# Supplementary Material (ESI) for Photochemical & Photobiological Sciences # This journal is (c) The Royal Society of Chemistry and Owner Societies 2009 data_global _journal_name_full Photochem.Photobiol.Sci. _journal_coden_Cambridge 0171 _publ_contact_author_name 'Ken Sakai' _publ_contact_author_email KSAKAI@CHEM.KYUSHU-UNIV.JP _publ_section_title ; Synthesis, crystal structure, solution and spectroscopic properties, and hydrogen-evolving activity of [K(18-Crown-6)][Pt(II)(2-phenylpyridinato)Cl2] ; loop_ _publ_author_name 'Ken Sakai' 'Masayuki Kobayashi' 'Shigeyuki Masaoka' #====================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #========================================================================= # END of CIF #========================================================================= # Attachment 'compound1_revi.cif' #=================================================================== data_071221ptppycl2 _database_code_depnum_ccdc_archive 'CCDC 712234' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; NONE ; _chemical_name_common NONE _chemical_formula_iupac ? _chemical_formula_moiety 'C23 H34 Cl2 K N O7 Pt, C23 H32 Cl2 K N O6 Pt' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H66 Cl4 K2 N2 O13 Pt2' _chemical_formula_weight 1465.19 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' K K 0.2009 0.2494 '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' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6085(18) _cell_length_b 14.149(2) _cell_length_c 19.981(4) _cell_angle_alpha 110.600(2) _cell_angle_beta 103.178(2) _cell_angle_gamma 92.221(2) _cell_volume 2710.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.04 _cell_special_details ; ? # Insert any comments here. ; _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 5.568 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.716 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART APEX CCD-detector diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26240 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.37 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 9847 _reflns_number_gt 8188 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976) ; #========================================================================= # 8. Refinement Data _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+61.7929P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression not_refined _refine_ls_number_reflns 9847 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1580 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 6.780 _refine_diff_density_min -4.533 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.87754(4) 0.59170(3) 0.23887(3) 0.01941(14) Uani 1 1 d . . . Pt2 Pt 0.39121(4) -0.02632(3) 0.24643(3) 0.01852(14) Uani 1 1 d . . . K1 K 0.5578(3) 0.3898(2) 0.25523(17) 0.0278(6) Uani 1 1 d . . . K2 K 0.0610(3) 0.1476(2) 0.25845(16) 0.0258(6) Uani 1 1 d . . . Cl1 Cl 0.7018(3) 0.4739(2) 0.14929(19) 0.0309(7) Uani 1 1 d . . . Cl2 Cl 0.8072(3) 0.5585(2) 0.33340(19) 0.0289(7) Uani 1 1 d . . . Cl3 Cl 0.2404(3) 0.0239(2) 0.16202(18) 0.0287(7) Uani 1 1 d . . . Cl4 Cl 0.3405(3) 0.1030(2) 0.34736(18) 0.0290(7) Uani 1 1 d . . . O1 O 0.4359(9) 0.5625(7) 0.2907(6) 0.036(2) Uani 1 1 d . . . O2 O 0.3316(9) 0.4131(7) 0.1490(6) 0.034(2) Uani 1 1 d . . . O3A O 0.436(3) 0.2254(15) 0.1253(12) 0.040(7) Uani 0.65(4) 1 d P . . O3B O 0.488(5) 0.245(4) 0.110(2) 0.051(12) Uani 0.35(4) 1 d P . . O4A O 0.6690(17) 0.2023(10) 0.2046(9) 0.030(6) Uani 0.65(4) 1 d P . . O4B O 0.607(3) 0.181(2) 0.2265(18) 0.036(11) Uani 0.35(4) 1 d P . . O5 O 0.6856(10) 0.3215(8) 0.3662(6) 0.044(3) Uani 1 1 d . . . O6 O 0.5337(10) 0.4906(7) 0.4040(6) 0.039(2) Uani 1 1 d . . . O7 O 0.0264(9) 0.3481(6) 0.2596(5) 0.027(2) Uani 1 1 d . . . O8 O 0.0895(9) 0.3207(8) 0.3967(5) 0.034(2) Uani 1 1 d . . . O9 O -0.0089(9) 0.1275(7) 0.3902(5) 0.034(2) Uani 1 1 d . . . O10 O -0.0661(9) -0.0378(7) 0.2571(6) 0.037(2) Uani 1 1 d . . . O11 O -0.1377(10) -0.0035(7) 0.1213(7) 0.045(3) Uani 1 1 d . . . O12 O -0.0311(9) 0.1858(7) 0.1242(5) 0.035(2) Uani 1 1 d . . . O13 O 0.3414(10) 0.2683(9) 0.2682(6) 0.046(3) Uani 1 1 d . . . N1A N 0.9506(10) 0.6273(8) 0.1661(7) 0.023(2) Uani 0.50 1 d P . . N1B N 1.0280(11) 0.6939(9) 0.3079(6) 0.025(2) Uani 0.50 1 d P . . N2A N 0.4363(11) -0.1426(8) 0.1671(6) 0.023(2) Uani 0.50 1 d P . . N2B N 0.5165(11) -0.0807(9) 0.3105(7) 0.025(3) Uani 0.50 1 d P . . C1 C 0.9057(13) 0.5870(10) 0.0912(8) 0.032(3) Uani 1 1 d . . . H1 H 0.8305 0.5373 0.0693 0.039 Uiso 1 1 calc R . . C2 C 0.9671(14) 0.6168(11) 0.0452(8) 0.032(3) Uani 1 1 d . . . H2 H 0.9343 0.5868 -0.0070 0.039 Uiso 1 1 calc R . . C3 C 1.0754(13) 0.6898(11) 0.0763(8) 0.031(3) Uani 1 1 d . . . H3 H 1.1182 0.7105 0.0458 0.037 Uiso 1 1 calc R . . C4 C 1.1201(13) 0.7320(10) 0.1519(8) 0.030(3) Uani 1 1 d . . . H4 H 1.1947 0.7823 0.1738 0.036 Uiso 1 1 calc R . . C5 C 1.0589(12) 0.7027(9) 0.1967(7) 0.024(3) Uani 1 1 d . . . C6 C 1.1016(12) 0.7411(8) 0.2770(7) 0.021(3) Uani 1 1 d . . . C7 C 