#------------------------------------------------------------------------------ #$Date: 2021-02-05 01:22:55 +0200 (Fri, 05 Feb 2021) $ #$Revision: 261711 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557791.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_1557791 loop_ _publ_author_name 'Kobayashi, Atsushi' 'Imada, Shin-Ichiro' 'Wang, Dongjin' 'Nagao, Yuki' 'Yoshida, Masaki' 'Kato, Masako' _publ_section_title ; Cooperative phenomenon of vapochromism and proton conduction of luminescent Pt(ii) complexes for the visualisation of proton conductivity. ; _journal_name_full 'Faraday discussions' _journal_page_first 184 _journal_page_last 196 _journal_paper_doi 10.1039/d0fd00001a _journal_volume 225 _journal_year 2021 _chemical_formula_moiety 'C20 H14 Cl N4 Pt, Cl, H2 O' _chemical_formula_sum 'C20 H16 Cl2 N4 O Pt' _chemical_formula_weight 595.36 _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 dual _audit_creation_date 2020-01-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-06 deposited with the CCDC. 2020-04-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.5420(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.30460(10) _cell_length_b 21.6781(3) _cell_length_c 15.9776(2) _cell_measurement_reflns_used 7650 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 75.3120 _cell_measurement_theta_min 3.4290 _cell_volume 1831.55(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _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 -50.00 -8.00 0.50 0.48 -- -42.80 104.00-135.00 84 2 \w -1.00 84.00 0.50 0.48 -- 42.80-104.00 123.00 170 3 \w -107.00 -82.00 0.50 0.80 -- -84.50-104.00 123.00 50 4 \w -71.00 -38.00 0.50 0.80 -- -84.50 104.00-135.00 66 5 \w 49.00 109.00 0.50 0.80 -- 108.63-104.00 123.00 120 6 \w 86.00 149.00 0.50 0.80 -- 108.63 104.00-135.00 126 7 \w -104.00 -70.00 0.50 0.48 -- -42.80-125.00 -90.00 68 8 \w -103.00 -72.00 0.50 0.48 -- -42.80-125.00-150.00 62 9 \w 22.00 70.00 0.50 0.48 -- 42.80 57.00 -30.00 96 10 \w 76.00 117.00 0.50 0.48 -- 42.80 125.00 -30.00 82 11 \w 87.00 116.00 0.50 0.48 -- 42.80 57.00 -30.00 58 12 \w 91.00 116.00 0.50 0.80 -- 108.63-125.00 -30.00 50 13 \w 35.00 63.00 0.50 0.80 -- 108.63-125.00 -30.00 56 14 \w 35.00 66.00 0.50 0.80 -- 108.63 -30.00 150.00 62 15 \w 76.00 138.00 0.50 0.80 -- 108.63 -77.00 150.00 124 16 \w 34.00 59.00 0.50 0.80 -- 108.63 -30.00 -60.00 50 17 \w 30.00 60.00 0.50 0.80 -- 108.63 -30.00 0.00 60 18 \w 34.00 60.00 0.50 0.80 -- 108.63 -45.00 90.00 52 19 \w 36.00 117.00 0.50 0.80 -- 108.63 -61.00 -90.00 162 20 \w 37.00 66.00 0.50 0.80 -- 108.63 -30.00 60.00 58 21 \w 47.00 115.00 0.50 0.80 -- 108.63-125.00 60.00 136 22 \w 30.00 56.00 0.50 0.80 -- 108.63 -30.00 90.00 52 23 \w 44.00 77.00 0.50 0.80 -- 108.63 -45.00 -30.00 66 24 \w 39.00 78.00 0.50 0.80 -- 108.63 -45.00 -90.00 78 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0032831000 _diffrn_orient_matrix_UB_12 