# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Raymond Ziessel' _publ_contact_author_address ; Laboratoire de Chimie Moleculaire d'Electronique et de Photonique Moleculaires 25 rue Becquerel Strasbourg 67087 FRANCE ; _publ_contact_author_email ZIESSEL@CHIMIE.U-STRASBG.FR _publ_section_title ; Design and Preparation of Novel Substituted Fluorene- and Carbazole based Platinum(II)-acetylide Complexes ; loop_ _publ_author_name 'Raymond Ziessel' 'Pascal Retailleau' 'Julie Batcha Seneclauze' data_jbs3942a _database_code_depnum_ccdc_archive 'CCDC 644875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H24 N2 Pt' _chemical_formula_sum 'C33 H24 N2 Pt' _chemical_formula_weight 643.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .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 monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2707(6) _cell_length_b 12.3313(10) _cell_length_c 28.699(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.684(2) _cell_angle_gamma 90.00 _cell_volume 2555.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 5.515 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31394 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 31.00 _reflns_number_total 8052 _reflns_number_gt 7626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Structure contains solvent accessible voids of 83.00 A**3. Dichloromethane, methanol, ethanol, diethyether and hexane were the solvents used for crystallization. Absence of significant residual density in the void was veryfied with PLATON/SQUEEZE. ; _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^)+(0.0254P)^2^+9.6112P] 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 8052 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.581 _refine_ls_restrained_S_all 1.581 _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 Pt1 Pt 0.75566(2) 0.814337(13) 0.037160(6) 0.01715(5) Uani 1 1 d . . . N2 N 0.7619(5) 0.9500(3) 0.00020(13) 0.0163(7) Uani 1 1 d . . . N1 N 0.6693(6) 0.9208(3) 0.08461(14) 0.0220(8) Uani 1 1 d . . . C1 C 0.8449(6) 0.7542(4) -0.02364(15) 0.0189(8) Uani 1 1 d . . . C16 C 0.7160(6) 1.0434(4) 0.02054(17) 0.0196(8) Uani 1 1 d . . . C12 C 0.8157(6) 0.9447(4) -0.04322(16) 0.0210(9) Uani 1 1 d . . . C7 C 0.6624(6) 1.0280(4) 0.06806(16) 0.0184(8) Uani 1 1 d . . . C13 C 0.8211(7) 1.0391(4) -0.06927(17) 0.0246(10) Uani 1 1 d . . . H7 H 0.8555 1.0371 -0.0995 0.030 Uiso 1 1 calc R . . C10 C 0.5578(7) 0.9832(4) 0.15557(17) 0.0246(9) Uani 1 1 d . . . H14 H 0.5221 0.9677 0.1849 0.030 Uiso 1 1 calc R . . C3 C 0.9293(7) 0.8079(5) -0.09929(17) 0.0296(11) Uani 1 1 d . . . H4 H 0.9395 0.8617 -0.1216 0.036 Uiso 1 1 calc R . . C2 C 0.8629(7) 0.8339(4) -0.05672(17) 0.0223(9) Uani 1 1 d . . . C11 C 0.6152(6) 0.9000(4) 0.12815(16) 0.0208(8) Uani 1 1 d . . . H15 H 0.6172 0.8292 0.1393 0.025 Uiso 1 1 calc R . . C8 C 0.6060(7) 1.1119(4) 0.09581(18) 0.0239(9) Uani 1 1 d . . . H12 H 0.6039 1.1830 0.0849 0.029 Uiso 1 1 calc R . . C9 C 0.5533(8) 1.0892(4) 0.13961(18) 0.0272(10) Uani 1 1 d . . . H13 H 0.5151 1.1448 0.1582 0.033 Uiso 1 1 calc R . . C15 C 0.7193(7) 1.1396(4) -0.00474(18) 0.0243(9) Uani 1 1 d . . . H9 H 0.6852 1.2049 0.0081 0.029 Uiso 1 1 calc R . . C14 C 0.7748(7) 1.1362(5) -0.04965(19) 0.0283(11) Uani 1 1 d . . . H8 H 0.7806 1.2001 -0.0666 0.034 Uiso 1 1 calc R . . C6 C 0.8951(7) 0.6506(5) -0.03299(19) 0.0288(10) Uani 1 1 d . . . H2 H 0.8855 0.5968 -0.0107 0.035 Uiso 1 1 calc R . . C5 C 0.9608(8) 0.6235(5) -0.0754(2) 0.0334(12) Uani 1 1 d . . . H3 H 0.9919 0.5521 -0.0815 0.040 Uiso 1 1 calc R . . C18 C 0.8426(6) 0.5160(4) 0.17560(16) 0.0188(8) Uani 1 1 d . . . H29 H 0.9453 0.5614 0.1794 0.023 Uiso 1 1 calc R . . C24 C 0.8269(7) 0.3302(4) 0.27663(16) 0.0200(8) Uani 1 1 d . . . C22 C 0.5594(6) 0.4543(4) 0.13031(16) 0.0198(8) Uani 1 1 d . . . H27 H 0.4753 0.4585 