#------------------------------------------------------------------------------ #$Date: 2021-09-15 12:06:18 +0300 (Wed, 15 Sep 2021) $ #$Revision: 269153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564652.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_1564652 loop_ _publ_author_name 'Abo-Amer, Anwar' 'Boyle, Paul D.' 'Puddephatt, Richard J.' _publ_section_title ; Push-pull ligands and the oxidation of monomethylplatinum(II) complexes with oxygen or hydrogen peroxide ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119580 _journal_paper_doi 10.1016/j.ica.2020.119580 _journal_volume 507 _journal_year 2020 _chemical_formula_sum 'C21 H24 Cl3 N3 O Pt' _chemical_formula_weight 635.87 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 103.420(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0301(18) _cell_length_b 14.053(2) _cell_length_c 18.120(5) _cell_measurement_reflns_used 9952 _cell_measurement_temperature 110 _cell_measurement_theta_max 31.36 _cell_measurement_theta_min 2.31 _cell_volume 2236.6(8) _computing_cell_refinement SAINT _computing_data_collection Apex2 _computing_data_reduction SAINT _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _computing_structure_refinement SHELXL _computing_structure_solution SHELXT _diffrn_ambient_temperature 110 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker Kappa Axis Apex2' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_unetI/netI 0.0521 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 94448 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.486 _diffrn_reflns_theta_min 2.728 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 6.650 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.888 _exptl_crystal_description prism _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.174 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.077 _refine_diff_density_max 1.874 _refine_diff_density_min -3.349 _refine_diff_density_rms 0.213 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 10925 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0389 _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^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.0828 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7908 _reflns_number_total 10925 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-507-119580.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564652 _shelx_shelxl_version_number 2016/6 _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_min 0.391 _shelx_estimated_absorpt_t_max 0.628 _shelx_res_file ; TITL b18269 in P2(1)/n b18269.res created by SHELXL-2016/6 at 10:29:36 on 06-Mar-2018 CELL 0.71073 9.03007 14.05298 18.11972 90.0000 103.4199 90.0000 ZERR 4 0.00179 0.00243 0.00480 0.0000 0.0047 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O CL PT UNIT 84 96 