#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:09:07 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296019 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573220.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_1573220 loop_ _publ_author_name 'Atterberry, Benjamin A.' 'Wimmer, Erik' 'Klostermann, Sina' 'Frey, Wolfgang' 'K\"astner, Johannes' 'Estes, Deven' 'Rossini, Aaron J.' _publ_section_title ; Structural Characterization of Surface Immobilized Platinum Hydrides by Sensitivity-Enhanced 195Pt Solid State NMR Spectroscopy and DFT Calculations ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06450J _journal_year 2024 _chemical_formula_moiety 'C26 H58 N P2 Pt, B F4' _chemical_formula_sum 'C26 H58 B F4 N P2 Pt' _chemical_formula_weight 728.57 _chemical_name_systematic 'Pt-H_PtBu3_2-CH3CN [BF3]' _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_block_doi 10.5517/ccdc.csd.cc2jjpnf _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2024-03-12 deposited with the CCDC. 2024-11-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.461(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.585(2) _cell_length_b 12.110(3) _cell_length_c 29.773(6) _cell_measurement_reflns_used 5278 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.392 _cell_measurement_theta_min 1.682 _cell_volume 3095.2(12) _computing_cell_refinement 'Bruker APEXII Software Suite, 2008' _computing_data_collection 'Bruker APEXII Software Suite, 2008' _computing_data_reduction 'Bruker APEXII Software Suite, 2008' _computing_molecular_graphics 'SHELXTL-plus, XP (sheldrick, 1998)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker Kappa APEXII Duo' _diffrn_measurement_method 'Omega + Phi Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1200 _diffrn_reflns_av_unetI/netI 0.1473 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 28228 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.392 _diffrn_reflns_theta_min 1.682 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.677 _exptl_absorpt_correction_T_max 0.7365 _exptl_absorpt_correction_T_min 0.6496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, 1995' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.563 _exptl_crystal_description prism _exptl_crystal_F_000 1480 _exptl_crystal_size_max 0.073 _exptl_crystal_size_mid 0.062 _exptl_crystal_size_min 0.043 _refine_diff_density_max 5.440 _refine_diff_density_min -3.319 _refine_diff_density_rms 0.284 _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 7714 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0863 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+97.6813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1705 _refine_ls_wR_factor_ref 0.1980 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5278 _reflns_number_total 7714 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06450j2.cif _cod_data_source_block Pt-H-PtBu3_2-CH3CN-BF4 _cod_original_cell_volume 