#------------------------------------------------------------------------------ #$Date: 2021-09-15 12:06:18 +0300 (Wed, 15 Sep 2021) $ #$Revision: 269153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564656.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_1564656 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 H27 Cl2 N3 O5 Pt' _chemical_formula_weight 655.43 _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 mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 96.462(10) _cell_angle_beta 99.179(10) _cell_angle_gamma 103.836(12) _cell_formula_units_Z 2 _cell_length_a 10.600(3) _cell_length_b 10.954(2) _cell_length_c 11.714(3) _cell_measurement_reflns_used 9967 _cell_measurement_temperature 110 _cell_measurement_theta_max 33.81 _cell_measurement_theta_min 2.40 _cell_volume 1287.6(6) _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 0.997 _diffrn_measured_fraction_theta_max 0.990 _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 0.0622 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 120466 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 42.262 _diffrn_reflns_theta_min 2.940 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 5.689 _exptl_absorpt_correction_T_max 0.7483 _exptl_absorpt_correction_T_min 0.6564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.691 _exptl_crystal_description prism _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _refine_diff_density_max 3.804 _refine_diff_density_min -2.821 _refine_diff_density_rms 0.193 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 18088 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0366 _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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0852 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 14828 _reflns_number_total 18088 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-507-119580.cif _cod_data_source_block 5 _cod_original_cell_volume 1287.5(5) _cod_database_code 1564656 _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 0.092 _shelx_estimated_absorpt_t_max 0.600 _shelx_res_file ; TITL b18209 in P-1 b18209.res created by SHELXL-2016/6 at 11:24:28 on 11-Jan-2018 CELL 0.71073 10.59993 10.95381 11.71403 96.4619 99.1787 103.8362 ZERR 2 0.00250 0.00247 0.00286 0.0095 0.0097 0.0119 LATT 1 SFAC C H N O CL PT UNIT 40 54 6 10 4 2 TEMP -163.110 SIZE 0.10 0.12 0.80 ACTA REM omit reflections blocked by beamstop OMIT 0 0 1 OMIT 0 1 0 OMIT 1 0 0 OMIT 0 -1 1 OMIT 0 0 2 OMIT -1 2 0 OMIT 0 2 2 OMIT -2 0 3 REM the following two reflections were