#------------------------------------------------------------------------------ #$Date: 2021-10-12 01:59:08 +0300 (Tue, 12 Oct 2021) $ #$Revision: 269892 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708541.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_7708541 loop_ _publ_author_name 'Dobrynin, Mikhail V.' 'Kasatkina, Svetlana' 'Baykov, Sergey' 'Savko, Polina' 'Antonov, Nikita' 'Mikherdov, Alexander S.' 'Boyarskiy, Vadim' 'Islamova, Regina M.' _publ_section_title ; Deprotonated diaminocarbene platinum complexes for thermoresponsive luminescent silicone materials: both catalysts and luminophores ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02823E _journal_year 2021 _chemical_formula_moiety 'C27 H30 Cl N5 O Pt' _chemical_formula_sum 'C27 H30 Cl N5 O Pt' _chemical_formula_weight 671.10 _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 geom _audit_creation_date 2021-04-25 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-08-10 deposited with the CCDC. 2021-10-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.3680(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.55950(10) _cell_length_b 29.0139(4) _cell_length_c 11.9767(2) _cell_measurement_reflns_used 7392 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 70.2220 _cell_measurement_theta_min 3.0280 _cell_volume 2575.32(7) _computing_cell_refinement 'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.992 _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 -82.00 -44.00 0.50 0.20 -- -38.82 120.00 -63.00 76 2 \w -78.00 -26.00 0.50 0.20 -- -38.82 155.00 94.00 104 3 \w 23.00 83.00 0.50 0.20 -- 38.82-155.00 55.00 120 4 \w 20.00 45.00 0.50 0.20 -- 38.82-120.00-147.00 50 5 \w 85.00 115.00 0.50 0.71 -- 100.00-155.00 55.00 60 6 \w 48.00 74.00 0.50 0.71 -- 100.00-120.00-147.00 52 7 \w 95.00 134.00 0.50 0.71 -- 100.00 120.00 -63.00 78 8 \w -56.00 -23.00 0.50 0.20 -- -38.82 54.00 -60.00 66 9 \w -19.00 14.00 0.50 0.20 -- -38.82 54.00 -60.00 66 10 \w -63.00 -27.00 0.50 0.20 -- -38.82 77.00-120.00 72 11 \w -3.00 27.00 0.50 0.20 -- -38.82 77.00-120.00 60 12 \w 3.00 29.00 0.50 0.20 -- -38.82 32.00 90.00 52 13 \w -44.00 -16.00 0.50 0.20 -- -38.82 32.00 90.00 56 14 \w -52.00 -15.00 0.50 0.20 -- -38.82 32.00-180.00 74 15 \w -105.00 -35.00 0.50 0.20 -- -38.82 -43.00-180.00 140 16 \w 21.00 91.00 0.50 0.20 -- 38.82-138.00 -30.00 140 17 \w 33.00 105.00 0.50 0.20 -- 38.82 32.00 -60.00 144 18 \w 70.00 104.00 0.50 0.20 -- 38.82 43.00 150.00 68 19 \w 26.00 56.00 0.50 0.20 -- 38.82 32.00 30.00 60 20 \w 33.00 62.00 0.50 0.20 -- 38.82 43.00 150.00 58 21 \w 26.00 57.00 0.50 0.71 -- 100.00 -93.00-150.00 62 22 \w 57.00 83.00 0.50 0.71 -- 100.00 178.00 0.00 52 23 \w 31.00 114.00 0.50 0.71 -- 100.00 -30.00-180.00 166 24 \w 86.00 113.00 0.50 0.71 -- 100.00 -77.00-120.00 54 25 \w 93.00 119.00 0.50 0.71 -- 100.00 77.00 -60.00 52 26 \w 31.00 107.00 0.50 0.71 -- 100.00-111.00 30.00 152 27 \w 101.00 140.00 0.50 0.71 -- 100.00 111.00 -90.00 78 28 \w 37.00 71.00 0.50 0.71 -- 100.00-111.00 -30.00 68 29 \w 93.00 118.00 0.50 0.71 -- 100.00-133.00-180.00 50 30 \w 80.00 157.00 0.50 0.71 -- 100.00 53.00 120.00 154 31 \w 35.00 62.00 0.50 0.71 -- 100.00 -77.00-120.00 54 32 \w 36.00 94.00 0.50 0.71 -- 100.00-133.00 -30.00 116 33 \w 47.00 77.00 0.50 0.71 -- 100.00-133.00-180.00 60 34 \w 84.00 109.00 0.50 0.71 -- 100.00 77.00-180.00 50 35 \w 88.00 157.00 0.50 0.71 -- 100.00 37.00 90.00 138 36 \w 100.00 139.00 0.50 0.71 -- 100.00 178.00 0.00 78 37 \w 57.00 105.00 0.50 0.71 -- 100.00 -93.00 150.00 96 38 \w 71.00 106.00 0.50 0.71 -- 100.00-111.00-120.00 70 39 \w 85.00 152.00 0.50 0.71 -- 100.00 93.00 120.00 134 40 \w 108.00 153.00 0.50 0.71 -- 100.00 77.00-120.00 90 41 \w 88.00 113.00 0.50 0.71 -- 100.00-133.00 0.00 50 42 \w 54.00 72.50 0.50 0.71 -- 100.00 -61.00-180.00 37 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0357665000 _diffrn_orient_matrix_UB_12 0.0140266000 _diffrn_orient_matrix_UB_13 0.1176207000 _diffrn_orient_matrix_UB_21 0.0343847000 _diffrn_orient_matrix_UB_22 0.0508362000 _diffrn_orient_matrix_UB_23 -0.0262335000 _diffrn_orient_matrix_UB_31 -0.2018476000 _diffrn_orient_matrix_UB_32 0.0061524000 _diffrn_orient_matrix_UB_33 -0.0518990000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14904 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.424 _diffrn_reflns_theta_min 3.046 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.378 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.731 _exptl_crystal_description prism _exptl_crystal_F_000 1320 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: 1,2-dichloroethane' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.159 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 323 _refine_ls_number_reflns 4890 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0281 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.9747P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.0717 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4399 _reflns_number_total 4890 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02823e2.cif _cod_data_source_block bsc-450 _cod_database_code 7708541 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C27 H30 Cl N5 O 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 0.396 _shelx_estimated_absorpt_t_min 0.209 _reflns_odcompleteness_completeness 98.18 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C2(H2), C18(H18), C11(H11), C1(H1), C4(H4), C9(H9), C19(H19), C20(H20), C10(H10) 1.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C23(H23A,H23B, H23C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C) ; _shelx_res_file ; TITL pols-31_a.res in P2(1)/c bsc-450.res created by SHELXL-2018/3 at 00:53:35 on 20-Apr-2021 REM Old TITL REM SHELXT solution in P2(1)/c: R1 0.054, Rweak 0.003, Alpha 0.026 REM 0.549 for 121 systematic absences, Orientation as input REM Formula found by SHELXT: C27 Cl N5 O Pt CELL 1.54184 7.5595 29.0139 11.9767 90 101.368 90 ZERR 4 0.0001 0.0004 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Pt