#------------------------------------------------------------------------------ #$Date: 2019-05-18 04:10:05 +0300 (Sat, 18 May 2019) $ #$Revision: 215289 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/34/7123496.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7123496 loop_ _publ_author_name 'Hidalgo, Nereida' 'Maya, Celia' 'Campos, Jes\'us' _publ_section_title ; Cooperative Activation of X-H (X = H, C, O, N) Bonds by a Pt(0)/Ag(I) Metal-Only Lewis Pair ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC03008E _journal_year 2019 _chemical_formula_sum 'C50 H108 Ag2 F6 O6 P4 Pt2 S2' _chemical_formula_weight 1713.28 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-04-10 deposited with the CCDC. 2019-05-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.020(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.4375(6) _cell_length_b 16.5694(9) _cell_length_c 17.6644(9) _cell_measurement_reflns_used 9877 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 22.10 _cell_measurement_theta_min 2.48 _cell_volume 3274.2(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type AgK\a _diffrn_radiation_wavelength 0.56086 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 83347 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 19.665 _diffrn_reflns_theta_max 26.341 _diffrn_reflns_theta_min 1.733 _exptl_absorpt_coefficient_mu 2.742 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.738 _exptl_crystal_description prism _exptl_crystal_F_000 1704 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.658 _refine_diff_density_min -4.535 _refine_diff_density_rms 0.235 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 374 _refine_ls_number_reflns 13080 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 0.952 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0478 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.3311P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1263 _refine_ls_wR_factor_ref 0.1487 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9470 _reflns_number_total 13080 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc03008e2.cif _cod_data_source_block 3 _cod_database_code 7123496 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL ag_ner1318a_0m in P2(1)/c ag_ner1318a_0m.res created by SHELXL-2018/3 at 11:56:06 on 28-Mar-2019 CELL 0.56086 11.4375 16.5694 17.6644 90.000 102.020 90.000 ZERR 2.00 0.0006 0.0009 0.0009 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O F P S Ag Pt UNIT 100 216 12 12 8 4 4 4 L.S. 10 ACTA BOND FMAP 2 PLAN 4 sadi c25 f1b C25 f2b c25 f3b sadi s1 o1b s1 o2b s1 o3b sadi o1b o2b o2b o3b o3b o1b sadi f1b f2b f2b f3b f3b f1b TEMP 0.000 WGHT 0.100000 0.331100 FVAR 0.06969 0.91057 0.73272 0.72889 MOLE 1 PT1 8 0.191200 