# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Gabriele Wagner' 'Jannine Arbour' 'Benjamin Rohrmoser' 'Julien Sarju' 'James Sayer' 'W Scherer' _publ_contact_author_name 'Gabriele Wagner' _publ_contact_author_email G.WAGNER@SURREY.AC.UK _publ_section_title ; Synthesis and Characterisation of Mixed Ligand Pt(II) and Pt(IV) Oxadiazoline Complexes. ; # Attachment 'GW_Ptexchange_Xray.cif' data_ptbr2 _database_code_depnum_ccdc_archive 'CCDC 686813' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 Br2 N4 O2 Pt' _chemical_formula_structural ? _chemical_formula_sum 'C30 H28 Br2 N4 O2 Pt' _chemical_formula_iupac ? _chemical_formula_weight 831.44 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' C C 0.0033 0.0016 '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_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 11.5694(9) _cell_length_b 7.9671(9) _cell_length_c 16.1920(12) _cell_angle_alpha 90 _cell_angle_beta 96.953(6) _cell_angle_gamma 90 _cell_volume 1481.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_reflns_used 19481 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 27.1 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 7.466 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; A multi-scan absorption correction was performed using 'Sortav' R. H. Blessing Acta Crystallogr. 1995, A51, 33-37. ; _exptl_absorpt_correction_T_min 0.20 _exptl_absorpt_correction_T_max 0.43 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed X-ray tube,12x0.4mmlong-finefocus' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10019 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.3 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.84 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3018 # number of observed reflections (> n sig(I)) _reflns_number_gt 2487 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area, (STOE&Cie, 2006)' _computing_cell_refinement 'X-Area, (STOE&Cie, 2006)' _computing_data_reduction 'SORTAV, (Blessing 1995)' _computing_structure_solution 'SIR92 (Altomare (1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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 sigma _refine_ls_weighting_details ; 'w=1/sigma^2(Fo)^2 + (0.0277*P)^2 where P=(Max(Fo^2,0) + 2*Fc^2)/3' ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr # H-atoms refinements were employing riding restains, the U(iso) of the # individual H atoms were related to their respective parents atoms # U(iso) sp2 = 1.2 x U(iso) parent carbon atom # U(iso) sp3 = 1.5 x U(iso) parent carbon atom _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3018 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.004 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.097 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 1.00000 0.00000 0.00000 1.000 0.0370(1) . . Br1 Br Uani 0.94257(4) -0.24411(5) 0.07581(3) 1.000 0.0587(1) . . O1 O Uani 0.6557(2) 0.1687(3) -0.0085(2) 1.000 0.0559(9) . . N1 N Uani 0.8432(2) 0.1063(3) 0.0044(2) 1.000 0.0409(9) . . N2 N Uani 0.7139(3) 0.3158(4) 0.0337(3) 1.000 0.0563(13) . . C1 C Uani 0.7417(3) 0.0664(5) -0.0282(3) 1.000 0.0448(13) . . C2 C Uani 0.7018(3) -0.0700(5) -0.0868(3) 1.000 0.0457(13) . . C3 C Uani 0.5873(4) -0.1274(5) -0.0904(3) 1.000 0.0604(16) . . C4 C Uani 0.5442(4) -0.2420(6) -0.1488(4) 