#------------------------------------------------------------------------------ #$Date: 2020-04-15 13:19:05 +0300 (Wed, 15 Apr 2020) $ #$Revision: 250759 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557792.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_1557792 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_paper_doi 10.1039/D0FD00001A _journal_year 2020 _chemical_formula_moiety 'C20 H14 Cl N4 Pt, Cl, C H4 O' _chemical_formula_sum 'C21 H18 Cl2 N4 O Pt' _chemical_formula_weight 608.38 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _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 69.402(2) _cell_angle_beta 86.254(2) _cell_angle_gamma 72.413(2) _cell_formula_units_Z 2 _cell_length_a 8.01850(10) _cell_length_b 10.5928(2) _cell_length_c 13.0124(3) _cell_measurement_reflns_used 7707 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 75.3320 _cell_measurement_theta_min 3.6270 _cell_volume 985.20(4) _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 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -96.00 -71.00 0.50 0.21 -- -42.55 158.00 25.00 50 2 \w -110.00 -49.00 0.50 0.21 -- -42.55-158.00 -8.00 122 3 \w -50.00 -25.00 0.50 0.21 -- -42.55 118.00-128.00 50 4 \w 56.00 82.00 0.50 0.21 -- 42.55-158.00 -8.00 52 5 \w 49.00 84.00 0.50 0.21 -- 42.55 158.00 25.00 70 6 \w 6.00 92.00 0.50 0.21 -- 42.55-118.00 145.00 172 7 \w -74.00 -49.00 0.50 0.26 -- -84.50 118.00-128.00 50 8 \w -142.00-117.00 0.50 0.26 -- -84.50-118.00 145.00 50 9 \w -80.00 -54.00 0.50 0.26 -- -84.50-158.00 -8.00 52 10 \w 105.00 131.00 0.50 0.26 -- 108.63 158.00 25.00 52 11 \w 74.00 107.00 0.50 0.26 -- 108.63-118.00 145.00 66 12 \w 103.00 141.00 0.50 0.26 -- 108.63 118.00-128.00 76 13 \w 78.00 105.00 0.50 0.26 -- 108.63-158.00 -8.00 54 14 \w -114.00 -89.00 0.50 0.21 -- -42.55 -57.00 30.00 50 15 \w -115.00 -70.00 0.50 0.21 -- -42.55-125.00-150.00 90 16 \w -86.00 -22.00 0.50 0.21 -- -42.55 -57.00 30.00 128 17 \w 75.00 100.00 0.50 0.21 -- 42.55 125.00-180.00 50 18 \w 81.00 113.00 0.50 0.21 -- 42.55 77.00-120.00 64 19 \w 83.00 116.00 0.50 0.21 -- 42.55 125.00 -30.00 66 20 \w 14.00 72.00 0.50 0.21 -- 42.55 77.00-120.00 116 21 \w -160.00-110.00 0.50 0.26 -- -84.50 -45.00 150.00 100 22 \w -65.00 -7.00 0.50 0.26 -- -84.50 30.00 90.00 116 23 \w -105.00 -68.00 0.50 0.26 -- -84.50 -45.00 150.00 74 24 \w 30.00 65.00 0.50 0.26 -- 108.63 -30.00 90.00 70 25 \w 65.00 130.00 0.50 0.26 -- 108.63 -61.00 120.00 130 26 \w 38.00 108.00 0.50 0.26 -- 108.63 -94.00-180.00 140 27 \w 45.00 76.00 0.50 0.26 -- 108.63 -45.00-150.00 62 28 \w 43.00 78.00 0.50 0.26 -- 108.63 -45.00 -60.00 70 29 \w 87.00 117.00 0.50 0.26 -- 108.63 45.00 -30.00 60 30 \w 63.00 88.00 0.50 0.26 -- 108.63 -77.00-180.00 50 31 \w 51.00 76.00 0.50 0.26 -- 108.63 -45.00 30.00 