UNIT 108 120 4 20 4 4 L.S. 10 PLAN 4 SIZE 0.1 0.2 0.14 TEMP -173(2) CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT 8 9 1 OMIT 8 7 4 OMIT 8 9 3 REM REM REM WGHT 0.032800 0.974700 FVAR 0.27705 PT1 6 0.747441 0.658563 0.350423 11.00000 0.01874 0.01157 = 0.01597 -0.00043 0.00241 -0.00133 CL1 3 0.933202 0.630633 0.522237 11.00000 0.02696 0.01851 = 0.01971 0.00434 -0.00142 -0.00301 O1 5 0.620082 0.751902 0.008198 11.00000 0.03035 0.02466 = 0.02209 0.00502 0.00758 0.00185 N1 4 0.867918 0.721871 0.361391 11.00000 0.01953 0.01524 = 0.01765 -0.00206 0.00477 -0.00080 N4 4 0.574346 0.562908 0.337332 11.00000 0.02454 0.01529 = 0.01957 0.00030 0.00156 -0.00088 N2 4 0.654755 0.733207 0.199688 11.00000 0.02351 0.01575 = 0.01962 -0.00109 0.00004 -0.00447 N3 4 0.461184 0.675936 0.136645 11.00000 0.02212 0.01224 = 0.02007 -0.00016 0.00212 -0.00063 N5 4 0.460691 0.792589 0.116854 11.00000 0.02759 0.01623 = 0.02273 0.00223 0.00441 -0.00032 C16 1 0.509521 0.517518 0.328562 11.00000 0.02825 0.01003 = 0.01723 0.00080 -0.00011 -0.00418 C6 1 0.597615 0.687401 0.211370 11.00000 0.02298 0.01225 = 0.01984 -0.00117 0.00641 0.00256 C15 1 0.632870 0.599611 0.335745 11.00000 0.01990 0.02041 = 0.01417 0.00063 0.00291 0.00097 C7 1 0.396846 0.630722 0.119013 11.00000 0.02121 0.01255 = 0.01449 0.00256 -0.00208 -0.00096 C12 1 0.482317 0.600388 0.055572 11.00000 0.02494 0.01884 = 0.01711 0.00062 -0.00230 0.00266 C5 1 0.797954 0.751226 0.276569 11.00000 0.02050 0.01701 = 0.01358 -0.00105 0.00158 0.00115 C17 1 0.352460 0.507535 0.369769 11.00000 0.02795 0.02034 = 0.01445 0.00299 -0.00152 -0.00150 C2 1 1.077523 0.780468 0.440827 11.00000 0.02288 0.02285 = 0.01979 -0.00209 -0.00214 -0.00406 AFIX 43 H2 2 1.176049 0.789674 0.498663 11.00000 -1.20000 AFIX 0 C8 1 0.234165 0.617992 0.152839 11.00000 0.02291 0.02322 = 0.01699 0.00255 -0.00117 -0.00093 C18 1 0.290160 0.462714 0.356373 11.00000 0.02603 0.02282 = 0.02292 0.00411 -0.00078 -0.00716 AFIX 43 H18 2 0.183672 0.454499 0.382540 11.00000 -1.20000 AFIX 0 C21 1 0.605701 0.484985 0.277811 11.00000 0.02796 0.01950 = 0.02048 -0.00016 0.00049 -0.00006 C24 1 0.576567 0.759452 0.098730 11.00000 0.02174 0.01486 = 0.02138 0.00300 0.00115 -0.00131 C26 1 0.403114 0.825855 0.025460 11.00000 0.02620 0.02705 = 0.03083 0.00950 0.00398 0.00324 AFIX 137 H26A 2 0.499120 0.848547 0.025397 11.00000 -1.50000 H26B 2 0.293734 0.841605 0.037514 11.00000 -1.50000 H26C 2 0.377836 0.809745 -0.047881 11.00000 -1.50000 AFIX 0 C11 1 0.405683 0.557490 0.028250 11.00000 0.03292 0.01823 = 0.02144 -0.00191 -0.00315 0.00545 AFIX 43 H11 2 0.462282 0.536727 -0.015057 11.00000 -1.20000 AFIX 0 C1 1 1.005227 0.737156 0.442646 11.00000 0.02052 0.02128 = 0.02228 -0.00050 0.00173 -0.00055 AFIX 43 H1 2 1.053845 0.717077 0.503655 11.00000 -1.20000 AFIX 0 C3 1 1.004980 0.811050 0.353015 11.00000 0.02417 0.01699 = 0.02338 -0.00078 0.00452 -0.00316 C4 1 0.864393 0.795537 0.269488 11.00000 0.02465 0.01876 = 0.02205 0.00066 0.00438 -0.00078 AFIX 43 H4 2 0.813668 