0.426202 0.242478 11.00000 0.01721 0.01571 = 0.01847 0.00094 -0.00018 -0.00265 PART 1 AG1 7 0.324442 0.474250 0.372868 21.00000 0.02570 0.05205 = 0.02346 -0.01200 0.00240 -0.01268 PART 2 AG1B 7 0.341627 0.444044 0.376023 -21.00000 0.03600 PART 0 S1 6 0.432814 0.617209 0.494423 11.00000 0.03076 0.03742 = 0.03869 -0.01944 -0.00262 -0.00088 P1 5 0.046416 0.382178 0.305588 11.00000 0.01787 0.01987 = 0.02355 0.00780 -0.00052 -0.00373 P2 5 0.331689 0.460355 0.171528 11.00000 0.01515 0.01861 = 0.01934 -0.00029 0.00147 0.00215 PART 1 F1 4 0.260319 0.714787 0.456335 41.00000 0.26883 0.19518 = 0.11253 0.01634 -0.06177 0.18076 F2 4 0.408514 0.765323 0.513979 41.00000 0.34060 0.01988 = 0.23289 0.01047 0.25018 0.00910 F3 4 0.310350 0.703886 0.578926 41.00000 0.05300 0.06008 = 0.06563 0.02753 0.03725 0.03135 PART 2 F1B 4 0.217715 0.686770 0.476497 -41.00000 0.02194 F2B 4 0.362832 0.777545 0.501371 -41.00000 0.03465 F3B 4 0.333709 0.690772 0.590814 -41.00000 0.02765 PART 1 O1 3 0.354852 0.552932 0.480667 31.00000 0.06280 0.04710 = 0.04874 -0.03046 0.01946 -0.03099 O2 3 0.480864 0.642263 0.427699 31.00000 0.17626 0.07642 = 0.10728 -0.07090 0.12269 -0.08197 O3 3 0.518065 0.609500 0.566637 31.00000 0.07141 0.13950 = 0.05807 -0.04524 -0.03322 0.06302 PART 2 O1B 3 0.364373 0.557961 0.524575 -31.00000 0.09560 O2B 3 0.419663 0.615398 0.418113 -31.00000 0.08749 O3B 3 0.534857 0.634106 0.541826 -31.00000 0.02604 PART 0 C1 1 -0.041283 0.470480 0.333734 11.00000 0.02572 0.02097 = 0.03792 0.00727 0.01156 -0.00083 C2 1 0.044237 0.535776 0.374598 11.00000 0.04951 0.02784 = 0.04859 -0.00857 0.02466 -0.00673 AFIX 137 H2A 2 0.096903 0.552174 0.341643 11.00000 -1.50000 H2B 2 0.090385 0.514546 0.422086 11.00000 -1.50000 H2C 2 -0.001070 0.581461 0.385631 11.00000 -1.50000 AFIX 0 C3 1 -0.133258 0.451162 0.385322 11.00000 0.03128 0.04361 = 0.06754 0.00834 0.02733 0.00152 AFIX 137 H3A 2 -0.183165 0.497406 0.387135 11.00000 -1.50000 H3B 2 -0.091244 0.438027 0.436745 11.00000 -1.50000 H3C 2 -0.181905 0.406177 0.363799 11.00000 -1.50000 AFIX 0 C4 1 -0.111460 0.512336 0.261074 11.00000 0.03792 0.03434 = 0.06336 0.01637 0.01834 0.01317 AFIX 137 H4A 2 -0.145661 0.561456 0.275476 11.00000 -1.50000 H4B 2 -0.174089 0.477315 0.235271 11.00000 -1.50000 H4C 2 -0.058637 0.524485 0.226910 11.00000 -1.50000 AFIX 0 C5 1 0.102910 0.316671 0.395666 11.00000 0.02576 0.03622 = 0.03956 0.02254 0.00352 0.00035 C6 1 0.205840 0.265788 0.381721 11.00000 0.04016 0.05718 = 0.05989 0.02761 0.01144 0.01680 AFIX 137 H6A 2 0.244581 0.240612 0.429301 11.00000 -1.50000 H6B 2 0.262071 0.299401 0.363011 11.00000 -1.50000 H6C 2 0.176334 0.224986 0.343984 11.00000 -1.50000 AFIX 0 C7 1 0.153520 0.370574 0.467442 11.00000 0.04720 0.07035 = 0.03074 0.01503 -0.00170 -0.01106 AFIX 137 H7A 2 0.199370 0.337865 0.507816 11.00000 -1.50000 H7B 2 0.088548 0.395252 0.485601 11.00000 -1.50000 H7C 2 0.203779 0.411769 0.453069 11.00000 -1.50000 AFIX 0 C8 1 0.006741 0.265719 0.420666 11.00000 0.04021 0.04656 = 0.04900 0.02907 0.01031 0.00221 AFIX 137 H8A 2 -0.019537 0.224432 0.382819 11.00000 -1.50000 H8B 2 -0.059748 0.299441 0.425116 11.00000 -1.50000 H8C 2 0.038895 0.241171 0.469820 11.00000 -1.50000 AFIX 0 C9 1 -0.058869 0.316630 0.232645 11.00000 0.02893 0.02998 = 0.04155 0.00054 -0.00210 -0.01364 C10 1 -0.081353 0.358383 0.154347 11.00000 0.06038 0.05524 = 0.02777 -0.00345 -0.00251 -0.02636 AFIX 137 H10A 2 -0.007429 0.363149 0.137077 11.00000 -1.50000 H10B 2 -0.113809 0.411164 0.158914 11.00000 -1.50000 H10C 2 -0.137024 0.327212 0.117588 11.00000 -1.50000 AFIX 0 C11 1 0.002133 0.236942 0.224755 11.00000 0.06142 0.03288 = 0.07512 -0.01833 0.01213 -0.01278 AFIX 137 H11A 2 -0.052707 0.201494 0.192026 11.00000 -1.50000 H11B 2 0.027228 0.212811 0.274922 11.00000 -1.50000 H11C 2 0.070576 0.245969 0.202312 11.00000 -1.50000 AFIX 0 C12 1 -0.184578 0.299934 0.251881 11.00000 0.03140 0.05493 = 0.05125 0.00781 -0.00323 -0.02035 AFIX 137 H12A 2 -0.227475 0.261918 0.215373 11.00000 -1.50000 H12B 2 -0.228848 0.349471 0.248816 11.00000 -1.50000 H12C 2 -0.174310 0.278200 0.303222 11.00000 -1.50000 AFIX 0 C13 1 0.436297 0.547634 0.209787 11.00000 0.02289 0.02744 = 0.05112 -0.00957 0.01767 -0.01044 C14 1 0.502758 0.585456 0.150849 11.00000 0.05040 0.04564 = 0.07337 -0.00505 0.04075 -0.01907 AFIX 137 H14A 2 0.551564 0.629370 0.174791 11.00000 -1.50000 H14B 2 0.445623 0.605141 0.107043 11.00000 -1.50000 H14C 2 0.552410 0.545371 0.134069 11.00000 -1.50000 AFIX 0 C15 1 0.532068 0.520969 0.279209 11.00000 0.02332 0.06912 = 0.04397 -0.03060 0.01317 -0.01577 AFIX 137 H15A 2 0.582124 0.480772 0.263003 11.00000 -1.50000 H15B 2 0.494377 0.498753 0.318280 11.00000 -1.50000 H15C 2 0.579813 0.566645 0.299917 11.00000 -1.50000 AFIX 0 C16 1 0.360836 0.614003 0.237902 11.00000 0.05704 0.02163 = 0.08646 -0.01754 0.04507 -0.01213 AFIX 137 H16A 2 0.307297 0.589806 0.266582 11.00000 -1.50000 H16B 2 0.315515 0.642341 0.194065 11.00000 -1.50000 H16C 2 0.412732 0.651167 0.270554 11.00000 -1.50000 AFIX 0 C17 1 0.424118 0.366939 0.163890 11.00000 0.03462 0.02841 = 0.02466 -0.00205 0.00392 0.01418 C18 1 0.343515 0.302303 0.115954 11.00000 0.07891 0.03128 = 0.04932 -0.02212 0.01883 -0.00358 AFIX 137 H18A 2 0.324489 0.318364 0.062580 11.00000 -1.50000 H18B 2 0.271123 0.296853 0.134926 11.00000 -1.50000 H18C 2 0.384868 0.251546 0.120580 11.00000 -1.50000 AFIX 0 C19 1 0.534548 0.379321 0.129208 11.00000 0.04083 0.05256 = 0.03040 -0.00310 0.01122 0.02592 AFIX 137 H19A 2 0.590684 0.413264 0.162777 11.00000 -1.50000 H19B 2 0.511443 0.404455 0.079363 11.00000 -1.50000 H19C 2 0.570893 0.328024 0.123694 11.00000 -1.50000 AFIX 0 C20 1 0.464488 0.331370 0.245734 11.00000 0.05586 0.03826 = 0.03786 0.00600 0.01173 0.03252 AFIX 137 H20A 2 0.514237 0.285106 0.243624 11.00000 -1.50000 H20B 2 0.395587 0.315545 0.265239 11.00000 -1.50000 H20C 2 0.508802 0.371290 0.279347 11.00000 -1.50000 AFIX 0 C21 1 0.248119 0.490067 0.069726 11.00000 0.02276 0.06195 = 0.02544 0.02068 0.00485 0.00729 C22 1 0.199017 0.576355 0.071829 11.00000 0.03488 0.07761 = 0.08146 0.05893 0.02467 0.02782 AFIX 137 H22A 2 0.264165 0.614067 0.080436 11.00000 -1.50000 H22B 2 0.156201 0.580651 0.112982 11.00000 -1.50000 H22C 2 0.146064 0.588160 0.023381 11.00000 -1.50000 AFIX 0 C23 1 0.137311 0.436550 0.047265 11.00000 0.02641 0.11097 = 0.02640 0.01320 -0.00240 -0.00981 AFIX 137 H23A 2 0.098540 0.447392 -0.005368 11.00000 -1.50000 H23B 2 0.083148 0.447833 0.080766 11.00000 -1.50000 H23C 2 0.160712 0.380844 0.052303 11.00000 -1.50000 AFIX 0 C24 1 0.320577 0.482987 0.005525 11.00000 0.03157 0.09957 = 0.02760 0.01743 0.00456 0.00409 AFIX 137 H24A 2 0.345039 0.427977 0.001686 11.00000 -1.50000 H24B 2 0.389946 0.516944 0.017891 11.00000 -1.50000 H24C 2 0.271852 0.499634 -0.042969 11.00000 -1.50000 AFIX 0 C25 1 0.340437 0.700354 0.513561 11.00000 0.08917 0.03239 = 0.03714 0.01009 0.01173 0.02216 HKLF 4 REM ag_ner1318a_0m in P2(1)/c REM wR2 = 0.1487, GooF = S = 0.948, Restrained GooF = 0.952 for all data REM R1 = 0.0478 for 9470 Fo > 4sig(Fo) and 0.0777 for all 13080 data REM 374 parameters refined using 12 restraints END WGHT 0.0575 3.7292 REM Highest difference peak 1.658, deepest hole -4.535, 1-sigma level 0.235 Q1 1 -0.1886 0.2178 0.2585 11.00000 0.05 1.66 Q2 1 0.3562 0.5473 0.5455 11.00000 0.05 1.51 Q3 1 0.1096 0.4185 0.2701 11.00000 0.05 1.37 Q4 1 0.0978 0.4511 0.2294 11.00000 0.05 1.34 ; _shelx_res_checksum 52358 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.19120(2) 0.42620(2) 0.24248(2) 0.01769(6) Uani 1 1 d . . . . . Ag1 Ag 0.32444(8) 0.47425(11) 0.37287(3) 0.0341(3) Uani 0.911(6) 1 d . . P A 1 Ag1B Ag 0.3416(8) 0.4440(8) 0.3760(4) 0.0360(18) Uiso 0.089(6) 1 d . . P A 2 S1 S 0.43281(13) 0.61721(9) 0.49442(8) 0.0370(3) Uani 1 1 d D . . . . P1 P 0.04642(10) 0.38218(7) 0.30559(7) 0.0211(2) Uani 1 1 d . . . . . P2 P 0.33169(10) 0.46035(7) 0.17153(6) 0.0180(2) Uani 1 1 d . . . . . F1 F 0.260(2) 0.7148(12) 0.4563(7) 0.207(9) Uani 0.729(18) 1 d . . P B 1 F2 F 0.409(2) 0.7653(4) 0.5140(11) 0.170(8) Uani 0.729(18) 1 d . . P B 1 F3 F 0.3104(7) 0.7039(5) 0.5789(5) 0.056(2) Uani 0.729(18) 1 d . . P B 1 F1B F 0.2177(10) 0.6868(7) 0.4765(6) 0.022(3) Uiso 0.271(18) 1 d D . P B 2 F2B F 0.3628(13) 0.7775(9) 0.5014(9) 0.035(4) Uiso 0.271(18) 1 d