# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1782 data_compound9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H69 In P2' _chemical_formula_weight 678.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'In' 'In' -0.7276 1.3100 '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 8.036(2) _cell_length_b 9.8530(10) _cell_length_c 12.361(2) _cell_angle_alpha 80.611(9) _cell_angle_beta 89.472(10) _cell_angle_gamma 68.470(7) _cell_volume 896.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type diffabs _exptl_absorpt_correction_T_min 0.8969 _exptl_absorpt_correction_T_max 0.7824 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5411 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.40 _reflns_number_total 5411 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.1514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5411 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 In1 In 0.0000 0.0000 0.0000 0.02329(6) Uani 1 2 d S . . P1 P -0.15444(4) -0.10517(4) 0.20252(3) 0.01347(7) Uani 1 1 d . . . C1 C -0.01498(18) -0.16530(15) 0.33417(11) 0.0157(2) Uani 1 1 d . . . H1 H -0.0356 -0.0754 0.3652 0.019 Uiso 1 1 calc R . . C2 C 0.1853(2) -0.22580(18) 0.31008(13) 0.0221(3) Uani 1 1 d . . . H2A H 0.2111 -0.3130 0.2762 0.027 Uiso 1 1 calc R . . H2B H 0.2114 -0.1517 0.2585 0.027 Uiso 1 1 calc R . . C3 C 0.3059(2) -0.26612(19) 0.41446(14) 0.0254(3) Uani 1 1 d . . . H3A H 0.4301 -0.3102 0.3967 0.030 Uiso 1 1 calc R . . H3B H 0.2912 -0.1768 0.4433 0.030 Uiso 1 1 calc R . . C4 C 0.2618(2) -0.37455(18) 0.50209(13) 0.0236(3) Uani 1 1 d . . . H4A H 0.2876 -0.4677 0.4763 0.028 Uiso 1 1 calc R . . H4B H 0.3362 -0.3938 0.5685 0.028 Uiso 1 1 calc R . . C5 C 0.0652(2) -0.31106(18) 0.52739(13) 0.0232(3) Uani 1 1 d . . . H5A H 0.0420 -0.2220 0.5585 0.028 Uiso 1 1 calc R . . H5B H 0.0384 -0.3823 0.5814 0.028 Uiso 1 1 calc R . . C6 C -0.05638(19) -0.27418(17) 0.42397(12) 0.0197(3) Uani 1 1 d . . . H6A H -0.1804 -0.2311 0.4422 0.024 Uiso 1 1 calc R . . H6B H -0.0403 -0.3646 0.3964 0.024 Uiso 1 1 calc R . . C7 C -0.36525(18) 0.04367(15) 0.22873(11) 0.0156(2) Uani 1 1 d . . . H7 H -0.4393 0.0736 0.1601 0.019 Uiso 1 1 calc R . . C8 C -0.4809(2) 0.00272(16) 0.31755(14) 0.0235(3) Uani 1 1 d . . . H8A H -0.4174 -0.0222 0.3887 0.028 Uiso 1 1 calc R . . H8B H -0.5027 -0.0836 0.3038 0.028 Uiso 1 1 calc R . . C9 C -0.6601(2) 0.13133(18) 0.31889(17) 0.0292(3) Uani 1 1 d . . . H9A H -0.7280 0.1510 0.2498 0.035 Uiso 1 1 calc R . . H9B H -0.7293 0.1043 0.3774 0.035 Uiso 1 1 calc R . . C10 C -0.6298(2) 0.27071(17) 0.33633(14) 0.0257(3) Uani 1 1 d . . . H10A H -0.7444 0.3523 0.3325 0.031 Uiso 1 1 calc R . . H10B H -0.5735 0.2542 0.4088 0.031 Uiso 1 1 calc R . . C11 C -0.5115(2) 0.31146(16) 0.24999(13) 0.0237(3) Uani 1 1 d . . . H11A H -0.4883 0.3963 0.2659 0.028 Uiso 1 1 calc R . . H11B H -0.5740 0.3390 0.1783 0.028 Uiso 1 1 calc R . . C12 C -0.3333(2) 0.18218(16) 0.24777(13) 0.0203(3) Uani 1 1 d . . . H12A H -0.2652 0.1609 0.3170 0.024 Uiso 1 1 calc R . . H12B H -0.2638 0.2095 0.1896 0.024 Uiso 1 1 calc R . . C13 C -0.22755(18) -0.25963(15) 0.18806(11) 0.0151(2) Uani 1 1 d . . . H13 H -0.2759 -0.2888 0.2573 0.018 Uiso 1 1 calc R . . C14 C -0.06796(19) -0.39404(16) 0.16346(13) 0.0198(3) Uani 1 1 d . . . H14A H -0.0151 -0.3650 0.0972 0.024 Uiso 1 1 calc R . . H14B H 0.0225 -0.4272 0.2234 0.024 Uiso 1 1 calc R . . C15 C -0.1265(2) -0.52158(16) 0.14862(14) 0.0239(3) Uani 1 1 d . . . H15A H -0.0244 -0.6031 0.1305 0.029 Uiso 1 1 calc R . . H15B H -0.1699 -0.5564 0.2170 0.029 Uiso 1 1 calc R . . C16 C -0.2737(2) -0.47198(18) 0.05786(14) 0.0249(3) Uani 1 1 d . . . H16A H -0.3136 -0.5526 0.0530 0.030 Uiso 1 1 calc R . . H16B H -0.2263 -0.4473 -0.0119 0.030 Uiso 1 1 calc R . . C17 C -0.4321(2) -0.33773(18) 0.08007(14) 0.0233(3) Uani 1 1 d . . . H17A H -0.4876 -0.3659 0.1455 0.028 Uiso 1 1 calc R . . H17B H -0.5204 -0.3049 0.0190 0.028 Uiso 1 1 calc R . . C18 C -0.3750(2) -0.21037(16) 0.09584(13) 0.0197(3) Uani 1 1 d . . . H18A H -0.4778 -0.1292 0.1137 0.024 Uiso 1 1 calc R . . H18B H -0.3311 -0.1750 0.0278 0.024 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 In1 0.01682(8) 0.01917(8) 0.03227(10) -0.00829(6) -0.00047(6) -0.00313(5) P1 0.01361(15) 0.01294(15) 0.01384(16) -0.00207(12) 0.00127(12) -0.00500(12) C1 0.0152(6) 0.0159(6) 0.0158(6) -0.0014(5) -0.0008(5) -0.0061(5) C2 0.0152(6) 0.0286(7) 0.0216(7) 0.0000(6) 0.0004(5) -0.0090(5) C3 0.0167(6) 0.0289(8) 0.0293(8) -0.0005(6) -0.0043(6) -0.0086(6) C4 0.0206(7) 0.0221(7) 0.0236(7) 0.0012(6) -0.0056(6) -0.0047(5) C5 0.0223(7) 0.0270(7) 0.0178(7) 0.0005(6) -0.0019(5) -0.0081(6) C6 0.0174(6) 0.0236(7) 0.0168(6) 0.0013(5) -0.0005(5) -0.0080(5) C7 0.0160(6) 0.0123(5) 0.0178(6) -0.0030(5) 0.0000(5) -0.0042(5) C8 0.0201(7) 0.0159(6) 0.0336(8) -0.0057(6) 0.0105(6) -0.0052(5) C9 0.0190(7) 0.0227(7) 0.0446(10) -0.0109(7) 0.0094(7) -0.0045(6) C10 0.0232(7) 0.0184(7) 0.0312(8) -0.0083(6) 0.0036(6) -0.0010(5) C11 0.0286(7) 0.0136(6) 0.0246(7) -0.0031(5) -0.0007(6) -0.0028(5) C12 0.0232(7) 0.0152(6) 0.0234(7) -0.0042(5) 0.0023(5) -0.0077(5) C13 0.0158(6) 0.0132(5) 0.0166(6) -0.0034(5) 0.0008(5) -0.0052(5) C14 0.0181(6) 0.0153(6) 0.0246(7) -0.0065(5) -0.0004(5) -0.0032(5) C15 0.0272(7) 0.0152(6) 0.0281(8) -0.0052(6) -0.0027(6) -0.0056(6) C16 0.0316(8) 0.0195(7) 0.0265(8) -0.0084(6) -0.0035(6) -0.0107(6) C17 0.0232(7) 0.0228(7) 0.0269(7) -0.0065(6) -0.0032(6) -0.0110(6) C18 0.0186(6) 0.0166(6) 0.0228(7) -0.0035(5) -0.0041(5) -0.0051(5) _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 In1 P1 2.9869(5) 2 ? In1 P1 2.9869(5) . ? P1 C13 1.8548(14) . ? P1 C7 1.8567(14) . ? P1 C1 1.8674(14) . ? C1 C6 1.536(2) . ? C1 C2 1.543(2) . ? C2 C3 1.528(2) . ? C3 C4 1.528(2) . ? C4 C5 1.522(2) . ? C5 C6 1.527(2) . ? C7 C8 1.531(2) . ? C7 C12 1.5321(19) . ? C8 C9 1.532(2) . ? C9 C10 1.528(2) . ? C10 C11 1.525(2) . ? C11 C12 1.532(2) . ? C13 C18 1.537(2) . ? C13 C14 1.5391(19) . ? C14 C15 1.531(2) . ? C15 C16 1.522(2) . ? C16 C17 1.524(2) . ? C17 C18 1.526(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 P1 In1 P1 180.000(17) 2 . ? C13 P1 C7 103.20(6) . . ? C13 P1 C1 105.80(6) . . ? C7 P1 C1 105.61(6) . . ? C13 P1 In1 113.09(5) . . ? C7 P1 In1 109.73(5) . . ? C1 P1 In1 118.14(5) . . ? C6 C1 C2 110.39(12) . . ? C6 C1 P1 117.27(10) . . ? C2 C1 P1 109.66(10) . . ? C3 C2 C1 111.82(13) . . ? C4 C3 C2 111.65(13) . . ? C5 C4 C3 110.33(13) . . ? C4 C5 C6 111.20(13) . . ? C5 C6 C1 111.50(12) . . ? C8 C7 C12 110.08(12) . . ? C8 C7 P1 117.46(10) . . ? C12 C7 P1 111.82(10) . . ? C7 C8 C9 110.93(13) . . ? C10 C9 C8 110.65(14) . . ? C11 C10 C9 111.19(13) . . ? C10 C11 C12 111.39(12) . . ? C11 C12 C7 110.74(13) . . ? C18 C13 C14 109.76(11) . . ? C18 C13 P1 110.44(9) . . ? C14 C13 P1 110.49(10) . . ? C15 C14 C13 111.27(12) . . ? C16 C15 C14 110.89(13) . . ? C15 C16 C17 111.01(13) . . ? C16 C17 C18 111.78(13) . . ? C17 C18 C13 111.15(12) . . ? 