0.815047 0.207745 11.00000 -1.20000 AFIX 0 C9 1 0.164302 0.574383 0.123900 11.00000 0.02806 0.02731 = 0.01922 0.00450 -0.00292 -0.00849 AFIX 43 H9 2 0.056229 0.565236 0.146901 11.00000 -1.20000 AFIX 0 C19 1 0.380109 0.429347 0.305357 11.00000 0.03740 0.01618 = 0.02971 -0.00067 -0.00015 -0.00783 AFIX 43 H19 2 0.334180 0.398802 0.296729 11.00000 -1.20000 AFIX 0 C27 1 1.074828 0.859316 0.349427 11.00000 0.03107 0.02044 = 0.02378 -0.00290 0.00232 -0.00576 AFIX 137 H27A 2 1.010091 0.879720 0.392824 11.00000 -1.50000 H27B 2 1.056013 0.869821 0.270195 11.00000 -1.50000 H27C 2 1.204007 0.859935 0.382917 11.00000 -1.50000 AFIX 0 C22 1 0.258993 0.544405 0.425527 11.00000 0.03186 0.02489 = 0.02045 0.00215 0.00612 -0.00143 AFIX 137 H22A 2 0.345967 0.558884 0.487029 11.00000 -1.50000 H22B 2 0.161110 0.530528 0.456898 11.00000 -1.50000 H22C 2 0.209181 0.567755 0.368876 11.00000 -1.50000 AFIX 0 C23 1 0.776654 0.498240 0.239906 11.00000 0.02977 0.02470 = 0.02535 -0.00271 0.00284 -0.00034 AFIX 137 H23A 2 0.750726 0.522528 0.182128 11.00000 -1.50000 H23B 2 0.826086 0.471261 0.207479 11.00000 -1.50000 H23C 2 0.864706 0.509579 0.305377 11.00000 -1.50000 AFIX 0 C20 1 0.536738 0.440443 0.266952 11.00000 0.03401 0.01676 = 0.02872 -0.00290 0.00316 0.00148 AFIX 43 H20 2 0.597434 0.417290 0.232848 11.00000 -1.20000 AFIX 0 C14 1 0.652116 0.615037 0.017303 11.00000 0.02623 0.02913 = 0.02618 -0.00421 0.00758 0.00367 AFIX 137 H14A 2 0.633368 0.645287 -0.019538 11.00000 -1.50000 H14B 2 0.681915 0.592416 -0.036887 11.00000 -1.50000 H14C 2 0.751502 0.616938 0.083445 11.00000 -1.50000 AFIX 0 C13 1 0.141967 0.651633 0.218010 11.00000 0.03043 0.03238 = 0.02494 -0.00080 0.01029 -0.00053 AFIX 137 H13A 2 0.225436 0.660845 0.287805 11.00000 -1.50000 H13B 2 0.035297 0.637070 0.237810 11.00000 -1.50000 H13C 2 0.105096 0.678905 0.170878 11.00000 -1.50000 AFIX 0 C25 1 0.400733 0.799801 0.223934 11.00000 0.03974 0.02888 = 0.03333 -0.00135 0.01374 0.00568 AFIX 137 H25A 2 0.427112 0.772252 0.271655 11.00000 -1.50000 H25B 2 0.270512 0.805663 0.208435 11.00000 -1.50000 H25C 2 0.464249 0.826340 0.263731 11.00000 -1.50000 AFIX 0 C10 1 0.248365 0.544008 0.062441 11.00000 0.04099 0.01413 = 0.02533 0.00114 -0.00851 -0.00616 AFIX 43 H10 2 0.199104 0.514226 0.043771 11.00000 -1.20000 AFIX 0 HKLF 4 REM pols-31_a.res in P2(1)/c REM wR2 = 0.0717, GooF = S = 1.098, Restrained GooF = 1.098 for all data REM R1 = 0.0281 for 4399 Fo > 4sig(Fo) and 0.0317 for all 4890 data REM 323 parameters refined using 0 restraints END WGHT 0.0328 0.9747 REM Highest difference peak 1.159, deepest hole -1.274, 1-sigma level 0.120 Q1 1 0.6762 0.6587 0.4077 11.00000 0.05 1.16 Q2 1 0.7452 0.6584 0.2613 11.00000 0.05 0.98 Q3 1 0.9119 0.6433 0.3356 11.00000 0.05 0.76 Q4 1 0.5802 0.6718 0.3480 11.00000 0.05 0.70 ; _shelx_res_checksum 32249 _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 1.389 _oxdiff_exptl_absorpt_empirical_full_min 0.782 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 0.74744(2) 0.65856(2) 