# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Tristram Chivers' 'Jamie S Ritch' 'Stuart D. Robertson' _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Palladium and platinum complexes of tellurium-containing imidodiphosphinate ligands: nucleophilic attack of Li[(PiPr2)(TePiPr2)N] on coordinated 1,5-cyclooctadiene ; # Attachment 'Crystallographic_Data.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 735944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pd Te4' _chemical_formula_sum 'C24 H56 N2 P4 Pd Te4' _chemical_formula_weight 1113.39 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 9.6389(4) _cell_length_b 9.9764(4) _cell_length_c 10.1102(3) _cell_angle_alpha 78.098(2) _cell_angle_beta 84.617(3) _cell_angle_gamma 88.695(2) _cell_volume 947.11(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12123 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15850 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.40 _reflns_number_total 4270 _reflns_number_gt 3355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0250P)^2^+0.4918P] 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 4270 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Pd1 Pd 0.5000 0.5000 1.0000 0.02285(11) Uani 1 2 d S . . Te1 Te 0.67086(3) 0.68016(3) 1.04587(3) 0.02758(8) Uani 1 1 d . . . Te2 Te 0.60877(3) 0.47137(3) 0.76139(3) 0.02824(9) Uani 1 1 d . . . P1 P 0.79590(11) 0.80387(11) 0.83365(10) 0.0258(2) Uani 1 1 d . . . P2 P 0.63131(11) 0.70780(11) 0.63966(10) 0.0238(2) Uani 1 1 d . . . N1 N 0.7346(4) 0.8047(3) 0.6918(3) 0.0281(8) Uani 1 1 d . . . C10 C 0.9780(4) 0.7455(5) 0.8286(4) 0.0355(11) Uani 1 1 d . . . H10A H 1.0299 0.8026 0.7469 0.043 Uiso 1 1 calc R . . C11 C 1.0463(5) 0.7659(6) 0.9540(5) 0.0475(13) Uani 1 1 d . . . H11A H 1.1398 0.7250 0.9535 0.071 Uiso 1 1 calc R . . H11B H 0.9896 0.7217 1.0363 0.071 Uiso 1 1 calc R . . H11C H 1.0534 0.8641 0.9524 0.071 Uiso 1 1 calc R . . C12 C 0.9888(5) 0.5969(5) 0.8137(5) 0.0451(12) Uani 1 1 d . . . H12A H 1.0868 0.5683 0.8107 0.068 Uiso 1 1 calc R . . H12B H 0.9505 0.5877 0.7296 0.068 Uiso 1 1 calc R . . H12C H 0.9360 0.5388 0.8913 0.068 Uiso 1 1 calc R . . C20 C 0.8039(5) 0.9835(4) 0.8502(4) 0.0349(11) Uani 1 1 d . . . H20A H 0.8393 0.9848 0.9398 0.042 Uiso 1 1 calc R . . C21 C 0.9038(6) 1.0680(5) 0.7395(5) 0.0531(14) Uani 1 1 d . . . H21A H 0.9000 1.1641 0.7483 0.080 Uiso 1 1 calc R . . H21B H 0.8765 1.0613 0.6501 0.080 Uiso 1 1 calc R . . H21C H 0.9989 1.0329 0.7490 0.080 Uiso 1 1 calc R . . C22 C 0.6606(6) 1.0483(5) 0.8495(6) 0.0534(14) Uani 1 1 d . . . H22A H 0.6669 1.1426 0.8625 0.080 Uiso 1 1 calc R . . H22B H 0.5984 0.9956 0.9232 0.080 Uiso 1 1 calc R . . H22C H 0.6236 1.0489 0.7624 0.080 Uiso 1 1 calc R . . C30 C 0.4578(4) 0.7888(5) 0.6288(4) 0.0300(10) Uani 1 1 d . . . H30A H 0.4722 0.8841 0.5746 0.036 Uiso 1 1 calc R . . C31 C 0.3590(5) 0.7183(6) 0.5555(5) 0.0499(13) Uani 1 1 d . . . H31A H 0.2710 0.7693 0.5489 0.075 Uiso 1 1 calc R . . H31B H 0.3410 0.6246 0.6064 0.075 Uiso 1 1 calc R . . H31C H 0.4015 0.7156 0.4641 0.075 Uiso 1 1 calc R . . C32 C 0.3899(5) 0.8017(5) 0.7688(4) 0.0365(11) Uani 1 1 d . . . H32A H 0.3051 0.8574 0.7581 0.055 Uiso 1 1 calc R . . H32B H 0.4552 0.8455 0.8153 0.055 Uiso 1 1 calc R . . H32C H 0.3661 0.7104 0.8226 0.055 Uiso 1 1 calc R . . C40 C 0.6971(4) 0.7014(4) 0.4648(4) 0.0282(9) Uani 1 1 d . . . H40A H 0.6313 0.6450 0.4284 0.034 Uiso 1 1 calc R . . C41 C 0.6997(5) 0.8470(5) 0.3761(4) 0.0379(11) Uani 1 1 d . . . H41A H 0.7443 0.8445 0.2855 0.057 Uiso 1 1 calc R . . H41B H 0.7523 0.9076 0.4178 0.057 Uiso 1 1 calc R . . H41C H 0.6041 0.8814 0.3686 0.057 Uiso 1 1 calc R . . C42 C 0.8402(5) 0.6363(5) 0.4566(4) 0.0366(11) Uani 1 1 d . . . H42A H 0.8707 0.6342 0.3618 0.055 Uiso 1 1 calc R . . H42B H 0.8363 0.5426 0.5106 0.055 Uiso 1 1 calc R . . H42C H 0.9064 0.6899 0.4922 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 Pd1 0.0264(2) 0.0208(2) 0.0211(2) -0.00372(17) -0.00127(18) -0.00292(18) Te1 0.03063(16) 0.02874(16) 0.02412(14) -0.00666(11) -0.00190(11) -0.00683(12) Te2 0.03736(18) 0.02194(15) 0.02508(15) -0.00574(11) 0.00177(12) -0.00336(12) P1 0.0236(6) 0.0276(6) 0.0275(6) -0.0096(5) 0.0008(4) -0.0044(5) P2 0.0262(6) 0.0218(6) 0.0227(5) -0.0040(4) 0.0006(4) -0.0024(4) N1 0.030(2) 0.028(2) 0.0274(18) -0.0090(15) -0.0002(15) -0.0057(16) C10 0.024(2) 0.050(3) 0.034(2) -0.013(2) -0.0003(19) -0.003(2) C11 0.031(3) 0.062(4) 0.054(3) -0.016(3) -0.009(2) -0.010(2) C12 0.039(3) 0.055(3) 0.046(3) -0.021(2) -0.009(2) 0.015(2) C20 0.045(3) 0.031(3) 0.032(2) -0.015(2) 0.002(2) -0.014(2) C21 0.059(4) 0.040(3) 0.058(3) -0.010(2) 0.011(3) -0.025(3) C22 0.062(4) 0.021(3) 0.074(4) -0.011(2) 0.014(3) -0.002(2) C30 0.029(2) 0.034(3) 0.027(2) -0.0055(18) -0.0030(18) 0.0011(19) C31 0.035(3) 0.063(4) 0.059(3) -0.024(3) -0.015(2) 0.006(3) C32 0.033(3) 0.038(3) 0.035(2) -0.002(2) 0.002(2) 0.005(2) C40 0.033(2) 0.032(2) 0.021(2) -0.0073(17) -0.0018(17) -0.0067(19) C41 0.048(3) 0.036(3) 0.028(2) -0.005(2) 0.000(2) -0.005(2) C42 0.038(3) 0.044(3) 0.028(2) -0.011(2) 0.005(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Te1 2.6038(3) 2_667 ? Pd1 Te1 2.6038(3) . ? Pd1 Te2 2.6070(3) . ? Pd1 Te2 2.6070(3) 2_667 ? Te1 P1 2.4636(14) . ? Te2 P2 2.4293(13) . ? P1 N1 1.599(4) . ? P1 C10 1.836(5) . ? P1 C20 1.838(4) . ? P2 N1 1.599(4) . ? P2 C40 1.835(4) . ? P2 C30 1.843(4) . ? C10 C12 1.521(6) . ? C10 C11 1.534(6) . ? C20 C22 1.512(7) . ? C20 C21 1.529(6) . ? C30 C31 1.527(6) . ? C30 C32 1.531(6) . ? C40 C42 1.515(6) . ? C40 C41 1.540(6) . ? 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 Te1 Pd1 Te1 180.0 2_667 . ? Te1 Pd1 Te2 80.49(3) 2_667 . ? Te1 Pd1 Te2 99.51(1) . . ? Te1 Pd1 Te2 99.51(1) 2_667 2_667 ? Te1 Pd1 Te2 80.49(3) . 2_667 ? Te2 Pd1 Te2 180.000(1) . 2_667 ? P1 Te1 Pd1 111.47(4) . . ? P2 Te2 Pd1 101.91(4) . . ? N1 P1 C10 110.34(19) . . ? N1 P1 C20 106.7(2) . . ? C10 P1 C20 104.7(2) . . ? N1 P1 Te1 119.60(13) . . ? C10 P1 Te1 108.35(16) . . ? C20 P1 Te1 106.02(14) . . ? N1 P2 C40 106.71(19) . . ? N1 P2 C30 109.58(19) . . ? C40 P2 C30 105.89(19) . . ? N1 P2 Te2 117.80(14) . . ? C40 P2 Te2 106.22(14) . . ? C30 P2 Te2 109.90(15) . . ? P2 N1 P1 134.7(2) . . ? C12 C10 C11 111.0(4) . . ? C12 C10 P1 111.0(3) . . ? C11 C10 P1 111.3(3) . . ? C22 C20 C21 110.1(4) . . ? C22 C20 P1 111.0(3) . . ? C21 C20 P1 112.2(3) . . ? C31 C30 C32 110.4(4) . . ? C31 C30 P2 113.7(3) . . ? C32 C30 P2 111.7(3) . . ? C42 C40 C41 110.3(4) . . ? C42 C40 P2 112.3(3) . . ? C41 C40 P2 109.8(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.819 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.238 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 735945' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pt Te4' _chemical_formula_sum 'C24 H56 N2 P4 Pt Te4' _chemical_formula_weight 1202.08 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' Te Te -0.5308 1.6751 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.6125(1) _cell_length_b 14.5167(2) _cell_length_c 24.7377(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3811.05(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 6.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.287 _exptl_absorpt_correction_T_max 0.512 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) _exptl_special_details ; _diffrn_ambient_temperature 173(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 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59738 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.10 _reflns_number_total 9203 _reflns_number_gt 8126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0411P)^2^+3.9031P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(4) _refine_ls_number_reflns 9203 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.96584(2) 0.946320(17) 0.107052(10) 0.02106(6) Uani 1 1 d . . . Te1 Te 0.89362(4) 1.04150(3) 0.023737(17) 0.02886(11) Uani 1 1 d . . . Te2 Te 1.20147(4) 0.99617(3) 0.106557(17) 0.02546(9) Uani 1 1 d . . . P1 P 1.07282(16) 1.07403(11) -0.03669(6) 0.0218(3) Uani 1 1 d . . . P2 P 1.25961(14) 0.95328(12) 0.01462(6) 0.0196(3) Uani 1 1 d . . . N1 N 1.1953(5) 1.0102(4) -0.03345(19) 0.0231(11) Uani 1 1 d . . . C10 C 1.0127(6) 1.0619(4) -0.1063(3) 0.0278(14) Uani 1 1 d . . . H10A H 1.0824 1.0804 -0.1312 0.033 Uiso 1 1 calc R . . C11 C 0.9013(8) 1.1263(6) -0.1177(3) 0.043(2) Uani 1 1 d . . . H11A H 0.8776 1.1216 -0.1559 0.065 Uiso 1 1 calc R . . H11B H 0.9255 1.1899 -0.1095 0.065 Uiso 1 1 calc R . . H11C H 0.8295 1.1085 -0.0950 0.065 Uiso 1 1 calc R . . C12 C 0.9815(8) 0.9616(5) -0.1186(3) 0.0401(18) Uani 1 1 d . . . H12A H 0.9518 0.9563 -0.1559 0.060 Uiso 1 1 calc R . . H12B H 0.9156 0.9402 -0.0939 0.060 Uiso 1 1 calc R . . H12C H 1.0572 0.9238 -0.1138 0.060 Uiso 1 1 calc R . . C20 C 1.1128(8) 1.1973(5) -0.0318(3) 0.0320(16) Uani 1 1 d . . . H20A H 1.0338 1.2330 -0.0386 0.038 Uiso 1 1 calc R . . C21 C 1.2072(9) 1.2245(6) -0.0751(3) 0.047(2) Uani 1 1 d . . . H21A