# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1880 data_global _publ_requested_journal ' J.Chem.Soc.Dalton.Trans.' _publ_contact_author ; Kim R. Dunbar Dept. of Chemistry Texas A&M University PO Box 30012 College Station, TX 77842-3012 ; _publ_contact_author_email ' dunbar@mail.chem.tamu.edu' _publ_section_title ; Homoleptic complexes of Ag(I), Cu(I), Pd(II) and Pt(II) with Tetrathiafulvalene-Functionalized Phosphine Ligands ; data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 B Cl4 F4 P4 Pd0.50 S4' _chemical_formula_weight 1250.84 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 P2(1)/c _symmetry_Int_Tables_number 14 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 17.0665(8) _cell_length_b 19.0941(9) _cell_length_c 19.2877(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.1380(10) _cell_angle_gamma 90.00 _cell_volume 5690.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63739 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.31 _reflns_number_total 13718 _reflns_number_gt 8740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13718 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1230 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.082 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 1.0000 0.0000 0.02086(12) Uani 1 2 d S . . P1 P 0.60971(6) 1.08407(5) 0.02737(6) 0.0235(2) Uani 1 1 d . B . S4 S 1.00299(7) 0.94416(6) 0.28111(7) 0.0372(3) Uani 1 1 d . . . P2 P 0.61235(6) 0.92417(5) 0.07409(6) 0.0240(2) Uani 1 1 d . . . S3 S 1.01528(7) 1.08871(6) 0.23676(7) 0.0365(3) Uani 1 1 d . C . S2 S 0.79703(6) 0.94935(6) 0.20185(6) 0.0330(3) Uani 1 1 d . . . P3 P 1.18027(8) 0.90064(7) 0.28403(8) 0.0399(3) Uani 1 1 d . . . C3 C 0.8604(3) 1.0221(2) 0.2017(2) 0.0283(9) Uani 1 1 d . . . S1 S 0.79839(6) 1.09605(5) 0.15412(7) 0.0330(3) Uani 1 1 d . . . P4 P 1.19696(8) 1.06765(6) 0.23734(7) 0.0379(3) Uani 1 1 d . C . C1 C 0.7046(2) 1.0470(2) 0.1042(2) 0.0262(9) Uani 1 1 d . . . C2 C 0.7041(2) 0.9801(2) 0.1254(2) 0.0249(8) Uani 1 1 d . . . C4 C 0.9469(3) 1.0196(2) 0.2355(2) 0.0319(10) Uani 1 1 d . . . C6 C 1.0967(3) 0.9655(2) 0.2676(2) 0.0334(10) Uani 1 1 d . C . C5 C 1.1023(3) 1.0332(2) 0.2495(2) 0.0329(10) Uani 1 1 d . . . C7 C 0.5985(3) 1.0628(2) -0.1174(3) 0.0357(10) Uani 1 1 d . . . H7A H 0.5547 1.0314 -0.1225 0.043 Uiso 1 1 calc R . . C8 C 0.6227(3) 1.0710(3) -0.1775(3) 0.0494(13) Uani 1 1 d . . . H8A H 0.5964 1.0447 -0.2220 0.059 Uiso 1 1 calc R . . C9 C 0.6865(3) 1.1191(3) -0.1696(3) 0.0573(15) Uani 1 1 d . . . H9A H 0.7021 1.1256 -0.2099 0.069 Uiso 1 1 calc R . . C10 C 0.7273(3) 1.1574(3) -0.1038(3) 0.0545(14) Uani 1 1 d . . . H10A H 0.7707 1.1889 -0.0995 0.065 Uiso 1 1 calc R . . C11 C 0.7038(3) 1.1495(3) -0.0436(3) 0.0415(11) Uani 1 1 d . . . H11A H 0.7306 1.1762 0.0007 0.050 Uiso 1 1 calc R . . C12 C 0.6390(2) 1.1006(2) -0.0503(2) 0.0291(9) Uani 1 1 d . . . C13 C 0.5996(2) 1.1670(2) 0.0689(2) 0.0283(9) Uani 1 1 d . . . C18 C 0.6017(3) 1.1660(3) 0.1417(3) 0.0408(11) Uani 1 1 d . B . H18A H 0.6093 1.1237 0.1678 0.050(15) Uiso 1 1 calc R A 1 C14 C 0.5881(3) 1.2301(2) 0.0302(3) 0.0437(12) Uani 1.009(6) 1 d P B 1 H14A H 0.5871 1.2316 -0.0183 0.052 Uiso 1.009(6) 1 calc PR B 1 C15 C 0.5779(4) 1.2913(3) 0.0650(4) 0.0633(17) Uani 1.009(6) 1 d P B 1 H15A H 0.5697 1.3338 0.0394 0.076 Uiso 1.009(6) 1 calc PR B 1 C16 C 0.5801(3) 1.2892(3) 0.1371(4) 0.0643(18) Uani 1.009(6) 1 d P B 1 H16A H 0.5730 1.3303 0.1596 0.077 Uiso 1.009(6) 1 calc PR B 1 C17 C 0.59249(16) 1.22760(14) 0.17559(16) 0.0600(16) Uani 1.009(6) 1 d P B 1 H17A H 0.5948 1.2268 0.2246 0.072 Uiso 1.009(6) 1 calc PR B 1 C19 C 0.64688(16) 0.86507(14) 0.01893(16) 0.0289(9) Uani 1 1 d R . . C20 C 0.61529(16) 0.87438(14) -0.05903(16) 0.0380(11) Uani 1 1 d R . . H20A H 0.5740 0.9087 -0.0831 0.046 Uiso 1 1 d R . . C21 C 0.6450(3) 0.8325(3) -0.1018(3) 0.0510(13) Uani 1 1 d . . . H21A H 0.6244 0.8395 -0.1543 0.061 Uiso 1 1 calc R . . C22 C 0.7051(3) 0.7807(3) -0.0665(3) 0.0552(14) Uani 1 1 d . . . H22A H 0.7245 0.7523 -0.0951 0.066 Uiso 1 1 calc R . . C23 C 0.7362(3) 0.7715(3) 0.0114(3) 0.0531(14) Uani 1 1 d . . . H23A H 0.7770 0.7367 0.0351 0.064 Uiso 1 1 calc R . . C24 C 0.7082(3) 0.8125(2) 0.0548(3) 0.0438(12) Uani 1 1 d . . . H24A H 0.7297 0.8055 0.1074 0.053 Uiso 1 1 calc R . . C25 C 0.6021(3) 0.8744(2) 0.1487(2) 0.0322(10) Uani 1 1 d . . . C26 C 0.6117(3) 0.9082(3) 0.2154(3) 0.0401(11) Uani 1 1 d . . . H26A H 0.6284 0.9550 0.2225 0.048 Uiso 1 1 calc R . . C27 C 0.5967(3) 0.8730(3) 0.2720(3) 0.0579(15) Uani 1 1 d . . . H27A H 0.6038 0.8955 0.3170 0.069 Uiso 1 1 calc R . . C28 C 0.5709(4) 0.8037(4) 0.2594(4) 0.0711(19) Uani 1 1 d . . . H28A H 0.5595 0.7799 0.2961 0.085 Uiso 1 1 calc R . . C29 C 0.5619(4) 0.7695(3) 0.1942(4) 0.0663(17) Uani 1 1 d . . . H29A H 0.5450 0.7227 0.1873 0.080 Uiso 1 1 calc R . . C30 C 0.5777(3) 0.8041(2) 0.1384(3) 0.0447(12) Uani 1 1 d . . . H30A H 0.5721 0.7806 0.0943 0.054 Uiso 1 1 calc R . . C31 C 1.1219(3) 0.8311(2) 0.2172(3) 0.0381(10) Uani 1 1 d . C . C32 C 1.0470(4) 0.8432(3) 0.1516(3) 0.0575(15) Uani 1 1 d . . . H32A H 1.0218 0.8874 0.1429 0.069 Uiso 1 1 calc R C . C33 C 1.0095(5) 0.7908(4) 0.0991(3) 0.089(2) Uani 1 1 d . C . H33A H 0.9596 0.7997 0.0548 0.106 Uiso 1 1 calc R . . C34 C 1.0463(5) 0.7242(3) 0.1123(3) 0.085(2) Uani 1 1 d . . . H34A H 1.0205 0.6883 0.0774 0.102 Uiso 1 1 calc R C . C35 C 1.1207(4) 0.7116(3) 0.1771(3) 0.0672(17) Uani 1 1 d . C . H35A H 1.1453 0.6672 0.1863 0.081 Uiso 1 1 calc R . . C36 C 1.1590(4) 0.7650(3) 0.2286(3) 0.0502(13) Uani 1 1 d . . . H36A H 1.2103 0.7565 0.2717 0.060 Uiso 1 1 calc R C . C37 C 1.1914(3) 0.8660(3) 0.3757(3) 0.0524(15) Uani 1.004(5) 1 d P C 1 C38 C 1.2598(4) 0.8948(3) 0.4404(3) 0.082(2) Uani 1.004(5) 1 d P C 1 H38A H 1.2975 0.9267 0.4342 0.098 Uiso 1.004(5) 1 calc PR C 1 C39 C 1.2707(8) 0.8760(5) 0.5120(4) 0.134(5) Uani 1.004(5) 1 d P C 1 H39A H 1.3157 0.8954 0.5546 0.161 Uiso 1.004(5) 1 calc PR C 1 C40 C 1.2157(8) 0.8287(5) 0.5215(5) 0.116(4) Uani 1.004(5) 1 d P C 1 H40A H 1.2237 0.8163 0.5707 0.139 Uiso 1.004(5) 1 calc PR C 1 C41 C 1.1483(6) 0.7990(4) 0.4590(4) 0.098(3) Uani 1.004(5) 1 d P C 1 H41A H 1.1111 0.7669 0.4657 0.117 Uiso 1.004(5) 1 calc PR C 1 C42 C 1.1372(4) 0.8186(3) 0.3848(3) 0.0620(17) Uani 1.004(5) 1 d P C 1 H42A H 1.0927 0.7990 0.3421 0.074 Uiso 1.004(5) 1 calc PR C 1 C43 C 1.2776(3) 1.0726(2) 0.3375(3) 0.0396(11) Uani 1 1 d . . . C44 C 1.3639(3) 1.0702(3) 0.3495(3) 0.0526(14) Uani 1 1 d . C . H44A H 1.3778 1.0684 0.3078 0.063 Uiso 1 1 calc R . . C45 C 1.4291(4) 1.0702(4) 0.4230(4) 0.0741(19) Uani 1 1 d . . . H45A H 1.4866 1.0675 0.4306 0.089 Uiso 1 1 calc R C . C46 C 1.4094(4) 1.0742(3) 0.4846(4) 0.0717(19) Uani 1 1 d . C . H46A H 1.4538 1.0747 0.5339 0.086 Uiso 1 1 calc R . . C47 C 1.3245(4) 1.0775(3) 0.4746(3) 0.0593(15) Uani 1 1 d . . . H47A H 1.3113 1.0807 0.5166 0.071 Uiso 1 1 calc R C . C48 C 1.2587(3) 1.0760(3) 0.4003(3) 0.0514(13) Uani 1 1 d . C . H48A H 1.2013 1.0774 0.3930 0.062 Uiso 1 1 calc R . . C49 C 1.1626(3) 1.1591(2) 0.2142(3) 0.0375(10) Uani 1 1 d . . . C50 C 1.1387(4) 1.1806(3) 0.1406(3) 0.0557(14) Uani 1 1 d . C . H50A H 1.1439 1.1498 0.1054 0.067 Uiso 1 1 calc R . . C51 C 1.1069(4) 1.2474(3) 0.1172(3) 0.0702(18) Uani 1 1 d . . . H51A H 1.0912 1.2611 0.0667 0.084 Uiso 1 1 calc R C . C52 C 1.0987(4) 1.2935(3) 0.1683(3) 0.0620(15) Uani 1 1 d . C . H52A H 1.0770 1.3383 0.1525 0.074 Uiso 1 1 calc R . . C53 C 1.1226(3) 1.2732(3) 0.2432(3) 0.0526(14) Uani 1 1 d . . . H53A H 1.1167 1.3039 0.2781 0.063 Uiso 1 1 calc R C . C54 C 1.1552(3) 1.2072(3) 0.2656(3) 0.0499(13) Uani 1 1 d . C . H54A H 1.1728 1.1940 0.3164 0.060 Uiso 1 1 calc R . . B1 B 0.4311(5) 0.5698(4) 0.2033(4) 0.0652(19) Uani 1 1 d . . . F2 F 0.3464(2) 0.5673(2) 0.1976(2) 0.0877(12) Uani 1 1 d . . . F1 F 0.4861(3) 0.5581(2) 0.2788(2) 0.0920(13) Uani 1 1 d . . . F4 F 0.4436(3) 0.6342(2) 0.1811(2) 0.1052(14) Uani 1 1 d . . . F3 F 0.4408(3) 0.5193(2) 0.1579(2) 0.1020(14) Uani 1 1 d . . . C1S C 0.1579(9) 0.4930(4) 0.0563(8) 0.169(6) Uani 1 1 d . . . H1SA H 0.2179 0.5012 0.0912 0.202 Uiso 1 1 calc R . . H1SB H 0.1457 0.5204 0.0105 0.202 Uiso 1 1 calc R . . Cl2 Cl 0.09420(17) 0.52261(13) 0.09766(12) 0.1122(7) Uani 1 1 d . . . Cl1 Cl 0.1456(2) 0.40700(12) 0.0321(2) 0.1496(12) Uani 1 1 d . . . C2S C 0.1351(6) 0.5127(4) 0.5314(5) 0.074(3) Uani 0.788(6) 1 d P D 2 H2SA H 0.1887 0.5353 0.5650 0.089 Uiso 1 1 calc R D 2 H2SB H 0.1097 0.4919 0.5630 0.089 Uiso 1 1 calc R D 2 Cl4 Cl 0.1574(2) 0.4467(2) 0.4790(2) 0.0817(9) Uani 0.788(6) 1 d P D 2 Cl3 Cl 0.06385(15) 0.57551(12) 0.47077(14) 0.0809(10) Uani 0.788(6) 1 d P D 2 C2SB C 0.098(2) 0.500(2) 0.471(2) 0.079(10) Uiso 0.212(6) 1 d P D 3 H2SC H 0.0607 0.4846 0.4201 0.095 Uiso 0.212(6) 1 calc PR D 3 H2SD H 0.1144 0.5485 0.4688 0.095 Uiso 0.212(6) 1 calc PR D 3 Cl3B Cl 0.054(3) 0.495(5) 0.520(2) 0.88(8) Uani 0.212(6) 1 d P . 3 Cl4B Cl 0.168(3) 0.460(2) 0.502(3) 0.33(3) Uani 0.212(6) 1 d P D 3 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 0.0165(2) 0.0202(2) 0.0224(2) 0.00068(17) 0.00485(16) -0.00130(16) P1 0.0186(5) 0.0227(5) 0.0258(5) 0.0006(4) 0.0063(4) -0.0016(4) S4 0.0230(5) 0.0367(6) 0.0466(7) 0.0086(5) 0.0095(5) 0.0024(4) P2 0.0192(5) 0.0221(5) 0.0260(5) 0.0010(4) 0.0050(4) -0.0006(4) S3 0.0229(5) 0.0312(6) 0.0476(7) 0.0014(5) 0.0074(5) -0.0015(4) S2 0.0215(5) 0.0314(6) 0.0346(6) 0.0065(5) 0.0008(4) -0.0025(4) P3 0.0278(6) 0.0400(7) 0.0481(8) -0.0045(6) 0.0124(6) 0.0040(5) C3 0.022(2) 0.030(2) 0.027(2) -0.0005(17) 0.0059(17) -0.0012(16) S1 0.0204(5) 0.0260(5) 0.0409(6) -0.0009(5) 0.0015(4) -0.0030(4) P4 0.0300(6) 0.0384(7) 0.0433(7) -0.0004(5) 0.0137(5) -0.0030(5) C1 0.0180(19) 0.030(2) 0.025(2) -0.0052(17) 0.0044(16) -0.0026(16) C2 0.0187(19) 0.029(2) 0.023(2) 0.0002(16) 0.0052(15) -0.0003(16) C4 0.026(2) 0.030(2) 0.033(2) 0.0011(18) 0.0050(18) -0.0021(17) C6 0.023(2) 0.041(3) 0.032(2) -0.0037(19) 0.0074(18) 0.0001(18) C5 0.025(2) 0.030(2) 0.035(2) -0.0032(19) 0.0045(18) -0.0016(17) C7 0.027(2) 0.042(3) 0.039(3) 0.004(2) 0.015(2) -0.0018(19) C8 0.047(3) 0.069(4) 0.034(3) 0.001(2) 0.019(2) 0.005(3) C9 0.044(3) 0.091(4) 0.047(3) 0.009(3) 0.029(3) 0.000(3) C10 0.040(3) 0.070(4) 0.059(3) 0.007(3) 0.026(3) -0.018(3) C11 0.032(2) 0.049(3) 0.046(3) 0.001(2) 0.019(2) -0.009(2) C12 0.021(2) 0.037(2) 0.029(2) 0.0053(18) 0.0102(17) 0.0017(17) C13 0.0176(19) 0.023(2) 0.040(2) -0.0076(18) 0.0079(18) -0.0011(16) C18 0.034(2) 0.044(3) 0.042(3) -0.011(2) 0.014(2) 0.002(2) C14 0.038(3) 0.028(2) 0.057(3) 0.000(2) 0.014(2) 0.002(2) C15 0.059(4) 0.027(3) 0.094(5) 0.001(3) 0.022(3) 0.009(2) C16 0.049(3) 0.051(3) 0.085(5) -0.029(3) 0.021(3) 0.003(3) C17 0.045(3) 0.074(4) 0.057(4) -0.028(3) 0.018(3) 0.003(3) C19 0.021(2) 0.025(2) 0.033(2) -0.0044(17) 0.0034(17) 0.0021(16) C20 0.033(2) 0.034(2) 0.039(3) -0.005(2) 0.007(2) -0.0002(19) C21 0.057(3) 0.055(3) 0.038(3) -0.015(2) 0.017(2) -0.001(3) C22 0.050(3) 0.050(3) 0.063(4) -0.021(3) 0.022(3) 0.007(3) C23 0.044(3) 0.045(3) 0.057(3) -0.012(2) 0.008(3) 0.017(2) C24 0.040(3) 0.042(3) 0.038(3) -0.007(2) 0.006(2) 0.010(2) C25 0.021(2) 0.036(2) 0.033(2) 0.0106(19) 0.0054(18) 0.0024(17) C26 0.030(2) 0.050(3) 0.039(3) 0.010(2) 0.014(2) -0.003(2) C27 0.049(3) 0.083(4) 0.044(3) 0.019(3) 0.022(3) 0.011(3) C28 0.055(4) 0.082(5) 0.078(5) 0.046(4) 0.030(3) 0.007(3) C29 0.054(4) 0.051(4) 0.087(5) 0.025(3) 0.023(3) -0.014(3) C30 0.041(3) 0.035(3) 0.053(3) 0.011(2) 0.015(2) -0.006(2) C31 0.046(3) 0.037(3) 0.031(2) 0.0012(19) 0.017(2) 0.001(2) C32 0.069(4) 0.048(3) 0.042(3) 0.000(2) 0.010(3) 0.017(3) C33 0.107(6) 0.075(5) 0.039(3) -0.014(3) -0.012(3) 0.012(4) C34 0.123(6) 0.056(4) 0.046(4) -0.014(3) 0.007(4) -0.002(4) C35 0.105(5) 0.046(3) 0.046(3) 0.003(3) 0.027(3) 0.011(3) C36 0.065(4) 0.037(3) 0.043(3) 0.002(2) 0.017(3) 0.005(2) C37 0.057(3) 0.058(3) 0.037(3) 0.003(2) 0.015(3) 0.034(3) C38 0.082(5) 0.062(4) 0.051(4) -0.016(3) -0.021(3) 0.033(3) C39 0.187(11) 0.111(8) 0.044(5) -0.013(5) -0.010(5) 0.093(8) C40 0.199(12) 0.106(7) 0.052(5) 0.030(5) 0.063(7) 0.089(8) C41 0.124(7) 0.105(6) 0.080(5) 0.041(5) 0.058(5) 0.071(5) C42 0.070(4) 0.082(4) 0.041(3) 0.025(3) 0.031(3) 0.039(3) C43 0.032(2) 0.036(2) 0.048(3) 0.000(2) 0.014(2) -0.0041(19) C44 0.028(3) 0.064(4) 0.060(3) -0.007(3) 0.014(2) -0.003(2) C45 0.033(3) 0.101(5) 0.075(5) -0.005(4) 0.011(3) -0.008(3) C46 0.042(3) 0.082(5) 0.062(4) -0.001(3) -0.005(3) -0.018(3) C47 0.055(4) 0.065(4) 0.046(3) -0.005(3) 0.011(3) -0.016(3) C48 0.036(3) 0.061(3) 0.053(3) -0.005(3) 0.015(2) -0.008(2) C49 0.030(2) 0.037(3) 0.043(3) -0.001(2) 0.013(2) -0.0068(19) C50 0.077(4) 0.044(3) 0.050(3) -0.002(2) 0.032(3) 0.003(3) C51 0.109(5) 0.055(4) 0.041(3) 0.012(3) 0.027(3) 0.022(3) C52 0.074(4) 0.045(3) 0.057(4) -0.006(3) 0.019(3) 0.005(3) C53 0.052(3) 0.051(3) 0.048(3) -0.014(3) 0.015(3) -0.005(3) C54 0.048(3) 0.045(3) 0.047(3) -0.006(2) 0.011(2) -0.006(2) B1 0.067(5) 0.068(5) 0.051(4) 0.006(4) 0.016(4) -0.011(4) F2 0.064(2) 0.103(3) 0.083(3) 0.022(2) 0.018(2) -0.006(2) F1 0.086(3) 0.089(3) 0.060(2) -0.009(2) -0.008(2) 0.018(2) F4 0.110(3) 0.087(3) 0.111(3) 0.010(2) 0.039(3) -0.035(3) F3 0.149(4) 0.096(3) 0.071(3) -0.015(2) 0.056(3) -0.017(3) C1S 0.253(14) 0.080(6) 0.282(15) -0.060(7) 0.219(13) -0.059(7) Cl2 0.1293(19) 0.1277(18) 0.0821(14) -0.0170(13) 0.0473(13) 0.0176(15) Cl1 0.168(3) 0.0779(15) 0.265(4) -0.0328(18) 0.152(3) -0.0245(15) C2S 0.083(6) 0.071(6) 0.047(5) 0.008(4) 0.007(4) -0.021(5) Cl4 0.0876(18) 0.0836(18) 0.0898(18) 0.0208(14) 0.0530(16) 0.0196(14) Cl3 0.0765(16) 0.0818(17) 0.0869(18) 0.0221(12) 0.0372(13) 0.0150(11) Cl3B 0.49(8) 1.9(2) 0.20(3) 0.39(7) 0.13(4) 0.68(11) Cl4B 0.47(6) 0.23(3) 0.47(6) 0.00(3) 0.39(5) 0.04(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 Pd1 P2 2.3425(10) . ? Pd1 P2 2.3425(10) 3_675 ? Pd1 P1 2.3498(10) 3_675 ? Pd1 P1 2.3499(10) . ? P1 C12 1.797(4) . ? P1 C1 1.812(4) . ? P1 C13 1.816(4) . ? S4 C4 1.746(4) . ? S4 C6 1.772(4) . ? P2 C25 1.794(4) . ? P2 C2 1.805(4) . ? P2 C19 1.813(3) . ? S3 C5 1.754(4) . ? S3 C4 1.755(4) . ? S2 C2 1.745(4) . ? S2 C3 1.762(4) . ? P3 C6 1.813(4) . ? P3 C37 1.821(5) . ? P3 C31 1.824(5) . ? C3 C4 1.338(5) . ? C3 S1 1.769(4) . ? S1 C1 1.748(4) . ? P4 C49 1.835(5) . ? P4 C43 1.837(5) . ? P4 C5 1.849(5) . ? C1 C2 1.342(6) . ? C6 C5 1.355(6) . ? C7 C12 1.384(6) . ? C7 C8 1.393(6) . ? C8 C9 1.382(7) . ? C9 C10 1.372(7) . ? C10 C11 1.387(7) . ? C11 C12 1.412(6) . ? C13 C14 1.385(6) . ? C13 C18 1.389(6) . ? C18 C17 1.388(5) . ? C14 C15 1.394(7) . ? C15 C16 1.375(8) . ? C16 C17 1.358(7) . ? C19 C20 1.3764 . ? C19 C24 1.402(5) . ? C20 C21 1.390(5) . ? C21 C22 1.378(7) . ? C22 C23 1.375(7) . ? C23 C24 1.372(7) . ? C25 C26 1.385(6) . ? C25 C30 1.394(6) . ? C26 C27 1.396(7) . ? C27 C28 1.381(9) . ? C28 C29 1.367(9) . ? C29 C30 1.383(7) . ? C31 C32 1.384(6) . ? C31 C36 1.387(6) . ? C32 C33 1.373(8) . ? C33 C34 1.393(9) . ? C34 C35 1.373(8) . ? C35 C36 1.378(7) . ? C37 C42 1.356(8) . ? C37 C38 1.410(7) . ? C38 C39 1.360(11) . ? C39 C40 1.371(14) . ? C40 C41 1.386(12) . ? C41 C42 1.412(8) . ? C43 C48 1.380(7) . ? C43 C44 1.392(6) . ? C44 C45 1.382(8) . ? C45 C46 1.367(9) . ? C46 C47 1.380(8) . ? C47 C48 1.395(7) . ? C49 C50 1.364(7) . ? C49 C54 1.395(7) . ? C50 C51 1.385(7) . ? C51 C52 1.373(8) . ? C52 C53 1.379(7) . ? C53 C54 1.372(7) . ? B1 F4 1.348(8) . ? B1 F3 1.359(9) . ? B1 F1 1.374(8) . ? B1 F2 1.403(8) . ? C1S Cl2 1.696(9) . ? C1S Cl1 1.696(8) . ? C2S Cl4 1.756(11) . ? C2S Cl3 1.754(9) . ? C2SB Cl4B 1.33(5) . ? C2SB Cl3B 1.43(6) . ? Cl3B Cl3B 1.68(9) 3_566 ? Cl3B Cl4B 2.21(5) . ? 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 P2 Pd1 P2 180.0 . 3_675 ? P2 Pd1 P1 94.72(3) . 