Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name T.Chivers 'Jari Konu' _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_address ; Department of Chemistry University of Calgary 2500 University Drive NW Calgary T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, spectroscopic and structural characterization of tertiary phosphine tellurium dihalides Et3PTeX2 (X = Cl, Br, I) ; _journal_name_full 'Dalton Transactions' _publ_contact_author 'Professor Tristram Chivers' data_1a _database_code_depnum_ccdc_archive 'CCDC 610264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 Cl2 P Te' _chemical_formula_sum 'C6 H15 Cl2 P Te' _chemical_formula_weight 316.65 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6125(15) _cell_length_b 13.301(3) _cell_length_c 10.905(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.51(3) _cell_angle_gamma 90.00 _cell_volume 1104.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2578 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 3.262 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2624 _exptl_absorpt_correction_T_max 0.3035 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2758 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1851 _reflns_number_gt 1789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _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^)+(0.0441P)^2^+4.5051P] 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 1851 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _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 Te1 Te 0.18987(4) 0.60376(2) 0.61192(2) 0.01337(15) Uani 1 1 d . . . Cl1 Cl 0.10745(19) 0.59041(9) 0.38747(11) 0.0247(3) Uani 1 1 d . . . Cl2 Cl 0.31067(17) 0.63831(9) 0.83205(10) 0.0221(3) Uani 1 1 d . . . P1 P 0.32590(14) 0.76908(8) 0.57475(10) 0.0100(2) Uani 1 1 d . . . C1 C 0.5616(6) 0.7634(4) 0.5995(4) 0.0188(10) Uani 1 1 d . . . H1A H 0.6158 0.8243 0.5638 0.023 Uiso 1 1 calc R . . H1B H 0.5861 0.7640 0.6888 0.023 Uiso 1 1 calc R . . C2 C 0.6473(7) 0.6709(4) 0.5436(5) 0.0282(12) Uani 1 1 d . . . H2A H 0.6132 0.6110 0.5900 0.042 Uiso 1 1 calc R . . H2B H 0.7753 0.6784 0.5466 0.042 Uiso 1 1 calc R . . H2C H 0.6085 0.6637 0.4581 0.042 Uiso 1 1 calc R . . C3 C 0.2370(6) 0.8616(3) 0.6793(4) 0.0161(9) Uani 1 1 d . . . H3A H 0.2632 0.8403 0.7645 0.019 Uiso 1 1 calc R . . H3B H 0.2967 0.9266 0.6655 0.019 Uiso 1 1 calc R . . C4 C 0.0384(7) 0.8767(4) 0.6650(5) 0.0256(11) Uani 1 1 d . . . H4A H 0.0110 0.8969 0.5806 0.038 Uiso 1 1 calc R . . H4B H -0.0005 0.9293 0.7216 0.038 Uiso 1 1 calc R . . H4C H -0.0223 0.8137 0.6837 0.038 Uiso 1 1 calc R . . C5 C 0.2813(6) 0.8116(4) 0.4199(4) 0.0171(10) Uani 1 1 d . . . H5A H 0.3460 0.7682 0.3619 0.021 Uiso 1 1 calc R . . H5B H 0.1543 0.8037 0.4021 0.021 Uiso 1 1 calc R . . C6 C 0.3333(7) 0.9213(4) 0.3978(4) 0.0237(11) Uani 1 1 d . . . H6A H 0.2643 0.9651 0.4511 0.036 Uiso 1 1 calc R . . H6B H 0.3103 0.9388 0.3118 0.036 Uiso 1 1 calc R . . H6C H 0.4586 0.9300 0.4163 0.036 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 Te1 0.0151(2) 0.0093(2) 0.0156(2) 0.00018(10) -0.00117(13) -0.00243(10) Cl1 0.0364(7) 0.0189(6) 0.0187(6) -0.0013(4) -0.0075(5) -0.0089(5) Cl2 0.0302(7) 0.0195(6) 0.0165(5) 0.0015(5) -0.0045(5) -0.0045(5) P1 0.0105(5) 0.0082(5) 0.0111(5) -0.0002(4) -0.0001(4) -0.0007(4) C1 0.011(2) 0.024(3) 0.022(2) 0.003(2) -0.0022(18) -0.0005(19) C2 0.018(2) 0.026(3) 0.040(3) 0.000(2) 0.005(2) 0.009(2) C3 0.020(2) 0.010(2) 0.018(2) -0.0029(18) 0.0016(18) 0.0003(18) C4 0.017(3) 0.027(3) 0.033(3) -0.005(2) 0.009(2) 0.006(2) C5 0.021(2) 0.018(3) 0.012(2) 0.0005(18) -0.0010(18) -0.0007(19) C6 0.027(3) 0.024(3) 0.020(2) 0.008(2) 0.001(2) 0.000(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 Te1 P1 2.4656(12) . ? Te1 Cl1 2.5275(13) . ? Te1 Cl2 2.6038(13) . ? P1 C5 1.810(4) . ? P1 C3 1.812(5) . ? P1 C1 1.814(5) . ? C1 C2 1.522(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.532(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.531(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Cl1 90.26(4) . . ? P1 Te1 Cl2 81.30(4) . . ? Cl1 Te1 Cl2 171.02(4) . . ? C5 P1 C3 107.9(2) . . ? C5 P1 C1 109.2(2) . . ? C3 P1 C1 108.0(2) . . ? C5 P1 Te1 110.88(16) . . ? C3 P1 Te1 110.01(16) . . ? C1 P1 Te1 110.79(17) . . ? C2 C1 P1 113.6(4) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.5(3) . . ? C4 C3 H3A 108.9 . . ? P1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? P1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 113.4(3) . . ? C6 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Te1 P1 C5 7.67(17) . . . . ? Cl2 Te1 P1 C5 -175.41(18) . . . . ? Cl1 Te1 P1 C3 126.92(17) . . . . ? Cl2 Te1 P1 C3 -56.16(16) . . . . ? Cl1 Te1 P1 C1 -113.72(17) . . . . ? Cl2 Te1 P1 C1 63.20(17) . . . . ? C5 P1 C1 C2 -78.3(4) . . . . ? C3 P1 C1 C2 164.6(4) . . . . ? Te1 P1 C1 C2 44.1(4) . . . . ? C5 P1 C3 C4 60.1(4) . . . . ? C1 P1 C3 C4 178.0(4) . . . . ? Te1 P1 C3 C4 -61.0(4) . . . . ? C3 P1 C5 C6 49.1(4) . . . . ? C1 P1 C5 C6 -68.0(4) . . . . ? Te1 P1 C5 C6 169.