#------------------------------------------------------------------------------ #$Date: 2019-05-18 04:10:05 +0300 (Sat, 18 May 2019) $ #$Revision: 215289 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/34/7123495.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_7123495 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 'C26 H57 F6 N O5 P2 Pt S2' _chemical_formula_weight 898.87 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _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 107.260(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.3950(7) _cell_length_b 11.6828(4) _cell_length_c 18.9417(8) _cell_measurement_reflns_used 9906 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 21.95 _cell_measurement_theta_min 2.20 _cell_volume 3676.0(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 0.999 _diffrn_measured_fraction_theta_max 0.996 _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 0.0481 _diffrn_reflns_av_unetI/netI 0.0505 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 31111 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 19.665 _diffrn_reflns_theta_max 22.013 _diffrn_reflns_theta_min 1.637 _exptl_absorpt_coefficient_mu 2.214 _exptl_absorpt_correction_T_max 0.7447 _exptl_absorpt_correction_T_min 0.5948 _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 colourless _exptl_crystal_density_diffrn 1.624 _exptl_crystal_description prism _exptl_crystal_F_000 1816 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.060 _refine_diff_density_max 2.019 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.149 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 419 _refine_ls_number_reflns 9156 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.810 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0343 _refine_ls_shift/su_max 0.016 _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^+0.9779P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.1127 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7474 _reflns_number_total 9156 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc03008e2.cif _cod_data_source_block 8 _cod_database_code 7123495 _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_estimated_absorpt_t_min 0.718 _shelx_estimated_absorpt_t_max 0.879 _shelx_res_file ; TITL ner1819a in P2(1)/n ner1819a.res created by SHELXL-2018/3 at 12:19:11 on 28-Mar-2019 CELL 0.56086 17.3950 11.6828 18.9417 90.000 107.260 90.000 ZERR 4.00 0.0007 0.0004 0.0008 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H F P S Pt N O UNIT 104 228 24 8 8 4 4 20 L.S. 4 ACTA BOND FMAP 2 PLAN 10 SIZE 0.06 0.14 0.16 FREE C18 H18C TEMP 0.000 WGHT 0.100000 0.977900 FVAR 0.07050 MOLE 1 PT1 6 0.978211 0.863524 0.208858 0.99927 0.01075 0.00817 = 