# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'ccdc_sub.cif' _publ_contact_author ; Evamarie Hey-Hawkins Structure Determination: L\"onnecke, Peter Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_phone '49 / 341 / 9736151' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email hey@rz.uni-leipzig.de _publ_section_title ; Reaction of a Heterotopic P,SAs-Ligand with Group 10 Metal(II) Complexes: Metal-mediated As-S Bond Cleavage and Formation of Two Unusual Trinuclear Structural Isomers (for Pd and Pt) ; loop_ _publ_author_name _publ_author_address I.Sarosi ; Faculty of Chemistry and Chemical Engineering Babe\,s-Bolyai University Kog\(alniceanu 1 400084 Cluj-Napoca Romania and Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; A.Hildebrand ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; P.Lonnecke ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; L.Silaghi-Dumitrescu ; Faculty of Chemistry and Chemical Engineering Babe\,s-Bolyai University Kog\(alniceanu 1 400084 Cluj-Napoca Romania ; ; E.Hey-Hawkins ; ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Germany ; _publ_requested_category FO _publ_contact_author_name 'Evamarie Hey-Hawkins' #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-07-14 at 15:50:43 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\xray\wingx\files\archive.dat # CIF files read : x1078fin x1078 data_x1078fin _database_code_depnum_ccdc_archive 'CCDC 856663' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2010-07-14T15:50:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C30 H24 As P S' _chemical_formula_weight 522.44 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.4830(2) _cell_length_b 9.8797(3) _cell_length_c 48.4808(13) _cell_angle_alpha 90 _cell_angle_beta 93.390(2) _cell_angle_gamma 90 _cell_volume 5012.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 16373 _cell_measurement_theta_min 2.8297 _cell_measurement_theta_max 31.3939 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.52 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.84906 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_ub_11 -0.0034756 _diffrn_orient_matrix_ub_12 -0.0567022 _diffrn_orient_matrix_ub_13 0.0088968 _diffrn_orient_matrix_ub_21 -0.0057558 _diffrn_orient_matrix_ub_22 0.0439894 _diffrn_orient_matrix_ub_23 0.0114168 _diffrn_orient_matrix_ub_31 -0.067481 _diffrn_orient_matrix_ub_32 -0.0008218 _diffrn_orient_matrix_ub_33 -0.0022785 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.0714 _diffrn_reflns_number 45613 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 69 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 15249 _reflns_number_gt 11034 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0130P)^2^+24.0654P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15249 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.13 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.127 _refine_diff_density_min -1 _refine_diff_density_rms 0.116 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 As1 As 0.95950(4) 0.39723(4) 0.023221(8) 0.01646(9) Uani 1 1 d . . . As2 As 0.50900(4) 0.06182(4) 0.182178(9) 0.02001(10) Uani 1 1 d . . . S1 S 0.88633(9) 0.30935(10) 0.06246(2) 0.01771(19) Uani 1 1 d . . . S2 S 0.69613(9) 0.05343(11) 0.20717(2) 0.0219(2) Uani 1 1 d . . . P1 P 0.73390(10) 0.58215(10) 0.06582(2) 0.0169(2) Uani 1 1 d . . . P2 P 0.88904(10) -0.01161(10) 0.16099(2) 0.0167(2) Uani 1 1 d . . . C1 C 0.8395(4) 0.3125(4) -0.00365(8) 0.0174(7) Uani 1 1 d . . . C2 C 0.7098(4) 0.3031(4) 0.00128(9) 0.0215(8) Uani 1 1 d . . . H2 H 0.6818 0.3231 0.0191 0.026 Uiso 1 1 calc R . . C3 C 0.6221(4) 0.2648(5) -0.01975(10) 0.0271(9) Uani 1 1 d . . . H3 H 0.5343 0.2564 -0.0162 0.032 Uiso 1 1 calc R . . C4 C 0.6621(4) 0.2386(4) -0.04596(9) 0.0284(10) Uani 1 1 d . . . H4 H 0.6017 0.2128 -0.0604 0.034 Uiso 1 1 calc R . . C5 C 0.7901(4) 0.2501(4) -0.05118(9) 0.0247(9) Uani 1 1 d . . . H5 H 0.8171 0.2336 -0.0692 0.03 Uiso 1 1 calc R . . C6 C 0.8787(4) 0.2856(4) -0.03009(8) 0.0201(8) Uani 1 1 d . . . H6 H 0.9666 0.2918 -0.0337 0.024 Uiso 1 1 calc R . . C7 C 1.1087(4) 0.2801(4) 0.02036(8) 0.0172(8) Uani 1 1 d . . . C8 C 1.1005(4) 0.1411(4) 0.01638(8) 0.0180(8) Uani 1 1 d . . . H8 H 1.019 0.0998 0.0134 0.022 Uiso 1 1 calc R . . C9 C 1.2090(4) 0.0625(4) 0.01678(8) 0.0232(8) Uani 1 1 d . . . H9 H 1.2021 -0.0324 0.0139 0.028 Uiso 1 1 calc R . . C10 C 1.3284(4) 0.1214(5) 0.02131(9) 0.0249(9) Uani 1 1 d . . . H10 H 1.4033 0.0672 0.0217 0.03 Uiso 1 1 calc R . . C11 C 1.3374(4) 0.2592(5) 0.02522(10) 0.0293(10) Uani 1 1 d . . . H11 H 1.419 0.3 0.0284 0.035 Uiso 1 1 calc R . . C12 C 1.2282(4) 0.3390(4) 0.02461(9) 0.0240(9) Uani 1 1 d . . . H12 H 1.2354 0.4341 0.0271 0.029 Uiso 1 1 calc R . . C13 C 0.9517(4) 0.4412(4) 0.08410(8) 0.0173(7) Uani 1 1 d . . . C14 C 0.8862(4) 0.5644(4) 0.08630(8) 0.0177(7) Uani 1 1 d . . . C15 C 0.9411(4) 0.6658(4) 0.10302(9) 0.0208(8) Uani 1 1 d . . . H15 H 0.8983 0.75 0.1046 0.025 Uiso 1 1 calc R . . C16 C 1.0581(4) 0.6449(4) 0.11742(9) 0.0238(9) Uani 1 1 d . . . H16 H 1.0947 0.7151 0.1287 0.029 Uiso 1 1 calc R . . C17 C 1.1213(4) 0.5233(5) 0.11550(9) 0.0256(9) Uani 1 1 d . . . H17 H 1.2009 0.5095 0.1255 0.031 Uiso 1 1 calc R . . C18 C 1.0682(4) 0.4210(4) 0.09886(9) 0.0216(8) Uani 1 1 d . . . H18 H 1.1115 0.3369 0.0975 0.026 Uiso 1 1 calc R . . C19 C 0.6906(4) 0.7588(4) 0.07255(8) 0.0179(8) Uani 1 1 d . . . C20 C 0.6309(4) 0.8048(4) 0.09570(9) 0.0235(9) Uani 1 1 d . . . H20 H 0.6099 0.7429 0.1097 0.028 Uiso 1 1 calc R . . C21 C 0.6019(4) 0.9414(5) 0.09828(9) 0.0269(9) Uani 1 1 d . . . H21 H 0.5616 0.9721 0.1142 0.032 Uiso 1 1 calc R . . C22 C 0.6308(4) 1.0325(4) 0.07819(10) 0.0281(10) Uani 1 1 d . . . H22 H 0.6105 1.1256 0.0802 0.034 Uiso 1 1 calc R . . C23 C 0.6894(5) 0.9879(4) 0.05509(10) 0.0299(10) Uani 1 1 d . . . H23 H 0.7097 1.0503 0.0411 0.036 Uiso 1 1 calc R . . C24 C 0.7187(4) 0.8513(4) 0.05239(9) 0.0244(9) Uani 1 1 d . . . H24 H 0.7587 0.8211 0.0364 0.029 Uiso 1 1 calc R . . C25 C 0.6267(4) 0.4852(4) 0.08726(8) 0.0174(8) Uani 1 1 d . . . C26 C 0.5009(4) 0.4681(5) 0.07712(9) 0.0268(9) Uani 1 1 d . . . H26 H 0.4723 0.5109 0.0603 0.032 Uiso 1 1 calc R . . C27 C 0.4170(4) 0.3897(6) 0.09114(10) 0.0354(11) Uani 1 1 d . . . H27 H 0.3309 0.3807 0.0842 0.043 Uiso 1 1 calc R . . C28 C 0.4573(4) 0.3247(5) 0.11511(10) 0.0293(10) Uani 1 1 d . . . H28 H 0.3999 0.2695 0.1246 0.035 Uiso 1 1 calc R . . C29 C 0.5820(4) 0.3402(5) 0.12538(9) 0.0274(9) Uani 1 1 d . . . H29 H 0.6103 0.2963 0.1421 0.033 Uiso 1 1 calc R . . C30 C 0.6658(4) 0.4194(4) 0.11150(9) 0.0246(9) Uani 1 1 d . . . H30 H 0.7515 0.4289 0.1187 0.03 Uiso 1 1 calc R . . C31 C 0.3979(4) 0.1400(4) 0.20882(9) 0.0234(9) Uani 1 1 d . . . C32 C 0.2993(4) 0.2227(4) 0.19818(11) 0.0291(10) Uani 1 1 d . . . H32 H 0.2856 0.2327 0.1787 0.035 Uiso 1 1 calc R . . C33 C 0.2208(5) 0.2909(5) 0.21564(13) 0.0405(13) Uani 1 1 d . . . H33 H 0.153 0.3461 0.2082 0.049 Uiso 1 1 calc R . . C34 C 0.2420(5) 0.2778(6) 0.24366(12) 0.0431(14) Uani 1 1 d . . . H34 H 0.189 0.3252 0.2556 0.052 Uiso 1 1 calc R . . C35 C 0.3388(5) 0.1969(6) 0.25475(12) 0.0439(14) Uani 1 1 d . . . H35 H 0.3522 0.1884 0.2742 0.053 Uiso 1 1 calc R . . C36 C 0.4172(5) 0.1273(5) 0.23723(10) 0.0349(11) Uani 1 1 d . . . H36 H 0.484 0.0711 0.2448 0.042 Uiso 1 1 calc R . . C37 C 0.4745(3) -0.1318(4) 0.18520(9) 0.0199(8) Uani 1 1 d . . . C38 C 0.3812(4) -0.1888(5) 0.20014(11) 0.0332(11) Uani 1 1 d . . . H38 H 0.3302 -0.1328 0.211 0.04 Uiso 1 1 calc R . . C39 C 0.3608(5) -0.3280(5) 0.19948(14) 0.0466(15) Uani 1 1 d . . . H39 H 0.2966 -0.367 0.21 0.056 Uiso 1 1 calc R . . C40 C 0.4343(5) -0.4096(5) 0.18344(12) 0.0431(13) Uani 1 1 d . . . H40 H 0.4203 -0.5046 0.1829 0.052 Uiso 1 1 calc R . . C41 C 0.5279(5) -0.3533(5) 0.16817(11) 0.0364(11) Uani 1 1 d . . . H41 H 0.5773 -0.4091 0.1569 0.044 Uiso 1 1 calc R . . C42 C 0.5494(4) -0.2148(5) 0.16934(9) 0.0263(9) Uani 1 1 d . . . H42 H 0.6154 -0.1762 0.1593 0.032 Uiso 1 1 calc R . . C43 C 0.7750(4) 0.1905(4) 0.19145(8) 0.0186(8) Uani 1 1 d . . . C44 C 0.8678(4) 0.1641(4) 0.17245(8) 0.0176(8) Uani 1 1 d . . . C45 C 0.9324(4) 0.2738(4) 0.16163(8) 0.0183(8) Uani 1 1 d . . . H45 H 0.9973 0.2583 0.1491 0.022 Uiso 1 1 calc R . . C46 C 0.9026(4) 0.4056(4) 0.16899(9) 0.0241(9) Uani 1 1 d . . . H46 H 0.9465 0.4793 0.1613 0.029 Uiso 1 1 calc R . . C47 C 0.8101(4) 0.4300(4) 0.18736(9) 0.0247(9) Uani 1 1 d . . . H47 H 0.7901 0.5204 0.1922 0.03 Uiso 1 1 calc R . . C48 C 0.7461(4) 0.3235(4) 0.19877(9) 0.0216(8) Uani 1 1 d . . . H48 H 0.6827 0.3404 0.2115 0.026 Uiso 1 1 calc R . . C49 C 1.0224(4) 0.0049(4) 0.13816(8) 0.0184(8) Uani 1 1 d . . . C50 C 0.9913(4) 0.0299(4) 0.11023(9) 0.0261(9) Uani 1 1 d . . . H50 H 0.9043 0.0409 0.104 0.031 Uiso 1 1 calc R . . C51 C 1.0856(5) 0.0390(4) 0.09158(9) 0.0299(10) Uani 1 1 d . . . H51 H 1.0631 0.0574 0.0727 0.036 Uiso 1 1 calc R . . C52 C 1.2117(5) 0.0215(5) 0.10019(10) 0.0304(10) Uani 1 1 d . . . H52 H 1.2761 0.028 0.0873 0.036 Uiso 1 1 calc R . . C53 C 1.2445(4) -0.0054(5) 0.12746(10) 0.0310(10) Uani 1 1 d . . . H53 H 1.3316 -0.0186 0.1334 0.037 Uiso 1 1 calc R . . C54 C 1.1504(4) -0.0133(5) 0.14642(9) 0.0249(9) Uani 1 1 d . . . H54 H 1.1739 -0.0314 0.1653 0.03 Uiso 1 1 calc R . . C55 C 0.9687(3) -0.0915(4) 0.19137(8) 0.0165(7) Uani 1 1 d . . . C56 C 1.0271(4) -0.0220(4) 0.21365(8) 0.0192(8) Uani 1 1 d . . . H56 H 1.0276 0.0742 0.2136 0.023 Uiso 1 1 calc R . . C57 C 1.0844(4) -0.0917(5) 0.23586(8) 0.0230(8) Uani 1 1 d . . . H57 H 1.1245 -0.0433 0.2509 0.028 Uiso 1 1 calc R . . C58 C 1.0834(4) -0.2316(4) 0.23612(9) 0.0238(9) Uani 1 1 d . . . H58 H 1.1221 -0.2792 0.2515 0.029 Uiso 1 1 calc R . . C59 C 1.0265(4) -0.3023(4) 0.21420(9) 0.0252(9) Uani 1 1 d . . . H59 H 1.0271 -0.3984 0.2143 0.03 Uiso 1 1 calc R . . C60 C 0.9683(4) -0.2327(4) 0.19211(8) 0.0217(8) Uani 1 1 d . . . H60 H 0.9275 -0.2818 0.1772 0.026 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 As1 0.01751(18) 0.01376(18) 0.01831(19) -0.00077(16) 0.00289(14) -0.00137(15) As2 0.01873(19) 0.0218(2) 0.0198(2) 0.00039(17) 0.00320(15) -0.00039(16) S1 0.0211(5) 0.0141(4) 0.0185(5) -0.0010(4) 0.0058(4) -0.0018(4) S2 0.0172(5) 0.0248(5) 0.0239(5) 0.0055(4) 0.0019(4) -0.0012(4) P1 0.0215(5) 0.0144(5) 0.0149(5) -0.0001(4) 0.0021(4) -0.0008(4) P2 0.0172(5) 0.0154(5) 0.0175(5) 0.0003(4) 0.0009(4) -0.0014(4) C1 0.0221(19) 0.0120(17) 0.0179(19) 0.0015(15) 0.0009(15) 0.0000(14) C2 0.0173(19) 0.022(2) 0.026(2) -0.0012(17) 0.0052(16) 0.0022(15) C3 0.0124(18) 0.031(2) 0.038(3) 0.001(2) 0.0001(17) 0.0009(17) C4 0.031(2) 0.026(2) 0.027(2) -0.0004(19) -0.0120(19) 0.0024(18) C5 0.035(2) 0.019(2) 0.019(2) 0.0007(16) -0.0003(17) -0.0027(18) C6 0.026(2) 0.0153(18) 0.019(2) -0.0001(15) 0.0059(16) -0.0013(15) C7 0.0205(19) 0.0177(18) 0.0136(18) -0.0002(15) 0.0025(14) 0.0008(15) C8 0.0172(18) 0.0191(19) 0.0182(19) -0.0006(15) 0.0058(15) -0.0040(14) C9 0.030(2) 0.0185(19) 0.022(2) 0.0021(17) 0.0046(16) 0.0021(17) C10 0.0165(19) 0.032(2) 0.027(2) 0.0008(19) 0.0031(16) 0.0073(17) C11 0.017(2) 0.033(2) 0.037(3) -0.003(2) 0.0014(18) -0.0034(18) C12 0.024(2) 0.0182(19) 0.030(2) -0.0022(17) 0.0028(17) -0.0023(16) C13 0.0208(18) 0.0172(18) 0.0144(17) -0.0017(15) 0.0055(14) -0.0054(15) C14 0.0210(18) 0.0156(18) 0.0171(18) -0.0008(15) 0.0060(14) -0.0024(15) C15 0.0206(19) 0.0175(19) 0.025(2) -0.0027(16) 0.0082(16) -0.0034(15) C16 0.020(2) 0.026(2) 0.026(2) -0.0065(18) 0.0031(16) -0.0066(16) C17 0.019(2) 0.031(2) 0.027(2) -0.0035(19) -0.0002(17) 0.0010(17) C18 0.0201(19) 0.019(2) 0.026(2) 0.0007(16) 0.0044(16) 0.0008(15) C19 0.0176(18) 0.0169(18) 0.0191(19) -0.0009(15) -0.0016(15) 0.0016(14) C20 0.026(2) 0.023(2) 0.021(2) 0.0018(17) 0.0017(17) 0.0005(17) C21 0.027(2) 0.029(2) 0.025(2) -0.0082(19) 0.0026(17) 0.0040(18) C22 0.031(2) 0.019(2) 0.033(2) -0.0027(18) -0.0021(19) 0.0047(17) C23 0.044(3) 0.018(2) 0.027(2) 0.0079(18) 0.000(2) -0.0014(19) C24 0.032(2) 0.020(2) 0.022(2) 0.0017(17) 0.0066(17) 0.0003(17) C25 0.0187(18) 0.0149(17) 0.0188(19) -0.0026(15) 0.0022(15) 0.0002(14) C26 0.020(2) 0.033(2) 0.027(2) 0.0069(19) -0.0019(17) 0.0022(17) C27 0.014(2) 0.051(3) 0.041(3) 0.000(2) 0.0036(18) -0.004(2) C28 0.027(2) 0.032(2) 