# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Suning Wang' _publ_contact_author_email WANGS@CHEM.QUEENSU.CA _publ_section_title ; Impact of the Linker Groups in Bis(7-azaindol-1-yl) Chelate Ligands on Structures and Stability of Pt(N,N-L)R2 Complexes ; loop_ _publ_author_name 'Suning Wang.' 'Guohui Liu.' 'Datong Song.' 'Shu-Bin Zhao.' # Attachment '1.cif' data_sdt62a _database_code_depnum_ccdc_archive 'CCDC 697407' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 N4 Pt' _chemical_formula_weight 597.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.238(3) _cell_length_b 11.930(3) _cell_length_c 18.202(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.953(6) _cell_angle_gamma 90.00 _cell_volume 2651.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 5.312 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4164 _exptl_absorpt_correction_T_max 0.4164 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Apex _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 17999 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5766 _reflns_number_gt 3678 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5766 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0382 _refine_ls_goodness_of_fit_ref 0.723 _refine_ls_restrained_S_all 0.723 _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 0.682506(10) 0.831730(13) 0.066753(9) 0.03883(5) Uani 1 1 d . . . N1 N 0.6144(2) 0.7979(3) -0.1201(2) 0.0489(9) Uani 1 1 d . . . N2 N 0.6509(2) 0.6961(3) -0.00740(18) 0.0418(8) Uani 1 1 d . . . N3 N 0.7727(2) 0.9159(3) -0.10097(19) 0.0480(9) Uani 1 1 d . . . N4 N 0.8370(2) 0.8510(3) 0.02107(18) 0.0424(8) Uani 1 1 d . . . C1 C 0.5852(3) 0.7676(4) -0.1921(3) 0.0667(14) Uani 1 1 d . . . H1A H 0.5767 0.8172 -0.2314 0.080 Uiso 1 1 calc R . . C2 C 0.5709(3) 0.6557(5) -0.1970(3) 0.0673(13) Uani 1 1 d . . . H2A H 0.5492 0.6155 -0.2393 0.081 Uiso 1 1 calc R . . C3 C 0.5949(3) 0.6112(4) -0.1261(3) 0.0545(12) Uani 1 1 d . . . C4 C 0.5988(3) 0.5055(4) -0.0944(3) 0.0660(13) Uani 1 1 d . . . H4A H 0.5808 0.4422 -0.1224 0.079 Uiso 1 1 calc R . . C5 C 0.6299(3) 0.4966(4) -0.0211(3) 0.0623(12) Uani 1 1 d . . . H5A H 0.6346 0.4263 0.0009 0.075 Uiso 1 1 calc R . . C6 C 0.6543(3) 0.5913(4) 0.0204(2) 0.0524(11) Uani 1 1 d . . . H6A H 0.6741 0.5823 0.0703 0.063 Uiso 1 1 calc R . . C7 C 0.6222(3) 0.7022(3) -0.0785(3) 0.0422(10) Uani 1 1 d . . . C8 C 0.8241(4) 0.9396(3) -0.1645(3) 0.0672(13) Uani 1 1 d . . . H8A H 0.7884 0.9631 -0.2086 0.081 Uiso 1 1 calc R . . C9 C 0.9337(4) 0.9238(3) -0.1537(3) 0.0719(15) Uani 1 1 d . . . H9A H 0.9853 0.9336 -0.1884 0.086 Uiso 1 1 calc R . . C10 C 0.9551(3) 0.8893(3) -0.0791(3) 0.0527(12) Uani 1 1 d . . . C11 C 1.0466(3) 0.8621(4) -0.0342(3) 0.0660(15) Uani 1 1 d . . . H11A H 1.1160 0.8657 -0.0518 0.079 Uiso 1 1 calc R . . C12 C 1.0333(3) 0.8300(4) 0.0359(3) 0.0656(13) Uani 1 1 d . . . H12A H 1.0942 0.8110 0.0668 0.079 Uiso 1 1 calc R . . C13 C 0.9294(3) 0.8253(3) 0.0621(2) 0.0551(11) Uani 1 1 d . . . H13A H 0.9233 0.8031 0.1106 0.066 Uiso 1 1 calc R . . C14 C 0.8511(3) 0.8833(3) -0.0480(2) 0.0435(10) Uani 1 1 d . . . C15 C 0.6549(3) 0.9086(3) -0.0985(2) 0.0511(11) Uani 1 1 d . . . H15A H 0.6205 0.9643 -0.1313 0.061 Uiso 1 1 calc R . . H15B H 0.6351 0.9249 -0.0489 0.061 Uiso 1 1 calc R . . C16 C 0.7167(3) 0.9533(3) 0.1390(2) 0.0405(10) Uani 1 1 d . . . C17 C 0.6789(3) 1.0614(4) 0.1299(2) 0.0586(12) Uani 1 1 d . . . H17A H 0.6328 1.0777 0.0886 0.070 Uiso 1 1 calc R . . C18 C 0.7060(4) 1.1471(4) 0.1791(3) 0.0721(14) Uani 1 1 d . . . H18A H 0.6788 1.2190 0.1704 0.087 Uiso 1 1 calc R . . C19 C 0.7730(4) 1.1251(4) 0.2405(3) 0.0765(16) Uani 1 1 d . . . H19A H 0.7919 1.1819 0.2739 0.092 Uiso 1 1 calc R . . C20 C 0.8118(3) 1.0196(4) 0.2523(2) 0.0657(14) Uani 1 1 d . . . H20A H 0.8567 1.0039 0.2943 0.079 Uiso 1 1 calc R . . C21 C 0.7854(3) 0.9362(3) 0.2027(2) 0.0498(11) Uani 1 1 d . . . H21A H 0.8143 0.8650 0.2117 0.060 Uiso 1 1 calc R . . C22 C 0.5341(3) 0.8152(3) 0.1044(2) 0.0379(9) Uani 1 1 d . . . C23 C 0.5089(3) 0.8123(3) 0.1771(2) 0.0521(11) Uani 1 1 d . . . H23A H 0.5654 0.8206 0.2135 0.063 Uiso 1 1 calc R . . C24 C 0.4029(3) 0.7975(3) 0.1984(2) 0.0588(13) Uani 1 1 d . . . H24A H 0.3906 0.7941 0.2482 0.071 Uiso 1 1 calc R . . C25 C 0.3168(3) 0.7879(3) 0.1470(3) 0.0546(12) Uani 1 1 d . . . H25A H 0.2459 0.7780 0.1613 0.066 Uiso 1 1 calc R . . C26 C 0.3365(3) 0.7929(3) 0.0749(3) 0.0568(13) Uani 1 1 d . . . H26A H 0.2785 0.7885 0.0392 0.068 Uiso 1 1 calc R . . C27 C 0.4432(3) 0.8047(3) 0.0539(2) 0.0442(11) Uani 1 1 d . . . H27A H 0.4546 0.8056 0.0039 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03297(7) 0.04079(9) 0.04279(10) -0.00270(10) 0.00304(6) -0.00052(9) N1 0.0476(19) 0.058(3) 0.040(2) -0.0082(19) -0.0024(18) 0.0016(18) N2 0.0372(16) 0.043(2) 0.045(2) -0.0019(17) 0.0045(16) 0.0005(15) N3 0.0469(19) 0.046(2) 0.052(2) 0.0074(18) 0.0081(19) -0.0012(17) N4 0.0346(16) 0.043(2) 0.049(2) -0.0041(18) 0.0044(16) -0.0014(15) C1 0.061(3) 0.083(4) 0.055(4) -0.002(3) 0.000(3) 0.001(3) C2 0.060(3) 0.086(4) 0.055(3) -0.023(3) -0.002(2) -0.006(3) C3 0.047(2) 0.055(3) 0.062(4) -0.015(3) 0.009(2) -0.001(2) C4 0.057(3) 0.058(3) 0.085(4) -0.031(3) 0.016(3) -0.009(3) C5 0.064(3) 0.047(3) 0.076(4) -0.004(3) 0.012(3) -0.009(2) C6 0.052(2) 0.053(3) 0.052(3) -0.006(3) 0.005(2) -0.003(2) C7 0.034(2) 0.042(3) 0.051(3) -0.007(2) 0.008(2) -0.0024(18) C8 0.083(3) 0.062(3) 0.059(4) 0.006(3) 0.026(3) -0.007(3) C9 0.075(3) 0.058(3) 0.088(4) 0.006(3) 0.039(3) -0.009(3) C10 0.049(2) 0.040(3) 0.072(4) -0.007(2) 0.026(3) -0.005(2) C11 0.043(2) 0.070(4) 0.088(4) -0.016(3) 0.022(3) -0.007(2) C12 0.034(2) 0.075(3) 0.088(4) -0.010(3) 0.002(2) 0.006(2) C13 0.043(2) 0.061(3) 0.062(3) -0.002(3) 0.004(2) 0.003(2) C14 0.049(2) 0.033(2) 0.050(3) -0.009(2) 0.013(2) -0.0047(19) C15 0.050(2) 0.049(3) 0.054(3) 0.004(2) 0.002(2) 0.005(2) C16 0.0329(19) 0.046(3) 0.043(3) 0.002(2) 0.0079(19) -0.0026(18) C17 0.061(3) 0.056(3) 0.059(3) -0.001(3) 0.004(2) 0.007(2) C18 0.085(3) 0.044(3) 0.090(4) -0.011(3) 0.022(3) 0.004(3) C19 0.067(3) 0.072(4) 0.092(5) -0.036(3) 0.019(3) -0.015(3) C20 0.048(2) 0.091(4) 0.058(3) -0.024(3) 0.002(2) -0.007(3) C21 0.050(2) 0.050(3) 0.049(3) -0.008(2) 0.002(2) 0.000(2) C22 0.0400(19) 0.033(2) 0.041(2) -0.001(2) 0.0016(18) 0.0010(18) C23 0.043(2) 0.065(3) 0.047(3) -0.001(2) 0.002(2) 0.001(2) C24 0.057(3) 0.073(4) 0.048(3) 0.003(2) 0.014(2) -0.002(2) C25 0.037(2) 0.059(3) 0.070(4) -0.003(3) 0.015(2) -0.001(2) C26 0.037(2) 0.070(3) 0.063(3) -0.009(3) -0.003(2) 0.003(2) C27 0.040(2) 0.052(3) 0.041(3) 0.002(2) 0.0029(19) 0.0031(19) _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 C16 1.983(4) . ? Pt1 C22 1.994(3) . ? Pt1 N2 2.125(3) . ? Pt1 N4 2.130(3) . ? N1 C7 1.369(4) . ? N1 C1 1.382(5) . ? N1 C15 1.455(4) . ? N2 C7 1.319(5) . ? N2 C6 1.349(5) . ? N3 C14 1.369(4) . ? N3 C8 1.383(5) . ? N3 C15 1.448(4) . ? N4 C14 1.337(4) . ? N4 C13 1.346(4) . ? C1 C2 1.348(6) . ? C2 C3 1.409(6) . ? C3 C4 1.386(6) . ? C3 C7 1.414(5) . ? C4 C5 1.365(5) . ? C5 C6 1.381(5) . ? C8 C9 1.355(5) . ? C9 C10 1.426(6) . ? C10 C11 1.378(5) . ? C10 C14 1.431(5) . ? C11 C12 1.352(5) . ? C12 C13 1.390(5) . ? C16 C17 1.376(5) . ? C16 C21 1.400(5) . ? C17 C18 1.384(5) . ? C18 C19 1.365(6) . ? C19 C20 1.358(6) . ? C20 C21 1.366(5) . ? C22 C23 1.380(5) . ? C22 C27 1.399(4) . ? C23 C24 1.390(4) . ? C24 C25 1.365(5) . ? C25 C26 1.352(5) . ? C26 C27 1.393(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 C16 Pt1 C22 90.01(14) . . ? C16 Pt1 N2 177.20(15) . . ? C22 Pt1 N2 90.72(13) . . ? C16 Pt1 N4 91.57(12) . . ? C22 Pt1 N4 177.04(14) . . ? N2 Pt1 N4 87.82(11) . . ? C7 N1 C1 108.0(4) . . ? C7 N1 C15 126.7(4) . . ? C1 N1 C15 123.7(4) . . ? C7 N2 C6 114.7(3) . . ? C7 N2 Pt1 127.3(3) . . ? C6 N2 Pt1 117.9(3) . . ? C14 N3 C8 108.0(3) . . ? C14 N3 C15 127.7(3) . . ? C8 N3 C15 123.4(4) . . ? C14 N4 C13 115.4(3) . . ? C14 N4 Pt1 125.0(2) . . ? C13 N4 Pt1 119.6(3) . . ? C2 C1 N1 110.3(4) . . ? C1 C2 C3 107.1(4) . . ? C4 C3 C2 136.3(5) . . ? C4 C3 C7 116.3(4) . . ? C2 C3 C7 107.3(4) . . ? C5 C4 C3 118.5(5) . . ? C4 C5 C6 120.4(5) . . ? N2 C6 C5 123.7(4) . . ? N2 C7 N1 126.3(4) . . ? N2 C7 C3 126.5(4) . . ? N1 C7 C3 107.2(4) . . ? C9 C8 N3 110.7(4) . . ? C8 C9 C10 107.0(4) . . ? C11 C10 C9 136.2(4) . . ? C11 C10 C14 117.5(4) . . ? C9 C10 C14 106.3(4) . . ? C12 C11 C10 118.8(4) . . ? C11 C12 C13 120.5(4) . . ? N4 C13 C12 123.6(4) . . ? N4 C14 N3 128.0(3) . . ? N4 C14 C10 124.2(4) . . ? N3 C14 C10 107.9(4) . . ? N3 C15 N1 111.6(3) . . ? C17 C16 C21 114.4(4) . . ? C17 C16 Pt1 123.5(3) . . ? C21 C16 Pt1 122.0(3) . . ? C16 C17 C18 123.5(4) . . ? C19 C18 C17 119.4(5) . . ? C20 C19 C18 119.5(5) . . ? C19 C20 C21 120.4(5) . . ? C20 C21 C16 122.8(4) . . ? C23 C22 C27 114.0(3) . . ? C23 C22 Pt1 127.0(3) . . ? C27 C22 Pt1 119.0(3) . . ? C22 C23 C24 123.1(4) . . ? C25 C24 C23 120.7(4) . . ? C26 C25 C24 118.7(4) . . ? C25 C26 C27 120.2(4) . . ? C26 C27 C22 123.2(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.031 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.080 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 -0.001 0.500 283.7 76.3 2 1.000 0.499 0.000 283.7 76.0 _platon_squeeze_details ;One disordered THF per molecule was found and removed by squeeze. ; # Attachment '2.cif' data_sdt50 _database_code_depnum_ccdc_archive 'CCDC 697408' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N4 Pt' _chemical_formula_weight 659.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c 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 15.404(3) _cell_length_b 11.527(2) _cell_length_c 15.536(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.390(4) _cell_angle_gamma 90.00 _cell_volume 2550.