1.2039(13) 0.8162(9) 0.3193(8) 0.029(3) Uani 1 1 d . . . H7 H 1.2508 0.8487 0.2964 0.035 Uiso 1 1 calc R . . C8 C 1.2390(13) 0.8447(10) 0.3958(8) 0.031(3) Uani 1 1 d . . . H8 H 1.3115 0.8951 0.4253 0.037 Uiso 1 1 calc R . . C9 C 1.1678(14) 0.7992(10) 0.4283(8) 0.032(3) Uani 1 1 d . . . H9 H 1.1887 0.8198 0.4806 0.039 Uiso 1 1 calc R . . C10 C 1.0652(14) 0.7229(9) 0.3844(7) 0.029(3) Uani 1 1 d . . . H10 H 1.0192 0.6896 0.4073 0.035 Uiso 1 1 calc R . . C11A C 1.0280(11) 0.6939(9) 0.3079(6) 0.025(2) Uani 0.50 1 d P . . C11B C 0.9506(10) 0.6273(8) 0.1661(7) 0.023(2) Uani 0.50 1 d P . . C12 C 0.3336(15) 0.5782(11) 0.2387(10) 0.044(4) Uani 1 1 d . . . H12A H 0.3373 0.6515 0.2467 0.053 Uiso 1 1 calc R . . H12B H 0.2483 0.5549 0.2438 0.053 Uiso 1 1 calc R . . C13 C 0.3498(15) 0.5167(11) 0.1613(10) 0.043(4) Uani 1 1 d . . . H13A H 0.2849 0.5315 0.1233 0.052 Uiso 1 1 calc R . . H13B H 0.4382 0.5360 0.1579 0.052 Uiso 1 1 calc R . . C14 C 0.3539(15) 0.3527(12) 0.0793(8) 0.039(3) Uani 1 1 d . . . H14A H 0.4421 0.3753 0.0773 0.047 Uiso 1 1 calc R . . H14B H 0.2891 0.3624 0.0387 0.047 Uiso 1 1 calc R . . C15 C 0.3432(16) 0.2434(11) 0.0689(9) 0.042(4) Uani 1 1 d . . . C16 C 0.4930(15) 0.1350(11) 0.1005(8) 0.036(3) Uani 1 1 d . . . C17 C 0.584(2) 0.1199(15) 0.1620(11) 0.072(6) Uani 1 1 d . . . C18 C 0.745(2) 0.1878(15) 0.2714(9) 0.069(7) Uani 1 1 d . . . C19 C 0.6896(15) 0.2125(12) 0.3373(11) 0.055(5) Uani 1 1 d . . . H19A H 0.6006 0.1755 0.3225 0.066 Uiso 1 1 calc R . . H19B H 0.7449 0.1919 0.3756 0.066 Uiso 1 1 calc R . . C20 C 0.6380(16) 0.3570(13) 0.4310(9) 0.045(4) Uani 1 1 d . . . H20A H 0.6949 0.3413 0.4714 0.054 Uiso 1 1 calc R . . H20B H 0.5485 0.3229 0.4204 0.054 Uiso 1 1 calc R . . C21 C 0.6375(16) 0.4692(12) 0.4536(9) 0.043(4) Uani 1 1 d . . . H21A H 0.6265 0.4981 0.5045 0.052 Uiso 1 1 calc R . . H21B H 0.7219 0.5012 0.4533 0.052 Uiso 1 1 calc R . . C22 C 0.5407(15) 0.5973(10) 0.4174(9) 0.041(4) Uani 1 1 d . . . H22A H 0.6232 0.6216 0.4098 0.049 Uiso 1 1 calc R . . H22B H 0.5384 0.6360 0.4691 0.049 Uiso 1 1 calc R . . C23 C 0.4255(15) 0.6129(10) 0.3642(10) 0.044(4) Uani 1 1 d . . . H23A H 0.3434 0.5851 0.3701 0.053 Uiso 1 1 calc R . . H23B H 0.4239 0.6866 0.3748 0.053 Uiso 1 1 calc R . . C24 C 0.3898(13) -0.1686(10) 0.0916(7) 0.029(3) Uani 1 1 d . . . H24 H 0.3387 -0.1247 0.0736 0.035 Uiso 1 1 calc R . . C25 C 0.4163(15) -0.2573(10) 0.0414(8) 0.037(3) Uani 1 1 d . . . H25 H 0.3797 -0.2757 -0.0102 0.044 Uiso 1 1 calc R . . C26 C 0.4970(14) -0.3189(11) 0.0674(8) 0.035(3) Uani 1 1 d . . . H26 H 0.5166 -0.3795 0.0337 0.042 Uiso 1 1 calc R . . C27 C 0.5488(13) -0.2911(10) 0.1432(8) 0.031(3) Uani 1 1 d . . . H27 H 0.6063 -0.3313 0.1615 0.037 Uiso 1 1 calc R . . C28 C 0.5159(11) -0.2036(9) 0.1922(7) 0.022(3) Uani 1 1 d . . . C29 C 0.5617(12) -0.1710(8) 0.2702(7) 0.023(3) Uani 1 1 d . . . C30 C 0.6391(13) -0.2217(11) 0.3100(8) 0.033(3) Uani 1 1 d . . . H30 H 0.6642 -0.2853 0.2839 0.040 Uiso 1 1 calc R . . C31 C 0.6787(13) -0.1817(10) 0.3846(8) 0.032(3) Uani 1 1 d . . . H31 H 0.7340 -0.2159 0.4104 0.039 Uiso 1 1 calc R . . C32 C 0.6388(15) -0.0908(12) 0.4240(9) 0.042(4) Uani 1 1 d . . . H32 H 0.6672 -0.0633 0.4766 0.051 Uiso 1 1 calc R . . C33 C 0.5579(13) -0.0399(10) 0.3872(7) 0.029(3) Uani 1 1 d . . . H33 H 0.5312 0.0224 0.4143 0.035 Uiso 1 1 calc R . . C34A C 0.5165(11) -0.0807(9) 0.3105(7) 0.025(3) Uani 0.50 1 d P . . C34B C 0.4363(11) -0.1426(8) 0.1671(6) 0.023(2) Uani 0.50 1 d P . . C35 C 0.0960(13) 0.4229(10) 0.3258(8) 0.032(3) Uani 1 1 d . . . H35A H 0.0825 0.4908 0.3238 0.038 Uiso 1 1 calc R . . H35B H 0.1904 0.4169 0.3326 0.038 Uiso 1 1 calc R . . C36 C 0.0543(15) 0.4144(11) 0.3907(8) 0.037(3) Uani 1 1 d . . . H36A H 0.0987 0.4724 0.4366 0.044 Uiso 1 1 calc R . . H36B H -0.0412 0.4148 0.3829 0.044 Uiso 1 1 calc R . . C37 C 0.0515(14) 0.3060(12) 0.4564(7) 0.037(3) Uani 1 1 d . . . H37A H -0.0428 0.3109 0.4511 0.045 Uiso 1 1 calc R . . H37B H 0.1009 0.3589 0.5039 0.045 Uiso 1 1 calc R . . C38 C 0.0804(14) 0.2011(13) 0.4548(8) 0.040(4) Uani 1 1 d . . . H38A H 0.1716 0.1925 0.4525 0.049 Uiso 1 1 calc R . . H38B H 0.0682 0.1922 0.5000 0.049 Uiso 1 1 calc R . . C39 C 0.0076(17) 0.0287(12) 0.3875(10) 0.047(4) Uani 1 1 d . . . H39A H -0.0035 0.0215 0.4334 0.057 Uiso 1 1 calc R . . H39B H 0.0964 0.0141 0.3828 0.057 Uiso 1 1 calc R . . C40 C -0.0935(15) -0.0444(11) 0.3214(10) 0.044(4) Uani 1 1 d . . . H40A H -0.0900 -0.1148 0.3204 0.053 Uiso 1 1 calc R . . H40B H -0.1819 -0.0264 0.3241 0.053 Uiso 1 1 calc R . . C41 C -0.1531(15) -0.1073(11) 0.1904(10) 0.049(5) Uani 1 1 d . . . H41A H -0.2435 -0.0909 0.1879 0.059 Uiso 1 1 calc R . . H41B H -0.1511 -0.1778 0.1892 0.059 Uiso 1 1 calc R . . C42 C -0.1098(16) -0.0982(10) 0.1257(10) 0.046(4) Uani 1 1 d . . . H42A H -0.0150 -0.1023 0.1328 0.055 Uiso 1 1 calc R . . H42B H -0.1569 -0.1544 0.0793 0.055 Uiso 1 1 calc R . . C43 C -0.1023(17) 0.0092(11) 0.0609(9) 0.047(4) Uani 1 1 d . . . H43A H -0.1561 -0.0426 0.0140 0.056 Uiso 1 1 calc R . . H43B H -0.0095 -0.0003 0.0639 0.056 Uiso 1 