3095.2(14) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1573220 _shelx_shelxl_version_number 2014/7 _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 0.726 _shelx_estimated_absorpt_t_max 0.824 _shelx_res_file ; tech11.res created by SHELXL-2014/7 TITL tech11 in P2(1)/n CELL 0.71073 8.5850 12.1100 29.7726 90.000 90.461 90.000 ZERR 4.00 0.0024 0.0034 0.0061 0.000 0.009 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H B N F P PT UNIT 104 232 4 4 16 8 4 TEMP -123.150 SIZE 0.043 0.062 0.073 REM Tmax: 0.7365 Tmin: 0.6496 (multi-scan) REM prism, colourless OMIT -3 57 OMIT 4 0 2 OMIT 0 0 2 OMIT 7 7 3 OMIT 8 3 11 OMIT -8 6 3 L.S. 14 BOND $H CONF ACTA WPDB -1 FMAP 2 PLAN 20 TWIN -1 0 0 0 -1 0 0 0 1 ISOR 0.005 F4 C4 C6 WGHT 0.050100 97.681297 EXTI 0.001806 BASF 0.26111 FVAR 0.08199 MOLE 1 PT1 7 0.301286 0.618903 0.119677 11.00000 0.02636 0.01249 = 0.01261 0.00128 0.00026 -0.00053 AFIX 1 H1 2 0.209300 0.582100 0.087500 11.00000 -1.20000 AFIX 0 P1 6 0.290145 0.453955 0.160808 11.00000 0.01474 0.01094 = 0.01347 0.00055 0.00105 0.00074 P2 6 0.243069 0.759559 0.068958 11.00000 0.02252 0.01397 = 0.01213 0.00056 0.00129 0.00100 C1 1 0.178700 0.345479 0.127982 11.00000 0.02257 0.01118 = 0.01726 -0.00432 0.00313 -0.00325 C2 1 0.181987 0.228053 0.147506 11.00000 0.02958 0.02193 = 0.01991 -0.00007 -0.00380 -0.00591 AFIX 33 H2A 2 0.146266 0.229804 0.178678 11.00000 -1.50000 H2B 2 0.113204 0.180211 0.129699 11.00000 -1.50000 H2C 2 0.288589 0.199244 0.146595 11.00000 -1.50000 AFIX 0 C3 1 0.235866 0.337803 0.079027 11.00000 0.02278 0.03512 = 0.01717 -0.00614 -0.00194 -0.00281 AFIX 33 H3A 2 0.235277 0.411541 0.065466 11.00000 -1.50000 H3B 2 0.341990 0.308015 0.078725 11.00000 -1.50000 H3C 2 0.166605 0.288982 0.061828 11.00000 -1.50000 AFIX 0 C4 1 0.002519 0.377993 0.124337 11.00000 0.03727 0.02511 = 0.03050 -0.00087 -0.00336 -0.01220 AFIX 33 H4A 2 -0.006702 0.452736 0.111981 11.00000 -1.50000 H4B 2 -0.051700 0.325778 0.104513 11.00000 -1.50000 H4C 2 -0.044306 0.375815 0.154234 11.00000 -1.50000 AFIX 0 C5 1 0.482896 0.388798 0.176565 11.00000 0.03342 0.01434 = 0.01795 0.00010 0.00257 -0.00601 C6 1 0.553202 0.330935 0.135272 11.00000 0.04203 0.02474 = 0.03012 -0.00351 0.00783 0.00911 AFIX 33 H6A 2 0.479974 0.275272 0.123921 11.00000 -1.50000 H6B 2 0.572990 0.385677 0.111757 11.00000 -1.50000 H6C 2 0.651314 0.295090 0.143901 11.00000 -1.50000 AFIX 0 C7 1 0.609381 0.473944 0.191013 11.00000 0.03997 0.01608 = 0.02873 -0.00231 -0.00685 0.00757 AFIX 33 H7A 2 0.573533 0.514808 0.217395 11.00000 -1.50000 H7B 2 0.706308 0.435040 0.198446 11.00000 -1.50000 H7C 2 0.627985 0.525626 0.166302 11.00000 -1.50000 AFIX 0 C8 1 0.474402 0.302110 0.215503 11.00000 0.04013 0.01563 = 0.01836 0.00146 -0.01215 0.00007 AFIX 33 H8A 2 0.429997 0.336903 0.242219 11.00000 -1.50000 H8B 2 0.408474 0.240059 0.206126 11.00000 -1.50000 H8C 2 0.579421 0.275122 0.222530 11.00000 -1.50000 AFIX 0 C9 1 0.179963 0.489493 0.213553 11.00000 