Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Robertus J.M. (Bert) Klein Gebbink' _publ_contact_author_address ; Organic Chemistry & Catalysis Utrecht University, Faculty of Science Padualaan 8 Utrecht 3584 CH NETHERLANDS ; _publ_contact_author_email R.J.M.KLEINGEBBINK@CHEM.UU.NL _publ_section_title ; "Click" 1,2,3-triazoles as tunable ligands for late transition metal complexes ; loop_ _publ_author_name 'Robertus J.M. Klein Gebbink' 'Bas N. H. Aerts' 'Harm P. Dijkstra' 'Martin Lutz' 'A. Spek' ; B.M.J.M.Suijkerbuijk ; 'G.van Koten' data_s3617a _database_code_depnum_ccdc_archive 'CCDC 624055' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 N5 Pd, B F4' _chemical_formula_sum 'C27 H32 B F4 N5 Pd' _chemical_formula_weight 619.79 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.7077(2) _cell_length_b 13.95732(10) _cell_length_c 20.6417(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5389.74(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35573 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102749 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6200 _reflns_number_gt 4874 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction EvalCCD _computing_structure_solution 'coordinates taken from Pt compound' _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^)+(0.0210P)^2^+5.3977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6200 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _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 Pd1 Pd -0.019581(8) 0.542885(10) 0.316191(7) 0.01808(5) Uani 1 1 d . . . N1 N 0.03571(9) 0.58082(12) 0.23112(8) 0.0233(4) Uani 1 1 d . . . N2 N -0.08345(9) 0.46831(12) 0.38322(8) 0.0244(4) Uani 1 1 d . . . N3 N 0.05346(9) 0.61171(12) 0.38303(8) 0.0222(4) Uani 1 1 d . . . N4 N 0.11738(9) 0.57054(12) 0.38696(8) 0.0248(4) Uani 1 1 d . . . N5 N 0.15785(9) 0.62966(12) 0.42191(8) 0.0233(4) Uani 1 1 d . . . C1 C -0.08126(11) 0.48056(14) 0.25504(10) 0.0224(4) Uani 1 1 d . . . C2 C -0.06810(11) 0.49227(15) 0.18926(10) 0.0262(4) Uani 1 1 d . . . C3 C -0.11206(13) 0.44426(17) 0.14542(11) 0.0360(6) Uani 1 1 d . . . H3 H -0.1039 0.4501 0.1002 0.043 Uiso 1 1 calc R . . C4 C -0.16754(13) 0.38805(18) 0.16808(13) 0.0408(6) Uani 1 1 d . . . H4 H -0.1968 0.3546 0.1380 0.049 Uiso 1 1 calc R . . C5 C -0.18124(12) 0.37950(16) 0.23365(13) 0.0373(6) Uani 1 1 d . . . H5 H -0.2201 0.3414 0.2483 0.045 Uiso 1 1 calc R . . C6 C -0.13805(11) 0.42675(15) 0.27818(11) 0.0267(5) Uani 1 1 d . . . C7 C -0.01273(12) 0.56655(16) 0.17324(10) 0.0295(5) Uani 1 1 d . . . H7A H -0.0364 0.6278 0.1620 0.035 Uiso 1 1 calc R . . H7B H 0.0158 0.5454 0.1354 0.035 Uiso 1 1 calc R . . C8 C 0.06471(13) 0.67973(16) 0.23104(11) 0.0343(5) Uani 1 1 d . . . H8A H 0.0993 0.6867 0.2664 0.051 Uiso 1 1 calc R . . H8B H 0.0256 0.7255 0.2371 0.051 Uiso 1 1 calc R . . H8C H 0.0884 0.6923 0.1896 0.051 Uiso 1 1 calc R . . C9 C 0.09621(12) 0.51220(16) 0.22557(11) 0.0311(5) Uani 1 1 d . . . H9A H 0.1257 0.5292 0.1880 0.047 Uiso 1 1 calc R . . H9B H 0.0775 0.4471 0.2200 0.047 Uiso 1 1 calc R . . H9C H 0.1254 0.5151 0.2650 0.047 Uiso 1 1 calc R . . C10 C -0.15102(11) 0.43439(16) 0.34982(11) 0.0316(5) Uani 1 1 d . . . H10A H -0.1653 0.3711 0.3673 0.038 Uiso 1 1 calc R . . H10B H -0.1903 0.4802 0.3582 0.038 Uiso 1 1 calc R . . C11 C -0.04032(13) 0.38311(16) 0.40211(11) 0.0337(5) Uani 1 1 d . . . H11A H 0.0038 0.4042 0.4233 0.051 Uiso 1 1 calc R . . H11B H -0.0284 0.3458 0.3634 0.051 Uiso 1 1 calc R . . H11C H -0.0680 0.3432 0.4321 0.051 Uiso 1 1 calc R . . C12 C -0.10274(13) 0.52233(17) 0.44254(11) 0.0351(5) Uani 1 1 d . . . H12A H -0.1322 0.4818 0.4707 0.053 Uiso 1 1 calc R . . H12B H -0.1297 0.5799 0.4305 0.053 Uiso 1 1 calc R . . H12C H -0.0591 0.5410 0.4656 0.053 Uiso 1 1 calc R . . C13 C 0.12172(11) 0.70811(15) 0.44018(9) 0.0242(4) Uani 1 1 d . . . H13 H 0.1393 0.7604 0.4650 0.029 Uiso 1 1 calc R . . C14 C 0.05397(11) 0.69688(14) 0.41551(9) 0.0208(4) Uani 1 1 d . . . C15 C 0.23453(11) 0.60814(17) 0.43153(11) 0.0303(5) Uani 1 1 d . . . H15A H 0.2428 0.5386 0.4257 0.036 Uiso 1 1 calc R . . H15B H 0.2487 0.6255 0.4762 0.036 Uiso 1 1 calc R . . C16 C 0.27946(11) 0.66343(15) 0.38383(11) 0.0269(5) Uani 1 1 d . . . C17 C 0.31719(12) 0.74386(18) 0.40332(13) 0.0387(6) Uani 1 1 d . . . H17 H 0.3167 0.7634 0.4474 0.046 Uiso 1 1 calc R . . C18 C 0.35629(13) 0.79622(19) 0.35694(16) 0.0487(7) Uani 1 1 d . . . H18 H 0.3819 0.8519 0.3696 0.058 Uiso 1 1 calc R . . C19 C 0.35732(13) 0.7668(2) 0.29342(15) 0.0471(7) Uani 1 1 d . . . H19 H 0.3844 0.8019 0.2626 0.056 Uiso 1 1 calc R . . C20 C 0.32000(13) 0.68766(18) 0.27396(13) 0.0413(6) Uani 1 1 d . . . H20 H 0.3208 0.6682 0.2299 0.050 Uiso 1 1 calc R . . C21 C 0.28118(12) 0.63636(16) 0.31898(11) 0.0315(5) Uani 1 1 d . . . H21 H 0.2551 0.5815 0.3054 0.038 Uiso 1 1 calc R . . C22 C -0.00800(11) 0.76115(14) 0.42187(9) 0.0219(4) Uani 1 1 d . . . C23 C -0.00794(12) 0.83183(16) 0.46990(11) 0.0316(5) Uani 1 1 d . . . H23 H 0.0314 0.8368 0.4988 0.038 Uiso 1 1 calc R . . C24 C -0.06482(13) 0.89443(17) 0.47547(12) 0.0380(6) Uani 1 1 d . . . H24 H -0.0637 0.9430 0.5077 0.046 Uiso 1 1 calc R . . C25 C -0.12335(12) 0.88732(16) 0.43482(11) 0.0331(5) Uani 1 1 d . . . H25 H -0.1623 0.9305 0.4390 0.040 Uiso 1 1 calc R . . C26 C -0.12443(12) 0.81667(16) 0.38811(11) 0.0307(5) Uani 1 1 d . . . H26 H -0.1648 0.8104 0.3606 0.037 Uiso 1 1 calc R . . C27 C -0.06699(11) 0.75477(15) 0.38104(10) 0.0266(5) Uani 1 1 d . . . H27 H -0.0679 0.7075 0.3480 0.032 Uiso 1 1 calc R . . F1 F 0.26633(9) 0.11517(14) 0.12487(8) 0.0680(5) Uani 1 1 d . . . F2 F 0.27781(9) 0.24384(11) 0.05949(8) 0.0548(4) Uani 1 1 d . . . F3 F 0.37083(7) 0.14576(13) 0.07560(8) 0.0570(4) Uani 1 1 d . . . F4 F 0.27713(11) 0.09705(13) 0.01680(9) 0.0789(6) Uani 1 1 d . . . B1 B 0.29734(14) 0.1497(2) 0.06955(13) 0.0324(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 Pd1 0.01887(8) 0.01733(7) 0.01804(7) -0.00102(6) 0.00238(6) -0.00270(6) N1 0.0273(9) 0.0203(8) 0.0224(8) 0.0006(7) 0.0057(7) -0.0015(7) N2 0.0236(9) 0.0253(9) 0.0245(8) 0.0030(7) 0.0059(7) -0.0020(7) N3 0.0201(9) 0.0235(9) 0.0229(8) 0.0004(7) 0.0009(7) -0.0008(7) N4 0.0225(9) 0.0260(9) 0.0260(9) 0.0016(7) 0.0008(7) -0.0007(7) N5 0.0194(8) 0.0279(9) 0.0226(8) 0.0059(7) 0.0000(7) -0.0026(7) C1 0.0229(10) 0.0177(9) 0.0267(10) -0.0040(8) -0.0028(8) 0.0013(8) C2 0.0279(11) 0.0245(10) 0.0263(11) -0.0070(9) -0.0016(9) 0.0058(9) C3 0.0400(13) 0.0375(13) 0.0306(12) -0.0152(10) -0.0089(10) 0.0118(11) C4 0.0351(13) 0.0350(13) 0.0525(16) -0.0231(12) -0.0143(12) 0.0046(11) C5 0.0266(12) 0.0254(11) 0.0600(16) -0.0098(11) -0.0061(11) -0.0028(10) C6 0.0232(11) 0.0194(10) 0.0374(12) -0.0023(9) -0.0014(9) 0.0008(8) C7 0.0370(12) 0.0311(11) 0.0204(10) 0.0009(8) 0.0023(9) 0.0040(10) C8 0.0443(14) 0.0249(11) 0.0336(12) 0.0032(9) 0.0109(11) -0.0086(10) C9 0.0305(12) 0.0345(12) 0.0285(11) -0.0002(9) 0.0089(10) 0.0051(10) C10 0.0220(11) 0.0306(12) 0.0422(13) 0.0033(10) 0.0033(10) -0.0058(9) C11 0.0365(13) 0.0303(12) 0.0343(12) 0.0105(10) 0.0050(10) 0.0027(10) C12 0.0379(13) 0.0408(14) 0.0267(11) 0.0006(10) 0.0145(10) -0.0013(10) C13 0.0251(11) 0.0262(10) 0.0211(10) 0.0011(8) 0.0000(8) -0.0046(9) C14 0.0230(10) 0.0233(10) 0.0161(9) 0.0007(8) 0.0013(8) -0.0051(8) C15 0.0202(11) 0.0373(13) 0.0335(12) 0.0103(10) -0.0035(9) 0.0024(9) C16 0.0169(10) 0.0275(11) 0.0364(12) 0.0071(9) 0.0002(9) 0.0046(9) C17 0.0235(12) 0.0376(13) 0.0549(15) -0.0018(12) -0.0053(11) 0.0016(10) C18 0.0222(12) 0.0324(14) 0.091(2) 0.0091(14) -0.0062(14) -0.0049(10) C19 0.0301(13) 0.0468(16) 0.0643(18) 0.0238(14) 0.0129(13) 0.0079(12) C20 0.0375(14) 0.0428(15) 0.0435(14) 0.0131(12) 0.0113(12) 0.0151(12) C21 0.0286(11) 0.0273(11) 0.0387(12) 0.0072(10) 0.0042(10) 