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 P1 In1 P1 C13 -101(100) 2 . . . ? P1 In1 P1 C7 145(100) 2 . . . ? P1 In1 P1 C1 24(100) 2 . . . ? C13 P1 C1 C6 -27.95(12) . . . . ? C7 P1 C1 C6 81.04(12) . . . . ? In1 P1 C1 C6 -155.80(9) . . . . ? C13 P1 C1 C2 98.95(11) . . . . ? C7 P1 C1 C2 -152.06(10) . . . . ? In1 P1 C1 C2 -28.90(11) . . . . ? C6 C1 C2 C3 -53.50(17) . . . . ? P1 C1 C2 C3 175.82(11) . . . . ? C1 C2 C3 C4 54.92(18) . . . . ? C2 C3 C4 C5 -56.25(18) . . . . ? C3 C4 C5 C6 57.27(18) . . . . ? C4 C5 C6 C1 -57.19(17) . . . . ? C2 C1 C6 C5 54.57(16) . . . . ? P1 C1 C6 C5 -178.88(10) . . . . ? C13 P1 C7 C8 49.18(12) . . . . ? C1 P1 C7 C8 -61.67(12) . . . . ? In1 P1 C7 C8 169.98(10) . . . . ? C13 P1 C7 C12 177.84(10) . . . . ? C1 P1 C7 C12 66.99(11) . . . . ? In1 P1 C7 C12 -61.36(10) . . . . ? C12 C7 C8 C9 57.78(17) . . . . ? P1 C7 C8 C9 -172.73(11) . . . . ? C7 C8 C9 C10 -57.11(19) . . . . ? C8 C9 C10 C11 55.62(19) . . . . ? C9 C10 C11 C12 -55.38(18) . . . . ? C10 C11 C12 C7 56.12(17) . . . . ? C8 C7 C12 C11 -57.00(16) . . . . ? P1 C7 C12 C11 170.53(10) . . . . ? C7 P1 C13 C18 57.33(11) . . . . ? C1 P1 C13 C18 168.04(10) . . . . ? In1 P1 C13 C18 -61.15(10) . . . . ? C7 P1 C13 C14 178.95(10) . . . . ? C1 P1 C13 C14 -70.34(11) . . . . ? In1 P1 C13 C14 60.47(10) . . . . ? C18 C13 C14 C15 -56.67(16) . . . . ? P1 C13 C14 C15 -178.70(10) . . . . ? C13 C14 C15 C16 56.94(17) . . . . ? C14 C15 C16 C17 -55.66(18) . . . . ? C15 C16 C17 C18 55.49(18) . . . . ? C16 C17 C18 C13 -55.96(17) . . . . ? C14 C13 C18 C17 55.93(16) . . . . ? P1 C13 C18 C17 177.99(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.541 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.071 data_compound14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 In P Te3' _chemical_formula_weight 1009.33 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' 'In' 'In' -0.7276 1.3100 '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 10.3689(10) _cell_length_b 12.0296(19) _cell_length_c 15.862(2) _cell_angle_alpha 85.164(9) _cell_angle_beta 82.62(2) _cell_angle_gamma 72.022(10) _cell_volume 1864.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.000 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.5194 _exptl_absorpt_correction_T_max 0.6108 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 cad4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7958 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.29 _reflns_number_total 7524 _reflns_number_gt 4484 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7524 _refine_ls_number_parameters 370 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1498 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1700 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.280 _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 In1 In 0.07917(9) 0.74044(8) 0.25244(5) 0.0188(2) Uani 1 1 d . . . Te1 Te 0.18997(9) 0.83042(8) 0.10740(5) 0.0261(2) Uani 1 1 d . . . Te2 Te 0.11444(9) 0.50449(7) 0.25700(5) 0.0224(2) Uani 1 1 d . . . Te3 Te 0.18324(9) 0.78868(8) 0.39259(6) 0.0257(2) Uani 1 1 d . . . P1 P -0.1887(3) 0.8119(3) 0.2880(2) 0.0180(7) Uani 1 1 d . . . C1 C -0.2277(12) 0.6909(12) 0.3565(8) 0.022(3) Uani 1 1 d . . . H1 H -0.1825 0.6186 0.3268 0.027 Uiso 1 1 calc R . . C2 C -0.3825(13) 0.6992(12) 0.3755(9) 0.030(3) Uani 1 1 d . . . H2A H -0.4295 0.7635 0.4120 0.036 Uiso 1 1 calc R . . H2B H -0.4245 0.7132 0.3228 0.036 Uiso 1 1 calc R . . C3 C -0.3934(14) 0.5817(14) 0.4203(10) 0.040(4) Uani 1 1 d . . . H3A H -0.4884 0.5846 0.4331 0.048 Uiso 1 1 calc R . . H3B H -0.3481 0.5174 0.3835 0.048 Uiso 1 1 calc R . . C4 C -0.3242(14) 0.5632(13) 0.5040(9) 0.033(3) Uani 1 1 d . . . H4A H -0.3737 0.6254 0.5417 0.040 Uiso 1 1 calc R . . H4B H -0.3283 0.4895 0.5325 0.040 Uiso 1 1 calc R . . C5 C -0.1754(14) 0.5621(14) 0.4864(9) 0.034(4) Uani 1 1 d . . . H5A H -0.1349 0.5501 0.5396 0.041 Uiso 1 1 calc R . . H5B H -0.1247 0.4981 0.4506 0.041 Uiso 1 1 calc R . . C6 C -0.1667(13) 0.6767(13) 0.4428(7) 0.026(3) Uani 1 1 d . . . H6A H -0.0724 0.6766 0.4330 0.031 Uiso 1 1 calc R . . H6B H -0.2174 0.7412 0.4782 0.031 Uiso 1 1 calc R . . C7 C -0.2879(11) 0.8299(10) 0.1965(7) 0.015(3) Uani 1 1 d . . . H7 H -0.3846 0.8511 0.2187 0.018 Uiso 1 1 calc R . . C8 C -0.2528(13) 0.7133(11) 0.1543(7) 0.023(3) Uani 1 1 d . . . H8A H -0.1562 0.6874 0.1347 0.028 Uiso 1 1 calc R . . H8B H -0.2724 0.6548 0.1956 0.028 Uiso 1 1 calc R . . C9 C -0.3345(14) 0.7257(12) 0.0800(9) 0.030(3) Uani 1 1 d . . . H9A H -0.3054 0.6522 0.0516 0.036 Uiso 1 1 calc R . . H9B H -0.4300 0.7407 0.1013 0.036 Uiso 1 1 calc R . . C10 C -0.3205(14) 0.8211(13) 0.0166(8) 0.030(3) Uani 1 1 d . . . H10A H -0.3806 0.8282 -0.0269 0.036 Uiso 1 1 calc R . . H10B H -0.2276 0.8012 -0.0107 0.036 Uiso 1 1 calc R . . C11 C -0.3552(13) 0.9377(12) 0.0582(7) 0.025(3) Uani 1 1 d . . . H11A H -0.3371 0.9964 0.0165 0.029 Uiso 1 1 calc R . . H11B H -0.4513 0.9631 0.0791 0.029 Uiso 1 1 calc R . . C12 C -0.2700(13) 0.9248(12) 0.1313(7) 0.023(3) Uani 1 1 d . . . H12A H -0.1746 0.9067 0.1090 0.027 Uiso 1 1 calc R . . H12B H -0.2956 0.9987 0.1589 0.027 Uiso 1 1 calc R . . C13 C -0.2408(12) 0.9466(11) 0.3471(8) 0.021(3) Uani 1 1 d . . . H13 H -0.2105 0.9239 0.4038 0.025 Uiso 1 1 calc R . . C14 C -0.3960(12) 1.0046(12) 0.3608(9) 0.027(3) Uani 1 1 d . . . H14A H -0.4307 1.0308 0.3062 0.032 Uiso 1 1 calc R . . H14B H -0.4399 0.9480 0.3874 0.032 Uiso 1 1 calc R . . C15 C -0.4292(14) 1.1076(14) 0.4165(10) 0.037(4) Uani 1 1 d . . . H15A H -0.4014 1.0799 0.4726 0.045 Uiso 1 1 calc R . . H15B H -0.5271 1.1448 0.4229 0.045 Uiso 1 1 calc R . . C16 C -0.3586(14) 1.1972(12) 0.3800(9) 0.035(4) Uani 1 1 d . . . H16A H -0.3945 1.2316 0.3270 0.042 Uiso 1 1 calc R . . H16B H -0.3788 1.2593 0.4193 0.042 Uiso 1 1 calc R . . C17 C -0.2053(13) 1.1439(12) 0.3635(9) 0.031(3) Uani 1 1 d . . . H17A H -0.1670 1.1204 0.4172 0.037 Uiso 1 1 calc R . . H17B H -0.1654 1.2017 0.3345 0.037 Uiso 1 1 calc R . . C18 C -0.1696(13) 1.0353(12) 0.3078(9) 0.026(3) Uani 1 1 d . . . H18A H -0.1971 1.0607 0.2514 0.032 Uiso 1 1 calc R . . H18B H -0.0717 0.9983 0.3021 0.032 Uiso 1 1 calc R . . C19 C 0.1068(12) 0.7681(12) 0.0120(7) 0.021(3) Uani 1 1 d . . . C20 C 0.0605(13) 0.8503(12) -0.0549(8) 0.025(3) Uani 1 1 d . . . H20 H 0.0591 0.9277 -0.0527 0.030 Uiso 1 1 calc R . . C21 C 0.0166(14) 0.8134(13) -0.1248(9) 0.032(3) Uani 1 1 d . . . H21 H -0.0116 0.8663 -0.1699 0.039 Uiso 1 1 calc R . . C22 C 0.0150(13) 0.7014(13) -0.1270(9) 0.029(3) Uani 1 1 d . . . H22 H -0.0144 0.6783 -0.1737 0.035 Uiso 1 1 calc R . . C23 C 0.0564(14) 0.6214(13) -0.0608(9) 0.035(4) Uani 1 1 d . . . H23 H 0.0530 0.5453 -0.0626 0.042 Uiso 1 1 calc R . . C24 C 0.1037(13) 0.6546(11) 0.0093(9) 0.028(3) Uani 1 1 d . . . H24 H 0.1328 0.6005 0.0536 0.033 Uiso 1 1 calc R . . C25 C 0.3207(13) 0.4550(10) 0.2052(8) 0.021(3) Uani 1 1 d . . . C26 C 0.4188(14) 0.4839(11) 0.2437(8) 0.027(3) Uani 1 1 d U . . H26 H 0.3931 0.5254 0.2931 0.033 Uiso 1 1 calc R . . C27 C 0.5553(15) 0.4514(15) 0.2089(10) 0.045(4) Uani 1 1 d . . . H27 H 0.6191 0.4750 0.2332 0.054 Uiso 1 1 calc R . . C28 C 0.5951(15) 0.3838(17) 0.1381(10) 0.051(5) Uani 1 1 d . . . H28 H 0.6864 0.3564 0.1167 0.061 Uiso 1 1 calc R . . C29 C 0.4992(17) 0.3590(18) 0.1013(11) 0.060(6) Uani 1 1 d . . . H29 H 0.5250 0.3179 0.0517 0.072 Uiso 1 1 calc R . . C30 C 0.3625(16) 0.3918(14) 0.1337(9) 0.041(4) Uani 1 1 d . . . H30 H 0.2995 0.3708 0.1067 0.050 Uiso 1 1 calc R . . C31 C 0.2141(12) 0.9519(11) 0.3462(8) 0.021(3) Uani 1 1 d U . . C32 C 0.1496(15) 1.0519(13) 0.3889(9) 0.033(3) Uani 