# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cameron Jones' _publ_contact_author_email CAMERON.JONES@SCI.MONASH.EDU.AU _publ_section_title ; Using "Click" Chemistry to Access a New Class of Tripodal P3-Ligand Containing P=C Bonds ; loop_ _publ_author_name 'Cameron Jones' 'Sam L Choong' 'Andreas Stasch' # Attachment 'compound3.CIF' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 766028' #TrackingRef 'compound3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H42 N9 P3' _chemical_formula_weight 585.61 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.543(4) _cell_length_b 10.510(2) _cell_length_c 30.197(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6202(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12852 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6767 _reflns_number_gt 5294 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+1.8574P] 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 6767 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.14941(2) 0.64620(4) 0.113027(13) 0.02130(11) Uani 1 1 d . . . N1 N 0.19071(6) 0.66894(12) 0.06442(4) 0.0214(3) Uani 1 1 d . . . C1 C 0.09986(8) 0.75390(14) 0.01545(5) 0.0199(3) Uani 1 1 d . . . P2 P -0.09544(2) 0.74653(4) 0.114560(15) 0.02764(12) Uani 1 1 d . . . N2 N 0.24591(7) 0.59478(14) 0.05711(4) 0.0277(3) Uani 1 1 d . . . C2 C 0.04885(8) 0.83115(15) 0.03425(5) 0.0219(3) Uani 1 1 d . . . P3 P 0.02501(2) 0.75828(4) -0.124124(14) 0.02472(11) Uani 1 1 d . . . N3 N 0.25629(7) 0.51842(13) 0.09062(4) 0.0270(3) Uani 1 1 d . . . C3 C -0.01919(8) 0.81933(15) 0.01915(5) 0.0231(3) Uani 1 1 d . . . N4 N -0.11966(7) 0.82947(13) 0.06930(4) 0.0257(3) Uani 1 1 d . . . C4 C -0.03642(8) 0.72997(15) -0.01355(5) 0.0227(3) Uani 1 1 d . . . N5 N -0.18646(7) 0.82542(17) 0.05950(5) 0.0407(4) Uani 1 1 d . . . C5 C 0.01496(8) 0.65012(15) -0.03070(5) 0.0216(3) Uani 1 1 d . . . N6 N -0.22017(7) 0.75646(17) 0.08819(5) 0.0386(4) Uani 1 1 d . . . C6 C 0.08316(8) 0.66287(15) -0.01711(5) 0.0210(3) Uani 1 1 d . . . N7 N 0.00353(6) 0.60715(13) -0.11042(4) 0.0206(3) Uani 1 1 d . . . C7 C 0.17409(8) 0.76445(15) 0.02976(5) 0.0226(3) Uani 1 1 d . . . H7A H 0.2042 0.7512 0.0038 0.027 Uiso 1 1 calc R . . H7B H 0.1828 0.8510 0.0414 0.027 Uiso 1 1 calc R . . N8 N -0.01048(7) 0.52857(12) -0.14415(4) 0.0223(3) Uani 1 1 d . . . C8 C 0.06533(9) 0.92574(16) 0.07073(5) 0.0280(4) Uani 1 1 d . . . H8A H 0.1143 0.9222 0.0775 0.042 Uiso 1 1 calc R . . H8B H 0.0390 0.9044 0.0973 0.042 Uiso 1 1 calc R . . H8C H 0.0533 1.0117 0.0609 0.042 Uiso 1 1 calc R . . N9 N -0.00449(6) 0.58721(12) -0.18221(4) 0.0225(3) Uani 1 1 d . . . C9 C -0.07526(8) 0.90261(16) 0.03890(5) 0.0283(4) Uani 1 1 d . . . H9A H -0.0541 0.9742 0.0552 0.034 Uiso 1 1 calc R . . H9B H -0.1034 0.9387 0.0147 0.034 Uiso 1 1 calc R . . C10 C -0.10879(8) 0.72008(18) -0.03094(6) 0.0311(4) Uani 1 1 d . . . H10A H -0.1313 0.6459 -0.0177 0.047 Uiso 1 1 calc R . . H10B H -0.1078 0.7107 -0.0632 0.047 Uiso 1 1 calc R . . H10C H -0.1342 0.7973 -0.0231 0.047 Uiso 1 1 calc R . . C11 C -0.00393(8) 0.55298(15) -0.06557(5) 0.0239(3) Uani 1 1 d . . . H11A H 0.0260 0.4775 -0.0626 0.029 Uiso 1 1 calc R . . H11B H -0.0518 0.5252 -0.0610 0.029 Uiso 1 1 calc R . . C12 C 0.13954(8) 0.58482(17) -0.03802(5) 0.0278(4) Uani 1 1 d . . . H12A H 0.1195 0.5130 -0.0541 0.042 Uiso 1 1 calc R . . H12B H 0.1701 0.5527 -0.0149 0.042 Uiso 1 1 calc R . . H12C H 0.1656 0.6382 -0.0586 0.042 Uiso 1 1 calc R . . C13 C 0.21032(7) 0.53243(15) 0.12407(5) 0.0204(3) Uani 1 1 d . . . C14 C 0.21705(8) 0.44993(15) 0.16514(5) 0.0226(3) Uani 1 1 d . . . C15 C 0.29252(8) 0.43918(17) 0.17883(6) 0.0289(4) Uani 1 1 d . . . H15A H 0.3188 0.4002 0.1547 0.043 Uiso 1 1 calc R . . H15B H 0.2962 0.3863 0.2054 0.043 Uiso 1 1 calc R . . H15C H 0.3107 0.5242 0.1850 0.043 Uiso 1 1 calc R . . C16 C 0.17649(9) 0.50917(16) 0.20326(5) 0.0272(4) Uani 1 1 d . . . H16A H 0.1942 0.5946 0.2094 0.041 Uiso 1 1 calc R . . H16B H 0.1812 0.4560 0.2298 0.041 Uiso 1 1 calc R . . H16C H 0.1281 0.5148 0.1950 0.041 Uiso 1 1 calc R . . C17 C 0.18812(9) 0.31736(15) 0.15474(6) 0.0278(4) Uani 1 1 d . . . H17A H 0.1391 