0.1034 0.024 Uiso 1 1 calc R . . C23 C 0.9375(7) 0.4179(4) 0.25550(16) 0.0193(8) Uani 1 1 d . . . C29 C 0.6676(7) 0.3028(3) 0.24659(16) 0.0190(8) Uani 1 1 d . . . C19 C 0.8157(6) 0.4402(4) 0.20975(15) 0.0165(7) Uani 1 1 d . . . C20 C 0.6595(6) 0.3722(3) 0.20467(15) 0.0168(8) Uani 1 1 d . . . C21 C 0.5298(6) 0.3793(4) 0.16490(16) 0.0184(8) Uani 1 1 d . . . H26 H 0.4257 0.3348 0.1616 0.022 Uiso 1 1 calc R . . C17 C 0.7144(7) 0.5240(4) 0.13525(16) 0.0186(8) Uani 1 1 d . . . C26 C 0.7459(9) 0.1957(5) 0.3311(2) 0.0342(13) Uani 1 1 d . . . H21 H 0.7705 0.1597 0.3596 0.041 Uiso 1 1 calc R . . C28 C 0.5485(7) 0.2223(4) 0.25837(19) 0.0254(10) Uani 1 1 d . . . H23 H 0.4431 0.2047 0.2382 0.031 Uiso 1 1 calc R . . C27 C 0.5895(9) 0.1682(4) 0.3009(2) 0.0327(13) Uani 1 1 d . . . H22 H 0.5117 0.1134 0.3092 0.039 Uiso 1 1 calc R . . C25 C 0.8665(8) 0.2762(4) 0.31932(17) 0.0276(10) Uani 1 1 d . . . H20 H 0.9716 0.2936 0.3396 0.033 Uiso 1 1 calc R . . C30 C 0.9611(8) 0.5197(4) 0.28661(18) 0.0274(10) Uani 1 1 d . . . H16A H 0.8417 0.5450 0.2930 0.041 Uiso 1 1 calc R . . H16B H 1.0217 0.5754 0.2707 0.041 Uiso 1 1 calc R . . H16C H 1.0346 0.5023 0.3156 0.041 Uiso 1 1 calc R . . C31 C 1.1275(7) 0.3744(4) 0.24582(18) 0.0259(10) Uani 1 1 d . . . H17A H 1.1940 0.4304 0.2317 0.039 Uiso 1 1 calc R . . H17B H 1.1106 0.3135 0.2249 0.039 Uiso 1 1 calc R . . H17C H 1.1965 0.3522 0.2748 0.039 Uiso 1 1 calc R . . C4 C 0.9790(8) 0.7034(6) -0.10819(18) 0.0345(13) Uani 1 1 d . . . H31 H 1.0249 0.6864 -0.1362 0.041 Uiso 1 1 calc R . . C2" C 0.7357(7) 0.6078(4) 0.10170(16) 0.0210(9) Uani 1 1 d . . . C1" C 0.7488(6) 0.6837(4) 0.07556(16) 0.0202(8) 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 0.01771(8) 0.01868(8) 0.01552(8) 0.00479(6) 0.00388(5) 0.00096(6) N2 0.0123(15) 0.0202(17) 0.0161(16) 0.0060(13) -0.0003(12) 0.0001(13) N1 0.0208(19) 0.0234(19) 0.0214(18) 0.0032(15) 0.0010(15) -0.0002(15) C1 0.0140(19) 0.027(2) 0.0161(18) -0.0006(16) 0.0028(15) 0.0029(16) C16 0.0135(18) 0.018(2) 0.027(2) 0.0068(16) 0.0005(16) 0.0014(15) C12 0.0129(18) 0.030(2) 0.0201(19) 0.0093(18) 0.0010(15) -0.0014(17) C7 0.0144(19) 0.0167(19) 0.022(2) 0.0021(15) -0.0043(15) -0.0021(14) C13 0.018(2) 0.034(3) 0.021(2) 0.0121(19) -0.0023(16) -0.0055(18) C10 0.022(2) 0.036(3) 0.0163(19) -0.0031(18) 0.0034(17) 0.0043(19) C3 0.021(2) 0.050(3) 0.018(2) 0.005(2) 0.0015(17) 0.001(2) C2 0.017(2) 0.030(2) 0.020(2) 0.0031(17) 0.0011(16) 0.0014(17) C11 0.020(2) 0.024(2) 0.0192(19) 0.0007(16) 0.0032(16) 0.0006(16) C8 0.021(2) 0.018(2) 0.032(2) -0.0003(18) -0.0030(18) 0.0023(16) C9 0.029(3) 0.025(2) 0.026(2) -0.0073(19) -0.0024(19) 0.0053(19) C15 0.020(2) 0.021(2) 0.030(2) 0.0080(18) -0.0061(18) -0.0053(17) C14 0.020(2) 0.033(3) 0.030(2) 0.017(2) -0.0055(18) -0.0091(19) C6 0.025(2) 0.036(3) 0.026(2) -0.003(2) 0.005(2) 0.005(2) C5 0.026(3) 0.046(3) 0.029(3) -0.009(2) 0.004(2) 0.009(2) C18 0.020(2) 0.0142(18) 0.024(2) 0.0008(15) 0.0089(16) 0.0000(15) C24 0.026(2) 0.017(2) 0.0185(19) 0.0010(15) 0.0074(16) 0.0087(16) C22 0.021(2) 0.019(2) 0.0200(19) -0.0006(16) 0.0025(16) 0.0005(16) C23 0.021(2) 0.019(2) 0.0180(19) -0.0005(15) 0.0019(16) 0.0022(16) C29 0.023(2) 0.0134(18) 0.022(2) 0.0013(15) 0.0107(16) 0.0041(15) C19 0.0177(19) 0.0155(18) 0.0172(18) -0.0008(15) 0.0057(15) 0.0006(15) C20 0.020(2) 0.0119(17) 0.0193(19) 0.0006(14) 0.0062(15) 0.0004(14) C21 0.018(2) 0.0147(18) 0.023(2) -0.0021(15) 0.0068(16) -0.0031(15) C17 0.023(2) 0.0148(18) 0.0192(19) 0.0021(15) 0.0079(16) 0.0027(15) C26 0.048(3) 0.030(3) 0.028(2) 0.014(2) 0.018(2) 0.020(2) C28 0.027(2) 0.020(2) 0.031(2) 0.0057(18) 0.014(2) 0.0043(18) C27 0.042(3) 0.021(2) 0.041(3) 0.013(2) 0.026(3) 0.008(2) C25 0.034(3) 0.031(2) 0.019(2) 0.0032(18) 0.0076(19) 0.014(2) C30 0.031(3) 0.026(2) 0.024(2) -0.0098(18) -0.0029(19) 0.0010(19) C31 0.021(2) 0.031(3) 