0.031(2) -0.004(2) 0.0146(19) -0.0096(19) C29 0.032(2) 0.027(2) 0.023(2) 0.0040(18) 0.0057(18) -0.0038(18) C30 0.0185(19) 0.031(2) 0.024(2) 0.0043(18) -0.0005(16) -0.0042(17) C31 0.020(2) 0.021(2) 0.030(2) -0.0051(17) 0.0072(17) -0.0040(16) C32 0.023(2) 0.023(2) 0.041(3) -0.008(2) 0.0011(19) -0.0001(17) C33 0.025(2) 0.029(3) 0.067(4) -0.016(3) 0.003(2) 0.001(2) C34 0.027(2) 0.044(3) 0.060(4) -0.033(3) 0.020(2) -0.010(2) C35 0.035(3) 0.061(4) 0.036(3) -0.019(3) 0.011(2) -0.008(3) C36 0.031(2) 0.044(3) 0.031(3) -0.007(2) 0.007(2) 0.002(2) C37 0.0088(16) 0.025(2) 0.026(2) -0.0029(17) 0.0035(14) 0.0005(14) C38 0.021(2) 0.028(2) 0.051(3) 0.002(2) 0.007(2) 0.0004(18) C39 0.030(3) 0.031(3) 0.080(4) 0.006(3) 0.014(3) -0.009(2) C40 0.036(3) 0.024(2) 0.069(4) -0.004(3) 0.005(3) -0.004(2) C41 0.039(3) 0.031(3) 0.040(3) -0.010(2) 0.004(2) 0.005(2) C42 0.020(2) 0.033(2) 0.026(2) -0.0016(19) 0.0050(17) 0.0004(18) C43 0.0167(18) 0.0213(19) 0.0176(19) 0.0042(16) -0.0016(14) -0.0030(15) C44 0.0170(18) 0.0162(18) 0.0193(19) 0.0010(15) -0.0016(15) 0.0000(14) C45 0.0162(18) 0.0206(19) 0.0185(19) 0.0021(15) 0.0037(15) -0.0016(15) C46 0.027(2) 0.0173(19) 0.028(2) 0.0034(17) -0.0008(17) -0.0050(16) C47 0.028(2) 0.017(2) 0.028(2) -0.0019(17) -0.0031(17) 0.0033(17) C48 0.0166(19) 0.024(2) 0.024(2) -0.0004(17) 0.0002(15) 0.0025(16) C49 0.024(2) 0.0121(17) 0.0193(19) -0.0016(15) 0.0027(15) -0.0013(15) C50 0.032(2) 0.025(2) 0.021(2) 0.0042(17) 0.0016(17) 0.0071(18) C51 0.051(3) 0.024(2) 0.015(2) 0.0008(17) 0.0045(19) 0.011(2) C52 0.037(3) 0.027(2) 0.029(2) -0.0038(19) 0.016(2) -0.0065(19) C53 0.022(2) 0.042(3) 0.029(2) -0.006(2) 0.0010(18) -0.009(2) C54 0.025(2) 0.032(2) 0.018(2) -0.0026(18) 0.0013(16) -0.0076(18) C55 0.0153(17) 0.0168(18) 0.0178(18) 0.0011(15) 0.0044(14) -0.0012(14) C56 0.0181(18) 0.0171(18) 0.023(2) -0.0020(16) 0.0049(15) -0.0011(14) C57 0.0207(19) 0.031(2) 0.0169(19) -0.0027(17) 0.0001(15) 0.0010(17) C58 0.020(2) 0.030(2) 0.022(2) 0.0089(18) 0.0030(16) 0.0037(17) C59 0.029(2) 0.0172(19) 0.030(2) 0.0048(17) 0.0050(18) 0.0014(17) C60 0.028(2) 0.0189(19) 0.018(2) -0.0017(16) 0.0019(16) -0.0017(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 As1 C1 1.946(4) . ? As1 C7 1.957(4) . ? As1 S1 2.2660(10) . ? As2 C31 1.949(4) . ? As2 C37 1.954(4) . ? As2 S2 2.2453(11) . ? S1 C13 1.784(4) . ? S2 C43 1.781(4) . ? P1 C19 1.837(4) . ? P1 C14 1.838(4) . ? P1 C25 1.843(4) . ? P2 C55 1.828(4) . ? P2 C44 1.840(4) . ? P2 C49 1.841(4) . ? C1 C6 1.395(5) . ? C1 C2 1.397(5) . ? C2 C3 1.385(6) . ? C3 C4 1.386(6) . ? C4 C5 1.384(6) . ? C5 C6 1.386(6) . ? C7 C12 1.385(5) . ? C7 C8 1.389(5) . ? C8 C9 1.377(6) . ? C9 C10 1.386(6) . ? C10 C11 1.377(6) . ? C11 C12 1.389(6) . ? C13 C18 1.394(5) . ? C13 C14 1.404(5) . ? C14 C15 1.392(5) . ? C15 C16 1.390(6) . ? C16 C17 1.379(6) . ? C17 C18 1.389(6) . ? C19 C24 1.383(6) . ? C19 C20 1.393(6) . ? C20 C21 1.390(6) . ? C21 C22 1.373(6) . ? C22 C23 1.381(7) . ? C23 C24 1.392(6) . ? C25 C30 1.384(6) . ? C25 C26 1.390(6) . ? C26 C27 1.381(6) . ? C27 C28 1.372(7) . ? C28 C29 1.379(6) . ? C29 C30 1.381(6) . ? C31 C36 1.386(6) . ? C31 C32 1.392(6) . ? C32 C33 1.390(7) . ? C33 C34 1.369(8) . ? C34 C35 1.376(8) . ? C35 C36 1.398(7) . ? C37 C38 1.372(6) . ? C37 C42 1.396(6) . ? C38 C39 1.392(7) . ? C39 C40 1.386(8) . ? C40 C41 1.381(7) . ? C41 C42 1.387(7) . ? C43 C48 1.399(6) . ? C43 C44 1.402(6) . ? C44 C45 1.397(5) . ? C45 C46 1.390(6) . ? C46 C47 1.377(6) . ? C47 C48 1.381(6) . ? C49 C54 1.389(6) . ? C49 C50 1.396(6) . ? C50 C51 1.381(6) . ? C51 C52 1.373(7) . ? C52 C53 1.372(7) . ? C53 C54 1.390(6) . ? C55 C56 1.391(5) . ? C55 C60 1.396(5) . ? C56 C57 1.385(6) . ? C57 C58 1.382(6) . ? C58 C59 1.378(6) . ? C59 C60 1.383(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 C1 As1 C7 100.74(16) . . ? C1 As1 S1 99.18(12) . . ? C7 As1 S1 98.32(12) . . ? C31 As2 C37 102.60(17) . . ? C31 As2 S2 101.19(13) . . ? C37 As2 S2 94.76(12) . . ? C13 S1 As1 94.39(13) . . ? C43 S2 As2 98.86(13) . . ? C19 P1 C14 102.15(18) . . ? C19 P1 C25 103.18(18) . . ? C14 P1 C25 100.65(17) . . ? C55 P2 C44 102.82(18) . . ? C55 P2 C49 101.28(17) . . ? C44 P2 C49 101.99(18) . . ? C6 C1 C2 119.2(4) . . ? C6 C1 As1 118.9(3) . . ? C2 C1 As1 120.8(3) . . ? C3 C2 C1 120.2(4) . . ? C2 C3 C4 120.1(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 120.0(4) . . ? C5 C6 C1 120.4(4) . . ? C12 C7 C8 119.0(4) . . ? C12 C7 As1 117.4(3) . . ? C8 C7 As1 123.4(3) . . ? C9 C8 C7 120.7(4) . . ? C8 C9 C10 120.2(4) . . ? C11 C10 C9 119.5(4) . . ? C10 C11 C12 120.5(4) . . ? C7 C12 C11 120.1(4) . . ? C18 C13 C14 120.2(4) . . ? C18 C13 S1 119.4(3) . . ? C14 C13 S1 120.4(3) . . ? C15 C14 C13 118.8(4) . . ? C15 C14 P1 124.2(3) . . ? C13 C14 P1 117.0(3) . . ? C16 C15 C14 120.5(4) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C18 119.7(4) . . ? C17 C18 C13 120.2(4) . . ? C24 C19 C20 118.6(4) . . ? C24 C19 P1 115.9(3) . . ? C20 C19 P1 125.5(3) . . ? C21 C20 C19 120.0(4) . . ? C22 C21 C20 120.9(4) . . ? C21 C22 C23 119.6(4) . . ? C22 C23 C24 119.8(4) . . ? C19 C24 C23 121.1(4) . . ? C30 C25 C26 118.0(4) . . ? C30 C25 P1 124.3(3) . . ? C26 C25 P1 117.5(3) . . ? C27 C26 C25 120.9(4) . . ? C28 C27 C26 120.4(4) . . ? C27 C28 C29 119.4(4) . . ? C28 C29 C30 120.3(4) . . ? C29 C30 C25 121.0(4) . . ? C36 C31 C32 118.9(4) . . ? C36 C31 As2 124.4(3) . . ? C32 C31 As2 116.5(3) . . ? C33 C32 C31 120.8(5) . . ? C34 C33 C32 119.4(5) . . ? C33 C34 C35 121.0(5) . . ? C34 C35 C36 119.7(5) . . ? C31 C36 C35 120.2(5) . . ? C38 C37 C42 119.4(4) . . ? C38 C37 As2 125.6(3) . . ? C42 C37 As2 114.9(3) . . ? C37 C38 C39 120.4(5) . . ? C40 C39 C38 119.9(5) . . ? C41 C40 C39 120.2(5) . . ? C40 C41 C42 119.6(5) . . ? C41 C42 C37 120.4(4) . . ? C48 C43 C44 120.7(4) . . ? C48 C43 S2 119.5(3) . . ? C44 C43 S2 119.8(3) . . ? C45 C44 C43 118.2(4) . . ? C45 C44 P2 123.3(3) . . ? C43 C44 P2 118.3(3) . . ? C46 C45 C44 120.6(4) . . ? C47 C46 C45 120.5(4) . . ? C46 C47 C48 120.2(4) . . ? C47 C48 C43 119.8(4) . . ? C54 C49 C50 118.0(4) . . ? C54 C49 P2 124.7(3) . . ? C50 C49 P2 117.1(3) . . ? C51 C50 C49 120.7(4) . . ? C52 C51 C50 120.4(4) . . ? C53 C52 C51 120.0(4) . . ? C52 C53 C54 120.0(4) . . ? C49 C54 C53 120.9(4) . . ? C56 C55 C60 118.4(4) . . ? C56 C55 P2 124.8(3) . . ? C60 C55 P2 116.8(3) . . ? C57 C56 C55 120.6(4) . . ? C58 C57 C56 120.1(4) . . ? C59 C58 C57 120.2(4) . . ? C58 C59 C60 119.8(4) . . ? C59 C60 C55 121.0(4) . . ? # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-09-01 at 13:17:13 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\xray\wingx\files\archive.dat # CIF files read : x1115fin x1115 data_x1115fin _database_code_depnum_ccdc_archive 'CCDC 856664' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2010-09-01T13:17:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C55 H44 Cl5 P3 Pd3 S3' _chemical_formula_weight 1390.44 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 19.6305(2) _cell_length_b 11.40760(10) _cell_length_c 23.9533(2) _cell_angle_alpha 90 _cell_angle_beta 96.7390(10) _cell_angle_gamma 90 _cell_volume 5326.97(8) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 15893 _cell_measurement_theta_min 2.7994 _cell_measurement_theta_max 32.3716 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.98929 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_orient_matrix_ub_11 0.0305413 _diffrn_orient_matrix_ub_12 -0.0197534 _diffrn_orient_matrix_ub_13 -0.0101197 _diffrn_orient_matrix_ub_21 -0.0161063 _diffrn_orient_matrix_ub_22 -0.0541254 _diffrn_orient_matrix_ub_23 -0.007903 _diffrn_orient_matrix_ub_31 -0.0115024 _diffrn_orient_matrix_ub_32 0.0233466 _diffrn_orient_matrix_ub_33 -0.0269098 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0766 _diffrn_reflns_number 45773 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 16241 _reflns_number_gt 10687 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 16241 _refine_ls_number_parameters 634 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.627 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.721083(10) 0.969227(16) 0.223428(7) 0.01548(4) Uani 1 1 d . . . Pd2 Pd 0.820230(9) 0.754684(16) 0.299148(7) 0.01427(4) Uani 1 1 d . . . Pd3 Pd 0.698847(9) 0.929784(16) 0.374016(7) 0.01449(4) Uani 1 1 d . . . Cl1 Cl 0.72964(4) 1.15776(6) 0.18784(2) 0.02885(15) Uani 1 1 d . . . Cl2 Cl 0.87505(3) 0.76026(6) 0.21856(2) 0.02397(14) Uani 1 1 d . . . Cl3 Cl 0.62506(3) 0.83925(6) 0.43010(2) 0.02528(14) Uani 1 1 d . . . P1 P 0.67940(3) 0.91023(6) 0.13741(2) 0.01729(13) Uani 1 1 d . . . P2 P 0.91709(3) 0.74014(6) 0.35782(2) 0.01622(13) Uani 1 1 d . . . P3 P 0.64049(3) 1.09807(6) 0.37300(2) 0.01711(13) Uani 1 1 d . . . S1 S 0.70893(3) 0.77836(5) 0.24994(2) 0.01603(12) Uani 1 1 d . . . S2 S 0.76401(3) 0.75092(5) 0.37686(2) 0.01569(12) Uani 1 1 d . . . S3 S 0.76879(3) 1.02230(5) 0.31802(2) 0.01538(12) Uani 1 1 d . . . C1 C 0.68481(12) 0.7520(2) 0.13546(9) 0.0167(5) Uani 1 1 d . . . C2 C 0.70226(12) 0.6953(2) 0.18654(9) 0.0171(5) Uani 1 1 d . . . C3 C 0.71003(13) 0.5749(2) 0.18801(10) 0.0225(6) Uani 1 1 d . . . H3 H 0.722 0.5365 0.223 0.027 Uiso 1 1 calc R . . C4 C 0.70058(13) 0.5098(2) 0.13899(10) 0.0257(6) Uani 1 1 d . . . H4 H 0.7059 0.4271 0.1404 0.031 Uiso 1 1 calc R . . C5 C 0.68333(13) 0.5656(2) 0.08787(10) 0.0254(6) Uani 1 1 d . . . H5 H 0.6768 0.5211 0.0542 0.031 Uiso 1 1 calc R . . C6 C 0.67554(13) 0.6862(2) 0.08590(9) 0.0212(6) Uani 1 1 d . . . H6 H 0.6639 0.7243 0.0508 0.025 Uiso 1 1 calc R . . C7 C 0.72713(13) 0.9570(2) 0.08095(9) 0.0208(5) Uani 1 1 d . . . C8 C 0.79757(15) 0.9706(3) 0.09189(12) 0.0400(8) Uani 1 1 d . . . H8 H 0.82 0.9579 0.1288 0.048 Uiso 1 1 calc R . . C9 C 0.83515(17) 1.0026(3) 0.04911(13) 0.0550(10) Uani 1 1 d . . . H9 H 0.8833 1.0142 0.0566 0.066 Uiso 1 1 calc R . . C10 C 0.80220(19) 1.0179(3) -0.00497(13) 0.0491(9) Uani 1 1 d . . . H10 H 0.828 1.0398 -0.0345 0.059 Uiso 1 1 calc R . . C11 C 0.73340(18) 1.0018(3) -0.01586(12) 0.0428(8) Uani 1 1 d . . . H11 H 0.7113 1.0101 -0.0531 0.051 Uiso 1 1 calc R . . C12 C 0.69546(15) 0.9733(2) 0.02736(10) 0.0320(7) Uani 1 1 d . . . H12 H 0.6471 0.965 0.0199 0.038 Uiso 1 1 calc R . . C13 C 0.59035(13) 0.9527(2) 0.11843(9) 0.0190(5) Uani 1 1 d . . . C14 C 0.54549(14) 0.8893(2) 0.08060(10) 0.0281(6) Uani 1 1 d . . . H14 H 0.5603 0.818 0.0655 0.034 Uiso 1 1 calc R . . C15 C 0.47939(14) 0.9292(2) 0.06474(11) 0.0313(7) Uani 1 1 d . . . H15 H 0.4492 0.8856 0.0387 0.038 Uiso 1 1 calc R . . C16 C 0.45761(13) 1.0321(2) 0.08686(10) 0.0276(6) Uani 1 1 d . . . H16 H 0.4127 1.0604 0.0752 0.033 Uiso 1 1 calc R . . C17 C 0.50027(14) 1.0939(2) 0.12557(11) 0.0301(6) Uani 1 1 d . . . H17 H 0.4846 1.1638 0.1414 0.036 Uiso 1 1 calc R . . C18 C 0.56674(14) 1.0541(2) 0.14160(10) 0.0278(6) Uani 1 1 d . . . H18 H 0.5962 1.0967 0.1686 0.033 Uiso 1 1 calc R . . C19 C 0.89666(13) 0.7823(2) 0.42694(9) 0.0172(5) Uani 1 1 d . . . C20 C 0.82773(13) 0.7807(2) 0.43444(9) 0.0170(5) Uani 1 1 d . . . C21 C 0.80803(14) 0.8006(2) 0.48785(9) 0.0281(6) Uani 1 1 d . . . H21 H 0.761 0.7966 0.4936 0.034 Uiso 1 1 calc R . . C22 C 0.85717(15) 0.8261(3) 0.53210(10) 0.0341(7) Uani 1 1 d . . . H22 H 0.8438 0.8387 0.5685 0.041 Uiso 1 1 calc R . . C23 C 0.92564(15) 0.8335(2) 0.52414(10) 0.0300(7) Uani 1 1 d . . . H23 H 0.9589 0.8546 0.5546 0.036 Uiso 1 1 calc R . . C24 C 0.94576(14) 0.8101(2) 0.47163(10) 0.0241(6) Uani 1 1 d . . . H24 H 0.9929 0.813 0.4662 0.029 Uiso 1 1 calc R . . C25 C 0.99085(13) 0.8261(2) 0.34433(9) 0.0188(5) Uani 1 1 d . . . C26 C 0.98236(14) 0.9465(2) 0.33898(9) 0.0239(6) Uani 1 1 d . . . H26 H 0.9387 0.9808 0.3413 0.029 Uiso 1 1 calc R . . C27 C 1.03746(14) 1.0161(2) 0.33035(10) 0.0278(6) Uani 1 1 d . . . H27 H 1.0318 1.0986 0.3273 0.033 Uiso 1 1 calc R . . C28 C 1.10115(14) 0.9665(3) 0.32608(10) 0.0300(6) Uani 1 1 d . . . H28 H 1.1391 1.0149 0.3204 0.036 Uiso 1 1 calc R . . C29 C 1.10906(14) 0.8474(3) 0.33011(10) 0.0321(7) Uani 1 1 d . . . H29 H 1.1525 0.8134 0.3263 0.038 Uiso 1 1 calc R . . C30 C 1.05460(13) 0.7761(2) 0.33961(10) 0.0269(6) Uani 1 1 d . . . H30 H 1.0606 0.6936 0.3429 0.032 Uiso 1 1 calc R . . C31 C 0.94621(12) 0.5905(2) 0.36412(9) 0.0178(5) Uani 1 1 d . . . C32 C 0.95987(14) 0.5327(2) 0.31526(10) 0.0258(6) Uani 1 1 