#------------------------------------------------------------------------------ #$Date: 2024-06-28 01:08:19 +0300 (Fri, 28 Jun 2024) $ #$Revision: 292626 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572006.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_1572006 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_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02115K _journal_year 2024 _chemical_formula_moiety 'C52 H60 N12 O4 Pt, 2(B F4)' _chemical_formula_sum 'C52 H60 B2 F8 N12 O4 Pt' _chemical_formula_weight 1285.83 _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 106.062(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.1096(12) _cell_length_b 19.8229(13) _cell_length_c 11.4298(12) _cell_measurement_reflns_used 5197 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.7040 _cell_measurement_theta_min 2.1080 _cell_volume 2636.6(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 -41.00 66.00 1.00 45.00 -- -11.94 38.00-120.00 107 2 \w -76.00 106.00 1.00 45.00 -- 14.91 0.00-180.00 182 3 \w -42.00 23.00 1.00 45.00 -- -11.94 -77.00 -90.00 65 4 \w -42.00 23.00 1.00 45.00 -- -11.94 -77.00 150.00 65 5 \w -15.00 30.00 1.00 45.00 -- -11.94 -99.00 150.00 45 6 \w -15.00 57.00 1.00 45.00 -- 14.91 -99.00 150.00 72 7 \w -15.00 57.00 1.00 45.00 -- 14.91 -99.00 0.00 72 8 \w -63.00 44.00 1.00 45.00 -- 14.91 -38.00 60.00 107 9 \w -42.00 -21.00 1.00 45.00 -- -11.94 -77.00 30.00 21 ; _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 0.0187000000 _diffrn_orient_matrix_UB_12 -0.0203569000 _diffrn_orient_matrix_UB_13 0.0528721000 _diffrn_orient_matrix_UB_21 -0.0517418000 _diffrn_orient_matrix_UB_22 -0.0187960000 _diffrn_orient_matrix_UB_23 -0.0183108000 _diffrn_orient_matrix_UB_31 0.0261940000 _diffrn_orient_matrix_UB_32 -0.0226628000 _diffrn_orient_matrix_UB_33 -0.0322552000 _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 0.2593 _diffrn_reflns_av_unetI/netI 0.1535 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _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 39122 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.025 _diffrn_reflns_theta_max 25.025 _diffrn_reflns_theta_min 2.029 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.748 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.797 _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 light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.620 _exptl_crystal_description block _exptl_crystal_F_000 1296 _exptl_crystal_size_max 0.121 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.031 _refine_diff_density_max 1.420 _refine_diff_density_min -1.939 _refine_diff_density_rms 0.199 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 4655 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0660 _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^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1315 _refine_ls_wR_factor_ref 0.1601 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2732 _reflns_number_total 4655 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02115k2.cif _cod_data_source_block pag22_s2619_sn1002 _cod_database_code 1572006 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C52 H60 B2 F8 N12 O4 Pt' _chemical_oxdiff_usercomment 'propyl Pt' _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 0.920 _shelx_estimated_absorpt_t_min 0.732 _olex2_refinement_description ; 1. Restrained distances N41-H41 \\sim N44-H44 \\sim N14-H14 \\sim N11-H11 with sigma of 0.02 2.