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.671 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.164 #===END data_1b _database_code_depnum_ccdc_archive 'CCDC 610265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 Br2 P Te' _chemical_formula_sum 'C6 H15 Br2 P Te' _chemical_formula_weight 405.57 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6660(15) _cell_length_b 13.669(3) _cell_length_c 11.269(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.32(3) _cell_angle_gamma 90.00 _cell_volume 1180.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3991 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 9.366 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1335 _exptl_absorpt_correction_T_max 0.2560 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3991 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2071 _reflns_number_gt 1949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _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^)+(0.0470P)^2^+1.0253P] 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 2071 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Te1 Te 0.80362(3) 0.103532(16) 0.60667(2) 0.01917(12) Uani 1 1 d . . . Br1 Br 0.88895(6) 0.08731(3) 0.37688(4) 0.02896(14) Uani 1 1 d . . . Br2 Br 0.68183(6) 0.13209(3) 0.83341(3) 0.02798(14) Uani 1 1 d . . . P1 P 0.66996(12) 0.26594(7) 0.57327(8) 0.0162(2) Uani 1 1 d . . . C1 C 0.4367(5) 0.2611(3) 0.5972(3) 0.0240(8) Uani 1 1 d . . . H1A H 0.4145 0.2597 0.6836 0.029 Uiso 1 1 calc R . . H1B H 0.3832 0.3216 0.5650 0.029 Uiso 1 1 calc R . . C2 C 0.3483(5) 0.1731(3) 0.5399(4) 0.0371(11) Uani 1 1 d . . . H2A H 0.3824 0.1688 0.4564 0.056 Uiso 1 1 calc R . . H2B H 0.2214 0.1804 0.5451 0.056 Uiso 1 1 calc R . . H2C H 0.3843 0.1133 0.5815 0.056 Uiso 1 1 calc R . . C3 C 0.7637(5) 0.3541(3) 0.6754(3) 0.0207(8) Uani 1 1 d . . . H3A H 0.7068 0.4183 0.6624 0.025 Uiso 1 1 calc R . . H3B H 0.7381 0.3333 0.7576 0.025 Uiso 1 1 calc R . . C4 C 0.9601(5) 0.3665(3) 0.6624(4) 0.0321(10) Uani 1 1 d . . . H4A H 1.0179 0.3036 0.6768 0.048 Uiso 1 1 calc R . . H4B H 1.0022 0.4148 0.7201 0.048 Uiso 1 1 calc R . . H4C H 0.9865 0.3890 0.5819 0.048 Uiso 1 1 calc R . . C5 C 0.7109(5) 0.3086(3) 0.4239(3) 0.0218(8) Uani 1 1 d . . . H5A H 0.8355 0.2980 0.4051 0.026 Uiso 1 1 calc R . . H5B H 0.6407 0.2691 0.3676 0.026 Uiso 1 1 calc R . . C6 C 0.6671(6) 0.4175(3) 0.4054(4) 0.0316(10) Uani 1 1 d . . . H6A H 0.5444 0.4289 0.4250 0.047 Uiso 1 1 calc R . . H6B H 0.6876 0.4353 0.3225 0.047 Uiso 1 1 calc R . . H6C H 0.7415 0.4575 0.4572 0.047 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 Te1 0.02173(17) 0.01539(17) 0.02040(17) 0.00002(9) 0.00166(11) 0.00258(9) Br1 0.0390(3) 0.0250(2) 0.0230(2) -0.00123(16) 0.00655(18) 0.00890(17) Br2 0.0365(3) 0.0265(3) 0.0211(2) 0.00254(16) 0.00455(17) 0.00402(17) P1 0.0168(5) 0.0146(5) 0.0172(4) 0.0001(4) 0.0004(4) 0.0007(4) C1 0.0214(19) 0.025(2) 0.0257(19) 0.0017(16) 0.0032(16) 0.0024(16) C2 0.023(2) 0.034(3) 0.054(3) 0.002(2) -0.0060(19) -0.0079(19) C3 0.022(2) 0.0164(18) 0.0235(19) -0.0020(15) -0.0010(15) -0.0020(15) C4 0.028(2) 0.029(2) 0.039(2) -0.0004(19) -0.0086(18) -0.0065(18) C5 0.026(2) 0.020(2) 0.0192(18) 0.0019(15) 0.0024(15) 0.0015(16) C6 0.036(2) 0.025(2) 0.034(2) 0.0083(18) 0.0022(19) 0.0036(18) _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 Te1 P1 2.4730(10) . ? Te1 Br1 2.6837(7) . ? Te1 Br2 2.7531(8) . ? P1 C5 1.811(4) . ? P1 C1 1.811(4) . ? P1 C3 1.812(4) . ? C1 C2 1.523(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.523(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.539(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 Br1 91.74(3) . . ? P1 Te1 Br2 82.62(3) . . ? Br1 Te1 Br2 173.237(15) . . ? C5 P1 C1 109.07(18) . . ? C5 P1 C3 107.81(18) . . ? C1 P1 C3 108.54(18) . . ? C5 P1 Te1 110.90(13) . . ? C1 P1 Te1 110.69(13) . . ? C3 P1 Te1 109.76(12) . . ? C2 C1 P1 113.8(3) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.7(3) . . ? C4 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 113.4(3) . . ? C6 C5 H5A 108.9 . . ? P1 C5 H5A 108.9 . . ? C6 C5 H5B 108.9 . . ? P1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Te1 P1 C5 -7.48(14) . . . . ? Br2 Te1 P1 C5 176.27(14) . . . . ? Br1 Te1 P1 C1 113.72(14) . . . . ? Br2 Te1 P1 C1 -62.54(14) . . . . ? Br1 Te1 P1 C3 -126.50(14) . . . . ? Br2 Te1 P1 C3 57.25(14) . . . . ? C5 P1 C1 C2 77.2(3) . . . . ? C3 P1 C1 C2 -165.6(3) . . . . ? Te1 P1 C1 C2 -45.1(3) . . . . ? C5 P1 C3 C4 -60.9(3) . . . . ? C1 P1 C3 C4 -178.9(3) . . . . ? Te1 P1 C3 C4 60.0(3) . . . . ? C1 P1 C5 C6 70.5(3) . . . . ? C3 P1 C5 C6 -47.2(3) . . . . ? Te1 P1 C5 C6 -167.