d . . . H32 H 0.9519 0.5721 0.2801 0.031 Uiso 1 1 calc R . . C33 C 0.98451(15) 0.4204(2) 0.31708(11) 0.0326(7) Uani 1 1 d . . . H33 H 0.994 0.3822 0.2836 0.039 Uiso 1 1 calc R . . C34 C 0.99533(18) 0.3635(3) 0.36785(12) 0.0464(9) Uani 1 1 d . . . H34 H 1.0133 0.2861 0.3696 0.056 Uiso 1 1 calc R . . C35 C 0.98038(19) 0.4179(3) 0.41628(11) 0.0501(10) Uani 1 1 d . . . H35 H 0.9869 0.3768 0.451 0.06 Uiso 1 1 calc R . . C36 C 0.95610(15) 0.5312(2) 0.41491(10) 0.0302(7) Uani 1 1 d . . . H36 H 0.9462 0.5684 0.4485 0.036 Uiso 1 1 calc R . . C37 C 0.69411(13) 1.2118(2) 0.34880(9) 0.0172(5) Uani 1 1 d . . . C38 C 0.75125(12) 1.1748(2) 0.32458(9) 0.0162(5) Uani 1 1 d . . . C39 C 0.79611(13) 1.2566(2) 0.30623(9) 0.0226(5) Uani 1 1 d . . . H39 H 0.8349 1.231 0.2892 0.027 Uiso 1 1 calc R . . C40 C 0.78443(14) 1.3747(2) 0.31267(10) 0.0268(6) Uani 1 1 d . . . H40 H 0.8159 1.4303 0.3009 0.032 Uiso 1 1 calc R . . C41 C 0.72699(14) 1.4129(2) 0.33621(9) 0.0247(6) Uani 1 1 d . . . H41 H 0.7185 1.4944 0.3396 0.03 Uiso 1 1 calc R . . C42 C 0.68243(14) 1.3326(2) 0.35455(9) 0.0228(6) Uani 1 1 d . . . H42 H 0.6435 1.3588 0.3712 0.027 Uiso 1 1 calc R . . C43 C 0.56124(13) 1.0938(2) 0.32604(10) 0.0218(6) Uani 1 1 d . . . C44 C 0.52623(15) 1.1951(3) 0.31022(13) 0.0407(8) Uani 1 1 d . . . H44 H 0.5439 1.2684 0.3241 0.049 Uiso 1 1 calc R . . C45 C 0.46588(15) 1.1917(3) 0.27457(13) 0.0469(9) Uani 1 1 d . . . H45 H 0.4424 1.2623 0.2636 0.056 Uiso 1 1 calc R . . C46 C 0.43981(15) 1.0860(3) 0.25500(12) 0.0415(8) Uani 1 1 d . . . H46 H 0.3988 1.0833 0.2297 0.05 Uiso 1 1 calc R . . C47 C 0.47289(18) 0.9848(3) 0.27202(15) 0.0600(11) Uani 1 1 d . . . H47 H 0.4536 0.9114 0.2599 0.072 Uiso 1 1 calc R . . C48 C 0.53455(17) 0.9882(3) 0.30702(13) 0.0495(9) Uani 1 1 d . . . H48 H 0.5581 0.9175 0.3177 0.059 Uiso 1 1 calc R . . C49 C 0.61824(14) 1.1452(2) 0.44064(9) 0.0218(6) Uani 1 1 d . . . C50 C 0.55452(15) 1.1188(2) 0.45696(11) 0.0300(7) Uani 1 1 d . . . H50 H 0.5206 1.0816 0.4314 0.036 Uiso 1 1 calc R . . C51 C 0.54061(18) 1.1470(3) 0.51112(12) 0.0425(9) Uani 1 1 d . . . H51 H 0.497 1.1293 0.5224 0.051 Uiso 1 1 calc R . . C52 C 0.5893(2) 1.1998(3) 0.54783(12) 0.0472(10) Uani 1 1 d . . . H52 H 0.5796 1.2175 0.5848 0.057 Uiso 1 1 calc R . . C53 C 0.65221(18) 1.2278(2) 0.53204(11) 0.0398(8) Uani 1 1 d . . . H53 H 0.6856 1.2654 0.5579 0.048 Uiso 1 1 calc R . . C54 C 0.66703(15) 1.2013(2) 0.47821(10) 0.0283(6) Uani 1 1 d . . . H54 H 0.7104 1.2214 0.4671 0.034 Uiso 1 1 calc R . . Cl4 Cl 1.11251(7) 0.80454(13) 0.57164(5) 0.0449(5) Uiso 0.620(3) 1 d PD A 1 Cl5 Cl 1.15504(9) 0.87333(18) 0.46364(7) 0.0462(4) Uiso 0.620(3) 1 d PD A 1 C55 C 1.1542(3) 0.9117(4) 0.53451(17) 0.0277(11) Uiso 0.620(3) 1 d PD A 1 H55A H 1.1305 0.9878 0.5368 0.033 Uiso 0.620(3) 1 calc PR A 1 H55B H 1.202 0.9212 0.5524 0.033 Uiso 0.620(3) 1 calc PR A 1 Cl4F Cl 1.0916(2) 0.8948(3) 0.56950(15) 0.0401(13) Uiso 0.223(3) 1 d PD B 2 Cl5F Cl 1.1487(2) 0.8303(5) 0.46888(17) 0.0413(13) Uiso 0.223(3) 1 d PD B 2 C55F C 1.1642(7) 0.8472(15) 0.5424(5) 0.047(4) Uiso 0.223(3) 1 d PD B 2 H55C H 1.179 0.7712 0.5598 0.056 Uiso 0.223(3) 1 calc PR B 2 H55D H 1.2017 0.9045 0.5517 0.056 Uiso 0.223(3) 1 calc PR B 2 Cl4G Cl 1.1232(4) 0.9105(6) 0.5503(3) 0.063(2) Uiso 0.153(2) 1 d PD C 3 Cl5G Cl 1.1522(3) 0.7406(6) 0.4687(2) 0.056(2) Uiso 0.153(2) 1 d PD C 3 C55G C 1.124(2) 0.888(2) 0.4759(8) 0.118(15) Uiso 0.153(2) 1 d PD C 3 H55E H 1.0773 0.8993 0.4557 0.142 Uiso 0.153(2) 1 calc PR C 3 H55F H 1.1556 0.944 0.4606 0.142 Uiso 0.153(2) 1 calc PR C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01700(10) 0.01624(9) 0.01294(8) -0.00006(7) 0.00063(7) -0.00134(8) Pd2 0.01410(9) 0.01659(9) 0.01210(8) 0.00049(7) 0.00146(6) 0.00157(8) Pd3 0.01469(9) 0.01528(9) 0.01387(8) 0.00052(7) 0.00326(7) 0.00063(8) Cl1 0.0424(4) 0.0207(3) 0.0218(3) 0.0045(2) -0.0029(3) -0.0078(3) Cl2 0.0221(3) 0.0330(4) 0.0180(3) 0.0020(3) 0.0071(2) 0.0021(3) Cl3 0.0245(4) 0.0256(3) 0.0281(3) 0.0047(3) 0.0129(3) 0.0000(3) P1 0.0199(3) 0.0187(3) 0.0128(3) 0.0004(2) 0.0001(3) -0.0001(3) P2 0.0152(3) 0.0188(3) 0.0145(3) 0.0004(2) 0.0011(2) 0.0024(3) P3 0.0167(3) 0.0175(3) 0.0175(3) 0.0003(2) 0.0036(3) 0.0019(3) S1 0.0160(3) 0.0182(3) 0.0134(3) 0.0002(2) -0.0001(2) 0.0002(2) S2 0.0166(3) 0.0164(3) 0.0145(3) 0.0013(2) 0.0031(2) 0.0016(3) S3 0.0150(3) 0.0172(3) 0.0141(3) -0.0010(2) 0.0023(2) -0.0009(3) C1 0.0159(12) 0.0172(12) 0.0173(11) -0.0012(10) 0.0026(9) 0.0004(11) C2 0.0132(12) 0.0208(13) 0.0171(11) -0.0014(10) 0.0008(10) -0.0015(10) C3 0.0255(14) 0.0235(14) 0.0176(12) 0.0035(10) -0.0014(11) 0.0016(12) C4 0.0287(15) 0.0181(14) 0.0305(14) -0.0046(11) 0.0038(12) -0.0014(12) C5 0.0290(15) 0.0276(15) 0.0196(12) -0.0065(11) 0.0028(11) -0.0010(13) C6 0.0239(14) 0.0262(14) 0.0138(11) -0.0007(10) 0.0032(10) 0.0001(12) C7 0.0266(14) 0.0194(14) 0.0170(12) 0.0010(10) 0.0045(11) 0.0002(11) C8 0.0300(17) 0.060(2) 0.0304(15) 0.0082(15) 0.0051(13) 0.0022(17) C9 0.0323(19) 0.083(3) 0.054(2) 0.0095(19) 0.0212(17) -0.0054(19) C10 0.068(3) 0.045(2) 0.0417(18) 0.0151(15) 0.0373(18) 0.0126(19) C11 0.057(2) 0.049(2) 0.0245(15) 0.0141(13) 0.0139(15) 0.0175(18) C12 0.0341(17) 0.0420(18) 0.0202(13) 0.0074(12) 0.0051(12) 0.0068(15) C13 0.0196(13) 0.0201(14) 0.0168(11) 0.0035(10) -0.0006(10) -0.0009(11) C14 0.0266(15) 0.0254(15) 0.0305(15) -0.0039(11) -0.0038(12) 0.0014(13) C15 0.0250(15) 0.0326(16) 0.0334(15) -0.0005(13) -0.0093(12) -0.0030(14) C16 0.0178(14) 0.0354(16) 0.0294(14) 0.0072(12) 0.0022(11) 0.0015(13) C17 0.0268(16) 0.0285(16) 0.0351(15) -0.0033(12) 0.0046(13) 0.0076(13) C18 0.0228(14) 0.0310(16) 0.0285(14) -0.0059(12) -0.0015(12) 0.0020(13) C19 0.0204(13) 0.0170(13) 0.0139(11) 0.0007(9) 0.0006(10) 0.0043(10) C20 0.0228(13) 0.0164(13) 0.0114(11) 0.0010(9) 0.0000(10) 0.0021(10) C21 0.0250(15) 0.0418(17) 0.0183(13) 0.0006(11) 0.0063(11) 0.0057(13) C22 0.0394(18) 0.0466(19) 0.0157(13) -0.0019(12) 0.0011(12) 0.0133(16) C23 0.0349(17) 0.0347(17) 0.0176(13) -0.0036(11) -0.0089(12) 0.0080(14) C24 0.0241(15) 0.0249(14) 0.0212(13) -0.0010(11) -0.0058(11) 0.0036(12) C25 0.0186(13) 0.0251(14) 0.0124(11) -0.0002(10) 0.0002(10) -0.0021(11) C26 0.0241(14) 0.0240(15) 0.0246(13) 0.0021(10) 0.0068(11) 0.0021(12) C27 0.0346(17) 0.0241(15) 0.0251(13) -0.0008(11) 0.0058(12) -0.0053(13) C28 0.0250(15) 0.0407(18) 0.0242(13) 0.0023(12) 0.0019(12) -0.0113(14) C29 0.0188(15) 0.0466(19) 0.0314(15) 0.0038(13) 0.0055(12) -0.0006(14) C30 0.0237(15) 0.0282(16) 0.0284(14) 0.0032(11) 0.0013(11) 0.0008(12) C31 0.0151(12) 0.0195(13) 0.0183(12) -0.0006(10) 0.0007(10) 0.0020(10) C32 0.0287(15) 0.0288(15) 0.0202(12) 0.0019(11) 0.0039(11) 0.0084(13) C33 0.0408(18) 0.0319(17) 0.0247(14) -0.0029(12) 0.0018(13) 0.0109(15) C34 0.075(3) 0.0286(17) 0.0355(17) 0.0011(13) 0.0048(17) 0.0245(17) C35 0.093(3) 0.0353(19) 0.0218(15) 0.0076(13) 0.0051(16) 0.0299(19) C36 0.0438(18) 0.0287(16) 0.0183(13) -0.0008(11) 0.0043(12) 0.0104(14) C37 0.0224(13) 0.0163(12) 0.0123(11) -0.0012(9) -0.0001(10) -0.0002(10) C38 0.0207(13) 0.0146(12) 0.0128(11) -0.0008(9) -0.0001(10) -0.0023(10) C39 0.0245(14) 0.0239(14) 0.0198(12) 0.0007(11) 0.0037(10) -0.0045(12) C40 0.0356(17) 0.0214(14) 0.0228(13) 0.0024(11) 0.0016(12) -0.0104(13) C41 0.0374(17) 0.0163(13) 0.0195(12) 0.0024(10) -0.0006(12) -0.0021(12) C42 0.0314(16) 0.0202(14) 0.0164(12) -0.0014(10) 0.0006(11) 0.0040(12) C43 0.0167(13) 0.0260(15) 0.0232(13) -0.0013(11) 0.0048(10) 0.0007(11) C44 0.0262(17) 0.0286(17) 0.064(2) 0.0111(15) -0.0095(15) -0.0007(14) C45 0.0260(17) 0.044(2) 0.068(2) 0.0242(17) -0.0090(16) 0.0008(16) C46 0.0237(16) 0.064(2) 0.0348(16) -0.0066(16) -0.0064(13) 0.0145(17) C47 0.045(2) 0.047(2) 0.080(3) -0.0335(19) -0.0259(19) 0.0111(19) C48 0.041(2) 0.0344(19) 0.066(2) -0.0194(16) -0.0229(17) 0.0148(16) C49 0.0302(15) 0.0182(13) 0.0185(12) 0.0024(10) 0.0089(11) 0.0056(12) C50 0.0366(18) 0.0213(15) 0.0351(15) 0.0048(12) 0.0166(13) 0.0053(13) C51 0.058(2) 0.0295(17) 0.0467(19) 0.0088(14) 0.0367(17) 0.0126(16) C52 0.094(3) 0.0265(17) 0.0268(16) 0.0066(13) 0.0308(18) 0.0196(19) C53 0.072(2) 0.0278(17) 0.0200(13) 0.0020(11) 0.0084(15) 0.0072(16) C54 0.0404(18) 0.0233(14) 0.0216(13) 0.0018(11) 0.0053(12) 0.0060(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2299(6) . ? Pd1 S1 2.2884(6) . ? Pd1 Cl1 2.3268(6) . ? Pd1 S3 2.4249(6) . ? Pd2 P2 2.2340(6) . ? Pd2 S2 2.2730(5) . ? Pd2 Cl2 2.3186(6) . ? Pd2 S1 2.3731(6) . ? Pd3 P3 2.2343(7) . ? Pd3 S3 2.2870(6) . ? Pd3 Cl3 2.3295(6) . ? Pd3 S2 2.4050(6) . ? P1 C1 1.809(2) . ? P1 C7 1.814(2) . ? P1 C13 1.819(3) . ? P2 C31 1.801(2) . ? P2 C25 1.809(2) . ? P2 C19 1.814(2) . ? P3 C37 1.808(2) . ? P3 C49 1.808(2) . ? P3 C43 1.810(3) . ? S1 C2 1.782(2) . ? S2 C20 1.783(2) . ? S3 C38 1.784(2) . ? C1 C2 1.391(3) . ? C1 C6 1.399(3) . ? C2 C3 1.382(3) . ? C3 C4 1.383(3) . ? C4 C5 1.386(3) . ? C5 C6 1.384(3) . ? C7 C12 1.372(3) . ? C7 C8 1.386(4) . ? C8 C9 1.380(4) . ? C9 C10 1.389(4) . ? C10 C11 1.358(4) . ? C11 C12 1.383(4) . ? C13 C18 1.386(3) . ? C13 C14 1.390(3) . ? C14 C15 1.385(4) . ? C15 C16 1.377(4) . ? C16 C17 1.370(4) . ? C17 C18 1.392(4) . ? C19 C20 1.386(3) . ? C19 C24 1.390(3) . ? C20 C21 1.398(3) . ? C21 C22 1.378(3) . ? C22 C23 1.382(4) . ? C23 C24 1.388(3) . ? C25 C26 1.387(3) . ? C25 C30 1.392(3) . ? C26 C27 1.377(3) . ? C27 C28 1.387(4) . ? C28 C29 1.369(4) . ? C29 C30 1.384(3) . ? C31 C36 1.386(3) . ? C31 C32 1.396(3) . ? C32 C33 1.369(3) . ? C33 C34 1.372(4) . ? C34 C35 1.377(4) . ? C35 C36 1.377(4) . ? C37 C38 1.387(3) . ? C37 C42 1.407(3) . ? C38 C39 1.389(3) . ? C39 C40 1.379(3) . ? C40 C41 1.389(3) . ? C41 C42 1.374(3) . ? C43 C48 1.370(4) . ? C43 C44 1.375(4) . ? C44 C45 1.377(4) . ? C45 C46 1.371(4) . ? C46 C47 1.364(4) . ? C47 C48 1.390(4) . ? C49 C50 1.387(3) . ? C49 C54 1.391(4) . ? C50 C51 1.395(3) . ? C51 C52 1.361(4) . ? C52 C53 1.371(4) . ? C53 C54 1.388(3) . ? Cl4 C55 1.769(5) . ? Cl5 C55 1.755(5) . ? Cl4F C55F 1.721(13) . ? Cl5F C55F 1.763(11) . ? Cl4G C55G 1.802(18) . ? Cl5G C55G 1.789(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 S1 86.01(2) . . ? P1 Pd1 Cl1 88.56(2) . . ? S1 Pd1 Cl1 174.57(2) . . ? P1 Pd1 S3 176.78(2) . . ? S1 Pd1 S3 91.13(2) . . ? Cl1 Pd1 S3 94.30(2) . . ? P2 Pd2 S2 86.71(2) . . ? P2 Pd2 Cl2 94.70(2) . . ? S2 Pd2 Cl2 178.54(2) . . ? P2 Pd2 S1 170.73(2) . . ? S2 Pd2 S1 84.36(2) . . ? Cl2 Pd2 S1 94.22(2) . . ? P3 Pd3 S3 86.53(2) . . ? P3 Pd3 Cl3 91.98(2) . . ? S3 Pd3 Cl3 178.35(2) . . ? P3 Pd3 S2 178.48(2) . . ? S3 Pd3 S2 93.10(2) . . ? Cl3 Pd3 S2 88.41(2) . . ? C1 P1 C7 103.74(11) . . ? C1 P1 C13 108.47(11) . . ? C7 P1 C13 107.49(11) . . ? C1 P1 Pd1 107.98(7) . . ? C7 P1 Pd1 115.75(8) . . ? C13 P1 Pd1 112.84(8) . . ? C31 P2 C25 106.02(11) . . ? C31 P2 C19 106.08(10) . . ? C25 P2 C19 106.65(11) . . ? C31 P2 Pd2 111.20(8) . . ? C25 P2 Pd2 119.16(8) . . ? C19 P2 Pd2 106.95(8) . . ? C37 P3 C49 106.56(11) . . ? C37 P3 C43 108.07(11) . . ? C49 P3 C43 106.52(12) . . ? C37 P3 Pd3 107.62(8) . . ? C49 P3 Pd3 115.02(8) . . ? C43 P3 Pd3 112.70(9) . . ? C2 S1 Pd1 105.61(8) . . ? C2 S1 Pd2 109.52(8) . . ? Pd1 S1 Pd2 97.25(2) . . ? C20 S2 Pd2 105.43(8) . . ? C20 S2 Pd3 100.52(8) . . ? Pd2 S2 Pd3 105.58(2) . . ? C38 S3 Pd3 105.25(8) . . ? C38 S3 Pd1 105.57(7) . . ? Pd3 S3 Pd1 103.89(2) . . ? C2 C1 C6 119.4(2) . . ? C2 C1 P1 116.79(17) . . ? C6 C1 P1 123.76(18) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 S1 120.67(18) . . ? C1 C2 S1 119.21(18) . . ? C2 C3 C4 120.6(2) . . ? C3 C4 C5 119.9(2) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C1 120.1(2) . . ? C12 C7 C8 119.6(2) . . ? C12 C7 P1 121.4(2) . . ? C8 C7 P1 118.90(19) . . ? C9 C8 C7 119.8(3) . . ? C8 C9 C10 119.6(3) . . ? C11 C10 C9 120.4(3) . . ? C10 C11 C12 119.9(3) . . ? C7 C12 C11 120.5(3) . . ? C18 C13 C14 118.6(2) . . ? C18 C13 P1 118.61(19) . . ? C14 C13 P1 122.7(2) . . ? C15 C14 C13 120.6(3) . . ? C16 C15 C14 119.8(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 119.8(3) . . ? C13 C18 C17 120.6(3) . . ? C20 C19 C24 120.2(2) . . ? C20 C19 P2 116.02(17) . . ? C24 C19 P2 123.77(19) . . ? C19 C20 C21 119.7(2) . . ? C19 C20 S2 120.61(16) . . ? C21 C20 S2 119.66(19) . . ? C22 C21 C20 119.6(2) . . ? C21 C22 C23 120.7(2) . . ? C22 C23 C24 119.9(2) . . ? C23 C24 C19 119.8(2) . . ? C26 C25 C30 119.9(2) . . ? C26 C25 P2 117.59(19) . . ? C30 C25 P2 122.5(2) . . ? C27 C26 C25 119.8(2) . . ? C26 C27 C28 120.5(3) . . ? C29 C28 C27 119.7(3) . . ? C28 C29 C30 120.8(3) . . ? C29 C30 C25 119.4(3) . . ? C36 C31 C32 119.0(2) . . ? C36 C31 P2 123.15(18) . . ? C32 C31 P2 117.87(18) . . ? C33 C32 C31 121.1(2) . . ? C32 C33 C34 119.2(2) . . ? C33 C34 C35 120.5(3) . . ? C36 C35 C34 120.7(3) . . ? C35 C36 C31 119.5(2) . . ? C38 C37 C42 119.2(2) . . ? C38 C37 P3 116.47(18) . . ? C42 C37 P3 124.32(19) . . ? C37 C38 C39 120.1(2) . . ? C37 C38 S3 120.45(18) . . ? C39 C38 S3 119.38(18) . . ? C40 C39 C38 120.0(2) . . ? C39 C40 C41 120.4(2) . . ? C42 C41 C40 119.9(2) . . ? C41 C42 C37 120.3(2) . . ? C48 C43 C44 119.2(2) . . ? C48 C43 P3 119.8(2) . . ? C44 C43 P3 120.9(2) . . ? C43 C44 C45 120.9(3) . . ? C46 C45 C44 119.7(3) . . ? C47 C46 C45 119.8(3) . . ? C46 C47 C48 120.5(3) . . ? C43 C48 C47 119.8(3) . . ? C50 C49 C54 119.5(2) . . ? C50 C49 P3 120.6(2) . . ? C54 C49 P3 119.7(2) . . ? C49 C50 C51 119.6(3) . . ? C52 C51 C50 120.3(3) . . ? C51 C52 C53 120.8(3) . . ? C52 C53 C54 120.0(3) . . ? C53 C54 C49 119.9(3) . . ? Cl5 C55 Cl4 111.8(3) . . ? Cl4F C55F Cl5F 110.9(8) . . ? Cl5G C55G Cl4G 105.4(11) . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-03-14 at 11:02:44 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : x1231fin x1231 data_x1231fin _database_code_depnum_ccdc_archive 'CCDC 856665' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2011-03-14T11:02:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C56 H46 Cl7 P3 Pd3 S3' _chemical_formula_weight 1475.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 17.0782(4) _cell_length_b 11.9468(3) _cell_length_c 28.3540(7) _cell_angle_alpha 90 _cell_angle_beta 100.312(2) _cell_angle_gamma 90 _cell_volume 5691.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 7411 _cell_measurement_theta_min 2.8621 _cell_measurement_theta_max 28.5514 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'thin needles' _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.98634 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0308189 _diffrn_orient_matrix_ub_12 0.0097314 _diffrn_orient_matrix_ub_13 0.0132733 _diffrn_orient_matrix_ub_21 -0.0281024 _diffrn_orient_matrix_ub_22 0.002854 _diffrn_orient_matrix_ub_23 -0.0216578 _diffrn_orient_matrix_ub_31 -0.0064713 _diffrn_orient_matrix_ub_32 -0.0585054 _diffrn_orient_matrix_ub_33 0.00116 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_unetI/netI 0.1002 _diffrn_reflns_number 44068 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 11622 _reflns_number_gt 8047 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0266P)^2^+20.9719P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11622 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.449 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.15 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' S S 0.1246 0.1234 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.76394(3) 0.36272(4) 0.351577(19) 0.01482(13) Uani 1 1 d . . . Pd2 Pd 0.92169(3) 0.20642(4) 0.330615(18) 0.01533(13) Uani 1 1 d . . . Pd3 Pd 0.73359(3) 0.19847(4) 0.242909(19) 0.01785(13) Uani 1 1 d . . . Cl1 Cl 0.97193(12) 0.26976(14) 0.40803(6) 0.0278(4) Uani 1 1 d . . . Cl2 Cl 0.61492(11) 0.29899(16) 0.23145(7) 0.0301(4) Uani 1 1 d . . . Cl3 Cl 0.73444(11) 0.18767(16) 0.16105(6) 0.0311(5) Uani 1 1 d . . . S1 S 0.86363(10) 0.38132(14) 0.30493(6) 0.0168(4) Uani 1 1 d . . . S2 S 0.73241(10) 0.18169(14) 0.32293(6) 0.0175(4) Uani 1 1 d . . . S3 S 0.86481(10) 0.14150(14) 0.25698(6) 0.0169(4) Uani 1 1 d . . . P1 P 0.80355(11) 0.53705(14) 0.37804(7) 0.0166(4) Uani 1 1 d . . . P2 P 0.66021(11) 0.34341(15) 0.39041(7) 0.0183(4) Uani 1 1 d . . . P3 P 0.97405(11) 0.03708(14) 0.34594(6) 0.0169(4) Uani 1 1 d . . . C1 C 0.9057(4) 0.5524(5) 0.3699(2) 0.0142(15) Uani 1 1 d . . . C2 C 0.9303(4) 0.4833(5) 0.3358(2) 0.0171(15) Uani 1 1 d . . . C3 C 1.0062(4) 0.4925(5) 0.3261(3) 0.0210(16) Uani 1 1 d . . . H3 H 1.0227 0.4454 0.3027 0.025 Uiso 1 1 calc R . . C4 C 1.0586(4) 0.5703(5) 0.3504(3) 0.0204(16) Uani 1 1 d . . . H4 H 1.1109 0.5766 0.3436 0.024 Uiso 1 1 calc R . . C5 C 1.0349(4) 0.6383(6) 0.3844(3) 0.0217(16) Uani 1 1 d . . . H5 H 1.0713 0.6906 0.4015 0.026 Uiso 1 1 calc R . . C6 C 0.9579(4) 0.6309(6) 0.3939(3) 0.0234(17) Uani 1 1 d . . . H6 H 0.9412 0.6794 0.4167 0.028 Uiso 1 1 calc R . . C7 C 0.7497(4) 0.6439(5) 0.3405(2) 0.0187(15) Uani 1 1 d . . . C8 C 0.6940(5) 0.6114(6) 0.3004(3) 0.0298(19) Uani 1 1 d . . . H8 H 0.6823 0.5343 0.2948 0.036 Uiso 1 1 calc R . . C9 C 0.6563(5) 0.6897(7) 0.2692(3) 0.040(2) Uani 1 1 d . . . H9 H 0.6187 0.667 0.242 0.048 Uiso 1 1 calc R . . C10 C 0.6732(5) 0.8023(7) 0.2773(3) 0.035(2) Uani 1 1 d . . . H10 H 0.647 0.8567 0.2556 0.042 Uiso 1 1 calc R . . C11 C 0.7274(5) 0.8358(6) 0.3163(3) 0.0292(19) Uani 1 1 d . . . H11 H 0.7386 0.9131 0.3217 0.035 Uiso 1 1 calc R . . C12 C 0.7660(4) 0.7568(6) 0.3479(3) 0.0241(17) Uani 1 1 d . . . H12 H 0.8039 0.7801 0.3748 0.029 Uiso 1 1 calc R . . C13 C 0.8081(4) 0.5750(5) 0.4405(2) 0.0178(15) Uani 1 1 d . . . C14 C 0.8631(4) 0.5187(6) 0.4744(3) 0.0270(18) Uani 1 1 d . . . H14 H 0.8952 0.4612 0.4647 0.032 Uiso 1 1 calc R . . C15 C 0.8709(5) 0.5466(7) 0.5219(3) 0.037(2) Uani 1 1 d . . . H15 H 0.9102 0.5107 0.5449 0.044 Uiso 1 1 calc R . . C16 C 0.8222(5) 0.6263(7) 0.5367(3) 0.0311(19) Uani 1 1 d . . . H16 H 0.8268 0.6427 0.5698 0.037 Uiso 1 1 calc R . . C17 C 0.7670(4) 0.6823(6) 0.5039(3) 0.0275(18) Uani 1 1 d . . . H17 H 0.7336 0.7376 0.5141 0.033 Uiso 1 1 calc R . . C18 C 0.7607(4) 0.6567(6) 0.4554(3) 0.0221(16) Uani 1 1 d . . . H18 H 0.7234 0.6958 0.4324 0.026 Uiso 1 1 calc R . . C19 C 0.6007(4) 0.2273(5) 0.3628(3) 0.0214(17) Uani 1 1 d . . . C20 C 0.6328(4) 0.1600(6) 0.3317(2) 0.0199(16) Uani 1 1 d . . . C21 C 0.5886(4) 0.0707(6) 0.3088(3) 0.0228(17) Uani 1 1 d . . . H21 H 0.6095 0.0264 0.2862 0.027 Uiso 1 1 calc R . . C22 C 0.5150(4) 0.0472(6) 0.3192(3) 0.0294(19) Uani 1 1 d . . . H22 H 0.4855 -0.0145 0.3042 0.035 Uiso 1 1 calc R . . C23 C 0.4833(4) 0.1125(6) 0.3513(3) 0.034(2) Uani 1 1 d . . . H23 H 0.4324 0.0955 0.3585 0.04 Uiso 1 1 calc R . . C24 C 0.5258(4) 0.2025(6) 0.3729(3) 0.0298(18) Uani 1 1 d . . . H24 H 0.5039 0.2478 0.3949 0.036 Uiso 1 1 calc R . . C25 C 0.6878(4) 0.3047(6) 0.4528(2) 0.0223(16) Uani 1 1 d . . . C26 C 0.6359(5) 0.3104(6) 0.4854(3) 0.0301(18) Uani 1 1 d . . . H26 H 0.5848 0.343 0.4758 0.036 Uiso 1 1 calc R . . C27 C 0.6571(5) 0.2700(6) 0.5309(3) 0.038(2) Uani 1 1 d . . . H27 H 0.6216 0.2767 0.553 0.046 Uiso 1 1 calc R . . C28 C 0.7310(5) 0.2189(8) 0.5449(3) 0.044(2) Uani 1 1 d . . . H28 H 0.7462 0.1906 0.5765 0.053 Uiso 1 1 calc R . . C29 C 0.7812(5) 0.2099(8) 0.5130(3) 0.042(2) Uani 1 1 d . . . H29 H 0.8309 0.1732 0.5223 0.051 Uiso 1 1 calc R . . C30 C 0.7609(5) 0.2534(7) 0.4672(3) 0.033(2) Uani 1 1 d . . . H30 H 0.7973 0.2481 0.4456 0.039 Uiso 1 1 calc R . . C31 C 0.5927(4) 0.4603(6) 0.3843(3) 0.0209(16) Uani 1 1 d . . . C32 C 0.5932(4) 0.5393(6) 0.4199(3) 0.0257(17) Uani 1 1 d . . . H32 H 0.6262 0.529 0.4503 0.031 Uiso 1 1 calc R . . C33 C 0.5450(5) 0.6348(6) 0.4112(3) 0.034(2) Uani 1 1 d . . . H33 H 0.5457 0.6894 0.4356 0.04 Uiso 1 1 calc R . . C34 C 0.4971(5) 0.6495(7) 0.3676(3) 0.038(2) Uani 1 1 d . . . H34 H 0.4644 0.7142 0.3618 0.046 Uiso 1 1 calc R . . C35 C 0.4959(5) 0.5703(7) 0.3317(3) 0.042(2) Uani 1 1 d . . . H35 H 0.4625 0.581 0.3015 0.05 Uiso 1 1 calc R . . C36 C 0.5431(5) 0.4761(7) 0.3399(3) 0.037(2) Uani 1 1 d . . . H36 H 0.5419 0.4218 0.3152 0.045 Uiso 1 1 calc R . . C37 C 0.9274(4) -0.0548(6) 0.2982(2) 0.0181(15) Uani 1 1 d . . . C38 C 0.8731(4) -0.0075(5) 0.2614(2) 0.0133(14) Uani 1 1 d . . . C39 C 0.8314(4) -0.0735(6) 0.2257(2) 0.0204(16) Uani 1 1 d . . . H39 H 0.7924 -0.0409 0.2015 0.024 Uiso 1 1 calc R . . C40 C 0.8463(4) -0.1872(6) 0.2250(3) 0.0246(17) Uani 1 1 d . . . H40 H 0.8182 -0.2325 0.2001 0.029 Uiso 1 1 calc R . . C41 C 0.9020(4) -0.2345(6) 0.2607(3) 0.0242(17) Uani 1 1 d . . . H41 H 0.9124 -0.3126 0.26 0.029 Uiso 1 1 calc R . . C42 C 0.9429(4) -0.1696(6) 0.2973(3) 0.0228(17) Uani 1 1 d . . . H42 H 0.9812 -0.2028 0.3218 0.027 Uiso 1 1 calc R . . C43 C 1.0805(4) 0.0331(5) 0.3484(2) 0.0190(16) Uani 1 1 d . . . C44 C 1.1159(4) -0.0229(6) 0.3155(3) 0.0241(17) Uani 1 1 d . . . H44 H 1.0837 -0.0621 0.29 0.029 Uiso 1 1 calc R . . C45 C 1.1981(5) -0.0230(7) 0.3191(3) 0.033(2) Uani 1 1 d . . . H45 H 1.2218 -0.0621 0.2961 0.039 Uiso 1 1 calc R . . C46 C 1.2450(5) 0.0336(7) 0.3560(3) 0.037(2) Uani 1 1 d . . . H46 H 1.3013 0.0341 0.3588 0.045 Uiso 1 1 calc R . . C47 C 1.2093(5) 0.0893(7) 0.3887(3) 0.042(2) Uani 1 1 d . . . H47 H 1.2416 0.1266 0.4148 0.05 Uiso 1 1 calc R . . C48 C 1.1285(4) 0.0924(6) 0.3847(3) 0.0290(18) Uani 1 1 d . . . H48 H 1.105 0.1352 0.4068 0.035 Uiso 1 1 calc R . . C49 C 0.9565(4) -0.0269(5) 0.4014(2) 0.0159(15) Uani 1 1 d . . . C50 C 1.0133(4) -0.0892(6) 0.4304(3) 0.0231(17) Uani 1 1 d . . . H50 H 1.0645 -0.0988 0.4223 0.028 Uiso 1 1 calc R . . C51 C 0.9956(5) -0.1380(6) 0.4715(3) 0.0265(18) Uani 1 1 d . . . H51 H 1.0352 -0.1807 0.4915 0.032 Uiso 1 1 calc R . . C52 C 0.9219(5) -0.1259(6) 0.4838(3) 0.0299(19) Uani 1 1 d . . . H52 H 0.91 -0.1615 0.5117 0.036 Uiso 1 1 calc R . . C53 C 0.8655(5) -0.0617(6) 0.4555(3) 0.0283(18) Uani 1 1 d . . . H53 H 0.8147 -0.0518 0.464 0.034 Uiso 1 1 calc R . . C54 C 0.8824(4) -0.0112(6) 0.4145(3) 0.0244(17) Uani 1 1 d . . . H54 H 0.8435 0.0341 0.3952 0.029 Uiso 1 1 calc R . . Cl4 Cl 0.58141(12) 0.5781(2) 0.54172(8) 0.0429(5) Uani 1 1 d . . . Cl5 Cl 0.67335(15) 0.6631(2) 0.63005(10) 0.0630(8) Uani 1 1 d . . . C55 C 0.6484(5) 0.5459(7) 0.5945(3) 0.043(2) Uani 1 1 d . . . H55A H 0.6241 0.4892 0.6129 0.051 Uiso 1 1 calc R . . H55B H 0.6973 0.5132 0.5861 0.051 Uiso 1 1 calc R . . Cl6 Cl 0.64306(18) 0.9293(3) 0.42373(12) 0.0785(9) Uani 1 1 d . . . Cl7 Cl 0.5893(2) 0.8955(3) 0.51402(13) 0.0962(11) Uani 1 1 d . . . C56 C 0.6019(11) 0.9884(11) 0.4674(5) 0.133(7) Uani 1 1 d . . . H56A H 0.5494 1.0195 0.4529 0.16 Uiso 1 1 calc R . . H56B H 0.636 1.0515 0.4813 0.16 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 0.0169(3) 0.0137(3) 0.0143(3) -0.0017(2) 0.0040(2) -0.0010(2) Pd2 0.0202(3) 0.0129(3) 0.0128(3) -0.0013(2) 0.0026(2) -0.0002(2) Pd3 0.0211(3) 0.0168(3) 0.0144(3) -0.0020(2) 0.0000(2) 0.0033(2) Cl1 0.0442(12) 0.0180(9) 0.0172(10) -0.0029(7) -0.0049(8) 0.0009(8) Cl2 0.0313(10) 0.0295(10) 0.0278(10) -0.0009(9) 0.0005(8) 0.0123(9) Cl3 0.0362(11) 0.0386(11) 0.0163(10) -0.0026(9) -0.0009(8) 0.0097(9) S1 0.0229(9) 0.0140(8) 0.0143(9) -0.0008(7) 0.0054(7) -0.0024(7) S2 0.0188(9) 0.0168(9) 0.0169(9) -0.0028(7) 0.0030(7) -0.0012(7) S3 0.0217(9) 0.0158(9) 0.0129(9) 0.0003(7) 0.0025(7) 0.0011(7) P1 0.0176(10) 0.0159(9) 0.0171(10) -0.0031(8) 0.0052(8) -0.0013(8) P2 0.0171(10) 0.0205(10) 0.0174(10) -0.0008(8) 0.0038(8) -0.0004(8) P3 0.0206(10) 0.0150(9) 0.0147(10) -0.0017(8) 0.0019(8) -0.0004(8) C1 0.016(4) 0.011(3) 0.015(4) 0.003(3) 0.003(3) 0.001(3) C2 0.018(4) 0.014(3) 0.016(4) 0.003(3) -0.007(3) -0.006(3) C3 0.033(4) 0.014(4) 0.018(4) 0.000(3) 0.010(3) 0.001(3) C4 0.019(4) 0.017(4) 0.027(4) 0.006(3) 0.007(3) 0.000(3) C5 0.020(4) 0.022(4) 0.021(4) 0.003(3) 0.000(3) -0.005(3) C6 0.032(4) 0.013(3) 0.026(4) 0.001(3) 0.005(3) 0.004(3) C7 0.021(4) 0.016(3) 0.021(4) 0.004(3) 0.006(3) -0.003(3) C8 0.035(5) 0.025(4) 0.027(5) 0.001(4) -0.001(4) -0.001(4) C9 0.048(5) 0.033(5) 0.029(5) -0.005(4) -0.019(4) 0.004(4) C10 0.048(5) 0.030(4) 0.024(4) 0.013(4) -0.001(4) 0.011(4) C11 0.039(5) 0.020(4) 0.028(5) 0.004(3) 0.005(4) 0.007(3) C12 0.023(4) 0.030(4) 0.021(4) 0.001(3) 0.007(3) -0.004(3) C13 0.019(4) 0.017(4) 0.018(4) -0.005(3) 0.004(3) -0.009(3) C14 0.034(5) 0.024(4) 0.023(4) 0.000(3) 0.003(4) 0.007(4) C15 0.043(5) 0.040(5) 0.023(5) 0.005(4) -0.006(4) 0.000(4) C16 0.035(5) 0.039(5) 0.019(4) -0.011(4) 0.007(4) -0.010(4) C17 0.033(5) 0.028(4) 0.027(4) -0.010(4) 0.020(4) -0.004(4) C18 0.020(4) 0.023(4) 0.026(4) 0.002(3) 0.010(3) 0.002(3) C19 0.025(4) 0.018(4) 0.020(4) -0.003(3) 0.001(3) -0.007(3) C20 0.023(4) 0.020(4) 0.016(4) 0.003(3) 0.000(3) 0.005(3) C21 0.025(4) 0.024(4) 0.017(4) 0.005(3) 0.001(3) 0.007(3) C22 