1 1 d . . . H32 H 0.0929 1.0491 0.4389 0.039 Uiso 1 1 calc R . . C33 C 0.1689(16) 1.1565(12) 0.3575(11) 0.040(4) Uani 1 1 d . . . H33 H 0.1233 1.2245 0.3859 0.048 Uiso 1 1 calc R . . C34 C 0.2559(16) 1.1614(14) 0.2838(11) 0.043(4) Uani 1 1 d . . . H34 H 0.2708 1.2316 0.2632 0.052 Uiso 1 1 calc R . . C35 C 0.3185(14) 1.0611(13) 0.2424(10) 0.038(4) Uani 1 1 d . . . H35 H 0.3764 1.0638 0.1929 0.046 Uiso 1 1 calc R . . C36 C 0.2995(13) 0.9572(13) 0.2709(9) 0.032(3) Uani 1 1 d . . . H36 H 0.3427 0.8902 0.2408 0.038 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 In1 0.0188(5) 0.0201(5) 0.0175(5) -0.0031(4) -0.0023(4) -0.0050(4) Te1 0.0277(5) 0.0352(5) 0.0205(5) 0.0008(4) -0.0039(4) -0.0169(4) Te2 0.0208(5) 0.0195(4) 0.0264(5) -0.0054(4) 0.0026(4) -0.0061(4) Te3 0.0286(5) 0.0282(5) 0.0237(5) -0.0009(4) -0.0114(4) -0.0102(4) P1 0.0122(16) 0.0240(17) 0.0170(16) -0.0005(13) -0.0026(13) -0.0040(13) C1 0.007(6) 0.032(7) 0.029(7) 0.005(6) 0.000(5) -0.011(5) C2 0.025(7) 0.035(8) 0.034(8) 0.020(6) -0.017(6) -0.015(6) C3 0.016(7) 0.057(10) 0.048(9) 0.017(8) -0.006(7) -0.014(7) C4 0.024(8) 0.039(9) 0.037(8) 0.011(7) -0.005(6) -0.014(7) C5 0.025(8) 0.053(10) 0.024(7) 0.021(7) -0.012(6) -0.012(7) C6 0.020(7) 0.051(9) 0.012(6) 0.000(6) -0.004(5) -0.018(7) C7 0.009(6) 0.023(6) 0.017(6) -0.014(5) -0.005(5) -0.004(5) C8 0.030(7) 0.031(7) 0.009(6) -0.008(5) -0.007(5) -0.007(6) C9 0.030(8) 0.026(7) 0.040(9) -0.006(6) -0.014(7) -0.012(6) C10 0.027(8) 0.051(9) 0.018(7) -0.014(6) -0.005(6) -0.015(7) C11 0.026(7) 0.035(8) 0.012(6) 0.009(6) -0.008(5) -0.009(6) C12 0.024(7) 0.036(8) 0.010(6) -0.008(5) -0.006(5) -0.008(6) C13 0.013(6) 0.033(7) 0.016(6) -0.005(5) -0.001(5) -0.004(6) C14 0.010(6) 0.031(8) 0.039(8) -0.016(6) 0.009(6) -0.007(6) C15 0.016(7) 0.051(10) 0.043(9) -0.017(8) 0.014(6) -0.010(7) C16 0.027(8) 0.029(8) 0.038(8) -0.015(7) -0.002(7) 0.010(6) C17 0.022(7) 0.027(8) 0.040(9) -0.009(7) 0.001(6) -0.003(6) C18 0.020(7) 0.033(8) 0.032(8) 0.000(6) -0.009(6) -0.015(6) C19 0.015(6) 0.042(8) 0.013(6) -0.008(6) 0.006(5) -0.019(6) C20 0.024(7) 0.027(7) 0.027(7) -0.004(6) 0.002(6) -0.014(6) C21 0.027(8) 0.044(9) 0.026(8) 0.006(7) -0.006(6) -0.014(7) C22 0.025(8) 0.041(9) 0.028(8) -0.014(7) 0.004(6) -0.018(7) C23 0.034(8) 0.033(8) 0.045(9) -0.009(7) 0.007(7) -0.024(7) C24 0.028(8) 0.019(7) 0.029(7) -0.001(6) 0.005(6) -0.001(6) C25 0.024(7) 0.013(6) 0.026(7) 0.002(5) -0.002(6) -0.006(5) C26 0.032(5) 0.027(5) 0.023(5) -0.008(4) -0.002(4) -0.007(4) C27 0.031(9) 0.064(12) 0.047(10) -0.013(9) -0.010(8) -0.020(8) C28 0.019(8) 0.093(14) 0.043(10) -0.043(10) 0.010(7) -0.016(9) C29 0.031(9) 0.097(16) 0.049(11) -0.047(11) 0.012(8) -0.010(10) C30 0.037(9) 0.057(11) 0.033(9) -0.010(8) -0.002(7) -0.018(8) C31 0.018(4) 0.023(4) 0.025(5) -0.003(4) -0.010(4) -0.007(4) C32 0.035(9) 0.038(9) 0.025(8) -0.002(7) -0.012(6) -0.010(7) C33 0.048(10) 0.011(7) 0.066(11) -0.004(7) -0.029(9) -0.007(7) C34 0.039(9) 0.032(9) 0.069(12) 0.010(8) -0.028(9) -0.022(8) C35 0.026(8) 0.044(10) 0.050(10) 0.014(8) -0.016(7) -0.018(7) C36 0.018(7) 0.039(9) 0.042(9) -0.008(7) -0.011(6) -0.009(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 In1 P1 2.642(3) . ? In1 Te1 2.7301(13) . ? In1 Te2 2.7435(13) . ? In1 Te3 2.7681(13) . ? Te1 C19 2.126(12) . ? Te2 C25 2.109(12) . ? Te3 C31 2.140(13) . ? P1 C13 1.838(13) . ? P1 C7 1.845(11) . ? P1 C1 1.857(12) . ? C1 C6 1.554(16) . ? C1 C2 1.568(16) . ? C2 C3 1.558(19) . ? C3 C4 1.557(19) . ? C4 C5 1.529(18) . ? C5 C6 1.513(18) . ? C7 C12 1.513(17) . ? C7 C8 1.525(16) . ? C8 C9 1.511(17) . ? C9 C10 1.490(19) . ? C10 C11 1.521(18) . ? C11 C12 1.515(16) . ? C13 C18 1.526(17) . ? C13 C14 1.539(16) . ? C14 C15 1.510(18) . ? C15 C16 1.52(2) . ? C16 C17 1.517(18) . ? C17 C18 1.560(18) . ? C19 C24 1.380(17) . ? C19 C20 1.413(18) . ? C20 C21 1.402(18) . ? C21 C22 1.356(19) . ? C22 C23 1.38(2) . ? C23 C24 1.405(19) . ? C25 C30 1.367(18) . ? C25 C26 1.394(17) . ? C26 C27 1.398(19) . ? C27 C28 1.39(2) . ? C28 C29 1.33(2) . ? C29 C30 1.39(2) . ? C31 C32 1.370(18) . ? C31 C36 1.402(18) . ? C32 C33 1.377(19) . ? C33 C34 1.39(2) . ? C34 C35 1.36(2) . ? C35 C36 1.356(19) . ? 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 In1 Te1 118.06(8) . . ? P1 In1 Te2 98.05(8) . . ? Te1 In1 Te2 115.66(4) . . ? P1 In1 Te3 105.72(8) . . ? Te1 In1 Te3 109.96(4) . . ? Te2 In1 Te3 108.31(4) . . ? C19 Te1 In1 101.6(3) . . ? C25 Te2 In1 96.4(3) . . ? C31 Te3 In1 98.6(3) . . ? C13 P1 C7 110.9(5) . . ? C13 P1 C1 110.1(6) . . ? C7 P1 C1 105.4(6) . . ? C13 P1 In1 110.0(4) . . ? C7 P1 In1 115.7(4) . . ? C1 P1 In1 104.4(4) . . ? C6 C1 C2 108.4(10) . . ? C6 C1 P1 111.3(8) . . ? C2 C1 P1 115.9(8) . . ? C3 C2 C1 108.4(10) . . ? C4 C3 C2 107.9(12) . . ? C5 C4 C3 111.5(11) . . ? C6 C5 C4 110.2(11) . . ? C5 C6 C1 108.1(11) . . ? C12 C7 C8 110.3(10) . . ? C12 C7 P1 114.3(8) . . ? C8 C7 P1 109.5(8) . . ? C9 C8 C7 110.4(10) . . ? C10 C9 C8 113.5(11) . . ? C9 C10 C11 111.6(11) . . ? C12 C11 C10 109.7(11) . . ? C7 C12 C11 112.4(10) . . ? C18 C13 C14 110.4(11) . . ? C18 C13 P1 112.4(8) . . ? C14 C13 P1 114.1(8) . . ? C15 C14 C13 110.2(11) . . ? C14 C15 C16 112.1(11) . . ? C17 C16 C15 112.3(12) . . ? C16 C17 C18 110.4(11) . . ? C13 C18 C17 111.4(11) . . ? C24 C19 C20 119.8(12) . . ? C24 C19 Te1 124.8(10) . . ? C20 C19 Te1 115.2(9) . . ? C21 C20 C19 119.0(12) . . ? C22 C21 C20 120.6(13) . . ? C21 C22 C23 120.8(13) . . ? C22 C23 C24 120.1(13) . . ? C19 C24 C23 119.6(13) . . ? C30 C25 C26 118.0(12) . . ? C30 C25 Te2 120.9(10) . . ? C26 C25 Te2 121.0(9) . . ? C25 C26 C27 120.8(12) . . ? C28 C27 C26 119.6(13) . . ? C29 C28 C27 118.4(14) . . ? C28 C29 C30 123.0(15) . . ? C25 C30 C29 119.9(14) . . ? C32 C31 C36 119.5(13) . . ? C32 C31 Te3 120.6(10) . . ? C36 C31 Te3 119.9(10) . . ? C31 C32 C33 119.9(14) . . ? C32 C33 C34 120.6(14) . . ? C35 C34 C33 118.4(14) . . ? C36 C35 C34 122.3(15) . . ? C35 C36 C31 119.3(14) . . ? 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 P1 In1 Te1 C19 -63.4(4) . . . . ? Te2 In1 Te1 C19 52.2(4) . . . . ? Te3 In1 Te1 C19 175.2(4) . . . . ? P1 In1 Te2 C25 169.5(4) . . . . ? Te1 In1 Te2 C25 43.0(4) . . . . ? Te3 In1 Te2 C25 -80.9(3) . . . . ? P1 In1 Te3 C31 -97.0(4) . . . . ? Te1 In1 Te3 C31 31.4(3) . . . . ? Te2 In1 Te3 C31 158.7(3) . . . . ? Te1 In1 P1 C13 -86.6(4) . . . . ? Te2 In1 P1 C13 148.6(4) . . . . ? Te3 In1 P1 C13 36.9(4) . . . . ? Te1 In1 P1 C7 40.0(4) . . . . ? Te2 In1 P1 C7 -84.8(4) . . . . ? Te3 In1 P1 C7 163.5(4) . . . . ? Te1 In1 P1 C1 155.4(4) . . . . ? Te2 In1 P1 C1 30.5(4) . . . . ? Te3 In1 P1 C1 -81.1(4) . . . . ? C13 P1 C1 C6 -52.6(10) . . . . ? C7 P1 C1 C6 -172.2(9) . . . . ? In1 P1 C1 C6 65.4(9) . . . . ? C13 P1 C1 C2 71.9(11) . . . . ? C7 P1 C1 C2 -47.8(11) . . . . ? In1 P1 C1 C2 -170.1(9) . . . . ? C6 C1 C2 C3 -63.4(15) . . . . ? P1 C1 C2 C3 170.7(10) . . . . ? C1 C2 C3 C4 59.4(15) . . . . ? C2 C3 C4 C5 -57.9(16) . . . . ? C3 C4 C5 C6 59.5(17) . . . . ? C4 C5 C6 C1 -61.2(15) . . . . ? C2 C1 C6 C5 63.5(14) . . . . ? P1 C1 C6 C5 -167.9(9) . . . . ? C13 P1 C7 C12 61.4(10) . . . . ? C1 P1 C7 C12 -179.5(9) . . . . ? In1 P1 C7 C12 -64.8(9) . . . . ? C13 P1 C7 C8 -174.2(8) . . . . ? C1 P1 C7 C8 -55.1(10) . . . . ? In1 P1 C7 C8 59.6(9) . . . . ? C12 C7 C8 C9 -54.2(14) . . . . ? P1 