0.3242 0.1485 0.042 Uiso 1 1 calc R . . H17B H 0.1952 0.2612 0.1803 0.042 Uiso 1 1 calc R . . H17C H 0.2117 0.2821 0.1289 0.042 Uiso 1 1 calc R . . C18 C -0.18044(8) 0.70654(16) 0.12027(5) 0.0250(3) Uani 1 1 d . . . C19 C -0.21282(8) 0.62734(17) 0.15671(6) 0.0296(4) Uani 1 1 d . . . C20 C -0.16361(9) 0.52224(17) 0.17113(6) 0.0314(4) Uani 1 1 d . . . H20A H -0.1574 0.4618 0.1468 0.047 Uiso 1 1 calc R . . H20B H -0.1826 0.4777 0.1969 0.047 Uiso 1 1 calc R . . H20C H -0.1194 0.5598 0.1790 0.047 Uiso 1 1 calc R . . C21 C -0.22664(13) 0.7142(2) 0.19654(7) 0.0532(6) Uani 1 1 d . . . H21A H -0.1836 0.7527 0.2064 0.080 Uiso 1 1 calc R . . H21B H -0.2463 0.6639 0.2207 0.080 Uiso 1 1 calc R . . H21C H -0.2588 0.7813 0.1879 0.080 Uiso 1 1 calc R . . C22 C -0.27945(10) 0.5673(2) 0.14037(9) 0.0582(7) Uani 1 1 d . . . H22A H -0.3123 0.6345 0.1331 0.087 Uiso 1 1 calc R . . H22B H -0.2985 0.5129 0.1637 0.087 Uiso 1 1 calc R . . H22C H -0.2702 0.5160 0.1139 0.087 Uiso 1 1 calc R . . C23 C 0.01390(8) 0.71150(15) -0.17829(5) 0.0215(3) Uani 1 1 d . . . C24 C 0.02147(8) 0.79072(16) -0.21985(5) 0.0252(3) Uani 1 1 d . . . C25 C 0.04350(10) 0.92584(17) -0.20814(6) 0.0346(4) Uani 1 1 d . . . H25A H 0.0090 0.9650 -0.1890 0.052 Uiso 1 1 calc R . . H25B H 0.0482 0.9760 -0.2353 0.052 Uiso 1 1 calc R . . H25C H 0.0875 0.9233 -0.1926 0.052 Uiso 1 1 calc R . . C26 C 0.07482(9) 0.72834(17) -0.25021(6) 0.0322(4) Uani 1 1 d . . . H26A H 0.1197 0.7300 -0.2357 0.048 Uiso 1 1 calc R . . H26B H 0.0772 0.7752 -0.2782 0.048 Uiso 1 1 calc R . . H26C H 0.0616 0.6400 -0.2561 0.048 Uiso 1 1 calc R . . C27 C -0.04764(9) 0.79507(19) -0.24405(6) 0.0367(4) Uani 1 1 d . . . H27A H -0.0623 0.7083 -0.2511 0.055 Uiso 1 1 calc R . . H27B H -0.0428 0.8442 -0.2715 0.055 Uiso 1 1 calc R . . H27C H -0.0819 0.8356 -0.2250 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0183(2) 0.0234(2) 0.0222(2) 0.00077(16) 0.00087(16) 0.00206(16) N1 0.0170(6) 0.0257(7) 0.0216(7) -0.0001(5) -0.0020(5) -0.0012(5) C1 0.0204(8) 0.0228(8) 0.0165(7) 0.0052(6) 0.0004(6) -0.0029(6) P2 0.0208(2) 0.0339(3) 0.0282(2) 0.00959(18) -0.00128(17) 0.00037(18) N2 0.0224(7) 0.0362(8) 0.0246(7) -0.0006(6) 0.0016(6) 0.0063(6) C2 0.0262(8) 0.0227(8) 0.0169(7) 0.0050(6) 0.0007(6) -0.0012(6) P3 0.0321(2) 0.0231(2) 0.0190(2) 0.00064(16) -0.00024(17) -0.00431(17) N3 0.0235(7) 0.0341(8) 0.0232(7) -0.0010(6) 0.0019(6) 0.0060(6) C3 0.0250(8) 0.0264(8) 0.0178(7) 0.0078(6) 0.0035(6) 0.0022(6) N4 0.0218(7) 0.0328(8) 0.0226(7) 0.0031(6) 0.0029(6) 0.0060(6) C4 0.0206(8) 0.0308(9) 0.0167(7) 0.0083(6) 0.0001(6) -0.0015(6) N5 0.0233(8) 0.0672(12) 0.0315(8) 0.0156(8) 0.0016(6) 0.0062(7) C5 0.0230(8) 0.0260(8) 0.0157(7) 0.0041(6) 0.0001(6) -0.0040(6) N6 0.0230(7) 0.0637(11) 0.0290(8) 0.0138(8) 0.0013(6) 0.0026(7) C6 0.0223(8) 0.0247(8) 0.0160(7) 0.0043(6) 0.0018(6) -0.0013(6) N7 0.0201(6) 0.0246(7) 0.0171(6) 0.0005(5) -0.0021(5) -0.0019(5) C7 0.0206(8) 0.0268(8) 0.0203(8) 0.0025(6) -0.0008(6) -0.0039(6) N8 0.0230(7) 0.0254(7) 0.0186(6) -0.0003(5) -0.0010(5) -0.0011(5) C8 0.0336(9) 0.0260(8) 0.0244(8) -0.0014(7) 0.0003(7) 0.0000(7) N9 0.0238(7) 0.0254(7) 0.0183(6) 0.0010(5) 0.0001(5) 0.0003(5) C9 0.0276(9) 0.0328(9) 0.0245(8) 0.0077(7) 0.0044(7) 0.0052(7) C10 0.0213(8) 0.0446(10) 0.0275(9) 0.0051(8) -0.0024(7) -0.0009(7) C11 0.0264(8) 0.0283(8) 0.0170(7) 0.0051(6) -0.0026(6) -0.0068(7) C12 0.0243(8) 0.0341(9) 0.0250(8) -0.0045(7) 0.0023(7) -0.0004(7) C13 0.0171(7) 0.0221(8) 0.0221(8) -0.0042(6) -0.0023(6) -0.0014(6) C14 0.0218(8) 0.0234(8) 0.0225(8) -0.0016(6) -0.0030(6) 0.0024(6) C15 0.0246(9) 0.0301(9) 0.0320(9) -0.0001(7) -0.0063(7) 0.0031(7) C16 0.0307(9) 0.0301(9) 0.0208(8) -0.0009(7) -0.0011(7) 0.0040(7) C17 0.0260(9) 0.0243(8) 0.0330(9) -0.0015(7) -0.0006(7) 0.0007(7) C18 0.0221(8) 0.0289(8) 0.0241(8) -0.0008(7) 0.0022(6) 0.0035(7) C19 0.0238(9) 0.0318(9) 0.0331(9) 0.0057(7) 0.0057(7) 0.0018(7) C20 0.0290(9) 0.0311(9) 0.0340(9) 0.0052(7) 0.0018(7) 0.0029(7) C21 0.0770(16) 0.0391(11) 0.0434(12) 0.0079(9) 0.0368(11) 0.0150(11) C22 0.0270(10) 0.0667(15) 0.0810(17) 0.0342(14) -0.0061(10) -0.0103(10) C23 0.0182(7) 0.0256(8) 0.0208(8) 