50 32 \w 69.00 116.00 0.50 0.26 -- 108.63-125.00 30.00 94 33 \w 30.00 63.00 0.50 0.26 -- 108.63 -30.00 150.00 66 34 \w 121.00 147.00 0.50 0.26 -- 108.63 45.00-180.00 52 35 \w 97.00 137.00 0.50 0.26 -- 108.63 -77.00-180.00 80 36 \w 57.00 107.00 0.50 0.26 -- 108.63 -94.00 0.00 100 37 \w 42.00 78.00 0.50 0.26 -- 108.63 -45.00 60.00 72 38 \w 40.00 77.00 0.50 0.26 -- 108.63 -45.00 0.00 74 39 \w 31.00 59.00 0.50 0.26 -- 108.63 -30.00 -60.00 56 40 \w 115.00 176.00 0.50 0.26 -- 108.63 30.00 60.00 122 41 \w 32.00 66.00 0.50 0.26 -- 108.63 -30.00-150.00 68 42 \w 91.00 116.00 0.50 0.26 -- 108.63-125.00 90.00 50 43 \w 60.00 86.00 0.50 0.26 -- 108.63-125.00 90.00 52 44 \w 85.00 111.00 0.50 0.26 -- 108.63 30.00 60.00 52 45 \w 33.00 58.00 0.50 0.26 -- 108.63 -30.00-180.00 50 46 \w 34.00 63.00 0.50 0.26 -- 108.63 -30.00 -90.00 58 47 \w 44.00 69.00 0.50 0.26 -- 108.63-125.00-180.00 50 48 \w 73.00 100.00 0.50 0.26 -- 108.63-125.00-180.00 54 49 \w 94.00 119.00 0.50 0.26 -- 108.63 45.00-180.00 50 50 \w 128.00 164.00 0.50 0.26 -- 108.63 45.00 -30.00 72 51 \w 140.00 165.00 0.50 0.26 -- 108.63 158.00 25.00 50 ; _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 -0.0292560000 _diffrn_orient_matrix_UB_12 0.0348741000 _diffrn_orient_matrix_UB_13 -0.1240163000 _diffrn_orient_matrix_UB_21 -0.0443499000 _diffrn_orient_matrix_UB_22 0.1587729000 _diffrn_orient_matrix_UB_23 -0.0190453000 _diffrn_orient_matrix_UB_31 0.1946368000 _diffrn_orient_matrix_UB_32 -0.0090182000 _diffrn_orient_matrix_UB_33 -0.0169551000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0297 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10329 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.071 _diffrn_reflns_theta_max 67.071 _diffrn_reflns_theta_min 3.633 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 15.992 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.38652 _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 'clear light orange' _exptl_crystal_density_diffrn 2.051 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.277 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.144 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.740 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 3525 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.740 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0261 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.0811 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3434 _reflns_number_total 3525 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_152meohtolueneblockorange_a.res in P-1 exp_152meohtolueneblockorange.res created by SHELXL-2018/3 at 10:47:46 on 06-Jan-2020 REM Old TITL exp_152meohtoluene block orange in P-1 REM SHELXT solution in P-1: R1 0.043, Rweak 0.010, Alpha 0.058 