# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Frederic-Georges Fontaine' _publ_contact_author_email FREDERIC.FONTAINE@CHM.ULAVAL.CA _publ_section_title ; Synthesis and Solid-State Characterization of Platinum Complexes with Hexadentate Amino- and Iminophosphine Ligands ; loop_ _publ_author_name 'Frederic-Georges Fontaine' 'Bryan E.G. Lucier' 'Robert Schurko' "Marie-H\'el\`ene Thibault" # Attachment '1.cif' data_ff _database_code_depnum_ccdc_archive 'CCDC 718421' _audit_update_record ; 2009-01-28 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H54 N3 P3' _chemical_formula_weight 946.00 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' _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 14.094(4) _cell_length_b 14.538(4) _cell_length_c 14.725(4) _cell_angle_alpha 94.118(4) _cell_angle_beta 109.789(4) _cell_angle_gamma 111.535(4) _cell_volume 2573.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 8087 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.10 _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.221 #_exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9391 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 17424 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11038 _reflns_number_gt 7424 _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^)+(0.0651P)^2^+1.6991P] 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 constr _refine_ls_number_reflns 11038 _refine_ls_number_parameters 838 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 P1 P 0.26244(6) 0.55256(5) 0.40249(5) 0.03750(17) Uani 1 1 d . . . P2 P 0.64194(6) 0.43538(6) 0.89920(5) 0.04333(19) Uani 1 1 d . . . P3 P 1.19359(6) 0.94409(6) 0.72375(5) 0.04311(19) Uani 1 1 d . . . C1 C 0.6633(2) 0.7883(2) 0.5984(2) 0.0405(6) Uani 1 1 d . . . C2 C 0.6758(2) 0.7647(2) 0.7008(2) 0.0432(6) Uani 1 1 d . . . C3 C 0.7761(2) 0.7394(2) 0.7451(2) 0.0416(6) Uani 1 1 d . . . C4 C 0.8815(3) 0.8235(2) 0.7481(2) 0.0471(7) Uani 1 1 d . . . C5 C 0.8698(2) 0.8507(2) 0.6474(2) 0.0444(6) Uani 1 1 d . . . C6 C 0.7698(2) 0.8753(2) 0.6045(2) 0.0432(6) Uani 1 1 d . . . N7 N 0.5686(2) 0.81491(17) 0.56316(16) 0.0438(5) Uani 1 1 d . . . C8 C 0.4790(2) 0.7497(2) 0.49614(19) 0.0390(6) Uani 1 1 d . . . C9 C 0.3755(2) 0.76513(19) 0.46251(18) 0.0383(6) Uani 1 1 d . . . C10 C 0.2702(2) 0.6824(2) 0.42372(17) 0.0378(6) Uani 1 1 d . . . C11 C 0.1762(3) 0.7029(2) 0.3989(2) 0.0456(7) Uani 1 1 d . . . C12 C 0.1866(3) 0.8028(3) 0.4114(2) 0.0545(8) Uani 1 1 d . . . C13 C 0.2884(3) 0.8826(3) 0.4475(2) 0.0556(8) Uani 1 1 d . . . C14 C 0.3824(3) 0.8638(2) 0.4737(2) 0.0496(7) Uani 1 1 d . . . C15 C 0.1143(2) 0.4735(2) 0.3640(2) 0.0426(6) Uani 1 1 d . . . C16 C 0.0465(3) 0.4598(3) 0.2650(2) 0.0569(8) Uani 1 1 d . . . C17 C -0.0668(3) 0.4028(3) 0.2296(3) 0.0670(9) Uani 1 1 d . . . C18 C -0.1145(3) 0.3556(3) 0.2909(3) 0.0690(10) Uani 1 1 d . . . C19 C -0.0488(3) 0.3653(3) 0.3879(3) 0.0729(11) Uani 1 1 d . . . C20 C 0.0650(3) 0.4245(3) 0.4249(3) 0.0586(8) Uani 1 1 d . . . C21 C 0.3240(2) 0.54157(19) 0.53038(18) 0.0371(6) Uani 1 1 d . . . C22 C 0.3100(3) 0.5856(2) 0.6097(2) 0.0490(7) Uani 1 1 d . . . C23 C 0.3635(3) 0.5781(3) 0.7051(2) 0.0572(8) Uani 1 1 d . . . C24 C 0.4330(3) 0.5289(2) 0.7233(2) 0.0544(8) Uani 1 1 d . . . C25 C 0.4486(3) 0.4861(2) 0.6463(2) 0.0495(7) Uani 1 1 d . . . C26 C 0.3936(2) 0.4913(2) 0.5507(2) 0.0417(6) Uani 1 1 d . . . N27 N 0.79232(19) 0.73066(18) 0.84770(16) 0.0438(5) Uani 1 1 d . . . C28 C 0.7825(2) 0.6462(2) 0.8703(2) 0.0403(6) Uani 1 1 d . . . C29 C 0.8032(2) 0.6375(2) 0.97464(19) 0.0388(6) Uani 1 1 d . . . C30 C 0.7473(2) 0.5469(2) 0.99901(19) 0.0397(6) Uani 1 1 d . . . C31 C 0.7668(3) 0.5473(2) 1.0990(2) 0.0492(7) Uani 1 1 d . . . C32 C 0.8389(3) 0.6341(3) 1.1724(2) 0.0546(8) Uani 1 1 d . . . C33 C 0.8940(3) 0.7224(3) 1.1482(2) 0.0504(7) Uani 1 1 d . . . C34 C 0.8774(2) 0.7237(2) 1.0501(2) 0.0452(6) Uani 1 1 d . . . C35 C 0.5719(2) 0.3520(2) 0.9664(2) 0.0411(6) Uani 1 1 d . . . C36 C 0.4719(3) 0.3522(2) 0.9632(3) 0.0547(8) Uani 1 1 d . . . C37 C 0.4153(3) 0.2924(3) 1.0136(3) 0.0627(9) Uani 1 1 d . . . C38 C 0.4561(3) 0.2321(2) 1.0663(2) 0.0538(8) Uani 1 1 d . . . C39 C 0.5547(2) 0.2297(2) 1.0698(2) 0.0435(6) Uani 1 1 d . . . C40 C 0.6123(2) 0.2897(2) 1.02007(19) 0.0398(6) Uani 1 1 d . . . C41 C 0.7237(2) 0.3704(2) 0.87593(19) 0.0404(6) Uani 1 1 d . . . C42 C 0.6652(3) 0.2775(3) 0.8085(2) 0.0508(7) Uani 1 1 d . . . C43 C 0.7189(3) 0.2218(3) 0.7865(2) 0.0530(8) Uani 1 1 d . . . C44 C 0.8327(3) 0.2595(2) 0.8292(2) 0.0520(7) Uani 1 1 d . . . C45 C 0.8926(3) 0.3517(3) 0.8950(3) 0.0588(8) Uani 1 1 d . . . C46 C 0.8381(3) 0.4071(2) 0.9189(2) 0.0509(7) Uani 1 1 d . . . N47 N 0.97967(19) 0.92961(18) 0.66208(17) 0.0480(6) Uani 1 1 d . . . C48 C 0.9912(3) 1.0031(2) 0.6221(2) 0.0466(7) Uani 1 1 d . . . C49 C 1.1028(2) 1.0791(2) 0.63951(18) 0.0417(6) Uani 1 1 d . . . C50 C 1.2003(2) 1.0653(2) 0.68905(19) 0.0418(6) Uani 1 1 d . . . C51 C 1.3017(3) 1.1444(2) 0.7029(2) 0.0532(7) Uani 1 1 d . . . C52 C 1.3067(3) 1.2329(3) 0.6713(3) 0.0572(8) Uani 1 1 d . . . C53 C 1.2113(3) 1.2446(2) 0.6216(2) 0.0512(7) Uani 1 1 d . . . C54 C 1.1099(3) 1.1674(2) 0.6051(2) 0.0480(7) Uani 1 1 d . . . C55 C 1.1800(2) 0.9551(2) 0.84343(18) 0.0379(6) Uani 1 1 d . . . C56 C 1.1736(3) 1.0365(2) 0.8910(2) 0.0512(7) Uani 1 1 d . . . C57 C 1.1570(3) 1.0348(3) 0.9794(2) 0.0574(8) Uani 1 1 d . . . C58 C 1.1453(3) 0.9505(3) 1.0190(2) 0.0585(8) Uani 1 1 d . . . C59 C 1.1529(3) 0.8696(3) 0.9736(2) 0.0630(9) Uani 1 1 d . . . C60 C 1.1699(3) 0.8716(2) 0.8863(2) 0.0512(7) Uani 1 1 d . . . C61 C 1.3406(2) 0.9635(2) 0.76835(19) 0.0439(6) Uani 1 1 d . . . C62 C 1.4246(3) 1.0229(2) 0.8586(2) 0.0472(7) Uani 1 1 d . . . C63 C 1.5315(3) 1.0309(2) 0.8842(2) 0.0517(7) Uani 1 1 d . . . C64 C 1.5574(3) 0.9795(3) 0.8204(2) 0.0552(8) Uani 1 1 d . . . C65 C 1.4751(3) 0.9190(3) 0.7313(2) 0.0629(9) Uani 1 1 d . . . C66 C 1.3679(3) 0.9105(3) 0.7056(2) 0.0555(8) Uani 1 1 d . . . H1 H 0.649(2) 0.727(2) 0.556(2) 0.042(7) Uiso 1 1 d . . . H2A H 0.610(2) 0.707(2) 0.698(2) 0.049(8) Uiso 1 1 d . . . H2B H 0.686(2) 0.825(2) 0.745(2) 0.056(9) Uiso 1 1 d . . . H3 H 0.761(2) 0.674(2) 0.704(2) 0.042(7) Uiso 1 1 d . . . H4A H 0.949(3) 0.800(2) 0.775(2) 0.067(10) Uiso 1 1 d . . . H4B H 0.892(2) 0.882(2) 0.787(2) 0.037(7) Uiso 1 1 d . . . H5 H 0.857(2) 0.789(2) 0.598(2) 0.056(8) Uiso 1 1 d . . . H6A H 0.759(2) 0.889(2) 0.539(2) 0.049(8) Uiso 1 1 d . . . H6B H 0.778(3) 0.934(3) 0.644(3) 0.069(10) Uiso 1 1 d . . . H8 H 0.477(2) 0.685(2) 0.468(2) 0.048(8) Uiso 1 1 d . . . H11 H 0.106(2) 0.6502(18) 0.3766(17) 0.022(6) Uiso 1 1 d . . . H12 H 0.123(3) 0.810(2) 0.394(2) 0.062(10) Uiso 1 1 d . . . H13 H 0.295(2) 0.951(2) 0.455(2) 0.056(9) Uiso 1 1 d . . . H14 H 0.455(3) 0.921(3) 0.500(2) 0.063(10) Uiso 1 1 d . . . H16 H 0.080(3) 0.492(2) 0.222(2) 0.060(9) Uiso 1 1 d . . . H17 H -0.116(3) 0.394(3) 0.161(3) 0.099(14) Uiso 1 1 d . . . H18 H -0.191(3) 0.312(3) 0.265(3) 0.080(11) Uiso 1 1 d . . . H19 H -0.080(3) 0.324(3) 0.430(3) 0.094(13) Uiso 1 1 d . . . H20 H 0.112(3) 0.432(2) 0.493(2) 0.060(9) Uiso 1 1 d . . . H22 H 0.261(2) 0.618(2) 0.595(2) 0.052(8) Uiso 1 1 d . . . H23 H 0.357(3) 0.611(3) 0.759(3) 0.079(11) Uiso 1 1 d . . . H24 H 0.474(3) 0.527(3) 0.790(3) 0.084(12) Uiso 1 1 d . . . H25 H 0.496(2) 0.452(2) 0.659(2) 0.052(8) Uiso 1 1 d . . . H26 H 0.403(3) 0.463(2) 0.498(2) 0.061(9) Uiso 1 1 d . . . H28 H 0.757(2) 0.583(2) 0.818(2) 0.046(8) Uiso 1 1 d . . . H31 H 0.727(3) 0.484(2) 1.115(2) 0.056(9) Uiso 1 1 d . . . H32 H 0.854(3) 0.634(3) 1.242(3) 0.075(11) Uiso 1 1 d . . . H33 H 0.942(2) 0.784(2) 1.196(2) 0.049(8) Uiso 1 1 d . . . H34 H 0.918(2) 0.785(2) 1.0323(19) 0.038(7) Uiso 1 1 d . . . H36 H 0.443(3) 0.397(2) 0.929(2) 0.057(9) Uiso 1 1 d . . . H37 H 0.347(3) 0.291(3) 1.008(3) 0.080(11) Uiso 1 1 d . . . H38 H 0.415(3) 0.188(3) 1.098(2) 0.069(10) Uiso 1 1 d . . . H39 H 0.583(2) 0.187(2) 1.104(2) 0.046(8) Uiso 1 1 d . . . H40 H 0.682(2) 0.2868(19) 1.0211(19) 0.039(7) Uiso 1 1 d . . . H42 H 0.589(3) 0.255(2) 0.779(2) 0.045(8) Uiso 1 1 d . . . H43 H 0.676(3) 0.158(3) 0.744(3) 0.065(10) Uiso 1 1 d . . . H44 H 0.871(2) 0.218(2) 0.813(2) 0.046(8) Uiso 1 1 d . . . H45 H 0.969(3) 0.376(3) 0.928(3) 0.078(12) Uiso 1 1 d . . . H46 H 0.880(3) 0.469(2) 0.965(2) 0.055(9) Uiso 1 1 d . . . H48 H 0.919(3) 1.012(3) 0.582(3) 0.088(12) Uiso 1 1 d . . . H51 H 1.370(3) 1.136(3) 0.737(3) 0.081(11) Uiso 1 1 d . . . H52 H 1.378(3) 1.287(3) 0.687(2) 0.070(10) Uiso 1 1 d . . . H53 H 1.212(2) 1.302(2) 0.600(2) 0.045(8) Uiso 1 1 d . . . H54 H 1.038(3) 1.173(2) 0.565(2) 0.061(9) Uiso 1 1 d . . . H56 H 1.184(3) 1.094(3) 0.864(3) 0.068(10) Uiso 1 1 d . . . H57 H 1.154(3) 1.097(3) 1.010(3) 0.079(11) Uiso 1 1 d . . . H58 H 1.129(3) 0.945(3) 1.077(3) 0.080(11) Uiso 1 1 d . . . H59 H 1.145(3) 0.814(3) 0.995(3) 0.086(13) Uiso 1 1 d . . . H60 H 1.170(3) 0.815(3) 0.855(2) 0.068(10) Uiso 1 1 d . . . H62 H 1.407(2) 1.057(2) 0.905(2) 0.055(9) Uiso 1 1 d . . . H63 H 1.589(3) 1.075(2) 0.943(2) 0.061(9) Uiso 1 1 d . . . H64 H 1.631(3) 0.986(2) 0.840(2) 0.051(8) Uiso 1 1 d . . . H65 H 1.495(3) 0.884(3) 0.691(3) 0.086(12) Uiso 1 1 d . . . H66 H 1.308(3) 0.866(2) 0.641(2) 0.063(9) 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 P1 0.0425(4) 0.0375(4) 0.0352(3) 0.0085(3) 0.0182(3) 0.0169(3) P2 0.0427(4) 0.0485(4) 0.0446(4) 0.0208(3) 0.0185(3) 0.0219(3) P3 0.0491(4) 0.0408(4) 0.0355(4) 0.0122(3) 0.0172(3) 0.0134(3) C1 0.0456(16) 0.0310(14) 0.0412(14) 0.0072(11) 0.0149(12) 0.0142(12) C2 0.0442(16) 0.0375(15) 0.0467(15) 0.0144(12) 0.0203(13) 0.0128(13) C3 0.0457(16) 0.0401(15) 0.0409(14) 0.0163(12) 0.0198(12) 0.0159(13) C4 0.0453(17) 0.0490(18) 0.0435(15) 0.0180(14) 0.0179(13) 0.0140(15) C5 0.0423(16) 0.0434(16) 0.0405(14) 0.0130(12) 0.0162(12) 0.0098(13) C6 0.0545(18) 0.0342(15) 0.0378(14) 0.0122(11) 0.0209(13) 0.0120(13) N7 0.0508(14) 0.0368(12) 0.0403(12) 0.0092(10) 0.0153(11) 0.0171(11) C8 0.0475(16) 0.0331(14) 0.0391(14) 0.0127(11) 0.0198(13) 0.0162(13) C9 0.0480(16) 0.0381(14) 0.0306(12) 0.0117(10) 0.0155(11) 0.0192(13) C10 0.0490(16) 0.0435(15) 0.0296(12) 0.0141(11) 0.0182(11) 0.0248(13) C11 0.0480(18) 0.0575(19) 0.0385(14) 0.0145(13) 0.0185(13) 0.0274(16) C12 0.068(2) 0.075(2) 0.0455(16) 0.0221(15) 0.0253(16) 0.052(2) C13 0.080(3) 0.0511(19) 