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.885 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.162 #===END data_1c _database_code_depnum_ccdc_archive 'CCDC 610266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 I2 P Te' _chemical_formula_sum 'C6 H15 I2 P Te' _chemical_formula_weight 499.55 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.6469(17) _cell_length_b 11.051(2) _cell_length_c 13.897(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.06(3) _cell_angle_gamma 90.00 _cell_volume 1288.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3786 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 7.175 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1821 _exptl_absorpt_correction_T_max 0.3279 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3786 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2247 _reflns_number_gt 2151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _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^)+(0.0285P)^2^+4.1926P] 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 2247 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 Te1 Te 0.02016(3) 0.86820(2) 0.133456(19) 0.01747(10) Uani 1 1 d . . . I1 I 0.28532(4) 0.99553(3) 0.07265(2) 0.02801(11) Uani 1 1 d . . . I2 I -0.24208(4) 0.73665(4) 0.18235(3) 0.03588(12) Uani 1 1 d . . . P1 P 0.19591(13) 0.77888(10) 0.28573(8) 0.0156(2) Uani 1 1 d . . . C1 C 0.2429(6) 0.6230(4) 0.2666(4) 0.0246(10) Uani 1 1 d . . . H1A H 0.3116 0.5911 0.3291 0.030 Uiso 1 1 calc R . . H1B H 0.1428 0.5755 0.2518 0.030 Uiso 1 1 calc R . . C2 C 0.3263(7) 0.6031(5) 0.1839(4) 0.0348(12) Uani 1 1 d . . . H2A H 0.2678 0.6451 0.1240 0.052 Uiso 1 1 calc R . . H2B H 0.3300 0.5163 0.1702 0.052 Uiso 1 1 calc R . . H2C H 0.4352 0.6350 0.2039 0.052 Uiso 1 1 calc R . . C3 C 0.3792(6) 0.8651(4) 0.3225(3) 0.0245(10) Uani 1 1 d . . . H3A H 0.4407 0.8553 0.2715 0.029 Uiso 1 1 calc R . . H3B H 0.3527 0.9520 0.3254 0.029 Uiso 1 1 calc R . . C4 C 0.4835(6) 0.8262(6) 0.4233(4) 0.0394(13) Uani 1 1 d . . . H4A H 0.4238 0.8365 0.4743 0.059 Uiso 1 1 calc R . . H4B H 0.5799 0.8763 0.4397 0.059 Uiso 1 1 calc R . . H4C H 0.5134 0.7410 0.4202 0.059 Uiso 1 1 calc R . . C5 C 0.1012(6) 0.7752(4) 0.3884(3) 0.0239(10) Uani 1 1 d . . . H5A H 0.0094 0.7190 0.3715 0.029 Uiso 1 1 calc R . . H5B H 0.1780 0.7418 0.4471 0.029 Uiso 1 1 calc R . . C6 C 0.0426(8) 0.8964(5) 0.4165(4) 0.0407(14) Uani 1 1 d . . . H6A H 0.1323 0.9530 0.4336 0.061 Uiso 1 1 calc R . . H6B H -0.0038 0.8860 0.4736 0.061 Uiso 1 1 calc R . . H6C H -0.0384 0.9284 0.3603 0.061 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 Te1 0.01889(17) 0.01839(17) 0.01432(17) 0.00049(11) 0.00247(12) 0.00085(11) I1 0.02967(19) 0.0324(2) 0.02104(18) 0.00365(13) 0.00437(13) -0.01022(13) I2 0.02419(19) 0.0472(2) 0.0357(2) 0.00337(16) 0.00616(14) -0.01280(15) P1 0.0178(5) 0.0138(5) 0.0148(5) 0.0003(4) 0.0032(4) -0.0001(4) C1 0.028(2) 0.019(2) 0.027(3) 0.0003(19) 0.007(2) 0.0027(19) C2 0.034(3) 0.033(3) 0.038(3) -0.009(2) 0.011(2) 0.006(2) C3 0.025(2) 0.023(2) 0.021(2) 0.0027(19) -0.0024(19) -0.0039(19) C4 0.030(3) 0.044(3) 0.036(3) 0.013(3) -0.008(2) -0.005(2) C5 0.030(3) 0.026(2) 0.016(2) 0.0051(19) 0.0072(19) 0.007(2) C6 0.055(4) 0.038(3) 0.033(3) 0.003(2) 0.019(3) 0.018(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 Te1 P1 2.4899(13) . ? Te1 I2 2.9096(6) . ? Te1 I1 2.9819(7) . ? P1 C1 1.805(5) . ? P1 C5 1.810(5) . ? P1 C3 1.813(5) . ? C1 C2 1.515(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.531(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.515(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Te1 I2 87.30(3) . . ? P1 Te1 I1 94.32(3) . . ? I2 Te1 I1 176.803(14) . . ? C1 P1 C5 104.8(2) . . ? C1 P1 C3 109.3(2) . . ? C5 P1 C3 108.8(2) . . ? C1 P1 Te1 111.49(17) . . ? C5 P1 Te1 112.29(16) . . ? C3 P1 Te1 110.03(15) . . ? C2 C1 P1 114.6(4) . . ? C2 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.0(3) . . ? C4 C3 H3A 109.0 . . ? P1 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? P1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 115.2(4) . . ? C6 C5 H5A 108.5 . . ? P1 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? P1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I2 Te1 P1 C1 76.98(18) . . . . ? I1 Te1 P1 C1 -100.26(18) . . . . ? I2 Te1 P1 C5 -40.30(18) . . . . ? I1 Te1 P1 C5 142.46(18) . . . . ? I2 Te1 P1 C3 -161.58(18) . . . . ? I1 Te1 P1 C3 21.18(18) . . . . ? C5 P1 C1 C2 -179.2(4) . . . . ? C3 P1 C1 C2 -62.8(4) . . . . ? Te1 P1 C1 C2 59.1(4) . . . . ? C1 P1 C3 C4 -65.1(4) . . . . ? C5 P1 C3 C4 48.8(5) . . . . ? Te1 P1 C3 C4 172.2(4) . . . . ? C1 P1 C5 C6 -177.3(4) . . . . ? C3 P1 C5 C6 65.9(5) . . . . ? Te1 P1 C5 C6 -56.