3_675 ? P2 Pd1 P1 85.27(3) 3_675 3_675 ? P2 Pd1 P1 85.28(3) . . ? P2 Pd1 P1 94.72(3) 3_675 . ? P1 Pd1 P1 180.0 3_675 . ? C12 P1 C1 106.42(18) . . ? C12 P1 C13 109.0(2) . . ? C1 P1 C13 101.51(18) . . ? C12 P1 Pd1 114.19(14) . . ? C1 P1 Pd1 105.48(13) . . ? C13 P1 Pd1 118.63(13) . . ? C4 S4 C6 94.2(2) . . ? C25 P2 C2 103.41(19) . . ? C25 P2 C19 107.92(18) . . ? C2 P2 C19 105.49(16) . . ? C25 P2 Pd1 118.89(14) . . ? C2 P2 Pd1 105.29(13) . . ? C19 P2 Pd1 114.37(10) . . ? C5 S3 C4 93.8(2) . . ? C2 S2 C3 94.08(19) . . ? C6 P3 C37 99.6(2) . . ? C6 P3 C31 102.8(2) . . ? C37 P3 C31 102.8(2) . . ? C4 C3 S2 121.4(3) . . ? C4 C3 S1 125.1(3) . . ? S2 C3 S1 113.4(2) . . ? C1 S1 C3 93.68(19) . . ? C49 P4 C43 103.0(2) . . ? C49 P4 C5 99.4(2) . . ? C43 P4 C5 100.9(2) . . ? C2 C1 S1 117.7(3) . . ? C2 C1 P1 120.1(3) . . ? S1 C1 P1 122.1(2) . . ? C1 C2 S2 117.2(3) . . ? C1 C2 P2 120.8(3) . . ? S2 C2 P2 122.0(2) . . ? C3 C4 S4 122.1(3) . . ? C3 C4 S3 124.6(3) . . ? S4 C4 S3 113.2(2) . . ? C5 C6 S4 115.1(3) . . ? C5 C6 P3 124.1(3) . . ? S4 C6 P3 120.7(3) . . ? C6 C5 S3 117.7(3) . . ? C6 C5 P4 122.3(3) . . ? S3 C5 P4 120.1(2) . . ? C12 C7 C8 120.8(4) . . ? C9 C8 C7 118.8(5) . . ? C10 C9 C8 121.4(5) . . ? C9 C10 C11 120.2(5) . . ? C10 C11 C12 119.3(5) . . ? C7 C12 C11 119.4(4) . . ? C7 C12 P1 118.9(3) . . ? C11 C12 P1 121.6(3) . . ? C14 C13 C18 119.5(4) . . ? C14 C13 P1 122.7(4) . . ? C18 C13 P1 117.8(3) . . ? C17 C18 C13 120.3(4) . . ? C13 C14 C15 119.2(5) . . ? C16 C15 C14 120.4(5) . . ? C17 C16 C15 120.6(5) . . ? C16 C17 C18 119.9(4) . . ? C20 C19 C24 119.7(2) . . ? C20 C19 P2 119.13(9) . . ? C24 C19 P2 121.1(3) . . ? C19 C20 C21 120.1(3) . . ? C22 C21 C20 120.1(5) . . ? C23 C22 C21 119.6(5) . . ? C24 C23 C22 121.3(5) . . ? C23 C24 C19 119.2(4) . . ? C26 C25 C30 119.5(4) . . ? C26 C25 P2 118.9(3) . . ? C30 C25 P2 121.4(4) . . ? C25 C26 C27 120.8(5) . . ? C28 C27 C26 118.3(6) . . ? C29 C28 C27 121.5(5) . . ? C28 C29 C30 120.3(5) . . ? C29 C30 C25 119.6(5) . . ? C32 C31 C36 118.6(4) . . ? C32 C31 P3 122.7(4) . . ? C36 C31 P3 118.4(4) . . ? C33 C32 C31 120.9(5) . . ? C32 C33 C34 119.8(6) . . ? C35 C34 C33 119.8(6) . . ? C34 C35 C36 119.9(6) . . ? C35 C36 C31 120.9(5) . . ? C42 C37 C38 120.0(6) . . ? C42 C37 P3 124.9(4) . . ? C38 C37 P3 115.0(5) . . ? C39 C38 C37 120.0(9) . . ? C38 C39 C40 120.2(9) . . ? C39 C40 C41 121.0(8) . . ? C40 C41 C42 118.5(9) . . ? C37 C42 C41 120.2(7) . . ? C48 C43 C44 118.7(5) . . ? C48 C43 P4 125.1(4) . . ? C44 C43 P4 116.1(4) . . ? C45 C44 C43 120.3(6) . . ? C46 C45 C44 120.3(6) . . ? C45 C46 C47 120.8(6) . . ? C46 C47 C48 118.8(6) . . ? C43 C48 C47 121.1(5) . . ? C50 C49 C54 117.6(5) . . ? C50 C49 P4 117.6(4) . . ? C54 C49 P4 124.7(4) . . ? C49 C50 C51 121.3(5) . . ? C52 C51 C50 120.1(5) . . ? C51 C52 C53 119.8(5) . . ? C54 C53 C52 119.2(5) . . ? C53 C54 C49 121.9(5) . . ? F4 B1 F3 111.2(6) . . ? F4 B1 F1 110.8(6) . . ? F3 B1 F1 110.6(6) . . ? F4 B1 F2 107.7(6) . . ? F3 B1 F2 109.2(6) . . ? F1 B1 F2 107.1(6) . . ? Cl2 C1S Cl1 115.0(5) . . ? Cl4 C2S Cl3 111.5(5) . . ? Cl4B C2SB Cl3B 106(3) . . ? C2SB Cl3B Cl3B 118(3) . 3_566 ? C2SB Cl3B Cl4B 35(2) . . ? Cl3B Cl3B Cl4B 146(5) 3_566 . ? C2SB Cl4B Cl3B 38(2) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.676 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.090 #==END data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C276 H232 B4 Cl8 F16 P16 Pd2 S16' _chemical_formula_weight 5400.94 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' 'B' 'B' 0.0013 0.0007 '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' '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 22.527(4) _cell_length_b 16.736(3) _cell_length_c 17.944(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.40(3) _cell_angle_gamma 90.00 _cell_volume 6255(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD ' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26077 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.1323 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.23 _reflns_number_total 7653 _reflns_number_gt 4418 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7653 _refine_ls_number_parameters 519 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 4.528 _refine_ls_shift/su_mean 0.069 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 0.5000 0.0000 1.0000 0.0162(2) Uani 1 4 d S . . S1 S 0.38568(7) 0.08864(7) 0.71061(7) 0.0377(4) Uani 1 1 d . . . S3 S 0.28579(9) 0.08749(8) 0.52143(8) 0.0554(5) Uani 1 1 d . . . P1 P 0.45290(6) 0.09518(7) 0.89804(6) 0.0189(3) Uani 1 1 d . . . P3 P 0.19457(8) 0.10046(9) 0.34000(8) 0.0430(4) Uani 1 1 d . . . C1 C 0.4201(2) 0.0402(3) 0.8039(2) 0.0212(10) Uani 1 1 d . . . C3 C 0.3549(4) 0.0000 0.6557(4) 0.0325(18) Uani 1 2 d S . . C4 C 0.3129(4) 0.0000 0.5776(4) 0.0348(19) Uani 1 2 d S . . C5 C 0.2375(3) 0.0407(3) 0.4304(3) 0.0381(14) Uani 1 1 d . . . C10 C 0.3852(2) 0.1486(3) 0.9042(3) 0.0218(10) Uani 1 1 d . . . C11 C 0.3576(2) 0.1200(3) 0.9566(3) 0.0277(12) Uani 1 1 d . . . C12 C 0.3037(3) 0.1574(3) 0.9610(3) 0.0350(13) Uani 1 1 d . . . C13 C 0.2790(3) 0.2242(4) 0.9140(3) 0.0430(16) Uani 1 1 d . . . C14 C 0.3055(3) 0.2536(3) 0.8609(3) 0.0396(14) Uani 1 1 d . . . C15 C 0.3581(3) 0.2159(3) 0.8555(3) 0.0301(12) Uani 1 1 d . . . C20 C 0.5076(2) 0.1657(3) 0.8813(3) 0.0223(10) Uani 1 1 d . . . C21 C 0.5108(3) 0.2452(3) 0.9074(3) 0.0281(12) Uani 1 1 d . . . C22 C 0.5568(3) 0.2952(4) 0.8997(4) 0.0423(16) Uani 1 1 d . . . C23 C 0.6001(3) 0.2686(4) 0.8676(3) 0.0440(16) Uani 1 1 d . . . C24 C 0.5970(3) 0.1890(4) 0.8417(3) 0.0409(14) Uani 1 1 d . . . C25 C 0.5511(3) 0.1389(3) 0.8487(3) 0.0318(12) Uani 1 1 d . . . C50 C 0.1375(3) 0.1605(3) 0.3673(3) 0.0410(15) Uani 1 1 d . . . C51 C 0.1521(3) 0.2081(4) 0.4362(4) 0.0481(16) Uani 1 1 d . . . C52 C 0.1058(3) 0.2528(4) 0.4497(4) 0.0565(18) Uani 1 1 d . . . C53 C 0.0422(4) 0.2506(5) 0.3938(4) 0.071(2) Uani 1 1 d . . . C54 C 0.0279(4) 0.2027(5) 0.3258(4) 0.071(2) Uani 1 1 d . . . C55 C 0.0751(4) 0.1588(4) 0.3126(4) 0.058(2) Uani 1 1 d . . . C60 C 0.2577(3) 0.1728(3) 0.3453(3) 0.0422(15) Uani 1 1 d . . . C61 C 0.2515(4) 0.2543(4) 0.3484(3) 0.0470(16) Uani 1 1 d . . . C62 C 0.3001(4) 0.3043(5) 0.3432(4) 0.063(2) Uani 1 1 d . . . C63 C 0.3525(5) 0.2733(6) 0.3333(4) 0.072(2) Uani 1 1 d . . . C64 C 0.3591(5) 0.1917(6) 0.3312(5) 0.076(2) Uani 1 1 d . . . C65 C 0.3126(4) 0.1420(5) 0.3355(4) 0.0604(19) Uani 1 1 d . . . H11A H 0.376(2) 0.074(3) 0.988(3) 0.030(14) Uiso 1 1 d . . . H12A H 0.287(3) 0.141(4) 0.996(4) 0.06(2) Uiso 1 1 d . . . H13A H 0.244(3) 0.244(3) 0.918(3) 0.043(17) Uiso 1 1 d . . . H14A H 0.288(2) 0.306(3) 0.824(3) 0.029(13) Uiso 1 1 d . . . H15A H 0.379(2) 0.237(3) 0.822(3) 0.026(14) Uiso 1 1 d . . . H21A H 0.479(2) 0.265(3) 0.928(3) 0.033(15) Uiso 1 1 d . . . H22A H 0.557(3) 0.336(3) 0.908(4) 0.04(2) Uiso 1 1 d . . . H23A H 0.632(3) 0.308(4) 0.861(3) 0.063(19) Uiso 1 1 d . . . H24A H 0.627(3) 0.172(3) 0.820(3) 0.055(19) Uiso 1 1 d . . . H25A H 0.552(3) 0.090(3) 0.838(3) 0.042(17) Uiso 1 1 d . . . H51A H 0.197(3) 0.211(3) 0.480(3) 0.043(15) Uiso 1 1 d . . . H52A H 0.118(3) 0.292(4) 0.505(4) 0.08(2) Uiso 1 1 d . . . H53A H 0.010(3) 0.292(4) 0.410(4) 0.07(2) Uiso 1 1 d . . . H54A H -0.017(4) 0.196(5) 0.289(5) 0.12(3) Uiso 1 1 d . . . H55A H 0.071(4) 0.122(5) 0.267(5) 0.10(3) Uiso 1 1 d . . . H61A H 0.217(3) 0.271(4) 0.355(3) 0.05(2) Uiso 1 1 d . . . H62A H 0.293(3) 0.361(4) 0.345(4) 0.07(2) Uiso 1 1 d . . . H63A H 0.383(3) 0.305(3) 0.327(3) 0.037(16) Uiso 1 1 d . . . H64A H 0.398(4) 0.168(5) 0.327(4) 0.09(3) Uiso 1 1 d . . . H65A H 0.305(3) 0.079(5) 0.330(4) 0.09(3) Uiso 1 1 d . . . C1S C 0.18045(14) 0.0000 -0.2076(3) 0.049(2) Uani 1 2 d SD . . C2S C 0.1225(2) 0.0000 -0.2742(3) 0.063(3) Uani 1 2 d SD . . H2A H 0.1226 0.0000 -0.3260 0.19(7) Uiso 1 2 calc SR . . C3S C 0.06448(16) 0.0000 -0.2633(5) 0.077(3) Uani 1 2 d SD . . H3A H 0.0259 0.0000 -0.3078 0.6(3) Uiso 1 2 calc SR . . C4S C 0.0643(3) 0.0000 -0.1857(6) 0.074(3) Uani 1 2 d SD . . H4A H 0.0256 0.0000 -0.1784 0.14(5) Uiso 1 2 calc SR . . C5S C 0.1222(4) 0.0000 -0.1190(4) 0.074(3) Uani 1 2 d SD . . H5SA H 0.1221 0.0000 -0.0672 0.088 Uiso 1 2 calc SR . . C6S C 0.1803(3) 0.0000 -0.1299(3) 0.057(3) Uani 1 2 d SD . . H6A H 0.2189 0.0000 -0.0854 0.17(6) Uiso 1 2 calc SR . . C7S C 0.2422(3) 0.0000 -0.2209(6) 0.071(3) Uani 1 2 d SD . . H7SA H 0.2331 0.0000 -0.2777 0.106 Uiso 1 2 calc SR . . H7SB H 0.2666 -0.0468 -0.1968 0.106 Uiso 0.50 1 calc PR . . H7SC H 0.2666 0.0468 -0.1968 0.106 Uiso 0.50 1 calc PR . . Cl1 Cl 0.08346(16) 0.08336(13) 0.09546(17) 0.1403(13) Uani 1 1 d . . . C8S C 0.1317(5) 0.0000 0.1276(7) 0.053(3) Uani 1 2 d S . . H8A H 0.149(5) 0.0000 0.093(6) 0.08(4) Uiso 1 2 d S . . H8B H 0.146(4) 0.0000 0.184(6) 0.06(3) Uiso 1 2 d S . . F1 F 0.3547(4) 0.0000 0.2124(4) 0.106(2) Uani 1 2 d S . . F2 F 0.2698(2) 0.0684(2) 0.1283(3) 0.0879(14) Uani 1 1 d . . . F4 F 0.3356(3) 0.0000 0.0838(3) 0.0666(15) Uani 1 2 d S . . B1 B 0.3054(5) 0.0000 0.1369(6) 0.046(3) Uani 1 2 d S . . C11S C 0.03395(17) -0.0111(9) 0.4939(9) 0.054(6) Uiso 0.25 1 d PD A -1 C12S C 0.0132(5) 0.0663(8) 0.4998(14) 0.030(6) Uiso 0.25 1 d PD A -1 H12B H 0.0400 0.1096 0.5035 0.036 Uiso 0.25 1 calc PR A -1 C13S C -0.0479(7) 0.0787(9) 0.5001(17) 0.068(9) Uiso 0.25 1 d PD A -1 H13B H -0.0629 0.1304 0.5005 0.081 Uiso 0.25 1 calc PR A -1 C14S C -0.0866(6) 0.0134(11) 0.4998(15) 0.058(8) Uiso 0.25 1 d PD A -1 H14B H -0.1253 0.0212 0.5062 0.069 Uiso 0.25 1 calc PR A -1 C15S C -0.0671(6) -0.0636(10) 0.4899(19) 0.093(12) Uiso 0.25 1 d PD A -1 H15B H -0.0943 -0.1068 0.4849 0.111 Uiso 0.25 1 calc PR A -1 C16S C -0.0066(7) -0.0758(9) 0.487(2) 0.089(12) Uiso 0.25 1 d PD A -1 H16A H 0.0066 -0.1272 0.4813 0.107 Uiso 0.25 1 calc PR A -1 C17S C 0.1008(5) -0.0248(11) 0.4976(19) 0.109(9) Uiso 0.25 1 d PD A -1 H17D H 0.1070 -0.0807 0.4913 0.163 Uiso 0.25 1 calc PR A -1 H17A H 0.1312 -0.0069 0.5488 0.163 Uiso 0.25 1 calc PR A -1 H17B H 0.1070 0.0046 0.4552 0.163 Uiso 0.25 1 calc PR A -1 C21S C 0.4970(5) -0.0161(18) 0.3936(7) 0.086(10) Uiso 0.25 1 d PD B -2 C22S C 0.4466(6) 0.0209(16) 0.4074(10) 0.091(11) Uiso 0.25 1 d PD B -2 H22B H 0.4114 0.0401 0.3642 0.109 Uiso 0.25 1 calc PR B -2 C23S C 0.4491(9) 0.029(2) 0.4859(12) 0.098(15) Uiso 0.25 1 d PD B -2 H23B H 0.4160 0.0549 0.4952 0.117 Uiso 0.25 1 calc PR B -2 C24S C 0.5013(10) -0.001(4) 0.5505(7) 0.081(7) Uiso 0.50 2 d SPD B -2 H24B H 0.5019 0.0015 0.6025 0.097 Uiso 0.50 2 calc SPR B -2 C25S C 0.5527(10) -0.036(2) 0.5369(9) 0.071(10) Uiso 0.25 1 d PD B -2 H25B H 0.5884 -0.0540 0.5802 0.085 Uiso 0.25 1 calc PR B -2 C26S C 0.5505(8) -0.0433(19) 0.4585(11) 0.111(13) Uiso 0.25 1 d PD B -2 H26A H 0.5847 -0.0664 0.4495 0.133 Uiso 0.25 1 calc PR B -2 C27S C 0.4936(16) -0.027(4) 0.3091(8) 0.69(12) Uiso 0.25 1 d PD B -2 H27A H 0.4496 -0.0242 0.2722 1.038 Uiso 0.25 1 calc PR B -2 H27B H 0.5114 -0.0776 0.3043 1.038 Uiso 0.25 1 calc PR B -2 H27C H 0.5176 0.0151 0.2967 1.038 Uiso 0.25 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0191(4) 0.0161(4) 0.0105(3) 0.000 0.0026(3) 0.000 S1 0.0611(10) 0.0227(6) 0.0142(6) 0.0029(5) -0.0028(6) -0.0021(6) S3 0.0895(13) 0.0260(7) 0.0198(7) 0.0019(6) -0.0138(7) -0.0001(7) P1 0.0236(7) 0.0177(6) 0.0120(5) -0.0003(4) 0.0029(5) 0.0002(5) P3 0.0599(10) 0.0325(8) 0.0187(7) 0.0026(6) -0.0050(7) -0.0007(7) C1 0.026(3) 0.024(2) 0.010(2) -0.0001(17) 0.0033(18) -0.001(2) C3 0.056(5) 0.018(3) 0.013(3) 0.000 0.002(3) 0.000 C4 0.055(5) 0.014(3) 0.022(4) 0.000 0.000(3) 0.000 C5 0.053(4) 0.032(3) 0.017(2) -0.003(2) -0.002(2) -0.001(3) C10 0.025(3) 0.021(2) 0.016(2) -0.0013(18) 0.0032(19) 0.004(2) C11 0.026(3) 0.027(3) 0.025(3) -0.004(2) 0.003(2) -0.002(2) C12 0.032(3) 0.041(3) 0.034(3) -0.007(3) 0.014(3) -0.003(3) C13 0.027(3) 0.057(4) 0.034(3) -0.016(3) 0.000(3) 0.013(3) C14 0.046(4) 0.041(3) 0.025(3) 0.004(2) 0.006(3) 0.022(3) C15 0.035(3) 0.033(3) 0.019(2) 0.002(2) 0.007(2) 0.006(2) C20 0.021(2) 0.022(2) 0.017(2) 0.0047(18) -0.0012(18) -0.0027(19) C21 0.032(3) 0.024(3) 0.024(3) -0.001(2) 0.006(2) -0.004(2) C22 0.047(4) 0.025(3) 0.046(4) 0.002(3) 0.009(3) -0.008(3) C23 0.037(3) 0.046(4) 0.040(3) 0.013(3) 0.005(3) -0.014(3) C24 0.033(3) 0.055(4) 0.040(3) 0.013(3) 0.019(3) -0.003(3) C25 0.034(3) 0.032(3) 0.029(3) 0.000(2) 0.012(2) 0.004(3) C50 0.051(4) 0.028(3) 0.030(3) 0.009(2) 0.000(3) -0.005(3) C51 0.045(4) 0.054(4) 0.035(3) -0.002(3) 0.003(3) -0.004(3) C52 0.060(5) 0.064(4) 0.037(4) 0.004(3) 0.009(3) 0.002(4) C53 0.070(5) 0.084(6) 0.054(5) 0.009(4) 0.017(4) 0.010(5) C54 0.058(5) 0.089(6) 0.050(4) 0.009(4) 0.002(4) 0.001(5) C55 0.065(5) 0.059(4) 0.029(3) 0.008(3) -0.005(3) 0.000(4) C60 0.062(4) 0.040(3) 0.020(3) 0.004(2) 0.012(3) 0.001(3) C61 0.056(4) 0.048(4) 0.028(3) 0.000(3) 0.007(3) 0.005(4) C62 0.088(6) 0.053(5) 0.039(4) 0.005(3) 0.015(4) -0.017(4) C63 0.077(6) 0.101(7) 0.049(4) 0.004(4) 0.036(4) -0.030(6) C64 0.089(7) 0.093(7) 0.060(5) -0.008(5) 0.042(5) -0.008(6) C65 0.080(6) 0.061(5) 0.041(4) -0.004(3) 0.024(4) 0.000(4) C1S 0.055(6) 0.042(5) 0.040(5) 0.000 0.007(4) 0.000 C2S 0.056(7) 0.055(6) 0.064(7) 0.000 0.007(5) 0.000 C3S 0.070(8) 0.064(7) 0.076(8) 0.000 0.005(6) 0.000 C4S 0.063(8) 0.039(6) 0.120(11) 0.000 0.035(7) 0.000 C5S 0.121(10) 0.035(5) 0.093(9) 0.000 0.072(8) 0.000 C6S 0.075(7) 0.030(5) 0.057(6) 0.000 0.015(6) 0.000 C7S 0.054(7) 0.083(8) 0.064(7) 0.000 0.009(5) 0.000 Cl1 0.188(3) 0.0553(13) 0.118(2) 0.0110(13) -0.0080(19) 0.0415(16) C8S 0.064(7) 0.044(5) 0.052(6) 0.000 0.023(6) 0.000 F1 0.135(6) 0.114(6) 0.053(4) 0.000 0.016(4) 0.000 F2 0.089(3) 0.050(2) 0.149(4) 0.001(3) 0.073(3) 0.016(2) F4 0.080(4) 0.056(3) 0.084(4) 0.000 0.053(3) 0.000 B1 0.068(7) 0.031(5) 0.047(6) 0.000 0.030(6) 0.000 _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 P1 2.3518(12) 6 ? Pd1 P1 2.3518(12) 2_657 ? Pd1 P1 2.3518(12) . ? Pd1 P1 2.3518(12) 5_657 ? S1 C1 1.752(4) . ? S1 C3 1.770(4) . ? S3 C4 1.751(4) . ? S3 C5 1.763(5) . ? P1 C10 1.806(5) . ? P1 C20 1.813(5) . ? P1 C1 1.815(4) . ? P3 C5 1.837(5) . ? P3 C50 1.839(6) . ? P3 C60 1.843(6) . ? C1 C1 1.346(9) 6 ? C3 C4 1.358(9) . ? C3 S1 1.770(4) 6 ? C4 S3 1.751(4) 6 ? C5 C5 1.361(10) 6 ? C10 C11 1.395(7) . ? C10 C15 1.414(6) . ? C11 C12 1.396(7) . ? C12 C13 1.382(8) . ? C13 C14 1.393(9) . ? C14 C15 1.379(8) . ? C20 C25 1.392(7) . ? C20 C21 1.404(6) . ? C21 C22 1.380(8) . ? C22 C23 1.382(9) . ? C23 C24 1.402(9) . ? C24 C25 1.374(8) . ? C50 C55 1.374(8) . ? C50 C51 1.399(8) . ? C51 C52 1.378(9) . ? C52 C53 1.403(10) . ? C53 C54 1.391(11) . ? C54 C55 1.386(11) . ? C60 C61 1.374(8) . ? C60 C65 1.411(9) . ? C61 C62 1.410(10) . ? C62 C63 1.360(11) . ? C63 C64 1.377(12) . ? C64 C65 1.363(11) . ? C1S C2S 1.3945(19) . ? C1S C6S 1.3947(18) . ? C1S C7S 1.5000(3) . ? C2S C3S 1.3942(18) . ? C3S C4S 1.3940(18) . ? C4S C5S 1.3950(19) . ? C5S C6S 1.3942(18) . ? Cl1 C8S 1.726(7) . ? C8S Cl1 1.726(7) 6 ? F1 B1 1.386(12) . ? F2 B1 1.372(7) . ? F4 B1 1.365(11) . ? B1 F2 1.372(7) 6 ? C11S C16S 1.3942(19) . ? C11S C12S 1.3944(19) . ? C11S C17S 1.5000(3) . ? C12S C13S 1.3940(19) . ? C13S C14S 1.3964(19) . ? C14S C15S 1.3951(19) . ? C15S C16S 1.3945(19) . ? C21S C22S 1.3946(19) . ? C21S C26S 1.3953(19) . ? C21S C27S 1.5000(4) . ? C22S C23S 1.3950(19) . ? C23S C24S 1.3953(19) . ? C24S C25S 1.3954(18) . ? C25S C26S 1.3946(19) . ? 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 P1 Pd1 P1 180.0 6 2_657 ? P1 Pd1 P1 85.27(6) 6 . ? P1 Pd1 P1 94.73(6) 2_657 . ? P1 Pd1 P1 94.73(6) 6 5_657 ? P1 Pd1 P1 85.27(6) 2_657 5_657 ? P1 Pd1 P1 180.0 . 5_657 ? C1 S1 C3 94.7(2) . . ? C4 S3 C5 96.8(3) . . ? C10 P1 C20 109.4(2) . . ? C10 P1 C1 104.7(2) . . ? C20 P1 C1 103.7(2) . . ? C10 P1 Pd1 115.38(15) . . ? C20 P1 Pd1 115.87(14) . . ? C1 P1 Pd1 106.48(14) . . ? C5 P3 C50 104.4(2) . . ? C5 P3 C60 100.1(2) . . ? C50 P3 C60 103.4(3) . . ? C1 C1 S1 117.54(15) 6 . ? C1 C1 P1 120.45(14) 6 . ? S1 C1 P1 122.0(3) . . ? C4 C3 S1 123.04(17) . . ? C4 C3 S1 123.04(17) . 6 ? S1 C3 S1 113.9(3) . 6 ? C3 C4 S3 123.15(19) . 6 ? C3 C4 S3 123.15(19) . . ? S3 C4 S3 113.5(4) 6 . ? C5 C5 S3 116.39(17) 6 . ? C5 C5 P3 123.01(16) 6 . ? S3 C5 P3 120.5(3) . . ? C11 C10 C15 119.5(5) . . ? C11 C10 P1 118.4(3) . . ? C15 C10 P1 122.1(4) . . ? C10 C11 C12 120.3(5) . . ? C13 C12 C11 119.0(6) . . ? C12 C13 C14 121.7(6) . . ? C15 C14 C13 119.3(5) . . ? C14 C15 C10 120.1(5) . . ? C25 C20 C21 119.5(5) . . ? C25 C20 P1 119.5(4) . . ? C21 C20 P1 120.8(4) . . ? C22 C21 C20 119.1(6) . . ? C23 C22 C21 121.5(6) . . ? C22 C23 C24 119.4(6) . . ? C25 C24 C23 119.6(6) . . ? C24 C25 C20 121.0(5) . . ? C55 C50 C51 118.4(6) . . ? C55 C50 P3 115.3(5) . . ? C51 C50 P3 126.4(5) . . ? C52 C51 C50 121.7(6) . . ? C51 C52 C53 119.8(7) . . ? C54 C53 C52 118.2(8) . . ? C55 C54 C53 121.3(7) . . ? C50 C55 C54 120.7(7) . . ? C61 C60 C65 118.4(6) . . ? C61 C60 P3 124.4(5) . . ? C65 C60 P3 116.6(5) . . ? C60 C61 C62 119.5(7) . . ? C63 C62 C61 121.1(8) . . ? C62 C63 C64 119.4(8) . . ? C65 C64 C63 120.6(9) . . ? C64 C65 C60 120.9(8) . . ? C2S C1S C6S 119.95(12) . . ? C2S C1S C7S 119.0(6) . . ? C6S C1S C7S 121.0(5) . . ? C3S C2S C1S 120.01(12) . . ? C2S C3S C4S 120.04(13) . . ? C3S C4S C5S 119.97(12) . . ? C6S C5S C4S 119.99(12) . . ? C5S C6S C1S 120.04(13) . . ? Cl1 C8S Cl1 107.8(6) 6 . ? F4 B1 F2 110.3(5) . . ? F4 B1 F2 110.3(5) . 6 ? F2 B1 F2 113.0(9) . 