#------------------------------------------------------------------------------ #$Date: 2021-09-15 12:06:18 +0300 (Wed, 15 Sep 2021) $ #$Revision: 269153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564655.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_1564655 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 'C20 H26 Cl N3 O4 Pt' _chemical_formula_weight 602.98 _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 107.866(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9331(19) _cell_length_b 20.468(4) _cell_length_c 11.961(2) _cell_measurement_reflns_used 9939 _cell_measurement_temperature 110 _cell_measurement_theta_max 32.33 _cell_measurement_theta_min 2.42 _cell_volume 2547.5(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 0.997 _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 0.0663 _diffrn_reflns_av_unetI/netI 0.0382 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 117929 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 36.400 _diffrn_reflns_theta_min 2.424 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 5.639 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.4747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.572 _exptl_crystal_description needle _exptl_crystal_F_000 1176 _exptl_crystal_size_max 0.335 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.048 _refine_diff_density_max 3.045 _refine_diff_density_min -2.121 _refine_diff_density_rms 0.158 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 12379 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0350 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+4.0421P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.0868 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9302 _reflns_number_total 12379 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-507-119580.cif _cod_data_source_block 4 _cod_original_cell_volume 2547.4(8) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1564655 _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 0.254 _shelx_estimated_absorpt_t_max 0.774 _shelx_res_file ; TITL b18140 in P2(1)/c b18140.res created by SHELXL-2016/6 at 10:51:44 on 22-Sep-2017 CELL 0.71073 10.93306 20.46769 11.96067 90.0000 107.8659 90.0000 ZERR 4 0.00193 0.00409 0.00203 0.0000 0.0098 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O CL PT UNIT 80 104 12 16 4 4 TEMP -163 SIZE 0.048 0.055 0.335 ACTA REM omit reflections blocked by beamstop OMIT 1 0 0 OMIT 0 2 0 OMIT 1 1 1 OMIT 0 3 2 OMIT 0 2 3 ABIN L.S. 12 0 34 FMAP 2 PLAN 30 BOND $H CONF REM Instructions for potential hydrogen