0.025(2) -0.0048(19) 0.0033(18) 0.0059(19) C4 0.027(3) 0.058(4) 0.019(2) -0.004(2) 0.0030(19) 0.010(2) C2" 0.028(2) 0.0163(19) 0.020(2) 0.0010(16) 0.0073(17) 0.0013(17) C1" 0.022(2) 0.020(2) 0.0193(19) -0.0007(16) 0.0070(16) 0.0015(17) _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" 1.956(5) . ? Pt1 N2 1.984(4) . ? Pt1 N1 2.042(4) . ? Pt1 C1 2.068(4) . ? N2 C12 1.350(6) . ? N2 C16 1.352(6) . ? N1 C11 1.377(6) . ? N1 C7 1.404(6) . ? C1 C6 1.364(7) . ? C1 C2 1.383(7) . ? C16 C15 1.392(6) . ? C16 C7 1.473(6) . ? C12 C13 1.387(6) . ? C12 C2 1.472(7) . ? C7 C8 1.396(7) . ? C13 C14 1.381(8) . ? C13 H7 0.9300 . ? C10 C9 1.384(8) . ? C10 C11 1.387(7) . ? C10 H14 0.9300 . ? C3 C4 1.370(9) . ? C3 C2 1.402(7) . ? C3 H4 0.9300 . ? C11 H15 0.9300 . ? C8 C9 1.385(7) . ? C8 H12 0.9300 . ? C9 H13 0.9300 . ? C15 C14 1.395(8) . ? C15 H9 0.9300 . ? C14 H8 0.9300 . ? C6 C5 1.399(7) . ? C6 H2 0.9300 . ? C5 C4 1.379(9) . ? C5 H3 0.9300 . ? C18 C19 1.385(6) . ? C18 C17 1.403(7) . ? C18 H29 0.9300 . ? C24 C25 1.395(6) . ? C24 C29 1.402(7) . ? C24 C23 1.515(7) . ? C22 C21 1.392(6) . ? C22 C17 1.411(6) . ? C22 H27 0.9300 . ? C23 C19 1.521(6) . ? C23 C31 1.537(7) . ? C23 C30 1.539(7) . ? C29 C28 1.385(7) . ? C29 C20 1.472(6) . ? C19 C20 1.405(6) . ? C20 C21 1.397(6) . ? C21 H26 0.9300 . ? C17 C2" 1.434(6) . ? C26 C27 1.388(10) . ? C26 C25 1.391(8) . ? C26 H21 0.9300 . ? C28 C27 1.394(7) . ? C28 H23 0.9300 . ? C27 H22 0.9300 . ? C25 H20 0.9300 . ? C30 H16A 0.9600 . ? C30 H16B 0.9600 . ? C30 H16C 0.9600 . ? C31 H17A 0.9600 . ? C31 H17B 0.9600 . ? C31 H17C 0.9600 . ? C4 H31 0.9300 . ? C2" C1" 1.210(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 C1" Pt1 N2 178.00(17) . . ? C1" Pt1 N1 97.11(17) . . ? N2 Pt1 N1 80.95(16) . . ? C1" Pt1 C1 102.20(19) . . ? N2 Pt1 C1 79.74(17) . . ? N1 Pt1 C1 160.69(18) . . ? C12 N2 C16 123.5(4) . . ? C12 N2 Pt1 118.7(3) . . ? C16 N2 Pt1 117.8(3) . . ? C11 N1 C7 118.7(4) . . ? C11 N1 Pt1 128.9(3) . . ? C7 N1 Pt1 112.4(3) . . ? C6 C1 C2 118.8(4) . . ? C6 C1 Pt1 128.2(4) . . ? C2 C1 Pt1 112.9(3) . . ? N2 C16 C15 118.8(4) . . ? N2 C16 C7 113.3(4) . . ? C15 C16 C7 127.9(5) . . ? N2 C12 C13 119.1(5) . . ? N2 C12 C2 112.9(4) . . ? C13 C12 C2 128.0(4) . . ? C8 C7 N1 120.4(4) . . ? C8 C7 C16 124.0(4) . . ? N1 C7 C16 115.6(4) . . ? C14 C13 C12 118.9(5) . . ? C14 C13 H7 120.5 . . ? C12 C13 H7 120.5 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H14 119.7 . . ? C11 C10 H14 119.7 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H4 119.9 . . ? C2 C3 H4 119.9 . . ? C1 C2 C3 120.3(5) . . ? C1 C2 C12 115.8(4) . . ? C3 C2 C12 123.8(5) . . ? N1 C11 C10 120.9(5) . . ? N1 C11 H15 119.5 . . ? C10 C11 H15 119.5 . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H12 120.0 . . ? C7 C8 H12 120.0 . . ? C10 C9 C8 119.5(5) . . ? C10 C9 H13 120.2 . . ? C8 C9 H13 120.2 . . ? C16 C15 C14 118.7(5) . . ? C16 C15 H9 120.7 . . ? C14 C15 H9 120.7 . . ? C13 C14 C15 120.9(5) . . ? C13 C14 H8 119.5 . . ? C15 C14 H8 119.5 . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H2 119.3 . . ? C5 C6 H2 119.3 . . ? C4 C5 C6 119.5(6) . . ? C4 C5 H3 120.3 . . ? C6 C5 H3 120.3 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H29 120.1 . . ? C17 C18 H29 120.1 . . ? C25 C24 C29 119.7(5) . . ? C25 C24 C23 128.9(5) . . ? C29 C24 C23 111.4(4) . . ? C21 C22 C17 121.4(4) . . ? C21 C22 H27 119.3 . . ? C17 C22 H27 119.3 . . ? C24 C23 C19 101.1(4) . . ? C24 C23 C31 110.7(4) . . ? C19 C23 C31 110.6(4) . . ? C24 C23 C30 112.2(4) . . ? C19 C23 C30 111.5(4) . . ? C31 C23 C30 110.3(4) . . ? C28 C29 C24 121.2(4) . . ? C28 C29 C20 130.5(5) . . ? C24 C29 C20 108.3(4) . . ? C18 C19 C20 120.6(4) . . ? C18 C19 C23 128.1(4) . . ? C20 C19 C23 111.3(4) . . ? C21 C20 C19 120.6(4) . . ? C21 C20 C29 131.5(4) . . ? C19 C20 C29 107.9(4) . . ? C22 C21 C20 118.6(4) . . ? C22 C21 