1.000 0.0695(16) . . C5 C Uani 0.6119(5) -0.3003(6) -0.2055(4) 1.000 0.0719(17) . . C6 C Uani 0.7261(5) -0.2481(7) -0.2025(3) 1.000 0.0751(17) . . C7 C Uani 0.7719(4) -0.1318(6) -0.1426(3) 1.000 0.0608(16) . . C8 C Uani 0.8341(3) 0.2578(5) 0.0568(3) 1.000 0.0468(10) . . C9 C Uani 0.8594(3) 0.2193(4) 0.1483(3) 1.000 0.0456(11) . . C10 C Uani 0.9470(4) 0.3089(5) 0.1961(3) 1.000 0.0627(14) . . C11 C Uani 0.9659(5) 0.2821(7) 0.2810(4) 1.000 0.081(2) . . C12 C Uani 0.8996(6) 0.1687(8) 0.3190(4) 1.000 0.083(2) . . C13 C Uani 0.8145(5) 0.0811(7) 0.2719(4) 1.000 0.081(2) . . C14 C Uani 0.7950(4) 0.1049(6) 0.1870(3) 1.000 0.0649(17) . . C15 C Uani 0.7088(6) 0.4432(7) -0.0338(4) 1.000 0.087(2) . . H3 H Uiso 0.53980 -0.08700 -0.05240 1.000 0.0720 calc R H4 H Uiso 0.46810 -0.28020 -0.14990 1.000 0.0830 calc R H5 H Uiso 0.58130 -0.37550 -0.24640 1.000 0.0860 calc R H6 H Uiso 0.77290 -0.29060 -0.24040 1.000 0.0900 calc R H7 H Uiso 0.84880 -0.09650 -0.14060 1.000 0.0730 calc R H8 H Uiso 0.88840 0.34380 0.04180 1.000 0.0560 calc R H10 H Uiso 0.99220 0.38580 0.17110 1.000 0.0750 calc R H11 H Uiso 1.02420 0.34160 0.31300 1.000 0.0970 calc R H12 H Uiso 0.91280 0.15210 0.37620 1.000 0.0990 calc R H13 H Uiso 0.76920 0.00470 0.29720 1.000 0.0970 calc R H14 H Uiso 0.73750 0.04280 0.15560 1.000 0.0780 calc R H15A H Uiso 0.62980 0.47920 -0.04820 1.000 0.1310 calc R H15B H Uiso 0.73730 0.39480 -0.08170 1.000 0.1310 calc R H15C H Uiso 0.75620 0.53790 -0.01500 1.000 0.1310 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 0.0337(1) 0.0371(1) 0.0393(1) 0.0008(1) 0.0001(1) -0.0034(1) Br1 0.0600(2) 0.0496(2) 0.0675(3) 0.0151(2) 0.0114(2) -0.0062(2) O1 0.0394(14) 0.0486(13) 0.078(2) -0.0070(14) -0.0003(14) 0.0026(11) N1 0.0357(14) 0.0422(14) 0.0445(19) -0.0012(12) 0.0033(13) 0.0001(11) N2 0.0515(19) 0.0463(16) 0.068(3) -0.0064(15) -0.0055(17) 0.0066(14) C1 0.0399(18) 0.0440(16) 0.050(3) 0.0046(16) 0.0035(17) 0.0001(14) C2 0.0417(19) 0.0418(16) 0.051(3) 0.0037(16) -0.0047(17) -0.0013(14) C3 0.041(2) 0.053(2) 0.087(4) -0.006(2) 0.007(2) -0.0009(16) C4 0.049(2) 0.056(2) 0.099(4) -0.007(3) -0.009(2) -0.010(2) C5 0.074(3) 0.067(3) 0.068(3) -0.010(2) -0.019(3) -0.012(2) C6 0.075(3) 0.094(3) 0.056(3) -0.018(3) 0.007(2) -0.011(3) C7 0.052(2) 0.076(3) 0.054(3) -0.005(2) 0.005(2) -0.012(2) C8 0.0407(17) 0.0415(16) 0.057(2) -0.0004(17) 0.0017(16) -0.0011(15) C9 0.0447(18) 0.0433(18) 0.049(2) -0.0048(15) 0.0067(16) 0.0050(14) C10 0.059(2) 0.057(2) 0.069(3) -0.008(2) -0.005(2) -0.0064(18) C11 0.082(3) 0.086(4) 0.069(4) -0.023(3) -0.017(3) 0.005(3) C12 0.096(4) 0.097(4) 0.054(3) 0.008(3) 0.004(3) 0.022(3) C13 0.089(4) 0.081(3) 0.074(4) 0.021(3) 0.019(3) -0.001(3) C14 0.066(3) 0.064(3) 0.064(3) 0.002(2) 0.005(2) -0.014(2) C15 0.093(4) 0.055(2) 0.104(5) 0.019(3) -0.030(4) 0.002(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Br1 2.4348(5) . . yes Pt1 N1 2.011(2) . . yes Pt1 Br1 2.4348(5) . 3_755 yes Pt1 N1 2.011(2) . 