H 1.2368 1.2874 -0.0683 0.071 Uiso 1 1 calc R . . H21B H 1.1668 1.2216 -0.1107 0.071 Uiso 1 1 calc R . . H21C H 1.2789 1.1820 -0.0742 0.071 Uiso 1 1 calc R . . C22 C 1.1593(8) 1.2231(5) 0.0245(3) 0.0432(19) Uani 1 1 d . . . H22A H 1.1709 1.2900 0.0267 0.065 Uiso 1 1 calc R . . H22B H 1.2398 1.1923 0.0316 0.065 Uiso 1 1 calc R . . H22C H 1.0972 1.2037 0.0515 0.065 Uiso 1 1 calc R . . C30 C 1.4312(6) 0.9704(5) 0.0110(3) 0.0262(15) Uani 1 1 d . . . H30A H 1.4710 0.9316 0.0397 0.031 Uiso 1 1 calc R . . C31 C 1.4834(7) 0.9399(6) -0.0429(3) 0.0420(19) Uani 1 1 d . . . H31A H 1.5752 0.9470 -0.0429 0.063 Uiso 1 1 calc R . . H31B H 1.4470 0.9778 -0.0717 0.063 Uiso 1 1 calc R . . H31C H 1.4618 0.8751 -0.0491 0.063 Uiso 1 1 calc R . . C32 C 1.4661(7) 1.0709(5) 0.0223(3) 0.0373(17) Uani 1 1 d . . . H32A H 1.5581 1.0771 0.0233 0.056 Uiso 1 1 calc R . . H32B H 1.4308 1.0897 0.0572 0.056 Uiso 1 1 calc R . . H32C H 1.4319 1.1102 -0.0064 0.056 Uiso 1 1 calc R . . C40 C 1.2336(6) 0.8295(4) 0.0038(3) 0.0258(14) Uani 1 1 d . . . H40A H 1.2747 0.8136 -0.0314 0.031 Uiso 1 1 calc R . . C41 C 1.0966(7) 0.8053(5) -0.0019(3) 0.0331(16) Uani 1 1 d . . . H41A H 1.0887 0.7410 -0.0136 0.050 Uiso 1 1 calc R . . H41B H 1.0575 0.8457 -0.0288 0.050 Uiso 1 1 calc R . . H41C H 1.0543 0.8132 0.0330 0.050 Uiso 1 1 calc R . . C42 C 1.2960(8) 0.7702(5) 0.0466(3) 0.0377(18) Uani 1 1 d . . . H42A H 1.2863 0.7051 0.0370 0.057 Uiso 1 1 calc R . . H42B H 1.2561 0.7817 0.0817 0.057 Uiso 1 1 calc R . . H42C H 1.3858 0.7855 0.0487 0.057 Uiso 1 1 calc R . . Te3 Te 0.73261(4) 0.89199(3) 0.101705(17) 0.02765(10) Uani 1 1 d . . . Te4 Te 1.04230(4) 0.85861(4) 0.192517(18) 0.03300(11) Uani 1 1 d . . . P3 P 0.65464(15) 0.90258(12) 0.19394(7) 0.0224(3) Uani 1 1 d . . . P4 P 0.86176(16) 0.79590(13) 0.24297(7) 0.0251(4) Uani 1 1 d . . . N2 N 0.7285(5) 0.8458(4) 0.2397(2) 0.0296(13) Uani 1 1 d . . . C50 C 0.4903(6) 0.8622(5) 0.1916(3) 0.0270(14) Uani 1 1 d . . . H50A H 0.4435 0.9010 0.1650 0.032 Uiso 1 1 calc R . . C51 C 0.4829(8) 0.7612(5) 0.1728(3) 0.0404(18) Uani 1 1 d . . . H51A H 0.3945 0.7420 0.1710 0.061 Uiso 1 1 calc R . . H51B H 0.5282 0.7219 0.1985 0.061 Uiso 1 1 calc R . . H51C H 0.5213 0.7555 0.1369 0.061 Uiso 1 1 calc R . . C52 C 0.4259(7) 0.8728(6) 0.2471(3) 0.0418(19) Uani 1 1 d . . . H52A H 0.3390 0.8502 0.2448 0.063 Uiso 1 1 calc R . . H52B H 0.4255 0.9379 0.2575 0.063 Uiso 1 1 calc R . . H52C H 0.4722 0.8370 0.2742 0.063 Uiso 1 1 calc R . . C60 C 0.6439(7) 1.0244(5) 0.2140(3) 0.0330(16) Uani 1 1 d . . . H60A H 0.6029 1.0256 0.2504 0.040 Uiso 1 1 calc R . . C61 C 0.5616(9) 1.0827(6) 0.1768(4) 0.052(2) Uani 1 1 d . . . H61A H 0.5588 1.1461 0.1902 0.078 Uiso 1 1 calc R . . H61B H 0.4761 1.0572 0.1759 0.078 Uiso 1 1 calc R . . H61C H 0.5971 1.0821 0.1402 0.078 Uiso 1 1 calc R . . C62 C 0.7742(8) 1.0661(6) 0.2211(4) 0.049(2) Uani 1 1 d . . . H62A H 0.7664 1.1290 0.2349 0.074 Uiso 1 1 calc R . . H62B H 0.8176 1.0672 0.1861 0.074 Uiso 1 1 calc R . . H62C H 0.8228 1.0288 0.2467 0.074 Uiso 1 1 calc R . . C70 C 0.9041(7) 0.7984(6) 0.3153(3) 0.0370(18) Uani 1 1 d . . . H70A H 0.8305 0.7731 0.3357 0.044 Uiso 1 1 calc R . . C71 C 0.9232(9) 0.8974(7) 0.3344(3) 0.059(3) Uani 1 1 d . . . H71A H 0.9386 0.8978 0.3734 0.089 Uiso 1 1 calc R . . H71B H 0.8476 0.9336 0.3263 0.089 Uiso 1 1 calc R . . H71C H 0.9958 0.9243 0.3156 0.089 Uiso 1 1 calc R . . C72 C 1.0183(8) 0.7371(9) 0.3287(3) 0.066(3) Uani 1 1 d . . . H72A H 1.0389 0.7431 0.3671 0.099 Uiso 1 1 calc R . . H72B H 1.0907 0.7565 0.3069 0.099 Uiso 1 1 calc R . . H72C H 0.9980 0.6727 0.3206 0.099 Uiso 1 1 calc R . . C80 C 0.8522(10) 0.6728(6) 0.2264(4) 0.054(2) Uani 1 1 d . . . H80A H 0.9348 0.6450 0.2370 0.065 Uiso 1 1 calc R . . C81 C 0.8343(12) 0.6522(7) 0.1687(4) 0.073(3) Uani 1 1 d . . . H81A H 0.8263 0.5854 0.1637 0.110 Uiso 1 1 calc R . . H81B H 0.9070 0.6747 0.1481 0.110 Uiso 1 1 calc R . . H81C H 0.7576 0.6826 0.1557 0.110 Uiso 1 1 calc R . . C82 C 0.7501(11) 0.6244(7) 0.2607(4) 0.067(3) Uani 1 1 d . . . H82A H 0.7478 0.5587 0.2515 0.101 Uiso 1 1 calc R . . H82B H 0.6678 0.6521 0.2531 0.101 Uiso 1 1 calc R . . H82C H 0.7700 0.6315 0.2991 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01861(11) 0.02805(12) 0.01652(10) 0.00021(10) -0.00063(9) 0.00423(9) Te1 0.0231(2) 0.0391(3) 0.0244(2) 0.00880(19) 0.00086(17) 0.0114(2) Te2 0.02153(19) 0.0357(2) 0.01919(19) -0.00253(19) -0.00374(17) -0.00115(17) P1 0.0241(8) 0.0214(8) 0.0200(8) 0.0021(6) -0.0027(6) 0.0030(6) P2 0.0186(7) 0.0210(8) 0.0194(7) 0.0024(7) -0.0015(6) -0.0001(7) N1 0.021(3) 0.031(3) 0.018(3) 0.002(2) -0.004(2) 0.006(2) C10 0.025(3) 0.034(4) 0.025(3) 0.002(3) -0.010(3) 0.001(3) C11 0.048(5) 0.051(5) 0.032(4) 0.010(3) -0.008(3) 0.014(4) C12 0.053(5) 0.042(4) 0.025(4) -0.006(3) -0.013(3) -0.002(4) C20 0.043(4) 0.021(3) 0.032(4) 0.003(3) -0.006(3) -0.004(3) C21 0.056(5) 0.034(4) 0.053(5) 0.011(4) 0.003(4) -0.015(4) C22 0.047(5) 0.026(4) 0.057(5) -0.004(4) -0.011(4) -0.001(3) C30 0.017(3) 0.033(4) 0.028(3) 0.011(3) -0.005(2) 0.000(3) C31 0.029(4) 0.050(5) 0.047(4) 0.005(4) 0.007(3) 0.001(4) C32 0.026(4) 0.036(4) 0.049(4) 0.007(3) -0.003(3) -0.011(3) C40 0.029(3) 0.024(3) 0.025(3) -0.003(3) 0.007(3) 0.004(3) C41 0.039(4) 0.024(4) 0.036(4) 0.001(3) -0.003(3) -0.004(3) C42 0.039(4) 0.031(4) 0.044(4) 0.011(3) 0.004(3) 0.014(3) Te3 0.0201(2) 0.0434(3) 0.0195(2) -0.00172(19) -0.00286(16) 0.00111(18) Te4 0.0196(2) 0.0533(3) 0.0261(2) 0.0146(2) -0.00145(18) 0.0045(2) P3 0.0175(8) 0.0280(9) 0.0215(8) 0.0023(7) -0.0014(6) 0.0004(7) P4 0.0232(8) 0.0331(10) 0.0190(8) 0.0058(7) -0.0010(6) 0.0033(7) N2 0.021(3) 0.047(4) 0.021(3) 0.006(3) -0.002(2) 0.001(3) C50 0.018(3) 0.033(4) 0.030(3) 0.006(3) -0.004(3) 0.000(3) C51 0.039(4) 0.037(4) 0.045(4) -0.002(3) -0.003(3) -0.015(4) C52 0.027(4) 0.057(5) 0.041(4) 0.008(4) 0.010(3) -0.002(4) C60 0.035(4) 0.031(4) 0.033(4) 0.000(3) 0.006(3) 0.002(3) C61 0.053(6) 0.034(4) 0.069(6) 0.002(4) -0.004(5) 0.015(4) C62 0.052(5) 0.032(4) 0.064(5) -0.009(4) 0.003(4) -0.012(4) C70 0.026(4) 0.064(5) 0.021(3) 0.009(3) -0.002(3) 0.010(4) C71 0.051(6) 0.094(8) 0.033(4) -0.026(5) -0.003(4) -0.017(5) C72 0.034(5) 0.130(10) 0.035(5) 0.031(5) -0.001(4) 0.025(6) C80 0.073(6) 0.047(5) 0.043(5) 0.001(4) 0.013(5) 0.005(5) C81 0.089(8) 0.052(6) 0.078(7) -0.009(5) 0.004(6) 0.000(6) C82 0.088(8) 0.048(6) 0.064(6) 0.012(5) 0.001(6) -0.017(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 Te1 2.5970(6) . ? Pt1 Te4 2.5980(6) . ? Pt1 Te3 2.6012(7) . ? Pt1 Te2 2.6032(7) . ? Te1 P1 2.4646(18) . ? Te2 P2 2.4373(16) . ? P1 N1 1.599(5) . ? P1 C20 1.843(7) . ? P1 C10 1.844(7) . ? P2 N1 1.601(5) . ? P2 C40 1.838(7) . ? P2 C30 1.840(6) . ? C10 C12 1.524(10) . ? C10 C11 1.533(10) . ? C20 C21 1.519(11) . ? C20 C22 1.525(10) . ? C30 C31 1.511(10) . ? C30 C32 1.530(9) . ? C40 C41 1.502(10) . ? C40 C42 1.516(10) . ? Te3 P3 2.4319(17) . ? Te4 P4 2.4612(18) . ? P3 N2 1.604(6) . ? P3 C60 1.841(7) . ? P3 C50 1.841(7) . ? P4 N2 1.591(6) . ? P4 C80 1.836(9) . ? P4 C70 1.845(7) . ? C50 C52 1.540(10) . ? C50 C51 1.540(10) . ? C60 C62 1.520(11) . ? C60 C61 1.526(11) . ? C70 C71 1.527(13) . ? C70 C72 1.539(11) . ? C80 C81 1.471(13) . ? C80 C82 1.546(13) . ? 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 Te1 Pt1 Te4 177.16(2) . . ? Te1 Pt1 Te3 80.800(16) . . ? Te4 Pt1 Te3 100.951(18) . . ? Te1 Pt1 Te2 97.577(17) . . ? Te4 Pt1 Te2 80.797(17) . . ? Te3 Pt1 Te2 176.466(16) . . ? P1 Te1 Pt1 110.83(4) . . ? P2 Te2 Pt1 100.17(4) . . ? N1 P1 C20 111.9(3) . . ? N1 P1 C10 105.8(3) . . ? C20 P1 C10 103.5(3) . . ? N1 P1 Te1 119.1(2) . . ? C20 P1 Te1 108.9(3) . . ? C10 P1 Te1 106.3(2) . . ? N1 P2 C40 109.4(3) . . ? N1 P2 C30 108.4(3) . . ? C40 P2 C30 105.9(3) . . ? N1 P2 Te2 117.0(2) . . ? C40 P2 Te2 110.4(2) . . ? C30 P2 Te2 105.1(2) . . ? P1 N1 P2 133.1(3) . . ? C12 C10 C11 112.2(6) . . ? C12 C10 P1 110.6(5) . . ? C11 C10 P1 112.4(5) . . ? C21 C20 C22 111.5(7) . . ? C21 C20 P1 111.0(5) . . ? C22 C20 P1 111.9(5) . . ? C31 C30 C32 110.6(6) . . ? C31 C30 P2 111.4(5) . . ? C32 C30 P2 111.1(5) . . ? C41 C40 C42 110.8(6) . . ? C41 C40 P2 112.8(5) . . ? C42 C40 P2 112.8(5) . . ? P3 Te3 Pt1 104.89(4) . . ? P4 Te4 Pt1 110.54(4) . . ? N2 P3 C60 109.5(3) . . ? N2 P3 C50 108.7(3) . . ? C60 P3 C50 104.8(3) . . ? N2 P3 Te3 117.6(2) . . ? C60 P3 Te3 109.6(2) . . ? C50 P3 Te3 105.9(2) . . ? N2 P4 C80 112.5(4) . . ? N2 P4 C70 104.9(3) . . ? C80 P4 C70 104.4(4) . . ? N2 P4 Te4 119.8(2) . . ? C80 P4 Te4 106.8(3) . . ? C70 P4 Te4 107.2(3) . . ? P4 N2 P3 134.8(4) . . ? C52 C50 C51 110.0(6) . . ? C52 C50 P3 111.2(5) . . ? C51 C50 P3 111.1(5) . . ? C62 C60 C61 111.7(7) . . ? C62 C60 P3 110.9(5) . . ? C61 C60 P3 113.9(6) . . ? C71 C70 C72 111.8(8) . . ? C71 C70 P4 110.5(5) . . ? C72 C70 P4 112.9(6) . . ? C81 C80 C82 110.4(9) . . ? C81 C80 P4 115.0(7) . . ? C82 C80 P4 111.0(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.008 _refine_diff_density_min -2.286 _refine_diff_density_rms 0.353 #===END data_compound-cis7 _database_code_depnum_ccdc_archive 'CCDC 735946' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pd Te2' _chemical_formula_sum 'C24 H56 N2 P4 Pd Te2' _chemical_formula_weight 858.19 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.172(5) _cell_length_b 9.906(2) _cell_length_c 14.318(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.15(3) _cell_angle_gamma 90.00 _cell_volume 3351.