628(14) . ? N1 C8A 1.73(2) . ? N2 C16 1.493(7) . ? N2 C18 1.489(8) . ? N2 C13 1.504(8) . ? N2 C17 1.506(9) . ? N3 C27 1.512(8) . ? N3 C22 1.497(7) . ? N3 C25 1.506(7) . ? N3 C26 1.502(7) . ? N4 C30 1.327(9) . ? N4 C28 1.454(9) . ? N4 C29 1.449(9) . ? C1 C6 1.385(8) . ? C1 C2 1.386(8) . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? C3 C4 1.370(9) . ? C3 H3 0.9500 . ? C4 C5 1.377(9) . ? C5 C6 1.365(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10 C11 1.393(8) . ? C10 C15 1.402(8) . ? C11 C12 1.384(8) . ? C11 H11 0.9500 . ? C12 C13 1.369(8) . ? C12 H12 0.9500 . ? C13 C14 1.381(8) . ? C14 C15 1.382(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.381(8) . ? C19 C20 1.402(8) . ? C20 C21 1.373(8) . ? C20 H20 0.9500 . ? C21 C22 1.392(8) . ? C21 H21 0.9500 . ? C22 C23 1.377(8) . ? C23 C24 1.385(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? 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 S2 Zn1 S1 129.59(6) . . ? S2 Zn1 S3 112.38(6) . . ? S1 Zn1 S3 100.05(6) . . ? S2 Zn1 S3 111.24(6) . 2 ? S1 Zn1 S3 98.38(6) . 2 ? S3 Zn1 S3 101.10(6) . 2 ? S2 Zn1 Zn1 133.98(4) . 2 ? S1 Zn1 Zn1 96.38(4) . 2 ? S3 Zn1 Zn1 51.43(4) . 2 ? S3 Zn1 Zn1 50.63(5) 2 2 ? F4 P1 F6 91.9(3) . . ? F4 P1 F2 89.6(3) . . ? F6 P1 F2 90.8(3) . . ? F4 P1 F3 179.4(3) . . ? F6 P1 F3 88.6(3) . . ? F2 P1 F3 90.7(4) . . ? F4 P1 F5 88.6(3) . . ? F6 P1 F5 179.1(3) . . ? F2 P1 F5 90.0(3) . . ? F3 P1 F5 90.9(3) . . ? F4 P1 F1 89.3(4) . . ? F6 P1 F1 88.7(3) . . ? F2 P1 F1 178.8(4) . . ? F3 P1 F1 90.3(4) . . ? F5 P1 F1 90.6(3) . . ? F8 P2 F9 90.0(3) . . ? F8 P2 F7 179.6(3) . . ? F9 P2 F7 90.4(3) . . ? F8 P2 F11 89.7(2) . . ? F9 P2 F11 90.8(2) . . ? F7 P2 F11 90.3(2) . . ? F8 P2 F12 90.1(2) . . ? F9 P2 F12 89.8(2) . . ? F7 P2 F12 89.9(2) . . ? F11 P2 F12 179.4(2) . . ? F8 P2 F10 90.3(3) . . ? F9 P2 F10 179.7(3) . . ? F7 P2 F10 89.3(3) . . ? F11 P2 F10 89.1(2) . . ? F12 P2 F10 90.3(2) . . ? C1 S1 Zn1 108.2(2) . . ? C10 S2 Zn1 102.8(2) . . ? C19 S3 Zn1 116.72(19) . . ? C19 S3 Zn1 102.91(18) . 2 ? Zn1 S3 Zn1 77.94(6) . 2 ? H32 O2 H31 108(10) . . ? C8 N1 C9A 52.2(10) . . ? C8 N1 C7A 111.1(12) . . ? C9A N1 C7A 129.9(12) . . ? C8 N1 C7 129.8(9) . . ? C9A N1 C7 121.7(10) . . ? C8 N1 C4 109.2(7) . . ? C9A N1 C4 116.9(9) . . ? C7A N1 C4 113.2(10) . . ? C7 N1 C4 113.8(7) . . ? C8 N1 C9 107.2(8) . . ? C9A N1 C9 55.2(10) . . ? C7A N1 C9 109.6(11) . . ? C7 N1 C9 84.7(8) . . ? C4 N1 C9 106.2(6) . . ? C8 N1 C8A 49.3(9) . . ? C9A N1 C8A 99.1(12) . . ? C7A N1 C8A 69.4(12) . . ? C7 N1 C8A 95.3(10) . . ? C4 N1 C8A 103.7(7) . . ? C9 N1 C8A 147.2(9) . . ? C16 N2 C18 109.5(5) . . ? C16 N2 C13 108.6(5) . . ? C18 N2 C13 110.8(5) . . ? C16 N2 C17 107.8(5) . . ? C18 N2 C17 108.2(6) . . ? C13 N2 C17 111.9(5) . . ? C27 N3 C22 111.5(4) . . ? C27 N3 C25 108.5(5) . . ? C22 N3 C25 109.7(4) . . ? C27 N3 C26 107.2(5) . . ? C22 N3 C26 110.9(4) . . ? C25 N3 C26 108.9(5) . . ? C30 N4 C28 121.0(7) . . ? C30 N4 C29 121.5(6) . . ? C28 N4 C29 117.5(6) . . ? C6 C1 C2 117.1(5) . . ? C6 C1 S1 119.1(4) . . ? C2 C1 S1 123.7(4) . . ? C3 C2 C1 122.0(6) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C4 C3 C2 119.0(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 N1 118.7(6) . . ? C5 C4 N1 121.2(6) . . ? C6 C5 C4 120.2(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121.5(6) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N1 C7A H7A1 109.5 . . ? N1 C7A H7A2 109.5 . . ? N1 C7A H7A3 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? N1 C8A H8A1 109.5 . . ? N1 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? N1 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? N1 C9A H9A1 109.5 . . ? N1 C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? N1 C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C11 C10 C15 116.8(5) . . ? C11 C10 S2 119.1(4) . . ? C15 C10 S2 123.9(4) . . ? C12 C11 C10 121.1(6) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 120.7(6) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.9(6) . . ? C12 C13 N2 119.1(5) . . ? C14 C13 N2 120.9(5) . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C10 122.0(5) . . ? C14 C15 H15 119.0 . . ? C10 C15 H15 119.0 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.6(5) . . ? C24 C19 S3 117.4(4) . . ? C20 C19 S3 123.9(4) . . ? C21 C20 C19 121.1(5) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.1(5) . . ? C23 C22 N3 118.6(5) . . ? C21 C22 N3 121.3(5) . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C19 120.5(5) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 N4 124.5(7) . . ? O1 C30 H30 117.8 . . ? N4 C30 H30 117.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H32 O1 0.74(11) 2.18(6) 2.912(9) 166(10) 5_566 O2 H31 O1 0.75(5) 2.11(6) 2.789(8) 152(7) . C3 H3 F2 0.95 2.51 3.454(8) 170.6 7_566 C9 H9B F10 0.98 2.35 3.268(14) 156.5 . C17 H17B F3 0.98 2.52 3.425(17) 152.8 4_545 C26 H26B O2 0.98 2.30 3.247(9) 163.7 5_556 C27 H27B O2 0.98 2.55 3.435(9) 150.0 5_556 C7 H7C F11 0.98 2.40 3.149(15) 132.9 . C26 H26C F9 0.98 2.53 3.461(8) 159.1 5_566 C17 H17B F10 0.98 2.53 2.953(8) 106.1 6_575 C29 H29C O1 0.98 2.38 2.785(8) 104.0 . C9 H9A F6 0.98 2.41 2.989(14) 117.6 7_576 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.099 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 865710' #TrackingRef 'JPLang.