# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Yu-Man Ho.' 'Chi-Kin Koo.' 'Ka-Leung Wong.' 'Kong, Karen' 'Chan, Chris' 'Wai-Ming Kwok.' 'Cheuk-Fai Chow.' 'Lam, Michael' 'Wai-Yeung Wong.' _publ_contact_author_name 'Lam, Michael' _publ_contact_author_email bhmhwlam@cityu.edu.hk _publ_section_title ; The Synthesis and Photophysical Studies of Cyclometalated Pt(II) Complexes with C,N,N-Ligands Containing Imidazolyl Donors ; # Attachment '- [Pt(L2)(PPh3)](ClO4) (3-ClO4).cif' data_wy1851wm _database_code_depnum_ccdc_archive 'CCDC 828775' #TrackingRef '- [Pt(L2)(PPh3)](ClO4) (3-ClO4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H25 Cl N3 O4 P Pt' _chemical_formula_weight 777.06 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4058(5) _cell_length_b 12.5485(7) _cell_length_c 13.1386(7) _cell_angle_alpha 70.9460(10) _cell_angle_beta 73.1280(10) _cell_angle_gamma 79.9880(10) _cell_volume 1397.30(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 5.219 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6620 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8661 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6468 _reflns_number_gt 6261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0304P)^2^+1.1737P] 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_number_reflns 6468 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 C1 C 0.1015(3) 0.5161(2) 0.2688(2) 0.0208(5) Uani 1 1 d . . . C2 C 0.2159(3) 0.4562(2) 0.2084(2) 0.0246(5) Uani 1 1 d . . . H2A H 0.2888 0.4968 0.1479 0.029 Uiso 1 1 calc R . . C3 C 0.2255(3) 0.3381(2) 0.2352(2) 0.0278(6) Uani 1 1 d . . . H3A H 0.3043 0.3004 0.1922 0.033 Uiso 1 1 calc R . . C4 C 0.1231(3) 0.2758(2) 0.3226(2) 0.0280(6) Uani 1 1 d . . . H4A H 0.1317 0.1956 0.3407 0.034 Uiso 1 1 calc R . . C5 C 0.0070(3) 0.3316(2) 0.3838(2) 0.0253(5) Uani 1 1 d . . . H5A H -0.0651 0.2896 0.4439 0.030 Uiso 1 1 calc R . . C6 C -0.0043(3) 0.4495(2) 0.3574(2) 0.0212(5) Uani 1 1 d . . . C7 C -0.1253(3) 0.5114(2) 0.4214(2) 0.0212(5) Uani 1 1 d . . . C8 C -0.2482(3) 0.4701(3) 0.5071(2) 0.0285(6) Uani 1 1 d . . . H8A H -0.2624 0.3917 0.5319 0.034 Uiso 1 1 calc R . . C9 C -0.3492(3) 0.5449(3) 0.5555(2) 0.0324(6) Uani 1 1 d . . . H9A H -0.4333 0.5172 0.6137 0.039 Uiso 1 1 calc R . . C10 C -0.3296(3) 0.6599(3) 0.5204(2) 0.0282(6) Uani 1 1 d . . . H10A H -0.3988 0.7113 0.5535 0.034 Uiso 1 1 calc R . . C11 C -0.2054(3) 0.6964(2) 0.4353(2) 0.0216(5) Uani 1 1 d . . . C12 C -0.1596(3) 0.8110(2) 0.3853(2) 0.0226(5) Uani 1 1 d . . . C13 C -0.1333(4) 0.9906(3) 0.3460(3) 0.0366(7) Uani 1 1 d . . . H13A H -0.1488 1.0669 0.3476 0.044 Uiso 1 1 calc R . . C14 C -0.0209(3) 0.9457(3) 0.2751(3) 0.0328(6) Uani 1 1 d . . . H14A H 0.0558 0.9858 0.2180 0.039 Uiso 1 1 calc R . . C15 C 0.2670(3) 0.8966(2) 0.0683(2) 0.0209(5) Uani 1 1 d . . . C16 C 0.1947(4) 0.9688(3) -0.0111(3) 0.0318(6) Uani 1 1 d . . . H16A H 0.1466 0.9380 -0.0481 0.038 Uiso 1 1 calc R . . C17 C 0.1929(4) 1.0853(3) -0.0364(3) 0.0406(8) Uani 1 1 d . . . H17A H 0.1443 1.1337 -0.0910 0.049 Uiso 1 1 calc R . . C18 C 0.2611(4) 1.1314(3) 0.0174(3) 0.0361(7) Uani 1 1 d . . . H18A H 0.2581 1.2112 0.0008 0.043 Uiso 1 1 calc R . . C19 C 0.3337(3) 1.0611(3) 0.0951(3) 0.0323(6) Uani 1 1 d . . . H19A H 0.3805 1.0927 0.1322 0.039 Uiso 1 1 calc R . . C20 C 0.3389(3) 0.9443(2) 0.1197(2) 0.0269(5) Uani 1 1 d . . . H20A H 0.3919 0.8967 0.1719 0.032 Uiso 1 1 calc R . . C21 C 0.2373(3) 0.7245(2) -0.0176(2) 0.0207(5) Uani 1 1 d . . . C22 C 0.3456(3) 0.7623(3) -0.1165(2) 0.0277(6) Uani 1 1 d . . . H22A H 0.4302 0.7935 -0.1155 0.033 Uiso 1 1 calc R . . C23 C 0.3314(4) 0.7549(3) -0.2155(2) 0.0342(6) Uani 1 1 d . . . H23A H 0.4069 0.7792 -0.2820 0.041 Uiso 1 1 calc R . . C24 C 0.2060(4) 0.7118(3) -0.2173(3) 0.0369(7) Uani 1 1 d . . . H24A H 0.1960 0.7068 -0.2855 0.044 Uiso 1 1 calc R . . C25 C 0.0962(4) 0.6764(3) -0.1212(3) 0.0335(7) Uani 1 1 d . . . H25A H 0.0101 0.6483 -0.1234 0.040 Uiso 1 1 calc R . . C26 C 0.1116(3) 0.6818(2) -0.0202(2) 0.0259(5) Uani 1 1 d . . . H26A H 0.0365 0.6565 0.0464 0.031 Uiso 1 1 calc R . . C27 C 0.4338(3) 0.6787(2) 0.1311(2) 0.0189(4) Uani 1 1 d . . . C28 C 0.4731(3) 0.6873(2) 0.2227(2) 0.0214(5) Uani 1 1 d . . . H28A H 0.4049 0.7249 0.2717 0.026 Uiso 1 1 calc R . . C29 C 0.6117(3) 0.6411(2) 0.2422(2) 0.0265(5) Uani 1 1 d . . . H29A H 0.6398 0.6507 0.3023 0.032 Uiso 1 1 calc R . . C30 C 0.7086(3) 0.5813(2) 0.1748(2) 0.0273(5) Uani 1 1 d . . . H30A H 0.8025 0.5488 0.1891 0.033 Uiso 1 1 calc R . . C31 C 0.6683(3) 0.5687(2) 0.0859(2) 0.0265(5) Uani 1 1 d . . . H31A H 0.7340 0.5261 0.0405 0.032 Uiso 1 1 calc R . . C32 C 0.5325(3) 0.6180(2) 0.0633(2) 0.0225(5) Uani 1 1 d . . . H32A H 0.5066 0.6105 0.0014 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.38690(9) 0.90320(7) 0.41285(6) 0.03533(15) Uani 1 1 d . . . N1 N -0.1087(2) 0.62301(19) 0.38847(18) 0.0197(4) Uani 1 1 d . . . N2 N -0.0379(2) 0.83214(19) 0.30068(19) 0.0237(4) Uani 1 1 d . . . N3 N -0.2190(3) 0.9049(2) 0.4141(2) 0.0305(5) Uani 1 1 d . . . H3B H -0.2993 0.9106 0.4675 0.037 Uiso 1 1 calc R . . O1 O 0.5148(3) 0.8793(3) 0.3309(2) 0.0528(7) Uani 1 1 d . . . O2 O 0.2782(4) 0.8316(4) 0.4290(4) 0.0946(13) Uani 1 1 d . . . O3 O 0.4314(4) 0.8886(3) 0.5131(2) 0.0591(8) Uani 1 1 d . . . O4 O 0.3305(4) 1.0178(3) 0.3756(3) 0.0735(11) Uani 1 1 d . . . P1 P 0.25167(7) 0.74438(5) 0.10960(5) 0.01750(12) Uani 1 1 d . . . Pt1 Pt 0.063716(9) 0.682225(7) 0.258270(7) 0.01737(4) 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 C1 0.0201(11) 0.0207(12) 0.0230(11) -0.0074(10) -0.0070(9) -0.0008(9) C2 0.0239(12) 0.0221(13) 0.0284(13) -0.0114(11) -0.0028(10) -0.0025(10) C3 0.0282(13) 0.0230(13) 0.0356(14) -0.0161(11) -0.0079(11) 0.0035(11) C4 0.0335(14) 0.0175(12) 0.0363(14) -0.0086(11) -0.0141(12) 0.0000(11) C5 0.0279(13) 0.0211(13) 0.0271(13) -0.0043(10) -0.0099(10) -0.0031(10) C6 0.0214(11) 0.0212(12) 0.0233(11) -0.0076(10) -0.0084(9) -0.0007(10) C7 0.0212(11) 0.0206(12) 0.0211(11) -0.0052(9) -0.0063(9) -0.0002(9) C8 0.0284(13) 0.0251(14) 0.0259(13) -0.0013(11) -0.0031(11) -0.0052(11) C9 0.0275(14) 0.0338(16) 0.0256(13) -0.0028(12) 0.0030(11) -0.0043(12) C10 0.0256(13) 0.0298(15) 0.0231(12) -0.0076(11) 0.0001(10) 0.0022(11) C11 0.0207(11) 0.0224(12) 0.0214(11) -0.0079(10) -0.0050(9) 0.0011(10) C12 0.0208(11) 0.0223(12) 0.0241(12) -0.0098(10) -0.0036(9) 0.0024(10) C13 0.0398(17) 0.0211(14) 0.0442(17) -0.0160(13) 0.0015(14) 0.0021(12) C14 0.0315(14) 0.0201(13) 0.0414(16) -0.0130(12) 0.0036(12) -0.0021(11) C15 0.0200(11) 0.0174(11) 0.0228(11) -0.0059(9) -0.0012(9) -0.0024(9) C16 0.0363(15) 0.0248(14) 0.0364(15) -0.0073(12) -0.0169(13) 0.0019(12) C17 0.054(2) 0.0229(15) 0.0433(18) -0.0044(13) -0.0206(16) 0.0053(14) C18 0.0393(16) 0.0165(13) 0.0452(17) -0.0039(12) -0.0039(14) -0.0050(12) C19 0.0325(14) 0.0238(14) 0.0423(16) -0.0121(12) -0.0053(12) -0.0087(12) C20 0.0281(13) 0.0213(13) 0.0325(14) -0.0083(11) -0.0089(11) -0.0019(10) C21 0.0217(11) 0.0190(12) 0.0227(11) -0.0086(9) -0.0072(9) 0.0023(9) C22 0.0258(13) 0.0315(15) 0.0270(13) -0.0121(11) -0.0056(10) -0.0003(11) C23 0.0405(16) 0.0360(16) 0.0252(13) -0.0116(12) -0.0087(12) 0.0045(13) C24 0.0528(19) 0.0324(16) 0.0343(15) -0.0164(13) -0.0243(14) 0.0092(14) C25 0.0400(16) 0.0275(14) 0.0444(17) -0.0145(13) -0.0262(14) 0.0025(12) C26 0.0252(12) 0.0224(13) 0.0331(14) -0.0101(11) -0.0108(11) -0.0003(10) C27 0.0181(11) 0.0164(11) 0.0216(11) -0.0053(9) -0.0043(9) -0.0013(9) C28 0.0250(12) 0.0175(11) 0.0211(11) -0.0057(9) -0.0045(9) -0.0019(10) C29 0.0306(13) 0.0244(13) 0.0274(13) -0.0061(11) -0.0135(11) -0.0017(11) C30 0.0228(12) 