12 4 12 4 TEMP -163.170 SIZE 0.077 0.127 0.174 ACTA REM omit reflections either wholly or partially obscured by beamstop OMIT 0 1 1 OMIT -1 1 1 OMIT 0 2 0 OMIT 1 1 1 L.S. 12 4 FMAP 2 PLAN 20 BOND $H CONF REM Instructions for potential hydrogen bonds EQIV $1 x, y+1, z HTAB C2 Cl2X_$1 HTAB C7 O1 EQIV $2 -x+1, -y+1, -z+1 HTAB C7 Cl1_$2 HTAB C8 Cl1_$2 EQIV $3 x+1, y, z HTAB C10 O1_$3 HTAB C10 Cl1_$3 EQIV $4 -x+3/2, y+1/2, -z+3/2 HTAB C12 Cl1_$4 HTAB C19 Cl1 HTAB O1 Cl1 HTAB C1X Cl1 WGHT 0.035100 FVAR 0.05218 PT1 6 0.741802 0.790480 0.601060 11.00000 0.01475 0.01183 = 0.02043 -0.00120 0.00280 -0.00170 N1 3 0.517026 0.777478 0.558077 11.00000 0.01588 0.01649 = 0.02182 0.00007 0.00322 0.00055 N2 3 0.734590 0.641170 0.604607 11.00000 0.01539 0.01836 = 0.02111 -0.00296 0.00210 -0.00249 N3 3 0.965992 0.770122 0.641035 11.00000 0.01577 0.01691 = 0.01803 -0.00154 0.00365 -0.00289 C1 1 0.753216 0.935285 0.593658 11.00000 0.02512 0.01880 = 0.03264 0.00262 0.00495 -0.00303 AFIX 137 H1A 2 0.752301 0.963606 0.642974 11.00000 -1.50000 H1B 2 0.665452 0.958516 0.555389 11.00000 -1.50000 H1C 2 0.847368 0.953178 0.579061 11.00000 -1.50000 AFIX 0 C2 1 0.407765 0.844760 0.550846 11.00000 0.01983 0.01610 = 0.02969 0.00265 0.00552 0.00302 AFIX 43 H2 2 0.436093 0.907614 0.567686 11.00000 -1.20000 AFIX 0 C3 1 0.256847 0.825272 0.519906 11.00000 0.01892 0.02743 = 0.02985 0.00437 0.00557 0.00718 AFIX 43 H3 2 0.183098 0.874594 0.514117 11.00000 -1.20000 AFIX 0 C4 1 0.212678 0.732792 0.497091 11.00000 0.01730 0.02793 = 0.02375 -0.00048 0.00107 -0.00296 AFIX 43 H4 2 0.109086 0.717753 0.475564 11.00000 -1.20000 AFIX 0 C5 1 0.324423 0.663644 0.506786 11.00000 0.01731 0.02217 = 0.02273 -0.00310 0.00247 -0.00217 AFIX 43 H5 2 0.297264 0.599680 0.492944 11.00000 -1.20000 AFIX 0 C6 1 0.475254 0.686718 0.536425 11.00000 0.01573 0.01599 = 0.01728 0.00019 0.00193 -0.00194 C7 1 0.602979 0.616104 0.541193 11.00000 0.01651 0.01628 = 0.01783 -0.00273 0.00221 -0.00122 AFIX 23 H7A 2 0.566367 0.551460 0.549472 11.00000 -1.20000 H7B 2 0.635902 0.615850 0.492747 11.00000 -1.20000 AFIX 0 C8 1 0.885454 0.613387 0.588853 11.00000 0.01562 0.01502 = 0.02103 -0.00169 0.00230 0.00043 AFIX 23 H8A 2 0.881661 0.620329 0.534074 11.00000 -1.20000 H8B 2 0.908597 0.546129 0.603292 11.00000 -1.20000 AFIX 0 C9 1 1.007015 0.677342 0.634454 11.00000 0.01765 0.01697 = 0.01875 -0.00069 0.00657 -0.00240 C10 1 1.153380 0.646174 0.665417 11.00000 0.01698 0.02231 = 0.02454 0.00008 0.00565 0.00081 AFIX 43 H10 2 1.179789 0.581313 0.661097 11.00000 -1.20000 AFIX 0 C11 1 1.260968 0.710403 0.702750 11.00000 0.01262 0.04744 = 0.02687 -0.00377 0.00121 -0.00099 AFIX 43 H11 2 1.362111 0.690070 0.724262 11.00000 -1.20000 AFIX 0 C12 1 1.219917 0.805154 0.708577 11.00000 0.01953 0.03021 = 0.02403 -0.00476 0.00319 -0.00660 AFIX 43 H12 2 1.292888 0.850540 