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C45(H45A,H45B), C46(H46A,H46B) 2.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) 2.c Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C47(H47A,H47B,H47C) ; _shelx_res_file ; TITL pag22_s2619_sn1002_a.res in P2(1)/c pag22_s2619_sn1002.res created by SHELXL-2018/3 at 14:45:43 on 04-Jul-2023 REM Old TITL pag22_s2619_sn1002 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.212, Rweak 0.011, Alpha 0.116 REM 0.446 for 175 systematic absences, Orientation as input REM Formula found by SHELXT: C48 B6 N20 O10 F8 Pt CELL 0.71073 12.1096 19.8229 11.4298 90 106.062 90 ZERR 2 0.0012 0.0013 0.0012 0 0.011 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F N O Pt UNIT 104 120 4 16 24 8 2 SADI N41 H41 N44 H44 N14 H14 N11 H11 L.S. 12 PLAN 10 SIZE 0.031 0.072 0.121 TEMP -173(2) CONF HTAB N11 F62 HTAB N14 F62 HTAB N41 F65 HTAB N44 F65 BOND LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 100 0.84 REM REM REM WGHT 0.056400 FVAR 0.30991 N1 5 0.549219 0.402033 0.517238 11.00000 0.03092 0.02619 = 0.01922 0.00290 0.01077 -0.00976 PT1 7 0.500000 0.500000 0.500000 10.50000 0.02478 0.01839 = 0.02478 0.00141 0.01246 -0.00065 C2 1 0.508764 0.359301 0.586016 11.00000 0.01992 0.03856 = 0.01305 -0.00065 0.00312 0.00502 AFIX 43 H2 2 0.457516 0.375544 0.629236 11.00000 -1.20000 AFIX 0 C3 1 0.540545 0.290639 0.595767 11.00000 0.02459 0.01365 = 0.01681 -0.00595 -0.00354 -0.00502 C4 1 0.498502 0.243915 0.669578 11.00000 0.02372 0.03053 = 0.03230 -0.00267 0.01260 -0.01581 C5 1 0.524307 0.175716 0.663951 11.00000 0.05225 0.01881 = 0.04142 0.00696 0.02619 0.00026 AFIX 43 H5 2 0.494587 0.143868 0.709478 11.00000 -1.20000 AFIX 0 C6 1 0.593466 0.153783 0.591978 11.00000 0.06343 0.02652 = 0.04883 0.00306 0.02283 0.01139 AFIX 43 H6 2 0.608207 0.106873 0.588286 11.00000 -1.20000 AFIX 0 C7 1 0.640256 0.196888 0.527305 11.00000 0.04771 0.02701 = 0.03854 -0.00580 0.01748 0.00447 AFIX 43 H7 2 0.690873 0.180679 0.483302 11.00000 -1.20000 AFIX 0 C8 1 0.612747 0.267208 0.525810 11.00000 0.01271 0.02433 = 0.02830 0.00307 -0.00522 0.01026 C9 1 0.657988 0.315250 0.461662 11.00000 0.02730 0.03289 = 0.02484 0.00443 0.01188 -0.00110 AFIX 43 H9 2 0.712732 0.301766 0.420657 11.00000 -1.20000 AFIX 0 C10 1 0.625017 0.379840 0.457488 11.00000 0.03335 0.03162 = 0.02952 0.00098 0.01241 -0.00109 AFIX 43 H10 2 0.655419 0.411076 0.411485 11.00000 -1.20000 AFIX 0 N11 5 0.431320 0.269160 0.741494 11.00000 0.04020 0.02097 = 0.03045 0.00181 0.01680 0.00040 H11 2 0.466617 0.314037 0.776532 11.00000 -1.20000 C12 1 0.365987 0.231743 0.801278 11.00000 0.03883 0.02407 = 0.04131 0.00567 0.01836 -0.00620 O13 6 0.355705 0.171699 0.795887 11.00000 0.04936 0.01877 = 0.04823 -0.00120 0.02589 -0.01085 N14 5 0.315507 0.271849 0.869696 11.00000 0.03654 0.02500 = 0.04064 0.00349 0.02154 0.00085 H14 2 0.328930 0.319428 0.904980 11.00000 -1.20000 C15 