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22297 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.44 _exptl_crystal_description rod _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.467 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6651 _exptl_absorpt_correction_T_max 0.9078 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22297 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3819 _reflns_number_gt 3502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0206P)^2^+13.7698P] 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 3819 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.18444(3) 0.2500 0.01581(7) Uani 1 2 d S . . Te1 Te 0.565300(8) -0.019869(19) 0.226489(17) 0.02880(7) Uani 1 1 d . . . N1 N 0.63370(10) 0.2748(2) 0.22938(17) 0.0205(5) Uani 1 1 d . . . C2 C 0.70746(12) 0.0511(3) 0.2336(2) 0.0288(7) Uani 1 1 d . . . H2A H 0.7365 0.1111 0.2146 0.035 Uiso 1 1 calc R . . C5 C 0.63206(14) 0.1334(3) 0.0565(2) 0.0310(7) Uani 1 1 d . . . H5A H 0.6400 0.0407 0.0351 0.037 Uiso 1 1 calc R . . C6 C 0.57268(17) 0.1719(5) 0.0039(2) 0.0476(10) Uani 1 1 d . . . H6A H 0.5710 0.1720 -0.0651 0.071 Uiso 1 1 calc R . . H6B H 0.5634 0.2622 0.0241 0.071 Uiso 1 1 calc R . . H6C H 0.5454 0.1064 0.0189 0.071 Uiso 1 1 calc R . . C3 C 0.71357(15) -0.0885(4) 0.1913(3) 0.0458(10) Uani 1 1 d . . . H3A H 0.7512 -0.1248 0.2186 0.069 Uiso 1 1 calc R . . H3B H 0.7088 -0.0811 0.1218 0.069 Uiso 1 1 calc R . . H3C H 0.6846 -0.1490 0.2065 0.069 Uiso 1 1 calc R . . C4 C 0.6767(2) 0.2285(5) 0.0312(3) 0.0552(11) Uani 1 1 d . . . H4A H 0.6729 0.2308 -0.0383 0.083 Uiso 1 1 calc R . . H4B H 0.7146 0.1959 0.0612 0.083 Uiso 1 1 calc R . . H4C H 0.6713 0.3195 0.0545 0.083 Uiso 1 1 calc R . . C1 C 0.72015(18) 0.0454(5) 0.3417(3) 0.0511(10) Uani 1 1 d . . . H1A H 0.7573 0.0038 0.3647 0.077 Uiso 1 1 calc R . . H1B H 0.6911 -0.0084 0.3629 0.077 Uiso 1 1 calc R . . H1C H 0.7203 0.1371 0.3674 0.077 Uiso 1 1 calc R . . P2 P 0.57910(3) 0.32744(7) 0.27128(5) 0.01656(14) Uani 1 1 d . . . C8 C 0.60228(13) 0.3487(3) 0.4032(2) 0.0255(6) Uani 1 1 d . . . H8A H 0.5809 0.4272 0.4217 0.031 Uiso 1 1 calc R . . C9 C 0.58681(15) 0.2254(4) 0.4565(2) 0.0357(8) Uani 1 1 d . . . H9A H 0.5997 0.2391 0.5255 0.054 Uiso 1 1 calc R . . H9B H 0.6052 0.1450 0.4370 0.054 Uiso 1 1 calc R . . H9C H 0.5457 0.2129 0.4413 0.054 Uiso 1 1 calc R . . C11 C 0.57026(12) 0.5041(3) 0.2283(2) 0.0240(6) Uani 1 1 d . . . H11A H 0.5430 0.5490 0.2620 0.029 Uiso 1 1 calc R . . C7 C 0.66591(15) 0.3800(5) 0.4379(3) 0.0439(9) Uani 1 1 d . . . H7A H 0.6746 0.3900 0.5075 0.066 Uiso 1 1 calc R . . H7B H 0.6751 0.4640 0.4084 0.066 Uiso 1 1 calc R . . H7C H 0.6883 0.3059 0.4197 0.066 Uiso 1 1 calc R . . C12 C 0.54447(16) 0.5077(4) 0.1213(3) 0.0375(8) Uani 1 1 d . . . H12A H 0.5304 0.5988 0.1031 0.056 Uiso 1 1 calc R . . H12B H 0.5131 0.4432 0.1066 0.056 Uiso 1 1 calc R . . H12C H 0.5734 0.4834 0.0855 0.056 Uiso 1 1 calc R . . C10 C 0.62467(14) 0.5868(3) 0.2480(3) 0.0393(8) Uani 1 1 d . . . H10A H 0.6180 0.6736 0.2146 0.059 Uiso 1 1 calc R . . H10B H 0.6544 0.5374 0.2253 0.059 Uiso 1 1 calc R . . H10C H 0.6366 0.6027 0.3169 0.059 Uiso 1 1 calc R . . P1 P 0.63766(3) 0.12740(7) 0.18630(5) 0.01912(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01453(14) 0.01412(14) 0.01948(14) 0.000 0.00515(10) 0.000 Te1 0.02242(11) 0.01507(10) 0.05362(14) -0.00196(8) 0.01867(9) -0.00019(7) N1 0.0189(11) 0.0175(11) 0.0261(12) -0.0028(10) 0.0070(9) -0.0021(9) C2 0.0163(13) 0.0230(15) 0.0479(19) -0.0026(13) 0.0085(13) 0.0005(11) C5 0.0371(17) 0.0303(17) 0.0285(15) -0.0068(13) 0.0136(13) -0.0016(14) C6 0.050(2) 0.061(3) 0.0272(17) -0.0071(17) -0.0012(16) 0.010(2) C3 0.0266(17) 0.0300(19) 0.081(3) -0.0130(19) 0.0127(18) 0.0068(14) C4 0.071(3) 0.060(3) 0.042(2) 0.000(2) 0.028(2) -0.016(2) C1 0.046(2) 0.051(2) 0.048(2) 0.0031(19) -0.0086(18) 0.0223(19) P2 0.0162(3) 0.0151(3) 0.0186(3) -0.0011(3) 0.0041(2) -0.0006(2) C8 0.0268(15) 0.0276(16) 0.0214(13) -0.0048(12) 0.0040(11) 0.0046(12) C9 0.0421(19) 0.043(2) 0.0200(14) 0.0065(14) 0.0024(13) 0.0027(16) C11 0.0195(14) 0.0175(14) 0.0366(16) 0.0011(12) 0.0096(12) 0.0022(11) C7 0.0327(18) 0.061(3) 0.0322(18) -0.0136(17) -0.0055(14) -0.0077(17) C12 0.0396(19) 0.0337(19) 0.0391(18) 0.0139(15) 0.0081(15) -0.0012(15) C10 0.0310(17) 0.0196(16) 0.067(2) 0.0037(16) 0.0105(17) -0.0059(13) P1 0.0160(3) 0.0179(3) 0.0244(3) -0.0028(3) 0.0062(3) -0.0010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.3473(8) . ? Pd1 P2 2.3473(8) 2_655 ? Pd1 Te1 2.6315(5) 2_655 ? Pd1 Te1 2.6315(5) . ? Te1 P1 2.4376(8) . ? N1 P1 1.595(2) . ? N1 P2 1.645(2) . ? C2 C1 1.514(5) . ? C2 C3 1.529(5) . ? C2 P1 1.843(3) . ? C5 C6 1.522(5) . ? C5 C4 1.533(5) . ? C5 P1 1.836(3) . ? P2 C11 1.853(3) . ? P2 C8 1.865(3) . ? C8 C9 1.528(5) . ? C8 C7 1.545(4) . ? C11 C10 1.525(4) . ? C11 C12 1.528(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pd1 P2 105.76(4) . 2_655 ? P2 Pd1 Te1 160.335(19) . 2_655 ? P2 Pd1 Te1 89.24(2) 2_655 2_655 ? P2 Pd1 Te1 89.24(2) . . ? P2 Pd1 Te1 160.335(19) 2_655 . ? Te1 Pd1 Te1 79.45(2) 2_655 . ? P1 Te1 Pd1 92.83(2) . . ? P1 N1 P2 123.30(15) . . ? C1 C2 C3 110.8(3) . . ? C1 C2 P1 111.3(2) . . ? C3 C2 P1 112.5(2) . . ? C6 C5 C4 111.5(3) . . ? C6 C5 P1 111.7(2) . . ? C4 C5 P1 110.7(2) . . ? N1 P2 C11 102.92(13) . . ? N1 P2 C8 108.17(13) . . ? C11 P2 C8 102.66(14) . . ? N1 P2 Pd1 117.08(9) . . ? C11 P2 Pd1 119.55(10) . . ? C8 P2 Pd1 105.21(10) . . ? C9 C8 C7 109.3(3) . . ? C9 C8 P2 111.3(2) . . ? C7 C8 P2 114.5(2) . . ? C10 C11 C12 109.1(3) . . ? C10 C11 P2 114.3(2) . . ? C12 C11 P2 110.5(2) . . ? N1 P1 C5 111.35(14) . . ? N1 P1 C2 110.97(14) . . ? C5 P1 C2 104.58(15) . . ? N1 P1 Te1 110.61(9) . . ? C5 P1 Te1 110.78(11) . . ? C2 P1 Te1 108.36(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.867 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.095 #===END data_compound-trans7 _database_code_depnum_ccdc_archive 'CCDC 735947' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pd Te2' _chemical_formula_sum 'C24 H56 N2 P4 Pd Te2' _chemical_formula_weight 858.19 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7995(18) _cell_length_b 10.319(2) _cell_length_c 10.726(2) _cell_angle_alpha 107.70(3) _cell_angle_beta 109.99(3) _cell_angle_gamma 96.57(3) _cell_volume 845.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11867 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 27.53 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7921 _exptl_absorpt_correction_T_max 0.8672 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11867 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3852 _reflns_number_gt 3670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0181P)^2^+0.8707P] 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 3852 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 Pd1 Pd 0.5000 0.5000 0.5000 0.01586(6) Uani 1 2 d S . . Te1 Te 0.353022(18) 0.296868(14) 0.546698(14) 0.02358(5) Uani 1 1 d . . . P1 P 0.25858(7) 0.13605(6) 0.29887(6) 0.01954(11) Uani 1 1 d . . . C1 C 0.0434(4) -0.0588(3) 0.3333(3) 0.0383(6) Uani 1 1 d . . . H1A H -0.0720 -0.1088 0.3041 0.057 Uiso 1 1 calc R . . H1B H 0.0872 0.0041 0.4335 0.057 Uiso 1 1 calc R . . H1C H 0.1117 -0.1266 0.3218 0.057 Uiso 1 1 calc R . . C2 C 0.0486(3) 0.0269(3) 0.2405(2) 0.0288(5) Uani 1 1 d . . . H2A H 0.0164 -0.0405 0.1410 0.035 Uiso 1 1 calc R . . C3 C -0.0773(3) 0.1169(3) 0.2367(3) 0.0455(7) Uani 1 1 d . . . H3A H -0.1901 0.0563 0.1942 0.068 Uiso 1 1 calc R . . H3B H -0.0688 0.1732 0.1793 0.068 Uiso 1 1 calc R . . H3C H -0.0539 0.1792 0.3340 0.068 Uiso 1 1 calc R . . C4 C 0.3470(5) -0.0817(3) 0.1353(3) 0.0510(8) Uani 1 1 d . . . H4A H 0.4159 -0.1499 0.1325 0.076 Uiso 1 1 calc R . . H4B H 0.3666 -0.0241 0.0820 0.076 Uiso 1 1 calc R . . H4C H 0.2291 -0.1315 0.0921 0.076 Uiso 1 1 calc R . . C5 C 0.3932(3) 0.0128(3) 0.2907(3) 0.0307(5) Uani 1 1 d . . . H5A H 0.3721 -0.0485 0.3426 0.037 Uiso 1 1 calc R . . C6 C 0.5779(3) 0.0882(3) 0.3633(3) 0.0430(7) Uani 1 1 d . . . H6A H 0.6452 0.0189 0.3582 0.064 Uiso 1 1 calc R . . H6B H 0.6054 0.1444 0.4635 0.064 Uiso 1 1 calc R . . H6C H 0.6017 0.1496 0.3149 0.064 Uiso 1 1 calc R . . N1 N 0.2575(2) 0.21941(19) 0.19646(19) 0.0220(4) Uani 1 1 d . . . P2 P 0.33685(6) 0.38940(6) 0.25474(5) 0.01757(11) Uani 1 1 d . . . C7 C 0.5991(3) 0.3525(3) 0.1683(3) 0.0331(5) Uani 1 1 d . . . H7A H 0.6594 0.3733 0.1122 0.050 Uiso 1 1 calc R . . H7B H 0.5714 0.2511 0.1457 0.050 Uiso 1 1 calc R . . H7C H 0.6694 0.4005 0.2702 0.050 Uiso 1 1 calc R . . C8 C 