0.0681334000 _diffrn_orient_matrix_UB_13 0.0274478000 _diffrn_orient_matrix_UB_21 0.2779960000 _diffrn_orient_matrix_UB_22 -0.0067545000 _diffrn_orient_matrix_UB_23 0.0347809000 _diffrn_orient_matrix_UB_31 0.0874367000 _diffrn_orient_matrix_UB_32 0.0189783000 _diffrn_orient_matrix_UB_33 -0.0859679000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9949 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.024 _diffrn_reflns_theta_max 67.024 _diffrn_reflns_theta_min 3.443 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 17.184 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.58908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.159 _exptl_crystal_description plate _exptl_crystal_F_000 1140 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.634 _refine_diff_density_min -4.067 _refine_diff_density_rms 0.251 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 3262 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0432 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.1562P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1223 _refine_ls_wR_factor_ref 0.1242 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3044 _reflns_number_total 3262 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL o-ptpy2_a.res in P2(1)/c o-ptpy2.res created by SHELXL-2018/3 at 13:23:53 on 06-Jan-2020 REM Old TITL o-ptpy2_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.056, Rweak 0.004, Alpha 0.029 REM 0.617 for 109 systematic absences, Orientation as input REM Formula found by SHELXT: C21 Cl2 N4 Pt CELL 1.54184 5.3046 21.6781 15.9776 90 94.542 90 ZERR 4 0.0001 0.0003 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Pt UNIT 80 68 8 16 4 4 L.S. 25 PLAN 20 BOND LIST 4 fmap 2 acta REM REM REM WGHT 0.102000 0.156200 FVAR 0.22404 PT1 6 0.917660 0.459097 0.345972 11.00000 0.01580 0.01701 = 0.01942 -0.00111 0.00222 -0.00009 CL1 3 1.238681 0.530929 0.364188 11.00000 0.02233 0.02510 = 0.03059 -0.00349 0.00324 -0.00612 CL2 3 -0.569071 0.314388 0.035566 11.00000 0.03077 0.03061 = 0.02747 -0.00137 -0.00437 -0.00012 N1 4 1.008769 0.406633 0.448879 11.00000 0.01724 0.01816 = 0.02284 -0.00459 0.00421 -0.00200 N3 4 0.741873 0.491521 0.238785 11.00000 0.02082 0.01899 = 0.02285 0.00412 0.00393 0.00453 N2 4 0.649713 0.398489 0.330403 11.00000 0.01497 0.01787 = 0.01830 0.00041 0.00013 0.00464 AFIX 6 O1 5 -0.069002 0.392994 0.051091 11.00000 0.02838 0.03937 = 0.06434 0.00384 -0.00839 -0.00275 H1A 2 -0.209643 0.374315 0.052086 11.00000 -1.50000 H1B 2 0.040604 0.364315 0.052857 11.00000 -1.50000 AFIX 0 N4 4 -0.097848 0.275831 0.229509 11.00000 0.02195 0.02888 = 0.01828 -0.00077 0.00120 -0.00114 C5 1 0.852825 0.357064 0.454362 11.00000 0.01903 0.02108 = 0.01353 -0.00039 0.00050 -0.00051 C6 1 0.644310 0.352820 0.387393 11.00000 0.01400 0.01876 = 0.01973 -0.00330 0.00668 -0.00180 C1 1 1.207049 0.414117 0.506220 11.00000 0.01614 0.02407 = 0.02250 -0.00615 0.00172 -0.00212 AFIX 43 H1 2 1.310285 0.448549 0.502753 11.00000 -1.20000 AFIX 0 C8 1 0.274042 0.312740 0.309856 11.00000 0.01747 0.02061 = 0.01758 -0.00261 0.00420 0.00844 C10 1 0.484353 0.403513 0.262663 11.00000 0.01556 0.02453 = 0.01464 -0.00332 -0.00004 0.00306 C16 1 0.064850 0.267451 0.297685 11.00000 0.02174 0.02052 = 0.01593 -0.00499 0.00223 -0.00158 C11 1 0.533428 0.457346 0.210461 11.00000 0.01428 0.02049 = 0.02529 -0.00243 0.00357 0.00367 C7 1 0.453590 0.309120 0.378779 11.00000 0.01742 0.01826 = 0.01762 0.00109 0.00077 0.00546 AFIX 43 H7 2 0.444908 0.277804 0.418231 11.00000 -1.20000 AFIX 0 C9 1 0.290867 0.360443 0.251083 11.00000 0.01529 0.02213 = 0.01705 -0.00240 -0.00001 0.00256 AFIX 43 H9 2 0.173478 0.363171 0.204812 11.00000 -1.20000 AFIX 0 C17 1 0.038123 0.219347 0.354188 11.00000 0.01904 0.02411 = 0.02265 0.00174 -0.00885 0.00160 AFIX 43 H17 2 0.154120 0.213924 0.400366 11.00000 -1.20000 AFIX 0 C3 1 1.103416 0.321756 0.575366 11.00000 0.02051 0.02902 = 0.02186 0.00255 0.00432 0.00199 AFIX 43 H3 2 1.136794 0.293214 0.618270 11.00000 -1.20000 AFIX 0 C19 1 -0.330496 0.187151 0.269427 11.00000 0.02331 0.02644 = 0.02782 -0.00406 0.00114 -0.00531 AFIX 43 H19 2 -0.464126 0.159959 0.257498 11.00000 -1.20000 AFIX 0 C20 1 -0.291668 0.236672 0.216135 11.00000 0.02066 0.03216 = 0.01966 -0.00366 -0.00033 0.00197 AFIX 43 H20 2 -0.405151 0.242683 0.169438 11.00000 -1.20000 AFIX 0 C4 1 0.897228 0.313468 0.517805 11.00000 0.01789 0.02444 = 0.02631 -0.00268 0.00291 0.00126 AFIX 43 H4 2 0.790951 0.279613 0.521411 11.00000 -1.20000 AFIX 0 C12 1 0.382714 0.474546 0.140195 11.00000 0.03322 0.02186 = 0.02372 -0.00476 0.00656 0.00186 AFIX 43 H12 2 0.241358 0.451265 0.122281 11.00000 -1.20000 AFIX 0 C13 1 0.443994 0.526817 0.096606 11.00000 0.03490 0.02712 = 0.02368 0.00143 0.00376 0.00582 AFIX 43 H13 2 0.343087 0.539186 0.049332 11.00000 -1.20000 AFIX 0 C2 1 1.260175 0.372336 0.569364 11.00000 0.02454 0.03470 = 0.02009 -0.00498 -0.00170 -0.00192 AFIX 43 H2 2 1.399628 0.377850 0.607699 11.00000 -1.20000 AFIX 0 C18 1 -0.168339 0.179368 0.339519 11.00000 0.02177 0.02282 = 0.03118 0.00220 -0.00085 -0.00024 AFIX 43 H18 2 -0.194855 0.147767 0.377197 11.00000 -1.20000 AFIX 0 C14 1 0.656053 0.560629 0.123626 11.00000 0.03328 0.02621 = 0.02994 0.00964 0.00466 0.00479 AFIX 43 H14 2 0.701210 0.595409 0.094188 11.00000 -1.20000 AFIX 0 C15 1 0.800250 0.541906 0.195229 11.00000 0.02882 0.02475 = 0.02568 -0.00104 0.00154 -0.00307 AFIX 43 H15 2 0.941820 0.564911 0.213731 11.00000 -1.20000 AFIX 0 HKLF 4 REM o-ptpy2_a.res in P2(1)/c REM wR2 = 0.1242, GooF = S = 1.035, Restrained GooF = 1.035 for all data REM R1 = 0.0432 for 3044 Fo > 4sig(Fo) and 0.0451 for all 3262 data REM 256 parameters refined using 0 restraints END WGHT 0.1021 0.1171 REM Highest difference peak 1.634, deepest hole -4.067, 1-sigma level 0.251 Q1 1 -0.0088 0.3423 0.1627 11.00000 