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 Cd N3 S3, 2(F6 P), C3 H7 N O' _chemical_formula_sum 'C30 H46 Cd F12 N4 O P2 S3' _chemical_formula_weight 977.27 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' P P 0.1023 0.0942 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.3927(1) _cell_length_b 30.565(6) _cell_length_c 17.713(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.84(3) _cell_angle_gamma 90.00 _cell_volume 3988.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11530 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9029 _exptl_absorpt_correction_T_max 0.9178 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Corp.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rigaku Mercury' _diffrn_measurement_method \w _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 11530 _diffrn_reflns_av_R_equivalents 0.1554 _diffrn_reflns_av_sigmaI/netI 0.1229 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7085 _reflns_number_gt 5725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0091P)^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 SHELXL _refine_ls_extinction_coef 0.00028(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 22354 _refine_ls_number_parameters 496 _refine_ls_number_restraints 243 _refine_ls_R_factor_all 0.1595 _refine_ls_R_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.2329 _refine_ls_wR_factor_gt 0.1902 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.77793(8) 0.005442(16) 0.54865(3) 0.02826(17) Uani 1 1 d . . . S1 S 0.8088(3) 0.02002(6) 0.68857(11) 0.0331(5) Uani 1 1 d . . . S2 S 0.5468(3) 0.04572(5) 0.45894(10) 0.0247(4) Uani 1 1 d . . . S3 S 1.0507(3) 0.05999(5) 0.50151(10) 0.0274(4) Uani 1 1 d . . . C1 C 1.0113(10) -0.0023(2) 0.7302(4) 0.0250(16) Uani 1 1 d . . . C2 C 1.0668(10) 0.0076(2) 0.8040(4) 0.033(2) Uani 1 1 d . . . H2A H 0.9944 0.0270 0.8305 0.039 Uiso 1 1 calc R . . C3 C 1.2205(12) -0.0090(2) 0.8411(4) 0.034(2) Uani 1 1 d . . . H3A H 1.2516 -0.0018 0.8927 0.041 Uiso 1 1 calc R . . C4 C 1.3321(10) -0.0366(2) 0.8027(4) 0.0214(16) Uani 1 1 d . . . C5 C 1.2877(12) -0.0468(2) 0.7278(4) 0.0321(19) Uani 1 1 d . . . H5A H 1.3650 -0.0644 0.7001 0.039 Uiso 1 1 calc R . . C6 C 1.1208(12) -0.0299(2) 0.6937(5) 0.041(2) Uani 1 1 d . . . H6A H 1.0835 -0.0383 0.6431 0.049 Uiso 1 1 calc R . . C7 C 1.6163(13) -0.0182(2) 0.8769(4) 0.041(2) Uani 1 1 d . . . H7A H 1.7276 -0.0300 0.9032 0.062 Uiso 1 1 calc R . . H7B H 1.5484 -0.0020 0.9130 0.062 Uiso 1 1 calc R . . H7C H 1.6478 0.0015 0.8364 0.062 Uiso 1 1 calc R . . C8 C 1.6183(12) -0.0809(2) 0.7938(5) 0.043(2) Uani 1 1 d . . . H8A H 1.7270 -0.0915 0.8238 0.065 Uiso 1 1 calc R . . H8B H 1.6543 -0.0624 0.7525 0.065 Uiso 1 1 calc R . . H8C H 1.5484 -0.1060 0.7725 0.065 Uiso 1 1 calc R . . C9 C 1.4543(13) -0.0837(2) 0.9083(4) 0.036(2) Uani 1 1 d . . . H9A H 1.5657 -0.0955 0.9348 0.055 Uiso 1 1 calc R . . H9B H 1.3780 -0.1080 0.8881 0.055 Uiso 1 1 calc R . . H9C H 1.3880 -0.0666 0.9438 0.055 Uiso 1 1 calc R . . C10 C 0.5327(11) 0.10275(19) 0.4738(4) 0.0250(17) Uani 1 1 d . . . C11 C 0.6386(12) 0.1253(2) 0.5291(4) 0.0308(19) Uani 1 1 d . . . H11A H 0.7220 0.1094 0.5624 0.037 Uiso 1 1 calc R . . C12 C 0.6271(10) 0.1705(2) 0.5376(4) 0.0280(18) Uani 1 1 d . . . H12A H 0.6992 0.1854 0.5765 0.034 Uiso 1 1 calc R . . C13 C 0.5098(11) 0.1926(2) 0.4885(4) 0.033(2) Uani 1 1 d . B . C14 C 0.3945(11) 0.1711(2) 0.4335(4) 0.031(2) Uani 1 1 d . . . H14A H 0.3072 0.1870 0.4021 0.038 Uiso 1 1 calc R . . C15 C 0.4105(14) 0.1263(3) 0.4259(5) 0.0537(11) Uani 1 1 d . . . H15A H 0.3371 0.1115 0.3874 0.064 Uiso 1 1 calc R . . C19 C 1.1788(9) 0.0816(2) 0.5827(4) 0.0218(16) Uani 1 1 d . . . C20 C 1.3026(10) 0.0579(2) 0.6260(4) 0.0255(17) Uani 1 1 d . . . H20A H 1.3271 0.0286 0.6118 0.031 Uiso 1 1 calc R . . C21 C 1.3959(12) 0.0756(2) 0.6914(4) 0.0299(18) Uani 1 1 d . . . H21A H 1.4830 0.0587 0.7211 0.036 Uiso 1 1 calc R . . C22 C 1.3591(11) 0.1174(2) 0.7113(4) 0.0323(19) Uani 1 1 d . A . C23 C 1.2401(10) 0.1422(2) 0.6670(4) 0.033(2) Uani 1 1 d . . . H23A H 1.2171 0.1716 0.6808 0.040 Uiso 1 1 calc R . . C24 C 1.1538(14) 0.1250(3) 0.6027(5) 0.0537(11) Uani 1 1 d . . . H24A H 1.0751 0.1430 0.5709 0.064 Uiso 1 1 calc R . . C25 C 1.3351(14) 0.1637(3) 0.8238(5) 0.0537(11) Uani 1 1 d . A 1 H25A H 1.4024 0.1763 0.8687 0.081 Uiso 1 1 calc R A 1 H25B H 1.2375 0.1450 0.8396 0.081 Uiso 1 1 calc R A 1 H25C H 1.2829 0.1873 0.7915 0.081 Uiso 1 1 calc R A 1 C26 C 1.6050(15) 0.1665(3) 0.7583(5) 0.0537(11) Uani 1 1 d . A 1 H26A H 1.6687 0.1790 0.8041 0.081 Uiso 1 1 calc R A 1 H26B H 1.5491 0.1901 0.7269 0.081 Uiso 1 1 calc R A 1 H26C H 1.6916 0.1506 0.7295 0.081 Uiso 1 1 calc R A 1 C27 C 1.5450(14) 0.1039(2) 0.8327(4) 0.0537(11) Uani 1 1 d . A 1 H27A H 1.6098 0.1188 0.8759 0.081 Uiso 1 1 calc R A 1 H27B H 1.6303 0.0857 0.8071 0.081 Uiso 1 1 calc R A 1 H27C H 1.4492 0.0854 0.8507 0.081 Uiso 1 1 calc R A 1 C28 C -0.0118(19) 0.1465(3) 0.2447(6) 0.081(3) Uani 1 1 d . . . H28A H 0.0460 0.1633 0.2061 0.121 Uiso 1 1 calc R . . H28B H -0.1338 0.1376 0.2245 0.121 Uiso 1 1 calc R . . H28C H 0.0610 0.1205 0.2584 0.121 Uiso 1 1 calc R . . C29 C -0.1052(16) 0.1555(3) 0.3724(5) 0.071(3) Uani 1 1 d . . . H29A H -0.1034 0.1774 0.4128 0.107 Uiso 1 1 calc R . . H29B H -0.0375 