0.00946 -0.00024 0.00070 0.00062 S2 5 0.803759 0.887177 0.536876 11.00000 0.01884 0.01741 = 0.01463 -0.00597 0.00795 -0.00733 S1 5 0.942035 0.832348 0.497814 11.00000 0.01940 0.01263 = 0.01694 -0.00106 0.00785 -0.00392 P2 4 0.877231 1.000508 0.167576 11.00000 0.01429 0.00948 = 0.01480 0.00087 -0.00101 0.00162 P1 4 1.070367 0.714794 0.218599 11.00000 0.00994 0.01047 = 0.01074 -0.00242 0.00136 0.00018 C14 1 0.801260 0.885018 0.259162 11.00000 0.02985 0.05326 = 0.07497 0.02885 0.02783 0.00647 AFIX 137 H14A 2 0.774742 0.888745 0.296908 11.00000 -1.50000 H14B 2 0.853654 0.851633 0.279213 11.00000 -1.50000 H14C 2 0.770021 0.838876 0.218898 11.00000 -1.50000 AFIX 0 C13 1 0.809818 1.005960 0.231184 11.00000 0.02304 0.03468 = 0.03777 0.01082 0.01440 0.01056 C16 1 0.726334 1.060626 0.198735 11.00000 0.02118 0.05005 = 0.05095 0.01385 0.01081 0.01705 AFIX 137 H16A 2 0.695385 1.015785 0.157636 11.00000 -1.50000 H16B 2 0.732411 1.136918 0.182334 11.00000 -1.50000 H16C 2 0.699091 1.063301 0.235978 11.00000 -1.50000 AFIX 0 N1 7 0.848046 0.827266 0.485200 11.00000 0.01638 0.02013 = 0.01322 -0.01000 0.00424 -0.00436 C26 1 0.777360 1.028554 0.493131 11.00000 0.02107 0.02950 = 0.01789 -0.00254 0.00555 -0.00021 F4 3 0.842568 1.088347 0.495381 11.00000 0.02455 0.02344 = 0.03345 0.00703 0.00501 -0.00424 F6 3 0.733563 1.086302 0.528371 11.00000 0.03325 0.03118 = 0.03241 -0.00292 0.01442 0.01211 F5 3 0.733240 1.017235 0.422596 11.00000 0.02711 0.04341 = 0.01698 -0.00217 0.00077 0.00561 O4 8 0.727537 0.833238 0.526322 11.00000 0.02778 0.03147 = 0.03594 -0.01715 0.01964 -0.01788 O3 8 0.986709 0.910660 0.552759 11.00000 0.02547 0.02182 = 0.02482 -0.00845 0.00757 -0.00762 C25 1 0.975252 0.690721 0.536052 11.00000 0.02935 0.02380 = 0.03289 0.00505 0.00964 0.00329 F2 3 1.054654 0.681741 0.549195 11.00000 0.03040 0.04255 = 0.06618 0.00809 0.00398 0.01086 F3 3 0.959841 0.676396 0.599811 11.00000 0.08613 0.03644 = 0.03608 0.01795 0.02874 0.01121 C9 1 1.040525 0.620062 0.131941 11.00000 0.01934 0.01775 = 0.01062 -0.00720 0.00113 0.00427 C11 1 1.105425 0.533787 0.125774 11.00000 0.02918 0.02128 = 0.02414 -0.01156 0.01296 0.00051 AFIX 137 H11A 2 1.125318 0.492801 0.171509 11.00000 -1.50000 H11B 2 1.148966 0.574159 0.115490 11.00000 -1.50000 H11C 2 1.082358 0.480742 0.086489 11.00000 -1.50000 AFIX 0 C10 1 0.965117 0.553079 0.130809 11.00000 0.02269 0.05312 = 0.06487 -0.04122 0.00761 -0.01156 AFIX 137 H10A 2 0.947506 0.509375 0.085966 11.00000 -1.50000 H10B 2 0.923380 0.605321 0.133246 11.00000 -1.50000 H10C 2 0.976903 0.502295 0.172500 11.00000 -1.50000 AFIX 0 C12 1 1.019402 0.690944 0.060537 11.00000 0.11697 0.04679 = 0.00817 -0.00490 0.00476 0.03848 AFIX 137 H12A 2 1.034486 0.769304 0.072251 11.00000 -1.50000 H12B 