0.733097 11.00000 -1.20000 AFIX 0 C13 1 1.071618 0.831804 0.678138 11.00000 0.02511 0.01845 = 0.02078 -0.00560 0.00625 -0.00727 AFIX 43 H13 2 1.042715 0.895977 0.683482 11.00000 -1.20000 AFIX 0 C14 1 0.718484 0.601251 0.679850 11.00000 0.01680 0.01845 = 0.01798 -0.00080 0.00390 -0.00389 AFIX 23 H14A 2 0.805954 0.623225 0.719915 11.00000 -1.20000 H14B 2 0.624920 0.627766 0.691505 11.00000 -1.20000 AFIX 0 C15 1 0.710866 0.494037 0.683151 11.00000 0.01582 0.01635 = 0.01938 0.00004 0.00319 -0.00124 C16 1 0.842157 0.438575 0.701587 11.00000 0.01701 0.02199 = 0.02360 0.00561 0.00123 -0.00217 AFIX 43 H16 2 0.938432 0.469151 0.715631 11.00000 -1.20000 AFIX 0 C17 1 0.836243 0.340534 0.700017 11.00000 0.02120 0.02145 = 0.02958 0.00770 0.00410 0.00356 AFIX 43 H17 2 0.927247 0.304007 0.711023 11.00000 -1.20000 AFIX 0 C18 1 0.695545 0.296191 0.682141 11.00000 0.02422 0.01526 = 0.03051 0.00757 0.00651 0.00090 AFIX 43 H18 2 0.690491 0.228669 0.680880 11.00000 -1.20000 AFIX 0 C19 1 0.562684 0.348353 0.666144 11.00000 0.01793 0.01725 = 0.02396 0.00198 0.00504 -0.00488 AFIX 43 H19 2 0.466941 0.316908 0.654751 11.00000 -1.20000 AFIX 0 C20 1 0.569397 0.447288 0.666754 11.00000 0.01514 0.01835 = 0.02137 0.00016 0.00458 -0.00091 O1 4 0.442308 0.502772 0.651502 11.00000 0.01278 0.01865 = 0.04437 -0.00246 0.00689 -0.00197 AFIX 147 H1 2 0.364563 0.467984 0.641570 11.00000 -1.50000 AFIX 0 CL1 5 0.150523 0.392730 0.607512 11.00000 0.01579 0.01913 = 0.02174 -0.00011 0.00302 -0.00075 C1X 1 0.252251 0.152526 0.599931 11.00000 0.02710 0.01798 = 0.03394 0.00188 0.00517 -0.00087 AFIX 23 H1X1 2 0.250236 0.212286 0.628614 11.00000 -1.20000 H1X2 2 0.244673 0.169351 0.546126 11.00000 -1.20000 AFIX 0 CL1X 5 0.095527 0.081465 0.606730 11.00000 0.03236 0.04023 = 0.06718 0.01224 -0.00135 -0.01667 CL2X 5 0.425773 0.092813 0.636072 11.00000 0.03050 0.03127 = 0.05692 -0.01134 -0.00497 0.00523 HKLF 4 REM b18269 in P2(1)/n REM R1 = 0.0389 for 7908 Fo > 4sig(Fo) and 0.0636 for all 10925 data REM 264 parameters refined using 0 restraints END WGHT 0.0351 0.0000 REM Highest difference peak 1.874, deepest hole -3.349, 1-sigma level 0.213 Q1 1 0.6766 0.7873 0.6465 11.00000 0.05 1.87 Q2 1 0.7917 0.7860 0.5527 11.00000 0.05 1.80 Q3 1 0.7068 0.7895 0.5425 11.00000 0.05 1.78 Q4 1 0.7687 0.7879 0.6611 11.00000 0.05 1.74 Q5 1 0.7024 0.8177 0.6036 11.00000 0.05 1.66 Q6 1 0.7521 0.7367 0.5572 11.00000 0.05 1.61 Q7 1 0.7442 0.8585 0.5711 11.00000 0.05 1.55 Q8 1 0.7337 0.7332 0.6449 11.00000 0.05 1.44 Q9 1 0.7783 0.8151 0.5985 11.00000 0.05 1.37 Q10 1 0.7394 0.8566 0.6309 11.00000 0.05 1.36 Q11 1 0.8666 0.7846 0.6125 11.00000 0.05 1.30 Q12 1 0.6438 0.7622 0.6134 11.00000 0.05 1.26 Q13 1 0.7090 0.7608 0.6035 11.00000 0.05 1.25 Q14 1 0.8150 0.7435 0.6349 11.00000 0.05 1.13 Q15 1 0.6159 0.7942 0.5946 11.00000 0.05 1.09 Q16 1 0.8206 