0.0005(6) 0.0008(6) 0.0012(6) C24 0.0255(8) 0.0298(9) 0.0202(8) 0.0041(7) -0.0003(6) 0.0000(7) C25 0.0457(11) 0.0296(9) 0.0286(9) 0.0060(7) 0.0000(8) -0.0037(8) C26 0.0354(10) 0.0356(9) 0.0257(9) 0.0051(7) 0.0088(8) -0.0008(8) C27 0.0317(9) 0.0466(11) 0.0318(10) 0.0148(8) -0.0074(8) -0.0002(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 N1 1.6920(13) . ? P1 C13 1.7198(16) . ? N1 N2 1.3491(18) . ? N1 C7 1.4860(19) . ? C1 C2 1.406(2) . ? C1 C6 1.410(2) . ? C1 C7 1.518(2) . ? P2 N4 1.6887(14) . ? P2 C18 1.7222(17) . ? N2 N3 1.3073(19) . ? C2 C3 1.411(2) . ? C2 C8 1.518(2) . ? P3 N7 1.6943(14) . ? P3 C23 1.7217(16) . ? N3 C13 1.3599(19) . ? C3 C4 1.404(2) . ? C3 C9 1.524(2) . ? N4 N5 1.3393(19) . ? N4 C9 1.479(2) . ? C4 C5 1.407(2) . ? C4 C10 1.512(2) . ? N5 N6 1.308(2) . ? C5 C6 1.401(2) . ? C5 C11 1.512(2) . ? N6 C18 1.348(2) . ? C6 C12 1.512(2) . ? N7 N8 1.3398(18) . ? N7 C11 1.4763(19) . ? N8 N9 1.3092(18) . ? N9 C23 1.360(2) . ? C13 C14 1.519(2) . ? C14 C16 1.530(2) . ? C14 C15 1.536(2) . ? C14 C17 1.536(2) . ? C18 C19 1.518(2) . ? C19 C20 1.528(2) . ? C19 C22 1.529(3) . ? C19 C21 1.534(3) . ? C23 C24 1.513(2) . ? C24 C25 1.525(2) . ? C24 C26 1.535(2) . ? C24 C27 1.536(2) . ? 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 P1 C13 86.35(7) . . ? N2 N1 C7 116.73(12) . . ? N2 N1 P1 116.22(10) . . ? C7 N1 P1 127.02(10) . . ? C2 C1 C6 120.62(14) . . ? C2 C1 C7 121.38(14) . . ? C6 C1 C7 117.99(14) . . ? N4 P2 C18 86.37(7) . . ? N3 N2 N1 110.61(12) . . ? C1 C2 C3 119.14(14) . . ? C1 C2 C8 121.38(14) . . ? C3 C2 C8 119.47(14) . . ? N7 P3 C23 86.17(7) . . ? N2 N3 C13 113.96(13) . . ? C4 C3 C2 120.81(14) . . ? C4 C3 C9 119.15(14) . . ? C2 C3 C9 120.03(15) . . ? N5 N4 C9 116.83(13) . . ? N5 N4 P2 115.83(11) . . ? C9 N4 P2 127.32(11) . . ? C3 C4 C5 119.12(14) . . ? C3 C4 C10 120.97(15) . . ? C5 C4 C10 119.91(15) . . ? N6 N5 N4 111.23(14) . . ? C6 C5 C4 120.93(14) . . ? C6 C5 C11 120.05(14) . . ? C4 C5 C11 118.98(14) . . ? N5 N6 C18 113.69(14) . . ? C5 C6 C1 119.30(14) . . ? C5 C6 C12 121.28(14) . . ? C1 C6 C12 119.38(14) . . ? N8 N7 C11 116.08(12) . . ? N8 N7 P3 116.28(10) . . ? C11 N7 P3 127.60(10) . . ? N1 C7 C1 111.10(12) . . ? N9 N8 N7 111.04(12) . . ? N8 N9 C23 113.54(13) . . ? N4 C9 C3 111.49(13) . . ? N7 C11 C5 110.75(12) . . ? N3 C13 C14 119.18(13) . . ? N3 C13 P1 112.85(11) . . ? C14 C13 P1 127.96(11) . . ? C13 C14 C16 109.70(13) . . ? C13 C14 C15 110.17(13) . . ? C16 C14 C15 108.96(13) . . ? C13 C14 C17 108.60(13) . . ? C16 C14 C17 109.41(13) . . ? C15 C14 C17 109.98(13) . . ? N6 C18 C19 119.62(14) . . ? N6 C18 P2 112.88(12) . . ? C19 C18 P2 127.48(12) . . ? C18 C19 C20 109.91(13) . . ? C18 C19 C22 110.34(15) . . ? C20 C19 C22 109.25(16) . . ? C18 C19 C21 108.40(15) . . ? C20 C19 C21 108.50(15) . . ? C22 C19 C21 110.41(17) . . ? N9 C23 C24 118.83(13) . . ? N9 C23 P3 112.97(11) . . ? C24 C23 P3 128.20(12) . . ? C23 C24 C25 110.35(13) . . ? C23 C24 C26 109.06(13) . . ? C25 C24 C26 110.14(14) . . ? C23 C24 C27 108.96(13) . . ? C25 C24 C27 109.31(15) . . ? C26 C24 C27 109.01(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.348 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.050 # Attachment 'compound4.CIF' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 766029' #TrackingRef 'compound4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N9 P3' _chemical_formula_weight 459.37 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 hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.456(3) _cell_length_b 17.456(3) _cell_length_c 12.415(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3276.2(9) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2982 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.00 _reflns_number_total 1586 _reflns_number_gt 1048 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^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 1586 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.48199(4) 0.81988(5) 0.04234(6) 0.0344(3) Uani 1 1 d . . . N1 N 0.54622(12) 0.83217(12) -0.06637(16) 0.0270(5) Uani 1 1 d . . . C1 C 0.42182(14) 0.73489(14) -0.18349(18) 0.0224(5) Uani 