D . P B 2 F3B F 0.3337(16) 0.6908(10) 0.5908(8) 0.028(4) Uiso 0.271(18) 1 d D . P B 2 O1 O 0.3549(7) 0.5529(4) 0.4807(5) 0.052(2) Uani 0.733(17) 1 d . . P A 1 O2 O 0.4809(11) 0.6423(5) 0.4277(6) 0.106(5) Uani 0.733(17) 1 d . . P A 1 O3 O 0.5181(10) 0.6095(10) 0.5666(6) 0.096(5) Uani 0.733(17) 1 d . . P A 1 O1B O 0.364(2) 0.5580(17) 0.5246(16) 0.096(11) Uiso 0.267(17) 1 d D . P A 2 O2B O 0.420(2) 0.6154(19) 0.4181(11) 0.087(9) Uiso 0.267(17) 1 d D . P A 2 O3B O 0.5349(15) 0.6341(10) 0.5418(9) 0.026(4) Uiso 0.267(17) 1 d D . P A 2 C1 C -0.0413(4) 0.4705(3) 0.3337(3) 0.0275(9) Uani 1 1 d . . . . . C2 C 0.0442(6) 0.5358(3) 0.3746(4) 0.0399(13) Uani 1 1 d . . . . . H2A H 0.096903 0.552174 0.341643 0.060 Uiso 1 1 calc R U . . . H2B H 0.090385 0.514546 0.422086 0.060 Uiso 1 1 calc R U . . . H2C H -0.001070 0.581461 0.385631 0.060 Uiso 1 1 calc R U . . . C3 C -0.1333(6) 0.4512(4) 0.3853(4) 0.0450(15) Uani 1 1 d . . . . . H3A H -0.183165 0.497406 0.387135 0.068 Uiso 1 1 calc R U . . . H3B H -0.091244 0.438027 0.436745 0.068 Uiso 1 1 calc R U . . . H3C H -0.181905 0.406177 0.363799 0.068 Uiso 1 1 calc R U . . . C4 C -0.1115(6) 0.5123(4) 0.2611(4) 0.0441(14) Uani 1 1 d . . . . . H4A H -0.145661 0.561456 0.275476 0.066 Uiso 1 1 calc R U . . . H4B H -0.174089 0.477315 0.235271 0.066 Uiso 1 1 calc R U . . . H4C H -0.058637 0.524485 0.226910 0.066 Uiso 1 1 calc R U . . . C5 C 0.1029(5) 0.3167(3) 0.3957(3) 0.0343(12) Uani 1 1 d . . . . . C6 C 0.2058(6) 0.2658(4) 0.3817(4) 0.0523(17) Uani 1 1 d . . . . . H6A H 0.244581 0.240612 0.429301 0.078 Uiso 1 1 calc R U . . . H6B H 0.262071 0.299401 0.363011 0.078 Uiso 1 1 calc R U . . . H6C H 0.176334 0.224986 0.343984 0.078 Uiso 1 1 calc R U . . . C7 C 0.1535(6) 0.3706(5) 0.4674(3) 0.0509(17) Uani 1 1 d . . . . . H7A H 0.199370 0.337865 0.507816 0.076 Uiso 1 1 calc R U . . . H7B H 0.088548 0.395252 0.485601 0.076 Uiso 1 1 calc R U . . . H7C H 0.203779 0.411769 0.453069 0.076 Uiso 1 1 calc R U . . . C8 C 0.0067(6) 0.2657(4) 0.4207(4) 0.0451(15) Uani 1 1 d . . . . . H8A H -0.019537 0.224432 0.382819 0.068 Uiso 1 1 calc R U . . . H8B H -0.059748 0.299441 0.425116 0.068 Uiso 1 1 calc R U . . . H8C H 0.038895 0.241171 0.469820 0.068 Uiso 1 1 calc R U . . . C9 C -0.0589(5) 0.3166(3) 0.2326(3) 0.0349(11) Uani 1 1 d . . . . . C10 C -0.0814(6) 0.3584(4) 0.1543(3) 0.0495(17) Uani 1 1 d . . . . . H10A H -0.007429 0.363149 0.137077 0.074 Uiso 1 1 calc R U . . . H10B H -0.113809 0.411164 0.158914 0.074 Uiso 1 1 calc R U . . . H10C H -0.137024 0.327212 0.117588 0.074 Uiso 1 1 calc R U . . . C11 C 0.0021(7) 0.2369(4) 0.2248(5) 0.0568(18) Uani 1 1 d . . . . . H11A H -0.052707 0.201494 0.192026 0.085 Uiso 1 1 calc R U . . . H11B H 0.027228 0.212811 0.274922 0.085 Uiso 1 1 calc R U . . . H11C H 0.070576 0.245969 0.202312 0.085 Uiso 1 1 calc R U . . . C12 C -0.1846(5) 0.2999(5) 0.2519(4) 0.0476(16) Uani 1 1 d . . . . . H12A H -0.227475 0.261918 0.215373 0.071 Uiso 1 1 calc R U . . . H12B H -0.228848 0.349471 0.248816 0.071 Uiso 1 1 calc R U . . . H12C H -0.174310 0.278200 0.303222 0.071 Uiso 1 1 calc R U . . . C13 C 0.4363(5) 0.5476(3) 0.2098(3) 0.0324(11) Uani 1 1 d . . . . . C14 C 0.5028(7) 0.5855(4) 0.1508(5) 0.0524(18) Uani 1 1 d . . . . . H14A H 0.551564 0.629370 0.174791 0.079 Uiso 1 1 calc R U . . . H14B H 0.445623 0.605141 0.107043 0.079 Uiso 1 1 calc R U . . . H14C H 0.552410 0.545371 0.134069 0.079 Uiso 1 1 calc R U . . . C15 C 0.5321(5) 0.5210(4) 0.2792(4) 0.0446(15) Uani 1 1 d . . . . . H15A H 0.582124 0.480772 0.263003 0.067 Uiso 1 1 calc R U . . . H15B H 0.494377 0.498753 0.318280 0.067 Uiso 1 1 calc R U . . . H15C H 0.579813 0.566645 0.299917 0.067 Uiso 1 1 calc R U . . . C16 C 0.3608(6) 0.6140(3) 0.2379(4) 0.0507(18) Uani 1 1 d . . . . . H16A H 0.307297 0.589806 0.266582 0.076 Uiso 1 1 calc R U . . . H16B H 0.315515 0.642341 0.194065 0.076 Uiso 1 1 calc R U . . . H16C H 0.412732 0.651167 0.270554 0.076 Uiso 1 1 calc R U . . . C17 C 0.4241(5) 0.3669(3) 0.1639(3) 0.0296(10) Uani 1 1 d . . . . . C18 C 0.3435(7) 0.3023(4) 0.1160(4) 0.0524(17) Uani 1 1 d . . . . . H18A H 0.324489 0.318364 0.062580 0.079 Uiso 1 1 calc R U . . . H18B H 0.271123 0.296853 0.134926 0.079 Uiso 1 1 calc R U . . . H18C H 0.384868 0.251546 0.120580 0.079 Uiso 1 1 calc R U . . . C19 C 0.5345(5) 0.3793(4) 0.1292(3) 0.0407(14) Uani 1 1 d . . . . . H19A H 0.590684 0.413264 0.162777 0.061 Uiso 1 1 calc R U . . . H19B H 0.511443 0.404455 0.079363 0.061 Uiso 1 1 calc R U . . . H19C H 0.570893 0.328024 0.123694 0.061 Uiso 1 1 calc R U . . . C20 C 0.4645(6) 0.3314(4) 0.2457(3) 0.0437(15) Uani 1 1 d . . . . . H20A H 0.514237 0.285106 0.243624 0.066 Uiso 1 1 calc R U . . . H20B H 0.395587 0.315545 0.265239 0.066 Uiso 1 1 calc R U . . . H20C H 0.508802 0.371290 0.279347 0.066 Uiso 1 1 calc R U . . . C21 C 0.2481(5) 0.4901(4) 0.0697(3) 0.0367(13) Uani 1 1 d . . . . . C22 C 0.1990(6) 0.5764(4) 0.0718(5) 0.063(2) Uani 1 1 d . . . . . H22A H 0.264165 0.614067 0.080436 0.094 Uiso 1 1 calc R U . . . H22B H 0.156201 0.580651 0.112982 0.094 Uiso 1 1 calc R U . . . H22C H 0.146064 0.588160 0.023381 0.094 Uiso 1 1 calc R U . . . C23 C 0.1373(6) 0.4366(5) 0.0473(4) 0.056(2) Uani 1 1 d . . . . . H23A H 0.098540 0.447392 -0.005368 0.084 Uiso 1 1 calc R U . . . H23B H 0.083148 0.447833 0.080766 0.084 Uiso 1 1 calc R U . . . H23C H 0.160712 0.380844 0.052303 0.084 Uiso 1 1 calc R U . . . C24 C 0.3206(6) 0.4830(5) 0.0055(3) 0.0531(18) Uani 1 1 d . . . . . H24A H 0.345039 0.427977 0.001686 0.080 Uiso 1 1 calc R