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.746 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.160 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 610267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H31 O2 P2, 0.5(I6 Te2)' _chemical_formula_sum 'C12 H31 I3 O2 P2 Te' _chemical_formula_weight 777.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 25.840(5) _cell_length_b 13.095(3) _cell_length_c 15.944(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.89(3) _cell_angle_gamma 90.00 _cell_volume 4812(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8142 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 5.219 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2859 _exptl_absorpt_correction_T_max 0.4217 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8142 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _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 2.84 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4229 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _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^)+(0.0301P)^2^+18.0756P] 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 4229 _refine_ls_number_parameters 187 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 I1 I 0.673594(13) 0.16032(2) 0.41228(2) 0.04170(10) Uani 1 1 d . . . I2 I 0.576535(13) 0.42850(3) 0.33499(2) 0.04033(10) Uani 1 1 d . . . I3 I 0.716492(14) 0.60770(3) 0.49271(2) 0.04007(10) Uani 1 1 d . . . Te1 Te 0.695995(12) 0.39584(2) 0.452529(18) 0.02837(9) Uani 1 1 d . . . P1 P 0.61683(5) 0.23562(9) 0.68149(8) 0.0302(3) Uani 1 1 d . . . P2 P 0.43920(5) 0.18692(9) 0.41895(8) 0.0288(2) Uani 1 1 d . . . O1 O 0.57948(14) 0.1548(3) 0.6104(2) 0.0372(8) Uani 1 1 d D . . H1 H 0.550(3) 0.172(9) 0.594(8) 0.045 Uiso 0.50 1 d PD . . O2 O 0.47512(14) 0.1687(3) 0.5246(2) 0.0374(8) Uani 1 1 d D . . H2 H 0.508(3) 0.163(9) 0.541(7) 0.045 Uiso 0.50 1 d PD . . C1 C 0.5847(2) 0.2738(4) 0.7551(3) 0.0473(13) Uani 1 1 d . . . H1A H 0.6074 0.3310 0.7956 0.057 Uiso 1 1 calc R . . H1B H 0.5449 0.2993 0.7150 0.057 Uiso 1 1 calc R . . C2 C 0.5815(3) 0.1886(6) 0.8171(4) 0.075(2) Uani 1 1 d . . . H2A H 0.5635 0.2144 0.8555 0.112 Uiso 1 1 calc R . . H2B H 0.6208 0.1641 0.8583 0.112 Uiso 1 1 calc R . . H2C H 0.5582 0.1323 0.7776 0.112 Uiso 1 1 calc R . . C3 C 0.6866(2) 0.1842(4) 0.7541(3) 0.0426(12) Uani 1 1 d . . . H3A H 0.7076 0.2314 0.8072 0.051 Uiso 1 1 calc R . . H3B H 0.6819 0.1185 0.7805 0.051 Uiso 1 1 calc R . . C4 C 0.7234(3) 0.1663(5) 0.7029(4) 0.0614(16) Uani 1 1 d . . . H4A H 0.7611 0.1381 0.7469 0.092 Uiso 1 1 calc R . . H4B H 0.7292 0.2313 0.6778 0.092 Uiso 1 1 calc R . . H4C H 0.7034 0.1182 0.6511 0.092 Uiso 1 1 calc R . . C5 C 0.6253(2) 0.3446(4) 0.6226(3) 0.0431(12) Uani 1 1 d . . . H5A H 0.6387 0.3214 0.5766 0.052 Uiso 1 1 calc R . . H5B H 0.5868 0.3766 0.5867 0.052 Uiso 1 1 calc R . . C6 C 0.6676(3) 0.4266(4) 0.6855(4) 0.0530(14) Uani 1 1 d . . . H6A H 0.6691 0.4831 0.6463 0.079 Uiso 1 1 calc R . . H6B H 0.7064 0.3969 0.7201 0.079 Uiso 1 1 calc R . . H6C H 0.6543 0.4522 0.7302 0.079 Uiso 1 1 calc R . . C7 C 0.3807(2) 0.0985(4) 0.3709(4) 0.0409(12) Uani 1 1 d . . . H7A H 0.3573 0.1132 0.3032 0.049 Uiso 1 1 calc R . . H7B H 0.3967 0.0287 0.3766 0.049 Uiso 1 1 calc R . . C8 C 0.3412(3) 0.1012(5) 0.4186(5) 0.0611(16) Uani 1 1 d . . . H8A H 0.3100 0.0510 0.3890 0.092 Uiso 1 1 calc R . . H8B H 0.3244 0.1696 0.4120 0.092 Uiso 1 1 calc R . . H8C H 0.3638 0.0849 0.4855 0.092 Uiso 1 1 calc R . . C9 C 0.4090(2) 0.3138(4) 0.3979(4) 0.0446(12) Uani 1 1 d . . . H9A H 0.3914 0.3283 0.3296 0.054 Uiso 1 1 calc R . . H9B H 0.3780 0.3173 0.4179 0.054 Uiso 1 1 calc R . . C10 C 0.4543(3) 0.3945(4) 0.4501(5) 0.0627(18) Uani 1 1 d . . . H10A H 0.4361 0.4620 0.4366 0.094 Uiso 1 1 calc R . . H10B H 0.4848 0.3922 0.4296 0.094 Uiso 1 1 calc R . . H10C H 0.4714 0.3812 0.5179 0.094 Uiso 1 1 calc R . . C11 C 0.4823(2) 0.1723(4) 0.3573(3) 0.0373(11) Uani 1 1 d . . . H11A H 0.4570 0.1807 0.2891 0.045 Uiso 1 1 calc R . . H11B H 0.5119 0.2270 0.3775 0.045 Uiso 1 1 calc R . . C12 C 0.5124(2) 0.0700(4) 0.3741(3) 0.0379(11) Uani 1 1 d . . . H12A H 0.5351 0.0665 0.3389 0.057 Uiso 1 1 calc R . . H12B H 0.4833 0.0154 0.3530 0.057 Uiso 1 1 calc R . . H12C H 0.5382 0.0617 0.4414 0.057 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 I1 0.02840(17) 0.0418(2) 0.03942(18) 0.00130(14) 0.00175(14) -0.00461(14) I2 0.02253(16) 0.0479(2) 0.04098(18) 0.00287(15) 0.00592(14) -0.00294(13) I3 0.03639(19) 0.03960(19) 0.03719(19) -0.00615(14) 0.01045(15) -0.00485(14) Te1 