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 5.530 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4043 _exptl_absorpt_correction_T_max 0.6078 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ApexII _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 17073 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5546 _reflns_number_gt 4334 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5546 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0363 _refine_ls_wR_factor_gt 0.0340 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 0.289526(7) 0.114882(8) 0.179963(6) 0.03958(4) Uani 1 1 d . . . N1 N 0.18404(17) 0.3927(2) 0.14260(17) 0.0554(6) Uani 1 1 d . . . N2 N 0.29990(16) 0.27225(19) 0.25840(14) 0.0448(5) Uani 1 1 d . . . N3 N 0.29405(16) 0.3378(2) 0.03875(15) 0.0479(6) Uani 1 1 d . . . N4 N 0.39583(15) 0.19662(18) 0.14388(14) 0.0403(5) Uani 1 1 d . . . C1 C 0.1558(2) 0.5075(3) 0.1427(3) 0.0763(10) Uani 1 1 d . . . H1A H 0.1100 0.5444 0.0927 0.092 Uiso 1 1 calc R . . C2 C 0.2040(3) 0.5572(3) 0.2251(3) 0.0840(11) Uani 1 1 d . . . H2A H 0.1967 0.6329 0.2419 0.101 Uiso 1 1 calc R . . C3 C 0.2677(2) 0.4749(3) 0.2819(2) 0.0610(8) Uani 1 1 d . . . C4 C 0.3354(3) 0.4727(3) 0.3714(2) 0.0734(10) Uani 1 1 d . . . H4A H 0.3476 0.5382 0.4091 0.088 Uiso 1 1 calc R . . C5 C 0.3837(2) 0.3723(3) 0.4029(2) 0.0679(9) Uani 1 1 d . . . H5A H 0.4296 0.3689 0.4627 0.081 Uiso 1 1 calc R . . C6 C 0.3647(2) 0.2748(3) 0.34594(19) 0.0565(8) Uani 1 1 d . . . H6A H 0.3987 0.2075 0.3697 0.068 Uiso 1 1 calc R . . C7 C 0.2539(2) 0.3718(2) 0.22834(19) 0.0472(7) Uani 1 1 d . . . C8 C 0.3087(2) 0.4419(3) 0.0022(2) 0.0673(9) Uani 1 1 d . . . H8A H 0.2614 0.4885 -0.0383 0.081 Uiso 1 1 calc R . . C9 C 0.4012(2) 0.4663(3) 0.0339(2) 0.0700(9) Uani 1 1 d . . . H9A H 0.4284 0.5320 0.0200 0.084 Uiso 1 1 calc R . . C10 C 0.4497(2) 0.3726(2) 0.09261(19) 0.0502(7) Uani 1 1 d . . . C11 C 0.5422(2) 0.3438(3) 0.1439(2) 0.0595(8) Uani 1 1 d . . . H11A H 0.5909 0.3927 0.1457 0.071 Uiso 1 1 calc R . . C12 C 0.5601(2) 0.2413(3) 0.1919(2) 0.0584(8) Uani 1 1 d . . . H12A H 0.6218 0.2185 0.2251 0.070 Uiso 1 1 calc R . . C13 C 0.4867(2) 0.1712(3) 0.19130(18) 0.0521(7) Uani 1 1 d . . . H13A H 0.5012 0.1028 0.2256 0.063 Uiso 1 1 calc R . . C14 C 0.38016(19) 0.2940(2) 0.09400(17) 0.0406(6) Uani 1 1 d . . . C15 C 0.1483(2) 0.3170(2) 0.06428(18) 0.0483(7) Uani 1 1 d . . . C16 C 0.0571(2) 0.2768(3) 0.0349(2) 0.0626(8) Uani 1 1 d . . . H16A H 0.0191 0.2991 0.0663 0.075 Uiso 1 1 calc R . . C17 C 0.0223(2) 0.2039(3) -0.0404(2) 0.0706(9) Uani 1 1 d . . . H17A H -0.0392 0.1774 -0.0600 0.085 Uiso 1 1 calc R . . C18 C 0.0785(2) 0.1701(3) -0.0870(2) 0.0698(9) Uani 1 1 d . . . H18A H 0.0555 0.1189 -0.1368 0.084 Uiso 1 1 calc R . . C19 C 0.1690(2) 0.2123(3) -0.05951(18) 0.0584(8) Uani 1 1 d . . . H19A H 0.2064 0.1910 -0.0918 0.070 Uiso 1 1 calc R . . C20 C 0.20349(19) 0.2858(2) 0.01544(17) 0.0453(7) Uani 1 1 d . . . C21 C 0.28522(19) -0.0272(2) 0.10484(16) 0.0415(6) Uani 1 1 d . . . C22 C 0.3655(2) -0.0909(2) 0.11216(19) 0.0527(7) Uani 1 1 d . . . H22A H 0.4237 -0.0665 0.1544 0.063 Uiso 1 1 calc R . . C23 C 0.3613(2) -0.1879(3) 0.0593(2) 0.0632(9) Uani 1 1 d . . . H23A H 0.4160 -0.2285 0.0676 0.076 Uiso 1 1 calc R . . C24 C 0.2783(3) -0.2252(3) -0.0048(2) 0.0640(9) Uani 1 1 d . . . H24A H 0.2760 -0.2908 -0.0405 0.077 Uiso 1 1 calc R . . C25 C 0.1981(2) -0.1647(3) -0.0162(2) 0.0648(9) Uani 1 1 d . . . H25A H 0.1410 -0.1889 -0.0606 0.078 Uiso 1 1 calc R . . C26 C 0.2015(2) -0.0676(3) 0.03792(19) 0.0551(8) Uani 1 1 d . . . H26A H 0.1460 -0.0282 0.0292 0.066 Uiso 1 1 calc R . . C27 C 0.19730(19) 0.0444(2) 0.22725(16) 0.0426(6) Uani 1 1 d . . . C28 C 0.1963(2) -0.0728(3) 0.24967(17) 0.0498(7) Uani 1 1 d . . . H28A H 0.2385 -0.1229 0.2391 0.060 Uiso 1 1 calc R . . C29 C 0.1344(2) -0.1171(3) 0.28730(18) 0.0608(8) Uani 1 1 d . . . H29A H 0.1364 -0.1955 0.3018 0.073 Uiso 1 1 calc R . . C30 C 0.0702(2) -0.0464(3) 0.30328(19) 0.0656(9) Uani 1 1 d . . . H30A H 0.0294 -0.0762 0.3290 0.079 Uiso 1 1 calc R . . C31 C 0.0675(2) 0.0673(3) 0.2809(2) 0.0659(9) Uani 1 1 d . . . H31A H 0.0236 0.1159 0.2902 0.079 Uiso 1 1 calc R . . C32 C 0.1299(2) 0.1124(3) 0.24404(19) 0.0552(7) Uani 1 1 d . . . H32A H 0.1266 0.1911 0.2299 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.04281(7) 0.03777(6) 0.04050(6) -0.00199(5) 0.01848(5) -0.00426(6) N1 0.0536(16) 0.0473(15) 0.0677(16) -0.0061(13) 0.0259(14) 0.0028(13) N2 0.0476(15) 0.0438(14) 0.0486(13) -0.0089(11) 0.0246(12) -0.0085(12) N3 0.0395(14) 0.0501(14) 0.0546(13) 0.0123(12) 0.0186(12) -0.0021(12) N4 0.0390(13) 0.0401(13) 0.0454(12) -0.0015(10) 0.0200(11) -0.0019(11) C1 0.067(2) 0.054(2) 0.109(3) 0.004(2) 0.034(2) 0.0159(19) C2 0.091(3) 0.050(2) 0.119(3) -0.026(2) 0.049(3) 0.000(2) C3 0.066(2) 0.049(2) 0.079(2) -0.0212(18) 0.041(2) -0.0120(18) C4 0.083(3) 0.071(2) 0.080(2) -0.035(2) 0.046(2) -0.027(2) C5 0.074(2) 0.080(3) 0.0554(18) -0.0224(19) 0.0307(17) -0.024(2) C6 0.058(2) 0.064(2) 0.0523(17) -0.0058(16) 0.0260(16) -0.0090(17) C7 0.0477(17) 0.0454(18) 0.0578(17) -0.0095(15) 0.0306(15) -0.0113(15) C8 0.059(2) 0.061(2) 0.084(2) 0.0280(18) 0.0297(19) 0.0041(18) C9 0.058(2) 0.060(2) 0.096(2) 0.0239(19) 0.033(2) -0.0089(18) C10 0.0437(17) 0.0516(19) 0.0584(16) 0.0030(15) 0.0229(14) -0.0075(15) C11 0.0440(19) 0.066(2) 0.0691(19) -0.0024(17) 0.0218(16) -0.0166(17) C12 0.0379(18) 0.065(2) 0.0662(19) 0.0020(17) 0.0137(15) -0.0020(16) C13 0.0498(19) 0.0508(18) 0.0540(16) 0.0038(14) 0.0178(15) 0.0031(16) C14 0.0399(16) 0.0447(16) 0.0404(14) -0.0009(13) 0.0189(13) -0.0027(14) C15 0.0434(18) 0.0504(18) 0.0501(16) 0.0021(14) 0.0166(14) -0.0013(15) C16 0.046(2) 0.074(2) 0.072(2) 0.0010(18) 0.0272(17) 0.0005(18) C17 0.0440(19) 0.083(3) 0.076(2) 0.002(2) 0.0126(18) -0.0156(18) C18 0.062(2) 0.080(2) 0.0533(18) -0.0095(17) 0.0062(17) -0.014(2) C19 0.055(2) 0.072(2) 0.0465(16) 0.0007(16) 0.0176(15) -0.0022(17) C20 0.0369(16) 0.0510(18) 0.0442(15) 0.0109(13) 0.0113(13) -0.0001(14) C21 0.0472(18) 0.0378(15) 0.0421(14) 0.0013(12) 0.0200(14) -0.0035(14) C22 0.0560(19) 0.0465(19) 0.0499(16) -0.0007(14) 0.0136(15) 0.0018(15) C23 0.068(2) 0.051(2) 0.067(2) -0.0075(16) 0.0217(19) 0.0107(18) C24 0.082(3) 0.0447(19) 0.068(2) -0.0133(16) 0.032(2) -0.0013(19) C25 0.064(2) 0.061(2) 0.068(2) -0.0234(18) 0.0244(18) -0.0184(19) C26 0.053(2) 0.0539(18) 0.0615(18) -0.0109(16) 0.0257(16) -0.0071(16) C27 0.0432(17) 0.0477(17) 0.0373(13) -0.0017(12) 0.0157(13) -0.0075(14) C28 0.0493(18) 0.0516(18) 0.0470(15) 0.0036(14) 0.0167(14) -0.0048(15) C29 0.066(2) 0.063(2) 0.0483(16) 0.0125(15) 0.0163(16) -0.0170(19) C30 0.068(2) 0.083(3) 0.0566(18) -0.0035(18) 0.0352(17) -0.027(2) C31 0.063(2) 0.075(2) 0.073(2) -0.0151(18) 0.0409(18) -0.0107(19) C32 0.061(2) 0.0507(18) 0.0631(17) -0.0046(15) 0.0344(16) -0.0074(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 C21 1.998(3) . ? Pt1 C27 2.003(3) . ? Pt1 N4 2.141(2) . ? Pt1 N2 2.157(2) . ? N1 C7 1.378(4) . ? N1 C1 1.394(4) . ? N1 C15 1.426(3) . ? N2 C7 1.335(3) . ? N2 C6 1.346(3) . ? N3 C14 1.373(3) . ? N3 C8 1.381(3) . ? N3 C20 1.432(3) . ? N4 C14 1.333(3) . ? N4 C13 1.343(3) . ? C1 C2 1.340(4) . ? C2 C3 1.407(5) . ? C3 C4 1.385(4) . ? C3 C7 1.420(4) . ? C4 C5 1.362(4) . ? C5 C6 1.390(4) . ? C8 C9 1.349(4) . ? C9 C10 1.428(4) . ? C10 C11 1.382(4) . ? C10 C14 1.409(3) . ? C11 C12 1.369(4) . ? C12 C13 1.387(4) . ? C15 C16 1.381(4) . ? C15 C20 1.386(3) . ? C16 C17 1.372(4) . ? C17 C18 1.379(4) . ? C18 C19 1.382(4) . ? C19 C20 1.373(4) . ? C21 C26 1.393(4) . ? C21 C22 1.405(4) . ? C22 C23 1.374(4) . ? C23 C24 1.356(4) . ? C24 C25 1.370(4) . ? C25 C26 1.390(4) . ? C27 C28 1.396(4) . ? C27 C32 1.403(4) . ? C28 C29 1.393(4) . ? C29 C30 1.374(4) . ? C30 C31 1.353(4) . ? C31 C32 1.392(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 C21 Pt1 C27 90.66(10) . . ? C21 Pt1 N4 93.81(9) . . ? C27 Pt1 N4 174.03(8) . . ? C21 Pt1 N2 176.82(9) . . ? C27 Pt1 N2 92.52(9) . . ? N4 Pt1 N2 83.01(7) . . ? C7 N1 C1 107.1(3) . . ? C7 N1 C15 128.6(2) . . ? C1 N1 C15 124.2(3) . . ? C7 N2 C6 115.1(2) . . ? C7 N2 Pt1 127.55(18) . . ? C6 N2 Pt1 117.1(2) . . ? C14 N3 C8 107.8(2) . . ? C14 N3 C20 128.3(2) . . ? C8 N3 C20 123.7(2) . . ? C14 N4 C13 115.0(2) . . ? C14 N4 Pt1 122.40(18) . . ? C13 N4 Pt1 120.11(18) . . ? C2 C1 N1 110.4(3) . . ? C1 C2 C3 108.1(3) . . ? C4 C3 C2 136.0(3) . . ? C4 C3 C7 117.4(3) . . ? C2 C3 C7 106.6(3) . . ? C5 C4 C3 118.4(3) . . ? C4 C5 C6 120.3(3) . . ? N2 C6 C5 123.8(3) . . ? N2 C7 N1 127.1(2) . . ? N2 C7 C3 125.0(3) . . ? N1 C7 C3 107.9(3) . . ? C9 C8 N3 110.3(3) . . ? C8 C9 C10 107.4(3) . . ? C11 C10 C14 117.4(3) . . ? C11 C10 C9 136.4(3) . . ? C14 C10 C9 106.3(3) . . ? C12 C11 C10 118.1(3) . . ? C11 C12 C13 120.4(3) . . ? N4 C13 C12 123.6(3) . . ? N4 C14 N3 126.2(2) . . ? N4 C14 C10 125.4(3) . . ? N3 C14 C10 108.3(2) . . ? C16 C15 C20 119.4(3) . . ? C16 C15 N1 120.1(3) . . ? C20 C15 N1 120.5(2) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 120.1(3) . . ? C17 C18 C19 120.0(3) . . ? C20 C19 C18 119.9(3) . . ? C19 C20 C15 120.3(3) . . ? C19 C20 N3 119.9(2) . . ? C15 C20 N3 119.7(2) . . ? C26 C21 C22 115.0(2) . . ? C26 C21 Pt1 121.7(2) . . ? C22 C21 Pt1 123.3(2) . . ? C23 C22 C21 122.5(3) . . ? C24 C23 C22 120.9(3) . . ? C23 C24 C25 118.9(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 122.1(3) . . ? C28 C27 C32 114.5(2) . . ? C28 C27 Pt1 124.1(2) . . ? C32 C27 Pt1 121.4(2) . . ? C29 C28 C27 122.2(3) . . ? C30 C29 C28 120.9(3) . . ? C31 C30 C29 118.8(3) . . ? C30 C31 C32 120.6(3) . . ? C31 C32 C27 123.0(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.821 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.061 # Attachment '3.cif' data_zs192 _database_code_depnum_ccdc_archive 'CCDC 697409' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H26 N4 Pt' _chemical_formula_weight 625.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.27880(10) _cell_length_b 10.28780(10) _cell_length_c 15.4456(3) _cell_angle_alpha 73.3860(10) _cell_angle_beta 89.3110(10) _cell_angle_gamma 69.1100(10) _cell_volume 1171.77(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6651 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.14 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 6.013 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3793 _exptl_absorpt_correction_T_max 0.3793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 10077 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4573 _reflns_number_gt 4264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^+0.9800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4573 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.175147(15) 0.127810(13) 0.749796(8) 0.01952(5) Uani 1 1 d . . . N1 N 0.3619(4) 0.0118(3) 0.86691(18) 0.0233(6) Uani 1 1 d . . . N2 N 0.6078(3) 0.0680(3) 0.80378(18) 0.0231(6) Uani 1 1 d . . . N3 N 0.3180(3) -0.0650(3) 0.71094(18) 0.0225(6) Uani 1 1 d . . . N4 N 0.5349(4) 0.0065(3) 0.62316(18) 0.0246(6) Uani 1 1 d . . . C1 C 0.3205(5) -0.0780(4) 0.9382(2) 0.0271(7) Uani 1 1 d . . . H1A H 0.2011 -0.0627 0.9434 0.032 Uiso 1 1 calc R . . C2 C 0.4423(5) -0.1916(4) 1.0044(2) 0.0307(8) Uani 1 1 d . . . H2A H 0.4046 -0.2504 1.0534 0.037 Uiso 1 1 calc R . . C3 C 0.6181(5) -0.2200(4) 0.9998(2) 0.0304(8) Uani 1 1 d . . . H3A H 0.7026 -0.2989 1.0440 0.036 Uiso 1 1 calc R . . C4 C 0.6660(4) -0.1290(4) 0.9284(2) 0.0258(7) Uani 1 1 d . . . C5 C 0.8258(4) -0.1165(4) 0.8993(2) 0.0297(8) Uani 1 1 d . . . H5A H 0.9393 -0.1800 0.9267 0.036 Uiso 1 1 calc R . . C6 C 0.7853(4) 0.0023(4) 0.8257(2) 0.0280(8) Uani 1 1 d . . . H6A H 0.8680 0.0362 0.7932 0.034 Uiso 1 1 calc R . . C7 C 0.5329(4) -0.0128(4) 0.8658(2) 0.0217(7) Uani 1 1 d . . . C8 C 0.5237(4) 0.2170(4) 0.7431(2) 0.0254(7) Uani 1 1 d . . . H8A H 0.5672 0.2826 0.7634 0.030 Uiso 1 1 calc R . . H8B H 0.3970 0.2494 0.7481 0.030 Uiso 1 1 calc R . . C9 C 0.5551(4) 0.2319(4) 0.6441(2) 0.0265(7) Uani 1 1 d . . . H9A H 0.5190 0.3370 0.6106 0.032 Uiso 1 1 calc R . . H9B H 0.6815 0.1863 0.6410 0.032 Uiso 1 1 calc R . . C10 C 0.4629(4) 0.1653(4) 0.5958(2) 0.0250(7) Uani 1 1 d . . . H10A H 0.3390 0.1979 0.6073 0.030 Uiso 1 1 calc R . . H10B H 0.4679 0.2027 0.5296 0.030 Uiso 1 1 calc R . . C11 C 0.2797(5) -0.1839(4) 0.7511(2) 0.0291(8) Uani 1 1 d . . . H11A H 0.1736 -0.1692 0.7782 0.035 Uiso 1 1 calc R . . C12 C 0.3826(5) -0.3245(4) 0.7558(3) 0.0344(8) Uani 1 1 d . . . H12A H 0.3465 -0.4026 0.7853 0.041 Uiso 1 1 calc R . . C13 C 0.5399(5) -0.3529(4) 0.7173(2) 0.0327(8) Uani 1 1 d . . . H13A H 0.6143 -0.4497 0.7213 0.039 Uiso 1 1 calc R . . C14 C 0.5830(4) -0.2347(4) 0.6732(2) 0.0256(7) Uani 1 1 d . . . C15 C 0.7243(5) -0.2156(4) 0.6249(2) 0.0323(8) Uani 1 1 d . . . H15A H 0.8235 -0.2904 0.6150 0.039 Uiso 1 1 calc R . . C16 C 0.6905(5) -0.0706(4) 0.5957(2) 0.0310(8) Uani 1 1 d . . . H16A H 0.7637 -0.0273 0.5609 0.037 Uiso 1 1 calc R . . C17 C 0.4664(4) -0.0928(4) 0.6705(2) 0.0229(7) Uani 1 1 d . . . C18 C 0.0096(4) 0.2255(4) 0.6357(2) 0.0219(7) Uani 1 1 d . . . C19 