U . . . H24B H 0.389946 0.516944 0.017891 0.080 Uiso 1 1 calc R U . . . H24C H 0.271852 0.499634 -0.042969 0.080 Uiso 1 1 calc R U . . . C25 C 0.3404(7) 0.7004(4) 0.5136(3) 0.0531(18) Uani 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01721(9) 0.01571(8) 0.01847(9) 0.00094(5) -0.00018(6) -0.00265(5) Ag1 0.0257(3) 0.0521(7) 0.0235(3) -0.0120(3) 0.00240(19) -0.0127(3) S1 0.0308(7) 0.0374(7) 0.0387(7) -0.0194(6) -0.0026(5) -0.0009(5) P1 0.0179(5) 0.0199(5) 0.0235(5) 0.0078(4) -0.0005(4) -0.0037(4) P2 0.0152(5) 0.0186(5) 0.0193(5) -0.0003(4) 0.0015(4) 0.0021(4) F1 0.269(18) 0.195(14) 0.113(9) 0.016(9) -0.062(11) 0.181(13) F2 0.341(19) 0.020(3) 0.233(13) 0.010(5) 0.250(14) 0.009(6) F3 0.053(4) 0.060(4) 0.066(4) 0.028(3) 0.037(3) 0.031(3) O1 0.063(5) 0.047(4) 0.049(4) -0.030(3) 0.019(3) -0.031(3) O2 0.176(10) 0.076(5) 0.107(7) -0.071(5) 0.123(7) -0.082(6) O3 0.071(6) 0.139(11) 0.058(6) -0.045(7) -0.033(5) 0.063(7) C1 0.026(2) 0.021(2) 0.038(3) 0.0073(18) 0.012(2) -0.0008(17) C2 0.050(3) 0.028(3) 0.049(3) -0.009(2) 0.025(3) -0.007(2) C3 0.031(3) 0.044(3) 0.068(4) 0.008(3) 0.027(3) 0.002(3) C4 0.038(3) 0.034(3) 0.063(4) 0.016(3) 0.018(3) 0.013(2) C5 0.026(2) 0.036(3) 0.040(3) 0.023(2) 0.004(2) 0.000(2) C6 0.040(3) 0.057(4) 0.060(4) 0.028(3) 0.011(3) 0.017(3) C7 0.047(4) 0.070(4) 0.031(3) 0.015(3) -0.002(3) -0.011(3) C8 0.040(3) 0.047(3) 0.049(3) 0.029(3) 0.010(3) 0.002(3) C9 0.029(3) 0.030(2) 0.042(3) 0.001(2) -0.002(2) -0.014(2) C10 0.060(4) 0.055(4) 0.028(3) -0.003(3) -0.003(3) -0.026(3) C11 0.061(5) 0.033(3) 0.075(5) -0.018(3) 0.012(4) -0.013(3) C12 0.031(3) 0.055(4) 0.051(4) 0.008(3) -0.003(3) -0.020(3) C13 0.023(2) 0.027(2) 0.051(3) -0.010(2) 0.018(2) -0.0104(19) C14 0.050(4) 0.046(3) 0.073(5) -0.005(3) 0.041(4) -0.019(3) C15 0.023(2) 0.069(4) 0.044(3) -0.031(3) 0.013(2) -0.016(3) C16 0.057(4) 0.022(2) 0.086(5) -0.018(3) 0.045(4) -0.012(2) C17 0.035(3) 0.028(2) 0.025(2) -0.0021(18) 0.0039(19) 0.014(2) C18 0.079(5) 0.031(3) 0.049(4) -0.022(3) 0.019(3) -0.004(3) C19 0.041(3) 0.053(3) 0.030(3) -0.003(2) 0.011(2) 0.026(3) C20 0.056(4) 0.038(3) 0.038(3) 0.006(2) 0.012(3) 0.033(3) C21 0.023(2) 0.062(4) 0.025(2) 0.021(2) 0.0049(19) 0.007(2) C22 0.035(3) 0.078(5) 0.081(5) 0.059(4) 0.025(3) 0.028(3) C23 0.026(3) 0.111(6) 0.026(3) 0.013(3) -0.002(2) -0.010(3) C24 0.032(3) 0.100(6) 0.028(3) 0.017(3) 0.005(2) 0.004(3) C25 0.089(5) 0.032(3) 0.037(3) 0.010(2) 0.012(3) 0.022(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -1.6473 0.7167 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -0.6812 5.7081 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P1 Pt1 P2 174.69(4) . . P1 Pt1 Ag1 90.92(3) . . P2 Pt1 Ag1 93.44(3) . . P1 Pt1 Ag1B 90.20(16) . . P2 Pt1 Ag1B 93.45(17) . . O1 Ag1 O3 89.4(3) . 