0.025(4) 0.025(4) 0.036(5) 0.002(4) -0.002(4) -0.002(3) C23 0.010(4) 0.035(5) 0.053(6) -0.001(4) -0.002(4) -0.010(3) C24 0.020(4) 0.030(4) 0.040(5) -0.003(4) 0.008(4) -0.004(4) C25 0.025(4) 0.025(4) 0.017(4) 0.000(3) 0.006(3) -0.002(3) C26 0.031(4) 0.029(4) 0.029(5) 0.005(4) 0.004(4) 0.005(4) C27 0.050(6) 0.037(5) 0.036(5) 0.010(4) 0.029(4) 0.014(4) C28 0.057(6) 0.060(6) 0.014(4) 0.008(4) 0.004(4) 0.009(5) C29 0.031(5) 0.066(6) 0.028(5) 0.003(5) -0.003(4) 0.023(5) C30 0.023(4) 0.046(5) 0.028(5) -0.003(4) 0.000(4) -0.001(4) C31 0.019(4) 0.025(4) 0.021(4) 0.009(3) 0.011(3) 0.005(3) C32 0.024(4) 0.032(4) 0.023(4) 0.000(4) 0.011(3) -0.002(3) C33 0.034(5) 0.024(4) 0.044(5) -0.006(4) 0.007(4) 0.011(4) C34 0.031(5) 0.033(5) 0.053(6) 0.004(5) 0.011(4) 0.010(4) C35 0.041(5) 0.044(5) 0.041(6) 0.003(5) 0.006(4) 0.010(4) C36 0.044(5) 0.035(5) 0.031(5) -0.007(4) 0.000(4) 0.013(4) C37 0.016(4) 0.022(4) 0.015(4) 0.001(3) 0.001(3) 0.000(3) C38 0.016(4) 0.013(3) 0.014(4) -0.002(3) 0.011(3) -0.003(3) C39 0.021(4) 0.023(4) 0.017(4) -0.001(3) 0.004(3) 0.000(3) C40 0.033(4) 0.021(4) 0.020(4) -0.005(3) 0.005(3) -0.011(3) C41 0.034(5) 0.016(4) 0.024(4) 0.002(3) 0.007(4) 0.000(3) C42 0.027(4) 0.020(4) 0.020(4) 0.005(3) -0.001(3) 0.001(3) C43 0.023(4) 0.017(4) 0.016(4) 0.009(3) 0.002(3) 0.003(3) C44 0.018(4) 0.031(4) 0.022(4) -0.006(3) -0.001(3) 0.003(3) C45 0.027(4) 0.047(5) 0.026(5) -0.015(4) 0.010(4) 0.000(4) C46 0.018(4) 0.054(6) 0.040(5) 0.005(5) 0.008(4) -0.003(4) C47 0.029(5) 0.057(6) 0.036(5) -0.011(5) -0.001(4) -0.014(4) C48 0.026(4) 0.034(4) 0.029(5) -0.008(4) 0.010(4) -0.004(4) C49 0.027(4) 0.011(3) 0.010(4) -0.004(3) 0.003(3) 0.001(3) C50 0.031(4) 0.019(4) 0.020(4) -0.002(3) 0.004(3) 0.002(3) C51 0.036(5) 0.023(4) 0.018(4) -0.001(3) 0.000(3) -0.007(4) C52 0.048(5) 0.022(4) 0.021(4) -0.003(3) 0.012(4) -0.017(4) C53 0.031(4) 0.023(4) 0.033(5) -0.003(4) 0.012(4) -0.007(4) C54 0.030(4) 0.019(4) 0.024(4) 0.000(3) 0.004(4) 0.000(3) Cl4 0.0350(12) 0.0649(15) 0.0286(12) -0.0012(11) 0.0055(10) 0.0028(11) Cl5 0.0543(16) 0.0583(16) 0.0641(18) -0.0179(14) -0.0229(13) 0.0081(13) C55 0.042(5) 0.042(5) 0.039(5) 0.006(4) -0.007(4) 0.004(4) Cl6 0.072(2) 0.076(2) 0.089(2) 0.0216(18) 0.0189(17) 0.0192(16) Cl7 0.089(2) 0.114(3) 0.092(3) 0.013(2) 0.031(2) 0.037(2) C56 0.217(18) 0.069(9) 0.136(14) 0.034(9) 0.096(14) 0.067(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.2588(19) . ? Pd1 P1 2.2752(18) . ? Pd1 S2 2.3389(17) . ? Pd1 S1 2.3460(18) . ? Pd2 P3 2.2231(18) . ? Pd2 S3 2.2755(18) . ? Pd2 Cl1 2.3350(18) . ? Pd2 S1 2.3710(17) . ? Pd3 S2 2.2815(18) . ? Pd3 S3 2.3074(18) . ? Pd3 Cl3 2.3271(19) . ? Pd3 Cl2 2.3280(18) . ? S1 C2 1.786(6) . ? S2 C20 1.781(7) . ? S3 C38 1.788(6) . ? P1 C7 1.805(7) . ? P1 C1 1.810(7) . ? P1 C13 1.815(7) . ? P2 C31 1.800(7) . ? P2 C25 1.807(7) . ? P2 C19 1.813(7) . ? P3 C43 1.808(7) . ? P3 C37 1.813(7) . ? P3 C49 1.822(7) . ? C1 C6 1.385(9) . ? C1 C2 1.393(9) . ? C2 C3 1.376(9) . ? C3 C4 1.385(9) . ? C4 C5 1.376(9) . ? C5 C6 1.392(10) . ? C7 C12 1.385(9) . ? C7 C8 1.402(10) . ? C8 C9 1.366(10) . ? C9 C10 1.387(10) . ? C10 C11 1.369(10) . ? C11 C12 1.383(10) . ? C13 C18 1.382(9) . ? C13 C14 1.392(10) . ? C14 C15 1.372(10) . ? C15 C16 1.377(11) . ? C16 C17 1.373(10) . ? C17 C18 1.393(10) . ? C19 C20 1.377(9) . ? C19 C24 1.392(10) . ? C20 C21 1.398(10) . ? C21 C22 1.370(10) . ? C22 C23 1.381(11) . ? C23 C24 1.377(10) . ? C25 C30 1.385(10) . ? C25 C26 1.393(10) . ? C26 C27 1.364(10) . ? C27 C28 1.395(11) . ? C28 C29 1.356(11) . ? C29 C30 1.385(11) . ? C31 C32 1.381(10) . ? C31 C36 1.400(10) . ? C32 C33 1.403(10) . ? C33 C34 1.367(11) . ? C34 C35 1.385(11) . ? C35 C36 1.380(11) . ? C37 C38 1.385(9) . ? C37 C42 1.398(9) . ? C38 C39 1.377(9) . ? C39 C40 1.382(9) . ? C40 C41 1.379(10) . ? C41 C42 1.382(10) . ? C43 C44 1.373(9) . ? C43 C48 1.389(10) . ? C44 C45 1.389(10) . ? C45 C46 1.377(11) . ? C46 C47 1.370(11) . ? C47 C48 1.366(10) . ? C49 C50 1.372(9) . ? C49 C54 1.392(10) . ? C50 C51 1.384(10) . ? C51 C52 1.373(10) . ? C52 C53 1.372(10) . ? C53 C54 1.385(10) . ? Cl4 C55 1.756(8) . ? Cl5 C55 1.733(9) . ? Cl6 C56 1.683(13) . ? Cl7 C56 1.770(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 P2 Pd1 P1 98.37(7) . . ? P2 Pd1 S2 85.58(6) . . ? P1 Pd1 S2 175.83(7) . . ? P2 Pd1 S1 174.96(7) . . ? P1 Pd1 S1 84.05(6) . . ? S2 Pd1 S1 92.12(6) . . ? P3 Pd2 S3 87.70(6) . . ? P3 Pd2 Cl1 92.52(7) . . ? S3 Pd2 Cl1 176.03(7) . . ? P3 Pd2 S1 173.48(7) . . ? S3 Pd2 S1 86.11(6) . . ? Cl1 Pd2 S1 93.80(6) . . ? S2 Pd3 S3 89.04(6) . . ? S2 Pd3 Cl3 171.78(7) . . ? S3 Pd3 Cl3 88.68(7) . . ? S2 Pd3 Cl2 91.24(7) . . ? S3 Pd3 Cl2 166.07(7) . . ? Cl3 Pd3 Cl2 92.87(7) . . ? C2 S1 Pd1 104.6(2) . . ? C2 S1 Pd2 104.8(2) . . ? Pd1 S1 Pd2 92.81(6) . . ? C20 S2 Pd3 109.2(2) . . ? C20 S2 Pd1 104.6(2) . . ? Pd3 S2 Pd1 102.80(7) . . ? C38 S3 Pd2 105.0(2) . . ? C38 S3 Pd3 111.6(2) . . ? Pd2 S3 Pd3 107.46(7) . . ? C7 P1 C1 104.7(3) . . ? C7 P1 C13 109.1(3) . . ? C1 P1 C13 103.0(3) . . ? C7 P1 Pd1 111.3(2) . . ? C1 P1 Pd1 106.7(2) . . ? C13 P1 Pd1 120.5(2) . . ? C31 P2 C25 110.0(3) . . ? C31 P2 C19 104.6(3) . . ? C25 P2 C19 104.8(3) . . ? C31 P2 Pd1 114.8(2) . . ? C25 P2 Pd1 114.4(2) . . ? C19 P2 Pd1 107.2(2) . . ? C43 P3 C37 108.5(3) . . ? C43 P3 C49 106.0(3) . . ? C37 P3 C49 105.8(3) . . ? C43 P3 Pd2 113.5(2) . . ? C37 P3 Pd2 107.3(2) . . ? C49 P3 Pd2 115.4(2) . . ? C6 C1 C2 119.7(6) . . ? C6 C1 P1 123.8(5) . . ? C2 C1 P1 116.5(5) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 S1 119.8(5) . . ? C1 C2 S1 120.0(5) . . ? C2 C3 C4 120.1(7) . . ? C5 C4 C3 120.1(7) . . ? C4 C5 C6 120.3(7) . . ? C1 C6 C5 119.7(7) . . ? C12 C7 C8 118.7(6) . . ? C12 C7 P1 122.2(5) . . ? C8 C7 P1 118.9(5) . . ? C9 C8 C7 120.6(7) . . ? C8 C9 C10 119.8(7) . . ? C11 C10 C9 120.5(7) . . ? C10 C11 C12 119.9(7) . . ? C11 C12 C7 120.5(7) . . ? C18 C13 C14 119.3(7) . . ? C18 C13 P1 123.4(5) . . ? C14 C13 P1 117.4(5) . . ? C15 C14 C13 119.8(7) . . ? C14 C15 C16 120.6(8) . . ? C17 C16 C15 120.7(7) . . ? C16 C17 C18 118.9(7) . . ? C13 C18 C17 120.8(7) . . ? C20 C19 C24 119.6(6) . . ? C20 C19 P2 117.8(5) . . ? C24 C19 P2 122.6(6) . . ? C19 C20 C21 119.9(7) . . ? C19 C20 S2 120.3(5) . . ? C21 C20 S2 119.8(5) . . ? C22 C21 C20 119.8(7) . . ? C21 C22 C23 120.6(7) . . ? C24 C23 C22 119.8(7) . . ? C23 C24 C19 120.3(7) . . ? C30 C25 C26 118.2(7) . . ? C30 C25 P2 117.7(6) . . ? C26 C25 P2 123.5(6) . . ? C27 C26 C25 121.2(7) . . ? C26 C27 C28 119.8(8) . . ? C29 C28 C27 119.5(8) . . ? C28 C29 C30 121.0(8) . . ? C29 C30 C25 120.2(8) . . ? C32 C31 C36 119.4(7) . . ? C32 C31 P2 122.7(6) . . ? C36 C31 P2 117.7(6) . . ? C31 C32 C33 119.9(7) . . ? C34 C33 C32 120.2(8) . . ? C33 C34 C35 120.2(8) . . ? C36 C35 C34 120.2(8) . . ? C35 C36 C31 120.1(8) . . ? C38 C37 C42 119.4(6) . . ? C38 C37 P3 117.4(5) . . ? C42 C37 P3 123.2(5) . . ? C39 C38 C37 120.5(6) . . ? C39 C38 S3 119.6(5) . . ? C37 C38 S3 119.5(5) . . ? C38 C39 C40 120.0(7) . . ? C41 C40 C39 119.8(7) . . ? C40 C41 C42 120.7(7) . . ? C41 C42 C37 119.4(6) . . ? C44 C43 C48 118.6(7) . . ? C44 C43 P3 123.2(5) . . ? C48 C43 P3 118.1(6) . . ? C43 C44 C45 120.8(7) . . ? C46 C45 C44 119.9(7) . . ? C47 C46 C45 119.0(7) . . ? C48 C47 C46 121.5(8) . . ? C47 C48 C43 120.1(7) . . ? C50 C49 C54 119.5(7) . . ? C50 C49 P3 122.4(6) . . ? C54 C49 P3 118.0(5) . . ? C49 C50 C51 119.7(7) . . ? C52 C51 C50 121.2(7) . . ? C53 C52 C51 119.2(7) . . ? C52 C53 C54 120.4(7) . . ? C53 C54 C49 119.9(7) . . ? Cl5 C55 Cl4 112.0(5) . . ? Cl6 C56 Cl7 114.2(7) . . ? # END of CIF #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-12-08 at 18:04:38 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : x1167fin x1167 data_x1167fin _database_code_depnum_ccdc_archive 'CCDC 856666' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2010-12-08T18:04:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C56 H46 Cl4 I3 P3 Pt3 S3' _chemical_formula_weight 2015.79 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 23.3381(4) _cell_length_b 11.44520(10) _cell_length_c 23.9386(4) _cell_angle_alpha 90 _cell_angle_beta 112.458(2) _cell_angle_gamma 90 _cell_volume 5909.28(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 27433 _cell_measurement_theta_min 2.8275 _cell_measurement_theta_max 32.4078 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2672 _exptl_crystal_size_mid 0.1098 _exptl_crystal_size_min 0.0859 _exptl_crystal_density_diffrn 2.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -31 0 2 0.0443 -6 16 0 0.0352 3 -16 5 0.0347 -17 -1 33 0.1204 20 1 -33 0.1177 30 0 0 0.045 2 -13 -20 0.0826 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.057 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.224 _exptl_absorpt_correction_T_max 0.572 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0305731 _diffrn_orient_matrix_ub_12 0.0119299 _diffrn_orient_matrix_ub_13 -0.0207051 _diffrn_orient_matrix_ub_21 -0.0056714 _diffrn_orient_matrix_ub_22 -0.0607946 _diffrn_orient_matrix_ub_23 -0.0047614 _diffrn_orient_matrix_ub_31 -0.010718 _diffrn_orient_matrix_ub_32 -0.0017998 _diffrn_orient_matrix_ub_33 0.024003 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_unetI/netI 0.039 _diffrn_reflns_number 72568 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 18027 _reflns_number_gt 15008 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ; SHELXS-97 Program for Crystal Structure Analysis (Release 97-2) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0164P)^2^+36.4813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 18027 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.21 _refine_diff_density_min -4.345 _refine_diff_density_rms 0.192 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.212702(9) 0.035396(15) 0.382479(8) 0.01611(4) Uani 1 1 d . . . Pt2 Pt 0.304295(8) 0.253225(15) 0.348294(8) 0.01538(4) Uani 1 1 d . . . Pt3 Pt 0.184633(8) 0.074096(15) 0.223887(7) 0.01345(4) Uani 1 1 d . . . I1 I 0.22286(3) -0.17393(3) 0.42784(2) 0.04743(13) Uani 1 1 d . . . I2 I 0.363042(16) 0.27296(3) 0.465527(15) 0.02666(7) Uani 1 1 d . . . I3 I 0.105676(15) 0.18902(3) 0.132660(14) 0.02313(7) Uani 1 1 d . . . S1 S 0.20471(5) 0.22720(10) 0.35143(5) 0.0156(2) Uani 1 1 d . . . S2 S 0.24844(5) 0.24451(10) 0.24708(5) 0.0152(2) Uani 1 1 d . . . S3 S 0.25283(5) -0.02111(10) 0.30659(5) 0.0154(2) Uani 1 1 d . . . P1 P 0.17324(6) 0.09468(10) 0.44899(5) 0.0163(2) Uani 1 1 d . . . P2 P 0.39021(6) 0.25998(11) 0.32810(6) 0.0196(2) Uani 1 1 d . . . P3 P 0.12985(6) -0.09142(10) 0.19889(5) 0.0158(2) Uani 1 1 d . . . C1 C 0.1795(2) 0.2512(4) 0.4535(2) 0.0169(9) Uani 1 1 d . . . C2 C 0.1956(2) 0.3085(4) 0.4107(2) 0.0176(9) Uani 1 1 d . . . C3 C 0.2003(3) 0.4296(4) 0.4118(2) 0.0248(11) Uani 1 1 d . . . H3 H 0.2104 0.469 0.3818 0.03 Uiso 1 1 calc R . . C4 C 0.1904(3) 0.4932(5) 0.4567(3) 0.0308(12) Uani 1 1 d . . . H4 H 0.1941 0.5759 0.4576 0.037 Uiso 1 1 calc R . . C5 C 0.1750(3) 0.4364(4) 0.5002(2) 0.0264(11) Uani 1 1 d . . . H5 H 0.1679 0.4801 0.5307 0.032 Uiso 1 1 calc R . . C6 C 0.1700(2) 0.3161(4) 0.4992(2) 0.0221(10) Uani 1 1 d . . . H6 H 0.1602 0.2771 0.5294 0.026 Uiso 1 1 calc R . . C7 C 0.2101(2) 0.0489(4) 0.5269(2) 0.0185(9) Uani 1 1 d . . . C8 C 0.2741(3) 0.0576(6) 0.5550(3) 0.0378(14) Uani 1 1 d . . . H8 H 0.2979 0.0832 0.5328 0.045 Uiso 1 1 calc R . . C9 C 0.3031(3) 0.0293(6) 0.6151(3) 0.0371(14) Uani 1 1 d . . . H9 H 0.3469 0.0361 0.6342 0.045 Uiso 1 1 calc R . . C10 C 0.2695(3) -0.0088(5) 0.6479(3) 0.0312(12) Uani 1 1 d . . . H10 H 0.29 -0.0314 0.689 0.037 Uiso 1 1 calc R . . C11 C 0.2069(3) -0.0137(6) 0.6211(3) 0.0404(15) Uani 1 1 d . . . H11 H 0.1833 -0.0362 0.6441 0.048 Uiso 1 1 calc R . . C12 C 0.1768(3) 0.0139(6) 0.5602(3) 0.0344(14) Uani 1 1 d . . . H12 H 0.1329 0.0084 0.5416 0.041 Uiso 1 1 calc R . . C13 C 0.0914(2) 0.0602(4) 0.4265(2) 0.0204(9) Uani 1 1 d . . . C14 C 0.0522(3) 0.1218(5) 0.4458(3) 0.0364(14) Uani 1 1 d . . . H14 H 0.067 0.1898 0.4698 0.044 Uiso 1 1 calc R . . C15 C -0.0088(3) 0.0870(6) 0.4312(3) 0.0411(15) Uani 1 1 d . . . H15 H -0.0349 0.1308 0.4456 0.049 Uiso 1 1 calc R . . C16 C -0.0312(3) -0.0086(5) 0.3968(3) 0.0342(13) Uani 1 1 d . . . H16 H -0.0725 -0.0336 0.3881 0.041 Uiso 1 1 calc R . . C17 C 0.0066(3) -0.0704(7) 0.3743(3) 