6 ? F4 B1 F1 104.8(9) . . ? F2 B1 F1 109.1(6) . . ? F2 B1 F1 109.1(6) 6 . ? C16S C11S C12S 120.03(13) . . ? C16S C11S C17S 120.00(15) . . ? C12S C11S C17S 119.94(15) . . ? C13S C12S C11S 119.90(13) . . ? C12S C13S C14S 119.96(16) . . ? C15S C14S C13S 119.81(17) . . ? C16S C15S C14S 119.91(14) . . ? C11S C16S C15S 120.02(13) . . ? C22S C21S C26S 119.96(13) . . ? C22S C21S C27S 120.04(12) . . ? C26S C21S C27S 120.00(12) . . ? C21S C22S C23S 120.03(13) . . ? C22S C23S C24S 119.97(15) . . ? C25S C24S C23S 119.93(16) . . ? C26S C25S C24S 120.00(14) . . ? C25S C26S C21S 120.00(13) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.856 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.107 #==END data_new1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 B Cl4 F4 P4 Pt0.50 S4' _chemical_formula_weight 1295.19 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 P2(1)/c _symmetry_Int_Tables_number 14 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 17.109(3) _cell_length_b 19.069(4) _cell_length_c 19.339(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.17(3) _cell_angle_gamma 90.00 _cell_volume 5710(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular box' _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 1.735 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31256 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.21 _reflns_number_total 9020 _reflns_number_gt 6209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9020 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.005 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.5000 1.0000 1.0000 0.02327(15) Uani 1 2 d S . . P1 P 1.38837(11) 0.92417(9) 0.92626(10) 0.0279(5) Uani 1 1 d . . . P2 P 1.39100(11) 1.08348(9) 0.97448(10) 0.0265(5) Uani 1 1 d . . . P3 P 0.82028(13) 0.89973(11) 0.71574(13) 0.0449(6) Uani 1 1 d . . . P4 P 0.80331(13) 1.06684(11) 0.76359(12) 0.0409(6) Uani 1 1 d . . . S1 S 1.20318(11) 0.94939(9) 0.79890(10) 0.0357(5) Uani 1 1 d . . . S2 S 1.20184(11) 1.09647(9) 0.84778(11) 0.0358(5) Uani 1 1 d . . . S3 S 0.99766(11) 0.94394(10) 0.71988(11) 0.0401(5) Uani 1 1 d . . . S4 S 0.98486(11) 1.08867(10) 0.76472(11) 0.0400(5) Uani 1 1 d . . . C1 C 1.2960(4) 0.9803(3) 0.8748(4) 0.0285(18) Uani 1 1 d . . . C2 C 1.2959(4) 1.0467(3) 0.8975(4) 0.0299(18) Uani 1 1 d . . . C3 C 1.1400(4) 1.0224(4) 0.7995(4) 0.0329(19) Uani 1 1 d . . . C4 C 1.0537(5) 1.0196(4) 0.7654(4) 0.0343(19) Uani 1 1 d . . . C5 C 0.9043(4) 0.9647(4) 0.7335(4) 0.039(2) Uani 1 1 d . . . C6 C 0.8979(4) 1.0321(4) 0.7520(4) 0.039(2) Uani 1 1 d . . . C10 C 1.3985(4) 0.8753(4) 0.8508(4) 0.035(2) Uani 1 1 d . . . C20 C 1.3540(4) 0.8638(3) 0.9807(4) 0.0315(19) Uani 1 1 d . . . C21 C 1.3845(5) 0.8732(4) 1.0591(4) 0.041(2) Uani 1 1 d . . . H21A H 1.4246 0.9083 1.0833 0.050 Uiso 1 1 calc R . . C30 C 1.3623(4) 1.0999(3) 1.0525(4) 0.0299(18) Uani 1 1 d . . . C60 C 0.8789(5) 0.8309(4) 0.7834(4) 0.044(2) Uani 1 1 d . . . C70 C 0.7221(5) 1.0716(4) 0.6636(5) 0.045(2) Uani 1 1 d . . . C71 C 0.7401(6) 1.0743(4) 0.6007(5) 0.054(2) Uani 1 1 d . . . H71A H 0.7974 1.0749 0.6080 0.065 Uiso 1 1 calc R . . C31 C 1.4015(5) 1.0602(4) 1.1192(4) 0.038(2) Uani 1 1 d . . . H31A H 1.4436 1.0274 1.1235 0.045 Uiso 1 1 calc R . . C50 C 0.8114(6) 0.8642(5) 0.6248(5) 0.056(3) Uani 1 1 d . . . C32 C 1.3784(5) 1.0693(5) 1.1784(5) 0.049(2) Uani 1 1 d . . . H32A H 1.4055 1.0434 1.2230 0.059 Uiso 1 1 calc R . . C35 C 1.2973(5) 1.1485(4) 1.0457(5) 0.045(2) Uani 1 1 d . . . H35A H 1.2696 1.1748 1.0014 0.054 Uiso 1 1 calc R . . C62 C 0.8796(7) 0.7102(5) 0.8244(5) 0.072(3) Uani 1 1 d . . . H62A H 0.8548 0.6659 0.8161 0.087 Uiso 1 1 calc R . . C45 C 1.4128(5) 1.2304(4) 0.9719(5) 0.044(2) Uani 1 1 d . . . H45A H 1.4152 1.2319 1.0208 0.053 Uiso 1 1 calc R . . C41 C 1.3992(5) 1.1655(4) 0.8607(5) 0.044(2) Uani 1 1 d . . . H41A H 1.3914 1.1232 0.8346 0.053 Uiso 1 1 calc R . . C25 C 1.2936(5) 0.8119(4) 0.9448(5) 0.046(2) Uani 1 1 d . . . H25A H 1.2718 0.8060 0.8922 0.055 Uiso 1 1 calc R . . C33 C 1.3140(5) 1.1177(5) 1.1715(5) 0.059(3) Uani 1 1 d . . . H33A H 1.2975 1.1235 1.2112 0.071 Uiso 1 1 calc R . . C40 C 1.4015(4) 1.1668(3) 0.9341(4) 0.0299(18) Uani 1 1 d . . . C11 C 1.4220(5) 0.8046(4) 0.8599(5) 0.048(2) Uani 1 1 d . . . H11A H 1.4266 0.7806 0.9033 0.057 Uiso 1 1 calc R . . C15 C 1.3887(4) 0.9099(4) 0.7852(4) 0.041(2) Uani 1 1 d . . . H15A H 1.3721 0.9568 0.7789 0.050 Uiso 1 1 calc R . . C61 C 0.8410(6) 0.7634(4) 0.7713(5) 0.052(2) Uani 1 1 d . . . H61A H 0.7904 0.7544 0.7278 0.062 Uiso 1 1 calc R . . C75 C 0.6361(5) 1.0709(4) 0.6513(5) 0.057(2) Uani 1 1 d . . . H75A H 0.6224 1.0699 0.6930 0.068 Uiso 1 1 calc R . . C24 C 1.2657(5) 0.7689(4) 0.9870(5) 0.055(2) Uani 1 1 d . . . H24A H 1.2268 0.7329 0.9629 0.066 Uiso 1 1 calc R . . C22 C 1.3557(5) 0.8306(4) 1.1016(5) 0.054(2) Uani 1 1 d . . . H22A H 1.3768 0.8368 1.1541 0.065 Uiso 1 1 calc R . . C14 C 1.4032(5) 0.8759(5) 0.7282(5) 0.058(3) Uani 1 1 d . . . H14A H 1.3960 0.8993 0.6837 0.069 Uiso 1 1 calc R . . C81 C 0.8443(5) 1.2067(4) 0.7344(5) 0.054(2) Uani 1 1 d . . . H81A H 0.8273 1.1933 0.6838 0.065 Uiso 1 1 calc R . . C80 C 0.8364(5) 1.1591(4) 0.7865(4) 0.042(2) Uani 1 1 d . . . C23 C 1.2950(5) 0.7786(4) 1.0653(5) 0.056(3) Uani 1 1 d . . . H23A H 1.2742 0.7506 1.0932 0.067 Uiso 1 1 calc R . . C42 C 1.4086(5) 1.2274(5) 0.8271(5) 0.061(3) Uani 1 1 d . . . H42A H 1.4070 1.2267 0.7784 0.073 Uiso 1 1 calc R . . C44 C 1.4206(6) 1.2922(4) 0.9367(6) 0.068(3) Uani 1 1 d . . . H44A H 1.4261 1.3350 0.9614 0.081 Uiso 1 1 calc R . . Cl2 Cl 0.8423(2) 1.05285(18) 0.0197(2) 0.1107(11) Uani 1 1 d . . . Cl1 Cl 0.9349(2) 0.92515(19) 0.0280(2) 0.1178(12) Uani 1 1 d . . . C82 C 0.8766(5) 1.2729(5) 0.7572(5) 0.058(3) Uani 1 1 d . . . H82A H 0.8841 1.3033 0.7229 0.070 Uiso 1 1 calc R . . C72 C 0.6754(6) 1.0760(5) 0.5268(5) 0.067(3) Uani 1 1 d . . . H72A H 0.6889 1.0787 0.4851 0.080 Uiso 1 1 calc R . . C73 C 0.5908(7) 1.0738(5) 0.5164(6) 0.073(3) Uani 1 1 d . . . H73A H 0.5469 1.0738 0.4671 0.087 Uiso 1 1 calc R . . C84 C 0.8905(7) 1.2484(5) 0.8831(5) 0.071(3) Uani 1 1 d . . . H84A H 0.9059 1.2624 0.9333 0.086 Uiso 1 1 calc R . . C83 C 0.8982(6) 1.2941(4) 0.8319(5) 0.061(3) Uani 1 1 d . . . H83A H 0.9179 1.3395 0.8471 0.074 Uiso 1 1 calc R . . C43 C 1.4202(6) 1.2897(5) 0.8660(6) 0.064(3) Uani 1 1 d . . . H43A H 1.4279 1.3308 0.8437 0.077 Uiso 1 1 calc R . . C13 C 1.4285(6) 0.8066(6) 0.7391(6) 0.077(3) Uani 1 1 d . . . H13A H 1.4392 0.7836 0.7016 0.092 Uiso 1 1 calc R . . C34 C 1.2757(6) 1.1558(5) 1.1066(5) 0.058(3) Uani 1 1 d . . . H34A H 1.2334 1.1881 1.1028 0.069 Uiso 1 1 calc R . . C12 C 1.4385(6) 0.7704(5) 0.8045(7) 0.073(3) Uani 1 1 d . . . H12A H 1.4560 0.7237 0.8110 0.088 Uiso 1 1 calc R . . C85 C 0.8598(6) 1.1815(4) 0.8601(5) 0.059(3) Uani 1 1 d . . . H85A H 0.8549 1.1507 0.8954 0.071 Uiso 1 1 calc R . . C1S C 0.8663(9) 0.9885(5) -0.0311(7) 0.112(5) Uani 1 1 d . . . H1SA H 0.8931 1.0100 -0.0611 0.135 Uiso 1 1 calc R . . H1SB H 0.8131 0.9664 -0.0661 0.135 Uiso 1 1 calc R . . C51 C 0.8659(7) 0.8160(5) 0.6169(5) 0.068(3) Uani 1 1 d . . . H51A H 0.9094 0.7963 0.6602 0.081 Uiso 1 1 calc R . . C65 C 0.9533(6) 0.8424(5) 0.8498(5) 0.063(3) Uani 1 1 d . . . H65A H 0.9776 0.8869 0.8603 0.076 Uiso 1 1 calc R . . C74 C 0.5702(6) 1.0715(5) 0.5777(7) 0.077(3) Uani 1 1 d . . . H74A H 0.5127 1.0705 0.5701 0.093 Uiso 1 1 calc R . . C63 C 0.9536(8) 0.7228(5) 0.8884(6) 0.086(4) Uani 1 1 d . . . H63A H 0.9785 0.6872 0.9239 0.103 Uiso 1 1 calc R . . C55 C 0.7452(7) 0.8923(6) 0.5595(6) 0.099(5) Uani 1 1 d . . . H55A H 0.7077 0.9252 0.5644 0.119 Uiso 1 1 calc R . . C53 C 0.7920(15) 0.8257(9) 0.4827(9) 0.135(9) Uani 1 1 d . . . H53A H 0.7862 0.8138 0.4341 0.162 Uiso 1 1 calc R . . C64 C 0.9914(7) 0.7884(5) 0.9004(5) 0.095(4) Uani 1 1 d . . . H64A H 1.0431 0.7962 0.9431 0.113 Uiso 1 1 calc R . . C52 C 0.8568(10) 0.7959(7) 0.5442(8) 0.115(5) Uani 1 1 d . . . H52A H 0.8938 0.7632 0.5382 0.138 Uiso 1 1 calc R . . C54 C 0.7354(13) 0.8722(10) 0.4892(8) 0.152(9) Uani 1 1 d . . . H54A H 0.6902 0.8899 0.4458 0.182 Uiso 1 1 calc R . . Cl4 Cl 0.9064(3) 0.9799(2) 0.40177(19) 0.1164(12) Uani 1 1 d . . . Cl3 Cl 0.8537(3) 1.09197(19) 0.4696(3) 0.1554(18) Uani 1 1 d . . . F4 F 1.5130(4) 0.9377(3) 0.2243(3) 0.100(2) Uani 1 1 d . . . F3 F 1.6535(4) 0.9304(3) 0.3013(3) 0.0923(19) Uani 1 1 d . . . F2 F 1.5603(5) 0.8627(4) 0.3222(4) 0.115(2) Uani 1 1 d . . . F1 F 1.5627(5) 0.9776(4) 0.3447(4) 0.110(2) Uani 1 1 d . . . B1 B 1.5702(9) 0.9270(7) 0.2983(7) 0.069(3) Uani 1 1 d . . . C2S C 0.8428(12) 1.0068(6) 0.4412(12) 0.173(9) Uani 1 1 d . . . H2SA H 0.8534 0.9775 0.4853 0.208 Uiso 1 1 calc R . . H2SB H 0.7833 0.9992 0.4049 0.208 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 Pt1 0.01907(19) 0.02192(19) 0.0239(2) -0.00052(18) 0.00435(14) 0.00113(17) P1 0.0214(9) 0.0240(9) 0.0305(10) -0.0005(8) 0.0035(8) 0.0017(7) P2 0.0227(9) 0.0231(9) 0.0281(10) -0.0018(8) 0.0055(8) 0.0019(7) P3 0.0321(11) 0.0432(12) 0.0545(14) 0.0076(10) 0.0136(10) -0.0027(9) P4 0.0335(11) 0.0417(12) 0.0455(13) 0.0019(10) 0.0147(10) 0.0051(9) S1 0.0262(9) 0.0335(10) 0.0352(10) -0.0057(8) 0.0015(8) 0.0020(8) S2 0.0226(9) 0.0281(9) 0.0430(11) -0.0002(8) 0.0009(8) 0.0023(7) S3 0.0266(10) 0.0365(10) 0.0488(12) -0.0093(9) 0.0078(9) -0.0027(8) S4 0.0260(10) 0.0344(10) 0.0495(12) -0.0030(9) 0.0064(9) 0.0031(8) C1 0.020(3) 0.032(4) 0.030(4) 0.000(3) 0.007(3) -0.002(3) C2 0.021(3) 0.032(4) 0.032(4) 0.012(3) 0.007(3) 0.005(3) C3 0.028(4) 0.033(4) 0.033(4) -0.003(3) 0.008(3) -0.001(3) C4 0.037(4) 0.030(4) 0.031(4) -0.001(3) 0.009(3) 0.000(3) C5 0.027(4) 0.044(5) 0.037(4) 0.006(4) 0.005(3) -0.002(4) C6 0.028(4) 0.034(4) 0.042(5) 0.003(4) 0.002(3) -0.003(3) C10 0.019(4) 0.041(4) 0.034(4) -0.015(4) 0.000(3) -0.001(3) C20 0.031(4) 0.024(4) 0.028(4) 0.007(3) 0.001(3) 0.002(3) C21 0.033(4) 0.031(4) 0.048(5) 0.009(4) 0.006(4) 0.005(3) C30 0.020(3) 0.031(4) 0.034(4) 0.000(3) 0.006(3) -0.003(3) C60 0.060(5) 0.038(4) 0.037(5) 0.000(4) 0.024(4) 0.002(4) C70 0.039(5) 0.040(5) 0.047(5) 0.004(4) 0.010(4) 0.009(4) C71 0.050(5) 0.059(6) 0.050(6) 0.005(5) 0.017(5) 0.011(4) C31 0.035(4) 0.041(4) 0.035(5) -0.002(4) 0.013(4) 0.002(3) C50 0.058(6) 0.059(6) 0.040(5) -0.001(4) 0.009(5) -0.034(5) C32 0.046(5) 0.068(6) 0.035(5) 0.001(4) 0.019(4) -0.005(4) C35 0.034(4) 0.046(5) 0.048(5) 0.000(4) 0.011(4) 0.008(4) C62 0.117(9) 0.045(5) 0.049(6) -0.001(5) 0.030(6) -0.008(6) C45 0.036(4) 0.032(4) 0.053(5) 0.002(4) 0.007(4) -0.006(3) C41 0.038(5) 0.044(5) 0.046(5) 0.011(4) 0.015(4) -0.003(4) C25 0.039(4) 0.041(5) 0.042(5) 0.005(4) 0.002(4) -0.006(4) C33 0.044(5) 0.095(8) 0.049(6) -0.011(5) 0.030(5) -0.002(5) C40 0.018(3) 0.023(4) 0.039(4) 0.000(3) 0.003(3) -0.005(3) C11 0.041(5) 0.035(4) 0.051(5) -0.018(4) 0.004(4) 0.005(4) C15 0.030(4) 0.057(5) 0.037(5) -0.012(4) 0.015(4) -0.002(4) C61 0.064(6) 0.045(5) 0.043(5) -0.004(4) 0.021(4) -0.003(4) C75 0.030(5) 0.067(6) 0.068(6) 0.012(5) 0.017(4) 0.007(4) C24 0.055(5) 0.036(5) 0.059(6) 0.001(4) 0.011(5) -0.022(4) C22 0.053(5) 0.063(6) 0.043(5) 0.016(5) 0.017(4) 0.002(5) C14 0.046(5) 0.084(7) 0.044(5) -0.017(5) 0.020(4) -0.008(5) C81 0.057(5) 0.043(5) 0.046(5) 0.000(4) 0.006(4) 0.006(4) C80 0.039(5) 0.041(5) 0.044(5) -0.003(4) 0.018(4) 0.009(4) C23 0.052(5) 0.049(5) 0.066(6) 0.021(5) 0.023(5) -0.012(4) C42 0.048(5) 0.071(7) 0.057(6) 0.028(5) 0.015(5) -0.005(5) C44 0.062(6) 0.033(5) 0.098(8) 0.000(5) 0.025(6) -0.008(4) Cl2 0.127(3) 0.102(2) 0.124(3) 0.025(2) 0.074(2) 0.026(2) Cl1 0.113(3) 0.113(3) 0.127(3) 0.029(2) 0.051(2) 0.018(2) C82 0.061(6) 0.053(6) 0.050(6) 0.014(5) 0.015(5) 0.005(5) C72 0.057(6) 0.080(7) 0.054(6) 0.003(5) 0.014(5) 0.009(5) C73 0.061(7) 0.084(8) 0.054(7) 0.005(6) 0.007(6) 0.011(6) C84 0.119(9) 0.050(6) 0.050(6) -0.004(5) 0.041(6) -0.016(6) C83 0.079(7) 0.038(5) 0.059(6) 0.002(5) 0.022(5) -0.005(5) C43 0.053(6) 0.044(6) 0.087(8) 0.029(6) 0.022(6) -0.007(4) C13 0.061(6) 0.085(8) 0.076(8) -0.053(7) 0.021(6) -0.003(6) C34 0.052(6) 0.079(7) 0.053(6) -0.003(5) 0.033(5) 0.017(5) C12 0.058(6) 0.055(6) 0.090(8) -0.032(6) 0.016(6) 0.013(5) C85 0.099(8) 0.044(5) 0.044(5) 0.008(4) 0.039(5) -0.005(5) C1S 0.138(12) 0.083(9) 0.066(7) 0.017(6) -0.005(7) -0.013(8) C51 0.082(7) 0.079(7) 0.054(6) -0.031(5) 0.040(6) -0.047(6) C65 0.080(7) 0.046(5) 0.047(5) 0.001(4) 0.010(5) -0.012(5) C74 0.040(5) 0.088(8) 0.085(8) 0.022(6) 0.009(6) 0.011(5) C63 0.135(10) 0.050(6) 0.051(6) 0.011(5) 0.018(7) 0.000(6) C55 0.108(9) 0.073(7) 0.057(7) 0.015(6) -0.024(6) -0.050(6) C53 0.25(3) 0.118(14) 0.069(10) -0.055(11) 0.096(14) -0.106(15) C64 0.110(9) 0.072(7) 0.052(6) 0.019(5) -0.014(6) -0.019(7) C52 0.145(13) 0.130(12) 0.082(9) -0.056(9) 0.060(9) -0.089(10) C54 0.21(2) 0.136(15) 0.049(9) 0.018(9) -0.003(10) -0.114(14) Cl4 0.144(3) 0.122(3) 0.082(2) -0.0117(19) 0.047(2) 0.025(2) Cl3 0.171(4) 0.086(2) 0.266(5) -0.037(3) 0.147(4) -0.025(2) F4 0.080(4) 0.104(5) 0.073(4) -0.010(3) -0.009(3) 0.023(3) F3 0.070(4) 0.105(5) 0.083(4) 0.023(4) 0.014(3) -0.008(3) F2 0.135(6) 0.088(5) 0.120(6) 0.006(4) 0.053(5) -0.043(4) F1 0.155(7) 0.098(5) 0.080(4) -0.022(4) 0.053(5) -0.027(5) B1 0.073(9) 0.064(8) 0.058(8) 0.000(6) 0.018(7) -0.013(6) C2S 0.23(2) 0.102(11) 0.31(3) -0.096(12) 0.23(2) -0.072(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 Pt1 P1 2.3355(18) 3_877 ? Pt1 P1 2.3356(18) . ? Pt1 P2 2.3392(17) 3_877 ? Pt1 P2 2.3393(17) . ? P1 C10 1.802(8) . ? P1 C1 1.815(7) . ? P1 C20 1.818(7) . ? P2 C30 1.802(8) . ? P2 C40 1.813(7) . ? P2 C2 1.815(7) . ? P3 C5 1.816(8) . ? P3 C50 1.829(10) . ? P3 C60 1.823(8) . ? P4 C80 1.843(8) . ? P4 C70 1.841(8) . ? P4 C6 1.848(8) . ? S1 C1 1.744(7) . ? S1 C3 1.765(7) . ? S2 C2 1.761(6) . ? S2 C3 1.774(7) . ? S3 C4 1.750(7) . ? S3 C5 1.771(8) . ? S4 C4 1.763(7) . ? S4 C6 1.768(8) . ? C1 C2 1.340(10) . ? C3 C4 1.337(9) . ? C5 C6 1.351(11) . ? C10 C15 1.376(10) . ? C10 C11 1.395(10) . ? C20 C21 1.391(10) . ? C20 C25 1.386(9) . ? C21 C22 1.385(11) . ? C30 C31 1.397(9) . ? C30 C35 1.409(10) . ? C60 C65 1.388(10) . ? C60 C61 1.416(11) . ? C70 C71 1.377(11) . ? C70 C75 1.387(11) . ? C71 C72 1.387(11) . ? C31 C32 1.372(11) . ? C50 C51 1.364(13) . ? C50 C55 1.395(12) . ? C32 C33 1.399(12) . ? C35 C34 1.383(11) . ? C62 C63 1.362(13) . ? C62 C61 1.393(11) . ? C45 C40 1.387(9) . ? C45 C44 1.394(11) . ? C41 C42 1.389(11) . ? C41 C40 1.403(10) . ? C25 C24 1.378(11) . ? C33 C34 1.355(12) . ? C11 C12 1.381(12) . ? C15 C14 1.390(11) . ? C75 C74 1.391(12) . ? C24 C23 1.390(12) . ? C22 C23 1.391(11) . ? C14 C13 1.378(13) . ? C81 C82 1.373(11) . ? C81 C80 1.406(11) . ? C80 C85 1.374(11) . ? C42 C43 1.374(13) . ? C44 C43 1.366(13) . ? Cl2 C1S 1.726(14) . ? Cl1 C1S 1.733(11) . ? C82 C83 1.391(12) . ? C72 C73 1.374(13) . ? C73 C74 1.374(13) . ? C84 C83 1.368(12) . ? C84 C85 1.380(11) . ? C13 C12 1.388(14) . ? C51 C52 1.402(14) . ? C65 C64 1.377(12) . ? C63 C64 1.383(13) . ? C55 C54 1.352(19) . ? C53 C52 1.36(2) . ? C53 C54 1.36(2) . ? Cl4 C2S 1.655(14) . ? Cl3 C2S 1.700(11) . ? F4 B1 1.362(12) . ? F3 B1 1.403(14) . ? F2 B1 1.346(13) . ? F1 B1 1.360(14) . ? 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 P1 Pt1 P1 179.997(1) 3_877 . ? P1 Pt1 P2 85.47(6) 3_877 3_877 ? P1 Pt1 P2 94.53(6) . 3_877 ? P1 Pt1 P2 94.53(6) 3_877 . ? P1 Pt1 P2 85.47(6) . . ? P2 Pt1 P2 179.998(1) 3_877 . ? C10 P1 C1 102.9(3) . . ? C10 P1 C20 107.9(4) . . ? C1 P1 C20 105.7(3) . . ? C10 P1 Pt1 118.6(2) . . ? C1 P1 Pt1 105.4(2) . . ? C20 P1 Pt1 114.9(2) . . ? C30 P2 C40 108.7(3) . . ? C30 P2 C2 106.6(3) . . ? C40 P2 C2 101.8(3) . . ? C30 P2 Pt1 114.7(2) . . ? C40 P2 Pt1 118.1(2) . . ? C2 P2 Pt1 105.4(2) . . ? C5 P3 C50 99.8(4) . . ? C5 P3 C60 101.9(3) . . ? C50 P3 C60 102.7(4) . . ? C80 P4 C70 102.9(3) . . ? C80 P4 C6 100.1(4) . . ? C70 P4 C6 101.5(4) . . ? C1 S1 C3 94.0(3) . . ? C2 S2 C3 93.4(3) . . ? C4 S3 C5 94.4(4) . . ? C4 S4 C6 93.8(4) . . ? C2 C1 S1 117.9(5) . . ? C2 C1 P1 120.0(5) . . ? S1 C1 P1 122.1(4) . . ? C1 C2 S2 117.3(5) . . ? C1 C2 P2 120.5(5) . . ? S2 C2 P2 122.1(4) . . ? C4 C3 S1 121.1(5) . . ? C4 C3 S2 125.2(6) . . ? S1 C3 S2 113.7(4) . . ? C3 C4 S3 122.3(6) . . ? C3 C4 S4 124.7(6) . . ? S3 C4 S4 113.0(4) . . ? C6 C5 S3 115.6(6) . . ? C6 C5 P3 123.6(6) . . ? S3 C5 P3 120.7(5) . . ? C5 C6 S4 117.3(6) . . ? C5 C6 P4 123.1(6) . . ? S4 C6 P4 119.6(4) . . ? C15 C10 C11 119.7(7) . . ? C15 C10 P1 118.9(6) . . ? C11 C10 P1 121.3(6) . . ? C21 C20 C25 119.4(7) . . ? C21 C20 P1 119.1(5) . . ? C25 C20 P1 121.3(6) . . ? C22 C21 C20 120.6(7) . . ? C31 C30 C35 119.5(7) . . ? C31 C30 P2 118.9(6) . . ? C35 C30 P2 121.4(6) . . ? C65 C60 C61 118.1(7) . . ? C65 C60 P3 124.0(6) . . ? C61 C60 P3 117.6(6) . . ? C71 C70 C75 117.9(8) . . ? C71 C70 P4 125.3(6) . . ? C75 C70 P4 116.8(7) . . ? C70 C71 C72 122.1(9) . . ? C32 C31 C30 120.4(7) . . ? C51 C50 C55 119.2(10) . . ? C51 C50 P3 125.2(7) . . ? C55 C50 P3 115.6(9) . . ? C31 C32 C33 120.0(8) . . ? C34 C35 C30 118.2(8) . . ? C63 C62 C61 120.5(9) . . ? C40 C45 C44 120.1(8) . . ? C42 C41 C40 119.9(8) . . ? C24 C25 C20 120.1(7) . . ? C34 C33 C32 119.4(9) . . ? C45 C40 C41 119.1(7) . . ? C45 C40 P2 123.8(6) . . ? C41 C40 P2 117.1(5) . . ? C12 C11 C10 120.1(9) . . ? C10 C15 C14 121.0(8) . . ? C62 C61 C60 119.9(8) . . ? C74 C75 C70 121.0(10) . . ? C25 C24 C23 120.7(7) . . ? C21 C22 C23 119.8(8) . . ? C13 C14 C15 118.5(10) . . ? C82 C81 C80 120.8(8) . . ? C85 C80 C81 117.9(7) . . ? C85 C80 P4 118.1(6) . . ? C81 C80 P4 123.9(6) . . ? C22 C23 C24 119.4(8) . . ? C43 C42 C41 119.8(9) . . ? C43 C44 C45 119.9(9) . . ? C81 C82 C83 119.6(8) . . ? C73 C72 C71 118.6(10) . . ? C74 C73 C72 121.1(9) . . ? C83 C84 C85 119.8(9) . . ? C84 C83 C82 120.1(8) . . ? C44 C43 C42 121.0(9) . . ? C14 C13 C12 121.7(10) . . ? C33 C34 C35 122.5(8) . . ? C11 C12 C13 119.0(9) . . ? C80 C85 C84 121.7(8) . . ? Cl2 C1S Cl1 