# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1612 data_global _audit_creation_method SHELXL-97 # SUBMISSION DETAILS _publ_contact_author ; Dr Jonathan P. H. Charmant School of Chemistry University of Bristol Bristol BS8 1TS UK ; _publ_contact_author_email jon.charmant@bris.ac.uk _publ_contact_author_fax '+44(0)117 929 0509' _publ_contact_author_phone '+44(0)117 928 9812' _publ_contact_letter ; Please consider this CIF submission for publication in Chemical Communications ; _publ_requested_journal 'Chemical Communications' # TITLE AND AUTHOR LIST _publ_section_title ; 1,2-Phenylenediisocyanide for Triangles ; loop_ _publ_author_name _publ_author_address 'Pablo Espinet' ; Departmento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Valladolid E-47005 Valladolid Spain ; 'Katerina Soulantica' ; Departmento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Valladolid E-47005 Valladolid Spain ; 'Jonathan P. H. Charmant' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'A. Guy Orpen' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; ######################################################################### data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H28 F30 N6 O2 Pt3' _chemical_formula_weight 2116.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.732(2) _cell_length_b 11.9065(15) _cell_length_c 26.506(3) _cell_angle_alpha 78.765(9) _cell_angle_beta 83.179(9) _cell_angle_gamma 65.113(11) _cell_volume 3291.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 205 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 6.497 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ; Parameters determined using XPREP (Bruker AXS Inc.) software with 3249 Psi-scan data and a lamina model of crystal shape. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'frames each covering 0.3\% in \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 30636 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.1185 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14436 _reflns_number_gt 8872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14436 _refine_ls_number_parameters 1001 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.40185(3) 0.62485(3) 0.253999(14) 0.02872(10) Uani 1 1 d . . . Pt2 Pt 0.35462(3) 0.16573(3) 0.313157(15) 0.02891(10) Uani 1 1 d . . . Pt3 Pt -0.01529(3) 0.56694(3) 0.191966(16) 0.03384(11) Uani 1 1 d . . . C1 C 0.5270(8) 0.4844(9) 0.2938(4) 0.030(2) Uani 1 1 d . . . C2 C 0.6941(7) 0.3068(8) 0.3514(4) 0.030(2) Uani 1 1 d . . . C3 C 0.7880(9) 0.3280(10) 0.3695(4) 0.039(2) Uani 1 1 d . . . H3 H 0.7898 0.4085 0.3601 0.047 Uiso 1 1 calc R . . C4 C 0.8756(9) 0.2396(10) 0.3996(4) 0.045(3) Uani 1 1 d . . . H4 H 0.9383 0.2574 0.4117 0.054 Uiso 1 1 calc R . . C5 C 0.8756(9) 0.1204(10) 0.4135(4) 0.049(3) Uani 1 1 d . . . H5 H 0.9390 0.0568 0.4347 0.059 Uiso 1 1 calc R . . C6 C 0.7841(8) 0.0946(9) 0.3965(4) 0.035(2) Uani 1 1 d . . . H6 H 0.7831 0.0139 0.4059 0.042 Uiso 1 1 calc R . . C7 C 0.6940(7) 0.1889(8) 0.3655(4) 0.029(2) Uani 1 1 d . . . C8 C 0.5045(7) 0.1680(8) 0.3326(4) 0.029(2) Uani 1 1 d . . . C9 C 