#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:53:04 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572004.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_1572004 loop_ _publ_author_name 'Wang, Patrick' 'Fares, Mohamed' 'Eladwy, Radwa A.' 'Bhuyan, Deep J.' 'Wu, Xin' 'Lewis, William' 'Loeb, Stephen J.' 'Macreadie, Lauren K.' 'Gale, Philip A.' _publ_section_title ; Platinum-based metal complexes as chloride transporters that trigger apoptosis. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11584 _journal_page_last 11593 _journal_paper_doi 10.1039/d4sc02115k _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C48 H52 N12 O4 Pt, 2(B F4)' _chemical_formula_sum 'C48 H52 B2 F8 N12 O4 Pt' _chemical_formula_weight 1229.72 _chemical_name_systematic 'Ethyl platinum complex' _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 iterative _audit_creation_date 2024-02-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-02-16 deposited with the CCDC. 2024-06-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.529(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.4301(13) _cell_length_b 19.8030(14) _cell_length_c 11.2570(9) _cell_measurement_reflns_used 5395 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.7060 _cell_measurement_theta_min 2.0520 _cell_volume 2477.3(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2930 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -26.00 71.00 1.00 45.00 -- -11.94 19.00 90.00 97 2 \w -15.00 30.00 1.00 45.00 -- -11.94 -99.00 -90.00 45 3 \w -15.00 57.00 1.00 45.00 -- 14.91 -99.00 -30.00 72 4 \w 37.00 105.00 1.00 45.00 -- 14.91-178.00 -60.00 68 5 \w -14.00 92.00 1.00 45.00 -- 14.91 38.00 90.00 106 6 \w -89.00 17.00 1.00 45.00 -- -11.94 -38.00 90.00 106 7 \w -52.00 3.00 1.00 45.00 -- -11.94 91.00 31.00 55 8 \w -15.00 30.00 1.00 45.00 -- -11.94 -99.00-180.00 45 9 \w -15.00 24.00 1.00 45.00 -- 14.91 -99.00 120.00 39 10 \w -68.00 26.00 1.00 45.00 -- 14.91 -19.00 90.00 94 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0281019000 _diffrn_orient_matrix_UB_12 0.0298633000 _diffrn_orient_matrix_UB_13 0.0143295000 _diffrn_orient_matrix_UB_21 -0.0572154000 _diffrn_orient_matrix_UB_22 -0.0136881000 _diffrn_orient_matrix_UB_23 -0.0278469000 _diffrn_orient_matrix_UB_31 -0.0038922000 _diffrn_orient_matrix_UB_32 -0.0142569000 _diffrn_orient_matrix_UB_33 0.0567209000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2077 _diffrn_reflns_av_unetI/netI 0.1094 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 37769 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.024 _diffrn_reflns_theta_max 25.024 _diffrn_reflns_theta_min 1.832 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.920 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.568 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.649 _exptl_crystal_description block _exptl_crystal_F_000 1232 _exptl_crystal_preparation 'Heating platinum complex with isoquinoline urea derivative in acetonitrile' _exptl_crystal_recrystallization_method 'From DMF/ether' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.656 _refine_diff_density_min -2.608 _refine_diff_density_rms 0.180 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 4374 _refine_ls_number_restraints 144 _refine_ls_restrained_S_all 0.988 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0540 _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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1139 _refine_ls_wR_factor_ref 0.1342 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2787 _reflns_number_total 4374 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02115k2.cif _cod_data_source_block pag22_s2618_sn994-2_auto _cod_depositor_comments 'Adding full bibliography for 1572002--1572006.cif.' _cod_database_code 1572004 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C48H52B2F8N12O4Pt _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_max 0.971 _shelx_estimated_absorpt_t_min 0.868 _olex2_refinement_description ; 1. Uiso/Uaniso restraints and constraints N31 \\sim C32 \\sim C33 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.2 within 2A N1 \\sim C2 \\sim C3 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 2. Rigid body (RIGU) restrains N31, C32, C33, C38, C39, C40 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N1, C2, C3, C8, C9, C10 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C45(H45A,H45B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C32(H32), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40) 3.c Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C46(H46A,H46B,H46C) ; _shelx_res_file ; TITL pag22_s2618_sn994-2_auto_a.res in P2(1)/c pag22_s2618_sn994-2_auto.res created by SHELXL-2018/3 at 14:35:37 on 04-Jul-2023 REM Old TITL pag22_s2618_sn994-2_auto in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.148, Rweak 0.007, Alpha 0.043 REM 0.445 for 166 systematic absences, Orientation as input REM Formula found by SHELXT: C52 B2 N8 O4 F8 Pt CELL 0.71073 11.4301 19.803 11.257 90 103.529 90 ZERR 2 0.0013 0.0014 0.0009 0 0.01 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F N O Pt UNIT 96 104 4 16 24 8 2 RIGU N31 C32 C33 C38 > C40 RIGU N1 C2 C3 C8 > C10 SIMU 0.01 0.2 2 N31 C32 C33 C38 > C40 SIMU 0.01 0.02 2 N1 C2 C3 C8 > C10 L.S. 12 PLAN 5 SIZE 0.01 0.03 0.05 TEMP -173(2) CONF HTAB N11 F52 HTAB N14 F52 HTAB N41 F54 HTAB N44 F55 BOND list 4 MORE -1 BOND $H fmap 2 acta SHEL 1200 0.84 REM REM REM WGHT 0.055700 FVAR 0.42613 N1 5 0.549836 0.402188 0.497525 11.00000 0.02666 0.02161 = 0.01376 0.00372 0.00706 -0.00556 PT1 7 0.500000 0.500000 0.500000 10.50000 0.02422 0.01341 = 0.02050 0.00008 0.01363 -0.00217 C2 1 0.505863 0.357946 0.560964 11.00000 0.02711 0.01878 = 0.01343 -0.00484 0.01131 0.00035 AFIX 43 H2 2 0.453397 0.373708 0.609085 11.00000 -1.20000 AFIX 0 C3 1 0.531319 0.287556 0.562853 11.00000 0.02531 0.02428 = 0.01713 -0.00251 0.00363 -0.00208 C4 1 0.484035 0.239279 0.632527 11.00000 0.02812 0.01631 = 0.02365 0.00729 0.01123 0.00247 C5 1 0.506643 0.171118 0.619250 11.00000 0.05048 0.01732 = 0.02963 0.00778 0.02167 0.00314 AFIX 43 H5 2 0.471860 0.138213 0.661901 11.00000 -1.20000 AFIX 0 C6 1 0.580865 0.151083 0.542799 