0.0076(9) C22 0.0219(10) 0.0217(10) 0.0222(10) 0.0006(8) 0.0045(8) -0.0037(8) C23 0.0315(12) 0.0344(12) 0.0290(11) -0.0088(10) 0.0017(9) -0.0037(10) C24 0.0434(14) 0.0324(13) 0.0383(13) -0.0146(10) 0.0108(11) -0.0018(11) C25 0.0326(12) 0.0276(11) 0.0392(13) 0.0023(10) 0.0140(10) 0.0044(10) C26 0.0268(11) 0.0322(12) 0.0332(12) 0.0015(10) 0.0006(9) 0.0021(9) C27 0.0280(11) 0.0252(10) 0.0267(10) -0.0045(9) -0.0018(9) 0.0011(9) F1 0.0491(10) 0.0954(14) 0.0594(10) 0.0384(10) 0.0082(8) -0.0190(9) F2 0.0626(10) 0.0382(8) 0.0637(10) 0.0074(7) 0.0186(8) 0.0123(8) F3 0.0299(8) 0.0859(12) 0.0553(9) 0.0236(9) 0.0029(7) 0.0010(8) F4 0.1065(16) 0.0612(12) 0.0691(12) -0.0241(10) -0.0345(11) 0.0019(11) B1 0.0323(14) 0.0339(14) 0.0310(13) 0.0052(11) -0.0029(11) -0.0037(11) _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 Pd1 C1 1.919(2) . ? Pd1 N2 2.1037(16) . ? Pd1 N1 2.1056(16) . ? Pd1 N3 2.1664(17) . ? N1 C8 1.483(3) . ? N1 C9 1.487(3) . ? N1 C7 1.513(3) . ? N2 C12 1.483(3) . ? N2 C11 1.489(3) . ? N2 C10 1.516(3) . ? N3 N4 1.329(2) . ? N3 C14 1.365(2) . ? N4 N5 1.332(2) . ? N5 C13 1.341(3) . ? N5 C15 1.479(3) . ? C1 C6 1.386(3) . ? C1 C2 1.390(3) . ? C2 C3 1.394(3) . ? C2 C7 1.502(3) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 C10 1.502(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.375(3) . ? C13 H13 0.9500 . ? C14 C22 1.472(3) . ? C15 C16 1.507(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.386(3) . ? C16 C21 1.391(3) . ? C17 C18 1.409(4) . ? C17 H17 0.9500 . ? C18 C19 1.374(4) . ? C18 H18 0.9500 . ? C19 C20 1.367(4) . ? C19 H19 0.9500 . ? C20 C21 1.380(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.391(3) . ? C22 C23 1.399(3) . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 C25 1.383(3) . ? C24 H24 0.9500 . ? C25 C26 1.379(3) . ? C25 H25 0.9500 . ? C26 C27 1.387(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? F1 B1 1.368(3) . ? F2 B1 1.380(3) . ? F3 B1 1.382(3) . ? F4 B1 1.367(3) . ? 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 C1 Pd1 N2 82.35(8) . . ? C1 Pd1 N1 82.00(8) . . ? N2 Pd1 N1 162.16(7) . . ? C1 Pd1 N3 177.85(7) . . ? N2 Pd1 N3 99.14(6) . . ? N1 Pd1 N3 96.30(6) . . ? C8 N1 C9 108.72(17) . . ? C8 N1 C7 109.92(17) . . ? C9 N1 C7 108.08(16) . . ? C8 N1 Pd1 114.49(13) . . ? C9 N1 Pd1 106.04(12) . . ? C7 N1 Pd1 109.35(12) . . ? C12 N2 C11 108.77(17) . . ? C12 N2 C10 109.35(17) . . ? C11 N2 C10 108.77(17) . . ? C12 N2 Pd1 115.46(13) . . ? C11 N2 Pd1 105.05(12) . . ? C10 N2 Pd1 109.21(12) . . ? N4 N3 C14 109.89(16) . . ? N4 N3 Pd1 114.50(12) . . ? C14 N3 Pd1 134.71(14) . . ? N3 N4 N5 106.06(16) . . ? N4 N5 C13 111.82(16) . . ? N4 N5 C15 119.88(17) . . ? C13 N5 C15 128.09(18) . . ? C6 C1 C2 122.43(19) . . ? C6 C1 Pd1 118.68(16) . . ? C2 C1 Pd1 118.88(15) . . ? C1 C2 C3 118.2(2) . . ? C1 C2 C7 114.73(18) . . ? C3 C2 C7 126.5(2) . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 121.3(2) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 118.3(2) . . ? C1 C6 C10 115.12(18) . . ? C5 C6 C10 126.2(2) . . ? C2 C7 N1 109.27(16) . . ? C2 C7 H7A 109.8 . . ? N1 C7 H7A 109.8 . . ? C2 C7 H7B 109.8 . . ? N1 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 109.58(17) . . ? C6 C10 H10A 109.8 . . ? N2 C10 H10A 109.8 . . ? C6 C10 H10B 109.8 . . ? N2 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 105.51(18) . . ? N5 C13 H13 127.2 . . ? C14 C13 H13 127.2 . . ? N3 C14 C13 106.72(18) . . ? N3 C14 C22 124.70(18) . . ? C13 C14 C22 128.57(18) . . ? N5 C15 C16 110.44(16) . . ? N5 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N5 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C21 119.2(2) . . ? C17 C16 C15 120.6(2) . . ? C21 C16 C15 120.2(2) . . ? C16 C17 C18 119.2(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 121.0(2) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 119.4(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C16 121.3(2) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? C27 C22 C23 118.36(19) . . ? C27 C22 C14 122.11(18) . . ? C23 C22 C14 119.52(19) . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.9(2) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 119.1(2) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 120.5(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.7(2) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? F4 B1 F1 111.0(2) . . ? F4 B1 F2 108.6(2) . . ? F1 B1 F2 110.4(2) . . ? F4 B1 F3 109.0(2) . . ? F1 B1 F3 109.4(2) . . ? F2 B1 F3 108.4(2) . . ? 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 C1 Pd1 N1 C8 140.85(16) . . . . ? N2 Pd1 N1 C8 169.7(2) . . . . ? N3 Pd1 N1 C8 -40.46(15) . . . . ? C1 Pd1 N1 C9 -99.28(14) . . . . ? N2 Pd1 N1 C9 -70.4(3) . . . . ? N3 Pd1 N1 C9 79.40(13) . . . . ? C1 Pd1 N1 C7 17.02(13) . . . . ? N2 Pd1 N1 C7 45.9(3) . . . . ? N3 Pd1 N1 C7 -164.30(13) . . . . ? C1 Pd1 N2 C12 -139.92(16) . . . . ? N1 Pd1 N2 C12 -168.8(2) . . . . ? N3 Pd1 N2 C12 41.65(16) . . . . ? C1 Pd1 N2 C11 100.27(14) . . . . ? N1 Pd1 N2 C11 71.4(3) . . . . ? N3 Pd1 N2 C11 -78.16(14) . . . . ? C1 Pd1 N2 C10 -16.24(13) . . . . ? N1 Pd1 N2 C10 -45.1(3) . . . . ? N3 Pd1 N2 C10 165.33(13) . . . . ? N2 Pd1 N3 N4 102.28(13) . . . . ? N1 Pd1 N3 N4 -68.75(14) . . . . ? N2 Pd1 N3 C14 -90.01(18) . . . . ? N1 Pd1 N3 C14 98.96(18) . . . . ? C14 N3 N4 N5 0.1(2) . . . . ? Pd1 N3 N4 N5 170.84(11) . . . . ? N3 N4 N5 C13 -0.4(2) . . . . ? N3 N4 N5 C15 -175.59(16) . . . . ? N2 Pd1 C1 C6 4.95(16) . . . . ? N1 Pd1 C1 C6 176.37(17) . . . . ? N2 Pd1 C1 C2 -176.08(17) . . . . ? N1 Pd1 C1 C2 -4.66(16) . . . . ? C6 C1 C2 C3 -3.0(3) . . . . ? Pd1 C1 C2 C3 178.12(16) . . . . ? C6 C1 C2 C7 169.56(19) . . . . ? Pd1 C1 C2 C7 -9.4(3) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C7 C2 C3 C4 -170.6(2) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C2 C1 C6 C5 2.9(3) . . . . ? Pd1 C1 C6 C5 -178.13(16) . . . . ? C2 C1 C6 C10 -170.81(19) . . . . ? Pd1 C1 C6 C10 8.1(2) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C4 C5 C6 C10 172.1(2) . . . . ? C1 C2 C7 N1 23.2(3) . . . . ? C3 C2 C7 N1 -165.0(2) . . . . ? C8 N1 C7 C2 -151.81(17) . . . . ? C9 N1 C7 C2 89.7(2) . . . . ? Pd1 N1 C7 C2 -25.33(19) . . . . ? C1 C6 C10 N2 -21.4(3) . . . . ? C5 C6 C10 N2 165.4(2) . . . . ? C12 N2 C10 C6 150.98(18) . . . . ? C11 N2 C10 C6 -90.4(2) . . . . ? Pd1 N2 C10 C6 23.8(2) . . . . ? N4 N5 C13 C14 0.6(2) . . . . ? C15 N5 C13 C14 175.24(18) . . . . ? N4 N3 C14 C13 0.2(2) . . . . ? Pd1 N3 C14 C13 -167.87(14) . . . . ? N4 N3 C14 C22 -179.24(17) . . . . ? Pd1 N3 C14 C22 12.6(3) . . . . ? N5 C13 C14 N3 -0.5(2) . . . . ? N5 C13 C14 C22 178.98(18) . . . . ? N4 N5 C15 C16 97.5(2) . . . . ? C13 N5 C15 C16 -76.8(3) . . . . ? N5 C15 C16 C17 103.7(2) . . . . ? N5 C15 C16 C21 -73.7(3) . . . . ? C21 C16 C17 C18 0.1(3) . . . . ? C15 C16 C17 C18 -177.4(2) . . . . ? C16 C17 C18 C19 -0.7(4) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? C18 C19 C20 C21 -0.5(4) . . . . ? C19 C20 C21 C16 -0.2(3) . . . . ? C17 C16 C21 C20 0.4(3) . . . . ? C15 C16 C21 C20 177.8(2) . . . . ? N3 C14 C22 C27 -18.2(3) . . . . ? C13 C14 C22 C27 162.4(2) . . . . ? N3 C14 C22 C23 162.44(19) . . . . ? C13 C14 C22 C23 -16.9(3) . . . . ? C27 C22 C23 C24 -1.1(3) . . . . ? C14 C22 C23 C24 178.3(2) . . . . ? C22 C23 C24 C25 1.4(4) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 C27 -1.3(3) . . . . ? C25 C26 C27 C22 1.6(3) . . . . ? C23 C22 C27 C26 -0.3(3) . . . . ? C14 C22 C27 C26 -179.72(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.465 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.064 #===END data_s3618a _database_code_depnum_ccdc_archive 'CCDC 624056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 N5 Pt, B F4' _chemical_formula_sum 'C27 H32 B F4 N5 Pt' _chemical_formula_weight 708.48 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6226(4) _cell_length_b 13.9422(7) _cell_length_c 20.7557(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5389.