0.01774 0.01417 = 0.01805 0.00052 0.00587 0.00118 C10 1 0.110350 0.391376 0.238339 11.00000 0.03795 0.02962 = 0.01938 -0.00726 0.01055 -0.01359 AFIX 33 H10A 2 0.193307 0.339188 0.246322 11.00000 -1.50000 H10B 2 0.059315 0.417250 0.265719 11.00000 -1.50000 H10C 2 0.033645 0.354571 0.218921 11.00000 -1.50000 AFIX 0 C11 1 0.287848 0.549898 0.247246 11.00000 0.03023 0.02541 = 0.01179 -0.00506 -0.00288 0.00271 AFIX 33 H11A 2 0.373286 0.500763 0.256228 11.00000 -1.50000 H11B 2 0.330569 0.616240 0.233078 11.00000 -1.50000 H11C 2 0.228161 0.571028 0.273818 11.00000 -1.50000 AFIX 0 C12 1 0.052356 0.569464 0.201341 11.00000 0.03784 0.02201 = 0.02166 0.00826 0.01194 0.00970 AFIX 33 H12A 2 0.096925 0.632652 0.185390 11.00000 -1.50000 H12B 2 -0.024321 0.532575 0.181940 11.00000 -1.50000 H12C 2 0.001349 0.595254 0.228738 11.00000 -1.50000 AFIX 0 C13 1 0.318082 0.713172 0.012385 11.00000 0.02186 0.02395 = 0.01459 0.00210 0.00510 0.00325 C14 1 0.216163 0.619956 -0.007132 11.00000 0.05329 0.03133 = 0.02812 -0.00781 -0.00552 0.01608 AFIX 33 H14A 2 0.205308 0.561143 0.015235 11.00000 -1.50000 H14B 2 0.113029 0.649274 -0.014917 11.00000 -1.50000 H14C 2 0.265262 0.590104 -0.034141 11.00000 -1.50000 AFIX 0 C15 1 0.331757 0.803132 -0.023727 11.00000 0.05680 0.03297 = 0.01880 -0.00056 0.00189 -0.00772 AFIX 33 H15A 2 0.396238 0.863800 -0.012226 11.00000 -1.50000 H15B 2 0.379995 0.771916 -0.050612 11.00000 -1.50000 H15C 2 0.227763 0.831086 -0.031388 11.00000 -1.50000 AFIX 0 C16 1 0.480980 0.661561 0.019536 11.00000 0.04279 0.03306 = 0.04402 -0.00165 0.01943 0.01205 AFIX 33 H16A 2 0.475093 0.603773 0.042503 11.00000 -1.50000 H16B 2 0.516880 0.629326 -0.008743 11.00000 -1.50000 H16C 2 0.554295 0.718845 0.029384 11.00000 -1.50000 AFIX 0 C17 1 0.330394 0.900347 0.084198 11.00000 0.04537 0.02804 = 0.01004 -0.00163 -0.00630 -0.00440 C18 1 0.303418 0.924576 0.134152 11.00000 0.06460 0.02478 = 0.01054 -0.00408 -0.01076 0.00148 AFIX 33 H18A 2 0.336102 0.860729 0.152123 11.00000 -1.50000 H18B 2 0.364390 0.989441 0.143141 11.00000 -1.50000 H18C 2 0.192543 0.939023 0.139078 11.00000 -1.50000 AFIX 0 C19 1 0.280869 0.997600 0.055806 11.00000 0.03136 0.02626 = 0.02871 0.00116 0.01976 0.00463 AFIX 33 H19A 2 0.298787 0.980876 0.024059 11.00000 -1.50000 H19B 2 0.169904 1.012336 0.060426 11.00000 -1.50000 H19C 2 0.341751 1.062753 0.064490 11.00000 -1.50000 AFIX 0 C20 1 0.509736 0.892240 0.078320 11.00000 0.04113 0.03433 = 0.03565 0.00895 0.00096 -0.01346 AFIX 33 H20A 2 0.550003 0.830145 0.096041 11.00000 -1.50000 H20B 2 0.533657 0.880567 0.046542 11.00000 -1.50000 H20C 2 0.558642 0.960896 0.088669 11.00000 -1.50000 AFIX 0 C21 1 0.023210 0.782504 0.063842 11.00000 0.00721 0.02983 = 0.04581 0.00429 -0.00625 -0.00201 C22 1 -0.032382 0.846703 0.104342 11.00000 0.03006 0.03705 = 0.04024 0.00682 0.00862 -0.00361 AFIX 33 H22A 2 0.000743 0.808698 0.131865 11.00000 -1.50000 H22B 2 0.012445 0.921112 0.103836 11.00000 -1.50000 H22C 2 -0.146293 