Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Paul Sharp' _publ_contact_author_address ;125 Chemistry University of Missouri Columbia, MO 65211 USA ; _publ_contact_author_email sharpp@missouri.edu _publ_contact_author_phone 572-882-7715 _publ_contact_author_fax 573-882-2754 loop_ _publ_author_name _publ_author_address A.Singh ;125 Chemistry University of Missouri Columbia, MO 65211 USA ; U.Anandhi ;125 Chemistry University of Missouri Columbia, MO 65211 USA ; M.A.Cinellu ;Dipartinmento di Chimica Universita di Sassari Via Vienna 2 I-07100, Sassari Italy ; P.R.Sharp ;125 Chemistry University of Missouri Columbia, MO 65211 USA ; _publ_section_title ;Diimine Supported Group 10 Hydroxo, Oxo, Amido, and Imido Complexes ; data_Pt2(Bian)2O2AuLBF4_(5) _database_code_depnum_ccdc_archive 'CCDC 663517' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H95 Au N4 O2 P Pt2 1+, B F4 1-, 0.5(C H2 Cl2), 3(C7 H8), 0.5(C7)' _chemical_formula_sum 'C115 H120 Au B Cl F4 N4 O2 P Pt2' _chemical_formula_weight 2330.56 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8799(14) _cell_length_b 31.125(3) _cell_length_c 25.166(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.968(2) _cell_angle_gamma 90.00 _cell_volume 10503.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6573 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.05 _exptl_crystal_description NEEDLE _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 _exptl_absorpt_coefficient_mu 4.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2552 _exptl_absorpt_correction_T_max 0.5732 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 65823 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1203 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.15 _reflns_number_total 23218 _reflns_number_gt 12928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the 4 toluene sites is located on an inversion center. The ring carbon atoms were identified but the Me group could not be located and was omitted as were the ring hydrogen atoms. ; _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^)+(0.0555P)^2^+1.7780P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23218 _refine_ls_number_parameters 1165 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.18986(2) 0.873870(10) 0.672273(14) 0.02739(9) Uani 1 1 d . . . Pt1 Pt 0.07914(2) 0.823918(10) 0.570567(13) 0.02425(9) Uani 1 1 d . . . P1 P 0.16181(17) 0.91867(7) 0.73514(10) 0.0294(5) Uani 1 1 d . . . F1 F -0.3810(7) 1.0825(4) 0.7711(4) 0.155(4) Uani 1 1 d . . . O1 O 0.2217(4) 0.83541(16) 0.6127(2) 0.0262(13) Uani 1 1 d . . . N1 N 0.0580(5) 0.8646(2) 0.5062(3) 0.0281(16) Uani 1 1 d . . . C73 C 0.0445(6) 0.9478(3) 0.7113(3) 0.028(2) Uani 1 1 d . . . B1 B -0.3766(13) 1.0697(6) 0.7210(8) 0.084(5) Uani 1 1 d . . . Pt2 Pt 0.24118(2) 0.776804(10) 0.648645(14) 0.02403(9) Uani 1 1 d . . . F2 F -0.3944(7) 1.1097(3) 0.6881(5) 0.155(4) Uani 1 1 d . . . O2 O 0.0943(4) 0.77996(17) 0.6279(2) 0.0304(14) Uani 1 1 d . . . N2 N -0.0675(5) 0.8180(2) 0.5388(3) 0.0326(17) Uani 1 1 d . . . C74 C -0.0098(7) 0.9629(3) 0.7464(4) 0.040(2) Uani 1 1 d . . . H2 H 0.0115 0.9563 0.7845 0.048 Uiso 1 1 calc R . . F3 F -0.4514(5) 1.0446(2) 0.6963(3) 0.101(3) Uani 1 1 d . . . N3 N 0.3906(5) 0.7767(2) 0.6753(3) 0.0258(15) Uani 1 1 d . . . C75 C -0.0949(7) 0.9873(3) 0.7268(4) 0.047(3) Uani 1 1 d . . . H3 H -0.1306 0.9976 0.7517 0.056 Uiso 1 1 calc R . . F4 F -0.2874(5) 1.0595(3) 0.7177(4) 0.113(3) Uani 1 1 d . . . N4 N 0.2639(5) 0.71583(19) 0.6748(3) 0.0285(17) Uani 1 1 d . . . C76 C -0.1286(7) 0.9970(3) 0.6716(5) 0.053(3) Uani 1 1 d . . . H4 H -0.1863 1.0143 0.6586 0.063 Uiso 1 1 calc R . . C77 C -0.0770(9) 0.9810(3) 0.6353(5) 0.065(3) Uani 1 1 d . . . H5 H -0.1006 0.9861 0.5969 0.078 Uiso 1 1 calc R . . C78 C 0.0108(8) 0.9572(3) 0.6564(4) 0.051(3) Uani 1 1 d . . . H6 H 0.0479 0.9474 0.6319 0.062 Uiso 1 1 calc R . . C79 C 0.1574(6) 0.8929(3) 0.7993(3) 0.029(2) Uani 1 1 d . . . C80 C 0.1808(8) 0.9144(3) 0.8498(4) 0.048(3) Uani 1 1 d . . . H12 H 0.2015 0.9436 0.8517 0.058 Uiso 1 1 calc R . . C81 C 0.1737(9) 0.8934(3) 0.8963(4) 0.058(3) Uani 1 1 d . . . H13 H 0.1888 0.9084 0.9303 0.070 Uiso 1 1 calc R . . C82 C 0.1453(8) 0.8512(3) 0.8949(4) 0.055(3) Uani 1 1 d . . . H14 H 0.1406 0.8369 0.9275 0.065 Uiso 1 1 calc R . . C83 C 0.1237(8) 0.8301(3) 0.8456(4) 0.056(3) Uani 1 1 d . . . H15 H 0.1040 0.8008 0.8444 0.067 Uiso 1 1 calc R . . C84 C 0.1294(7) 0.8497(3) 0.7980(4) 0.041(2) Uani 1 1 d . . . H16 H 0.1146 0.8342 0.7643 0.050 Uiso 1 1 calc R . . C85 C 0.2556(6) 0.9606(3) 0.7526(3) 0.027(2) Uani 1 1 d . . . C86 C 0.2393(7) 0.9990(3) 0.7789(4) 0.035(2) Uani 1 1 d . . . H22 H 0.1772 1.0039 0.7872 0.042 Uiso 1 1 calc R . . C87 C 0.3146(7) 1.0297(3) 0.7926(4) 0.043(3) Uani 1 1 d . . . H23 H 0.3042 1.0556 0.8104 0.052 Uiso 1 1 calc R . . C88 C 0.4062(7) 1.0223(3) 0.7800(4) 0.039(2) Uani 1 1 d . . . H24 H 0.4577 1.0432 0.7894 0.047 Uiso 1 1 calc R . . C89 C 0.4212(7) 0.9853(3) 0.7545(4) 0.044(3) Uani 1 1 d . . . H25 H 0.4830 0.9808 0.7457 0.053 Uiso 1 1 calc R . . C90 C 0.3476(7) 0.9544(3) 0.7412(4) 0.041(2) Uani 1 1 d . . . H26 H 0.3599 0.9285 0.7240 0.049 Uiso 1 1 calc R . . C1 C -0.0356(7) 0.8710(3) 0.4817(4) 0.034(2) Uani 1 1 d . . . C2 C -0.1075(6) 0.8465(3) 0.5016(4) 0.034(2) Uani 1 1 d . . . C3 C -0.3034(8) 0.8465(4) 0.4698(5) 0.065(3) Uani 1 1 d . . . H3A H -0.3153 0.8268 0.4962 0.079 Uiso 1 1 calc R . . C4 C -0.3828(9) 0.8653(5) 0.4298(5) 0.085(5) Uani 1 1 d . . . H4A H -0.4492 0.8576 0.4295 0.102 Uiso 1 1 calc R . . C5 C -0.3687(9) 0.8939(5) 0.3915(5) 0.087(5) Uani 1 1 d . . . H5A H -0.4247 0.9068 0.3668 0.104 Uiso 1 1 calc R . . C6 C -0.2411(12) 0.9327(4) 0.3516(5) 0.077(5) Uani 1 1 d . . . H6A H -0.2908 0.9474 0.3247 0.093 Uiso 1 1 calc R . . C7 C -0.1462(11) 0.9396(4) 0.3530(5) 0.069(4) Uani 1 1 d . . . H7A H -0.1310 0.9570 0.3252 0.083 Uiso 1 1 calc R . . C8 C -0.0667(9) 0.9219(3) 0.3943(4) 0.055(3) Uani 1 1 d . . . H8A H 0.0009 0.9283 0.3957 0.067 Uiso 1 1 calc R . . C9 C -0.0916(8) 0.8949(3) 0.4327(4) 0.047(3) Uani 1 1 d . . . C10 C -0.2078(7) 0.8580(3) 0.4689(4) 0.042(2) Uani 1 1 d . . . C11 C -0.2725(9) 0.9043(3) 0.3884(4) 0.057(3) Uani 1 1 d . . . C12 C -0.1920(8) 0.8866(3) 0.4298(4) 0.046(3) Uani 1 1 d . . . C13 C 0.1323(7) 0.8784(3) 0.4779(3) 0.030(2) Uani 1 1 d . . . C14 C 0.1422(7) 0.8536(3) 0.4334(4) 0.040(2) Uani 1 1 d . . . C15 C 0.2072(8) 0.8683(3) 0.4040(4) 0.050(3) Uani 1 1 d . . . H15A H 0.2135 0.8525 0.3728 0.060 Uiso 1 1 calc R . . C16 C 0.2632(7) 0.9053(3) 0.4184(4) 0.044(3) Uani 1 1 d . . . H16A H 0.3069 0.9146 0.3972 0.053 Uiso 1 1 calc R . . C17 C 0.2554(7) 0.9281(3) 0.4629(4) 0.038(2) Uani 1 1 d . . . H17A H 0.2951 0.9531 0.4731 0.046 Uiso 1 1 calc R . . C18 C 0.1895(7) 0.9155(3) 0.4947(4) 0.036(2) Uani 1 1 d . . . C19 C 0.0884(8) 0.8107(3) 0.4190(4) 0.045(3) Uani 1 1 d . . . H19A H 0.0346 0.8097 0.4388 0.055 Uiso 1 1 calc R . . C22 C 0.1814(7) 0.9421(3) 0.5437(4) 0.038(2) Uani 1 1 d . . . H20A H 0.1375 0.9260 0.5626 0.046 Uiso 1 1 calc R . . C20 C 0.0387(9) 0.8053(3) 0.3586(4) 0.067(3) Uani 1 1 d . . . H21A H 0.0897 0.8037 0.3380 0.100 Uiso 1 1 calc R . . H21B H -0.0052 0.8299 0.3456 0.100 Uiso 1 1 calc R . . H21C H -0.0008 0.7788 0.3530 0.100 Uiso 1 1 calc R . . C21 C 0.1592(10) 0.7740(3) 0.4409(5) 0.088(4) Uani 1 1 d . . . H22A H 0.1215 0.7471 0.4382 0.131 Uiso 1 1 calc R . . H22B H 0.1938 0.7795 0.4794 0.131 Uiso 1 1 calc R . . H22C H 0.2082 0.7716 0.4191 0.131 Uiso 1 1 calc R . . C23 C 0.1328(10) 0.9841(3) 0.5261(5) 0.084(4) Uani 1 1 d . . . H23A H 0.1816 1.0040 0.5176 0.126 Uiso 1 1 calc R . . H23B H 0.1073 0.9961 0.5558 0.126 Uiso 1 1 calc R . . H23C H 0.0775 0.9800 0.4933 0.126 Uiso 1 1 calc R . . C24 C 0.2823(8) 0.9482(3) 0.5855(4) 0.056(3) Uani 1 1 d . . . H24A H 0.3273 0.9641 0.5684 0.084 Uiso 1 1 calc R . . H24B H 0.3113 0.9201 0.5978 0.084 Uiso 1 1 calc R . . H24C H 0.2730 0.9644 0.6172 0.084 Uiso 1 1 calc R . . C25 C -0.1301(6) 0.7877(3) 0.5590(4) 0.039(2) Uani 1 1 d . . . C26 C -0.1433(7) 0.7462(3) 0.5349(4) 0.043(2) Uani 1 1 d . . . C27 C -0.2021(8) 0.7176(4) 0.5556(5) 0.064(3) Uani 1 1 d . . . H27A H -0.2127 0.6892 0.5414 0.077 Uiso 1 1 calc R . . C28 C -0.2447(9) 0.7308(4) 0.5966(6) 0.080(4) Uani 1 1 d . . . H28A H -0.2870 0.7114 0.6090 0.096 Uiso 1 1 calc R . . C29 C -0.2283(7) 0.7713(4) 0.6206(5) 0.057(3) Uani 1 1 d . . . H29A H -0.2586 0.7790 0.6491 0.068 Uiso 1 1 calc R . . C30 C -0.1679(7) 0.8004(3) 0.6031(4) 0.044(3) Uani 1 1 d . . . C31 C -0.0924(7) 0.7334(3) 0.4914(4) 0.047(3) Uani 1 1 d . . . H31A H -0.0275 0.7491 0.4983 0.056 Uiso 1 1 calc R . . C34 C -0.1444(7) 0.8434(3) 0.6312(4) 0.051(3) Uani 1 1 d . . . H32A H -0.1017 0.8592 0.6112 0.061 Uiso 1 1 calc R . . C32 C -0.1588(9) 0.7473(4) 0.4336(4) 0.068(3) Uani 1 1 d . . . H33A H -0.2256 0.7348 0.4280 0.101 Uiso 1 1 calc R . . H33B H -0.1286 0.7370 0.4049 0.101 Uiso 1 1 calc R . . H33C H -0.1639 0.7787 0.4320 0.101 Uiso 1 1 calc R . . C33 C -0.0714(9) 0.6851(3) 0.4911(5) 0.072(4) Uani 1 1 d . . . H34A H -0.0283 0.6765 0.5268 0.108 Uiso 1 1 calc R . . H34B H -0.0379 0.6786 0.4621 0.108 Uiso 1 1 calc R . . H34C H -0.1344 0.6692 0.4840 0.108 Uiso 1 1 calc R . . C35 C -0.2378(10) 0.8717(4) 0.6272(6) 0.110(6) Uani 1 1 d . . . H35A H -0.2829 0.8690 0.5904 0.164 Uiso 1 1 calc R . . H35B H -0.2174 0.9018 0.6341 0.164 Uiso 1 1 calc R . . H35C H -0.2721 0.8622 0.6547 0.164 Uiso 1 1 calc R . . C36 C -0.0836(12) 0.8385(4) 0.6892(5) 0.109(5) Uani 1 1 d . . . H36A H -0.1213 0.8218 0.7101 0.163 Uiso 1 1 calc R . . H36B H -0.0683 0.8669 0.7060 0.163 Uiso 1 1 calc R . . H36C H -0.0214 0.8235 0.6896 0.163 Uiso 1 1 calc R . . C37 C 0.4285(6) 0.7402(3) 0.6948(3) 0.0266(19) Uani 1 1 d . . . C38 C 0.3565(6) 0.7052(3) 0.6938(4) 0.030(2) Uani 1 1 d . . . C39 C 0.3913(7) 0.6242(3) 0.7248(4) 0.042(2) Uani 1 1 d . . . H3B H 0.3239 0.6154 0.7192 0.051 Uiso 1 1 calc R . . C40 C 0.4706(8) 0.5952(3) 0.7442(4) 0.047(3) Uani 1 1 d . . . H4B H 0.4554 0.5666 0.7526 0.057 Uiso 1 1 calc R . . C41 C 0.5683(8) 0.6065(3) 0.7517(4) 0.046(3) Uani 1 1 d . . . H5B H 0.6189 0.5855 0.7637 0.056 Uiso 1 1 calc R . . C42 C 0.6922(7) 0.6658(3) 0.7482(4) 0.049(3) Uani 1 1 d . . . H6B H 0.7481 0.6473 0.7592 0.059 Uiso 1 1 calc R . . C43 C 0.7067(7) 0.7091(4) 0.7388(4) 0.054(3) Uani 1 1 d . . . H7B H 0.7728 0.7196 0.7442 0.064 Uiso 1 1 calc R . . C44 C 0.6243(7) 0.7385(3) 0.7212(4) 0.044(3) Uani 1 1 d . . . H8B H 0.6353 0.7680 0.7149 0.052 Uiso 1 1 calc R . . C45 C 0.5299(6) 0.7227(3) 0.7138(4) 0.034(2) Uani 1 1 d . . . C46 C 0.4152(6) 0.6660(3) 0.7140(4) 0.031(2) Uani 1 1 d . . . C47 C 0.5954(7) 0.6493(3) 0.7417(4) 0.039(2) Uani 1 1 d . . . C48 C 0.5158(6) 0.6782(3) 0.7235(3) 0.032(2) Uani 1 1 d . . . C49 C 0.4505(6) 0.8150(3) 0.6775(4) 0.032(2) Uani 1 1 d . . . C50 C 0.4887(6) 0.8350(3) 0.7278(4) 0.035(2) Uani 1 1 d . . . C51 C 0.5370(7) 0.8742(3) 0.7280(4) 0.045(3) Uani 1 1 d . . . H15B H 0.5635 0.8889 0.7617 0.054 Uiso 1 1 calc R . . C52 C 0.5464(8) 0.8917(3) 0.6791(5) 0.057(3) Uani 1 1 d . . . H16B H 0.5789 0.9186 0.6794 0.069 Uiso 1 1 calc R . . C53 C 0.5097(8) 0.8710(4) 0.6303(5) 0.056(3) Uani 1 1 d . . . H17B H 0.5183 0.8837 0.5975 0.068 Uiso 1 1 calc R . . C54 C 0.4600(6) 0.8319(3) 0.6271(4) 0.038(2) Uani 1 1 d . . . C55 C 0.4770(7) 0.8173(3) 0.7829(4) 0.044(2) Uani 1 1 d . . . H19B H 0.4624 0.7859 0.7779 0.053 Uiso 1 1 calc R . . C58 C 0.4206(7) 0.8077(3) 0.5744(4) 0.045(3) Uani 1 1 d . . . H20B H 0.3543 0.7952 0.5744 0.054 Uiso 1 1 calc R . . C56 C 0.5699(9) 0.8223(4) 0.8300(5) 0.087(4) Uani 1 1 d . . . H21D H 0.6260 0.8078 0.8207 0.130 Uiso 1 1 calc R . . H21E H 0.5582 0.8095 0.8634 0.130 Uiso 1 1 calc R . . H21F H 0.5853 0.8529 0.8363 0.130 Uiso 1 1 calc R . . C57 C 0.3899(9) 0.8384(4) 0.8000(5) 0.082(4) Uani 1 1 d . . . H22D H 0.3915 0.8298 0.8377 0.124 Uiso 1 1 calc R . . H22E H 0.3268 0.8291 0.7750 0.124 Uiso 1 1 calc R . . H22F H 0.3956 0.8697 0.7982 0.124 Uiso 1 1 calc R . . C59 C 0.4931(9) 0.7700(4) 0.5699(5) 0.074(4) Uani 1 1 d . . . H23D H 0.5555 0.7819 0.5648 0.111 Uiso 1 1 calc R . . H23E H 0.4619 0.7518 0.5384 0.111 Uiso 1 1 calc R . . H23F H 0.5072 0.7529 0.6037 0.111 Uiso 1 1 calc R . . C60 C 0.4077(8) 0.8366(4) 0.5232(4) 0.065(3) Uani 1 1 d . . . H24D H 0.3732 0.8631 0.5285 0.097 Uiso 1 1 calc R . . H24E H 0.3683 0.8214 0.4907 0.097 Uiso 1 1 calc R . . H24F H 0.4734 0.8437 0.5179 0.097 Uiso 1 1 calc R . . C61 C 0.1889(6) 0.6823(2) 0.6626(4) 0.031(2) Uani 1 1 d . . . C62 C 0.1196(7) 0.6813(3) 0.6946(4) 0.042(2) Uani 1 1 d . . . C63 C 0.0463(7) 0.6488(3) 0.6819(5) 0.049(3) Uani 1 1 d . . . H27B H -0.0014 0.6463 0.7029 0.059 Uiso 1 1 calc R . . C64 C 0.0436(9) 0.6204(4) 0.6390(6) 0.067(4) Uani 1 1 d . . . H28B H -0.0061 0.5987 0.6309 0.080 Uiso 1 1 calc R . . C65 C 0.1114(8) 0.6232(3) 0.6082(5) 0.054(3) Uani 1 1 d . . . H29B H 0.1072 0.6035 0.5788 0.065 Uiso 1 1 calc R . . C66 C 0.1867(7) 0.6543(3) 0.6190(4) 0.041(2) Uani 1 1 d . . . C67 C 0.1230(8) 0.7125(3) 0.7410(4) 0.048(3) Uani 1 1 d . . . H31B H 0.1567 0.7392 0.7331 0.058 Uiso 1 1 calc R . . C70 C 0.2575(8) 0.6588(3) 0.5815(4) 0.051(3) Uani 1 1 d . . . H32B H 0.3168 0.6756 0.6023 0.062 Uiso 1 1 calc R . . C68 C 0.1848(11) 0.6942(5) 0.7946(5) 0.100(5) Uani 1 1 d . . . H33D H 0.1484 0.6706 0.8063 0.150 Uiso 1 1 calc R . . H33E H 0.1978 0.7168 0.8228 0.150 Uiso 1 1 calc R . . H33F H 0.2482 0.6835 0.7895 0.150 Uiso 1 1 calc R . . C69 C 0.0171(9) 0.7248(4) 0.7439(6) 0.087(4) Uani 1 1 d . . . H34D H -0.0137 0.7433 0.7126 0.131 Uiso 1 1 calc R . . H34E H 0.0207 0.7402 0.7783 0.131 Uiso 1 1 calc R . . H34F H -0.0230 0.6987 0.7426 0.131 Uiso 1 1 calc R . . C71 C 0.2103(10) 0.6836(4) 0.5308(5) 0.078(4) Uani 1 1 d . . . H35D H 0.1497 0.6688 0.5104 0.117 Uiso 1 1 calc R . . H35E H 0.2571 0.6858 0.5077 0.117 Uiso 1 1 calc R . . H35F H 0.1932 0.7124 0.5410 0.117 Uiso 1 1 calc R . . C72 C 0.2950(12) 0.6156(4) 0.5677(6) 0.111(6) Uani 1 1 d . . . H36D H 0.2381 0.5968 0.5520 0.166 Uiso 1 1 calc R . . H36E H 0.3367 0.6024 0.6012 0.166 Uiso 1 1 calc R . . H36F H 0.3345 0.6195 0.5409 0.166 Uiso 1 1 calc R . . C21T C 0.4061(11) 0.9622(5) 0.9543(7) 0.089(4) Uani 1 1 d . . . C22T C 0.4096(14) 0.9347(5) 0.9963(8) 0.114(6) Uani 1 1 d . . . H22T H 0.4597 0.9131 1.0039 0.136 Uiso 1 1 calc R . . C23T C 0.3373(15) 0.9370(6) 1.0312(8) 0.120(7) Uani 1 1 d . . . H23T H 0.3390 0.9172 1.0602 0.144 Uiso 1 1 calc R . . C24T C 0.2684(13) 0.9694(6) 1.0187(7) 0.109(5) Uani 1 1 d . . . H24T H 0.2203 0.9724 1.0393 0.130 Uiso 1 1 calc R . . C25T C 0.2677(10) 0.9983(4) 0.9760(7) 0.087(4) Uani 1 1 d . . . H25T H 0.2193 1.0206 0.9683 0.105 Uiso 1 1 calc R . . C26T C 0.3372(10) 0.9951(4) 0.9441(5) 0.068(3) Uani 1 1 d . . . H26T H 0.3366 1.0154 0.9158 0.082 Uiso 1 1 calc R . . C27T C 0.4810(12) 0.9538(7) 0.9226(7) 0.164(9) Uani 1 1 d . . . H27C H 0.5381 0.9732 0.9354 0.245 Uiso 1 1 calc R . . H27D H 0.4507 0.9589 0.8834 0.245 Uiso 1 1 calc R . . H27E H 0.5037 0.9240 0.9281 0.245 Uiso 1 1 calc R . . C1T C 0.5476(12) 0.5423(5) 0.5903(7) 0.093(5) Uani 1 1 d . . . C2T C 0.6222(13) 0.5704(7) 0.6225(6) 0.119(6) Uani 1 1 d . . . H2T H 0.6562 0.5606 0.6582 0.142 Uiso 1 1 calc R . . C3T C 0.650(2) 0.6109(8) 0.6068(8) 0.203(16) Uani 1 1 d . . . H3T H 0.6954 0.6289 0.6318 0.244 Uiso 1 1 calc R . . C4T C 0.6120(18) 0.6220(7) 0.5577(13) 0.177(11) Uani 1 1 d . . . H4T H 0.6309 0.6490 0.5460 0.213 Uiso 1 1 calc R . . C5T C 0.5377(13) 0.5950(6) 0.5158(8) 0.120(6) Uani 1 1 d . . . H5T H 0.5129 0.6037 0.4786 0.144 Uiso 1 1 calc R . . C6T C 0.5078(10) 0.5557(5) 0.5361(7) 0.094(5) Uani 1 1 d . . . H6T H 0.4594 0.5382 0.5121 0.113 Uiso 1 1 calc R . . C7T C 0.5135(12) 0.5019(4) 0.6088(6) 0.115(6) Uani 1 1 d . . . H7T1 H 0.4609 0.5077 0.6273 0.172 Uiso 1 1 calc R . . H7T2 H 0.5696 0.4876 0.6345 0.172 Uiso 1 1 calc R . . H7T3 H 0.4873 0.4832 0.5770 0.172 Uiso 1 1 calc R . . C11T C 0.8047(17) 0.8922(6) 0.8386(7) 0.179(9) Uiso 1 1 d D . . C12T C 0.7795(14) 0.8974(5) 0.8900(6) 0.150(7) Uiso 1 1 d D . . H12T H 0.7976 0.8766 0.9185 0.226 Uiso 1 1 calc R . . C13T C 0.7281(14) 0.9337(6) 0.8956(6) 0.160(8) Uiso 1 1 d D . . H13T H 0.7146 0.9388 0.9302 0.240 Uiso 1 1 calc R . . C14T C 0.6943(15) 0.9636(5) 0.8543(7) 0.173(8) Uiso 1 1 d D . . H14T H 0.6554 0.9875 0.8598 0.259 Uiso 1 1 calc R . . C15T C 0.7184(13) 0.9580(5) 0.8046(7) 0.146(7) Uiso 1 1 d D . . H15T H 0.6990 0.9784 0.7758 0.220 Uiso 1 1 calc R . . C16T C 0.7721(13) 0.9211(5) 0.7982(6) 0.141(7) Uiso 1 1 d D . . H16T H 0.7861 0.9162 0.7637 0.212 Uiso 1 1 calc R . . C17T C 0.855(3) 0.8579(12) 0.8342(11) 0.316(18) Uiso 1 1 d D . . H17C H 0.9260 0.8625 0.8548 0.474 Uiso 1 1 d . . . H17D H 0.8508 0.8517 0.7965 0.474 Uiso 1 1 d . . . H17E H 0.8296 0.8335 0.8519 0.474 Uiso 1 1 d . . . C31T C 0.5209(19) 0.9982(8) 0.5263(9) 0.067(7) Uiso 0.50 1 d P . . C32T C 0.4670(10) 1.0265(4) 0.5278(6) 0.078(4) Uiso 1 1 d . . . C33T C 0.395(2) 1.0447(8) 0.4820(11) 0.079(8) Uiso 0.50 1 d P . . C34T C 0.3980(12) 1.0245(5) 0.4269(6) 0.104(5) Uiso 1 1 d . . . C35T C 0.463(2) 0.9940(8) 0.4276(11) 0.076(7) Uiso 0.50 1 d P . . Cl1 Cl 0.8548(12) 0.7534(6) 0.8569(7) 0.242(7) Uani 0.50 1 d P . . Cl2 Cl 1.0406(8) 0.7389(3) 0.9244(5) 0.148(4) Uani 0.50 1 d P . . C1M C 0.941(2) 0.7176(10) 0.8766(11) 0.105(11) Uani 0.50 1 d P . . H1M1 H 0.9637 0.7073 0.8445 0.158 Uiso 0.50 1 calc PR . . H1M2 H 0.9146 0.6927 0.8927 0.158 Uiso 0.50 1 calc PR . . 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 Au1 0.02860(18) 0.02645(18) 0.02653(19) -0.00047(14) 0.00604(15) 0.00048(14) Pt1 0.02269(17) 0.02626(17) 0.02329(18) 0.00198(14) 0.00501(14) 0.00053(14) P1 0.0301(13) 0.0274(12) 0.0306(14) -0.0020(10) 0.0076(11) 0.0019(10) F1 0.115(8) 0.242(12) 0.128(9) -0.083(8) 0.067(7) -0.037(8) O1 0.025(3) 0.029(3) 0.022(3) 0.002(2) 0.002(3) -0.001(2) N1 0.037(4) 0.026(4) 0.020(4) -0.002(3) 0.006(3) -0.002(3) C73 0.033(5) 0.027(5) 0.020(5) -0.004(4) -0.004(4) 0.000(4) B1 0.073(12) 0.084(13) 0.097(15) -0.009(11) 0.030(11) -0.027(10) Pt2 0.02123(17) 0.02411(17) 0.02650(19) 0.00238(14) 0.00570(14) 0.00050(14) F2 0.099(7) 0.136(8) 0.202(12) 0.028(8) -0.014(7) -0.036(6) O2 0.026(3) 0.038(3) 0.028(3) 0.007(3) 0.009(3) -0.005(3) N2 0.020(4) 0.045(5) 0.031(4) 0.003(4) 0.002(3) 0.002(3) C74 0.045(6) 0.033(5) 0.041(6) -0.006(4) 0.007(5) 0.003(4) F3 0.071(5) 0.108(6) 0.116(7) -0.002(5) 0.009(5) -0.040(5) N3 0.019(4) 0.028(4) 0.028(4) -0.002(3) 0.003(3) 0.000(3) C75 0.044(6) 0.043(6) 0.058(8) -0.008(5) 0.021(6) 0.006(5) F4 0.043(4) 0.130(7) 0.175(9) -0.040(6) 0.047(5) 0.003(4) N4 0.031(4) 0.019(4) 0.033(4) 0.002(3) 0.004(3) -0.002(3) C76 0.033(6) 0.055(7) 0.065(8) 0.012(6) 0.002(6) 0.018(5) C77 0.069(8) 0.064(8) 0.056(8) 0.020(6) 0.005(7) 0.021(6) C78 0.061(7) 0.058(7) 0.037(7) 0.005(5) 0.016(6) 0.011(6) C79 0.027(5) 0.031(5) 0.029(5) 0.003(4) 0.004(4) -0.004(4) C80 0.065(7) 0.033(6) 0.044(7) -0.005(5) 0.009(6) -0.004(5) C81 0.077(9) 0.055(7) 0.040(7) 0.003(5) 0.012(6) -0.001(6) C82 0.071(8) 0.054(7) 0.041(7) 0.014(5) 0.020(6) 0.003(6) C83 0.074(8) 0.045(6) 0.051(7) -0.002(6) 0.019(6) -0.015(6) C84 0.055(7) 0.039(6) 0.029(6) -0.001(4) 0.010(5) -0.008(5) C85 0.029(5) 0.031(5) 0.020(5) 0.003(4) 0.002(4) 0.006(4) C86 0.032(5) 0.035(5) 0.035(6) 0.001(4) 0.004(4) 0.001(4) C87 0.055(7) 0.023(5) 0.044(6) -0.001(4) -0.003(5) 0.003(4) C88 0.038(6) 0.030(5) 0.048(6) 0.000(4) 0.009(5) -0.011(4) C89 0.028(5) 0.054(7) 0.057(7) -0.010(5) 0.021(5) -0.004(5) C90 0.049(6) 0.031(5) 0.044(6) -0.001(4) 0.013(5) 0.005(5) C1 0.039(6) 0.026(5) 0.027(5) -0.010(4) -0.010(4) 0.008(4) C2 0.026(5) 0.047(6) 0.025(5) 0.002(4) 0.001(4) 0.003(4) C3 0.040(7) 0.098(9) 0.050(8) -0.002(6) -0.003(6) 0.016(6) C4 0.039(7) 0.160(14) 0.051(9) 0.012(9) 0.003(6) 0.041(8) C5 0.053(8) 0.147(14) 0.049(9) -0.018(8) -0.008(7) 0.059(9) C6 0.127(13) 0.060(8) 0.032(7) 0.006(6) -0.004(8) 0.070(9) C7 0.107(11) 0.056(8) 0.038(7) 0.008(5) 0.008(8) 0.050(8) C8 0.093(9) 0.041(6) 0.031(6) -0.009(5) 0.012(6) 0.017(6) C9 0.069(8) 0.043(6) 0.023(6) -0.002(5) 0.001(5) 0.023(5) C10 0.032(6) 0.055(6) 0.027(6) -0.002(5) -0.010(4) 0.014(5) C11 0.074(9) 0.058(7) 0.031(6) -0.011(5) -0.001(6) 0.038(6) C12 0.049(7) 0.056(7) 0.023(6) -0.005(5) -0.009(5) 0.030(5) C13 0.046(6) 0.032(5) 0.013(4) 0.005(4) 0.006(4) 0.005(4) C14 0.058(7) 0.034(5) 0.031(6) 0.008(4) 0.019(5) 0.007(5) C15 0.059(7) 0.061(7) 0.034(6) 0.007(5) 0.017(5) 0.012(6) C16 0.048(6) 0.052(6) 0.043(7) 0.006(5) 0.027(5) 0.001(5) C17 0.044(6) 0.034(5) 0.039(6) 0.007(4) 0.014(5) 0.000(4) C18 0.046(6) 0.027(5) 0.036(6) 0.000(4) 0.014(5) 0.003(4) C19 0.067(7) 0.042(6) 0.031(6) -0.011(4) 0.020(5) -0.009(5) C22 0.045(6) 0.042(6) 0.030(6) -0.004(4) 0.013(5) -0.011(5) C20 0.087(9) 0.058(7) 0.047(8) -0.008(6) 0.002(7) -0.008(7) C21 0.117(12) 0.038(7) 0.086(10) -0.002(6) -0.014(9) 0.005(7) C23 0.123(12) 0.059(8) 0.055(8) -0.029(6) -0.005(8) 0.048(8) C24 0.055(7) 0.070(8) 0.038(7) 0.004(5) 0.005(6) -0.014(6) C25 0.014(4) 0.061(7) 0.035(6) 0.011(5) -0.005(4) -0.006(4) C26 0.031(5) 0.051(6) 0.045(7) 0.001(5) 0.005(5) -0.004(5) C27 0.045(7) 0.065(8) 0.088(10) -0.016(7) 0.029(7) -0.022(6) C28 0.051(8) 0.093(10) 0.097(11) 0.002(8) 0.021(8) -0.039(7) C29 0.036(6) 0.078(8) 0.061(8) -0.014(6) 0.020(6) -0.026(6) C30 0.022(5) 0.067(7) 0.045(7) -0.002(5) 0.012(5) 0.002(5) C31 0.045(6) 0.055(7) 0.047(7) -0.008(5) 0.022(5) -0.020(5) C34 0.038(6) 0.063(7) 0.053(7) -0.005(6) 0.016(5) -0.013(5) C32 0.088(10) 0.064(8) 0.054(8) -0.018(6) 0.022(7) -0.019(7) C33 0.070(8) 0.053(8) 0.084(10) -0.008(6) 0.003(7) 0.002(6) C35 0.094(11) 0.100(11) 0.111(13) -0.043(9) -0.016(9) 0.048(9) C36 0.137(14) 0.097(11) 0.059(10) -0.021(8) -0.037(9) -0.005(10) C37 0.030(5) 0.027(5) 0.029(5) 0.002(4) 0.017(4) 0.003(4) C38 0.030(5) 0.031(5) 0.031(5) 0.000(4) 0.008(4) 0.003(4) C39 0.044(6) 0.041(6) 0.035(6) 0.008(5) -0.003(5) -0.002(5) C40 0.052(7) 0.037(6) 0.048(7) 0.008(5) 0.005(6) 0.012(5) C41 0.058(7) 0.046(6) 0.035(6) 0.004(5) 0.011(5) 0.025(5) C42 0.038(6) 0.053(7) 0.059(7) 0.014(5) 0.019(5) 0.019(5) C43 0.014(5) 0.087(9) 0.063(8) 0.010(6) 0.016(5) 0.011(5) C44 0.031(5) 0.047(6) 0.054(7) 0.012(5) 0.012(5) 0.008(4) C45 0.027(5) 0.041(5) 0.037(6) 0.011(4) 0.015(4) 0.007(4) C46 0.029(5) 0.028(5) 0.036(6) -0.001(4) 0.009(4) 0.006(4) C47 0.044(6) 0.040(6) 0.037(6) 0.003(4) 0.016(5) 0.013(5) C48 0.039(5) 0.031(5) 0.027(5) 0.003(4) 0.012(4) 0.011(4) C49 0.023(5) 0.026(5) 0.045(6) 0.007(4) 0.005(4) 0.001(4) C50 0.028(5) 0.034(5) 0.041(6) 0.009(4) 0.006(4) 0.000(4) C51 0.035(6) 0.036(6) 0.060(7) 0.000(5) 0.004(5) -0.011(4) C52 0.049(7) 0.045(7) 0.081(9) 0.015(6) 0.022(7) -0.019(5) C53 0.042(6) 0.064(8) 0.065(8) 0.029(6) 0.017(6) 0.001(6) C54 0.019(5) 0.044(6) 0.051(7) 0.021(5) 0.007(4) 0.005(4) C55 0.038(6) 0.043(6) 0.046(7) 0.008(5) 0.002(5) -0.005(5) C58 0.033(5) 0.063(7) 0.042(6) 0.017(5) 0.017(5) 0.008(5) C56 0.058(8) 0.123(12) 0.061(9) 0.024(8) -0.017(7) -0.006(8) C57 0.093(10) 0.110(11) 0.058(9) 0.040(7) 0.043(8) 0.058(8) C59 0.096(10) 0.076(9) 0.052(8) 0.001(6) 0.019(7) 0.035(7) C60 0.068(8) 0.087(9) 0.039(7) 0.032(6) 0.013(6) 0.016(7) C61 0.029(5) 0.017(4) 0.042(6) 0.010(4) 0.001(4) 0.003(4) C62 0.036(5) 0.042(6) 0.043(6) 0.024(5) 0.001(5) 0.004(5) C63 0.035(6) 0.051(7) 0.057(8) 0.019(6) 0.003(5) -0.002(5) C64 0.053(8) 0.048(7) 0.087(10) 0.035(7) -0.005(7) -0.013(6) C65 0.058(7) 0.032(6) 0.053(7) -0.002(5) -0.019(6) 0.005(5) C66 0.045(6) 0.028(5) 0.037(6) 0.005(4) -0.016(5) -0.001(4) C67 0.061(7) 0.053(7) 0.037(6) 0.017(5) 0.025(6) 0.003(5) C70 0.051(7) 0.054(7) 0.040(7) -0.005(5) -0.005(5) 0.014(5) C68 0.134(14) 0.124(12) 0.041(8) -0.003(8) 0.017(9) 0.048(10) C69 0.056(8) 0.090(10) 0.119(13) -0.033(9) 0.029(8) -0.006(7) C71 0.087(10) 0.073(9) 0.076(10) 0.020(7) 0.026(8) 0.026(7) C72 0.166(16) 0.087(11) 0.095(12) -0.005(9) 0.062(12) 0.048(10) C21T 0.080(11) 0.081(11) 0.095(12) -0.011(9) 0.004(9) -0.001(9) C22T 0.099(14) 0.069(11) 0.142(18) 0.008(11) -0.025(12) 0.006(9) C23T 0.102(14) 0.110(15) 0.112(16) 0.031(11) -0.040(12) -0.007(12) C24T 0.093(13) 0.142(16) 0.094(13) -0.005(11) 0.029(11) -0.047(12) C25T 0.070(10) 0.066(9) 0.130(14) 0.000(9) 0.035(10) 0.003(7) C26T 0.088(10) 0.060(8) 0.053(8) 0.005(6) 0.013(7) 0.001(7) C27T 0.087(13) 0.30(3) 0.116(16) -0.088(16) 0.047(12) -0.047(15) C1T 0.088(12) 0.128(14) 0.069(11) 0.013(10) 0.033(10) 0.018(10) C2T 0.111(14) 0.181(19) 0.067(11) -0.051(12) 0.030(11) -0.008(13) C3T 0.36(4) 0.18(2) 0.059(13) 0.013(13) 0.020(18) -0.16(2) C4T 0.17(2) 0.115(17) 0.26(3) -0.03(2) 0.07(2) -0.072(16) C5T 0.095(13) 0.157(17) 0.123(16) 0.042(13) 0.056(12) 0.032(12) C6T 0.065(9) 0.097(11) 0.140(16) 0.019(10) 0.062(11) 0.013(8) C7T 0.140(15) 0.102(12) 0.119(14) 0.060(10) 0.065(12) 0.006(10) Cl1 0.185(14) 0.282(18) 0.248(18) -0.049(14) 0.035(13) 0.059(13) Cl2 0.122(8) 0.168(9) 0.158(10) 0.079(8) 0.043(7) -0.005(7) C1M 0.09(2) 0.18(3) 0.06(2) 0.06(2) 0.037(18) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 O1 2.054(5) . ? Au1 P1 2.218(2) . ? Au1 Pt1 3.0494(5) . ? Au1 Pt2 3.1949(5) . ? Pt1 O2 1.961(5) . ? Pt1 N2 1.993(7) . ? Pt1 N1 2.018(6) . ? Pt1 O1 2.021(5) . ? P1 C85 