1 calc R . . C44 C -0.1228(15) 0.1132(11) 0.0618(8) 0.041(4) Uani 1 1 d . . . H44A H -0.1106 0.1192 0.0157 0.049 Uiso 1 1 calc R . . H44B H -0.2128 0.1259 0.0648 0.049 Uiso 1 1 calc R . . C45 C -0.0480(16) 0.2888(11) 0.1303(8) 0.040(4) Uani 1 1 d . . . H45A H -0.1381 0.3015 0.1332 0.048 Uiso 1 1 calc R . . H45B H -0.0332 0.2998 0.0863 0.048 Uiso 1 1 calc R . . C46 C 0.0480(14) 0.3597(10) 0.1987(8) 0.032(3) Uani 1 1 d . . . H46A H 0.1377 0.3460 0.1956 0.038 Uiso 1 1 calc R . . H46B H 0.0405 0.4309 0.2025 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0160(2) 0.0158(2) 0.0290(3) 0.0095(2) 0.00851(19) 0.00380(17) Pt2 0.0142(2) 0.0181(2) 0.0254(3) 0.0103(2) 0.00563(18) 0.00233(17) K1 0.0238(14) 0.0192(13) 0.0396(16) 0.0112(12) 0.0057(12) 0.0057(11) K2 0.0209(14) 0.0244(14) 0.0367(16) 0.0137(12) 0.0116(12) 0.0078(11) Cl1 0.0224(16) 0.0256(16) 0.0422(19) 0.0101(14) 0.0082(14) -0.0013(12) Cl2 0.0230(16) 0.0288(16) 0.0409(18) 0.0184(14) 0.0115(14) 0.0025(13) Cl3 0.0220(15) 0.0307(16) 0.0364(18) 0.0157(14) 0.0075(13) 0.0073(13) Cl4 0.0233(16) 0.0270(16) 0.0364(18) 0.0101(14) 0.0091(13) 0.0074(13) O1 0.027(5) 0.022(5) 0.057(7) 0.009(5) 0.014(5) 0.013(4) O2 0.033(5) 0.030(5) 0.050(6) 0.024(5) 0.019(5) 0.011(4) O3A 0.056(15) 0.027(10) 0.022(10) -0.002(7) -0.006(9) 0.023(9) O3B 0.06(3) 0.08(3) 0.016(17) 0.013(17) 0.012(16) 0.00(2) O4A 0.028(10) 0.024(8) 0.045(10) 0.024(7) 0.005(7) 0.000(6) O4B 0.034(19) 0.038(18) 0.06(2) 0.027(16) 0.029(16) 0.016(14) O5 0.031(6) 0.039(6) 0.055(7) 0.011(5) 0.005(5) 0.010(5) O6 0.035(6) 0.028(5) 0.048(6) 0.009(5) 0.010(5) -0.001(4) O7 0.035(5) 0.016(4) 0.029(5) 0.011(4) 0.004(4) 0.002(4) O8 0.034(5) 0.043(6) 0.031(5) 0.015(4) 0.013(4) 0.017(4) O9 0.032(5) 0.039(6) 0.045(6) 0.027(5) 0.015(5) 0.018(4) O10 0.026(5) 0.027(5) 0.058(7) 0.018(5) 0.009(5) 0.000(4) O11 0.035(6) 0.025(5) 0.063(8) 0.009(5) -0.001(5) 0.008(4) O12 0.039(6) 0.031(5) 0.033(5) 0.014(4) 0.004(4) 0.016(4) O13 0.034(6) 0.054(7) 0.051(7) 0.018(6) 0.011(5) 0.016(5) N1A 0.017(6) 0.018(5) 0.036(7) 0.010(5) 0.009(5) 0.007(4) N1B 0.023(6) 0.024(6) 0.030(6) 0.009(5) 0.011(5) 0.011(5) N2A 0.020(6) 0.020(6) 0.032(6) 0.013(5) 0.011(5) 0.003(4) N2B 0.016(6) 0.028(6) 0.037(7) 0.020(5) 0.007(5) -0.003(5) C1 0.028(7) 0.025(7) 0.044(9) 0.010(6) 0.014(6) 0.002(6) C2 0.035(8) 0.037(8) 0.031(7) 0.018(6) 0.011(6) 0.007(6) C3 0.031(7) 0.039(8) 0.037(8) 0.026(7) 0.016(6) 0.007(6) C4 0.025(7) 0.030(7) 0.049(9) 0.026(7) 0.017(6) 0.010(6) C5 0.021(6) 0.025(6) 0.034(7) 0.017(6) 0.012(5) 0.011(5) C6 0.023(6) 0.008(5) 0.036(7) 0.009(5) 0.013(5) 0.009(5) C7 0.025(7) 0.018(6) 0.044(8) 0.010(6) 0.011(6) 0.001(5) C8 0.025(7) 0.020(6) 0.042(8) 0.002(6) 0.016(6) -0.004(5) C9 0.042(8) 0.028(7) 0.024(7) 0.005(6) 0.010(6) 0.008(6) C10 0.041(8) 0.016(6) 0.029(7) 0.002(5) 0.018(6) 0.000(5) C11A 0.023(6) 0.024(6) 0.030(6) 0.009(5) 0.011(5) 0.011(5) C11B 0.017(6) 0.018(5) 0.036(7) 0.010(5) 0.009(5) 0.007(4) C12 0.035(8) 0.027(8) 0.082(12) 0.031(8) 0.020(8) 0.009(6) C13 0.029(8) 0.029(8) 0.078(12) 0.028(8) 0.011(8) 0.007(6) C14 0.039(9) 0.053(9) 0.027(7) 0.019(7) 0.007(6) 0.005(7) C15 0.044(9) 0.029(8) 0.044(9) 0.008(7) 0.005(7) 0.006(7) C16 0.042(9) 0.031(8) 0.029(7) 0.004(6) 0.010(6) 0.008(6) C17 0.089(16) 0.044(11) 0.055(12) -0.001(9) -0.009(11) 0.027(11) C18 0.088(14) 0.070(13) 0.034(9) 0.006(9) 0.000(9) 0.067(12) C19 0.024(8) 0.042(9) 0.089(14) 0.028(9) -0.013(8) 0.006(7) C20 0.035(9) 0.058(10) 0.053(10) 0.031(9) 0.017(7) 0.005(7) C21 0.043(9) 0.051(10) 0.038(9) 0.016(8) 0.016(7) 0.003(7) C22 0.045(9) 0.019(7) 0.054(10) 0.004(7) 0.021(8) 0.003(6) C23 0.034(8) 0.018(7) 0.079(12) 0.005(7) 0.030(8) 0.006(6) C24 0.033(7) 0.033(7) 0.029(7) 0.015(6) 0.016(6) 0.009(6) C25 0.048(9) 0.026(7) 0.040(8) 0.011(6) 0.019(7) 0.001(6) C26 0.043(9) 0.029(7) 0.036(8) 0.009(6) 0.019(7) 0.006(6) C27 0.029(7) 0.022(7) 0.058(9) 0.024(7) 0.026(7) 0.012(5) C28 0.016(6) 0.021(6) 0.038(7) 0.020(6) 0.012(5) 0.002(5) C29 0.021(6) 0.011(5) 0.029(7) 0.003(5) -0.003(5) 0.009(5) C30 0.026(7) 0.032(7) 0.043(9) 0.016(7) 0.009(6) 0.011(6) C31 0.028(7) 0.033(8) 0.040(8) 0.021(7) 0.004(6) 0.008(6) C32 0.043(9) 0.041(9) 0.037(8) 0.016(7) -0.003(7) -0.003(7) C33 0.026(7) 0.026(7) 0.029(7) 0.010(6) -0.001(6) -0.007(5) C34A 0.016(6) 0.028(6) 0.037(7) 0.020(5) 0.007(5) -0.003(5) C34B 0.020(6) 0.020(6) 0.032(6) 0.013(5) 0.011(5) 0.003(4) C35 0.024(7) 0.024(7) 0.045(8) 0.014(6) 0.003(6) 0.004(5) C36 0.040(8) 0.034(8) 0.029(7) 0.006(6) 0.002(6) 0.019(7) C37 0.030(8) 0.056(9) 0.021(7) 0.008(7) 0.007(6) 0.001(7) C38 0.030(8) 0.067(11) 0.037(8) 0.029(8) 0.015(7) 0.024(8) C39 0.065(11) 0.045(9) 0.069(11) 0.046(9) 0.043(9) 0.041(9) C40 0.039(9) 0.025(7) 0.085(13) 0.025(8) 0.039(9) 0.011(6) C41 0.027(8) 0.021(7) 0.088(13) 0.020(8) -0.003(8) 0.008(6) C42 0.038(9) 0.018(7) 0.060(11) -0.001(7) -0.007(8) 0.009(6) C43 0.048(10) 0.031(8) 0.036(9) -0.002(7) -0.014(7) 0.012(7) C44 0.044(9) 0.037(8) 0.028(8) 0.006(6) -0.006(7) 0.006(7) C45 0.059(10) 0.032(8) 0.038(8) 0.018(7) 0.017(7) 0.020(7) C46 0.033(8) 0.019(6) 