3_755 yes O1 N2 1.477(4) . . yes O1 C1 1.354(4) . . yes N1 C1 1.268(5) . . yes N1 C8 1.486(5) . . yes N2 C8 1.470(5) . . yes N2 C15 1.488(7) . . yes C1 C2 1.479(6) . . no C2 C3 1.396(6) . . no C2 C7 1.376(6) . . no C3 C4 1.365(7) . . no C4 C5 1.359(8) . . no C5 C6 1.380(8) . . no C6 C7 1.398(7) . . no C8 C9 1.507(7) . . no C9 C10 1.395(6) . . no C9 C14 1.375(6) . . no C10 C11 1.382(8) . . no C11 C12 1.378(9) . . no C12 C13 1.363(9) . . no C13 C14 1.379(8) . . no C3 H3 0.9300 . . no C4 H4 0.9300 . . no C5 H5 0.9300 . . no C6 H6 0.9300 . . no C7 H7 0.9300 . . no C8 H8 0.9800 . . no C10 H10 0.9300 . . no C11 H11 0.9300 . . no C12 H12 0.9300 . . no C13 H13 0.9300 . . no C14 H14 0.9300 . . no C15 H15A 0.9600 . . no C15 H15B 0.9600 . . no C15 H15C 0.9600 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Pt1 N1 90.93(8) . . . yes Br1 Pt1 Br1 180.00 . . 3_755 yes Br1 Pt1 N1 89.08(8) . . 3_755 yes Br1 Pt1 N1 89.08(8) 3_755 . . yes N1 Pt1 N1 180.00 . . 3_755 yes Br1 Pt1 N1 90.93(8) 3_755 . 3_755 yes N2 O1 C1 106.3(3) . . . yes Pt1 N1 C1 132.3(3) . . . yes Pt1 N1 C8 119.3(2) . . . yes C1 N1 C8 108.4(3) . . . yes O1 N2 C8 103.4(3) . . . yes O1 N2 C15 103.1(4) . . . yes C8 N2 C15 110.7(4) . . . yes O1 C1 N1 114.9(4) . . . yes O1 C1 C2 114.3(3) . . . yes N1 C1 C2 130.7(3) . . . yes C1 C2 C3 119.2(4) . . . no C1 C2 C7 121.4(4) . . . no C3 C2 C7 119.2(4) . . . no C2 C3 C4 120.9(4) . . . no C3 C4 C5 120.3(5) . . . no C4 C5 C6 120.1(5) . . . no C5 C6 C7 120.3(5) . . . no C2 C7 C6 119.2(4) . . . no N1 C8 N2 103.9(3) . . . yes N1 C8 C9 112.2(3) . . . yes N2 C8 C9 112.3(3) . . . yes C8 C9 C10 118.9(3) . . . no C8 C9 C14 122.1(4) . . . no C10 C9 C14 118.9(4) . . . no C9 C10 C11 119.3(4) . . . no C10 C11 C12 121.1(5) . . . no C11 C12 C13 119.3(6) . . . no C12 C13 C14 120.5(5) . . . no C9 C14 C13 120.9(5) . . . no C2 C3 H3 120.00 . . . no C4 C3 H3 120.00 . . . no C3 C4 H4 120.00 . . . no C5 C4 H4 120.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C2 C7 H7 120.00 . . . no C6 C7 H7 120.00 . . . no N1 C8 H8 110.00 . . . no N2 C8 H8 109.00 . . . no C9 C8 H8 109.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 119.00 . . . no C11 C12 H12 120.00 . . . no C13 C12 H12 120.00 . . . no C12 C13 H13 120.00 . . . no C14 C13 H13 120.00 . . . no C9 C14 H14 120.00 . . . no C13 C14 H14 119.00 . . . no N2 C15 H15A 110.00 . . . no N2 C15 H15B 109.00 . . . no N2 C15 H15C 109.00 . . . no H15A C15 H15B 110.00 . . . no H15A C15 H15C 109.00 . . . no H15B C15 H15C 109.00 . . . no 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 _geom_torsion_publ_flag Br1 Pt1 N1 C1 -66.3(4) . . . . no Br1 Pt1 N1 C8 110.9(3) . . . . no Br1 Pt1 N1 C1 113.7(4) 3_755 . . . no Br1 Pt1 N1 C8 -69.2(3) 3_755 . . . no N2 O1 C1 N1 10.5(5) . . . . no N2 O1 C1 C2 -167.4(4) . . . . no C1 O1 N2 C8 -16.8(4) . . . . no C1 O1 N2 C15 98.6(4) . . . . no Pt1 N1 C1 O1 178.2(3) . . . . no C8 N1 C1 C2 178.2(4) . . . . no Pt1 N1 C8 N2 170.6(2) . . . . no Pt1 N1 C8 C9 -67.9(3) . . . . no C1 N1 C8 N2 -11.6(4) . . . . no C1 N1 C8 C9 109.9(4) . . . . no Pt1 N1 C1 C2 -4.4(7) . . . . no C8 N1 C1 O1 0.8(5) . . . . no O1 N2 C8 N1 16.7(4) . . . . no O1 N2 C8 C9 -104.7(4) . . . . no C15 N2 C8 N1 -93.1(4) . . . . no C15 N2 C8 C9 145.5(4) . . . . no O1 C1 C2 C3 -25.9(6) . . . . no O1 C1 C2 C7 148.6(4) . . . . no N1 C1 C2 C3 156.6(5) . . . . no N1 C1 C2 C7 -28.9(7) . . . . no C1 C2 C3 C4 174.0(4) . . . . no C7 C2 C3 C4 -0.7(7) . . . . no C1 C2 C7 C6 -173.3(4) . . . . no C3 C2 C7 C6 1.2(7) . . . . no C2 C3 C4 C5 -1.1(8) . . . . no C3 C4 C5 C6 2.2(8) . . . . no C4 C5 C6 C7 -1.7(8) . . . . no C5 C6 C7 C2 -0.1(8) . . . . no N1 C8 C9 C10 