3_666 O1 Ag1 Pt1 150.9(2) . . O3 Ag1 Pt1 118.3(2) 3_666 . O3B Ag1B Pt1 136.8(7) 3_666 . O3B S1 O2B 123.3(11) . . O3B S1 O1B 113.1(10) . . O2B S1 O1B 114.2(10) . . O1 S1 O3 112.4(8) . . O1 S1 O2 114.6(4) . . O3 S1 O2 116.1(8) . . O3B S1 C25 101.2(9) . . O2B S1 C25 105.1(13) . . O1 S1 C25 103.9(4) . . O1B S1 C25 93.8(14) . . O3 S1 C25 102.5(4) . . O2 S1 C25 105.5(5) . . C1 P1 C9 108.8(2) . . C1 P1 C5 108.9(2) . . C9 P1 C5 107.1(2) . . C1 P1 Pt1 110.84(14) . . C9 P1 Pt1 105.67(18) . . C5 P1 Pt1 115.36(17) . . C17 P2 C13 109.0(2) . . C17 P2 C21 108.6(2) . . C13 P2 C21 106.9(3) . . C17 P2 Pt1 107.49(17) . . C13 P2 Pt1 116.75(16) . . C21 P2 Pt1 107.78(16) . . S1 O1 Ag1 124.8(4) . . S1 O3 Ag1 140.3(6) . 3_666 S1 O3B Ag1B 130.6(11) . 3_666 C4 C1 C2 104.3(4) . . C4 C1 C3 106.4(5) . . C2 C1 C3 108.1(5) . . C4 C1 P1 110.1(4) . . C2 C1 P1 110.3(4) . . C3 C1 P1 116.9(4) . . C6 C5 C8 111.9(5) . . C6 C5 C7 106.4(5) . . C8 C5 C7 104.5(5) . . C6 C5 P1 108.6(4) . . C8 C5 P1 114.5(4) . . C7 C5 P1 110.7(4) . . C11 C9 C10 107.9(6) . . C11 C9 C12 109.1(5) . . C10 C9 C12 106.8(5) . . C11 C9 P1 108.7(4) . . C10 C9 P1 108.6(4) . . C12 C9 P1 115.6(4) . . C15 C13 C16 107.6(5) . . C15 C13 C14 106.7(5) . . C16 C13 C14 108.3(5) . . C15 C13 P2 110.9(4) . . C16 C13 P2 107.6(4) . . C14 C13 P2 115.4(4) . . C19 C17 C20 108.4(5) . . C19 C17 C18 108.8(5) . . C20 C17 C18 106.1(5) . . C19 C17 P2 116.0(4) . . C20 C17 P2 108.0(3) . . C18 C17 P2 109.1(4) . . C23 C21 C22 104.9(5) . . C23 C21 C24 108.0(5) . . C22 C21 C24 110.1(5) . . C23 C21 P2 108.6(4) . . C22 C21 P2 109.2(5) . . C24 C21 P2 115.5(4) . . F1 C25 F3 116.0(13) . . F1 C25 F2 100.5(12) . . F3 C25 F2 103.1(8) . . F2B C25 F3B 108.7(9) . . F2B C25 F1B 106.2(8) . . F3B C25 F1B 100.4(8) . . F1 C25 S1 110.9(7) . . F3 C25 S1 118.9(5) . . F2 C25 S1 104.7(8) . . F2B C25 S1 124.2(9) . . F3B C25 S1 104.5(9) . . F1B C25 S1 110.4(6) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 P1 2.2991(11) . Pt1 P2 2.3047(11) . Pt1 Ag1 2.6076(5) . Pt1 Ag1B 2.631(7) . Ag1 O1 2.274(6) . Ag1 O3 2.347(10) 3_666 Ag1B O3B 2.22(2) 3_666 S1 O3B 1.317(16) . S1 O2B 1.325(18) . S1 O1 1.378(6) . S1 O1B 1.426(19) . S1 O3 1.441(8) . S1 O2 1.461(7) . S1 C25 1.810(7) . P1 C1 1.898(5) . P1 C9 1.909(5) . P1 C5 1.923(5) . P2 C17 1.895(5) . P2 C13 1.909(5) . P2 C21 1.917(5) . F1 C25 1.238(12) . F2 C25 1.328(15) . F3 C25 1.273(10) . F1B C25 1.438(12) . F2B C25 1.331(13) . F3B C25 1.392(14) . C1 C4 1.531(8) . C1 C2 1.534(8) . C1 C3 1.562(7) . C5 C6 1.509(8) . C5 C8 1.523(7) . C5 C7 1.560(9) . C9 C11 1.513(9) . C9 C10 1.520(8) . C9 C12 1.569(8) . C13 C15 1.529(9) . C13 C16 1.543(7) . C13 C14 1.544(8) . C17 C19 1.528(8) . C17 C20 1.540(7) . C17 C18 1.546(8) . C21 C23 1.530(9) . C21 C22 1.539(9) . C21 C24 1.542(8) .