0.1295 0.3910 0.107 Uiso 1 1 calc R . . H29C H -0.2310 0.1473 0.3569 0.107 Uiso 1 1 calc R . . C30 C 0.0154(17) 0.2154(3) 0.3090(7) 0.078(4) Uani 1 1 d . . . H30A H 0.0538 0.2272 0.2633 0.094 Uiso 1 1 calc R . . P1 P 0.9958(3) 0.09800(7) 0.98094(12) 0.0355(6) Uani 1 1 d . . . P2 P 0.5122(4) 0.22619(11) 0.1916(2) 0.0573(9) Uani 1 1 d D . . F1 F 1.0066(8) 0.08387(15) 1.0666(2) 0.0542(14) Uani 1 1 d . . . F2 F 1.1425(9) 0.13541(16) 1.0006(4) 0.0708(18) Uani 1 1 d . . . F3 F 0.8379(8) 0.13168(15) 0.9954(3) 0.0573(15) Uani 1 1 d . . . F4 F 1.1551(8) 0.06434(15) 0.9658(3) 0.0555(15) Uani 1 1 d . . . F5 F 0.8488(8) 0.06134(15) 0.9585(3) 0.0573(15) Uani 1 1 d . . . F6 F 0.9852(8) 0.11245(17) 0.8940(3) 0.0690(17) Uani 1 1 d . . . F7 F 0.712(2) 0.2453(8) 0.1989(11) 0.088(2) Uani 0.406(7) 1 d PDU B 1 F8 F 0.561(3) 0.1974(10) 0.2644(14) 0.088(2) Uani 0.406(7) 1 d PDU B 1 F9 F 0.536(4) 0.1956(8) 0.1248(12) 0.112(6) Uani 0.406(7) 1 d PDU B 1 F10 F 0.3012(17) 0.2239(8) 0.1997(14) 0.112(6) Uani 0.406(7) 1 d PDU B 1 F11 F 0.470(4) 0.2685(5) 0.1411(12) 0.085(6) Uani 0.406(7) 1 d PDU B 1 F12 F 0.504(4) 0.2581(7) 0.2640(9) 0.129(6) Uani 0.406(7) 1 d PDU B 1 F7A F 0.687(2) 0.2490(6) 0.2272(7) 0.088(2) Uani 0.594(7) 1 d PDU B 2 F8A F 0.501(2) 0.1942(6) 0.2587(9) 0.088(2) Uani 0.594(7) 1 d PDU B 2 F9A F 0.6446(18) 0.1914(4) 0.1610(8) 0.093(5) Uani 0.594(7) 1 d PDU B 2 F10A F 0.3549(19) 0.1969(4) 0.1500(7) 0.081(4) Uani 0.594(7) 1 d PDU B 2 F11A F 0.521(2) 0.2531(4) 0.1138(6) 0.076(5) Uani 0.594(7) 1 d PDU B 2 F12A F 0.384(2) 0.2603(4) 0.2218(8) 0.100(4) Uani 0.594(7) 1 d PDU B 2 N1 N 1.5028(9) -0.0547(2) 0.8438(3) 0.0326(16) Uani 1 1 d . . . N2 N 0.4979(9) 0.2428(2) 0.4936(4) 0.043(2) Uani 1 1 d D . . N3 N 1.4640(9) 0.13640(18) 0.7797(3) 0.0312(16) Uani 1 1 d . . . N4 N -0.0245(11) 0.1730(2) 0.3102(4) 0.051(2) Uani 1 1 d . . . O1 O 0.0063(15) 0.2407(2) 0.3630(4) 0.104(4) Uani 1 1 d . . . C16 C 0.303(2) 0.2537(8) 0.5120(14) 0.0537(11) Uani 0.406(7) 1 d PDU B 1 H16A H 0.2312 0.2267 0.5114 0.081 Uiso 0.406(7) 1 calc PR B 1 H16B H 0.2481 0.2740 0.4739 0.081 Uiso 0.406(7) 1 calc PR B 1 H16C H 0.3060 0.2672 0.5622 0.081 Uiso 0.406(7) 1 calc PR B 1 C17 C 0.494(4) 0.2596(7) 0.4134(9) 0.0537(11) Uani 0.406(7) 1 d PDU B 1 H17A H 0.3700 0.2579 0.3893 0.081 Uiso 0.406(7) 1 calc PR B 1 H17B H 0.5748 0.2418 0.3848 0.081 Uiso 0.406(7) 1 calc PR B 1 H17C H 0.5350 0.2901 0.4139 0.081 Uiso 0.406(7) 1 calc PR B 1 C18 C 0.617(4) 0.2612(7) 0.5564(13) 0.064(8) Uani 0.406(7) 1 d PDU B 1 H18A H 0.5530 0.2610 0.6028 0.097 Uiso 0.406(7) 1 calc PR B 1 H18B H 0.6490 0.2913 0.5442 0.097 Uiso 0.406(7) 1 calc PR B 1 H18C H 0.7272 0.2435 0.5642 0.097 Uiso 0.406(7) 1 calc PR B 1 C16A C 0.368(2) 0.2633(5) 0.4361(8) 0.0537(11) Uani 0.594(7) 1 d PDU B 2 H16D H 0.2446 0.2537 0.4439 0.081 Uiso 0.594(7) 1 calc PR B 2 H16E H 0.3981 0.2547 0.3853 0.081 Uiso 0.594(7) 1 calc PR B 2 H16F H 0.3758 0.2953 0.4409 0.081 Uiso 0.594(7) 1 calc PR B 2 C17A C 0.6910(17) 0.2582(5) 0.4777(10) 0.0537(11) Uani 0.594(7) 1 d PDU B 2 H17D H 0.7618 0.2331 0.4624 0.081 Uiso 0.594(7) 1 calc PR B 2 H17E H 0.7513 0.2713 0.5236 0.081 Uiso 0.594(7) 1 calc PR B 2 H17F H 0.6820 0.2800 0.4369 0.081 Uiso 0.594(7) 1 calc PR B 2 C18A C 0.471(3) 0.2566(5) 0.5718(9) 0.064(5) Uani 0.594(7) 1 d PDU B 2 H18D H 0.3503 0.2471 0.5848 0.097 Uiso 0.594(7) 1 calc PR B 2 H18E H 0.4792 0.2885 0.5756 0.097 Uiso 0.594(7) 1 calc PR B 2 H18F H 0.5640 0.2432 0.6071 0.097 Uiso 0.594(7) 1 calc PR B 2 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 0.0217(3) 0.0338(3) 0.0284(3) -0.0018(2) -0.0026(3) 0.0061(3) S1 0.0208(11) 0.0515(12) 0.0264(11) -0.0020(9) -0.0009(10) 0.0072(9) S2 0.0177(9) 0.0219(9) 0.0336(11) -0.0014(7) -0.0034(10) 0.0003(7) S3 0.0246(10) 0.0250(10) 0.0321(11) -0.0018(8) -0.0010(11) 0.0016(8) C1 0.017(4) 0.037(4) 0.021(4) 0.004(3) 0.002(4) 0.002(4) C2 0.019(5) 0.044(5) 0.036(5) -0.015(4) 0.004(4) 0.009(4) C3 0.027(5) 0.057(5) 0.017(4) -0.012(4) -0.001(4) -0.008(4) C4 0.010(4) 0.045(5) 0.009(4) 0.003(3) 0.001(3) 0.005(3) C5 0.025(5) 0.032(5) 0.040(5) 0.002(3) 0.004(5) 0.007(4) C6 0.040(5) 0.041(5) 0.041(5) -0.004(4) 0.003(5) 0.001(4) C7 0.034(5) 0.031(4) 0.057(6) 0.000(4) -0.010(5) 0.008(4) C8 0.034(5) 0.035(5) 0.060(6) -0.001(4) 0.005(5) 0.015(4) C9 0.040(5) 0.035(4) 0.033(5) 0.012(3) -0.005(5) 0.009(4) C10 0.025(4) 0.014(4) 0.037(4) 0.000(3) 0.012(4) 0.010(3) C11 0.036(5) 0.022(4) 0.033(4) 0.004(3) -0.010(4) 0.003(4) C12 0.027(5) 0.036(4) 0.019(4) 0.007(3) -0.006(4) 0.007(3) C13 0.036(5) 0.025(4) 0.039(5) -0.001(3) 0.012(4) -0.003(4) C14 0.036(5) 0.017(4) 0.041(5) 0.004(3) -0.002(4) 0.012(3) C15 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C19 0.007(3) 0.024(4) 0.035(4) -0.010(3) 0.002(4) 0.002(3) C20 0.023(4) 0.018(4) 0.036(5) 0.000(3) 0.006(4) -0.003(3) C21 0.039(5) 0.022(4) 0.029(4) 0.009(3) 0.004(4) 0.011(4) C22 0.034(5) 0.036(4) 0.026(4) -0.004(3) -0.002(4) -0.005(4) C23 0.027(5) 0.022(4) 0.050(5) -0.012(3) -0.005(4) 0.011(3) C24 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C25 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C26 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C27 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C28 0.078(9) 0.075(7) 0.095(9) -0.002(6) 0.035(9) 0.008(7) C29 