#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:09:07 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296019 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573221.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_1573221 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 'C24 H57 O P2 Pt, B F4' _chemical_formula_sum 'C24 H57 B F4 O P2 Pt' _chemical_formula_weight 705.53 _chemical_name_systematic 'Pt-H_PtBu3_2-H2O [BF3]' _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_block_doi 10.5517/ccdc.csd.cc2jjppg _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 106.800(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.5231(4) _cell_length_b 16.5896(4) _cell_length_c 16.5713(5) _cell_measurement_reflns_used 5080 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.319 _cell_measurement_theta_min 1.776 _cell_volume 3032.63(16) _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 0.999 _diffrn_measured_fraction_theta_max 0.998 _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 0.0787 _diffrn_reflns_av_unetI/netI 0.0962 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 28688 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.319 _diffrn_reflns_theta_min 1.776 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.772 _exptl_absorpt_correction_T_max 0.8595 _exptl_absorpt_correction_T_min 0.7542 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS, Bruker 2008' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.545 _exptl_crystal_description prism _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.143 _exptl_crystal_size_mid 0.099 _exptl_crystal_size_min 0.074 _refine_diff_density_max 1.218 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.188 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 328 _refine_ls_number_reflns 7528 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0125P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.0611 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5080 _reflns_number_total 7528 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06450j2.cif _cod_data_source_block Pt-H-PtBu3_2-H2O-BF4 _cod_original_cell_volume 3032.62(16) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1573221 _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 0.549 _shelx_estimated_absorpt_t_max 0.719 _shelx_res_file ; tech12a.res created by SHELXL-2014/7 TITL tech12a in P2(1)/c CELL 0.71073 11.5231 16.5896 16.5713 90.000 106.800 90.000 ZERR 4.00 0.0004 0.0004 0.0005 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B O F P PT UNIT 96 228 4 4 16 8 4 TEMP -123.150 SIZE 0.074 0.099 0.143 REM Tmax: 0.8595 Tmin: 0.7542 (numerical) REM prism, colourless OMIT -3 57 L.S. 14 BOND $H CONF ACTA WPDB -1 FMAP 2 PLAN 60 DFIX 2.00 0.03 H18C H22B REM EXTI 0.000067 ISOR 0.006 C23 WGHT 0.012500 FVAR 0.08227 MOLE 1 PT1 7 0.236172 0.433614 0.270347 11.00000 0.01236 0.01347 = 0.01483 0.00020 0.00402 -0.00188 H1 2 0.167263 0.410116 0.187017 11.00000 0.05315 P1 6 0.084233 0.364152 0.308558 11.00000 0.01231 0.01737 = 0.01630 0.00330 0.00270 -0.00199 P2 6 0.360162 0.488690 0.195511 11.00000 0.01331 0.01481 = 0.01656 -0.00012 0.00572 -0.00097 O1 4 0.326404 0.471337 0.400627 11.00000 0.02222 0.03318 = 0.01781 -0.00520 -0.00069 -0.00388 H1A 2 0.393718 0.443054 0.423608 11.00000 0.06558 H1B 2 0.323409 0.523670 0.419508 11.00000 0.09241 C1 1 0.150792 0.299679 0.406545 11.00000 0.01801 0.02106 = 0.02588 0.01325 0.00462 -0.00014 C2 1 0.067415 0.231875 0.420738 11.00000 0.03702 0.03874 = 0.03194 0.01933 0.00313 -0.01113 AFIX 137 H2A 2 0.048951 0.194751 0.372698 11.00000 -1.50000 H2B 2 -0.008059 0.255304 0.426134 11.00000 -1.50000 H2C 2 0.108326 0.202447 0.472408 11.00000 -1.50000 AFIX 0 C3 1 0.269850 0.262887 0.399522 11.00000 0.02906 0.02251 = 0.03936 0.00966 0.00159 0.00255 AFIX 137 H3A 2 0.307795 0.231373 0.450321 11.00000 -1.50000 H3B 2 0.324864 0.306132 0.393786 11.00000 -1.50000 H3C 2 0.252833 0.227690 0.349978 11.00000 -1.50000 AFIX 0 C4 1 0.184377 0.350970 0.487123 11.00000 0.03438 0.03380 = 0.01889 0.01333 0.00017 -0.00846 AFIX 137 H4A 2 0.223996 0.316901 0.535564 11.00000 -1.50000 H4B 2 0.110753 0.374643 0.495427 11.00000 -1.50000 H4C 2 0.239816 0.394100 0.481801 11.00000 -1.50000 AFIX 0 C5 1 -0.027518 0.439573 0.330149 11.00000 0.01577 0.02600 = 0.03461 0.00254 0.01177 0.00453 C6 1 -0.104475 0.475951 0.247350 11.00000 0.01753 0.03509 = 0.05657 0.01509 0.00475 0.01176 AFIX 137 H6A 2 -0.159273 0.434729 0.214803 11.00000 -1.50000 H6B 2 -0.051460 0.495534 0.214790 11.00000 -1.50000 H6C 2 -0.152102 0.520947 0.259297 11.00000 -1.50000 AFIX 0 C7 1 -0.113853 0.405224 0.378262 11.00000 0.01778 0.05717 = 0.04280 -0.00007 0.01484 0.00192 AFIX 137 H7A 2 -0.166436 0.448369 0.387854 11.00000 -1.50000 H7B 2 -0.065911 0.383270 0.432572 11.00000 -1.50000 H7C 2 -0.163728 0.362341 0.344741 11.00000 -1.50000 AFIX 0 C8 1 0.045056 0.509373 0.382214 11.00000 0.03099 0.02577 = 0.05267 -0.00886 0.01845 0.00467 AFIX 137 H8A 2 0.096940 0.533813 0.351341 11.00000 -1.50000 H8B 2 0.095510 0.488731 0.436426 11.00000 -1.50000 H8C 2 -0.011059 0.550031 0.392037 11.00000 -1.50000 AFIX 0 C9 1 -0.001434 0.293091 0.219760 11.00000 0.02860 0.02327 = 0.02108 -0.00307 0.00129 -0.01694 C10 1 0.078083 0.222009 0.213143 11.00000 0.04994 0.02930 = 0.03604 -0.01485 0.01320 -0.01369 AFIX 137 H10A 2 0.086754 0.186172 0.261542 11.00000 -1.50000 H10B 2 0.158156 0.241539 0.212689 11.00000 -1.50000 H10C 2 0.040718 0.192386 0.160920 11.00000 -1.50000 AFIX 0 C11 1 -0.123908 0.262395 0.229437 11.00000 0.03080 0.03708 = 0.03461 -0.00003 0.00151 -0.02224 AFIX 137 H11A 2 -0.157486 0.221328 0.186530 11.00000 -1.50000 H11B 2 -0.180823 0.307553 0.222258 11.00000 -1.50000 H11C 2 -0.110769 0.238918 0.285636 11.00000 -1.50000 AFIX 0 C12 1 -0.031417 0.335023 0.132758 11.00000 0.04672 0.04848 = 0.01996 -0.00194 