# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _publ_contact_author_name 'Jenkins, David' _publ_contact_author_address ; ; _publ_contact_author_email jenkins@ion.chem.utk.edu loop_ _publ_author_name Z.Lu S.Cramer D.Jenkins data_2 _database_code_depnum_ccdc_archive 'CCDC 882737' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H54 Ag F9 N8 O9 S3' _chemical_formula_weight 1514.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5330(12) _cell_length_b 20.0767(14) _cell_length_c 21.7131(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.3870(10) _cell_angle_gamma 90.00 _cell_volume 7595.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9831 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88183 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.65 _reflns_number_total 18384 _reflns_number_gt 11100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains two disordered CH2Cl2 which have no close interaction with the macrocycle, therefore, both of them were sqeezed out to simplify the refinement. ; _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^)+(0.0985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18384 _refine_ls_number_parameters 892 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _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 Ag1 Ag 0.803967(16) 0.372407(13) 0.028386(12) 0.02947(10) Uani 1 1 d . . . S1 S 0.96821(6) 0.59022(5) 0.03762(6) 0.0444(3) Uani 1 1 d . . . S2 S 0.61441(6) 0.31863(6) 0.05743(5) 0.0472(3) Uani 1 1 d . . . S3 S 0.08015(10) 0.42790(8) 0.24635(9) 0.0831(5) Uani 1 1 d . . . F4 F 0.92720(14) 0.69079(13) 0.10447(12) 0.0526(6) Uani 1 1 d . . . O4 O 0.6743(2) 0.33031(19) 0.10568(15) 0.0724(11) Uani 1 1 d . . . C2 C 0.7638(2) 0.46926(18) 0.01107(17) 0.0289(8) Uani 1 1 d . . . O6 O 0.6401(2) 0.31949(16) -0.00304(14) 0.0535(8) Uani 1 1 d . . . F5 F 1.00642(18) 0.71653(13) 0.04084(17) 0.0799(10) Uani 1 1 d . . . N6 N 0.73458(17) 0.51116(14) 0.05000(14) 0.0282(7) Uani 1 1 d . . . F2 F 0.5356(3) 0.2130(3) 0.0242(2) 0.156(2) Uani 1 1 d . . . C1 C 0.8616(2) 0.28141(18) 0.04188(16) 0.0274(8) Uani 1 1 d . . . N1 N 0.92451(17) 0.26799(14) 0.08216(14) 0.0282(7) Uani 1 1 d . . . N2 N 0.84789(16) 0.22363(14) 0.01121(13) 0.0263(6) Uani 1 1 d . . . N8 N 0.91390(17) 0.35880(14) 0.15254(14) 0.0281(7) Uani 1 1 d . . . F6 F 0.8876(2) 0.69782(16) 0.00782(15) 0.0789(9) Uani 1 1 d . . . N5 N 0.76217(16) 0.50454(14) -0.04305(13) 0.0277(7) Uani 1 1 d . . . F1 F 0.6495(4) 0.19401(19) 0.0604(2) 0.1281(18) Uani 1 1 d . . . O9 O 0.90218(17) 0.55630(16) 0.05375(16) 0.0547(8) Uani 1 1 d . . . N7 N 0.84472(18) 0.44387(15) 0.16840(14) 0.0313(7) Uani 1 1 d . . . F3 F 0.5711(4) 0.2185(3) 0.1216(2) 0.169(3) Uani 1 1 d . . . O8 O 0.9802(3) 0.58619(17) -0.02469(19) 0.0925(15) Uani 1 1 d . . . N3 N 0.76816(16) 0.30477(15) -0.11429(13) 0.0272(7) Uani 1 1 d . . . N4 N 0.76822(17) 0.41210(15) -0.11282(13) 0.0295(7) Uani 1 1 d . . . O1 O 0.0774(2) 0.3620(3) 0.2227(3) 0.117(2) Uani 1 1 d . . . O7 O 1.0366(2) 0.58266(18) 0.0807(2) 0.0806(13) Uani 1 1 d . . . C9 C 0.7820(2) 0.21266(19) -0.03598(17) 0.0306(8) Uani 1 1 d . . . H9A H 0.7370 0.2364 -0.0229 0.037 Uiso 1 1 calc R . . H9B H 0.7697 0.1645 -0.0373 0.037 Uiso 1 1 calc R . . C43 C 0.7709(2) 0.40657(18) 0.25436(17) 0.0316(8) Uani 1 1 d . . . C14 C 0.7318(2) 0.56850(18) -0.03692(18) 0.0311(8) Uani 1 1 d . . . C6 C 0.7946(2) 0.48017(18) -0.09839(17) 0.0319(8) Uani 1 1 d . . . H6A H 0.7785 0.5097 -0.1340 0.038 Uiso 1 1 calc R . . H6B H 0.8513 0.4809 -0.0910 0.038 Uiso 1 1 calc R . . C10 C 0.7940(2) 0.23579(18) -0.10220(17) 0.0294(8) Uani 1 1 d . . . H10A H 0.8491 0.2324 -0.1078 0.035 Uiso 1 1 calc R . . H10B H 0.7653 0.2059 -0.1327 0.035 Uiso 1 1 calc R . . C5 C 0.9664(2) 0.31570(18) 0.12383(17) 0.0317(8) Uani 1 1 d . . . H5A H 0.9993 0.2914 0.1564 0.038 Uiso 1 1 calc R . . H5B H 1.0001 0.3431 0.1003 0.038 Uiso 1 1 calc R . . C16 C 0.8240(2) 0.39320(18) 0.20739(16) 0.0303(8) Uani 1 1 d . . . C13 C 0.7148(2) 0.57270(18) 0.02209(18) 0.0296(8) Uani 1 1 d . . . C4 C 0.8116(2) 0.35833(17) -0.10090(16) 0.0283(8) Uani 1 1 d . . . H4 H 0.8645 0.3582 -0.0855 0.034 Uiso 1 1 calc R . . C12 C 0.8999(2) 0.17361(17) 0.03129(17) 0.0269(8) Uani 1 1 d . . . C7 C 0.7278(2) 0.49617(18) 0.11502(17) 0.0308(8) Uani 1 1 d . . . H7A H 0.7110 0.4493 0.1183 0.037 Uiso 1 1 calc R . . H7B H 0.6875 0.5250 0.1294 0.037 Uiso 1 1 calc R . . C15 C 0.8671(2) 0.33969(18) 0.19698(17) 0.0305(8) Uani 1 1 d . . . C3 C 0.8991(2) 0.42164(18) 0.13569(18) 0.0323(8) Uani 1 1 d . . . H3 H 0.9231 0.4461 0.1057 0.039 Uiso 1 1 calc R . . C19 C 1.0143(2) 0.17210(18) 0.11635(17) 0.0324(8) Uani 1 1 d . . . C62 C 0.6013(2) 0.23179(19) -0.12252(19) 0.0366(9) Uani 1 1 d . . . H62 H 0.6228 0.2260 -0.0808 0.044 Uiso 1 1 calc R . . C17 C 0.6935(2) 0.32502(19) -0.13551(17) 0.0307(8) Uani 1 1 d . . . C11 C 0.9489(2) 0.20148(18) 0.07671(17) 0.0303(8) Uani 1 1 d . . . C25 C 0.8999(2) 0.10629(18) 0.00492(18) 0.0308(8) Uani 1 1 d . . . C18 C 0.6941(2) 0.39268(19) -0.13386(16) 0.0294(8) Uani 1 1 d . . . C8 C 0.8026(2) 0.50629(18) 0.15794(18) 0.0325(8) Uani 1 1 d . . . H8A H 0.8352 0.5392 0.1392 0.039 Uiso 1 1 calc R . . H8B H 0.7905 0.5244 0.1982 0.039 Uiso 1 1 calc R . . C38 C 0.6499(2) 0.6507(2) -0.0971(2) 0.0421(10) Uani 1 1 d . . . H38 H 0.6104 0.6403 -0.0721 0.051 Uiso 1 1 calc R . . C30 C 0.9423(2) 0.09356(19) -0.04428(18) 0.0340(9) Uani 1 1 d . . . H30 H 0.9698 0.1286 -0.0613 0.041 Uiso 1 1 calc R . . C37 C 0.7201(2) 0.61826(18) -0.08688(18) 0.0328(8) Uani 1 1 d . . . C61 C 0.6314(2) 0.27966(19) -0.15891(18) 0.0348(9) Uani 1 1 d . . . C53 C 0.8033(3) 0.1647(2) 0.2254(2) 0.0565(13) Uani 1 1 d . . . H53 H 0.7606 0.1366 0.2138 0.068 Uiso 1 1 calc R . . C55 C 0.6306(2) 0.4418(2) -0.14560(19) 0.0386(10) Uani 1 1 d . . . C42 C 0.7774(2) 0.63410(18) -0.12395(19) 0.0356(9) Uani 1 1 d . . . H42 H 0.8262 0.6133 -0.1168 0.043 Uiso 1 1 calc R . . C23 C 1.0610(3) 0.0890(2) 0.19095(19) 0.0428(10) Uani 1 1 d . . . H23 H 1.0517 0.0528 0.2173 0.051 Uiso 1 1 calc R . . C44 C 0.8020(2) 0.4300(2) 0.31172(18) 0.0384(9) Uani 1 1 d . . . H44 H 0.8560 0.4346 0.3203 0.046 Uiso 1 1 calc R . . C24 C 1.0003(2) 0.11824(19) 0.15402(17) 0.0346(9) Uani 1 1 d . . . H24 H 0.9496 0.1016 0.1544 0.042 Uiso 1 1 calc R . . C29 C 0.9444(2) 0.0294(2) -0.0685(2) 0.0406(10) Uani 1 1 d . . . H29 H 0.9731 0.0205 -0.1023 0.049 Uiso 1 1 calc R . . C57 C 0.5216(3) 0.4968(3) -0.1123(3) 0.0584(14) Uani 1 1 d . . . H57 H 0.4846 0.5010 -0.0837 0.070 Uiso 1 1 calc R . . O5 O 0.5453(3) 0.3537(3) 0.0612(3) 0.146(2) Uani 1 1 d . . . C50 C 0.9279(3) 0.2458(2) 0.25942(19) 0.0446(11) Uani 1 1 d . . . H50 H 0.9709 0.2734 0.2717 0.054 Uiso 1 1 calc R . . C31 C 0.6870(2) 0.62886(19) 0.05809(18) 0.0346(9) Uani 1 1 d . . . C26 C 0.8601(2) 0.05536(19) 0.02929(19) 0.0380(9) Uani 1 1 d . . . H26 H 0.8306 0.0641 0.0626 0.046 Uiso 1 1 calc R . . C20 C 1.0887(2) 0.19517(19) 0.1150(2) 0.0379(9) Uani 1 1 d . . . H20 H 1.0983 0.2316 0.0890 0.045 Uiso 1 1 calc R . . C41 C 0.7630(3) 0.68034(19) -0.1715(2) 0.0442(10) Uani 1 1 d . . . H41 H 0.8016 0.6903 -0.1976 0.053 Uiso 1 1 calc R . . C56 C 0.5767(2) 0.4474(2) -0.1037(2) 0.0459(11) Uani 1 1 d . . . H56 H 0.5777 0.4177 -0.0696 0.055 Uiso 1 1 calc R . . C49 C 0.8660(2) 0.27106(19) 0.22133(17) 0.0347(9) Uani 1 1 d . . . C28 C 0.9051(3) -0.0207(2) -0.0436(2) 0.0445(11) Uani 1 1 d . . . H28 H 0.9067 -0.0645 -0.0601 0.053 Uiso 1 1 calc R . . C45 C 0.7553(3) 0.4467(2) 0.3565(2) 0.0424(10) Uani 1 1 d . . . H45 H 0.7774 0.4618 0.3960 0.051 Uiso 1 1 calc R . . C63 C 0.5398(2) 0.1920(2) -0.1464(2) 0.0449(11) Uani 1 1 d . . . H63 H 0.5200 0.1587 -0.1214 0.054 Uiso 1 1 calc R . . C48 C 0.6925(3) 0.3998(2) 0.24281(19) 0.0443(11) Uani 1 1 d . . . H48 H 0.6705 0.3825 0.2041 0.053 Uiso 1 1 calc R . . C58 C 0.5199(3) 0.5402(3) -0.1620(3) 0.0672(16) Uani 1 1 d . . . H58 H 0.4822 0.5743 -0.1672 0.081 Uiso 1 1 calc R . . C27 C 0.8627(3) -0.0086(2) 0.0056(2) 0.0472(11) Uani 1 1 d . . . H27 H 0.8357 -0.0439 0.0228 0.057 Uiso 1 1 calc R . . C52 C 0.8648(4) 0.1408(2) 0.2621(2) 0.0578(15) Uani 1 1 d . . . H52 H 0.8647 0.0959 0.2759 0.069 Uiso 1 1 calc R . . C46 C 0.6769(3) 0.4415(2) 0.34393(19) 0.0413(10) Uani 1 1 d . . . H46 H 0.6445 0.4541 0.3743 0.050 Uiso 1 1 calc R . . O2 O 0.1321(6) 0.4710(2) 0.2176(3) 0.196(4) Uani 1 1 d . . . C40 C 0.6923(3) 0.7119(2) -0.1809(2) 0.0500(12) Uani 1 1 d . . . H40 H 0.6823 0.7433 -0.2135 0.060 Uiso 1 1 calc R . . C54 C 0.8027(3) 0.2310(2) 0.2045(2) 0.0432(10) Uani 1 1 d . . . H54 H 0.7594 0.2482 0.1792 0.052 Uiso 1 1 calc R . . C64 C 0.5081(3) 0.2019(2) -0.2067(2) 0.0548(13) Uani 1 1 d . . . H64 H 0.4659 0.1753 -0.2232 0.066 Uiso 1 1 calc R . . C21 C 1.1489(3) 0.1654(2) 0.1513(2) 0.0459(11) Uani 1 1 d . . . H21 H 1.1999 0.1810 0.1503 0.055 Uiso 1 1 calc R . . C68 C 0.9466(3) 0.6771(2) 0.0480(2) 0.0483(11) Uani 1 1 d . . . C39 C 0.6370(3) 0.6978(2) -0.1432(2) 0.0537(13) Uani 1 1 d . . . H39 H 0.5893 0.7206 -0.1488 0.064 Uiso 1 1 calc R . . C47 C 0.6456(3) 0.4179(2) 0.2872(2) 0.0507(12) Uani 1 1 d . . . H47 H 0.5914 0.4141 0.2785 0.061 Uiso 1 1 calc R . . C36 C 0.6098(3) 0.6429(2) 0.0568(2) 0.0492(11) Uani 1 1 d . . . H36 H 0.5729 0.6162 0.0328 0.059 Uiso 1 1 calc R . . C51 C 0.9273(3) 0.1804(2) 0.2797(2) 0.0531(13) Uani 1 1 d . . . H51 H 0.9699 0.1630 0.3056 0.064 Uiso 1 1 calc R . . C22 C 1.1342(3) 0.1125(2) 0.1894(2) 0.0521(12) Uani 1 1 d . . . H22 H 1.1754 0.0921 0.2147 0.063 Uiso 1 1 calc R . . O3 O 0.0082(3) 0.4475(4) 0.2663(4) 0.212(5) Uani 1 1 d . . . C34 C 0.6400(3) 0.7347(3) 0.1261(3) 0.0690(16) Uani 1 1 d . . . H34 H 0.6238 0.7718 0.1484 0.083 Uiso 1 1 calc R . . C35 C 0.5861(3) 0.6964(3) 0.0908(3) 0.0665(15) Uani 1 1 d . . . H35 H 0.5331 0.7066 0.0897 0.080 Uiso 1 1 calc R . . C66 C 0.5979(3) 0.2887(3) -0.2191(2) 0.0573(13) Uani 1 1 d . . . H66 H 0.6172 0.3222 -0.2442 0.069 Uiso 1 1 calc R . . C65 C 0.5369(3) 0.2497(3) -0.2434(2) 0.0723(17) Uani 1 1 d . . . H65 H 0.5149 0.2559 -0.2850 0.087 Uiso 1 1 calc R . . C60 C 0.6279(3) 0.4852(2) -0.1957(2) 0.0515(12) Uani 1 1 d . . . H60 H 0.6644 0.4813 -0.2247 0.062 Uiso 1 1 calc R . . C32 C 0.7396(3) 0.6660(2) 0.0949(2) 0.0503(12) Uani 1 1 d . . . H32 H 0.7926 0.6553 0.0971 0.060 Uiso 1 1 calc R . . C33 C 0.7155(3) 0.7199(3) 0.1295(3) 0.0711(16) Uani 1 1 d . . . H33 H 0.7520 0.7457 0.1549 0.085 Uiso 1 1 calc R . . C59 C 0.5720(3) 0.5341(3) -0.2031(3) 0.0683(16) Uani 1 1 d . . . H59 H 0.5701 0.5636 -0.2374 0.082 Uiso 1 1 calc R . . C67 C 0.5898(5) 0.2332(4) 0.0682(3) 0.091(2) Uani 1 1 d . . . C70 C 0.1290(14) 0.4206(7) 0.3139(6) 0.270(11) Uani 1 1 d . . . F8 F 0.1437(4) 0.4797(3) 0.3435(3) 0.206(3) Uani 1 1 d . . . F7 F 0.2024(4) 0.3871(4) 0.3126(3) 0.205(4) Uani 1 1 d . . . F9 F 0.1123(7) 0.3806(4) 0.3573(4) 0.243(4) 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 Ag1 0.03446(16) 0.02585(15) 0.02796(15) 0.00063(11) 0.00285(11) 0.00565(12) S1 0.0443(6) 0.0382(6) 0.0537(7) -0.0002(5) 0.0181(5) -0.0077(5) S2 0.0346(6) 0.0627(7) 0.0445(6) -0.0222(5) 0.0055(5) 0.0013(5) S3 0.0761(10) 0.0666(10) 0.0978(13) -0.0321(9) -0.0298(9) 0.0226(8) F4 0.0494(15) 0.0568(16) 0.0531(16) -0.0002(13) 0.0123(12) 0.0000(12) O4 0.090(3) 0.076(3) 0.046(2) -0.0030(18) -0.0147(19) -0.027(2) C2 0.0272(19) 0.0278(19) 0.031(2) -0.0013(15) 0.0011(15) -0.0009(15) O6 0.075(2) 0.0488(18) 0.0365(17) -0.0074(14) 0.0068(16) -0.0027(16) F5 0.081(2) 0.0405(16) 0.130(3) -0.0058(17) 0.064(2) -0.0134(15) N6 0.0291(16) 0.0243(15) 0.0316(17) -0.0005(13) 0.0056(13) 0.0027(12) F2 0.165(5) 0.180(5) 0.118(4) -0.026(3) -0.003(3) -0.131(4) C1 0.0275(19) 0.0292(19) 0.0260(19) 0.0026(15) 0.0049(15) 0.0035(15) N1 0.0319(17) 0.0224(15) 0.0307(16) 0.0007(12) 0.0047(13) 0.0005(13) N2 0.0246(15) 0.0278(16) 0.0266(16) -0.0008(12) 0.0027(12) 0.0011(12) N8 0.0298(16) 0.0254(16) 0.0283(16) -0.0013(12) -0.0007(13) -0.0003(12) F6 0.102(3) 0.064(2) 0.068(2) 0.0161(16) -0.0003(18) 0.0181(18) N5 0.0262(16) 0.0284(16) 0.0284(16) 0.0002(13) 0.0028(13) 0.0017(13) F1 0.221(6) 0.052(2) 0.121(4) 0.020(2) 0.061(4) -0.015(3) O9 0.0353(17) 0.0522(19) 0.077(2) 0.0065(17) 0.0085(16) -0.0096(14) N7 0.0384(18) 0.0258(16) 0.0284(16) -0.0016(13) -0.0016(14) 0.0016(14) F3 0.256(6) 0.179(5) 0.089(3) -0.022(3) 0.091(4) -0.130(5) O8 0.173(5) 0.040(2) 0.075(3) 0.0002(18) 0.057(3) -0.001(2) N3 0.0245(15) 0.0311(16) 0.0260(16) -0.0004(13) 0.0028(12) 0.0073(13) N4 0.0305(17) 0.0347(17) 0.0232(16) -0.0002(13) 0.0021(13) 0.0024(14) O1 0.049(2) 0.143(4) 0.155(5) -0.099(4) -0.008(3) 0.001(3) O7 0.055(2) 0.057(2) 0.121(3) -0.031(2) -0.032(2) 0.0256(18) C9 0.0273(19) 0.032(2) 0.032(2) -0.0008(16) 0.0034(16) 0.0010(16) C43 0.040(2) 0.0256(19) 0.0280(19) -0.0008(15) -0.0023(16) -0.0009(16) C14 0.0262(19) 0.0289(19) 0.037(2) 0.0061(16) -0.0012(16) 0.0015(15) C6 0.034(2) 0.031(2) 0.031(2) 0.0028(16) 0.0051(16) 0.0015(16) C10 0.0290(19) 0.0277(19) 0.031(2) -0.0018(15) 0.0032(15) 0.0065(15) C5 0.029(2) 0.033(2) 0.033(2) -0.0022(16) -0.0010(16) 0.0030(16) C16 0.040(2) 0.0276(18) 0.0226(18) -0.0009(14) -0.0021(16) -0.0048(16) C13 0.0233(18) 0.0274(19) 0.037(2) 0.0009(16) 0.0002(16) 0.0005(15) C4 0.0287(19) 0.031(2) 0.0259(18) 0.0017(15) 0.0043(15) 0.0049(15) C12 0.0250(18) 0.0242(17) 0.0318(19) 0.0055(15) 0.0038(15) 0.0039(14) C7 0.036(2) 0.0239(18) 0.034(2) 0.0003(15) 0.0099(17) 0.0006(16) C15 0.035(2) 0.0295(19) 0.0255(19) -0.0015(15) -0.0033(16) -0.0013(16) C3 0.037(2) 0.0244(18) 0.035(2) -0.0011(16) 0.0023(17) -0.0029(16) C19 0.038(2) 0.0251(18) 0.033(2) -0.0007(16) 0.0008(17) 0.0059(16) C62 0.032(2) 0.036(2) 0.040(2) -0.0110(18) -0.0014(17) 0.0030(17) C17 0.0267(19) 0.039(2) 0.0260(19) 0.0011(16) 0.0010(15) 0.0058(16) C11 0.030(2) 0.0267(18) 0.034(2) 0.0015(15) 0.0034(16) 0.0043(15) C25 0.031(2) 0.0268(18) 0.033(2) 0.0012(15) -0.0019(16) 0.0069(15) C18 0.029(2) 0.036(2) 0.0226(18) -0.0003(15) 0.0014(15) 0.0037(16) C8 0.040(2) 0.0250(19) 0.032(2) -0.0015(15) 0.0022(17) 0.0048(16) C38 0.035(2) 0.038(2) 0.051(3) 0.003(2) -0.0027(19) 0.0050(18) C30 0.030(2) 0.032(2) 0.039(2) -0.0011(17) -0.0008(17) 0.0051(16) C37 0.034(2) 0.029(2) 0.034(2) 0.0001(16) -0.0032(16) 0.0008(16) C61 0.034(2) 0.034(2) 0.036(2) -0.0024(17) -0.0027(17) 0.0065(17) C53 0.075(4) 0.037(3) 0.063(3) -0.003(2) 0.034(3) -0.011(2) C55 0.036(2) 0.039(2) 0.036(2) -0.0085(18) -0.0135(18) 0.0084(18) C42 0.039(2) 0.0249(19) 0.042(2) -0.0033(17) 0.0003(18) 0.0008(16) C23 0.058(3) 0.035(2) 0.034(2) 0.0055(18) -0.005(2) 0.005(2) C44 0.037(2) 0.045(2) 0.031(2) -0.0073(18) -0.0012(17) 0.0030(18) C24 0.044(2) 0.033(2) 0.0277(19) 0.0003(16) 0.0064(17) 0.0002(17) C29 0.038(2) 0.040(2) 0.043(2) -0.0079(19) -0.0014(19) 0.0061(18) C57 0.037(3) 0.059(3) 0.076(4) -0.017(3) -0.006(2) 0.018(2) O5 0.077(3) 0.163(5) 0.202(7) -0.060(5) 0.041(4) 0.046(3) C50 0.063(3) 0.038(2) 0.031(2) 0.0028(18) 0.000(2) 0.012(2) C31 0.038(2) 0.0280(19) 0.037(2) 0.0035(17) 0.0050(17) 0.0040(17) C26 0.047(2) 0.033(2) 0.034(2) -0.0010(17) 0.0052(18) -0.0009(18) C20 0.037(2) 0.028(2) 0.047(2) 0.0046(17) -0.0013(18) 0.0002(17) C41 0.064(3) 0.029(2) 0.038(2) 0.0042(18) -0.001(2) -0.008(2) C56 0.038(2) 0.044(2) 0.052(3) -0.006(2) -0.009(2) 0.011(2) C49 0.048(2) 0.031(2) 0.0257(19) -0.0016(16) 0.0060(17) 0.0045(18) C28 0.047(3) 0.035(2) 0.048(3) -0.0098(19) -0.010(2) 0.0113(19) C45 0.049(3) 0.041(2) 0.036(2) -0.0073(18) -0.0009(19) -0.005(2) C63 0.041(2) 0.037(2) 0.057(3) -0.012(2) 0.006(2) -0.0025(19) C48 0.045(3) 0.063(3) 0.025(2) 0.0021(19) 0.0016(18) -0.014(2) C58 0.056(3) 0.051(3) 0.086(4) -0.014(3) -0.029(3) 0.027(3) C27 0.060(3) 0.033(2) 0.045(3) 0.0068(19) -0.008(2) -0.002(2) C52 0.103(4) 0.033(2) 0.045(3) 0.014(2) 0.038(3) 0.019(3) C46 0.050(3) 0.047(2) 0.029(2) 0.0034(18) 0.0087(19) -0.005(2) O2 0.405(11) 0.050(3) 0.167(6) 0.016(3) 0.181(7) 0.027(5) C40 0.065(3) 0.036(2) 0.045(3) 0.009(2) -0.014(2) -0.002(2) C54 0.045(3) 0.038(2) 0.048(3) -0.0021(19) 0.015(2) -0.005(2) C64 0.042(3) 0.057(3) 0.061(3) -0.021(2) -0.015(2) -0.005(2) C21 0.040(2) 0.037(2) 0.057(3) 0.002(2) -0.014(2) -0.0012(19) C68 0.043(3) 0.052(3) 0.053(3) 0.013(2) 0.019(2) -0.004(2) C39 0.047(3) 0.043(3) 0.065(3) 0.007(2) -0.018(2) 0.007(2) C47 0.041(3) 0.071(3) 0.040(3) 0.012(2) 0.007(2) -0.011(2) C36 0.041(3) 0.050(3) 0.056(3) -0.008(2) 0.007(2) 0.012(2) C51 0.080(4) 0.050(3) 0.031(2) 0.013(2) 0.015(2) 0.026(3) C22 0.058(3) 0.038(2) 0.055(3) 0.007(2) -0.017(2) 0.006(2) O3 0.105(4) 0.253(8) 0.261(8) -0.194(7) -0.060(5) 0.101(5) C34 0.065(4) 0.046(3) 0.097(4) -0.020(3) 0.016(3) 0.019(3) C35 0.046(3) 0.069(3) 0.085(4) -0.017(3) 0.007(3) 0.022(3) C66 0.058(3) 0.068(3) 0.041(3) 0.002(2) -0.015(2) -0.016(3) C65 0.079(4) 0.086(4) 0.044(3) 0.002(3) -0.026(3) -0.029(3) C60 0.060(3) 0.051(3) 0.040(3) 0.008(2) -0.010(2) 0.012(2) C32 0.035(2) 0.049(3) 0.069(3) -0.018(2) 0.015(2) -0.004(2) C33 0.062(3) 0.058(3) 0.096(4) -0.035(3) 0.022(3) -0.015(3) C59 0.077(4) 0.049(3) 0.070(4) 0.013(3) -0.030(3) 0.017(3) C67 0.114(6) 0.107(6) 0.060(4) -0.024(4) 0.043(4) -0.068(5) C70 0.60(4) 0.138(10) 0.098(8) -0.034(8) 0.154(15) 0.064(15) F8 0.288(8) 0.185(6) 0.129(4) -0.110(4) -0.054(5) 0.075(5) F7 0.193(6) 0.263(8) 0.133(5) -0.106(5) -0.090(5) 0.124(6) F9 0.393(13) 0.202(8) 0.139(6) 0.033(5) 0.054(7) 0.118(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 Ag1 C2 2.088(4) . ? Ag1 C1 2.093(3) . ? S1 O8 1.394(4) . ? S1 O9 1.420(3) . ? S1 O7 1.445(4) . ? S1 C68 1.805(5) . ? S2 O5 1.411(5) . ? S2 O4 1.418(3) . ? S2 O6 1.435(3) . ? S2 C67 1.789(7) . ? S3 O1 1.417(5) . ? S3 O3 1.435(6) . ? S3 O2 1.446(7) . ? S3 C70 1.621(18) . ? F4 C68 1.337(5) . ? C2 N6 1.335(4) . ? C2 N5 1.370(5) . ? F5 C68 1.336(5) . ? N6 C13 1.402(4) . ? N6 C7 1.461(5) . ? F2 C67 1.334(7) . ? C1 N2 1.346(4) . ? C1 N1 1.356(4) . ? N1 C11 1.411(4) . ? N1 C5 1.459(5) . ? N2 C12 1.393(4) . ? N2 C9 1.473(4) . ? N8 C3 1.331(4) . ? N8 C15 1.389(5) . ? N8 C5 1.454(5) . ? F6 C68 1.342(5) . ? N5 C14 1.402(5) . ? N5 C6 1.469(5) . ? F1 C67 1.335(9) . ? N7 C3 1.329(5) . ? N7 C16 1.397(5) . ? N7 C8 1.459(5) . ? F3 C67 1.274(7) . ? N3 C4 1.331(5) . ? N3 C17 1.399(4) . ? N3 C10 1.472(4) . ? N4 C4 1.329(4) . ? N4 C18 1.385(5) . ? N4 C6 1.465(5) . ? C9 C10 1.547(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C43 C48 1.376(6) . ? C43 C44 1.385(5) . ? C43 C16 1.481(5) . ? C14 C13 1.350(5) . ? C14 C37 1.472(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C16 C15 1.346(5) . ? C13 C31 1.485(5) . ? C4 H4 0.9500 . ? C12 C11 1.355(5) . ? C12 C25 1.468(5) . ? C7 C8 1.536(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C15 C49 1.477(5) . ? C3 H3 0.9500 . ? C19 C20 1.388(5) . ? C19 C24 1.394(5) . ? C19 C11 1.477(5) . ? C62 C61 1.386(6) . ? C62 C63 1.394(6) . ? C62 H62 0.9500 . ? C17 C18 1.359(5) . ? C17 C61 1.466(5) . ? C25 C26 1.377(5) . ? C25 C30 1.391(5) . ? C18 C55 1.487(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C38 C39 1.376(6) . ? C38 C37 1.388(5) . ? C38 H38 0.9500 . ? C30 C29 1.394(5) . ? C30 H30 0.9500 . ? C37 C42 1.392(6) . ? C61 C66 1.385(6) . ? C53 C52 1.355(7) . ? C53 C54 1.407(6) . ? C53 H53 0.9500 . ? C55 C56 1.387(6) . ? C55 C60 1.390(6) . ? C42 C41 1.391(6) . ? C42 H42 0.9500 . ? C23 C22 1.372(7) . ? C23 C24 1.389(6) . ? C23 H23 0.9500 . ? C44 C45 1.380(6) . ? C44 H44 0.9500 . ? C24 H24 0.9500 . ? C29 C28 1.365(6) . ? C29 H29 0.9500 . ? C57 C56 1.382(6) . ? C57 C58 1.385(8) . ? C57 H57 0.9500 . ? C50 C51 1.385(6) . ? C50 C49 1.386(6) . ? C50 H50 0.9500 . ? C31 C32 1.371(6) . ? C31 C36 1.381(6) . ? C26 C27 1.387(6) . ? C26 H26 0.9500 . ? C20 C21 1.382(5) . ? C20 H20 0.9500 . ? C41 C40 1.387(6) . ? C41 H41 0.9500 . ? C56 H56 0.9500 . ? C49 C54 1.386(6) . ? C28 C27 1.388(6) . ? C28 H28 0.9500 . ? C45 C46 1.376(6) . ? C45 H45 0.9500 . ? C63 C64 1.379(7) . ? C63 H63 0.9500 . ? C48 C47 1.385(6) . ? C48 H48 0.9500 . ? C58 C59 1.351(8) . ? C58 H58 0.9500 . ? C27 H27 0.9500 . ? C52 C51 1.372(7) . ? C52 H52 0.9500 . ? C46 C47 1.375(6) . ? C46 H46 0.9500 . ? C40 C39 1.365(7) . ? C40 H40 0.9500 . ? C54 H54 0.9500 . ? C64 C65 1.379(7) . ? C64 H64 0.9500 . ? C21 C22 1.387(6) . ? C21 H21 0.9500 . ? C39 H39 0.9500 . ? C47 H47 0.9500 . ? C36 C35 1.392(6) . ? C36 H36 0.9500 . ? C51 H51 0.9500 . ? C22 H22 0.9500 . ? C34 C33 1.350(7) . ? C34 C35 1.383(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C66 C65 1.382(7) . ? C66 H66 0.9500 . ? C65 H65 0.9500 . ? C60 C59 1.385(7) . ? C60 H60 0.9500 . ? C32 C33 1.409(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C59 H59 0.9500 . ? C70 F9 1.295(14) . ? C70 F8 1.360(14) . ? C70 F7 1.46(2) . ? 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 Ag1 C1 170.45(14) . . ? O8 S1 O9 115.2(3) . . ? O8 S1 O7 114.8(3) . . ? O9 S1 O7 115.5(2) . . ? O8 S1 C68 103.5(2) . . ? O9 S1 C68 104.2(2) . . ? O7 S1 C68 101.0(2) . . ? O5 S2 O4 116.4(3) . . ? O5 S2 O6 113.9(3) . . ? O4 S2 O6 113.1(2) . . ? O5 S2 C67 104.5(4) . . ? O4 S2 C67 103.4(3) . . ? O6 S2 C67 103.6(2) . . ? O1 S3 O3 111.7(4) . . ? O1 S3 O2 113.5(3) . . ? O3 S3 O2 125.7(5) . . ? O1 S3 C70 103.7(5) . . ? O3 S3 C70 98.3(7) . . ? O2 S3 C70 98.6(8) . . ? N6 C2 N5 104.1(3) . . ? N6 C2 Ag1 128.2(3) . . ? N5 C2 Ag1 127.7(3) . . ? C2 N6 C13 112.0(3) . . ? C2 N6 C7 124.1(3) . . ? C13 N6 C7 123.8(3) . . ? N2 C1 N1 103.6(3) . . ? N2 C1 Ag1 128.8(3) . . ? N1 C1 Ag1 127.5(3) . . ? C1 N1 C11 111.5(3) . . ? C1 N1 C5 126.0(3) . . ? C11 N1 C5 122.5(3) . . ? C1 N2 C12 113.0(3) . . ? C1 N2 C9 123.8(3) . . ? C12 N2 C9 123.0(3) . . ? C3 N8 C15 109.9(3) . . ? C3 N8 C5 124.0(3) . . ? C15 N8 C5 125.8(3) . . ? C2 N5 C14 111.4(3) . . ? C2 N5 C6 123.8(3) . . ? C14 N5 C6 124.6(3) . . ? C3 N7 C16 109.2(3) . . ? C3 N7 C8 125.9(3) . . ? C16 N7 C8 124.0(3) . . ? C4 N3 C17 109.2(3) . . ? C4 N3 C10 124.3(3) . . ? C17 N3 C10 126.2(3) . . ? C4 N4 C18 109.3(3) . . ? C4 N4 C6 123.8(3) . . ? C18 N4 C6 126.5(3) . . ? N2 C9 C10 115.1(3) . . ? N2 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? N2 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C48 C43 C44 118.9(4) . . ? C48 C43 C16 123.3(3) . . ? C44 C43 C16 117.8(4) . . ? C13 C14 N5 105.9(3) . . ? C13 C14 C37 129.0(3) . . ? N5 C14 C37 125.1(3) . . ? N4 C6 N5 110.1(3) . . ? N4 C6 H6A 109.6 . . ? N5 C6 H6A 109.6 . . ? N4 C6 H6B 109.6 . . ? N5 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? N3 C10 C9 112.2(3) . . ? N3 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N3 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N8 C5 N1 110.9(3) . . ? N8 C5 H5A 109.5 . . ? N1 C5 H5A 109.5 . . ? N8 C5 H5B 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? C15 C16 N7 106.9(3) . . ? C15 C16 C43 131.9(3) . . ? N7 C16 C43 120.7(3) . . ? C14 C13 N6 106.6(3) . . ? C14 C13 C31 131.8(3) . . ? N6 C13 C31 121.4(3) . . ? N4 C4 N3 108.2(3) . . ? N4 C4 H4 125.9 . . ? N3 C4 H4 125.9 . . ? C11 C12 N2 105.7(3) . . ? C11 C12 C25 129.5(3) . . ? N2 C12 C25 124.8(3) . . ? N6 C7 C8 113.8(3) . . ? N6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C16 C15 N8 106.4(3) . . ? C16 C15 C49 130.9(4) . . ? N8 C15 C49 122.6(3) . . ? N7 C3 N8 107.5(3) . . ? N7 C3 H3 126.2 . . ? N8 C3 H3 126.2 . . ? C20 C19 C24 119.9(4) . . ? C20 C19 C11 121.6(3) . . ? C24 C19 C11 118.4(4) . . ? C61 C62 C63 120.9(4) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C18 C17 N3 106.1(3) . . ? C18 C17 C61 129.3(3) . . ? N3 C17 C61 124.4(3) . . ? C12 C11 N1 106.1(3) . . ? C12 C11 C19 130.3(3) . . ? N1 C11 C19 123.5(3) . . ? C26 C25 C30 119.7(4) . . ? C26 C25 C12 120.8(3) . . ? C30 C25 C12 119.5(3) . . ? C17 C18 N4 107.1(3) . . ? C17 C18 C55 130.9(4) . . ? N4 C18 C55 121.8(3) . . ? N7 C8 C7 111.3(3) . . ? N7 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N7 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C39 C38 C37 120.6(4) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C25 C30 C29 119.9(4) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C38 C37 C42 118.9(4) . . ? C38 C37 C14 119.0(4) . . ? C42 C37 C14 122.1(3) . . ? C66 C61 C62 118.7(4) . . ? C66 C61 C17 117.8(4) . . ? C62 C61 C17 123.3(3) . . ? C52 C53 C54 120.1(5) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C56 C55 C60 119.7(4) . . ? C56 C55 C18 119.5(4) . . ? C60 C55 C18 120.6(4) . . ? C41 C42 C37 120.0(4) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C45 C44 C43 120.8(4) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C23 C24 C19 119.5(4) . . ? C23 C24 H24 120.2 . . ? C19 C24 H24 120.2 . . ? C28 C29 C30 119.7(4) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C56 C57 C58 120.7(5) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C51 C50 C49 120.3(5) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C32 C31 C36 119.7(4) . . ? C32 C31 C13 118.7(4) . . ? C36 C31 C13 121.6(4) . . ? C25 C26 C27 120.4(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C40 C41 C42 119.9(4) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C57 C56 C55 119.2(5) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C54 C49 C50 119.7(4) . . ? C54 C49 C15 119.3(4) . . ? C50 C49 C15 121.0(4) . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C46 C45 C44 120.0(4) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C64 C63 C62 118.9(4) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C43 C48 C47 120.4(4) . . ? C43 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C59 C58 C57 120.0(5) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C26 C27 C28 119.4(4) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C53 C52 C51 121.2(4) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C47 C46 C45 119.6(4) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C39 C40 C41 120.0(4) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C49 C54 C53 119.1(4) . . ? C49 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C65 C64 C63 121.0(4) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? F4 C68 F5 105.6(4) . . ? F4 C68 F6 106.1(4) . . ? F5 C68 F6 107.4(4) . . ? F4 C68 S1 113.0(3) . . ? F5 C68 S1 112.3(3) . . ? F6 C68 S1 112.0(3) . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C46 C47 C48 120.4(4) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C31 C36 C35 119.8(5) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C52 C51 C50 119.6(5) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C33 C34 C35 120.9(5) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 119.8(5) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C65 C66 C61 121.0(5) . . ? C65 C66 H66 119.5 . . ? C61 C66 H66 119.5 . . ? C64 C65 C66 119.5(5) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? C59 C60 C55 119.8(5) . . ? C59 C60 H60 120.1 . . ? C55 C60 H60 120.1 . . ? C31 C32 C33 120.4(4) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 119.3(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C58 C59 C60 120.6(5) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? F3 C67 F2 110.2(5) . . ? F3 C67 F1 105.2(8) . . ? F2 C67 F1 103.6(6) . . ? F3 C67 S2 115.6(5) . . ? F2 C67 S2 111.1(6) . . ? F1 C67 S2 110.2(4) . . ? F9 C70 F8 104.0(9) . . ? F9 C70 F7 89.9(12) . . ? F8 C70 F7 106.9(17) . . ? F9 C70 S3 125.1(17) . . ? F8 C70 S3 113.7(11) . . ? F7 C70 S3 113.8(6) . . ? 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 C1 Ag1 C2 N6 -120.1(8) . . . . ? C1 Ag1 C2 N5 59.4(10) . . . . ? N5 C2 N6 C13 -0.5(4) . . . . ? Ag1 C2 N6 C13 179.0(3) . . . . ? N5 C2 N6 C7 -177.3(3) . . . . ? Ag1 C2 N6 C7 2.2(5) . . . . ? C2 Ag1 C1 N2 -116.7(8) . . . . ? C2 Ag1 C1 N1 59.8(10) . . . . ? N2 C1 N1 C11 -0.7(4) . . . . ? Ag1 C1 N1 C11 -177.9(3) . . . . ? N2 C1 N1 C5 175.6(3) . . . . ? Ag1 C1 N1 C5 -1.7(5) . . . . ? N1 C1 N2 C12 0.6(4) . . . . ? Ag1 C1 N2 C12 177.8(2) . . . . ? N1 C1 N2 C9 176.9(3) . . . . ? Ag1 C1 N2 C9 -5.9(5) . . . . ? N6 C2 N5 C14 0.1(4) . . . . ? Ag1 C2 N5 C14 -179.4(3) . . . . ? N6 C2 N5 C6 175.0(3) . . . . ? Ag1 C2 N5 C6 -4.5(5) . . . . ? C1 N2 C9 C10 84.6(4) . . . . ? C12 N2 C9 C10 -99.4(4) . . . . ? C2 N5 C14 C13 0.3(4) . . . . ? C6 N5 C14 C13 -174.6(3) . . . . ? C2 N5 C14 C37 -178.2(3) . . . . ? C6 N5 C14 C37 6.9(6) . . . . ? C4 N4 C6 N5 -103.7(4) . . . . ? C18 N4 C6 N5 68.6(4) . . . . ? C2 N5 C6 N4 48.8(4) . . . . ? C14 N5 C6 N4 -137.0(3) . . . . ? C4 N3 C10 C9 87.0(4) . . . . ? C17 N3 C10 C9 -86.3(4) . . . . ? N2 C9 C10 N3 -91.7(4) . . . . ? C3 N8 C5 N1 -103.7(4) . . . . ? C15 N8 C5 N1 70.3(4) . . . . ? C1 N1 C5 N8 42.2(5) . . . . ? C11 N1 C5 N8 -141.9(3) . . . . ? C3 N7 C16 C15 -0.4(4) . . . . ? C8 N7 C16 C15 169.3(3) . . . . ? C3 N7 C16 C43 172.9(3) . . . . ? C8 N7 C16 C43 -17.4(5) . . . . ? C48 C43 C16 C15 -98.4(5) . . . . ? C44 C43 C16 C15 84.6(5) . . . . ? C48 C43 C16 N7 90.2(5) . . . . ? C44 C43 C16 N7 -86.7(5) . . . . ? N5 C14 C13 N6 -0.6(4) . . . . ? C37 C14 C13 N6 177.8(4) . . . . ? N5 C14 C13 C31 174.6(4) . . . . ? C37 C14 C13 C31 -7.0(7) . . . . ? C2 N6 C13 C14 0.7(4) . . . . ? C7 N6 C13 C14 177.5(3) . . . . ? C2 N6 C13 C31 -175.1(3) . . . . ? C7 N6 C13 C31 1.8(5) . . . . ? C18 N4 C4 N3 0.8(4) . . . . ? C6 N4 C4 N3 174.2(3) . . . . ? C17 N3 C4 N4 -0.3(4) . . . . ? C10 N3 C4 N4 -174.6(3) . . . . ? C1 N2 C12 C11 -0.2(4) . . . . ? C9 N2 C12 C11 -176.6(3) . . . . ? C1 N2 C12 C25 -178.2(3) . . . . ? C9 N2 C12 C25 5.5(5) . . . . ? C2 N6 C7 C8 80.8(4) . . . . ? C13 N6 C7 C8 -95.6(4) . . . . ? N7 C16 C15 N8 0.7(4) . . . . ? C43 C16 C15 N8 -171.5(4) . . . . ? N7 C16 C15 C49 -175.0(4) . . . . ? C43 C16 C15 C49 12.8(7) . . . . ? C3 N8 C15 C16 -0.9(4) . . . . ? C5 N8 C15 C16 -175.5(3) . . . . ? C3 N8 C15 C49 175.3(3) . . . . ? C5 N8 C15 C49 0.6(5) . . . . ? C16 N7 C3 N8 -0.1(4) . . . . ? C8 N7 C3 N8 -169.6(3) . . . . ? C15 N8 C3 N7 0.6(4) . . . . ? C5 N8 C3 N7 175.4(3) . . . . ? C4 N3 C17 C18 -0.4(4) . . . . ? C10 N3 C17 C18 173.8(3) . . . . ? C4 N3 C17 C61 175.3(3) . . . . ? C10 N3 C17 C61 -10.6(5) . . . . ? N2 C12 C11 N1 -0.2(4) . . . . ? C25 C12 C11 N1 177.6(4) . . . . ? N2 C12 C11 C19 177.8(4) . . . . ? C25 C12 C11 C19 -4.4(7) . . . . ? C1 N1 C11 C12 0.6(4) . . . . ? C5 N1 C11 C12 -175.8(3) . . . . ? C1 N1 C11 C19 -177.6(3) . . . . ? C5 N1 C11 C19 6.0(5) . . . . ? C20 C19 C11 C12 118.0(5) . . . . ? C24 C19 C11 C12 -59.5(6) . . . . ? C20 C19 C11 N1 -64.2(5) . . . . ? C24 C19 C11 N1 118.3(4) . . . . ? C11 C12 C25 C26 90.8(5) . . . . ? N2 C12 C25 C26 -91.8(5) . . . . ? C11 C12 C25 C30 -87.6(5) . . . . ? N2 C12 C25 C30 89.8(5) . . . . ? N3 C17 C18 N4 0.8(4) . . . . ? C61 C17 C18 N4 -174.5(4) . . . . ? N3 C17 C18 C55 -174.0(4) . . . . ? C61 C17 C18 C55 10.7(7) . . . . ? C4 N4 C18 C17 -1.0(4) . . . . ? C6 N4 C18 C17 -174.2(3) . . . . ? C4 N4 C18 C55 174.4(3) . . . . ? C6 N4 C18 C55 1.2(5) . . . . ? C3 N7 C8 C7 92.5(4) . . . . ? C16 N7 C8 C7 -75.5(4) . . . . ? N6 C7 C8 N7 -95.8(4) . . . . ? C26 C25 C30 C29 -0.2(6) . . . . ? C12 C25 C30 C29 178.3(3) . . . . ? C39 C38 C37 C42 0.0(6) . . . . ? C39 C38 C37 C14 179.7(4) . . . . ? C13 C14 C37 C38 -46.6(6) . . . . ? N5 C14 C37 C38 131.6(4) . . . . ? C13 C14 C37 C42 133.1(4) . . . . ? N5 C14 C37 C42 -48.8(5) . . . . ? C63 C62 C61 C66 1.8(6) . . . . ? C63 C62 C61 C17 177.0(4) . . . . ? C18 C17 C61 C66 54.2(6) . . . . ? N3 C17 C61 C66 -120.4(4) . . . . ? C18 C17 C61 C62 -121.0(5) . . . . ? N3 C17 C61 C62 64.5(5) . . . . ? C17 C18 C55 C56 69.7(6) . . . . ? N4 C18 C55 C56 -104.4(5) . . . . ? C17 C18 C55 C60 -114.8(5) . . . . ? N4 C18 C55 C60 71.0(5) . . . . ? C38 C37 C42 C41 -1.9(6) . . . . ? C14 C37 C42 C41 178.5(4) . . . . ? C48 C43 C44 C45 -0.5(6) . . . . ? C16 C43 C44 C45 176.6(4) . . . . ? C22 C23 C24 C19 -1.1(6) . . . . ? C20 C19 C24 C23 1.4(6) . . . . ? C11 C19 C24 C23 178.9(4) . . . . ? C25 C30 C29 C28 -0.3(6) . . . . ? C14 C13 C31 C32 -95.4(5) . . . . ? N6 C13 C31 C32 79.1(5) . . . . ? C14 C13 C31 C36 86.7(6) . . . . ? N6 C13 C31 C36 -98.7(5) . . . . ? C30 C25 C26 C27 0.7(6) . . . . ? C12 C25 C26 C27 -177.7(4) . . . . ? C24 C19 C20 C21 -0.6(6) . . . . ? C11 C19 C20 C21 -178.1(4) . . . . ? C37 C42 C41 C40 1.7(6) . . . . ? C58 C57 C56 C55 0.1(7) . . . . ? C60 C55 C56 C57 -0.7(6) . . . . ? C18 C55 C56 C57 174.8(4) . . . . ? C51 C50 C49 C54 1.2(6) . . . . ? C51 C50 C49 C15 -177.2(4) . . . . ? C16 C15 C49 C54 66.8(6) . . . . ? N8 C15 C49 C54 -108.3(4) . . . . ? C16 C15 C49 C50 -114.8(5) . . . . ? N8 C15 C49 C50 70.1(5) . . . . ? C30 C29 C28 C27 0.2(6) . . . . ? C43 C44 C45 C46 -1.3(6) . . . . ? C61 C62 C63 C64 -1.3(6) . . . . ? C44 C43 C48 C47 1.9(6) . . . . ? C16 C43 C48 C47 -175.1(4) . . . . ? C56 C57 C58 C59 0.7(8) . . . . ? C25 C26 C27 C28 -0.8(6) . . . . ? C29 C28 C27 C26 0.4(6) . . . . ? C54 C53 C52 C51 0.1(7) . . . . ? C44 C45 C46 C47 1.7(6) . . . . ? C42 C41 C40 C39 0.3(6) . . . . ? C50 C49 C54 C53 -1.4(6) . . . . ? C15 C49 C54 C53 177.0(4) . . . . ? C52 C53 C54 C49 0.8(7) . . . . ? C62 C63 C64 C65 0.6(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? O8 S1 C68 F4 175.1(4) . . . . ? O9 S1 C68 F4 54.3(4) . . . . ? O7 S1 C68 F4 -65.8(4) . . . . ? O8 S1 C68 F5 -65.6(4) . . . . ? O9 S1 C68 F5 173.6(3) . . . . ? O7 S1 C68 F5 53.5(4) . . . . ? O8 S1 C68 F6 55.4(4) . . . . ? O9 S1 C68 F6 -65.5(4) . . . . ? O7 S1 C68 F6 174.4(3) . . . . ? C41 C40 C39 C38 -2.2(7) . . . . ? C37 C38 C39 C40 2.0(7) . . . . ? C45 C46 C47 C48 -0.3(7) . . . . ? C43 C48 C47 C46 -1.5(7) . . . . ? C32 C31 C36 C35 2.7(7) . . . . ? C13 C31 C36 C35 -179.4(4) . . . . ? C53 C52 C51 C50 -0.3(7) . . . . ? C49 C50 C51 C52 -0.4(6) . . . . ? C24 C23 C22 C21 0.2(7) . . . . ? C20 C21 C22 C23 0.6(7) . . . . ? C33 C34 C35 C36 -1.7(9) . . . . ? C31 C36 C35 C34 -0.7(8) . . . . ? C62 C61 C66 C65 -1.7(7) . . . . ? C17 C61 C66 C65 -177.1(5) . . . . ? C63 C64 C65 C66 -0.5(9) . . . . ? C61 C66 C65 C64 1.1(9) . . . . ? C56 C55 C60 C59 0.6(7) . . . . ? C18 C55 C60 C59 -174.8(4) . . . . ? C36 C31 C32 C33 -2.5(7) . . . . ? C13 C31 C32 C33 179.6(5) . . . . ? C35 C34 C33 C32 2.0(10) . . . . ? C31 C32 C33 C34 0.1(9) . . . . ? C57 C58 C59 C60 -0.8(8) . . . . ? C55 C60 C59 C58 0.2(8) . . . . ? O5 S2 C67 F3 -66.1(8) . . . . ? O4 S2 C67 F3 56.1(7) . . . . ? O6 S2 C67 F3 174.3(6) . . . . ? O5 S2 C67 F2 60.5(6) . . . . ? O4 S2 C67 F2 -177.3(5) . . . . ? O6 S2 C67 F2 -59.1(6) . . . . ? O5 S2 C67 F1 174.8(5) . . . . ? O4 S2 C67 F1 -63.0(5) . . . . ? O6 S2 C67 F1 55.2(5) . . . . ? O1 S3 C70 F9 -55.4(14) . . . . ? O3 S3 C70 F9 59.5(13) . . . . ? O2 S3 C70 F9 -172.2(12) . . . . ? O1 S3 C70 F8 175.4(12) . . . . ? O3 S3 C70 F8 -69.7(14) . . . . ? O2 S3 C70 F8 58.5(14) . . . . ? O1 S3 C70 F7 52.6(13) . . . . ? O3 S3 C70 F7 167.5(11) . . . . ? O2 S3 C70 F7 -64.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.707 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.094 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 1.000 697.3 153.8 2 0.114 0.234 0.278 12.9 0.5 3 0.114 0.266 0.778 12.9 0.5 4 0.500 0.500 0.500 697.4 153.1 5 0.886 0.734 0.222 12.9 0.5 6 0.886 0.766 0.722 12.8 0.5 _platon_squeeze_details ; ? ; data_3a _database_code_depnum_ccdc_archive 'CCDC 882738' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C136 H104 Ag4 F12 N16 O12 S4' _chemical_formula_weight 2942.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 17.1508(14) _cell_length_b 16.7972(14) _cell_length_c 24.955(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.2860(10) _cell_angle_gamma 90.00 _cell_volume 6900.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9024 _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78615 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.53 _reflns_number_total 15803 _reflns_number_gt 12499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains disorderness groups in several phenyl rings and one of the triflate anions. Each disordered group was refined with an independently free variable and the position of each atom in the group was splitted into two Parts with the sum of the occupancy equals to 1.The heavy disorderness of the triflate anoin caused a large ADP max/min Ratio for F12 and O21 and atom C8A was refined isotropically. ; _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^)+(0.1161P)^2^+37.3213P] 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 15803 _refine_ls_number_parameters 894 _refine_ls_number_restraints 199 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2372 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.089 _refine_ls_shift/su_mean 0.003 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 C45 C 0.4791(3) 0.1619(4) 0.6048(3) 0.082(4) Uani 1 1 d G . . C50 C 0.5068(4) 0.1017(5) 0.6437(3) 0.096(4) Uani 1 1 d G . . H50 H 0.4923 0.1018 0.6778 0.115 Uiso 1 1 calc R . . C51 C 0.5556(5) 0.0413(4) 0.6328(4) 0.101(4) Uani 1 1 d G . . H51 H 0.5745 0.0002 0.6593 0.121 Uiso 1 1 calc R . . C55 C 0.5767(4) 0.0412(5) 0.5829(4) 0.127(7) Uani 1 1 d G . . H55 H 0.6101 -0.0001 0.5754 0.152 Uiso 1 1 calc R . . C54 C 0.5490(5) 0.1014(6) 0.5440(3) 0.125(6) Uani 1 1 d G . . H54 H 0.5634 0.1013 0.5099 0.150 Uiso 1 1 calc R . . C53 C 0.5002(4) 0.1618(5) 0.5550(3) 0.104(5) Uani 1 1 d G . . H53 H 0.4813 0.2029 0.5284 0.124 Uiso 1 1 calc R . . C64' C 0.5040(5) 0.3611(6) 0.6039(4) 0.046(4) Uani 0.609(17) 1 d PG A 6 C65' C 0.4952(6) 0.4161(8) 0.5610(3) 0.082(7) Uani 0.609(17) 1 d PG A 6 H65' H 0.4431 0.4259 0.5361 0.099 Uiso 0.609(17) 1 calc PR A 6 C66' C 0.5626(7) 0.4567(8) 0.5547(4) 0.117(11) Uani 0.609(17) 1 d PG A 6 H66' H 0.5566 0.4943 0.5253 0.140 Uiso 0.609(17) 1 calc PR A 6 C67' C 0.6389(6) 0.4424(7) 0.5912(5) 0.078(5) Uiso 0.609(17) 1 d PG A 6 H67' H 0.6850 0.4701 0.5868 0.094 Uiso 0.609(17) 1 calc PR A 6 C68' C 0.6477(5) 0.3874(6) 0.6341(5) 0.072(6) Uani 0.609(17) 1 d PG A 6 H68' H 0.6999 0.3775 0.6591 0.086 Uiso 0.609(17) 1 calc PR A 6 C69' C 0.5803(6) 0.3467(5) 0.6405(4) 0.048(4) Uani 0.609(17) 1 d PG A 6 H69' H 0.5863 0.3091 0.6698 0.058 Uiso 0.609(17) 1 calc PR A 6 C64 C 0.5286(6) 0.3281(7) 0.6235(6) 0.028(4) Uani 0.391(17) 1 d PG A 5 C65 C 0.5343(7) 0.3725(8) 0.5777(5) 0.042(4) Uani 0.391(17) 1 d PGU A 5 H65 H 0.4885 0.3774 0.5459 0.050 Uiso 0.391(17) 1 calc PR A 5 C66 C 0.6069(9) 0.4098(9) 0.5784(6) 0.074(7) Uani 0.391(17) 1 d PGU A 5 H66 H 0.6108 0.4402 0.5471 0.089 Uiso 0.391(17) 1 calc PR A 5 C69 C 0.6739(7) 0.4027(10) 0.6249(7) 0.064(7) Uiso 0.391(17) 1 d PG A 5 H69 H 0.7236 0.4282 0.6253 0.077 Uiso 0.391(17) 1 calc PR A 5 C68 C 0.6683(7) 0.3583(10) 0.6706(6) 0.072(7) Uani 0.391(17) 1 d PGU A 5 H68 H 0.7141 0.3535 0.7024 0.087 Uiso 0.391(17) 1 calc PR A 5 C67 C 0.5956(7) 0.3210(8) 0.6699(5) 0.041(4) Uani 0.391(17) 1 d PGU A 5 H67 H 0.5918 0.2907 0.7012 0.049 Uiso 0.391(17) 1 calc PR A 5 C19' C 0.3989(9) 0.6016(7) 0.6311(5) 0.030(5) Uani 0.307(11) 1 d PG B 2 C20' C 0.3395(8) 0.6133(8) 0.5809(6) 0.037(5) Uani 0.307(11) 1 d PGU B 2 H20' H 0.2898 0.5846 0.5732 0.044 Uiso 0.307(11) 1 calc PR B 2 C56' C 0.3526(9) 0.6671(9) 0.5419(5) 0.041(5) Uani 0.307(11) 1 d PGU B 2 H56' H 0.3119 0.6751 0.5076 0.050 Uiso 0.307(11) 1 calc PR B 2 C57' C 0.4252(10) 0.7091(9) 0.5532(6) 0.058(7) Uani 0.307(11) 1 d PGU B 2 H57' H 0.4342 0.7458 0.5266 0.070 Uiso 0.307(11) 1 calc PR B 2 C58' C 0.4847(8) 0.6974(10) 0.6034(7) 0.059(7) Uani 0.307(11) 1 d PGU B 2 H58' H 0.5343 0.7261 0.6111 0.070 Uiso 0.307(11) 1 calc PR B 2 C59' C 0.4716(9) 0.6436(9) 0.6423(5) 0.051(6) Uiso 0.307(11) 1 d PG B 2 H59' H 0.5122 0.6356 0.6766 0.061 Uiso 0.307(11) 1 calc PR B 2 C19 C 0.4366(4) 0.5775(4) 0.6413(3) 0.032(2) Uani 0.693(11) 1 d PG B 1 C59 C 0.5160(4) 0.5670(5) 0.6390(3) 0.068(4) Uani 0.693(11) 1 d PG B 1 H59 H 0.5502 0.5294 0.6629 0.081 Uiso 0.693(11) 1 calc PR B 1 C58 C 0.5452(4) 0.6114(6) 0.6018(4) 0.091(6) Uani 0.693(11) 1 d PG B 1 H58 H 0.5994 0.6042 0.6002 0.109 Uiso 0.693(11) 1 calc PR B 1 C57 C 0.4950(5) 0.6665(5) 0.5669(3) 0.069(4) Uani 0.693(11) 1 d PG B 1 H57 H 0.5150 0.6969 0.5415 0.083 Uiso 0.693(11) 1 calc PR B 1 C56 C 0.4157(5) 0.6770(5) 0.5692(4) 0.073(5) Uani 0.693(11) 1 d PG B 1 H56 H 0.3814 0.7146 0.5454 0.088 Uiso 0.693(11) 1 calc PR B 1 C20 C 0.3864(4) 0.6326(4) 0.6065(3) 0.049(3) Uani 0.693(11) 1 d PG B 1 H20 H 0.3322 0.6398 0.6080 0.058 Uiso 0.693(11) 1 calc PR B 1 Ag2 Ag 0.19212(3) 0.31067(2) 0.622385(16) 0.02711(13) Uani 1 1 d . B . Ag1 Ag 0.33504(2) 0.30768(2) 0.734724(15) 0.02275(13) Uani 1 1 d . . . C3 C 0.3548(3) 0.1839(3) 0.7525(2) 0.0224(10) Uani 1 1 d . . . C6 C 0.4182(3) 0.0674(3) 0.7881(2) 0.0256(10) Uani 1 1 d . . . C1 C 0.3549(3) 0.4285(3) 0.7176(2) 0.0281(11) Uani 1 1 d . B . C44 C 0.3954(4) 0.5587(3) 0.7315(2) 0.0297(11) Uani 1 1 d . B . C40 C 0.4005(5) 0.5370(4) 0.6803(3) 0.0457(17) Uani 1 1 d . . . C7 C 0.4219(4) 0.4744(3) 0.8570(2) 0.0304(12) Uani 1 1 d . . . H7A H 0.4638 0.5157 0.8589 0.037 Uiso 1 1 calc R . . H7B H 0.4052 0.4774 0.8919 0.037 Uiso 1 1 calc R . . C8 C 0.4517(3) 0.1862(3) 0.8505(2) 0.0281(11) Uani 1 1 d . . . H8A H 0.4181 0.1786 0.8765 0.034 Uiso 1 1 calc R . . H8B H 0.5040 0.1586 0.8665 0.034 Uiso 1 1 calc R . . C9 C 0.3487(3) 0.4913(3) 0.8074(2) 0.0254(10) Uani 1 1 d . B . H9A H 0.3067 0.4504 0.8061 0.030 Uiso 1 1 calc R . . H9B H 0.3256 0.5437 0.8129 0.030 Uiso 1 1 calc R . . C10 C 0.3540(6) 0.4224(5) 0.6164(3) 0.062(3) Uani 1 1 d . . . H10A H 0.2957 0.4321 0.5980 0.074 Uiso 1 1 calc R B . H10B H 0.3855 0.4494 0.5939 0.074 Uiso 1 1 calc R . . C11 C 0.2673(3) 0.1301(3) 0.6625(2) 0.0238(10) Uani 1 1 d . . . H11A H 0.2335 0.1775 0.6635 0.029 Uiso 1 1 calc R . . H11B H 0.2312 0.0829 0.6562 0.029 Uiso 1 1 calc R . . C12 C 0.3032(3) 0.1382(4) 0.6139(2) 0.0309(12) Uani 1 1 d . . . H12A H 0.3413 0.0937 0.6147 0.037 Uiso 1 1 calc R . . H12B H 0.2592 0.1348 0.5785 0.037 Uiso 1 1 calc R . . C14 C 0.3538(5) 0.6955(4) 0.7487(3) 0.0454(16) Uani 1 1 d . B . H14 H 0.3014 0.6851 0.7243 0.055 Uiso 1 1 calc R . . C13 C 0.4131(4) 0.6365(3) 0.7594(2) 0.0291(11) Uani 1 1 d . . . C15 C 0.4896(4) 0.6543(4) 0.7939(3) 0.0417(14) Uani 1 1 d . B . H15 H 0.5310 0.6149 0.8011 0.050 Uiso 1 1 calc R . . C17 C 0.4461(5) 0.7853(4) 0.8085(3) 0.0452(17) Uani 1 1 d . B . H17 H 0.4566 0.8359 0.8262 0.054 Uiso 1 1 calc R . . C16 C 0.5065(5) 0.7287(4) 0.8181(3) 0.0456(16) Uani 1 1 d . . . H16 H 0.5594 0.7407 0.8412 0.055 Uiso 1 1 calc R B . C18 C 0.3711(5) 0.7687(4) 0.7736(3) 0.056(2) Uani 1 1 d . . . H18 H 0.3302 0.8086 0.7663 0.068 Uiso 1 1 calc R B . C21 C -0.0360(3) 0.3015(3) 0.6642(3) 0.0317(12) Uani 1 1 d . . . C22 C -0.0295(3) 0.3824(3) 0.6611(3) 0.0335(12) Uani 1 1 d . . . C24 C -0.0847(3) 0.4450(4) 0.6685(4) 0.0463(18) Uani 1 1 d . . . C26 C -0.1034(4) 0.2523(4) 0.6716(4) 0.052(2) Uani 1 1 d . . . C25 C -0.1230(4) 0.4974(4) 0.6253(4) 0.065(2) Uani 1 1 d U . . H25 H -0.1133 0.4925 0.5898 0.078 Uiso 1 1 calc R . . C23 C -0.1013(4) 0.4519(4) 0.7193(4) 0.0549(19) Uani 1 1 d U . . H23 H -0.0757 0.4171 0.7491 0.066 Uiso 1 1 calc R . . C28 C -0.1768(4) 0.2521(5) 0.6310(4) 0.063(2) Uani 1 1 d U . . H28 H -0.1862 0.2874 0.6001 0.075 Uiso 1 1 calc R . . C27 C -0.0934(6) 0.2011(7) 0.7168(7) 0.118(6) Uani 1 1 d U . . H27 H -0.0419 0.1996 0.7439 0.141 Uiso 1 1 calc R . . C30 C 0.4547(4) -0.0090(3) 0.8779(2) 0.0335(12) Uani 1 1 d . . . H30 H 0.4049 0.0069 0.8842 0.040 Uiso 1 1 calc R . . C29 C 0.4742(3) 0.0164(3) 0.8296(2) 0.0303(12) Uani 1 1 d . . . C31 C 0.5074(4) -0.0567(4) 0.9159(3) 0.0445(16) Uani 1 1 d . . . H31 H 0.4933 -0.0745 0.9481 0.053 Uiso 1 1 calc R . . C33 C 0.5487(4) -0.0073(5) 0.8215(3) 0.053(2) Uani 1 1 d . . . H33 H 0.5632 0.0092 0.7892 0.064 Uiso 1 1 calc R . . C32 C 0.5806(5) -0.0790(5) 0.9078(3) 0.060(2) Uani 1 1 d . . . H32 H 0.6173 -0.1112 0.9347 0.072 Uiso 1 1 calc R . . C37 C 0.2735(3) -0.0575(4) 0.6864(2) 0.0309(11) Uani 1 1 d . . . H37 H 0.2297 -0.0330 0.6964 0.037 Uiso 1 1 calc R . . C34 C 0.3519(3) -0.0250(3) 0.7048(2) 0.0291(11) Uani 1 1 d . . . C35 C 0.4148(4) -0.0629(4) 0.6907(3) 0.0410(14) Uani 1 1 d . . . H35 H 0.4684 -0.0421 0.7032 0.049 Uiso 1 1 calc R . . C38 C 0.2600(4) -0.1252(4) 0.6537(3) 0.0413(15) Uani 1 1 d . . . H38 H 0.2069 -0.1470 0.6411 0.050 Uiso 1 1 calc R . . C36 C 0.3999(5) -0.1317(5) 0.6581(4) 0.057(2) Uani 1 1 d . . . H36 H 0.4436 -0.1581 0.6491 0.068 Uiso 1 1 calc R . . C39 C 0.6005(5) -0.0546(7) 0.8608(4) 0.073(3) Uani 1 1 d . . . H39 H 0.6508 -0.0707 0.8553 0.087 Uiso 1 1 calc R . . N2 N 0.3684(3) 0.4917(3) 0.75343(18) 0.0256(9) Uani 1 1 d . . . N3 N 0.0433(3) 0.3959(3) 0.64705(18) 0.0283(10) Uani 1 1 d . . . N1 N 0.3754(4) 0.4583(4) 0.6727(2) 0.0443(14) Uani 1 1 d . B . N6 N 0.3284(2) 0.1218(3) 0.71686(17) 0.0236(9) Uani 1 1 d . . . N5 N 0.4100(2) 0.1490(3) 0.79658(18) 0.0247(9) Uani 1 1 d . . . C4 C 0.3104(4) 0.2851(4) 0.6159(2) 0.0357(14) Uani 1 1 d . . . C42 C 0.4409(5) 0.3023(6) 0.6156(4) 0.074(3) Uani 1 1 d U . . C41 C 0.4278(4) 0.2234(5) 0.6159(3) 0.057(2) Uani 1 1 d U A . C43 C 0.3239(5) -0.1612(4) 0.6393(3) 0.055(2) Uani 1 1 d . . . H43 H 0.3142 -0.2070 0.6160 0.066 Uiso 1 1 calc R . . C2 C 0.0816(3) 0.3283(3) 0.6423(2) 0.0269(11) Uani 1 1 d . . . N9 N 0.3463(3) 0.2139(4) 0.6157(2) 0.0381(13) Uani 1 1 d . A . C46 C 0.3666(3) 0.0504(3) 0.7371(2) 0.0267(10) Uani 1 1 d . . . N8 N 0.3690(4) 0.3395(4) 0.6162(2) 0.0526(18) Uani 1 1 d . A . N7 N 0.0329(3) 0.2699(3) 0.65329(18) 0.0278(9) Uani 1 1 d . . . C47 C -0.1739(5) 0.5552(5) 0.6340(6) 0.084(3) Uani 1 1 d U . . H47 H -0.1980 0.5914 0.6049 0.100 Uiso 1 1 calc R . . S1 S 0.77845(12) 0.76994(19) 0.94830(11) 0.0786(8) Uani 1 1 d . . . C49 C -0.2383(6) 0.1981(8) 0.6362(7) 0.101(5) Uani 1 1 d U . . H49 H -0.2880 0.1947 0.6074 0.122 Uiso 1 1 calc R . . C48 C -0.1555(5) 0.5096(5) 0.7272(5) 0.073(3) Uani 1 1 d U . . H48 H -0.1683 0.5133 0.7618 0.088 Uiso 1 1 calc R . . C52 C -0.1905(5) 0.5615(5) 0.6839(8) 0.108(6) Uani 1 1 d . . . H52 H -0.2264 0.6019 0.6892 0.129 Uiso 1 1 calc R . . O3 O 0.7908(8) 0.8480(7) 0.9848(4) 0.164(6) Uani 1 1 d . . . O1 O 0.6990(5) 0.7498(6) 0.9256(9) 0.239(10) Uani 1 1 d . . . O2 O 0.8384(4) 0.7072(4) 0.9774(3) 0.078(2) Uani 1 1 d . . . F3 F 0.8895(8) 0.8275(8) 0.9150(7) 0.227(8) Uani 1 1 d U . . F2 F 0.7960(10) 0.7272(7) 0.8618(6) 0.257(10) Uani 1 1 d U . . F1 F 0.7682(12) 0.8611(11) 0.8712(10) 0.337(13) Uani 1 1 d U . . C60 C 0.8123(16) 0.8024(12) 0.8921(5) 0.173(11) Uani 1 1 d . . . C61 C -0.1535(7) 0.1526(8) 0.7243(9) 0.162(10) Uani 1 1 d U . . H61 H -0.1454 0.1214 0.7572 0.195 Uiso 1 1 calc R . . C62 C -0.2258(7) 0.1503(7) 0.6834(8) 0.124(7) Uani 1 1 d . . . H62 H -0.2677 0.1158 0.6872 0.149 Uiso 1 1 calc R . . C8A C 0.3754(3) 0.6746(3) 0.9261(2) 0.0000(10) Uiso 0.679(6) 1 d PD C 3 S2 S 0.4140(4) 0.6544(4) 1.0095(3) 0.133(3) Uani 0.679(6) 1 d PD C 3 O21 O 0.4478(12) 0.7180(9) 1.0320(4) 0.191(13) Uani 0.679(6) 1 d PDU C 3 O23 O 0.3302(8) 0.6222(11) 1.0142(7) 0.172(10) Uani 0.679(6) 1 d PDU C 3 O22 O 0.4516(9) 0.5760(6) 1.0150(5) 0.117(5) Uani 0.679(6) 1 d PDU C 3 F12 F 0.3549(16) 0.7455(7) 0.9228(4) 0.275(16) Uani 0.679(6) 1 d PD C 3 F13 F 0.3346(9) 0.6128(9) 0.9091(6) 0.287(18) Uani 0.679(6) 1 d PD C 3 F14 F 0.4448(7) 0.6501(10) 0.9210(6) 0.150(6) Uani 0.679(6) 1 d PD C 3 S2' S 0.3514(3) 0.6507(3) 0.9408(3) 0.065(3) Uani 0.321(6) 1 d PD C 4 C8A' C 0.4393(11) 0.7101(12) 0.9617(9) 0.082(9) Uiso 0.321(6) 1 d PD C 4 F13' F 0.4955(12) 0.6771(12) 0.9416(9) 0.088(4) Uiso 0.321(6) 1 d PD C 4 O22' O 0.3151(10) 0.6442(10) 0.8814(5) 0.052(3) Uiso 0.321(6) 1 d PD C 4 F14' F 0.4136(12) 0.7781(11) 0.9350(9) 0.088(4) Uiso 0.321(6) 1 d PD C 4 O23' O 0.3784(10) 0.5819(8) 0.9838(6) 0.052(3) Uiso 0.321(6) 1 d PD C 4 O21' O 0.3022(9) 0.6874(9) 0.9773(7) 0.052(3) Uiso 0.321(6) 1 d PD C 4 F12' F 0.4653(14) 0.7182(15) 1.0176(8) 0.088(4) Uiso 0.321(6) 1 d PD C 4 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 C45 0.042(4) 0.133(9) 0.092(7) -0.090(7) 0.049(5) -0.055(5) C50 0.122(10) 0.099(8) 0.103(9) -0.035(7) 0.093(8) -0.029(7) C51 0.114(9) 0.087(8) 0.141(11) -0.023(7) 0.100(9) -0.029(7) C55 0.074(7) 0.158(14) 0.175(15) -0.119(12) 0.078(9) -0.041(8) C54 0.099(10) 0.186(17) 0.112(11) -0.078(11) 0.066(9) -0.012(10) C53 0.099(8) 0.148(11) 0.090(8) -0.068(8) 0.069(7) -0.044(8) C64' 0.046(7) 0.048(8) 0.060(8) -0.034(7) 0.039(7) -0.029(6) C65' 0.098(13) 0.123(16) 0.032(6) -0.011(8) 0.027(7) -0.081(13) C66' 0.115(16) 0.19(2) 0.048(8) -0.002(11) 0.032(9) -0.114(18) C68' 0.064(9) 0.056(8) 0.115(15) -0.049(10) 0.055(10) -0.024(8) C69' 0.049(8) 0.037(7) 0.070(9) -0.028(6) 0.036(7) -0.013(5) C64 0.015(8) 0.020(7) 0.055(11) -0.024(7) 0.019(7) -0.008(6) C65 0.047(8) 0.035(7) 0.054(8) -0.006(6) 0.029(7) -0.008(6) C66 0.083(11) 0.071(11) 0.087(11) -0.010(8) 0.055(9) -0.005(8) C68 0.053(9) 0.070(10) 0.091(11) -0.021(8) 0.013(8) 0.001(8) C67 0.027(6) 0.036(7) 0.059(9) -0.008(6) 0.009(6) 0.000(5) C19' 0.055(14) 0.007(8) 0.032(11) -0.010(7) 0.021(11) -0.004(8) C20' 0.048(9) 0.027(7) 0.038(8) 0.001(6) 0.016(7) 0.006(7) C56' 0.047(9) 0.038(8) 0.041(8) -0.003(7) 0.018(7) 0.001(7) C57' 0.064(11) 0.061(11) 0.055(10) -0.001(8) 0.027(8) 0.005(8) C58' 0.063(10) 0.055(10) 0.062(11) -0.001(8) 0.024(8) -0.016(8) C19 0.044(5) 0.036(5) 0.020(4) -0.008(4) 0.015(4) -0.013(4) C59 0.054(7) 0.104(11) 0.045(6) 0.020(6) 0.015(5) -0.027(7) C58 0.049(7) 0.166(17) 0.063(8) 0.038(10) 0.026(6) -0.026(9) C57 0.078(9) 0.104(11) 0.037(6) 0.006(6) 0.033(6) -0.030(8) C56 0.105(12) 0.048(7) 0.088(10) 0.038(7) 0.062(10) 0.027(7) C20 0.048(6) 0.039(6) 0.069(8) 0.017(5) 0.033(6) 0.017(5) Ag2 0.0329(2) 0.0304(2) 0.0180(2) -0.00195(14) 0.00699(16) -0.01254(15) Ag1 0.0199(2) 0.0306(2) 0.0181(2) -0.00496(13) 0.00584(14) -0.00239(13) C3 0.016(2) 0.031(3) 0.021(2) -0.0048(19) 0.0063(18) -0.0010(18) C6 0.018(2) 0.031(3) 0.028(2) -0.005(2) 0.0082(19) 0.0025(19) C1 0.025(2) 0.039(3) 0.022(2) -0.007(2) 0.0079(19) -0.012(2) C44 0.037(3) 0.034(3) 0.022(2) -0.003(2) 0.014(2) -0.006(2) C40 0.064(4) 0.051(4) 0.029(3) -0.017(3) 0.025(3) -0.034(3) C7 0.040(3) 0.027(3) 0.019(2) -0.008(2) -0.001(2) 0.015(2) C8 0.025(2) 0.032(3) 0.024(3) -0.008(2) 0.000(2) 0.003(2) C9 0.026(2) 0.035(3) 0.017(2) 0.0008(19) 0.0085(19) 0.009(2) C10 0.106(7) 0.065(5) 0.027(3) -0.024(3) 0.038(4) -0.060(5) C11 0.016(2) 0.035(3) 0.019(2) -0.002(2) 0.0031(17) -0.0038(19) C12 0.025(2) 0.046(3) 0.024(2) -0.012(2) 0.011(2) -0.013(2) C14 0.045(4) 0.045(4) 0.038(3) -0.005(3) -0.002(3) 0.008(3) C13 0.038(3) 0.032(3) 0.020(2) -0.002(2) 0.013(2) -0.002(2) C15 0.044(3) 0.030(3) 0.046(4) -0.010(3) 0.005(3) 0.005(3) C17 0.080(5) 0.025(3) 0.026(3) -0.002(2) 0.007(3) 0.005(3) C16 0.051(4) 0.039(3) 0.039(3) -0.011(3) -0.001(3) -0.003(3) C18 0.073(5) 0.038(4) 0.052(4) -0.003(3) 0.009(4) 0.022(4) C21 0.019(2) 0.030(3) 0.042(3) 0.013(2) 0.002(2) 0.000(2) C22 0.026(3) 0.029(3) 0.039(3) 0.010(2) -0.003(2) -0.003(2) C24 0.020(3) 0.023(3) 0.087(5) 0.020(3) 0.000(3) -0.004(2) C26 0.029(3) 0.019(3) 0.113(7) 0.013(3) 0.030(4) 0.000(2) C25 0.038(3) 0.028(3) 0.101(6) 0.022(3) -0.023(4) -0.006(3) C23 0.043(3) 0.032(3) 0.094(5) 0.016(3) 0.027(4) 0.010(3) C28 0.032(3) 0.067(5) 0.088(6) -0.041(5) 0.016(4) -0.015(3) C27 0.041(5) 0.116(9) 0.212(15) 0.120(10) 0.061(7) 0.029(5) C30 0.032(3) 0.033(3) 0.031(3) -0.007(2) -0.001(2) 0.008(2) C29 0.023(2) 0.033(3) 0.029(3) -0.012(2) -0.001(2) 0.006(2) C31 0.053(4) 0.047(4) 0.025(3) -0.006(3) -0.004(3) 0.014(3) C33 0.033(3) 0.085(6) 0.041(4) 0.006(4) 0.009(3) 0.027(4) C32 0.048(4) 0.078(6) 0.043(4) -0.004(4) -0.007(3) 0.036(4) C37 0.028(3) 0.033(3) 0.028(3) 0.000(2) 0.002(2) 0.000(2) C34 0.028(3) 0.030(3) 0.029(3) -0.005(2) 0.007(2) 0.000(2) C35 0.036(3) 0.046(4) 0.045(4) -0.010(3) 0.017(3) 0.002(3) C38 0.045(4) 0.031(3) 0.038(3) -0.007(3) -0.005(3) -0.005(3) C36 0.060(5) 0.049(4) 0.064(5) -0.017(4) 0.021(4) 0.016(4) C39 0.039(4) 0.111(8) 0.065(5) 0.008(5) 0.010(4) 0.041(5) N2 0.027(2) 0.031(2) 0.020(2) -0.0051(17) 0.0091(17) -0.0024(18) N3 0.028(2) 0.028(2) 0.023(2) 0.0106(17) -0.0016(17) -0.0069(18) N1 0.060(3) 0.053(3) 0.028(3) -0.019(2) 0.026(2) -0.034(3) N6 0.0179(19) 0.035(2) 0.0180(19) -0.0071(17) 0.0045(15) -0.0028(17) N5 0.0186(19) 0.029(2) 0.026(2) -0.0067(17) 0.0045(16) 0.0030(16) C4 0.040(3) 0.053(4) 0.019(2) -0.016(2) 0.016(2) -0.025(3) C42 0.064(5) 0.113(7) 0.068(5) -0.071(5) 0.058(4) -0.068(5) C41 0.038(3) 0.092(6) 0.053(4) -0.055(4) 0.034(3) -0.041(4) C43 0.074(5) 0.032(3) 0.049(4) -0.017(3) 0.003(4) 0.008(3) C2 0.027(3) 0.032(3) 0.018(2) 0.004(2) 0.0000(19) -0.011(2) N9 0.035(3) 0.059(3) 0.026(2) -0.020(2) 0.019(2) -0.027(2) C46 0.020(2) 0.034(3) 0.028(3) -0.004(2) 0.0087(19) -0.001(2) N8 0.069(4) 0.067(4) 0.037(3) -0.033(3) 0.039(3) -0.048(3) N7 0.022(2) 0.035(2) 0.023(2) 0.0070(18) 0.0019(17) -0.0054(18) C47 0.036(4) 0.042(4) 0.146(8) 0.027(5) -0.018(5) -0.001(3) S1 0.0293(9) 0.120(2) 0.0826(16) -0.0499(16) 0.0097(9) -0.0072(11) C49 0.046(5) 0.119(10) 0.156(12) -0.083(9) 0.058(7) -0.033(6) C48 0.055(4) 0.043(4) 0.128(7) 0.004(4) 0.036(5) 0.013(3) C52 0.029(4) 0.019(3) 0.261(18) 0.017(6) 0.017(7) 0.010(3) O3 0.257(14) 0.185(10) 0.073(5) 0.044(6) 0.085(7) 0.173(11) O1 0.035(4) 0.068(5) 0.58(3) -0.022(11) 0.037(9) 0.010(4) O2 0.054(4) 0.075(4) 0.107(6) 0.009(4) 0.029(4) 0.023(3) F3 0.148(9) 0.216(13) 0.316(18) 0.201(14) 0.065(11) 0.019(9) F2 0.286(16) 0.121(8) 0.247(14) -0.083(9) -0.115(12) 0.102(10) F1 0.264(18) 0.246(17) 0.48(3) 0.24(2) 0.069(18) 0.141(15) C60 0.27(3) 0.180(18) 0.034(5) 0.002(7) -0.016(9) 0.145(18) C61 0.057(6) 0.112(10) 0.35(3) 0.144(14) 0.107(11) 0.035(6) C62 0.082(8) 0.053(6) 0.28(2) 0.023(9) 0.118(12) 0.001(5) S2 0.126(5) 0.111(5) 0.135(6) 0.044(4) -0.007(4) -0.012(4) O21 0.32(3) 0.180(16) 0.029(5) -0.041(7) -0.017(9) 0.185(19) O23 0.113(11) 0.230(19) 0.213(17) 0.168(16) 0.110(12) 0.113(12) O22 0.189(14) 0.067(7) 0.063(7) 0.011(5) -0.016(8) 0.033(8) F12 0.60(4) 0.118(10) 0.035(5) -0.003(5) -0.026(10) 0.243(18) F13 0.29(3) 0.50(4) 0.088(10) 0.096(16) 0.081(13) 0.32(3) F14 0.095(8) 0.209(15) 0.140(11) -0.114(11) 0.022(7) 0.016(9) S2' 0.021(2) 0.013(2) 0.137(7) -0.005(3) -0.021(3) -0.0018(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 C45 C50 1.3900 . ? C45 C53 1.3900 . ? C45 C41 1.432(10) . ? C50 C51 1.3900 . ? C50 H50 0.9500 . ? C51 C55 1.3900 . ? C51 H51 0.9500 . ? C55 C54 1.3900 . ? C55 H55 0.9500 . ? C54 C53 1.3900 . ? C54 H54 0.9500 . ? C53 H53 0.9500 . ? C64' C65' 1.3900 . ? C64' C69' 1.3900 . ? C64' C42 1.552(9) . ? C65' C66' 1.3900 . ? C65' H65' 0.9500 . ? C66' C67' 1.3900 . ? C66' H66' 0.9500 . ? C67' C68' 1.3900 . ? C67' H67' 0.9500 . ? C68' C69' 1.3900 . ? C68' H68' 0.9500 . ? C69' H69' 0.9500 . ? C64 C65 1.3900 . ? C64 C67 1.3900 . ? C64 C42 1.525(11) . ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 C69 1.3900 . ? C66 H66 0.9500 . ? C69 C68 1.3900 . ? C69 H69 0.9500 . ? C68 C67 1.3900 . ? C68 H68 0.9500 . ? C67 H67 0.9500 . ? C19' C20' 1.3900 . ? C19' C59' 1.3900 . ? C19' C40 1.634(12) . ? C20' C56' 1.3900 . ? C20' H20' 0.9500 . ? C56' C57' 1.3900 . ? C56' H56' 0.9500 . ? C57' C58' 1.3900 . ? C57' H57' 0.9500 . ? C58' C59' 1.3900 . ? C58' H58' 0.9500 . ? C59' H59' 0.9500 . ? C19 C59 1.3900 . ? C19 C20 1.3900 . ? C19 C40 1.460(7) . ? C59 C58 1.3900 . ? C59 H59 0.9500 . ? C58 C57 1.3900 . ? C58 H58 0.9500 . ? C57 C56 1.3900 . ? C57 H57 0.9500 . ? C56 C20 1.3900 . ? C56 H56 0.9500 . ? C20 H20 0.9500 . ? Ag2 C2 2.111(6) . ? Ag2 C4 2.123(6) . ? Ag2 Ag1 3.1648(6) . ? Ag1 C1 2.121(6) . ? Ag1 C3 2.134(5) . ? Ag1 Ag1 3.2152(8) 2_556 ? C3 N6 1.363(6) . ? C3 N5 1.366(7) . ? C6 C46 1.361(7) . ? C6 N5 1.399(7) . ? C6 C29 1.473(7) . ? C1 N1 1.361(7) . ? C1 N2 1.366(7) . ? C44 C40 1.353(8) . ? C44 N2 1.387(7) . ? C44 C13 1.471(8) . ? C40 N1 1.387(8) . ? C7 N3 1.463(6) 2_556 ? C7 C9 1.522(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N7 1.439(7) 2_556 ? C8 N5 1.474(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.478(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N8 1.417(11) . ? C10 N1 1.477(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N6 1.471(6) . ? C11 C12 1.511(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N9 1.464(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C18 1.371(10) . ? C14 C13 1.392(9) . ? C14 H14 0.9500 . ? C13 C15 1.386(9) . ? C15 C16 1.384(9) . ? C15 H15 0.9500 . ? C17 C18 1.365(11) . ? C17 C16 1.376(10) . ? C17 H17 0.9500 . ? C16 H16 0.9500 . ? C18 H18 0.9500 . ? C21 C22 1.368(8) . ? C21 N7 1.389(8) . ? C21 C26 1.474(8) . ? C22 N3 1.408(8) . ? C22 C24 1.462(9) . ? C24 C23 1.379(12) . ? C24 C25 1.403(9) . ? C26 C28 1.376(11) . ? C26 C27 1.391(13) . ? C25 C47 1.364(15) . ? C25 H25 0.9500 . ? C23 C48 1.394(10) . ? C23 H23 0.9500 . ? C28 C49 1.425(14) . ? C28 H28 0.9500 . ? C27 C61 1.368(13) . ? C27 H27 0.9500 . ? C30 C31 1.369(8) . ? C30 C29 1.405(9) . ? C30 H30 0.9500 . ? C29 C33 1.406(8) . ? C31 C32 1.379(10) . ? C31 H31 0.9500 . ? C33 C39 1.375(11) . ? C33 H33 0.9500 . ? C32 C39 1.372(13) . ? C32 H32 0.9500 . ? C37 C38 1.379(8) . ? C37 C34 1.404(8) . ? C37 H37 0.9500 . ? C34 C35 1.382(8) . ? C34 C46 1.484(8) . ? C35 C36 1.395(10) . ? C35 H35 0.9500 . ? C38 C43 1.385(11) . ? C38 H38 0.9500 . ? C36 C43 1.349(12) . ? C36 H36 0.9500 . ? C39 H39 0.9500 . ? N3 C2 1.333(8) . ? N3 C7 1.463(6) 2_556 ? N6 C46 1.392(7) . ? C4 N9 1.346(9) . ? C4 N8 1.357(7) . ? C42 C41 1.345(13) . ? C42 N8 1.386(12) . ? C41 N9 1.406(7) . ? C43 H43 0.9500 . ? C2 N7 1.365(7) . ? N7 C8 1.439(7) 2_556 ? C47 C52 1.356(19) . ? C47 H47 0.9500 . ? S1 O1 1.363(9) . ? S1 O2 1.509(7) . ? S1 O3 1.577(12) . ? S1 C60 1.75(2) . ? C49 C62 1.39(2) . ? C49 H49 0.9500 . ? C48 C52 1.387(16) . ? C48 H48 0.9500 . ? C52 H52 0.9500 . ? F3 C60 1.35(3) . ? F2 C60 1.46(2) . ? F1 C60 1.263(16) . ? C61 C62 1.37(2) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C8A F12 1.236(9) . ? C8A F13 1.257(17) . ? C8A F14 1.300(11) . ? C8A S2 2.029(8) . ? S2 O21 1.268(15) . ? S2 O22 1.456(11) . ? S2 O23 1.569(13) . ? S2' O22' 1.443(11) . ? S2' O21' 1.533(13) . ? S2' O23' 1.557(13) . ? S2' C8A' 1.761(16) . ? C8A' F13' 1.326(17) . ? C8A' F14' 1.334(18) . ? C8A' F12' 1.347(17) . ? 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 C50 C45 C53 120.0 . . ? C50 C45 C41 119.9(6) . . ? C53 C45 C41 120.1(6) . . ? C51 C50 C45 120.0 . . ? C51 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C55 C51 C50 120.0 . . ? C55 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C55 C54 120.0 . . ? C51 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C53 C45 120.0 . . ? C54 C53 H53 120.0 . . ? C45 C53 H53 120.0 . . ? C65' C64' C69' 120.0 . . ? C65' C64' C42 129.5(7) . . ? C69' C64' C42 110.1(8) . . ? C66' C65' C64' 120.0 . . ? C66' C65' H65' 120.0 . . ? C64' C65' H65' 120.0 . . ? C67' C66' C65' 120.0 . . ? C67' C66' H66' 120.0 . . ? C65' C66' H66' 120.0 . . ? C66' C67' C68' 120.0 . . ? C66' C67' H67' 120.0 . . ? C68' C67' H67' 120.0 . . ? C69' C68' C67' 120.0 . . ? C69' C68' H68' 120.0 . . ? C67' C68' H68' 120.0 . . ? C68' C69' C64' 120.0 . . ? C68' C69' H69' 120.0 . . ? C64' C69' H69' 120.0 . . ? C65 C64 C67 120.0 . . ? C65 C64 C42 109.9(9) . . ? C67 C64 C42 129.6(9) . . ? C64 C65 C66 120.0 . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C69 C66 C65 120.0 . . ? C69 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C69 C68 120.0 . . ? C66 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C68 C67 C64 120.0 . . ? C68 C67 H67 120.0 . . ? C64 C67 H67 120.0 . . ? C20' C19' C59' 120.0 . . ? C20' C19' C40 128.7(9) . . ? C59' C19' C40 111.1(9) . . ? C56' C20' C19' 120.0 . . ? C56' C20' H20' 120.0 . . ? C19' C20' H20' 120.0 . . ? C20' C56' C57' 120.0 . . ? C20' C56' H56' 120.0 . . ? C57' C56' H56' 120.0 . . ? C58' C57' C56' 120.0 . . ? C58' C57' H57' 120.0 . . ? C56' C57' H57' 120.0 . . ? C59' C58' C57' 120.0 . . ? C59' C58' H58' 120.0 . . ? C57' C58' H58' 120.0 . . ? C58' C59' C19' 120.0 . . ? C58' C59' H59' 120.0 . . ? C19' C59' H59' 120.0 . . ? C59 C19 C20 120.0 . . ? C59 C19 C40 124.8(6) . . ? C20 C19 C40 115.1(6) . . ? C58 C59 C19 120.0 . . ? C58 C59 H59 120.0 . . ? C19 C59 H59 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C57 C56 C20 120.0 . . ? C57 C56 H56 120.0 . . ? C20 C56 H56 120.0 . . ? C56 C20 C19 120.0 . . ? C56 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C2 Ag2 C4 170.5(2) . . ? C2 Ag2 Ag1 108.48(14) . . ? C4 Ag2 Ag1 62.93(14) . . ? C1 Ag1 C3 161.7(2) . . ? C1 Ag1 Ag2 86.25(14) . . ? C3 Ag1 Ag2 103.79(13) . . ? C1 Ag1 Ag1 104.82(15) . 2_556 ? C3 Ag1 Ag1 93.02(13) . 2_556 ? Ag2 Ag1 Ag1 71.413(16) . 2_556 ? N6 C3 N5 103.1(4) . . ? N6 C3 Ag1 127.2(4) . . ? N5 C3 Ag1 128.3(4) . . ? C46 C6 N5 106.3(5) . . ? C46 C6 C29 131.2(5) . . ? N5 C6 C29 122.5(5) . . ? N1 C1 N2 102.6(5) . . ? N1 C1 Ag1 127.7(4) . . ? N2 C1 Ag1 128.3(4) . . ? C40 C44 N2 105.7(5) . . ? C40 C44 C13 128.8(5) . . ? N2 C44 C13 125.5(5) . . ? C44 C40 N1 106.7(5) . . ? C44 C40 C19 130.9(6) . . ? N1 C40 C19 121.7(6) . . ? C44 C40 C19' 122.6(7) . . ? N1 C40 C19' 126.2(7) . . ? C19 C40 C19' 27.1(5) . . ? N3 C7 C9 111.8(4) 2_556 . ? N3 C7 H7A 109.3 2_556 . ? C9 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 2_556 . ? C9 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N7 C8 N5 113.9(5) 2_556 . ? N7 C8 H8A 108.8 2_556 . ? N5 C8 H8A 108.8 . . ? N7 C8 H8B 108.8 2_556 . ? N5 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C7 113.3(4) . . ? N2 C9 H9A 108.9 . . ? C7 C9 H9A 108.9 . . ? N2 C9 H9B 108.9 . . ? C7 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N8 C10 N1 114.0(7) . . ? N8 C10 H10A 108.7 . . ? N1 C10 H10A 108.7 . . ? N8 C10 H10B 108.7 . . ? N1 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N6 C11 C12 113.8(4) . . ? N6 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N9 C12 C11 111.7(4) . . ? N9 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N9 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C18 C14 C13 119.9(7) . . ? C18 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C15 C13 C14 118.7(6) . . ? C15 C13 C44 121.3(5) . . ? C14 C13 C44 120.0(6) . . ? C16 C15 C13 120.7(6) . . ? C16 C15 H15 119.6 . . ? C13 C15 H15 119.6 . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C16 C15 119.6(6) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C17 C18 C14 121.2(7) . . ? C17 C18 H18 119.4 . . ? C14 C18 H18 119.4 . . ? C22 C21 N7 106.3(5) . . ? C22 C21 C26 130.0(6) . . ? N7 C21 C26 123.5(5) . . ? C21 C22 N3 105.4(5) . . ? C21 C22 C24 130.0(6) . . ? N3 C22 C24 124.6(5) . . ? C23 C24 C25 118.8(7) . . ? C23 C24 C22 119.0(6) . . ? C25 C24 C22 122.2(8) . . ? C28 C26 C27 118.4(8) . . ? C28 C26 C21 119.7(7) . . ? C27 C26 C21 121.7(7) . . ? C47 C25 C24 120.4(11) . . ? C47 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C24 C23 C48 120.3(8) . . ? C24 C23 H23 119.8 . . ? C48 C23 H23 119.8 . . ? C26 C28 C49 118.8(11) . . ? C26 C28 H28 120.6 . . ? C49 C28 H28 120.6 . . ? C61 C27 C26 123.6(12) . . ? C61 C27 H27 118.2 . . ? C26 C27 H27 118.2 . . ? C31 C30 C29 120.2(6) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C29 C33 118.8(6) . . ? C30 C29 C6 121.0(5) . . ? C33 C29 C6 120.3(6) . . ? C30 C31 C32 120.5(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C39 C33 C29 119.5(7) . . ? C39 C33 H33 120.2 . . ? C29 C33 H33 120.2 . . ? C39 C32 C31 120.0(7) . . ? C39 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C38 C37 C34 120.0(6) . . ? C38 C37 H37 120.0 . . ? C34 C37 H37 120.0 . . ? C35 C34 C37 118.8(5) . . ? C35 C34 C46 120.4(5) . . ? C37 C34 C46 120.8(5) . . ? C34 C35 C36 120.1(6) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C38 C43 120.0(6) . . ? C37 C38 H38 120.0 . . ? C43 C38 H38 120.0 . . ? C43 C36 C35 120.6(7) . . ? C43 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C32 C39 C33 121.0(7) . . ? C32 C39 H39 119.5 . . ? C33 C39 H39 119.5 . . ? C1 N2 C44 112.7(4) . . ? C1 N2 C9 123.6(5) . . ? C44 N2 C9 123.5(4) . . ? C2 N3 C22 112.2(4) . . ? C2 N3 C7 122.8(5) . 2_556 ? C22 N3 C7 124.7(5) . 2_556 ? C1 N1 C40 112.3(5) . . ? C1 N1 C10 125.5(5) . . ? C40 N1 C10 120.4(5) . . ? C3 N6 C46 112.6(4) . . ? C3 N6 C11 123.4(5) . . ? C46 N6 C11 123.9(4) . . ? C3 N5 C6 112.0(4) . . ? C3 N5 C8 127.0(4) . . ? C6 N5 C8 120.7(4) . . ? N9 C4 N8 105.0(6) . . ? N9 C4 Ag2 128.9(4) . . ? N8 C4 Ag2 125.8(6) . . ? C41 C42 N8 107.1(6) . . ? C41 C42 C64 116.1(9) . . ? N8 C42 C64 136.0(8) . . ? C41 C42 C64' 139.0(8) . . ? N8 C42 C64' 112.7(9) . . ? C64 C42 C64' 29.3(5) . . ? C42 C41 N9 106.2(7) . . ? C42 C41 C45 126.7(6) . . ? N9 C41 C45 125.5(6) . . ? C36 C43 C38 120.4(6) . . ? C36 C43 H43 119.8 . . ? C38 C43 H43 119.8 . . ? N3 C2 N7 104.4(5) . . ? N3 C2 Ag2 129.6(4) . . ? N7 C2 Ag2 126.0(4) . . ? C4 N9 C41 110.8(6) . . ? C4 N9 C12 122.9(5) . . ? C41 N9 C12 126.3(6) . . ? C6 C46 N6 106.0(5) . . ? C6 C46 C34 130.9(5) . . ? N6 C46 C34 123.1(5) . . ? C4 N8 C42 110.9(7) . . ? C4 N8 C10 121.8(7) . . ? C42 N8 C10 127.2(6) . . ? C2 N7 C21 111.6(5) . . ? C2 N7 C8 123.6(5) . 2_556 ? C21 N7 C8 124.6(5) . 2_556 ? C52 C47 C25 120.7(9) . . ? C52 C47 H47 119.7 . . ? C25 C47 H47 119.7 . . ? O1 S1 O2 119.6(6) . . ? O1 S1 O3 113.8(8) . . ? O2 S1 O3 109.9(5) . . ? O1 S1 C60 105.2(12) . . ? O2 S1 C60 105.5(6) . . ? O3 S1 C60 100.5(8) . . ? C62 C49 C28 120.1(12) . . ? C62 C49 H49 119.9 . . ? C28 C49 H49 119.9 . . ? C52 C48 C23 119.2(11) . . ? C52 C48 H48 120.4 . . ? C23 C48 H48 120.4 . . ? C47 C52 C48 120.6(9) . . ? C47 C52 H52 119.7 . . ? C48 C52 H52 119.7 . . ? F1 C60 F3 109(2) . . ? F1 C60 F2 117.1(19) . . ? F3 C60 F2 120.8(17) . . ? F1 C60 S1 106.2(18) . . ? F3 C60 S1 105.3(9) . . ? F2 C60 S1 95.0(18) . . ? C62 C61 C27 118.4(13) . . ? C62 C61 H61 120.8 . . ? C27 C61 H61 120.8 . . ? C61 C62 C49 120.6(9) . . ? C61 C62 H62 119.7 . . ? C49 C62 H62 119.7 . . ? F12 C8A F13 130.7(14) . . ? F12 C8A F14 123.3(16) . . ? F13 C8A F14 98.3(10) . . ? F12 C8A S2 103.5(5) . . ? F13 C8A S2 101.4(8) . . ? F14 C8A S2 90.1(7) . . ? O21 S2 O22 125.7(10) . . ? O21 S2 O23 124.8(13) . . ? O22 S2 O23 94.2(9) . . ? O21 S2 C8A 106.9(8) . . ? O22 S2 C8A 104.9(7) . . ? O23 S2 C8A 95.3(7) . . ? O22' S2' O21' 119.3(10) . . ? O22' S2' O23' 127.7(10) . . ? O21' S2' O23' 89.8(9) . . ? O22' S2' C8A' 115.7(10) . . ? O21' S2' C8A' 99.5(9) . . ? O23' S2' C8A' 98.7(9) . . ? F13' C8A' F14' 110.0(18) . . ? F13' C8A' F12' 111.8(19) . . ? F14' C8A' F12' 113.4(19) . . ? F13' C8A' S2' 107.7(15) . . ? F14' C8A' S2' 101.6(14) . . ? F12' C8A' S2' 111.7(15) . . ? 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 C53 C45 C50 C51 0.0 . . . . ? C41 C45 C50 C51 179.1(5) . . . . ? C45 C50 C51 C55 0.0 . . . . ? C50 C51 C55 C54 0.0 . . . . ? C51 C55 C54 C53 0.0 . . . . ? C55 C54 C53 C45 0.0 . . . . ? C50 C45 C53 C54 0.0 . . . . ? C41 C45 C53 C54 -179.1(5) . . . . ? C69' C64' C65' C66' 0.0 . . . . ? C42 C64' C65' C66' -172.5(9) . . . . ? C64' C65' C66' C67' 0.0 . . . . ? C65' C66' C67' C68' 0.0 . . . . ? C66' C67' C68' C69' 0.0 . . . . ? C67' C68' C69' C64' 0.0 . . . . ? C65' C64' C69' C68' 0.0 . . . . ? C42 C64' C69' C68' 173.8(7) . . . . ? C67 C64 C65 C66 0.0 . . . . ? C42 C64 C65 C66 172.9(9) . . . . ? C64 C65 C66 C69 0.0 . . . . ? C65 C66 C69 C68 0.0 . . . . ? C66 C69 C68 C67 0.0 . . . . ? C69 C68 C67 C64 0.0 . . . . ? C65 C64 C67 C68 0.0 . . . . ? C42 C64 C67 C68 -171.4(12) . . . . ? C59' C19' C20' C56' 0.0 . . . . ? C40 C19' C20' C56' -174.3(13) . . . . ? C19' C20' C56' C57' 0.0 . . . . ? C20' C56' C57' C58' 0.0 . . . . ? C56' C57' C58' C59' 0.0 . . . . ? C57' C58' C59' C19' 0.0 . . . . ? C20' C19' C59' C58' 0.0 . . . . ? C40 C19' C59' C58' 175.2(11) . . . . ? C20 C19 C59 C58 0.0 . . . . ? C40 C19 C59 C58 -177.1(7) . . . . ? C19 C59 C58 C57 0.0 . . . . ? C59 C58 C57 C56 0.0 . . . . ? C58 C57 C56 C20 0.0 . . . . ? C57 C56 C20 C19 0.0 . . . . ? C59 C19 C20 C56 0.0 . . . . ? C40 C19 C20 C56 177.4(6) . . . . ? C2 Ag2 Ag1 C1 -98.5(2) . . . . ? C4 Ag2 Ag1 C1 86.0(2) . . . . ? C2 Ag2 Ag1 C3 97.0(2) . . . . ? C4 Ag2 Ag1 C3 -78.5(2) . . . . ? C2 Ag2 Ag1 Ag1 8.50(16) . . . 2_556 ? C4 Ag2 Ag1 Ag1 -167.0(2) . . . 2_556 ? C1 Ag1 C3 N6 -105.9(7) . . . . ? Ag2 Ag1 C3 N6 15.9(4) . . . . ? Ag1 Ag1 C3 N6 87.5(4) 2_556 . . . ? C1 Ag1 C3 N5 58.3(8) . . . . ? Ag2 Ag1 C3 N5 -179.9(4) . . . . ? Ag1 Ag1 C3 N5 -108.3(4) 2_556 . . . ? C3 Ag1 C1 N1 63.0(9) . . . . ? Ag2 Ag1 C1 N1 -61.1(5) . . . . ? Ag1 Ag1 C1 N1 -130.8(5) 2_556 . . . ? C3 Ag1 C1 N2 -100.8(7) . . . . ? Ag2 Ag1 C1 N2 135.1(5) . . . . ? Ag1 Ag1 C1 N2 65.5(5) 2_556 . . . ? N2 C44 C40 N1 0.9(8) . . . . ? C13 C44 C40 N1 -178.4(6) . . . . ? N2 C44 C40 C19 -169.4(8) . . . . ? C13 C44 C40 C19 11.4(14) . . . . ? N2 C44 C40 C19' 158.2(8) . . . . ? C13 C44 C40 C19' -21.0(12) . . . . ? C59 C19 C40 C44 92.1(10) . . . . ? C20 C19 C40 C44 -85.1(10) . . . . ? C59 C19 C40 N1 -76.9(9) . . . . ? C20 C19 C40 N1 105.9(8) . . . . ? C59 C19 C40 C19' 174.7(15) . . . . ? C20 C19 C40 C19' -2.5(12) . . . . ? C20' C19' C40 C44 -112.3(10) . . . . ? C59' C19' C40 C44 72.9(10) . . . . ? C20' C19' C40 N1 40.5(15) . . . . ? C59' C19' C40 N1 -134.2(9) . . . . ? C20' C19' C40 C19 130.6(18) . . . . ? C59' C19' C40 C19 -44.2(12) . . . . ? N3 C7 C9 N2 -61.5(7) 2_556 . . . ? N6 C11 C12 N9 -68.0(6) . . . . ? C18 C14 C13 C15 -1.8(11) . . . . ? C18 C14 C13 C44 -178.2(7) . . . . ? C40 C44 C13 C15 -91.7(9) . . . . ? N2 C44 C13 C15 89.2(8) . . . . ? C40 C44 C13 C14 84.6(9) . . . . ? N2 C44 C13 C14 -94.6(8) . . . . ? C14 C13 C15 C16 1.0(10) . . . . ? C44 C13 C15 C16 177.3(6) . . . . ? C18 C17 C16 C15 -2.6(12) . . . . ? C13 C15 C16 C17 1.2(11) . . . . ? C16 C17 C18 C14 1.8(13) . . . . ? C13 C14 C18 C17 0.4(13) . . . . ? N7 C21 C22 N3 1.3(6) . . . . ? C26 C21 C22 N3 -173.0(7) . . . . ? N7 C21 C22 C24 179.6(6) . . . . ? C26 C21 C22 C24 5.3(12) . . . . ? C21 C22 C24 C23 61.4(10) . . . . ? N3 C22 C24 C23 -120.6(7) . . . . ? C21 C22 C24 C25 -117.1(8) . . . . ? N3 C22 C24 C25 60.9(9) . . . . ? C22 C21 C26 C28 64.6(11) . . . . ? N7 C21 C26 C28 -108.8(7) . . . . ? C22 C21 C26 C27 -120.3(11) . . . . ? N7 C21 C26 C27 66.3(12) . . . . ? C23 C24 C25 C47 1.7(10) . . . . ? C22 C24 C25 C47 -179.8(6) . . . . ? C25 C24 C23 C48 0.3(11) . . . . ? C22 C24 C23 C48 -178.2(7) . . . . ? C27 C26 C28 C49 -1.7(13) . . . . ? C21 C26 C28 C49 173.6(7) . . . . ? C28 C26 C27 C61 -3(2) . . . . ? C21 C26 C27 C61 -177.9(14) . . . . ? C31 C30 C29 C33 -0.7(9) . . . . ? C31 C30 C29 C6 179.8(6) . . . . ? C46 C6 C29 C30 -103.6(7) . . . . ? N5 C6 C29 C30 76.7(7) . . . . ? C46 C6 C29 C33 77.0(9) . . . . ? N5 C6 C29 C33 -102.8(7) . . . . ? C29 C30 C31 C32 1.3(10) . . . . ? C30 C29 C33 C39 0.1(12) . . . . ? C6 C29 C33 C39 179.6(8) . . . . ? C30 C31 C32 C39 -1.3(13) . . . . ? C38 C37 C34 C35 -1.5(9) . . . . ? C38 C37 C34 C46 176.4(6) . . . . ? C37 C34 C35 C36 0.8(10) . . . . ? C46 C34 C35 C36 -177.1(7) . . . . ? C34 C37 C38 C43 0.3(10) . . . . ? C34 C35 C36 C43 1.1(12) . . . . ? C31 C32 C39 C33 0.7(16) . . . . ? C29 C33 C39 C32 -0.1(15) . . . . ? N1 C1 N2 C44 0.6(6) . . . . ? Ag1 C1 N2 C44 167.5(4) . . . . ? N1 C1 N2 C9 175.0(5) . . . . ? Ag1 C1 N2 C9 -18.1(7) . . . . ? C40 C44 N2 C1 -1.0(7) . . . . ? C13 C44 N2 C1 178.3(5) . . . . ? C40 C44 N2 C9 -175.3(5) . . . . ? C13 C44 N2 C9 4.0(9) . . . . ? C7 C9 N2 C1 99.0(6) . . . . ? C7 C9 N2 C44 -87.3(6) . . . . ? C21 C22 N3 C2 -1.0(6) . . . . ? C24 C22 N3 C2 -179.4(6) . . . . ? C21 C22 N3 C7 -175.6(5) . . . 2_556 ? C24 C22 N3 C7 6.0(9) . . . 2_556 ? N2 C1 N1 C40 -0.1(7) . . . . ? Ag1 C1 N1 C40 -167.1(5) . . . . ? N2 C1 N1 C10 -164.3(7) . . . . ? Ag1 C1 N1 C10 28.7(10) . . . . ? C44 C40 N1 C1 -0.5(9) . . . . ? C19 C40 N1 C1 170.8(7) . . . . ? C19' C40 N1 C1 -156.9(9) . . . . ? C44 C40 N1 C10 164.6(7) . . . . ? C19 C40 N1 C10 -24.0(12) . . . . ? C19' C40 N1 C10 8.3(13) . . . . ? N8 C10 N1 C1 -47.0(11) . . . . ? N8 C10 N1 C40 150.0(7) . . . . ? N5 C3 N6 C46 -1.1(5) . . . . ? Ag1 C3 N6 C46 166.2(4) . . . . ? N5 C3 N6 C11 -180.0(4) . . . . ? Ag1 C3 N6 C11 -12.7(7) . . . . ? C12 C11 N6 C3 97.2(6) . . . . ? C12 C11 N6 C46 -81.5(6) . . . . ? N6 C3 N5 C6 0.6(5) . . . . ? Ag1 C3 N5 C6 -166.5(4) . . . . ? N6 C3 N5 C8 -172.8(5) . . . . ? Ag1 C3 N5 C8 20.1(7) . . . . ? C46 C6 N5 C3 0.1(6) . . . . ? C29 C6 N5 C3 179.9(5) . . . . ? C46 C6 N5 C8 173.9(5) . . . . ? C29 C6 N5 C8 -6.2(7) . . . . ? N7 C8 N5 C3 -32.2(7) 2_556 . . . ? N7 C8 N5 C6 154.9(5) 2_556 . . . ? C2 Ag2 C4 N9 66.2(15) . . . . ? Ag1 Ag2 C4 N9 92.8(5) . . . . ? C2 Ag2 C4 N8 -107.3(14) . . . . ? Ag1 Ag2 C4 N8 -80.7(5) . . . . ? C65 C64 C42 C41 120.8(9) . . . . ? C67 C64 C42 C41 -67.1(11) . . . . ? C65 C64 C42 N8 -71.2(13) . . . . ? C67 C64 C42 N8 100.8(15) . . . . ? C65 C64 C42 C64' -26.6(11) . . . . ? C67 C64 C42 C64' 145.4(17) . . . . ? C65' C64' C42 C41 112.8(14) . . . . ? C69' C64' C42 C41 -60.3(13) . . . . ? C65' C64' C42 N8 -51.7(9) . . . . ? C69' C64' C42 N8 135.2(7) . . . . ? C65' C64' C42 C64 160.2(16) . . . . ? C69' C64' C42 C64 -12.9(11) . . . . ? N8 C42 C41 N9 0.9(9) . . . . ? C64 C42 C41 N9 172.2(8) . . . . ? C64' C42 C41 N9 -164.1(11) . . . . ? N8 C42 C41 C45 167.2(7) . . . . ? C64 C42 C41 C45 -21.5(13) . . . . ? C64' C42 C41 C45 2.1(18) . . . . ? C50 C45 C41 C42 124.9(9) . . . . ? C53 C45 C41 C42 -56.0(10) . . . . ? C50 C45 C41 N9 -71.4(9) . . . . ? C53 C45 C41 N9 107.7(8) . . . . ? C35 C36 C43 C38 -2.3(13) . . . . ? C37 C38 C43 C36 1.6(12) . . . . ? C22 N3 C2 N7 0.2(6) . . . . ? C7 N3 C2 N7 174.9(4) 2_556 . . . ? C22 N3 C2 Ag2 -180.0(4) . . . . ? C7 N3 C2 Ag2 -5.3(7) 2_556 . . . ? C4 Ag2 C2 N3 115.7(13) . . . . ? Ag1 Ag2 C2 N3 90.9(5) . . . . ? C4 Ag2 C2 N7 -64.5(15) . . . . ? Ag1 Ag2 C2 N7 -89.3(4) . . . . ? N8 C4 N9 C41 0.0(7) . . . . ? Ag2 C4 N9 C41 -174.6(5) . . . . ? N8 C4 N9 C12 -178.4(5) . . . . ? Ag2 C4 N9 C12 7.0(8) . . . . ? C42 C41 N9 C4 -0.6(8) . . . . ? C45 C41 N9 C4 -167.1(7) . . . . ? C42 C41 N9 C12 177.7(6) . . . . ? C45 C41 N9 C12 11.2(11) . . . . ? C11 C12 N9 C4 -58.0(7) . . . . ? C11 C12 N9 C41 123.9(6) . . . . ? N5 C6 C46 N6 -0.7(5) . . . . ? C29 C6 C46 N6 179.5(5) . . . . ? N5 C6 C46 C34 176.7(5) . . . . ? C29 C6 C46 C34 -3.1(10) . . . . ? C3 N6 C46 C6 1.2(6) . . . . ? C11 N6 C46 C6 -179.9(4) . . . . ? C3 N6 C46 C34 -176.5(5) . . . . ? C11 N6 C46 C34 2.4(7) . . . . ? C35 C34 C46 C6 -58.0(9) . . . . ? C37 C34 C46 C6 124.1(6) . . . . ? C35 C34 C46 N6 119.0(6) . . . . ? C37 C34 C46 N6 -58.8(8) . . . . ? N9 C4 N8 C42 0.6(7) . . . . ? Ag2 C4 N8 C42 175.4(5) . . . . ? N9 C4 N8 C10 179.8(6) . . . . ? Ag2 C4 N8 C10 -5.4(8) . . . . ? C41 C42 N8 C4 -1.0(9) . . . . ? C64 C42 N8 C4 -169.7(11) . . . . ? C64' C42 N8 C4 168.4(6) . . . . ? C41 C42 N8 C10 179.8(7) . . . . ? C64 C42 N8 C10 11.1(16) . . . . ? C64' C42 N8 C10 -10.7(11) . . . . ? N1 C10 N8 C4 93.8(8) . . . . ? N1 C10 N8 C42 -87.1(8) . . . . ? N3 C2 N7 C21 0.7(6) . . . . ? Ag2 C2 N7 C21 -179.2(4) . . . . ? N3 C2 N7 C8 176.0(5) . . . 2_556 ? Ag2 C2 N7 C8 -3.8(7) . . . 2_556 ? C22 C21 N7 C2 -1.3(6) . . . . ? C26 C21 N7 C2 173.4(6) . . . . ? C22 C21 N7 C8 -176.6(5) . . . 2_556 ? C26 C21 N7 C8 -1.9(9) . . . 2_556 ? C24 C25 C47 C52 -2.1(13) . . . . ? C26 C28 C49 C62 4.1(14) . . . . ? C24 C23 C48 C52 -2.0(13) . . . . ? C25 C47 C52 C48 0.5(14) . . . . ? C23 C48 C52 C47 1.6(14) . . . . ? O1 S1 C60 F1 60(2) . . . . ? O2 S1 C60 F1 -172.7(18) . . . . ? O3 S1 C60 F1 -58(2) . . . . ? O1 S1 C60 F3 175.9(11) . . . . ? O2 S1 C60 F3 -56.7(13) . . . . ? O3 S1 C60 F3 57.6(12) . . . . ? O1 S1 C60 F2 -60.2(11) . . . . ? O2 S1 C60 F2 67.1(12) . . . . ? O3 S1 C60 F2 -178.6(10) . . . . ? C26 C27 C61 C62 5(3) . . . . ? C27 C61 C62 C49 -2(2) . . . . ? C28 C49 C62 C61 -2.2(19) . . . . ? F12 C8A S2 O21 -34.9(17) . . . . ? F13 C8A S2 O21 -172.1(12) . . . . ? F14 C8A S2 O21 89.5(12) . . . . ? F12 C8A S2 O22 -170.3(16) . . . . ? F13 C8A S2 O22 52.5(11) . . . . ? F14 C8A S2 O22 -45.9(11) . . . . ? F12 C8A S2 O23 93.9(16) . . . . ? F13 C8A S2 O23 -43.2(10) . . . . ? F14 C8A S2 O23 -141.7(11) . . . . ? O22' S2' C8A' F13' -62.0(18) . . . . ? O21' S2' C8A' F13' 168.9(15) . . . . ? O23' S2' C8A' F13' 77.6(16) . . . . ? O22' S2' C8A' F14' 53.6(18) . . . . ? O21' S2' C8A' F14' -75.5(16) . . . . ? O23' S2' C8A' F14' -166.8(15) . . . . ? O22' S2' C8A' F12' 174.9(17) . . . . ? O21' S2' C8A' F12' 45.7(18) . . . . ? O23' S2' C8A' F12' -45.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.951 _refine_diff_density_min -1.952 _refine_diff_density_rms 0.165 # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 347.4 68.8 2 0.500 0.000 1.000 347.3 68.8 3 0.250 0.165 0.250 182.2 22.5 4 0.750 -0.165 0.750 182.3 23.3 5 0.750 0.316 0.750 18.9 -0.2 6 0.213 0.433 0.489 46.5 12.8 7 0.287 0.433 0.011 46.4 13.9 8 0.787 0.567 0.511 46.3 14.2 9 0.713 0.567 -0.011 46.4 12.3 10 0.250 0.684 0.250 19.0 0.0 _platon_squeeze_details ; ? ; data_3b _database_code_depnum_ccdc_archive 'CCDC 882739' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H104 Ag4 F24 N16 P4' _chemical_formula_weight 2925.67 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.122(2) _cell_length_b 17.707(3) _cell_length_c 32.571(5) _cell_angle_alpha 93.111(2) _cell_angle_beta 97.694(2) _cell_angle_gamma 109.952(2) _cell_volume 7542.9(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8841 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'bruker apex II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 85528 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.54 _reflns_number_total 33835 _reflns_number_gt 24139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure contains a large number of disordered water and acetone molecules that had no visible interactions with the silver compound and thus they were squeezed out for simplification. ; _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^)+(0.0650P)^2^+0.5283P] 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 33835 _refine_ls_number_parameters 1622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Ag3 Ag 0.619294(17) 0.227428(13) 0.242354(7) 0.01380(6) Uani 1 1 d . A 1 Ag1 Ag 0.855554(17) 0.210077(13) 0.244097(7) 0.01352(6) Uani 1 1 d . A 1 Ag2 Ag 0.836873(17) 0.382224(14) 0.243788(7) 0.01356(6) Uani 1 1 d . A 1 Ag4 Ag 1.069106(17) 0.362692(13) 0.244467(7) 0.01434(6) Uani 1 1 d . A 1 C85 C 0.7174(2) 0.37084(19) 0.06836(10) 0.0177(7) Uani 1 1 d . A 1 C19 C 0.8412(2) 0.15584(19) 0.06801(10) 0.0170(6) Uani 1 1 d . A 1 C62 C 1.1338(3) 0.0316(2) 0.18047(11) 0.0232(7) Uani 1 1 d . A 1 H62 H 1.1874 0.0522 0.2036 0.028 Uiso 1 1 calc R A 1 C88 C 0.5988(3) 0.3177(2) -0.01049(11) 0.0262(8) Uani 1 1 d . A 1 H88 H 0.5580 0.2979 -0.0371 0.031 Uiso 1 1 calc R A 1 C61 C 1.0523(2) 0.05962(19) 0.17627(10) 0.0179(7) Uani 1 1 d . A 1 C65 C 0.9780(3) -0.0287(2) 0.11233(11) 0.0265(8) Uani 1 1 d . A 1 H65 H 0.9249 -0.0493 0.0890 0.032 Uiso 1 1 calc R A 1 C64 C 1.0591(3) -0.0563(2) 0.11696(11) 0.0308(9) Uani 1 1 d . A 1 H64 H 1.0616 -0.0960 0.0967 0.037 Uiso 1 1 calc R A 1 C89 C 0.6992(3) 0.3219(2) -0.00366(11) 0.0281(8) Uani 1 1 d . A 1 H89 H 0.7284 0.3071 -0.0260 0.034 Uiso 1 1 calc R A 1 C86 C 0.6174(3) 0.3700(2) 0.06090(11) 0.0279(8) Uani 1 1 d . A 1 H86 H 0.5895 0.3884 0.0827 0.034 Uiso 1 1 calc R A 1 C66 C 0.9745(2) 0.02957(19) 0.14207(10) 0.0201(7) Uani 1 1 d . A 1 H66 H 0.9191 0.0488 0.1390 0.024 Uiso 1 1 calc R A 1 C24 C 0.7700(3) 0.1575(2) 0.03417(10) 0.0239(7) Uani 1 1 d . A 1 H24 H 0.7024 0.1514 0.0381 0.029 Uiso 1 1 calc R A 1 C22 C 0.8948(3) 0.1792(2) -0.01111(10) 0.0251(8) Uani 1 1 d . A 1 H22 H 0.9137 0.1887 -0.0378 0.030 Uiso 1 1 calc R A 1 C87 C 0.5583(3) 0.3426(3) 0.02177(11) 0.0325(9) Uani 1 1 d . A 1 H87 H 0.4898 0.3410 0.0172 0.039 Uiso 1 1 calc R A 1 C20 C 0.9382(3) 0.1642(2) 0.06080(11) 0.0294(8) Uani 1 1 d . A 1 H20 H 0.9873 0.1613 0.0831 0.035 Uiso 1 1 calc R A 1 C91 C 0.7577(3) 0.3475(2) 0.03558(10) 0.0249(8) Uani 1 1 d . A 1 H91 H 0.8262 0.3490 0.0400 0.030 Uiso 1 1 calc R A 1 C23 C 0.7972(3) 0.1679(2) -0.00497(11) 0.0288(8) Uani 1 1 d . A 1 H23 H 0.7474 0.1671 -0.0279 0.035 Uiso 1 1 calc R A 1 C63 C 1.1361(3) -0.0265(2) 0.15084(11) 0.0281(8) Uani 1 1 d . A 1 H63 H 1.1913 -0.0460 0.1538 0.034 Uiso 1 1 calc R A 1 C21 C 0.9655(3) 0.1767(3) 0.02188(11) 0.0325(9) Uani 1 1 d . A 1 H21 H 1.0332 0.1836 0.0178 0.039 Uiso 1 1 calc R A 1 C92 C 0.9394(2) 0.50754(19) 0.09193(9) 0.0172(6) Uani 1 1 d . A 1 C97 C 1.0301(3) 0.5013(2) 0.08277(10) 0.0217(7) Uani 1 1 d . A 1 H97 H 1.0560 0.4637 0.0954 0.026 Uiso 1 1 calc R A 1 C93 C 0.9026(3) 0.5633(2) 0.07351(11) 0.0259(8) Uani 1 1 d . A 1 H93 H 0.8411 0.5683 0.0798 0.031 Uiso 1 1 calc R A 1 C95 C 1.0448(3) 0.6049(2) 0.03690(11) 0.0264(8) Uani 1 1 d . A 1 H95 H 1.0809 0.6380 0.0180 0.032 Uiso 1 1 calc R A 1 C94 C 0.9563(3) 0.6118(2) 0.04587(12) 0.0287(8) Uani 1 1 d . A 1 H94 H 0.9311 0.6497 0.0332 0.034 Uiso 1 1 calc R A 1 C96 C 1.0825(3) 0.5498(2) 0.05536(11) 0.0263(8) Uani 1 1 d . A 1 H96 H 1.1444 0.5455 0.0491 0.032 Uiso 1 1 calc R A 1 C128 C 1.0028(2) 0.65748(19) 0.22413(10) 0.0167(6) Uani 1 1 d . A 1 C133 C 0.9159(3) 0.6384(2) 0.19392(10) 0.0212(7) Uani 1 1 d . A 1 H133 H 0.8697 0.5843 0.1880 0.025 Uiso 1 1 calc R A 1 C129 C 1.0691(3) 0.7372(2) 0.23277(11) 0.0225(7) Uani 1 1 d . A 1 H129 H 1.1284 0.7502 0.2533 0.027 Uiso 1 1 calc R A 1 C132 C 0.8971(3) 0.6993(2) 0.17253(11) 0.0272(8) Uani 1 1 d . A 1 H132 H 0.8381 0.6863 0.1519 0.033 Uiso 1 1 calc R A 1 C131 C 0.9641(3) 0.7788(2) 0.18117(12) 0.0291(8) Uani 1 1 d . A 1 H131 H 0.9515 0.8200 0.1663 0.035 Uiso 1 1 calc R A 1 C130 C 1.0502(3) 0.7975(2) 0.21192(12) 0.0286(8) Uani 1 1 d . A 1 H130 H 1.0956 0.8518 0.2184 0.034 Uiso 1 1 calc R A 1 C98 C 0.5876(2) 0.50660(18) 0.17633(10) 0.0172(6) Uani 1 1 d . A 1 C103 C 0.5073(3) 0.5348(2) 0.17913(11) 0.0218(7) Uani 1 1 d . A 1 H103 H 0.4680 0.5209 0.2009 0.026 Uiso 1 1 calc R A 1 C101 C 0.5420(3) 0.6034(2) 0.11825(11) 0.0278(8) Uani 1 1 d . A 1 H101 H 0.5269 0.6370 0.0985 0.033 Uiso 1 1 calc R A 1 C99 C 0.6443(2) 0.52709(19) 0.14410(10) 0.0199(7) Uani 1 1 d . A 1 H99 H 0.6991 0.5082 0.1421 0.024 Uiso 1 1 calc R A 1 C100 C 0.6210(3) 0.5751(2) 0.11495(10) 0.0251(8) Uani 1 1 d . A 1 H100 H 0.6592 0.5884 0.0928 0.030 Uiso 1 1 calc R A 1 C102 C 0.4853(3) 0.5834(2) 0.14975(11) 0.0269(8) Uani 1 1 d . A 1 H102 H 0.4308 0.6028 0.1516 0.032 Uiso 1 1 calc R A 1 C120 C 1.0960(3) 0.4683(2) 0.47230(11) 0.0247(7) Uani 1 1 d . A 1 H120 H 1.1217 0.4340 0.4882 0.030 Uiso 1 1 calc R A 1 C116 C 0.9816(2) 0.48586(19) 0.41492(10) 0.0171(6) Uani 1 1 d . A 1 C121 C 1.0203(2) 0.4356(2) 0.43817(10) 0.0204(7) Uani 1 1 d . A 1 H121 H 0.9945 0.3789 0.4304 0.024 Uiso 1 1 calc R A 1 C119 C 1.1346(3) 0.5511(2) 0.48350(11) 0.0310(8) Uani 1 1 d . A 1 H119 H 1.1875 0.5735 0.5068 0.037 Uiso 1 1 calc R A 1 C117 C 1.0198(3) 0.5687(2) 0.42665(10) 0.0224(7) Uani 1 1 d . A 1 H117 H 0.9934 0.6031 0.4112 0.027 Uiso 1 1 calc R A 1 C118 C 1.0963(3) 0.6012(2) 0.46091(11) 0.0286(8) Uani 1 1 d . A 1 H118 H 1.1224 0.6578 0.4688 0.034 Uiso 1 1 calc R A 1 C40 C 0.7262(3) -0.1106(2) 0.38779(11) 0.0238(7) Uani 1 1 d . A 1 H40 H 0.7361 -0.1403 0.4104 0.029 Uiso 1 1 calc R A 1 C39 C 0.6352(3) -0.0965(2) 0.37893(11) 0.0231(7) Uani 1 1 d . A 1 H39 H 0.5833 -0.1161 0.3955 0.028 Uiso 1 1 calc R A 1 C38 C 0.6202(3) -0.0534(2) 0.34572(10) 0.0210(7) Uani 1 1 d . A 1 H38 H 0.5575 -0.0445 0.3393 0.025 Uiso 1 1 calc R A 1 C37 C 0.6969(2) -0.02335(18) 0.32184(10) 0.0163(6) Uani 1 1 d . A 1 C41 C 0.8019(3) -0.0823(2) 0.36420(11) 0.0239(7) Uani 1 1 d . A 1 H41 H 0.8638 -0.0925 0.3703 0.029 Uiso 1 1 calc R A 1 C42 C 0.7871(3) -0.0382(2) 0.33108(10) 0.0218(7) Uani 1 1 d . A 1 H42 H 0.8396 -0.0182 0.3148 0.026 Uiso 1 1 calc R A 1 C110 C 0.7506(2) 0.48933(19) 0.39588(9) 0.0161(6) Uani 1 1 d . A 1 C115 C 0.6943(3) 0.4429(2) 0.42327(10) 0.0231(7) Uani 1 1 d . A 1 H115 H 0.6900 0.3884 0.4244 0.028 Uiso 1 1 calc R A 1 C111 C 0.7547(3) 0.5689(2) 0.39451(12) 0.0281(8) Uani 1 1 d . A 1 H111 H 0.7932 0.6014 0.3760 0.034 Uiso 1 1 calc R A 1 C113 C 0.6486(3) 0.5548(2) 0.44703(11) 0.0292(8) Uani 1 1 d . A 1 H113 H 0.6138 0.5770 0.4645 0.035 Uiso 1 1 calc R A 1 C114 C 0.6441(3) 0.4757(2) 0.44896(11) 0.0281(8) Uani 1 1 d . A 1 H114 H 0.6066 0.4438 0.4679 0.034 Uiso 1 1 calc R A 1 C30 C 0.5380(3) 0.0321(2) 0.08206(11) 0.0234(7) Uani 1 1 d . A 1 H30 H 0.5235 0.0758 0.0947 0.028 Uiso 1 1 calc R A 1 C25 C 0.6355(2) 0.02833(19) 0.09077(10) 0.0178(7) Uani 1 1 d . A 1 C29 C 0.4623(3) -0.0277(2) 0.05500(12) 0.0299(8) Uani 1 1 d . A 1 H29 H 0.3961 -0.0246 0.0487 0.036 Uiso 1 1 calc R A 1 C26 C 0.6559(3) -0.0362(2) 0.07264(11) 0.0238(7) Uani 1 1 d . A 1 H26 H 0.7222 -0.0391 0.0785 0.029 Uiso 1 1 calc R A 1 C27 C 0.5789(3) -0.0965(2) 0.04588(12) 0.0284(8) Uani 1 1 d . A 1 H27 H 0.5925 -0.1409 0.0337 0.034 Uiso 1 1 calc R A 1 C28 C 0.4825(3) -0.0920(2) 0.03704(11) 0.0266(8) Uani 1 1 d . A 1 H28 H 0.4301 -0.1330 0.0186 0.032 Uiso 1 1 calc R A 1 C104 C 0.6440(2) 0.55279(19) 0.27541(10) 0.0169(6) Uani 1 1 d . A 1 C105 C 0.7216(3) 0.6239(2) 0.27040(11) 0.0240(7) Uani 1 1 d . A 1 H105 H 0.7680 0.6231 0.2519 0.029 Uiso 1 1 calc R A 1 C109 C 0.5750(3) 0.5551(2) 0.30170(11) 0.0225(7) Uani 1 1 d . A 1 H109 H 0.5212 0.5070 0.3048 0.027 Uiso 1 1 calc R A 1 C108 C 0.5847(3) 0.6279(2) 0.32347(12) 0.0279(8) Uani 1 1 d . A 1 H108 H 0.5374 0.6294 0.3414 0.033 Uiso 1 1 calc R A 1 C107 C 0.6627(3) 0.6981(2) 0.31899(12) 0.0329(9) Uani 1 1 d . A 1 H107 H 0.6696 0.7477 0.3340 0.040 Uiso 1 1 calc R A 1 C106 C 0.7306(3) 0.6961(2) 0.29269(12) 0.0306(8) Uani 1 1 d . A 1 H106 H 0.7842 0.7444 0.2897 0.037 Uiso 1 1 calc R A 1 C122 C 1.0650(2) 0.64949(19) 0.32355(10) 0.0185(7) Uani 1 1 d . A 1 C127 C 1.1569(3) 0.6810(2) 0.35124(10) 0.0235(7) Uani 1 1 d . A 1 H127 H 1.2121 0.6635 0.3476 0.028 Uiso 1 1 calc R A 1 C126 C 1.1675(3) 0.7384(2) 0.38429(11) 0.0289(8) Uani 1 1 d . A 1 H126 H 1.2296 0.7591 0.4035 0.035 Uiso 1 1 calc R A 1 C123 C 0.9858(3) 0.67585(19) 0.32932(10) 0.0212(7) Uani 1 1 d . A 1 H123 H 0.9229 0.6542 0.3107 0.025 Uiso 1 1 calc R A 1 C125 C 1.0885(3) 0.7652(2) 0.38918(11) 0.0291(8) Uani 1 1 d . A 1 H125 H 1.0968 0.8054 0.4113 0.035 Uiso 1 1 calc R A 1 C124 C 0.9966(3) 0.7334(2) 0.36185(11) 0.0259(8) Uani 1 1 d . A 1 H124 H 0.9415 0.7510 0.3655 0.031 Uiso 1 1 calc R A 1 C32 C 0.7477(2) -0.0608(2) 0.19088(10) 0.0207(7) Uani 1 1 d . A 1 H32 H 0.7854 -0.0085 0.1843 0.025 Uiso 1 1 calc R A 1 C36 C 0.6355(3) -0.1452(2) 0.23251(11) 0.0236(7) Uani 1 1 d . A 1 H36 H 0.5952 -0.1514 0.2541 0.028 Uiso 1 1 calc R A 1 C31 C 0.6887(2) -0.06834(19) 0.22220(10) 0.0172(6) Uani 1 1 d . A 1 C34 C 0.7002(3) -0.2045(2) 0.17934(12) 0.0311(9) Uani 1 1 d . A 1 H34 H 0.7043 -0.2510 0.1647 0.037 Uiso 1 1 calc R A 1 C33 C 0.7523(3) -0.1282(2) 0.16917(11) 0.0274(8) Uani 1 1 d . A 1 H33 H 0.7914 -0.1222 0.1472 0.033 Uiso 1 1 calc R A 1 C35 C 0.6423(3) -0.2127(2) 0.21085(12) 0.0292(8) Uani 1 1 d . A 1 H35 H 0.6065 -0.2651 0.2179 0.035 Uiso 1 1 calc R A 1 C43 C 0.8397(2) 0.17833(19) 0.41544(10) 0.0177(7) Uani 1 1 d . A 1 C45 C 0.7527(3) 0.2181(2) 0.46673(11) 0.0293(8) Uani 1 1 d . A 1 H45 H 0.7290 0.2570 0.4788 0.035 Uiso 1 1 calc R A 1 C48 C 0.8204(3) 0.1041(2) 0.43120(11) 0.0251(8) Uani 1 1 d . A 1 H48 H 0.8429 0.0646 0.4190 0.030 Uiso 1 1 calc R A 1 C44 C 0.8060(2) 0.2357(2) 0.43388(10) 0.0229(7) Uani 1 1 d . A 1 H44 H 0.8199 0.2870 0.4237 0.027 Uiso 1 1 calc R A 1 C46 C 0.7334(3) 0.1436(3) 0.48215(11) 0.0334(9) Uani 1 1 d . A 1 H46 H 0.6963 0.1312 0.5046 0.040 Uiso 1 1 calc R A 1 C47 C 0.7686(3) 0.0877(2) 0.46463(11) 0.0323(9) Uani 1 1 d . A 1 H47 H 0.7571 0.0373 0.4757 0.039 Uiso 1 1 calc R A 1 C112 C 0.7034(3) 0.6013(2) 0.41979(12) 0.0315(9) Uani 1 1 d . A 1 H112 H 0.7061 0.6554 0.4183 0.038 Uiso 1 1 calc R A 1 C55 C 1.0668(2) 0.04954(19) 0.27453(10) 0.0168(6) Uani 1 1 d . A 1 C60 C 0.9860(3) -0.0239(2) 0.26814(11) 0.0243(7) Uani 1 1 d . A 1 H60 H 0.9249 -0.0300 0.2499 0.029 Uiso 1 1 calc R A 1 C59 C 0.9954(3) -0.0887(2) 0.28881(13) 0.0346(9) Uani 1 1 d . A 1 H59 H 0.9402 -0.1389 0.2846 0.042 Uiso 1 1 calc R A 1 C57 C 1.1643(3) -0.0077(2) 0.32126(13) 0.0331(9) Uani 1 1 d . A 1 H57 H 1.2253 -0.0023 0.3394 0.040 Uiso 1 1 calc R A 1 C58 C 1.0828(3) -0.0807(2) 0.31483(13) 0.0347(9) Uani 1 1 d . A 1 H58 H 1.0882 -0.1253 0.3287 0.042 Uiso 1 1 calc R A 1 C56 C 1.1560(3) 0.0567(2) 0.30117(11) 0.0275(8) Uani 1 1 d . A 1 H56 H 1.2117 0.1066 0.3055 0.033 Uiso 1 1 calc R A 1 C13 C 1.0602(2) 0.11646(18) 0.25074(10) 0.0158(6) Uani 1 1 d . A 1 C14 C 1.0511(2) 0.12022(18) 0.20878(10) 0.0157(6) Uani 1 1 d . A 1 C4 C 1.0648(2) 0.24328(18) 0.23874(10) 0.0150(6) Uani 1 1 d . A 1 N8 N 1.05429(19) 0.19834(15) 0.20295(8) 0.0150(5) Uani 1 1 d . A 1 N7 N 1.06839(18) 0.19300(15) 0.26843(8) 0.0130(5) Uani 1 1 d . A 1 N6 N 0.98450(19) 0.20016(15) 0.32873(8) 0.0138(5) Uani 1 1 d . A 1 N5 N 0.84391(19) 0.20924(15) 0.34060(8) 0.0144(5) Uani 1 1 d . A 1 C3 C 0.9012(2) 0.21342(18) 0.30986(10) 0.0149(6) Uani 1 1 d . A 1 C11 C 0.9808(2) 0.18770(19) 0.37069(9) 0.0165(6) Uani 1 1 d . A 1 C49 C 1.0617(2) 0.1702(2) 0.39818(10) 0.0193(7) Uani 1 1 d . A 1 C10 C 0.8910(2) 0.19293(19) 0.37820(9) 0.0164(6) Uani 1 1 d . A 1 C54 C 1.0677(3) 0.0934(2) 0.39499(11) 0.0270(8) Uani 1 1 d . A 1 H54 H 1.0193 0.0519 0.3754 0.032 Uiso 1 1 calc R A 1 C50 C 1.1330(3) 0.2306(2) 0.42668(11) 0.0268(8) Uani 1 1 d . A 1 H50 H 1.1309 0.2837 0.4287 0.032 Uiso 1 1 calc R A 1 C51 C 1.2078(3) 0.2123(3) 0.45227(12) 0.0362(9) Uani 1 1 d . A 1 H51 H 1.2558 0.2531 0.4723 0.043 Uiso 1 1 calc R A 1 C53 C 1.1441(3) 0.0771(2) 0.42033(12) 0.0317(9) Uani 1 1 d . A 1 H53 H 1.1484 0.0247 0.4177 0.038 Uiso 1 1 calc R A 1 C52 C 1.2135(3) 0.1364(3) 0.44915(12) 0.0343(9) Uani 1 1 d . A 1 H52 H 1.2650 0.1249 0.4668 0.041 Uiso 1 1 calc R A 1 C12 C 1.0826(2) 0.21839(19) 0.31252(9) 0.0158(6) Uani 1 1 d . A 1 H12A H 1.1209 0.2773 0.3176 0.019 Uiso 1 1 calc R A 1 H12B H 1.1242 0.1909 0.3280 0.019 Uiso 1 1 calc R A 1 C16 C 0.9600(2) 0.25647(18) 0.15097(10) 0.0161(6) Uani 1 1 d . A 1 H16A H 0.9620 0.2990 0.1724 0.019 Uiso 1 1 calc R A 1 H16B H 0.9653 0.2804 0.1242 0.019 Uiso 1 1 calc R A 1 C15 C 1.0523(2) 0.23198(19) 0.16268(9) 0.0160(6) Uani 1 1 d . A 1 H15A H 1.0525 0.1912 0.1407 0.019 Uiso 1 1 calc R A 1 H15B H 1.1151 0.2798 0.1639 0.019 Uiso 1 1 calc R A 1 C17 C 0.8079(2) 0.14431(19) 0.10903(10) 0.0162(6) Uani 1 1 d . A 1 C18 C 0.7193(2) 0.09237(19) 0.11814(9) 0.0153(6) Uani 1 1 d . A 1 C1 C 0.8081(2) 0.16998(18) 0.17889(10) 0.0148(6) Uani 1 1 d . A 1 N2 N 0.72110(19) 0.10901(15) 0.16078(8) 0.0146(5) Uani 1 1 d . A 1 N1 N 0.86140(19) 0.19083(15) 0.14679(8) 0.0144(5) Uani 1 1 d . A 1 C5 C 0.6326(2) 0.06548(19) 0.18051(10) 0.0168(6) Uani 1 1 d . A 1 H5A H 0.5805 0.0912 0.1752 0.020 Uiso 1 1 calc R A 1 H5B H 0.6020 0.0091 0.1671 0.020 Uiso 1 1 calc R A 1 C84 C 0.7827(2) 0.39860(19) 0.10968(9) 0.0162(6) Uani 1 1 d . A 1 C83 C 0.8785(2) 0.45417(18) 0.11922(9) 0.0145(6) Uani 1 1 d . A 1 C67 C 0.8370(2) 0.39929(18) 0.17935(9) 0.0146(6) Uani 1 1 d . A 1 N10 N 0.75803(19) 0.36597(15) 0.14689(8) 0.0147(5) Uani 1 1 d . A 1 N9 N 0.90993(19) 0.45384(15) 0.16190(8) 0.0150(5) Uani 1 1 d . A 1 C74 C 0.6327(2) 0.47670(19) 0.25077(10) 0.0159(6) Uani 1 1 d . A 1 C73 C 0.6115(2) 0.45783(18) 0.20874(10) 0.0152(6) Uani 1 1 d . A 1 C68 C 0.6218(2) 0.34554(18) 0.23749(10) 0.0154(6) Uani 1 1 d . A 1 N12 N 0.63899(19) 0.40717(15) 0.26750(8) 0.0153(5) Uani 1 1 d . A 1 N11 N 0.60567(19) 0.37770(15) 0.20148(8) 0.0139(5) Uani 1 1 d . A 1 C71 C 0.6635(2) 0.30089(18) 0.15015(10) 0.0157(6) Uani 1 1 d . A 1 H71A H 0.6782 0.2675 0.1718 0.019 Uiso 1 1 calc R A 1 H71B H 0.6390 0.2660 0.1233 0.019 Uiso 1 1 calc R A 1 C72 C 0.5783(2) 0.32925(19) 0.16085(9) 0.0154(6) Uani 1 1 d . A 1 H72A H 0.5623 0.3618 0.1390 0.018 Uiso 1 1 calc R A 1 H72B H 0.5161 0.2815 0.1610 0.018 Uiso 1 1 calc R A 1 C75 C 0.6598(2) 0.39913(19) 0.31125(9) 0.0154(6) Uani 1 1 d . A 1 H75A H 0.6264 0.3420 0.3159 0.018 Uiso 1 1 calc R A 1 H75B H 0.6296 0.4320 0.3270 0.018 Uiso 1 1 calc R A 1 P2 P 0.36482(7) 0.93800(6) 0.24942(3) 0.0256(2) Uani 1 1 d . B 1 P3 P 0.35900(7) 0.29692(6) 0.27768(3) 0.0294(2) Uani 1 1 d . C 1 F13 F 0.28662(16) 0.34971(13) 0.27996(8) 0.0374(5) Uani 1 1 d . C 1 F18 F 0.27464(16) 0.23382(14) 0.24226(7) 0.0402(6) Uani 1 1 d . C 1 F17 F 0.30605(16) 0.24643(13) 0.31274(7) 0.0360(5) Uani 1 1 d . C 1 F15 F 0.44290(16) 0.36058(13) 0.31249(7) 0.0371(5) Uani 1 1 d . C 1 F14 F 0.40934(16) 0.34893(15) 0.24212(8) 0.0422(6) Uani 1 1 d . C 1 C77 C 0.9027(2) 0.45420(18) 0.37716(9) 0.0149(6) Uani 1 1 d . A 1 C76 C 0.8070(2) 0.45642(18) 0.36907(9) 0.0156(6) Uani 1 1 d . A 1 C69 C 0.8397(2) 0.40414(18) 0.30927(10) 0.0151(6) Uani 1 1 d . A 1 N13 N 0.77004(19) 0.42475(15) 0.32762(8) 0.0134(5) Uani 1 1 d . A 1 N14 N 0.92120(19) 0.42210(15) 0.34051(8) 0.0141(5) Uani 1 1 d . A 1 C78 C 1.0166(2) 0.41043(18) 0.33601(10) 0.0151(6) Uani 1 1 d . A 1 H78A H 1.0042 0.3700 0.3118 0.018 Uiso 1 1 calc R A 1 H78B H 1.0398 0.3885 0.3612 0.018 Uiso 1 1 calc R A 1 C79 C 1.1006(2) 0.48799(19) 0.32993(9) 0.0159(6) Uani 1 1 d . A 1 H79A H 1.1122 0.5292 0.3537 0.019 Uiso 1 1 calc R A 1 H79B H 1.1649 0.4775 0.3293 0.019 Uiso 1 1 calc R A 1 N15 N 1.07244(19) 0.51874(15) 0.29081(8) 0.0140(5) Uani 1 1 d . A 1 C80 C 1.0527(2) 0.59029(18) 0.28735(10) 0.0158(6) Uani 1 1 d . A 1 C81 C 1.0250(2) 0.59335(18) 0.24634(9) 0.0140(6) Uani 1 1 d . A 1 C6 C 0.6789(2) 0.00293(18) 0.24437(10) 0.0156(6) Uani 1 1 d . A 1 C7 C 0.6806(2) 0.02053(18) 0.28598(9) 0.0138(6) Uani 1 1 d . A 1 C9 C 0.7446(2) 0.21824(18) 0.33535(10) 0.0161(6) Uani 1 1 d . A 1 H9A H 0.7386 0.2494 0.3114 0.019 Uiso 1 1 calc R A 1 H9B H 0.7392 0.2493 0.3606 0.019 Uiso 1 1 calc R A 1 C8 C 0.6564(2) 0.13661(18) 0.32793(10) 0.0160(6) Uani 1 1 d . A 1 H8A H 0.6624 0.1049 0.3516 0.019 Uiso 1 1 calc R A 1 H8B H 0.5906 0.1457 0.3263 0.019 Uiso 1 1 calc R A 1 F10 F 0.29789(17) 0.88481(14) 0.28008(7) 0.0424(6) Uani 1 1 d . B 1 F9 F 0.44356(19) 0.89220(16) 0.25791(9) 0.0505(7) Uani 1 1 d . B 1 F11 F 0.30159(18) 0.87224(16) 0.21114(8) 0.0522(7) Uani 1 1 d . B 1 F7 F 0.43376(19) 0.98983(16) 0.21851(8) 0.0527(7) Uani 1 1 d . B 1 F12 F 0.2872(2) 0.98390(17) 0.24140(9) 0.0565(7) Uani 1 1 d . B 1 F8 F 0.42925(17) 1.00434(13) 0.28764(7) 0.0378(5) Uani 1 1 d . B 1 F16 F 0.43144(16) 0.24473(14) 0.27620(8) 0.0406(6) Uani 1 1 d . C 1 N4 N 0.65759(19) 0.09136(15) 0.28940(8) 0.0132(5) Uani 1 1 d . A 1 N3 N 0.65660(19) 0.06397(15) 0.22470(8) 0.0137(5) Uani 1 1 d . A 1 N16 N 1.02802(19) 0.52279(15) 0.22608(8) 0.0149(5) Uani 1 1 d . A 1 C2 C 0.6433(2) 0.11871(19) 0.25225(9) 0.0166(6) Uani 1 1 d . A 1 C70 C 1.0585(2) 0.47638(18) 0.25346(9) 0.0142(6) Uani 1 1 d . A 1 C82 C 1.0151(2) 0.50278(19) 0.18137(9) 0.0159(6) Uani 1 1 d . A 1 H82A H 1.0606 0.4730 0.1757 0.019 Uiso 1 1 calc R A 1 H82B H 1.0370 0.5536 0.1681 0.019 Uiso 1 1 calc R A 1 P4 P 0.47568(9) 0.73215(7) 0.46342(4) 0.0399(3) Uani 1 1 d . D 1 F21 F 0.5247(3) 0.6735(2) 0.48551(10) 0.0828(11) Uani 1 1 d . D 1 F24 F 0.4273(3) 0.7909(2) 0.44177(12) 0.0960(13) Uani 1 1 d . D 1 F22 F 0.5840(3) 0.7961(3) 0.46529(17) 0.1375(19) Uani 1 1 d . D 1 F20 F 0.4856(5) 0.6975(3) 0.42106(11) 0.166(3) Uani 1 1 d . D 1 F19 F 0.3722(3) 0.6745(3) 0.4662(3) 0.240(5) Uani 1 1 d . D 1 F23 F 0.4783(5) 0.7759(3) 0.50715(13) 0.139(2) Uani 1 1 d . D 1 P1 P 0.23229(7) 0.24168(5) 0.95464(3) 0.02351(19) Uani 1 1 d . E 1 F1 F 0.21365(19) 0.23285(16) 0.90488(7) 0.0464(6) Uani 1 1 d . E 1 F2 F 0.23104(18) 0.15079(14) 0.95332(8) 0.0429(6) Uani 1 1 d . E 1 F4 F 0.11216(19) 0.20829(16) 0.95352(9) 0.0539(7) Uani 1 1 d . E 1 F3 F 0.35168(19) 0.27478(16) 0.95454(9) 0.0570(7) Uani 1 1 d . E 1 F6 F 0.2326(2) 0.33208(14) 0.95440(8) 0.0470(6) Uani 1 1 d . E 1 F5 F 0.2489(3) 0.25026(18) 1.00348(8) 0.0839(12) Uani 1 1 d . E 1 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 Ag3 0.01624(12) 0.01316(11) 0.01239(12) 0.00140(9) 0.00159(9) 0.00595(9) Ag1 0.01353(11) 0.01592(12) 0.01015(11) 0.00052(9) 0.00063(9) 0.00458(9) Ag2 0.01388(11) 0.01600(12) 0.00999(11) 0.00056(9) 0.00108(9) 0.00467(9) Ag4 0.01560(12) 0.01449(12) 0.01306(12) 0.00077(9) 0.00155(9) 0.00588(9) C85 0.0204(16) 0.0207(16) 0.0112(15) 0.0029(12) 0.0000(12) 0.0072(13) C19 0.0166(16) 0.0200(16) 0.0133(16) -0.0005(12) 0.0019(12) 0.0055(13) C62 0.0256(18) 0.0265(18) 0.0192(18) 0.0054(14) 0.0037(14) 0.0110(15) C88 0.0269(19) 0.032(2) 0.0122(17) 0.0025(14) -0.0067(14) 0.0045(16) C61 0.0214(17) 0.0156(15) 0.0158(16) 0.0004(12) 0.0046(13) 0.0049(13) C65 0.034(2) 0.0210(17) 0.0194(18) -0.0022(14) 0.0051(15) 0.0030(15) C64 0.052(2) 0.0218(18) 0.0183(18) -0.0011(14) 0.0123(17) 0.0108(17) C89 0.0290(19) 0.041(2) 0.0133(17) -0.0025(15) 0.0027(14) 0.0128(17) C86 0.0256(19) 0.045(2) 0.0145(17) 0.0037(16) 0.0012(14) 0.0153(17) C66 0.0189(16) 0.0195(16) 0.0182(17) 0.0015(13) 0.0029(13) 0.0023(13) C24 0.0196(17) 0.036(2) 0.0144(17) 0.0024(14) 0.0019(13) 0.0085(15) C22 0.033(2) 0.0303(19) 0.0110(16) -0.0016(14) 0.0060(14) 0.0089(16) C87 0.0199(18) 0.055(3) 0.0222(19) 0.0039(18) -0.0015(15) 0.0142(18) C20 0.0236(18) 0.050(2) 0.0164(18) 0.0028(16) 0.0036(14) 0.0158(17) C91 0.0196(17) 0.036(2) 0.0164(17) -0.0015(15) 0.0009(13) 0.0085(15) C23 0.032(2) 0.040(2) 0.0108(16) 0.0024(15) 0.0002(14) 0.0105(17) C63 0.037(2) 0.0273(19) 0.027(2) 0.0054(15) 0.0104(16) 0.0176(17) C21 0.0232(19) 0.055(3) 0.0202(19) -0.0003(17) 0.0092(15) 0.0130(18) C92 0.0187(16) 0.0209(16) 0.0095(15) 0.0015(12) -0.0005(12) 0.0047(13) C97 0.0231(17) 0.0234(17) 0.0186(17) 0.0047(14) 0.0048(14) 0.0073(14) C93 0.0231(18) 0.0305(19) 0.030(2) 0.0127(16) 0.0106(15) 0.0134(16) C95 0.0288(19) 0.0299(19) 0.0219(18) 0.0085(15) 0.0095(15) 0.0092(16) C94 0.0282(19) 0.035(2) 0.029(2) 0.0154(16) 0.0095(16) 0.0149(17) C96 0.0246(18) 0.0313(19) 0.028(2) 0.0061(16) 0.0121(15) 0.0124(16) C128 0.0172(16) 0.0187(16) 0.0148(16) 0.0029(12) 0.0038(12) 0.0064(13) C133 0.0239(18) 0.0217(17) 0.0196(17) 0.0018(13) 0.0021(14) 0.0106(14) C129 0.0225(17) 0.0206(17) 0.0240(18) 0.0045(14) 0.0036(14) 0.0067(14) C132 0.0270(19) 0.031(2) 0.0244(19) 0.0063(15) 0.0009(15) 0.0119(16) C131 0.034(2) 0.0258(19) 0.033(2) 0.0135(16) 0.0033(16) 0.0158(16) C130 0.0253(19) 0.0178(17) 0.043(2) 0.0068(16) 0.0055(17) 0.0080(15) C98 0.0180(16) 0.0130(15) 0.0171(16) 0.0013(12) -0.0004(13) 0.0022(13) C103 0.0212(17) 0.0243(17) 0.0199(17) -0.0013(14) 0.0001(14) 0.0099(14) C101 0.038(2) 0.0213(18) 0.0213(19) 0.0064(14) -0.0067(16) 0.0109(16) C99 0.0171(16) 0.0200(16) 0.0193(17) 0.0007(13) 0.0010(13) 0.0032(13) C100 0.031(2) 0.0235(18) 0.0147(17) 0.0067(14) 0.0015(14) 0.0021(15) C102 0.032(2) 0.0249(18) 0.029(2) 0.0011(15) -0.0024(16) 0.0194(16) C120 0.0235(18) 0.0323(19) 0.0187(18) 0.0074(15) -0.0001(14) 0.0110(15) C116 0.0173(16) 0.0204(16) 0.0124(15) 0.0004(12) 0.0014(12) 0.0057(13) C121 0.0226(17) 0.0236(17) 0.0148(16) 0.0038(13) 0.0022(13) 0.0081(14) C119 0.029(2) 0.041(2) 0.0165(18) -0.0026(16) -0.0062(15) 0.0090(17) C117 0.0265(18) 0.0227(17) 0.0163(17) -0.0007(13) -0.0036(14) 0.0097(15) C118 0.032(2) 0.0247(19) 0.0227(19) -0.0057(15) -0.0063(15) 0.0068(16) C40 0.035(2) 0.0192(17) 0.0170(17) 0.0025(13) -0.0004(14) 0.0101(15) C39 0.0258(18) 0.0202(17) 0.0216(18) 0.0038(14) 0.0072(14) 0.0043(14) C38 0.0228(17) 0.0230(17) 0.0180(17) 0.0060(13) 0.0035(14) 0.0083(14) C37 0.0216(16) 0.0118(14) 0.0125(15) -0.0002(12) -0.0013(12) 0.0037(13) C41 0.0265(18) 0.0222(17) 0.0238(19) 0.0026(14) -0.0031(14) 0.0121(15) C42 0.0221(17) 0.0211(17) 0.0200(17) 0.0017(14) 0.0028(14) 0.0055(14) C110 0.0133(15) 0.0219(16) 0.0120(15) -0.0028(12) -0.0024(12) 0.0071(13) C115 0.0266(18) 0.0261(18) 0.0171(17) 0.0015(14) 0.0046(14) 0.0096(15) C111 0.036(2) 0.0231(18) 0.028(2) 0.0027(15) 0.0086(16) 0.0127(16) C113 0.0268(19) 0.045(2) 0.0193(18) -0.0064(16) 0.0009(15) 0.0196(17) C114 0.030(2) 0.038(2) 0.0209(19) 0.0017(16) 0.0094(15) 0.0155(17) C30 0.0200(17) 0.0236(17) 0.0259(19) -0.0011(14) -0.0006(14) 0.0090(14) C25 0.0182(16) 0.0227(17) 0.0103(15) 0.0015(12) 0.0020(12) 0.0045(13) C29 0.0188(18) 0.032(2) 0.033(2) -0.0062(16) -0.0083(15) 0.0084(16) C26 0.0180(17) 0.0283(19) 0.0227(18) -0.0074(14) -0.0009(14) 0.0080(15) C27 0.0249(19) 0.030(2) 0.031(2) -0.0090(16) 0.0011(15) 0.0129(16) C28 0.0230(18) 0.0287(19) 0.0212(18) -0.0040(15) -0.0058(14) 0.0050(15) C104 0.0175(16) 0.0187(16) 0.0152(16) 0.0018(12) -0.0001(12) 0.0082(13) C105 0.0229(18) 0.0214(17) 0.0259(19) 0.0014(14) 0.0041(14) 0.0056(14) C109 0.0202(17) 0.0198(17) 0.0285(19) 0.0024(14) 0.0049(14) 0.0079(14) C108 0.031(2) 0.0241(18) 0.031(2) -0.0024(15) 0.0090(16) 0.0124(16) C107 0.041(2) 0.0221(19) 0.036(2) -0.0056(16) 0.0017(18) 0.0141(17) C106 0.030(2) 0.0150(17) 0.038(2) -0.0004(15) 0.0012(17) 0.0000(15) C122 0.0213(17) 0.0145(15) 0.0160(16) 0.0006(12) 0.0025(13) 0.0019(13) C127 0.0268(18) 0.0207(17) 0.0189(18) -0.0009(14) 0.0006(14) 0.0048(15) C126 0.037(2) 0.0227(18) 0.0161(18) -0.0021(14) -0.0004(15) -0.0004(16) C123 0.0275(18) 0.0189(16) 0.0161(17) 0.0013(13) 0.0033(14) 0.0071(14) C125 0.047(2) 0.0187(17) 0.0172(18) -0.0038(14) 0.0068(16) 0.0061(16) C124 0.038(2) 0.0216(17) 0.0225(18) 0.0046(14) 0.0118(16) 0.0132(16) C32 0.0196(17) 0.0185(16) 0.0235(18) 0.0038(13) 0.0052(14) 0.0053(14) C36 0.0255(18) 0.0205(17) 0.0274(19) 0.0038(14) 0.0070(15) 0.0101(15) C31 0.0132(15) 0.0167(15) 0.0204(17) 0.0012(13) 0.0001(12) 0.0047(12) C34 0.031(2) 0.0245(19) 0.040(2) -0.0099(16) 0.0052(17) 0.0136(16) C33 0.0274(19) 0.032(2) 0.0249(19) -0.0018(15) 0.0067(15) 0.0123(16) C35 0.030(2) 0.0200(18) 0.037(2) -0.0001(16) 0.0096(17) 0.0076(15) C43 0.0165(16) 0.0224(17) 0.0112(15) 0.0009(12) 0.0010(12) 0.0037(13) C45 0.0236(19) 0.044(2) 0.0157(18) -0.0069(16) 0.0010(14) 0.0080(17) C48 0.0275(19) 0.0254(18) 0.0190(18) 0.0002(14) 0.0026(14) 0.0056(15) C44 0.0185(17) 0.0289(19) 0.0164(17) -0.0016(14) -0.0004(13) 0.0040(14) C46 0.0257(19) 0.048(2) 0.0180(18) -0.0018(17) 0.0091(15) 0.0002(18) C47 0.036(2) 0.037(2) 0.0191(19) 0.0121(16) 0.0065(16) 0.0050(18) C112 0.036(2) 0.031(2) 0.032(2) -0.0031(16) 0.0041(17) 0.0192(18) C55 0.0198(16) 0.0158(15) 0.0161(16) 0.0029(12) 0.0049(13) 0.0069(13) C60 0.0209(17) 0.0200(17) 0.030(2) 0.0017(14) 0.0059(15) 0.0047(14) C59 0.030(2) 0.0222(19) 0.050(3) 0.0122(18) 0.0126(19) 0.0027(16) C57 0.033(2) 0.032(2) 0.036(2) 0.0101(17) -0.0010(17) 0.0160(18) C58 0.046(2) 0.025(2) 0.040(2) 0.0155(17) 0.0126(19) 0.0186(18) C56 0.033(2) 0.0198(17) 0.027(2) 0.0038(15) -0.0028(16) 0.0092(16) C13 0.0122(15) 0.0151(15) 0.0176(16) -0.0012(12) 0.0002(12) 0.0028(12) C14 0.0128(15) 0.0147(15) 0.0185(16) 0.0027(12) 0.0013(12) 0.0038(12) C4 0.0094(14) 0.0179(15) 0.0159(16) 0.0033(12) 0.0017(12) 0.0024(12) N8 0.0113(12) 0.0180(13) 0.0161(14) 0.0017(11) 0.0033(10) 0.0053(11) N7 0.0116(12) 0.0146(12) 0.0128(13) 0.0004(10) 0.0017(10) 0.0049(10) N6 0.0143(13) 0.0165(13) 0.0106(13) 0.0002(10) 0.0010(10) 0.0059(11) N5 0.0150(13) 0.0135(12) 0.0118(13) 0.0012(10) 0.0014(10) 0.0014(10) C3 0.0143(15) 0.0132(14) 0.0156(16) -0.0023(12) 0.0004(12) 0.0042(12) C11 0.0170(16) 0.0178(15) 0.0110(15) 0.0017(12) 0.0012(12) 0.0018(13) C49 0.0182(16) 0.0293(18) 0.0114(16) 0.0060(13) 0.0029(12) 0.0087(14) C10 0.0182(16) 0.0179(16) 0.0117(15) -0.0002(12) -0.0001(12) 0.0058(13) C54 0.0297(19) 0.032(2) 0.0207(18) 0.0074(15) 0.0014(15) 0.0131(16) C50 0.0217(18) 0.035(2) 0.0189(18) 0.0041(15) -0.0022(14) 0.0063(16) C51 0.027(2) 0.049(3) 0.027(2) 0.0051(18) -0.0052(16) 0.0088(18) C53 0.032(2) 0.040(2) 0.031(2) 0.0118(17) 0.0078(17) 0.0201(18) C52 0.028(2) 0.052(3) 0.026(2) 0.0167(18) 0.0031(16) 0.0168(19) C12 0.0140(15) 0.0193(16) 0.0130(15) 0.0005(12) 0.0003(12) 0.0052(13) C16 0.0152(15) 0.0144(15) 0.0158(16) 0.0024(12) 0.0015(12) 0.0017(12) C15 0.0148(15) 0.0197(16) 0.0134(15) 0.0034(12) 0.0037(12) 0.0051(13) C17 0.0158(15) 0.0198(16) 0.0141(16) 0.0002(12) 0.0018(12) 0.0079(13) C18 0.0162(15) 0.0186(15) 0.0111(15) -0.0004(12) -0.0004(12) 0.0075(13) C1 0.0121(14) 0.0144(15) 0.0186(16) 0.0023(12) -0.0001(12) 0.0066(12) N2 0.0135(13) 0.0160(13) 0.0122(13) 0.0009(10) -0.0013(10) 0.0039(10) N1 0.0146(13) 0.0170(13) 0.0109(13) -0.0004(10) -0.0004(10) 0.0057(11) C5 0.0158(15) 0.0191(16) 0.0147(16) 0.0011(12) 0.0019(12) 0.0053(13) C84 0.0173(16) 0.0212(16) 0.0121(15) 0.0038(12) 0.0034(12) 0.0087(13) C83 0.0201(16) 0.0163(15) 0.0090(14) 0.0009(12) 0.0028(12) 0.0084(13) C67 0.0159(15) 0.0136(15) 0.0139(15) -0.0005(12) 0.0015(12) 0.0055(12) N10 0.0160(13) 0.0184(13) 0.0114(13) 0.0020(10) 0.0029(10) 0.0079(11) N9 0.0142(13) 0.0178(13) 0.0129(13) 0.0001(10) 0.0023(10) 0.0059(11) C74 0.0118(15) 0.0173(15) 0.0172(16) 0.0005(12) 0.0014(12) 0.0040(12) C73 0.0129(15) 0.0146(15) 0.0167(16) -0.0003(12) 0.0021(12) 0.0034(12) C68 0.0165(15) 0.0167(15) 0.0133(15) 0.0000(12) -0.0006(12) 0.0074(13) N12 0.0162(13) 0.0162(13) 0.0125(13) -0.0001(10) 0.0010(10) 0.0053(11) N11 0.0145(13) 0.0143(13) 0.0121(13) 0.0007(10) 0.0021(10) 0.0041(10) C71 0.0161(15) 0.0144(15) 0.0142(16) 0.0004(12) 0.0020(12) 0.0026(12) C72 0.0130(15) 0.0182(15) 0.0127(15) -0.0008(12) 0.0006(12) 0.0038(12) C75 0.0132(15) 0.0201(16) 0.0129(15) 0.0007(12) -0.0001(12) 0.0067(13) P2 0.0181(4) 0.0278(5) 0.0277(5) 0.0039(4) 0.0008(4) 0.0052(4) P3 0.0148(4) 0.0295(5) 0.0406(6) 0.0072(4) 0.0054(4) 0.0029(4) F13 0.0205(11) 0.0368(13) 0.0531(15) 0.0040(11) 0.0011(10) 0.0099(10) F18 0.0176(11) 0.0480(14) 0.0443(14) -0.0071(11) 0.0059(10) -0.0005(10) F17 0.0267(12) 0.0314(12) 0.0460(14) 0.0075(10) 0.0119(10) 0.0024(10) F15 0.0228(11) 0.0333(12) 0.0475(14) 0.0073(11) 0.0006(10) 0.0016(10) F14 0.0207(11) 0.0556(15) 0.0479(15) 0.0209(12) 0.0077(10) 0.0075(11) C77 0.0169(15) 0.0170(15) 0.0114(15) 0.0048(12) 0.0037(12) 0.0055(13) C76 0.0192(16) 0.0159(15) 0.0097(15) 0.0005(12) 0.0015(12) 0.0040(13) C69 0.0144(15) 0.0125(14) 0.0164(16) 0.0038(12) 0.0025(12) 0.0018(12) N13 0.0139(13) 0.0141(12) 0.0109(13) -0.0006(10) 0.0015(10) 0.0037(10) N14 0.0140(13) 0.0157(13) 0.0105(13) 0.0008(10) 0.0003(10) 0.0034(10) C78 0.0156(15) 0.0161(15) 0.0139(15) 0.0029(12) 0.0022(12) 0.0058(12) C79 0.0152(15) 0.0208(16) 0.0117(15) 0.0045(12) 0.0013(12) 0.0064(13) N15 0.0118(12) 0.0132(12) 0.0146(13) 0.0007(10) 0.0008(10) 0.0019(10) C80 0.0123(15) 0.0151(15) 0.0191(16) 0.0017(12) 0.0021(12) 0.0041(12) C81 0.0090(14) 0.0145(15) 0.0153(16) 0.0009(12) 0.0009(11) 0.0005(12) C6 0.0135(15) 0.0143(15) 0.0193(16) 0.0020(12) 0.0033(12) 0.0049(12) C7 0.0120(14) 0.0155(15) 0.0135(15) 0.0010(12) 0.0013(12) 0.0046(12) C9 0.0168(15) 0.0169(15) 0.0140(16) -0.0014(12) 0.0017(12) 0.0060(13) C8 0.0187(16) 0.0152(15) 0.0135(15) 0.0005(12) 0.0046(12) 0.0046(13) F10 0.0358(13) 0.0449(14) 0.0372(14) 0.0054(11) 0.0098(11) 0.0005(11) F9 0.0393(14) 0.0519(16) 0.0689(19) 0.0049(14) 0.0075(13) 0.0276(13) F11 0.0374(14) 0.0586(17) 0.0395(15) -0.0160(12) 0.0058(11) -0.0063(12) F7 0.0439(15) 0.0557(16) 0.0391(15) 0.0141(12) 0.0079(12) -0.0089(12) F12 0.0490(16) 0.0617(18) 0.0650(19) 0.0067(14) -0.0094(14) 0.0342(14) F8 0.0341(13) 0.0353(13) 0.0344(13) -0.0013(10) -0.0044(10) 0.0044(10) F16 0.0273(12) 0.0386(13) 0.0592(16) 0.0090(12) 0.0140(11) 0.0128(10) N4 0.0120(12) 0.0126(12) 0.0138(13) 0.0009(10) 0.0013(10) 0.0032(10) N3 0.0128(12) 0.0119(12) 0.0145(13) -0.0028(10) 0.0011(10) 0.0030(10) N16 0.0124(12) 0.0149(13) 0.0181(14) 0.0012(10) 0.0039(10) 0.0054(10) C2 0.0160(15) 0.0213(16) 0.0110(15) 0.0034(12) 0.0013(12) 0.0050(13) C70 0.0127(14) 0.0141(15) 0.0134(15) 0.0017(12) 0.0015(12) 0.0017(12) C82 0.0137(15) 0.0185(16) 0.0113(15) -0.0017(12) -0.0006(12) 0.0020(12) P4 0.0413(6) 0.0408(6) 0.0432(7) 0.0153(5) 0.0089(5) 0.0192(5) F21 0.129(3) 0.110(3) 0.065(2) 0.0365(19) 0.041(2) 0.100(3) F24 0.114(3) 0.068(2) 0.106(3) 0.022(2) -0.035(2) 0.050(2) F22 0.064(3) 0.138(4) 0.171(5) 0.032(4) -0.004(3) -0.009(3) F20 0.322(8) 0.199(5) 0.028(2) -0.021(3) -0.023(3) 0.180(6) F19 0.048(2) 0.117(4) 0.559(14) 0.173(6) 0.062(5) 0.008(3) F23 0.252(6) 0.176(5) 0.072(3) 0.030(3) 0.044(3) 0.170(5) P1 0.0275(5) 0.0224(4) 0.0215(5) 0.0024(4) 0.0045(4) 0.0096(4) F1 0.0552(16) 0.0583(16) 0.0209(12) 0.0034(11) 0.0038(11) 0.0149(13) F2 0.0460(14) 0.0313(12) 0.0503(15) 0.0000(11) -0.0024(12) 0.0165(11) F4 0.0416(15) 0.0516(16) 0.0734(19) 0.0076(14) 0.0319(14) 0.0143(13) F3 0.0310(13) 0.0518(16) 0.081(2) 0.0144(15) -0.0047(13) 0.0093(12) F6 0.0582(16) 0.0356(13) 0.0550(16) 0.0100(12) 0.0197(13) 0.0218(12) F5 0.146(3) 0.0554(18) 0.0142(13) -0.0015(12) -0.0018(16) -0.0041(19) _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 Ag3 C68 2.095(3) . ? Ag3 C2 2.099(3) . ? Ag3 Ag2 3.3400(5) . ? Ag1 C3 2.144(3) . ? Ag1 C1 2.143(3) . ? Ag1 Ag2 3.1484(5) . ? Ag1 Ag4 3.2897(5) . ? Ag2 C67 2.137(3) . ? Ag2 C69 2.139(3) . ? Ag4 C70 2.077(3) . ? Ag4 C4 2.092(3) . ? C85 C86 1.396(5) . ? C85 C91 1.382(5) . ? C85 C84 1.480(4) . ? C19 C20 1.380(5) . ? C19 C24 1.398(4) . ? C19 C17 1.477(4) . ? C62 C63 1.383(5) . ? C62 C61 1.394(5) . ? C62 H62 0.9500 . ? C88 C89 1.381(5) . ? C88 C87 1.381(5) . ? C88 H88 0.9500 . ? C61 C66 1.393(5) . ? C61 C14 1.472(4) . ? C65 C64 1.386(5) . ? C65 C66 1.394(5) . ? C65 H65 0.9500 . ? C64 C63 1.380(5) . ? C64 H64 0.9500 . ? C89 C91 1.386(5) . ? C89 H89 0.9500 . ? C86 C87 1.388(5) . ? C86 H86 0.9500 . ? C66 H66 0.9500 . ? C24 C23 1.384(5) . ? C24 H24 0.9500 . ? C22 C21 1.379(5) . ? C22 C23 1.367(5) . ? C22 H22 0.9500 . ? C87 H87 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C91 H91 0.9500 . ? C23 H23 0.9500 . ? C63 H63 0.9500 . ? C21 H21 0.9500 . ? C92 C97 1.391(4) . ? C92 C93 1.391(5) . ? C92 C83 1.471(4) . ? C97 C96 1.382(5) . ? C97 H97 0.9500 . ? C93 C94 1.395(5) . ? C93 H93 0.9500 . ? C95 C94 1.363(5) . ? C95 C96 1.389(5) . ? C95 H95 0.9500 . ? C94 H94 0.9500 . ? C96 H96 0.9500 . ? C128 C133 1.395(4) . ? C128 C129 1.390(5) . ? C128 C81 1.478(4) . ? C133 C132 1.394(5) . ? C133 H133 0.9500 . ? C129 C130 1.378(5) . ? C129 H129 0.9500 . ? C132 C131 1.390(5) . ? C132 H132 0.9500 . ? C131 C130 1.398(5) . ? C131 H131 0.9500 . ? C130 H130 0.9500 . ? C98 C99 1.394(4) . ? C98 C103 1.397(4) . ? C98 C73 1.475(4) . ? C103 C102 1.395(5) . ? C103 H103 0.9500 . ? C101 C102 1.373(5) . ? C101 C100 1.385(5) . ? C101 H101 0.9500 . ? C99 C100 1.388(5) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? C102 H102 0.9500 . ? C120 C121 1.379(5) . ? C120 C119 1.387(5) . ? C120 H120 0.9500 . ? C116 C117 1.389(5) . ? C116 C121 1.400(4) . ? C116 C77 1.483(4) . ? C121 H121 0.9500 . ? C119 C118 1.383(5) . ? C119 H119 0.9500 . ? C117 C118 1.389(5) . ? C117 H117 0.9500 . ? C118 H118 0.9500 . ? C40 C41 1.371(5) . ? C40 C39 1.388(5) . ? C40 H40 0.9500 . ? C39 C38 1.391(5) . ? C39 H39 0.9500 . ? C38 C37 1.392(4) . ? C38 H38 0.9500 . ? C37 C42 1.384(4) . ? C37 C7 1.473(4) . ? C41 C42 1.400(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C110 C115 1.389(4) . ? C110 C111 1.393(5) . ? C110 C76 1.478(4) . ? C115 C114 1.388(5) . ? C115 H115 0.9500 . ? C111 C112 1.387(5) . ? C111 H111 0.9500 . ? C113 C112 1.375(5) . ? C113 C114 1.386(5) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C30 C25 1.393(4) . ? C30 C29 1.384(5) . ? C30 H30 0.9500 . ? C25 C26 1.391(5) . ? C25 C18 1.474(4) . ? C29 C28 1.383(5) . ? C29 H29 0.9500 . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 C28 1.384(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C104 C105 1.392(5) . ? C104 C109 1.390(4) . ? C104 C74 1.479(4) . ? C105 C106 1.394(5) . ? C105 H105 0.9500 . ? C109 C108 1.392(5) . ? C109 H109 0.9500 . ? C108 C107 1.382(5) . ? C108 H108 0.9500 . ? C107 C106 1.376(5) . ? C107 H107 0.9500 . ? C106 H106 0.9500 . ? C122 C123 1.382(5) . ? C122 C127 1.395(5) . ? C122 C80 1.485(4) . ? C127 C126 1.396(5) . ? C127 H127 0.9500 . ? C126 C125 1.377(5) . ? C126 H126 0.9500 . ? C123 C124 1.385(5) . ? C123 H123 0.9500 . ? C125 C124 1.390(5) . ? C125 H125 0.9500 . ? C124 H124 0.9500 . ? C32 C33 1.381(5) . ? C32 C31 1.385(4) . ? C32 H32 0.9500 . ? C36 C31 1.396(4) . ? C36 C35 1.393(5) . ? C36 H36 0.9500 . ? C31 C6 1.476(4) . ? C34 C35 1.380(5) . ? C34 C33 1.382(5) . ? C34 H34 0.9500 . ? C33 H33 0.9500 . ? C35 H35 0.9500 . ? C43 C48 1.390(5) . ? C43 C44 1.399(5) . ? C43 C10 1.485(4) . ? C45 C44 1.379(5) . ? C45 C46 1.390(6) . ? C45 H45 0.9500 . ? C48 C47 1.381(5) . ? C48 H48 0.9500 . ? C44 H44 0.9500 . ? C46 C47 1.379(6) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C112 H112 0.9500 . ? C55 C60 1.389(5) . ? C55 C56 1.393(5) . ? C55 C13 1.473(4) . ? C60 C59 1.397(5) . ? C60 H60 0.9500 . ? C59 C58 1.360(6) . ? C59 H59 0.9500 . ? C57 C56 1.377(5) . ? C57 C58 1.389(5) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C56 H56 0.9500 . ? C13 C14 1.363(4) . ? C13 N7 1.404(4) . ? C14 N8 1.393(4) . ? C4 N8 1.336(4) . ? C4 N7 1.357(4) . ? N8 C15 1.470(4) . ? N7 C12 1.448(4) . ? N6 C3 1.352(4) . ? N6 C11 1.401(4) . ? N6 C12 1.487(4) . ? N5 C3 1.358(4) . ? N5 C10 1.406(4) . ? N5 C9 1.454(4) . ? C11 C10 1.356(4) . ? C11 C49 1.482(4) . ? C49 C54 1.392(5) . ? C49 C50 1.388(5) . ? C54 C53 1.389(5) . ? C54 H54 0.9500 . ? C50 C51 1.394(5) . ? C50 H50 0.9500 . ? C51 C52 1.373(6) . ? C51 H51 0.9500 . ? C53 C52 1.375(6) . ? C53 H53 0.9500 . ? C52 H52 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C16 N1 1.461(4) . ? C16 C15 1.518(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.358(4) . ? C17 N1 1.406(4) . ? C18 N2 1.399(4) . ? C1 N2 1.362(4) . ? C1 N1 1.364(4) . ? N2 C5 1.477(4) . ? C5 N3 1.438(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C84 C83 1.357(4) . ? C84 N10 1.406(4) . ? C83 N9 1.403(4) . ? C67 N9 1.361(4) . ? C67 N10 1.370(4) . ? N10 C71 1.457(4) . ? N9 C82 1.472(4) . ? C74 C73 1.359(4) . ? C74 N12 1.398(4) . ? C73 N11 1.398(4) . ? C68 N11 1.357(4) . ? C68 N12 1.359(4) . ? N12 C75 1.441(4) . ? N11 C72 1.466(4) . ? C71 C72 1.525(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C75 N13 1.477(4) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? P2 F12 1.577(3) . ? P2 F10 1.589(2) . ? P2 F9 1.590(2) . ? P2 F11 1.594(3) . ? P2 F8 1.602(2) . ? P2 F7 1.599(2) . ? P3 F17 1.596(2) . ? P3 F15 1.597(2) . ? P3 F16 1.599(2) . ? P3 F18 1.607(2) . ? P3 F14 1.607(2) . ? P3 F13 1.609(2) . ? C77 C76 1.356(4) . ? C77 N14 1.388(4) . ? C76 N13 1.392(4) . ? C69 N13 1.355(4) . ? C69 N14 1.365(4) . ? N14 C78 1.455(4) . ? C78 C79 1.521(4) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 N15 1.472(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? N15 C70 1.348(4) . ? N15 C80 1.394(4) . ? C80 C81 1.350(4) . ? C81 N16 1.397(4) . ? C6 C7 1.370(4) . ? C6 N3 1.390(4) . ? C7 N4 1.401(4) . ? C9 C8 1.534(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8 N4 1.457(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N4 C2 1.343(4) . ? N3 C2 1.362(4) . ? N16 C70 1.369(4) . ? N16 C82 1.452(4) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? P4 F19 1.488(4) . ? P4 F20 1.523(4) . ? P4 F22 1.553(4) . ? P4 F23 1.574(4) . ? P4 F24 1.575(3) . ? P4 F21 1.585(3) . ? P1 F5 1.568(3) . ? P1 F3 1.585(3) . ? P1 F4 1.589(3) . ? P1 F1 1.597(2) . ? P1 F2 1.602(2) . ? P1 F6 1.599(2) . ? 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 C68 Ag3 C2 170.04(12) . . ? C68 Ag3 Ag2 58.16(8) . . ? C2 Ag3 Ag2 112.62(9) . . ? C3 Ag1 C1 162.73(11) . . ? C3 Ag1 Ag2 98.12(8) . . ? C1 Ag1 Ag2 99.02(8) . . ? C3 Ag1 Ag4 87.62(8) . . ? C1 Ag1 Ag4 101.84(8) . . ? Ag2 Ag1 Ag4 63.927(12) . . ? C67 Ag2 C69 161.82(11) . . ? C67 Ag2 Ag1 100.62(8) . . ? C69 Ag2 Ag1 97.40(8) . . ? C67 Ag2 Ag3 102.90(8) . . ? C69 Ag2 Ag3 87.16(8) . . ? Ag1 Ag2 Ag3 64.093(11) . . ? C70 Ag4 C4 173.34(12) . . ? C70 Ag4 Ag1 115.07(8) . . ? C4 Ag4 Ag1 58.81(8) . . ? C86 C85 C91 118.6(3) . . ? C86 C85 C84 122.2(3) . . ? C91 C85 C84 119.1(3) . . ? C20 C19 C24 117.8(3) . . ? C20 C19 C17 124.1(3) . . ? C24 C19 C17 118.1(3) . . ? C63 C62 C61 119.7(3) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C89 C88 C87 119.3(3) . . ? C89 C88 H88 120.3 . . ? C87 C88 H88 120.3 . . ? C66 C61 C62 119.8(3) . . ? C66 C61 C14 121.9(3) . . ? C62 C61 C14 118.3(3) . . ? C64 C65 C66 119.7(3) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C63 C64 C65 120.3(3) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C88 C89 C91 120.5(3) . . ? C88 C89 H89 119.7 . . ? C91 C89 H89 119.7 . . ? C85 C86 C87 120.4(3) . . ? C85 C86 H86 119.8 . . ? C87 C86 H86 119.8 . . ? C61 C66 C65 120.0(3) . . ? C61 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C19 C24 C23 120.5(3) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C88 C87 C86 120.3(3) . . ? C88 C87 H87 119.8 . . ? C86 C87 H87 119.8 . . ? C19 C20 C21 121.3(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C89 C91 C85 120.7(3) . . ? C89 C91 H91 119.7 . . ? C85 C91 H91 119.7 . . ? C22 C23 C24 120.8(3) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C64 C63 C62 120.6(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C22 C21 C20 120.3(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C97 C92 C93 119.5(3) . . ? C97 C92 C83 121.8(3) . . ? C93 C92 C83 118.7(3) . . ? C96 C97 C92 120.0(3) . . ? C96 C97 H97 120.0 . . ? C92 C97 H97 120.0 . . ? C94 C93 C92 119.8(3) . . ? C94 C93 H93 120.1 . . ? C92 C93 H93 120.1 . . ? C94 C95 C96 120.3(3) . . ? C94 C95 H95 119.9 . . ? C96 C95 H95 119.9 . . ? C95 C94 C93 120.3(3) . . ? C95 C94 H94 119.8 . . ? C93 C94 H94 119.8 . . ? C97 C96 C95 120.1(3) . . ? C97 C96 H96 119.9 . . ? C95 C96 H96 119.9 . . ? C133 C128 C129 119.5(3) . . ? C133 C128 C81 120.3(3) . . ? C129 C128 C81 120.2(3) . . ? C128 C133 C132 119.7(3) . . ? C128 C133 H133 120.2 . . ? C132 C133 H133 120.2 . . ? C130 C129 C128 120.9(3) . . ? C130 C129 H129 119.5 . . ? C128 C129 H129 119.5 . . ? C133 C132 C131 120.5(3) . . ? C133 C132 H132 119.7 . . ? C131 C132 H132 119.7 . . ? C130 C131 C132 119.4(3) . . ? C130 C131 H131 120.3 . . ? C132 C131 H131 120.3 . . ? C129 C130 C131 120.0(3) . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C99 C98 C103 119.6(3) . . ? C99 C98 C73 122.1(3) . . ? C103 C98 C73 118.3(3) . . ? C102 C103 C98 119.6(3) . . ? C102 C103 H103 120.2 . . ? C98 C103 H103 120.2 . . ? C102 C101 C100 120.6(3) . . ? C102 C101 H101 119.7 . . ? C100 C101 H101 119.7 . . ? C98 C99 C100 120.2(3) . . ? C98 C99 H99 119.9 . . ? C100 C99 H99 119.9 . . ? C101 C100 C99 119.8(3) . . ? C101 C100 H100 120.1 . . ? C99 C100 H100 120.1 . . ? C101 C102 C103 120.3(3) . . ? C101 C102 H102 119.9 . . ? C103 C102 H102 119.9 . . ? C121 C120 C119 120.2(3) . . ? C121 C120 H120 119.9 . . ? C119 C120 H120 119.9 . . ? C117 C116 C121 119.4(3) . . ? C117 C116 C77 118.3(3) . . ? C121 C116 C77 122.3(3) . . ? C120 C121 C116 120.1(3) . . ? C120 C121 H121 120.0 . . ? C116 C121 H121 120.0 . . ? C118 C119 C120 120.2(3) . . ? C118 C119 H119 119.9 . . ? C120 C119 H119 119.9 . . ? C118 C117 C116 120.2(3) . . ? C118 C117 H117 119.9 . . ? C116 C117 H117 119.9 . . ? C117 C118 C119 120.0(3) . . ? C117 C118 H118 120.0 . . ? C119 C118 H118 120.0 . . ? C41 C40 C39 120.6(3) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C39 C38 119.8(3) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C42 C37 C38 119.2(3) . . ? C42 C37 C7 120.3(3) . . ? C38 C37 C7 120.4(3) . . ? C40 C41 C42 119.5(3) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C37 C42 C41 120.7(3) . . ? C37 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C115 C110 C111 118.6(3) . . ? C115 C110 C76 121.3(3) . . ? C111 C110 C76 120.0(3) . . ? C114 C115 C110 120.4(3) . . ? C114 C115 H115 119.8 . . ? C110 C115 H115 119.8 . . ? C112 C111 C110 121.0(3) . . ? C112 C111 H111 119.5 . . ? C110 C111 H111 119.5 . . ? C112 C113 C114 120.0(3) . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C115 C114 C113 120.2(3) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C25 C30 C29 119.9(3) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C26 C25 C30 119.8(3) . . ? C26 C25 C18 118.5(3) . . ? C30 C25 C18 121.7(3) . . ? C28 C29 C30 120.3(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C26 C27 119.8(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C105 C104 C109 119.6(3) . . ? C105 C104 C74 119.4(3) . . ? C109 C104 C74 120.9(3) . . ? C104 C105 C106 119.5(3) . . ? C104 C105 H105 120.2 . . ? C106 C105 H105 120.2 . . ? C104 C109 C108 120.1(3) . . ? C104 C109 H109 120.0 . . ? C108 C109 H109 120.0 . . ? C107 C108 C109 120.2(3) . . ? C107 C108 H108 119.9 . . ? C109 C108 H108 119.9 . . ? C108 C107 C106 119.8(3) . . ? C108 C107 H107 120.1 . . ? C106 C107 H107 120.1 . . ? C107 C106 C105 120.8(3) . . ? C107 C106 H106 119.6 . . ? C105 C106 H106 119.6 . . ? C123 C122 C127 119.2(3) . . ? C123 C122 C80 119.8(3) . . ? C127 C122 C80 120.9(3) . . ? C122 C127 C126 119.8(3) . . ? C122 C127 H127 120.1 . . ? C126 C127 H127 120.1 . . ? C125 C126 C127 120.3(3) . . ? C125 C126 H126 119.8 . . ? C127 C126 H126 119.8 . . ? C122 C123 C124 121.0(3) . . ? C122 C123 H123 119.5 . . ? C124 C123 H123 119.5 . . ? C126 C125 C124 120.0(3) . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C124 C123 119.6(3) . . ? C125 C124 H124 120.2 . . ? C123 C124 H124 120.2 . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C31 C36 C35 119.3(3) . . ? C31 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C31 C32 119.3(3) . . ? C36 C31 C6 119.1(3) . . ? C32 C31 C6 121.5(3) . . ? C35 C34 C33 119.5(3) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C32 C33 C34 120.2(3) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C34 C35 C36 120.9(3) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C48 C43 C44 119.1(3) . . ? C48 C43 C10 118.9(3) . . ? C44 C43 C10 121.9(3) . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C43 C48 C47 120.0(3) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C47 C46 C45 119.7(3) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 120.8(4) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C113 C112 C111 119.8(4) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C60 C55 C56 119.2(3) . . ? C60 C55 C13 119.7(3) . . ? C56 C55 C13 120.9(3) . . ? C55 C60 C59 119.5(3) . . ? C55 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C58 C59 C60 120.7(3) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C56 C57 C58 119.6(4) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C59 C58 C57 120.3(3) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C57 C56 C55 120.8(3) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C14 C13 N7 105.9(3) . . ? C14 C13 C55 129.0(3) . . ? N7 C13 C55 124.9(3) . . ? C13 C14 N8 105.7(3) . . ? C13 C14 C61 128.0(3) . . ? N8 C14 C61 125.8(3) . . ? N8 C4 N7 104.2(3) . . ? N8 C4 Ag4 125.7(2) . . ? N7 C4 Ag4 130.1(2) . . ? C4 N8 C14 112.8(3) . . ? C4 N8 C15 121.7(3) . . ? C14 N8 C15 125.4(3) . . ? C4 N7 C13 111.4(3) . . ? C4 N7 C12 122.7(3) . . ? C13 N7 C12 125.9(3) . . ? C3 N6 C11 112.6(3) . . ? C3 N6 C12 125.3(3) . . ? C11 N6 C12 120.0(2) . . ? C3 N5 C10 111.8(3) . . ? C3 N5 C9 124.5(3) . . ? C10 N5 C9 123.6(2) . . ? N6 C3 N5 103.5(3) . . ? N6 C3 Ag1 126.5(2) . . ? N5 C3 Ag1 128.2(2) . . ? C10 C11 N6 105.7(3) . . ? C10 C11 C49 130.8(3) . . ? N6 C11 C49 123.4(3) . . ? C54 C49 C50 119.5(3) . . ? C54 C49 C11 120.1(3) . . ? C50 C49 C11 120.4(3) . . ? C11 C10 N5 106.2(3) . . ? C11 C10 C43 131.4(3) . . ? N5 C10 C43 122.2(3) . . ? C49 C54 C53 120.2(4) . . ? C49 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C49 C50 C51 119.2(4) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C52 C51 C50 121.3(4) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C52 C53 C54 120.3(4) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C51 C52 C53 119.6(4) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? N7 C12 N6 112.8(2) . . ? N7 C12 H12A 109.0 . . ? N6 C12 H12A 109.0 . . ? N7 C12 H12B 109.0 . . ? N6 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N1 C16 C15 115.0(2) . . ? N1 C16 H16A 108.5 . . ? C15 C16 H16A 108.5 . . ? N1 C16 H16B 108.5 . . ? C15 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N8 C15 C16 113.1(2) . . ? N8 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N8 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C18 C17 N1 105.9(3) . . ? C18 C17 C19 128.6(3) . . ? N1 C17 C19 125.3(3) . . ? C17 C18 N2 106.5(3) . . ? C17 C18 C25 129.6(3) . . ? N2 C18 C25 123.9(3) . . ? N2 C1 N1 103.6(3) . . ? N2 C1 Ag1 126.8(2) . . ? N1 C1 Ag1 129.1(2) . . ? C1 N2 C18 112.0(3) . . ? C1 N2 C5 127.5(3) . . ? C18 N2 C5 120.4(2) . . ? C1 N1 C17 111.9(2) . . ? C1 N1 C16 123.7(3) . . ? C17 N1 C16 124.3(3) . . ? N3 C5 N2 114.2(2) . . ? N3 C5 H5A 108.7 . . ? N2 C5 H5A 108.7 . . ? N3 C5 H5B 108.7 . . ? N2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C83 C84 N10 106.4(3) . . ? C83 C84 C85 128.5(3) . . ? N10 C84 C85 124.9(3) . . ? C84 C83 N9 106.4(3) . . ? C84 C83 C92 128.7(3) . . ? N9 C83 C92 124.9(3) . . ? N9 C67 N10 103.8(3) . . ? N9 C67 Ag2 128.0(2) . . ? N10 C67 Ag2 127.7(2) . . ? C67 N10 C84 111.5(3) . . ? C67 N10 C71 123.9(2) . . ? C84 N10 C71 124.5(3) . . ? C67 N9 C83 112.0(3) . . ? C67 N9 C82 127.9(3) . . ? C83 N9 C82 119.8(2) . . ? C73 C74 N12 105.9(3) . . ? C73 C74 C104 129.0(3) . . ? N12 C74 C104 125.1(3) . . ? C74 C73 N11 106.3(3) . . ? C74 C73 C98 128.5(3) . . ? N11 C73 C98 124.9(3) . . ? N11 C68 N12 103.7(3) . . ? N11 C68 Ag3 125.8(2) . . ? N12 C68 Ag3 130.5(2) . . ? C68 N12 C74 112.2(3) . . ? C68 N12 C75 122.4(3) . . ? C74 N12 C75 125.4(3) . . ? C68 N11 C73 111.9(3) . . ? C68 N11 C72 121.7(3) . . ? C73 N11 C72 126.2(3) . . ? N10 C71 C72 114.4(2) . . ? N10 C71 H71A 108.7 . . ? C72 C71 H71A 108.7 . . ? N10 C71 H71B 108.7 . . ? C72 C71 H71B 108.7 . . ? H71A C71 H71B 107.6 . . ? N11 C72 C71 112.5(2) . . ? N11 C72 H72A 109.1 . . ? C71 C72 H72A 109.1 . . ? N11 C72 H72B 109.1 . . ? C71 C72 H72B 109.1 . . ? H72A C72 H72B 107.8 . . ? N12 C75 N13 113.1(2) . . ? N12 C75 H75A 109.0 . . ? N13 C75 H75A 109.0 . . ? N12 C75 H75B 109.0 . . ? N13 C75 H75B 109.0 . . ? H75A C75 H75B 107.8 . . ? F12 P2 F10 90.54(15) . . ? F12 P2 F9 179.47(18) . . ? F10 P2 F9 89.34(14) . . ? F12 P2 F11 90.12(15) . . ? F10 P2 F11 90.14(13) . . ? F9 P2 F11 90.39(15) . . ? F12 P2 F8 90.10(14) . . ? F10 P2 F8 90.35(13) . . ? F9 P2 F8 89.38(14) . . ? F11 P2 F8 179.45(15) . . ? F12 P2 F7 90.95(16) . . ? F10 P2 F7 178.46(16) . . ? F9 P2 F7 89.17(15) . . ? F11 P2 F7 89.46(14) . . ? F8 P2 F7 90.04(13) . . ? F17 P3 F15 90.73(13) . . ? F17 P3 F16 90.53(13) . . ? F15 P3 F16 89.82(13) . . ? F17 P3 F18 89.91(13) . . ? F15 P3 F18 179.23(15) . . ? F16 P3 F18 90.60(13) . . ? F17 P3 F14 178.12(13) . . ? F15 P3 F14 89.75(13) . . ? F16 P3 F14 91.30(13) . . ? F18 P3 F14 89.60(13) . . ? F17 P3 F13 88.89(13) . . ? F15 P3 F13 89.47(13) . . ? F16 P3 F13 179.08(15) . . ? F18 P3 F13 90.12(13) . . ? F14 P3 F13 89.29(13) . . ? C76 C77 N14 106.6(3) . . ? C76 C77 C116 130.1(3) . . ? N14 C77 C116 123.0(3) . . ? C77 C76 N13 106.0(3) . . ? C77 C76 C110 129.9(3) . . ? N13 C76 C110 124.0(3) . . ? N13 C69 N14 103.5(3) . . ? N13 C69 Ag2 126.5(2) . . ? N14 C69 Ag2 127.8(2) . . ? C69 N13 C76 112.2(3) . . ? C69 N13 C75 125.7(3) . . ? C76 N13 C75 120.4(2) . . ? C69 N14 C77 111.7(3) . . ? C69 N14 C78 124.4(3) . . ? C77 N14 C78 123.9(3) . . ? N14 C78 C79 113.0(2) . . ? N14 C78 H78A 109.0 . . ? C79 C78 H78A 109.0 . . ? N14 C78 H78B 109.0 . . ? C79 C78 H78B 109.0 . . ? H78A C78 H78B 107.8 . . ? N15 C79 C78 110.6(2) . . ? N15 C79 H79A 109.5 . . ? C78 C79 H79A 109.5 . . ? N15 C79 H79B 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 108.1 . . ? C70 N15 C80 112.3(3) . . ? C70 N15 C79 121.6(3) . . ? C80 N15 C79 126.0(3) . . ? C81 C80 N15 106.6(3) . . ? C81 C80 C122 129.8(3) . . ? N15 C80 C122 123.5(3) . . ? C80 C81 N16 105.8(3) . . ? C80 C81 C128 130.6(3) . . ? N16 C81 C128 123.4(3) . . ? C7 C6 N3 106.0(3) . . ? C7 C6 C31 129.7(3) . . ? N3 C6 C31 124.1(3) . . ? C6 C7 N4 105.8(3) . . ? C6 C7 C37 130.9(3) . . ? N4 C7 C37 123.3(3) . . ? N5 C9 C8 112.4(2) . . ? N5 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? N5 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? N4 C8 C9 110.7(2) . . ? N4 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C2 N4 C7 112.1(3) . . ? C2 N4 C8 121.3(3) . . ? C7 N4 C8 126.4(2) . . ? C2 N3 C6 112.0(3) . . ? C2 N3 C5 121.0(3) . . ? C6 N3 C5 126.2(3) . . ? C70 N16 C81 112.0(3) . . ? C70 N16 C82 121.1(3) . . ? C81 N16 C82 126.4(3) . . ? N4 C2 N3 104.1(3) . . ? N4 C2 Ag3 125.8(2) . . ? N3 C2 Ag3 129.8(2) . . ? N15 C70 N16 103.3(3) . . ? N15 C70 Ag4 125.1(2) . . ? N16 C70 Ag4 131.4(2) . . ? N16 C82 N9 114.4(2) . . ? N16 C82 H82A 108.7 . . ? N9 C82 H82A 108.7 . . ? N16 C82 H82B 108.7 . . ? N9 C82 H82B 108.7 . . ? H82A C82 H82B 107.6 . . ? F19 P4 F20 97.7(5) . . ? F19 P4 F22 173.9(5) . . ? F20 P4 F22 88.3(4) . . ? F19 P4 F23 89.1(4) . . ? F20 P4 F23 173.2(4) . . ? F22 P4 F23 84.9(3) . . ? F19 P4 F24 90.5(3) . . ? F20 P4 F24 90.3(2) . . ? F22 P4 F24 90.0(3) . . ? F23 P4 F24 89.4(2) . . ? F19 P4 F21 89.6(3) . . ? F20 P4 F21 90.1(2) . . ? F22 P4 F21 89.8(3) . . ? F23 P4 F21 90.22(19) . . ? F24 P4 F21 179.6(2) . . ? F5 P1 F3 91.49(19) . . ? F5 P1 F4 89.91(19) . . ? F3 P1 F4 178.60(17) . . ? F5 P1 F1 179.13(19) . . ? F3 P1 F1 89.34(15) . . ? F4 P1 F1 89.26(15) . . ? F5 P1 F2 90.98(16) . . ? F3 P1 F2 90.74(14) . . ? F4 P1 F2 89.25(14) . . ? F1 P1 F2 89.26(14) . . ? F5 P1 F6 90.80(16) . . ? F3 P1 F6 89.39(14) . . ? F4 P1 F6 90.58(14) . . ? F1 P1 F6 88.95(14) . . ? F2 P1 F6 178.21(15) . . ? 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 C3 Ag1 Ag2 C67 163.37(12) . . . . ? C1 Ag1 Ag2 C67 -18.77(12) . . . . ? Ag4 Ag1 Ag2 C67 80.06(8) . . . . ? C3 Ag1 Ag2 C69 -14.15(12) . . . . ? C1 Ag1 Ag2 C69 163.71(11) . . . . ? Ag4 Ag1 Ag2 C69 -97.46(8) . . . . ? C3 Ag1 Ag2 Ag3 -97.34(8) . . . . ? C1 Ag1 Ag2 Ag3 80.52(8) . . . . ? Ag4 Ag1 Ag2 Ag3 179.353(9) . . . . ? C68 Ag3 Ag2 C67 -79.38(13) . . . . ? C2 Ag3 Ag2 C67 104.86(12) . . . . ? C68 Ag3 Ag2 C69 85.31(13) . . . . ? C2 Ag3 Ag2 C69 -90.45(12) . . . . ? C68 Ag3 Ag2 Ag1 -175.06(10) . . . . ? C2 Ag3 Ag2 Ag1 9.18(9) . . . . ? C3 Ag1 Ag4 C70 -91.21(12) . . . . ? C1 Ag1 Ag4 C70 103.37(12) . . . . ? Ag2 Ag1 Ag4 C70 9.02(9) . . . . ? C3 Ag1 Ag4 C4 85.84(13) . . . . ? C1 Ag1 Ag4 C4 -79.58(13) . . . . ? Ag2 Ag1 Ag4 C4 -173.93(10) . . . . ? C63 C62 C61 C66 -0.6(5) . . . . ? C63 C62 C61 C14 178.8(3) . . . . ? C66 C65 C64 C63 0.0(5) . . . . ? C87 C88 C89 C91 2.8(6) . . . . ? C91 C85 C86 C87 3.0(5) . . . . ? C84 C85 C86 C87 -179.3(3) . . . . ? C62 C61 C66 C65 0.3(5) . . . . ? C14 C61 C66 C65 -179.0(3) . . . . ? C64 C65 C66 C61 0.0(5) . . . . ? C20 C19 C24 C23 -0.6(5) . . . . ? C17 C19 C24 C23 -179.8(3) . . . . ? C89 C88 C87 C86 -1.3(6) . . . . ? C85 C86 C87 C88 -1.6(6) . . . . ? C24 C19 C20 C21 2.3(6) . . . . ? C17 C19 C20 C21 -178.5(4) . . . . ? C88 C89 C91 C85 -1.3(6) . . . . ? C86 C85 C91 C89 -1.6(5) . . . . ? C84 C85 C91 C89 -179.4(3) . . . . ? C21 C22 C23 C24 2.8(6) . . . . ? C19 C24 C23 C22 -2.0(6) . . . . ? C65 C64 C63 C62 -0.3(5) . . . . ? C61 C62 C63 C64 0.6(5) . . . . ? C23 C22 C21 C20 -1.1(6) . . . . ? C19 C20 C21 C22 -1.6(6) . . . . ? C93 C92 C97 C96 -0.5(5) . . . . ? C83 C92 C97 C96 176.8(3) . . . . ? C97 C92 C93 C94 0.5(5) . . . . ? C83 C92 C93 C94 -176.8(3) . . . . ? C96 C95 C94 C93 -0.3(6) . . . . ? C92 C93 C94 C95 -0.2(6) . . . . ? C92 C97 C96 C95 0.0(5) . . . . ? C94 C95 C96 C97 0.3(6) . . . . ? C129 C128 C133 C132 0.6(5) . . . . ? C81 C128 C133 C132 -178.5(3) . . . . ? C133 C128 C129 C130 0.0(5) . . . . ? C81 C128 C129 C130 179.1(3) . . . . ? C128 C133 C132 C131 -0.3(5) . . . . ? C133 C132 C131 C130 -0.7(6) . . . . ? C128 C129 C130 C131 -1.0(5) . . . . ? C132 C131 C130 C129 1.3(6) . . . . ? C99 C98 C103 C102 -0.3(5) . . . . ? C73 C98 C103 C102 177.8(3) . . . . ? C103 C98 C99 C100 -0.1(5) . . . . ? C73 C98 C99 C100 -178.1(3) . . . . ? C102 C101 C100 C99 -1.0(5) . . . . ? C98 C99 C100 C101 0.8(5) . . . . ? C100 C101 C102 C103 0.6(5) . . . . ? C98 C103 C102 C101 0.1(5) . . . . ? C119 C120 C121 C116 -0.6(5) . . . . ? C117 C116 C121 C120 -0.2(5) . . . . ? C77 C116 C121 C120 177.9(3) . . . . ? C121 C120 C119 C118 1.0(6) . . . . ? C121 C116 C117 C118 0.6(5) . . . . ? C77 C116 C117 C118 -177.6(3) . . . . ? C116 C117 C118 C119 -0.1(5) . . . . ? C120 C119 C118 C117 -0.7(6) . . . . ? C41 C40 C39 C38 0.3(5) . . . . ? C40 C39 C38 C37 -1.1(5) . . . . ? C39 C38 C37 C42 1.2(5) . . . . ? C39 C38 C37 C7 178.4(3) . . . . ? C39 C40 C41 C42 0.5(5) . . . . ? C38 C37 C42 C41 -0.5(5) . . . . ? C7 C37 C42 C41 -177.7(3) . . . . ? C40 C41 C42 C37 -0.4(5) . . . . ? C111 C110 C115 C114 -0.6(5) . . . . ? C76 C110 C115 C114 178.3(3) . . . . ? C115 C110 C111 C112 -0.2(5) . . . . ? C76 C110 C111 C112 -179.1(3) . . . . ? C110 C115 C114 C113 1.0(5) . . . . ? C112 C113 C114 C115 -0.4(6) . . . . ? C29 C30 C25 C26 -0.8(5) . . . . ? C29 C30 C25 C18 177.6(3) . . . . ? C25 C30 C29 C28 1.0(6) . . . . ? C30 C25 C26 C27 0.1(5) . . . . ? C18 C25 C26 C27 -178.4(3) . . . . ? C25 C26 C27 C28 0.5(6) . . . . ? C26 C27 C28 C29 -0.4(6) . . . . ? C30 C29 C28 C27 -0.3(6) . . . . ? C109 C104 C105 C106 1.7(5) . . . . ? C74 C104 C105 C106 178.2(3) . . . . ? C105 C104 C109 C108 -1.2(5) . . . . ? C74 C104 C109 C108 -177.6(3) . . . . ? C104 C109 C108 C107 0.1(6) . . . . ? C109 C108 C107 C106 0.5(6) . . . . ? C108 C107 C106 C105 0.0(6) . . . . ? C104 C105 C106 C107 -1.1(6) . . . . ? C123 C122 C127 C126 0.1(5) . . . . ? C80 C122 C127 C126 178.1(3) . . . . ? C122 C127 C126 C125 -1.3(5) . . . . ? C127 C122 C123 C124 0.5(5) . . . . ? C80 C122 C123 C124 -177.4(3) . . . . ? C127 C126 C125 C124 1.8(5) . . . . ? C126 C125 C124 C123 -1.2(5) . . . . ? C122 C123 C124 C125 0.0(5) . . . . ? C35 C36 C31 C32 -0.5(5) . . . . ? C35 C36 C31 C6 178.2(3) . . . . ? C33 C32 C31 C36 1.7(5) . . . . ? C33 C32 C31 C6 -177.0(3) . . . . ? C31 C32 C33 C34 -1.9(5) . . . . ? C35 C34 C33 C32 1.1(6) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C31 C36 C35 C34 -0.3(6) . . . . ? C44 C43 C48 C47 0.0(5) . . . . ? C10 C43 C48 C47 -177.0(3) . . . . ? C46 C45 C44 C43 1.0(5) . . . . ? C48 C43 C44 C45 -1.2(5) . . . . ? C10 C43 C44 C45 175.7(3) . . . . ? C44 C45 C46 C47 0.5(6) . . . . ? C45 C46 C47 C48 -1.7(6) . . . . ? C43 C48 C47 C46 1.5(6) . . . . ? C114 C113 C112 C111 -0.5(6) . . . . ? C110 C111 C112 C113 0.8(6) . . . . ? C56 C55 C60 C59 0.6(5) . . . . ? C13 C55 C60 C59 175.9(3) . . . . ? C55 C60 C59 C58 -0.4(6) . . . . ? C60 C59 C58 C57 0.0(6) . . . . ? C56 C57 C58 C59 0.1(6) . . . . ? C58 C57 C56 C55 0.1(6) . . . . ? C60 C55 C56 C57 -0.5(5) . . . . ? C13 C55 C56 C57 -175.7(3) . . . . ? C60 C55 C13 C14 -62.1(5) . . . . ? C56 C55 C13 C14 113.1(4) . . . . ? C60 C55 C13 N7 121.9(3) . . . . ? C56 C55 C13 N7 -62.9(4) . . . . ? N7 C13 C14 N8 0.1(3) . . . . ? C55 C13 C14 N8 -176.5(3) . . . . ? N7 C13 C14 C61 172.1(3) . . . . ? C55 C13 C14 C61 -4.4(5) . . . . ? C66 C61 C14 C13 126.6(4) . . . . ? C62 C61 C14 C13 -52.8(5) . . . . ? C66 C61 C14 N8 -62.9(4) . . . . ? C62 C61 C14 N8 117.7(3) . . . . ? C70 Ag4 C4 N8 119.6(10) . . . . ? Ag1 Ag4 C4 N8 95.9(3) . . . . ? C70 Ag4 C4 N7 -58.1(11) . . . . ? Ag1 Ag4 C4 N7 -81.9(3) . . . . ? N7 C4 N8 C14 0.0(3) . . . . ? Ag4 C4 N8 C14 -178.3(2) . . . . ? N7 C4 N8 C15 -177.0(2) . . . . ? Ag4 C4 N8 C15 4.8(4) . . . . ? C13 C14 N8 C4 0.0(3) . . . . ? C61 C14 N8 C4 -172.3(3) . . . . ? C13 C14 N8 C15 176.8(3) . . . . ? C61 C14 N8 C15 4.5(5) . . . . ? N8 C4 N7 C13 0.1(3) . . . . ? Ag4 C4 N7 C13 178.2(2) . . . . ? N8 C4 N7 C12 178.1(2) . . . . ? Ag4 C4 N7 C12 -3.8(4) . . . . ? C14 C13 N7 C4 -0.1(3) . . . . ? C55 C13 N7 C4 176.6(3) . . . . ? C14 C13 N7 C12 -178.0(3) . . . . ? C55 C13 N7 C12 -1.3(5) . . . . ? C11 N6 C3 N5 0.0(3) . . . . ? C12 N6 C3 N5 -163.7(3) . . . . ? C11 N6 C3 Ag1 -165.8(2) . . . . ? C12 N6 C3 Ag1 30.5(4) . . . . ? C10 N5 C3 N6 -0.4(3) . . . . ? C9 N5 C3 N6 -178.8(3) . . . . ? C10 N5 C3 Ag1 165.0(2) . . . . ? C9 N5 C3 Ag1 -13.4(4) . . . . ? C1 Ag1 C3 N6 61.0(5) . . . . ? Ag2 Ag1 C3 N6 -126.1(2) . . . . ? Ag4 Ag1 C3 N6 -62.9(3) . . . . ? C1 Ag1 C3 N5 -101.3(4) . . . . ? Ag2 Ag1 C3 N5 71.5(3) . . . . ? Ag4 Ag1 C3 N5 134.8(3) . . . . ? C3 N6 C11 C10 0.4(3) . . . . ? C12 N6 C11 C10 165.1(3) . . . . ? C3 N6 C11 C49 178.7(3) . . . . ? C12 N6 C11 C49 -16.6(4) . . . . ? C10 C11 C49 C54 100.9(4) . . . . ? N6 C11 C49 C54 -76.9(4) . . . . ? C10 C11 C49 C50 -80.3(5) . . . . ? N6 C11 C49 C50 101.8(4) . . . . ? N6 C11 C10 N5 -0.6(3) . . . . ? C49 C11 C10 N5 -178.8(3) . . . . ? N6 C11 C10 C43 174.0(3) . . . . ? C49 C11 C10 C43 -4.2(6) . . . . ? C3 N5 C10 C11 0.7(3) . . . . ? C9 N5 C10 C11 179.1(3) . . . . ? C3 N5 C10 C43 -174.5(3) . . . . ? C9 N5 C10 C43 3.9(4) . . . . ? C48 C43 C10 C11 -55.4(5) . . . . ? C44 C43 C10 C11 127.6(4) . . . . ? C48 C43 C10 N5 118.5(3) . . . . ? C44 C43 C10 N5 -58.5(4) . . . . ? C50 C49 C54 C53 0.4(5) . . . . ? C11 C49 C54 C53 179.2(3) . . . . ? C54 C49 C50 C51 -1.6(5) . . . . ? C11 C49 C50 C51 179.7(3) . . . . ? C49 C50 C51 C52 1.4(6) . . . . ? C49 C54 C53 C52 1.0(6) . . . . ? C50 C51 C52 C53 -0.1(6) . . . . ? C54 C53 C52 C51 -1.1(6) . . . . ? C4 N7 C12 N6 93.9(3) . . . . ? C13 N7 C12 N6 -88.3(3) . . . . ? C3 N6 C12 N7 -44.6(4) . . . . ? C11 N6 C12 N7 152.8(3) . . . . ? C4 N8 C15 C16 -65.5(4) . . . . ? C14 N8 C15 C16 118.0(3) . . . . ? N1 C16 C15 N8 -60.5(4) . . . . ? C20 C19 C17 C18 -136.5(4) . . . . ? C24 C19 C17 C18 42.7(5) . . . . ? C20 C19 C17 N1 48.3(5) . . . . ? C24 C19 C17 N1 -132.5(3) . . . . ? N1 C17 C18 N2 0.4(3) . . . . ? C19 C17 C18 N2 -175.5(3) . . . . ? N1 C17 C18 C25 -178.2(3) . . . . ? C19 C17 C18 C25 5.8(6) . . . . ? C26 C25 C18 C17 63.1(5) . . . . ? C30 C25 C18 C17 -115.4(4) . . . . ? C26 C25 C18 N2 -115.3(3) . . . . ? C30 C25 C18 N2 66.2(4) . . . . ? C3 Ag1 C1 N2 60.2(5) . . . . ? Ag2 Ag1 C1 N2 -112.6(2) . . . . ? Ag4 Ag1 C1 N2 -177.7(2) . . . . ? C3 Ag1 C1 N1 -110.3(4) . . . . ? Ag2 Ag1 C1 N1 76.8(3) . . . . ? Ag4 Ag1 C1 N1 11.8(3) . . . . ? N1 C1 N2 C18 -0.5(3) . . . . ? Ag1 C1 N2 C18 -173.0(2) . . . . ? N1 C1 N2 C5 -177.0(3) . . . . ? Ag1 C1 N2 C5 10.6(4) . . . . ? C17 C18 N2 C1 0.1(3) . . . . ? C25 C18 N2 C1 178.8(3) . . . . ? C17 C18 N2 C5 176.8(3) . . . . ? C25 C18 N2 C5 -4.5(4) . . . . ? N2 C1 N1 C17 0.8(3) . . . . ? Ag1 C1 N1 C17 173.0(2) . . . . ? N2 C1 N1 C16 177.9(3) . . . . ? Ag1 C1 N1 C16 -9.8(4) . . . . ? C18 C17 N1 C1 -0.8(3) . . . . ? C19 C17 N1 C1 175.4(3) . . . . ? C18 C17 N1 C16 -177.9(3) . . . . ? C19 C17 N1 C16 -1.8(5) . . . . ? C15 C16 N1 C1 89.9(3) . . . . ? C15 C16 N1 C17 -93.3(3) . . . . ? C1 N2 C5 N3 -26.6(4) . . . . ? C18 N2 C5 N3 157.2(3) . . . . ? C86 C85 C84 C83 -128.2(4) . . . . ? C91 C85 C84 C83 49.5(5) . . . . ? C86 C85 C84 N10 57.3(5) . . . . ? C91 C85 C84 N10 -125.0(3) . . . . ? N10 C84 C83 N9 0.2(3) . . . . ? C85 C84 C83 N9 -175.1(3) . . . . ? N10 C84 C83 C92 -177.9(3) . . . . ? C85 C84 C83 C92 6.8(6) . . . . ? C97 C92 C83 C84 -116.0(4) . . . . ? C93 C92 C83 C84 61.2(5) . . . . ? C97 C92 C83 N9 66.2(4) . . . . ? C93 C92 C83 N9 -116.5(4) . . . . ? C69 Ag2 C67 N9 59.3(5) . . . . ? Ag1 Ag2 C67 N9 -112.8(3) . . . . ? Ag3 Ag2 C67 N9 -178.4(2) . . . . ? C69 Ag2 C67 N10 -110.6(4) . . . . ? Ag1 Ag2 C67 N10 77.3(3) . . . . ? Ag3 Ag2 C67 N10 11.7(3) . . . . ? N9 C67 N10 C84 1.1(3) . . . . ? Ag2 C67 N10 C84 172.9(2) . . . . ? N9 C67 N10 C71 177.0(3) . . . . ? Ag2 C67 N10 C71 -11.2(4) . . . . ? C83 C84 N10 C67 -0.8(3) . . . . ? C85 C84 N10 C67 174.7(3) . . . . ? C83 C84 N10 C71 -176.7(3) . . . . ? C85 C84 N10 C71 -1.2(5) . . . . ? N10 C67 N9 C83 -1.0(3) . . . . ? Ag2 C67 N9 C83 -172.7(2) . . . . ? N10 C67 N9 C82 -174.4(3) . . . . ? Ag2 C67 N9 C82 13.9(4) . . . . ? C84 C83 N9 C67 0.5(3) . . . . ? C92 C83 N9 C67 178.7(3) . . . . ? C84 C83 N9 C82 174.5(3) . . . . ? C92 C83 N9 C82 -7.3(4) . . . . ? C105 C104 C74 C73 -62.2(5) . . . . ? C109 C104 C74 C73 114.2(4) . . . . ? C105 C104 C74 N12 120.1(3) . . . . ? C109 C104 C74 N12 -63.5(4) . . . . ? N12 C74 C73 N11 0.0(3) . . . . ? C104 C74 C73 N11 -178.0(3) . . . . ? N12 C74 C73 C98 173.8(3) . . . . ? C104 C74 C73 C98 -4.2(5) . . . . ? C99 C98 C73 C74 123.3(4) . . . . ? C103 C98 C73 C74 -54.7(5) . . . . ? C99 C98 C73 N11 -63.9(4) . . . . ? C103 C98 C73 N11 118.0(3) . . . . ? C2 Ag3 C68 N11 119.1(7) . . . . ? Ag2 Ag3 C68 N11 95.9(3) . . . . ? C2 Ag3 C68 N12 -60.8(8) . . . . ? Ag2 Ag3 C68 N12 -84.0(3) . . . . ? N11 C68 N12 C74 0.7(3) . . . . ? Ag3 C68 N12 C74 -179.4(2) . . . . ? N11 C68 N12 C75 180.0(3) . . . . ? Ag3 C68 N12 C75 -0.1(4) . . . . ? C73 C74 N12 C68 -0.4(3) . . . . ? C104 C74 N12 C68 177.7(3) . . . . ? C73 C74 N12 C75 -179.7(3) . . . . ? C104 C74 N12 C75 -1.6(5) . . . . ? N12 C68 N11 C73 -0.7(3) . . . . ? Ag3 C68 N11 C73 179.4(2) . . . . ? N12 C68 N11 C72 -176.6(2) . . . . ? Ag3 C68 N11 C72 3.5(4) . . . . ? C74 C73 N11 C68 0.4(3) . . . . ? C98 C73 N11 C68 -173.7(3) . . . . ? C74 C73 N11 C72 176.1(3) . . . . ? C98 C73 N11 C72 2.0(5) . . . . ? C67 N10 C71 C72 92.4(3) . . . . ? C84 N10 C71 C72 -92.2(3) . . . . ? C68 N11 C72 C71 -65.2(4) . . . . ? C73 N11 C72 C71 119.5(3) . . . . ? N10 C71 C72 N11 -61.8(3) . . . . ? C68 N12 C75 N13 92.9(3) . . . . ? C74 N12 C75 N13 -87.9(3) . . . . ? C117 C116 C77 C76 -62.7(5) . . . . ? C121 C116 C77 C76 119.1(4) . . . . ? C117 C116 C77 N14 110.4(4) . . . . ? C121 C116 C77 N14 -67.8(4) . . . . ? N14 C77 C76 N13 0.5(3) . . . . ? C116 C77 C76 N13 174.5(3) . . . . ? N14 C77 C76 C110 -175.8(3) . . . . ? C116 C77 C76 C110 -1.8(6) . . . . ? C115 C110 C76 C77 -86.8(4) . . . . ? C111 C110 C76 C77 92.1(4) . . . . ? C115 C110 C76 N13 97.5(4) . . . . ? C111 C110 C76 N13 -83.6(4) . . . . ? C67 Ag2 C69 N13 61.5(5) . . . . ? Ag1 Ag2 C69 N13 -126.4(2) . . . . ? Ag3 Ag2 C69 N13 -63.0(2) . . . . ? C67 Ag2 C69 N14 -99.1(4) . . . . ? Ag1 Ag2 C69 N14 73.0(3) . . . . ? Ag3 Ag2 C69 N14 136.4(3) . . . . ? N14 C69 N13 C76 1.2(3) . . . . ? Ag2 C69 N13 C76 -163.2(2) . . . . ? N14 C69 N13 C75 -163.6(3) . . . . ? Ag2 C69 N13 C75 32.0(4) . . . . ? C77 C76 N13 C69 -1.1(3) . . . . ? C110 C76 N13 C69 175.5(3) . . . . ? C77 C76 N13 C75 164.6(3) . . . . ? C110 C76 N13 C75 -18.8(4) . . . . ? N12 C75 N13 C69 -46.0(4) . . . . ? N12 C75 N13 C76 150.3(3) . . . . ? N13 C69 N14 C77 -0.9(3) . . . . ? Ag2 C69 N14 C77 163.2(2) . . . . ? N13 C69 N14 C78 -179.9(3) . . . . ? Ag2 C69 N14 C78 -15.9(4) . . . . ? C76 C77 N14 C69 0.2(3) . . . . ? C116 C77 N14 C69 -174.3(3) . . . . ? C76 C77 N14 C78 179.3(3) . . . . ? C116 C77 N14 C78 4.8(4) . . . . ? C69 N14 C78 C79 99.9(3) . . . . ? C77 N14 C78 C79 -79.1(3) . . . . ? N14 C78 C79 N15 -63.6(3) . . . . ? C78 C79 N15 C70 -63.3(4) . . . . ? C78 C79 N15 C80 113.6(3) . . . . ? C70 N15 C80 C81 0.1(3) . . . . ? C79 N15 C80 C81 -177.0(3) . . . . ? C70 N15 C80 C122 -178.2(3) . . . . ? C79 N15 C80 C122 4.6(5) . . . . ? C123 C122 C80 C81 53.9(5) . . . . ? C127 C122 C80 C81 -124.0(4) . . . . ? C123 C122 C80 N15 -128.2(3) . . . . ? C127 C122 C80 N15 53.9(4) . . . . ? N15 C80 C81 N16 0.5(3) . . . . ? C122 C80 C81 N16 178.7(3) . . . . ? N15 C80 C81 C128 -175.0(3) . . . . ? C122 C80 C81 C128 3.2(6) . . . . ? C133 C128 C81 C80 -133.0(4) . . . . ? C129 C128 C81 C80 47.9(5) . . . . ? C133 C128 C81 N16 52.2(4) . . . . ? C129 C128 C81 N16 -126.9(3) . . . . ? C36 C31 C6 C7 43.7(5) . . . . ? C32 C31 C6 C7 -137.6(4) . . . . ? C36 C31 C6 N3 -130.2(3) . . . . ? C32 C31 C6 N3 48.5(4) . . . . ? N3 C6 C7 N4 0.8(3) . . . . ? C31 C6 C7 N4 -174.0(3) . . . . ? N3 C6 C7 C37 177.9(3) . . . . ? C31 C6 C7 C37 3.1(6) . . . . ? C42 C37 C7 C6 59.9(5) . . . . ? C38 C37 C7 C6 -117.4(4) . . . . ? C42 C37 C7 N4 -123.4(3) . . . . ? C38 C37 C7 N4 59.4(4) . . . . ? C3 N5 C9 C8 97.6(3) . . . . ? C10 N5 C9 C8 -80.6(3) . . . . ? N5 C9 C8 N4 -62.7(3) . . . . ? C6 C7 N4 C2 -0.8(3) . . . . ? C37 C7 N4 C2 -178.2(3) . . . . ? C6 C7 N4 C8 -176.0(3) . . . . ? C37 C7 N4 C8 6.5(5) . . . . ? C9 C8 N4 C2 -63.8(4) . . . . ? C9 C8 N4 C7 111.0(3) . . . . ? C7 C6 N3 C2 -0.5(3) . . . . ? C31 C6 N3 C2 174.7(3) . . . . ? C7 C6 N3 C5 -170.5(3) . . . . ? C31 C6 N3 C5 4.7(5) . . . . ? N2 C5 N3 C2 96.3(3) . . . . ? N2 C5 N3 C6 -94.5(3) . . . . ? C80 C81 N16 C70 -0.9(3) . . . . ? C128 C81 N16 C70 175.0(3) . . . . ? C80 C81 N16 C82 -172.8(3) . . . . ? C128 C81 N16 C82 3.0(5) . . . . ? C7 N4 C2 N3 0.5(3) . . . . ? C8 N4 C2 N3 176.0(2) . . . . ? C7 N4 C2 Ag3 -174.7(2) . . . . ? C8 N4 C2 Ag3 0.8(4) . . . . ? C6 N3 C2 N4 0.0(3) . . . . ? C5 N3 C2 N4 170.6(2) . . . . ? C6 N3 C2 Ag3 174.9(2) . . . . ? C5 N3 C2 Ag3 -14.5(4) . . . . ? C68 Ag3 C2 N4 68.7(8) . . . . ? Ag2 Ag3 C2 N4 90.0(3) . . . . ? C68 Ag3 C2 N3 -105.2(7) . . . . ? Ag2 Ag3 C2 N3 -83.9(3) . . . . ? C80 N15 C70 N16 -0.7(3) . . . . ? C79 N15 C70 N16 176.6(2) . . . . ? C80 N15 C70 Ag4 -175.4(2) . . . . ? C79 N15 C70 Ag4 2.0(4) . . . . ? C81 N16 C70 N15 1.0(3) . . . . ? C82 N16 C70 N15 173.4(2) . . . . ? C81 N16 C70 Ag4 175.2(2) . . . . ? C82 N16 C70 Ag4 -12.4(4) . . . . ? C4 Ag4 C70 N15 66.5(11) . . . . ? Ag1 Ag4 C70 N15 88.8(3) . . . . ? C4 Ag4 C70 N16 -106.6(10) . . . . ? Ag1 Ag4 C70 N16 -84.3(3) . . . . ? C70 N16 C82 N9 94.5(3) . . . . ? C81 N16 C82 N9 -94.3(3) . . . . ? C67 N9 C82 N16 -29.7(4) . . . . ? C83 N9 C82 N16 157.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.827 _refine_diff_density_min -1.584 _refine_diff_density_rms 0.105 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 -0.002 -0.002 1943 575 ' ' 2 0.000 1.000 0.500 224 62 ' ' _platon_squeeze_details ; ; data_4 _database_code_depnum_ccdc_archive 'CCDC 882740' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 F6 N8 O6 Pt S2' _chemical_formula_weight 1450.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.295(3) _cell_length_b 8.8080(10) _cell_length_c 29.743(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.6370(10) _cell_angle_gamma 90.00 _cell_volume 7346.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.32 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 2.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8877 _exptl_absorpt_correction_T_max 0.9231 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD Detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74568 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.36 _reflns_number_total 14944 _reflns_number_gt 11053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains four disordered solvent molecules CH2Cl2, which were SQUEEZED out with the SQUEEZE routine in Platon software package. ; _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^)+(0.0585P)^2^+105.6052P] 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 14944 _refine_ls_number_parameters 778 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1794 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.077 _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 Pt1 Pt 0.250705(12) 0.04616(4) 0.374630(10) 0.01715(10) Uani 1 1 d . . . S2 S 0.18918(11) 0.6489(3) 0.46915(10) 0.0424(7) Uani 1 1 d . . . S1 S 0.31310(10) 0.6825(3) 0.27659(8) 0.0313(5) Uani 1 1 d . . . C1 C 0.2174(3) 0.0429(10) 0.3100(3) 0.0227(18) Uani 1 1 d . . . C4 C 0.3153(3) 0.0508(10) 0.3546(3) 0.0205(17) Uani 1 1 d . . . C3 C 0.2848(3) 0.0241(10) 0.4390(3) 0.0172(16) Uani 1 1 d . . . C2 C 0.1863(3) 0.0403(10) 0.3949(2) 0.0187(16) Uani 1 1 d . . . C7 C 0.1084(3) -0.0190(9) 0.3962(3) 0.0180(17) Uani 1 1 d U . . C5 C 0.1884(3) 0.0618(9) 0.2356(3) 0.0206(17) Uani 1 1 d U . . C12 C 0.3806(3) 0.1083(10) 0.3222(3) 0.0210(18) Uani 1 1 d U . . C8 C 0.1208(3) 0.0815(10) 0.4295(3) 0.0218(18) Uani 1 1 d U . . C11 C 0.3929(3) -0.0029(8) 0.3528(3) 0.0144(16) Uani 1 1 d U . . C9 C 0.3109(3) 0.0083(9) 0.5138(3) 0.0192(18) Uani 1 1 d U . . C10 C 0.3444(3) -0.0580(9) 0.4924(3) 0.0197(17) Uani 1 1 d U . . C6 C 0.1547(3) -0.0059(8) 0.2560(3) 0.0147(16) Uani 1 1 d U . . C14 C 0.1997(3) 0.2160(10) 0.4574(3) 0.0211(9) Uani 1 1 d . . . H14A H 0.1796 0.2887 0.4717 0.025 Uiso 1 1 calc R . . H14B H 0.2196 0.2753 0.4388 0.025 Uiso 1 1 calc R . . C13 C 0.1544(3) -0.1229(10) 0.3331(3) 0.0189(17) Uani 1 1 d . . . H13A H 0.1232 -0.1640 0.3195 0.023 Uiso 1 1 calc R . . H13B H 0.1768 -0.2089 0.3396 0.023 Uiso 1 1 calc R . . C15 C 0.2317(3) 0.1371(10) 0.4939(3) 0.0211(9) Uani 1 1 d . . . H15A H 0.2428 0.2129 0.5175 0.025 Uiso 1 1 calc R . . H15B H 0.2125 0.0612 0.5080 0.025 Uiso 1 1 calc R . . C18 C 0.2711(3) 0.1651(10) 0.2574(3) 0.0211(9) Uani 1 1 d . . . H18A H 0.2627 0.2388 0.2325 0.025 Uiso 1 1 calc R . . H18B H 0.2905 0.0842 0.2458 0.025 Uiso 1 1 calc R . . C17 C 0.3016(3) 0.2464(9) 0.2965(3) 0.0211(9) Uani 1 1 d . . . H17A H 0.3214 0.3246 0.2840 0.025 Uiso 1 1 calc R . . H17B H 0.2805 0.2984 0.3156 0.025 Uiso 1 1 calc R . . C16 C 0.3459(3) -0.1362(10) 0.4096(3) 0.0223(18) Uani 1 1 d . . . H16A H 0.3767 -0.1843 0.4213 0.027 Uiso 1 1 calc R . . H16B H 0.3231 -0.2169 0.3982 0.027 Uiso 1 1 calc R . . C25 C 0.1071(3) -0.0679(9) 0.2373(3) 0.0197(17) Uani 1 1 d . . . C20 C 0.2191(3) 0.0461(11) 0.1601(3) 0.0287(19) Uani 1 1 d . . . H20 H 0.2445 -0.0172 0.1732 0.034 Uiso 1 1 calc R . . C24 C 0.1520(3) 0.2018(11) 0.1676(3) 0.0264(19) Uani 1 1 d . . . H24 H 0.1304 0.2459 0.1858 0.032 Uiso 1 1 calc R . . C30 C 0.0673(3) -0.0204(11) 0.2575(3) 0.029(2) Uani 1 1 d . . . H30 H 0.0706 0.0505 0.2818 0.034 Uiso 1 1 calc R . . C19 C 0.1873(3) 0.1040(10) 0.1869(3) 0.0228(18) Uani 1 1 d . . . C26 C 0.1019(3) -0.1681(10) 0.2012(3) 0.0222(18) Uani 1 1 d . . . H26 H 0.1290 -0.1986 0.1878 0.027 Uiso 1 1 calc R . . C21 C 0.2146(4) 0.0790(11) 0.1144(3) 0.030(2) Uani 1 1 d . . . H21 H 0.2361 0.0351 0.0961 0.037 Uiso 1 1 calc R . . C28 C 0.0180(4) -0.1805(14) 0.2043(3) 0.043(3) Uani 1 1 d . . . H28 H -0.0126 -0.2190 0.1930 0.052 Uiso 1 1 calc R . . C29 C 0.0225(3) -0.0810(12) 0.2407(3) 0.034(2) Uani 1 1 d . . . H29 H -0.0049 -0.0537 0.2544 0.041 Uiso 1 1 calc R . . C22 C 0.1791(4) 0.1751(12) 0.0948(3) 0.036(2) Uani 1 1 d . . . H22 H 0.1764 0.1986 0.0634 0.043 Uiso 1 1 calc R . . C27 C 0.0567(4) -0.2247(11) 0.1843(3) 0.031(2) Uani 1 1 d . . . H27 H 0.0530 -0.2928 0.1593 0.037 Uiso 1 1 calc R . . C23 C 0.1481(4) 0.2358(11) 0.1210(3) 0.034(2) Uani 1 1 d . . . H23 H 0.1236 0.3018 0.1078 0.041 Uiso 1 1 calc R . . C38 C 0.0750(4) 0.0582(12) 0.4939(3) 0.032(2) Uani 1 1 d . . . H38 H 0.0810 -0.0479 0.4941 0.039 Uiso 1 1 calc R . . C36 C 0.0205(3) -0.0362(10) 0.3734(3) 0.0237(18) Uani 1 1 d . . . H36 H 0.0180 0.0705 0.3772 0.028 Uiso 1 1 calc R . . C42 C 0.0851(4) 0.3040(13) 0.4636(4) 0.037(3) Uani 1 1 d . . . H42 H 0.0985 0.3689 0.4431 0.044 Uiso 1 1 calc R . . C31 C 0.0644(3) -0.1068(10) 0.3821(2) 0.0185(17) Uani 1 1 d . . . C37 C 0.0936(3) 0.1451(11) 0.4633(3) 0.0230(19) Uani 1 1 d . . . C32 C 0.0664(4) -0.2654(10) 0.3775(3) 0.022(2) Uani 1 1 d . . . H32 H 0.0961 -0.3163 0.3839 0.026 Uiso 1 1 calc R . . C34 C -0.0168(4) -0.2798(12) 0.3538(3) 0.033(2) Uani 1 1 d . . . H34 H -0.0442 -0.3384 0.3432 0.039 Uiso 1 1 calc R . . C33 C 0.0260(3) -0.3473(10) 0.3639(3) 0.0261(19) Uani 1 1 d . . . H33 H 0.0282 -0.4545 0.3615 0.031 Uiso 1 1 calc R . . C40 C 0.0391(4) 0.2655(10) 0.5248(3) 0.029(2) Uani 1 1 d . . . H40 H 0.0200 0.3046 0.5462 0.034 Uiso 1 1 calc R . . C35 C -0.0206(3) -0.1233(13) 0.3590(3) 0.031(2) Uani 1 1 d . . . H35 H -0.0508 -0.0751 0.3528 0.038 Uiso 1 1 calc R . . C41 C 0.0567(4) 0.3642(13) 0.4947(4) 0.040(3) Uani 1 1 d . . . H41 H 0.0498 0.4697 0.4951 0.048 Uiso 1 1 calc R . . C39 C 0.0483(4) 0.1154(11) 0.5245(3) 0.029(2) Uani 1 1 d . . . H39 H 0.0360 0.0500 0.5455 0.035 Uiso 1 1 calc R . . C43 C 0.3120(3) 0.0428(12) 0.5627(3) 0.029(2) Uani 1 1 d . . . C49 C 0.3885(3) -0.1352(10) 0.5096(3) 0.0232(18) Uani 1 1 d . . . C54 C 0.4308(3) -0.1081(11) 0.4924(3) 0.028(2) Uani 1 1 d . . . H54 H 0.4323 -0.0307 0.4704 0.034 Uiso 1 1 calc R . . C45 C 0.2795(5) 0.0212(12) 0.6341(3) 0.041(3) Uani 1 1 d . . . H45 H 0.2564 -0.0197 0.6511 0.049 Uiso 1 1 calc R . . C52 C 0.4707(4) -0.3009(12) 0.5397(3) 0.038(3) Uani 1 1 d . . . H52 H 0.4987 -0.3580 0.5496 0.046 Uiso 1 1 calc R . . C51 C 0.4288(4) -0.3280(12) 0.5590(3) 0.037(2) Uani 1 1 d . . . H51 H 0.4287 -0.4008 0.5825 0.044 Uiso 1 1 calc R . . C53 C 0.4716(3) -0.1949(12) 0.5074(3) 0.033(2) Uani 1 1 d . . . H53 H 0.5001 -0.1784 0.4945 0.039 Uiso 1 1 calc R . . C48 C 0.3488(4) 0.1288(13) 0.5847(3) 0.037(2) Uani 1 1 d . . . H48 H 0.3728 0.1662 0.5680 0.044 Uiso 1 1 calc R . . C44 C 0.2770(4) -0.0067(11) 0.5875(3) 0.030(2) Uani 1 1 d . . . H44 H 0.2505 -0.0614 0.5725 0.036 Uiso 1 1 calc R . . C46 C 0.3172(4) 0.1118(15) 0.6550(3) 0.053(4) Uani 1 1 d . . . H46 H 0.3184 0.1379 0.6862 0.063 Uiso 1 1 calc R . . C50 C 0.3884(4) -0.2490(9) 0.5437(3) 0.027(2) Uani 1 1 d . . . H50 H 0.3598 -0.2702 0.5559 0.032 Uiso 1 1 calc R . . C47 C 0.3518(4) 0.1622(15) 0.6311(4) 0.053(4) Uani 1 1 d . . . H47 H 0.3779 0.2196 0.6458 0.064 Uiso 1 1 calc R . . C60 C 0.4796(3) -0.0014(9) 0.3799(3) 0.0215(18) Uani 1 1 d . . . H60 H 0.4792 0.1064 0.3806 0.026 Uiso 1 1 calc R . . C62 C 0.4281(3) 0.0938(11) 0.2580(3) 0.027(2) Uani 1 1 d . . . H62 H 0.4230 -0.0128 0.2566 0.033 Uiso 1 1 calc R . . C61 C 0.4095(3) 0.1827(10) 0.2902(3) 0.0207(19) Uani 1 1 d . . . C57 C 0.4821(4) -0.3136(12) 0.3784(3) 0.036(2) Uani 1 1 d . . . H57 H 0.4824 -0.4215 0.3781 0.043 Uiso 1 1 calc R . . C55 C 0.4381(3) -0.0837(9) 0.3656(3) 0.0208(18) Uani 1 1 d . . . C66 C 0.4166(3) 0.3370(12) 0.2910(3) 0.028(2) Uani 1 1 d . . . H66 H 0.4040 0.3971 0.3132 0.034 Uiso 1 1 calc R . . C56 C 0.4389(4) -0.2440(12) 0.3638(3) 0.033(3) Uani 1 1 d . . . H56 H 0.4112 -0.3011 0.3531 0.039 Uiso 1 1 calc R . . C65 C 0.4418(3) 0.4054(12) 0.2599(3) 0.034(2) Uani 1 1 d . . . H65 H 0.4460 0.5124 0.2604 0.040 Uiso 1 1 calc R . . C64 C 0.4609(3) 0.3205(10) 0.2281(3) 0.0234(14) Uani 1 1 d . . . H64 H 0.4781 0.3683 0.2067 0.028 Uiso 1 1 calc R . . C58 C 0.5236(4) -0.2439(9) 0.3930(3) 0.0234(14) Uani 1 1 d . . . H58 H 0.5520 -0.2994 0.4023 0.028 Uiso 1 1 calc R . . C63 C 0.4550(3) 0.1679(10) 0.2275(3) 0.0248(19) Uani 1 1 d . . . H63 H 0.4692 0.1091 0.2061 0.030 Uiso 1 1 calc R . . C59 C 0.5227(3) -0.0835(11) 0.3936(3) 0.030(2) Uani 1 1 d . . . H59 H 0.5512 -0.0293 0.4032 0.036 Uiso 1 1 calc R . . C68 C 0.2496(3) 0.6189(9) 0.4928(3) 0.0193(17) Uani 1 1 d . . . C67 C 0.2497(3) 0.6564(9) 0.2539(3) 0.0221(18) Uani 1 1 d . . . N7 N 0.3524(2) -0.0305(9) 0.3731(2) 0.0236(16) Uani 1 1 d . . . N3 N 0.1493(2) -0.0439(9) 0.3746(2) 0.0206(14) Uani 1 1 d . . . N2 N 0.1727(2) -0.0166(7) 0.3011(2) 0.0161(14) Uani 1 1 d . . . N6 N 0.3273(2) -0.0480(9) 0.4461(2) 0.0232(15) Uani 1 1 d . . . N5 N 0.2745(2) 0.0584(8) 0.4811(2) 0.0176(7) Uani 1 1 d . . . N4 N 0.1692(2) 0.1172(8) 0.4280(2) 0.0176(7) Uani 1 1 d . . . N8 N 0.3325(2) 0.1407(8) 0.3244(2) 0.0176(7) Uani 1 1 d . . . N1 N 0.2270(2) 0.0972(8) 0.2689(2) 0.0176(7) Uani 1 1 d . . . F4 F 0.2621(3) 0.4698(6) 0.4921(3) 0.058(2) Uani 1 1 d . . . F1 F 0.2400(2) 0.5021(5) 0.2531(2) 0.0337(13) Uani 1 1 d . . . F5 F 0.2805(3) 0.6826(8) 0.4645(2) 0.0566(18) Uani 1 1 d . . . F2 F 0.2401(3) 0.7084(8) 0.2130(2) 0.0552(18) Uani 1 1 d . . . F3 F 0.2219(2) 0.7172(7) 0.2796(3) 0.0530(18) Uani 1 1 d . . . F6 F 0.2626(3) 0.6742(10) 0.5319(3) 0.079(3) Uani 1 1 d . . . O5 O 0.1834(4) 0.8171(13) 0.4762(4) 0.085(3) Uani 1 1 d . . . O1 O 0.3372(3) 0.5828(8) 0.2503(2) 0.0402(18) Uani 1 1 d . . . O6 O 0.1646(3) 0.5533(10) 0.4971(3) 0.058(2) Uani 1 1 d . . . O4 O 0.1858(3) 0.6083(11) 0.4229(3) 0.064(3) Uani 1 1 d . . . O2 O 0.3158(3) 0.6353(10) 0.3233(2) 0.051(2) Uani 1 1 d . . . O3 O 0.3196(3) 0.8343(7) 0.2696(2) 0.0355(16) 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 Pt1 0.01854(16) 0.02319(16) 0.00951(14) 0.00109(14) 0.00110(10) 0.00069(15) S2 0.0545(18) 0.0306(14) 0.0440(15) 0.0008(12) 0.0136(13) 0.0032(13) S1 0.0434(15) 0.0198(12) 0.0306(12) 0.0027(9) 0.0051(11) -0.0023(10) C1 0.026(4) 0.026(4) 0.016(4) 0.002(4) 0.004(3) 0.017(4) C4 0.025(4) 0.023(4) 0.014(4) -0.003(3) 0.002(3) -0.001(4) C3 0.012(4) 0.025(4) 0.013(4) 0.000(3) -0.002(3) -0.001(3) C2 0.024(4) 0.022(4) 0.011(3) 0.009(3) 0.003(3) 0.010(4) C7 0.025(4) 0.015(4) 0.015(4) 0.010(3) 0.004(3) 0.003(3) C5 0.026(4) 0.017(4) 0.018(4) 0.006(3) -0.002(3) 0.004(3) C12 0.018(4) 0.032(5) 0.012(4) 0.009(3) 0.001(3) 0.001(4) C8 0.018(4) 0.029(5) 0.018(4) 0.001(3) 0.000(3) 0.004(3) C11 0.016(4) 0.012(4) 0.015(4) 0.004(3) 0.003(3) 0.002(3) C9 0.027(5) 0.023(4) 0.008(4) 0.001(3) 0.004(3) -0.002(3) C10 0.030(5) 0.013(4) 0.015(4) 0.001(3) -0.001(3) -0.005(4) C6 0.024(4) 0.006(3) 0.014(4) 0.000(3) 0.002(3) 0.006(3) C14 0.022(2) 0.028(2) 0.0138(18) -0.0057(18) 0.0021(15) 0.0091(19) C13 0.020(4) 0.024(4) 0.012(4) 0.001(3) 0.002(3) 0.003(3) C15 0.022(2) 0.028(2) 0.0138(18) -0.0057(18) 0.0021(15) 0.0091(19) C18 0.022(2) 0.028(2) 0.0138(18) -0.0057(18) 0.0021(15) 0.0091(19) C17 0.022(2) 0.028(2) 0.0138(18) -0.0057(18) 0.0021(15) 0.0091(19) C16 0.028(5) 0.027(5) 0.011(4) -0.002(3) -0.001(3) 0.011(4) C25 0.028(4) 0.016(4) 0.015(4) 0.013(3) 0.000(3) -0.002(3) C20 0.035(5) 0.029(5) 0.022(4) -0.004(4) 0.005(4) -0.007(4) C24 0.030(5) 0.028(5) 0.019(4) 0.004(4) -0.004(4) 0.001(4) C30 0.030(5) 0.029(5) 0.026(5) 0.007(4) 0.001(4) -0.002(4) C19 0.025(5) 0.028(5) 0.013(4) 0.007(3) -0.003(3) -0.004(4) C26 0.026(5) 0.021(4) 0.018(4) 0.000(3) -0.001(3) -0.007(4) C21 0.039(6) 0.029(5) 0.025(5) -0.001(4) 0.010(4) -0.008(4) C28 0.023(5) 0.078(9) 0.026(5) 0.022(5) -0.007(4) -0.021(5) C29 0.022(5) 0.043(6) 0.037(5) 0.003(4) 0.006(4) -0.003(4) C22 0.052(7) 0.039(6) 0.015(4) 0.010(4) 0.001(4) -0.009(5) C27 0.035(6) 0.031(5) 0.024(5) 0.006(4) -0.005(4) -0.012(4) C23 0.038(6) 0.036(6) 0.024(5) 0.020(4) -0.006(4) -0.004(4) C38 0.039(6) 0.033(5) 0.026(5) -0.007(4) 0.011(4) 0.005(5) C36 0.029(5) 0.021(4) 0.022(4) -0.001(4) 0.008(3) -0.001(4) C42 0.027(5) 0.046(7) 0.036(6) -0.012(5) 0.004(4) 0.016(5) C31 0.026(5) 0.023(4) 0.007(3) -0.002(3) 0.008(3) -0.004(3) C37 0.010(4) 0.037(5) 0.021(4) -0.003(4) -0.002(3) 0.004(4) C32 0.028(5) 0.025(5) 0.013(4) 0.001(3) 0.006(4) -0.001(4) C34 0.022(5) 0.044(6) 0.032(5) -0.017(5) 0.002(4) 0.002(4) C33 0.036(5) 0.014(4) 0.029(5) -0.005(4) 0.006(4) -0.006(4) C40 0.039(6) 0.021(5) 0.024(5) -0.008(4) -0.001(4) 0.011(4) C35 0.016(4) 0.056(7) 0.021(4) 0.004(4) 0.001(3) 0.001(4) C41 0.041(6) 0.035(6) 0.042(6) -0.013(5) -0.002(5) 0.007(5) C39 0.041(6) 0.020(5) 0.029(5) -0.003(4) 0.013(4) 0.003(4) C43 0.031(5) 0.043(6) 0.014(4) -0.005(4) 0.001(3) 0.013(5) C49 0.026(5) 0.029(5) 0.013(4) 0.001(3) -0.002(3) 0.010(4) C54 0.037(5) 0.033(5) 0.013(4) 0.001(4) 0.002(4) 0.007(4) C45 0.072(8) 0.033(6) 0.017(4) 0.005(4) 0.008(5) 0.016(5) C52 0.049(7) 0.032(6) 0.032(5) -0.008(5) -0.008(5) 0.005(5) C51 0.040(6) 0.039(6) 0.030(5) 0.013(5) 0.002(4) 0.005(5) C53 0.021(5) 0.052(7) 0.024(5) -0.008(5) 0.003(4) 0.010(4) C48 0.029(5) 0.053(7) 0.026(5) -0.012(5) -0.005(4) 0.003(5) C44 0.040(6) 0.030(5) 0.020(4) 0.001(4) 0.006(4) 0.005(4) C46 0.062(8) 0.082(9) 0.013(4) -0.007(5) 0.004(5) 0.041(7) C50 0.039(6) 0.016(5) 0.024(5) 0.005(3) 0.004(4) 0.006(4) C47 0.041(6) 0.074(9) 0.038(6) -0.043(6) -0.012(5) 0.017(6) C60 0.029(5) 0.013(4) 0.021(4) 0.001(3) -0.002(4) 0.000(3) C62 0.026(5) 0.034(5) 0.023(4) 0.005(4) 0.007(4) -0.002(4) C61 0.018(4) 0.031(5) 0.012(4) 0.014(3) -0.001(3) -0.009(4) C57 0.035(6) 0.040(6) 0.033(5) -0.001(4) 0.008(4) 0.016(5) C55 0.021(4) 0.020(4) 0.020(4) 0.006(3) -0.001(3) 0.006(3) C66 0.018(5) 0.046(6) 0.020(4) 0.002(4) 0.003(4) -0.002(4) C56 0.032(6) 0.049(7) 0.015(5) 0.002(4) -0.006(4) 0.004(4) C65 0.023(5) 0.045(6) 0.032(5) 0.006(4) 0.000(4) -0.012(4) C64 0.027(4) 0.018(3) 0.025(3) 0.012(2) 0.003(3) 0.004(2) C58 0.027(4) 0.018(3) 0.025(3) 0.012(2) 0.003(3) 0.004(2) C63 0.033(5) 0.020(4) 0.022(4) 0.014(4) 0.006(4) -0.003(4) C59 0.029(5) 0.035(6) 0.026(5) 0.004(4) 0.003(4) -0.001(4) C68 0.028(5) 0.018(4) 0.009(4) 0.000(3) -0.008(3) -0.009(3) C67 0.035(5) 0.012(4) 0.021(4) -0.002(3) 0.008(4) -0.003(4) N7 0.019(4) 0.037(4) 0.015(3) 0.009(3) 0.002(3) -0.005(3) N3 0.021(4) 0.031(4) 0.009(3) 0.002(3) 0.001(3) -0.008(3) N2 0.020(4) 0.011(3) 0.018(3) 0.002(2) 0.002(3) 0.000(3) N6 0.022(4) 0.035(4) 0.012(3) 0.005(3) 0.002(3) 0.004(3) N5 0.0190(16) 0.0178(17) 0.0159(15) -0.0024(14) 0.0016(12) 0.0004(14) N4 0.0190(16) 0.0178(17) 0.0159(15) -0.0024(14) 0.0016(12) 0.0004(14) N8 0.0190(16) 0.0178(17) 0.0159(15) -0.0024(14) 0.0016(12) 0.0004(14) N1 0.0190(16) 0.0178(17) 0.0159(15) -0.0024(14) 0.0016(12) 0.0004(14) F4 0.066(4) 0.011(3) 0.087(5) 0.000(3) -0.027(4) -0.001(3) F1 0.038(3) 0.005(2) 0.055(4) 0.002(2) -0.006(3) -0.004(2) F5 0.064(5) 0.049(4) 0.061(4) 0.006(3) 0.023(4) -0.003(4) F2 0.056(4) 0.063(4) 0.042(4) 0.001(3) -0.011(3) 0.011(4) F3 0.048(4) 0.033(3) 0.083(5) -0.014(3) 0.024(4) 0.004(3) F6 0.099(7) 0.075(6) 0.059(5) -0.010(4) -0.004(4) -0.036(5) O5 0.066(7) 0.093(8) 0.099(8) -0.020(7) 0.026(6) 0.029(6) O1 0.042(4) 0.039(4) 0.042(4) 0.007(3) 0.015(3) 0.001(3) O6 0.064(6) 0.045(5) 0.071(6) 0.000(4) 0.029(5) -0.019(4) O4 0.073(6) 0.072(6) 0.042(5) -0.003(4) -0.003(4) 0.020(5) O2 0.057(5) 0.068(6) 0.025(4) 0.001(4) -0.002(3) -0.014(4) O3 0.046(4) 0.025(4) 0.036(4) -0.018(3) 0.008(3) -0.004(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 Pt1 C2 1.995(8) . ? Pt1 C4 1.996(8) . ? Pt1 C1 2.025(8) . ? Pt1 C3 2.035(7) . ? S2 O4 1.413(9) . ? S2 O6 1.428(8) . ? S2 O5 1.508(11) . ? S2 C68 1.779(9) . ? S1 O3 1.369(7) . ? S1 O1 1.410(7) . ? S1 O2 1.443(7) . ? S1 C67 1.845(9) . ? C1 N2 1.361(11) . ? C1 N1 1.373(10) . ? C4 N7 1.327(11) . ? C4 N8 1.339(10) . ? C3 N6 1.351(10) . ? C3 N5 1.357(10) . ? C2 N4 1.338(10) . ? C2 N3 1.357(11) . ? C7 C8 1.339(12) . ? C7 N3 1.415(10) . ? C7 C31 1.477(12) . ? C5 C6 1.338(12) . ? C5 N1 1.408(10) . ? C5 C19 1.493(11) . ? C12 C11 1.350(11) . ? C12 N8 1.400(10) . ? C12 C61 1.486(11) . ? C8 N4 1.413(11) . ? C8 C37 1.457(12) . ? C11 N7 1.388(10) . ? C11 C55 1.468(11) . ? C9 C10 1.344(12) . ? C9 N5 1.391(10) . ? C9 C43 1.481(11) . ? C10 N6 1.401(10) . ? C10 C49 1.453(12) . ? C6 N2 1.371(10) . ? C6 C25 1.491(12) . ? C14 N4 1.437(11) . ? C14 C15 1.490(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13 N3 1.440(10) . ? C13 N2 1.478(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 N5 1.486(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C18 N1 1.465(11) . ? C18 C17 1.531(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C17 N8 1.460(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C16 N7 1.458(10) . ? C16 N6 1.488(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C25 C26 1.384(12) . ? C25 C30 1.409(13) . ? C20 C19 1.378(13) . ? C20 C21 1.380(12) . ? C20 H20 0.9500 . ? C24 C19 1.384(12) . ? C24 C23 1.407(12) . ? C24 H24 0.9500 . ? C30 C29 1.405(13) . ? C30 H30 0.9500 . ? C26 C27 1.401(12) . ? C26 H26 0.9500 . ? C21 C22 1.381(14) . ? C21 H21 0.9500 . ? C28 C27 1.370(15) . ? C28 C29 1.386(15) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C22 C23 1.358(15) . ? C22 H22 0.9500 . ? C27 H27 0.9500 . ? C23 H23 0.9500 . ? C38 C37 1.349(13) . ? C38 C39 1.354(12) . ? C38 H38 0.9500 . ? C36 C31 1.383(12) . ? C36 C35 1.411(13) . ? C36 H36 0.9500 . ? C42 C41 1.407(14) . ? C42 C37 1.420(14) . ? C42 H42 0.9500 . ? C31 C32 1.406(12) . ? C32 C33 1.366(13) . ? C32 H32 0.9500 . ? C34 C33 1.348(13) . ? C34 C35 1.393(14) . ? C34 H34 0.9500 . ? C33 H33 0.9500 . ? C40 C39 1.348(12) . ? C40 C41 1.387(15) . ? C40 H40 0.9500 . ? C35 H35 0.9500 . ? C41 H41 0.9500 . ? C39 H39 0.9500 . ? C43 C44 1.381(13) . ? C43 C48 1.382(14) . ? C49 C54 1.387(13) . ? C49 C50 1.425(12) . ? C54 C53 1.406(13) . ? C54 H54 0.9500 . ? C45 C44 1.400(12) . ? C45 C46 1.410(18) . ? C45 H45 0.9500 . ? C52 C53 1.343(15) . ? C52 C51 1.405(15) . ? C52 H52 0.9500 . ? C51 C50 1.364(13) . ? C51 H51 0.9500 . ? C53 H53 0.9500 . ? C48 C47 1.404(13) . ? C48 H48 0.9500 . ? C44 H44 0.9500 . ? C46 C47 1.360(18) . ? C46 H46 0.9500 . ? C50 H50 0.9500 . ? C47 H47 0.9500 . ? C60 C55 1.399(12) . ? C60 C59 1.428(13) . ? C60 H60 0.9500 . ? C62 C61 1.393(13) . ? C62 C63 1.420(12) . ? C62 H62 0.9500 . ? C61 C66 1.374(14) . ? C57 C58 1.346(14) . ? C57 C56 1.384(14) . ? C57 H57 0.9500 . ? C55 C56 1.413(13) . ? C66 C65 1.381(13) . ? C66 H66 0.9500 . ? C56 H56 0.9500 . ? C65 C64 1.371(13) . ? C65 H65 0.9500 . ? C64 C63 1.354(13) . ? C64 H64 0.9500 . ? C58 C59 1.413(12) . ? C58 H58 0.9500 . ? C63 H63 0.9500 . ? C59 H59 0.9500 . ? C68 F6 1.270(10) . ? C68 F4 1.361(10) . ? C68 F5 1.408(10) . ? C67 F3 1.285(10) . ? C67 F2 1.295(10) . ? C67 F1 1.386(9) . ? 