0.2021(9) 0.1546(9) 0.2949(4) 0.032(2) Uani 1 1 d . . . C10 C 0.0188(8) 0.1232(8) 0.2733(3) 0.0229(19) Uani 1 1 d . . . C11 C 0.0152(9) 0.0079(9) 0.2896(4) 0.039(2) Uani 1 1 d . . . H11 H 0.0798 -0.0553 0.3104 0.047 Uiso 1 1 calc R . . C12 C -0.0805(9) -0.0179(10) 0.2763(4) 0.042(3) Uani 1 1 d . . . H12 H -0.0815 -0.0980 0.2883 0.051 Uiso 1 1 calc R . . C13 C -0.1752(8) 0.0726(9) 0.2455(3) 0.034(2) Uani 1 1 d . . . H13 H -0.2399 0.0540 0.2356 0.041 Uiso 1 1 calc R . . C14 C -0.1744(8) 0.1912(9) 0.2291(4) 0.031(2) Uani 1 1 d . . . H14 H -0.2409 0.2545 0.2093 0.037 Uiso 1 1 calc R . . C15 C -0.0784(8) 0.2173(8) 0.2414(3) 0.0244(19) Uani 1 1 d . . . C16 C -0.0485(8) 0.4191(9) 0.2130(4) 0.035(2) Uani 1 1 d . . . C17 C 0.0093(8) 0.7208(10) 0.1707(4) 0.038(2) Uani 1 1 d . . . C18 C 0.0236(8) 0.9324(8) 0.1404(4) 0.031(2) Uani 1 1 d . . . C19 C -0.0646(8) 1.0238(9) 0.1084(4) 0.038(2) Uani 1 1 d . . . H19 H -0.1280 1.0077 0.0959 0.046 Uiso 1 1 calc R . . C20 C -0.0599(10) 1.1405(9) 0.0947(4) 0.045(3) Uani 1 1 d . . . H20 H -0.1217 1.2052 0.0731 0.053 Uiso 1 1 calc R . . C21 C 0.0315(9) 1.1632(9) 0.1115(4) 0.040(2) Uani 1 1 d . . . H21 H 0.0338 1.2433 0.1013 0.048 Uiso 1 1 calc R . . C22 C 0.1235(9) 1.0694(9) 0.1440(4) 0.035(2) Uani 1 1 d . . . H22 H 0.1883 1.0848 0.1557 0.042 Uiso 1 1 calc R . . C23 C 0.1166(8) 0.9552(8) 0.1584(3) 0.0231(19) Uani 1 1 d . . . C24 C 0.2767(8) 0.7672(9) 0.2144(4) 0.032(2) Uani 1 1 d . . . C25 C 0.4865(8) 0.5597(8) 0.1868(3) 0.028(2) Uani 1 1 d . . . C26 C 0.4277(9) 0.5310(9) 0.1516(4) 0.037(2) Uani 1 1 d . . . C27 C 0.4810(10) 0.4875(9) 0.1069(4) 0.040(3) Uani 1 1 d . . . C28 C 0.6059(10) 0.4636(10) 0.0950(4) 0.042(3) Uani 1 1 d . . . C29 C 0.6710(8) 0.4912(9) 0.1280(4) 0.037(2) Uani 1 1 d . . . C30 C 0.6094(9) 0.5367(9) 0.1722(4) 0.036(2) Uani 1 1 d . . . C31 C 0.3201(8) 0.6918(9) 0.3220(4) 0.034(2) Uani 1 1 d . . . C32 C 0.3810(9) 0.7196(10) 0.3545(4) 0.045(3) Uani 1 1 d . . . C33 C 0.3272(11) 0.7644(11) 0.3998(5) 0.054(3) Uani 1 1 d . . . C34 C 0.2073(11) 0.7772(11) 0.4156(4) 0.051(3) Uani 1 1 d . . . C35 C 0.1406(10) 0.7478(9) 0.3848(4) 0.043(3) Uani 1 1 d . . . C36 C 0.1979(9) 0.7065(9) 0.3389(4) 0.034(2) Uani 1 1 d . . . C37 C 0.4398(7) 0.1078(9) 0.2449(4) 0.028(2) Uani 1 1 d . . . C38 C 0.5075(8) 0.1673(8) 0.2112(3) 0.028(2) Uani 1 1 d . . . C39 C 0.5631(9) 0.1311(10) 0.1646(4) 0.041(3) Uani 1 1 d . . . C40 C 0.5589(9) 0.0283(10) 0.1505(4) 0.039(2) Uani 1 1 d . . . C41 C 0.4926(9) -0.0340(10) 0.1819(4) 0.043(3) Uani 1 1 d . . . C42 C 0.4367(9) 0.0072(9) 0.2264(4) 0.037(2) Uani 1 1 d . . . C43 C 0.2679(8) 0.2256(9) 0.3812(3) 0.027(2) Uani 1 1 d . . . C44 C 0.2573(8) 0.3349(10) 0.3954(4) 0.040(3) Uani 1 1 d . . . C45 C 0.1984(9) 0.3794(10) 0.4401(4) 0.043(3) Uani 1 1 d . . . C46 C 0.1453(9) 0.3089(10) 0.4743(4) 0.042(3) Uani 1 1 d . . . C47 C 0.1521(9) 0.2006(10) 0.4630(4) 0.036(2) Uani 1 1 d . . . C48 C 0.2119(9) 0.1602(9) 0.4169(4) 0.040(2) Uani 1 1 d . . . C49 C 0.0725(9) 0.5037(9) 0.1246(4) 0.036(2) Uani 1 1 d . . . C50 C 0.1674(9) 0.3868(10) 0.1233(4) 0.036(2) Uani 1 1 d . . . C51 C 0.2292(9) 0.3396(10) 0.0793(4) 