omitted because they gave Error/ESD REM of greater than 10. Looking at the frames, they seemed to be misaligned in REM Z direction (the centroid was not where the orientation matrix predicts it t OMIT 2 -1 2 OMIT -4 3 1 ABIN L.S. 12 0 38 FMAP 2 PLAN 25 BOND $H CONF REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+2, -z+2 HTAB O2 Cl2_$1 EQIV $2 x, y-1, z HTAB C5 Cl2_$2 HTAB C8 O2W EQIV $3 x-1, y, z HTAB C13 O3W_$3 HTAB O1W O1 HTAB O1W O3W_$3 HTAB O2W O2_$1 HTAB O2W O2 HTAB O3W O2W WGHT 0.044100 FVAR 0.12440 PT1 6 0.711695 0.716438 0.874424 11.00000 0.01561 0.01414 = 0.01355 0.00069 0.00389 0.00284 O1 4 0.543142 0.611576 0.766323 11.00000 0.01703 0.01916 = 0.02153 -0.00255 0.00355 0.00366 O2 4 0.873697 0.823898 0.985439 11.00000 0.01991 0.01985 = 0.01848 0.00044 0.00062 0.00221 AFIX 3 H2H 2 0.882687 0.807097 1.054018 11.00000 -1.50000 AFIX 0 N1 3 0.778680 0.560616 0.900227 11.00000 0.02083 0.01499 = 0.01528 0.00255 0.00166 0.00237 N2 3 0.679857 0.876760 0.819807 11.00000 0.02038 0.01727 = 0.02181 -0.00008 0.00173 0.00595 N3 3 0.819314 0.720307 0.735275 11.00000 0.01720 0.01566 = 0.01479 0.00223 0.00356 0.00294 C1 1 0.608712 0.721276 1.007340 11.00000 0.02643 0.03221 = 0.02034 -0.00051 0.01045 0.00547 AFIX 137 H1A 2 0.637752 0.670283 1.064790 11.00000 -1.50000 H1B 2 0.513835 0.686372 0.975660 11.00000 -1.50000 H1C 2 0.625127 0.809495 1.045357 11.00000 -1.50000 AFIX 0 C2 1 0.735031 0.471288 0.965860 11.00000 0.02673 0.01981 = 0.02165 0.00610 0.00305 -0.00006 AFIX 43 H2 2 0.670706 0.481755 1.011413 11.00000 -1.20000 AFIX 0 C3 1 0.783646 0.364416 0.967065 11.00000 0.03734 0.01977 = 0.02912 0.01095 -0.00039 0.00145 AFIX 43 H3 2 0.751573 0.301403 1.012439 11.00000 -1.20000 AFIX 0 C4 1 0.877777 0.349688 0.902938 11.00000 0.03589 0.01755 = 0.02893 0.00292 -0.00258 0.00759 AFIX 43 H4 2 0.911780 0.276976 0.903971 11.00000 -1.20000 AFIX 0 C5 1 0.922919 0.441932 0.836526 11.00000 0.02939 0.01977 = 0.02385 -0.00013 -0.00042 0.00979 AFIX 43 H5 2 0.987958 0.432920 0.791334 11.00000 -1.20000 AFIX 0 C6 1 0.872253 0.547600 0.836632 11.00000 0.02032 0.01742 = 0.01595 0.00013 -0.00003 0.00571 C7 1 0.922699 0.653402 0.769305 11.00000 0.01768 0.02020 = 0.01822 0.00209 0.00489 0.00677 AFIX 23 H7A 2 1.002034 0.714980 0.818413 11.00000 -1.20000 H7B 2 0.948786 0.617247 0.698128 11.00000 -1.20000 AFIX 0 C8 1 0.871610 0.858843 0.732485 11.00000 0.01980 0.01620 = 0.02306 0.00574 0.00500 0.00244 AFIX 23 H8A 2 0.896366 0.871256 0.655791 11.00000 -1.20000 H8B 2 0.951609 0.894845 0.794401 11.00000 -1.20000 AFIX 0 C9 1 0.765805 0.925893 