0.00066 -0.02524 AFIX 137 H12A 2 0.043644 0.344264 0.117594 11.00000 -1.50000 H12B 2 -0.071188 0.386765 0.135413 11.00000 -1.50000 H12C 2 -0.085699 0.300601 0.090160 11.00000 -1.50000 AFIX 0 C13 1 0.257097 0.534060 0.093750 11.00000 0.02293 0.01827 = 0.02283 0.00403 0.01201 0.00570 C14 1 0.188710 0.468492 0.033528 11.00000 0.03986 0.04304 = 0.03174 0.01343 -0.00823 -0.00476 AFIX 137 H14A 2 0.120566 0.492789 -0.009287 11.00000 -1.50000 H14B 2 0.158081 0.428039 0.065340 11.00000 -1.50000 H14C 2 0.243722 0.442691 0.005996 11.00000 -1.50000 AFIX 0 C15 1 0.157614 0.582459 0.115596 11.00000 0.04498 0.06329 = 0.03898 0.00525 0.00451 0.03245 AFIX 137 H15A 2 0.193756 0.628659 0.150776 11.00000 -1.50000 H15B 2 0.115836 0.548078 0.146433 11.00000 -1.50000 H15C 2 0.099377 0.601712 0.063606 11.00000 -1.50000 AFIX 0 C16 1 0.319612 0.586484 0.044488 11.00000 0.03726 0.06028 = 0.04529 0.03493 -0.00033 -0.00287 AFIX 137 H16A 2 0.387094 0.556622 0.033849 11.00000 -1.50000 H16B 2 0.350657 0.635220 0.076990 11.00000 -1.50000 H16C 2 0.261644 0.601620 -0.009337 11.00000 -1.50000 AFIX 0 C17 1 0.450390 0.403331 0.167427 11.00000 0.01563 0.01429 = 0.03234 0.00375 0.00854 0.00808 C18 1 0.549536 0.376582 0.243711 11.00000 0.05957 0.04010 = 0.06911 -0.00685 -0.00286 0.02495 AFIX 137 H18A 2 0.581444 0.324435 0.232212 11.00000 -1.50000 H18B 2 0.516847 0.371285 0.291874 11.00000 -1.50000 H18C 2 0.614872 0.416608 0.256716 11.00000 -1.50000 AFIX 0 C19 1 0.506273 0.421090 0.096078 11.00000 0.08901 0.04131 = 0.09306 0.01957 0.07685 0.02955 AFIX 137 H19A 2 0.561699 0.467038 0.111709 11.00000 -1.50000 H19B 2 0.441798 0.433928 0.044519 11.00000 -1.50000 H19C 2 0.551127 0.373683 0.086293 11.00000 -1.50000 AFIX 0 C20 1 0.370102 0.328616 0.141305 11.00000 0.03055 0.03591 = 0.07144 -0.02901 0.00251 0.01100 AFIX 137 H20A 2 0.416499 0.285763 0.124115 11.00000 -1.50000 H20B 2 0.299356 0.342292 0.094042 11.00000 -1.50000 H20C 2 0.343106 0.310008 0.189053 11.00000 -1.50000 AFIX 0 C21 1 0.469558 0.571246 0.250885 11.00000 0.01997 0.02963 = 0.03147 -0.00476 0.01095 -0.01527 C22 1 0.543043 0.543615 0.337806 11.00000 0.03648 0.05004 = 0.03722 -0.00969 -0.00649 -0.01990 AFIX 137 H22A 2 0.596205 0.587467 0.366315 11.00000 -1.50000 H22B 2 0.592293 0.496850 0.332515 11.00000 -1.50000 H22C 2 0.488149 0.528660 0.370795 11.00000 -1.50000 AFIX 0 C23 1 0.393811 0.643638 0.264141 11.00000 0.03858 0.02187 = 0.09201 -0.03066 0.00382 -0.00571 AFIX 137 H23A 2 0.328085 0.624704 0.285912 11.00000 -1.50000 H23B 2 0.359408 0.671352 0.210289 11.00000 -1.50000 H23C 2 0.445654 0.681009 0.304672 11.00000 -1.50000 AFIX 0 C24 1 0.563009 0.598733 0.206624 11.00000 0.05008 0.06585 = 0.05204 -0.00664 0.02289 -0.04008 AFIX 137 H24A 2 0.520754 0.620030 0.150681 11.00000 -1.50000 H24B 2 0.613393 0.552774 0.200764 11.00000 -1.50000 H24C 2 0.614469 0.640922 0.240205 11.00000 -1.50000 AFIX 0 MOLE 2 B1 3 0.373772 0.668228 0.498132 