0.044(3) Uani 1 1 d . . . C52 C 0.1947(10) 0.4144(10) 0.0317(4) 0.044(3) Uani 1 1 d . . . C53 C 0.1004(10) 0.5360(11) 0.0308(4) 0.044(3) Uani 1 1 d . . . C54 C 0.0416(9) 0.5757(10) 0.0752(4) 0.044(3) Uani 1 1 d . . . C55 C -0.0982(8) 0.6261(9) 0.2601(4) 0.037(2) Uani 1 1 d . . . C56 C -0.1929(9) 0.7419(10) 0.2658(4) 0.044(3) Uani 1 1 d . . . C57 C -0.2509(9) 0.7832(9) 0.3112(4) 0.044(3) Uani 1 1 d . . . C58 C -0.2089(10) 0.7020(11) 0.3562(5) 0.050(3) Uani 1 1 d . . . C59 C -0.1155(10) 0.5857(10) 0.3550(4) 0.045(3) Uani 1 1 d . . . C60 C -0.0629(9) 0.5523(9) 0.3089(4) 0.037(2) Uani 1 1 d . . . F1 F 0.3042(5) 0.5503(6) 0.1612(2) 0.0560(17) Uani 1 1 d . . . F2 F 0.4195(6) 0.4605(7) 0.0748(3) 0.067(2) Uani 1 1 d . . . F3 F 0.6645(5) 0.4183(6) 0.0518(2) 0.0527(16) Uani 1 1 d . . . F4 F 0.7931(5) 0.4693(6) 0.1176(2) 0.0544(17) Uani 1 1 d . . . F5 F 0.6798(5) 0.5581(6) 0.2038(2) 0.0473(15) Uani 1 1 d . . . F6 F 0.5012(5) 0.7066(6) 0.3429(2) 0.0581(18) Uani 1 1 d . . . F7 F 0.3951(7) 0.7903(7) 0.4308(3) 0.078(2) Uani 1 1 d . . . F8 F 0.1542(7) 0.8221(7) 0.4597(2) 0.078(2) Uani 1 1 d . . . F9 F 0.0204(6) 0.7676(6) 0.3968(3) 0.071(2) Uani 1 1 d . . . F10 F 0.1267(5) 0.6816(6) 0.3094(2) 0.0491(16) Uani 1 1 d . . . F11 F 0.5174(5) 0.2664(5) 0.2229(2) 0.0448(14) Uani 1 1 d . . . F12 F 0.6301(5) 0.1886(6) 0.1353(2) 0.0531(16) Uani 1 1 d . . . F13 F 0.6176(6) -0.0125(6) 0.1062(2) 0.0594(18) Uani 1 1 d . . . F14 F 0.4875(7) -0.1334(7) 0.1672(3) 0.069(2) Uani 1 1 d . . . F15 F 0.3733(5) -0.0585(5) 0.2552(2) 0.0489(16) Uani 1 1 d . . . F16 F 0.3104(5) 0.4069(5) 0.3635(2) 0.0499(15) Uani 1 1 d . . . F17 F 0.1888(6) 0.4883(6) 0.4511(2) 0.0604(18) Uani 1 1 d . . . F18 F 0.0845(6) 0.3513(6) 0.5180(2) 0.0635(19) Uani 1 1 d . . . F19 F 0.1008(5) 0.1288(6) 0.4960(2) 0.0571(17) Uani 1 1 d . . . F20 F 0.2121(5) 0.0516(5) 0.4077(2) 0.0492(15) Uani 1 1 d . . . F21 F 0.2052(5) 0.3041(5) 0.1682(2) 0.0464(15) Uani 1 1 d . . . F22 F 0.3200(6) 0.2228(6) 0.0810(2) 0.0578(17) Uani 1 1 d . . . F23 F 0.2522(6) 0.3726(6) -0.0119(2) 0.0610(18) Uani 1 1 d . . . F24 F 0.0679(6) 0.6084(6) -0.0153(2) 0.0620(19) Uani 1 1 d . . . F25 F -0.0472(5) 0.6924(5) 0.0709(2) 0.0539(16) Uani 1 1 d . . . F26 F -0.2354(5) 0.8266(5) 0.2215(2) 0.0569(17) Uani 1 1 d . . . F27 F -0.3403(6) 0.8969(6) 0.3128(3) 0.0668(19) Uani 1 1 d . . . F28 F -0.2600(6) 0.7380(7) 0.4015(3) 0.072(2) Uani 1 1 d . . . F29 F -0.0763(6) 0.5049(6) 0.3999(2) 0.0572(17) Uani 1 1 d . . . F30 F 0.0303(5) 0.4309(5) 0.3102(2) 0.0498(15) Uani 1 1 d . . . N1 N 0.6026(7) 0.4026(7) 0.3198(3) 0.0310(18) Uani 1 1 d . . . N2 N 0.5953(7) 0.1696(7) 0.3474(3) 0.0312(18) Uani 1 1 d . . . N3 N 0.1141(7) 0.1482(7) 0.2853(3) 0.0349(19) Uani 1 1 d . . . N4 N -0.0706(6) 0.3309(7) 0.2246(3) 0.0299(17) Uani 1 1 d . . . N5 N 0.0176(7) 0.8156(7) 0.1568(3) 0.0356(19) Uani 1 1 d . . . N6 N 0.2052(7) 0.8565(7) 0.1902(3) 0.0315(18) Uani 1 1 d . . . C78 C 0.4587(13) 0.9185(13) 0.5130(5) 0.069(4) Uani 1 1 d . . . C79 C 0.5322(13) 0.943(2) 0.4643(6) 0.116(8) Uani 1 1 d . . . O79 O 0.3882(17) 1.0267(17) 0.5388(7) 0.070(5) Uani 0.50 1 d P . . O80A O 0.417(2) 