1 1 d . . . N2 N 0.63367(13) 0.87651(14) -0.04878(19) 0.0357(6) Uani 1 1 d . . . C2 C 0.40185(14) 0.64612(15) -0.18384(18) 0.0222(5) Uani 1 1 d . . . N3 N 0.65213(14) 0.90207(14) 0.05178(18) 0.0355(6) Uani 1 1 d . . . C3 C 0.51760(14) 0.80737(15) -0.17964(18) 0.0257(6) Uani 1 1 d . . . H3A H 0.5550 0.7867 -0.2147 0.031 Uiso 1 1 calc R . . H3B H 0.5250 0.8597 -0.2196 0.031 Uiso 1 1 calc R . . C4 C 0.47662(15) 0.62604(16) -0.1826(2) 0.0283(6) Uani 1 1 d . . . H4A H 0.4527 0.5627 -0.1698 0.043 Uiso 1 1 calc R . . H4B H 0.5183 0.6600 -0.1251 0.043 Uiso 1 1 calc R . . H4C H 0.5073 0.6424 -0.2521 0.043 Uiso 1 1 calc R . . C5 C 0.57951(16) 0.87912(16) 0.1127(2) 0.0334(6) Uani 1 1 d . . . C6 C 0.59193(18) 0.90748(19) 0.2280(2) 0.0427(7) Uani 1 1 d . . . H6A H 0.6258 0.8845 0.2652 0.064 Uiso 1 1 calc R . . H6B H 0.5340 0.8843 0.2625 0.064 Uiso 1 1 calc R . . H6C H 0.6241 0.9722 0.2318 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0238(4) 0.0409(5) 0.0321(4) -0.0025(3) -0.0008(3) 0.0115(3) N1 0.0204(11) 0.0218(10) 0.0363(13) -0.0009(9) -0.0011(9) 0.0086(9) C1 0.0236(12) 0.0223(13) 0.0192(12) 0.0010(9) 0.0034(9) 0.0100(10) N2 0.0217(11) 0.0350(13) 0.0491(15) -0.0012(11) -0.0016(10) 0.0131(10) C2 0.0264(13) 0.0249(13) 0.0174(12) 0.0013(9) 0.0028(9) 0.0143(10) N3 0.0287(12) 0.0338(13) 0.0436(14) -0.0034(11) -0.0063(11) 0.0153(10) C3 0.0234(12) 0.0235(13) 0.0283(13) 0.0062(10) 0.0069(11) 0.0103(11) C4 0.0263(13) 0.0281(13) 0.0324(14) -0.0029(11) 0.0037(11) 0.0149(11) C5 0.0298(14) 0.0264(14) 0.0425(16) 0.0027(12) -0.0042(12) 0.0129(12) C6 0.0396(16) 0.0407(17) 0.0391(18) -0.0045(13) -0.0078(13) 0.0136(14) _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 N1 1.698(2) . ? P1 C5 1.723(3) . ? N1 N2 1.340(3) . ? N1 C3 1.483(3) . ? C1 C2 1.404(3) 2_665 ? C1 C2 1.408(3) . ? C1 C3 1.511(3) . ? N2 N3 1.311(3) . ? C2 C1 1.404(3) 3_565 ? C2 C4 1.511(3) . ? N3 C5 1.353(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.494(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 P1 C5 86.30(12) . . ? N2 N1 C3 116.33(19) . . ? N2 N1 P1 115.65(16) . . ? C3 N1 P1 127.74(15) . . ? C2 C1 C2 120.6(2) 2_665 . ? C2 C1 C3 120.5(2) 2_665 . ? C2 C1 C3 118.9(2) . . ? N3 N2 N1 111.5(2) . . ? C1 C2 C1 119.4(2) 3_565 . ? C1 C2 C4 121.4(2) 3_565 . ? C1 C2 C4 119.2(2) . . ? N2 N3 C5 113.4(2) . . ? N1 C3 C1 110.16(18) . . ? N1 C3 H3A 109.6 . . ? C1 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C1 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 118.6(2) . . ? N3 C5 P1 113.1(2) . . ? C6 C5 P1 128.4(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.429 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.066 # Attachment 'compound7.CIF' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 766030' #TrackingRef 'compound7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H58 N9 P3 Pt2' _chemical_formula_weight 1160.05 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.300(3) _cell_length_b 10.424(2) _cell_length_c 28.869(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.59(3) _cell_angle_gamma 90.00 _cell_volume 4900.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 5.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.329 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16459 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.1188 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8596 _reflns_number_gt 5222 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diffraction data for the structure were very weak at theta angles higher than 23 deg. The thin plate crystal selected for the diffraction experiment was found to be a non-merohedral twin. Efforts to deconvolute the two diffraction patterns from the twin were not successful. During the course of refinement two molecules of toluene were located in the crystal lattice. Their atomic positions were refined at 50% occupancy. Due to significant and apparently diffuse residual electron density about the atomic positions of these molecules, their refinements required using the DFIX and DANG commands of SHELXL. Attempts to model disorder of the two toluene molecules over two