0.0222(13) 0.0345(14) -0.0033(11) -0.0108(11) 0.0004(10) C31 0.0238(12) 0.0223(13) 0.0318(13) -0.0109(11) -0.0042(10) 0.0032(10) C32 0.0219(12) 0.0210(12) 0.0261(12) -0.0104(10) -0.0056(10) 0.0006(10) Cl1 0.0366(4) 0.0344(4) 0.0372(4) -0.0193(3) -0.0084(3) 0.0069(3) N1 0.0181(9) 0.0203(10) 0.0212(10) -0.0079(8) -0.0044(8) -0.0005(8) N2 0.0228(10) 0.0189(11) 0.0279(11) -0.0105(9) -0.0013(9) 0.0006(8) N3 0.0291(12) 0.0258(12) 0.0321(12) -0.0144(10) 0.0021(10) 0.0042(10) O1 0.0407(13) 0.079(2) 0.0496(14) -0.0419(15) -0.0099(11) 0.0097(13) O2 0.068(2) 0.092(3) 0.122(3) -0.045(3) 0.012(2) -0.039(2) O3 0.0714(19) 0.070(2) 0.0334(12) -0.0237(13) -0.0164(13) 0.0228(16) O4 0.108(3) 0.0529(18) 0.0607(19) -0.0272(15) -0.0398(19) 0.0429(19) P1 0.0166(3) 0.0162(3) 0.0204(3) -0.0078(2) -0.0033(2) -0.0008(2) Pt1 0.01585(5) 0.01565(5) 0.02041(5) -0.00775(4) -0.00205(4) -0.00037(3) _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. ; 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 C1 C2 1.401(4) . ? C1 C6 1.423(4) . ? C1 Pt1 2.019(3) . ? C2 C3 1.400(4) . ? C2 H2A 0.9500 . ? C3 C4 1.376(4) . ? C3 H3A 0.9500 . ? C4 C5 1.387(4) . ? C4 H4A 0.9500 . ? C5 C6 1.397(4) . ? C5 H5A 0.9500 . ? C6 C7 1.473(4) . ? C7 N1 1.347(3) . ? C7 C8 1.394(4) . ? C8 C9 1.384(4) . ? C8 H8A 0.9500 . ? C9 C10 1.392(4) . ? C9 H9A 0.9500 . ? C10 C11 1.385(4) . ? C10 H10A 0.9500 . ? C11 N1 1.345(3) . ? C11 C12 1.456(4) . ? C12 N3 1.335(4) . ? C12 N2 1.338(3) . ? C13 N3 1.363(4) . ? C13 C14 1.367(4) . ? C13 H13A 0.9500 . ? C14 N2 1.380(4) . ? C14 H14A 0.9500 . ? C15 C20 1.394(4) . ? C15 C16 1.398(4) . ? C15 P1 1.827(3) . ? C16 C17 1.388(4) . ? C16 H16A 0.9500 . ? C17 C18 1.379(5) . ? C17 H17A 0.9500 . ? C18 C19 1.376(4) . ? C18 H18A 0.9500 . ? C19 C20 1.389(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.393(4) . ? C21 C22 1.396(4) . ? C21 P1 1.814(3) . ? C22 C23 1.379(4) . ? C22 H22A 0.9500 . ? C23 C24 1.390(5) . ? C23 H23A 0.9500 . ? C24 C25 1.377(5) . ? C24 H24A 0.9500 . ? C25 C26 1.400(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C32 1.397(4) . ? C27 C28 1.397(3) . ? C27 P1 1.825(2) . ? C28 C29 1.392(4) . ? C28 H28A 0.9500 . ? C29 C30 1.380(4) . ? C29 H29A 0.9500 . ? C30 C31 1.389(4) . ? C30 H30A 0.9500 . ? C31 C32 1.390(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? Cl1 O2 1.402(4) . ? Cl1 O4 1.420(3) . ? Cl1 O1 1.425(3) . ? Cl1 O3 1.442(3) . ? N1 Pt1 2.022(2) . ? N2 Pt1 2.124(2) . ? N3 H3B 0.8800 . ? P1 Pt1 2.2426(6) . ? 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 C2 C1 C6 115.9(2) . . ? C2 C1 Pt1 131.4(2) . . ? C6 C1 Pt1 112.67(18) . . ? C1 C2 C3 121.6(3) . . ? C1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 122.0(2) . . ? C5 C6 C7 121.6(2) . . ? C1 C6 C7 116.4(2) . . ? N1 C7 C8 118.8(2) . . ? N1 C7 C6 112.1(2) . . ? C8 C7 C6 129.1(3) . . ? C9 C8 C7 119.1(3) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 117.5(3) . . ? C11 C10 H10A 121.3 . . ? C9 C10 H10A 121.3 . . ? N1 C11 C10 120.8(3) . . ? N1 C11 C12 111.4(2) . . ? C10 C11 C12 127.9(2) . . ? N3 C12 N2 110.6(2) . . ? N3 C12 C11 129.4(2) . . ? N2 C12 C11 120.0(2) . . ? N3 C13 C14 107.0(3) . . ? N3 C13 H13A 126.5 . . ? C14 C13 H13A 126.5 . . ? C13 C14 N2 108.3(3) . . ? C13 C14 H14A 125.9 . . ? N2 C14 H14A 125.9 . . ? C20 C15 C16 118.5(3) . . ? C20 C15 P1 122.1(2) . . ? C16 C15 P1 119.3(2) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C19 C20 C15 120.4(3) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? C26 C21 C22 119.2(2) . . ? C26 C21 P1 120.5(2) . . ? C22 C21 P1 119.9(2) . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 119.8(3) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C32 C27 C28 118.9(2) . . ? C32 C27 P1 123.52(19) . . ? C28 C27 P1 117.51(19) . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C30 C29 C28 120.4(2) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.8(2) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 120.3(3) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C27 120.3(2) . . ? C31 C32 H32A 119.9 . . ? C27 C32 H32A 119.9 . . ? O2 Cl1 O4 109.7(3) . . ? O2 Cl1 O1 108.5(2) . . ? O4 Cl1 O1 109.6(2) . . ? O2 Cl1 O3 112.7(3) . . ? O4 Cl1 O3 107.72(19) . . ? O1 Cl1 O3 108.61(17) . . ? C11 N1 C7 122.7(2) . . ? C11 N1 Pt1 119.15(18) . . ? C7 N1 Pt1 118.06(17) . . ? C12 N2 C14 106.2(2) . . ? C12 N2 Pt1 111.16(18) . . ? C14 N2 Pt1 142.55(19) . . ? C12 N3 C13 108.0(2) . . ? C12 N3 H3B 126.0 . . ? C13 N3 H3B 126.0 . . ? C21 P1 C15 101.98(12) . . ? C21 P1 C27 107.01(12) . . ? C15 P1 C27 105.09(12) . . ? C21 P1 Pt1 114.52(9) . . ? C15 P1 Pt1 114.44(9) . . ? C27 P1 Pt1 112.77(8) . . ? C1 Pt1 N1 80.64(10) . . ? C1 Pt1 N2 158.77(10) . . ? N1 Pt1 N2 78.21(9) . . ? C1 Pt1 P1 97.94(8) . . ? N1 Pt1 P1 177.56(6) . . ? N2 Pt1 P1 103.26(6) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.939 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.105 # Attachment '- [Pt(L2)Cl] (1).cif' data_wy1853wm _database_code_depnum_ccdc_archive 'CCDC 828776' #TrackingRef '- [Pt(L2)Cl] (1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cl N3 O Pt' _chemical_formula_weight 468.81 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 9.7720(6) _cell_length_b 12.5346(7) _cell_length_c 11.1227(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.4410(10) _cell_angle_gamma 90.00 _cell_volume 1343.94(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 10.637 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.5128 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6192 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2313 _reflns_number_gt 2140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0520P)^2^+0.9140P] 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_number_reflns 2313 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 C1 C 0.0310(5) 0.1958(4) 0.6811(5) 0.0314(10) Uani 1 1 d . . . C2 C -0.0406(6) 0.2857(4) 0.7147(5) 0.0384(12) Uani 1 1 d . . . H2A H -0.1122 0.2769 0.7623 0.046 Uiso 1 1 calc R . . C3 C -0.0064(6) 0.3882(5) 0.6781(6) 0.0462(14) Uani 1 1 d . . . H3A H -0.0583 0.4478 0.6980 0.055 Uiso 1 1 calc R . . C4 C 0.1005(6) 0.4038(4) 0.6140(6) 0.0472(14) Uani 1 1 d . . . H4A H 0.1256 0.4740 0.5939 0.057 Uiso 1 1 calc R . . C5 C 0.1717(5) 0.3166(4) 0.5786(5) 0.0419(12) Uani 1 1 d . . . H5A H 0.2447 0.3264 0.5329 0.050 Uiso 1 1 calc R . . C6 C 0.1350(5) 0.2142(4) 0.6110(5) 0.0331(11) Uani 1 1 d . . . C7 C 0.1992(5) 0.1180(4) 0.5699(4) 0.0316(10) Uani 1 1 d . . . C8 C 0.2966(5) 0.1086(5) 0.4919(5) 0.0408(12) Uani 1 1 d . . . H8A H 0.3348 0.1707 0.4613 0.049 Uiso 1 1 calc R . . C9 C 0.3372(5) 0.0088(6) 0.4594(5) 0.0462(13) Uani 1 1 d . . . H9A H 0.4013 0.0024 0.4042 0.055 Uiso 1 1 calc R . . C10 C 0.2848(5) -0.0831(5) 0.5068(5) 0.0446(13) Uani 1 1 d . . . H10A H 0.3146 -0.1521 0.4870 0.053 Uiso 1 1 calc R . . C11 C 0.1895(5) -0.0702(4) 0.5825(5) 0.0344(11) Uani 1 1 d . . . C12 C 0.1157(5) -0.1533(4) 0.6403(5) 0.0332(11) Uani 1 1 d . . . C13 C 0.0354(7) -0.3020(5) 0.6990(6) 0.0501(14) Uani 1 1 d . . . H13A H 0.0201 -0.3758 0.7106 0.060 Uiso 1 1 calc R . . C14 C -0.0297(6) -0.2195(4) 0.7465(6) 0.0404(12) Uani 1 1 d . . . H14A H -0.0993 -0.2262 0.7965 0.049 Uiso 1 1 calc R . . Cl1 Cl -0.16530(15) 0.06158(11) 0.83675(14) 0.0412(3) Uani 1 1 d . . . N1 N 0.1474(4) 0.0281(3) 0.6130(4) 0.0287(9) Uani 1 1 d . . . N2 N 0.0220(4) -0.1258(4) 0.7102(4) 0.0332(10) Uani 1 1 d . . . N3 N 0.1258(5) -0.2591(3) 0.6322(4) 0.0420(11) Uani 1 1 d . . . H3B H 0.1809 -0.2945 0.5913 0.050 Uiso 1 1 calc R . . Pt1 Pt 0.003697(16) 0.042145(15) 0.715131(16) 0.02679(11) Uani 1 1 d . . . O1 O 0.3267(5) 0.6420(3) 0.5153(4) 