0.0450(16) 0.0156(14) 0.0204(16) 0.0399(19) C14 0.065(2) 0.0400(16) 0.0432(15) 0.0147(13) 0.0172(15) 0.0246(16) C15 0.0448(16) 0.0421(15) 0.0420(14) 0.0080(12) 0.0183(12) 0.0185(13) C16 0.0522(19) 0.057(2) 0.0489(17) 0.0124(15) 0.0140(15) 0.0147(16) C17 0.054(2) 0.065(2) 0.058(2) 0.0005(17) 0.0042(18) 0.0181(18) C18 0.042(2) 0.068(2) 0.076(3) -0.0102(19) 0.0188(18) 0.0097(18) C19 0.058(2) 0.076(3) 0.072(2) 0.007(2) 0.037(2) 0.0072(19) C20 0.0529(19) 0.067(2) 0.0491(18) 0.0117(15) 0.0231(16) 0.0153(17) C21 0.0399(14) 0.0347(13) 0.0392(13) 0.0103(10) 0.0193(12) 0.0146(12) C22 0.0610(19) 0.0592(19) 0.0430(15) 0.0165(13) 0.0229(14) 0.0392(17) C23 0.072(2) 0.068(2) 0.0400(16) 0.0163(15) 0.0235(15) 0.0366(19) C24 0.0544(19) 0.0547(19) 0.0487(17) 0.0264(15) 0.0135(15) 0.0206(16) C25 0.0430(16) 0.0430(16) 0.067(2) 0.0266(14) 0.0207(15) 0.0209(14) C26 0.0425(16) 0.0321(14) 0.0558(17) 0.0144(12) 0.0246(14) 0.0155(12) N27 0.0459(14) 0.0477(14) 0.0431(12) 0.0166(10) 0.0220(11) 0.0198(11) C28 0.0388(15) 0.0438(16) 0.0466(15) 0.0166(12) 0.0219(12) 0.0200(13) C29 0.0393(15) 0.0450(15) 0.0435(14) 0.0166(12) 0.0206(12) 0.0245(13) C30 0.0424(15) 0.0454(15) 0.0428(14) 0.0187(12) 0.0206(12) 0.0254(13) C31 0.0565(19) 0.0533(18) 0.0474(16) 0.0220(14) 0.0260(15) 0.0259(16) C32 0.067(2) 0.065(2) 0.0426(16) 0.0178(15) 0.0253(16) 0.0342(18) C33 0.0520(18) 0.0553(19) 0.0469(16) 0.0084(14) 0.0175(14) 0.0278(16) C34 0.0446(16) 0.0473(17) 0.0518(16) 0.0180(13) 0.0221(14) 0.0236(14) C35 0.0389(15) 0.0436(15) 0.0465(15) 0.0131(12) 0.0207(12) 0.0192(13) C36 0.0467(18) 0.0555(19) 0.075(2) 0.0228(16) 0.0279(16) 0.0298(16) C37 0.0476(19) 0.065(2) 0.092(3) 0.0198(19) 0.0435(19) 0.0263(17) C38 0.0538(19) 0.0492(18) 0.064(2) 0.0127(15) 0.0381(17) 0.0141(15) C39 0.0491(17) 0.0412(16) 0.0417(15) 0.0107(12) 0.0230(13) 0.0153(14) C40 0.0376(15) 0.0441(15) 0.0432(14) 0.0127(12) 0.0203(12) 0.0184(13) C41 0.0480(16) 0.0470(16) 0.0356(13) 0.0219(12) 0.0224(12) 0.0220(13) C42 0.0481(19) 0.065(2) 0.0385(15) 0.0129(14) 0.0189(14) 0.0210(16) C43 0.072(2) 0.057(2) 0.0361(15) 0.0134(14) 0.0270(15) 0.0270(18) C44 0.069(2) 0.0586(19) 0.0507(17) 0.0268(15) 0.0349(16) 0.0376(18) C45 0.048(2) 0.061(2) 0.074(2) 0.0211(17) 0.0252(18) 0.0274(17) C46 0.0469(18) 0.0444(17) 0.0608(19) 0.0140(15) 0.0213(15) 0.0181(15) N47 0.0466(14) 0.0503(14) 0.0419(13) 0.0143(11) 0.0167(11) 0.0146(12) C48 0.0475(17) 0.0495(17) 0.0388(14) 0.0116(13) 0.0175(13) 0.0152(14) C49 0.0440(16) 0.0484(16) 0.0313(13) 0.0092(11) 0.0193(12) 0.0137(13) C50 0.0473(16) 0.0391(15) 0.0353(13) 0.0137(11) 0.0191(12) 0.0103(13) C51 0.0465(18) 0.0508(18) 0.0571(18) 0.0247(14) 0.0192(15) 0.0135(15) C52 0.0519(19) 0.0502(19) 0.065(2) 0.0247(15) 0.0278(16) 0.0105(16) C53 0.062(2) 0.0480(18) 0.0550(18) 0.0241(14) 0.0338(16) 0.0222(16) C54 0.0549(19) 0.0552(18) 0.0437(15) 0.0154(13) 0.0259(14) 0.0263(16) C55 0.0362(14) 0.0393(14) 0.0352(13) 0.0136(11) 0.0127(11) 0.0127(12) C56 0.065(2) 0.0479(18) 0.0454(16) 0.0188(13) 0.0235(15) 0.0250(16) C57 0.068(2) 0.064(2) 0.0470(17) 0.0130(15) 0.0255(16) 0.0324(18) C58 0.060(2) 0.073(2) 0.0411(16) 0.0196(15) 0.0252(15) 0.0201(18) C59 0.080(2) 0.056(2) 0.0500(18) 0.0296(16) 0.0279(17) 0.0206(19) C60 0.065(2) 0.0430(17) 0.0484(17) 0.0175(13) 0.0239(15) 0.0230(16) C61 0.0536(17) 0.0427(15) 0.0364(14) 0.0145(11) 0.0206(13) 0.0176(14) C62 0.0532(18) 0.0445(16) 0.0427(15) 0.0085(12) 0.0194(14) 0.0188(14) C63 0.0538(19) 0.0486(18) 0.0454(16) 0.0104(14) 0.0154(15) 0.0175(15) C64 0.056(2) 0.065(2) 0.0562(19) 0.0232(16) 0.0274(16) 0.0296(17) C65 0.073(2) 0.082(2) 0.0475(18) 0.0110(16) 0.0330(17) 0.039(2) C66 0.060(2) 0.069(2) 0.0372(15) 0.0071(14) 0.0203(15) 0.0257(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 P1 C15 1.829(3) . ? P1 C21 1.834(3) . ? P1 C10 1.847(3) . ? P2 C41 1.833(3) . ? P2 C35 1.838(3) . ? P2 C30 1.845(3) . ? P3 C55 1.838(3) . ? P3 C50 1.848(3) . ? P3 C61 1.851(3) . ? C1 N7 1.463(4) . ? C1 C6 1.535(4) . ? C1 C2 1.536(4) . ? C1 H1 0.96(3) . ? C2 C3 1.534(4) . ? C2 H2A 0.98(3) . ? C2 H2B 0.99(3) . ? C3 N27 1.472(3) . ? C3 C4 1.523(4) . ? C3 H3 1.00(3) . ? C4 C5 1.532(4) . ? C4 H4A 1.08(3) . ? C4 H4B 0.92(3) . ? C5 N47 1.481(4) . ? C5 C6 1.520(4) . ? C5 H5 1.03(3) . ? C6 H6A 0.97(3) . ? C6 H6B 0.95(4) . ? N7 C8 1.269(3) . ? C8 C9 1.479(4) . ? C8 H8 1.00(3) . ? C9 C14 1.396(4) . ? C9 C10 1.412(4) . ? C10 C11 1.399(4) . ? C11 C12 1.396(4) . ? C11 H11 0.93(2) . ? C12 C13 1.363(5) . ? C12 H12 0.89(3) . ? C13 C14 1.383(5) . ? C13 H13 0.97(3) . ? C14 H14 0.98(3) . ? C15 C20 1.394(4) . ? C15 C16 1.398(4) . ? C16 C17 1.382(5) . ? C16 H16 0.96(3) . ? C17 C18 1.378(5) . ? C17 H17 0.98(4) . ? C18 C19 1.377(5) . ? C18 H18 0.95(4) . ? C19 C20 1.393(5) . ? C19 H19 1.00(4) . ? C20 H20 0.97(3) . ? C21 C26 1.393(4) . ? C21 C22 1.398(4) . ? C22 C23 1.386(4) . ? C22 H22 0.95(3) . ? C23 C24 1.380(5) . ? C23 H23 0.95(4) . ? C24 C25 1.374(5) . ? C24 H24 0.96(4) . ? C25 C26 1.381(4) . ? C25 H25 0.94(3) . ? C26 H26 0.93(3) . ? N27 C28 1.266(3) . ? C28 C29 1.488(4) . ? C28 H28 1.02(3) . ? C29 C34 1.396(4) . ? C29 C30 1.408(4) . ? C30 C31 1.402(4) . ? C31 C32 1.383(4) . ? C31 H31 0.98(3) . ? C32 C33 1.378(5) . ? C32 H32 0.97(4) . ? C33 C34 1.386(4) . ? C33 H33 0.95(3) . ? C34 H34 0.98(3) . ? C35 C36 1.394(4) . ? C35 C40 1.395(4) . ? C36 C37 1.387(5) . ? C36 H36 0.98(3) . ? C37 C38 1.367(5) . ? C37 H37 0.94(4) . ? C38 C39 1.385(4) . ? C38 H38 0.96(3) . ? C39 C40 1.390(4) . ? C39 H39 0.93(3) . ? C40 H40 0.99(3) . ? C41 C46 1.383(4) . ? C41 C42 1.387(4) . ? C42 C43 1.383(4) . ? C42 H42 0.93(3) . ? C43 C44 1.375(5) . ? C43 H43 0.94(3) . ? C44 C45 1.371(5) . ? C44 H44 1.00(3) . ? C45 C46 1.401(4) . ? C45 H45 0.93(4) . ? C46 H46 0.93(3) . ? N47 C48 1.243(4) . ? C48 C49 1.473(4) . ? C48 H48 1.05(4) . ? C49 C54 1.396(4) . ? C49 C50 1.416(4) . ? C50 C51 1.403(4) . ? C51 C52 1.384(4) . ? C51 H51 0.98(4) . ? C52 C53 1.376(5) . ? C52 H52 0.95(4) . ? C53 C54 1.382(4) . ? C53 H53 0.91(3) . ? C54 H54 1.02(3) . ? C55 C56 1.378(4) . ? C55 C60 1.392(4) . ? C56 C57 1.398(4) . ? C56 H56 0.94(3) . ? C57 C58 1.375(5) . ? C57 H57 1.00(4) . ? C58 C59 1.367(5) . ? C58 H58 0.96(4) . ? C59 C60 1.385(4) . ? C59 H59 0.87(4) . ? C60 H60 0.91(3) . ? C61 C62 1.391(4) . ? C61 C66 1.396(4) . ? C62 C63 1.380(4) . ? C62 H62 0.97(3) . ? C63 C64 1.382(4) . ? C63 H63 0.94(3) . ? C64 C65 1.376(5) . ? C64 H64 0.95(3) . ? C65 C66 1.382(5) . ? C65 H65 0.92(4) . ? C66 H66 1.00(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 P1 C21 103.89(12) . . ? C15 P1 C10 102.61(12) . . ? C21 P1 C10 100.65(11) . . ? C41 P2 C35 100.68(12) . . ? C41 P2 C30 102.93(13) . . ? C35 P2 C30 102.28(12) . . ? C55 P3 C50 104.04(12) . . ? C55 P3 C61 99.03(12) . . ? C50 P3 C61 102.29(13) . . ? N7 C1 C6 111.0(2) . . ? N7 C1 C2 107.8(2) . . ? C6 C1 C2 110.7(2) . . ? N7 C1 H1 110.3(16) . . ? C6 C1 H1 110.2(16) . . ? C2 C1 H1 106.7(16) . . ? C3 C2 C1 111.3(2) . . ? C3 C2 H2A 108.0(17) . . ? C1 C2 H2A 111.7(17) . . ? C3 C2 H2B 109.3(18) . . ? C1 C2 H2B 108.2(18) . . ? H2A C2 H2B 108(2) . . ? N27 C3 C4 107.6(2) . . ? N27 C3 C2 108.7(2) . . ? C4 C3 C2 111.1(2) . . ? N27 C3 H3 111.0(16) . . ? C4 C3 H3 110.0(16) . . ? C2 C3 H3 108.4(16) . . ? C3 C4 C5 112.9(2) . . ? C3 C4 H4A 108.6(18) . . ? C5 C4 H4A 110.7(17) . . ? C3 C4 H4B 106.9(17) . . ? C5 C4 H4B 103.4(17) . . ? H4A C4 H4B 114(2) . . ? N47 C5 C6 117.5(2) . . ? N47 C5 C4 106.1(2) . . ? C6 C5 C4 111.4(2) . . ? N47 C5 H5 105.7(17) . . ? C6 C5 H5 107.0(17) . . ? C4 C5 H5 108.7(17) . . ? C5 C6 C1 111.2(2) . . ? C5 C6 H6A 112.2(17) . . ? C1 C6 H6A 108.7(17) . . ? C5 C6 H6B 111(2) . . ? C1 C6 H6B 107(2) . . ? H6A C6 H6B 106(3) . . ? C8 N7 C1 118.0(2) . . ? N7 C8 C9 122.1(2) . . ? N7 C8 H8 119.0(16) . . ? C9 C8 H8 118.8(16) . . ? C14 C9 C10 119.3(3) . . ? C14 C9 C8 119.1(3) . . ? C10 C9 C8 121.5(2) . . ? C11 C10 C9 118.3(3) . . ? C11 C10 P1 123.0(2) . . ? C9 C10 P1 118.70(19) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.0(15) . . ? C10 C11 H11 120.3(15) . . ? C13 C12 C11 121.0(3) . . ? C13 C12 H12 123(2) . . ? C11 C12 H12 116(2) . . ? C12 C13 C14 119.2(3) . . ? C12 C13 H13 120.3(18) . . ? C14 C13 H13 120.4(19) . . ? C13 C14 C9 121.6(3) . . ? C13 C14 H14 119.2(19) . . ? C9 C14 H14 119.2(19) . . ? C20 C15 C16 118.0(3) . . ? C20 C15 P1 125.1(2) . . ? C16 C15 P1 116.8(2) . . ? C17 C16 C15 120.9(3) . . ? C17 C16 H16 120.5(19) . . ? C15 C16 H16 118.6(19) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 117(2) . . ? C16 C17 H17 122(2) . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120(2) . . ? C17 C18 H18 120(2) . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19 121(2) . . ? C20 C19 H19 119(2) . . ? C19 C20 C15 120.6(3) . . ? C19 C20 H20 120.8(19) . . ? C15 C20 H20 118.7(19) . . ? C26 C21 C22 117.9(3) . . ? C26 C21 P1 118.29(19) . . ? C22 C21 P1 123.7(2) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 122.0(18) . . ? C21 C22 H22 117.6(18) . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 120(2) . . ? C22 C23 H23 120(2) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 119(2) . . ? C23 C24 H24 121(2) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 119.8(18) . . ? C26 C25 H25 120.4(18) . . ? C25 C26 C21 121.4(3) . . ? C25 C26 H26 121(2) . . ? C21 C26 H26 117(2) . . ? C28 N27 C3 119.1(2) . . ? N27 C28 C29 119.6(3) . . ? N27 C28 H28 121.7(16) . . ? C29 C28 H28 118.7(16) . . ? C34 C29 C30 119.4(2) . . ? C34 C29 C28 118.3(2) . . ? C30 C29 C28 122.2(2) . . ? C31 C30 C29 118.3(3) . . ? C31 C30 P2 121.9(2) . . ? C29 C30 P2 119.56(19) . . ? C32 C31 C30 121.4(3) . . ? C32 C31 H31 120.7(18) . . ? C30 C31 H31 118.0(18) . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32 119(2) . . ? C31 C32 H32 121(2) . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 122.4(18) . . ? C34 C33 H33 117.8(18) . . ? C33 C34 C29 121.0(3) . . ? C33 C34 H34 120.5(16) . . ? C29 C34 H34 118.4(16) . . ? C36 C35 C40 118.5(3) . . ? C36 C35 P2 117.1(2) . . ? C40 C35 P2 124.4(2) . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36 118.5(19) . . ? C35 C36 H36 121.1(19) . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37 120(2) . . ? C36 C37 H37 119(2) . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38 120(2) . . ? C39 C38 H38 119(2) . . ? C38 C39 C40 119.6(3) . . ? C38 C39 H39 121.5(18) . . ? C40 C39 H39 118.9(18) . . ? C39 C40 C35 120.8(3) . . ? C39 C40 H40 119.7(16) . . ? C35 C40 H40 119.5(16) . . ? C46 C41 C42 118.0(3) . . ? C46 C41 P2 125.3(2) . . ? C42 C41 P2 116.7(2) . . ? C43 C42 C41 121.3(3) . . ? C43 C42 H42 121.4(18) . . ? C41 C42 H42 117.3(18) . . ? C44 C43 C42 120.1(3) . . ? C44 C43 H43 121(2) . . ? C42 C43 H43 119(2) . . ? C45 C44 C43 119.7(3) . . ? C45 C44 H44 120.7(17) . . ? C43 C44 H44 119.5(17) . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45 121(2) . . ? C46 C45 H45 119(2) . . ? C41 C46 C45 120.7(3) . . ? C41 C46 H46 120.6(19) . . ? C45 C46 H46 118.7(19) . . ? C48 N47 C5 123.1(3) . . ? N47 C48 C49 120.5(3) . . ? N47 C48 H48 117(2) . . ? C49 C48 H48 122(2) . . ? C54 C49 C50 120.2(3) . . ? C54 C49 C48 117.2(3) . . ? C50 C49 C48 122.6(3) . . ? C51 C50 C49 116.9(3) . . ? C51 C50 P3 121.4(2) . . ? C49 C50 P3 121.4(2) . . ? C52 C51 C50 121.8(3) . . ? C52 C51 H51 120(2) . . ? C50 C51 H51 118(2) . . ? C53 C52 C51 120.7(3) . . ? C53 C52 H52 121(2) . . ? C51 C52 H52 118(2) . . ? C52 C53 C54 119.1(3) . . ? C52 C53 H53 123.0(18) . . ? C54 C53 H53 117.9(18) . . ? C53 C54 C49 121.3(3) . . ? C53 C54 H54 120.3(18) . . ? C49 C54 H54 118.4(18) . . ? C56 C55 C60 118.0(3) . . ? C56 C55 P3 125.5(2) . . ? C60 C55 P3 116.4(2) . . ? C55 C56 C57 120.9(3) . . ? C55 C56 H56 119(2) . . ? C57 C56 H56 120(2) . . ? C58 C57 C56 119.9(3) . . ? C58 C57 H57 124(2) . . ? C56 C57 H57 116(2) . . ? C59 C58 C57 120.0(3) . . ? C59 C58 H58 118(2) . . ? C57 C58 H58 122(2) . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 124(3) . . ? C60 C59 H59 116(3) . . ? C59 C60 C55 121.1(3) . . ? C59 C60 H60 118(2) . . ? C55 C60 H60 121(2) . . ? C62 C61 C66 117.5(3) . . ? C62 C61 P3 126.4(2) . . ? C66 C61 P3 116.1(2) . . ? C63 C62 C61 121.1(3) . . ? C63 C62 H62 119.4(18) . . ? C61 C62 H62 119.4(18) . . ? C62 C63 C64 120.5(3) . . ? C62 C63 H63 121(2) . . ? C64 C63 H63 118(2) . . ? C65 C64 C63 119.2(3) . . ? C65 C64 H64 121.9(18) . . ? C63 C64 H64 118.8(19) . . ? C64 C65 C66 120.4(3) . . ? C64 C65 H65 117(2) . . ? C66 C65 H65 122(2) . . ? C65 C66 C61 121.1(3) . . ? C65 C66 H66 120.2(18) . . ? C61 C66 H66 118.6(19) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.777 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.055 # Attachment '2.cif' data_mht004 _database_code_depnum_ccdc_archive 'CCDC 718422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H60 N3 P3' _chemical_formula_weight 952.05 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' _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 13.895(1) _cell_length_b 14.198(1) _cell_length_c 14.874(1) _cell_angle_alpha 94.163(1) _cell_angle_beta 106.963(1) _cell_angle_gamma 109.808(1) _cell_volume 2592.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6668 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.06 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9365 _exptl_absorpt_correction_T_max 0.9771 _exptl_absorpt_process_details 'XPREP (Bruker, 2005a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Bruker Smart APEX II CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31797 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.22 _reflns_number_total 12227 _reflns_number_gt 9657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2005b)' _computing_cell_refinement 'APEX 2 (Bruker, 2005b)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0750P)^2^+0.5544P] 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 12227 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 P1 P -0.21977(3) 0.55285(3) 0.26139(3) 0.03590(10) Uani 1 1 d . . . P2 P 0.72448(3) 0.95346(3) 0.58263(3) 0.03568(10) Uani 1 1 d . . . P3 P 0.34293(3) 1.05450(3) 0.10390(3) 0.03798(11) Uani 1 1 d . . . N1 N 0.02083(11) 0.52508(10) 0.30297(10) 0.0383(3) Uani 1 1 d . . . N3 N 0.25320(12) 0.78469(11) 0.17761(10) 0.0399(3) Uani 1 1 d . . . N2 N 0.40943(11) 0.67996(10) 0.47793(11) 0.0433(3) Uani 1 1 d . . . C6 C 0.21482(12) 0.60880(11) 0.39561(11) 0.0347(3) Uani 1 1 d . . . H6A H 0.2025 0.5914 0.4542 0.042 Uiso 1 1 calc R . . H6B H 0.2251 0.5525 0.3641 0.042 Uiso 1 1 calc R . . C11 C -0.13321(12) 0.41644(11) 0.34753(10) 0.0335(3) Uani 1 1 d . . . C12 C -0.22825(12) 0.42722(11) 0.29159(10) 0.0337(3) Uani 1 1 d . . . C3 C 0.23594(12) 0.75471(12) 0.26630(11) 0.0353(3) Uani 1 1 d . . . H3 H 0.2254 0.8093 0.3016 0.042 Uiso 1 1 calc R . . C5 C 0.31763(12) 0.70397(11) 0.42055(11) 0.0346(3) Uani 1 1 d . . . H5 H 0.3107 0.7590 0.4587 0.042 Uiso 1 1 calc R . . C2 C 0.13464(12) 0.65704(12) 0.24103(11) 0.0377(3) Uani 1 1 d . . . H2A H 0.0720 0.6690 0.2022 0.045 Uiso 1 1 calc R . . H2B H 0.1434 0.6037 0.2036 0.045 Uiso 1 1 calc R . . C1 C 0.11491(12) 0.62222(11) 0.33065(11) 0.0337(3) Uani 1 1 d . . . H1 H 0.0995 0.6737 0.3653 0.040 Uiso 1 1 calc R . . C4 C 0.33424(12) 0.73694(12) 0.32892(12) 0.0375(3) Uani 1 1 d . . . H4A H 0.3982 0.7993 0.3454 0.045 Uiso 1 1 calc R . . H4B H 0.3465 0.6847 0.2934 0.045 Uiso 1 1 calc R . . C7 C -0.02413(12) 0.50340(13) 0.37984(11) 0.0390(4) Uani 1 1 d . . . H7A H -0.0314 0.5642 0.4061 0.047 Uiso 1 1 calc R . . H7B H 0.0264 0.4871 0.4306 0.047 Uiso 1 1 calc R . . C14 C -0.33258(14) 0.25334(12) 0.29720(13) 0.0443(4) Uani 1 1 d . . . H14 H -0.3992 0.1992 0.2803 0.053 Uiso 1 1 calc R . . C16 C -0.14067(13) 0.32365(12) 0.37631(11) 0.0384(3) Uani 1 1 d . . . H16 H -0.0778 0.3159 0.4125 0.046 Uiso 1 1 calc R . . C8 C 0.19208(15) 0.84707(14) 0.13739(13) 0.0447(4) Uani 1 1 d . . . H8A H 0.2261 0.9151 0.1763 0.054 Uiso 1 1 calc R . . H8B H 0.1186 0.8174 0.1386 0.054 Uiso 1 1 calc R . . C13 C -0.32705(13) 0.34454(12) 0.26704(13) 0.0426(4) Uani 1 1 d . . . H13 H -0.3904 0.3508 0.2297 0.051 Uiso 1 1 calc R . . C15 C -0.23954(14) 0.24287(12) 0.35221(12) 0.0411(4) Uani 1 1 d . . . H15 H -0.2431 0.1820 0.3730 0.049 Uiso 1 1 calc R . . C9 C 0.51082(13) 0.76814(12) 0.52339(14) 0.0461(4) Uani 1 1 d . . . H9A H 0.5099 0.7985 0.5836 0.055 Uiso 1 1 calc R . . H9B H 0.5150 0.8186 0.4825 0.055 Uiso 1 1 calc R . . C22 C -0.44232(14) 0.48843(12) 0.14034(12) 0.0417(4) Uani 1 1 d . . . H22 H -0.4252 0.4581 0.0928 0.050 Uiso 1 1 calc R . . C21 C -0.36120(14) 0.54093(12) 0.22770(11) 0.0380(3) Uani 1 1 d . . . C26 C -0.38937(17) 0.58701(16) 0.29666(13) 0.0539(5) Uani 1 1 d . . . H26 H -0.3361 0.6236 0.3547 0.065 Uiso 1 1 calc R . . C23 C -0.54824(15) 0.48120(14) 0.12405(13) 0.0480(4) Uani 1 1 d . . . H23 H -0.6019 0.4460 0.0657 0.058 Uiso 1 1 calc R . . C24 C -0.57431(17) 0.52602(17) 0.19392(15) 0.0567(5) Uani 1 1 d . . . H24 H -0.6456 0.5205 0.1829 0.068 Uiso 1 1 calc R . . C25 C -0.49501(19) 0.57905(19) 0.28004(15) 0.0652(6) Uani 1 1 d . . . H25 H -0.5127 0.6095 0.3270 0.078 Uiso 1 1 calc R . . C31 C -0.19940(12) 0.54619(11) 0.14478(11) 0.0351(3) Uani 1 1 d . . . C34 C -0.15193(15) 0.55660(15) -0.02507(13) 0.0484(4) Uani 1 1 d . . . H34 H -0.1352 0.5601 -0.0812 0.058 Uiso 1 1 calc R . . C36 C -0.20812(14) 0.45951(12) 0.08898(12) 0.0413(4) Uani 1 1 d . . . H36 H -0.2299 0.3971 0.1083 0.050 Uiso 1 1 calc R . . C35 C -0.18474(15) 0.46422(14) 0.00434(13) 0.0468(4) Uani 1 1 d . . . H35 H -0.1912 0.4052 -0.0326 0.056 Uiso 1 1 calc R . . C32 C -0.16698(15) 0.63855(13) 0.11350(12) 0.0445(4) Uani 1 1 d . . . H32 H -0.1607 0.6977 0.1500 0.053 Uiso 1 1 calc R . . C33 C -0.14415(16) 0.64337(14) 0.02937(13) 0.0513(4) Uani 1 1 d . . . H33 H -0.1234 0.7054 0.0093 0.062 Uiso 1 1 calc R . . C42 C 0.71456(13) 0.81997(11) 0.56672(10) 0.0348(3) Uani 1 1 d . . . C41 C 0.61118(13) 0.74209(12) 0.54243(11) 0.0370(3) Uani 1 1 d . . . C43 C 0.80455(14) 0.79281(13) 0.58023(12) 0.0421(4) Uani 1 1 d . . . H43 H 0.8731 0.8436 0.5951 0.051 Uiso 1 1 calc R . . C46 C 0.60239(15) 0.64124(12) 0.53498(13) 0.0458(4) Uani 1 1 d . . . H46 H 0.5343 0.5896 0.5195 0.055 Uiso 1 1 calc R . . C44 C 0.79371(16) 0.69141(15) 0.57185(13) 0.0494(4) Uani 1 1 d . . . H44 H 0.8546 0.6746 0.5810 0.059 Uiso 1 1 calc R . . C45 C 0.69292(16) 0.61616(14) 0.55007(13) 0.0511(4) Uani 1 1 d . . . H45 H 0.6854 0.5482 0.5454 0.061 Uiso 1 1 calc R . . C51 C 0.67220(13) 0.96320(12) 0.45656(11) 0.0374(3) Uani 1 1 d . . . C53 C 0.54435(14) 1.00693(12) 0.33526(14) 0.0479(4) Uani 1 1 d . . . H53 H 0.4923 1.0359 0.3190 0.057 Uiso 1 1 calc R . . C52 C 0.59591(13) 1.00790(11) 0.43038(13) 0.0412(4) Uani 1 1 d . . . H52 H 0.5792 1.0391 0.4777 0.049 Uiso 1 1 calc R . . C56 C 0.69799(17) 0.91964(16) 0.38463(13) 0.0544(5) Uani 1 1 d . . . H56 H 0.7492 0.8897 0.4003 0.065 Uiso 1 1 calc R . . C54 C 0.57012(17) 0.96336(14) 0.26521(14) 0.0558(5) Uani 1 1 d . . . H54 H 0.5355 0.9625 0.2012 0.067 Uiso 1 1 calc R . . C55 C 0.6474(2) 0.92075(17) 0.28960(14) 0.0630(6) Uani 1 1 d . . . H55 H 0.6659 0.8925 0.2419 0.076 Uiso 1 1 calc R . . C61 C 0.87048(14) 1.02703(12) 0.61809(12) 0.0409(4) Uani 1 1 d . . . C66 C 0.93522(16) 1.02563(15) 0.70890(14) 0.0555(5) Uani 1 1 d . . . H66 H 0.9035 0.9853 0.7470 0.067 Uiso 1 1 calc R . . C63 C 1.02959(19) 1.14899(19) 0.60025(19) 0.0749(7) Uani 1 1 d . . . H63 H 1.0610 1.1922 0.5639 0.090 Uiso 1 1 calc R . . C62 C 0.91977(17) 1.09020(16) 0.56422(16) 0.0600(5) Uani 1 1 d . . . H62 H 0.8786 1.0930 0.5034 0.072 Uiso 1 1 calc R . . C65 C 1.04538(18) 1.08268(17) 0.74355(17) 0.0684(6) Uani 1 1 d . . . H65 H 1.0876 1.0794 0.8037 0.082 Uiso 1 1 calc R . . C64 C 1.09277(18) 1.14490(18) 0.68808(19) 0.0705(7) Uani 1 1 d . . . H64 H 1.1670 1.1835 0.7106 0.085 Uiso 1 1 calc R . . C72 C 0.24736(12) 0.94344(12) 0.01007(11) 0.0356(3) Uani 1 1 d . . . C71 C 0.18860(13) 0.85352(12) 0.03552(12) 0.0386(4) Uani 1 1 d . . . C73 C 0.23842(14) 0.94131(13) -0.08653(12) 0.0429(4) Uani 1 1 d . . . H73 H 0.2752 1.0005 -0.1049 0.051 Uiso 1 1 calc R . . C76 C 0.12650(14) 0.76646(13) -0.03500(14) 0.0466(4) Uani 1 1 d . . . H76 H 0.0876 0.7072 -0.0181 0.056 Uiso 1 1 calc R . . C74 C 0.17650(16) 0.85367(15) -0.15494(14) 0.0511(4) Uani 1 1 d . . . H74 H 0.1722 0.8542 -0.2185 0.061 Uiso 1 1 calc R . . C75 C 0.12086(15) 0.76519(15) -0.12909(15) 0.0516(4) Uani 1 1 d . . . H75 H 0.0801 0.7055 -0.1747 0.062 Uiso 1 1 calc R . . C81 C 0.25847(13) 1.12139(13) 0.12679(11) 0.0380(3) Uani 1 1 d . . . C85 C 0.08899(15) 1.14064(15) 0.11416(14) 0.0507(4) Uani 1 1 d . . . H85 H 0.0135 1.1149 0.0894 0.061 Uiso 1 1 calc R . . C84 C 0.14412(16) 1.23344(15) 0.17563(13) 0.0477(4) Uani 1 1 d . . . H84 