11.00000 0.03863 0.02258 = 0.02973 0.00211 0.00008 -0.00132 F2 5 0.283474 0.626634 0.439811 11.00000 0.03809 0.04381 = 0.07164 -0.01259 -0.01239 -0.00946 F3 5 0.331362 0.696385 0.561401 11.00000 0.11063 0.05566 = 0.06006 -0.00705 0.04923 -0.00325 F4 5 0.415476 0.729060 0.460357 11.00000 0.09554 0.03751 = 0.05846 0.00707 0.02732 -0.02128 F5 5 0.466376 0.612872 0.530180 11.00000 0.04714 0.05297 = 0.06743 0.00684 -0.00796 0.01586 HKLF 4 REM tech12a in P2(1)/c REM R1 = 0.0412 for 5080 Fo > 4sig(Fo) and 0.0839 for all 7528 data REM 328 parameters refined using 7 restraints END WGHT 0.0173 0.0000 REM Highest difference peak 1.218, deepest hole -1.158, 1-sigma level 0.188 Q1 1 0.5800 0.4359 0.1552 11.00000 0.05 1.22 Q2 1 0.3292 0.5351 0.0195 11.00000 0.05 0.91 Q3 1 0.1418 0.4865 0.0768 11.00000 0.05 0.87 Q4 1 0.2222 0.6164 0.1039 11.00000 0.05 0.84 Q5 1 0.4790 0.3474 0.2457 11.00000 0.05 0.81 Q6 1 0.3830 0.3594 0.0981 11.00000 0.05 0.75 Q7 1 0.2799 0.3376 0.1354 11.00000 0.05 0.73 Q8 1 -0.1312 0.1889 0.2565 11.00000 0.05 0.72 Q9 1 -0.0196 0.3086 0.1768 11.00000 0.05 0.70 Q10 1 0.3942 0.3253 0.1611 11.00000 0.05 0.69 Q11 1 0.2183 0.5037 0.3143 11.00000 0.05 0.69 Q12 1 0.0569 0.5901 0.2208 11.00000 0.05 0.69 Q13 1 0.0360 0.4351 0.3782 11.00000 0.05 0.67 Q14 1 0.3156 0.1770 0.5070 11.00000 0.05 0.67 Q15 1 0.5029 0.6357 0.2034 11.00000 0.05 0.67 Q16 1 0.4840 0.5572 0.2951 11.00000 0.05 0.65 Q17 1 0.6329 0.2742 0.3216 11.00000 0.05 0.65 Q18 1 0.6565 0.6347 0.1456 11.00000 0.05 0.65 Q19 1 0.6172 0.3263 0.3438 11.00000 0.05 0.64 Q20 1 0.4059 0.4382 0.5154 11.00000 0.05 0.64 Q21 1 0.4346 0.2483 0.2379 11.00000 0.05 0.64 Q22 1 0.6567 0.5358 0.1563 11.00000 0.05 0.64 Q23 1 0.4030 0.3133 0.2761 11.00000 0.05 0.64 Q24 1 0.4408 0.6776 0.4594 11.00000 0.05 0.64 Q25 1 0.2784 0.2720 0.3385 11.00000 0.05 0.63 Q26 1 0.3205 0.6277 0.3605 11.00000 0.05 0.63 Q27 1 0.7181 0.6599 0.2422 11.00000 0.05 0.63 Q28 1 0.2815 0.6572 0.1994 11.00000 0.05 0.63 Q29 1 0.4967 0.3731 0.3567 11.00000 0.05 0.62 Q30 1 0.3659 0.5778 0.3368 11.00000 0.05 0.62 Q31 1 0.1132 0.4540 0.2763 11.00000 0.05 0.62 Q32 1 -0.1999 0.2799 0.2221 11.00000 0.05 0.62 Q33 1 -0.2216 0.5653 0.2402 11.00000 0.05 0.62 Q34 1 0.3244 0.7146 0.1018 11.00000 0.05 0.60 Q35 1 0.2566 0.2521 0.1190 11.00000 0.05 0.60 Q36 1 -0.0998 0.2359 0.3804 11.00000 0.05 0.60 Q37 1 0.5038 0.4769 0.3809 11.00000 0.05 0.60 Q38 1 0.1414 0.5054 0.2581 11.00000 0.05 0.60 Q39 1 -0.0780 0.1887 0.2258 11.00000 0.05 0.60 Q40 1 0.2703 0.5546 0.0691 11.00000 0.05 0.60 Q41 1 -0.0878 0.3772 0.0572 11.00000 0.05 0.59 Q42 1 0.2603 0.1839 0.3044 11.00000 0.05 0.59 Q43 1 0.0129 0.2850 0.0795 11.00000 0.05 0.59 Q44 1 0.1603 0.5144 0.3543 11.00000 0.05 0.58 Q45 1 0.6454 0.3826 0.1438 11.00000 0.05 0.58 Q46 1 0.2501 0.5208 0.2601 11.00000 0.05 0.58 Q47 1 -0.1964 0.4974 0.2392 11.00000 0.05 0.58 Q48 1 -0.0114 0.2986 0.0171 11.00000 0.05 0.58 Q49 1 0.3390 0.3664 0.0487 