0.0583(11) 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 C1 0.031(2) 0.032(3) 0.031(2) 0.000(2) 0.004(2) -0.001(2) C2 0.040(2) 0.032(3) 0.044(3) -0.004(2) 0.011(2) 0.004(2) C3 0.062(4) 0.030(3) 0.045(3) 0.000(3) 0.007(3) 0.004(2) C4 0.062(3) 0.031(3) 0.047(3) 0.008(2) 0.002(3) -0.010(2) C5 0.041(3) 0.043(3) 0.041(3) 0.007(2) 0.007(2) -0.011(2) C6 0.031(2) 0.036(3) 0.031(3) 0.003(2) 0.003(2) 0.000(2) C7 0.025(2) 0.042(3) 0.028(2) 0.004(2) 0.0048(19) -0.007(2) C8 0.031(2) 0.059(3) 0.033(3) 0.002(3) 0.008(2) -0.005(2) C9 0.027(3) 0.076(4) 0.039(3) -0.001(3) 0.014(2) 0.005(3) C10 0.033(3) 0.056(3) 0.045(3) -0.013(3) 0.004(2) 0.012(2) C11 0.032(2) 0.040(3) 0.029(3) -0.003(2) 0.001(2) 0.006(2) C12 0.035(2) 0.034(3) 0.029(2) -0.003(2) 0.001(2) 0.004(2) C13 0.069(4) 0.031(3) 0.047(3) -0.002(3) 0.001(3) -0.005(3) C14 0.054(3) 0.023(3) 0.044(3) -0.001(2) 0.009(3) -0.006(2) Cl1 0.0475(8) 0.0387(6) 0.0433(8) 0.0004(6) 0.0250(6) -0.0027(5) N1 0.024(2) 0.038(2) 0.025(2) -0.0015(17) 0.0079(18) 0.0036(16) N2 0.037(2) 0.031(2) 0.032(2) -0.0002(17) 0.006(2) 0.0008(17) N3 0.052(3) 0.032(2) 0.039(2) -0.006(2) -0.001(2) 0.010(2) Pt1 0.02772(15) 0.02561(16) 0.02860(16) -0.00036(6) 0.00921(10) -0.00080(6) O1 0.075(3) 0.051(2) 0.047(2) -0.0086(19) 0.003(2) 0.031(2) _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. ; 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 C1 C6 1.397(7) . ? C1 C2 1.409(7) . ? C1 Pt1 1.990(5) . ? C2 C3 1.405(8) . ? C2 H2A 0.9500 . ? C3 C4 1.372(9) . ? C3 H3A 0.9500 . ? C4 C5 1.387(8) . ? C4 H4A 0.9500 . ? C5 C6 1.396(7) . ? C5 H5A 0.9500 . ? C6 C7 1.466(7) . ? C7 N1 1.356(6) . ? C7 C8 1.394(7) . ? C8 C9 1.379(9) . ? C8 H8A 0.9500 . ? C9 C10 1.398(9) . ? C9 H9A 0.9500 . ? C10 C11 1.364(8) . ? C10 H10A 0.9500 . ? C11 N1 1.359(7) . ? C11 C12 1.474(8) . ? C12 N3 1.334(6) . ? C12 N2 1.339(7) . ? C13 N3 1.355(9) . ? C13 C14 1.364(9) . ? C13 H13A 0.9500 . ? C14 N2 1.366(7) . ? C14 H14A 0.9500 . ? Cl1 Pt1 2.3129(14) . ? N1 Pt1 1.953(4) . ? N2 Pt1 2.114(5) . ? N3 H3B 0.8800 . ? 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 C6 C1 C2 117.1(5) . . ? C6 C1 Pt1 113.4(4) . . ? C2 C1 Pt1 129.4(4) . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C5 C6 C1 122.4(5) . . ? C5 C6 C7 122.3(5) . . ? C1 C6 C7 115.2(4) . . ? N1 C7 C8 118.8(5) . . ? N1 C7 C6 111.7(4) . . ? C8 C7 C6 129.4(5) . . ? C9 C8 C7 119.7(5) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C10 120.7(5) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 117.6(6) . . ? C11 C10 H10A 121.2 . . ? C9 C10 H10A 121.2 . . ? N1 C11 C10 121.8(5) . . ? N1 C11 C12 110.0(5) . . ? C10 C11 C12 128.1(5) . . ? N3 C12 N2 111.1(5) . . ? N3 C12 C11 128.8(5) . . ? N2 C12 C11 120.0(5) . . ? N3 C13 C14 107.4(5) . . ? N3 C13 H13A 126.3 . . ? C14 C13 H13A 126.3 . . ? C13 C14 N2 108.5(6) . . ? C13 C14 H14A 125.7 . . ? N2 C14 H14A 125.7 . . ? C7 N1 C11 121.3(5) . . ? C7 N1 Pt1 118.4(3) . . ? C11 N1 Pt1 120.2(4) . . ? C12 N2 C14 105.8(5) . . ? C12 N2 Pt1 109.9(4) . . ? C14 N2 Pt1 144.2(4) . . ? C12 N3 C13 107.1(5) . . ? C12 N3 H3B 126.4 . . ? C13 N3 H3B 126.4 . . ? N1 Pt1 C1 81.09(19) . . ? N1 Pt1 N2 79.79(16) . . ? C1 Pt1 N2 160.8(2) . . ? N1 Pt1 Cl1 179.09(12) . . ? C1 Pt1 Cl1 98.07(16) . . ? N2 Pt1 Cl1 101.06(12) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.901 _refine_diff_density_min -1.856 _refine_diff_density_rms 0.171 # Attachment '- [Pt(L3)(PPh3)](ClO4) (4-ClO4).cif' data_wy1929wm _database_code_depnum_ccdc_archive 'CCDC 828777' #TrackingRef '- [Pt(L3)(PPh3)](ClO4) (4-ClO4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H25 Cl N3 O4 P Pt' _chemical_formula_weight 777.06 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1983(4) _cell_length_b 9.5114(4) _cell_length_c 16.4668(7) _cell_angle_alpha 91.5660(10) _cell_angle_beta 92.5240(10) _cell_angle_gamma 92.9470(10) _cell_volume 1436.73(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 5.