1.815(9) . ? P1 C79 1.818(9) . ? P1 C73 1.825(9) . ? F1 B1 1.337(19) . ? O1 Pt2 2.023(5) . ? N1 C1 1.301(10) . ? N1 C13 1.461(10) . ? C73 C78 1.369(12) . ? C73 C74 1.383(12) . ? B1 F4 1.302(18) . ? B1 F3 1.319(17) . ? B1 F2 1.483(19) . ? Pt2 O2 1.972(5) . ? Pt2 N4 2.007(6) . ? Pt2 N3 2.009(6) . ? N2 C2 1.306(10) . ? N2 C25 1.461(10) . ? C74 C75 1.386(12) . ? N3 C37 1.294(9) . ? N3 C49 1.445(10) . ? C75 C76 1.378(14) . ? N4 C38 1.293(10) . ? N4 C61 1.450(10) . ? C76 C77 1.391(14) . ? C77 C78 1.409(14) . ? C79 C80 1.397(12) . ? C79 C84 1.399(11) . ? C80 C81 1.367(13) . ? C81 C82 1.369(13) . ? C82 C83 1.368(14) . ? C83 C84 1.365(13) . ? C85 C90 1.393(12) . ? C85 C86 1.414(11) . ? C86 C87 1.392(12) . ? C87 C88 1.405(13) . ? C88 C89 1.360(12) . ? C89 C90 1.381(12) . ? C1 C2 1.442(12) . ? C1 C9 1.478(12) . ? C2 C10 1.466(12) . ? C3 C10 1.380(14) . ? C3 C4 1.414(15) . ? C4 C5 1.363(17) . ? C5 C11 1.396(17) . ? C6 C7 1.326(17) . ? C6 C11 1.426(16) . ? C7 C8 1.417(14) . ? C8 C9 1.392(13) . ? C9 C12 1.400(14) . ? C10 C12 1.385(13) . ? C11 C12 1.428(13) . ? C13 C14 1.395(11) . ? C13 C18 1.402(12) . ? C14 C15 1.385(13) . ? C14 C19 1.527(12) . ? C15 C16 1.382(13) . ? C16 C17 1.355(12) . ? C17 C18 1.417(12) . ? C18 C22 1.514(12) . ? C19 C20 1.508(13) . ? C19 C21 1.515(14) . ? C22 C23 1.485(13) . ? C22 C24 1.532(13) . ? C25 C30 1.401(13) . ? C25 C26 1.418(13) . ? C26 C27 1.395(13) . ? C26 C31 1.503(13) . ? C27 C28 1.378(16) . ? C28 C29 1.392(15) . ? C29 C30 1.380(13) . ? C30 C34 1.511(13) . ? C31 C33 1.532(13) . ? C31 C32 1.567(14) . ? C34 C36 1.493(15) . ? C34 C35 1.548(15) . ? C37 C45 1.469(11) . ? C37 C38 1.474(11) . ? C38 C46 1.483(11) . ? C39 C46 1.387(11) . ? C39 C40 1.409(12) . ? C40 C41 1.367(13) . ? C41 C47 1.423(13) . ? C42 C43 1.390(13) . ? C42 C47 1.408(13) . ? C43 C44 1.443(12) . ? C44 C45 1.366(12) . ? C45 C48 1.430(11) . ? C46 C48 1.406(12) . ? C47 C48 1.406(11) . ? C49 C50 1.388(12) . ? C49 C54 1.410(12) . ? C50 C51 1.390(11) . ? C50 C55 1.538(12) . ? C51 C52 1.384(14) . ? C52 C53 1.362(15) . ? C53 C54 1.390(13) . ? C54 C58 1.501(13) . ? C55 C56 1.517(14) . ? C55 C57 1.532(13) . ? C58 C60 1.543(12) . ? C58 C59 1.568(13) . ? C61 C66 1.392(12) . ? C61 C62 1.407(12) . ? C62 C63 1.412(13) . ? C62 C67 1.509(13) . ? C63 C64 1.388(15) . ? C64 C65 1.366(15) . ? C65 C66 1.400(13) . ? C66 C70 1.534(14) . ? C67 C68 1.510(15) . ? C67 C69 1.538(14) . ? C70 C71 1.489(14) . ? C70 C72 1.517(14) . ? C21T C22T 1.35(2) . ? C21T C26T 1.378(17) . ? C21T C27T 1.489(19) . ? C22T C23T 1.50(2) . ? C23T C24T 1.37(2) . ? C24T C25T 1.400(19) . ? C25T C26T 1.409(17) . ? C1T C6T 1.394(19) . ? C1T C2T 1.43(2) . ? C1T C7T 1.463(18) . ? C2T C3T 1.41(2) . ? C3T C4T 1.26(3) . ? C4T C5T 1.52(3) . ? C5T C6T 1.428(19) . ? C11T C17T 1.30(4) . ? C11T C16T 1.345(13) . ? C11T C12T 1.432(13) . ? C12T C13T 1.365(12) . ? C13T C14T 1.384(13) . ? C14T C15T 1.387(13) . ? C15T C16T 1.401(12) . ? C31T C35T 1.15(3) 3_676 ? C31T C32T 1.16(3) . ? C31T C31T 1.30(5) 3_676 ? C31T C34T 1.57(3) 3_676 ? C31T C32T 1.61(3) 3_676 ? C31T C33T 1.83(4) 3_676 ? C32T C35T 1.43(3) 3_676 ? C32T C33T 1.44(3) . ? C32T C31T 1.61(3) 3_676 ? C33T C34T 1.54(3) . ? C33T C31T 1.83(4) 3_676 ? C34T C35T 1.30(3) . ? C34T C31T 1.57(3) 3_676 ? C35T C31T 1.15(3) 3_676 ? C35T C32T 1.43(3) 3_676 ? Cl1 C1M 1.62(3) . ? Cl2 C1M 1.71(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Au1 P1 176.24(15) . . ? O1 Au1 Pt1 41.15(15) . . ? P1 Au1 Pt1 140.91(6) . . ? O1 Au1 Pt2 38.06(14) . . ? P1 Au1 Pt2 144.69(6) . . ? Pt1 Au1 Pt2 56.626(10) . . ? O2 Pt1 N2 97.8(3) . . ? O2 Pt1 N1 174.4(2) . . ? N2 Pt1 N1 79.3(3) . . ? O2 Pt1 O1 80.4(2) . . ? N2 Pt1 O1 170.6(2) . . ? N1 Pt1 O1 103.3(2) . . ? O2 Pt1 Au1 78.62(16) . . ? N2 Pt1 Au1 128.6(2) . . ? N1 Pt1 Au1 106.96(18) . . ? O1 Pt1 Au1 41.97(15) . . ? C85 P1 C79 106.8(4) . . ? C85 P1 C73 104.2(4) . . ? C79 P1 C73 106.3(4) . . ? C85 P1 Au1 112.2(3) . . ? C79 P1 Au1 114.2(3) . . ? C73 P1 Au1 112.6(3) . . ? Pt1 O1 Pt2 94.3(2) . . ? Pt1 O1 Au1 96.9(2) . . ? Pt2 O1 Au1 103.2(2) . . ? C1 N1 C13 118.0(7) . . ? C1 N1 Pt1 113.3(6) . . ? C13 N1 Pt1 127.0(5) . . ? C78 C73 C74 118.1(8) . . ? C78 C73 P1 118.8(7) . . ? C74 C73 P1 123.0(7) . . ? F4 B1 F3 118.1(15) . . ? F4 B1 F1 114.2(16) . . ? F3 B1 F1 113.6(14) . . ? F4 B1 F2 101.0(13) . . ? F3 B1 F2 103.6(14) . . ? F1 B1 F2 103.5(14) . . ? O2 Pt2 N4 101.4(2) . . ? O2 Pt2 N3 175.1(2) . . ? N4 Pt2 N3 80.1(3) . . ? O2 Pt2 O1 80.1(2) . . ? N4 Pt2 O1 172.3(2) . . ? N3 Pt2 O1 99.1(2) . . ? O2 Pt2 Au1 74.76(16) . . ? N4 Pt2 Au1 149.0(2) . . ? N3 Pt2 Au1 101.51(18) . . ? O1 Pt2 Au1 38.75(15) . . ? Pt1 O2 Pt2 97.8(2) . . ? C2 N2 C25 120.5(7) . . ? C2 N2 Pt1 115.2(6) . . ? C25 N2 Pt1 123.9(5) . . ? C73 C74 C75 120.8(9) . . ? C37 N3 C49 122.4(7) . . ? C37 N3 Pt2 114.3(5) . . ? C49 N3 Pt2 123.1(5) . . ? C76 C75 C74 121.1(9) . . ? C38 N4 C61 119.0(7) . . ? C38 N4 Pt2 114.8(6) . . ? C61 N4 Pt2 124.6(5) . . ? C75 C76 C77 119.1(9) . . ? C76 C77 C78 118.7(10) . . ? C73 C78 C77 122.1(10) . . ? C80 C79 C84 118.7(8) . . ? C80 C79 P1 122.9(7) . . ? C84 C79 P1 118.4(7) . . ? C81 C80 C79 119.9(9) . . ? C80 C81 C82 121.4(10) . . ? C83 C82 C81 118.5(10) . . ? C84 C83 C82 122.3(10) . . ? C83 C84 C79 119.2(9) . . ? C90 C85 C86 118.7(8) . . ? C90 C85 P1 119.2(6) . . ? C86 C85 P1 122.0(6) . . ? C87 C86 C85 119.7(9) . . ? C86 C87 C88 119.8(8) . . ? C89 C88 C87 120.2(8) . . ? C88 C89 C90 120.8(9) . . ? C89 C90 C85 120.8(8) . . ? N1 C1 C2 116.9(8) . . ? N1 C1 C9 135.8(9) . . ? C2 C1 C9 107.0(8) . . ? N2 C2 C1 113.8(8) . . ? N2 C2 C10 137.2(9) . . ? C1 C2 C10 108.6(8) . . ? C10 C3 C4 117.2(12) . . ? C5 C4 C3 123.1(13) . . ? C4 C5 C11 120.4(11) . . ? C7 C6 C11 123.4(11) . . ? C6 C7 C8 122.5(12) . . ? C9 C8 C7 117.2(12) . . ? C8 C9 C12 119.9(10) . . ? C8 C9 C1 135.5(11) . . ? C12 C9 C1 104.6(9) . . ? C3 C10 C12 120.5(9) . . ? C3 C10 C2 134.8(10) . . ? C12 C10 C2 104.7(9) . . ? C5 C11 C6 129.6(12) . . ? C5 C11 C12 116.6(11) . . ? C6 C11 C12 113.6(12) . . ? C10 C12 C9 114.7(9) . . ? C10 C12 C11 122.0(11) . . ? C9 C12 C11 123.2(11) . . ? C14 C13 C18 122.2(8) . . ? C14 C13 N1 117.1(8) . . ? C18 C13 N1 120.7(7) . . ? C15 C14 C13 117.2(9) . . ? C15 C14 C19 120.6(9) . . ? C13 C14 C19 122.1(8) . . ? C16 C15 C14 122.4(9) . . ? C17 C16 C15 119.5(9) . . ? C16 C17 C18 121.6(9) . . ? C13 C18 C17 117.1(8) . . ? C13 C18 C22 122.8(8) . . ? C17 C18 C22 120.2(8) . . ? C20 C19 C21 111.5(9) . . ? C20 C19 C14 113.9(8) . . ? C21 C19 C14 110.0(9) . . ? C23 C22 C18 111.3(8) . . ? C23 C22 C24 111.1(9) . . ? C18 C22 C24 112.4(8) . . ? C30 C25 C26 124.2(9) . . ? C30 C25 N2 118.1(9) . . ? C26 C25 N2 117.6(8) . . ? C27 C26 C25 116.4(9) . . ? C27 C26 C31 122.2(9) . . ? C25 C26 C31 121.3(8) . . ? C28 C27 C26 119.6(11) . . ? C27 C28 C29 122.8(11) . . ? C30 C29 C28 120.0(10) . . ? C29 C30 C25 116.7(10) . . ? C29 C30 C34 120.4(9) . . ? C25 C30 C34 122.8(9) . . ? C26 C31 C33 113.0(8) . . ? C26 C31 C32 109.2(9) . . ? C33 C31 C32 109.4(8) . . ? C36 C34 C30 111.4(9) . . ? C36 C34 C35 112.0(10) . . ? C30 C34 C35 113.5(9) . . ? N3 C37 C45 135.3(8) . . ? N3 C37 C38 115.8(7) . . ? C45 C37 C38 108.6(7) . . ? N4 C38 C37 115.0(7) . . ? N4 C38 C46 137.9(8) . . ? C37 C38 C46 107.0(7) . . ? C46 C39 C40 117.7(9) . . ? C41 C40 C39 122.8(9) . . ? C40 C41 C47 121.0(9) . . ? C43 C42 C47 120.7(9) . . ? C42 C43 C44 121.9(9) . . ? C45 C44 C43 118.0(9) . . ? C44 C45 C48 119.7(8) . . ? C44 C45 C37 135.6(8) . . ? C48 C45 C37 104.7(7) . . ? C39 C46 C48 119.8(8) . . ? C39 C46 C38 134.5(8) . . ? C48 C46 C38 105.7(7) . . ? C48 C47 C42 116.7(9) . . ? C48 C47 C41 115.7(9) . . ? C42 C47 C41 127.5(9) . . ? C46 C48 C47 123.1(8) . . ? C46 C48 C45 113.9(7) . . ? C47 C48 C45 123.0(8) . . ? C50 C49 C54 123.4(8) . . ? C50 C49 N3 119.0(8) . . ? C54 C49 N3 117.3(8) . . ? C49 C50 C51 117.8(8) . . ? C49 C50 C55 123.9(8) . . ? C51 C50 C55 118.3(9) . . ? C52 C51 C50 119.9(10) . . ? C53 C52 C51 121.0(10) . . ? C52 C53 C54 122.1(10) . . ? C53 C54 C49 115.7(9) . . ? C53 C54 C58 123.5(9) . . ? C49 C54 C58 120.7(8) . . ? C56 C55 C57 108.0(10) . . ? C56 C55 C50 113.7(8) . . ? C57 C55 C50 112.0(8) . . ? C54 C58 C60 112.5(9) . . ? C54 C58 C59 110.2(8) . . ? C60 C58 C59 108.4(8) . . ? C66 C61 C62 123.9(9) . . ? C66 C61 N4 119.1(8) . . ? C62 C61 N4 116.9(8) . . ? C61 C62 C63 116.5(9) . . ? C61 C62 C67 122.7(8) . . ? C63 C62 C67 120.8(9) . . ? C64 C63 C62 120.3(10) . . ? C65 C64 C63 121.2(10) . . ? C64 C65 C66 121.5(10) . . ? C61 C66 C65 116.7(10) . . ? C61 C66 C70 122.6(8) . . ? C65 C66 C70 120.5(9) . . ? C62 C67 C68 110.3(9) . . ? C62 C67 C69 111.0(9) . . ? C68 C67 C69 112.4(10) . . ? C71 C70 C72 111.3(10) . . ? C71 C70 C66 111.4(9) . . ? C72 C70 C66 111.9(9) . . ? C22T C21T C26T 120.0(16) . . ? C22T C21T C27T 114.8(18) . . ? C26T C21T C27T 125.2(17) . . ? C21T C22T C23T 122.3(16) . . ? C24T C23T C22T 115.8(16) . . ? C23T C24T C25T 121.1(17) . . ? C24T C25T C26T 121.4(14) . . ? C21T C26T C25T 119.4(13) . . ? C6T C1T C2T 114.7(16) . . ? C6T C1T C7T 119.3(16) . . ? C2T C1T C7T 126.0(17) . . ? C3T C2T C1T 126.7(18) . . ? C4T C3T C2T 116(2) . . ? C3T C4T C5T 124(2) . . ? C6T C5T C4T 115.6(18) . . ? C1T C6T C5T 121.8(17) . . ? C17T C11T C16T 124.6(12) . . ? C17T C11T C12T 115.7(11) . . ? C16T C11T C12T 119.6(10) . . ? C13T C12T C11T 116.3(9) . . ? C12T C13T C14T 124.3(10) . . ? C13T C14T C15T 118.6(9) . . ? C14T C15T C16T 117.8(9) . . ? C11T C16T C15T 123.1(10) . . ? C35T C31T C32T 77(2) 3_676 . ? C35T C31T C31T 158(4) 3_676 3_676 ? C32T C31T C31T 81(2) . 3_676 ? C35T C31T C34T 54.5(17) 3_676 3_676 ? C32T C31T C34T 131(2) . 3_676 ? C31T C31T C34T 148(3) 3_676 3_676 ? C35T C31T C32T 157(3) 3_676 3_676 ? C32T C31T C32T 127(2) . 3_676 ? C31T C31T C32T 45.5(17) 3_676 3_676 ? C34T C31T C32T 102.1(18) 3_676 3_676 ? C35T C31T C33T 108(2) 3_676 3_676 ? C32T C31T C33T 175(2) . 3_676 ? C31T C31T C33T 94(3) 3_676 3_676 ? C34T C31T C33T 53.1(13) 3_676 3_676 ? C32T C31T C33T 49.0(12) 3_676 3_676 ? C31T C32T C35T 51.3(15) . 3_676 ? C31T C32T C33T 126(2) . . ? C35T C32T C33T 176.9(19) 3_676 . ? C31T C32T C31T 53(2) . 3_676 ? C35T C32T C31T 104.5(19) 3_676 3_676 ? C33T C32T C31T 73.4(15) . 3_676 ? C32T C33T C34T 112.6(19) . . ? C32T C33T C31T 57.7(13) . 3_676 ? C34T C33T C31T 55.0(12) . 3_676 ? C35T C34T C33T 118(2) . . ? C35T C34T C31T 45.9(14) . 3_676 ? C33T C34T C31T 71.9(16) . 3_676 ? C31T C35T C34T 80(2) 3_676 . ? C31T C35T C32T 52.1(18) 3_676 3_676 ? C34T C35T C32T 132(2) . 3_676 ? Cl1 C1M Cl2 110(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.561 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.177 data_Pt(bian)_hydroxo_oxo_(2) _database_code_depnum_ccdc_archive 'CCDC 663518' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H79 N4 O2 Pt2 1+, B F4 1-' _chemical_formula_sum 'C72 H79 B F4 N4 O2 Pt2' _chemical_formula_weight 1509.38 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 18.4678(18) _cell_length_b 15.3307(15) _cell_length_c 24.099(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.058(2) _cell_angle_gamma 90.00 _cell_volume 6738.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5261 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.05 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 4.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2840 _exptl_absorpt_correction_T_max 0.8173 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 40450 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.11 _reflns_number_total 14761 _reflns_number_gt 7298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+96.9490P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14761 _refine_ls_number_parameters 782 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.46360(3) 0.58417(3) 0.476088(17) 0.03531(14) Uani 1 1 d . . . C11 C 0.4071(6) 0.7193(8) 0.4045(4) 0.031(3) Uani 1 1 d . . . Pt1' Pt 0.02202(4) 0.57988(3) 0.035575(17) 0.0537(2) Uani 1 1 d . . . C10' C 0.1046(7) 0.8388(7) 0.1433(4) 0.030(3) Uani 1 1 d . . . C9 C 0.3802(7) 0.7930(7) 0.3668(5) 0.039(3) Uani 1 1 d . . . C31' C -0.0188(8) 0.6033(8) 0.1947(5) 0.047(4) Uani 1 1 d . . . H31' H -0.0176 0.6482 0.1648 0.057 Uiso 1 1 calc R . . C8 C 0.3899(8) 0.8137(9) 0.3132(5) 0.048(4) Uani 1 1 d . . . H8 H 0.4143 0.7752 0.2914 0.058 Uiso 1 1 calc R . . N2' N 0.0763(6) 0.6108(5) 0.1101(3) 0.032(2) Uani 1 1 d . . . C35' C 0.2223(10) 0.4111(10) 0.0883(7) 0.074(5) Uani 1 1 d . . . H35A H 0.2474 0.3744 0.1187 0.110 Uiso 1 1 calc R . . H35B H 0.2536 0.4180 0.0593 0.110 Uiso 1 1 calc R . . H35C H 0.1760 0.3835 0.0718 0.110 Uiso 1 1 calc R . . O1' O 0.0350(9) 0.4498(6) 0.0388(4) 0.108(6) Uani 1 1 d . . . C13' C -0.0402(8) 0.7483(7) -0.0139(4) 0.037(3) Uani 1 1 d . . . N2 N 0.4439(6) 0.6501(7) 0.4031(4) 0.036(2) Uani 1 1 d . . . C10 C 0.3460(9) 0.8495(10) 0.3992(6) 0.055(4) Uani 1 1 d . . . O1 O 0.4835(6) 0.5186(6) 0.5486(4) 0.064(3) Uani 1 1 d . . . N1' N 0.0115(6) 0.7086(6) 0.0303(3) 0.040(3) Uani 1 1 d . . . C22' C -0.1288(9) 0.7731(9) 0.0573(6) 0.055(4) Uani 1 1 d . . . H22' H -0.0830 0.7630 0.0848 0.066 Uiso 1 1 calc R . . C12' C 0.0866(7) 0.6940(7) 0.1173(4) 0.034(3) Uani 1 1 d . . . C14' C -0.1079(9) 0.7758(8) -0.0008(5) 0.053(4) Uani 1 1 d . . . C18' C -0.0230(9) 0.7494(8) -0.0667(4) 0.046(4) Uani 1 1 d . . . N1 N 0.4119(6) 0.6859(7) 0.5008(4) 0.044(3) Uani 1 1 d . . . C8' C 0.1625(7) 0.7405(8) 0.2156(4) 0.033(3) Uani 1 1 d . . . H8' H 0.1744 0.6838 0.2302 0.039 Uiso 1 1 calc R . . F1 F 0.2717(6) 0.2469(7) 0.2264(4) 0.095(3) Uani 1 1 d . . . C34' C 0.2065(8) 0.5016(8) 0.1120(5) 0.046(3) Uani 1 1 d . . . H34' H 0.1819 0.5385 0.0803 0.056 Uiso 1 1 calc R . . C11' C 0.0489(6) 0.7497(7) 0.0728(5) 0.030(3) Uani 1 1 d . . . C31 C 0.5669(9) 0.7415(13) 0.3759(9) 0.083(6) Uani 1 1 d . . . H31 H 0.5326 0.7596 0.4020 0.099 Uiso 1 1 calc R . . C33' C -0.0210(10) 0.6524(10) 0.2500(6) 0.073(5) Uani 1 1 d . . . H33A H -0.0235 0.6104 0.2803 0.110 Uiso 1 1 calc R . . H33B H -0.0644 0.6902 0.2458 0.110 Uiso 1 1 calc R . . H33C H 0.0233 0.6881 0.2592 0.110 Uiso 1 1 calc R . . C9' C 0.1199(7) 0.7517(7) 0.1627(4) 0.032(3) Uani 1 1 d . . . F3 F 0.2034(7) 0.2339(7) 0.2934(5) 0.111(4) Uani 1 1 d . . . C25 C 0.4717(10) 0.6251(10) 0.3529(6) 0.060(5) Uani 1 1 d . . . C17' C -0.0780(11) 0.7765(9) -0.1110(5) 0.057(5) Uani 1 1 d . . . H17' H -0.0678 0.7781 -0.1484 0.069 Uiso 1 1 calc R . . C12 C 0.3864(9) 0.7377(8) 0.4607(5) 0.054(4) Uani 1 1 d . . . C25' C 0.0967(7) 0.5499(7) 0.1559(4) 0.032(3) Uani 1 1 d . . . C28' C 0.1231(10) 0.4271(9) 0.2389(5) 0.059(4) Uani 1 1 d . . . H28' H 0.1327 0.3847 0.2679 0.071 Uiso 1 1 calc R . . C5 C 0.3163(11) 0.9293(10) 0.3782(7) 0.078(5) Uani 1 1 d . . . C5' C 0.1276(6) 0.9127(8) 0.1747(5) 0.034(3) Uani 1 1 d . . . C7 C 0.3621(9) 0.8952(9) 0.2916(6) 0.060(4) Uani 1 1 d . . . H7 H 0.3668 0.9110 0.2542 0.072 Uiso 1 1 calc R . . C15' C -0.1605(10) 0.8040(9) -0.0457(7) 0.065(5) Uani 1 1 d . . . H15' H -0.2064 0.8257 -0.0388 0.078 Uiso 1 1 calc R . . C13 C 0.4100(12) 0.7095(11) 0.5583(6) 0.078(6) Uani 1 1 d . . . C30' C 0.0495(8) 0.5465(8) 0.1962(5) 0.044(4) Uani 1 1 d . . . C19' C 0.0539(11) 0.7271(11) -0.0797(5) 0.075(6) Uani 1 1 d . . . H19' H 0.0804 0.6956 -0.0462 0.090 Uiso 1 1 calc R . . C26' C 0.1557(8) 0.4939(8) 0.1556(5) 0.044(3) Uani 1 1 d . . . C30 C 0.5295(11) 0.6698(13) 0.3403(7) 0.074(6) Uani 1 1 d . . . F4 F 0.3102(8) 0.1662(7) 0.3021(5) 0.131(5) Uani 1 1 d . . . C16' C -0.1450(11) 0.8000(10) -0.1006(6) 0.066(5) Uani 1 1 d . . . H16' H -0.1824 0.8142 -0.1311 0.079 Uiso 1 1 calc R . . C4' C 0.1062(8) 0.9926(8) 0.1476(5) 0.047(4) Uani 1 1 d . . . H4' H 0.1229 1.0453 0.1661 0.057 Uiso 1 1 calc R . . C7' C 0.1871(7) 0.8143(8) 0.2463(5) 0.041(3) Uani 1 1 d . . . H7' H 0.2158 0.8069 0.2823 0.049 Uiso 1 1 calc R . . C26 C 0.4370(10) 0.5524(11) 0.3201(5) 0.061(5) Uani 1 1 d . . . C32' C -0.0883(9) 0.5497(10) 0.1781(6) 0.064(4) Uani 1 1 d . . . H32A H -0.0897 0.5272 0.1399 0.096 Uiso 1 1 calc R . . H32B H -0.1313 0.5867 0.1795 0.096 Uiso 1 1 calc R . . H32C H -0.0886 0.5008 0.2043 0.096 Uiso 1 1 calc R . . C1 C 0.3447(11) 0.8225(11) 0.4548(6) 0.080(6) Uani 1 1 d . . . C36' C 0.2774(10) 0.5470(12) 0.1383(7) 0.083(6) Uani 1 1 d . . . H36A H 0.2662 0.6061 0.1500 0.125 Uiso 1 1 calc R . . H36B H 0.3110 0.5503 0.1107 0.125 Uiso 1 1 calc R . . H36C H 0.3005 0.5138 0.1712 0.125 Uiso 1 1 calc R . . F2 F 0.2196(6) 0.1184(7) 0.2387(4) 0.095(3) Uani 1 1 d . . . C6 C 0.3284(10) 0.9519(10) 0.3238(7) 0.077(6) Uani 1 1 d . . . H6 H 0.3129 1.0074 0.3089 0.092 Uiso 1 1 calc R . . C28 C 0.5288(15) 0.5734(16) 0.2627(9) 0.112(10) Uani 1 1 d . . . H28 H 0.5506 0.5527 0.2321 0.135 Uiso 1 1 calc R . . C29 C 0.5616(14) 0.6434(16) 0.2927(9) 0.108(9) Uani 1 1 d . . . H29 H 0.6030 0.6724 0.2824 0.130 Uiso 1 1 calc R . . C6' C 0.1716(7) 0.8973(9) 0.2269(5) 0.043(3) Uani 1 1 d . . . H6' H 0.1911 0.9454 0.2492 0.051 Uiso 1 1 calc R . . C34 C 0.3704(13) 0.5076(11) 0.3364(7) 0.093(7) Uani 1 1 d . . . H34 H 0.3764 0.5080 0.3784 0.112 Uiso 1 1 calc R . . C22 C 0.3109(11) 0.600(2) 0.5616(8) 0.110(9) Uani 1 1 d . . . H22 H 0.3330 0.5741 0.5299 0.131 Uiso 1 1 calc R . . C24' C -0.1797(11) 0.6951(13) 0.0608(7) 0.090(6) Uani 1 1 d . . . H24A H -0.2247 0.7028 0.0336 0.135 Uiso 1 1 calc R . . H24B H -0.1922 0.6914 0.0987 0.135 Uiso 1 1 calc R . . H24C H -0.1550 0.6414 0.0522 0.135 Uiso 1 1 calc R . . C20' C 0.0537(15) 0.6666(11) -0.1307(7) 0.126(10) Uani 1 1 d . . . H20A H 0.0224 0.6915 -0.1634 0.188 Uiso 1 1 calc R . . H20B H 0.0349 0.6091 -0.1223 0.188 Uiso 1 1 calc R . . H20C H 0.1038 0.6605 -0.1388 0.188 Uiso 1 1 calc R . . C14 C 0.3621(15) 0.6721(17) 0.5868(8) 0.105(8) Uani 1 1 d . . . C36 C 0.2973(13) 0.5607(12) 0.3138(9) 0.115(8) Uani 1 1 d . . . H36D H 0.2875 0.5578 0.2727 0.173 Uiso 1 1 calc R . . H36E H 0.3036 0.6217 0.3257 0.173 Uiso 1 1 calc R . . H36F H 0.2561 0.5352 0.3292 0.173 Uiso 1 1 calc R . . C21' C 0.0969(11) 0.8112(13) -0.0861(8) 0.093(6) Uani 1 1 d . . . H21A H 0.1469 0.7964 -0.0916 0.139 Uiso 1 1 calc R . . H21B H 0.0986 0.8469 -0.0522 0.139 Uiso 1 1 calc R . . H21C H 0.0726 0.8440 -0.1188 0.139 Uiso 1 1 calc R . . C15 C 0.361(2) 0.703(2) 0.6435(9) 0.165(16) Uani 1 1 d . . . H15 H 0.3269 0.6796 0.6652 0.198 Uiso 1 1 calc R . . C27 C 0.4653(16) 0.5301(14) 0.2740(7) 0.114(9) Uani 1 1 d . . . H27 H 0.4428 0.4860 0.2494 0.137 Uiso 1 1 calc R . . C18 C 0.4595(18) 0.7761(14) 0.5812(6) 0.124(11) Uani 1 1 d . . . C2 C 0.3107(18) 0.8736(15) 0.4904(9) 0.173(15) Uani 1 1 d . . . H2 H 0.3090 0.8569 0.5281 0.208 Uiso 1 1 calc R . . C23' C -0.1649(13) 0.8572(13) 0.0747(8) 0.107(7) Uani 1 1 d . . . H23A H -0.1297 0.9054 0.0770 0.161 Uiso 1 1 calc R . . H23B H -0.1802 0.8486 0.1115 0.161 Uiso 1 1 calc R . . H23C H -0.2079 0.8711 0.0468 0.161 Uiso 1 1 calc R . . C35 C 0.3630(17) 0.4147(14) 0.3183(9) 0.156(12) Uani 1 1 d . . . H35D H 0.3395 0.4119 0.2789 0.235 Uiso 1 1 calc R . . H35E H 0.3330 0.3834 0.3418 0.235 Uiso 1 1 calc R . . H35F H 0.4117 0.3879 0.3222 0.235 Uiso 1 1 calc R . . C33 C 0.6377(12) 0.7116(15) 0.4130(11) 0.141(10) Uani 1 1 d . . . H33D H 0.6273 0.6610 0.4353 0.212 Uiso 1 1 calc R . . H33E H 0.6570 0.7592 0.4383 0.212 Uiso 1 1 calc R . . H33F H 0.6741 0.6955 0.3893 0.212 Uiso 1 1 calc R . . C32 C 0.5824(12) 0.8248(16) 0.3424(12) 0.166(14) Uani 1 1 d . . . H32D H 0.6273 0.8164 0.3261 0.249 Uiso 1 1 calc R . . H32E H 0.5884 0.8751 0.3678 0.249 Uiso 1 1 calc R . . H32F H 0.5411 0.8353 0.3122 0.249 Uiso 1 1 calc R . . B1 B 0.2519(11) 0.1913(11) 0.2653(6) 0.053(5) Uani 1 1 d . . . C4 C 0.2811(17) 0.9797(16) 0.4138(9) 0.161(14) Uani 1 1 d . . . H4 H 0.2587 1.0333 0.4009 0.193 Uiso 1 1 calc R . . C24 C 0.3014(14) 0.526(2) 0.6015(11) 0.186(15) Uani 1 1 d . . . H24D H 0.2779 0.5476 0.6324 0.279 Uiso 1 1 calc R . . H24E H 0.3495 0.5011 0.6165 0.279 Uiso 1 1 calc R . . H24F H 0.2706 0.4801 0.5812 0.279 Uiso 1 1 calc R . . C17 C 0.460(2) 0.7966(15) 0.6375(8) 0.21(2) Uani 1 1 d . . . H17 H 0.4967 0.8343 0.6558 0.253 Uiso 1 1 calc R . . C16 C 0.411(3) 0.766(2) 0.6659(10) 0.20(2) Uani 1 1 d . . . H16 H 0.4094 0.7878 0.7027 0.245 Uiso 1 1 calc R . . C3 C 0.2787(19) 0.9521(17) 0.4676(11) 0.183(15) Uani 1 1 d . . . H3 H 0.2540 0.9878 0.4909 0.220 Uiso 1 1 calc R . . C23 C 0.2354(16) 0.628(3) 0.5376(13) 0.23(2) Uani 1 1 d . . . H23D H 0.2005 0.6052 0.5605 0.343 Uiso 1 1 calc R . . H23E H 0.2229 0.6066 0.4990 0.343 Uiso 1 1 calc R . . H23F H 0.2332 0.6923 0.5374 0.343 Uiso 1 1 calc R . . C19 C 0.520(2) 0.811(2) 0.5505(10) 0.188(18) Uani 1 1 d . . . H19 H 0.5048 0.7993 0.5094 0.225 Uiso 1 1 calc R . . C20 C 0.591(2) 0.770(3) 0.5675(13) 0.25(3) Uani 1 1 d . . . H20D H 0.6046 0.7729 0.6085 0.380 Uiso 1 1 calc R . . H20E H 0.6285 0.8009 0.5500 0.380 Uiso 1 1 calc R . . H20F H 0.5894 0.7088 0.5556 0.380 Uiso 1 1 calc R . . C21 C 0.522(3) 0.9126(18) 0.5597(13) 0.32(3) Uani 1 1 d . . . H21D H 0.4979 0.9272 0.5918 0.473 Uiso 1 1 calc R . . H21E H 0.4969 0.9415 0.5259 0.473 Uiso 1 1 calc R . . H21F H 0.5734 0.9322 0.5671 0.473 Uiso 1 1 calc R . . C27' C 0.1670(9) 0.4326(9) 0.1989(6) 0.057(4) Uani 1 1 d . . . H27' H 0.2069 0.3932 0.2004 0.068 Uiso 1 1 calc R . . C29' C 0.0650(10) 0.4825(9) 0.2375(5) 0.057(4) Uani 1 1 d . . . H29' H 0.0342 0.4774 0.2654 0.068 Uiso 1 1 calc R . . C2' C 0.0388(8) 0.9224(8) 0.0660(5) 0.048(3) Uani 1 1 d . . . H2' H 0.0086 0.9263 0.0303 0.057 Uiso 1 1 calc R . . C3' C 0.0633(8) 0.9981(8) 0.0968(6) 0.048(4) Uani 1 1 d . . . H3' H 0.0493 1.0539 0.0816 0.058 Uiso 1 1 calc R . . C1' C 0.0603(7) 0.8421(7) 0.0896(4) 0.032(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0411(3) 0.0365(3) 0.0273(2) 0.0059(2) 0.00251(19) 0.0045(3) C11 0.020(6) 0.053(8) 0.019(5) -0.004(5) -0.001(5) 0.031(6) Pt1' 0.1175(6) 0.0161(2) 0.0208(2) -0.0007(2) -0.0096(3) -0.0171(3) C10' 0.044(8) 0.018(6) 0.029(6) -0.011(4) 0.006(6) -0.012(6) C9 0.052(9) 0.017(6) 0.039(6) 0.001(5) -0.016(6) 0.010(6) C31' 0.080(11) 0.031(7) 0.033(6) -0.003(5) 0.013(7) -0.006(7) C8 0.069(11) 0.035(8) 0.036(7) 0.008(6) -0.005(7) 0.006(7) N2' 0.058(7) 0.012(4) 0.023(4) 0.003(3) -0.002(5) -0.011(5) C35' 0.098(14) 0.053(10) 0.073(10) 0.001(9) 0.020(10) 0.004(11) O1' 0.242(17) 0.014(4) 0.045(6) -0.009(4) -0.049(8) -0.028(7) C13' 0.088(11) 0.010(5) 0.013(5) -0.002(4) 0.009(6) -0.026(6) N2 0.041(7) 0.042(6) 0.025(5) 0.000(4) 0.008(5) 0.006(5) C10 0.068(11) 0.050(9) 0.043(7) 0.001(6) -0.006(7) 0.024(8) O1 0.100(9) 0.048(6) 0.044(5) 0.018(5) 0.014(6) 0.021(6) N1' 0.081(9) 0.019(5) 0.016(4) 0.007(4) -0.003(5) -0.019(5) C22' 0.067(11) 0.045(9) 0.050(8) -0.005(7) -0.004(7) -0.018(8) C12' 0.055(9) 0.019(6) 0.029(6) -0.011(5) 0.005(6) -0.018(6) C14' 0.088(12) 0.031(7) 0.034(7) -0.003(6) -0.004(8) -0.039(8) C18' 0.103(12) 0.014(6) 0.017(5) 0.005(5) 0.001(6) 0.001(7) N1 0.067(8) 0.046(7) 0.021(5) 0.009(4) 0.013(5) 0.012(6) C8' 0.049(8) 0.023(6) 0.025(5) 0.000(5) 0.002(5) 0.002(6) F1 0.116(9) 0.068(6) 0.103(7) 0.038(6) 0.024(6) -0.005(7) C34' 0.065(10) 0.033(7) 0.043(7) 0.001(6) 0.014(7) -0.006(7) C11' 0.032(7) 0.020(6) 0.042(6) -0.018(5) 0.012(5) -0.021(5) C31 0.044(11) 0.091(14) 0.115(15) 0.059(13) 0.018(10) 0.011(10) C33' 0.114(16) 0.060(11) 0.052(8) -0.030(8) 0.031(10) -0.023(10) C9' 0.047(8) 0.019(6) 0.031(5) 0.000(5) 0.006(5) -0.011(6) F3 0.173(12) 0.073(7) 0.100(8) 0.004(6) 0.058(8) 0.001(8) C25 0.085(13) 0.058(10) 0.044(8) 0.028(7) 0.031(9) 0.044(9) C17' 0.103(15) 0.035(8) 0.029(7) 0.006(6) -0.004(8) -0.025(9) C12 0.083(12) 0.028(7) 0.049(8) -0.001(6) 0.004(8) 0.018(8) C25' 0.068(9) 0.016(5) 0.011(4) -0.002(4) 0.003(5) -0.011(6) C28' 0.103(13) 0.031(8) 0.037(7) 0.021(6) -0.007(8) -0.013(9) C5 0.120(16) 0.044(10) 0.061(9) -0.008(8) -0.010(10) 0.032(10) C5' 0.033(7) 0.025(6) 0.045(6) -0.010(6) 0.006(5) -0.009(6) C7 0.075(12) 0.042(9) 0.053(8) 0.012(7) -0.020(8) -0.015(8) C15' 0.083(13) 0.032(8) 0.077(11) 0.012(7) 0.003(10) -0.021(8) C13 0.144(18) 0.066(11) 0.024(7) -0.001(7) 0.012(9) 0.044(12) C30' 0.080(11) 0.023(6) 0.024(6) 0.005(5) -0.002(6) -0.014(7) C19' 0.139(17) 0.062(11) 0.026(7) 0.011(7) 0.022(9) 0.036(12) C26' 0.070(10) 0.023(7) 0.037(6) -0.002(5) 0.000(7) -0.001(7) C30 0.085(14) 0.083(13) 0.060(10) 0.039(10) 0.035(10) 0.037(12) F4 0.201(14) 0.069(8) 0.096(8) 0.021(6) -0.060(9) 0.011(8) C16' 0.085(14) 0.049(10) 0.051(9) 0.017(7) -0.029(9) -0.041(10) C4' 0.069(11) 0.020(7) 0.051(8) -0.011(6) 0.001(8) -0.011(7) C7' 0.056(9) 0.035(7) 0.029(6) -0.004(5) 0.000(6) -0.004(7) C26 0.089(13) 0.064(11) 0.031(7) 0.000(7) 0.015(8) 0.024(10) C32' 0.079(12) 0.054(10) 0.062(9) -0.013(8) 0.020(9) -0.008(9) C1 0.133(17) 0.068(11) 0.038(8) 0.010(7) 0.011(9) 0.043(12) C36' 0.085(14) 0.091(14) 0.078(12) -0.013(10) 0.028(10) -0.042(11) F2 0.138(10) 0.065(7) 0.076(6) -0.012(5) -0.002(6) -0.037(7) C6 0.099(15) 0.024(8) 0.088(12) 0.018(8) -0.047(11) -0.001(9) C28 0.17(3) 0.099(18) 0.089(15) 0.038(14) 0.082(17) 0.091(19) C29 0.14(2) 0.104(18) 0.093(15) 0.060(13) 0.055(15) 0.081(17) C6' 0.034(8) 0.043(8) 0.048(7) -0.021(6) -0.003(6) -0.006(6) C34 0.16(2) 0.052(11) 0.063(10) -0.037(9) 0.000(13) -0.015(13) C22 0.065(14) 0.20(3) 0.073(12) 0.062(16) 0.043(11) 0.048(17) C24' 0.102(16) 0.102(15) 0.069(11) 0.004(11) 