11.00000 0.05 0.58 Q50 1 0.3655 0.3787 0.5382 11.00000 0.05 0.57 Q51 1 0.2462 0.3779 0.1851 11.00000 0.05 0.57 Q52 1 0.5000 0.5000 0.5000 10.50000 0.05 0.57 Q53 1 0.4033 0.6305 0.3176 11.00000 0.05 0.57 Q54 1 0.3799 0.6491 0.3215 11.00000 0.05 0.57 Q55 1 0.7021 0.4270 0.1384 11.00000 0.05 0.57 Q56 1 0.4674 0.6932 0.5175 11.00000 0.05 0.57 Q57 1 0.2620 0.1470 0.4649 11.00000 0.05 0.57 Q58 1 0.4232 0.6844 0.1191 11.00000 0.05 0.57 Q59 1 0.5158 0.5969 0.5744 11.00000 0.05 0.56 Q60 1 0.1647 0.3672 0.5970 11.00000 0.05 0.56 ; _shelx_res_checksum 130 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 0.23617(2) 0.43361(2) 0.27035(2) 0.01353(5) Uani 1 1 d . . . . . H1 H 0.167(5) 0.410(3) 0.187(3) 0.053(17) Uiso 1 1 d . . . . . P1 P 0.08423(12) 0.36415(7) 0.30856(8) 0.0156(3) Uani 1 1 d . . . . . P2 P 0.36016(12) 0.48869(7) 0.19551(8) 0.0146(3) Uani 1 1 d . . . . . O1 O 0.3264(4) 0.4713(3) 0.4006(2) 0.0258(9) Uani 1 1 d . . . . . H1A H 0.394(6) 0.443(4) 0.424(4) 0.07(2) Uiso 1 1 d . . . . . H1B H 0.323(6) 0.524(4) 0.420(4) 0.09(3) Uiso 1 1 d . . . . . C1 C 0.1508(5) 0.2997(3) 0.4065(3) 0.0220(12) Uani 1 1 d . . . . . C2 C 0.0674(5) 0.2319(3) 0.4207(3) 0.0373(16) Uani 1 1 d . . . . . H2A H 0.0490 0.1948 0.3727 0.056 Uiso 1 1 calc R U . . . H2B H -0.0081 0.2553 0.4261 0.056 Uiso 1 1 calc R U . . . H2C H 0.1083 0.2024 0.4724 0.056 Uiso 1 1 calc R U . . . C3 C 0.2699(5) 0.2629(3) 0.3995(3) 0.0321(15) Uani 1 1 d . . . . . H3A H 0.3078 0.2314 0.4503 0.048 Uiso 1 1 calc R U . . . H3B H 0.3249 0.3061 0.3938 0.048 Uiso 1 1 calc R U . . . H3C H 0.2528 0.2277 0.3500 0.048 Uiso 1 1 calc R U . . . C4 C 0.1844(5) 0.3510(3) 0.4871(3) 0.0306(14) Uani 1 1 d . . . . . H4A H 0.2240 0.3169 0.5356 0.046 Uiso 1 1 calc R U . . . H4B H 0.1108 0.3746 0.4954 0.046 Uiso 1 1 calc R U . . . H4C H 0.2398 0.3941 0.4818 0.046 Uiso 1 1 calc R U . . . C5 C -0.0275(4) 0.4396(3) 0.3301(3) 0.0245(12) Uani 1 1 d . . . . . C6 C -0.1045(5) 0.4760(3) 0.2473(4) 0.0376(16) Uani 1 1 d . . . . . H6A H -0.1593 0.4347 0.2148 0.056 Uiso 1 1 calc R U . . . H6B H -0.0515 0.4955 0.2148 0.056 Uiso 1 1 calc R U . . . H6C H -0.1521 0.5209 0.2593 0.056 Uiso 1 1 calc R U . . . C7 C -0.1139(5) 0.4052(3) 0.3783(4) 0.0380(16) Uani 1 1 d . . . . . H7A H -0.1664 0.4484 0.3879 0.057 Uiso 1 1 calc R U . . . H7B H -0.0659 0.3833 0.4326 0.057 Uiso 1 1 calc R U . . . H7C H -0.1637 0.3623 0.3447 0.057 Uiso 1 1 calc R U . . . C8 C 0.0451(5) 0.5094(3) 0.3822(4) 0.0351(15) Uani 1 1 d . . . . . H8A H 0.0969 0.5338 0.3513 0.053 Uiso 1 1 calc R U . . . H8B H 0.0955 0.4887 0.4364 0.053 Uiso 1 1 calc R U . . . H8C H -0.0111 0.5500 0.3920 0.053 Uiso 1 1 calc R U . . . C9 C -0.0014(5) 0.2931(3) 0.2198(3) 0.0256(13) Uani 1 1 d . . . . . C10 C 0.0781(5) 0.2220(3) 0.2131(3) 0.0383(16) Uani 1 1 d . . . . . H10A H 0.0868 0.1862 0.2615 0.057 Uiso 1 1 calc R U . . . H10B H 0.1582 0.2415 0.2127 0.057 Uiso 1 1 calc R U . . . H10C H 0.0407 