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49492 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 5.261 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 133892 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6195 _reflns_number_gt 5229 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, ABST' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _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^)+(0.0131P)^2^+5.9104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6195 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0371 _refine_ls_wR_factor_gt 0.0340 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.004 _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 Pt1 Pt -0.017882(4) 0.540423(5) 0.316444(3) 0.01706(3) Uani 1 1 d . . . N1 N 0.03803(10) 0.58011(13) 0.23329(8) 0.0218(4) Uani 1 1 d . . . N2 N -0.08293(10) 0.46850(13) 0.38279(8) 0.0222(4) Uani 1 1 d . . . N3 N 0.05445(10) 0.60945(13) 0.38246(8) 0.0206(4) Uani 1 1 d . . . N4 N 0.11908(10) 0.56873(14) 0.38723(9) 0.0235(4) Uani 1 1 d . . . N5 N 0.15896(10) 0.62874(14) 0.42250(8) 0.0222(4) Uani 1 1 d . . . C1 C -0.07987(12) 0.47831(15) 0.25497(10) 0.0215(4) Uani 1 1 d . . . C2 C -0.06596(13) 0.48992(17) 0.18942(10) 0.0250(5) Uani 1 1 d . . . C3 C -0.11042(14) 0.44278(18) 0.14524(12) 0.0326(6) Uani 1 1 d . . . H3 H -0.1018 0.4486 0.1003 0.039 Uiso 1 1 calc R . . C4 C -0.16705(14) 0.3876(2) 0.16755(13) 0.0380(6) Uani 1 1 d . . . H4 H -0.1965 0.3548 0.1374 0.046 Uiso 1 1 calc R . . C5 C -0.18202(13) 0.37902(18) 0.23307(13) 0.0340(6) Uani 1 1 d . . . H5 H -0.2217 0.3418 0.2473 0.041 Uiso 1 1 calc R . . C6 C -0.13816(12) 0.42565(16) 0.27748(11) 0.0255(5) Uani 1 1 d . . . C7 C -0.01035(14) 0.56505(18) 0.17459(10) 0.0285(5) Uani 1 1 d . . . H7A H -0.0343 0.6261 0.1632 0.034 Uiso 1 1 calc R . . H7B H 0.0190 0.5444 0.1373 0.034 Uiso 1 1 calc R . . C8 C 0.06520(15) 0.68050(17) 0.23311(12) 0.0325(6) Uani 1 1 d . . . H8A H 0.1004 0.6886 0.2678 0.049 Uiso 1 1 calc R . . H8B H 0.0250 0.7248 0.2398 0.049 Uiso 1 1 calc R . . H8C H 0.0880 0.6942 0.1916 0.049 Uiso 1 1 calc R . . C9 C 0.10048(13) 0.51383(18) 0.22671(11) 0.0302(5) Uani 1 1 d . . . H9A H 0.1295 0.5329 0.1894 0.045 Uiso 1 1 calc R . . H9B H 0.0831 0.4481 0.2206 0.045 Uiso 1 1 calc R . . H9C H 0.1299 0.5169 0.2658 0.045 Uiso 1 1 calc R . . C10 C -0.15140(12) 0.43546(18) 0.34890(12) 0.0295(5) Uani 1 1 d . . . H10A H -0.1669 0.3730 0.3668 0.035 Uiso 1 1 calc R . . H10B H -0.1902 0.4826 0.3565 0.035 Uiso 1 1 calc R . . C11 C -0.04210(14) 0.38177(18) 0.40362(12) 0.0312(5) Uani 1 1 d . . . H11A H 0.0023 0.4016 0.4251 0.047 Uiso 1 1 calc R . . H11B H -0.0303 0.3426 0.3659 0.047 Uiso 1 1 calc R . . H11C H -0.0715 0.3441 0.4335 0.047 Uiso 1 1 calc R . . C12 C -0.10332(14) 0.52443(18) 0.44106(11) 0.0327(6) Uani 1 1 d . . . H12A H -0.1341 0.4851 0.4688 0.049 Uiso 1 1 calc R . . H12B H -0.1294 0.5823 0.4280 0.049 Uiso 1 1 calc R . . H12C H -0.0599 0.5427 0.4647 0.049 Uiso 1 1 calc R . . C13 C 0.12196(12) 0.70683(16) 0.44018(10) 0.0226(4) Uani 1 1 d . . . H13 H 0.1390 0.7594 0.4650 0.027 Uiso 1 1 calc R . . C14 C 0.05385(12) 0.69525(15) 0.41495(9) 0.0191(4) Uani 1 1 d . . . C15 C 0.23602(12) 0.60785(18) 0.43263(11) 0.0286(5) Uani 1 1 d . . . H15A H 0.2448 0.5384 0.4267 0.034 Uiso 1 1 calc R . . H15B H 0.2497 0.6251 0.4772 0.034 Uiso 1 1 calc R . . C16 C 0.28122(12) 0.66419(17) 0.38547(12) 0.0261(5) Uani 1 1 d . . . C17 C 0.31816(13) 0.7456(2) 0.40482(15) 0.0387(6) Uani 1 1 d . . . H17 H 0.3170 0.7659 0.4485 0.046 Uiso 1 1 calc R . . C18 C 0.35768(14) 0.7979(2) 0.35836(18) 0.0506(8) Uani 1 1 d . . . H18 H 0.3830 0.8541 0.3707 0.061 Uiso 1 1 calc R . . C19 C 0.35943(15) 0.7675(2) 0.29545(16) 0.0492(8) Uani 1 1 d . . . H19 H 0.3868 0.8026 0.2648 0.059 Uiso 1 1 calc R . . C20 C 0.32282(15) 0.6882(2) 0.27606(14) 0.0434(7) Uani 1 1 d . . . H20 H 0.3240 0.6686 0.2322 0.052 Uiso 1 1 calc R . . C21 C 0.28379(14) 0.63626(18) 0.32082(12) 0.0325(6) Uani 1 1 d . . . H21 H 0.2583 0.5807 0.3074 0.039 Uiso 1 1 calc R . . C22 C -0.00814(12) 0.75998(15) 0.42130(10) 0.0206(4) Uani 1 1 d . . . C23 C -0.00827(14) 0.82927(18) 0.47000(12) 0.0309(5) Uani 1 1 d . . . H23 H 0.0308 0.8325 0.4994 0.037 Uiso 1 1 calc R . . C24 C -0.06470(15) 0.89312(19) 0.47571(12) 0.0364(6) Uani 1 1 d . . . H24 H -0.0635 0.9409 0.5083 0.044 Uiso 1 1 calc R . . C25 C -0.12301(14) 0.88824(18) 0.43442(12) 0.0325(6) Uani 1 1 d . . . H25 H -0.1618 0.9320 0.4387 0.039 Uiso 1 1 calc R . . C26 C -0.12400(13) 0.81897(17) 0.38689(12) 0.0296(5) Uani 1 1 d . . . H26 H -0.1642 0.8144 0.3589 0.036 Uiso 1 1 calc R . . C27 C -0.06696(12) 0.75599(17) 0.37963(11) 0.0246(5) Uani 1 1 d . . . H27 H -0.0679 0.7097 0.3460 0.030 Uiso 1 1 calc R . . F1 F 0.26579(9) 0.11822(15) 0.12545(9) 0.0652(6) Uani 1 1 d . . . F2 F 0.27879(10) 0.24687(12) 0.06002(8) 0.0497(4) Uani 1 1 d . . . F3 F 0.37203(8) 0.14813(14) 0.07763(8) 0.0528(5) Uani 1 1 d . . . F4 F 0.27819(13) 0.09916(14) 0.01785(10) 0.0755(7) Uani 1 1 d . . . B1 B 0.29796(16) 0.1521(2) 0.07048(14) 0.0318(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 Pt1 0.01794(4) 0.01640(4) 0.01684(4) -0.00109(3) 0.00244(3) -0.00241(3) N1 0.0263(10) 0.0193(9) 0.0197(9) 0.0004(7) 0.0052(7) -0.0015(8) N2 0.0224(9) 0.0235(10) 0.0206(9) 0.0020(7) 0.0054(7) -0.0034(8) N3 0.0205(9) 0.0224(9) 0.0189(8) -0.0003(7) 0.0006(7) -0.0012(8) N4 0.0216(9) 0.0239(10) 0.0249(9) 0.0017(8) -0.0003(8) -0.0016(8) N5 0.0187(9) 0.0267(10) 0.0211(9) 0.0045(8) -0.0009(7) -0.0027(8) C1 0.0232(11) 0.0167(10) 0.0244(11) -0.0043(8) -0.0028(9) 0.0005(8) C2 0.0275(12) 0.0235(11) 0.0239(11) -0.0060(9) -0.0012(9) 0.0033(9) C3 0.0377(14) 0.0333(14) 0.0268(12) -0.0124(10) -0.0066(10) 0.0092(11) C4 0.0335(14) 0.0342(14) 0.0464(15) -0.0206(12) -0.0132(12) 0.0038(12) C5 0.0254(12) 0.0243(12) 0.0523(16) -0.0073(11) -0.0043(11) -0.0032(10) C6 0.0224(11) 0.0182(11) 0.0358(13) -0.0019(9) -0.0023(10) -0.0007(9) C7 0.0345(13) 0.0321(13) 0.0189(11) 0.0008(9) 0.0017(9) 0.0032(11) C8 0.0457(16) 0.0227(12) 0.0291(12) 0.0033(10) 0.0099(11) -0.0083(11) C9 0.0300(13) 0.0335(13) 0.0272(12) 0.0017(10) 0.0096(10) 0.0056(11) C10 0.0196(11) 0.0313(14) 0.0376(13) 0.0014(10) 0.0046(10) -0.0074(10) C11 0.0348(13) 0.0275(12) 0.0313(12) 0.0111(10) 0.0048(10) 0.0011(11) C12 0.0351(14) 0.0367(14) 0.0263(12) -0.0004(10) 0.0122(10) -0.0031(11) C13 0.0234(11) 0.0257(12) 0.0187(10) 0.0007(9) 0.0003(8) -0.0037(9) C14 0.0219(10) 0.0203(10) 0.0152(9) 0.0017(8) 0.0019(8) -0.0048(9) C15 0.0197(11) 0.0353(14) 0.0309(12) 0.0105(10) -0.0033(9) 0.0008(10) C16 0.0161(10) 0.0256(12) 0.0368(13) 0.0071(10) 0.0011(9) 0.0028(9) C17 0.0228(12) 0.0352(15) 0.0580(17) -0.0006(13) -0.0076(12) 0.0008(11) C18 0.0244(13) 0.0288(15) 0.099(3) 0.0117(16) -0.0096(15) -0.0051(12) C19 0.0298(14) 0.0486(19) 0.069(2) 0.0256(16) 0.0147(14) 0.0093(14) C20 0.0413(16) 0.0447(17) 0.0444(16) 0.0163(13) 0.0133(13) 0.0176(14) C21 0.0317(13) 0.0282(13) 0.0376(13) 0.0074(11) 0.0055(11) 0.0087(11) C22 0.0218(11) 0.0189(10) 0.0211(10) 0.0009(8) 0.0051(8) -0.0035(9) C23 0.0314(13) 0.0329(13) 0.0283(12) -0.0089(10) 0.0022(10) -0.0032(11) C24 0.0423(16) 0.0310(14) 0.0360(13) -0.0138(11) 0.0110(12) -0.0011(12) C25 0.0325(13) 0.0257(12) 0.0392(14) 0.0021(10) 0.0150(11) 0.0040(11) C26 0.0265(12) 0.0290(13) 0.0334(13) 0.0032(10) 0.0006(10) 0.0032(10) C27 0.0255(12) 0.0239(11) 0.0245(11) -0.0026(9) 0.0000(9) -0.0001(10) F1 0.0453(11) 0.0924(15) 0.0580(11) 0.0391(11) 0.0069(9) -0.0172(10) F2 0.0562(11) 0.0365(9) 0.0564(10) 0.0061(8) 0.0135(8) 0.0098(8) F3 0.0299(8) 0.0779(13) 0.0507(10) 0.0195(9) 