0.049(9) 0.013(6) 0.020(7) 0.006(5) #========================================================================= # 10. Molecular Geometry 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 N1B 1.989(12) . ? Pt1 N1A 1.993(11) . ? Pt1 Cl2 2.363(3) . ? Pt1 Cl1 2.365(3) . ? Pt2 N2B 1.999(11) . ? Pt2 N2A 2.005(11) . ? Pt2 Cl3 2.369(3) . ? Pt2 Cl4 2.383(3) . ? K1 O1 2.755(9) . ? K1 O3A 2.794(18) . ? K1 O3B 2.81(4) . ? K1 O5 2.817(11) . ? K1 O6 2.885(11) . ? K1 O4A 2.890(15) . ? K1 O4B 2.90(3) . ? K1 O13 2.927(12) . ? K1 O2 2.932(10) . ? K1 Cl2 3.185(4) . ? K1 Cl1 3.368(4) . ? K1 C13 3.522(15) . ? K2 O7 2.868(9) . ? K2 O12 2.883(10) . ? K2 O10 2.890(10) . ? K2 O8 2.920(10) . ? K2 O9 2.993(10) . ? K2 O11 3.068(11) . ? K2 Cl3 3.155(4) . ? K2 Cl4 3.298(4) . ? K2 O13 3.303(11) . ? K2 C18 3.47(2) 1_455 ? O1 C12 1.403(18) . ? O1 C23 1.423(19) . ? O2 C13 1.397(16) . ? O2 C14 1.433(17) . ? O3A O3B 0.78(4) . ? O3A C16 1.41(2) . ? O3A C15 1.42(2) . ? O4A O4B 0.96(3) . ? O4A C17 1.33(2) . ? O4A C18 1.48(2) . ? O5 C20 1.429(19) . ? O5 C19 1.450(19) . ? O6 C21 1.423(18) . ? O6 C22 1.432(16) . ? O7 C46 1.351(16) . ? O7 C35 1.388(16) . ? O8 C37 1.418(16) . ? O8 C36 1.428(16) . ? O9 C39 1.400(16) . ? O9 C38 1.438(19) . ? O10 C40 1.414(19) . ? O10 C41 1.429(18) . ? O11 C43 1.41(2) . ? O11 C42 1.411(17) . ? O12 C44 1.423(17) . ? O12 C45 1.440(16) . ? N1A C1 1.358(18) . ? N1A C5 1.399(17) . ? N1B C6 1.381(16) . ? N2A C28 1.371(16) . ? N2A C24 1.383(17) . ? N2B C29 1.417(16) . ? C1 C2 1.404(19) . ? C1 H1 0.9500 . ? C2 C3 1.38(2) . ? C2 H2 0.9500 . ? C3 C4 1.37(2) . ? C3 H3 0.9500 . ? C4 C5 1.379(18) . ? C4 H4 0.9500 . ? C5 C6 1.452(18) . ? C6 C7 1.372(17) . ? C7 C8 1.39(2) . ? C7 H7 0.9500 . ? C8 C9 1.375(19) . ? C8 H8 0.9500 . ? C9 C10 1.388(19) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C13 1.54(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.48(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 C17 1.46(2) . ? C18 C19 1.50(3) . ? C18 K2 3.47(2) 1_655 ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.49(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.51(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.389(19) . ? C24 H24 0.9500 . ? C25 C26 1.39(2) . ? C25 H25 0.9500 . ? C26 C27 1.39(2) . ? C26 H26 0.9500 . ? C27 C28 1.396(18) . ? C27 H27 0.9500 . ? C28 C29 1.417(18) . ? C29 C30 1.404(17) . ? C30 C31 1.35(2) . ? C30 H30 0.9500 . ? C31 C32 1.39(2) . ? C31 H31 0.9500 . ? C32 C33 1.39(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C35 C36 1.50(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.52(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.51(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.51(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.49(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.49(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? 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 N1B Pt1 N1A 80.3(5) . . ? N1B Pt1 Cl2 94.6(3) . . ? N1A Pt1 Cl2 174.9(3) . . ? N1B Pt1 Cl1 175.5(3) . . ? N1A Pt1 Cl1 95.3(3) . . ? Cl2 Pt1 Cl1 89.79(12) . . ? N2B Pt2 N2A 81.0(5) . . ? N2B Pt2 Cl3 175.0(4) . . ? N2A Pt2 Cl3 94.2(3) . . ? N2B Pt2 Cl4 94.6(4) . . ? N2A Pt2 Cl4 174.9(3) . . ? Cl3 Pt2 Cl4 90.02(11) . . ? O1 K1 O3A 117.8(4) . . ? O1 K1 O3B 120.0(10) . . ? O3A K1 O3B 16.0(7) . . ? O1 K1 O5 120.6(3) . . ? O3A K1 O5 110.8(5) . . ? O3B K1 O5 116.3(10) . . ? O1 K1 O6 59.6(3) . . ? O3A K1 O6 140.2(7) . . ? O3B K1 O6 156.2(11) . . ? O5 K1 O6 61.4(3) . . ? O1 K1 O4A 174.7(4) . . ? O3A K1 O4A 57.0(5) . . ? O3B K1 O4A 54.7(10) . . ? O5 K1 O4A 64.2(4) . . ? O6 K1 O4A 124.8(4) . . ? O1 K1 O4B 160.5(8) . . ? O3A K1 O4B 55.8(7) . . ? O3B K1 O4B 59.8(12) . . ? O5 K1 O4B 56.6(7) . . ? O6 K1 O4B 111.9(7) . . ? O4A K1 O4B 19.1(6) . . ? O1 K1 O13 91.9(3) . . ? O3A K1 O13 65.7(7) . . ? O3B K1 O13 81.7(11) . . ? O5 K1 O13 78.5(3) . . ? O6 K1 O13 74.6(3) . . ? O4A K1 O13 86.8(4) . . ? O4B K1 O13 68.6(8) . . ? O1 K1 O2 59.1(3) . . ? O3A K1 O2 59.5(4) . . ? O3B K1 O2 61.4(10) . . ? O5 K1 O2 155.2(3) . . ? O6 K1 O2 109.8(3) . . ? O4A K1 O2 115.6(4) . . ? O4B K1 O2 114.3(7) . . ? O13 K1 O2 76.7(3) . . ? O1 K1 Cl2 80.3(2) . . ? O3A K1 Cl2 143.8(7) . . ? O3B K1 Cl2 128.0(11) . . ? O5 K1 Cl2 79.9(2) . . ? O6 K1 Cl2 75.7(2) . . ? O4A K1 Cl2 103.4(3) . . ? O4B K1 Cl2 115.9(7) . . ? O13 K1 Cl2 149.1(2) . . ? O2 K1 Cl2 122.0(2) . . ? O1 K1 Cl1 90.0(2) . . ? O3A K1 Cl1 86.5(7) . . ? O3B K1 Cl1 70.9(11) . . ? O5 K1 Cl1 125.8(2) . . ? O6 K1 Cl1 131.2(2) . . ? O4A K1 Cl1 88.5(4) . . ? O4B K1 Cl1 107.0(7) . . ? O13 K1 Cl1 149.4(2) . . ? O2 K1 Cl1 78.2(2) . . ? Cl2 K1 Cl1 61.17(10) . . ? O1 K1 C13 42.3(4) . . ? O3A K1 C13 80.2(5) . . ? O3B K1 C13 78.4(10) . . ? O5 K1 C13 161.6(4) . . ? O6 K1 C13 100.6(4) . . ? O4A K1 C13 132.6(4) . . ? O4B K1 C13 135.9(7) . . ? O13 K1 C13 93.6(3) . . ? O2 K1 C13 22.7(3) . . ? Cl2 K1 C13 100.1(3) . . ? Cl1 K1 C13 68.0(3) . . ? O7 K2 O12 57.8(3) . . ? O7 K2 O10 144.9(3) . . ? O12 K2 O10 114.1(3) . . ? O7 K2 O8 58.7(3) . . ? O12 K2 O8 116.1(3) . . ? O10 K2 O8 