C -0.0004(4) 0.1483(4) 0.5759(2) 0.0298(8) Uani 1 1 d . . . H19A H 0.0665 0.0467 0.5921 0.036 Uiso 1 1 calc R . . C20 C -0.1051(5) 0.2147(4) 0.4930(2) 0.0347(9) Uani 1 1 d . . . H20A H -0.1070 0.1576 0.4546 0.042 Uiso 1 1 calc R . . C21 C -0.2042(5) 0.3598(4) 0.4664(2) 0.0362(9) Uani 1 1 d . . . H21A H -0.2749 0.4048 0.4100 0.043 Uiso 1 1 calc R . . C22 C -0.1986(6) 0.4399(5) 0.5242(3) 0.0515(12) Uani 1 1 d . . . H22A H -0.2669 0.5412 0.5073 0.062 Uiso 1 1 calc R . . C23 C -0.0947(5) 0.3742(4) 0.6060(3) 0.0394(9) Uani 1 1 d . . . H23A H -0.0942 0.4325 0.6438 0.047 Uiso 1 1 calc R . . C24 C 0.0552(4) 0.2891(4) 0.8030(2) 0.0232(7) Uani 1 1 d . . . C25 C -0.0535(4) 0.2733(4) 0.8719(2) 0.0277(7) Uani 1 1 d . . . H25A H -0.0757 0.1854 0.8912 0.033 Uiso 1 1 calc R . . C26 C -0.1306(5) 0.3808(4) 0.9134(2) 0.0326(8) Uani 1 1 d . . . H26A H -0.2041 0.3657 0.9599 0.039 Uiso 1 1 calc R . . C27 C -0.1003(5) 0.5095(4) 0.8871(3) 0.0363(9) Uani 1 1 d . . . H27A H -0.1516 0.5830 0.9156 0.044 Uiso 1 1 calc R . . C28 C 0.0056(5) 0.5298(4) 0.8187(3) 0.0340(8) Uani 1 1 d . . . H28A H 0.0268 0.6181 0.7998 0.041 Uiso 1 1 calc R . . C29 C 0.0809(4) 0.4224(4) 0.7777(2) 0.0264(7) Uani 1 1 d . . . H29A H 0.1528 0.4392 0.7307 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01762(7) 0.01954(7) 0.02333(7) -0.00834(5) 0.00433(5) -0.00768(5) N1 0.0251(14) 0.0227(15) 0.0237(14) -0.0097(11) 0.0036(11) -0.0087(12) N2 0.0222(14) 0.0260(15) 0.0243(14) -0.0082(11) 0.0033(11) -0.0120(12) N3 0.0201(14) 0.0224(15) 0.0258(14) -0.0092(11) 0.0037(11) -0.0072(12) N4 0.0239(14) 0.0223(15) 0.0294(15) -0.0100(12) 0.0059(12) -0.0091(12) C1 0.0307(18) 0.0298(19) 0.0259(17) -0.0100(14) 0.0094(14) -0.0162(16) C2 0.043(2) 0.0291(19) 0.0237(18) -0.0076(14) 0.0086(15) -0.0176(17) C3 0.038(2) 0.0243(18) 0.0252(18) -0.0086(14) -0.0007(15) -0.0067(16) C4 0.0296(18) 0.0230(18) 0.0259(17) -0.0118(14) -0.0011(14) -0.0073(15) C5 0.0210(17) 0.033(2) 0.0330(19) -0.0112(15) -0.0006(14) -0.0072(15) C6 0.0193(16) 0.034(2) 0.0325(19) -0.0129(15) 0.0055(14) -0.0095(15) C7 0.0240(17) 0.0243(17) 0.0202(16) -0.0119(13) 0.0015(13) -0.0085(14) C8 0.0269(18) 0.0227(18) 0.0288(18) -0.0083(14) 0.0036(14) -0.0113(15) C9 0.0239(17) 0.0233(18) 0.0308(18) -0.0044(14) 0.0051(14) -0.0098(14) C10 0.0242(17) 0.0250(18) 0.0236(17) -0.0038(13) 0.0040(13) -0.0092(14) C11 0.0301(19) 0.0259(19) 0.038(2) -0.0125(15) 0.0079(15) -0.0156(16) C12 0.041(2) 0.0228(19) 0.043(2) -0.0092(16) 0.0060(17) -0.0158(17) C13 0.037(2) 0.0224(19) 0.040(2) -0.0142(15) 0.0035(16) -0.0089(16) C14 0.0227(17) 0.0262(18) 0.0285(18) -0.0125(14) 0.0004(14) -0.0062(14) C15 0.0273(19) 0.032(2) 0.039(2) -0.0173(16) 0.0082(16) -0.0066(16) C16 0.0257(18) 0.038(2) 0.0334(19) -0.0152(16) 0.0108(15) -0.0134(16) C17 0.0214(16) 0.0262(18) 0.0205(16) -0.0075(13) -0.0022(13) -0.0078(14) C18 0.0174(15) 0.0267(18) 0.0247(16) -0.0086(13) 0.0063(13) -0.0113(14) C19 0.0241(17) 0.032(2) 0.0336(19) -0.0164(15) 0.0036(14) -0.0052(15) C20 0.034(2) 0.048(2) 0.032(2) -0.0238(17) 0.0107(16) -0.0187(19) C21 0.042(2) 0.044(2) 0.0248(18) -0.0026(16) -0.0022(16) -0.024(2) C22 0.068(3) 0.027(2) 0.048(3) 0.0019(18) -0.022(2) -0.014(2) C23 0.050(2) 0.028(2) 0.039(2) -0.0106(16) -0.0143(18) -0.0129(19) C24 0.0207(16) 0.0211(17) 0.0267(17) -0.0083(13) -0.0003(13) -0.0055(14) C25 0.0259(18) 0.0267(19) 0.0322(19) -0.0120(15) 0.0050(14) -0.0094(15) C26 0.0300(19) 0.037(2) 0.0304(19) -0.0138(16) 0.0071(15) -0.0091(17) C27 0.031(2) 0.033(2) 0.045(2) -0.0254(18) 0.0010(17) -0.0011(17) C28 0.032(2) 0.026(2) 0.044(2) -0.0114(16) -0.0034(17) -0.0091(16) C29 0.0270(18) 0.0216(18) 0.0310(18) -0.0078(14) 0.0037(14) -0.0096(15) _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 C24 2.000(3) . ? Pt1 C18 2.014(3) . ? Pt1 N1 2.146(3) . ? Pt1 N3 2.164(3) . ? N1 C7 1.347(4) . ? N1 C1 1.349(4) . ? N2 C7 1.375(4) . ? N2 C6 1.380(4) . ? N2 C8 1.464(4) . ? N3 C17 1.346(4) . ? N3 C11 1.349(4) . ? N4 C17 1.370(4) . ? N4 C16 1.385(4) . ? N4 C10 1.455(4) . ? C1 C2 1.389(5) . ? C1 H1A 0.9500 . ? C2 C3 1.384(5) . ? C2 H2A 0.9500 . ? C3 C4 1.384(5) . ? C3 H3A 0.9500 . ? C4 C7 1.415(4) . ? C4 C5 1.429(5) . ? C5 C6 1.350(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C8 C9 1.522(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.374(5) . ? C11 H11A 0.9500 . ? C12 C13 1.394(5) . ? C12 H12A 0.9500 . ? C13 C14 1.379(5) . ? C13 H13A 0.9500 . ? C14 C15 1.422(5) . ? C14 C17 1.423(5) . ? C15 C16 1.352(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C18 C19 1.400(5) . ? C18 C23 1.401(5) . ? C19 C20 1.401(5) . ? C19 H19A 0.9500 . ? C20 C21 1.362(5) . ? C20 H20A 0.9500 . ? C21 C22 1.388(6) . ? C21 H21A 0.9500 . ? C22 C23 1.385(5) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.396(5) . ? C24 C29 1.406(5) . ? C25 C26 1.391(5) . ? C25 H25A 0.9500 . ? C26 C27 1.381(5) . ? C26 H26A 0.9500 . ? C27 C28 1.382(5) . ? C27 H27A 0.9500 . ? C28 C29 1.382(5) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? 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 C24 Pt1 C18 92.56(13) . . ? C24 Pt1 N1 91.61(11) . . ? C18 Pt1 N1 175.82(11) . . ? C24 Pt1 N3 172.24(11) . . ? C18 Pt1 N3 94.62(12) . . ? N1 Pt1 N3 81.24(10) . . ? C7 N1 C1 114.8(3) . . ? C7 N1 Pt1 124.2(2) . . ? C1 N1 Pt1 118.0(2) . . ? C7 N2 C6 107.3(3) . . ? C7 N2 C8 127.7(3) . . ? C6 N2 C8 122.8(3) . . ? C17 N3 C11 114.4(3) . . ? C17 N3 Pt1 127.9(2) . . ? C11 N3 Pt1 115.5(2) . . ? C17 N4 C16 107.4(3) . . ? C17 N4 C10 130.3(3) . . ? C16 N4 C10 122.1(3) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C4 117.3(3) . . ? C2 C3 H3A 121.3 . . ? C4 C3 H3A 121.3 . . ? C3 C4 C7 118.2(3) . . ? C3 C4 C5 135.8(3) . . ? C7 C4 C5 106.0(3) . . ? C6 C5 C4 107.2(3) . . ? C6 C5 H5A 126.4 . . ? C4 C5 H5A 126.4 . . ? C5 C6 N2 110.9(3) . . ? C5 C6 H6A 124.5 . . ? N2 C6 H6A 124.5 . . ? N1 C7 N2 126.3(3) . . ? N1 C7 C4 125.1(3) . . ? N2 C7 C4 108.6(3) . . ? N2 C8 C9 113.5(3) . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 116.1(3) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N4 C10 C9 114.2(3) . . ? N4 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? N4 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N3 C11 C12 124.9(3) . . ? N3 C11 H11A 117.6 . . ? C12 C11 H11A 117.6 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 117.2(3) . . ? C14 C13 H13A 121.4 . . ? C12 C13 H13A 121.4 . . ? C13 C14 C15 135.0(3) . . ? C13 C14 C17 118.5(3) . . ? C15 C14 C17 106.6(3) . . ? C16 C15 C14 106.8(3) . . ? C16 C15 H15A 126.6 . . ? C14 C15 H15A 126.6 . . ? C15 C16 N4 111.1(3) . . ? C15 C16 H16A 124.5 . . ? N4 C16 H16A 124.5 . . ? N3 C17 N4 127.1(3) . . ? N3 C17 C14 124.7(3) . . ? N4 C17 C14 108.2(3) . . ? C19 C18 C23 114.4(3) . . ? C19 C18 Pt1 121.1(3) . . ? C23 C18 Pt1 124.4(3) . . ? C18 C19 C20 122.7(3) . . ? C18 C19 H19A 118.7 . . ? C20 C19 H19A 118.7 . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 117.9(3) . . ? C20 C21 H21A 121.1 . . ? C22 C21 H21A 121.1 . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C18 122.9(4) . . ? C22 C23 H23A 118.5 . . ? C18 C23 H23A 118.5 . . ? C25 C24 C29 115.4(3) . . ? C25 C24 Pt1 121.7(2) . . ? C29 C24 Pt1 122.9(2) . . ? C26 C25 C24 122.7(3) . . ? C26 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C24 122.4(3) . . ? C28 C29 H29A 118.8 . . ? C24 C29 H29A 118.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.314 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.093 # Attachment '4.cif' data_joy1 _database_code_depnum_ccdc_archive 'CCDC 697410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 N4 Pt' _chemical_formula_weight 639.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0677(16) _cell_length_b 10.5124(12) _cell_length_c 19.077(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.140(2) _cell_angle_gamma 90.00 _cell_volume 2475.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'thin plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 5.694 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3955 _exptl_absorpt_correction_T_max 0.5998 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 16791 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5408 _reflns_number_gt 3812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5408 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 0.005245(19) 0.45170(2) 0.231902(13) 0.04218(9) Uani 1 1 d . . . N1 N 0.1188(4) 0.5553(5) 0.3249(3) 0.0522(13) Uani 1 1 d . . . N2 N 0.0059(5) 0.6479(5) 0.3911(3) 0.0501(13) Uani 1 1 d . . . N3 N 0.0325(4) 0.2796(5) 0.2977(3) 0.0456(12) Uani 1 1 d . . . N4 N -0.1443(4) 0.2211(4) 0.3050(3) 0.0419(11) Uani 1 1 d . . . C1 C 0.2211(6) 0.5554(7) 0.3228(5) 0.070(2) Uani 1 1 d . . . H1A H 0.2367 0.5062 0.2857 0.084 Uiso 1 1 calc R . . C2 C 0.3045(6) 0.6242(8) 0.3724(6) 0.086(3) Uani 1 1 d . . . H2A H 0.3754 0.6203 0.3692 0.104 Uiso 1 1 calc R . . C3 C 0.2848(7) 0.6973(8) 0.4257(5) 0.085(3) Uani 1 1 d . . . H3A H 0.3417 0.7454 0.4591 0.102 Uiso 1 1 calc R . . C4 C 0.1825(6) 0.7012(7) 0.4312(4) 0.064(2) Uani 1 1 d . . . C5 C 0.1310(7) 0.7644(7) 0.4755(4) 0.068(2) Uani 1 1 d . . . H5A H 0.1645 0.8206 0.5154 0.081 Uiso 1 1 calc R . . C6 C 0.0255(6) 0.7308(6) 0.4509(4) 0.0570(18) Uani 1 1 d . . . H6A H -0.0275 0.7595 0.4715 0.068 Uiso 1 1 calc R . . C7 C 0.1021(5) 0.6279(5) 0.3780(3) 0.0454(15) Uani 1 1 d . . . C8 C 0.1333(5) 0.2316(6) 0.3105(4) 0.0543(16) Uani 1 1 d . . . H8A H 0.1862 0.2863 0.3024 0.065 Uiso 1 1 calc R . . C9 C 0.1650(6) 0.1099(6) 0.3343(4) 0.0559(17) Uani 1 1 d . . . H9A H 0.2370 0.0828 0.3412 0.067 Uiso 1 1 calc R . . C10 C 0.0923(6) 0.0278(6) 0.3481(4) 0.0552(18) Uani 1 1 d . . . H10A H 0.1123 -0.0571 0.3638 0.066 Uiso 1 1 calc R . . C11 C -0.0121(5) 0.0728(5) 0.3383(3) 0.0443(14) Uani 1 1 d . . . C12 C -0.1061(6) 0.0219(6) 0.3485(4) 0.0530(17) Uani 1 1 d . . . H12A H -0.1137 -0.0605 0.3667 0.064 Uiso 1 1 calc R . . C13 C -0.1834(5) 0.1132(5) 0.3274(3) 0.0491(15) Uani 1 1 d . . . H13A H -0.2554 0.1036 0.3282 0.059 Uiso 1 1 calc R . . C14 C -0.0377(5) 0.1999(5) 0.3124(3) 0.0424(14) Uani 1 1 d . . . C15 C -0.0994(5) 0.5909(5) 0.3543(3) 0.0449(14) Uani 1 1 d . . . H15A H -0.1047 0.5676 0.3030 0.054 Uiso 1 1 calc R . . H15B H -0.1566 0.6543 0.3515 0.054 Uiso 1 1 calc R . . C16 C -0.1188(5) 0.4737(5) 0.3942(3) 0.0451(14) Uani 1 1 d . . . H16A H -0.1245 0.4983 0.4429 0.054 Uiso 1 1 calc R . . H16B H -0.0570 0.4145 0.4031 0.054 Uiso 1 1 calc R . . C17 C -0.2231(5) 0.4077(6) 0.3477(3) 0.0465(15) Uani 1 1 d . . . H17A H -0.2463 0.3478 0.3797 0.056 Uiso 1 1 calc R . . H17B H -0.2808 0.4723 0.3291 0.056 Uiso 1 1 calc R . . C18 C -0.2103(5) 0.3350(5) 0.2821(3) 0.0440(14) Uani 1 1 d . . . H18A H -0.2828 0.3106 0.2482 0.053 Uiso 1 1 calc R . . H18B H -0.1764 0.3914 0.2544 0.053 Uiso 1 1 calc R . . C19 C 0.0035(5) 0.6042(5) 0.1693(3) 0.0429(14) Uani 1 1 d . . . C20 C -0.0055(5) 0.7280(6) 0.1925(4) 0.0518(16) Uani 1 1 d . . . H20A H -0.0213 0.7402 0.2372 0.062 Uiso 1 1 calc R . . C21 C 0.0074(6) 0.8339(6) 0.1534(4) 0.0582(18) Uani 1 1 d . . . H21A H 0.0002 0.9168 0.1712 0.070 Uiso 1 1 calc R . . C22 C 0.0309(5) 0.8187(6) 0.0881(4) 0.0565(17) Uani 1 1 d . . . H22A H 0.0404 0.8911 0.0610 0.068 Uiso 1 1 calc R . . C23 C 0.0405(5) 0.6987(6) 0.0627(3) 0.0512(16) Uani 1 1 d . . . H23A H 0.0571 0.6880 0.0182 0.061 Uiso 1 1 calc R . . C24 C 0.0262(5) 0.5928(6) 0.1021(4) 0.0477(15) Uani 1 1 d . . . H24A H 0.0317 0.5104 0.0832 0.057 