0.024(11) -0.039(13) C20' 0.28(3) 0.049(11) 0.058(11) -0.007(9) 0.069(16) -0.004(15) C14 0.14(2) 0.12(2) 0.059(12) 0.021(12) 0.052(14) 0.060(17) C36 0.15(2) 0.061(14) 0.106(15) -0.002(11) -0.058(15) -0.005(14) C21' 0.100(16) 0.085(15) 0.089(13) -0.015(11) 0.002(12) 0.008(13) C15 0.28(4) 0.17(3) 0.059(14) 0.053(16) 0.06(2) 0.15(3) C27 0.22(3) 0.084(15) 0.044(10) -0.002(9) 0.025(14) 0.065(18) C18 0.26(3) 0.078(15) 0.021(7) -0.003(8) -0.011(13) 0.046(18) C2 0.34(4) 0.111(18) 0.083(14) 0.009(13) 0.08(2) 0.16(2) C23' 0.15(2) 0.082(15) 0.091(14) -0.023(12) 0.024(14) -0.017(15) C35 0.28(4) 0.075(16) 0.093(15) -0.016(13) -0.029(19) -0.04(2) C33 0.106(19) 0.11(2) 0.20(3) 0.079(19) -0.003(18) -0.014(16) C32 0.091(18) 0.16(2) 0.25(3) 0.15(2) 0.010(19) -0.009(17) B1 0.079(14) 0.046(10) 0.033(8) 0.004(7) 0.005(9) -0.002(10) C4 0.29(4) 0.12(2) 0.077(14) 0.007(14) 0.020(19) 0.14(2) C24 0.12(2) 0.29(4) 0.16(3) 0.10(3) 0.06(2) 0.01(3) C17 0.52(7) 0.081(17) 0.020(9) -0.006(10) 0.006(19) 0.01(3) C16 0.46(7) 0.11(2) 0.041(13) -0.016(14) 0.05(2) 0.08(3) C3 0.31(4) 0.12(2) 0.12(2) -0.010(17) 0.05(2) 0.15(3) C23 0.13(3) 0.37(5) 0.20(3) 0.17(4) 0.08(2) 0.08(3) C19 0.28(5) 0.19(4) 0.058(15) -0.009(17) -0.06(2) -0.11(4) C20 0.27(5) 0.35(6) 0.11(2) 0.01(3) -0.05(3) -0.19(5) C21 0.68(10) 0.09(2) 0.12(2) 0.039(18) -0.10(4) -0.12(4) C27' 0.086(12) 0.032(8) 0.050(8) 0.015(6) 0.004(8) -0.009(8) C29' 0.092(13) 0.038(8) 0.041(7) 0.006(6) 0.012(8) -0.015(9) C2' 0.069(10) 0.026(7) 0.047(7) -0.002(6) 0.003(7) 0.005(8) C3' 0.073(11) 0.011(6) 0.060(8) -0.002(6) 0.006(8) -0.011(7) C1' 0.049(9) 0.016(6) 0.028(5) 0.003(4) -0.002(6) -0.005(6) _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 N1 1.969(10) . ? Pt1 O1 1.994(10) 3_666 ? Pt1 O1 2.000(8) . ? Pt1 N2 2.010(9) . ? Pt1 Pt1 3.0511(10) 3_666 ? C11 N2 1.264(14) . ? C11 C9 1.485(15) . ? C11 C12 1.492(16) . ? Pt1' N2' 1.972(9) . ? Pt1' O1' 1.984(9) 3_565 ? Pt1' N1' 1.985(9) . ? Pt1' O1' 2.009(9) . ? Pt1' Pt1' 3.0268(9) 3_565 ? C10' C5' 1.391(14) . ? C10' C1' 1.419(15) . ? C10' C9' 1.429(15) . ? C9 C8 1.368(16) . ? C9 C10 1.385(18) . ? C31' C32' 1.524(19) . ? C31' C30' 1.528(19) . ? C31' C33' 1.537(16) . ? C31' H31' 1.0000 . ? C8 C7 1.419(18) . ? C8 H8 0.9500 . ? N2' C12' 1.297(13) . ? N2' C25' 1.450(13) . ? C35' C34' 1.546(19) . ? C35' H35A 0.9800 . ? C35' H35B 0.9800 . ? C35' H35C 0.9800 . ? O1' Pt1' 1.984(9) 3_565 ? C13' C18' 1.360(15) . ? C13' C14' 1.40(2) . ? C13' N1' 1.447(15) . ? N2 C25 1.440(16) . ? C10 C5 1.401(19) . ? C10 C1 1.407(19) . ? O1 Pt1 1.994(10) 3_666 ? N1' C11' 1.304(13) . ? C22' C14' 1.509(18) . ? C22' C24' 1.53(2) . ? C22' C23' 1.54(2) . ? C22' H22' 1.0000 . ? C12' C11' 1.459(16) . ? C12' C9' 1.465(14) . ? C14' C15' 1.40(2) . ? C18' C17' 1.414(19) . ? C18' C19' 1.54(2) . ? N1 C12 1.280(15) . ? N1 C13 1.440(15) . ? C8' C7' 1.388(16) . ? C8' C9' 1.399(15) . ? C8' H8' 0.9500 . ? F1 B1 1.358(18) . ? C34' C26' 1.520(18) . ? C34' C36' 1.53(2) . ? C34' H34' 1.0000 . ? C11' C1' 1.481(14) . ? C31 C30 1.49(3) . ? C31 C33 1.53(2) . ? C31 C32 1.56(2) . ? C31 H31 1.0000 . ? C33' H33A 0.9800 . ? C33' H33B 0.9800 . ? C33' H33C 0.9800 . ? F3 B1 1.37(2) . ? C25 C30 1.34(2) . ? C25 C26 1.45(2) . ? C17' C16' 1.35(2) . ? C17' H17' 0.9500 . ? C12 C1 1.51(2) . ? C25' C26' 1.388(18) . ? C25' C30' 1.403(17) . ? C28' C27' 1.36(2) . ? C28' C29' 1.36(2) . ? C28' H28' 0.9500 . ? C5 C4 1.39(2) . ? C5 C6 1.41(2) . ? C5' C6' 1.406(16) . ? C5' C4' 1.415(17) . ? C7 C6 1.38(2) . ? C7 H7 0.9500 . ? C15' C16' 1.40(2) . ? C15' H15' 0.9500 . ? C13 C14 1.33(3) . ? C13 C18 1.42(3) . ? C30' C29' 1.396(17) . ? C19' C21' 1.53(2) . ? C19' C20' 1.54(2) . ? C19' H19' 1.0000 . ? C26' C27' 1.395(16) . ? C30 C29 1.43(2) . ? F4 B1 1.34(2) . ? C16' H16' 0.9500 . ? C4' C3' 1.351(17) . ? C4' H4' 0.9500 . ? C7' C6' 1.370(17) . ? C7' H7' 0.9500 . ? C26 C27 1.34(2) . ? C26 C34 1.51(2) . ? C32' H32A 0.9800 . ? C32' H32B 0.9800 . ? C32' H32C 0.9800 . ? C1 C2 1.38(2) . ? C36' H36A 0.9800 . ? C36' H36B 0.9800 . ? C36' H36C 0.9800 . ? F2 B1 1.378(19) . ? C6 H6 0.9500 . ? C28 C29 1.38(3) . ? C28 C27 1.41(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C6' H6' 0.9500 . ? C34 C35 1.49(2) . ? C34 C36 1.60(3) . ? C34 H34 1.0000 . ? C22 C23 1.49(3) . ? C22 C24 1.52(3) . ? C22 C14 1.52(3) . ? C22 H22 1.0000 . ? C24' H24A 0.9800 . ? C24' H24B 0.9800 . ? C24' H24C 0.9800 . ? C20' H20A 0.9800 . ? C20' H20B 0.9800 . ? C20' H20C 0.9800 . ? C14 C15 1.45(3) . ? C36 H36D 0.9800 . ? C36 H36E 0.9800 . ? C36 H36F 0.9800 . ? C21' H21A 0.9800 . ? C21' H21B 0.9800 . ? C21' H21C 0.9800 . ? C15 C16 1.39(5) . ? C15 H15 0.9500 . ? C27 H27 0.9500 . ? C18 C17 1.39(2) . ? C18 C19 1.53(4) . ? C2 C3 1.41(3) . ? C2 H2 0.9500 . ? C23' H23A 0.9800 . ? C23' H23B 0.9800 . ? C23' H23C 0.9800 . ? C35 H35D 0.9800 . ? C35 H35E 0.9800 . ? C35 H35F 0.9800 . ? C33 H33D 0.9800 . ? C33 H33E 0.9800 . ? C33 H33F 0.9800 . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? C4 C3 1.37(3) . ? C4 H4 0.9500 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C17 C16 1.30(5) . ? C17 H17 0.9500 . ? C16 H16 0.9500 . ? C3 H3 0.9500 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C23 H23F 0.9800 . ? C19 C20 1.46(5) . ? C19 C21 1.58(4) . ? C19 H19 1.0000 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 H21D 0.9800 . ? C21 H21E 0.9800 . ? C21 H21F 0.9800 . ? C27' H27' 0.9500 . ? C29' H29' 0.9500 . ? C2' C1' 1.387(16) . ? C2' C3' 1.414(17) . ? C2' H2' 0.9500 . ? C3' H3' 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 O1 179.6(5) . 3_666 ? N1 Pt1 O1 99.5(4) . . ? O1 Pt1 O1 80.4(4) 3_666 . ? N1 Pt1 N2 80.6(4) . . ? O1 Pt1 N2 99.5(4) 3_666 . ? O1 Pt1 N2 179.9(4) . . ? N1 Pt1 Pt1 139.6(3) . 3_666 ? O1 Pt1 Pt1 40.3(2) 3_666 3_666 ? O1 Pt1 Pt1 40.1(3) . 3_666 ? N2 Pt1 Pt1 139.8(3) . 3_666 ? N2 C11 C9 138.8(10) . . ? N2 C11 C12 113.4(10) . . ? C9 C11 C12 107.7(10) . . ? N2' Pt1' O1' 178.5(5) . 3_565 ? N2' Pt1' N1' 81.4(4) . . ? O1' Pt1' N1' 97.9(4) 3_565 . ? N2' Pt1' O1' 99.4(4) . . ? O1' Pt1' O1' 81.4(4) 3_565 . ? N1' Pt1' O1' 178.0(5) . . ? N2' Pt1' Pt1' 139.8(2) . 3_565 ? O1' Pt1' Pt1' 41.0(3) 3_565 3_565 ? N1' Pt1' Pt1' 138.9(2) . 3_565 ? O1' Pt1' Pt1' 40.4(3) . 3_565 ? C5' C10' C1' 123.3(11) . . ? C5' C10' C9' 123.8(11) . . ? C1' C10' C9' 112.8(9) . . ? C8 C9 C10 121.8(12) . . ? C8 C9 C11 132.3(12) . . ? C10 C9 C11 105.6(10) . . ? C32' C31' C30' 110.9(11) . . ? C32' C31' C33' 110.8(12) . . ? C30' C31' C33' 113.2(12) . . ? C32' C31' H31' 107.2 . . ? C30' C31' H31' 107.2 . . ? C33' C31' H31' 107.2 . . ? C9 C8 C7 117.2(13) . . ? C9 C8 H8 121.4 . . ? C7 C8 H8 121.4 . . ? C12' N2' C25' 121.1(9) . . ? C12' N2' Pt1' 113.6(7) . . ? C25' N2' Pt1' 124.9(6) . . ? C34' C35' H35A 109.5 . . ? C34' C35' H35B 109.5 . . ? H35A C35' H35B 109.5 . . ? C34' C35' H35C 109.5 . . ? H35A C35' H35C 109.5 . . ? H35B C35' H35C 109.5 . . ? Pt1' O1' Pt1' 98.6(4) 3_565 . ? C18' C13' C14' 123.7(13) . . ? C18' C13' N1' 118.1(13) . . ? C14' C13' N1' 117.9(10) . . ? C11 N2 C25 120.6(10) . . ? C11 N2 Pt1 115.1(7) . . ? C25 N2 Pt1 124.2(8) . . ? C9 C10 C5 122.1(13) . . ? C9 C10 C1 115.5(13) . . ? C5 C10 C1 122.4(14) . . ? Pt1 O1 Pt1 99.6(4) 3_666 . ? C11' N1' C13' 125.5(10) . . ? C11' N1' Pt1' 113.3(8) . . ? C13' N1' Pt1' 120.8(7) . . ? C14' C22' C24' 108.7(11) . . ? C14' C22' C23' 114.6(13) . . ? C24' C22' C23' 109.9(15) . . ? C14' C22' H22' 107.8 . . ? C24' C22' H22' 107.8 . . ? C23' C22' H22' 107.8 . . ? N2' C12' C11' 115.7(10) . . ? N2' C12' C9' 136.7(11) . . ? C11' C12' C9' 107.0(9) . . ? C13' C14' C15' 116.9(13) . . ? C13' C14' C22' 124.6(13) . . ? C15' C14' C22' 118.4(16) . . ? C13' C18' C17' 117.6(15) . . ? C13' C18' C19' 123.1(12) . . ? C17' C18' C19' 119.3(12) . . ? C12 N1 C13 120.6(11) . . ? C12 N1 Pt1 113.7(8) . . ? C13 N1 Pt1 125.2(9) . . ? C7' C8' C9' 118.4(11) . . ? C7' C8' H8' 120.8 . . ? C9' C8' H8' 120.8 . . ? C26' C34' C36' 109.2(11) . . ? C26' C34' C35' 111.1(11) . . ? C36' C34' C35' 111.3(14) . . ? C26' C34' H34' 108.4 . . ? C36' C34' H34' 108.4 . . ? C35' C34' H34' 108.4 . . ? N1' C11' C12' 115.3(10) . . ? N1' C11' C1' 135.5(11) . . ? C12' C11' C1' 109.1(9) . . ? C30 C31 C33 113.0(18) . . ? C30 C31 C32 114.3(18) . . ? C33 C31 C32 109.8(16) . . ? C30 C31 H31 106.4 . . ? C33 C31 H31 106.4 . . ? C32 C31 H31 106.4 . . ? C31' C33' H33A 109.5 . . ? C31' C33' H33B 109.5 . . ? H33A C33' H33B 109.5 . . ? C31' C33' H33C 109.5 . . ? H33A C33' H33C 109.5 . . ? H33B C33' H33C 109.5 . . ? C8' C9' C10' 117.8(10) . . ? C8' C9' C12' 135.8(11) . . ? C10' C9' C12' 106.3(10) . . ? C30 C25 N2 117.1(16) . . ? C30 C25 C26 124.5(15) . . ? N2 C25 C26 118.4(14) . . ? C16' C17' C18' 120.6(14) . . ? C16' C17' H17' 119.7 . . ? C18' C17' H17' 119.7 . . ? N1 C12 C11 116.8(11) . . ? N1 C12 C1 136.8(12) . . ? C11 C12 C1 106.1(11) . . ? C26' C25' C30' 123.7(10) . . ? C26' C25' N2' 120.3(10) . . ? C30' C25' N2' 115.8(11) . . ? C27' C28' C29' 119.9(12) . . ? C27' C28' H28' 120.0 . . ? C29' C28' H28' 120.0 . . ? C4 C5 C10 117.3(16) . . ? C4 C5 C6 126.6(17) . . ? C10 C5 C6 116.0(15) . . ? C10' C5' C6' 115.7(11) . . ? C10' C5' C4' 114.5(10) . . ? C6' C5' C4' 129.7(11) . . ? C6 C7 C8 121.2(14) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C16' C15' C14' 119.8(17) . . ? C16' C15' H15' 120.1 . . ? C14' C15' H15' 120.1 . . ? C14 C13 C18 123.3(18) . . ? C14 C13 N1 120.5(19) . . ? C18 C13 N1 116.2(17) . . ? C29' C30' C25' 116.0(13) . . ? C29' C30' C31' 119.5(12) . . ? C25' C30' C31' 124.3(10) . . ? C21' C19' C20' 111.2(14) . . ? C21' C19' C18' 110.0(13) . . ? C20' C19' C18' 114.2(17) . . ? C21' C19' H19' 107.0 . . ? C20' C19' H19' 107.0 . . ? C18' C19' H19' 107.0 . . ? C25' C26' C27' 116.0(13) . . ? C25' C26' C34' 121.8(11) . . ? C27' C26' C34' 122.2(13) . . ? C25 C30 C29 119(2) . . ? C25 C30 C31 124.0(15) . . ? C29 C30 C31 117(2) . . ? C17' C16' C15' 121.1(15) . . ? C17' C16' H16' 119.4 . . ? C15' C16' H16' 119.4 . . ? C3' C4' C5' 123.6(11) . . ? C3' C4' H4' 118.2 . . ? C5' C4' H4' 118.2 . . ? C6' C7' C8' 122.8(11) . . ? C6' C7' H7' 118.6 . . ? C8' C7' H7' 118.6 . . ? C27 C26 C25 116.6(19) . . ? C27 C26 C34 122.5(19) . . ? C25 C26 C34 120.8(13) . . ? C31' C32' H32A 109.5 . . ? C31' C32' H32B 109.5 . . ? H32A C32' H32B 109.5 . . ? C31' C32' H32C 109.5 . . ? H32A C32' H32C 109.5 . . ? H32B C32' H32C 109.5 . . ? C2 C1 C10 120.1(16) . . ? C2 C1 C12 134.9(15) . . ? C10 C1 C12 105.0(13) . . ? C34' C36' H36A 109.5 . . ? C34' C36' H36B 109.5 . . ? H36A C36' H36B 109.5 . . ? C34' C36' H36C 109.5 . . ? H36A C36' H36C 109.5 . . ? H36B C36' H36C 109.5 . . ? C7 C6 C5 121.5(14) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C29 C28 C27 125.0(19) . . ? C29 C28 H28 117.5 . . ? C27 C28 H28 117.5 . . ? C28 C29 C30 116(2) . . ? C28 C29 H29 122.1 . . ? C30 C29 H29 122.1 . . ? C7' C6' C5' 121.5(11) . . ? C7' C6' H6' 119.3 . . ? C5' C6' H6' 119.3 . . ? C35 C34 C26 113.5(19) . . ? C35 C34 C36 110.7(18) . . ? C26 C34 C36 111.0(16) . . ? C35 C34 H34 107.1 . . ? C26 C34 H34 107.1 . . ? C36 C34 H34 107.1 . . ? C23 C22 C24 106(2) . . ? C23 C22 C14 115(3) . . ? C24 C22 C14 115(2) . . ? C23 C22 H22 106.8 . . ? C24 C22 H22 106.8 . . ? C14 C22 H22 106.8 . . ? C22' C24' H24A 109.5 . . ? C22' C24' H24B 109.5 . . ? H24A C24' H24B 109.5 . . ? C22' C24' H24C 109.5 . . ? H24A C24' H24C 109.5 . . ? H24B C24' H24C 109.5 . . ? C19' C20' H20A 109.5 . . ? C19' C20' H20B 109.5 . . ? H20A C20' H20B 109.5 . . ? C19' C20' H20C 109.5 . . ? H20A C20' H20C 109.5 . . ? H20B C20' H20C 109.5 . . ? C13 C14 C15 117(3) . . ? C13 C14 C22 121.9(18) . . ? C15 C14 C22 121(3) . . ? C34 C36 H36D 109.5 . . ? C34 C36 H36E 109.5 . . ? H36D C36 H36E 109.5 . . ? C34 C36 H36F 109.5 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? C19' C21' H21A 109.5 . . ? C19' C21' H21B 109.5 . . ? H21A C21' H21B 109.5 . . ? C19' C21' H21C 109.5 . . ? H21A C21' H21C 109.5 . . ? H21B C21' H21C 109.5 . . ? C16 C15 C14 119(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C26 C27 C28 119(2) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C17 C18 C13 116(3) . . ? C17 C18 C19 120(3) . . ? C13 C18 C19 122.4(17) . . ? C1 C2 C3 116(2) . . ? C1 C2 H2 121.8 . . ? C3 C2 H2 121.8 . . ? C22' C23' H23A 109.5 . . ? C22' C23' H23B 109.5 . . ? H23A C23' H23B 109.5 . . ? C22' C23' H23C 109.5 . . ? H23A C23' H23C 109.5 . . ? H23B C23' H23C 109.5 . . ? C34 C35 H35D 109.5 . . ? C34 C35 H35E 109.5 . . ? H35D C35 H35E 109.5 . . ? C34 C35 H35F 109.5 . . ? H35D C35 H35F 109.5 . . ? H35E C35 H35F 109.5 . . ? C31 C33 H33D 109.5 . . ? C31 C33 H33E 109.5 . . ? H33D C33 H33E 109.5 . . ? C31 C33 H33F 109.5 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? C31 C32 H32D 109.5 . . ? C31 C32 H32E 109.5 . . ? H32D C32 H32E 109.5 . . ? C31 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? F4 B1 F1 111.3(16) . . ? F4 B1 F3 109.3(13) . . ? F1 B1 F3 108.1(14) . . ? F4 B1 F2 108.6(14) . . ? F1 B1 F2 109.3(12) . . ? F3 B1 F2 110.3(16) . . ? C3 C4 C5 120.0(19) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C22 C24 H24D 109.5 . . ? C22 C24 H24E 109.5 . . ? H24D C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C16 C17 C18 122(3) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C16 C15 121(2) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C4 C3 C2 124(2) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C22 C23 H23D 109.5 . . ? C22 C23 H23E 109.5 . . ? H23D C23 H23E 109.5 . . ? C22 C23 H23F 109.5 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C20 C19 C18 115(3) . . ? C20 C19 C21 112(3) . . ? C18 C19 C21 106(4) . . ? C20 C19 H19 107.8 . . ? C18 C19 H19 107.8 . . ? C21 C19 H19 107.8 . . ? C19 C20 H20D 109.5 . . ? C19 C20 H20E 109.5 . . ? H20D C20 H20E 109.5 . . ? C19 C20 H20F 109.5 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? C19 C21 H21D 109.5 . . ? C19 C21 H21E 109.5 . . ? H21D C21 H21E 109.5 . . ? C19 C21 H21F 109.5 . . ? H21D C21 H21F 109.5 . . ? H21E C21 H21F 109.5 . . ? C28' C27' C26' 122.5(15) . . ? C28' C27' H27' 118.7 . . ? C26' C27' H27' 118.7 . . ? C28' C29' C30' 121.9(14) . . ? C28' C29' H29' 119.1 . . ? C30' C29' H29' 119.1 . . ? C1' C2' C3' 117.7(12) . . ? C1' C2' H2' 121.1 . . ? C3' C2' H2' 121.1 . . ? C4' C3' C2' 121.2(12) . . ? C4' C3' H3' 119.4 . . ? C2' C3' H3' 119.4 . . ? C2' C1' C10' 119.5(10) . . ? C2' C1' C11' 135.8(11) . . ? C10' C1' C11' 104.6(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.627 _refine_diff_density_min -2.377 _refine_diff_density_rms 0.195 data_OxoHydroxo_(6) _database_code_depnum_ccdc_archive 'CCDC 663519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C73 H83 N4 O2 Pt2 1+, C F3 O3 S 1-, C H2 Cl2, 0.5 (C7 H8)' _chemical_formula_sum 'C78.50 H89 Cl2 F3 N4 O5 Pt2 S' _chemical_formula_weight 1718.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.346(3) _cell_length_b 28.541(6) _cell_length_c 15.987(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.362(4) _cell_angle_gamma 90.00 _cell_volume 7359(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 844 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 18.50 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 3.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3830 _exptl_absorpt_correction_T_max 0.9615 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 67494 _diffrn_reflns_av_R_equivalents 0.2689 _diffrn_reflns_av_sigmaI/netI 0.2998 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.22 _reflns_number_total 16297 _reflns_number_gt 6309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The triflate anion is disordered and was modeled two sites differing by a slight rotation about a vector bisecting the C-S bond. Occupancy refinement indicated an even distribution between the two sites. Only the C and S atoms were refined anisotropically. The toluene molecule is disordered about an inversion center and was so modeled. ; _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^)+(0.1021P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00232(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16297 _refine_ls_number_parameters 821 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.2518 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2475 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.42447(4) 0.09928(2) 0.33699(4) 0.0311(2) Uani 1 1 d . . . Pt2 Pt 0.59121(4) 0.15042(2) 0.37384(4) 0.0301(2) Uani 1 1 d . . . N4 N 0.7045(8) 0.1406(4) 0.3496(8) 0.027(3) Uani 1 1 d . . . C32 C 0.5142(10) -0.0175(5) 0.3757(11) 0.038(4) Uani 1 1 d . . . H32 H 0.4847 0.0097 0.3964 0.045 Uiso 1 1 calc R . . C54 C 0.4956(15) 0.2996(7) 0.4757(16) 0.078(7) Uani 1 1 d . . . H54 H 0.4522 0.3193 0.4490 0.093 Uiso 1 1 calc R . . N2 N 0.3826(8) 0.0387(4) 0.2840(8) 0.033(3) Uani 1 1 d . . . C3 C 0.3077(9) 0.0288(5) 0.2929(10) 0.028(4) Uani 1 1 d . . . C67 C 0.7908(10) 0.0702(5) 0.3851(10) 0.031(4) Uani 1 1 d . . . C26 C 0.4293(11) 0.0085(5) 0.2378(11) 0.038(4) Uani 1 1 d . . . C44 C 0.8568(13) 0.3260(7) 0.4400(13) 0.060(6) Uani 1 1 d . . . H44 H 0.8600 0.3567 0.4635 0.072 Uiso 1 1 calc R . . C6 C 0.1079(12) -0.0661(6) 0.2320(12) 0.052(5) Uani 1 1 d . . . H6 H 0.0615 -0.0864 0.2204 0.062 Uiso 1 1 calc R . . O1 O 0.5420(6) 0.0922(4) 0.3285(7) 0.042(3) Uani 1 1 d . . . C51 C 0.6249(12) 0.2416(6) 0.5560(11) 0.048(5) Uani 1 1 d . . . C41 C 0.9691(12) 0.1955(8) 0.3018(14) 0.069(6) Uani 1 1 d . . . H41 H 1.0120 0.1809 0.2778 0.083 Uiso 1 1 calc R . . C12 C 0.1726(10) 0.0057(5) 0.2815(9) 0.033(4) Uani 1 1 d . . . C39 C 0.7516(9) 0.1772(4) 0.3604(9) 0.024(4) Uani 1 1 d . . . O2 O 0.4727(8) 0.1601(4) 0.3897(9) 0.054(4) Uani 1 1 d . . . N3 N 0.6437(8) 0.2105(4) 0.4176(8) 0.034(3) Uani 1 1 d . . . C70 C 0.7181(13) 0.1276(7) 0.1089(13) 0.068(6) Uani 1 1 d . . . H70A H 0.6845 0.1469 0.0658 0.102 Uiso 1 1 calc R . . H70B H 0.7393 0.1004 0.0818 0.102 Uiso 1 1 calc R . . H70C H 0.7647 0.1461 0.1380 0.102 Uiso 1 1 calc R . . C2 C 0.2626(10) 0.0665(6) 0.3228(10) 0.033(4) Uani 1 1 d . . . N1 N 0.3038(8) 0.1054(4) 0.3447(8) 0.033(3) Uani 1 1 d . . . C21 C 0.2789(14) 0.2014(9) 0.1519(19) 0.125(12) Uani 1 1 d . . . H21A H 0.3303 0.2134 0.1851 0.188 Uiso 1 1 calc R . . H21B H 0.2390 0.2271 0.1395 0.188 Uiso 1 1 calc R . . H21C H 0.2907 0.1880 0.0987 0.188 Uiso 1 1 calc R . . C25 C 0.2206(18) 0.1031(9) 0.5467(14) 0.123(13) Uani 1 1 d . . . H25A H 0.2431 0.0828 0.5944 0.184 Uiso 1 1 calc R . . H25B H 0.1927 0.0839 0.4998 0.184 Uiso 1 1 calc R . . H25C H 0.1807 0.1251 0.5647 0.184 Uiso 1 1 calc R . . C46 C 0.7792(10) 0.2547(5) 0.4120(10) 0.030(4) Uani 1 1 d . . . C73 C 0.7654(12) 0.0588(7) 0.5346(12) 0.061(6) Uani 1 1 d . . . H73A H 0.7808 0.0701 0.5930 0.092 Uiso 1 1 calc R . . H73B H 0.7791 0.0255 0.5321 0.092 Uiso 1 1 calc R . . H73C H 0.7057 0.0632 0.5162 0.092 Uiso 1 1 calc R . . C38 C 0.7188(11) 0.2179(5) 0.4004(10) 0.034(4) Uani 1 1 d . . . C71 C 0.8128(11) 0.0863(6) 0.4768(10) 0.038(4) Uani 1 1 d . . . H71 H 0.7983 0.1202 0.4800 0.046 Uiso 1 1 calc R . . C10 C 0.1746(10) 0.0527(5) 0.3173(10) 0.030(4) Uani 1 1 d . . . C13 C 0.0983(11) -0.0202(5) 0.2645(12) 0.041(5) Uani 1 1 d . . . C65 C 0.7961(11) 0.0106(6) 0.2811(12) 0.046(5) Uani 1 1 d . . . H65 H 0.8153 -0.0194 0.2670 0.055 Uiso 1 1 calc R . . C40 C 0.8962(10) 0.1686(7) 0.3074(12) 0.047(5) Uani 1 1 d . . . H40 H 0.8896 0.1375 0.2864 0.057 Uiso 1 1 calc R . . C62 C 0.7399(9) 0.0962(5) 0.3253(10) 0.028(4) Uani 1 1 d . . . C64 C 0.7474(11) 0.0358(5) 0.2209(10) 0.038(5) Uani 1 1 d . . . H64 H 0.7329 0.0235 0.1653 0.046 Uiso 1 1 calc R . . C34 C 0.4777(13) -0.0627(6) 0.4097(12) 0.059(6) Uani 1 1 d . . . H34A H 0.4894 -0.0627 0.4718 0.088 Uiso 1 1 calc R . . H34B H 0.5031 -0.0903 0.3880 0.088 Uiso 1 1 calc R . . H34C H 0.4176 -0.0634 0.3908 0.088 Uiso 1 1 calc R . . C23 C 0.2883(13) 0.1295(7) 0.5186(14) 0.060(6) Uiso 1 1 d . . . H23 H 0.3282 0.1065 0.5006 0.072 Uiso 1 1 calc R . . C9 C 0.1017(10) 0.0715(6) 0.3353(12) 0.044(5) Uani 1 1 d . . . H9 H 0.1006 0.1022 0.3580 0.053 Uiso 1 1 calc R . . C63 C 0.7180(10) 0.0804(5) 0.2403(11) 0.035(4) Uani 1 1 d . . . C8 C 0.0286(10) 0.0442(6) 0.3191(12) 0.047(5) Uani 1 1 d . . . H8 H -0.0217 0.0571 0.3314 0.056 Uiso 1 1 calc R . . C11 C 0.2493(9) -0.0098(5) 0.2640(10) 0.027(4) Uani 1 1 d . . . C4 C 0.2579(11) -0.0547(5) 0.2341(10) 0.042(5) Uani 1 1 d . . . H4 H 0.3099 -0.0670 0.2256 0.051 Uiso 1 1 calc R . . C56 C 0.6915(13) 0.2107(6) 0.6010(12) 0.055(5) Uani 1 1 d . . . H56 H 0.7340 0.2077 0.5628 0.066 Uiso 1 1 calc R . . C66 C 0.8179(10) 0.0270(6) 0.3608(13) 0.044(5) Uani 1 1 d . . . H66 H 0.8528 0.0084 0.4013 0.052 Uiso 1 1 calc R . . C47 C 0.8351(10) 0.1906(5) 0.3454(10) 0.030(4) Uani 1 1 d . . . C48 C 0.8464(10) 0.2366(5) 0.3760(11) 0.034(4) Uani 1 1 d . . . C31 C 0.4080(10) 0.0068(5) 0.1497(10) 0.032(4) Uani 1 1 d . . . C68 C 0.6639(13) 0.1107(6) 0.1741(11) 0.049(5) Uani 1 1 d . . . H68 H 0.6442 0.1386 0.2030 0.059 Uiso 1 1 calc R . . C19 C 0.2574(13) 0.1608(6) 0.4444(13) 0.062(6) Uani 1 1 d . . . C69 C 0.5878(11) 0.0826(6) 0.1302(12) 0.053(5) Uani 1 1 d . . . H69A H 0.5541 0.1025 0.0879 0.080 Uiso 1 1 calc R . . H69B H 0.5544 0.0726 0.1726 0.080 Uiso 1 1 calc R . . H69C H 0.6067 0.0551 0.1021 0.080 Uiso 1 1 calc R . . C29 C 0.5237(12) -0.0452(6) 0.1474(13) 0.053(5) Uani 1 1 d . . . H29 H 0.5565 -0.0638 0.1164 0.063 Uiso 1 1 calc R . . C30 C 0.4556(11) -0.0202(6) 0.1051(11) 0.043(5) Uani 1 1 d . . . H30 H 0.4423 -0.0218 0.0451 0.051 Uiso 1 1 calc R . . C15 C 0.2314(11) 0.1779(6) 0.2901(14) 0.049(5) Uani 1 1 d . . . C50 C 0.6035(11) 0.2445(5) 0.4682(11) 0.036(4) Uani 1 1 d . . . C42 C 0.9810(11) 0.2414(7) 0.3290(14) 0.058(6) Uani 1 1 d . . . H42 H 1.0292 0.2581 0.3206 0.070 Uiso 1 1 calc R . . C37 C 0.2885(14) 0.0095(8) 0.0266(15) 0.101(9) Uani 1 1 d . . . H37A H 0.2433 0.0292 -0.0019 0.151 Uiso 1 1 calc R . . H37B H 0.2653 -0.0191 0.0472 0.151 Uiso 1 1 calc R . . H37C H 0.3256 0.0012 -0.0135 0.151 Uiso 1 1 calc R . . C20 C 0.2421(14) 0.1631(8) 0.2031(17) 0.076(7) Uani 1 1 d . . . H20 H 0.2813 0.1359 0.2090 0.091 Uiso 1 1 calc R . . C52 C 0.5786(13) 0.2688(6) 0.6052(13) 0.055(6) Uani 1 1 d . . . H52 H 0.5913 0.2687 0.6653 0.066 Uiso 1 1 calc R . . C27 C 0.4959(11) -0.0168(5) 0.2814(11) 0.038(4) Uani 1 1 d . . . C7 C 0.0280(10) 0.0000(7) 0.2865(12) 0.049(5) Uani 1 1 d . . . H7 H -0.0222 -0.0174 0.2787 0.059 Uiso 1 1 calc R . . C35 C 0.3380(10) 0.0368(6) 0.1027(12) 0.048(5) Uani 1 1 d . . . H35 H 0.2990 0.0441 0.1431 0.058 Uiso 1 1 calc R . . C45 C 0.7852(12) 0.2992(5) 0.4423(11) 0.050(5) Uani 1 1 d . . . H45 H 0.7404 0.3123 0.4654 0.060 Uiso 1 1 calc R . . C57 C 0.6609(14) 0.1619(7) 0.6135(14) 0.081(7) Uani 1 1 d . . . H57A H 0.7068 0.1427 0.6423 0.121 Uiso 1 1 calc R . . H57B H 0.6393 0.1480 0.5583 0.121 Uiso 1 1 calc R . . H57C H 0.6167 0.1631 0.6482 0.121 Uiso 1 1 calc R . . C53 C 0.5134(16) 0.2958(8) 0.5630(17) 0.082(8) Uani 1 1 d . . . H53 H 0.4795 0.3123 0.5959 0.099 Uiso 1 1 calc R . . C72 C 0.9074(11) 0.0799(8) 0.5125(13) 0.069(6) Uani 1 1 d . . . H72A H 0.9186 0.0907 0.5715 0.103 Uiso 1 1 calc R . . H72B H 0.9404 0.0983 0.4784 0.103 Uiso 1 1 calc R . . H72C H 0.9223 0.0468 0.5101 0.103 Uiso 1 1 calc R . . C58 C 0.7363(15) 0.2301(8) 0.6839(13) 0.086(8) Uani 1 1 d . . . H58A H 0.7790 0.2078 0.7090 0.128 Uiso 1 1 calc R . . H58B H 0.6966 0.2350 0.7229 0.128 Uiso 1 1 calc R . . H58C H 0.7624 0.2600 0.6736 0.128 Uiso 1 1 calc R . . C14 C 0.2619(10) 0.1481(5) 0.3616(12) 0.036(4) Uani 1 1 d . . . C55 C 0.5439(14) 0.2734(7) 0.4284(14) 0.067(6) Uani 1 1 d . . . C1 C 0.448(2) 0.1760(13) 0.466(3) 0.20(2) Uani 1 1 d . . . H1A H 0.4914 0.1957 0.4975 0.298 Uiso 1 1 calc R . . H1B H 0.4380 0.1490 0.5012 0.298 Uiso 1 1 calc R . . H1C H 0.3965 0.1943 0.4527 0.298 Uiso 1 1 calc R . . C49 C 0.9206(11) 0.2625(6) 0.3693(13) 0.050(5) Uani 1 1 d . . . C5 C 0.1845(13) -0.0809(6) 0.2173(12) 0.055(6) Uani 1 1 d . . . H5 H 0.1879 -0.1113 0.1939 0.066 Uiso 1 1 calc R . . C28 C 0.5427(11) -0.0426(5) 0.2341(11) 0.038(4) Uani 1 1 d . . . H28 H 0.5896 -0.0591 0.2623 0.046 Uiso 1 1 calc R . . C36 C 0.3678(12) 0.0827(6) 0.0716(12) 0.058(6) Uani 1 1 d . . . H36A H 0.3202 0.1006 0.0429 0.087 Uiso 1 1 calc R . . H36B H 0.4062 0.0765 0.0318 0.087 Uiso 1 1 calc R . . H36C H 0.3962 0.1007 0.1199 0.087 Uiso 1 1 calc R . . C43 C 0.9243(13) 0.3090(6) 0.4039(13) 0.061(6) Uani 1 1 d . . . H43 H 0.9716 0.3281 0.4025 0.073 Uiso 1 1 calc R . . C17 C 0.1926(14) 0.2324(6) 0.3917(16) 0.073(8) Uani 1 1 d . . . H17 H 0.1659 0.2608 0.4030 0.088 Uiso 1 1 calc R . . C33 C 0.6074(11) -0.0121(7) 0.4118(13) 0.066(6) Uani 1 1 d . . . H33A H 0.6151 -0.0124 0.4739 0.099 Uiso 1 1 calc R . . H33B H 0.6277 0.0177 0.3925 0.099 Uiso 1 1 calc R . . H33C H 0.6384 -0.0380 0.3919 0.099 Uiso 1 1 calc R . . C22 C 0.1610(17) 0.1465(9) 0.1542(14) 0.103(9) Uani 1 1 d . . . H22A H 0.1691 0.1363 0.0976 0.154 Uiso 1 1 calc R . . H22B H 0.1207 0.1722 0.1489 0.154 Uiso 1 1 calc R . . H22C H 0.1402 0.1203 0.1841 0.154 Uiso 1 1 calc R . . C18 C 0.2248(18) 0.2039(8) 0.4557(17) 0.116(11) Uani 1 1 d . . . H18 H 0.2248 0.2143 0.5121 0.139 Uiso 1 1 calc R . . C59 C 0.5267(18) 0.2801(9) 0.3327(16) 0.097(9) Uani 1 1 d . . . H59 H 0.5629 0.2573 0.3084 