11.00000 0.04862 0.02122 = 0.03780 -0.00433 0.01469 0.01026 AFIX 43 H6 2 0.596828 0.104341 0.535993 11.00000 -1.20000 AFIX 0 C7 1 0.631762 0.196716 0.476890 11.00000 0.03888 0.02078 = 0.04177 0.00790 0.02166 0.01536 AFIX 43 H7 2 0.683269 0.181679 0.427182 11.00000 -1.20000 AFIX 0 C8 1 0.606264 0.265317 0.484523 11.00000 0.02103 0.02441 = 0.01764 -0.00022 0.00121 0.00192 C9 1 0.653740 0.315072 0.420272 11.00000 0.02176 0.03010 = 0.02530 -0.00162 0.01016 -0.00010 AFIX 43 H9 2 0.708051 0.302422 0.371918 11.00000 -1.20000 AFIX 0 C10 1 0.623252 0.380660 0.426275 11.00000 0.02621 0.02722 = 0.02108 0.00011 0.00872 -0.00433 AFIX 43 H10 2 0.654230 0.412841 0.379028 11.00000 -1.20000 AFIX 0 N11 5 0.412056 0.263455 0.708997 11.00000 0.03987 0.00697 = 0.03533 -0.00140 0.01897 0.00024 H11 2 0.407940 0.301691 0.725554 11.00000 -1.20000 C12 1 0.347358 0.225869 0.779088 11.00000 0.02840 0.02266 = 0.02436 0.00511 0.00752 -0.00385 O13 6 0.349678 0.164219 0.782301 11.00000 0.04152 0.01564 = 0.03479 0.00084 0.01657 -0.00322 N14 5 0.283926 0.264395 0.838184 11.00000 0.03904 0.01524 = 0.03632 0.00664 0.02114 -0.00195 H14 2 0.280945 0.310832 0.837649 11.00000 -1.20000 C15 1 0.209292 0.232622 0.912885 11.00000 0.02223 0.03100 = 0.03463 0.00576 0.01256 0.00019 AFIX 23 H15A 2 0.258304 0.199327 0.968828 11.00000 -1.20000 H15B 2 0.141801 0.208157 0.858869 11.00000 -1.20000 AFIX 0 C16 1 0.160325 0.283647 0.985766 11.00000 0.03505 0.03751 = 0.03482 0.00393 0.00841 0.00315 AFIX 137 H16A 2 0.102396 0.312616 0.930638 11.00000 -1.50000 H16B 2 0.226323 0.311335 1.032448 11.00000 -1.50000 H16C 2 0.120063 0.260532 1.042125 11.00000 -1.50000 AFIX 0 N31 5 0.359949 0.484837 0.354886 11.00000 0.02231 0.01671 = 0.02320 0.00318 0.01322 0.00505 C32 1 0.254384 0.463174 0.379024 11.00000 0.02382 0.01160 = 0.02065 -0.00344 0.01419 0.00435 AFIX 43 H32 2 0.249500 0.458227 0.461667 11.00000 -1.20000 AFIX 0 C33 1 0.152633 0.447954 0.285337 11.00000 0.02284 0.01541 = 0.02462 0.00261 0.00888 0.00277 C34 1 0.042072 0.424918 0.310306 11.00000 0.02852 0.02034 = 0.02931 -0.00726 0.01320 0.00326 C35 1 -0.050181 0.407573 0.214743 11.00000 0.02789 0.03206 = 0.03061 0.00392 0.01206 0.00503 AFIX 43 H35 2 -0.124054 0.392122 0.229827 11.00000 -1.20000 AFIX 0 C36 1 -0.037184 0.412261 0.096631 11.00000 0.02085 0.03221 = 0.02575 -0.00193 -0.00104 0.00334 AFIX 43 H36 2 -0.102837 0.399194 0.032119 11.00000 -1.20000 AFIX 0 C37 1 0.064641 0.434597 0.067889 11.00000 0.04495 0.02881 = 0.01799 0.00594 0.00719 0.01264 AFIX 43 H37 2 0.070236 0.436514 -0.014925 11.00000 -1.20000 AFIX 0 C38 1 0.162019 0.454921 0.162236 11.00000 0.02921 0.01945 = 0.02358 0.00016 0.00717 0.00349 C39 1 0.272821 0.479251 0.141904 11.00000 0.03688 0.02515 = 0.01633 0.00788 0.01478 0.00609 AFIX 43 H39 2 0.281605 0.485436 0.060754 11.00000 -1.20000 AFIX 0 C40 1 0.365964 0.493671 0.237576 11.00000 0.03034 0.01728 = 0.02467 0.00955 0.01661 0.00883 AFIX 43 H40 2 0.438386 0.510680 0.221384 11.00000 -1.20000 AFIX 0 N41 5 0.034252 0.419568 0.434684 11.00000 0.03042 0.03340 = 0.02237 0.00045 0.01430 -0.00181 H41 2 0.079415 0.459492 