0.02279(16) 0.03830(18) 0.02258(15) 0.00083(12) 0.00900(13) -0.00269(12) P1 0.0320(6) 0.0337(6) 0.0236(5) -0.0001(5) 0.0113(5) -0.0024(5) P2 0.0290(6) 0.0266(6) 0.0309(6) 0.0004(5) 0.0136(5) 0.0014(5) O1 0.0352(18) 0.0365(19) 0.0339(18) -0.0055(15) 0.0103(17) -0.0006(16) O2 0.0333(18) 0.046(2) 0.0344(18) 0.0002(15) 0.0165(16) 0.0029(16) C1 0.042(3) 0.066(4) 0.036(3) -0.012(3) 0.019(2) -0.007(3) C2 0.074(4) 0.111(6) 0.057(4) 0.002(4) 0.046(4) -0.018(4) C3 0.032(3) 0.048(3) 0.038(3) 0.004(2) 0.008(2) 0.002(2) C4 0.051(4) 0.067(4) 0.068(4) -0.001(3) 0.029(3) 0.014(3) C5 0.045(3) 0.043(3) 0.036(3) 0.010(2) 0.014(2) -0.003(2) C6 0.060(4) 0.041(3) 0.061(4) -0.001(3) 0.030(3) -0.013(3) C7 0.039(3) 0.041(3) 0.042(3) -0.007(2) 0.018(2) -0.003(2) C8 0.052(4) 0.057(4) 0.083(4) -0.014(3) 0.038(4) -0.016(3) C9 0.047(3) 0.029(3) 0.056(3) 0.001(2) 0.022(3) 0.006(2) C10 0.053(4) 0.027(3) 0.100(5) -0.011(3) 0.028(4) -0.004(2) C11 0.039(3) 0.042(3) 0.034(2) 0.000(2) 0.019(2) -0.001(2) C12 0.043(3) 0.040(3) 0.036(3) 0.000(2) 0.024(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 I1 Te1 3.1501(7) . ? I1 Te1 3.1581(13) 7_656 ? I2 Te1 2.8269(11) . ? I3 Te1 2.8427(7) . ? Te1 I1 3.1581(13) 7_656 ? P1 O1 1.532(4) . ? P1 C5 1.775(5) . ? P1 C3 1.777(5) . ? P1 C1 1.790(5) . ? P1 H1 1.86(10) . ? P2 O2 1.530(3) . ? P2 C7 1.779(5) . ? P2 C11 1.797(4) . ? P2 C9 1.801(5) . ? O1 H1 0.72(5) . ? O2 H2 0.76(5) . ? C1 C2 1.517(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.523(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.537(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.524(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.516(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.511(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Te1 I1 Te1 92.745(16) . 7_656 ? I2 Te1 I3 92.181(16) . . ? I2 Te1 I1 88.172(15) . . ? I3 Te1 I1 178.81(3) . . ? I2 Te1 I1 174.841(14) . 7_656 ? I3 Te1 I1 92.343(17) . 7_656 ? I1 Te1 I1 87.255(16) . 7_656 ? O1 P1 C5 110.5(2) . . ? O1 P1 C3 109.5(2) . . ? C5 P1 C3 108.5(3) . . ? O1 P1 C1 110.8(2) . . ? C5 P1 C1 109.1(3) . . ? C3 P1 C1 108.3(2) . . ? C5 P1 H1 105(3) . . ? C3 P1 H1 130(3) . . ? C1 P1 H1 94(3) . . ? O2 P2 C7 110.3(2) . . ? O2 P2 C11 111.6(2) . . ? C7 P2 C11 108.1(2) . . ? O2 P2 C9 110.2(2) . . ? C7 P2 C9 108.0(2) . . ? C11 P2 C9 108.6(2) . . ? P1 O1 H1 105(10) . . ? P2 O2 H2 114(8) . . ? C2 C1 P1 113.5(4) . . ? C2 C1 H1A 108.9 . . ? P1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.8(4) . . ? C4 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 116.0(4) . . ? C6 C5 H5A 108.3 . . ? P1 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? P1 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P2 113.6(4) . . ? C8 C7 H7A 108.8 . . ? P2 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? P2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P2 112.3(4) . . ? C10 C9 H9A 109.1 . . ? P2 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? P2 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P2 113.2(3) . . ? C12 C11 H11A 108.9 . . ? P2 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? P2 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Te1 I1 Te1 I2 -177.61(3) 7_656 . . . ? Te1 I1 Te1 I1 0.0 7_656 . . 7_656 ? O1 P1 C1 C2 64.5(5) . . . . ? C5 P1 C1 C2 -173.6(4) . . . . ? C3 P1 C1 C2 -55.6(5) . . . . ? O1 P1 C3 C4 69.6(5) . . . . ? C5 P1 C3 C4 -51.2(5) . . . . ? C1 P1 C3 C4 -169.5(4) . . . . ? O1 P1 C5 C6 -173.2(4) . . . . ? C3 P1 C5 C6 -53.1(5) . . . . ? C1 P1 C5 C6 64.7(5) . . . . ? O2 P2 C7 C8 56.6(5) . . . . ? C11 P2 C7 C8 178.8(4) . . . . ? C9 P2 C7 C8 -63.9(5) . . . . ? O2 P2 C9 C10 49.8(5) . . . . ? C7 P2 C9 C10 170.3(4) . . . . ? C11 P2 C9 C10 -72.6(5) . . . . ? O2 P2 C11 C12 55.4(4) . . . . ? C7 P2 C11 C12 -66.0(4) . . . . ? C9 P2 C11 C12 177.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.538 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.113 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 610268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C12 H31 O2 P2), I4 Te' _chemical_formula_sum 'C24 H62 I4 O4 P4 Te' _chemical_formula_weight 1173.82 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.548(2) _cell_length_b 11.297(2) _cell_length_c 18.344(4) _cell_angle_alpha 93.47(3) _cell_angle_beta 91.30(3) _cell_angle_gamma 104.45(3) _cell_volume 2111.