0.752060 11.00000 0.02286 0.01630 = 0.02127 0.00246 -0.00022 0.00239 C10 1 0.759448 1.036679 0.706864 11.00000 0.03626 0.01702 = 0.02449 0.00441 -0.00164 0.00582 AFIX 43 H10 2 0.819298 1.070321 0.658898 11.00000 -1.20000 AFIX 0 C11 1 0.664224 1.097516 0.732886 11.00000 0.04454 0.02040 = 0.03058 0.00180 -0.00793 0.01319 AFIX 43 H11 2 0.659874 1.174669 0.704643 11.00000 -1.20000 AFIX 0 C12 1 0.575639 1.044786 0.800356 11.00000 0.03724 0.02674 = 0.03200 -0.00598 -0.00653 0.01832 AFIX 43 H12 2 0.509106 1.084662 0.817699 11.00000 -1.20000 AFIX 0 C13 1 0.585064 0.933502 0.842200 11.00000 0.02448 0.02531 = 0.02540 -0.00436 -0.00022 0.01143 AFIX 43 H13 2 0.523602 0.896519 0.887495 11.00000 -1.20000 AFIX 0 C14 1 0.731661 0.658279 0.619251 11.00000 0.02035 0.01979 = 0.01451 0.00298 0.00274 0.00292 AFIX 23 H14A 2 0.672599 0.712364 0.595354 11.00000 -1.20000 H14B 2 0.787620 0.653383 0.559702 11.00000 -1.20000 AFIX 0 C15 1 0.648687 0.527243 0.621083 11.00000 0.01805 0.01900 = 0.01398 0.00036 0.00059 0.00348 C16 1 0.554164 0.511218 0.692700 11.00000 0.01670 0.01770 = 0.01496 0.00078 0.00067 0.00332 C17 1 0.466502 0.391844 0.686863 11.00000 0.01950 0.01933 = 0.01926 0.00184 0.00179 0.00129 AFIX 43 H17 2 0.401611 0.381371 0.734858 11.00000 -1.20000 AFIX 0 C18 1 0.474849 0.288237 0.610199 11.00000 0.02450 0.01749 = 0.02007 0.00131 -0.00359 0.00193 AFIX 43 H18 2 0.415465 0.206853 0.605210 11.00000 -1.20000 AFIX 0 C19 1 0.570858 0.305315 0.541266 11.00000 0.02748 0.01919 = 0.01653 -0.00211 -0.00167 0.00681 CL1 5 0.581827 0.175221 0.446629 11.00000 0.04730 0.02399 = 0.02570 -0.00751 0.00279 0.01009 C20 1 0.657541 0.422460 0.546331 11.00000 0.02402 0.02260 = 0.01579 -0.00180 0.00275 0.00675 AFIX 43 H20 2 0.723160 0.431866 0.499058 11.00000 -1.20000 AFIX 0 O1W 4 0.279489 0.620893 0.766761 11.00000 0.03807 0.05590 = 0.05347 0.00538 0.02419 0.01591 AFIX 3 H1WA 2 0.357199 0.613442 0.772341 11.00000 -1.50000 H1WB 2 0.280689 0.697413 0.786229 11.00000 -1.50000 AFIX 0 O2W 4 1.129412 0.922229 0.980981 11.00000 0.02497 0.02071 = 0.03358 -0.00217 0.00269 0.00491 AFIX 3 H2WA 2 1.122952 0.996929 0.996951 11.00000 -1.50000 H2WB 2 1.048132 0.887889 0.973812 11.00000 -1.50000 AFIX 0 O3W 4 1.284043 0.870167 0.829800 11.00000 0.06426 0.06343 = 0.10132 0.00944 0.05306 0.02617 AFIX 3 H3WA 2 1.245162 0.881487 0.765090 11.00000 -1.50000 H3WB 2 1.238853 0.908837 0.865580 11.00000 -1.50000 AFIX 0 CL2 5 1.108189 1.213447 0.762252 11.00000 0.10361 0.11205 = 0.08873 0.03409 0.04182 0.05699 HKLF 4 REM b18209 in P-1 REM R1 = 0.0366 for 14828 Fo > 4sig(Fo) and 