bonds HTAB C8 Cl1 HTAB C10 Cl0 EQIV $1 -x+1, -y+2, -z+2 HTAB C10 Cl2_$1 EQIV $2 -x+1, y-1/2, -z+3/2 HTAB C13 Cl2_$2 HTAB C14 Cl2 EQIV $3 -x+1, y+1/2, -z+3/2 HTAB C14 Cl3_$3 HTAB O1W O1 EQIV $4 x, -y+3/2, z-1/2 HTAB O1W O2_$4 HTAB O2W O1W SUMP 1.0 0.0001 1.0 2 1.0 3 1.0 4 1.0 5 WGHT 0.038000 4.042100 FVAR 0.08527 0.30033 0.17232 0.29792 0.22945 PT1 6 0.633667 0.817315 0.656503 11.00000 0.02798 0.01796 = 0.01692 0.00138 0.01043 0.00381 O1 4 0.537968 0.861763 0.502790 11.00000 0.03359 0.02189 = 0.01668 0.00164 0.00968 0.00656 O2 4 0.727279 0.773356 0.807666 11.00000 0.03387 0.03000 = 0.02093 0.00726 0.00841 0.00879 AFIX 3 H2H 2 0.807872 0.771025 0.829296 11.00000 -1.50000 AFIX 0 N1 3 0.802638 0.853233 0.649599 11.00000 0.02631 0.03696 = 0.02601 0.01063 0.01368 0.00683 N2 3 0.633854 0.904826 0.752786 11.00000 0.02486 0.01730 = 0.01857 0.00025 0.00836 -0.00109 N3 3 0.469603 0.799763 0.694110 11.00000 0.02923 0.01653 = 0.01952 0.00196 0.00814 -0.00224 C1 1 0.640479 0.732831 0.566684 11.00000 0.05319 0.02320 = 0.02557 0.00159 0.01898 0.00957 AFIX 137 H1A 2 0.728842 0.716289 0.590037 11.00000 -1.50000 H1B 2 0.611815 0.741706 0.482089 11.00000 -1.50000 H1C 2 0.584037 0.700094 0.584968 11.00000 -1.50000 AFIX 0 C2 1 0.868705 0.835246 0.575363 11.00000 0.03423 0.05383 = 0.03588 0.01826 0.02075 0.02064 AFIX 43 H2 2 0.834984 0.802075 0.518729 11.00000 -1.20000 AFIX 0 C3 1 0.983857 0.864340 0.580875 11.00000 0.03923 0.06842 = 0.04692 0.02930 0.02645 0.02378 AFIX 43 H3 2 1.028862 0.851755 0.527831 11.00000 -1.20000 AFIX 0 C4 1 1.032587 0.911185 0.662778 11.00000 0.02573 0.07886 = 0.05659 0.04137 0.01881 0.01204 AFIX 43 H4 2 1.113167 0.930667 0.668571 11.00000 -1.20000 AFIX 0 C5 1 0.964336 0.930844 0.738729 11.00000 0.02332 0.05346 = 0.04165 0.02124 0.00591 -0.00049 AFIX 43 H5 2 0.996931 0.964250 0.795163 11.00000 -1.20000 AFIX 0 C6 1 0.848729 0.900755 0.730057 11.00000 0.02348 0.03889 = 0.02976 0.01333 0.00849 0.00488 C7 1 0.772708 0.916636 0.812589 11.00000 0.02392 0.03274 = 0.02560 -0.00049 0.00549 -0.00604 AFIX 23 H7A 2 0.802394 0.888959 0.883690 11.00000 -1.20000 H7B 2 0.786387 0.962937 0.837203 11.00000 -1.20000 AFIX 0 C8 1 0.558813 0.888634 0.833429 11.00000 0.02909 0.02004 = 0.01837 -0.00215 0.01200 -0.00279 AFIX 23 H8A 2 0.520471 0.929064 0.853527 11.00000 -1.20000 H8B 2 0.617018 0.870112 0.907042 11.00000 -1.20000 AFIX 0 C9 1 0.453450 0.840170 0.778666 11.00000 0.02549 0.01835 = 0.02043 0.00330 0.00944 0.00181 C10 1 0.345368 0.834951 0.815929 11.00000 0.02685 0.02928 = 0.03149 0.00769 0.01315 0.00465 AFIX 43 H10 2 0.334550 0.863336 0.875030 