0.35042(2) 0.01556(7) Uani 1 1 d . . . . . Cl1 Cl 0.93320(12) 0.63063(3) 0.52224(8) 0.02255(19) Uani 1 1 d . . . . . O1 O 0.6201(4) 0.75190(10) 0.0082(2) 0.0254(6) Uani 1 1 d . . . . . N1 N 0.8679(4) 0.72187(11) 0.3614(3) 0.0173(6) Uani 1 1 d . . . . . N4 N 0.5743(4) 0.56291(12) 0.3373(3) 0.0202(7) Uani 1 1 d . . . . . N2 N 0.6548(4) 0.73321(12) 0.1997(3) 0.0202(7) Uani 1 1 d . . . . . N3 N 0.4612(4) 0.67594(11) 0.1366(3) 0.0184(6) Uani 1 1 d . . . . . N5 N 0.4607(4) 0.79259(12) 0.1169(3) 0.0223(7) Uani 1 1 d . . . . . C16 C 0.5095(5) 0.51752(13) 0.3286(3) 0.0191(8) Uani 1 1 d . . . . . C6 C 0.5976(5) 0.68740(13) 0.2114(3) 0.0181(7) Uani 1 1 d . . . . . C15 C 0.6329(5) 0.59961(14) 0.3357(3) 0.0182(8) Uani 1 1 d . . . . . C7 C 0.3968(5) 0.63072(13) 0.1190(3) 0.0168(7) Uani 1 1 d . . . . . C12 C 0.4823(5) 0.60039(14) 0.0556(3) 0.0212(8) Uani 1 1 d . . . . . C5 C 0.7980(5) 0.75123(13) 0.2766(3) 0.0173(7) Uani 1 1 d . . . . . C17 C 0.3525(5) 0.50754(14) 0.3698(3) 0.0217(8) Uani 1 1 d . . . . . C2 C 1.0775(5) 0.78047(15) 0.4408(3) 0.0227(8) Uani 1 1 d . . . . . H2 H 1.176049 0.789674 0.498663 0.027 Uiso 1 1 calc R . . . . C8 C 0.2342(5) 0.61799(16) 0.1528(3) 0.0217(8) Uani 1 1 d . . . . . C18 C 0.2902(6) 0.46271(15) 0.3564(3) 0.0247(9) Uani 1 1 d . . . . . H18 H 0.183672 0.454499 0.382540 0.030 Uiso 1 1 calc R . . . . C21 C 0.6057(5) 0.48499(14) 0.2778(3) 0.0232(8) Uani 1 1 d . . . . . C24 C 0.5766(5) 0.75945(13) 0.0987(3) 0.0197(8) Uani 1 1 d . . . . . C26 C 0.4031(6) 0.82586(16) 0.0255(4) 0.0283(9) Uani 1 1 d . . . . . H26A H 0.499120 0.848547 0.025397 0.042 Uiso 1 1 calc GR . . . . H26B H 0.293734 0.841605 0.037514 0.042 Uiso 1 1 calc GR . . . . H26C H 0.377836 0.809745 -0.047881 0.042 Uiso 1 1 calc GR . . . . C11 C 0.4057(6) 0.55749(15) 0.0283(3) 0.0254(9) Uani 1 1 d . . . . . H11 H 0.462282 0.536727 -0.015057 0.030 Uiso 1 1 calc R . . . . C1 C 1.0052(5) 0.73716(15) 0.4426(3) 0.0217(8) Uani 1 1 d . . . . . H1 H 1.053845 0.717077 0.503655 0.026 Uiso 1 1 calc R . . . . C3 C 1.0050(5) 0.81105(14) 0.3530(3) 0.0215(8) Uani 1 1 d . . . . . C4 C 0.8644(5) 0.79554(14) 0.2695(3) 0.0219(8) Uani 1 1 d . . . . . H4 H 0.813668 0.815047 0.207745 0.026 Uiso 1 1 calc R . . . . C9 C 0.1643(6) 0.57438(16) 0.1239(3) 0.0259(9) Uani 1 1 d . . . . . H9 H 0.056229 0.565236 0.146901 0.031 Uiso 1 1 calc R . . . . C19 C 0.3801(6) 0.42935(15) 0.3054(4) 0.0287(9) Uani 1 1 d . . . . . H19 H 0.334180 0.398802 0.296729 0.034 Uiso 1 1 calc R . . . . C27 C 1.0748(6) 0.85932(15) 0.3494(4) 0.0255(9) Uani 1 1 d . . . . . H27A H 1.010091 0.879720 0.392824 0.038 Uiso 1 1 calc GR . . . . H27B H 1.056013 0.869821 0.270195 0.038 Uiso 1 1 calc GR . . . . H27C H 1.204007 0.859935 0.382917 0.038 Uiso 1 1 calc GR . . . . C22 C 0.2590(6) 0.54441(15) 0.4255(3) 0.0256(9) Uani 1 1 d . . . . . H22A H 0.345967 0.558884 0.487029 0.038 Uiso 1 1 calc GR . . . . H22B H 0.161110 0.530528 0.456898 0.038 Uiso 1 1 calc GR . . . . H22C H 0.209181 0.567755 0.368876 0.038 Uiso 1 1 calc GR . . . . C23 