0.0505 for all 18088 data REM 281 parameters refined using 0 restraints END WGHT 0.0441 0.0000 REM Highest difference peak 3.804, deepest hole -2.821, 1-sigma level 0.193 Q1 1 0.7213 0.7745 0.8193 11.00000 0.05 1.46 Q2 1 0.6860 0.6412 0.9149 11.00000 0.05 1.26 Q3 1 0.7836 0.6857 0.8609 11.00000 0.05 1.25 Q4 1 0.6948 0.7292 0.8251 11.00000 0.05 1.19 Q5 1 0.7391 0.7129 0.9279 11.00000 0.05 1.16 Q6 1 0.6357 0.7443 0.8827 11.00000 0.05 1.08 Q7 1 0.7638 0.7273 0.8094 11.00000 0.05 1.08 Q8 1 0.6373 0.6611 0.8968 11.00000 0.05 1.05 Q9 1 0.6776 0.7768 0.9997 11.00000 0.05 1.04 Q10 1 0.6996 0.6779 0.8712 11.00000 0.05 0.98 Q11 1 0.6627 0.7143 0.9383 11.00000 0.05 0.96 Q12 1 0.7816 0.7294 0.8979 11.00000 0.05 0.94 Q13 1 0.7866 0.7730 0.8492 11.00000 0.05 0.94 Q14 1 0.6978 0.7297 0.9633 11.00000 0.05 0.89 Q15 1 0.7374 0.6560 0.8291 11.00000 0.05 0.83 Q16 1 0.6967 0.6672 0.7990 11.00000 0.05 0.82 Q17 1 0.7383 0.6381 0.8697 11.00000 0.05 0.81 Q18 1 0.8179 0.7879 0.7375 11.00000 0.05 0.81 Q19 1 0.7126 0.7818 0.9399 11.00000 0.05 0.79 Q20 1 0.5032 0.4599 0.7127 11.00000 0.05 0.78 Q21 1 0.5362 0.1513 0.4742 11.00000 0.05 0.78 Q22 1 0.9015 0.4949 0.8324 11.00000 0.05 0.77 Q23 1 1.2935 1.0051 0.7265 11.00000 0.05 0.76 Q24 1 1.1778 1.1987 0.6670 11.00000 0.05 0.76 Q25 1 0.6416 0.4783 0.5694 11.00000 0.05 0.75 ; 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 0.71170(2) 0.71644(2) 0.87442(2) 0.01462(2) Uani 1 1 d . . . . . O1 O 0.54314(16) 0.61158(15) 0.76632(15) 0.0199(3) Uani 1 1 d . . . . . O2 O 0.87370(17) 0.82390(15) 0.98544(15) 0.0205(3) Uani 1 1 d . . . . . H2H H 0.882687 0.807097 1.054018 0.031 Uiso 1 1 d R U . . . N1 N 0.77868(19) 0.56062(17) 0.90023(16) 0.0176(3) Uani 1 1 d . . . . . N2 N 0.67986(19) 0.87676(18) 0.81981(18) 0.0202(3) Uani 1 1 d . . . . . N3 N 0.81931(18) 0.72031(17) 0.73527(15) 0.0161(3) Uani 1 1 d . . . . . C1 C 0.6087(3) 0.7213(3) 1.0073(2) 0.0264(5) Uani 1 1 d . . . . . H1A H 0.637752 0.670283 1.064790 0.040 Uiso 1 1 calc R U . . . H1B H 0.513835 0.686372 0.975660 0.040 Uiso 1 1 calc R U . . . H1C H 0.625127 0.809495 1.045357 0.040 Uiso 1 1 calc R U . . . C2 C 0.7350(3) 0.4713(2) 0.9659(2) 0.0238(4) Uani 1 1 d . . . . . H2 H 0.670706 0.481755 1.011413 0.029 Uiso 1 1 calc R U . . . C3 C 0.7836(3) 0.3644(2) 0.9671(2) 0.0300(5) Uani 1 1 d . . . . . H3 H 0.751573 0.301403 1.012439 0.036 Uiso 1 1 calc R U . . . C4 C 0.8778(3) 0.3497(2) 0.9029(2) 0.0284(5) Uani 1 1 d . . . . . H4 H 0.911780 0.276976 0.903971 0.034 Uiso 1 1 calc R U . . . C5 C 0.9229(3) 0.4419(2) 0.8365(2) 0.0247(4) Uani 1 1 d . . . . . H5 H 0.987958 0.432920 0.791334 0.030 Uiso 1 1 calc R U . . . C6 C 0.8723(2) 0.54760(19) 0.83663(18) 0.0184(3) Uani 1 1 d . . . . . C7 C 0.9227(2) 0.6534(2) 0.76931(19) 0.0183(3) Uani 1 1 d . . . . . H7A H 1.002034 0.714980 0.818413 0.022 Uiso 1 1 calc R U . . . H7B H 0.948786 0.617247 0.698128 0.022 Uiso 1 1 calc R U . . . C8 C 0.8716(2) 0.8588(2) 0.7325(2) 0.0198(4) Uani 1 1 d . . . . . H8A H 0.896366 0.871256 0.655791 0.024 Uiso 1 1 calc R U . . . H8B H 0.951609 0.894845 0.794401 0.024 Uiso 1 1 calc R U . . . C9 C 0.7658(2) 0.9259(2) 0.7521(2) 0.0212(4) Uani 1 1 d . . . . . C10 C 0.7594(3) 1.0367(2) 0.7069(2) 0.0269(5) Uani 1 1 d . . . . . H10 H 0.819298 1.070321 0.658898 0.032 Uiso 1 1 calc R U . . . C11 C 0.6642(3) 1.0975(2) 0.7329(3) 0.0329(6) Uani 1 1 d . . . . . H11 H 0.659874 1.174669 0.704643 0.040 Uiso 1 1 calc R U . . . C12 C 0.5756(3) 1.0448(3) 0.8004(3) 0.0326(6) Uani 1 1 d . . . . . H12 H 0.509106 1.084662 0.817699 0.039 Uiso 1 1 calc R U . . . C13 C 0.5851(3) 0.9335(2) 0.8422(2) 0.0255(4) Uani 1 1 d . . . . . H13 H 0.523602 0.896519 0.887495 0.031 Uiso 1 1 calc R U . . . C14 C 0.7317(2) 0.6583(2) 0.61925(18) 0.0187(3) Uani 1 1 d . . . . . H14A H 0.672599 0.712364 0.595354 0.022 Uiso 1 1 calc R U . . . H14B H 0.787620 0.653383 0.559702 0.022 Uiso 1 1 calc R U . . . C15 C 0.6487(2) 0.5272(2) 0.62108(18) 0.0177(3) Uani 1 1 d . . . . . C16 C 0.5542(2) 0.51122(19) 0.69270(18) 0.0171(3) Uani 1 1 d . . . . . C17 C 0.4665(2) 0.3918(2) 0.6869(2) 0.0203(4) Uani 1 1 d . . . . . H17 H 0.401611 0.381371 0.734858 0.024 Uiso 1 1 calc R U . . . C18 C 0.4748(2) 0.2882(2) 0.6102(2) 0.0223(4) Uani 1 1 d . . . . . H18 H 0.415465 0.206853 0.605210 0.027 Uiso 1 1 calc R U . . . C19 C 0.5709(2) 0.3053(2) 0.54127(19) 0.0220(4) Uani 1 1 d . . . . . Cl1 Cl 0.58183(8) 0.17522(6) 0.44663(6) 0.03360(14) Uani 1 1 d . . . . . C20 C 0.6575(2) 0.4225(2) 0.54633(19) 0.0212(4) Uani 1 1 d . . . . . H20 H 0.723160 0.431866 0.499058 0.025 Uiso 1 1 calc R U . . . O1W O 0.2795(2) 0.6209(3) 0.7668(2) 0.0470(6) Uani 1 1 d . . . . . H1WA H 0.357199 0.613442 0.772341 0.071 Uiso 1 1 d R U . . . H1WB H 0.280689 0.697413 0.786229 0.071 Uiso 1 1 d R U . . . O2W O 1.12941(19) 0.92223(17) 0.98098(17) 0.0275(4) Uani 1 1 d . . . . . H2WA H 1.122952 0.996929 0.996951 0.041 Uiso 1 1 d R U . . . H2WB H 1.048132 0.887889 0.973812 0.041 Uiso 1 1 d R U . . . O3W O 1.2840(3) 0.8702(3) 0.8298(3) 0.0707(10) Uani 1 1 d . . . . . H3WA H 1.245162 0.881487 0.765090 0.106 Uiso 1 1 d R U . . . H3WB H 1.238853 0.908837 0.865580 0.106 Uiso 1 1 d R U . . . Cl2 