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14415 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 3.805 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5166 _exptl_absorpt_correction_T_max 0.5812 _exptl_absorpt_process_details 'SADABS (SHELXTL-NT v5.1, Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD (Nonius, FR540C)' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14415 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7429 _reflns_number_gt 6407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'WinGX v1.70-01 (L. J. Farrugia)' _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^)+(0.0234P)^2^+2.8707P] 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 7429 _refine_ls_number_parameters 349 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 I1 I 0.33089(2) 0.67315(2) 0.491183(14) 0.03296(7) Uani 1 1 d . . . I2 I 0.38410(3) 0.41368(3) 0.639620(14) 0.03854(8) Uani 1 1 d . . . I3 I -0.09976(3) 0.46670(2) 0.149457(13) 0.03284(7) Uani 1 1 d . . . I4 I 0.16426(2) 0.32486(2) 0.021934(14) 0.03099(7) Uani 1 1 d . . . Te1 Te 0.5000 0.5000 0.5000 0.02346(8) Uani 1 2 d S . . Te2 Te 0.0000 0.5000 0.0000 0.02220(8) Uani 1 2 d S . . P1 P 0.48013(10) 1.03553(9) 0.30764(6) 0.0312(2) Uani 1 1 d . . . P2 P 0.41433(9) 0.72956(8) 0.11869(5) 0.0254(2) Uani 1 1 d . . . P3 P 0.09131(9) 0.27951(8) 0.37553(5) 0.0233(2) Uani 1 1 d . . . P4 P -0.08268(11) -0.02826(9) 0.18984(5) 0.0319(2) Uani 1 1 d . . . O1 O 0.3873(3) 0.9829(3) 0.24094(15) 0.0391(7) Uani 1 1 d D . . H1 H 0.411(10) 0.938(8) 0.209(4) 0.047 Uiso 0.50 1 d PD . . O2 O 0.4574(3) 0.8656(2) 0.14246(16) 0.0395(7) Uani 1 1 d D . . H2 H 0.444(10) 0.905(8) 0.179(4) 0.047 Uiso 0.50 1 d PD . . O3 O 0.0648(3) 0.1447(2) 0.34742(15) 0.0341(6) Uani 1 1 d D . . H3 H 0.010(8) 0.122(9) 0.317(4) 0.041 Uiso 0.50 1 d PD . . O4 O -0.1059(3) 0.0509(3) 0.25595(16) 0.0432(7) Uani 1 1 d D . . H4 H -0.042(8) 0.090(8) 0.285(4) 0.052 Uiso 0.50 1 d PD . . C1 C 0.5564(5) 0.9224(4) 0.3398(2) 0.0446(11) Uani 1 1 d . . . H1A H 0.4871 0.8525 0.3547 0.053 Uiso 1 1 calc R . . H1B H 0.6013 0.8917 0.2987 0.053 Uiso 1 1 calc R . . C2 C 0.6545(5) 0.9665(5) 0.4031(3) 0.0622(15) Uani 1 1 d . . . H2A H 0.6913 0.8991 0.4168 0.093 Uiso 1 1 calc R . . H2B H 0.6107 0.9945 0.4449 0.093 Uiso 1 1 calc R . . H2C H 0.7250 1.0344 0.3887 0.093 Uiso 1 1 calc R . . C3 C 0.3827(4) 1.0830(4) 0.3766(2) 0.0356(9) Uani 1 1 d . . . H3A H 0.4401 1.1195 0.4199 0.043 Uiso 1 1 calc R . . H3B H 0.3446 1.1475 0.3580 0.043 Uiso 1 1 calc R . . C4 C 0.2733(4) 0.9807(4) 0.4001(2) 0.0439(11) Uani 1 1 d . . . H4A H 0.2234 1.0132 0.4373 0.066 Uiso 1 1 calc R . . H4B H 0.3103 0.9178 0.4206 0.066 Uiso 1 1 calc R . . H4C H 0.2153 0.9445 0.3578 0.066 Uiso 1 1 calc R . . C5 C 0.6061(4) 1.1658(4) 0.2862(2) 0.0440(11) Uani 1 1 d . . . H5A H 0.6520 1.2064 0.3322 0.053 Uiso 1 1 calc R . . H5B H 0.6708 1.1373 0.2561 0.053 Uiso 1 1 calc R . . C6 C 0.5562(5) 1.2587(5) 0.2457(3) 0.0608(14) Uani 1 1 d . . . H6A H 0.6299 1.3272 0.2357 0.091 Uiso 1 1 calc R . . H6B H 0.4938 1.2892 0.2757 0.091 Uiso 1 1 calc R . . H6C H 0.5124 1.2200 0.1995 0.091 Uiso 1 1 calc R . . C7 C 0.5455(4) 0.6603(4) 0.1398(2) 0.0320(9) Uani 1 1 d . . . H7A H 0.6248 0.7045 0.1156 0.038 Uiso 1 1 calc R . . H7B H 0.5648 0.6721 0.1931 0.038 Uiso 1 1 calc R . . C8 C 0.5203(4) 0.5244(4) 0.1172(3) 0.0419(10) Uani 1 1 d . . . H8A H 0.5970 0.4954 0.1309 0.063 Uiso 1 1 calc R . . H8B H 0.5039 0.5114 0.0641 0.063 Uiso 1 1 calc R . . H8C H 0.4437 0.4789 0.1419 0.063 Uiso 1 1 calc R . . C9 C 0.2700(4) 0.6517(3) 0.1623(2) 0.0283(8) Uani 1 1 d . . . H9A H 0.1959 0.6841 0.1459 0.034 Uiso 1 1 calc R . . H9B H 0.2493 0.5636 0.1458 0.034 Uiso 1 1 calc R . . C10 C 0.2801(4) 0.6634(4) 0.2456(2) 0.0337(9) Uani 1 1 d . . . H10A H 0.1974 0.6184 0.2650 0.051 Uiso 1 1 calc R . . H10B H 0.2980 0.7500 0.2627 0.051 Uiso 1 1 calc R . . H10C H 0.3515 0.6293 0.2626 0.051 Uiso 1 1 calc R . . C11 C 0.3774(4) 0.7106(3) 0.0226(2) 0.0310(9) Uani 1 1 d . . . H11A H 0.3598 0.6225 0.0066 0.037 Uiso 1 1 calc R . . H11B H 0.2967 0.7375 0.0124 0.037 Uiso 1 1 calc R . . C12 C 0.4875(5) 0.7825(5) -0.0219(2) 0.0472(11) Uani 1 1 d . . . H12A H 0.4618 0.7687 -0.0740 0.071 Uiso 1 1 calc R . . H12B H 0.5672 0.7550 -0.0130 0.071 Uiso 1 1 calc R . . H12C H 0.5041 0.8701 -0.0072 0.071 Uiso 1 1 calc R . . C13 C 0.1266(4) 0.2919(3) 0.47183(19) 0.0303(9) Uani 1 1 d . . . H13A H 0.2094 0.2681 0.4811 0.036 Uiso 1 1 calc R . . H13B H 0.1400 0.3785 0.4902 0.036 Uiso 1 1 calc R . . C14 C 0.0190(5) 0.2127(5) 0.5145(2) 0.0503(12) Uani 1 1 d . . . H14A H 0.0444 0.2233 0.5666 0.075 Uiso 1 1 calc R . . H14B H 0.0062 0.1265 0.4974 0.075 Uiso 1 1 calc R . . H14C H -0.0628 0.2373 0.5068 0.075 Uiso 1 1 calc R . . C15 C -0.0479(4) 0.3382(3) 0.3558(2) 0.0319(9) Uani 1 1 d . . . H15A H -0.0685 0.3256 0.3025 0.038 Uiso 1 1 calc R . . H15B H -0.1241 0.2899 0.3807 0.038 Uiso 1 1 calc R . . C16 C -0.0303(4) 0.4736(4) 0.3788(2) 0.0386(10) Uani 1 1 d . . . H16A H -0.1106 0.4978 0.3663 0.058 Uiso 1 1 calc R . . H16B H 0.0430 0.5228 0.3533 0.058 Uiso 1 1 calc R . . H16C H -0.0119 0.4871 0.4317 0.058 Uiso 1 