0.4388(3) 0.4033(2) 0.1323(2) 0.0237(4) Uani 1 1 d . . . H8A H 0.4688 0.5043 0.1452 0.028 Uiso 1 1 calc R . . C9 C 0.3213(3) 0.3205(3) -0.0242(2) 0.0330(5) Uani 1 1 d . . . H9A H 0.3781 0.3309 -0.0861 0.050 Uiso 1 1 calc R . . H9B H 0.2211 0.3566 -0.0475 0.050 Uiso 1 1 calc R . . H9C H 0.2896 0.2211 -0.0391 0.050 Uiso 1 1 calc R . . C10 C 0.0883(3) 0.5054(3) 0.3198(3) 0.0384(6) Uani 1 1 d . . . H10A H -0.0158 0.5340 0.2850 0.058 Uiso 1 1 calc R . . H10B H 0.1704 0.5828 0.4042 0.058 Uiso 1 1 calc R . . H10C H 0.0670 0.4235 0.3449 0.058 Uiso 1 1 calc R . . C11 C 0.1561(3) 0.4679(2) 0.2024(2) 0.0269(5) Uani 1 1 d . . . H11A H 0.0657 0.3944 0.1156 0.032 Uiso 1 1 calc R . . C12 C 0.1908(3) 0.5961(3) 0.1642(3) 0.0347(6) Uani 1 1 d . . . H12A H 0.0921 0.6344 0.1443 0.052 Uiso 1 1 calc R . . H12B H 0.2171 0.5686 0.0796 0.052 Uiso 1 1 calc R . . H12C H 0.2855 0.6675 0.2443 0.052 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 Pd1 0.01659(10) 0.01470(11) 0.01382(10) 0.00439(8) 0.00461(8) 0.00163(8) Te1 0.03034(9) 0.01958(8) 0.01634(8) 0.00489(6) 0.00835(6) -0.00264(6) P1 0.0237(3) 0.0162(3) 0.0173(2) 0.0049(2) 0.0089(2) 0.0009(2) C1 0.0421(15) 0.0344(14) 0.0334(13) 0.0104(11) 0.0173(11) -0.0100(11) C2 0.0290(12) 0.0258(12) 0.0230(11) 0.0039(9) 0.0091(9) -0.0074(9) C3 0.0234(12) 0.0498(18) 0.0563(18) 0.0206(15) 0.0092(12) 0.0002(12) C4 0.087(2) 0.0342(15) 0.0461(17) 0.0123(13) 0.0411(17) 0.0275(16) C5 0.0451(14) 0.0246(12) 0.0350(13) 0.0164(10) 0.0241(11) 0.0143(10) C6 0.0395(15) 0.0537(18) 0.0577(18) 0.0348(15) 0.0276(14) 0.0260(13) N1 0.0282(9) 0.0174(9) 0.0178(8) 0.0057(7) 0.0081(7) 0.0013(7) P2 0.0188(2) 0.0163(3) 0.0148(2) 0.0053(2) 0.00458(19) 0.00180(19) C7 0.0343(13) 0.0363(14) 0.0306(12) 0.0084(11) 0.0190(11) 0.0068(11) C8 0.0304(11) 0.0205(11) 0.0186(10) 0.0064(8) 0.0104(9) 0.0003(9) C9 0.0442(14) 0.0296(13) 0.0180(10) 0.0061(9) 0.0097(10) -0.0017(11) C10 0.0286(13) 0.0433(16) 0.0471(15) 0.0175(13) 0.0166(12) 0.0162(11) C11 0.0220(10) 0.0231(11) 0.0269(11) 0.0087(9) 0.0002(9) 0.0046(9) C12 0.0344(13) 0.0274(13) 0.0359(13) 0.0145(11) 0.0032(11) 0.0106(10) _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 Pd1 P2 2.3455(13) . ? Pd1 P2 2.3455(13) 2_666 ? Pd1 Te1 2.6035(7) 2_666 ? Pd1 Te1 2.6035(7) . ? Te1 P1 2.4501(13) . ? P1 N1 1.5861(19) . ? P1 C5 1.838(3) . ? P1 C2 1.839(2) . ? C1 C2 1.526(3) . ? C2 C3 1.523(4) . ? C4 C5 1.534(4) . ? C5 C6 1.527(4) . ? N1 P2 1.646(2) . ? P2 C8 1.855(2) . ? P2 C11 1.860(2) . ? C7 C8 1.528(3) . ? C8 C9 1.535(3) . ? C10 C11 1.537(4) . ? C11 C12 1.527(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 P2 Pd1 P2 180.0 . 2_666 ? P2 Pd1 Te1 89.98(4) . 2_666 ? P2 Pd1 Te1 90.02(4) 2_666 2_666 ? P2 Pd1 Te1 90.02(4) . . ? P2 Pd1 Te1 89.98(4) 2_666 . ? Te1 Pd1 Te1 180.0 2_666 . ? P1 Te1 Pd1 92.72(3) . . ? N1 P1 C5 111.88(11) . . ? N1 P1 C2 109.88(11) . . ? C5 P1 C2 105.28(12) . . ? N1 P1 Te1 111.12(7) . . ? C5 P1 Te1 108.69(9) . . ? C2 P1 Te1 109.82(9) . . ? C3 C2 C1 111.1(2) . . ? C3 C2 P1 110.47(17) . . ? C1 C2 P1 112.10(18) . . ? C6 C5 C4 111.0(2) . . ? C6 C5 P1 112.05(18) . . ? C4 C5 P1 110.1(2) . . ? P1 N1 P2 123.35(12) . . ? N1 P2 C8 102.49(10) . . ? N1 P2 C11 105.77(11) . . ? C8 P2 C11 103.82(11) . . ? N1 P2 Pd1 116.37(8) . . ? C8 P2 Pd1 116.86(8) . . ? C11 P2 Pd1 110.23(8) . . ? C7 C8 C9 110.1(2) . . ? C7 C8 P2 110.70(15) . . ? C9 C8 P2 111.47(16) . . ? C12 C11 C10 109.4(2) . . ? C12 C11 P2 114.77(17) . . ? C10 C11 P2 110.63(16) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.430 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.078 #===END data_compound-trans7-alternatecell _database_code_depnum_ccdc_archive 'CCDC 735948' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pd Te2' _chemical_formula_sum 'C24 H56 N2 P4 Pd Te2' _chemical_formula_weight 858.19 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7536(18) _cell_length_b 12.623(3) _cell_length_c 15.669(3) _cell_angle_alpha 102.22(3) _cell_angle_beta 91.05(3) _cell_angle_gamma 94.24(3) _cell_volume 1686.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21391 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 2.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32623 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5953 _reflns_number_gt 4590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0565P)^2^+1.9124P] 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 5953 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Pd1 Pd 0.24115(4) 0.25946(3) 0.24186(2) 0.01890(11) Uani 1 1 d . . . Te1 Te 0.13910(4) 0.10766(3) 0.11147(2) 0.03862(13) Uani 1 1 d . . . P1 P 0.24494(13) 0.19785(9) -0.00023(7) 0.0209(3) Uani 1 1 d . . . C1 C 0.1513(6) 0.2281(5) -0.1656(3) 0.0396(13) Uani 1 1 d . . . H1A H 0.0644 0.2294 -0.2057 0.059 Uiso 1 1 calc R . . H1B H 0.2228 0.1772 -0.1948 0.059 Uiso 1 1 calc R . . H1C H 0.2038 0.3011 -0.1487 0.059 Uiso 1 1 calc R . . C2 C 0.0931(5) 0.1917(4) -0.0841(3) 0.0292(11) Uani 1 1 d . . . H2A H 0.0507 0.1142 -0.1025 0.035 Uiso 1 1 calc R . . C3 C -0.0369(6) 0.2584(5) -0.0466(4) 0.0476(15) Uani 1 1 d . . . H3A H -0.1214 0.2480 -0.0902 0.071 Uiso 1 1 calc R . . H3B H -0.0002 0.3355 -0.0311 0.071 Uiso 1 1 calc R . . H3C H -0.0729 0.2348 0.0058 0.071 Uiso 1 1 calc R . . C4 C 0.5121(6) 0.1748(5) -0.0989(4) 0.0459(15) Uani 1 1 d . . . H4A H 0.6028 0.1335 -0.1104 0.069 Uiso 1 1 calc R . . H4B H 0.5426 0.2473 -0.0635 0.069 Uiso 1 1 calc R . . H4C H 0.4647 0.1816 -0.1544 0.069 Uiso 1 1 calc R . . C5 C 0.3978(6) 0.1156(4) -0.0496(3) 0.0316(11) Uani 1 1 d . . . H5A H 0.4577 0.0995 0.0004 0.038 Uiso 1 1 calc R . . C6 C 0.3346(6) 0.0044(4) -0.1038(4) 0.0406(13) Uani 1 1 d . . . H6A H 0.4194 -0.0414 -0.1202 0.061 Uiso 1 1 calc R . . H6B H 0.2811 0.0144 -0.1567 0.061 Uiso 1 1 calc R . . H6C H 0.2629 -0.0307 -0.0690 0.061 Uiso 1 1 calc R . . N1 N 0.3085(4) 0.3190(3) 0.0409(2) 0.0220(8) Uani 1 1 d . . . P2 P 0.32917(12) 0.37103(9) 0.14639(7) 0.0184(3) Uani 1 1 d . . . C7 C 0.6235(5) 0.3110(4) 0.1666(4) 0.0368(13) Uani 1 1 d . . . H7A H 0.7323 0.3332 0.1806 0.055 Uiso 1 1 calc R . . H7B H 0.6124 0.2617 0.1091 0.055 Uiso 1 1 calc R . . H7C H 0.5815 0.2737 0.2109 0.055 Uiso 1 1 calc R . . C8 C 0.5367(5) 0.4115(4) 0.1656(3) 0.0238(10) Uani 1 1 d . . . H8A H 0.5513 0.4610 0.2246 0.029 Uiso 1 1 calc R . . C9 C 0.6038(5) 0.4722(4) 0.0985(3) 0.0317(12) Uani 1 1 d . . . H9A H 0.7124 0.4940 0.1134 0.047 Uiso 1 1 calc R . . H9B H 0.5484 0.5370 0.0989 0.047 Uiso 1 1 calc R . . H9C H 0.5935 0.4244 0.0403 0.047 Uiso 1 1 calc R . . C10 C 0.3050(6) 0.5979(4) 0.2236(3) 0.0363(12) Uani 1 1 d . . . H10A H 0.2478 0.6613 0.2219 0.054 Uiso 1 1 calc R . . H10B H 0.4126 0.6139 0.2112 0.054 Uiso 1 1 calc R . . H10C H 0.2987 0.5808 0.2817 0.054 Uiso 1 1 calc R . . C11 C 0.2364(5) 0.5006(4) 0.1550(3) 0.0255(10) Uani 1 1 d . . . H11A H 0.2466 0.5214 0.0971 0.031 Uiso 1 1 calc R . . C12 C 0.0650(6) 0.4804(4) 0.1676(4) 0.0384(13) Uani 1 1 d . . . H12A H 0.0135 0.5456 0.1637 0.058 Uiso 1 1 calc R . . H12B H 0.0491 0.4635 0.2252 0.058 Uiso 1 1 calc R . . H12C H 0.0224 0.4191 0.1221 0.058 Uiso 1 1 calc R . . Te2 Te 0.33761(4) 0.40792(2) 0.37569(2) 0.02935(12) Uani 1 1 d . . . P3 P 0.25360(13) 0.30512(9) 0.48504(7) 0.0188(3) Uani 1 1 d . . . C13 C 0.1719(6) 0.4903(4) 0.6052(4) 0.0386(13) Uani 1 1 d . . . H13A H 0.0879 0.5337 0.6286 0.058 Uiso 1 1 calc R . . H13B H 0.2368 0.5307 0.5706 0.058 Uiso 1 1 calc R . . H13C H 0.2334 0.4752 0.6535 0.058 Uiso 1 1 calc R . . C14 C 0.1053(5) 0.3820(4) 0.5464(3) 0.0271(11) Uani 1 1 d . . . H14A H 0.0373 0.4025 0.5016 0.033 Uiso 1 1 calc R . . C15 C 0.0022(6) 0.3155(5) 0.5957(4) 0.0443(14) Uani 1 1 d . . . H15A H -0.0892 0.3540 0.6133 0.066 Uiso 1 1 calc R . . H15B H 0.0578 0.3052 0.6478 0.066 Uiso 1 1 calc R . . H15C H -0.0285 0.2445 0.5579 0.066 Uiso 1 1 calc R . . C16 C 0.3676(6) 0.2403(5) 0.6310(4) 0.0479(15) Uani 1 1 d . . . H16A H 0.4574 0.2356 0.6679 0.072 Uiso 1 1 calc R . . H16B H 0.3252 0.1669 0.6029 0.072 Uiso 1 1 calc R . . H16C H 0.2898 0.2783 0.6671 0.072 Uiso 1 1 calc R . . C17 C 0.4145(5) 0.3026(4) 0.5615(3) 0.0261(10) Uani 1 1 d . . . H17A H 0.4453 0.3794 0.5917 0.031 Uiso 1 1 calc R . . C18 C 0.5534(6) 0.2566(5) 0.5141(4) 0.0424(14) Uani 1 1 d . . . H18A H 0.6396 0.2629 0.5562 0.064 Uiso 1 1 calc R . . H18B H 0.5814 0.2975 0.4693 0.064 Uiso 1 1 calc R . . H18C H 0.5286 0.1799 0.4865 0.064 Uiso 1 1 calc R . . N2 N 0.1885(4) 0.1853(3) 0.4390(2) 0.0209(8) Uani 1 1 d . . . P4 P 0.16009(12) 0.14242(9) 0.33401(7) 0.0179(2) Uani 1 1 d . . . C19 C -0.1326(6) 0.2041(5) 0.3189(4) 0.0496(16) Uani 1 1 d . . . H19A H -0.2416 0.1833 0.3043 0.074 Uiso 1 1 calc R . . H19B H -0.0894 0.2435 0.2762 0.074 Uiso 1 1 calc R . . H19C H -0.1213 0.2510 0.3774 0.074 Uiso 1 1 calc R . . C20 C -0.0481(5) 0.1023(4) 0.3168(3) 0.0260(10) Uani 1 1 d . . . H20A H -0.0646 0.0548 0.2571 0.031 Uiso 1 1 calc R . . C21 C -0.1162(6) 0.0402(5) 0.3818(4) 0.0464(15) Uani 1 1 d . . . H21A H -0.2280 0.0312 0.3733 0.070 