0.1924 0.1609 0.057 Uiso 1 1 calc R U . . . C11 C -0.1239(5) 0.2624(3) 0.2294(3) 0.0358(15) Uani 1 1 d . . . . . H11A H -0.1575 0.2213 0.1865 0.054 Uiso 1 1 calc R U . . . H11B H -0.1808 0.3076 0.2223 0.054 Uiso 1 1 calc R U . . . H11C H -0.1108 0.2389 0.2856 0.054 Uiso 1 1 calc R U . . . C12 C -0.0314(5) 0.3350(3) 0.1328(3) 0.0403(16) Uani 1 1 d . . . . . H12A H 0.0436 0.3443 0.1176 0.060 Uiso 1 1 calc R U . . . H12B H -0.0712 0.3868 0.1354 0.060 Uiso 1 1 calc R U . . . H12C H -0.0857 0.3006 0.0902 0.060 Uiso 1 1 calc R U . . . C13 C 0.2571(5) 0.5341(3) 0.0938(3) 0.0202(12) Uani 1 1 d . . . . . C14 C 0.1887(5) 0.4685(3) 0.0335(3) 0.0421(17) Uani 1 1 d . . . . . H14A H 0.1206 0.4928 -0.0093 0.063 Uiso 1 1 calc R U . . . H14B H 0.1581 0.4280 0.0653 0.063 Uiso 1 1 calc R U . . . H14C H 0.2437 0.4427 0.0060 0.063 Uiso 1 1 calc R U . . . C15 C 0.1576(6) 0.5825(3) 0.1156(4) 0.0507(19) Uani 1 1 d . . . . . H15A H 0.1938 0.6287 0.1508 0.076 Uiso 1 1 calc R U . . . H15B H 0.1158 0.5481 0.1464 0.076 Uiso 1 1 calc R U . . . H15C H 0.0994 0.6017 0.0636 0.076 Uiso 1 1 calc R U . . . C16 C 0.3196(5) 0.5865(3) 0.0445(4) 0.0502(19) Uani 1 1 d . . . . . H16A H 0.3871 0.5566 0.0338 0.075 Uiso 1 1 calc R U . . . H16B H 0.3507 0.6352 0.0770 0.075 Uiso 1 1 calc R U . . . H16C H 0.2616 0.6016 -0.0093 0.075 Uiso 1 1 calc R U . . . C17 C 0.4504(5) 0.4033(3) 0.1674(3) 0.0204(12) Uani 1 1 d . . . . . C18 C 0.5495(6) 0.3766(3) 0.2437(4) 0.061(2) Uani 1 1 d . . . . . H18A H 0.5814 0.3244 0.2322 0.091 Uiso 1 1 calc R U . . . H18B H 0.5168 0.3713 0.2919 0.091 Uiso 1 1 calc R U . . . H18C H 0.6149 0.4166 0.2567 0.091 Uiso 1 1 calc DR U . . . C19 C 0.5063(6) 0.4211(3) 0.0961(4) 0.064(2) Uani 1 1 d . . . . . H19A H 0.5617 0.4670 0.1117 0.096 Uiso 1 1 calc R U . . . H19B H 0.4418 0.4339 0.0445 0.096 Uiso 1 1 calc R U . . . H19C H 0.5511 0.3737 0.0863 0.096 Uiso 1 1 calc R U . . . C20 C 0.3701(5) 0.3286(3) 0.1413(4) 0.0485(19) Uani 1 1 d . . . . . H20A H 0.4165 0.2858 0.1241 0.073 Uiso 1 1 calc R U . . . H20B H 0.2994 0.3423 0.0940 0.073 Uiso 1 1 calc R U . . . H20C H 0.3431 0.3100 0.1891 0.073 Uiso 1 1 calc R U . . . C21 C 0.4696(4) 0.5712(3) 0.2509(3) 0.0263(12) Uani 1 1 d . . . . . C22 C 0.5430(5) 0.5436(3) 0.3378(3) 0.0448(17) Uani 1 1 d . . . . . H22A H 0.5962 0.5875 0.3663 0.067 Uiso 1 1 calc R U . . . H22B H 0.5923 0.4968 0.3325 0.067 Uiso 1 1 calc DR U . . . H22C H 0.4881 0.5287 0.3708 0.067 Uiso 1 1 calc R U . . . C23 C 0.3938(6) 0.6436(3) 0.2641(4) 0.054(2) Uani 1 1 d . U . . . H23A H 0.3281 0.6247 0.2859 0.081 Uiso 1 1 calc R U . . . H23B H 0.3594 0.6714 0.2103 0.081 Uiso 1 1 calc R U . . . H23C H 0.4457 0.6810 0.3047 0.081 Uiso 1 1 calc R U . . . C24 C 0.5630(6) 0.5987(3) 0.2066(4) 0.054(2) Uani 1 1 d . . . . . H24A H 0.5208 0.6200 0.1507 0.081 Uiso 1 1 calc R U . . . H24B H 0.6134 0.5528 0.2008 0.081 Uiso 1 1 calc R U . . . H24C H 0.6145 0.6409 0.2402 0.081 Uiso 1 1 calc R U . . . B1 B 0.3738(7) 0.6682(4) 0.4981(5) 0.0324(17) Uani 1 1 d . . . . . F2 F 0.2835(3) 0.62663(19) 0.4398(2) 0.0571(11) Uani 1 1 d . . . . . F3 F 0.3314(4) 0.6964(2) 0.5614(2) 0.0703(13) Uani 1 1 d . . . . . F4 F 0.4155(4) 0.72906(18) 0.4604(2) 0.0628(12) Uani 1 1 d . . . . . F5 F 0.4664(3) 0.6129(2) 0.5302(2) 0.0610(11) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01236(9) 0.01347(9) 0.01483(10) 0.00020(10) 0.00402(7) -0.00188(10) P1 0.0123(7) 0.0174(7) 0.0163(8) 0.0033(6) 0.0027(6) -0.0020(6) P2 0.0133(7) 0.0148(6) 0.0166(8) -0.0001(5) 0.0057(6) -0.0010(5) O1 0.022(2) 0.033(2) 0.018(2) -0.0052(18) -0.0007(19) -0.004(2) C1 0.018(3) 0.021(3) 0.026(3) 0.013(2) 0.005(3) 0.000(2) C2 0.037(4) 0.039(3) 0.032(4) 0.019(3) 0.003(3) -0.011(3) C3 0.029(4) 0.023(3) 0.039(4) 0.010(3) 0.002(3) 0.003(3) C4 0.034(4) 0.034(3) 0.019(3) 0.013(3) 0.000(3) -0.008(3) C5 0.016(3) 0.026(3) 0.035(3) 0.003(3) 0.012(3) 0.005(3) C6 0.018(3) 0.035(3) 0.057(5) 0.015(3) 0.005(3) 0.012(3) C7 0.018(3) 0.057(4) 0.043(4) 0.000(3) 0.015(3) 0.002(3) C8 0.031(4) 0.026(3) 0.053(4) -0.009(3) 0.018(3) 0.005(3) C9 0.029(3) 0.023(3) 0.021(3) -0.003(2) 0.001(3) -0.017(3) C10 0.050(4) 0.029(3) 0.036(4) -0.015(3) 0.013(3) -0.014(3) C11 0.031(4) 0.037(3) 0.035(4) 0.000(3) 0.002(3) -0.022(3) C12 0.047(4) 0.048(4) 0.020(4) -0.002(3) 0.001(3) -0.025(3) C13 0.023(3) 0.018(3) 0.023(3) 0.004(2) 0.012(3) 0.006(2) C14 0.040(4) 0.043(4) 0.032(4) 0.013(3) -0.008(3) -0.005(3) C15 0.045(4) 0.063(5) 0.039(4) 0.005(3) 0.005(3) 0.032(4) C16 0.037(4) 0.060(4) 0.045(4) 0.035(3) 0.000(3) -0.003(3) C17 0.016(3) 0.014(3) 0.032(4) 0.004(2) 0.009(3) 0.008(2) C18 0.060(5) 0.040(4) 0.069(6) -0.007(4) -0.003(4) 0.025(4) C19 0.089(6) 0.041(4) 0.093(6) 0.020(4) 0.077(5) 0.030(4) C20 0.031(4) 0.036(4) 0.071(5) -0.029(3) 0.003(4) 0.011(3) C21 0.020(3) 0.030(3) 0.031(3) -0.005(3) 0.011(3) -0.015(3) C22 0.036(4) 0.050(4) 0.037(4) -0.010(3) -0.006(3) -0.020(3) C23 0.039(4) 0.022(3) 0.092(5) -0.031(3) 0.004(4) -0.006(3) C24 0.050(5) 0.066(4) 0.052(5) -0.007(3) 0.023(4) -0.040(4) B1 0.039(5) 0.023(4) 0.030(5) 0.002(3) 0.000(4) -0.001(3) F2 0.038(2) 0.044(2) 0.072(3) -0.0126(19) -0.012(2) -0.0095(18) F3 0.111(4) 0.056(2) 0.060(3) -0.007(2) 0.049(3) -0.003(2) F4 0.096(3) 0.038(2) 0.058(3) 0.0071(18) 0.027(3) -0.021(2) F5 0.047(3) 0.053(2) 0.067(3) 0.007(2) -0.008(2) 0.016(2) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 P1 93.04(10) . . ? O1 Pt1 P2 102.83(10) . . ? P1 Pt1 P2 164.10(5) . . ? O1 Pt1 H1 175(2) . . ? P1 Pt1 H1 82.9(19) . . ? P2 Pt1 H1 81.3(19) . . ? C5 P1 C1 109.6(2) . . ? C5 P1 C9 108.8(2) . . ? C1 P1 C9 107.4(2) . . ? C5 P1 Pt1 109.17(16) . . ? C1 P1 Pt1 111.05(16) . . ? C9 P1 Pt1 110.81(16) . . ? C17 P2 C21 108.8(2) . . ? C17 P2 C13 108.8(2) . . ? C21 P2 C13 107.3(2) . . ? C17 P2 Pt1 107.59(16) . . ? C21 P2 Pt1 116.54(16) . . ? C13 P2 Pt1 107.64(16) . . ? C17 P2 H1 97.8(10) . . ? C21 P2 H1 147.1(11) . . ? C13 P2 H1 81.0(11) . . ? Pt1 P2 H1 33.8(11) . . ? Pt1 O1 H1A 112(4) . . ? Pt1 O1 H1B 123(4) . . ? H1A O1 H1B 117(6) . . ? C3 C1 C2 109.4(4) . . ? C3 C1 C4 106.3(4) . . ? C2 C1 C4 106.5(4) . . ? C3 C1 P1 107.8(3) . . ? C2 C1 P1 115.1(4) . . ? C4 C1 P1 111.5(3) . . ? 