Cl 1.10819(18) 1.21345(17) 0.76225(15) 0.0923(5) 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 0.01561(3) 0.01414(3) 0.01355(3) 0.00069(2) 0.00389(2) 0.00284(2) O1 0.0170(7) 0.0192(7) 0.0215(7) -0.0025(5) 0.0036(5) 0.0037(5) O2 0.0199(7) 0.0199(7) 0.0185(7) 0.0004(5) 0.0006(5) 0.0022(5) N1 0.0208(8) 0.0150(7) 0.0153(7) 0.0026(5) 0.0017(6) 0.0024(6) N2 0.0204(8) 0.0173(7) 0.0218(8) -0.0001(6) 0.0017(6) 0.0059(6) N3 0.0172(7) 0.0157(7) 0.0148(7) 0.0022(5) 0.0036(5) 0.0029(5) C1 0.0264(11) 0.0322(12) 0.0203(10) -0.0005(8) 0.0104(8) 0.0055(9) C2 0.0267(11) 0.0198(9) 0.0216(10) 0.0061(7) 0.0031(8) -0.0001(8) C3 0.0373(14) 0.0198(10) 0.0291(12) 0.0109(9) -0.0004(10) 0.0015(9) C4 0.0359(13) 0.0175(9) 0.0289(12) 0.0029(8) -0.0026(10) 0.0076(9) C5 0.0294(11) 0.0198(9) 0.0239(10) -0.0001(8) -0.0004(8) 0.0098(8) C6 0.0203(9) 0.0174(8) 0.0159(8) 0.0001(6) 0.0000(7) 0.0057(7) C7 0.0177(8) 0.0202(8) 0.0182(9) 0.0021(7) 0.0049(7) 0.0068(7) C8 0.0198(9) 0.0162(8) 0.0231(10) 0.0057(7) 0.0050(7) 0.0024(7) C9 0.0229(10) 0.0163(8) 0.0213(10) 0.0025(7) -0.0002(7) 0.0024(7) C10 0.0363(13) 0.0170(9) 0.0245(11) 0.0044(8) -0.0016(9) 0.0058(8) C11 0.0445(16) 0.0204(10) 0.0306(13) 0.0018(9) -0.0079(11) 0.0132(10) C12 0.0372(14) 0.0267(11) 0.0320(13) -0.0060(9) -0.0065(11) 0.0183(11) C13 0.0245(10) 0.0253(10) 0.0254(11) -0.0044(8) -0.0002(8) 0.0114(8) C14 0.0203(9) 0.0198(8) 0.0145(8) 0.0030(6) 0.0027(7) 0.0029(7) C15 0.0180(8) 0.0190(8) 0.0140(8) 0.0004(6) 0.0006(6) 0.0035(6) C16 0.0167(8) 0.0177(8) 0.0150(8) 0.0008(6) 0.0007(6) 0.0033(6) C17 0.0195(9) 0.0193(8) 0.0193(9) 0.0018(7) 0.0018(7) 0.0013(7) C18 0.0245(10) 0.0175(8) 0.0201(9) 0.0013(7) -0.0036(8) 0.0019(7) C19 0.0275(11) 0.0192(9) 0.0165(9) -0.0021(7) -0.0017(7) 0.0068(8) Cl1 0.0473(4) 0.0240(3) 0.0257(3) -0.0075(2) 0.0028(3) 0.0101(3) C20 0.0240(10) 0.0226(9) 0.0158(8) -0.0018(7) 0.0028(7) 0.0067(8) O1W 0.0381(12) 0.0559(15) 0.0535(15) 0.0054(12) 0.0242(11) 0.0159(11) O2W 0.0250(8) 0.0207(7) 0.0336(10) -0.0022(6) 0.0027(7) 0.0049(6) O3W 0.0643(19) 0.0634(19) 0.101(3) 0.0094(18) 0.0531(19) 0.0262(16) Cl2 0.1036(12) 0.1120(12) 0.0887(10) 0.0341(9) 0.0418(9) 0.0570(10) 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 N2 88.55(7) . . O2 Pt1 O1 177.47(6) . . N2 Pt1 O1 90.41(8) . . O2 Pt1 N1 88.82(7) . . N2 Pt1 N1 164.73(8) . . O1 Pt1 N1 92.78(7) . . O2 Pt1 C1 88.82(9) . . N2 Pt1 C1 95.62(10) . . O1 Pt1 C1 88.99(9) . . N1 Pt1 C1 99.37(10) . . O2 Pt1 N3 90.40(7) . . N2 Pt1 N3 81.84(8) . . O1 Pt1 N3 91.73(7) . . N1 Pt1 N3 83.13(7) . . C1 Pt1 N3 177.36(8) . . C16 O1 Pt1 116.33(13) . . Pt1 O2 H2H 115.4 . . C2 N1 C6 120.19(19) . . C2 N1 Pt1 127.32(17) . . C6 N1 Pt1 112.38(14) . . C13 N2 C9 120.3(2) . . C13 N2 Pt1 127.12(18) . . C9 N2 Pt1 112.58(14) . . C7 N3 C8 114.48(17) . . C7 N3 C14 111.87(16) . . C8 N3 C14 108.98(16) . . C7 N3 Pt1 105.27(13) . . C8 N3 Pt1 103.80(13) . . C14 N3 Pt1 112.16(13) . . 