Uiso 1 1 calc R . . H21B H -0.0893 0.0808 0.4413 0.070 Uiso 1 1 calc R . . H21C H -0.0755 -0.0314 0.3727 0.070 Uiso 1 1 calc R . . C22 C 0.4286(6) 0.0428(5) 0.2998(4) 0.0483(15) Uani 1 1 d . . . H22A H 0.4805 -0.0242 0.2822 0.072 Uiso 1 1 calc R . . H22B H 0.4713 0.0836 0.3565 0.072 Uiso 1 1 calc R . . H22C H 0.4438 0.0873 0.2559 0.072 Uiso 1 1 calc R . . C23 C 0.2573(5) 0.0143(4) 0.3070(3) 0.0283(11) Uani 1 1 d . . . H23A H 0.2169 -0.0265 0.2482 0.034 Uiso 1 1 calc R . . C24 C 0.2318(8) -0.0600(5) 0.3704(5) 0.070(2) Uani 1 1 d . . . H24A H 0.2914 -0.1234 0.3532 0.105 Uiso 1 1 calc R . . H24B H 0.1227 -0.0841 0.3696 0.105 Uiso 1 1 calc R . . H24C H 0.2649 -0.0207 0.4295 0.105 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 Pd1 0.0239(2) 0.0183(2) 0.0135(2) 0.00340(14) -0.00115(14) -0.00435(14) Te1 0.0649(3) 0.0305(2) 0.01560(19) 0.00464(15) -0.00418(16) -0.02580(17) P1 0.0262(6) 0.0212(6) 0.0144(6) 0.0044(5) -0.0023(5) -0.0046(5) C1 0.050(3) 0.047(3) 0.023(3) 0.013(3) -0.006(2) -0.002(3) C2 0.031(3) 0.034(3) 0.021(3) 0.006(2) -0.007(2) -0.010(2) C3 0.031(3) 0.066(4) 0.045(4) 0.011(3) -0.007(3) 0.003(3) C4 0.036(3) 0.047(3) 0.045(4) -0.013(3) 0.011(3) -0.003(2) C5 0.042(3) 0.025(3) 0.025(3) -0.001(2) -0.007(2) 0.002(2) C6 0.052(3) 0.025(3) 0.041(3) -0.001(2) -0.007(3) 0.005(2) N1 0.028(2) 0.023(2) 0.014(2) 0.0062(16) 0.0017(15) -0.0049(16) P2 0.0217(6) 0.0176(6) 0.0154(6) 0.0039(5) -0.0013(4) -0.0029(4) C7 0.026(3) 0.043(3) 0.045(3) 0.018(3) -0.002(2) 0.001(2) C8 0.019(2) 0.027(3) 0.025(3) 0.007(2) -0.0046(18) -0.0063(18) C9 0.023(2) 0.039(3) 0.034(3) 0.013(2) -0.002(2) -0.009(2) C10 0.058(3) 0.023(3) 0.026(3) 0.000(2) 0.001(2) 0.004(2) C11 0.031(3) 0.023(2) 0.025(3) 0.008(2) 0.000(2) 0.0039(19) C12 0.037(3) 0.038(3) 0.040(3) 0.004(3) 0.002(2) 0.012(2) Te2 0.0475(2) 0.02189(19) 0.01595(19) 0.00321(14) -0.00136(14) -0.01222(14) P3 0.0218(6) 0.0188(6) 0.0154(6) 0.0039(5) -0.0008(4) -0.0013(4) C13 0.050(3) 0.028(3) 0.035(3) -0.002(2) 0.007(2) 0.009(2) C14 0.027(2) 0.027(3) 0.026(3) 0.002(2) 0.000(2) 0.004(2) C15 0.040(3) 0.049(4) 0.040(3) 0.001(3) 0.019(3) -0.004(3) C16 0.046(3) 0.064(4) 0.040(3) 0.031(3) -0.009(3) -0.008(3) C17 0.025(2) 0.027(3) 0.024(3) 0.004(2) -0.0079(19) -0.0040(19) C18 0.034(3) 0.053(4) 0.039(3) 0.007(3) -0.005(2) 0.008(3) N2 0.025(2) 0.021(2) 0.017(2) 0.0056(16) 0.0017(15) -0.0021(15) P4 0.0209(6) 0.0166(6) 0.0152(6) 0.0030(5) -0.0002(4) -0.0021(4) C19 0.031(3) 0.048(4) 0.073(5) 0.022(3) -0.005(3) 0.002(3) C20 0.021(2) 0.031(3) 0.024(3) 0.003(2) -0.0036(19) -0.0067(19) C21 0.029(3) 0.061(4) 0.052(4) 0.024(3) 0.002(2) -0.013(3) C22 0.036(3) 0.044(3) 0.059(4) -0.007(3) 0.006(3) 0.015(3) C23 0.037(3) 0.018(2) 0.027(3) 0.000(2) -0.001(2) 0.004(2) C24 0.086(5) 0.059(4) 0.085(5) 0.045(4) 0.039(4) 0.040(4) _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 Pd1 P4 2.3572(13) . ? Pd1 P2 2.3641(13) . ? Pd1 Te2 2.5808(11) . ? Pd1 Te1 2.5820(11) . ? Te1 P1 2.4422(13) . ? P1 N1 1.583(4) . ? P1 C5 1.836(5) . ? P1 C2 1.838(5) . ? C1 C2 1.529(6) . ? C2 C3 1.519(7) . ? C4 C5 1.522(7) . ? C5 C6 1.536(7) . ? N1 P2 1.646(4) . ? P2 C8 1.851(4) . ? P2 C11 1.860(5) . ? C7 C8 1.530(7) . ? C8 C9 1.527(6) . ? C10 C11 1.527(7) . ? C11 C12 1.527(7) . ? Te2 P3 2.4508(13) . ? P3 N2 1.590(4) . ? P3 C17 1.839(4) . ? P3 C14 1.841(5) . ? C13 C14 1.545(7) . ? C14 C15 1.517(7) . ? C16 C17 1.518(7) . ? C17 C18 1.523(7) . ? N2 P4 1.628(4) . ? P4 C20 1.854(4) . ? P4 C23 1.856(5) . ? C19 C20 1.525(7) . ? C20 C21 1.515(7) . ? C22 C23 1.528(7) . ? C23 C24 1.513(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Pd1 P2 177.53(4) . . ? P4 Pd1 Te2 90.58(4) . . ? P2 Pd1 Te2 90.75(4) . . ? P4 Pd1 Te1 87.55(4) . . ? P2 Pd1 Te1 91.14(4) . . ? Te2 Pd1 Te1 178.04(4) . . ? P1 Te1 Pd1 95.11(4) . . ? N1 P1 C5 111.5(2) . . ? N1 P1 C2 111.9(2) . . ? C5 P1 C2 108.3(2) . . ? N1 P1 Te1 111.16(14) . . ? C5 P1 Te1 105.91(16) . . ? C2 P1 Te1 107.72(15) . . ? C3 C2 C1 110.1(4) . . ? C3 C2 P1 110.6(4) . . ? C1 C2 P1 113.1(3) . . ? C4 C5 C6 112.7(4) . . ? C4 C5 P1 114.3(4) . . ? C6 C5 P1 112.2(4) . . ? P1 N1 P2 124.6(2) . . ? N1 P2 C8 105.0(2) . . ? N1 P2 C11 101.4(2) . . ? C8 P2 C11 105.3(2) . . ? N1 P2 Pd1 117.02(13) . . ? C8 P2 Pd1 110.99(15) . . ? C11 P2 Pd1 115.90(16) . . ? C9 C8 C7 110.0(4) . . ? C9 C8 P2 113.2(3) . . ? C7 C8 P2 109.7(3) . . ? C10 C11 C12 110.6(4) . . ? C10 C11 P2 116.6(3) . . ? C12 C11 P2 109.3(3) . . ? P3 Te2 Pd1 95.64(4) . . ? N2 P3 C17 111.1(2) . . ? N2 P3 C14 111.6(2) . . ? C17 P3 C14 108.0(2) . . ? N2 P3 Te2 110.55(14) . . ? C17 P3 Te2 109.49(15) . . ? C14 P3 Te2 105.94(16) . . ? C15 C14 C13 112.3(4) . . ? C15 C14 P3 113.9(3) . . ? C13 C14 P3 112.5(3) . . ? C16 C17 C18 110.8(4) . . ? C16 C17 P3 111.4(3) . . ? C18 C17 P3 111.8(3) . . ? P3 N2 P4 124.5(2) . . ? N2 P4 C20 105.9(2) . . ? N2 P4 C23 104.9(2) . . ? C20 P4 C23 106.1(2) . . ? N2 P4 Pd1 118.31(13) . . ? C20 P4 Pd1 110.65(15) . . ? C23 P4 Pd1 110.29(16) . . ? C21 C20 C19 109.6(4) . . ? C21 C20 P4 114.8(3) . . ? C19 C20 P4 108.8(3) . . ? C24 C23 C22 110.3(5) . . ? C24 C23 P4 114.8(4) . . ? C22 C23 P4 108.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.699 _refine_diff_density_min -2.273 _refine_diff_density_rms 0.249 #===END data_compound-trans8 _database_code_depnum_ccdc_archive 'CCDC 735949' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pt Te2' _chemical_formula_sum 'C24 H56 N2 P4 Pt Te2' _chemical_formula_weight 946.88 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8463(18) _cell_length_b 10.321(2) _cell_length_c 10.669(2) _cell_angle_alpha 107.58(3) _cell_angle_beta 109.89(3) _cell_angle_gamma 96.93(3) _cell_volume 845.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12371 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 6.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.229 _exptl_absorpt_correction_T_max 0.484 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14511 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.34 _reflns_number_total 3759 _reflns_number_gt 3711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0740P)^2^+0.6987P] 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 3759 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.0000 1.0000 1.0000 0.01698(10) Uani 1 2 d S . . Te1 Te 0.14417(4) 1.20392(3) 0.95206(3) 0.02548(11) Uani 1 1 d . . . P1 P 0.24193(14) 1.36551(11) 1.20122(12) 0.0215(2) Uani 1 1 d . . . P2 P 0.16397(13) 1.11024(11) 1.24424(10) 0.0191(2) Uani 1 1 d . . . N1 N 0.2448(5) 1.2807(4) 1.3029(4) 0.0242(8) Uani 1 1 d . . . C5 C 0.0625(6) 1.0964(5) 1.3672(5) 0.0271(9) Uani 1 1 d . . . H5A H 0.0321 0.9952 1.3542 0.033 Uiso 1 1 calc R . . C8 C 0.4502(6) 1.4740(5) 1.2572(5) 0.0315(11) Uani 1 1 d . . . H8A H 0.4832 1.5411 1.3575 0.038 Uiso 1 1 calc R . . C2 C 0.3440(6) 1.0336(5) 1.2984(5) 0.0309(9) Uani 1 1 d . . . H2A H 0.4332 1.1074 1.3862 0.037 Uiso 1 1 calc R . . C6 C -0.0967(7) 1.1468(6) 1.3308(5) 0.0373(11) Uani 1 1 d . . . H6A H -0.1573 1.1254 1.3867 0.056 Uiso 1 1 calc R . . H6B H -0.1663 1.0991 1.2283 0.056 Uiso 1 1 calc R . . H6C H -0.0687 1.2484 1.3540 0.056 Uiso 1 1 calc R . . C11 C 0.1101(7) 1.4887(5) 1.2125(5) 0.0340(10) Uani 1 1 d . . . H11A H 0.1306 1.5504 1.1606 0.041 Uiso 1 1 calc R . . C4 C 0.1800(7) 1.1791(5) 1.5246(5) 0.0361(11) Uani 1 1 d . . . H4A H 0.1220 1.1716 1.5867 0.054 Uiso 1 1 calc R . . H4B H 0.2156 1.2780 1.5388 0.054 Uiso 1 1 calc R . . H4C H 0.2774 1.1405 1.5488 0.054 Uiso 1 1 calc R . . C3 C 0.3087(7) 0.9049(5) 1.3360(6) 0.0386(11) Uani 1 1 d . . . H3A H 0.4075 0.8679 1.3578 0.058 Uiso 1 1 calc R . . H3B H 0.2157 0.8328 1.2545 0.058 Uiso 1 1 calc R . . H3C H 0.2800 0.9314 1.4197 0.058 Uiso 1 1 calc R . . C12 C -0.0740(7) 1.4130(7) 1.1399(7) 0.0478(14) Uani 1 1 d . . . H12A H -0.1404 1.4819 1.1510 0.072 Uiso 1 1 calc R . . H12B H -0.0965 1.3467 1.1843 0.072 Uiso 1 1 calc R . . H12C H -0.1035 1.3620 1.0377 0.072 Uiso 1 1 calc R . . C9 C 0.4540(8) 1.5611(6) 1.1651(6) 0.0432(14) Uani 1 1 d . . . H9A H 0.5694 1.6033 1.1862 0.065 Uiso 1 1 calc R . . H9B H 0.3970 1.6355 1.1864 0.065 Uiso 1 1 calc R . . H9C H 0.3978 1.5007 1.0636 0.065 Uiso 1 1 calc R . . C1 C 0.4132(7) 0.9980(6) 1.1812(6) 0.0415(12) Uani 1 1 d . . . H1A H 0.5194 0.9742 1.2179 0.062 Uiso 1 1 calc R . . H1B H 0.4300 1.0793 1.1537 0.062 Uiso 1 1 calc R . . H1C H 0.3343 0.9179 1.0973 0.062 Uiso 1 1 calc R . . C10 C 0.1566(10) 1.5823(6) 1.3677(7) 0.0560(17) Uani 1 1 d . . . H10A H 0.0847 1.6473 1.3713 0.084 Uiso 1 1 calc R . . H10B H 0.2726 1.6357 1.4092 0.084 Uiso 1 1 calc R . . H10C H 0.1424 1.5241 1.4224 0.084 Uiso 1 1 calc R . . C7 C 0.5756(7) 1.3851(7) 1.2608(7) 0.0499(14) Uani 1 1 d . . . H7A H 0.6868 1.4460 1.2961 0.075 Uiso 1 1 calc R . . H7B H 0.5469 1.3178 1.1639 0.075 Uiso 1 1 calc R . . H7C H 0.5738 1.3342 1.3245 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01888(14) 0.01513(14) 0.01330(14) 0.00434(9) 0.00469(10) -0.00097(9) Te1 0.03397(19) 0.02053(18) 0.01593(17) 0.00515(12) 