112.3(7) . . ? C50 C51 C52 120.6(12) . . ? C64 C65 C60 120.7(8) . . ? C73 C74 C75 119.3(9) . . ? C62 C63 C64 120.0(9) . . ? C54 C55 C50 120.5(15) . . ? C52 C53 C54 122.8(16) . . ? C65 C64 C63 120.7(9) . . ? C53 C52 C51 117.6(16) . . ? C53 C54 C55 119.3(17) . . ? F2 B1 F1 111.0(11) . . ? F2 B1 F4 110.9(9) . . ? F1 B1 F4 111.1(10) . . ? F2 B1 F3 107.5(10) . . ? F1 B1 F3 108.6(9) . . ? F4 B1 F3 107.5(10) . . ? Cl4 C2S Cl3 116.2(8) . . ? _diffrn_measured_fraction_theta_max 0.641 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.641 _refine_diff_density_max 0.769 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.101 #==END data_final _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C276 H232 B4 Cl8 F16 P16 Pt2 S16' _chemical_formula_weight 5578.26 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' 'B' 'B' 0.0013 0.0007 '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' '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' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 22.540(4) _cell_length_b 16.739(3) _cell_length_c 17.929(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.35(3) _cell_angle_gamma 90.00 _cell_volume 6256(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular _exptl_crystal_colour red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 1.507 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19638 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7555 _reflns_number_gt 6224 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7555 _refine_ls_number_parameters 540 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 1.632 _refine_ls_shift/su_mean 0.011 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 Pt Pt 0.0000 0.0000 -0.5000 0.01532(12) Uani 1 4 d S . . S1 S 0.11438(8) 0.08875(8) -0.21125(7) 0.0370(3) Uani 1 1 d . . . S3 S 0.21384(9) 0.08741(9) -0.02167(8) 0.0552(5) Uani 1 1 d . . . P1 P 0.04729(5) 0.09471(7) -0.39883(6) 0.0178(2) Uani 1 1 d . . . P3 P 0.30502(8) 0.10038(9) 0.15970(8) 0.0414(4) Uani 1 1 d . . . C1 C 0.0799(2) 0.0403(3) -0.3043(2) 0.0228(10) Uani 1 1 d . . . C3 C 0.1448(4) 0.0000 -0.1566(4) 0.0304(16) Uani 1 2 d S . . C4 C 0.1856(4) 0.0000 -0.0788(4) 0.0360(18) Uani 1 2 d S . . C6 C 0.2620(3) 0.0404(3) 0.0690(3) 0.0371(13) Uani 1 1 d . . . C11 C -0.0073(2) 0.1660(3) -0.3827(2) 0.0211(9) Uani 1 1 d . . . C12 C -0.0106(2) 0.2448(3) -0.4080(3) 0.0296(11) Uani 1 1 d . . . C13 C -0.0566(3) 0.2959(3) -0.4000(3) 0.0395(13) Uani 1 1 d . . . C14 C -0.0988(3) 0.2681(4) -0.3669(4) 0.0420(14) Uani 1 1 d . . . C15 C -0.0965(3) 0.1901(4) -0.3428(3) 0.0402(14) Uani 1 1 d . . . C16 C -0.0502(2) 0.1375(3) -0.3491(3) 0.0274(10) Uani 1 1 d . . . C21 C 0.1147(2) 0.1487(3) -0.4053(3) 0.0212(9) Uani 1 1 d . . . C22 C 0.1412(2) 0.2145(3) -0.3566(3) 0.0295(11) Uani 1 1 d . . . C23 C 0.1947(3) 0.2519(4) -0.3618(3) 0.0389(14) Uani 1 1 d . . . C24 C 0.2217(2) 0.2240(4) -0.4138(3) 0.0363(13) Uani 1 1 d . . . C25 C 0.1967(2) 0.1576(4) -0.4610(3) 0.0346(12) Uani 1 1 d . . . C26 C 0.1429(2) 0.1195(3) -0.4571(3) 0.0259(10) Uani 1 1 d . . . C51 C 0.3622(3) 0.1600(4) 0.1324(3) 0.0436(14) Uani 1 1 d . . . C52 C 0.4256(3) 0.1586(5) 0.1869(4) 0.0563(19) Uani 1 1 d . . . C53 C 0.4721(4) 0.2032(6) 0.1734(5) 0.069(2) Uani 1 1 d . . . C54 C 0.4570(4) 0.2494(6) 0.1062(5) 0.069(2) Uani 1 1 d . . . C55 C 0.3949(4) 0.2526(5) 0.0507(4) 0.0563(17) Uani 1 1 d . . . C56 C 0.3472(3) 0.2081(4) 0.0640(4) 0.0472(15) Uani 1 1 d . . . C61 C 0.2421(3) 0.1720(4) 0.1544(3) 0.0444(14) Uani 1 1 d . . . C62 C 0.2477(3) 0.2532(4) 0.1506(3) 0.0448(15) Uani 1 1 d . . . C63 C 0.2003(4) 0.3048(5) 0.1569(4) 0.0596(19) Uani 1 1 d . . . C64 C 0.1478(4) 0.2728(6) 0.1666(5) 0.068(2) Uani 1 1 d . . . C65 C 0.1407(5) 0.1926(6) 0.1692(5) 0.071(2) Uani 1 1 d . . . C66 C 0.1876(4) 0.1414(5) 0.1644(4) 0.0589(18) Uani 1 1 d . . . H12A H 0.020(2) 0.257(3) -0.436(3) 0.011(10) Uiso 1 1 d . . . H13A H -0.060(2) 0.351(3) -0.421(3) 0.018(12) Uiso 1 1 d . . . H14A H -0.129(3) 0.301(3) -0.360(3) 0.030(14) Uiso 1 1 d . . . H15A H -0.123(3) 0.170(4) -0.321(4) 0.052(19) Uiso 1 1 d . . . H16A H -0.049(2) 0.080(3) -0.334(3) 0.024(13) Uiso 1 1 d . . . H22A H 0.124(2) 0.230(3) -0.315(3) 0.020(12) Uiso 1 1 d . . . H23A H 0.210(2) 0.296(3) -0.334(3) 0.017(12) Uiso 1 1 d . . . H24A H 0.256(2) 0.250(3) -0.417(3) 0.022(12) Uiso 1 1 d . . . H25A H 0.219(3) 0.138(3) -0.494(3) 0.034(15) Uiso 1 1 d . . . H26A H 0.125(2) 0.073(3) -0.491(3) 0.028(14) Uiso 1 1 d . . . H52A H 0.434(3) 0.133(4) 0.232(4) 0.050(19) Uiso 1 1 d . . . H53A H 0.516(3) 0.200(4) 0.215(4) 0.07(2) Uiso 1 1 d . . . H54A H 0.485(4) 0.284(5) 0.096(5) 0.09(3) Uiso 1 1 d . . . H55A H 0.380(3) 0.290(4) -0.002(4) 0.048(17) Uiso 1 1 d . . . H56A H 0.300(3) 0.209(4) 0.019(4) 0.051(18) Uiso 1 1 d . . . H62A H 0.281(3) 0.278(3) 0.143(3) 0.030(15) Uiso 1 1 d . . . H63A H 0.209(3) 0.367(4) 0.157(4) 0.048(17) Uiso 1 1 d . . . H64A H 0.117(4) 0.313(6) 0.171(5) 0.09(3) Uiso 1 1 d . . . H65A H 0.099(4) 0.169(6) 0.174(5) 0.10(3) Uiso 1 1 d . . . H66A H 0.186(3) 0.073(5) 0.166(4) 0.07(2) Uiso 1 1 d . . . C11S C 0.3197(4) 0.0000 0.7068(6) 0.050(2) Uani 1 2 d SD . . C12S C 0.3193(6) 0.0000 0.6290(6) 0.059(3) Uani 1 2 d S . . H12B H 0.2808 0.0000 0.5845 0.16(7) Uiso 1 2 calc SR . . C13S C 0.3775(7) 0.0000 0.6188(8) 0.076(4) Uani 1 2 d S . . H13B H 0.3780 0.0000 0.5671 0.05(3) Uiso 1 2 calc SR . . C14S C 0.4358(6) 0.0000 0.6866(10) 0.078(4) Uani 1 2 d S . . H14B H 0.4746 0.0000 0.6795 0.05(3) Uiso 1 2 calc SR . . C15S C 0.4356(6) 0.0000 0.7608(8) 0.074(3) Uani 1 2 d S . . H15B H 0.4742 0.0000 0.8052 0.08(4) Uiso 1 2 calc SR . . C16S C 0.3780(5) 0.0000 0.7722(7) 0.063(3) Uani 1 2 d S . . H16B H 0.3784 0.0000 0.8242 0.13(6) Uiso 1 2 calc SR . . C17S C 0.2577(5) 0.0000 0.7193(7) 0.068(3) Uani 1 2 d SD . . H17A H 0.2225 0.0000 0.6680 0.12(5) Uiso 1 2 calc SR . . H17B H 0.2554 0.0468 0.7490 0.28(12) Uiso 0.50 1 calc PR . . H17C H 0.2554 -0.0468 0.7490 0.0(3) Uiso 0.50 1 calc PR . . C21S C 0.4624(5) 0.0062(12) 0.0026(10) 0.057(5) Uiso 0.25 1 d PD A -1 C22S C 0.5029(7) 0.0709(9) 0.0079(16) 0.059(8) Uiso 0.25 1 d PD A -1 H22S H 0.4896(14) 0.1225(12) 0.013(4) 0.071 Uiso 0.25 1 d PD B -1 C23S C 0.5635(7) 0.0582(9) 0.0061(16) 0.065(8) Uiso 0.25 1 d PD A -1 H23S H 0.5905(14) 0.1013(11) 0.010(4) 0.078 Uiso 0.25 1 d PD C -1 C24S C 0.5836(7) -0.0192(10) -0.0010(16) 0.069(9) Uiso 0.25 1 d PD A -1 H24S H 0.6249(13) -0.0280(14) 0.001(4) 0.082 Uiso 0.25 1 d PD D -1 C25S C 0.5439(10) -0.0841(8) -0.004(3) 0.115(16) Uiso 0.25 1 d PD A -1 H25S H 0.5568(17) -0.1356(11) -0.011(5) 0.138 Uiso 0.25 1 d PD E -1 C26S C 0.4826(8) -0.0712(10) -0.0045(18) 0.052(9) Uiso 0.25 1 d PD A -1 H26S H 0.4554(16) -0.1143(13) -0.009(5) 0.062 Uiso 0.25 1 d PD F -1 C27S C 0.3961(7) 0.0064(12) 0.0031(10) 0.087(9) Uiso 0.25 1 d PD A -1 H27A H 0.3987 0.0064 0.0578 0.131 Uiso 0.25 1 calc PRD A -1 H27B H 0.3735 -0.0404 -0.0241 0.131 Uiso 0.25 1 calc PRD A -1 H27C H 0.3736 0.0533 -0.0240 0.131 Uiso 0.25 1 calc PRD A -1 Cl1 Cl 0.41645(18) 0.08363(15) 0.40399(19) 0.1354(13) Uani 1 1 d . . . C1S C 0.3695(5) 0.0000 0.3722(6) 0.048(2) Uani 1 2 d S . . H1A H 0.360(8) 0.0000 0.283(11) 0.18(7) Uiso 1 2 d S . . H1B H 0.340(4) 0.0000 0.388(5) 0.04(3) Uiso 1 2 d S . . F1 F 0.1452(4) 0.0000 0.2861(4) 0.115(3) Uani 1 2 d S . . F2 F 0.2298(2) 0.0682(3) 0.3700(4) 0.0877(16) Uani 1 1 d . . . F4 F 0.1643(3) 0.0000 0.4157(4) 0.0652(16) Uani 1 2 d S . . B1 B 0.1948(5) 0.0000 0.3623(7) 0.045(2) Uani 1 2 d S . . C31S C 0.5008(10) 0.491(2) -0.0496(8) 0.074(8) Uiso 0.25 1 d PD G -2 C32S C 0.5493(8) 0.4661(17) 0.0220(12) 0.066(9) Uiso 0.25 1 d PD G -2 H32A H 0.5851 0.4395 0.0206 0.079 Uiso 0.25 1 calc PR G -2 C33S C 0.5441(10) 0.4813(17) 0.0958(8) 0.070(9) Uiso 0.25 1 d PD G -2 H33A H 0.5762 0.4644 0.1435 0.084 Uiso 0.25 1 calc PR G -2 C34S C 0.4907(15) 0.522(2) 0.0980(12) 0.117(16) Uiso 0.25 1 d PD G -2 H34A H 0.4878 0.5333 0.1472 0.140 Uiso 0.25 1 calc PR G -2 C35S C 0.4417(13) 0.545(2) 0.0263(19) 0.15(2) Uiso 0.25 1 d PD G -2 H35A H 0.4062 0.5725 0.0277 0.176 Uiso 0.25 1 calc PR G -2 C36S C 0.4460(10) 0.528(3) -0.0476(13) 0.111(17) Uiso 0.25 1 d PD G -2 H36A H 0.4123 0.5407 -0.0955 0.133 Uiso 0.25 1 calc PR G -2 C37S C 0.489(2) 0.486(5) -0.1376(12) 0.15(2) Uiso 0.25 1 d PD G -2 H37A H 0.4458 0.5022 -0.1689 0.226 Uiso 0.50 2 calc SPR G -2 H37B H 0.4949 0.4315 -0.1512 0.226 Uiso 0.25 1 calc PR G -2 H37C H 0.5185 0.5199 -0.1492 0.226 Uiso 0.25 1 calc PR G -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 Pt 0.01677(18) 0.01593(18) 0.01099(17) 0.000 0.00272(12) 0.000 S1 0.0594(9) 0.0230(7) 0.0138(6) -0.0024(5) -0.0030(6) 0.0024(6) S3 0.0895(13) 0.0254(7) 0.0194(7) -0.0013(5) -0.0145(7) 0.0026(7) P1 0.0213(6) 0.0180(6) 0.0110(5) -0.0003(4) 0.0024(4) -0.0009(4) P3 0.0580(10) 0.0313(8) 0.0184(7) -0.0019(6) -0.0042(6) 0.0003(7) C1 0.028(2) 0.022(2) 0.013(2) -0.0004(17) 0.0017(18) -0.0015(18) C3 0.042(4) 0.028(4) 0.013(3) 0.000 0.001(3) 0.000 C4 0.052(5) 0.026(4) 0.017(3) 0.000 -0.002(3) 0.000 C6 0.049(3) 0.033(3) 0.016(2) 0.000(2) -0.003(2) -0.003(2) C11 0.024(2) 0.024(2) 0.012(2) -0.0051(17) 0.0024(17) 0.0032(18) C12 0.032(3) 0.030(3) 0.024(2) 0.003(2) 0.008(2) 0.008(2) C13 0.046(3) 0.029(3) 0.036(3) -0.002(2) 0.007(3) 0.012(3) C14 0.035(3) 0.045(4) 0.042(3) -0.014(3) 0.010(3) 0.012(3) C15 0.029(3) 0.060(4) 0.035(3) -0.014(3) 0.015(2) -0.003(3) C16 0.034(3) 0.027(3) 0.025(2) -0.002(2) 0.015(2) 0.000(2) C21 0.023(2) 0.022(2) 0.014(2) 0.0006(17) 0.0014(17) -0.0014(18) C22 0.035(3) 0.031(3) 0.019(2) -0.002(2) 0.006(2) -0.005(2) C23 0.038(3) 0.046(3) 0.026(3) -0.001(3) 0.005(2) -0.023(3) C24 0.023(2) 0.051(4) 0.031(3) 0.008(3) 0.005(2) -0.012(2) C25 0.027(3) 0.043(3) 0.036(3) 0.012(3) 0.015(2) 0.004(2) C26 0.027(2) 0.028(3) 0.020(2) 0.001(2) 0.0058(19) 0.003(2) C51 0.051(3) 0.040(3) 0.028(3) -0.004(2) 0.002(3) 0.006(3) C52 0.058(4) 0.058(4) 0.030(3) -0.001(3) -0.010(3) 0.004(3) C53 0.046(4) 0.090(6) 0.053(4) -0.001(4) -0.002(3) -0.006(4) C54 0.055(5) 0.086(6) 0.059(5) -0.007(5) 0.014(4) -0.008(4) C55 0.065(4) 0.056(4) 0.041(4) 0.000(3) 0.013(3) 0.002(4) C56 0.053(4) 0.046(4) 0.030(3) 0.002(3) 0.002(3) 0.005(3) C61 0.058(4) 0.046(4) 0.020(3) -0.004(2) 0.005(2) -0.001(3) C62 0.056(4) 0.040(3) 0.029(3) -0.003(3) 0.005(3) -0.001(3) C63 0.082(5) 0.049(4) 0.041(4) -0.007(3) 0.015(4) 0.016(4) C64 0.071(5) 0.086(6) 0.050(4) 0.000(4) 0.027(4) 0.019(5) C65 0.081(6) 0.093(7) 0.048(4) 0.007(4) 0.033(4) 0.006(5) C66 0.076(5) 0.062(5) 0.039(4) -0.001(3) 0.023(3) -0.005(4) C11S 0.050(5) 0.038(5) 0.050(5) 0.000 0.006(4) 0.000 C12S 0.084(8) 0.039(5) 0.051(6) 0.000 0.020(6) 0.000 C13S 0.130(12) 0.037(6) 0.077(8) 0.000 0.057(9) 0.000 C14S 0.071(8) 0.039(6) 0.132(13) 0.000 0.049(9) 0.000 C15S 0.060(7) 0.061(7) 0.084(9) 0.000 0.010(7) 0.000 C16S 0.050(6) 0.062(7) 0.068(7) 0.000 0.010(5) 0.000 C17S 0.062(7) 0.080(8) 0.061(7) 0.000 0.023(6) 0.000 Cl1 0.182(3) 0.0504(13) 0.114(2) -0.0060(14) -0.011(2) -0.0401(17) C1S 0.053(6) 0.045(5) 0.048(5) 0.000 0.021(5) 0.000 F1 0.139(7) 0.121(7) 0.063(5) 0.000 0.013(5) 0.000 F2 0.081(3) 0.058(3) 0.152(5) 0.000(3) 0.076(3) -0.012(2) F4 0.086(4) 0.048(3) 0.087(4) 0.000 0.062(4) 0.000 B1 0.055(6) 0.033(5) 0.054(6) 0.000 0.029(5) 0.000 _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 Pt P1 2.3387(12) 5_554 ? Pt P1 2.3387(12) . ? Pt P1 2.3387(12) 6 ? Pt P1 2.3387(12) 2_554 ? S1 C1 1.749(4) . ? S1 C3 1.768(4) . ? S3 C4 1.760(4) . ? S3 C6 1.761(5) . ? P1 C21 1.809(5) . ? P1 C11 1.814(5) . ? P1 C1 1.815(4) . ? P3 C61 1.832(7) . ? P3 C51 1.838(7) . ? P3 C6 1.842(5) . ? C1 C1 1.351(10) 6 ? C3 C4 1.348(10) . ? C3 S1 1.768(4) 6 ? C4 S3 1.760(4) 6 ? C6 C6 1.351(11) 6 ? C11 C12 1.388(7) . ? C11 C16 1.403(7) . ? C12 C13 1.394(7) . ? C13 C14 1.379(9) . ? C14 C15 1.370(9) . ? C15 C16 1.404(7) . ? C21 C22 1.393(7) . ? C21 C26 1.397(6) . ? C22 C23 1.392(7) . ? C23 C24 1.374(8) . ? C24 C25 1.382(8) . ? C25 C26 1.395(7) . ? C51 C52 1.391(9) . ? C51 C56 1.397(8) . ? C52 C53 1.382(11) . ? C53 C54 1.362(12) . ? C54 C55 1.376(10) . ? C55 C56 1.401(10) . ? C61 C62 1.369(9) . ? C61 C66 1.405(10) . ? C62 C63 1.411(10) . ? C63 C64 1.368(11) . ? C64 C65 1.354(12) . ? C65 C66 1.388(11) . ? C11S C16S 1.388(13) . ? C11S C12S 1.391(13) . ? C11S C17S 1.499(12) . ? C12S C13S 1.392(16) . ? C13S C14S 1.411(18) . ? C14S C15S 1.332(18) . ? C15S C16S 1.389(16) . ? C21S C22S 1.3946(18) . ? C21S C26S 1.3949(18) . ? C21S C27S 1.499(12) . ? C22S C23S 1.3948(18) . ? C23S C24S 1.3950(18) . ? C24S C25S 1.3950(19) . ? C25S C26S 1.3950(18) . ? Cl1 C1S 1.717(6) . ? C1S Cl1 1.717(6) 6 ? F1 B1 1.398(13) . ? F2 B1 1.364(7) . ? F4 B1 1.376(11) . ? B1 F2 1.364(7) 6 ? C31S C32S 1.3950(19) . ? C31S C36S 1.3952(19) . ? C31S C37S 1.499(12) . ? C32S C33S 1.3949(19) . ? C33S C34S 1.3947(19) . ? C34S C35S 1.3949(19) . ? C35S C36S 1.3950(19) . ? 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 P1 Pt P1 180.00(4) 5_554 . ? P1 Pt P1 94.64(6) 5_554 6 ? P1 Pt P1 85.36(6) . 6 ? P1 Pt P1 85.36(6) 5_554 2_554 ? P1 Pt P1 94.64(6) . 2_554 ? P1 Pt P1 180.00(4) 6 2_554 ? C1 S1 C3 94.4(2) . . ? C4 S3 C6 97.2(3) . . ? C21 P1 C11 108.6(2) . . ? C21 P1 C1 105.0(2) . . ? C11 P1 C1 103.8(2) . . ? C21 P1 Pt 115.79(15) . . ? C11 P1 Pt 115.63(15) . . ? C1 P1 Pt 106.71(15) . . ? C61 P3 C51 103.8(3) . . ? C61 P3 C6 100.0(3) . . ? C51 P3 C6 104.3(3) . . ? C1 C1 S1 117.60(16) 6 . ? C1 C1 P1 120.10(15) 6 . ? S1 C1 P1 122.3(3) . . ? C4 C3 S1 122.81(18) . 6 ? C4 C3 S1 122.81(18) . . ? S1 C3 S1 114.3(4) 6 . ? C3 C4 S3 123.7(2) . . ? C3 C4 S3 123.7(2) . 6 ? S3 C4 S3 112.5(4) . 6 ? C6 C6 S3 116.57(18) 6 . ? C6 C6 P3 123.06(17) 6 . ? S3 C6 P3 120.2(3) . . ? C12 C11 C16 120.2(4) . . ? C12 C11 P1 121.9(4) . . ? C16 C11 P1 117.7(4) . . ? C11 C12 C13 119.9(5) . . ? C14 C13 C12 120.0(5) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 120.9(5) . . ? C11 C16 C15 118.5(5) . . ? C22 C21 C26 119.9(4) . . ? C22 C21 P1 121.7(4) . . ? C26 C21 P1 118.2(4) . . ? C23 C22 C21 119.4(5) . . ? C24 C23 C22 120.7(5) . . ? C23 C24 C25 120.4(5) . . ? C24 C25 C26 119.8(5) . . ? C25 C26 C21 119.8(5) . . ? C52 C51 C56 117.9(7) . . ? C52 C51 P3 116.1(5) . . ? C56 C51 P3 125.9(5) . . ? C53 C52 C51 120.8(7) . . ? C54 C53 C52 120.7(7) . . ? C53 C54 C55 120.3(8) . . ? C54 C55 C56 119.6(7) . . ? C51 C56 C55 120.6(6) . . ? C62 C61 C66 118.0(7) . . ? C62 C61 P3 124.7(5) . . ? C66 C61 P3 116.9(5) . . ? C61 C62 C63 121.1(7) . . ? C64 C63 C62 119.2(8) . . ? C65 C64 C63 120.8(8) . . ? C64 C65 C66 120.5(9) . . ? C65 C66 C61 120.4(8) . . ? C16S C11S C12S 119.4(10) . . ? C16S C11S C17S 120.6(10) . . ? C12S C11S C17S 120.0(9) . . ? C11S C12S C13S 119.0(11) . . ? C12S C13S C14S 120.1(12) . . ? C15S C14S C13S 120.3(12) . . ? C14S C15S C16S 120.4(12) . . ? C11S C16S C15S 120.8(12) . . ? C22S C21S C26S 119.99(13) . . ? C22S C21S C27S 128.7(5) . . ? C26S C21S C27S 111.3(5) . . ? C21S C22S C23S 120.02(12) . . ? C22S C23S C24S 119.99(12) . . ? C25S C24S C23S 119.96(14) . . ? C24S C25S C26S 119.97(15) . . ? C21S C26S C25S 119.97(14) . . ? Cl1 C1S Cl1 109.2(6) 6 . ? F2 B1 F2 113.6(8) 6 . ? F2 B1 F4 110.6(6) 6 . ? F2 B1 F4 110.6(6) . . ? F2 B1 F1 108.4(6) 6 . ? F2 B1 F1 108.4(6) . . ? F4 B1 F1 104.7(8) . . ? C32S C31S C36S 119.95(15) . . ? C32S C31S C37S 136(3) . . ? C36S C31S C37S 104(2) . . ? C33S C32S C31S 119.98(13) . . ? C34S C33S C32S 120.01(13) . . ? C33S C34S C35S 119.99(13) . . ? C36S C35S C34S 119.98(14) . . ? C35S C36S C31S 119.95(16) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.804 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.131 #==END data_texas _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.65 H57.53 Ag B Cl0.48 F4 N1.68 P4 S8' _chemical_formula_weight 1486.07 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' '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 P2(1)/n _symmetry_Int_Tables_number 14 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 25.569(5) _cell_length_b 21.376(4) _cell_length_c 27.209(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.75(3) _cell_angle_gamma 90.00 _cell_volume 13714(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular box' _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6075 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 159669 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.43 _reflns_number_total 32878 _reflns_number_gt 24019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32878 _refine_ls_number_parameters 1707 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 2.073 _refine_ls_shift/su_mean 0.025 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 0.195877(9) 0.709004(9) 0.125980(8) 0.02377(6) Uani 1 1 d . . . Ag2 Ag 0.695881(9) 0.797580(9) 0.150987(8) 0.02445(6) Uani 1 1 d . . . P1 P 0.20855(3) 0.82567(3) 0.12977(3) 0.02259(15) Uani 1 1 d . . . P2 P 0.09312(3) 0.73370(3) 0.10066(3) 0.02308(15) Uani 1 1 d . . . P3 P 0.22588(3) 0.61606(3) 0.08800(3) 0.02262(15) Uani 