0.807(3) 0.0107(8) 0.17(2) Uani 0.56(4) 1 d PD A 1 O80B O 0.326(5) 0.960(4) 0.0183(12) 0.33(5) Uani 0.44(4) 1 d PD A 2 C81 C 0.382(2) 0.851(3) 0.0640(10) 0.228(17) Uani 1 1 d D . . C82 C 0.2874(15) 0.8070(18) 0.0779(7) 0.111(6) Uani 1 1 d D A . C83 C 0.246(2) 0.792(2) 0.0349(7) 0.154(9) Uani 1 1 d D . . C84 C 0.273(3) 0.875(3) -0.0010(10) 0.26(2) Uani 1 1 d D A . C98 C 0.4822(16) 0.4466(16) 0.4695(8) 0.114(6) Uani 1 1 d . . . C99 C 0.3981(18) 0.4937(17) 0.5156(7) 0.117(7) Uani 1 1 d . . . O99 O 0.5563(16) 0.5052(15) 0.4354(6) 0.071(5) Uani 0.50 1 d P . . 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 0.02461(18) 0.0213(2) 0.0383(2) -0.00009(15) -0.00661(15) -0.00812(15) Pt2 0.02434(18) 0.0245(2) 0.0399(2) -0.00121(16) -0.00816(16) -0.01189(15) Pt3 0.0303(2) 0.0212(2) 0.0517(3) 0.00528(17) -0.01172(17) -0.01433(16) C1 0.028(5) 0.023(5) 0.047(6) -0.011(4) -0.004(4) -0.014(4) C2 0.016(4) 0.024(5) 0.046(6) -0.005(4) -0.003(4) -0.004(4) C3 0.040(6) 0.034(6) 0.051(7) -0.001(5) -0.012(5) -0.023(5) C4 0.037(6) 0.041(7) 0.066(8) -0.007(5) -0.026(5) -0.018(5) C5 0.028(5) 0.043(7) 0.063(8) -0.002(5) -0.017(5) -0.001(5) C6 0.027(5) 0.036(6) 0.039(6) -0.001(4) -0.003(4) -0.011(4) C7 0.010(4) 0.022(5) 0.048(6) -0.002(4) -0.007(4) 0.000(3) C8 0.015(4) 0.024(5) 0.042(6) 0.002(4) -0.006(4) -0.005(4) C9 0.039(5) 0.025(5) 0.042(6) -0.003(4) -0.007(5) -0.020(5) C10 0.028(4) 0.027(5) 0.024(5) -0.012(4) 0.003(4) -0.020(4) C11 0.038(5) 0.028(6) 0.052(7) 0.001(5) -0.012(5) -0.015(5) C12 0.052(6) 0.032(6) 0.058(7) -0.001(5) -0.015(5) -0.030(5) C13 0.035(5) 0.031(6) 0.036(6) -0.005(4) -0.016(4) -0.010(4) C14 0.023(4) 0.026(5) 0.043(6) -0.002(4) -0.006(4) -0.010(4) C15 0.026(4) 0.014(4) 0.036(5) -0.001(4) 0.000(4) -0.012(4) C16 0.029(5) 0.033(6) 0.048(6) 0.000(5) -0.018(4) -0.017(4) C17 0.029(5) 0.036(6) 0.053(7) 0.002(5) -0.009(4) -0.018(5) C18 0.032(5) 0.018(5) 0.040(6) 0.003(4) 0.002(4) -0.011(4) C19 0.025(5) 0.029(6) 0.059(7) 0.003(5) -0.007(4) -0.012(4) C20 0.051(6) 0.021(6) 0.053(7) 0.012(5) -0.012(5) -0.011(5) C21 0.050(6) 0.023(6) 0.051(7) 0.004(4) -0.019(5) -0.018(5) C22 0.040(5) 0.032(6) 0.036(6) -0.003(4) -0.008(4) -0.018(5) C23 0.026(4) 0.021(5) 0.020(5) 0.004(3) -0.003(4) -0.010(4) C24 0.023(5) 0.030(6) 0.048(6) -0.011(5) 0.000(4) -0.014(4) C25 0.029(5) 0.023(5) 0.032(5) 0.006(4) -0.013(4) -0.011(4) C26 0.034(5) 0.028(6) 0.049(7) 0.001(5) 0.001(5) -0.016(4) C27 0.049(6) 0.033(6) 0.050(7) -0.013(5) -0.006(5) -0.025(5) C28 0.048(6) 0.036(6) 0.049(7) -0.018(5) 0.004(5) -0.019(5) C29 0.020(4) 0.025(5) 0.055(7) -0.007(5) 0.007(4) 0.000(4) C30 0.031(5) 0.027(6) 0.044(6) 0.004(4) -0.010(5) -0.006(4) C31 0.032(5) 0.024(5) 0.044(6) 0.004(4) -0.009(4) -0.011(4) C32 0.038(6) 0.031(6) 0.064(8) -0.016(5) -0.008(5) -0.006(5) C33 0.064(8) 0.040(7) 0.056(8) -0.017(6) -0.025(6) -0.010(6) C34 0.052(7) 0.045(7) 0.042(7) -0.005(5) 0.002(6) -0.008(6) C35 0.049(6) 0.020(6) 0.049(7) 0.002(5) 0.001(6) -0.006(5) C36 0.037(5) 0.025(5) 0.038(6) 0.007(4) -0.019(5) -0.013(4) C37 0.014(4) 0.027(5) 0.043(6) -0.002(4) -0.012(4) -0.007(4) C38 0.029(5) 0.021(5) 0.032(5) 