11.00000 -1.20000 AFIX 0 C11 1 0.253817 0.788190 0.766392 11.00000 0.02524 0.03935 = 0.04653 0.01486 0.01000 -0.00263 AFIX 43 H11 2 0.180517 0.783466 0.792489 11.00000 -1.20000 AFIX 0 C12 1 0.269448 0.748369 0.678760 11.00000 0.03242 0.03523 = 0.04116 0.00837 0.00221 -0.01236 AFIX 43 H12 2 0.206157 0.716693 0.642612 11.00000 -1.20000 AFIX 0 C13 1 0.378352 0.755135 0.644207 11.00000 0.03890 0.02596 = 0.02680 0.00029 0.00308 -0.00747 AFIX 43 H13 2 0.389232 0.727712 0.583880 11.00000 -1.20000 AFIX 0 C14 1 0.578286 0.961605 0.673867 11.00000 0.02794 0.01543 = 0.02351 0.00083 0.01126 -0.00171 AFIX 23 H14A 2 0.571848 0.999683 0.722792 11.00000 -1.20000 H14B 2 0.637356 0.973451 0.628795 11.00000 -1.20000 AFIX 0 C15 1 0.447781 0.947258 0.589490 11.00000 0.02598 0.01668 = 0.02153 0.00319 0.00962 0.00090 C16 1 0.341075 0.984151 0.590118 11.00000 0.03338 0.02023 = 0.03168 0.00586 0.01710 0.00456 AFIX 43 H16 2 0.348950 1.016452 0.648951 11.00000 -1.20000 AFIX 0 C17 1 0.223542 0.974159 0.505699 11.00000 0.02695 0.03221 = 0.03847 0.01369 0.01510 0.00544 AFIX 43 H17 2 0.151492 0.999984 0.506141 11.00000 -1.20000 AFIX 0 C18 1 0.210914 0.926674 0.420815 11.00000 0.02623 0.03597 = 0.03492 0.01268 0.00464 -0.00307 AFIX 43 H18 2 0.130395 0.920226 0.362462 11.00000 -1.20000 AFIX 0 C19 1 0.315835 0.888272 0.420583 11.00000 0.03359 0.02332 = 0.02504 0.00283 0.00517 -0.00416 AFIX 43 H19 2 0.306124 0.854845 0.363408 11.00000 -1.20000 AFIX 0 C20 1 0.435309 0.898681 0.504048 11.00000 0.02637 0.01916 = 0.02142 0.00429 0.00918 0.00006 O1W 4 0.620701 0.850845 0.311622 11.00000 0.07063 0.03151 = 0.03331 -0.00505 0.03143 -0.00099 AFIX 3 H1WA 2 0.594911 0.854315 0.370672 11.00000 -1.50000 H1WB 2 0.652781 0.813684 0.310152 11.00000 -1.50000 AFIX 0 O2W 4 0.843841 0.915455 0.284660 11.00000 0.07022 0.06176 = 0.08225 -0.01557 0.03496 -0.00398 AFIX 3 H2WA 2 0.778529 0.896744 0.292401 11.00000 -1.50000 H2WB 2 0.889047 0.888594 0.261669 11.00000 -1.50000 AFIX 0 PART 1 CL0 5 0.277270 0.991993 0.936312 21.00000 0.04327 0.04983 = 0.03810 -0.01165 -0.00189 0.01512 PART 2 CL1 5 0.331415 1.011626 0.896364 31.00000 0.11937 0.08880 = 0.08186 -0.00115 0.04017 0.00278 PART 3 CL2 5 0.603638 1.085037 0.902989 41.00000 0.10425 0.03111 = 0.02894 -0.00386 0.01632 0.01556 PART 4 CL3 5 0.492912 0.583930 0.613777 51.00000 0.12081 0.07852 = 0.03919 -0.00336 0.02033 -0.04075 PART 0 HKLF 4 REM b18140 in P2(1)/c REM R1 = 0.0350 for 9302 Fo > 4sig(Fo) and 0.0569 for all 12379 data REM 294 parameters refined using 1 restraints END WGHT 0.0380 4.0421 REM Highest difference peak 3.045, deepest