0.00855(13) -0.00590(13) P1 0.0282(6) 0.0163(5) 0.0179(5) 0.0053(4) 0.0102(4) -0.0019(4) P2 0.0217(5) 0.0170(5) 0.0142(4) 0.0049(4) 0.0046(4) -0.0013(4) N1 0.030(2) 0.0207(18) 0.0149(16) 0.0050(14) 0.0050(15) -0.0034(15) C5 0.036(2) 0.023(2) 0.0172(19) 0.0044(16) 0.0102(18) -0.0039(18) C8 0.035(2) 0.027(2) 0.021(2) 0.0042(18) 0.0090(19) -0.0140(19) C2 0.028(2) 0.027(2) 0.027(2) 0.0084(18) 0.0001(17) 0.0021(17) C6 0.041(3) 0.039(3) 0.034(2) 0.009(2) 0.022(2) 0.003(2) C11 0.054(3) 0.027(2) 0.037(3) 0.019(2) 0.028(2) 0.014(2) C4 0.050(3) 0.032(2) 0.017(2) 0.0058(18) 0.010(2) -0.005(2) C3 0.044(3) 0.029(2) 0.039(3) 0.017(2) 0.006(2) 0.010(2) C12 0.048(3) 0.052(3) 0.067(4) 0.037(3) 0.034(3) 0.025(3) C9 0.048(3) 0.039(3) 0.034(3) 0.009(2) 0.018(2) -0.013(2) C1 0.032(2) 0.049(3) 0.048(3) 0.021(3) 0.016(2) 0.018(2) C10 0.095(5) 0.036(3) 0.047(3) 0.012(3) 0.041(4) 0.023(3) C7 0.029(3) 0.053(3) 0.056(4) 0.020(3) 0.010(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.3296(15) . ? Pt1 P2 2.3296(15) 2_577 ? Pt1 Te1 2.6008(8) 2_577 ? Pt1 Te1 2.6008(7) . ? Te1 P1 2.4505(16) . ? P1 N1 1.582(4) . ? P1 C11 1.831(5) . ? P1 C8 1.832(5) . ? P2 N1 1.651(4) . ? P2 C5 1.853(5) . ? P2 C2 1.858(5) . ? C5 C6 1.527(7) . ? C5 C4 1.537(6) . ? C8 C7 1.520(8) . ? C8 C9 1.525(7) . ? C2 C3 1.526(7) . ? C2 C1 1.540(7) . ? C11 C10 1.522(8) . ? C11 C12 1.527(8) . ? 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 P2 Pt1 P2 180.0 . 2_577 ? P2 Pt1 Te1 90.09(4) . 2_577 ? P2 Pt1 Te1 89.91(4) 2_577 2_577 ? P2 Pt1 Te1 89.91(4) . . ? P2 Pt1 Te1 90.09(4) 2_577 . ? Te1 Pt1 Te1 180.0 2_577 . ? P1 Te1 Pt1 93.08(4) . . ? N1 P1 C11 112.2(2) . . ? N1 P1 C8 109.9(2) . . ? C11 P1 C8 105.4(2) . . ? N1 P1 Te1 110.32(16) . . ? C11 P1 Te1 109.16(18) . . ? C8 P1 Te1 109.78(16) . . ? N1 P2 C5 102.6(2) . . ? N1 P2 C2 105.1(2) . . ? C5 P2 C2 103.7(2) . . ? N1 P2 Pt1 116.59(15) . . ? C5 P2 Pt1 116.30(16) . . ? C2 P2 Pt1 111.17(16) . . ? P1 N1 P2 123.8(2) . . ? C6 C5 C4 110.3(4) . . ? C6 C5 P2 110.7(3) . . ? C4 C5 P2 111.4(3) . . ? C7 C8 C9 111.6(5) . . ? C7 C8 P1 111.0(4) . . ? C9 C8 P1 112.2(4) . . ? C3 C2 C1 109.7(4) . . ? C3 C2 P2 114.6(4) . . ? C1 C2 P2 110.3(3) . . ? C10 C11 C12 111.1(5) . . ? C10 C11 P1 110.8(4) . . ? C12 C11 P1 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.339 _refine_diff_density_min -5.268 _refine_diff_density_rms 0.291 #===END data_compound-trans8-alternatecell _database_code_depnum_ccdc_archive 'CCDC 735950' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N2 P4 Pt Te2' _chemical_formula_sum 'C24 H56 N2 P4 Pt Te2' _chemical_formula_weight 946.88 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7764(18) _cell_length_b 12.625(3) _cell_length_c 15.646(3) _cell_angle_alpha 102.31(3) _cell_angle_beta 91.21(3) _cell_angle_gamma 94.28(3) _cell_volume 1687.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22937 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 6.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26384 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5930 _reflns_number_gt 4199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0264P)^2^+4.0009P] 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 5930 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.25868(3) 0.24127(2) 0.258119(19) 0.02125(10) Uani 1 1 d . . . Te1 Te 0.16282(6) 0.09214(4) 0.12412(3) 0.03185(15) Uani 1 1 d . . . Te2 Te 0.36004(7) 0.39333(5) 0.38917(3) 0.04182(17) Uani 1 1 d . . . P2 P 0.33902(19) 0.35771(15) 0.16670(12) 0.0197(4) Uani 1 1 d . . . P1 P 0.2455(2) 0.19528(15) 0.01473(12) 0.0213(4) Uani 1 1 d . . . P4 P 0.1720(2) 0.13027(15) 0.35253(12) 0.0201(4) Uani 1 1 d . . . P3 P 0.2550(2) 0.30273(16) 0.50063(12) 0.0230(4) Uani 1 1 d . . . N2 N 0.1917(6) 0.1825(5) 0.4581(4) 0.0236(13) Uani 1 1 d . . . N1 N 0.3113(6) 0.3145(5) 0.0610(4) 0.0241(14) Uani 1 1 d . . . C8 C 0.5470(7) 0.3979(6) 0.1834(5) 0.0253(17) Uani 1 1 d . . . H8A H 0.5646 0.4452 0.2433 0.030 Uiso 1 1 calc R . . C24 C -0.1009(8) 0.0272(6) 0.4000(5) 0.0307(18) Uani 1 1 d . . . H24A H -0.2109 0.0098 0.3877 0.046 Uiso 1 1 calc R . . H24B H -0.0837 0.0723 0.4592 0.046 Uiso 1 1 calc R . . H24C H -0.0503 -0.0402 0.3959 0.046 Uiso 1 1 calc R . . C23 C -0.0347(7) 0.0895(6) 0.3332(5) 0.0259(17) Uani 1 1 d . . . H23A H -0.0492 0.0403 0.2739 0.031 Uiso 1 1 calc R . . C20 C 0.2641(8) 0.0021(6) 0.3441(5) 0.0302(18) Uani 1 1 d . . . H20A H 0.2529 -0.0186 0.4020 0.036 Uiso 1 1 calc R . . C2 C 0.0854(8) 0.1981(6) -0.0614(5) 0.0289(18) Uani 1 1 d . . . H2A H 0.0552 0.1213 -0.0922 0.035 Uiso 1 1 calc R . . C21 C 0.4356(8) 0.0217(7) 0.3328(6) 0.039(2) Uani 1 1 d . . . H21A H 0.4857 -0.0443 0.3357 0.059 Uiso 1 1 calc R . . H21B H 0.4783 0.0818 0.3796 0.059 Uiso 1 1 calc R . . H21C H 0.4528 0.0403 0.2759 0.059 Uiso 1 1 calc R . . C5 C 0.3914(8) 0.1181(6) -0.0474(5) 0.0339(19) Uani 1 1 d . . . H5A H 0.4595 0.0981 -0.0023 0.041 Uiso 1 1 calc R . . C22 C -0.1198(8) 0.1889(7) 0.3322(6) 0.038(2) Uani 1 1 d . . . H22A H -0.2289 0.1670 0.3197 0.058 Uiso 1 1 calc R . . H22B H -0.0797 0.2250 0.2868 0.058 Uiso 1 1 calc R . . H22C H -0.1060 0.2392 0.3894 0.058 Uiso 1 1 calc R . . C15 C 0.1631(9) 0.4956(6) 0.6049(5) 0.040(2) Uani 1 1 d . . . H15A H 0.0781 0.5409 0.6217 0.061 Uiso 1 1 calc R . . H15B H 0.2342 0.5315 0.5705 0.061 Uiso 1 1 calc R . . H15C H 0.2168 0.4851 0.6576 0.061 Uiso 1 1 calc R . . C17 C 0.4070(8) 0.3097(6) 0.5850(5) 0.0287(18) Uani 1 1 d . . . H17A H 0.4491 0.3872 0.6035 0.034 Uiso 1 1 calc R . . C14 C 0.1015(8) 0.3858(6) 0.5503(5) 0.0348(19) Uani 1 1 d . . . H14A H 0.0412 0.4018 0.5003 0.042 Uiso 1 1 calc R . . C9 C 0.6147(9) 0.4590(7) 0.1188(6) 0.048(2) Uani 1 1 d . . . H9A H 0.7265 0.4608 0.1231 0.072 Uiso 1 1 calc R . . H9B H 0.5835 0.5335 0.1319 0.072 Uiso 1 1 calc R . . H9C H 0.5784 0.4225 0.0595 0.072 Uiso 1 1 calc R . . C11 C 0.2428(8) 0.4850(6) 0.1933(5) 0.0298(18) Uani 1 1 d . . . H11A H 0.2818 0.5253 0.2527 0.036 Uiso 1 1 calc R . . C19 C 0.1960(9) -0.0969(6) 0.2745(5) 0.038(2) Uani 1 1 d . . . H19A H 0.2576 -0.1587 0.2740 0.058 Uiso 1 1 calc R . . H19B H 0.1965 -0.0786 0.2167 0.058 Uiso 1 1 calc R . . H19C H 0.0907 -0.1164 0.2885 0.058 Uiso 1 1 calc R . . C13 C -0.0125(9) 0.3239(7) 0.5999(6) 0.046(2) Uani 1 1 d . . . H13A H -0.1006 0.3666 0.6153 0.069 Uiso 1 1 calc R . . H13B H 0.0380 0.3127 0.6533 0.069 Uiso 1 1 calc R . . H13C H -0.0472 0.2533 0.5624 0.069 Uiso 1 1 calc R . . C4 C 0.4959(9) 0.1849(7) -0.0964(6) 0.047(2) Uani 1 1 d . . . H4A H 0.5869 0.1463 -0.1138 0.071 Uiso 1 1 calc R . . H4B H 0.5268 0.2558 -0.0582 0.071 Uiso 1 1 calc R . . H4C H 0.4410 0.1956 -0.1487 0.071 Uiso 1 1 calc R . . C1 C -0.0537(9) 0.2427(8) -0.0137(6) 0.048(2) Uani 1 1 d . . . H1A H -0.1422 0.2307 -0.0549 0.072 Uiso 1 1 calc R . . H1B H -0.0327 0.3209 0.0104 0.072 Uiso 1 1 calc R . . H1C H -0.0757 0.2053 0.0340 0.072 Uiso 1 1 calc R . . C7 C 0.6308(8) 0.2959(7) 0.1805(7) 0.048(2) Uani 1 1 d . . . H7A H 0.7381 0.3167 0.1992 0.072 Uiso 1 1 calc R . . H7B H 0.6252 0.2521 0.1206 0.072 Uiso 1 1 calc R . . H7C H 0.5830 0.2534 0.2198 0.072 Uiso 1 1 calc R . . C18 C 0.3478(10) 0.2726(7) 0.6670(5) 0.042(2) Uani 1 1 d . . . H18A H 0.4326 0.2783 0.7100 0.063 Uiso 1 1 calc R . . H18B H 0.3047 0.1968 0.6505 0.063 Uiso 1 1 calc R . . H18C H 0.2686 0.3189 0.6928 0.063 Uiso 1 1 calc R . . C6 C 0.3292(9) 0.0101(7) -0.1056(5) 0.042(2) Uani 1 1 d . . . H6A H 0.4143 -0.0341 -0.1252 0.063 Uiso 1 1 calc R . . H6B H 0.2736 0.0238 -0.1567 0.063 Uiso 1 1 calc R . . H6C H 0.2598 -0.0289 -0.0725 0.063 Uiso 1 1 calc R . . C3 C 0.1319(10) 0.2608(8) -0.1307(6) 0.051(2) Uani 1 1 d . . . H3A H 0.0440 0.2608 -0.1703 0.077 Uiso 1 1 calc R . . H3B H 0.2150 0.2263 -0.1640 0.077 Uiso 1 1 calc R . . H3C H 0.1668 0.3359 -0.1024 0.077 Uiso 1 1 calc R . . C16 C 0.5365(9) 0.2426(8) 0.5466(6) 0.054(3) Uani 1 1 d . . . H16A H 0.6234 0.2556 0.5889 0.081 Uiso 1 1 calc R . . H16B H 0.5683 0.2638 0.4926 0.081 Uiso 1 1 calc R . . H16C H 0.5011 0.1651 0.5337 0.081 Uiso 1 1 calc R . . C12 C 0.0725(9) 0.4592(7) 0.1981(7) 0.053(3) Uani 1 1 d . . . H12A H 0.0225 0.5270 0.2148 0.079 Uiso 1 1 calc R . . H12B H 0.0536 0.4150 0.2419 0.079 Uiso 1 1 calc R . . H12C H 0.0311 0.4187 0.1408 0.079 Uiso 1 1 calc R . . C10 C 0.2705(13) 0.5591(9) 0.1316(8) 0.079(4) Uani 1 1 d . . . H10A H 0.2074 0.6207 0.1469 0.119 Uiso 1 1 calc R . . H10B H 0.2435 0.5193 0.0717 0.119 Uiso 1 1 calc R . . H10C H 0.3787 0.5859 0.1358 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02608(16) 0.02094(17) 0.01568(16) 0.00447(11) 0.00013(10) -0.00633(11) Te1 0.0517(3) 0.0237(3) 0.0175(3) 0.0047(2) -0.0007(2) -0.0147(2) Te2 0.0692(4) 0.0338(3) 0.0175(3) 0.0066(3) -0.0029(3) -0.0298(3) P2 0.0208(10) 0.0193(10) 0.0187(10) 0.0056(8) 0.0006(7) -0.0045(7) P1 0.0241(10) 0.0219(11) 0.0172(10) 0.0045(8) 0.0002(7) -0.0037(8) P4 0.0226(10) 0.0210(11) 0.0173(10) 0.0076(8) -0.0002(7) -0.0046(7) P3 0.0266(10) 0.0242(11) 0.0166(10) 0.0043(9) -0.0021(8) -0.0078(8) N2 0.024(3) 0.024(3) 0.020(3) 