sites were not successful. The problems with the refinement of the toluene molecules were the source of the Level A alerts in the cifcheck output and the unusual thermal paramaters for C(28). However, despite the problems with the structure refinement, and the consequential poor quality of the structure, the molecular connectivity of the molecule is unambiguous and fully consistent with its spectroscopic data. The spectroscopic data also confirm the presence of one molecule of toluene per molecule of compound 7 in the crystal lattice. ; _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^)+(0.0925P)^2^+11.1884P] 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 8596 _refine_ls_number_parameters 503 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.00257(4) 0.11705(5) 0.175090(17) 0.03163(19) Uani 1 1 d . . . P1 P -0.0219(2) -0.0038(3) 0.23537(11) 0.0317(9) Uani 1 1 d . . . N1 N -0.1006(7) -0.0990(10) 0.2447(3) 0.033(3) Uani 1 1 d . . . C1 C -0.1756(9) -0.0456(13) 0.1695(4) 0.038(4) Uani 1 1 d . . . C48 C -0.379(4) 0.536(2) 0.0474(14) 0.29(5) Uiso 0.50 1 d PD . . H48A H -0.3794 0.5860 0.0186 0.435 Uiso 0.50 1 calc PR . . H48B H -0.3257 0.5439 0.0639 0.435 Uiso 0.50 1 calc PR . . H48C H -0.4222 0.5685 0.0670 0.435 Uiso 0.50 1 calc PR . . Pt2 Pt 0.02301(4) 0.26577(5) 0.103940(18) 0.03346(19) Uani 1 1 d . . . P2 P 0.0489(3) 0.0487(3) 0.10416(12) 0.0354(9) Uani 1 1 d . . . N2 N -0.1017(8) -0.1588(11) 0.2861(4) 0.041(3) Uani 1 1 d . . . C2 C -0.1435(8) -0.0946(13) 0.1286(4) 0.034(4) Uani 1 1 d . . . P3 P -0.0458(2) 0.3323(3) 0.16763(11) 0.0321(9) Uani 1 1 d . . . N3 N -0.0335(8) -0.1255(11) 0.3100(4) 0.039(3) Uani 1 1 d . . . C3 C -0.1426(8) -0.0091(12) 0.0905(4) 0.025(3) Uani 1 1 d . . . N4 N -0.0037(7) -0.0504(10) 0.0664(3) 0.031(3) Uani 1 1 d . . . C4 C -0.1738(9) 0.1165(13) 0.0932(4) 0.036(4) Uani 1 1 d . . . N5 N 0.0436(8) -0.1486(11) 0.0502(4) 0.038(3) Uani 1 1 d . . . C5 C -0.2015(9) 0.1594(12) 0.1354(4) 0.031(3) Uani 1 1 d . . . N6 N 0.1177(8) -0.1443(11) 0.0680(4) 0.041(3) Uani 1 1 d . . . C6 C -0.2051(9) 0.0792(12) 0.1737(4) 0.032(3) Uani 1 1 d . . . N7 N -0.1481(7) 0.3650(10) 0.1674(3) 0.030(3) Uani 1 1 d . . . C7 C -0.1757(8) -0.1337(12) 0.2134(4) 0.030(3) Uani 1 1 d . . . H7A H -0.2267 -0.1201 0.2301 0.035 Uiso 1 1 calc R . . H7B H -0.1731 -0.2249 0.2041 0.035 Uiso 1 1 calc R . . N8 N -0.1686(8) 0.4611(10) 0.1948(4) 0.038(3) Uani 1 1 d . . . C8 C -0.1093(9) -0.2287(12) 0.1261(5) 0.037(4) Uani 1 1 d . . . H8A H -0.0539 -0.2307 0.1408 0.055 Uiso 1 1 calc R . . H8B H -0.1070 -0.2546 0.0935 0.055 Uiso 1 1 calc R . . H8C H -0.1449 -0.2879 0.1423 0.055 Uiso 1 1 calc R . . N9 N -0.1051(8) 0.5146(11) 0.2159(4) 0.044(3) Uani 1 1 d . . . C9 C -0.0905(9) -0.0468(14) 0.0512(5) 0.044(4) Uani 1 1 d . . . H9A H -0.1076 -0.1323 0.0395 0.053 Uiso 1 1 calc R . . H9B H -0.0985 0.0157 0.0256 0.053 Uiso 1 1 calc R . . C10 C -0.1772(10) 0.2016(13) 0.0510(4) 0.040(4) Uani 1 1 d . . . H10A H -0.2215 0.2644 0.0536 0.060 Uiso 1 1 calc R . . H10B H -0.1877 0.1492 0.0232 0.060 Uiso 1 1 calc R . . H10C H -0.1247 0.2465 0.0488 0.060 Uiso 1 1 calc R . . C11 C -0.2176(8) 0.3013(12) 0.1411(4) 0.033(3) Uani 1 1 d . . . H11A H -0.2253 0.3416 0.1102 0.039 Uiso 1 1 calc R . . H11B H -0.2688 0.3134 0.1578 0.039 Uiso 1 1 calc R . . C12 C -0.2337(9) 0.1326(13) 0.2188(4) 0.033(3) Uani 1 1 d . . . H12A H -0.1958 0.2000 0.2300 0.049 Uiso 1 1 calc R . . H12B H -0.2349 0.0637 0.2419 0.049 Uiso 1 1 calc R . . H12C H -0.2889 0.1686 0.2138 0.049 Uiso 1 1 calc R . . C13 C 0.0166(9) -0.0422(13) 0.2897(4) 0.037(4) Uani 1 1 d . . . C14 C 0.0997(10) -0.0080(15) 0.3134(5) 0.045(4) Uani 1 1 d . . . C15 C 0.0795(12) 0.049(2) 0.3612(6) 0.081(6) Uani 1 1 d . . . H15A H 0.0485 0.1286 0.3566 0.121 Uiso 1 1 calc R . . H15B H 0.1307 0.0665 0.3791 0.121 Uiso 1 1 calc R . . H15C H 0.0466 -0.0130 0.3780 0.121 Uiso 1 1 calc R . . C16 C 0.1526(10) -0.1265(16) 0.3194(6) 0.067(5) Uani 1 1 d . . . H16A H 0.1262 -0.1873 0.3399 0.100 Uiso 1 1 calc R . . H16B H 0.2066 -0.1024 0.3331 0.100 Uiso 1 1 calc R . . H16C H 0.1594 -0.1667 0.2891 0.100 Uiso 1 1 calc R . . C17 C 0.1429(11) 