# 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 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Armando J. L. Pombeiro' _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_section_title ; New Water-soluble Azido- and Derived Tetrazolato-platinum(II) Complexes with 1,3,5-triaza-7-phosphaadamantane (PTA). Easy Metal-mediated Synthesis and Isolation, from Aqueous Medium, of 5-substituted Tetrazoles ; loop_ _publ_author_name 'Armando J. L. Pombeiro' 'Adilia Charmier' "Maria de F\'atima Guedes da Silva" 'Suman Mukhopadhyay' ; P.Smolenski ; # Attachment 'Compound_1_piotr11001f1-revised.cif' data_piotr11001f1 _database_code_depnum_ccdc_archive 'CCDC 688071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H24 N12 P2 Pt), 11(H2 O)' _chemical_formula_sum 'C24 H70 N24 O11 P4 Pt2' _chemical_formula_weight 1385.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.079(7) _cell_length_b 9.283(3) _cell_length_c 18.982(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.845(16) _cell_angle_gamma 90.00 _cell_volume 4670(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3223 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.35 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 6.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2757 _exptl_absorpt_correction_T_max 0.4016 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 14147 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4761 _reflns_number_gt 3665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0313P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4761 _refine_ls_number_parameters 297 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.83117(18) 0.6019(6) 0.6045(3) 0.0162(12) Uani 1 1 d . . . H11A H 0.8399 0.5191 0.5766 0.019 Uiso 1 1 calc R . . H11B H 0.8349 0.6910 0.5774 0.019 Uiso 1 1 calc R . . C12 C 0.77270(18) 0.4309(6) 0.6779(3) 0.0167(12) Uani 1 1 d . . . H12A H 0.7410 0.4169 0.6953 0.020 Uiso 1 1 calc R . . H12B H 0.7794 0.3421 0.6525 0.020 Uiso 1 1 calc R . . C13 C 0.76434(19) 0.7316(6) 0.6804(3) 0.0168(12) Uani 1 1 d . . . H13A H 0.7656 0.8257 0.6562 0.020 Uiso 1 1 calc R . . H13B H 0.7324 0.7269 0.6980 0.020 Uiso 1 1 calc R . . C14 C 0.86241(19) 0.4744(6) 0.7166(3) 0.0173(12) Uani 1 1 d . . . H14A H 0.8672 0.3904 0.6865 0.021 Uiso 1 1 calc R . . H14B H 0.8903 0.4738 0.7595 0.021 Uiso 1 1 calc R . . C15 C 0.8055(2) 0.5836(6) 0.7809(3) 0.0171(12) Uani 1 1 d . . . H15A H 0.8310 0.5870 0.8264 0.021 Uiso 1 1 calc R . . H15B H 0.7719 0.5740 0.7933 0.021 Uiso 1 1 calc R . . C16 C 0.85507(19) 0.7302(6) 0.7188(3) 0.0174(12) Uani 1 1 d . . . H16A H 0.8825 0.7384 0.7620 0.021 Uiso 1 1 calc R . . H16B H 0.8552 0.8194 0.6903 0.021 Uiso 1 1 calc R . . C21 C 0.63097(19) 0.5116(6) 0.6371(3) 0.0161(12) Uani 1 1 d . . . H21A H 0.6294 0.4070 0.6268 0.019 Uiso 1 1 calc R . . H21B H 0.6592 0.5291 0.6784 0.019 Uiso 1 1 calc R . . C22 C 0.63336(18) 0.7960(5) 0.5866(3) 0.0169(12) Uani 1 1 d . . . H22A H 0.6618 0.8232 0.6260 0.020 Uiso 1 1 calc R . . H22B H 0.6331 0.8627 0.5458 0.020 Uiso 1 1 calc R . . C23 C 0.58157(18) 0.5829(6) 0.4964(3) 0.0168(12) Uani 1 1 d . . . H23A H 0.5799 0.6429 0.4528 0.020 Uiso 1 1 calc R . . H23B H 0.5782 0.4807 0.4812 0.020 Uiso 1 1 calc R . . C24 C 0.58490(19) 0.7132(6) 0.6730(3) 0.0153(12) Uani 1 1 d . . . H24A H 0.6154 0.7320 0.7107 0.018 Uiso 1 1 calc R . . H24B H 0.5551 0.7372 0.6936 0.018 Uiso 1 1 