0.116 Uiso 1 1 calc R . . C16 C 0.1987(11) 0.2202(6) 0.3106(17) 0.067(7) Uani 1 1 d . . . H16 H 0.1797 0.2417 0.2663 0.080 Uiso 1 1 calc R . . C24 C 0.333(2) 0.1566(9) 0.5961(14) 0.159(17) Uani 1 1 d . . . H24A H 0.3800 0.1740 0.5799 0.238 Uiso 1 1 calc R . . H24B H 0.3539 0.1345 0.6415 0.238 Uiso 1 1 calc R . . H24C H 0.2946 0.1785 0.6161 0.238 Uiso 1 1 calc R . . C61 C 0.5519(19) 0.3298(9) 0.3055(16) 0.122(12) Uani 1 1 d . . . H61A H 0.5414 0.3322 0.2436 0.184 Uiso 1 1 calc R . . H61B H 0.6110 0.3350 0.3263 0.184 Uiso 1 1 calc R . . H61C H 0.5193 0.3535 0.3297 0.184 Uiso 1 1 calc R . . C60 C 0.436(2) 0.2689(11) 0.2914(17) 0.154(15) Uani 1 1 d . . . H60A H 0.4298 0.2730 0.2299 0.232 Uiso 1 1 calc R . . H60B H 0.3978 0.2902 0.3142 0.232 Uiso 1 1 calc R . . H60C H 0.4226 0.2365 0.3042 0.232 Uiso 1 1 calc R . . Cl1 Cl -0.0857(5) 0.3036(4) 0.1094(7) 0.174(4) Uani 1 1 d . . . Cl2 Cl 0.0496(9) 0.2518(6) 0.0750(8) 0.267(8) Uani 1 1 d . . . C1S C 0.0145(17) 0.3039(9) 0.067(3) 0.174(19) Uani 1 1 d . . . H1S1 H 0.0053 0.3141 0.0070 0.209 Uiso 1 1 calc R . . H1S2 H 0.0543 0.3258 0.1002 0.209 Uiso 1 1 calc R . . C2S C 0.016(3) 0.5141(14) 0.472(3) 0.103(19) Uiso 0.50 1 d PD A 3 C3S C 0.043(8) 0.4692(18) 0.459(7) 0.17(5) Uiso 0.50 1 d PD A 3 H3S H 0.0768 0.4635 0.4177 0.200 Uiso 0.50 1 calc PR A 3 C4S C 0.020(3) 0.4328(12) 0.507(3) 0.076(14) Uiso 0.50 1 d PD A 3 H4S H 0.0414 0.4022 0.5014 0.092 Uiso 0.50 1 calc PR A 3 C5S C -0.034(4) 0.4408(14) 0.563(4) 0.12(3) Uiso 0.50 1 d PD A 3 H5S H -0.0531 0.4153 0.5929 0.144 Uiso 0.50 1 calc PR A 3 C6S C -0.061(3) 0.4857(17) 0.576(3) 0.12(2) Uiso 0.50 1 d PD A 3 H6S H -0.0996 0.4910 0.6131 0.145 Uiso 0.50 1 calc PR A 3 C7S C -0.030(7) 0.5227(15) 0.535(7) 0.16(5) Uiso 0.50 1 d PD A 3 H7S H -0.0415 0.5540 0.5498 0.188 Uiso 0.50 1 calc PR A 3 C8S C 0.064(6) 0.557(3) 0.415(7) 0.21(4) Uiso 0.50 1 d P A 3 H8S1 H 0.0419 0.5885 0.4255 0.310 Uiso 0.50 1 calc PR A 3 H8S2 H 0.0517 0.5506 0.3540 0.310 Uiso 0.50 1 calc PR A 3 H8S3 H 0.1239 0.5570 0.4338 0.310 Uiso 0.50 1 calc PR A 3 S1 S 0.1304(6) 0.3647(4) 0.2832(8) 0.047(4) Uani 0.505(16) 1 d PG B 1 O3 O 0.0867(8) 0.3523(6) 0.3520(10) 0.089(11) Uiso 0.505(16) 1 d PG B 1 O4 O 0.1426(9) 0.3255(5) 0.2290(9) 0.060(8) Uiso 0.505(16) 1 d PG B 1 O5 O 0.0973(8) 0.4060(5) 0.2369(12) 0.18(3) Uiso 0.505(16) 1 d PG B 1 F1 F 0.2783(7) 0.3931(5) 0.2762(10) 0.052(6) Uiso 0.505(16) 1 d PG B 1 F2 F 0.2288(10) 0.4169(5) 0.3851(10) 0.094(9) Uiso 0.505(16) 1 d PG B 1 F3 F 0.2688(8) 0.3456(6) 0.3781(10) 0.087(12) Uiso 0.505(16) 1 d PG B 1 C1T C 0.2320(6) 0.3809(4) 0.3333(7) 0.057(13) Uiso 0.505(16) 1 d PG B 1 S1' S 0.1296(9) 0.3778(6) 0.3172(11) 0.156(13) Uani 0.495(16) 1 d PG B 2 O3' O 0.0932(12) 0.3314(8) 0.3160(18) 0.124(15) Uiso 0.495(16) 1 d PG B 2 O4' O 0.1081(10) 0.4029(7) 0.2378(12) 0.034(8) Uiso 0.495(16) 1 d PG B 2 O5' O 0.1182(15) 0.4053(10) 0.3907(13) 0.42(7) Uiso 0.495(16) 1 d PG B 2 F1' F 0.2790(10) 0.4084(8) 0.3303(18) 0.152(15) Uiso 0.495(16) 1 d PG B 2 F2' F 0.2658(14) 0.3452(9) 0.3995(16) 0.16(2) Uiso 0.495(16) 1 d PG B 2 F3' F 0.2569(12) 0.3431(9) 0.2642(17) 0.168(17) Uiso 0.495(16) 1 d PG B 2 C1T' C 0.2386(9) 0.3681(7) 0.3284(13) 0.12(3) Uiso 0.495(16) 1 d PG 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 Pt1 0.0278(4) 0.0337(4) 0.0327(4) -0.0021(3) 0.0077(3) -0.0031(3) Pt2 0.0281(4) 0.0326(4) 0.0312(4) -0.0047(3) 0.0097(3) -0.0009(3) N4 0.039(8) 0.016(6) 0.029(8) -0.010(5) 0.012(6) -0.003(6) C32 0.036(10) 0.026(9) 0.053(13) 0.010(8) 0.013(9) -0.006(8) C54 0.099(19) 0.062(14) 0.09(2) 0.002(13) 0.060(16) 0.029(13) N2 0.046(9) 0.022(7) 0.035(9) -0.006(6) 0.017(7) 0.003(6) C3 0.020(9) 0.031(9) 0.033(10) 0.003(7) 0.006(7) 0.008(7) C67 0.041(10) 0.018(8) 0.041(11) 0.000(7) 0.031(9) 0.010(7) C26 0.051(12) 0.029(9) 0.033(11) -0.006(8) 0.006(9) -0.010(8) C44 0.076(16) 0.040(11) 0.069(16) -0.004(10) 0.023(13) -0.027(11) C6 0.036(11) 0.047(11) 0.068(15) -0.008(10) -0.009(10) -0.016(9) O1 0.033(6) 0.047(7) 0.051(8) -0.012(6) 0.020(6) -0.014(6) C51 0.064(13) 0.052(11) 0.027(11) -0.020(9) 0.004(10) 0.009(10) C41 0.046(13) 0.078(16) 0.087(18) -0.006(13) 0.024(12) -0.009(12) C12 0.046(11) 0.041(10) 0.013(9) -0.004(7) 0.008(8) -0.016(8) C39 0.039(10) 0.011(7) 0.023(9) 0.000(6) 0.005(7) 0.002(7) O2 0.045(8) 0.064(9) 0.059(10) -0.021(7) 0.023(7) -0.008(7) N3 0.040(9) 0.038(8) 0.029(8) 0.002(6) 0.017(7) 0.012(7) C70 0.070(15) 0.067(14) 0.067(16) 0.018(12) 0.008(13) -0.001(12) C2 0.028(9) 0.044(10) 0.028(10) 0.026(8) 0.003(8) 0.004(8) N1 0.026(7) 0.030(7) 0.043(9) 0.001(6) 0.012(7) -0.011(6) C21 0.056(16) 0.16(3) 0.17(3) 0.11(2) 0.027(17) -0.009(17) C25 0.18(3) 0.14(2) 0.037(14) 0.007(15) -0.008(17) 0.13(2) C46 0.039(10) 0.029(8) 0.022(9) -0.003(7) 0.008(8) 0.010(8) C73 0.074(15) 0.073(14) 0.039(13) 0.021(11) 0.017(11) -0.003(12) C38 0.051(12) 0.032(9) 0.018(9) -0.007(7) -0.002(8) -0.013(8) C71 0.059(12) 0.037(9) 0.016(9) 0.004(7) -0.002(9) 0.000(8) C10 0.032(9) 0.030(8) 0.029(10) -0.001(7) 0.012(8) 0.003(7) C13 0.043(11) 0.016(8) 0.061(13) 0.002(8) -0.002(10) -0.001(8) C65 0.053(12) 0.032(10) 0.053(14) 0.006(9) 0.013(11) 0.002(9) C40 0.032(10) 0.054(11) 0.061(14) -0.006(10) 0.021(10) 0.003(9) C62 0.027(9) 0.028(8) 0.031(10) -0.001(7) 0.008(7) 0.002(7) C64 0.081(14) 0.017(8) 0.021(10) -0.002(7) 0.019(9) 0.005(8) C34 0.084(16) 0.038(11) 0.055(14) 0.013(9) 0.014(12) -0.015(10) C9 0.029(10) 0.040(10) 0.065(14) 0.001(9) 0.011(9) -0.002(8) C63 0.032(10) 0.027(8) 0.048(12) 0.026(8) 0.015(9) -0.003(7) C8 0.018(9) 0.058(12) 0.065(14) 0.002(10) 0.008(9) 0.010(9) C11 0.029(9) 0.022(8) 0.031(10) -0.004(7) 0.013(8) -0.003(7) C4 0.056(12) 0.035(10) 0.035(11) -0.006(8) 0.003(9) -0.004(9) C56 0.079(15) 0.035(10) 0.049(13) -0.006(9) 0.003(11) -0.005(10) C66 0.028(10) 0.039(10) 0.064(15) 0.021(9) 0.009(10) -0.001(8) C47 0.040(10) 0.021(8) 0.030(10) -0.001(7) 0.013(8) -0.008(7) C48 0.027(9) 0.037(9) 0.039(11) 0.013(8) 0.005(8) -0.008(8) C31 0.035(10) 0.039(9) 0.023(10) -0.006(7) 0.009(8) -0.005(8) C68 0.094(16) 0.034(10) 0.030(11) 0.008(8) 0.039(11) 0.002(10) C19 0.086(16) 0.040(11) 0.055(14) -0.019(9) -0.006(12) 0.038(11) C69 0.057(13) 0.058(12) 0.044(13) -0.004(10) 0.005(10) -0.011(10) C29 0.058(13) 0.053(12) 0.052(14) -0.010(10) 0.021(11) 0.008(10) C30 0.062(13) 0.049(11) 0.018(10) -0.021(8) 0.008(9) -0.002(10) C15 0.043(12) 0.025(9) 0.081(16) 0.009(10) 0.018(11) 0.012(8) C50 0.047(11) 0.025(8) 0.038(11) -0.011(8) 0.017(9) -0.002(8) C42 0.035(11) 0.047(12) 0.099(19) 0.001(11) 0.029(12) -0.008(9) C37 0.084(19) 0.101(19) 0.10(2) -0.041(16) -0.042(16) 0.000(15) C20 0.065(16) 0.069(15) 0.10(2) 0.035(14) 0.035(15) 0.036(13) C52 0.087(16) 0.045(11) 0.038(12) -0.016(9) 0.028(12) 0.007(11) C27 0.045(11) 0.032(9) 0.041(12) -0.015(8) 0.024(9) -0.007(8) C7 0.023(10) 0.061(12) 0.062(14) -0.005(10) 0.002(9) -0.006(9) C35 0.029(10) 0.068(13) 0.048(13) -0.005(10) 0.007(9) -0.002(9) C45 0.079(15) 0.024(9) 0.051(13) -0.011(8) 0.027(11) -0.005(9) C57 0.082(17) 0.088(17) 0.066(17) 0.003(13) -0.009(14) 0.008(14) C53 0.10(2) 0.078(16) 0.08(2) 0.000(15) 0.072(17) 0.010(15) C72 0.040(12) 0.104(17) 0.053(15) -0.019(12) -0.017(11) 0.000(12) C58 0.10(2) 0.100(18) 0.051(16) -0.023(13) 0.006(14) -0.035(16) C14 0.031(9) 0.021(8) 0.055(12) 0.008(8) 0.001(9) 0.005(7) C55 0.082(16) 0.055(13) 0.069(17) 0.005(11) 0.029(13) 0.034(12) C1 0.15(4) 0.21(4) 0.24(5) 0.12(4) 0.03(3) 0.07(3) C49 0.042(12) 0.041(11) 0.067(14) 0.023(10) 0.010(10) -0.017(9) C5 0.073(15) 0.032(10) 0.055(14) -0.008(9) -0.002(12) -0.023(10) C28 0.049(11) 0.029(9) 0.042(12) -0.002(8) 0.022(9) 0.003(8) C36 0.065(14) 0.053(12) 0.055(14) -0.004(10) 0.003(11) -0.017(11) C43 0.071(15) 0.031(10) 0.081(17) 0.000(10) 0.016(13) -0.018(10) C17 0.101(19) 0.030(11) 0.077(18) -0.019(11) -0.021(15) 0.032(11) C33 0.040(12) 0.075(14) 0.074(16) -0.011(12) -0.021(11) 0.002(11) C22 0.14(3) 0.13(2) 0.038(15) 0.005(15) 0.027(16) -0.04(2) C18 0.17(3) 0.078(17) 0.08(2) -0.039(15) -0.036(19) 0.063(19) C59 0.13(2) 0.12(2) 0.053(17) 0.021(15) 0.041(17) 0.073(19) C16 0.032(12) 0.039(11) 0.12(2) 0.019(13) -0.006(13) 0.004(9) C24 0.30(4) 0.11(2) 0.034(15) -0.044(14) -0.08(2) 0.10(3) C61 0.18(3) 0.12(2) 0.08(2) 0.057(18) 0.05(2) 0.05(2) C60 0.21(4) 0.19(3) 0.046(19) 0.001(19) -0.04(2) 0.08(3) Cl1 0.093(6) 0.221(11) 0.209(11) 0.077(9) 0.030(7) -0.009(7) Cl2 0.250(15) 0.373(19) 0.148(11) -0.016(12) -0.056(10) 0.144(15) C1S 0.08(2) 0.063(18) 0.36(6) 0.03(3) -0.03(3) 0.004(17) S1 0.027(6) 0.038(6) 0.077(9) 0.030(6) 0.014(5) 0.005(4) S1' 0.101(16) 0.079(14) 0.32(4) 0.03(2) 0.11(2) 0.014(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 O1 1.959(10) . ? Pt1 N2 1.995(12) . ? Pt1 N1 2.003(12) . ? Pt1 O2 2.032(12) . ? Pt1 Pt2 3.0633(10) . ? Pt2 O1 1.936(10) . ? Pt2 N4 1.972(12) . ? Pt2 N3 1.993(13) . ? Pt2 O2 2.013(12) . ? N4 C39 1.293(16) . ? N4 C62 1.471(17) . ? C32 C27 1.49(2) . ? C32 C33 1.55(2) . ? C32 C34 1.55(2) . ? C54 C53 1.38(3) . ? C54 C55 1.40(3) . ? N2 C3 1.287(18) . ? N2 C26 1.435(19) . ? C3 C2 1.43(2) . ? C3 C11 1.48(2) . ? C67 C62 1.38(2) . ? C67 C66 1.39(2) . ? C67 C71 1.52(2) . ? C26 C27 1.39(2) . ? C26 C31 1.39(2) . ? C44 C45 1.40(2) . ? C44 C43 1.41(3) . ? C6 C5 1.38(2) . ? C6 C13 1.43(2) . ? C51 C50 1.39(2) . ? C51 C52 1.41(2) . ? C51 C56 1.49(2) . ? C41 C42 1.38(3) . ? C41 C40 1.43(2) . ? C12 C11 1.40(2) . ? C12 C13 1.41(2) . ? C12 C10 1.46(2) . ? C39 C38 1.47(2) . ? C39 C47 1.47(2) . ? O2 C1 1.43(4) . ? N3 C38 1.318(19) . ? N3 C50 1.483(18) . ? C70 C68 1.55(2) . ? C2 N1 1.316(19) . ? C2 C10 1.48(2) . ? N1 C14 1.445(18) . ? C21 C20 1.54(3) . ? C25 C23 1.47(3) . ? C46 C45 1.36(2) . ? C46 C48 1.42(2) . ? C46 C38 1.43(2) . ? C73 C71 1.52(2) . ? C71 C72 1.57(2) . ? C10 C9 1.38(2) . ? C13 C7 1.38(2) . ? C65 C66 1.35(2) . ? C65 C64 1.35(2) . ? C40 C47 1.40(2) . ? C62 C63 1.42(2) . ? C64 C63 1.41(2) . ? C23 C19 1.50(3) . ? C23 C24 1.54(3) . ? C9 C8 1.41(2) . ? C63 C68 1.53(2) . ? C8 C7 1.37(2) . ? C11 C4 1.38(2) . ? C4 C5 1.40(2) . ? C56 C57 1.50(2) . ? C56 C58 1.51(2) . ? C47 C48 1.40(2) . ? C48 C49 1.44(2) . ? C31 C30 1.38(2) . ? C31 C35 1.52(2) . ? C68 C69 1.55(2) . ? C19 C18 1.36(2) . ? C19 C14 1.39(2) . ? C29 C28 1.37(2) . ? C29 C30 1.40(2) . ? C15 C16 1.38(2) . ? C15 C14 1.45(2) . ? C15 C20 1.49(3) . ? C50 C55 1.35(2) . ? C42 C49 1.40(2) . ? C37 C35 1.56(2) . ? C20 C22 1.50(3) . ? C52 C53 1.40(3) . ? C27 C28 1.37(2) . ? C35 C36 1.51(2) . ? C55 C59 1.52(3) . ? C49 C43 1.43(2) . ? C17 C18 1.35(3) . ? C17 C16 1.36(3) . ? C59 C60 1.56(4) . ? C59 C61 1.56(3) . ? Cl1 C1S 1.87(3) . ? Cl2 C1S 1.59(3) . ? C2S C7S 1.38(3) . ? C2S C3S 1.38(3) . ? C2S C8S 1.79(10) . ? C3S C4S 1.38(3) . ? C4S C5S 1.37(3) . ? C5S C6S 1.38(3) . ? C6S C7S 1.38(3) . ? S1 O3 1.4497 . ? S1 O5 1.4497 . ? S1 O4 1.4507 . ? S1 C1T 1.7840 . ? F1 C1T 1.3242 . ? F2 C1T 1.3252 . ? F3 C1T 1.3238 . ? S1' O3' 1.4498 . ? S1' O4' 1.4499 . ? S1' O5' 1.4499 . ? S1' C1T' 1.7840 . ? F1' C1T' 1.3240 . ? F2' C1T' 1.3243 . ? F3' C1T' 1.3246 . ? 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 O1 Pt1 N2 98.8(5) . . ? O1 Pt1 N1 179.0(5) . . ? N2 Pt1 N1 80.1(5) . . ? O1 Pt1 O2 78.4(5) . . ? N2 Pt1 O2 177.2(5) . . ? N1 Pt1 O2 102.7(5) . . ? O1 Pt1 Pt2 37.9(3) . . ? N2 Pt1 Pt2 136.6(4) . . ? N1 Pt1 Pt2 143.2(4) . . ? O2 Pt1 Pt2 40.5(4) . . ? O1 Pt2 N4 98.6(4) . . ? O1 Pt2 N3 178.3(5) . . ? N4 Pt2 N3 80.1(5) . . ? O1 Pt2 O2 79.4(5) . . ? N4 Pt2 O2 176.0(5) . . ? N3 Pt2 O2 101.9(5) . . ? O1 Pt2 Pt1 38.4(3) . . ? N4 Pt2 Pt1 136.8(3) . . ? N3 Pt2 Pt1 142.8(4) . . ? O2 Pt2 Pt1 41.0(3) . . ? C39 N4 C62 118.6(12) . . ? C39 N4 Pt2 114.6(9) . . ? C62 N4 Pt2 126.7(9) . . ? C27 C32 C33 113.6(15) . . ? C27 C32 C34 109.9(14) . . ? C33 C32 C34 111.3(15) . . ? C53 C54 C55 117(2) . . ? C3 N2 C26 121.3(13) . . ? C3 N2 Pt1 114.3(10) . . ? C26 N2 Pt1 124.4(10) . . ? N2 C3 C2 115.0(14) . . ? N2 C3 C11 134.9(14) . . ? C2 C3 C11 108.8(13) . . ? C62 C67 C66 118.0(16) . . ? C62 C67 C71 121.9(13) . . ? C66 C67 C71 120.0(15) . . ? C27 C26 C31 122.3(16) . . ? C27 C26 N2 119.4(15) . . ? C31 C26 N2 118.3(15) . . ? C45 C44 C43 122.2(17) . . ? C5 C6 C13 120.1(16) . . ? Pt2 O1 Pt1 103.7(5) . . ? C50 C51 C52 117.3(17) . . ? C50 C51 C56 124.5(16) . . ? C52 C51 C56 118.2(18) . . ? C42 C41 C40 124.3(19) . . ? C11 C12 C13 124.5(14) . . ? C11 C12 C10 114.1(14) . . ? C13 C12 C10 121.5(15) . . ? N4 C39 C38 116.5(14) . . ? N4 C39 C47 137.4(13) . . ? C38 C39 C47 106.1(12) . . ? C1 O2 Pt2 124.6(18) . . ? C1 O2 Pt1 118.8(18) . . ? Pt2 O2 Pt1 98.5(5) . . ? C38 N3 C50 121.3(13) . . ? C38 N3 Pt2 115.2(10) . . ? C50 N3 Pt2 123.5(10) . . ? N1 C2 C3 116.9(14) . . ? N1 C2 C10 133.8(15) . . ? C3 C2 C10 109.1(14) . . ? C2 N1 C14 121.5(13) . . ? C2 N1 Pt1 112.2(10) . . ? C14 N1 Pt1 126.0(9) . . ? C45 C46 C48 118.1(16) . . ? C45 C46 C38 137.8(16) . . ? C48 C46 C38 104.0(13) . . ? N3 C38 C46 137.4(15) . . ? N3 C38 C39 112.5(13) . . ? C46 C38 C39 110.1(14) . . ? C73 C71 C67 111.6(14) . . ? C73 C71 C72 106.8(15) . . ? C67 C71 C72 112.4(14) . . ? C9 C10 C12 118.4(15) . . ? C9 C10 C2 138.4(15) . . ? C12 C10 C2 103.2(13) . . ? C7 C13 C12 117.2(15) . . ? C7 C13 C6 128.5(17) . . ? C12 C13 C6 114.1(16) . . ? C66 C65 C64 121.4(17) . . ? C47 C40 C41 116.5(17) . . ? C67 C62 C63 121.5(14) . . ? C67 C62 N4 120.0(14) . . ? C63 C62 N4 118.5(13) . . ? C65 C64 C63 120.4(16) . . ? C25 C23 C19 111.9(18) . . ? C25 C23 C24 107(2) . . ? C19 C23 C24 113.0(18) . . ? C10 C9 C8 118.7(16) . . ? C64 C63 C62 117.0(14) . . ? C64 C63 C68 122.4(16) . . ? C62 C63 C68 120.6(14) . . ? C7 C8 C9 122.1(16) . . ? C4 C11 C12 120.5(15) . . ? C4 C11 C3 134.5(15) . . ? C12 C11 C3 104.7(12) . . ? C11 C4 C5 115.4(17) . . ? C51 C56 C57 112.3(17) . . ? C51 C56 C58 114.7(16) . . ? C57 C56 C58 110.3(18) . . ? C65 C66 C67 121.6(17) . . ? C40 C47 C48 120.5(15) . . ? C40 C47 C39 134.3(14) . . ? C48 C47 C39 105.1(13) . . ? C47 C48 C46 114.6(14) . . ? C47 C48 C49 121.4(16) . . ? C46 C48 C49 124.0(15) . . ? C30 C31 C26 118.2(16) . . ? C30 C31 C35 120.1(16) . . ? C26 C31 C35 121.5(15) . . ? C63 C68 C69 110.7(13) . . ? C63 C68 C70 108.1(15) . . ? C69 C68 C70 111.1(15) . . ? C18 C19 C14 116.3(19) . . ? C18 C19 C23 121(2) . . ? C14 C19 C23 122.4(16) . . ? C28 C29 C30 119.4(17) . . ? C31 C30 C29 120.5(16) . . ? C16 C15 C14 115(2) . . ? C16 C15 C20 125.3(19) . . ? C14 C15 C20 119.6(15) . . ? C55 C50 C51 123.7(17) . . ? C55 C50 N3 119.4(16) . . ? C51 C50 N3 116.7(15) . . ? C41 C42 C49 118.6(17) . . ? C15 C20 C22 110.3(18) . . ? C15 C20 C21 114(2) . . ? C22 C20 C21 109(2) . . ? C53 C52 C51 118.1(19) . . ? C28 C27 C26 117.5(17) . . ? C28 C27 C32 120.8(17) . . ? C26 C27 C32 121.7(15) . . ? C8 C7 C13 122.0(16) . . ? C36 C35 C31 113.1(14) . . ? C36 C35 C37 109.3(17) . . ? C31 C35 C37 111.0(16) . . ? C46 C45 C44 120.8(18) . . ? C54 C53 C52 123(2) . . ? C19 C14 N1 119.9(14) . . ? C19 C14 C15 122.5(16) . . ? N1 C14 C15 117.4(16) . . ? C50 C55 C54 120(2) . . ? C50 C55 C59 123.4(18) . . ? C54 C55 C59 117(2) . . ? C42 C49 C43 126.0(17) . . ? C42 C49 C48 118.5(17) . . ? C43 C49 C48 115.5(18) . . ? C6 C5 C4 125.2(17) . . ? C27 C28 C29 122.1(18) . . ? C44 C43 C49 119.4(18) . . ? C18 C17 C16 119(2) . . ? C17 C18 C19 124(2) . . ? C55 C59 C60 114(2) . . ? C55 C59 C61 112(2) . . ? C60 C59 C61 110(2) . . ? C17 C16 C15 123(2) . . ? Cl2 C1S Cl1 106.9(18) . . ? C7S C2S C3S 120.0(13) . . ? C7S C2S C8S 126(4) . . ? C3S C2S C8S 113(4) . . ? C2S C3S C4S 119.9(11) . . ? C5S C4S C3S 119.8(11) . . ? C4S C5S C6S 120.2(11) . . ? C5S C6S C7S 119.6(12) . . ? C2S C7S C6S 119.6(15) . . ? O3 S1 O5 113.5 . . ? O3 S1 O4 113.4 . . ? O5 S1 O4 113.5 . . ? O3 S1 C1T 105.1 . . ? O5 S1 C1T 105.1 . . ? O4 S1 C1T 105.1 . . ? F3 C1T F1 108.3 . . ? F3 C1T F2 108.2 . . ? F1 C1T F2 108.2 . . ? F3 C1T S1 110.7 . . ? F1 C1T S1 110.7 . . ? F2 C1T S1 110.7 . . ? O3' S1' O4' 113.5 . . ? O3' S1' O5' 113.5 . . ? O4' S1' O5' 113.4 . . ? O3' S1' C1T' 105.1 . . ? O4' S1' C1T' 105.1 . . ? O5' S1' C1T' 105.1 . . ? F1' C1T' F2' 108.2 . . ? F1' C1T' F3' 108.2 . . ? F2' C1T' F3' 108.2 . . ? F1' C1T' S1' 110.7 . . ? F2' C1T' S1' 110.7 . . ? F3' C1T' S1' 110.7 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.413 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.273 data_Hydroxo_trimer_(7) _database_code_depnum_ccdc_archive 'CCDC 663520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H67 N2 O3 Pt3 3+, 3(S1 F3 O3 C1 1-), Cl2 C1 H2' _chemical_formula_sum 'C56 H69 Cl2 F9 N2 O12 Pt3 S3' _chemical_formula_weight 1885.48 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1910(10) _cell_length_b 14.2422(10) _cell_length_c 17.7064(13) _cell_angle_alpha 93.3520(10) _cell_angle_beta 92.0490(10) _cell_angle_gamma 117.1220(10) _cell_volume 3171.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5281 _cell_measurement_theta_min 2.725 _cell_measurement_theta_max 26.284 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 6.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1972 _exptl_absorpt_correction_T_max 0.4256 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 22962 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.1140 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.12 _reflns_number_total 13697 _reflns_number_gt 8791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two triflate ions are located on inversion centers and were refined with C/S and O/F atoms occupying the same sites (EXYZ) at half occupancy with the same thermal parameters (EADP). ; _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^)+(0.0423P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13697 _refine_ls_number_parameters 792 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.89442(3) 0.80221(3) 0.221552(19) 0.01801(10) Uani 1 1 d . . . Pt2 Pt 0.88592(3) 1.04728(3) 0.21154(2) 0.01999(10) Uani 1 1 d . . . Pt3 Pt 1.14657(3) 1.03604(3) 0.21798(2) 0.02108(10) Uani 1 1 d . . . Cl1 Cl 0.7160(4) 0.3849(4) 0.0433(3) 0.1154(18) Uani 1 1 d . . . Cl2 Cl 0.6564(3) 0.3371(4) 0.1972(3) 0.0841(13) Uani 1 1 d . . . S1 S 0.9257(2) 0.8359(3) -0.01834(15) 0.0399(7) Uani 1 1 d . . . S2 S 1.1757(3) 1.3670(3) 0.3877(2) 0.0599(10) Uani 1 1 d . . . F1 F 0.9183(7) 0.6553(7) -0.0652(5) 0.080(3) Uani 1 1 d . . . F2 F 0.8335(6) 0.6490(6) 0.0344(5) 0.067(2) Uani 1 1 d . . . F3 F 0.7673(6) 0.6564(7) -0.0753(5) 0.081(3) Uani 1 1 d . . . F4 F 1.2075(10) 1.4609(10) 0.2635(7) 0.138(5) Uani 1 1 d . . . F5 F 1.3065(9) 1.5584(7) 0.3592(8) 0.141(5) Uani 1 1 d . . . F6 F 1.3344(8) 1.4360(8) 0.3013(8) 0.136(5) Uani 1 1 d . . . O1 O 1.0358(5) 0.8863(5) 0.1804(3) 0.0208(15) Uani 1 1 d . . . H1O H 1.0199 0.8897 0.1261 0.025 Uiso 1 1 d R . . O2 O 0.8430(5) 0.8945(5) 0.1714(3) 0.0205(14) Uani 1 1 d . . . H2O H 0.8652 0.8979 0.1188 0.025 Uiso 1 1 d R . . O3 O 1.0279(5) 1.0664(5) 0.2614(4) 0.0256(16) Uani 1 1 d . . . H3O H 1.0652 1.1421 0.2805 0.031 Uiso 1 1 d R . . O4 O 1.0199(6) 0.8568(6) 0.0284(4) 0.042(2) Uani 1 1 d . . . O5 O 0.8500(6) 0.8592(6) 0.0209(4) 0.046(2) Uani 1 1 d . . . O6 O 0.9437(7) 0.8699(8) -0.0940(4) 0.062(3) Uani 1 1 d . . . O7 O 1.0992(9) 1.4060(8) 0.3994(8) 0.112(5) Uani 1 1 d . . . O8 O 1.2448(13) 1.3736(10) 0.4465(9) 0.169(8) Uani 1 1 d . . . O9 O 1.1308(6) 1.2671(6) 0.3438(5) 0.057(3) Uani 1 1 d . . . N1 N 0.9378(6) 0.7054(6) 0.2738(4) 0.0204(18) Uani 1 1 d . . . N2 N 0.7542(6) 0.7071(6) 0.2624(4) 0.0154(16) Uani 1 1 d . . . C1 C 0.8605(8) 0.6301(7) 0.3034(5) 0.021(2) Uani 1 1 d . . . C2 C 0.7562(8) 0.6296(7) 0.2965(5) 0.021(2) Uani 1 1 d . . . C3 C 0.5790(8) 0.5079(8) 0.3557(6) 0.029(2) Uani 1 1 d . . . H3 H 0.5367 0.5380 0.3361 0.035 Uiso 1 1 calc R . . C4 C 0.5370(9) 0.4229(9) 0.4033(6) 0.040(3) Uani 1 1 d . . . H4 H 0.4652 0.3965 0.4157 0.048 Uiso 1 1 calc R . . C5 C 0.5962(9) 0.3777(9) 0.4321(7) 0.044(3) Uani 1 1 d . . . H5 H 0.5645 0.3196 0.4623 0.053 Uiso 1 1 calc R . . C6 C 0.7760(10) 0.3805(8) 0.4436(6) 0.038(3) Uani 1 1 d . . . H6 H 0.7525 0.3241 0.4758 0.046 Uiso 1 1 calc R . . C7 C 0.8780(9) 0.4242(8) 0.4243(6) 0.038(3) Uani 1 1 d . . . H7 H 0.9236 0.3976 0.4438 0.046 Uiso 1 1 calc R . . C8 C 0.9188(9) 0.5068(8) 0.3769(6) 0.033(3) Uani 1 1 d . . . H8 H 0.9902 0.5353 0.3634 0.040 Uiso 1 1 calc R . . C9 C 0.8512(8) 0.5459(8) 0.3502(5) 0.028(2) Uani 1 1 d . . . C10 C 0.7447(8) 0.4990(8) 0.3699(6) 0.026(2) Uani 1 1 d . . . C11 C 0.6840(8) 0.5449(7) 0.3390(5) 0.022(2) Uani 1 1 d . . . C12 C 0.7025(9) 0.4166(8) 0.4171(6) 0.033(3) Uani 1 1 d . . . C13 C 1.0459(8) 0.7251(8) 0.2909(6) 0.024(2) Uani 1 1 d . . . C14 C 1.0990(8) 0.6936(8) 0.2369(5) 0.028(2) Uani 1 1 d . . . C15 C 1.1972(9) 0.7059(9) 0.2595(6) 0.038(3) Uani 1 1 d . . . H15 H 1.2328 0.6801 0.2262 0.045 Uiso 1 1 calc R . . C16 C 1.2461(9) 0.7549(9) 0.3299(6) 0.041(3) Uani 1 1 d . . . H16 H 1.3148 0.7629 0.3439 0.050 Uiso 1 1 calc R . . C17 C 1.1965(9) 0.7919(9) 0.3796(6) 0.038(3) Uani 1 1 d . . . H17 H 1.2327 0.8271 0.4269 0.045 Uiso 1 1 calc R . . C18 C 1.0949(8) 0.7797(8) 0.3629(5) 0.025(2) Uani 1 1 d . . . C19 C 1.0431(8) 0.6414(8) 0.1600(6) 0.031(3) Uani 1 1 d . . . H19 H 0.9850 0.6613 0.1503 0.037 Uiso 1 1 calc R . . C20 C 0.9930(11) 0.5210(9) 0.1595(7) 0.061(4) Uani 1 1 d . . . H20A H 1.0471 0.5002 0.1757 0.091 Uiso 1 1 calc R . . H20B H 0.9637 0.4889 0.1081 0.091 Uiso 1 1 calc R . . H20C H 0.9360 0.4965 0.1943 0.091 Uiso 1 1 calc R . . C21 C 1.1189(10) 0.6795(10) 0.0959(7) 0.051(3) Uani 1 1 d . . . H21A H 1.1461 0.7560 0.0941 0.077 Uiso 1 1 calc R . . H21B H 1.0805 0.6431 0.0474 0.077 Uiso 1 1 calc R . . H21C H 1.1783 0.6634 0.1054 0.077 Uiso 1 1 calc R . . C22 C 1.0417(8) 0.8221(8) 0.4166(5) 0.029(2) Uani 1 1 d . . . H22 H 0.9636 0.7851 0.4025 0.035 Uiso 1 1 calc R . . C23 C 1.0814(12) 0.9388(9) 0.4092(6) 0.056(4) Uani 1 1 d . . . H23A H 1.1576 0.9767 0.4241 0.083 Uiso 1 1 calc R . . H23B H 1.0434 0.9655 0.4422 0.083 Uiso 1 1 calc R . . H23C H 1.0691 0.9501 0.3564 0.083 Uiso 1 1 calc R . . C24 C 1.0596(12) 0.8054(12) 0.4992(6) 0.067(4) Uani 1 1 d . . . H24A H 1.0373 0.7301 0.5040 0.101 Uiso 1 1 calc R . . H24B H 1.0180 0.8288 0.5311 0.101 Uiso 1 1 calc R . . H24C H 1.1351 0.8466 0.5155 0.101 Uiso 1 1 calc R . . C25 C 0.6636(7) 0.7257(7) 0.2622(5) 0.020(2) Uani 1 1 d . . . C26 C 0.5997(8) 0.7060(8) 0.1936(6) 0.028(2) Uani 1 1 d . . . C27 C 0.5167(9) 0.7312(8) 0.1949(6) 0.034(3) Uani 1 1 d . . . H27 H 0.4699 0.7158 0.1511 0.041 Uiso 1 1 calc R . . C28 C 0.5024(9) 0.7789(9) 0.2605(7) 0.043(3) Uani 1 1 d . . . H28 H 0.4460 0.7973 0.2600 0.052 Uiso 1 1 calc R . . C29 C 0.5649(9) 0.8010(9) 0.3258(7) 0.039(3) Uani 1 1 d . . . H29 H 0.5528 0.8359 0.3690 0.047 Uiso 1 1 calc R . . C30 C 0.6461(8) 0.7726(9) 0.3292(6) 0.032(3) Uani 1 1 d . . . C31 C 0.6164(9) 0.6487(8) 0.1245(6) 0.033(3) Uani 1 1 d . . . H31 H 0.6929 0.6651 0.1261 0.039 Uiso 1 1 calc R . . C32 C 0.5894(10) 0.6852(10) 0.0513(6) 0.045(3) Uani 1 1 d . . . H32A H 0.5129 0.6625 0.0459 0.068 Uiso 1 1 calc R . . H32B H 0.6097 0.6540 0.0080 0.068 Uiso 1 1 calc R . . H32C H 0.6282 0.7625 0.0528 0.068 Uiso 1 1 calc R . . C33 C 0.5499(12) 0.5297(9) 0.1268(7) 0.063(4) Uani 1 1 d . . . H33A H 0.5675 0.5079 0.1746 0.094 Uiso 1 1 calc R . . H33B H 0.5650 0.4929 0.0841 0.094 Uiso 1 1 calc R . . H33C H 0.4744 0.5118 0.1233 0.094 Uiso 1 1 calc R . . C34 C 0.7200(9) 0.8007(8) 0.4007(5) 0.031(3) Uani 1 1 d . . . H34 H 0.7536 0.7524 0.3982 0.037 Uiso 1 1 calc R . . C35 C 0.6604(11) 0.7812(11) 0.4727(6) 0.060(4) Uani 1 1 d . . . H35A H 0.6369 0.8355 0.4819 0.090 Uiso 1 1 calc R . . H35B H 0.7075 0.7845 0.5157 0.090 Uiso 1 1 calc R . . H35C H 0.5985 0.7112 0.4667 0.090 Uiso 1 1 calc R . . C36 C 0.8089(10) 0.9128(10) 0.4018(7) 0.060(4) Uani 1 1 d . . . H36A H 0.8345 0.9263 0.3510 0.090 Uiso 1 1 calc R . . H36B H 0.8673 0.9216 0.4375 0.090 Uiso 1 1 calc R . . H36C H 0.7825 0.9630 0.4178 0.090 Uiso 1 1 calc R . . C37 C 0.8887(8) 1.1727(8) 0.2880(6) 0.029(3) Uani 1 1 d . . . H37 H 0.9425 1.1950 0.3320 0.035 Uiso 1 1 calc R . . C38 C 0.9308(8) 1.2142(7) 0.2204(6) 0.031(3) Uani 1 1 d . . . H38 H 1.0092 1.2612 0.2249 0.037 Uiso 1 1 calc R . . C39 C 0.8697(9) 1.2436(9) 0.1609(6) 0.037(3) Uani 1 1 d . . . H39A H 0.9200 1.3056 0.1359 0.044 Uiso 1 1 calc R . . H39B H 0.8190 1.2628 0.1860 0.044 Uiso 1 1 calc R . . C40 C 0.8088(9) 1.1489(9) 0.1008(6) 0.036(3) Uani 1 1 d . . . H40A H 0.7461 1.1541 0.0795 0.043 Uiso 1 1 calc R . . H40B H 0.8554 1.1555 0.0590 0.043 Uiso 1 1 calc R . . C41 C 0.7727(8) 1.0434(8) 0.1281(5) 0.026(2) Uani 1 1 d . . . H41 H 0.7504 0.9847 0.0870 0.031 Uiso 1 1 calc R . . C42 C 0.7233(7) 1.0122(8) 0.1961(5) 0.024(2) Uani 1 1 d . . . H42 H 0.6736 0.9348 0.1942 0.028 Uiso 1 1 calc R . . C43 C 0.6907(8) 1.0783(8) 0.2470(6) 0.035(3) Uani 1 1 d . . . H43A H 0.6251 1.0317 0.2706 0.042 Uiso 1 1 calc R . . H43B H 0.6749 1.1262 0.2164 0.042 Uiso 1 1 calc R . . C44 C 0.7784(8) 1.1449(8) 0.3098(6) 0.032(3) Uani 1 1 d . . . H44A H 0.7740 1.2112 0.3234 0.038 Uiso 1 1 calc R . . H44B H 0.7649 1.1050 0.3555 0.038 Uiso 1 1 calc R . . C45 C 1.2690(8) 1.1549(8) 0.2952(6) 0.036(3) Uani 1 1 d . . . H45 H 1.2411 1.1812 0.3382 0.043 Uiso 1 1 calc R . . C46 C 1.2652(8) 1.1977(8) 0.2281(6) 0.033(3) Uani 1 1 d . . . H46 H 1.2364 1.2500 0.2317 0.039 Uiso 1 1 calc R . . C47 C 1.3479(10) 1.2196(9) 0.1697(7) 0.049(3) Uani 1 1 d . . . H47A H 1.3552 1.2815 0.1430 0.058 Uiso 1 1 calc R . . H47B H 1.4173 1.2384 0.1966 0.058 Uiso 1 1 calc R . . C48 C 1.3219(10) 1.1290(9) 0.1127(6) 0.044(3) Uani 1 1 d . . . H48A H 1.2873 1.1394 0.0666 0.053 Uiso 1 1 calc R . . H48B H 1.3889 1.1294 0.0984 0.053 Uiso 1 1 calc R . . C49 C 1.2517(8) 1.0243(9) 0.1385(6) 0.031(3) Uani 1 1 d . . . H49 H 1.2153 0.9676 0.0963 0.037 Uiso 1 1 calc R . . C50 C 1.2672(8) 0.9870(9) 0.2061(6) 0.032(3) Uani 1 1 d . . . H50 H 1.2395 0.9084 0.2030 0.039 Uiso 1 1 calc R . . C51 C 1.3621(9) 1.0455(9) 0.2609(7) 0.042(3) Uani 1 1 d . . . H51A H 1.4242 1.0881 0.2325 0.051 Uiso 1 1 calc R . . H51B H 1.3773 0.9937 0.2868 0.051 Uiso 1 1 calc R . . C52 C 1.3475(9) 1.1179(10) 0.3201(7) 0.047(3) Uani 1 1 d . . . H52A H 1.3239 1.0802 0.3664 0.057 Uiso 1 1 calc R . . H52B H 1.4169 1.1805 0.3335 0.057 Uiso 1 1 calc R . . C53 C 0.8587(11) 0.6939(12) -0.0325(8) 0.059(4) Uani 1 1 d . . . C54 C 1.2572(14) 1.4638(14) 0.3243(12) 0.083(5) Uani 1 1 d . . . C57 C 0.6234(10) 0.3045(10) 0.1023(9) 0.067(4) Uani 1 1 d . . . H57A H 0.5555 0.3060 0.0904 0.081 Uiso 1 1 calc R . . H57B H 0.6113 0.2308 0.0907 0.081 Uiso 1 1 calc R . . S3 S 0.4862(4) 0.9683(4) 0.0384(3) 0.0446(13) Uani 0.50 1 d P . . F7 F 0.3755(7) 0.9083(7) 0.0428(6) 0.086(3) Uani 0.50 1 d P . . F8 F 0.5257(7) 1.0400(7) 0.1051(5) 0.074(3) Uani 0.50 1 d P . . F9 F 0.5304(8) 0.8979(7) 0.0403(6) 0.090(3) Uani 0.50 1 d P . . O10 O 0.3755(7) 0.9083(7) 0.0428(6) 0.086(3) Uani 0.50 1 d P . . O11 O 0.5257(7) 1.0400(7) 0.1051(5) 0.074(3) Uani 0.50 1 d P . . O12 O 0.5304(8) 0.8979(7) 0.0403(6) 0.090(3) Uani 0.50 1 d P . . C55 C 0.4862(4) 0.9683(4) 0.0384(3) 0.0446(13) Uani 0.50 1 d P . . S4 S 0.5482(4) 0.0448(4) 0.4682(3) 0.0397(11) Uani 0.50 1 d P . . F10 F 0.4978(8) 0.0125(9) 0.3973(5) 0.095(4) Uani 0.50 1 d P . . F11 F 0.5637(8) 0.1441(7) 0.4931(7) 0.104(4) Uani 0.50 1 d P . . F12 F 0.6377(6) 0.0346(7) 0.4734(5) 0.066(2) Uani 0.50 1 d P . . O13 O 0.4978(8) 0.0125(9) 0.3973(5) 0.095(4) Uani 0.50 1 d P . . O14 O 0.5637(8) 0.1441(7) 0.4931(7) 0.104(4) Uani 0.50 1 d P . . O15 O 0.6377(6) 0.0346(7) 0.4734(5) 0.066(2) Uani 0.50 1 d P . . C56 C 0.5482(4) 0.0448(4) 0.4682(3) 0.0397(11) Uani 0.50 1 d P . . 