113.2(3) . . ? O7 K2 O9 109.0(3) . . ? O12 K2 O9 145.6(3) . . ? O10 K2 O9 56.2(3) . . ? O8 K2 O9 57.3(3) . . ? O7 K2 O11 107.3(3) . . ? O12 K2 O11 57.0(3) . . ? O10 K2 O11 57.3(3) . . ? O8 K2 O11 144.1(3) . . ? O9 K2 O11 106.6(3) . . ? O7 K2 Cl3 117.5(2) . . ? O12 K2 Cl3 79.2(2) . . ? O10 K2 Cl3 91.3(2) . . ? O8 K2 Cl3 138.5(2) . . ? O9 K2 Cl3 129.9(2) . . ? O11 K2 Cl3 77.2(2) . . ? O7 K2 Cl4 120.5(2) . . ? O12 K2 Cl4 135.8(2) . . ? O10 K2 Cl4 89.6(2) . . ? O8 K2 Cl4 83.6(2) . . ? O9 K2 Cl4 78.58(19) . . ? O11 K2 Cl4 127.4(2) . . ? Cl3 K2 Cl4 62.73(9) . . ? O7 K2 O13 69.9(3) . . ? O12 K2 O13 84.4(3) . . ? O10 K2 O13 145.1(3) . . ? O8 K2 O13 80.4(3) . . ? O9 K2 O13 123.2(3) . . ? O11 K2 O13 128.6(3) . . ? Cl3 K2 O13 62.1(2) . . ? Cl4 K2 O13 59.1(2) . . ? O7 K2 C18 72.5(4) . 1_455 ? O12 K2 C18 81.5(4) . 1_455 ? O10 K2 C18 72.6(4) . 1_455 ? O8 K2 C18 74.4(4) . 1_455 ? O9 K2 C18 64.1(4) . 1_455 ? O11 K2 C18 69.8(4) . 1_455 ? Cl3 K2 C18 146.9(3) . 1_455 ? Cl4 K2 C18 142.6(3) . 1_455 ? O13 K2 C18 141.8(4) . 1_455 ? Pt1 Cl1 K1 101.78(12) . . ? Pt1 Cl2 K1 107.24(13) . . ? Pt2 Cl3 K2 103.35(12) . . ? Pt2 Cl4 K2 99.01(12) . . ? C12 O1 C23 111.6(11) . . ? C12 O1 K1 121.6(8) . . ? C23 O1 K1 120.4(8) . . ? C13 O2 C14 110.9(11) . . ? C13 O2 K1 103.1(8) . . ? C14 O2 K1 102.4(8) . . ? O3B O3A C16 81(4) . . ? O3B O3A C15 85(4) . . ? C16 O3A C15 114.6(15) . . ? O3B O3A K1 83(4) . . ? C16 O3A K1 122.2(12) . . ? C15 O3A K1 119.0(11) . . ? O3A O3B K1 80(4) . . ? O4B O4A C17 63(2) . . ? O4B O4A C18 73(2) . . ? C17 O4A C18 110.2(16) . . ? O4B O4A K1 81(2) . . ? C17 O4A K1 115.6(13) . . ? C18 O4A K1 107.0(10) . . ? O4A O4B K1 80(2) . . ? C20 O5 C19 114.2(13) . . ? C20 O5 K1 112.8(8) . . ? C19 O5 K1 111.7(9) . . ? C21 O6 C22 111.7(11) . . ? C21 O6 K1 108.5(8) . . ? C22 O6 K1 106.8(8) . . ? C46 O7 C35 114.2(10) . . ? C46 O7 K2 111.9(7) . . ? C35 O7 K2 111.7(7) . . ? C37 O8 C36 110.9(11) . . ? C37 O8 K2 119.7(8) . . ? C36 O8 K2 116.8(7) . . ? C39 O9 C38 110.3(12) . . ? C39 O9 K2 107.6(8) . . ? C38 O9 K2 107.0(8) . . ? C40 O10 C41 112.8(12) . . ? C40 O10 K2 121.7(8) . . ? C41 O10 K2 120.0(9) . . ? C43 O11 C42 111.2(12) . . ? C43 O11 K2 104.7(8) . . ? C42 O11 K2 102.2(8) . . ? C44 O12 C45 112.0(11) . . ? C44 O12 K2 121.1(8) . . ? C45 O12 K2 118.2(8) . . ? K1 O13 K2 168.5(4) . . ? C1 N1A C5 117.7(11) . . ? C1 N1A Pt1 126.9(9) . . ? C5 N1A Pt1 115.3(9) . . ? C6 N1B Pt1 116.9(9) . . ? C28 N2A C24 118.6(11) . . ? C28 N2A Pt2 114.9(9) . . ? C24 N2A Pt2 126.4(9) . . ? C29 N2B Pt2 113.5(9) . . ? N1A C1 C2 121.9(13) . . ? N1A C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.7(13) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 118.8(12) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 121.2(13) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 N1A 120.7(12) . . ? C4 C5 C6 124.9(12) . . ? N1A C5 C6 114.3(11) . . ? C7 C6 N1B 122.2(12) . . ? C7 C6 C5 124.8(12) . . ? N1B C6 C5 113.0(11) . . ? C6 C7 C8 119.9(12) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 119.3(12) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.8(13) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 H10 119.2 . . ? O1 C12 C13 107.5(12) . . ? O1 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? O1 C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? O2 C13 C12 108.8(13) . . ? O2 C13 K1 54.2(7) . . ? C12 C13 K1 83.9(8) . . ? O2 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? K1 C13 H13A 162.7 . . ? O2 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? K1 C13 H13B 75.0 . . ? H13A C13 H13B 108.3 . . ? O2 C14 C15 110.6(12) . . ? O2 C14 K1 54.2(6) . . ? C15 C14 K1 84.6(8) . . ? O2 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? K1 C14 H14A 75.3 . . ? O2 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? K1 C14 H14B 162.5 . . ? H14A C14 H14B 108.1 . . ? O3A C15 C14 111.6(14) . . ? O3A C16 C17 111.4(14) . . ? O4A C17 C16 112.7(17) . . ? O4A C18 C19 118.3(15) . . ? O4A C18 K2 110.6(13) . 1_655 ? C19 C18 K2 129.7(10) . 1_655 ? O5 C19 C18 107.9(15) . . ? O5 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O5 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? O5 C20 C21 108.2(12) . . ? O5 C20 H20A 110.1 . . ? C21 C20 H20A 110.1 . . ? O5 C20 H20B 110.1 . . ? C21 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? O6 C21 C20 110.0(13) . . ? O6 C21 H21A 109.7 . . ? C20 C21 H21A 109.7 . . ? O6 C21 H21B 109.7 . . ? C20 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? O6 C22 C23 108.0(12) . . ? O6 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? O6 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? O1 C23 C22 109.1(11) . . ? O1 C23 H23A 109.9 . . ? C22 C23 H23A 109.9 . . ? O1 C23 H23B 109.9 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? N2A C24 C25 121.5(13) . . ? N2A C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 119.4(14) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 119.4(13) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 119.7(12) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? N2A