1 1 d . . . P4 P 0.24695(3) 0.65577(3) 0.21425(3) 0.02365(15) Uani 1 1 d . . . P5 P 0.72011(3) 0.68340(3) 0.16160(3) 0.02476(15) Uani 1 1 d . . . P6 P 0.59638(3) 0.76225(3) 0.12458(3) 0.02270(15) Uani 1 1 d . . . P7 P 0.73323(3) 0.87299(3) 0.10318(3) 0.02301(15) Uani 1 1 d . . . P8 P 0.74989(3) 0.85933(3) 0.23275(3) 0.02453(15) Uani 1 1 d . . . S1 S 0.12456(3) 0.93667(3) 0.09677(3) 0.02822(16) Uani 1 1 d . . . S2 S 0.02295(3) 0.85648(3) 0.06897(3) 0.02770(16) Uani 1 1 d . . . S3 S -0.05633(3) 0.97996(3) 0.05034(3) 0.02940(16) Uani 1 1 d . . . S4 S 0.04340(3) 1.06160(3) 0.07614(3) 0.02918(16) Uani 1 1 d . . . S5 S 0.29700(3) 0.49825(4) 0.13761(3) 0.03230(17) Uani 1 1 d . . . S6 S 0.31592(3) 0.53218(4) 0.24772(3) 0.03113(17) Uani 1 1 d . . . S7 S 0.40969(4) 0.41607(4) 0.17595(3) 0.03634(19) Uani 1 1 d . . . S8 S 0.43171(3) 0.44045(3) 0.28848(3) 0.02901(16) Uani 1 1 d . . . S11 S 0.64665(3) 0.56548(3) 0.11865(3) 0.03012(16) Uani 1 1 d . . . S12 S 0.53841(3) 0.63564(3) 0.08372(3) 0.02677(15) Uani 1 1 d . . . S13 S 0.57606(3) 0.43451(3) 0.08804(3) 0.02860(16) Uani 1 1 d . . . S14 S 0.46905(3) 0.50442(3) 0.05756(3) 0.03008(16) Uani 1 1 d . . . S15 S 0.83390(3) 0.96870(4) 0.25472(3) 0.02966(16) Uani 1 1 d . . . S16 S 0.81882(3) 0.98334(3) 0.14232(3) 0.02878(16) Uani 1 1 d . . . S17 S 0.95319(3) 1.04289(4) 0.29330(3) 0.02831(16) Uani 1 1 d . . . S18 S 0.93982(3) 1.06009(3) 0.18171(3) 0.02849(16) Uani 1 1 d . . . C1 C 0.13570(11) 0.85536(12) 0.10573(11) 0.0227(6) Uani 1 1 d . . . C2 C 0.08931(11) 0.81892(13) 0.09374(11) 0.0239(6) Uani 1 1 d . . . C3 C 0.05049(12) 0.93343(13) 0.07720(11) 0.0244(6) Uani 1 1 d . . . C4 C 0.01746(12) 0.98454(13) 0.06905(11) 0.0240(6) Uani 1 1 d . . . C5 C -0.02277(13) 1.09799(14) 0.06404(11) 0.0297(7) Uani 1 1 d . . . C6 C -0.06726(12) 1.06069(14) 0.05290(11) 0.0276(6) Uani 1 1 d . . . C7 C -0.02185(15) 1.16831(15) 0.06645(14) 0.0434(8) Uani 1 1 d . . . H7A H -0.0593 1.1836 0.0596 0.065 Uiso 1 1 calc R . . H7B H -0.0091 1.1846 0.0401 0.065 Uiso 1 1 calc R . . H7C H 0.0035 1.1817 0.1012 0.065 Uiso 1 1 calc R . . C8 C -0.12783(13) 1.07977(16) 0.04029(13) 0.0393(8) Uani 1 1 d . . . H8A H -0.1299 1.1244 0.0428 0.059 Uiso 1 1 calc R . . H8B H -0.1410 1.0605 0.0652 0.059 Uiso 1 1 calc R . . H8C H -0.1511 1.0666 0.0048 0.059 Uiso 1 1 calc R . . C9 C 0.26643(11) 0.56883(13) 0.14653(11) 0.0238(6) Uani 1 1 d . . . C10 C 0.27503(12) 0.58441(13) 0.19726(11) 0.0247(6) Uani 1 1 d . . . C11 C 0.34063(12) 0.48998(13) 0.20537(11) 0.0272(6) Uani 1 1 d . . . C12 C 0.38746(12) 0.45428(13) 0.22167(11) 0.0274(6) Uani 1 1 d . . . C13 C 0.47783(13) 0.39694(14) 0.22299(12) 0.0297(6) Uani 1 1 d . . . C15 C 0.51665(15) 0.36843(16) 0.19971(14) 0.0413(8) Uani 1 1 d . . . H15A H 0.5527 0.3597 0.2277 0.062 Uiso 1 1 calc R . . H15B H 0.5218 0.3971 0.1748 0.062 Uiso 1 1 calc R . . H15C H 0.5004 0.3302 0.1817 0.062 Uiso 1 1 calc R . . C14 C 0.48773(12) 0.40727(13) 0.27405(12) 0.0274(6) Uani 1 1 d . . . C16 C 0.54016(13) 0.38991(15) 0.32092(12) 0.0347(7) Uani 1 1 d . . . H16A H 0.5676 0.3727 0.3086 0.052 Uiso 1 1 calc R . . H16B H 0.5309 0.3594 0.3422 0.052 Uiso 1 1 calc R . . H16C H 0.5556 0.4265 0.3420 0.052 Uiso 1 1 calc R . . C101 C 0.78660(12) 0.91715(13) 0.20862(11) 0.0261(6) Uani 1 1 d . . . C102 C 0.77930(11) 0.92364(13) 0.15691(11) 0.0233(6) Uani 1 1 d . . . C103 C 0.86190(12) 0.99848(13) 0.20971(11) 0.0259(6) Uani 1 1 d . . . C104 C 0.91150(12) 1.02943(13) 0.22578(11) 0.0246(6) Uani 1 1 d . . . C105 C 1.01114(12) 1.07613(13) 0.28205(11) 0.0265(6) Uani 1 1 d . . . C106 C 1.00504(12) 1.08366(13) 0.23178(12) 0.0284(6) Uani 1 1 d . . . C107 C 1.06058(13) 1.09626(16) 0.33100(12) 0.0380(8) Uani 1 1 d . . . H10A H 1.0896 1.1136 0.3208 0.057 Uiso 1 1 calc R . . H10B H 1.0755 1.0608 0.3538 0.057 Uiso 1 1 calc R . . H10C H 1.0483 1.1273 0.3497 0.057 Uiso 1 1 calc R . . C108 C 1.04553(14) 1.11372(16) 0.21151(13) 0.0373(7) Uani 1 1 d . . . H10D H 1.0796 1.1251 0.2410 0.056 Uiso 1 1 calc R . . H10E H 1.0285 1.1505 0.1915 0.056 Uiso 1 1 calc R . . H10F H 1.0546 1.0849 0.1889 0.056 Uiso 1 1 calc R . . C109 C 0.60130(12) 0.67864(12) 0.11242(11) 0.0237(6) Uani 1 1 d . . . C110 C 0.65085(11) 0.64709(12) 0.12755(11) 0.0237(6) Uani 1 1 d . . . C111 C 0.57214(12) 0.56200(12) 0.09221(11) 0.0235(6) Uani 1 1 d . . . C112 C 0.54327(11) 0.50807(12) 0.08030(10) 0.0225(6) Uani 1 1 d . . . C113 C 0.46439(13) 0.42224(14) 0.05102(11) 0.0296(6) Uani 1 1 d . . . C114 C 0.51293(13) 0.39046(13) 0.06399(11) 0.0301(7) Uani 1 1 d . . . C115 C 0.40546(14) 0.39563(17) 0.03146(15) 0.0458(9) Uani 1 1 d . . . H11A H 0.4073 0.3509 0.0294 0.069 Uiso 1 1 calc R . . H11B H 0.3835 0.4122 -0.0032 0.069 Uiso 1 1 calc R . . H11C H 0.3879 0.4068 0.0557 0.069 Uiso 1 1 calc R . . C116 C 0.51995(15) 0.32144(14) 0.06174(14) 0.0424(8) Uani 1 1 d . . . H11D H 0.4833 0.3018 0.0483 0.064 Uiso 1 1 calc R . . H11E H 0.5418 0.3060 0.0969 0.064 Uiso 1 1 calc R . . H11F H 0.5393 0.3121 0.0386 0.064 Uiso 1 1 calc R . . C17 C 0.23922(12) 0.85665(13) 0.19747(11) 0.0260(6) Uani 1 1 d . . . C18 C 0.20887(14) 0.84801(15) 0.23032(12) 0.0343(7) Uani 1 1 d . . . H18A H 0.1722 0.8320 0.2160 0.041 Uiso 1 1 calc R . . C19 C 0.23339(15) 0.86322(17) 0.28402(13) 0.0419(8) Uani 1 1 d . . . H19A H 0.2130 0.8576 0.3055 0.050 Uiso 1 1 calc R . . C20 C 0.28802(16) 0.88667(16) 0.30566(13) 0.0445(9) Uani 1 1 d . . . H20A H 0.3044 0.8963 0.3418 0.053 Uiso 1 1 calc R . . C21 C 0.31817(14) 0.89579(15) 0.27428(13) 0.0390(8) Uani 1 1 d . . . H21A H 0.3545 0.9125 0.2889 0.047 Uiso 1 1 calc R . . C22 C 0.29426(13) 0.87993(14) 0.21996(13) 0.0327(7) Uani 1 1 d . . . H22A H 0.3153 0.8850 0.1990 0.039 Uiso 1 1 calc R . . C23 C 0.23940(11) 0.87038(14) 0.09009(11) 0.0267(6) Uani 1 1 d . . . C24 C 0.25421(12) 0.93350(14) 0.09828(13) 0.0326(7) Uani 1 1 d . . . H24A H 0.2501 0.9550 0.1263 0.039 Uiso 1 1 calc R . . C25 C 0.27503(13) 0.96420(17) 0.06464(14) 0.0424(8) Uani 1 1 d . . . H25A H 0.2845 1.0064 0.0700 0.051 Uiso 1 1 calc R . . C26 C 0.28175(14) 0.93226(19) 0.02299(15) 0.0475(9) Uani 1 1 d . . . H26A H 0.2960 0.9529 0.0008 0.057 Uiso 1 1 calc R . . C27 C 0.26728(14) 0.87017(19) 0.01462(14) 0.0449(9) Uani 1 1 d . . . H27A H 0.2715 0.8489 -0.0134 0.054 Uiso 1 1 calc R . . C28 C 0.24620(13) 0.83876(16) 0.04817(12) 0.0339(7) Uani 1 1 d . . . H28A H 0.2367 0.7966 0.0425 0.041 Uiso 1 1 calc R . . C29 C 0.06531(12) 0.71666(13) 0.15125(12) 0.0276(6) Uani 1 1 d . . . C30 C 0.06121(14) 0.76122(14) 0.18705(13) 0.0339(7) Uani 1 1 d . . . H30A H 0.0703 0.8027 0.1839 0.041 Uiso 1 1 calc R . . C31 C 0.04371(17) 0.74395(17) 0.22730(15) 0.0467(9) Uani 1 1 d . . . H31A H 0.0422 0.7737 0.2516 0.056 Uiso 1 1 calc R . . C32 C 0.02858(18) 0.68296(18) 0.23153(16) 0.0534(10) Uani 1 1 d . . . H32A H 0.0158 0.6720 0.2581 0.064 Uiso 1 1 calc R . . C33 C 0.03230(16) 0.63798(16) 0.19655(15) 0.0468(9) Uani 1 1 d . . . H33A H 0.0222 0.5968 0.1996 0.056 Uiso 1 1 calc R . . C34 C 0.05108(14) 0.65461(15) 0.15708(13) 0.0364(7) Uani 1 1 d . . . H34A H 0.0543 0.6241 0.1340 0.044 Uiso 1 1 calc R . . C35 C 0.03728(13) 0.70564(13) 0.03994(12) 0.0289(6) Uani 1 1 d . . . C36 C -0.01969(14) 0.70600(15) 0.03273(14) 0.0399(8) Uani 1 1 d . . . H36A H -0.0303 0.7213 0.0595 0.048 Uiso 1 1 calc R . . C37 C -0.06082(17) 0.68362(18) -0.01437(17) 0.0559(11) Uani 1 1 d . . . H37A H -0.0988 0.6845 -0.0191 0.067 Uiso 1 1 calc R . . C38 C -0.04541(18) 0.66024(17) -0.05386(16) 0.0568(12) Uani 1 1 d . . . H38A H -0.0731 0.6451 -0.0852 0.068 Uiso 1 1 calc R . . C39 C 0.0111(2) 0.65902(16) -0.04736(14) 0.0555(11) Uani 1 1 d . . . H39A H 0.0212 0.6433 -0.0743 0.067 Uiso 1 1 calc R . . C40 C 0.05250(16) 0.68136(15) -0.00036(13) 0.0413(8) Uani 1 1 d . . . H40A H 0.0905 0.6801 0.0042 0.050 Uiso 1 1 calc R . . C41 C 0.16782(12) 0.56362(14) 0.05058(12) 0.0313(7) Uani 1 1 d . . . C42 C 0.14656(15) 0.55977(17) -0.00459(14) 0.0451(9) Uani 1 1 d . . . H42A H 0.1644 0.5810 -0.0236 0.054 Uiso 1 1 calc R . . C43 C 0.09794(18) 0.5237(2) -0.03156(18) 0.0674(14) Uani 1 1 d . . . H43A H 0.0838 0.5203 -0.0685 0.081 Uiso 1 1 calc R . . C44 C 0.07139(18) 0.4936(2) -0.0030(3) 0.0795(17) Uani 1 1 d . . . H44A H 0.0391 0.4699 -0.0210 0.095 Uiso 1 1 calc R . . C45 C 0.09161(18) 0.4978(2) 0.0516(2) 0.0714(14) Uani 1 1 d . . . H45A H 0.0730 0.4775 0.0703 0.086 Uiso 1 1 calc R . . C46 C 0.13987(14) 0.53245(16) 0.07820(17) 0.0483(9) Uani 1 1 d . . . H46A H 0.1539 0.5350 0.1152 0.058 Uiso 1 1 calc R . . C47 C 0.27428(13) 0.61824(15) 0.05356(12) 0.0314(7) Uani 1 1 d . . . C48 C 0.30885(15) 0.67101(17) 0.06281(15) 0.0444(9) Uani 1 1 d . . . H48A H 0.3035 0.7041 0.0826 0.053 Uiso 1 1 calc R . . C49 C 0.35111(18) 0.6746(2) 0.0429(2) 0.0670(13) Uani 1 1 d . . . H49A H 0.3746 0.7095 0.0501 0.080 Uiso 1 1 calc R . . C50 C 0.3583(2) 0.6264(3) 0.0124(2) 0.0723(15) Uani 1 1 d . . . H50A H 0.3860 0.6293 -0.0017 0.087 Uiso 1 1 calc R . . C51 C 0.32468(18) 0.5743(2) 0.00268(16) 0.0608(12) Uani 1 1 d . . . H51A H 0.3300 0.5418 -0.0176 0.073 Uiso 1 1 calc R . . C52 C 0.28243(16) 0.56988(18) 0.02323(13) 0.0444(9) Uani 1 1 d . . . H52A H 0.2597 0.5344 0.0165 0.053 Uiso 1 1 calc R . . C53 C 0.20933(12) 0.62793(14) 0.25463(12) 0.0289(6) Uani 1 1 d . . . C54 C 0.19586(15) 0.67079(16) 0.28613(14) 0.0428(8) Uani 1 1 d . . . H54A H 0.2077 0.7121 0.2877 0.051 Uiso 1 1 calc R . . C55 C 0.16464(17) 0.6518(2) 0.31537(16) 0.0538(10) Uani 1 1 d . . . H55A H 0.1560 0.6807 0.3367 0.065 Uiso 1 1 calc R . . C56 C 0.14631(17) 0.5914(2) 0.31326(16) 0.0541(10) Uani 1 1 d . . . H56A H 0.1263 0.5790 0.3337 0.065 Uiso 1 1 calc R . . C57 C 0.15787(16) 0.54881(17) 0.28037(16) 0.0469(9) Uani 1 1 d . . . H57A H 0.1443 0.5080 0.2778 0.056 Uiso 1 1 calc R . . C58 C 0.18952(14) 0.56684(15) 0.25135(14) 0.0378(7) Uani 1 1 d . . . H58A H 0.1975 0.5380 0.2296 0.045 Uiso 1 1 calc R . . C59 C 0.31134(12) 0.69497(13) 0.25969(12) 0.0286(6) Uani 1 1 d . . . C60 C 0.33151(15) 0.69162(18) 0.31479(14) 0.0451(9) Uani 1 1 d . . . H60A H 0.3128 0.6671 0.3311 0.054 Uiso 1 1 calc R . . C61 C 0.37966(16) 0.7249(2) 0.34570(15) 0.0554(11) Uani 1 1 d . . . H61A H 0.3923 0.7238 0.3827 0.066 Uiso 1 1 calc R . . C62 C 0.40869(16) 0.75959(18) 0.32184(17) 0.0526(10) Uani 1 1 d . . . H62A H 0.4414 0.7810 0.3428 0.063 Uiso 1 1 calc R . . C63 C 0.38959(15) 0.76283(16) 0.26709(16) 0.0468(9) Uani 1 1 d . . . H63A H 0.4093 0.7862 0.2511 0.056 Uiso 1 1 calc R . . C64 C 0.34041(13) 0.73079(14) 0.23591(14) 0.0361(7) Uani 1 1 d . . . H64A H 0.3270 0.7334 0.1990 0.043 Uiso 1 1 calc R . . C117 C 0.76544(12) 0.65088(13) 0.13024(12) 0.0292(6) Uani 1 1 d . . . C118 C 0.74374(15) 0.63122(16) 0.07737(14) 0.0418(8) Uani 1 1 d . . . H11G H 0.7047 0.6311 0.0581 0.050 Uiso 1 1 calc R . . C119 C 0.7797(2) 0.61181(18) 0.05303(18) 0.0584(11) Uani 1 1 d . . . H11H H 0.7646 0.5984 0.0178 0.070 Uiso 1 1 calc R . . C120 C 0.8377(2) 0.61237(18) 0.0808(2) 0.0638(13) Uani 1 1 d . . . H12A H 0.8617 0.5987 0.0646 0.077 Uiso 1 1 calc R . . C121 C 0.85970(17) 0.63310(19) 0.1324(2) 0.0593(12) Uani 1 1 d . . . H12B H 0.8988 0.6341 0.1510 0.071 Uiso 1 1 calc R . . C122 C 0.82399(13) 0.65267(16) 0.15723(15) 0.0414(8) Uani 1 1 d . . . H12C H 0.8395 0.6671 0.1922 0.050 Uiso 1 1 calc R . . C123 C 0.74339(12) 0.64669(14) 0.22749(12) 0.0291(6) Uani 1 1 d . . . C124 C 0.72168(15) 0.67192(17) 0.26290(14) 0.0423(8) Uani 1 1 d . . . H12D H 0.6983 0.7069 0.2530 0.051 Uiso 1 1 calc R . . C125 C 0.73465(18) 0.64542(18) 0.31263(15) 0.0519(10) Uani 1 1 d . . . H12E H 0.7188 0.6615 0.3355 0.062 Uiso 1 1 calc R . . C126 C 0.77122(17) 0.59490(18) 0.32815(14) 0.0499(10) Uani 1 1 d . . . H12F H 0.7806 0.5776 0.3618 0.060 Uiso 1 1 calc R . . C127 C 0.79385(17) 0.57009(17) 0.29386(15) 0.0475(9) Uani 1 1 d . . . H12G H 0.8190 0.5367 0.3046 0.057 Uiso 1 1 calc R . . C128 C 0.77887(14) 0.59529(15) 0.24305(13) 0.0367(7) Uani 1 1 d . . . H12H H 0.7928 0.5774 0.2194 0.044 Uiso 1 1 calc R . . C129 C 0.53503(12) 0.79044(12) 0.06794(12) 0.0254(6) Uani 1 1 d . . . C130 C 0.54411(14) 0.82057(15) 0.02681(13) 0.0352(7) Uani 1 1 d . . . H13A H 0.5808 0.8249 0.0282 0.042 Uiso 1 1 calc R . . C131 C 0.49896(16) 0.84422(16) -0.01633(14) 0.0444(9) Uani 1 1 d . . . H13B H 0.5053 0.8636 -0.0441 0.053 Uiso 1 1 calc R . . C132 C 0.44468(15) 0.83894(15) -0.01787(14) 0.0440(9) Uani 1 1 d . . . H13C H 0.4144 0.8554 -0.0466 0.053 Uiso 1 1 calc R . . C133 C 0.43495(14) 0.80955(16) 0.02263(15) 0.0422(8) Uani 1 1 d . . . H13D H 0.3981 0.8063 0.0212 0.051 Uiso 1 1 calc R . . C134 C 0.47952(13) 0.78469(15) 0.06563(13) 0.0339(7) Uani 1 1 d . . . H13E H 0.4727 0.7643 0.0928 0.041 Uiso 1 1 calc R . . C135 C 0.57188(12) 0.76351(14) 0.17928(12) 0.0285(6) Uani 1 1 d . . . C136 C 0.57897(15) 0.71259(15) 0.21355(14) 0.0388(8) Uani 1 1 d . . . H13F H 0.5935 0.6750 0.2071 0.047 Uiso 1 1 calc R . . C137 C 0.56408(17) 0.71868(18) 0.25761(15) 0.0504(10) Uani 1 1 d . . . H13G H 0.5689 0.6850 0.2806 0.060 Uiso 1 1 calc R . . C138 C 0.54235(16) 0.7739(2) 0.26735(16) 0.0521(10) Uani 1 1 d . . . H13H H 0.5325 0.7775 0.2967 0.062 Uiso 1 1 calc R . . C139 C 0.53514(15) 0.82425(19) 0.23341(15) 0.0473(9) Uani 1 1 d . . . H13I H 0.5203 0.8616 0.2399 0.057 Uiso 1 1 calc R . . C140 C 0.55006(13) 0.81896(16) 0.18994(13) 0.0356(7) Uani 1 1 d . . . H14A H 0.5454 0.8531 0.1674 0.043 Uiso 1 1 calc R . . C141 C 0.77823(12) 0.85518(14) 0.06672(12) 0.0288(6) Uani 1 1 d . . . C142 C 0.78706(14) 0.89701(15) 0.03116(12) 0.0342(7) Uani 1 1 d . . . H14B H 0.7682 0.9352 0.0240 0.041 Uiso 1 1 calc R . . C143 C 0.82385(15) 0.88166(18) 0.00657(14) 0.0447(9) Uani 1 1 d . . . H14C H 0.8288 0.9093 -0.0177 0.054 Uiso 1 1 calc R . . C144 C 0.85319(19) 0.8258(2) 0.01772(19) 0.0613(12) Uani 1 1 d . . . H14D H 0.8783 0.8161 0.0016 0.074 Uiso 1 1 calc R . . C145 C 0.8448(2) 0.78473(19) 0.0530(2) 0.0656(13) Uani 1 1 d . . . H14E H 0.8646 0.7471 0.0608 0.079 Uiso 1 1 calc R . . C146 C 0.80718(16) 0.79891(16) 0.07720(16) 0.0460(9) Uani 1 1 d . . . H14F H 0.8015 0.7704 0.1005 0.055 Uiso 1 1 calc R . . C147 C 0.67738(12) 0.92478(12) 0.06015(11) 0.0247(6) Uani 1 1 d . . . C148 C 0.65323(13) 0.91659(14) 0.00502(12) 0.0314(7) Uani 1 1 d . . . H14G H 0.6687 0.8877 -0.0111 0.038 Uiso 1 1 calc R . . C149 C 0.60607(14) 0.95156(15) -0.02594(13) 0.0392(8) Uani 1 1 d . . . H14H H 0.5906 0.9465 -0.0628 0.047 Uiso 1 1 calc R . . C150 C 0.58216(15) 0.99384(16) -0.00213(15) 0.0444(9) Uani 1 1 d . . . H15D H 0.5510 1.0176 -0.0230 0.053 Uiso 1 1 calc R . . C151 C 0.60476(15) 1.00074(16) 0.05271(15) 0.0452(9) Uani 1 1 d . . . H15E H 0.5882 1.0284 0.0689 0.054 Uiso 1 1 calc R . . C152 C 0.65228(14) 0.96623(15) 0.08362(13) 0.0366(7) Uani 1 1 d . . . H15F H 0.6674 0.9710 0.1205 0.044 Uiso 1 1 calc R . . C153 C 0.80738(13) 0.81171(14) 0.27820(12) 0.0324(7) Uani 1 1 d . . . C154 C 0.84765(14) 0.78829(15) 0.26086(15) 0.0407(8) Uani 1 1 d . . . H15G H 0.8483 0.8020 0.2286 0.049 Uiso 1 1 calc R . . C155 C 0.88736(15) 0.74444(17) 0.29113(17) 0.0523(10) Uani 1 1 d . . . H15H H 0.9149 0.7295 0.2796 0.063 Uiso 1 1 calc R . . C156 C 0.88538(17) 0.72326(18) 0.33868(18) 0.0597(12) Uani 1 1 d . . . H15I H 0.9115 0.6936 0.3589 0.072 Uiso 1 1 calc R . . C157 C 0.84581(18) 0.7453(2) 0.35588(17) 0.0622(12) Uani 1 1 d . . . H15J H 0.8449 0.7306 0.3877 0.075 Uiso 1 1 calc R . . C158 C 0.80647(16) 0.78994(18) 0.32636(15) 0.0505(10) Uani 1 1 d . . . H15K H 0.7797 0.8052 0.3386 0.061 Uiso 1 1 calc R . . C159 C 0.72226(13) 0.90432(14) 0.27428(12) 0.0296(6) Uani 1 1 d . . . C160 C 0.66415(15) 0.91334(17) 0.25513(14) 0.0432(8) Uani 1 1 d . . . H16D H 0.6412 0.8971 0.2221 0.052 Uiso 1 1 calc R . . C161 C 0.63970(18) 0.9466(2) 0.28497(17) 0.0565(11) Uani 1 1 d . . . H16E H 0.6006 0.9525 0.2718 0.068 Uiso 1 1 calc R . . C162 C 0.67329(19) 0.97032(18) 0.33372(17) 0.0559(11) Uani 1 1 d . . . H16F H 0.6569 0.9921 0.3537 0.067 Uiso 1 1 calc R . . C163 C 0.73124(18) 0.96216(18) 0.35329(15) 0.0530(10) Uani 1 1 d . . . H16G H 0.7538 0.9787 0.3863 0.064 Uiso 1 1 calc R . . C164 C 0.75591(14) 0.92961(16) 0.32401(13) 0.0394(8) Uani 1 1 d . . . H16H H 0.7951 0.9244 0.3374 0.047 Uiso 1 1 calc R . . F4 F 1.09184(12) 0.72959(13) 0.44403(10) 0.0744(7) Uani 1 1 d . . . F3 F 1.08165(13) 0.75048(13) 0.35947(11) 0.0850(9) Uani 1 1 d . . . F2 F 1.10194(15) 0.65336(14) 0.39200(12) 0.0996(11) Uani 1 1 d . . . F1 F 1.01568(13) 0.6938(2) 0.37393(14) 0.1249(14) Uani 1 1 d . . . B1 B 1.0725(2) 0.7070(2) 0.3924(2) 0.0536(12) Uani 1 1 d . . . F11 F 0.46532(15) 0.96935(17) 0.34607(12) 0.1093(12) Uani 1 1 d . A . F14 F 0.4592(3) 0.9414(4) 0.26563(17) 0.169(4) Uani 0.837(8) 1 d P A 1 F12 F 0.5225(4) 0.8940(4) 0.3378(3) 0.126(4) Uani 0.837(8) 1 d P A 1 F13 F 0.5327(2) 0.9909(2) 0.3214(3) 0.149(3) Uani 0.837(8) 1 d P A 1 F14A F 0.5024(6) 0.9789(7) 0.2773(5) 0.037(4) Uani 0.163(8) 1 d P A 2 F12A F 0.4576(7) 0.8980(7) 0.2943(10) 0.069(7) Uani 0.163(8) 1 d P A 2 F13A F 0.5429(12) 0.9174(19) 0.3419(13) 