0.0952(16) 0.2848(6) 0.064(5) Uani 1 1 d . . . H17A H 0.1531 0.0611 0.2540 0.096 Uiso 1 1 calc R . . H17B H 0.1952 0.1186 0.3006 0.096 Uiso 1 1 calc R . . H17C H 0.1078 0.1713 0.2817 0.096 Uiso 1 1 calc R . . C18 C 0.1327(9) -0.0448(13) 0.0963(4) 0.034(3) Uani 1 1 d . . . C19 C 0.2171(11) -0.0371(15) 0.1217(5) 0.050(4) Uani 1 1 d . . . C20 C 0.2207(15) -0.146(2) 0.1601(8) 0.111(8) Uani 1 1 d U . . H20A H 0.2502 -0.2208 0.1485 0.167 Uiso 1 1 calc R . . H20B H 0.1647 -0.1717 0.1671 0.167 Uiso 1 1 calc R . . H20C H 0.2493 -0.1140 0.1883 0.167 Uiso 1 1 calc R . . C21 C 0.2809(19) -0.047(3) 0.0834(10) 0.162(12) Uani 1 1 d U . . H21A H 0.3091 0.0355 0.0806 0.243 Uiso 1 1 calc R . . H21B H 0.2526 -0.0687 0.0538 0.243 Uiso 1 1 calc R . . H21C H 0.3211 -0.1139 0.0917 0.243 Uiso 1 1 calc R . . C22 C 0.2305(12) 0.0889(17) 0.1474(6) 0.076(6) Uani 1 1 d U . . H22A H 0.2866 0.0916 0.1612 0.114 Uiso 1 1 calc R . . H22B H 0.1912 0.0959 0.1720 0.114 Uiso 1 1 calc R . . H22C H 0.2225 0.1605 0.1257 0.114 Uiso 1 1 calc R . . C23 C -0.0354(10) 0.4558(12) 0.2066(5) 0.040(4) Uani 1 1 d . . . C24 C 0.0448(10) 0.5083(14) 0.2304(5) 0.046(4) Uani 1 1 d . . . C25 C 0.0425(14) 0.498(2) 0.2823(5) 0.095(8) Uani 1 1 d . . . H25A H 0.0030 0.5607 0.2936 0.142 Uiso 1 1 calc R . . H25B H 0.0971 0.5166 0.2963 0.142 Uiso 1 1 calc R . . H25C H 0.0257 0.4116 0.2908 0.142 Uiso 1 1 calc R . . C26 C 0.0570(12) 0.6477(15) 0.2150(7) 0.078(7) Uani 1 1 d . . . H26A H 0.0491 0.6536 0.1813 0.117 Uiso 1 1 calc R . . H26B H 0.1126 0.6758 0.2244 0.117 Uiso 1 1 calc R . . H26C H 0.0169 0.7028 0.2297 0.117 Uiso 1 1 calc R . . C27 C 0.1208(10) 0.4258(14) 0.2153(5) 0.052(5) Uani 1 1 d . . . H27A H 0.1184 0.4161 0.1815 0.078 Uiso 1 1 calc R . . H27B H 0.1191 0.3410 0.2298 0.078 Uiso 1 1 calc R . . H27C H 0.1719 0.4694 0.2251 0.078 Uiso 1 1 calc R . . C28 C 0.0663(8) 0.3260(12) 0.0373(4) 0.023(3) Uani 1 1 d . . . H28 H 0.0309 0.2615 0.0245 0.028 Uiso 1 1 calc R . . C29 C 0.0425(10) 0.4334(12) 0.0628(4) 0.037(4) Uani 1 1 d . . . H29 H -0.0117 0.4527 0.0713 0.044 Uiso 1 1 calc R . . C30 C 0.1176(10) 0.5124(14) 0.0742(5) 0.044(4) Uani 1 1 d . . . C31 C 0.1852(10) 0.4053(13) 0.0788(5) 0.043(4) Uani 1 1 d . . . H31A H 0.2415 0.4407 0.0782 0.052 Uiso 1 1 calc R . . H31B H 0.1798 0.3521 0.1069 0.052 Uiso 1 1 calc R . . C32 C 0.1600(10) 0.3319(14) 0.0339(4) 0.042(4) Uani 1 1 d . . . C33 C 0.1711(10) 0.4475(13) 0.0002(5) 0.044(4) Uani 1 1 d . . . H33A H 0.1370 0.4357 -0.0287 0.053 Uiso 1 1 calc R . . H33B H 0.2293 0.4560 -0.0077 0.053 Uiso 1 1 calc R . . C34 C 0.1425(10) 0.5686(13) 0.0274(5) 0.044(4) Uani 1 1 d . . . H34A H 0.1878 0.6313 0.0319 0.053 Uiso 1 1 calc R . . H34B H 0.0953 0.6109 0.0109 0.053 Uiso 1 1 calc R . . C35 C -0.338(2) -0.216(3) 0.0812(8) 0.086(13) Uiso 0.50 1 d PD . . C36 C -0.367(2) -0.103(2) 0.0995(11) 0.18(3) Uiso 0.50 1 d PD . . H36 H -0.3734 -0.0286 0.0809 0.218 Uiso 0.50 1 calc PR . . C37 C -0.385(3) -0.102(2) 0.1465(11) 0.13(2) Uiso 0.50 1 d PD . . H37 H -0.3996 -0.0237 0.1612 0.155 Uiso 0.50 1 calc PR . . C38 C -0.383(2) -0.216(3) 0.1711(8) 0.083(12) Uiso 0.50 1 d PD . . H38 H -0.4068 -0.2210 0.2004 0.099 Uiso 0.50 1 calc PR . . C39 C -0.3454(17) -0.324(2) 0.1534(8) 0.043(7) Uiso 0.50 1 d PD . . H39 H -0.3303 -0.3942 0.1731 0.051 Uiso 0.50 1 calc PR . . C40 C -0.330(2) -0.328(2) 0.1060(8) 0.084(12) Uiso 0.50 1 d PD . . H40 H -0.3151 -0.4057 0.0915 0.100 Uiso 0.50 1 calc PR . . C41 C -0.338(4) -0.225(4) 0.0304(8) 0.22(4) Uiso 0.50 1 d PD . . H41A H -0.3872 -0.1824 0.0168 0.327 Uiso 0.50 1 calc PR . . H41B H -0.3391 -0.3160 0.0214 0.327 Uiso 0.50 1 calc PR . . H41C H -0.2889 -0.1844 0.0192 0.327 Uiso 0.50 1 calc PR . . C42 C -0.3954(18) 0.401(2) 0.0363(8) 0.091(13) Uiso 0.50 1 d PD . . C43 C -0.4167(16) 0.320(3) 0.0710(7) 0.052(9) Uiso 0.50 1 d PD . . H43 H -0.4191 0.3509 0.1019 0.063 Uiso 0.50 1 calc PR . . C44 C -0.435(2) 0.192(2) 0.0604(9) 0.124(18) Uiso 0.50 1 d PD . . H44 H -0.4544 0.1353 0.0832 0.148 Uiso 0.50 1 calc PR . . C45 C -0.424(3) 0.150(2) 0.0150(10) 0.126(18) Uiso 0.50 1 d PD . . H45 H -0.4210 0.0608 0.0086 0.151 Uiso 0.50 1 calc PR . . C46 C -0.418(2) 0.239(3) -0.0206(8) 0.071(11) Uiso 0.50 1 d PD . . H46 H -0.4310 0.2156 -0.0519 0.085 Uiso 0.50 1 calc PR . . C47 C -0.390(2) 0.363(2) -0.0091(7) 0.065(10) Uiso 0.50 1 d PD . . H47 H -0.3695 0.4187 -0.0318 0.078 Uiso 0.50 1 calc PR . . 