C7 C8 C9 179.2(9) . . . . ? C7 C8 C9 C10 54.2(16) . . . . ? C8 C9 C10 C11 -54.6(16) . . . . ? C9 C10 C11 C12 54.2(14) . . . . ? C8 C7 C12 C11 57.0(14) . . . . ? P1 C7 C12 C11 -179.0(9) . . . . ? C10 C11 C12 C7 -56.4(14) . . . . ? C7 P1 C13 C18 -83.6(10) . . . . ? C1 P1 C13 C18 160.1(8) . . . . ? In1 P1 C13 C18 45.7(9) . . . . ? C7 P1 C13 C14 43.1(11) . . . . ? C1 P1 C13 C14 -73.2(10) . . . . ? In1 P1 C13 C14 172.4(8) . . . . ? C18 C13 C14 C15 -57.5(15) . . . . ? P1 C13 C14 C15 174.8(10) . . . . ? C13 C14 C15 C16 56.9(16) . . . . ? C14 C15 C16 C17 -55.7(17) . . . . ? C15 C16 C17 C18 53.0(16) . . . . ? C14 C13 C18 C17 56.4(14) . . . . ? P1 C13 C18 C17 -174.9(9) . . . . ? C16 C17 C18 C13 -54.1(15) . . . . ? In1 Te1 C19 C24 -46.7(11) . . . . ? In1 Te1 C19 C20 137.5(8) . . . . ? C24 C19 C20 C21 -2.3(18) . . . . ? Te1 C19 C20 C21 173.8(9) . . . . ? C19 C20 C21 C22 2(2) . . . . ? C20 C21 C22 C23 0(2) . . . . ? C21 C22 C23 C24 -1(2) . . . . ? C20 C19 C24 C23 1.0(19) . . . . ? Te1 C19 C24 C23 -174.7(10) . . . . ? C22 C23 C24 C19 1(2) . . . . ? In1 Te2 C25 C30 -123.6(11) . . . . ? In1 Te2 C25 C26 57.5(10) . . . . ? C30 C25 C26 C27 1(2) . . . . ? Te2 C25 C26 C27 -179.7(11) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C26 C27 C28 C29 5(3) . . . . ? C27 C28 C29 C30 -4(3) . . . . ? C26 C25 C30 C29 0(2) . . . . ? Te2 C25 C30 C29 -179.2(13) . . . . ? C28 C29 C30 C25 2(3) . . . . ? In1 Te3 C31 C32 120.5(10) . . . . ? In1 Te3 C31 C36 -58.7(10) . . . . ? C36 C31 C32 C33 0.1(19) . . . . ? Te3 C31 C32 C33 -179.0(10) . . . . ? C31 C32 C33 C34 -1(2) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C33 C34 C35 C36 0(2) . . . . ? C34 C35 C36 C31 -1(2) . . . . ? C32 C31 C36 C35 1.1(19) . . . . ? Te3 C31 C36 C35 -179.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.746 _refine_diff_density_min -2.069 #(near In1) _refine_diff_density_rms 0.333 data_cmpound11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 In3 P3' _chemical_formula_weight 942.31 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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2825(9) _cell_length_b 30.403(2) _cell_length_c 13.5672(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.14(2) _cell_angle_gamma 90.00 _cell_volume 4230.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type difabs _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7801 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 cad4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8567 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.30 _reflns_number_total 8567 _reflns_number_gt 7053 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+1.4092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8567 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 1.01113(7) 0.10703(2) 0.32084(5) 0.01392(15) Uani 1 1 d . . . P2 P 1.08550(7) 0.22498(2) 0.17244(6) 0.01364(15) Uani 1 1 d . . . P3 P 0.99623(7) 0.10706(2) 0.02130(6) 0.01384(15) Uani 1 1 d . . . In1 In 0.93771(2) 0.059878(7) 0.168605(15) 0.01625(6) Uani 1 1 d . . . H1' H 1.038(4) 0.0123(16) 0.173(3) 0.066(15) Uiso 1 1 d . . . H2' H 0.774(4) 0.0505(14) 0.158(3) 0.052(13) Uiso 1 1 d . . . In2 In 1.14934(2) 0.178660(7) 0.327585(15) 0.01536(6) Uani 1 1 d . . . H3' H 1.106(4) 0.2016(13) 0.429(3) 0.037(11) Uiso 1 1 d . . . H4' H 1.312(4) 0.1631(15) 0.328(3) 0.064(14) Uiso 1 1 d . . . In3 In 0.95099(2) 0.191338(7) 0.022537(16) 0.01674(6) Uani 1 1 d . . . H5' H 1.021(5) 0.2124(17) -0.085(4) 0.082(17) Uiso 1 1 d . . . H6' H 0.793(5) 0.1978(16) 0.028(4) 0.077(17) Uiso 1 1 d . . . C1 C 0.8592(3) 0.12206(9) 0.3795(2) 0.0149(6) Uani 1 1 d . . . H1 H 0.8836 0.1416 0.4353 0.018 Uiso 1 1 calc R . . C2 C 0.7859(3) 0.08291(10) 0.4195(2) 0.0176(6) Uani 1 1 d . . . H2A H 0.8421 0.0676 0.4686 0.021 Uiso 1 1 calc R . . H2B H 0.7625 0.0626 0.3660 0.021 Uiso 1 1 calc R . . C3 C 0.6622(3) 0.09815(11) 0.4661(2) 0.0225(7) Uani 1 1 d . . . H3A H 0.6150 0.0726 0.4873 0.027 Uiso 1 1 calc R . . H3B H 0.6865 0.1158 0.5240 0.027 Uiso 1 1 calc R . . C4 C 0.5739(3) 0.12491(11) 0.3944(2) 0.0247(7) Uani 1 1 d . . . H4A H 0.5002 0.1357 0.4281 0.030 Uiso 1 1 calc R . . H4B H 0.5406 0.1062 0.3404 0.030 Uiso 1 1 calc R . . C5 C 0.6468(3) 0.16387(11) 0.3528(3) 0.0274(7) Uani 1 1 d . . . H5A H 0.6712 0.1845 0.4055 0.033 Uiso 1 1 calc R . . H5B H 0.5900 0.1790 0.3037 0.033 Uiso 1 1 calc R . . C6 C 0.7694(3) 0.14803(10) 0.3055(2) 0.0209(7) Uani 1 1 d . . . H6A H 0.7443 0.1295 0.2491 0.025 Uiso 1 1 calc R . . H6B H 0.8162 0.1732 0.2821 0.025 Uiso 1 1 calc R . . C7 C 1.0998(3) 0.06791(9) 0.4077(2) 0.0148(6) Uani 1 1 d . . . H7 H 1.0443 0.0419 0.4126 0.018 Uiso 1 1 calc R . . C8 C 1.2264(3) 0.05270(10) 0.3666(2) 0.0184(6) Uani 1 1 d . . . H8A H 1.2835 0.0778 0.3603 0.022 Uiso 1 1 calc R . . H8B H 1.2074 0.0402 0.3013 0.022 Uiso 1 1 calc R . . C9 C 1.2958(3) 0.01805(10) 0.4345(2) 0.0216(7) Uani 1 1 d . . . H9A H 1.2434 -0.0085 0.4338 0.026 Uiso 1 1 calc R . . H9B H 1.3790 0.0107 0.4094 0.026 Uiso 1 1 calc R . . C10 C 1.3180(3) 0.03442(11) 0.5395(2) 0.0247(7) Uani 1 1 d . . . H10A H 1.3817 0.0580 0.5417 0.030 Uiso 1 1 calc R . . H10B H 1.3535 0.0107 0.5810 0.030 Uiso 1 1 calc R . . C11 C 1.1935(3) 0.05110(10) 0.5805(2) 0.0227(7) Uani 1 1 d . . . H11A H 1.2139 0.0637 0.6454 0.027 Uiso 1 1 calc R . . H11B H 1.1342 0.0267 0.5874 0.027 Uiso 1 1 calc R . . C12 C 1.1271(3) 0.08600(10) 0.5122(2) 0.0201(6) Uani 1 1 d . . . H12A H 1.0457 0.0950 0.5381 0.024 Uiso 1 1 calc R . . H12B H 1.1829 0.1117 0.5102 0.024 Uiso 1 1 calc R . . C13 C 1.0002(3) 0.27516(9) 0.2135(2) 0.0152(6) Uani 1 1 d . . . H13 H 1.0567 0.2889 0.2661 0.018 Uiso 1 1 calc R . . C14 C 0.8715(3) 0.26377(10) 0.2570(2) 0.0183(6) Uani 1 1 d . . . H14A H 0.8880 0.2436 0.3118 0.022 Uiso 1 1 calc R . . H14B H 0.8146 0.2492 0.2071 0.022 Uiso 1 1 calc R . . C15 C 0.8038(3) 0.30492(11) 0.2930(3) 0.0235(7) Uani 1 1 d . . . H15A H 0.7206 0.2967 0.3171 0.028 Uiso 1 1 calc R . . H15B H 0.8568 0.3179 0.3475 0.028 Uiso 1 1 calc R . . C16 C 0.7817(3) 0.33863(10) 0.2109(3) 0.0234(7) Uani 1 1 d . . . H16A H 0.7434 0.3650 0.2369 0.028 Uiso 1 1 calc R . . H16B H 0.7211 0.3269 0.1594 0.028 Uiso 1 1 calc R . . C17 C 0.9092(3) 0.35028(10) 0.1674(3) 0.0271(8) Uani 1 1 d . . . H17A H 0.9664 0.3648 0.2173 0.033 Uiso 1 1 calc R . . H17B H 0.8922 0.3706 0.1129 0.033 Uiso 1 1 calc R . . C18 C 0.9771(3) 0.30923(10) 0.1304(3) 0.0226(7) Uani 1 1 d . . . H18A H 1.0601 0.3175 0.1060 0.027 Uiso 1 1 calc R . . H18B H 0.9237 0.2963 0.0761 0.027 Uiso 1 1 calc R . . C19 C 1.2378(3) 0.24665(9) 0.1244(2) 0.0155(6) Uani 1 1 d . . . H19 H 1.2126 0.2657 0.0680 0.019 Uiso 1 1 calc R . . C20 C 1.3194(3) 0.27440(10) 0.2006(2) 0.0197(7) Uani 1 1 d . . . H20A H 1.2681 0.2992 0.2204 0.024 Uiso 1 1 calc R . . H20B H 1.3420 0.2567 0.2589 0.024 Uiso 1 1 calc R . . C21 C 1.4441(3) 0.29114(10) 0.1582(2) 0.0215(7) Uani 1 1 d . . . H21A H 1.4214 0.3113 0.1043 0.026 Uiso 1 1 calc R . . H21B H 1.4959 0.3071 0.2090 0.026 Uiso 1 1 calc R . . C22 C 1.5243(3) 0.25359(10) 0.1208(2) 0.0193(6) Uani 1 1 d . . . H22A H 1.5545 0.2350 0.1758 0.023 Uiso 1 1 calc R . . H22B H 1.6002 0.2653 0.0913 0.023 Uiso 1 1 calc R . . C23 C 1.4438(3) 0.22633(11) 0.0444(2) 0.0220(7) Uani 1 1 d . . . H23A H 1.4204 0.2443 -0.0132 0.026 