0.05 1.63 Q2 1 1.0533 0.3886 0.3388 11.00000 0.05 1.53 Q3 1 1.0517 0.5305 0.3378 11.00000 0.05 1.51 Q4 1 0.7810 0.5299 0.3614 11.00000 0.05 1.38 Q5 1 0.7786 0.3899 0.3532 11.00000 0.05 1.27 Q6 1 0.8990 0.4591 0.2764 11.00000 0.05 1.19 Q7 1 0.9469 0.4584 0.4175 11.00000 0.05 1.13 Q8 1 0.8568 0.3706 0.2954 11.00000 0.05 1.05 Q9 1 0.9916 0.3781 0.3972 11.00000 0.05 1.00 Q10 1 0.8196 0.3825 0.3922 11.00000 0.05 0.94 Q11 1 0.9277 0.4209 0.3480 11.00000 0.05 0.87 Q12 1 -0.0119 0.3827 0.2677 11.00000 0.05 0.87 Q13 1 1.1465 0.4625 0.5875 11.00000 0.05 0.85 Q14 1 0.9840 0.5374 0.2741 11.00000 0.05 0.84 Q15 1 0.9871 0.5427 0.2496 11.00000 0.05 0.83 Q16 1 0.8331 0.5422 0.3059 11.00000 0.05 0.81 Q17 1 0.8715 0.3804 0.4401 11.00000 0.05 0.79 Q18 1 0.9871 0.5436 0.3957 11.00000 0.05 0.76 Q19 1 0.9169 0.4958 0.3439 11.00000 0.05 0.73 Q20 1 0.7732 0.4238 0.4592 11.00000 0.05 0.73 REM The information below was added by Olex2. REM REM R1 = 0.0432 for 3044 Fo > 4sig(Fo) and 0.0451 for all 10143 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.63, deepest hole -4.07 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0451 REM R1_gt = 0.0432 REM wR_ref = 0.1242 REM GOOF = 1.035 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 10143 REM Reflections_gt = 3044 REM Parameters = n/a REM Hole = -4.07 REM Peak = 1.63 REM Flack = n/a ; _cod_data_source_file d0fd00001a2.cif _cod_data_source_block o-Pt _cod_depositor_comments 'Adding full bibliography for 1557791--1557793.cif.' _cod_database_code 1557791 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula PtClC20N4H16 _chemical_oxdiff_usercomment 150K _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. ; _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2.a Free rotating group: O1(H1A,H1B) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C7(H7), C9(H9), C17(H17), C3(H3), C19(H19), C20(H20), C4(H4), C12(H12), C13(H13), C2(H2), C18(H18), C14(H14), C15(H15) ; _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 2.600 _oxdiff_exptl_absorpt_empirical_full_min 0.403 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 0.91766(4) 0.45910(2) 0.34597(2) 0.01737(15) Uani 1 1 d . . . . . Cl1 Cl 1.2387(3) 0.53093(6) 0.36419(9) 0.0259(3) Uani 1 1 d . . . . . Cl2 Cl -0.5691(3) 0.31439(7) 0.03557(9) 0.0300(3) Uani 1 1 d . . . . . N1 N 1.0088(8) 0.4066(2) 0.4489(3) 0.0193(9) Uani 1 1 d . . . . . N3 N 0.7419(8) 0.4915(2) 0.2388(3) 0.0208(9) Uani 1 1 d . . . . . N2 N 0.6497(8) 0.3985(2) 0.3304(3) 0.0171(9) Uani 1 1 d . . . . . O1 O -0.0690(9) 0.3930(2) 0.0511(4) 0.0447(12) Uani 1 1 d . . . . . H1A H -0.209643 0.374315 0.052086 0.067 Uiso 1 1 d G . . . . H1B H 0.040604 0.364315 0.052857 0.067 Uiso 1 1 d G . . . . N4 N -0.0978(9) 0.2758(2) 0.2295(3) 0.0231(10) Uani 1 1 d . . . . . C5 C 0.8528(10) 0.3571(2) 0.4544(3) 0.0179(10) Uani 1 1 d . . . . . C6 C 0.6443(9) 0.3528(2) 0.3874(3) 0.0172(10) Uani 1 1 d . . . . . C1 C 1.2070(10) 0.4141(3) 0.5062(3) 0.0209(11) Uani 1 1 d . . . . . H1 H 1.310285 0.448549 0.502753 0.025 Uiso 1 1 calc R . . . . C8 C 0.2740(10) 0.3127(3) 0.3099(3) 0.0184(11) Uani 1 1 d . . . . . C10 C 0.4844(10) 0.4035(3) 0.2627(3) 0.0183(10) Uani 1 1 d . . . . . C16 C 0.0649(10) 0.2675(2) 0.2977(3) 0.0194(11) Uani 1 1 d . . . . . C11 C 0.5334(11) 0.4573(2) 0.2105(4) 0.0199(12) Uani 1 1 d . . . . . C7 C 0.4536(10) 0.3091(3) 0.3788(3) 0.0178(10) Uani 1 1 d . . . . . H7 H 0.444908 0.277804 0.418231 0.021 Uiso 1 1 calc R . . . . C9 C 0.2909(10) 0.3604(3) 0.2511(3) 0.0182(11) Uani 1 1 d . . . . . H9 H 0.173478 0.363171 0.204812 0.022 Uiso 1 1 calc R . . . . C17 C 0.0381(10) 0.2193(3) 0.3542(4) 0.0225(11) Uani 1 1 d . . . . . H17 H 0.154120 0.213924 0.400366 0.027 Uiso 1 1 calc R . . . . C3 C 1.1034(11) 0.3218(3) 0.5754(4) 0.0237(12) Uani 1 1 d . . . . . H3 H 1.136794 0.293214 0.618270 0.028 Uiso 1 1 calc R . . . . C19 C -0.3305(11) 0.1872(3) 0.2694(4) 0.0259(12) Uani 1 1 d . . . . . H19 H -0.464126 0.159959 0.257498 0.031 Uiso 1 1 calc R . . . . C20 C -0.2917(11) 0.2367(3) 0.2161(4) 0.0243(12) Uani 1 1 d . . . . . H20 H -0.405151 0.242683 0.169438 0.029 Uiso 1 1 calc R . . . . C4 C 0.8972(11) 0.3135(3) 0.5178(4) 0.0228(12) Uani 1 1 d . . . . . H4 H 0.790951 0.279613 0.521411 0.027 Uiso 1 1 calc R . . . . C12 C 0.3827(12) 0.4745(3) 0.1402(4) 0.0260(12) Uani 1 1 d . . . . . H12 H 0.241358 0.451265 0.122281 0.031 Uiso 1 1 calc R . . . . C13 C 0.4440(13) 0.5268(3) 0.0966(4) 0.0285(13) Uani 1 1 d . . . . . H13 H 0.343087 0.539186 0.049332 0.034 Uiso 1 1 calc R . . . . C2 C 1.2602(11) 0.3723(3) 0.5694(4) 0.0266(12) Uani 1 1 d . . . . . H2 H 1.399628 0.377850 0.607699 0.032 Uiso 1 1 calc R . . . . C18 C -0.1683(11) 0.1794(3) 0.3395(4) 0.0254(12) Uani 1 1 d . . . . . H18 H -0.194855 0.147767 0.377197 0.030 Uiso 1 1 calc R . . . . C14 C 0.6561(12) 0.5606(3) 0.1236(4) 0.0297(13) Uani 1 1 d . . . . . H14 H 0.701210 0.595409 0.094188 0.036 Uiso 1 1 calc R . . . . C15 C 0.8002(14) 0.5419(2) 0.1952(4) 0.0264(15) Uani 1 1 d . . . . . H15 H 0.941820 0.564911 0.213731 0.032 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 0.0158(2) 0.0170(2) 0.0194(2) -0.00111(7) 0.00222(13) -0.00009(6) Cl1 0.0223(7) 0.0251(6) 0.0306(8) -0.0035(5) 0.0032(6) -0.0061(5) Cl2 0.0308(7) 0.0306(8) 0.0275(7) -0.0014(6) -0.0044(6) -0.0001(5) N1 0.017(2) 0.018(2) 0.023(2) -0.0046(19) 0.0042(18) -0.0020(17) N3 0.021(2) 0.019(2) 0.023(2) 0.0041(19) 0.0039(18) 0.0045(18) N2 0.015(2) 0.018(2) 0.018(2) 0.0004(18) 0.0001(16) 0.0046(17) O1 0.028(2) 0.039(3) 0.064(3) 0.004(3) -0.008(2) -0.003(2) N4 0.022(2) 0.029(3) 0.018(2) -0.001(2) 0.0012(19) -0.001(2) C5 0.019(2) 0.021(3) 0.014(2) 0.000(2) 0.0005(19) -0.001(2) C6 0.014(2) 0.019(3) 0.020(3) -0.003(2) 0.007(2) -0.0018(19) C1 0.016(2) 0.024(3) 0.023(3) -0.006(2) 0.002(2) -0.002(2) C8 0.017(3) 0.021(3) 0.018(3) -0.003(2) 