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 0.0196(2) 0.0182(2) 0.01585(18) 0.00028(14) 0.00223(14) 0.00843(17) Pt2 0.0216(2) 0.0213(2) 0.01788(19) -0.00019(15) 0.00158(15) 0.01069(17) Pt3 0.0188(2) 0.0232(2) 0.01947(19) 0.00103(15) 0.00164(15) 0.00812(17) Cl1 0.061(3) 0.150(5) 0.107(4) 0.006(3) 0.029(3) 0.023(3) Cl2 0.081(3) 0.104(3) 0.093(3) 0.004(3) 0.001(2) 0.064(3) S1 0.0415(18) 0.061(2) 0.0207(13) -0.0008(13) 0.0040(12) 0.0264(16) S2 0.062(3) 0.044(2) 0.064(2) -0.0187(18) -0.0071(19) 0.0193(19) F1 0.078(6) 0.092(7) 0.081(6) -0.036(5) 0.000(5) 0.055(5) F2 0.063(6) 0.063(6) 0.072(6) 0.005(4) 0.008(4) 0.025(4) F3 0.056(6) 0.095(7) 0.070(6) -0.031(5) -0.015(4) 0.020(5) F4 0.120(11) 0.154(12) 0.138(11) 0.051(9) -0.002(8) 0.058(9) F5 0.140(10) 0.029(6) 0.220(14) -0.021(7) 0.000(9) 0.014(6) F6 0.051(7) 0.094(8) 0.247(15) -0.009(8) 0.029(8) 0.020(6) O1 0.023(4) 0.024(4) 0.012(3) 0.000(3) 0.001(3) 0.009(3) O2 0.025(4) 0.021(4) 0.017(3) 0.002(3) 0.007(3) 0.012(3) O3 0.024(4) 0.026(4) 0.029(4) 0.004(3) 0.003(3) 0.013(3) O4 0.034(5) 0.068(6) 0.020(4) -0.003(4) -0.002(3) 0.022(4) O5 0.050(5) 0.067(6) 0.025(4) -0.007(4) -0.001(4) 0.032(5) O6 0.058(6) 0.111(8) 0.021(4) 0.014(5) 0.008(4) 0.042(6) O7 0.110(10) 0.062(7) 0.179(13) -0.002(8) 0.072(9) 0.051(7) O8 0.215(16) 0.077(9) 0.166(14) -0.013(9) -0.142(13) 0.037(10) O9 0.031(5) 0.048(6) 0.082(7) -0.036(5) -0.009(4) 0.013(4) N1 0.027(5) 0.018(4) 0.015(4) -0.003(3) -0.001(3) 0.010(4) N2 0.018(4) 0.015(4) 0.011(4) 0.003(3) 0.005(3) 0.005(3) C1 0.026(6) 0.016(5) 0.014(5) -0.002(4) -0.003(4) 0.003(4) C2 0.027(6) 0.014(5) 0.017(5) 0.005(4) -0.004(4) 0.006(4) C3 0.025(6) 0.032(6) 0.030(6) 0.010(5) 0.002(5) 0.011(5) C4 0.036(7) 0.039(7) 0.047(7) 0.020(6) 0.014(6) 0.015(6) C5 0.038(8) 0.033(7) 0.050(8) 0.016(6) 0.012(6) 0.003(6) C6 0.055(8) 0.022(6) 0.040(7) 0.017(5) 0.013(6) 0.019(6) C7 0.037(7) 0.028(7) 0.047(7) 0.010(5) -0.006(6) 0.013(6) C8 0.034(7) 0.029(6) 0.039(6) 0.006(5) 0.005(5) 0.016(5) C9 0.038(7) 0.024(6) 0.021(5) 0.006(4) 0.003(5) 0.014(5) C10 0.027(6) 0.017(5) 0.030(6) 0.000(4) -0.001(5) 0.007(5) C11 0.021(5) 0.016(5) 0.022(5) 0.004(4) 0.005(4) 0.001(4) C12 0.043(7) 0.024(6) 0.031(6) 0.008(5) 0.009(5) 0.014(5) C13 0.019(6) 0.024(6) 0.032(6) 0.009(4) 0.014(4) 0.009(5) C14 0.039(7) 0.029(6) 0.022(5) 0.000(4) -0.003(5) 0.022(5) C15 0.036(7) 0.040(7) 0.047(7) -0.002(6) 0.006(6) 0.025(6) C16 0.034(7) 0.057(8) 0.039(7) 0.009(6) 0.000(6) 0.026(6) C17 0.034(7) 0.039(7) 0.034(6) 0.002(5) -0.002(5) 0.012(6) C18 0.023(6) 0.028(6) 0.017(5) 0.001(4) -0.004(4) 0.005(5) C19 0.025(6) 0.036(7) 0.033(6) -0.005(5) 0.004(5) 0.015(5) C20 0.073(10) 0.037(8) 0.054(8) -0.014(6) 0.003(7) 0.011(7) C21 0.054(9) 0.051(8) 0.042(7) 0.000(6) 0.015(6) 0.018(7) C22 0.030(6) 0.035(7) 0.022(5) -0.003(4) -0.005(5) 0.016(5) C23 0.116(12) 0.037(7) 0.029(6) 0.009(5) 0.022(7) 0.046(8) C24 0.115(13) 0.087(11) 0.031(7) 0.012(7) 0.025(8) 0.071(10) C25 0.022(5) 0.021(5) 0.023(5) 0.008(4) 0.015(4) 0.012(4) C26 0.018(6) 0.035(6) 0.030(6) 0.004(5) 0.004(4) 0.011(5) C27 0.033(7) 0.036(7) 0.037(6) -0.004(5) -0.009(5) 0.020(6) C28 0.030(7) 0.040(8) 0.068(9) 0.006(6) 0.009(6) 0.023(6) C29 0.043(8) 0.044(8) 0.043(7) -0.001(6) 0.013(6) 0.030(6) C30 0.026(6) 0.039(7) 0.031(6) 0.012(5) 0.012(5) 0.013(5) C31 0.032(7) 0.035(7) 0.028(6) -0.014(5) -0.004(5) 0.016(5) C32 0.046(8) 0.053(8) 0.035(7) -0.008(6) -0.009(6) 0.023(7) C33 0.114(13) 0.040(8) 0.039(7) -0.010(6) -0.009(8) 0.042(8) C34 0.047(7) 0.034(6) 0.017(5) -0.001(4) 0.007(5) 0.023(6) C35 0.074(10) 0.087(11) 0.025(6) 0.017(7) 0.017(6) 0.041(9) C36 0.066(10) 0.052(9) 0.035(7) -0.011(6) -0.017(7) 0.006(7) C37 0.033(6) 0.029(6) 0.029(6) -0.021(5) -0.011(5) 0.020(5) C38 0.030(6) 0.012(5) 0.035(6) -0.008(4) 0.003(5) -0.004(5) C39 0.038(7) 0.037(7) 0.040(7) 0.006(5) 0.007(5) 0.020(6) C40 0.042(7) 0.047(8) 0.027(6) 0.007(5) 0.000(5) 0.028(6) C41 0.029(6) 0.026(6) 0.027(5) 0.004(4) -0.004(4) 0.017(5) C42 0.020(6) 0.018(5) 0.029(5) 0.001(4) 0.004(4) 0.005(4) C43 0.034(7) 0.036(7) 0.036(6) 0.005(5) 0.010(5) 0.017(6) C44 0.035(7) 0.039(7) 0.029(6) 0.000(5) 0.006(5) 0.024(6) C45 0.024(6) 0.035(7) 0.039(7) -0.023(5) -0.013(5) 0.009(5) C46 0.025(6) 0.023(6) 0.040(6) -0.005(5) 0.004(5) 0.004(5) C47 0.049(8) 0.033(7) 0.054(8) 0.008(6) 0.015(7) 0.009(6) C48 0.051(8) 0.047(8) 0.039(7) 0.020(6) 0.022(6) 0.024(7) C49 0.033(7) 0.045(7) 0.029(6) 0.011(5) 0.023(5) 0.028(6) C50 0.021(6) 0.043(7) 0.039(6) -0.004(5) 0.001(5) 0.021(5) C51 0.036(7) 0.051(8) 0.047(7) 0.005(6) -0.001(6) 0.026(6) C52 0.023(7) 0.073(9) 0.044(7) -0.014(6) -0.011(5) 0.023(6) C53 0.053(9) 0.073(11) 0.057(9) -0.011(8) -0.011(7) 0.036(8) C54 0.065(12) 0.067(13) 0.126(17) 0.023(12) -0.002(11) 0.036(10) C57 0.042(9) 0.046(9) 0.110(13) -0.012(8) -0.006(8) 0.019(7) S3 0.041(3) 0.050(3) 0.046(3) -0.013(2) -0.011(2) 0.026(3) F7 0.048(6) 0.086(7) 0.099(8) -0.031(6) -0.005(5) 0.013(5) F8 0.055(6) 0.102(7) 0.063(6) -0.040(5) -0.017(4) 0.042(5) F9 0.111(8) 0.074(7) 0.108(8) -0.029(6) -0.033(6) 0.070(6) O10 0.048(6) 0.086(7) 0.099(8) -0.031(6) -0.005(5) 0.013(5) O11 0.055(6) 0.102(7) 0.063(6) -0.040(5) -0.017(4) 0.042(5) O12 0.111(8) 0.074(7) 0.108(8) -0.029(6) -0.033(6) 0.070(6) C55 0.041(3) 0.050(3) 0.046(3) -0.013(2) -0.011(2) 0.026(3) S4 0.040(3) 0.045(3) 0.037(3) 0.006(2) 0.004(2) 0.021(3) F10 0.076(7) 0.183(11) 0.042(5) 0.027(6) 0.004(5) 0.070(7) F11 0.087(8) 0.035(6) 0.190(12) 0.030(6) 0.056(8) 0.022(5) F12 0.040(5) 0.071(6) 0.076(6) -0.012(5) 0.009(4) 0.018(4) O13 0.076(7) 0.183(11) 0.042(5) 0.027(6) 0.004(5) 0.070(7) O14 0.087(8) 0.035(6) 0.190(12) 0.030(6) 0.056(8) 0.022(5) O15 0.040(5) 0.071(6) 0.076(6) -0.012(5) 0.009(4) 0.018(4) C56 0.040(3) 0.045(3) 0.037(3) 0.006(2) 0.004(2) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.001(6) . ? Pt1 O2 2.003(6) . ? Pt1 N1 2.004(7) . ? Pt1 N2 2.019(7) . ? Pt2 O2 2.047(6) . ? Pt2 O3 2.064(6) . ? Pt2 C41 2.123(9) . ? Pt2 C42 2.130(9) . ? Pt2 C38 2.156(9) . ? Pt2 C37 2.161(9) . ? Pt3 O1 2.040(6) . ? Pt3 O3 2.080(6) . ? Pt3 C50 2.136(10) . ? Pt3 C46 2.136(10) . ? Pt3 C49 2.141(9) . ? Pt3 C45 2.152(9) . ? Cl1 C57 1.732(15) . ? Cl2 C57 1.705(15) . ? S1 O6 1.442(8) . ? S1 O4 1.445(7) . ? S1 O5 1.449(8) . ? S1 C53 1.797(15) . ? S2 O8 1.374(11) . ? S2 O9 1.430(8) . ? S2 O7 1.443(11) . ? S2 C54 1.822(19) . ? F1 C53 1.333(14) . ? F2 C53 1.360(16) . ? F3 C53 1.339(14) . ? F4 C54 1.254(19) . ? F5 C54 1.30(2) . ? F6 C54 1.388(18) . ? N1 C1 1.290(12) . ? N1 C13 1.445(12) . ? N2 C2 1.299(10) . ? N2 C25 1.426(11) . ? C1 C9 1.457(13) . ? C1 C2 1.478(13) . ? C2 C11 1.451(12) . ? C3 C11 1.386(13) . ? C3 C4 1.425(13) . ? C4 C5 1.371(15) . ? C5 C12 1.392(15) . ? C6 C7 1.356(15) . ? C6 C12 1.434(15) . ? C7 C8 1.398(14) . ? C8 C9 1.392(14) . ? C9 C10 1.414(14) . ? C10 C12 1.394(13) . ? C10 C11 1.410(13) . ? C13 C14 1.411(13) . ? C13 C18 1.429(13) . ? C14 C15 1.365(14) . ? C14 C19 1.517(13) . ? C15 C16 1.384(15) . ? C16 C17 1.370(15) . ? C17 C18 1.390(14) . ? C18 C22 1.496(13) . ? C19 C20 1.528(15) . ? C19 C21 1.538(14) . ? C22 C23 1.508(14) . ? C22 C24 1.525(14) . ? C25 C30 1.412(13) . ? C25 C26 1.423(13) . ? C26 C27 1.378(13) . ? C26 C31 1.517(13) . ? C27 C28 1.379(15) . ? C28 C29 1.361(16) . ? C29 C30 1.386(14) . ? C30 C34 1.525(14) . ? C31 C33 1.521(15) . ? C31 C32 1.525(14) . ? C34 C36 1.517(15) . ? C34 C35 1.524(14) . ? C37 C38 1.396(14) . ? C37 C44 1.500(13) . ? C38 C39 1.534(14) . ? C39 C40 1.550(15) . ? C40 C41 1.467(13) . ? C41 C42 1.406(13) . ? C42 C43 1.497(13) . ? C43 C44 1.546(14) . ? C45 C46 1.377(15) . ? C45 C52 1.495(14) . ? C46 C47 1.527(15) . ? C47 C48 1.486(15) . ? C48 C49 1.477(14) . ? C49 C50 1.389(14) . ? C50 C51 1.496(14) . ? C51 C52 1.512(15) . ? S3 F9 1.406(9) . ? S3 F7 1.413(10) . ? S3 F8 1.430(9) . ? S3 C55 1.635(10) 2_675 ? S3 S3 1.635(10) 2_675 ? S4 F12 1.344(9) . ? S4 F10 1.366(9) . ? S4 F11 1.370(10) . ? S4 C56 1.858(10) 2_656 ? S4 S4 1.858(10) 2_656 ? 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 O1 Pt1 O2 88.3(2) . . ? O1 Pt1 N1 94.8(3) . . ? O2 Pt1 N1 176.8(3) . . ? O1 Pt1 N2 175.3(3) . . ? O2 Pt1 N2 95.7(3) . . ? N1 Pt1 N2 81.2(3) . . ? O2 Pt2 O3 92.4(2) . . ? O2 Pt2 C41 86.4(3) . . ? O3 Pt2 C41 160.2(3) . . ? O2 Pt2 C42 88.2(3) . . ? O3 Pt2 C42 161.1(3) . . ? C41 Pt2 C42 38.6(4) . . ? O2 Pt2 C38 163.9(3) . . ? O3 Pt2 C38 94.5(3) . . ? C41 Pt2 C38 82.2(4) . . ? C42 Pt2 C38 89.9(4) . . ? O2 Pt2 C37 156.6(3) . . ? O3 Pt2 C37 91.3(3) . . ? C41 Pt2 C37 97.7(4) . . ? C42 Pt2 C37 81.0(4) . . ? C38 Pt2 C37 37.7(4) . . ? O1 Pt3 O3 90.0(2) . . ? O1 Pt3 C50 89.0(3) . . ? O3 Pt3 C50 162.7(3) . . ? O1 Pt3 C46 165.9(3) . . ? O3 Pt3 C46 95.3(3) . . ? C50 Pt3 C46 89.8(4) . . ? O1 Pt3 C49 89.3(3) . . ? O3 Pt3 C49 159.4(3) . . ? C50 Pt3 C49 37.9(4) . . ? C46 Pt3 C49 81.1(4) . . ? O1 Pt3 C45 155.4(4) . . ? O3 Pt3 C45 93.4(3) . . ? C50 Pt3 C45 80.7(4) . . ? C46 Pt3 C45 37.5(4) . . ? C49 Pt3 C45 95.8(4) . . ? O6 S1 O4 115.5(5) . . ? O6 S1 O5 115.4(5) . . ? O4 S1 O5 113.9(4) . . ? O6 S1 C53 104.2(6) . . ? O4 S1 C53 102.8(6) . . ? O5 S1 C53 102.6(6) . . ? O8 S2 O9 112.8(7) . . ? O8 S2 O7 120.4(10) . . ? O9 S2 O7 112.3(7) . . ? O8 S2 C54 105.1(10) . . ? O9 S2 C54 105.5(8) . . ? O7 S2 C54 98.0(7) . . ? Pt1 O1 Pt3 126.9(3) . . ? Pt1 O2 Pt2 123.1(3) . . ? Pt2 O3 Pt3 131.1(3) . . ? C1 N1 C13 120.3(8) . . ? C1 N1 Pt1 113.4(7) . . ? C13 N1 Pt1 125.4(6) . . ? C2 N2 C25 121.3(8) . . ? C2 N2 Pt1 113.1(6) . . ? C25 N2 Pt1 125.3(6) . . ? N1 C1 C9 134.9(10) . . ? N1 C1 C2 116.7(9) . . ? C9 C1 C2 108.2(8) . . ? N2 C2 C11 136.6(9) . . ? N2 C2 C1 115.5(8) . . ? C11 C2 C1 107.4(8) . . ? C11 C3 C4 117.4(9) . . ? C5 C4 C3 122.5(11) . . ? C4 C5 C12 120.2(11) . . ? C7 C6 C12 122.1(10) . . ? C6 C7 C8 122.6(10) . . ? C9 C8 C7 117.7(10) . . ? C8 C9 C10 119.3(9) . . ? C8 C9 C1 135.9(10) . . ? C10 C9 C1 104.8(9) . . ? C12 C10 C11 122.2(10) . . ? C12 C10 C9 123.8(9) . . ? C11 C10 C9 114.0(9) . . ? C3 C11 C10 119.6(9) . . ? C3 C11 C2 134.7(9) . . ? C10 C11 C2 105.6(9) . . ? C5 C12 C10 118.0(10) . . ? C5 C12 C6 127.6(10) . . ? C10 C12 C6 114.4(10) . . ? C14 C13 C18 123.2(9) . . ? C14 C13 N1 120.1(9) . . ? C18 C13 N1 116.6(8) . . ? C15 C14 C13 116.8(9) . . ? C15 C14 C19 123.2(9) . . ? C13 C14 C19 119.8(9) . . ? C14 C15 C16 121.5(10) . . ? C17 C16 C15 120.7(11) . . ? C16 C17 C18 122.1(10) . . ? C17 C18 C13 115.2(9) . . ? C17 C18 C22 122.0(9) . . ? C13 C18 C22 122.8(9) . . ? C14 C19 C20 110.7(9) . . ? C14 C19 C21 111.8(9) . . ? C20 C19 C21 110.2(9) . . ? C18 C22 C23 109.7(9) . . ? C18 C22 C24 113.0(9) . . ? C23 C22 C24 109.0(9) . . ? C30 C25 C26 121.9(9) . . ? C30 C25 N2 118.2(8) . . ? C26 C25 N2 119.7(8) . . ? C27 C26 C25 117.8(9) . . ? C27 C26 C31 121.7(9) . . ? C25 C26 C31 120.2(9) . . ? C26 C27 C28 119.3(10) . . ? C29 C28 C27 123.5(11) . . ? C28 C29 C30 119.8(11) . . ? C29 C30 C25 117.6(10) . . ? C29 C30 C34 120.7(10) . . ? C25 C30 C34 121.4(9) . . ? C26 C31 C33 109.8(9) . . ? C26 C31 C32 111.4(9) . . ? C33 C31 C32 110.6(9) . . ? C36 C34 C35 112.5(10) . . ? C36 C34 C30 110.7(9) . . ? C35 C34 C30 112.4(9) . . ? C38 C37 C44 125.6(9) . . ? C38 C37 Pt2 70.9(5) . . ? C44 C37 Pt2 109.9(6) . . ? C37 C38 C39 122.8(10) . . ? C37 C38 Pt2 71.3(5) . . ? C39 C38 Pt2 112.5(7) . . ? C38 C39 C40 110.1(8) . . ? C41 C40 C39 115.8(8) . . ? C42 C41 C40 124.8(9) . . ? C42 C41 Pt2 70.9(5) . . ? C40 C41 Pt2 109.6(7) . . ? C41 C42 C43 124.6(9) . . ? C41 C42 Pt2 70.4(5) . . ? C43 C42 Pt2 115.0(7) . . ? C42 C43 C44 111.6(9) . . ? C37 C44 C43 114.0(8) . . ? C46 C45 C52 126.7(11) . . ? C46 C45 Pt3 70.6(6) . . ? C52 C45 Pt3 110.4(7) . . ? C45 C46 C47 122.9(11) . . ? C45 C46 Pt3 71.9(6) . . ? C47 C46 Pt3 112.1(7) . . ? C48 C47 C46 113.9(10) . . ? C49 C48 C47 114.5(9) . . ? C50 C49 C48 125.4(11) . . ? C50 C49 Pt3 70.9(6) . . ? C48 C49 Pt3 111.0(7) . . ? C49 C50 C51 124.1(10) . . ? C49 C50 Pt3 71.2(5) . . ? C51 C50 Pt3 113.9(7) . . ? C50 C51 C52 113.2(9) . . ? C45 C52 C51 113.9(9) . . ? F1 C53 F3 107.2(11) . . ? F1 C53 F2 106.3(11) . . ? F3 C53 F2 106.1(12) . . ? F1 C53 S1 112.2(11) . . ? F3 C53 S1 113.0(10) . . ? F2 C53 S1 111.6(9) . . ? F4 C54 F5 113.0(16) . . ? F4 C54 F6 103.9(18) . . ? F5 C54 F6 107.1(15) . . ? F4 C54 S2 113.3(14) . . ? F5 C54 S2 111.3(15) . . ? F6 C54 S2 107.7(11) . . ? Cl2 C57 Cl1 115.6(8) . . ? F9 S3 F7 107.3(7) . . ? F9 S3 F8 108.1(6) . . ? F7 S3 F8 107.1(6) . . ? F9 S3 C55 111.4(7) . 2_675 ? F7 S3 C55 111.4(6) . 2_675 ? F8 S3 C55 111.3(6) . 2_675 ? F9 S3 S3 111.4(7) . 2_675 ? F7 S3 S3 111.4(6) . 2_675 ? F8 S3 S3 111.3(6) . 2_675 ? C55 S3 S3 0.0(4) 2_675 2_675 ? F12 S4 F10 111.9(6) . . ? F12 S4 F11 112.8(7) . . ? F10 S4 F11 112.6(8) . . ? F12 S4 C56 109.4(6) . 2_656 ? F10 S4 C56 104.8(6) . 2_656 ? F11 S4 C56 104.8(6) . 2_656 ? F12 S4 S4 109.4(6) . 2_656 ? F10 S4 S4 104.8(6) . 2_656 ? F11 S4 S4 104.8(6) . 2_656 ? C56 S4 S4 0.0(5) 2_656 2_656 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.572 _refine_diff_density_min -1.505 _refine_diff_density_rms 0.243 data_Ni3O2bpy_(8) _database_code_depnum_ccdc_archive 'CCDC 663521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H120 N6 Ni3 O8 2+, 2(B F4 1-)' _chemical_formula_sum 'C78 H120 B2 F8 N6 Ni3 O8' _chemical_formula_weight 1619.55 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/ncm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x, z+1/2' '-x+1/2, -y+1/2, z' 'y, -x+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'y-1/2, -x, -z-1/2' 'x-1/2, y-1/2, -z' '-y, x-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' '-y-1/2, -x-1/2, z' 'y, x, z' _cell_length_a 18.8011(11) _cell_length_b 18.8011(11) _cell_length_c 25.787(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9115.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5958 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 24.61 _exptl_crystal_description PLATE _exptl_crystal_colour RED _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7496 _exptl_absorpt_correction_T_max 0.8761 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 62843 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.13 _reflns_number_total 5266 _reflns_number_gt 3744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1213P)^2^+16.7913P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5266 _refine_ls_number_parameters 276 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2381 _refine_ls_wR_factor_gt 0.2174 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.2500 0.2500 0.69189(4) 0.0303(3) Uani 1 4 d S . . Ni2 Ni 0.29793(3) 0.29793(3) 0.77447(3) 0.0280(3) Uani 1 2 d S . . F1 F 0.6053(5) 0.4780(5) 0.7568(4) 0.130(4) Uani 0.50 1 d PD A 1 F2 F 0.5752(3) 0.5752(3) 0.7372(4) 0.170(4) Uani 1 2 d SD A 1 F3 F 0.53641(19) 0.53641(19) 0.8142(2) 0.0837(17) Uani 1 2 d SD A 1 F4 F 0.4902(2) 0.4902(2) 0.7431(2) 0.0873(19) Uani 1 2 d SD A 1 O1 O 0.20677(15) 0.29323(15) 0.74819(16) 0.0298(9) Uani 1 2 d S . . O2 O 0.3250(4) 0.3250(4) 0.4563(3) 0.121(3) Uani 1 2 d S . . O3 O 0.4681(9) 0.3034(8) 0.6124(6) 0.282(8) Uani 1 1 d D . . N1 N 0.2977(2) 0.2023(2) 0.6380(2) 0.0363(12) Uani 1 2 d S . . N2 N 0.29822(19) 0.3928(2) 0.79679(14) 0.0319(8) Uani 1 1 d . . . C1 C 0.2779(2) 0.2221(2) 0.5898(2) 0.0384(15) Uani 1 2 d S . . C2 C 0.3070(3) 0.1930(3) 0.5462(3) 0.0488(19) Uani 1 2 d S . . H2 H 0.2917 0.2083 0.5129 0.059 Uiso 1 2 calc SR . . C3 C 0.3592(3) 0.1408(3) 0.5506(3) 0.057(2) Uani 1 2 d S . . C4 C 0.3791(3) 0.1209(3) 0.6013(3) 0.054(2) Uani 1 2 d S . . H4 H 0.4145 0.0855 0.6065 0.064 Uiso 1 2 calc SR . . C5 C 0.3476(3) 0.1524(3) 0.6429(3) 0.0424(16) Uani 1 2 d S . . H5 H 0.3618 0.1382 0.6768 0.051 Uiso 1 2 calc SR . . C6 C 0.3932(3) 0.1068(3) 0.5031(3) 0.084(4) Uani 1 2 d S . . C7 C 0.3655(6) 0.1345(6) 0.4555(5) 0.31(2) Uani 1 2 d S . . H7A H 0.3140 0.1266 0.4542 0.458 Uiso 0.50 1 calc PR . . H7B H 0.3882 0.1103 0.4262 0.458 Uiso 1 2 calc SR . . H7C H 0.3753 0.1856 0.4534 0.458 Uiso 0.50 1 calc PR . . C8 C 0.3813(11) 0.0303(7) 0.5046(6) 0.272(11) Uani 1 1 d . . . H8A H 0.4000 0.0109 0.5371 0.408 Uiso 1 1 calc R . . H8B H 0.4057 0.0079 0.4752 0.408 Uiso 1 1 calc R . . H8C H 0.3302 0.0205 0.5023 0.408 Uiso 1 1 calc R . . C9 C 0.2436(3) 0.4384(3) 0.79476(19) 0.0392(11) Uani 1 1 d . . . H9 H 0.1991 0.4223 0.7818 0.047 Uiso 1 1 calc R . . C10 C 0.2500(3) 0.5078(3) 0.8108(2) 0.0499(13) Uani 1 1 d . . . H10 H 0.2100 0.5386 0.8091 0.060 Uiso 1 1 calc R . . C11 C 0.3140(3) 0.5332(3) 0.8294(2) 0.0467(12) Uani 1 1 d . . . C12 C 0.3706(3) 0.4862(2) 0.83089(19) 0.0407(11) Uani 1 1 d . . . H12 H 0.4158 0.5017 0.8428 0.049 Uiso 1 1 calc R . . C13 C 0.3615(2) 0.4170(2) 0.81516(15) 0.0313(9) Uani 1 1 d . . . C14 C 0.3219(4) 0.6113(3) 0.8472(3) 0.076(2) Uani 1 1 d . . . C15 C 0.2556(6) 0.6320(6) 0.8801(7) 0.192(7) Uani 1 1 d . . . H15A H 0.2539 0.6024 0.9113 0.288 Uiso 1 1 calc R . . H15B H 0.2124 0.6245 0.8596 0.288 Uiso 1 1 calc R . . H15C H 0.2589 0.6822 0.8901 0.288 Uiso 1 1 calc R . . C16 C 0.3225(10) 0.6570(5) 0.8009(4) 0.221(10) Uani 1 1 d . . . H16A H 0.2800 0.6475 0.7800 0.331 Uiso 1 1 calc R . . H16B H 0.3651 0.6469 0.7802 0.331 Uiso 1 1 calc R . . H16C H 0.3228 0.7070 0.8115 0.331 Uiso 1 1 calc R . . C17 C 0.3856(5) 0.6230(4) 0.8810(3) 0.092(3) Uani 1 1 d . . . H17A H 0.3829 0.5915 0.9112 0.138 Uiso 1 1 calc R . . H17B H 0.3866 0.6726 0.8926 0.138 Uiso 1 1 calc R . . H17C H 0.4289 0.6126 0.8613 0.138 Uiso 1 1 calc R . . C18 C 0.3398(8) 0.3398(8) 0.4034(5) 0.143(6) Uani 1 2 d S . . H18A H 0.2961 0.3564 0.3858 0.172 Uiso 0.50 1 calc PR . . H18B H 0.3564 0.2961 0.3858 0.172 Uiso 0.50 1 calc PR . . C19 C 0.3943(8) 0.3943(8) 0.4004(7) 0.213(13) Uani 1 2 d S . . H19A H 0.4367 0.3762 0.3819 0.256 Uiso 0.50 1 calc PR . . H19B H 0.3762 0.4367 0.3819 0.256 Uiso 0.50 1 calc PR . . C20 C 0.4108(9) 0.4108(9) 0.4509(8) 0.247(16) Uani 1 2 d S . . H20A H 0.4016 0.4619 0.4573 0.296 Uiso 0.50 1 calc PR . . H20B H 0.4619 0.4016 0.4573 0.296 Uiso 0.50 1 calc PR . . C21 C 0.3695(7) 0.3695(7) 0.4843(5) 0.170(9) Uani 1 2 d S . . H21A H 0.4010 0.3407 0.5068 0.204 Uiso 0.50 1 calc PR . . H21B H 0.3407 0.4010 0.5068 0.204 Uiso 0.50 1 calc PR . . C22 C 0.4879(11) 0.3082(11) 0.6660(5) 0.245(12) Uani 1 1 d D . . H22A H 0.4574 0.3429 0.6845 0.294 Uiso 1 1 calc R . . H22B H 0.4834 0.2613 0.6833 0.294 Uiso 1 1 calc R . . C23 C 0.5566(13) 0.3301(10) 0.6657(10) 0.37(2) Uani 1 1 d D . . H23A H 0.5730 0.3441 0.7008 0.438 Uiso 1 1 calc R . . H23B H 0.5887 0.2932 0.6515 0.438 Uiso 1 1 calc R . . C24 C 0.5514(11) 0.3849(11) 0.6347(7) 0.241(11) Uani 1 1 d D . . H24A H 0.5987 0.4011 0.6226 0.289 Uiso 1 1 calc R . . H24B H 0.5263 0.4251 0.6516 0.289 Uiso 1 1 calc R . . C25 C 0.5133(12) 0.3573(12) 0.5963(5) 0.268(13) Uani 1 1 d D . . H25A H 0.5460 0.3383 0.5696 0.321 Uiso 1 1 calc R . . H25B H 0.4847 0.3955 0.5801 0.321 Uiso 1 1 calc R . . B1 B 0.5483(5) 0.5223(6) 0.7632(4) 0.060(6) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0334(4) 0.0334(4) 0.0241(5) 0.000 0.000 0.0059(5) Ni2 0.0285(3) 0.0285(3) 0.0272(4) 0.0007(2) 0.0007(2) -0.0004(3) F1 0.080(7) 0.140(10) 0.171(11) 0.006(8) 0.055(7) 0.006(6) F2 0.172(6) 0.172(6) 0.167(8) 0.041(4) 0.041(4) -0.091(8) F3 0.083(3) 0.083(3) 0.086(4) -0.0116(19) -0.0116(19) -0.037(3) F4 0.099(3) 0.099(3) 0.064(3) -0.0033(19) -0.0033(19) -0.040(4) O1 0.0309(14) 0.0309(14) 0.028(2) -0.0007(12) 0.0007(12) 0.0024(18) O2 0.154(5) 0.154(5) 0.054(4) 0.005(4) 0.005(4) 0.005(7) O3 0.319(19) 0.279(17) 0.247(16) 0.035(13) -0.083(14) -0.141(14) N1 0.0414(19) 0.0414(19) 0.026(2) 0.0015(15) -0.0015(15) 0.009(2) N2 0.0303(19) 0.0325(19) 0.0329(18) 0.0028(15) -0.0007(15) 0.0009(15) C1 0.041(2) 0.041(2) 0.032(3) 0.0010(19) -0.0010(19) 0.012(3) C2 0.061(3) 0.061(3) 0.025(3) 0.0013(19) -0.0013(19) 0.028(4) C3 0.068(4) 0.068(4) 0.035(4) -0.006(2) 0.006(2) 0.034(4) C4 0.062(3) 0.062(3) 0.038(4) -0.001(2) 0.001(2) 0.032(4) C5 0.047(2) 0.047(2) 0.032(3) 0.0036(19) -0.0036(19) 0.014(3) C6 0.109(6) 0.109(6) 0.035(4) -0.005(3) 0.005(3) 0.067(7) C7 0.44(3) 0.44(3) 0.042(6) -0.021(5) 0.021(5) 0.36(4) C8 0.47(3) 0.148(12) 0.200(13) -0.123(11) 0.204(17) -0.056(14) C9 0.037(3) 0.035(2) 0.046(2) 0.003(2) 0.000(2) 0.001(2) C10 0.045(3) 0.037(3) 0.068(3) 0.000(2) -0.008(3) 0.009(2) C11 0.050(3) 0.030(2) 0.060(3) -0.001(2) -0.009(3) 0.002(2) C12 0.042(3) 0.033(2) 0.048(3) 0.002(2) -0.006(2) -0.007(2) C13 0.033(2) 0.032(2) 0.029(2) 0.0031(17) 0.0030(17) -0.0009(18) C14 0.075(4) 0.031(3) 0.124(6) -0.008(3) -0.033(4) 0.004(3) C15 0.118(9) 0.104(8) 0.35(2) -0.132(12) 0.036(11) 0.011(7) C16 0.47(3) 0.045(5) 0.148(9) 0.028(6) -0.160(14) -0.070(9) C17 0.111(6) 0.048(4) 0.117(6) -0.026(4) -0.051(5) 0.005(4) C18 0.186(11) 0.186(11) 0.059(7) 0.004(7) 0.004(7) -0.004(15) C19 0.27(2) 0.27(2) 0.103(13) 0.022(8) 0.022(8) -0.15(2) C20 0.32(3) 0.32(3) 0.104(14) 0.000(11) 0.000(11) -0.16(3) C21 0.223(14) 0.223(14) 0.064(8) -0.006(7) -0.006(7) -0.077(18) C22 0.31(3) 0.33(3) 0.096(9) 0.076(13) 0.045(13) 0.12(2) C23 0.33(3) 0.136(14) 0.63(6) 0.12(2) -0.35(4) -0.076(18) C24 0.32(3) 0.25(2) 0.150(13) -0.029(15) 0.004(16) -0.14(2) C25 0.42(3) 0.28(2) 0.100(10) 0.029(13) 0.012(15) -0.19(2) B1 0.053(10) 0.055(10) 0.072(8) -0.003(6) 0.020(6) -0.027(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.852(4) . ? Ni1 O1 1.852(4) 3 ? Ni1 N1 1.880(5) 3 ? Ni1 N1 1.880(5) . ? Ni1 Ni2 2.4816(12) . ? Ni1 Ni2 2.4816(12) 3 ? Ni2 O1 1.845(3) 3 ? Ni2 O1 1.845(3) . ? Ni2 N2 1.874(4) 16 ? Ni2 N2 1.874(4) . ? Ni2 Ni2 2.5488(15) 3 ? F1 B1 1.367(12) . ? F2 B1 1.303(10) . ? F2 B1 1.303(10) 16 ? F3 B1 1.359(10) 16 ? F3 B1 1.359(10) . ? F4 B1 1.353(10) 16 ? F4 B1 1.353(10) . ? O1 Ni2 1.845(3) 3 ? O2 C21 1.387(18) . ? O2 C18 1.419(15) . ? O3 C25 1.386(14) . ? O3 C22 1.435(15) . ? N1 C5 1.335(8) . ? N1 C1 1.352(8) . ? N2 C9 1.339(6) . ? N2 C13 1.360(6) . ? C1 C2 1.365(9) . ? C1 C1 1.481(13) 3 ? C2 C3 1.394(10) . ? C3 C4 1.411(10) . ? C3 C6 1.521(11) . ? C4 C5 1.361(10) . ? C6 C7 1.434(17) . ? C6 C8 1.457(13) 15_665 ? C6 C8 1.457(13) . ? C9 C10 1.375(7) . ? C10 C11 1.381(7) . ? C11 C12 1.383(7) . ? C11 C14 1.546(8) . ? C12 C13 1.372(6) . ? C13 C13 1.475(9) 16 ? C14 C16 1.471(12) . ? C14 C17 1.496(9) . ? C14 C15 1.558(13) . ? C18 C19 1.45(2) . ? C19 C20 1.37(2) . ? C20 C21 1.40(2) . ? C22 C23 1.356(17) . ? C23 C24 1.308(15) . ? C24 C25 1.328(14) . ? B1 B1 0.69(2) 16 ? 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 O1 Ni1 O1 76.7(3) . 3 ? O1 Ni1 N1 99.2(2) . 3 ? O1 Ni1 N1 176.0(2) 3 3 ? O1 Ni1 N1 176.0(2) . . ? O1 Ni1 N1 99.2(2) 3 . ? N1 Ni1 N1 84.8(3) 3 . ? O1 Ni1 Ni2 47.72(9) . . ? O1 Ni1 Ni2 47.72(9) 3 . ? N1 Ni1 Ni2 129.32(12) 3 . ? N1 Ni1 Ni2 129.32(12) . . ? O1 Ni1 Ni2 47.72(9) . 3 ? O1 Ni1 Ni2 47.72(9) 3 3 ? N1 Ni1 Ni2 129.32(12) 3 3 ? N1 Ni1 Ni2 129.32(12) . 3 ? Ni2 Ni1 Ni2 61.80(4) . 3 ? O1 Ni2 O1 77.1(2) 3 . ? O1 Ni2 N2 99.27(15) 3 16 ? O1 Ni2 N2 175.51(17) . 