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 Pt1 C4 179.6(4) . . ? C2 Pt1 C1 87.5(3) . . ? C4 Pt1 C1 92.7(3) . . ? C2 Pt1 C3 93.0(3) . . ? C4 Pt1 C3 86.8(3) . . ? C1 Pt1 C3 173.7(3) . . ? O4 S2 O6 116.2(6) . . ? O4 S2 O5 112.9(6) . . ? O6 S2 O5 115.4(6) . . ? O4 S2 C68 106.5(5) . . ? O6 S2 C68 101.5(5) . . ? O5 S2 C68 101.9(5) . . ? O3 S1 O1 116.1(4) . . ? O3 S1 O2 115.9(5) . . ? O1 S1 O2 112.7(5) . . ? O3 S1 C67 102.1(4) . . ? O1 S1 C67 103.7(4) . . ? O2 S1 C67 104.0(4) . . ? N2 C1 N1 104.4(7) . . ? N2 C1 Pt1 119.6(6) . . ? N1 C1 Pt1 135.8(7) . . ? N7 C4 N8 105.0(7) . . ? N7 C4 Pt1 124.8(6) . . ? N8 C4 Pt1 130.0(6) . . ? N6 C3 N5 104.9(6) . . ? N6 C3 Pt1 119.5(6) . . ? N5 C3 Pt1 135.5(6) . . ? N4 C2 N3 105.8(7) . . ? N4 C2 Pt1 129.9(6) . . ? N3 C2 Pt1 124.2(6) . . ? C8 C7 N3 106.8(7) . . ? C8 C7 C31 133.2(8) . . ? N3 C7 C31 119.9(7) . . ? C6 C5 N1 108.2(7) . . ? C6 C5 C19 128.8(8) . . ? N1 C5 C19 122.9(7) . . ? C11 C12 N8 106.3(7) . . ? C11 C12 C61 129.5(8) . . ? N8 C12 C61 124.1(7) . . ? C7 C8 N4 106.6(7) . . ? C7 C8 C37 130.8(8) . . ? N4 C8 C37 122.6(7) . . ? C12 C11 N7 105.5(7) . . ? C12 C11 C55 131.6(8) . . ? N7 C11 C55 122.9(7) . . ? C10 C9 N5 108.0(7) . . ? C10 C9 C43 129.0(8) . . ? N5 C9 C43 122.6(7) . . ? C9 C10 N6 105.4(7) . . ? C9 C10 C49 131.5(7) . . ? N6 C10 C49 123.0(7) . . ? C5 C6 N2 106.2(7) . . ? C5 C6 C25 131.1(7) . . ? N2 C6 C25 122.7(7) . . ? N4 C14 C15 114.7(7) . . ? N4 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N4 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N3 C13 N2 109.3(7) . . ? N3 C13 H13A 109.8 . . ? N2 C13 H13A 109.8 . . ? N3 C13 H13B 109.8 . . ? N2 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N5 C15 C14 117.9(7) . . ? N5 C15 H15A 107.8 . . ? C14 C15 H15A 107.8 . . ? N5 C15 H15B 107.8 . . ? C14 C15 H15B 107.8 . . ? H15A C15 H15B 107.2 . . ? N1 C18 C17 115.1(7) . . ? N1 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? N1 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? N8 C17 C18 111.7(7) . . ? N8 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N8 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? N7 C16 N6 107.5(7) . . ? N7 C16 H16A 110.2 . . ? N6 C16 H16A 110.2 . . ? N7 C16 H16B 110.2 . . ? N6 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C26 C25 C30 120.8(8) . . ? C26 C25 C6 121.4(8) . . ? C30 C25 C6 117.8(7) . . ? C19 C20 C21 120.7(9) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C19 C24 C23 119.8(9) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C29 C30 C25 118.1(9) . . ? C29 C30 H30 121.0 . . ? C25 C30 H30 121.0 . . ? C20 C19 C24 118.8(8) . . ? C20 C19 C5 122.5(8) . . ? C24 C19 C5 118.6(8) . . ? C25 C26 C27 120.2(9) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C20 C21 C22 120.7(9) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C27 C28 C29 121.7(9) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C30 120.1(9) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C23 C22 C21 119.2(8) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C28 C27 C26 119.1(9) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C22 C23 C24 120.7(9) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C37 C38 C39 123.0(10) . . ? C37 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C31 C36 C35 119.7(9) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C41 C42 C37 119.2(10) . . ? C41 C42 H42 120.4 . . ? C37 C42 H42 120.4 . . ? C36 C31 C32 118.3(8) . . ? C36 C31 C7 121.3(8) . . ? C32 C31 C7 120.4(8) . . ? C38 C37 C42 118.2(9) . . ? C38 C37 C8 122.5(9) . . ? C42 C37 C8 119.3(8) . . ? C33 C32 C31 120.8(9) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C33 C34 C35 119.4(9) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C33 C32 121.7(9) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C39 C40 C41 121.6(9) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C34 C35 C36 120.0(9) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C40 C41 C42 118.3(10) . . ? C40 C41 H41 120.9 . . ? C42 C41 H41 120.9 . . ? C40 C39 C38 119.7(10) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C44 C43 C48 118.0(8) . . ? C44 C43 C9 122.4(9) . . ? C48 C43 C9 119.6(9) . . ? C54 C49 C50 117.8(8) . . ? C54 C49 C10 122.2(8) . . ? C50 C49 C10 119.9(8) . . ? C49 C54 C53 120.1(9) . . ? C49 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C44 C45 C46 118.3(10) . . ? C44 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? C53 C52 C51 120.5(10) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C50 C51 C52 119.5(9) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C52 C53 C54 120.8(10) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C43 C48 C47 121.6(10) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C43 C44 C45 121.9(10) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C47 C46 C45 120.6(9) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C51 C50 C49 121.1(9) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C46 C47 C48 119.5(11) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C55 C60 C59 118.3(8) . . ? C55 C60 H60 120.8 . . ? C59 C60 H60 120.8 . . ? C61 C62 C63 117.7(9) . . ? C61 C62 H62 121.1 . . ? C63 C62 H62 121.1 . . ? C66 C61 C62 120.0(7) . . ? C66 C61 C12 121.1(8) . . ? C62 C61 C12 118.9(8) . . ? C58 C57 C56 126.5(10) . . ? C58 C57 H57 116.7 . . ? C56 C57 H57 116.7 . . ? C60 C55 C56 120.8(8) . . ? C60 C55 C11 119.7(7) . . ? C56 C55 C11 119.6(8) . . ? C61 C66 C65 120.5(9) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C57 C56 C55 116.7(10) . . ? C57 C56 H56 121.6 . . ? C55 C56 H56 121.6 . . ? C64 C65 C66 120.7(10) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C63 C64 C65 119.5(8) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C57 C58 C59 116.3(9) . . ? C57 C58 H58 121.8 . . ? C59 C58 H58 121.8 . . ? C64 C63 C62 121.5(9) . . ? C64 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C58 C59 C60 121.3(9) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? F6 C68 F4 109.8(8) . . ? F6 C68 F5 105.5(7) . . ? F4 C68 F5 101.1(7) . . ? F6 C68 S2 116.9(8) . . ? F4 C68 S2 112.1(6) . . ? F5 C68 S2 110.2(6) . . ? F3 C67 F2 110.0(8) . . ? F3 C67 F1 106.4(7) . . ? F2 C67 F1 108.4(7) . . ? F3 C67 S1 111.9(6) . . ? F2 C67 S1 111.9(6) . . ? F1 C67 S1 108.0(6) . . ? C4 N7 C11 112.3(7) . . ? C4 N7 C16 118.8(7) . . ? C11 N7 C16 128.9(7) . . ? C2 N3 C7 110.0(7) . . ? C2 N3 C13 119.0(7) . . ? C7 N3 C13 130.3(7) . . ? C1 N2 C6 112.3(7) . . ? C1 N2 C13 120.9(7) . . ? C6 N2 C13 123.8(7) . . ? C3 N6 C10 111.5(7) . . ? C3 N6 C16 121.7(7) . . ? C10 N6 C16 125.1(7) . . ? C3 N5 C9 110.2(6) . . ? C3 N5 C15 128.5(7) . . ? C9 N5 C15 121.3(6) . . ? C2 N4 C8 110.8(7) . . ? C2 N4 C14 120.6(7) . . ? C8 N4 C14 128.5(7) . . ? C4 N8 C12 110.7(7) . . ? C4 N8 C17 121.0(7) . . ? C12 N8 C17 128.1(7) . . ? C1 N1 C5 108.8(7) . . ? C1 N1 C18 128.8(7) . . ? C5 N1 C18 122.0(6) . . ? 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 C2 Pt1 C1 N2 -24.4(7) . . . . ? C4 Pt1 C1 N2 155.3(7) . . . . ? C3 Pt1 C1 N2 70(3) . . . . ? C2 Pt1 C1 N1 150.5(9) . . . . ? C4 Pt1 C1 N1 -29.8(9) . . . . ? C3 Pt1 C1 N1 -115(3) . . . . ? C2 Pt1 C4 N7 -15(61) . . . . ? C1 Pt1 C4 N7 -137.2(8) . . . . ? C3 Pt1 C4 N7 36.5(8) . . . . ? C2 Pt1 C4 N8 172(100) . . . . ? C1 Pt1 C4 N8 49.8(8) . . . . ? C3 Pt1 C4 N8 -136.5(8) . . . . ? C2 Pt1 C3 N6 149.0(7) . . . . ? C4 Pt1 C3 N6 -30.7(7) . . . . ? C1 Pt1 C3 N6 55(3) . . . . ? C2 Pt1 C3 N5 -26.4(9) . . . . ? C4 Pt1 C3 N5 153.9(9) . . . . ? C1 Pt1 C3 N5 -121(3) . . . . ? C4 Pt1 C2 N4 101(60) . . . . ? C1 Pt1 C2 N4 -137.7(8) . . . . ? C3 Pt1 C2 N4 48.6(8) . . . . ? C4 Pt1 C2 N3 -82(60) . . . . ? C1 Pt1 C2 N3 39.3(7) . . . . ? C3 Pt1 C2 N3 -134.4(7) . . . . ? N3 C7 C8 N4 -0.1(9) . . . . ? C31 C7 C8 N4 175.3(8) . . . . ? N3 C7 C8 C37 -178.2(9) . . . . ? C31 C7 C8 C37 -2.8(16) . . . . ? N8 C12 C11 N7 -1.6(9) . . . . ? C61 C12 C11 N7 -179.3(9) . . . . ? N8 C12 C11 C55 179.6(8) . . . . ? C61 C12 C11 C55 1.9(16) . . . . ? N5 C9 C10 N6 -0.4(9) . . . . ? C43 C9 C10 N6 -173.8(9) . . . . ? N5 C9 C10 C49 -176.8(9) . . . . ? C43 C9 C10 C49 9.8(16) . . . . ? N1 C5 C6 N2 -1.8(9) . . . . ? C19 C5 C6 N2 -178.8(8) . . . . ? N1 C5 C6 C25 -179.3(8) . . . . ? C19 C5 C6 C25 3.6(15) . . . . ? N4 C14 C15 N5 76.3(10) . . . . ? N1 C18 C17 N8 84.2(9) . . . . ? C5 C6 C25 C26 51.3(12) . . . . ? N2 C6 C25 C26 -125.8(8) . . . . ? C5 C6 C25 C30 -128.4(9) . . . . ? N2 C6 C25 C30 54.4(10) . . . . ? C26 C25 C30 C29 1.7(12) . . . . ? C6 C25 C30 C29 -178.5(8) . . . . ? C21 C20 C19 C24 -3.1(14) . . . . ? C21 C20 C19 C5 175.1(8) . . . . ? C23 C24 C19 C20 2.4(14) . . . . ? C23 C24 C19 C5 -175.9(8) . . . . ? C6 C5 C19 C20 -119.3(10) . . . . ? N1 C5 C19 C20 64.1(12) . . . . ? C6 C5 C19 C24 58.9(13) . . . . ? N1 C5 C19 C24 -117.7(9) . . . . ? C30 C25 C26 C27 -0.4(12) . . . . ? C6 C25 C26 C27 179.9(8) . . . . ? C19 C20 C21 C22 2.4(14) . . . . ? C27 C28 C29 C30 1.2(16) . . . . ? C25 C30 C29 C28 -2.1(14) . . . . ? C20 C21 C22 C23 -0.9(15) . . . . ? C29 C28 C27 C26 0.2(15) . . . . ? C25 C26 C27 C28 -0.6(13) . . . . ? C21 C22 C23 C24 0.1(15) . . . . ? C19 C24 C23 C22 -0.9(15) . . . . ? C35 C36 C31 C32 -1.9(12) . . . . ? C35 C36 C31 C7 178.5(7) . . . . ? C8 C7 C31 C36 53.1(13) . . . . ? N3 C7 C31 C36 -131.9(8) . . . . ? C8 C7 C31 C32 -126.4(10) . . . . ? N3 C7 C31 C32 48.5(10) . . . . ? C39 C38 C37 C42 1.0(14) . . . . ? C39 C38 C37 C8 -177.6(9) . . . . ? C41 C42 C37 C38 -2.0(14) . . . . ? C41 C42 C37 C8 176.7(9) . . . . ? C7 C8 C37 C38 60.6(13) . . . . ? N4 C8 C37 C38 -117.1(10) . . . . ? C7 C8 C37 C42 -117.9(11) . . . . ? N4 C8 C37 C42 64.3(11) . . . . ? C36 C31 C32 C33 1.3(12) . . . . ? C7 C31 C32 C33 -179.2(8) . . . . ? C35 C34 C33 C32 -2.6(15) . . . . ? C31 C32 C33 C34 1.0(14) . . . . ? C33 C34 C35 C36 1.9(14) . . . . ? C31 C36 C35 C34 0.4(13) . . . . ? C39 C40 C41 C42 -0.5(16) . . . . ? C37 C42 C41 C40 1.8(15) . . . . ? C41 C40 C39 C38 -0.5(16) . . . . ? C37 C38 C39 C40 0.3(16) . . . . ? C10 C9 C43 C44 -125.2(10) . . . . ? N5 C9 C43 C44 62.3(13) . . . . ? C10 C9 C43 C48 55.4(14) . . . . ? N5 C9 C43 C48 -117.1(10) . . . . ? C9 C10 C49 C54 -134.8(10) . . . . ? N6 C10 C49 C54 49.3(13) . . . . ? C9 C10 C49 C50 48.7(14) . . . . ? N6 C10 C49 C50 -127.1(9) . . . . ? C50 C49 C54 C53 2.1(13) . . . . ? C10 C49 C54 C53 -174.5(8) . . . . ? C53 C52 C51 C50 2.0(16) . . . . ? C51 C52 C53 C54 0.5(15) . . . . ? C49 C54 C53 C52 -2.5(14) . . . . ? C44 C43 C48 C47 1.7(16) . . . . ? C9 C43 C48 C47 -178.9(10) . . . . ? C48 C43 C44 C45 -3.3(15) . . . . ? C9 C43 C44 C45 177.3(9) . . . . ? C46 C45 C44 C43 4.5(15) . . . . ? C44 C45 C46 C47 -4.2(16) . . . . ? C52 C51 C50 C49 -2.4(15) . . . . ? C54 C49 C50 C51 0.4(14) . . . . ? C10 C49 C50 C51 177.0(9) . . . . ? C45 C46 C47 C48 2.7(18) . . . . ? C43 C48 C47 C46 -1.4(18) . . . . ? C63 C62 C61 C66 1.3(12) . . . . ? C63 C62 C61 C12 179.1(8) . . . . ? C11 C12 C61 C66 -122.4(10) . . . . ? N8 C12 C61 C66 60.3(11) . . . . ? C11 C12 C61 C62 59.8(13) . . . . ? N8 C12 C61 C62 -117.5(10) . . . . ? C59 C60 C55 C56 -1.2(13) . . . . ? C59 C60 C55 C11 178.0(8) . . . . ? C12 C11 C55 C60 55.5(13) . . . . ? N7 C11 C55 C60 -123.1(9) . . . . ? C12 C11 C55 C56 -125.3(11) . . . . ? N7 C11 C55 C56 56.0(12) . . . . ? C62 C61 C66 C65 0.5(13) . . . . ? C12 C61 C66 C65 -177.3(8) . . . . ? C58 C57 C56 C55 -1.9(16) . . . . ? C60 C55 C56 C57 2.2(14) . . . . ? C11 C55 C56 C57 -176.9(8) . . . . ? C61 C66 C65 C64 -1.1(14) . . . . ? C66 C65 C64 C63 -0.2(14) . . . . ? C56 C57 C58 C59 0.4(16) . . . . ? C65 C64 C63 C62 2.1(13) . . . . ? C61 C62 C63 C64 -2.7(13) . . . . ? C57 C58 C59 C60 0.8(14) . . . . ? C55 C60 C59 C58 -0.4(13) . . . . ? O4 S2 C68 F6 167.4(8) . . . . ? O6 S2 C68 F6 -70.5(8) . . . . ? O5 S2 C68 F6 48.9(9) . . . . ? O4 S2 C68 F4 -64.6(8) . . . . ? O6 S2 C68 F4 57.5(8) . . . . ? O5 S2 C68 F4 176.9(7) . . . . ? O4 S2 C68 F5 47.1(8) . . . . ? O6 S2 C68 F5 169.2(6) . . . . ? O5 S2 C68 F5 -71.4(7) . . . . ? O3 S1 C67 F3 -71.4(7) . . . . ? O1 S1 C67 F3 167.6(6) . . . . ? O2 S1 C67 F3 49.5(8) . . . . ? O3 S1 C67 F2 52.6(7) . . . . ? O1 S1 C67 F2 -68.4(7) . . . . ? O2 S1 C67 F2 173.5(7) . . . . ? O3 S1 C67 F1 171.8(5) . . . . ? O1 S1 C67 F1 50.8(6) . . . . ? O2 S1 C67 F1 -67.3(7) . . . . ? N8 C4 N7 C11 -4.7(9) . . . . ? Pt1 C4 N7 C11 -179.2(6) . . . . ? N8 C4 N7 C16 177.1(7) . . . . ? Pt1 C4 N7 C16 2.6(11) . . . . ? C12 C11 N7 C4 4.1(10) . . . . ? C55 C11 N7 C4 -177.0(8) . . . . ? C12 C11 N7 C16 -178.0(8) . . . . ? C55 C11 N7 C16 1.0(13) . . . . ? N6 C16 N7 C4 -56.5(10) . . . . ? N6 C16 N7 C11 125.6(9) . . . . ? N4 C2 N3 C7 -0.6(9) . . . . ? Pt1 C2 N3 C7 -178.2(5) . . . . ? N4 C2 N3 C13 171.0(7) . . . . ? Pt1 C2 N3 C13 -6.6(10) . . . . ? C8 C7 N3 C2 0.5(9) . . . . ? C31 C7 N3 C2 -175.7(7) . . . . ? C8 C7 N3 C13 -169.9(8) . . . . ? C31 C7 N3 C13 13.9(12) . . . . ? N2 C13 N3 C2 -49.6(10) . . . . ? N2 C13 N3 C7 120.1(9) . . . . ? N1 C1 N2 C6 1.8(9) . . . . ? Pt1 C1 N2 C6 178.1(5) . . . . ? N1 C1 N2 C13 163.0(7) . . . . ? Pt1 C1 N2 C13 -20.7(10) . . . . ? C5 C6 N2 C1 0.0(9) . . . . ? C25 C6 N2 C1 177.8(7) . . . . ? C5 C6 N2 C13 -160.6(7) . . . . ? C25 C6 N2 C13 17.2(11) . . . . ? N3 C13 N2 C1 66.2(9) . . . . ? N3 C13 N2 C6 -134.7(7) . . . . ? N5 C3 N6 C10 -0.8(10) . . . . ? Pt1 C3 N6 C10 -177.5(6) . . . . ? N5 C3 N6 C16 165.4(7) . . . . ? Pt1 C3 N6 C16 -11.2(11) . . . . ? C9 C10 N6 C3 0.8(10) . . . . ? C49 C10 N6 C3 177.6(8) . . . . ? C9 C10 N6 C16 -164.9(8) . . . . ? C49 C10 N6 C16 11.9(13) . . . . ? N7 C16 N6 C3 62.2(10) . . . . ? N7 C16 N6 C10 -133.5(8) . . . . ? N6 C3 N5 C9 0.5(9) . . . . ? Pt1 C3 N5 C9 176.4(7) . . . . ? N6 C3 N5 C15 -179.4(8) . . . . ? Pt1 C3 N5 C15 -3.6(14) . . . . ? C10 C9 N5 C3 0.0(10) . . . . ? C43 C9 N5 C3 173.8(8) . . . . ? C10 C9 N5 C15 179.9(7) . . . . ? C43 C9 N5 C15 -6.2(12) . . . . ? C14 C15 N5 C3 -12.9(13) . . . . ? C14 C15 N5 C9 167.1(8) . . . . ? N3 C2 N4 C8 0.5(9) . . . . ? Pt1 C2 N4 C8 177.9(6) . . . . ? N3 C2 N4 C14 178.5(7) . . . . ? Pt1 C2 N4 C14 -4.1(11) . . . . ? C7 C8 N4 C2 -0.2(9) . . . . ? C37 C8 N4 C2 178.0(8) . . . . ? C7 C8 N4 C14 -178.0(8) . . . . ? C37 C8 N4 C14 0.2(13) . . . . ? C15 C14 N4 C2 -78.5(10) . . . . ? C15 C14 N4 C8 99.1(9) . . . . ? N7 C4 N8 C12 3.6(9) . . . . ? Pt1 C4 N8 C12 177.6(6) . . . . ? N7 C4 N8 C17 179.1(7) . . . . ? Pt1 C4 N8 C17 -6.8(11) . . . . ? C11 C12 N8 C4 -1.2(9) . . . . ? C61 C12 N8 C4 176.7(8) . . . . ? C11 C12 N8 C17 -176.3(7) . . . . ? C61 C12 N8 C17 1.5(13) . . . . ? C18 C17 N8 C4 -77.2(9) . . . . ? C18 C17 N8 C12 97.5(10) . . . . ? N2 C1 N1 C5 -2.9(9) . . . . ? Pt1 C1 N1 C5 -178.2(7) . . . . ? N2 C1 N1 C18 -175.9(7) . . . . ? Pt1 C1 N1 C18 8.7(14) . . . . ? C6 C5 N1 C1 3.0(9) . . . . ? C19 C5 N1 C1 -179.8(8) . . . . ? C6 C5 N1 C18 176.6(7) . . . . ? C19 C5 N1 C18 -6.1(12) . . . . ? C17 C18 N1 C1 -28.3(12) . . . . ? C17 C18 N1 C5 159.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.816 _refine_diff_density_min -5.689 _refine_diff_density_rms 0.183 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.253 0.557 0.378 463.3 208.1 2 0.253 0.943 0.878 463.3 210.1 3 0.747 0.443 0.622 463.1 205.9 4 0.747 0.057 1.122 463.1 202.1 _platon_squeeze_details ; ? ; data_9 _database_code_depnum_ccdc_archive 'CCDC 882741' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 F6 N8 O8 Ru S4' _chemical_formula_weight 1512.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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' 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 12.306(2) _cell_length_b 18.427(4) _cell_length_c 16.292(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.907(2) _cell_angle_gamma 90.00 _cell_volume 3627.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9644 _exptl_absorpt_correction_T_max 0.9919 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29065 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.31 _reflns_number_total 5241 _reflns_number_gt 3250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5241 _refine_ls_number_parameters 434 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1459 _refine_ls_R_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.3419 _refine_ls_wR_factor_gt 0.3146 _refine_ls_goodness_of_fit_ref 1.249 _refine_ls_restrained_S_all 1.280 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.003 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 Ru1 Ru 0.5000 0.5000 0.0000 0.0462(5) Uani 1 2 d S . . S1 S 0.4864(3) 0.3846(2) 0.05342(19) 0.0755(11) Uani 1 1 d . . . N3 N 0.6118(6) 0.5553(5) 0.1745(4) 0.043(2) Uani 1 1 d . . . N2 N 0.7431(6) 0.5165(5) 0.0923(4) 0.046(2) Uani 1 1 d . . . N4 N 0.4467(5) 0.5308(4) 0.1791(4) 0.0369(19) Uani 1 1 d . . . N1 N 0.7403(6) 0.4395(4) -0.0044(4) 0.040(2) Uani 1 1 d . . . C33 C 0.7093(7) 0.5770(6) 0.1393(5) 0.041(2) Uani 1 1 d . . . H33A H 0.6905 0.6195 0.1020 0.049 Uiso 1 1 calc R . . H33B H 0.7708 0.5909 0.1850 0.049 Uiso 1 1 calc R . . C27 C 0.4440(7) 0.5340(5) 0.3332(5) 0.036(2) Uani 1 1 d . . . C5 C 0.6029(7) 0.5611(5) 0.2573(5) 0.034(2) Uani 1 1 d . . . C2 C 0.5177(7) 0.5361(6) 0.1241(5) 0.040(2) Uani 1 1 d . . . C7 C 0.3256(7) 0.5252(6) 0.1528(5) 0.038(2) Uani 1 1 d . . . H7A H 0.2899 0.5291 0.2022 0.046 Uiso 1 1 calc R . . H7B H 0.3060 0.4776 0.1260 0.046 Uiso 1 1 calc R . . C1 C 0.6738(8) 0.4868(6) 0.0272(6) 0.045(3) Uani 1 1 d . . . C8 C 0.7160(8) 0.4134(6) -0.0906(5) 0.044(2) Uani 1 1 d . . . H8A H 0.6590 0.3749 -0.0957 0.053 Uiso 1 1 calc R . . H8B H 0.7837 0.3919 -0.1049 0.053 Uiso 1 1 calc R . . C6 C 0.4975(7) 0.5458(5) 0.2618(5) 0.034(2) Uani 1 1 d . . . C21 C 0.7017(7) 0.5773(6) 0.3272(5) 0.040(2) Uani 1 1 d . . . C28 C 0.4311(7) 0.5891(6) 0.3890(5) 0.040(2) Uani 1 1 d . . . H28 H 0.4557 0.6368 0.3798 0.048 Uiso 1 1 calc R . . C29 C 0.3833(7) 0.5757(6) 0.4572(6) 0.046(3) Uani 1 1 d . . . H29 H 0.3757 0.6139 0.4948 0.056 Uiso 1 1 calc R . . C14 C 1.0452(8) 0.4059(6) 0.0433(5) 0.045(2) Uani 1 1 d . . . H14 H 1.0655 0.4543 0.0591 0.054 Uiso 1 1 calc R . . C22 C 0.7019(7) 0.6355(6) 0.3759(5) 0.043(2) Uani 1 1 d . . . H22 H 0.6417 0.6686 0.3662 0.051 Uiso 1 1 calc R . . C23 C 0.7930(9) 0.6475(6) 0.4422(6) 0.056(3) Uani 1 1 d . . . H23 H 0.7944 0.6894 0.4764 0.067 Uiso 1 1 calc R . . C32 C 0.4057(7) 0.4647(5) 0.3469(6) 0.041(2) Uani 1 1 d . . . H32 H 0.4126 0.4263 0.3093 0.050 Uiso 1 1 calc R . . C3 C 0.8509(7) 0.4871(5) 0.1051(5) 0.038(2) Uani 1 1 d . . . C4 C 0.8488(7) 0.4376(5) 0.0456(5) 0.038(2) Uani 1 1 d . . . C9 C 0.9340(8) 0.3857(6) 0.0300(5) 0.043(3) Uani 1 1 d . . . C30 C 0.3464(8) 0.5074(6) 0.4712(6) 0.045(3) Uani 1 1 d . . . H30 H 0.3136 0.4983 0.5185 0.054 Uiso 1 1 calc R . . C31 C 0.3571(7) 0.4522(6) 0.4167(6) 0.046(3) Uani 1 1 d . . . H31 H 0.3312 0.4050 0.4264 0.056 Uiso 1 1 calc R . . C26 C 0.7900(8) 0.5290(6) 0.3401(6) 0.044(2) Uani 1 1 d . . . H26 H 0.7899 0.4880 0.3046 0.053 Uiso 1 1 calc R . . C15 C 0.9417(8) 0.5116(5) 0.1729(6) 0.040(2) Uiso 1 1 d . . . O1 O 0.3779(8) 0.3608(7) 0.0666(7) 0.115(4) Uani 1 1 d . . . C13 C 1.1276(9) 0.3554(8) 0.0337(7) 0.063(3) Uani 1 1 d . . . H13 H 1.2030 0.3701 0.0438 0.076 Uiso 1 1 calc R . . C16 C 0.9768(7) 0.5813(6) 0.1801(5) 0.046(3) Uani 1 1 d . . . H16 H 0.9411 0.6168 0.1421 0.055 Uiso 1 1 calc R . . C17 C 1.0649(8) 0.6011(7) 0.2428(6) 0.055(3) Uani 1 1 d . . . H17 H 1.0882 0.6503 0.2468 0.066 Uiso 1 1 calc R . . C20 C 0.9946(8) 0.4592(7) 0.2290(5) 0.048(3) Uani 1 1 d . . . H20 H 0.9704 0.4101 0.2248 0.058 Uiso 1 1 calc R . . C19 C 1.0840(9) 0.4802(7) 0.2917(7) 0.059(3) Uani 1 1 d . . . H19 H 1.1210 0.4451 0.3296 0.071 Uiso 1 1 calc R . . C24 C 0.8786(8) 0.5993(6) 0.4573(6) 0.050(3) Uani 1 1 d . . . H24 H 0.9377 0.6062 0.5034 0.060 Uiso 1 1 calc R . . C25 C 0.8786(8) 0.5412(7) 0.4056(7) 0.058(3) Uani 1 1 d . . . H25 H 0.9397 0.5087 0.4143 0.069 Uiso 1 1 calc R . . C18 C 1.1186(8) 0.5525(8) 0.2984(6) 0.062(3) Uani 1 1 d . . . H18 H 1.1783 0.5672 0.3410 0.074 Uiso 1 1 calc R . . C10 C 0.9085(9) 0.3143(6) 0.0073(6) 0.054(3) Uani 1 1 d . . . H10 H 0.8335 0.2991 -0.0011 0.065 Uiso 1 1 calc R . . C12 C 1.1010(10) 0.2861(7) 0.0102(7) 0.070(4) Uani 1 1 d . . . H12 H 1.1564 0.2521 0.0029 0.084 Uiso 1 1 calc R . . C11 C 0.9869(10) 0.2660(7) -0.0032(7) 0.067(4) Uani 1 1 d . . . H11 H 0.9659 0.2178 -0.0197 0.080 Uiso 1 1 calc R . . C34 C 0.5788(16) 0.3634(11) 0.1492(11) 0.130(7) Uani 1 1 d . . . H34A H 0.5638 0.3957 0.1936 0.195 Uiso 1 1 calc R . . H34B H 0.6554 0.3701 0.1419 0.195 Uiso 1 1 calc R . . H34C H 0.5678 0.3129 0.1645 0.195 Uiso 1 1 calc R . . C35 C 0.5334(15) 0.3082(11) -0.0014(12) 0.131(7) Uani 1 1 d . . . H35A H 0.5346 0.2643 0.0327 0.197 Uiso 1 1 calc R . . H35B H 0.6080 0.3181 -0.0115 0.197 Uiso 1 1 calc R . . H35C H 0.4827 0.3011 -0.0550 0.197 Uiso 1 1 calc R . . S2 S 0.8815(7) 0.2941(4) 0.3039(5) 0.050(4) Uiso 0.287(10) 1 d PD A 1 F3 F 0.7181(17) 0.3640(10) 0.3614(13) 0.050(4) Uiso 0.287(10) 1 d PD A 1 F2 F 0.8009(16) 0.2785(10) 0.4420(10) 0.050(4) Uiso 0.287(10) 1 d PD A 1 O4 O 0.8316(15) 0.3226(9) 0.2228(9) 0.026(4) Uiso 0.287(10) 1 d PD A 1 O2 O 0.9017(14) 0.2157(7) 0.3010(11) 0.026(4) Uiso 0.287(10) 1 d PD A 1 O3 O 0.9702(12) 0.3326(8) 0.3555(10) 0.026(4) Uiso 0.287(10) 1 d PD A 1 F4 F 0.6819(14) 0.2536(9) 0.3291(12) 0.050(4) Uiso 0.287(10) 1 d PD A 1 C40 C 0.7683(15) 0.2991(9) 0.3608(11) 0.062(11) Uiso 0.287(10) 1 d PD A 1 C40' C 0.817(3) 0.3190(19) 0.3846(18) 0.34(4) Uiso 0.713(10) 1 d PD A 2 S2' S 0.8089(17) 0.2664(11) 0.2820(12) 0.296(9) Uiso 0.713(10) 1 d PD A 2 O2' O 0.917(2) 0.2299(15) 0.3297(18) 0.213(12) Uiso 0.713(10) 1 d PD A 2 F1' F 0.903(3) 0.3684(15) 0.3834(17) 0.268(13) Uiso 0.713(10) 1 d PD A 2 O3' O 0.7052(15) 0.2275(10) 0.2862(12) 0.131(6) Uiso 0.713(10) 1 d PD A 2 O4' O 0.788(2) 0.3311(14) 0.2287(16) 0.204(12) Uiso 0.713(10) 1 d PD A 2 F2' F 0.867(6) 0.267(3) 0.442(2) 0.56(4) Uiso 0.713(10) 1 d PD A 2 F3' F 0.722(4) 0.358(2) 0.367(3) 0.342(19) Uiso 0.713(10) 1 d PD A 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 Ru1 0.0196(7) 0.0937(11) 0.0257(7) -0.0127(6) 0.0052(5) -0.0170(6) S1 0.0434(18) 0.131(3) 0.0543(19) -0.0118(18) 0.0135(15) -0.0082(18) N3 0.017(4) 0.083(6) 0.031(4) -0.005(4) 0.010(3) -0.015(4) N2 0.021(4) 0.098(7) 0.020(4) -0.015(4) 0.009(3) -0.019(4) N4 0.015(4) 0.073(5) 0.021(4) -0.004(4) 0.000(3) 0.000(4) N1 0.026(4) 0.071(6) 0.018(4) -0.003(4) -0.005(3) -0.013(4) C33 0.027(5) 0.076(7) 0.022(5) -0.012(4) 0.012(4) -0.025(5) C27 0.009(4) 0.066(6) 0.029(5) 0.002(5) -0.004(4) -0.005(4) C5 0.025(5) 0.064(6) 0.014(4) -0.005(4) 0.006(4) -0.015(4) C2 0.014(5) 0.074(7) 0.032(5) -0.013(5) 0.003(4) -0.011(4) C7 0.014(4) 0.078(7) 0.021(5) -0.006(4) 0.000(4) -0.003(4) C1 0.032(6) 0.086(8) 0.018(5) -0.011(5) 0.007(4) -0.019(5) C8 0.035(6) 0.070(7) 0.024(5) -0.001(4) -0.003(4) 0.000(5) C6 0.022(5) 0.066(6) 0.011(4) -0.007(4) -0.004(3) -0.008(4) C21 0.021(5) 0.074(7) 0.023(5) -0.009(5) 0.002(4) -0.017(5) C28 0.025(5) 0.065(7) 0.027(5) -0.010(4) -0.001(4) -0.012(4) C29 0.020(5) 0.087(8) 0.030(5) -0.021(5) 0.000(4) -0.010(5) C14 0.036(6) 0.073(7) 0.022(5) -0.001(4) -0.004(4) -0.004(5) C22 0.026(5) 0.067(7) 0.031(5) -0.007(5) -0.006(4) -0.009(5) C23 0.053(7) 0.073(7) 0.036(6) -0.003(5) -0.009(5) -0.020(6) C32 0.027(5) 0.053(6) 0.040(6) -0.009(5) -0.003(4) -0.005(5) C3 0.019(5) 0.073(7) 0.021(5) -0.004(4) 0.001(4) -0.013(4) C4 0.023(5) 0.062(6) 0.024(5) 0.002(5) -0.006(4) -0.009(4) C9 0.030(5) 0.068(7) 0.025(5) 0.011(5) -0.010(4) -0.010(5) C30 0.023(5) 0.089(8) 0.021(5) 0.000(5) -0.001(4) 0.004(5) C31 0.019(5) 0.085(8) 0.037(6) 0.014(6) 0.009(4) 0.005(5) C26 0.027(5) 0.078(7) 0.027(5) 0.001(5) 0.009(4) -0.002(5) O1 0.070(7) 0.161(10) 0.123(9) 0.014(8) 0.040(6) 0.001(7) C13 0.031(6) 0.101(10) 0.053(7) 0.006(7) -0.006(5) 0.010(6) C16 0.025(5) 0.087(8) 0.025(5) 0.000(5) 0.006(4) -0.009(5) C17 0.022(5) 0.103(9) 0.041(6) -0.019(6) 0.009(5) -0.024(6) C20 0.034(6) 0.090(8) 0.022(5) -0.008(5) 0.007(4) -0.005(5) C19 0.025(6) 0.114(11) 0.037(6) -0.011(6) 0.002(5) 0.015(6) C24 0.023(5) 0.101(9) 0.022(5) -0.011(5) -0.008(4) 0.000(5) C25 0.019(5) 0.106(9) 0.048(7) 0.009(7) 0.007(5) -0.004(5) C18 0.023(6) 0.134(12) 0.028(6) -0.018(7) 0.000(5) -0.007(7) C10 0.050(7) 0.063(8) 0.040(6) 0.010(5) -0.016(5) 0.001(6) C12 0.065(9) 0.078(9) 0.054(7) -0.007(6) -0.022(6) 0.025(7) C11 0.065(9) 0.058(7) 0.062(8) 0.005(6) -0.029(6) -0.002(6) C34 0.134(16) 0.150(16) 0.113(14) 0.045(12) 0.041(12) 0.041(13) C35 0.103(13) 0.167(18) 0.141(17) 0.014(13) 0.068(13) -0.005(13) _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 Ru1 C2 2.100(9) 3_665 ? Ru1 C2 2.100(9) . ? Ru1 C1 2.114(10) . ? Ru1 C1 2.114(10) 3_665 ? Ru1 S1 2.316(4) 3_665 ? Ru1 S1 2.316(4) . ? S1 O1 1.459(10) . ? S1 C34 1.792(17) . ? S1 C35 1.819(19) . ? N3 C2 1.334(11) . ? N3 C5 1.377(10) . ? N3 C33 1.480(10) . ? N2 C1 1.345(12) . ? N2 C3 1.412(12) . ? N2 C33 1.458(12) . ? N4 C2 1.368(11) . ? N4 C6 1.402(10) . ? N4 C7 1.474(10) . ? N1 C1 1.361(12) . ? N1 C4 1.427(11) . ? N1 C8 1.461(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C27 C28 1.393(13) . ? C27 C32 1.394(14) . ? C27 C6 1.457(12) . ? C5 C6 1.342(11) . ? C5 C21 1.530(12) . ? C7 C8 1.539(13) 3_665 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C7 1.539(13) 3_665 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C21 C22 1.334(13) . ? C21 C26 1.390(14) . ? C28 C29 1.374(13) . ? C28 H28 0.9500 . ? C29 C30 1.371(14) . ? C29 H29 0.9500 . ? C14 C9 1.395(13) . ? C14 C13 1.407(15) . ? C14 H14 0.9500 . ? C22 C23 1.420(13) . ? C22 H22 0.9500 . ? C23 C24 1.364(15) . ? C23 H23 0.9500 . ? C32 C31 1.400(13) . ? C32 H32 0.9500 . ? C3 C4 1.328(13) . ? C3 C15 1.484(13) . ? C4 C9 1.477(14) . ? C9 C10 1.385(14) . ? C30 C31 1.373(14) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C26 C25 1.392(14) . ? C26 H26 0.9500 . ? C15 C16 1.353(13) . ? C15 C20 1.403(14) . ? C13 C12 1.355(17) . ? C13 H13 0.9500 . ? C16 C17 1.392(13) . ? C16 H16 0.9500 . ? C17 C18 1.353(16) . ? C17 H17 0.9500 . ? C20 C19 1.406(14) . ? C20 H20 0.9500 . ? C19 C18 1.396(17) . ? C19 H19 0.9500 . ? C24 C25 1.363(15) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C18 H18 0.9500 . ? C10 C11 1.348(15) . ? C10 H10 0.9500 . ? C12 C11 1.429(16) . ? C12 H12 0.9500 . ? C11 H11 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 . ? S2 O3 1.433(13) . ? S2 O4 1.447(14) . ? S2 O2 1.468(12) . ? S2 C40 1.816(18) . ? F3 C40 1.347(16) . ? F2 C40 1.363(16) . ? F4 C40 1.375(16) . ? C40' F3' 1.36(2) . ? C40' F1' 1.39(2) . ? C40' F2' 1.39(2) . ? C40' S2' 1.917(19) . ? S2' O4' 1.470(17) . ? S2' O3' 1.476(17) . ? S2' O2' 1.563(18) . ? 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 Ru1 C2 180.0(5) 3_665 . ? C2 Ru1 C1 94.7(3) 3_665 . ? C2 Ru1 C1 85.3(3) . . ? C2 Ru1 C1 85.3(3) 3_665 3_665 ? C2 Ru1 C1 94.7(3) . 3_665 ? C1 Ru1 C1 180.0 . 3_665 ? C2 Ru1 S1 86.0(3) 3_665 3_665 ? C2 Ru1 S1 94.0(3) . 3_665 ? C1 Ru1 S1 92.4(3) . 3_665 ? C1 Ru1 S1 87.6(3) 3_665 3_665 ? C2 Ru1 S1 94.0(3) 3_665 . ? C2 Ru1 S1 86.0(3) . . ? C1 Ru1 S1 87.6(3) . . ? C1 Ru1 S1 92.4(3) 3_665 . ? S1 Ru1 S1 180.00(17) 3_665 . ? O1 S1 C34 104.7(8) . . ? O1 S1 C35 103.0(8) . . ? C34 S1 C35 92.9(9) . . ? O1 S1 Ru1 117.7(5) . . ? C34 S1 Ru1 116.6(7) . . ? C35 S1 Ru1 118.3(6) . . ? C2 N3 C5 113.7(7) . . ? C2 N3 C33 120.4(7) . . ? C5 N3 C33 125.4(7) . . ? C1 N2 C3 113.5(8) . . ? C1 N2 C33 121.6(8) . . ? C3 N2 C33 124.7(7) . . ? C2 N4 C6 113.1(7) . . ? C2 N4 C7 123.4(7) . . ? C6 N4 C7 122.4(7) . . ? C1 N1 C4 111.4(7) . . ? C1 N1 C8 123.1(8) . . ? C4 N1 C8 122.7(8) . . ? N2 C33 N3 109.3(7) . . ? N2 C33 H33A 109.8 . . ? N3 C33 H33A 109.8 . . ? N2 C33 H33B 109.8 . . ? N3 C33 H33B 109.8 . . ? H33A C33 H33B 108.3 . . ? C28 C27 C32 118.7(8) . . ? C28 C27 C6 122.5(9) . . ? C32 C27 C6 118.8(8) . . ? C6 C5 N3 107.2(7) . . ? C6 C5 C21 129.7(7) . . ? N3 C5 C21 123.0(7) . . ? N3 C2 N4 101.7(7) . . ? N3 C2 Ru1 126.6(6) . . ? N4 C2 Ru1 130.2(6) . . ? N4 C7 C8 109.4(8) . 3_665 ? N4 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 3_665 . ? N4 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 3_665 . ? H7A C7 H7B 108.2 . . ? N2 C1 N1 102.8(8) . . ? N2 C1 Ru1 125.7(7) . . ? N1 C1 Ru1 130.7(6) . . ? N1 C8 C7 111.9(8) . 3_665 ? N1 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 3_665 . ? N1 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 3_665 . ? H8A C8 H8B 107.9 . . ? C5 C6 N4 104.3(7) . . ? C5 C6 C27 131.5(7) . . ? N4 C6 C27 123.5(7) . . ? C22 C21 C26 120.8(8) . . ? C22 C21 C5 120.8(9) . . ? C26 C21 C5 118.5(9) . . ? C29 C28 C27 121.0(9) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 120.4(9) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C9 C14 C13 120.9(10) . . ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C21 C22 C23 119.4(10) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.4(10) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C27 C32 C31 119.3(9) . . ? C27 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C4 C3 N2 105.5(7) . . ? C4 C3 C15 131.3(9) . . ? N2 C3 C15 123.2(8) . . ? C3 C4 N1 106.7(8) . . ? C3 C4 C9 130.9(8) . . ? N1 C4 C9 122.4(8) . . ? C10 C9 C14 117.4(10) . . ? C10 C9 C4 121.9(9) . . ? C14 C9 C4 120.5(9) . . ? C29 C30 C31 119.8(9) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C32 120.8(10) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C21 C26 C25 119.3(10) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C16 C15 C20 119.7(9) . . ? C16 C15 C3 122.4(9) . . ? C20 C15 C3 117.9(9) . . ? C12 C13 C14 120.9(11) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C16 C17 120.3(10) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 122.2(11) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C15 C20 C19 119.1(11) . . ? C15 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C18 C19 C20 120.4(11) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C23 C24 C25 119.4(9) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 120.6(10) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C17 C18 C19 118.4(10) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C11 C10 C9 122.0(11) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C13 C12 C11 117.7(11) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C10 C11 C12 121.0(11) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? S1 C34 H34A 109.5 . . ? S1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? S1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? S1 C35 H35A 109.5 . . ? S1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? S1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O3 S2 O4 120.0(9) . . ? O3 S2 O2 113.1(9) . . ? O4 S2 O2 111.9(9) . . ? O3 S2 C40 104.4(8) . . ? O4 S2 C40 102.3(9) . . ? O2 S2 C40 102.6(8) . . ? F3 C40 F2 107.0(16) . . ? F3 C40 F4 102.7(16) . . ? F2 C40 F4 105.0(16) . . ? F3 C40 S2 116.5(14) . . ? F2 C40 S2 111.6(13) . . ? F4 C40 S2 113.0(13) . . ? F3' C40' F1' 106(4) . . ? F3' C40' F2' 139(5) . . ? F1' C40' F2' 103(4) . . ? F3' C40' S2' 101(2) . . ? F1' C40' S2' 103.6(19) . . ? F2' C40' S2' 101(2) . . ? O4' S2' O3' 111(2) . . ? O4' S2' O2' 133(2) . . ? O3' S2' O2' 116(2) . . ? O4' S2' C40' 94.6(16) . . ? O3' S2' C40' 96.3(14) . . ? O2' S2' C40' 83.3(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.345 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.157 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.246 0.765 0.255 131.3 29.3 2 -0.246 0.235 0.745 131.2 29.1 3 0.254 0.265 0.245 131.6 29.5 4 0.133 0.583 0.488 7.1 0.1 5 0.366 0.083 0.012 6.9 -0.1 6 0.746 0.735 0.755 131.0 28.7 7 0.633 0.917 0.988 7.4 0.2 8 0.866 0.417 0.512 7.2 -0.1 _platon_squeeze_details ; ? ; data_8 _database_code_depnum_ccdc_archive 'CCDC 882742' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H54 Cl2 Co F6 N8 O6 S2' _chemical_formula_weight 1399.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 16.995(4) _cell_length_b 13.564(3) _cell_length_c 27.388(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.097(3) _cell_angle_gamma 90.00 _cell_volume 6304(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2876 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8680 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69534 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.80 _reflns_number_total 14610 _reflns_number_gt 10438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains a disordered triflate anion. It was refined into to position with an independent free varaible. The sum of the occupancies of the two parts equals to 1. ; _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^)+(0.1251P)^2^+44.8241P] 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 14610 _refine_ls_number_parameters 851 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2770 _refine_ls_wR_factor_gt 0.2390 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.004 _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 S2 S 0.7638(2) 0.3866(5) 0.27625(13) 0.0581(14) Uani 0.559(6) 1 d PD A -1 C70 C 0.7790(9) 0.5213(10) 0.2723(6) 0.080(5) Uiso 0.559(6) 1 d PD A -1 F7 F 0.8002(7) 0.5704(10) 0.3138(4) 0.106(4) Uiso 0.559(6) 1 d PD A -1 F6 F 0.8221(7) 0.5506(10) 0.2393(5) 0.109(4) Uiso 0.559(6) 1 d PD A -1 O4 O 0.8445(5) 0.3633(7) 0.2854(3) 0.046(2) Uiso 0.559(6) 1 d PD A -1 O6 O 0.7135(5) 0.3885(7) 0.3149(3) 0.046(2) Uiso 0.559(6) 1 d PD A -1 F5 F 0.7077(8) 0.5760(11) 0.2648(5) 0.118(4) Uiso 0.559(6) 1 d PD A -1 O5 O 0.7297(5) 0.3505(8) 0.2290(3) 0.042(2) Uiso 0.559(6) 1 d PD A -1 F7' F 0.7515(9) 0.1589(12) 0.3052(6) 0.107(5) Uiso 0.441(6) 1 d PD A -2 F5' F 0.7681(11) 0.1717(14) 0.2337(6) 0.122(6) Uiso 0.441(6) 1 d PD A -2 F6' F 0.6416(4) 0.1288(5) 0.2727(2) 0.0281(17) Uiso 0.441(6) 1 d PD A -2 O5' O 0.7343(5) 0.3844(7) 0.2279(3) 0.0198(19) Uiso 0.441(6) 1 d PD A -2 O4' O 0.8434(6) 0.3033(9) 0.2795(4) 0.048(3) Uiso 0.441(6) 1 d PD A -2 O6' O 0.7158(10) 0.3113(14) 0.3145(6) 0.090(5) Uiso 0.441(6) 1 d PD A -2 S2' S 0.7610(3) 0.3266(4) 0.27448(16) 0.0390(11) Uani 0.441(6) 1 d PD A -2 C70' C 0.7071(12) 0.1999(15) 0.2650(9) 0.169(17) Uiso 0.441(6) 1 d PD A -2 Co1 Co 0.68999(3) 0.38267(5) 0.14315(2) 0.01767(17) Uani 1 1 d D . . C1 C 0.7427(3) 0.2665(3) 0.12327(17) 0.0187(9) Uani 1 1 d . A . C3 C 0.6301(3) 0.5003(3) 0.15124(17) 0.0195(9) Uani 1 1 d . A . C2 C 0.5953(3) 0.3103(3) 0.15958(17) 0.0187(9) Uani 1 1 d . A . C4 C 0.7872(3) 0.4524(4) 0.12954(17) 0.0200(9) Uani 1 1 d . A . C5 C 0.8419(3) 0.1606(3) 0.10723(17) 0.0185(9) Uani 1 1 d . A . C7 C 0.5004(3) 0.1983(4) 0.17698(17) 0.0193(9) Uani 1 1 d . A . C10 C 0.5609(3) 0.6402(3) 0.13325(17) 0.0190(9) Uani 1 1 d . A . C9 C 0.5300(3) 0.5993(3) 0.17282(17) 0.0189(9) Uani 1 1 d . A . C8 C 0.4913(3) 0.2770(3) 0.20610(17) 0.0175(9) Uani 1 1 d . A . C6 C 0.7769(3) 0.1323(3) 0.07969(18) 0.0195(9) Uani 1 1 d . A . C12 C 0.9211(3) 0.4711(4) 0.12819(18) 0.0209(9) Uani 1 1 d . A . C11 C 0.8868(3) 0.5546(4) 0.10981(17) 0.0200(9) Uani 1 1 d . A . C13 C 0.6354(3) 0.1985(4) 0.07075(17) 0.0189(9) Uani 1 1 d . A . H13A H 0.6316 0.1589 0.0403 0.023 Uiso 1 1 calc R . . H13B H 0.6192 0.2668 0.0623 0.023 Uiso 1 1 calc R . . C15 C 0.5595(3) 0.4398(3) 0.21960(17) 0.0197(9) Uani 1 1 d . A . H15A H 0.5118 0.4568 0.2370 0.024 Uiso 1 1 calc R . . H15B H 0.6047 0.4360 0.2439 0.024 Uiso 1 1 calc R . . C14 C 0.5794(3) 0.1566(4) 0.10645(18) 0.0227(10) Uani 1 1 d . A . H14A H 0.5288 0.1414 0.0884 0.027 Uiso 1 1 calc R . . H14B H 0.6015 0.0936 0.1193 0.027 Uiso 1 1 calc R . . C17 C 0.7522(3) 0.6166(4) 0.08851(19) 0.0240(10) Uani 1 1 d . A . H17A H 0.7745 0.6390 0.0578 0.029 Uiso 1 1 calc R . . H17B H 0.7515 0.6740 0.1108 0.029 Uiso 1 1 calc R . . C16 C 0.6682(3) 0.5848(4) 0.07697(17) 0.0211(9) Uani 1 1 d . A . H16A H 0.6424 0.6326 0.0540 0.025 Uiso 1 1 calc R . . H16B H 0.6681 0.5197 0.0606 0.025 Uiso 1 1 calc R . . C18 C 0.8696(3) 0.3116(3) 0.16132(18) 0.0203(9) Uani 1 1 d . A . H18A H 0.9254 0.2910 0.1601 0.024 Uiso 1 1 calc R . . H18B H 0.8557 0.3123 0.1960 0.024 Uiso 1 1 calc R . . C19 C 0.9219(3) 0.1181(4) 0.10972(18) 0.0212(9) Uani 1 1 d . . . C24 C 0.7665(3) 0.0527(4) 0.04323(18) 0.0209(9) Uani 1 1 d . . . C26 C 0.7598(4) -0.1192(4) 0.0216(2) 0.0382(14) Uani 1 1 d . . . H26 H 0.7636 -0.1866 0.0309 0.046 Uiso 1 1 calc R . . C27 C 0.7431(3) -0.0954(5) -0.0267(2) 0.0377(14) Uani 1 1 d . . . H27 H 0.7337 -0.1460 -0.0503 0.045 Uiso 1 1 calc R . . C25 C 0.7713(3) -0.0461(4) 0.0570(2) 0.0298(11) Uani 1 1 d . . . H25 H 0.7822 -0.0635 0.0903 0.036 Uiso 1 1 calc R . . C29 C 0.7529(3) 0.0763(4) -0.0059(2) 0.0289(11) Uani 1 1 d . . . H29 H 0.7526 0.1436 -0.0156 0.035 Uiso 1 1 calc R . . C21 C 1.0737(3) 0.0412(4) 0.1133(2) 0.0302(11) Uani 1 1 d . . . H21 H 1.1259 0.0159 0.1147 0.036 Uiso 1 1 calc R . . C28 C 0.7398(3) 0.0033(5) -0.0409(2) 0.0384(14) Uani 1 1 d . . . H28 H 0.7288 0.0204 -0.0742 0.046 Uiso 1 1 calc R . . C20 C 1.0318(3) 0.0433(4) 0.1546(2) 0.0304(11) Uani 1 1 d . . . H20 H 1.0548 0.0182 0.1845 0.037 Uiso 1 1 calc R . . C23 C 0.9640(3) 0.1141(4) 0.0677(2) 0.0318(12) Uani 1 1 d . . . H23 H 0.9407 0.1375 0.0376 0.038 Uiso 1 1 calc R . . C22 C 1.0399(3) 0.0759(4) 0.0695(2) 0.0351(13) Uani 1 1 d . . . H22 H 1.0686 0.0736 0.0407 0.042 Uiso 1 1 calc R . . C30 C 0.9558(3) 0.0820(4) 0.1534(2) 0.0268(10) Uani 1 1 d . . . H30 H 0.9273 0.0837 0.1822 0.032 Uiso 1 1 calc R . . C36 C 0.3748(3) 0.1037(4) 0.17054(18) 0.0236(10) Uani 1 1 d . . . H36 H 0.3468 0.1639 0.1659 0.028 Uiso 1 1 calc R . . C32 C 0.4970(3) 0.0154(4) 0.18232(19) 0.0255(10) Uani 1 1 d . . . H32 H 0.5528 0.0153 0.1866 0.031 Uiso 1 1 calc R . . C31 C 0.4571(3) 0.1042(4) 0.17565(18) 0.0219(10) Uani 1 1 d . . . C34 C 0.3744(3) -0.0729(4) 0.1780(2) 0.0335(12) Uani 1 1 d . . . H34 H 0.3465 -0.1335 0.1786 0.040 Uiso 1 1 calc R . . C35 C 0.3339(3) 0.0146(4) 0.1723(2) 0.0305(12) Uani 1 1 d . . . H35 H 0.2780 0.0144 0.1696 0.037 Uiso 1 1 calc R . . C33 C 0.4563(3) -0.0727(4) 0.1827(2) 0.0314(12) Uani 1 1 d . . . H33 H 0.4842 -0.1331 0.1863 0.038 Uiso 1 1 calc R . . C37 C 0.4347(3) 0.2933(3) 0.24480(17) 0.0194(9) Uani 1 1 d . . . C39 C 0.3949(3) 0.2659(4) 0.3267(2) 0.0309(12) Uani 1 1 d . . . H39 H 0.4043 0.2368 0.3580 0.037 Uiso 1 1 calc R . . C41 C 0.3136(3) 0.3623(4) 0.2709(2) 0.0274(11) Uani 1 1 d . . . H41 H 0.2674 0.4004 0.2642 0.033 Uiso 1 1 calc R . . C42 C 0.3667(3) 0.3482(4) 0.23460(19) 0.0258(10) Uani 1 1 d . . . H42 H 0.3566 0.3758 0.2030 0.031 Uiso 1 1 calc R . . C40 C 0.3279(3) 0.3214(4) 0.31659(19) 0.0270(11) Uani 1 1 d . . . H40 H 0.2915 0.3314 0.3412 0.032 Uiso 1 1 calc R . . C38 C 0.4486(3) 0.2529(4) 0.29062(19) 0.0279(11) Uani 1 1 d . . . H38 H 0.4953 0.2159 0.2977 0.033 Uiso 1 1 calc R . . C43 C 0.4656(3) 0.6330(3) 0.20302(17) 0.0182(9) Uani 1 1 d . . . C48 C 0.4813(3) 0.7002(4) 0.24058(19) 0.0242(10) Uani 1 1 d . . . H48 H 0.5332 0.7248 0.2467 0.029 Uiso 1 1 calc R . . C46 C 0.3452(3) 0.6964(4) 0.2604(2) 0.0285(11) Uani 1 1 d . . . H46 H 0.3043 0.7172 0.2804 0.034 Uiso 1 1 calc R . . C47 C 0.4209(3) 0.7317(4) 0.2692(2) 0.0307(11) Uani 1 1 d . . . H47 H 0.4318 0.7776 0.2949 0.037 Uiso 1 1 calc R . . C45 C 0.3291(3) 0.6310(4) 0.2226(2) 0.0336(12) Uani 1 1 d . . . H45 H 0.2768 0.6082 0.2161 0.040 Uiso 1 1 calc R . . C44 C 0.3891(3) 0.5982(4) 0.1940(2) 0.0294(11) Uani 1 1 d . . . H44 H 0.3779 0.5522 0.1684 0.035 Uiso 1 1 calc R . . C49 C 0.5357(3) 0.7281(4) 0.10517(17) 0.0211(9) Uani 1 1 d . . . C50 C 0.4568(3) 0.7369(4) 0.08891(19) 0.0245(10) Uani 1 1 d . . . H50 H 0.4208 0.6855 0.0952 0.029 Uiso 1 1 calc R . . C51 C 0.4305(3) 0.8199(4) 0.0637(2) 0.0306(11) Uani 1 1 d . . . H51 H 0.3763 0.8258 0.0537 0.037 Uiso 1 1 calc R . . C53 C 0.5613(3) 0.8864(4) 0.0686(2) 0.0300(11) Uani 1 1 d . . . H53 H 0.5972 0.9373 0.0614 0.036 Uiso 1 1 calc R . . C52 C 0.4822(3) 0.8942(4) 0.0530(2) 0.0324(12) Uani 1 1 d . . . H52 H 0.4639 0.9504 0.0350 0.039 Uiso 1 1 calc R . . C54 C 0.5876(3) 0.8042(4) 0.09465(19) 0.0261(10) Uani 1 1 d . . . H54 H 0.6415 0.7994 0.1055 0.031 Uiso 1 1 calc R . . C55 C 0.9249(3) 0.6431(4) 0.09054(18) 0.0211(9) Uani 1 1 d . . . C60 C 0.9790(3) 0.6329(4) 0.0541(2) 0.0263(10) Uani 1 1 d . . . H60 H 0.9894 0.5694 0.0413 0.032 Uiso 1 1 calc R . . C58 C 1.0018(3) 0.8072(4) 0.0550(2) 0.0314(12) Uani 1 1 d . . . H58 H 1.0279 0.8633 0.0429 0.038 Uiso 1 1 calc R . . C56 C 0.9099(3) 0.7373(4) 0.10886(19) 0.0254(10) Uani 1 1 d . . . H56 H 0.8734 0.7454 0.1336 0.030 Uiso 1 1 calc R . . C59 C 1.0177(3) 0.7142(4) 0.0365(2) 0.0307(11) Uani 1 1 d . . . H59 H 1.0547 0.7066 0.0121 0.037 Uiso 1 1 calc R . . C57 C 0.9484(3) 0.8187(4) 0.0907(2) 0.0297(11) Uani 1 1 d . . . H57 H 0.9379 0.8826 0.1030 0.036 Uiso 1 1 calc R . . C61 C 1.0051(3) 0.4466(4) 0.13623(19) 0.0251(10) Uani 1 1 d . . . C66 C 1.0422(3) 0.3834(5) 0.1047(2) 0.0382(14) Uani 1 1 d . . . H66 H 1.0129 0.3518 0.0787 0.046 Uiso 1 1 calc R . . C62 C 1.0480(3) 0.4898(4) 0.1748(3) 0.0384(14) Uani 1 1 d . . . H62 H 1.0225 0.5316 0.1968 0.046 Uiso 1 1 calc R . . C64 C 1.1651(4) 0.4117(6) 0.1498(3) 0.059(2) Uani 1 1 d . . . H64 H 1.2202 0.4005 0.1543 0.071 Uiso 1 1 calc R . . C65 C 1.1233(4) 0.3672(6) 0.1120(3) 0.052(2) Uani 1 1 d . . . H65 H 1.1495 0.3250 0.0904 0.063 Uiso 1 1 calc R . . C63 C 1.1284(4) 0.4723(6) 0.1814(3) 0.054(2) Uani 1 1 d . . . H63 H 1.1578 0.5023 0.2078 0.065 Uiso 1 1 calc R . . N1 N 0.8191(2) 0.2432(3) 0.13368(15) 0.0192(8) Uani 1 1 d . . . N2 N 0.7173(2) 0.1990(3) 0.09027(14) 0.0178(8) Uani 1 1 d . . . N8 N 0.8589(2) 0.4098(3) 0.14004(15) 0.0195(8) Uani 1 1 d . . . N3 N 0.5633(2) 0.2207(3) 0.14819(14) 0.0180(8) Uani 1 1 d . . . N6 N 0.6227(2) 0.5780(3) 0.12076(15) 0.0189(8) Uani 1 1 d . . . N5 N 0.5741(2) 0.5143(3) 0.18364(14) 0.0179(8) Uani 1 1 d . . . N7 N 0.8055(2) 0.5417(3) 0.11101(15) 0.0195(8) Uani 1 1 d . . . N4 N 0.5485(2) 0.3446(3) 0.19495(14) 0.0179(8) Uani 1 1 d . . . S1 S 0.36123(9) 0.34946(12) 0.07190(5) 0.0355(3) Uani 1 1 d . . . O3 O 0.3000(2) 0.3506(3) 0.03308(16) 0.0368(9) Uani 1 1 d . . . O2 O 0.3967(4) 0.2546(4) 0.0824(2) 0.0715(18) Uani 1 1 d . . . O1 O 0.3457(3) 0.4077(5) 0.11338(19) 0.0698(18) Uani 1 1 d . . . C67 C 0.4408(4) 0.4174(5) 0.0466(2) 0.0403(14) Uani 1 1 d . . . F2 F 0.4166(3) 0.5050(4) 0.0306(2) 0.0742(15) Uani 1 1 d . . . F3 F 0.5012(2) 0.4294(4) 0.07861(16) 0.0572(11) Uani 1 1 d . . . F1 F 0.4688(2) 0.3711(4) 0.00864(16) 0.0658(14) Uani 1 1 d . . . Cl1 Cl 0.25567(11) 0.16487(17) 0.41135(7) 0.0577(5) Uani 1 1 d . . . Cl2 Cl 0.28981(13) 0.11205(15) 0.51215(7) 0.0588(5) Uani 1 1 d . . . C69 C 0.2909(4) 0.0722(5) 0.4506(2) 0.0432(15) Uani 1 1 d . . . H69A H 0.3453 0.0547 0.4429 0.052 Uiso 1 1 calc R . . H69B H 0.2576 0.0127 0.4460 0.052 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 S2 0.0279(15) 0.121(5) 0.0256(15) 0.008(2) 0.0018(11) 0.016(2) S2' 0.0286(18) 0.063(3) 0.0266(18) 0.005(2) 0.0092(13) 0.009(2) Co1 0.0120(3) 0.0166(3) 0.0248(3) 0.0006(2) 0.0042(2) 0.0015(2) C1 0.015(2) 0.017(2) 0.025(2) 0.0049(17) 0.0055(17) 0.0005(16) C3 0.014(2) 0.020(2) 0.025(2) -0.0002(18) 0.0034(17) -0.0008(17) C2 0.014(2) 0.018(2) 0.025(2) -0.0001(17) 0.0037(17) 0.0031(17) C4 0.014(2) 0.022(2) 0.024(2) -0.0014(18) 0.0040(17) 0.0031(17) C5 0.018(2) 0.016(2) 0.022(2) 0.0012(17) 0.0026(17) 0.0019(17) C7 0.014(2) 0.021(2) 0.023(2) 0.0014(18) 0.0045(17) 0.0003(17) C10 0.016(2) 0.016(2) 0.025(2) -0.0024(17) 0.0015(17) -0.0003(17) C9 0.015(2) 0.016(2) 0.025(2) -0.0046(17) 0.0016(17) -0.0005(16) C8 0.0135(19) 0.017(2) 0.023(2) 0.0026(17) 0.0032(16) 0.0035(16) C6 0.015(2) 0.018(2) 0.025(2) 0.0028(18) 0.0022(17) 0.0040(17) C12 0.014(2) 0.021(2) 0.027(2) -0.0010(18) 0.0032(17) -0.0031(17) C11 0.014(2) 0.021(2) 0.025(2) -0.0027(18) 0.0031(17) 0.0005(17) C13 0.013(2) 0.022(2) 0.022(2) -0.0008(18) 0.0028(16) 0.0023(17) C15 0.019(2) 0.019(2) 0.021(2) -0.0005(17) 0.0041(17) -0.0006(17) C14 0.022(2) 0.020(2) 0.027(2) -0.0045(19) 0.0088(18) -0.0023(18) C17 0.018(2) 0.023(2) 0.032(3) 0.006(2) 0.0045(19) 0.0019(19) C16 0.018(2) 0.022(2) 0.023(2) 0.0011(18) 0.0053(17) 0.0022(18) C18 0.014(2) 0.019(2) 0.027(2) 0.0015(18) -0.0015(17) 0.0002(17) C19 0.015(2) 0.019(2) 0.030(2) -0.0016(19) 0.0049(18) 0.0005(17) C24 0.0113(19) 0.020(2) 0.032(3) -0.0013(19) 0.0059(17) 0.0039(17) C26 0.039(3) 0.022(3) 0.054(4) -0.009(3) 0.015(3) -0.005(2) C27 0.029(3) 0.037(3) 0.048(4) -0.021(3) 0.007(2) -0.001(2) C25 0.030(3) 0.024(3) 0.037(3) 0.003(2) 0.010(2) 0.002(2) C29 0.025(2) 0.029(3) 0.033(3) -0.004(2) 0.001(2) 0.010(2) C21 0.016(2) 0.026(3) 0.049(3) -0.003(2) 0.003(2) 0.0043(19) C28 0.030(3) 0.049(4) 0.036(3) -0.011(3) 0.000(2) 0.014(3) C20 0.024(2) 0.033(3) 0.034(3) -0.001(2) -0.003(2) 0.010(2) C23 0.024(3) 0.034(3) 0.037(3) 0.007(2) 0.007(2) 0.007(2) C22 0.025(3) 0.036(3) 0.046(3) 0.004(3) 0.015(2) 0.005(2) C30 0.022(2) 0.029(3) 0.029(3) -0.001(2) 0.0015(19) 0.005(2) C36 0.021(2) 0.025(2) 0.025(2) 0.0021(19) 0.0060(18) -0.0033(19) C32 0.023(2) 0.023(2) 0.032(3) 0.002(2) 0.0106(19) 0.0001(19) C31 0.022(2) 0.021(2) 0.023(2) -0.0023(18) 0.0065(18) -0.0022(18) C34 0.039(3) 0.026(3) 0.037(3) -0.002(2) 0.014(2) -0.015(2) C35 0.026(3) 0.038(3) 0.029(3) 0.000(2) 0.008(2) -0.013(2) C33 0.037(3) 0.021(3) 0.038(3) 0.002(2) 0.014(2) -0.001(2) C37 0.014(2) 0.020(2) 0.025(2) -0.0012(18) 0.0053(17) -0.0023(17) C39 0.029(3) 0.039(3) 0.025(3) 0.008(2) 0.007(2) 0.001(2) C41 0.018(2) 0.029(3) 0.036(3) 0.000(2) 0.008(2) 0.0054(19) C42 0.021(2) 0.030(3) 0.027(2) 0.006(2) 0.0028(19) 0.007(2) C40 0.023(2) 0.030(3) 0.030(3) -0.002(2) 0.0095(19) -0.003(2) C38 0.023(2) 0.033(3) 0.027(3) 0.005(2) 0.0025(19) 0.005(2) C43 0.018(2) 0.013(2) 0.025(2) -0.0005(17) 0.0045(17) 0.0024(16) C48 0.021(2) 0.022(2) 0.030(3) -0.0038(19) 0.0021(19) 0.0002(19) C46 0.022(2) 0.029(3) 0.036(3) 0.004(2) 0.010(2) 0.011(2) C47 0.032(3) 0.030(3) 0.030(3) -0.010(2) 0.004(2) 0.007(2) C45 0.018(2) 0.032(3) 0.052(3) -0.006(2) 0.010(2) 0.001(2) C44 0.021(2) 0.025(3) 0.043(3) -0.012(2) 0.005(2) -0.003(2) C49 0.019(2) 0.021(2) 0.023(2) -0.0025(18) 0.0048(17) 0.0040(18) C50 0.020(2) 0.023(2) 0.030(3) 0.000(2) 0.0023(19) 0.0024(19) C51 0.025(3) 0.035(3) 0.032(3) 0.001(2) 0.001(2) 0.010(2) C53 0.032(3) 0.022(2) 0.036(3) 0.003(2) 0.011(2) 0.002(2) C52 0.035(3) 0.028(3) 0.034(3) 0.006(2) 0.005(2) 0.011(2) C54 0.023(2) 0.024(2) 0.032(3) 0.000(2) 0.0044(19) 0.002(2) C55 0.017(2) 0.022(2) 0.025(2) -0.0013(18) 0.0019(17) -0.0022(18) C60 0.026(2) 0.021(2) 0.032(3) -0.002(2) 0.005(2) -0.0015(19) C58 0.033(3) 0.025(3) 0.037(3) 0.003(2) 0.006(2) -0.010(2) C56 0.021(2) 0.027(3) 0.029(3) -0.005(2) 0.0045(19) -0.0015(19) C59 0.031(3) 0.032(3) 0.031(3) 0.001(2) 0.010(2) -0.007(2) C57 0.031(3) 0.020(2) 0.039(3) -0.003(2) 0.003(2) -0.004(2) C61 0.014(2) 0.026(2) 0.036(3) 0.009(2) 0.0046(19) -0.0014(18) C66 0.028(3) 0.054(4) 0.034(3) 0.009(3) 0.009(2) 0.016(3) C62 0.027(3) 0.029(3) 0.058(4) 0.007(3) -0.010(3) -0.007(2) C64 0.014(3) 0.080(6) 0.082(5) 0.056(5) 0.004(3) -0.002(3) C65 0.031(3) 0.074(5) 0.054(4) 0.030(4) 0.019(3) 0.026(3) C63 0.026(3) 0.050(4) 0.083(5) 0.028(4) -0.022(3) -0.018(3) N1 0.0163(18) 0.0165(19) 0.025(2) 0.0013(15) 0.0035(15) 0.0021(15) N2 0.0117(17) 0.0173(18) 0.0247(19) 0.0002(15) 0.0043(14) 0.0033(14) N8 0.0133(17) 0.0195(19) 0.026(2) 0.0016(16) 0.0036(15) 0.0023(15) N3 0.0141(17) 0.0156(18) 0.0249(19) 0.0011(15) 0.0061(14) 0.0023(14) N6 0.0135(17) 0.0174(19) 0.026(2) -0.0010(15) 0.0039(15) 0.0000(14) N5 0.0135(17) 0.0165(18) 0.0239(19) -0.0010(15) 0.0029(14) 0.0020(14) N7 0.0128(17) 0.0191(19) 0.027(2) 0.0003(16) 0.0048(15) 0.0008(15) N4 0.0140(17) 0.0169(18) 0.0230(19) -0.0005(15) 0.0029(14) 0.0007(14) S1 0.0361(7) 0.0382(8) 0.0323(7) 0.0040(6) 0.0024(6) -0.0094(6) O3 0.031(2) 0.040(2) 0.039(2) 0.0003(18) 0.0014(17) -0.0058(18) O2 0.071(4) 0.044(3) 0.095(4) 0.026(3) -0.037(3) -0.010(3) O1 0.057(3) 0.111(5) 0.042(3) -0.018(3) 0.008(2) -0.021(3) C67 0.035(3) 0.048(4) 0.037(3) 0.006(3) -0.001(2) -0.007(3) F2 0.075(3) 0.055(3) 0.090(4) 0.030(3) -0.021(3) -0.027(2) F3 0.042(2) 0.074(3) 0.054(2) -0.004(2) -0.0157(18) -0.014(2) F1 0.034(2) 0.117(4) 0.048(2) -0.017(2) 0.0154(17) -0.009(2) Cl1 0.0470(9) 0.0743(13) 0.0520(10) 0.0200(9) 0.0048(8) 0.0060(9) Cl2 0.0764(13) 0.0608(11) 0.0409(9) 0.0075(8) 0.0190(9) -0.0121(10) C69 0.042(3) 0.043(4) 0.045(4) -0.002(3) 0.003(3) -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 S2 O6 1.396(8) . ? S2 O4 1.417(9) . ? S2 O5 1.472(9) . ? S2 C70 1.849(14) . ? C70 F6 1.258(15) . ? C70 F7 1.349(15) . ? C70 F5 1.425(15) . ? F7' C70' 1.415(19) . ? F5' C70' 1.432(19) . ? F6' C70' 1.496(15) . ? O5' S2' 1.546(9) . ? O5' Co1 2.401(7) . ? O4' S2' 1.435(11) . ? O6' S2' 1.388(14) . ? S2' C70' 1.958(16) . ? Co1 C1 1.907(5) . ? Co1 C3 1.913(5) . ? Co1 C4 1.957(5) . ? Co1 C2 1.958(5) . ? C1 N2 1.341(6) . ? C1 N1 1.352(6) . ? C3 N6 1.346(6) . ? C3 N5 1.349(6) . ? C2 N3 1.362(6) . ? C2 N4 1.368(6) . ? C4 N7 1.355(6) . ? C4 N8 1.366(6) . ? C5 C6 1.359(7) . ? C5 N1 1.400(6) . ? C5 C19 1.475(6) . ? C7 C8 1.346(7) . ? C7 N3 1.397(6) . ? C7 C31 1.474(7) . ? C10 C9 1.349(7) . ? C10 N6 1.404(6) . ? C10 C49 1.470(7) . ? C9 N5 1.398(6) . ? C9 C43 1.479(6) . ? C8 N4 1.382(6) . ? C8 C37 1.487(6) . ? C6 N2 1.400(6) . ? C6 C24 1.475(7) . ? C12 C11 1.358(7) . ? C12 N8 1.397(6) . ? C12 C61 1.470(6) . ? C11 N7 1.395(6) . ? C11 C55 1.475(7) . ? C13 N2 1.465(6) . ? C13 C14 1.511(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 N5 1.442(6) . ? C15 N4 1.464(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C14 N3 1.473(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C17 N7 1.474(6) . ? C17 C16 1.509(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C16 N6 1.464(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 N1 1.449(6) . ? C18 N8 1.461(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C30 1.387(7) . ? C19 C23 1.388(7) . ? C24 C29 1.390(7) . ? C24 C25 1.393(7) . ? C26 C27 1.377(10) . ? C26 C25 1.395(8) . ? C26 H26 0.9500 . ? C27 C28 1.393(9) . ? C27 H27 0.9500 . ? C25 H25 0.9500 . ? C29 C28 1.388(8) . ? C29 H29 0.9500 . ? C21 C20 1.370(8) . ? C21 C22 1.385(8) . ? C21 H21 0.9500 . ? C28 H28 0.9500 . ? C20 C30 1.393(7) . ? C20 H20 0.9500 . ? C23 C22 1.388(7) . ? C23 H23 0.9500 . ? C22 H22 0.9500 . ? C30 H30 0.9500 . ? C36 C35 1.396(7) . ? C36 C31 1.398(7) . ? C36 H36 0.9500 . ? C32 C33 1.381(7) . ? C32 C31 1.389(7) . ? C32 H32 0.9500 . ? C34 C35 1.377(9) . ? C34 C33 1.389(8) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C33 H33 0.9500 . ? C37 C38 1.378(7) . ? C37 C42 1.389(7) . ? C39 C40 1.381(8) . ? C39 C38 1.391(7) . ? C39 H39 0.9500 . ? C41 C40 1.378(8) . ? C41 C42 1.392(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C40 H40 0.9500 . ? C38 H38 0.9500 . ? C43 C48 1.390(7) . ? C43 C44 1.392(7) . ? C48 C47 1.392(7) . ? C48 H48 0.9500 . ? C46 C45 1.379(8) . ? C46 C47 1.381(8) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C45 C44 1.393(7) . ? C45 H45 0.9500 . ? C44 H44 0.9500 . ? C49 C50 1.395(7) . ? C49 C54 1.398(7) . ? C50 C51 1.381(7) . ? C50 H50 0.9500 . ? C51 C52 1.379(8) . ? C51 H51 0.9500 . ? C53 C54 1.384(7) . ? C53 C52 1.394(8) . ? C53 H53 0.9500 . ? C52 H52 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.400(7) . ? C55 C56 1.400(7) . ? C60 C59 1.383(7) . ? C60 H60 0.9500 . ? C58 C57 1.378(8) . ? C58 C59 1.392(8) . ? C58 H58 0.9500 . ? C56 C57 1.389(7) . ? C56 H56 0.9500 . ? C59 H59 0.9500 . ? C57 H57 0.9500 . ? C61 C62 1.381(8) . ? C61 C66 1.391(8) . ? C66 C65 1.400(8) . ? C66 H66 0.9500 . ? C62 C63 1.388(8) . ? C62 H62 0.9500 . ? C64 C65 1.365(12) . ? C64 C63 1.367(12) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C63 H63 0.9500 . ? S1 O1 1.420(6) . ? S1 O2 1.444(6) . ? S1 O3 1.447(4) . ? S1 C67 1.806(6) . ? C67 F3 1.324(7) . ? C67 F1 1.324(8) . ? C67 F2 1.324(8) . ? Cl1 C69 1.739(7) . ? Cl2 C69 1.771(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 S2 O4 119.8(6) . . ? O6 S2 O5 116.3(6) . . ? O4 S2 O5 114.4(6) . . ? O6 S2 C70 96.9(7) . . ? O4 S2 C70 95.4(7) . . ? O5 S2 C70 109.1(7) . . ? F6 C70 F7 108.1(13) . . ? F6 C70 F5 104.8(13) . . ? F7 C70 F5 93.0(12) . . ? F6 C70 S2 116.2(12) . . ? F7 C70 S2 118.1(12) . . ? F5 C70 S2 113.7(11) . . ? S2' O5' Co1 148.9(6) . . ? O6' S2' O4' 118.1(9) . . ? O6' S2' O5' 125.3(9) . . ? O4' S2' O5' 115.6(6) . . ? O6' S2' C70' 72.5(11) . . ? O4' S2' C70' 105.5(9) . . ? O5' S2' C70' 102.8(9) . . ? F7' C70' F5' 89.3(16) . . ? F7' C70' F6' 90.4(13) . . ? F5' C70' F6' 118.8(16) . . ? F7' C70' S2' 90.8(12) . . ? F5' C70' S2' 88.0(11) . . ? F6' C70' S2' 153.2(17) . . ? C1 Co1 C3 169.8(2) . . ? C1 Co1 C4 86.03(19) . . ? C3 Co1 C4 94.51(19) . . ? C1 Co1 C2 93.23(19) . . ? C3 Co1 C2 86.68(19) . . ? C4 Co1 C2 177.3(2) . . ? C1 Co1 O5' 99.0(3) . . ? C3 Co1 O5' 91.2(3) . . ? C4 Co1 O5' 87.5(3) . . ? C2 Co1 O5' 90.1(3) . . ? N2 C1 N1 104.7(4) . . ? N2 C1 Co1 128.1(3) . . ? N1 C1 Co1 126.4(4) . . ? N6 C3 N5 104.7(4) . . ? N6 C3 Co1 127.9(3) . . ? N5 C3 Co1 126.3(3) . . ? N3 C2 N4 103.1(4) . . ? N3 C2 Co1 135.9(3) . . ? N4 C2 Co1 120.6(3) . . ? N7 C4 N8 103.7(4) . . ? N7 C4 Co1 135.8(3) . . ? N8 C4 Co1 120.5(3) . . ? C6 C5 N1 105.9(4) . . ? C6 C5 C19 129.4(4) . . ? N1 C5 C19 124.7(4) . . ? C8 C7 N3 106.1(4) . . ? C8 C7 C31 129.0(4) . . ? N3 C7 C31 124.8(4) . . ? C9 C10 N6 106.2(4) . . ? C9 C10 C49 129.6(4) . . ? N6 C10 C49 124.1(4) . . ? C10 C9 N5 106.3(4) . . ? C10 C9 C43 130.9(4) . . ? N5 C9 C43 122.7(4) . . ? C7 C8 N4 107.0(4) . . ? C7 C8 C37 129.7(4) . . ? N4 C8 C37 123.3(4) . . ? C5 C6 N2 106.1(4) . . ? C5 C6 C24 130.3(4) . . ? N2 C6 C24 123.5(4) . . ? C11 C12 N8 105.6(4) . . ? C11 C12 C61 129.6(4) . . ? N8 C12 C61 124.8(4) . . ? C12 C11 N7 107.0(4) . . ? C12 C11 C55 128.6(4) . . ? N7 C11 C55 124.4(4) . . ? N2 C13 C14 112.6(4) . . ? N2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N5 C15 N4 109.0(4) . . ? N5 C15 H15A 109.9 . . ? N4 C15 H15A 109.9 . . ? N5 C15 H15B 109.9 . . ? N4 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N3 C14 C13 115.5(4) . . ? N3 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? N3 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? N7 C17 C16 116.4(4) . . ? N7 C17 H17A 108.2 . . ? C16 C17 H17A 108.2 . . ? N7 C17 H17B 108.2 . . ? C16 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? N6 C16 C17 112.4(4) . . ? N6 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N6 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? N1 C18 N8 108.5(4) . . ? N1 C18 H18A 110.0 . . ? N8 C18 H18A 110.0 . . ? N1 C18 H18B 110.0 . . ? N8 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C30 C19 C23 119.4(5) . . ? C30 C19 C5 121.1(4) . . ? C23 C19 C5 119.5(5) . . ? C29 C24 C25 119.3(5) . . ? C29 C24 C6 119.6(4) . . ? C25 C24 C6 121.1(5) . . ? C27 C26 C25 121.1(6) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 119.7(5) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C24 C25 C26 119.4(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C28 C29 C24 121.0(5) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? C20 C21 C22 119.9(5) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C29 C28 C27 119.4(6) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C21 C20 C30 120.7(5) . . ? C21 C20 H20 119.7 . . ? C30 C20 H20 119.7 . . ? C19 C23 C22 120.3(5) . . ? C19 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C19 C30 C20 119.7(5) . . ? C19 C30 H30 120.1 . . ? C20 C30 H30 120.1 . . ? C35 C36 C31 119.8(5) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C33 C32 C31 120.6(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C31 C36 119.2(5) . . ? C32 C31 C7 120.6(4) . . ? C36 C31 C7 120.1(4) . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C32 C33 C34 120.0(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C38 C37 C42 119.8(4) . . ? C38 C37 C8 120.2(4) . . ? C42 C37 C8 120.0(4) . . ? C40 C39 C38 119.5(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C40 C41 C42 120.3(5) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 119.6(5) . . ? C37 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C41 C40 C39 120.3(5) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C37 C38 C39 120.6(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C48 C43 C44 119.6(4) . . ? C48 C43 C9 119.9(4) . . ? C44 C43 C9 120.5(4) . . ? C43 C48 C47 120.1(5) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C45 C46 C47 119.9(5) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.2(5) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C46 C45 C44 120.5(5) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C43 C44 C45 119.7(5) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C50 C49 C54 118.5(5) . . ? C50 C49 C10 119.0(4) . . ? C54 C49 C10 122.5(4) . . ? C51 C50 C49 120.6(5) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C52 C51 C50 120.7(5) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C54 C53 C52 119.9(5) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C51 C52 C53 119.6(5) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C53 C54 C49 120.7(5) . . ? C53 C54 H54 119.6 . . ? C49 C54 H54 119.6 . . ? C60 C55 C56 119.1(4) . . ? C60 C55 C11 119.5(4) . . ? C56 C55 C11 121.4(4) . . ? C59 C60 C55 120.7(5) . . ? C59 C60 H60 119.6 . . ? C55 C60 H60 119.6 . . ? C57 C58 C59 120.5(5) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C57 C56 C55 119.9(5) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C60 C59 C58 119.5(5) . . ? C60 C59 H59 120.3 . . ? C58 C59 H59 120.3 . . ? C58 C57 C56 120.3(5) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C62 C61 C66 119.8(5) . . ? C62 C61 C12 119.2(5) . . ? C66 C61 C12 121.0(5) . . ? C61 C66 C65 119.0(6) . . ? C61 C66 H66 120.5 . . ? C65 C66 H66 120.5 . . ? C61 C62 C63 120.2(7) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C65 C64 C63 120.6(6) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? C64 C65 C66 120.4(7) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C64 C63 C62 119.9(7) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C1 N1 C5 111.6(4) . . ? C1 N1 C18 119.7(4) . . ? C5 N1 C18 127.6(4) . . ? C1 N2 C6 111.7(4) . . ? C1 N2 C13 121.0(4) . . ? C6 N2 C13 127.3(4) . . ? C4 N8 C12 112.1(4) . . ? C4 N8 C18 124.1(4) . . ? C12 N8 C18 123.8(4) . . ? C2 N3 C7 111.9(4) . . ? C2 N3 C14 128.1(4) . . ? C7 N3 C14 119.4(4) . . ? C3 N6 C10 111.4(4) . . ? C3 N6 C16 121.5(4) . . ? C10 N6 C16 126.6(4) . . ? C3 N5 C9 111.4(4) . . ? C3 N5 C15 120.3(4) . . ? C9 N5 C15 127.8(4) . . ? C4 N7 C11 111.6(4) . . ? C4 N7 C17 128.6(4) . . ? C11 N7 C17 119.4(4) . . ? C2 N4 C8 111.9(4) . . ? C2 N4 C15 124.1(4) . . ? C8 N4 C15 123.9(4) . . ? O1 S1 O2 115.5(4) . . ? O1 S1 O3 115.1(3) . . ? O2 S1 O3 115.6(3) . . ? O1 S1 C67 101.5(3) . . ? O2 S1 C67 102.6(4) . . ? O3 S1 C67 103.7(3) . . ? F3 C67 F1 106.3(5) . . ? F3 C67 F2 108.9(6) . . ? F1 C67 F2 106.6(6) . . ? F3 C67 S1 112.2(4) . . ? F1 C67 S1 111.6(5) . . ? F2 C67 S1 111.0(5) . . ? Cl1 C69 Cl2 110.3(4) . . ? Cl1 C69 H69A 109.6 . . ? Cl2 C69 H69A 109.6 . . ? Cl1 C69 H69B 109.6 . . ? Cl2 C69 H69B 109.6 . . ? H69A C69 H69B 108.1 . . ? 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 O6 S2 C70 F6 -178.6(13) . . . . ? O4 S2 C70 F6 60.5(14) . . . . ? O5 S2 C70 F6 -57.6(14) . . . . ? O6 S2 C70 F7 50.6(13) . . . . ? O4 S2 C70 F7 -70.3(13) . . . . ? O5 S2 C70 F7 171.6(11) . . . . ? O6 S2 C70 F5 -56.8(12) . . . . ? O4 S2 C70 F5 -177.7(11) . . . . ? O5 S2 C70 F5 64.2(12) . . . . ? Co1 O5' S2' O6' -105.1(14) . . . . ? Co1 O5' S2' O4' 86.7(12) . . . . ? Co1 O5' S2' C70' -27.7(13) . . . . ? O6' S2' C70' F7' -66.9(14) . . . . ? O4' S2' C70' F7' 48.3(14) . . . . ? O5' S2' C70' F7' 169.8(11) . . . . ? O6' S2' C70' F5' -156.2(16) . . . . ? O4' S2' C70' F5' -41.1(14) . . . . ? O5' S2' C70' F5' 80.5(13) . . . . ? O6' S2' C70' F6' 26(4) . . . . ? O4' S2' C70' F6' 141(3) . . . . ? O5' S2' C70' F6' -98(4) . . . . ? S2' O5' Co1 C1 -30.5(10) . . . . ? S2' O5' Co1 C3 149.4(10) . . . . ? S2' O5' Co1 C4 -116.1(10) . . . . ? S2' O5' Co1 C2 62.8(10) . . . . ? C3 Co1 C1 N2 -35.1(13) . . . . ? C4 Co1 C1 N2 -128.5(4) . . . . ? C2 Co1 C1 N2 54.1(4) . . . . ? O5' Co1 C1 N2 144.7(4) . . . . ? C3 Co1 C1 N1 133.2(10) . . . . ? C4 Co1 C1 N1 39.8(4) . . . . ? C2 Co1 C1 N1 -137.6(4) . . . . ? O5' Co1 C1 N1 -47.0(5) . . . . ? C1 Co1 C3 N6 -41.5(13) . . . . ? C4 Co1 C3 N6 51.1(4) . . . . ? C2 Co1 C3 N6 -131.3(4) . . . . ? O5' Co1 C3 N6 138.7(5) . . . . ? C1 Co1 C3 N5 124.1(10) . . . . ? C4 Co1 C3 N5 -143.2(4) . . . . ? C2 Co1 C3 N5 34.3(4) . . . . ? O5' Co1 C3 N5 -55.7(5) . . . . ? C1 Co1 C2 N3 -19.2(5) . . . . ? C3 Co1 C2 N3 150.6(5) . . . . ? C4 Co1 C2 N3 -93(4) . . . . ? O5' Co1 C2 N3 -118.3(5) . . . . ? C1 Co1 C2 N4 151.5(4) . . . . ? C3 Co1 C2 N4 -38.7(4) . . . . ? C4 Co1 C2 N4 77(4) . . . . ? O5' Co1 C2 N4 52.4(4) . . . . ? C1 Co1 C4 N7 143.6(5) . . . . ? C3 Co1 C4 N7 -26.2(5) . . . . ? C2 Co1 C4 N7 -142(4) . . . . ? O5' Co1 C4 N7 -117.2(5) . . . . ? C1 Co1 C4 N8 -37.4(4) . . . . ? C3 Co1 C4 N8 152.8(4) . . . . ? C2 Co1 C4 N8 37(4) . . . . ? O5' Co1 C4 N8 61.8(4) . . . . ? N6 C10 C9 N5 0.6(5) . . . . ? C49 C10 C9 N5 177.3(5) . . . . ? N6 C10 C9 C43 177.8(5) . . . . ? C49 C10 C9 C43 -5.6(9) . . . . ? N3 C7 C8 N4 -0.4(5) . . . . ? C31 C7 C8 N4 177.0(5) . . . . ? N3 C7 C8 C37 -178.5(4) . . . . ? C31 C7 C8 C37 -1.1(8) . . . . ? N1 C5 C6 N2 0.3(5) . . . . ? C19 C5 C6 N2 -178.4(5) . . . . ? N1 C5 C6 C24 177.1(5) . . . . ? C19 C5 C6 C24 -1.6(9) . . . . ? N8 C12 C11 N7 0.0(5) . . . . ? C61 C12 C11 N7 -178.4(5) . . . . ? N8 C12 C11 C55 -178.5(5) . . . . ? C61 C12 C11 C55 3.1(9) . . . . ? N2 C13 C14 N3 73.4(5) . . . . ? N7 C17 C16 N6 74.9(5) . . . . ? C6 C5 C19 C30 -120.7(6) . . . . ? N1 C5 C19 C30 60.8(7) . . . . ? C6 C5 C19 C23 59.2(7) . . . . ? N1 C5 C19 C23 -119.3(6) . . . . ? C5 C6 C24 C29 -111.2(6) . . . . ? N2 C6 C24 C29 65.1(6) . . . . ? C5 C6 C24 C25 67.8(7) . . . . ? N2 C6 C24 C25 -115.9(5) . . . . ? C25 C26 C27 C28 2.0(9) . . . . ? C29 C24 C25 C26 -2.1(8) . . . . ? C6 C24 C25 C26 179.0(5) . . . . ? C27 C26 C25 C24 -0.7(9) . . . . ? C25 C24 C29 C28 3.5(8) . . . . ? C6 C24 C29 C28 -177.5(5) . . . . ? C24 C29 C28 C27 -2.2(8) . . . . ? C26 C27 C28 C29 -0.6(9) . . . . ? C22 C21 C20 C30 -1.3(9) . . . . ? C30 C19 C23 C22 -1.2(8) . . . . ? C5 C19 C23 C22 178.9(5) . . . . ? C20 C21 C22 C23 0.9(9) . . . . ? C19 C23 C22 C21 0.4(9) . . . . ? C23 C19 C30 C20 0.8(8) . . . . ? C5 C19 C30 C20 -179.3(5) . . . . ? C21 C20 C30 C19 0.5(8) . . . . ? C33 C32 C31 C36 1.6(8) . . . . ? C33 C32 C31 C7 177.8(5) . . . . ? C35 C36 C31 C32 0.2(7) . . . . ? C35 C36 C31 C7 -176.1(5) . . . . ? C8 C7 C31 C32 -122.5(6) . . . . ? N3 C7 C31 C32 54.4(7) . . . . ? C8 C7 C31 C36 53.7(7) . . . . ? N3 C7 C31 C36 -129.4(5) . . . . ? C33 C34 C35 C36 1.1(8) . . . . ? C31 C36 C35 C34 -1.5(8) . . . . ? C31 C32 C33 C34 -2.0(8) . . . . ? C35 C34 C33 C32 0.7(9) . . . . ? C7 C8 C37 C38 79.8(7) . . . . ? N4 C8 C37 C38 -98.0(6) . . . . ? C7 C8 C37 C42 -99.1(6) . . . . ? N4 C8 C37 C42 83.0(6) . . . . ? C38 C37 C42 C41 0.5(8) . . . . ? C8 C37 C42 C41 179.4(5) . . . . ? C40 C41 C42 C37 -0.7(8) . . . . ? C42 C41 C40 C39 -0.1(8) . . . . ? C38 C39 C40 C41 1.0(9) . . . . ? C42 C37 C38 C39 0.5(8) . . . . ? C8 C37 C38 C39 -178.4(5) . . . . ? C40 C39 C38 C37 -1.3(9) . . . . ? C10 C9 C43 C48 -84.0(7) . . . . ? N5 C9 C43 C48 92.8(6) . . . . ? C10 C9 C43 C44 95.8(6) . . . . ? N5 C9 C43 C44 -87.5(6) . . . . ? C44 C43 C48 C47 0.6(8) . . . . ? C9 C43 C48 C47 -179.7(5) . . . . ? C45 C46 C47 C48 -1.1(9) . . . . ? C43 C48 C47 C46 -0.1(8) . . . . ? C47 C46 C45 C44 1.7(9) . . . . ? C48 C43 C44 C45 0.0(8) . . . . ? C9 C43 C44 C45 -179.7(5) . . . . ? C46 C45 C44 C43 -1.2(9) . . . . ? C9 C10 C49 C50 -50.6(7) . . . . ? N6 C10 C49 C50 125.6(5) . . . . ? C9 C10 C49 C54 128.5(6) . . . . ? N6 C10 C49 C54 -55.4(7) . . . . ? C54 C49 C50 C51 -1.1(7) . . . . ? C10 C49 C50 C51 178.0(5) . . . . ? C49 C50 C51 C52 1.8(8) . . . . ? C50 C51 C52 C53 -1.3(8) . . . . ? C54 C53 C52 C51 0.1(8) . . . . ? C52 C53 C54 C49 0.6(8) . . . . ? C50 C49 C54 C53 -0.2(7) . . . . ? C10 C49 C54 C53 -179.2(5) . . . . ? C12 C11 C55 C60 52.9(7) . . . . ? N7 C11 C55 C60 -125.4(5) . . . . ? C12 C11 C55 C56 -125.3(6) . . . . ? N7 C11 C55 C56 56.5(7) . . . . ? C56 C55 C60 C59 0.4(8) . . . . ? C11 C55 C60 C59 -177.8(5) . . . . ? C60 C55 C56 C57 0.1(8) . . . . ? C11 C55 C56 C57 178.3(5) . . . . ? C55 C60 C59 C58 -0.7(8) . . . . ? C57 C58 C59 C60 0.4(9) . . . . ? C59 C58 C57 C56 0.2(9) . . . . ? C55 C56 C57 C58 -0.4(8) . . . . ? C11 C12 C61 C62 74.2(7) . . . . ? N8 C12 C61 C62 -103.9(6) . . . . ? C11 C12 C61 C66 -103.6(7) . . . . ? N8 C12 C61 C66 78.3(7) . . . . ? C62 C61 C66 C65 -1.8(9) . . . . ? C12 C61 C66 C65 175.9(5) . . . . ? C66 C61 C62 C63 1.5(9) . . . . ? C12 C61 C62 C63 -176.2(5) . . . . ? C63 C64 C65 C66 0.4(10) . . . . ? C61 C66 C65 C64 0.9(10) . . . . ? C65 C64 C63 C62 -0.7(10) . . . . ? C61 C62 C63 C64 -0.3(10) . . . . ? N2 C1 N1 C5 -0.1(5) . . . . ? Co1 C1 N1 C5 -170.6(3) . . . . ? N2 C1 N1 C18 168.5(4) . . . . ? Co1 C1 N1 C18 -2.0(6) . . . . ? C6 C5 N1 C1 -0.1(5) . . . . ? C19 C5 N1 C1 178.7(4) . . . . ? C6 C5 N1 C18 -167.6(4) . . . . ? C19 C5 N1 C18 11.2(7) . . . . ? N8 C18 N1 C1 -47.9(5) . . . . ? N8 C18 N1 C5 118.7(5) . . . . ? N1 C1 N2 C6 0.3(5) . . . . ? Co1 C1 N2 C6 170.6(3) . . . . ? N1 C1 N2 C13 178.4(4) . . . . ? Co1 C1 N2 C13 -11.3(6) . . . . ? C5 C6 N2 C1 -0.4(5) . . . . ? C24 C6 N2 C1 -177.5(4) . . . . ? C5 C6 N2 C13 -178.4(4) . . . . ? C24 C6 N2 C13 4.6(7) . . . . ? C14 C13 N2 C1 -76.4(5) . . . . ? C14 C13 N2 C6 101.4(5) . . . . ? N7 C4 N8 C12 -0.1(5) . . . . ? Co1 C4 N8 C12 -179.4(3) . . . . ? N7 C4 N8 C18 179.7(4) . . . . ? Co1 C4 N8 C18 0.4(6) . . . . ? C11 C12 N8 C4 0.1(5) . . . . ? C61 C12 N8 C4 178.6(5) . . . . ? C11 C12 N8 C18 -179.7(4) . . . . ? C61 C12 N8 C18 -1.2(7) . . . . ? N1 C18 N8 C4 49.2(6) . . . . ? N1 C18 N8 C12 -131.0(4) . . . . ? N4 C2 N3 C7 -2.2(5) . . . . ? Co1 C2 N3 C7 169.6(4) . . . . ? N4 C2 N3 C14 168.0(4) . . . . ? Co1 C2 N3 C14 -20.3(8) . . . . ? C8 C7 N3 C2 1.7(5) . . . . ? C31 C7 N3 C2 -175.8(4) . . . . ? C8 C7 N3 C14 -169.4(4) . . . . ? C31 C7 N3 C14 13.1(7) . . . . ? C13 C14 N3 C2 -3.3(7) . . . . ? C13 C14 N3 C7 166.2(4) . . . . ? N5 C3 N6 C10 -1.2(5) . . . . ? Co1 C3 N6 C10 166.8(3) . . . . ? N5 C3 N6 C16 -173.5(4) . . . . ? Co1 C3 N6 C16 -5.5(6) . . . . ? C9 C10 N6 C3 0.4(5) . . . . ? C49 C10 N6 C3 -176.5(4) . . . . ? C9 C10 N6 C16 172.2(4) . . . . ? C49 C10 N6 C16 -4.7(7) . . . . ? C17 C16 N6 C3 -78.3(5) . . . . ? C17 C16 N6 C10 110.7(5) . . . . ? N6 C3 N5 C9 1.6(5) . . . . ? Co1 C3 N5 C9 -166.7(3) . . . . ? N6 C3 N5 C15 174.2(4) . . . . ? Co1 C3 N5 C15 5.9(6) . . . . ? C10 C9 N5 C3 -1.4(5) . . . . ? C43 C9 N5 C3 -178.9(4) . . . . ? C10 C9 N5 C15 -173.3(4) . . . . ? C43 C9 N5 C15 9.2(7) . . . . ? N4 C15 N5 C3 -51.0(5) . . . . ? N4 C15 N5 C9 120.2(5) . . . . ? N8 C4 N7 C11 0.1(5) . . . . ? Co1 C4 N7 C11 179.3(4) . . . . ? N8 C4 N7 C17 173.0(4) . . . . ? Co1 C4 N7 C17 -7.8(8) . . . . ? C12 C11 N7 C4 -0.1(5) . . . . ? C55 C11 N7 C4 178.5(4) . . . . ? C12 C11 N7 C17 -173.7(4) . . . . ? C55 C11 N7 C17 4.9(7) . . . . ? C16 C17 N7 C4 -10.9(7) . . . . ? C16 C17 N7 C11 161.6(4) . . . . ? N3 C2 N4 C8 2.0(5) . . . . ? Co1 C2 N4 C8 -171.4(3) . . . . ? N3 C2 N4 C15 179.5(4) . . . . ? Co1 C2 N4 C15 6.2(6) . . . . ? C7 C8 N4 C2 -1.0(5) . . . . ? C37 C8 N4 C2 177.2(4) . . . . ? C7 C8 N4 C15 -178.6(4) . . . . ? C37 C8 N4 C15 -0.3(7) . . . . ? N5 C15 N4 C2 44.7(6) . . . . ? N5 C15 N4 C8 -138.0(4) . . . . ? O1 S1 C67 F3 56.3(6) . . . . ? O2 S1 C67 F3 -63.4(6) . . . . ? O3 S1 C67 F3 176.0(5) . . . . ? O1 S1 C67 F1 175.4(5) . . . . ? O2 S1 C67 F1 55.8(5) . . . . ? O3 S1 C67 F1 -64.9(5) . . . . ? O1 S1 C67 F2 -65.8(6) . . . . ? O2 S1 C67 F2 174.5(5) . . . . ? O3 S1 C67 F2 53.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.367 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.145 data_11 _database_code_depnum_ccdc_archive 'CCDC 882743' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H58 Cl2 Cr F6 N10 P' _chemical_formula_weight 1307.13 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.1931(13) _cell_length_b 13.7529(15) _cell_length_c 18.886(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.4710(10) _cell_angle_gamma 90.00 _cell_volume 3166.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8271 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 23 _exptl_crystal_description plate _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1350 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9787 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER APEX II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25634 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 23.31 _reflns_number_total 9105 _reflns_number_gt 6678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 9105 _refine_ls_number_parameters 814 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _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 Cr1 Cr 0.28431(6) 0.35978(7) 0.10959(5) 0.0181(2) Uani 1 1 d . . . Cl2 Cl 0.35819(10) 0.51601(10) 0.09226(7) 0.0239(3) Uani 1 1 d . . . Cl1 Cl 0.20923(10) 0.20540(10) 0.12746(7) 0.0222(3) Uani 1 1 d . . . N8 N 0.3143(3) 0.3608(4) 0.2716(2) 0.0192(10) Uani 1 1 d . . . N6 N 0.0386(3) 0.4551(3) 0.1060(2) 0.0180(11) Uani 1 1 d . . . N3 N 0.4068(3) 0.3652(3) -0.0350(2) 0.0168(10) Uani 1 1 d . . . N4 N 0.2372(3) 0.3276(3) -0.0493(2) 0.0181(11) Uani 1 1 d . . . N2 N 0.5291(3) 0.2703(3) 0.1106(2) 0.0174(11) Uani 1 1 d . . . N1 N 0.4578(3) 0.2739(3) 0.2129(2) 0.0184(10) Uani 1 1 d . . . N5 N 0.0765(3) 0.3712(3) 0.0139(2) 0.0181(10) Uani 1 1 d . . . N7 N 0.2174(3) 0.4838(3) 0.2402(2) 0.0191(11) Uani 1 1 d . . . C3 C 0.1220(4) 0.4039(4) 0.0777(3) 0.0183(12) Uani 1 1 d . . . C1 C 0.4370(4) 0.2980(4) 0.1444(3) 0.0191(13) Uani 1 1 d . . . C4 C 0.2626(4) 0.4021(4) 0.2148(3) 0.0212(13) Uani 1 1 d . . . C2 C 0.3166(4) 0.3402(4) 0.0018(3) 0.0168(13) Uani 1 1 d . . . C8 C 0.0404(4) 0.5091(5) 0.1735(3) 0.0249(14) Uani 1 1 d . . . H8A H 0.0155 0.4650 0.2113 0.030 Uiso 1 1 calc R . . H8B H -0.0131 0.5631 0.1696 0.030 Uiso 1 1 calc R . . C5 C 0.5519(4) 0.2799(4) 0.0353(3) 0.0223(14) Uani 1 1 d . . . H5A H 0.5167 0.2247 0.0099 0.027 Uiso 1 1 calc R . . H5B H 0.6321 0.2735 0.0296 0.027 Uiso 1 1 calc R . . C6 C 0.5146(4) 0.3734(4) -0.0008(3) 0.0204(13) Uani 1 1 d . . . H6A H 0.5131 0.4261 0.0348 0.024 Uiso 1 1 calc R . . H6B H 0.5687 0.3916 -0.0367 0.024 Uiso 1 1 calc R . . C9 C 0.1517(4) 0.5512(4) 0.1964(3) 0.0224(13) Uani 1 1 d . . . H9A H 0.1930 0.5682 0.1537 0.027 Uiso 1 1 calc R . . H9B H 0.1399 0.6119 0.2234 0.027 Uiso 1 1 calc R . . C7 C 0.1274(4) 0.2989(4) -0.0313(3) 0.0177(13) Uani 1 1 d . . . H7A H 0.1302 0.2355 -0.0064 0.021 Uiso 1 1 calc R . . H7B H 0.0823 0.2907 -0.0752 0.021 Uiso 1 1 calc R . . C10 C 0.3730(4) 0.2683(4) 0.2663(3) 0.0197(13) Uani 1 1 d . . . H10A H 0.3204 0.2160 0.2534 0.024 Uiso 1 1 calc R . . H10B H 0.4074 0.2519 0.3128 0.024 Uiso 1 1 calc R . . C12 C 0.6063(4) 0.2278(4) 0.1586(3) 0.0177(13) Uani 1 1 d . . . C11 C 0.5613(4) 0.2318(4) 0.2231(3) 0.0180(13) Uani 1 1 d . . . C18 C 0.3043(4) 0.4183(4) 0.3324(3) 0.0196(13) Uani 1 1 d . . . C17 C 0.2426(4) 0.4953(4) 0.3129(3) 0.0208(13) Uani 1 1 d . . . C15 C -0.0332(4) 0.3997(4) 0.0035(3) 0.0189(13) Uani 1 1 d . . . C13 C 0.3825(4) 0.3703(4) -0.1073(3) 0.0191(12) Uani 1 1 d . . . C14 C 0.2749(4) 0.3475(4) -0.1162(3) 0.0171(12) Uani 1 1 d . . . C16 C -0.0575(4) 0.4525(4) 0.0624(3) 0.0198(13) Uani 1 1 d . . . C43 C -0.1010(4) 0.3685(4) -0.0573(3) 0.0208(13) Uani 1 1 d . . . C19 C 0.6064(4) 0.2008(4) 0.2935(3) 0.0183(13) Uani 1 1 d . . . C42 C 0.1600(4) 0.2556(4) -0.2061(3) 0.0243(14) Uani 1 1 d . . . H42 H 0.1768 0.1969 -0.1816 0.029 Uiso 1 1 calc R . . C25 C 0.7163(4) 0.1925(4) 0.1386(3) 0.0190(13) Uani 1 1 d . . . C37 C 0.2028(4) 0.3433(4) -0.1813(3) 0.0211(14) Uani 1 1 d . . . C31 C 0.4613(4) 0.4035(4) -0.1608(3) 0.0199(13) Uani 1 1 d . . . C26 C 0.8090(4) 0.2276(4) 0.1734(3) 0.0225(14) Uani 1 1 d . . . H26 H 0.8022 0.2725 0.2113 0.027 Uiso 1 1 calc R . . C35 C 0.5420(5) 0.3842(5) -0.2742(3) 0.0373(18) Uani 1 1 d . . . H35 H 0.5484 0.3487 -0.3171 0.045 Uiso 1 1 calc R . . C22 C 0.6926(5) 0.1434(5) 0.4246(3) 0.0316(16) Uani 1 1 d . . . H22 H 0.7203 0.1234 0.4698 0.038 Uiso 1 1 calc R . . C44 C -0.0852(4) 0.4046(5) -0.1245(3) 0.0256(14) Uani 1 1 d . . . H44 H -0.0294 0.4515 -0.1321 0.031 Uiso 1 1 calc R . . C41 C 0.0931(5) 0.2536(5) -0.2664(3) 0.0334(16) Uani 1 1 d . . . H41 H 0.0628 0.1938 -0.2826 0.040 Uiso 1 1 calc R . . C28 C 0.9222(5) 0.1319(4) 0.0980(3) 0.0268(15) Uani 1 1 d . . . H28 H 0.9931 0.1124 0.0839 0.032 Uiso 1 1 calc R . . C27 C 0.9112(4) 0.1978(5) 0.1532(3) 0.0313(16) Uani 1 1 d . . . H27 H 0.9749 0.2224 0.1771 0.038 Uiso 1 1 calc R . . C32 C 0.5272(4) 0.4849(4) -0.1496(3) 0.0233(14) Uani 1 1 d . . . H32 H 0.5225 0.5202 -0.1065 0.028 Uiso 1 1 calc R . . C21 C 0.6650(5) 0.2394(5) 0.4132(3) 0.0350(16) Uani 1 1 d . . . H21 H 0.6753 0.2858 0.4500 0.042 Uiso 1 1 calc R . . C23 C 0.6801(5) 0.0762(5) 0.3708(3) 0.0315(15) Uani 1 1 d . . . H23 H 0.7018 0.0106 0.3783 0.038 Uiso 1 1 calc R . . C40 C 0.0703(5) 0.3382(5) -0.3032(3) 0.0309(16) Uani 1 1 d . . . H40 H 0.0252 0.3361 -0.3450 0.037 Uiso 1 1 calc R . . C48 C -0.1824(4) 0.3004(4) -0.0465(3) 0.0242(14) Uani 1 1 d . . . H48 H -0.1934 0.2757 -0.0002 0.029 Uiso 1 1 calc R . . C33 C 0.5998(4) 0.5152(5) -0.2007(3) 0.0301(15) Uani 1 1 d . . . H33 H 0.6455 0.5701 -0.1920 0.036 Uiso 1 1 calc R . . C20 C 0.6219(5) 0.2684(5) 0.3475(3) 0.0265(14) Uani 1 1 d . . . H20 H 0.6031 0.3346 0.3396 0.032 Uiso 1 1 calc R . . C36 C 0.4692(4) 0.3525(5) -0.2243(3) 0.0303(15) Uani 1 1 d . . . H36 H 0.4251 0.2966 -0.2331 0.036 Uiso 1 1 calc R . . C30 C 0.7265(4) 0.1232(4) 0.0839(3) 0.0240(14) Uani 1 1 d . . . H30 H 0.6629 0.0965 0.0613 0.029 Uiso 1 1 calc R . . C29 C 0.8296(5) 0.0947(4) 0.0635(3) 0.0298(15) Uani 1 1 d . . . H29 H 0.8371 0.0496 0.0258 0.036 Uiso 1 1 calc R . . C39 C 0.1128(5) 0.4260(5) -0.2798(3) 0.0334(16) Uani 1 1 d . . . H39 H 0.0967 0.4842 -0.3051 0.040 Uiso 1 1 calc R . . C45 C -0.1512(4) 0.3723(5) -0.1813(3) 0.0274(14) Uani 1 1 d . . . H45 H -0.1412 0.3978 -0.2274 0.033 Uiso 1 1 calc R . . C24 C 0.6353(4) 0.1050(4) 0.3054(3) 0.0239(14) Uani 1 1 d . . . H24 H 0.6247 0.0584 0.2687 0.029 Uiso 1 1 calc R . . C47 C -0.2482(4) 0.2679(4) -0.1026(3) 0.0271(15) Uani 1 1 d . . . H47 H -0.3045 0.2217 -0.0947 0.033 Uiso 1 1 calc R . . C46 C -0.2316(5) 0.3027(4) -0.1702(3) 0.0287(15) Uani 1 1 d . . . H46 H -0.2751 0.2791 -0.2089 0.034 Uiso 1 1 calc R . . C38 C 0.1800(4) 0.4287(4) -0.2181(3) 0.0243(14) Uani 1 1 d . . . H38 H 0.2096 0.4888 -0.2017 0.029 Uiso 1 1 calc R . . C34 C 0.6054(5) 0.4658(5) -0.2635(3) 0.0367(17) Uani 1 1 d . . . H34 H 0.6527 0.4879 -0.2994 0.044 Uiso 1 1 calc R . . C56 C 0.2673(5) 0.6668(5) 0.3522(3) 0.0305(15) Uani 1 1 d . . . H56 H 0.3321 0.6705 0.3255 0.037 Uiso 1 1 calc R . . C49 C -0.1630(4) 0.4986(4) 0.0784(3) 0.0206(13) Uani 1 1 d . . . C55 C 0.2085(4) 0.5805(4) 0.3535(3) 0.0241(14) Uani 1 1 d . . . C61 C 0.3543(4) 0.3918(5) 0.4024(3) 0.0256(14) Uani 1 1 d . . . C66 C 0.3345(5) 0.3018(5) 0.4327(3) 0.0363(17) Uani 1 1 d . . . H66 H 0.2850 0.2581 0.4095 0.044 Uiso 1 1 calc R . . C60 C 0.1129(5) 0.5766(5) 0.3940(3) 0.0293(15) Uani 1 1 d . . . H60 H 0.0708 0.5186 0.3958 0.035 Uiso 1 1 calc R . . C50 C -0.2164(4) 0.5524(4) 0.0249(3) 0.0237(13) Uani 1 1 d . . . H50 H -0.1832 0.5596 -0.0197 0.028 Uiso 1 1 calc R . . C58 C 0.1394(5) 0.7445(5) 0.4283(3) 0.0305(15) Uani 1 1 d . . . H58 H 0.1156 0.8009 0.4526 0.037 Uiso 1 1 calc R . . C53 C -0.3157(4) 0.5295(5) 0.1541(3) 0.0311(16) Uani 1 1 d . . . H53 H -0.3506 0.5206 0.1981 0.037 Uiso 1 1 calc R . . C57 C 0.2331(5) 0.7470(5) 0.3890(3) 0.0321(16) Uani 1 1 d . . . H57 H 0.2749 0.8052 0.3875 0.039 Uiso 1 1 calc R . . C59 C 0.0807(5) 0.6594(5) 0.4318(3) 0.0328(16) Uani 1 1 d . . . H59 H 0.0175 0.6566 0.4601 0.039 Uiso 1 1 calc R . . C51 C -0.3181(5) 0.5955(4) 0.0365(4) 0.0297(15) Uani 1 1 d . . . H51 H -0.3535 0.6321 -0.0001 0.036 Uiso 1 1 calc R . . C52 C -0.3670(5) 0.5851(4) 0.1012(4) 0.0332(17) Uani 1 1 d . . . H52 H -0.4353 0.6156 0.1096 0.040 Uiso 1 1 calc R . . C65 C 0.3845(7) 0.2746(7) 0.4952(4) 0.058(2) Uani 1 1 d . . . H65 H 0.3716 0.2120 0.5146 0.069 Uiso 1 1 calc R . . C62 C 0.4245(5) 0.4572(5) 0.4365(3) 0.0367(17) Uani 1 1 d . . . H62 H 0.4390 0.5190 0.4164 0.044 Uiso 1 1 calc R . . C64 C 0.4525(7) 0.3378(7) 0.5290(4) 0.065(3) Uani 1 1 d . . . H64 H 0.4866 0.3188 0.5726 0.078 Uiso 1 1 calc R . . C54 C -0.2141(4) 0.4868(4) 0.1434(3) 0.0290(15) Uani 1 1 d . . . H54 H -0.1794 0.4498 0.1801 0.035 Uiso 1 1 calc R . . C63 C 0.4741(6) 0.4290(7) 0.5024(4) 0.062(3) Uani 1 1 d . . . H63 H 0.5214 0.4724 0.5276 0.075 Uiso 1 1 calc R . . P1 P 0.15304(14) 0.04774(14) 0.41714(9) 0.0372(4) Uani 1 1 d . . . F2 F 0.1535(3) 0.1376(3) 0.47127(18) 0.0407(9) Uani 1 1 d . . . F1 F 0.1774(4) 0.1208(3) 0.3540(2) 0.0557(11) Uani 1 1 d . . . F5 F 0.1532(3) -0.0406(3) 0.3625(2) 0.0540(11) Uani 1 1 d . . . F6 F 0.0258(3) 0.0614(4) 0.4035(2) 0.0691(14) Uani 1 1 d . . . F4 F 0.1289(4) -0.0235(3) 0.4814(2) 0.0692(13) Uani 1 1 d . . . F3 F 0.2816(3) 0.0353(3) 0.4311(2) 0.0629(13) Uani 1 1 d . . . N9 N 0.8985(5) 0.3986(5) 0.3045(3) 0.0591(18) Uani 1 1 d . . . N10 N 0.5587(6) 0.6423(5) 0.3201(4) 0.066(2) Uani 1 1 d . . . C69 C 0.9359(6) 0.3496(6) 0.3450(4) 0.0489(19) Uani 1 1 d . . . C70 C 0.9885(12) 0.2922(12) 0.3997(8) 0.186(9) Uani 1 1 d . . . H70A H 1.0680 0.3020 0.3987 0.279 Uiso 1 1 calc R . . H70B H 0.9717 0.2233 0.3917 0.279 Uiso 1 1 calc R . . H70C H 0.9615 0.3121 0.4459 0.279 Uiso 1 1 calc R . . C68 C 0.7341(8) 0.5708(8) 0.3775(5) 0.086(3) Uani 1 1 d . . . H68A H 0.7154 0.5367 0.4211 0.130 Uiso 1 1 calc R . . H68B H 0.7863 0.6231 0.3888 0.130 Uiso 1 1 calc R . . H68C H 0.7673 0.5250 0.3446 0.130 Uiso 1 1 calc R . . C67 C 0.6365(7) 0.6114(6) 0.3454(4) 0.0485(19) 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 Cr1 0.0102(4) 0.0266(5) 0.0174(5) 0.0003(4) -0.0006(3) 0.0007(4) Cl2 0.0154(7) 0.0272(8) 0.0290(8) 0.0000(7) 0.0019(6) -0.0011(6) Cl1 0.0148(7) 0.0278(8) 0.0241(8) 0.0018(6) -0.0005(6) -0.0027(6) N8 0.011(2) 0.031(3) 0.016(2) 0.000(2) 0.0015(18) 0.000(2) N6 0.010(2) 0.024(3) 0.020(3) -0.004(2) -0.002(2) 0.001(2) N3 0.012(2) 0.020(2) 0.019(2) 0.004(2) 0.0013(18) 0.002(2) N4 0.011(2) 0.019(3) 0.024(3) 0.001(2) 0.001(2) -0.0027(19) N2 0.008(2) 0.025(3) 0.019(3) -0.002(2) -0.0001(19) 0.005(2) N1 0.011(2) 0.024(3) 0.020(3) -0.001(2) -0.0008(19) -0.0015(19) N5 0.009(2) 0.023(3) 0.023(3) -0.004(2) 0.0016(18) -0.001(2) N7 0.015(2) 0.024(3) 0.018(3) 0.007(2) -0.001(2) 0.002(2) C3 0.015(3) 0.024(3) 0.016(3) 0.000(3) 0.003(2) -0.002(2) C1 0.012(3) 0.023(3) 0.022(3) -0.004(3) 0.001(2) -0.002(2) C4 0.011(3) 0.022(3) 0.031(4) 0.006(3) -0.001(2) -0.004(2) C2 0.007(3) 0.024(3) 0.020(3) -0.003(3) -0.001(2) 0.003(2) C8 0.015(3) 0.035(4) 0.025(3) -0.006(3) 0.000(2) 0.002(3) C5 0.012(3) 0.035(4) 0.021(3) 0.005(3) 0.002(2) 0.004(2) C6 0.005(2) 0.027(3) 0.029(3) 0.002(3) -0.002(2) 0.002(2) C9 0.017(3) 0.026(3) 0.024(3) 0.000(3) 0.003(2) 0.003(3) C7 0.009(3) 0.021(3) 0.022(3) -0.003(3) 0.000(2) 0.004(2) C10 0.019(3) 0.023(3) 0.017(3) -0.001(3) 0.003(2) 0.002(3) C12 0.014(3) 0.013(3) 0.026(3) 0.004(3) -0.006(2) -0.001(2) C11 0.013(3) 0.021(3) 0.020(3) -0.001(3) -0.002(2) 0.002(2) C18 0.018(3) 0.028(3) 0.013(3) -0.005(3) 0.001(2) -0.007(3) C17 0.019(3) 0.028(4) 0.015(3) -0.005(3) 0.002(2) -0.001(3) C15 0.009(3) 0.024(3) 0.023(3) 0.003(3) -0.004(2) -0.003(2) C13 0.017(3) 0.022(3) 0.018(3) -0.004(3) 0.000(2) 0.004(3) C14 0.011(3) 0.027(3) 0.014(3) -0.001(3) 0.001(2) 0.005(2) C16 0.007(3) 0.028(3) 0.024(3) 0.007(3) -0.001(2) 0.000(2) C43 0.013(3) 0.027(3) 0.023(3) 0.000(3) -0.004(2) 0.004(3) C19 0.014(3) 0.029(4) 0.012(3) 0.003(3) 0.001(2) 0.003(2) C42 0.020(3) 0.025(3) 0.028(4) 0.000(3) -0.001(3) -0.002(3) C25 0.015(3) 0.022(3) 0.021(3) 0.008(3) 0.003(2) 0.001(2) C37 0.010(3) 0.034(4) 0.020(3) -0.003(3) 0.003(2) -0.002(3) C31 0.009(3) 0.027(3) 0.024(3) 0.009(3) -0.001(2) 0.005(3) C26 0.014(3) 0.028(3) 0.025(3) -0.001(3) -0.007(2) -0.002(3) C35 0.029(3) 0.066(5) 0.017(3) -0.003(3) 0.005(3) 0.013(4) C22 0.031(4) 0.045(4) 0.018(3) 0.005(3) -0.006(3) 0.003(3) C44 0.014(3) 0.033(3) 0.030(4) 0.001(3) 0.001(3) -0.004(3) C41 0.026(3) 0.046(4) 0.028(4) -0.006(3) -0.002(3) -0.008(3) C28 0.013(3) 0.030(4) 0.037(4) 0.008(3) 0.003(3) 0.005(3) C27 0.014(3) 0.039(4) 0.041(4) 0.001(3) -0.008(3) -0.001(3) C32 0.019(3) 0.032(4) 0.019(3) 0.005(3) 0.000(3) 0.006(3) C21 0.028(3) 0.054(5) 0.023(4) -0.009(3) -0.005(3) 0.000(3) C23 0.030(4) 0.034(4) 0.030(4) 0.007(3) -0.005(3) -0.002(3) C40 0.024(3) 0.052(5) 0.016(3) 0.007(3) -0.006(3) 0.001(3) C48 0.013(3) 0.028(3) 0.031(4) 0.001(3) 0.001(3) 0.006(3) C33 0.015(3) 0.035(4) 0.040(4) 0.017(3) 0.000(3) 0.002(3) C20 0.026(3) 0.032(4) 0.022(3) 0.002(3) -0.007(3) 0.004(3) C36 0.018(3) 0.049(4) 0.024(3) -0.010(3) 0.000(3) -0.002(3) C30 0.019(3) 0.029(4) 0.024(3) 0.004(3) 0.000(3) 0.004(3) C29 0.029(4) 0.028(4) 0.033(4) -0.001(3) 0.009(3) 0.006(3) C39 0.026(3) 0.050(5) 0.024(4) 0.006(3) -0.002(3) 0.005(3) C45 0.026(3) 0.037(4) 0.020(3) 0.007(3) -0.005(3) 0.008(3) C24 0.016(3) 0.029(4) 0.026(3) -0.001(3) -0.002(3) -0.004(3) C47 0.013(3) 0.028(4) 0.040(4) -0.006(3) 0.001(3) 0.004(3) C46 0.021(3) 0.035(4) 0.030(4) -0.013(3) -0.004(3) 0.004(3) C38 0.019(3) 0.025(4) 0.028(4) 0.002(3) 0.002(3) 0.000(3) C34 0.017(3) 0.064(5) 0.030(4) 0.021(4) 0.009(3) 0.005(3) C56 0.021(3) 0.038(4) 0.034(4) 0.001(3) 0.009(3) 0.001(3) C49 0.015(3) 0.019(3) 0.028(4) 0.001(3) 0.000(3) 0.004(2) C55 0.015(3) 0.037(4) 0.020(3) 0.001(3) -0.004(3) -0.003(3) C61 0.021(3) 0.038(4) 0.017(3) 0.000(3) 0.002(3) 0.008(3) C66 0.040(4) 0.055(5) 0.014(3) 0.001(3) 0.004(3) 0.003(3) C60 0.025(3) 0.034(4) 0.029(4) -0.002(3) 0.001(3) 0.003(3) C50 0.015(3) 0.020(3) 0.036(4) -0.003(3) -0.001(3) -0.002(2) C58 0.030(4) 0.036(4) 0.025(4) -0.006(3) -0.003(3) 0.007(3) C53 0.015(3) 0.044(4) 0.035(4) -0.010(3) 0.005(3) -0.008(3) C57 0.025(3) 0.033(4) 0.038(4) -0.004(3) 0.001(3) 0.003(3) C59 0.021(3) 0.043(4) 0.035(4) -0.007(3) 0.003(3) 0.006(3) C51 0.021(3) 0.026(4) 0.042(4) -0.001(3) -0.006(3) 0.002(3) C52 0.012(3) 0.027(4) 0.061(5) -0.010(3) 0.002(3) -0.004(3) C65 0.067(5) 0.081(6) 0.025(4) 0.007(4) -0.006(4) 0.014(5) C62 0.029(4) 0.051(5) 0.030(4) -0.009(3) -0.005(3) 0.009(3) C64 0.073(6) 0.085(7) 0.036(5) 0.019(5) -0.014(4) 0.029(5) C54 0.018(3) 0.035(4) 0.034(4) -0.007(3) -0.001(3) 0.001(3) C63 0.050(5) 0.090(7) 0.046(5) -0.035(5) -0.019(4) 0.007(5) P1 0.0344(10) 0.0394(11) 0.0379(11) -0.0088(9) 0.0032(8) 0.0022(8) F2 0.041(2) 0.043(2) 0.038(2) -0.0106(19) 0.0013(18) -0.0006(18) F1 0.080(3) 0.053(3) 0.034(2) 0.001(2) 0.005(2) -0.002(2) F5 0.065(3) 0.047(3) 0.050(3) -0.021(2) 0.013(2) -0.003(2) F6 0.031(2) 0.097(3) 0.079(3) -0.042(3) -0.003(2) -0.002(2) F4 0.119(4) 0.047(3) 0.042(3) -0.004(2) 0.023(3) -0.021(3) F3 0.036(2) 0.084(3) 0.068(3) -0.019(3) -0.004(2) 0.020(2) N9 0.067(4) 0.069(5) 0.041(4) 0.009(4) -0.005(3) -0.021(4) N10 0.067(5) 0.074(5) 0.059(5) 0.014(4) 0.008(4) 0.012(4) C69 0.051(4) 0.056(5) 0.041(5) 0.007(4) 0.013(4) 0.000(4) C70 0.163(13) 0.210(16) 0.189(14) 0.160(13) 0.092(11) 0.126(12) C68 0.086(7) 0.117(9) 0.056(6) -0.006(6) -0.013(5) 0.036(6) C67 0.058(5) 0.047(5) 0.041(5) -0.007(4) 0.001(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C4 2.094(6) . ? Cr1 C2 2.101(5) . ? Cr1 C1 2.135(5) . ? Cr1 C3 2.142(5) . ? Cr1 Cl1 2.3400(16) . ? Cr1 Cl2 2.3558(16) . ? N8 C4 1.356(7) . ? N8 C18 1.401(7) . ? N8 C10 1.464(7) . ? N6 C3 1.357(7) . ? N6 C16 1.414(6) . ? N6 C8 1.476(7) . ? N3 C2 1.359(6) . ? N3 C13 1.392(6) . ? N3 C6 1.455(6) . ? N4 C2 1.360(7) . ? N4 C14 1.383(7) . ? N4 C7 1.444(6) . ? N2 C1 1.361(7) . ? N2 C12 1.415(7) . ? N2 C5 1.463(7) . ? N1 C1 1.353(7) . ? N1 C11 1.397(7) . ? N1 C10 1.464(7) . ? N5 C3 1.388(7) . ? N5 C15 1.403(6) . ? N5 C7 1.460(7) . ? N7 C4 1.345(7) . ? N7 C17 1.409(7) . ? N7 C9 1.467(7) . ? C8 C9 1.527(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C5 C6 1.520(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 C11 1.350(8) . ? C12 C25 1.484(7) . ? C11 C19 1.488(7) . ? C18 C17 1.344(8) . ? C18 C61 1.487(8) . ? C17 C55 1.467(8) . ? C15 C16 1.367(8) . ? C15 C43 1.462(7) . ? C13 C14 1.355(7) . ? C13 C31 1.484(7) . ? C14 C37 1.494(7) . ? C16 C49 1.472(7) . ? C43 C44 1.381(8) . ? C43 C48 1.383(8) . ? C19 C24 1.381(8) . ? C19 C20 1.390(8) . ? C42 C41 1.385(8) . ? C42 C37 1.391(8) . ? C42 H42 0.9500 . ? C25 C26 1.380(7) . ? C25 C30 1.413(8) . ? C37 C38 1.390(8) . ? C31 C32 1.391(8) . ? C31 C36 1.395(8) . ? C26 C27 1.376(8) . ? C26 H26 0.9500 . ? C35 C34 1.375(10) . ? C35 C36 1.383(8) . ? C35 H35 0.9500 . ? C22 C23 1.378(9) . ? C22 C21 1.379(9) . ? C22 H22 0.9500 . ? C44 C45 1.398(8) . ? C44 H44 0.9500 . ? C41 C40 1.380(9) . ? C41 H41 0.9500 . ? C28 C29 1.386(8) . ? C28 C27 1.390(8) . ? C28 H28 0.9500 . ? C27 H27 0.9500 . ? C32 C33 1.390(8) . ? C32 H32 0.9500 . ? C21 C20 1.392(8) . ? C21 H21 0.9500 . ? C23 C24 1.395(8) . ? C23 H23 0.9500 . ? C40 C39 1.383(9) . ? C40 H40 0.9500 . ? C48 C47 1.387(8) . ? C48 H48 0.9500 . ? C33 C34 1.371(9) . ? C33 H33 0.9500 . ? C20 H20 0.9500 . ? C36 H36 0.9500 . ? C30 C29 1.381(8) . ? C30 H30 0.9500 . ? C29 H29 0.9500 . ? C39 C38 1.406(8) . ? C39 H39 0.9500 . ? C45 C46 1.389(8) . ? C45 H45 0.9500 . ? C24 H24 0.9500 . ? C47 C46 1.382(9) . ? C47 H47 0.9500 . ? C46 H46 0.9500 . ? C38 H38 0.9500 . ? C34 H34 0.9500 . ? C56 C57 1.374(9) . ? C56 C55 1.387(8) . ? C56 H56 0.9500 . ? C49 C50 1.398(8) . ? C49 C54 1.401(8) . ? C55 C60 1.411(8) . ? C61 C62 1.388(9) . ? C61 C66 1.388(9) . ? C66 C65 1.367(9) . ? C66 H66 0.9500 . ? C60 C59 1.405(8) . ? C60 H60 0.9500 . ? C50 C51 1.397(8) . ? C50 H50 0.9500 . ? C58 C59 1.373(9) . ? C58 C57 1.379(8) . ? C58 H58 0.9500 . ? C53 C54 1.390(8) . ? C53 C52 1.394(9) . ? C53 H53 0.9500 . ? C57 H57 0.9500 . ? C59 H59 0.9500 . ? C51 C52 1.381(9) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C65 C64 1.351(12) . ? C65 H65 0.9500 . ? C62 C63 1.423(10) . ? C62 H62 0.9500 . ? C64 C63 1.379(12) . ? C64 H64 0.9500 . ? C54 H54 0.9500 . ? C63 H63 0.9500 . ? P1 F6 1.578(4) . ? P1 F3 1.592(4) . ? P1 F1 1.593(4) . ? P1 F4 1.593(5) . ? P1 F5 1.594(4) . ? P1 F2 1.604(4) . ? N9 C69 1.109(9) . ? N10 C67 1.134(9) . ? C69 C70 1.437(13) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C68 C67 1.435(12) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 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 C4 Cr1 C2 170.6(2) . . ? C4 Cr1 C1 87.1(2) . . ? C2 Cr1 C1 93.7(2) . . ? C4 Cr1 C3 92.8(2) . . ? C2 Cr1 C3 87.64(19) . . ? C1 Cr1 C3 172.6(2) . . ? C4 Cr1 Cl1 93.22(16) . . ? C2 Cr1 Cl1 96.14(15) . . ? C1 Cr1 Cl1 86.33(15) . . ? C3 Cr1 Cl1 86.31(15) . . ? C4 Cr1 Cl2 86.34(16) . . ? C2 Cr1 Cl2 84.30(15) . . ? C1 Cr1 Cl2 94.13(15) . . ? C3 Cr1 Cl2 93.22(15) . . ? Cl1 Cr1 Cl2 179.34(6) . . ? C4 N8 C18 111.3(5) . . ? C4 N8 C10 121.9(5) . . ? C18 N8 C10 126.9(4) . . ? C3 N6 C16 112.1(4) . . ? C3 N6 C8 127.3(4) . . ? C16 N6 C8 120.7(4) . . ? C2 N3 C13 111.1(4) . . ? C2 N3 C6 121.8(4) . . ? C13 N3 C6 126.8(4) . . ? C2 N4 C14 112.0(4) . . ? C2 N4 C7 121.0(5) . . ? C14 N4 C7 126.9(4) . . ? C1 N2 C12 111.0(5) . . ? C1 N2 C5 127.6(4) . . ? C12 N2 C5 121.3(4) . . ? C1 N1 C11 112.3(4) . . ? C1 N1 C10 123.6(4) . . ? C11 N1 C10 122.3(4) . . ? C3 N5 C15 112.9(4) . . ? C3 N5 C7 124.2(4) . . ? C15 N5 C7 121.8(4) . . ? C4 N7 C17 111.1(4) . . ? C4 N7 C9 123.4(5) . . ? C17 N7 C9 125.5(5) . . ? N6 C3 N5 102.9(4) . . ? N6 C3 Cr1 137.1(4) . . ? N5 C3 Cr1 119.9(4) . . ? N1 C1 N2 104.1(4) . . ? N1 C1 Cr1 122.2(4) . . ? N2 C1 Cr1 133.7(4) . . ? N7 C4 N8 104.7(5) . . ? N7 C4 Cr1 129.3(4) . . ? N8 C4 Cr1 124.6(4) . . ? N3 C2 N4 103.9(4) . . ? N3 C2 Cr1 129.6(4) . . ? N4 C2 Cr1 123.7(3) . . ? N6 C8 C9 115.4(4) . . ? N6 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? N6 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? N2 C5 C6 116.8(5) . . ? N2 C5 H5A 108.1 . . ? C6 C5 H5A 108.1 . . ? N2 C5 H5B 108.1 . . ? C6 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? N3 C6 C5 113.0(5) . . ? N3 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N7 C9 C8 112.8(5) . . ? N7 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? N7 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N4 C7 N5 111.2(4) . . ? N4 C7 H7A 109.4 . . ? N5 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? N5 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N8 C10 N1 110.9(4) . . ? N8 C10 H10A 109.5 . . ? N1 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C11 C12 N2 106.3(4) . . ? C11 C12 C25 129.3(5) . . ? N2 C12 C25 124.3(5) . . ? C12 C11 N1 106.3(4) . . ? C12 C11 C19 130.1(5) . . ? N1 C11 C19 123.6(5) . . ? C17 C18 N8 106.3(5) . . ? C17 C18 C61 130.5(5) . . ? N8 C18 C61 123.2(5) . . ? C18 C17 N7 106.5(5) . . ? C18 C17 C55 130.6(5) . . ? N7 C17 C55 122.8(5) . . ? C16 C15 N5 105.1(4) . . ? C16 C15 C43 131.7(5) . . ? N5 C15 C43 123.1(5) . . ? C14 C13 N3 106.9(4) . . ? C14 C13 C31 129.0(5) . . ? N3 C13 C31 123.9(4) . . ? C13 C14 N4 106.0(4) . . ? C13 C14 C37 131.2(5) . . ? N4 C14 C37 122.8(4) . . ? C15 C16 N6 107.0(4) . . ? C15 C16 C49 127.1(5) . . ? N6 C16 C49 125.8(5) . . ? C44 C43 C48 119.8(5) . . ? C44 C43 C15 121.7(5) . . ? C48 C43 C15 118.5(5) . . ? C24 C19 C20 119.3(5) . . ? C24 C19 C11 120.4(5) . . ? C20 C19 C11 120.3(5) . . ? C41 C42 C37 120.1(6) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C26 C25 C30 119.9(5) . . ? C26 C25 C12 119.9(5) . . ? C30 C25 C12 120.2(5) . . ? C38 C37 C42 119.8(5) . . ? C38 C37 C14 119.1(5) . . ? C42 C37 C14 121.2(5) . . ? C32 C31 C36 118.9(5) . . ? C32 C31 C13 121.7(5) . . ? C36 C31 C13 119.4(5) . . ? C27 C26 C25 120.0(6) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C34 C35 C36 121.7(6) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C23 C22 C21 120.3(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C40 C41 C42 120.3(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C29 C28 C27 120.0(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C26 C27 C28 120.5(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C33 C32 C31 120.8(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C22 C21 C20 119.9(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C23 C24 119.7(6) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C41 C40 C39 120.4(5) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C43 C48 C47 120.6(6) . . ? C43 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C34 C33 C32 120.0(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C19 C20 C21 120.2(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C35 C36 C31 119.2(6) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C29 C30 C25 119.6(5) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C30 C29 C28 120.0(6) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C40 C39 C38 119.6(6) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C46 C45 C44 119.9(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C19 C24 C23 120.5(6) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C46 C47 C48 119.9(6) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C46 C45 119.9(5) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C37 C38 C39 119.8(6) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C33 C34 C35 119.4(6) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C57 C56 C55 121.0(6) . . ? C57 C56 H56 119.5 . . ? C55 C56 H56 119.5 . . ? C50 C49 C54 119.0(5) . . ? C50 C49 C16 118.3(5) . . ? C54 C49 C16 122.7(5) . . ? C56 C55 C60 118.4(6) . . ? C56 C55 C17 121.4(5) . . ? C60 C55 C17 120.2(5) . . ? C62 C61 C66 119.9(6) . . ? C62 C61 C18 119.2(6) . . ? C66 C61 C18 120.9(6) . . ? C65 C66 C61 121.4(7) . . ? C65 C66 H66 119.3 . . ? C61 C66 H66 119.3 . . ? C59 C60 C55 119.3(6) . . ? C59 C60 H60 120.3 . . ? C55 C60 H60 120.3 . . ? C51 C50 C49 120.7(6) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C59 C58 C57 119.2(6) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C54 C53 C52 120.8(6) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C56 C57 C58 121.2(6) . . ? C56 C57 H57 119.4 . . ? C58 C57 H57 119.4 . . ? C58 C59 C60 120.9(6) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C52 C51 C50 119.9(6) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 119.7(6) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C64 C65 C66 119.2(8) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C61 C62 C63 118.2(7) . . ? C61 C62 H62 120.9 . . ? C63 C62 H62 120.9 . . ? C65 C64 C63 122.3(7) . . ? C65 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? C53 C54 C49 119.8(6) . . ? C53 C54 H54 120.1 . . ? C49 C54 H54 120.1 . . ? C64 C63 C62 119.1(7) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? F6 P1 F3 179.3(3) . . ? F6 P1 F1 90.2(3) . . ? F3 P1 F1 89.5(3) . . ? F6 P1 F4 89.9(3) . . ? F3 P1 F4 90.5(3) . . ? F1 P1 F4 178.8(2) . . ? F6 P1 F5 90.1(2) . . ? F3 P1 F5 90.5(2) . . ? F1 P1 F5 89.6(2) . . ? F4 P1 F5 91.6(2) . . ? F6 P1 F2 90.0(2) . . ? F3 P1 F2 89.4(2) . . ? F1 P1 F2 89.6(2) . . ? F4 P1 F2 89.2(2) . . ? F5 P1 F2 179.2(2) . . ? N9 C69 C70 175.8(11) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N10 C67 C68 179.1(10) . . ? 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 C16 N6 C3 N5 1.7(6) . . . . ? C8 N6 C3 N5 -178.4(5) . . . . ? C16 N6 C3 Cr1 -173.4(4) . . . . ? C8 N6 C3 Cr1 6.5(9) . . . . ? C15 N5 C3 N6 -1.2(6) . . . . ? C7 N5 C3 N6 -169.3(5) . . . . ? C15 N5 C3 Cr1 174.9(4) . . . . ? C7 N5 C3 Cr1 6.8(7) . . . . ? C4 Cr1 C3 N6 10.7(6) . . . . ? C2 Cr1 C3 N6 -159.9(6) . . . . ? C1 Cr1 C3 N6 99.8(17) . . . . ? Cl1 Cr1 C3 N6 103.7(6) . . . . ? Cl2 Cr1 C3 N6 -75.8(6) . . . . ? C4 Cr1 C3 N5 -163.8(4) . . . . ? C2 Cr1 C3 N5 25.6(4) . . . . ? C1 Cr1 C3 N5 -74.7(18) . . . . ? Cl1 Cr1 C3 N5 -70.7(4) . . . . ? Cl2 Cr1 C3 N5 109.8(4) . . . . ? C11 N1 C1 N2 0.2(6) . . . . ? C10 N1 C1 N2 -164.6(5) . . . . ? C11 N1 C1 Cr1 178.0(4) . . . . ? C10 N1 C1 Cr1 13.2(7) . . . . ? C12 N2 C1 N1 0.8(6) . . . . ? C5 N2 C1 N1 -179.5(5) . . . . ? C12 N2 C1 Cr1 -176.7(4) . . . . ? C5 N2 C1 Cr1 3.0(8) . . . . ? C4 Cr1 C1 N1 21.5(4) . . . . ? C2 Cr1 C1 N1 -167.9(4) . . . . ? C3 Cr1 C1 N1 -68.0(18) . . . . ? Cl1 Cr1 C1 N1 -72.0(4) . . . . ? Cl2 Cr1 C1 N1 107.6(4) . . . . ? C4 Cr1 C1 N2 -161.5(5) . . . . ? C2 Cr1 C1 N2 9.2(5) . . . . ? C3 Cr1 C1 N2 109.1(17) . . . . ? Cl1 Cr1 C1 N2 105.1(5) . . . . ? Cl2 Cr1 C1 N2 -75.4(5) . . . . ? C17 N7 C4 N8 1.3(6) . . . . ? C9 N7 C4 N8 -179.2(4) . . . . ? C17 N7 C4 Cr1 -165.5(4) . . . . ? C9 N7 C4 Cr1 14.0(7) . . . . ? C18 N8 C4 N7 -1.9(6) . . . . ? C10 N8 C4 N7 179.0(4) . . . . ? C18 N8 C4 Cr1 165.8(3) . . . . ? C10 N8 C4 Cr1 -13.4(7) . . . . ? C2 Cr1 C4 N7 48.4(15) . . . . ? C1 Cr1 C4 N7 143.0(5) . . . . ? C3 Cr1 C4 N7 -44.4(5) . . . . ? Cl1 Cr1 C4 N7 -130.9(4) . . . . ? Cl2 Cr1 C4 N7 48.7(4) . . . . ? C2 Cr1 C4 N8 -116.1(12) . . . . ? C1 Cr1 C4 N8 -21.4(4) . . . . ? C3 Cr1 C4 N8 151.2(4) . . . . ? Cl1 Cr1 C4 N8 64.7(4) . . . . ? Cl2 Cr1 C4 N8 -115.8(4) . . . . ? C13 N3 C2 N4 1.5(6) . . . . ? C6 N3 C2 N4 -172.1(5) . . . . ? C13 N3 C2 Cr1 -159.7(4) . . . . ? C6 N3 C2 Cr1 26.7(7) . . . . ? C14 N4 C2 N3 -2.1(6) . . . . ? C7 N4 C2 N3 179.2(4) . . . . ? C14 N4 C2 Cr1 160.5(4) . . . . ? C7 N4 C2 Cr1 -18.2(7) . . . . ? C4 Cr1 C2 N3 43.9(15) . . . . ? C1 Cr1 C2 N3 -50.2(5) . . . . ? C3 Cr1 C2 N3 137.1(5) . . . . ? Cl1 Cr1 C2 N3 -136.9(5) . . . . ? Cl2 Cr1 C2 N3 43.6(5) . . . . ? C4 Cr1 C2 N4 -114.0(12) . . . . ? C1 Cr1 C2 N4 151.9(4) . . . . ? C3 Cr1 C2 N4 -20.8(4) . . . . ? Cl1 Cr1 C2 N4 65.2(4) . . . . ? Cl2 Cr1 C2 N4 -114.3(4) . . . . ? C3 N6 C8 C9 30.3(8) . . . . ? C16 N6 C8 C9 -149.8(5) . . . . ? C1 N2 C5 C6 39.8(7) . . . . ? C12 N2 C5 C6 -140.5(5) . . . . ? C2 N3 C6 C5 58.2(7) . . . . ? C13 N3 C6 C5 -114.3(6) . . . . ? N2 C5 C6 N3 -94.0(6) . . . . ? C4 N7 C9 C8 70.1(6) . . . . ? C17 N7 C9 C8 -110.5(6) . . . . ? N6 C8 C9 N7 -90.0(6) . . . . ? C2 N4 C7 N5 61.5(6) . . . . ? C14 N4 C7 N5 -117.0(5) . . . . ? C3 N5 C7 N4 -55.2(7) . . . . ? C15 N5 C7 N4 137.7(5) . . . . ? C4 N8 C10 N1 56.9(6) . . . . ? C18 N8 C10 N1 -122.1(5) . . . . ? C1 N1 C10 N8 -57.0(6) . . . . ? C11 N1 C10 N8 139.7(5) . . . . ? C1 N2 C12 C11 -1.4(6) . . . . ? C5 N2 C12 C11 178.9(5) . . . . ? C1 N2 C12 C25 -178.3(5) . . . . ? C5 N2 C12 C25 2.0(8) . . . . ? N2 C12 C11 N1 1.4(6) . . . . ? C25 C12 C11 N1 178.0(5) . . . . ? N2 C12 C11 C19 -177.9(5) . . . . ? C25 C12 C11 C19 -1.2(10) . . . . ? C1 N1 C11 C12 -1.0(6) . . . . ? C10 N1 C11 C12 164.0(5) . . . . ? C1 N1 C11 C19 178.3(5) . . . . ? C10 N1 C11 C19 -16.7(8) . . . . ? C4 N8 C18 C17 1.7(6) . . . . ? C10 N8 C18 C17 -179.2(5) . . . . ? C4 N8 C18 C61 -179.0(5) . . . . ? C10 N8 C18 C61 0.1(8) . . . . ? N8 C18 C17 N7 -0.8(6) . . . . ? C61 C18 C17 N7 180.0(5) . . . . ? N8 C18 C17 C55 -177.7(5) . . . . ? C61 C18 C17 C55 3.1(10) . . . . ? C4 N7 C17 C18 -0.3(6) . . . . ? C9 N7 C17 C18 -179.8(5) . . . . ? C4 N7 C17 C55 176.9(5) . . . . ? C9 N7 C17 C55 -2.6(8) . . . . ? C3 N5 C15 C16 0.3(6) . . . . ? C7 N5 C15 C16 168.7(5) . . . . ? C3 N5 C15 C43 -175.6(5) . . . . ? C7 N5 C15 C43 -7.2(8) . . . . ? C2 N3 C13 C14 -0.3(6) . . . . ? C6 N3 C13 C14 172.8(5) . . . . ? C2 N3 C13 C31 174.9(5) . . . . ? C6 N3 C13 C31 -11.9(9) . . . . ? N3 C13 C14 N4 -0.9(6) . . . . ? C31 C13 C14 N4 -175.8(5) . . . . ? N3 C13 C14 C37 178.3(6) . . . . ? C31 C13 C14 C37 3.4(10) . . . . ? C2 N4 C14 C13 1.9(6) . . . . ? C7 N4 C14 C13 -179.4(5) . . . . ? C2 N4 C14 C37 -177.4(5) . . . . ? C7 N4 C14 C37 1.3(8) . . . . ? N5 C15 C16 N6 0.7(6) . . . . ? C43 C15 C16 N6 176.1(6) . . . . ? N5 C15 C16 C49 -179.5(5) . . . . ? C43 C15 C16 C49 -4.0(10) . . . . ? C3 N6 C16 C15 -1.6(6) . . . . ? C8 N6 C16 C15 178.5(5) . . . . ? C3 N6 C16 C49 178.6(5) . . . . ? C8 N6 C16 C49 -1.3(8) . . . . ? C16 C15 C43 C44 112.7(7) . . . . ? N5 C15 C43 C44 -72.6(8) . . . . ? C16 C15 C43 C48 -67.7(8) . . . . ? N5 C15 C43 C48 107.0(6) . . . . ? C12 C11 C19 C24 -60.3(8) . . . . ? N1 C11 C19 C24 120.5(6) . . . . ? C12 C11 C19 C20 118.4(7) . . . . ? N1 C11 C19 C20 -60.8(7) . . . . ? C11 C12 C25 C26 -52.0(8) . . . . ? N2 C12 C25 C26 124.1(6) . . . . ? C11 C12 C25 C30 128.3(6) . . . . ? N2 C12 C25 C30 -55.6(7) . . . . ? C41 C42 C37 C38 -1.4(8) . . . . ? C41 C42 C37 C14 179.8(5) . . . . ? C13 C14 C37 C38 -65.5(8) . . . . ? N4 C14 C37 C38 113.6(6) . . . . ? C13 C14 C37 C42 113.3(7) . . . . ? N4 C14 C37 C42 -67.5(7) . . . . ? C14 C13 C31 C32 130.3(6) . . . . ? N3 C13 C31 C32 -43.8(8) . . . . ? C14 C13 C31 C36 -49.1(9) . . . . ? N3 C13 C31 C36 136.7(6) . . . . ? C30 C25 C26 C27 2.2(8) . . . . ? C12 C25 C26 C27 -177.5(5) . . . . ? C48 C43 C44 C45 -0.1(8) . . . . ? C15 C43 C44 C45 179.5(5) . . . . ? C37 C42 C41 C40 1.4(9) . . . . ? C25 C26 C27 C28 -0.3(9) . . . . ? C29 C28 C27 C26 -0.9(9) . . . . ? C36 C31 C32 C33 0.0(8) . . . . ? C13 C31 C32 C33 -179.4(5) . . . . ? C23 C22 C21 C20 1.5(9) . . . . ? C21 C22 C23 C24 -2.4(9) . . . . ? C42 C41 C40 C39 -0.9(9) . . . . ? C44 C43 C48 C47 0.2(8) . . . . ? C15 C43 C48 C47 -179.4(5) . . . . ? C31 C32 C33 C34 1.4(8) . . . . ? C24 C19 C20 C21 -0.8(8) . . . . ? C11 C19 C20 C21 -179.5(5) . . . . ? C22 C21 C20 C19 0.2(9) . . . . ? C34 C35 C36 C31 -1.2(9) . . . . ? C32 C31 C36 C35 -0.1(8) . . . . ? C13 C31 C36 C35 179.4(5) . . . . ? C26 C25 C30 C29 -2.9(8) . . . . ? C12 C25 C30 C29 176.7(5) . . . . ? C25 C30 C29 C28 1.8(9) . . . . ? C27 C28 C29 C30 0.1(9) . . . . ? C41 C40 C39 C38 0.3(9) . . . . ? C43 C44 C45 C46 -1.0(9) . . . . ? C20 C19 C24 C23 -0.2(8) . . . . ? C11 C19 C24 C23 178.5(5) . . . . ? C22 C23 C24 C19 1.8(9) . . . . ? C43 C48 C47 C46 0.8(8) . . . . ? C48 C47 C46 C45 -1.8(8) . . . . ? C44 C45 C46 C47 1.9(8) . . . . ? C42 C37 C38 C39 0.7(8) . . . . ? C14 C37 C38 C39 179.6(5) . . . . ? C40 C39 C38 C37 -0.2(9) . . . . ? C32 C33 C34 C35 -2.6(9) . . . . ? C36 C35 C34 C33 2.6(9) . . . . ? C15 C16 C49 C50 -46.2(8) . . . . ? N6 C16 C49 C50 133.6(6) . . . . ? C15 C16 C49 C54 130.6(6) . . . . ? N6 C16 C49 C54 -49.6(8) . . . . ? C57 C56 C55 C60 -0.4(9) . . . . ? C57 C56 C55 C17 178.4(6) . . . . ? C18 C17 C55 C56 94.8(8) . . . . ? N7 C17 C55 C56 -81.7(7) . . . . ? C18 C17 C55 C60 -86.4(8) . . . . ? N7 C17 C55 C60 97.1(7) . . . . ? C17 C18 C61 C62 -56.5(8) . . . . ? N8 C18 C61 C62 124.4(6) . . . . ? C17 C18 C61 C66 125.6(7) . . . . ? N8 C18 C61 C66 -53.5(7) . . . . ? C62 C61 C66 C65 -1.4(10) . . . . ? C18 C61 C66 C65 176.5(6) . . . . ? C56 C55 C60 C59 -0.3(8) . . . . ? C17 C55 C60 C59 -179.1(5) . . . . ? C54 C49 C50 C51 1.3(8) . . . . ? C16 C49 C50 C51 178.3(5) . . . . ? C55 C56 C57 C58 -0.2(9) . . . . ? C59 C58 C57 C56 1.6(9) . . . . ? C57 C58 C59 C60 -2.3(9) . . . . ? C55 C60 C59 C58 1.7(9) . . . . ? C49 C50 C51 C52 -0.2(9) . . . . ? C50 C51 C52 C53 -1.5(9) . . . . ? C54 C53 C52 C51 2.0(9) . . . . ? C61 C66 C65 C64 1.7(11) . . . . ? C66 C61 C62 C63 -0.1(9) . . . . ? C18 C61 C62 C63 -178.0(6) . . . . ? C66 C65 C64 C63 -0.5(13) . . . . ? C52 C53 C54 C49 -0.8(9) . . . . ? C50 C49 C54 C53 -0.8(8) . . . . ? C16 C49 C54 C53 -177.6(5) . . . . ? C65 C64 C63 C62 -1.0(13) . . . . ? C61 C62 C63 C64 1.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.431 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.129 data_13 _database_code_depnum_ccdc_archive 'CCDC 882744' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H54 Ag3 Cl4 F3 N8 O3 S' _chemical_formula_weight 1585.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' 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 33.096(2) _cell_length_b 16.4589(12) _cell_length_c 26.678(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.0400(10) _cell_angle_gamma 90.00 _cell_volume 12580(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7401 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 22.56 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6352 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9428 _exptl_absorpt_correction_T_max 0.9651 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 66367 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.42 _reflns_number_total 12877 _reflns_number_gt 9094 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1002P] 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 12877 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Ag1 Ag 0.099725(13) 0.16093(2) 0.188308(16) 0.02127(11) Uani 1 1 d . . . Ag2 Ag 0.008094(13) 0.20020(2) 0.079573(17) 0.02447(11) Uani 1 1 d . . . Ag3 Ag 0.010035(13) 0.12317(2) 0.196595(17) 0.02537(12) Uani 1 1 d . . . Cl2 Cl -0.03966(4) 0.03077(8) 0.12393(6) 0.0293(3) Uani 1 1 d . . . Cl1 Cl -0.04531(4) 0.27154(8) 0.09664(6) 0.0304(3) Uani 1 1 d . . . S5 S 0.22831(5) 0.15153(9) 0.25927(6) 0.0334(3) Uani 1 1 d . . . C1 C 0.09487(16) 0.0343(3) 0.1912(2) 0.0203(10) Uani 1 1 d . . . C2 C 0.05848(18) 0.1415(3) 0.0671(2) 0.0233(11) Uani 1 1 d . . . C3 C 0.09608(17) 0.2878(3) 0.1812(2) 0.0220(11) Uani 1 1 d . . . C4 C 0.06521(17) 0.1829(3) 0.2671(2) 0.0220(11) Uani 1 1 d . . . N8 N 0.10195(14) 0.1460(2) 0.31277(17) 0.0213(9) Uani 1 1 d . . . N1 N 0.11023(13) -0.0107(2) 0.23929(17) 0.0204(9) Uani 1 1 d . . . N4 N 0.09247(14) 0.1745(2) 0.05934(17) 0.0195(9) Uani 1 1 d . . . N6 N 0.07294(14) 0.3420(2) 0.19580(17) 0.0200(9) Uani 1 1 d . . . N5 N 0.10860(14) 0.3313(2) 0.14827(17) 0.0204(9) Uani 1 1 d . . . N2 N 0.07055(14) -0.0189(2) 0.14768(17) 0.0196(8) Uani 1 1 d . . . N7 N 0.07724(13) 0.2626(2) 0.27350(16) 0.0188(8) Uani 1 1 d . . . N3 N 0.06738(14) 0.0602(2) 0.07025(17) 0.0205(9) Uani 1 1 d . . . C12 C 0.13701(17) 0.2013(3) 0.3475(2) 0.0206(10) Uani 1 1 d . . . C8 C 0.12138(17) 0.1147(3) 0.0568(2) 0.0206(10) Uani 1 1 d . . . C9 C 0.09289(16) 0.4116(3) 0.1416(2) 0.0187(10) Uani 1 1 d . . . C10 C 0.07043(16) 0.4180(3) 0.1717(2) 0.0188(10) Uani 1 1 d . . . C11 C 0.12140(17) 0.2751(3) 0.3221(2) 0.0206(10) Uani 1 1 d . . . C7 C 0.10652(17) 0.0435(3) 0.0652(2) 0.0198(10) Uani 1 1 d . . . C6 C 0.07066(17) -0.0968(3) 0.1692(2) 0.0206(10) Uani 1 1 d . . . C5 C 0.09542(18) -0.0908(3) 0.2270(2) 0.0235(11) Uani 1 1 d . . . C13 C 0.04331(18) 0.0016(3) 0.0860(2) 0.0245(11) Uani 1 1 d . . . H13A H 0.0376 -0.0483 0.0626 0.029 Uiso 1 1 calc R . . H13B H 0.0127 0.0240 0.0772 0.029 Uiso 1 1 calc R . . C16 C 0.05134(17) 0.3234(3) 0.2313(2) 0.0214(10) Uani 1 1 d . . . H16A H 0.0501 0.3734 0.2511 0.026 Uiso 1 1 calc R . . H16B H 0.0190 0.3042 0.2060 0.026 Uiso 1 1 calc R . . C15 C 0.13347(17) 0.2962(3) 0.1209(2) 0.0235(11) Uani 1 1 d . . . H15A H 0.1539 0.2519 0.1458 0.028 Uiso 1 1 calc R . . H15B H 0.1536 0.3385 0.1184 0.028 Uiso 1 1 calc R . . C17 C 0.13784(17) 0.0222(3) 0.2978(2) 0.0240(11) Uani 1 1 d . . . H17A H 0.1589 0.0649 0.2977 0.029 Uiso 1 1 calc R . . H17B H 0.1575 -0.0216 0.3241 0.029 Uiso 1 1 calc R . . C14 C 0.10084(17) 0.2623(3) 0.0600(2) 0.0230(11) Uani 1 1 d . . . H14A H 0.0705 0.2911 0.0431 0.028 Uiso 1 1 calc R . . H14B H 0.1146 0.2736 0.0352 0.028 Uiso 1 1 calc R . . C18 C 0.10768(18) 0.0585(3) 0.3212(2) 0.0268(11) Uani 1 1 d . . . H18A H 0.0766 0.0323 0.3013 0.032 Uiso 1 1 calc R . . H18B H 0.1223 0.0462 0.3630 0.032 Uiso 1 1 calc R . . C19 C 0.10621(17) -0.1531(3) 0.2720(2) 0.0245(11) Uani 1 1 d . . . C20 C 0.0865(2) -0.1514(3) 0.3067(3) 0.0362(14) Uani 1 1 d . . . H20 H 0.0645 -0.1102 0.3011 0.043 Uiso 1 1 calc R . . C23 C 0.1487(2) -0.2731(4) 0.3222(3) 0.0412(15) Uani 1 1 d . . . H23 H 0.1700 -0.3154 0.3271 0.049 Uiso 1 1 calc R . . C22 C 0.1286(2) -0.2693(4) 0.3570(3) 0.0388(14) Uani 1 1 d . . . H22 H 0.1363 -0.3094 0.3860 0.047 Uiso 1 1 calc R . . C24 C 0.1373(2) -0.2142(3) 0.2800(3) 0.0350(13) Uani 1 1 d . . . H24 H 0.1511 -0.2161 0.2562 0.042 Uiso 1 1 calc R . . C21 C 0.0983(2) -0.2092(4) 0.3501(3) 0.0445(16) Uani 1 1 d . . . H21 H 0.0851 -0.2065 0.3746 0.053 Uiso 1 1 calc R . . C25 C 0.04607(18) -0.1675(3) 0.1321(2) 0.0239(11) Uani 1 1 d . . . C28 C 0.0711(2) -0.2260(3) 0.1211(2) 0.0327(13) Uani 1 1 d . . . H28 H 0.1035 -0.2182 0.1353 0.039 Uiso 1 1 calc R . . C29 C 0.0494(2) -0.2948(3) 0.0901(2) 0.0338(13) Uani 1 1 d . . . H29 H 0.0667 -0.3341 0.0826 0.041 Uiso 1 1 calc R . . C26 C -0.00115(19) -0.1786(3) 0.1107(2) 0.0295(12) Uani 1 1 d . . . H26 H -0.0188 -0.1388 0.1172 0.035 Uiso 1 1 calc R . . C27 C -0.0225(2) -0.2486(3) 0.0795(2) 0.0305(12) Uani 1 1 d . . . H27 H -0.0550 -0.2565 0.0647 0.037 Uiso 1 1 calc R . . C35 C 0.10947(18) -0.0995(3) 0.0331(2) 0.0250(11) Uani 1 1 d . . . H35 H 0.0826 -0.0890 -0.0034 0.030 Uiso 1 1 calc R . . C30 C 0.12708(17) -0.0391(3) 0.0750(2) 0.0218(10) Uani 1 1 d . . . C31 C 0.16672(18) -0.0549(3) 0.1279(2) 0.0276(12) Uani 1 1 d . . . H31 H 0.1794 -0.0137 0.1567 0.033 Uiso 1 1 calc R . . C32 C 0.18799(19) -0.1308(3) 0.1390(2) 0.0300(12) Uani 1 1 d . . . H32 H 0.2149 -0.1414 0.1754 0.036 Uiso 1 1 calc R . . C33 C 0.17019(19) -0.1902(3) 0.0974(2) 0.0297(12) Uani 1 1 d . . . H33 H 0.1849 -0.2419 0.1050 0.036 Uiso 1 1 calc R . . C34 C 0.13084(19) -0.1751(3) 0.0443(2) 0.0301(12) Uani 1 1 d . . . H34 H 0.1185 -0.2164 0.0156 0.036 Uiso 1 1 calc R . . C41 C 0.19608(19) 0.1791(3) 0.0721(2) 0.0269(12) Uani 1 1 d . . . H41 H 0.2003 0.2053 0.1061 0.032 Uiso 1 1 calc R . . C36 C 0.15753(17) 0.1293(3) 0.0405(2) 0.0207(10) Uani 1 1 d . . . C39 C 0.22253(19) 0.1525(3) 0.0058(2) 0.0304(12) Uani 1 1 d . . . H39 H 0.2449 0.1603 -0.0062 0.036 Uiso 1 1 calc R . . C40 C 0.22814(19) 0.1908(3) 0.0542(2) 0.0299(12) Uani 1 1 d . . . H40 H 0.2542 0.2255 0.0756 0.036 Uiso 1 1 calc R . . C37 C 0.15221(19) 0.0903(3) -0.0088(2) 0.0310(12) Uani 1 1 d . . . H37 H 0.1263 0.0555 -0.0306 0.037 Uiso 1 1 calc R . . C38 C 0.1848(2) 0.1027(4) -0.0258(3) 0.0389(14) Uani 1 1 d . . . H38 H 0.1812 0.0765 -0.0595 0.047 Uiso 1 1 calc R . . C42 C 0.06424(18) 0.4811(3) 0.0474(2) 0.0238(11) Uani 1 1 d . . . H42 H 0.0362 0.4507 0.0331 0.029 Uiso 1 1 calc R . . C45 C 0.14434(19) 0.5721(3) 0.0891(2) 0.0303(12) Uani 1 1 d . . . H45 H 0.1718 0.6042 0.1036 0.036 Uiso 1 1 calc R . . C47 C 0.09935(17) 0.4707(3) 0.1039(2) 0.0203(10) Uani 1 1 d . . . C46 C 0.13961(19) 0.5169(3) 0.1248(2) 0.0268(11) Uani 1 1 d . . . H46 H 0.1640 0.5106 0.1637 0.032 Uiso 1 1 calc R . . C44 C 0.1086(2) 0.5810(3) 0.0314(2) 0.0284(12) Uani 1 1 d . . . H44 H 0.1120 0.6186 0.0068 0.034 Uiso 1 1 calc R . . C43 C 0.0691(2) 0.5357(3) 0.0108(2) 0.0289(12) Uani 1 1 d . . . H43 H 0.0450 0.5411 -0.0284 0.035 Uiso 1 1 calc R . . C49 C -0.00087(17) 0.4853(3) 0.1609(2) 0.0272(12) Uani 1 1 d . . . H49 H -0.0178 0.4368 0.1437 0.033 Uiso 1 1 calc R . . C48 C 0.04648(17) 0.4884(3) 0.1797(2) 0.0221(10) Uani 1 1 d . . . C53 C 0.07046(19) 0.5599(3) 0.2041(2) 0.0267(11) Uani 1 1 d . . . H53 H 0.1029 0.5638 0.2171 0.032 Uiso 1 1 calc R . . C50 C -0.0237(2) 0.5517(4) 0.1668(3) 0.0376(14) Uani 1 1 d . . . H50 H -0.0560 0.5483 0.1544 0.045 Uiso 1 1 calc R . . C52 C 0.0464(2) 0.6265(3) 0.2094(2) 0.0340(13) Uani 1 1 d . . . H52 H 0.0627 0.6754 0.2265 0.041 Uiso 1 1 calc R . . C51 C 0.0000(2) 0.6218(3) 0.1902(2) 0.0336(14) Uani 1 1 d . . . H51 H -0.0160 0.6679 0.1931 0.040 Uiso 1 1 calc R . . C56 C 0.17925(19) 0.3774(3) 0.3295(2) 0.0276(12) Uani 1 1 d . . . H56 H 0.1900 0.3395 0.3119 0.033 Uiso 1 1 calc R . . C54 C 0.14312(17) 0.3568(3) 0.3388(2) 0.0232(11) Uani 1 1 d . . . C58 C 0.1848(2) 0.5072(4) 0.3725(3) 0.0433(16) Uani 1 1 d . . . H58 H 0.1996 0.5586 0.3849 0.052 Uiso 1 1 calc R . . C57 C 0.1488(2) 0.4878(4) 0.3814(3) 0.0392(15) Uani 1 1 d . . . H57 H 0.1382 0.5262 0.3988 0.047 Uiso 1 1 calc R . . C55 C 0.12771(19) 0.4120(3) 0.3649(2) 0.0317(13) Uani 1 1 d . . . H55 H 0.1029 0.3980 0.3715 0.038 Uiso 1 1 calc R . . C62 C 0.25774(19) 0.1343(3) 0.5051(2) 0.0309(12) Uani 1 1 d . . . H62 H 0.2847 0.1203 0.5406 0.037 Uiso 1 1 calc R . . C61 C 0.2136(2) 0.1232(3) 0.4980(2) 0.0310(13) Uani 1 1 d . . . H61 H 0.2103 0.1000 0.5284 0.037 Uiso 1 1 calc R . . C63 C 0.26219(19) 0.1659(3) 0.4598(2) 0.0286(12) Uani 1 1 d . . . H63 H 0.2923 0.1719 0.4642 0.034 Uiso 1 1 calc R . . C59 C 0.17921(17) 0.1780(3) 0.4016(2) 0.0217(11) Uani 1 1 d . . . C60 C 0.17453(19) 0.1460(3) 0.4468(2) 0.0277(12) Uani 1 1 d . . . H60 H 0.1444 0.1398 0.4424 0.033 Uiso 1 1 calc R . . C64 C 0.22337(18) 0.1887(3) 0.4086(2) 0.0243(11) Uani 1 1 d . . . H64 H 0.2268 0.2117 0.3783 0.029 Uiso 1 1 calc R . . C65 C 0.2772(2) 0.1676(4) 0.2485(2) 0.0334(13) Uani 1 1 d . . . F3 F 0.31607(12) 0.1876(2) 0.29700(15) 0.0454(9) Uani 1 1 d . . . F1 F 0.26820(13) 0.2283(2) 0.21098(15) 0.0533(10) Uani 1 1 d . . . F2 F 0.28701(14) 0.1020(2) 0.22789(18) 0.0598(11) Uani 1 1 d . . . O1 O 0.19150(13) 0.1314(2) 0.20186(17) 0.0361(9) Uani 1 1 d . . . O2 O 0.22313(16) 0.2281(3) 0.2803(2) 0.0543(12) Uani 1 1 d . . . O3 O 0.24386(16) 0.0870(3) 0.3016(2) 0.0584(14) Uani 1 1 d . . . C66 C 0.0028(2) -0.3067(3) 0.0700(2) 0.0339(13) Uani 1 1 d . . . H66 H -0.0121 -0.3549 0.0495 0.041 Uiso 1 1 calc R . . C67 C 0.1999(2) 0.4534(3) 0.3459(3) 0.0375(14) Uani 1 1 d . . . H67 H 0.2243 0.4682 0.3388 0.045 Uiso 1 1 calc R . . C68 C 0.2283(3) 0.4506(5) 0.0810(5) 0.089(3) Uani 1 1 d . . . H68A H 0.2471 0.4717 0.0643 0.106 Uiso 1 1 calc R . . H68B H 0.2209 0.4970 0.0985 0.106 Uiso 1 1 calc R . . Cl3 Cl 0.17319(9) 0.40895(14) 0.02174(11) 0.0815(7) Uani 1 1 d . . . Cl4 Cl 0.25918(9) 0.38739(13) 0.13066(12) 0.0884(8) 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 Ag1 0.0268(2) 0.01464(19) 0.0243(2) 0.00184(15) 0.01428(17) 0.00014(15) Ag2 0.0254(2) 0.0223(2) 0.0274(2) 0.00040(16) 0.01446(18) 0.00290(15) Ag3 0.0243(2) 0.0260(2) 0.0249(2) -0.00215(16) 0.01172(17) -0.00570(16) Cl2 0.0267(7) 0.0320(7) 0.0315(7) -0.0086(6) 0.0163(6) -0.0070(5) Cl1 0.0247(7) 0.0329(7) 0.0300(7) -0.0056(6) 0.0111(6) 0.0047(5) S5 0.0292(7) 0.0348(8) 