0.072(8) 0.063(6) 0.082(8) 0.033(6) 0.028(7) 0.011(6) C30 0.065(7) 0.051(7) 0.115(10) 0.044(6) -0.021(9) -0.013(6) P1 0.0291(13) 0.0336(13) 0.0433(14) 0.0040(10) -0.0003(11) 0.0006(10) P2 0.0363(17) 0.070(2) 0.065(2) 0.0209(17) 0.0000(17) -0.0029(15) F1 0.059(4) 0.061(3) 0.043(3) 0.012(2) 0.005(3) 0.009(3) F2 0.052(3) 0.044(3) 0.114(5) -0.001(3) -0.011(4) -0.020(3) F3 0.048(3) 0.037(3) 0.085(4) 0.000(3) -0.003(4) 0.014(3) F4 0.046(3) 0.046(3) 0.072(4) -0.019(3) -0.009(4) 0.014(3) F5 0.042(3) 0.046(3) 0.082(4) -0.011(3) -0.002(4) -0.010(3) F6 0.052(4) 0.108(4) 0.046(3) 0.032(3) 0.002(3) 0.000(3) F7 0.075(5) 0.108(4) 0.075(4) 0.047(4) -0.024(5) -0.028(5) F8 0.075(5) 0.108(4) 0.075(4) 0.047(4) -0.024(5) -0.028(5) F9 0.132(13) 0.103(10) 0.096(13) -0.045(9) -0.013(12) -0.027(12) F10 0.054(9) 0.144(13) 0.133(13) 0.015(11) -0.027(11) -0.040(10) F11 0.082(13) 0.057(9) 0.110(13) 0.037(9) -0.018(11) -0.031(9) F12 0.136(13) 0.157(11) 0.097(12) 0.005(10) 0.028(12) 0.009(12) F7A 0.075(5) 0.108(4) 0.075(4) 0.047(4) -0.024(5) -0.028(5) F8A 0.075(5) 0.108(4) 0.075(4) 0.047(4) -0.024(5) -0.028(5) F9A 0.078(9) 0.076(7) 0.122(12) -0.051(8) -0.001(9) 0.006(8) F10A 0.093(8) 0.065(7) 0.078(8) 0.004(5) -0.031(8) -0.047(7) F11A 0.058(9) 0.110(10) 0.057(7) 0.030(7) -0.014(7) -0.010(7) F12A 0.085(8) 0.091(7) 0.125(10) 0.004(7) 0.023(9) 0.017(7) N1 0.027(4) 0.042(4) 0.028(4) 0.000(3) -0.003(4) 0.003(3) N2 0.052(5) 0.022(4) 0.054(5) 0.000(3) -0.005(4) 0.007(4) N3 0.033(4) 0.031(4) 0.028(4) -0.009(3) 0.000(3) -0.007(3) N4 0.049(5) 0.050(5) 0.055(5) 0.007(4) 0.005(5) 0.000(4) O1 0.125(8) 0.059(5) 0.115(7) -0.021(4) -0.065(8) -0.004(6) C16 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C17 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C18 0.099(19) 0.019(11) 0.066(15) 0.007(10) -0.042(16) 0.010(12) C16A 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C17A 0.050(2) 0.054(2) 0.055(2) -0.0098(19) -0.010(2) -0.003(2) C18A 0.054(12) 0.043(10) 0.099(14) -0.031(9) 0.021(12) 0.004(9) _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 S1 2.510(2) . ? Cd1 S2 2.5497(19) . ? Cd1 S3 2.5658(19) 3_756 ? Cd1 S3 2.798(2) . ? Cd1 S2 2.8589(19) 3_656 ? S1 C1 1.751(7) . ? S2 C10 1.767(6) . ? S2 Cd1 2.8589(19) 3_656 ? S3 C19 1.780(7) . ? S3 Cd1 2.5658(19) 3_756 ? C1 C6 1.368(11) . ? C1 C2 1.370(9) . ? C2 C3 1.362(11) . ? C2 H2A 0.9500 . ? C3 C4 1.397(10) . ? C3 H3A 0.9500 . ? C4 C5 1.374(9) . ? C4 N1 1.507(9) . ? C5 C6 1.425(12) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 N1 1.486(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.513(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.514(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.388(11) . ? C10 C11 1.385(9) . ? C11 C12 1.393(8) . ? C11 H11A 0.9500 . ? C12 C13 1.355(10) . ? C12 H12A 0.9500 . ? C13 C14 1.403(10) . ? C13 N2 1.539(9) . ? C14 C15 1.381(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C19 C20 1.353(9) . ? C19 C24 1.391(9) . ? C20 C21 1.406(9) . ? C20 H20A 0.9500 . ? C21 C22 1.358(9) . ? C21 H21A 0.9500 . ? C22 C23 1.361(10) . ? C22 N3 1.500(8) . ? C23 C24 1.363(10) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 N3 1.530(11) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N3 1.464(11) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N3 1.459(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N4 1.423(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N4 1.403(11) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O1 1.236(12) . ? C30 N4 1.331(10) . ? C30 H30A 0.9500 . ? P1 F1 1.572(5) . ? P1 F5 1.588(5) . ? P1 F3 1.593(6) . ? P1 F6 1.598(5) . ? P1 F2 1.594(6) . ? P1 F4 1.603(5) . ? P2 F9 1.529(13) . ? P2 F12A 1.534(10) . ? P2 F8A 1.547(9) . ? P2 F7A 1.553(11) . ? P2 F8 1.579(12) . ? P2 F9A 1.572(10) . ? P2 F11 1.587(12) . ? P2 F10 1.580(13) . ? P2 F7 1.584(13) . ? P2 F10A 1.596(9) . ? P2 F11A 1.609(9) . ? P2 F12 1.617(12) . ? N2 C18 1.470(14) . ? N2 C18A 1.478(12) . ? N2 C16A 1.479(11) . ? N2 C17 1.509(13) . ? N2 C16 1.539(14) . ? N2 C17A 1.552(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? 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 S1 Cd1 S2 122.01(7) . . ? S1 Cd1 S3 118.29(6) . 3_756 ? S2 Cd1 S3 119.01(6) . 3_756 ? S1 Cd1 S3 100.44(7) . . ? S2 Cd1 S3 89.33(6) . . ? S3 Cd1 S3 88.38(6) 3_756 . ? S1 Cd1 S2 98.60(7) . 3_656 ? S2 Cd1 S2 73.67(6) . 3_656 ? S3 Cd1 S2 89.69(6) 3_756 3_656 ? S3 Cd1 S2 159.31(6) . 3_656 ? C1 S1 Cd1 110.5(2) . . ? C10 S2 Cd1 115.4(3) . . ? C10 S2 Cd1 119.1(3) . 3_656 ? Cd1 S2 Cd1 106.33(6) . 3_656 ? C19 S3 Cd1 108.9(2) . 3_756 ? C19 S3 Cd1 109.1(2) . . ? Cd1 S3 Cd1 91.62(6) 3_756 . ? C6 C1 C2 116.4(7) . . ? C6 C1 S1 124.1(6) . . ? C2 C1 S1 119.4(6) . . ? C3 C2 C1 123.2(7) . . ? C3 C2 H2A 118.4 . . ? C1 C2 H2A 118.4 . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.2(7) . . ? C5 C4 N1 120.4(7) . . ? C3 C4 N1 119.4(6) . . ? C4 C5 C6 117.0(8) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C1 C6 C5 123.3(8) . . ? C1 C6 H6A 118.3 . . ? C5 C6 H6A 118.3 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.3(6) . . ? C15 C10 S2 117.7(6) . . ? C11 C10 S2 124.0(6) . . ? C10 C11 C12 122.3(7) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 117.8(7) . . ? C13 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C12 C13 C14 122.0(7) . . ? C12 C13 N2 119.7(7) . . ? C14 C13 N2 118.3(7) . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C10 C15 C14 120.7(8) . . ? C10 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C20 C19 C24 117.7(7) . . ? C20 C19 S3 123.2(5) . . ? C24 C19 S3 119.1(6) . . ? C19 C20 C21 121.5(6) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C22 C21 C20 118.8(7) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C21 C22 C23 120.6(7) . . ? C21 C22 N3 118.2(7) . . ? C23 C22 N3 121.0(6) . . ? C24 C23 C22 120.1(7) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C19 121.2(8) . . ? C23 C24 H24A 119.4 . . ? C19 C24 H24A 119.4 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 N4 124.9(11) . . ? O1 C30 H30A 117.6 . . ? N4 C30 H30A 117.6 . . ? F1 P1 F5 91.5(3) . . ? F1 P1 F3 90.1(3) . . ? F5 P1 F3 90.1(3) . . ? F1 P1 F6 179.9(4) . . ? F5 P1 F6 88.7(3) . . ? F3 P1 F6 89.9(3) . . ? F1 P1 F2 90.5(3) . . ? F5 P1 F2 178.0(3) . . ? F3 P1 F2 89.7(3) . . ? F6 P1 F2 89.4(3) . . ? F1 P1 F4 90.4(3) . . ? F5 P1 F4 90.1(3) . . ? F3 P1 F4 179.5(4) . . ? F6 P1 F4 89.6(3) . . ? F2 P1 F4 90.1(3) . . ? F9 P2 F12A 143.2(12) . . ? F9 P2 F8A 103.0(14) . . ? F12A P2 F8A 95.0(11) . . ? F9 P2 F7A 116.2(13) . . ? F12A P2 F7A 93.9(9) . . ? F8A P2 F7A 93.8(7) . . ? F9 P2 F8 104.9(17) . . ? F12A P2 F8 101.4(14) . . ? F7A P2 F8 78.2(9) . . ? F12A P2 F9A 179.5(8) . . ? F8A P2 F9A 85.0(11) . . ? F7A P2 F9A 85.6(9) . . ? F8 P2 F9A 78.4(14) . . ? F9 P2 F11 95.3(13) . . ? F12A P2 F11 63.0(9) . . ? F8A P2 F11 158.0(14) . . ? F7A P2 F11 88.8(11) . . ? F8 P2 F11 159.2(16) . . ? F9A P2 F11 117.0(11) . . ? F9 P2 F10 102.9(14) . . ? F12A P2 F10 50.0(9) . . ? F8A P2 F10 77.6(10) . . ? F7A P2 F10 140.9(12) . . ? F8 P2 F10 93.3(13) . . ? F9A P2 F10 130.5(11) . . ? F11 P2 F10 86.6(13) . . ? F9 P2 F7 97.0(14) . . ? F12A P2 F7 108.5(12) . . ? F8A P2 F7 106.2(9) . . ? F8 P2 F7 89.6(10) . . ? F9A P2 F7 71.0(11) . . ? F11 P2 F7 83.2(12) . . ? F10 P2 F7 158.4(15) . . ? F9 P2 F10A 55.1(11) . . ? F12A P2 F10A 95.5(8) . . ? F8A P2 F10A 85.2(7) . . ? F7A P2 F10A 170.6(9) . . ? F8 P2 F10A 99.8(10) . . ? F9A P2 F10A 85.0(7) . . ? F11 P2 F10A 95.6(10) . . ? F10 P2 F10A 48.0(9) . . ? F7 P2 F10A 151.9(12) . . ? F9 P2 F11A 68.6(11) . . ? F12A P2 F11A 91.2(7) . . ? F8A P2 F11A 171.5(10) . . ? F7A P2 F11A 91.6(7) . . ? F8 P2 F11A 164.2(11) . . ? F9A P2 F11A 88.9(8) . . ? F10 P2 F11A 102.2(11) . . ? F7 P2 F11A 77.2(9) . . ? F10A P2 F11A 88.3(7) . . ? F9 P2 F12 175.4(15) . . ? F8A P2 F12 76.2(13) . . ? F7A P2 F12 59.4(12) . . ? F8 P2 F12 73.0(15) . . ? F9A P2 F12 138.3(11) . . ? F11 P2 F12 86.4(11) . . ? F10 P2 F12 81.5(14) . . ? F7 P2 F12 78.9(15) . . ? F10A P2 F12 129.1(13) . . ? F11A P2 F12 112.2(10) . . ? C7 N1 C8 107.5(7) . . ? C7 N1 C9 107.8(6) . . ? C8 N1 C9 108.2(6) . . ? C7 N1 C4 109.8(6) . . ? C8 N1 C4 113.6(5) . . ? C9 N1 C4 109.8(6) . . ? C18 N2 C18A 45.7(16) . . ? C18 N2 C16A 132.1(11) . . ? C18A N2 C16A 113.2(11) . . ? C18 N2 C17 123.0(16) . . ? C18A N2 C17 142.4(12) . . ? C18 N2 C16 105.5(16) . . ? C18A N2 C16 62.4(12) . . ? C16A N2 C16 59.4(11) . . ? C17 N2 C16 100.5(15) . . ? C18 N2 C17A 61.4(15) . . ? C18A N2 C17A 106.6(12) . . ? C16A N2 C17A 107.4(10) . . ? C17 N2 C17A 70.7(12) . . ? C16 N2 C17A 149.9(13) . . ? C18 N2 C13 113.0(10) . . ? C18A N2 C13 110.6(8) . . ? C16A N2 C13 114.8(8) . . ? C17 N2 C13 106.3(9) . . ? C16 N2 C13 106.7(11) . . ? C17A N2 C13 103.5(8) . . ? C27 N3 C26 109.4(7) . . ? C27 N3 C22 114.3(6) . . ? C26 N3 C22 111.4(6) . . ? C27 N3 C25 106.3(6) . . ? C26 N3 C25 106.1(6) . . ? C22 N3 C25 108.8(6) . . ? C30 N4 C29 119.5(9) . . ? C30 N4 C28 120.8(9) . . ? C29 N4 C28 119.0(8) . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.4 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C16A H16D 109.5 . . ? N2 C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? N2 C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? N2 C17A H17D 109.5 . . ? N2 C17A H17E 109.4 . . ? H17D C17A H17E 109.5 . . ? N2 C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? N2 C18A H18D 109.5 . . ? N2 C18A H18E 109.4 . . ? H18D C18A H18E 109.5 . . ? N2 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3A F4 0.95 2.54 3.213(9) 128.3 . C25 H25B F6 0.98 2.39 3.351(11) 167.9 . C29 H29A O1 0.98 2.30 2.742(11) 106.1 . C6 H6A S3 0.95 2.75 3.698(9) 175.5 3_756 C20 H20A S2 0.95 2.79 3.717(7) 164.2 3_756 C16A H16F F3 0.98 2.46 3.389(15) 158.5 4_565 C17A H17E F10A 0.98 2.50 3.47(2) 170.4 4_666 C23 H23A F7A 0.95 2.58 3.524(17) 174.0 4_666 C25 H25C F7A 0.98 2.34 3.308(17) 170.8 4_666 C18A H18D F11A 0.98 2.53 3.48(3) 162.8 4_566 C21 H21A S1 0.95 2.79 3.498(8) 132.4 1_655 C28 H28B F9A 0.98 2.52 3.146(18) 121.7 1_455 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.109 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.127 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 865711' #TrackingRef '- JPLang (revsied).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H78 Hg2 N6 S6, 2(C3 H7 N O), 4(F6 P), 2(H2 O)' _chemical_formula_sum 'C60 H96 F24 Hg2 N8 O4 P4 S6' _chemical_formula_weight 2166.93 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.285(8) _cell_length_b 9.6841(19) _cell_length_c 29.024(6) _cell_angle_alpha 90.00 _cell_angle_beta 130.91(3) _cell_angle_gamma 90.00 _cell_volume 8345(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 13576 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4304 _exptl_absorpt_coefficient_mu 4.