C 0.7767(5) 0.49824(15) 0.2399(4) 0.0270(9) Uani 1 1 d . . . . . H23A H 0.750726 0.522528 0.182128 0.040 Uiso 1 1 calc GR . . . . H23B H 0.826086 0.471261 0.207479 0.040 Uiso 1 1 calc GR . . . . H23C H 0.864706 0.509579 0.305377 0.040 Uiso 1 1 calc GR . . . . C20 C 0.5367(6) 0.44044(15) 0.2670(4) 0.0269(9) Uani 1 1 d . . . . . H20 H 0.597434 0.417290 0.232848 0.032 Uiso 1 1 calc R . . . . C14 C 0.6521(5) 0.61504(16) 0.0173(4) 0.0269(9) Uani 1 1 d . . . . . H14A H 0.633368 0.645287 -0.019538 0.040 Uiso 1 1 calc GR . . . . H14B H 0.681915 0.592416 -0.036887 0.040 Uiso 1 1 calc GR . . . . H14C H 0.751502 0.616938 0.083445 0.040 Uiso 1 1 calc GR . . . . C13 C 0.1420(6) 0.65163(16) 0.2180(4) 0.0286(9) Uani 1 1 d . . . . . H13A H 0.225436 0.660845 0.287805 0.043 Uiso 1 1 calc GR . . . . H13B H 0.035297 0.637070 0.237810 0.043 Uiso 1 1 calc GR . . . . H13C H 0.105096 0.678905 0.170878 0.043 Uiso 1 1 calc GR . . . . C25 C 0.4007(6) 0.79980(17) 0.2239(4) 0.0331(10) Uani 1 1 d . . . . . H25A H 0.427112 0.772252 0.271655 0.050 Uiso 1 1 calc GR . . . . H25B H 0.270512 0.805663 0.208435 0.050 Uiso 1 1 calc GR . . . . H25C H 0.464249 0.826340 0.263731 0.050 Uiso 1 1 calc GR . . . . C10 C 0.2484(6) 0.54401(14) 0.0624(4) 0.0289(9) Uani 1 1 d . . . . . H10 H 0.199104 0.514226 0.043771 0.035 Uiso 1 1 calc R . . . . 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 0.01874(9) 0.01157(10) 0.01597(10) -0.00043(5) 0.00241(6) -0.00133(6) Cl1 0.0270(4) 0.0185(4) 0.0197(4) 0.0043(4) -0.0014(3) -0.0030(4) O1 0.0303(14) 0.0247(15) 0.0221(14) 0.0050(12) 0.0076(12) 0.0019(12) N1 0.0195(14) 0.0152(15) 0.0177(14) -0.0021(13) 0.0048(12) -0.0008(13) N4 0.0245(15) 0.0153(17) 0.0196(15) 0.0003(13) 0.0016(13) -0.0009(14) N2 0.0235(15) 0.0157(16) 0.0196(15) -0.0011(14) 0.0000(13) -0.0045(13) N3 0.0221(15) 0.0122(15) 0.0201(15) -0.0002(13) 0.0021(13) -0.0006(13) N5 0.0276(16) 0.0162(16) 0.0227(16) 0.0022(14) 0.0044(13) -0.0003(14) C16 0.0283(18) 0.0100(17) 0.0172(17) 0.0008(14) -0.0001(15) -0.0042(15) C6 0.0230(17) 0.0122(17) 0.0198(17) -0.0012(15) 0.0064(15) 0.0026(15) C15 0.0199(16) 0.020(2) 0.0142(16) 0.0006(15) 0.0029(14) 0.0010(16) C7 0.0212(17) 0.0125(17) 0.0145(16) 0.0026(14) -0.0021(14) -0.0010(15) C12 0.0249(18) 0.0188(19) 0.0171(17) 0.0006(15) -0.0023(15) 0.0027(16) C5 0.0205(16) 0.0170(18) 0.0136(16) -0.0011(14) 0.0016(14) 0.0011(15) C17 0.0279(18) 0.020(2) 0.0145(17) 0.0030(15) -0.0015(15) -0.0015(17) C2 0.0229(18) 0.023(2) 0.0198(18) -0.0021(16) -0.0021(15) -0.0041(16) C8 0.0229(18) 0.023(2) 0.0170(18) 0.0026(15) -0.0012(15) -0.0009(16) C18 0.0260(18) 0.023(2) 0.023(2) 0.0041(16) -0.0008(16) -0.0072(17) C21 0.0280(18) 0.020(2) 0.0205(18) -0.0002(16) 0.0005(16) -0.0001(17) C24 0.0217(17) 0.0149(18) 0.0214(18) 0.0030(16) 0.0011(15) -0.0013(15) C26 0.0262(19) 0.027(2) 0.031(2) 0.0095(19) 0.0040(17) 0.0032(18) C11 0.033(2) 0.0182(19) 0.0214(19) -0.0019(17) -0.0032(16) 0.0055(17) C1 0.0205(17) 0.021(2) 0.0223(18) -0.0005(16) 0.0017(15) -0.0005(16) C3 0.0242(17) 