0.112(18) Uani 0.163(8) 1 d P A 2 B2 B 0.4933(2) 0.9457(2) 0.3175(2) 0.0545(12) Uani 1 1 d . . . N2 N 0.38071(18) 0.7988(2) 0.13620(18) 0.0843(14) Uani 1 1 d D . . C3S C 0.39661(17) 0.8486(3) 0.13867(17) 0.0680(14) Uani 1 1 d D . . C4S C 0.4177(2) 0.9118(3) 0.1416(2) 0.0899(17) Uani 1 1 d D . . H4S1 H 0.4507 0.9118 0.1328 0.135 Uiso 1 1 calc R . . H4S2 H 0.4277 0.9277 0.1770 0.135 Uiso 1 1 calc R . . H4S3 H 0.3889 0.9378 0.1168 0.135 Uiso 1 1 calc R . . N4 N 0.7944(3) 0.6616(5) -0.0694(3) 0.129(4) Uani 0.775(8) 1 d PD B 3 C7S C 0.7124(3) 0.7300(4) -0.0632(4) 0.114(4) Uani 0.775(8) 1 d PD B 3 H7S1 H 0.7025 0.7128 -0.0353 0.171 Uiso 0.775(8) 1 calc PR B 3 H7S2 H 0.6798 0.7295 -0.0961 0.171 Uiso 0.775(8) 1 calc PR B 3 H7S3 H 0.7253 0.7723 -0.0544 0.171 Uiso 0.775(8) 1 calc PR B 3 C7SA C 0.7878(7) 0.7349(9) -0.0898(5) 0.051(5) Uani 0.225(8) 1 d PD B 4 H7S4 H 0.8228 0.7161 -0.0872 0.076 Uiso 0.225(8) 1 calc PR B 4 H7S5 H 0.7955 0.7731 -0.0698 0.076 Uiso 0.225(8) 1 calc PR B 4 H7S6 H 0.7650 0.7437 -0.1265 0.076 Uiso 0.225(8) 1 calc PR B 4 N4A N 0.7097(14) 0.6593(16) -0.0831(10) 0.177(18) Uani 0.225(8) 1 d PD B 4 C8S C 0.7577(3) 0.6925(4) -0.0688(2) 0.114(3) Uani 1 1 d D . . C2BS C 0.530(2) 1.0590(13) 0.2103(14) 0.039(14) Uani 0.081(4) 1 d PD A 1 H2BA H 0.4912 1.0546 0.2065 0.058 Uiso 0.081(4) 1 calc PR A 1 H2BB H 0.5376 1.1021 0.2057 0.058 Uiso 0.081(4) 1 calc PR A 1 H2BC H 0.5546 1.0452 0.2451 0.058 Uiso 0.081(4) 1 calc PR A 1 N1AS N 0.5604(11) 0.9816(13) 0.1551(12) 0.007(6) Uani 0.081(4) 1 d PD A 1 C2S C 0.5420(5) 1.0747(3) 0.2056(4) 0.152(5) Uani 0.837(8) 1 d PD A 2 H2SA H 0.5797 1.0918 0.2195 0.227 Uiso 0.837(8) 1 calc PR A 2 H2SB H 0.5324 1.0605 0.2345 0.227 Uiso 0.837(8) 1 calc PR A 2 H2SC H 0.5156 1.1063 0.1858 0.227 Uiso 0.837(8) 1 calc PR A 2 N1 N 0.5377(3) 0.9856(3) 0.1417(3) 0.084(2) Uani 0.837(8) 1 d PD A 2 C1S C 0.5397(3) 1.0209(3) 0.1697(2) 0.0841(17) Uani 1 1 d D . . Cl1 Cl -0.2291(4) 1.3103(5) 0.0789(4) 0.085(3) Uani 0.279(17) 1 d PD C 4 Cl2 Cl -0.1232(5) 1.2668(11) 0.0870(7) 0.113(5) Uani 0.279(17) 1 d PD C 4 C5S C -0.1587(4) 1.3091(19) 0.1170(10) 0.082(12) Uani 0.279(17) 1 d PD C 4 H5SA H -0.1441 1.3515 0.1228 0.099 Uiso 0.279(17) 1 calc PR C 4 H5SB H -0.1525 1.2909 0.1515 0.099 Uiso 0.279(17) 1 calc PR C 4 Cl2B Cl -0.1330(10) 1.2319(12) 0.1028(6) 0.118(9) Uani 0.215(17) 1 d PD D 5 Cl1B Cl -0.2356(9) 1.284(2) 0.0812(8) 0.177(12) Uani 0.215(17) 1 d PD D 5 C5SB C -0.1652(10) 1.2952(16) 0.1163(18) 0.23(5) Uani 0.215(17) 1 d PD D 5 H5SC H -0.1570 1.2979 0.1541 0.272 Uiso 0.215(17) 1 calc PR D 5 H5SD H -0.1526 1.3334 0.1050 0.272 Uiso 0.215(17) 1 calc PR D 5 N6S N -0.1602(7) 1.2614(9) 0.0481(6) 0.147(8) Uani 0.430(9) 1 d PD E 6 C6SB C -0.1630(8) 1.3317(8) 0.1192(7) 0.086(6) Uani 0.430(9) 1 d PD E 6 H6SA H -0.1868 1.3238 0.1385 0.128 Uiso 0.430(9) 1 calc PR E 6 H6SB H -0.1757 1.3689 0.0981 0.128 Uiso 0.430(9) 1 calc PR E 6 H6SC H -0.1246 1.3373 0.1439 0.128 Uiso 0.430(9) 1 calc PR E 6 C6S C -0.1657(7) 1.2827(8) 0.0869(9) 0.114(8) Uani 0.430(9) 1 d PD E 6 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 0.02257(11) 0.01908(10) 0.02830(12) 0.00093(8) 0.00833(9) 0.00436(8) Ag2 0.02279(11) 0.01995(11) 0.02823(12) 0.00051(8) 0.00724(9) -0.00445(8) P1 0.0198(3) 0.0196(3) 0.0265(4) 0.0016(3) 0.0069(3) 0.0019(3) P2 0.0206(3) 0.0184(3) 0.0284(4) 0.0001(3) 0.0074(3) 0.0020(3) P3 0.0219(4) 0.0209(3) 0.0237(4) -0.0004(3) 0.0073(3) 0.0028(3) P4 0.0237(4) 0.0216(4) 0.0248(4) 0.0003(3) 0.0085(3) 0.0046(3) P5 0.0214(4) 0.0205(3) 0.0295(4) 0.0019(3) 0.0066(3) -0.0002(3) P6 0.0202(3) 0.0182(3) 0.0278(4) 0.0003(3) 0.0071(3) -0.0012(3) P7 0.0236(4) 0.0210(3) 0.0227(4) -0.0004(3) 0.0071(3) -0.0037(3) P8 0.0222(4) 0.0259(4) 0.0236(4) 0.0012(3) 0.0067(3) -0.0058(3) S1 0.0237(4) 0.0193(3) 0.0409(4) 0.0028(3) 0.0116(3) 0.0027(3) S2 0.0204(3) 0.0212(3) 0.0385(4) 0.0019(3) 0.0081(3) 0.0033(3) S3 0.0245(4) 0.0266(4) 0.0365(4) 0.0008(3) 0.0112(3) 0.0042(3) S4 0.0292(4) 0.0219(3) 0.0355(4) -0.0007(3) 0.0115(3) 0.0026(3) S5 0.0373(4) 0.0266(4) 0.0277(4) -0.0016(3) 0.0066(3) 0.0137(3) S6 0.0338(4) 0.0324(4) 0.0265(4) 0.0048(3) 0.0109(3) 0.0145(3) S7 0.0398(5) 0.0393(4) 0.0277(4) 0.0000(3) 0.0106(3) 0.0185(4) S8 0.0318(4) 0.0291(4) 0.0265(4) 0.0041(3) 0.0116(3) 0.0099(3) S11 0.0251(4) 0.0182(3) 0.0445(4) 0.0006(3) 0.0106(3) -0.0003(3) S12 0.0222(3) 0.0199(3) 0.0348(4) -0.0021(3) 0.0074(3) -0.0028(3) S13 0.0289(4) 0.0214(3) 0.0330(4) -0.0009(3) 0.0092(3) -0.0003(3) S14 0.0252(4) 0.0267(4) 0.0352(4) -0.0031(3) 0.0082(3) -0.0018(3) S15 0.0291(4) 0.0362(4) 0.0232(4) -0.0048(3) 0.0096(3) -0.0139(3) S16 0.0301(4) 0.0299(4) 0.0236(4) 0.0001(3) 0.0075(3) -0.0117(3) S17 0.0298(4) 0.0326(4) 0.0228(3) -0.0046(3) 0.0105(3) -0.0102(3) S18 0.0313(4) 0.0314(4) 0.0232(3) -0.0042(3) 0.0111(3) -0.0110(3) C1 0.0206(13) 0.0202(13) 0.0259(14) 0.0025(11) 0.0073(11) 0.0046(10) C2 0.0221(14) 0.0211(14) 0.0265(14) 0.0020(11) 0.0071(11) 0.0048(11) C3 0.0249(14) 0.0240(14) 0.0245(14) 0.0016(11) 0.0097(12) 0.0029(11) C4 0.0258(14) 0.0222(14) 0.0235(14) 0.0002(11) 0.0092(12) 0.0031(11) C5 0.0364(17) 0.0275(15) 0.0228(14) 0.0001(12) 0.0089(13) 0.0107(13) C6 0.0266(15) 0.0300(15) 0.0233(14) 0.0004(12) 0.0065(12) 0.0103(12) C7 0.051(2) 0.0279(17) 0.043(2) -0.0017(14) 0.0089(17) 0.0109(15) C8 0.0326(18) 0.047(2) 0.0347(17) 0.0030(15) 0.0093(14) 0.0158(15) C9 0.0197(13) 0.0212(13) 0.0279(14) 0.0024(11) 0.0061(11) 0.0045(10) C10 0.0220(14) 0.0233(14) 0.0277(15) 0.0011(11) 0.0086(12) 0.0037(11) C11 0.0303(16) 0.0235(14) 0.0264(15) 0.0030(11) 0.0093(12) 0.0068(12) C12 0.0286(15) 0.0259(15) 0.0268(15) 0.0016(11) 0.0097(12) 0.0068(12) C13 0.0301(16) 0.0274(15) 0.0332(16) 0.0044(12) 0.0138(13) 0.0089(12) C15 0.042(2) 0.0401(19) 0.047(2) 0.0012(16) 0.0227(16) 0.0138(15) C14 0.0253(15) 0.0229(14) 0.0346(16) 0.0036(12) 0.0123(13) 0.0047(11) C16 0.0341(17) 0.0333(17) 0.0337(17) 0.0020(13) 0.0098(14) 0.0044(13) C101 0.0238(14) 0.0233(14) 0.0299(15) -0.0013(11) 0.0090(12) -0.0051(11) C102 0.0216(14) 0.0210(13) 0.0251(14) -0.0006(11) 0.0069(11) -0.0044(10) C103 0.0268(15) 0.0259(15) 0.0256(14) -0.0014(11) 0.0109(12) -0.0044(11) C104 0.0266(15) 0.0241(14) 0.0234(14) -0.0038(11) 0.0100(12) -0.0057(11) C105 0.0267(15) 0.0258(15) 0.0262(15) -0.0045(11) 0.0095(12) -0.0063(11) C106 0.0270(15) 0.0259(15) 0.0326(16) -0.0048(12) 0.0119(13) -0.0070(12) C107 0.0301(17) 0.047(2) 0.0320(17) -0.0057(14) 0.0065(14) -0.0120(14) C108 0.0350(18) 0.0415(19) 0.0397(18) -0.0015(15) 0.0192(15) -0.0132(14) C109 0.0248(14) 0.0185(13) 0.0280(15) -0.0017(11) 0.0104(12) -0.0035(11) C110 0.0233(14) 0.0195(13) 0.0280(15) 0.0004(11) 0.0099(12) -0.0027(11) C111 0.0252(14) 0.0193(13) 0.0256(14) 0.0010(11) 0.0096(12) -0.0010(11) C112 0.0243(14) 0.0216(13) 0.0195(13) -0.0002(10) 0.0062(11) -0.0014(11) C113 0.0335(16) 0.0258(15) 0.0247(15) -0.0023(12) 0.0062(13) -0.0114(12) C114 0.0386(17) 0.0230(14) 0.0250(15) -0.0023(11) 0.0083(13) -0.0088(12) C115 0.0352(19) 0.044(2) 0.046(2) -0.0055(16) 0.0027(16) -0.0159(16) C116 0.052(2) 0.0238(16) 0.044(2) -0.0014(14) 0.0095(17) -0.0046(15) C17 0.0269(15) 0.0198(14) 0.0268(15) 0.0018(11) 0.0054(12) 0.0052(11) C18 0.0317(17) 0.0367(17) 0.0321(17) -0.0011(13) 0.0098(14) 0.0000(13) C19 0.045(2) 0.048(2) 0.0322(17) 0.0011(15) 0.0150(16) 0.0055(16) C20 0.054(2) 0.0394(19) 0.0280(17) -0.0024(14) 0.0030(16) 0.0102(16) C21 0.0331(18) 0.0338(18) 0.0385(18) -0.0029(14) 0.0009(15) 0.0007(14) C22 0.0284(16) 0.0278(16) 0.0388(17) -0.0012(13) 0.0094(14) -0.0005(12) C23 0.0190(14) 0.0303(15) 0.0300(15) 0.0078(12) 0.0089(12) 0.0035(11) C24 0.0239(15) 0.0289(16) 0.0402(18) 0.0071(13) 0.0071(13) 0.0004(12) C25 0.0303(17) 0.0402(19) 0.050(2) 0.0155(16) 0.0085(16) -0.0060(14) C26 0.0294(18) 0.063(2) 0.050(2) 0.0259(19) 0.0154(16) -0.0002(16) C27 0.0336(18) 0.064(2) 0.041(2) 0.0125(17) 0.0177(16) 0.0098(17) C28 0.0255(15) 0.0377(18) 0.0367(17) 0.0054(14) 0.0100(13) 0.0037(13) C29 0.0235(14) 0.0237(14) 0.0331(16) 0.0029(12) 0.0083(12) 0.0038(11) C30 0.0426(18) 0.0248(16) 0.0368(17) 0.0033(13) 0.0183(15) 0.0043(13) C31 0.065(2) 0.0360(19) 0.049(2) 0.0026(16) 0.0331(19) 0.0107(17) C32 0.070(3) 0.046(2) 0.060(2) 0.0207(19) 0.042(2) 0.012(2) C33 0.055(2) 0.0309(18) 0.059(2) 0.0105(16) 0.0269(19) -0.0026(16) C34 0.0397(18) 0.0277(16) 0.0404(18) 0.0020(14) 0.0141(15) -0.0012(14) C35 0.0305(16) 0.0178(14) 0.0319(16) 0.0019(11) 0.0048(13) 0.0035(11) C36 0.0341(18) 0.0335(18) 0.044(2) 0.0012(14) 0.0068(15) -0.0068(14) C37 0.040(2) 0.046(2) 0.059(3) 0.0077(19) -0.0061(19) -0.0134(17) C38 0.063(3) 0.0321(19) 0.042(2) 0.0045(16) -0.0170(19) -0.0092(18) C39 0.088(3) 0.0306(19) 0.0314(19) -0.0030(15) 0.005(2) 0.0092(19) C40 0.050(2) 0.0319(17) 0.0356(18) 0.0003(14) 0.0097(16) 0.0129(15) C41 0.0235(15) 0.0240(15) 0.0378(17) -0.0022(12) 0.0024(13) 0.0065(12) C42 0.0347(18) 0.046(2) 0.0398(19) -0.0137(16) -0.0018(15) 0.0098(15) C43 0.047(2) 0.060(3) 0.061(3) -0.032(2) -0.017(2) 0.015(2) C44 0.036(2) 0.042(2) 0.124(5) -0.023(3) -0.009(3) -0.0043(19) C45 0.040(2) 0.046(2) 0.113(4) 0.008(3) 0.012(3) -0.0143(19) C46 0.0298(18) 0.0368(19) 0.068(3) 0.0102(17) 0.0074(17) -0.0038(15) C47 0.0295(16) 0.0350(17) 0.0327(16) 0.0076(13) 0.0152(13) 0.0096(13) C48 0.041(2) 0.0385(19) 0.060(2) 0.0106(17) 0.0272(18) 0.0055(15) C49 0.048(2) 0.071(3) 0.094(4) 0.030(3) 0.041(2) 0.005(2) C50 0.061(3) 0.098(4) 0.079(3) 0.037(3) 0.050(3) 0.030(3) C51 0.064(3) 0.082(3) 0.049(2) 0.011(2) 0.036(2) 0.035(2) C52 0.048(2) 0.049(2) 0.0395(19) 0.0014(16) 0.0196(17) 0.0165(17) C53 0.0285(15) 0.0307(16) 0.0302(15) 0.0040(12) 0.0143(13) 0.0065(12) C54 0.049(2) 0.0352(18) 0.052(2) -0.0047(16) 0.0276(18) 0.0022(15) C55 0.060(3) 0.058(3) 0.058(2) -0.005(2) 0.039(2) 0.008(2) C56 0.052(2) 0.064(3) 0.061(3) 0.018(2) 0.038(2) 0.011(2) C57 0.053(2) 0.0368(19) 0.063(2) 0.0132(17) 0.036(2) 0.0057(16) C58 0.0396(19) 0.0337(17) 0.047(2) 0.0051(15) 0.0237(16) 0.0060(14) C59 0.0252(15) 0.0258(15) 0.0303(16) -0.0050(12) 0.0059(12) 0.0033(12) C60 0.0352(19) 0.061(2) 0.0349(19) -0.0073(16) 0.0089(15) 0.0023(17) C61 0.040(2) 0.077(3) 0.037(2) -0.022(2) 0.0013(17) 0.004(2) C62 0.0340(19) 0.043(2) 0.064(3) -0.0213(19) 0.0002(18) 0.0016(16) C63 0.0344(19) 0.0325(18) 0.064(3) 0.0031(17) 0.0082(17) 0.0005(14) C64 0.0284(16) 0.0284(16) 0.0437(19) 0.0031(14) 0.0054(14) 0.0034(13) C117 0.0277(15) 0.0212(14) 0.0407(17) 0.0043(12) 0.0153(13) 0.0013(11) C118 0.042(2) 0.0420(19) 0.045(2) -0.0044(16) 0.0215(16) -0.0118(15) C119 0.079(3) 0.050(2) 0.065(3) -0.010(2) 0.048(2) -0.013(2) C120 0.080(3) 0.043(2) 0.101(4) 0.005(2) 0.071(3) 0.007(2) C121 0.040(2) 0.054(2) 0.094(3) 0.020(2) 0.038(2) 0.0119(18) C122 0.0277(17) 0.0408(19) 0.053(2) 0.0080(16) 0.0128(15) 0.0018(14) C123 0.0272(15) 0.0244(15) 0.0310(16) 0.0000(12) 0.0060(13) -0.0029(12) C124 0.046(2) 0.040(2) 0.0399(19) 0.0027(15) 0.0158(16) 0.0065(16) C125 0.066(3) 0.052(2) 0.042(2) 0.0042(17) 0.0245(19) 0.006(2) C126 0.061(2) 0.045(2) 0.0335(19) 0.0100(16) 0.0072(18) -0.0104(18) C127 0.056(2) 0.0348(19) 0.046(2) 0.0162(16) 0.0126(18) 0.0075(16) C128 0.0391(18) 0.0309(17) 0.0374(18) 0.0055(14) 0.0116(15) 0.0009(14) C129 0.0246(14) 0.0178(13) 0.0294(15) -0.0017(11) 0.0055(12) -0.0007(11) C130 0.0336(17) 0.0345(17) 0.0350(17) 0.0024(14) 0.0106(14) -0.0040(13) C131 0.054(2) 0.0366(19) 0.0346(18) 0.0089(15) 0.0084(16) -0.0027(16) C132 0.044(2) 0.0273(17) 0.042(2) 0.0012(14) -0.0049(16) 0.0017(14) C133 0.0259(17) 0.0411(19) 0.050(2) 0.0008(16) 0.0044(15) 0.0003(14) C134 0.0255(16) 0.0342(17) 0.0381(18) 0.0047(13) 0.0080(14) -0.0002(13) C135 0.0210(14) 0.0311(16) 0.0324(16) -0.0032(12) 0.0093(12) -0.0036(12) C136 0.049(2) 0.0318(17) 0.0412(19) -0.0028(14) 0.0234(16) -0.0088(15) C137 0.064(3) 0.050(2) 0.043(2) -0.0027(17) 0.0275(19) -0.0190(19) C138 0.049(2) 0.071(3) 0.049(2) -0.016(2) 0.0321(19) -0.016(2) C139 0.0358(19) 0.057(2) 0.050(2) -0.0128(18) 0.0181(17) 0.0057(17) C140 0.0278(16) 0.0365(18) 0.0396(18) -0.0029(14) 0.0100(14) 0.0047(13) C141 0.0290(15) 0.0271(15) 0.0301(15) -0.0041(12) 0.0112(13) -0.0046(12) C142 0.0380(18) 0.0325(17) 0.0344(17) 0.0005(13) 0.0164(14) -0.0045(14) C143 0.049(2) 0.050(2) 0.044(2) -0.0056(16) 0.0276(17) -0.0142(17) C144 0.066(3) 0.055(3) 0.087(3) -0.010(2) 0.056(3) -0.009(2) C145 0.072(3) 0.043(2) 0.110(4) 0.008(2) 0.067(3) 0.014(2) C146 0.055(2) 0.0318(18) 0.065(3) 0.0094(16) 0.038(2) 0.0030(16) C147 0.0242(14) 0.0187(13) 0.0283(15) -0.0001(11) 0.0069(12) -0.0039(11) C148 0.0336(17) 0.0280(16) 0.0296(16) -0.0013(12) 0.0091(13) -0.0024(13) C149 0.0411(19) 0.0360(18) 0.0287(16) 0.0048(14) 0.0007(14) -0.0065(14) C150 0.0389(19) 0.0341(18) 0.049(2) 0.0079(16) 0.0048(16) 0.0052(15) C151 0.048(2) 0.0351(19) 0.050(2) 0.0003(16) 0.0159(18) 0.0134(16) C152 0.0425(19) 0.0336(17) 0.0306(16) -0.0049(13) 0.0106(14) 0.0038(14) C153 0.0275(16) 0.0285(15) 0.0327(16) 0.0064(13) 0.0023(13) -0.0065(12) C154 0.0301(17) 0.0355(18) 0.048(2) 0.0023(15) 0.0062(15) -0.0045(14) C155 0.0323(19) 0.039(2) 0.071(3) -0.0018(19) 0.0041(18) -0.0039(15) C156 0.039(2) 0.040(2) 0.069(3) 0.017(2) -0.014(2) -0.0024(17) C157 0.051(2) 0.068(3) 0.049(2) 0.030(2) -0.001(2) -0.002(2) C158 0.045(2) 0.059(2) 0.043(2) 0.0199(18) 0.0123(17) -0.0033(18) C159 0.0305(16) 0.0311(16) 0.0296(16) -0.0024(12) 0.0141(13) -0.0088(12) C160 0.0362(19) 0.050(2) 0.044(2) -0.0102(16) 0.0164(16) -0.0039(16) C161 0.047(2) 0.064(3) 0.068(3) -0.009(2) 0.033(2) 0.003(2) C162 0.073(3) 0.045(2) 0.069(3) -0.015(2) 0.049(2) -0.012(2) C163 0.070(3) 0.055(2) 0.043(2) -0.0209(18) 0.032(2) -0.029(2) C164 0.0355(18) 0.050(2) 0.0331(17) -0.0086(15) 0.0132(14) -0.0170(15) F4 0.0873(19) 0.0792(18) 0.0630(16) -0.0068(14) 0.0358(15) -0.0014(15) F3 0.109(2) 0.0716(18) 0.0701(18) 0.0292(15) 0.0300(17) 0.0165(16) F2 0.165(3) 0.0735(19) 0.102(2) 0.0328(17) 0.098(2) 0.051(2) F1 0.068(2) 0.206(4) 0.101(3) -0.041(3) 0.0330(19) -0.035(2) B1 0.059(3) 0.052(3) 0.061(3) 0.006(2) 0.035(3) 0.015(2) F11 0.121(3) 0.142(3) 0.086(2) -0.006(2) 0.064(2) 0.045(2) F14 0.178(6) 0.228(8) 0.054(3) -0.037(4) -0.008(3) 0.121(6) F12 0.230(10) 0.086(3) 0.077(4) 0.032(3) 0.077(6) 0.080(5) F13 0.111(4) 0.118(4) 0.246(9) 0.053(5) 0.101(5) 0.023(3) F14A 0.036(8) 0.060(9) 0.013(6) 0.026(5) 0.005(5) 0.014(6) F12A 0.038(9) 0.050(10) 0.136(19) -0.032(10) 0.050(11) -0.030(7) F13A 0.062(13) 0.23(5) 0.036(10) 0.01(2) 0.015(10) 0.11(2) B2 0.060(3) 0.056(3) 0.052(3) -0.001(2) 0.026(2) 0.012(2) N2 0.056(3) 0.121(4) 0.073(3) -0.004(3) 0.021(2) -0.016(3) C3S 0.027(2) 0.127(5) 0.045(2) -0.001(3) 0.0092(18) 0.008(3) C4S 0.051(3) 0.100(4) 0.097(4) 0.002(3) 0.004(3) 0.014(3) N4 0.055(4) 0.252(11) 0.078(4) -0.062(6) 0.023(3) 0.003(5) C7S 0.071(5) 0.147(9) 0.116(7) 0.045(6) 0.027(5) 0.044(5) C7SA 0.070(12) 0.069(13) 0.011(7) -0.008(7) 0.013(7) -0.023(10) N4A 0.24(3) 0.25(4) 0.106(18) -0.12(2) 0.14(2) -0.19(3) C8S 0.081(5) 0.190(8) 0.057(3) 0.012(4) 0.010(3) -0.037(5) C2BS 0.13(4) 0.000(15) 0.001(14) 0.017(11) 0.036(19) -0.01(2) N1AS 0.000(12) 0.000(11) 0.018(16) 0.001(10) -0.002(11) 0.014(9) C2S 0.330(15) 0.057(5) 0.158(8) 0.065(5) 0.192(10) 0.111(7) N1 0.096(6) 0.095(5) 0.055(4) 0.001(3) 0.022(4) -0.021(4) C1S 0.081(4) 0.114(5) 0.054(3) 0.008(3) 0.022(3) -0.017(4) Cl1 0.078(5) 0.116(6) 0.053(3) 0.019(3) 0.018(3) 0.059(4) Cl2 0.103(6) 0.133(11) 0.129(9) -0.049(8) 0.074(6) -0.006(6) C5S 0.051(11) 0.10(2) 0.085(18) -0.080(19) 0.011(11) 0.028(12) Cl2B 0.129(12) 0.119(12) 0.088(7) -0.033(7) 0.022(6) 0.062(10) Cl1B 0.187(17) 0.27(3) 0.093(9) 0.006(13) 0.080(10) 0.079(16) C5SB 0.34(9) 0.10(3) 0.08(3) -0.07(2) -0.10(4) 0.14(4) N6S 0.095(11) 0.23(2) 0.100(12) -0.063(13) 0.017(10) 0.020(11) C6SB 0.116(14) 0.065(12) 0.085(11) -0.017(8) 0.049(10) 0.024(9) C6S 0.077(12) 0.079(10) 0.142(18) -0.045(11) -0.008(11) 0.035(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 P3 2.4933(8) . ? Ag1 P2 2.5013(10) . ? Ag1 P1 2.5118(9) . ? Ag1 P4 2.5184(10) . ? Ag2 P6 2.4790(9) . ? Ag2 P7 2.4826(8) . ? Ag2 P8 2.4944(10) . ? Ag2 P5 2.5071(9) . ? P1 C17 1.825(3) . ? P1 C1 1.832(3) . ? P1 C23 1.833(3) . ? P2 C29 1.814(3) . ? P2 C35 1.818(3) . ? P2 C2 1.830(3) . ? P3 C47 1.819(3) . ? P3 C41 1.824(3) . ? P3 C9 1.831(3) . ? P4 C53 1.818(3) . ? P4 C10 1.820(3) . ? P4 C59 1.835(3) . ? P5 C117 1.822(3) . ? P5 C110 1.824(3) . ? P5 C123 1.833(3) . ? P6 C129 1.825(3) . ? P6 C135 1.825(3) . ? P6 C109 1.831(3) . ? P7 C141 1.826(3) . ? P7 C147 1.828(3) . ? P7 C102 1.834(3) . ? P8 C101 1.821(3) . ? P8 C159 1.822(3) . ? P8 C153 1.822(3) . ? S1 C3 1.759(3) . ? S1 C1 1.763(3) . ? S2 C2 1.759(3) . ? S2 C3 1.769(3) . ? S3 C6 1.754(3) . ? S3 C4 1.756(3) . ? S4 C4 1.758(3) . ? S4 C5 1.773(3) . ? S5 C11 1.756(3) . ? S5 C9 1.759(3) . ? S6 C11 1.762(3) . ? S6 C10 1.765(3) . ? S7 C12 1.756(3) . ? S7 C13 1.765(3) . ? S8 C12 1.755(3) . ? S8 C14 1.773(3) . ? S11 C111 1.759(3) . ? S11 C110 1.759(3) . ? S12 C109 1.752(3) . ? S12 C111 1.767(3) . ? S13 C112 1.756(3) . ? S13 C114 1.762(3) . ? S14 