2 0.962530 0.686543 0.036458 11.00000 -1.50000 H12C 2 1.047976 0.661325 0.028237 11.00000 -1.50000 AFIX 0 C8 1 1.186348 0.881991 0.280647 11.00000 0.02056 0.03905 = 0.07010 -0.03369 0.01621 -0.01421 AFIX 137 H8A 2 1.191522 0.855539 0.329826 11.00000 -1.50000 H8B 2 1.140931 0.932484 0.264767 11.00000 -1.50000 H8C 2 1.234342 0.922242 0.280282 11.00000 -1.50000 AFIX 0 C5 1 1.173896 0.778689 0.227731 11.00000 0.01822 0.02171 = 0.04194 -0.02023 0.01502 -0.00918 C7 1 1.172814 0.830913 0.151483 11.00000 0.06388 0.04075 = 0.06163 -0.02193 0.05198 -0.03079 AFIX 137 H7A 2 1.222237 0.871303 0.156622 11.00000 -1.50000 H7B 2 1.128334 0.882918 0.135102 11.00000 -1.50000 H7C 2 1.167205 0.770597 0.115888 11.00000 -1.50000 AFIX 0 C1 1 1.075029 0.619790 0.301458 11.00000 0.03019 0.02202 = 0.01200 0.00787 0.00858 0.01082 C3 1 0.989839 0.607507 0.308460 11.00000 0.04102 0.02873 = 0.03804 0.00961 0.02639 0.00759 AFIX 137 H3A 2 0.957782 0.561752 0.268390 11.00000 -1.50000 H3B 2 0.965899 0.681883 0.306784 11.00000 -1.50000 H3C 2 0.992496 0.571195 0.354589 11.00000 -1.50000 AFIX 0 C2 1 1.116621 0.505201 0.303314 11.00000 0.06029 0.02029 = 0.03545 0.01214 0.02154 0.02068 AFIX 137 H2A 2 1.121531 0.467984 0.349632 11.00000 -1.50000 H2B 2 1.169200 0.517032 0.297915 11.00000 -1.50000 H2C 2 1.085449 0.458078 0.263570 11.00000 -1.50000 AFIX 0 C21 1 0.812257 0.963374 0.070091 11.00000 0.04184 0.02827 = 0.02136 -0.01339 -0.02271 0.01623 C24 1 0.754187 1.058015 0.031515 11.00000 0.03547 0.02689 = 0.03144 -0.00023 -0.01704 0.01202 AFIX 137 H24A 2 0.784297 1.122480 0.022676 11.00000 -1.50000 H24B 2 0.722009 1.081030 0.062379 11.00000 -1.50000 H24C 2 0.719804 1.029943 -0.014727 11.00000 -1.50000 AFIX 0 C22 1 0.762090 0.855522 0.077053 11.00000 0.05607 0.02039 = 0.07793 -0.00912 -0.03911 0.00322 AFIX 137 H22A 2 0.735073 0.826374 0.028655 11.00000 -1.50000 H22B 2 0.722998 0.876026 0.101521 11.00000 -1.50000 H22C 2 0.797336 0.797814 0.105268 11.00000 -1.50000 AFIX 0 C23 1 0.861191 0.931621 0.018618 11.00000 0.09484 0.11081 = 0.01679 -0.01204 -0.01194 0.06944 AFIX 137 H23A 2 0.825800 0.921674 -0.030619 11.00000 -1.50000 H23B 2 0.889702 0.861558 0.035107 11.00000 -1.50000 H23C 2 0.899011 0.991555 0.018820 11.00000 -1.50000 AFIX 0 C17 1 0.922705 1.148669 0.164409 11.00000 0.02707 0.01773 = 0.03155 0.01561 -0.00061 0.00107 C4 1 1.124935 0.684393 0.373497 11.00000 0.06095 0.03907 = 0.01363 0.00451 0.00178 0.02653 AFIX 137 H4A 2 1.120493 0.643982 0.416243 11.00000 -1.50000 H4B 2 1.104273 0.760601 0.373434 11.00000 -1.50000 H4C 2 1.180448 0.687962 0.374707 11.00000 -1.50000 AFIX 0 C6 1 1.244854 0.697413 0.251360 11.00000 0.01827 0.03739 = 0.10751 -0.02117 0.02570 -0.00115 AFIX 137 H6A 2 1.293334 0.737574 0.252427 11.00000 -1.50000 