hole -2.121, 1-sigma level 0.158 Q1 1 0.6967 0.8236 0.6719 11.00000 0.05 3.04 Q2 1 0.2211 0.9374 1.0251 11.00000 0.05 1.55 Q3 1 0.6320 0.8219 0.6050 11.00000 0.05 1.07 Q4 1 0.3965 1.0016 0.9473 11.00000 0.05 1.04 Q5 1 0.6479 0.7694 0.6593 11.00000 0.05 0.96 Q6 1 0.5808 0.8253 0.5741 11.00000 0.05 0.94 Q7 1 0.3033 1.0397 0.8357 11.00000 0.05 0.93 Q8 1 0.3383 0.9981 0.9438 11.00000 0.05 0.93 Q9 1 0.3564 1.0122 0.8708 11.00000 0.05 0.93 Q10 1 0.6952 0.7369 0.8003 11.00000 0.05 0.91 Q11 1 0.5516 0.8632 0.2719 11.00000 0.05 0.89 Q12 1 0.3865 1.0202 0.8816 11.00000 0.05 0.89 Q13 1 0.5995 0.7900 0.5847 11.00000 0.05 0.89 Q14 1 0.3280 1.0386 0.9046 11.00000 0.05 0.82 Q15 1 0.6332 0.8660 0.6577 11.00000 0.05 0.82 Q16 1 0.9082 0.7777 0.8415 11.00000 0.05 0.81 Q17 1 0.6796 0.7782 0.6908 11.00000 0.05 0.80 Q18 1 0.7954 0.9378 0.2134 11.00000 0.05 0.80 Q19 1 0.6428 1.1086 0.8727 11.00000 0.05 0.78 Q20 1 0.5482 0.8201 0.6557 11.00000 0.05 0.77 Q21 1 0.6257 0.7819 0.5974 11.00000 0.05 0.73 Q22 1 0.4591 0.5703 0.5998 11.00000 0.05 0.73 Q23 1 0.2661 1.0401 0.9018 11.00000 0.05 0.73 Q24 1 0.5808 1.1131 0.8986 11.00000 0.05 0.73 Q25 1 0.6821 0.8085 0.7463 11.00000 0.05 0.71 Q26 1 0.4185 1.0395 0.8991 11.00000 0.05 0.71 Q27 1 0.5094 0.5949 0.5989 11.00000 0.05 0.70 Q28 1 0.5507 1.1003 0.8447 11.00000 0.05 0.70 Q29 1 0.1832 0.8097 0.2725 11.00000 0.05 0.69 Q30 1 0.6627 0.8534 0.6270 11.00000 0.05 0.69 ; 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 0.63367(2) 0.81731(2) 0.65650(2) 0.02016(3) Uani 1 1 d . . . . . O1 O 0.5380(2) 0.86176(10) 0.50279(18) 0.0236(4) Uani 1 1 d . . . . . O2 O 0.7273(2) 0.77336(11) 0.80767(19) 0.0283(5) Uani 1 1 d . . . . . H2H H 0.807872 0.771025 0.829296 0.042 Uiso 1 1 d R U . . . N1 N 0.8026(3) 0.85323(15) 0.6496(2) 0.0285(5) Uani 1 1 d . . . . . N2 N 0.6339(2) 0.90483(11) 0.7528(2) 0.0199(4) Uani 1 1 d . . . . . N3 N 0.4696(3) 0.79976(12) 0.6941(2) 0.0216(4) Uani 1 1 d . . . . . C1 C 0.6405(4) 0.73283(16) 0.5667(3) 0.0324(7) Uani 1 1 d . . . . . H1A H 0.728842 0.716289 0.590037 0.049 Uiso 1 1 calc R U . . . H1B H 0.611815 0.741706 0.482089 0.049 Uiso 1 1 calc R U . . . H1C H 0.584037 0.700094 0.584968 0.049 Uiso 1 1 calc R U . . . C2 C 0.8687(4) 0.8352(2) 0.5754(3) 0.0391(9) Uani 1 1 d . . . . . H2 H 0.834984 0.802075 0.518729 0.047 Uiso 1 1 calc R U . . . C3 C 0.9839(4) 0.8643(3) 0.5809(4) 0.0485(11) Uani 1 1 d . . . . . H3 H 1.028862 0.851755 0.527831 0.058 Uiso 1 1 calc R U . . . C4 C 1.0326(4) 0.9112(3) 0.6628(4) 0.0523(13) Uani 1 1 d . . . . . H4 H 1.113167 0.930667 0.668571 0.063 Uiso 1 1 calc R U . . . C5 C 0.9643(3) 0.9308(2) 0.7387(4) 0.0404(9) Uani 1 1 d . . . . . H5 H 0.996931 0.964250 0.795163 0.048 Uiso 1 1 calc R U . . . C6 C 0.8487(3) 0.90075(18) 0.7301(3) 0.0306(7) Uani 1 1 d . . . . . C7 C 0.7727(3) 0.91664(17) 0.8126(3) 0.0279(6) Uani 1 1 d . . . . . H7A H 0.802394 0.888959 0.883690 0.033 Uiso 1 1 calc R U . . . H7B H 0.786387 0.962937 0.837203 0.033 Uiso 1 1 calc R U . . . C8 C 0.5588(3) 0.88863(14) 0.8334(2) 0.0214(5) Uani 1 1 d . . . . . H8A H 0.520471 0.929064 0.853527 0.026 Uiso 1 1 calc R U . . . H8B H 0.617018 0.870112 0.907042 0.026 Uiso 1 1 calc R U . . . C9 C 0.4534(3) 0.84017(14) 0.7787(2) 0.0209(5) Uani 1 1 d . . . . . C10 C 0.3454(3) 0.83495(17) 0.8159(3) 0.0283(6) Uani 1 1 d . . . . . H10 H 0.334550 0.863336 0.875030 0.034 Uiso 1 1 calc R U . . . C11 C 0.2538(3) 0.7882(2) 0.7664(4) 0.0373(8) Uani 1 1 d . . . . . H11 H 0.180517 0.783466 0.792489 0.045 Uiso 1 1 calc R U . . . C12 C 0.2694(4) 0.74837(19) 0.6788(4) 0.0383(8) Uani 1 1 d . . . . . H12 H 0.206157 0.716693 0.642612 0.046 Uiso 1 1 calc R U . . . C13 C 0.3784(3) 0.75514(17) 0.6442(3) 0.0321(7) Uani 1 1 d . . . . . H13 H 0.389232 0.727712 0.583880 0.039 Uiso 1 1 calc R U . . . C14 C 0.5783(3) 0.96160(13) 0.6739(3) 0.0215(5) Uani 1 1 d . . . . . H14A H 0.571848 0.999683 0.722792 0.026 Uiso 1 1 calc R U . . . H14B H 0.637356 0.973451 0.628795 0.026 Uiso 1 1 calc R U . . . C15 C 0.4478(3) 0.94726(14) 0.5895(2) 0.0209(5) Uani 1 1 d . . . . . C16 C 0.3411(3) 0.98415(15) 0.5901(3) 0.0268(6) Uani 1 1 d . . . . . H16 H 0.348950 1.016452 0.648951 0.032 Uiso 1 1 calc R U . . . C17 C 0.2235(3) 0.97416(17) 0.5057(3) 0.0314(7) Uani 1 1 d . . . . . H17 H 0.151492 0.999984 0.506141 0.038 Uiso 1 1 calc R U . . . C18 C 0.2109(3) 0.92667(18) 0.4208(3) 0.0334(7) Uani 1 1 d . . . . . H18 H 0.130395 0.920226 0.362462 0.040 Uiso 1 1 calc R U . . . C19 C 0.3158(3) 0.88827(16) 0.4206(3) 0.0282(6) Uani 1 1 d . . . . . H19 H 0.306124 0.854845 0.363408 0.034 Uiso 1 1 calc R U . . . C20 C 0.4353(3) 0.89868(14) 0.5040(3) 0.0219(5) Uani 1 1 d . . . . . O1W O 0.6207(3) 0.85084(13) 0.3116(2) 0.0417(7) Uani 1 1 d . . . . . H1WA H 0.594911 0.854315 0.370672 0.062 Uiso 1 1 d R U . . . H1WB H 0.652781 0.813684 0.310152 0.062 Uiso 1 1 d R U . . . O2W O 0.8438(4) 0.91546(19) 0.2847(4) 0.0688(10) Uani 1 1 d . . . . . H2WA H 0.778529 0.896744 0.292401 0.103 Uiso 1 1 d R U . . . H2WB H 0.889047 0.888594 0.261669 0.103 Uiso 1 1 d R U . . . Cl0 Cl 0.2773(4) 0.9920(2) 0.9363(3) 0.0470(10) Uani 0.300(3) 1 d . . P A 1 Cl1 Cl 0.3314(14) 1.0116(6) 0.8964(11) 0.095(4) Uani 0.172(3) 1 d . . P