Uiso 1 1 calc R . . C25 C -0.0922(5) 0.3563(6) 0.1440(3) 0.0434(14) Uani 1 1 d . . . C26 C -0.1802(5) 0.4116(6) 0.0890(3) 0.0495(15) Uani 1 1 d . . . H26A H -0.1919 0.5004 0.0914 0.059 Uiso 1 1 calc R . . C27 C -0.2503(6) 0.3435(7) 0.0316(4) 0.0569(16) Uani 1 1 d . . . H27A H -0.3094 0.3857 -0.0034 0.068 Uiso 1 1 calc R . . C28 C -0.2361(6) 0.2142(7) 0.0242(4) 0.0591(18) Uani 1 1 d . . . H28A H -0.2847 0.1667 -0.0151 0.071 Uiso 1 1 calc R . . C29 C -0.1492(6) 0.1570(6) 0.0758(4) 0.0567(17) Uani 1 1 d . . . H29A H -0.1362 0.0690 0.0709 0.068 Uiso 1 1 calc R . . C30 C -0.0810(5) 0.2231(5) 0.1339(3) 0.0458(15) Uani 1 1 d . . . H30A H -0.0237 0.1786 0.1692 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.04143(15) 0.04633(13) 0.04282(14) 0.00854(11) 0.01933(10) 0.00186(12) N1 0.039(3) 0.056(3) 0.059(3) 0.018(3) 0.012(3) -0.005(3) N2 0.058(4) 0.048(3) 0.040(3) 0.006(2) 0.012(3) -0.008(3) N3 0.043(3) 0.053(3) 0.041(3) 0.005(2) 0.013(2) 0.001(2) N4 0.041(3) 0.044(2) 0.040(3) 0.004(2) 0.012(2) -0.004(2) C1 0.043(4) 0.076(5) 0.093(6) 0.010(4) 0.023(4) -0.001(4) C2 0.037(4) 0.092(6) 0.121(8) 0.020(6) 0.014(5) -0.009(4) C3 0.063(6) 0.084(5) 0.081(6) 0.013(5) -0.014(5) -0.023(5) C4 0.056(5) 0.062(4) 0.059(5) 0.025(4) -0.004(4) -0.006(4) C5 0.082(6) 0.059(4) 0.047(4) 0.012(3) 0.000(4) -0.016(4) C6 0.077(5) 0.053(4) 0.043(4) 0.003(3) 0.021(4) -0.006(4) C7 0.040(4) 0.047(3) 0.041(3) 0.010(3) 0.004(3) -0.006(3) C8 0.045(4) 0.065(4) 0.052(4) 0.012(3) 0.015(3) 0.007(3) C9 0.048(4) 0.069(4) 0.050(4) 0.012(3) 0.014(3) 0.018(3) C10 0.059(4) 0.054(4) 0.046(4) 0.011(3) 0.008(3) 0.016(3) C11 0.047(4) 0.044(3) 0.037(3) 0.004(2) 0.008(3) 0.000(3) C12 0.056(4) 0.048(3) 0.048(4) 0.007(3) 0.008(3) -0.005(3) C13 0.049(4) 0.050(3) 0.047(4) -0.001(3) 0.014(3) -0.015(3) C14 0.047(4) 0.045(3) 0.030(3) 0.002(2) 0.007(3) -0.002(3) C15 0.042(4) 0.049(3) 0.043(3) 0.004(3) 0.014(3) 0.001(3) C16 0.050(4) 0.052(3) 0.037(3) 0.004(3) 0.019(3) 0.002(3) C17 0.048(4) 0.050(3) 0.047(4) 0.007(3) 0.024(3) 0.000(3) C18 0.040(3) 0.049(3) 0.043(3) 0.006(3) 0.013(3) 0.001(3) C19 0.037(3) 0.048(3) 0.043(4) 0.007(3) 0.013(3) 0.000(3) C20 0.051(4) 0.061(4) 0.045(4) 0.005(3) 0.018(3) 0.000(3) C21 0.059(4) 0.047(3) 0.066(5) 0.013(3) 0.018(4) 0.003(3) C22 0.052(4) 0.058(4) 0.059(4) 0.020(3) 0.017(3) -0.004(3) C23 0.044(4) 0.068(4) 0.048(4) 0.015(3) 0.023(3) 0.003(3) C24 0.036(3) 0.053(3) 0.055(4) 0.004(3) 0.016(3) 0.003(3) C25 0.044(4) 0.056(3) 0.038(3) 0.008(3) 0.023(3) 0.007(3) C26 0.053(4) 0.056(3) 0.045(4) 0.007(3) 0.025(3) 0.009(3) C27 0.050(4) 0.079(4) 0.044(4) 0.005(3) 0.019(3) 0.006(4) C28 0.062(5) 0.074(4) 0.049(4) -0.005(4) 0.027(4) -0.018(4) C29 0.075(5) 0.050(3) 0.053(4) 0.003(3) 0.033(4) -0.002(3) C30 0.049(4) 0.051(3) 0.046(4) 0.006(3) 0.028(3) 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 C19 1.995(6) . ? Pt1 C25 2.010(6) . ? Pt1 N3 2.163(5) . ? Pt1 N1 2.193(5) . ? N1 C7 1.341(8) . ? N1 C1 1.350(9) . ? N2 C7 1.377(8) . ? N2 C6 1.393(8) . ? N2 C15 1.452(8) . ? N3 C14 1.338(7) . ? N3 C8 1.356(8) . ? N4 C13 1.370(7) . ? N4 C14 1.371(7) . ? N4 C18 1.457(7) . ? C1 C2 1.389(11) . ? C2 C3 1.366(12) . ? C3 C4 1.375(11) . ? C4 C5 1.408(11) . ? C4 C7 1.424(9) . ? C5 C6 1.349(10) . ? C8 C9 1.375(8) . ? C9 C10 1.371(9) . ? C10 C11 1.398(9) . ? C11 C12 1.410(9) . ? C11 C14 1.426(7) . ? C12 C13 1.356(9) . ? C15 C16 1.513(8) . ? C16 C17 1.528(8) . ? C17 C18 1.522(8) . ? C19 C20 1.392(8) . ? C19 C24 1.414(8) . ? C20 C21 1.381(8) . ? C21 C22 1.388(9) . ? C22 C23 1.371(9) . ? C23 C24 1.390(8) . ? C25 C26 1.403(8) . ? C25 C30 1.428(8) . ? C26 C27 1.375(9) . ? C27 C28 1.386(10) . ? C28 C29 1.374(9) . ? C29 C30 1.363(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Pt1 C25 91.3(2) . . ? C19 Pt1 N3 170.6(2) . . ? C25 Pt1 N3 90.3(2) . . ? C19 Pt1 N1 87.5(2) . . ? C25 Pt1 N1 176.7(2) . . ? N3 Pt1 N1 90.40(18) . . ? C7 N1 C1 115.4(6) . . ? C7 N1 Pt1 131.2(4) . . ? C1 N1 Pt1 113.0(5) . . ? C7 N2 C6 108.1(5) . . ? C7 N2 C15 128.8(5) . . ? C6 N2 C15 123.0(6) . . ? C14 N3 C8 114.9(5) . . ? C14 N3 Pt1 130.7(4) . . ? C8 N3 Pt1 112.4(4) . . ? C13 N4 C14 107.7(5) . . ? C13 N4 C18 122.0(5) . . ? C14 N4 C18 130.2(5) . . ? N1 C1 C2 122.9(8) . . ? C3 C2 C1 120.2(8) . . ? C2 C3 C4 119.9(8) . . ? C3 C4 C5 136.6(8) . . ? C3 C4 C7 116.0(8) . . ? C5 C4 C7 107.4(7) . . ? C6 C5 C4 107.6(7) . . ? C5 C6 N2 110.0(7) . . ? N1 C7 N2 127.5(5) . . ? N1 C7 C4 125.6(7) . . ? N2 C7 C4 107.0(6) . . ? N3 C8 C9 125.1(7) . . ? C10 C9 C8 119.8(6) . . ? C9 C10 C11 117.9(6) . . ? C10 C11 C12 135.2(6) . . ? C10 C11 C14 118.1(6) . . ? C12 C11 C14 106.7(6) . . ? C13 C12 C11 106.8(5) . . ? C12 C13 N4 111.1(6) . . ? N3 C14 N4 128.3(5) . . ? N3 C14 C11 124.1(6) . . ? N4 C14 C11 107.6(5) . . ? N2 C15 C16 112.4(5) . . ? C15 C16 C17 110.0(5) . . ? C18 C17 C16 112.8(5) . . ? N4 C18 C17 112.3(5) . . ? C20 C19 C24 115.6(5) . . ? C20 C19 Pt1 123.2(5) . . ? C24 C19 Pt1 120.7(4) . . ? C21 C20 C19 123.0(6) . . ? C20 C21 C22 119.6(6) . . ? C23 C22 C21 119.7(6) . . ? C22 C23 C24 120.2(6) . . ? C23 C24 C19 121.8(6) . . ? C26 C25 C30 113.6(6) . . ? C26 C25 Pt1 123.9(5) . . ? C30 C25 Pt1 122.4(5) . . ? C27 C26 C25 123.2(6) . . ? C26 C27 C28 121.0(7) . . ? C29 C28 C27 117.6(7) . . ? C30 C29 C28 121.7(6) . . ? C29 C30 C25 122.7(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.784 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.135 # Attachment '5.cif' data_joy2a _database_code_depnum_ccdc_archive 'CCDC 697411' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H48 N4 Pt2 S2' _chemical_formula_weight 1099.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7088(15) _cell_length_b 12.9165(17) _cell_length_c 14.9862(19) _cell_angle_alpha 80.192(2) _cell_angle_beta 83.251(3) _cell_angle_gamma 63.096(2) _cell_volume 1989.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour light _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 7.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3282 _exptl_absorpt_correction_T_max 0.5343 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ApexII CCD 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 14309 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.2145 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9042 _reflns_number_gt 3316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9042 _refine_ls_number_parameters 470 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1638 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.808 _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 -0.00512(4) 0.22205(4) 0.76078(3) 0.06209(18) Uani 1 1 d D A 1 Pt2 Pt 0.50639(4) 0.31860(4) 0.75840(3) 0.05488(16) Uani 1 1 d D A 1 S1 S 0.0882(3) 0.0300(3) 0.8374(2) 0.0839(11) Uani 1 1 d D A 1 S2 S 0.5492(4) 0.3591(4) 0.60208(19) 0.1135(15) Uani 1 1 d D A 1 N1 N 0.0792(8) 0.2903(7) 0.9473(5) 0.062(3) Uani 1 1 d . A 1 N2 N -0.0963(7) 0.2810(7) 0.8859(5) 0.041(2) Uani 1 1 d . A 1 N3 N 0.1976(9) 0.5312(9) 0.7004(5) 0.052(3) Uani 1 1 d . A 1 N4 N 0.3992(8) 0.5036(7) 0.7463(5) 0.042(2) Uani 1 1 d . A 1 C1 C 0.1040(12) 0.2964(11) 1.0345(7) 0.089(4) Uani 1 1 d . A 1 H1A H 0.1811 0.2933 1.0517 0.107 Uiso 1 1 calc R A 1 C2 C 0.0017(11) 0.3075(10) 1.0901(7) 0.076(4) Uani 1 1 d . A 1 H2A H -0.0072 0.3173 1.1524 0.092 Uiso 1 1 calc R A 1 C3 C -0.0887(10) 0.3021(9) 1.0417(7) 0.046(3) Uani 1 1 d . A 1 C4 C -0.2054(10) 0.3044(8) 1.0630(7) 0.054(3) Uani 1 1 d . A 1 H4A H -0.2411 0.3098 1.1233 0.065 Uiso 1 1 calc R A 1 C5 C -0.2706(9) 0.2989(8) 0.9948(7) 0.047(3) Uani 1 1 d . A 1 H5A H -0.3543 0.3039 1.0069 0.056 Uiso 1 1 calc R A 1 C6 C -0.2150(9) 0.2864(8) 0.9101(6) 0.047(3) Uani 1 1 d . A 1 H6A H -0.2615 0.2809 0.8647 0.056 Uiso 1 1 calc R A 1 C7 C -0.0410(10) 0.2907(9) 0.9505(7) 0.043(3) Uani 1 1 d . A 1 C8 C 0.0990(12) 0.6245(14) 0.6638(7) 0.067(4) Uani 1 1 d . A 1 H8A H 0.0233 0.6223 0.6495 0.081 Uiso 1 1 calc R A 1 C9 C 0.1150(11) 0.7201(11) 0.6489(6) 0.065(4) Uani 1 1 d . A 1 H9A H 0.0568 0.7956 0.6224 0.078 Uiso 1 1 calc R A 1 C10 C 0.2337(11) 0.6880(12) 0.6796(7) 0.052(3) Uani 1 1 d . A 1 C11 C 0.3056(12) 0.7451(10) 0.6822(7) 0.072(4) Uani 1 1 d . A 1 H11A H 0.2748 0.8260 0.6600 0.086 Uiso 1 1 calc R A 1 C12 C 0.4230(12) 0.6830(11) 0.7176(7) 0.069(4) Uani 1 1 d . A 1 H12A H 0.4754 0.7210 0.7201 0.083 Uiso 1 1 calc R A 1 C13 C 0.4673(10) 0.5652(11) 0.7500(6) 0.061(3) Uani 1 1 d . A 1 H13A H 0.5488 0.5253 0.7761 0.073 Uiso 1 1 calc R A 1 C14 C 0.2854(12) 0.5689(12) 0.7123(6) 0.047(3) Uani 1 1 d . A 1 C15 C -0.0895(9) 0.3866(10) 0.6940(7) 0.052(3) Uani 1 1 d . A 1 C16 C -0.0873(13) 0.4153(13) 0.6007(9) 0.103(5) Uani 1 1 d . A 1 H16A H -0.0418 0.3550 0.5635 0.123 Uiso 1 1 calc R A 1 C17 C -0.1505(13) 0.5309(15) 0.5603(8) 0.093(5) Uani 1 1 d . A 1 H17A H -0.1493 0.5451 0.4959 0.111 Uiso 1 1 calc R A 1 C18 C -0.2124(11) 0.6229(12) 0.6052(9) 0.083(4) Uani 1 1 d . A 1 H18A H -0.2494 0.7012 0.5756 0.100 Uiso 1 1 calc R A 1 C19 C -0.2183(10) 0.5970(12) 0.6927(8) 0.065(4) Uani 1 1 d . A 1 H19A H -0.2640 0.6583 0.7289 0.078 Uiso 1 1 calc R A 1 C20 C -0.1611(10) 0.4848(11) 0.7342(7) 0.059(3) Uani 1 1 d . A 1 H20A H -0.1724 0.4737 0.7983 0.070 Uiso 1 1 calc R A 1 C21 C 0.0929(10) 0.1509(10) 0.6480(6) 0.078(4) Uani 1 1 d D A 1 C22 C 0.2159(12) 0.1448(12) 0.6303(8) 0.109(5) Uani 1 1 d . A 1 H22A H 0.2442 0.1816 0.6665 0.131 Uiso 1 1 calc R A 1 C23 C 0.2945(15) 0.0885(13) 0.5639(10) 0.134(7) Uani 1 1 d . A 1 H23A H 0.3789 0.0822 0.5537 0.161 Uiso 1 1 calc R A 1 C24 C 0.2487(16) 0.0411(13) 0.5120(9) 0.107(5) Uani 1 1 d . A 1 H24A H 0.2996 0.0080 0.4607 0.129 Uiso 1 1 calc R A 1 C25 C 0.1327(14) 0.0384(12) 0.5296(10) 0.110(5) Uani 1 1 d . A 1 H25A H 0.1038 0.0012 0.4943 0.132 Uiso 1 1 calc R A 1 C26 C 0.0632(13) 0.0913(12) 0.5997(9) 0.121(6) Uani 1 1 d . A 1 H26A H -0.0147 0.0854 0.6163 0.145 Uiso 1 1 calc R A 1 C27 C 0.6106(11) 0.1495(7) 0.7581(7) 0.071(5) Uani 1 1 d D A 1 C28 C 0.7340(15) 0.0920(12) 0.7698(9) 0.108(5) Uani 1 1 d . A 1 H28A H 0.7782 0.1335 0.7826 0.130 Uiso 1 1 calc R A 1 C29 C 0.8046(15) -0.0298(15) 0.7643(9) 0.122(5) Uiso 1 1 d . A 1 H29A H 0.8937 -0.0665 0.7745 0.146 Uiso 1 1 calc R A 1 C30 C 0.7503(15) -0.0955(12) 0.7450(9) 0.101(5) Uani 1 1 d . A 1 H30A H 0.8001 -0.1772 0.7433 0.121 Uiso 1 1 calc R A 1 C31 C 0.6264(16) -0.0444(14) 0.7285(8) 0.082(4) Uani 1 1 d . A 1 H31A H 0.5850 -0.0864 0.7120 0.099 Uiso 1 1 calc R A 1 C32 C 0.5585(11) 0.0791(16) 0.7371(7) 0.101(6) Uani 1 1 d . A 1 H32A H 0.4692 0.1161 0.7276 0.121 Uiso 1 1 calc R A 1 C33 C 0.4703(9) 0.2910(10) 0.8927(6) 0.043(3) Uani 1 1 d . A 1 C34 C 0.4949(10) 0.1870(10) 0.9444(7) 0.058(3) Uani 1 1 d . A 1 H34A H 0.5332 0.1187 0.9149 0.069 Uiso 1 1 calc R A 1 C35 C 0.4687(10) 0.1728(10) 1.0359(7) 0.059(3) Uani 1 1 d . A 1 H35A H 0.4882 0.0970 1.0677 0.071 Uiso 1 1 calc R A 1 C36 C 0.4154(9) 0.2667(11) 1.0805(7) 0.056(3) Uani 1 1 d . A 1 H36A H 0.3982 0.2565 1.1441 0.067 Uiso 1 1 calc R A 1 C37 C 0.3862(9) 0.3737(10) 1.0375(7) 0.053(3) Uani 1 1 d . A 1 H37A H 0.3487 0.4401 1.0692 0.064 Uiso 1 1 calc R A 1 C38 C 0.4135(8) 0.3854(9) 0.9410(6) 0.047(3) Uani 1 1 d . A 1 H38A H 0.3915 0.4616 0.9091 0.056 Uiso 1 1 calc R A 1 C39 C 0.1627(9) 0.2921(9) 0.8683(6) 0.068(3) Uani 1 1 d . A 1 H39A H 0.1480 0.2545 0.8214 0.081 Uiso 1 1 calc R A 1 H39B H 0.2531 0.2463 0.8852 0.081 Uiso 1 1 calc R A 1 C40 C 0.1394(8) 0.4178(10) 0.8288(6) 0.060(3) Uani 1 1 d . A 1 H40A H 0.0460 0.4695 0.8277 0.072 Uiso 1 1 calc R A 1 H40B H 0.1774 0.4477 0.8676 0.072 Uiso 1 1 calc R A 1 C41 C 0.1983(9) 0.4196(10) 0.7343(6) 0.068(4) Uani 1 1 d . A 1 H41A H 0.2878 0.3576 0.7341 0.082 Uiso 1 1 calc R A 1 H41B H 0.1503 0.4023 0.6936 0.082 Uiso 1 1 calc R A 1 C42A C 0.069(3) -0.051(3) 0.7634(18) 0.166(15) Uiso 0.45 1 d PD A 1 H42A H 0.0737 -0.1250 0.7970 0.249 Uiso 0.45 1 calc PR A 1 H42B H 0.1372 -0.0680 0.7156 0.249 Uiso 0.45 1 calc PR A 1 H42C H -0.0146 -0.0062 0.7362 0.249 Uiso 0.45 1 calc PR A 1 C42 C 0.012(3) 0.010(3) 0.9469(13) 0.163(12) Uiso 0.55 1 d PD . 