0.0014(7) 0.0008(9) F4 0.1026(18) 0.0565(13) 0.0673(13) -0.0225(10) -0.0371(12) 0.0022(12) B1 0.0333(15) 0.0313(15) 0.0307(14) 0.0075(11) -0.0021(12) -0.0044(13) _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 Pt1 C1 1.926(2) . ? Pt1 N1 2.0901(17) . ? Pt1 N2 2.0903(17) . ? Pt1 N3 2.1490(18) . ? N1 C8 1.488(3) . ? N1 C9 1.492(3) . ? N1 C7 1.530(3) . ? N2 C12 1.488(3) . ? N2 C11 1.492(3) . ? N2 C10 1.527(3) . ? N3 N4 1.334(3) . ? N3 C14 1.373(3) . ? N4 N5 1.337(3) . ? N5 C13 1.340(3) . ? N5 C15 1.479(3) . ? C1 C6 1.391(3) . ? C1 C2 1.394(3) . ? C2 C3 1.399(3) . ? C2 C7 1.505(3) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 C10 1.509(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.382(3) . ? C13 H13 0.9500 . ? C14 C22 1.471(3) . ? C15 C16 1.511(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.387(4) . ? C16 C21 1.398(3) . ? C17 C18 1.415(4) . ? C17 H17 0.9500 . ? C18 C19 1.373(5) . ? C18 H18 0.9500 . ? C19 C20 1.360(4) . ? C19 H19 0.9500 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.397(3) . ? C22 C23 1.398(3) . ? C23 C24 1.382(4) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.386(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? F1 B1 1.372(3) . ? F2 B1 1.386(3) . ? F3 B1 1.388(3) . ? F4 B1 1.369(3) . ? 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 C1 Pt1 N1 82.56(8) . . ? C1 Pt1 N2 82.73(8) . . ? N1 Pt1 N2 163.67(7) . . ? C1 Pt1 N3 177.87(8) . . ? N1 Pt1 N3 95.49(7) . . ? N2 Pt1 N3 99.10(7) . . ? C8 N1 C9 108.50(19) . . ? C8 N1 C7 109.10(18) . . ? C9 N1 C7 107.53(17) . . ? C8 N1 Pt1 114.86(14) . . ? C9 N1 Pt1 107.46(13) . . ? C7 N1 Pt1 109.15(13) . . ? C12 N2 C11 108.61(18) . . ? C12 N2 C10 108.63(18) . . ? C11 N2 C10 108.32(18) . . ? C12 N2 Pt1 115.58(14) . . ? C11 N2 Pt1 106.51(13) . . ? C10 N2 Pt1 108.97(13) . . ? N4 N3 C14 109.97(18) . . ? N4 N3 Pt1 114.97(13) . . ? C14 N3 Pt1 134.27(15) . . ? N3 N4 N5 105.99(17) . . ? N4 N5 C13 111.89(18) . . ? N4 N5 C15 119.57(19) . . ? C13 N5 C15 128.32(19) . . ? C6 C1 C2 122.3(2) . . ? C6 C1 Pt1 118.84(17) . . ? C2 C1 Pt1 118.87(17) . . ? C1 C2 C3 118.4(2) . . ? C1 C2 C7 114.09(19) . . ? C3 C2 C7 126.9(2) . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.8(2) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 119.2(2) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C1 C6 C5 118.8(2) . . ? C1 C6 C10 114.2(2) . . ? C5 C6 C10 126.6(2) . . ? C2 C7 N1 109.75(18) . . ? C2 C7 H7A 109.7 . . ? N1 C7 H7A 109.7 . . ? C2 C7 H7B 109.7 . . ? N1 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 110.08(18) . . ? C6 C10 H10A 109.6 . . ? N2 C10 H10A 109.6 . . ? C6 C10 H10B 109.6 . . ? N2 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 105.87(19) . . ? N5 C13 H13 127.1 . . ? C14 C13 H13 127.1 . . ? N3 C14 C13 106.28(19) . . ? N3 C14 C22 125.79(19) . . ? C13 C14 C22 127.9(2) . . ? N5 C15 C16 110.24(18) . . ? N5 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N5 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C21 119.3(2) . . ? C17 C16 C15 120.9(2) . . ? C21 C16 C15 119.7(2) . . ? C16 C17 C18 118.8(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 121.4(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.3(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C16 121.1(3) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? C27 C22 C23 118.3(2) . . ? C27 C22 C14 122.38(19) . . ? C23 C22 C14 119.3(2) . . ? C24 C23 C22 120.5(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.7(2) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.1(2) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 120.7(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.6(2) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? F4 B1 F1 111.1(2) . . ? F4 B1 F2 108.6(2) . . ? F1 B1 F2 110.2(2) . . ? F4 B1 F3 109.3(2) . . ? F1 B1 F3 109.3(2) . . ? F2 B1 F3 108.1(2) . . ? 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 C1 Pt1 N1 C8 139.02(18) . . . . ? N2 Pt1 N1 C8 164.9(2) . . . . ? N3 Pt1 N1 C8 -41.84(17) . . . . ? C1 Pt1 N1 C9 -100.17(15) . . . . ? N2 Pt1 N1 C9 -74.2(3) . . . . ? N3 Pt1 N1 C9 78.97(15) . . . . ? C1 Pt1 N1 C7 16.16(15) . . . . ? N2 Pt1 N1 C7 42.1(3) . . . . ? N3 Pt1 N1 C7 -164.70(14) . . . . ? C1 Pt1 N2 C12 -139.04(17) . . . . ? N1 Pt1 N2 C12 -165.0(2) . . . . ? N3 Pt1 N2 C12 42.06(17) . . . . ? C1 Pt1 N2 C11 100.24(15) . . . . ? N1 Pt1 N2 C11 74.3(3) . . . . ? N3 Pt1 N2 C11 -78.66(15) . . . . ? C1 Pt1 N2 C10 -16.42(15) . . . . ? N1 Pt1 N2 C10 -42.3(3) . . . . ? N3 Pt1 N2 C10 164.69(14) . . . . ? N1 Pt1 N3 N4 -69.52(15) . . . . ? N2 Pt1 N3 N4 103.11(15) . . . . ? N1 Pt1 N3 C14 99.06(19) . . . . ? N2 Pt1 N3 C14 -88.32(19) . . . . ? C14 N3 N4 N5 -0.1(2) . . . . ? Pt1 N3 N4 N5 171.24(12) . . . . ? N3 N4 N5 C13 -0.3(2) . . . . ? N3 N4 N5 C15 -175.33(17) . . . . ? N1 Pt1 C1 C6 177.97(19) . . . . ? N2 Pt1 C1 C6 5.09(17) . . . . ? N1 Pt1 C1 C2 -3.83(18) . . . . ? N2 Pt1 C1 C2 -176.71(19) . . . . ? C6 C1 C2 C3 -3.2(3) . . . . ? Pt1 C1 C2 C3 178.64(17) . . . . ? C6 C1 C2 C7 168.0(2) . . . . ? Pt1 C1 C2 C7 -10.1(3) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C7 C2 C3 C4 -169.0(2) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C2 C1 C6 C5 3.3(3) . . . . ? Pt1 C1 C6 C5 -178.60(17) . . . . ? C2 C1 C6 C10 -170.0(2) . . . . ? Pt1 C1 C6 C10 8.1(3) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C4 C5 C6 C10 171.3(2) . . . . ? C1 C2 C7 N1 23.2(3) . . . . ? C3 C2 C7 N1 -166.5(2) . . . . ? C8 N1 C7 C2 -151.09(19) . . . . ? C9 N1 C7 C2 91.4(2) . . . . ? Pt1 N1 C7 C2 -24.9(2) . . . . ? C1 C6 C10 N2 -21.6(3) . . . . ? C5 C6 C10 N2 165.7(2) . . . . ? C12 N2 C10 C6 150.92(19) . . . . ? C11 N2 C10 C6 -91.3(2) . . . . ? Pt1 N2 C10 C6 24.2(2) . . . . ? N4 N5 C13 C14 0.6(2) . . . . ? C15 N5 C13 C14 175.04(19) . . . . ? N4 N3 C14 C13 0.4(2) . . . . ? Pt1 N3 C14 C13 -168.56(15) . . . . ? N4 N3 C14 C22 -179.05(19) . . . . ? Pt1 N3 C14 C22 12.0(3) . . . . ? N5 C13 C14 N3 -0.6(2) . . . . ? N5 C13 C14 C22 178.88(19) . . . . ? N4 N5 C15 C16 97.7(2) . . . . ? C13 N5 C15 C16 -76.4(3) . . . . ? N5 C15 C16 C17 103.2(2) . . . . ? N5 C15 C16 C21 -74.3(3) . . . . ? C21 C16 C17 C18 -0.2(4) . . . . ? C15 C16 C17 C18 -177.7(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 1.0(4) . . . . ? C18 C19 C20 C21 -0.9(4) . . . . ? C19 C20 C21 C16 0.2(4) . . . . ? C17 C16 C21 C20 0.3(4) . . . . ? C15 C16 C21 C20 177.9(2) . . . . ? N3 C14 C22 C27 -19.6(3) . . . . ? C13 C14 C22 C27 161.1(2) . . . . ? N3 C14 C22 C23 161.4(2) . . . . ? C13 C14 C22 C23 -17.9(3) . . . . ? C27 C22 C23 C24 -1.2(4) . . . . ? C14 C22 C23 C24 177.8(2) . . . . ? C22 C23 C24 C25 1.6(4) . . . . ? C23 C24 C25 C26 -0.5(4) . . . . ? C24 C25 C26 C27 -1.1(4) . . . . ? C25 C26 C27 C22 1.6(4) . . . . ? C23 C22 C27 C26 -0.4(3) . . . . ? C14 C22 C27 C26 -179.4(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.673 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.073 #===END data_s3607a _database_code_depnum_ccdc_archive 'CCDC 624057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 N5 Pt, B F4, 0.5(C H2 Cl2)' _chemical_formula_sum 'C27.50 H33 B Cl F4 N5 Pt' _chemical_formula_weight 750.94 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1861(3) _cell_length_b 12.05785(13) _cell_length_c 12.9754(4) _cell_angle_alpha 78.165(1) _cell_angle_beta 68.692(1) _cell_angle_gamma 63.542(1) _cell_volume 1457.75(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 20038 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 4.