0.004(4) -0.012(4) -0.009(4) C39 0.038(6) 0.039(7) 0.040(6) 0.000(5) -0.006(5) -0.012(5) C40 0.039(6) 0.039(6) 0.037(6) -0.004(5) -0.003(5) -0.013(5) C41 0.043(6) 0.031(6) 0.064(8) -0.009(5) -0.011(5) -0.020(5) C42 0.031(5) 0.032(6) 0.050(7) -0.001(5) -0.004(5) -0.016(5) C43 0.021(4) 0.027(5) 0.031(5) 0.000(4) -0.013(4) -0.008(4) C44 0.025(5) 0.045(7) 0.048(7) -0.001(5) -0.013(5) -0.012(5) C45 0.034(5) 0.041(7) 0.047(7) -0.006(5) -0.013(5) -0.008(5) C46 0.030(5) 0.046(7) 0.040(7) -0.002(5) -0.004(5) -0.008(5) C47 0.032(5) 0.034(6) 0.039(6) 0.004(5) -0.010(4) -0.011(5) C48 0.042(6) 0.016(5) 0.057(7) 0.006(4) -0.023(5) -0.008(4) C49 0.035(5) 0.037(6) 0.047(6) 0.005(5) -0.014(5) -0.026(5) C50 0.033(5) 0.038(6) 0.040(6) 0.005(5) -0.008(5) -0.022(5) C51 0.034(5) 0.030(6) 0.067(8) 0.000(5) -0.002(5) -0.015(5) C52 0.046(6) 0.039(7) 0.048(7) -0.002(5) 0.000(5) -0.023(5) C53 0.049(6) 0.049(7) 0.044(7) 0.009(5) -0.012(5) -0.034(6) C54 0.040(6) 0.035(7) 0.060(8) 0.011(5) -0.013(5) -0.023(5) C55 0.023(5) 0.030(6) 0.053(7) -0.006(5) -0.009(4) -0.006(4) C56 0.037(6) 0.039(7) 0.055(7) 0.006(5) -0.014(5) -0.020(5) C57 0.032(5) 0.025(6) 0.069(8) -0.009(5) -0.012(5) -0.003(4) C58 0.047(7) 0.038(7) 0.067(8) -0.014(6) -0.015(6) -0.014(5) C59 0.041(6) 0.035(7) 0.058(8) 0.002(5) -0.014(5) -0.016(5) C60 0.037(5) 0.030(6) 0.045(7) 0.000(5) -0.013(5) -0.015(5) F1 0.038(3) 0.084(5) 0.065(4) -0.031(4) 0.002(3) -0.035(3) F2 0.057(4) 0.098(6) 0.068(5) -0.039(4) 0.003(3) -0.045(4) F3 0.051(4) 0.058(4) 0.051(4) -0.020(3) 0.001(3) -0.020(3) F4 0.030(3) 0.072(5) 0.050(4) -0.010(3) -0.005(3) -0.010(3) F5 0.030(3) 0.070(5) 0.049(4) -0.014(3) -0.004(3) -0.025(3) F6 0.040(3) 0.068(5) 0.081(5) -0.025(4) -0.013(3) -0.028(3) F7 0.090(5) 0.065(5) 0.077(5) -0.036(4) -0.029(4) -0.013(4) F8 0.101(6) 0.067(5) 0.043(4) -0.014(4) 0.006(4) -0.012(4) F9 0.053(4) 0.070(5) 0.068(5) -0.009(4) 0.027(3) -0.013(4) F10 0.031(3) 0.050(4) 0.075(4) -0.015(3) -0.006(3) -0.022(3) F11 0.045(3) 0.034(4) 0.059(4) -0.004(3) -0.003(3) -0.021(3) F12 0.052(4) 0.057(4) 0.060(4) -0.005(3) 0.013(3) -0.038(3) F13 0.069(4) 0.067(5) 0.052(4) -0.020(3) 0.013(3) -0.036(4) F14 0.091(5) 0.072(5) 0.074(5) -0.042(4) 0.024(4) -0.055(4) F15 0.063(4) 0.043(4) 0.059(4) -0.016(3) 0.015(3) -0.040(3) F16 0.059(4) 0.036(4) 0.064(4) -0.006(3) 0.002(3) -0.030(3) F17 0.075(4) 0.048(4) 0.065(4) -0.028(3) 0.003(3) -0.025(4) F18 0.069(4) 0.069(5) 0.048(4) -0.020(3) 0.006(3) -0.021(4) F19 0.055(4) 0.065(5) 0.050(4) 0.006(3) 0.004(3) -0.032(4) F20 0.054(4) 0.042(4) 0.059(4) -0.004(3) -0.003(3) -0.029(3) F21 0.048(3) 0.037(4) 0.045(4) 0.006(3) -0.011(3) -0.012(3) F22 0.054(4) 0.038(4) 0.067(4) -0.007(3) -0.003(3) -0.005(3) F23 0.073(4) 0.062(5) 0.052(4) -0.006(3) 0.005(3) -0.036(4) F24 0.064(4) 0.059(5) 0.056(4) 0.020(3) -0.019(3) -0.026(4) F25 0.056(4) 0.031(4) 0.064(4) 0.015(3) -0.020(3) -0.012(3) F26 0.049(4) 0.029(4) 0.075(5) 0.010(3) -0.012(3) -0.004(3) F27 0.052(4) 0.036(4) 0.095(5) -0.023(3) -0.008(4) 0.005(3) F28 0.073(5) 0.062(5) 0.067(5) -0.031(4) 0.001(4) -0.007(4) F29 0.061(4) 0.050(4) 0.054(4) -0.007(3) -0.018(3) -0.013(3) F30 0.052(4) 