B 2 Cl2 Cl 0.6036(6) 1.08504(18) 0.9030(3) 0.0557(13) Uani 0.298(3) 1 d . . P C 3 Cl3 Cl 0.4929(10) 0.5839(4) 0.6138(5) 0.080(3) Uani 0.229(3) 1 d . . P D 4 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 0.02798(5) 0.01796(5) 0.01692(5) 0.00138(4) 0.01043(3) 0.00381(4) O1 0.0336(11) 0.0219(10) 0.0167(9) 0.0016(7) 0.0097(8) 0.0066(8) O2 0.0339(12) 0.0300(11) 0.0209(10) 0.0073(8) 0.0084(8) 0.0088(9) N1 0.0263(13) 0.0370(15) 0.0260(12) 0.0106(11) 0.0137(10) 0.0068(11) N2 0.0249(11) 0.0173(10) 0.0186(10) 0.0003(8) 0.0084(8) -0.0011(8) N3 0.0292(12) 0.0165(9) 0.0195(10) 0.0020(8) 0.0081(9) -0.0022(8) C1 0.053(2) 0.0232(14) 0.0256(14) 0.0016(11) 0.0190(14) 0.0096(14) C2 0.0342(18) 0.054(2) 0.0359(18) 0.0183(16) 0.0208(15) 0.0206(16) C3 0.039(2) 0.068(3) 0.047(2) 0.029(2) 0.0265(18) 0.024(2) C4 0.0257(17) 0.079(3) 0.057(3) 0.041(3) 0.0188(17) 0.0120(19) C5 0.0233(15) 0.053(2) 0.042(2) 0.0212(17) 0.0059(14) -0.0005(14) C6 0.0235(14) 0.0389(18) 0.0298(15) 0.0133(13) 0.0085(12) 0.0049(12) C7 0.0239(14) 0.0327(16) 0.0256(14) -0.0005(12) 0.0055(11) -0.0060(11) C8 0.0291(14) 0.0200(12) 0.0184(11) -0.0021(9) 0.0120(10) -0.0028(10) C9 0.0255(13) 0.0184(11) 0.0204(12) 0.0033(9) 0.0094(10) 0.0018(10) C10 0.0268(15) 0.0293(15) 0.0315(15) 0.0077(12) 0.0131(12) 0.0046(11) C11 0.0252(15) 0.0394(19) 0.047(2) 0.0149(16) 0.0100(14) -0.0026(13) C12 0.0324(17) 0.0352(18) 0.0412(19) 0.0084(15) 0.0022(14) -0.0124(14) C13 0.0389(18) 0.0260(15) 0.0268(15) 0.0003(12) 0.0031(13) -0.0075(13) C14 0.0279(13) 0.0154(11) 0.0235(12) 0.0008(9) 0.0113(10) -0.0017(9) C15 0.0260(13) 0.0167(11) 0.0215(12) 0.0032(9) 0.0096(10) 0.0009(9) C16 0.0334(16) 0.0202(13) 0.0317(15) 0.0059(11) 0.0171(12) 0.0046(11) C17 0.0270(15) 0.0322(16) 0.0385(17) 0.0137(13) 0.0151(13) 0.0054(12) C18 0.0262(15) 0.0360(17) 0.0349(17) 0.0127(14) 0.0046(13) -0.0031(13) C19 0.0336(16) 0.0233(14) 0.0250(14) 0.0028(11) 0.0052(12) -0.0042(11) C20 0.0264(13) 0.0192(12) 0.0214(12) 0.0043(9) 0.0092(10) 0.0001(10) O1W 0.071(2) 0.0315(13) 0.0333(13) -0.0050(10) 0.0314(13) -0.0010(13) O2W 0.070(3) 0.062(2) 0.082(3) -0.016(2) 0.035(2) -0.0040(19) Cl0 0.0433(19) 0.050(2) 0.0381(17) -0.0116(15) -0.0019(14) 0.0151(15) Cl1 0.119(10) 0.089(8) 0.082(7) -0.001(6) 0.040(7) 0.003(7) Cl2 0.104(4) 0.0311(16) 0.0289(15) -0.0039(12) 0.016(2) 0.016(2) Cl3 0.121(7) 0.079(5) 0.039(3) -0.003(3) 0.020(4) -0.041(5) 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 O2 Pt1 N3 87.80(10) . . O2 Pt1 N1 88.84(11) . . N3 Pt1 N1 165.25(11) . . O2 Pt1 O1 179.79(10) . . N3 Pt1 O1 92.03(10) . . N1 Pt1 O1 91.36(10) . . O2 Pt1 