124.0(4) . . . . no N1 C8 C9 C14 -59.4(5) . . . . no N2 C8 C9 C10 -119.5(4) . . . . no N2 C8 C9 C14 57.1(5) . . . . no C8 C9 C10 C11 175.9(4) . . . . no C14 C9 C10 C11 -0.8(6) . . . . no C8 C9 C14 C13 -175.2(4) . . . . no C10 C9 C14 C13 1.4(7) . . . . no C9 C10 C11 C12 -0.1(8) . . . . no C10 C11 C12 C13 0.4(9) . . . . no C11 C12 C13 C14 0.3(9) . . . . no C12 C13 C14 C9 -1.2(8) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt1 C7 3.453(5) . . no Pt1 C10 4.121(5) . . no Pt1 C14 4.151(5) . . no Pt1 C14 4.151(5) . 3_755 no Pt1 C7 3.453(5) . 3_755 no Pt1 C10 4.121(5) . 3_755 no Pt1 H7 2.8100 . . no Pt1 H7 2.8100 . 3_755 no Br1 N1 3.183(3) . . no Br1 C1 3.662(4) . . no Br1 N1 3.133(3) . 3_755 no Br1 C8 3.556(4) . 3_755 no Br1 H15C 3.0100 . 1_545 no Br1 H8 3.0000 . 3_755 no O1 N1 2.211(3) . . no O1 C14 3.412(6) . . no O1 C3 3.416(5) . 3_655 no O1 H3 2.4900 . . no O1 H14 2.8900 . . no O1 H3 2.6600 . 3_655 no N1 Br1 3.183(3) . . no N1 N2 2.328(4) . . no N1 Br1 3.133(3) . 3_755 no N2 N1 2.328(4) . . no N1 H15B 2.8800 . . no N1 H7 2.8600 . . no N1 H14 2.9100 . . no N2 H14 2.9300 . . no C1 C14 3.478(7) . . no C3 O1 3.416(5) . 3_655 no C4 C15 3.539(8) . 1_545 no C5 C15 3.523(9) . 1_545 no C7 Pt1 3.453(5) . . no C10 Pt1 4.121(5) . . no C14 C1 3.478(7) . . no C14 Pt1 4.151(5) . . no C14 O1 3.412(6) . . no C15 C4 3.539(8) . 1_565 no C15 C5 3.523(9) . 1_565 no C1 H15B 2.7500 . . no C1 H14 2.9900 . . no C2 H11 3.0600 . 4_454 no C3 H11 2.8100 . 4_454 no C4 H15A 2.8600 . 1_545 no C5 H15A 3.0800 . 1_545 no C9 H13 2.9100 . 2_655 no C10 H13 2.9600 . 2_655 no H3 O1 2.4900 . . no H3 O1 2.6600 . 3_655 no H3 H3 2.4600 . 3_655 no H7 Pt1 2.8100 . . no H7 N1 2.8600 . . no H8 H10 2.3100 . . no H8 H15B 2.5200 . . no H8 H15C 2.2900 . . no H8 Br1 3.0000 . 3_755 no H10 H8 2.3100 . . no H11 C2 3.0600 . 4_555 no H11 C3 2.8100 . 4_555 no H13 C9 2.9100 . 2_645 no H13 C10 2.9600 . 2_645 no H14 O1 2.8900 . . no H14 N1 2.9100 . . no H14 N2 2.9300 . . no H14 C1 2.9900 . . no H15A C4 2.8600 . 1_565 no H15A C5 3.0800 . 1_565 no H15B N1 2.8800 . . no H15B C1 2.7500 . . no H15B H8 2.5200 . . no H15C Br1 3.0100 . 1_565 no H15C H8 2.2900 . . no # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END # CIF-file generated for ptcl2 (compound 6 in the manuscript) #============================================================================== data_ptcl2 _database_code_depnum_ccdc_archive 'CCDC 686814' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H19 Cl2 N3 O Pt' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C20 H19 Cl2 N3 O Pt' _chemical_formula_iupac ? _chemical_formula_weight 583.36 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 16.4796(10) _cell_length_b 8.9290(6) _cell_length_c 15.4594(10) _cell_angle_alpha 90 _cell_angle_beta 113.062(4) _cell_angle_gamma 90 _cell_volume 2093.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 23750 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.71 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 6.974 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; A multi-scan absorption correction was performed using 'Sortav' R. H. Blessing Acta Crystallogr. 