0.488379 11.00000 -1.20000 C42 1 -0.026282 0.367737 0.478379 11.00000 0.02930 0.04293 = 0.04300 0.00597 0.02194 -0.00201 O43 6 -0.081273 0.322987 0.410028 11.00000 0.03425 0.03510 = 0.03656 -0.00134 0.00713 -0.00478 N44 5 -0.018038 0.371477 0.599383 11.00000 0.05259 0.05330 = 0.03084 -0.01072 0.02229 -0.01982 H44 2 0.026377 0.401494 0.629480 11.00000 -1.20000 C45 1 -0.062677 0.316439 0.665769 11.00000 0.04079 0.05695 = 0.02407 -0.00571 0.01233 -0.00409 AFIX 23 H45A 2 -0.109742 0.284066 0.606294 11.00000 -1.20000 H45B 2 0.006509 0.291912 0.716955 11.00000 -1.20000 AFIX 0 C46 1 -0.139030 0.343259 0.743955 11.00000 0.04986 0.06063 = 0.04418 0.00253 0.02364 -0.00271 AFIX 137 H46A 2 -0.209846 0.365392 0.692849 11.00000 -1.50000 H46B 2 -0.093052 0.376089 0.801600 11.00000 -1.50000 H46C 2 -0.164896 0.306105 0.789337 11.00000 -1.50000 AFIX 0 B51 3 0.272327 0.453382 0.765333 11.00000 0.04817 0.02798 = 0.03234 0.00331 0.03196 0.00052 F52 4 0.355388 0.406208 0.749733 11.00000 0.09106 0.02913 = 0.09166 0.00550 0.06631 0.01436 F53 4 0.327920 0.505472 0.836804 11.00000 0.05772 0.03503 = 0.04756 -0.01243 0.00290 -0.00786 F54 4 0.213151 0.479268 0.651207 11.00000 0.05975 0.06975 = 0.02712 0.00174 0.01785 -0.01389 F55 4 0.188834 0.422670 0.817975 11.00000 0.05306 0.05196 = 0.04979 0.00421 0.03609 -0.00605 HKLF 4 REM pag22_s2618_sn994-2_auto_a.res in P2(1)/c REM wR2 = 0.1342, GooF = S = 1.003, Restrained GooF = 0.988 for all data REM R1 = 0.0540 for 2787 Fo > 4sig(Fo) and 0.0970 for all 4374 data REM 354 parameters refined using 144 restraints END WGHT 0.0561 0.0000 REM Highest difference peak 1.656, deepest hole -2.608, 1-sigma level 0.180 Q1 1 0.4149 0.5003 0.5410 11.00000 0.05 1.66 Q2 1 0.5451 0.5001 0.4457 11.00000 0.05 1.44 Q3 1 0.4925 0.5404 0.6032 11.00000 0.05 1.42 Q4 1 0.5055 0.5388 0.3995 11.00000 0.05 1.31 Q5 1 0.5899 0.4554 0.5149 11.00000 0.05 1.04 ; _shelx_res_checksum 11318 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 3.079 _oxdiff_exptl_absorpt_empirical_full_min 0.218 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 N1 N 0.5498(6) 0.4022(3) 0.4975(6) 0.0203(14) Uani 1 1 d . U . . . Pt1 Pt 0.500000 0.500000 0.500000 0.01799(16) Uani 1 2 d S . P . . C2 C 0.5059(7) 0.3579(4) 0.5610(7) 0.0187(16) Uani 1 1 d . U . . . H2 H 0.453397 0.373708 0.609085 0.022 Uiso 1 1 calc R U . . . C3 C 0.5313(8) 0.2876(4) 0.5629(8) 0.0225(17) Uani 1 1 d . U . . . C4 C 0.4840(8) 0.2393(4) 0.6325(7) 0.022(2) Uani 1 1 d . . . . . C5 C 0.5066(9) 0.1711(4) 0.6193(8) 0.030(2) Uani 1 1 d . . . . . H5 H 0.471860 0.138213 0.661901 0.037 Uiso 1 1 calc R U . . . C6 C 0.5809(9) 0.1511(4) 0.5428(8) 0.035(2) Uani 1 1 d . . . . . H6 H 0.596828 0.104341 0.535993 0.042 Uiso 1 1 calc R U . . . C7 C 0.6318(8) 0.1967(4) 0.4769(8) 0.032(2) Uani 1 1 d . . . . . H7 H 0.683269 0.181679 0.427182 0.038 Uiso 1 1 calc R U . . . C8 C 0.6063(7) 0.2653(4) 0.4845(7) 0.0216(17) Uani 1 1 d . U . . . C9 C 0.6537(8) 0.3151(4) 0.4203(8) 0.0250(18) Uani 1 1 d . U . . . H9 H 0.708051 0.302422 0.371918 0.030 Uiso 1 1 calc R U . . . C10 C 0.6233(8) 0.3807(4) 0.4263(7) 0.0243(17) Uani 