calc R . . C25 C 0.54244(19) 0.7736(6) 0.5536(3) 0.0183(12) Uani 1 1 d . . . H25A H 0.5109 0.7985 0.5696 0.022 Uiso 1 1 calc R . . H25B H 0.5440 0.8340 0.5111 0.022 Uiso 1 1 calc R . . C26 C 0.53995(18) 0.5328(6) 0.5953(3) 0.0175(12) Uani 1 1 d . . . H26A H 0.5401 0.4301 0.5813 0.021 Uiso 1 1 calc R . . H26B H 0.5083 0.5509 0.6123 0.021 Uiso 1 1 calc R . . N1 N 0.76693(17) 0.5114(5) 0.4581(3) 0.0196(11) Uani 1 1 d . . . N2 N 0.78325(16) 0.3911(6) 0.4547(2) 0.0189(11) Uani 1 1 d . . . N3 N 0.80191(19) 0.2808(6) 0.4485(3) 0.0322(13) Uani 1 1 d . . . N4 N 0.65858(16) 0.5070(5) 0.4176(3) 0.0225(11) Uani 1 1 d . . . N5 N 0.67151(16) 0.4494(5) 0.3671(3) 0.0186(10) Uani 1 1 d . . . N6 N 0.68039(18) 0.3986(5) 0.3157(3) 0.0235(11) Uani 1 1 d . . . N11 N 0.86607(15) 0.6067(5) 0.6753(2) 0.0147(10) Uani 1 1 d . . . N12 N 0.81493(15) 0.4571(5) 0.7401(2) 0.0152(10) Uani 1 1 d . . . N13 N 0.80727(15) 0.7203(4) 0.7416(2) 0.0140(10) Uani 1 1 d . . . N21 N 0.58319(15) 0.5590(5) 0.6554(2) 0.0142(9) Uani 1 1 d . . . N22 N 0.58563(15) 0.8095(5) 0.6116(2) 0.0148(10) Uani 1 1 d . . . N23 N 0.54004(16) 0.6218(5) 0.5317(2) 0.0187(11) Uani 1 1 d . . . O1 O 0.59061(17) 0.1884(6) 0.4913(3) 0.0539(15) Uani 1 1 d D . . O2 O 0.55477(15) 0.1187(4) 0.6129(2) 0.0301(10) Uani 1 1 d . . . O3 O 0.46436(14) 0.1960(4) 0.6575(2) 0.0312(10) Uani 1 1 d D . . O4 O 0.54915(14) 0.4735(4) 0.7828(2) 0.0233(9) Uani 1 1 d D . . O5 O 0.55922(15) 0.7468(5) 0.8477(2) 0.0327(11) Uani 1 1 d D . . O6 O 0.5000 0.9277(6) 0.7500 0.048(2) Uani 1 2 d SD . . P1 P 0.76561(5) 0.58488(14) 0.61501(7) 0.0125(3) Uani 1 1 d . . . P2 P 0.64242(5) 0.61028(15) 0.55768(7) 0.0134(3) Uani 1 1 d . . . Pt1 Pt 0.709434(7) 0.55467(2) 0.512321(11) 0.01252(7) Uani 1 1 d . . . H1A H 0.5908 0.1477 0.5368 0.050 Uiso 1 1 d D . . H1B H 0.6224(9) 0.199(7) 0.505(4) 0.050 Uiso 1 1 d D . . H2A H 0.5265 0.1403 0.6195 0.050 Uiso 1 1 d . . . H2B H 0.5612 0.0346 0.6194 0.050 Uiso 1 1 d . . . H4A H 0.5616 0.4977 0.7475 0.050 Uiso 1 1 d D . . H6A H 0.5209 0.8573 0.7838 0.050 Uiso 1 1 d D . . H5A H 0.5723 0.7726 0.8915 0.050 Uiso 1 1 d D . . H5B H 0.5619 0.6695 0.8343 0.050 Uiso 1 1 d D . . H4B H 0.5680 0.4376 0.8215 0.050 Uiso 1 1 d D . . H3A H 0.4351 0.1610 0.6592 0.050 Uiso 1 1 d D . . H3B H 0.4746 0.2387 0.6982 0.050 Uiso 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 C11 0.017(3) 0.019(3) 0.015(3) 0.003(2) 0.008(2) -0.002(2) C12 0.015(3) 0.020(3) 0.015(3) 0.003(2) 0.002(2) 0.002(2) C13 0.020(3) 0.015(3) 0.018(3) 0.003(2) 0.010(2) 0.002(2) C14 0.018(3) 0.017(3) 0.017(3) -0.001(2) 0.003(2) 0.003(2) C15 0.019(3) 0.017(3) 0.015(3) 0.001(2) 0.003(2) 0.000(2) C16 0.020(3) 0.010(3) 0.021(3) 0.005(2) 0.001(2) 0.000(2) C21 0.024(3) 0.009(3) 0.016(3) 0.005(2) 0.006(2) 0.000(2) C22 0.017(3) 0.010(3) 0.024(3) -0.005(2) 0.005(2) 0.001(2) C23 0.016(3) 0.018(3) 0.017(3) -0.004(2) 0.005(2) 0.000(2) C24 0.019(3) 0.015(3) 0.012(3) -0.004(2) 0.006(2) 0.001(2) C25 0.016(3) 0.019(3) 0.019(3) 0.003(2) 0.003(2) 0.003(2) C26 0.015(3) 0.017(3) 0.022(3) -0.004(2) 0.006(2) -0.005(2) N1 0.022(2) 0.016(3) 0.023(3) -0.001(2) 0.009(2) 0.002(2) N2 0.016(2) 0.026(3) 0.015(3) -0.001(2) 0.0051(18) -0.006(2) N3 0.034(3) 0.019(3) 0.049(4) 0.000(2) 0.021(3) 0.010(2) N4 0.018(2) 0.032(3) 0.019(3) -0.005(2) 0.009(2) 0.004(2) N5 0.017(2) 0.015(3) 0.023(3) 0.003(2) 0.0010(19) 0.003(2) N6 0.030(3) 0.027(3) 0.014(3) -0.003(2) 0.005(2) 