H6B 2 1.236885 0.635134 0.216873 11.00000 -1.50000 H6C 2 1.249283 0.668057 0.299744 11.00000 -1.50000 AFIX 0 C18 1 0.996125 1.162422 0.233711 11.00000 0.03576 0.01715 = 0.04822 0.00740 -0.00083 -0.00782 AFIX 137 H18A 2 1.021865 1.234469 0.231536 11.00000 -1.50000 H18B 2 1.033549 1.101321 0.235466 11.00000 -1.50000 H18C 2 0.978599 1.160024 0.277207 11.00000 -1.50000 AFIX 0 C19 1 0.864102 1.247926 0.157217 11.00000 0.03802 0.01392 = 0.04005 0.01055 -0.00915 0.00314 AFIX 137 H19A 2 0.846258 1.251410 0.200513 11.00000 -1.50000 H19B 2 0.818583 1.236644 0.114373 11.00000 -1.50000 H19C 2 0.890529 1.318282 0.152233 11.00000 -1.50000 AFIX 0 C15 1 0.853261 1.073884 0.302404 11.00000 0.04493 0.06807 = 0.02774 0.00352 0.02181 0.02770 AFIX 137 H15A 2 0.824781 1.063984 0.338319 11.00000 -1.50000 H15B 2 0.854533 1.153664 0.290664 11.00000 -1.50000 H15C 2 0.907301 1.045956 0.322219 11.00000 -1.50000 AFIX 0 C20 1 0.957400 1.153455 0.098409 11.00000 0.04831 0.06410 = 0.04959 0.03626 0.01452 -0.00996 AFIX 137 H20A 2 0.914063 1.155903 0.053105 11.00000 -1.50000 H20B 2 0.989686 1.086683 0.098785 11.00000 -1.50000 H20C 2 0.990051 1.220758 0.102248 11.00000 -1.50000 AFIX 0 O5 8 0.851060 0.913416 0.611422 11.00000 0.02623 0.02377 = 0.01268 -0.00448 0.00503 -0.00484 O2 8 0.956255 0.828291 0.427245 11.00000 0.03193 0.02369 = 0.02480 -0.00003 0.01727 -0.00268 F1 3 0.941069 0.606888 0.491109 11.00000 0.04412 0.01249 = 0.06117 -0.00566 0.01857 -0.00160 O1 8 1.024830 0.921791 0.325986 11.00000 0.02276 0.01714 = 0.01312 -0.00430 0.00617 -0.00492 H1 2 1.007783 0.905861 0.359158 11.00000 0.00498 H2 2 1.059356 0.949010 0.350010 11.00000 0.04659 H3P 2 0.943725 0.817432 0.139230 11.00000 0.05820 HKLF 4 REM ner1819a in P2(1)/n REM wR2 = 0.1127, GooF = S = 0.810, Restrained GooF = 0.810 for all data REM R1 = 0.0343 for 7474 Fo > 4sig(Fo) and 0.0494 for all 9156 data REM 419 parameters refined using 0 restraints END WGHT 0.0321 6.4049 REM Highest difference peak 2.019, deepest hole -1.274, 1-sigma level 0.149 Q1 1 0.9223 0.8612 0.2397 11.00000 0.05 2.02 Q2 1 1.0361 0.8627 0.1783 11.00000 0.05 2.00 Q3 1 1.2022 0.7923 0.3255 11.00000 0.05 0.91 Q4 1 1.0561 0.6612 0.3636 11.00000 0.05 0.80 Q5 1 0.9924 0.5233 0.2691 11.00000 0.05 0.77 Q6 1 1.0361 0.7936 0.3939 11.00000 0.05 0.76 Q7 1 0.9825 0.9853 0.2012 11.00000 0.05 0.64 Q8 1 0.9518 0.8013 0.2231 11.00000 0.05 0.62 Q9 1 1.1628 0.8857 0.1953 11.00000 0.05 0.62 Q10 1 0.9224 0.9643 0.2237 11.00000 0.05 0.61 ; _shelx_res_checksum 4897 loop_ _space_group_symop_operation_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' 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 Pt1 Pt 0.97821(2) 0.86352(2) 0.20886(2) 0.00996(7) Uani 1.000(2) 1 d . . S2 S 0.80376(7) 0.88718(10) 