0.0350(8) -0.0003(6) 0.0152(6) -0.0007(6) C1 0.021(2) 0.016(2) 0.027(3) 0.001(2) 0.015(2) 0.0014(19) C2 0.029(3) 0.019(3) 0.024(3) 0.000(2) 0.014(2) 0.002(2) C3 0.026(3) 0.019(3) 0.019(2) -0.003(2) 0.009(2) -0.004(2) C4 0.020(3) 0.025(3) 0.023(3) 0.002(2) 0.012(2) 0.000(2) N8 0.024(2) 0.018(2) 0.023(2) -0.0018(17) 0.0124(19) -0.0055(17) N1 0.019(2) 0.014(2) 0.026(2) 0.0005(17) 0.0098(18) -0.0028(16) N4 0.027(2) 0.0132(19) 0.022(2) -0.0013(16) 0.0146(19) -0.0010(16) N6 0.021(2) 0.016(2) 0.024(2) -0.0006(17) 0.0120(18) 0.0031(16) N5 0.025(2) 0.016(2) 0.021(2) 0.0004(17) 0.0113(18) -0.0016(17) N2 0.024(2) 0.015(2) 0.025(2) 0.0037(17) 0.0162(18) 0.0040(16) N7 0.020(2) 0.018(2) 0.017(2) 0.0052(16) 0.0090(17) 0.0002(16) N3 0.024(2) 0.017(2) 0.025(2) -0.0013(17) 0.0162(19) -0.0023(17) C12 0.026(3) 0.020(3) 0.017(2) -0.0026(19) 0.012(2) -0.005(2) C8 0.024(3) 0.022(3) 0.019(2) -0.003(2) 0.013(2) 0.000(2) C9 0.020(2) 0.013(2) 0.020(2) 0.0015(19) 0.007(2) 0.0011(19) C10 0.020(2) 0.015(2) 0.022(2) -0.0001(19) 0.011(2) 0.0002(19) C11 0.023(3) 0.019(2) 0.023(3) 0.000(2) 0.013(2) -0.001(2) C7 0.022(2) 0.017(2) 0.020(2) 0.0001(19) 0.011(2) -0.0003(19) C6 0.027(3) 0.013(2) 0.029(3) 0.003(2) 0.019(2) 0.0013(19) C5 0.027(3) 0.015(2) 0.031(3) 0.004(2) 0.017(2) 0.000(2) C13 0.028(3) 0.019(3) 0.030(3) 0.004(2) 0.017(2) 0.001(2) C16 0.025(3) 0.021(3) 0.020(2) 0.002(2) 0.012(2) -0.001(2) C15 0.026(3) 0.021(3) 0.029(3) 0.000(2) 0.018(2) 0.003(2) C17 0.028(3) 0.018(3) 0.027(3) 0.001(2) 0.015(2) -0.002(2) C14 0.027(3) 0.016(2) 0.026(3) 0.001(2) 0.013(2) 0.004(2) C18 0.028(3) 0.020(3) 0.026(3) -0.002(2) 0.009(2) -0.008(2) C19 0.024(3) 0.020(3) 0.023(3) -0.002(2) 0.007(2) -0.002(2) C20 0.046(4) 0.022(3) 0.050(4) 0.011(3) 0.032(3) 0.005(3) C23 0.048(4) 0.027(3) 0.045(4) 0.009(3) 0.020(3) 0.011(3) C22 0.054(4) 0.027(3) 0.032(3) 0.008(3) 0.019(3) -0.005(3) C24 0.038(3) 0.032(3) 0.040(3) 0.009(3) 0.023(3) 0.006(3) C21 0.064(4) 0.038(4) 0.047(4) 0.011(3) 0.040(4) 0.003(3) C25 0.032(3) 0.021(3) 0.023(3) 0.002(2) 0.017(2) -0.002(2) C28 0.035(3) 0.028(3) 0.038(3) -0.003(2) 0.020(3) -0.002(2) C29 0.047(4) 0.022(3) 0.039(3) -0.007(2) 0.026(3) 0.005(2) C26 0.036(3) 0.024(3) 0.030(3) -0.008(2) 0.017(3) -0.001(2) C27 0.034(3) 0.026(3) 0.031(3) -0.008(2) 0.016(3) -0.010(2) C35 0.024(3) 0.023(3) 0.026(3) -0.001(2) 0.010(2) -0.005(2) C30 0.022(2) 0.019(3) 0.028(3) 0.002(2) 0.014(2) 0.001(2) C31 0.030(3) 0.021(3) 0.030(3) 0.002(2) 0.014(2) -0.002(2) C32 0.027(3) 0.028(3) 0.033(3) 0.004(2) 0.012(2) 0.002(2) C33 0.035(3) 0.022(3) 0.045(3) 0.005(2) 0.029(3) 0.009(2) C34 0.040(3) 0.024(3) 0.031(3) -0.006(2) 0.021(3) -0.005(2) C41 0.036(3) 0.019(3) 0.030(3) 0.000(2) 0.020(3) 0.002(2) C36 0.027(3) 0.015(2) 0.024(3) 0.005(2) 0.015(2) 0.004(2) C39 0.034(3) 0.034(3) 0.037(3) 0.006(2) 0.027(3) 0.004(2) C40 0.029(3) 0.026(3) 0.036(3) 0.001(2) 0.016(3) 0.000(2) C37 0.035(3) 0.031(3) 0.034(3) -0.007(2) 0.022(3) -0.008(2) C38 0.048(4) 0.039(3) 0.047(4) -0.010(3) 0.036(3) -0.007(3) C42 0.034(3) 0.013(2) 0.027(3) -0.001(2) 0.017(2) 0.000(2) C45 0.033(3) 0.025(3) 0.041(3) -0.002(2) 0.025(3) -0.006(2) C47 0.027(3) 0.011(2) 0.023(3) 0.0003(19) 0.013(2) 0.0001(19) C46 0.033(3) 0.019(3) 0.029(3) 0.000(2) 0.016(2) -0.003(2) C44 0.047(3) 0.015(3) 0.032(3) 0.003(2) 0.026(3) 0.002(2) C43 0.038(3) 0.024(3) 0.026(3) 0.003(2) 0.017(2) 0.005(2) C49 0.023(3) 0.028(3) 0.029(3) 0.002(2) 0.012(2) 0.002(2) C48 0.030(3) 0.020(3) 0.020(3) 0.003(2) 0.015(2) 0.000(2) C53 0.030(3) 0.022(3) 0.032(3) 0.002(2) 0.018(2) 0.001(2) C50 0.030(3) 0.039(3) 0.048(4) 0.007(3) 0.023(3) 0.011(3) C52 0.055(4) 0.019(3) 0.030(3) -0.005(2) 0.023(3) -0.004(3) C51 0.048(4) 0.028(3) 0.036(3) 0.009(2) 0.029(3) 0.015(3) C56 0.034(3) 0.021(3) 0.028(3) 0.003(2) 0.016(2) -0.002(2) C54 0.024(3) 0.017(2) 0.020(3) 0.004(2) 0.004(2) 0.004(2) C58 0.046(4) 0.020(3) 0.044(4) 0.004(3) 0.007(3) -0.005(3) C57 0.034(3) 0.031(3) 0.035(3) -0.006(3) 0.004(3) 0.011(3) C55 0.028(3) 0.026(3) 0.034(3) -0.004(2) 0.009(2) 0.002(2) C62 0.031(3) 0.025(3) 0.027(3) -0.002(2) 0.007(2) 0.003(2) C61 0.043(3) 0.023(3) 0.026(3) 0.004(2) 0.016(3) 0.004(2) C63 0.027(3) 0.026(3) 0.030(3) -0.003(2) 0.013(2) 0.001(2) C59 0.029(3) 0.015(2) 0.019(3) 0.0013(19) 0.012(2) 0.001(2) C60 0.033(3) 0.026(3) 0.026(3) 0.000(2) 0.017(2) -0.003(2) C64 0.031(3) 0.019(3) 0.025(3) 0.000(2) 0.016(2) -0.002(2) C65 0.035(3) 0.033(3) 0.032(3) 0.002(3) 0.017(3) -0.004(2) F3 0.0356(19) 0.055(2) 0.039(2) 0.0002(17) 0.0137(17) -0.0101(17) F1 0.047(2) 0.068(3) 0.041(2) 0.0157(19) 0.0196(18) -0.0149(19) F2 0.056(2) 0.063(3) 0.072(3) -0.021(2) 0.041(2) 0.005(2) O1 0.027(2) 0.033(2) 0.042(2) -0.0012(18) 0.0131(19) -0.0048(17) O2 0.055(3) 0.057(3) 0.059(3) -0.022(2) 0.035(3) 0.002(2) O3 0.044(3) 0.070(3) 0.059(3) 0.028(3) 0.025(2) -0.002(2) C66 0.047(4) 0.024(3) 0.026(3) -0.004(2) 0.014(3) -0.004(3) C67 0.038(3) 0.027(3) 0.043(4) 0.007(3) 0.017(3) -0.008(3) C68 0.087(6) 0.060(5) 0.184(10) -0.045(6) 0.116(7) -0.036(5) Cl3 0.1001(17) 0.0807(15) 0.1029(17) 0.0476(13) 0.0802(16) 0.0477(13) Cl4 0.0816(16) 0.0457(12) 0.118(2) -0.0185(12) 0.0352(15) -0.0208(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C1 2.095(5) . ? Ag1 C3 2.095(5) . ? Ag1 Ag2 3.0367(6) . ? Ag1 Ag3 3.1470(6) . ? Ag2 C2 2.092(5) . ? Ag2 Cl1 2.3485(13) . ? Ag2 Ag3 3.3403(7) . ? Ag3 C4 2.097(5) . ? Ag3 Cl2 2.3630(13) . ? Ag3 Ag3 3.2335(8) 2 ? S5 O2 1.425(4) . ? S5 O1 1.439(4) . ? S5 O3 1.444(5) . ? S5 C65 1.798(6) . ? C1 N1 1.342(6) . ? C1 N2 1.351(6) . ? C2 N4 1.355(6) . ? C2 N3 1.365(6) . ? C3 N5 1.349(6) . ? C3 N6 1.354(6) . ? C4 N7 1.357(6) . ? C4 N8 1.359(6) . ? N8 C12 1.398(6) . ? N8 C18 1.456(6) . ? N1 C5 1.387(6) . ? N1 C17 1.462(6) . ? N4 C8 1.398(6) . ? N4 C14 1.469(6) . ? N6 C10 1.389(6) . ? N6 C16 1.477(6) . ? N5 C9 1.399(6) . ? N5 C15 1.464(6) . ? N2 C6 1.405(6) . ? N2 C13 1.466(6) . ? N7 C11 1.401(6) . ? N7 C16 1.427(6) . ? N3 C7 1.395(6) . ? N3 C13 1.440(6) . ? C12 C11 1.360(7) . ? C12 C59 1.471(7) . ? C8 C7 1.333(7) . ? C8 C36 1.483(7) . ? C9 C10 1.343(7) . ? C9 C47 1.489(6) . ? C10 C48 1.479(7) . ? C11 C54 1.485(7) . ? C7 C30 1.483(7) . ? C6 C5 1.341(7) . ? C6 C25 1.480(7) . ? C5 C19 1.479(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C15 C14 1.537(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 C18 1.538(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.374(8) . ? C19 C24 1.377(7) . ? C20 C21 1.394(8) . ? C20 H20 0.9500 . ? C23 C24 1.386(8) . ? C23 C22 1.387(8) . ? C23 H23 0.9500 . ? C22 C21 1.357(9) . ? C22 H22 0.9500 . ? C24 H24 0.9500 . ? C21 H21 0.9500 . ? C25 C26 1.382(7) . ? C25 C28 1.394(7) . ? C28 C29 1.375(7) . ? C28 H28 0.9500 . ? C29 C66 1.372(8) . ? C29 H29 0.9500 . ? C26 C27 1.389(7) . ? C26 H26 0.9500 . ? C27 C66 1.376(8) . ? C27 H27 0.9500 . ? C35 C30 1.388(7) . ? C35 C34 1.388(7) . ? C35 H35 0.9500 . ? C30 C31 1.388(7) . ? C31 C32 1.391(7) . ? C31 H31 0.9500 . ? C32 C33 1.372(8) . ? C32 H32 0.9500 . ? C33 C34 1.384(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C41 C40 1.376(7) . ? C41 C36 1.391(7) . ? C41 H41 0.9500 . ? C36 C37 1.395(7) . ? C39 C40 1.364(7) . ? C39 C38 1.373(8) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C37 C38 1.378(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C42 C47 1.379(7) . ? C42 C43 1.394(7) . ? C42 H42 0.9500 . ? C45 C46 1.381(7) . ? C45 C44 1.402(8) . ? C45 H45 0.9500 . ? C47 C46 1.386(7) . ? C46 H46 0.9500 . ? C44 C43 1.358(8) . ? C44 H44 0.9500 . ? C43 H43 0.9500 . ? C49 C50 1.382(7) . ? C49 C48 1.387(7) . ? C49 H49 0.9500 . ? C48 C53 1.386(7) . ? C53 C52 1.404(7) . ? C53 H53 0.9500 . ? C50 C51 1.360(8) . ? C50 H50 0.9500 . ? C52 C51 1.354(8) . ? C52 H52 0.9500 . ? C51 H51 0.9500 . ? C56 C54 1.379(7) . ? C56 C67 1.386(7) . ? C56 H56 0.9500 . ? C54 C55 1.387(7) . ? C58 C57 1.361(9) . ? C58 C67 1.378(9) . ? C58 H58 0.9500 . ? C57 C55 1.390(8) . ? C57 H57 0.9500 . ? C55 H55 0.9500 . ? C62 C61 1.388(8) . ? C62 C63 1.389(8) . ? C62 H62 0.9500 . ? C61 C60 1.382(7) . ? C61 H61 0.9500 . ? C63 C64 1.378(7) . ? C63 H63 0.9500 . ? C59 C64 1.389(7) . ? C59 C60 1.394(7) . ? C60 H60 0.9500 . ? C64 H64 0.9500 . ? C65 F2 1.324(7) . ? C65 F3 1.331(6) . ? C65 F1 1.339(6) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 Cl4 1.590(11) . ? C68 Cl3 1.846(9) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? 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 C1 Ag1 C3 173.29(18) . . ? C1 Ag1 Ag2 100.86(13) . . ? C3 Ag1 Ag2 73.54(13) . . ? C1 Ag1 Ag3 73.06(13) . . ? C3 Ag1 Ag3 100.93(14) . . ? Ag2 Ag1 Ag3 65.362(14) . . ? C2 Ag2 Cl1 176.79(14) . . ? C2 Ag2 Ag1 63.85(14) . . ? Cl1 Ag2 Ag1 114.19(4) . . ? C2 Ag2 Ag3 109.22(14) . . ? Cl1 Ag2 Ag3 70.90(4) . . ? Ag1 Ag2 Ag3 58.911(13) . . ? C4 Ag3 Cl2 166.71(14) . . ? C4 Ag3 Ag1 62.75(13) . . ? Cl2 Ag3 Ag1 111.29(3) . . ? C4 Ag3 Ag3 71.36(13) . 2 ? Cl2 Ag3 Ag3 110.93(3) . 2 ? Ag1 Ag3 Ag3 132.76(2) . 2 ? C4 Ag3 Ag2 105.14(13) . . ? Cl2 Ag3 Ag2 78.33(4) . . ? Ag1 Ag3 Ag2 55.727(11) . . ? Ag3 Ag3 Ag2 155.135(13) 2 . ? O2 S5 O1 114.7(3) . . ? O2 S5 O3 114.1(3) . . ? O1 S5 O3 116.3(3) . . ? O2 S5 C65 103.2(3) . . ? O1 S5 C65 102.4(3) . . ? O3 S5 C65 103.6(3) . . ? N1 C1 N2 104.0(4) . . ? N1 C1 Ag1 125.8(3) . . ? N2 C1 Ag1 129.6(3) . . ? N4 C2 N3 103.4(4) . . ? N4 C2 Ag2 128.9(3) . . ? N3 C2 Ag2 127.4(4) . . ? N5 C3 N6 103.9(4) . . ? N5 C3 Ag1 124.4(3) . . ? N6 C3 Ag1 130.2(4) . . ? N7 C4 N8 104.1(4) . . ? N7 C4 Ag3 129.4(4) . . ? N8 C4 Ag3 125.6(4) . . ? C4 N8 C12 112.1(4) . . ? C4 N8 C18 124.7(4) . . ? C12 N8 C18 122.7(4) . . ? C1 N1 C5 112.3(4) . . ? C1 N1 C17 123.5(4) . . ? C5 N1 C17 124.2(4) . . ? C2 N4 C8 111.5(4) . . ? C2 N4 C14 123.9(4) . . ? C8 N4 C14 124.3(4) . . ? C3 N6 C10 111.8(4) . . ? C3 N6 C16 125.0(4) . . ? C10 N6 C16 123.2(4) . . ? C3 N5 C9 111.6(4) . . ? C3 N5 C15 123.2(4) . . ? C9 N5 C15 125.1(4) . . ? C1 N2 C6 111.2(4) . . ? C1 N2 C13 125.6(4) . . ? C6 N2 C13 122.9(4) . . ? C4 N7 C11 111.3(4) . . ? C4 N7 C16 123.8(4) . . ? C11 N7 C16 124.3(4) . . ? C2 N3 C7 111.7(4) . . ? C2 N3 C13 122.7(4) . . ? C7 N3 C13 124.9(4) . . ? C11 C12 N8 105.6(4) . . ? C11 C12 C59 131.1(4) . . ? N8 C12 C59 123.1(4) . . ? C7 C8 N4 107.0(4) . . ? C7 C8 C36 127.7(4) . . ? N4 C8 C36 124.9(4) . . ? C10 C9 N5 106.2(4) . . ? C10 C9 C47 131.4(4) . . ? N5 C9 C47 122.2(4) . . ? C9 C10 N6 106.5(4) . . ? C9 C10 C48 130.1(4) . . ? N6 C10 C48 123.4(4) . . ? C12 C11 N7 106.8(4) . . ? C12 C11 C54 130.8(5) . . ? N7 C11 C54 122.3(4) . . ? C8 C7 N3 106.4(4) . . ? C8 C7 C30 131.3(5) . . ? N3 C7 C30 122.0(4) . . ? C5 C6 N2 106.1(4) . . ? C5 C6 C25 130.1(4) . . ? N2 C6 C25 123.8(4) . . ? C6 C5 N1 106.4(4) . . ? C6 C5 C19 130.0(5) . . ? N1 C5 C19 123.6(5) . . ? N3 C13 N2 111.2(4) . . ? N3 C13 H13A 109.4 . . ? N2 C13 H13A 109.4 . . ? N3 C13 H13B 109.4 . . ? N2 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N7 C16 N6 111.0(4) . . ? N7 C16 H16A 109.4 . . ? N6 C16 H16A 109.4 . . ? N7 C16 H16B 109.4 . . ? N6 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N5 C15 C14 113.4(4) . . ? N5 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? N5 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N1 C17 C18 113.0(4) . . ? N1 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N1 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N4 C14 C15 113.5(4) . . ? N4 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? N4 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? N8 C18 C17 112.5(4) . . ? N8 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? N8 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C24 118.6(5) . . ? C20 C19 C5 122.0(5) . . ? C24 C19 C5 119.4(5) . . ? C19 C20 C21 121.1(5) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C24 C23 C22 118.9(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C21 C22 C23 120.9(6) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C19 C24 C23 121.1(6) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C22 C21 C20 119.3(6) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C26 C25 C28 119.4(5) . . ? C26 C25 C6 120.7(5) . . ? C28 C25 C6 119.8(5) . . ? C29 C28 C25 120.6(5) . . ? C29 C28 H28 119.7 . . ? C25 C28 H28 119.7 . . ? C66 C29 C28 119.9(5) . . ? C66 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C25 C26 C27 119.3(5) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C66 C27 C26 120.8(5) . . ? C66 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C30 C35 C34 120.4(5) . . ? C30 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C30 C31 119.1(5) . . ? C35 C30 C7 122.9(5) . . ? C31 C30 C7 117.9(4) . . ? C30 C31 C32 120.3(5) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 120.1(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.1(5) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C40 C41 C36 120.4(5) . . ? C40 C41 H41 119.8 . . ? C36 C41 H41 119.8 . . ? C41 C36 C37 119.1(5) . . ? C41 C36 C8 123.3(4) . . ? C37 C36 C8 117.6(4) . . ? C40 C39 C38 120.5(5) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.0(5) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C38 C37 C36 119.5(5) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C39 C38 C37 120.5(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C47 C42 C43 121.1(5) . . ? C47 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C46 C45 C44 120.0(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C42 C47 C46 119.0(5) . . ? C42 C47 C9 119.5(4) . . ? C46 C47 C9 121.4(4) . . ? C45 C46 C47 120.2(5) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C43 C44 C45 120.0(5) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C43 C42 119.7(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C50 C49 C48 120.9(5) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C53 C48 C49 118.6(5) . . ? C53 C48 C10 120.7(5) . . ? C49 C48 C10 120.6(4) . . ? C48 C53 C52 119.3(5) . . ? C48 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C51 C50 C49 120.0(5) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C52 C53 120.7(5) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C52 C51 C50 120.4(5) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C54 C56 C67 120.0(5) . . ? C54 C56 H56 120.0 . . ? C67 C56 H56 120.0 . . ? C56 C54 C55 119.9(5) . . ? C56 C54 C11 120.1(5) . . ? C55 C54 C11 119.9(5) . . ? C57 C58 C67 120.9(6) . . ? C57 C58 H58 119.6 . . ? C67 C58 H58 119.6 . . ? C58 C57 C55 120.0(6) . . ? C58 C57 H57 120.0 . . ? C55 C57 H57 120.0 . . ? C54 C55 C57 119.6(6) . . ? C54 C55 H55 120.2 . . ? C57 C55 H55 120.2 . . ? C61 C62 C63 119.6(5) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C60 C61 C62 119.9(5) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C64 C63 C62 120.8(5) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C64 C59 C60 119.8(5) . . ? C64 C59 C12 121.1(4) . . ? C60 C59 C12 119.1(5) . . ? C61 C60 C59 120.2(5) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C63 C64 C59 119.7(5) . . ? C63 C64 H64 120.2 . . ? C59 C64 H64 120.2 . . ? F2 C65 F3 106.7(5) . . ? F2 C65 F1 107.8(5) . . ? F3 C65 F1 106.7(5) . . ? F2 C65 S5 112.0(4) . . ? F3 C65 S5 113.0(4) . . ? F1 C65 S5 110.4(4) . . ? C29 C66 C27 120.0(5) . . ? C29 C66 H66 120.0 . . ? C27 C66 H66 120.0 . . ? C58 C67 C56 119.6(6) . . ? C58 C67 H67 120.2 . . ? C56 C67 H67 120.2 . . ? Cl4 C68 Cl3 114.7(4) . . ? Cl4 C68 H68A 108.6 . . ? Cl3 C68 H68A 108.6 . . ? Cl4 C68 H68B 108.6 . . ? Cl3 C68 H68B 108.6 . . ? H68A C68 H68B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.888 _refine_diff_density_min -1.626 _refine_diff_density_rms 0.127 data_5 _database_code_depnum_ccdc_archive 'CCDC 888976' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 F6 N8 O6 Pd S2' _chemical_formula_weight 1361.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.290(3) _cell_length_b 8.8229(9) _cell_length_c 29.690(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.8150(10) _cell_angle_gamma 90.00 _cell_volume 7341.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9851 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD Detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75128 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.35 _reflns_number_total 14909 _reflns_number_gt 8650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four methtlene chloride and one water molecules were sqeezed out with SQUEEZE routine in Platon software package due to disorderness. ; _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^)+(0.0910P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14909 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1163 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Pd1 Pd 0.251102(13) 0.94659(4) 0.374595(12) 0.01502(11) Uani 1 1 d . . . S2 S 0.31217(5) 0.31152(16) 0.27771(5) 0.0285(3) Uani 1 1 d . . . S3 S 0.18995(5) 0.33954(17) 0.47021(5) 0.0341(4) Uani 1 1 d . . . C4 C 0.31551(16) 0.9394(5) 0.35500(14) 0.0145(9) Uani 1 1 d . . . C1 C 0.21757(16) 0.9542(5) 0.30952(15) 0.0157(10) Uani 1 1 d . . . C2 C 0.18665(16) 0.9531(5) 0.39465(15) 0.0152(10) Uani 1 1 d . . . C3 C 0.28450(16) 0.9692(5) 0.43969(15) 0.0129(10) Uani 1 1 d . . . C5 C 0.18860(16) 0.9336(5) 0.23481(15) 0.0157(10) Uani 1 1 d . . . C12 C 0.38057(16) 0.8871(6) 0.32148(16) 0.0186(11) Uani 1 1 d . . . C8 C 0.12156(16) 0.9142(5) 0.42979(15) 0.0173(11) Uani 1 1 d . . . C7 C 0.10948(17) 1.0155(5) 0.39565(15) 0.0144(10) Uani 1 1 d . . . C10 C 0.34384(17) 1.0538(6) 0.49253(15) 0.0188(10) Uani 1 1 d . . . C11 C 0.39239(18) 0.9970(6) 0.35278(17) 0.0212(11) Uani 1 1 d . . . C9 C 0.31135(18) 0.9856(6) 0.51431(16) 0.0216(11) Uani 1 1 d . . . C6 C 0.15509(17) 1.0046(5) 0.25527(16) 0.0172(10) Uani 1 1 d . . . C14 C 0.20089(18) 0.7740(6) 0.45735(18) 0.0228(12) Uani 1 1 d . . . H14A H 0.2212 0.7160 0.4389 0.027 Uiso 1 1 calc R . . H14B H 0.1809 0.7007 0.4715 0.027 Uiso 1 1 calc R . . C13 C 0.15464(17) 1.1194(6) 0.33382(15) 0.0186(11) Uani 1 1 d . . . H13A H 0.1766 1.2063 0.3407 0.022 Uiso 1 1 calc R . . H13B H 0.1231 1.1589 0.3204 0.022 Uiso 1 1 calc R . . C16 C 0.34599(19) 1.1283(6) 0.41044(16) 0.0228(12) Uani 1 1 d . . . H16A H 0.3769 1.1754 0.4225 0.027 Uiso 1 1 calc R . . H16B H 0.3234 1.2100 0.3993 0.027 Uiso 1 1 calc R . . C18 C 0.27093(16) 0.8318(6) 0.25691(16) 0.0184(11) Uani 1 1 d . . . H18A H 0.2909 0.9114 0.2455 0.022 Uiso 1 1 calc R . . H18B H 0.2620 0.7593 0.2317 0.022 Uiso 1 1 calc R . . C17 C 0.30122(17) 0.7482(5) 0.29518(17) 0.0172(11) Uani 1 1 d . . . H17A H 0.2802 0.6953 0.3141 0.021 Uiso 1 1 calc R . . H17B H 0.3208 0.6709 0.2822 0.021 Uiso 1 1 calc R . . C15 C 0.23226(17) 0.8578(5) 0.49418(15) 0.0175(10) Uani 1 1 d . . . H15A H 0.2124 0.9344 0.5072 0.021 Uiso 1 1 calc R . . H15B H 0.2432 0.7847 0.5187 0.021 Uiso 1 1 calc R . . C19 C 0.10731(15) 1.0652(5) 0.23747(15) 0.0152(10) Uani 1 1 d . . . C23 C 0.02220(18) 1.0785(6) 0.24148(19) 0.0288(13) Uani 1 1 d . . . H23 H -0.0048 1.0522 0.2557 0.035 Uiso 1 1 calc R . . C22 C 0.01762(19) 1.1768(7) 0.20501(18) 0.0324(14) Uani 1 1 d . . . H22 H -0.0130 1.2153 0.1934 0.039 Uiso 1 1 calc R . . C20 C 0.10143(18) 1.1630(6) 0.20141(16) 0.0216(11) Uani 1 1 d . . . H20 H 0.1283 1.1922 0.1874 0.026 Uiso 1 1 calc R . . C21 C 0.0567(2) 1.2196(6) 0.18520(19) 0.0307(14) Uani 1 1 d . . . H21 H 0.0530 1.2883 0.1603 0.037 Uiso 1 1 calc R . . C24 C 0.06735(18) 1.0182(6) 0.25717(18) 0.0277(13) Uani 1 1 d . . . H24 H 0.0709 0.9457 0.2811 0.033 Uiso 1 1 calc R . . C26 C 0.21817(19) 0.9535(6) 0.15933(18) 0.0287(12) Uani 1 1 d . . . H26 H 0.2428 1.0196 0.1724 0.034 Uiso 1 1 calc R . . C30 C 0.15087(19) 0.7938(6) 0.16651(16) 0.0232(11) Uani 1 1 d . . . H30 H 0.1298 0.7481 0.1848 0.028 Uiso 1 1 calc R . . C25 C 0.18673(17) 0.8927(6) 0.18654(16) 0.0187(11) Uani 1 1 d . . . C27 C 0.2142(2) 0.9195(7) 0.11362(18) 0.0322(13) Uani 1 1 d . . . H27 H 0.2362 0.9607 0.0954 0.039 Uiso 1 1 calc R . . C28 C 0.1779(2) 0.8250(6) 0.09442(18) 0.0315(14) Uani 1 1 d . . . H28 H 0.1749 0.8028 0.0628 0.038 Uiso 1 1 calc R . . C29 C 0.14599(19) 0.7623(6) 0.12052(19) 0.0281(13) Uani 1 1 d . . . H29 H 0.1210 0.6983 0.1070 0.034 Uiso 1 1 calc R . . C32 C 0.02152(17) 1.0326(6) 0.37396(16) 0.0222(11) Uani 1 1 d . . . H32 H 0.0192 0.9263 0.3782 0.027 Uiso 1 1 calc R . . C33 C -0.01926(18) 1.1166(7) 0.35920(17) 0.0268(12) Uani 1 1 d . . . H33 H -0.0493 1.0674 0.3524 0.032 Uiso 1 1 calc R . . C31 C 0.06534(18) 1.1031(6) 0.38251(16) 0.0196(11) Uani 1 1 d . . . C36 C 0.0680(2) 1.2599(6) 0.37846(18) 0.0252(13) Uani 1 1 d . . . H36 H 0.0979 1.3090 0.3857 0.030 Uiso 1 1 calc R . . C34 C -0.01599(19) 1.2714(6) 0.35447(18) 0.0264(13) Uani 1 1 d . . . H34 H -0.0440 1.3283 0.3445 0.032 Uiso 1 1 calc R . . C35 C 0.02776(18) 1.3460(6) 0.36407(17) 0.0229(12) Uani 1 1 d . . . H35 H 0.0299 1.4528 0.3608 0.027 Uiso 1 1 calc R . . C42 C 0.08592(19) 0.6888(7) 0.46334(19) 0.0313(14) Uani 1 1 d . . . H42 H 0.0992 0.6240 0.4428 0.038 Uiso 1 1 calc R . . C37 C 0.09380(17) 0.8487(6) 0.46271(17) 0.0207(11) Uani 1 1 d . . . C38 C 0.07491(18) 0.9406(7) 0.49350(16) 0.0280(12) Uani 1 1 d . . . H38 H 0.0807 1.0467 0.4937 0.034 Uiso 1 1 calc R . . C41 C 0.0581(2) 0.6292(8) 0.4950(2) 0.0376(16) Uani 1 1 d . . . H41 H 0.0519 0.5235 0.4957 0.045 Uiso 1 1 calc R . . C40 C 0.03986(19) 0.7253(8) 0.52477(19) 0.0330(15) Uani 1 1 d . . . H40 H 0.0215 0.6841 0.5463 0.040 Uiso 1 1 calc R . . C39 C 0.04738(19) 0.8782(7) 0.52426(18) 0.0314(13) Uani 1 1 d . . . H39 H 0.0338 0.9419 0.5449 0.038 Uiso 1 1 calc R . . C43 C 0.31195(18) 0.9575(6) 0.56397(16) 0.0247(12) Uani 1 1 d . . . C48 C 0.3495(2) 0.8803(7) 0.58713(19) 0.0340(14) Uani 1 1 d . . . H48 H 0.3746 0.8472 0.5713 0.041 Uiso 1 1 calc R . . C45 C 0.2783(2) 0.9781(7) 0.63370(19) 0.0347(14) Uani 1 1 d . . . H45 H 0.2540 1.0147 0.6500 0.042 Uiso 1 1 calc R . . C44 C 0.2762(2) 1.0055(7) 0.58816(17) 0.0326(14) Uani 1 1 d . . . H44 H 0.2496 1.0587 0.5728 0.039 Uiso 1 1 calc R . . C46 C 0.3165(2) 0.8962(8) 0.65582(19) 0.0422(17) Uani 1 1 d . . . H46 H 0.3178 0.8732 0.6872 0.051 Uiso 1 1 calc R . . C47 C 0.3518(2) 0.8492(8) 0.6329(2) 0.0408(16) Uani 1 1 d . . . H47 H 0.3782 0.7948 0.6482 0.049 Uiso 1 1 calc R . . C54 C 0.43098(19) 1.1030(7) 0.49195(18) 0.0297(13) Uani 1 1 d . . . H54 H 0.4323 1.0243 0.4703 0.036 Uiso 1 1 calc R . . C53 C 0.4718(2) 1.1905(7) 0.50680(19) 0.0353(14) Uani 1 1 d . . . H53 H 0.5004 1.1721 0.4943 0.042 Uiso 1 1 calc R . . C49 C 0.38840(18) 1.1335(6) 0.50951(16) 0.0236(12) Uani 1 1 d . . . C52 C 0.4710(2) 1.3010(7) 0.5386(2) 0.0374(15) Uani 1 1 d . . . H52 H 0.4990 1.3579 0.5483 0.045 Uiso 1 1 calc R . . C51 C 0.4294(2) 1.3311(7) 0.5572(2) 0.0388(15) Uani 1 1 d . . . H51 H 0.4291 1.4069 0.5799 0.047 Uiso 1 1 calc R . . C50 C 0.3881(2) 1.2492(6) 0.54229(19) 0.0275(13) Uani 1 1 d . . . H50 H 0.3594 1.2714 0.5543 0.033 Uiso 1 1 calc R . . C61 C 0.40924(17) 0.8123(6) 0.28904(16) 0.0177(11) Uani 1 1 d . . . C55 C 0.43820(17) 1.0815(6) 0.36527(16) 0.0197(11) Uani 1 1 d . . . C66 C 0.41510(18) 0.6583(6) 0.28955(18) 0.0257(12) Uani 1 1 d . . . H66 H 0.4017 0.5976 0.3110 0.031 Uiso 1 1 calc R . . C60 C 0.48007(18) 0.9982(6) 0.37935(16) 0.0240(12) Uani 1 1 d . . . H60 H 0.4794 0.8905 0.3795 0.029 Uiso 1 1 calc R . . C62 C 0.42881(18) 0.9051(7) 0.25768(17) 0.0270(13) Uani 1 1 d . . . H62 H 0.4233 1.0114 0.2562 0.032 Uiso 1 1 calc R . . C56 C 0.43864(19) 1.2374(6) 0.36454(17) 0.0219(12) Uani 1 1 d . . . H56 H 0.4103 1.2932 0.3549 0.026 Uiso 1 1 calc R . . C65 C 0.44119(19) 0.5921(7) 0.25804(19) 0.0330(14) Uani 1 1 d . . . H65 H 0.4444 0.4850 0.2571 0.040 Uiso 1 1 calc R . . C58 C 0.5236(2) 1.2325(7) 0.39278(19) 0.0293(14) Uani 1 1 d . . . H58 H 0.5524 1.2855 0.4024 0.035 Uiso 1 1 calc R . . C64 C 0.46232(19) 0.6818(6) 0.22817(19) 0.0299(14) Uani 1 1 d . . . H64 H 0.4807 0.6369 0.2072 0.036 Uiso 1 1 calc R . . C57 C 0.48179(19) 1.3116(7) 0.37831(18) 0.0304(13) Uani 1 1 d . . . H57 H 0.4826 1.4192 0.3778 0.036 Uiso 1 1 calc R . . C59 C 0.52274(18) 1.0759(7) 0.39310(19) 0.0321(14) Uani 1 1 d . . . H59 H 0.5512 1.0209 0.4027 0.038 Uiso 1 1 calc R . . C63 C 0.45656(19) 0.8324(7) 0.22904(18) 0.0295(13) Uani 1 1 d . . . H63 H 0.4722 0.8926 0.2091 0.035 Uiso 1 1 calc R . . C67 C 0.25007(19) 0.3459(6) 0.25367(18) 0.0236(12) Uani 1 1 d . . . C68 C 0.25226(19) 0.3776(6) 0.49260(16) 0.0225(11) Uani 1 1 d . . . O1 O 0.31870(15) 0.1528(4) 0.26968(14) 0.0375(10) Uani 1 1 d . . . O3 O 0.33813(13) 0.4112(4) 0.25185(14) 0.0348(10) Uani 1 1 d . . . O2 O 0.31301(15) 0.3531(5) 0.32465(13) 0.0438(11) Uani 1 1 d . . . O4 O 0.18483(16) 0.1816(5) 0.47882(16) 0.0483(12) Uani 1 1 d . . . O5 O 0.18742(17) 0.3803(6) 0.42292(14) 0.0520(12) Uani 1 1 d . . . O6 O 0.16535(16) 0.4405(5) 0.49710(15) 0.0447(11) Uani 1 1 d . . . F3 F 0.23976(11) 0.4930(3) 0.25175(11) 0.0347(8) Uani 1 1 d . . . F6 F 0.26211(12) 0.5249(3) 0.49318(13) 0.0441(9) Uani 1 1 d . . . F4 F 0.28144(12) 0.3120(4) 0.46636(13) 0.0462(9) Uani 1 1 d . . . F2 F 0.22019(13) 0.2815(4) 0.27893(13) 0.0461(10) Uani 1 1 d . . . F5 F 0.26326(14) 0.3238(4) 0.53411(12) 0.0528(10) Uani 1 1 d . . . F1 F 0.24043(13) 0.2906(4) 0.21248(12) 0.0480(10) Uani 1 1 d . . . N7 N 0.35237(13) 1.0254(4) 0.37324(12) 0.0137(8) Uani 1 1 d . . . N3 N 0.15024(14) 1.0360(4) 0.37505(13) 0.0158(8) Uani 1 1 d . . . N8 N 0.33282(13) 0.8534(4) 0.32395(12) 0.0140(8) Uani 1 1 d . . . N6 N 0.32753(13) 1.0437(5) 0.44625(12) 0.0161(8) Uani 1 1 d . . . N4 N 0.16985(13) 0.8761(5) 0.42750(13) 0.0156(9) Uani 1 1 d . . . N5 N 0.27457(13) 0.9353(5) 0.48131(13) 0.0167(8) Uani 1 1 d . . . N2 N 0.17351(14) 1.0159(4) 0.30136(12) 0.0141(8) Uani 1 1 d . . . N1 N 0.22693(13) 0.9035(4) 0.26819(13) 0.0137(8) 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 Pd1 0.01316(18) 0.01983(19) 0.01110(17) -0.00016(17) -0.00184(12) -0.00089(17) S2 0.0331(8) 0.0276(8) 0.0241(7) -0.0004(6) 0.0016(6) 0.0033(6) S3 0.0327(8) 0.0325(8) 0.0373(9) -0.0003(7) 0.0054(7) -0.0003(7) C4 0.017(2) 0.017(2) 0.009(2) -0.003(2) -0.0003(18) -0.005(2) C1 0.014(2) 0.019(2) 0.014(2) -0.004(2) 0.0021(18) -0.005(2) C2 0.017(2) 0.014(2) 0.014(2) 0.000(2) -0.0037(18) 0.001(2) C3 0.014(2) 0.011(2) 0.015(2) -0.0016(18) 0.0040(18) 0.0013(18) C5 0.013(2) 0.020(3) 0.013(2) 0.004(2) -0.0034(18) -0.001(2) C12 0.010(2) 0.028(3) 0.017(3) -0.002(2) -0.0018(19) -0.002(2) C8 0.015(2) 0.025(3) 0.011(2) 0.0011(19) -0.0007(19) -0.002(2) C7 0.020(3) 0.017(3) 0.005(2) -0.0011(18) -0.0012(18) 0.0034(19) C10 0.018(2) 0.024(3) 0.012(2) -0.005(2) -0.0058(18) -0.001(2) C11 0.018(3) 0.029(3) 0.016(3) 0.001(2) 0.003(2) -0.002(2) C9 0.021(3) 0.028(3) 0.013(2) 0.000(2) -0.005(2) 0.000(2) C6 0.014(2) 0.020(3) 0.016(2) 0.0035(19) -0.0008(19) -0.0045(19) C14 0.015(3) 0.031(3) 0.023(3) 0.003(2) 0.006(2) -0.001(2) C13 0.018(3) 0.026(3) 0.012(2) 0.002(2) 0.004(2) -0.002(2) C16 0.028(3) 0.022(3) 0.018(3) -0.006(2) -0.001(2) -0.011(2) C18 0.007(2) 0.030(3) 0.019(3) -0.002(2) 0.0015(19) 0.000(2) C17 0.013(3) 0.025(3) 0.012(3) 0.0033(19) -0.004(2) -0.0042(19) C15 0.021(3) 0.018(3) 0.014(2) 0.0042(19) 0.001(2) -0.003(2) C19 0.011(2) 0.022(3) 0.011(2) -0.010(2) -0.0015(17) 0.000(2) C23 0.014(3) 0.036(4) 0.035(3) -0.009(3) 0.000(2) -0.003(2) C22 0.019(3) 0.049(4) 0.024(3) -0.010(3) -0.012(2) 0.018(3) C20 0.019(3) 0.024(3) 0.019(3) -0.007(2) -0.006(2) 0.006(2) C21 0.041(4) 0.027(3) 0.020(3) -0.005(2) -0.012(3) 0.002(3) C24 0.018(3) 0.037(3) 0.028(3) -0.002(2) 0.002(2) -0.002(2) C26 0.029(3) 0.035(3) 0.025(3) 0.000(3) 0.011(2) 0.001(3) C30 0.025(3) 0.031(3) 0.014(3) -0.005(2) 0.000(2) -0.001(2) C25 0.014(2) 0.022(3) 0.019(3) 0.000(2) -0.001(2) 0.002(2) C27 0.034(3) 0.039(4) 0.024(3) 0.006(3) 0.007(2) 0.008(3) C28 0.038(3) 0.036(3) 0.019(3) -0.007(2) -0.004(2) 0.013(3) C29 0.016(3) 0.038(3) 0.028(3) -0.009(2) -0.004(2) 0.004(2) C32 0.024(3) 0.024(3) 0.019(3) 0.003(2) 0.005(2) 0.002(2) C33 0.012(3) 0.043(3) 0.025(3) -0.003(2) 0.001(2) 0.000(2) C31 0.023(3) 0.025(3) 0.013(2) -0.003(2) 0.008(2) 0.002(2) C36 0.020(3) 0.035(3) 0.022(3) 0.000(2) 0.005(2) 0.002(2) C34 0.014(3) 0.041(3) 0.023(3) 0.006(2) -0.004(2) 0.008(2) C35 0.023(3) 0.019(3) 0.027(3) 0.011(2) 0.005(2) 0.007(2) C42 0.022(3) 0.044(4) 0.027(3) 0.004(3) 0.000(2) -0.010(3) C37 0.010(2) 0.030(3) 0.021(3) 0.008(2) -0.001(2) 0.003(2) C38 0.024(3) 0.044(3) 0.017(3) 0.003(3) 0.007(2) 0.003(3) C41 0.022(3) 0.049(4) 0.038(4) 0.022(3) -0.009(3) -0.010(3) C40 0.017(3) 0.066(4) 0.016(3) 0.010(3) 0.004(2) -0.013(3) C39 0.023(3) 0.050(4) 0.024(3) 0.000(3) 0.011(2) -0.007(3) C43 0.022(3) 0.037(3) 0.014(2) -0.006(2) -0.002(2) -0.008(2) C48 0.027(3) 0.047(4) 0.025(3) 0.002(3) -0.007(2) -0.011(3) C45 0.044(4) 0.036(4) 0.026(3) -0.005(3) 0.011(3) -0.005(3) C44 0.030(3) 0.055(4) 0.013(3) -0.005(2) 0.003(2) -0.003(3) C46 0.045(4) 0.063(4) 0.017(3) 0.007(3) -0.002(3) -0.027(3) C47 0.032(3) 0.057(4) 0.030(3) 0.016(3) -0.009(3) -0.012(3) C54 0.022(3) 0.044(4) 0.023(3) 0.003(2) 0.003(2) 0.003(2) C53 0.017(3) 0.058(4) 0.030(3) 0.001(3) 0.000(2) -0.006(3) C49 0.025(3) 0.032(3) 0.013(3) 0.006(2) -0.001(2) -0.004(2) C52 0.027(3) 0.052(4) 0.031(3) 0.002(3) -0.006(3) -0.009(3) C51 0.041(4) 0.048(4) 0.025(3) -0.003(3) -0.003(3) 0.000(3) C50 0.029(3) 0.030(3) 0.023(3) -0.008(2) 0.002(2) -0.001(2) C61 0.013(2) 0.024(3) 0.015(3) 0.001(2) -0.003(2) -0.002(2) C55 0.017(3) 0.025(3) 0.016(2) 0.000(2) -0.0027(19) -0.009(2) C66 0.015(3) 0.037(3) 0.023(3) -0.006(2) -0.004(2) 0.005(2) C60 0.020(3) 0.032(3) 0.017(3) 0.001(2) -0.004(2) -0.011(2) C62 0.022(3) 0.039(3) 0.020(3) -0.006(2) 0.001(2) -0.004(2) C56 0.022(3) 0.027(3) 0.015(3) 0.001(2) -0.006(2) -0.004(2) C65 0.023(3) 0.042(4) 0.033(3) -0.009(3) 0.002(2) 0.011(3) C58 0.019(3) 0.042(4) 0.028(3) -0.004(3) 0.008(3) -0.006(2) C64 0.024(3) 0.035(4) 0.030(3) -0.018(3) 0.004(2) 0.003(3) C57 0.029(3) 0.031(3) 0.030(3) 0.003(3) 0.003(2) -0.009(3) C59 0.012(3) 0.049(4) 0.033(3) 0.007(3) -0.001(2) 0.000(3) C63 0.025(3) 0.038(3) 0.024(3) -0.012(3) 0.000(2) -0.002(3) C67 0.027(3) 0.018(3) 0.026(3) 0.004(2) 0.005(2) 0.000(2) C68 0.030(3) 0.025(3) 0.012(3) 0.002(2) 0.001(2) 0.007(2) O1 0.042(3) 0.031(2) 0.039(2) -0.0020(19) 0.0014(19) 0.0117(19) O3 0.027(2) 0.032(2) 0.046(3) -0.0014(18) 0.0084(18) -0.0100(17) O2 0.050(3) 0.056(3) 0.022(2) -0.002(2) -0.0089(19) 0.006(2) O4 0.049(3) 0.039(3) 0.059(3) 0.007(2) 0.013(2) -0.010(2) O5 0.060(3) 0.061(3) 0.034(3) 0.004(2) 0.002(2) -0.020(2) O6 0.054(3) 0.033(2) 0.051(3) 0.004(2) 0.020(2) 0.005(2) F3 0.0251(17) 0.0252(17) 0.050(2) 0.0038(15) -0.0064(15) 0.0021(13) F6 0.044(2) 0.0156(18) 0.067(3) -0.0034(16) -0.0145(18) 0.0004(14) F4 0.038(2) 0.040(2) 0.063(3) -0.0080(18) 0.0114(18) 0.0097(17) F2 0.043(2) 0.0297(19) 0.068(3) 0.0110(18) 0.019(2) -0.0115(16) F5 0.061(3) 0.055(3) 0.038(2) -0.0002(18) -0.0117(19) 0.017(2) F1 0.041(2) 0.059(2) 0.040(2) -0.0124(19) -0.0079(17) -0.0059(18) N7 0.015(2) 0.015(2) 0.0104(19) -0.0028(15) -0.0010(15) 0.0037(16) N3 0.018(2) 0.016(2) 0.014(2) 0.0013(17) 0.0044(16) 0.0030(17) N8 0.0070(19) 0.022(2) 0.012(2) 0.0004(16) -0.0027(15) 0.0011(16) N6 0.014(2) 0.025(2) 0.0093(19) -0.0029(17) 0.0030(15) -0.0027(18) N4 0.0095(19) 0.022(2) 0.015(2) 0.0034(17) -0.0004(16) -0.0006(17) N5 0.0123(19) 0.022(2) 0.015(2) -0.0006(18) -0.0018(15) -0.0041(17) N2 0.017(2) 0.014(2) 0.0109(19) -0.0004(15) -0.0006(16) 0.0014(16) N1 0.0096(19) 0.014(2) 0.017(2) 0.0022(16) -0.0006(16) 0.0004(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C4 1.988(4) . ? Pd1 C2 1.994(5) . ? Pd1 C1 2.035(4) . ? Pd1 C3 2.042(4) . ? S2 O3 1.434(4) . ? S2 O1 1.437(4) . ? S2 O2 1.438(4) . ? S2 C67 1.829(5) . ? S3 O4 1.427(4) . ? S3 O6 1.437(4) . ? S3 O5 1.442(4) . ? S3 C68 1.829(5) . ? C4 N8 1.338(6) . ? C4 N7 1.343(6) . ? C1 N2 1.351(6) . ? C1 N1 1.365(6) . ? C2 N4 1.328(6) . ? C2 N3 1.331(6) . ? C3 N5 1.338(6) . ? C3 N6 1.374(6) . ? C5 C6 1.348(7) . ? C5 N1 1.391(5) . ? C5 C25 1.472(6) . ? C12 C11 1.353(7) . ? C12 N8 1.395(6) . ? C12 C61 1.495(7) . ? C8 C7 1.360(6) . ? C8 N4 1.417(6) . ? C8 C37 1.454(7) . ? C7 N3 1.389(6) . ? C7 C31 1.475(7) . ? C10 C9 1.337(7) . ? C10 N6 1.392(5) . ? C10 C49 1.472(7) . ? C11 N7 1.379(6) . ? C11 C55 1.497(7) . ? C9 N5 1.401(6) . ? C9 C43 1.493(7) . ? C6 N2 1.400(6) . ? C6 C19 1.483(6) . ? C14 N4 1.468(6) . ? C14 C15 1.505(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13 N3 1.448(6) . ? C13 N2 1.479(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C16 N6 1.453(6) . ? C16 N7 1.460(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 N1 1.475(6) . ? C18 C17 1.518(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C17 N8 1.477(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C15 N5 1.473(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C19 C20 1.367(7) . ? C19 C24 1.404(7) . ? C23 C22 1.379(8) . ? C23 C24 1.404(7) . ? C23 H23 0.9500 . ? C22 C21 1.374(8) . ? C22 H22 0.9500 . ? C20 C21 1.384(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C24 H24 0.9500 . ? C26 C27 1.379(7) . ? C26 C25 1.388(7) . ? C26 H26 0.9500 . ? C30 C29 1.382(7) . ? C30 C25 1.407(7) . ? C30 H30 0.9500 . ? C27 C28 1.383(8) . ? C27 H27 0.9500 . ? C28 C29 1.384(8) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C32 C31 1.379(7) . ? C32 C33 1.391(7) . ? C32 H32 0.9500 . ? C33 C34 1.377(8) . ? C33 H33 0.9500 . ? C31 C36 1.392(7) . ? C36 C35 1.386(7) . ? C36 H36 0.9500 . ? C34 C35 1.396(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C42 C41 1.407(8) . ? C42 C37 1.429(8) . ? C42 H42 0.9500 . ? C37 C38 1.383(7) . ? C38 C39 1.392(7) . ? C38 H38 0.9500 . ? C41 C40 1.375(9) . ? C41 H41 0.9500 . ? C40 C39 1.366(8) . ? C40 H40 0.9500 . ? C39 H39 0.9500 . ? C43 C48 1.366(8) . ? C43 C44 1.384(7) . ? C48 C47 1.380(8) . ? C48 H48 0.9500 . ? C45 C44 1.367(7) . ? C45 C46 1.389(9) . ? C45 H45 0.9500 . ? C44 H44 0.9500 . ? C46 C47 1.347(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C54 C49 1.402(7) . ? C54 C53 1.408(8) . ? C54 H54 0.9500 . ? C53 C52 1.360(8) . ? C53 H53 0.9500 . ? C49 C50 1.411(7) . ? C52 C51 1.391(8) . ? C52 H52 0.9500 . ? C51 C50 1.394(8) . ? C51 H51 0.9500 . ? C50 H50 0.9500 . ? C61 C66 1.368(7) . ? C61 C62 1.409(7) . ? C55 C56 1.376(7) . ? C55 C60 1.408(7) . ? C66 C65 1.396(7) . ? C66 H66 0.9500 . ? C60 C59 1.400(7) . ? C60 H60 0.9500 . ? C62 C63 1.390(7) . ? C62 H62 0.9500 . ? C56 C57 1.396(7) . ? C56 H56 0.9500 . ? C65 C64 1.384(8) . ? C65 H65 0.9500 . ? C58 C59 1.381(8) . ? C58 C57 1.390(8) . ? C58 H58 0.9500 . ? C64 C63 1.340(8) . ? C64 H64 0.9500 . ? C57 H57 0.9500 . ? C59 H59 0.9500 . ? C63 H63 0.9500 . ? C67 F1 1.311(6) . ? C67 F3 1.329(6) . ? C67 F2 1.331(6) . ? C68 F5 1.318(6) . ? C68 F6 1.328(6) . ? C68 F4 1.341(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Pd1 C2 179.6(2) . . ? C4 Pd1 C1 92.91(17) . . ? C2 Pd1 C1 87.45(18) . . ? C4 Pd1 C3 87.45(17) . . ? C2 Pd1 C3 92.22(17) . . ? C1 Pd1 C3 172.50(18) . . ? O3 S2 O1 115.0(2) . . ? O3 S2 O2 114.9(3) . . ? O1 S2 O2 115.1(3) . . ? O3 S2 C67 102.9(2) . . ? O1 S2 C67 103.6(2) . . ? O2 S2 C67 103.0(3) . . ? O4 S3 O6 115.9(3) . . ? O4 S3 O5 115.2(3) . . ? O6 S3 O5 115.0(3) . . ? O4 S3 C68 103.3(3) . . ? O6 S3 C68 101.5(3) . . ? O5 S3 C68 103.0(3) . . ? N8 C4 N7 105.2(4) . . ? N8 C4 Pd1 131.0(3) . . ? N7 C4 Pd1 123.8(3) . . ? N2 C1 N1 104.9(4) . . ? N2 C1 Pd1 118.9(3) . . ? N1 C1 Pd1 136.1(3) . . ? N4 C2 N3 105.6(4) . . ? N4 C2 Pd1 129.6(3) . . ? N3 C2 Pd1 124.7(3) . . ? N5 C3 N6 105.6(4) . . ? N5 C3 Pd1 136.4(3) . . ? N6 C3 Pd1 117.9(3) . . ? C6 C5 N1 107.2(4) . . ? C6 C5 C25 128.2(4) . . ? N1 C5 C25 124.6(4) . . ? C11 C12 N8 105.5(4) . . ? C11 C12 C61 130.8(4) . . ? N8 C12 C61 123.6(4) . . ? C7 C8 N4 105.4(4) . . ? C7 C8 C37 131.2(4) . . ? N4 C8 C37 123.4(4) . . ? C8 C7 N3 105.9(4) . . ? C8 C7 C31 131.3(4) . . ? N3 C7 C31 122.6(4) . . ? C9 C10 N6 106.9(4) . . ? C9 C10 C49 131.5(4) . . ? N6 C10 C49 121.5(4) . . ? C12 C11 N7 107.0(4) . . ? C12 C11 C55 130.7(5) . . ? N7 C11 C55 122.4(4) . . ? C10 C9 N5 107.4(4) . . ? C10 C9 C43 129.5(4) . . ? N5 C9 C43 123.1(4) . . ? C5 C6 N2 106.4(4) . . ? C5 C6 C19 132.1(4) . . ? N2 C6 C19 121.5(4) . . ? N4 C14 C15 112.5(4) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N3 C13 N2 108.5(4) . . ? N3 C13 H13A 110.0 . . ? N2 C13 H13A 110.0 . . ? N3 C13 H13B 110.0 . . ? N2 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? N6 C16 N7 109.1(4) . . ? N6 C16 H16A 109.9 . . ? N7 C16 H16A 109.9 . . ? N6 C16 H16B 109.9 . . ? N7 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N1 C18 C17 116.5(4) . . ? N1 C18 H18A 108.2 . . ? C17 C18 H18A 108.2 . . ? N1 C18 H18B 108.2 . . ? C17 C18 H18B 108.2 . . ? H18A C18 H18B 107.3 . . ? N8 C17 C18 111.3(4) . . ? N8 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? N8 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N5 C15 C14 117.3(4) . . ? N5 C15 H15A 108.0 . . ? C14 C15 H15A 108.0 . . ? N5 C15 H15B 108.0 . . ? C14 C15 H15B 108.0 . . ? H15A C15 H15B 107.2 . . ? C20 C19 C24 119.6(4) . . ? C20 C19 C6 121.0(4) . . ? C24 C19 C6 119.4(4) . . ? C22 C23 C24 118.9(5) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C21 C22 C23 120.9(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C19 C20 C21 120.5(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C24 C19 119.9(5) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C27 C26 C25 121.0(5) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C29 C30 C25 120.8(5) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C26 C25 C30 118.4(5) . . ? C26 C25 C5 122.1(4) . . ? C30 C25 C5 119.5(4) . . ? C26 C27 C28 119.6(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 121.0(5) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 119.2(5) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C32 C33 120.3(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 119.7(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C32 C31 C36 119.3(5) . . ? C32 C31 C7 121.3(5) . . ? C36 C31 C7 119.3(5) . . ? C35 C36 C31 121.3(5) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 118.2(5) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C41 C42 C37 118.7(6) . . ? C41 C42 H42 120.7 . . ? C37 C42 H42 120.7 . . ? C38 C37 C42 119.7(5) . . ? C38 C37 C8 120.3(5) . . ? C42 C37 C8 120.0(5) . . ? C37 C38 C39 120.2(6) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C41 C42 119.5(6) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C39 C40 C41 121.9(5) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C40 C39 C38 120.0(6) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C48 C43 C44 117.7(5) . . ? C48 C43 C9 118.9(5) . . ? C44 C43 C9 123.4(5) . . ? C43 C48 C47 121.6(6) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C44 C45 C46 119.2(6) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C45 C44 C43 121.4(6) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C47 C46 C45 120.2(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.8(6) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C49 C54 C53 119.1(5) . . ? C49 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C52 C53 C54 121.4(6) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C54 C49 C50 118.8(5) . . ? C54 C49 C10 121.3(5) . . ? C50 C49 C10 119.7(5) . . ? C53 C52 C51 120.4(6) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C51 C50 119.6(6) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C50 C49 120.6(5) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C66 C61 C62 121.8(5) . . ? C66 C61 C12 120.4(4) . . ? C62 C61 C12 117.7(5) . . ? C56 C55 C60 121.1(5) . . ? C56 C55 C11 120.2(5) . . ? C60 C55 C11 118.6(5) . . ? C61 C66 C65 118.8(5) . . ? C61 C66 H66 120.6 . . ? C65 C66 H66 120.6 . . ? C59 C60 C55 119.2(5) . . ? C59 C60 H60 120.4 . . ? C55 C60 H60 120.4 . . ? C63 C62 C61 116.2(5) . . ? C63 C62 H62 121.9 . . ? C61 C62 H62 121.9 . . ? C55 C56 C57 118.3(5) . . ? C55 C56 H56 120.9 . . ? C57 C56 H56 120.9 . . ? C64 C65 C66 120.3(6) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C59 C58 C57 119.3(5) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C63 C64 C65 119.4(5) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C58 C57 C56 121.9(5) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C58 C59 C60 120.2(5) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C64 C63 C62 123.4(6) . . ? C64 C63 H63 118.3 . . ? C62 C63 H63 118.3 . . ? F1 C67 F3 107.9(4) . . ? F1 C67 F2 107.4(4) . . ? F3 C67 F2 106.8(4) . . ? F1 C67 S2 111.7(4) . . ? F3 C67 S2 111.9(4) . . ? F2 C67 S2 111.0(4) . . ? F5 C68 F6 108.5(4) . . ? F5 C68 F4 107.6(4) . . ? F6 C68 F4 106.6(4) . . ? F5 C68 S3 111.5(4) . . ? F6 C68 S3 112.0(3) . . ? F4 C68 S3 110.4(4) . . ? C4 N7 C11 111.0(4) . . ? C4 N7 C16 119.2(4) . . ? C11 N7 C16 129.8(4) . . ? C2 N3 C7 112.1(4) . . ? C2 N3 C13 119.9(4) . . ? C7 N3 C13 127.6(4) . . ? C4 N8 C12 111.3(4) . . ? C4 N8 C17 120.4(4) . . ? C12 N8 C17 128.1(4) . . ? C3 N6 C10 109.8(4) . . ? C3 N6 C16 122.8(4) . . ? C10 N6 C16 125.8(4) . . ? C2 N4 C8 110.9(4) . . ? C2 N4 C14 120.8(4) . . ? C8 N4 C14 128.1(4) . . ? C3 N5 C9 110.2(4) . . ? C3 N5 C15 128.6(4) . . ? C9 N5 C15 121.2(4) . . ? C1 N2 C6 111.0(4) . . ? C1 N2 C13 122.5(4) . . ? C6 N2 C13 124.2(4) . . ? C1 N1 C5 110.5(4) . . ? C1 N1 C18 128.1(4) . . ? C5 N1 C18 121.3(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 C2 Pd1 C4 N8 107(33) . . . . ? C1 Pd1 C4 N8 -48.3(5) . . . . ? C3 Pd1 C4 N8 139.2(5) . . . . ? C2 Pd1 C4 N7 -71(33) . . . . ? C1 Pd1 C4 N7 133.6(4) . . . . ? C3 Pd1 C4 N7 -38.9(4) . . . . ? C4 Pd1 C1 N2 -155.5(4) . . . . ? C2 Pd1 C1 N2 24.7(4) . . . . ? C3 Pd1 C1 N2 -63.0(15) . . . . ? C4 Pd1 C1 N1 28.7(5) . . . . ? C2 Pd1 C1 N1 -151.1(5) . . . . ? C3 Pd1 C1 N1 121.3(13) . . . . ? C4 Pd1 C2 N4 -17(33) . . . . ? C1 Pd1 C2 N4 138.4(4) . . . . ? C3 Pd1 C2 N4 -49.1(4) . . . . ? C4 Pd1 C2 N3 166(100) . . . . ? C1 Pd1 C2 N3 -38.6(4) . . . . ? C3 Pd1 C2 N3 133.9(4) . . . . ? C4 Pd1 C3 N5 -152.6(5) . . . . ? C2 Pd1 C3 N5 27.2(5) . . . . ? C1 Pd1 C3 N5 114.5(14) . . . . ? C4 Pd1 C3 N6 31.6(4) . . . . ? C2 Pd1 C3 N6 -148.7(4) . . . . ? C1 Pd1 C3 N6 -61.3(15) . . . . ? N4 C8 C7 N3 -0.9(5) . . . . ? C37 C8 C7 N3 -179.6(5) . . . . ? N4 C8 C7 C31 -175.7(5) . . . . ? C37 C8 C7 C31 5.6(9) . . . . ? N8 C12 C11 N7 0.5(5) . . . . ? C61 C12 C11 N7 179.4(5) . . . . ? N8 C12 C11 C55 -178.5(5) . . . . ? C61 C12 C11 C55 0.4(10) . . . . ? N6 C10 C9 N5 -0.9(6) . . . . ? C49 C10 C9 N5 176.8(5) . . . . ? N6 C10 C9 C43 176.9(5) . . . . ? C49 C10 C9 C43 -5.5(10) . . . . ? N1 C5 C6 N2 -0.4(5) . . . . ? C25 C5 C6 N2 179.5(5) . . . . ? N1 C5 C6 C19 179.3(5) . . . . ? C25 C5 C6 C19 -0.8(9) . . . . ? N1 C18 C17 N8 -83.1(5) . . . . ? N4 C14 C15 N5 -77.6(5) . . . . ? C5 C6 C19 C20 -52.6(8) . . . . ? N2 C6 C19 C20 127.1(5) . . . . ? C5 C6 C19 C24 125.6(6) . . . . ? N2 C6 C19 C24 -54.7(6) . . . . ? C24 C23 C22 C21 -2.3(8) . . . . ? C24 C19 C20 C21 2.1(7) . . . . ? C6 C19 C20 C21 -179.6(5) . . . . ? C23 C22 C21 C20 0.8(8) . . . . ? C19 C20 C21 C22 -0.7(8) . . . . ? C22 C23 C24 C19 3.8(8) . . . . ? C20 C19 C24 C23 -3.7(7) . . . . ? C6 C19 C24 C23 178.0(5) . . . . ? C27 C26 C25 C30 0.7(8) . . . . ? C27 C26 C25 C5 -176.7(5) . . . . ? C29 C30 C25 C26 -2.3(8) . . . . ? C29 C30 C25 C5 175.1(5) . . . . ? C6 C5 C25 C26 116.8(6) . . . . ? N1 C5 C25 C26 -63.3(7) . . . . ? C6 C5 C25 C30 -60.6(7) . . . . ? N1 C5 C25 C30 119.3(5) . . . . ? C25 C26 C27 C28 0.9(8) . . . . ? C26 C27 C28 C29 -0.9(8) . . . . ? C25 C30 C29 C28 2.3(8) . . . . ? C27 C28 C29 C30 -0.7(8) . . . . ? C31 C32 C33 C34 -2.0(8) . . . . ? C33 C32 C31 C36 3.3(7) . . . . ? C33 C32 C31 C7 -176.5(4) . . . . ? C8 C7 C31 C32 -54.4(7) . . . . ? N3 C7 C31 C32 131.5(5) . . . . ? C8 C7 C31 C36 125.8(6) . . . . ? N3 C7 C31 C36 -48.2(6) . . . . ? C32 C31 C36 C35 -2.9(8) . . . . ? C7 C31 C36 C35 176.8(5) . . . . ? C32 C33 C34 C35 0.3(8) . . . . ? C31 C36 C35 C34 1.2(8) . . . . ? C33 C34 C35 C36 0.1(8) . . . . ? C41 C42 C37 C38 1.3(7) . . . . ? C41 C42 C37 C8 -178.7(5) . . . . ? C7 C8 C37 C38 -62.0(7) . . . . ? N4 C8 C37 C38 119.5(5) . . . . ? C7 C8 C37 C42 117.9(6) . . . . ? N4 C8 C37 C42 -60.5(6) . . . . ? C42 C37 C38 C39 -1.5(7) . . . . ? C8 C37 C38 C39 178.4(5) . . . . ? C37 C42 C41 C40 -1.0(8) . . . . ? C42 C41 C40 C39 1.0(8) . . . . ? C41 C40 C39 C38 -1.2(9) . . . . ? C37 C38 C39 C40 1.5(8) . . . . ? C10 C9 C43 C48 -55.9(8) . . . . ? N5 C9 C43 C48 121.5(6) . . . . ? C10 C9 C43 C44 124.2(7) . . . . ? N5 C9 C43 C44 -58.4(8) . . . . ? C44 C43 C48 C47 0.7(9) . . . . ? C9 C43 C48 C47 -179.2(5) . . . . ? C46 C45 C44 C43 -2.0(9) . . . . ? C48 C43 C44 C45 0.5(9) . . . . ? C9 C43 C44 C45 -179.6(5) . . . . ? C44 C45 C46 C47 2.4(9) . . . . ? C45 C46 C47 C48 -1.2(9) . . . . ? C43 C48 C47 C46 -0.4(9) . . . . ? C49 C54 C53 C52 1.8(9) . . . . ? C53 C54 C49 C50 -1.3(8) . . . . ? C53 C54 C49 C10 175.1(5) . . . . ? C9 C10 C49 C54 132.3(6) . . . . ? N6 C10 C49 C54 -50.3(7) . . . . ? C9 C10 C49 C50 -51.3(8) . . . . ? N6 C10 C49 C50 126.1(5) . . . . ? C54 C53 C52 C51 -0.5(9) . . . . ? C53 C52 C51 C50 -1.2(9) . . . . ? C52 C51 C50 C49 1.7(9) . . . . ? C54 C49 C50 C51 -0.4(8) . . . . ? C10 C49 C50 C51 -176.9(5) . . . . ? C11 C12 C61 C66 122.9(6) . . . . ? N8 C12 C61 C66 -58.4(6) . . . . ? C11 C12 C61 C62 -58.5(7) . . . . ? N8 C12 C61 C62 120.2(5) . . . . ? C12 C11 C55 C56 125.4(6) . . . . ? N7 C11 C55 C56 -53.4(7) . . . . ? C12 C11 C55 C60 -57.0(8) . . . . ? N7 C11 C55 C60 124.1(5) . . . . ? C62 C61 C66 C65 0.0(7) . . . . ? C12 C61 C66 C65 178.5(5) . . . . ? C56 C55 C60 C59 0.4(8) . . . . ? C11 C55 C60 C59 -177.1(5) . . . . ? C66 C61 C62 C63 -3.4(7) . . . . ? C12 C61 C62 C63 177.9(4) . . . . ? C60 C55 C56 C57 -0.2(8) . . . . ? C11 C55 C56 C57 177.3(5) . . . . ? C61 C66 C65 C64 2.7(8) . . . . ? C66 C65 C64 C63 -1.6(8) . . . . ? C59 C58 C57 C56 0.8(9) . . . . ? C55 C56 C57 C58 -0.4(8) . . . . ? C57 C58 C59 C60 -0.6(8) . . . . ? C55 C60 C59 C58 0.0(8) . . . . ? C65 C64 C63 C62 -2.2(8) . . . . ? C61 C62 C63 C64 4.7(8) . . . . ? O3 S2 C67 F1 70.9(4) . . . . ? O1 S2 C67 F1 -49.2(4) . . . . ? O2 S2 C67 F1 -169.4(4) . . . . ? O3 S2 C67 F3 -50.2(4) . . . . ? O1 S2 C67 F3 -170.3(4) . . . . ? O2 S2 C67 F3 69.5(4) . . . . ? O3 S2 C67 F2 -169.3(4) . . . . ? O1 S2 C67 F2 70.6(4) . . . . ? O2 S2 C67 F2 -49.6(4) . . . . ? O4 S3 C68 F5 -49.6(4) . . . . ? O6 S3 C68 F5 70.9(4) . . . . ? O5 S3 C68 F5 -169.8(4) . . . . ? O4 S3 C68 F6 -171.4(4) . . . . ? O6 S3 C68 F6 -51.0(4) . . . . ? O5 S3 C68 F6 68.3(4) . . . . ? O4 S3 C68 F4 70.0(4) . . . . ? O6 S3 C68 F4 -169.6(4) . . . . ? O5 S3 C68 F4 -50.3(4) . . . . ? N8 C4 N7 C11 1.8(5) . . . . ? Pd1 C4 N7 C11 -179.6(3) . . . . ? N8 C4 N7 C16 -176.9(4) . . . . ? Pd1 C4 N7 C16 1.6(6) . . . . ? C12 C11 N7 C4 -1.5(6) . . . . ? C55 C11 N7 C4 177.6(4) . . . . ? C12 C11 N7 C16 177.1(5) . . . . ? C55 C11 N7 C16 -3.8(8) . . . . ? N6 C16 N7 C4 53.4(6) . . . . ? N6 C16 N7 C11 -125.1(5) . . . . ? N4 C2 N3 C7 1.1(5) . . . . ? Pd1 C2 N3 C7 178.7(3) . . . . ? N4 C2 N3 C13 -172.0(4) . . . . ? Pd1 C2 N3 C13 5.6(6) . . . . ? C8 C7 N3 C2 -0.1(5) . . . . ? C31 C7 N3 C2 175.3(4) . . . . ? C8 C7 N3 C13 172.4(4) . . . . ? C31 C7 N3 C13 -12.2(7) . . . . ? N2 C13 N3 C2 49.0(6) . . . . ? N2 C13 N3 C7 -122.9(5) . . . . ? N7 C4 N8 C12 -1.5(5) . . . . ? Pd1 C4 N8 C12 -179.9(4) . . . . ? N7 C4 N8 C17 -177.1(4) . . . . ? Pd1 C4 N8 C17 4.5(7) . . . . ? C11 C12 N8 C4 0.6(5) . . . . ? C61 C12 N8 C4 -178.4(4) . . . . ? C11 C12 N8 C17 175.8(4) . . . . ? C61 C12 N8 C17 -3.2(7) . . . . ? C18 C17 N8 C4 78.1(5) . . . . ? C18 C17 N8 C12 -96.7(5) . . . . ? N5 C3 N6 C10 0.4(5) . . . . ? Pd1 C3 N6 C10 177.5(3) . . . . ? N5 C3 N6 C16 -166.2(4) . . . . ? Pd1 C3 N6 C16 10.8(6) . . . . ? C9 C10 N6 C3 0.3(6) . . . . ? C49 C10 N6 C3 -177.6(4) . . . . ? C9 C10 N6 C16 166.5(5) . . . . ? C49 C10 N6 C16 -11.5(8) . . . . ? N7 C16 N6 C3 -61.1(6) . . . . ? N7 C16 N6 C10 134.5(5) . . . . ? N3 C2 N4 C8 -1.7(5) . . . . ? Pd1 C2 N4 C8 -179.2(3) . . . . ? N3 C2 N4 C14 -178.6(4) . . . . ? Pd1 C2 N4 C14 3.9(7) . . . . ? C7 C8 N4 C2 1.7(5) . . . . ? C37 C8 N4 C2 -179.5(4) . . . . ? C7 C8 N4 C14 178.3(5) . . . . ? C37 C8 N4 C14 -2.9(8) . . . . ? C15 C14 N4 C2 79.3(6) . . . . ? C15 C14 N4 C8 -97.1(6) . . . . ? N6 C3 N5 C9 -1.0(5) . . . . ? Pd1 C3 N5 C9 -177.2(4) . . . . ? N6 C3 N5 C15 178.8(4) . . . . ? Pd1 C3 N5 C15 2.5(8) . . . . ? C10 C9 N5 C3 1.2(6) . . . . ? C43 C9 N5 C3 -176.7(5) . . . . ? C10 C9 N5 C15 -178.6(4) . . . . ? C43 C9 N5 C15 3.5(7) . . . . ? C14 C15 N5 C3 15.2(7) . . . . ? C14 C15 N5 C9 -165.1(4) . . . . ? N1 C1 N2 C6 -0.1(5) . . . . ? Pd1 C1 N2 C6 -177.0(3) . . . . ? N1 C1 N2 C13 -163.4(4) . . . . ? Pd1 C1 N2 C13 19.7(6) . . . . ? C5 C6 N2 C1 0.3(5) . . . . ? C19 C6 N2 C1 -179.4(4) . . . . ? C5 C6 N2 C13 163.3(4) . . . . ? C19 C6 N2 C13 -16.5(7) . . . . ? N3 C13 N2 C1 -64.6(5) . . . . ? N3 C13 N2 C6 134.4(4) . . . . ? N2 C1 N1 C5 -0.2(5) . . . . ? Pd1 C1 N1 C5 175.9(4) . . . . ? N2 C1 N1 C18 177.4(4) . . . . ? Pd1 C1 N1 C18 -6.5(8) . . . . ? C6 C5 N1 C1 0.4(5) . . . . ? C25 C5 N1 C1 -179.5(4) . . . . ? C6 C5 N1 C18 -177.4(4) . . . . ? C25 C5 N1 C18 2.7(7) . . . . ? C17 C18 N1 C1 26.4(7) . . . . ? C17 C18 N1 C5 -156.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.194 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.118 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.253 0.444 0.378 468.7 191.2 2 0.253 0.056 0.878 468.6 191.5 3 0.747 0.556 0.622 468.5 198.7 4 0.747 0.944 1.122 468.6 197.4 _platon_squeeze_details ; ? ; data_6 _database_code_depnum_ccdc_archive 'CCDC 888977' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 F6 N8 Ni O6 S2' _chemical_formula_weight 1314.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' 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 17.1544(5) _cell_length_b 28.6906(9) _cell_length_c 29.7309(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.5920(10) _cell_angle_gamma 90.00 _cell_volume 14160.