0.031(3) 0.054(4) -0.001(3) -0.016(3) -0.004(3) N1 0.029(4) 0.022(4) 0.041(5) -0.002(3) -0.012(4) -0.009(3) N2 0.030(4) 0.026(4) 0.037(5) -0.003(3) -0.004(3) -0.011(3) N3 0.034(4) 0.029(5) 0.044(5) -0.004(4) -0.010(4) -0.014(4) N4 0.026(4) 0.030(5) 0.040(5) -0.004(4) -0.008(3) -0.016(4) N5 0.028(4) 0.023(5) 0.052(5) 0.003(4) -0.007(4) -0.010(4) N6 0.031(4) 0.025(5) 0.037(5) -0.004(3) -0.002(4) -0.011(4) C78 0.084(10) 0.057(9) 0.066(9) 0.001(7) 0.003(7) -0.034(8) C79 0.041(8) 0.17(2) 0.096(13) 0.021(12) 0.004(8) -0.028(11) O79 0.080(13) 0.069(13) 0.077(13) -0.036(10) 0.019(10) -0.042(11) O80A 0.105(19) 0.23(4) 0.081(19) 0.039(18) 0.041(14) -0.013(18) O80B 0.77(14) 0.31(7) 0.12(3) -0.09(4) 0.16(5) -0.44(9) C81 0.14(2) 0.43(5) 0.18(3) -0.05(3) 0.02(2) -0.19(3) C82 0.086(12) 0.157(19) 0.102(14) -0.070(13) 0.018(10) -0.046(12) C83 0.17(2) 0.18(3) 0.110(17) -0.046(16) -0.042(15) -0.058(19) C84 0.36(5) 0.39(5) 0.18(3) 0.14(3) -0.14(3) -0.34(5) C98 0.099(13) 0.061(12) 0.157(19) 0.000(11) 0.011(12) -0.021(10) C99 0.152(17) 0.096(14) 0.108(14) -0.032(11) -0.083(13) -0.030(13) O99 0.084(13) 0.042(11) 0.066(12) 0.001(8) 0.005(10) -0.010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 1.918(10) . ? Pt1 C24 1.925(10) . ? Pt1 C25 2.057(9) . ? Pt1 C31 2.076(10) . ? Pt2 C8 1.902(9) . ? Pt2 C9 1.970(9) . ? Pt2 C37 2.056(9) . ? Pt2 C43 2.062(9) . ? Pt3 C16 1.925(10) . ? Pt3 C17 1.939(10) . ? Pt3 C55 2.051(10) . ? Pt3 C49 2.062(10) . ? C1 N1 1.170(11) . ? C2 C7 1.380(12) . ? C2 C3 1.384(12) . ? C2 N1 1.402(11) . ? C3 C4 1.326(13) . ? C4 C5 1.395(14) . ? C5 C6 1.376(13) . ? C6 C7 1.379(12) . ? C7 N2 1.423(11) . ? C8 N2 1.188(10) . ? C9 N3 1.128(11) . ? C10 N3 1.357(10) . ? C10 C11 1.372(12) . ? C10 C15 1.434(12) . ? C11 C12 1.380(12) . ? C12 C13 1.389(13) . ? C13 C14 1.398(12) . ? C14 C15 1.375(11) . ? C15 N4 1.377(10) . ? C16 N4 1.161(11) . ? C17 N5 1.159(11) . ? C18 C19 1.369(12) . ? C18 C23 1.383(12) . ? C18 N5 1.403(11) . ? C19 C20 1.388(13) . ? C20 C21 1.351(13) . ? C21 C22 1.410(13) . ? C22 C23 1.373(12) . ? C23 N6 1.403(11) . ? C24 N6 1.166(11) . ? C25 C30 1.371(12) . ? C25 C26 1.392(13) . ? C26 C27 1.362(13) . ? C26 F1 1.368(10) . ? C27 F2 1.339(11) . ? C27 C28 1.379(13) . ? C28 F3 1.349(11) . ? C28 C29 1.393(14) . ? C29 F4 1.347(10) . ? C29 C30 1.380(13) . ? C30 F5 1.368(11) . ? C31 C32 1.348(14) . ? C31 C36 1.397(12) . ? C32 F6 1.356(11) . ? C32 C33 1.383(14) . ? C33 F7 1.366(12) . ? C33 C34 1.372(15) . ? C34 F8 1.352(12) . ? C34 C35 1.376(16) . ? C35 F9 1.338(11) . ? C35 C36 1.391(13) . ? C36 F10 1.361(10) . ? C37 C42 1.394(13) . ? C37 C38 1.409(12) . ? C38 F11 1.330(10) . ? C38 C39 1.386(13) . ? C39 F12 1.338(11) . ? C39 C40 1.367(15) . ? C40 F13 1.355(11) . ? C40 C41 1.392(13) . ? C41 F14 1.342(11) . ? C41 C42 1.355(14) . ? C42 F15 1.367(10) . ? C43 C44 1.376(14) . ? C43 C48 1.389(12) . ? C44 F16 1.371(11) . ? C44 C45 1.381(14) . ? C45 F17 1.340(12) . ? C45 C46 1.387(14) . ? C46 C47 1.346(14) . ? C46 F18 1.355(11) . ? C47 F19 1.370(10) . ? C47 C48 1.400(14) . ? C48 F20 1.361(11) . ? C49 C50 1.372(13) . ? C49 C54 1.412(13) . ? C50 F21 