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2970 _exptl_absorpt_correction_T_max 0.6738 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Rikagu Mercury' _diffrn_measurement_method \w _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 39512 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7627 _reflns_number_gt 6736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The distance between H atom and O atom of the water solvent molecule was fixed to be 0.82 /%A. The U~ij~ values of N2 and C13 atoms were restrained by the EADP instruction. ; _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^)+(0.0534P)^2^+168.3106P] 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 7627 _refine_ls_number_parameters 435 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _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 Hg1 Hg 0.057191(12) 0.40331(4) 0.299870(17) 0.04208(15) Uani 1 1 d . . . S1 S 0.00407(8) 0.4302(2) 0.32352(10) 0.0352(5) Uani 1 1 d . . . S2 S 0.06029(8) 0.1482(3) 0.30047(10) 0.0379(5) Uani 1 1 d . . . S3 S 0.10912(8) 0.5919(3) 0.33187(12) 0.0430(6) Uani 1 1 d . . . N1 N -0.0197(3) 1.0079(8) 0.3768(3) 0.0374(18) Uani 1 1 d . . . N2 N 0.2358(4) -0.0106(14) 0.5450(5) 0.085(2) Uani 1 1 d . . . N3 N 0.1837(4) 0.5011(13) 0.2066(5) 0.0744(18) Uani 1 1 d . . . N4 N 0.1024(4) 0.5404(13) 0.4935(5) 0.0691(17) Uani 1 1 d . . . C1 C -0.0034(3) 0.6002(9) 0.3357(4) 0.0318(19) Uani 1 1 d . . . C2 C -0.0252(4) 0.6228(10) 0.3573(5) 0.044(2) Uani 1 1 d . . . H2 H -0.0369 0.5465 0.3637 0.053 Uiso 1 1 calc R . . C3 C -0.0306(4) 0.7562(11) 0.3700(5) 0.046(2) Uani 1 1 d . . . H3 H -0.0461 0.7695 0.3846 0.055 Uiso 1 1 calc R . . C4 C -0.0138(3) 0.8677(9) 0.3618(4) 0.0319(19) Uani 1 1 d . . . C5 C 0.0069(4) 0.8475(10) 0.3386(4) 0.041(2) Uani 1 1 d . . . H5 H 0.0174 0.9248 0.3309 0.049 Uiso 1 1 calc R . . C6 C 0.0127(4) 0.7165(11) 0.3263(5) 0.044(2) Uani 1 1 d . . . H6 H 0.0278 0.7047 0.3112 0.053 Uiso 1 1 calc R . . C7 C -0.0090(4) 1.0069(11) 0.4371(4) 0.046(3) Uani 1 1 d . . . H7A H -0.0312 0.9499 0.4337 0.068 Uiso 1 1 calc R . . H7B H -0.0102 1.1015 0.4481 0.068 Uiso 1 1 calc R . . H7C H 0.0212 0.9687 0.4687 0.068 Uiso 1 1 calc R . . C8 C -0.0667(4) 1.0558(13) 0.3286(5) 0.068(4) Uani 1 1 d . . . H8A H -0.0730 1.0652 0.2900 0.103 Uiso 1 1 calc R . . H8B H -0.0707 1.1454 0.3402 0.103 Uiso 1 1 calc R . . H8C H -0.0875 0.9884 0.3236 0.103 Uiso 1 1 calc R . . C9 C 0.0115(5) 1.1115(10) 0.3831(6) 0.064(4) Uani 1 1 d . . . H9A H 0.0428 1.0828 0.4159 0.096 Uiso 1 1 calc R . . H9B H 0.0066 1.2022 0.3928 0.096 Uiso 1 1 calc R . . H9C H 0.0056 1.1173 0.3447 0.096 Uiso 1 1 calc R . . C10 C 0.1114(3) 0.1085(9) 0.3725(4) 0.0297(18) Uani 1 1 d . . . C11 C 0.1250(4) -0.0295(11) 0.3842(4) 0.047(3) Uani 1 1 d . . . H11 H 0.1064 -0.0971 0.3536 0.057 Uiso 1 1 calc R . . C12 C 0.1655(4) -0.0694(10) 0.4402(5) 0.049(3) Uani 1 1 d . . . H12 H 0.1749 -0.1631 0.4472 0.058 Uiso 1 1 calc R . . C13 C 0.1917(5) 0.0273(18) 0.4850(6) 0.085(2) Uani 1 1 d . . . C14 C 0.1789(3) 0.1623(11) 0.4753(5) 0.048(3) Uani 1 1 d . . . H14 H 0.1970 0.2289 0.5066 0.057 Uiso 1 1 calc R . . C15 C 0.1390(3) 0.2002(10) 0.4189(4) 0.042(2) Uani 1 1 d . . . H15 H 0.1304 0.2946 0.4120 0.051 Uiso 1 1 calc R . . C16 C 0.2414(5) -0.1600(17) 0.5576(6) 0.085(2) Uani 1 1 d . . . H16A H 0.2372 -0.2092 0.5247 0.127 Uiso 1 1 calc R . . H16B H 0.2190 -0.1920 0.5602 0.127 Uiso 1 1 calc R . . H16C H 0.2717 -0.1782 0.5964 0.127 Uiso 1 1 calc R . . C17 C 0.2430(5) 0.0539(17) 0.5964(6) 0.085(2) Uani 1 1 d . . . H17A H 0.2721 0.0238 0.6347 0.127 Uiso 1 1 calc R . . H17B H 0.2188 0.0264 0.5960 0.127 Uiso 1 1 calc R . . H17C H 0.2430 0.1545 0.5930 0.127 Uiso 1 1 calc R . . C18 C 0.2723(5) 0.0389(17) 0.5479(6) 0.085(2) Uani 1 1 d . . . H18A H 0.2685 0.1381 0.5389 0.127 Uiso 1 1 calc R . . H18B H 0.2715 -0.0107 0.5178 0.127 Uiso 1 1 calc R . . H18C H 0.3012 0.0227 0.5888 0.127 Uiso 1 1 calc R . . C19 C 0.1282(3) 0.5602(10) 0.2929(4) 0.038(2) Uani 1 1 d . . . C20 C 0.1300(3) 0.4287(10) 0.2738(5) 0.041(2) Uani 1 1 d . . . H20 H 0.1190 0.3512 0.2808 0.049 Uiso 1 1 calc R . . C21 C 0.1471(3) 0.4094(10) 0.2453(4) 0.042(2) Uani 1 1 d . . . H21 H 0.1482 0.3194 0.2333 0.050 Uiso 1 1 calc R . . C22 C 0.1626(3) 0.5203(10) 0.2342(4) 0.040(2) Uani 1 1 d . . . C23 C 0.1615(3) 0.6530(10) 0.2524(4) 0.042(2) Uani 1 1 d . . . H23 H 0.1726 0.7300 0.2456 0.050 Uiso 1 1 calc R . . C24 C 0.1442(3) 0.6698(10) 0.2800(4) 0.043(2) Uani 1 1 d . . . H24 H 0.1428 0.7605 0.2911 0.051 Uiso 1 1 calc R . . C25 C 0.1661(5) 0.6026(15) 0.1568(6) 0.0744(18) Uani 1 1 d . . . H25A H 0.1332 0.5966 0.1265 0.112 Uiso 1 1 calc R . . H25B H 0.1785 0.5819 0.1374 0.112 Uiso 1 1 calc R . . H25C H 0.1750 0.6961 0.1739 0.112 Uiso 1 1 calc R . . C26 C 0.1750(5) 0.3623(16) 0.1787(6) 0.0744(18) Uani 1 1 d . . . H26A H 0.1897 0.2915 0.2106 0.112 Uiso 1 1 calc R . . H26B H 0.1872 0.3590 0.1581 0.112 Uiso 1 1 calc R . . H26C H 0.1425 0.3452 0.1490 0.112 Uiso 1 1 calc R . . C27 C 0.2331(5) 0.5168(16) 0.2547(6) 0.0744(18) Uani 1 1 d . . . H27A H 0.2399 0.6060 0.2752 0.112 Uiso 1 