0.004(2) N11 0.016(2) 0.008(2) 0.020(3) 0.0004(18) 0.0045(19) 0.0010(17) N12 0.016(2) 0.012(3) 0.017(2) 0.0016(19) 0.0011(17) 0.0038(19) N13 0.014(2) 0.011(2) 0.016(2) -0.0013(18) 0.0013(18) -0.0017(17) N21 0.014(2) 0.013(2) 0.017(2) -0.0011(19) 0.0058(17) -0.0019(19) N22 0.016(2) 0.013(3) 0.015(2) 0.0041(18) 0.0040(18) -0.0012(18) N23 0.016(2) 0.023(3) 0.017(3) -0.001(2) 0.0022(19) 0.0024(19) O1 0.036(3) 0.093(5) 0.031(3) 0.020(3) 0.003(2) -0.006(3) O2 0.032(2) 0.023(2) 0.039(3) 0.005(2) 0.016(2) 0.0062(18) O3 0.026(2) 0.025(3) 0.045(3) -0.006(2) 0.0133(19) -0.0060(18) O4 0.028(2) 0.022(3) 0.022(2) 0.0088(17) 0.0091(17) 0.0022(17) O5 0.040(3) 0.035(3) 0.025(3) -0.0077(19) 0.010(2) -0.009(2) O6 0.042(4) 0.022(4) 0.074(6) 0.000 -0.003(4) 0.000 P1 0.0148(7) 0.0112(8) 0.0120(7) 0.0007(5) 0.0039(5) 0.0012(5) P2 0.0159(7) 0.0131(7) 0.0114(7) -0.0017(5) 0.0032(5) 0.0005(5) Pt1 0.01574(10) 0.01114(12) 0.01128(10) 0.00009(9) 0.00416(7) 0.00182(9) _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 C11 N11 1.476(6) . ? C11 P1 1.833(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N12 1.486(6) . ? C12 P1 1.846(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N13 1.469(6) . ? C13 P1 1.847(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N12 1.454(6) . ? C14 N11 1.472(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N12 1.456(7) . ? C15 N13 1.478(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N13 1.450(6) . ? C16 N11 1.478(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 N21 1.475(6) . ? C21 P2 1.843(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N22 1.471(6) . ? C22 P2 1.841(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N23 1.468(7) . ? C23 P2 1.829(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N21 1.468(6) . ? C24 N22 1.474(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N23 1.467(7) . ? C25 N22 1.470(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N23 1.463(7) . ? C26 N21 1.478(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N1 N2 1.207(6) . ? N1 Pt1 2.074(5) . ? N2 N3 1.159(6) . ? N4 N5 1.210(6) . ? N4 Pt1 2.076(5) . ? N5 N6 1.153(6) . ? O1 H1A 0.942 . ? O1 H1B 0.85(2) . ? O2 H2A 0.826 . ? O2 H2B 0.804 . ? O3 H3A 0.862 . ? O3 H3B 0.862 . ? O4 H4A 0.841 . ? O4 H4B 0.869 . ? O5 H5A 0.869 . ? O5 H5B 0.769 . ? O6 H6A 1.005 . ? P1 Pt1 2.2305(14) . ? P2 Pt1 2.2232(15) . ? 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 N11 C11 P1 110.9(4) . . ? N11 C11 H11A 109.5 . . ? P1 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? N12 C12 P1 110.4(3) . . ? N12 C12 H12A 109.6 . . ? P1 C12 H12A 109.6 . . ? N12 C12 H12B 109.6 . . ? P1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N13 C13 P1 111.0(3) . . ? N13 C13 H13A 109.4 . . ? P1 C13 H13A 109.4 . . ? N13 C13 H13B 109.4 . . ? P1 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N12 C14 N11 114.6(4) . . ? N12 C14 H14A 108.6 . . ? N11 C14 H14A 108.6 . . ? N12 C14 H14B 108.6 . . ? N11 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N12 C15 N13 113.4(4) . . ? N12 C15 H15A 108.9 . . ? N13 C15 H15A 108.9 . . ? N12 C15 H15B 108.9 . . ? N13 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N13 C16 N11 114.4(4) . . ? N13 C16 H16A 108.7 . . ? N11 C16 H16A 108.7 . . ? N13 C16 H16B 108.7 . . ? N11 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N21 C21 P2 110.4(3) . . ? N21 C21 H21A 109.6 . . ? P2 