1995, A51, 33-37. ; _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.45 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed X-ray tube,12x0.4mmlong-finefocus' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 13473 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 4222 # number of observed reflections (> n sig(I)) _reflns_number_gt 3504 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area, (STOE&Cie, 2006)' _computing_cell_refinement 'X-Area, (STOE&Cie, 2006)' _computing_data_reduction 'SORTAV, (Blessing 1995)' _computing_structure_solution 'SIR92 (Altomare (1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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 sigma _refine_ls_weighting_details ; 'w=1/sigma^2(Fo)^2 + (0.042*P)^2 where P=(Max(Fo^2,0) + 2*Fc^2)/3' ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr # H-atoms refinements were employing riding restains, the U(iso) of the # individual H atoms were related to their respective parents atoms # U(iso) sp2 = 1.2 x U(iso) parent carbon atom # U(iso) sp3 = 1.5 x U(iso) parent carbon atom _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 4222 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.415 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.116 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 0.17010(1) 0.22220(3) 0.18745(1) 1.000 0.0449(1) . . Cl1 Cl Uani 0.09561(10) 0.09872(19) 0.26555(12) 1.000 0.0618(5) . . Cl2 Cl Uani 0.24478(12) 0.3418(2) 0.10944(13) 1.000 0.0741(6) . . O1 O Uani 0.4191(3) 0.1226(5) 0.3939(3) 1.000 0.0546(14) . . N1 N Uani 0.2849(3) 0.1910(5) 0.2981(3) 1.000 0.0440(14) . . N2 N Uani 0.3971(3) 0.2553(6) 0.4391(4) 1.000 0.0528(17) . . N3 N Uani 0.0551(3) 0.2605(5) 0.0795(3) 1.000 0.0494(14) . . C1 C Uani 0.4248(5) 0.2158(11) 0.5383(5) 1.000 0.086(3) . . C2 C Uani 0.3532(4) 0.1123(6) 0.3088(4) 1.000 0.0458(17) . . C3 C Uani 0.3005(4) 0.2689(7) 0.3889(4) 1.000 0.0475(17) . . C4 C Uani 0.3700(4) 0.0132(6) 0.2424(4) 1.000 0.0488(17) . . C5 C Uani 0.4569(4) -0.0147(8) 0.2538(5) 1.000 0.061(2) . . C6 C Uani 0.4749(5) -0.1087(9) 0.1931(6) 1.000 0.077(3) . . C7 C Uani 0.4081(6) -0.1717(10) 0.1201(6) 1.000 0.079(3) . . C8 C Uani 0.3216(6) -0.1446(9) 0.1059(5) 1.000 0.076(3) . . C9 C Uani 0.3023(5) -0.0539(8) 0.1683(5) 1.000 0.065(2) . . C10 C Uani 0.2723(4) 0.4303(7) 0.3759(4) 1.000 0.0523(19) . . C11 C Uani 0.1874(5) 0.4666(9) 0.3662(5) 1.000 0.071(3) . . C12 C Uani 0.1580(6) 0.6140(13) 0.3478(6) 1.000 0.097(4) . . C13 C Uani 0.2137(9) 0.7222(12) 0.3427(7) 1.000 0.104(4) . . C14 C Uani 0.2981(7) 0.6890(10) 0.3542(7) 1.000 0.091(4) . . C15 C Uani 0.3271(6) 0.5433(9) 0.3707(6) 1.000 0.074(3) . . C16 C Uani -0.0057(4) 0.3505(7) 0.0896(4) 1.000 0.0517(19) . . C17 C Uani -0.0836(4) 0.3851(8) 0.0172(5) 1.000 0.063(2) . . C18 C Uani -0.1027(5) 0.3237(9) -0.0707(5) 1.000 0.072(3) . . C19 C Uani -0.0417(6) 0.2299(10) -0.0824(5) 1.000 0.085(3) . . C20 C Uani 0.0369(5) 0.1990(8) -0.0062(5) 1.000 0.069(2) . . H1A H Uiso 0.48790 0.20870 0.56670 1.000 0.1290 calc R H1B H Uiso 0.39950 0.12110 0.54350 1.000 0.1290 calc R H1C H Uiso 0.40520 0.29150 0.56980 1.000 0.1290 calc R H3 H Uiso 0.27050 0.21540 0.42320 1.000 0.0570 calc R H5 H Uiso 0.50300 0.03050 0.30290 1.000 0.0730 calc R H6 H Uiso 0.53300 -0.12900 0.20220 1.000 0.0920 calc R H7 H Uiso 0.42090 -0.23420 0.07900 1.000 0.0950 calc R H8 H Uiso 0.27620 -0.18680 0.05460 1.000 0.0920 calc R H9 H Uiso 0.24400 -0.03850 