H 0.1061 1.2708 0.1920 0.057 Uiso 1 1 calc R . . C82 C 0.31255(15) 1.21518(16) 0.18989(13) 0.0502(4) Uani 1 1 d . . . H82 H 0.3879 1.2405 0.2168 0.060 Uiso 1 1 calc R . . C86 C 0.14608(14) 1.08497(13) 0.08887(13) 0.0434(4) Uani 1 1 d . . . H86 H 0.1083 1.0229 0.0462 0.052 Uiso 1 1 calc R . . C83 C 0.25587(17) 1.27086(16) 0.21287(13) 0.0524(4) Uani 1 1 d . . . H83 H 0.2933 1.3340 0.2538 0.063 Uiso 1 1 calc R . . C91 C 0.41440(13) 1.13872(12) 0.03711(11) 0.0360(3) Uani 1 1 d . . . C92 C 0.37443(14) 1.20344(13) -0.01528(12) 0.0409(4) Uani 1 1 d . . . H92 H 0.3079 1.2058 -0.0169 0.049 Uiso 1 1 calc R . . C96 C 0.51470(13) 1.13813(13) 0.03941(13) 0.0425(4) Uani 1 1 d . . . H96 H 0.5430 1.0964 0.0748 0.051 Uiso 1 1 calc R . . C93 C 0.43326(15) 1.26388(13) -0.06476(13) 0.0456(4) Uani 1 1 d . . . H93 H 0.4060 1.3064 -0.0998 0.055 Uiso 1 1 calc R . . C95 C 0.57330(14) 1.19876(14) -0.01018(14) 0.0491(4) Uani 1 1 d . . . H95 H 0.6402 1.1973 -0.0083 0.059 Uiso 1 1 calc R . . C94 C 0.53259(15) 1.26118(13) -0.06221(14) 0.0492(4) Uani 1 1 d . . . H94 H 0.5719 1.3017 -0.0958 0.059 Uiso 1 1 calc R . . H1N H -0.0301(17) 0.5305(16) 0.2540(15) 0.056(6) Uiso 1 1 d . . . H3N H 0.3281(18) 0.8238(16) 0.1930(14) 0.054(5) Uiso 1 1 d . . . H2N H 0.3910(17) 0.6472(17) 0.5221(16) 0.059(6) 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 P1 0.0393(2) 0.02927(19) 0.0340(2) 0.00999(15) 0.01130(17) 0.00686(16) P2 0.0379(2) 0.0322(2) 0.0364(2) 0.00610(15) 0.01588(17) 0.00987(16) P3 0.0366(2) 0.0474(2) 0.0393(2) 0.02256(18) 0.01645(17) 0.02111(18) N1 0.0299(7) 0.0444(7) 0.0313(6) 0.0151(6) 0.0093(5) 0.0019(6) N3 0.0368(7) 0.0453(8) 0.0522(8) 0.0282(6) 0.0261(6) 0.0198(6) N2 0.0326(7) 0.0334(7) 0.0501(8) 0.0144(6) 0.0022(6) 0.0046(5) C6 0.0316(7) 0.0322(7) 0.0363(8) 0.0146(6) 0.0096(6) 0.0071(6) C11 0.0322(7) 0.0372(8) 0.0269(7) 0.0116(6) 0.0125(6) 0.0048(6) C12 0.0340(8) 0.0320(7) 0.0331(7) 0.0128(6) 0.0134(6) 0.0068(6) C3 0.0357(8) 0.0344(7) 0.0446(8) 0.0193(6) 0.0215(7) 0.0149(6) C5 0.0302(7) 0.0299(7) 0.0400(8) 0.0099(6) 0.0095(6) 0.0082(6) C2 0.0313(7) 0.0422(8) 0.0376(8) 0.0194(7) 0.0116(6) 0.0091(6) C1 0.0293(7) 0.0339(7) 0.0371(8) 0.0149(6) 0.0128(6) 0.0080(6) C4 0.0299(7) 0.0351(8) 0.0486(9) 0.0154(7) 0.0163(7) 0.0095(6) C7 0.0324(8) 0.0450(9) 0.0303(7) 0.0144(6) 0.0096(6) 0.0025(6) C14 0.0362(8) 0.0340(8) 0.0573(10) 0.0183(7) 0.0176(8) 0.0034(6) C16 0.0368(8) 0.0448(9) 0.0341(8) 0.0163(7) 0.0129(6) 0.0134(7) C8 0.0504(10) 0.0481(9) 0.0589(11) 0.0327(8) 0.0342(9) 0.0286(8) C13 0.0315(8) 0.0367(8) 0.0532(10) 0.0171(7) 0.0111(7) 0.0062(6) C15 0.0464(9) 0.0355(8) 0.0436(9) 0.0186(7) 0.0201(7) 0.0115(7) C9 0.0337(8) 0.0329(8) 0.0596(11) 0.0061(7) 0.0040(8) 0.0084(7) C22 0.0475(9) 0.0379(8) 0.0385(8) 0.0078(7) 0.0131(7) 0.0157(7) C21 0.0452(9) 0.0353(8) 0.0353(8) 0.0124(6) 0.0140(7) 0.0160(7) C26 0.0586(11) 0.0669(12) 0.0377(9) 0.0033(8) 0.0100(8) 0.0321(10) C23 0.0465(10) 0.0494(10) 0.0424(9) 0.0109(8) 0.0076(8) 0.0171(8) C24 0.0511(11) 0.0720(13) 0.0576(11) 0.0184(10) 0.0172(9) 0.0357(10) C25 0.0680(13) 0.0933(17) 0.0479(11) 0.0066(11) 0.0183(10) 0.0495(13) C31 0.0337(8) 0.0331(7) 0.0356(8) 0.0123(6) 0.0111(6) 0.0084(6) C34 0.0467(10) 0.0594(11) 0.0388(9) 0.0163(8) 0.0172(8) 0.0159(8) C36 0.0479(9) 0.0351(8) 0.0419(9) 0.0138(7) 0.0156(7) 0.0153(7) C35 0.0529(10) 0.0493(10) 0.0423(9) 0.0101(7) 0.0166(8) 0.0234(8) C32 0.0557(10) 0.0332(8) 0.0428(9) 0.0138(7) 0.0187(8) 0.0115(7) C33 0.0583(11) 0.0442(9) 0.0467(10) 0.0222(8) 0.0199(9) 0.0090(8) C42 0.0384(8) 0.0347(7) 0.0288(7) 0.0072(6) 0.0087(6) 0.0129(6) C41 0.0367(8) 0.0341(7) 0.0333(7) 0.0063(6) 0.0041(6) 0.0117(6) C43 0.0404(9) 0.0459(9) 0.0394(8) 0.0076(7) 0.0125(7) 0.0165(7) C46 0.0448(9) 0.0324(8) 0.0462(9) 0.0046(7) 0.0010(7) 0.0102(7) C44 0.0518(10) 0.0554(11) 0.0460(10) 0.0078(8) 0.0116(8) 0.0309(9) C45 0.0593(11) 0.0397(9) 0.0480(10) 0.0044(7) 0.0036(8) 0.0241(8) C51 0.0407(8) 0.0330(7) 0.0406(8) 0.0108(6) 0.0157(7) 0.0139(6) C53 0.0392(9) 0.0346(8) 0.0686(12) 0.0272(8) 0.0156(8) 0.0111(7) C52 0.0401(8) 0.0276(7) 0.0604(10) 0.0172(7) 0.0235(8) 0.0108(6) C56 0.0721(13) 0.0684(12) 0.0410(9) 0.0164(9) 0.0206(9) 0.0462(11) C54 0.0595(12) 0.0467(10) 0.0496(10) 0.0234(8) 0.0055(9) 0.0142(9) C55 0.0901(16) 0.0721(14) 0.0407(10) 0.0161(9) 0.0231(10) 0.0455(13) C61 0.0424(9) 0.0347(8) 0.0436(9) 0.0040(7) 0.0185(7) 0.0095(7) C66 0.0527(11) 0.0507(10) 0.0500(11) 0.0080(8) 0.0121(9) 0.0083(9) C63 0.0608(14) 0.0694(14) 0.0816(16) 0.0069(12) 0.0391(13) -0.0025(11) C62 0.0560(12) 0.0600(12) 0.0574(12) 0.0158(9) 0.0260(10) 0.0074(9) C65 0.0531(12) 0.0621(13) 0.0651(13) -0.0067(11) 0.0003(10) 0.0122(10) C64 0.0433(11) 0.0633(13) 0.0856(17) -0.0167(12) 0.0230(11) 0.0021(10) C72 0.0357(8) 0.0411(8) 0.0432(8) 0.0213(7) 0.0206(7) 0.0213(7) C71 0.0376(8) 0.0426(8) 0.0528(9) 0.0248(7) 0.0254(7) 0.0241(7) C73 0.0468(9) 0.0464(9) 0.0461(9) 0.0204(7) 0.0241(8) 0.0208(8) C76 0.0411(9) 0.0402(9) 0.0711(12) 0.0221(8) 0.0274(9) 0.0209(7) C74 0.0556(11) 0.0597(11) 0.0465(10) 0.0135(8) 0.0228(9) 0.0268(9) C75 0.0467(10) 0.0470(10) 0.0644(12) 0.0060(9) 0.0188(9) 0.0228(8) C81 0.0413(8) 0.0492(9) 0.0333(7) 0.0203(7) 0.0182(7) 0.0217(7) C85 0.0440(10) 0.0576(11) 0.0595(11) 0.0180(9) 0.0189(8) 0.0274(9) C84 0.0588(11) 0.0581(11) 0.0421(9) 0.0192(8) 0.0241(8) 0.0332(9) C82 0.0427(9) 0.0666(12) 0.0390(9) 0.0070(8) 0.0139(7) 0.0184(9) C86 0.0398(9) 0.0434(9) 0.0492(9) 0.0131(7) 0.0144(7) 0.0180(7) C83 0.0626(12) 0.0580(11) 0.0384(9) 0.0052(8) 0.0192(8) 0.0240(9) C91 0.0349(8) 0.0377(8) 0.0396(8) 0.0138(6) 0.0156(6) 0.0146(6) C92 0.0413(9) 0.0443(9) 0.0477(9) 0.0198(7) 0.0211(7) 0.0216(7) C96 0.0365(8) 0.0419(9) 0.0542(10) 0.0136(7) 0.0177(7) 0.0180(7) C93 0.0562(10) 0.0377(8) 0.0484(9) 0.0183(7) 0.0230(8) 0.0181(8) C95 0.0383(9) 0.0461(10) 0.0678(12) 0.0117(8) 0.0280(9) 0.0132(7) C94 0.0525(10) 0.0396(9) 0.0577(11) 0.0140(8) 0.0319(9) 0.0079(8) _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 P1 C21 1.8247(17) . ? P1 C31 1.8379(16) . ? P1 C12 1.8444(15) . ? P2 C61 1.8287(17) . ? P2 C51 1.8368(16) . ? P2 C42 1.8455(16) . ? P3 C81 1.8266(17) . ? P3 C91 1.8293(15) . ? P3 C72 1.8378(18) . ? N1 C7 1.4592(19) . ? N1 C1 1.4703(19) . ? N1 H1N 0.88(2) . ? N3 C8 1.468(2) . ? N3 C3 1.4750(19) . ? N3 H3N 0.95(2) . ? N2 C9 1.461(2) . ? N2 C5 1.4743(19) . ? N2 H2N 0.88(2) . ? C6 C5 1.521(2) . ? C6 C1 1.523(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C11 C16 1.395(2) . ? C11 C12 1.405(2) . ? C11 C7 1.508(2) . ? C12 C13 1.396(2) . ? C3 C4 1.524(2) . ? C3 C2 1.529(2) . ? C3 H3 0.9800 . ? C5 C4 1.527(2) . ? C5 H5 0.9800 . ? C2 C1 1.521(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1 0.9800 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C14 C15 1.376(2) . ? C14 C13 1.386(2) . ? C14 H14 0.9300 . ? C16 C15 1.384(2) . ? C16 H16 0.9300 . ? C8 C71 1.512(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C9 C41 1.515(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C22 C23 1.386(2) . ? C22 C21 1.396(2) . ? C22 H22 0.9300 . ? C21 C26 1.394(2) . ? C26 C25 1.378(3) . ? C26 H26 0.9300 . ? C23 C24 1.377(3) . ? C23 H23 0.9300 . ? C24 C25 1.377(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C36 1.382(2) . ? C31 C32 1.396(2) . ? C34 C33 1.378(3) . ? C34 C35 1.384(2) . ? C34 H34 0.9300 . ? C36 C35 1.390(2) . ? C36 H36 0.9300 . ? C35 H35 0.9300 . ? C32 C33 1.379(2) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C42 C43 1.394(2) . ? C42 C41 1.407(2) . ? C41 C46 1.388(2) . ? C43 C44 1.388(3) . ? C43 H43 0.9300 . ? C46 C45 1.382(3) . ? C46 H46 0.9300 . ? C44 C45 1.371(3) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C51 C52 1.389(2) . ? C51 C56 1.390(2) . ? C53 C54 1.368(3) . ? C53 C52 1.384(3) . ? C53 H53 0.9300 . ? C52 H52 0.9300 . ? C56 C55 1.387(3) . ? C56 H56 0.9300 . ? C54 C55 1.377(3) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C61 C62 1.387(3) . ? C61 C66 1.393(3) . ? C66 C65 1.380(3) . ? C66 H66 0.9300 . ? C63 C64 1.363(4) . ? C63 C62 1.381(3) . ? C63 H63 0.9300 . ? C62 H62 0.9300 . ? C65 C64 1.387(3) . ? C65 H65 0.9300 . ? C64 H64 0.9300 . ? C72 C73 1.403(2) . ? C72 C71 1.409(2) . ? C71 C76 1.390(3) . ? C73 C74 1.380(3) . ? C73 H73 0.9300 . ? C76 C75 1.377(3) . ? C76 H76 0.9300 . ? C74 C75 1.382(3) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C81 C86 1.386(2) . ? C81 C82 1.395(3) . ? C85 C84 1.375(3) . ? C85 C86 1.397(2) . ? C85 H85 0.9300 . ? C84 C83 1.377(3) . ? C84 H84 0.9300 . ? C82 C83 1.379(3) . ? C82 H82 0.9300 . ? C86 H86 0.9300 . ? C83 H83 0.9300 . ? C91 C96 1.387(2) . ? C91 C92 1.399(2) . ? C92 C93 1.383(2) . ? C92 H92 0.9300 . ? C96 C95 1.384(2) . ? C96 H96 0.9300 . ? C93 C94 1.383(3) . ? C93 H93 0.9300 . ? C95 C94 1.374(3) . ? C95 H95 0.9300 . ? C94 H94 0.9300 . ? 