H26 120.7 . . ? C20 C21 H26 120.7 . . ? C18 C17 C22 119.1(4) . . ? C18 C17 C2" 119.4(4) . . ? C22 C17 C2" 121.3(4) . . ? C27 C26 C25 121.1(5) . . ? C27 C26 H21 119.4 . . ? C25 C26 H21 119.4 . . ? C29 C28 C27 118.7(5) . . ? C29 C28 H23 120.6 . . ? C27 C28 H23 120.6 . . ? C26 C27 C28 120.4(5) . . ? C26 C27 H22 119.8 . . ? C28 C27 H22 119.8 . . ? C26 C25 C24 118.8(5) . . ? C26 C25 H20 120.6 . . ? C24 C25 H20 120.6 . . ? C23 C30 H16A 109.5 . . ? C23 C30 H16B 109.5 . . ? H16A C30 H16B 109.5 . . ? C23 C30 H16C 109.5 . . ? H16A C30 H16C 109.5 . . ? H16B C30 H16C 109.5 . . ? C23 C31 H17A 109.5 . . ? C23 C31 H17B 109.5 . . ? H17A C31 H17B 109.5 . . ? C23 C31 H17C 109.5 . . ? H17A C31 H17C 109.5 . . ? H17B C31 H17C 109.5 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H31 120.1 . . ? C5 C4 H31 120.1 . . ? C1" C2" C17 175.4(5) . . ? C2" C1" Pt1 174.5(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 N2 C12 166(5) . . . . ? N1 Pt1 N2 C12 179.8(3) . . . . ? C1 Pt1 N2 C12 -0.2(3) . . . . ? C1" Pt1 N2 C16 -12(5) . . . . ? N1 Pt1 N2 C16 1.4(3) . . . . ? C1 Pt1 N2 C16 -178.6(3) . . . . ? C1" Pt1 N1 C11 -3.3(4) . . . . ? N2 Pt1 N1 C11 177.2(4) . . . . ? C1 Pt1 N1 C11 177.1(5) . . . . ? C1" Pt1 N1 C7 178.6(3) . . . . ? N2 Pt1 N1 C7 -0.9(3) . . . . ? C1 Pt1 N1 C7 -1.0(7) . . . . ? C1" Pt1 C1 C6 -3.1(5) . . . . ? N2 Pt1 C1 C6 176.4(5) . . . . ? N1 Pt1 C1 C6 176.4(5) . . . . ? C1" Pt1 C1 C2 -179.3(3) . . . . ? N2 Pt1 C1 C2 0.2(3) . . . . ? N1 Pt1 C1 C2 0.3(7) . . . . ? C12 N2 C16 C15 1.7(7) . . . . ? Pt1 N2 C16 C15 -180.0(3) . . . . ? C12 N2 C16 C7 -179.9(4) . . . . ? Pt1 N2 C16 C7 -1.5(5) . . . . ? C16 N2 C12 C13 -1.4(7) . . . . ? Pt1 N2 C12 C13 -179.8(3) . . . . ? C16 N2 C12 C2 178.4(4) . . . . ? Pt1 N2 C12 C2 0.1(5) . . . . ? C11 N1 C7 C8 1.6(6) . . . . ? Pt1 N1 C7 C8 179.9(3) . . . . ? C11 N1 C7 C16 -177.9(4) . . . . ? Pt1 N1 C7 C16 0.4(5) . . . . ? N2 C16 C7 C8 -178.8(4) . . . . ? C15 C16 C7 C8 -0.5(7) . . . . ? N2 C16 C7 N1 0.7(6) . . . . ? C15 C16 C7 N1 178.9(4) . . . . ? N2 C12 C13 C14 1.2(7) . . . . ? C2 C12 C13 C14 -178.6(5) . . . . ? C6 C1 C2 C3 0.9(7) . . . . ? Pt1 C1 C2 C3 177.4(4) . . . . ? C6 C1 C2 C12 -176.8(4) . . . . ? Pt1 C1 C2 C12 -0.3(5) . . . . ? C4 C3 C2 C1 -0.8(8) . . . . ? C4 C3 C2 C12 176.7(5) . . . . ? N2 C12 C2 C1 0.2(6) . . . . ? C13 C12 C2 C1 180.0(5) . . . . ? N2 C12 C2 C3 -177.5(4) . . . . ? C13 C12 C2 C3 2.4(8) . . . . ? C7 N1 C11 C10 -1.1(7) . . . . ? Pt1 N1 C11 C10 -179.1(4) . . . . ? C9 C10 C11 N1 0.2(7) . . . . ? N1 C7 C8 C9 -1.2(7) . . . . ? C16 C7 C8 C9 178.2(4) . . . . ? C11 C10 C9 C8 0.2(8) . . . . ? C7 C8 C9 C10 0.3(7) . . . . ? N2 C16 C15 C14 -1.7(7) . . . . ? C7 C16 C15 C14 -179.9(4) . . . . ? C12 C13 C14 C15 -1.4(7) . . . . ? C16 C15 C14 C13 1.6(7) . . . . ? C2 C1 C6 C5 -1.1(8) . . . . ? Pt1 C1 C6 C5 -177.1(4) . . . . ? C1 C6 C5 C4 1.4(9) . . . . ? C25 C24 C23 C19 -179.5(4) . . . . ? C29 C24 C23 C19 2.0(5) . . . . ? C25 C24 C23 C31 63.2(6) . . . . ? C29 C24 C23 C31 -115.2(4) . . . . ? C25 C24 C23 C30 -60.5(6) . . . . ? C29 C24 C23 C30 121.0(4) . . . . ? C25 C24 C29 C28 -0.3(7) . . . . ? C23 C24 C29 C28 178.3(4) . . . . ? C25 C24 C29 C20 179.7(4) . . . . ? C23 C24 C29 C20 -1.7(5) . . . . ? C17 C18 C19 C20 -0.9(6) . . . . ? C17 C18 C19 C23 179.5(4) . . . . ? C24 C23 C19 C18 178.0(4) . . . . ? C31 C23 C19 C18 -64.7(6) . . . . ? C30 C23 C19 C18 58.5(6) . . . . ? C24 C23 C19 C20 -1.7(5) . . . . ? C31 C23 C19 C20 115.7(4) . . . . ? C30 C23 C19 C20 -121.1(4) . . . . ? C18 C19 C20 C21 0.6(6) . . . . ? C23 C19 C20 C21 -179.8(4) . . . . ? C18 C19 C20 C29 -178.9(4) . . . . ? C23 C19 C20 C29 0.8(5) . . . . ? C28 C29 C20 C21 1.2(8) . . . . ? C24 C29 C20 C21 -178.8(4) . . . . ? C28 C29 C20 C19 -179.5(5) . . . . ? C24 C29 C20 C19 0.6(5) . . . . ? C17 C22 C21 C20 -1.4(7) . . . . ? C19 C20 C21 C22 0.6(6) . . . . ? C29 