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N4 Cl2 Pt CELL 1.54184 8.0185 10.5928 13.0124 69.402 86.254 72.413 ZERR 2 0.0001 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H Cl N O Pt UNIT 42 36 4 8 2 2 L.S. 99 0 0 PLAN 20 BOND LIST 4 fmap 2 53 acta REM REM REM WGHT 0.100000 FVAR 0.28875 PT1 6 1.023383 0.123063 0.545939 11.00000 0.01562 0.01919 = 0.01712 -0.00520 -0.00017 -0.00407 CL1 3 1.292064 -0.021536 0.628262 11.00000 0.01830 0.03238 = 0.02674 -0.00554 -0.00328 -0.00228 CL2 3 0.660537 0.701149 0.065859 11.00000 0.02761 0.03259 = 0.02312 -0.00258 0.00235 -0.00773 N2 4 0.798907 0.250033 0.477630 11.00000 0.01881 0.02040 = 0.01755 -0.00737 0.00246 -0.00573 N1 4 0.873003 0.075175 0.675175 11.00000 0.02413 0.02159 = 0.01579 -0.00595 0.00267 -0.00940 N3 4 1.101166 0.214226 0.394770 11.00000 0.01322 0.02249 = 0.02029 -0.00787 0.00582 -0.00662 N4 4 0.174000 0.521018 0.397554 11.00000 0.01981 0.02626 = 0.02321 -0.00953 0.00249 -0.00531 O008 5 0.299077 0.811686 -0.058886 11.00000 0.05051 0.03937 = 0.04569 -0.00678 -0.01692 -0.01149 AFIX 147 H008 2 0.389311 0.796555 -0.024392 11.00000 -1.50000 AFIX 0 C10 1 0.795163 0.337007 0.373456 11.00000 0.02074 0.02120 = 0.01551 -0.00522 0.00108 -0.00815 C6 1 0.656216 0.247400 0.537514 11.00000 0.02295 0.02386 = 0.01847 -0.00884 0.00442 -0.01019 C11 1 0.967703 0.316267 0.325221 11.00000 0.02495 0.02255 = 0.02221 -0.00849 -0.00018 -0.00790 C5 1 0.697893 0.144425 0.651673 11.00000 0.02202 0.02088 = 0.02097 -0.00632 -0.00218 -0.00843 C20 1 0.308695 0.529191 0.331835 11.00000 0.02114 0.02185 = 0.02153 -0.00847 -0.00163 -0.00497 C1 1 0.923547 -0.014813 0.779584 11.00000 0.02258 0.02467 = 0.01465 -0.00106 -0.00411 -0.00618 AFIX 43 H1 2 1.041957 -0.062175 0.797028 11.00000 -1.20000 AFIX 0 C8 1 0.484142 0.431312 0.381444 11.00000 0.02385 0.02148 = 0.02013 -0.00684 0.00095 -0.00640 C14 1 1.298616 0.253201 0.250467 11.00000 0.01980 0.03087 = 0.03299 -0.01482 0.00331 -0.00639 AFIX 43 H14 2 1.411498 0.229398 0.226026 11.00000 -1.20000 AFIX 0 C19 1 0.287992 0.623338 0.223768 11.00000 0.02320 0.02885 = 0.01956 -0.00680 0.00132 -0.01146 AFIX 43 H19 2 0.384528 0.628814 0.180645 11.00000 -1.20000 AFIX 0 C15 1 1.263957 0.184892 0.357202 11.00000 0.01583 0.02456 = 0.02550 -0.00825 0.00146 -0.00552 AFIX 43 H15 2 1.355244 0.116687 0.404680 11.00000 -1.20000 AFIX 0 C12 1 0.998256 0.390397 0.217685 11.00000 0.02257 0.02259 = 0.01966 -0.00658 0.00378 -0.00578 AFIX 43 H12 2 0.907628 0.461605 0.171519 11.00000 -1.20000 AFIX 0 C9 1 0.635529 0.432518 0.323155 11.00000 0.02140 0.02272 = 0.01758 -0.00667 0.00162 -0.00521 AFIX 43 H9 2 0.630641 0.495908 0.251789 11.00000 -1.20000 AFIX 0 C7 1 0.494689 0.335109 0.489606 11.00000 0.01948 0.02376 = 0.01967 -0.00566 0.00281 -0.00935 AFIX 43 H7 2 