1 calc R . . H27B H 0.2469 0.5128 0.2364 0.112 Uiso 1 1 calc R . . H27C H 0.2451 0.4421 0.2846 0.112 Uiso 1 1 calc R . . C28 C 0.1065(4) 0.3879(14) 0.4956(6) 0.0691(17) Uani 1 1 d . . . H28A H 0.0918 0.3479 0.5097 0.104 Uiso 1 1 calc R . . H28B H 0.1384 0.3621 0.5237 0.104 Uiso 1 1 calc R . . H28C H 0.0919 0.3530 0.4547 0.104 Uiso 1 1 calc R . . C29 C 0.1229(4) 0.6199(15) 0.4750(6) 0.0691(17) Uani 1 1 d . . . H29A H 0.1192 0.7187 0.4781 0.104 Uiso 1 1 calc R . . H29B H 0.1083 0.5972 0.4328 0.104 Uiso 1 1 calc R . . H29C H 0.1551 0.5978 0.5017 0.104 Uiso 1 1 calc R . . C30 C 0.0795(4) 0.6017(16) 0.5063(6) 0.0691(17) Uani 1 1 d . . . H30A H 0.0765 0.6993 0.5025 0.083 Uiso 1 1 calc R . . P1 P 0.36513(10) 0.4964(3) 0.40349(14) 0.0523(7) Uani 1 1 d . . . P2 P 0.22733(10) 0.0335(3) 0.35747(14) 0.0494(7) Uani 1 1 d . . . F1 F 0.3876(4) 0.5068(13) 0.4721(4) 0.127(4) Uani 1 1 d . . . F2 F 0.3427(4) 0.4862(14) 0.3363(4) 0.134(4) Uani 1 1 d . . . F3 F 0.3993(3) 0.3812(9) 0.4187(5) 0.109(3) Uani 1 1 d . . . F4 F 0.3320(3) 0.3821(8) 0.3938(5) 0.095(3) Uani 1 1 d . . . F5 F 0.3307(3) 0.6098(9) 0.3887(5) 0.099(3) Uani 1 1 d . . . F6 F 0.3987(3) 0.6097(8) 0.4150(5) 0.094(3) Uani 1 1 d . . . F7 F 0.2057(4) 0.1463(9) 0.3698(7) 0.133(4) Uani 1 1 d . . . F8 F 0.2727(4) 0.0689(14) 0.4190(6) 0.174(6) Uani 1 1 d . . . F9 F 0.2492(5) -0.0776(9) 0.3451(6) 0.130(4) Uani 1 1 d . . . F10 F 0.2346(4) 0.1470(9) 0.3267(5) 0.117(4) Uani 1 1 d . . . F11 F 0.2172(4) -0.0803(9) 0.3849(5) 0.102(3) Uani 1 1 d . . . F12 F 0.1807(4) 0.0012(14) 0.2951(5) 0.182(7) Uani 1 1 d . . . O1 O 0.0619(3) 0.5395(8) 0.5227(4) 0.092(3) Uani 1 1 d . . . O2 O -0.0104(3) 0.3364(8) 0.4554(4) 0.131(5) Uani 1 1 d RD . . H32 H 0.0128 0.3830 0.4684 0.197 Uiso 1 1 d RD . . H31 H -0.0344 0.3515 0.4491 0.197 Uiso 1 1 d RD . . 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 Hg1 0.0328(2) 0.0383(2) 0.0442(2) 0.00848(17) 0.02047(19) 0.00293(16) S1 0.0417(13) 0.0329(12) 0.0319(11) -0.0015(9) 0.0245(11) -0.0006(10) S2 0.0339(12) 0.0349(12) 0.0296(11) 0.0001(10) 0.0141(10) 0.0056(10) S3 0.0384(13) 0.0397(13) 0.0508(14) -0.0108(11) 0.0291(12) -0.0063(11) N1 0.050(5) 0.034(4) 0.037(4) 0.001(3) 0.032(4) 0.009(4) N2 0.064(4) 0.104(5) 0.043(3) 0.012(3) 0.016(3) 0.030(4) N3 0.077(4) 0.095(5) 0.062(4) 0.002(3) 0.050(4) 0.006(4) N4 0.062(4) 0.086(5) 0.054(3) -0.003(3) 0.035(3) 0.007(3) C1 0.025(4) 0.033(5) 0.030(4) 0.005(4) 0.015(4) 0.000(4) C2 0.060(6) 0.033(5) 0.063(7) -0.019(5) 0.051(6) -0.021(5) C3 0.056(6) 0.044(6) 0.065(7) -0.007(5) 0.052(6) -0.003(5) C4 0.033(5) 0.030(5) 0.025(4) -0.003(4) 0.016(4) 0.002(4) C5 0.059(6) 0.038(5) 0.049(6) 0.004(4) 0.045(6) 0.005(5) C6 0.056(6) 0.045(6) 0.048(6) 0.000(5) 0.042(5) 0.007(5) C7 0.072(7) 0.046(6) 0.040(5) -0.008(5) 0.046(6) -0.002(5) C8 0.083(9) 0.059(8) 0.050(7) 0.010(6) 0.037(7) 0.038(7) C9 0.123(11) 0.028(5) 0.094(9) -0.013(6) 0.095(10) -0.009(6) C10 0.029(4) 0.030(5) 0.028(4) 0.000(4) 0.018(4) 0.002(4) C11 0.047(6) 0.039(6) 0.031(5) 0.000(4) 0.015(5) 0.006(5) C12 0.054(6) 0.034(5) 0.042(6) 0.001(4) 0.024(5) 0.014(5) C13 0.064(4) 0.104(5) 0.043(3) 0.012(3) 0.016(3) 0.030(4) C14 0.045(6) 0.037(5) 0.038(5) -0.005(4) 0.017(5) 0.009(5) C15 0.040(5) 0.030(5) 0.033(5) 0.000(4) 0.014(4) 0.013(4) C16 0.064(4) 0.104(5) 0.043(3) 0.012(3) 0.016(3) 0.030(4) C17 0.064(4) 0.104(5) 0.043(3) 0.012(3) 0.016(3) 0.030(4) C18 0.064(4) 0.104(5) 0.043(3) 0.012(3) 0.016(3) 0.030(4) C19 0.020(4) 0.038(5) 0.037(5) -0.006(4) 0.011(4) 0.002(4) C20 0.037(5) 0.030(5) 0.053(6) -0.003(4) 0.029(5) -0.007(4) C21 0.040(5) 0.035(5) 0.047(6) -0.007(4) 0.026(5) 0.000(4) C22 0.032(5) 0.045(6) 0.037(5) -0.002(4) 0.020(4) -0.002(4) C23 0.042(6) 0.033(5) 0.041(5) -0.002(4) 0.023(5) -0.005(4) C24 0.039(5) 0.037(5) 0.041(5) 0.001(4) 0.021(5) -0.004(4) C25 0.077(4) 0.095(5) 0.062(4) 0.002(3) 0.050(4) 0.006(4) C26 0.077(4) 0.095(5) 0.062(4) 0.002(3) 0.050(4) 0.006(4) C27 0.077(4) 0.095(5) 0.062(4) 0.002(3) 0.050(4) 0.006(4) C28 0.062(4) 0.086(5) 0.054(3) -0.003(3) 0.035(3) 0.007(3) C29 0.062(4) 0.086(5) 0.054(3) -0.003(3) 0.035(3) 0.007(3) C30 0.062(4) 0.086(5) 0.054(3) -0.003(3) 0.035(3) 0.007(3) P1 0.0388(15) 0.0590(18) 0.0560(17) -0.0032(14) 0.0297(14) 0.0003(13) P2 0.0580(18) 0.0431(15) 0.0526(17) -0.0102(13) 0.0385(15) -0.0091(13) F1 0.132(9) 0.173(11) 0.062(5) 0.002(6) 0.058(6) 0.003(8) F2 0.147(10) 0.182(12) 0.075(6) -0.011(7) 0.072(7) -0.010(9) F3 0.075(5) 0.066(5) 0.192(10) 0.004(6) 0.090(7) 0.009(4) F4 0.086(6) 0.066(5) 0.165(9) -0.013(5) 0.096(6) -0.010(4) F5 0.084(6) 0.080(6) 0.161(9) 0.036(6) 0.092(6) 0.031(5) F6 0.081(5) 0.066(5) 0.154(8) -0.004(5) 0.085(6) -0.013(4) F7 0.185(11) 0.062(5) 0.257(14) 0.004(7) 0.190(12) 0.017(6) F8 0.090(8) 0.159(12) 0.113(9) -0.041(8) -0.004(6) -0.005(7) F9 0.228(13) 0.066(6) 0.233(13) 0.007(7) 0.210(12) 0.020(7) F10 0.207(11) 0.064(5) 0.172(10) 0.012(6) 0.165(10) -0.002(6) F11 0.161(9) 0.069(5) 0.140(8) 0.012(5) 0.126(8) -0.002(6) F12 0.134(10) 0.146(11) 0.091(8) 0.003(7) -0.001(7) -0.048(9) O1 0.103(8) 0.078(7) 0.150(10) -0.028(7) 0.107(8) -0.011(6) O2 0.174(12) 0.072(7) 0.252(16) -0.079(9) 0.185(13) -0.054(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 S3 2.425(3) . ? Hg1 S2 2.473(3) . ? Hg1 S1 2.602(2) . ? Hg1 S1 2.720(3) 2 ? Hg1 Hg1 3.3961(18) 