C21 H21A 109.6 . . ? N21 C21 H21B 109.6 . . ? P2 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N22 C22 P2 110.8(3) . . ? N22 C22 H22A 109.5 . . ? P2 C22 H22A 109.5 . . ? N22 C22 H22B 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N23 C23 P2 110.5(4) . . ? N23 C23 H23A 109.6 . . ? P2 C23 H23A 109.6 . . ? N23 C23 H23B 109.6 . . ? P2 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N21 C24 N22 114.6(4) . . ? N21 C24 H24A 108.6 . . ? N22 C24 H24A 108.6 . . ? N21 C24 H24B 108.6 . . ? N22 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? N23 C25 N22 114.3(4) . . ? N23 C25 H25A 108.7 . . ? N22 C25 H25A 108.7 . . ? N23 C25 H25B 108.7 . . ? N22 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? N23 C26 N21 114.1(4) . . ? N23 C26 H26A 108.7 . . ? N21 C26 H26A 108.7 . . ? N23 C26 H26B 108.7 . . ? N21 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? N2 N1 Pt1 121.7(4) . . ? N3 N2 N1 174.1(6) . . ? N5 N4 Pt1 122.1(4) . . ? N6 N5 N4 174.6(5) . . ? C14 N11 C11 111.0(4) . . ? C14 N11 C16 107.8(4) . . ? C11 N11 C16 111.5(4) . . ? C14 N12 C15 109.7(4) . . ? C14 N12 C12 111.0(4) . . ? C15 N12 C12 111.4(4) . . ? C16 N13 C13 111.7(4) . . ? C16 N13 C15 109.1(4) . . ? C13 N13 C15 111.0(4) . . ? C24 N21 C21 110.9(4) . . ? C24 N21 C26 108.6(4) . . ? C21 N21 C26 111.3(4) . . ? C25 N22 C22 110.8(4) . . ? C25 N22 C24 108.5(4) . . ? C22 N22 C24 111.0(4) . . ? C26 N23 C25 108.5(4) . . ? C26 N23 C23 111.7(4) . . ? C25 N23 C23 111.8(4) . . ? H1A O1 H1B 88 . . ? H2A O2 H2B 112.9 . . ? H3A O3 H3B 105.5 . . ? H4A O4 H4B 120.8 . . ? H5A O5 H5B 121.8 . . ? C11 P1 C12 99.4(2) . . ? C11 P1 C13 99.3(2) . . ? C12 P1 C13 98.7(2) . . ? C11 P1 Pt1 114.70(17) . . ? C12 P1 Pt1 115.42(17) . . ? C13 P1 Pt1 125.18(17) . . ? C23 P2 C22 99.3(2) . . ? C23 P2 C21 99.8(2) . . ? C22 P2 C21 99.6(3) . . ? C23 P2 Pt1 114.93(18) . . ? C22 P2 Pt1 120.13(18) . . ? C21 P2 Pt1 119.27(18) . . ? N1 Pt1 N4 87.75(18) . . ? N1 Pt1 P2 173.05(13) . . ? N4 Pt1 P2 86.33(13) . . ? N1 Pt1 P1 90.64(13) . . ? N4 Pt1 P1 174.87(14) . . ? P2 Pt1 P1 95.56(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.324 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.169 # Attachment 'Compound_4_piotrptazoleb-revised.cif' data_piotrptazoleb _database_code_depnum_ccdc_archive 'CCDC 688072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 N14 P2 Pt' _chemical_formula_sum 'C26 H34 N14 P2 Pt' _chemical_formula_weight 799.70 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.176(2) _cell_length_b 16.211(6) _cell_length_c 17.019(6) _cell_angle_alpha 95.176(19) _cell_angle_beta 92.28(2) _cell_angle_gamma 94.15(2) _cell_volume 1690.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1148 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 23.51 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 4.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5127 _exptl_absorpt_correction_T_max 0.8473 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 14928 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.1830 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6209 _reflns_number_gt 4049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution ? _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^)+(0.0812P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6209 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 -0.012 0.000 0.500 273.9 17.2 _platon_squeeze_details ; ; 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 C11 C 0.056(2) 0.4664(9) 0.2159(8) 0.025(3) Uani 1 1 d . . . H11A H 0.0568 0.4601 0.2732 0.030 Uiso 1 1 calc R . . H11B H 0.2066 0.4821 0.2022 0.030 Uiso 1 1 calc R . . C12 C -0.324(2) 0.3619(10) 0.1855(10) 0.033(4) Uani 1 1 d . . . H12A H -0.4040 0.3151 0.1528 0.039 Uiso 1 1 calc R . . H12B H -0.3355 0.3515 0.2416 0.039 Uiso 1 1 calc R . . C13 C -0.063(2) 0.4043(10) 0.0617(8) 0.029(4) Uani 1 1 d . . . H13A H 0.0839 0.4200 0.0437 0.035 Uiso 1 1 calc R . . H13B H -0.1307 0.3590 0.0238 0.035 Uiso 1 1 calc R . . C14 C -0.414(2) 0.4572(10) 0.0880(9) 0.032(4) Uani 1 1 d . . . H14A H -0.4801 0.4079 0.0547 0.038 Uiso 1 1 calc R . . H14B H -0.5018 0.5043 0.0790 0.038 Uiso 1 1 calc R . . C15 C -0.308(2) 0.5132(10) 0.2201(9) 0.034(4) Uani 1 1 d . . . H15A H -0.3914 0.5625 0.2151 0.040 Uiso 1 1 calc R . . H15B H -0.3057 0.5017 0.2763 0.040 Uiso 1 1 calc R . . C16 C -0.089(2) 0.5449(8) 0.1140(8) 0.022(3) Uani 1 1 d . . . H16A H -0.1651 0.5955 0.1060 0.026 Uiso 1 1 calc R . . H16B H 0.0620 0.5550 0.0979 0.026 Uiso 1 1 calc R . . C21 C 0.281(2) 0.0623(10) 0.2524(9) 0.032(4) Uani 1 1 d . . . H21A H 0.3076 0.0922 0.3056 0.038 Uiso 1 1 calc R . . H21B H 0.1261 0.0420 0.2462 0.038 Uiso 1 1 calc R . . C22 C 0.648(2) 0.1476(9) 0.1921(9) 0.028(4) Uani 1 1 d . . . H22A H 0.7129 0.1778 0.1497 0.033 Uiso 1 1 calc R . . H22B H 0.6863 0.1806 0.2432 0.033 Uiso 1 1 calc R . . C23 C 0.327(2) 0.0575(9) 0.0884(8) 0.025(3) Uani 1 1 d . . . H23A H 0.1731 0.0367 0.0776 0.030 Uiso 1 1 calc R . . H23B H 0.3768 0.0846 0.0418 0.030 Uiso 1 1 calc R . . C24 C 0.649(2) 0.0182(11) 0.2542(11) 0.043(5) Uani 1 1 d . . . H24A H 0.6751 0.0525 0.3053 0.052 Uiso 1 1 calc R . . H24B H 0.7295 -0.0320 0.2572 0.052 Uiso 1 1 calc R . . C25 C 0.379(3) -0.0563(10) 0.1678(10) 0.040(4) Uani 1 1 d . . . H25A H 0.2211 -0.0721 0.1590 0.048 Uiso 1 1 calc R . . H25B H 0.4538 -0.1081 0.1691 0.048 Uiso 1 1 calc R . . C26 C 0.685(2) 0.0149(9) 0.1153(9) 0.030(4) Uani 1 1 d . . . H26A H 0.7341 0.0481 0.0725 0.035 Uiso 1 1 calc R . . H26B H 0.7688 -0.0350 0.1135 0.035 Uiso 1 1 calc R . . C41 C 0.210(2) 0.2302(9) -0.0674(8) 0.020(3) Uani 1 1 d . . . C42 C 0.314(2) 0.2448(9) -0.1411(8) 0.025(3) Uani 1 1 d . . . C43 C 0.209(3) 0.2185(12) -0.2157(11) 0.046(5) Uani 1 1 d . . . H43 H 0.0631 0.1948 -0.2178 0.055 Uiso 1 1 calc R . . C44 C 0.310(3) 0.2265(11) -0.2840(9) 0.041(4) Uani 1 1 d . . . H44 H 0.2365 0.2072 -0.3330 0.049 Uiso 1 1 calc R . . C45 C 0.523(3) 0.2626(11) -0.2832(10) 0.042(5) Uani 1 1 d . . . H45 H 0.5946 0.2680 -0.3310 0.051 Uiso 1 1 calc R . . C46 C 0.624(3) 0.2899(10) -0.2124(10) 0.036(4) Uani 1 1 d . . . H46 H 0.7647 0.3179 -0.2121 0.044 Uiso 1 1 calc R . . C47 C 0.533(3) 0.2788(9) -0.1402(9) 0.033(4) Uani 1 1 d . . . H47 H 0.6145 0.2935 -0.0918 0.040 Uiso 1 1 calc R . . C51 C 0.112(3) 0.3163(9) 0.4033(8) 0.027(4) Uani 1 1 d . . . C52 C -0.003(3) 0.3511(10) 0.4722(10) 0.040(4) Uani 1 1 d . . . C53 C 0.088(3) 0.3464(12) 0.5472(10) 0.054(5) Uani 1 1 d . . . H53 H 0.2232 0.3231 0.5540 0.065 Uiso 1 1 calc R . . C54 C -0.020(4) 0.3756(13) 0.6115(11) 0.061(6) Uani 1 1 d . . . H54 H 0.0389 0.3708 0.6632 0.073 Uiso 1 1 calc R . . C55 C -0.216(4) 0.4124(12) 0.6016(12) 0.058(6) Uani 1 1 d . . . H55 H -0.2819 0.4367 0.6466 0.070 Uiso 1 1 calc R . . C56 C -0.315(3) 0.4142(14) 0.5280(12) 0.065(6) Uani 