1 C43 C 0.2506(11) -0.0263(11) 0.8392(9) 0.158(6) Uiso 1 1 d D A 1 H43A H 0.2876 -0.1119 0.8523 0.237 Uiso 1 1 calc R A 1 H43B H 0.2730 0.0046 0.8863 0.237 Uiso 1 1 calc R A 1 H43C H 0.2847 -0.0042 0.7801 0.237 Uiso 1 1 calc R A 1 C44 C 0.4811(13) 0.3016(14) 0.5431(7) 0.163(8) Uani 1 1 d D A 1 H44A H 0.5030 0.3140 0.4783 0.245 Uiso 1 1 calc R A 1 H44B H 0.3878 0.3402 0.5535 0.245 Uiso 1 1 calc R A 1 H44C H 0.5134 0.2175 0.5637 0.245 Uiso 1 1 calc R A 1 C45 C 0.7130(10) 0.2727(12) 0.5760(7) 0.144(7) Uani 1 1 d D A 1 H45A H 0.7321 0.2904 0.5114 0.216 Uiso 1 1 calc R A 1 H45B H 0.7327 0.1896 0.5902 0.216 Uiso 1 1 calc R A 1 H45C H 0.7654 0.2900 0.6120 0.216 Uiso 1 1 calc R A 1 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 0.0544(4) 0.0724(4) 0.0588(3) -0.0254(3) 0.0084(3) -0.0242(3) Pt2 0.0514(3) 0.0752(4) 0.0418(3) -0.0177(3) 0.0076(2) -0.0302(3) S1 0.085(3) 0.072(2) 0.072(2) -0.013(2) 0.0241(19) -0.021(2) S2 0.098(3) 0.217(5) 0.0459(19) -0.036(3) 0.019(2) -0.087(3) N1 0.054(7) 0.081(7) 0.048(6) -0.011(6) 0.007(5) -0.029(6) N2 0.031(5) 0.046(6) 0.036(5) -0.003(5) -0.002(4) -0.010(5) N3 0.032(6) 0.079(8) 0.037(5) -0.004(6) 0.005(4) -0.021(6) N4 0.038(6) 0.070(7) 0.027(5) -0.008(5) 0.004(4) -0.034(6) C1 0.093(11) 0.147(13) 0.058(8) -0.027(9) -0.016(8) -0.073(10) C2 0.068(10) 0.106(11) 0.043(7) -0.010(8) 0.000(7) -0.029(9) C3 0.038(7) 0.051(8) 0.047(7) -0.008(6) 0.001(6) -0.018(6) C4 0.056(8) 0.043(8) 0.048(7) 0.006(6) 0.014(6) -0.018(7) C5 0.037(7) 0.039(7) 0.065(7) -0.020(6) 0.016(6) -0.016(6) C6 0.044(7) 0.045(7) 0.051(7) -0.014(6) 0.001(5) -0.017(6) C7 0.045(8) 0.039(7) 0.040(7) 0.006(6) 0.000(6) -0.017(6) C8 0.047(9) 0.119(13) 0.031(7) -0.027(8) 0.001(6) -0.028(10) C9 0.052(9) 0.085(11) 0.036(7) 0.015(7) -0.010(6) -0.017(8) C10 0.041(8) 0.074(11) 0.039(7) 0.003(7) -0.012(6) -0.027(8) C11 0.063(10) 0.068(10) 0.053(8) 0.027(7) -0.017(7) -0.011(8) C12 0.090(11) 0.068(10) 0.069(8) 0.021(8) -0.022(7) -0.058(9) C13 0.059(8) 0.083(10) 0.039(6) 0.012(7) -0.019(6) -0.032(8) C14 0.049(9) 0.066(10) 0.032(6) -0.004(7) -0.002(6) -0.032(8) C15 0.050(7) 0.068(9) 0.037(6) -0.013(7) 0.010(6) -0.027(7) C16 0.138(14) 0.105(13) 0.076(11) -0.036(10) -0.009(10) -0.055(12) C17 0.104(13) 0.133(15) 0.030(7) 0.029(10) -0.021(7) -0.052(12) C18 0.067(10) 0.094(12) 0.078(11) -0.017(10) 0.016(8) -0.029(9) C19 0.053(9) 0.077(11) 0.054(8) -0.016(8) 0.014(7) -0.021(8) C20 0.045(8) 0.067(9) 0.060(8) -0.015(8) 0.010(7) -0.022(8) C21 0.046(8) 0.081(10) 0.075(9) -0.048(8) 0.005(7) 0.010(7) C22 0.089(11) 0.174(15) 0.089(10) -0.071(10) 0.054(9) -0.076(11) C23 0.177(17) 0.140(15) 0.121(13) -0.091(12) 0.085(12) -0.097(13) C24 0.126(14) 0.094(12) 0.057(9) -0.024(8) 0.040(9) -0.015(11) C25 0.088(12) 0.114(13) 0.093(11) -0.062(10) -0.028(9) 0.008(11) C26 0.108(12) 0.130(14) 0.118(12) -0.100(11) -0.012(10) -0.016(10) C27 0.062(10) 0.147(15) 0.042(7) -0.021(8) -0.002(6) -0.075(11) C28 0.102(12) 0.080(11) 0.173(14) -0.058(10) -0.031(11) -0.047(10) C30 0.077(11) 0.078(11) 0.136(13) -0.036(10) 0.008(10) -0.019(10) C31 0.096(13) 0.099(13) 0.069(9) -0.022(9) 0.009(9) -0.057(11) C32 0.037(9) 0.150(15) 0.039(7) 0.024(10) -0.004(6) 0.013(10) C33 0.035(7) 0.063(8) 0.035(6) -0.010(6) 0.000(5) -0.024(6) C34 0.076(9) 0.063(9) 0.044(7) -0.007(7) -0.004(6) -0.039(8) C35 0.076(9) 0.062(9) 0.050(7) -0.001(7) -0.003(7) -0.043(8) C36 0.062(8) 0.073(10) 0.031(6) -0.003(7) 0.002(6) -0.030(8) C37 0.050(8) 0.062(9) 0.043(7) -0.010(7) -0.002(6) -0.020(7) C38 0.042(7) 0.058(8) 0.032(6) -0.003(6) -0.012(5) -0.014(6) C39 0.053(8) 0.094(10) 0.069(8) -0.023(8) 0.022(6) -0.045(8) C40 0.026(6) 0.107(10) 0.056(7) -0.018(7) -0.004(5) -0.033(7) C41 0.049(8) 0.125(12) 0.050(7) -0.039(8) 0.017(6) -0.051(8) C44 0.160(16) 0.35(2) 0.065(9) -0.075(12) 0.038(9) -0.175(17) C45 0.094(12) 0.30(2) 0.077(9) -0.085(12) 0.034(8) -0.106(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 C15 2.026(11) . ? Pt1 C21 2.035(7) . ? Pt1 N2 2.125(7) . ? Pt1 S1 2.353(3) . ? Pt2 C27 1.962(8) . ? Pt2 C33 2.013(9) . ? Pt2 N4 2.124(8) . ? Pt2 S2 2.357(3) . ? S1 C43 1.702(11) . ? S1 C42A 1.746(17) . ? S1 C42 1.809(15) . ? S2 C44 1.700(9) . ? S2 C45 1.765(10) . ? N1 C1 1.394(11) . ? N1 C7 1.400(11) . ? N1 C39 1.449(10) . ? N2 C7 1.278(10) . ? N2 C6 1.369(9) . ? N3 C8 1.323(12) . ? N3 C14 1.361(11) . ? N3 C41 1.441(12) . ? N4 C14 1.320(12) . ? N4 C13 1.368(11) . ? C1 C2 1.343(12) . ? C2 C3 1.384(12) . ? C3 C4 1.354(11) . ? C3 C7 1.420(11) . ? C4 C5 1.375(11) . ? C5 C6 1.357(10) . ? C8 C9 1.310(13) . ? C9 C10 1.371(13) . ? C10 C11 1.354(13) . ? C10 C14 1.394(13) . ? C11 C12 1.358(13) . ? C12 C13 1.383(13) . ? C15 C20 1.362(12) . ? C15 C16 1.385(14) . ? C16 C17 1.394(15) . ? C17 C18 1.329(15) . ? C18 C19 1.299(13) . ? C19 C20 1.358(13) . ? C21 C26 1.314(13) . ? C21 C22 1.402(13) . ? C22 C23 1.338(13) . ? C23 C24 1.351(17) . ? C24 C25 1.368(16) . ? C25 C26 1.331(14) . ? C27 C28 1.309(14) . ? C27 C32 1.393(16) . ? C28 C29 1.420(16) . ? C29 C30 1.350(15) . ? C30 C31 1.328(15) . ? C31 C32 1.447(16) . ? C33 C34 1.355(12) . ? C33 C38 1.380(11) . ? C34 C35 1.369(11) . ? C35 C36 1.341(11) . ? C36 C37 1.327(12) . ? C37 C38 1.441(11) . ? C39 C40 1.539(12) . ? C40 C41 1.502(11) . ? C42 C42 1.58(3) 2_557 ? 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 C15 Pt1 C21 93.8(4) . . ? C15 Pt1 N2 91.5(4) . . ? C21 Pt1 N2 174.5(4) . . ? C15 Pt1 S1 178.4(3) . . ? C21 Pt1 S1 86.1(3) . . ? N2 Pt1 S1 88.5(2) . . ? C27 Pt2 C33 89.8(4) . . ? C27 Pt2 N4 174.8(3) . . ? C33 Pt2 N4 95.3(4) . . ? C27 Pt2 S2 92.4(3) . . ? C33 Pt2 S2 177.3(3) . . ? N4 Pt2 S2 82.5(2) . . ? C43 S1 C42A 102.4(11) . . ? C43 S1 C42 113.6(11) . . ? C42A S1 C42 109.7(13) . . ? C43 S1 Pt1 112.4(5) . . ? C42A S1 Pt1 102.7(11) . . ? C42 S1 Pt1 114.7(10) . . ? C44 S2 C45 100.4(6) . . ? C44 S2 Pt2 109.1(4) . . ? C45 S2 Pt2 109.0(4) . . ? C1 N1 C7 108.2(8) . . ? C1 N1 C39 123.8(9) . . ? C7 N1 C39 127.9(9) . . ? C7 N2 C6 113.9(8) . . ? C7 N2 Pt1 125.3(7) . . ? C6 N2 Pt1 119.3(6) . . ? C8 N3 C14 105.9(11) . . ? C8 N3 C41 125.2(11) . . ? C14 N3 C41 128.1(11) . . ? C14 N4 C13 113.2(10) . . ? C14 N4 Pt2 128.1(8) . . ? C13 N4 Pt2 116.0(8) . . ? C2 C1 N1 109.2(10) . . ? C1 C2 C3 108.6(10) . . ? C4 C3 C2 134.3(10) . . ? C4 C3 C7 117.2(10) . . ? C2 C3 C7 108.4(9) . . ? C3 C4 C5 118.0(9) . . ? C6 C5 C4 119.8(9) . . ? C5 C6 N2 124.2(9) . . ? N2 C7 N1 127.7(9) . . ? N2 C7 C3 126.8(10) . . ? N1 C7 C3 105.5(9) . . ? C9 C8 N3 114.1(12) . . ? C8 C9 C10 105.2(12) . . ? C11 C10 C9 134.2(15) . . ? C11 C10 C14 118.1(12) . . ? C9 C10 C14 107.7(11) . . ? C10 C11 C12 117.9(12) . . ? C11 C12 C13 120.8(11) . . ? N4 C13 C12 123.1(10) . . ? N4 C14 N3 126.1(12) . . ? N4 C14 C10 126.9(11) . . ? N3 C14 C10 107.0(11) . . ? C20 C15 C16 110.0(11) . . ? C20 C15 Pt1 124.9(9) . . ? C16 C15 Pt1 125.0(10) . . ? C15 C16 C17 121.2(12) . . ? C18 C17 C16 124.8(12) . . ? C19 C18 C17 114.6(13) . . ? C18 C19 C20 122.1(12) . . ? C19 C20 C15 127.2(11) . . ? C26 C21 C22 115.9(10) . . ? C26 C21 Pt1 126.3(10) . . ? C22 C21 Pt1 116.5(9) . . ? C23 C22 C21 121.8(12) . . ? C22 C23 C24 117.2(15) . . ? C23 C24 C25 123.3(13) . . ? C26 C25 C24 115.5(14) . . ? C21 C26 C25 125.7(15) . . ? C28 C27 C32 112.7(10) . . ? C28 C27 Pt2 125.9(9) . . ? C32 C27 Pt2 121.2(10) . . ? C27 C28 C29 122.9(12) . . ? C30 C29 C28 122.7(15) . . ? C31 C30 C29 119.1(15) . . ? C30 C31 C32 115.9(13) . . ? C27 C32 C31 126.7(12) . . ? C34 C33 C38 113.5(8) . . ? C34 C33 Pt2 127.2(8) . . ? C38 C33 Pt2 119.3(8) . . ? C33 C34 C35 125.0(10) . . ? C36 C35 C34 119.5(10) . . ? C37 C36 C35 121.4(10) . . ? C36 C37 C38 117.5(10) . . ? C33 C38 C37 123.1(9) . . ? N1 C39 C40 111.8(8) . . ? C41 C40 C39 110.1(9) . . ? N3 C41 C40 111.9(8) . . ? C42 C42 S1 161(3) 2_557 . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.188 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.132 # Attachment '6new.cif' data_zs131b _database_code_depnum_ccdc_archive 'CCDC 697412' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 N4 Pt1' _chemical_formula_weight 501.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9960(11) _cell_length_b 9.6192(13) _cell_length_c 11.9856(16) _cell_angle_alpha 84.184(2) _cell_angle_beta 72.328(2) _cell_angle_gamma 87.362(2) _cell_volume 873.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 8.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2963 _exptl_absorpt_correction_T_max 0.5004 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 6093 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3768 _reflns_number_gt 3130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3768 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 0.25445(3) 0.83962(3) 0.26479(2) 0.02710(8) Uani 1 1 d . . . C1 C 0.2749(7) 0.8789(7) 0.4229(5) 0.0373(15) Uani 1 1 d . . . H1A H 0.3656 0.9487 0.4114 0.056 Uiso 1 1 calc R . . H1B H 0.3069 0.7925 0.4628 0.056 Uiso 1 1 calc R . . H1C H 0.1621 0.9147 0.4711 0.056 Uiso 1 1 calc R . . C2 C 0.3682(7) 1.0245(6) 0.1930(6) 0.0378(15) Uani 1 1 d . . . H2A H 0.2783 1.0989 0.2045 0.057 Uiso 1 1 calc R . . H2B H 0.4254 1.0195 0.1086 0.057 Uiso 1 1 calc R . . H2C H 0.4558 1.0445 0.2310 0.057 Uiso 1 1 calc R . . C3 C 0.2619(8) 0.5285(7) 0.3178(5) 0.0333(14) Uani 1 1 d . . . H3A H 0.3814 0.5494 0.3059 0.040 Uiso 1 1 calc R . . C4 C 0.2194(8) 0.3900(6) 0.3208(5) 0.0369(15) Uani 1 1 d . . . H4A H 0.3087 0.3197 0.3113 0.044 Uiso 1 1 calc R . . C5 C 0.0462(8) 0.3533(7) 0.3378(5) 0.0373(15) Uani 1 1 d . . . H5A H 0.0155 0.2590 0.3383 0.045 Uiso 1 1 calc R . . C6 C -0.0793(7) 0.4595(6) 0.3537(5) 0.0294(13) Uani 1 1 d . . . C7 C -0.2636(8) 0.4685(7) 0.3734(5) 0.0403(16) Uani 1 1 d . . . H7A H -0.3389 0.3930 0.3786 0.048 Uiso 1 1 calc R . . C8 C -0.3121(7) 0.6042(7) 0.3835(5) 0.0363(15) Uani 1 1 d . . . H8A H -0.4291 0.6393 0.3982 0.044 Uiso 1 1 calc R . . C9 C -0.0225(7) 0.5988(6) 0.3507(4) 0.0270(13) Uani 1 1 d . . . C10 C 0.3671(7) 0.7088(7) 0.0346(5) 0.0356(14) Uani 1 1 d . . . H10A H 0.4771 0.7105 0.0494 0.043 Uiso 1 1 calc R . . C11 C 0.3557(8) 0.6299(7) -0.0519(5) 0.0373(15) Uani 1 1 d . . . H11A H 0.4565 0.5808 -0.0952 0.045 Uiso 1 1 calc R . . C12 C 0.1997(8) 0.6213(7) -0.0762(5) 0.0369(15) Uani 1 1 d . . . H12A H 0.1893 0.5637 -0.1335 0.044 Uiso 1 1 calc R . . C13 C 0.0580(7) 0.6991(6) -0.0146(5) 0.0309(13) Uani 1 1 d . . . C14 C -0.1178(8) 0.7246(7) -0.0168(5) 0.0392(16) Uani 1 1 d . . . H14A H -0.1747 0.6833 -0.0639 0.047 Uiso 1 1 calc R . . C15 C -0.1878(8) 0.8189(7) 0.0613(6) 0.0402(16) Uani 1 1 d . . . H15A H -0.3036 0.8566 0.0761 0.048 Uiso 1 1 calc R . . C16 C 0.0826(7) 0.7820(6) 0.0705(5) 0.0274(13) Uani 1 1 d . . . C17 C -0.1823(7) 0.8292(7) 0.3990(5) 0.0343(14) Uani 1 1 d . . . H17A H -0.0674 0.8589 0.4028 0.041 Uiso 1 1 calc R . . H17B H -0.2680 0.8338 0.4780 0.041 Uiso 1 1 calc R . . C18 