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5424 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Apex II CCD Detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 182037 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 26.37 _reflns_number_total 28851 _reflns_number_gt 17652 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains disordered solvent molecules CH2Cl2, which were SQUEEZED out with the SQUEEZE routine in Platon software package. ; _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^)+(0.0926P)^2^+4.2379P] 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 28851 _refine_ls_number_parameters 1639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.140 _refine_ls_shift/su_mean 0.006 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 Ni1 Ni 0.07741(3) 0.490250(17) 0.260690(15) 0.02677(13) Uani 1 1 d . . . S2 S 0.18411(6) 0.34799(3) 0.24507(3) 0.0315(2) Uani 1 1 d . . . O5 O 0.18022(17) 0.35477(9) 0.19654(9) 0.0346(7) Uani 1 1 d . . . O6 O 0.12610(18) 0.37477(10) 0.26150(10) 0.0442(8) Uani 1 1 d . . . O4 O 0.19479(19) 0.30064(10) 0.26082(10) 0.0437(8) Uani 1 1 d . . . C3 C 0.1442(2) 0.49315(13) 0.21984(12) 0.0264(9) Uani 1 1 d . . . C2 C 0.1669(2) 0.48288(12) 0.31329(12) 0.0239(8) Uani 1 1 d . . . C4 C -0.0128(3) 0.48844(13) 0.20696(13) 0.0306(9) Uani 1 1 d . . . C1 C 0.0127(2) 0.49354(13) 0.30294(12) 0.0263(9) Uani 1 1 d . . . C8 C 0.2860(2) 0.48037(13) 0.36910(12) 0.0243(8) Uani 1 1 d . . . C10 C 0.2338(2) 0.51813(13) 0.18052(13) 0.0284(9) Uani 1 1 d . . . C6 C -0.0291(2) 0.48342(13) 0.36875(13) 0.0268(9) Uani 1 1 d . . . C9 C 0.1885(2) 0.48391(12) 0.15479(12) 0.0252(8) Uani 1 1 d . . . C7 C 0.2335(2) 0.45334(13) 0.38413(12) 0.0240(8) Uani 1 1 d . . . C5 C -0.0735(2) 0.51820(13) 0.34386(13) 0.0293(9) Uani 1 1 d . . . C11 C -0.1298(2) 0.49261(13) 0.15068(12) 0.0278(9) Uani 1 1 d . . . C12 C -0.0780(2) 0.46806(13) 0.13286(12) 0.0260(8) Uani 1 1 d . . . C14 C 0.2875(3) 0.52995(14) 0.30141(13) 0.0334(10) Uani 1 1 d . . . H14A H 0.3288 0.5125 0.2916 0.040 Uiso 1 1 calc R . . H14B H 0.3144 0.5536 0.3232 0.040 Uiso 1 1 calc R . . C13 C 0.0864(2) 0.43313(13) 0.35201(13) 0.0247(8) Uani 1 1 d . . . H13A H 0.0912 0.4200 0.3827 0.030 Uiso 1 1 calc R . . H13B H 0.0731 0.4082 0.3293 0.030 Uiso 1 1 calc R . . C18 C -0.0758(3) 0.55680(13) 0.26616(13) 0.0345(10) Uani 1 1 d . . . H18A H -0.0305 0.5710 0.2574 0.041 Uiso 1 1 calc R . . H18B H -0.1052 0.5813 0.2772 0.041 Uiso 1 1 calc R . . C16 C 0.0639(2) 0.43908(13) 0.16552(13) 0.0250(8) Uani 1 1 d . . . H16A H 0.0588 0.4279 0.1341 0.030 Uiso 1 1 calc R . . H16B H 0.0693 0.4123 0.1860 0.030 Uiso 1 1 calc R . . C15 C 0.2353(3) 0.55407(13) 0.25951(12) 0.0334(10) Uani 1 1 d . . . H15A H 0.1900 0.5685 0.2682 0.040 Uiso 1 1 calc R . . H15B H 0.2662 0.5786 0.2497 0.040 Uiso 1 1 calc R . . C17 C -0.1302(3) 0.53409(15) 0.22411(13) 0.0365(10) Uani 1 1 d . . . H17A H -0.1693 0.5151 0.2343 0.044 Uiso 1 1 calc R . . H17B H -0.1597 0.5584 0.2042 0.044 Uiso 1 1 calc R . . C19 C -0.1366(3) 0.54832(14) 0.35434(13) 0.0327(10) Uani 1 1 d . . . C24 C -0.1144(3) 0.58726(13) 0.38259(13) 0.0314(9) Uani 1 1 d . . . H24 H -0.0604 0.5942 0.3951 0.038 Uiso 1 1 calc R . . C21 C -0.2768(3) 0.5675(2) 0.34589(17) 0.0611(15) Uani 1 1 d . . . H21 H -0.3311 0.5608 0.3339 0.073 Uiso 1 1 calc R . . C23 C -0.1741(3) 0.61547(15) 0.39177(15) 0.0445(12) Uani 1 1 d . . . H23 H -0.1595 0.6413 0.4109 0.053 Uiso 1 1 calc R . . C20 C -0.2177(3) 0.53810(18) 0.33595(16) 0.0515(13) Uani 1 1 d . . . H20 H -0.2327 0.5120 0.3172 0.062 Uiso 1 1 calc R . . C22 C -0.2541(3) 0.60626(19) 0.37340(15) 0.0522(14) Uani 1 1 d . . . H22 H -0.2930 0.6261 0.3795 0.063 Uiso 1 1 calc R . . C25 C -0.0316(2) 0.46445(13) 0.41437(13) 0.0266(9) Uani 1 1 d . . . C30 C 0.0378(2) 0.45916(13) 0.44983(13) 0.0277(9) Uani 1 1 d . . . H30 H 0.0876 0.4667 0.4447 0.033 Uiso 1 1 calc R . . C27 C -0.1093(3) 0.43902(15) 0.46671(15) 0.0378(10) Uani 1 1 d . . . H27 H -0.1590 0.4328 0.4726 0.045 Uiso 1 1 calc R . . C28 C -0.0401(3) 0.43292(14) 0.50179(15) 0.0388(11) Uani 1 1 d . . . H28 H -0.0430 0.4224 0.5309 0.047 Uiso 1 1 calc R . . C29 C 0.0331(3) 0.44254(13) 0.49316(13) 0.0317(9) Uani 1 1 d . . . H29 H 0.0801 0.4379 0.5164 0.038 Uiso 1 1 calc R . . C26 C -0.1064(2) 0.45421(13) 0.42288(14) 0.0328(10) Uani 1 1 d . . . H26 H -0.1535 0.4575 0.3994 0.039 Uiso 1 1 calc R . . C31 C 0.2448(2) 0.42605(13) 0.42724(12) 0.0217(8) Uani 1 1 d . . . C36 C 0.2433(2) 0.37762(13) 0.42610(13) 0.0250(8) Uani 1 1 d . . . H36 H 0.2313 0.3622 0.3977 0.030 Uiso 1 1 calc R . . C35 C 0.2597(2) 0.35218(14) 0.46708(13) 0.0305(9) Uani 1 1 d . . . H35 H 0.2606 0.3198 0.4661 0.037 Uiso 1 1 calc R . . C32 C 0.2602(3) 0.44828(15) 0.46995(13) 0.0364(10) Uani 1 1 d . . . H32 H 0.2615 0.4807 0.4712 0.044 Uiso 1 1 calc R . . C34 C 0.2746(2) 0.37489(15) 0.50937(14) 0.0350(10) Uani 1 1 d . . . H34 H 0.2852 0.3578 0.5368 0.042 Uiso 1 1 calc R . . C33 C 0.2738(3) 0.42293(16) 0.51066(14) 0.0422(11) Uani 1 1 d . . . H33 H 0.2825 0.4383 0.5390 0.051 Uiso 1 1 calc R . . C37 C 0.3714(2) 0.49078(13) 0.39167(12) 0.0247(8) Uani 1 1 d . . . C38 C 0.4318(3) 0.46570(17) 0.38204(18) 0.0520(13) Uani 1 1 d . . . H38 H 0.4199 0.4421 0.3599 0.062 Uiso 1 1 calc R . . C42 C 0.3899(3) 0.52508(17) 0.42467(16) 0.0496(13) Uani 1 1 d . . . H42 H 0.3492 0.5425 0.4322 0.060 Uiso 1 1 calc R . . C40 C 0.5298(3) 0.50852(18) 0.43691(16) 0.0464(12) Uani 1 1 d . . . H40 H 0.5831 0.5146 0.4521 0.056 Uiso 1 1 calc R . . C39 C 0.5117(3) 0.47487(19) 0.4050(2) 0.0583(14) Uani 1 1 d . . . H39 H 0.5528 0.4574 0.3980 0.070 Uiso 1 1 calc R . . C41 C 0.4698(3) 0.5335(2) 0.44678(18) 0.0662(16) Uani 1 1 d . . . H41 H 0.4823 0.5570 0.4690 0.079 Uiso 1 1 calc R . . C45 C 0.1888(2) 0.39959(13) 0.05825(13) 0.0311(9) Uani 1 1 d . . . H45 H 0.1868 0.3676 0.0533 0.037 Uiso 1 1 calc R . . C47 C 0.1944(2) 0.47645(14) 0.02978(13) 0.0302(9) Uani 1 1 d . . . H47 H 0.1968 0.4966 0.0057 0.036 Uiso 1 1 calc R . . C44 C 0.1884(2) 0.41666(13) 0.10147(13) 0.0272(9) Uani 1 1 d . . . H44 H 0.1869 0.3963 0.1256 0.033 Uiso 1 1 calc R . . C48 C 0.1933(2) 0.49429(13) 0.07262(12) 0.0267(9) Uani 1 1 d . . . H48 H 0.1945 0.5264 0.0773 0.032 Uiso 1 1 calc R . . C46 C 0.1919(2) 0.42900(14) 0.02227(13) 0.0305(9) Uani 1 1 d . . . H46 H 0.1925 0.4171 -0.0067 0.037 Uiso 1 1 calc R . . C43 C 0.1903(2) 0.46437(13) 0.10883(12) 0.0251(8) Uani 1 1 d . . . C54 C 0.2982(3) 0.54764(14) 0.17207(13) 0.0341(10) Uani 1 1 d . . . C49 C 0.3781(3) 0.53306(15) 0.18500(14) 0.0425(11) Uani 1 1 d . . . H49 H 0.3909 0.5042 0.1991 0.051 Uiso 1 1 calc R . . C53 C 0.2799(3) 0.59109(15) 0.15202(15) 0.0487(13) Uani 1 1 d . . . H53 H 0.2266 0.6011 0.1434 0.058 Uiso 1 1 calc R . . C52 C 0.3402(4) 0.61977(18) 0.14467(17) 0.0642(16) Uani 1 1 d . . . H52 H 0.3274 0.6489 0.1311 0.077 Uiso 1 1 calc R . . C51 C 0.4185(4) 0.6053(2) 0.15733(18) 0.0711(18) Uani 1 1 d . . . H51 H 0.4588 0.6250 0.1528 0.085 Uiso 1 1 calc R . . C50 C 0.4394(3) 0.56139(18) 0.17698(17) 0.0582(14) Uani 1 1 d . . . H50 H 0.4926 0.5513 0.1845 0.070 Uiso 1 1 calc R . . C55 C -0.2143(2) 0.50558(13) 0.12817(13) 0.0292(9) Uani 1 1 d . . . C57 C -0.3072(3) 0.54096(15) 0.06282(16) 0.0425(11) Uani 1 1 d . . . H57 H -0.3164 0.5573 0.0350 0.051 Uiso 1 1 calc R . . C56 C -0.2294(2) 0.53051(15) 0.08696(14) 0.0346(10) Uani 1 1 d . . . H56 H -0.1866 0.5403 0.0754 0.042 Uiso 1 1 calc R . . C60 C -0.2792(3) 0.49256(14) 0.14644(16) 0.0371(10) Uani 1 1 d . . . H60 H -0.2699 0.4768 0.1746 0.044 Uiso 1 1 calc R . . C59 C -0.3568(3) 0.50339(17) 0.12215(19) 0.0514(13) Uani 1 1 d . . . H59 H -0.4000 0.4948 0.1340 0.062 Uiso 1 1 calc R . . C58 C -0.3709(3) 0.52728(16) 0.07971(18) 0.0491(12) Uani 1 1 d . . . H58 H -0.4234 0.5338 0.0631 0.059 Uiso 1 1 calc R . . C66 C -0.0361(2) 0.45793(14) 0.05887(13) 0.0290(9) Uani 1 1 d . . . H66 H 0.0067 0.4782 0.0698 0.035 Uiso 1 1 calc R . . C64 C -0.1121(3) 0.40878(14) -0.00200(14) 0.0344(10) Uani 1 1 d . . . H64 H -0.1197 0.3956 -0.0314 0.041 Uiso 1 1 calc R . . C62 C -0.1540(2) 0.41818(14) 0.06840(14) 0.0326(9) Uani 1 1 d . . . H62 H -0.1902 0.4114 0.0861 0.039 Uiso 1 1 calc R . . C61 C -0.0886(2) 0.44752(13) 0.08634(13) 0.0268(9) Uani 1 1 d . . . C65 C -0.0477(3) 0.43807(14) 0.01519(13) 0.0340(10) Uani 1 1 d . . . H65 H -0.0117 0.4446 -0.0027 0.041 Uiso 1 1 calc R . . C63 C -0.1653(3) 0.39929(15) 0.02505(14) 0.0388(11) Uani 1 1 d . . . H63 H -0.2091 0.3798 0.0135 0.047 Uiso 1 1 calc R . . N2 N 0.02366(18) 0.46864(10) 0.34217(10) 0.0242(7) Uani 1 1 d . . . N1 N -0.0456(2) 0.52329(11) 0.30390(10) 0.0296(8) Uani 1 1 d . . . N3 N -0.0899(2) 0.50469(11) 0.19636(10) 0.0287(8) Uani 1 1 d . . . N4 N -0.00683(18) 0.46621(11) 0.16765(10) 0.0273(7) Uani 1 1 d . . . N5 N 0.13448(18) 0.46908(10) 0.17982(10) 0.0238(7) Uani 1 1 d . . . N6 N 0.2050(2) 0.52248(10) 0.22054(10) 0.0285(8) Uani 1 1 d . . . N7 N 0.24501(19) 0.49777(10) 0.32603(10) 0.0259(7) Uani 1 1 d . . . N8 N 0.16160(18) 0.45502(10) 0.34981(10) 0.0231(7) Uani 1 1 d . . . C134 C 0.2795(3) 0.37562(15) 0.27248(15) 0.0428(12) Uani 1 1 d . . . F5 F 0.28015(15) 0.42070(8) 0.26114(9) 0.0457(6) Uani 1 1 d . . . F6 F 0.34030(16) 0.35507(9) 0.25962(11) 0.0626(8) Uani 1 1 d . . . F4 F 0.2948(2) 0.37297(11) 0.31897(9) 0.0763(10) Uani 1 1 d . . . Ni2 Ni 0.09507(3) 0.746734(15) 0.283897(15) 0.01890(12) Uani 1 1 d . . . C68 C 0.2062(2) 0.73913(12) 0.30833(11) 0.0201(8) Uani 1 1 d . . . C67 C 0.0860(2) 0.74858(11) 0.34644(12) 0.0190(7) Uani 1 1 d . . . C69 C 0.1051(2) 0.75264(12) 0.22127(12) 0.0197(8) Uani 1 1 d . . . C70 C -0.0154(2) 0.74751(12) 0.25880(12) 0.0200(8) Uani 1 1 d . . . C74 C 0.3286(2) 0.74071(12) 0.35983(12) 0.0225(8) Uani 1 1 d . . . C73 C 0.3295(2) 0.70651(13) 0.32808(12) 0.0230(8) Uani 1 1 d . . . C71 C 0.0537(2) 0.74443(12) 0.41617(12) 0.0232(8) Uani 1 1 d . . . C72 C 0.1243(2) 0.76783(12) 0.42348(12) 0.0230(8) Uani 1 1 d . . . C76 C 0.0744(2) 0.78210(12) 0.14787(12) 0.0201(8) Uani 1 1 d . . . C75 C 0.1409(2) 0.75615(12) 0.15323(12) 0.0210(8) Uani 1 1 d . . . C78 C -0.1439(2) 0.72186(13) 0.23345(12) 0.0234(8) Uani 1 1 d . . . C77 C -0.1355(2) 0.75891(13) 0.20655(12) 0.0234(8) Uani 1 1 d . . . C79 C -0.0399(2) 0.70336(12) 0.35025(12) 0.0214(8) Uani 1 1 d . . . H79A H -0.0876 0.7221 0.3487 0.026 Uiso 1 1 calc R . . H79B H -0.0398 0.6785 0.3723 0.026 Uiso 1 1 calc R . . C80 C -0.0471(2) 0.68172(12) 0.30303(12) 0.0226(8) Uani 1 1 d . . . H80A H 0.0039 0.6676 0.3023 0.027 Uiso 1 1 calc R . . H80B H -0.0876 0.6573 0.2980 0.027 Uiso 1 1 calc R . . C81 C 0.2129(2) 0.79313(12) 0.37054(12) 0.0232(8) Uani 1 1 d . . . H81A H 0.1959 0.8204 0.3513 0.028 Uiso 1 1 calc R . . H81B H 0.2501 0.8030 0.3992 0.028 Uiso 1 1 calc R . . C83 C 0.2217(2) 0.70240(13) 0.21185(12) 0.0248(8) Uani 1 1 d . . . H83A H 0.2734 0.7173 0.2145 0.030 Uiso 1 1 calc R . . H83B H 0.2148 0.6794 0.1872 0.030 Uiso 1 1 calc R . . C82 C 0.2246(2) 0.67727(12) 0.25674(12) 0.0238(8) Uani 1 1 d . . . H82A H 0.1711 0.6660 0.2563 0.029 Uiso 1 1 calc R . . H82B H 0.2599 0.6504 0.2592 0.029 Uiso 1 1 calc R . . C84 C -0.0101(2) 0.80613(12) 0.20271(12) 0.0202(8) Uani 1 1 d . . . H84A H -0.0449 0.8205 0.1754 0.024 Uiso 1 1 calc R . . H84B H 0.0132 0.8305 0.2246 0.024 Uiso 1 1 calc R . . C85 C 0.0077(2) 0.72909(13) 0.44928(12) 0.0257(9) Uani 1 1 d . . . C89 C -0.0005(2) 0.68541(15) 0.51676(14) 0.0348(10) Uani 1 1 d . . . H89 H 0.0240 0.6665 0.5418 0.042 Uiso 1 1 calc R . . C88 C -0.0786(3) 0.69863(17) 0.51074(15) 0.0421(11) Uani 1 1 d . . . H88 H -0.1080 0.6879 0.5310 0.051 Uiso 1 1 calc R . . C90 C 0.0424(2) 0.70005(14) 0.48566(13) 0.0296(9) Uani 1 1 d . . . H90 H 0.0953 0.6901 0.4894 0.036 Uiso 1 1 calc R . . C86 C -0.0712(2) 0.74312(15) 0.44423(14) 0.0362(10) Uani 1 1 d . . . H86 H -0.0953 0.7630 0.4200 0.043 Uiso 1 1 calc R . . C87 C -0.1145(3) 0.72798(18) 0.47460(15) 0.0452(12) Uani 1 1 d . . . H87 H -0.1676 0.7375 0.4708 0.054 Uiso 1 1 calc R . . C91 C 0.1758(2) 0.78701(12) 0.46746(12) 0.0254(8) Uani 1 1 d . . . C96 C 0.2575(2) 0.77583(14) 0.48233(13) 0.0302(9) Uani 1 1 d . . . H96 H 0.2798 0.7551 0.4650 0.036 Uiso 1 1 calc R . . C95 C 0.3058(3) 0.79497(15) 0.52233(13) 0.0372(10) Uani 1 1 d . . . H95 H 0.3603 0.7875 0.5317 0.045 Uiso 1 1 calc R . . C92 C 0.1424(3) 0.81693(15) 0.49386(14) 0.0385(10) Uani 1 1 d . . . H92 H 0.0880 0.8245 0.4848 0.046 Uiso 1 1 calc R . . C94 C 0.2730(3) 0.82494(15) 0.54803(14) 0.0421(11) Uani 1 1 d . . . H94 H 0.3056 0.8382 0.5748 0.050 Uiso 1 1 calc R . . C93 C 0.1926(3) 0.83588(15) 0.53503(14) 0.0469(12) Uani 1 1 d . . . H93 H 0.1709 0.8558 0.5534 0.056 Uiso 1 1 calc R . . C98 C 0.4154(2) 0.80478(14) 0.39792(13) 0.0323(10) Uani 1 1 d . . . H98 H 0.3944 0.8230 0.3718 0.039 Uiso 1 1 calc R . . C97 C 0.3906(2) 0.75858(13) 0.39913(13) 0.0268(9) Uani 1 1 d . . . C99 C 0.4709(3) 0.82346(15) 0.43533(14) 0.0399(11) Uani 1 1 d . . . H99 H 0.4872 0.8543 0.4343 0.048 Uiso 1 1 calc R . . C102 C 0.4249(2) 0.73181(15) 0.43795(13) 0.0337(10) Uani 1 1 d . . . H102 H 0.4104 0.7006 0.4387 0.040 Uiso 1 1 calc R . . C101 C 0.4801(3) 0.75075(16) 0.47536(14) 0.0413(11) Uani 1 1 d . . . H101 H 0.5022 0.7325 0.5013 0.050 Uiso 1 1 calc R . . C100 C 0.5024(3) 0.79680(16) 0.47431(14) 0.0426(11) Uani 1 1 d . . . H100 H 0.5387 0.8099 0.4998 0.051 Uiso 1 1 calc R . . C103 C 0.4163(2) 0.63558(14) 0.34890(14) 0.0326(9) Uani 1 1 d . . . H103 H 0.3954 0.6306 0.3745 0.039 Uiso 1 1 calc R . . C105 C 0.3927(2) 0.67461(13) 0.32081(13) 0.0270(9) Uani 1 1 d . . . C106 C 0.4250(3) 0.68111(16) 0.28312(15) 0.0402(11) Uani 1 1 d . . . H106 H 0.4111 0.7074 0.2646 0.048 Uiso 1 1 calc R . . C108 C 0.4999(3) 0.61030(17) 0.30063(18) 0.0464(12) Uani 1 1 d . . . H108 H 0.5348 0.5883 0.2935 0.056 Uiso 1 1 calc R . . C104 C 0.4706(3) 0.60434(15) 0.33881(17) 0.0427(11) Uani 1 1 d . . . H104 H 0.4874 0.5789 0.3583 0.051 Uiso 1 1 calc R . . C107 C 0.4783(3) 0.64856(19) 0.27264(17) 0.0505(13) Uani 1 1 d . . . H107 H 0.4989 0.6528 0.2468 0.061 Uiso 1 1 calc R . . C110 C 0.1571(2) 0.72322(13) 0.07895(13) 0.0271(9) Uani 1 1 d . . . H110 H 0.1031 0.7147 0.0717 0.033 Uiso 1 1 calc R . . C111 C 0.2039(3) 0.71302(14) 0.04823(14) 0.0352(10) Uani 1 1 d . . . H111 H 0.1809 0.6980 0.0203 0.042 Uiso 1 1 calc R . . C113 C 0.3183(3) 0.74801(15) 0.10005(14) 0.0358(10) Uani 1 1 d . . . H113 H 0.3726 0.7561 0.1073 0.043 Uiso 1 1 calc R . . C109 C 0.1908(2) 0.74603(12) 0.12016(12) 0.0219(8) Uani 1 1 d . . . C114 C 0.2714(2) 0.75878(14) 0.13038(13) 0.0280(9) Uani 1 1 d . . . H114 H 0.2941 0.7747 0.1578 0.034 Uiso 1 1 calc R . . C112 C 0.2840(3) 0.72511(14) 0.05888(14) 0.0338(10) Uani 1 1 d . . . H112 H 0.3151 0.7179 0.0384 0.041 Uiso 1 1 calc R . . C116 C -0.0551(2) 0.80000(14) 0.08973(12) 0.0272(9) Uani 1 1 d . . . H116 H -0.0811 0.7776 0.1033 0.033 Uiso 1 1 calc R . . C118 C -0.0588(2) 0.85820(14) 0.03103(13) 0.0343(10) Uani 1 1 d . . . H118 H -0.0877 0.8756 0.0060 0.041 Uiso 1 1 calc R . . C115 C 0.0268(2) 0.80806(12) 0.10723(11) 0.0212(8) Uani 1 1 d . . . C117 C -0.0980(2) 0.82572(14) 0.05169(13) 0.0310(9) Uani 1 1 d . . . H117 H -0.1531 0.8210 0.0402 0.037 Uiso 1 1 calc R . . C120 C 0.0654(2) 0.84066(14) 0.08557(13) 0.0313(9) Uani 1 1 d . . . H120 H 0.1202 0.8461 0.0969 0.038 Uiso 1 1 calc R . . C119 C 0.0219(3) 0.86487(15) 0.04712(14) 0.0387(11) Uani 1 1 d . . . H119 H 0.0481 0.8859 0.0322 0.046 Uiso 1 1 calc R . . C121 C -0.1923(2) 0.78401(13) 0.16902(13) 0.0258(8) Uani 1 1 d . . . C126 C -0.2355(2) 0.76036(15) 0.12969(13) 0.0334(10) Uani 1 1 d . . . H126 H -0.2297 0.7283 0.1275 0.040 Uiso 1 1 calc R . . C122 C -0.2030(2) 0.83169(15) 0.17187(15) 0.0369(10) Uani 1 1 d . . . H122 H -0.1756 0.8477 0.1983 0.044 Uiso 1 1 calc R . . C124 C -0.2951(2) 0.83152(15) 0.09639(15) 0.0391(11) Uani 1 1 d . . . H124 H -0.3283 0.8477 0.0718 0.047 Uiso 1 1 calc R . . C123 C -0.2532(3) 0.85550(16) 0.13645(16) 0.0439(11) Uani 1 1 d . . . H123 H -0.2597 0.8875 0.1388 0.053 Uiso 1 1 calc R . . C125 C -0.2867(3) 0.78434(16) 0.09391(15) 0.0401(11) Uani 1 1 d . . . H125 H -0.3157 0.7682 0.0679 0.048 Uiso 1 1 calc R . . C127 C -0.2122(2) 0.69019(14) 0.23178(14) 0.0306(9) Uani 1 1 d . . . C129 C -0.2953(3) 0.62459(17) 0.1983(2) 0.0625(17) Uani 1 1 d . . . H129 H -0.3083 0.6012 0.1759 0.075 Uiso 1 1 calc R . . C128 C -0.2313(3) 0.65620(15) 0.19757(17) 0.0438(11) Uani 1 1 d . . . H128 H -0.2030 0.6541 0.1747 0.053 Uiso 1 1 calc R . . C132 C -0.2561(3) 0.6919(2) 0.26460(16) 0.0592(15) Uani 1 1 d . . . H132 H -0.2433 0.7144 0.2878 0.071 Uiso 1 1 calc R . . C130 C -0.3371(3) 0.6283(2) 0.2312(2) 0.0709(18) Uani 1 1 d . . . H130 H -0.3791 0.6077 0.2309 0.085 Uiso 1 1 calc R . . C131 C -0.3185(3) 0.6614(3) 0.2643(2) 0.076(2) Uani 1 1 d . . . H131 H -0.3475 0.6637 0.2868 0.091 Uiso 1 1 calc R . . N9 N 0.14329(17) 0.77036(10) 0.38064(10) 0.0206(7) Uani 1 1 d . . . N10 N 0.03157(17) 0.73289(10) 0.36872(9) 0.0193(6) Uani 1 1 d . . . N11 N 0.25183(17) 0.76020(10) 0.34642(10) 0.0204(7) Uani 1 1 d . . . N12 N 0.25325(17) 0.70676(10) 0.29721(10) 0.0204(7) Uani 1 1 d . . . N13 N 0.05329(16) 0.77996(10) 0.18974(9) 0.0187(6) Uani 1 1 d . . . N14 N 0.15845(17) 0.73778(10) 0.19768(10) 0.0209(7) Uani 1 1 d . . . N16 N -0.05664(17) 0.77415(10) 0.22392(10) 0.0214(7) Uani 1 1 d . . . N15 N -0.06933(17) 0.71610(10) 0.26567(10) 0.0204(7) Uani 1 1 d . . . S1 S 0.14879(7) 0.59695(4) 0.38174(4) 0.0357(3) Uani 1 1 d . . . O1 O 0.16212(19) 0.55181(9) 0.40273(11) 0.0456(8) Uani 1 1 d . . . O3 O 0.07163(18) 0.61671(11) 0.38001(13) 0.0612(10) Uani 1 1 d . . . O2 O 0.1795(3) 0.60303(12) 0.34095(11) 0.0682(11) Uani 1 1 d . . . C133 C 0.2153(2) 0.63436(13) 0.42301(14) 0.0294(9) Uani 1 1 d . . . F2 F 0.21141(15) 0.67857(8) 0.40941(8) 0.0432(6) Uani 1 1 d . . . F3 F 0.29291(15) 0.62216(9) 0.43005(10) 0.0556(7) Uani 1 1 d . . . F1 F 0.20057(18) 0.63331(9) 0.46502(8) 0.0575(8) Uani 1 1 d . . . S3 S 0.01335(9) 0.35995(4) 0.83927(4) 0.0501(3) Uani 1 1 d . . . O7 O 0.0335(2) 0.31492(11) 0.85749(12) 0.0575(9) Uani 1 1 d . . . O8 O -0.0429(4) 0.36545(16) 0.79917(14) 0.120(2) Uani 1 1 d . . . O9 O 0.0889(3) 0.38675(16) 0.8409(2) 0.1176(19) Uani 1 1 d . . . C135 C -0.0168(4) 0.3925(2) 0.8830(2) 0.0629(15) Uani 1 1 d . . . F7 F -0.03481(19) 0.43623(10) 0.87083(11) 0.0680(9) Uani 1 1 d . . . F9 F -0.0859(3) 0.37090(15) 0.8885(2) 0.138(2) Uani 1 1 d . . . F8 F 0.0327(3) 0.39202(15) 0.92251(11) 0.1239(18) Uani 1 1 d . . . S4 S 0.10955(9) 0.02768(5) 0.74257(5) 0.0620(4) Uani 1 1 d . . . O12 O 0.0521(2) 0.04036(16) 0.70006(14) 0.0859(14) Uani 1 1 d . . . O10 O 0.1167(3) -0.02068(15) 0.74989(15) 0.1058(17) Uani 1 1 d . . . O11 O 0.1850(3) 0.0511(2) 0.75268(17) 0.1096(18) Uani 1 1 d . . . C136 C 0.0662(4) 0.0447(3) 0.7885(3) 0.106(3) Uani 1 1 d . . . F10 F -0.0025(3) 0.0233(2) 0.78522(17) 0.172(3) Uani 1 1 d . . . F11 F 0.1155(3) 0.0361(2) 0.83023(17) 0.154(2) Uani 1 1 d . . . F12 F 0.0519(3) 0.0898(2) 0.7872(3) 0.267(5) 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 Ni1 0.0399(3) 0.0222(3) 0.0158(2) -0.0006(2) 0.0026(2) 0.0073(2) S2 0.0440(6) 0.0254(5) 0.0216(5) -0.0007(4) 0.0017(4) 0.0103(5) O5 0.0476(18) 0.0286(15) 0.0216(14) -0.0014(12) -0.0027(13) 0.0066(13) O6 0.056(2) 0.0390(18) 0.0416(18) -0.0016(14) 0.0189(15) 0.0141(15) O4 0.064(2) 0.0290(16) 0.0364(17) 0.0040(13) 0.0085(15) 0.0092(15) C3 0.038(2) 0.020(2) 0.0189(19) 0.0014(15) 0.0031(17) 0.0101(18) C2 0.042(2) 0.0151(18) 0.0151(18) -0.0037(14) 0.0085(16) -0.0027(17) C4 0.047(3) 0.024(2) 0.0200(19) 0.0018(16) 0.0058(18) 0.0101(19) C1 0.034(2) 0.0199(19) 0.0215(19) -0.0053(16) 0.0004(17) 0.0057(17) C8 0.033(2) 0.022(2) 0.0181(18) 0.0011(15) 0.0055(16) 0.0049(17) C10 0.042(2) 0.021(2) 0.022(2) 0.0035(16) 0.0070(18) 0.0072(18) C6 0.029(2) 0.026(2) 0.024(2) -0.0054(16) 0.0045(17) 0.0010(17) C9 0.034(2) 0.0182(19) 0.0209(19) 0.0018(15) 0.0031(17) 0.0045(16) C7 0.029(2) 0.023(2) 0.0177(18) -0.0046(15) 0.0033(16) 0.0023(17) C5 0.039(2) 0.024(2) 0.024(2) -0.0045(16) 0.0053(18) 0.0032(18) C11 0.036(2) 0.026(2) 0.0201(19) 0.0024(16) 0.0035(17) 0.0074(18) C12 0.029(2) 0.025(2) 0.0215(19) 0.0007(16) 0.0011(16) 0.0069(17) C14 0.051(3) 0.029(2) 0.0181(19) -0.0001(16) 0.0040(18) -0.016(2) C13 0.031(2) 0.022(2) 0.0208(19) 0.0006(15) 0.0065(16) -0.0005(17) C18 0.056(3) 0.023(2) 0.022(2) -0.0012(16) 0.0044(19) 0.017(2) C16 0.029(2) 0.023(2) 0.0208(19) -0.0030(15) 0.0016(16) 0.0050(17) C15 0.062(3) 0.021(2) 0.0177(19) -0.0008(16) 0.0109(19) -0.009(2) C17 0.043(3) 0.041(3) 0.025(2) 0.0009(19) 0.0084(19) 0.024(2) C19 0.044(3) 0.031(2) 0.020(2) 0.0026(17) 0.0029(18) 0.0120(19) C24 0.045(3) 0.027(2) 0.025(2) 0.0018(17) 0.0141(19) 0.0057(19) C21 0.043(3) 0.079(4) 0.052(3) -0.021(3) -0.006(2) 0.029(3) C23 0.078(4) 0.035(3) 0.025(2) 0.0004(19) 0.022(2) 0.015(2) C20 0.047(3) 0.060(3) 0.039(3) -0.019(2) -0.005(2) 0.020(2) C22 0.060(3) 0.067(4) 0.028(2) -0.003(2) 0.007(2) 0.034(3) C25 0.036(2) 0.020(2) 0.024(2) -0.0037(16) 0.0080(17) 0.0007(17) C30 0.033(2) 0.025(2) 0.025(2) -0.0018(16) 0.0069(17) 0.0026(17) C27 0.038(3) 0.033(2) 0.046(3) -0.001(2) 0.019(2) -0.008(2) C28 0.056(3) 0.030(2) 0.036(2) -0.0004(19) 0.022(2) -0.003(2) C29 0.042(3) 0.027(2) 0.024(2) -0.0008(17) 0.0048(18) 0.0026(19) C26 0.034(2) 0.024(2) 0.038(2) -0.0081(18) 0.0052(19) -0.0013(18) C31 0.0183(19) 0.027(2) 0.0198(19) 0.0037(15) 0.0043(15) 0.0005(16) C36 0.028(2) 0.026(2) 0.0203(19) -0.0015(16) 0.0052(16) 0.0039(17) C35 0.028(2) 0.031(2) 0.034(2) 0.0076(18) 0.0116(18) 0.0011(18) C32 0.055(3) 0.027(2) 0.026(2) -0.0056(17) 0.008(2) -0.014(2) C34 0.036(2) 0.041(3) 0.026(2) 0.0113(19) 0.0039(18) -0.008(2) C33 0.059(3) 0.045(3) 0.019(2) -0.0033(19) 0.002(2) -0.020(2) C37 0.032(2) 0.024(2) 0.0182(18) 0.0032(16) 0.0071(16) -0.0015(17) C38 0.042(3) 0.047(3) 0.071(3) -0.027(3) 0.020(3) -0.011(2) C42 0.040(3) 0.054(3) 0.049(3) -0.023(2) 0.000(2) 0.002(2) C40 0.036(3) 0.056(3) 0.042(3) 0.009(2) -0.001(2) -0.007(2) C39 0.038(3) 0.056(3) 0.086(4) -0.006(3) 0.025(3) -0.001(2) C41 0.056(3) 0.080(4) 0.049(3) -0.027(3) -0.012(3) -0.017(3) C45 0.048(3) 0.0165(19) 0.026(2) 0.0001(16) 0.0045(19) 0.0094(18) C47 0.039(2) 0.027(2) 0.023(2) 0.0050(16) 0.0050(18) 0.0039(18) C44 0.038(2) 0.019(2) 0.023(2) 0.0018(16) 0.0045(17) 0.0054(17) C48 0.038(2) 0.020(2) 0.0214(19) -0.0023(15) 0.0044(17) 0.0065(17) C46 0.042(2) 0.030(2) 0.0191(19) -0.0040(17) 0.0069(18) 0.0065(19) C43 0.031(2) 0.024(2) 0.0165(18) 0.0020(15) -0.0015(16) 0.0068(17) C54 0.057(3) 0.024(2) 0.0179(19) -0.0004(16) 0.0049(19) -0.007(2) C49 0.063(3) 0.030(2) 0.029(2) 0.0017(19) 0.001(2) -0.012(2) C53 0.078(4) 0.030(2) 0.033(2) 0.008(2) 0.005(2) -0.007(2) C52 0.105(5) 0.042(3) 0.037(3) 0.013(2) 0.002(3) -0.026(3) C51 0.105(5) 0.053(4) 0.050(3) 0.000(3) 0.009(3) -0.047(4) C50 0.069(4) 0.051(3) 0.050(3) -0.003(2) 0.006(3) -0.025(3) C55 0.038(2) 0.024(2) 0.025(2) -0.0022(16) 0.0074(18) 0.0085(18) C57 0.041(3) 0.038(3) 0.044(3) 0.003(2) 0.001(2) 0.011(2) C56 0.029(2) 0.038(2) 0.033(2) 0.0015(19) 0.0017(18) 0.0104(19) C60 0.042(3) 0.025(2) 0.046(3) 0.0013(19) 0.014(2) 0.0019(19) C59 0.036(3) 0.044(3) 0.077(4) -0.001(3) 0.018(3) -0.003(2) C58 0.031(3) 0.043(3) 0.066(3) -0.002(2) -0.002(2) 0.011(2) C66 0.029(2) 0.029(2) 0.024(2) -0.0025(17) -0.0020(17) 0.0107(17) C64 0.045(3) 0.030(2) 0.022(2) -0.0055(17) -0.0019(19) 0.013(2) C62 0.034(2) 0.031(2) 0.031(2) -0.0029(18) 0.0063(18) 0.0042(19) C61 0.031(2) 0.023(2) 0.0224(19) -0.0016(16) 0.0005(17) 0.0102(17) C65 0.041(3) 0.034(2) 0.025(2) 0.0023(18) 0.0046(19) 0.017(2) C63 0.040(3) 0.032(2) 0.037(2) -0.0086(19) -0.003(2) 0.006(2) N2 0.0321(18) 0.0209(16) 0.0184(16) -0.0017(13) 0.0040(13) 0.0043(14) N1 0.046(2) 0.0227(17) 0.0175(16) -0.0028(13) 0.0036(15) 0.0083(15) N3 0.040(2) 0.0261(18) 0.0177(16) -0.0007(13) 0.0029(14) 0.0142(15) N4 0.0307(18) 0.0247(17) 0.0243(17) -0.0021(14) 0.0027(14) 0.0109(14) N5 0.0341(18) 0.0189(16) 0.0159(15) -0.0003(12) 0.0019(13) 0.0058(14) N6 0.052(2) 0.0166(16) 0.0145(15) -0.0014(12) 0.0039(15) 0.0013(15) N7 0.041(2) 0.0179(16) 0.0182(16) -0.0006(13) 0.0057(14) -0.0018(14) N8 0.0321(18) 0.0180(16) 0.0173(15) 0.0000(12) 0.0029(13) 0.0008(13) C134 0.055(3) 0.033(3) 0.032(2) -0.0071(19) -0.004(2) 0.017(2) F5 0.0482(15) 0.0269(13) 0.0536(16) -0.0104(11) -0.0030(12) 0.0061(11) F6 0.0415(16) 0.0382(16) 0.096(2) -0.0109(15) -0.0059(15) 0.0148(13) F4 0.108(3) 0.065(2) 0.0301(15) -0.0074(14) -0.0312(15) 0.0127(18) Ni2 0.0208(2) 0.0172(2) 0.0160(2) 0.00003(18) -0.00041(18) -0.00074(19) C68 0.026(2) 0.0183(19) 0.0152(17) 0.0012(14) 0.0033(15) -0.0039(16) C67 0.0208(18) 0.0120(17) 0.0218(18) 0.0014(14) 0.0009(15) 0.0021(15) C69 0.0153(17) 0.0207(19) 0.0203(18) -0.0012(15) -0.0005(14) -0.0028(15) C70 0.026(2) 0.0163(18) 0.0181(18) -0.0011(14) 0.0057(15) 0.0020(16) C74 0.0227(19) 0.0202(19) 0.0229(19) 0.0083(15) 0.0027(15) -0.0009(15) C73 0.0206(19) 0.025(2) 0.0195(19) 0.0064(15) -0.0013(15) 0.0006(16) C71 0.025(2) 0.0214(19) 0.0203(19) -0.0019(15) -0.0001(15) 0.0028(16) C72 0.029(2) 0.0198(19) 0.0195(19) -0.0017(15) 0.0042(16) 0.0043(16) C76 0.023(2) 0.0179(18) 0.0177(18) 0.0007(14) 0.0018(15) -0.0041(15) C75 0.0228(19) 0.0202(19) 0.0176(18) -0.0016(15) 0.0002(15) -0.0031(16) C78 0.026(2) 0.024(2) 0.0175(18) -0.0003(15) 0.0009(16) -0.0008(16) C77 0.021(2) 0.027(2) 0.0201(19) -0.0045(15) 0.0011(15) -0.0012(16) C79 0.0218(19) 0.023(2) 0.0185(18) 0.0008(15) 0.0038(15) -0.0023(16) C80 0.0229(19) 0.0203(19) 0.0222(19) 0.0002(15) 0.0015(15) -0.0053(15) C81 0.030(2) 0.0156(18) 0.0203(19) -0.0004(15) 0.0000(16) -0.0023(16) C83 0.025(2) 0.023(2) 0.0236(19) -0.0018(16) 0.0002(16) 0.0031(16) C82 0.025(2) 0.0187(19) 0.025(2) -0.0010(15) 0.0013(16) 0.0041(16) C84 0.0210(19) 0.0205(19) 0.0171(18) 0.0026(14) 0.0011(15) 0.0003(15) C85 0.027(2) 0.028(2) 0.0191(19) -0.0105(16) 0.0016(16) -0.0014(17) C89 0.037(3) 0.037(2) 0.034(2) 0.0004(19) 0.0166(19) -0.001(2) C88 0.039(3) 0.058(3) 0.035(2) -0.013(2) 0.019(2) -0.014(2) C90 0.028(2) 0.032(2) 0.029(2) -0.0017(18) 0.0091(18) -0.0010(18) C86 0.035(2) 0.050(3) 0.024(2) -0.0078(19) 0.0086(18) 0.011(2) C87 0.027(2) 0.073(4) 0.037(3) -0.018(2) 0.009(2) 0.005(2) C91 0.034(2) 0.0188(19) 0.0203(19) -0.0030(15) 0.0018(17) -0.0066(17) C96 0.038(2) 0.026(2) 0.023(2) 0.0040(16) 0.0003(18) -0.0040(18) C95 0.045(3) 0.034(2) 0.025(2) 0.0059(19) -0.0053(19) -0.009(2) C92 0.050(3) 0.036(2) 0.026(2) -0.0085(19) 0.004(2) 0.001(2) C94 0.057(3) 0.032(2) 0.027(2) 0.0023(19) -0.008(2) -0.017(2) C93 0.081(4) 0.030(2) 0.027(2) -0.0091(19) 0.009(2) -0.005(2) C98 0.034(2) 0.030(2) 0.027(2) 0.0089(17) -0.0038(18) -0.0043(18) C97 0.022(2) 0.031(2) 0.024(2) 0.0052(17) 0.0008(16) -0.0031(17) C99 0.042(3) 0.034(2) 0.034(2) 0.0028(19) -0.008(2) -0.013(2) C102 0.032(2) 0.034(2) 0.030(2) 0.0110(18) -0.0038(18) -0.0102(19) C101 0.040(3) 0.046(3) 0.029(2) 0.010(2) -0.0083(19) -0.010(2) C100 0.038(3) 0.053(3) 0.026(2) 0.004(2) -0.0107(19) -0.011(2) C103 0.029(2) 0.033(2) 0.034(2) 0.0072(18) 0.0033(18) 0.0022(18) C105 0.021(2) 0.028(2) 0.029(2) 0.0008(17) -0.0001(16) 0.0005(16) C106 0.038(3) 0.044(3) 0.040(3) 0.008(2) 0.010(2) 0.006(2) C108 0.029(2) 0.044(3) 0.066(3) -0.009(3) 0.012(2) 0.003(2) C104 0.033(2) 0.031(2) 0.058(3) 0.009(2) 0.000(2) 0.005(2) C107 0.043(3) 0.067(4) 0.046(3) 0.003(3) 0.018(2) 0.012(3) C110 0.026(2) 0.027(2) 0.029(2) -0.0032(17) 0.0075(17) -0.0037(17) C111 0.048(3) 0.033(2) 0.026(2) -0.0046(18) 0.0107(19) -0.001(2) C113 0.032(2) 0.048(3) 0.029(2) 0.007(2) 0.0092(18) -0.002(2) C109 0.025(2) 0.023(2) 0.0189(18) 0.0021(15) 0.0074(15) 0.0020(16) C114 0.027(2) 0.033(2) 0.0214(19) 0.0001(16) 0.0021(16) -0.0006(17) C112 0.043(3) 0.030(2) 0.035(2) 0.0049(18) 0.021(2) 0.011(2) C116 0.027(2) 0.032(2) 0.0209(19) 0.0005(16) 0.0029(16) -0.0056(17) C118 0.038(2) 0.036(2) 0.024(2) 0.0091(18) -0.0014(18) 0.009(2) C115 0.025(2) 0.025(2) 0.0120(17) -0.0025(14) 0.0022(15) 0.0014(16) C117 0.027(2) 0.037(2) 0.026(2) -0.0042(18) -0.0005(17) 0.0053(18) C120 0.025(2) 0.041(2) 0.026(2) 0.0051(18) 0.0023(17) -0.0067(18) C119 0.043(3) 0.040(3) 0.030(2) 0.0168(19) 0.003(2) -0.005(2) C121 0.021(2) 0.030(2) 0.025(2) 0.0058(16) 0.0026(16) 0.0007(17) C126 0.035(2) 0.029(2) 0.029(2) 0.0023(17) -0.0056(18) -0.0001(18) C122 0.032(2) 0.037(3) 0.037(2) -0.0062(19) -0.0001(19) 0.0069(19) C124 0.030(2) 0.040(3) 0.042(3) 0.012(2) -0.001(2) 0.007(2) C123 0.037(3) 0.032(3) 0.053(3) 0.003(2) -0.004(2) 0.011(2) C125 0.038(3) 0.043(3) 0.034(2) 0.003(2) -0.003(2) -0.002(2) C127 0.023(2) 0.031(2) 0.031(2) 0.0087(18) -0.0048(17) -0.0078(17) C129 0.032(3) 0.030(3) 0.106(5) -0.010(3) -0.019(3) 0.004(2) C128 0.032(2) 0.029(2) 0.065(3) -0.002(2) 0.004(2) -0.004(2) C132 0.050(3) 0.090(4) 0.034(3) 0.002(3) 0.002(2) -0.033(3) C130 0.042(3) 0.072(4) 0.095(5) 0.038(4) 0.011(3) -0.016(3) C131 0.050(3) 0.120(6) 0.053(3) 0.010(4) 0.003(3) -0.042(4) N9 0.0239(17) 0.0182(16) 0.0184(15) -0.0004(12) 0.0026(13) -0.0012(13) N10 0.0219(16) 0.0166(15) 0.0184(15) -0.0019(12) 0.0031(13) -0.0008(12) N11 0.0219(16) 0.0179(16) 0.0182(15) 0.0017(12) -0.0010(13) -0.0044(13) N12 0.0208(16) 0.0192(16) 0.0195(15) 0.0029(12) 0.0018(13) -0.0008(13) N13 0.0190(15) 0.0190(16) 0.0173(15) -0.0009(12) 0.0035(12) -0.0012(12) N14 0.0223(16) 0.0196(16) 0.0192(15) 0.0016(12) 0.0023(13) 0.0010(13) N16 0.0215(16) 0.0203(16) 0.0217(16) 0.0006(13) 0.0040(13) 0.0016(13) N15 0.0180(15) 0.0210(16) 0.0193(15) -0.0024(12) -0.0007(12) -0.0027(13) S1 0.0416(6) 0.0246(5) 0.0355(6) -0.0029(4) -0.0002(5) 0.0003(5) O1 0.056(2) 0.0207(15) 0.058(2) -0.0003(14) 0.0108(16) 0.0037(14) O3 0.0330(18) 0.040(2) 0.099(3) 0.0048(19) -0.0058(18) -0.0033(15) O2 0.115(3) 0.051(2) 0.0366(19) -0.0094(16) 0.017(2) -0.006(2) C133 0.032(2) 0.025(2) 0.033(2) 0.0025(17) 0.0119(18) 0.0020(18) F2 0.0525(16) 0.0210(12) 0.0524(15) 0.0030(11) 0.0059(13) -0.0048(11) F3 0.0318(15) 0.0531(17) 0.0748(19) 0.0051(14) 0.0005(13) 0.0018(13) F1 0.093(2) 0.0542(17) 0.0285(14) -0.0069(12) 0.0210(14) -0.0064(16) S3 0.0767(9) 0.0351(7) 0.0394(7) -0.0095(5) 0.0162(6) -0.0005(6) O7 0.064(2) 0.0302(18) 0.078(2) -0.0064(16) 0.0159(19) 0.0031(16) O8 0.186(5) 0.082(3) 0.051(3) -0.010(2) -0.047(3) -0.004(3) O9 0.089(3) 0.089(3) 0.211(6) 0.002(4) 0.104(4) -0.020(3) C135 0.073(4) 0.051(4) 0.064(4) 0.004(3) 0.018(3) 0.017(3) F7 0.082(2) 0.0378(17) 0.085(2) -0.0030(15) 0.0206(18) 0.0191(15) F9 0.139(4) 0.100(3) 0.220(5) 0.061(3) 0.132(4) 0.023(3) F8 0.192(5) 0.118(3) 0.0351(19) -0.023(2) -0.020(2) 0.069(3) S4 0.0660(9) 0.0674(10) 0.0577(8) 0.0226(7) 0.0251(7) 0.0117(8) O12 0.074(3) 0.103(3) 0.077(3) 0.055(3) 0.012(2) 0.012(2) O10 0.153(4) 0.055(3) 0.077(3) -0.001(2) -0.030(3) 0.029(3) O11 0.058(3) 0.161(5) 0.113(4) 0.058(3) 0.027(3) -0.013(3) C136 0.057(4) 0.137(8) 0.121(7) -0.055(6) 0.016(4) -0.024(5) F10 0.103(3) 0.314(8) 0.125(4) -0.128(5) 0.074(3) -0.101(4) F11 0.092(3) 0.273(7) 0.102(3) -0.097(4) 0.032(3) -0.026(4) F12 0.118(4) 0.115(4) 0.522(13) -0.209(7) -0.006(6) 0.020(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 Ni1 C3 1.870(4) . ? Ni1 C1 1.877(4) . ? Ni1 C2 1.907(4) . ? Ni1 C4 1.925(4) . ? S2 O4 1.434(3) . ? S2 O6 1.437(3) . ? S2 O5 1.440(3) . ? S2 C134 1.816(5) . ? C3 N6 1.336(5) . ? C3 N5 1.349(4) . ? C2 N7 1.366(5) . ? C2 N8 1.370(4) . ? C4 N4 1.358(5) . ? C4 N3 1.362(5) . ? C1 N1 1.321(5) . ? C1 N2 1.340(5) . ? C8 C7 1.347(5) . ? C8 N7 1.389(4) . ? C8 C37 1.480(5) . ? C10 C9 1.361(5) . ? C10 N6 1.404(5) . ? C10 C54 1.463(6) . ? C6 C5 1.356(5) . ? C6 N2 1.408(5) . ? C6 C25 1.472(5) . ? C9 N5 1.393(5) . ? C9 C43 1.485(5) . ? C7 N8 1.390(4) . ? C7 C31 1.473(5) . ? C5 N1 1.396(5) . ? C5 C19 1.478(5) . ? C11 C12 1.343(5) . ? C11 N3 1.402(5) . ? C11 C55 1.483(5) . ? C12 N4 1.388(5) . ? C12 C61 1.472(5) . ? C14 N7 1.480(5) . ? C14 C15 1.507(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C13 N8 1.451(5) . ? C13 N2 1.457(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C18 N1 1.469(5) . ? C18 C17 1.507(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C16 N4 1.457(5) . ? C16 N5 1.458(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C15 N6 1.460(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 N3 1.469(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C24 1.392(5) . ? C19 C20 1.392(6) . ? C24 C23 1.385(6) . ? C24 H24 0.9300 . ? C21 C22 1.377(7) . ? C21 C20 1.407(6) . ? C21 H21 0.9300 . ? C23 C22 1.368(7) . ? C23 H23 0.9300 . ? C20 H20 0.9300 . ? C22 H22 0.9300 . ? C25 C30 1.385(5) . ? C25 C26 1.400(5) . ? C30 C29 1.395(5) . ? C30 H30 0.9300 . ? C27 C28 1.380(6) . ? C27 C26 1.387(6) . ? C27 H27 0.9300 . ? C28 C29 1.372(6) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.386(5) . ? C31 C36 1.390(5) . ? C36 C35 1.387(5) . ? C36 H36 0.9300 . ? C35 C34 1.382(6) . ? C35 H35 0.9300 . ? C32 C33 1.381(6) . ? C32 H32 0.9300 . ? C34 C33 1.379(6) . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C37 C38 1.349(6) . ? C37 C42 1.369(6) . ? C38 C39 1.394(7) . ? C38 H38 0.9300 . ? C42 C41 1.384(6) . ? C42 H42 0.9300 . ? C40 C39 1.334(7) . ? C40 C41 1.346(7) . ? C40 H40 0.9300 . ? C39 H39 0.9300 . ? C41 H41 0.9300 . ? C45 C46 1.374(5) . ? C45 C44 1.377(5) . ? C45 H45 0.9300 . ? C47 C48 1.377(5) . ? C47 C46 1.378(5) . ? C47 H47 0.9300 . ? C44 C43 1.385(5) . ? C44 H44 0.9300 . ? C48 C43 1.388(5) . ? C48 H48 0.9300 . ? C46 H46 0.9300 . ? C54 C53 1.383(6) . ? C54 C49 1.392(6) . ? C49 C50 1.395(6) . ? C49 H49 0.9300 . ? C53 C52 1.381(7) . ? C53 H53 0.9300 . ? C52 C51 1.366(8) . ? C52 H52 0.9300 . ? C51 C50 1.396(8) . ? C51 H51 0.9300 . ? C50 H50 0.9300 . ? C55 C56 1.386(5) . ? C55 C60 1.406(6) . ? C57 C58 1.370(6) . ? C57 C56 1.379(6) . ? C57 H57 0.9300 . ? C56 H56 0.9300 . ? C60 C59 1.381(6) . ? C60 H60 0.9300 . ? C59 C58 1.402(7) . ? C59 H59 0.9300 . ? C58 H58 0.9300 . ? C66 C65 1.386(5) . ? C66 C61 1.392(5) . ? C66 H66 0.9300 . ? C64 C65 1.379(6) . ? C64 C63 1.387(6) . ? C64 H64 0.9300 . ? C62 C63 1.366(5) . ? C62 C61 1.396(5) . ? C62 H62 0.9300 . ? C65 H65 0.9300 . ? C63 H63 0.9300 . ? C134 F6 1.335(5) . ? C134 F5 1.337(5) . ? C134 F4 1.342(5) . ? Ni2 C70 1.854(4) . ? Ni2 C68 1.874(4) . ? Ni2 C67 1.905(3) . ? Ni2 C69 1.920(3) . ? C68 N12 1.326(4) . ? C68 N11 1.347(4) . ? C67 N10 1.351(4) . ? C67 N9 1.373(4) . ? C69 N14 1.354(4) . ? C69 N13 1.365(4) . ? C70 N16 1.338(4) . ? C70 N15 1.343(4) . ? C74 C73 1.364(5) . ? C74 N11 1.394(4) . ? C74 C97 1.460(5) . ? C73 N12 1.396(4) . ? C73 C105 1.477(5) . ? C71 C72 1.353(5) . ? C71 N10 1.405(4) . ? C71 C85 1.475(5) . ? C72 N9 1.394(4) . ? C72 C91 1.487(5) . ? C76 C75 1.338(5) . ? C76 N13 1.383(4) . ? C76 C115 1.478(5) . ? C75 N14 1.384(4) . ? C75 C109 1.486(5) . ? C78 C77 1.360(5) . ? C78 N15 1.402(4) . ? C78 C127 1.473(5) . ? C77 N16 1.392(4) . ? C77 C121 1.471(5) . ? C79 N10 1.477(4) . ? C79 C80 1.511(5) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 N15 1.462(4) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 N11 1.447(5) . ? C81 N9 1.457(5) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C83 N14 1.468(4) . ? C83 C82 1.507(5) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C82 N12 1.452(4) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C84 N13 1.451(4) . ? C84 N16 1.459(4) . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C90 1.376(5) . ? C85 C86 1.384(5) . ? C89 C88 1.360(6) . ? C89 C90 1.385(5) . ? C89 H89 0.9300 . ? C88 C87 1.382(6) . ? C88 H88 0.9300 . ? C90 H90 0.9300 . ? C86 C87 1.376(6) . ? C86 H86 0.9300 . ? C87 H87 0.9300 . ? C91 C92 1.381(5) . ? C91 C96 1.397(5) . ? C96 C95 1.381(5) . ? C96 H96 0.9300 . ? C95 C94 1.363(6) . ? C95 H95 0.9300 . ? C92 C93 1.416(6) . ? C92 H92 0.9300 . ? C94 C93 1.372(7) . ? C94 H94 0.9300 . ? C93 H93 0.9300 . ? C98 C99 1.377(5) . ? C98 C97 1.395(5) . ? C98 H98 0.9300 . ? C97 C102 1.388(5) . ? C99 C100 1.380(6) . ? C99 H99 0.9300 . ? C102 C101 1.378(5) . ? C102 H102 0.9300 . ? C101 C100 1.378(6) . ? C101 H101 0.9300 . ? C100 H100 0.9300 . ? C103 C104 1.379(6) . ? C103 C105 1.394(5) . ? C103 H103 0.9300 . ? C105 C106 1.382(5) . ? C106 C107 1.395(6) . ? C106 H106 0.9300 . ? C108 C104 1.363(6) . ? C108 C107 1.371(7) . ? C108 H108 0.9300 . ? C104 H104 0.9300 . ? C107 H107 0.9300 . ? C110 C109 1.381(5) . ? C110 C111 1.390(5) . ? C110 H110 0.9300 . ? C111 C112 1.375(6) . ? C111 H111 0.9300 . ? C113 C112 1.383(6) . ? C113 C114 1.387(5) . ? C113 H113 0.9300 . ? C109 C114 1.388(5) . ? C114 H114 0.9300 . ? C112 H112 0.9300 . ? C116 C115 1.389(5) . ? C116 C117 1.395(5) . ? C116 H116 0.9300 . ? C118 C119 1.359(6) . ? C118 C117 1.381(6) . ? C118 H118 0.9300 . ? C115 C120 1.394(5) . ? C117 H117 0.9300 . ? C120 C119 1.384(5) . ? C120 H120 0.9300 . ? C119 H119 0.9300 . ? C121 C122 1.386(6) . ? C121 C126 1.393(5) . ? C126 C125 1.381(5) . ? C126 H126 0.9300 . ? C122 C123 1.364(6) . ? C122 H122 0.9300 . ? C124 C125 1.365(6) . ? C124 C123 1.406(6) . ? C124 H124 0.9300 . ? C123 H123 0.9300 . ? C125 H125 0.9300 . ? C127 C132 1.376(6) . ? C127 C128 1.387(6) . ? C129 C130 1.355(8) . ? C129 C128 1.428(7) . ? C129 H129 0.9300 . ? C128 H128 0.9300 . ? C132 C131 1.382(7) . ? C132 H132 0.9300 . ? C130 C131 1.349(9) . ? C130 H130 0.9300 . ? C131 H131 0.9300 . ? S1 O3 1.429(3) . ? S1 O1 1.431(3) . ? S1 O2 1.450(4) . ? S1 C133 1.803(4) . ? C133 F2 1.328(4) . ? C133 F1 1.335(4) . ? C133 F3 1.342(4) . ? S3 O8 1.341(4) . ? S3 O7 1.410(3) . ? S3 O9 1.497(4) . ? S3 C135 1.780(6) . ? C135 F8 1.265(6) . ? C135 F7 1.320(6) . ? C135 F9 1.385(7) . ? S4 O10 1.405(4) . ? S4 O11 1.422(5) . ? S4 O12 1.440(4) . ? S4 C136 1.780(8) . ? C136 F10 1.311(8) . ? C136 F12 1.316(10) . ? C136 F11 1.337(9) . ? 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 C3 Ni1 C1 174.38(16) . . ? C3 Ni1 C2 92.24(16) . . ? C1 Ni1 C2 86.93(16) . . ? C3 Ni1 C4 87.63(17) . . ? C1 Ni1 C4 93.96(16) . . ? C2 Ni1 C4 172.07(16) . . ? O4 S2 O6 115.98(19) . . ? O4 S2 O5 115.16(17) . . ? O6 S2 O5 114.02(17) . . ? O4 S2 C134 103.93(19) . . ? O6 S2 C134 103.69(19) . . ? O5 S2 C134 101.52(19) . . ? N6 C3 N5 105.0(3) . . ? N6 C3 Ni1 128.4(3) . . ? N5 C3 Ni1 126.2(3) . . ? N7 C2 N8 102.6(3) . . ? N7 C2 Ni1 136.3(3) . . ? N8 C2 Ni1 121.0(3) . . ? N4 C4 N3 104.0(3) . . ? N4 C4 Ni1 120.5(3) . . ? N3 C4 Ni1 135.5(3) . . ? N1 C1 N2 105.5(3) . . ? N1 C1 Ni1 128.7(3) . . ? N2 C1 Ni1 125.3(3) . . ? C7 C8 N7 106.7(3) . . ? C7 C8 C37 129.3(3) . . ? N7 C8 C37 124.0(3) . . ? C9 C10 N6 105.5(3) . . ? C9 C10 C54 132.0(4) . . ? N6 C10 C54 122.4(3) . . ? C5 C6 N2 105.5(3) . . ? C5 C6 C25 129.2(4) . . ? N2 C6 C25 125.3(3) . . ? C10 C9 N5 106.4(3) . . ? C10 C9 C43 130.4(4) . . ? N5 C9 C43 123.2(3) . . ? C8 C7 N8 106.3(3) . . ? C8 C7 C31 130.0(3) . . ? N8 C7 C31 123.7(3) . . ? C6 C5 N1 106.0(3) . . ? C6 C5 C19 131.0(4) . . ? N1 C5 C19 123.0(3) . . ? C12 C11 N3 107.6(3) . . ? C12 C11 C55 128.5(3) . . ? N3 C11 C55 123.9(3) . . ? C11 C12 N4 105.8(3) . . ? C11 C12 C61 130.0(3) . . ? N4 C12 C61 124.2(3) . . ? N7 C14 C15 115.6(3) . . ? N7 C14 H14A 108.4 . . ? C15 C14 H14A 108.4 . . ? N7 C14 H14B 108.4 . . ? C15 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? N8 C13 N2 108.0(3) . . ? N8 C13 H13A 110.1 . . ? N2 C13 H13A 110.1 . . ? N8 C13 H13B 110.1 . . ? N2 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N1 C18 C17 112.1(3) . . ? N1 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N1 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N4 C16 N5 108.1(3) . . ? N4 C16 H16A 110.1 . . ? N5 C16 H16A 110.1 . . ? N4 C16 H16B 110.1 . . ? N5 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? N6 C15 C14 112.9(3) . . ? N6 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? N6 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N3 C17 C18 115.7(3) . . ? N3 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? N3 C17 H17B 108.4 . . ? C18 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C24 C19 C20 120.0(4) . . ? C24 C19 C5 119.6(4) . . ? C20 C19 C5 120.4(4) . . ? C23 C24 C19 119.0(4) . . ? C23 C24 H24 120.5 . . ? C19 C24 H24 120.5 . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C22 C23 C24 121.7(4) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C30 C25 C26 119.4(4) . . ? C30 C25 C6 121.5(4) . . ? C26 C25 C6 119.0(4) . . ? C25 C30 C29 120.2(4) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C28 C27 C26 121.4(4) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 120.6(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C27 C26 C25 119.2(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C32 C31 C36 118.7(3) . . ? C32 C31 C7 120.4(3) . . ? C36 C31 C7 120.8(3) . . ? C35 C36 C31 120.4(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C33 C32 C31 120.8(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C33 C34 C35 119.7(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C32 C33 C34 120.2(4) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C38 C37 C42 118.9(4) . . ? C38 C37 C8 121.4(4) . . ? C42 C37 C8 119.6(4) . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C37 C42 C41 119.3(4) . . ? C37 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C39 C40 C41 119.2(5) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C39 C38 120.5(5) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C40 C41 C42 121.5(5) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C46 C45 C44 121.2(4) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C48 C47 C46 120.7(4) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C45 C44 C43 119.6(4) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C47 C48 C43 120.0(4) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C45 C46 C47 119.1(4) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C44 C43 C48 119.5(3) . . ? C44 C43 C9 120.9(3) . . ? C48 C43 C9 119.6(3) . . ? C53 C54 C49 119.4(4) . . ? C53 C54 C10 119.8(4) . . ? C49 C54 C10 120.8(4) . . ? C50 C49 C54 120.6(4) . . ? C50 C49 H49 119.7 . . ? C54 C49 H49 119.7 . . ? C54 C53 C52 120.5(5) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C51 C52 C53 119.9(5) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C52 C51 C50 121.4(5) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C50 C49 118.2(6) . . ? C51 C50 H50 120.9 . . ? C49 C50 H50 120.9 . . ? C56 C55 C60 119.3(4) . . ? C56 C55 C11 118.2(4) . . ? C60 C55 C11 122.5(3) . . ? C58 C57 C56 120.2(4) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C56 C55 120.9(4) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C59 C60 C55 119.4(4) . . ? C59 C60 H60 120.3 . . ? C55 C60 H60 120.3 . . ? C60 C59 C58 120.3(4) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C57 C58 C59 119.8(4) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C65 C66 C61 120.0(4) . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C65 C64 C63 119.1(4) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C63 C62 C61 120.6(4) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C66 C61 C62 118.8(3) . . ? C66 C61 C12 121.4(4) . . ? C62 C61 C12 119.8(4) . . ? C64 C65 C66 120.7(4) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C62 C63 C64 120.8(4) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C1 N2 C6 111.0(3) . . ? C1 N2 C13 118.8(3) . . ? C6 N2 C13 130.1(3) . . ? C1 N1 C5 112.0(3) . . ? C1 N1 C18 122.0(3) . . ? C5 N1 C18 126.0(3) . . ? C4 N3 C11 110.4(3) . . ? C4 N3 C17 129.3(3) . . ? C11 N3 C17 120.2(3) . . ? C4 N4 C12 112.3(3) . . ? C4 N4 C16 122.2(3) . . ? C12 N4 C16 125.0(3) . . ? C3 N5 C9 111.3(3) . . ? C3 N5 C16 117.9(3) . . ? C9 N5 C16 129.7(3) . . ? C3 N6 C10 111.8(3) . . ? C3 N6 C15 121.6(3) . . ? C10 N6 C15 126.6(3) . . ? C2 N7 C8 112.1(3) . . ? C2 N7 C14 129.0(3) . . ? C8 N7 C14 118.8(3) . . ? C2 N8 C7 112.2(3) . . ? C2 N8 C13 121.7(3) . . ? C7 N8 C13 125.9(3) . . ? F6 C134 F5 107.3(4) . . ? F6 C134 F4 107.7(4) . . ? F5 C134 F4 107.6(3) . . ? F6 C134 S2 111.0(3) . . ? F5 C134 S2 111.9(3) . . ? F4 C134 S2 111.0(4) . . ? C70 Ni2 C68 173.96(15) . . ? C70 Ni2 C67 93.80(15) . . ? C68 Ni2 C67 87.12(14) . . ? C70 Ni2 C69 86.63(14) . . ? C68 Ni2 C69 93.15(14) . . ? C67 Ni2 C69 173.33(15) . . ? N12 C68 N11 105.2(3) . . ? N12 C68 Ni2 127.5(3) . . ? N11 C68 Ni2 126.4(3) . . ? N10 C67 N9 104.0(3) . . ? N10 C67 Ni2 134.9(3) . . ? N9 C67 Ni2 121.1(2) . . ? N14 C69 N13 103.5(3) . . ? N14 C69 Ni2 135.4(3) . . ? N13 C69 Ni2 120.9(2) . . ? N16 C70 N15 104.6(3) . . ? N16 C70 Ni2 127.3(3) . . ? N15 C70 Ni2 127.2(3) . . ? C73 C74 N11 105.4(3) . . ? C73 C74 C97 132.3(3) . . ? N11 C74 C97 122.2(3) . . ? C74 C73 N12 106.2(3) . . ? C74 C73 C105 133.1(3) . . ? N12 C73 C105 120.6(3) . . ? C72 C71 N10 106.4(3) . . ? C72 C71 C85 130.4(3) . . ? N10 C71 C85 123.0(3) . . ? C71 C72 N9 106.5(3) . . ? C71 C72 C91 129.4(3) . . ? N9 C72 C91 124.1(3) . . ? C75 C76 N13 106.1(3) . . ? C75 C76 C115 131.1(3) . . ? N13 C76 C115 122.8(3) . . ? C76 C75 N14 107.5(3) . . ? C76 C75 C109 130.2(3) . . ? N14 C75 C109 122.3(3) . . ? C77 C78 N15 106.3(3) . . ? C77 C78 C127 131.6(3) . . ? N15 C78 C127 122.1(3) . . ? C78 C77 N16 105.4(3) . . ? C78 C77 C121 132.9(3) . . ? N16 C77 C121 121.6(3) . . ? N10 C79 C80 116.6(3) . . ? N10 C79 H79A 108.1 . . ? C80 C79 H79A 108.2 . . ? N10 C79 H79B 108.1 . . ? C80 C79 H79B 108.1 . . ? H79A C79 H79B 107.3 . . ? N15 C80 C79 111.9(3) . . ? N15 C80 H80A 109.2 . . ? C79 C80 H80A 109.2 . . ? N15 C80 H80B 109.2 . . ? C79 C80 H80B 109.2 . . ? H80A C80 H80B 107.9 . . ? N11 C81 N9 108.3(3) . . ? N11 C81 H81A 110.0 . . ? N9 C81 H81A 110.0 . . ? N11 C81 H81B 110.0 . . ? N9 C81 H81B 110.0 . . ? H81A C81 H81B 108.4 . . ? N14 C83 C82 116.2(3) . . ? N14 C83 H83A 108.2 . . ? C82 C83 H83A 108.2 . . ? N14 C83 H83B 108.2 . . ? C82 C83 H83B 108.2 . . ? H83A C83 H83B 107.4 . . ? N12 C82 C83 112.6(3) . . ? N12 C82 H82A 109.1 . . ? C83 C82 H82A 109.1 . . ? N12 C82 H82B 109.1 . . ? C83 C82 H82B 109.1 . . ? H82A C82 H82B 107.8 . . ? N13 C84 N16 108.5(3) . . ? N13 C84 H84A 110.0 . . ? N16 C84 H84A 110.0 . . ? N13 C84 H84B 110.0 . . ? N16 C84 H84B 110.0 . . ? H84A C84 H84B 108.4 . . ? C90 C85 C86 118.6(4) . . ? C90 C85 C71 120.5(3) . . ? C86 C85 C71 120.9(3) . . ? C88 C89 C90 120.0(4) . . ? C88 C89 H89 120.0 . . ? C90 C89 H89 120.0 . . ? C89 C88 C87 120.2(4) . . ? C89 C88 H88 119.9 . . ? C87 C88 H88 119.9 . . ? C85 C90 C89 120.7(4) . . ? C85 C90 H90 119.6 . . ? C89 C90 H90 119.6 . . ? C87 C86 C85 120.8(4) . . ? C87 C86 H86 119.6 . . ? C85 C86 H86 119.6 . . ? C86 C87 C88 119.6(4) . . ? C86 C87 H87 120.2 . . ? C88 C87 H87 120.2 . . ? C92 C91 C96 119.3(4) . . ? C92 C91 C72 119.4(4) . . ? C96 C91 C72 121.3(3) . . ? C95 C96 C91 121.2(4) . . ? C95 C96 H96 119.4 . . ? C91 C96 H96 119.4 . . ? C94 C95 C96 119.4(4) . . ? C94 C95 H95 120.3 . . ? C96 C95 H95 120.3 . . ? C91 C92 C93 118.8(4) . . ? C91 C92 H92 120.6 . . ? C93 C92 H92 120.6 . . ? C95 C94 C93 121.0(4) . . ? C95 C94 H94 119.5 . . ? C93 C94 H94 119.5 . . ? C94 C93 C92 120.3(4) . . ? C94 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? C99 C98 C97 120.1(4) . . ? C99 C98 H98 119.9 . . ? C97 C98 H98 119.9 . . ? C102 C97 C98 118.6(4) . . ? C102 C97 C74 122.8(3) . . ? C98 C97 C74 118.6(3) . . ? C100 C99 C98 120.5(4) . . ? C100 C99 H99 119.8 . . ? C98 C99 H99 119.8 . . ? C101 C102 C97 121.0(4) . . ? C101 C102 H102 119.5 . . ? C97 C102 H102 119.5 . . ? C100 C101 C102 119.9(4) . . ? C100 C101 H101 120.1 . . ? C102 C101 H101 120.1 . . ? C99 C100 C101 119.9(4) . . ? C99 C100 H100 120.1 . . ? C101 C100 H100 120.1 . . ? C104 C103 C105 120.1(4) . . ? C104 C103 H103 120.0 . . ? C105 C103 H103 120.0 . . ? C106 C105 C103 118.6(4) . . ? C106 C105 C73 119.6(3) . . ? C103 C105 C73 121.5(3) . . ? C105 C106 C107 120.6(4) . . ? C105 C106 H106 119.7 . . ? C107 C106 H106 119.7 . . ? C104 C108 C107 120.4(4) . . ? C104 C108 H108 119.8 . . ? C107 C108 H108 119.8 . . ? C108 C104 C103 120.7(4) . . ? C108 C104 H104 119.6 . . ? C103 C104 H104 119.6 . . ? C108 C107 C106 119.5(4) . . ? C108 C107 H107 120.2 . . ? C106 C107 H107 120.2 . . ? C109 C110 C111 120.1(4) . . ? C109 C110 H110 120.0 . . ? C111 C110 H110 120.0 . . ? C112 C111 C110 120.3(4) . . ? C112 C111 H111 119.9 . . ? C110 C111 H111 119.9 . . ? C112 C113 C114 119.6(4) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C110 C109 C114 119.4(3) . . ? C110 C109 C75 119.8(3) . . ? C114 C109 C75 120.8(3) . . ? C109 C114 C113 120.6(4) . . ? C109 C114 H114 119.7 . . ? C113 C114 H114 119.7 . . ? C111 C112 C113 120.1(4) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C115 C116 C117 119.5(4) . . ? C115 C116 H116 120.2 . . ? C117 C116 H116 120.2 . . ? C119 C118 C117 120.4(4) . . ? C119 C118 H118 119.8 . . ? C117 C118 H118 119.8 . . ? C116 C115 C120 119.4(3) . . ? C116 C115 C76 121.4(3) . . ? C120 C115 C76 119.2(3) . . ? C118 C117 C116 120.0(4) . . ? C118 C117 H117 120.0 . . ? C116 C117 H117 120.0 . . ? C119 C120 C115 119.9(4) . . ? C119 C120 H120 120.0 . . ? C115 C120 H120 120.0 . . ? C118 C119 C120 120.6(4) . . ? C118 C119 H119 119.7 . . ? C120 C119 H119 119.7 . . ? C122 C121 C126 118.8(4) . . ? C122 C121 C77 120.6(3) . . ? C126 C121 C77 120.6(3) . . ? C125 C126 C121 120.3(4) . . ? C125 C126 H126 119.9 . . ? C121 C126 H126 119.9 . . ? C123 C122 C121 121.0(4) . . ? C123 C122 H122 119.5 . . ? C121 C122 H122 119.5 . . ? C125 C124 C123 119.5(4) . . ? C125 C124 H124 120.3 . . ? C123 C124 H124 120.3 . . ? C122 C123 C124 119.8(4) . . ? C122 C123 H123 120.1 . . ? C124 C123 H123 120.1 . . ? C124 C125 C126 120.5(4) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? C132 C127 C128 118.4(4) . . ? C132 C127 C78 121.8(4) . . ? C128 C127 C78 119.8(4) . . ? C130 C129 C128 120.7(5) . . ? C130 C129 H129 119.7 . . ? C128 C129 H129 119.7 . . ? C127 C128 C129 118.4(5) . . ? C127 C128 H128 120.8 . . ? C129 C128 H128 120.8 . . ? C127 C132 C131 122.3(5) . . ? C127 C132 H132 118.8 . . ? C131 C132 H132 118.8 . . ? C131 C130 C129 120.8(5) . . ? C131 C130 H130 119.6 . . ? C129 C130 H130 119.6 . . ? C130 C131 C132 119.4(6) . . ? C130 C131 H131 120.3 . . ? C132 C131 H131 120.3 . . ? C67 N9 C72 111.4(3) . . ? C67 N9 C81 121.5(3) . . ? C72 N9 C81 127.1(3) . . ? C67 N10 C71 111.6(3) . . ? C67 N10 C79 128.3(3) . . ? C71 N10 C79 119.8(3) . . ? C68 N11 C74 111.6(3) . . ? C68 N11 C81 117.8(3) . . ? C74 N11 C81 129.9(3) . . ? C68 N12 C73 111.6(3) . . ? C68 N12 C82 121.0(3) . . ? C73 N12 C82 127.4(3) . . ? C69 N13 C76 111.7(3) . . ? C69 N13 C84 121.1(3) . . ? C76 N13 C84 126.9(3) . . ? C69 N14 C75 111.2(3) . . ? C69 N14 C83 128.0(3) . . ? C75 N14 C83 120.3(3) . . ? C70 N16 C77 112.5(3) . . ? C70 N16 C84 117.0(3) . . ? C77 N16 C84 128.6(3) . . ? C70 N15 C78 111.2(3) . . ? C70 N15 C80 120.7(3) . . ? C78 N15 C80 128.1(3) . . ? O3 S1 O1 114.8(2) . . ? O3 S1 O2 116.8(2) . . ? O1 S1 O2 115.0(2) . . ? O3 S1 C133 102.1(2) . . ? O1 S1 C133 103.77(18) . . ? O2 S1 C133 101.3(2) . . ? F2 C133 F1 107.4(3) . . ? F2 C133 F3 105.5(3) . . ? F1 C133 F3 105.2(3) . . ? F2 C133 S1 112.8(3) . . ? F1 C133 S1 112.8(3) . . ? F3 C133 S1 112.6(3) . . ? O8 S3 O7 120.1(3) . . ? O8 S3 O9 113.0(4) . . ? O7 S3 O9 109.4(3) . . ? O8 S3 C135 108.1(3) . . ? O7 S3 C135 106.8(2) . . ? O9 S3 C135 96.6(3) . . ? F8 C135 F7 108.8(5) . . ? F8 C135 F9 106.3(5) . . ? F7 C135 F9 108.0(4) . . ? F8 C135 S3 115.0(4) . . ? F7 C135 S3 113.0(4) . . ? F9 C135 S3 105.4(4) . . ? O10 S4 O11 113.3(3) . . ? O10 S4 O12 113.5(3) . . ? O11 S4 O12 116.8(3) . . ? O10 S4 C136 100.9(4) . . ? O11 S4 C136 104.0(3) . . ? O12 S4 C136 106.1(3) . . ? F10 C136 F12 107.5(7) . . ? F10 C136 F11 109.2(8) . . ? F12 C136 F11 106.1(7) . . ? F10 C136 S4 110.9(5) . . ? F12 C136 S4 111.0(8) . . ? F11 C136 S4 111.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.116 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.078 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.799 -0.050 0.048 50.2 -1.4 2 -0.043 -0.003 0.457 3223.8 619.7 3 0.201 0.050 0.952 50.3 -1.2 4 0.701 0.450 0.452 50.2 -1.3 5 0.299 0.550 0.548 50.2 -1.2 _platon_squeeze_details ; ? ; data_7 _database_code_depnum_ccdc_archive 'CCDC 888978' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H52 F6 I2 N8 P Rh' _chemical_formula_weight 1458.84 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.646(5) _cell_length_b 13.785(6) _cell_length_c 18.779(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.702(5) _cell_angle_gamma 90.00 _cell_volume 3273(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9502 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'BRUKER APEX II CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25850 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.1666 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 23.43 _reflns_number_total 9456 _reflns_number_gt 5913 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The poor crystal data prevent most of the atoms from being refinied aniso- tropically. Attempts to obtain better crystal were failed. ; _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^)+(0.1682P)^2^+41.0809P] 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 0.00(7) _refine_ls_number_reflns 9456 _refine_ls_number_parameters 311 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1692 _refine_ls_R_factor_gt 0.1127 _refine_ls_wR_factor_ref 0.3143 _refine_ls_wR_factor_gt 0.2865 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.171 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C50 C 0.3544(10) -0.0482(12) 0.0954(8) 0.027(6) Uiso 1 1 d G . . C52 C 0.3118(13) -0.0349(13) 0.1626(8) 0.032(7) Uiso 1 1 d G . . H52 H 0.3511 -0.0014 0.1984 0.039 Uiso 1 1 calc R . . C64 C 0.2116(14) -0.0706(15) 0.1774(7) 0.066(10) Uiso 1 1 d G . . H64 H 0.1825 -0.0615 0.2233 0.079 Uiso 1 1 calc R . . C63 C 0.1542(11) -0.1196(15) 0.1251(10) 0.047(8) Uiso 1 1 d G . . H63 H 0.0857 -0.1440 0.1353 0.056 Uiso 1 1 calc R . . C62 C 0.1968(12) -0.1328(13) 0.0580(8) 0.039(7) Uiso 1 1 d G . . H62 H 0.1576 -0.1663 0.0222 0.047 Uiso 1 1 calc R . . C51 C 0.2970(12) -0.0971(12) 0.0431(7) 0.017(5) Uiso 1 1 d G . . H51 H 0.3261 -0.1062 -0.0028 0.020 Uiso 1 1 calc R . . C21 C 0.8625(19) 0.0370(18) 0.4055(13) 0.047(8) Uiso 1 1 d G . . C55 C 0.833(2) 0.1151(18) 0.4476(17) 0.100(15) Uiso 1 1 d G . . H55 H 0.7770 0.1565 0.4325 0.119 Uiso 1 1 calc R . . C61 C 0.885(3) 0.133(2) 0.5119(16) 0.111(17) Uiso 1 1 d G . . H61 H 0.8651 0.1859 0.5407 0.133 Uiso 1 1 calc R . . C66 C 0.967(3) 0.072(3) 0.5340(14) 0.17(3) Uiso 1 1 d G . . H66 H 1.0029 0.0839 0.5779 0.199 Uiso 1 1 calc R . . C57 C 0.997(2) -0.006(3) 0.4918(18) 0.13(2) Uiso 1 1 d G . . H57 H 1.0527 -0.0476 0.5069 0.160 Uiso 1 1 calc R . . C56 C 0.944(2) -0.0236(17) 0.4276(16) 0.067(11) Uiso 1 1 d G . . H56 H 0.9646 -0.0770 0.3987 0.080 Uiso 1 1 calc R . . C1 C 0.8202(18) 0.1092(17) 0.0042(12) 0.017(5) Uiso 1 1 d . . . C2 C 0.6360(18) 0.0414(16) 0.0833(12) 0.014(5) Uiso 1 1 d . . . C3 C 0.772(2) 0.0382(19) 0.2109(14) 0.027(6) Uiso 1 1 d . . . C4 C 0.9420(18) 0.1447(17) 0.1505(13) 0.014(5) Uiso 1 1 d . . . C5 C 1.0409(17) 0.1722(16) 0.0367(11) 0.013(5) Uiso 1 1 d . . . H5A H 1.1167 0.1850 0.0281 0.016 Uiso 1 1 calc R . . H5B H 1.0009 0.2260 0.0142 0.016 Uiso 1 1 calc R . . C6 C 1.0122(18) 0.0799(18) -0.0046(12) 0.022(5) Uiso 1 1 d . . . H6A H 1.0632 0.0706 -0.0436 0.027 Uiso 1 1 calc R . . H6B H 1.0176 0.0233 0.0277 0.027 Uiso 1 1 calc R . . C7 C 0.6319(15) 0.1477(15) -0.0279(11) 0.006(5) Uiso 1 1 d . . . H7A H 0.6292 0.2129 -0.0059 0.007 Uiso 1 1 calc R . . H7B H 0.5894 0.1496 -0.0726 0.007 Uiso 1 1 calc R . . C8 C 0.5584(15) -0.0583(15) 0.1799(11) 0.008(5) Uiso 1 1 d . . . H8A H 0.5008 -0.1069 0.1784 0.009 Uiso 1 1 calc R . . H8B H 0.5429 -0.0129 0.2192 0.009 Uiso 1 1 calc R . . C9 C 0.6602(18) -0.1106(17) 0.1982(13) 0.022(6) Uiso 1 1 d . . . H9A H 0.6452 -0.1715 0.2241 0.027 Uiso 1 1 calc R . . H9B H 0.6992 -0.1267 0.1543 0.027 Uiso 1 1 calc R . . C10 C 0.8786(17) 0.1672(16) 0.2693(12) 0.015(5) Uiso 1 1 d . . . H10A H 0.8276 0.2203 0.2602 0.018 Uiso 1 1 calc R . . H10B H 0.9140 0.1801 0.3156 0.018 Uiso 1 1 calc R . . C11 C 0.8829(16) 0.0814(17) -0.1072(11) 0.013(5) Uiso 1 1 d . . . C12 C 0.7789(15) 0.1082(15) -0.1174(11) 0.008(5) Uiso 1 1 d . . . C13 C 0.7490(17) -0.0574(16) 0.3155(12) 0.014(5) Uiso 1 1 d . . . C14 C 0.8105(18) 0.0139(17) 0.3317(13) 0.020(6) Uiso 1 1 d . . . C15 C 1.0581(18) 0.2042(16) 0.2261(12) 0.015(5) Uiso 1 1 d . . . C16 C 1.0954(16) 0.2166(15) 0.1580(11) 0.010(5) Uiso 1 1 d . . . C17 C 0.7048(18) -0.1418(17) 0.3553(13) 0.020(6) Uiso 1 1 d . . . C18 C 0.6267(15) -0.1339(16) 0.4004(10) 0.052(9) Uiso 1 1 d . . . H18 H 0.5970 -0.0711 0.4064 0.062 Uiso 1 1 calc R . . C19 C 0.7513(15) -0.2353(16) 0.3489(10) 0.059(9) Uiso 1 1 d R . . H19 H 0.8032 -0.2459 0.3136 0.070 Uiso 1 1 d R . . C20 C 0.7245(15) -0.3029(16) 0.3872(10) 0.054(9) Uiso 1 1 d R . . H20 H 0.7700 -0.3569 0.3945 0.065 Uiso 1 1 d R . . C22 C 1.103(2) 0.241(2) 0.2999(15) 0.041(7) Uiso 1 1 d . . . C23 C 1.2033(17) 0.2552(18) 0.1392(12) 0.018(5) Uiso 1 1 d . . . C24 C 1.295(2) 0.212(2) 0.1753(16) 0.038(7) Uiso 1 1 d . . . H24 H 1.2878 0.1635 0.2107 0.046 Uiso 1 1 calc R . . C25 C 0.7056(18) 0.1061(17) -0.1808(13) 0.020(6) Uiso 1 1 d . . . C26 C 0.664(2) 0.197(2) -0.2001(15) 0.034(7) Uiso 1 1 d . . . H26 H 0.6800 0.2556 -0.1756 0.041 Uiso 1 1 calc R . . C27 C 0.9517(19) 0.0612(18) -0.1617(13) 0.025(6) Uiso 1 1 d . . . C28 C 1.0257(16) -0.0182(15) -0.1643(12) 0.011(5) Uiso 1 1 d . . . H28 H 1.0332 -0.0577 -0.1231 0.013 Uiso 1 1 calc R . . C29 C 0.698(2) 0.0233(19) -0.2180(14) 0.026(6) Uiso 1 1 d . . . H29 H 0.7329 -0.0347 -0.2036 0.031 Uiso 1 1 calc R . . C30 C 0.592(3) 0.191(3) -0.2629(18) 0.058(10) Uiso 1 1 d . . . H30 H 0.5503 0.2462 -0.2753 0.069 Uiso 1 1 calc R . . C31 C 0.5845(16) 0.1097(15) -0.3031(11) 0.033(7) Uiso 1 1 d . . . H31 H 0.5445 0.1115 -0.3462 0.040 Uiso 1 1 calc R . . C32 C 0.5823(16) -0.2105(15) 0.4413(11) 0.047(8) Uiso 1 1 d R . . H32 H 0.5323 -0.1999 0.4779 0.056 Uiso 1 1 d R . . C33 C 1.3958(19) 0.2487(19) 0.1536(13) 0.027(6) Uiso 1 1 d . . . H33 H 1.4575 0.2268 0.1781 0.033 Uiso 1 1 calc R . . C34 C 0.958(3) 0.118(2) -0.2252(17) 0.050(9) Uiso 1 1 d . . . H34 H 0.9113 0.1721 -0.2291 0.060 Uiso 1 1 calc R . . C35 C 0.4535(18) -0.0033(16) 0.0729(12) 0.016(5) Uiso 1 1 d . . . C36 C 0.4784(19) 0.0456(17) 0.0114(13) 0.018(6) Uiso 1 1 d . . . C37 C 0.4147(17) 0.0815(18) -0.0496(11) 0.017(5) Uiso 1 1 d . . . C38 C 1.123(2) 0.340(2) 0.3087(16) 0.035(7) Uiso 1 1 d . . . H38 H 1.1028 0.3852 0.2733 0.042 Uiso 1 1 calc R . . C39 C 1.407(2) 0.3185(17) 0.0951(13) 0.024(6) Uiso 1 1 d . . . H39 H 1.4754 0.3365 0.0786 0.028 Uiso 1 1 calc R . . C40 C 1.082(2) -0.039(2) -0.2188(16) 0.045(8) Uiso 1 1 d . . . H40 H 1.1204 -0.0984 -0.2154 0.054 Uiso 1 1 calc R . . C41 C 1.025(2) 0.101(2) -0.2821(15) 0.036(7) Uiso 1 1 d . . . H41 H 1.0275 0.1455 -0.3209 0.044 Uiso 1 1 calc R . . C42 C 1.096(2) 0.012(2) -0.2815(17) 0.046(8) Uiso 1 1 d . . . H42 H 1.1420 -0.0065 -0.3186 0.055 Uiso 1 1 calc R . . C43 C 1.174(3) 0.369(3) 0.370(2) 0.080(12) Uiso 1 1 d . . . H43 H 1.1969 0.4336 0.3766 0.096 Uiso 1 1 calc R . . C44 C 0.323(2) 0.1386(18) -0.0328(15) 0.029(6) Uiso 1 1 d . . . H44 H 0.3083 0.1564 0.0150 0.035 Uiso 1 1 calc R . . C45 C 0.251(2) 0.1685(18) -0.0916(13) 0.026(6) Uiso 1 1 d . . . H45 H 0.1928 0.2108 -0.0864 0.032 Uiso 1 1 calc R . . C46 C 0.2833(15) 0.1240(13) -0.1598(11) 0.004(4) Uiso 1 1 d . . . H46 H 0.2422 0.1418 -0.2005 0.005 Uiso 1 1 calc R . . C47 C 0.365(2) 0.060(2) -0.1717(17) 0.045(8) Uiso 1 1 d . . . H47 H 0.3757 0.0325 -0.2174 0.054 Uiso 1 1 calc R . . C48 C 1.2153(15) 0.3227(14) 0.0868(10) 0.012(5) Uiso 1 1 d . . . H48 H 1.1535 0.3476 0.0641 0.014 Uiso 1 1 calc R . . C49 C 0.6171(15) -0.3011(14) 0.4226(10) 0.077(12) Uiso 1 1 d R . . H49 H 0.5772 -0.3582 0.4312 0.093 Uiso 1 1 d R . . C53 C 1.115(2) 0.173(2) 0.3486(16) 0.044(8) Uiso 1 1 d . . . H53 H 1.0967 0.1072 0.3398 0.053 Uiso 1 1 calc R . . C54 C 1.315(2) 0.358(2) 0.0641(15) 0.033(7) Uiso 1 1 d . . . H54 H 1.3198 0.4070 0.0288 0.040 Uiso 1 1 calc R . . C60 C 0.630(3) 0.029(3) -0.2843(19) 0.060(10) Uiso 1 1 d . . . H60 H 0.6212 -0.0270 -0.3129 0.072 Uiso 1 1 calc R . . C65 C 0.426(2) 0.0395(19) -0.1180(14) 0.027(6) Uiso 1 1 d . . . H65 H 0.4815 -0.0060 -0.1249 0.032 Uiso 1 1 calc R . . C67 C 1.162(4) 0.205(4) 0.419(3) 0.111(17) Uiso 1 1 d . . . H67 H 1.1686 0.1607 0.4579 0.133 Uiso 1 1 calc R . . C68 C 1.190(3) 0.291(3) 0.426(2) 0.083(13) Uiso 1 1 d . . . H68 H 1.2247 0.3095 0.4687 0.100 Uiso 1 1 calc R . . N1 N 0.9051(12) 0.0853(13) -0.0345(8) 0.008(4) Uiso 1 1 d . . . N2 N 0.7431(14) 0.1236(13) -0.0448(10) 0.014(4) Uiso 1 1 d . . . N3 N 0.5864(13) 0.0780(13) 0.0199(9) 0.012(4) Uiso 1 1 d . . . N4 N 0.5546(14) -0.0038(13) 0.1133(10) 0.013(4) Uiso 1 1 d . . . N5 N 0.7208(15) -0.0456(14) 0.2422(10) 0.021(5) Uiso 1 1 d . . . N6 N 0.8202(15) 0.0742(15) 0.2739(10) 0.022(5) Uiso 1 1 d . . . N7 N 0.9531(15) 0.1676(14) 0.2167(11) 0.022(5) Uiso 1 1 d . . . N8 N 1.0259(14) 0.1799(13) 0.1106(10) 0.011(4) Uiso 1 1 d . . . F1 F 0.351(2) 0.8050(18) 0.5415(11) 0.115(9) Uiso 1 1 d D . . F2 F 0.2085(19) 0.857(3) 0.611(2) 0.22(2) Uiso 1 1 d D . . F3 F 0.460(2) 0.888(3) 0.607(2) 0.24(2) Uiso 1 1 d D . . F4 F 0.345(3) 0.779(2) 0.6562(17) 0.23(2) Uiso 1 1 d D . . F5 F 0.330(3) 0.948(3) 0.6700(18) 0.25(2) Uiso 1 1 d D . . F6 F 0.313(4) 0.963(3) 0.555(2) 0.43(6) Uiso 1 1 d D . . P1 P 0.3342(16) 0.8726(13) 0.6069(11) 0.183(10) Uani 1 1 d D . . Rh1 Rh 0.79028(14) 0.08486(14) 0.11355(9) 0.0077(4) Uiso 1 1 d . . . I1 I 0.87713(12) -0.08731(11) 0.09544(11) 0.0348(4) Uani 1 1 d U . . I2 I 0.70935(12) 0.26064(10) 0.13729(11) 0.0348(4) 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 P1 0.19(2) 0.129(16) 0.23(3) -0.118(18) 0.013(18) -0.007(14) I1 0.0133(5) 0.0213(6) 0.0694(9) -0.0083(6) -0.0089(5) 0.0050(5) I2 0.0133(5) 0.0213(6) 0.0694(9) -0.0083(6) -0.0089(5) 0.0050(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 C50 C52 1.3900 . ? C50 C51 1.3900 . ? C50 C35 1.46(3) . ? C52 C64 1.3900 . ? C52 H52 0.9500 . ? C64 C63 1.3900 . ? C64 H64 0.9500 . ? C63 C62 1.3900 . ? C63 H63 0.9500 . ? C62 C51 1.3900 . ? C62 H62 0.9500 . ? C51 H51 0.9500 . ? C21 C55 1.3900 . ? C21 C56 1.3900 . ? C21 C14 1.56(3) . ? C55 C61 1.3900 . ? C55 H55 0.9500 . ? C61 C66 1.3900 . ? C61 H61 0.9500 . ? C66 C57 1.3900 . ? C66 H66 0.9500 . ? C57 C56 1.3900 . ? C57 H57 0.9500 . ? C56 H56 0.9500 . ? C1 N1 1.34(3) . ? C1 N2 1.35(3) . ? C1 Rh1 2.12(2) . ? C2 N4 1.33(3) . ? C2 N3 1.43(3) . ? C2 Rh1 2.11(2) . ? C3 N6 1.41(3) . ? C3 N5 1.45(3) . ? C3 Rh1 1.95(3) . ? C4 N7 1.29(3) . ? C4 N8 1.39(3) . ? C4 Rh1 2.19(2) . ? C5 N8 1.41(3) . ? C5 C6 1.53(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.46(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N3 1.44(3) . ? C7 N2 1.48(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.46(3) . ? C8 C9 1.51(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N5 1.44(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N7 1.37(3) . ? C10 N6 1.48(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.38(3) . ? C11 C27 1.38(3) . ? C11 N1 1.39(3) . ? C12 N2 1.46(3) . ? C12 C25 1.50(3) . ? C13 C14 1.29(3) . ? C13 N5 1.43(3) . ? C13 C17 1.50(3) . ? C14 N6 1.37(3) . ? C15 C16 1.38(3) . ? C15 N7 1.43(3) . ? C15 C22 1.57(4) . ? C16 N8 1.34(3) . ? C16 C23 1.51(3) . ? C17 C18 1.31(3) . ? C17 C19 1.42(3) . ? C18 C32 1.42(3) . ? C18 H18 0.9500 . ? C19 C20 1.2268 . ? C19 H19 0.9500 . ? C20 C49 1.52(3) . ? C20 H20 0.9500 . ? C22 C53 1.32(4) . ? C22 C38 1.40(4) . ? C23 C48 1.36(3) . ? C23 C24 1.46(4) . ? C24 C33 1.44(4) . ? C24 H24 0.9500 . ? C25 C29 1.34(3) . ? C25 C26 1.41(4) . ? C26 C30 1.48(4) . ? C26 H26 0.9500 . ? C27 C34 1.43(4) . ? C27 C28 1.44(3) . ? C28 C40 1.29(4) . ? C28 H28 0.9500 . ? C29 C60 1.50(4) . ? C29 H29 0.9500 . ? C30 C31 1.36(4) . ? C30 H30 0.9500 . ? C31 C60 1.30(4) . ? C31 H31 0.9500 . ? C32 C49 1.37(3) . ? C32 H32 0.9500 . ? C33 C39 1.47(3) . ? C33 H33 0.9500 . ? C34 C41 1.40(4) . ? C34 H34 0.9500 . ? C35 C36 1.38(3) . ? C35 N4 1.48(3) . ? C36 N3 1.44(3) . ? C36 C37 1.48(3) . ? C37 C65 1.42(3) . ? C37 C44 1.44(3) . ? C38 C43 1.36(5) . ? C38 H38 0.9500 . ? C39 C54 1.40(4) . ? C39 H39 0.9500 . ? C40 C42 1.38(4) . ? C40 H40 0.9500 . ? C41 C42 1.52(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C68 1.51(6) . ? C43 H43 0.9500 . ? C44 C45 1.48(4) . ? C44 H44 0.9500 . ? C45 C46 1.48(3) . ? C45 H45 0.9500 . ? C46 C47 1.38(3) . ? C46 H46 0.9500 . ? C47 C65 1.30(4) . ? C47 H47 0.9500 . ? C48 C54 1.43(3) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C53 C67 1.51(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C60 H60 0.9500 . ? C65 H65 0.9500 . ? C67 C68 1.25(6) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? F1 P1 1.558(16) . ? F2 P1 1.607(17) . ? F3 P1 1.603(18) . ? F4 P1 1.592(18) . ? F5 P1 1.575(18) . ? F6 P1 1.592(18) . ? Rh1 I1 2.639(3) . ? Rh1 I2 2.670(3) . ? 