0.004(2) 0.008(2) C10 0.016(2) 0.025(3) 0.015(2) -0.003(2) 0.0000(19) 0.003(2) C16 0.022(3) 0.021(3) 0.016(2) -0.005(2) 0.002(2) -0.002(2) C11 0.014(3) 0.020(3) 0.025(3) -0.002(2) 0.004(2) 0.0037(18) C7 0.017(2) 0.018(2) 0.018(3) 0.001(2) 0.001(2) 0.0055(19) C9 0.015(2) 0.022(3) 0.017(2) -0.002(2) 0.000(2) 0.003(2) C17 0.019(3) 0.024(3) 0.023(3) 0.002(2) -0.009(2) 0.002(2) C3 0.021(3) 0.029(3) 0.022(3) 0.003(2) 0.004(2) 0.002(2) C19 0.023(3) 0.026(3) 0.028(3) -0.004(2) 0.001(2) -0.005(2) C20 0.021(3) 0.032(3) 0.020(3) -0.004(2) 0.000(2) 0.002(2) C4 0.018(3) 0.024(3) 0.026(3) -0.003(2) 0.003(2) 0.001(2) C12 0.033(3) 0.022(3) 0.024(3) -0.005(2) 0.007(2) 0.002(3) C13 0.035(4) 0.027(3) 0.024(3) 0.001(3) 0.004(3) 0.006(3) C2 0.025(3) 0.035(3) 0.020(3) -0.005(2) -0.002(2) -0.002(2) C18 0.022(3) 0.023(3) 0.031(3) 0.002(2) -0.001(2) 0.000(2) C14 0.033(3) 0.026(3) 0.030(3) 0.010(3) 0.005(3) 0.005(3) C15 0.029(4) 0.025(4) 0.026(3) -0.001(2) 0.002(3) -0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 98.64(13) . . ? N3 Pt1 Cl1 99.16(14) . . ? N3 Pt1 N1 162.20(19) . . ? N2 Pt1 Cl1 179.66(13) . . ? N2 Pt1 N1 81.31(18) . . ? N2 Pt1 N3 80.89(18) . . ? C5 N1 Pt1 112.8(3) . . ? C1 N1 Pt1 127.4(4) . . ? C1 N1 C5 119.7(5) . . ? C11 N3 Pt1 113.4(4) . . ? C15 N3 Pt1 127.9(4) . . ? C15 N3 C11 118.6(5) . . ? C6 N2 Pt1 117.8(3) . . ? C10 N2 Pt1 118.3(4) . . ? C10 N2 C6 123.9(5) . . ? C20 N4 C16 118.6(5) . . ? N1 C5 C6 115.2(5) . . ? N1 C5 C4 120.9(5) . . ? C4 C5 C6 123.9(5) . . ? N2 C6 C5 112.9(4) . . ? N2 C6 C7 119.3(5) . . ? C7 C6 C5 127.8(5) . . ? N1 C1 C2 121.7(5) . . ? C7 C8 C16 121.4(5) . . ? C7 C8 C9 119.5(5) . . ? C9 C8 C16 119.1(5) . . ? N2 C10 C11 112.8(5) . . ? N2 C10 C9 118.8(5) . . ? C9 C10 C11 128.3(5) . . ? N4 C16 C8 116.2(5) . . ? N4 C16 C17 122.2(5) . . ? C17 C16 C8 121.6(5) . . ? N3 C11 C10 114.5(5) . . ? C12 C11 N3 121.4(5) . . ? C12 C11 C10 124.1(6) . . ? C6 C7 C8 119.1(5) . . ? C10 C9 C8 119.4(5) . . ? C16 C17 C18 118.2(5) . . ? C4 C3 C2 120.3(5) . . ? C18 C19 C20 118.7(5) . . ? N4 C20 C19 122.7(5) . . ? C3 C4 C5 118.4(5) . . ? C11 C12 C13 119.2(6) . . ? C12 C13 C14 119.7(6) . . ? C1 C2 C3 119.1(5) . . ? C19 C18 C17 119.5(6) . . ? C13 C14 C15 119.0(6) . . ? N3 C15 C14 122.0(6) . . ? 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 2.3089(14) . ? Pt1 N1 2.026(5) . ? Pt1 N3 2.011(5) . ? Pt1 N2 1.937(4) . ? N1 C5 1.363(7) . ? N1 C1 1.349(7) . ? N3 C11 1.377(8) . ? N3 C15 1.344(8) . ? N2 C6 1.347(7) . ? N2 C10 1.343(7) . ? N4 C16 1.347(7) . ? N4 C20 1.337(8) . ? C5 C6 1.480(7) . ? C5 C4 1.392(8) . ? C6 C7 1.385(8) . ? C1 C2 1.368(8) . ? C8 C16 1.483(8) . ? C8 C7 1.400(8) . ? C8 C9 1.404(8) . ? C10 C11 1.470(8) . ? C10 C9 1.389(8) . ? C16 C17 1.394(8) . ? C11 C12 1.377(9) . ? C17 C18 1.402(8) . ? C3 C4 1.384(8) . ? C3 C2 1.384(9) . ? C19 C20 1.396(9) . ? C19 C18 1.367(9) . ? C12 C13 1.382(9) . ? C13 C14 1.383(10) . ? C14 C15 1.386(10) . ?