C20 C21 C22 179.9(4) . . . . ? C19 C18 C17 C22 0.1(6) . . . . ? C19 C18 C17 C2" 175.4(4) . . . . ? C21 C22 C17 C18 1.1(7) . . . . ? C21 C22 C17 C2" -174.1(4) . . . . ? C24 C29 C28 C27 -0.1(7) . . . . ? C20 C29 C28 C27 179.9(4) . . . . ? C25 C26 C27 C28 -1.1(8) . . . . ? C29 C28 C27 C26 0.8(7) . . . . ? C27 C26 C25 C24 0.7(8) . . . . ? C29 C24 C25 C26 0.0(7) . . . . ? C23 C24 C25 C26 -178.3(4) . . . . ? C2 C3 C4 C5 1.1(8) . . . . ? C6 C5 C4 C3 -1.3(9) . . . . ? C18 C17 C2" C1" -76(7) . . . . ? C22 C17 C2" C1" 99(7) . . . . ? C17 C2" C1" Pt1 -12(11) . . . . ? N2 Pt1 C1" C2" 29(8) . . . . ? N1 Pt1 C1" C2" 15(5) . . . . ? C1 Pt1 C1" C2" -165(5) . . . . ? _diffrn_measured_fraction_theta_max .987 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full .987 _refine_diff_density_max 2.223 _refine_diff_density_min -2.334 _refine_diff_density_rms .274 data_jbs032 _database_code_depnum_ccdc_archive 'CCDC 644876' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H21 N3 Pt' _chemical_formula_sum 'C31 H21 N3 Pt' _chemical_formula_weight 630.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .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 21 21 21' _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' _cell_length_a 7.301(5) _cell_length_b 12.688(5) _cell_length_c 25.728(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2383.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2340 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour ' brown' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 5.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.185 _exptl_absorpt_correction_T_max 0.495 _exptl_absorpt_process_details 'Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa-CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14854 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.43 _reflns_number_total 4276 _reflns_number_gt 3759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare, A et al, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0490P)^2^+0.8601P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(13) _refine_ls_number_reflns 4276 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Pt1 Pt 1.26254(4) 0.633037(18) 0.286316(10) 0.04622(11) Uani 1 1 d . . . N1 N 1.5194(9) 0.5684(6) 0.3077(3) 0.0554(17) Uani 1 1 d . . . N2 N 1.3198(8) 0.5421(5) 0.2253(2) 0.0484(16) Uani 1 1 d . . . N4 N 0.9330(11) 1.0253(6) 0.5495(3) 0.066(2) Uani 1 1 d . . . C1 C 1.0406(11) 0.6640(6) 0.2442(3) 0.051(2) Uani 1 1 d . . . C2 C 1.0380(10) 0.6056(6) 0.1963(3) 0.053(2) Uani 1 1 d . . . C3 C 0.8895(11) 0.6152(7) 0.1614(3) 0.064(2) Uani 1 1 d . . . H12 H 0.8910 0.5799 0.1297 0.077 Uiso 1 1 calc R . . C4 C 0.7441(14) 0.6767(7) 0.1748(4) 0.074(2) Uani 1 1 d . . . H13 H 0.6429 0.6795 0.1529 0.088 Uiso 1 1 calc R . . C5 C 0.7435(13) 0.7333(7) 0.2186(4) 0.077(3) Uani 1 1 d . . . H14 H 0.6431 0.7757 0.2262 0.093 Uiso 1 1 calc R . . C6 C 0.8897(12) 0.7300(7) 0.2531(4) 0.066(2) Uani 1 1 d . . . H15 H 0.8875 0.7723 0.2826 0.080 Uiso 1 1 calc R . . C7 C 1.5883(10) 0.4990(7) 0.2728(4) 0.056(2) Uani 1 1 d . . . C8 C 1.7507(11) 0.4485(7) 0.2802(4) 0.070(2) Uani 1 1 d . . . H2 H 1.7924 0.4006 0.2555 0.084 Uiso 1 1 calc R . . C9 C 1.8535(14) 0.4680(9) 0.3240(5) 0.090(3) Uani 1 1 d . . . H3 H 1.9628 0.4326 0.3301 0.108 Uiso 1 1 calc R . . C10 C 1.7869(13) 0.5432(8) 0.3586(4) 0.079(3) Uani 1 1 d . . . H4 H 1.8564 0.5619 0.3875 0.095 Uiso 1 1 calc R . . C11 C 1.6196(12) 0.5901(8) 0.3506(3) 0.066(2) Uani 1 1 d . . . H5 H 1.5745 0.6375 0.3750 0.079 Uiso 1 1 calc R . . C12 C 1.1952(10) 0.5399(5) 0.1864(3) 0.0500(19) Uani 1 1 d . . . C13 C 1.2290(13) 0.4730(6) 0.1445(3) 0.063(2) Uani 1 1 d . . . H9 H 1.1466 0.4702 0.1170 0.075 Uiso 1 1 calc R . . C14 C 1.3831(12) 0.4115(7) 0.1437(4) 0.068(2) Uani 1 1 d . . . H8 H 1.4041 0.3660 0.1159 0.081 Uiso 