0.0170(19) 0.0234(19) -0.0008(16) 0.0045(15) -0.0032(16) C4 0.0247(18) 0.0188(19) 0.0220(19) 0.0007(16) 0.0044(15) -0.0008(16) C9 0.0281(19) 0.027(2) 0.0192(19) 0.0045(17) -0.0029(16) -0.0085(18) C19 0.037(2) 0.016(2) 0.030(2) -0.0007(18) -0.0001(18) -0.0078(18) C27 0.031(2) 0.020(2) 0.024(2) -0.0029(17) 0.0023(17) -0.0058(17) C22 0.032(2) 0.025(2) 0.0204(19) 0.0021(17) 0.0061(16) -0.0014(18) C23 0.0298(19) 0.025(2) 0.025(2) -0.0027(18) 0.0028(17) -0.0003(18) C20 0.034(2) 0.017(2) 0.029(2) -0.0029(17) 0.0032(17) 0.0015(18) C14 0.0262(19) 0.029(2) 0.026(2) -0.0042(18) 0.0076(16) 0.0037(18) C13 0.030(2) 0.032(2) 0.025(2) -0.0008(19) 0.0103(18) -0.0005(19) C25 0.040(2) 0.029(2) 0.033(2) -0.001(2) 0.0137(19) 0.006(2) C10 0.041(2) 0.0141(19) 0.025(2) 0.0011(17) -0.0085(18) -0.0062(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 Cl1 94.05(9) . . ? C6 Pt1 Cl1 175.11(11) . . ? C6 Pt1 N1 81.36(14) . . ? C15 Pt1 Cl1 87.39(11) . . ? C15 Pt1 N1 178.42(14) . . ? C15 Pt1 C6 97.22(16) . . ? C5 N1 Pt1 114.5(2) . . ? C1 N1 Pt1 127.7(3) . . ? C1 N1 C5 117.8(3) . . ? C15 N4 C16 174.0(4) . . ? C6 N2 C24 119.6(3) . . ? C5 N2 C6 120.4(3) . . ? C5 N2 C24 119.6(3) . . ? C6 N3 C7 124.2(3) . . ? C24 N5 C26 117.3(3) . . ? C24 N5 C25 124.7(3) . . ? C25 N5 C26 117.8(3) . . ? N4 C16 C17 118.4(4) . . ? C21 C16 N4 117.5(3) . . ? C21 C16 C17 124.1(4) . . ? N2 C6 Pt1 110.0(3) . . ? N3 C6 Pt1 136.4(3) . . ? N3 C6 N2 113.5(3) . . ? N4 C15 Pt1 173.1(3) . . ? N3 C7 C12 119.1(3) . . ? N3 C7 C8 119.7(4) . . ? C12 C7 C8 120.7(4) . . ? C7 C12 C14 120.0(4) . . ? C11 C12 C7 118.5(4) . . ? C11 C12 C14 121.6(4) . . ? N1 C5 N2 113.7(3) . . ? N1 C5 C4 122.5(3) . . ? N2 C5 C4 123.8(3) . . ? C16 C17 C22 120.8(4) . . ? C18 C17 C16 116.5(4) . . ? C18 C17 C22 122.7(4) . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.6(3) . . ? C3 C2 H2 120.2 . . ? C7 C8 C13 119.7(4) . . ? C9 C8 C7 118.3(4) . . ? C9 C8 C13 121.9(4) . . ? C17 C18 H18 119.3 . . ? C17 C18 C19 121.4(4) . . ? C19 C18 H18 119.3 . . ? C16 C21 C23 120.6(4) . . ? C20 C21 C16 116.7(4) . . ? C20 C21 C23 122.6(4) . . ? O1 C24 N2 120.8(3) . . ? O1 C24 N5 124.9(4) . . ? N5 C24 N2 114.3(3) . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C12 C11 H11 119.1 . . ? C12 C11 C10 121.8(4) . . ? C10 C11 H11 119.1 . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C2 C3 C27 121.6(4) . . ? C4 C3 C2 117.9(4) . . ? C4 C3 C27 120.5(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.2 . . ? C8 C9 H9 119.3 . . ? C10 C9 C8 121.5(4) . . ? C10 C9 H9 119.3 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.4(4) . . ? C20 C19 H19 119.8 . . ? C3 C27 H27A 109.5 . . ? C3 C27 H27B 109.5 . . ? C3 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C20 H20 119.6 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C11 C10 H10 120.4 . . ? C9 C10 C11 119.2(4) . . ? C9 C10 H10 120.4 . . ? 