1 1 d . . . H56 H -0.4548 0.4340 0.5217 0.078 Uiso 1 1 calc R . . C57 C -0.199(3) 0.3850(12) 0.4615(11) 0.050(5) Uani 1 1 d . . . H57 H -0.2573 0.3888 0.4096 0.060 Uiso 1 1 calc R . . N1 N 0.1367(19) 0.2306(8) 0.0525(7) 0.029(3) Uani 1 1 d . . . N2 N -0.0236(18) 0.1863(8) 0.0118(8) 0.031(3) Uani 1 1 d . . . N3 N 0.0209(19) 0.1847(9) -0.0661(7) 0.032(3) Uani 1 1 d . . . N4 N 0.2927(18) 0.2576(7) 0.0040(7) 0.023(3) Uani 1 1 d . . . N5 N 0.1718(19) 0.2758(8) 0.2888(8) 0.030(3) Uani 1 1 d . . . N6 N 0.346(2) 0.2547(9) 0.3343(8) 0.040(3) Uani 1 1 d . . . N7 N 0.302(2) 0.2805(9) 0.4070(8) 0.045(4) Uani 1 1 d . . . N8 N 0.0307(18) 0.3139(8) 0.3288(7) 0.028(3) Uani 1 1 d . . . N11 N -0.0836(18) 0.5333(7) 0.1983(7) 0.025(3) Uani 1 1 d . . . N12 N -0.424(2) 0.4405(8) 0.1717(7) 0.029(3) Uani 1 1 d . . . N13 N -0.1945(19) 0.4764(8) 0.0621(7) 0.030(3) Uani 1 1 d . . . N21 N 0.416(2) -0.0076(8) 0.2444(7) 0.030(3) Uani 1 1 d . . . N22 N 0.7371(19) 0.0649(8) 0.1925(8) 0.034(3) Uani 1 1 d . . . N23 N 0.456(2) -0.0116(8) 0.1001(8) 0.033(3) Uani 1 1 d . . . P1 P -0.0372(6) 0.3667(2) 0.1611(2) 0.0209(8) Uani 1 1 d . . . P2 P 0.3478(6) 0.1344(2) 0.1756(2) 0.0229(9) Uani 1 1 d . . . Pt1 Pt 0.15885(9) 0.25187(4) 0.17016(4) 0.01992(19) 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 C11 0.027(8) 0.036(9) 0.014(8) 0.013(7) 0.005(6) 0.000(7) C12 0.020(8) 0.030(9) 0.048(11) 0.001(8) 0.004(7) 0.007(7) C13 0.037(9) 0.040(10) 0.012(8) 0.008(7) -0.002(6) 0.008(7) C14 0.019(8) 0.041(10) 0.038(10) 0.015(8) -0.001(7) 0.011(7) C15 0.044(10) 0.038(10) 0.026(9) 0.021(8) 0.011(7) 0.019(8) C16 0.028(8) 0.012(7) 0.025(8) 0.005(6) 0.000(6) 0.003(6) C21 0.023(8) 0.038(10) 0.034(10) 0.004(8) -0.003(7) 0.003(7) C22 0.037(9) 0.027(9) 0.020(8) -0.006(7) 0.010(7) 0.011(7) C23 0.027(8) 0.030(9) 0.018(8) -0.001(7) 0.006(6) 0.010(7) C24 0.024(9) 0.046(11) 0.059(13) 0.013(10) -0.015(8) 0.003(8) C25 0.038(10) 0.032(10) 0.052(12) 0.020(9) 0.005(8) -0.002(8) C26 0.021(8) 0.027(9) 0.044(10) 0.011(8) 0.005(7) 0.014(7) C41 0.027(8) 0.021(8) 0.012(7) 0.004(6) 0.007(6) 0.002(6) C42 0.039(9) 0.032(9) 0.009(7) 0.007(6) 0.005(6) 0.016(7) C43 0.030(10) 0.067(13) 0.044(12) 0.009(10) 0.009(8) 0.024(9) C44 0.051(11) 0.053(12) 0.021(9) 0.006(8) -0.004(8) 0.013(9) C45 0.066(13) 0.043(11) 0.021(9) 0.001(8) 0.018(8) 0.020(10) C46 0.035(9) 0.046(11) 0.033(10) 0.013(8) 0.022(7) 0.014(8) C47 0.052(11) 0.021(9) 0.025(9) 0.001(7) -0.003(7) -0.001(8) C51 0.055(10) 0.014(8) 0.012(8) -0.001(6) 0.010(7) 0.001(7) C52 0.053(11) 0.032(10) 0.036(11) 0.000(8) 0.020(8) 0.002(8) C53 0.082(15) 0.067(14) 0.014(9) 0.014(9) -0.001(9) -0.004(11) C54 0.091(17) 0.064(14) 0.025(11) -0.010(10) 0.016(10) 0.001(12) C55 0.080(15) 0.053(13) 0.041(13) -0.001(10) 0.033(11) -0.010(11) C56 0.065(14) 0.078(16) 0.048(14) -0.015(12) 0.030(11) 0.001(12) C57 0.046(11) 0.074(14) 0.037(11) 0.005(10) 0.009(8) 0.038(10) N1 0.030(7) 0.036(8) 0.021(7) -0.006(6) 0.007(6) 0.004(6) N2 0.016(6) 0.040(8) 0.035(8) -0.002(6) -0.002(5) -0.006(6) N3 0.026(7) 0.052(9) 0.017(7) 0.007(6) 0.006(5) -0.005(6) N4 0.030(7) 0.021(7) 0.017(7) -0.008(5) 0.007(5) -0.006(5) N5 0.021(7) 0.034(8) 0.035(8) -0.001(6) -0.001(6) 0.005(6) N6 0.047(8) 0.048(9) 0.022(7) -0.008(6) -0.007(6) 0.001(7) N7 0.054(10) 0.054(10) 0.025(8) -0.016(7) -0.009(7) 0.019(8) N8 0.020(6) 0.043(8) 0.020(7) -0.003(6) 0.004(5) 0.005(6) N11 0.018(6) 0.021(7) 