0.16040 1.000 0.0770 calc R H11 H Uiso 0.15000 0.39270 0.37190 1.000 0.0860 calc R H12 H Uiso 0.10040 0.63820 0.33900 1.000 0.1160 calc R H13 H Uiso 0.19400 0.82060 0.33130 1.000 0.1250 calc R H14 H Uiso 0.33580 0.76440 0.35090 1.000 0.1090 calc R H15 H Uiso 0.38470 0.52070 0.37840 1.000 0.0890 calc R H16 H Uiso 0.00560 0.39120 0.14850 1.000 0.0630 calc R H17 H Uiso -0.12350 0.44950 0.02710 1.000 0.0750 calc R H18 H Uiso -0.15550 0.34550 -0.12070 1.000 0.0870 calc R H19 H Uiso -0.05280 0.18710 -0.14080 1.000 0.1020 calc R H20 H Uiso 0.07780 0.13480 -0.01440 1.000 0.0830 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 0.0388(1) 0.0525(1) 0.0437(1) 0.0054(1) 0.0166(1) 0.0107(1) Cl1 0.0513(8) 0.0706(10) 0.0643(9) 0.0134(7) 0.0235(7) 0.0005(7) Cl2 0.0574(9) 0.1016(13) 0.0722(10) 0.0321(10) 0.0351(8) 0.0178(9) O1 0.044(2) 0.065(3) 0.053(2) 0.0063(19) 0.0170(19) 0.0121(19) N1 0.036(2) 0.047(3) 0.048(2) 0.0052(18) 0.0155(19) 0.0103(19) N2 0.041(3) 0.063(3) 0.053(3) 0.003(2) 0.017(2) 0.010(2) N3 0.045(2) 0.057(3) 0.044(2) 0.006(2) 0.015(2) 0.012(2) C1 0.063(4) 0.138(8) 0.048(3) 0.015(4) 0.012(3) 0.031(5) C2 0.038(3) 0.047(3) 0.051(3) 0.009(2) 0.016(3) 0.003(2) C3 0.040(3) 0.058(3) 0.044(3) 0.004(2) 0.016(2) 0.005(2) C4 0.045(3) 0.049(3) 0.054(3) 0.010(2) 0.021(3) 0.010(2) C5 0.051(4) 0.066(4) 0.070(4) 0.009(3) 0.029(3) 0.010(3) C6 0.070(5) 0.089(5) 0.089(5) 0.006(4) 0.050(5) 0.022(4) C7 0.099(6) 0.081(5) 0.072(5) 0.004(4) 0.049(5) 0.032(5) C8 0.086(5) 0.074(5) 0.065(4) -0.003(4) 0.025(4) 0.019(4) C9 0.058(4) 0.071(4) 0.063(4) 0.001(3) 0.022(3) 0.017(3) C10 0.049(3) 0.063(4) 0.043(3) -0.001(3) 0.016(3) 0.013(3) C11 0.052(4) 0.082(5) 0.074(4) -0.021(4) 0.018(3) 0.016(3) C12 0.071(5) 0.113(8) 0.083(5) -0.032(5) 0.006(4) 0.042(5) C13 0.126(9) 0.075(5) 0.076(5) 0.008(5) 0.003(6) 0.049(6) C14 0.121(8) 0.066(6) 0.088(6) 0.015(4) 0.044(6) 0.011(5) C15 0.078(5) 0.075(5) 0.080(5) 0.018(4) 0.042(4) 0.015(4) C16 0.047(3) 0.060(4) 0.050(3) 0.008(3) 0.021(3) 0.006(3) C17 0.046(3) 0.071(4) 0.070(4) 0.023(3) 0.021(3) 0.013(3) C18 0.056(4) 0.080(5) 0.064(4) 0.013(4) 0.006(3) -0.001(4) C19 0.087(6) 0.100(6) 0.051(4) -0.006(4) 0.008(4) 0.003(5) C20 0.070(4) 0.077(5) 0.052(3) -0.008(3) 0.015(3) 0.015(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.3111(18) . . yes Pt1 Cl2 2.296(2) . . yes Pt1 N1 2.012(5) . . yes Pt1 N3 2.004(5) . . yes O1 N2 1.491(7) . . yes O1 C2 1.341(7) . . yes N1 C2 1.282(8) . . yes N1 C3 1.496(7) . . yes N2 C1 1.462(9) . . yes N2 C3 1.478(9) . . yes N3 C16 1.340(8) . . yes N3 C20 1.355(8) . . yes C2 C4 1.462(8) . . no C3 C10 1.503(9) . . no C4 C5 1.395(10) . . no C4 C9 1.384(10) . . no C5 C6 1.375(11) . . no C6 C7 1.352(13) . . no C7 C8 1.376(15) . . no C8 C9 1.389(11) . . no C10 C11 1.386(11) . . no C10 C15 1.377(11) . . no C11 C12 1.393(14) . . no C12 C13 1.356(17) . . no C13 C14 1.364(19) . . no C14 C15 1.375(12) . . no C16 C17 1.368(10) . . no C17 C18 1.382(10) . . no C18 C19 1.374(13) . . no C19 C20 1.395(11) . . no C1 H1A 0.9600 . . no C1 H1B 0.9600 . . no C1 H1C 0.9600 . . no C3 H3 0.9800 . . no C5 H5 0.9300 . . no C6 H6 0.9300 . . no C7 H7 0.9300 . . no C8 H8 0.9300 . . no C9 H9 0.9300 . . no C11 H11 0.9300 . . no C12 H12 0.9300 . . no C13 H13 0.9300 . . no C14 H14 0.9300 . . no C15 H15 0.9300 . . no C16 