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 P1 C31 101.97(7) . . ? C21 P1 C12 102.10(7) . . ? C31 P1 C12 103.56(7) . . ? C61 P2 C51 103.74(8) . . ? C61 P2 C42 103.37(7) . . ? C51 P2 C42 99.50(7) . . ? C81 P3 C91 100.55(7) . . ? C81 P3 C72 104.22(7) . . ? C91 P3 C72 102.40(7) . . ? C7 N1 C1 112.14(12) . . ? C7 N1 H1N 107.6(13) . . ? C1 N1 H1N 107.4(14) . . ? C8 N3 C3 112.58(12) . . ? C8 N3 H3N 108.2(12) . . ? C3 N3 H3N 107.5(12) . . ? C9 N2 C5 114.86(13) . . ? C9 N2 H2N 109.2(14) . . ? C5 N2 H2N 109.3(14) . . ? C5 C6 C1 112.81(12) . . ? C5 C6 H6A 109.0 . . ? C1 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C1 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C16 C11 C12 118.99(13) . . ? C16 C11 C7 119.18(14) . . ? C12 C11 C7 121.80(13) . . ? C13 C12 C11 118.71(13) . . ? C13 C12 P1 122.23(12) . . ? C11 C12 P1 118.88(11) . . ? N3 C3 C4 110.24(12) . . ? N3 C3 C2 109.50(13) . . ? C4 C3 C2 109.61(12) . . ? N3 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C2 C3 H3 109.2 . . ? N2 C5 C6 107.94(12) . . ? N2 C5 C4 111.27(13) . . ? C6 C5 C4 109.84(13) . . ? N2 C5 H5 109.3 . . ? C6 C5 H5 109.3 . . ? C4 C5 H5 109.3 . . ? C1 C2 C3 111.28(13) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N1 C1 C2 109.29(12) . . ? N1 C1 C6 109.81(12) . . ? C2 C1 C6 110.38(12) . . ? N1 C1 H1 109.1 . . ? C2 C1 H1 109.1 . . ? C6 C1 H1 109.1 . . ? C3 C4 C5 111.30(12) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C7 C11 113.23(13) . . ? N1 C7 H7A 108.9 . . ? C11 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C11 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C15 C14 C13 120.03(15) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C16 C11 121.49(15) . . ? C15 C16 H16 119.3 . . ? C11 C16 H16 119.3 . . ? N3 C8 C71 110.76(13) . . ? N3 C8 H8A 109.5 . . ? C71 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C71 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C14 C13 C12 121.26(15) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C14 C15 C16 119.51(14) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N2 C9 C41 113.39(14) . . ? N2 C9 H9A 108.9 . . ? C41 C9 H9A 108.9 . . ? N2 C9 H9B 108.9 . . ? C41 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C23 C22 C21 120.38(16) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C26 C21 C22 118.27(16) . . ? C26 C21 P1 116.25(13) . . ? C22 C21 P1 125.47(13) . . ? C25 C26 C21 120.96(18) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C24 C23 C22 120.22(17) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.11(18) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.05(19) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C36 C31 C32 118.15(15) . . ? C36 C31 P1 125.70(11) . . ? C32 C31 P1 116.07(12) . . ? C33 C34 C35 119.56(16) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C31 C36 C35 120.93(15) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C34 C35 C36 120.05(17) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C33 C32 C31 121.04(16) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 120.25(16) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C43 C42 C41 118.62(14) . . ? C43 C42 P2 123.26(12) . . ? C41 C42 P2 118.09(12) . . ? C46 C41 C42 119.11(15) . . ? C46 C41 C9 120.59(14) . . ? C42 C41 C9 120.29(14) . . ? C44 C43 C42 121.25(16) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C46 C41 121.27(16) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? C45 C44 C43 119.70(17) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.03(16) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C52 C51 C56 118.23(16) . . ? C52 C51 P2 118.61(13) . . ? C56 C51 P2 122.89(13) . . ? C54 C53 C52 119.89(17) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C52 C51 121.24(17) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C55 C56 C51 120.13(18) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? C53 C54 C55 119.90(18) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 120.59(19) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C62 C61 C66 117.80(17) . . ? C62 C61 P2 124.59(15) . . ? C66 C61 P2 117.40(13) . . ? C65 C66 C61 121.47(19) . . ? C65 C66 H66 119.3 . . ? C61 C66 H66 119.3 . . ? C64 C63 C62 121.3(2) . . ? C64 C63 H63 119.4 . . ? C62 C63 H63 119.4 . . ? C63 C62 C61 120.4(2) . . ? C63 C62 H62 119.8 . . ? C61 C62 H62 119.8 . . ? C66 C65 C64 119.6(2) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C63 C64 C65 119.4(2) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C73 C72 C71 117.98(16) . . ? C73 C72 P3 121.93(12) . . ? C71 C72 P3 119.79(12) . . ? C76 C71 C72 119.09(16) . . ? C76 C71 C8 118.37(15) . . ? C72 C71 C8 122.52(16) . . ? C74 C73 C72 121.66(16) . . ? C74 C73 H73 119.2 . . ? C72 C73 H73 119.2 . . ? C75 C76 C71 122.07(16) . . ? C75 C76 H76 119.0 . . ? C71 C76 H76 119.0 . . ? C73 C74 C75 120.02(18) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 119.15(18) . . ? C76 C75 H75 120.4 . . ? C74 C75 H75 120.4 . . ? C86 C81 C82 118.21(16) . . ? C86 C81 P3 125.23(14) . . ? C82 C81 P3 116.54(13) . . ? C84 C85 C86 120.18(18) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C84 C83 119.71(17) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C83 C82 C81 120.94(17) . . ? C83 C82 H82 119.5 . . ? C81 C82 H82 119.5 . . ? C81 C86 C85 120.56(17) . . ? C81 C86 H86 119.7 . . ? C85 C86 H86 119.7 . . ? C84 C83 C82 120.37(18) . . ? C84 C83 H83 119.8 . . ? C82 C83 H83 119.8 . . ? C96 C91 C92 118.44(14) . . ? C96 C91 P3 117.43(12) . . ? C92 C91 P3 124.13(12) . . ? C93 C92 C91 120.40(15) . . ? C93 C92 H92 119.8 . . ? C91 C92 H92 119.8 . . ? C95 C96 C91 120.95(16) . . ? C95 C96 H96 119.5 . . ? C91 C96 H96 119.5 . . ? C94 C93 C92 120.10(16) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C94 C95 C96 120.02(16) . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C95 C94 C93 120.07(15) . . ? C95 C94 H94 120.0 . . ? C93 C94 H94 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 C11 C12 C13 0.2(2) . . . . ? C7 C11 C12 C13 -177.82(15) . . . . ? C16 C11 C12 P1 175.39(12) . . . . ? C7 C11 C12 P1 -2.6(2) . . . . ? C21 P1 C12 C13 13.78(15) . . . . ? C31 P1 C12 C13 -91.88(14) . . . . ? C21 P1 C12 C11 -161.22(12) . . . . ? C31 P1 C12 C11 93.12(13) . . . . ? C8 N3 C3 C4 -153.10(14) . . . . ? C8 N3 C3 C2 86.23(17) . . . . ? C9 N2 C5 C6 -168.73(15) . . . . ? C9 N2 C5 C4 70.68(19) . . . . ? C1 C6 C5 N2 -176.33(13) . . . . ? C1 C6 C5 C4 -54.84(17) . . . . ? N3 C3 C2 C1 178.96(12) . . . . ? C4 C3 C2 C1 57.91(17) . . . . ? C7 N1 C1 C2 -161.76(13) . . . . ? C7 N1 C1 C6 77.03(17) . . . . ? C3 C2 C1 N1 -176.62(13) . . . . ? C3 C2 C1 C6 -55.75(17) . . . . ? C5 C6 C1 N1 175.23(13) . . . . ? C5 C6 C1 C2 54.67(18) . . . . ? N3 C3 C4 C5 -179.01(13) . . . . ? C2 C3 C4 C5 -58.41(17) . . . . ? N2 C5 C4 C3 176.08(13) . . . . ? C6 C5 C4 C3 56.62(17) . . . . ? C1 N1 C7 C11 168.15(13) . . . . ? C16 C11 C7 N1 108.20(16) . . . . ? C12 C11 C7 N1 -73.8(2) . . . . ? C12 C11 C16 C15 -1.0(2) . . . . ? C7 C11 C16 C15 177.10(15) . . . . ? C3 N3 C8 C71 -165.56(14) . . . . ? C15 C14 C13 C12 -0.2(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? P1 C12 C13 C14 -174.64(14) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C11 C16 C15 C14 1.2(3) . . . . ? C5 N2 C9 C41 -154.00(15) . . . . ? C23 C22 C21 C26 -1.2(2) . . . . ? C23 C22 C21 P1 177.52(13) . . . . ? C31 P1 C21 C26 -152.01(14) . . . . ? C12 P1 C21 C26 101.09(14) . . . . ? C31 P1 C21 C22 29.28(15) . . . . ? C12 P1 C21 C22 -77.62(15) . . . . ? C22 C21 C26 C25 1.5(3) . . . . ? P1 C21 C26 C25 -177.33(17) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C22 C23 C24 C25 0.6(3) . . . . ? C23 C24 C25 C26 -0.3(3) . . . . ? C21 C26 C25 C24 -0.8(3) . . . . ? C21 P1 C31 C36 -95.95(15) . . . . ? C12 P1 C31 C36 9.81(16) . . . . ? C21 P1 C31 C32 87.48(14) . . . . ? C12 P1 C31 C32 -166.76(13) . . . . ? C32 C31 C36 C35 0.3(2) . . . . ? P1 C31 C36 C35 -176.18(13) . . . . ? C33 C34 C35 C36 -0.9(3) . . . . ? C31 C36 C35 C34 0.2(3) . . . . ? C36 C31 C32 C33 -0.1(3) . . . . ? P1 C31 C32 C33 176.78(14) . . . . ? C35 C34 C33 C32 1.2(3) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? C61 P2 C42 C43 -0.54(15) . . . . ? C51 P2 C42 C43 106.16(14) . . . . ? C61 P2 C42 C41 177.59(12) . . . . ? C51 P2 C42 C41 -75.71(13) . . . . ? C43 C42 C41 C46 1.5(2) . . . . ? P2 C42 C41 C46 -176.68(13) . . . . ? C43 C42 C41 C9 -177.65(15) . . . . ? P2 C42 C41 C9 4.1(2) . . . . ? N2 C9 C41 C46 -12.6(2) . . . . ? N2 C9 C41 C42 166.53(15) . . . . ? C41 C42 C43 C44 -1.2(2) . . . . ? P2 C42 C43 C44 176.93(13) . . . . ? C42 C41 C46 C45 -0.6(3) . . . . ? C9 C41 C46 C45 178.56(17) . . . . ? C42 C43 C44 C45 -0.1(3) . . . . ? C43 C44 C45 C46 1.1(3) . . . . ? C41 C46 C45 C44 -0.7(3) . . . . ? C61 P2 C51 C52 -119.49(13) . . . . ? C42 P2 C51 C52 134.11(13) . . . . ? C61 P2 C51 C56 66.54(17) . . . . ? C42 P2 C51 C56 -39.87(17) . . . . ? C54 C53 C52 C51 -1.5(2) . . . . ? C56 C51 C52 C53 1.8(2) . . . . ? P2 C51 C52 C53 -172.48(12) . . . . ? C52 C51 C56 C55 -0.5(3) . . . . ? P2 C51 C56 C55 173.48(17) . . . . ? C52 C53 C54 C55 -0.1(3) . . . . ? C53 C54 C55 C56 1.4(3) . . . . ? C51 C56 C55 C54 -1.1(3) . . . . ? C51 P2 C61 C62 11.54(18) . . . . ? C42 P2 C61 C62 115.00(17) . . . . ? C51 P2 C61 C66 -173.82(14) . . . . ? C42 P2 C61 C66 -70.35(15) . . . . ? C62 C61 C66 C65 -1.9(3) . . . . ? P2 C61 C66 C65 -176.87(17) . . . . ? C64 C63 C62 C61 1.6(4) . . . . ? C66 C61 C62 C63 0.3(3) . . . . ? P2 C61 C62 C63 174.88(18) . . . . ? C61 C66 C65 C64 1.6(3) . . . . ? C62 C63 C64 C65 -1.8(4) . . . . ? C66 C65 C64 C63 0.3(4) . . . . ? C81 P3 C72 C73 100.70(13) . . . . ? C91 P3 C72 C73 -3.73(14) . . . . ? C81 P3 C72 C71 -85.77(13) . . . . ? C91 P3 C72 C71 169.80(12) . . . . ? C73 C72 C71 C76 1.3(2) . . . . ? P3 C72 C71 C76 -172.46(12) . . . . ? C73 C72 C71 C8 -179.96(14) . . . . ? P3 C72 C71 C8 6.3(2) . . . . ? N3 C8 C71 C76 70.09(19) . . . . ? N3 C8 C71 C72 -108.63(17) . . . . ? C71 C72 C73 C74 -1.6(2) . . . . ? P3 C72 C73 C74 172.02(13) . . . . ? C72 C71 C76 C75 0.2(2) . . . . ? C8 C71 C76 C75 -178.54(15) . . . . ? C72 C73 C74 C75 0.3(3) . . . . ? C71 C76 C75 C74 -1.5(3) . . . . ? C73 C74 C75 C76 1.3(3) . . . . ? C91 P3 C81 C86 113.50(14) . . . . ? C72 P3 C81 C86 7.68(15) . . . . ? C91 P3 C81 C82 -68.50(14) . . . . ? C72 P3 C81 C82 -174.32(12) . . . . ? C86 C85 C84 C83 -0.6(3) . . . . ? C86 C81 C82 C83 -0.9(3) . . . . ? P3 C81 C82 C83 -179.06(14) . . . . ? C82 C81 C86 C85 -0.6(2) . . . . ? P3 C81 C86 C85 177.39(13) . . . . ? C84 C85 C86 C81 1.3(3) . . . . ? C85 C84 C83 C82 -0.9(3) . . . . ? C81 C82 C83 C84 1.7(3) . . . . ? C81 P3 C91 C96 154.72(14) . . . . ? C72 P3 C91 C96 -98.02(14) . . . . ? C81 P3 C91 C92 -24.97(16) . . . . ? C72 P3 C91 C92 82.29(15) . . . . ? C96 C91 C92 C93 1.1(3) . . . . ? P3 C91 C92 C93 -179.24(14) . . . . ? C92 C91 C96 C95 -1.1(3) . . . . ? P3 C91 C96 C95 179.23(14) . . . . ? C91 C92 C93 C94 -0.4(3) . . . . ? C91 C96 C95 C94 0.4(3) . . . . ? C96 C95 C94 C93 0.3(3) . . . . ? C92 C93 C94 C95 -0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.540 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.050 # Attachment '6.cif' data_mht014d_0m _database_code_depnum_ccdc_archive 'CCDC 718423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H54 I6 N3 P3 Pt3' _chemical_formula_weight 2292.67 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' I I -0.4742 1.8119 '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_ # _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 0.674 0.000 0.500 881.2 102.5 # 2 0.712 0.500 0.000 881.2 105.1 #_platon_squeeze_details ? 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 17.9294(17) _cell_length_b 15.1394(15) _cell_length_c 28.744(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.2310(10) _cell_angle_gamma 90.00 _cell_volume 7789.