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39400 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6685 _reflns_number_gt 6187 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _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^)+(0.0122P)^2^+1.8780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6685 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0377 _refine_ls_wR_factor_gt 0.0366 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _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 Pt1 Pt 0.561477(9) 0.687562(8) 0.292867(7) 0.01273(3) Uani 1 1 d . . . N1 N 0.6433(2) 0.51031(17) 0.23729(15) 0.0161(4) Uani 1 1 d . . . N2 N 0.5043(2) 0.83727(18) 0.38265(16) 0.0181(4) Uani 1 1 d . . . N3 N 0.4527(2) 0.78524(17) 0.17374(16) 0.0157(4) Uani 1 1 d . . . N4 N 0.3196(2) 0.80065(18) 0.20955(16) 0.0183(4) Uani 1 1 d . . . N5 N 0.2728(2) 0.84581(18) 0.12199(17) 0.0199(4) Uani 1 1 d . . . C1 C 0.6459(2) 0.5969(2) 0.40662(18) 0.0165(5) Uani 1 1 d . . . C2 C 0.6914(3) 0.4691(2) 0.41594(19) 0.0191(5) Uani 1 1 d . . . C3 C 0.7523(3) 0.4032(3) 0.4983(2) 0.0283(6) Uani 1 1 d . . . H3 H 0.7862 0.3153 0.5055 0.034 Uiso 1 1 calc R . . C4 C 0.7630(3) 0.4672(3) 0.5698(2) 0.0328(7) Uani 1 1 d . . . H4 H 0.8052 0.4220 0.6256 0.039 Uiso 1 1 calc R . . C5 C 0.7136(3) 0.5959(3) 0.5618(2) 0.0300(6) Uani 1 1 d . . . H5 H 0.7201 0.6382 0.6124 0.036 Uiso 1 1 calc R . . C6 C 0.6544(3) 0.6618(2) 0.4783(2) 0.0229(5) Uani 1 1 d . . . C7 C 0.6574(3) 0.4195(2) 0.3374(2) 0.0206(5) Uani 1 1 d . . . H7A H 0.5684 0.4089 0.3753 0.025 Uiso 1 1 calc R . . H7B H 0.7330 0.3376 0.3131 0.025 Uiso 1 1 calc R . . C8 C 0.7859(3) 0.4822(2) 0.1554(2) 0.0233(5) Uani 1 1 d . . . H8A H 0.8241 0.3988 0.1291 0.035 Uiso 1 1 calc R . . H8B H 0.8478 0.4860 0.1907 0.035 Uiso 1 1 calc R . . H8C H 0.7794 0.5431 0.0925 0.035 Uiso 1 1 calc R . . C9 C 0.5552(3) 0.4909(2) 0.1860(2) 0.0209(5) Uani 1 1 d . . . H9A H 0.5538 0.5419 0.1168 0.031 Uiso 1 1 calc R . . H9B H 0.4592 0.5147 0.2371 0.031 Uiso 1 1 calc R . . H9C H 0.5946 0.4032 0.1703 0.031 Uiso 1 1 calc R . . C10 C 0.6029(3) 0.7993(2) 0.4512(2) 0.0265(6) Uani 1 1 d . . . H10A H 0.6837 0.8212 0.4092 0.032 Uiso 1 1 calc R . . H10B H 0.5528 0.8443 0.5205 0.032 Uiso 1 1 calc R . . C11 C 0.3591(3) 0.8660(3) 0.4593(2) 0.0316(6) Uani 1 1 d . . . H11A H 0.3280 0.9388 0.5003 0.047 Uiso 1 1 calc R . . H11B H 0.3578 0.7949 0.5115 0.047 Uiso 1 1 calc R . . H11C H 0.2957 0.8832 0.4166 0.047 Uiso 1 1 calc R . . C12 C 0.5075(3) 0.9507(2) 0.3133(2) 0.0273(6) Uani 1 1 d . . . H12A H 0.4431 0.9763 0.2697 0.041 Uiso 1 1 calc R . . H12B H 0.6031 0.9334 0.2633 0.041 Uiso 1 1 calc R . . H12C H 0.4784 1.0173 0.3611 0.041 Uiso 1 1 calc R . . C13 C 0.3728(3) 0.8600(2) 0.0314(2) 0.0206(5) Uani 1 1 d . . . H13 H 0.3645 0.8905 -0.0403 0.025 Uiso 1 1 calc R . . C14 C 0.4901(3) 0.8211(2) 0.06388(19) 0.0167(5) Uani 1 1 d . . . C15 C 0.1313(3) 0.8613(2) 0.1316(2) 0.0249(6) Uani 1 1 d . . . H15A H 0.1106 0.8992 0.0614 0.030 Uiso 1 1 calc R . . H15B H 0.0611 0.9178 0.1915 0.030 Uiso 1 1 calc R . . C16 C 0.1204(3) 0.7374(2) 0.1569(2) 0.0233(5) Uani 1 1 d . . . C17 C -0.0007(3) 0.7285(3) 0.2308(3) 0.0356(7) Uani 1 1 d . . . H17 H -0.0772 0.8006 0.2648 0.043 Uiso 1 1 calc R . . C18 C -0.0116(3) 0.6150(3) 0.2558(3) 0.0422(8) Uani 1 1 d . . . H18 H -0.0953 0.6099 0.3068 0.051 Uiso 1 1 calc R . . C19 C 0.0985(3) 0.5100(3) 0.2070(3) 0.0343(7) Uani 1 1 d . . . H19 H 0.0912 0.4323 0.2245 0.041 Uiso 1 1 calc R . . C20 C 0.2195(3) 0.5178(3) 0.1326(2) 0.0296(6) Uani 1 1 d . . . H20 H 0.2955 0.4454 0.0987 0.036 Uiso 1 1 calc R . . C21 C 0.2303(3) 0.6310(2) 0.1071(2) 0.0267(6) Uani 1 1 d . . . H21 H 0.3136 0.6359 0.0551 0.032 Uiso 1 1 calc R . . C22 C 0.6293(3) 0.8177(2) -0.00418(19) 0.0173(5) Uani 1 1 d . . . C23 C 0.6601(3) 0.8317(2) -0.1195(2) 0.0254(6) Uani 1 1 d . . . H23 H 0.5934 0.8389 -0.1522 0.030 Uiso 1 1 calc R . . C24 C 0.7874(3) 0.8351(3) -0.1861(2) 0.0293(6) Uani 1 1 d . . . H24 H 0.8066 0.8459 -0.2642 0.035 Uiso 1 1 calc R . . C25 C 0.8866(3) 0.8229(2) -0.1402(2) 0.0262(6) Uani 1 1 d . . . H25 H 0.9734 0.8258 -0.1864 0.031 Uiso 1 1 calc R . . C26 C 0.8585(3) 0.8062(2) -0.0263(2) 0.0249(5) Uani 1 1 d . . . H26 H 0.9268 0.7966 0.0057 0.030 Uiso 1 1 calc R . . C27 C 0.7308(3) 0.8035(2) 0.0411(2) 0.0207(5) Uani 1 1 d . . . H27 H 0.7126 0.7919 0.1191 0.025 Uiso 1 1 calc R . . F1 F 0.8066(2) 0.19123(17) 0.13097(17) 0.0547(6) Uani 1 1 d . . . F2 F 0.61106(17) 0.17037(15) 0.24524(17) 0.0439(5) Uani 1 1 d . . . F3 F 0.79211(17) 0.00833(14) 0.14830(13) 0.0319(4) Uani 1 1 d . . . F4 F 0.8149(2) 0.0741(2) 0.28804(17) 0.0713(7) Uani 1 1 d . . . B1 B 0.7548(3) 0.1100(3) 0.2054(2) 0.0231(6) Uani 1 1 d . . . Cl1 Cl -0.00183(16) 0.04539(17) 0.44870(13) 0.0466(4) Uani 0.50 1 d P . . Cl2 Cl 0.10516(16) 0.20385(16) 0.49489(12) 0.0404(4) Uani 0.50 1 d P . . C28 C 0.0180(6) 0.1048(6) 0.5521(4) 0.0362(14) Uani 0.50 1 d P . . H28A H -0.0758 0.1508 0.6037 0.043 Uiso 0.50 1 calc PR . . H28B H 0.0719 0.0351 0.5950 0.043 Uiso 0.50 1 calc PR . . 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 0.01418(5) 0.01288(4) 0.01269(4) 0.00036(3) -0.00504(3) -0.00659(3) N1 0.0191(10) 0.0137(9) 0.0163(9) 0.0003(7) -0.0071(8) -0.0066(8) N2 0.0214(11) 0.0183(10) 0.0173(10) -0.0024(8) -0.0039(8) -0.0114(9) N3 0.0170(10) 0.0137(9) 0.0181(9) 0.0012(7) -0.0080(8) -0.0065(8) N4 0.0170(10) 0.0167(10) 0.0239(10) 0.0027(8) -0.0111(8) -0.0070(8) N5 0.0201(11) 0.0169(10) 0.0260(11) 0.0038(8) -0.0131(9) -0.0076(9) C1 0.0147(12) 0.0210(12) 0.0160(11) 0.0030(9) -0.0063(9) -0.0096(10) C2 0.0180(12) 0.0220(12) 0.0203(12) 0.0040(9) -0.0090(10) -0.0103(10) C3 0.0288(15) 0.0270(14) 0.0329(14) 0.0114(11) -0.0179(12) -0.0134(12) C4 0.0348(16) 0.0469(18) 0.0276(14) 0.0138(12) -0.0214(12) -0.0236(14) C5 0.0382(17) 0.0464(17) 0.0205(13) 0.0058(12) -0.0153(12) -0.0285(14) C6 0.0262(14) 0.0324(14) 0.0184(12) 0.0019(10) -0.0090(10) -0.0186(12) C7 0.0237(13) 0.0151(11) 0.0234(12) 0.0039(9) -0.0110(10) -0.0074(10) C8 0.0185(13) 0.0221(13) 0.0241(13) -0.0058(10) -0.0014(10) -0.0060(10) C9 0.0262(13) 0.0175(12) 0.0234(12) -0.0026(9) -0.0115(10) -0.0090(10) C10 0.0383(16) 0.0301(14) 0.0235(13) -0.0022(11) -0.0141(11) -0.0205(13) C11 0.0260(15) 0.0296(15) 0.0319(15) -0.0151(12) 0.0070(12) -0.0118(12) C12 0.0426(17) 0.0153(12) 0.0276(13) -0.0005(10) -0.0099(12) -0.0159(12) C13 0.0268(14) 0.0171(12) 0.0226(12) 0.0044(9) -0.0129(10) -0.0110(10) C14 0.0221(12) 0.0113(11) 0.0188(11) 0.0024(8) -0.0095(9) -0.0074(9) C15 0.0198(13) 0.0221(13) 0.0378(15) 0.0059(11) -0.0178(11) -0.0090(11) C16 0.0223(13) 0.0252(13) 0.0314(14) 0.0054(10) -0.0186(11) -0.0122(11) C17 0.0175(14) 0.0285(15) 0.060(2) -0.0013(14) -0.0122(13) -0.0087(12) C18 0.0230(15) 0.0379(17) 0.069(2) 0.0005(15) -0.0100(15) -0.0198(14) C19 0.0372(17) 0.0286(15) 0.0521(18) 0.0031(13) -0.0235(14) -0.0209(14) C20 0.0379(16) 0.0276(14) 0.0294(14) -0.0035(11) -0.0137(12) -0.0151(13) C21 0.0321(15) 0.0308(14) 0.0227(13) 0.0002(11) -0.0097(11) -0.0172(12) C22 0.0220(13) 0.0101(10) 0.0198(11) 0.0027(8) -0.0067(9) -0.0077(9) C23 0.0312(15) 0.0262(14) 0.0221(12) 0.0042(10) -0.0126(11) -0.0134(12) C24 0.0329(15) 0.0285(14) 0.0197(13) 0.0056(10) -0.0048(11) -0.0123(12) C25 0.0239(14) 0.0201(13) 0.0280(13) 0.0005(10) -0.0001(11) -0.0103(11) C26 0.0216(13) 0.0233(13) 0.0306(14) -0.0047(11) -0.0076(11) -0.0088(11) C27 0.0232(13) 0.0222(12) 0.0181(11) -0.0006(9) -0.0060(10) -0.0110(11) F1 0.0498(12) 0.0359(10) 0.0702(14) -0.0104(9) 0.0082(10) -0.0283(9) F2 0.0192(8) 0.0249(9) 0.0750(13) -0.0033(8) -0.0032(8) -0.0069(7) F3 0.0395(10) 0.0198(8) 0.0415(9) -0.0047(7) -0.0213(8) -0.0081(7) F4 0.0707(15) 0.0777(16) 0.0441(12) -0.0270(11) -0.0381(11) 0.0141(12) B1 0.0219(15) 0.0223(14) 0.0259(14) -0.0047(11) -0.0097(12) -0.0065(12) Cl1 0.0288(8) 0.0681(11) 0.0448(9) -0.0169(8) -0.0025(7) -0.0223(8) Cl2 0.0300(8) 0.0544(10) 0.0369(8) -0.0108(7) -0.0136(6) -0.0112(7) C28 0.020(3) 0.054(4) 0.022(3) -0.004(3) -0.009(2) -0.003(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 Pt1 C1 1.923(2) . ? Pt1 N2 2.0778(19) . ? Pt1 N1 2.0822(19) . ? Pt1 N3 2.1449(19) . ? N1 C9 1.488(3) . ? N1 C8 1.491(3) . ? N1 C7 1.524(3) . ? N2 C12 1.482(3) . ? N2 C11 1.488(3) . ? N2 C10 1.521(3) . ? N3 N4 1.324(3) . ? N3 C14 1.367(3) . ? N4 N5 1.337(3) . ? N5 C13 1.340(3) . ? N5 C15 1.469(3) . ? C1 C2 1.385(3) . ? C1 C6 1.385(3) . ? C2 C3 1.391(3) . ? C2 C7 1.509(3) . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.391(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C10 1.503(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.375(3) . ? C13 H13 0.9500 . ? C14 C22 1.472(3) . ? C15 C16 1.513(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.382(4) . ? C16 C21 1.390(4) . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 C19 1.376(4) . ? C18 H18 0.9500 . ? C19 C20 1.377(4) . ? C19 H19 0.9500 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.391(3) . ? C22 C23 1.399(3) . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.381(4) . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 H25 0.9500 . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? F1 B1 1.392(3) . ? F2 B1 1.375(3) . ? F3 B1 1.386(3) . ? F4 B1 1.365(3) . ? Cl1 Cl1 1.541(4) 2_556 ? Cl1 C28 1.764(6) . ? Cl1 C28 1.900(7) 2_556 ? Cl2 C28 1.754(7) . ? C28 H28A 0.9900 . ? C28 H28B 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 C1 Pt1 N2 82.02(9) . . ? C1 Pt1 N1 82.11(9) . . ? N2 Pt1 N1 164.13(7) . . ? C1 Pt1 N3 175.29(8) . . ? N2 Pt1 N3 98.48(8) . . ? N1 Pt1 N3 97.31(7) . . ? C9 N1 C8 108.65(18) . . ? C9 N1 C7 108.38(18) . . ? C8 N1 C7 108.44(18) . . ? C9 N1 Pt1 114.51(14) . . ? C8 N1 Pt1 109.55(14) . . ? C7 N1 Pt1 107.14(13) . . ? C12 N2 C11 108.6(2) . . ? C12 N2 C10 109.13(19) . . ? C11 N2 C10 108.6(2) . . ? C12 N2 Pt1 114.04(15) . . ? C11 N2 Pt1 107.88(15) . . ? C10 N2 Pt1 108.47(15) . . ? N4 N3 C14 110.31(19) . . ? N4 N3 Pt1 113.10(14) . . ? C14 N3 Pt1 135.82(16) . . ? N3 N4 N5 105.86(18) . . ? N4 N5 C13 111.8(2) . . ? N4 N5 C15 119.3(2) . . ? C13 N5 C15 128.6(2) . . ? C2 C1 C6 122.6(2) . . ? C2 C1 Pt1 118.44(17) . . ? C6 C1 Pt1 118.95(18) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 C7 113.5(2) . . ? C3 C2 C7 127.8(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 121.7(2) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C1 C6 C5 118.8(2) . . ? C1 C6 C10 113.7(2) . . ? C5 C6 C10 127.4(2) . . ? C2 C7 N1 109.13(19) . . ? C2 C7 H7A 109.9 . . ? N1 C7 H7A 109.9 . . ? C2 C7 H7B 109.9 . . ? N1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 109.65(19) . . ? C6 C10 H10A 109.7 . . ? N2 C10 H10A 109.7 . . ? C6 C10 H10B 109.7 . . ? N2 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 105.7(2) . . ? N5 C13 H13 127.2 . . ? C14 C13 H13 127.2 . . ? N3 C14 C13 106.4(2) . . ? N3 C14 C22 125.8(2) . . ? C13 C14 C22 127.8(2) . . ? N5 C15 C16 110.5(2) . . ? N5 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N5 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C21 118.8(2) . . ? C17 C16 C15 119.9(2) . . ? C21 C16 C15 121.3(2) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.5(3) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C27 C22 C23 118.5(2) . . ? C27 C22 C14 122.9(2) . . ? C23 C22 C14 118.6(2) . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.7(2) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.5(2) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 120.2(3) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.7(2) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? F4 B1 F2 111.9(2) . . ? F4 B1 F3 110.2(2) . . ? F2 B1 F3 110.3(2) . . ? F4 B1 F1 108.3(3) . . ? F2 B1 F1 108.3(2) . . ? F3 B1 F1 107.7(2) . . ? Cl1 Cl1 C28 69.8(2) 2_556 . ? Cl1 Cl1 C28 60.6(2) 2_556 2_556 ? C28 Cl1 C28 130.4(2) . 2_556 ? Cl2 C28 Cl1 111.6(3) . . ? Cl2 C28 H28A 109.3 . . ? Cl1 C28 H28A 109.3 . . ? Cl2 C28 H28B 109.3 . . ? Cl1 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? 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 C1 Pt1 N1 C9 145.17(17) . . . . ? N2 Pt1 N1 C9 144.3(3) . . . . ? N3 Pt1 N1 C9 -30.12(16) . . . . ? C1 Pt1 N1 C8 -92.49(16) . . . . ? N2 Pt1 N1 C8 -93.4(3) . . . . ? N3 Pt1 N1 C8 92.22(15) . . . . ? C1 Pt1 N1 C7 24.95(15) . . . . ? N2 Pt1 N1 C7 24.1(4) . . . . ? N3 Pt1 N1 C7 -150.34(14) . . . . ? C1 Pt1 N2 C12 143.31(19) . . . . ? N1 Pt1 N2 C12 144.2(3) . . . . ? N3 Pt1 N2 C12 -41.42(18) . . . . ? C1 Pt1 N2 C11 -95.92(18) . . . . ? N1 Pt1 N2 C11 -95.0(3) . . . . ? N3 Pt1 N2 C11 79.36(17) . . . . ? C1 Pt1 N2 C10 21.49(15) . . . . ? N1 Pt1 N2 C10 22.4(4) . . . . ? N3 Pt1 N2 C10 -163.24(15) . . . . ? N2 Pt1 N3 N4 -85.05(16) . . . . ? N1 Pt1 N3 N4 93.41(16) . . . . ? N2 Pt1 N3 C14 106.3(2) . . . . ? N1 Pt1 N3 C14 -75.3(2) . . . . ? C14 N3 N4 N5 0.3(2) . . . . ? Pt1 N3 N4 N5 -171.28(14) . . . . ? N3 N4 N5 C13 -0.3(3) . . . . ? N3 N4 N5 C15 173.8(2) . . . . ? N2 Pt1 C1 C2 167.3(2) . . . . ? N1 Pt1 C1 C2 -12.43(18) . . . . ? N2 Pt1 C1 C6 -10.40(19) . . . . ? N1 Pt1 C1 C6 169.8(2) . . . . ? C6 C1 C2 C3 -2.2(4) . . . . ? Pt1 C1 C2 C3 -179.90(19) . . . . ? C6 C1 C2 C7 173.5(2) . . . . ? Pt1 C1 C2 C7 -4.1(3) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C7 C2 C3 C4 -173.8(3) . . . . ? C2 C3 C4 C5 0.4(4) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C2 C1 C6 C5 1.3(4) . . . . ? Pt1 C1 C6 C5 178.97(19) . . . . ? C2 C1 C6 C10 178.4(2) . . . . ? Pt1 C1 C6 C10 -4.0(3) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C4 C5 C6 C10 -176.1(3) . . . . ? C1 C2 C7 N1 25.3(3) . . . . ? C3 C2 C7 N1 -159.4(2) . . . . ? C9 N1 C7 C2 -156.87(19) . . . . ? C8 N1 C7 C2 85.4(2) . . . . ? Pt1 N1 C7 C2 -32.8(2) . . . . ? C1 C6 C10 N2 22.1(3) . . . . ? C5 C6 C10 N2 -161.2(2) . . . . ? C12 N2 C10 C6 -153.3(2) . . . . ? C11 N2 C10 C6 88.4(2) . . . . ? Pt1 N2 C10 C6 -28.5(2) . . . . ? N4 N5 C13 C14 0.1(3) . . . . ? C15 N5 C13 C14 -173.3(2) . . . . ? N4 N3 C14 C13 -0.3(3) . . . . ? Pt1 N3 C14 C13 168.63(17) . . . . ? N4 N3 C14 C22 179.8(2) . . . . ? Pt1 N3 C14 C22 -11.3(4) . . . . ? N5 C13 C14 N3 0.1(3) . . . . ? N5 C13 C14 C22 -180.0(2) . . . . ? N4 N5 C15 C16 -61.9(3) . . . . ? C13 N5 C15 C16 111.0(3) . . . . ? N5 C15 C16 C17 140.6(3) . . . . ? N5 C15 C16 C21 -39.4(3) . . . . ? C21 C16 C17 C18 0.8(4) . . . . ? C15 C16 C17 C18 -179.2(3) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C20 -0.4(5) . . . . ? C18 C19 C20 C21 0.1(4) . . . . ? C19 C20 C21 C16 0.7(4) . . . . ? C17 C16 C21 C20 -1.1(4) . . . . ? C15 C16 C21 C20 178.9(2) . . . . ? N3 C14 C22 C27 -14.9(4) . . . . ? C13 C14 C22 C27 165.1(2) . . . . ? N3 C14 C22 C23 166.3(2) . . . . ? C13 C14 C22 C23 -13.7(4) . . . . ? C27 C22 C23 C24 -2.0(4) . . . . ? C14 C22 C23 C24 176.9(2) . . . . ? C22 C23 C24 C25 1.0(4) . . . . ? C23 C24 C25 C26 0.4(4) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C25 C26 C27 C22 -0.2(4) . . . . ? C23 C22 C27 C26 1.6(4) . . . . ? C14 C22 C27 C26 -177.2(2) . . . . ? Cl1 Cl1 C28 Cl2 152.9(4) 2_556 . . . ? C28 Cl1 C28 Cl2 152.9(4) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.213 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.086 #===END data_s3680a _database_code_depnum_ccdc_archive 'CCDC 624058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N5 Pt, B F4' _chemical_formula_sum 'C28 H34 B F4 N5 Pt' _chemical_formula_weight 722.50 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5401(5) _cell_length_b 10.8373(5) _cell_length_c 13.5859(5) _cell_angle_alpha 90.459(2) _cell_angle_beta 112.708(2) _cell_angle_gamma 99.581(2) _cell_volume 1407.14(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34132 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 5.