16 ? O1 Ni2 N2 175.51(17) 3 . ? O1 Ni2 N2 99.27(15) . . ? N2 Ni2 N2 84.3(2) 16 . ? O1 Ni2 Ni1 47.95(13) 3 . ? O1 Ni2 Ni1 47.95(13) . . ? N2 Ni2 Ni1 127.60(11) 16 . ? N2 Ni2 Ni1 127.60(11) . . ? O1 Ni2 Ni2 46.32(9) 3 3 ? O1 Ni2 Ni2 46.32(9) . 3 ? N2 Ni2 Ni2 132.45(11) 16 3 ? N2 Ni2 Ni2 132.45(11) . 3 ? Ni1 Ni2 Ni2 59.10(2) . 3 ? B1 F2 B1 30.8(10) . 16 ? B1 F3 B1 29.5(10) 16 . ? B1 F4 B1 29.7(10) 16 . ? Ni2 O1 Ni2 87.37(18) . 3 ? Ni2 O1 Ni1 84.33(15) . . ? Ni2 O1 Ni1 84.33(15) 3 . ? C21 O2 C18 105.1(13) . . ? C25 O3 C22 94.8(14) . . ? C5 N1 C1 118.4(6) . . ? C5 N1 Ni1 127.0(4) . . ? C1 N1 Ni1 114.7(4) . . ? C9 N2 C13 118.1(4) . . ? C9 N2 Ni2 126.5(3) . . ? C13 N2 Ni2 115.4(3) . . ? N1 C1 C2 122.4(6) . . ? N1 C1 C1 112.9(4) . 3 ? C2 C1 C1 124.6(4) . 3 ? C1 C2 C3 119.9(6) . . ? C2 C3 C4 116.7(6) . . ? C2 C3 C6 121.7(7) . . ? C4 C3 C6 121.6(7) . . ? C5 C4 C3 120.1(7) . . ? N1 C5 C4 122.5(6) . . ? C7 C6 C8 109.0(9) . 15_665 ? C7 C6 C8 109.0(9) . . ? C8 C6 C8 107.6(18) 15_665 . ? C7 C6 C3 112.7(8) . . ? C8 C6 C3 109.3(6) 15_665 . ? C8 C6 C3 109.3(6) . . ? N2 C9 C10 121.9(5) . . ? C9 C10 C11 120.6(5) . . ? C10 C11 C12 117.3(5) . . ? C10 C11 C14 121.0(5) . . ? C12 C11 C14 121.7(5) . . ? C13 C12 C11 120.1(5) . . ? N2 C13 C12 121.9(4) . . ? N2 C13 C13 112.5(2) . 16 ? C12 C13 C13 125.6(3) . 16 ? C16 C14 C17 112.4(8) . . ? C16 C14 C11 108.3(6) . . ? C17 C14 C11 112.9(5) . . ? C16 C14 C15 107.6(10) . . ? C17 C14 C15 106.6(8) . . ? C11 C14 C15 108.8(6) . . ? O2 C18 C19 109.3(14) . . ? C20 C19 C18 105.6(17) . . ? C19 C20 C21 109.4(19) . . ? O2 C21 C20 110.6(13) . . ? C23 C22 O3 105.1(12) . . ? C24 C23 C22 99.9(14) . . ? C23 C24 C25 100.8(13) . . ? C24 C25 O3 113.2(10) . . ? B1 B1 F2 74.6(5) 16 . ? B1 B1 F4 75.2(5) 16 . ? F2 B1 F4 117.1(9) . . ? B1 B1 F3 75.2(5) 16 . ? F2 B1 F3 114.4(9) . . ? F4 B1 F3 109.0(7) . . ? B1 B1 F1 170.0(6) 16 . ? F2 B1 F1 95.7(7) . . ? F4 B1 F1 108.3(8) . . ? F3 B1 F1 111.5(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.843 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.107 data_Pt2Au2O2_(9,M=Pt) _database_code_depnum_ccdc_archive 'CCDC 663522' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H78 Au2 N4 O2 P2 Pt2 2+, 2(B F4 -1), 2(C H2 Cl2)' _chemical_formula_sum 'C74 H82 Au2 B2 Cl4 F8 N4 O2 P2 Pt2' _chemical_formula_weight 2220.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.5140(7) _cell_length_b 15.3931(8) _cell_length_c 18.8441(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.2570(10) _cell_angle_gamma 90.00 _cell_volume 3896.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5393 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.14 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 7.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1768 _exptl_absorpt_correction_T_max 0.7032 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 27397 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.15 _reflns_number_total 8598 _reflns_number_gt 6769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.0786P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8598 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.684954(16) 0.432033(12) 0.036959(11) 0.02273(7) Uani 1 1 d . . . Pt1 Pt 0.463399(16) 0.413104(12) 0.026988(11) 0.02045(7) Uani 1 1 d . . . Cl1 Cl 0.34130(19) 0.32243(16) 0.26675(13) 0.0800(7) Uani 1 1 d . . . P1 P 0.80393(12) 0.33645(9) 0.02277(8) 0.0259(3) Uani 1 1 d . . . F1 F 0.8028(4) -0.1271(3) -0.2766(2) 0.0708(14) Uani 1 1 d . . . O1 O 0.5653(3) 0.5069(2) 0.05751(18) 0.0201(8) Uiso 1 1 d . . . N1 N 0.4932(3) 0.3300(3) 0.1078(2) 0.0229(10) Uiso 1 1 d . . . C1 C 0.9040(5) 0.3746(3) -0.0261(3) 0.0308(14) Uani 1 1 d . . . B1 B 0.7857(6) -0.0561(5) -0.2353(4) 0.0372(17) Uani 1 1 d . . . Cl2 Cl 0.2201(2) 0.37634(16) 0.13957(16) 0.0942(8) Uani 1 1 d . . . F2 F 0.8753(3) -0.0168(2) -0.2121(2) 0.0520(11) Uani 1 1 d . . . N2 N 0.3680(3) 0.3187(3) -0.0055(2) 0.0218(10) Uiso 1 1 d . . . C2 C 0.8804(6) 0.4079(4) -0.0933(4) 0.0432(17) Uani 1 1 d . . . H2 H 0.8129 0.4092 -0.1136 0.052 Uiso 1 1 calc R . . F3 F 0.7250(3) 0.0041(3) -0.2727(3) 0.0726(14) Uani 1 1 d . . . C3 C 0.9548(7) 0.4398(4) -0.1321(4) 0.052(2) Uani 1 1 d . . . H3 H 0.9384 0.4619 -0.1789 0.062 Uiso 1 1 calc R . . F4 F 0.7401(3) -0.0840(2) -0.1759(2) 0.0475(10) Uani 1 1 d . . . C4 C 1.0511(7) 0.4389(4) -0.1021(5) 0.055(2) Uani 1 1 d . . . H4 H 1.1019 0.4608 -0.1283 0.065 Uiso 1 1 calc R . . C5 C 1.0756(6) 0.4072(4) -0.0351(5) 0.052(2) Uani 1 1 d . . . H5 H 1.1431 0.4075 -0.0147 0.063 Uiso 1 1 calc R . . C6 C 1.0015(5) 0.3743(4) 0.0038(4) 0.0402(16) Uani 1 1 d . . . H6 H 1.0184 0.3518 0.0505 0.048 Uiso 1 1 calc R . . C7 C 0.8630(4) 0.2915(4) 0.1057(3) 0.0276(13) Uani 1 1 d . . . C8 C 0.8649(5) 0.3398(4) 0.1679(3) 0.0325(14) Uani 1 1 d . . . H8 H 0.8311 0.3940 0.1675 0.039 Uiso 1 1 calc R . . C9 C 0.9163(5) 0.3092(4) 0.2308(4) 0.0436(17) Uani 1 1 d . . . H9 H 0.9182 0.3427 0.2732 0.052 Uiso 1 1 calc R . . C10 C 0.9641(5) 0.2306(4) 0.2316(4) 0.0444(17) Uani 1 1 d . . . H10 H 0.9994 0.2100 0.2747 0.053 Uiso 1 1 calc R . . C11 C 0.9614(5) 0.1810(4) 0.1703(4) 0.0456(18) Uani 1 1 d . . . H11 H 0.9941 0.1264 0.1714 0.055 Uiso 1 1 calc R . . C12 C 0.9112(5) 0.2112(4) 0.1076(4) 0.0396(16) Uani 1 1 d . . . H12 H 0.9093 0.1771 0.0654 0.048 Uiso 1 1 calc R . . C13 C 0.7498(4) 0.2434(4) -0.0267(3) 0.0296(13) Uani 1 1 d . . . C14 C 0.7966(5) 0.2010(4) -0.0797(4) 0.0403(16) Uani 1 1 d . . . H14 H 0.8596 0.2206 -0.0912 0.048 Uiso 1 1 calc R . . C15 C 0.7512(6) 0.1304(4) -0.1154(4) 0.0485(19) Uani 1 1 d . . . H15 H 0.7840 0.1014 -0.1507 0.058 Uiso 1 1 calc R . . C16 C 0.6596(6) 0.1020(4) -0.1006(4) 0.0482(19) Uani 1 1 d . . . H16 H 0.6288 0.0536 -0.1254 0.058 Uiso 1 1 calc R . . C17 C 0.6129(6) 0.1444(4) -0.0493(4) 0.055(2) Uani 1 1 d . . . H17 H 0.5489 0.1256 -0.0393 0.065 Uiso 1 1 calc R . . C18 C 0.6569(5) 0.2130(4) -0.0126(4) 0.0423(17) Uani 1 1 d . . . H18 H 0.6236 0.2405 0.0231 0.051 Uiso 1 1 calc R . . C19 C 0.5641(4) 0.3415(3) 0.1636(3) 0.0246(12) Uani 1 1 d . . . H19 H 0.5963 0.3963 0.1694 0.029 Uiso 1 1 calc R . . C20 C 0.5912(4) 0.2769(4) 0.2118(3) 0.0290(13) Uani 1 1 d . . . H20 H 0.6411 0.2874 0.2504 0.035 Uiso 1 1 calc R . . C21 C 0.5447(5) 0.1947(4) 0.2042(3) 0.0290(13) Uani 1 1 d . . . C22 C 0.4703(4) 0.1850(3) 0.1490(3) 0.0262(13) Uani 1 1 d . . . H22 H 0.4355 0.1314 0.1434 0.031 Uiso 1 1 calc R . . C23 C 0.4450(4) 0.2526(3) 0.1011(3) 0.0230(12) Uani 1 1 d . . . C24 C 0.3698(4) 0.2477(3) 0.0385(3) 0.0238(12) Uani 1 1 d . . . C25 C 0.3063(4) 0.1789(3) 0.0222(3) 0.0263(12) Uani 1 1 d . . . H25 H 0.3091 0.1300 0.0530 0.032 Uiso 1 1 calc R . . C26 C 0.2378(5) 0.1799(4) -0.0388(3) 0.0310(14) Uani 1 1 d . . . C27 C 0.2403(5) 0.2517(4) -0.0831(3) 0.0301(13) Uani 1 1 d . . . H27 H 0.1967 0.2547 -0.1261 0.036 Uiso 1 1 calc R . . C28 C 0.3058(4) 0.3187(3) -0.0648(3) 0.0266(13) Uani 1 1 d . . . H28 H 0.3063 0.3670 -0.0962 0.032 Uiso 1 1 calc R . . C29 C 0.5805(5) 0.1210(4) 0.2555(3) 0.0410(17) Uani 1 1 d . . . C30 C 0.6913(6) 0.1043(5) 0.2471(5) 0.063(2) Uani 1 1 d . . . H30A H 0.6992 0.0948 0.1966 0.094 Uiso 1 1 calc R . . H30B H 0.7142 0.0528 0.2747 0.094 Uiso 1 1 calc R . . H30C H 0.7309 0.1548 0.2646 0.094 Uiso 1 1 calc R . . C31 C 0.5675(7) 0.1475(5) 0.3315(4) 0.064(2) Uani 1 1 d . . . H31A H 0.6051 0.2009 0.3436 0.095 Uiso 1 1 calc R . . H31B H 0.5921 0.1011 0.3644 0.095 Uiso 1 1 calc R . . H31C H 0.4967 0.1578 0.3357 0.095 Uiso 1 1 calc R . . C32 C 0.5234(6) 0.0367(4) 0.2364(4) 0.058(2) Uani 1 1 d . . . H32A H 0.4520 0.0469 0.2372 0.087 Uiso 1 1 calc R . . H32B H 0.5456 -0.0084 0.2712 0.087 Uiso 1 1 calc R . . H32C H 0.5361 0.0178 0.1886 0.087 Uiso 1 1 calc R . . C33 C 0.1653(5) 0.1050(4) -0.0558(4) 0.0448(18) Uani 1 1 d . . . C34 C 0.1110(10) 0.0873(9) 0.0091(6) 0.156(7) Uani 1 1 d . . . H34A H 0.0519 0.1244 0.0074 0.234 Uiso 1 1 calc R . . H34B H 0.1553 0.1000 0.0526 0.234 Uiso 1 1 calc R . . H34C H 0.0909 0.0262 0.0092 0.234 Uiso 1 1 calc R . . C35 C 0.0923(9) 0.1213(7) -0.1175(7) 0.161(7) Uani 1 1 d . . . H35A H 0.0418 0.0753 -0.1210 0.241 Uiso 1 1 calc R . . H35B H 0.1259 0.1219 -0.1611 0.241 Uiso 1 1 calc R . . H35C H 0.0602 0.1776 -0.1119 0.241 Uiso 1 1 calc R . . C36 C 0.2247(9) 0.0240(6) -0.0677(8) 0.127(5) Uani 1 1 d . . . H36A H 0.1791 -0.0243 -0.0807 0.190 Uiso 1 1 calc R . . H36B H 0.2671 0.0096 -0.0237 0.190 Uiso 1 1 calc R . . H36C H 0.2663 0.0343 -0.1063 0.190 Uiso 1 1 calc R . . C1M C 0.2384(6) 0.2965(5) 0.2045(5) 0.064(2) Uani 1 1 d . . . H1M1 H 0.2502 0.2400 0.1817 0.077 Uiso 1 1 calc R . . H1M2 H 0.1780 0.2910 0.2295 0.077 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 Au1 0.02245(13) 0.01937(11) 0.02580(12) 0.00131(8) 0.00009(9) 0.00079(8) Pt1 0.02262(13) 0.01559(10) 0.02295(12) 0.00231(7) 0.00162(9) -0.00078(8) Cl1 0.0808(18) 0.0816(16) 0.0787(17) 0.0017(13) 0.0147(13) -0.0084(13) P1 0.0247(9) 0.0245(7) 0.0280(8) -0.0019(6) 0.0004(6) 0.0013(6) F1 0.107(4) 0.053(3) 0.056(3) -0.026(2) 0.028(3) -0.018(3) C1 0.033(4) 0.021(3) 0.038(4) -0.005(2) 0.002(3) 0.000(2) B1 0.044(5) 0.029(4) 0.038(4) 0.000(3) 0.002(4) 0.001(3) Cl2 0.107(2) 0.0690(15) 0.104(2) 0.0122(15) 0.0016(17) 0.0143(15) F2 0.039(2) 0.042(2) 0.074(3) -0.001(2) -0.002(2) 0.0010(18) C2 0.050(5) 0.047(4) 0.032(4) -0.001(3) 0.006(3) -0.012(3) F3 0.053(3) 0.074(3) 0.088(4) 0.043(3) -0.005(3) -0.001(2) C3 0.069(6) 0.047(4) 0.042(4) -0.005(3) 0.019(4) -0.013(4) F4 0.062(3) 0.043(2) 0.039(2) 0.0070(17) 0.013(2) -0.0035(18) C4 0.064(6) 0.034(4) 0.073(6) -0.015(4) 0.042(5) -0.015(4) C5 0.041(5) 0.040(4) 0.080(6) -0.010(4) 0.026(4) -0.002(3) C6 0.036(4) 0.031(3) 0.055(4) -0.006(3) 0.012(3) 0.005(3) C7 0.027(3) 0.028(3) 0.027(3) 0.001(2) 0.000(3) 0.005(2) C8 0.033(4) 0.032(3) 0.033(3) 0.002(3) 0.004(3) 0.005(3) C9 0.047(5) 0.050(4) 0.034(4) 0.002(3) 0.001(3) -0.001(3) C10 0.045(4) 0.040(4) 0.044(4) 0.016(3) -0.010(3) 0.002(3) C11 0.044(5) 0.032(3) 0.057(5) 0.007(3) -0.011(3) 0.010(3) C12 0.049(4) 0.023(3) 0.045(4) 0.002(3) -0.004(3) 0.001(3) C13 0.030(4) 0.028(3) 0.029(3) 0.000(2) -0.005(3) 0.002(2) C14 0.038(4) 0.034(3) 0.048(4) -0.009(3) 0.003(3) -0.003(3) C15 0.068(6) 0.039(4) 0.039(4) -0.014(3) 0.010(4) -0.005(4) C16 0.054(5) 0.027(3) 0.062(5) -0.012(3) -0.006(4) -0.010(3) C17 0.039(5) 0.036(4) 0.089(6) -0.014(4) 0.010(4) -0.010(3) C18 0.032(4) 0.037(4) 0.060(5) -0.008(3) 0.014(3) -0.004(3) C19 0.025(3) 0.022(3) 0.026(3) -0.001(2) 0.000(2) -0.004(2) C20 0.030(3) 0.031(3) 0.024(3) 0.005(2) -0.005(3) -0.007(2) C21 0.034(4) 0.029(3) 0.024(3) 0.003(2) -0.001(3) -0.004(2) C22 0.030(3) 0.020(3) 0.029(3) 0.005(2) 0.001(3) -0.006(2) C23 0.028(3) 0.018(2) 0.024(3) 0.003(2) 0.004(2) -0.002(2) C24 0.021(3) 0.028(3) 0.022(3) 0.004(2) 0.002(2) 0.000(2) C25 0.030(3) 0.022(3) 0.027(3) 0.004(2) 0.003(3) -0.004(2) C26 0.035(4) 0.027(3) 0.030(3) 0.004(2) -0.001(3) -0.005(2) C27 0.031(4) 0.028(3) 0.030(3) 0.001(2) -0.004(3) -0.005(2) C28 0.037(4) 0.023(3) 0.019(3) 0.006(2) 0.001(2) -0.003(2) C29 0.045(4) 0.034(3) 0.040(4) 0.017(3) -0.012(3) -0.010(3) C30 0.046(5) 0.054(5) 0.084(6) 0.023(4) -0.013(4) 0.008(4) C31 0.093(7) 0.057(5) 0.039(4) 0.020(4) -0.004(4) -0.005(4) C32 0.063(5) 0.028(3) 0.077(6) 0.023(4) -0.024(4) -0.011(3) C33 0.045(5) 0.039(4) 0.047(4) 0.009(3) -0.010(3) -0.018(3) C34 0.154(13) 0.231(16) 0.083(8) 0.012(9) 0.006(8) -0.156(12) C35 0.140(11) 0.120(9) 0.189(13) 0.091(9) -0.135(10) -0.108(9) C36 0.111(10) 0.041(5) 0.215(15) -0.031(7) -0.047(9) -0.011(6) C1M 0.070(6) 0.052(5) 0.073(6) -0.006(4) 0.020(5) -0.005(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 Au1 O1 2.057(3) . ? Au1 P1 2.2170(15) . ? Au1 Pt1 2.9937(3) . ? Au1 Pt1 3.2600(3) 3_665 ? Pt1 N2 1.994(4) . ? Pt1 N1 1.996(4) . ? Pt1 O1 2.017(3) 3_665 ? Pt1 O1 2.034(3) . ? Pt1 Pt1 3.0642(4) 3_665 ? Pt1 Au1 3.2600(3) 3_665 ? Cl1 C1M 1.764(9) . ? P1 C7 1.812(6) . ? P1 C1 1.815(6) . ? P1 C13 1.818(6) . ? F1 B1 1.374(8) . ? O1 Pt1 2.017(3) 3_665 ? N1 C19 1.355(7) . ? N1 C23 1.357(6) . ? C1 C2 1.371(9) . ? C1 C6 1.375(9) . ? B1 F2 1.381(9) . ? B1 F3 1.380(8) . ? B1 F4 1.404(9) . ? Cl2 C1M 1.732(8) . ? N2 C28 1.323(7) . ? N2 C24 1.370(6) . ? C2 C3 1.395(10) . ? C3 C4 1.361(11) . ? C4 C5 1.360(11) . ? C5 C6 1.399(9) . ? C7 C8 1.386(8) . ? C7 C12 1.396(8) . ? C8 C9 1.389(8) . ? C9 C10 1.371(9) . ? C10 C11 1.381(9) . ? C11 C12 1.379(9) . ? C13 C18 1.393(8) . ? C13 C14 1.401(8) . ? C14 C15 1.385(9) . ? C15 C16 1.369(10) . ? C16 C17 1.376(10) . ? C17 C18 1.362(9) . ? C19 C20 1.369(7) . ? C20 C21 1.414(8) . ? C21 C22 1.373(8) . ? C21 C29 1.534(8) . ? C22 C23 1.396(7) . ? C23 C24 1.471(7) . ? C24 C25 1.377(7) . ? C25 C26 1.395(8) . ? C26 C27 1.388(7) . ? C26 C33 1.524(8) . ? C27 C28 1.378(8) . ? C29 C31 1.519(10) . ? C29 C32 1.532(9) . ? C29 C30 1.544(10) . ? C33 C35 1.463(11) . ? C33 C36 1.513(12) . ? C33 C34 1.517(13) . ? 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 O1 Au1 P1 171.91(10) . . ? O1 Au1 Pt1 42.68(9) . . ? P1 Au1 Pt1 131.40(4) . . ? O1 Au1 Pt1 36.42(9) . 3_665 ? P1 Au1 Pt1 149.95(4) . 3_665 ? Pt1 Au1 Pt1 58.493(8) . 3_665 ? N2 Pt1 N1 80.63(18) . . ? N2 Pt1 O1 98.06(16) . 3_665 ? N1 Pt1 O1 177.60(15) . 3_665 ? N2 Pt1 O1 177.42(16) . . ? N1 Pt1 O1 99.50(16) . . ? O1 Pt1 O1 81.71(15) 3_665 . ? N2 Pt1 Au1 134.35(12) . . ? N1 Pt1 Au1 84.12(13) . . ? O1 Pt1 Au1 95.45(10) 3_665 . ? O1 Pt1 Au1 43.26(10) . . ? N2 Pt1 Pt1 139.07(12) . 3_665 ? N1 Pt1 Pt1 140.11(13) . 3_665 ? O1 Pt1 Pt1 41.07(10) 3_665 3_665 ? O1 Pt1 Pt1 40.64(10) . 3_665 ? Au1 Pt1 Pt1 65.102(8) . 3_665 ? N2 Pt1 Au1 93.91(12) . 3_665 ? N1 Pt1 Au1 144.61(13) . 3_665 ? O1 Pt1 Au1 37.26(10) 3_665 3_665 ? O1 Pt1 Au1 87.45(10) . 3_665 ? Au1 Pt1 Au1 121.507(8) . 3_665 ? Pt1 Pt1 Au1 56.405(8) 3_665 3_665 ? C7 P1 C1 106.2(3) . . ? C7 P1 C13 104.8(3) . . ? C1 P1 C13 106.0(3) . . ? C7 P1 Au1 113.97(19) . . ? C1 P1 Au1 115.88(19) . . ? C13 P1 Au1 109.2(2) . . ? Pt1 O1 Pt1 98.29(15) 3_665 . ? Pt1 O1 Au1 106.31(16) 3_665 . ? Pt1 O1 Au1 94.06(14) . . ? C19 N1 C23 118.6(4) . . ? C19 N1 Pt1 125.1(4) . . ? C23 N1 Pt1 115.9(4) . . ? C2 C1 C6 119.7(6) . . ? C2 C1 P1 118.5(5) . . ? C6 C1 P1 121.7(5) . . ? F1 B1 F2 109.4(6) . . ? F1 B1 F3 111.9(6) . . ? F2 B1 F3 108.6(5) . . ? F1 B1 F4 109.0(5) . . ? F2 B1 F4 109.1(6) . . ? F3 B1 F4 108.9(6) . . ? C28 N2 C24 118.7(5) . . ? C28 N2 Pt1 126.1(4) . . ? C24 N2 Pt1 115.2(4) . . ? C1 C2 C3 120.4(7) . . ? C4 C3 C2 119.3(8) . . ? C3 C4 C5 120.9(7) . . ? C4 C5 C6 120.0(8) . . ? C1 C6 C5 119.6(7) . . ? C8 C7 C12 119.2(6) . . ? C8 C7 P1 119.3(4) . . ? C12 C7 P1 121.4(5) . . ? C7 C8 C9 120.0(6) . . ? C10 C9 C8 120.1(6) . . ? C9 C10 C11 120.5(6) . . ? C12 C11 C10 119.8(6) . . ? C11 C12 C7 120.3(6) . . ? C18 C13 C14 117.7(6) . . ? C18 C13 P1 119.2(5) . . ? C14 C13 P1 123.1(5) . . ? C15 C14 C13 120.1(6) . . ? C16 C15 C14 121.0(7) . . ? C15 C16 C17 119.0(6) . . ? C18 C17 C16 121.1(7) . . ? C17 C18 C13 121.1(7) . . ? N1 C19 C20 122.4(5) . . ? C19 C20 C21 119.9(5) . . ? C22 C21 C20 117.0(5) . . ? C22 C21 C29 123.5(5) . . ? C20 C21 C29 119.5(5) . . ? C21 C22 C23 121.1(5) . . ? N1 C23 C22 120.8(5) . . ? N1 C23 C24 113.7(4) . . ? C22 C23 C24 125.4(5) . . ? N2 C24 C25 120.5(5) . . ? N2 C24 C23 114.2(5) . . ? C25 C24 C23 125.3(5) . . ? C24 C25 C26 121.2(5) . . ? C27 C26 C25 116.5(5) . . ? C27 C26 C33 122.2(5) . . ? C25 C26 C33 121.3(5) . . ? C28 C27 C26 120.2(5) . . ? N2 C28 C27 122.9(5) . . ? C31 C29 C32 110.0(6) . . ? C31 C29 C21 109.5(6) . . ? C32 C29 C21 111.2(5) . . ? C31 C29 C30 110.8(6) . . ? C32 C29 C30 107.7(6) . . ? C21 C29 C30 107.5(5) . . ? C35 C33 C36 110.3(9) . . ? C35 C33 C34 109.2(10) . . ? C36 C33 C34 106.4(9) . . ? C35 C33 C26 113.6(6) . . ? C36 C33 C26 108.3(6) . . ? C34 C33 C26 108.8(7) . . ? Cl2 C1M Cl1 110.5(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.562 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.170 data_Pd2(NHPh)2(bpy)2(BF4)2_(12,Ar=Ph) _database_code_depnum_ccdc_archive 'CCDC 663523' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 N6 Pd2 2+, 2(B F4 1-), 4(C4 H8 O)' _chemical_formula_sum 'C64 H92 B2 F8 N6 O4 Pd2' _chemical_formula_weight 1395.86 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.4761(8) _cell_length_b 11.1520(5) _cell_length_c 18.0618(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.2730(10) _cell_angle_gamma 90.00 _cell_volume 3322.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7740 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.06 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8618 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 23148 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.13 _reflns_number_total 7335 _reflns_number_gt 5355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+2.3700P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7335 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.451127(13) 0.02220(2) 0.412065(12) 0.01900(8) Uani 1 1 d . . . F1 F 0.60453(12) 0.2816(2) 0.45299(13) 0.0510(6) Uani 1 1 d . . . O1 O 0.72464(18) 0.1184(3) 0.2208(2) 0.0672(9) Uani 1 1 d . . . N1 N 0.33611(15) 0.0075(2) 0.33736(14) 0.0229(6) Uani 1 1 d . . . C6 C 0.27474(19) -0.0457(3) 0.35294(18) 0.0294(8) Uani 1 1 d . . . H6 H 0.2842 -0.0779 0.4039 0.035 Uiso 1 1 calc R . . B1 B 0.6836(3) 0.3241(4) 0.4693(2) 0.0367(10) Uani 1 1 d . . . F2 F 0.72785(13) 0.2816(2) 0.54448(12) 0.0520(6) Uani 1 1 d . . . O2 O 0.0970(3) 0.3182(4) 0.2691(3) 0.1152(16) Uani 1 1 d . . . N2 N 0.46571(14) 0.0852(2) 0.31124(13) 0.0221(5) Uani 1 1 d . . . C5 C 0.19834(19) -0.0560(3) 0.29861(18) 0.0285(7) Uani 1 1 d . . . H5 H 0.1570 -0.0965 0.3122 0.034 Uiso 1 1 calc R . . F3 F 0.68456(18) 0.4457(2) 0.46904(18) 0.0756(8) Uani 1 1 d . . . N3 N 0.56858(15) 0.0258(3) 0.48599(14) 0.0204(5) Uani 1 1 d . . . C4 C 0.18134(17) -0.0075(3) 0.22415(17) 0.0233(7) Uani 1 1 d . . . F4 F 0.71626(16) 0.2763(2) 0.41608(13) 0.0596(7) Uani 1 1 d . . . C3 C 0.24612(18) 0.0463(3) 0.20763(17) 0.0237(7) Uani 1 1 d . . . H3 H 0.2377 0.0802 0.1573 0.028 Uiso 1 1 calc R . . C2 C 0.32247(18) 0.0507(3) 0.26368(17) 0.0213(7) Uani 1 1 d . . . C7 C 0.39550(17) 0.0965(3) 0.24906(17) 0.0221(7) Uani 1 1 d . . . C8 C 0.39551(18) 0.1400(3) 0.17732(17) 0.0247(7) Uani 1 1 d . . . H8 H 0.3456 0.1481 0.1356 0.030 Uiso 1 1 calc R . . C9 C 0.46780(18) 0.1723(3) 0.16545(17) 0.0252(7) Uani 1 1 d . . . C10 C 0.53831(19) 0.1606(3) 0.22952(18) 0.0280(7) Uani 1 1 d . . . H10 H 0.5891 0.1814 0.2245 0.034 Uiso 1 1 calc R . . C11 C 0.53502(18) 0.1189(3) 0.30066(17) 0.0248(7) Uani 1 1 d . . . H11 H 0.5840 0.1139 0.3438 0.030 Uiso 1 1 calc R . . C12 C 0.09813(18) -0.0183(3) 0.16142(18) 0.0281(7) Uani 1 1 d . . . C13 C 0.03295(19) -0.0561(4) 0.1968(2) 0.0396(9) Uani 1 1 d . . . H13A H 0.0465 -0.1352 0.2213 0.059 Uiso 1 1 calc R . . H13B H -0.0199 -0.0598 0.1552 0.059 Uiso 1 1 calc R . . H13C H 0.0307 0.0026 0.2364 0.059 Uiso 1 1 calc R . . C14 C 0.1039(2) -0.1144(4) 0.1024(2) 0.0454(10) Uani 1 1 d . . . H14A H 0.1433 -0.0891 0.0775 0.068 Uiso 1 1 calc R . . H14B H 0.0506 -0.1249 0.0622 0.068 Uiso 1 1 calc R . . H14C H 0.1213 -0.1906 0.1299 0.068 Uiso 1 1 calc R . . C15 C 0.0730(2) 0.1029(4) 0.1192(2) 0.0420(9) Uani 1 1 d . . . H15A H 0.0745 0.1653 0.1579 0.063 Uiso 1 1 calc R . . H15B H 0.0179 0.0966 0.0817 0.063 Uiso 1 1 calc R . . H15C H 0.1105 0.1238 0.0912 0.063 Uiso 1 1 calc R . . C16 C 0.46675(19) 0.2173(3) 0.08513(18) 0.0316(8) Uani 1 1 d . . . C18 C 0.4237(2) 0.1249(4) 0.0225(2) 0.0414(9) Uani 1 1 d . . . H18A H 0.4523 0.0481 0.0346 0.062 Uiso 1 1 calc R . . H18B H 0.4234 0.1530 -0.0290 0.062 Uiso 1 1 calc R . . H18C H 0.3678 0.1145 0.0218 0.062 Uiso 1 1 calc R . . C17 C 0.5525(2) 0.2383(5) 0.0823(2) 0.0539(12) Uani 1 1 d . . . H17A H 0.5799 0.2991 0.1212 0.081 Uiso 1 1 calc R . . H17B H 0.5492 0.2662 0.0299 0.081 Uiso 1 1 calc R . . H17C H 0.5832 0.1632 0.0940 0.081 Uiso 1 1 calc R . . C19 C 0.4204(2) 0.3362(4) 0.0668(2) 0.0463(10) Uani 1 1 d . . . H19A H 0.3657 0.3249 0.0692 0.069 Uiso 1 1 calc R . . H19B H 0.4169 0.3630 0.0142 0.069 Uiso 1 1 calc R . . H19C H 0.4490 0.3967 0.1054 0.069 Uiso 1 1 calc R . . C20 C 0.62053(17) -0.0553(3) 0.46389(16) 0.0227(7) Uani 1 1 d . . . C21 C 0.5999(2) -0.1759(3) 0.45322(18) 0.0287(7) Uani 1 1 d . . . H21 H 0.5517 -0.2033 0.4612 0.034 Uiso 1 1 calc R . . C22 C 0.6485(2) -0.2565(3) 0.4311(2) 0.0383(9) Uani 1 1 d . . . H22 H 0.6337 -0.3387 0.4240 0.046 Uiso 1 1 calc R . . C23 C 0.7189(2) -0.2173(4) 0.4193(2) 0.0438(10) Uani 1 1 d . . . H23 H 0.7523 -0.2724 0.4040 0.053 Uiso 1 1 calc R . . C24 C 0.7402(2) -0.0976(4) 0.4298(2) 0.0393(9) Uani 1 1 d . . . H24 H 0.7884 -0.0706 0.4217 0.047 Uiso 1 1 calc R . . C25 C 0.69146(19) -0.0163(3) 0.45211(18) 0.0302(7) Uani 1 1 d . . . H25 H 0.7065 0.0659 0.4593 0.036 Uiso 1 1 calc R . . C26 C 0.7997(3) 0.1425(5) 0.2801(3) 0.0731(14) Uani 1 1 d . . . H26A H 0.7921 0.1474 0.3319 0.088 Uiso 1 1 calc R . . H26B H 0.8219 0.2199 0.2696 0.088 Uiso 1 1 calc R . . C27 C 0.8556(3) 0.0445(4) 0.2795(4) 0.0794(17) Uani 1 1 d . . . H27A H 0.8897 0.0234 0.3336 0.095 Uiso 1 1 calc R . . H27B H 0.8914 0.0673 0.2492 0.095 Uiso 1 1 calc R . . C28 C 0.8022(4) -0.0575(5) 0.2415(3) 0.0817(17) Uani 1 1 d . . . H28A H 0.7955 -0.1135 0.2815 0.098 Uiso 1 1 calc R . . H28B H 0.8253 -0.1020 0.2064 0.098 Uiso 1 1 calc R . . C29 C 0.7230(4) -0.0018(4) 0.1958(4) 0.094(2) Uani 1 1 d . . . H29A H 0.7151 -0.0049 0.1390 0.113 Uiso 1 1 calc R . . H29B H 0.6779 -0.0456 0.2054 0.113 Uiso 1 1 calc R . . C30 C 0.0187(4) 0.3054(6) 0.2777(4) 0.100(2) Uani 1 1 d . . . H30A H -0.0138 0.3789 0.2594 0.120 Uiso 1 1 calc R . . H30B H -0.0106 0.2369 0.2461 0.120 Uiso 1 1 calc R . . C31 C 0.0295(4) 0.2869(9) 0.3535(3) 0.127(3) Uani 1 1 d . . . H31A H -0.0087 0.2252 0.3596 0.153 Uiso 1 1 calc R . . H31B H 0.0201 0.3620 0.3785 0.153 Uiso 1 1 calc R . . C32 C 0.1139(5) 0.2462(13) 0.3901(4) 0.237(7) Uani 1 1 d . . . H32A H 0.1370 0.2822 0.4430 0.285 Uiso 1 1 calc R . . H32B H 0.1151 0.1579 0.3960 0.285 Uiso 1 1 calc R . . C33 C 0.1599(4) 0.2796(6) 0.3442(4) 0.098(2) Uani 1 1 d . . . H33A H 0.1921 0.2113 0.3354 0.118 Uiso 1 1 calc R . . H33B H 0.1970 0.3465 0.3685 0.118 Uiso 1 1 calc R . . H1 H 0.5843(19) 0.093(3) 0.4872(18) 0.019(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01556(11) 0.02515(13) 0.01473(11) 0.00143(10) 0.00292(8) -0.00051(10) F1 0.0363(12) 0.0551(15) 0.0490(13) -0.0023(11) -0.0029(10) -0.0040(11) O1 0.0465(18) 0.062(2) 0.094(3) 0.0032(19) 0.0250(18) 0.0066(15) N1 0.0211(12) 0.0299(16) 0.0168(12) 0.0014(10) 0.0052(10) -0.0023(11) C6 0.0273(17) 0.041(2) 0.0183(15) 0.0045(14) 0.0052(13) -0.0060(15) B1 0.044(2) 0.030(2) 0.035(2) -0.0019(18) 0.0107(19) -0.0013(19) F2 0.0399(12) 0.0757(17) 0.0328(12) -0.0012(11) 0.0018(10) 0.0028(11) O2 0.140(4) 0.120(4) 0.105(3) -0.016(3) 0.066(3) -0.045(3) N2 0.0179(12) 0.0293(15) 0.0174(12) -0.0001(11) 0.0036(10) -0.0003(11) C5 0.0209(16) 0.040(2) 0.0237(16) 0.0014(14) 0.0062(13) -0.0079(14) F3 0.100(2) 0.0299(15) 0.114(2) -0.0035(14) 0.0590(19) -0.0053(13) N3 0.0190(12) 0.0224(14) 0.0183(12) 0.0010(12) 0.0042(10) -0.0015(12) C4 0.0179(14) 0.030(2) 0.0213(14) -0.0017(12) 0.0049(12) -0.0002(12) F4 0.0890(19) 0.0550(16) 0.0473(14) -0.0038(11) 0.0391(14) 0.0037(13) C3 0.0210(15) 0.031(2) 0.0174(14) 0.0031(12) 0.0038(12) 0.0007(13) C2 0.0215(15) 0.0228(18) 0.0184(14) 0.0011(12) 0.0049(12) -0.0005(12) C7 0.0172(14) 0.0279(18) 0.0197(14) -0.0010(12) 0.0041(12) 0.0019(12) C8 0.0192(15) 0.0343(19) 0.0184(15) 0.0006(13) 0.0032(12) 0.0005(13) C9 0.0259(16) 0.0325(19) 0.0181(15) -0.0012(13) 0.0084(13) -0.0025(14) C10 0.0210(16) 0.038(2) 0.0265(16) 0.0007(14) 0.0105(13) -0.0027(14) C11 0.0179(15) 0.0334(19) 0.0220(15) 0.0014(13) 0.0049(12) -0.0012(13) C12 0.0180(15) 0.043(2) 0.0215(14) 0.0001(14) 0.0037(12) -0.0042(14) C13 0.0208(17) 0.062(3) 0.0317(18) 0.0020(17) 0.0024(14) -0.0062(16) C14 0.031(2) 0.063(3) 0.035(2) -0.0180(19) 0.0009(16) -0.0029(18) C15 0.0258(18) 0.055(3) 0.039(2) 0.0166(18) 0.0028(16) 0.0060(17) C16 0.0265(17) 0.050(2) 0.0202(16) 0.0053(15) 0.0108(14) -0.0014(16) C18 0.043(2) 0.057(3) 0.0276(18) -0.0009(17) 0.0161(17) 0.0010(19) C17 0.036(2) 0.096(4) 0.033(2) 0.012(2) 0.0158(17) -0.011(2) C19 0.059(3) 0.050(3) 0.035(2) 0.0115(18) 0.0229(19) 0.001(2) C20 0.0187(15) 0.0308(19) 0.0164(14) 0.0027(12) 0.0030(12) 0.0040(13) C21 0.0290(17) 0.032(2) 0.0252(16) -0.0008(14) 0.0093(14) -0.0007(14) C22 0.045(2) 0.034(2) 0.036(2) -0.0007(16) 0.0126(17) 0.0083(17) C23 0.040(2) 0.052(3) 0.043(2) -0.0051(18) 0.0175(18) 0.0151(19) C24 0.0269(18) 0.053(3) 0.042(2) 0.0026(18) 0.0172(16) 0.0056(17) C25 0.0258(16) 0.0358(19) 0.0293(17) 0.0025(15) 0.0096(14) 0.0002(15) C26 0.066(3) 0.070(4) 0.077(4) -0.004(3) 0.015(3) 0.003(3) C27 0.050(3) 0.054(4) 0.138(5) 0.015(3) 0.036(3) 0.006(2) C28 0.116(5) 0.065(4) 0.059(3) -0.005(3) 0.023(3) 0.036(3) C29 0.127(6) 0.040(4) 0.092(4) -0.005(3) 0.005(4) 0.008(3) C30 0.087(5) 0.072(4) 0.150(7) 0.025(4) 0.052(5) 0.001(3) C31 0.066(4) 0.269(11) 0.054(4) -0.024(5) 0.029(3) -0.006(5) C32 0.105(6) 0.53(2) 0.082(5) 0.129(9) 0.042(5) 0.088(10) C33 0.094(5) 0.094(5) 0.096(5) 0.008(4) 0.017(4) -0.021(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 N1 2.024(2) . ? Pd1 N2 2.045(2) . ? Pd1 N3 2.047(2) . ? Pd1 N3 2.053(2) 3_656 ? Pd1 Pd1 3.1099(4) 3_656 ? F1 B1 1.397(5) . ? O1 C29 1.412(5) . ? O1 C26 1.418(5) . ? N1 C6 1.334(4) . ? N1 C2 1.361(4) . ? C6 C5 1.376(4) . ? B1 F3 1.356(5) . ? B1 F4 1.377(5) . ? B1 F2 1.406(5) . ? O2 C30 1.434(7) . ? O2 C33 1.500(7) . ? N2 C11 1.341(4) . ? N2 C7 1.369(4) . ? C5 C4 1.388(4) . ? N3 C20 1.428(4) . ? N3 Pd1 2.053(2) 3_656 ? C4 C3 1.397(4) . ? C4 C12 1.525(4) . ? C3 C2 1.384(4) . ? C2 C7 1.477(4) . ? C7 C8 1.384(4) . ? C8 C9 1.397(4) . ? C9 C10 1.390(4) . ? C9 C16 1.529(4) . ? C10 C11 1.386(4) . ? C12 C13 1.538(4) . ? C12 C14 1.538(5) . ? C12 C15 1.543(5) . ? C16 C19 1.531(5) . ? C16 C18 1.532(5) . ? C16 C17 1.534(4) . ? C20 C21 1.389(5) . ? C20 C25 1.395(4) . ? C21 C22 1.384(5) . ? C22 C23 1.387(5) . ? C23 C24 1.382(6) . ? C24 C25 1.391(5) . ? C26 C27 1.468(6) . ? C27 C28 1.487(7) . ? C28 C29 1.493(8) . ? C30 C31 1.335(8) . ? C31 C32 1.474(9) . ? C32 C33 1.384(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 79.77(9) . . ? N1 Pd1 N3 176.29(11) . . ? N2 Pd1 N3 100.45(10) . . ? N1 Pd1 N3 98.81(10) . 