1.373(10) . ? C50 C51 1.383(14) . ? C51 F22 1.346(11) . ? C51 C52 1.389(14) . ? C52 F23 1.339(12) . ? C52 C53 1.402(15) . ? C53 F24 1.342(11) . ? C53 C54 1.355(15) . ? C54 F25 1.333(11) . ? C55 C56 1.382(13) . ? C55 C60 1.413(13) . ? C56 F26 1.377(11) . ? C56 C57 1.381(14) . ? C57 F27 1.323(11) . ? C57 C58 1.375(15) . ? C58 F28 1.340(12) . ? C58 C59 1.360(14) . ? C59 C60 1.355(14) . ? C59 F29 1.364(12) . ? C60 F30 1.396(11) . ? C78 O79 1.46(2) . ? C78 C79 1.514(17) . ? C78 C79 1.91(3) 2_676 ? C79 O79 1.12(2) 2_676 ? C79 C78 1.91(3) 2_676 ? O79 C79 1.12(2) 2_676 ? O80A C81 1.55(2) . ? O80A C84 1.58(2) . ? O80B C81 1.56(2) . ? O80B C84 1.57(2) . ? C81 C82 1.396(17) . ? C82 C83 1.363(16) . ? C83 C84 1.348(18) . ? C98 O99 1.46(2) . ? C98 C99 1.51(2) . ? C98 C99 1.93(2) 2_666 ? C99 O99 1.47(2) 2_666 ? C99 C98 1.93(2) 2_666 ? O99 C99 1.47(2) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C24 179.3(4) . . ? C1 Pt1 C25 90.9(4) . . ? C24 Pt1 C25 89.4(4) . . ? C1 Pt1 C31 88.6(4) . . ? C24 Pt1 C31 91.0(4) . . ? C25 Pt1 C31 178.6(4) . . ? C8 Pt2 C9 177.1(4) . . ? C8 Pt2 C37 91.3(4) . . ? C9 Pt2 C37 88.9(4) . . ? C8 Pt2 C43 89.0(4) . . ? C9 Pt2 C43 90.9(4) . . ? C37 Pt2 C43 179.4(4) . . ? C16 Pt3 C17 177.2(4) . . ? C16 Pt3 C55 89.1(4) . . ? C17 Pt3 C55 89.7(4) . . ? C16 Pt3 C49 90.4(4) . . ? C17 Pt3 C49 90.8(4) . . ? C55 Pt3 C49 178.4(4) . . ? N1 C1 Pt1 176.5(8) . . ? C7 C2 C3 117.8(8) . . ? C7 C2 N1 121.6(8) . . ? C3 C2 N1 120.6(8) . . ? C4 C3 C2 122.0(9) . . ? C3 C4 C5 119.9(9) . . ? C6 C5 C4 120.2(9) . . ? C5 C6 C7 118.3(9) . . ? C6 C7 C2 121.6(9) . . ? C6 C7 N2 121.3(8) . . ? C2 C7 N2 117.0(7) . . ? N2 C8 Pt2 176.4(8) . . ? N3 C9 Pt2 178.8(9) . . ? N3 C10 C11 121.5(8) . . ? N3 C10 C15 119.6(7) . . ? C11 C10 C15 118.9(8) . . ? C10 C11 C12 121.3(9) . . ? C11 C12 C13 120.4(9) . . ? C12 C13 C14 119.2(9) . . ? C15 C14 C13 120.8(8) . . ? C14 C15 N4 123.2(8) . . ? C14 C15 C10 119.3(7) . . ? N4 C15 C10 117.5(7) . . ? N4 C16 Pt3 178.2(8) . . ? N5 C17 Pt3 176.3(8) . . ? C19 C18 C23 120.8(8) . . ? C19 C18 N5 120.0(9) . . ? C23 C18 N5 119.2(8) . . ? C18 C19 C20 118.8(9) . . ? C21 C20 C19 120.9(9) . . ? C20 C21 C22 120.8(9) . . ? C23 C22 C21 118.0(9) . . ? C22 C23 C18 120.8(8) . . ? C22 C23 N6 121.5(8) . . ? C18 C23 N6 117.7(8) . . ? N6 C24 Pt1 176.4(8) . . ? C30 C25 C26 112.2(9) . . ? C30 C25 Pt1 123.4(7) . . ? C26 C25 Pt1 124.4(7) . . ? C27 C26 F1 115.6(9) . . ? C27 C26 C25 125.9(9) . . ? F1 C26 C25 118.4(9) . . ? F2 C27 C26 123.1(9) . . ? F2 C27 C28 117.8(9) . . ? C26 C27 C28 119.0(10) . . ? F3 C28 C27 121.8(10) . . ? F3 C28 C29 119.7(9) . . ? C27 C28 C29 118.5(9) . . ? F4 C29 C30 121.1(9) . . ? F4 C29 C28 120.1(9) . . ? C30 C29 C28 118.7(9) . . ? F5 C30 C25 118.6(9) . . ? F5 C30 C29 115.8(8) . . ? C25 C30 C29 125.6(10) . . ? C32 C31 C36 114.4(10) . . ? C32 C31 Pt1 123.4(7) . . ? C36 C31 Pt1 122.1(8) . . ? C31 C32 F6 120.0(9) . . ? C31 C32 C33 123.8(10) . . ? F6 C32 C33 116.2(10) . . ? F7 C33 C34 119.1(11) . . ? F7 C33 C32 120.4(11) . . ? C34 C33 C32 120.4(11) . . ? F8 C34 C33 120.5(12) . . ? F8 C34 C35 120.7(10) . . ? C33 C34 C35 118.8(11) . . ? F9 C35 C34 