H16 0.9300 . . no C17 H17 0.9300 . . no C18 H18 0.9300 . . no C19 H19 0.9300 . . no C20 H20 0.9300 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pt1 Cl2 179.22(6) . . . yes Cl1 Pt1 N1 90.27(15) . . . yes Cl1 Pt1 N3 89.65(15) . . . yes Cl2 Pt1 N1 89.54(15) . . . yes Cl2 Pt1 N3 90.56(15) . . . yes N1 Pt1 N3 177.83(18) . . . yes N2 O1 C2 105.2(5) . . . yes Pt1 N1 C2 132.2(4) . . . yes Pt1 N1 C3 119.5(4) . . . yes C2 N1 C3 108.3(5) . . . yes O1 N2 C1 105.5(5) . . . yes O1 N2 C3 103.2(5) . . . yes C1 N2 C3 113.6(6) . . . yes Pt1 N3 C16 120.8(4) . . . yes Pt1 N3 C20 121.3(5) . . . yes C16 N3 C20 117.9(5) . . . yes O1 C2 N1 114.9(5) . . . yes O1 C2 C4 115.3(6) . . . yes N1 C2 C4 129.8(5) . . . yes N1 C3 N2 102.0(5) . . . yes N1 C3 C10 112.9(5) . . . yes N2 C3 C10 111.2(5) . . . yes C2 C4 C5 119.1(6) . . . no C2 C4 C9 122.0(7) . . . no C5 C4 C9 118.8(6) . . . no C4 C5 C6 120.5(7) . . . no C5 C6 C7 120.1(8) . . . no C6 C7 C8 120.9(8) . . . no C7 C8 C9 119.8(8) . . . no C4 C9 C8 119.9(8) . . . no C3 C10 C11 119.0(6) . . . no C3 C10 C15 122.3(7) . . . no C11 C10 C15 118.7(7) . . . no C10 C11 C12 119.9(8) . . . no C11 C12 C13 119.7(10) . . . no C12 C13 C14 121.1(10) . . . no C13 C14 C15 119.5(10) . . . no C10 C15 C14 121.1(9) . . . no N3 C16 C17 123.0(6) . . . yes C16 C17 C18 119.6(7) . . . no C17 C18 C19 118.3(7) . . . no C18 C19 C20 119.7(7) . . . no N3 C20 C19 121.5(7) . . . yes N2 C1 H1A 109.00 . . . no N2 C1 H1B 109.00 . . . no N2 C1 H1C 109.00 . . . no H1A C1 H1B 109.00 . . . no H1A C1 H1C 110.00 . . . no H1B C1 H1C 110.00 . . . no N1 C3 H3 110.00 . . . no N2 C3 H3 110.00 . . . no C10 C3 H3 110.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C6 C7 H7 119.00 . . . no C8 C7 H7 120.00 . . . no C7 C8 H8 120.00 . . . no C9 C8 H8 120.00 . . . no C4 C9 H9 120.00 . . . no C8 C9 H9 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C11 C12 H12 120.00 . . . no C13 C12 H12 120.00 . . . no C12 C13 H13 119.00 . . . no C14 C13 H13 120.00 . . . no C13 C14 H14 120.00 . . . no C15 C14 H14 120.00 . . . no C10 C15 H15 120.00 . . . no C14 C15 H15 119.00 . . . no N3 C16 H16 118.00 . . . no C17 C16 H16 119.00 . . . no C16 C17 H17 120.00 . . . no C18 C17 H17 120.00 . . . no C17 C18 H18 121.00 . . . no C19 C18 H18 121.00 . . . no C18 C19 H19 120.00 . . . no C20 C19 H19 120.00 . . . no N3 C20 H20 119.00 . . . no C19 C20 H20 119.00 . . . no 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 _geom_torsion_publ_flag Cl1 Pt1 N1 C2 112.8(5) . . . . no Cl1 Pt1 N1 C3 -67.0(4) . . . . no Cl2 Pt1 N1 C2 -66.4(5) . . . . no Cl2 Pt1 N1 C3 113.7(4) . . . . no Cl1 Pt1 N3 C16 66.3(5) . . . . no Cl1 Pt1 N3 C20 -115.0(5) . . . . no Cl2 Pt1 N3 C16 -114.5(5) . . . . no Cl2 Pt1 N3 C20 64.2(5) . . . . no C2 O1 N2 C1 143.0(6) . . . . no C2 O1 N2 C3 23.5(6) . . . . no N2 O1 C2 N1 -14.1(7) . . . . no N2 O1 C2 C4 165.9(5) . . . . no Pt1 N1 C2 O1 178.5(4) . . . . no Pt1 N1 C2 C4 -1.6(10) . . . . no C3 N1 C2 O1 -1.7(7) . . . . no C3 N1 C2 C4 178.3(6) . . . . no Pt1 N1 C3 N2 -163.5(4) . . . . no Pt1 N1 C3 C10 -44.0(7) . . . . no C2 N1 C3 N2 16.7(6) . . . . no C2 N1 C3 C10 136.1(6) . . . . no O1 N2 C3 N1 -23.5(5) . . . . no O1 N2 C3 C10 -144.2(5) . . . . no C1 N2 C3 N1 -137.2(6) . . . . no C1 N2 C3 C10 102.2(7) . . . . no Pt1 N3 C16 C17 177.2(5) . . . . no C20 N3 