1 0.236971 0.240479 0.931823 11.00000 0.02947 0.03266 = 0.02925 0.00905 0.00849 0.00277 AFIX 23 H15A 2 0.278407 0.204957 0.987871 11.00000 -1.20000 H15B 2 0.172283 0.218940 0.870797 11.00000 -1.20000 AFIX 0 C16 1 0.191578 0.291279 1.001457 11.00000 0.03689 0.03624 = 0.04049 0.00480 0.01519 -0.01211 AFIX 23 H16A 2 0.148598 0.326228 0.945115 11.00000 -1.20000 H16B 2 0.256360 0.313573 1.061154 11.00000 -1.20000 AFIX 0 C17 1 0.113050 0.258827 1.067680 11.00000 0.05501 0.03663 = 0.05965 0.00676 0.03694 -0.00664 AFIX 137 H17A 2 0.154476 0.222753 1.120547 11.00000 -1.50000 H17B 2 0.045757 0.239875 1.008241 11.00000 -1.50000 H17C 2 0.088055 0.292834 1.117146 11.00000 -1.50000 AFIX 0 N31 5 0.358553 0.477395 0.366939 11.00000 0.03307 0.02947 = 0.02497 0.00798 0.01641 0.00585 C32 1 0.260104 0.459287 0.391648 11.00000 0.02956 0.01517 = 0.03587 0.00120 0.01895 -0.00358 AFIX 43 H32 2 0.261564 0.456559 0.475043 11.00000 -1.20000 AFIX 0 C33 1 0.157730 0.444392 0.307375 11.00000 0.03330 0.01708 = 0.03205 0.00626 0.00281 0.00472 C34 1 0.054488 0.426161 0.340041 11.00000 0.04472 0.02742 = 0.02812 -0.00379 -0.00110 0.00274 C35 1 -0.045833 0.415728 0.246586 11.00000 0.03781 0.04555 = 0.03217 0.01059 0.01302 0.00862 AFIX 43 H35 2 -0.115053 0.405096 0.266317 11.00000 -1.20000 AFIX 0 C36 1 -0.046589 0.420599 0.124452 11.00000 0.03785 0.05001 = 0.04873 -0.01238 0.01000 -0.01390 AFIX 43 H36 2 -0.116355 0.413697 0.062532 11.00000 -1.20000 AFIX 0 C37 1 0.054168 0.435530 0.092008 11.00000 0.04243 0.02958 = 0.03339 -0.00517 0.00174 -0.00042 AFIX 43 H37 2 0.052995 0.436567 0.008576 11.00000 -1.20000 AFIX 0 C38 1 0.156874 0.448966 0.182319 11.00000 0.02935 0.01379 = 0.03714 0.00055 0.00445 -0.00502 C39 1 0.258389 0.467360 0.156222 11.00000 0.03266 0.02602 = 0.02729 0.00902 0.00531 0.01137 AFIX 43 H39 2 0.259446 0.469678 0.073520 11.00000 -1.20000 AFIX 0 C40 1 0.357296 0.482313 0.245860 11.00000 0.02812 0.02680 = 0.02959 0.00248 0.01291 -0.01097 AFIX 43 H40 2 0.424468 0.495962 0.224674 11.00000 -1.20000 AFIX 0 N41 5 0.060978 0.422984 0.462691 11.00000 0.02653 0.04883 = 0.03161 -0.00456 0.01299 -0.00247 H41 2 0.134982 0.415549 0.530548 11.00000 -1.20000 C42 1 -0.028187 0.409329 0.516188 11.00000 0.03777 0.02863 = 0.03879 0.00120 0.00733 -0.01357 O43 6 -0.127350 0.399314 0.453901 11.00000 0.02168 0.11278 = 0.05754 0.01614 0.01028 -0.01144 N44 5 0.007229 0.406134 0.638630 11.00000 0.03747 0.04096 = 0.03546 0.00864 0.01928 0.00636 H44 2 0.094151 0.409835 0.674195 11.00000 -1.20000 C45 1 -0.070283 0.386659 0.708929 11.00000 0.02899 0.03895 = 0.05194 -0.00615 0.01915 0.00669 AFIX 23 H45A 2 -0.147895 0.404307 0.668243 11.00000 -1.20000 H45B 2 -0.044369 0.407949 0.790302 11.00000 -1.20000 AFIX 0 C46 1 -0.078079 0.312476 0.724625 11.00000 0.05457 0.02087 = 0.04565 -0.01020 0.01782 -0.00616 AFIX 23 H46A 2 -0.000005 0.294218 0.760973 11.00000 -1.20000 H46B 2 -0.108889 0.291284 0.643708 11.00000 -1.20000 AFIX 0 C47 1 -0.153951 0.293873 0.804643 11.00000 0.03987 0.05237 = 0.05549 0.01081 0.01469 -0.00293 AFIX 137 H47A 2 -0.234348 0.303142 0.761251 11.00000 -1.50000 H47B 2 -0.131901 0.320618 0.879634 11.00000 -1.50000 H47C 2 -0.144828 0.245791 0.824959 11.00000 -1.50000 AFIX 0 B61 3 0.324638 0.447762 0.779967 11.00000 0.05727 0.01483 = 0.05742 0.00912 0.03259 0.00111 F62 4 0.419586 0.408862 0.835549 11.00000 0.05543 0.03299 = 0.05357 -0.00070 0.00721 0.00186 F63 4 0.246214 0.447955 0.848771 11.00000 0.07254 0.10239 = 0.05034 -0.00102 0.03749 -0.00052 F64 4 0.358596 0.510147 0.758880 11.00000 0.07089 0.04662 = 0.07348 0.00575 0.02137 -0.01190 F65 4 0.271009 0.416562 0.669625 11.00000 0.05391 0.06459 = 0.03633 -0.01095 0.01485 -0.00389 HKLF 4 REM pag22_s2619_sn1002_a.res in P2(1)/c REM wR2 = 0.1601, GooF = S = 0.989, Restrained GooF = 0.989 for all data REM R1 = 0.0660 for 2732 Fo > 4sig(Fo) and 0.1254 for all 4655 data REM 372 parameters refined using 6 restraints END WGHT 0.0562 0.0000 REM Highest difference peak 1.420, deepest hole -1.939, 1-sigma level 0.199 Q1 1 0.5196 0.5289 0.5811 11.00000 0.05 1.42 Q2 1 0.4779 0.5282 0.4342 11.00000 0.05 1.29 Q3 1 0.4233 0.5004 0.4991 11.00000 0.05 1.26 Q4 1 0.4666 0.5269 0.3636 11.00000 0.05 1.24 Q5 1 0.3323 0.5346 0.3737 11.00000 0.05 0.97 Q6 1 0.5766 0.0950 0.6616 11.00000 0.05 0.91 Q7 1 0.3538 0.4997 0.3181 11.00000 0.05 0.88 Q8 1 0.1001 0.4890 0.2575 11.00000 0.05 0.81 Q9 1 0.4696 0.5322 0.2298 11.00000 0.05 0.78 Q10 1 0.1945 0.4994 0.6085 11.00000 0.05 0.77 ; _shelx_res_checksum 49791 _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 1.911 _oxdiff_exptl_absorpt_empirical_full_min 0.222 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 0.5492(8) 0.4020(4) 0.5172(7) 0.025(2) Uani 1 1 d . . . . . Pt1 Pt 0.500000 0.500000 0.500000 0.0215(2) Uani 1 2 d S . P . . C2 C 0.5088(9) 0.3593(5) 0.5860(9) 0.024(3) Uani 1 1 d . . . . . H2 H 0.457516 0.375544 0.629236 0.029 Uiso 1 1 calc R U . . . C3 C 0.5405(9) 0.2906(5) 0.5958(9) 0.020(2) Uani 1 1 d . . . . . C4 C 0.4985(10) 0.2439(5) 0.6696(10) 0.028(3) Uani 1 1 d . . . . . C5 C 0.5243(11) 0.1757(5) 0.6640(10) 0.035(3) Uani 1 1 d . . . . . H5 H 0.494587 0.143868 0.709478 0.042 Uiso 1 1 calc R U . . . C6 C 0.5935(12) 0.1538(6) 0.5920(11) 0.045(4) Uani 1 1 d . . . . . H6 H 0.608207 0.106873 0.588286 0.054 Uiso 1 1 calc R U . . . C7 C 0.6403(11) 0.1969(5) 0.5273(10) 0.037(3) Uani 1 1 d . . . . . H7 H 0.690873 0.180679 0.483302 0.044 Uiso 1 1 calc R U . . . C8 C 0.6127(9) 0.2672(5) 0.5258(9) 0.024(2) Uani 1 1 d . . . . . C9 C 0.6580(10) 0.3153(5) 0.4617(9) 0.027(3) Uani 1 1 d . . . . . H9 H 0.712732 0.301766 0.420657 0.033 Uiso 1 1 calc R U . . . C10 C 0.6250(10) 0.3798(5) 0.4575(10) 0.031(3) Uani 1 1 d . . . . . H10 H 0.655419 0.411076 0.411485 0.037 Uiso 1 1 calc R U . . . N11 N 0.4313(9) 0.2692(4) 0.7415(8) 0.029(2) Uani 1 1 d D . . . . H11 H 0.467(9) 0.314(4) 0.777(8) 0.035 Uiso 1 1 d D U . . . C12 C 0.3660(11) 0.2317(5) 0.8013(10) 0.033(3) Uani 1 1 d . . . . . O13 O 0.3557(7) 0.1717(3) 0.7959(7) 0.036(2) Uani 1 1 d . . . . . N14 N 0.3155(8) 0.2718(4) 0.8697(8) 0.032(2) Uani 1 1 d D . . . . H14 H 0.329(9) 0.319(3) 0.905(9) 0.038 Uiso 1 1 d D U . . . C15 C 0.2370(10) 0.2405(5) 0.9318(10) 0.030(3) Uani 1 1 d . . . . . H15A H 0.278407 0.204957 0.987871 0.036 Uiso 1 1 calc R U . . . H15B H 0.172283 0.218940 0.870797 0.036 Uiso 1 1 calc R U . . . C16 C 0.1916(11) 0.2913(5) 1.0015(10) 