C -0.2414(7) 0.9317(6) 0.3107(5) 0.0360(15) Uani 1 1 d . . . H18A H -0.3433 0.8915 0.2954 0.043 Uiso 1 1 calc R . . H18B H -0.2819 1.0196 0.3476 0.043 Uiso 1 1 calc R . . C19 C -0.1038(7) 0.9669(6) 0.1941(5) 0.0323(14) Uani 1 1 d . . . H19A H -0.1428 1.0512 0.1536 0.039 Uiso 1 1 calc R . . H19B H 0.0069 0.9894 0.2087 0.039 Uiso 1 1 calc R . . N1 N 0.1448(6) 0.6358(5) 0.3307(4) 0.0290(11) Uani 1 1 d . . . N2 N -0.1664(6) 0.6851(5) 0.3691(4) 0.0293(11) Uani 1 1 d . . . N3 N 0.2326(6) 0.7845(5) 0.1004(4) 0.0273(11) Uani 1 1 d . . . N4 N -0.0695(6) 0.8538(5) 0.1170(4) 0.0300(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02479(12) 0.02550(14) 0.03206(13) -0.00535(9) -0.00937(9) 0.00024(8) C1 0.028(3) 0.046(4) 0.038(4) -0.012(3) -0.006(3) -0.002(3) C2 0.032(3) 0.032(4) 0.050(4) 0.003(3) -0.016(3) 0.000(3) C3 0.033(3) 0.036(4) 0.031(3) -0.003(3) -0.010(3) 0.006(3) C4 0.039(3) 0.025(4) 0.044(4) -0.002(3) -0.008(3) 0.005(3) C5 0.046(4) 0.031(4) 0.034(4) -0.003(3) -0.009(3) -0.006(3) C6 0.033(3) 0.032(4) 0.023(3) -0.001(3) -0.007(2) -0.006(3) C7 0.035(3) 0.049(5) 0.036(4) -0.002(3) -0.008(3) -0.015(3) C8 0.027(3) 0.045(4) 0.036(4) -0.005(3) -0.007(3) -0.005(3) C9 0.030(3) 0.031(4) 0.019(3) -0.001(2) -0.006(2) 0.001(3) C10 0.030(3) 0.036(4) 0.040(4) -0.004(3) -0.009(3) -0.001(3) C11 0.042(4) 0.036(4) 0.029(3) -0.007(3) -0.003(3) 0.002(3) C12 0.054(4) 0.030(4) 0.027(3) -0.003(3) -0.012(3) -0.007(3) C13 0.040(3) 0.026(3) 0.029(3) 0.001(3) -0.014(3) 0.000(3) C14 0.042(4) 0.041(4) 0.042(4) -0.004(3) -0.022(3) -0.007(3) C15 0.031(3) 0.047(5) 0.048(4) -0.001(3) -0.021(3) -0.003(3) C16 0.028(3) 0.023(3) 0.029(3) 0.005(2) -0.008(2) -0.001(2) C17 0.029(3) 0.044(4) 0.030(3) -0.009(3) -0.008(3) 0.007(3) C18 0.032(3) 0.030(4) 0.046(4) -0.011(3) -0.011(3) 0.005(3) C19 0.031(3) 0.027(4) 0.040(4) -0.004(3) -0.012(3) 0.001(3) N1 0.025(2) 0.033(3) 0.030(3) -0.002(2) -0.008(2) 0.001(2) N2 0.026(2) 0.033(3) 0.028(3) -0.003(2) -0.006(2) -0.001(2) N3 0.025(2) 0.026(3) 0.027(3) 0.002(2) -0.003(2) -0.005(2) N4 0.027(2) 0.034(3) 0.032(3) -0.004(2) -0.013(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C2 2.023(6) . ? Pt1 C1 2.025(5) . ? Pt1 N3 2.150(4) . ? Pt1 N1 2.159(5) . ? C3 N1 1.349(7) . ? C3 C4 1.384(8) . ? C4 C5 1.394(8) . ? C5 C6 1.384(8) . ? C6 C7 1.420(8) . ? C6 C9 1.427(8) . ? C7 C8 1.352(9) . ? C8 N2 1.388(7) . ? C9 N1 1.344(6) . ? C9 N2 1.362(7) . ? C10 N3 1.356(7) . ? C10 C11 1.371(8) . ? C11 C12 1.372(8) . ? C12 C13 1.384(8) . ? C13 C16 1.420(8) . ? C13 C14 1.423(8) . ? C14 C15 1.349(9) . ? C15 N4 1.383(6) . ? C16 N3 1.354(6) . ? C16 N4 1.363(7) . ? C17 N2 1.457(7) . ? C17 C18 1.538(8) . ? C18 C19 1.510(8) . ? C19 N4 1.460(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt1 C1 89.9(3) . . ? C2 Pt1 N3 93.3(2) . . ? C1 Pt1 N3 176.5(2) . . ? C2 Pt1 N1 176.0(2) . . ? C1 Pt1 N1 93.0(2) . . ? N3 Pt1 N1 83.75(17) . . ? N1 C3 C4 124.3(5) . . ? C3 C4 C5 120.3(6) . . ? C6 C5 C4 117.5(6) . . ? C5 C6 C7 135.7(6) . . ? C5 C6 C9 117.9(5) . . ? C7 C6 C9 106.3(5) . . ? C8 C7 C6 107.4(5) . . ? C7 C8 N2 110.2(5) . . ? N1 C9 N2 127.0(5) . . ? N1 C9 C6 125.0(5) . . ? N2 C9 C6 107.9(5) . . ? N3 C10 C11 124.7(5) . . ? C10 C11 C12 120.4(6) . . ? C11 C12 C13 118.0(6) . . ? C12 C13 C16 118.0(5) . . ? C12 C13 C14 135.6(5) . . ? C16 C13 C14 106.4(5) . . ? C15 C14 C13 106.5(5) . . ? C14 C15 N4 111.4(5) . . ? N3 C16 N4 126.9(5) . . ? N3 C16 C13 124.5(5) . . ? N4 C16 C13 108.5(4) . . ? N2 C17 C18 113.4(5) . . ? C19 C18 C17 115.7(5) . . ? N4 C19 C18 113.3(5) . . ? C9 N1 C3 114.9(5) . . ? C9 N1 Pt1 126.7(4) . . ? C3 N1 Pt1 115.4(4) . . ? C9 N2 C8 108.1(5) . . ? C9 N2 C17 128.1(4) . . ? C8 N2 C17 122.1(5) . . ? C16 N3 C10 114.2(5) . . ? C16 N3 Pt1 126.2(4) . . ? C10 N3 Pt1 116.9(3) . . ? C16 N4 C15 107.1(5) . . ? C16 N4 C19 129.6(4) . . ? C15 N4 C19 122.3(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.738 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.154 # Attachment '7.cif' data_zs123 _database_code_depnum_ccdc_archive 'CCDC 697413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 N4 Pt' _chemical_formula_weight 515.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0310(7) _cell_length_b 10.7070(8) _cell_length_c 13.8631(11) _cell_angle_alpha 82.4630(10) _cell_angle_beta 85.1300(10) _cell_angle_gamma 83.6180(10) _cell_volume 1171.44(16) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yello' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 5.997 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2663 _exptl_absorpt_correction_T_max 0.3801 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7432 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4542 _reflns_number_gt 4131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0160P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4542 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0407 _refine_ls_wR_factor_gt 0.0405 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 0.031347(16) 0.139313(10) 0.292349(9) 0.02217(4) Uani 1 1 d . . . N1 N 0.0181(3) 0.3413(2) 0.29564(19) 0.0272(6) Uani 1 1 d . . . N2 N -0.1693(4) 0.3816(2) 0.4397(2) 0.0299(7) Uani 1 1 d . . . N3 N -0.0904(3) 0.1648(2) 0.15669(18) 0.0238(6) Uani 1 1 d . . . N4 N -0.3853(4) 0.1430(3) 0.20871(19) 0.0301(6) Uani 1 1 d . . . C1 C 0.1132(5) 0.4011(3) 0.2237(2) 0.0334(8) Uani 1 1 d . . . H1A H 0.1752 0.3516 0.1782 0.040 Uiso 1 1 calc R . . C2 C 0.1274(5) 0.5312(3) 0.2110(3) 0.0394(9) Uani 1 1 d . . . H2A H 0.1963 0.5676 0.1580 0.047 Uiso 1 1 calc R . . C3 C 0.0413(5) 0.6064(3) 0.2756(3) 0.0385(9) Uani 1 1 d . . . H3A H 0.0493 0.6950 0.2681 0.046 Uiso 1 1 calc R . . C4 C -0.0569(5) 0.5497(3) 0.3516(3) 0.0318(8) Uani 1 1 d . . . C5 C -0.1602(5) 0.5928(3) 0.4312(3) 0.0401(10) Uani 1 1 d . . . H5A H -0.1799 0.6776 0.4460 0.048 Uiso 1 1 calc R . . C6 C -0.2254(5) 0.4908(3) 0.4820(3) 0.0381(9) Uani 1 1 d . . . H6A H -0.2996 0.4934 0.5390 0.046 Uiso 1 1 calc R . . C7 C -0.0647(4) 0.4165(3) 0.3592(2) 0.0269(8) Uani 1 1 d . . . C8 C 0.0135(5) 0.1760(3) 0.0748(2) 0.0323(8) Uani 1 1 d . . . H8A H 0.1287 0.1826 0.0821 0.039 Uiso 1 1 calc R . . C9 C -0.0354(5) 0.1787(3) -0.0188(2) 0.0358(9) Uani 1 1 d . . . H9A H 0.0454 0.1863 -0.0729 0.043 Uiso 1 1 calc R . . C10 C -0.2013(5) 0.1705(3) -0.0337(3) 0.0367(9) Uani 1 1 d . . . H10A H -0.2366 0.1725 -0.0976 0.044 Uiso 1 1 calc R . . C11 C -0.3143(4) 0.1592(3) 0.0466(2) 0.0299(8) Uani 1 1 d . . . C12 C -0.4892(5) 0.1487(3) 0.0624(3) 0.0403(9) Uani 1 1 d . . . H12A H -0.5656 0.1486 0.0137 0.048 Uiso 1 1 calc R . . C13 C -0.5263(5) 0.1390(3) 0.1596(3) 0.0416(9) Uani 1 1 d . . . H13A H -0.6355 0.1305 0.1902 0.050 Uiso 1 1 calc R . . C14 C -0.2506(4) 0.1559(3) 0.1405(2) 0.0269(8) Uani 1 1 d . . . C15 C -0.3838(5) 0.1349(3) 0.3151(2) 0.0313(8) Uani 1 1 d . . . H15A H -0.2687 0.1056 0.3344 0.038 Uiso 1 1 calc R . . H15B H -0.4590 0.0716 0.3460 0.038 Uiso 1 1 calc R . . C16 C -0.4400(5) 0.2611(3) 0.3520(2) 0.0334(8) Uani 1 1 d . . . H16A H -0.5610 0.2841 0.3430 0.040 Uiso 1 1 calc R . . H16B H -0.3768 0.3279 0.3141 0.040 Uiso 1 1 calc R . . C17 C -0.4093(4) 0.2533(3) 0.4603(2) 0.0361(9) Uani 1 1 d . . . H17A H -0.4783 0.3241 0.4883 0.043 Uiso 1 1 calc R . . H17B H -0.4468 0.1732 0.4947 0.043 Uiso 1 1 calc R . . C18 C -0.2262(4) 0.2589(3) 0.4783(2) 0.0331(8) Uani 1 1 d . . . H18A H -0.2124 0.2430 0.5493 0.040 Uiso 1 1 calc R . . H18B H -0.1556 0.1915 0.4469 0.040 Uiso 1 1 calc R . . C19 C 0.1650(4) 0.1040(3) 0.4128(2) 0.0280(8) Uani 1 1 d . . . H19A H 0.0933 0.0701 0.4687 0.042 Uiso 1 1 calc R . . H19B H 0.2043 0.1829 0.4266 0.042 Uiso 1 1 calc R . . H19C H 0.2618 0.0422 0.4013 0.042 Uiso 1 1 calc R . . C20 C 0.0535(5) -0.0505(3) 0.2859(2) 0.0322(8) Uani 1 1 d . . . H20A H -0.0016 -0.0929 0.3450 0.048 Uiso 1 1 calc R . . H20B H 0.1727 -0.0825 0.2809 0.048 Uiso 1 1 calc R . . H20C H 0.0002 -0.0676 0.2286 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02278(8) 0.01931(6) 0.02406(7) -0.00336(5) 0.00060(5) -0.00152(5) N1 0.0291(17) 0.0230(13) 0.0294(16) -0.0041(12) -0.0025(13) -0.0013(12) N2 0.0312(18) 0.0266(14) 0.0316(16) -0.0081(12) -0.0033(13) 0.0041(13) N3 0.0240(16) 0.0233(13) 0.0232(15) -0.0007(11) 0.0015(12) -0.0033(12) N4 0.0227(16) 0.0410(16) 0.0260(16) -0.0011(13) -0.0011(13) -0.0048(13) C1 0.043(2) 0.0273(17) 0.030(2) -0.0037(15) 0.0038(17) -0.0078(16) C2 0.050(3) 0.0265(17) 0.041(2) 0.0007(16) -0.0006(19) -0.0108(17) C3 0.049(3) 0.0221(17) 0.046(2) -0.0028(16) -0.013(2) -0.0055(17) C4 0.036(2) 0.0219(16) 0.039(2) -0.0083(15) -0.0138(17) 0.0043(15) C5 0.044(2) 0.0302(18) 0.048(2) -0.0153(17) -0.0147(19) 0.0089(17) C6 0.038(2) 0.042(2) 0.035(2) -0.0177(17) -0.0059(18) 0.0100(18) C7 0.031(2) 0.0225(15) 0.0275(19) -0.0033(14) -0.0090(16) 0.0018(15) C8 0.030(2) 0.0353(18) 0.030(2) -0.0031(15) 0.0021(16) -0.0011(16) C9 0.039(2) 0.042(2) 0.0252(19) -0.0059(16) 0.0052(17) -0.0019(18) C10 0.049(3) 0.0333(18) 0.028(2) -0.0041(15) -0.0086(18) 0.0003(18) C11 0.029(2) 0.0311(17) 0.0287(19) -0.0037(14) -0.0040(16) 0.0005(15) C12 0.034(2) 0.051(2) 0.037(2) -0.0071(18) -0.0111(18) -0.0012(19) C13 0.029(2) 0.050(2) 0.047(2) -0.0048(18) -0.0058(18) -0.0069(18) C14 0.032(2) 0.0227(15) 0.0264(18) -0.0045(13) 0.0002(16) -0.0023(15) C15 0.027(2) 0.0353(18) 0.0296(19) 0.0003(15) 0.0015(16) -0.0015(16) C16 0.028(2) 0.0352(18) 0.036(2) -0.0033(16) 0.0009(16) -0.0004(16) C17 0.032(2) 0.0399(19) 0.034(2) -0.0073(16) 0.0075(17) 0.0017(17) C18 0.039(2) 0.0323(18) 0.0248(19) -0.0021(14) 0.0046(16) 0.0034(16) C19 0.0222(19) 0.0297(16) 0.0326(19) -0.0031(14) -0.0009(15) -0.0065(15) C20 0.039(2) 0.0239(16) 0.034(2) -0.0065(14) -0.0013(17) -0.0010(15) _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 C19 2.033(3) . ? Pt1 C20 2.034(3) . ? Pt1 N1 2.160(2) . ? Pt1 N3 2.165(3) . ? N1 C1 1.341(4) . ? N1 C7 1.354(4) . ? N2 C7 1.376(4) . ? N2 C6 1.389(4) . ? N2 C18 1.459(4) . ? N3 C14 1.340(4) . ? N3 C8 1.351(4) . ? N4 C13 1.377(4) . ? N4 C14 1.382(4) . ? N4 C15 1.467(4) . ? C1 C2 1.397(4) . ? C2 C3 1.374(5) . ? C3 C4 1.378(5) . ? C4 C5 1.418(5) . ? C4 C7 1.424(4) . ? C5 C6 1.351(5) . ? C8 C9 1.384(5) . ? C9 C10 1.380(5) . ? C10 C11 1.377(5) . ? C11 C12 1.417(5) . ? C11 C14 1.433(4) . ? C12 C13 1.349(5) . ? C15 C16 1.516(4) . ? C16 C17 1.531(5) . ? C17 C18 1.521(5) . ? 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 C19 Pt1 C20 88.13(13) . . ? C19 Pt1 N1 91.72(11) . . ? C20 Pt1 N1 177.54(12) . . ? C19 Pt1 N3 174.07(11) . . ? C20 Pt1 N3 88.13(11) . . ? N1 Pt1 N3 91.82(9) . . ? C1 N1 C7 115.0(3) . . ? C1 N1 Pt1 113.8(2) . . ? C7 N1 Pt1 131.2(2) . . ? C7 N2 C6 107.1(3) . . ? C7 N2 C18 130.8(2) . . ? C6 N2 C18 122.0(3) . . ? C14 N3 C8 114.0(3) . . ? C14 N3 Pt1 130.0(2) . . ? C8 N3 Pt1 115.4(2) . . ? C13 N4 C14 108.0(3) . . ? C13 N4 C15 124.6(3) . . ? C14 N4 C15 127.4(3) . . ? N1 C1 C2 124.6(3) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C4 118.2(3) . . ? C3 C4 C5 134.9(3) . . ? C3 C4 C7 118.5(3) . . ? C5 C4 C7 106.6(3) . . ? C6 C5 C4 107.2(3) . . ? C5 C6 N2 110.9(3) . . ? N1 C7 N2 127.8(3) . . ? N1 C7 C4 124.0(3) . . ? N2 C7 C4 108.2(3) . . ? N3 C8 C9 124.8(3) . . ? C10 C9 C8 120.1(3) . . ? C11 C10 C9 118.2(3) . . ? C10 C11 C12 135.5(3) . . ? C10 C11 C14 117.4(3) . . ? C12 C11 C14 107.1(3) . . ? C13 C12 C11 106.9(3) . . ? C12 C13 N4 111.2(3) . . ? N3 C14 N4 127.7(3) . . ? N3 C14 C11 125.5(3) . . ? N4 C14 C11 106.8(3) . . ? N4 C15 C16 112.2(3) . . ? C15 C16 C17 110.1(3) . . ? C18 C17 C16 113.3(3) . . ? N2 C18 C17 111.6(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.229 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.087 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.022 0.500 0.000 317.0 86.2 _platon_squeeze_details ; Disordered THF solvent molcules were removed by squeeze. ; # Attachment '8.cif' data_sdt36 _database_code_depnum_ccdc_archive 'CCDC 697414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 N4 Pt' _chemical_formula_weight 659.