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 C52 C50 C51 120.0 . . ? C52 C50 C35 123.4(14) . . ? C51 C50 C35 116.3(14) . . ? C50 C52 C64 120.0 . . ? C50 C52 H52 120.0 . . ? C64 C52 H52 120.0 . . ? C63 C64 C52 120.0 . . ? C63 C64 H64 120.0 . . ? C52 C64 H64 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C51 C62 C63 120.0 . . ? C51 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C51 C50 120.0 . . ? C62 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C55 C21 C56 120.0 . . ? C55 C21 C14 123.4(19) . . ? C56 C21 C14 116.5(19) . . ? C61 C55 C21 120.0 . . ? C61 C55 H55 120.0 . . ? C21 C55 H55 120.0 . . ? C55 C61 C66 120.0 . . ? C55 C61 H61 120.0 . . ? C66 C61 H61 120.0 . . ? C57 C66 C61 120.0 . . ? C57 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C56 C57 C66 120.0 . . ? C56 C57 H57 120.0 . . ? C66 C57 H57 120.0 . . ? C57 C56 C21 120.0 . . ? C57 C56 H56 120.0 . . ? C21 C56 H56 120.0 . . ? N1 C1 N2 104.0(19) . . ? N1 C1 Rh1 129.7(16) . . ? N2 C1 Rh1 123.3(16) . . ? N4 C2 N3 100.5(18) . . ? N4 C2 Rh1 137.2(17) . . ? N3 C2 Rh1 121.2(15) . . ? N6 C3 N5 97.5(19) . . ? N6 C3 Rh1 127.8(18) . . ? N5 C3 Rh1 134.3(18) . . ? N7 C4 N8 111(2) . . ? N7 C4 Rh1 118.9(16) . . ? N8 C4 Rh1 129.0(17) . . ? N8 C5 C6 121.9(19) . . ? N8 C5 H5A 106.8 . . ? C6 C5 H5A 106.8 . . ? N8 C5 H5B 106.8 . . ? C6 C5 H5B 106.8 . . ? H5A C5 H5B 106.7 . . ? N1 C6 C5 111.4(19) . . ? N1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N1 C6 H6B 109.4 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N3 C7 N2 111.8(16) . . ? N3 C7 H7A 109.3 . . ? N2 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 . . ? N2 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N4 C8 C9 117.4(18) . . ? N4 C8 H8A 107.9 . . ? C9 C8 H8A 107.9 . . ? N4 C8 H8B 107.9 . . ? C9 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? N5 C9 C8 106.3(18) . . ? N5 C9 H9A 110.5 . . ? C8 C9 H9A 110.5 . . ? N5 C9 H9B 110.5 . . ? C8 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? N7 C10 N6 113.2(19) . . ? N7 C10 H10A 108.9 . . ? N6 C10 H10A 108.9 . . ? N7 C10 H10B 108.9 . . ? N6 C10 H10B 108.9 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C27 124(2) . . ? C12 C11 N1 107.9(17) . . ? C27 C11 N1 128(2) . . ? C11 C12 N2 102.4(17) . . ? C11 C12 C25 133.3(19) . . ? N2 C12 C25 123.3(18) . . ? C14 C13 N5 107(2) . . ? C14 C13 C17 135(2) . . ? N5 C13 C17 118.7(19) . . ? C13 C14 N6 110(2) . . ? C13 C14 C21 128(2) . . ? N6 C14 C21 122(2) . . ? C16 C15 N7 104.9(19) . . ? C16 C15 C22 131(2) . . ? N7 C15 C22 123(2) . . ? N8 C16 C15 109.9(19) . . ? N8 C16 C23 124.3(19) . . ? C15 C16 C23 125(2) . . ? C18 C17 C19 116(2) . . ? C18 C17 C13 123(2) . . ? C19 C17 C13 120.3(19) . . ? C17 C18 C32 126(2) . . ? C17 C18 H18 116.9 . . ? C32 C18 H18 116.9 . . ? C20 C19 C17 121.4(13) . . ? C20 C19 H19 119.3 . . ? C17 C19 H19 119.3 . . ? C19 C20 C49 119.9(11) . . ? C19 C20 H20 120.6 . . ? C49 C20 H20 119.5 . . ? C53 C22 C38 126(3) . . ? C53 C22 C15 115(3) . . ? C38 C22 C15 119(3) . . ? C48 C23 C24 121(2) . . ? C48 C23 C16 121.2(19) . . ? C24 C23 C16 117(2) . . ? C33 C24 C23 115(2) . . ? C33 C24 H24 122.3 . . ? C23 C24 H24 122.3 . . ? C29 C25 C26 127(2) . . ? C29 C25 C12 118(2) . . ? C26 C25 C12 114(2) . . ? C25 C26 C30 113(3) . . ? C25 C26 H26 123.7 . . ? C30 C26 H26 123.7 . . ? C11 C27 C34 123(2) . . ? C11 C27 C28 126(2) . . ? C34 C27 C28 110(2) . . ? C40 C28 C27 124(2) . . ? C40 C28 H28 117.9 . . ? C27 C28 H28 117.9 . . ? C25 C29 C60 115(3) . . ? C25 C29 H29 122.5 . . ? C60 C29 H29 122.5 . . ? C31 C30 C26 122(3) . . ? C31 C30 H30 119.2 . . ? C26 C30 H30 119.2 . . ? C60 C31 C30 122(3) . . ? C60 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C49 C32 C18 114.0(18) . . ? C49 C32 H32 122.9 . . ? C18 C32 H32 123.0 . . ? C24 C33 C39 123(2) . . ? C24 C33 H33 118.7 . . ? C39 C33 H33 118.7 . . ? C41 C34 C27 126(3) . . ? C41 C34 H34 117.0 . . ? C27 C34 H34 117.0 . . ? C36 C35 C50 131(2) . . ? C36 C35 N4 103.2(19) . . ? C50 C35 N4 125.9(19) . . ? C35 C36 N3 107(2) . . ? C35 C36 C37 133(2) . . ? N3 C36 C37 119.2(19) . . ? C65 C37 C44 121(2) . . ? C65 C37 C36 120(2) . . ? C44 C37 C36 116(2) . . ? C43 C38 C22 118(3) . . ? C43 C38 H38 120.9 . . ? C22 C38 H38 120.9 . . ? C54 C39 C33 118(2) . . ? C54 C39 H39 120.9 . . ? C33 C39 H39 120.9 . . ? C28 C40 C42 130(3) . . ? C28 C40 H40 115.2 . . ? C42 C40 H40 115.2 . . ? C34 C41 C42 119(3) . . ? C34 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C40 C42 C41 110(3) . . ? C40 C42 H42 125.1 . . ? C41 C42 H42 125.1 . . ? C38 C43 C68 116(4) . . ? C38 C43 H43 122.1 . . ? C68 C43 H43 122.1 . . ? C37 C44 C45 118(2) . . ? C37 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? C44 C45 C46 111(2) . . ? C44 C45 H45 124.4 . . ? C46 C45 H45 124.4 . . ? C47 C46 C45 128(2) . . ? C47 C46 H46 116.0 . . ? C45 C46 H46 116.0 . . ? C65 C47 C46 117(3) . . ? C65 C47 H47 121.4 . . ? C46 C47 H47 121.4 . . ? C23 C48 C54 124(2) . . ? C23 C48 H48 118.2 . . ? C54 C48 H48 118.2 . . ? C32 C49 C20 114.8(17) . . ? C32 C49 H49 122.6 . . ? C20 C49 H49 122.7 . . ? C22 C53 C67 117(3) . . ? C22 C53 H53 121.7 . . ? C67 C53 H53 121.7 . . ? C39 C54 C48 119(2) . . ? C39 C54 H54 120.7 . . ? C48 C54 H54 120.7 . . ? C31 C60 C29 121(3) . . ? C31 C60 H60 119.4 . . ? C29 C60 H60 119.4 . . ? C47 C65 C37 123(3) . . ? C47 C65 H65 118.4 . . ? C37 C65 H65 118.4 . . ? C68 C67 C53 118(5) . . ? C68 C67 H67 121.0 . . ? C53 C67 H67 121.0 . . ? C67 C68 C43 125(5) . . ? C67 C68 H68 117.6 . . ? C43 C68 H68 117.6 . . ? C1 N1 C11 112.8(17) . . ? C1 N1 C6 123.2(17) . . ? C11 N1 C6 123.4(16) . . ? C1 N2 C12 112.8(18) . . ? C1 N2 C7 124.5(18) . . ? C12 N2 C7 122.6(17) . . ? C2 N3 C7 125.4(17) . . ? C2 N3 C36 112.8(17) . . ? C7 N3 C36 121.4(17) . . ? C2 N4 C8 125.8(19) . . ? C2 N4 C35 116.6(19) . . ? C8 N4 C35 117.5(17) . . ? C13 N5 C9 127.6(19) . . ? C13 N5 C3 111.9(18) . . ? C9 N5 C3 120(2) . . ? C14 N6 C3 114(2) . . ? C14 N6 C10 128.2(19) . . ? C3 N6 C10 117.7(19) . . ? C4 N7 C10 129(2) . . ? C4 N7 C15 107.2(19) . . ? C10 N7 C15 124(2) . . ? C16 N8 C4 105.7(19) . . ? C16 N8 C5 126.0(18) . . ? C4 N8 C5 128.1(19) . . ? F1 P1 F5 173.0(18) . . ? F1 P1 F6 90.6(17) . . ? F5 P1 F6 86.4(17) . . ? F1 P1 F4 87.9(15) . . ? F5 P1 F4 95.6(17) . . ? F6 P1 F4 175(2) . . ? F1 P1 F3 86.3(15) . . ? F5 P1 F3 87.5(16) . . ? F6 P1 F3 93.2(18) . . ? F4 P1 F3 91.6(17) . . ? F1 P1 F2 95.9(16) . . ? F5 P1 F2 90.4(16) . . ? F6 P1 F2 88.6(17) . . ? F4 P1 F2 86.7(16) . . ? F3 P1 F2 177(2) . . ? C3 Rh1 C2 92.3(10) . . ? C3 Rh1 C1 169.4(10) . . ? C2 Rh1 C1 87.7(9) . . ? C3 Rh1 C4 86.6(10) . . ? C2 Rh1 C4 173.4(10) . . ? C1 Rh1 C4 94.7(9) . . ? C3 Rh1 I1 83.0(8) . . ? C2 Rh1 I1 95.5(6) . . ? C1 Rh1 I1 86.4(6) . . ? C4 Rh1 I1 90.9(6) . . ? C3 Rh1 I2 95.3(8) . . ? C2 Rh1 I2 87.0(6) . . ? C1 Rh1 I2 95.3(6) . . ? C4 Rh1 I2 86.6(6) . . ? I1 Rh1 I2 177.09(9) . . ? 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 C51 C50 C52 C64 0.0 . . . . ? C35 C50 C52 C64 172.6(19) . . . . ? C50 C52 C64 C63 0.0 . . . . ? C52 C64 C63 C62 0.0 . . . . ? C64 C63 C62 C51 0.0 . . . . ? C63 C62 C51 C50 0.0 . . . . ? C52 C50 C51 C62 0.0 . . . . ? C35 C50 C51 C62 -173.1(18) . . . . ? C56 C21 C55 C61 0.0 . . . . ? C14 C21 C55 C61 -178(3) . . . . ? C21 C55 C61 C66 0.0 . . . . ? C55 C61 C66 C57 0.0 . . . . ? C61 C66 C57 C56 0.0 . . . . ? C66 C57 C56 C21 0.0 . . . . ? C55 C21 C56 C57 0.0 . . . . ? C14 C21 C56 C57 178(2) . . . . ? N8 C5 C6 N1 93(2) . . . . ? N4 C8 C9 N5 94(2) . . . . ? C27 C11 C12 N2 -178(2) . . . . ? N1 C11 C12 N2 -2(2) . . . . ? C27 C11 C12 C25 13(4) . . . . ? N1 C11 C12 C25 -171(2) . . . . ? N5 C13 C14 N6 3(3) . . . . ? C17 C13 C14 N6 -177(2) . . . . ? N5 C13 C14 C21 179(2) . . . . ? C17 C13 C14 C21 -1(4) . . . . ? C55 C21 C14 C13 -110(3) . . . . ? C56 C21 C14 C13 72(3) . . . . ? C55 C21 C14 N6 66(3) . . . . ? C56 C21 C14 N6 -112(2) . . . . ? N7 C15 C16 N8 -7(2) . . . . ? C22 C15 C16 N8 -174(2) . . . . ? N7 C15 C16 C23 179(2) . . . . ? C22 C15 C16 C23 12(4) . . . . ? C14 C13 C17 C18 76(4) . . . . ? N5 C13 C17 C18 -103(3) . . . . ? C14 C13 C17 C19 -100(3) . . . . ? N5 C13 C17 C19 81(3) . . . . ? C19 C17 C18 C32 -2(4) . . . . ? C13 C17 C18 C32 -178(2) . . . . ? C18 C17 C19 C20 -5(3) . . . . ? C13 C17 C19 C20 171.3(15) . . . . ? C17 C19 C20 C49 22.3(15) . . . . ? C16 C15 C22 C53 -127(3) . . . . ? N7 C15 C22 C53 67(3) . . . . ? C16 C15 C22 C38 54(4) . . . . ? N7 C15 C22 C38 -111(3) . . . . ? N8 C16 C23 C48 52(3) . . . . ? C15 C16 C23 C48 -135(2) . . . . ? N8 C16 C23 C24 -123(2) . . . . ? C15 C16 C23 C24 49(3) . . . . ? C48 C23 C24 C33 2(4) . . . . ? C16 C23 C24 C33 178(2) . . . . ? C11 C12 C25 C29 50(4) . . . . ? N2 C12 C25 C29 -117(2) . . . . ? C11 C12 C25 C26 -121(3) . . . . ? N2 C12 C25 C26 72(3) . . . . ? C29 C25 C26 C30 10(4) . . . . ? C12 C25 C26 C30 180(2) . . . . ? C12 C11 C27 C34 42(4) . . . . ? N1 C11 C27 C34 -133(3) . . . . ? C12 C11 C27 C28 -137(3) . . . . ? N1 C11 C27 C28 48(4) . . . . ? C11 C27 C28 C40 174(3) . . . . ? C34 C27 C28 C40 -5(4) . . . . ? C26 C25 C29 C60 -5(4) . . . . ? C12 C25 C29 C60 -175(2) . . . . ? C25 C26 C30 C31 -11(4) . . . . ? C26 C30 C31 C60 8(5) . . . . ? C17 C18 C32 C49 -9(3) . . . . ? C23 C24 C33 C39 -5(4) . . . . ? C11 C27 C34 C41 -180(3) . . . . ? C28 C27 C34 C41 -1(4) . . . . ? C52 C50 C35 C36 -133(2) . . . . ? C51 C50 C35 C36 40(3) . . . . ? C52 C50 C35 N4 49(3) . . . . ? C51 C50 C35 N4 -138.3(19) . . . . ? C50 C35 C36 N3 177(2) . . . . ? N4 C35 C36 N3 -5(2) . . . . ? C50 C35 C36 C37 9(4) . . . . ? N4 C35 C36 C37 -173(2) . . . . ? C35 C36 C37 C65 -113(3) . . . . ? N3 C36 C37 C65 80(3) . . . . ? C35 C36 C37 C44 50(4) . . . . ? N3 C36 C37 C44 -117(2) . . . . ? C53 C22 C38 C43 9(5) . . . . ? C15 C22 C38 C43 -172(3) . . . . ? C24 C33 C39 C54 6(4) . . . . ? C27 C28 C40 C42 8(5) . . . . ? C27 C34 C41 C42 4(5) . . . . ? C28 C40 C42 C41 -4(5) . . . . ? C34 C41 C42 C40 -3(4) . . . . ? C22 C38 C43 C68 -7(5) . . . . ? C65 C37 C44 C45 -12(4) . . . . ? C36 C37 C44 C45 -175(2) . . . . ? C37 C44 C45 C46 6(3) . . . . ? C44 C45 C46 C47 2(3) . . . . ? C45 C46 C47 C65 -4(4) . . . . ? C24 C23 C48 C54 -1(4) . . . . ? C16 C23 C48 C54 -177(2) . . . . ? C18 C32 C49 C20 25(2) . . . . ? C19 C20 C49 C32 -33(2) . . . . ? C38 C22 C53 C67 -3(5) . . . . ? C15 C22 C53 C67 178(3) . . . . ? C33 C39 C54 C48 -5(4) . . . . ? C23 C48 C54 C39 3(4) . . . . ? C30 C31 C60 C29 -2(5) . . . . ? C25 C29 C60 C31 1(4) . . . . ? C46 C47 C65 C37 -2(4) . . . . ? C44 C37 C65 C47 10(4) . . . . ? C36 C37 C65 C47 172(3) . . . . ? C22 C53 C67 C68 -4(6) . . . . ? C53 C67 C68 C43 5(8) . . . . ? C38 C43 C68 C67 0(7) . . . . ? N2 C1 N1 C11 -2(2) . . . . ? Rh1 C1 N1 C11 158.6(17) . . . . ? N2 C1 N1 C6 168.8(19) . . . . ? Rh1 C1 N1 C6 -31(3) . . . . ? C12 C11 N1 C1 3(3) . . . . ? C27 C11 N1 C1 179(2) . . . . ? C12 C11 N1 C6 -168(2) . . . . ? C27 C11 N1 C6 8(4) . . . . ? C5 C6 N1 C1 -51(3) . . . . ? C5 C6 N1 C11 119(2) . . . . ? N1 C1 N2 C12 0(2) . . . . ? Rh1 C1 N2 C12 -161.8(14) . . . . ? N1 C1 N2 C7 177.3(18) . . . . ? Rh1 C1 N2 C7 15(3) . . . . ? C11 C12 N2 C1 1(2) . . . . ? C25 C12 N2 C1 171(2) . . . . ? C11 C12 N2 C7 -175.8(18) . . . . ? C25 C12 N2 C7 -6(3) . . . . ? N3 C7 N2 C1 -55(3) . . . . ? N3 C7 N2 C12 122(2) . . . . ? N4 C2 N3 C7 168.6(19) . . . . ? Rh1 C2 N3 C7 -2(3) . . . . ? N4 C2 N3 C36 -5(2) . . . . ? Rh1 C2 N3 C36 -175.5(15) . . . . ? N2 C7 N3 C2 46(3) . . . . ? N2 C7 N3 C36 -140.5(19) . . . . ? C35 C36 N3 C2 6(3) . . . . ? C37 C36 N3 C2 176.8(19) . . . . ? C35 C36 N3 C7 -167.5(18) . . . . ? C37 C36 N3 C7 3(3) . . . . ? N3 C2 N4 C8 178.1(18) . . . . ? Rh1 C2 N4 C8 -14(4) . . . . ? N3 C2 N4 C35 2(2) . . . . ? Rh1 C2 N4 C35 170.0(18) . . . . ? C9 C8 N4 C2 -32(3) . . . . ? C9 C8 N4 C35 144(2) . . . . ? C36 C35 N4 C2 2(3) . . . . ? C50 C35 N4 C2 -180(2) . . . . ? C36 C35 N4 C8 -174.8(18) . . . . ? C50 C35 N4 C8 4(3) . . . . ? C14 C13 N5 C9 175(2) . . . . ? C17 C13 N5 C9 -6(3) . . . . ? C14 C13 N5 C3 2(3) . . . . ? C17 C13 N5 C3 -178.7(19) . . . . ? C8 C9 N5 C13 114(2) . . . . ? C8 C9 N5 C3 -74(3) . . . . ? N6 C3 N5 C13 -5(2) . . . . ? Rh1 C3 N5 C13 167.5(19) . . . . ? N6 C3 N5 C9 -178.8(19) . . . . ? Rh1 C3 N5 C9 -6(3) . . . . ? C13 C14 N6 C3 -7(3) . . . . ? C21 C14 N6 C3 177(2) . . . . ? C13 C14 N6 C10 177(2) . . . . ? C21 C14 N6 C10 1(4) . . . . ? N5 C3 N6 C14 7(2) . . . . ? Rh1 C3 N6 C14 -166.3(18) . . . . ? N5 C3 N6 C10 -176.1(18) . . . . ? Rh1 C3 N6 C10 10(3) . . . . ? N7 C10 N6 C14 123(2) . . . . ? N7 C10 N6 C3 -53(3) . . . . ? N8 C4 N7 C10 163(2) . . . . ? Rh1 C4 N7 C10 -6(3) . . . . ? N8 C4 N7 C15 -11(3) . . . . ? Rh1 C4 N7 C15 180.0(15) . . . . ? N6 C10 N7 C4 51(3) . . . . ? N6 C10 N7 C15 -135(2) . . . . ? C16 C15 N7 C4 11(2) . . . . ? C22 C15 N7 C4 180(2) . . . . ? C16 C15 N7 C10 -164(2) . . . . ? C22 C15 N7 C10 5(3) . . . . ? C15 C16 N8 C4 1(2) . . . . ? C23 C16 N8 C4 175(2) . . . . ? C15 C16 N8 C5 -174(2) . . . . ? C23 C16 N8 C5 -1(3) . . . . ? N7 C4 N8 C16 7(2) . . . . ? Rh1 C4 N8 C16 174.2(16) . . . . ? N7 C4 N8 C5 -178(2) . . . . ? Rh1 C4 N8 C5 -11(3) . . . . ? C6 C5 N8 C16 135(2) . . . . ? C6 C5 N8 C4 -39(3) . . . . ? N6 C3 Rh1 C2 -151(2) . . . . ? N5 C3 Rh1 C2 39(2) . . . . ? N6 C3 Rh1 C1 120(5) . . . . ? N5 C3 Rh1 C1 -51(7) . . . . ? N6 C3 Rh1 C4 23(2) . . . . ? N5 C3 Rh1 C4 -148(2) . . . . ? N6 C3 Rh1 I1 114(2) . . . . ? N5 C3 Rh1 I1 -57(2) . . . . ? N6 C3 Rh1 I2 -63(2) . . . . ? N5 C3 Rh1 I2 126(2) . . . . ? N4 C2 Rh1 C3 -3(3) . . . . ? N3 C2 Rh1 C3 163.3(18) . . . . ? N4 C2 Rh1 C1 167(3) . . . . ? N3 C2 Rh1 C1 -27.3(18) . . . . ? N4 C2 Rh1 C4 -82(9) . . . . ? N3 C2 Rh1 C4 84(9) . . . . ? N4 C2 Rh1 I1 81(2) . . . . ? N3 C2 Rh1 I1 -113.5(17) . . . . ? N4 C2 Rh1 I2 -98(2) . . . . ? N3 C2 Rh1 I2 68.1(17) . . . . ? N1 C1 Rh1 C3 -46(7) . . . . ? N2 C1 Rh1 C3 111(6) . . . . ? N1 C1 Rh1 C2 -136(2) . . . . ? N2 C1 Rh1 C2 21.3(19) . . . . ? N1 C1 Rh1 C4 50(2) . . . . ? N2 C1 Rh1 C4 -152.5(19) . . . . ? N1 C1 Rh1 I1 -40(2) . . . . ? N2 C1 Rh1 I1 116.9(18) . . . . ? N1 C1 Rh1 I2 137(2) . . . . ? N2 C1 Rh1 I2 -65.5(18) . . . . ? N7 C4 Rh1 C3 -27(2) . . . . ? N8 C4 Rh1 C3 167(2) . . . . ? N7 C4 Rh1 C2 53(9) . . . . ? N8 C4 Rh1 C2 -114(8) . . . . ? N7 C4 Rh1 C1 163.7(19) . . . . ? N8 C4 Rh1 C1 -3(2) . . . . ? N7 C4 Rh1 I1 -109.8(18) . . . . ? N8 C4 Rh1 I1 83.6(19) . . . . ? N7 C4 Rh1 I2 68.7(18) . . . . ? N8 C4 Rh1 I2 -97.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.43 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.134 _refine_diff_density_min -4.251 _refine_diff_density_rms 0.326 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.351 0.487 0.618 229.8 98.2 2 0.349 0.988 0.380 225.7 94.7 _platon_squeeze_details ; ? ; data_12 _database_code_depnum_ccdc_archive 'CCDC 888979' #TrackingRef '- Jenkins_combined_FINALCIF_06252012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H52 Au F9 N8 O9 S3' _chemical_formula_weight 1601.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' 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 18.2751(17) _cell_length_b 13.6076(13) _cell_length_c 27.721(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.9260(10) _cell_angle_gamma 90.00 _cell_volume 6884.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 22.89 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 2.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6547 _exptl_absorpt_correction_T_max 0.9552 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker CCD Apex II' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58315 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 24.49 _reflns_number_total 11062 _reflns_number_gt 7777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The triflate anion close to the metal is disordered which prevents the aniostropic refinement of C70. The structure also contains two disordered dichloromethane molecules, which have no close interaction with the macrocycle, and therefore were squeezed out with Platon to improve the refinement. ; _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^)+(0.1282P)^2^+18.0635P] 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 11062 _refine_ls_number_parameters 869 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.2208 _refine_ls_wR_factor_gt 0.2040 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S3 S 0.7335(4) 0.6684(11) 0.7456(2) 0.457(14) Uani 1 1 d DU . . C1 C 0.9340(5) 0.9691(7) 0.7214(3) 0.029(2) Uani 1 1 d . . . C6 C 0.9740(5) 1.1116(7) 0.6927(3) 0.035(2) Uani 1 1 d . . . C5 C 0.9309(5) 1.0674(8) 0.6567(4) 0.038(2) Uani 1 1 d . . . C4 C 0.9359(5) 0.7722(8) 0.6965(4) 0.036(2) Uani 1 1 d . . . C12 C 0.9183(5) 0.7407(9) 0.6169(4) 0.043(3) Uani 1 1 d . . . C11 C 0.9595(6) 0.6699(8) 0.6346(4) 0.041(3) Uani 1 1 d . . . C3 C 0.9327(5) 0.7203(7) 0.8011(3) 0.035(2) Uani 1 1 d . . . C10 C 0.9774(5) 0.5884(6) 0.8399(4) 0.030(2) Uani 1 1 d . . . C9 C 0.9195(5) 0.6221(6) 0.8649(3) 0.028(2) Uani 1 1 d . . . C2 C 0.9094(5) 0.9165(6) 0.8238(3) 0.025(2) Uani 1 1 d . . . C8 C 0.8639(5) 0.9366(6) 0.8966(3) 0.0236(19) Uani 1 1 d . . . C7 C 0.8969(5) 1.0206(6) 0.8851(3) 0.026(2) Uani 1 1 d . . . C14 C 1.0081(6) 0.6133(8) 0.7155(4) 0.047(3) Uani 1 1 d . . . H14A H 1.0488 0.5855 0.6975 0.056 Uiso 1 1 calc R . . H14B H 0.9736 0.5591 0.7214 0.056 Uiso 1 1 calc R . . C15 C 1.0389(6) 0.6491(7) 0.7632(4) 0.041(3) Uani 1 1 d . . . H15A H 1.0800 0.6059 0.7742 0.049 Uiso 1 1 calc R . . H15B H 1.0588 0.7161 0.7592 0.049 Uiso 1 1 calc R . . C16 C 0.8379(5) 0.7759(6) 0.8525(3) 0.027(2) Uani 1 1 d . . . H16A H 0.8168 0.7560 0.8832 0.032 Uiso 1 1 calc R . . H16B H 0.7978 0.7786 0.8272 0.032 Uiso 1 1 calc R . . C17 C 0.9740(5) 1.0852(6) 0.8210(3) 0.031(2) Uani 1 1 d . . . H17A H 1.0087 1.1076 0.8473 0.037 Uiso 1 1 calc R . . H17B H 0.9428 1.1421 0.8113 0.037 Uiso 1 1 calc R . . C18 C 1.0182(5) 1.0553(6) 0.7779(3) 0.0251(19) Uani 1 1 d . . . H18A H 1.0571 1.1048 0.7736 0.030 Uiso 1 1 calc R . . H18B H 1.0424 0.9916 0.7851 0.030 Uiso 1 1 calc R . . C19 C 0.8648(6) 0.8970(8) 0.6520(4) 0.040(3) Uani 1 1 d . . . H19A H 0.8175 0.8894 0.6675 0.049 Uiso 1 1 calc R . . H19B H 0.8541 0.9135 0.6175 0.049 Uiso 1 1 calc R . . C20 C 0.9098(6) 1.1016(9) 0.6076(4) 0.043(3) Uani 1 1 d . . . C21 C 0.9271(6) 1.0437(8) 0.5661(4) 0.044(3) Uani 1 1 d . . . H21 H 0.9527 0.9831 0.5697 0.053 Uiso 1 1 calc R . . C22 C 0.9055(6) 1.0790(9) 0.5210(4) 0.052(3) Uani 1 1 d . . . H22 H 0.9144 1.0414 0.4930 0.062 Uiso 1 1 calc R . . C23 C 0.8693(6) 1.1734(10) 0.5162(5) 0.056(3) Uani 1 1 d . . . H23 H 0.8601 1.2017 0.4852 0.067 Uiso 1 1 calc R . . C24 C 0.8488(6) 1.2207(8) 0.5559(4) 0.048(3) Uani 1 1 d . . . H24 H 0.8200 1.2786 0.5523 0.058 Uiso 1 1 calc R . . C25 C 0.8688(6) 1.1869(7) 0.6024(4) 0.039(2) Uani 1 1 d . . . H25 H 0.8544 1.2220 0.6300 0.047 Uiso 1 1 calc R . . C26 C 1.0185(6) 1.1995(7) 0.6923(4) 0.042(3) Uani 1 1 d . . . C27 C 1.0140(7) 1.2731(8) 0.7276(4) 0.050(3) Uani 1 1 d . . . H27 H 0.9796 1.2675 0.7519 0.060 Uiso 1 1 calc R . . C28 C 1.0602(8) 1.3537(8) 0.7267(5) 0.063(4) Uani 1 1 d . . . H28 H 1.0602 1.4012 0.7518 0.076 Uiso 1 1 calc R . . C29 C 1.1047(8) 1.3641(9) 0.6902(6) 0.068(4) Uani 1 1 d . . . H29 H 1.1346 1.4211 0.6887 0.081 Uiso 1 1 calc R . . C30 C 1.1079(8) 1.2931(9) 0.6546(5) 0.066(4) Uani 1 1 d . . . H30 H 1.1395 1.3020 0.6288 0.079 Uiso 1 1 calc R . . C31 C 1.0666(6) 1.2114(7) 0.6564(4) 0.047(3) Uani 1 1 d . . . H31 H 1.0708 1.1617 0.6327 0.056 Uiso 1 1 calc R . . C32 C 0.8901(6) 0.7674(8) 0.5663(4) 0.045(3) Uani 1 1 d . . . C33 C 0.9428(6) 0.7835(10) 0.5314(4) 0.055(3) Uani 1 1 d . . . H33 H 0.9938 0.7770 0.5392 0.066 Uiso 1 1 calc R . . C34 C 0.9160(7) 0.8092(9) 0.4851(5) 0.056(3) Uani 1 1 d . . . H34 H 0.9500 0.8216 0.4610 0.068 Uiso 1 1 calc R . . C35 C 0.8397(8) 0.8178(9) 0.4726(5) 0.060(3) Uani 1 1 d . . . H35 H 0.8225 0.8412 0.4417 0.073 Uiso 1 1 calc R . . C36 C 0.7929(6) 0.7913(8) 0.5064(5) 0.050(3) Uani 1 1 d . . . H36 H 0.7418 0.7905 0.4982 0.060 Uiso 1 1 calc R . . C37 C 0.8173(3) 0.7655(3) 0.55213(19) 0.046(3) Uani 1 1 d . . . H37 H 0.7827 0.7457 0.5747 0.055 Uiso 1 1 calc R . . C38 C 0.9922(3) 0.5875(3) 0.60944(19) 0.051(3) Uani 1 1 d R . . C39 C 1.0706(3) 0.5819(3) 0.60590(19) 0.056(3) Uani 1 1 d R . . H39 H 1.1008 0.6342 0.6180 0.067 Uiso 1 1 d R . . C66 C 1.1028(3) 0.5000(3) 0.58479(19) 0.084(5) Uani 1 1 d R . . H66 H 1.1542 0.4897 0.5881 0.101 Uiso 1 1 d R . . C67 C 1.0575(3) 0.4338(3) 0.55885(19) 0.127(8) Uani 1 1 d R . . H67 H 1.0779 0.3846 0.5393 0.152 Uiso 1 1 d R . . C68 C 0.9816(3) 0.4413(3) 0.56221(19) 0.106(7) Uani 1 1 d R . . H68 H 0.9506 0.3969 0.5444 0.127 Uiso 1 1 d R . . C69 C 0.9504(3) 0.5118(3) 0.59087(19) 0.095(6) Uani 1 1 d R . . H69 H 0.9001 0.5074 0.5976 0.114 Uiso 1 1 d R . . C40 C 1.0284(5) 0.5070(6) 0.8524(3) 0.031(2) Uani 1 1 d . . . C41 C 1.1025(6) 0.5247(9) 0.8596(4) 0.047(3) Uani 1 1 d . . . H41 H 1.1208 0.5896 0.8567 0.057 Uiso 1 1 calc R . . C42 C 1.1504(6) 0.4478(10) 0.8710(4) 0.055(3) Uani 1 1 d . . . H42 H 1.2014 0.4603 0.8756 0.066 Uiso 1 1 calc R . . C43 C 1.1250(8) 0.3570(9) 0.8755(5) 0.060(4) Uani 1 1 d . . . H43 H 1.1583 0.3050 0.8831 0.072 Uiso 1 1 calc R . . C44 C 1.0486(7) 0.3357(8) 0.8691(4) 0.050(3) Uani 1 1 d . . . H44 H 1.0304 0.2710 0.8733 0.059 Uiso 1 1 calc R . . C45 C 1.0023(6) 0.4125(8) 0.8568(4) 0.042(3) Uani 1 1 d . . . H45 H 0.9514 0.4002 0.8511 0.050 Uiso 1 1 calc R . . C46 C 0.8886(5) 0.5893(7) 0.9102(4) 0.033(2) Uani 1 1 d . . . C47 C 0.9343(6) 0.5854(7) 0.9518(4) 0.040(2) Uani 1 1 d . . . H47 H 0.9849 0.6009 0.9508 0.047 Uiso 1 1 calc R . . C48 C 0.9036(6) 0.5580(7) 0.9952(4) 0.043(3) Uani 1 1 d . . . H48 H 0.9334 0.5574 1.0243 0.052 Uiso 1 1 calc R . . C49 C 0.8312(6) 0.5321(7) 0.9962(4) 0.041(3) Uani 1 1 d . . . H49 H 0.8111 0.5139 1.0259 0.050 Uiso 1 1 calc R . . C50 C 0.7870(5) 0.5326(7) 0.9537(4) 0.037(2) Uani 1 1 d . . . H50 H 0.7372 0.5127 0.9543 0.045 Uiso 1 1 calc R . . C51 C 0.8152(5) 0.5619(6) 0.9107(4) 0.033(2) Uani 1 1 d . . . H51 H 0.7850 0.5634 0.8818 0.040 Uiso 1 1 calc R . . C52 C 0.8254(5) 0.9130(7) 0.9409(3) 0.027(2) Uani 1 1 d . . . C53 C 0.8467(6) 0.8360(7) 0.9707(4) 0.039(2) Uani 1 1 d . . . H53 H 0.8867 0.7960 0.9622 0.047 Uiso 1 1 calc R . . C54 C 0.8121(7) 0.8151(8) 1.0121(4) 0.048(3) Uani 1 1 d . . . H54 H 0.8265 0.7600 1.0313 0.057 Uiso 1 1 calc R . . C55 C 0.7551(7) 0.8762(9) 1.0258(4) 0.047(3) Uani 1 1 d . . . H55 H 0.7312 0.8637 1.0547 0.057 Uiso 1 1 calc R . . C56 C 0.7346(6) 0.9527(9) 0.9976(4) 0.050(3) Uani 1 1 d . . . H56 H 0.6960 0.9939 1.0072 0.060 Uiso 1 1 calc R . . C57 C 0.7685(6) 0.9739(7) 0.9544(3) 0.038(2) Uani 1 1 d . . . H57 H 0.7530 1.0282 0.9348 0.045 Uiso 1 1 calc R . . C58 C 0.9060(5) 1.1134(7) 0.9135(3) 0.028(2) Uani 1 1 d . . . C59 C 0.9456(6) 1.1117(8) 0.9580(3) 0.038(2) Uani 1 1 d . . . H59 H 0.9688 1.0527 0.9689 0.046 Uiso 1 1 calc R . . C60 C 0.9512(7) 1.1954(10) 0.9864(5) 0.058(3) Uani 1 1 d . . . H60 H 0.9789 1.1936 1.0163 0.070 Uiso 1 1 calc R . . C61 C 0.9181(6) 1.2787(9) 0.9721(4) 0.053(3) Uani 1 1 d . . . H61 H 0.9207 1.3346 0.9927 0.063 Uiso 1 1 calc R . . C62 C 0.8801(7) 1.2843(8) 0.9276(5) 0.053(3) Uani 1 1 d . . . H62 H 0.8595 1.3452 0.9169 0.064 Uiso 1 1 calc R . . C63 C 0.8718(6) 1.1998(7) 0.8980(4) 0.045(3) Uani 1 1 d . . . H63 H 0.8436 1.2021 0.8682 0.054 Uiso 1 1 calc R . . N1 N 0.9741(4) 1.0462(5) 0.7323(3) 0.0265(17) Uani 1 1 d . . . N2 N 0.9072(4) 0.9785(6) 0.6758(3) 0.0352(19) Uani 1 1 d . . . N3 N 0.9041(4) 0.8068(7) 0.6552(3) 0.040(2) Uani 1 1 d . . . N4 N 0.9698(5) 0.6862(6) 0.6844(3) 0.040(2) Uani 1 1 d . . . N5 N 0.9838(4) 0.6512(5) 0.8005(3) 0.0307(18) Uani 1 1 d . . . N6 N 0.8927(4) 0.7043(5) 0.8392(3) 0.0281(17) Uani 1 1 d . . . N7 N 0.8726(4) 0.8746(5) 0.8583(3) 0.0245(16) Uani 1 1 d . . . N8 N 0.9265(4) 1.0084(5) 0.8406(3) 0.0265(17) Uani 1 1 d . . . Au1 Au 0.92805(2) 0.84456(3) 0.760514(14) 0.03465(18) Uani 1 1 d . . . C64 C 0.1780(9) 0.8363(10) 0.8955(5) 0.069(4) Uani 1 1 d U . . O1 O 0.0890(4) 0.8448(5) 0.8206(3) 0.0411(17) Uani 1 1 d . . . O2 O 0.0718(6) 0.9576(9) 0.8878(4) 0.103(4) Uani 1 1 d . . . O3 O 0.0400(5) 0.7850(8) 0.8931(3) 0.080(3) Uani 1 1 d . . . F1 F 0.2205(4) 0.9048(7) 0.8782(3) 0.098(3) Uani 1 1 d . . . F2 F 0.1796(5) 0.8542(8) 0.9438(3) 0.107(4) Uani 1 1 d . . . F3 F 0.1991(6) 0.7458(6) 0.8851(4) 0.109(3) Uani 1 1 d . . . S1 S 0.08532(16) 0.8491(2) 0.87152(11) 0.0513(8) Uani 1 1 d U . . C65 C 0.1502(8) 0.8898(11) 0.6879(6) 0.075(4) Uani 1 1 d U . . C70 C 0.7801(12) 0.5714(13) 0.7111(7) 0.154(10) Uiso 1 1 d D . . O4 O 0.0518(4) 0.8859(7) 0.6151(4) 0.084(3) Uani 1 1 d . . . O5 O 0.1557(5) 0.9908(6) 0.6131(4) 0.083(3) Uani 1 1 d . . . O6 O 0.1755(6) 0.8096(7) 0.6059(4) 0.084(3) Uani 1 1 d . . . O7 O 0.6635(7) 0.673(2) 0.7246(5) 0.328(19) Uani 1 1 d DU . . O8 O 0.7386(12) 0.6133(16) 0.7933(4) 0.230(12) Uani 1 1 d DU . . O9 O 0.7761(6) 0.7634(14) 0.7429(5) 0.221(11) Uani 1 1 d DU . . F4 F 0.2216(4) 0.9037(7) 0.6991(3) 0.088(3) Uani 1 1 d . . . F5 F 0.1158(6) 0.9704(9) 0.7085(4) 0.125(4) Uani 1 1 d . . . F6 F 0.1242(6) 0.8080(9) 0.7046(5) 0.134(5) Uani 1 1 d . . . F7 F 0.7520(10) 0.4832(14) 0.7050(6) 0.198(7) Uani 1 1 d D . . F8 F 0.7840(8) 0.6055(18) 0.6659(5) 0.237(10) Uani 1 1 d D . . F9 F 0.8463(8) 0.5503(15) 0.7307(7) 0.255(10) Uani 1 1 d D . . S2 S 0.1246(2) 0.8978(3) 0.62486(13) 0.0720(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 S3 0.159(7) 1.14(4) 0.081(5) -0.148(11) 0.044(5) -0.340(15) C1 0.033(5) 0.030(5) 0.026(5) 0.001(4) 0.006(4) 0.001(4) C6 0.035(6) 0.037(6) 0.032(5) 0.006(5) 0.006(4) 0.019(5) C5 0.026(5) 0.050(6) 0.038(6) -0.008(5) 0.002(4) 0.011(5) C4 0.031(5) 0.044(6) 0.036(6) -0.005(5) 0.012(5) -0.012(5) C12 0.026(5) 0.066(8) 0.039(6) -0.028(6) 0.016(5) -0.029(6) C11 0.050(7) 0.041(6) 0.033(6) -0.014(5) 0.014(5) -0.026(5) C3 0.037(6) 0.037(6) 0.032(5) -0.023(4) 0.009(4) -0.016(5) C10 0.022(5) 0.025(5) 0.044(6) -0.006(4) 0.008(4) -0.003(4) C9 0.021(5) 0.019(4) 0.042(6) -0.010(4) 0.002(4) -0.003(4) C2 0.022(5) 0.023(5) 0.032(5) 0.000(4) -0.001(4) -0.001(4) C8 0.027(5) 0.022(5) 0.021(5) -0.002(4) -0.004(4) -0.002(4) C7 0.023(5) 0.025(5) 0.030(5) -0.006(4) 0.004(4) 0.010(4) C14 0.060(7) 0.034(6) 0.048(7) -0.010(5) 0.027(6) -0.008(5) C15 0.041(6) 0.026(5) 0.058(7) -0.010(5) 0.023(5) -0.007(4) C16 0.027(5) 0.022(5) 0.032(5) -0.008(4) 0.008(4) 0.000(4) C17 0.042(6) 0.015(4) 0.037(5) -0.002(4) 0.008(4) -0.007(4) C18 0.033(5) 0.019(4) 0.023(5) -0.002(4) -0.004(4) 0.003(4) C19 0.035(6) 0.058(7) 0.029(5) -0.005(5) 0.007(4) -0.015(5) C20 0.030(6) 0.066(8) 0.034(6) 0.003(5) 0.001(4) 0.002(5) C21 0.038(6) 0.049(7) 0.046(6) 0.001(5) 0.004(5) -0.004(5) C22 0.047(7) 0.060(8) 0.048(7) 0.013(6) 0.001(5) -0.011(6) C23 0.033(6) 0.088(10) 0.048(7) 0.025(7) 0.002(5) 0.010(6) C24 0.060(7) 0.035(6) 0.049(7) 0.017(5) -0.009(6) -0.006(5) C25 0.046(6) 0.030(5) 0.042(6) 0.006(5) 0.003(5) -0.006(5) C26 0.061(7) 0.025(5) 0.038(6) 0.009(5) -0.005(5) 0.007(5) C27 0.072(8) 0.033(6) 0.045(7) 0.005(5) 0.017(6) 0.015(6) C28 0.104(11) 0.030(6) 0.058(8) 0.000(5) 0.026(8) -0.001(6) C29 0.077(10) 0.030(7) 0.098(11) 0.000(7) 0.021(8) -0.013(6) C30 0.075(9) 0.044(7) 0.081(10) 0.003(7) 0.020(7) -0.010(7) C31 0.064(7) 0.021(5) 0.057(7) 0.002(5) 0.024(6) -0.008(5) C32 0.045(6) 0.056(7) 0.037(6) -0.013(5) 0.014(5) -0.017(5) C33 0.042(6) 0.076(9) 0.046(7) -0.017(6) 0.000(5) -0.020(6) C34 0.053(8) 0.062(8) 0.054(8) -0.004(6) 0.005(6) -0.022(6) C35 0.081(10) 0.058(8) 0.043(7) -0.016(6) 0.009(7) -0.024(7) C36 0.034(6) 0.040(7) 0.076(9) 0.004(6) -0.003(6) 0.002(5) C37 0.034(6) 0.042(6) 0.062(7) 0.025(6) 0.007(5) 0.001(5) C38 0.063(8) 0.039(6) 0.054(7) -0.019(5) 0.018(6) -0.015(6) C39 0.057(8) 0.056(7) 0.056(7) -0.006(6) 0.013(6) -0.003(6) C66 0.073(10) 0.085(11) 0.097(11) -0.033(9) 0.033(9) 0.024(8) C67 0.098(13) 0.102(14) 0.18(2) -0.109(14) 0.048(13) -0.032(11) C68 0.080(11) 0.047(8) 0.184(18) -0.067(10) -0.058(12) 0.007(8) C69 0.056(8) 0.044(8) 0.181(18) -0.047(10) -0.029(10) -0.001(7) C40 0.034(5) 0.023(5) 0.036(5) -0.017(4) 0.008(4) 0.004(4) C41 0.034(6) 0.052(7) 0.056(7) -0.007(6) 0.001(5) -0.005(5) C42 0.035(6) 0.070(9) 0.062(8) 0.006(7) 0.018(6) 0.016(6) C43 0.072(9) 0.055(8) 0.053(8) 0.009(6) 0.017(7) 0.034(7) C44 0.071(9) 0.031(6) 0.048(7) 0.001(5) 0.007(6) 0.015(6) C45 0.042(6) 0.043(6) 0.041(6) -0.019(5) 0.012(5) -0.005(5) C46 0.033(5) 0.022(5) 0.043(6) -0.005(4) 0.005(5) 0.001(4) C47 0.033(6) 0.037(6) 0.049(7) -0.005(5) 0.007(5) -0.003(5) C48 0.050(7) 0.036(6) 0.042(6) -0.006(5) -0.006(5) 0.016(5) C49 0.054(7) 0.033(6) 0.038(6) 0.004(5) 0.015(5) 0.013(5) C50 0.036(6) 0.023(5) 0.053(7) -0.002(5) 0.016(5) 0.008(4) C51 0.036(5) 0.017(5) 0.047(6) -0.007(4) 0.011(5) 0.002(4) C52 0.025(5) 0.029(5) 0.028(5) -0.004(4) 0.003(4) -0.001(4) C53 0.048(6) 0.035(6) 0.034(6) -0.005(5) -0.005(5) 0.006(5) C54 0.071(8) 0.038(6) 0.035(6) 0.009(5) 0.005(6) -0.001(6) C55 0.064(8) 0.055(7) 0.026(6) -0.003(5) 0.018(5) -0.012(6) C56 0.057(7) 0.052(7) 0.042(7) -0.002(6) 0.021(6) 0.008(6) C57 0.048(6) 0.036(6) 0.031(5) -0.003(4) 0.012(5) 0.012(5) C58 0.026(5) 0.021(5) 0.037(5) -0.001(4) 0.006(4) 0.000(4) C59 0.040(6) 0.043(6) 0.031(6) -0.003(5) -0.004(5) 0.003(5) C60 0.058(8) 0.059(8) 0.057(8) -0.029(7) 0.002(6) -0.002(7) C61 0.054(7) 0.047(7) 0.059(8) -0.035(6) 0.023(6) -0.023(6) C62 0.060(8) 0.027(6) 0.074(9) -0.008(6) 0.025(7) 0.002(5) C63 0.055(7) 0.028(6) 0.053(7) -0.005(5) 0.009(6) 0.010(5) N1 0.028(4) 0.028(4) 0.024(4) 0.002(3) 0.009(3) 0.008(3) N2 0.024(4) 0.043(5) 0.039(5) 0.008(4) 0.000(4) 0.000(4) N3 0.028(4) 0.055(5) 0.038(5) -0.020(4) 0.012(4) -0.012(4) N4 0.045(5) 0.039(5) 0.039(5) -0.021(4) 0.024(4) -0.026(4) N5 0.020(4) 0.030(4) 0.043(5) -0.018(4) 0.011(3) -0.007(3) N6 0.030(4) 0.020(4) 0.035(4) -0.008(3) 0.006(4) -0.005(3) N7 0.025(4) 0.021(4) 0.028(4) -0.003(3) 0.004(3) 0.002(3) N8 0.031(4) 0.024(4) 0.025(4) -0.003(3) 0.004(3) 0.004(3) Au1 0.0326(3) 0.0363(3) 0.0358(3) -0.00816(17) 0.00939(17) -0.00525(17) C64 0.082(10) 0.051(8) 0.073(10) -0.002(7) -0.014(8) 0.010(7) O1 0.041(4) 0.038(4) 0.043(4) -0.003(3) -0.005(3) -0.004(3) O2 0.120(9) 0.117(9) 0.071(7) -0.015(6) 0.000(6) 0.078(8) O3 0.067(6) 0.127(9) 0.043(5) 0.016(5) -0.003(4) -0.053(6) F1 0.056(5) 0.127(8) 0.109(7) 0.022(6) -0.009(5) -0.051(5) F2 0.094(7) 0.156(10) 0.067(6) 0.004(5) -0.034(5) -0.050(6) F3 0.139(9) 0.052(5) 0.133(8) -0.017(5) -0.016(7) 0.019(5) S1 0.0391(16) 0.068(2) 0.0457(17) -0.0063(15) -0.0048(13) -0.0130(14) C65 0.066(10) 0.064(9) 0.097(11) 0.006(8) 0.033(9) 0.019(8) O4 0.031(5) 0.072(6) 0.147(10) 0.017(6) -0.017(5) -0.003(4) O5 0.059(6) 0.042(5) 0.150(10) 0.035(6) 0.016(6) -0.006(4) O6 0.119(9) 0.053(5) 0.075(7) -0.003(5) -0.031(6) -0.007(6) O7 0.094(11) 0.80(6) 0.089(10) -0.118(19) 0.021(8) -0.21(2) O8 0.26(2) 0.38(3) 0.044(7) -0.001(12) -0.015(10) -0.19(2) O9 0.038(6) 0.54(4) 0.087(9) -0.022(15) 0.017(6) -0.102(13) F4 0.059(5) 0.126(8) 0.077(5) -0.002(5) -0.012(4) 0.009(5) F5 0.124(8) 0.167(11) 0.089(7) -0.013(7) 0.038(6) 0.062(8) F6 0.104(8) 0.131(9) 0.168(11) 0.097(8) 0.009(7) -0.022(7) F7 0.224(17) 0.211(17) 0.161(13) -0.003(12) 0.037(12) -0.087(14) F8 0.135(12) 0.46(3) 0.116(11) 0.062(15) 0.023(9) -0.041(16) F9 0.119(11) 0.35(3) 0.29(2) 0.022(19) -0.032(13) -0.141(15) S2 0.088(3) 0.051(2) 0.073(2) 0.0087(17) -0.037(2) -0.0216(19) _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 S3 O7 1.379(13) . ? S3 O9 1.513(15) . ? S3 O8 1.519(15) . ? S3 C70 1.863(15) . ? C1 N1 1.306(12) . ? C1 N2 1.340(12) . ? C1 Au1 2.017(9) . ? C6 C5 1.378(14) . ? C6 N1 1.413(12) . ? C6 C26 1.448(15) . ? C5 N2 1.399(13) . ? C5 C20 1.470(14) . ? C4 N3 1.341(13) . ? C4 N4 1.373(13) . ? C4 Au1 2.042(10) . ? C12 C11 1.304(16) . ? C12 N3 1.427(12) . ? C12 C32 1.512(16) . ? C11 N4 1.400(13) . ? C11 C38 1.464(12) . ? C3 N5 1.326(12) . ? C3 N6 1.334(12) . ? C3 Au1 2.030(11) . ? C10 C9 1.371(12) . ? C10 N5 1.397(12) . ? C10 C40 1.478(13) . ? C9 N6 1.401(12) . ? C9 C46 1.474(13) . ? C2 N7 1.325(11) . ? C2 N8 1.367(11) . ? C2 Au1 2.052(9) . ? C8 C7 1.338(12) . ? C8 N7 1.372(11) . ? C8 C52 1.483(12) . ? C7 N8 1.381(11) . ? C7 C58 1.493(12) . ? C14 N4 1.469(15) . ? C14 C15 1.492(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N5 1.481(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N6 1.458(11) . ? C16 N7 1.490(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N8 1.480(11) . ? C17 C18 1.532(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N1 1.468(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N3 1.423(14) . ? C19 N2 1.489(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.386(15) . ? C20 C21 1.443(15) . ? C21 C22 1.377(15) . ? C21 H21 0.9500 . ? C22 C23 1.447(17) . ? C22 H22 0.9500 . ? C23 C24 1.344(17) . ? C23 H23 0.9500 . ? C24 C25 1.400(14) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.370(15) . ? C26 C27 1.404(15) . ? C27 C28 1.385(17) . ? C27 H27 0.9500 . ? C28 C29 1.337(18) . ? C28 H28 0.9500 . ? C29 C30 1.384(18) . ? C29 H29 0.9500 . ? C30 C31 1.346(16) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.369(12) . ? C32 C33 1.416(15) . ? C33 C34 1.395(16) . ? C33 H33 0.9500 . ? C34 C35 1.425(18) . ? C34 H34 0.9500 . ? C35 C36 1.350(17) . ? C35 H35 0.9500 . ? C36 C37 1.369(13) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C69 1.3679 . ? C38 C39 1.4442 . ? C39 C66 1.4014 . ? C39 H39 0.9500 . ? C66 C67 1.3973 . ? C66 H66 0.9500 . ? C67 C68 1.3983 . ? C67 H67 0.9500 . ? C68 C69 1.3862 . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C40 C45 1.379(14) . ? C40 C41 1.379(14) . ? C41 C42 1.390(16) . ? C41 H41 0.9500 . ? C42 C43 1.329(17) . ? C42 H42 0.9500 . ? C43 C44 1.427(19) . ? C43 H43 0.9500 . ? C44 C45 1.378(15) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.390(14) . ? C46 C51 1.391(13) . ? C47 C48 1.404(15) . ? C47 H47 0.9500 . ? C48 C49 1.371(15) . ? C48 H48 0.9500 . ? C49 C50 1.396(15) . ? C49 H49 0.9500 . ? C50 C51 1.382(14) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.378(13) . ? C52 C57 1.395(13) . ? C53 C54 1.369(15) . ? C53 H53 0.9500 . ? C54 C55 1.399(16) . ? C54 H54 0.9500 . ? C55 C56 1.343(16) . ? C55 H55 0.9500 . ? C56 C57 1.406(14) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C63 1.390(14) . ? C58 C59 1.398(13) . ? C59 C60 1.385(16) . ? C59 H59 0.9500 . ? C60 C61 1.334(18) . ? C60 H60 0.9500 . ? C61 C62 1.388(17) . ? C61 H61 0.9500 . ? C62 C63 1.417(15) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 F1 1.320(16) . ? C64 F3 1.328(15) . ? C64 F2 1.358(17) . ? C64 S1 1.796(15) . ? O1 S1 1.418(8) . ? O2 S1 1.567(11) . ? O3 S1 1.362(9) . ? C65 F6 1.304(17) . ? C65 F4 1.339(17) . ? C65 F5 1.399(16) . ? C65 S2 1.791(17) . ? C70 F7 1.312(16) . ? C70 F9 1.332(16) . ? C70 F8 1.340(16) . ? O4 S2 1.353(9) . ? O5 S2 1.432(9) . ? O6 S2 1.623(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 O7 S3 O9 114.2(15) . . ? O7 S3 O8 113.9(12) . . ? O9 S3 O8 117.1(9) . . ? O7 S3 C70 104.7(12) . . ? O9 S3 C70 109.2(9) . . ? O8 S3 C70 95.0(13) . . ? N1 C1 N2 108.4(8) . . ? N1 C1 Au1 126.6(7) . . ? N2 C1 Au1 124.1(7) . . ? C5 C6 N1 105.5(9) . . ? C5 C6 C26 130.9(9) . . ? N1 C6 C26 123.2(9) . . ? C6 C5 N2 106.1(9) . . ? C6 C5 C20 130.3(10) . . ? N2 C5 C20 123.6(9) . . ? N3 C4 N4 105.8(9) . . ? N3 C4 Au1 121.7(8) . . ? N4 C4 Au1 132.5(8) . . ? C11 C12 N3 107.9(10) . . ? C11 C12 C32 133.6(10) . . ? N3 C12 C32 118.3(11) . . ? C12 C11 N4 107.5(9) . . ? C12 C11 C38 128.9(9) . . ? N4 C11 C38 123.6(10) . . ? N5 C3 N6 107.9(9) . . ? N5 C3 Au1 126.5(7) . . ? N6 C3 Au1 124.5(7) . . ? C9 C10 N5 106.7(8) . . ? C9 C10 C40 128.9(9) . . ? N5 C10 C40 124.3(8) . . ? C10 C9 N6 105.7(8) . . ? C10 C9 C46 131.9(9) . . ? N6 C9 C46 122.3(8) . . ? N7 C2 N8 105.2(7) . . ? N7 C2 Au1 121.6(6) . . ? N8 C2 Au1 133.2(6) . . ? C7 C8 N7 105.7(7) . . ? C7 C8 C52 128.4(8) . . ? N7 C8 C52 126.0(8) . . ? C8 C7 N8 108.1(7) . . ? C8 C7 C58 129.5(8) . . ? N8 C7 C58 122.3(8) . . ? N4 C14 C15 116.6(9) . . ? N4 C14 H14A 108.2 . . ? C15 C14 H14A 108.2 . . ? N4 C14 H14B 108.2 . . ? C15 C14 H14B 108.2 . . ? H14A C14 H14B 107.3 . . ? N5 C15 C14 112.8(9) . . ? N5 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? N5 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N6 C16 N7 109.5(7) . . ? N6 C16 H16A 109.8 . . ? N7 C16 H16A 109.8 . . ? N6 C16 H16B 109.8 . . ? N7 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N8 C17 C18 116.2(7) . . ? N8 C17 H17A 108.2 . . ? C18 C17 H17A 108.2 . . ? N8 C17 H17B 108.2 . . ? C18 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? N1 C18 C17 113.9(7) . . ? N1 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N1 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? N3 C19 N2 111.4(8) . . ? N3 C19 H19A 109.4 . . ? N2 C19 H19A 109.4 . . ? N3 C19 H19B 109.4 . . ? N2 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C25 C20 C21 121.0(10) . . ? C25 C20 C5 118.4(9) . . ? C21 C20 C5 120.5(10) . . ? C22 C21 C20 117.9(11) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? C21 C22 C23 120.1(12) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.6(11) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.8(11) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C20 C25 C24 119.0(10) . . ? C20 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C31 C26 C27 118.9(10) . . ? C31 C26 C6 119.0(9) . . ? C27 C26 C6 122.1(10) . . ? C28 C27 C26 119.7(11) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 119.5(12) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.9(12) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 120.4(13) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C26 120.5(11) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.8 . . ? C37 C32 C33 119.5(9) . . ? C37 C32 C12 122.8(8) . . ? C33 C32 C12 117.3(10) . . ? C34 C33 C32 116.7(11) . . ? C34 C33 H33 121.7 . . ? C32 C33 H33 121.7 . . ? C33 C34 C35 122.5(11) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C36 C35 C34 117.1(12) . . ? C36 C35 H35 121.4 . . ? C34 C35 H35 121.4 . . ? C35 C36 C37 121.6(11) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C32 121.8(8) . . ? C36 C37 H37 119.1 . . ? C32 C37 H37 119.1 . . ? C69 C38 C39 118.1 . . ? C69 C38 C11 121.6(5) . . ? C39 C38 C11 120.2(5) . . ? C66 C39 C38 120.6 . . ? C66 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C67 C66 C39 118.6 . . ? C67 C66 H66 120.7 . . ? C39 C66 H66 120.7 . . ? C66 C67 C68 118.8 . . ? C66 C67 H67 120.6 . . ? C68 C67 H67 120.6 . . ? C69 C68 C67 121.8 . . ? C69 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? C38 C69 C68 119.9 . . ? C38 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C45 C40 C41 119.5(10) . . ? C45 C40 C10 120.1(9) . . ? C41 C40 C10 120.4(9) . . ? C40 C41 C42 120.2(11) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C43 C42 C41 120.1(12) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 121.4(11) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C45 C44 C43 117.5(11) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? C44 C45 C40 121.1(10) . . ? C44 C45 H45 119.4 . . ? C40 C45 H45 119.4 . . ? C47 C46 C51 121.4(9) . . ? C47 C46 C9 118.5(8) . . ? C51 C46 C9 120.1(9) . . ? C46 C47 C48 118.1(9) . . ? C46 C47 H47 121.0 . . ? C48 C47 H47 121.0 . . ? C49 C48 C47 121.0(10) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 C50 119.9(10) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 120.3(10) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C46 119.2(10) . . ? C50 C51 H51 120.4 . . ? C46 C51 H51 120.4 . . ? C53 C52 C57 119.0(9) . . ? C53 C52 C8 121.9(8) . . ? C57 C52 C8 119.0(8) . . ? C54 C53 C52 122.1(10) . . ? C54 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? C53 C54 C55 119.1(10) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 119.5(10) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 C56 C57 122.2(10) . . ? C55 C56 H56 118.9 . . ? C57 C56 H56 118.9 . . ? C52 C57 C56 118.2(9) . . ? C52 C57 H57 120.9 . . ? C56 C57 H57 120.9 . . ? C63 C58 C59 119.4(9) . . ? C63 C58 C7 121.0(9) . . ? C59 C58 C7 119.4(8) . . ? C60 C59 C58 120.5(11) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C61 C60 C59 120.7(12) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 120.6(10) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? C61 C62 C63 120.3(11) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C58 C63 C62 118.3(11) . . ? C58 C63 H63 120.8 . . ? C62 C63 H63 120.8 . . ? C1 N1 C6 110.3(8) . . ? C1 N1 C18 122.9(7) . . ? C6 N1 C18 126.5(8) . . ? C1 N2 C5 109.6(8) . . ? C1 N2 C19 120.3(8) . . ? C5 N2 C19 129.8(8) . . ? C4 N3 C19 123.6(8) . . ? C4 N3 C12 109.1(10) . . ? C19 N3 C12 127.3(9) . . ? C4 N4 C11 109.7(10) . . ? C4 N4 C14 129.7(8) . . ? C11 N4 C14 120.5(9) . . ? C3 N5 C10 109.8(8) . . ? C3 N5 C15 121.7(9) . . ? C10 N5 C15 128.5(8) . . ? C3 N6 C9 109.9(8) . . ? C3 N6 C16 120.2(8) . . ? C9 N6 C16 129.2(7) . . ? C2 N7 C8 112.1(7) . . ? C2 N7 C16 122.6(7) . . ? C8 N7 C16 124.8(7) . . ? C2 N8 C7 108.8(7) . . ? C2 N8 C17 130.5(7) . . ? C7 N8 C17 120.5(7) . . ? C1 Au1 C3 174.5(4) . . ? C1 Au1 C4 86.0(4) . . ? C3 Au1 C4 94.4(4) . . ? C1 Au1 C2 94.2(3) . . ? C3 Au1 C2 85.9(3) . . ? C4 Au1 C2 174.5(4) . . ? F1 C64 F3 113.2(14) . . ? F1 C64 F2 104.3(11) . . ? F3 C64 F2 112.9(12) . . ? F1 C64 S1 111.0(9) . . ? F3 C64 S1 106.8(10) . . ? F2 C64 S1 108.7(11) . . ? O3 S1 O1 118.2(5) . . ? O3 S1 O2 111.6(7) . . ? O1 S1 O2 110.0(5) . . ? O3 S1 C64 111.0(7) . . ? O1 S1 C64 105.9(6) . . ? O2 S1 C64 98.3(6) . . ? F6 C65 F4 114.0(13) . . ? F6 C65 F5 110.2(12) . . ? F4 C65 F5 104.3(13) . . ? F6 C65 S2 108.5(12) . . ? F4 C65 S2 114.9(10) . . ? F5 C65 S2 104.4(10) . . ? F7 C70 F9 101.4(16) . . ? F7 C70 F8 103.7(18) . . ? F9 C70 F8 112(2) . . ? F7 C70 S3 121.8(17) . . ? F9 C70 S3 111.8(16) . . ? F8 C70 S3 106.3(14) . . ? O4 S2 O5 117.3(6) . . ? O4 S2 O6 114.9(6) . . ? O5 S2 O6 109.8(6) . . ? O4 S2 C65 113.2(7) . . ? O5 S2 C65 101.0(7) . . ? O6 S2 C65 98.3(6) . . ? 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 N1 C6 C5 N2 0.0(10) . . . . ? C26 C6 C5 N2 173.4(10) . . . . ? N1 C6 C5 C20 178.8(9) . . . . ? C26 C6 C5 C20 -7.7(18) . . . . ? N3 C12 C11 N4 2.6(11) . . . . ? C32 C12 C11 N4 177.3(10) . . . . ? N3 C12 C11 C38 -176.2(8) . . . . ? C32 C12 C11 C38 -1.6(18) . . . . ? N5 C10 C9 N6 0.3(9) . . . . ? C40 C10 C9 N6 176.0(9) . . . . ? N5 C10 C9 C46 -177.0(9) . . . . ? C40 C10 C9 C46 -1.3(17) . . . . ? N7 C8 C7 N8 -1.2(9) . . . . ? C52 C8 C7 N8 178.9(8) . . . . ? N7 C8 C7 C58 -178.6(8) . . . . ? C52 C8 C7 C58 1.5(16) . . . . ? N4 C14 C15 N5 83.3(11) . . . . ? N8 C17 C18 N1 73.8(10) . . . . ? C6 C5 C20 C25 -62.3(15) . . . . ? N2 C5 C20 C25 116.4(11) . . . . ? C6 C5 C20 C21 121.9(12) . . . . ? N2 C5 C20 C21 -59.4(14) . . . . ? C25 C20 C21 C22 3.9(16) . . . . ? C5 C20 C21 C22 179.5(10) . . . . ? C20 C21 C22 C23 2.5(16) . . . . ? C21 C22 C23 C24 -8.2(17) . . . . ? C22 C23 C24 C25 7.4(18) . . . . ? C21 C20 C25 C24 -4.8(16) . . . . ? C5 C20 C25 C24 179.5(10) . . . . ? C23 C24 C25 C20 -1.0(17) . . . . ? C5 C6 C26 C31 -49.6(16) . . . . ? N1 C6 C26 C31 122.9(11) . . . . ? C5 C6 C26 C27 130.6(11) . . . . ? N1 C6 C26 C27 -57.0(14) . . . . ? C31 C26 C27 C28 -2.7(17) . . . . ? C6 C26 C27 C28 177.2(11) . . . . ? C26 C27 C28 C29 5(2) . . . . ? C27 C28 C29 C30 -3(2) . . . . ? C28 C29 C30 C31 -1(2) . . . . ? C29 C30 C31 C26 3(2) . . . . ? C27 C26 C31 C30 -1.2(17) . . . . ? C6 C26 C31 C30 179.0(11) . . . . ? C11 C12 C32 C37 114.8(13) . . . . ? N3 C12 C32 C37 -71.0(12) . . . . ? C11 C12 C32 C33 -57.6(17) . . . . ? N3 C12 C32 C33 116.6(11) . . . . ? C37 C32 C33 C34 8.1(17) . . . . ? C12 C32 C33 C34 -179.2(11) . . . . ? C32 C33 C34 C35 -1.0(19) . . . . ? C33 C34 C35 C36 -5.8(19) . . . . ? C34 C35 C36 C37 5.6(17) . . . . ? C35 C36 C37 C32 1.5(15) . . . . ? C33 C32 C37 C36 -8.7(14) . . . . ? C12 C32 C37 C36 179.0(9) . . . . ? C12 C11 C38 C69 -71.2(11) . . . . ? N4 C11 C38 C69 110.2(8) . . . . ? C12 C11 C38 C39 112.2(10) . . . . ? N4 C11 C38 C39 -66.5(9) . . . . ? C69 C38 C39 C66 -1.2 . . . . ? C11 C38 C39 C66 175.6(6) . . . . ? C38 C39 C66 C67 12.6 . . . . ? C39 C66 C67 C68 -11.6 . . . . ? C66 C67 C68 C69 -0.7 . . . . ? C39 C38 C69 C68 -11.2 . . . . ? C11 C38 C69 C68 172.1(6) . . . . ? C67 C68 C69 C38 12.4 . . . . ? C9 C10 C40 C45 60.9(14) . . . . ? N5 C10 C40 C45 -124.1(10) . . . . ? C9 C10 C40 C41 -119.2(11) . . . . ? N5 C10 C40 C41 55.8(13) . . . . ? C45 C40 C41 C42 0.2(16) . . . . ? C10 C40 C41 C42 -179.7(10) . . . . ? C40 C41 C42 C43 -0.6(18) . . . . ? C41 C42 C43 C44 -0.5(19) . . . . ? C42 C43 C44 C45 1.9(18) . . . . ? C43 C44 C45 C40 -2.2(16) . . . . ? C41 C40 C45 C44 1.3(15) . . . . ? C10 C40 C45 C44 -178.8(9) . . . . ? C10 C9 C46 C47 56.5(14) . . . . ? N6 C9 C46 C47 -120.4(10) . . . . ? C10 C9 C46 C51 -122.7(11) . . . . ? N6 C9 C46 C51 60.4(12) . . . . ? C51 C46 C47 C48 -3.3(14) . . . . ? C9 C46 C47 C48 177.4(9) . . . . ? C46 C47 C48 C49 2.4(15) . . . . ? C47 C48 C49 C50 0.2(15) . . . . ? C48 C49 C50 C51 -2.0(14) . . . . ? C49 C50 C51 C46 1.1(13) . . . . ? C47 C46 C51 C50 1.6(13) . . . . ? C9 C46 C51 C50 -179.2(8) . . . . ? C7 C8 C52 C53 -121.4(11) . . . . ? N7 C8 C52 C53 58.7(13) . . . . ? C7 C8 C52 C57 55.0(13) . . . . ? N7 C8 C52 C57 -124.9(10) . . . . ? C57 C52 C53 C54 2.4(15) . . . . ? C8 C52 C53 C54 178.8(9) . . . . ? C52 C53 C54 C55 -2.6(17) . . . . ? C53 C54 C55 C56 1.3(17) . . . . ? C54 C55 C56 C57 0.1(18) . . . . ? C53 C52 C57 C56 -0.9(15) . . . . ? C8 C52 C57 C56 -177.4(9) . . . . ? C55 C56 C57 C52 -0.3(17) . . . . ? C8 C7 C58 C63 -113.9(12) . . . . ? N8 C7 C58 C63 69.1(12) . . . . ? C8 C7 C58 C59 61.8(13) . . . . ? N8 C7 C58 C59 -115.3(10) . . . . ? C63 C58 C59 C60 -0.4(15) . . . . ? C7 C58 C59 C60 -176.2(10) . . . . ? C58 C59 C60 C61 1.0(18) . . . . ? C59 C60 C61 C62 -2.8(18) . . . . ? C60 C61 C62 C63 4.1(17) . . . . ? C59 C58 C63 C62 1.7(15) . . . . ? C7 C58 C63 C62 177.3(9) . . . . ? C61 C62 C63 C58 -3.5(16) . . . . ? N2 C1 N1 C6 0.7(10) . . . . ? Au1 C1 N1 C6 169.7(6) . . . . ? N2 C1 N1 C18 -173.3(7) . . . . ? Au1 C1 N1 C18 -4.3(12) . . . . ? C5 C6 N1 C1 -0.4(10) . . . . ? C26 C6 N1 C1 -174.5(9) . . . . ? C5 C6 N1 C18 173.4(8) . . . . ? C26 C6 N1 C18 -0.7(14) . . . . ? C17 C18 N1 C1 -79.6(10) . . . . ? C17 C18 N1 C6 107.3(9) . . . . ? N1 C1 N2 C5 -0.7(10) . . . . ? Au1 C1 N2 C5 -170.1(6) . . . . ? N1 C1 N2 C19 174.4(8) . . . . ? Au1 C1 N2 C19 5.1(12) . . . . ? C6 C5 N2 C1 0.5(10) . . . . ? C20 C5 N2 C1 -178.5(9) . . . . ? C6 C5 N2 C19 -174.1(9) . . . . ? C20 C5 N2 C19 6.9(15) . . . . ? N3 C19 N2 C1 -52.8(11) . . . . ? N3 C19 N2 C5 121.3(10) . . . . ? N4 C4 N3 C19 -178.1(8) . . . . ? Au1 C4 N3 C19 2.1(12) . . . . ? N4 C4 N3 C12 0.3(10) . . . . ? Au1 C4 N3 C12 -179.4(6) . . . . ? N2 C19 N3 C4 48.8(12) . . . . ? N2 C19 N3 C12 -129.4(9) . . . . ? C11 C12 N3 C4 -1.9(11) . . . . ? C32 C12 N3 C4 -177.5(8) . . . . ? C11 C12 N3 C19 176.5(9) . . . . ? C32 C12 N3 C19 0.9(14) . . . . ? N3 C4 N4 C11 1.3(10) . . . . ? Au1 C4 N4 C11 -179.0(7) . . . . ? N3 C4 N4 C14 -174.8(9) . . . . ? Au1 C4 N4 C14 4.9(15) . . . . ? C12 C11 N4 C4 -2.6(11) . . . . ? C38 C11 N4 C4 176.4(8) . . . . ? C12 C11 N4 C14 174.0(9) . . . . ? C38 C11 N4 C14 -7.1(13) . . . . ? C15 C14 N4 C4 -24.4(15) . . . . ? C15 C14 N4 C11 159.8(9) . . . . ? N6 C3 N5 C10 -0.5(10) . . . . ? Au1 C3 N5 C10 167.6(6) . . . . ? N6 C3 N5 C15 -178.5(8) . . . . ? Au1 C3 N5 C15 -10.3(12) . . . . ? C9 C10 N5 C3 0.1(10) . . . . ? C40 C10 N5 C3 -175.8(8) . . . . ? C9 C10 N5 C15 177.9(8) . . . . ? C40 C10 N5 C15 2.0(14) . . . . ? C14 C15 N5 C3 -75.6(11) . . . . ? C14 C15 N5 C10 106.9(11) . . . . ? N5 C3 N6 C9 0.7(10) . . . . ? Au1 C3 N6 C9 -167.7(6) . . . . ? N5 C3 N6 C16 172.5(7) . . . . ? Au1 C3 N6 C16 4.0(12) . . . . ? C10 C9 N6 C3 -0.6(10) . . . . ? C46 C9 N6 C3 177.0(8) . . . . ? C10 C9 N6 C16 -171.4(8) . . . . ? C46 C9 N6 C16 6.2(14) . . . . ? N7 C16 N6 C3 -54.0(10) . . . . ? N7 C16 N6 C9 115.9(9) . . . . ? N8 C2 N7 C8 1.3(10) . . . . ? Au1 C2 N7 C8 -177.6(6) . . . . ? N8 C2 N7 C16 174.5(7) . . . . ? Au1 C2 N7 C16 -4.3(11) . . . . ? C7 C8 N7 C2 0.0(10) . . . . ? C52 C8 N7 C2 179.9(8) . . . . ? C7 C8 N7 C16 -173.1(8) . . . . ? C52 C8 N7 C16 6.8(13) . . . . ? N6 C16 N7 C2 54.9(11) . . . . ? N6 C16 N7 C8 -132.7(8) . . . . ? N7 C2 N8 C7 -2.0(9) . . . . ? Au1 C2 N8 C7 176.7(7) . . . . ? N7 C2 N8 C17 172.2(8) . . . . ? Au1 C2 N8 C17 -9.1(14) . . . . ? C8 C7 N8 C2 2.0(10) . . . . ? C58 C7 N8 C2 179.7(8) . . . . ? C8 C7 N8 C17 -172.8(8) . . . . ? C58 C7 N8 C17 4.8(12) . . . . ? C18 C17 N8 C2 -7.4(14) . . . . ? C18 C17 N8 C7 166.2(8) . . . . ? N1 C1 Au1 C3 -40(4) . . . . ? N2 C1 Au1 C3 127(3) . . . . ? N1 C1 Au1 C4 -135.0(8) . . . . ? N2 C1 Au1 C4 32.4(8) . . . . ? N1 C1 Au1 C2 50.6(8) . . . . ? N2 C1 Au1 C2 -142.1(8) . . . . ? N5 C3 Au1 C1 -41(4) . . . . ? N6 C3 Au1 C1 125(3) . . . . ? N5 C3 Au1 C4 53.3(8) . . . . ? N6 C3 Au1 C4 -140.4(8) . . . . ? N5 C3 Au1 C2 -132.2(8) . . . . ? N6 C3 Au1 C2 34.1(8) . . . . ? N3 C4 Au1 C1 -36.4(8) . . . . ? N4 C4 Au1 C1 144.0(9) . . . . ? N3 C4 Au1 C3 149.1(8) . . . . ? N4 C4 Au1 C3 -30.5(9) . . . . ? N3 C4 Au1 C2 56(4) . . . . ? N4 C4 Au1 C2 -123(4) . . . . ? N7 C2 Au1 C1 152.5(7) . . . . ? N8 C2 Au1 C1 -26.0(9) . . . . ? N7 C2 Au1 C3 -33.1(7) . . . . ? N8 C2 Au1 C3 148.4(9) . . . . ? N7 C2 Au1 C4 60(4) . . . . ? N8 C2 Au1 C4 -118(4) . . . . ? F1 C64 S1 O3 -173.6(10) . . . . ? F3 C64 S1 O3 62.6(13) . . . . ? F2 C64 S1 O3 -59.5(11) . . . . ? F1 C64 S1 O1 57.0(11) . . . . ? F3 C64 S1 O1 -66.8(11) . . . . ? F2 C64 S1 O1 171.1(8) . . . . ? F1 C64 S1 O2 -56.6(11) . . . . ? F3 C64 S1 O2 179.6(11) . . . . ? F2 C64 S1 O2 57.5(10) . . . . ? O7 S3 C70 F7 -53(2) . . . . ? O9 S3 C70 F7 -175.6(17) . . . . ? O8 S3 C70 F7 63.3(19) . . . . ? O7 S3 C70 F9 -172.9(18) . . . . ? O9 S3 C70 F9 64.5(18) . . . . ? O8 S3 C70 F9 -56.6(18) . . . . ? O7 S3 C70 F8 65.2(19) . . . . ? O9 S3 C70 F8 -57.5(17) . . . . ? O8 S3 C70 F8 -178.5(16) . . . . ? F6 C65 S2 O4 52.7(12) . . . . ? F4 C65 S2 O4 -178.4(10) . . . . ? F5 C65 S2 O4 -64.8(12) . . . . ? F6 C65 S2 O5 178.9(10) . . . . ? F4 C65 S2 O5 -52.2(12) . . . . ? F5 C65 S2 O5 61.4(11) . . . . ? F6 C65 S2 O6 -69.0(11) . . . . ? F4 C65 S2 O6 59.9(12) . . . . ? F5 C65 S2 O6 173.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 24.49 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.369 _refine_diff_density_min -2.188 _refine_diff_density_rms 0.169 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.766 -0.141 0.224 122 40 ' ' 2 0.234 0.141 0.775 122 40 ' ' 3 0.347 0.112 0.239 49 13 ' ' 4 0.734 0.359 0.275 122 40 ' ' 5 0.847 0.388 0.739 49 13 ' ' 6 0.266 0.641 0.724 122 40 ' ' 7 0.153 0.612 0.261 49 13 ' ' 8 0.653 0.888 0.761 49 13 ' ' _platon_squeeze_details ; ;