Uiso 1 1 calc R . . H23B H 1.4956 0.2018 0.0237 0.026 Uiso 1 1 calc R . . C24 C 1.3206(3) 0.20904(10) 0.0865(2) 0.0183(6) Uani 1 1 d . . . H24A H 1.3442 0.1889 0.1403 0.022 Uiso 1 1 calc R . . H24B H 1.2696 0.1929 0.0356 0.022 Uiso 1 1 calc R . . C25 C 1.1706(3) 0.09652(10) 0.0003(2) 0.0153(6) Uani 1 1 d . . . H25 H 1.2003 0.1203 -0.0413 0.018 Uiso 1 1 calc R . . C26 C 1.1962(3) 0.05291(10) -0.0513(2) 0.0198(6) Uani 1 1 d . . . H26A H 1.1461 0.0518 -0.1146 0.024 Uiso 1 1 calc R . . H26B H 1.1687 0.0286 -0.0113 0.024 Uiso 1 1 calc R . . C27 C 1.3418(3) 0.04835(11) -0.0669(3) 0.0245(7) Uani 1 1 d . . . H27A H 1.3572 0.0202 -0.0977 0.029 Uiso 1 1 calc R . . H27B H 1.3672 0.0713 -0.1113 0.029 Uiso 1 1 calc R . . C28 C 1.4253(3) 0.05160(11) 0.0305(3) 0.0233(7) Uani 1 1 d . . . H28A H 1.4069 0.0268 0.0721 0.028 Uiso 1 1 calc R . . H28B H 1.5167 0.0505 0.0175 0.028 Uiso 1 1 calc R . . C29 C 1.3977(3) 0.09420(11) 0.0841(2) 0.0219(7) Uani 1 1 d . . . H29A H 1.4251 0.1190 0.0458 0.026 Uiso 1 1 calc R . . H29B H 1.4472 0.0947 0.1477 0.026 Uiso 1 1 calc R . . C30 C 1.2523(3) 0.09815(10) 0.0991(2) 0.0175(6) Uani 1 1 d . . . H30A H 1.2361 0.1257 0.1322 0.021 Uiso 1 1 calc R . . H30B H 1.2264 0.0743 0.1410 0.021 Uiso 1 1 calc R . . C31 C 0.9038(3) 0.08484(10) -0.0903(2) 0.0154(6) Uani 1 1 d . . . H31 H 0.9297 0.0540 -0.0972 0.018 Uiso 1 1 calc R . . C32 C 0.7566(3) 0.08555(12) -0.0798(2) 0.0237(7) Uani 1 1 d . . . H32A H 0.7371 0.0695 -0.0209 0.028 Uiso 1 1 calc R . . H32B H 0.7277 0.1157 -0.0728 0.028 Uiso 1 1 calc R . . C33 C 0.6838(3) 0.06476(12) -0.1702(2) 0.0261(7) Uani 1 1 d . . . H33A H 0.7068 0.0339 -0.1736 0.031 Uiso 1 1 calc R . . H33B H 0.5907 0.0667 -0.1637 0.031 Uiso 1 1 calc R . . C34 C 0.7168(3) 0.08751(11) -0.2649(2) 0.0229(7) Uani 1 1 d . . . H34A H 0.6850 0.1176 -0.2647 0.027 Uiso 1 1 calc R . . H34B H 0.6731 0.0725 -0.3210 0.027 Uiso 1 1 calc R . . C35 C 0.8632(3) 0.08772(11) -0.2756(2) 0.0224(7) Uani 1 1 d . . . H35A H 0.8817 0.1041 -0.3343 0.027 Uiso 1 1 calc R . . H35B H 0.8936 0.0578 -0.2830 0.027 Uiso 1 1 calc R . . C36 C 0.9353(3) 0.10876(10) -0.1848(2) 0.0181(6) Uani 1 1 d . . . H36A H 1.0285 0.1076 -0.1916 0.022 Uiso 1 1 calc R . . H36B H 0.9101 0.1394 -0.1805 0.022 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0157(4) 0.0121(4) 0.0142(4) 0.0010(3) 0.0022(3) -0.0004(3) P2 0.0131(3) 0.0102(3) 0.0175(4) 0.0006(3) 0.0002(3) 0.0001(3) P3 0.0138(3) 0.0130(4) 0.0147(4) -0.0003(3) 0.0015(3) 0.0005(3) In1 0.02012(11) 0.01317(11) 0.01555(11) -0.00056(8) 0.00195(8) -0.00308(8) In2 0.01687(11) 0.01134(10) 0.01760(11) 0.00106(8) -0.00058(8) -0.00011(8) In3 0.01714(11) 0.01332(11) 0.01930(11) -0.00104(8) -0.00187(8) 0.00113(8) C1 0.0152(14) 0.0149(14) 0.0148(14) 0.0021(11) 0.0027(11) 0.0015(11) C2 0.0184(15) 0.0169(15) 0.0175(15) 0.0064(12) 0.0022(12) 0.0020(12) C3 0.0203(16) 0.0267(18) 0.0212(16) 0.0061(13) 0.0060(13) 0.0027(13) C4 0.0137(15) 0.0349(19) 0.0255(17) 0.0059(15) 0.0025(13) 0.0077(14) C5 0.0228(17) 0.0251(17) 0.0338(19) 0.0075(15) -0.0010(14) 0.0098(14) C6 0.0204(16) 0.0180(16) 0.0243(17) 0.0083(13) 0.0011(13) 0.0008(12) C7 0.0153(14) 0.0122(14) 0.0165(14) 0.0019(11) -0.0008(11) -0.0003(11) C8 0.0174(15) 0.0154(14) 0.0223(16) -0.0009(12) 0.0021(12) 0.0029(12) C9 0.0200(15) 0.0153(15) 0.0296(18) 0.0031(13) 0.0015(13) 0.0024(12) C10 0.0231(16) 0.0185(16) 0.0311(18) 0.0017(14) -0.0086(14) 0.0017(13) C11 0.0289(17) 0.0191(16) 0.0193(16) 0.0016(13) -0.0033(13) -0.0004(13) C12 0.0209(15) 0.0185(15) 0.0208(16) -0.0010(13) 0.0016(12) 0.0015(12) C13 0.0127(14) 0.0110(14) 0.0220(16) -0.0019(12) 0.0009(12) 0.0010(11) C14 0.0189(15) 0.0164(15) 0.0193(15) 0.0041(12) 0.0000(12) 0.0020(12) C15 0.0174(15) 0.0225(17) 0.0309(18) -0.0001(14) 0.0042(13) 0.0025(13) C16 0.0176(15) 0.0162(16) 0.0367(19) 0.0036(14) 0.0027(14) 0.0019(12) C17 0.0193(16) 0.0144(16) 0.048(2) 0.0078(15) 0.0048(15) 0.0020(13) C18 0.0190(15) 0.0144(15) 0.0347(19) 0.0075(14) 0.0047(14) 0.0007(12) C19 0.0158(14) 0.0110(14) 0.0197(15) 0.0035(12) 0.0012(12) -0.0019(11) C20 0.0166(15) 0.0164(15) 0.0262(17) -0.0056(13) 0.0030(13) -0.0006(12) C21 0.0203(16) 0.0164(15) 0.0280(17) -0.0045(13) 0.0014(13) -0.0052(12) C22 0.0172(14) 0.0206(16) 0.0202(16) -0.0010(12) 0.0027(12) -0.0028(12) C23 0.0195(15) 0.0248(17) 0.0222(16) -0.0050(13) 0.0050(13) -0.0027(13) C24 0.0201(15) 0.0150(15) 0.0201(16) -0.0054(12) 0.0029(12) -0.0039(12) C25 0.0126(13) 0.0150(15) 0.0188(15) 0.0005(12) 0.0045(11) 0.0018(11) C26 0.0203(16) 0.0165(15) 0.0225(16) -0.0045(13) 0.0015(13) 0.0016(12) C27 0.0181(16) 0.0247(17) 0.0311(18) -0.0065(14) 0.0044(13) 0.0031(13) C28 0.0153(15) 0.0203(16) 0.0345(19) 0.0019(14) 0.0024(13) 0.0033(12) C29 0.0132(15) 0.0254(17) 0.0265(17) -0.0005(14) -0.0026(13) -0.0007(12) C30 0.0154(14) 0.0151(15) 0.0217(16) -0.0004(12) -0.0002(12) -0.0012(11) C31 0.0158(14) 0.0158(14) 0.0145(14) -0.0008(11) 0.0012(11) 0.0004(11) C32 0.0185(16) 0.0352(19) 0.0176(16) -0.0010(14) 0.0024(12) -0.0030(14) C33 0.0173(15) 0.038(2) 0.0228(17) 0.0008(15) -0.0030(13) -0.0062(14) C34 0.0232(16) 0.0265(17) 0.0183(16) -0.0005(13) -0.0040(13) 0.0004(13) C35 0.0248(17) 0.0240(17) 0.0180(16) 0.0017(13) -0.0005(13) 0.0011(13) C36 0.0184(15) 0.0196(16) 0.0166(15) 0.0023(12) 0.0030(12) -0.0002(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.861(3) . ? P1 C7 1.865(3) . ? P1 In1 2.5818(8) . ? P1 In2 2.5985(8) . ? P2 C19 1.860(3) . ? P2 C13 1.865(3) . ? P2 In2 2.5778(8) . ? P2 In3 2.5862(9) . ? P3 C31 1.856(3) . ? P3 C25 1.863(3) . ? P3 In1 2.5666(8) . ? P3 In3 2.6044(8) . ? C1 C2 1.529(4) . ? C1 C6 1.532(4) . ? C2 C3 1.532(4) . ? C3 C4 1.518(4) . ? C4 C5 1.531(5) . ? C5 C6 1.533(4) . ? C7 C8 1.525(4) . ? C7 C12 1.527(4) . ? C8 C9 1.541(4) . ? C9 C10 1.511(5) . ? C10 C11 1.519(5) . ? C11 C12 1.536(4) . ? C13 C14 1.527(4) . ? C13 C18 1.537(4) . ? C14 C15 1.529(4) . ? C15 C16 1.519(5) . ? C16 C17 1.519(4) . ? C17 C18 1.532(4) . ? C19 C24 1.536(4) . ? C19 C20 1.536(4) . ? C20 C21 1.530(4) . ? C21 C22 1.517(4) . ? C22 C23 1.524(4) . ? C23 C24 1.520(4) . ? C25 C30 1.530(4) . ? C25 C26 1.531(4) . ? C26 C27 1.533(4) . ? C27 C28 1.526(5) . ? C28 C29 1.522(4) . ? C29 C30 1.529(4) . ? C31 C36 1.529(4) . ? C31 C32 1.531(4) . ? C32 C33 1.527(4) . ? C33 C34 1.518(4) . ? C34 C35 1.523(4) . ? C35 C36 1.531(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C7 105.88(13) . . ? C1 P1 In1 105.80(10) . . ? C7 P1 In1 104.64(9) . . ? C1 P1 In2 104.67(10) . . ? C7 P1 In2 105.73(9) . . ? In1 P1 In2 128.40(3) . . ? C19 P2 C13 103.94(13) . . ? C19 P2 In2 107.97(10) . . ? C13 P2 In2 107.48(10) . . ? C19 P2 In3 106.29(10) . . ? C13 P2 In3 108.81(10) . . ? In2 P2 In3 121.08(3) . . ? C31 P3 C25 104.72(13) . . ? C31 P3 In1 107.27(9) . . ? C25 P3 In1 107.78(10) . . ? C31 P3 In3 106.39(10) . . ? C25 P3 In3 110.15(10) . . ? In1 P3 In3 119.53(3) . . ? P3 In1 P1 103.95(2) . . ? P2 In2 P1 108.83(3) . . ? P2 In3 P3 107.97(2) . . ? C2 C1 C6 110.2(2) . . ? C2 C1 P1 114.3(2) . . ? C6 C1 P1 109.3(2) . . ? C1 C2 C3 110.9(2) . . ? C4 C3 C2 111.9(3) . . ? C3 C4 C5 111.4(3) . . ? C4 C5 C6 110.5(3) . . ? C1 C6 C5 111.3(3) . . ? C8 C7 C12 110.2(2) . . ? C8 C7 P1 110.7(2) . . ? C12 C7 P1 113.9(2) . . ? C7 C8 C9 111.0(2) . . ? C10 C9 C8 111.8(3) . . ? C9 C10 C11 112.4(3) . . ? C10 C11 C12 111.1(3) . . ? C7 C12 C11 110.8(2) . . ? C14 C13 C18 110.1(2) . . ? C14 C13 P2 111.7(2) . . ? C18 C13 P2 112.5(2) . . ? C13 C14 C15 111.4(2) . . ? C16 C15 C14 111.4(3) . . ? C15 C16 C17 110.8(3) . . ? C16 C17 C18 111.4(3) . . ? C17 C18 C13 111.0(3) . . ? C24 C19 C20 110.2(2) . . ? C24 C19 P2 110.78(19) . . ? C20 C19 P2 113.0(2) . . ? C21 C20 C19 111.2(3) . . ? C22 C21 C20 111.5(3) . . ? C21 C22 C23 110.8(3) . . ? C24 C23 C22 111.0(3) . . ? C23 C24 C19 111.4(2) . . ? C30 C25 C26 109.1(2) . . ? C30 C25 P3 109.5(2) . . ? C26 C25 P3 114.7(2) . . ? C25 C26 C27 110.1(2) . . ? C28 C27 C26 111.6(3) . . ? C29 C28 C27 110.9(3) . . ? C28 C29 C30 110.4(2) . . ? C29 C30 C25 111.2(2) . . ? C36 C31 C32 110.0(2) . . ? C36 C31 P3 112.6(2) . . ? C32 C31 P3 111.8(2) . . ? C33 C32 C31 110.5(3) . . ? C34 C33 C32 111.4(3) . . ? C33 C34 C35 111.4(3) . . ? C34 C35 C36 110.5(3) . . ? C31 C36 C35 110.9(2) . . ? 