0.851824 0.103523 11.00000 -1.50000 AFIX 0 C23 1 -0.029603 0.843102 0.021048 11.00000 0.03161 0.03234 = 0.04950 0.00266 -0.00875 0.00416 AFIX 33 H23A 2 0.005796 0.802220 -0.005379 11.00000 -1.50000 H23B 2 -0.143524 0.848235 0.020451 11.00000 -1.50000 H23C 2 0.015215 0.917523 0.020764 11.00000 -1.50000 AFIX 0 C24 1 -0.066031 0.670844 0.065737 11.00000 0.03748 0.04161 = 0.05154 0.01646 -0.00521 0.00663 AFIX 33 H24A 2 -0.035469 0.624634 0.040263 11.00000 -1.50000 H24B 2 -0.040454 0.632738 0.093883 11.00000 -1.50000 H24C 2 -0.178396 0.684806 0.064259 11.00000 -1.50000 AFIX 0 N1 4 0.474496 0.696991 0.157917 11.00000 0.02428 0.01560 = 0.02743 0.00113 -0.00136 -0.01102 C25 1 0.576811 0.732047 0.176583 11.00000 0.01644 0.01228 = 0.02708 -0.00116 -0.00772 0.00227 C26 1 0.708388 0.775872 0.203018 11.00000 0.01786 0.04220 = 0.03103 0.00740 -0.00740 -0.00273 AFIX 137 H26A 2 0.716678 0.855688 0.198160 11.00000 -1.50000 H26B 2 0.804950 0.739899 0.193539 11.00000 -1.50000 H26C 2 0.691217 0.761234 0.234970 11.00000 -1.50000 AFIX 0 MOLE 2 B1 3 0.793111 0.081375 0.173782 11.00000 0.01424 0.03510 = 0.03265 -0.00292 0.01102 0.00106 F1 5 0.837251 0.178624 0.197190 11.00000 0.03131 0.03541 = 0.04347 -0.01429 0.00621 -0.00482 F2 5 0.805061 0.101909 0.128419 11.00000 0.08304 0.04515 = 0.03917 -0.00464 -0.01398 0.01348 F3 5 0.903009 -0.000826 0.185073 11.00000 0.05883 0.02535 = 0.04465 -0.00434 -0.00878 0.00819 F4 5 0.649797 0.050242 0.184398 11.00000 0.02772 0.05046 = 0.07458 -0.00217 0.00588 -0.00667 HKLF 4 REM tech11 in P2(1)/n REM R1 = 0.0863 for 5278 Fo > 4sig(Fo) and 0.1365 for all 7714 data REM 319 parameters refined using 18 restraints END WGHT 0.0047 94.8963 REM Highest difference peak 5.440, deepest hole -3.319, 1-sigma level 0.284 Q1 1 0.1798 0.6200 0.1223 11.00000 0.05 5.44 Q2 1 0.0376 0.6200 0.1197 11.00000 0.05 3.57 Q3 1 -0.2714 0.8778 0.1410 11.00000 0.05 2.98 Q4 1 -0.1388 0.8836 0.1419 11.00000 0.05 2.87 Q5 1 0.3033 0.6183 0.0982 11.00000 0.05 2.57 Q6 1 0.2992 0.6207 0.1421 11.00000 0.05 2.41 Q7 1 0.4179 0.6215 0.1155 11.00000 0.05 2.17 Q8 1 0.7619 0.3529 0.1380 11.00000 0.05 1.92 Q9 1 0.8591 0.0423 0.1015 11.00000 0.05 1.51 Q10 1 0.4372 0.7777 0.0710 11.00000 0.05 1.40 Q11 1 0.1261 0.1562 0.1195 11.00000 0.05 1.39 Q12 1 0.5924 0.8880 0.1607 11.00000 0.05 1.31 Q13 1 0.2382 0.1255 0.1260 11.00000 0.05 1.29 Q14 1 0.1889 1.0052 0.1644 11.00000 0.05 1.24 Q15 1 0.7604 0.1931 0.1072 11.00000 0.05 1.21 Q16 1 0.4043 0.6839 0.0992 11.00000 0.05 1.19 Q17 1 0.2337 0.5235 0.1223 11.00000 0.05 1.19 Q18 1 0.3965 0.5455 0.1014 11.00000 0.05 1.19 Q19 1 0.3616 0.1462 0.1090 11.00000 0.05 1.18 Q20 1 0.2786 0.5243 0.0960 11.00000 0.05 1.18 ; _shelx_res_checksum 94796 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.30129(9) 0.61890(4) 0.11968(2) 0.01715(17) Uani 1 1 d . . . . . H1 H 0.2093 0.5821 0.0875 0.021 Uiso 1 1 d . U . . . P1 P 0.2901(5) 0.4540(3) 0.16081(11) 0.0130(7) Uani 1 1 d . . . . . P2 P 0.2431(5) 