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 0.0389(4) 0.0245(3) 0.0314(3) -0.0010(2) 0.0009(3) 0.0004(3) P1 0.036(2) 0.0290(19) 0.0295(19) -0.0016(15) 0.0003(17) -0.0007(17) N1 0.048(8) 0.030(6) 0.021(6) 0.002(5) -0.005(5) -0.003(6) C1 0.044(10) 0.040(9) 0.029(8) -0.002(6) -0.007(7) -0.007(7) Pt2 0.0425(4) 0.0254(3) 0.0325(3) -0.0004(2) 0.0015(3) 0.0015(3) P2 0.043(3) 0.0262(19) 0.037(2) -0.0021(16) 0.0011(18) 0.0016(18) N2 0.043(8) 0.044(7) 0.035(7) 0.011(6) -0.007(6) -0.013(6) C2 0.024(9) 0.039(8) 0.037(8) -0.006(7) -0.019(7) -0.012(7) P3 0.042(3) 0.0250(18) 0.0296(19) -0.0008(15) 0.0011(17) 0.0087(18) N3 0.046(9) 0.036(7) 0.035(6) 0.007(5) 0.005(6) 0.002(6) C3 0.025(8) 0.029(7) 0.020(6) -0.005(5) -0.006(6) 0.002(6) N4 0.030(7) 0.036(7) 0.028(6) -0.003(5) 0.001(5) 0.009(6) C4 0.039(10) 0.036(8) 0.033(8) -0.001(6) 0.009(7) -0.020(7) N5 0.055(9) 0.034(7) 0.025(6) -0.005(5) -0.008(6) 0.004(6) C5 0.034(9) 0.019(7) 0.038(8) -0.003(6) -0.006(7) -0.003(6) N6 0.062(10) 0.036(7) 0.026(6) -0.003(5) -0.003(6) 0.006(7) C6 0.029(9) 0.030(8) 0.036(8) 0.008(6) 0.001(7) -0.006(6) N7 0.025(7) 0.031(6) 0.034(6) -0.007(5) 0.007(5) -0.001(5) C7 0.036(9) 0.030(7) 0.023(7) 0.001(6) 0.003(6) -0.011(6) N8 0.046(9) 0.026(6) 0.043(7) -0.006(5) 0.010(6) 0.003(6) C8 0.039(10) 0.030(8) 0.041(8) -0.003(6) -0.002(7) -0.003(7) N9 0.051(9) 0.035(7) 0.047(7) -0.018(6) -0.005(7) 0.018(7) C9 0.041(11) 0.045(9) 0.044(9) -0.005(7) -0.011(8) 0.002(8) C10 0.049(11) 0.040(8) 0.032(8) 0.007(6) 0.003(7) 0.013(8) C11 0.032(9) 0.031(8) 0.033(7) 0.001(6) -0.019(7) 0.006(6) C12 0.034(9) 0.038(8) 0.027(7) -0.005(6) 0.000(6) -0.002(7) C13 0.047(10) 0.036(8) 0.028(7) -0.001(6) -0.009(7) -0.007(7) C14 0.043(11) 0.056(10) 0.037(8) -0.009(7) 0.003(8) 0.007(8) C15 0.067(15) 0.108(16) 0.065(12) -0.038(11) -0.017(11) -0.004(12) C16 0.040(11) 0.060(12) 0.097(14) 0.000(10) -0.024(10) -0.002(9) C17 0.054(13) 0.064(12) 0.074(12) 0.016(10) 0.000(10) -0.013(10) C18 0.045(10) 0.032(8) 0.027(7) 0.006(6) 0.014(7) 0.005(7) C19 0.064(13) 0.051(10) 0.034(8) -0.002(7) -0.006(8) 0.017(9) C20 0.113(10) 0.103(10) 0.116(10) 0.010(7) -0.017(7) -0.005(7) C21 0.154(14) 0.173(14) 0.159(13) -0.010(7) 0.003(7) -0.001(7) C22 0.074(8) 0.067(8) 0.086(8) -0.011(6) -0.007(6) -0.002(6) C23 0.060(12) 0.020(7) 0.040(8) -0.001(6) -0.009(8) 0.003(8) C24 0.041(10) 0.039(9) 0.058(10) -0.019(8) -0.012(8) 0.013(8) C25 0.13(2) 0.112(17) 0.042(10) -0.031(11) -0.009(11) 0.043(15) C26 0.083(15) 0.032(9) 0.114(16) -0.017(10) -0.051(13) -0.009(9) C27 0.048(11) 0.051(10) 0.056(10) -0.003(8) -0.021(9) -0.008(9) C28 0.028(8) 0.029(7) 0.014(6) -0.003(5) 0.014(6) -0.022(6) C29 0.047(10) 0.027(8) 0.039(8) 0.002(6) 0.017(7) -0.002(7) C30 0.055(11) 0.041(9) 0.035(8) 0.005(7) 0.004(8) -0.003(8) C31 0.055(11) 0.036(8) 0.039(8) 0.014(7) 0.013(8) -0.004(8) C32 0.063(12) 0.039(8) 0.025(7) 0.010(6) 0.003(7) -0.007(8) C33 0.049(11) 0.048(9) 0.035(8) -0.004(7) 0.009(7) -0.009(8) C34 0.063(12) 0.029(8) 0.042(8) 0.002(7) 0.013(8) 0.000(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 Pt1 P1 2.183(3) . ? Pt1 P2 2.358(4) . ? Pt1 P3 2.359(3) . ? Pt1 Pt2 2.6218(8) . ? P1 N1 1.654(12) . ? P1 C13 1.710(13) . ? N1 N2 1.349(14) . ? N1 C7 1.532(16) . ? C1 C6 1.394(18) . ? C1 C2 1.408(19) . ? C1 C7 1.564(17) . ? C48 C42 1.463(8) . ? Pt2 C29 2.145(12) . ? Pt2 C28 2.172(10) . ? Pt2 P2 2.302(4) . ? Pt2 P3 2.304(4) . ? P2 C18 1.702(14) . ? P2 N4 1.706(11) . ? N2 N3 1.328(15) . ? C2 C3 1.416(17) . ? C2 C8 1.508(18) . ? P3 N7 1.702(11) . ? P3 C23 1.712(13) . ? N3 C13 1.345(17) . ? C3 C4 1.408(18) . ? C3 C9 1.500(18) . ? N4 N5 1.376(15) . ? N4 C9 1.461(17) . ? C4 C5 1.394(18) . ? C4 C10 1.505(17) . ? N5 N6 1.291(16) . ? C5 C6 1.389(17) . ? C5 C11 1.513(17) . ? N6 C18 1.336(16) . ? C6 C12 1.508(18) . ? N7 N8 1.328(14) . ? N7 C11 1.491(15) . ? N8 N9 1.302(16) . ? N9 C23 1.330(19) . ? C13 C14 1.53(2) . ? C14 C16 