0.037(3) Uani 1 1 d . . . . . H16A H 0.148598 0.326228 0.945115 0.044 Uiso 1 1 calc R U . . . H16B H 0.256360 0.313573 1.061154 0.044 Uiso 1 1 calc R U . . . C17 C 0.1130(12) 0.2588(6) 1.0677(11) 0.046(4) Uani 1 1 d . . . . . H17A H 0.154476 0.222753 1.120547 0.069 Uiso 1 1 calc R U . . . H17B H 0.045757 0.239875 1.008241 0.069 Uiso 1 1 calc R U . . . H17C H 0.088055 0.292834 1.117146 0.069 Uiso 1 1 calc R U . . . N31 N 0.3586(8) 0.4774(4) 0.3669(8) 0.027(2) Uani 1 1 d . . . . . C32 C 0.2601(10) 0.4593(5) 0.3916(10) 0.025(3) Uani 1 1 d . . . . . H32 H 0.261564 0.456559 0.475043 0.030 Uiso 1 1 calc R U . . . C33 C 0.1577(10) 0.4444(5) 0.3074(10) 0.029(3) Uani 1 1 d . . . . . C34 C 0.0545(11) 0.4262(5) 0.3400(10) 0.036(3) Uani 1 1 d . . . . . C35 C -0.0458(11) 0.4157(6) 0.2466(10) 0.038(3) Uani 1 1 d . . . . . H35 H -0.115053 0.405096 0.266317 0.045 Uiso 1 1 calc R U . . . C36 C -0.0466(12) 0.4206(6) 0.1245(12) 0.046(3) Uani 1 1 d . . . . . H36 H -0.116355 0.413697 0.062532 0.055 Uiso 1 1 calc R U . . . C37 C 0.0542(11) 0.4355(5) 0.0920(11) 0.037(3) Uani 1 1 d . . . . . H37 H 0.052995 0.436567 0.008576 0.044 Uiso 1 1 calc R U . . . C38 C 0.1569(10) 0.4490(5) 0.1823(10) 0.028(3) Uani 1 1 d . . . . . C39 C 0.2584(10) 0.4674(5) 0.1562(10) 0.029(3) Uani 1 1 d . . . . . H39 H 0.259446 0.469678 0.073520 0.035 Uiso 1 1 calc R U . . . C40 C 0.3573(10) 0.4823(5) 0.2459(10) 0.027(3) Uani 1 1 d . . . . . H40 H 0.424468 0.495962 0.224674 0.033 Uiso 1 1 calc R U . . . N41 N 0.0610(9) 0.4230(5) 0.4627(9) 0.035(2) Uani 1 1 d D . . . . H41 H 0.135(6) 0.416(5) 0.531(7) 0.042 Uiso 1 1 d D U . . . C42 C -0.0282(11) 0.4093(6) 0.5162(11) 0.036(3) Uani 1 1 d . . . . . O43 O -0.1273(8) 0.3993(5) 0.4539(8) 0.064(3) Uani 1 1 d . . . . . N44 N 0.0072(9) 0.4061(5) 0.6386(9) 0.036(3) Uani 1 1 d D . . . . H44 H 0.094(5) 0.410(6) 0.674(9) 0.043 Uiso 1 1 d D U . . . C45 C -0.0703(10) 0.3867(5) 0.7089(11) 0.038(3) Uani 1 1 d . . . . . H45A H -0.147895 0.404307 0.668243 0.046 Uiso 1 1 calc R U . . . H45B H -0.044369 0.407949 0.790302 0.046 Uiso 1 1 calc R U . . . C46 C -0.0781(12) 0.3125(5) 0.7246(11) 0.040(3) Uani 1 1 d . . . . . H46A H -0.000005 0.294218 0.760973 0.047 Uiso 1 1 calc R U . . . H46B H -0.108889 0.291284 0.643708 0.047 Uiso 1 1 calc R U . . . C47 C -0.1540(11) 0.2939(6) 0.8046(12) 0.049(4) Uani 1 1 d . . . . . H47A H -0.234348 0.303142 0.761251 0.073 Uiso 1 1 calc R U . . . H47B H -0.131901 0.320618 0.879634 0.073 Uiso 1 1 calc R U . . . H47C H -0.144828 0.245791 0.824959 0.073 Uiso 1 1 calc R U . . . B61 B 0.3246(14) 0.4478(6) 0.7800(14) 0.040(4) Uani 1 1 d . . . . . F62 F 0.4196(6) 0.4089(3) 0.8355(6) 0.0489(19) Uani 1 1 d . . . . . F63 F 0.2462(8) 0.4480(4) 0.8488(7) 0.071(3) Uani 1 1 d . . . . . F64 F 0.3586(7) 0.5101(3) 0.7589(7) 0.063(2) Uani 1 1 d . . . . . F65 F 0.2710(6) 0.4166(4) 0.6696(6) 0.051(2) 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 0.031(5) 0.026(5) 0.019(5) 0.003(4) 0.011(5) -0.010(4) Pt1 0.0248(3) 0.0184(3) 0.0248(3) 0.0014(3) 0.0125(2) -0.0006(3) C2 0.020(6) 0.039(7) 0.013(6) -0.001(5) 0.003(5) 0.005(5) C3 0.025(6) 0.014(5) 0.017(6) -0.006(4) -0.004(5) -0.005(5) C4 0.024(7) 0.031(6) 0.032(7) -0.003(5) 