0.7596(3) 0.06896(13) 0.0162(9) Uani 1 1 d . . . . . C1 C 0.179(2) 0.3455(12) 0.1280(5) 0.017(3) Uani 1 1 d . . . . . C2 C 0.182(2) 0.2281(13) 0.1475(5) 0.024(4) Uani 1 1 d . . . . . H2A H 0.1463 0.2298 0.1787 0.036 Uiso 1 1 calc R U . . . H2B H 0.1132 0.1802 0.1297 0.036 Uiso 1 1 calc R U . . . H2C H 0.2886 0.1992 0.1466 0.036 Uiso 1 1 calc R U . . . C3 C 0.236(2) 0.3378(15) 0.0790(5) 0.025(4) Uani 1 1 d . . . . . H3A H 0.2353 0.4115 0.0655 0.038 Uiso 1 1 calc R U . . . H3B H 0.3420 0.3080 0.0787 0.038 Uiso 1 1 calc R U . . . H3C H 0.1666 0.2890 0.0618 0.038 Uiso 1 1 calc R U . . . C4 C 0.003(2) 0.3780(16) 0.1243(6) 0.031(4) Uani 1 1 d . U . . . H4A H -0.0067 0.4527 0.1120 0.046 Uiso 1 1 calc R U . . . H4B H -0.0517 0.3258 0.1045 0.046 Uiso 1 1 calc R U . . . H4C H -0.0443 0.3758 0.1542 0.046 Uiso 1 1 calc R U . . . C5 C 0.483(2) 0.3888(14) 0.1766(5) 0.022(3) Uani 1 1 d . . . . . C6 C 0.553(2) 0.3309(16) 0.1353(6) 0.032(4) Uani 1 1 d . U . . . H6A H 0.4800 0.2753 0.1239 0.048 Uiso 1 1 calc R U . . . H6B H 0.5730 0.3857 0.1118 0.048 Uiso 1 1 calc R U . . . H6C H 0.6513 0.2951 0.1439 0.048 Uiso 1 1 calc R U . . . C7 C 0.609(2) 0.4739(14) 0.1910(6) 0.028(4) Uani 1 1 d . . . . . H7A H 0.5735 0.5148 0.2174 0.042 Uiso 1 1 calc R U . . . H7B H 0.7063 0.4350 0.1984 0.042 Uiso 1 1 calc R U . . . H7C H 0.6280 0.5256 0.1663 0.042 Uiso 1 1 calc R U . . . C8 C 0.474(2) 0.3021(14) 0.2155(5) 0.025(4) Uani 1 1 d . . . . . H8A H 0.4300 0.3369 0.2422 0.037 Uiso 1 1 calc R U . . . H8B H 0.4085 0.2401 0.2061 0.037 Uiso 1 1 calc R U . . . H8C H 0.5794 0.2751 0.2225 0.037 Uiso 1 1 calc R U . . . C9 C 0.180(2) 0.4895(12) 0.2136(5) 0.017(3) Uani 1 1 d . . . . . C10 C 0.110(2) 0.3914(16) 0.2383(5) 0.029(4) Uani 1 1 d . . . . . H10A H 0.1933 0.3392 0.2463 0.043 Uiso 1 1 calc R U . . . H10B H 0.0593 0.4172 0.2657 0.043 Uiso 1 1 calc R U . . . H10C H 0.0336 0.3546 0.2189 0.043 Uiso 1 1 calc R U . . . C11 C 0.288(2) 0.5499(13) 0.2472(5) 0.022(3) Uani 1 1 d . . . . . H11A H 0.3733 0.5008 0.2562 0.034 Uiso 1 1 calc R U . . . H11B H 0.3306 0.6162 0.2331 0.034 Uiso 1 1 calc R U . . . H11C H 0.2282 0.5710 0.2738 0.034 Uiso 1 1 calc R U . . . C12 C 0.052(2) 0.5695(15) 0.2013(6) 0.027(4) Uani 1 1 d . . . . . H12A H 0.0969 0.6327 0.1854 0.041 Uiso 1 1 calc R U . . . H12B H -0.0243 0.5326 0.1819 0.041 Uiso 1 1 calc R U . . . H12C H 0.0013 0.5953 0.2287 0.041 Uiso 1 1 calc R U . . . C13 C 0.318(2) 0.7132(13) 0.0124(5) 0.020(3) Uani 1 1 d . . . . . C14 C 0.216(3) 0.6200(16) -0.0071(5) 0.038(5) Uani 1 1 d . . . . . H14A H 0.2053 0.5611 0.0152 0.056 Uiso 1 1 calc R U . . . H14B H 0.1130 0.6493 -0.0149 0.056 Uiso 1 1 calc R U . . . H14C H 0.2653 0.5901 -0.0341 0.056 Uiso 1 1 calc R U . . . C15 C 0.332(3) 0.8031(16) -0.0237(5) 0.036(5) Uani 1 1 d . . . . . H15A H 0.3962 0.8638 -0.0122 0.054 Uiso 1 1 calc R U . . . H15B H 0.3800 0.7719 -0.0506 0.054 Uiso 1 1 calc R U . . . H15C H 0.2278 0.8311 -0.0314 0.054 Uiso 1 1 calc R U . . . C16 