0.0457(17) Uani 1 1 d . . . H17 H -0.0093 -0.1363 0.349 0.055 Uiso 1 1 calc R . . C18 C 0.0677(3) -0.0358(6) 0.3889(3) 0.0439(17) Uani 1 1 d . . . H18 H 0.0933 -0.0777 0.3732 0.053 Uiso 1 1 calc R . . C19 C 0.3665(2) 0.2250(4) 0.2484(2) 0.0214(10) Uani 1 1 d . . . C20 C 0.3034(2) 0.2128(4) 0.2143(2) 0.0195(9) Uani 1 1 d . . . C21 C 0.2825(3) 0.1829(5) 0.1530(2) 0.0270(11) Uani 1 1 d . . . H21 H 0.2393 0.1758 0.1298 0.032 Uiso 1 1 calc R . . C22 C 0.3248(3) 0.1637(6) 0.1266(3) 0.0373(14) Uani 1 1 d . . . H22 H 0.3107 0.1418 0.0853 0.045 Uiso 1 1 calc R . . C23 C 0.3876(3) 0.1762(6) 0.1599(3) 0.0387(15) Uani 1 1 d . . . H23 H 0.4163 0.1642 0.1411 0.046 Uiso 1 1 calc R . . C24 C 0.4086(3) 0.2059(5) 0.2201(3) 0.0321(13) Uani 1 1 d . . . H24 H 0.4519 0.2135 0.2428 0.039 Uiso 1 1 calc R . . C25 C 0.4517(3) 0.1585(5) 0.3670(2) 0.0270(11) Uani 1 1 d . . . C26 C 0.4387(3) 0.0564(5) 0.3914(3) 0.0335(13) Uani 1 1 d . . . H26 H 0.3979 0.0414 0.3891 0.04 Uiso 1 1 calc R . . C27 C 0.4859(3) -0.0237(6) 0.4193(3) 0.0436(16) Uani 1 1 d . . . H27 H 0.4774 -0.0938 0.4359 0.052 Uiso 1 1 calc R . . C28 C 0.5450(4) -0.0009(7) 0.4226(4) 0.057(2) Uani 1 1 d . . . H28 H 0.577 -0.0556 0.442 0.069 Uiso 1 1 calc R . . C29 C 0.5587(3) 0.0995(7) 0.3985(4) 0.0532(19) Uani 1 1 d . . . H29 H 0.5997 0.1132 0.4008 0.064 Uiso 1 1 calc R . . C30 C 0.5122(3) 0.1803(6) 0.3709(3) 0.0383(14) Uani 1 1 d . . . H30 H 0.5213 0.2503 0.3546 0.046 Uiso 1 1 calc R . . C31 C 0.4254(2) 0.4039(5) 0.3376(3) 0.0250(11) Uani 1 1 d . . . C32 C 0.4619(3) 0.4432(6) 0.3952(3) 0.0373(14) Uani 1 1 d . . . H32 H 0.4722 0.3922 0.4289 0.045 Uiso 1 1 calc R . . C33 C 0.4831(3) 0.5581(6) 0.4029(4) 0.0476(18) Uani 1 1 d . . . H33 H 0.5081 0.5856 0.4421 0.057 Uiso 1 1 calc R . . C34 C 0.4680(3) 0.6322(6) 0.3542(4) 0.0474(18) Uani 1 1 d . . . H34 H 0.4818 0.711 0.3602 0.057 Uiso 1 1 calc R . . C35 C 0.4333(3) 0.5935(5) 0.2973(4) 0.0465(18) Uani 1 1 d . . . H35 H 0.4238 0.6449 0.2638 0.056 Uiso 1 1 calc R . . C36 C 0.4121(3) 0.4788(5) 0.2884(3) 0.0327(13) Uani 1 1 d . . . H36 H 0.3885 0.4516 0.2488 0.039 Uiso 1 1 calc R . . C37 C 0.1794(2) -0.2068(4) 0.2442(2) 0.0189(9) Uani 1 1 d . . . C38 C 0.2355(2) -0.1726(4) 0.2892(2) 0.0164(9) Uani 1 1 d . . . C39 C 0.2794(2) -0.2557(4) 0.3210(2) 0.0226(10) Uani 1 1 d . . . H39 H 0.3181 -0.2321 0.3507 0.027 Uiso 1 1 calc R . . C40 C 0.2662(3) -0.3733(4) 0.3087(2) 0.0246(11) Uani 1 1 d . . . H40 H 0.2962 -0.4302 0.3301 0.03 Uiso 1 1 calc R . . C41 C 0.2102(3) -0.4089(4) 0.2660(2) 0.0261(11) Uani 1 1 d . . . H41 H 0.2011 -0.4898 0.2589 0.031 Uiso 1 1 calc R . . C42 C 0.1671(3) -0.3261(4) 0.2334(2) 0.0225(10) Uani 1 1 d . . . H42 H 0.1288 -0.3505 0.2035 0.027 Uiso 1 1 calc R . . C43 C 0.0568(2) -0.0934(5) 0.2089(2) 0.0236(10) Uani 1 1 d . . . C44 C 0.0190(3) -0.1929(5) 0.1935(3) 0.0336(13) Uani 1 1 d . . . H44 H 0.0325 -0.2611 0.1795 0.04 Uiso 1 1 calc R . . C45 C -0.0384(3) -0.1917(6) 0.1988(3) 0.0385(14) Uani 1 1 d . . . H45 H -0.0635 -0.26 0.1898 0.046 Uiso 1 1 calc R . . C46 C -0.0587(3) -0.0925(7) 0.2170(3) 0.0472(18) Uani 1 1 d . . . H46 H -0.0972 -0.093 0.2218 0.057 Uiso 1 1 calc R . . C47 C -0.0239(3) 0.0085(7) 0.2285(4) 0.055(2) Uani 1 1 d . . . H47 H -0.0395 0.0785 0.2387 0.066 Uiso 1 1 calc R . . C48 C 0.0344(3) 0.0072(6) 0.2249(3) 0.0386(15) Uani 1 1 d . . . H48 H 0.0589 0.0762 0.2336 0.046 Uiso 1 1 calc R . . C49 C 0.1108(2) -0.1371(4) 0.1212(2) 0.0194(9) Uani 1 1 d . . . C50 C 0.0537(3) -0.1103(5) 0.0769(2) 0.0285(12) Uani 1 1 d . . . H50 H 0.0229 -0.0727 0.0873 0.034 Uiso 1 1 calc R . . C51 C 0.0416(3) -0.1388(5) 0.0169(3) 0.0401(16) Uani 1 1 d . . . H51 H 0.0024 -0.121 -0.0135 0.048 Uiso 1 1 calc R . . C52 C 0.0863(4) -0.1927(5) 0.0013(3) 0.0433(17) Uani 1 1 d . . . H52 H 0.0777 -0.2118 -0.0398 0.052 Uiso 1 1 calc R . . C53 C 0.1435(3) -0.2188(5) 0.0453(3) 0.0351(14) Uani 1 1 d . . . H53 H 0.1743 -0.2562 0.0346 0.042 Uiso 1 1 calc R . . C54 C 0.1560(3) -0.1902(5) 0.1052(2) 0.0282(12) Uani 1 1 d . . . H54 H 0.1956 -0.2069 0.1354 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.33054(10) 0.8087(2) 0.18406(11) 0.0704(6) Uani 1 1 d . . . Cl2 Cl 0.45310(8) 0.90511(16) 0.24966(10) 0.0521(4) Uani 1 1 d . . . C55 C 0.3751(4) 0.9044(6) 0.2403(4) 0.056(2) Uani 1 1 d . . . H55A H 0.372 0.882 0.279 0.067 Uiso 1 1 calc R . . H55B H 0.3581 0.9844 0.2301 0.067 Uiso 1 1 calc R . . Cl3 Cl 0.40784(11) 0.7260(2) 0.47532(10) 0.0713(6) Uani 1 1 d . . . Cl4 Cl 0.35559(12) 0.6056(2) 0.55170(10) 0.0735(7) Uani 1 1 d . . . C56 C 0.3598(5) 0.6144(7) 0.4794(3) 0.067(3) Uani 1 1 d . . . H56A H 0.3754 0.5393 0.4702 0.081 Uiso 1 1 calc R . . H56B H 0.3177 0.6272 0.4484 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02317(9) 0.01358(8) 0.01396(8) 0.00097(6) 0.00976(7) 0.00069(7) Pt2 0.01536(8) 0.01573(8) 0.01466(8) 0.00123(6) 0.00530(6) -0.00199(6) Pt3 0.01390(8) 0.01437(8) 0.01250(8) 0.00110(6) 0.00551(6) 0.00018(6) I1 0.1012(4) 0.01846(17) 0.0471(2) 0.00936(15) 0.0557(3) 0.0115(2) I2 0.02627(17) 0.03237(18) 0.01666(15) 0.00027(12) 0.00295(13) -0.00506(14) I3 0.02240(16) 0.02115(15) 0.01983(15) 0.00449(11) 0.00137(12) 0.00239(12) S1 0.0183(5) 0.0152(5) 0.0150(5) 0.0008(4) 0.0085(4) -0.0009(4) S2 0.0150(5) 0.0163(5) 0.0153(5) 0.0016(4) 0.0070(4) -0.0007(4) S3 0.0167(5) 0.0165(5) 0.0134(5) 0.0011(4) 0.0062(4) 0.0009(4) P1 0.0227(6) 0.0149(5) 0.0138(5) 0.0005(4) 0.0098(5) -0.0010(5) P2 0.0139(5) 0.0205(6) 0.0236(6) 0.0023(5) 0.0062(5) -0.0014(5) P3 0.0172(6) 0.0153(5) 0.0152(5) -0.0004(4) 0.0065(5) -0.0013(4) C1 0.021(2) 0.014(2) 0.017(2) -0.0015(16) 0.0073(18) 0.0019(18) C2 0.020(2) 0.017(2) 0.018(2) 0.0002(16) 0.0099(19) 0.0010(18) C3 0.039(3) 0.019(2) 0.024(3) 0.0038(18) 0.021(2) -0.001(2) C4 0.046(4) 0.017(2) 0.035(3) -0.003(2) 0.021(3) -0.002(2) C5 0.039(3) 0.020(2) 0.027(3) -0.0018(19) 0.020(2) 0.003(2) C6 0.031(3) 0.020(2) 0.017(2) 0.0014(17) 0.012(2) -0.001(2) C7 0.030(3) 0.013(2) 0.016(2) 0.0021(15) 0.012(2) 0.0031(18) C8 0.029(3) 0.058(4) 0.028(3) 0.004(3) 0.013(3) -0.003(3) C9 0.029(3) 0.056(4) 0.024(3) 0.003(3) 0.008(2) 0.008(3) C10 0.038(3) 0.034(3) 0.022(3) 0.005(2) 0.012(2) 0.002(3) C11 0.041(4) 0.059(4) 0.024(3) 0.010(3) 0.015(3) -0.013(3) C12 0.027(3) 0.054(4) 0.024(3) 0.013(2) 0.012(2) -0.003(3) C13 0.025(2) 0.019(2) 0.019(2) 0.0029(17) 0.010(2) -0.0026(19) C14 0.031(3) 0.025(3) 0.054(4) -0.005(3) 0.016(3) -0.002(2) C15 0.028(3) 0.030(3) 0.070(5) -0.001(3) 0.025(3) 0.000(3) C16 0.025(3) 0.038(3) 0.038(3) 0.008(2) 0.011(3) -0.007(2) C17 0.040(4) 0.051(4) 0.050(4) -0.018(3) 0.021(3) -0.022(3) C18 0.045(4) 0.052(4) 0.045(4) -0.022(3) 0.030(3) -0.016(3) C19 0.020(2) 0.021(2) 0.025(3) 0.0020(18) 0.011(2) -0.0042(19) C20 0.021(2) 0.016(2) 0.024(2) 0.0031(17) 0.012(2) -0.0014(18) C21 0.026(3) 0.034(3) 0.024(3) -0.006(2) 0.013(2) -0.006(2) C22 0.039(3) 0.047(4) 0.037(3) -0.011(3) 0.026(3) -0.005(3) C23 0.034(3) 0.053(4) 0.041(4) -0.005(3) 0.029(3) -0.006(3) C24 0.019(3) 0.044(3) 0.038(3) 0.003(3) 0.016(2) -0.003(2) C25 0.025(3) 0.024(3) 0.027(3) 0.000(2) 0.005(2) 0.003(2) C26 0.038(3) 0.031(3) 0.031(3) 0.005(2) 0.012(3) 0.004(3) C27 0.052(4) 0.031(3) 0.045(4) 0.014(3) 0.016(3) 0.013(3) C28 0.050(5) 0.049(4) 0.064(5) 0.016(4) 0.011(4) 0.028(4) C29 0.030(3) 0.050(4) 0.073(5) 0.006(4) 0.011(4) 0.016(3) C30 0.025(3) 0.037(3) 0.050(4) 0.003(3) 0.012(3) 0.005(3) C31 0.012(2) 0.023(3) 0.041(3) -0.004(2) 0.011(2) 0.0001(19) C32 0.034(3) 0.035(3) 0.043(4) -0.008(3) 0.016(3) -0.013(3) C33 0.036(4) 0.045(4) 0.062(5) -0.023(3) 0.019(3) -0.022(3) C34 0.031(3) 0.026(3) 0.091(6) -0.007(3) 0.029(4) -0.010(3) C35 0.035(3) 0.023(3) 0.084(6) 0.014(3) 0.025(4) 0.003(3) C36 0.021(3) 0.026(3) 0.045(4) 0.010(2) 0.006(2) -0.001(2) C37 0.026(2) 0.012(2) 0.020(2) 0.0001(16) 0.011(2) 0.0035(18) C38 0.022(2) 0.018(2) 0.013(2) 0.0013(15) 0.0106(18) 0.0018(18) C39 0.026(3) 0.024(2) 0.019(2) 0.0032(18) 0.009(2) 0.007(2) C40 0.038(3) 0.020(2) 0.020(2) 0.0031(18) 0.015(2) 0.008(2) C41 0.040(3) 0.015(2) 0.027(3) -0.0023(18) 0.017(2) 0.003(2) C42 0.032(3) 0.018(2) 0.020(2) -0.0013(17) 0.013(2) 0.002(2) C43 0.023(2) 0.025(3) 0.024(3) -0.0034(19) 0.011(2) -0.003(2) C44 0.022(3) 0.029(3) 0.051(4) 0.001(2) 0.015(3) 0.000(2) C45 0.028(3) 0.036(3) 0.049(4) -0.001(3) 0.013(3) -0.007(3) C46 0.031(3) 0.061(5) 0.059(5) -0.022(4) 0.028(3) -0.017(3) C47 0.043(4) 0.053(5) 0.085(6) -0.026(4) 0.042(4) -0.006(3) C48 0.033(3) 0.036(3) 0.056(4) -0.017(3) 0.027(3) -0.008(3) C49 0.025(2) 0.018(2) 0.016(2) 0.0004(16) 0.0088(19) -0.0046(19) C50 0.037(3) 0.020(2) 0.023(3) -0.0008(19) 0.006(2) -0.008(2) C51 0.056(4) 0.030(3) 0.018(3) 0.002(2) -0.004(3) -0.007(3) C52 0.082(5) 0.027(3) 0.020(3) -0.003(2) 0.019(3) -0.017(3) C53 0.062(4) 0.027(3) 0.024(3) -0.007(2) 0.026(3) -0.013(3) C54 0.038(3) 0.032(3) 0.020(3) -0.004(2) 0.016(2) -0.006(2) Cl1 0.0462(11) 0.0894(17) 0.0632(14) -0.0008(11) 0.0071(10) -0.0062(11) Cl2 0.0411(9) 0.0383(9) 0.0814(14) -0.0024(8) 0.0285(9) 0.0017(7) C55 0.053(4) 0.037(4) 0.093(6) -0.007(4) 0.045(5) 0.000(3) Cl3 0.0580(13) 0.1073(19) 0.0467(12) 0.0053(11) 0.0180(10) -0.0015(13) Cl4 0.0786(15) 0.0780(15) 0.0533(12) 0.0133(10) 0.0132(11) -0.0245(13) C56 0.096(7) 0.041(4) 0.040(4) -0.002(3) -0.003(4) 0.009(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2279(11) . ? Pt1 S1 2.3022(11) . ? Pt1 S3 2.4280(11) . ? Pt1 I1 2.6036(4) . ? Pt2 P2 2.2363(12) . ? Pt2 S2 2.2730(11) . ? Pt2 S1 2.3726(11) . ? Pt2 I2 2.6205(4) . ? Pt3 P3 2.2354(12) . ? Pt3 S3 2.2876(11) . ? Pt3 S2 2.3872(11) . ? Pt3 I3 2.6116(4) . ? S1 C2 1.775(5) . ? S2 C20 1.779(5) . ? S3 C38 1.793(5) . ? P1 C1 1.797(5) . ? P1 C7 1.807(5) . ? P1 C13 1.819(5) . ? P2 C25 1.804(6) . ? P2 C19 1.816(5) . ? P2 C31 1.816(5) . ? P3 C43 1.811(5) . ? P3 C49 1.816(5) . ? P3 C37 1.817(5) . ? C1 C2 1.385(6) . ? C1 C6 1.407(6) . ? C2 C3 1.391(7) . ? C3 C4 1.390(7) . ? C4 C5 1.386(7) . ? C5 C6 1.380(7) . ? C7 C12 1.370(7) . ? C7 C8 1.388(8) . ? C8 C9 1.374(8) . ? C9 C10 1.376(8) . ? C10 C11 1.353(9) . ? C11 C12 1.392(8) . ? C13 C14 1.369(8) . ? C13 C18 1.394(8) . ? C14 C15 1.387(8) . ? C15 C16 1.349(9) . ? C16 C17 1.389(9) . ? C17 C18 1.390(9) . ? C19 C20 1.390(7) . ? C19 C24 1.409(7) . ? C20 C21 1.399(7) . ? C21 C22 1.379(7) . ? C22 C23 1.383(9) . ? C23 C24 1.377(9) . ? C25 C26 1.391(8) . ? C25 C30 1.402(8) . ? C26 C27 1.391(8) . ? C27 C28 1.375(11) . ? C28 C29 1.377(11) . ? C29 C30 1.387(9) . ? C31 C32 1.390(8) . ? C31 C36 1.391(8) . ? C32 C33 1.393(9) . ? C33 C34 1.374(11) . ? C34 C35 1.366(11) . ? C35 C36 1.390(8) . ? C37 C38 1.396(7) . ? C37 C42 1.399(7) . ? C38 C39 1.392(7) . ? C39 C40 1.387(7) . ? C40 C41 1.379(8) . ? C41 C42 1.385(7) . ? C43 C48 1.378(8) . ? C43 C44 1.400(8) . ? C44 C45 1.394(8) . ? C45 C46 1.363(9) . ? C46 C47 1.379(10) . ? C47 C48 1.395(9) . ? C49 C50 1.383(7) . ? C49 C54 1.394(7) . ? C50 C51 1.393(8) . ? C51 C52 1.380(10) . ? C52 C53 1.381(10) . ? C53 C54 1.389(7) . ? Cl1 C55 1.739(8) . ? Cl2 C55 1.747(7) . ? Cl3 C56 1.727(10) . ? Cl4 C56 1.775(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 P1 Pt1 S1 86.31(4) . . ? P1 Pt1 S3 177.06(4) . . ? S1 Pt1 S3 91.10(4) . . ? P1 Pt1 I1 88.78(3) . . ? S1 Pt1 I1 174.45(3) . . ? S3 Pt1 I1 93.86(3) . . ? P2 Pt2 S2 88.14(4) . . ? P2 Pt2 S1 168.89(4) . . ? S2 Pt2 S1 81.86(4) . . ? P2 Pt2 I2 94.76(4) . . ? S2 Pt2 I2 176.14(3) . . ? S1 Pt2 I2 95.45(3) . . ? P3 Pt3 S3 88.04(4) . . ? P3 Pt3 S2 175.47(4) . . ? S3 Pt3 S2 91.25(4) . . ? P3 Pt3 I3 93.11(3) . . ? S3 Pt3 I3 177.49(3) . . ? S2 Pt3 I3 87.78(3) . . ? C2 S1 Pt1 105.16(16) . . ? C2 S1 Pt2 112.17(16) . . ? Pt1 S1 Pt2 99.81(4) . . ? C20 S2 Pt2 105.23(17) . . ? C20 S2 Pt3 102.81(16) . . ? Pt2 S2 Pt3 109.67(4) . . ? C38 S3 Pt3 103.83(16) . . ? C38 S3 Pt1 108.31(14) . . ? Pt3 S3 Pt1 100.43(4) . . ? C1 P1 C7 103.4(2) . . ? C1 P1 C13 106.6(2) . . ? C7 P1 C13 106.0(2) . . ? C1 P1 Pt1 107.49(15) . . ? C7 P1 Pt1 118.99(16) . . ? C13 P1 Pt1 113.36(16) . . ? C25 P2 C19 105.3(2) . . ? C25 P2 C31 106.7(2) . . ? C19 P2 C31 105.9(2) . . ? C25 P2 Pt2 117.91(19) . . ? C19 P2 Pt2 106.27(16) . . ? C31 P2 Pt2 113.85(17) . . ? C43 P3 C49 104.9(2) . . ? C43 P3 C37 109.2(2) . . ? C49 P3 C37 104.7(2) . . ? C43 P3 Pt3 116.53(17) . . ? C49 P3 Pt3 114.18(16) . . ? C37 P3 Pt3 106.71(17) . . ? C2 C1 C6 119.5(4) . . ? C2 