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 C8 106.7(4) . . ? C6 C5 C7 108.4(4) . . ? C8 C5 C7 108.3(4) . . ? C6 C5 P1 109.9(4) . . ? C8 C5 P1 108.2(3) . . ? C7 C5 P1 115.1(4) . . ? 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 . . ? C10 C9 C12 105.0(4) . . ? C10 C9 C11 109.8(4) . . ? C12 C9 C11 106.2(4) . . ? C10 C9 P1 110.2(4) . . ? C12 C9 P1 111.4(3) . . ? C11 C9 P1 113.8(4) . . ? 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 . . ? C16 C13 C15 109.5(4) . . ? C16 C13 C14 107.0(5) . . ? C15 C13 C14 104.4(5) . . ? C16 C13 P2 115.5(4) . . ? C15 C13 P2 108.4(4) . . ? C14 C13 P2 111.5(3) . . ? 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 . . ? C18 C17 C19 108.6(5) . . ? C18 C17 C20 104.4(4) . . ? C19 C17 C20 107.0(5) . . ? C18 C17 P2 110.6(4) . . ? C19 C17 P2 115.5(3) . . ? C20 C17 P2 110.2(3) . . ? 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 106.5(5) . . ? C22 C21 C24 105.5(5) . . ? C23 C21 C24 110.0(5) . . ? C22 C21 P2 110.5(4) . . ? C23 C21 P2 107.8(3) . . ? C24 C21 P2 116.1(4) . . ? 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 . . ? F4 B1 F3 110.9(5) . . ? F4 B1 F2 110.3(6) . . ? F3 B1 F2 110.2(6) . . ? F4 B1 F5 109.5(6) . . ? F3 B1 F5 109.8(6) . . ? F2 B1 F5 106.1(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.199(4) . ? Pt1 P1 2.3313(13) . ? Pt1 P2 2.3320(12) . ? Pt1 H1 1.43(5) . ? P1 C5 1.902(5) . ? P1 C1 1.910(5) . ? P1 C9 1.921(5) . ? P2 C17 1.893(5) . ? P2 C21 1.907(5) . ? P2 C13 1.914(5) . ? P2 H1 2.55(5) . ? O1 H1A 0.89(6) . ? O1 H1B 0.93(6) . ? C1 C3 1.536(7) . ? C1 C2 1.541(6) . ? C1 C4 1.536(7) . ? 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 1.526(7) . ? C5 C8 1.539(7) . ? C5 C7 1.552(6) . ? 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 C10 1.517(7) . ? C9 C12 1.547(7) . ? C9 C11 1.552(7) . ? 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 C16 1.511(6) . ? C13 C15 1.526(7) . ? C13 C14 1.532(7) . ? 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 C18 1.505(8) . ? C17 C19 1.530(6) . ? C17 C20 1.532(7) . ? 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 1.516(7) . ? C21 C23 1.537(7) . ? C21 C24 1.537(6) . ? 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 . ? B1 F4 1.347(7) . ? B1 F3 1.361(7) . ? B1 F2 1.383(7) . ? B1 F5 1.392(7) . ? 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 C21 P2 C17 C18 52.4(5) . . . . ? C13 P2 C17 C18 168.9(4) . . . . ? Pt1 P2 C17 C18 -74.7(4) . . . . ? C21 P2 C17 C19 -71.4(5) . . . . ? C13 P2 C17 C19 45.1(5) . . . . ? Pt1 P2 C17 C19 161.5(4) . . . . ? C21 P2 C17 C20 167.3(4) . . . . ? C13 P2 C17 C20 -76.2(4) . . . . ? Pt1 P2 C17 C20 40.2(4) . . . . ?