0.393710 0.330758 0.528362 11.00000 -1.20000 AFIX 0 C18 1 0.121463 0.708589 0.181611 11.00000 0.02622 0.02823 = 0.02281 -0.00463 -0.00578 -0.00476 AFIX 43 H18 2 0.103961 0.770692 0.109238 11.00000 -1.20000 AFIX 0 C17 1 -0.018648 0.699714 0.249187 11.00000 0.01315 0.02428 = 0.02900 -0.00887 -0.00069 -0.00348 AFIX 43 H17 2 -0.131814 0.755898 0.223036 11.00000 -1.20000 AFIX 0 C13 1 1.166492 0.356245 0.180415 11.00000 0.02327 0.02534 = 0.02210 -0.00685 0.00543 -0.00802 AFIX 43 H13 2 1.189197 0.403124 0.108292 11.00000 -1.20000 AFIX 0 C3 1 0.629084 0.031347 0.836182 11.00000 0.03335 0.02805 = 0.02263 -0.00871 0.00971 -0.00886 AFIX 43 H3 2 0.547838 0.016081 0.889971 11.00000 -1.20000 AFIX 0 C4 1 0.575142 0.124598 0.730020 11.00000 0.02683 0.02278 = 0.02420 -0.00724 0.00468 -0.00495 AFIX 43 H4 2 0.457135 0.173196 0.712047 11.00000 -1.20000 AFIX 0 C16 1 0.012799 0.606097 0.355856 11.00000 0.02006 0.03691 = 0.02790 -0.01444 0.00821 -0.01106 AFIX 43 H16 2 -0.081412 0.601345 0.401178 11.00000 -1.20000 AFIX 0 C2 1 0.805260 -0.038203 0.860415 11.00000 0.03669 0.02524 = 0.02113 -0.00289 -0.00052 -0.00881 AFIX 43 H2 2 0.843970 -0.100656 0.931091 11.00000 -1.20000 AFIX 0 C00T 1 0.297739 0.687697 -0.075003 11.00000 0.04984 0.04792 = 0.03859 -0.01365 -0.00628 -0.01619 AFIX 137 H00A 2 0.307980 0.700389 -0.151668 11.00000 -1.50000 H00B 2 0.189916 0.667497 -0.050731 11.00000 -1.50000 H00C 2 0.394406 0.610436 -0.033631 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_152meohtolueneblockorange_a.res in P-1 REM wR2 = 0.0811, GooF = S = 0.740, Restrained GooF = 0.740 for all data REM R1 = 0.0261 for 3434 Fo > 4sig(Fo) and 0.0267 for all 3525 data REM 264 parameters refined using 0 restraints END WGHT 0.0500 0.4097 REM Highest difference peak 2.277, deepest hole -1.215, 1-sigma level 0.144 Q1 1 1.0130 0.1611 0.4634 11.00000 0.05 2.28 Q2 1 1.0348 0.0832 0.6292 11.00000 0.05 2.19 Q3 1 0.8961 0.0353 0.7028 11.00000 0.05 0.74 Q4 1 0.9929 0.2148 0.5583 11.00000 0.05 0.73 Q5 1 0.4843 0.3851 0.4390 11.00000 0.05 0.68 Q6 1 1.1591 0.2184 0.3847 11.00000 0.05 0.67 Q7 1 1.0576 0.0231 0.5406 11.00000 0.05 0.66 Q8 1 0.9770 0.3434 0.2839 11.00000 0.05 0.63 Q9 1 0.6718 0.1839 0.6072 11.00000 0.05 0.60 Q10 1 0.0671 0.6040 0.3657 11.00000 0.05 0.53 Q11 1 1.1110 -0.0187 0.5994 11.00000 0.05 0.50 Q12 1 1.2064 0.2676 0.2173 11.00000 0.05 0.49 Q13 1 0.2896 0.5657 0.2746 11.00000 0.05 0.48 Q14 1 1.0782 -0.0468 0.6780 11.00000 0.05 0.48 Q15 1 1.3053 -0.0555 0.7142 11.00000 0.05 0.46 Q16 1 0.6643 0.6667 0.1579 11.00000 0.05 0.45 Q17 1 0.9361 0.2569 0.4991 11.00000 0.05 0.43 Q18 1 1.3202 0.0006 0.5554 11.00000 0.05 0.43 Q19 1 0.9207 -0.1387 0.7190 11.00000 0.05 0.41 Q20 1 1.4433 -0.1797 0.5970 11.00000 0.05 0.41 REM The information below was added by Olex2. REM