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 120.4(2) . . N1 C2 H2 119.8 . . C3 C2 H2 119.8 . . C4 C3 C2 120.1(2) . . C4 C3 H3 120.0 . . C2 C3 H3 120.0 . . C3 C4 C5 119.3(2) . . C3 C4 H4 120.3 . . C5 C4 H4 120.3 . . C4 C5 C6 119.4(2) . . C4 C5 H5 120.3 . . C6 C5 H5 120.3 . . N1 C6 C5 120.6(2) . . N1 C6 C7 118.14(18) . . C5 C6 C7 121.2(2) . . N3 C7 C6 110.85(17) . . N3 C7 H7A 109.5 . . C6 C7 H7A 109.5 . . N3 C7 H7B 109.5 . . C6 C7 H7B 109.5 . . H7A C7 H7B 108.1 . . N3 C8 C9 108.94(18) . . N3 C8 H8A 109.9 . . C9 C8 H8A 109.9 . . N3 C8 H8B 109.9 . . C9 C8 H8B 109.9 . . H8A C8 H8B 108.3 . . N2 C9 C10 120.8(2) . . N2 C9 C8 117.50(19) . . C10 C9 C8 121.7(2) . . C9 C10 C11 119.0(3) . . C9 C10 H10 120.5 . . C11 C10 H10 120.5 . . C12 C11 C10 119.5(2) . . C12 C11 H11 120.3 . . C10 C11 H11 120.3 . . C13 C12 C11 119.3(3) . . C13 C12 H12 120.3 . . C11 C12 H12 120.3 . . N2 C13 C12 121.1(3) . . N2 C13 H13 119.5 . . C12 C13 H13 119.5 . . C15 C14 N3 113.45(17) . . C15 C14 H14A 108.9 . . N3 C14 H14A 108.9 . . C15 C14 H14B 108.9 . . N3 C14 H14B 108.9 . . H14A C14 H14B 107.7 . . C20 C15 C16 119.5(2) . . C20 C15 C14 121.0(2) . . C16 C15 C14 119.37(18) . . O1 C16 C15 120.80(19) . . O1 C16 C17 118.9(2) . . C15 C16 C17 120.28(19) . . C18 C17 C16 119.7(2) . . C18 C17 H17 120.2 . . C16 C17 H17 120.2 . . C19 C18 C17 119.3(2) . . C19 C18 H18 120.3 . . C17 C18 H18 120.3 . . C20 C19 C18 121.5(2) . . C20 C19 Cl1 119.43(19) . . C18 C19 Cl1 119.11(18) . . C19 C20 C15 119.8(2) . . C19 C20 H20 120.1 . . C15 C20 H20 120.1 . . H1WA O1W H1WB 110.1 . . H2WA O2W H2WB 95.0 . . H3WA O3W H3WB 91.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pt1 O2 2.0004(17) . Pt1 N2 2.0186(19) . Pt1 O1 2.0210(17) . Pt1 N1 2.0337(18) . Pt1 C1 2.042(2) . Pt1 N3 2.1320(18) . O1 C16 1.359(3) . O2 H2H 0.8400 . N1 C2 1.352(3) . N1 C6 1.356(3) . N2 C13 1.346(3) . N2 C9 1.357(3) . N3 C7 1.486(3) . N3 C8 1.492(3) . N3 C14 1.503(3) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C2 C3 1.388(4) . C2 H2 0.9500 . C3 C4 1.369(4) . C3 H3 0.9500 . C4 C5 1.385(4) . C4 H4 0.9500 . C5 C6 1.388(3) . C5 H5 0.9500 . C6 C7 1.515(3) . C7 H7A 0.9900 . C7 H7B 0.9900 . C8 C9 1.513(3) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 C10 