C 0.481(3) 0.6616(17) 0.0195(7) 0.040(5) Uani 1 1 d . . . . . H16A H 0.4751 0.6038 0.0425 0.060 Uiso 1 1 calc R U . . . H16B H 0.5169 0.6293 -0.0087 0.060 Uiso 1 1 calc R U . . . H16C H 0.5543 0.7188 0.0294 0.060 Uiso 1 1 calc R U . . . C17 C 0.330(2) 0.9003(14) 0.0842(5) 0.028(4) Uani 1 1 d . . . . . C18 C 0.303(3) 0.9246(14) 0.1342(5) 0.033(4) Uani 1 1 d . . . . . H18A H 0.3361 0.8607 0.1521 0.050 Uiso 1 1 calc R U . . . H18B H 0.3644 0.9894 0.1431 0.050 Uiso 1 1 calc R U . . . H18C H 0.1925 0.9390 0.1391 0.050 Uiso 1 1 calc R U . . . C19 C 0.281(2) 0.9976(14) 0.0558(5) 0.029(4) Uani 1 1 d . . . . . H19A H 0.2988 0.9809 0.0241 0.043 Uiso 1 1 calc R U . . . H19B H 0.1699 1.0123 0.0604 0.043 Uiso 1 1 calc R U . . . H19C H 0.3418 1.0628 0.0645 0.043 Uiso 1 1 calc R U . . . C20 C 0.510(2) 0.8922(17) 0.0783(6) 0.037(5) Uani 1 1 d . . . . . H20A H 0.5500 0.8301 0.0960 0.056 Uiso 1 1 calc R U . . . H20B H 0.5337 0.8806 0.0465 0.056 Uiso 1 1 calc R U . . . H20C H 0.5586 0.9609 0.0887 0.056 Uiso 1 1 calc R U . . . C21 C 0.023(2) 0.7825(16) 0.0638(7) 0.028(4) Uani 1 1 d . . . . . C22 C -0.032(2) 0.8467(17) 0.1043(6) 0.036(5) Uani 1 1 d . . . . . H22A H 0.0007 0.8087 0.1319 0.054 Uiso 1 1 calc R U . . . H22B H 0.0124 0.9211 0.1038 0.054 Uiso 1 1 calc R U . . . H22C H -0.1463 0.8518 0.1035 0.054 Uiso 1 1 calc R U . . . C23 C -0.030(2) 0.8431(17) 0.0210(7) 0.038(5) Uani 1 1 d . . . . . H23A H 0.0058 0.8022 -0.0054 0.057 Uiso 1 1 calc R U . . . H23B H -0.1435 0.8482 0.0205 0.057 Uiso 1 1 calc R U . . . H23C H 0.0152 0.9175 0.0208 0.057 Uiso 1 1 calc R U . . . C24 C -0.066(3) 0.6708(18) 0.0657(7) 0.044(5) Uani 1 1 d . . . . . H24A H -0.0355 0.6246 0.0403 0.065 Uiso 1 1 calc R U . . . H24B H -0.0405 0.6327 0.0939 0.065 Uiso 1 1 calc R U . . . H24C H -0.1784 0.6848 0.0643 0.065 Uiso 1 1 calc R U . . . N1 N 0.4745(18) 0.6970(11) 0.1579(5) 0.022(3) Uani 1 1 d . . . . . C25 C 0.577(2) 0.7320(13) 0.1766(5) 0.019(3) Uani 1 1 d . . . . . C26 C 0.708(2) 0.7759(16) 0.2030(5) 0.030(4) Uani 1 1 d . . . . . H26A H 0.7167 0.8557 0.1982 0.046 Uiso 1 1 calc R U . . . H26B H 0.8049 0.7399 0.1935 0.046 Uiso 1 1 calc R U . . . H26C H 0.6912 0.7612 0.2350 0.046 Uiso 1 1 calc R U . . . B1 B 0.793(3) 0.0814(17) 0.1738(7) 0.027(4) Uani 1 1 d . . . . . F1 F 0.8373(13) 0.1786(9) 0.1972(4) 0.037(3) Uani 1 1 d . . . . . F2 F 0.805(2) 0.1019(9) 0.1284(3) 0.056(3) Uani 1 1 d . . . . . F3 F 0.9030(15) -0.0008(9) 0.1851(4) 0.043(3) Uani 1 1 d . . . . . F4 F 0.6498(14) 0.0502(11) 0.1844(5) 0.051(3) Uani 1 1 d . U . . . 