1.51(2) . ? C14 C17 1.54(2) . ? C14 C15 1.55(2) . ? C18 C19 1.53(2) . ? C19 C22 1.52(2) . ? C19 C21 1.56(3) . ? C19 C20 1.59(2) . ? C23 C24 1.55(2) . ? C24 C25 1.51(2) . ? C24 C26 1.53(2) . ? C24 C27 1.59(2) . ? C28 C29 1.404(17) . ? C28 C32 1.54(2) . ? C29 C30 1.50(2) . ? C30 C34 1.544(18) . ? C30 C31 1.57(2) . ? C31 C32 1.546(19) . ? C32 C33 1.564(19) . ? C33 C34 1.568(18) . ? C35 C36 1.374(10) . ? C35 C40 1.376(10) . ? C35 C41 1.470(8) . ? C36 C37 1.403(9) . ? C37 C38 1.392(9) . ? C38 C39 1.386(9) . ? C39 C40 1.403(9) . ? C42 C43 1.363(8) . ? C42 C47 1.376(8) . ? C43 C44 1.403(9) . ? C44 C45 1.400(9) . ? C45 C46 1.390(9) . ? C46 C47 1.405(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 126.01(13) . . ? P1 Pt1 P3 124.65(13) . . ? P2 Pt1 P3 108.94(12) . . ? P1 Pt1 Pt2 178.61(10) . . ? P2 Pt1 Pt2 54.74(9) . . ? P3 Pt1 Pt2 54.79(9) . . ? N1 P1 C13 88.0(6) . . ? N1 P1 Pt1 128.1(4) . . ? C13 P1 Pt1 143.7(5) . . ? N2 N1 C7 111.8(10) . . ? N2 N1 P1 117.6(8) . . ? C7 N1 P1 130.6(8) . . ? C6 C1 C2 123.7(12) . . ? C6 C1 C7 117.7(12) . . ? C2 C1 C7 118.7(12) . . ? C29 Pt2 C28 38.0(5) . . ? C29 Pt2 P2 140.4(4) . . ? C28 Pt2 P2 102.7(3) . . ? C29 Pt2 P3 106.7(4) . . ? C28 Pt2 P3 144.1(4) . . ? P2 Pt2 P3 112.94(13) . . ? C29 Pt2 Pt1 161.5(3) . . ? C28 Pt2 Pt1 159.1(3) . . ? P2 Pt2 Pt1 56.79(9) . . ? P3 Pt2 Pt1 56.79(9) . . ? C18 P2 N4 87.2(6) . . ? C18 P2 Pt2 135.3(5) . . ? N4 P2 Pt2 120.4(4) . . ? C18 P2 Pt1 127.5(5) . . ? N4 P2 Pt1 123.3(4) . . ? Pt2 P2 Pt1 68.47(10) . . ? N3 N2 N1 107.1(10) . . ? C1 C2 C3 116.1(12) . . ? C1 C2 C8 122.0(12) . . ? C3 C2 C8 121.9(12) . . ? N7 P3 C23 85.4(7) . . ? N7 P3 Pt2 124.8(4) . . ? C23 P3 Pt2 135.5(6) . . ? N7 P3 Pt1 118.6(4) . . ? C23 P3 Pt1 129.4(5) . . ? Pt2 P3 Pt1 68.42(10) . . ? N2 N3 C13 117.0(11) . . ? C4 C3 C2 121.8(12) . . ? C4 C3 C9 120.2(12) . . ? C2 C3 C9 116.7(12) . . ? N5 N4 C9 117.9(11) . . ? N5 N4 P2 113.2(9) . . ? C9 N4 P2 128.9(9) . . ? C5 C4 C3 118.5(12) . . ? C5 C4 C10 121.2(12) . . ? C3 C4 C10 120.3(12) . . ? N6 N5 N4 111.6(10) . . ? C6 C5 C4 122.1(12) . . ? C6 C5 C11 119.2(12) . . ? C4 C5 C11 118.3(12) . . ? N5 N6 C18 114.3(12) . . ? C5 C6 C1 117.7(13) . . ? C5 C6 C12 119.4(12) . . ? C1 C6 C12 122.7(11) . . ? N8 N7 C11 115.7(11) . . ? N8 N7 P3 114.9(9) . . ? C11 N7 P3 129.4(9) . . ? N1 C7 C1 108.0(10) . . ? N9 N8 N7 112.7(11) . . ? N8 N9 C23 112.1(11) . . ? N4 C9 C3 110.7(10) . . ? N7 C11 C5 111.1(10) . . ? N3 C13 C14 119.8(12) . . ? N3 C13 P1 110.2(10) . . ? C14 C13 P1 129.5(11) . . ? C16 C14 C13 110.4(13) . . ? C16 C14 C17 111.0(14) . . ? C13 C14 C17 109.8(12) . . ? C16 C14 C15 110.7(14) . . ? C13 C14 C15 105.6(13) . . ? C17 C14 C15 109.3(14) . . ? N6 C18 C19 118.0(12) . . ? N6 C18 P2 113.6(11) . . ? C19 C18 P2 127.9(10) . . ? C22 C19 C18 112.7(13) . . ? C22 C19 C21 108.6(18) . . ? C18 C19 C21 105.6(15) . . ? C22 C19 C20 106.2(13) . . ? C18 C19 C20 107.5(15) . . ? C21 C19 C20 116.4(18) . . ? N9 C23 C24 117.3(12) . . ? N9 C23 P3 114.8(11) . . ? C24 C23 P3 127.9(12) . . ? C25 C24 C26 111.2(14) . . ? C25 C24 C23 111.0(15) . . ? C26 C24 C23 108.9(12) . . ? C25 C24 C27 107.0(13) . . ? C26 C24 C27 108.8(14) . . ? C23 C24 C27 109.9(11) . . ? C29 C28 C32 107.5(11) . . ? C29 C28 Pt2 70.0(7) . . ? C32 C28 Pt2 115.6(8) . . ? C28 C29 C30 108.1(13) . . ? C28 C29 Pt2 72.1(7) . . ? C30 C29 Pt2 117.8(9) . . ? C29 C30 C34 105.1(11) . . ? C29 C30 C31 101.0(12) . . ? C34 C30 C31 97.7(11) . . ? C32 C31 C30 96.9(11) . . ? C28 C32 C31 101.2(11) . . ? C28 C32 C33 102.4(11) . . ? C31 C32 C33 96.1(11) . . ? C32 C33 C34 105.3(11) . . ? C30 C34 C33 103.2(11) . . ? C36 C35 C40 123.4(10) . . ? C36 C35 C41 117.2(9) . . ? C40 C35 C41 117.1(9) . . ? C35 C36 C37 118.3(10) . . ? C38 C37 C36 118.7(8) . . ? C39 C38 C37 120.8(9) . . ? C38 C39 C40 118.8(8) . . ? C35 C40 C39 117.9(10) . . ? C43 C42 C47 123.3(7) . . ? C43 C42 C48 118.8(8) . . ? C47 C42 C48 117.9(8) . . ? C42 C43 C44 119.2(7) . . ? C45 C44 C43 117.9(8) . . ? C46 C45 C44 120.1(9) . . ? C45 C46 C47 118.1(9) . . ? C42 C47 C46 117.4(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.908 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.240