0.8356 0.6367 11.00000 0.05 1.06 Q17 1 0.7599 0.7897 0.5863 11.00000 0.05 1.06 Q18 1 0.6713 0.7385 0.5669 11.00000 0.05 0.98 Q19 1 0.7476 0.6778 0.5665 11.00000 0.05 0.91 Q20 1 0.6715 0.8411 0.5660 11.00000 0.05 0.89 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.74180(2) 0.79048(2) 0.60106(2) 0.01588(3) Uani 1 1 d . . . . . N1 N 0.5170(3) 0.77748(17) 0.55808(15) 0.0183(5) Uani 1 1 d . . . . . N2 N 0.7346(3) 0.64117(18) 0.60461(13) 0.0186(5) Uani 1 1 d . . . . . N3 N 0.9660(3) 0.77012(17) 0.64104(14) 0.0169(5) Uani 1 1 d . . . . . C1 C 0.7532(4) 0.9353(2) 0.59366(19) 0.0258(7) Uani 1 1 d . . . . . H1A H 0.752301 0.963606 0.642974 0.039 Uiso 1 1 calc R U . . . H1B H 0.665452 0.958516 0.555389 0.039 Uiso 1 1 calc R U . . . H1C H 0.847368 0.953178 0.579061 0.039 Uiso 1 1 calc R U . . . C2 C 0.4078(4) 0.8448(2) 0.55085(18) 0.0219(6) Uani 1 1 d . . . . . H2 H 0.436093 0.907614 0.567686 0.026 Uiso 1 1 calc R U . . . C3 C 0.2568(4) 0.8253(2) 0.51991(19) 0.0254(7) Uani 1 1 d . . . . . H3 H 0.183098 0.874594 0.514117 0.031 Uiso 1 1 calc R U . . . C4 C 0.2127(4) 0.7328(2) 0.49709(19) 0.0236(6) Uani 1 1 d . . . . . H4 H 0.109086 0.717753 0.475564 0.028 Uiso 1 1 calc R U . . . C5 C 0.3244(4) 0.6636(2) 0.50679(17) 0.0211(6) Uani 1 1 d . . . . . H5 H 0.297264 0.599680 0.492944 0.025 Uiso 1 1 calc R U . . . C6 C 0.4753(3) 0.6867(2) 0.53642(16) 0.0166(5) Uani 1 1 d . . . . . C7 C 0.6030(3) 0.6161(2) 0.54119(16) 0.0172(5) Uani 1 1 d . . . . . H7A H 0.566367 0.551460 0.549472 0.021 Uiso 1 1 calc R U . . . H7B H 0.635902 0.615850 0.492747 0.021 Uiso 1 1 calc R U . . . C8 C 0.8855(3) 0.61339(19) 0.58885(16) 0.0175(5) Uani 1 1 d . . . . . H8A H 0.881661 0.620329 0.534074 0.021 Uiso 1 1 calc R U . . . H8B H 0.908597 0.546129 0.603292 0.021 Uiso 1 1 calc R U . . . C9 C 1.0070(3) 0.6773(2) 0.63445(16) 0.0174(5) Uani 1 1 d . . . . . C10 C 1.1534(3) 0.6462(2) 0.66542(17) 0.0211(6) Uani 1 1 d . . . . . H10 H 1.179789 0.581313 0.661097 0.025 Uiso 1 1 calc R U . . . C11 C 1.2610(4) 0.7104(3) 0.7028(2) 0.0295(8) Uani 1 1 d . . . . . H11 H 1.362111 0.690070 0.724262 0.035 Uiso 1 1 calc R U . . . C12 C 1.2199(4) 0.8052(2) 0.70858(19) 0.0249(7) Uani 1 1 d . . . . . H12 H 1.292888 0.850540 0.733097 0.030 Uiso 1 1 calc R U . . . C13 C 1.0716(4) 0.8318(2) 0.67814(17) 0.0213(6) Uani 1 1 d . . . . . H13 H 1.042715 0.895977 0.683482 0.026 Uiso 1 1 calc R U . . . C14 C 0.7185(3) 0.6013(2) 0.67985(16) 0.0178(5) Uani 1 1 d . . . . . H14A H 0.805954 0.623225 0.719915 0.021 Uiso 1 1 calc R U . . . H14B H 0.624920 0.627766 0.691505 0.021 Uiso 1 1 calc R U . . . C15 C 0.7109(3) 0.4940(2) 0.68315(16) 0.0173(5) Uani 1 1 d . . . . . C16 C 0.8422(4) 0.4386(2) 0.70159(17) 0.0214(6) Uani 1 1 d . . . . . H16 H 0.938432 0.469151 0.715631 0.026 Uiso 1 1 calc R U . . . C17 C 0.8362(4) 0.3405(2) 0.70002(19) 0.0244(6) Uani 