C1 P1 117.8(3) . . ? C6 C1 P1 122.7(4) . . ? C1 C2 C3 120.0(4) . . ? C1 C2 S1 119.5(4) . . ? C3 C2 S1 120.4(4) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 120.2(5) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 C1 120.3(4) . . ? C12 C7 C8 118.9(5) . . ? C12 C7 P1 122.2(4) . . ? C8 C7 P1 118.7(4) . . ? C9 C8 C7 120.0(5) . . ? C8 C9 C10 120.8(6) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C12 120.6(5) . . ? C7 C12 C11 120.3(5) . . ? C14 C13 C18 118.2(5) . . ? C14 C13 P1 123.4(4) . . ? C18 C13 P1 118.4(4) . . ? C13 C14 C15 121.4(6) . . ? C16 C15 C14 120.5(6) . . ? C15 C16 C17 119.6(6) . . ? C16 C17 C18 120.0(6) . . ? C17 C18 C13 120.2(6) . . ? C20 C19 C24 118.5(5) . . ? C20 C19 P2 118.0(4) . . ? C24 C19 P2 123.4(4) . . ? C19 C20 C21 120.6(5) . . ? C19 C20 S2 120.0(4) . . ? C21 C20 S2 119.3(4) . . ? C22 C21 C20 119.6(5) . . ? C21 C22 C23 120.5(6) . . ? C24 C23 C22 120.3(5) . . ? C23 C24 C19 120.5(5) . . ? C26 C25 C30 119.8(5) . . ? C26 C25 P2 120.0(4) . . ? C30 C25 P2 120.1(4) . . ? C25 C26 C27 119.7(6) . . ? C28 C27 C26 119.6(6) . . ? C27 C28 C29 121.5(6) . . ? C28 C29 C30 119.4(7) . . ? C29 C30 C25 119.8(6) . . ? C32 C31 C36 119.6(5) . . ? C32 C31 P2 119.6(4) . . ? C36 C31 P2 120.6(4) . . ? C31 C32 C33 119.3(6) . . ? C34 C33 C32 120.5(7) . . ? C35 C34 C33 120.6(6) . . ? C34 C35 C36 119.9(7) . . ? C35 C36 C31 120.1(6) . . ? C38 C37 C42 118.8(4) . . ? C38 C37 P3 116.9(3) . . ? C42 C37 P3 124.1(4) . . ? C39 C38 C37 120.5(4) . . ? C39 C38 S3 118.7(4) . . ? C37 C38 S3 120.8(4) . . ? C40 C39 C38 119.4(5) . . ? C41 C40 C39 121.0(5) . . ? C40 C41 C42 119.6(5) . . ? C41 C42 C37 120.7(5) . . ? C48 C43 C44 119.1(5) . . ? C48 C43 P3 120.1(4) . . ? C44 C43 P3 120.4(4) . . ? C45 C44 C43 119.9(6) . . ? C46 C45 C44 120.0(6) . . ? C45 C46 C47 120.8(6) . . ? C46 C47 C48 119.5(6) . . ? C43 C48 C47 120.5(6) . . ? C50 C49 C54 119.7(5) . . ? C50 C49 P3 120.6(4) . . ? C54 C49 P3 119.5(4) . . ? C49 C50 C51 119.6(6) . . ? C52 C51 C50 120.6(6) . . ? C51 C52 C53 120.0(5) . . ? C52 C53 C54 119.8(6) . . ? C53 C54 C49 120.3(6) . . ? Cl1 C55 Cl2 112.8(4) . . ? Cl3 C56 Cl4 112.1(4) . . ? # END of CIF #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-04 at 12:34:57 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\xray\wingx\files\archive.reqdat # CIF files read : x1271fin x1271 data_x1271fin _database_code_depnum_ccdc_archive 'CCDC 856667' #TrackingRef 'ccdc_sub.cif' _audit_creation_date 2011-05-04T12:34:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C56.50 H44.50 Cl7.50 I3 P3 Pt3 S3' _chemical_formula_weight 2144.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 14.2175(2) _cell_length_b 23.0616(3) _cell_length_c 20.2971(3) _cell_angle_alpha 90 _cell_angle_beta 105.7540(10) _cell_angle_gamma 90 _cell_volume 6404.99(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 34831 _cell_measurement_theta_min 2.8227 _cell_measurement_theta_max 32.4249 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3988 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.42221 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0397575 _diffrn_orient_matrix_ub_12 -0.0197495 _diffrn_orient_matrix_ub_13 -0.0081032 _diffrn_orient_matrix_ub_21 0.0093392 _diffrn_orient_matrix_ub_22 -0.0073342 _diffrn_orient_matrix_ub_23 0.0351185 _diffrn_orient_matrix_ub_31 -0.0318972 _diffrn_orient_matrix_ub_32 0.0224302 _diffrn_orient_matrix_ub_33 0.0043616 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_number 85269 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 19523 _reflns_number_gt 16550 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ; SIR92 A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838. ; #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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 solvent molecules (CHCl3) are found to be disordered. 61 restraints are used to model these molecules. ; _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^)+(0.0123P)^2^+12.6118P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 19523 _refine_ls_number_parameters 724 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.037 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.769 _refine_diff_density_min -1.728 _refine_diff_density_rms 0.157 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.180288(9) 0.781071(5) 0.415555(6) 0.01180(3) Uani 1 1 d . . . Pt2 Pt 0.043525(9) 0.739953(5) 0.403917(6) 0.01248(3) Uani 1 1 d . . . Pt3 Pt -0.151434(9) 0.625779(5) 0.386921(6) 0.01249(3) Uani 1 1 d . . . I1 I 0.090839(16) 0.849339(9) 0.424601(12) 0.01885(5) Uani 1 1 d . . . I2 I -0.336505(16) 0.609300(11) 0.376903(12) 0.02246(5) Uani 1 1 d . . . I3 I -0.160143(18) 0.550030(10) 0.289783(12) 0.02209(5) Uani 1 1 d . . . S1 S -0.11239(6) 0.75572(3) 0.32572(4) 0.01322(15) Uani 1 1 d . . . S2 S -0.12756(6) 0.69330(3) 0.47378(4) 0.01388(15) Uani 1 1 d . . . S3 S 0.00743(6) 0.64382(3) 0.38449(4) 0.01399(15) Uani 1 1 d . . . P1 P -0.23731(6) 0.85893(4) 0.34942(4) 0.01345(16) Uani 1 1 d . . . P2 P -0.23533(6) 0.80180(4) 0.50702(4) 0.01505(16) Uani 1 1 d . . . P3 P 0.18428(6) 0.71154(4) 0.47497(4) 0.01470(16) Uani 1 1 d . . . C1 C -0.1560(2) 0.87072(15) 0.29585(17) 0.0154(6) Uani 1 1 d . . . C2 C -0.1071(2) 0.82201(14) 0.28212(17) 0.0154(6) Uani 1 1 d . . . C3 C -0.0532(2) 0.82474(15) 0.23394(17) 0.0183(7) Uani 1 1 d . . . H3 H -0.0218 0.7911 0.2231 0.022 Uiso 1 1 calc R . . C4 C -0.0461(3) 0.87702(17) 0.20223(19) 0.0233(8) Uani 1 1 d . . . H4 H -0.0097 0.8791 0.1694 0.028 Uiso 1 1 calc R . . C5 C -0.0915(3) 0.92647(16) 0.21782(19) 0.0219(7) Uani 1 1 d . . . H5 H -0.0843 0.9624 0.1968 0.026 Uiso 1 1 calc R . . C6 C -0.1474(2) 0.92342(15) 0.26407(18) 0.0190(7) Uani 1 1 d . . . H6 H -0.1798 0.957 0.2741 0.023 Uiso 1 1 calc R . . C7 C -0.3520(2) 0.84176(15) 0.28689(18) 0.0182(7) Uani 1 1 d . . . C8 C -0.3961(3) 0.78804(17) 0.2898(2) 0.0243(8) Uani 1 1 d . . . H8 H -0.3699 0.7625 0.3269 0.029 Uiso 1 1 calc R . . C9 C -0.4782(3) 0.7720(2) 0.2383(2) 0.0355(10) Uani 1 1 d . . . H9 H -0.5078 0.7354 0.2401 0.043 Uiso 1 1 calc R . . C10 C -0.5168(3) 0.8092(2) 0.1845(2) 0.0414(12) Uani 1 1 d . . . H10 H -0.5736 0.7985 0.1497 0.05 Uiso 1 1 calc R . . C11 C -0.4726(3) 0.8620(2) 0.1814(2) 0.0391(11) Uani 1 1 d . . . H11 H -0.499 0.8874 0.1442 0.047 Uiso 1 1 calc R . . C12 C -0.3905(3) 0.87821(17) 0.2317(2) 0.0282(9) Uani 1 1 d . . . H12 H -0.3602 0.9144 0.2286 0.034 Uiso 1 1 calc R . . C13 C -0.2485(3) 0.92872(14) 0.38644(17) 0.0169(7) Uani 1 1 d . . . C14 C -0.1633(3) 0.95336(17) 0.4287(2) 0.0256(8) Uani 1 1 d . . . H14 H -0.1031 0.9331 0.4376 0.031 Uiso 1 1 calc R . . C15 C -0.1673(3) 1.00739(18) 0.4575(2) 0.0321(9) Uani 1 1 d . . . H15 H -0.1097 1.0238 0.4867 0.038 Uiso 1 1 calc R . . C16 C -0.2539(3) 1.03753(18) 0.4441(2) 0.0328(10) Uani 1 1 d . . . H16 H -0.2558 1.075 0.4632 0.039 Uiso 1 1 calc R . . C17 C -0.3382(3) 1.01311(18) 0.4028(2) 0.0315(9) Uani 1 1 d . . . H17 H -0.3981 1.0339 0.3937 0.038 Uiso 1 1 calc R . . C18 C -0.3361(3) 0.95837(16) 0.3744(2) 0.0251(8) Uani 1 1 d . . . H18 H -0.3945 0.9414 0.347 0.03 Uiso 1 1 calc R . . C19 C -0.2576(3) 0.73255(15) 0.54261(17) 0.0173(7) Uani 1 1 d . . . C20 C -0.2092(2) 0.68443(15) 0.52621(17) 0.0169(7) Uani 1 1 d . . . C21 C -0.2163(3) 0.63095(16) 0.55626(18) 0.0221(7) Uani 1 1 d . . . H21 H -0.1832 0.5981 0.5452 0.026 Uiso 1 1 calc R . . C22 C -0.2720(3) 0.62581(18) 0.6024(2) 0.0284(9) Uani 1 1 d . . . H22 H -0.2768 0.5894 0.6232 0.034 Uiso 1 1 calc R . . C23 C -0.3205(3) 0.67331(19) 0.6183(2) 0.0324(9) Uani 1 1 d . . . H23 H -0.3585 0.6693 0.6499 0.039 Uiso 1 1 calc R . . C24 C -0.3143(3) 0.72668(18) 0.5887(2) 0.0273(8) Uani 1 1 d . . . H24 H -0.3484 0.7591 0.5996 0.033 Uiso 1 1 calc R . . C25 C -0.1456(2) 0.83786(15) 0.57474(17) 0.0177(7) Uani 1 1 d . . . C26 C -0.1636(3) 0.85058(18) 0.63758(19) 0.0268(8) Uani 1 1 d . . . H26 H -0.2247 0.8406 0.6451 0.032 Uiso 1 1 calc R . . C27 C -0.0931(4) 0.87761(19) 0.6889(2) 0.0359(10) Uani 1 1 d . . . H27 H -0.106 0.8861 0.7314 0.043 Uiso 1 1 calc R . . C28 C -0.0036(4) 0.89247(19) 0.6788(2) 0.0380(11) Uani 1 1 d . . . H28 H 0.044 0.912 0.7137 0.046 Uiso 1 1 calc R . . C29 C 0.0157(3) 0.8787(2) 0.6180(2) 0.0369(10) Uani 1 1 d . . . H29 H 0.0779 0.8875 0.6116 0.044 Uiso 1 1 calc R . . C30 C -0.0546(3) 0.85205(17) 0.5657(2) 0.0262(8) Uani 1 1 d . . . H30 H -0.0407 0.8435 0.5235 0.031 Uiso 1 1 calc R . . C31 C -0.3488(2) 0.84134(15) 0.49496(18) 0.0176(7) Uani 1 1 d . . . C32 C -0.3527(3) 0.89651(17) 0.5213(2) 0.0276(8) Uani 1 1 d . . . H32 H -0.2944 0.9151 0.5466 0.033 Uiso 1 1 calc R . . C33 C -0.4422(3) 0.9243(2) 0.5106(2) 0.0394(11) Uani 1 1 d . . . H33 H -0.4452 0.9618 0.5294 0.047 Uiso 1 1 calc R . . C34 C -0.5267(3) 0.8980(2) 0.4727(2) 0.0374(11) Uani 1 1 d . . . H34 H -0.5877 0.9173 0.4656 0.045 Uiso 1 1 calc R . . C35 C -0.5225(3) 0.8441(2) 0.4454(2) 0.0360(10) Uani 1 1 d . . . H35 H -0.5807 0.8263 0.4185 0.043 Uiso 1 1 calc R . . C36 C -0.4344(3) 0.81528(19) 0.4565(2) 0.0288(9) Uani 1 1 d . . . H36 H -0.4322 0.7777 0.4379 0.035 Uiso 1 1 calc R . . C37 C 0.1649(2) 0.63797(15) 0.49950(18) 0.0174(7) Uani 1 1 d . . . C38 C 0.0870(2) 0.60802(14) 0.45639(18) 0.0162(6) Uani 1 1 d . . . C39 C 0.0746(3) 0.54902(16) 0.4659(2) 0.0222(8) Uani 1 1 d . . . H39 H 0.0235 0.5281 0.4352 0.027 Uiso 1 1 calc R . . C40 C 0.1379(3) 0.52119(16) 0.5208(2) 0.0252(8) Uani 1 1 d . . . H40 H 0.1303 0.4809 0.5274 0.03 Uiso 1 1 calc R . . C41 C 0.2120(3) 0.55133(17) 0.5661(2) 0.0262(8) Uani 1 1 d . . . H41 H 0.2531 0.5321 0.6047 0.031 Uiso 1 1 calc R . . C42 C 0.2264(3) 0.60929(16) 0.5553(2) 0.0236(8) Uani 1 1 d . . . H42 H 0.2782 0.6297 0.5859 0.028 Uiso 1 1 calc R . . C43 C 0.2807(2) 0.70625(15) 0.43221(19) 0.0193(7) Uani 1 1 d . . . C44 C 0.3669(3) 0.67663(19) 0.4623(2) 0.0305(9) Uani 1 1 d . . . H44 H 0.3768 0.6604 0.5067 0.037 Uiso 1 1 calc R . . C45 C 0.4380(3) 0.67076(19) 0.4283(2) 0.0345(10) Uani 1 1 d . . . H45 H 0.4967 0.6506 0.4494 0.041 Uiso 1 1 calc R . . C46 C 0.4243(3) 0.69386(19) 0.3642(2) 0.0327(9) Uani 1 1 d . . . H46 H 0.4732 0.6891 0.3407 0.039 Uiso 1 1 calc R . . C47 C 0.3398(3) 0.7241(2) 0.3336(2) 0.0344(10) Uani 1 1 d . . . H47 H 0.3308 0.7405 0.2894 0.041 Uiso 1 1 calc R . . C48 C 0.2682(3) 0.73040(17) 0.3681(2) 0.0258(8) Uani 1 1 d . . . H48 H 0.2103 0.7514 0.3474 0.031 Uiso 1 1 calc R . . C49 C 0.2360(3) 0.75048(16) 0.55308(18) 0.0228(8) Uani 1 1 d . . . C50 C 0.3206(3) 0.78365(19) 0.5614(2) 0.0353(10) Uani 1 1 d . . . H50 H 0.3536 0.784 0.5265 0.042 Uiso 1 1 calc R . . C51 C 0.3563(5) 0.8158(2) 0.6200(3) 0.0554(16) Uani 1 1 d . . . H51 H 0.4141 0.8381 0.6258 0.066 Uiso 1 1 calc R . . C52 C 0.3085(5) 0.8155(2) 0.6696(3) 0.0577(17) Uani 1 1 d . . . H52 H 0.3336 0.8377 0.71 0.069 Uiso 1 1 calc R . . C53 C 0.2256(5) 0.7841(2) 0.6625(2) 0.0547(15) Uani 1 1 d . . . H53 H 0.1931 0.7847 0.6977 0.066 Uiso 1 1 calc R . . C54 C 0.1878(4) 0.7507(2) 0.6035(2) 0.0361(10) Uani 1 1 d . . . H54 H 0.1298 0.7287 0.5983 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.26059(11) 0.88302(6) 0.29660(7) 0.0531(3) Uani 1 1 d D . . Cl2 Cl 0.22486(10) 0.98000(5) 0.37636(6) 0.0461(3) Uani 1 1 d D . . Cl3 Cl 0.14661(8) 0.98022(5) 0.22928(5) 0.0359(2) Uani 1 1 d D . . C55 C 0.1776(3) 0.93724(17) 0.3034(2) 0.0304(9) Uani 1 1 d D . . H55 H 0.1168 0.918 0.3082 0.036 Uiso 1 1 calc R . . Cl4 Cl 0.0910(3) 0.5801(2) 0.1764(2) 0.0863(11) Uani 0.563(4) 1 d PD A 1 Cl5 Cl 0.2017(3) 0.59496(18) 0.3137(2) 0.0549(10) Uani 0.563(4) 1 d PD A 1 Cl6 Cl 0.0935(9) 0.4867(4) 0.2724(5) 0.079(2) Uani 0.563(4) 1 d PD A 1 C56 C 0.0957(9) 0.5627(5) 0.2606(5) 0.049(2) Uani 0.563(4) 1 d PD A 1 H56 H 0.0374 0.58 0.2718 0.058 Uiso 0.563(4) 1 calc PR A 1 Cl4F Cl 0.1162(6) 0.5963(5) 0.2042(4) 0.0863(11) Uani 0.294(5) 1 d PD B 2 Cl5F Cl 0.2211(5) 0.5713(4) 0.3440(4) 0.0549(10) Uani 0.294(5) 1 d PD B 2 Cl6F Cl 0.0950(18) 0.4869(9) 0.2533(12) 0.079(2) Uani 0.294(5) 1 d PD B 2 C56F C 0.1130(16) 0.5602(10) 0.2786(8) 0.049(2) Uani 0.294(5) 1 d PD B 2 H56F H 0.056 0.5742 0.2941 0.058 Uiso 0.294(5) 1 calc PR B 2 Cl4G Cl 0.1043(8) 0.6484(7) 0.2169(6) 0.0863(11) Uani 0.142(2) 1 d PD C 3 Cl5G Cl 0.2024(13) 0.5712(9) 0.3346(9) 0.0549(10) Uani 0.142(2) 1 d PD C 3 Cl6G Cl 0.0897(8) 