0.039(8) -0.002(6) 0.008(5) 0.016(5) N12 0.047(8) 0.022(7) 0.020(7) 0.003(6) 0.005(6) 0.009(6) N13 0.022(7) 0.039(8) 0.029(8) 0.006(6) -0.004(5) 0.009(6) N21 0.033(7) 0.035(8) 0.025(7) 0.009(6) -0.003(6) 0.010(6) N22 0.019(7) 0.039(9) 0.044(9) 0.002(7) -0.006(6) 0.005(6) N23 0.031(7) 0.037(8) 0.031(8) 0.002(6) -0.003(6) 0.010(6) P1 0.0184(19) 0.025(2) 0.020(2) 0.0020(17) 0.0024(15) 0.0029(16) P2 0.020(2) 0.027(2) 0.021(2) 0.0000(17) 0.0019(15) 0.0057(16) Pt1 0.0173(3) 0.0248(3) 0.0184(3) 0.0036(2) 0.00251(19) 0.0039(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 C11 N11 1.476(17) . ? C11 P1 1.834(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N12 1.491(18) . ? C12 P1 1.831(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N13 1.471(18) . ? C13 P1 1.855(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N13 1.461(18) . ? C14 N12 1.476(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N11 1.470(19) . ? C15 N12 1.50(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N13 1.453(18) . ? C16 N11 1.464(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 N21 1.452(19) . ? C21 P2 1.869(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N22 1.485(18) . ? C22 P2 1.860(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N23 1.443(17) . ? C23 P2 1.845(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N22 1.45(2) . ? C24 N21 1.467(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N21 1.46(2) . ? C25 N23 1.49(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N23 1.456(18) . ? C26 N22 1.49(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C41 N4 1.324(17) . ? C41 N3 1.339(17) . ? C41 C42 1.462(18) . ? C42 C47 1.42(2) . ? C42 C43 1.42(2) . ? C43 C44 1.36(2) . ? C43 H43 0.9500 . ? C44 C45 1.40(2) . ? C44 H44 0.9500 . ? C45 C46 1.36(2) . ? C45 H45 0.9500 . ? C46 C47 1.39(2) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C51 N8 1.342(18) . ? C51 N7 1.348(19) . ? C51 C52 1.49(2) . ? C52 C57 1.38(2) . ? C52 C53 1.38(2) . ? C53 C54 1.37(3) . ? C53 H53 0.9500 . ? C54 C55 1.40(3) . ? C54 H54 0.9500 . ? C55 C56 1.38(3) . ? C55 H55 0.9500 . ? C56 C57 1.43(2) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? N1 N2 1.315(16) . ? N1 N4 1.367(16) . ? N1 Pt1 1.999(12) . ? N2 N3 1.363(17) . ? N5 N8 1.286(16) . ? N5 N6 1.383(17) . ? N5 Pt1 2.019(13) . ? N6 N7 1.314(18) . ? P1 Pt1 2.306(4) . ? P2 Pt1 2.311(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 N11 C11 P1 112.3(9) . . ? N11 C11 H11A 109.1 . . ? P1 C11 H11A 109.1 . . ? N11 C11 H11B 109.1 . . ? P1 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N12 C12 P1 111.7(10) . . ? N12 C12 H12A 109.3 . . ? P1 C12 H12A 109.3 . . ? N12 C12 H12B 109.3 . . ? P1 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N13 C13 P1 111.6(10) . . ? N13 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? N13 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? N13 C14 N12 114.7(12) . . ? N13 C14 H14A 108.6 . . ? N12 C14 H14A 108.6 . . ? N13 C14 H14B 108.6 . . ? N12 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N11 C15 N12 114.7(12) . . ? N11 C15 H15A 108.6 . . ? N12 C15 H15A 108.6 . . ? N11 C15 H15B 108.6 . . ? N12 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N13 C16 N11 115.6(11) . . ? N13 C16 H16A 108.4 . . ? N11 C16 H16A 108.4 . . ? N13 C16 H16B 108.4 . . ? N11 C16 H16B 108.4 . . ? H16A C16 H16B 107.4 . . ? N21 C21 P2 109.8(10) . . ? N21 