0.53688(7) 0.0163(2) Uani 1 1 d . . S1 S 0.94203(7) 0.83235(10) 0.49781(7) 0.0158(2) Uani 1 1 d . . P2 P 0.87723(7) 1.00051(9) 0.16758(7) 0.0140(3) Uani 1 1 d . . P1 P 1.07037(6) 0.71479(9) 0.21860(6) 0.0108(2) Uani 1 1 d . . C14 C 0.8013(4) 0.8850(6) 0.2592(5) 0.050(2) Uani 1 1 d . . H14A H 0.774742 0.888745 0.296908 0.075 Uiso 1 1 calc R U H14B H 0.853654 0.851633 0.279213 0.075 Uiso 1 1 calc R U H14C H 0.770021 0.838876 0.218898 0.075 Uiso 1 1 calc R U C13 C 0.8098(3) 1.0060(5) 0.2312(3) 0.0307(12) Uani 1 1 d . . C16 C 0.7263(3) 1.0606(6) 0.1987(4) 0.0407(15) Uani 1 1 d . . H16A H 0.695385 1.015785 0.157636 0.061 Uiso 1 1 calc R U H16B H 0.732411 1.136918 0.182334 0.061 Uiso 1 1 calc R U H16C H 0.699091 1.063301 0.235978 0.061 Uiso 1 1 calc R U N1 N 0.8480(2) 0.8273(3) 0.4852(2) 0.0166(8) Uani 1 1 d . . C26 C 0.7774(3) 1.0286(4) 0.4931(3) 0.0229(10) Uani 1 1 d . . F4 F 0.84257(17) 1.0883(3) 0.49538(18) 0.0279(7) Uani 1 1 d . . F6 F 0.73356(19) 1.0863(3) 0.52837(18) 0.0313(7) Uani 1 1 d . . F5 F 0.73324(18) 1.0172(3) 0.42260(17) 0.0304(7) Uani 1 1 d . . O4 O 0.7275(2) 0.8332(3) 0.5263(2) 0.0295(9) Uani 1 1 d . . O3 O 0.9867(2) 0.9107(3) 0.5528(2) 0.0240(8) Uani 1 1 d . . C25 C 0.9753(3) 0.6907(4) 0.5361(3) 0.0286(12) Uani 1 1 d . . F2 F 1.0547(2) 0.6817(3) 0.5492(2) 0.0486(10) Uani 1 1 d . . F3 F 0.9598(3) 0.6764(3) 0.5998(2) 0.0506(10) Uani 1 1 d . . C9 C 1.0405(3) 0.6201(4) 0.1319(3) 0.0166(9) Uani 1 1 d . . C11 C 1.1054(3) 0.5338(4) 0.1258(3) 0.0238(11) Uani 1 1 d . . H11A H 1.125318 0.492801 0.171509 0.036 Uiso 1 1 calc R U H11B H 1.148966 0.574159 0.115490 0.036 Uiso 1 1 calc R U H11C H 1.082358 0.480742 0.086489 0.036 Uiso 1 1 calc R U C10 C 0.9651(3) 0.5531(6) 0.1308(4) 0.0481(19) Uani 1 1 d . . H10A H 0.947506 0.509375 0.085966 0.072 Uiso 1 1 calc R U H10B H 0.923380 0.605321 0.133246 0.072 Uiso 1 1 calc R U H10C H 0.976903 0.502295 0.172500 0.072 Uiso 1 1 calc R U C12 C 1.0194(5) 0.6909(6) 0.0605(3) 0.060(3) Uani 1 1 d . . H12A H 1.034486 0.769304 0.072251 0.090 Uiso 1 1 calc R U H12B H 0.962530 0.686543 0.036458 0.090 Uiso 1 1 calc R U H12C H 1.047976 0.661325 0.028237 0.090 Uiso 1 1 calc R U C8 C 1.1863(3) 0.8820(5) 0.2806(4) 0.0426(18) Uani 1 1 d . . H8A H 1.191522 0.855539 0.329826 0.064 Uiso 1 1 calc R U H8B H 1.140931 0.932484 0.264767 0.064 Uiso 1 1 calc R U H8C H 1.234342 0.922242 0.280282 0.064 Uiso 1 1 calc R U C5 C 1.1739(3) 0.7787(4) 0.2277(3) 0.0260(12) Uani 1 1 d . . C7 C 1.1728(5) 0.8309(6) 0.1515(4) 0.0482(19) Uani 1 1 d . . H7A H 1.222237 0.871303 0.156622 0.072 Uiso 1 1 calc R U H7B H 1.128334 0.882918 0.135102 0.072 Uiso 1 1 calc R U H7C H 1.167205 0.770597 0.115888 0.072 Uiso 1 1 calc R U C1 C 1.0750(3) 0.6198(4) 0.3015(3) 0.0209(10) Uani 1 1 d . . C3 C 0.9898(4) 0.6075(5) 0.3085(4) 0.0328(13) Uani 1 1 d . . H3A H 0.957782 0.561752 0.268390 0.049 Uiso 1 1 calc R U H3B H 0.965899 0.681883 0.306784 0.049 Uiso 1 1 calc R U H3C H 0.992496 0.571195 0.354589 0.049 Uiso 1 1 calc R U C2 C 1.1166(4) 0.5052(4) 0.3033(3) 0.0371(15) Uani 1 1 d . . H2A H 1.121531 0.467984 0.349632 0.056 Uiso 1 1 calc R U H2B H 1.169200 0.517032 0.297915 0.056 Uiso 1 1 calc R U H2C H 1.085449 0.458078 0.263570 0.056 Uiso 1 1 calc R U C21 C 0.8123(4) 0.9634(5) 0.0701(3) 0.0375(16) Uani 1 1 d . . C24 C 0.7542(4) 1.0580(5) 0.0315(3) 0.0371(15) Uani 1 1 d . . H24A H 0.784297 1.122480 0.022676 0.056 Uiso 1 1 calc R U H24B H 0.722009 1.081030 0.062379 0.056 Uiso 1 1 calc R U H24C H 0.719804 1.029943 -0.014727 0.056 Uiso 1 1 calc R U C22 C 0.7621(5) 0.8555(5) 0.0771(5) 0.064(3) Uani 1 1 d . . H22A H 0.735073 0.826374 0.028655 0.096 Uiso 1 1 calc R U H22B H 0.722998 0.876026 0.101521 0.096 Uiso 1 1 calc R U H22C H 0.797336 0.797814 0.105268 0.096 Uiso 1 1 calc R U C23 C 0.8612(6) 0.9316(8) 0.0186(4) 0.080(3) Uani 1 1 d . . H23A H 0.825800 0.921674 -0.030619 0.120 Uiso 1 1 calc R U H23B H 0.889702 0.861558 0.035107 0.120 Uiso 1 1 calc R U H23C H 0.899011 0.991555 0.018820 0.120 Uiso 1 1 calc R U C17 C 0.9227(3) 1.1487(4) 0.1644(3) 0.0275(13) Uani 1 1 d . . C4 C 1.1249(4) 0.6844(5) 0.3735(3) 0.0399(16) Uani 1 1 d . . H4A H 1.120493 0.643982 0.416243 0.060 Uiso 1 1 calc R U H4B H 1.104273 0.760601 0.373434 0.060 Uiso 1 1 calc R U H4C H 1.180448 0.687962 0.374707 0.060 Uiso 1 1 calc R U C6 C 1.2449(3) 0.6974(5) 0.2514(5) 0.053(2) Uani 1 1 d . . H6A H 1.293334 0.737574 0.252427 0.079 Uiso 1 1 calc R U H6B H 1.236885 0.635134 0.216873 0.079 Uiso 1 1 calc R U H6C H 1.249283 0.668057 0.299744 0.079 Uiso 1 1 calc R U C18 C 0.9961(4) 1.1624(5) 0.2337(4) 0.0366(15) Uani 1 1 d . . H18A H 1.021865 1.234469 0.231536 0.055 Uiso 1 1 calc R U H18B H 1.033549 1.101321 0.235466 0.055 Uiso 1 1 calc R U H18C H 0.978599 1.160024 0.277207 0.055 Uiso 1 1 calc R U C19 C 0.8641(3) 1.2479(4) 0.1572(3) 0.0352(15) Uani 1 1 d . . H19A H 0.846258 1.251410 0.200513 0.053 Uiso 1 1 calc R U H19B H 0.818583 1.236644 0.114373 0.053 Uiso 1 1 calc R U H19C H 0.890529 1.318282 0.152233 0.053 Uiso 1 1 calc R U C15 C 0.8533(4) 1.0739(6) 0.3024(3) 0.0445(17) Uani 1 1 d . . H15A H 0.824781 1.063984 0.338319 0.067 Uiso 1 1 calc R U H15B H 0.854533 1.153664 0.290664 0.067 Uiso 1 1 calc R U H15C H 0.907301 1.045956 0.322219 0.067 Uiso 1 1 calc R U C20 C 0.9574(5) 1.1535(7) 0.0984(4) 0.054(2) Uani 1 1 d . . H20A H 0.914063 1.155903 0.053105 0.081 Uiso 1 1 calc R U H20B H 0.989686 1.086683 0.098785 0.081 Uiso 1 1 calc R U H20C H 0.990051 1.220758 0.102248 0.081 Uiso 1 1 calc R U O5 O 0.8511(2) 0.9134(3) 