3_656 ? N2 Pd1 N3 174.58(11) . 3_656 ? N3 Pd1 N3 81.31(11) . 3_656 ? N1 Pd1 Pd1 139.27(7) . 3_656 ? N2 Pd1 Pd1 140.94(7) . 3_656 ? N3 Pd1 Pd1 40.73(7) . 3_656 ? N3 Pd1 Pd1 40.58(7) 3_656 3_656 ? C29 O1 C26 109.7(4) . . ? C6 N1 C2 118.1(3) . . ? C6 N1 Pd1 125.9(2) . . ? C2 N1 Pd1 115.98(19) . . ? N1 C6 C5 123.0(3) . . ? F3 B1 F4 112.1(3) . . ? F3 B1 F1 110.6(3) . . ? F4 B1 F1 109.3(3) . . ? F3 B1 F2 109.7(3) . . ? F4 B1 F2 108.7(3) . . ? F1 B1 F2 106.2(3) . . ? C30 O2 C33 108.3(5) . . ? C11 N2 C7 117.7(2) . . ? C11 N2 Pd1 127.4(2) . . ? C7 N2 Pd1 114.89(19) . . ? C6 C5 C4 120.4(3) . . ? C20 N3 Pd1 113.49(19) . . ? C20 N3 Pd1 113.3(2) . 3_656 ? Pd1 N3 Pd1 98.69(11) . 3_656 ? C5 C4 C3 116.4(3) . . ? C5 C4 C12 122.4(3) . . ? C3 C4 C12 121.1(3) . . ? C2 C3 C4 120.8(3) . . ? N1 C2 C3 121.2(3) . . ? N1 C2 C7 114.5(2) . . ? C3 C2 C7 124.3(3) . . ? N2 C7 C8 121.6(3) . . ? N2 C7 C2 114.5(2) . . ? C8 C7 C2 123.8(3) . . ? C7 C8 C9 120.9(3) . . ? C10 C9 C8 116.5(3) . . ? C10 C9 C16 123.4(3) . . ? C8 C9 C16 120.1(3) . . ? C11 C10 C9 120.4(3) . . ? N2 C11 C10 122.8(3) . . ? C4 C12 C13 111.6(3) . . ? C4 C12 C14 107.8(3) . . ? C13 C12 C14 108.9(3) . . ? C4 C12 C15 110.1(3) . . ? C13 C12 C15 108.4(3) . . ? C14 C12 C15 109.9(3) . . ? C9 C16 C19 109.2(3) . . ? C9 C16 C18 109.2(3) . . ? C19 C16 C18 109.1(3) . . ? C9 C16 C17 112.1(3) . . ? C19 C16 C17 108.2(3) . . ? C18 C16 C17 109.0(3) . . ? C21 C20 C25 119.0(3) . . ? C21 C20 N3 119.4(3) . . ? C25 C20 N3 121.6(3) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C23 120.0(4) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C20 120.0(3) . . ? O1 C26 C27 107.8(4) . . ? C26 C27 C28 104.8(4) . . ? C27 C28 C29 105.3(4) . . ? O1 C29 C28 107.5(5) . . ? C31 C30 O2 108.0(6) . . ? C30 C31 C32 106.9(5) . . ? C33 C32 C31 110.0(6) . . ? C32 C33 O2 102.8(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H1 F1 0.80(3) 2.25(3) 3.022(4) 163(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.766 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.085 data_Pd2(NHtol)2(bpy)2(BF4)2_(12,Ar=tol) _database_code_depnum_ccdc_archive 'CCDC 663524' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H64 N6 Pd2 2+, 2(B F4 1-), 4(C H2 Cl2)' _chemical_formula_sum 'C54 H72 B2 Cl8 F8 N6 Pd2' _chemical_formula_weight 1475.20 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.627(4) _cell_length_b 24.551(8) _cell_length_c 11.490(4) _cell_angle_alpha 90.00 _cell_angle_beta 77.461(5) _cell_angle_gamma 90.00 _cell_volume 3201.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 946 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 27.07 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6456 _exptl_absorpt_correction_T_max 0.9102 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 19471 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.17 _reflns_number_total 7033 _reflns_number_gt 5786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+5.5886P] 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 7033 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.108257(19) 0.034388(9) 0.51337(2) 0.02004(8) Uani 1 1 d . . . Cl1 Cl -0.47055(11) 0.15508(5) 0.17605(11) 0.0564(3) Uani 1 1 d . . . F1 F -0.2353(3) 0.21495(14) 0.3952(3) 0.0901(11) Uani 1 1 d . . . N1 N 0.2529(2) 0.02823(10) 0.5852(2) 0.0213(5) Uani 1 1 d . . . B1 B -0.2728(4) 0.17232(19) 0.4690(4) 0.0392(10) Uiso 1 1 d . . . H1 H -0.074(3) 0.0678(17) 0.458(3) 0.034(10) Uiso 1 1 d . . . Cl2 Cl -0.24388(14) 0.13488(8) 0.01820(19) 0.0991(6) Uani 1 1 d . . . F2 F -0.3420(3) 0.13800(13) 0.4184(3) 0.0863(11) Uani 1 1 d . . . N3 N -0.0304(2) 0.03871(10) 0.4292(2) 0.0198(5) Uani 1 1 d . . . C2 C 0.3229(3) 0.07283(12) 0.5731(3) 0.0210(6) Uani 1 1 d . . . Cl3 Cl -0.01764(18) 0.26089(7) 0.65753(19) 0.1116(7) Uani 1 1 d . . . F3 F -0.3402(3) 0.19137(12) 0.5734(2) 0.0700(9) Uani 1 1 d . . . C3 C 0.4222(3) 0.07458(12) 0.6221(3) 0.0219(6) Uani 1 1 d . . . H3 H 0.4704 0.1062 0.6121 0.026 Uiso 1 1 calc R . . Cl4 Cl 0.00574(19) 0.15394(9) 0.74930(18) 0.1146(7) Uani 1 1 d . . . F4 F -0.1778(2) 0.14193(10) 0.4928(2) 0.0530(6) Uani 1 1 d . . . C4 C 0.4516(3) 0.03007(13) 0.6862(3) 0.0227(6) Uani 1 1 d . . . C5 C 0.3819(3) -0.01608(13) 0.6904(3) 0.0264(7) Uani 1 1 d . . . H5 H 0.4012 -0.0481 0.7285 0.032 Uiso 1 1 calc R . . C6 C 0.2846(3) -0.01564(13) 0.6397(3) 0.0270(7) Uani 1 1 d . . . H6 H 0.2383 -0.0478 0.6436 0.032 Uiso 1 1 calc R . . C7 C 0.5503(3) 0.03293(13) 0.7555(3) 0.0252(6) Uani 1 1 d . . . C8 C 0.6465(4) 0.07268(19) 0.6996(4) 0.0498(11) Uani 1 1 d . . . H8A H 0.7092 0.0722 0.7445 0.075 Uiso 1 1 calc R . . H8B H 0.6134 0.1095 0.7015 0.075 Uiso 1 1 calc R . . H8C H 0.6790 0.0621 0.6168 0.075 Uiso 1 1 calc R . . C9 C 0.6045(4) -0.02254(16) 0.7646(4) 0.0458(10) Uani 1 1 d . . . H9A H 0.6341 -0.0373 0.6844 0.069 Uiso 1 1 calc R . . H9B H 0.5448 -0.0471 0.8097 0.069 Uiso 1 1 calc R . . H9C H 0.6698 -0.0191 0.8055 0.069 Uiso 1 1 calc R . . N2 N 0.1815(2) 0.10922(10) 0.4710(2) 0.0214(5) Uani 1 1 d . . . C10 C 0.4939(4) 0.0539(2) 0.8808(4) 0.0544(12) Uani 1 1 d . . . H10A H 0.4353 0.0275 0.9210 0.082 Uiso 1 1 calc R . . H10B H 0.4555 0.0889 0.8745 0.082 Uiso 1 1 calc R . . H10C H 0.5550 0.0585 0.9269 0.082 Uiso 1 1 calc R . . C12 C 0.2833(3) 0.11876(12) 0.5073(3) 0.0213(6) Uani 1 1 d . . . C13 C 0.3417(3) 0.16827(13) 0.4863(3) 0.0229(6) Uani 1 1 d . . . H13 H 0.4141 0.1733 0.5104 0.028 Uiso 1 1 calc R . . C14 C 0.2952(3) 0.21084(13) 0.4299(3) 0.0244(6) Uani 1 1 d . . . C15 C 0.1889(3) 0.20028(13) 0.3974(3) 0.0293(7) Uani 1 1 d . . . H15 H 0.1527 0.2280 0.3602 0.035 Uiso 1 1 calc R . . C16 C 0.1353(3) 0.15005(13) 0.4184(3) 0.0285(7) Uani 1 1 d . . . H16 H 0.0630 0.1441 0.3948 0.034 Uiso 1 1 calc R . . C17 C 0.3529(3) 0.26719(13) 0.4096(3) 0.0278(7) Uani 1 1 d . . . C18 C 0.4810(3) 0.26590(15) 0.4225(4) 0.0353(8) Uani 1 1 d . . . H18A H 0.4838 0.2553 0.5041 0.053 Uiso 1 1 calc R . . H18B H 0.5161 0.3021 0.4054 0.053 Uiso 1 1 calc R . . H18C H 0.5253 0.2394 0.3663 0.053 Uiso 1 1 calc R . . C19 C 0.2819(3) 0.30582(14) 0.5038(4) 0.0389(9) Uani 1 1 d . . . H19A H 0.2022 0.3101 0.4898 0.058 Uiso 1 1 calc R . . H19B H 0.3209 0.3414 0.4981 0.058 Uiso 1 1 calc R . . H19C H 0.2774 0.2906 0.5835 0.058 Uiso 1 1 calc R . . C20 C 0.3500(4) 0.28818(16) 0.2845(4) 0.0431(10) Uani 1 1 d . . . H20A H 0.3904 0.2622 0.2247 0.065 Uiso 1 1 calc R . . H20B H 0.3898 0.3236 0.2716 0.065 Uiso 1 1 calc R . . H20C H 0.2680 0.2922 0.2773 0.065 Uiso 1 1 calc R . . C21 C 0.0092(3) 0.04192(12) 0.3022(3) 0.0216(6) Uani 1 1 d . . . C22 C 0.0793(3) 0.00016(14) 0.2411(3) 0.0280(7) Uani 1 1 d . . . H22 H 0.0975 -0.0307 0.2837 0.034 Uiso 1 1 calc R . . C23 C 0.1221(3) 0.00343(15) 0.1191(3) 0.0333(8) Uani 1 1 d . . . H23 H 0.1696 -0.0254 0.0794 0.040 Uiso 1 1 calc R . . C24 C 0.0975(3) 0.04774(16) 0.0529(3) 0.0323(8) Uani 1 1 d . . . C25 C 0.0254(3) 0.08849(15) 0.1136(3) 0.0320(7) Uani 1 1 d . . . H25 H 0.0061 0.1189 0.0704 0.038 Uiso 1 1 calc R . . C26 C -0.0192(3) 0.08570(13) 0.2360(3) 0.0270(7) Uani 1 1 d . . . H26 H -0.0693 0.1138 0.2749 0.032 Uiso 1 1 calc R . . C27 C 0.1470(4) 0.0513(2) -0.0794(3) 0.0467(10) Uani 1 1 d . . . H27A H 0.2235 0.0698 -0.0940 0.070 Uiso 1 1 calc R . . H27B H 0.0926 0.0718 -0.1170 0.070 Uiso 1 1 calc R . . H27C H 0.1571 0.0145 -0.1131 0.070 Uiso 1 1 calc R . . C1S C -0.3247(4) 0.17788(17) 0.1275(4) 0.0493(10) Uani 1 1 d . . . H1S1 H -0.3251 0.2152 0.0948 0.059 Uiso 1 1 calc R . . H1S2 H -0.2862 0.1794 0.1963 0.059 Uiso 1 1 calc R . . C2S C -0.0930(4) 0.20349(19) 0.7206(5) 0.0557(11) Uani 1 1 d . . . H2S1 H -0.1398 0.1885 0.6657 0.067 Uiso 1 1 calc R . . H2S2 H -0.1480 0.2136 0.7960 0.067 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 Pd1 0.02038(12) 0.01711(12) 0.02510(13) 0.00103(9) -0.01037(9) -0.00104(9) Cl1 0.0602(7) 0.0452(6) 0.0655(7) 0.0144(5) -0.0172(6) -0.0059(5) F1 0.083(2) 0.072(2) 0.102(3) 0.0484(19) 0.0071(19) -0.0087(18) N1 0.0219(12) 0.0171(12) 0.0263(13) 0.0004(10) -0.0083(10) -0.0007(10) Cl2 0.0689(9) 0.0983(12) 0.1288(15) -0.0523(11) -0.0188(9) 0.0253(9) F2 0.110(3) 0.0547(18) 0.116(3) -0.0107(18) -0.073(2) 0.0081(18) N3 0.0198(12) 0.0154(12) 0.0261(13) 0.0008(10) -0.0093(10) 0.0004(10) C2 0.0245(15) 0.0187(14) 0.0203(15) -0.0012(11) -0.0058(12) 0.0006(12) Cl3 0.1103(14) 0.0595(9) 0.1304(16) 0.0091(9) 0.0494(12) -0.0058(9) F3 0.084(2) 0.0573(17) 0.0573(17) 0.0079(13) 0.0106(15) 0.0352(15) C3 0.0227(15) 0.0191(14) 0.0250(15) 0.0003(12) -0.0074(12) -0.0014(11) Cl4 0.1246(15) 0.1083(14) 0.0962(13) 0.0096(10) 0.0084(11) 0.0692(12) F4 0.0421(13) 0.0531(15) 0.0626(16) -0.0047(12) -0.0081(12) 0.0132(11) C4 0.0212(14) 0.0237(15) 0.0240(15) -0.0013(12) -0.0069(12) 0.0010(12) C5 0.0269(16) 0.0227(15) 0.0327(18) 0.0058(13) -0.0130(14) -0.0004(12) C6 0.0278(16) 0.0214(15) 0.0354(18) 0.0036(13) -0.0151(14) -0.0047(12) C7 0.0237(15) 0.0261(16) 0.0289(16) 0.0014(13) -0.0125(12) 0.0000(13) C8 0.038(2) 0.056(3) 0.065(3) 0.027(2) -0.031(2) -0.0196(19) C9 0.039(2) 0.033(2) 0.076(3) -0.0054(19) -0.035(2) 0.0063(16) N2 0.0233(13) 0.0180(12) 0.0251(13) 0.0000(10) -0.0097(10) 0.0003(10) C10 0.045(2) 0.082(3) 0.042(2) -0.019(2) -0.0225(19) 0.012(2) C12 0.0212(14) 0.0229(15) 0.0203(15) -0.0016(11) -0.0058(12) 0.0010(11) C13 0.0239(15) 0.0234(15) 0.0229(15) 0.0010(12) -0.0080(12) -0.0020(12) C14 0.0279(16) 0.0216(15) 0.0239(16) 0.0017(12) -0.0061(13) -0.0007(12) C15 0.0334(18) 0.0219(16) 0.0373(19) 0.0068(13) -0.0183(15) -0.0007(13) C16 0.0307(17) 0.0234(16) 0.0362(18) 0.0020(13) -0.0180(14) -0.0003(13) C17 0.0325(17) 0.0194(15) 0.0328(18) 0.0044(13) -0.0102(14) -0.0039(13) C18 0.0343(19) 0.0280(18) 0.045(2) 0.0059(15) -0.0109(16) -0.0068(14) C19 0.042(2) 0.0219(17) 0.053(2) -0.0019(16) -0.0090(18) -0.0008(15) C20 0.054(2) 0.037(2) 0.043(2) 0.0157(17) -0.0202(19) -0.0130(18) C21 0.0190(14) 0.0221(15) 0.0262(15) -0.0005(12) -0.0104(12) -0.0036(11) C22 0.0232(15) 0.0267(17) 0.0361(18) -0.0020(13) -0.0107(14) 0.0015(13) C23 0.0239(16) 0.039(2) 0.0374(19) -0.0109(15) -0.0066(14) 0.0014(14) C24 0.0255(17) 0.044(2) 0.0286(17) -0.0031(15) -0.0082(14) -0.0091(14) C25 0.0336(18) 0.0355(19) 0.0290(18) 0.0067(14) -0.0118(14) -0.0061(15) C26 0.0259(16) 0.0258(16) 0.0308(17) 0.0015(13) -0.0092(13) 0.0006(13) C27 0.037(2) 0.069(3) 0.033(2) -0.0035(19) -0.0039(16) -0.013(2) C1S 0.056(3) 0.034(2) 0.060(3) -0.0018(19) -0.016(2) -0.0045(19) C2S 0.054(3) 0.045(3) 0.065(3) -0.006(2) -0.005(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.034(3) . ? Pd1 N2 2.039(3) . ? Pd1 N3 2.053(3) 3_556 ? Pd1 N3 2.055(2) . ? Pd1 Pd1 3.1015(8) 3_556 ? Cl1 C1S 1.758(5) . ? F1 B1 1.358(5) . ? N1 C6 1.337(4) . ? N1 C2 1.353(4) . ? B1 F3 1.365(5) . ? B1 F2 1.378(5) . ? B1 F4 1.407(5) . ? Cl2 C1S 1.750(5) . ? N3 C21 1.434(4) . ? N3 Pd1 2.053(3) 3_556 ? C2 C3 1.390(4) . ? C2 C12 1.485(4) . ? Cl3 C2S 1.733(5) . ? C3 C4 1.401(4) . ? Cl4 C2S 1.752(5) . ? C4 C5 1.388(4) . ? C4 C7 1.534(4) . ? C5 C6 1.381(4) . ? C7 C9 1.514(5) . ? C7 C8 1.518(5) . ? C7 C10 1.536(5) . ? N2 C16 1.341(4) . ? N2 C12 1.358(4) . ? C12 C13 1.387(4) . ? C13 C14 1.398(4) . ? C14 C15 1.391(4) . ? C14 C17 1.533(4) . ? C15 C16 1.379(5) . ? C17 C18 1.529(5) . ? C17 C20 1.535(5) . ? C17 C19 1.537(5) . ? C21 C26 1.397(4) . ? C21 C22 1.399(4) . ? C22 C23 1.385(5) . ? C23 C24 1.392(5) . ? C24 C25 1.392(5) . ? C24 C27 1.506(5) . ? C25 C26 1.391(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 N1 Pd1 N2 79.89(10) . . ? N1 Pd1 N3 98.64(10) . 3_556 ? N2 Pd1 N3 175.11(10) . 3_556 ? N1 Pd1 N3 175.83(10) . . ? N2 Pd1 N3 99.85(10) . . ? N3 Pd1 N3 81.96(10) 3_556 . ? N1 Pd1 Pd1 139.49(7) . 3_556 ? N2 Pd1 Pd1 140.61(7) . 3_556 ? N3 Pd1 Pd1 41.01(7) 3_556 3_556 ? N3 Pd1 Pd1 40.96(7) . 3_556 ? C6 N1 C2 118.7(3) . . ? C6 N1 Pd1 125.9(2) . . ? C2 N1 Pd1 115.46(19) . . ? F1 B1 F3 109.3(4) . . ? F1 B1 F2 110.2(4) . . ? F3 B1 F2 107.6(4) . . ? F1 B1 F4 111.8(4) . . ? F3 B1 F4 109.6(3) . . ? F2 B1 F4 108.2(4) . . ? C21 N3 Pd1 113.38(18) . 3_556 ? C21 N3 Pd1 111.70(18) . . ? Pd1 N3 Pd1 98.04(10) 3_556 . ? N1 C2 C3 121.1(3) . . ? N1 C2 C12 114.9(3) . . ? C3 C2 C12 124.0(3) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C7 121.1(3) . . ? C3 C4 C7 122.2(3) . . ? C6 C5 C4 120.3(3) . . ? N1 C6 C5 122.5(3) . . ? C9 C7 C8 109.2(3) . . ? C9 C7 C4 111.4(3) . . ? C8 C7 C4 112.1(3) . . ? C9 C7 C10 109.6(3) . . ? C8 C7 C10 107.9(3) . . ? C4 C7 C10 106.7(3) . . ? C16 N2 C12 118.0(3) . . ? C16 N2 Pd1 126.4(2) . . ? C12 N2 Pd1 115.40(19) . . ? N2 C12 C13 121.6(3) . . ? N2 C12 C2 114.4(3) . . ? C13 C12 C2 124.0(3) . . ? C12 C13 C14 120.8(3) . . ? C15 C14 C13 116.1(3) . . ? C15 C14 C17 120.8(3) . . ? C13 C14 C17 123.0(3) . . ? C16 C15 C14 120.9(3) . . ? N2 C16 C15 122.5(3) . . ? C18 C17 C14 111.7(3) . . ? C18 C17 C20 108.5(3) . . ? C14 C17 C20 110.3(3) . . ? C18 C17 C19 109.3(3) . . ? C14 C17 C19 107.4(3) . . ? C20 C17 C19 109.5(3) . . ? C26 C21 C22 118.1(3) . . ? C26 C21 N3 122.3(3) . . ? C22 C21 N3 119.6(3) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 121.8(3) . . ? C25 C24 C23 117.5(3) . . ? C25 C24 C27 121.4(3) . . ? C23 C24 C27 121.1(4) . . ? C26 C25 C24 121.5(3) . . ? C25 C26 C21 120.5(3) . . ? Cl2 C1S Cl1 111.5(2) . . ? Cl3 C2S Cl4 110.5(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.17 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.304 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.095 data_[Pd(t-Bu2bpy)(OTf)2_(16) _database_code_depnum_ccdc_archive 'CCDC 663525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 F6 N2 O6 Pd S2' _chemical_formula_weight 672.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.7290(12) _cell_length_b 14.0562(7) _cell_length_c 19.0437(9) _cell_angle_alpha 90.00 _cell_angle_beta 127.6470(10) _cell_angle_gamma 90.00 _cell_volume 5241.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5898 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.11 _exptl_crystal_description PRISM _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6485 _exptl_absorpt_correction_T_max 0.8330 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 18397 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.12 _reflns_number_total 5769 _reflns_number_gt 5051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+4.8028P] 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 5769 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0680 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.249293(8) 0.644502(11) 0.347392(9) 0.02775(6) Uani 1 1 d . . . S1 S 0.29356(3) 0.43957(4) 0.43205(3) 0.03772(13) Uani 1 1 d . . . F1 F 0.16696(8) 0.39172(16) 0.30792(12) 0.0712(5) Uani 1 1 d . . . O1 O 0.28732(8) 0.50908(10) 0.36903(9) 0.0358(3) Uani 1 1 d . . . N1 N 0.18041(9) 0.62352(12) 0.21812(10) 0.0282(4) Uani 1 1 d . . . C1 C 0.17632(11) 0.54522(15) 0.17478(13) 0.0329(5) Uani 1 1 d . . . H1 H 0.2035 0.4915 0.2079 0.039 Uiso 1 1 calc R . . S2 S 0.38854(3) 0.72442(4) 0.50566(3) 0.03390(12) Uani 1 1 d . . . F2 F 0.23878(9) 0.31838(12) 0.30068(11) 0.0596(4) Uani 1 1 d . . . O2 O 0.27101(12) 0.47549(14) 0.48003(12) 0.0611(5) Uani 1 1 d . . . N2 N 0.20559(8) 0.77084(12) 0.31422(10) 0.0278(4) Uani 1 1 d . . . C2 C 0.13387(11) 0.54073(15) 0.08355(13) 0.0332(5) Uani 1 1 d . . . H2 H 0.1322 0.4843 0.0548 0.040 Uiso 1 1 calc R . . F3 F 0.22828(12) 0.28144(13) 0.40163(13) 0.0805(6) Uani 1 1 d . . . O3 O 0.35599(10) 0.38771(14) 0.47737(13) 0.0640(6) Uani 1 1 d . . . C3 C 0.09336(10) 0.61847(15) 0.03301(13) 0.0290(4) Uani 1 1 d . A . F4 F 0.38528(10) 0.81308(15) 0.62311(12) 0.0755(5) Uani 1 1 d . . . O4 O 0.32402(8) 0.67892(11) 0.47835(9) 0.0374(4) Uani 1 1 d . . . C4 C 0.09805(10) 0.69877(15) 0.07915(13) 0.0296(4) Uani 1 1 d . . . H4 H 0.0709 0.7530 0.0472 0.036 Uiso 1 1 calc R . . F5 F 0.48550(8) 0.79443(13) 0.65885(9) 0.0665(5) Uani 1 1 d . . . O5 O 0.43626(10) 0.66082(14) 0.51206(13) 0.0569(5) Uani 1 1 d . . . C5 C 0.14182(10) 0.70079(14) 0.17101(12) 0.0267(4) Uani 1 1 d . . . F6 F 0.43322(9) 0.67681(14) 0.66514(9) 0.0748(6) Uani 1 1 d . . . O6 O 0.37808(9) 0.81384(12) 0.46341(11) 0.0465(4) Uani 1 1 d . . . C6 C 0.15397(10) 0.78372(14) 0.22588(12) 0.0268(4) Uani 1 1 d . . . C7 C 0.11892(10) 0.86883(14) 0.19458(13) 0.0291(4) Uani 1 1 d . . . H7 H 0.0831 0.8762 0.1330 0.035 Uiso 1 1 calc R . . C8 C 0.13546(10) 0.94423(15) 0.25243(13) 0.0288(4) Uani 1 1 d . B . C9 C 0.18841(11) 0.92812(15) 0.34223(13) 0.0331(5) Uani 1 1 d . . . H9 H 0.2017 0.9774 0.3840 0.040 Uiso 1 1 calc R . . C10 C 0.22147(11) 0.84205(15) 0.37086(13) 0.0336(5) Uani 1 1 d . . . H10 H 0.2566 0.8326 0.4324 0.040 Uiso 1 1 calc R . . C11 C 0.04850(11) 0.61530(16) -0.06815(13) 0.0342(5) Uani 1 1 d . . . C14 C 0.0961(3) 0.5952(6) -0.0932(3) 0.075(2) Uani 0.636(8) 1 d P A 1 H14A H 0.1217 0.5365 -0.0642 0.112 Uiso 0.636(8) 1 calc PR A 1 H14B H 0.1280 0.6484 -0.0737 0.112 Uiso 0.636(8) 1 calc PR A 1 H14C H 0.0687 0.5881 -0.1577 0.112 Uiso 0.636(8) 1 calc PR A 1 C13 C -0.0010(3) 0.5309(5) -0.1000(3) 0.0641(18) Uani 0.636(8) 1 d P A 1 H13A H 0.0252 0.4722 -0.0722 0.096 Uiso 0.636(8) 1 calc PR A 1 H13B H -0.0285 0.5252 -0.1646 0.096 Uiso 0.636(8) 1 calc PR A 1 H13C H -0.0311 0.5414 -0.0835 0.096 Uiso 0.636(8) 1 calc PR A 1 C12 C 0.0092(3) 0.7041(4) -0.1108(2) 0.0586(19) Uani 0.636(8) 1 d P A 1 H12A H -0.0184 0.6978 -0.1754 0.088 Uiso 0.636(8) 1 calc PR A 1 H12B H 0.0409 0.7576 -0.0910 0.088 Uiso 0.636(8) 1 calc PR A 1 H12C H -0.0208 0.7156 -0.0943 0.088 Uiso 0.636(8) 1 calc PR A 1 C15 C 0.09874(11) 1.03984(15) 0.22124(14) 0.0325(4) Uani 1 1 d . . . C16 C 0.0261(8) 1.0320(11) 0.1386(9) 0.045(3) Uani 0.45(2) 1 d P B 1 H16A H 0.0050 1.0952 0.1216 0.068 Uiso 0.45(2) 1 calc PR B 1 H16B H 0.0005 0.9900 0.1498 0.068 Uiso 0.45(2) 1 calc PR B 1 H16C H 0.0255 1.0057 0.0904 0.068 Uiso 0.45(2) 1 calc PR B 1 C17 C 0.0979(6) 1.0896(8) 0.2944(6) 0.041(2) Uani 0.45(2) 1 d P B 1 H17A H 0.1447 1.0951 0.3493 0.061 Uiso 0.45(2) 1 calc PR B 1 H17B H 0.0706 1.0516 0.3055 0.061 Uiso 0.45(2) 1 calc PR B 1 H17C H 0.0778 1.1532 0.2740 0.061 Uiso 0.45(2) 1 calc PR B 1 C18' C 0.1461(9) 1.1174(13) 0.2316(12) 0.047(3) Uani 0.55(2) 1 d P B 2 H18A H 0.1217 1.1783 0.2113 0.070 Uiso 0.55(2) 1 calc PR B 2 H18B H 0.1612 1.1013 0.1959 0.070 Uiso 0.55(2) 1 calc PR B 2 H18C H 0.1859 1.1227 0.2941 0.070 Uiso 0.55(2) 1 calc PR B 2 C19 C 0.22846(14) 0.35260(18) 0.35708(18) 0.0466(6) Uani 1 1 d . . . C20 C 0.42499(14) 0.7536(2) 0.61967(15) 0.0495(7) Uani 1 1 d . . . C12' C -0.0229(4) 0.6604(8) -0.1053(5) 0.059(3) Uani 0.364(8) 1 d P A 2 H12D H -0.0161 0.7251 -0.0820 0.088 Uiso 0.364(8) 1 calc PR A 2 H12E H -0.0451 0.6215 -0.0868 0.088 Uiso 0.364(8) 1 calc PR A 2 H12F H -0.0519 0.6626 -0.1702 0.088 Uiso 0.364(8) 1 calc PR A 2 C13' C 0.0372(8) 0.5190(7) -0.1063(5) 0.087(5) Uani 0.364(8) 1 d P A 2 H13D H 0.0082 0.5234 -0.1711 0.130 Uiso 0.364(8) 1 calc PR A 2 H13E H 0.0147 0.4791 -0.0888 0.130 Uiso 0.364(8) 1 calc PR A 2 H13F H 0.0812 0.4906 -0.0841 0.130 Uiso 0.364(8) 1 calc PR A 2 C14' C 0.0802(5) 0.6833(10) -0.0984(5) 0.075(4) Uani 0.364(8) 1 d P A 2 H14D H 0.0877 0.7460 -0.0713 0.112 Uiso 0.364(8) 1 calc PR A 2 H14E H 0.0490 0.6895 -0.1632 0.112 Uiso 0.364(8) 1 calc PR A 2 H14F H 0.1239 0.6574 -0.0800 0.112 Uiso 0.364(8) 1 calc PR A 2 C16' C 0.0379(7) 1.0348(8) 0.1197(9) 0.063(3) Uani 0.55(2) 1 d P B 2 H16D H 0.0045 0.9879 0.1095 0.095 Uiso 0.55(2) 1 calc PR B 2 H16E H 0.0551 1.0161 0.0871 0.095 Uiso 0.55(2) 1 calc PR B 2 H16F H 0.0161 1.0974 0.0991 0.095 Uiso 0.55(2) 1 calc PR B 2 C17' C 0.0738(9) 1.0591(11) 0.2752(12) 0.078(4) Uani 0.55(2) 1 d P B 2 H17D H 0.0424 1.0085 0.2647 0.117 Uiso 0.55(2) 1 calc PR B 2 H17E H 0.0501 1.1204 0.2576 0.117 Uiso 0.55(2) 1 calc PR B 2 H17F H 0.1129 1.0608 0.3384 0.117 Uiso 0.55(2) 1 calc PR B 2 C18 C 0.1413(13) 1.1037(17) 0.2106(16) 0.056(5) Uani 0.45(2) 1 d P B 1 H18D H 0.1880 1.1056 0.2661 0.084 Uiso 0.45(2) 1 calc PR B 1 H18E H 0.1219 1.1680 0.1957 0.084 Uiso 0.45(2) 1 calc PR B 1 H18F H 0.1421 1.0796 0.1629 0.084 Uiso 0.45(2) 1 calc PR B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02796(9) 0.02543(9) 0.02036(8) -0.00054(5) 0.00988(7) 0.00046(6) S1 0.0430(3) 0.0290(3) 0.0259(2) 0.0011(2) 0.0132(2) 0.0005(2) F1 0.0390(9) 0.1045(14) 0.0662(11) -0.0219(10) 0.0301(8) -0.0138(9) O1 0.0422(9) 0.0288(8) 0.0286(7) 0.0025(6) 0.0176(7) 0.0042(6) N1 0.0255(8) 0.0280(9) 0.0227(8) -0.0012(6) 0.0105(7) -0.0005(7) C1 0.0325(11) 0.0268(10) 0.0280(10) -0.0005(8) 0.0127(9) 0.0032(8) S2 0.0337(3) 0.0300(3) 0.0239(2) 0.00192(19) 0.0104(2) 0.0012(2) F2 0.0697(11) 0.0570(10) 0.0698(10) -0.0322(8) 0.0516(9) -0.0227(8) O2 0.0995(16) 0.0475(11) 0.0454(10) -0.0092(8) 0.0490(11) -0.0089(10) N2 0.0267(8) 0.0290(9) 0.0218(7) -0.0025(6) 0.0117(7) 0.0011(7) C2 0.0348(11) 0.0295(11) 0.0280(10) -0.0048(8) 0.0154(9) 0.0012(9) F3 0.1171(16) 0.0560(11) 0.0840(13) -0.0119(9) 0.0694(13) -0.0360(11) O3 0.0475(11) 0.0464(11) 0.0557(11) 0.0143(9) 0.0097(9) 0.0100(9) C3 0.0283(10) 0.0293(10) 0.0252(9) -0.0030(8) 0.0142(8) -0.0035(8) F4 0.0837(13) 0.0869(13) 0.0630(11) -0.0358(10) 0.0485(10) -0.0232(11) O4 0.0364(8) 0.0346(8) 0.0224(7) -0.0002(6) 0.0084(6) -0.0044(7) C4 0.0282(10) 0.0288(10) 0.0241(9) -0.0006(8) 0.0120(8) -0.0002(8) F5 0.0535(9) 0.0826(12) 0.0352(7) -0.0081(8) 0.0127(7) -0.0347(9) O5 0.0500(11) 0.0500(11) 0.0604(12) 0.0011(9) 0.0285(10) 0.0114(9) C5 0.0259(10) 0.0259(10) 0.0245(9) -0.0010(7) 0.0134(8) -0.0002(8) F6 0.0687(11) 0.0902(13) 0.0276(7) 0.0134(8) 0.0099(7) -0.0322(10) O6 0.0482(10) 0.0383(9) 0.0402(9) 0.0114(7) 0.0204(8) 0.0004(8) C6 0.0251(9) 0.0307(10) 0.0228(9) -0.0027(7) 0.0137(8) -0.0032(8) C7 0.0264(10) 0.0310(11) 0.0242(9) -0.0009(8) 0.0125(8) -0.0003(8) C8 0.0257(10) 0.0295(10) 0.0302(10) -0.0023(8) 0.0165(9) -0.0015(8) C9 0.0332(11) 0.0322(11) 0.0280(10) -0.0061(8) 0.0156(9) 0.0008(9) C10 0.0335(11) 0.0354(12) 0.0234(9) -0.0049(8) 0.0130(9) 0.0004(9) C11 0.0359(11) 0.0343(11) 0.0231(9) -0.0035(8) 0.0133(9) -0.0009(9) C14 0.054(3) 0.138(7) 0.036(2) -0.003(3) 0.029(2) 0.009(3) C13 0.063(4) 0.056(3) 0.031(2) -0.007(2) 0.007(2) -0.021(3) C12 0.074(4) 0.046(3) 0.0223(18) -0.0014(16) 0.012(2) 0.011(2) C15 0.0292(11) 0.0306(11) 0.0340(11) -0.0027(8) 0.0173(9) 0.0018(8) C16 0.034(4) 0.045(4) 0.034(4) -0.013(3) 0.010(3) 0.008(3) C17 0.048(4) 0.037(5) 0.042(4) -0.004(3) 0.030(3) 0.008(3) C18' 0.034(3) 0.023(4) 0.075(6) -0.012(4) 0.029(4) -0.006(3) C19 0.0528(15) 0.0445(14) 0.0512(15) -0.0123(11) 0.0362(13) -0.0132(12) C20 0.0486(15) 0.0560(16) 0.0273(11) -0.0079(10) 0.0145(11) -0.0191(13) C12' 0.040(4) 0.079(7) 0.027(3) -0.009(4) 0.005(3) 0.009(4) C13' 0.119(12) 0.046(5) 0.022(3) -0.012(3) 0.006(5) 0.015(6) C14' 0.081(7) 0.123(10) 0.030(4) -0.024(5) 0.038(4) -0.046(7) C16' 0.046(5) 0.026(3) 0.055(6) -0.001(3) 0.000(3) 0.010(3) C17' 0.103(9) 0.058(6) 0.135(10) 0.037(6) 0.105(9) 0.043(6) C18 0.067(10) 0.025(7) 0.093(12) 0.007(7) 0.058(10) 0.013(6) _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 N2 1.9715(17) . ? Pd1 N1 1.9815(16) . ? Pd1 O1 2.0503(15) . ? Pd1 O4 2.0589(14) . ? S1 O2 1.423(2) . ? S1 O3 1.425(2) . ? S1 O1 1.4806(15) . ? S1 C19 1.821(3) . ? F1 C19 1.324(3) . ? N1 C1 1.342(3) . ? N1 C5 1.360(3) . ? C1 C2 1.377(3) . ? S2 O5 1.4250(19) . ? S2 O6 1.4282(17) . ? S2 O4 1.4873(17) . ? S2 C20 1.818(2) . ? F2 C19 1.336(3) . ? N2 C10 1.342(3) . ? N2 C6 1.367(2) . ? C2 C3 1.395(3) . ? F3 C19 1.313(3) . ? C3 C4 1.391(3) . ? C3 C11 1.528(3) . ? F4 C20 1.321(3) . ? C4 C5 1.385(3) . ? F5 C20 1.327(3) . ? C5 C6 1.469(3) . ? F6 C20 1.320(3) . ? C6 C7 1.381(3) . ? C7 C8 1.398(3) . ? C8 C9 1.398(3) . ? C8 C15 1.525(3) . ? C9 C10 1.373(3) . ? C11 C13' 1.480(9) . ? C11 C12 1.483(5) . ? C11 C13 1.538(5) . ? C11 C14 1.542(5) . ? C11 C14' 1.553(9) . ? C11 C12' 1.580(8) . ? C15 C18 1.49(3) . ? C15 C16 1.504(15) . ? C15 C17' 1.511(10) . ? C15 C18' 1.523(19) . ? C15 C16' 1.566(13) . ? C15 C17 1.572(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 81.31(7) . . ? N2 Pd1 O1 174.27(6) . . ? N1 Pd1 O1 92.99(6) . . ? N2 Pd1 O4 95.00(6) . . ? N1 Pd1 O4 173.92(7) . . ? O1 Pd1 O4 90.72(6) . . ? O2 S1 O3 119.81(13) . . ? O2 S1 O1 113.50(11) . . ? O3 S1 O1 111.50(12) . . ? O2 S1 C19 103.65(13) . . ? O3 S1 C19 104.08(13) . . ? O1 S1 C19 101.71(11) . . ? S1 O1 Pd1 125.69(9) . . ? C1 N1 C5 119.36(17) . . ? C1 N1 Pd1 124.81(14) . . ? C5 N1 Pd1 115.16(13) . . ? N1 C1 C2 121.78(19) . . ? O5 S2 O6 117.12(12) . . ? O5 S2 O4 114.56(11) . . ? O6 S2 O4 113.27(10) . . ? O5 S2 C20 105.00(13) . . ? O6 S2 C20 105.15(12) . . ? O4 S2 C20 99.09(11) . . ? C10 N2 C6 119.01(17) . . ? C10 N2 Pd1 125.46(14) . . ? C6 N2 Pd1 115.51(13) . . ? C1 C2 C3 120.48(19) . . ? C4 C3 C2 116.88(18) . . ? C4 C3 C11 122.44(19) . . ? C2 C3 C11 120.63(18) . . ? S2 O4 Pd1 120.13(9) . . ? C5 C4 C3 120.90(19) . . ? N1 C5 C4 120.59(18) . . ? N1 C5 C6 114.09(16) . . ? C4 C5 C6 125.25(18) . . ? N2 C6 C7 120.93(17) . . ? N2 C6 C5 113.70(17) . . ? C7 C6 C5 125.36(17) . . ? C6 C7 C8 120.82(18) . . ? C7 C8 C9 116.48(19) . . ? C7 C8 C15 122.91(18) . . ? C9 C8 C15 120.61(18) . . ? C10 C9 C8 120.94(19) . . ? N2 C10 C9 121.80(19) . . ? C13' C11 C12 129.6(4) . . ? C13' C11 C3 114.8(4) . . ? C12 C11 C3 113.3(2) . . ? C13' C11 C13 40.0(6) . . ? C12 C11 C13 109.7(4) . . ? C3 C11 C13 108.1(3) . . ? C13' C11 C14 68.4(7) . . ? C12 C11 C14 110.6(4) . . ? C3 C11 C14 107.0(2) . . ? C13 C11 C14 108.1(4) . . ? C13' C11 C14' 111.6(7) . . ? C12 C11 C14' 65.7(5) . . ? C3 C11 C14' 107.9(3) . . ? C13 C11 C14' 142.0(4) . . ? C14 C11 C14' 49.0(5) . . ? C13' C11 C12' 108.8(7) . . ? C12 C11 C12' 40.3(4) . . ? C3 C11 C12' 107.8(3) . . ? C13 C11 C12' 74.4(5) . . ? C14 C11 C12' 142.2(4) . . ? C14' C11 C12' 105.4(6) . . ? C18 C15 C16 113.2(11) . . ? C18 C15 C17' 127.0(8) . . ? C16 C15 C17' 90.2(6) . . ? C18 C15 C18' 14.9(11) . . ? C16 C15 C18' 121.3(10) . . ? C17' C15 C18' 112.7(8) . . ? C18 C15 C8 106.4(9) . . ? C16 C15 C8 112.9(6) . . ? C17' C15 C8 106.6(4) . . ? C18' C15 C8 110.7(7) . . ? C18 C15 C16' 94.9(10) . . ? C16 C15 C16' 21.9(6) . . ? C17' C15 C16' 111.4(6) . . ? C18' C15 C16' 105.9(9) . . ? C8 C15 C16' 109.6(4) . . ? C18 C15 C17 104.3(7) . . ? C16 C15 C17 107.8(5) . . ? C17' C15 C17 23.7(5) . . ? C18' C15 C17 89.6(6) . . ? C8 C15 C17 112.0(4) . . ? C16' C15 C17 126.3(7) . . ? F3 C19 F1 108.5(2) . . ? F3 C19 F2 108.8(2) . . ? F1 C19 F2 106.4(2) . . ? F3 C19 S1 110.80(19) . . ? F1 C19 S1 111.05(18) . . ? F2 C19 S1 111.12(18) . . ? F6 C20 F4 107.8(2) . . ? F6 C20 F5 108.4(2) . . ? F4 C20 F5 108.4(2) . . ? F6 C20 S2 111.37(19) . . ? F4 C20 S2 111.14(18) . . ? F5 C20 S2 109.60(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.489 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.062 data_[Pt(tBu2bpy)(OH2)2](OTf)2_(17) _database_code_depnum_ccdc_archive 'CCDC 663526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H28 N2 O2 Pt +1, 2(C F3 O3 S, -1)' _chemical_formula_sum 'C20 H28 F6 N2 O8 Pt S2' _chemical_formula_weight 797.