C112 1.756(3) . ? S14 C113 1.765(3) . ? S15 C101 1.754(3) . ? S15 C103 1.759(3) . ? S16 C102 1.766(3) . ? S16 C103 1.766(3) . ? S17 C104 1.755(3) . ? S17 C105 1.773(3) . ? S18 C104 1.750(3) . ? S18 C106 1.770(3) . ? C1 C2 1.349(4) . ? C3 C4 1.346(4) . ? C5 C6 1.325(4) . ? C5 C7 1.504(4) . ? C6 C8 1.507(4) . ? C9 C10 1.353(4) . ? C11 C12 1.343(4) . ? C13 C14 1.331(4) . ? C13 C15 1.498(4) . ? C14 C16 1.496(4) . ? C101 C102 1.353(4) . ? C103 C104 1.345(4) . ? C105 C106 1.325(4) . ? C105 C107 1.502(4) . ? C106 C108 1.494(4) . ? C109 C110 1.351(4) . ? C111 C112 1.339(4) . ? C113 C114 1.337(4) . ? C113 C115 1.502(4) . ? C114 C116 1.490(4) . ? C17 C22 1.392(4) . ? C17 C18 1.404(4) . ? C18 C19 1.388(4) . ? C19 C20 1.383(5) . ? C20 C21 1.367(5) . ? C21 C22 1.405(4) . ? C23 C28 1.393(4) . ? C23 C24 1.396(4) . ? C24 C25 1.389(4) . ? C25 C26 1.390(5) . ? C26 C27 1.373(5) . ? C27 C28 1.398(4) . ? C29 C30 1.395(4) . ? C29 C34 1.400(4) . ? C30 C31 1.384(5) . ? C31 C32 1.377(5) . ? C32 C33 1.382(5) . ? C33 C34 1.382(5) . ? C35 C36 1.393(5) . ? C35 C40 1.397(5) . ? C36 C37 1.391(5) . ? C37 C38 1.374(6) . ? C38 C39 1.385(6) . ? C39 C40 1.392(5) . ? C41 C42 1.387(5) . ? C41 C46 1.391(5) . ? C42 C43 1.404(5) . ? C43 C44 1.373(7) . ? C44 C45 1.374(7) . ? C45 C46 1.380(5) . ? C47 C52 1.388(4) . ? C47 C48 1.395(5) . ? C48 C49 1.386(5) . ? C49 C50 1.379(7) . ? C50 C51 1.368(7) . ? C51 C52 1.399(5) . ? C53 C54 1.386(4) . ? C53 C58 1.391(4) . ? C54 C55 1.388(5) . ? C55 C56 1.368(6) . ? C56 C57 1.386(5) . ? C57 C58 1.386(5) . ? C59 C60 1.386(5) . ? C59 C64 1.389(4) . ? C60 C61 1.389(5) . ? C61 C62 1.376(6) . ? C62 C63 1.378(6) . ? C63 C64 1.395(5) . ? C117 C122 1.390(4) . ? C117 C118 1.392(5) . ? C118 C119 1.388(5) . ? C119 C120 1.380(6) . ? C120 C121 1.369(6) . ? C121 C122 1.393(5) . ? C123 C128 1.383(4) . ? C123 C124 1.393(4) . ? C124 C125 1.384(5) . ? C125 C126 1.383(5) . ? C126 C127 1.380(5) . ? C127 C128 1.392(5) . ? C129 C130 1.386(4) . ? C129 C134 1.402(4) . ? C130 C131 1.385(5) . ? C131 C132 1.377(5) . ? C132 C133 1.372(5) . ? C133 C134 1.385(4) . ? C135 C140 1.388(4) . ? C135 C136 1.399(4) . ? C136 C137 1.397(5) . ? C137 C138 1.374(5) . ? C138 C139 1.383(6) . ? C139 C140 1.381(5) . ? C141 C146 1.383(4) . ? C141 C142 1.398(4) . ? C142 C143 1.388(5) . ? C143 C144 1.379(6) . ? C144 C145 1.378(6) . ? C145 C146 1.394(5) . ? C147 C152 1.386(4) . ? C147 C148 1.395(4) . ? C148 C149 1.392(4) . ? C149 C150 1.384(5) . ? C150 C151 1.384(5) . ? C151 C152 1.392(5) . ? C153 C154 1.382(5) . ? C153 C158 1.399(5) . ? C154 C155 1.393(5) . ? C155 C156 1.390(6) . ? C156 C157 1.354(6) . ? C157 C158 1.393(5) . ? C159 C160 1.385(4) . ? C159 C164 1.401(4) . ? C160 C161 1.395(5) . ? C161 C162 1.369(6) . ? C162 C163 1.378(6) . ? C163 C164 1.380(5) . ? F4 B1 1.382(6) . ? F3 B1 1.374(5) . ? F2 B1 1.374(5) . ? F1 B1 1.370(6) . ? F11 B2 1.341(5) . ? F14 B2 1.345(6) . ? F12 B2 1.328(8) . ? F13 B2 1.371(7) . ? F14A B2 1.398(12) . ? F12A B2 1.350(14) . ? F13A B2 1.33(2) . ? N2 C3S 1.132(7) . ? C3S C4S 1.445(8) . ? N4 C8S 1.152(10) . ? C7S C8S 1.463(11) . ? C7SA C8S 1.444(15) . ? N4A C8S 1.337(18) . ? C2BS C1S 1.47(3) . ? N1AS C1S 1.14(2) . ? C2S C1S 1.493(9) . ? N1 C1S 1.061(8) . ? Cl1 C5S 1.6964(12) . ? Cl2 C5S 1.6955(11) . ? Cl2B C5SB 1.6963(12) . ? Cl1B C5SB 1.6959(13) . ? N6S C6S 1.21(2) . ? C6SB C6S 1.352(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 P3 Ag1 P2 120.85(3) . . ? P3 Ag1 P1 138.82(3) . . ? P2 Ag1 P1 84.65(2) . . ? P3 Ag1 P4 84.61(3) . . ? P2 Ag1 P4 117.40(4) . . ? P1 Ag1 P4 113.48(3) . . ? P6 Ag2 P7 127.27(3) . . ? P6 Ag2 P8 124.88(3) . . ? P7 Ag2 P8 86.06(3) . . ? P6 Ag2 P5 85.24(3) . . ? P7 Ag2 P5 124.36(3) . . ? P8 Ag2 P5 112.67(3) . . ? C17 P1 C1 102.44(13) . . ? C17 P1 C23 106.89(14) . . ? C1 P1 C23 102.64(13) . . ? C17 P1 Ag1 113.58(9) . . ? C1 P1 Ag1 103.42(9) . . ? C23 P1 Ag1 124.86(10) . . ? C29 P2 C35 102.87(14) . . ? C29 P2 C2 104.89(13) . . ? C35 P2 C2 104.07(13) . . ? C29 P2 Ag1 115.27(10) . . ? C35 P2 Ag1 123.57(11) . . ? C2 P2 Ag1 104.30(9) . . ? C47 P3 C41 107.29(15) . . ? C47 P3 C9 101.13(13) . . ? C41 P3 C9 102.20(14) . . ? C47 P3 Ag1 124.95(11) . . ? C41 P3 Ag1 113.98(10) . . ? C9 P3 Ag1 103.90(9) . . ? C53 P4 C10 103.42(13) . . ? C53 P4 C59 106.78(14) . . ? C10 P4 C59 102.39(13) . . ? C53 P4 Ag1 121.59(10) . . ? C10 P4 Ag1 104.27(9) . . ? C59 P4 Ag1 115.82(11) . . ? C117 P5 C110 105.56(13) . . ? C117 P5 C123 105.67(14) . . ? C110 P5 C123 101.47(13) . . ? C117 P5 Ag2 119.41(9) . . ? C110 P5 Ag2 101.98(9) . . ? C123 P5 Ag2 120.12(10) . . ? C129 P6 C135 103.29(14) . . ? C129 P6 C109 105.46(13) . . ? C135 P6 C109 103.36(13) . . ? C129 P6 Ag2 126.51(10) . . ? C135 P6 Ag2 113.37(10) . . ? C109 P6 Ag2 102.43(9) . . ? C141 P7 C147 106.17(14) . . ? C141 P7 C102 102.16(13) . . ? C147 P7 C102 104.76(13) . . ? C141 P7 Ag2 126.87(10) . . ? C147 P7 Ag2 111.42(9) . . ? C102 P7 Ag2 102.95(9) . . ? C101 P8 C159 104.06(13) . . ? C101 P8 C153 103.34(14) . . ? C159 P8 C153 106.17(15) . . ? C101 P8 Ag2 102.85(9) . . ? C159 P8 Ag2 128.24(10) . . ? C153 P8 Ag2 109.44(11) . . ? C3 S1 C1 95.77(13) . . ? C2 S2 C3 95.63(13) . . ? C6 S3 C4 95.94(14) . . ? C4 S4 C5 95.64(14) . . ? C11 S5 C9 94.43(13) . . ? C11 S6 C10 93.98(13) . . ? C12 S7 C13 95.34(14) . . ? C12 S8 C14 95.18(14) . . ? C111 S11 C110 95.57(13) . . ? C109 S12 C111 95.26(13) . . ? C112 S13 C114 96.18(14) . . ? C112 S14 C113 95.82(14) . . ? C101 S15 C103 94.77(13) . . ? C102 S16 C103 94.62(13) . . ? C104 S17 C105 95.44(13) . . ? C104 S18 C106 95.48(14) . . ? C2 C1 S1 117.1(2) . . ? C2 C1 P1 124.3(2) . . ? S1 C1 P1 118.58(15) . . ? C1 C2 S2 117.2(2) . . ? C1 C2 P2 122.9(2) . . ? S2 C2 P2 119.93(16) . . ? C4 C3 S1 123.5(2) . . ? C4 C3 S2 122.7(2) . . ? S1 C3 S2 113.84(15) . . ? C3 C4 S3 122.5(2) . . ? C3 C4 S4 123.8(2) . . ? S3 C4 S4 113.66(15) . . ? C6 C5 C7 127.5(3) . . ? C6 C5 S4 116.9(2) . . ? C7 C5 S4 115.6(2) . . ? C5 C6 C8 127.2(3) . . ? C5 C6 S3 117.7(2) . . ? C8 C6 S3 115.0(2) . . ? C10 C9 S5 116.5(2) . . ? C10 C9 P3 124.4(2) . . ? S5 C9 P3 119.03(16) . . ? C9 C10 S6 116.9(2) . . ? C9 C10 P4 122.8(2) . . ? S6 C10 P4 120.39(16) . . ? C12 C11 S5 121.8(2) . . ? C12 C11 S6 125.1(2) . . ? S5 C11 S6 113.10(15) . . ? C11 C12 S8 125.0(2) . . ? C11 C12 S7 121.5(2) . . ? S8 C12 S7 113.56(16) . . ? C14 C13 C15 128.3(3) . . ? C14 C13 S7 117.0(2) . . ? C15 C13 S7 114.7(2) . . ? C13 C14 C16 126.5(3) . . ? C13 C14 S8 117.0(2) . . ? C16 C14 S8 116.4(2) . . ? C102 C101 S15 117.3(2) . . ? C102 C101 P8 124.2(2) . . ? S15 C101 P8 118.52(16) . . ? C101 C102 S16 116.5(2) . . ? C101 C102 P7 123.8(2) . . ? S16 C102 P7 119.63(15) . . ? C104 C103 S15 122.6(2) . . ? C104 C103 S16 124.0(2) . . ? S15 C103 S16 113.46(15) . . ? C103 C104 S18 123.3(2) . . ? C103 C104 S17 122.4(2) . . ? S18 C104 S17 114.27(15) . . ? C106 C105 C107 127.1(3) . . ? C106 C105 S17 117.0(2) . . ? C107 C105 S17 115.8(2) . . ? C105 C106 C108 127.7(3) . . ? C105 C106 S18 117.4(2) . . ? C108 C106 S18 114.8(2) . . ? C110 C109 S12 117.7(2) . . ? C110 C109 P6 123.6(2) . . ? S12 C109 P6 118.51(16) . . ? C109 C110 S11 116.9(2) . . ? C109 C110 P5 123.6(2) . . ? S11 C110 P5 119.18(15) . . ? C112 C111 S11 123.0(2) . . ? C112 C111 S12 122.7(2) . . ? S11 C111 S12 114.37(15) . . ? C111 C112 S14 122.9(2) . . ? C111 C112 S13 123.3(2) . . ? S14 C112 S13 113.79(15) . . ? C114 C113 C115 127.1(3) . . ? C114 C113 S14 117.4(2) . . ? C115 C113 S14 115.6(2) . . ? C113 C114 C116 127.3(3) . . ? C113 C114 S13 116.8(2) . . ? C116 C114 S13 115.9(2) . . ? C22 C17 C18 118.7(3) . . ? C22 C17 P1 122.7(2) . . ? C18 C17 P1 117.9(2) . . ? C19 C18 C17 120.2(3) . . ? C20 C19 C18 120.3(3) . . ? C21 C20 C19 120.4(3) . . ? C20 C21 C22 120.1(3) . . ? C17 C22 C21 120.2(3) . . ? C28 C23 C24 119.2(3) . . ? C28 C23 P1 116.6(2) . . ? C24 C23 P1 124.2(2) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 120.4(3) . . ? C27 C26 C25 120.0(3) . . ? C26 C27 C28 120.2(3) . . ? C23 C28 C27 120.2(3) . . ? C30 C29 C34 118.3(3) . . ? C30 C29 P2 123.4(2) . . ? C34 C29 P2 118.1(2) . . ? C31 C30 C29 120.3(3) . . ? C32 C31 C30 120.4(3) . . ? C31 C32 C33 120.3(3) . . ? C34 C33 C32 119.6(3) . . ? C33 C34 C29 121.0(3) . . ? C36 C35 C40 119.0(3) . . ? C36 C35 P2 122.5(3) . . ? C40 C35 P2 118.5(2) . . ? C37 C36 C35 120.3(4) . . ? C38 C37 C36 120.2(4) . . ? C37 C38 C39 120.5(3) . . ? C38 C39 C40 119.8(4) . . ? C39 C40 C35 120.3(4) . . ? C42 C41 C46 119.2(3) . . ? C42 C41 P3 122.3(3) . . ? C46 C41 P3 118.0(3) . . ? C41 C42 C43 119.7(4) . . ? C44 C43 C42 119.5(4) . . ? C43 C44 C45 121.3(4) . . ? C44 C45 C46 119.3(5) . . ? C45 C46 C41 121.0(4) . . ? C52 C47 C48 118.6(3) . . ? C52 C47 P3 125.2(3) . . ? C48 C47 P3 116.0(2) . . ? C49 C48 C47 120.6(4) . . ? C50 C49 C48 120.0(4) . . ? C51 C50 C49 120.3(4) . . ? C50 C51 C52 120.2(4) . . ? C47 C52 C51 120.2(4) . . ? C54 C53 C58 119.2(3) . . ? C54 C53 P4 118.3(2) . . ? C58 C53 P4 122.2(2) . . ? C53 C54 C55 119.8(3) . . ? C56 C55 C54 121.0(4) . . ? C55 C56 C57 119.5(3) . . ? C58 C57 C56 120.2(3) . . ? C57 C58 C53 120.2(3) . . ? C60 C59 C64 119.3(3) . . ? C60 C59 P4 124.5(3) . . ? C64 C59 P4 116.1(2) . . ? C59 C60 C61 120.0(4) . . ? C62 C61 C60 120.2(4) . . ? C61 C62 C63 120.4(3) . . ? C62 C63 C64 119.5(4) . . ? C59 C64 C63 120.4(3) . . ? C122 C117 C118 118.2(3) . . ? C122 C117 P5 119.5(3) . . ? C118 C117 P5 121.9(2) . . ? C119 C118 C117 120.7(4) . . ? C120 C119 C118 120.4(4) . . ? C121 C120 C119 119.5(4) . . ? C120 C121 C122 120.5(4) . . ? C117 C122 C121 120.6(4) . . ? C128 C123 C124 119.0(3) . . ? C128 C123 P5 124.5(2) . . ? C124 C123 P5 116.4(2) . . ? C125 C124 C123 120.6(3) . . ? C126 C125 C124 119.7(4) . . ? C127 C126 C125 120.3(3) . . ? C126 C127 C128 119.8(3) . . ? C123 C128 C127 120.5(3) . . ? C130 C129 C134 119.2(3) . . ? C130 C129 P6 118.5(2) . . ? C134 C129 P6 122.3(2) . . ? C131 C130 C129 120.6(3) . . ? C132 C131 C130 119.7(3) . . ? C133 C132 C131 120.5(3) . . ? C132 C133 C134 120.6(3) . . ? C133 C134 C129 119.5(3) . . ? C140 C135 C136 119.0(3) . . ? C140 C135 P6 118.4(2) . . ? C136 C135 P6 122.4(2) . . ? C137 C136 C135 119.4(3) . . ? C138 C137 C136 120.7(4) . . ? C137 C138 C139 120.0(3) . . ? C140 C139 C138 119.9(3) . . ? C139 C140 C135 121.0(3) . . ? C146 C141 C142 118.8(3) . . ? C146 C141 P7 118.0(2) . . ? C142 C141 P7 123.1(2) . . ? C143 C142 C141 120.2(3) . . ? C144 C143 C142 120.7(3) . . ? C145 C144 C143 119.2(4) . . ? C144 C145 C146 120.8(4) . . ? C141 C146 C145 120.3(3) . . ? C152 C147 C148 119.0(3) . . ? C152 C147 P7 118.6(2) . . ? C148 C147 P7 121.6(2) . . ? C149 C148 C147 120.2(3) . . ? C150 C149 C148 120.2(3) . . ? C151 C150 C149 119.9(3) . . ? C150 C151 C152 119.9(3) . . ? C147 C152 C151 120.8(3) . . ? C154 C153 C158 118.9(3) . . ? C154 C153 P8 118.9(3) . . ? C158 C153 P8 121.3(3) . . ? C153 C154 C155 120.7(4) . . ? C156 C155 C154 119.3(4) . . ? C157 C156 C155 120.6(4) . . ? C156 C157 C158 120.6(4) . . ? C157 C158 C153 119.8(4) . . ? C160 C159 C164 118.6(3) . . ? C160 C159 P8 117.2(2) . . ? C164 C159 P8 124.2(2) . . ? C159 C160 C161 120.6(3) . . ? C162 C161 C160 119.9(4) . . ? C161 C162 C163 120.3(4) . . ? C162 C163 C164 120.3(3) . . ? C163 C164 C159 120.3(3) . . ? F1 B1 F3 108.8(4) . . ? F1 B1 F2 109.4(4) . . ? F3 B1 F2 109.1(4) . . ? F1 B1 F4 110.9(4) . . ? F3 B1 F4 110.0(4) . . ? F2 B1 F4 108.6(4) . . ? F12 B2 F13A 31(2) . . ? F12 B2 F11 114.4(5) . . ? F13A B2 F11 120.1(14) . . ? F12 B2 F14 114.3(6) . . ? F13A B2 F14 126.8(15) . . ? F11 B2 F14 111.1(5) . . ? F12 B2 F12A 74.8(10) . . ? F13A B2 F12A 103(2) . . ? F11 B2 F12A 98.0(8) . . ? F14 B2 F12A 54.0(9) . . ? F12 B2 F13 106.1(6) . . ? F13A B2 F13 76(2) . . ? F11 B2 F13 103.3(5) . . ? F14 B2 F13 106.6(6) . . ? F12A B2 F13 155.8(10) . . ? F12 B2 F14A 120.7(7) . . ? F13A B2 F14A 101.9(17) . . ? F11 B2 F14A 123.3(7) . . ? F14 B2 F14A 56.6(6) . . ? F12A B2 F14A 107.8(11) . . ? F13 B2 F14A 50.3(6) . . ? N2 C3S C4S 178.9(6) . . ? N4 C8S N4A 110.7(19) . . ? N4 C8S C7SA 78.0(10) . . ? N4A C8S C7SA 141.9(14) . . ? N4 C8S C7S 175.0(8) . . ? N4A C8S C7S 69.4(16) . . ? C7SA C8S C7S 105.1(11) . . ? N1 C1S N1AS 29.1(13) . . ? N1 C1S C2BS 163.9(17) . . ? N1AS C1S C2BS 155(2) . . ? N1 C1S C2S 175.0(8) . . ? N1AS C1S C2S 152.2(16) . . ? C2BS C1S C2S 19.6(14) . . ? Cl2 C5S Cl1 110.7(9) . . ? Cl1B C5SB Cl2B 105.2(17) . . ? N6S C6S C6SB 150(2) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.899 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.076 #==END 4 data_mono1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.40 H46.40 B0.80 Cu0.80 F3.20 N1.60 P3.20 S6.40' _chemical_formula_weight 1147.10 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 17.788(4) _cell_length_b 20.676(4) _cell_length_c 18.183(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.83(3) _cell_angle_gamma 90.00 _cell_volume 6687(2) _cell_formula_units_Z 5 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular box _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 Smart1000 CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33921 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.69 _reflns_number_total 11346 _reflns_number_gt 6459 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11346 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.037 _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 Cu1 Cu 0.15755(3) 0.74958(2) 0.13140(2) 0.02210(13) Uani 1 1 d . . . S5 S 0.32909(6) 0.56365(5) 0.16793(5) 0.0242(3) Uani 1 1 d . . . S6 S 0.24866(6) 0.54436(5) 0.02647(5) 0.0234(3) Uani 1 1 d . . . P4 P 0.16893(6) 0.67845(5) 0.03540(6) 0.0200(3) Uani 1 1 d . . . P3 P 0.25162(6) 0.69683(5) 0.19522(5) 0.0207(3) Uani 1 1 d . . . S2 S 0.06833(7) 0.97367(5) 0.17059(6) 0.0297(3) Uani 1 1 d . . . P1 P 0.03412(6) 0.76320(5) 0.16310(6) 0.0220(3) Uani 1 1 d . . . P2 P 0.17625(6) 0.85919(5) 0.13686(6) 0.0221(3) Uani 1 1 d . . . S7 S 0.45087(7) 0.45272(5) 0.12117(6) 0.0292(3) Uani 1 1 d . . . S8 S 0.36915(7) 0.43333(5) -0.01836(6) 0.0303(3) Uani 1 1 d . . . S3 S -0.15618(7) 1.01035(5) 0.25915(6) 0.0309(3) Uani 1 1 d . . . S4 S -0.03433(7) 1.09676(5) 0.21160(6) 0.0325(3) Uani 1 1 d . . . S1 S -0.05741(7) 0.88521(5) 0.20570(6) 0.0309(3) Uani 1 1 d . . . C1 C 0.0270(2) 0.85051(17) 0.1759(2) 0.0210(10) Uani 1 1 d . . . C2 C 0.0838(2) 0.89039(18) 0.1598(2) 0.0196(10) Uani 1 1 d . . . C10 C 0.2317(2) 0.61751(17) 0.0737(2) 0.0180(9) Uani 1 1 d . . . C11 C 0.3254(2) 0.52217(17) 0.0834(2) 0.0202(10) Uani 1 1 d . . . C3 C -0.0241(2) 0.96586(18) 0.2020(2) 0.0238(10) Uani 1 1 d . . . C9 C 0.2681(2) 0.62536(17) 0.1387(2) 0.0169(9) Uani 1 1 d . . . C14 C 0.4624(2) 0.40407(18) -0.0134(2) 0.0251(11) Uani 1 1 d . . . C13 C 0.4998(3) 0.41263(17) 0.0496(2) 0.0258(11) Uani 1 1 d . . . C12 C 0.3748(2) 0.47609(18) 0.0648(2) 0.0239(10) Uani 1 1 d . . . C4 C -0.0661(2) 1.01698(18) 0.2217(2) 0.0244(10) Uani 1 1 d . . . C5 C -0.1729(3) 1.09463(19) 0.2641(2) 0.0290(11) Uani 1 1 d . . . C6 C -0.1173(3) 1.13359(19) 0.2426(2) 0.0335(12) Uani 1 1 d . . . C15 C 0.5792(2) 0.3917(2) 0.0698(2) 0.0375(12) Uani 1 1 d . . . H15A H 0.6014 0.3706 0.0284 0.056 Uiso 1 1 calc R . . H15B H 0.5778 0.3622 0.1106 0.056 Uiso 1 1 calc R . . H15C H 0.6086 0.4289 0.0831 0.056 Uiso 1 1 calc R . . C7 C -0.2481(3) 1.1133(2) 0.2933(3) 0.0486(14) Uani 1 1 d . . . H7A H -0.2524 1.1596 0.2941 0.073 Uiso 1 1 calc R . . H7B H -0.2531 1.0968 0.3424 0.073 Uiso 1 1 calc R . . H7C H -0.2870 1.0955 0.2623 0.073 Uiso 1 1 calc R . . C16 C 0.4890(3) 0.37121(19) -0.0818(2) 0.0412(13) Uani 1 1 d . . . H16A H 0.5399 0.3570 -0.0746 0.062 Uiso 1 1 calc R . . H16B H 0.4865 0.4010 -0.1222 0.062 Uiso 1 1 calc R . . H16C H 0.4575 0.3346 -0.0924 0.062 Uiso 1 1 calc R . . C8 C -0.1162(3) 1.20658(18) 0.2421(3) 0.0515(15) Uani 1 1 d . . . H8A H -0.1632 1.2227 0.2597 0.077 Uiso 1 1 calc R . . H8B H -0.1087 1.2217 0.1928 0.077 Uiso 1 1 calc R . . H8C H -0.0759 1.2218 0.2733 0.077 Uiso 1 1 calc R . . F1 F 0.14837(17) 0.51782(12) 0.82678(15) 0.0633(9) Uani 1 1 d . . . F2 F 0.09428(18) 0.60001(13) 0.76473(15) 0.0676(9) Uani 1 1 d . . . F3 F 0.13131(19) 0.51188(14) 0.70267(15) 0.0747(10) Uani 1 1 d . . . F4 F 0.03275(19) 0.50634(17) 0.77679(15) 0.0868(11) Uani 1 1 d . . . B1 B 0.1028(4) 0.5344(3) 0.7677(3) 0.0427(16) Uani 1 1 d . . . C71 C 0.3407(2) 0.74053(17) 0.1898(2) 0.0203(10) Uani 1 1 d . . . C76 C 0.3713(2) 0.75004(19) 0.1201(2) 0.0278(10) Uani 1 1 d . . . H76A H 0.3484 0.7316 0.0788 0.033 Uiso 1 1 calc R . . C91 C 0.2123(2) 0.69763(18) -0.0520(2) 0.0200(10) Uani 1 1 d . . . C21 C 0.0019(2) 0.72998(18) 0.2498(2) 0.0219(10) Uani 1 1 d . . . C31 C -0.0402(2) 0.75266(18) 0.0942(2) 0.0246(10) Uani 1 1 d . . . C81 C 0.0846(2) 0.63238(17) 0.0160(2) 0.0209(10) Uani 1 1 d . . . C72 C 0.3745(2) 0.77006(19) 0.2505(2) 0.0282(11) Uani 1 1 d . . . H72A H 0.3539 0.7648 0.2969 0.034 Uiso 1 1 calc R . . C42 C 0.1525(3) 0.93267(19) 0.0087(2) 0.0323(12) Uani 1 1 d . . . H42A H 0.1017 0.9321 0.0201 0.039 Uiso 1 1 