C28 C27 121.3(12) . . ? N2A C28 C29 115.3(11) . . ? C27 C28 C29 123.4(11) . . ? C30 C29 N2B 118.2(12) . . ? C30 C29 C28 126.7(11) . . ? N2B C29 C28 115.0(10) . . ? C31 C30 C29 121.2(13) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 120.4(13) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 120.5(14) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 H33 120.3 . . ? O7 C35 C36 111.7(11) . . ? O7 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? O7 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? O8 C36 C35 107.4(11) . . ? O8 C36 H36A 110.2 . . ? C35 C36 H36A 110.2 . . ? O8 C36 H36B 110.2 . . ? C35 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? O8 C37 C38 107.9(11) . . ? O8 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O8 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? O9 C38 C37 107.4(11) . . ? O9 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? O9 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? O9 C39 C40 107.9(12) . . ? O9 C39 H39A 110.1 . . ? C40 C39 H39A 110.1 . . ? O9 C39 H39B 110.1 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? O10 C40 C39 107.8(11) . . ? O10 C40 H40A 110.1 . . ? C39 C40 H40A 110.1 . . ? O10 C40 H40B 110.1 . . ? C39 C40 H40B 110.1 . . ? H40A C40 H40B 108.5 . . ? O10 C41 C42 108.2(12) . . ? O10 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O10 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? O11 C42 C41 108.1(13) . . ? O11 C42 H42A 110.1 . . ? C41 C42 H42A 110.1 . . ? O11 C42 H42B 110.1 . . ? C41 C42 H42B 110.1 . . ? H42A C42 H42B 108.4 . . ? O11 C43 C44 109.6(13) . . ? O11 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? O11 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? O12 C44 C43 108.7(11) . . ? O12 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? O12 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? O12 C45 C46 108.4(11) . . ? O12 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? O12 C45 H45B 110.0 . . ? C46 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? O7 C46 C45 110.8(11) . . ? O7 C46 H46A 109.5 . . ? C45 C46 H46A 109.5 . . ? O7 C46 H46B 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) ; #====================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #========================================================================= # END of CIF #========================================================================= # Attachment 'compound10.cif' #=================================================================== data_080105ptppycldmf _database_code_depnum_ccdc_archive 'CCDC 712235' #===================================================================== # 5. Chemical Data _chemical_name_systematic ; NONE ; _chemical_name_common NONE _chemical_formula_iupac ? _chemical_formula_moiety 'C14 H15 Cl N2 O Pt' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H15 Cl N2 O Pt' _chemical_formula_weight 457.82 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' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 8.6659(12) _cell_length_b 8.0222(11) _cell_length_c 39.984(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.551(2) _cell_angle_gamma 90.00 _cell_volume 2778.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 7618 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.89 _cell_special_details ; ? # Insert any comments here. ; _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 10.284 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.735 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; The first 50 frames were rescanned at the end of data collection to evaluate any possible decay phenomenon. Since it was judged to be negligible, no decay correction was applied to the data. ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART APEX CCD-detector diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_interval_count ? _diffrn_standards_number ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14638 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.10 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _reflns_number_total 6068 _reflns_number_gt 5420 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'KENX (Sakai, 2002)' _computing_publication_material ; SHELXL97, TEXSAN (Molecular Structure Corporation, 2001), KENX, and ORTEP (Johnson, 1976) ; #========================================================================= # 8. Refinement Data _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+13.4598P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression not_refined _refine_ls_number_reflns 6068 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 5.974 _refine_diff_density_min -1.998 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.06444(3) 0.33173(3) 0.173463(7) 0.01989(10) Uani 1 1 d . . . Pt2 Pt 0.17169(3) 0.03355(3) 0.071397(7) 0.02294(10) Uani 1 1 d . . . Cl2 Cl 0.2150(2) 0.1281(2) 0.01780(5) 0.0298(4) Uani 1 1 d . . . Cl1 Cl -0.1720(2) 0.4548(2) 0.16252(5) 0.0271(4) Uani 1 1 d . . . O1 O 0.1534(7) 