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5825(5) _cell_length_b 10.9866(6) _cell_length_c 27.0029(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.5780(10) _cell_angle_gamma 90.00 _cell_volume 2842.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7946 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.11 _exptl_crystal_description NEEDLE _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 5.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1821 _exptl_absorpt_correction_T_max 0.7822 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 19603 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.11 _reflns_number_total 6244 _reflns_number_gt 4822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+10.9791P] 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 6244 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.71731(2) 0.67926(2) 0.233595(8) 0.01949(8) Uani 1 1 d . . . S1 S 1.03373(17) 0.47827(16) 0.16704(6) 0.0282(4) Uani 1 1 d . . . F1 F 1.2802(5) 0.4582(6) 0.1286(2) 0.0859(19) Uani 1 1 d . . . O1 O 0.6715(5) 0.6091(5) 0.16491(18) 0.0270(11) Uani 1 1 d . . . N1 N 0.5540(5) 0.6061(5) 0.26614(17) 0.0199(11) Uani 1 1 d . . . C1 C 0.4470(6) 0.5501(6) 0.2425(2) 0.0246(13) Uani 1 1 d . . . H1 H 0.4488 0.5421 0.2075 0.030 Uiso 1 1 calc R . . S2 S 0.72331(17) 0.87130(16) 0.08634(6) 0.0268(4) Uani 1 1 d . . . F2 F 1.1241(6) 0.3456(5) 0.09403(19) 0.0672(15) Uani 1 1 d . . . O2 O 0.8877(6) 0.7656(5) 0.20473(19) 0.0277(11) Uani 1 1 d . . . N2 N 0.7584(5) 0.7284(4) 0.30222(17) 0.0182(10) Uani 1 1 d . . . C2 C 0.3348(7) 0.5041(6) 0.2683(2) 0.0274(15) Uani 1 1 d . . . H2 H 0.2605 0.4657 0.2507 0.033 Uiso 1 1 calc R . . F3 F 1.1280(7) 0.5379(6) 0.0799(2) 0.090(2) Uani 1 1 d . . . O3 O 1.0649(6) 0.3777(5) 0.19897(19) 0.0462(14) Uani 1 1 d . . . C3 C 0.3292(6) 0.5132(6) 0.3194(2) 0.0225(13) Uani 1 1 d . . . F4 F 0.9489(5) 0.9140(5) 0.03649(19) 0.0698(16) Uani 1 1 d . . . O4 O 1.0774(5) 0.5965(4) 0.18565(18) 0.0370(12) Uani 1 1 d . . . C4 C 0.4407(6) 0.5726(5) 0.3428(2) 0.0195(13) Uani 1 1 d . . . H4 H 0.4403 0.5822 0.3778 0.023 Uiso 1 1 calc R . . F5 F 0.8115(6) 0.7835(6) 0.00223(18) 0.0724(16) Uani 1 1 d . . . O5 O 0.8955(5) 0.4768(5) 0.14522(18) 0.0372(12) Uani 1 1 d . . . C5 C 0.5511(6) 0.6175(5) 0.3162(2) 0.0198(13) Uani 1 1 d . . . F6 F 0.9339(5) 0.7327(5) 0.0661(2) 0.0737(17) Uani 1 1 d . . . O6 O 0.6576(5) 0.9698(5) 0.06089(19) 0.0430(13) Uani 1 1 d . . . C6 C 0.6708(6) 0.6850(6) 0.3369(2) 0.0208(12) Uani 1 1 d . . . O7 O 0.6390(5) 0.7621(4) 0.09207(16) 0.0317(11) Uani 1 1 d . . . C7 C 0.6924(6) 0.7074(5) 0.3868(2) 0.0204(13) Uani 1 1 d . . . H7 H 0.6297 0.6747 0.4103 0.025 Uiso 1 1 calc R . . O8 O 0.7982(5) 0.9034(4) 0.13116(17) 0.0361(12) Uani 1 1 d . . . C8 C 0.8053(6) 0.7776(5) 0.4029(2) 0.0200(13) Uani 1 1 d . . . C9 C 0.8931(6) 0.8221(6) 0.3659(2) 0.0264(13) Uani 1 1 d . . . H9 H 0.9708 0.8714 0.3748 0.032 Uiso 1 1 calc R . . C10 C 0.8680(6) 0.7954(5) 0.3172(2) 0.0229(14) Uani 1 1 d . . . H10 H 0.9306 0.8254 0.2930 0.028 Uiso 1 1 calc R . . C11 C 0.2029(6) 0.4660(6) 0.3478(2) 0.0275(14) Uani 1 1 d . . . C12 C 0.1852(11) 0.3303(8) 0.3375(5) 0.086(4) Uani 1 1 d . . . H12A H 0.1754 0.3171 0.3018 0.129 Uiso 1 1 calc R . . H12B H 0.1015 0.3005 0.3542 0.129 Uiso 1 1 calc R . . H12C H 0.2672 0.2862 0.3500 0.129 Uiso 1 1 calc R . . C13 C 0.2144(9) 0.4862(10) 0.4028(3) 0.063(3) Uani 1 1 d . . . H13A H 0.2975 0.4445 0.4157 0.095 Uiso 1 1 calc R . . H13B H 0.1311 0.4538 0.4189 0.095 Uiso 1 1 calc R . . H13C H 0.2220 0.5736 0.4096 0.095 Uiso 1 1 calc R . . C14 C 0.0737(8) 0.5332(10) 0.3284(3) 0.066(3) Uani 1 1 d . . . H14A H 0.0855 0.6209 0.3336 0.100 Uiso 1 1 calc R . . H14B H -0.0088 0.5049 0.3461 0.100 Uiso 1 1 calc R . . H14C H 0.0617 0.5169 0.2929 0.100 Uiso 1 1 calc R . . C15 C 0.8340(7) 0.8085(6) 0.4570(2) 0.0270(14) Uani 1 1 d . . . C16 C 0.8271(8) 0.9484(6) 0.4625(3) 0.0359(17) Uani 1 1 d . . . H16A H 0.8962 0.9862 0.4409 0.054 Uiso 1 1 calc R . . H16B H 0.8472 0.9707 0.4970 0.054 Uiso 1 1 calc R . . H16C H 0.7336 0.9770 0.4532 0.054 Uiso 1 1 calc R . . C17 C 0.9788(7) 0.7620(7) 0.4719(3) 0.0379(18) Uani 1 1 d . . . H17A H 0.9829 0.6737 0.4671 0.057 Uiso 1 1 calc R . . H17B H 0.9970 0.7814 0.5068 0.057 Uiso 1 1 calc R . . H17C H 1.0494 0.8013 0.4513 0.057 Uiso 1 1 calc R . . C18 C 0.7246(8) 0.7518(7) 0.4909(2) 0.0381(18) Uani 1 1 d . . . H18A H 0.6320 0.7834 0.4821 0.057 Uiso 1 1 calc R . . H18B H 0.7464 0.7727 0.5254 0.057 Uiso 1 1 calc R . . H18C H 0.7254 0.6631 0.4870 0.057 Uiso 1 1 calc R . . C19 C 1.1475(8) 0.4550(8) 0.1143(3) 0.0441(19) Uani 1 1 d . . . C20 C 0.8611(8) 0.8226(8) 0.0451(3) 0.0434(18) Uani 1 1 d . . . H2O1 H 0.651(8) 0.650(7) 0.148(3) 0.03(3) Uiso 1 1 d . . . H1O2 H 0.935(7) 0.731(7) 0.195(3) 0.02(2) Uiso 1 1 d . . . H2O2 H 0.868(9) 0.805(8) 0.175(3) 0.06(3) Uiso 1 1 d . . . H1O1 H 0.770(9) 0.569(8) 0.151(3) 0.06(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02089(12) 0.01671(12) 0.02089(12) -0.00096(11) 0.00119(8) -0.00181(11) S1 0.0250(8) 0.0240(9) 0.0355(9) -0.0014(7) -0.0017(7) -0.0032(7) F1 0.029(3) 0.098(5) 0.131(5) -0.033(4) 0.014(3) 0.004(3) O1 0.031(3) 0.029(3) 0.021(2) -0.001(2) 0.000(2) -0.001(2) N1 0.020(3) 0.015(3) 0.025(3) 0.001(2) -0.001(2) 0.002(2) C1 0.025(3) 0.021(3) 0.028(3) -0.001(3) -0.004(3) 0.002(3) S2 0.0258(8) 0.0239(9) 0.0306(9) 0.0021(7) 0.0009(7) 0.0010(7) F2 0.070(3) 0.059(4) 0.073(3) -0.029(3) 0.020(3) 0.002(3) O2 0.028(3) 0.026(3) 0.030(3) -0.004(2) 0.008(2) -0.006(2) N2 0.026(3) 0.012(2) 0.016(2) 0.001(2) 0.001(2) 0.001(2) C2 0.021(3) 0.024(4) 0.037(4) -0.005(3) -0.005(3) -0.001(3) F3 0.112(5) 0.088(4) 0.070(4) 0.032(3) 0.049(3) 0.025(4) O3 0.060(4) 0.031(3) 0.048(3) 0.007(2) -0.017(3) -0.009(3) C3 0.018(3) 0.017(3) 0.032(3) 0.007(3) -0.003(3) 0.002(2) F4 0.046(3) 0.085(4) 0.079(4) 0.022(3) 0.018(3) -0.017(3) O4 0.029(3) 0.028(3) 0.054(3) -0.009(2) -0.007(2) -0.008(2) C4 0.014(3) 0.023(3) 0.021(3) 0.000(3) 0.001(2) 0.000(2) F5 0.077(4) 0.097(5) 0.044(3) -0.018(3) 0.016(3) 0.008(3) O5 0.023(2) 0.036(3) 0.052(3) -0.015(2) -0.002(2) 0.002(2) C5 0.022(3) 0.014(3) 0.024(3) 0.000(2) -0.003(2) 0.000(2) F6 0.058(3) 0.074(4) 0.089(4) 0.017(3) 0.022(3) 0.038(3) O6 0.043(3) 0.030(3) 0.056(3) 0.007(3) -0.005(3) 0.011(2) C6 0.020(3) 0.019(3) 0.023(3) 0.002(3) -0.002(2) 0.003(3) O7 0.028(2) 0.032(3) 0.035(3) 0.005(2) -0.003(2) -0.011(2) C7 0.021(3) 0.016(3) 0.024(3) 0.002(2) 0.000(2) -0.003(2) O8 0.046(3) 0.021(3) 0.041(3) -0.001(2) -0.008(2) -0.007(2) C8 0.018(3) 0.012(3) 0.030(3) -0.002(2) 0.000(2) -0.002(2) C9 0.025(3) 0.025(3) 0.029(3) -0.001(3) -0.004(2) -0.003(3) C10 0.020(3) 0.015(3) 0.034(3) 0.004(2) 0.001(3) -0.005(2) C11 0.019(3) 0.025(4) 0.039(4) 0.004(3) 0.004(3) -0.002(3) C12 0.084(7) 0.035(5) 0.141(10) 0.001(6) 0.065(7) -0.024(5) C13 0.040(5) 0.107(9) 0.043(5) 0.017(5) 0.006(4) -0.028(5) C14 0.031(4) 0.107(8) 0.062(6) 0.034(6) 0.014(4) 0.019(5) C15 0.035(4) 0.022(4) 0.024(3) -0.003(3) -0.004(3) -0.005(3) C16 0.050(4) 0.021(4) 0.036(4) -0.003(3) -0.008(3) 0.002(3) C17 0.036(4) 0.045(5) 0.032(4) 0.003(4) -0.012(3) 0.002(4) C18 0.048(5) 0.037(5) 0.029(4) -0.005(3) 0.006(3) -0.010(4) C19 0.028(4) 0.044(5) 0.060(5) -0.001(4) 0.003(4) 0.003(4) C20 0.034(4) 0.048(5) 0.048(5) 0.010(4) 0.009(3) 0.009(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 Pt1 N2 1.966(5) . ? Pt1 N1 1.974(5) . ? Pt1 O2 2.049(5) . ? Pt1 O1 2.052(5) . ? S1 O3 1.431(5) . ? S1 O5 1.444(5) . ? S1 O4 1.453(5) . ? S1 C19 1.819(8) . ? F1 C19 1.325(9) . ? N1 C1 1.350(7) . ? N1 C5 1.359(7) . ? C1 C2 1.381(9) . ? S2 O6 1.425(5) . ? S2 O8 1.444(5) . ? S2 O7 1.455(5) . ? S2 C20 1.816(7) . ? F2 C19 1.339(9) . ? N2 C10 1.341(7) . ? N2 C6 1.352(7) . ? C2 C3 1.386(9) . ? F3 C19 1.314(9) . ? C3 C4 1.398(8) . ? C3 C11 1.530(8) . ? F4 C20 1.333(9) . ? C4 C5 1.376(8) . ? F5 C20 1.320(9) . ? C5 C6 1.472(8) . ? F6 C20 1.332(9) . ? C6 C7 1.382(8) . ? C7 C8 1.395(8) . ? C8 C9 1.400(8) . ? C8 C15 1.521(8) . ? C9 C10 1.368(8) . ? C11 C13 1.505(10) . ? C11 C12 1.525(11) . ? C11 C14 1.529(10) . ? C15 C17 1.529(9) . ? C15 C18 1.532(9) . ? C15 C16 1.546(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 81.1(2) . . ? N2 Pt1 O2 94.5(2) . . ? N1 Pt1 O2 175.1(2) . . ? N2 Pt1 O1 173.8(2) . . ? N1 Pt1 O1 94.9(2) . . ? O2 Pt1 O1 89.67(19) . . ? O3 S1 O5 115.0(3) . . ? O3 S1 O4 115.1(3) . . ? O5 S1 O4 114.3(3) . . ? O3 S1 C19 103.8(4) . . ? O5 S1 C19 103.5(3) . . ? O4 S1 C19 102.9(3) . . ? C1 N1 C5 119.3(5) . . ? C1 N1 Pt1 125.3(4) . . ? C5 N1 Pt1 115.4(4) . . ? N1 C1 C2 121.3(6) . . ? O6 S2 O8 115.6(3) . . ? O6 S2 O7 115.7(3) . . ? O8 S2 O7 112.5(3) . . ? O6 S2 C20 104.4(3) . . ? O8 S2 C20 103.1(3) . . ? O7 S2 C20 103.3(4) . . ? C10 N2 C6 118.3(5) . . ? C10 N2 Pt1 125.7(4) . . ? C6 N2 Pt1 115.9(4) . . ? C1 C2 C3 120.8(6) . . ? C2 C3 C4 116.6(6) . . ? C2 C3 C11 120.9(6) . . ? C4 C3 C11 122.5(5) . . ? C5 C4 C3 121.3(5) . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 113.7(5) . . ? C4 C5 C6 125.6(5) . . ? N2 C6 C7 121.7(5) . . ? N2 C6 C5 113.6(5) . . ? C7 C6 C5 124.6(5) . . ? C6 C7 C8 120.7(5) . . ? C7 C8 C9 116.1(5) . . ? C7 C8 C15 123.7(5) . . ? C9 C8 C15 120.2(5) . . ? C10 C9 C8 120.7(6) . . ? N2 C10 C9 122.5(6) . . ? C13 C11 C12 109.3(7) . . ? C13 C11 C14 108.5(7) . . ? C12 C11 C14 108.7(8) . . ? C13 C11 C3 113.2(6) . . ? C12 C11 C3 109.1(6) . . ? C14 C11 C3 107.8(6) . . ? C8 C15 C17 109.4(5) . . ? C8 C15 C18 111.5(5) . . ? C17 C15 C18 109.4(6) . . ? C8 C15 C16 107.9(5) . . ? C17 C15 C16 110.2(6) . . ? C18 C15 C16 108.4(6) . . ? F3 C19 F1 108.5(7) . . ? F3 C19 F2 108.1(7) . . ? F1 C19 F2 107.4(7) . . ? F3 C19 S1 111.9(6) . . ? F1 C19 S1 110.5(6) . . ? F2 C19 S1 110.3(5) . . ? F5 C20 F6 108.3(7) . . ? F5 C20 F4 108.3(6) . . ? F6 C20 F4 107.7(6) . . ? F5 C20 S2 112.1(5) . . ? F6 C20 S2 109.9(5) . . ? F4 C20 S2 110.5(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.729 _refine_diff_density_min -3.744 _refine_diff_density_rms 0.166 data_[Pt(tBu2bpy)(OH2)2](OTf)2.Et2O_(17.Et2O) _database_code_depnum_ccdc_archive 'CCDC 663527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H28 N2 O2 Pt +1, 2(C F3 O3 S, -1), C4 H10 O' _chemical_formula_sum 'C24 H38 F6 N2 O9 Pt S2' _chemical_formula_weight 871.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6959(8) _cell_length_b 12.3527(9) _cell_length_c 13.1273(9) _cell_angle_alpha 92.1490(10) _cell_angle_beta 113.6370(10) _cell_angle_gamma 104.7530(10) _cell_volume 1659.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.04 _exptl_crystal_description PRISM _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 4.436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2699 _exptl_absorpt_correction_T_max 0.3495 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; Siemens SMART CCD: The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.00 cm. Coverage of the unique set is over 95% complete to at least 26% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 11632 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7085 _reflns_number_gt 6638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ; _computing_molecular_graphics ; L. J. Barbour, X-Seed - Graphical Interface to SHELX-97 and POV-Ray, 1999 ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997) ; _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+1.7853P] 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 7085 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.290101(11) 0.380611(9) 0.155251(9) 0.02025(4) Uani 1 1 d . . . S1 S 0.20441(9) 0.72165(7) -0.04890(7) 0.03132(18) Uani 1 1 d . . . F1 F 0.2029(4) 0.5627(2) -0.1850(3) 0.0823(10) Uani 1 1 d . . . O1 O 0.1819(3) 0.4894(2) 0.0981(2) 0.0289(5) Uani 1 1 d . . . N1 N 0.3823(2) 0.2640(2) 0.1997(2) 0.0218(5) Uani 1 1 d . . . C1 C 0.4829(3) 0.2704(3) 0.2984(3) 0.0251(6) Uani 1 1 d . . . H1 H 0.5164 0.3367 0.3529 0.030 Uiso 1 1 calc R . . S2 S 0.21078(8) 0.64811(7) 0.36197(6) 0.02532(16) Uani 1 1 d . . . F2 F 0.3732(3) 0.7097(3) -0.1280(3) 0.0828(10) Uani 1 1 d . . . O2 O 0.4152(2) 0.4958(2) 0.2966(2) 0.0281(5) Uani 1 1 d . . . N2 N 0.1788(3) 0.2635(2) 0.0213(2) 0.0233(5) Uani 1 1 d . . . C2 C 0.5395(3) 0.1838(3) 0.3235(3) 0.0268(7) Uani 1 1 d . . . H2 H 0.6097 0.1906 0.3949 0.032 Uiso 1 1 calc R . . F3 F 0.1872(3) 0.7165(3) -0.2535(2) 0.0706(8) Uani 1 1 d . . . O3 O 0.2841(3) 0.6755(2) 0.0453(2) 0.0462(7) Uani 1 1 d . . . C3 C 0.4942(3) 0.0863(3) 0.2447(2) 0.0233(6) Uani 1 1 d . . . F4 F 0.0777(3) 0.4601(2) 0.3959(2) 0.0646(7) Uani 1 1 d . . . O4 O 0.2495(3) 0.8432(2) -0.0362(2) 0.0441(7) Uani 1 1 d . . . C4 C 0.3875(3) 0.0802(3) 0.1425(2) 0.0225(6) Uani 1 1 d . . . H4 H 0.3525 0.0147 0.0868 0.027 Uiso 1 1 calc R . . F5 F 0.1814(3) 0.5911(3) 0.5408(2) 0.0697(8) Uani 1 1 d . . . O5 O 0.0664(3) 0.6711(3) -0.0905(3) 0.0522(7) Uani 1 1 d . . . C5 C 0.3331(3) 0.1678(2) 0.1219(2) 0.0200(6) Uani 1 1 d . . . F6 F 0.0057(3) 0.6027(3) 0.4040(3) 0.0731(9) Uani 1 1 d . . . O6 O 0.3270(2) 0.6105(2) 0.4058(2) 0.0375(6) Uani 1 1 d . . . C6 C 0.2174(3) 0.1685(3) 0.0194(2) 0.0220(6) Uani 1 1 d . . . O7 O 0.2319(3) 0.7645(2) 0.4006(2) 0.0380(6) Uani 1 1 d . . . C7 C 0.1495(3) 0.0815(3) -0.0710(2) 0.0241(6) Uani 1 1 d . . . H7 H 0.1773 0.0155 -0.0703 0.029 Uiso 1 1 calc R . . O8 O 0.1297(2) 0.6089(2) 0.24323(19) 0.0356(6) Uani 1 1 d . . . C8 C 0.0400(3) 0.0900(3) -0.1639(2) 0.0251(6) Uani 1 1 d . . . O9 O 0.6360(2) 0.6423(2) 0.3181(2) 0.0389(6) Uani 1 1 d . . . C9 C 0.0041(3) 0.1891(3) -0.1587(3) 0.0305(7) Uani 1 1 d . . . H9 H -0.0693 0.1984 -0.2201 0.037 Uiso 1 1 calc R . . C10 C 0.0730(3) 0.2731(3) -0.0666(3) 0.0292(7) Uani 1 1 d . . . H10 H 0.0456 0.3389 -0.0648 0.035 Uiso 1 1 calc R . . C11 C 0.5530(3) -0.0122(3) 0.2676(3) 0.0272(7) Uani 1 1 d . . . C12 C 0.6812(4) 0.0200(3) 0.3752(3) 0.0448(10) Uani 1 1 d . . . H12A H 0.7436 0.0857 0.3680 0.067 Uiso 1 1 calc R . . H12B H 0.7177 -0.0441 0.3864 0.067 Uiso 1 1 calc R . . H12C H 0.6642 0.0388 0.4399 0.067 Uiso 1 1 calc R . . C13 C 0.5805(4) -0.0456(3) 0.1673(3) 0.0362(8) Uani 1 1 d . . . H13A H 0.4980 -0.0729 0.0994 0.054 Uiso 1 1 calc R . . H13B H 0.6230 -0.1057 0.1834 0.054 Uiso 1 1 calc R . . H13C H 0.6379 0.0207 0.1552 0.054 Uiso 1 1 calc R . . C14 C 0.4545(4) -0.1128(3) 0.2811(4) 0.0415(9) Uani 1 1 d . . . H14A H 0.4402 -0.0923 0.3469 0.062 Uiso 1 1 calc R . . H14B H 0.4888 -0.1781 0.2915 0.062 Uiso 1 1 calc R . . H14C H 0.3716 -0.1323 0.2135 0.062 Uiso 1 1 calc R . . C15 C -0.0358(3) 0.0003(3) -0.2693(3) 0.0303(7) Uani 1 1 d . . . C16 C -0.1821(3) -0.0276(3) -0.3017(3) 0.0400(8) Uani 1 1 d . . . H16A H -0.2302 -0.0851 -0.3695 0.060 Uiso 1 1 calc R . . H16B H -0.2092 0.0412 -0.3167 0.060 Uiso 1 1 calc R . . H16C H -0.2007 -0.0567 -0.2399 0.060 Uiso 1 1 calc R . . C17 C -0.0100(4) 0.0523(4) -0.3660(3) 0.0491(11) Uani 1 1 d . . . H17A H 0.0838 0.0733 -0.3464 0.074 Uiso 1 1 calc R . . H17B H -0.0399 0.1200 -0.3778 0.074 Uiso 1 1 calc R . . H17C H -0.0574 -0.0033 -0.4352 0.074 Uiso 1 1 calc R . . C18 C 0.0067(5) -0.1063(4) -0.2555(4) 0.0634(15) Uani 1 1 d . . . H18A H 0.1007 -0.0867 -0.2344 0.095 Uiso 1 1 calc R . . H18B H -0.0407 -0.1590 -0.3267 0.095 Uiso 1 1 calc R . . H18C H -0.0124 -0.1421 -0.1965 0.095 Uiso 1 1 calc R . . C19 C 0.2440(5) 0.6756(4) -0.1603(4) 0.0488(10) Uani 1 1 d . . . C20 C 0.1135(4) 0.5710(4) 0.4291(3) 0.0431(9) Uani 1 1 d . . . C21 C 0.5863(5) 0.6065(5) 0.1243(4) 0.0611(13) Uani 1 1 d . . . H21A H 0.5522 0.5247 0.1214 0.092 Uiso 1 1 calc R . . H21B H 0.6220 0.6198 0.0683 0.092 Uiso 1 1 calc R . . H21C H 0.5155 0.6412 0.1077 0.092 Uiso 1 1 calc R . . C22 C 0.6913(4) 0.6576(4) 0.2387(3) 0.0434(9) Uani 1 1 d . . . H22A H 0.7613 0.6204 0.2575 0.052 Uiso 1 1 calc R . . H22B H 0.7298 0.7394 0.2410 0.052 Uiso 1 1 calc R . . C23 C 0.7312(4) 0.6872(4) 0.4313(3) 0.0432(9) Uani 1 1 d . . . H23A H 0.7698 0.7698 0.4382 0.052 Uiso 1 1 calc R . . H23B H 0.8022 0.6511 0.4510 0.052 Uiso 1 1 calc R . . C24 C 0.6671(4) 0.6644(4) 0.5098(3) 0.0496(10) Uani 1 1 d . . . H24A H 0.5982 0.7017 0.4910 0.074 Uiso 1 1 calc R . . H24B H 0.7322 0.6941 0.5874 0.074 Uiso 1 1 calc R . . H24C H 0.6288 0.5825 0.5024 0.074 Uiso 1 1 calc R . . H1O2 H 0.382(4) 0.534(4) 0.332(4) 0.045(12) Uiso 1 1 d . . . H1O1 H 0.225(5) 0.559(4) 0.084(4) 0.057(14) Uiso 1 1 d . . . H2O2 H 0.484(5) 0.543(4) 0.302(4) 0.058(15) Uiso 1 1 d . . . H2O1 H 0.148(4) 0.503(4) 0.133(4) 0.044(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02618(7) 0.01756(6) 0.02015(6) 0.00275(4) 0.01085(5) 0.00996(4) S1 0.0355(4) 0.0233(4) 0.0352(4) 0.0056(3) 0.0148(4) 0.0090(3) F1 0.114(3) 0.0441(16) 0.094(2) -0.0142(15) 0.046(2) 0.0328(17) O1 0.0401(14) 0.0264(13) 0.0314(13) 0.0095(10) 0.0203(11) 0.0189(11) N1 0.0237(12) 0.0239(13) 0.0195(12) 0.0020(10) 0.0096(10) 0.0092(10) C1 0.0250(15) 0.0245(16) 0.0216(15) -0.0014(12) 0.0063(12) 0.0074(12) S2 0.0285(4) 0.0266(4) 0.0237(4) 0.0024(3) 0.0112(3) 0.0129(3) F2 0.0636(19) 0.112(3) 0.107(3) 0.040(2) 0.0614(19) 0.0376(19) O2 0.0280(12) 0.0219(12) 0.0341(13) -0.0021(9) 0.0138(10) 0.0067(10) N2 0.0267(13) 0.0223(13) 0.0247(13) 0.0068(10) 0.0114(11) 0.0123(11) C2 0.0246(15) 0.0304(17) 0.0212(15) 0.0010(12) 0.0041(12) 0.0109(13) F3 0.101(2) 0.080(2) 0.0403(14) 0.0107(14) 0.0332(15) 0.0366(18) O3 0.0509(16) 0.0330(14) 0.0464(16) 0.0156(12) 0.0115(13) 0.0130(12) C3 0.0246(15) 0.0245(15) 0.0215(14) 0.0040(12) 0.0083(12) 0.0110(12) F4 0.0602(16) 0.0444(15) 0.0695(18) 0.0158(13) 0.0189(14) -0.0036(12) O4 0.0601(17) 0.0214(12) 0.0372(14) 0.0026(10) 0.0066(13) 0.0131(12) C4 0.0236(14) 0.0217(15) 0.0207(14) 0.0007(11) 0.0072(12) 0.0081(12) F5 0.0742(19) 0.096(2) 0.0334(13) 0.0121(14) 0.0282(13) 0.0062(16) O5 0.0369(15) 0.0523(18) 0.072(2) 0.0180(16) 0.0265(15) 0.0134(13) C5 0.0225(14) 0.0217(15) 0.0173(13) 0.0018(11) 0.0084(11) 0.0094(12) F6 0.0437(15) 0.102(2) 0.088(2) 0.0112(18) 0.0403(15) 0.0248(15) O6 0.0324(13) 0.0461(15) 0.0373(14) 0.0010(11) 0.0118(11) 0.0227(12) C6 0.0252(15) 0.0239(15) 0.0193(14) 0.0033(11) 0.0089(12) 0.0120(12) O7 0.0488(15) 0.0282(13) 0.0326(13) -0.0022(10) 0.0104(11) 0.0163(11) C7 0.0269(15) 0.0240(15) 0.0220(15) 0.0032(12) 0.0080(12) 0.0126(13) O8 0.0449(14) 0.0383(14) 0.0246(12) -0.0012(10) 0.0113(11) 0.0203(12) C8 0.0261(15) 0.0287(16) 0.0187(14) -0.0002(12) 0.0065(12) 0.0107(13) O9 0.0368(14) 0.0421(15) 0.0361(14) 0.0035(11) 0.0168(11) 0.0069(11) C9 0.0315(17) 0.0351(18) 0.0225(16) 0.0038(13) 0.0035(13) 0.0191(15) C10 0.0350(17) 0.0297(17) 0.0251(16) 0.0052(13) 0.0082(13) 0.0202(14) C11 0.0291(16) 0.0267(16) 0.0254(16) 0.0043(13) 0.0075(13) 0.0146(13) C12 0.041(2) 0.046(2) 0.038(2) -0.0002(17) -0.0027(17) 0.0291(18) C13 0.0390(19) 0.038(2) 0.0384(19) 0.0055(16) 0.0167(16) 0.0222(16) C14 0.048(2) 0.034(2) 0.050(2) 0.0187(17) 0.0230(19) 0.0205(17) C15 0.0258(16) 0.0339(18) 0.0243(16) -0.0058(13) 0.0028(13) 0.0119(14) C16 0.0291(18) 0.041(2) 0.045(2) 0.0031(17) 0.0138(16) 0.0058(16) C17 0.040(2) 0.067(3) 0.031(2) -0.0111(19) 0.0168(17) 0.001(2) C18 0.057(3) 0.043(2) 0.056(3) -0.021(2) -0.015(2) 0.028(2) C19 0.057(3) 0.044(2) 0.057(3) 0.006(2) 0.031(2) 0.022(2) C20 0.037(2) 0.052(2) 0.039(2) 0.0083(18) 0.0168(17) 0.0092(18) C21 0.056(3) 0.085(4) 0.044(2) 0.006(2) 0.027(2) 0.013(3) C22 0.042(2) 0.046(2) 0.050(2) 0.0101(19) 0.0262(19) 0.0149(18) C23 0.0322(19) 0.044(2) 0.042(2) 0.0036(17) 0.0082(16) 0.0063(16) C24 0.051(2) 0.049(2) 0.033(2) -0.0027(18) 0.0114(18) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 1.974(3) . ? Pt1 N1 1.982(2) . ? Pt1 O1 2.038(2) . ? Pt1 O2 2.043(2) . ? S1 O5 1.431(3) . ? S1 O4 1.438(3) . ? S1 O3 1.457(3) . ? S1 C19 1.814(4) . ? F1 C19 1.335(5) . ? N1 C1 1.338(4) . ? N1 C5 1.369(4) . ? C1 C2 1.380(4) . ? S2 O7 1.431(2) . ? S2 O8 1.445(2) . ? S2 O6 1.452(2) . ? S2 C20 1.815(4) . ? F2 C19 1.337(5) . ? N2 C10 1.349(4) . ? N2 C6 1.362(4) . ? C2 C3 1.394(4) . ? F3 C19 1.326(5) . ? C3 C4 1.402(4) . ? C3 C11 1.526(4) . ? F4 C20 1.327(5) . ? C4 C5 1.373(4) . ? F5 C20 1.334(5) . ? C5 C6 1.479(4) . ? F6 C20 1.333(5) . ? C6 C7 1.382(4) . ? C7 C8 1.402(4) . ? C8 C9 1.399(4) . ? C8 C15 1.526(4) . ? O9 C22 1.426(5) . ? O9 C23 1.432(4) . ? C9 C10 1.374(5) . ? C11 C14 1.534(5) . ? C11 C12 1.536(4) . ? C11 C13 1.541(5) . ? C15 C18 1.514(5) . ? C15 C16 1.526(5) . ? C15 C17 1.545(5) . ? C21 C22 1.490(6) . ? C23 C24 1.496(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 81.52(10) . . ? N2 Pt1 O1 93.37(10) . . ? N1 Pt1 O1 174.78(10) . . ? N2 Pt1 O2 175.87(9) . . ? N1 Pt1 O2 94.51(10) . . ? O1 Pt1 O2 90.61(10) . . ? O5 S1 O4 116.60(18) . . ? O5 S1 O3 115.20(18) . . ? O4 S1 O3 113.27(16) . . ? O5 S1 C19 104.4(2) . . ? O4 S1 C19 103.1(2) . . ? O3 S1 C19 101.80(19) . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Pt1 125.8(2) . . ? C5 N1 Pt1 115.23(19) . . ? N1 C1 C2 122.0(3) . . ? O7 S2 O8 115.87(15) . . ? O7 S2 O6 114.58(16) . . ? O8 S2 O6 114.03(15) . . ? O7 S2 C20 103.62(18) . . ? O8 S2 C20 103.65(18) . . ? O6 S2 C20 102.79(17) . . ? C10 N2 C6 119.6(3) . . ? C10 N2 Pt1 124.9(2) . . ? C6 N2 Pt1 115.51(19) . . ? C1 C2 C3 120.4(3) . . ? C2 C3 C4 116.8(3) . . ? C2 C3 C11 122.8(3) . . ? C4 C3 C11 120.4(3) . . ? C5 C4 C3 120.7(3) . . ? N1 C5 C4 121.1(3) . . ? N1 C5 C6 113.6(2) . . ? C4 C5 C6 125.3(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 114.1(3) . . ? C7 C6 C5 124.8(3) . . ? C6 C7 C8 120.4(3) . . ? C9 C8 C7 116.7(3) . . ? C9 C8 C15 119.9(3) . . ? C7 C8 C15 123.4(3) . . ? C22 O9 C23 112.4(3) . . ? C10 C9 C8 121.3(3) . . ? N2 C10 C9 121.0(3) . . ? C3 C11 C14 108.6(3) . . ? C3 C11 C12 111.4(3) . . ? C14 C11 C12 109.1(3) . . ? C3 C11 C13 109.0(3) . . ? C14 C11 C13 109.8(3) . . ? C12 C11 C13 108.9(3) . . ? C18 C15 C8 112.7(3) . . ? C18 C15 C16 110.7(3) . . ? C8 C15 C16 109.9(3) . . ? C18 C15 C17 108.5(4) . . ? C8 C15 C17 107.3(3) . . ? C16 C15 C17 107.7(3) . . ? F3 C19 F1 107.9(4) . . ? F3 C19 F2 108.7(4) . . ? F1 C19 F2 108.2(4) . . ? F3 C19 S1 111.4(3) . . ? F1 C19 S1 110.2(3) . . ? F2 C19 S1 110.5(3) . . ? F4 C20 F6 108.1(3) . . ? F4 C20 F5 107.9(4) . . ? F6 C20 F5 108.4(4) . . ? F4 C20 S2 111.3(3) . . ? F6 C20 S2 110.6(3) . . ? F5 C20 S2 110.5(3) . . ? O9 C22 C21 108.6(3) . . ? O9 C23 C24 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.490 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.093