1 1 calc R . . C15 C 1.5080(11) 0.4172(7) 0.1843(4) 0.064(2) Uani 1 1 d . . . H7 H 1.6140 0.3766 0.1837 0.077 Uiso 1 1 calc R . . C16 C 1.4730(10) 0.4837(6) 0.2256(3) 0.053(2) Uani 1 1 d . . . C17 C 1.0933(11) 0.8269(6) 0.4302(3) 0.0491(19) Uani 1 1 d . . . C18 C 1.1944(10) 0.9132(6) 0.4474(3) 0.0480(18) Uani 1 1 d . . . H21 H 1.3062 0.9288 0.4318 0.058 Uiso 1 1 calc R . . C19 C 1.1306(10) 0.9753(6) 0.4869(3) 0.0468(18) Uani 1 1 d . . . C20 C 0.9656(11) 0.9507(6) 0.5116(3) 0.0504(19) Uani 1 1 d . . . C21 C 0.8642(11) 0.8646(7) 0.4968(3) 0.060(2) Uani 1 1 d . . . H18 H 0.7553 0.8480 0.5136 0.072 Uiso 1 1 calc R . . C22 C 0.9280(12) 0.8027(7) 0.4560(4) 0.062(2) Uani 1 1 d . . . H17 H 0.8604 0.7443 0.4456 0.074 Uiso 1 1 calc R . . C23 C 1.2028(12) 1.0697(6) 0.5125(3) 0.056(2) Uani 1 1 d . . . C24 C 1.3565(14) 1.1302(7) 0.5060(4) 0.076(3) Uani 1 1 d . . . H28 H 1.4424 1.1138 0.4805 0.091 Uiso 1 1 calc R . . C25 C 1.3806(19) 1.2158(9) 0.5379(6) 0.100(4) Uani 1 1 d . . . H27 H 1.4834 1.2583 0.5336 0.120 Uiso 1 1 calc R . . C26 C 1.256(2) 1.2401(8) 0.5761(5) 0.108(4) Uani 1 1 d . . . H26 H 1.2784 1.2966 0.5983 0.130 Uiso 1 1 calc R . . C27 C 1.1027(17) 1.1835(9) 0.5819(4) 0.089(3) Uani 1 1 d . . . H25 H 1.0171 1.2021 0.6070 0.107 Uiso 1 1 calc R . . C28 C 1.0723(14) 1.0967(7) 0.5500(3) 0.063(2) Uani 1 1 d . . . C29 C 0.7627(15) 1.0315(8) 0.5806(4) 0.086(3) Uani 1 1 d . . . H29A H 0.6870 0.9715 0.5730 0.129 Uiso 1 1 calc R . . H29B H 0.6979 1.0949 0.5719 0.129 Uiso 1 1 calc R . . H29C H 0.7930 1.0319 0.6169 0.129 Uiso 1 1 calc R . . C1" C 1.1919(11) 0.7168(6) 0.3477(3) 0.054(2) Uani 1 1 d . . . C2" C 1.1480(12) 0.7655(6) 0.3856(3) 0.053(2) 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 0.05191(17) 0.04296(16) 0.04378(16) -0.00424(12) 0.00571(15) -0.00335(15) N1 0.051(4) 0.056(4) 0.059(4) 0.005(4) 0.001(3) -0.007(3) N2 0.048(3) 0.045(3) 0.053(4) -0.008(3) 0.008(3) -0.003(3) N4 0.092(6) 0.059(4) 0.047(4) -0.003(3) 0.020(4) 0.020(4) C1 0.065(5) 0.042(4) 0.048(5) 0.005(4) 0.016(4) 0.004(4) C2 0.054(4) 0.048(5) 0.057(5) 0.000(4) 0.008(4) 0.000(4) C3 0.063(5) 0.071(6) 0.057(5) -0.007(5) -0.004(4) 0.003(5) C4 0.070(6) 0.076(5) 0.074(6) 0.000(5) -0.016(6) 0.008(5) C5 0.068(6) 0.063(5) 0.101(7) 0.003(5) -0.014(7) 0.028(5) C6 0.068(6) 0.057(5) 0.073(7) -0.004(5) 0.007(5) 0.004(4) C7 0.046(4) 0.057(5) 0.066(6) 0.001(4) 0.011(4) -0.011(4) C8 0.053(5) 0.071(5) 0.086(6) 0.011(4) 0.009(6) 0.002(5) C9 0.059(6) 0.100(8) 0.111(10) 0.034(8) 0.001(6) 0.001(6) C10 0.059(6) 0.097(7) 0.083(7) 0.016(6) -0.017(5) -0.031(5) C11 0.066(5) 0.081(6) 0.051(5) 0.006(5) 0.000(4) -0.017(5) C12 0.055(5) 0.044(4) 0.051(5) -0.009(3) 0.009(4) -0.013(3) C13 0.066(6) 0.066(5) 0.057(5) -0.014(4) 0.011(5) -0.011(5) C14 0.062(5) 0.070(6) 0.071(6) -0.026(5) 0.018(5) -0.012(4) C15 0.054(5) 0.055(5) 0.083(7) -0.016(5) 0.026(5) -0.003(4) C16 0.045(4) 0.053(5) 0.060(6) -0.002(4) 0.016(4) -0.008(4) C17 0.056(5) 0.047(4) 0.045(5) 0.003(4) 0.004(4) 0.010(4) C18 0.044(4) 0.056(4) 0.043(4) 0.001(3) 0.004(3) 0.004(3) C19 0.060(5) 0.051(4) 0.029(4) 0.005(3) 0.007(3) 0.006(4) C20 0.064(5) 0.047(5) 0.040(5) 0.004(4) 0.004(4) 0.010(4) C21 0.058(5) 0.067(5) 0.054(5) 0.006(5) 0.019(4) 0.001(5) C22 0.068(5) 0.052(5) 0.065(6) 0.002(4) 0.008(4) -0.006(4) C23 0.072(6) 0.051(4) 0.045(4) -0.001(4) -0.002(4) 0.003(4) C24 0.094(7) 0.055(5) 0.078(7) -0.005(6) -0.007(5) -0.007(6) C25 0.120(10) 0.075(8) 0.105(10) -0.001(7) -0.029(8) -0.020(7) C26 0.155(13) 0.073(6) 0.098(9) -0.026(6) -0.047(11) -0.004(10) C27 0.114(9) 0.088(8) 0.066(7) -0.036(6) -0.004(6) 0.028(7) C28 0.091(6) 0.050(5) 0.047(5) 0.003(4) 0.001(4) 0.012(5) C29 0.084(7) 0.103(7) 0.072(6) 0.001(5) 0.022(6) 0.032(7) C1" 0.058(5) 0.046(4) 0.057(5) 0.003(4) -0.001(4) -0.003(4) C2" 0.061(5) 0.051(5) 0.048(5) -0.004(4) 