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 0.0264(3) 0.0125(2) 0.0126(2) 0.0013(3) 0.0003(2) -0.0005(4) P1 0.015(2) 0.0109(17) 0.0135(16) 0.0005(13) 0.0010(16) 0.0007(18) P2 0.023(2) 0.014(2) 0.0121(17) 0.0006(15) 0.0013(15) 0.0010(16) C1 0.023(9) 0.011(6) 0.017(7) -0.004(5) 0.003(6) -0.003(6) C2 0.030(10) 0.022(8) 0.020(7) 0.000(6) -0.004(8) -0.006(8) C3 0.023(10) 0.035(10) 0.017(7) -0.006(7) -0.002(6) -0.003(8) C4 0.037(7) 0.025(7) 0.031(7) -0.001(7) -0.003(6) -0.012(7) C5 0.033(10) 0.014(8) 0.018(7) 0.000(7) 0.003(6) -0.006(8) C6 0.042(8) 0.025(7) 0.030(7) -0.004(6) 0.008(6) 0.009(7) C7 0.040(12) 0.016(9) 0.029(9) -0.002(7) -0.007(8) 0.008(8) C8 0.040(12) 0.016(8) 0.018(8) 0.001(7) -0.012(7) 0.000(8) C9 0.018(9) 0.014(7) 0.018(7) 0.001(6) 0.006(6) 0.001(7) C10 0.038(11) 0.030(10) 0.019(8) -0.007(7) 0.011(7) -0.014(9) C11 0.030(10) 0.025(9) 0.012(6) -0.005(6) -0.003(7) 0.003(9) C12 0.038(12) 0.022(9) 0.022(8) 0.008(7) 0.012(8) 0.010(8) C13 0.022(9) 0.024(8) 0.015(7) 0.002(6) 0.005(7) 0.003(8) C14 0.053(13) 0.031(9) 0.028(8) -0.008(8) -0.006(9) 0.016(12) C15 0.057(16) 0.033(10) 0.019(8) -0.001(7) 0.002(9) -0.008(10) C16 0.043(13) 0.033(11) 0.044(12) -0.002(9) 0.019(10) 0.012(10) C17 0.045(13) 0.028(10) 0.010(7) -0.002(6) -0.006(7) -0.004(9) C18 0.065(13) 0.025(9) 0.011(7) -0.004(6) -0.011(9) 0.001(11) C19 0.031(11) 0.026(9) 0.029(8) 0.001(7) 0.020(8) 0.005(9) C20 0.041(12) 0.034(12) 0.036(10) 0.009(9) 0.001(9) -0.013(10) C21 0.007(9) 0.030(10) 0.046(11) 0.004(9) -0.006(8) -0.002(8) C22 0.030(11) 0.037(12) 0.040(11) 0.007(9) 0.009(8) -0.004(9) C23 0.032(12) 0.032(11) 0.049(12) 0.003(9) -0.009(9) 0.004(9) C24 0.037(13) 0.042(13) 0.052(13) 0.016(10) -0.005(10) 0.007(11) N1 0.024(8) 0.016(7) 0.027(7) 0.001(6) -0.001(6) -0.011(6) C25 0.016(9) 0.012(8) 0.027(8) -0.001(7) -0.008(7) 0.002(7) C26 0.018(9) 0.042(11) 0.031(9) 0.007(8) -0.007(8) -0.003(10) B1 0.014(10) 0.035(11) 0.033(10) -0.003(8) 0.011(9) 0.001(10) F1 0.031(7) 0.035(6) 0.043(6) -0.014(5) 0.006(5) -0.005(5) F2 0.083(9) 0.045(7) 0.039(7) -0.005(5) -0.014(8) 0.013(8) F3 0.059(8) 0.025(6) 0.045(7) -0.004(5) -0.009(6) 0.008(6) F4 0.028(6) 0.050(7) 0.075(7) -0.002(6) 0.006(5) -0.007(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 P2 99.8(4) . . ? N1 Pt1 P1 97.6(4) . . ? P2 Pt1 P1 162.25(15) . . ? N1 Pt1 H1 166.0 . . ? P2 Pt1 H1 69.6 . . ? P1 Pt1 H1 93.7 . . ? C9 P1 C5 109.4(7) . . ? C9 P1 C1 109.4(7) . . ? C5 P1 C1 106.1(7) . . ? C9 P1 Pt1 105.2(5) . . ? C5 P1 Pt1 116.5(5) . . ? C1 P1 Pt1 110.1(5) . . ? C13 P2 C21 108.3(8) . . ? C13 P2 C17 109.8(7) . . ? C21 P2 C17 105.9(9) . . ? C13 P2 Pt1 106.7(5) . . ? C21 P2 Pt1 111.4(6) . . ? C17 P2 Pt1 114.6(5) . . ? C2 C1 C3 107.2(12) . . ? C2 C1 C4 105.9(14) . . ? C3 C1 C4 105.3(13) . . ? C2 C1 P1 116.1(10) . . ? C3 C1 P1 111.5(11) . . ? C4 C1 P1 110.2(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 104.2(14) . . ? C6 C5 C8 107.8(14) . . ? C7 C5 C8 106.0(13) . . ? C6 C5 P1 109.8(12) . . ? C7 C5 P1 113.6(12) . . ? C8 C5 P1 114.7(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C10 109.4(15) . . ? C12 C9 C11 106.5(13) . . ? C10 C9 C11 106.9(12) . . ? C12 C9 P1 108.3(10) . . ? C10 C9 P1 115.2(11) . . ? C11 C9 P1 110.3(11) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 107.6(13) . . ? C15 C13 C16 108.0(16) . . ? C14 C13 C16 105.5(15) . . ? C15 C13 P2 116.2(12) . . ? C14 C13 P2 