0.013(6) -0.016(5) C5 0.052(9) 0.019(6) 0.041(7) 0.007(5) 0.026(7) 0.000(6) C6 0.063(10) 0.027(6) 0.049(9) 0.003(6) 0.023(8) 0.011(7) C7 0.048(9) 0.027(6) 0.039(7) -0.006(6) 0.017(7) 0.004(6) C8 0.013(6) 0.024(6) 0.028(6) 0.003(5) -0.005(5) 0.010(5) C9 0.027(7) 0.033(6) 0.025(6) 0.004(5) 0.012(6) -0.001(6) C10 0.033(7) 0.032(7) 0.030(7) 0.001(5) 0.012(6) -0.001(6) N11 0.040(6) 0.021(5) 0.030(6) 0.002(4) 0.017(5) 0.000(5) C12 0.039(8) 0.024(6) 0.041(7) 0.006(6) 0.018(6) -0.006(6) O13 0.049(6) 0.019(4) 0.048(5) -0.001(4) 0.026(5) -0.011(4) N14 0.037(6) 0.025(5) 0.041(6) 0.003(5) 0.022(5) 0.001(5) C15 0.029(7) 0.033(6) 0.029(7) 0.009(5) 0.008(6) 0.003(6) C16 0.037(8) 0.036(7) 0.040(8) 0.005(6) 0.015(6) -0.012(6) C17 0.055(10) 0.037(7) 0.060(9) 0.007(6) 0.037(8) -0.007(7) N31 0.033(6) 0.029(5) 0.025(5) 0.008(4) 0.016(5) 0.006(4) C32 0.030(7) 0.015(6) 0.036(7) 0.001(5) 0.019(6) -0.004(5) C33 0.033(8) 0.017(6) 0.032(7) 0.006(5) 0.003(6) 0.005(5) C34 0.045(9) 0.027(6) 0.028(7) -0.004(5) -0.001(7) 0.003(6) C35 0.038(8) 0.046(7) 0.032(7) 0.011(6) 0.013(7) 0.009(6) C36 0.038(9) 0.050(8) 0.049(9) -0.012(7) 0.010(7) -0.014(7) C37 0.042(8) 0.030(7) 0.033(7) -0.005(5) 0.002(6) 0.000(6) C38 0.029(7) 0.014(5) 0.037(7) 0.001(5) 0.004(6) -0.005(5) C39 0.033(7) 0.026(6) 0.027(7) 0.009(5) 0.005(6) 0.011(6) C40 0.028(7) 0.027(6) 0.030(6) 0.002(5) 0.013(6) -0.011(5) N41 0.027(6) 0.049(6) 0.032(6) -0.005(5) 0.013(5) -0.002(5) C42 0.038(9) 0.029(6) 0.039(8) 0.001(6) 0.007(7) -0.014(6) O43 0.022(5) 0.113(8) 0.058(6) 0.016(6) 0.010(5) -0.011(6) N44 0.037(7) 0.041(6) 0.035(7) 0.009(5) 0.019(6) 0.006(5) C45 0.029(7) 0.039(7) 0.052(8) -0.006(6) 0.019(7) 0.007(6) C46 0.055(9) 0.021(6) 0.046(8) -0.010(5) 0.018(7) -0.006(6) C47 0.040(9) 0.052(8) 0.055(9) 0.011(7) 0.015(7) -0.003(7) B61 0.057(11) 0.015(7) 0.057(11) 0.009(7) 0.033(9) 0.001(7) F62 0.055(5) 0.033(4) 0.054(5) -0.001(3) 0.007(4) 0.002(4) F63 0.073(6) 0.102(7) 0.050(5) -0.001(5) 0.037(5) -0.001(5) F64 0.071(6) 0.047(5) 0.073(5) 0.006(4) 0.021(5) -0.012(4) F65 0.054(5) 0.065(5) 0.036(4) -0.011(4) 0.015(4) -0.004(4) 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 -3 21 -9 0.0290 10 -13 -13 0.0386 -6 -8 15 0.0220 -10 18 10 0.0328 -16 2 0 0.0114 16 -1 0 0.0183 5 -25 4 0.0423 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 121.3(7) . . ? C2 N1 C10 119.9(9) . . ? C10 N1 Pt1 118.9(6) . . ? N1 Pt1 N1 180.0 3_666 . ? N31 Pt1 N1 88.5(3) 3_666 . ? N31 Pt1 N1 88.5(3) . 3_666 ? N31 Pt1 N1 91.5(3) 3_666 3_666 ? N31 Pt1 N1 91.5(3) . . ? N31 Pt1 N31 180.0 3_666 . ? N1 C2 H2 119.3 . . ? N1 C2 C3 121.4(9) . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 122.3(9) . . ? C2 C3 C8 118.0(9) . . ? C8 C3 C4 119.6(9) . . ? C5 C4 C3 118.5(9) . . ? C5 C4 N11 123.3(9) . . ? N11 C4 C3 118.2(9) . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.6(10) . . ? C6 C5 H5 119.7 . . ? C5 C6 H6 118.8 . . ? C7 C6 C5 122.4(10) . . ? C7 C6 H6 118.8 . . ? C6 C7 H7 120.3 . . ? C6 C7 C8 119.4(10) . . ? C8 C7 H7 120.3 . . ? C3 C8 C7 119.4(9) . . ? C9 C8 C3 117.6(9) . . ? C9 C8 C7 123.0(9) . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.8(10) . . ? C10 C9 H9 119.6 . . ? N1 C10 H10 119.1 . . ? C9 C10 N1 121.9(10) . . ? C9 C10 H10 119.1 . . ? C4 N11 H11 107(6) . . ? C12 N11 C4 126.8(9) . . ? C12 N11 H11 120(5) . . ? O13 C12 N11 124.7(10) . . ? O13 C12 N14 123.3(10) . . ? N14 C12 N11 112.0(9) . . ? C12 N14 H14 135(6) . . ? C12 N14 C15 118.6(9) . . ? C15 N14 H14 105(6) . . ? N14 C15 H15A 109.5 . . ? N14 C15 H15B 109.5 . . ? N14 C15 C16 110.9(9) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C15 C16 C17 111.0(9) . . ? H16A C16 H16B 108.0 . . ? C17 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C32 N31 Pt1 121.4(7) . . ? C32 N31 C40 117.6(10) . . ? C40 N31 Pt1 121.0(7) . . ? N31 C32 H32 117.0 . . ? N31 C32 C33 126.1(10) . . ? C33 C32 H32 117.0 . . ? C32 C33 C34 123.3(10) . . ? C32 C33 C38 116.3(10) . . ? C38 C33 C34 120.4(11) . . ? C35 C34 C33 118.2(10) . . ? N41 C34 C33 117.5(11) . . ? N41 C34 C35 124.3(11) . . ? C34 C35 H35 119.4 . . ? C34 C35 C36 121.3(11) . . ? C36 C35 H35 119.4 . . ? C35 C36 H36 119.5 . . ? C35 C36 C37 120.9(13) . . ? C37 C36 H36 119.5 . . ? C36 C37 H37 119.9 . . ? C36 C37 C38 120.3(11) . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 118.9(10) . . ? C39 C38 C33 117.9(11) . . ? C39 C38 C37 123.2(11) . . ? C38 C39 H39 118.8 . . ? C40 C39 C38 122.4(10) . . ? C40 C39 H39 118.8 . . ? N31 C40 H40 120.1 . . ? C39 C40 N31 119.7(10) . . ? C39 C40 H40 120.1 . . ? C34 N41 H41 125(6) . . ? C34 N41 C42 127.9(11) . . ? C42 N41 H41 105(6) . . ? O43 C42 N41 121.5(11) . . ? O43 C42 N44 124.9(11) . . ? N44 C42 N41 113.5(11) . . ? C42 N44 H44 114(6) . . ? C42 N44 C45 121.4(11) . . ? C45 N44 H44 124(6) . . ? N44 C45 H45A 108.8 . . ? N44 C45 H45B 108.8 . . ? N44 C45 C46 113.8(9) . . ? H45A C45 H45B 107.7 . . ? C46 C45 H45A 108.8 . . ? C46 C45 H45B 108.8 . . ? C45 C46 H46A 109.1 . . ? C45 C46 H46B 109.1 . . ? C45 C46 C47 112.6(9) . . ? H46A C46 H46B 107.8 . . ? C47 C46 H46A 109.1 . . ? C47 C46 H46B 109.1 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? F62 B61 F63 110.6(11) . . ? F62 B61 F65 106.7(10) . . ? F63 B61 F65 107.0(12) . . ? F64 B61 F62 109.8(12) . . ? F64 B61 F63 112.9(10) . . ? F64 B61 F65 109.6(11) . . ? 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 2.025(8) . ? N1 C2 1.337(12) . ? N1 C10 1.360(12) . ? Pt1 N31 2.002(10) 3_666 ? Pt1 N31 2.002(10) . ? C2 H2 0.9500 . ? C2 C3 1.410(13) . ? C3 C4 1.438(13) . ? C3 C8 1.416(13) . ? C4 C5 1.393(14) . ? C4 N11 1.399(13) . ? C5 H5 0.9500 . ? C5 C6 1.396(15) . ? C6 H6 0.9500 . ? C6 C7 1.353(15) . ? C7 H7 0.9500 . ? C7 C8 1.432(14) . ? C8 C9 1.402(13) . ? C9 H9 0.9500 . ? C9 C10 1.338(14) . ? C10 H10 0.9500 . ? N11 H11 1.02(6) . ? N11 C12 1.394(13) . ? C12 O13 1.197(12) . ? C12 N14 1.372(13) . ? N14 H14 1.02(6) . ? N14 C15 1.473(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.480(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.513(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N31 C32 1.348(13) . ? N31 C40 1.383(12) . ? C32 H32 0.9500 . ? C32 C33 1.375(16) . ? C33 C34 1.446(16) . ? C33 C38 1.429(14) . ? C34 C35 1.393(16) . ? C34 N41 1.384(13) . ? C35 H35 0.9500 . ? C35 C36 1.397(15) . ? C36 H36 0.9500 . ? C36 C37 1.401(16) . ? C37 H37 0.9500 . ? C37 C38 1.405(16) . ? C38 C39 1.391(15) . ? C39 H39 0.9500 . ? C39 C40 1.376(15) . ? C40 H40 0.9500 . ? N41 H41 1.02(6) . ? N41 C42 1.407(15) . ? C42 O43 1.231(14) . ? C42 N44 1.347(14) . ? N44 H44 1.02(6) . ? N44 C45 1.447(13) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.488(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.511(14) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? B61 F62 1.384(17) . ? B61 F63 1.391(15) . ? B61 F64 1.346(14) . ? B61 F65 1.393(17) . ? 