1 calc R . . C17 C 0.2328(4) 0.3698(3) 0.33472(19) 0.0267(8) Uani 1 1 d . . . H17A H 0.2408 0.4575 0.3485 0.032 Uiso 1 1 calc R . . H17B H 0.3120 0.3487 0.3544 0.032 Uiso 1 1 calc R . . C18 C 0.2271(4) 0.3501(4) 0.2517(2) 0.0393(10) Uani 1 1 d . . . H18A H 0.3063 0.4015 0.2322 0.059 Uiso 1 1 calc R . . H18B H 0.1498 0.3724 0.2318 0.059 Uiso 1 1 calc R . . H18C H 0.2214 0.2638 0.2377 0.059 Uiso 1 1 calc R . . C19 C -0.1106(4) -0.1846(4) 0.2105(2) 0.0395(10) Uani 1 1 d . . . H19A H -0.2014 -0.2135 0.2267 0.047 Uiso 1 1 calc R . . H19B H -0.1020 -0.2346 0.1656 0.047 Uiso 1 1 calc R . . C20 C -0.0159(5) -0.2042(4) 0.2697(3) 0.0574(13) Uani 1 1 d . . . H20A H -0.0355 -0.2913 0.2789 0.086 Uiso 1 1 calc R . . H20B H -0.0253 -0.1564 0.3148 0.086 Uiso 1 1 calc R . . H20C H 0.0741 -0.1775 0.2536 0.086 Uiso 1 1 calc R . . C21 C 0.0813(4) 0.0258(4) 0.1606(2) 0.0417(10) Uani 1 1 d . . . H21A H 0.0935 0.1114 0.1472 0.050 Uiso 1 1 calc R . . H21B H 0.1426 0.0269 0.2025 0.050 Uiso 1 1 calc R . . C22 C 0.1188(5) -0.0486(5) 0.0962(3) 0.0584(13) Uani 1 1 d . . . H22A H 0.2097 -0.0121 0.0843 0.088 Uiso 1 1 calc R . . H22B H 0.0608 -0.0483 0.0538 0.088 Uiso 1 1 calc R . . H22C H 0.1100 -0.1330 0.1092 0.088 Uiso 1 1 calc R . . C23 C -0.1986(4) -0.0241(4) 0.1181(2) 0.0389(10) Uani 1 1 d . . . H23A H -0.1817 -0.0737 0.0748 0.047 Uiso 1 1 calc R . . H23B H -0.2876 -0.0625 0.1340 0.047 Uiso 1 1 calc R . . C24 C -0.1954(5) 0.1031(4) 0.0960(3) 0.0513(12) Uani 1 1 d . . . H24A H -0.2613 0.0981 0.0567 0.077 Uiso 1 1 calc R . . H24B H -0.1083 0.1413 0.0789 0.077 Uiso 1 1 calc R . . H24C H -0.2144 0.1525 0.1382 0.077 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 I1 0.03189(15) 0.02874(14) 0.04055(16) -0.00001(11) 0.00047(11) 0.01259(11) I2 0.03570(16) 0.05241(17) 0.03091(15) 0.00904(12) 0.00268(11) 0.01587(13) I3 0.03168(15) 0.03916(15) 0.02786(14) 0.00345(11) 0.00440(11) 0.00867(11) I4 0.02900(14) 0.02960(14) 0.03575(15) -0.00041(11) 0.00010(11) 0.01067(11) Te1 0.02094(18) 0.02368(17) 0.02444(18) -0.00211(13) -0.00428(13) 0.00446(13) Te2 0.01760(17) 0.02304(17) 0.02381(17) -0.00257(13) -0.00185(13) 0.00232(13) P1 0.0343(6) 0.0269(5) 0.0324(6) -0.0037(4) 0.0000(4) 0.0090(4) P2 0.0251(5) 0.0237(5) 0.0253(5) -0.0018(4) 0.0007(4) 0.0034(4) P3 0.0248(5) 0.0214(5) 0.0227(5) -0.0007(4) -0.0027(4) 0.0047(4) P4 0.0364(6) 0.0280(5) 0.0310(6) -0.0077(4) -0.0080(4) 0.0109(4) O1 0.0436(18) 0.0358(16) 0.0378(17) -0.0095(13) -0.0069(14) 0.0134(13) O2 0.0473(18) 0.0235(14) 0.0416(17) -0.0081(12) 0.0121(14) -0.0013(13) O3 0.0388(18) 0.0230(14) 0.0383(17) -0.0045(12) -0.0085(13) 0.0058(12) O4 0.0431(19) 0.0446(18) 0.0404(18) -0.0191(14) -0.0082(14) 0.0140(15) C1 0.049(3) 0.039(2) 0.050(3) -0.007(2) -0.008(2) 0.023(2) C2 0.073(4) 0.063(3) 0.055(3) -0.003(3) -0.026(3) 0.029(3) C3 0.034(2) 0.031(2) 0.040(2) -0.0026(18) -0.0008(18) 0.0080(18) C4 0.036(3) 0.051(3) 0.045(3) 0.008(2) 0.003(2) 0.008(2) C5 0.036(3) 0.047(3) 0.047(3) -0.001(2) 0.009(2) 0.008(2) C6 0.064(4) 0.051(3) 0.068(3) 0.021(3) 0.020(3) 0.011(3) C7 0.022(2) 0.044(2) 0.028(2) 0.0024(18) -0.0009(16) 0.0065(17) C8 0.036(2) 0.041(2) 0.054(3) 0.010(2) 0.008(2) 0.018(2) C9 0.025(2) 0.0281(19) 0.032(2) -0.0001(16) -0.0028(16) 0.0077(16) C10 0.037(2) 0.031(2) 0.033(2) 0.0010(17) 0.0065(18) 0.0071(18) C11 0.034(2) 0.033(2) 0.029(2) 0.0032(17) -0.0011(17) 0.0122(18) C12 0.046(3) 0.065(3) 0.036(2) 0.013(2) 0.010(2) 0.020(2) C13 0.033(2) 0.032(2) 0.024(2) 0.0034(16) -0.0032(16) 0.0055(17) C14 0.050(3) 0.064(3) 0.036(3) 0.016(2) 0.008(2) 0.010(2) C15 0.026(2) 0.035(2) 0.036(2) 0.0018(17) -0.0016(17) 0.0085(17) C16 0.039(3) 0.036(2) 0.047(3) 0.0064(19) 0.011(2) 0.0187(19) C17 0.027(2) 0.0243(19) 0.028(2) 0.0014(15) 0.0000(16) 0.0051(16) C18 0.048(3) 0.036(2) 0.033(2) 0.0041(18) 0.0086(19) 0.008(2) C19 0.044(3) 0.033(2) 0.039(2) -0.0049(18) -0.0094(19) 0.0065(19) C20 0.074(4) 0.046(3) 0.051(3) 0.009(2) -0.017(3) 0.014(3) C21 0.045(3) 0.041(2) 0.036(2) -0.0072(19) -0.006(2) 0.008(2) C22 0.045(3) 0.073(4) 0.054(3) -0.011(3) 0.005(2) 0.012(3) C23 0.038(2) 0.036(2) 0.042(2) -0.0023(19) -0.0063(19) 0.0095(19) C24 0.062(3) 0.044(3) 0.053(3) 0.008(2) -0.004(2) 0.023(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 I1 Te1 2.9667(8) . ? I2 Te1 2.9756(9) . ? I3 Te2 2.9703(8) . ? I4 Te2 2.9756(8) . ? P1 O1 1.542(3) . ? P1 C3 1.788(4) . ? P1 C5 1.790(4) . ? P1 C1 1.791(4) . ? P2 O2 1.523(3) . ? P2 C11 1.786(4) . ? P2 C9 1.790(4) . ? P2 C7 1.796(4) . ? P3 O3 1.532(3) . ? P3 C13 1.787(4) . ? P3 C17 1.792(4) . ? P3 C15 1.794(4) . ? P4 O4 1.524(3) . ? P4 C19 1.782(4) . ? P4 C23 1.786(4) . ? P4 C21 1.791(4) . ? O1 H1 0.83(5) . ? O2 H2 0.81(5) . ? O3 H3 0.77(4) . ? O4 H4 0.85(4) . ? C1 C2 