C1 90.20(12) . . N3 Pt1 C1 98.33(13) . . N1 Pt1 C1 96.04(14) . . O1 Pt1 C1 89.71(11) . . O2 Pt1 N2 88.52(9) . . N3 Pt1 N2 83.24(10) . . N1 Pt1 N2 82.32(11) . . O1 Pt1 N2 91.58(9) . . C1 Pt1 N2 177.94(13) . . C20 O1 Pt1 115.96(17) . . Pt1 O2 H2H 120.1 . . C6 N1 C2 120.3(3) . . C6 N1 Pt1 112.3(2) . . C2 N1 Pt1 127.4(3) . . C8 N2 C7 114.2(2) . . C8 N2 C14 112.6(2) . . C7 N2 C14 109.4(2) . . C8 N2 Pt1 104.77(16) . . C7 N2 Pt1 103.21(19) . . C14 N2 Pt1 112.19(17) . . C13 N3 C9 119.6(3) . . C13 N3 Pt1 127.7(2) . . C9 N3 Pt1 112.71(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 121.0(4) . . N1 C2 H2 119.5 . . C3 C2 H2 119.5 . . C4 C3 C2 119.4(4) . . C4 C3 H3 120.3 . . C2 C3 H3 120.3 . . C3 C4 C5 120.1(4) . . C3 C4 H4 119.9 . . C5 C4 H4 119.9 . . C6 C5 C4 118.7(4) . . C6 C5 H5 120.6 . . C4 C5 H5 120.6 . . N1 C6 C5 120.5(3) . . N1 C6 C7 117.5(3) . . C5 C6 C7 122.0(4) . . N2 C7 C6 109.7(3) . . N2 C7 H7A 109.7 . . C6 C7 H7A 109.7 . . N2 C7 H7B 109.7 . . C6 C7 H7B 109.7 . . H7A C7 H7B 108.2 . . N2 C8 C9 111.4(2) . . N2 C8 H8A 109.3 . . C9 C8 H8A 109.3 . . N2 C8 H8B 109.3 . . C9 C8 H8B 109.3 . . H8A C8 H8B 108.0 . . N3 C9 C10 120.6(3) . . N3 C9 C8 117.8(3) . . C10 C9 C8 121.5(3) . . C11 C10 C9 119.5(3) . . C11 C10 H10 120.3 . . C9 C10 H10 120.3 . . C12 C11 C10 119.6(3) . . C12 C11 H11 120.2 . . C10 C11 H11 120.2 . . C11 C12 C13 119.2(3) . . C11 C12 H12 120.4 . . C13 C12 H12 120.4 . . N3 C13 C12 121.6(3) . . N3 C13 H13 119.2 . . C12 C13 H13 119.2 . . C15 C14 N2 112.9(2) . . C15 C14 H14A 109.0 . . N2 C14 H14A 109.0 . . C15 C14 H14B 109.0 . . N2 C14 H14B 109.0 . . H14A C14 H14B 107.8 . . C16 C15 C20 119.6(3) . . C16 C15 C14 121.0(3) . . C20 C15 C14 119.2(3) . . C17 C16 C15 120.5(3) . . C17 C16 H16 119.7 . . C15 C16 H16 119.7 . . C18 C17 C16 120.1(3) . . C18 C17 H17 120.0 . . C16 C17 H17 120.0 . . C17 C18 C19 120.2(3) . . C17 C18 H18 119.9 . . C19 C18 H18 119.9 . . C18 C19 C20 120.2(3) . . C18 C19 H19 119.9 . . C20 C19 H19 119.9 . . O1 C20 C19 120.2(3) . . O1 C20 C15 120.5(3) . . C19 C20 C15 119.3(3) . . H1WA O1W H1WB 110.1 . . H2WA O2W H2WB 110.1 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 O2 1.998(2) . Pt1 N3 2.011(3) . Pt1 N1 2.013(3) . Pt1 O1 2.030(2) . Pt1 C1 2.049(3) . Pt1 N2 2.129(2) . O1 C20 1.357(4) . O2 H2H 0.8401 . N1 C6 1.352(5) . N1 C2 1.356(4) . N2 C8 1.483(4) . N2 C7 1.486(4) . N2 C14 1.503(4) . N3 C13 1.349(4) . N3 C9 1.359(4) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C2 C3 1.376(6) . C2 H2 0.9500 . C3 C4 1.357(8) . C3 H3 0.9500 . C4 C5 1.400(6) . C4 H4 0.9500 . C5 C6 1.381(5) . C5 H5 0.9500 . C6 C7 1.508(5) . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 C9 1.509(4) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 C10 1.389(4) . C10 C11 1.380(5) . C10 H10 0.9500 . C11 C12 1.379(6) . C11 H11 0.9500 . C12 C13 1.382(5) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C15 1.502(4) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C16 1.392(4) . C15 C20 1.402(4) . C16 C17 1.384(5) . C16 H16 0.9500 . C17 C18 1.381(6) . C17 H17 0.9500 . C18 C19 1.391(5) . C18 H18 0.9500 . C19 C20 1.396(4) . C19 H19 0.9500 . O1W H1WA 0.8400 . O1W H1WB 0.8400 . O2W H2WA 0.8400 . O2W H2WB 0.8400 . 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 C8 H8A Cl1 0.99 2.84 3.773(14) 158.2 . C10 H10 Cl0 0.95 2.85 3.690(5) 147.4 . C10 H10 Cl2 0.95 2.74 3.626(5) 155.0 3_677 C13 H13 Cl2 0.95 2.92 3.542(5) 123.8 2_646 C14 H14A Cl2 0.99 2.71 3.675(4) 164.1 . C14 H14A Cl3 0.99 2.85 3.813(7) 163.4 2_656 O1W H1WA O1 0.84 1.87 2.714(3) 179.7 . O1W H1WB O2 0.84 1.96 2.803(4) 179.6 4_575 O2W H2WA O1W 0.84 2.04 2.879(5) 179.6 . 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 0.6(5) . . . . Pt1 N1 C2 C3 180.0(3) . . . . N1 C2 C3 C4 0.8(6) . . . . C2 C3 C4 C5 -1.7(6) . . . . C3 C4 C5 C6 1.3(6) . . . . C2 N1 C6 C5 -0.9(5) . . . . Pt1 N1 C6 C5 179.6(3) . . . . C2 N1 C6 C7 -177.9(3) . . . . Pt1 N1 C6 C7 2.6(4) . . . . C4 C5 C6 N1 0.0(5) . . . . C4 C5 C6 C7 176.8(3) . . . . C8 N2 C7 C6 153.1(3) . . . . C14 N2 C7 C6 -79.7(3) . . . . Pt1 N2 C7 C6 39.9(3) . . . . N1 C6 C7 N2 -30.9(4) . . . . C5 C6 C7 N2 152.2(3) . . . . C7 N2 C8 C9 -145.2(3) . . . . C14 N2 C8 C9 89.2(3) . . . . Pt1 N2 C8 C9 -33.0(3) . . . . C13 N3 C9 C10 1.4(4) . . . . Pt1 N3 C9 C10 -179.9(2) . . . . C13 N3 C9 C8 179.1(3) . . . . Pt1 N3 C9 C8 -2.3(3) . . . . N2 C8 C9 N3 25.5(4) . . . . N2 C8 C9 C10 -156.9(3) . . . . N3 C9 C10 C11 0.0(5) . . . . C8 C9 C10 C11 -177.5(3) . . . . C9 C10 C11 C12 -1.5(5) . . . . C10 C11 C12 C13 1.5(5) . . . . C9 N3 C13 C12 -1.4(5) . . . . Pt1 N3 C13 C12 -179.9(3) . . . . C11 C12 C13 N3 0.0(5) . . . . C8 N2 C14 C15 -65.2(3) . . . . C7 N2 C14 C15 166.6(2) . . . . Pt1 N2 C14 C15 52.7(3) . . . . N2 C14 C15 C16 119.9(3) . . . . N2 C14 C15 C20 -64.2(3) . . . . C20 C15 C16 C17 -1.3(4) . . . . C14 C15 C16 C17 174.5(3) . . . . C15 C16 C17 C18 0.9(5) . . . . C16 C17 C18 C19 0.7(5) . . . . C17 C18 C19 C20 -1.8(5) . . . . Pt1 O1 C20 C19 -127.1(2) . . . . Pt1 O1 C20 C15 52.5(3) . . . . C18 C19 C20 O1 -179.1(3) . . . . C18 C19 C20 C15 1.3(4) . . . . C16 C15 C20 O1 -179.3(3) . . . . C14 C15 C20 O1 4.8(4) . . . . C16 C15 C20 C19 0.2(4) . . . . C14 C15 C20 C19 -175.7(3) . . . .