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.778(2) _cell_length_b 9.984(2) _cell_length_c 13.777(3) _cell_angle_alpha 103.297(4) _cell_angle_beta 96.241(4) _cell_angle_gamma 115.883(3) _cell_volume 1260.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 5.595 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2131 _exptl_absorpt_correction_T_max 0.2846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 8109 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4909 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4909 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.2071 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _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 0.53016(3) 0.72411(3) 0.19734(2) 0.0338(2) Uani 1 1 d . . . N1 N 0.8842(10) 1.0063(10) 0.3186(7) 0.0468(19) Uani 1 1 d . . . N2 N 0.7331(10) 0.8064(11) 0.1571(7) 0.0412(19) Uani 1 1 d . . . N3 N 0.4761(9) 1.0610(9) 0.2146(6) 0.0419(17) Uani 1 1 d . . . N4 N 0.4393(9) 0.8114(11) 0.0957(6) 0.0363(17) Uani 1 1 d . . . C1 C 1.0233(12) 1.0634(13) 0.3727(10) 0.057(3) Uani 1 1 d . . . H1A H 1.0651 1.1356 0.4381 0.069 Uiso 1 1 calc R . . C2 C 1.0898(11) 0.9958(15) 0.3136(10) 0.061(3) Uani 1 1 d . . . H2A H 1.1827 1.0140 0.3318 0.073 Uiso 1 1 calc R . . C3 C 0.9884(12) 0.8936(14) 0.2201(10) 0.056(3) Uani 1 1 d . . . C4 C 0.9869(13) 0.7942(16) 0.1309(10) 0.060(3) Uani 1 1 d . . . H4A H 1.0674 0.7841 0.1232 0.072 Uiso 1 1 calc R . . C5 C 0.8626(14) 0.7092(15) 0.0527(9) 0.057(3) Uani 1 1 d . . . H5A H 0.8614 0.6489 -0.0103 0.068 Uiso 1 1 calc R . . C6 C 0.7404(13) 0.7159(14) 0.0702(8) 0.045(2) Uani 1 1 d . . . H6A H 0.6575 0.6538 0.0184 0.054 Uiso 1 1 calc R . . C7 C 0.8620(11) 0.8990(12) 0.2271(8) 0.044(2) Uani 1 1 d . . . C8 C 0.4132(12) 1.1551(12) 0.2101(8) 0.048(2) Uani 1 1 d . . . H8A H 0.4320 1.2430 0.2633 0.058 Uiso 1 1 calc R . . C9 C 0.3227(13) 1.1037(13) 0.1199(9) 0.053(3) Uani 1 1 d . . . H9A H 0.2700 1.1495 0.0991 0.064 Uiso 1 1 calc R . . C10 C 0.3213(12) 0.9651(13) 0.0606(9) 0.044(2) Uani 1 1 d . . . C11 C 0.2445(13) 0.8535(14) -0.0346(8) 0.052(2) Uani 1 1 d . . . H11A H 0.1762 0.8616 -0.0767 0.063 Uiso 1 1 calc R . . C12 C 0.2728(13) 0.7326(14) -0.0640(8) 0.055(3) Uani 1 1 d . . . H12A H 0.2262 0.6596 -0.1289 0.066 Uiso 1 1 calc R . . C13 C 0.3690(12) 0.7148(12) -0.0003(8) 0.047(2) Uani 1 1 d . . . H13A H 0.3861 0.6312 -0.0252 0.057 Uiso 1 1 calc R . . C14 C 0.4188(10) 0.9402(11) 0.1224(7) 0.0371(19) Uani 1 1 d . . . C15 C 0.6769(15) 1.1383(17) 0.4742(9) 0.068(3) Uani 1 1 d . . . H15A H 0.6753 1.1722 0.5427 0.081 Uiso 1 1 calc R . . C16 C 0.7800(14) 1.1036(16) 0.4522(10) 0.058(3) Uani 1 1 d . . . H16A H 0.8469 1.1104 0.5044 0.070 Uiso 1 1 calc R . . C17 C 0.7851(12) 1.0570(12) 0.3491(8) 0.046(2) Uani 1 1 d . . . C18 C 0.6929(10) 1.0599(10) 0.2734(7) 0.0406(19) Uani 1 1 d . . . H18A H 0.7060 1.0457 0.2069 0.049 Uiso 1 1 calc R . . C19 C 0.5815(12) 1.0838(10) 0.2955(7) 0.043(2) Uani 1 1 d . . . C20 C 0.5731(14) 1.1252(14) 0.3984(9) 0.059(3) Uani 1 1 d . . . H20A H 0.4993 1.1433 0.4151 0.071 Uiso 1 1 calc R . . C21 C 0.3410(9) 0.6131(11) 0.2266(7) 0.0321(18) Uani 1 1 d . . . C22 C 0.2483(12) 0.6781(12) 0.2459(8) 0.047(2) Uani 1 1 d . . . H22A H 0.2764 0.7802 0.2453 0.056 Uiso 1 1 calc R . . C23 C 0.1193(13) 0.5947(17) 0.2652(12) 0.062(3) Uani 1 1 d . . . H23A H 0.0618 0.6413 0.2770 0.074 Uiso 1 1 calc R . . C24 C 0.0715(14) 0.4414(15) 0.2676(11) 0.062(3) Uani 1 1 d . . . H24A H -0.0144 0.3877 0.2841 0.074 Uiso 1 1 calc R . . C25 C 0.1543(12) 0.3720(13) 0.2450(10) 0.059(3) Uani 1 1 d . . . H25A H 0.1216 0.2676 0.2414 0.071 Uiso 1 1 calc R . . C26 C 0.2867(11) 0.4565(12) 0.2275(8) 0.047(2) Uani 1 1 d . . . H26A H 0.3424 0.4078 0.2158 0.056 Uiso 1 1 calc R . . C27 C 0.6116(11) 0.6519(11) 0.2985(8) 0.0348(19) Uani 1 1 d . . . C28 C 0.5879(12) 0.6709(13) 0.3971(8) 0.050(2) Uani 1 1 d . . . H28A H 0.5283 0.7129 0.4140 0.060 Uiso 1 1 calc R . . C29 C 0.6493(12) 0.6300(13) 0.4711(8) 0.052(2) Uani 1 1 d . . . H29A H 0.6377 0.6537 0.5378 0.062 Uiso 1 1 calc R . . C30 C 0.7261(13) 0.5555(13) 0.4465(9) 0.055(3) Uani 1 1 d . . . H30A H 0.7643 0.5240 0.4950 0.067 Uiso 1 1 calc R . . C31 C 0.7468(15) 0.5270(16) 0.3483(12) 0.058(3) Uani 1 1 d . . . H31A H 0.7986 0.4752 0.3303 0.069 Uiso 1 1 calc R . . C32 C 0.6913(13) 0.5749(13) 0.2767(9) 0.050(2) Uani 1 1 d . . . H32A H 0.7075 0.5551 0.2112 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0334(3) 0.0267(3) 0.0380(3) 0.00966(17) 0.00694(17) 0.01226(19) N1 0.044(5) 0.039(4) 0.051(5) 0.016(4) 0.008(4) 0.014(4) N2 0.038(4) 0.034(4) 0.044(4) 0.014(3) 0.008(3) 0.010(3) N3 0.056(5) 0.031(4) 0.043(4) 0.008(3) 0.011(3) 0.027(4) N4 0.037(4) 0.039(4) 0.036(4) 0.012(3) 0.008(3) 0.020(4) C1 0.039(5) 0.046(6) 0.066(7) 0.019(5) -0.006(5) 0.006(5) C2 0.030(5) 0.063(7) 0.083(8) 0.041(6) 0.002(5) 0.011(5) C3 0.047(6) 0.059(7) 0.068(7) 0.039(6) 0.021(5) 0.021(5) C4 0.052(7) 0.069(8) 0.078(8) 0.039(6) 0.035(6) 0.032(6) C5 0.062(7) 0.065(7) 0.059(6) 0.033(6) 0.030(5) 0.034(6) C6 0.053(6) 0.054(6) 0.036(5) 0.022(4) 0.013(4) 0.028(5) C7 0.038(5) 0.041(5) 0.056(5) 0.026(4) 0.010(4) 0.016(4) C8 0.052(6) 0.036(5) 0.053(6) 0.010(4) 0.013(5) 0.020(5) C9 0.069(7) 0.045(5) 0.064(6) 0.027(5) 0.023(5) 0.036(5) C10 0.042(5) 0.039(5) 0.053(6) 0.022(4) 0.013(4) 0.017(4) C11 0.055(7) 0.058(6) 0.045(5) 0.021(5) 0.013(5) 0.026(6) C12 0.066(7) 0.051(6) 0.038(5) 0.006(4) -0.004(5) 0.025(5) C13 0.057(6) 0.035(5) 0.042(5) 0.009(4) 0.005(4) 0.018(5) C14 0.034(5) 0.032(4) 0.044(5) 0.014(4) 0.012(4) 0.013(4) C15 0.078(9) 0.086(9) 0.040(6) 0.012(6) 0.006(5) 0.046(8) C16 0.050(7) 0.063(8) 0.046(6) 0.016(5) -0.004(5) 0.018(6) C17 0.044(5) 0.035(5) 0.051(5) 0.014(4) 0.006(4) 0.013(4) C18 0.040(5) 0.026(4) 0.049(5) 0.013(4) 0.013(4) 0.009(4) C19 0.062(6) 0.025(4) 0.039(4) 0.008(3) 0.011(4) 0.021(4) C20 0.062(7) 0.047(6) 0.060(7) 0.005(5) 0.012(5) 0.025(5) C21 0.016(4) 0.032(4) 0.035(4) 0.007(3) 0.001(3) 0.004(3) C22 0.057(6) 0.043(5) 0.053(5) 0.021(4) 0.016(5) 0.031(5) C23 0.044(6) 0.063(8) 0.089(9) 0.034(7) 0.016(6) 0.029(6) C24 0.052(7) 0.049(6) 0.082(8) 0.029(6) 0.021(6) 0.016(5) C25 0.042(6) 0.038(5) 0.082(8) 0.025(5) 0.015(5) 0.004(5) C26 0.043(5) 0.040(5) 0.062(6) 0.021(4) 0.016(5) 0.021(4) C27 0.034(5) 0.027(4) 0.046(5) 0.011(4) 0.010(4) 0.017(4) C28 0.044(6) 0.052(6) 0.047(5) 0.015(4) 0.010(4) 0.018(5) C29 0.045(6) 0.045(5) 0.049(5) 0.016(4) 0.008(4) 0.008(5) C30 0.053(6) 0.049(6) 0.055(6) 0.023(5) -0.003(5) 0.015(5) C31 0.057(7) 0.056(7) 0.079(8) 0.031(6) 0.015(6) 0.038(6) C32 0.052(6) 0.045(6) 0.063(6) 0.024(5) 0.015(5) 0.028(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 1.990(9) . ? Pt1 C27 1.996(10) . ? Pt1 N2 2.161(9) . ? Pt1 N4 2.165(8) . ? N1 C7 1.373(15) . ? N1 C1 1.394(14) . ? N1 C17 1.429(15) . ? N2 C6 1.358(15) . ? N2 C7 1.375(14) . ? N3 C8 1.385(13) . ? N3 C14 1.387(12) . ? N3 C19 1.402(13) . ? N4 C13 1.345(13) . ? N4 C14 1.374(13) . ? C1 C2 1.39(2) . ? C2 C3 1.418(18) . ? C3 C4 1.384(19) . ? C3 C7 1.400(16) . ? C4 C5 1.397(18) . ? C5 C6 1.391(17) . ? C8 C9 1.329(17) . ? C9 C10 1.429(15) . ? C10 C11 1.391(17) . ? C10 C14 1.422(15) . ? C11 C12 1.356(17) . ? C12 C13 1.382(16) . ? C15 C16 1.34(2) . ? C15 C20 1.384(18) . ? C16 C17 1.404(17) . ? C17 C18 1.375(14) . ? C18 C19 1.374(15) . ? C19 C20 1.407(15) . ? C21 C26 1.413(14) . ? C21 C22 1.427(14) . ? C22 C23 1.367(17) . ? C23 C24 1.396(18) . ? C24 C25 1.369(19) . ? C25 C26 1.386(15) . ? C27 C32 1.394(15) . ? C27 C28 1.395(15) . ? C28 C29 1.387(16) . ? C29 C30 1.355(18) . ? C30 C31 1.380(19) . ? C31 C32 1.378(17) . ? 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 C21 Pt1 C27 89.3(4) . . ? C21 Pt1 N2 170.4(4) . . ? C27 Pt1 N2 86.1(4) . . ? C21 Pt1 N4 89.2(4) . . ? C27 Pt1 N4 176.3(3) . . ? N2 Pt1 N4 95.9(3) . . ? C7 N1 C1 107.5(10) . . ? C7 N1 C17 125.8(9) . . ? C1 N1 C17 126.6(10) . . ? C6 N2 C7 113.2(10) . . ? C6 N2 Pt1 116.9(7) . . ? C7 N2 Pt1 124.3(7) . . ? C8 N3 C14 107.6(8) . . ? C8 N3 C19 127.1(8) . . ? C14 N3 C19 125.3(8) . . ? C13 N4 C14 114.1(9) . . ? C13 N4 Pt1 117.1(7) . . ? C14 N4 Pt1 127.3(7) . . ? C2 C1 N1 109.4(11) . . ? C1 C2 C3 106.7(10) . . ? C4 C3 C7 117.2(11) . . ? C4 C3 C2 135.6(12) . . ? C7 C3 C2 107.2(11) . . ? C3 C4 C5 118.9(12) . . ? C6 C5 C4 119.1(11) . . ? N2 C6 C5 124.9(11) . . ? N1 C7 N2 124.5(10) . . ? N1 C7 C3 109.1(10) . . ? N2 C7 C3 126.2(11) . . ? C9 C8 N3 111.3(9) . . ? C8 C9 C10 107.3(10) . . ? C11 C10 C14 117.7(10) . . ? C11 C10 C9 135.4(11) . . ? C14 C10 C9 106.7(10) . . ? C12 C11 C10 117.7(10) . . ? C11 C12 C13 121.8(10) . . ? N4 C13 C12 123.8(10) . . ? N4 C14 N3 128.3(9) . . ? N4 C14 C10 124.4(9) . . ? N3 C14 C10 107.1(9) . . ? C16 C15 C20 122.1(12) . . ? C15 C16 C17 119.0(11) . . ? C18 C17 C16 119.8(11) . . ? C18 C17 N1 117.7(9) . . ? C16 C17 N1 122.5(10) . . ? C19 C18 C17 120.3(9) . . ? C18 C19 N3 119.2(8) . . ? C18 C19 C20 119.3(10) . . ? N3 C19 C20 121.5(10) . . ? C15 C20 C19 118.7(12) . . ? C26 C21 C22 114.3(8) . . ? C26 C21 Pt1 120.7(7) . . ? C22 C21 Pt1 125.0(8) . . ? C23 C22 C21 121.9(10) . . ? C22 C23 C24 121.7(12) . . ? C25 C24 C23 118.4(12) . . ? C24 C25 C26 120.4(11) . . ? C25 C26 C21 123.3(10) . . ? C32 C27 C28 114.7(10) . . ? C32 C27 Pt1 123.8(8) . . ? C28 C27 Pt1 121.5(8) . . ? C29 C28 C27 122.9(11) . . ? C30 C29 C28 120.1(11) . . ? C29 C30 C31 119.0(10) . . ? C32 C31 C30 120.4(12) . . ? C31 C32 C27 122.5(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.384 _refine_diff_density_min -2.846 _refine_diff_density_rms 0.322 # Attachment '9a.cif' data_zs191 _database_code_depnum_ccdc_archive 'CCDC 697415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 N4 O Pt' _chemical_formula_weight 725.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6466(3) _cell_length_b 9.7584(2) _cell_length_c 17.6630(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.8460(10) _cell_angle_gamma 90.00 _cell_volume 2773.47(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5682 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.01 _exptl_crystal_description Block _exptl_crystal_colour clear _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 5.