1 1 d . U . . . H10 H 0.654230 0.412841 0.379028 0.029 Uiso 1 1 calc R U . . . N11 N 0.4121(7) 0.2635(3) 0.7090(7) 0.0257(19) Uani 1 1 d . . . . . H11 H 0.408(8) 0.302(4) 0.726(8) 0.031 Uiso 1 1 d . U . . . C12 C 0.3474(8) 0.2259(4) 0.7791(8) 0.025(2) Uani 1 1 d . . . . . O13 O 0.3497(6) 0.1642(3) 0.7823(5) 0.0294(15) Uani 1 1 d . . . . . N14 N 0.2839(7) 0.2644(4) 0.8382(7) 0.0282(19) Uani 1 1 d . . . . . H14 H 0.281(8) 0.311(4) 0.838(8) 0.034 Uiso 1 1 d . U . . . C15 C 0.2093(8) 0.2326(4) 0.9129(8) 0.028(2) Uani 1 1 d . . . . . H15A H 0.258304 0.199327 0.968828 0.034 Uiso 1 1 calc R U . . . H15B H 0.141801 0.208157 0.858869 0.034 Uiso 1 1 calc R U . . . C16 C 0.1603(9) 0.2836(5) 0.9858(8) 0.036(2) Uani 1 1 d . . . . . H16A H 0.102396 0.312616 0.930638 0.054 Uiso 1 1 calc R U . . . H16B H 0.226323 0.311335 1.032448 0.054 Uiso 1 1 calc R U . . . H16C H 0.120063 0.260532 1.042125 0.054 Uiso 1 1 calc R U . . . N31 N 0.3599(6) 0.4848(3) 0.3549(6) 0.0194(15) Uani 1 1 d . U . . . C32 C 0.2544(7) 0.4632(4) 0.3790(7) 0.0172(16) Uani 1 1 d . U . . . H32 H 0.249500 0.458227 0.461667 0.021 Uiso 1 1 calc R U . . . C33 C 0.1526(8) 0.4480(4) 0.2853(7) 0.0204(16) Uani 1 1 d . U . . . C34 C 0.0421(8) 0.4249(4) 0.3103(8) 0.025(2) Uani 1 1 d . . . . . C35 C -0.0502(8) 0.4076(4) 0.2147(8) 0.029(2) Uani 1 1 d . . . . . H35 H -0.124054 0.392122 0.229827 0.035 Uiso 1 1 calc R U . . . C36 C -0.0372(8) 0.4123(4) 0.0966(8) 0.027(2) Uani 1 1 d . . . . . H36 H -0.102837 0.399194 0.032119 0.033 Uiso 1 1 calc R U . . . C37 C 0.0646(9) 0.4346(4) 0.0679(8) 0.031(2) Uani 1 1 d . . . . . H37 H 0.070236 0.436514 -0.014925 0.037 Uiso 1 1 calc R U . . . C38 C 0.1620(8) 0.4549(4) 0.1622(8) 0.0239(17) Uani 1 1 d . U . . . C39 C 0.2728(8) 0.4793(4) 0.1419(8) 0.0247(18) Uani 1 1 d . U . . . H39 H 0.281605 0.485436 0.060754 0.030 Uiso 1 1 calc R U . . . C40 C 0.3660(8) 0.4937(4) 0.2376(7) 0.0224(16) Uani 1 1 d . U . . . H40 H 0.438386 0.510680 0.221384 0.027 Uiso 1 1 calc R U . . . N41 N 0.0343(7) 0.4196(4) 0.4347(7) 0.0274(18) Uani 1 1 d . . . . . H41 H 0.079(8) 0.459(4) 0.488(7) 0.033 Uiso 1 1 d . U . . . C42 C -0.0263(8) 0.3677(5) 0.4784(9) 0.036(3) Uani 1 1 d . . . . . O43 O -0.0813(6) 0.3230(3) 0.4100(6) 0.0355(16) Uani 1 1 d . . . . . N44 N -0.0180(8) 0.3715(5) 0.5994(8) 0.044(2) Uani 1 1 d . . . . . H44 H 0.026(10) 0.401(5) 0.629(9) 0.052 Uiso 1 1 d . U . . . C45 C -0.0627(9) 0.3164(5) 0.6658(8) 0.040(3) Uani 1 1 d . . . . . H45A H -0.109742 0.284066 0.606294 0.048 Uiso 1 1 calc R U . . . H45B H 0.006509 0.291912 0.716955 0.048 Uiso 1 1 calc R U . . . C46 C -0.1390(10) 0.3433(5) 0.7440(9) 0.049(3) Uani 1 1 d . . . . . H46A H -0.209846 0.365392 0.692849 0.074 Uiso 1 1 calc R U . . . H46B H -0.093052 0.376089 0.801600 0.074 Uiso 1 1 calc R U . . . H46C H -0.164896 0.306105 0.789337 0.074 Uiso 1 1 calc R U . . . B51 B 0.2723(11) 0.4534(5) 0.7653(10) 0.032(3) Uani 1 1 d . . . . . F52 F 0.3554(6) 0.4062(3) 0.7497(6) 0.063(2) Uani 1 1 d . . . . . F53 F 0.3279(5) 0.5055(3) 0.8368(5) 0.0483(15) Uani 1 1 d . . . . . F54 F 0.2132(6) 0.4793(3) 0.6512(5) 0.0509(16) Uani 1 1 