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5795 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8805 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6595 _reflns_number_gt 6108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0488P)^2^+0.2995P] 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_number_reflns 6595 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.004 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 C1 C 0.6722(4) 1.0217(4) 0.7454(2) 0.0399(7) Uani 1 1 d . . . C2 C 0.6710(5) 1.0744(4) 0.8258(3) 0.0471(9) Uani 1 1 d . . . H2A H 0.6207 1.0236 0.8640 0.057 Uiso 1 1 calc R . . C3 C 0.7450(5) 1.2032(5) 0.8491(3) 0.0580(11) Uani 1 1 d . . . H3A H 0.7423 1.2364 0.9026 0.070 Uiso 1 1 calc R . . C4 C 0.8197(5) 1.2793(5) 0.7955(4) 0.0645(13) Uani 1 1 d . . . H4A H 0.8666 1.3649 0.8121 0.077 Uiso 1 1 calc R . . C5 C 0.8268(5) 1.2304(5) 0.7157(3) 0.0568(11) Uani 1 1 d . . . H5A H 0.8799 1.2821 0.6789 0.068 Uiso 1 1 calc R . . C6 C 0.7535(4) 1.1026(4) 0.6908(3) 0.0451(8) Uani 1 1 d . . . C7 C 0.7499(4) 1.0486(4) 0.6054(3) 0.0490(9) Uani 1 1 d . . . C8 C 0.8267(5) 1.0979(5) 0.5411(3) 0.0630(12) Uani 1 1 d . . . H8A H 0.8946 1.1735 0.5488 0.076 Uiso 1 1 calc R . . C9 C 0.8021(6) 1.0342(6) 0.4654(3) 0.0740(16) Uani 1 1 d . . . H9A H 0.8539 1.0667 0.4218 0.089 Uiso 1 1 calc R . . C10 C 0.7005(6) 0.9217(6) 0.4538(3) 0.0699(14) Uani 1 1 d . . . H10A H 0.6830 0.8794 0.4024 0.084 Uiso 1 1 calc R . . C11 C 0.6258(5) 0.8732(5) 0.5192(2) 0.0501(9) Uani 1 1 d . . . C12 C 0.5165(5) 0.7586(4) 0.5215(2) 0.0485(9) Uani 1 1 d . . . C13 C 0.4424(6) 0.6749(5) 0.4632(3) 0.0604(12) Uani 1 1 d . . . H13A H 0.4553 0.6750 0.4076 0.072 Uiso 1 1 calc R . . C14 C 0.3602(5) 0.6230(4) 0.5830(3) 0.0495(9) Uani 1 1 d . . . H14A H 0.3057 0.5803 0.6227 0.059 Uiso 1 1 calc R . . C15 C 0.6117(4) 0.7264(4) 0.8822(2) 0.0368(7) Uani 1 1 d . . . C16 C 0.5700(5) 0.6731(4) 0.9559(2) 0.0480(9) Uani 1 1 d . . . H16A H 0.4720 0.6657 0.9676 0.058 Uiso 1 1 calc R . . C17 C 0.6752(5) 0.6310(5) 1.0124(3) 0.0588(11) Uani 1 1 d . . . H17A H 0.6473 0.5958 1.0618 0.071 Uiso 1 1 calc R . . C18 C 0.8216(6) 0.6416(6) 0.9949(3) 0.0673(14) Uani 1 1 d . . . H18A H 0.8923 0.6151 1.0328 0.081 Uiso 1 1 calc R . . C19 C 0.8606(5) 0.6916(5) 0.9214(3) 0.0615(11) Uani 1 1 d . . . H19A H 0.9584 0.6953 0.9091 0.074 Uiso 1 1 calc R . . C20 C 0.7588(4) 0.7368(4) 0.8649(2) 0.0442(8) Uani 1 1 d . . . H20A H 0.7881 0.7736 0.8161 0.053 Uiso 1 1 calc R . . C21 C 0.3317(4) 0.8605(4) 0.8444(2) 0.0365(7) Uani 1 1 d . . . C22 C 0.2139(5) 0.8855(4) 0.7910(3) 0.0468(8) Uani 1 1 d . . . H22A H 0.2115 0.8502 0.7377 0.056 Uiso 1 1 calc R . . C23 C 0.1001(5) 0.9634(5) 0.8179(3) 0.0547(10) Uani 1 1 d . . . H23A H 0.0203 0.9778 0.7831 0.066 Uiso 1 1 calc R . . C24 C 0.1062(5) 1.0187(5) 0.8959(3) 0.0596(11) Uani 1 1 d . . . H24A H 0.0311 1.0723 0.9135 0.071 Uiso 1 1 calc R . . C25 C 0.2219(5) 0.9955(5) 0.9478(3) 0.0614(12) Uani 1 1 d . . . H25A H 0.2247 1.0329 1.0007 0.074 Uiso 1 1 calc R . . C26 C 0.3346(5) 0.9173(4) 0.9227(2) 0.0475(9) Uani 1 1 d . . . H26A H 0.4130 0.9027 0.9586 0.057 Uiso 1 1 calc R . . C27 C 0.3971(4) 0.5805(4) 0.7844(2) 0.0341(7) Uani 1 1 d . . . C28 C 0.4928(4) 0.4803(4) 0.7621(2) 0.0452(8) Uani 1 1 d . . . H28A H 0.5904 0.5061 0.7556 0.054 Uiso 1 1 calc R . . C29 C 0.4423(5) 0.3406(4) 0.7495(3) 0.0519(9) Uani 1 1 d . . . H29A H 0.5072 0.2728 0.7360 0.062 Uiso 1 1 calc R . . C30 C 0.2991(6) 0.3022(4) 0.7569(3) 0.0577(11) Uani 1 1 d . . . H30A H 0.2661 0.2088 0.7480 0.069 Uiso 1 1 calc R . . C31 C 0.2046(5) 0.4012(5) 0.7771(3) 0.0621(12) Uani 1 1 d . . . H31A H 0.1066 0.3744 0.7816 0.075 Uiso 1 1 calc R . . C32 C 