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7535 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.70 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4200 _exptl_absorpt_coefficient_mu 7.848 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4041 _exptl_absorpt_correction_T_max 0.9618 _exptl_absorpt_process_details 'XPREP (Bruker, 2005a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker Smart APEX II CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94515 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.19 _reflns_number_total 18753 _reflns_number_gt 13836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2005b)' _computing_cell_refinement 'APEX 2 (Bruker, 2005b)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0492P)^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 18753 _refine_ls_number_parameters 712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 0.278414(12) 0.699736(14) 0.209354(7) 0.02910(6) Uani 1 1 d . . . Pt2 Pt 0.242193(13) 0.692635(15) 0.462343(8) 0.03502(6) Uani 1 1 d . . . Pt3 Pt -0.065463(13) 0.571391(16) 0.272662(10) 0.04488(8) Uani 1 1 d . . . I2 I 0.23822(3) 0.82325(3) 0.151044(15) 0.04796(11) Uani 1 1 d . . . I1 I 0.28936(2) 0.81442(2) 0.280035(14) 0.04011(10) Uani 1 1 d . . . I5 I 0.01114(3) 0.68415(3) 0.222708(16) 0.05453(12) Uani 1 1 d . A . I4 I 0.10438(3) 0.75399(4) 0.441402(17) 0.06121(14) Uani 1 1 d . . . I3 I 0.26913(4) 0.83154(4) 0.51205(2) 0.07503(17) Uani 1 1 d . . . P1 P 0.29821(9) 0.60551(10) 0.15228(5) 0.0348(3) Uani 1 1 d . . . P2 P 0.35091(8) 0.62725(10) 0.48105(5) 0.0344(3) Uani 1 1 d . . . P3 P -0.12864(8) 0.46942(11) 0.30903(6) 0.0429(4) Uani 1 1 d . A . N2 N 0.2181(2) 0.5824(3) 0.42226(15) 0.0276(10) Uani 1 1 d . A . N3 N 0.0293(2) 0.5014(3) 0.29353(14) 0.0252(9) Uani 1 1 d . A . N1 N 0.2816(2) 0.5966(3) 0.25570(15) 0.0276(10) Uani 1 1 d . . . C1 C 0.2222(3) 0.6023(3) 0.29061(17) 0.0262(11) Uani 1 1 d . . . H1 H 0.2021 0.6625 0.2891 0.031 Uiso 1 1 calc R . . C2 C 0.1590(3) 0.5402(3) 0.27579(18) 0.0271(11) Uani 1 1 d . A . H2A H 0.1759 0.4794 0.2777 0.033 Uiso 1 1 calc R . . H2B H 0.1414 0.5524 0.2439 0.033 Uiso 1 1 calc R . . C3 C 0.0960(3) 0.5558(3) 0.30907(17) 0.0256(11) Uani 1 1 d . . . H3 H 0.0817 0.6182 0.3072 0.031 Uiso 1 1 calc R A . C4 C 0.1219(3) 0.5353(4) 0.35952(17) 0.0291(12) Uani 1 1 d . A . H4A H 0.1370 0.4740 0.3625 0.035 Uiso 1 1 calc R . . H4B H 0.0816 0.5458 0.3800 0.035 Uiso 1 1 calc R . . C7 C 0.3178(3) 0.5243(4) 0.25425(18) 0.0282(11) Uani 1 1 d . . . H7 H 0.3099 0.4841 0.2780 0.034 Uiso 1 1 calc R . . C52 C 0.4037(3) 0.6078(4) 0.4295(2) 0.0359(13) Uani 1 1 d . . . C57 C 0.4192(3) 0.5240(4) 0.4135(2) 0.0405(14) Uani 1 1 d . . . H57 H 0.4063 0.4750 0.4308 0.049 Uiso 1 1 calc R . . C18 C 0.3701(3) 0.4967(4) 0.2200(2) 0.0359(13) Uani 1 1 d . . . C9 C 0.0376(3) 0.4181(4) 0.29403(19) 0.0326(12) Uani 1 1 d . . . H9 H 0.0859 0.3981 0.3013 0.039 Uiso 1 1 calc R A . C6 C 0.2522(3) 0.5865(4) 0.34040(18) 0.0295(12) Uani 1 1 d . A . H6A H 0.2913 0.6289 0.3488 0.035 Uiso 1 1 calc R . . H6B H 0.2733 0.5276 0.3433 0.035 Uiso 1 1 calc R . . C5 C 0.1882(3) 0.5964(4) 0.37256(17) 0.0282(11) Uani 1 1 d . . . H5 H 0.1702 0.6575 0.3699 0.034 Uiso 1 1 calc R A . C19 C 0.4178(3) 0.4276(4) 0.2324(2) 0.0416(15) Uani 1 1 d . . . H19 H 0.4163 0.4031 0.2620 0.050 Uiso 1 1 calc R . . C56 C 0.4531(4) 0.5124(5) 0.3729(2) 0.0519(17) Uani 1 1 d . . . H56 H 0.4632 0.4557 0.3626 0.062 Uiso 1 1 calc R . . C53 C 0.4242(4) 0.6801(4) 0.4044(2) 0.0484(16) Uani 1 1 d . . . H53 H 0.4149 0.7367 0.4152 0.058 Uiso 1 1 calc R . . C45 C 0.3268(3) 0.5188(4) 0.50152(19) 0.0356(13) Uani 1 1 d . . . C70 C -0.0192(3) 0.3491(4) 0.2846(2) 0.0333(13) Uani 1 1 d . A . C75 C -0.0953(3) 0.3621(4) 0.2903(2) 0.0381(14) Uani 1 1 d . . . C8 C 0.2291(3) 0.5052(4) 0.43556(19) 0.0336(13) Uani 1 1 d . . . H8 H 0.2101 0.4616 0.4154 0.040 Uiso 1 1 calc R A . C28 C 0.2198(4) 0.5378(4) 0.1343(2) 0.0398(14) Uani 1 1 d . . . C29 C 0.2279(4) 0.4562(4) 0.1152(2) 0.0529(17) Uani 1 1 d . . . H29 H 0.2752 0.4353 0.1095 0.064 Uiso 1 1 calc R . . C21 C 0.4205(4) 0.4939(5) 0.1435(2) 0.0512(17) Uani 1 1 d . . . H21 H 0.4218 0.5158 0.1133 0.061 Uiso 1 1 calc R . . C22 C 0.3694(3) 0.5286(4) 0.1736(2) 0.0367(13) Uani 1 1 d . . . C13 C 0.4682(4) 0.3935(5) 0.2015(3) 0.0501(17) Uani 1 1 d . . . H13 H 0.5006 0.3481 0.2108 0.060 Uiso 1 1 calc R . . C71 C 0.0070(3) 0.2659(4) 0.2744(2) 0.0439(15) Uani 1 1 d . . . H71 H 0.0580 0.2575 0.2719 0.053 Uiso 1 1 calc R A . C46 C 0.4180(4) 0.6701(4) 0.5251(2) 0.0450(16) Uani 1 1 d . . . C44 C 0.3670(4) 0.4773(5) 0.5384(2) 0.0466(16) Uani 1 1 d . A . H44 H 0.4071 0.5065 0.5534 0.056 Uiso 1 1 calc R . . C51 C 0.4906(4) 0.6843(5) 0.5169(3) 0.0566(19) Uani 1 1 d . . . H51 H 0.5071 0.6754 0.4871 0.068 Uiso 1 1 calc R . . C40 C 0.2683(3) 0.4727(4) 0.47902(19) 0.0344(13) Uani 1 1 d . A . C41 C 0.2512(4) 0.3856(5) 0.4927(2) 0.0490(17) Uani 1 1 d . . . H41 H 0.2138 0.3536 0.4765 0.059 Uiso 1 1 calc R A . C54 C 0.4588(4) 0.6688(5) 0.3627(3) 0.061(2) Uani 1 1 d . . . H54 H 0.4724 0.7176 0.3455 0.073 Uiso 1 1 calc R . . C55 C 0.4727(4) 0.5846(5) 0.3471(2) 0.057(2) Uani 1 1 d . . . H55 H 0.4953 0.5765 0.3190 0.069 Uiso 1 1 calc R . . C43 C 0.3485(4) 0.3947(5) 0.5527(3) 0.060(2) Uani 1 1 d . . . H43 H 0.3754 0.3693 0.5779 0.072 Uiso 1 1 calc R A . C42 C 0.2912(4) 0.3486(5) 0.5308(3) 0.065(2) Uani 1 1 d . A . H42 H 0.2790 0.2926 0.5413 0.078 Uiso 1 1 calc R . . C47 C 0.3933(4) 0.6855(5) 0.5698(2) 0.0572(19) Uani 1 1 d . . . H47 H 0.3437 0.6747 0.5759 0.069 Uiso 1 1 calc R . . C50 C 0.5408(4) 0.7123(6) 0.5527(3) 0.072(2) Uani 1 1 d . . . H50 H 0.5909 0.7201 0.5470 0.086 Uiso 1 1 calc R . . C49 C 0.5171(5) 0.7281(6) 0.5954(3) 0.077(3) Uani 1 1 d . . . H49 H 0.5510 0.7469 0.6190 0.092 Uiso 1 1 calc R . . C48 C 0.4425(5) 0.7166(6) 0.6046(3) 0.073(2) Uani 1 1 d . . . H48 H 0.4259 0.7297 0.6339 0.088 Uiso 1 1 calc R . . C30 C 0.1653(5) 0.4043(5) 0.1044(3) 0.067(2) Uani 1 1 d . . . H30 H 0.1716 0.3483 0.0918 0.080 Uiso 1 1 calc R . . C27 C 0.3366(4) 0.6502(4) 0.1006(2) 0.0492(17) Uani 1 1 d . . . C33 C 0.1494(4) 0.5672(4) 0.1430(2) 0.0525(18) Uani 1 1 d . . . H33 H 0.1435 0.6226 0.1562 0.063 Uiso 1 1 calc R . . C23 C 0.3993(5) 0.7029(5) 0.1031(3) 0.068(2) Uani 1 1 d . . . H23 H 0.4210 0.7178 0.1322 0.082 Uiso 1 1 calc R . . C26 C 0.3028(5) 0.6317(5) 0.0564(2) 0.066(2) Uani 1 1 d . . . H26 H 0.2595 0.5978 0.0539 0.079 Uiso 1 1 calc R . . C20 C 0.4693(4) 0.4273(5) 0.1581(3) 0.0555(19) Uani 1 1 d . . . H20 H 0.5034 0.4056 0.1377 0.067 Uiso 1 1 calc R . . C32 C 0.0864(4) 0.5147(5) 0.1321(3) 0.069(2) Uani 1 1 d . . . H32 H 0.0389 0.5344 0.1385 0.083 Uiso 1 1 calc R . . C31 C 0.0961(5) 0.4331(5) 0.1116(3) 0.073(2) Uani 1 1 d . . . H31 H 0.0549 0.3983 0.1030 0.087 Uiso 1 1 calc R . . C72 C -0.0402(4) 0.1956(5) 0.2680(3) 0.0568(19) Uani 1 1 d . A . H72 H -0.0219 0.1401 0.2609 0.068 Uiso 1 1 calc R . . C82 C -0.1097(3) 0.4668(5) 0.3716(3) 0.0475(16) Uani 1 1 d . . . C77 C -0.2609(4) 0.4509(5) 0.2567(3) 0.0567(19) Uani 1 1 d . A . H77 H -0.2303 0.4458 0.2318 0.068 Uiso 1 1 calc R . . C76 C -0.2295(3) 0.4636(4) 0.3008(2) 0.0431(15) Uani 1 1 d . . . C74 C -0.1421(4) 0.2892(5) 0.2831(3) 0.064(2) Uani 1 1 d . A . H74 H -0.1932 0.2959 0.2859 0.077 Uiso 1 1 calc R . . C81 C -0.2749(4) 0.4748(5) 0.3366(3) 0.061(2) Uani 1 1 d . A . H81 H -0.2544 0.4863 0.3664 0.073 Uiso 1 1 calc R . . C83 C -0.1217(4) 0.3920(6) 0.3970(3) 0.065(2) Uani 1 1 d . A . H83 H -0.1367 0.3404 0.3816 0.078 Uiso 1 1 calc R . . C87 C -0.0844(4) 0.5439(6) 0.3934(3) 0.071(2) Uani 1 1 d . A . H87 H -0.0744 0.5946 0.3765 0.085 Uiso 1 1 calc R . . C73 C -0.1149(4) 0.2085(5) 0.2721(3) 0.064(2) Uani 1 1 d . . . H73 H -0.1476 0.1614 0.2673 0.076 Uiso 1 1 calc R A . C24 C 0.4300(6) 0.7335(7) 0.0643(4) 0.094(3) Uani 1 1 d . . . H24 H 0.4726 0.7686 0.0669 0.113 Uiso 1 1 calc R . . C16 C 0.3335(7) 0.6638(6) 0.0162(3) 0.098(4) Uani 1 1 d . . . H16 H 0.3108 0.6525 -0.0131 0.117 Uiso 1 1 calc R . . C25 C 0.3983(7) 0.7128(7) 0.0211(4) 0.095(4) Uani 1 1 d . . . H25 H 0.4210 0.7322 -0.0054 0.114 Uiso 1 1 calc R . . C79 C -0.3821(4) 0.4542(6) 0.2863(3) 0.068(2) Uani 1 1 d . A . H79 H -0.4337 0.4495 0.2819 0.082 Uiso 1 1 calc R . . C78 C -0.3378(4) 0.4456(5) 0.2488(3) 0.066(2) Uani 1 1 d . . . H78 H -0.3590 0.4365 0.2190 0.079 Uiso 1 1 calc R A . C84 C -0.1122(5) 0.3917(8) 0.4444(3) 0.088(3) Uani 1 1 d . . . H84 H -0.1214 0.3409 0.4613 0.106 Uiso 1 1 calc R A . C85 C -0.0888(5) 0.4675(8) 0.4668(3) 0.085(3) Uani 1 1 d . A . H85 H -0.0826 0.4683 0.4991 0.102 Uiso 1 1 calc R . . C80 C -0.3512(4) 0.4693(7) 0.3286(3) 0.081(3) Uani 1 1 d . . . H80 H -0.3817 0.4763 0.3535 0.097 Uiso 1 1 calc R A . C86 C -0.0746(5) 0.5416(8) 0.4421(4) 0.095(3) Uani 1 1 d . . . H86 H -0.0580 0.5921 0.4579 0.114 Uiso 1 1 calc R A . I6A I -0.18030(6) 0.68020(8) 0.27237(6) 0.0763(4) Uani 0.50 1 d P A 1 I6B I -0.17875(6) 0.65218(9) 0.23251(6) 0.0857(4) Uani 0.50 1 d P A 2 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 0.02930(12) 0.02761(11) 0.03034(12) 0.00191(8) 0.00129(9) -0.00588(8) Pt2 0.03725(13) 0.03757(13) 0.03007(12) -0.00648(9) 0.00046(9) 0.00430(10) Pt3 0.02245(12) 0.04001(14) 0.07068(19) 0.01551(12) -0.01066(11) 0.00267(10) I2 0.0686(3) 0.0333(2) 0.0408(2) 0.00600(17) -0.0071(2) -0.00109(19) I1 0.0495(2) 0.0309(2) 0.0401(2) -0.00295(16) 0.00362(18) -0.00759(17) I5 0.0664(3) 0.0501(3) 0.0465(3) 0.0204(2) -0.0017(2) 0.0053(2) I4 0.0536(3) 0.0747(3) 0.0550(3) -0.0048(2) 0.0001(2) 0.0317(3) I3 0.0916(4) 0.0588(3) 0.0729(4) -0.0343(3) -0.0103(3) 0.0117(3) P1 0.0402(9) 0.0334(8) 0.0314(8) 0.0015(6) 0.0062(7) -0.0031(6) P2 0.0317(8) 0.0411(8) 0.0298(8) -0.0068(6) -0.0043(6) -0.0016(6) P3 0.0182(7) 0.0448(9) 0.0653(12) 0.0048(8) 0.0007(7) 0.0012(6) N2 0.020(2) 0.034(3) 0.029(2) 0.0025(19) 0.0042(18) 0.0013(18) N3 0.021(2) 0.031(2) 0.023(2) 0.0020(18) -0.0011(17) 0.0005(18) N1 0.019(2) 0.034(2) 0.029(2) 0.0043(19) 0.0009(18) -0.0074(18) C1 0.024(3) 0.028(3) 0.026(3) 0.002(2) 0.000(2) -0.001(2) C2 0.021(3) 0.031(3) 0.029(3) 0.002(2) -0.003(2) -0.005(2) C3 0.018(2) 0.029(3) 0.028(3) 0.000(2) -0.006(2) 0.000(2) C4 0.026(3) 0.040(3) 0.022(3) 0.006(2) 0.003(2) -0.003(2) C7 0.026(3) 0.033(3) 0.025(3) 0.005(2) 0.000(2) -0.007(2) C52 0.026(3) 0.046(3) 0.035(3) -0.004(3) -0.004(2) 0.002(3) C57 0.038(3) 0.043(4) 0.040(4) 