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.27 _exptl_absorpt_correction_T_max 0.40 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49444 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0118 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6453 _reflns_number_gt 6174 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _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^)+(0.0131P)^2^+0.6281P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6453 _refine_ls_number_parameters 393 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0132 _refine_ls_R_factor_gt 0.0117 _refine_ls_wR_factor_ref 0.0276 _refine_ls_wR_factor_gt 0.0272 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.005 _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 Pt1 Pt 0.704918(6) 0.427524(6) 0.394500(5) 0.01566(2) Uani 1 1 d . . . N1 N 0.60436(14) 0.27750(13) 0.44864(12) 0.0202(3) Uani 1 1 d . . . N2 N 0.81550(15) 0.60343(13) 0.38376(12) 0.0199(3) Uani 1 1 d . . . N3 N 0.66131(15) 0.33122(14) 0.24375(11) 0.0209(3) Uani 1 1 d . . . N4 N 0.72493(16) 0.23673(14) 0.24037(12) 0.0249(3) Uani 1 1 d . . . N5 N 0.66874(15) 0.19019(14) 0.13832(12) 0.0243(3) Uani 1 1 d . . . C1 C 0.74895(17) 0.50230(15) 0.53565(13) 0.0181(3) Uani 1 1 d . . . C2 C 0.68380(18) 0.44090(16) 0.59809(14) 0.0209(3) Uani 1 1 d . . . C3 C 0.7233(2) 0.48871(18) 0.70313(15) 0.0269(4) Uani 1 1 d . . . H3 H 0.6827 0.4471 0.7481 0.032 Uiso 1 1 calc R . . C4 C 0.8232(2) 0.59844(18) 0.74152(14) 0.0286(4) Uani 1 1 d . . . H4 H 0.8479 0.6324 0.8125 0.034 Uiso 1 1 calc R . . C5 C 0.88787(19) 0.65979(17) 0.67839(15) 0.0264(4) Uani 1 1 d . . . H5 H 0.9560 0.7343 0.7061 0.032 Uiso 1 1 calc R . . C6 C 0.85091(17) 0.61005(16) 0.57425(14) 0.0203(3) Uani 1 1 d . . . C7 C 0.57205(18) 0.33003(17) 0.53876(14) 0.0237(4) Uani 1 1 d . . . H7A H 0.4798 0.3562 0.5089 0.028 Uiso 1 1 calc R . . H7B H 0.5684 0.2645 0.5885 0.028 Uiso 1 1 calc R . . C8 C 0.7012(2) 0.18767(17) 0.49241(16) 0.0279(4) Uani 1 1 d . . . H8A H 0.6547 0.1167 0.5178 0.042 Uiso 1 1 calc R . . H8B H 0.7855 0.2302 0.5521 0.042 Uiso 1 1 calc R . . H8C H 0.7274 0.1569 0.4361 0.042 Uiso 1 1 calc R . . C9 C 0.47118(19) 0.20745(18) 0.36602(16) 0.0309(4) Uani 1 1 d . . . H9A H 0.4911 0.1660 0.3106 0.046 Uiso 1 1 calc R . . H9B H 0.4080 0.2661 0.3335 0.046 Uiso 1 1 calc R . . H9C H 0.4268 0.1441 0.3996 0.046 Uiso 1 1 calc R . . C10 C 0.91706(18) 0.65320(17) 0.49669(14) 0.0232(4) Uani 1 1 d . . . H10A H 1.0055 0.6214 0.5146 0.028 Uiso 1 1 calc R . . H10B H 0.9387 0.7461 0.5015 0.028 Uiso 1 1 calc R . . C11 C 0.71514(19) 0.69137(17) 0.34335(15) 0.0256(4) Uani 1 1 d . . . H11A H 0.7662 0.7746 0.3403 0.038 Uiso 1 1 calc R . . H11B H 0.6669 0.6974 0.3916 0.038 Uiso 1 1 calc R . . H11C H 0.6463 0.6599 0.2715 0.038 Uiso 1 1 calc R . . C12 C 0.8938(2) 0.60293(18) 0.31325(16) 0.0284(4) Uani 1 1 d . . . H12A H 0.8280 0.5744 0.2399 0.043 Uiso 1 1 calc R . . H12B H 0.9609 0.5461 0.3389 0.043 Uiso 1 1 calc R . . H12C H 0.9439 0.6880 0.3145 0.043 Uiso 1 1 calc R . . C13 C 0.56959(19) 0.25219(17) 0.07719(14) 0.0240(4) Uani 1 1 d . . . H13 H 0.5147 0.2361 0.0026 0.029 Uiso 1 1 calc R . . C14 C 0.56436(17) 0.34328(16) 0.14493(13) 0.0206(3) Uani 1 1 d . . . C15 C 0.47806(19) 0.44316(17) 0.12748(14) 0.0252(4) Uani 1 1 d . . . H15A H 0.5239 0.5160 0.1021 0.030 Uiso 1 1 calc R . . H15B H 0.4795 0.4709 0.1976 0.030 Uiso 1 1 calc R . . C16 C 0.32653(18) 0.40935(17) 0.04938(14) 0.0229(4) Uani 1 1 d . . . C17 C 0.2545(2) 0.28730(19) 0.01514(16) 0.0302(4) Uani 1 1 d . . . H17 H 0.3015 0.2189 0.0390 0.036 Uiso 1 1 calc R . . C18 C 0.1139(2) 0.2644(2) -0.05394(17) 0.0354(5) Uani 1 1 d . . . H18 H 0.0660 0.1804 -0.0772 0.042 Uiso 1 1 calc R . . C19 C 0.0435(2) 0.3626(2) -0.08895(16) 0.0356(5) Uani 1 1 d . . . H19 H -0.0526 0.3465 -0.1359 0.043 Uiso 1 1 calc R . . C20 C 0.1141(2) 0.4843(2) -0.05501(16) 0.0327(4) Uani 1 1 d . . . H20 H 0.0665 0.5524 -0.0790 0.039 Uiso 1 1 calc R . . C21 C 0.2536(2) 0.50763(18) 0.01366(14) 0.0263(4) Uani 1 1 d . . . H21 H 0.3007 0.5918 0.0370 0.032 Uiso 1 1 calc R . . C22 C 0.6991(2) 0.07164(19) 0.10518(17) 0.0326(4) Uani 1 1 d . . . H22A H 0.6770 0.0688 0.0273 0.039 Uiso 1 1 calc R . . H22B H 0.6369 0.0001 0.1179 0.039 Uiso 1 1 calc R . . C23 C 0.84862(19) 0.05587(17) 0.16314(16) 0.0265(4) Uani 1 1 d . . . C24 C 0.8900(2) 0.00752(18) 0.26234(18) 0.0353(5) Uani 1 1 d . . . H24 H 0.8256 -0.0104 0.2959 0.042 Uiso 1 1 calc R . . C25 C 1.0251(3) -0.0149(2) 0.3129(2) 0.0450(6) Uani 1 1 d . . . H25 H 1.0530 -0.0472 0.3813 0.054 Uiso 1 1 calc R . . C26 C 1.1191(2) 0.0094(2) 0.2648(2) 0.0453(6) Uani 1 1 d . . . H26 H 1.2109 -0.0079 0.2992 0.054 Uiso 1 1 calc R . . C27 C 1.0796(2) 0.0588(2) 0.1669(2) 0.0415(5) Uani 1 1 d . . . H27 H 1.1446 0.0766 0.1339 0.050 Uiso 1 1 calc R . . C28 C 0.9445(2) 0.08274(19) 0.11572(17) 0.0328(4) Uani 1 1 d . . . H28 H 0.9179 0.1175 0.0483 0.039 Uiso 1 1 calc R . . F1A F 0.5892(10) 0.0004(6) 0.8399(7) 0.042(2) Uani 0.515(11) 1 d PDU A 1 F2A F 0.4894(7) 0.1709(8) 0.8291(6) 0.0514(15) Uani 0.515(11) 1 d PDU A 1 F3A F 0.5145(13) 0.0917(5) 0.6855(4) 0.110(3) Uani 0.515(11) 1 d PDU A 1 F4A F 0.7019(5) 0.1892(5) 0.8280(11) 0.135(4) Uani 0.515(11) 1 d PDU A 1 F1B F 0.6026(11) 0.0096(7) 0.8434(8) 0.048(3) Uani 0.485(11) 1 d PDU A 2 F2B F 0.5345(8) 0.1971(8) 0.8451(6) 0.0521(16) Uani 0.485(11) 1 d PDU A 2 F3B F 0.4461(6) 0.0722(6) 0.6938(4) 0.0644(18) Uani 0.485(11) 1 d PDU A 2 F4B F 0.6694(6) 0.1663(7) 0.7563(6) 0.083(2) Uani 0.485(11) 1 d PDU A 2 B1 B 0.5692(2) 0.1134(2) 0.79015(18) 0.0326(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01491(3) 0.01530(3) 0.01618(3) 0.00052(2) 0.00553(2) 0.00269(2) N1 0.0168(7) 0.0177(7) 0.0237(7) 0.0022(6) 0.0059(6) 0.0019(5) N2 0.0199(7) 0.0179(7) 0.0237(7) 0.0026(6) 0.0107(6) 0.0027(5) N3 0.0205(7) 0.0211(7) 0.0208(7) -0.0009(6) 0.0079(6) 0.0041(6) N4 0.0237(7) 0.0254(8) 0.0237(8) -0.0050(6) 0.0063(6) 0.0076(6) N5 0.0208(7) 0.0258(8) 0.0249(8) -0.0055(6) 0.0078(6) 0.0041(6) C1 0.0182(8) 0.0192(8) 0.0173(8) 0.0008(6) 0.0061(6) 0.0066(6) C2 0.0221(8) 0.0217(8) 0.0216(8) 0.0045(7) 0.0100(7) 0.0081(7) C3 0.0343(10) 0.0314(10) 0.0227(9) 0.0069(7) 0.0158(8) 0.0149(8) C4 0.0361(10) 0.0312(10) 0.0189(8) -0.0019(7) 0.0079(8) 0.0148(8) C5 0.0261(9) 0.0226(9) 0.0260(9) -0.0043(7) 0.0045(7) 0.0073(7) C6 0.0199(8) 0.0180(8) 0.0220(8) 0.0001(6) 0.0065(7) 0.0050(6) C7 0.0227(9) 0.0250(9) 0.0272(9) 0.0062(7) 0.0137(7) 0.0047(7) C8 0.0285(9) 0.0205(9) 0.0352(10) 0.0074(8) 0.0113(8) 0.0085(7) C9 0.0207(9) 0.0281(10) 0.0340(10) -0.0001(8) 0.0040(8) -0.0055(7) C10 0.0192(8) 0.0202(8) 0.0269(9) -0.0012(7) 0.0073(7) -0.0008(7) C11 0.0262(9) 0.0186(8) 0.0332(10) 0.0060(7) 0.0120(8) 0.0064(7) C12 0.0301(10) 0.0299(10) 0.0319(10) 0.0047(8) 0.0198(8) 0.0045(8) C13 0.0239(9) 0.0258(9) 0.0208(8) -0.0012(7) 0.0078(7) 0.0028(7) C14 0.0198(8) 0.0219(8) 0.0189(8) 0.0008(6) 0.0068(7) 0.0023(6) C15 0.0276(9) 0.0210(9) 0.0232(9) -0.0012(7) 0.0054(7) 0.0056(7) C16 0.0245(9) 0.0267(9) 0.0188(8) 0.0011(7) 0.0096(7) 0.0058(7) C17 0.0276(10) 0.0284(10) 0.0340(10) -0.0029(8) 0.0112(8) 0.0062(8) C18 0.0281(10) 0.0392(12) 0.0369(11) -0.0104(9) 0.0140(9) -0.0015(9) C19 0.0226(9) 0.0573(14) 0.0267(10) -0.0024(9) 0.0093(8) 0.0079(9) C20 0.0308(10) 0.0463(12) 0.0283(10) 0.0102(9) 0.0147(8) 0.0186(9) C21 0.0307(10) 0.0290(9) 0.0237(9) 0.0048(7) 0.0142(8) 0.0084(8) C22 0.0269(10) 0.0295(10) 0.0369(11) -0.0143(8) 0.0076(8) 0.0056(8) C23 0.0237(9) 0.0188(8) 0.0343(10) -0.0080(7) 0.0093(8) 0.0025(7) C24 0.0386(11) 0.0225(9) 0.0443(12) 0.0039(8) 0.0172(10) 0.0024(8) C25 0.0464(13) 0.0266(11) 0.0500(14) 0.0077(10) 0.0053(11) 0.0079(9) C26 0.0263(10) 0.0265(11) 0.0675(17) -0.0102(11) 0.0020(11) 0.0044(8) C27 0.0280(10) 0.0315(11) 0.0659(16) -0.0173(11) 0.0229(11) -0.0023(8) C28 0.0350(11) 0.0278(10) 0.0366(11) -0.0091(8) 0.0166(9) 0.0022(8) F1A 0.062(4) 0.026(3) 0.035(4) 0.008(3) 0.016(3) 