0.4244(7) 0.12710(13) 0.0285(12) Uani 1 1 d . . . O2 O -0.0514(6) 0.1505(7) 0.07042(14) 0.0285(12) Uani 1 1 d . . . N1 N 0.2677(7) 0.2199(7) 0.18394(16) 0.0227(12) Uani 1 1 d . . . N2 N 0.1313(8) 0.5252(8) 0.07514(18) 0.0279(14) Uani 1 1 d . . . N3 N 0.1355(7) -0.0553(7) 0.11739(16) 0.0227(13) Uani 1 1 d . . . N4 N -0.2683(7) 0.2635(9) 0.04720(18) 0.0296(14) Uani 1 1 d . . . C1 C 0.3895(9) 0.2225(10) 0.1641(2) 0.0291(16) Uani 1 1 d . . . H1 H 0.3815 0.2807 0.1435 0.035 Uiso 1 1 calc R . . C2 C 0.5265(10) 0.1436(10) 0.1726(2) 0.0292(17) Uani 1 1 d . . . H2 H 0.6118 0.1489 0.1582 0.035 Uiso 1 1 calc R . . C3 C 0.5378(9) 0.0555(9) 0.2029(2) 0.0293(17) Uani 1 1 d . . . H3 H 0.6298 -0.0023 0.2091 0.035 Uiso 1 1 calc R . . C4 C 0.4122(10) 0.0549(9) 0.2233(2) 0.0279(16) Uani 1 1 d . . . H4 H 0.4184 -0.0009 0.2443 0.033 Uiso 1 1 calc R . . C5 C 0.2766(9) 0.1354(9) 0.21344(19) 0.0250(15) Uani 1 1 d . . . C6 C 0.1327(9) 0.1396(9) 0.23206(19) 0.0250(15) Uani 1 1 d . . . C7 C 0.1132(10) 0.0577(10) 0.26284(19) 0.0274(16) Uani 1 1 d . . . H7 H 0.1966 -0.0010 0.2733 0.033 Uiso 1 1 calc R . . C8 C -0.0289(10) 0.0639(9) 0.2776(2) 0.0292(17) Uani 1 1 d . . . H8 H -0.0445 0.0065 0.2980 0.035 Uiso 1 1 calc R . . C9 C -0.1486(10) 0.1536(10) 0.2627(2) 0.0286(17) Uani 1 1 d . . . H9 H -0.2456 0.1582 0.2732 0.034 Uiso 1 1 calc R . . C10 C -0.1290(9) 0.2364(10) 0.23293(19) 0.0269(16) Uani 1 1 d . . . H10 H -0.2128 0.2982 0.2234 0.032 Uiso 1 1 calc R . . C11 C 0.0114(9) 0.2318(9) 0.21622(17) 0.0221(14) Uani 1 1 d . . . C12 C 0.0743(9) 0.4864(9) 0.10377(19) 0.0250(15) Uani 1 1 d . . . H12 H -0.0323 0.5061 0.1071 0.030 Uiso 1 1 calc R . . C13 C 0.2953(10) 0.5017(12) 0.0678(2) 0.0361(19) Uani 1 1 d . . . H13A H 0.3509 0.4623 0.0879 0.054 Uiso 1 1 calc R . . H13B H 0.3394 0.6080 0.0606 0.054 Uiso 1 1 calc R . . H13C H 0.3049 0.4192 0.0499 0.054 Uiso 1 1 calc R . . C14 C 0.0350(11) 0.5964(12) 0.0477(2) 0.037(2) Uani 1 1 d . . . H14A H -0.0739 0.5917 0.0537 0.056 Uiso 1 1 calc R . . H14B H 0.0500 0.5322 0.0272 0.056 Uiso 1 1 calc R . . H14C H 0.0649 0.7127 0.0440 0.056 Uiso 1 1 calc R . . C15 C 0.0019(10) -0.0446(10) 0.1332(2) 0.0310(18) Uani 1 1 d . . . H15 H -0.0809 0.0158 0.1230 0.037 Uiso 1 1 calc R . . C16 C -0.0200(9) -0.1173(10) 0.1638(2) 0.0319(17) Uani 1 1 d . . . H16 H -0.1166 -0.1076 0.1743 0.038 Uiso 1 1 calc R . . C17 C 0.0976(11) -0.2032(10) 0.1788(2) 0.0313(18) Uani 1 1 d . . . H17 H 0.0833 -0.2556 0.1998 0.038 Uiso 1 1 calc R . . C18 C 0.2395(10) -0.2141(10) 0.1633(2) 0.0312(17) Uani 1 1 d . . . H18 H 0.3235 -0.2711 0.1739 0.037 Uiso 1 1 calc R . . C19 C 0.2563(10) -0.1405(10) 0.1321(2) 0.0279(16) Uani 1 1 d . . . C20 C 0.3927(9) -0.1461(9) 0.1114(2) 0.0267(16) Uani 1 1 d . . . C21 C 0.5313(9) -0.2233(10) 0.1215(2) 0.0288(16) Uani 1 1 d . . . H21 H 0.5413 -0.2727 0.1431 0.035 Uiso 1 1 calc R . . C22 C 0.6540(10) -0.2272(10) 0.0999(2) 0.0324(18) Uani 1 1 d . . . H22 H 0.7490 -0.2770 0.1068 0.039 Uiso 1 1 calc R . . C23 C 0.6379(10) -0.1591(10) 0.0684(2) 0.0311(17) Uani 1 1 d . . . H23 H 0.7214 -0.1646 0.0535 0.037 Uiso 1 1 calc R . . C24 C 0.5004(10) -0.0820(10) 0.0582(2) 0.0298(17) Uani 1 1 d . . . H24 H 0.4916 -0.0350 0.0364 0.036 Uiso 1 1 calc R . . C25 C 0.3750(9) -0.0727(10) 0.0794(2) 0.0275(16) Uani 1 1 d . . . C26 C -0.1340(10) 0.1854(9) 0.0451(2) 0.0278(16) Uani 1 1 d . . . H26 H -0.0990 0.1546 0.0237 0.033 Uiso 1 1 calc R . . C27 C -0.3326(10) 0.3091(11) 0.0795(2) 0.0353(19) Uani 1 1 d . . . H27A H -0.2562 0.2865 0.0974 0.053 Uiso 1 1 calc R . . H27B H -0.4258 0.2432 0.0832 0.053 Uiso 1 1 calc R . . H27C H -0.3587 0.4279 0.0794 0.053 Uiso 1 1 calc R . . C28 C -0.3590(11) 0.3033(11) 0.0171(2) 0.0360(19) Uani 1 1 d . . . H28A H -0.3109 0.2527 -0.0023 0.054 Uiso 1 1 calc R . . H28B H -0.3633 0.4245 0.0142 0.054 Uiso 1 1 calc R . . H28C H -0.4638 0.2595 0.0192 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02317(17) 0.01871(15) 0.01767(15) 0.00033(9) -0.00159(11) -0.00095(10) Pt2 0.02427(17) 0.02124(16) 0.02313(16) -0.00195(10) -0.00275(11) -0.00103(10) Cl1 0.0250(9) 0.0315(9) 0.0249(9) 0.0037(7) -0.0003(7) 0.0037(7) Cl2 0.0295(10) 0.0337(9) 0.0263(9) 0.0008(7) -0.0014(7) 0.0002(8) O1 0.034(3) 0.024(3) 0.028(3) 0.003(2) 0.000(2) 0.000(2) O2 0.023(3) 0.031(3) 0.031(3) 0.000(2) -0.001(2) 0.002(2) N1 0.026(3) 0.017(3) 0.025(3) -0.002(2) -0.001(2) 0.000(2) N2 0.023(3) 0.025(3) 0.036(4) 0.005(3) -0.001(3) -0.006(3) N3 0.022(3) 0.022(3) 0.024(3) -0.006(2) 0.001(2) -0.003(2) N4 0.019(3) 0.030(3) 0.040(4) 0.004(3) -0.002(3) 0.001(3) C1 0.034(4) 0.023(4) 0.029(4) 0.002(3) -0.002(3) -0.004(3) C2 0.028(4) 0.028(4) 0.032(4) -0.002(3) -0.002(3) 0.001(3) C3 0.022(4) 0.023(4) 0.042(5) -0.006(3) -0.008(3) -0.003(3) C4 0.032(4) 0.021(3) 0.030(4) 0.005(3) -0.007(3) -0.003(3) C5 0.032(4) 0.019(3) 0.024(4) 0.002(3) -0.005(3) -0.004(3) C6 0.029(4) 0.019(3) 0.027(4) 0.000(3) -0.007(3) -0.003(3) C7 0.034(4) 0.027(4) 0.020(4) -0.001(3) -0.005(3) -0.006(3) C8 0.044(5) 0.021(3) 0.023(4) 0.002(3) -0.003(3) -0.005(3) C9 0.029(4) 0.032(4) 0.025(4) 