0.000(3) 0.005(3) 0.000(3) C18 0.030(3) 0.039(3) 0.039(3) -0.002(3) 0.001(2) -0.006(2) C9 0.018(3) 0.045(3) 0.034(3) 0.005(3) -0.001(2) -0.002(2) C6 0.023(3) 0.031(3) 0.034(3) 0.001(2) -0.003(2) -0.007(2) C5 0.027(3) 0.034(3) 0.024(3) -0.006(2) -0.002(2) 0.004(2) C19 0.033(3) 0.056(4) 0.035(3) 0.003(3) 0.002(3) 0.004(3) C56 0.047(4) 0.062(4) 0.047(4) -0.004(3) 0.006(3) 0.015(3) C53 0.054(4) 0.034(3) 0.057(4) 0.004(3) 0.004(3) -0.003(3) C45 0.035(3) 0.047(3) 0.025(3) -0.005(2) -0.001(2) 0.004(3) C70 0.026(3) 0.034(3) 0.040(3) 0.005(2) 0.002(2) -0.004(2) C75 0.028(3) 0.037(3) 0.049(4) 0.001(3) -0.003(3) -0.006(2) C8 0.026(3) 0.043(3) 0.031(3) -0.001(2) -0.003(2) -0.003(2) C28 0.050(4) 0.035(3) 0.034(3) 0.003(3) -0.002(3) -0.002(3) C29 0.063(5) 0.049(4) 0.047(4) -0.003(3) -0.001(3) -0.006(3) C21 0.051(4) 0.055(4) 0.049(4) -0.002(3) 0.018(3) 0.007(3) C22 0.034(3) 0.041(3) 0.036(3) 0.002(3) 0.007(3) -0.004(3) C13 0.035(4) 0.050(4) 0.067(5) -0.005(3) 0.007(3) 0.004(3) C71 0.030(3) 0.048(4) 0.053(4) -0.011(3) -0.001(3) 0.001(3) C46 0.042(4) 0.049(4) 0.042(4) -0.011(3) -0.012(3) -0.001(3) C44 0.042(4) 0.069(5) 0.028(3) 0.001(3) -0.007(3) -0.003(3) C51 0.049(4) 0.064(5) 0.055(4) -0.014(4) -0.006(3) -0.009(4) C40 0.030(3) 0.043(3) 0.029(3) 0.006(2) -0.004(2) -0.003(2) C41 0.048(4) 0.058(4) 0.040(4) 0.011(3) -0.011(3) 0.000(3) C54 0.058(5) 0.066(5) 0.061(5) 0.020(4) 0.017(4) -0.003(4) C55 0.045(4) 0.089(6) 0.039(4) 0.004(4) 0.010(3) 0.019(4) C43 0.060(5) 0.073(5) 0.047(4) 0.025(4) -0.012(4) -0.004(4) C42 0.073(5) 0.057(5) 0.064(5) 0.026(4) -0.009(4) -0.016(4) C47 0.048(4) 0.078(5) 0.043(4) -0.021(4) -0.012(3) 0.002(4) C50 0.045(4) 0.095(6) 0.074(6) -0.034(5) -0.014(4) -0.013(4) C49 0.066(6) 0.083(6) 0.079(6) -0.026(5) -0.027(5) -0.008(5) C48 0.072(6) 0.085(6) 0.061(5) -0.032(4) -0.020(4) 0.001(5) C30 0.077(6) 0.055(5) 0.069(5) -0.016(4) -0.001(4) -0.016(4) C27 0.060(4) 0.044(4) 0.045(4) 0.008(3) 0.018(3) 0.006(3) C33 0.056(4) 0.043(4) 0.056(4) -0.007(3) -0.016(3) -0.002(3) C23 0.068(5) 0.063(5) 0.074(6) 0.022(4) 0.019(4) -0.014(4) C26 0.100(7) 0.055(5) 0.044(4) 0.005(3) 0.020(4) 0.013(4) C20 0.045(4) 0.062(5) 0.062(5) -0.003(4) 0.023(4) 0.005(3) C32 0.045(4) 0.070(5) 0.091(6) -0.021(5) -0.018(4) -0.009(4) C31 0.063(5) 0.068(5) 0.086(6) -0.015(5) -0.011(5) -0.018(4) C72 0.045(4) 0.044(4) 0.081(5) -0.011(4) 0.006(4) -0.004(3) C82 0.019(3) 0.057(4) 0.066(5) 0.000(4) 0.001(3) 0.001(3) C77 0.038(4) 0.076(5) 0.057(5) 0.001(4) 0.006(3) 0.008(4) C76 0.019(3) 0.053(4) 0.057(4) 0.000(3) 0.002(3) 0.002(3) C74 0.028(4) 0.071(5) 0.092(6) 0.002(4) -0.002(4) -0.016(3) C81 0.036(4) 0.079(5) 0.067(5) -0.013(4) 0.002(3) 0.005(4) C83 0.056(5) 0.083(6) 0.055(5) 0.006(4) 0.005(4) -0.005(4) C87 0.053(5) 0.079(6) 0.080(6) -0.001(5) -0.009(4) -0.004(4) C73 0.044(4) 0.044(4) 0.102(7) -0.006(4) -0.009(4) -0.014(3) C24 0.085(7) 0.093(7) 0.109(9) 0.033(7) 0.051(7) 0.008(6) C16 0.165(11) 0.072(6) 0.061(6) 0.022(5) 0.051(7) 0.026(7) C25 0.119(9) 0.080(7) 0.091(8) 0.046(6) 0.063(7) 0.031(6) C79 0.021(3) 0.098(6) 0.085(6) -0.017(5) 0.001(4) -0.007(4) C78 0.033(4) 0.091(6) 0.073(5) -0.017(4) -0.012(4) 0.003(4) C84 0.071(6) 0.120(9) 0.075(7) 0.000(6) 0.014(5) 0.012(6) C85 0.049(5) 0.138(10) 0.068(6) -0.003(7) 0.003(4) -0.004(6) C80 0.028(4) 0.129(8) 0.086(6) -0.028(6) 0.019(4) 0.005(4) C86 0.073(7) 0.112(9) 0.097(8) -0.032(7) -0.009(6) -0.007(6) I6A 0.0419(6) 0.0615(7) 0.1240(11) 0.0145(7) -0.0084(7) 0.0247(5) I6B 0.0366(6) 0.0863(9) 0.1323(12) 0.0459(9) -0.0106(7) 0.0211(6) _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 N1 2.051(4) . ? Pt1 P1 2.2176(15) . ? Pt1 I2 2.5863(5) . ? Pt1 I1 2.6713(5) . ? Pt2 N2 2.060(4) . ? Pt2 P2 2.2249(16) . ? Pt2 I3 2.5729(5) . ? Pt2 I4 2.6763(6) . ? Pt3 N3 2.063(4) . ? Pt3 P3 2.2121(17) . ? Pt3 I6B 2.5864(10) . ? Pt3 I6A 2.6366(10) . ? Pt3 I5 2.6616(5) . ? P1 C28 1.793(6) . ? P1 C27 1.805(6) . ? P1 C22 1.809(6) . ? P2 C45 1.805(6) . ? P2 C46 1.817(6) . ? P2 C52 1.826(6) . ? P3 C82 1.811(7) . ? P3 C76 1.813(6) . ? P3 C75 1.823(6) . ? N2 C8 1.242(7) . ? N2 C5 1.512(7) . ? N3 C9 1.269(7) . ? N3 C3 1.499(6) . ? N1 C7 1.275(7) . ? N1 C1 1.507(6) . ? C1 C2 1.515(7) . ? C1 C6 1.520(7) . ? C1 H1 0.9800 . ? C2 C3 1.539(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.529(7) . ? C3 H3 0.9800 . ? C4 C5 1.537(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C7 C18 1.457(8) . ? C7 H7 0.9300 . ? C52 C53 1.373(8) . ? C52 C57 1.383(8) . ? C57 C56 1.357(8) . ? C57 H57 0.9300 . ? C18 C19 1.386(8) . ? C18 C22 1.419(8) . ? C9 C70 1.473(7) . ? C9 H9 0.9300 . ? C6 C5 1.521(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 H5 0.9800 . ? C19 C13 1.401(9) . ? C19 H19 0.9300 . ? C56 C55 1.379(10) . ? C56 H56 0.9300 . ? C53 C54 1.390(10) . ? C53 H53 0.9300 . ? C45 C40 1.388(8) . ? C45 C44 1.397(8) . ? C70 C71 1.382(8) . ? C70 C75 1.398(8) . ? C75 C74 1.394(9) . ? C8 C40 1.482(7) . ? C8 H8 0.9300 . ? C28 C29 1.361(9) . ? C28 C33 1.374(9) . ? C29 C30 1.391(10) . ? C29 H29 0.9300 . ? C21 C20 1.385(9) . ? C21 C22 1.398(8) . ? C21 H21 0.9300 . ? C13 C20 1.348(10) . ? C13 H13 0.9300 . ? C71 C72 1.366(9) . ? C71 H71 0.9300 . ? C46 C51 1.353(9) . ? C46 C47 1.400(9) . ? C44 C43 1.363(9) . ? C44 H44 0.9300 . ? C51 C50 1.394(9) . ? C51 H51 0.9300 . ? C40 C41 1.415(9) . ? C41 C42 1.393(9) . ? C41 H41 0.9300 . ? C54 C55 1.378(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C43 C42 1.366(10) . ? C43 H43 0.9300 . ? C42 H42 0.9300 . ? C47 C48 1.379(9) . ? C47 H47 0.9300 . ? C50 C49 1.342(11) . ? C50 H50 0.9300 . ? C49 C48 1.391(12) . ? C49 H49 0.9300 . ? C48 H48 0.9300 . ? C30 C31 1.343(11) . ? C30 H30 0.9300 . ? C27 C23 1.377(10) . ? C27 C26 1.404(10) . ? C33 C32 1.402(9) . ? C33 H33 0.9300 . ? C23 C24 1.353(11) . ? C23 H23 0.9300 . ? C26 C16 1.394(11) . ? C26 H26 0.9300 . ? C20 H20 0.9300 . ? C32 C31 1.384(11) . ? C32 H32 0.9300 . ? C31 H31 0.9300 . ? C72 C73 1.364(10) . ? C72 H72 0.9300 . ? C82 C83 1.372(10) . ? C82 C87 1.390(10) . ? C77 C76 1.369(9) . ? C77 C78 1.387(9) . ? C77 H77 0.9300 . ? C76 C81 1.357(9) . ? C74 C73 1.359(10) . ? C74 H74 0.9300 . ? C81 C80 1.377(10) . ? C81 H81 0.9300 . ? C83 C84 1.364(12) . ? C83 H83 0.9300 . ? C87 C86 1.400(13) . ? C87 H87 0.9300 . ? C73 H73 0.9300 . ? C24 C25 1.374(14) . ? C24 H24 0.9300 . ? C16 C25 1.380(15) . ? C16 H16 0.9300 . ? C25 H25 0.9300 . ? C79 C80 1.328(11) . ? C79 C78 1.380(11) . ? C79 H79 0.9300 . ? C78 H78 0.9300 . ? C84 C85 1.369(13) . ? C84 H84 0.9300 . ? C85 C86 1.360(13) . ? C85 H85 0.9300 . ? C80 H80 0.9300 . ? C86 H86 0.9300 . ? 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 N1 Pt1 P1 89.48(13) . . ? N1 Pt1 I2 165.43(11) . . ? P1 Pt1 I2 92.07(4) . . ? N1 Pt1 I1 90.16(12) . . ? P1 Pt1 I1 166.60(4) . . ? I2 Pt1 I1 91.649(16) . . ? N2 Pt2 P2 85.87(12) . . ? N2 Pt2 I3 178.66(12) . . ? P2 Pt2 I3 95.45(4) . . ? N2 Pt2 I4 89.63(12) . . ? P2 Pt2 I4 173.68(4) . . ? I3 Pt2 I4 89.040(19) . . ? N3 Pt3 P3 86.52(12) . . ? N3 Pt3 I6B 170.40(12) . . ? P3 Pt3 I6B 97.51(5) . . ? N3 Pt3 I6A 162.23(12) . . ? P3 Pt3 I6A 90.97(5) . . ? I6B Pt3 I6A 27.07(4) . . ? N3 Pt3 I5 92.57(12) . . ? P3 Pt3 I5 174.97(5) . . ? I6B Pt3 I5 82.65(3) . . ? I6A Pt3 I5 91.38(3) . . ? C28 P1 C27 107.8(3) . . ? C28 P1 C22 104.9(3) . . ? C27 P1 C22 103.0(3) . . ? C28 P1 Pt1 115.2(2) . . ? C27 P1 Pt1 116.9(2) . . ? C22 P1 Pt1 107.6(2) . . ? C45 P2 C46 105.0(3) . . ? C45 P2 C52 105.2(3) . . ? C46 P2 C52 105.7(3) . . ? C45 P2 Pt2 105.09(19) . . ? C46 P2 Pt2 123.1(2) . . ? C52 P2 Pt2 111.28(19) . . ? C82 P3 C76 105.0(3) . . ? C82 P3 C75 103.1(3) . . ? C76 P3 C75 105.0(3) . . ? C82 P3 Pt3 114.4(2) . . ? C76 P3 Pt3 120.4(2) . . ? C75 P3 Pt3 107.3(2) . . ? C8 N2 C5 117.7(5) . . ? C8 N2 Pt2 124.4(4) . . ? C5 N2 Pt2 117.8(3) . . ? C9 N3 C3 116.9(4) . . ? C9 N3 Pt3 127.4(4) . . ? C3 N3 Pt3 115.7(3) . . ? C7 N1 C1 116.8(4) . . ? C7 N1 Pt1 128.9(4) . . ? C1 N1 Pt1 113.2(3) . . ? N1 C1 C2 108.8(4) . . ? N1 C1 C6 113.1(4) . . ? C2 C1 C6 112.7(4) . . ? N1 C1 H1 107.3 . . ? C2 C1 H1 107.3 . . ? C6 C1 H1 107.3 . . ? C1 C2 C3 107.1(4) . . ? C1 C2 H2A 110.3 . . ? C3 C2 H2A 110.3 . . ? C1 C2 H2B 110.3 . . ? C3 C2 H2B 110.3 . . ? H2A C2 H2B 108.6 . . ? N3 C3 C4 111.4(4) . . ? N3 C3 C2 109.4(4) . . ? C4 C3 C2 111.4(4) . . ? N3 C3 H3 108.2 . . ? C4 C3 H3 108.2 . . ? C2 C3 H3 108.2 . . ? C3 C4 C5 107.4(4) . . ? C3 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? C3 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N1 C7 C18 128.0(5) . . ? N1 C7 H7 116.0 . . ? C18 C7 H7 116.0 . . ? C53 C52 C57 119.5(6) . . ? C53 C52 P2 117.7(5) . . ? C57 C52 P2 122.7(5) . . ? C56 C57 C52 120.9(6) . . ? C56 C57 H57 119.6 . . ? C52 C57 H57 119.6 . . ? C19 C18 C22 118.0(6) . . ? C19 C18 C7 117.0(5) . . ? C22 C18 C7 124.5(5) . . ? N3 C9 C70 128.6(5) . . ? N3 C9 H9 115.7 . . ? C70 C9 H9 115.7 . . ? C1 C6 C5 108.5(4) . . ? C1 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? C1 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N2 C5 C6 108.7(4) . . ? N2 C5 C4 112.0(4) . . ? C6 C5 C4 113.1(4) . . ? N2 C5 H5 107.6 . . ? C6 C5 H5 107.6 . . ? C4 C5 H5 107.6 . . ? C18 C19 C13 121.8(6) . . ? C18 C19 H19 119.1 . . ? C13 C19 H19 119.1 . . ? C57 C56 C55 120.0(7) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C52 C53 C54 120.0(6) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C40 C45 C44 118.1(6) . . ? C40 C45 P2 119.6(4) . . ? C44 C45 P2 122.2(5) . . ? C71 C70 C75 119.9(5) . . ? C71 C70 C9 116.5(5) . . ? C75 C70 C9 123.3(5) . . ? C74 C75 C70 117.0(6) . . ? C74 C75 P3 123.1(5) . . ? C70 C75 P3 119.9(4) . . ? N2 C8 C40 129.1(5) . . ? N2 C8 H8 115.4 . . ? C40 C8 H8 115.4 . . ? C29 C28 C33 119.1(6) . . ? C29 C28 P1 122.4(5) . . ? C33 C28 P1 118.4(5) . . ? C28 C29 C30 120.0(7) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C20 C21 C22 120.7(6) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C18 119.0(6) . . ? C21 C22 P1 120.4(5) . . ? C18 C22 P1 120.4(4) . . ? C20 C13 C19 119.4(6) . . ? C20 C13 H13 120.3 . . ? C19 C13 H13 120.3 . . ? C72 C71 C70 121.5(6) . . ? C72 C71 H71 119.2 . . ? C70 C71 H71 119.2 . . ? C51 C46 C47 119.5(6) . . ? C51 C46 P2 122.7(5) . . ? C47 C46 P2 117.8(5) . . ? C43 C44 C45 121.2(6) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C51 C50 120.3(7) . . ? C46 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C45 