C21 H21A 109.7 . . ? P2 C21 H21A 109.7 . . ? N21 C21 H21B 109.7 . . ? P2 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N22 C22 P2 109.7(10) . . ? N22 C22 H22A 109.7 . . ? P2 C22 H22A 109.7 . . ? N22 C22 H22B 109.7 . . ? P2 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N23 C23 P2 111.7(10) . . ? N23 C23 H23A 109.3 . . ? P2 C23 H23A 109.3 . . ? N23 C23 H23B 109.3 . . ? P2 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? N22 C24 N21 115.5(12) . . ? N22 C24 H24A 108.4 . . ? N21 C24 H24A 108.4 . . ? N22 C24 H24B 108.4 . . ? N21 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? N21 C25 N23 113.7(12) . . ? N21 C25 H25A 108.8 . . ? N23 C25 H25A 108.8 . . ? N21 C25 H25B 108.8 . . ? N23 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N23 C26 N22 114.6(12) . . ? N23 C26 H26A 108.6 . . ? N22 C26 H26A 108.6 . . ? N23 C26 H26B 108.6 . . ? N22 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? N4 C41 N3 113.2(12) . . ? N4 C41 C42 124.6(13) . . ? N3 C41 C42 122.2(13) . . ? C47 C42 C43 117.6(13) . . ? C47 C42 C41 120.7(13) . . ? C43 C42 C41 121.4(14) . . ? C44 C43 C42 121.6(16) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C43 C44 C45 120.7(16) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 118.4(15) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C45 C46 C47 123.4(16) . . ? C45 C46 H46 118.3 . . ? C47 C46 H46 118.3 . . ? C46 C47 C42 118.0(14) . . ? C46 C47 H47 121.0 . . ? C42 C47 H47 121.0 . . ? N8 C51 N7 111.8(13) . . ? N8 C51 C52 122.6(15) . . ? N7 C51 C52 125.5(14) . . ? C57 C52 C53 121.0(17) . . ? C57 C52 C51 120.5(16) . . ? C53 C52 C51 118.5(17) . . ? C54 C53 C52 119(2) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 120.4(19) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C56 C55 C54 121.3(18) . . ? C56 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C55 C56 C57 117(2) . . ? C55 C56 H56 121.3 . . ? C57 C56 H56 121.3 . . ? C52 C57 C56 120.3(18) . . ? C52 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? N2 N1 N4 111.1(11) . . ? N2 N1 Pt1 124.9(10) . . ? N4 N1 Pt1 123.9(9) . . ? N1 N2 N3 107.7(11) . . ? C41 N3 N2 104.9(11) . . ? C41 N4 N1 103.0(11) . . ? N8 N5 N6 113.7(13) . . ? N8 N5 Pt1 125.2(10) . . ? N6 N5 Pt1 121.0(10) . . ? N7 N6 N5 104.3(13) . . ? N6 N7 C51 107.2(13) . . ? N5 N8 C51 102.9(12) . . ? C16 N11 C15 107.7(11) . . ? C16 N11 C11 111.0(11) . . ? C15 N11 C11 110.7(11) . . ? C14 N12 C12 110.7(12) . . ? C14 N12 C15 107.4(12) . . ? C12 N12 C15 111.2(12) . . ? C16 N13 C14 109.2(12) . . ? C16 N13 C13 109.7(11) . . ? C14 N13 C13 112.0(12) . . ? C21 N21 C25 112.4(12) . . ? C21 N21 C24 112.4(13) . . ? C25 N21 C24 107.7(13) . . ? C24 N22 C22 111.9(13) . . ? C24 N22 C26 108.0(13) . . ? C22 N22 C26 110.4(11) . . ? C23 N23 C26 112.0(12) . . ? C23 N23 C25 110.7(12) . . ? C26 N23 C25 108.4(12) . . ? C12 P1 C11 99.3(7) . . ? C12 P1 C13 99.2(7) . . ? C11 P1 C13 97.6(7) . . ? C12 P1 Pt1 119.9(5) . . ? C11 P1 Pt1 120.5(5) . . ? C13 P1 Pt1 116.0(5) . . ? C23 P2 C22 99.7(6) . . ? C23 P2 C21 98.4(7) . . ? C22 P2 C21 99.4(7) . . ? C23 P2 Pt1 118.0(5) . . ? C22 P2 Pt1 118.5(5) . . ? C21 P2 Pt1 118.9(5) . . ? N1 Pt1 N5 177.9(5) . . ? N1 Pt1 P1 89.3(4) . . ? N5 Pt1 P1 88.8(4) . . ? N1 Pt1 P2 89.1(4) . . ? N5 Pt1 P2 92.8(4) . . ? P1 Pt1 P2 178.00(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.303 _refine_diff_density_min -2.281 _refine_diff_density_rms 0.285