1 1 d . . . . . H17 H 0.927247 0.304007 0.711023 0.029 Uiso 1 1 calc R U . . . C18 C 0.6955(4) 0.2962(2) 0.68214(19) 0.0233(6) Uani 1 1 d . . . . . H18 H 0.690491 0.228669 0.680880 0.028 Uiso 1 1 calc R U . . . C19 C 0.5627(4) 0.3484(2) 0.66614(17) 0.0197(6) Uani 1 1 d . . . . . H19 H 0.466941 0.316908 0.654751 0.024 Uiso 1 1 calc R U . . . C20 C 0.5694(3) 0.4473(2) 0.66675(17) 0.0182(5) Uani 1 1 d . . . . . O1 O 0.4423(2) 0.50277(15) 0.65150(14) 0.0252(5) Uani 1 1 d . . . . . H1 H 0.364563 0.467984 0.641570 0.038 Uiso 1 1 calc R U . . . Cl1 Cl 0.15052(8) 0.39273(5) 0.60751(4) 0.01911(13) Uani 1 1 d . . . . . C1X C 0.2523(4) 0.1525(2) 0.59993(19) 0.0267(7) Uani 1 1 d . . . . . H1X1 H 0.250236 0.212286 0.628614 0.032 Uiso 1 1 calc R U . . . H1X2 H 0.244673 0.169351 0.546126 0.032 Uiso 1 1 calc R U . . . Cl1X Cl 0.09553(12) 0.08146(8) 0.60673(7) 0.0487(3) Uani 1 1 d . . . . . Cl2X Cl 0.42577(11) 0.09281(7) 0.63607(6) 0.0420(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 Pt1 0.01475(6) 0.01183(5) 0.02043(5) -0.00120(4) 0.00280(4) -0.00170(4) N1 0.0159(12) 0.0165(11) 0.0218(12) 0.0001(9) 0.0032(10) 0.0006(9) N2 0.0154(12) 0.0184(11) 0.0211(12) -0.0030(9) 0.0021(10) -0.0025(9) N3 0.0158(12) 0.0169(11) 0.0180(11) -0.0015(8) 0.0036(9) -0.0029(9) C1 0.0251(17) 0.0188(14) 0.0326(17) 0.0026(12) 0.0049(14) -0.0030(12) C2 0.0198(15) 0.0161(13) 0.0297(16) 0.0027(11) 0.0055(13) 0.0030(11) C3 0.0189(16) 0.0274(16) 0.0299(16) 0.0044(13) 0.0056(13) 0.0072(13) C4 0.0173(15) 0.0279(15) 0.0237(15) -0.0005(12) 0.0011(12) -0.0030(12) C5 0.0173(14) 0.0222(14) 0.0227(14) -0.0031(11) 0.0025(12) -0.0022(11) C6 0.0157(14) 0.0160(12) 0.0173(12) 0.0002(9) 0.0019(11) -0.0019(10) C7 0.0165(14) 0.0163(12) 0.0178(12) -0.0027(10) 0.0022(11) -0.0012(10) C8 0.0156(13) 0.0150(12) 0.0210(13) -0.0017(10) 0.0023(11) 0.0004(10) C9 0.0177(14) 0.0170(12) 0.0188(13) -0.0007(10) 0.0066(11) -0.0024(11) C10 0.0170(14) 0.0223(14) 0.0245(14) 0.0001(11) 0.0056(12) 0.0008(11) C11 0.0126(15) 0.047(2) 0.0269(16) -0.0038(15) 0.0012(12) -0.0010(14) C12 0.0195(16) 0.0302(17) 0.0240(15) -0.0048(12) 0.0032(13) -0.0066(12) C13 0.0251(16) 0.0185(13) 0.0208(14) -0.0056(11) 0.0062(12) -0.0073(12) C14 0.0168(14) 0.0185(13) 0.0180(12) -0.0008(10) 0.0039(11) -0.0039(10) C15 0.0158(13) 0.0164(12) 0.0194(13) 0.0000(10) 0.0032(11) -0.0012(10) C16 0.0170(14) 0.0220(14) 0.0236(14) 0.0056(11) 0.0012(12) -0.0022(11) C17 0.0212(16) 0.0214(14) 0.0296(16) 0.0077(12) 0.0041(13) 0.0036(12) C18 0.0242(16) 0.0153(13) 0.0305(16) 0.0076(11) 0.0065(13) 0.0009(11) C19 0.0179(14) 0.0173(13) 0.0240(14) 0.0020(11) 0.0050(12) -0.0049(11) C20 0.0151(13) 0.0183(13) 0.0214(13) 0.0002(10) 0.0046(11) -0.0009(11) O1 0.0128(10) 0.0186(10) 0.0444(14) -0.0025(10) 0.0069(10) -0.0020(8) Cl1 0.0158(3) 0.0191(3) 0.0217(3) -0.0001(2) 0.0030(3) -0.0008(2) C1X 