0.001(3) 0.000(2) -0.008(2) N1 0.028(3) 0.026(4) 0.016(3) 0.002(3) 0.001(2) -0.007(3) C8 0.021(4) 0.031(5) 0.023(4) 0.009(4) -0.003(3) -0.008(3) C24 0.021(4) 0.041(5) 0.032(4) 0.015(4) 0.005(3) -0.007(3) C23 0.026(4) 0.022(4) 0.030(4) 0.010(3) -0.005(3) -0.007(3) C20 0.039(5) 0.025(4) 0.025(4) 0.004(4) -0.002(3) -0.002(3) C2 0.029(4) 0.031(5) 0.028(4) 0.011(4) -0.002(3) 0.000(3) C21 0.035(5) 0.039(5) 0.040(5) -0.001(4) 0.001(4) 0.008(4) C5 0.030(4) 0.035(5) 0.033(5) -0.004(4) 0.005(3) 0.004(3) C22 0.025(4) 0.045(5) 0.049(6) 0.021(4) -0.003(4) 0.001(4) C15 0.056(5) 0.025(5) 0.035(5) -0.005(4) 0.000(4) 0.003(4) C17 0.031(4) 0.030(5) 0.020(4) 0.003(4) -0.009(3) -0.013(3) C14 0.030(4) 0.034(5) 0.038(5) 0.004(4) -0.002(4) 0.005(3) C9 0.027(5) 0.059(6) 0.063(6) 0.030(5) 0.002(4) -0.014(4) C11 0.044(5) 0.020(4) 0.025(4) 0.002(3) 0.005(3) 0.003(3) C19 0.051(5) 0.029(5) 0.032(5) -0.002(4) -0.001(4) 0.004(4) C13 0.033(5) 0.044(6) 0.049(6) -0.016(5) 0.012(4) -0.003(4) C4 0.041(5) 0.049(6) 0.048(6) 0.002(5) 0.016(4) -0.002(4) C1 0.034(5) 0.061(6) 0.049(6) 0.010(5) -0.004(4) 0.009(4) C7 0.024(4) 0.041(5) 0.081(7) 0.024(5) -0.008(4) -0.005(4) C18 0.060(6) 0.041(5) 0.028(5) 0.019(4) -0.011(4) -0.003(4) C6 0.038(5) 0.043(5) 0.037(5) -0.007(4) 0.007(4) 0.003(4) C3 0.047(5) 0.070(7) 0.044(6) 0.036(5) -0.013(4) -0.008(5) C16 0.033(5) 0.086(8) 0.044(6) 0.018(5) -0.007(4) 0.007(5) C12 0.036(5) 0.045(6) 0.070(7) -0.009(5) 0.011(4) 0.010(4) C10 0.092(8) 0.070(8) 0.102(10) 0.060(7) 0.046(7) 0.044(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 P2 2.343(2) . ? Pt1 P4 2.3444(19) . ? Pt1 Te1 2.5795(12) . ? Pt1 Te2 2.5827(12) . ? Te1 P1 2.452(2) . ? Te2 P3 2.441(2) . ? P2 N1 1.633(6) . ? P2 C11 1.844(7) . ? P2 C8 1.855(6) . ? P1 N1 1.585(6) . ? P1 C2 1.830(7) . ? P1 C5 1.836(7) . ? P4 N2 1.643(6) . ? P4 C20 1.844(7) . ? P4 C23 1.848(7) . ? P3 N2 1.576(6) . ? P3 C17 1.840(7) . ? P3 C14 1.851(7) . ? C8 C9 1.503(10) . ? C8 C7 1.522(10) . ? C24 C23 1.535(9) . ? C23 C22 1.510(10) . ? C20 C21 1.527(10) . ? C20 C19 1.545(10) . ? C2 C3 1.518(11) . ? C2 C1 1.526(10) . ? C5 C6 1.525(10) . ? C5 C4 1.527(11) . ? C15 C14 1.519(10) . ? C17 C16 1.526(11) . ? C17 C18 1.545(10) . ? C14 C13 1.545(11) . ? C11 C10 1.492(12) . ? C11 C12 1.513(10) . ? 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 P2 Pt1 P4 177.64(7) . . ? P2 Pt1 Te1 90.78(5) . . ? P4 Pt1 Te1 90.51(5) . . ? P2 Pt1 Te2 87.56(5) . . ? P4 Pt1 Te2 91.17(5) . . ? Te1 Pt1 Te2 178.23(2) . . ? P1 Te1 Pt1 95.50(5) . . ? P3 Te2 Pt1 95.11(5) . . ? N1 P2 C11 105.0(3) . . ? N1 P2 C8 105.2(3) . . ? C11 P2 C8 106.1(3) . . ? N1 P2 Pt1 118.3(2) . . ? C11 P2 Pt1 110.4(2) . . ? C8 P2 Pt1 111.0(2) . . ? N1 P1 C2 111.3(3) . . ? N1 P1 C5 111.8(3) . . ? C2 P1 C5 107.7(4) . . ? N1 P1 Te1 110.5(2) . . ? C2 P1 Te1 109.7(2) . . ? C5 P1 Te1 105.8(3) . . ? N2 P4 C20 101.5(3) . . ? N2 P4 C23 104.7(3) . . ? C20 P4 C23 105.3(3) . . ? N2 P4 Pt1 116.9(2) . . ? C20 P4 Pt1 116.0(3) . . ? C23 P4 Pt1 111.1(2) . . ? N2 P3 C17 112.8(3) . . ? N2 P3 C14 111.7(3) . . ? C17 P3 C14 108.3(4) . . ? N2 P3 Te2 110.4(2) . . ? C17 P3 Te2 107.6(2) . . ? C14 P3 Te2 105.7(3) . . ? P3 N2 P4 125.4(4) . . ? P1 N1 P2 124.6(4) . . ? C9 C8 C7 109.1(7) . . ? C9 C8 P2 115.2(5) . . ? C7 C8 P2 108.6(5) . . ? C22 C23 C24 110.9(6) . . ? C22 C23 P4 109.4(5) . . ? C24 C23 P4 113.1(5) . . ? C21 C20 C19 110.4(6) . . ? C21 C20 P4 109.9(5) . . ? C19 C20 P4 117.0(5) . . ? C3 C2 C1 111.1(7) . . ? C3 C2 P1 111.4(5) . . ? C1 C2 P1 111.8(5) . . ? C6 C5 C4 112.1(7) . . ? C6 C5 P1 114.2(5) . . ? C4 C5 P1 114.0(6) . . ? C16 C17 C18 110.4(7) . . ? C16 C17 P3 110.0(5) . . ? C18 C17 P3 112.7(5) . . ? C15 C14 C13 112.7(7) . . ? C15 C14 P3 112.6(5) . . ? C13 C14 P3 113.2(5) . . ? C10 C11 C12 109.2(8) . . ? C10 C11 P2 114.8(6) . . ? C12 C11 P2 109.8(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.131 _refine_diff_density_min -1.780 _refine_diff_density_rms 0.336 #===END data_compound9a _database_code_depnum_ccdc_archive 'CCDC 735951' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H75 N2 P4 Pt Te2' _chemical_formula_weight 1098.14 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.008(3) _cell_length_b 18.866(4) _cell_length_c 14.822(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.07(3) _cell_angle_gamma 90.00 _cell_volume 4322.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34668 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 27.46 _exptl_crystal_description rod _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 4.743 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5175 _exptl_absorpt_correction_T_max 0.7640 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34668 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9658 _reflns_number_gt 8472 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _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^)+(0.0325P)^2^+73.5363P] 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 9658 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 0.074881(18) 0.724523(15) 0.485725(19) 0.01815(8) Uani 1 1 d . . . Te1 Te 0.16936(3) 0.80024(3) 0.61546(4) 0.02351(12) Uani 1 1 d . . . Te2 Te -0.40515(4) 0.76094(4) 0.40002(4) 0.03313(15) Uani 1 1 d . . . P3 P -0.31521(13) 0.81114(11) 0.53919(14) 0.0216(4) Uani 1 1 d . . . P4 P -0.16073(13) 0.87738(11) 0.48251(13) 0.0195(4) Uani 1 1 d . . . P1 P 0.28107(13) 0.70797(11) 0.67281(14) 0.0206(4) Uani 1 1 d . . . P2 P 0.16172(13) 0.62417(10) 0.53743(13) 0.0193(4) Uani 1 1 d . . . C32 C -0.0115(5) 0.8256(4) 0.3373(5) 0.0228(15) Uani 1 1 d . . . H32A H -0.0630 0.8549 0.3089 0.027 Uiso 1 1 calc R . . H32B H 0.0402 0.8525 0.3323 0.027 Uiso 1 1 calc R . . N2 N -0.2317(4) 0.8545(4) 0.5338(5) 0.0259(14) Uani 1 1 d . . . N1 N 0.2543(5) 0.6374(4) 0.6144(5) 0.0276(15) Uani 1 1 d . . . C21 C -0.0461(5) 0.9042(4) 0.6522(5) 0.0246(16) Uani 1 1 d . . . H3A H -0.0090 0.9384 0.6941 0.037 Uiso 1 1 calc R . . H3B H -0.0108 0.8645 0.6406 0.037 Uiso 1 1 calc R . . H3C H -0.0904 0.8866 0.6813 0.037 Uiso 1 1 calc R . . C2 C 0.2968(6) 0.6951(5) 0.7998(5) 0.0266(17) Uani 1 1 d . . . H11A H 0.3226 0.7393 0.8326 0.032 Uiso 1 1 calc R . . C20 C -0.0893(5) 0.9402(4) 0.5605(5) 0.0220(15) Uani 1 1 d . . . H2A H -0.0435 0.9561 0.5302 0.026 Uiso 1 1 calc R . . C3 C 0.2120(5) 0.6806(5) 0.8245(6) 0.0288(18) Uani 1 1 d . . . H10A H 0.2216 0.6816 0.8926 0.043 Uiso 1 1 calc R . . H10B H 0.1901 0.6338 0.8008 0.043 Uiso 1 1 calc R . . H10C H 0.1695 0.7170 0.7962 0.043 Uiso 1 1 calc R . . C5 C 0.3850(5) 0.7427(5) 0.6617(6) 0.0251(16) Uani 1 1 d . . . H8A H 0.4307 0.7092 0.6960 0.030 Uiso 1 1 calc R . . C23 C -0.2037(6) 0.9216(5) 0.3677(6) 0.0274(17) Uani 1 1 d . . . H5A H -0.2115 0.8836 0.3193 0.033 Uiso 1 1 calc R . . C19 C -0.1405(7) 1.0056(5) 0.5780(6) 0.033(2) Uani 1 1 d . . . H1A H -0.1018 1.0377 0.6217 0.050 Uiso 1 1 calc R . . H1B H -0.1875 0.9904 0.6047 0.050 Uiso 1 1 calc R . . H1C H -0.1647 1.0302 0.5188 0.050 Uiso 1 1 calc R . . C24 C -0.1394(6) 0.9760(5) 0.3444(6) 0.033(2) Uani 1 1 d . . . H4A H -0.1555 0.9855 0.2771 0.050 Uiso 1 1 calc R . . H4B H -0.0807 0.9566 0.3630 0.050 Uiso 1 1 calc R . . H4C H -0.1416 1.0202 0.3785 0.050 Uiso 1 1 calc R . . C14 C -0.2794(5) 0.7409(5) 0.6274(5) 0.0274(17) Uani 1 1 d . . . H20A H -0.2453 0.7637 0.6864 0.033 Uiso 1 1 calc R . . C1 C 0.3609(6) 0.6327(5) 0.8349(6) 0.036(2) Uani 1 1 d . . . H12A H 0.3680 0.6257 0.9020 0.054 Uiso 1 1 calc R . . H12B H 0.4171 0.6439 0.8236 0.054 Uiso 1 1 calc R . . H12C H 0.3379 0.5893 0.8013 0.054 Uiso 1 1 calc R . . C12 C 0.2423(6) 0.6218(5) 0.3922(6) 0.0303(18) Uani 1 1 d . . . H15A H 0.2386 0.6032 0.3296 0.045 Uiso 1 1 calc R . . H15B H 0.3028 0.6213 0.4291 0.045 Uiso 1 1 calc R . . H15C H 0.2204 0.6706 0.3872 0.045 Uiso 1 1 calc R . . C11 C 0.1884(5) 0.5760(4) 0.4397(6) 0.0254(16) Uani 1 1 d . . . H14A H 0.1323 0.5673 0.3923 0.031 Uiso 1 1 calc R . . C10 C 0.2307(7) 0.5039(5) 0.4642(7) 0.038(2) Uani 1 1 d . . . H13A H 0.2480 0.4850 0.4101 0.056 Uiso 1 1 calc R . . H13B H 0.1896 0.4714 0.4811 0.056 Uiso 1 1 calc R . . H13C H 0.2819 0.5089 0.5171 0.056 Uiso 1 1 calc R . . C15 C -0.2211(6) 0.6866(5) 0.5971(6) 0.0333(19) Uani 1 1 d . . . H19A H -0.2018 0.6512 0.6465 0.050 Uiso 1 1 calc R . . H19B H -0.1706 0.7108 0.5856 0.050 Uiso 1 1 calc R . . H19C H -0.2534 0.6631 0.5397 0.050 Uiso 1 1 calc R . . C16 C -0.3290(6) 0.8923(6) 0.6938(7) 0.039(2) Uani 1 1 d . . . H16A H -0.3647 0.9246 0.7198 0.058 Uiso 1 1 calc R . . H16B H -0.2755 0.9165 0.6911 0.058 Uiso 1 1 calc R . . H16C H -0.3148 0.8502 0.7336 0.058 Uiso 1 1 calc R . . C17 C -0.3790(6) 0.8699(5) 0.5949(6) 0.0321(19) Uani 1 1 d . . . H17A H -0.4308 0.8426 0.6007 0.039 Uiso 1 1 calc R . . C9 C 0.1632(6) 0.5095(5) 0.6606(6) 0.0329(19) Uani 1 1 d . . . H24A H 0.1297 0.4730 0.6827 0.049 Uiso 1 1 calc R . . H24B H 0.1927 0.5396 0.7131 0.049 Uiso 1 1 calc R . . H24C H 0.2063 0.4867 0.6337 0.049 Uiso 1 1 calc R . . C8 C 0.1025(5) 0.5548(4) 0.5862(6) 0.0254(16) Uani 1 