0.011(3) F2A 0.056(3) 0.062(4) 0.038(3) 0.005(2) 0.013(3) 0.032(3) F3A 0.268(10) 0.048(3) 0.043(2) 0.021(2) 0.083(4) 0.053(5) F4A 0.076(3) 0.051(2) 0.285(11) -0.010(5) 0.094(5) -0.024(2) F1B 0.057(4) 0.050(5) 0.039(5) 0.006(4) 0.016(3) 0.021(3) F2B 0.073(4) 0.049(3) 0.033(2) -0.0134(17) 0.013(3) 0.024(3) F3B 0.073(3) 0.054(3) 0.037(2) -0.016(2) -0.0156(19) 0.027(2) F4B 0.086(4) 0.102(5) 0.105(4) 0.067(4) 0.072(3) 0.045(3) B1 0.0434(13) 0.0252(11) 0.0373(12) 0.0054(9) 0.0234(11) 0.0095(10) _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 Pt1 C1 1.9267(16) . ? Pt1 N1 2.0870(14) . ? Pt1 N2 2.1000(14) . ? Pt1 N3 2.1388(14) . ? N1 C8 1.488(2) . ? N1 C9 1.491(2) . ? N1 C7 1.521(2) . ? N2 C12 1.486(2) . ? N2 C11 1.491(2) . ? N2 C10 1.522(2) . ? N3 N4 1.324(2) . ? N3 C14 1.361(2) . ? N4 N5 1.335(2) . ? N5 C13 1.344(2) . ? N5 C22 1.482(2) . ? C1 C6 1.390(2) . ? C1 C2 1.393(2) . ? C2 C3 1.391(2) . ? C2 C7 1.504(2) . ? C3 C4 1.394(3) . ? C3 H3 0.9500 . ? C4 C5 1.397(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 C10 1.511(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.367(2) . ? C13 H13 0.9500 . ? C14 C15 1.490(2) . ? C15 C16 1.517(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.388(3) . ? C16 C21 1.398(3) . ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 C20 1.380(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.505(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.384(3) . ? C23 C28 1.389(3) . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 C27 1.374(4) . ? C26 H26 0.9500 . ? C27 C28 1.393(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? F1A B1 1.411(5) . ? F2A B1 1.374(5) . ? F3A B1 1.313(5) . ? F4A B1 1.397(4) . ? F1B B1 1.364(5) . ? F2B B1 1.351(5) . ? F3B B1 1.443(4) . ? F4B B1 1.354(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 N1 82.24(6) . . ? C1 Pt1 N2 80.95(6) . . ? N1 Pt1 N2 163.14(6) . . ? C1 Pt1 N3 175.38(6) . . ? N1 Pt1 N3 94.61(6) . . ? N2 Pt1 N3 102.24(6) . . ? C8 N1 C9 108.41(14) . . ? C8 N1 C7 108.64(14) . . ? C9 N1 C7 108.25(14) . . ? C8 N1 Pt1 108.96(11) . . ? C9 N1 Pt1 114.94(11) . . ? C7 N1 Pt1 107.49(10) . . ? C12 N2 C11 108.21(14) . . ? C12 N2 C10 109.39(14) . . ? C11 N2 C10 107.73(13) . . ? C12 N2 Pt1 115.06(11) . . ? C11 N2 Pt1 108.85(10) . . ? C10 N2 Pt1 107.38(10) . . ? N4 N3 C14 110.40(14) . . ? N4 N3 Pt1 119.58(11) . . ? C14 N3 Pt1 129.72(11) . . ? N3 N4 N5 105.59(14) . . ? N4 N5 C13 111.75(14) . . ? N4 N5 C22 121.56(15) . . ? C13 N5 C22 125.92(15) . . ? C6 C1 C2 122.34(16) . . ? C6 C1 Pt1 119.17(12) . . ? C2 C1 Pt1 118.34(13) . . ? C3 C2 C1 118.72(17) . . ? C3 C2 C7 127.82(16) . . ? C1 C2 C7 113.42(15) . . ? C2 C3 C4 119.19(17) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 121.79(17) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 118.94(17) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C1 C6 C5 118.97(16) . . ? C1 C6 C10 113.22(15) . . ? C5 C6 C10 127.62(16) . . ? C2 C7 N1 109.41(13) . . ? C2 C7 H7A 109.8 . . ? N1 C7 H7A 109.8 . . ? C2 C7 H7B 109.8 . . ? N1 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 N2 108.84(13) . . ? C6 C10 H10A 109.9 . . ? N2 C10 H10A 109.9 . . ? C6 C10 H10B 109.9 . . ? N2 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 105.46(15) . . ? N5 C13 H13 127.3 . . ? C14 C13 H13 127.3 . . ? N3 C14 C13 106.79(15) . . ? N3 C14 C15 120.86(15) . . ? C13 C14 C15 132.35(16) . . ? C14 C15 C16 117.10(15) . . ? C14 C15 H15A 108.0 . . ? C16 C15 H15A 108.0 . . ? C14 C15 H15B 108.0 . . ? C16 C15 H15B 108.0 . . ? H15A C15 H15B 107.3 . . ? C17 C16 C21 118.18(17) . . ? C17 C16 C15 124.16(17) . . ? C21 C16 C15 117.59(16) . . ? C16 C17 C18 120.49(19) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.6(2) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.29(19) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.35(19) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 121.06(19) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? N5 C22 C23 113.79(15) . . ? N5 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N5 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C28 119.17(19) . . ? C24 C23 C22 119.96(18) . . ? C28 C23 C22 120.77(19) . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 119.7(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 120.1(2) . . ? C23 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? F2B B1 F4B 112.7(4) . . ? F2B B1 F1B 113.2(5) . . ? F4B B1 F1B 111.7(5) . . ? F3A B1 F2A 113.6(4) . . ? F3A B1 F4A 112.6(4) . . ? F2A B1 F4A 106.6(3) . . ? F3A B1 F1A 110.5(4) . . ? F2A B1 F1A 107.9(4) . . ? F4A B1 F1A 105.1(5) . . ? F2B B1 F3B 106.0(4) . . ? F4B B1 F3B 105.3(3) . . ? F1B B1 F3B 107.3(4) . . ? 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 C1 Pt1 N1 C8 -94.58(12) . . . . ? N2 Pt1 N1 C8 -99.1(2) . . . . ? N3 Pt1 N1 C8 82.01(12) . . . . ? C1 Pt1 N1 C9 143.55(13) . . . . ? N2 Pt1 N1 C9 139.00(18) . . . . ? N3 Pt1 N1 C9 -39.86(13) . . . . ? C1 Pt1 N1 C7 22.97(11) . . . . ? N2 Pt1 N1 C7 18.4(2) . . . . ? N3 Pt1 N1 C7 -160.43(10) . . . . ? C1 Pt1 N2 C12 148.86(13) . . . . ? N1 Pt1 N2 C12 153.43(17) . . . . ? N3 Pt1 N2 C12 -27.74(13) . . . . ? C1 Pt1 N2 C11 -89.53(12) . . . . ? N1 Pt1 N2 C11 -85.0(2) . . . . ? N3 Pt1 N2 C11 93.87(11) . . . . ? C1 Pt1 N2 C10 26.83(10) . . . . ? N1 Pt1 N2 C10 31.4(2) . . . . ? N3 Pt1 N2 C10 -149.77(10) . . . . ? N1 Pt1 N3 N4 -69.79(13) . . . . ? N2 Pt1 N3 N4 110.54(13) . . . . ? N1 Pt1 N3 C14 103.33(15) . . . . ? N2 Pt1 N3 C14 -76.33(15) . . . . ? C14 N3 N4 N5 0.80(19) . . . . ? Pt1 N3 N4 N5 175.17(11) . . . . ? N3 N4 N5 C13 -0.8(2) . . . . ? N3 N4 N5 C22 -171.34(16) . . . . ? N1 Pt1 C1 C6 166.18(14) . . . . ? N2 Pt1 C1 C6 -15.16(13) . . . . ? N1 Pt1 C1 C2 -9.42(13) . . . . ? N2 Pt1 C1 C2 169.25(14) . . . . ? C6 C1 C2 C3 -0.6(2) . . . . ? Pt1 C1 C2 C3 174.86(13) . . . . ? C6 C1 C2 C7 177.24(15) . . . . ? Pt1 C1 C2 C7 -7.31(19) . . . . ? C1 C2 C3 C4 2.1(3) . . . . ? C7 C2 C3 C4 -175.42(17) . . . . ? C2 C3 C4 C5 -1.9(3) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C2 C1 C6 C5 -1.1(2) . . . . ? Pt1 C1 C6 C5 -176.48(13) . . . . ? C2 C1 C6 C10 174.32(15) . . . . ? Pt1 C1 C6 C10 -1.09(19) . . . . ? C4 C5 C6 C1 1.2(2) . . . . ? C4 C5 C6 C10 -173.44(17) . . . . ? C3 C2 C7 N1 -155.78(17) . . . . ? C1 C2 C7 N1 26.6(2) . . . . ? C8 N1 C7 C2 85.72(16) . . . . ? C9 N1 C7 C2 -156.75(14) . . . . ? Pt1 N1 C7 C2 -32.04(15) . . . . ? C1 C6 C10 N2 24.07(19) . . . . ? C5 C6 C10 N2 -161.03(16) . . . . ? C12 N2 C10 C6 -159.26(14) . . . . ? C11 N2 C10 C6 83.34(16) . . . . ? Pt1 N2 C10 C6 -33.76(15) . . . . ? N4 N5 C13 C14 0.4(2) . . . . ? C22 N5 C13 C14 170.51(17) . . . . ? N4 N3 C14 C13 -0.5(2) . . . . ? Pt1 N3 C14 C13 -174.17(12) . . . . ? N4 N3 C14 C15 179.92(16) . . . . ? Pt1 N3 C14 C15 6.3(2) . . . . ? N5 C13 C14 N3 0.1(2) . . . . ? N5 C13 C14 C15 179.52(18) . . . . ? N3 C14 C15 C16 -142.37(17) . . . . ? C13 C14 C15 C16 38.2(3) . . . . ? C14 C15 C16 C17 17.2(3) . . . . ? C14 C15 C16 C21 -165.77(16) . . . . ? C21 C16 C17 C18 0.8(3) . . . . ? C15 C16 C17 C18 177.76(18) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C18 C19 C20 C21 -0.3(3) . . . . ? C19 C20 C21 C16 0.6(3) . . . . ? C17 C16 C21 C20 -0.8(3) . . . . ? C15 C16 C21 C20 -178.04(17) . . . . ? N4 N5 C22 C23 -38.7(3) . . . . ? C13 N5 C22 C23 152.14(18) . . . . ? N5 C22 C23 C24 84.2(2) . . . . ? N5 C22 C23 C28 -99.4(2) . . . . ? C28 C23 C24 C25 -0.7(3) . . . . ? C22 C23 C24 C25 175.78(18) . . . . ? C23 C24 C25 C26 -0.7(3) . . . . ? C24 C25 C26 C27 1.4(3) . . . . ? C25 C26 C27 C28 -0.8(3) . . . . ? C24 C23 C28 C27 1.2(3) . . . . ? C22 C23 C28 C27 -175.17(17) . . . . ? C26 C27 C28 C23 -0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.354 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.056 #===END