REM R1 = 0.0261 for 3434 Fo > 4sig(Fo) and 0.0267 for all 10329 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.28, deepest hole -1.22 REM Mean Shift 0, Max Shift 0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0267 REM R1_gt = 0.0261 REM wR_ref = 0.0811 REM GOOF = 0.740 REM Shift_max = 0.003 REM Shift_mean = 0 REM Reflections_all = 10329 REM Reflections_gt = 3434 REM Parameters = n/a REM Hole = -1.22 REM Peak = 2.28 REM Flack = n/a ; _cod_data_source_file d0fd00001a2.cif _cod_data_source_block o-Pt-MeOH _cod_database_code 1557792 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C20H14N4PtCl _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 99.89 _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 C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C14(H14), C19(H19), C15(H15), C12(H12), C9(H9), C7(H7), C18(H18), C17(H17), C13(H13), C3(H3), C4(H4), C16(H16), C2(H2) 2.b Idealised Me refined as rotating group: C00T(H00A,H00B,H00C) 2.c Idealised tetrahedral OH refined as rotating group: O008(H008) ; _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 2.118 _oxdiff_exptl_absorpt_empirical_full_min 0.634 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 1.02338(2) 0.12306(2) 0.54594(2) 0.01785(10) Uani 1 1 d . . . . . Cl1 Cl 1.29206(13) -0.02154(12) 0.62826(9) 0.0282(2) Uani 1 1 d . . . . . Cl2 Cl 0.66054(13) 0.70115(10) 0.06586(8) 0.0301(2) Uani 1 1 d . . . . . N2 N 0.7989(5) 0.2500(4) 0.4776(3) 0.0188(8) Uani 1 1 d . . . . . N1 N 0.8730(5) 0.0752(4) 0.6752(3) 0.0201(7) Uani 1 1 d . . . . . N3 N 1.1012(4) 0.2142(4) 0.3948(3) 0.0185(7) Uani 1 1 d . . . . . N4 N 0.1740(5) 0.5210(4) 0.3976(3) 0.0233(8) Uani 1 1 d . . . . . O008 O 0.2991(5) 0.8117(4) -0.0589(3) 0.0470(9) Uani 1 1 d . . . . . H008 H 0.389311 0.796555 -0.024392 0.070 Uiso 1 1 calc GR . . . . C10 C 0.7952(5) 0.3370(4) 0.3735(3) 0.0190(7) Uani 1 1 d . . . . . C6 C 0.6562(6) 0.2474(4) 0.5375(3) 0.0208(8) Uani 1 1 d . . . . . C11 C 0.9677(5) 0.3163(4) 0.3252(3) 0.0228(8) Uani 1 1 d . . . . . C5 C 0.6979(6) 0.1444(4) 0.6517(3) 0.0209(8) Uani 1 1 d . . . . . C20 C 0.3087(6) 0.5292(5) 0.3318(4) 0.0215(9) Uani 1 1 d . . . . . C1 C 0.9235(5) -0.0148(4) 0.7796(3) 0.0222(8) Uani 1 1 d . . . . . H1 H 1.041957 -0.062175 0.797028 0.027 Uiso 1 1 calc R . . . . C8 C 0.4841(6) 0.4313(4) 0.3814(3) 0.0220(9) Uani 1 1 d . . . . . C14 C 1.2986(6) 0.2532(5) 0.2505(4) 0.0272(10) Uani 1 1 d . . . . . H14 H 1.411498 0.229398 0.226026 0.033 Uiso 1 1 calc R . . . . C19 C 0.2880(6) 0.6233(5) 0.2238(3) 0.0235(9) Uani 1 1 d . . . . . H19 H 0.384528 0.628814 0.180645 0.028 Uiso 1 1 calc R . . . . C15 C 1.2640(5) 0.1849(4) 0.3572(3) 0.0222(8) Uani 1 1 d . . . . . H15 H 1.355244 0.116687 0.404680 0.027 Uiso 1 1 calc R . . . . C12 C 0.9983(6) 0.3904(4) 