1 d . . . H23A H 0.0736 0.5227 0.5336 0.030 Uiso 1 1 calc R . . C7 C 0.0311(6) 0.5870(5) 0.6269(6) 0.0328(19) Uani 1 1 d . . . H22A H 0.0015 0.5489 0.6514 0.049 Uiso 1 1 calc R . . H22B H -0.0108 0.6125 0.5777 0.049 Uiso 1 1 calc R . . H22C H 0.0573 0.6198 0.6775 0.049 Uiso 1 1 calc R . . C22 C -0.2918(6) 0.9550(6) 0.3565(7) 0.040(2) Uani 1 1 d . . . H6A H -0.3103 0.9779 0.2951 0.061 Uiso 1 1 calc R . . H6B H -0.2885 0.9906 0.4055 0.061 Uiso 1 1 calc R . . H6C H -0.3337 0.9183 0.3615 0.061 Uiso 1 1 calc R . . C13 C -0.3568(6) 0.7024(6) 0.6490(7) 0.040(2) Uani 1 1 d . . . H21A H -0.3356 0.6656 0.6960 0.060 Uiso 1 1 calc R . . H21B H -0.3922 0.6806 0.5917 0.060 Uiso 1 1 calc R . . H21C H -0.3919 0.7366 0.6730 0.060 Uiso 1 1 calc R . . C6 C 0.4061(6) 0.8155(5) 0.7086(8) 0.040(2) Uani 1 1 d . . . H9A H 0.4642 0.8301 0.7060 0.060 Uiso 1 1 calc R . . H9B H 0.4039 0.8124 0.7739 0.060 Uiso 1 1 calc R . . H9C H 0.3637 0.8504 0.6757 0.060 Uiso 1 1 calc R . . C4 C 0.3893(7) 0.7430(7) 0.5610(7) 0.045(3) Uani 1 1 d . . . H7A H 0.4446 0.7633 0.5571 0.068 Uiso 1 1 calc R . . H7B H 0.3417 0.7717 0.5235 0.068 Uiso 1 1 calc R . . H7C H 0.3843 0.6944 0.5371 0.068 Uiso 1 1 calc R . . C18 C -0.4116(7) 0.9349(6) 0.5348(8) 0.048(3) Uani 1 1 d . . . H18A H -0.4521 0.9613 0.5616 0.071 Uiso 1 1 calc R . . H18B H -0.4411 0.9197 0.4713 0.071 Uiso 1 1 calc R . . H18C H -0.3625 0.9654 0.5329 0.071 Uiso 1 1 calc R . . C26 C -0.0938(5) 0.8010(4) 0.4655(5) 0.0199(15) Uani 1 1 d . . . H25A H -0.0787 0.7753 0.5266 0.024 Uiso 1 1 calc R . . C27 C -0.1521(5) 0.7499(4) 0.3955(5) 0.0222(15) Uani 1 1 d . . . H26A H -0.2105 0.7499 0.4065 0.027 Uiso 1 1 calc R . . H26B H -0.1578 0.7677 0.3313 0.027 Uiso 1 1 calc R . . C28 C -0.1185(5) 0.6733(4) 0.4017(6) 0.0251(16) Uani 1 1 d . . . H27A H -0.1250 0.6531 0.4611 0.030 Uiso 1 1 calc R . . H27B H -0.1575 0.6461 0.3505 0.030 Uiso 1 1 calc R . . C30 C 0.0193(5) 0.6940(4) 0.3418(5) 0.0217(15) Uani 1 1 d . . . H29A H 0.0572 0.6624 0.3154 0.026 Uiso 1 1 calc R . . C31 C -0.0166(5) 0.7568(5) 0.2806(5) 0.0258(17) Uani 1 1 d . . . H31A H -0.0777 0.7474 0.2475 0.031 Uiso 1 1 calc R . . H31B H 0.0163 0.7629 0.2331 0.031 Uiso 1 1 calc R . . C29 C -0.0262(5) 0.6588(5) 0.3971(5) 0.0235(16) Uani 1 1 d . . . H28A H -0.0116 0.6072 0.4036 0.028 Uiso 1 1 calc R . . C25 C -0.0068(5) 0.8146(4) 0.4419(5) 0.0193(14) Uani 1 1 d . . . H33A H 0.0213 0.8571 0.4776 0.023 Uiso 1 1 calc R . . C33 C 0.4938(9) 0.5229(8) 0.5389(10) 0.069(4) Uani 1 1 d . . . H42A H 0.4349 0.5433 0.5205 0.104 Uiso 1 1 calc R . . H42B H 0.5355 0.5626 0.5479 0.104 Uiso 1 1 calc R . . C34 C 0.5058(12) 0.4838(8) 0.6321(10) 0.076(4) Uani 1 1 d . . . H41A H 0.4682 0.4413 0.6226 0.091 Uiso 1 1 calc R . . H41B H 0.5666 0.4678 0.6547 0.091 Uiso 1 1 calc R . . C35 C 0.4842(10) 0.5296(10) 0.7027(12) 0.086(5) Uani 1 1 d . . . H40A H 0.4987 0.5053 0.7632 0.129 Uiso 1 1 calc R . . H40B H 0.4222 0.5403 0.6843 0.129 Uiso 1 1 calc R . . H40C H 0.5173 0.5738 0.7077 0.129 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01681(14) 0.02200(15) 0.01502(14) -0.00181(10) 0.00301(10) 0.00018(10) Te1 0.0222(3) 0.0234(3) 0.0215(3) -0.00376(19) -0.00054(19) 0.00090(19) Te2 0.0254(3) 0.0502(4) 0.0207(3) -0.0054(2) 0.0005(2) -0.0048(2) P3 0.0180(9) 0.0287(11) 0.0188(9) -0.0021(8) 0.0057(7) -0.0015(8) P4 0.0197(9) 0.0214(9) 0.0177(9) -0.0010(7) 0.0056(7) 0.0004(7) P1 0.0166(9) 0.0269(10) 0.0161(9) 0.0002(7) 0.0002(7) -0.0004(7) P2 0.0205(9) 0.0221(9) 0.0146(9) -0.0027(7) 0.0032(7) -0.0014(7) C32 0.021(4) 0.028(4) 0.018(4) 0.001(3) 0.002(3) 0.005(3) N2 0.026(4) 0.026(4) 0.029(4) -0.003(3) 0.013(3) -0.001(3) N1 0.030(4) 0.026(4) 0.027(4) -0.003(3) 0.007(3) 0.003(3) C21 0.028(4) 0.030(4) 0.013(3) -0.003(3) 0.000(3) 0.000(3) C2 0.033(4) 0.032(4) 0.016(4) -0.003(3) 0.007(3) 0.000(3) C20 0.014(3) 0.031(4) 0.020(4) -0.004(3) 0.002(3) 0.000(3) C3 0.027(4) 0.036(5) 0.023(4) 0.001(3) 0.005(3) 0.001(3) C5 0.018(4) 0.032(4) 0.025(4) -0.005(3) 0.003(3) -0.003(3) C23 0.031(4) 0.032(4) 0.019(4) 0.009(3) 0.006(3) 0.005(3) C19 0.049(6) 0.024(4) 0.027(4) -0.005(3) 0.010(4) 0.003(4) C24 0.042(5) 0.034(5) 0.023(4) 0.006(3) 0.007(4) 0.000(4) C14 0.026(4) 0.039(5) 0.014(4) -0.001(3) 0.000(3) 0.000(3) C1 0.039(5) 0.041(5) 0.024(4) 0.012(4) 0.003(4) 0.000(4) C12 0.038(5) 0.030(4) 0.026(4) 0.001(3) 0.012(4) 0.001(4) C11 0.026(4) 0.028(4) 0.021(4) -0.002(3) 0.003(3) 0.004(3) C10 0.058(6) 0.027(5) 0.032(5) -0.003(4) 0.019(4) 0.012(4) C15 0.036(5) 0.037(5) 0.026(4) 0.004(4) 0.005(4) 0.001(4) C16 0.035(5) 0.050(6) 0.032(5) -0.009(4) 0.011(4) 0.002(4) C17 0.024(4) 0.041(5) 0.035(5) -0.005(4) 0.014(4) 0.001(4) C9 0.047(5) 0.027(4) 0.026(4) 0.005(3) 0.012(4) -0.001(4) C8 0.023(4) 0.026(4) 0.028(4) -0.003(3) 0.009(3) -0.005(3) C7 0.032(5) 0.040(5) 0.031(5) 0.004(4) 0.016(4) 0.006(4) C22 0.028(5) 0.048(6) 0.041(5) 0.017(4) 0.000(4) 0.010(4) C13 0.037(5) 0.049(6) 0.034(5) 0.013(4) 0.012(4) -0.007(4) C6 0.033(5) 0.034(5) 0.052(6) -0.007(4) 0.009(4) -0.018(4) C4 0.032(5) 0.072(8) 0.035(5) -0.007(5) 0.013(4) -0.020(5) C18 0.043(6) 0.054(7) 0.048(6) -0.002(5) 0.015(5) 0.020(5) C26 0.019(4) 0.024(4) 0.016(3) -0.003(3) 0.004(3) -0.001(3) C27 0.018(4) 0.026(4) 0.021(4) -0.006(3) 0.003(3) 0.001(3) C28 0.020(4) 0.027(4) 0.024(4) -0.008(3) -0.001(3) -0.002(3) C30 0.024(4) 0.023(4) 0.019(4) -0.013(3) 0.006(3) -0.001(3) C31 0.024(4) 0.039(5) 0.012(3) 0.000(3) 0.001(3) 0.002(3) C29 0.016(4) 0.031(4) 0.020(4) -0.005(3) -0.003(3) -0.002(3) C25 0.015(3) 0.025(4) 0.014(3) -0.006(3) -0.002(3) 0.001(3) C33 0.051(7) 0.074(10) 0.083(10) -0.003(8) 0.018(7) -0.003(7) C34 0.099(12) 0.064(9) 0.066(9) -0.001(7) 0.023(8) -0.005(8) C35 0.052(8) 0.116(15) 0.093(12) -0.019(10) 0.025(8) -0.005(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 C25 2.140(7) . ? Pt1 C30 2.165(7) . ? Pt1 C29 2.186(7) . ? Pt1 P2 2.356(2) . ? Pt1 Te1 2.5521(9) . ? Te1 P1 2.482(2) . ? Te2 P3 2.383(2) . ? P3 N2 1.586(7) . ? P3 C17 1.842(9) . ? P3 C14 1.846(9) . ? P4 N2 1.583(7) . ? P4 C20 1.834(8) . ? P4 C26 1.852(8) . ? P4 C23 1.859(8) . ? P1 N1 1.584(7) . ? P1 C5 1.835(8) . ? P1 C2 1.849(8) . ? P2 N1 1.637(7) . ? P2 C11 1.851(8) . ? P2 C8 1.868(8) . ? C32 C31 1.536(11) . ? C32 C25 1.547(10) . ? C21 C20 1.517(11) . ? C2 C3 1.521(12) . ? C2 C1 1.560(12) . ? C20 C19 1.539(11) . ? C5 C4 1.512(12) . ? C5 C6 1.536(12) . ? C23 C22 1.514(12) . ? C23 C24 1.554(12) . ? C14 C15 1.530(12) . ? C14 C13 1.539(12) . ? C12 C11 1.518(12) . ? C11 C10 1.521(12) . ? C16 C17 1.535(13) . ? C17 C18 1.525(14) . ? C9 C8 1.528(12) . ? C8 C7 1.549(11) . ? C26 C27 1.542(10) . ? C26 C25 1.543(10) . ? C27 C28 1.536(11) . ? C28 C29 1.522(11) . ? C30 C29 1.397(11) . ? C30 C31 1.512(11) . ? C33 C33 1.49(3) 3_666 ? C33 C34 1.53(2) . ? C34 C35 1.47(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 C25 Pt1 C30 81.4(3) . . ? C25 Pt1 C29 88.3(3) . . ? C30 Pt1 C29 37.5(3) . . ? C25 Pt1 P2 178.0(2) . . ? C30 Pt1 P2 99.4(2) . . ? C29 Pt1 P2 91.2(2) . . ? C25 Pt1 Te1 88.84(19) . . ? C30 Pt1 Te1 154.5(2) . . ? C29 Pt1 Te1 166.3(2) . . ? P2 Pt1 Te1 91.19(5) . . ? P1 Te1 Pt1 95.66(5) . . ? N2 P3 C17 106.5(4) . . ? N2 P3 C14 107.2(4) . . ? C17 P3 C14 102.8(4) . . ? N2 P3 Te2 119.3(3) . . ? C17 P3 Te2 110.3(3) . . ? C14 P3 Te2 109.5(3) . . ? N2 P4 C20 106.4(4) . . ? N2 P4 C26 111.5(4) . . ? C20 P4 C26 107.5(3) . . ? N2 P4 C23 114.9(4) . . ? C20 P4 C23 107.9(4) . . ? C26 P4 C23 108.3(4) . . ? N1 P1 C5 112.0(4) . . ? N1 P1 C2 113.0(4) . . ? C5 P1 C2 104.6(4) . . ? N1 P1 Te1 109.5(3) . . ? C5 P1 Te1 107.9(3) . . ? C2 P1 Te1 109.6(3) . . ? N1 P2 C11 105.6(4) . . ? N1 P2 C8 107.2(4) . . ? C11 P2 C8 101.7(4) . . ? N1 P2 Pt1 117.0(3) . . ? C11 P2 Pt1 112.1(3) . . ? C8 P2 Pt1 111.9(3) . . ? C31 C32 C25 114.6(7) . . ? P4 N2 P3 152.2(5) . . ? P1 N1 P2 125.2(5) . . ? C3 C2 C1 109.6(7) . . ? C3 C2 P1 112.1(6) . . ? C1 C2 P1 110.1(6) . . ? C21 C20 C19 110.2(6) . . ? C21 C20 P4 109.9(6) . . ? C19 C20 P4 110.6(6) . . ? C4 C5 C6 112.4(8) . . ? C4 C5 P1 111.4(6) . . ? C6 C5 P1 112.1(6) . . ? C22 C23 C24 110.6(7) . . ? C22 C23 P4 113.6(6) . . ? C24 C23 P4 113.0(6) . . ? C15 C14 C13 109.4(8) . . ? C15 C14 P3 111.9(6) . . ? C13 C14 P3 111.6(6) . . ? C12 C11 C10 110.3(7) . . ? C12 C11 P2 111.0(6) . . ? C10 C11 P2 115.6(6) . . ? C18 C17 C16 110.5(8) . . ? C18 C17 P3 111.5(6) . . ? C16 C17 P3 112.5(6) . . ? C9 C8 C7 109.5(7) . . ? C9 C8 P2 112.3(6) . . ? C7 C8 P2 112.1(6) . . ? C27 C26 C25 112.1(6) . . ? C27 C26 P4 107.9(5) . . ? C25 C26 P4 119.4(5) . . ? C28 C27 C26 114.0(6) . . ? C29 C28 C27 119.6(7) . . ? C29 C30 C31 123.3(7) . . ? C29 C30 Pt1 72.1(4) . . ? C31 C30 Pt1 112.1(5) . . ? C30 C31 C32 112.1(6) . . ? C30 C29 C28 127.0(7) . . ? C30 C29 Pt1 70.5(4) . . ? C28 C29 Pt1 116.6(5) . . ? C26 C25 C32 115.9(6) . . ? C26 C25 Pt1 108.4(5) . . ? C32 C25 Pt1 106.1(5) . . ? C33 C33 C34 114.0(17) 3_666 . ? C35 C34 C33 111.2(14) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 3.308 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.215