0.000(4) -0.001(4) _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" 1.973(9) . ? Pt1 C1 1.988(9) . ? Pt1 N2 1.992(6) . ? Pt1 N1 2.119(7) . ? N1 C11 1.352(10) . ? N1 C7 1.355(11) . ? N2 C16 1.342(10) . ? N2 C12 1.353(10) . ? N4 C28 1.363(12) . ? N4 C20 1.379(11) . ? N4 C29 1.480(12) . ? C1 C6 1.403(11) . ? C1 C2 1.437(12) . ? C2 C3 1.414(11) . ? C2 C12 1.442(11) . ? C3 C4 1.362(12) . ? C3 H12 0.9300 . ? C4 C5 1.337(13) . ? C4 H13 0.9300 . ? C5 C6 1.388(13) . ? C5 H14 0.9300 . ? C6 H15 0.9300 . ? C7 C8 1.361(12) . ? C7 C16 1.489(11) . ? C8 C9 1.376(13) . ? C8 H2 0.9300 . ? C9 C10 1.394(14) . ? C9 H3 0.9300 . ? C10 C11 1.375(13) . ? C10 H4 0.9300 . ? C11 H5 0.9300 . ? C12 C13 1.395(10) . ? C13 C14 1.369(12) . ? C13 H9 0.9300 . ? C14 C15 1.390(12) . ? C14 H8 0.9300 . ? C15 C16 1.380(11) . ? C15 H7 0.9300 . ? C17 C18 1.393(11) . ? C17 C22 1.411(11) . ? C17 C2" 1.444(11) . ? C18 C19 1.369(10) . ? C18 H21 0.9300 . ? C19 C20 1.397(11) . ? C19 C23 1.464(11) . ? C20 C21 1.374(11) . ? C21 C22 1.389(11) . ? C21 H18 0.9300 . ? C22 H17 0.9300 . ? C23 C24 1.371(12) . ? C23 C28 1.399(12) . ? C24 C25 1.373(14) . ? C24 H28 0.9300 . ? C25 C26 1.375(18) . ? C25 H27 0.9300 . ? C26 C27 1.337(17) . ? C26 H26 0.9300 . ? C27 C28 1.391(13) . ? C27 H25 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C1" C2" 1.197(11) . ? 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 C1 96.7(3) . . ? C1" Pt1 N2 176.2(3) . . ? C1 Pt1 N2 81.7(3) . . ? C1" Pt1 N1 103.4(3) . . ? C1 Pt1 N1 159.9(3) . . ? N2 Pt1 N1 78.1(3) . . ? C11 N1 C7 118.2(8) . . ? C11 N1 Pt1 127.7(6) . . ? C7 N1 Pt1 114.1(6) . . ? C16 N2 C12 123.5(6) . . ? C16 N2 Pt1 119.4(5) . . ? C12 N2 Pt1 117.0(5) . . ? C28 N4 C20 109.6(7) . . ? C28 N4 C29 125.9(8) . . ? C20 N4 C29 124.2(8) . . ? C6 C1 C2 115.9(8) . . ? C6 C1 Pt1 132.0(7) . . ? C2 C1 Pt1 112.1(5) . . ? C3 C2 C1 120.8(7) . . ? C3 C2 C12 123.2(8) . . ? C1 C2 C12 116.0(7) . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H12 120.5 . . ? C2 C3 H12 120.5 . . ? C5 C4 C3 121.6(9) . . ? C5 C4 H13 119.2 . . ? C3 C4 H13 119.2 . . ? C4 C5 C6 121.3(9) . . ? C4 C5 H14 119.3 . . ? C6 C5 H14 119.3 . . ? C5 C6 C1 121.2(9) . . ? C5 C6 H15 119.4 . . ? C1 C6 H15 119.4 . . ? N1 C7 C8 122.5(8) . . ? N1 C7 C16 114.5(7) . . ? C8 C7 C16 123.0(8) . . ? C7 C8 C9 120.3(9) . . ? C7 C8 H2 119.9 . . ? C9 C8 H2 119.9 . . ? C8 C9 C10 117.2(9) . . ? C8 C9 H3 121.4 . . ? C10 C9 H3 121.4 . . ? C11 C10 C9 120.7(10) . . ? C11 C10 H4 119.7 . . ? C9 C10 H4 119.7 . . ? N1 C11 C10 121.0(10) . . ? N1 C11 H5 119.5 . . ? C10 C11 H5 119.5 . . ? N2 C12 C13 117.8(7) . . ? N2 C12 C2 113.1(7) . . ? C13 C12 C2 129.0(8) . . ? C14 C13 C12 120.3(8) . . ? C14 C13 H9 119.9 . . ? C12 C13 H9 119.9 . . ? C13 C14 C15 119.9(8) . . ? C13 C14 H8 120.1 . . ? C15 C14 H8 120.1 . . ? C16 C15 C14 119.3(8) . . ? C16 C15 H7 120.4 . . ? C14 C15 H7 120.4 . . ? N2 C16 C15 119.2(8) . . ? N2 C16 C7 113.8(7) . . ? C15 C16 C7 127.0(8) . . ? C18 C17 C22 118.3(7) . . ? C18 C17 C2" 122.0(7) . . ? C22 C17 C2" 119.6(7) . . ? C19 C18 C17 120.6(7) . . ? C19 C18 H21 119.7 . . ? C17 C18 H21 119.7 . . ? C18 C19 C20 120.2(7) . . ? C18 C19 C23 133.0(7) . . ? C20 C19 C23 106.8(7) . . ? C21 C20 N4 130.5(8) . . ? C21 C20 C19 121.0(7) . . ? N4 C20 C19 108.4(7) . . ? C20 C21 C22 118.6(7) . . ? C20 C21 H18 120.7 . . ? C22 C21 H18 120.7 . . ? C21 C22 C17 121.3(8) . . ? C21 C22 H17 119.4 . . ? C17 C22 H17 119.4 . . ? C24 C23 C28 120.3(8) . . ? C24 C23 C19 134.3(8) . . ? C28 C23 C19 105.4(8) . . ? C23 C24 C25 118.3(10) . . ? C23 C24 H28 120.8 . . ? C25 C24 H28 120.8 . . ? C24 C25 C26 121.3(12) . . ? C24 C25 H27 119.3 . . ? C26 C25 H27 119.3 . . ? C27 C26 C25 120.9(10) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 119.5(10) . . ? C26 C27 H25 120.2 . . ? C28 C27 H25 120.2 . . ? N4 C28 C27 130.7(9) . . ? N4 C28 C23 109.7(8) . . ? C27 C28 C23 119.5(10) . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C2" C1" Pt1 178.5(7) . . ? C1" C2" C17 178.2(9) . . ? 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 C11 -7.1(8) . . . . ? C1 Pt1 N1 C11 174.4(8) . . . . ? N2 Pt1 N1 C11 176.5(7) . . . . ? C1" Pt1 N1 C7 174.2(5) . . . . ? C1 Pt1 N1 C7 -4.3(11) . . . . ? N2 Pt1 N1 C7 -2.2(5) . . . . ? C1" Pt1 N2 C16 -112(4) . . . . ? C1 Pt1 N2 C16 -178.2(6) . . . . ? N1 Pt1 N2 C16 2.6(5) . . . . ? C1" Pt1 N2 C12 65(4) . . . . ? C1 Pt1 N2 C12 -0.9(5) . . . . ? N1 Pt1 N2 C12 179.8(6) . . . . ? C1" Pt1 C1 C6 4.4(8) . . . . ? N2 Pt1 C1 C6 -179.1(8) . . . . ? N1 Pt1 C1 C6 -177.0(7) . . . . ? C1" Pt1 C1 C2 -174.8(5) . . . . ? N2 Pt1 C1 C2 1.7(5) . . . . ? N1 Pt1 C1 C2 3.8(12) . . . . ? C6 C1 C2 C3 -0.6(11) . . . . ? Pt1 C1 C2 C3 178.8(6) . . . . ? C6 C1 C2 C12 178.4(7) . . . . ? Pt1 C1 C2 C12 -2.3(8) . . . . ? C1 C2 C3 C4 -3.1(12) . . . . ? C12 C2 C3 C4 178.0(8) . . . . ? C2 C3 C4 C5 4.2(14) . . . . ? C3 C4 C5 C6 -1.4(15) . . . . ? C4 C5 C6 C1 -2.5(15) . . . . ? C2 C1 C6 C5 3.3(12) . . . . ? Pt1 C1 C6 C5 -175.8(7) . . . . ? C11 N1 C7 C8 2.0(12) . . . . ? Pt1 N1 C7 C8 -179.1(6) . . . . ? C11 N1 C7 C16 -177.3(7) . . . . ? Pt1 N1 C7 C16 1.6(9) . . . . ? N1 C7 C8 C9 -1.0(13) . . . . ? C16 C7 C8 C9 178.3(8) . . . . ? C7 C8 C9 C10 -2.1(14) . . . . ? C8 C9 C10 C11 4.2(14) . . . . ? C7 N1 C11 C10 0.1(12) . . . . ? Pt1 N1 C11 C10 -178.6(6) . . . . ? C9 C10 C11 N1 -3.2(13) . . . . ? C16 N2 C12 C13 -0.1(11) . . . . ? Pt1 N2 C12 C13 -177.2(5) . . . . ? C16 N2 C12 C2 177.0(6) . . . . ? Pt1 N2 C12 C2 -0.1(8) . . . . ? C3 C2 C12 N2 -179.5(7) . . . . ? C1 C2 C12 N2 1.5(10) . . . . ? C3 C2 C12 C13 -2.8(13) . . . . ? C1 C2 C12 C13 178.3(7) . . . . ? N2 C12 C13 C14 0.7(11) . . . . ? C2 C12 C13 C14 -175.9(8) . . . . ? C12 C13 C14 C15 -1.2(13) . . . . ? C13 C14 C15 C16 1.2(13) . . . . ? C12 N2 C16 C15 0.0(11) . . . . ? Pt1 N2 C16 C15 177.1(6) . . . . ? C12 N2 C16 C7 -179.5(6) . . . . ? Pt1 N2 C16 C7 -2.5(8) . . . . ? C14 C15 C16 N2 -0.6(12) . . . . ? C14 C15 C16 C7 178.9(8) . . . . ? N1 C7 C16 N2 0.5(10) . . . . ? C8 C7 C16 N2 -178.8(7) . . . . ? N1 C7 C16 C15 -179.1(7) . . . . ? C8 C7 C16 C15 1.7(13) . . . . ? C22 C17 C18 C19 -2.6(11) . . . . ? C2" C17 C18 C19 174.2(7) . . . . ? C17 C18 C19 C20 2.0(11) . . . . ? C17 C18 C19 C23 -179.3(7) . . . . ? C28 N4 C20 C21 -179.8(8) . . . . ? C29 N4 C20 C21 -5.4(14) . . . . ? C28 N4 C20 C19 -0.3(9) . . . . ? C29 N4 C20 C19 174.0(7) . . . . ? C18 C19 C20 C21 -0.2(11) . . . . ? C23 C19 C20 C21 -179.3(7) . . . . ? C18 C19 C20 N4 -179.7(7) . . . . ? C23 C19 C20 N4 1.2(9) . . . . ? N4 C20 C21 C22 178.6(8) . . . . ? C19 C20 C21 C22 -0.8(12) . . . . ? C20 C21 C22 C17 0.1(13) . . . . ? C18 C17 C22 C21 1.6(12) . . . . ? C2" C17 C22 C21 -175.4(8) . . . . ? C18 C19 C23 C24 1.1(16) . . . . ? C20 C19 C23 C24 179.9(9) . . . . ? C18 C19 C23 C28 179.5(8) . . . . ? C20 C19 C23 C28 -1.7(9) . . . . ? C28 C23 C24 C25 1.7(13) . . . . ? C19 C23 C24 C25 179.9(10) . . . . ? C23 C24 C25 C26 0.9(17) . . . . ? C24 C25 C26 C27 -3(2) . . . . ? C25 C26 C27 C28 2.3(18) . . . . ? C20 N4 C28 C27 -178.0(10) . . . . ? C29 N4 C28 C27 7.8(16) . . . . ? C20 N4 C28 C23 -0.8(10) . . . . ? C29 N4 C28 C23 -175.0(8) . . . . ? C26 C27 C28 N4 177.2(10) . . . . ? C26 C27 C28 C23 0.2(15) . . . . ? C24 C23 C28 N4 -179.8(8) . . . . ? C19 C23 C28 N4 1.5(9) . . . . ? C24 C23 C28 C27 -2.3(13) . . . . ? C19 C23 C28 C27 179.1(8) . . . . ? C1 Pt1 C1" C2" 105(30) . . . . ? N2 Pt1 C1" C2" 39(33) . . . . ? N1 Pt1 C1" C2" -75(30) . . . . ? Pt1 C1" C2" C17 -148(24) . . . . ? C18 C17 C2" C1" -75(30) . . . . ? C22 C17 C2" C1" 102(30) . . . . ? _diffrn_measured_fraction_theta_max .986 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full .986 _refine_diff_density_max .698 _refine_diff_density_min -1.307 _refine_diff_density_rms .362