0.2177(3) 0.0222(8) Uani 1 1 d . . . . . H12 H 0.907628 0.461605 0.171519 0.027 Uiso 1 1 calc R . . . . C9 C 0.6355(5) 0.4325(4) 0.3232(3) 0.0210(7) Uani 1 1 d . . . . . H9 H 0.630641 0.495908 0.251789 0.025 Uiso 1 1 calc R . . . . C7 C 0.4947(6) 0.3351(5) 0.4896(4) 0.0209(8) Uani 1 1 d . . . . . H7 H 0.393710 0.330758 0.528362 0.025 Uiso 1 1 calc R . . . . C18 C 0.1215(6) 0.7086(5) 0.1816(4) 0.0274(9) Uani 1 1 d . . . . . H18 H 0.103961 0.770692 0.109238 0.033 Uiso 1 1 calc R . . . . C17 C -0.0186(5) 0.6997(4) 0.2492(4) 0.0227(8) Uani 1 1 d . . . . . H17 H -0.131814 0.755898 0.223036 0.027 Uiso 1 1 calc R . . . . C13 C 1.1665(6) 0.3562(4) 0.1804(3) 0.0240(8) Uani 1 1 d . . . . . H13 H 1.189197 0.403124 0.108292 0.029 Uiso 1 1 calc R . . . . C3 C 0.6291(6) 0.0313(4) 0.8362(3) 0.0285(9) Uani 1 1 d . . . . . H3 H 0.547838 0.016081 0.889971 0.034 Uiso 1 1 calc R . . . . C4 C 0.5751(6) 0.1246(4) 0.7300(3) 0.0256(8) Uani 1 1 d . . . . . H4 H 0.457135 0.173196 0.712047 0.031 Uiso 1 1 calc R . . . . C16 C 0.0128(6) 0.6061(5) 0.3559(4) 0.0272(9) Uani 1 1 d . . . . . H16 H -0.081412 0.601345 0.401178 0.033 Uiso 1 1 calc R . . . . C2 C 0.8053(7) -0.0382(5) 0.8604(4) 0.0292(10) Uani 1 1 d . . . . . H2 H 0.843970 -0.100656 0.931091 0.035 Uiso 1 1 calc R . . . . C00T C 0.2977(8) 0.6877(6) -0.0750(4) 0.0451(12) Uani 1 1 d . . . . . H00A H 0.307980 0.700389 -0.151668 0.068 Uiso 1 1 calc GR . . . . H00B H 0.189916 0.667497 -0.050731 0.068 Uiso 1 1 calc GR . . . . H00C H 0.394406 0.610436 -0.033631 0.068 Uiso 1 1 calc GR . . . . 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 0.01562(14) 0.01919(13) 0.01712(13) -0.00520(9) -0.00017(8) -0.00407(9) Cl1 0.0183(5) 0.0324(5) 0.0267(5) -0.0055(4) -0.0033(4) -0.0023(4) Cl2 0.0276(5) 0.0326(5) 0.0231(5) -0.0026(4) 0.0024(4) -0.0077(4) N2 0.0188(18) 0.0204(17) 0.0175(17) -0.0074(14) 0.0025(14) -0.0057(14) N1 0.0241(18) 0.0216(17) 0.0158(16) -0.0059(14) 0.0027(14) -0.0094(14) N3 0.0132(15) 0.0225(16) 0.0203(17) -0.0079(13) 0.0058(12) -0.0066(13) N4 0.0198(18) 0.0263(18) 0.0232(18) -0.0095(15) 0.0025(14) -0.0053(14) O008 0.051(2) 0.0394(18) 0.046(2) -0.0068(15) -0.0169(17) -0.0115(16) C10 0.0207(18) 0.0212(17) 0.0155(17) -0.0052(14) 0.0011(14) -0.0082(14) C6 0.023(2) 0.024(2) 0.0185(19) -0.0088(16) 0.0044(16) -0.0102(16) C11 0.025(2) 0.0226(18) 0.0222(19) -0.0085(16) -0.0002(16) -0.0079(16) C5 0.022(2) 0.0209(19) 0.021(2) -0.0063(16) -0.0022(16) -0.0084(16) C20 0.021(2) 0.022(2) 0.022(2) -0.0085(18) -0.0016(17) -0.0050(17) C1 0.023(2) 0.0247(19) 0.0147(18) -0.0011(15) -0.0041(15) -0.0062(16) C8 0.024(2) 0.0215(19) 0.020(2) -0.0068(17) 0.0010(16) -0.0064(16) C14 0.020(2) 0.031(2) 0.033(3) -0.015(2) 0.0033(19) -0.0064(19) C19 0.023(2) 0.029(2) 0.020(2) -0.0068(17) 0.0013(17) -0.0115(17) C15 