C40 C41 120.6(5) . . ? C45 C40 C8 122.4(5) . . ? C41 C40 C8 116.3(5) . . ? C42 C41 C40 118.9(6) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C55 C54 C53 119.5(7) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.1(6) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C44 C43 C42 121.2(6) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C42 C41 119.9(7) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C48 C47 C46 120.0(7) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C50 C51 120.4(8) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C49 C48 120.6(7) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C47 C48 C49 119.1(8) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C31 C30 C29 121.4(7) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C23 C27 C26 118.3(7) . . ? C23 C27 P1 121.4(6) . . ? C26 C27 P1 120.4(6) . . ? C28 C33 C32 120.9(7) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C24 C23 C27 121.5(9) . . ? C24 C23 H23 119.2 . . ? C27 C23 H23 119.2 . . ? C16 C26 C27 120.6(9) . . ? C16 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C13 C20 C21 121.0(6) . . ? C13 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C31 C32 C33 118.7(8) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C30 C31 C32 119.8(7) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C73 C72 C71 118.7(6) . . ? C73 C72 H72 120.6 . . ? C71 C72 H72 120.6 . . ? C83 C82 C87 120.7(7) . . ? C83 C82 P3 121.4(6) . . ? C87 C82 P3 117.9(6) . . ? C76 C77 C78 120.8(7) . . ? C76 C77 H77 119.6 . . ? C78 C77 H77 119.6 . . ? C81 C76 C77 119.1(6) . . ? C81 C76 P3 122.0(5) . . ? C77 C76 P3 118.9(5) . . ? C73 C74 C75 121.7(7) . . ? C73 C74 H74 119.1 . . ? C75 C74 H74 119.1 . . ? C76 C81 C80 120.0(7) . . ? C76 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C84 C83 C82 121.3(9) . . ? C84 C83 H83 119.3 . . ? C82 C83 H83 119.3 . . ? C82 C87 C86 116.6(9) . . ? C82 C87 H87 121.7 . . ? C86 C87 H87 121.7 . . ? C74 C73 C72 121.1(6) . . ? C74 C73 H73 119.5 . . ? C72 C73 H73 119.5 . . ? C23 C24 C25 120.1(10) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C25 C16 C26 118.2(10) . . ? C25 C16 H16 120.9 . . ? C26 C16 H16 120.9 . . ? C24 C25 C16 121.2(9) . . ? C24 C25 H25 119.4 . . ? C16 C25 H25 119.4 . . ? C80 C79 C78 120.1(7) . . ? C80 C79 H79 119.9 . . ? C78 C79 H79 119.9 . . ? C79 C78 C77 118.5(7) . . ? C79 C78 H78 120.7 . . ? C77 C78 H78 120.7 . . ? C83 C84 C85 119.0(10) . . ? C83 C84 H84 120.5 . . ? C85 C84 H84 120.5 . . ? C86 C85 C84 120.5(10) . . ? C86 C85 H85 119.8 . . ? C84 C85 H85 119.8 . . ? C79 C80 C81 121.4(7) . . ? C79 C80 H80 119.3 . . ? C81 C80 H80 119.3 . . ? C85 C86 C87 121.8(10) . . ? C85 C86 H86 119.1 . . ? C87 C86 H86 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 C28 73.9(2) . . . . ? I2 Pt1 P1 C28 -91.6(2) . . . . ? I1 Pt1 P1 C28 162.4(2) . . . . ? N1 Pt1 P1 C27 -158.0(3) . . . . ? I2 Pt1 P1 C27 36.5(3) . . . . ? I1 Pt1 P1 C27 -69.5(3) . . . . ? N1 Pt1 P1 C22 -42.7(2) . . . . ? I2 Pt1 P1 C22 151.8(2) . . . . ? I1 Pt1 P1 C22 45.8(3) . . . . ? N2 Pt2 P2 C45 -52.8(2) . . . . ? I3 Pt2 P2 C45 127.01(19) . . . . ? I4 Pt2 P2 C45 -8.1(5) . . . . ? N2 Pt2 P2 C46 -172.5(3) . . . . ? I3 Pt2 P2 C46 7.3(3) . . . . ? I4 Pt2 P2 C46 -127.8(4) . . . . ? N2 Pt2 P2 C52 60.6(2) . . . . ? I3 Pt2 P2 C52 -119.6(2) . . . . ? I4 Pt2 P2 C52 105.3(4) . . . . ? N3 Pt3 P3 C82 65.3(3) . . . . ? I6B Pt3 P3 C82 -123.5(2) . . . . ? I6A Pt3 P3 C82 -97.1(2) . . . . ? I5 Pt3 P3 C82 145.0(5) . . . . ? N3 Pt3 P3 C76 -168.3(3) . . . . ? I6B Pt3 P3 C76 3.0(3) . . . . ? I6A Pt3 P3 C76 29.4(3) . . . . ? I5 Pt3 P3 C76 -88.5(5) . . . . ? N3 Pt3 P3 C75 -48.4(2) . . . . ? I6B Pt3 P3 C75 122.8(2) . . . . ? I6A Pt3 P3 C75 149.2(2) . . . . ? I5 Pt3 P3 C75 31.3(6) . . . . ? P2 Pt2 N2 C8 45.7(4) . . . . ? I3 Pt2 N2 C8 -126(5) . . . . ? I4 Pt2 N2 C8 -129.8(4) . . . . ? P2 Pt2 N2 C5 -131.4(3) . . . . ? I3 Pt2 N2 C5 57(5) . . . . ? I4 Pt2 N2 C5 53.0(3) . . . . ? P3 Pt3 N3 C9 40.9(5) . . . . ? I6B Pt3 N3 C9 -74.3(9) . . . . ? I6A Pt3 N3 C9 123.2(5) . . . . ? I5 Pt3 N3 C9 -134.1(5) . . . . ? P3 Pt3 N3 C3 -140.1(3) . . . . ? I6B Pt3 N3 C3 104.6(7) . . . . ? I6A Pt3 N3 C3 -57.8(6) . . . . ? I5 Pt3 N3 C3 44.8(3) . . . . ? P1 Pt1 N1 C7 29.9(4) . . . . ? I2 Pt1 N1 C7 126.2(5) . . . . ? I1 Pt1 N1 C7 -136.7(4) . . . . ? P1 Pt1 N1 C1 -137.9(3) . . . . ? I2 Pt1 N1 C1 -41.7(7) . . . . ? I1 Pt1 N1 C1 55.5(3) . . . . ? C7 N1 C1 C2 -68.2(6) . . . . ? Pt1 N1 C1 C2 101.2(4) . . . . ? C7 N1 C1 C6 57.9(6) . . . . ? Pt1 N1 C1 C6 -132.7(4) . . . . ? N1 C1 C2 C3 -173.7(4) . . . . ? C6 C1 C2 C3 60.0(5) . . . . ? C9 N3 C3 C4 -60.7(6) . . . . ? Pt3 N3 C3 C4 120.2(4) . . . . ? C9 N3 C3 C2 62.8(6) . . . . ? Pt3 N3 C3 C2 -116.2(4) . . . . ? C1 C2 C3 N3 175.3(4) . . . . ? C1 C2 C3 C4 -61.1(5) . . . . ? N3 C3 C4 C5 -178.0(4) . . . . ? C2 C3 C4 C5 59.6(5) . . . . ? C1 N1 C7 C18 170.7(5) . . . . ? Pt1 N1 C7 C18 3.2(8) . . . . ? C45 P2 C52 C53 174.8(5) . . . . ? C46 P2 C52 C53 -74.4(5) . . . . ? Pt2 P2 C52 C53 61.5(5) . . . . ? C45 P2 C52 C57 -0.9(6) . . . . ? C46 P2 C52 C57 109.9(5) . . . . ? Pt2 P2 C52 C57 -114.2(5) . . . . ? C53 C52 C57 C56 -1.2(9) . . . . ? P2 C52 C57 C56 174.4(5) . . . . ? N1 C7 C18 C19 162.4(6) . . . . ? N1 C7 C18 C22 -25.2(9) . . . . ? C3 N3 C9 C70 174.2(5) . . . . ? Pt3 N3 C9 C70 -6.9(9) . . . . ? N1 C1 C6 C5 178.4(4) . . . . ? C2 C1 C6 C5 -57.6(6) . . . . ? C8 N2 C5 C6 -78.5(6) . . . . ? Pt2 N2 C5 C6 98.9(4) . . . . ? C8 N2 C5 C4 47.2(6) . . . . ? Pt2 N2 C5 C4 -135.5(4) . . . . ? C1 C6 C5 N2 -179.0(4) . . . . ? C1 C6 C5 C4 56.0(6) . . . . ? C3 C4 C5 N2 179.5(4) . . . . ? C3 C4 C5 C6 -57.3(6) . . . . ? C22 C18 C19 C13 4.6(9) . . . . ? C7 C18 C19 C13 177.5(5) . . . . ? C52 C57 C56 C55 0.1(10) . . . . ? C57 C52 C53 C54 1.4(10) . . . . ? P2 C52 C53 C54 -174.5(5) . . . . ? C46 P2 C45 C40 170.9(5) . . . . ? C52 P2 C45 C40 -77.9(5) . . . . ? Pt2 P2 C45 C40 39.7(5) . . . . ? C46 P2 C45 C44 -11.9(6) . . . . ? C52 P2 C45 C44 99.4(5) . . . . ? Pt2 P2 C45 C44 -143.0(5) . . . . ? N3 C9 C70 C71 162.1(6) . . . . ? N3 C9 C70 C75 -24.6(10) . . . . ? C71 C70 C75 C74 -2.8(9) . . . . ? C9 C70 C75 C74 -175.9(6) . . . . ? C71 C70 C75 P3 174.4(5) . . . . ? C9 C70 C75 P3 1.3(8) . . . . ? C82 P3 C75 C74 95.8(6) . . . . ? C76 P3 C75 C74 -13.9(7) . . . . ? Pt3 P3 C75 C74 -143.1(6) . . . . ? C82 P3 C75 C70 -81.1(5) . . . . ? C76 P3 C75 C70 169.1(5) . . . . ? Pt3 P3 C75 C70 40.0(5) . . . . ? C5 N2 C8 C40 169.5(5) . . . . ? Pt2 N2 C8 C40 -7.6(8) . . . . ? C27 P1 C28 C29 74.9(6) . . . . ? C22 P1 C28 C29 -34.4(6) . . . . ? Pt1 P1 C28 C29 -152.5(5) . . . . ? C27 P1 C28 C33 -109.5(5) . . . . ? C22 P1 C28 C33 141.2(5) . . . . ? Pt1 P1 C28 C33 23.1(6) . . . . ? C33 C28 C29 C30 0.7(10) . . . . ? P1 C28 C29 C30 176.2(6) . . . . ? C20 C21 C22 C18 2.3(10) . . . . ? C20 C21 C22 P1 -172.3(5) . . . . ? C19 C18 C22 C21 -4.9(9) . . . . ? C7 C18 C22 C21 -177.1(6) . . . . ? C19 C18 C22 P1 169.7(5) . . . . ? C7 C18 C22 P1 -2.6(8) . . . . ? C28 P1 C22 C21 90.5(6) . . . . ? C27 P1 C22 C21 -22.2(6) . . . . ? Pt1 P1 C22 C21 -146.3(5) . . . . ? C28 P1 C22 C18 -84.0(5) . . . . ? C27 P1 C22 C18 163.3(5) . . . . ? Pt1 P1 C22 C18 39.2(5) . . . . ? C18 C19 C13 C20 -1.6(10) . . . . ? C75 C70 C71 C72 2.4(10) . . . . ? C9 C70 C71 C72 175.9(6) . . . . ? C45 P2 C46 C51 112.6(6) . . . . ? C52 P2 C46 C51 1.7(7) . . . . ? Pt2 P2 C46 C51 -127.6(6) . . . . ? C45 P2 C46 C47 -64.9(6) . . . . ? C52 P2 C46 C47 -175.9(5) . . . . ? Pt2 P2 C46 C47 54.9(6) . . . . ? C40 C45 C44 C43 -1.5(10) . . . . ? P2 C45 C44 C43 -178.8(6) . . . . ? C47 C46 C51 C50 1.3(11) . . . . ? P2 C46 C51 C50 -176.2(6) . . . . ? C44 C45 C40 C41 -1.1(9) . . . . ? P2 C45 C40 C41 176.3(5) . . . . ? C44 C45 C40 C8 -171.1(5) . . . . ? P2 C45 C40 C8 6.2(8) . . . . ? N2 C8 C40 C45 -30.4(9) . . . . ? N2 C8 C40 C41 159.1(6) . . . . ? C45 C40 C41 C42 3.5(10) . . . . ? C8 C40 C41 C42 174.2(6) . . . . ? C52 C53 C54 C55 -0.4(11) . . . . ? C53 C54 C55 C56 -0.7(11) . . . . ? C57 C56 C55 C54 0.9(11) . . . . ? C45 C44 C43 C42 1.7(12) . . . . ? C44 C43 C42 C41 0.8(13) . . . . ? C40 C41 C42 C43 -3.4(12) . . . . ? C51 C46 C47 C48 1.3(11) . . . . ? P2 C46 C47 C48 178.9(6) . . . . ? C46 C51 C50 C49 -2.1(13) . . . . ? C51 C50 C49 C48 0.2(15) . . . . ? C46 C47 C48 C49 -3.2(13) . . . . ? C50 C49 C48 C47 2.5(14) . . . . ? C28 C29 C30 C31 1.0(12) . . . . ? C28 P1 C27 C23 -177.8(6) . . . . ? C22 P1 C27 C23 -67.3(7) . . . . ? Pt1 P1 C27 C23 50.5(7) . . . . ? C28 P1 C27 C26 2.2(7) . . . . ? C22 P1 C27 C26 112.7(6) . . . . ? Pt1 P1 C27 C26 -129.5(5) . . . . ? C29 C28 C33 C32 -0.6(10) . . . . ? P1 C28 C33 C32 -176.3(6) . . . . ? C26 C27 C23 C24 -2.8(12) . . . . ? P1 C27 C23 C24 177.2(7) . . . . ? C23 C27 C26 C16 2.0(11) . . . . ? P1 C27 C26 C16 -178.0(6) . . . . ? C19 C13 C20 C21 -1.2(11) . . . . ? C22 C21 C20 C13 0.8(11) . . . . ? C28 C33 C32 C31 -1.1(12) . . . . ? C29 C30 C31 C32 -2.7(14) . . . . ? C33 C32 C31 C30 2.7(13) . . . . ? C70 C71 C72 C73 -0.4(11) . . . . ? C76 P3 C82 C83 69.4(6) . . . . ? C75 P3 C82 C83 -40.4(6) . . . . ? Pt3 P3 C82 C83 -156.6(5) . . . . ? C76 P3 C82 C87 -108.9(6) . . . . ? C75 P3 C82 C87 141.3(5) . . . . ? Pt3 P3 C82 C87 25.2(6) . . . . ? C78 C77 C76 C81 -2.8(11) . . . . ? C78 C77 C76 P3 179.6(6) . . . . ? C82 P3 C76 C81 12.3(7) . . . . ? C75 P3 C76 C81 120.7(6) . . . . ? Pt3 P3 C76 C81 -118.4(6) . . . . ? C82 P3 C76 C77 -170.3(6) . . . . ? C75 P3 C76 C77 -61.9(6) . . . . ? Pt3 P3 C76 C77 59.1(6) . . . . ? C70 C75 C74 C73 1.4(11) . . . . ? P3 C75 C74 C73 -175.6(6) . . . . ? C77 C76 C81 C80 3.0(12) . . . . ? P3 C76 C81 C80 -179.6(7) . . . . ? C87 C82 C83 C84 2.6(12) . . . . ? P3 C82 C83 C84 -175.6(6) . . . . ? C83 C82 C87 C86 -2.1(11) . . . . ? P3 C82 C87 C86 176.2(6) . . . . ? C75 C74 C73 C72 0.4(13) . . . . ? C71 C72 C73 C74 -1.0(13) . . . . ? C27 C23 C24 C25 0.6(14) . . . . ? C27 C26 C16 C25 1.0(13) . . . . ? C23 C24 C25 C16 2.6(15) . . . . ? C26 C16 C25 C24 -3.3(15) . . . . ? C80 C79 C78 C77 1.5(14) . . . . ? C76 C77 C78 C79 0.6(12) . . . . ? C82 C83 C84 C85 -1.2(13) . . . . ? C83 C84 C85 C86 -0.7(14) . . . . ? C78 C79 C80 C81 -1.4(15) . . . . ? C76 C81 C80 C79 -0.9(14) . . . . ? C84 C85 C86 C87 1.1(15) . . . . ? C82 C87 C86 C85 0.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.138 _refine_diff_density_min -1.422 _refine_diff_density_rms 0.153