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 F62 1.02(6) 2.13(8) 2.988(10) 141(8) . yes N14 H14 F62 1.02(6) 2.34(8) 3.064(11) 127(7) . yes N41 H41 F65 1.02(6) 1.95(6) 2.958(13) 170(9) . yes N44 H44 F65 1.02(6) 2.16(7) 3.122(12) 156(8) . 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 179.7(10) . . . . ? N1 C2 C3 C8 -2.9(15) . . . . ? Pt1 N1 C2 C3 178.3(8) . . . . ? Pt1 N1 C10 C9 -177.7(9) . . . . ? Pt1 N31 C32 C33 178.3(8) . . . . ? Pt1 N31 C40 C39 -179.1(7) . . . . ? C2 N1 C10 C9 2.4(17) . . . . ? C2 C3 C4 C5 173.2(11) . . . . ? C2 C3 C4 N11 -5.3(16) . . . . ? C2 C3 C8 C7 -175.8(10) . . . . ? C2 C3 C8 C9 6.8(15) . . . . ? C3 C4 C5 C6 2.6(18) . . . . ? C3 C4 N11 C12 167.5(11) . . . . ? C3 C8 C9 C10 -6.3(16) . . . . ? C4 C3 C8 C7 1.6(16) . . . . ? C4 C3 C8 C9 -175.8(10) . . . . ? C4 C5 C6 C7 1(2) . . . . ? C4 N11 C12 O13 -2(2) . . . . ? C4 N11 C12 N14 176.5(11) . . . . ? C5 C4 N11 C12 -11.0(19) . . . . ? C5 C6 C7 C8 -4(2) . . . . ? C6 C7 C8 C3 2.4(18) . . . . ? C6 C7 C8 C9 179.7(12) . . . . ? C7 C8 C9 C10 176.3(11) . . . . ? C8 C3 C4 C5 -4.1(16) . . . . ? C8 C3 C4 N11 177.4(10) . . . . ? C8 C9 C10 N1 1.7(18) . . . . ? C10 N1 C2 C3 -1.8(16) . . . . ? N11 C4 C5 C6 -178.9(12) . . . . ? N11 C12 N14 C15 175.8(10) . . . . ? C12 N14 C15 C16 179.7(11) . . . . ? O13 C12 N14 C15 -5.2(18) . . . . ? N14 C15 C16 C17 -178.7(10) . . . . ? N31 C32 C33 C34 -179.1(10) . . . . ? N31 C32 C33 C38 -0.2(15) . . . . ? C32 N31 C40 C39 -1.5(14) . . . . ? C32 C33 C34 C35 176.6(11) . . . . ? C32 C33 C34 N41 -0.8(16) . . . . ? C32 C33 C38 C37 -178.9(10) . . . . ? C32 C33 C38 C39 0.5(14) . . . . ? C33 C34 C35 C36 1.9(17) . . . . ? C33 C34 N41 C42 177.1(10) . . . . ? C33 C38 C39 C40 -1.3(15) . . . . ? C34 C33 C38 C37 0.1(15) . . . . ? C34 C33 C38 C39 179.4(10) . . . . ? C34 C35 C36 C37 0.6(18) . . . . ? C34 N41 C42 O43 -1.2(19) . . . . ? C34 N41 C42 N44 176.5(11) . . . . ? C35 C34 N41 C42 -0.1(18) . . . . ? C35 C36 C37 C38 -3.0(17) . . . . ? C36 C37 C38 C33 2.6(16) . . . . ? C36 C37 C38 C39 -176.7(11) . . . . ? C37 C38 C39 C40 178.0(10) . . . . ? C38 C33 C34 C35 -2.3(15) . . . . ? C38 C33 C34 N41 -179.7(9) . . . . ? C38 C39 C40 N31 1.8(16) . . . . ? C40 N31 C32 C33 0.7(15) . . . . ? N41 C34 C35 C36 179.1(11) . . . . ? N41 C42 N44 C45 -174.4(9) . . . . ? C42 N44 C45 C46 86.3(14) . . . . ? O43 C42 N44 C45 3.2(19) . . . . ? N44 C45 C46 C47 176.5(11) . . . . ? 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 -3.0001 21.0000 -9.0001 -0.9594 -0.0747 -0.2642 9.9999 -12.9999 -13.0000 -0.2357 -0.0350 0.9759 -5.9999 -8.0000 15.0001 0.8437 0.1862 -0.4597 -9.9999 17.9999 10.0000 -0.0247 -0.0040 -0.9924 -16.0002 2.0002 0.0000 -0.3399 0.7903 -0.4644 16.0002 -1.0002 -0.0000 0.3196 -0.8091 0.4418 5.0000 -24.9999 4.0001 0.8139 0.1379 0.5685