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 C31 P3 In1 P1 -162.98(10) . . . . ? C25 P3 In1 P1 84.74(10) . . . . ? In3 P3 In1 P1 -41.94(4) . . . . ? C1 P1 In1 P3 114.10(10) . . . . ? C7 P1 In1 P3 -134.32(10) . . . . ? In2 P1 In1 P3 -9.95(4) . . . . ? C19 P2 In2 P1 -136.89(10) . . . . ? C13 P2 In2 P1 111.55(10) . . . . ? In3 P2 In2 P1 -14.22(4) . . . . ? C1 P1 In2 P2 -87.56(10) . . . . ? C7 P1 In2 P2 160.87(10) . . . . ? In1 P1 In2 P2 36.94(4) . . . . ? C19 P2 In3 P3 96.57(10) . . . . ? C13 P2 In3 P3 -152.05(10) . . . . ? In2 P2 In3 P3 -26.90(4) . . . . ? C31 P3 In3 P2 -177.51(10) . . . . ? C25 P3 In3 P2 -64.55(10) . . . . ? In1 P3 In3 P2 61.01(4) . . . . ? C7 P1 C1 C2 -46.6(2) . . . . ? In1 P1 C1 C2 64.1(2) . . . . ? In2 P1 C1 C2 -158.08(19) . . . . ? C7 P1 C1 C6 -170.6(2) . . . . ? In1 P1 C1 C6 -59.9(2) . . . . ? In2 P1 C1 C6 77.9(2) . . . . ? C6 C1 C2 C3 -56.3(3) . . . . ? P1 C1 C2 C3 -179.9(2) . . . . ? C1 C2 C3 C4 55.6(4) . . . . ? C2 C3 C4 C5 -54.9(4) . . . . ? C3 C4 C5 C6 55.0(4) . . . . ? C2 C1 C6 C5 57.5(3) . . . . ? P1 C1 C6 C5 -176.1(2) . . . . ? C4 C5 C6 C1 -56.7(4) . . . . ? C1 P1 C7 C8 179.3(2) . . . . ? In1 P1 C7 C8 67.8(2) . . . . ? In2 P1 C7 C8 -70.0(2) . . . . ? C1 P1 C7 C12 -55.9(2) . . . . ? In1 P1 C7 C12 -167.47(19) . . . . ? In2 P1 C7 C12 54.8(2) . . . . ? C12 C7 C8 C9 56.9(3) . . . . ? P1 C7 C8 C9 -176.2(2) . . . . ? C7 C8 C9 C10 -54.5(3) . . . . ? C8 C9 C10 C11 53.0(4) . . . . ? C9 C10 C11 C12 -53.9(4) . . . . ? C8 C7 C12 C11 -58.0(3) . . . . ? P1 C7 C12 C11 177.0(2) . . . . ? C10 C11 C12 C7 56.3(3) . . . . ? C19 P2 C13 C14 -179.4(2) . . . . ? In2 P2 C13 C14 -65.1(2) . . . . ? In3 P2 C13 C14 67.7(2) . . . . ? C19 P2 C13 C18 56.2(2) . . . . ? In2 P2 C13 C18 170.49(18) . . . . ? In3 P2 C13 C18 -56.8(2) . . . . ? C18 C13 C14 C15 -55.7(3) . . . . ? P2 C13 C14 C15 178.5(2) . . . . ? C13 C14 C15 C16 56.2(3) . . . . ? C14 C15 C16 C17 -55.8(4) . . . . ? C15 C16 C17 C18 56.0(4) . . . . ? C16 C17 C18 C13 -56.4(4) . . . . ? C14 C13 C18 C17 55.8(3) . . . . ? P2 C13 C18 C17 -179.0(2) . . . . ? C13 P2 C19 C24 -179.7(2) . . . . ? In2 P2 C19 C24 66.3(2) . . . . ? In3 P2 C19 C24 -65.0(2) . . . . ? C13 P2 C19 C20 56.0(2) . . . . ? In2 P2 C19 C20 -57.9(2) . . . . ? In3 P2 C19 C20 170.77(18) . . . . ? C24 C19 C20 C21 54.9(3) . . . . ? P2 C19 C20 C21 179.5(2) . . . . ? C19 C20 C21 C22 -55.8(3) . . . . ? C20 C21 C22 C23 56.2(3) . . . . ? C21 C22 C23 C24 -56.6(3) . . . . ? C22 C23 C24 C19 56.7(3) . . . . ? C20 C19 C24 C23 -55.7(3) . . . . ? P2 C19 C24 C23 178.5(2) . . . . ? C31 P3 C25 C30 -160.2(2) . . . . ? In1 P3 C25 C30 -46.2(2) . . . . ? In3 P3 C25 C30 85.8(2) . . . . ? C31 P3 C25 C26 -37.2(2) . . . . ? In1 P3 C25 C26 76.8(2) . . . . ? In3 P3 C25 C26 -151.25(19) . . . . ? C30 C25 C26 C27 -58.2(3) . . . . ? P3 C25 C26 C27 178.6(2) . . . . ? C25 C26 C27 C28 57.1(4) . . . . ? C26 C27 C28 C29 -55.5(4) . . . . ? C27 C28 C29 C30 55.3(4) . . . . ? C28 C29 C30 C25 -58.0(3) . . . . ? C26 C25 C30 C29 59.3(3) . . . . ? P3 C25 C30 C29 -174.4(2) . . . . ? C25 P3 C31 C36 -62.8(2) . . . . ? In1 P3 C31 C36 -177.11(18) . . . . ? In3 P3 C31 C36 53.9(2) . . . . ? C25 P3 C31 C32 172.8(2) . . . . ? In1 P3 C31 C32 58.5(2) . . . . ? In3 P3 C31 C32 -70.5(2) . . . . ? C36 C31 C32 C33 57.3(3) . . . . ? P3 C31 C32 C33 -176.8(2) . . . . ? C31 C32 C33 C34 -56.4(4) . . . . ? C32 C33 C34 C35 55.7(4) . . . . ? C33 C34 C35 C36 -55.6(4) . . . . ? C32 C31 C36 C35 -57.9(3) . . . . ? P3 C31 C36 C35 176.7(2) . . . . ? C34 C35 C36 C31 57.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.481 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.101 data_compound12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 In P S3' _chemical_formula_weight 722.71 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' 'In' 'In' -0.7276 1.3100 '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' 'S' 'S' 0.1246 0.1234 '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 11.6650(10) _cell_length_b 33.359(2) _cell_length_c 19.122(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.258(10) _cell_angle_gamma 90.00 _cell_volume 7106.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 cad4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15141 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.31 _reflns_number_total 14420 _reflns_number_gt 9843 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+3.7276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14420 _refine_ls_number_parameters 739 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.014 _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 S1 S 0.37403(8) 0.13477(3) 0.37854(5) 0.0570(2) Uani 1 1 d . . . S2 S 0.02877(8) 0.14243(3) 0.37215(5) 0.0635(3) Uani 1 1 d . . . S3 S 0.20140(10) 0.04981(3) 0.47702(5) 0.0645(3) Uani 1 1 d . . . P1 P 0.28758(6) 0.14954(2) 0.57550(4) 0.03226(16) Uani 1 1 d . . . In1 In 0.228475(19) 0.118996(6) 0.443895(11) 0.03908(6) Uani 1 1 d . . . C1 C 0.5021(3) 0.10325(11) 0.41204(17) 0.0478(8) Uani 1 1 d . . . C2 C 0.6139(3) 0.12009(12) 0.4220(2) 0.0601(10) Uani 1 1 d . . . H2 H 0.6209 0.1475 0.4154 0.072 Uiso 1 1 calc R . . C3 C 0.7167(3) 0.09612(16) 0.4420(2) 0.0730(12) Uani 1 1 d . . . H3 H 0.7917 0.1075 0.4475 0.088 Uiso 1 1 calc R . . C4 C 0.7072(4) 0.05588(16) 0.4534(2) 0.0808(13) Uani 1 1 d . . . H4 H 0.7755 0.0399 0.4671 0.097 Uiso 1 1 calc R . . C5 C 0.5967(5) 0.03941(14) 0.4447(3) 0.0841(14) Uani 1 1 d . . . H5 H 0.5902 0.0122 0.4531 0.101 Uiso 1 1 calc R . . C6 C 0.4941(4) 0.06294(12) 0.4234(2) 0.0669(11) Uani 1 1 d . . . H6 H 0.4192 0.0512 0.4168 0.080 Uiso 1 1 calc R . . C7 C 0.0362(3) 0.19237(11) 0.34293(18) 0.0503(8) Uani 1 1 d . . . C8 C -0.0531(4) 0.21852(14) 0.3465(2) 0.0764(12) Uani 1 1 d . . . H8 H -0.1141 0.2100 0.3652 0.092 Uiso 1 1 calc R . . C9 C -0.0522(5) 0.25765(16) 0.3223(4) 0.1101(19) Uani 1 1 d . . . H9 H -0.1125 0.2751 0.3254 0.132 Uiso 1 1 calc R . . C10 C 0.0346(5) 0.27101(15) 0.2941(3) 0.1037(18) Uani 1 1 d . . . H10 H 0.0339 0.2974 0.2782 0.124 Uiso 1 1 calc R . . C11 C 0.1226(4) 0.24537(13) 0.2895(2) 0.0765(12) Uani 1 1 d . . . H11 H 0.1822 0.2541 0.2698 0.092 Uiso 1 1 calc R . . C12 C 0.1237(3) 0.20628(11) 0.31388(19) 0.0577(9) Uani 1 1 d . . . H12 H 0.1846 0.1891 0.3106 0.069 Uiso 1 1 calc R . . C13 C 0.1151(3) 0.02976(10) 0.3916(2) 0.0557(9) Uani 1 1 d . . . C14 C -0.0052(4) 0.03835(14) 0.3619(3) 0.0918(16) Uani 1 1 d . . . H14 H -0.0434 0.0553 0.3866 0.110 Uiso 1 1 calc R . . C15 C -0.0695(5) 0.02175(17) 0.2951(3) 0.112(2) Uani 1 1 d . . . H15 H -0.1504 0.0278 0.2752 0.135 Uiso 1 1 calc R . . C16 C -0.0154(5) -0.00319(14) 0.2588(3) 0.0988(17) Uani 1 1 d . . . H16 H -0.0593 -0.0145 0.2145 0.119 Uiso 1 1 calc R . . C17 C 0.1023(5) -0.01150(12) 0.2871(2) 0.0758(12) Uani 1 1 d . . . H17 H 0.1397 -0.0285 0.2620 0.091 Uiso 1 1 calc R . . C18 C 0.1673(4) 0.00489(11) 0.3526(2) 0.0635(10) Uani 1 1 d . . . H18 H 0.2487 -0.0010 0.3710 0.076 Uiso 1 1 calc R . . C19 C 0.1906(2) 0.12587(9) 0.62420(16) 0.0376(7) Uani 1 1 d . . . H19 H 0.2052 0.0970 0.6232 0.045 Uiso 1 1 calc R . . C20 C 0.0571(3) 0.13174(12) 0.58493(19) 0.0549(9) Uani 1 1 d . . . H20A H 0.0367 0.1599 0.5859 0.066 Uiso 1 1 calc R . . H20B H 0.0399 0.1236 0.5341 0.066 Uiso 1 1 calc R . . C21 C -0.0186(3) 0.10710(13) 0.6216(2) 0.0608(10) Uani 1 1 d . . . H21A H -0.1029 0.1125 0.5978 0.073 Uiso 1 1 calc R . . H21B H -0.0045 0.0788 0.6157 0.073 Uiso 1 1 calc R . . C22 C 0.0105(3) 0.11669(13) 0.7017(2) 0.0689(11) Uani 1 1 d . . . H22A H -0.0132 0.1441 0.7075 0.083 Uiso 1 1 calc R . . H22B H -0.0350 0.0991 0.7240 0.083 Uiso 1 1 calc R . . C23 C 0.1414(4) 0.11179(16) 0.7400(2) 0.0854(15) Uani 1 1 d . . . H23A H 0.1630 0.0838 0.7391 0.102 Uiso 1 1 calc R . . H23B H 0.1577 0.1198 0.7908 0.102 Uiso 1 1 calc R . . C24 C 0.2183(3) 0.13696(14) 0.70425(18) 0.0679(12) Uani 1 1 d . . . H24A H 0.2019 0.1652 0.7087 0.081 Uiso 1 1 calc R . . H24B H 0.3027 0.1323 0.7291 0.081 Uiso 1 1 calc R . . C25 C 0.2636(3) 0.20425(9) 0.57510(16) 0.0395(7) Uani 1 1 d . . . H25 H 0.1782 0.2079 0.5700 0.047 Uiso 1 1 calc R . . C26 C 0.3313(3) 0.22666(10) 0.64481(17) 0.0532(9) Uani 1 1 d . . . H26A H 0.3134 0.2146 0.6865 0.064 Uiso 1 1 calc R . . H26B H 0.4170 0.2244 0.6523 0.064 Uiso 1 1 calc R . . C27 C 0.2957(4) 0.27074(10) 0.6397(2) 0.0648(11) Uani 1 1 d . . . H27A H 0.2113 0.2730 0.6364 0.078 Uiso 1 1 calc R . . H27B H 0.3418 0.2845 0.6837 0.078 Uiso 1 1 calc R . . C28 C 0.3176(4) 0.29035(11) 0.5736(2) 0.0695(11) Uani 1 1 d . . . H28A H 0.4029 0.2902 0.5789 0.083 Uiso 1 1 calc R . . H28B H 0.2912 0.3180 0.5705 0.083 Uiso 1 1 calc R . . C29 C 0.2507(4) 0.26847(10) 0.5041(2) 0.0582(9) Uani 1 1 d . . . H29A H 0.2692 0.2807 0.4627 0.070 Uiso 1 1 calc R . . H29B H 0.1649 0.2710 0.4963 0.070 Uiso 1 1 calc R . . C30 C 0.2845(3) 0.22434(10) 0.50818(18) 0.0513(8) Uani 1 1 d . . . H30A H 0.3684 0.2218 0.5106 0.062 Uiso 1 1 calc R . . H30B H 0.2370 0.2109 0.4642 0.062 Uiso 1 1 calc R . . C31 C 0.4426(2) 0.13662(9) 0.62801(16) 0.0366(7) Uani 1 1 d . . . H31 H 0.4579 0.1471 0.6778 0.044 Uiso 1 1 calc R . . C32 C 0.5341(3) 0.15541(10) 0.59442(18) 0.0449(8) Uani 1 1 d . . . H32A H 0.5153 0.1474 0.5435 0.054 Uiso 1 1 calc R . . H32B H 0.5282 0.1844 0.5960 0.054 Uiso 1 1 calc R . . C33 C 0.6617(3) 0.14269(10) 0.6349(2) 0.0521(9) Uani 1 1 d . . . H33A H 0.7162 0.1536 0.6101 0.063 Uiso 1 1 calc R . . H33B H 0.6840 0.1535 0.6842 0.063 Uiso 1 1 calc R . . C34 C 0.6741(3) 0.09764(11) 0.6388(2) 0.0559(9) Uani 1 1 d . . . H34A H 0.6600 0.0869 0.5897 0.067 Uiso 1 1 calc R . . H34B H 0.7552 0.0906 0.6672 0.067 Uiso 1 1 calc R . . C35 C 0.5861(3) 0.07926(11) 0.6735(2) 0.0601(10) Uani 1 1 d . . . H35A H 0.6051 0.0881 0.7240 0.072 Uiso 1 1 calc R . . H35B H 0.5936 0.0503 0.6734 0.072 Uiso 1 1 calc R . . C36 C 0.4575(3) 0.09099(10) 0.6328(2) 0.0519(9) Uani 1 1 d . . . H36A H 0.4038 0.0798 0.6579 0.062 Uiso 1 1 calc R . . H36B H 0.4357 0.0798 0.5837 0.062 Uiso 1 1 calc R . . S4 S -0.15029(9) 0.12916(3) -0.14188(5) 0.0637(3) Uani 1 1 d . . . S5 S -0.30446(11) 0.04074(3) -0.04195(6) 0.0736(3) Uani 1 1 d . . . S6 S -0.48684(9) 0.13521(4) -0.13670(6) 0.0716(3) Uani 1 1 d . . . P2 P -0.19560(7) 0.13978(2) 0.06117(4) 0.03932(18) Uani 1 1 d . . . In2 In -0.28605(2) 0.111301(7) -0.070792(12) 0.04342(6) Uani 1 1 d . . . C37 C -0.0112(3) 0.10505(12) -0.09804(18) 0.0536(9) Uani 1 1 d . . . C38 C -0.0017(4) 0.06434(12) -0.0892(2) 0.0694(11) Uani 1 1 d . . . H38 H -0.0703 0.0485 -0.1028 0.083 Uiso 1 1 calc R . . C39 C 0.1095(5) 0.04675(16) -0.0602(3) 0.0925(15) Uani 1 1 d . . . H39 H 0.1148 0.0191 -0.0546 0.111 Uiso 1 1 calc R . . C40 C 0.2108(5) 0.06900(19) -0.0399(3) 0.0914(16) Uani 1 1 d . . . H40 H 0.2852 0.0567 -0.0209 0.110 Uiso 1 1 calc R . . C41 C 0.2032(4) 0.10961(18) -0.0473(2) 0.0851(14) Uani 1 1 d . . . H41 H 0.2726 0.1251 -0.0329 0.102 Uiso 1 1 calc R . . C42 C 0.0921(4) 0.12810(13) -0.0764(2) 0.0668(11) Uani 1 1 d . . . H42 H 0.0874 0.1558 -0.0813 0.080 Uiso 1 1 calc R . . C43 C -0.4162(3) 0.02438(10) -0.1217(2) 0.0561(9) Uani 1 1 d . . . C44 C -0.3851(4) 0.00409(12) -0.1749(2) 0.0686(11) Uani 1 1 d . . . H44 H -0.3042 -0.0006 -0.1693 0.082 Uiso 1 1 calc R . . C45 C -0.4689(5) -0.00963(15) -0.2366(3) 0.0960(16) Uani 1 1 d . . . H45 H -0.4445 -0.0241 -0.2713 0.115 Uiso 1 1 calc R . . C46 C -0.5856(6) -0.00231(17) -0.2475(3) 0.1082(18) Uani 1 1 d U . . H46 H -0.6420 -0.0112 -0.2900 0.130 Uiso 1 1 calc R . . C47 C -0.6211(5) 0.01794(19) -0.1967(4) 0.124(2) Uani 1 1 d U . . H47 H -0.7023 0.0232 -0.2046 0.149 Uiso 1 1 calc R . . C48 C -0.5364(5) 0.03140(16) -0.1312(3) 0.1104(18) Uani 1 1 d U . . H48 H -0.5613 0.0447 -0.0955 0.132 Uiso 1 1 calc R . . C49 C -0.4709(3) 0.18687(12) -0.15323(19) 0.0567(9) Uani 1 1 d . . . C50 C -0.3940(3) 0.20162(13) -0.1888(2) 0.0635(10) Uani 1 1 d . . . H50 H -0.3442 0.1842 -0.2043 0.076 Uiso 1 1 calc R . . C51 C -0.3896(4) 0.24255(15) -0.2021(3) 0.0847(14) Uani 1 1 d . . . H51 H -0.3366 0.2524 -0.2260 0.102 Uiso 1 1 calc R . . C52 C -0.4638(5) 0.26833(16) -0.1799(3) 0.0994(19) Uani 1 1 d . . . H52 H -0.4612 0.2957 -0.1885 0.119 Uiso 1 1 calc R . . C53 C -0.5405(6) 0.25373(19) -0.1455(3) 0.106(2) Uani 1 1 d . . . H53 H -0.5910 0.2711 -0.1305 0.127 Uiso 1 1 calc R . . C54 C -0.5447(4) 0.21378(16) -0.1325(2) 0.0858(14) Uani 1 1 d . . . H54 H -0.5987 0.2043 -0.1091 0.103 Uiso 1 1 calc R . . C55 C -0.0399(3) 0.12051(9) 0.09518(16) 0.0425(7) Uani 1 1 d . . . H55 H -0.0045 0.1246 0.0552 0.051 Uiso 1 1 calc R . . C56 C -0.0364(3) 0.07521(10) 0.1090(2) 0.0588(10) Uani 1 1 d . . . H56A H -0.0697 0.0695 0.1487 0.071 Uiso 1 1 calc R . . H56B H -0.0853 0.0617 0.0654 0.071 Uiso 1 1 calc R . . C57 C 0.0915(3) 0.05954(11) 0.1283(2) 0.0669(11) Uani 1 1 d . . . H57A H 0.0919 0.0313 0.1401 0.080 Uiso 1 1 calc R . . H57B H 0.1207 0.0623 0.0860 0.080 Uiso 1 1 calc R . . C58 C 0.1753(3) 0.08165(12) 0.1924(2) 0.0667(11) Uani 1 1 d . . . H58A H 0.1522 0.0764 0.2363 0.080 Uiso 1 1 calc R . . H58B H 0.2567 0.0720 0.2006 0.080 Uiso 1 1 calc R . . C59 C 0.1711(3) 0.12621(11) 0.1779(2) 0.0614(10) Uani 1 1 d . . . H59A H 0.2006 0.1317 0.1365 0.074 Uiso 1 1 calc R . . H59B H 0.2227 0.1400 0.2203 0.074 Uiso 1 1 calc R . . C60 C 0.0433(3) 0.14195(11) 0.16186(18) 0.0546(9) Uani 1 1 d . . . H60A H 0.0422 0.1705 0.1525 0.065 Uiso 1 1 calc R . . H60B H 0.0150 0.1376 0.2041 0.065 Uiso 1 1 calc R . . C61 C -0.2824(3) 0.12203(10) 0.12201(17) 0.0495(8) Uani 1 1 d . . . H61 H -0.2576 0.0942 0.1340 0.059 Uiso 1 1 calc R . . C62 C -0.2535(4) 0.14410(14) 0.19518(19) 0.0699(11) Uani 1 1 d . . . H62A H -0.2753 0.1721 0.1866 0.084 Uiso 