120.7(10) . . ? F9 C35 C36 120.7(10) . . ? C34 C35 C36 118.4(10) . . ? F10 C36 C35 116.0(9) . . ? F10 C36 C31 119.9(9) . . ? C35 C36 C31 124.1(10) . . ? C42 C37 C38 112.6(9) . . ? C42 C37 Pt2 124.3(7) . . ? C38 C37 Pt2 123.1(7) . . ? F11 C38 C39 116.3(8) . . ? F11 C38 C37 120.0(8) . . ? C39 C38 C37 123.7(9) . . ? F12 C39 C40 119.6(9) . . ? F12 C39 C38 120.7(10) . . ? C40 C39 C38 119.5(9) . . ? F13 C40 C39 120.6(9) . . ? F13 C40 C41 119.8(10) . . ? C39 C40 C41 119.5(10) . . ? F14 C41 C42 122.4(9) . . ? F14 C41 C40 118.9(10) . . ? C42 C41 C40 118.7(10) . . ? C41 C42 F15 115.4(9) . . ? C41 C42 C37 125.9(9) . . ? F15 C42 C37 118.7(9) . . ? C44 C43 C48 113.3(9) . . ? C44 C43 Pt2 123.7(7) . . ? C48 C43 Pt2 122.9(7) . . ? F16 C44 C43 118.7(9) . . ? F16 C44 C45 115.7(10) . . ? C43 C44 C45 125.6(10) . . ? F17 C45 C44 122.6(10) . . ? F17 C45 C46 119.2(10) . . ? C44 C45 C46 118.1(11) . . ? C47 C46 F18 120.8(9) . . ? C47 C46 C45 119.6(10) . . ? F18 C46 C45 119.5(10) . . ? C46 C47 F19 121.0(9) . . ? C46 C47 C48 120.0(9) . . ? F19 C47 C48 119.0(9) . . ? F20 C48 C43 120.2(9) . . ? F20 C48 C47 116.5(9) . . ? C43 C48 C47 123.3(9) . . ? C50 C49 C54 113.1(10) . . ? C50 C49 Pt3 123.2(7) . . ? C54 C49 Pt3 123.7(8) . . ? C49 C50 F21 119.9(9) . . ? C49 C50 C51 125.6(9) . . ? F21 C50 C51 114.4(9) . . ? F22 C51 C50 122.2(9) . . ? F22 C51 C52 118.9(10) . . ? C50 C51 C52 118.9(10) . . ? F23 C52 C51 120.9(10) . . ? F23 C52 C53 121.1(10) . . ? C51 C52 C53 117.9(10) . . ? F24 C53 C54 121.9(10) . . ? F24 C53 C52 117.8(10) . . ? C54 C53 C52 120.2(10) . . ? F25 C54 C53 116.4(9) . . ? F25 C54 C49 119.4(10) . . ? C53 C54 C49 124.1(10) . . ? C56 C55 C60 110.0(9) . . ? C56 C55 Pt3 126.4(8) . . ? C60 C55 Pt3 123.7(7) . . ? F26 C56 C57 115.6(10) . . ? F26 C56 C55 117.1(10) . . ? C57 C56 C55 127.3(10) . . ? F27 C57 C58 119.9(10) . . ? F27 C57 C56 122.9(10) . . ? C58 C57 C56 117.1(10) . . ? F28 C58 C59 119.9(10) . . ? F28 C58 C57 119.7(10) . . ? C59 C58 C57 120.4(11) . . ? C60 C59 C58 118.9(10) . . ? C60 C59 F29 121.1(10) . . ? C58 C59 F29 119.9(11) . . ? C59 C60 F30 116.2(8) . . ? C59 C60 C55 126.2(10) . . ? F30 C60 C55 117.5(9) . . ? C1 N1 C2 178.6(9) . . ? C8 N2 C7 172.3(9) . . ? C9 N3 C10 171.9(9) . . ? C16 N4 C15 171.1(9) . . ? C17 N5 C18 178.2(9) . . ? C24 N6 C23 173.8(9) . . ? O79 C78 C79 115.3(14) . . ? O79 C78 C79 36.0(8) . 2_676 ? C79 C78 C79 88.5(12) . 2_676 ? O79 C79 C78 127(2) 2_676 . ? O79 C79 C78 49.6(14) 2_676 2_676 ? C78 C79 C78 91.5(12) . 2_676 ? C79 O79 C78 94.5(17) 2_676 . ? C81 O80A C84 87.8(16) . . ? C81 O80B C84 87.5(16) . . ? C82 C81 O80A 96.9(17) . . ? C82 C81 O80B 104(2) . . ? O80A C81 O80B 67(2) . . ? C83 C82 C81 109.6(18) . . ? C84 C83 C82 101(2) . . ? C83 C84 O80B 117(2) . . ? C83 C84 O80A 92(2) . . ? O80B C84 O80A 66(2) . . ? O99 C98 C99 127.8(17) . . ? O99 C98 C99 48.9(10) . 2_666 ? C99 C98 C99 92.0(17) . 2_666 ? O99 C99 C98 124.4(18) 2_666 . ? O99 C99 C98 48.8(10) 2_666 2_666 ? C98 C99 C98 88.0(17) . 2_666 ? C98 O99 C99 82.3(14) . 2_666 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.721 _refine_diff_density_min -1.954 _refine_diff_density_rms 0.186