2 ? S1 C1 1.748(9) . ? S1 Hg1 2.720(3) 2 ? S2 C10 1.748(9) . ? S3 C19 1.748(10) . ? N1 C8 1.483(14) . ? N1 C4 1.489(11) . ? N1 C9 1.500(14) . ? N1 C7 1.511(11) . ? N2 C18 1.462(19) . ? N2 C17 1.464(18) . ? N2 C16 1.47(2) . ? N2 C13 1.488(15) . ? N3 C27 1.478(17) . ? N3 C26 1.490(18) . ? N3 C25 1.491(17) . ? N3 C22 1.494(14) . ? N4 C30 1.315(16) . ? N4 C29 1.448(17) . ? N4 C28 1.482(17) . ? C1 C2 1.372(13) . ? C1 C6 1.402(13) . ? C2 C3 1.398(13) . ? C2 H2 0.9500 . ? C3 C4 1.366(13) . ? C3 H3 0.9500 . ? C4 C5 1.367(13) . ? C5 C6 1.376(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.365(13) . ? C10 C11 1.396(13) . ? C11 C12 1.389(14) . ? C11 H11 0.9500 . ? C12 C13 1.370(18) . ? C12 H12 0.9500 . ? C13 C14 1.362(18) . ? C14 C15 1.382(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.402(14) . ? C19 C20 1.407(13) . ? C20 C21 1.382(14) . ? C20 H20 0.9500 . ? C21 C22 1.372(14) . ? C21 H21 0.9500 . ? C22 C23 1.401(14) . ? C23 C24 1.356(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O1 1.228(15) . ? C30 H30A 0.9500 . ? P1 F2 1.530(10) . ? P1 F1 1.567(9) . ? P1 F5 1.568(8) . ? P1 F3 1.569(8) . ? P1 F6 1.575(8) . ? P1 F4 1.588(8) . ? P2 F8 1.521(10) . ? P2 F12 1.546(10) . ? P2 F11 1.555(8) . ? P2 F10 1.556(8) . ? P2 F9 1.559(9) . ? P2 F7 1.562(9) . ? O2 H32 0.8499 . ? O2 H31 0.8500 . ? 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 S3 Hg1 S2 136.45(8) . . ? S3 Hg1 S1 116.27(8) . . ? S2 Hg1 S1 98.18(8) . . ? S3 Hg1 S1 103.26(9) . 2 ? S2 Hg1 S1 95.85(7) . 2 ? S1 Hg1 S1 99.61(7) . 2 ? S3 Hg1 Hg1 129.65(6) . 2 ? S2 Hg1 Hg1 92.15(5) . 2 ? S1 Hg1 Hg1 51.89(5) . 2 ? S1 Hg1 Hg1 48.83(6) 2 2 ? C1 S1 Hg1 114.6(3) . . ? C1 S1 Hg1 103.6(3) . 2 ? Hg1 S1 Hg1 79.28(7) . 2 ? C10 S2 Hg1 104.0(3) . . ? C19 S3 Hg1 103.3(3) . . ? C8 N1 C4 110.1(8) . . ? C8 N1 C9 108.6(9) . . ? C4 N1 C9 112.0(7) . . ? C8 N1 C7 108.9(8) . . ? C4 N1 C7 110.8(7) . . ? C9 N1 C7 106.2(8) . . ? C18 N2 C17 105.9(12) . . ? C18 N2 C16 109.1(12) . . ? C17 N2 C16 105.6(12) . . ? C18 N2 C13 109.4(12) . . ? C17 N2 C13 112.8(11) . . ? C16 N2 C13 113.8(12) . . ? C27 N3 C26 107.3(11) . . ? C27 N3 C25 109.7(11) . . ? C26 N3 C25 105.8(10) . . ? C27 N3 C22 109.1(9) . . ? C26 N3 C22 113.2(10) . . ? C25 N3 C22 111.6(10) . . ? C30 N4 C29 120.8(13) . . ? C30 N4 C28 121.0(13) . . ? C29 N4 C28 118.2(11) . . ? C2 C1 C6 117.1(9) . . ? C2 C1 S1 118.7(7) . . ? C6 C1 S1 124.2(7) . . ? C1 C2 C3 121.2(9) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.6(9) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.0(9) . . ? C5 C4 N1 122.0(8) . . ? C3 C4 N1 119.0(8) . . ? C4 C5 C6 120.8(9) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 121.2(9) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 116.9(8) . . ? C15 C10 S2 125.8(7) . . ? C11 C10 S2 117.3(7) . . ? C12 C11 C10 120.8(9) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119.6(10) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.8(11) . . ? C14 C13 N2 117.9(13) . . ? C12 C13 N2 121.2(13) . . ? C13 C14 C15 118.6(10) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C10 C15 C14 123.2(9) . . ? C10 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.4 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.6 . . ? N2 C18 H18B 109.4 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.4 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 115.8(9) . . ? C24 C19 S3 119.8(8) . . ? C20 C19 S3 124.4(8) . . ? C21 C20 C19 121.7(9) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 C20 120.0(9) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.1(9) . . ? C21 C22 N3 121.0(10) . . ? C23 C22 N3 118.8(10) . . ? C24 C23 C22 119.0(9) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C19 123.4(10) . . ? C23 C24 H24 118.3 . . ? C19 C24 H24 118.3 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.4 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.4 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 N4 123.5(14) . . ? O1 C30 H30A 118.3 . . ? N4 C30 H30A 118.3 . . ? F2 P1 F1 179.4(7) . . ? F2 P1 F5 91.3(7) . . ? F1 P1 F5 88.3(6) . . ? F2 P1 F3 89.1(7) . . ? F1 P1 F3 91.3(6) . . ? F5 P1 F3 178.9(5) . . ? F2 P1 F6 91.1(6) . . ? F1 P1 F6 89.4(6) . . ? F5 P1 F6 91.4(5) . . ? F3 P1 F6 89.6(5) . . ? F2 P1 F4 90.5(6) . . ? F1 P1 F4 89.1(6) . . ? F5 P1 F4 88.8(4) . . ? F3 P1 F4 90.3(5) . . ? F6 P1 F4 178.5(6) . . ? F8 P2 F12 178.4(9) . . ? F8 P2 F11 93.1(8) . . ? F12 P2 F11 87.2(7) . . ? F8 P2 F10 90.0(8) . . ? F12 P2 F10 89.7(7) . . ? F11 P2 F10 176.8(7) . . ? F8 P2 F9 91.5(8) . . ? F12 P2 F9 90.0(8) . . ? F11 P2 F9 89.6(5) . . ? F10 P2 F9 91.1(5) . . ? F8 P2 F7 88.2(8) . . ? F12 P2 F7 90.3(8) . . ? F11 P2 F7 91.1(5) . . ? F10 P2 F7 88.3(5) . . ? F9 P2 F7 179.3(6) . . ? H32 O2 H31 135.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H31 O1 0.85 2.03 2.763(13) 144.6 5_566 O2 H32 O1 0.85 2.13 2.911 153.5 . C7 H7B O2 0.98 2.28 3.240(13) 164.5 1_565 C16 H16C F11 0.98 2.38 2.863(17) 110.0 7_546 C17 H17B F4 0.98 2.37 3.200(17) 141.9 7_556 C17 H17C F7 0.98 2.47 3.30(2) 141.9 7_556 C18 H18C S3 0.98 2.88 3.768(13) 150.7 7_556 C25 H25C F4 0.98 2.54 3.104(17) 116.2 4 C28 H28A O1 0.98 2.36 2.766(15) 104.3 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.232 _refine_diff_density_min -1.341 _refine_diff_density_rms 0.157 #===END