0.2508(4) 0.5420(4) 0.7914(3) 0.0476(9) Uani 1 1 d . . . H32A H 0.1850 0.6086 0.8053 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.92501(13) 0.63284(14) 0.63004(8) 0.0653(3) Uani 1 1 d . . . N1 N 0.6528(4) 0.9384(4) 0.5921(2) 0.0428(7) Uani 1 1 d . . . N2 N 0.4636(4) 0.7239(3) 0.59656(19) 0.0435(7) Uani 1 1 d . . . N3 N 0.3464(5) 0.5918(4) 0.5027(2) 0.0642(11) Uani 1 1 d . . . H3B H 0.2860 0.5291 0.4800 0.077 Uiso 1 1 calc R . . O1 O 1.0252(8) 0.5341(11) 0.6130(5) 0.191(4) Uani 1 1 d . . . O2 O 0.9609(11) 0.7709(8) 0.6498(6) 0.213(4) Uani 1 1 d . . . O3 O 0.8187(12) 0.6287(9) 0.5786(8) 0.307(8) Uani 1 1 d . . . O4 O 0.8746(18) 0.5858(10) 0.6962(10) 0.362(11) Uani 1 1 d . . . P1 P 0.47533(9) 0.76017(9) 0.80235(5) 0.03171(17) Uani 1 1 d . . . Pt1 Pt 0.560583(13) 0.855962(12) 0.690857(7) 0.03347(6) 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 C1 0.0349(17) 0.0370(17) 0.048(2) 0.0093(14) -0.0032(14) 0.0019(13) C2 0.047(2) 0.0425(19) 0.050(2) 0.0018(16) -0.0051(17) -0.0039(16) C3 0.053(2) 0.049(2) 0.069(3) -0.005(2) -0.012(2) -0.0060(18) C4 0.045(2) 0.047(2) 0.099(4) 0.000(2) -0.012(2) -0.0116(18) C5 0.037(2) 0.050(2) 0.083(3) 0.017(2) 0.001(2) -0.0068(16) C6 0.0332(17) 0.0423(19) 0.060(2) 0.0160(17) -0.0014(16) 0.0020(14) C7 0.0363(18) 0.050(2) 0.063(2) 0.0263(19) 0.0049(17) 0.0088(16) C8 0.048(2) 0.073(3) 0.072(3) 0.032(2) 0.018(2) 0.012(2) C9 0.065(3) 0.091(4) 0.072(3) 0.040(3) 0.028(3) 0.022(3) C10 0.077(3) 0.096(4) 0.041(2) 0.018(2) 0.016(2) 0.031(3) C11 0.051(2) 0.064(2) 0.0376(19) 0.0110(17) 0.0023(16) 0.0203(19) C12 0.055(2) 0.058(2) 0.0333(17) 0.0031(16) -0.0052(16) 0.0200(18) C13 0.078(3) 0.066(3) 0.038(2) -0.0044(19) -0.009(2) 0.025(2) C14 0.053(2) 0.052(2) 0.043(2) -0.0034(17) -0.0122(17) 0.0040(17) C15 0.0387(17) 0.0343(16) 0.0362(17) 0.0021(13) -0.0076(13) -0.0025(13) C16 0.051(2) 0.051(2) 0.0406(19) 0.0102(16) -0.0053(16) -0.0086(17) C17 0.065(3) 0.067(3) 0.043(2) 0.0194(19) -0.013(2) -0.004(2) C18 0.076(3) 0.064(3) 0.060(3) 0.017(2) -0.030(2) 0.006(2) C19 0.046(2) 0.064(3) 0.073(3) 0.000(2) -0.012(2) 0.010(2) C20 0.042(2) 0.0452(19) 0.045(2) 0.0047(15) -0.0030(15) 0.0036(15) C21 0.0360(17) 0.0346(16) 0.0388(17) 0.0002(13) 0.0006(13) 0.0017(13) C22 0.049(2) 0.046(2) 0.045(2) 0.0054(16) -0.0013(16) 0.0048(16) C23 0.045(2) 0.052(2) 0.067(3) 0.008(2) -0.0067(19) 0.0060(17) C24 0.049(2) 0.057(2) 0.075(3) -0.006(2) 0.014(2) 0.0122(19) C25 0.061(3) 0.065(3) 0.058(3) -0.015(2) 0.008(2) 0.008(2) C26 0.047(2) 0.053(2) 0.0417(19) -0.0070(16) -0.0029(16) 0.0030(17) C27 0.0322(16) 0.0369(16) 0.0323(16) 0.0043(13) -0.0042(12) -0.0046(12) C28 0.043(2) 0.0419(19) 0.051(2) -0.0015(16) -0.0003(16) 0.0023(15) C29 0.067(3) 0.042(2) 0.047(2) 0.0002(16) -0.0024(19) 0.0060(18) C30 0.078(3) 0.040(2) 0.052(2) -0.0001(17) -0.001(2) -0.018(2) C31 0.049(2) 0.066(3) 0.068(3) -0.007(2) 0.003(2) -0.025(2) C32 0.039(2) 0.049(2) 0.053(2) -0.0015(17) 0.0005(16) -0.0054(16) Cl1 0.0443(6) 0.0789(8) 0.0705(7) -0.0039(6) -0.0042(5) -0.0091(5) N1 0.0412(17) 0.0480(17) 0.0412(16) 0.0168(13) 0.0054(13) 0.0083(13) N2 0.0483(18) 0.0473(17) 0.0344(15) -0.0021(13) -0.0040(13) 0.0044(14) N3 0.078(3) 0.060(2) 0.052(2) -0.0115(18) -0.028(2) 0.012(2) O1 0.103(5) 0.307(11) 0.173(7) 0.017(7) 0.024(5) 0.101(6) O2 0.233(10) 0.149(6) 0.237(9) 0.029(6) -0.075(7) -0.118(7) O3 0.272(10) 0.169(7) 0.455(16) -0.192(9) -0.297(12) 0.133(7) O4 0.49(2) 0.168(8) 0.48(2) 0.164(11) 0.404(19) 0.142(11) P1 0.0313(4) 0.0328(4) 0.0306(4) 0.0033(3) -0.0022(3) -0.0011(3) Pt1 0.03349(8) 0.03570(8) 0.03119(8) 0.00598(5) -0.00122(5) 0.00111(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. ; 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 C1 C2 1.403(6) . ? C1 C6 1.413(5) . ? C1 Pt1 2.005(4) . ? C2 C3 1.406(6) . ? C2 H2A 0.9300 . ? C3 C4 