1.512(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.506(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.511(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.521(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.525(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.522(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.526(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.523(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.522(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.524(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.509(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Te1 I1 180.0 2_666 . ? I1 Te1 I2 88.75(3) 2_666 . ? I1 Te1 I2 91.25(3) . . ? I1 Te1 I2 91.25(3) 2_666 2_666 ? I1 Te1 I2 88.75(3) . 2_666 ? I2 Te1 I2 180.0 . 2_666 ? I3 Te2 I3 180.0 . 2_565 ? I3 Te2 I4 90.60(3) . . ? I3 Te2 I4 89.40(3) 2_565 . ? I3 Te2 I4 89.40(3) . 2_565 ? I3 Te2 I4 90.60(3) 2_565 2_565 ? I4 Te2 I4 180.0 . 2_565 ? O1 P1 C3 106.81(19) . . ? O1 P1 C5 111.6(2) . . ? C3 P1 C5 108.6(2) . . ? O1 P1 C1 110.77(18) . . ? C3 P1 C1 110.7(2) . . ? C5 P1 C1 108.3(2) . . ? O2 P2 C11 109.53(18) . . ? O2 P2 C9 112.80(17) . . ? C11 P2 C9 106.96(18) . . ? O2 P2 C7 108.75(18) . . ? C11 P2 C7 109.58(18) . . ? C9 P2 C7 109.18(18) . . ? O3 P3 C13 109.06(17) . . ? O3 P3 C17 110.69(17) . . ? C13 P3 C17 106.84(18) . . ? O3 P3 C15 110.37(17) . . ? C13 P3 C15 110.25(19) . . ? C17 P3 C15 109.58(18) . . ? O4 P4 C19 110.93(19) . . ? O4 P4 C23 108.92(19) . . ? C19 P4 C23 106.4(2) . . ? O4 P4 C21 110.22(19) . . ? C19 P4 C21 109.7(2) . . ? C23 P4 C21 110.6(2) . . ? P1 O1 H1 119(7) . . ? P2 O2 H2 132(7) . . ? P3 O3 H3 117(7) . . ? P4 O4 H4 121(7) . . ? C2 C1 P1 115.1(3) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 113.8(3) . . ? C4 C3 H3A 108.8 . . ? P1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? P1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 113.8(3) . . ? C6 C5 H5A 108.8 . . ? P1 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? P1 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P2 115.6(3) . . ? C8 C7 H7A 108.4 . . ? P2 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? P2 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P2 114.7(3) . . ? C10 C9 H9A 108.6 . . ? P2 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? P2 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P2 113.1(3) . . ? C12 C11 H11A 109.0 . . ? P2 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? P2 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P3 113.5(3) . . ? C14 C13 H13A 108.9 . . ? P3 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? P3 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P3 114.9(3) . . ? C16 C15 H15A 108.6 . . ? P3 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P3 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P3 112.8(3) . . ? C18 C17 H17A 109.0 . . ? P3 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 . . ? P3 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P4 112.8(3) . . ? C20 C19 H19A 109.0 . . ? P4 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? P4 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P4 115.5(3) . . ? C22 C21 H21A 108.4 . . ? P4 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? P4 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P4 114.2(3) . . ? C24 C23 H23A 108.7 . . ? P4 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? P4 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 C2 177.3(4) . . . . ? C3 P1 C1 C2 -64.4(4) . . . . ? C5 P1 C1 C2 54.6(4) . . . . ? O1 P1 C3 C4 60.1(3) . . . . ? C5 P1 C3 C4 -179.4(3) . . . . ? C1 P1 C3 C4 -60.6(4) . . . . ? O1 P1 C5 C6 47.3(4) . . . . ? C3 P1 C5 C6 -70.2(4) . . . . ? C1 P1 C5 C6 169.5(3) . . . . ? O2 P2 C7 C8 -178.1(3) . . . . ? C11 P2 C7 C8 -58.4(3) . . . . ? C9 P2 C7 C8 58.5(3) . . . . ? O2 P2 C9 C10 -56.4(3) . . . . ? C11 P2 C9 C10 -176.9(3) . . . . ? C7 P2 C9 C10 64.6(3) . . . . ? O2 P2 C11 C12 52.0(3) . . . . ? C9 P2 C11 C12 174.6(3) . . . . ? C7 P2 C11 C12 -67.2(3) . . . . ? O3 P3 C13 C14 -56.3(3) . . . . ? C17 P3 C13 C14 -175.9(3) . . . . ? C15 P3 C13 C14 65.1(4) . . . . ? O3 P3 C15 C16 -177.7(3) . . . . ? C13 P3 C15 C16 61.7(3) . . . . ? C17 P3 C15 C16 -55.6(3) . . . . ? O3 P3 C17 C18 51.2(3) . . . . ? C13 P3 C17 C18 169.8(3) . . . . ? C15 P3 C17 C18 -70.8(3) . . . . ? O4 P4 C19 C20 -63.4(4) . . . . ? C23 P4 C19 C20 178.3(3) . . . . ? C21 P4 C19 C20 58.6(4) . . . . ? O4 P4 C21 C22 178.0(3) . . . . ? C19 P4 C21 C22 55.5(4) . . . . ? C23 P4 C21 C22 -61.5(4) . . . . ? O4 P4 C23 C24 56.9(4) . . . . ? C19 P4 C23 C24 176.5(3) . . . . ? C21 P4 C23 C24 -64.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.186 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.102 #===END