0.000(3) 0.005(3) -0.005(3) C10 0.031(4) 0.026(4) 0.024(4) -0.004(3) -0.003(3) -0.004(3) C11 0.031(4) 0.021(3) 0.015(3) -0.004(3) -0.003(3) -0.006(3) C12 0.024(4) 0.027(4) 0.024(4) 0.001(3) 0.001(3) 0.003(3) C13 0.033(5) 0.040(5) 0.036(5) 0.005(4) 0.009(4) -0.005(4) C14 0.046(5) 0.044(5) 0.022(4) 0.011(3) -0.007(4) -0.002(4) C15 0.033(4) 0.025(4) 0.034(4) -0.006(3) -0.002(3) -0.004(3) C16 0.023(4) 0.033(4) 0.040(5) 0.001(4) 0.006(3) -0.002(3) C17 0.045(5) 0.019(3) 0.030(4) -0.006(3) -0.001(4) 0.002(3) C18 0.037(5) 0.027(4) 0.029(4) -0.003(3) -0.004(3) 0.000(3) C19 0.032(4) 0.023(4) 0.028(4) -0.005(3) -0.010(3) 0.000(3) C20 0.028(4) 0.020(3) 0.031(4) -0.005(3) -0.009(3) -0.002(3) C21 0.032(4) 0.024(4) 0.030(4) 0.001(3) -0.009(3) 0.007(3) C22 0.035(5) 0.029(4) 0.033(4) -0.005(3) -0.008(3) 0.005(3) C23 0.031(4) 0.030(4) 0.032(4) -0.003(3) 0.001(3) -0.001(3) C24 0.035(4) 0.027(4) 0.028(4) -0.002(3) -0.002(3) -0.005(3) C25 0.032(4) 0.023(3) 0.027(4) -0.004(3) -0.001(3) 0.000(3) C26 0.030(4) 0.022(4) 0.031(4) 0.001(3) 0.002(3) -0.005(3) C27 0.033(5) 0.039(5) 0.033(4) -0.008(4) -0.002(4) 0.000(4) C28 0.034(5) 0.043(5) 0.031(4) 0.005(4) -0.008(4) 0.006(4) #========================================================================= # 10. Molecular Geometry 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 2.3052(19) . ? Pt1 O1 2.159(5) . ? Pt1 N1 2.011(6) . ? Pt1 C11 1.954(7) . ? Pt2 Cl2 2.3133(19) . ? Pt2 O2 2.149(5) . ? Pt2 N3 2.005(6) . ? Pt2 C25 1.975(8) . ? O1 C12 1.246(9) . ? O2 C26 1.254(10) . ? N1 C1 1.337(10) . ? N1 C5 1.361(10) . ? N2 C12 1.297(10) . ? N2 C13 1.471(11) . ? N2 C14 1.476(10) . ? N3 C15 1.338(10) . ? N3 C19 1.369(10) . ? N4 C26 1.327(10) . ? N4 C27 1.466(11) . ? N4 C28 1.455(11) . ? C1 C2 1.380(12) . ? C1 H1 0.9500 . ? C2 C3 1.401(12) . ? C2 H2 0.9500 . ? C3 C4 1.380(12) . ? C3 H3 0.9500 . ? C4 C5 1.389(11) . ? C4 H4 0.9500 . ? C5 C6 1.470(11) . ? C6 C7 1.410(11) . ? C6 C11 1.420(11) . ? C7 H7 0.9500 . ? C7 C8 1.380(12) . ? C8 H8 0.9500 . ? C8 C9 1.383(12) . ? C9 C10 1.378(11) . ? C9 H9 0.9500 . ? C10 C11 1.404(10) . ? C10 H10 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 0.9500 . ? C15 C16 1.371(12) . ? C16 H16 0.9500 . ? C16 C17 1.357(13) . ? C17 C18 1.395(12) . ? C17 H17 0.9500 . ? C18 C19 1.392(11) . ? C18 H18 0.9500 . ? C19 C20 1.461(12) . ? C20 C21 1.401(11) . ? C20 C25 1.413(11) . ? C21 C22 1.390(12) . ? C21 H21 0.9500 . ? C22 C23 1.374(12) . ? C22 H22 0.9500 . ? C23 C24 1.395(12) . ? C23 H23 0.9500 . ? C24 C25 1.400(11) . ? C24 H24 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 Cl1 Pt1 O1 91.47(15) . . ? Cl1 Pt1 N1 178.35(18) . . ? Cl1 Pt1 C11 96.5(2) . . ? O1 Pt1 N1 90.1(2) . . ? O1 Pt1 C11 172.0(3) . . ? N1 Pt1 C11 82.0(3) . . ? Cl2 Pt2 O2 90.50(16) . . ? Cl2 Pt2 N3 178.28(17) . . ? Cl2 Pt2 C25 97.2(2) . . ? O2 Pt2 N3 90.5(2) . . ? O2 Pt2 C25 171.7(3) . . ? N3 Pt2 C25 81.8(3) . . ? Pt1 O1 C12 125.3(5) . . ? Pt2 O2 C26 127.2(5) . . ? Pt1 N1 C1 124.8(5) . . ? Pt1 N1 C5 115.5(5) . . ? C1 N1 C5 119.6(7) . . ? C12 N2 C13 122.6(7) . . ? C12 N2 C14 121.9(7) . . ? C13 N2 C14 115.5(7) . . ? Pt2 N3 C15 124.8(6) . . ? Pt2 N3 C19 115.8(5) . . ? C15 N3 C19 119.3(7) . . ? C26 N4 C27 121.9(7) . . ? C26 N4 C28 120.5(7) . . ? C27 N4 C28 117.6(7) . . ? N1 C1 C2 122.3(7) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.9(8) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 118.4(7) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 120.3(7) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 120.4(7) . . ? N1 C5 C6 113.5(7) . . ? C4 C5 C6 126.1(7) . . ? C5 C6 C7 123.7(7) . . ? C5 C6 C11 114.5(7) . . ? C7 C6 C11 121.8(7) . . ? C6 C7 C8 119.1(8) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C9 120.1(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 121.0(8) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C11 121.8(8) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? Pt1 C11 C6 114.5(5) . . ? Pt1 C11 C10 129.2(6) . . ? C6 C11 C10 116.2(7) . . ? O1 C12 N2 122.8(7) . . ? O1 C12 H12 118.6 . . ? N2 C12 H12 118.6 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 122.5(8) . . ? N3 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 119.7(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 119.1(8) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? N3 C19 C18 120.0(8) . . ? N3 C19 C20 113.1(7) . . ? C18 C19 C20 126.9(8) . . ? C19 C20 C21 123.4(7) . . ? C19 C20 C25 115.5(7) . . ? C21 C20 C25 121.1(8) . . ? C20 C21 C22 119.7(8) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 120.0(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.7(8) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 121.0(8) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? Pt2 C25 C20 113.7(6) . . ? Pt2 C25 C24 128.9(6) . . ? C20 C25 C24 117.5(7) . . ? O2 C26 N4 122.5(8) . . ? O2 C26 H26 118.8 . . ? N4 C26 H26 118.8 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Mean-plane data from final SHELXL refinement run:- Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) ;