d . . . . . F55 F 0.1888(5) 0.4227(3) 0.8180(5) 0.0476(16) 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 N1 0.027(4) 0.022(3) 0.014(3) 0.004(3) 0.007(3) -0.006(3) Pt1 0.0242(3) 0.0134(2) 0.0205(3) 0.0001(2) 0.01363(19) -0.0022(2) C2 0.027(4) 0.019(3) 0.013(4) -0.005(3) 0.011(3) 0.000(3) C3 0.025(4) 0.024(4) 0.017(4) -0.003(3) 0.004(3) -0.002(3) C4 0.028(5) 0.016(5) 0.024(5) 0.007(4) 0.011(4) 0.002(4) C5 0.050(7) 0.017(5) 0.030(6) 0.008(4) 0.022(5) 0.003(4) C6 0.049(7) 0.021(5) 0.038(6) -0.004(4) 0.015(5) 0.010(5) C7 0.039(6) 0.021(5) 0.042(6) 0.008(4) 0.022(5) 0.015(4) C8 0.021(4) 0.024(4) 0.018(4) 0.000(3) 0.001(3) 0.002(3) C9 0.022(4) 0.030(4) 0.025(4) -0.002(3) 0.010(3) 0.000(3) C10 0.026(4) 0.027(4) 0.021(4) 0.000(3) 0.009(3) -0.004(3) N11 0.040(5) 0.007(4) 0.035(5) -0.001(3) 0.019(4) 0.000(4) C12 0.028(6) 0.023(5) 0.024(5) 0.005(4) 0.008(4) -0.004(4) O13 0.042(4) 0.016(3) 0.035(4) 0.001(3) 0.017(3) -0.003(3) N14 0.039(5) 0.015(4) 0.036(5) 0.007(4) 0.021(4) -0.002(4) C15 0.022(5) 0.031(5) 0.035(6) 0.006(4) 0.013(4) 0.000(4) C16 0.035(6) 0.038(6) 0.035(6) 0.004(5) 0.008(5) 0.003(5) N31 0.022(3) 0.017(4) 0.023(3) 0.003(3) 0.013(3) 0.005(3) C32 0.024(4) 0.012(4) 0.021(4) -0.003(3) 0.014(3) 0.004(3) C33 0.023(4) 0.015(4) 0.025(4) 0.003(3) 0.009(3) 0.003(3) C34 0.029(6) 0.020(5) 0.029(5) -0.007(4) 0.013(4) 0.003(4) C35 0.028(6) 0.032(5) 0.031(6) 0.004(4) 0.012(5) 0.005(4) C36 0.021(5) 0.032(5) 0.026(5) -0.002(4) -0.001(4) 0.003(4) C37 0.045(7) 0.029(5) 0.018(5) 0.006(4) 0.007(5) 0.013(5) C38 0.029(4) 0.019(4) 0.024(4) 0.000(3) 0.007(3) 0.003(3) C39 0.037(4) 0.025(4) 0.016(4) 0.008(3) 0.015(3) 0.006(3) C40 0.030(4) 0.017(4) 0.025(3) 0.010(3) 0.017(3) 0.009(4) N41 0.030(5) 0.033(4) 0.022(4) 0.000(4) 0.014(4) -0.002(4) C42 0.029(7) 0.043(6) 0.043(7) 0.006(5) 0.022(6) -0.002(5) O43 0.034(4) 0.035(4) 0.037(4) -0.001(3) 0.007(3) -0.005(3) N44 0.053(7) 0.053(6) 0.031(5) -0.011(4) 0.022(5) -0.020(5) C45 0.041(7) 0.057(7) 0.024(6) -0.006(5) 0.012(5) -0.004(5) C46 0.050(8) 0.061(8) 0.044(7) 0.003(6) 0.024(6) -0.003(6) B51 0.048(8) 0.028(6) 0.032(7) 0.003(5) 0.032(6) 0.001(5) F52 0.091(5) 0.029(3) 0.092(5) 0.005(3) 0.066(4) 0.014(3) F53 0.058(4) 0.035(3) 0.048(3) -0.012(3) 0.003(3) -0.008(3) F54 0.060(4) 0.070(4) 0.027(3) 0.002(3) 0.018(3) -0.014(3) F55 0.053(4) 0.052(4) 0.050(4) 0.004(3) 0.036(3) -0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 3 5 0.1382 -2 -5 2 0.1035 1 -5 4 0.1442 -1 5 -4 0.0072 -5 3 3 0.0849 5 -3 -3 0.0010 -2 -5 1 0.0752 2 5 -1 0.0592 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 C2 N1 Pt1 119.4(5) . . ? C2 N1 C10 118.9(7) . . ? C10 N1 Pt1 121.6(5) . . ? N1 Pt1 N1 180.0(3) 3_666 . ? N1 Pt1 N31 88.9(3) 3_666 . ? N1 Pt1 N31 91.1(3) . . ? N1 Pt1 N31 91.1(3) 3_666 3_666 ? N1 Pt1 N31 88.9(3) . 3_666 ? N31 Pt1 N31 180.0 . 3_666 ? N1 C2 H2 117.9 . . ? N1 C2 C3 124.3(7) . . ? C3 C2 H2 117.9 . . ? C2 C3 C8 116.2(7) . . ? C4 C3 C2 124.4(7) . . ? C4 C3 C8 119.4(7) . . ? C5 C4 C3 119.3(7) . . ? C5 C4 N11 123.1(7) . . ? N11 C4 C3 117.5(7) . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(8) . . ? C6 C5 H5 120.1 . . ? C5 C6 H6 118.8 . . ? C7 C6 C5 122.5(8) . . ? C7 C6 H6 118.8 . . ? C6 C7 H7 120.5 . . ? C6 C7 C8 118.9(8) . . ? C8 C7 H7 120.5 . . ? C7 C8 C3 120.0(7) . . ? C7 C8 C9 122.7(7) . . ? C9 C8 C3 117.3(7) . . ? C8 C9 H9 119.5 . . ? C10 C9 C8 120.9(7) . . ? C10 C9 H9 119.5 . . ? N1 C10 H10 118.9 . . ? C9 C10 N1 122.3(7) . . ? C9 C10 H10 118.9 . . ? C4 N11 H11 123(6) . . ? C4 N11 C12 128.3(7) . . ? C12 N11 H11 108(6) . . ? O13 C12 N11 122.2(8) . . ? O13 C12 N14 124.6(7) . . ? N14 C12 N11 113.2(7) . . ? C12 N14 H14 126(5) . . ? C12 N14 C15 119.7(7) . . ? C15 N14 H14 114(5) . . ? N14 C15 H15A 109.3 . . ? N14 C15 H15B 109.3 . . ? N14 C15 C16 111.5(7) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C32 N31 Pt1 117.0(5) . . ? C40 N31 Pt1 124.0(6) . . ? C40 N31 C32 119.0(7) . . ? N31 C32 H32 118.9 . . ? N31 C32 C33 122.1(7) . . ? C33 C32 H32 118.9 . . ? C32 C33 C34 122.2(7) . . ? C32 C33 C38 118.2(7) . . ? C38 C33 C34 119.6(8) . . ? C35 C34 C33 118.7(8) . . ? C35 C34 N41 122.8(8) . . ? N41 C34 C33 118.5(8) . . ? C34 C35 H35 119.7 . . ? C34 C35 C36 120.5(8) . . ? C36 C35 H35 119.7 . . ? C35 C36 H36 118.4 . . ? C37 C36 C35 123.1(9) . . ? C37 C36 H36 118.4 . . ? C36 C37 H37 120.5 . . ? C36 C37 C38 119.1(8) . . ? C38 C37 H37 120.5 . . ? C33 C38 C39 117.6(8) . . ? C37 C38 C33 118.8(8) . . ? C37 C38 C39 123.6(8) . . ? C38 C39 H39 119.8 . . ? C40 C39 C38 120.4(8) . . ? C40 C39 H39 119.8 . . ? N31 C40 C39 122.7(8) . . ? N31 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C34 N41 H41 112(4) . . ? C42 N41 C34 123.5(8) . . ? C42 N41 H41 125(4) . . ? O43 C42 N41 121.9(9) . . ? O43 C42 N44 124.8(9) . . ? N44 C42 N41 113.3(9) . . ? C42 N44 H44 111(7) . . ? C42 N44 C45 121.4(8) . . ? C45 N44 H44 126(8) . . ? N44 C45 H45A 109.4 . . ? N44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C46 C45 N44 111.0(8) . . ? C46 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F52 B51 F54 109.4(8) . . ? F52 B51 F55 108.9(8) . . ? F53 B51 F52 110.4(10) . . ? F53 B51 F54 108.7(8) . . ? F53 B51 F55 110.7(8) . . ? F55 B51 F54 108.8(9) . . ? 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 N1 Pt1 2.021(7) . ? N1 C2 1.303(9) . ? N1 C10 1.358(10) . ? Pt1 N31 2.024(7) . ? Pt1 N31 2.024(7) 3_666 ? C2 H2 0.9500 . ? C2 C3 1.423(11) . ? C3 C4 1.421(11) . ? C3 C8 1.435(11) . ? C4 C5 1.389(11) . ? C4 N11 1.407(10) . ? C5 H5 0.9500 . ? C5 C6 1.400(11) . ? C6 H6 0.9500 . ? C6 C7 1.381(12) . ? C7 H7 0.9500 . ? C7 C8 1.396(11) . ? C8 C9 1.404(11) . ? C9 H9 0.9500 . ? C9 C10 1.351(11) . ? C10 H10 0.9500 . ? N11 H11 0.78(8) . ? N11 C12 1.413(10) . ? C12 O13 1.222(9) . ? C12 N14 1.333(10) . ? N14 H14 0.92(8) . ? N14 C15 1.472(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.491(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N31 C32 1.366(9) . ? N31 C40 1.350(10) . ? C32 H32 0.9500 . ? C32 C33 1.408(11) . ? C33 C34 1.432(11) . ? C33 C38 1.421(11) . ? C34 C35 1.362(12) . ? C34 N41 1.428(10) . ? C35 H35 0.9500 . ? C35 C36 1.375(11) . ? C36 H36 0.9500 . ? C36 C37 1.353(12) . ? C37 H37 0.9500 . ? C37 C38 1.406(12) . ? C38 C39 1.423(11) . ? C39 H39 0.9500 . ? C39 C40 1.356(12) . ? C40 H40 0.9500 . ? N41 H41 1.05(9) . ? N41 C42 1.390(11) . ? C42 O43 1.243(11) . ? C42 N44 1.345(12) . ? N44 H44 0.80(10) . ? N44 C45 1.478(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.476(12) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? B51 F52 1.372(11) . ? B51 F53 1.370(12) . ? B51 F54 1.402(13) . ? B51 F55 1.377(11) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N11 H11 F52 0.78(8) 2.19(8) 2.960(8) 167(9) . yes N14 H14 F52 0.92(8) 2.38(8) 3.151(9) 141(7) . yes N41 H41 F54 1.05(9) 2.13(9) 3.031(10) 142(7) . yes N44 H44 F55 0.80(10) 2.51(10) 3.155(11) 139(10) . yes 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 N1 C2 C3 C4 179.6(8) . . . . ? N1 C2 C3 C8 -2.9(13) . . . . ? Pt1 N1 C2 C3 177.8(7) . . . . ? Pt1 N1 C10 C9 -177.5(6) . . . . ? Pt1 N31 C32 C33 -177.0(6) . . . . ? Pt1 N31 C40 C39 175.9(6) . . . . ? C2 N1 C10 C9 -1.0(13) . . . . ? C2 C3 C4 C5 174.5(8) . . . . ? C2 C3 C4 N11 -3.2(13) . . . . ? C2 C3 C8 C7 -177.4(8) . . . . ? C2 C3 C8 C9 4.2(12) . . . . ? C3 C4 C5 C6 3.5(14) . . . . ? C3 C4 N11 C12 174.5(9) . . . . ? C3 C8 C9 C10 -4.2(13) . . . . ? C4 C3 C8 C7 0.3(13) . . . . ? C4 C3 C8 C9 -178.2(8) . . . . ? C4 C5 C6 C7 -1.3(15) . . . . ? C4 N11 C12 O13 1.6(15) . . . . ? C4 N11 C12 N14 -177.5(9) . . . . ? C5 C4 N11 C12 -3.1(15) . . . . ? C5 C6 C7 C8 -1.4(15) . . . . ? C6 C7 C8 C3 1.9(14) . . . . ? C6 C7 C8 C9 -179.7(9) . . . . ? C7 C8 C9 C10 177.4(9) . . . . ? C8 C3 C4 C5 -3.0(13) . . . . ? C8 C3 C4 N11 179.4(8) . . . . ? C8 C9 C10 N1 2.6(13) . . . . ? C10 N1 C2 C3 1.2(13) . . . . ? N11 C4 C5 C6 -179.0(9) . . . . ? N11 C12 N14 C15 178.5(8) . . . . ? C12 N14 C15 C16 171.5(9) . . . . ? O13 C12 N14 C15 -0.5(15) . . . . ? N31 C32 C33 C34 179.7(7) . . . . ? N31 C32 C33 C38 0.7(11) . . . . ? C32 N31 C40 C39 -2.8(11) . . . . ? C32 C33 C34 C35 -176.3(8) . . . . ? C32 C33 C34 N41 2.2(12) . . . . ? C32 C33 C38 C37 174.8(7) . . . . ? C32 C33 C38 C39 -2.2(11) . . . . ? C33 C34 C35 C36 -0.1(13) . . . . ? C33 C34 N41 C42 -141.9(9) . . . . ? C33 C38 C39 C40 1.3(12) . . . . ? C34 C33 C38 C37 -4.2(12) . . . . ? C34 C33 C38 C39 178.8(7) . . . . ? C34 C35 C36 C37 -0.8(13) . . . . ? C34 N41 C42 O43 -2.1(14) . . . . ? C34 N41 C42 N44 177.6(8) . . . . ? C35 C34 N41 C42 36.6(13) . . . . ? C35 C36 C37 C38 -0.8(13) . . . . ? C36 C37 C38 C33 3.3(12) . . . . ? C36 C37 C38 C39 -179.9(8) . . . . ? C37 C38 C39 C40 -175.5(8) . . . . ? C38 C33 C34 C35 2.6(12) . . . . ? C38 C33 C34 N41 -178.8(7) . . . . ? C38 C39 C40 N31 1.2(12) . . . . ? C40 N31 C32 C33 1.8(10) . . . . ? N41 C34 C35 C36 -178.6(8) . . . . ? N41 C42 N44 C45 -172.0(9) . . . . ? C42 N44 C45 C46 -131.3(10) . . . . ? O43 C42 N44 C45 7.7(16) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9976 3.0024 5.0043 0.1333 -0.2375 0.2372 -1.9988 -5.0015 1.9983 -0.0646 0.1272 0.1924 1.0005 -4.9963 4.0027 -0.1200 -0.1003 0.2944 -1.0005 4.9963 -4.0027 0.1200 0.1003 -0.2944 -5.0017 2.9924 2.9965 0.2729 0.1618 0.1468 5.0017 -2.9924 -2.9965 -0.2729 -0.1618 -0.1468 -1.9986 -5.0018 0.9977 -0.0789 0.1550 0.1357 1.9986 5.0018 -0.9977 0.0789 -0.1550 -0.1357