calc R . . C26 C 0.0170(2) 0.76355(18) 0.3156(2) 0.0267(11) Uani 1 1 d . . . H26A H 0.0359 0.8055 0.3139 0.032 Uiso 1 1 calc R . . C22 C -0.0262(2) 0.66731(19) 0.2540(2) 0.0275(11) Uani 1 1 d . . . H22A H -0.0352 0.6440 0.2110 0.033 Uiso 1 1 calc R . . C61 C 0.2501(2) 0.66160(17) 0.2872(2) 0.0194(10) Uani 1 1 d . . . C41 C 0.2044(2) 0.90462(17) 0.0560(2) 0.0214(10) Uani 1 1 d . . . C96 C 0.2210(2) 0.65229(19) -0.1080(2) 0.0238(10) Uani 1 1 d . . . H96A H 0.1987 0.6118 -0.1042 0.029 Uiso 1 1 calc R . . C92 C 0.2434(2) 0.75859(18) -0.0605(2) 0.0277(11) Uani 1 1 d . . . H92A H 0.2366 0.7896 -0.0242 0.033 Uiso 1 1 calc R . . C86 C 0.0520(2) 0.59905(18) 0.0747(2) 0.0280(11) Uani 1 1 d . . . H86A H 0.0774 0.5971 0.1198 0.034 Uiso 1 1 calc R . . C82 C 0.0459(2) 0.63367(19) -0.0503(2) 0.0314(11) Uani 1 1 d . . . H82A H 0.0667 0.6553 -0.0899 0.038 Uiso 1 1 calc R . . C62 C 0.3130(3) 0.63452(18) 0.3213(2) 0.0272(11) Uani 1 1 d . . . H62A H 0.3597 0.6375 0.2991 0.033 Uiso 1 1 calc R . . C75 C 0.4360(3) 0.78708(19) 0.1127(2) 0.0326(12) Uani 1 1 d . . . H75A H 0.4568 0.7928 0.0665 0.039 Uiso 1 1 calc R . . C36 C -0.1112(3) 0.72847(19) 0.1070(2) 0.0318(11) Uani 1 1 d . . . H36A H -0.1231 0.7133 0.1535 0.038 Uiso 1 1 calc R . . C63 C 0.3067(3) 0.60301(18) 0.3884(2) 0.0312(11) Uani 1 1 d . . . H63A H 0.3488 0.5845 0.4107 0.037 Uiso 1 1 calc R . . C95 C 0.2631(2) 0.6675(2) -0.1697(2) 0.0314(11) Uani 1 1 d . . . H95A H 0.2697 0.6369 -0.2066 0.038 Uiso 1 1 calc R . . C25 C 0.0040(3) 0.7346(2) 0.3828(2) 0.0339(12) Uani 1 1 d . . . H25A H 0.0147 0.7569 0.4261 0.041 Uiso 1 1 calc R . . C24 C -0.0251(3) 0.6723(2) 0.3860(2) 0.0367(12) Uani 1 1 d . . . H24A H -0.0338 0.6530 0.4313 0.044 Uiso 1 1 calc R . . C45 C 0.3031(3) 0.9346(2) -0.0274(3) 0.0415(13) Uani 1 1 d . . . H45A H 0.3539 0.9356 -0.0391 0.050 Uiso 1 1 calc R . . C23 C -0.0411(3) 0.6391(2) 0.3217(2) 0.0351(12) Uani 1 1 d . . . H23A H -0.0619 0.5978 0.3237 0.042 Uiso 1 1 calc R . . C74 C 0.4696(3) 0.81530(19) 0.1735(3) 0.0343(12) Uani 1 1 d . . . H74A H 0.5130 0.8399 0.1685 0.041 Uiso 1 1 calc R . . C32 C -0.0240(3) 0.7749(2) 0.0232(2) 0.0351(12) Uani 1 1 d . . . H32A H 0.0239 0.7905 0.0133 0.042 Uiso 1 1 calc R . . C85 C -0.0168(3) 0.56912(19) 0.0670(2) 0.0337(12) Uani 1 1 d . . . H85A H -0.0379 0.5475 0.1066 0.040 Uiso 1 1 calc R . . C64 C 0.2383(3) 0.5993(2) 0.4217(2) 0.0364(12) Uani 1 1 d . . . H64A H 0.2345 0.5780 0.4666 0.044 Uiso 1 1 calc R . . C73 C 0.4381(3) 0.8069(2) 0.2426(2) 0.0357(12) Uani 1 1 d . . . H73A H 0.4603 0.8263 0.2836 0.043 Uiso 1 1 calc R . . C51 C 0.2321(3) 0.8916(2) 0.2131(2) 0.0362(12) Uani 1 1 d . . . C84 C -0.0544(3) 0.5715(2) -0.0002(3) 0.0410(13) Uani 1 1 d . . . H84A H -0.1010 0.5515 -0.0059 0.049 Uiso 1 1 calc R . . C46 C 0.2801(3) 0.90434(18) 0.0374(2) 0.0313(11) Uani 1 1 d . . . H46A H 0.3153 0.8841 0.0680 0.038 Uiso 1 1 calc R . . C94 C 0.2952(3) 0.7282(2) -0.1760(2) 0.0403(13) Uani 1 1 d . . . H94A H 0.3239 0.7381 -0.2168 0.048 Uiso 1 1 calc R . . C65 C 0.1749(3) 0.6265(2) 0.3901(2) 0.0406(13) Uani 1 1 d . . . H65A H 0.1288 0.6240 0.4134 0.049 Uiso 1 1 calc R . . C66 C 0.1811(3) 0.65797(19) 0.3224(2) 0.0309(11) Uani 1 1 d . . . H66A H 0.1388 0.6767 0.3006 0.037 Uiso 1 1 calc R . . C34 C -0.1484(3) 0.7501(2) -0.0179(3) 0.0463(13) Uani 1 1 d . . . H34A H -0.1849 0.7498 -0.0551 0.056 Uiso 1 1 calc R . . C43 C 0.1761(3) 0.9620(2) -0.0564(2) 0.0415(13) Uani 1 1 d . . . H43A H 0.1410 0.9810 -0.0880 0.050 Uiso 1 1 calc R . . C44 C 0.2512(3) 0.9628(2) -0.0738(3) 0.0459(15) Uani 1 1 d . . . H44A H 0.2668 0.9825 -0.1170 0.055 Uiso 1 1 calc R . . C35 C -0.1653(3) 0.7266(2) 0.0509(3) 0.0419(13) Uani 1 1 d . . . H35A H -0.2126 0.7096 0.0598 0.050 Uiso 1 1 calc R . . C56 C 0.2225(3) 0.8619(3) 0.2806(3) 0.0599(17) Uani 1 1 d . . . H56A H 0.1898 0.8271 0.2846 0.072 Uiso 1 1 calc R . . C93 C 0.2845(3) 0.7740(2) -0.1220(2) 0.0395(13) Uani 1 1 d . . . H93A H 0.3050 0.8152 -0.1270 0.047 Uiso 1 1 calc R . . C83 C -0.0226(3) 0.6038(2) -0.0590(3) 0.0440(13) Uani 1 1 d . . . H83A H -0.0476 0.6052 -0.1043 0.053 Uiso 1 1 calc R . . C33 C -0.0777(3) 0.7741(2) -0.0319(3) 0.0459(14) Uani 1 1 d . . . H33A H -0.0664 0.7896 -0.0785 0.055 Uiso 1 1 calc R . . C52 C 0.2797(3) 0.9442(2) 0.2080(3) 0.0550(16) Uani 1 1 d . . . H52A H 0.2847 0.9652 0.1632 0.066 Uiso 1 1 calc R . . C54 C 0.3108(5) 0.9365(4) 0.3335(5) 0.119(5) Uani 1 1 d . . . H54A H 0.3384 0.9518 0.3737 0.143 Uiso 1 1 calc R . . C55 C 0.2628(5) 0.8847(4) 0.3443(4) 0.098(3) Uani 1 1 d . . . H55A H 0.2571 0.8657 0.3902 0.118 Uiso 1 1 calc R . . C53 C 0.3199(4) 0.9658(4) 0.2689(4) 0.100(3) Uani 1 1 d . . . H53A H 0.3529 1.0005 0.2649 0.120 Uiso 1 1 calc R . . C1S C -0.0424(3) 0.5208(2) 0.6191(3) 0.0525(15) Uani 1 1 d . . . H1S1 H -0.0688 0.5548 0.6438 0.079 Uiso 1 1 calc R . . H1S2 H -0.0168 0.4943 0.6548 0.079 Uiso 1 1 calc R . . H1S3 H -0.0777 0.4948 0.5917 0.079 Uiso 1 1 calc R . . C2S C 0.0119(3) 0.5487(2) 0.5694(3) 0.0503(15) Uani 1 1 d . . . N1S N 0.0531(3) 0.5717(2) 0.5308(3) 0.0759(17) Uani 1 1 d . . . C3S C 0.2042(4) 0.6483(2) 0.6213(3) 0.089(3) Uani 1 1 d . . . H3S1 H 0.2569 0.6533 0.6120 0.134 Uiso 1 1 calc R . . H3S2 H 0.1882 0.6059 0.6063 0.134 Uiso 1 1 calc R . . H3S3 H 0.1954 0.6537 0.6729 0.134 Uiso 1 1 calc R . . C4S C 0.1608(4) 0.6980(3) 0.5790(3) 0.061(2) Uani 1 1 d . . . N2S N 0.1327(3) 0.7359(3) 0.5485(3) 0.0773(18) 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 Cu1 0.0220(3) 0.0244(3) 0.0200(3) 0.0004(2) 0.0033(2) 0.0051(3) S5 0.0263(7) 0.0260(6) 0.0201(6) -0.0018(5) -0.0009(5) 0.0076(5) S6 0.0242(7) 0.0235(6) 0.0224(6) -0.0030(5) -0.0013(5) 0.0053(5) P4 0.0183(7) 0.0243(6) 0.0174(6) 0.0005(5) -0.0001(5) 0.0029(5) P3 0.0218(7) 0.0235(6) 0.0169(6) -0.0013(5) 0.0017(5) 0.0035(5) S2 0.0257(7) 0.0216(6) 0.0419(7) -0.0002(5) 0.0096(6) 0.0024(5) P1 0.0223(7) 0.0220(6) 0.0218(6) 0.0012(5) 0.0029(5) 0.0036(5) P2 0.0203(7) 0.0260(6) 0.0198(6) -0.0007(5) 0.0009(5) 0.0037(5) S7 0.0271(7) 0.0341(6) 0.0264(6) 0.0009(5) 0.0000(5) 0.0100(6) S8 0.0320(8) 0.0311(6) 0.0277(6) -0.0069(5) -0.0006(6) 0.0087(6) S3 0.0289(8) 0.0264(6) 0.0378(7) -0.0009(5) 0.0095(6) 0.0057(6) S4 0.0262(7) 0.0243(6) 0.0471(8) -0.0038(5) 0.0035(6) 0.0019(6) S1 0.0238(7) 0.0227(6) 0.0466(7) 0.0018(5) 0.0137(6) 0.0050(5) C1 0.020(3) 0.023(2) 0.020(2) 0.0019(18) 0.004(2) 0.007(2) C2 0.020(3) 0.023(2) 0.016(2) 0.0032(18) 0.0038(19) 0.005(2) C10 0.011(2) 0.020(2) 0.023(2) 0.0006(18) 0.0036(19) 0.0025(19) C11 0.022(3) 0.019(2) 0.019(2) 0.0005(18) 0.003(2) -0.001(2) C3 0.025(3) 0.024(2) 0.023(2) 0.0008(19) 0.003(2) 0.002(2) C9 0.015(2) 0.017(2) 0.018(2) 0.0036(17) 0.0050(19) 0.0026(19) C14 0.026(3) 0.020(2) 0.030(3) 0.0004(19) 0.008(2) 0.003(2) C13 0.030(3) 0.015(2) 0.033(3) 0.0033(19) 0.009(2) 0.002(2) C12 0.024(3) 0.026(2) 0.022(2) 0.0020(18) -0.001(2) 0.003(2) C4 0.023(3) 0.028(2) 0.022(2) 0.0009(19) 0.002(2) 0.006(2) C5 0.025(3) 0.028(2) 0.035(3) -0.006(2) -0.001(2) 0.012(2) C6 0.033(3) 0.025(2) 0.042(3) -0.009(2) -0.006(2) 0.008(2) C15 0.024(3) 0.037(3) 0.052(3) 0.006(2) 0.005(2) 0.007(2) C7 0.037(3) 0.038(3) 0.071(4) -0.017(3) 0.013(3) 0.004(3) C16 0.039(3) 0.036(3) 0.049(3) -0.015(2) 0.014(3) 0.004(3) C8 0.036(3) 0.025(3) 0.094(4) -0.013(3) -0.003(3) 0.005(3) F1 0.070(2) 0.0501(18) 0.069(2) 0.0037(15) -0.0233(18) 0.0098(17) F2 0.092(3) 0.0535(19) 0.056(2) 0.0035(15) -0.0144(18) 0.0260(19) F3 0.091(3) 0.077(2) 0.057(2) -0.0120(17) 0.030(2) -0.003(2) F4 0.071(3) 0.144(3) 0.046(2) 0.0091(19) -0.0035(18) -0.049(2) B1 0.051(5) 0.050(4) 0.028(3) 0.000(3) 0.004(3) -0.002(4) C71 0.019(2) 0.020(2) 0.022(2) -0.0009(18) 0.000(2) 0.005(2) C76 0.026(3) 0.028(2) 0.030(3) -0.002(2) 0.003(2) 0.000(2) C91 0.022(3) 0.023(2) 0.015(2) 0.0023(18) -0.0016(19) 0.003(2) C21 0.018(3) 0.025(2) 0.023(2) 0.0023(18) 0.003(2) 0.006(2) C31 0.026(3) 0.021(2) 0.027(2) 0.0005(19) 0.004(2) 0.007(2) C81 0.021(3) 0.020(2) 0.022(2) 0.0017(18) 0.005(2) 0.007(2) C72 0.026(3) 0.034(3) 0.024(2) -0.003(2) 0.000(2) 0.002(2) C42 0.035(3) 0.039(3) 0.022(3) 0.001(2) 0.005(2) 0.001(2) C26 0.027(3) 0.024(2) 0.029(3) 0.000(2) 0.001(2) 0.004(2) C22 0.027(3) 0.029(2) 0.027(3) -0.002(2) 0.008(2) 0.001(2) C61 0.020(3) 0.022(2) 0.016(2) -0.0023(17) 0.001(2) 0.005(2) C41 0.024(3) 0.019(2) 0.021(2) -0.0049(18) 0.004(2) -0.004(2) C96 0.024(3) 0.028(2) 0.019(2) 0.0056(19) -0.004(2) 0.002(2) C92 0.034(3) 0.027(2) 0.023(2) -0.0028(19) 0.001(2) -0.003(2) C86 0.030(3) 0.028(2) 0.026(3) 0.000(2) 0.002(2) 0.003(2) C82 0.024(3) 0.038(3) 0.033(3) 0.008(2) -0.002(2) -0.007(2) C62 0.031(3) 0.032(2) 0.019(2) -0.005(2) 0.002(2) 0.005(2) C75 0.032(3) 0.033(3) 0.033(3) 0.003(2) 0.008(2) 0.001(2) C36 0.030(3) 0.038(3) 0.028(3) 0.004(2) 0.001(2) 0.004(2) C63 0.045(3) 0.028(2) 0.021(2) 0.000(2) -0.002(2) 0.009(2) C95 0.034(3) 0.044(3) 0.017(2) -0.003(2) 0.003(2) 0.013(3) C25 0.039(3) 0.041(3) 0.021(3) -0.004(2) 0.006(2) 0.008(3) C24 0.042(3) 0.039(3) 0.030(3) 0.011(2) 0.011(2) 0.006(3) C45 0.041(4) 0.034(3) 0.050(3) -0.010(2) 0.025(3) -0.008(3) C23 0.034(3) 0.032(3) 0.040(3) 0.009(2) 0.010(2) 0.002(2) C74 0.025(3) 0.024(2) 0.054(3) -0.002(2) 0.005(3) -0.001(2) C32 0.034(3) 0.042(3) 0.029(3) 0.004(2) 0.001(2) 0.006(2) C85 0.035(3) 0.031(3) 0.035(3) 0.001(2) 0.012(3) -0.003(2) C64 0.055(4) 0.036(3) 0.019(3) 0.007(2) 0.002(3) 0.001(3) C73 0.033(3) 0.034(3) 0.039(3) -0.014(2) -0.009(2) 0.003(2) C51 0.033(3) 0.048(3) 0.028(3) -0.013(2) -0.006(2) 0.027(3) C84 0.029(3) 0.042(3) 0.052(3) -0.003(3) -0.001(3) -0.016(3) C46 0.032(3) 0.024(2) 0.038(3) -0.001(2) 0.007(2) 0.002(2) C94 0.029(3) 0.058(3) 0.034(3) 0.013(3) 0.008(2) -0.002(3) C65 0.041(3) 0.048(3) 0.034(3) 0.010(2) 0.010(3) 0.001(3) C66 0.029(3) 0.037(3) 0.026(3) 0.005(2) 0.001(2) 0.006(2) C34 0.050(4) 0.044(3) 0.045(3) -0.004(3) -0.018(3) 0.010(3) C43 0.052(4) 0.054(3) 0.018(3) 0.007(2) -0.004(3) -0.001(3) C44 0.066(4) 0.040(3) 0.033(3) -0.003(2) 0.020(3) -0.012(3) C35 0.028(3) 0.040(3) 0.057(4) -0.004(3) -0.008(3) 0.002(3) C56 0.068(4) 0.079(4) 0.033(3) -0.016(3) -0.011(3) 0.051(3) C93 0.041(3) 0.036(3) 0.041(3) 0.002(2) 0.009(3) -0.017(3) C83 0.032(3) 0.061(3) 0.039(3) 0.009(3) -0.017(3) -0.015(3) C33 0.052(4) 0.059(3) 0.026(3) 0.008(2) -0.007(3) 0.006(3) C52 0.031(3) 0.065(4) 0.068(4) -0.045(3) -0.015(3) 0.007(3) C54 0.112(8) 0.166(9) 0.079(6) -0.082(7) -0.058(6) 0.118(7) C55 0.128(8) 0.124(7) 0.043(4) -0.016(5) -0.011(5) 0.108(6) C53 0.041(4) 0.128(7) 0.129(7) -0.091(6) -0.042(5) 0.031(4) C1S 0.054(4) 0.046(3) 0.058(4) 0.000(3) -0.005(3) 0.007(3) C2S 0.067(5) 0.041(3) 0.042(4) 0.000(3) -0.002(3) -0.004(3) N1S 0.107(5) 0.068(3) 0.053(3) -0.008(3) 0.008(3) -0.026(3) C3S 0.191(8) 0.047(3) 0.029(3) 0.010(3) 0.005(4) -0.021(4) C4S 0.047(5) 0.090(6) 0.047(4) -0.017(4) 0.019(3) -0.026(4) N2S 0.055(4) 0.078(4) 0.099(5) -0.015(3) 0.014(3) 0.002(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 Cu1 P2 2.2923(12) . ? Cu1 P4 2.2938(11) . ? Cu1 P1 2.2953(13) . ? Cu1 P3 2.2978(13) . ? S5 C9 1.752(4) . ? S5 C11 1.761(4) . ? S6 C11 1.762(4) . ? S6 C10 1.768(4) . ? P4 C81 1.808(4) . ? P4 C10 1.815(4) . ? P4 C91 1.820(4) . ? P3 C61 1.825(4) . ? P3 C9 1.826(4) . ? P3 C71 1.828(4) . ? S2 C2 1.755(4) . ? S2 C3 1.756(4) . ? P1 C21 1.819(4) . ? P1 C31 1.821(4) . ? P1 C1 1.825(4) . ? P2 C2 1.820(4) . ? P2 C41 1.821(4) . ? P2 C51 1.822(5) . ? S7 C12 1.754(4) . ? S7 C13 1.780(4) . ? S8 C12 1.753(4) . ? S8 C14 1.767(4) . ? S3 C4 1.755(4) . ? S3 C5 1.770(4) . ? S4 C4 1.754(4) . ? S4 C6 1.761(4) . ? S1 C1 1.757(4) . ? S1 C3 1.771(4) . ? C1 C2 1.340(5) . ? C10 C9 1.350(5) . ? C11 C12 1.343(5) . ? C3 C4 1.346(5) . ? C14 C13 1.328(5) . ? C14 C16 1.500(5) . ? C13 C15 1.517(6) . ? C5 C6 1.338(6) . ? C5 C7 1.498(6) . ? C6 C8 1.509(5) . ? F1 B1 1.380(6) . ? F2 B1 1.366(6) . ? F3 B1 1.375(6) . ? F4 B1 1.386(7) . ? C71 C72 1.390(5) . ? C71 C76 1.401(5) . ? C76 C75 1.391(5) . ? C91 C92 1.387(5) . ? C91 C96 1.395(5) . ? C21 C22 1.392(5) . ? C21 C26 1.406(5) . ? C31 C36 1.383(6) . ? C31 C32 1.405(5) . ? C81 C82 1.379(5) . ? C81 C86 1.402(5) . ? C72 C73 1.372(6) . ? C42 C41 1.381(6) . ? C42 C43 1.400(5) . ? C26 C25 1.385(5) . ? C22 C23 1.392(5) . ? C61 C62 1.390(5) . ? C61 C66 1.394(5) . ? C41 C46 1.392(6) . ? C96 C95 1.393(5) . ? C92 C93 1.383(5) . ? C86 C85 1.377(6) . ? C82 C83 1.373(6) . ? C62 C63 1.389(5) . ? C75 C74 1.378(6) . ? C36 C35 1.391(6) . ? C63 C64 1.369(6) . ? C95 C94 1.384(5) . ? C25 C24 1.390(5) . ? C24 C23 1.383(6) . ? C45 C44 1.371(6) . ? C45 C46 1.401(5) . ? C74 C73 1.393(5) . ? C32 C33 1.374(6) . ? C85 C84 1.385(6) . ? C64 C65 1.378(6) . ? C51 C52 1.381(6) . ? C51 C56 1.385(6) . ? C84 C83 1.389(6) . ? C94 C93 1.380(5) . ? C65 C66 1.398(5) . ? C34 C33 1.378(6) . ? C34 C35 1.380(6) . ? C43 C44 1.378(6) . ? C56 C55 1.431(8) . ? C52 C53 1.384(7) . ? C54 C53 1.332(10) . ? C54 C55 1.386(10) . ? C1S C2S 1.453(7) . ? C2S N1S 1.127(6) . ? C3S C4S 1.491(8) . ? C4S N2S 1.079(7) . ? 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 P2 Cu1 P4 130.73(4) . . ? P2 Cu1 P1 90.38(4) . . ? P4 Cu1 P1 111.41(5) . . ? P2 Cu1 P3 110.07(4) . . ? P4 Cu1 P3 90.47(4) . . ? P1 Cu1 P3 128.58(4) . . ? C9 S5 C11 94.29(18) . . ? C11 S6 C10 94.24(18) . . ? C81 P4 C10 102.29(17) . . ? C81 P4 C91 107.82(18) . . ? C10 P4 C91 102.74(18) . . ? C81 P4 Cu1 113.82(13) . . ? C10 P4 Cu1 102.33(13) . . ? C91 P4 Cu1 124.59(13) . . ? C61 P3 C9 101.38(16) . . ? C61 P3 C71 105.73(18) . . ? C9 P3 C71 102.89(17) . . ? C61 P3 Cu1 129.18(14) . . ? C9 P3 Cu1 102.82(13) . . ? C71 P3 Cu1 111.33(12) . . ? C2 S2 C3 95.50(19) . . ? C21 P1 C31 108.44(19) . . ? C21 P1 C1 103.86(17) . . ? C31 P1 C1 98.93(18) . . ? C21 P1 Cu1 119.06(14) . . ? C31 P1 Cu1 119.98(13) . . ? C1 P1 Cu1 102.81(14) . . ? C2 P2 C41 105.19(18) . . ? C2 P2 C51 100.35(18) . . ? C41 P2 C51 105.7(2) . . ? C2 P2 Cu1 103.26(13) . . ? C41 P2 Cu1 121.10(12) . . ? C51 P2 Cu1 118.29(15) . . ? C12 S7 C13 94.7(2) . . ? C12 S8 C14 94.9(2) . . ? C4 S3 C5 95.6(2) . . ? C4 S4 C6 95.7(2) . . ? C1 S1 C3 94.88(19) . . ? C2 C1 S1 117.8(3) . . ? C2 C1 P1 121.8(3) . . ? S1 C1 P1 120.3(2) . . ? C1 C2 S2 117.3(3) . . ? C1 C2 P2 121.2(3) . . ? S2 C2 P2 121.2(2) . . ? C9 C10 S6 116.4(3) . . ? C9 C10 P4 122.5(3) . . ? S6 C10 P4 121.1(2) . . ? C12 C11 S5 123.3(3) . . ? C12 C11 S6 122.8(3) . . ? S5 C11 S6 113.9(2) . . ? C4 C3 S2 122.7(3) . . ? C4 C3 S1 122.8(3) . . ? S2 C3 S1 114.5(2) . . ? C10 C9 S5 117.8(3) . . ? C10 C9 P3 120.7(3) . . ? S5 C9 P3 121.5(2) . . ? C13 C14 C16 128.0(4) . . ? C13 C14 S8 117.2(3) . . ? C16 C14 S8 114.8(3) . . ? C14 C13 C15 128.5(4) . . ? C14 C13 S7 116.7(3) . . ? C15 C13 S7 114.8(3) . . ? C11 C12 S8 123.1(3) . . ? C11 C12 S7 123.4(3) . . ? S8 C12 S7 113.5(2) . . ? C3 C4 S4 122.0(3) . . ? C3 C4 S3 123.7(3) . . ? S4 C4 S3 114.3(2) . . ? C6 C5 C7 128.1(4) . . ? C6 C5 S3 116.9(3) . . ? C7 C5 S3 115.0(3) . . ? C5 C6 C8 127.9(4) . . ? C5 C6 S4 117.4(3) . . ? C8 C6 S4 114.8(3) . . ? F2 B1 F3 110.1(4) . . ? F2 B1 F1 109.9(5) . . ? F3 B1 F1 111.4(5) . . ? F2 B1 F4 108.7(5) . . ? F3 B1 F4 107.7(5) . . ? F1 B1 F4 108.8(4) . . ? C72 C71 C76 119.1(4) . . ? C72 C71 P3 122.7(3) . . ? C76 C71 P3 117.8(3) . . ? C75 C76 C71 119.9(4) . . ? C92 C91 C96 118.7(4) . . ? C92 C91 P4 118.1(3) . . ? C96 C91 P4 123.0(3) . . ? C22 C21 C26 118.6(4) . . ? C22 C21 P1 121.1(3) . . ? C26 C21 P1 119.5(3) . . ? C36 C31 C32 118.2(4) . . ? C36 C31 P1 125.7(3) . . ? C32 C31 P1 115.9(3) . . ? C82 C81 C86 117.9(4) . . ? C82 C81 P4 124.2(3) . . ? C86 C81 P4 117.5(3) . . ? C73 C72 C71 120.5(4) . . ? C41 C42 C43 120.2(4) . . ? C25 C26 C21 120.4(4) . . ? C23 C22 C21 120.8(4) . . ? C62 C61 C66 118.8(4) . . ? C62 C61 P3 123.2(3) . . ? C66 C61 P3 117.9(3) . . ? C42 C41 C46 119.4(4) . . ? C42 C41 P2 122.0(3) . . ? C46 C41 P2 118.2(3) . . ? C95 C96 C91 120.3(4) . . ? C93 C92 C91 121.1(4) . . ? C85 C86 C81 121.3(4) . . ? C83 C82 C81 121.5(4) . . ? C61 C62 C63 120.4(4) . . ? C74 C75 C76 120.3(4) . . ? C31 C36 C35 120.7(4) . . ? C64 C63 C62 119.9(4) . . ? C94 C95 C96 119.8(4) . . ? C26 C25 C24 120.4(4) . . ? C23 C24 C25 119.8(4) . . ? C44 C45 C46 120.3(5) . . ? C24 C23 C22 120.1(4) . . ? C75 C74 C73 119.7(4) . . ? C33 C32 C31 121.1(5) . . ? C86 C85 C84 119.4(4) . . ? C63 C64 C65 121.3(4) . . ? C72 C73 C74 120.4(4) . . ? C52 C51 C56 119.4(5) . . ? C52 C51 P2 124.5(4) . . ? C56 C51 P2 116.0(4) . . ? C85 C84 C83 119.9(4) . . ? C41 C46 C45 119.9(4) . . ? C93 C94 C95 120.2(4) . . ? C64 C65 C66 118.9(4) . . ? C61 C66 C65 120.7(4) . . ? C33 C34 C35 120.4(5) . . ? C44 C43 C42 120.2(5) . . ? C45 C44 C43 120.0(4) . . ? C34 C35 C36 119.8(5) . . ? C51 C56 C55 120.3(6) . . ? C94 C93 C92 119.8(4) . . ? C82 C83 C84 119.9(4) . . ? C32 C33 C34 119.7(4) . . ? C51 C52 C53 120.7(6) . . ? C53 C54 C55 124.0(9) . . ? C54 C55 C56 116.2(8) . . ? C54 C53 C52 119.4(8) . . ? N1S C2S C1S 178.3(6) . . ? N2S C4S C3S 176.2(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.868 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.077 #==END