0.0158(18) 0.0246(19) 0.026(2) -0.0083(16) 0.0015(16) -0.0055(15) C12 0.023(2) 0.0226(19) 0.020(2) -0.0066(16) 0.0038(16) -0.0058(16) C9 0.0214(18) 0.0227(18) 0.0176(17) -0.0067(15) 0.0016(14) -0.0052(15) C7 0.0195(19) 0.0238(19) 0.020(2) -0.0057(18) 0.0028(15) -0.0093(15) C18 0.026(2) 0.028(2) 0.023(2) -0.0046(17) -0.0058(17) -0.0048(17) C17 0.0132(18) 0.0243(19) 0.029(2) -0.0089(17) -0.0007(16) -0.0035(15) C13 0.023(2) 0.025(2) 0.0221(19) -0.0069(17) 0.0054(17) -0.0080(17) C3 0.033(2) 0.028(2) 0.023(2) -0.0087(17) 0.0097(17) -0.0089(18) C4 0.027(2) 0.0228(19) 0.024(2) -0.0072(16) 0.0047(17) -0.0049(16) C16 0.020(2) 0.037(2) 0.028(2) -0.0144(19) 0.0082(18) -0.0111(18) C2 0.037(3) 0.025(2) 0.021(2) -0.0029(17) -0.0005(18) -0.0088(19) C00T 0.050(3) 0.048(3) 0.039(3) -0.014(2) -0.006(2) -0.016(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 N2 Pt1 Cl1 178.03(11) . . ? N2 Pt1 N1 81.04(15) . . ? N2 Pt1 N3 80.92(14) . . ? N1 Pt1 Cl1 99.17(11) . . ? N1 Pt1 N3 161.95(16) . . ? N3 Pt1 Cl1 98.84(10) . . ? C10 N2 Pt1 118.0(3) . . ? C10 N2 C6 123.7(4) . . ? C6 N2 Pt1 118.3(3) . . ? C5 N1 Pt1 113.8(3) . . ? C1 N1 Pt1 128.4(3) . . ? C1 N1 C5 117.8(4) . . ? C11 N3 Pt1 113.4(3) . . ? C15 N3 Pt1 127.7(3) . . ? C15 N3 C11 119.0(3) . . ? C20 N4 C16 118.0(4) . . ? N2 C10 C11 113.2(3) . . ? N2 C10 C9 119.2(4) . . ? C9 C10 C11 127.7(3) . . ? N2 C6 C5 112.7(4) . . ? N2 C6 C7 119.1(4) . . ? C7 C6 C5 128.1(4) . . ? N3 C11 C10 114.5(3) . . ? N3 C11 C12 121.0(4) . . ? C12 C11 C10 124.5(4) . . ? N1 C5 C6 114.0(4) . . ? N1 C5 C4 122.0(4) . . ? C4 C5 C6 123.9(4) . . ? N4 C20 C8 115.9(4) . . ? N4 C20 C19 122.4(4) . . ? C19 C20 C8 121.7(4) . . ? N1 C1 C2 122.2(4) . . ? C9 C8 C20 121.7(4) . . ? C9 C8 C7 119.6(4) . . ? C7 C8 C20 118.8(4) . . ? C13 C14 C15 119.8(4) . . ? C18 C19 C20 119.0(4) . . ? N3 C15 C14 121.7(4) . . ? C13 C12 C11 118.8(4) . . ? C8 C9 C10 119.0(4) . . ? C6 C7 C8 119.3(4) . . ? C19 C18 C17 118.8(4) . . ? C16 C17 C18 118.8(4) . . ? C14 C13 C12 119.6(4) . . ? C2 C3 C4 118.9(4) . . ? C5 C4 C3 119.4(4) . . ? N4 C16 C17 123.0(4) . . ? C1 C2 C3 119.8(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 2.2996(10) . ? Pt1 N2 1.935(4) . ? Pt1 N1 2.011(4) . ? Pt1 N3 2.014(3) . ? N2 C10 1.341(5) . ? N2 C6 1.343(6) . ? N1 C5 1.371(6) . ? N1 C1 1.359(5) . ? N3 C11 1.368(5) . ? N3 C15 1.348(5) . ? N4 C20 1.338(6) . ? N4 C16 1.349(6) . ? O008 C00T 1.404(6) . ? C10 C11 1.468(6) . ? C10 C9 1.397(5) . ? C6 C5 1.487(6) . ? C6 C7 1.378(6) . ? C11 C12 1.390(6) . ? C5 C4 1.377(6) . ? C20 C8 1.496(6) . ? C20 C19 1.394(6) . ? C1 C2 1.377(6) . ? C8 C9 1.390(6) . ? C8 C7 1.407(6) . ? C14 C15 1.376(7) . ? C14 C13 1.368(6) . ? C19 C18 1.385(6) . ? C12 C13 1.389(6) . ? C18 C17 1.386(6) . ? C17 C16 1.378(6) . ? C3 C4 1.390(6) . ? C3 C2 1.380(7) . ?