1.346(7) . ? C3 H3A 0.9300 . ? C4 C5 1.388(8) . ? C4 H4A 0.9300 . ? C5 C6 1.402(6) . ? C5 H5A 0.9300 . ? C6 C7 1.481(6) . ? C7 N1 1.349(5) . ? C7 C8 1.378(6) . ? C8 C9 1.375(8) . ? C8 H8A 0.9300 . ? C9 C10 1.388(8) . ? C9 H9A 0.9300 . ? C10 C11 1.380(6) . ? C10 H10A 0.9300 . ? C11 N1 1.344(5) . ? C11 C12 1.447(6) . ? C12 C13 1.365(6) . ? C12 N2 1.390(5) . ? C13 N3 1.353(7) . ? C13 H13A 0.9300 . ? C14 N2 1.324(5) . ? C14 N3 1.347(5) . ? C14 H14A 0.9300 . ? C15 C16 1.390(5) . ? C15 C20 1.395(5) . ? C15 P1 1.823(4) . ? C16 C17 1.394(6) . ? C16 H16A 0.9300 . ? C17 C18 1.388(8) . ? C17 H17A 0.9300 . ? C18 C19 1.369(8) . ? C18 H18A 0.9300 . ? C19 C20 1.384(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.384(5) . ? C21 C22 1.399(5) . ? C21 P1 1.819(4) . ? C22 C23 1.394(6) . ? C22 H22A 0.9300 . ? C23 C24 1.372(7) . ? C23 H23A 0.9300 . ? C24 C25 1.367(7) . ? C24 H24A 0.9300 . ? C25 C26 1.378(6) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.383(5) . ? C27 C32 1.387(5) . ? C27 P1 1.831(3) . ? C28 C29 1.391(5) . ? C28 H28A 0.9300 . ? C29 C30 1.360(7) . ? C29 H29A 0.9300 . ? C30 C31 1.359(7) . ? C30 H30A 0.9300 . ? C31 C32 1.394(6) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? Cl1 O3 1.263(6) . ? Cl1 O4 1.285(9) . ? Cl1 O2 1.365(7) . ? Cl1 O1 1.381(7) . ? N1 Pt1 2.025(3) . ? N2 Pt1 2.107(3) . ? N3 H3B 0.8600 . ? P1 Pt1 2.2272(9) . ? 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 C2 C1 C6 116.7(3) . . ? C2 C1 Pt1 130.1(3) . . ? C6 C1 Pt1 112.9(3) . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 119.7(4) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 C7 122.3(4) . . ? C1 C6 C7 116.3(3) . . ? N1 C7 C8 118.7(5) . . ? N1 C7 C6 112.1(3) . . ? C8 C7 C6 129.2(4) . . ? C7 C8 C9 119.4(5) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 119.3(5) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? N1 C11 C10 118.6(5) . . ? N1 C11 C12 112.6(3) . . ? C10 C11 C12 128.9(4) . . ? C13 C12 N2 108.1(4) . . ? C13 C12 C11 133.8(4) . . ? N2 C12 C11 118.0(3) . . ? N3 C13 C12 106.3(4) . . ? N3 C13 H13A 126.8 . . ? C12 C13 H13A 126.8 . . ? N2 C14 N3 109.2(4) . . ? N2 C14 H14A 125.4 . . ? N3 C14 H14A 125.4 . . ? C16 C15 C20 119.7(4) . . ? C16 C15 P1 120.6(3) . . ? C20 C15 P1 119.2(3) . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 120.0(4) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 121.9(5) . . ? C18 C19 H19A 119.0 . . ? C20 C19 H19A 119.0 . . ? C19 C20 C15 119.0(4) . . ? C19 C20 H20A 120.5 . . ? C15 C20 H20A 120.5 . . ? C26 C21 C22 118.9(3) . . ? C26 C21 P1 124.9(3) . . ? C22 C21 P1 116.1(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.7(4) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C25 C26 C21 120.3(4) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C28 C27 C32 119.8(3) . . ? C28 C27 P1 116.3(3) . . ? C32 C27 P1 123.9(3) . . ? C27 C28 C29 119.7(4) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C27 C32 C31 118.6(4) . . ? C27 C32 H32A 120.7 . . ? C31 C32 H32A 120.7 . . ? O3 Cl1 O4 106.3(10) . . ? O3 Cl1 O2 107.8(5) . . ? O4 Cl1 O2 102.9(8) . . ? O3 Cl1 O1 112.6(6) . . ? O4 Cl1 O1 101.1(6) . . ? O2 Cl1 O1 124.1(6) . . ? C11 N1 C7 123.7(4) . . ? C11 N1 Pt1 119.0(3) . . ? C7 N1 Pt1 117.0(3) . . ? C14 N2 C12 107.1(3) . . ? C14 N2 Pt1 141.2(3) . . ? C12 N2 Pt1 111.5(3) . . ? C14 N3 C13 109.3(4) . . ? C14 N3 H3B 125.3 . . ? C13 N3 H3B 125.3 . . ? C21 P1 C15 109.87(17) . . ? C21 P1 C27 106.05(16) . . ? C15 P1 C27 99.08(15) . . ? C21 P1 Pt1 111.95(12) . . ? C15 P1 Pt1 115.70(12) . . ? C27 P1 Pt1 113.13(11) . . ? C1 Pt1 N1 81.11(15) . . ? C1 Pt1 N2 159.13(15) . . ? N1 Pt1 N2 78.56(14) . . ? C1 Pt1 P1 97.59(11) . . ? N1 Pt1 P1 175.78(9) . . ? N2 Pt1 P1 103.02(9) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.473 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.100