0.61142(18) 0.0211(7) Uani 1 1 d . . O2 O 0.9563(2) 0.8283(3) 0.4272(2) 0.0249(8) Uani 1 1 d . . F1 F 0.9411(2) 0.6069(3) 0.4911(2) 0.0386(9) Uani 1 1 d . . O1 O 1.0248(2) 0.9218(3) 0.3260(2) 0.0175(7) Uani 1 1 d . . H1 H 1.008(3) 0.906(4) 0.359(3) 0.005(12) Uiso 1 1 d . . H2 H 1.059(4) 0.949(7) 0.350(4) 0.05(2) Uiso 1 1 d . . H3P H 0.944(4) 0.817(6) 0.139(4) 0.06(2) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01075(9) 0.00817(10) 0.00946(10) -0.00024(5) 0.00070(6) 0.00062(5) S2 0.0188(5) 0.0174(5) 0.0146(6) -0.0060(4) 0.0079(4) -0.0073(4) S1 0.0194(5) 0.0126(5) 0.0169(6) -0.0011(4) 0.0079(4) -0.0039(4) P2 0.0143(5) 0.0095(5) 0.0148(6) 0.0009(4) -0.0010(4) 0.0016(4) P1 0.0099(5) 0.0105(5) 0.0107(5) -0.0024(4) 0.0014(4) 0.0002(4) C14 0.030(3) 0.053(4) 0.075(6) 0.029(4) 0.028(3) 0.006(3) C13 0.023(2) 0.035(3) 0.038(3) 0.011(2) 0.014(2) 0.011(2) C16 0.021(3) 0.050(4) 0.051(4) 0.014(3) 0.011(3) 0.017(3) N1 0.0164(18) 0.0201(18) 0.0132(19) -0.0100(16) 0.0042(15) -0.0044(15) C26 0.021(2) 0.030(3) 0.018(2) -0.003(2) 0.006(2) 0.000(2) F4 0.0246(15) 0.0234(15) 0.0335(18) 0.0070(13) 0.0050(13) -0.0042(12) F6 0.0333(16) 0.0312(17) 0.0324(18) -0.0029(14) 0.0144(14) 0.0121(14) F5 0.0271(16) 0.0434(19) 0.0170(15) -0.0022(13) 0.0008(13) 0.0056(14) O4 0.0278(19) 0.0315(19) 0.036(2) -0.0172(18) 0.0196(17) -0.0179(16) O3 0.0255(17) 0.0218(17) 0.0248(19) -0.0085(15) 0.0076(15) -0.0076(15) C25 0.029(3) 0.024(3) 0.033(3) 0.005(2) 0.010(2) 0.003(2) F2 0.0304(18) 0.043(2) 0.066(3) 0.008(2) 0.0040(18) 0.0109(16) F3 0.086(3) 0.0364(19) 0.036(2) 0.0179(17) 0.029(2) 0.011(2) C9 0.019(2) 0.018(2) 0.011(2) -0.0072(17) 0.0011(17) 0.0043(17) C11 0.029(3) 0.021(2) 0.024(3) -0.012(2) 0.013(2) 0.001(2) C10 0.023(3) 0.053(4) 0.065(5) -0.041(4) 0.008(3) -0.012(3) C12 0.117(7) 0.047(4) 0.008(3) -0.005(3) 0.005(3) 0.038(4) C8 0.021(3) 0.039(3) 0.070(5) -0.034(3) 0.016(3) -0.014(2) C5 0.018(2) 0.022(2) 0.042(3) -0.020(2) 0.015(2) -0.0092(19) C7 0.064(4) 0.041(3) 0.062(5) -0.022(3) 0.052(4) -0.031(3) C1 0.030(3) 0.022(2) 0.012(2) 0.0079(18) 0.009(2) 0.0108(19) C3 0.041(3) 0.029(3) 0.038(3) 0.010(3) 0.026(3) 0.008(2) C2 0.060(4) 0.020(3) 0.035(3) 0.012(2) 0.022(3) 0.021(3) C21 0.042(3) 0.028(3) 0.021(3) -0.013(2) -0.023(2) 0.016(2) C24 0.035(3) 0.027(3) 0.031(3) 0.000(2) -0.017(3) 0.012(2) C22 0.056(5) 0.020(3) 0.078(6) -0.009(3) -0.039(4) 0.003(3) C23 0.095(7) 0.111(7) 0.017(3) -0.012(4) -0.012(4) 0.069(6) C17 0.027(3) 0.018(2) 0.032(3) 0.016(2) -0.001(2) 0.001(2) C4 0.061(4) 0.039(3) 0.014(3) 0.005(2) 0.002(3) 0.027(3) C6 0.018(3) 0.037(3) 0.108(7) -0.021(4) 0.026(3) -0.001(2) C18 0.036(3) 0.017(2) 0.048(4) 0.007(3) -0.001(3) -0.008(2) C19 0.038(3) 0.014(2) 0.040(3) 0.011(2) -0.009(3) 0.003(2) C15 0.045(3) 0.068(5) 