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4288 _exptl_absorpt_correction_T_max 0.6297 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 16310 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.18 _reflns_number_total 6130 _reflns_number_gt 4843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0420P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6130 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 O1 O 0.3251(2) 0.8280(4) -0.25908(19) 0.0532(9) Uani 1 1 d . . . Pt1 Pt 0.290913(9) 0.941464(17) 0.096284(9) 0.02844(7) Uani 1 1 d . . . N1 N 0.1737(2) 1.0424(3) 0.0757(2) 0.0306(8) Uani 1 1 d . . . N2 N 0.1424(2) 1.1029(4) -0.0620(2) 0.0322(8) Uani 1 1 d . . . N3 N 0.3484(2) 1.1394(4) 0.1138(2) 0.0304(8) Uani 1 1 d . . . N4 N 0.3021(2) 1.2195(4) -0.0185(2) 0.0304(8) Uani 1 1 d . . . C1 C 0.1426(3) 1.0533(5) 0.1392(3) 0.0423(12) Uani 1 1 d . . . H1A H 0.1732 1.0131 0.1869 0.051 Uiso 1 1 calc R . . C2 C 0.0691(3) 1.1192(5) 0.1386(3) 0.0446(12) Uani 1 1 d . . . H2A H 0.0513 1.1250 0.1855 0.053 Uiso 1 1 calc R . . C3 C 0.0218(3) 1.1762(5) 0.0715(3) 0.0397(11) Uani 1 1 d . . . H3A H -0.0294 1.2202 0.0705 0.048 Uiso 1 1 calc R . . C4 C 0.0504(3) 1.1681(5) 0.0051(3) 0.0329(10) Uani 1 1 d . . . C5 C 0.0214(3) 1.2136(5) -0.0736(3) 0.0424(12) Uani 1 1 d . . . H5A H -0.0283 1.2634 -0.0949 0.051 Uiso 1 1 calc R . . C6 C 0.0778(3) 1.1730(5) -0.1126(3) 0.0434(12) Uani 1 1 d . . . H6A H 0.0736 1.1899 -0.1665 0.052 Uiso 1 1 calc R . . C7 C 0.1269(3) 1.0999(4) 0.0106(2) 0.0282(9) Uani 1 1 d . . . C8 C 0.3824(3) 1.1832(5) 0.1872(3) 0.0423(12) Uani 1 1 d . . . H8A H 0.3930 1.1173 0.2282 0.051 Uiso 1 1 calc R . . C9 C 0.4027(3) 1.3182(5) 0.2066(3) 0.0403(12) Uani 1 1 d . . . H9A H 0.4274 1.3421 0.2596 0.048 Uiso 1 1 calc R . . C10 C 0.3878(3) 1.4172(5) 0.1506(3) 0.0374(11) Uani 1 1 d . . . H10A H 0.4004 1.5105 0.1637 0.045 Uiso 1 1 calc R . . C11 C 0.3537(3) 1.3776(5) 0.0739(3) 0.0315(10) Uani 1 1 d . . . C12 C 0.3264(3) 1.4445(5) 0.0006(3) 0.0415(12) Uani 1 1 d . . . H12A H 0.3290 1.5402 -0.0084 0.050 Uiso 1 1 calc R . . C13 C 0.2960(3) 1.3485(5) -0.0538(3) 0.0403(11) Uani 1 1 d . . . H13A H 0.2739 1.3658 -0.1080 0.048 Uiso 1 1 calc R . . C14 C 0.3367(2) 1.2368(4) 0.0595(2) 0.0282(9) Uani 1 1 d . . . C15 C 0.2884(3) 1.0960(4) -0.0632(2) 0.0287(9) Uani 1 1 d . . . C16 C 0.3542(3) 1.0394(4) -0.0890(3) 0.0335(10) Uani 1 1 d . . . H16A H 0.4091 1.0740 -0.0711 0.040 Uiso 1 1 calc R . . C17 C 0.3364(3) 0.9333(5) -0.1404(3) 0.0360(11) Uani 1 1 d . . . C18 C 0.2561(3) 0.8806(5) -0.1663(3) 0.0363(11) Uani 1 1 d . . . C19 C 0.1915(3) 0.9334(5) -0.1394(3) 0.0360(11) Uani 1 1 d . . . H19A H 0.1370 0.8966 -0.1562 0.043 Uiso 1 1 calc R . . C20 C 0.2090(2) 1.0424(4) -0.0870(2) 0.0294(10) Uani 1 1 d . . . C21 C 0.2645(3) 0.7652(6) -0.2241(3) 0.0472(13) Uani 1 1 d . . . H21A H 0.2118 0.7340 -0.2613 0.057 Uiso 1 1 calc R . . C22 C 0.3155(4) 0.6578(6) -0.1761(3) 0.0580(15) Uani 1 1 d . . . H22A H 0.2967 0.5699 -0.1650 0.070 Uiso 1 1 calc R . . C23 C 0.3918(4) 0.7053(6) -0.1514(3) 0.0591(16) Uani 1 1 d . . . H23A H 0.4390 0.6598 -0.1197 0.071 Uiso 1 1 calc R . . C24 C 0.3874(3) 0.8487(6) -0.1848(3) 0.0504(14) Uani 1 1 d . . . H24A H 0.4413 0.8897 -0.1884 0.060 Uiso 1 1 calc R . . C25 C 0.4002(3) 0.8419(4) 0.1211(3) 0.0322(10) Uani 1 1 d . . . C26 C 0.4512(3) 0.8384(5) 0.1953(3) 0.0434(12) Uani 1 1 d . . . H26A H 0.4357 0.8877 0.2357 0.052 Uiso 1 1 calc R . . C27 C 0.5254(3) 0.7641(6) 0.2132(3) 0.0517(14) Uani 1 1 d . . . H27A H 0.5609 0.7674 0.2646 0.062 Uiso 1 1 calc R . . C28 C 0.5471(3) 0.6869(6) 0.1571(3) 0.0499(14) Uani 1 1 d . . . H28A H 0.5958 0.6317 0.1699 0.060 Uiso 1 1 calc R . . C29 C 0.4975(3) 0.6904(5) 0.0817(3) 0.0505(14) Uani 1 1 d . . . H29A H 0.5128 0.6402 0.0415 0.061 Uiso 1 1 calc R . . C30 C 0.4249(3) 0.7675(5) 0.0647(3) 0.0418(12) Uani 1 1 d . . . H30A H 0.3912 0.7690 0.0124 0.050 Uiso 1 1 calc R . . C31 C 0.2337(3) 0.7589(5) 0.0901(3) 0.0317(10) Uani 1 1 d . . . C32 C 0.1883(3) 0.7029(5) 0.0208(3) 0.0490(13) Uani 1 1 d . . . H32A H 0.1849 0.7518 -0.0264 0.059 Uiso 1 1 calc R . . C33 C 0.1467(4) 0.5768(6) 0.0167(4) 0.0600(17) Uani 1 1 d . . . H33A H 0.1164 0.5410 -0.0324 0.072 Uiso 1 1 calc R . . C34 C 0.1507(3) 0.5065(6) 0.0844(4) 0.0566(16) Uani 1 1 d . . . H34A H 0.1233 0.4207 0.0827 0.068 Uiso 1 1 calc R . . C35 C 0.1932(3) 0.5586(5) 0.1537(4) 0.0527(14) Uani 1 1 d . . . H35A H 0.1954 0.5100 0.2008 0.063 Uiso 1 1 calc R . . C36 C 0.2342(3) 0.6842(5) 0.1562(3) 0.0453(12) Uani 1 1 d . . . H36A H 0.2637 0.7194 0.2057 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.067(2) 0.059(2) 0.0381(18) -0.0045(18) 0.0222(17) 0.006(2) Pt1 0.02424(10) 0.02730(11) 0.03302(10) 0.00191(7) 0.00597(6) 0.00058(7) N1 0.0267(18) 0.029(2) 0.038(2) -0.0037(16) 0.0116(15) -0.0001(15) N2 0.0289(19) 0.037(2) 0.0327(19) -0.0036(16) 0.0116(15) 0.0061(16) N3 0.0268(18) 0.030(2) 0.0351(19) 0.0010(16) 0.0089(15) -0.0010(15) N4 0.0331(19) 0.023(2) 0.0359(19) -0.0008(16) 0.0096(15) -0.0013(15) C1 0.045(3) 0.046(3) 0.040(3) -0.001(2) 0.017(2) 0.001(2) C2 0.050(3) 0.045(3) 0.048(3) -0.003(2) 0.028(2) 0.004(2) C3 0.031(2) 0.038(3) 0.055(3) -0.007(2) 0.020(2) 0.001(2) C4 0.024(2) 0.031(3) 0.044(3) -0.006(2) 0.0097(18) 0.0003(19) C5 0.033(2) 0.046(3) 0.047(3) -0.003(2) 0.009(2) 0.012(2) C6 0.037(3) 0.053(3) 0.038(2) 0.004(2) 0.004(2) 0.012(2) C7 0.024(2) 0.027(2) 0.034(2) -0.0063(18) 0.0085(17) -0.0019(17) C8 0.043(3) 0.048(3) 0.033(2) 0.003(2) 0.003(2) 0.004(2) C9 0.039(3) 0.045(3) 0.033(2) -0.013(2) 0.0028(19) -0.001(2) C10 0.035(2) 0.032(3) 0.048(3) -0.014(2) 0.014(2) -0.006(2) C11 0.028(2) 0.026(2) 0.042(2) -0.006(2) 0.0108(19) 0.0015(18) C12 0.051(3) 0.029(3) 0.047(3) -0.004(2) 0.017(2) -0.004(2) C13 0.052(3) 0.029(3) 0.040(3) 0.003(2) 0.013(2) 0.002(2) C14 0.021(2) 0.030(2) 0.035(2) -0.0051(19) 0.0109(17) 0.0024(17) C15 0.034(2) 0.025(2) 0.030(2) -0.0021(17) 0.0110(18) -0.0013(18) C16 0.027(2) 0.034(3) 0.041(2) -0.002(2) 0.0112(18) -0.0016(19) C17 0.036(2) 0.036(3) 0.040(2) -0.003(2) 0.016(2) 0.005(2) C18 0.044(3) 0.027(2) 0.038(2) -0.004(2) 0.011(2) -0.003(2) C19 0.032(2) 0.038(3) 0.038(2) -0.003(2) 0.0082(19) -0.006(2) C20 0.030(2) 0.030(3) 0.030(2) -0.0010(18) 0.0102(18) 0.0022(19) C21 0.053(3) 0.049(3) 0.039(3) -0.012(2) 0.010(2) -0.005(3) C22 0.086(5) 0.036(3) 0.053(3) -0.002(3) 0.020(3) 0.010(3) C23 0.066(4) 0.050(4) 0.057(3) -0.014(3) 0.007(3) 0.025(3) C24 0.038(3) 0.055(4) 0.064(3) -0.017(3) 0.024(2) 0.002(3) C25 0.033(2) 0.024(2) 0.040(2) 0.0080(19) 0.0096(19) -0.0038(19) C26 0.038(3) 0.046(3) 0.047(3) 0.007(2) 0.013(2) 0.006(2) C27 0.034(3) 0.059(4) 0.058(3) 0.014(3) 0.004(2) 0.010(3) C28 0.030(3) 0.042(3) 0.077(4) 0.016(3) 0.012(2) 0.006(2) C29 0.036(3) 0.040(3) 0.077(4) -0.006(3) 0.018(3) 0.000(2) C30 0.029(2) 0.036(3) 0.059(3) 0.003(2) 0.007(2) -0.001(2) C31 0.026(2) 0.026(2) 0.044(3) 0.003(2) 0.0106(18) 0.0035(18) C32 0.050(3) 0.039(3) 0.055(3) -0.003(3) 0.007(2) 0.001(2) C33 0.053(4) 0.051(4) 0.071(4) -0.017(3) 0.006(3) -0.013(3) C34 0.040(3) 0.028(3) 0.105(5) -0.004(3) 0.025(3) -0.006(2) C35 0.046(3) 0.043(3) 0.076(4) 0.011(3) 0.026(3) -0.003(3) C36 0.037(3) 0.039(3) 0.057(3) 0.002(3) 0.008(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C21 1.446(6) . ? O1 C24 1.463(6) . ? Pt1 C25 2.009(4) . ? Pt1 C31 2.011(4) . ? Pt1 N1 2.132(3) . ? Pt1 N3 2.143(4) . ? N1 C7 1.337(5) . ? N1 C1 1.355(6) . ? N2 C7 1.372(5) . ? N2 C6 1.390(5) . ? N2 C20 1.422(5) . ? N3 C14 1.328(5) . ? N3 C8 1.344(5) . ? N4 C14 1.360(5) . ? N4 C13 1.398(6) . ? N4 C15 1.427(5) . ? C1 C2 1.380(7) . ? C1 H1A 0.9500 . ? C2 C3 1.363(7) . ? C2 H2A 0.9500 . ? C3 C4 1.377(6) . ? C3 H3A 0.9500 . ? C4 C7 1.417(6) . ? C4 C5 1.420(6) . ? C5 C6 1.358(7) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C8 C9 1.382(7) . ? C8 H8A 0.9500 . ? C9 C10 1.359(7) . ? C9 H9A 0.9500 . ? C10 C11 1.384(6) . ? C10 H10A 0.9500 . ? C11 C14 1.413(6) . ? C11 C12 1.416(6) . ? C12 C13 1.344(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C15 C20 1.383(6) . ? C15 C16 1.403(6) . ? C16 C17 1.359(6) . ? C16 H16A 0.9500 . ? C17 C18 1.396(6) . ? C17 C24 1.536(7) . ? C18 C19 1.381(7) . ? C18 C21 1.551(7) . ? C19 C20 1.390(6) . ? C19 H19A 0.9500 . ? C21 C22 1.473(7) . ? C21 H21A 1.0000 . ? C22 C23 1.317(8) . ? C22 H22A 0.9500 . ? C23 C24 1.513(8) . ? C23 H23A 0.9500 . ? C24 H24A 1.0000 . ? C25 C26 1.367(6) . ? C25 C30 1.378(7) . ? C26 C27 1.396(7) . ? C26 H26A 0.9500 . ? C27 C28 1.366(8) . ? C27 H27A 0.9500 . ? C28 C29 1.376(7) . ? C28 H28A 0.9500 . ? C29 C30 1.390(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.374(7) . ? C31 C32 1.377(6) . ? C32 C33 1.404(7) . ? C32 H32A 0.9500 . ? C33 C34 1.366(9) . ? C33 H33A 0.9500 . ? C34 C35 1.346(8) . ? C34 H34A 0.9500 . ? C35 C36 1.398(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? 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 C21 O1 C24 95.0(3) . . ? C25 Pt1 C31 88.49(16) . . ? C25 Pt1 N1 176.82(15) . . ? C31 Pt1 N1 89.98(15) . . ? C25 Pt1 N3 93.35(15) . . ? C31 Pt1 N3 174.14(16) . . ? N1 Pt1 N3 87.90(13) . . ? C7 N1 C1 114.7(4) . . ? C7 N1 Pt1 130.3(3) . . ? C1 N1 Pt1 115.0(3) . . ? C7 N2 C6 108.2(4) . . ? C7 N2 C20 129.0(4) . . ? C6 N2 C20 122.7(4) . . ? C14 N3 C8 114.6(4) . . ? C14 N3 Pt1 124.3(3) . . ? C8 N3 Pt1 119.2(3) . . ? C14 N4 C13 107.7(3) . . ? C14 N4 C15 129.2(4) . . ? C13 N4 C15 122.0(3) . . ? N1 C1 C2 123.8(5) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H3A 121.0 . . ? C4 C3 H3A 121.0 . . ? C3 C4 C7 118.0(4) . . ? C3 C4 C5 135.3(4) . . ? C7 C4 C5 106.8(4) . . ? C6 C5 C4 107.4(4) . . ? C6 C5 H5A 126.3 . . ? C4 C5 H5A 126.3 . . ? C5 C6 N2 109.8(4) . . ? C5 C6 H6A 125.1 . . ? N2 C6 H6A 125.1 . . ? N1 C7 N2 127.3(4) . . ? N1 C7 C4 124.9(4) . . ? N2 C7 C4 107.9(4) . . ? N3 C8 C9 123.9(4) . . ? N3 C8 H8A 118.0 . . ? C9 C8 H8A 118.0 . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 117.9(4) . . ? C9 C10 H10A 121.1 . . ? C11 C10 H10A 121.1 . . ? C10 C11 C14 117.4(4) . . ? C10 C11 C12 136.2(4) . . ? C14 C11 C12 106.4(4) . . ? C13 C12 C11 107.8(4) . . ? C13 C12 H12A 126.1 . . ? C11 C12 H12A 126.1 . . ? C12 C13 N4 109.7(4) . . ? C12 C13 H13A 125.1 . . ? N4 C13 H13A 125.1 . . ? N3 C14 N4 126.0(4) . . ? N3 C14 C11 125.5(4) . . ? N4 C14 C11 108.4(4) . . ? C20 C15 C16 121.1(4) . . ? C20 C15 N4 119.5(4) . . ? C16 C15 N4 119.0(4) . . ? C17 C16 C15 117.6(4) . . ? C17 C16 H16A 121.2 . . ? C15 C16 H16A 121.2 . . ? C16 C17 C18 121.8(4) . . ? C16 C17 C24 134.2(4) . . ? C18 C17 C24 104.0(4) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 C21 135.0(4) . . ? C17 C18 C21 104.1(4) . . ? C18 C19 C20 117.8(4) . . ? C18 C19 H19A 121.1 . . ? C20 C19 H19A 121.1 . . ? C15 C20 C19 120.8(4) . . ? C15 C20 N2 120.5(4) . . ? C19 C20 N2 118.6(4) . . ? O1 C21 C22 100.7(4) . . ? O1 C21 C18 99.4(4) . . ? C22 C21 C18 105.9(4) . . ? O1 C21 H21A 116.1 . . ? C22 C21 H21A 116.1 . . ? C18 C21 H21A 116.1 . . ? C23 C22 C21 107.7(5) . . ? C23 C22 H22A 126.1 . . ? C21 C22 H22A 126.1 . . ? C22 C23 C24 104.5(5) . . ? C22 C23 H23A 127.8 . . ? C24 C23 H23A 127.8 . . ? O1 C24 C23 100.0(4) . . ? O1 C24 C17 100.1(4) . . ? C23 C24 C17 106.0(4) . . ? O1 C24 H24A 116.1 . . ? C23 C24 H24A 116.1 . . ? C17 C24 H24A 116.1 . . ? C26 C25 C30 117.0(4) . . ? C26 C25 Pt1 121.7(4) . . ? C30 C25 Pt1 121.2(3) . . ? C25 C26 C27 121.7(5) . . ? C25 C26 H26A 119.2 . . ? C27 C26 H26A 119.2 . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 118.9(5) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C28 C29 C30 119.7(5) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C25 C30 C29 122.2(5) . . ? C25 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C36 C31 C32 115.3(4) . . ? C36 C31 Pt1 121.6(3) . . ? C32 C31 Pt1 123.0(4) . . ? C31 C32 C33 123.0(5) . . ? C31 C32 H32A 118.5 . . ? C33 C32 H32A 118.5 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 119.9(6) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C31 C36 C35 122.8(5) . . ? C31 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.297 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.124