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 Cl1 2.3925(9) . ? Pt1 N1 2.043(3) . ? Pt1 C6 2.003(4) . ? Pt1 C15 1.910(4) . ? O1 C24 1.213(5) . ? N1 C5 1.351(5) . ? N1 C1 1.350(5) . ? N4 C16 1.402(5) . ? N4 C15 1.155(5) . ? N2 C6 1.413(5) . ? N2 C5 1.378(5) . ? N2 C24 1.452(5) . ? N3 C6 1.269(5) . ? N3 C7 1.401(5) . ? N5 C24 1.347(5) . ? N5 C26 1.460(5) . ? N5 C25 1.457(6) . ? C16 C17 1.403(6) . ? C16 C21 1.401(6) . ? C7 C12 1.401(6) . ? C7 C8 1.418(5) . ? C12 C11 1.385(6) . ? C12 C14 1.507(6) . ? C5 C4 1.389(6) . ? C17 C18 1.382(6) . ? C17 C22 1.508(6) . ? C2 H2 0.9500 . ? C2 C1 1.372(6) . ? C2 C3 1.402(6) . ? C8 C9 1.388(6) . ? C8 C13 1.504(6) . ? C18 H18 0.9500 . ? C18 C19 1.392(7) . ? C21 C23 1.502(6) . ? C21 C20 1.390(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C11 H11 0.9500 . ? C11 C10 1.388(7) . ? C1 H1 0.9500 . ? C3 C4 1.383(6) . ? C3 C27 1.500(6) . ? C4 H4 0.9500 . ? C9 H9 0.9500 . ? C9 C10 1.381(7) . ? C19 H19 0.9500 . ? C19 C20 1.390(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C20 H20 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C10 H10 0.9500 . ? 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 Pt1 N1 C5 N2 1.5(4) . . . . ? Pt1 N1 C5 C4 -179.2(3) . . . . ? Pt1 N1 C1 C2 179.2(3) . . . . ? N1 C5 C4 C3 -1.4(6) . . . . ? N4 C16 C17 C18 178.1(3) . . . . ? N4 C16 C17 C22 -1.9(5) . . . . ? N4 C16 C21 C23 2.9(5) . . . . ? N4 C16 C21 C20 -178.3(3) . . . . ? N2 C5 C4 C3 177.8(4) . . . . ? N3 C7 C12 C11 -173.1(3) . . . . ? N3 C7 C12 C14 6.1(5) . . . . ? N3 C7 C8 C9 173.6(3) . . . . ? N3 C7 C8 C13 -6.2(5) . . . . ? C16 C17 C18 C19 0.5(6) . . . . ? C16 C21 C20 C19 -0.2(6) . . . . ? C6 N2 C5 N1 -2.1(5) . . . . ? C6 N2 C5 C4 178.6(4) . . . . ? C6 N2 C24 O1 -75.1(5) . . . . ? C6 N2 C24 N5 107.0(4) . . . . ? C6 N3 C7 C12 -80.1(5) . . . . ? C6 N3 C7 C8 107.7(4) . . . . ? C7 N3 C6 Pt1 -15.4(6) . . . . ? C7 N3 C6 N2 169.5(3) . . . . ? C7 C12 C11 C10 -0.3(6) . . . . ? C7 C8 C9 C10 -0.8(6) . . . . ? C12 C7 C8 C9 1.5(5) . . . . ? C12 C7 C8 C13 -178.2(4) . . . . ? C12 C11 C10 C9 1.0(6) . . . . ? C5 N1 C1 C2 -1.4(6) . . . . ? C5 N2 C6 Pt1 1.6(4) . . . . ? C5 N2 C6 N3 178.0(3) . . . . ? C5 N2 C24 O1 97.4(5) . . . . ? C5 N2 C24 N5 -80.4(4) . . . . ? C17 C16 C21 C23 -177.7(4) . . . . ? C17 C16 C21 C20 1.1(6) . . . . ? C17 C18 C19 C20 0.4(6) . . . . ? C2 C3 C4 C5 1.4(6) . . . . ? C8 C7 C12 C11 -1.0(5) . . . . ? C8 C7 C12 C14 178.1(3) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C18 C19 C20 C21 -0.5(7) . . . . ? C21 C16 C17 C18 -1.2(6) . . . . ? C21 C16 C17 C22 178.7(4) . . . . ? C24 N2 C6 Pt1 174.1(3) . . . . ? C24 N2 C6 N3 -9.5(5) . . . . ? C24 N2 C5 N1 -174.6(3) . . . . ? C24 N2 C5 C4 6.1(6) . . . . ? C26 N5 C24 O1 -9.0(6) . . . . ? C26 N5 C24 N2 168.8(3) . . . . ? C1 N1 C5 N2 -178.0(3) . . . . ? C1 N1 C5 C4 1.3(5) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C1 C2 C3 C27 177.8(4) . . . . ? C3 C2 C1 N1 1.5(6) . . . . ? C27 C3 C4 C5 -177.9(4) . . . . ? C22 C17 C18 C19 -179.5(4) . . . . ? C23 C21 C20 C19 178.6(4) . . . . ? C14 C12 C11 C10 -179.4(4) . . . . ? C13 C8 C9 C10 178.9(4) . . . . ? C25 N5 C24 O1 176.2(4) . . . . ? C25 N5 C24 N2 -6.0(5) . . . . ?