0.0271(18) 0.0180(13) 0.0339(17) 0.0019(12) 0.0052(14) -0.0009(13) Cl1X 0.0324(5) 0.0402(5) 0.0672(7) 0.0122(5) -0.0013(5) -0.0167(4) Cl2X 0.0305(5) 0.0313(5) 0.0569(6) -0.0113(4) -0.0050(4) 0.0052(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' 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' Cl Cl 0.1484 0.1585 '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_ _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 N3 Pt1 N1 166.49(10) . . N3 Pt1 C1 95.95(11) . . N1 Pt1 C1 97.30(11) . . N3 Pt1 N2 83.24(9) . . N1 Pt1 N2 83.41(9) . . C1 Pt1 N2 177.48(12) . . C2 N1 C6 118.7(3) . . C2 N1 Pt1 128.6(2) . . C6 N1 Pt1 112.63(19) . . C7 N2 C8 112.8(2) . . C7 N2 C14 112.4(2) . . C8 N2 C14 110.8(2) . . C7 N2 Pt1 103.72(17) . . C8 N2 Pt1 102.55(16) . . C14 N2 Pt1 114.10(17) . . C13 N3 C9 118.8(3) . . C13 N3 Pt1 128.8(2) . . C9 N3 Pt1 112.05(19) . . Pt1 C1 H1A 109.5 . . Pt1 C1 H1B 109.5 . . H1A C1 H1B 109.5 . . Pt1 C1 H1C 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . N1 C2 C3 122.2(3) . . N1 C2 H2 118.9 . . C3 C2 H2 118.9 . . C2 C3 C4 119.7(3) . . C2 C3 H3 120.2 . . C4 C3 H3 120.2 . . C5 C4 C3 117.9(3) . . C5 C4 H4 121.1 . . C3 C4 H4 121.1 . . C6 C5 C4 120.6(3) . . C6 C5 H5 119.7 . . C4 C5 H5 119.7 . . N1 C6 C5 120.9(3) . . N1 C6 C7 116.3(3) . . C5 C6 C7 122.6(3) . . N2 C7 C6 110.5(2) . . N2 C7 H7A 109.5 . . C6 C7 H7A 109.5 . . N2 C7 H7B 109.5 . . C6 C7 H7B 109.5 . . H7A C7 H7B 108.1 . . N2 C8 C9 108.5(2) . . N2 C8 H8A 110.0 . . C9 C8 H8A 110.0 . . N2 C8 H8B 110.0 . . C9 C8 H8B 110.0 . . H8A C8 H8B 108.4 . . N3 C9 C10 121.3(3) . . N3 C9 C8 116.0(3) . . C10 C9 C8 122.7(3) . . C9 C10 C11 119.3(3) . . C9 C10 H10 120.4 . . C11 C10 H10 120.4 . . C10 C11 C12 119.5(3) . . C10 C11 H11 120.3 . . C12 C11 H11 120.3 . . C13 C12 C11 118.8(3) . . C13 C12 H12 120.6 . . C11 C12 H12 120.6 . . N3 C13 C12 122.3(3) . . N3 C13 H13 118.8 . . C12 C13 H13 118.8 . . C15 C14 N2 114.9(2) . . C15 C14 H14A 108.5 . . N2 C14 H14A 108.5 . . C15 C14 H14B 108.5 . . N2 C14 H14B 108.5 . . H14A C14 H14B 107.5 . . C16 C15 C20 118.1(3) . . C16 C15 C14 121.6(3) . . C20 C15 C14 120.4(3) . . C17 C16 C15 121.8(3) . . C17 C16 H16 119.1 . . C15 C16 H16 119.1 . . C16 C17 C18 118.9(3) . . C16 C17 H17 120.5 . . C18 C17 H17 120.5 . . C19 C18 C17 121.1(3) . . C19 C18 H18 119.4 . . C17 C18 H18 119.4 . . C18 C19 C20 119.7(3) . . C18 C19 H19 120.1 . . C20 C19 H19 120.1 . . O1 C20 C19 122.5(3) . . O1 C20 C15 117.2(3) . . C19 C20 C15 120.3(3) . . C20 O1 H1 109.5 . . Cl1X C1X Cl2X 111.32(18) . . Cl1X C1X H1X1 109.4 . . Cl2X C1X H1X1 109.4 . . Cl1X C1X H1X2 109.4 . . Cl2X C1X H1X2 109.4 . . H1X1 C1X H1X2 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 N3 2.006(3) . Pt1 N1 2.006(3) . Pt1 C1 2.044(3) . Pt1 N2 2.101(3) . N1 C2 1.351(4) . N1 C6 1.362(3) . N2 C7 1.491(3) . N2 C8 1.507(4) . N2 C14 1.512(4) . N3 C13 1.347(4) . N3 C9 1.368(4) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C2 C3 1.375(4) . C2 H2 0.9500 . C3 C4 1.394(5) . C3 H3 0.9500 . C4 C5 1.382(5) . C4 H4 0.9500 . C5 C6 1.382(4) . C5 H5 0.9500 . C6 C7 1.509(4) . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 C9 1.508(4) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 C10 1.382(4) . C10 C11 1.382(4) . C10 H10 0.9500 . C11 C12 1.393(4) . C11 H11 0.9500 . C12 C13 1.377(5) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C15 1.510(4) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C16 1.393(4) . C15 C20 1.406(4) . C16 C17 1.379(4) . C16 H16 0.9500 . C17 C18 1.384(5) . C17 H17 0.9500 . C18 C19 1.378(4) . C18 H18 0.9500 . C19 C20 1.392(4) . C19 H19 0.9500 . C20 O1 1.362(3) . O1 H1 0.8400 . C1X Cl1X 1.760(3) . C1X Cl2X 1.764(3) . C1X H1X1 0.9900 . C1X H1X2 0.9900 . 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 C2 H2 Cl2X 0.95 2.89 3.801(3) 160.2 1_565 C7 H7A O1 0.99 2.47 3.160(4) 126.4 . C7 H7B Cl1 0.99 2.94 3.875(3) 157.2 3_666 C8 H8A Cl1 0.99 2.52 3.498(3) 169.2 3_666 C10 H10 O1 0.95 2.66 3.352(4) 130.5 1_655 C10 H10 Cl1 0.95 2.81 3.711(3) 158.0 1_655 C12 H12 Cl1 0.95 2.88 3.490(3) 123.4 2_656 C19 H19 Cl1 0.95 2.98 3.679(3) 131.2 . O1 H1 Cl1 0.84 2.16 2.999(2) 172.9 . C1X H1X1 Cl1 0.99 2.69 3.509(3) 140.5 . 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 C6 N1 C2 C3 -2.4(5) . . . . Pt1 N1 C2 C3 179.9(2) . . . . N1 C2 C3 C4 2.0(5) . . . . C2 C3 C4 C5 0.0(5) . . . . C3 C4 C5 C6 -1.6(5) . . . . C2 N1 C6 C5 0.7(4) . . . . Pt1 N1 C6 C5 178.8(2) . . . . C2 N1 C6 C7 176.3(3) . . . . Pt1 N1 C6 C7 -5.7(3) . . . . C4 C5 C6 N1 1.3(5) . . . . C4 C5 C6 C7 -174.0(3) . . . . C8 N2 C7 C6 -148.5(2) . . . . C14 N2 C7 C6 85.3(3) . . . . Pt1 N2 C7 C6 -38.4(3) . . . . N1 C6 C7 N2 31.4(3) . . . . C5 C6 C7 N2 -153.1(3) . . . . C7 N2 C8 C9 154.4(2) . . . . C14 N2 C8 C9 -78.6(3) . . . . Pt1 N2 C8 C9 43.5(2) . . . . C13 N3 C9 C10 0.4(4) . . . . Pt1 N3 C9 C10 -173.5(2) . . . . C13 N3 C9 C8 -177.0(3) . . . . Pt1 N3 C9 C8 9.1(3) . . . . N2 C8 C9 N3 -37.4(3) . . . . N2 C8 C9 C10 145.2(3) . . . . N3 C9 C10 C11 -1.0(5) . . . . C8 C9 C10 C11 176.2(3) . . . . C9 C10 C11 C12 0.1(5) . . . . C10 C11 C12 C13 1.3(5) . . . . C9 N3 C13 C12 1.1(4) . . . . Pt1 N3 C13 C12 173.8(2) . . . . C11 C12 C13 N3 -2.0(5) . . . . C7 N2 C14 C15 61.4(3) . . . . C8 N2 C14 C15 -65.7(3) . . . . Pt1 N2 C14 C15 179.18(19) . . . . N2 C14 C15 C16 86.2(3) . . . . N2 C14 C15 C20 -93.2(3) . . . . C20 C15 C16 C17 3.6(5) . . . . C14 C15 C16 C17 -175.8(3) . . . . C15 C16 C17 C18 -2.3(5) . . . . C16 C17 C18 C19 -0.1(5) . . . . C17 C18 C19 C20 1.0(5) . . . . C18 C19 C20 O1 -179.9(3) . . . . C18 C19 C20 C15 0.4(5) . . . . C16 C15 C20 O1 177.7(3) . . . . C14 C15 C20 O1 -2.9(4) . . . . C16 C15 C20 C19 -2.6(4) . . . . C14 C15 C20 C19 176.8(3) . . . .