C16 C17 -1.5(9) . . . . no Pt1 N3 C20 C19 -177.6(6) . . . . no C16 N3 C20 C19 1.2(10) . . . . no O1 C2 C4 C5 -24.9(8) . . . . no O1 C2 C4 C9 155.2(6) . . . . no N1 C2 C4 C5 155.1(7) . . . . no N1 C2 C4 C9 -24.8(10) . . . . no N1 C3 C10 C11 91.7(7) . . . . no N1 C3 C10 C15 -86.5(8) . . . . no N2 C3 C10 C11 -154.3(6) . . . . no N2 C3 C10 C15 27.5(8) . . . . no C2 C4 C5 C6 179.3(6) . . . . no C9 C4 C5 C6 -0.8(10) . . . . no C2 C4 C9 C8 178.6(6) . . . . no C5 C4 C9 C8 -1.3(10) . . . . no C4 C5 C6 C7 1.8(12) . . . . no C5 C6 C7 C8 -0.8(13) . . . . no C6 C7 C8 C9 -1.4(13) . . . . no C7 C8 C9 C4 2.4(11) . . . . no C3 C10 C11 C12 -175.7(6) . . . . no C15 C10 C11 C12 2.6(10) . . . . no C3 C10 C15 C14 176.8(7) . . . . no C11 C10 C15 C14 -1.4(11) . . . . no C10 C11 C12 C13 -2.3(12) . . . . no C11 C12 C13 C14 0.8(14) . . . . no C12 C13 C14 C15 0.4(15) . . . . no C13 C14 C15 C10 -0.1(14) . . . . no N3 C16 C17 C18 1.2(11) . . . . no C16 C17 C18 C19 -0.5(12) . . . . no C17 C18 C19 C20 0.2(13) . . . . no C18 C19 C20 N3 -0.6(13) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt1 C9 3.379(8) . . no Pt1 C11 3.444(8) . . no Pt1 C15 4.147(9) . . no Pt1 H9 2.7300 . . no Pt1 H11 3.3600 . . no Cl1 N1 3.071(5) . . no Cl1 N3 3.050(5) . . no Cl1 C3 3.507(7) . . no Cl1 C16 3.418(6) . . no Cl2 N3 3.063(6) . . no Cl2 C2 3.546(6) . . no Cl2 C20 3.429(8) . . no Cl2 C17 3.572(7) . 3_565 no Cl2 C1 3.582(9) . 4_554 no Cl2 N1 3.041(5) . . no Cl1 H16 3.1200 . 2_545 no Cl1 H3 3.1400 . . no Cl1 H11 3.0400 . . no Cl1 H13 2.9200 . 1_545 no Cl1 H12 3.0100 . 2_545 no Cl1 H19 3.1100 . 3_555 no Cl2 H17 2.9400 . 3_565 no Cl2 H1B 3.1100 . 4_554 no Cl2 H3 3.1100 . 4_554 no O1 N1 2.212(7) . . no O1 H5 2.4700 . . no O1 H7 2.8100 . 2_655 no N1 Cl1 3.071(5) . . no N1 Cl2 3.041(5) . . no N1 N2 2.311(7) . . no N2 N1 2.311(7) . . no N3 Cl1 3.050(5) . . no N3 Cl2 3.063(6) . . no N1 H9 2.8400 . . no N2 H15 2.5300 . . no C1 C5 3.528(11) . 3_656 no C1 Cl2 3.582(9) . 4_555 no C5 C1 3.528(11) . 3_656 no C9 Pt1 3.379(8) . . no C11 Pt1 3.444(8) . . no C15 Pt1 4.147(9) . . no C16 C17 3.517(10) . 3_565 no C16 C18 3.485(11) . 3_565 no C17 Cl2 3.572(7) . 3_565 no C17 C16 3.517(10) . 3_565 no C18 C16 3.485(11) . 3_565 no C2 H6 3.0200 . 2_655 no C4 H14 2.9700 . 1_545 no C5 H1A 3.0900 . 3_656 no C7 H5 3.0400 . 2_645 no C12 H8 3.0900 . 4_555 no C13 H8 3.0400 . 4_555 no C16 H12 2.9300 . 2_545 no H1A C5 3.0900 . 3_656 no H1B H3 2.3600 . . no H1B Cl2 3.1100 . 4_555 no H1C H3 2.5700 . . no H3 Cl1 3.1400 . . no H3 H1B 2.3600 . . no H3 H1C 2.5700 . . no H3 H11 2.4200 . . no H3 Cl2 3.1100 . 4_555 no H5 O1 2.4700 . . no H5 C7 3.0400 . 2_655 no H6 C2 3.0200 . 2_645 no H6 H15 2.5500 . 2_645 no H7 O1 2.8100 . 2_645 no H8 C12 3.0900 . 4_554 no H8 C13 3.0400 . 4_554 no H9 Pt1 2.7300 . . no H9 N1 2.8400 . . no H11 Pt1 3.3600 . . no H11 Cl1 3.0400 . . no H11 H3 2.4200 . . no H11 H20 2.4900 . 4_555 no H12 Cl1 3.0100 . 2_555 no H12 C16 2.9300 . 2_555 no H13 Cl1 2.9200 . 1_565 no H14 C4 2.9700 . 1_565 no H15 N2 2.5300 . . no H15 H6 2.5500 . 2_655 no H16 Cl1 3.1200 . 2_555 no H17 Cl2 2.9400 . 3_565 no H19 Cl1 3.1100 . 3_555 no H20 H11 2.4900 . 4_554 no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C15 H15 N2 0.9300 2.5300 2.847(10) 100.00 . yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; #===END