0.5220(5) 0.2054(8) 0.079(2) Uani 0.142(2) 1 d PD C 3 C56G C 0.107(2) 0.5835(8) 0.2598(11) 0.049(2) Uani 0.142(2) 1 d PD C 3 H56G H 0.0465 0.5846 0.2763 0.058 Uiso 0.142(2) 1 calc PR C 3 Cl7 Cl 0.1511(2) 1.02143(11) 0.06022(14) 0.0484(6) Uani 0.5 1 d PD D -1 Cl8 Cl -0.0276(7) 0.9592(5) 0.0449(4) 0.0708(15) Uani 0.5 1 d PD D -1 Cl9 Cl 0.0014(7) 1.0310(5) -0.0649(4) 0.0708(15) Uani 0.5 1 d PD D -1 C57 C 0.0563(6) 0.9847(4) 0.0030(4) 0.038(2) Uani 0.5 1 d PD D -1 H57 H 0.0843 0.9507 -0.0158 0.045 Uiso 0.5 1 calc PR D -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 Pt1 0.01266(5) 0.01022(5) 0.01209(5) 0.00043(4) 0.00266(4) 0.00062(4) Pt2 0.01184(5) 0.01077(5) 0.01434(6) 0.00127(4) 0.00271(4) 0.00017(4) Pt3 0.01225(5) 0.01015(5) 0.01411(6) 0.00010(4) 0.00196(4) 0.00018(4) I1 0.02067(10) 0.01250(10) 0.02135(11) 0.00081(8) 0.00226(9) -0.00322(8) I2 0.01246(9) 0.02925(13) 0.02417(12) -0.00193(10) 0.00238(9) -0.00135(9) I3 0.02780(12) 0.01686(11) 0.02245(11) -0.00751(9) 0.00825(9) -0.00603(9) S1 0.0139(3) 0.0120(4) 0.0134(4) 0.0006(3) 0.0029(3) 0.0010(3) S2 0.0168(4) 0.0111(4) 0.0133(4) 0.0002(3) 0.0033(3) 0.0003(3) S3 0.0132(3) 0.0114(4) 0.0170(4) -0.0002(3) 0.0036(3) 0.0008(3) P1 0.0130(4) 0.0114(4) 0.0153(4) 0.0013(3) 0.0028(3) 0.0010(3) P2 0.0165(4) 0.0140(4) 0.0155(4) 0.0003(3) 0.0059(3) 0.0014(3) P3 0.0124(4) 0.0138(4) 0.0166(4) 0.0011(3) 0.0017(3) -0.0004(3) C1 0.0127(14) 0.0174(16) 0.0139(15) 0.0018(13) -0.0004(12) 0.0010(12) C2 0.0148(15) 0.0147(15) 0.0138(15) 0.0019(12) -0.0007(12) 0.0009(12) C3 0.0189(16) 0.0195(17) 0.0165(16) 0.0023(13) 0.0047(13) 0.0034(14) C4 0.0193(17) 0.032(2) 0.0191(17) 0.0077(15) 0.0062(14) -0.0008(15) C5 0.0203(17) 0.0214(18) 0.0232(18) 0.0099(15) 0.0045(14) 0.0000(14) C6 0.0173(16) 0.0174(17) 0.0210(17) 0.0054(14) 0.0027(14) 0.0022(13) C7 0.0143(15) 0.0201(17) 0.0180(16) -0.0021(13) 0.0006(13) 0.0009(13) C8 0.0199(17) 0.0236(19) 0.0254(19) 0.0055(15) -0.0004(15) -0.0038(15) C9 0.028(2) 0.037(2) 0.034(2) 0.0066(19) -0.0036(18) -0.0116(18) C10 0.035(2) 0.041(3) 0.034(2) 0.006(2) -0.0155(19) -0.012(2) C11 0.035(2) 0.037(3) 0.032(2) 0.0089(19) -0.0133(19) -0.002(2) C12 0.0256(19) 0.0201(18) 0.031(2) 0.0061(16) -0.0060(16) -0.0009(15) C13 0.0216(16) 0.0115(15) 0.0179(16) 0.0014(13) 0.0060(13) 0.0020(13) C14 0.0253(19) 0.0221(19) 0.029(2) -0.0049(16) 0.0062(16) -0.0020(15) C15 0.036(2) 0.023(2) 0.035(2) -0.0080(17) 0.0055(19) -0.0057(17) C16 0.050(3) 0.0192(19) 0.031(2) -0.0054(17) 0.015(2) 0.0037(18) C17 0.037(2) 0.023(2) 0.033(2) -0.0035(17) 0.0071(19) 0.0124(17) C18 0.0239(18) 0.0199(18) 0.029(2) -0.0031(15) 0.0036(16) 0.0061(15) C19 0.0213(16) 0.0154(16) 0.0162(16) 0.0026(13) 0.0067(13) -0.0014(13) C20 0.0183(16) 0.0178(16) 0.0143(15) 0.0000(13) 0.0040(13) -0.0010(13) C21 0.0282(19) 0.0172(17) 0.0191(17) 0.0011(14) 0.0035(15) -0.0021(15) C22 0.036(2) 0.0235(19) 0.028(2) 0.0063(16) 0.0119(18) -0.0051(17) C23 0.036(2) 0.035(2) 0.032(2) 0.0070(18) 0.0207(19) -0.0041(19) C24 0.0276(19) 0.029(2) 0.031(2) 0.0039(17) 0.0174(17) 0.0038(16) C25 0.0194(16) 0.0144(16) 0.0171(16) -0.0003(13) 0.0012(13) 0.0023(13) C26 0.032(2) 0.029(2) 0.0191(18) -0.0007(16) 0.0053(16) 0.0037(17) C27 0.054(3) 0.034(2) 0.0161(18) -0.0017(17) 0.0033(18) 0.012(2) C28 0.047(3) 0.029(2) 0.028(2) -0.0016(18) -0.008(2) -0.003(2) C29 0.034(2) 0.036(2) 0.035(2) -0.002(2) -0.0006(19) -0.0075(19) C30 0.0255(19) 0.029(2) 0.0224(19) -0.0015(16) 0.0044(15) -0.0053(16) C31 0.0165(15) 0.0184(17) 0.0197(17) 0.0037(13) 0.0080(13) 0.0031(13) C32 0.0245(19) 0.0227(19) 0.033(2) -0.0029(17) 0.0036(17) 0.0048(16) C33 0.039(2) 0.032(2) 0.047(3) -0.002(2) 0.011(2) 0.015(2) C34 0.023(2) 0.045(3) 0.044(3) 0.005(2) 0.0105(19) 0.0155(19) C35 0.0198(18) 0.045(3) 0.041(3) 0.000(2) 0.0050(18) 0.0002(19) C36 0.0210(18) 0.030(2) 0.035(2) -0.0027(18) 0.0071(17) -0.0013(16) C37 0.0145(15) 0.0164(16) 0.0202(17) 0.0019(13) 0.0030(13) 0.0021(13) C38 0.0134(14) 0.0138(15) 0.0204(16) 0.0038(13) 0.0026(13) 0.0024(12) C39 0.0159(16) 0.0164(17) 0.033(2) 0.0022(15) 0.0041(15) -0.0009(13) C40 0.0238(18) 0.0155(17) 0.037(2) 0.0092(16) 0.0089(17) 0.0016(14) C41 0.0219(18) 0.0249(19) 0.029(2) 0.0132(16) 0.0017(16) 0.0028(15) C42 0.0203(17) 0.0225(18) 0.0250(19) 0.0050(15) 0.0008(15) 0.0014(15) C43 0.0160(15) 0.0157(16) 0.0265(18) -0.0011(14) 0.0061(14) 0.0008(13) C44 0.0228(19) 0.034(2) 0.036(2) 0.0094(18) 0.0107(17) 0.0038(17) C45 0.0203(18) 0.035(2) 0.051(3) 0.006(2) 0.0143(19) 0.0077(17) C46 0.027(2) 0.034(2) 0.045(3) 0.002(2) 0.0219(19) 0.0032(18) C47 0.034(2) 0.043(3) 0.032(2) 0.007(2) 0.0192(19) 0.006(2) C48 0.0231(18) 0.026(2) 0.032(2) 0.0065(16) 0.0124(16) 0.0072(15) C49 0.0262(18) 0.0202(18) 0.0168(17) 0.0005(14) -0.0029(14) 0.0037(15) C50 0.040(2) 0.031(2) 0.026(2) -0.0023(18) -0.0071(18) -0.0085(19) C51 0.083(4) 0.028(2) 0.038(3) 0.000(2) -0.013(3) -0.016(3) C52 0.103(5) 0.020(2) 0.032(3) -0.007(2) -0.013(3) 0.007(3) C53 0.086(4) 0.053(3) 0.022(2) 0.001(2) 0.009(3) 0.026(3) C54 0.045(3) 0.039(3) 0.024(2) 0.0018(18) 0.0099(19) 0.011(2) Cl1 0.0750(9) 0.0413(7) 0.0454(7) 0.0073(6) 0.0203(7) 0.0150(7) Cl2 0.0673(8) 0.0336(6) 0.0309(6) -0.0053(5) 0.0020(5) -0.0132(6) Cl3 0.0349(5) 0.0424(6) 0.0294(5) 0.0118(5) 0.0071(4) -0.0054(5) C55 0.036(2) 0.027(2) 0.026(2) -0.0004(17) 0.0050(17) -0.0111(18) Cl4 0.0526(19) 0.157(4) 0.056(2) -0.014(2) 0.0260(17) -0.015(2) Cl5 0.0326(13) 0.066(2) 0.066(2) -0.0407(16) 0.0144(15) -0.0078(15) Cl6 0.0426(10) 0.0493(11) 0.151(6) -0.033(3) 0.036(3) -0.0047(8) C56 0.026(4) 0.053(4) 0.074(6) -0.039(5) 0.026(4) -0.016(4) Cl4F 0.0526(19) 0.157(4) 0.056(2) -0.014(2) 0.0260(17) -0.015(2) Cl5F 0.0326(13) 0.066(2) 0.066(2) -0.0407(16) 0.0144(15) -0.0078(15) Cl6F 0.0426(10) 0.0493(11) 0.151(6) -0.033(3) 0.036(3) -0.0047(8) C56F 0.026(4) 0.053(4) 0.074(6) -0.039(5) 0.026(4) -0.016(4) Cl4G 0.0526(19) 0.157(4) 0.056(2) -0.014(2) 0.0260(17) -0.015(2) Cl5G 0.0326(13) 0.066(2) 0.066(2) -0.0407(16) 0.0144(15) -0.0078(15) Cl6G 0.0426(10) 0.0493(11) 0.151(6) -0.033(3) 0.036(3) -0.0047(8) C56G 0.026(4) 0.053(4) 0.074(6) -0.039(5) 0.026(4) -0.016(4) Cl7 0.0542(15) 0.0365(13) 0.0525(15) 0.0081(11) 0.0110(12) -0.0029(11) Cl8 0.078(4) 0.083(4) 0.055(4) 0.025(3) 0.026(3) 0.000(3) Cl9 0.078(4) 0.083(4) 0.055(4) 0.025(3) 0.026(3) 0.000(3) C57 0.049(5) 0.038(5) 0.025(4) 0.003(4) 0.011(4) 0.013(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P2 2.2531(9) . ? Pt1 P1 2.2566(8) . ? Pt1 S1 2.3568(8) . ? Pt1 S2 2.3612(8) . ? Pt2 P3 2.2242(9) . ? Pt2 S3 2.2857(8) . ? Pt2 S1 2.3779(8) . ? Pt2 I1 2.6151(3) . ? Pt3 S2 2.3071(8) . ? Pt3 S3 2.3102(8) . ? Pt3 I2 2.6113(3) . ? Pt3 I3 2.6118(3) . ? S1 C2 1.778(3) . ? S2 C20 1.787(3) . ? S3 C38 1.787(3) . ? P1 C13 1.802(3) . ? P1 C1 1.810(3) . ? P1 C7 1.817(3) . ? P2 C25 1.804(4) . ? P2 C31 1.812(3) . ? P2 C19 1.816(3) . ? P3 C49 1.797(4) . ? P3 C37 1.810(4) . ? P3 C43 1.814(4) . ? C1 C2 1.389(5) . ? C1 C6 1.396(5) . ? C2 C3 1.398(5) . ? C3 C4 1.383(5) . ? C4 C5 1.389(5) . ? C5 C6 1.387(5) . ? C7 C12 1.389(5) . ? C7 C8 1.397(5) . ? C8 C9 1.389(5) . ? C9 C10 1.380(6) . ? C10 C11 1.378(6) . ? C11 C12 1.377(5) . ? C13 C18 1.383(5) . ? C13 C14 1.400(5) . ? C14 C15 1.384(5) . ? C15 C16 1.376(6) . ? C16 C17 1.382(6) . ? C17 C18 1.391(5) . ? C19 C20 1.392(5) . ? C19 C24 1.397(5) . ? C20 C21 1.392(5) . ? C21 C22 1.386(5) . ? C22 C23 1.378(6) . ? C23 C24 1.383(6) . ? C25 C30 1.394(5) . ? C25 C26 1.399(5) . ? C26 C27 1.383(6) . ? C27 C28 1.385(7) . ? C28 C29 1.372(6) . ? C29 C30 1.389(5) . ? C31 C32 1.387(5) . ? C31 C36 1.390(5) . ? C32 C33 1.389(6) . ? C33 C34 1.379(6) . ? C34 C35 1.370(6) . ? C35 C36 1.382(6) . ? C37 C38 1.394(5) . ? C37 C42 1.396(5) . ? C38 C39 1.392(5) . ? C39 C40 1.385(5) . ? C40 C41 1.384(5) . ? C41 C42 1.379(5) . ? C43 C48 1.383(5) . ? C43 C44 1.391(5) . ? C44 C45 1.377(6) . ? C45 C46 1.370(6) . ? C46 C47 1.383(6) . ? C47 C48 1.390(5) . ? C49 C54 1.377(6) . ? C49 C50 1.396(6) . ? C50 C51 1.377(6) . ? C51 C52 1.359(8) . ? C52 C53 1.358(8) . ? C53 C54 1.402(7) . ? Cl1 C55 1.750(4) . ? Cl2 C55 1.753(4) . ? Cl3 C55 1.756(4) . ? Cl4 C56 1.741(10) . ? Cl5 C56 1.761(9) . ? Cl6 C56 1.772(10) . ? Cl4F C56F 1.734(15) . ? Cl5F C56F 1.755(14) . ? Cl6F C56F 1.767(14) . ? Cl4G C56G 1.728(15) . ? Cl5G C56G 1.765(15) . ? Cl6G C56G 1.772(16) . ? Cl7 C57 1.743(8) . ? Cl8 C57 1.744(11) . ? Cl9 C57 1.750(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 99.92(3) . . ? P2 Pt1 S1 175.56(3) . . ? P1 Pt1 S1 83.89(3) . . ? P2 Pt1 S2 84.47(3) . . ? P1 Pt1 S2 173.64(3) . . ? S1 Pt1 S2 91.92(3) . . ? P3 Pt2 S3 86.93(3) . . ? P3 Pt2 S1 171.65(3) . . ? S3 Pt2 S1 84.73(3) . . ? P3 Pt2 I1 91.90(2) . . ? S3 Pt2 I1 177.82(2) . . ? S1 Pt2 I1 96.44(2) . . ? S2 Pt3 S3 87.30(3) . . ? S2 Pt3 I2 95.38(2) . . ? S3 Pt3 I2 174.18(2) . . ? S2 Pt3 I3 174.39(2) . . ? S3 Pt3 I3 87.17(2) . . ? I2 Pt3 I3 90.208(8) . . ? C2 S1 Pt1 104.67(11) . . ? C2 S1 Pt2 107.81(11) . . ? Pt1 S1 Pt2 91.43(3) . . ? C20 S2 Pt3 113.16(12) . . ? C20 S2 Pt1 103.11(12) . . ? Pt3 S2 Pt1 103.61(3) . . ? C38 S3 Pt2 104.15(12) . . ? C38 S3 Pt3 107.76(11) . . ? Pt2 S3 Pt3 110.24(3) . . ? C13 P1 C1 105.05(16) . . ? C13 P1 C7 108.77(16) . . ? C1 P1 C7 102.21(15) . . ? C13 P1 Pt1 121.39(12) . . ? C1 P1 Pt1 106.98(11) . . ? C7 P1 Pt1 110.57(12) . . ? C25 P2 C31 106.89(16) . . ? C25 P2 C19 105.42(16) . . ? C31 P2 C19 104.57(16) . . ? C25 P2 Pt1 113.18(12) . . ? C31 P2 Pt1 119.43(12) . . ? C19 P2 Pt1 106.15(12) . . ? C49 P3 C37 106.39(17) . . ? C49 P3 C43 105.93(18) . . ? C37 P3 C43 105.07(16) . . ? C49 P3 Pt2 120.37(12) . . ? C37 P3 Pt2 106.07(11) . . ? C43 P3 Pt2 111.90(12) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 P1 115.8(3) . . ? C6 C1 P1 123.9(3) . . ? C1 C2 C3 120.2(3) . . ? C1 C2 S1 120.3(3) . . ? C3 C2 S1 119.5(3) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 120.8(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C1 119.6(3) . . ? C12 C7 C8 119.2(3) . . ? C12 C7 P1 120.9(3) . . ? C8 C7 P1 119.4(3) . . ? C9 C8 C7 119.9(4) . . ? C10 C9 C8 120.2(4) . . ? C11 C10 C9 119.7(4) . . ? C12 C11 C10 120.8(4) . . ? C11 C12 C7 120.1(4) . . ? C18 C13 C14 119.6(3) . . ? C18 C13 P1 123.1(3) . . ? C14 C13 P1 117.3(3) . . ? C15 C14 C13 119.8(4) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C17 119.8(4) . . ? C16 C17 C18 120.5(4) . . ? C13 C18 C17 119.7(4) . . ? C20 C19 C24 119.7(3) . . ? C20 C19 P2 117.1(3) . . ? C24 C19 P2 123.1(3) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 S2 119.9(3) . . ? C19 C20 S2 119.6(3) . . ? C22 C21 C20 119.6(4) . . ? C23 C22 C21 120.2(4) . . ? C22 C23 C24 120.8(4) . . ? C23 C24 C19 119.5(4) . . ? C30 C25 C26 118.5(3) . . ? C30 C25 P2 119.8(3) . . ? C26 C25 P2 121.6(3) . . ? C27 C26 C25 120.4(4) . . ? C26 C27 C28 120.5(4) . . ? C29 C28 C27 119.4(4) . . ? C28 C29 C30 120.8(4) . . ? C29 C30 C25 120.2(4) . . ? C32 C31 C36 119.6(3) . . ? C32 C31 P2 122.4(3) . . ? C36 C31 P2 118.0(3) . . ? C31 C32 C33 119.6(4) . . ? C34 C33 C32 120.5(4) . . ? C35 C34 C33 119.9(4) . . ? C34 C35 C36 120.5(4) . . ? C35 C36 C31 120.0(4) . . ? C38 C37 C42 119.4(3) . . ? C38 C37 P3 116.5(3) . . ? C42 C37 P3 124.0(3) . . ? C39 C38 C37 120.4(3) . . ? C39 C38 S3 119.3(3) . . ? C37 C38 S3 120.2(3) . . ? C40 C39 C38 119.0(3) . . ? C41 C40 C39 120.9(3) . . ? C42 C41 C40 120.0(3) . . ? C41 C42 C37 120.1(4) . . ? C48 C43 C44 118.9(3) . . ? C48 C43 P3 120.2(3) . . ? C44 C43 P3 120.8(3) . . ? C45 C44 C43 120.4(4) . . ? C46 C45 C44 120.3(4) . . ? C45 C46 C47 120.3(4) . . ? C46 C47 C48 119.5(4) . . ? C43 C48 C47 120.5(4) . . ? C54 C49 C50 119.6(4) . . ? C54 C49 P3 119.4(3) . . ? C50 C49 P3 120.9(3) . . ? C51 C50 C49 120.2(5) . . ? C52 C51 C50 119.8(5) . . ? C53 C52 C51 121.2(5) . . ? C52 C53 C54 120.3(5) . . ? C49 C54 C53 118.9(5) . . ? Cl1 C55 Cl2 110.9(2) . . ? Cl1 C55 Cl3 110.7(2) . . ? Cl2 C55 Cl3 110.8(2) . . ? Cl4 C56 Cl5 107.6(6) . . ? Cl4 C56 Cl6 111.3(8) . . ? Cl5 C56 Cl6 112.3(8) . . ? Cl4F C56F Cl5F 111.4(10) . . ? Cl4F C56F Cl6F 104.0(14) . . ? Cl5F C56F Cl6F 112.8(14) . . ? Cl4G C56G Cl5G 118.5(16) . . ? Cl4G C56G Cl6G 113.5(14) . . ? Cl5G C56G Cl6G 110.4(13) . . ? Cl7 C57 Cl8 110.2(5) . . ? Cl7 C57 Cl9 109.0(5) . . ? Cl8 C57 Cl9 111.9(7) . . ? # END of CIF #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#