110.9(12) . . ? C16 C13 P2 108.1(11) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.5(14) . . ? C19 C17 C20 105.1(15) . . ? C18 C17 C20 106.2(16) . . ? C19 C17 P2 117.0(12) . . ? C18 C17 P2 109.7(12) . . ? C20 C17 P2 107.7(13) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 108.8(16) . . ? C22 C21 C24 105.0(16) . . ? C23 C21 C24 107.7(16) . . ? C22 C21 P2 109.2(13) . . ? C23 C21 P2 114.8(14) . . ? C24 C21 P2 110.9(13) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 N1 Pt1 173.4(15) . . ? N1 C25 C26 177.4(19) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F4 B1 F2 111.2(19) . . ? F4 B1 F3 111.2(17) . . ? F2 B1 F3 107.8(15) . . ? F4 B1 F1 111.3(16) . . ? F2 B1 F1 108.1(15) . . ? F3 B1 F1 107.1(17) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.091(14) . ? Pt1 P2 2.328(4) . ? Pt1 P1 2.345(4) . ? Pt1 H1 1.3145 . ? P1 C9 1.889(15) . ? P1 C5 1.889(18) . ? P1 C1 1.892(15) . ? P2 C13 1.893(15) . ? P2 C21 1.913(18) . ? P2 C17 1.916(18) . ? C1 C2 1.54(2) . ? C1 C3 1.54(2) . ? C1 C4 1.57(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.54(2) . ? C5 C7 1.56(2) . ? C5 C8 1.57(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.50(2) . ? C9 C10 1.52(2) . ? C9 C11 1.54(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.54(2) . ? C13 C14 1.54(3) . ? C13 C16 1.54(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.51(2) . ? C17 C18 1.54(2) . ? C17 C20 1.55(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.52(3) . ? C21 C23 1.54(3) . ? C21 C24 1.56(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N1 C25 1.12(2) . ? C25 C26 1.47(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? B1 F4 1.33(2) . ? B1 F2 1.38(2) . ? B1 F3 1.41(2) . ? B1 F1 1.42(2) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 P1 C1 C2 -73.4(14) . . . . ? C5 P1 C1 C2 44.5(14) . . . . ? Pt1 P1 C1 C2 171.4(11) . . . . ? C9 P1 C1 C3 163.5(11) . . . . ? C5 P1 C1 C3 -78.6(12) . . . . ? Pt1 P1 C1 C3 48.2(12) . . . . ? C9 P1 C1 C4 46.9(12) . . . . ? C5 P1 C1 C4 164.8(11) . . . . ? Pt1 P1 C1 C4 -68.3(11) . . . . ? C9 P1 C5 C6 164.5(12) . . . . ? C1 P1 C5 C6 46.6(13) . . . . ? Pt1 P1 C5 C6 -76.4(12) . . . . ? C9 P1 C5 C7 -79.3(13) . . . . ? C1 P1 C5 C7 162.8(11) . . . . ? Pt1 P1 C5 C7 39.8(13) . . . . ? C9 P1 C5 C8 42.9(13) . . . . ? C1 P1 C5 C8 -75.1(12) . . . . ? Pt1 P1 C5 C8 162.0(9) . . . . ? C5 P1 C9 C12 163.6(12) . . . . ? C1 P1 C9 C12 -80.6(13) . . . . ? Pt1 P1 C9 C12 37.8(12) . . . . ? C5 P1 C9 C10 -73.6(14) . . . . ? C1 P1 C9 C10 42.2(15) . . . . ? Pt1 P1 C9 C10 160.5(12) . . . . ? C5 P1 C9 C11 47.5(12) . . . . ? C1 P1 C9 C11 163.3(10) . . . . ? Pt1 P1 C9 C11 -78.4(10) . . . . ? C21 P2 C13 C15 75.3(16) . . . . ? C17 P2 C13 C15 -40.0(17) . . . . ? Pt1 P2 C13 C15 -164.7(13) . . . . ? C21 P2 C13 C14 -48.0(14) . . . . ? C17 P2 C13 C14 -163.2(12) . . . . ? Pt1 P2 C13 C14 72.0(12) . . . . ? C21 P2 C13 C16 -163.2(13) . . . . ? C17 P2 C13 C16 81.6(13) . . . . ? Pt1 P2 C13 C16 -43.1(13) . . . . ?