1.389(3) . C10 C11 1.389(4) . C10 H10 0.9500 . C11 C12 1.386(5) . C11 H11 0.9500 . C12 C13 1.383(4) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C15 1.498(3) . C14 H14A 0.9900 . C14 H14B 0.9900 . C15 C20 1.394(3) . C15 C16 1.398(3) . C16 C17 1.399(3) . C17 C18 1.395(3) . C17 H17 0.9500 . C18 C19 1.388(4) . C18 H18 0.9500 . C19 C20 1.377(3) . C19 Cl1 1.743(2) . C20 H20 0.9500 . O1W H1WA 0.8400 . O1W H1WB 0.8400 . O2W H2WA 0.8400 . O2W H2WB 0.8400 . O3W H3WA 0.8401 . O3W H3WB 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 O2 H2H Cl2 0.84 2.18 3.011(2) 171.3 2_777 C5 H5 Cl2 0.95 2.99 3.645(3) 127.3 1_545 C8 H8B O2W 0.99 2.59 3.539(3) 161.5 . C13 H13 O3W 0.95 2.46 3.075(4) 122.4 1_455 O1W H1WA O1 0.84 1.99 2.822(3) 171.4 . O1W H1WB O3W 0.84 1.89 2.734(4) 179.7 1_455 O2W H2WA O2 0.84 1.94 2.773(2) 170.4 2_777 O2W H2WB O2 0.84 1.85 2.678(3) 170.0 . O3W H3WB O2W 0.84 1.93 2.701(3) 151.7 . 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 -1.2(3) . . . . Pt1 N1 C2 C3 174.65(18) . . . . N1 C2 C3 C4 1.0(4) . . . . C2 C3 C4 C5 -0.5(4) . . . . C3 C4 C5 C6 0.2(4) . . . . C2 N1 C6 C5 1.0(3) . . . . Pt1 N1 C6 C5 -175.45(17) . . . . C2 N1 C6 C7 -177.05(19) . . . . Pt1 N1 C6 C7 6.5(2) . . . . C4 C5 C6 N1 -0.5(3) . . . . C4 C5 C6 C7 177.5(2) . . . . C8 N3 C7 C6 146.96(18) . . . . C14 N3 C7 C6 -88.4(2) . . . . Pt1 N3 C7 C6 33.63(19) . . . . N1 C6 C7 N3 -28.7(3) . . . . C5 C6 C7 N3 153.3(2) . . . . C7 N3 C8 C9 -154.46(18) . . . . C14 N3 C8 C9 79.4(2) . . . . Pt1 N3 C8 C9 -40.26(19) . . . . C13 N2 C9 C10 1.4(3) . . . . Pt1 N2 C9 C10 -179.67(18) . . . . C13 N2 C9 C8 178.8(2) . . . . Pt1 N2 C9 C8 -2.3(2) . . . . N3 C8 C9 N2 30.6(3) . . . . N3 C8 C9 C10 -152.0(2) . . . . N2 C9 C10 C11 0.6(4) . . . . C8 C9 C10 C11 -176.7(2) . . . . C9 C10 C11 C12 -1.8(4) . . . . C10 C11 C12 C13 1.1(4) . . . . C9 N2 C13 C12 -2.2(4) . . . . Pt1 N2 C13 C12 179.08(18) . . . . C11 C12 C13 N2 0.9(4) . . . . C7 N3 C14 C15 66.1(2) . . . . C8 N3 C14 C15 -166.27(18) . . . . Pt1 N3 C14 C15 -51.9(2) . . . . N3 C14 C15 C20 -121.5(2) . . . . N3 C14 C15 C16 63.2(3) . . . . Pt1 O1 C16 C15 -51.9(2) . . . . Pt1 O1 C16 C17 130.03(17) . . . . C20 C15 C16 O1 -179.9(2) . . . . C14 C15 C16 O1 -4.6(3) . . . . C20 C15 C16 C17 -1.9(3) . . . . C14 C15 C16 C17 173.43(19) . . . . O1 C16 C17 C18 178.8(2) . . . . C15 C16 C17 C18 0.8(3) . . . . C16 C17 C18 C19 0.4(3) . . . . C17 C18 C19 C20 -0.4(3) . . . . C17 C18 C19 Cl1 179.41(17) . . . . C18 C19 C20 C15 -0.7(3) . . . . Cl1 C19 C20 C15 179.45(17) . . . . C16 C15 C20 C19 1.9(3) . . . . C14 C15 C20 C19 -173.4(2) . . . .