0.028(3) 0.004(3) 0.022(3) 0.028(3) C20 0.048(4) 0.064(5) 0.050(5) 0.036(4) 0.015(4) -0.010(3) O5 0.0262(17) 0.0238(17) 0.0127(16) -0.0045(14) 0.0050(14) -0.0048(14) O2 0.0319(19) 0.0237(17) 0.025(2) 0.0000(15) 0.0173(16) -0.0027(15) F1 0.044(2) 0.0125(13) 0.061(3) -0.0057(15) 0.0186(18) -0.0016(13) O1 0.0228(17) 0.0171(17) 0.0131(17) -0.0043(14) 0.0062(15) -0.0049(14) 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' 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' Pt Pt -0.6812 5.7081 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Pt1 P2 98.01(9) O1 Pt1 P1 96.32(9) P2 Pt1 P1 165.54(4) O4 S2 O5 117.9(2) O4 S2 N1 108.8(2) O5 S2 N1 117.4(2) O4 S2 C26 103.6(2) O5 S2 C26 104.1(2) N1 S2 C26 102.8(2) O3 S1 O2 119.6(2) O3 S1 N1 116.6(2) O2 S1 N1 108.4(2) O3 S1 C25 104.5(2) O2 S1 C25 102.6(3) N1 S1 C25 102.5(2) C21 P2 C17 107.9(3) C21 P2 C13 108.6(3) C17 P2 C13 109.0(3) C21 P2 Pt1 109.84(17) C17 P2 Pt1 110.75(17) C13 P2 Pt1 110.64(16) C1 P1 C5 110.2(3) C1 P1 C9 107.7(2) C5 P1 C9 108.1(2) C1 P1 Pt1 111.06(16) C5 P1 Pt1 108.87(16) C9 P1 Pt1 110.89(14) C14 C13 C16 110.1(5) C14 C13 C15 104.1(6) C16 C13 C15 107.0(5) C14 C13 P2 109.1(4) C16 C13 P2 116.4(4) C15 C13 P2 109.4(4) S2 N1 S1 124.2(2) F4 C26 F6 109.2(4) F4 C26 F5 108.5(4) F6 C26 F5 107.8(4) F4 C26 S2 111.2(3) F6 C26 S2 109.3(4) F5 C26 S2 110.7(4) F1 C25 F3 108.7(5) F1 C25 F2 107.8(5) F3 C25 F2 107.4(5) F1 C25 S1 112.8(4) F3 C25 S1 110.5(4) F2 C25 S1 109.5(4) C10 C9 C12 106.6(6) C10 C9 C11 108.0(4) C12 C9 C11 106.0(5) C10 C9 P1 108.8(4) C12 C9 P1 112.1(3) C11 C9 P1 115.0(3) C6 C5 C8 110.7(5) C6 C5 C7 107.6(6) C8 C5 C7 104.8(5) C6 C5 P1 116.4(4) C8 C5 P1 108.2(4) C7 C5 P1 108.5(4) C2 C1 C3 112.5(5) C2 C1 C4 105.4(4) C3 C1 C4 105.6(5) C2 C1 P1 115.9(4) C3 C1 P1 108.7(3) C4 C1 P1 108.2(4) C23 C21 C24 106.6(6) C23 C21 C22 106.9(6) C24 C21 C22 108.5(5) C23 C21 P2 113.2(5) C24 C21 P2 114.6(4) C22 C21 P2 106.7(5) C19 C17 C20 108.2(5) C19 C17 C18 111.1(5) C20 C17 C18 105.2(5) C19 C17 P2 114.8(4) C20 C17 P2 108.9(4) C18 C17 P2 108.2(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pt1 O1 2.231(4) Pt1 P2 2.3330(11) Pt1 P1 2.3340(11) S2 O4 1.427(4) S2 O5 1.441(3) S2 N1 1.578(4) S2 C26 1.844(5) S1 O3 1.430(3) S1 O2 1.431(4) S1 N1 1.582(4) S1 C25 1.830(5) P2 C21 1.907(5) P2 C17 1.911(5) P2 C13 1.916(6) P1 C1 1.904(5) P1 C5 1.909(5) P1 C9 1.919(5) C14 C13 1.532(8) C13 C16 1.538(7) C13 C15 1.554(9) C26 F4 1.322(6) C26 F6 1.335(6) C26 F5 1.335(6) C25 F1 1.318(7) C25 F3 1.323(7) C25 F2 1.333(6) C9 C10 1.522(8) C9 C12 1.535(8) C9 C11 1.543(6) C8 C5 1.542(7) C5 C6 1.516(8) C5 C7 1.563(9) C1 C2 1.517(7) C1 C3 1.533(8) C1 C4 1.576(8) C21 C23 1.518(11) C21 C24 1.529(7) C21 C22 1.560(10) C17 C19 1.523(7) C17 C20 1.542(10) C17 C18 1.544(8)