1 1 calc R . . H62B H -0.1680 0.1426 0.2197 0.084 Uiso 1 1 calc R . . C63 C -0.3223(4) 0.12553(16) 0.2440(2) 0.0860(14) Uani 1 1 d . . . H63A H -0.2937 0.0984 0.2570 0.103 Uiso 1 1 calc R . . H63B H -0.3067 0.1409 0.2889 0.103 Uiso 1 1 calc R . . C64 C -0.4552(4) 0.12459(15) 0.2065(2) 0.0838(14) Uani 1 1 d . . . H64A H -0.4854 0.1518 0.1982 0.101 Uiso 1 1 calc R . . H64B H -0.4953 0.1114 0.2379 0.101 Uiso 1 1 calc R . . C65 C -0.4842(4) 0.10270(14) 0.1340(2) 0.0749(12) Uani 1 1 d . . . H65A H -0.5699 0.1041 0.1099 0.090 Uiso 1 1 calc R . . H65B H -0.4624 0.0747 0.1428 0.090 Uiso 1 1 calc R . . C66 C -0.4177(3) 0.12062(11) 0.0844(2) 0.0572(9) Uani 1 1 d . . . H66A H -0.4470 0.1476 0.0706 0.069 Uiso 1 1 calc R . . H66B H -0.4335 0.1047 0.0401 0.069 Uiso 1 1 calc R . . C67 C -0.1823(3) 0.19465(9) 0.06639(17) 0.0433(7) Uani 1 1 d . . . H67 H -0.1443 0.2017 0.1178 0.052 Uiso 1 1 calc R . . C68 C -0.1018(3) 0.21051(10) 0.0225(2) 0.0526(9) Uani 1 1 d . . . H68A H -0.0242 0.1974 0.0387 0.063 Uiso 1 1 calc R . . H68B H -0.1377 0.2044 -0.0290 0.063 Uiso 1 1 calc R . . C69 C -0.0854(3) 0.25570(11) 0.0325(2) 0.0630(10) Uani 1 1 d . . . H69A H -0.0454 0.2616 0.0836 0.076 Uiso 1 1 calc R . . H69B H -0.0350 0.2654 0.0039 0.076 Uiso 1 1 calc R . . C70 C -0.2051(4) 0.27711(11) 0.0086(2) 0.0707(11) Uani 1 1 d . . . H70A H -0.2414 0.2735 -0.0436 0.085 Uiso 1 1 calc R . . H70B H -0.1926 0.3056 0.0180 0.085 Uiso 1 1 calc R . . C71 C -0.2889(4) 0.26117(11) 0.0492(3) 0.0742(12) Uani 1 1 d . . . H71A H -0.3667 0.2739 0.0302 0.089 Uiso 1 1 calc R . . H71B H -0.2574 0.2680 0.1007 0.089 Uiso 1 1 calc R . . C72 C -0.3040(3) 0.21611(10) 0.0416(2) 0.0594(10) Uani 1 1 d . . . H72A H -0.3443 0.2094 -0.0092 0.071 Uiso 1 1 calc R . . H72B H -0.3539 0.2069 0.0709 0.071 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 S1 0.0523(5) 0.0725(6) 0.0504(5) 0.0171(4) 0.0216(4) 0.0122(5) S2 0.0412(5) 0.0742(7) 0.0645(6) 0.0235(5) -0.0006(4) -0.0052(4) S3 0.0942(8) 0.0394(5) 0.0586(6) 0.0016(4) 0.0206(5) -0.0071(5) P1 0.0271(4) 0.0373(4) 0.0324(4) -0.0004(3) 0.0089(3) 0.0000(3) In1 0.04120(12) 0.03844(12) 0.03580(11) -0.00137(9) 0.00863(9) -0.00052(10) C1 0.053(2) 0.059(2) 0.0366(17) -0.0043(15) 0.0205(15) 0.0082(17) C2 0.053(2) 0.077(3) 0.054(2) 0.0135(19) 0.0223(17) 0.004(2) C3 0.045(2) 0.112(4) 0.066(3) 0.015(2) 0.022(2) 0.008(2) C4 0.074(3) 0.098(4) 0.077(3) 0.010(3) 0.032(3) 0.031(3) C5 0.091(4) 0.065(3) 0.099(4) 0.000(2) 0.032(3) 0.027(3) C6 0.066(3) 0.059(2) 0.077(3) -0.013(2) 0.025(2) 0.001(2) C7 0.046(2) 0.062(2) 0.0383(17) -0.0028(16) 0.0057(15) 0.0037(17) C8 0.057(3) 0.078(3) 0.095(3) -0.010(3) 0.025(2) 0.008(2) C9 0.089(4) 0.067(3) 0.172(6) -0.006(4) 0.036(4) 0.026(3) C10 0.099(4) 0.059(3) 0.143(5) 0.020(3) 0.020(4) 0.009(3) C11 0.090(3) 0.070(3) 0.071(3) 0.016(2) 0.026(2) 0.004(3) C12 0.059(2) 0.061(2) 0.055(2) 0.0046(18) 0.0189(18) 0.0109(18) C13 0.063(2) 0.0353(18) 0.069(2) -0.0050(16) 0.019(2) -0.0099(16) C14 0.063(3) 0.072(3) 0.137(5) -0.031(3) 0.025(3) -0.011(2) C15 0.062(3) 0.093(4) 0.153(5) -0.020(4) -0.012(3) -0.016(3) C16 0.119(5) 0.061(3) 0.095(4) -0.017(3) -0.001(3) -0.016(3) C17 0.103(4) 0.055(2) 0.067(3) -0.006(2) 0.023(3) -0.008(2) C18 0.071(3) 0.050(2) 0.068(3) -0.0002(19) 0.017(2) -0.0028(19) C19 0.0280(15) 0.0458(18) 0.0400(16) 0.0006(13) 0.0115(12) -0.0003(13) C20 0.0314(17) 0.081(3) 0.054(2) 0.0070(18) 0.0147(15) 0.0017(17) C21 0.0345(18) 0.085(3) 0.067(2) -0.001(2) 0.0217(17) -0.0137(18) C22 0.058(2) 0.092(3) 0.070(3) -0.010(2) 0.040(2) -0.022(2) C23 0.063(3) 0.151(5) 0.044(2) 0.009(2) 0.0200(19) -0.029(3) C24 0.049(2) 0.119(4) 0.0382(19) -0.006(2) 0.0175(17) -0.024(2) C25 0.0361(17) 0.0398(17) 0.0422(17) -0.0005(13) 0.0110(14) 0.0002(13) C26 0.068(2) 0.045(2) 0.0397(18) -0.0051(15) 0.0062(17) 0.0001(17) C27 0.088(3) 0.043(2) 0.062(2) -0.0101(18) 0.020(2) 0.0043(19) C28 0.087(3) 0.040(2) 0.085(3) -0.002(2) 0.032(2) -0.004(2) C29 0.074(3) 0.046(2) 0.060(2) 0.0123(17) 0.029(2) 0.0056(18) C30 0.065(2) 0.046(2) 0.0461(19) 0.0025(15) 0.0214(17) 0.0007(17) C31 0.0250(14) 0.0491(18) 0.0350(16) -0.0011(13) 0.0079(12) 0.0002(13) C32 0.0339(17) 0.0470(19) 0.057(2) 0.0085(15) 0.0190(15) 0.0005(14) C33 0.0303(17) 0.062(2) 0.067(2) 0.0048(18) 0.0183(16) -0.0011(15) C34 0.0334(18) 0.063(2) 0.073(2) 0.0144(19) 0.0180(17) 0.0128(16) C35 0.0378(19) 0.060(2) 0.082(3) 0.025(2) 0.0166(18) 0.0108(16) C36 0.0317(17) 0.051(2) 0.071(2) 0.0172(17) 0.0118(16) -0.0005(15) S4 0.0617(6) 0.0790(7) 0.0542(5) 0.0127(5) 0.0228(5) 0.0155(5) S5 0.0899(8) 0.0450(5) 0.0697(7) 0.0015(5) -0.0010(6) -0.0102(5) S6 0.0421(5) 0.0855(8) 0.0734(7) 0.0148(6) -0.0043(5) -0.0025(5) P2 0.0415(4) 0.0399(4) 0.0342(4) -0.0033(3) 0.0075(3) -0.0006(4) In2 0.04408(13) 0.04339(13) 0.03769(12) -0.00330(9) 0.00431(10) 0.00010(10) C37 0.055(2) 0.068(2) 0.0386(18) -0.0091(16) 0.0158(16) 0.0099(18) C38 0.071(3) 0.060(3) 0.072(3) -0.015(2) 0.013(2) 0.009(2) C39 0.091(4) 0.086(4) 0.093(4) -0.011(3) 0.016(3) 0.035(3) C40 0.071(3) 0.125(5) 0.072(3) -0.010(3) 0.012(2) 0.038(3) C41 0.056(3) 0.130(5) 0.067(3) -0.009(3) 0.015(2) -0.006(3) C42 0.066(3) 0.079(3) 0.059(2) -0.010(2) 0.025(2) -0.003(2) C43 0.046(2) 0.0385(19) 0.081(3) -0.0032(18) 0.0143(19) -0.0062(15) C44 0.071(3) 0.064(3) 0.073(3) -0.008(2) 0.024(2) -0.013(2) C45 0.131(5) 0.081(3) 0.076(3) -0.005(3) 0.031(3) -0.037(3) C46 0.101(3) 0.091(3) 0.109(3) -0.001(3) -0.006(3) -0.020(3) C47 0.077(3) 0.117(4) 0.160(4) -0.020(3) 0.007(3) -0.003(3) C48 0.085(3) 0.102(3) 0.142(4) -0.044(3) 0.030(3) -0.003(3) C49 0.046(2) 0.069(2) 0.045(2) -0.0035(18) -0.0005(16) 0.0134(18) C50 0.054(2) 0.074(3) 0.059(2) 0.000(2) 0.0099(19) 0.010(2) C51 0.065(3) 0.085(3) 0.089(3) 0.014(3) -0.001(2) -0.005(3) C52 0.098(4) 0.065(3) 0.101(4) -0.008(3) -0.024(3) 0.015(3) C53 0.112(5) 0.104(5) 0.085(4) -0.018(3) 0.002(3) 0.049(4) C54 0.078(3) 0.108(4) 0.069(3) 0.002(3) 0.019(2) 0.038(3) C55 0.0407(17) 0.0483(18) 0.0346(15) 0.0005(14) 0.0050(13) 0.0022(14) C56 0.053(2) 0.046(2) 0.067(2) -0.0019(17) 0.0016(18) 0.0039(16) C57 0.060(2) 0.054(2) 0.076(3) -0.006(2) 0.004(2) 0.0132(19) C58 0.049(2) 0.071(3) 0.067(3) 0.003(2) -0.0031(19) 0.0118(19) C59 0.047(2) 0.064(2) 0.061(2) -0.0034(19) -0.0014(17) -0.0020(18) C60 0.053(2) 0.050(2) 0.050(2) -0.0046(16) -0.0019(16) 0.0000(16) C61 0.052(2) 0.055(2) 0.0424(18) 0.0025(16) 0.0155(15) 0.0012(16) C62 0.062(2) 0.106(3) 0.042(2) -0.011(2) 0.0166(18) -0.011(2) C63 0.079(3) 0.135(4) 0.051(2) 0.009(3) 0.030(2) 0.007(3) C64 0.080(3) 0.119(4) 0.064(3) 0.006(3) 0.041(2) -0.001(3) C65 0.061(3) 0.090(3) 0.082(3) 0.008(2) 0.033(2) -0.008(2) C66 0.053(2) 0.066(2) 0.055(2) -0.0045(18) 0.0194(17) -0.0094(18) C67 0.0445(18) 0.0402(17) 0.0431(18) -0.0082(14) 0.0097(14) -0.0010(14) C68 0.049(2) 0.045(2) 0.062(2) 0.0002(16) 0.0140(17) 0.0007(16) C69 0.061(2) 0.050(2) 0.076(3) -0.0004(19) 0.017(2) -0.0063(18) C70 0.071(3) 0.044(2) 0.093(3) 0.000(2) 0.018(2) 0.0010(19) C71 0.073(3) 0.046(2) 0.106(3) -0.007(2) 0.030(3) 0.013(2) C72 0.046(2) 0.050(2) 0.082(3) -0.0031(19) 0.0197(19) 0.0058(16) _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 S1 C1 1.784(3) . ? S1 In1 2.4456(10) . ? S2 C7 1.768(4) . ? S2 In1 2.4544(9) . ? S3 C13 1.775(4) . ? S3 In1 2.4384(9) . ? P1 C31 1.841(3) . ? P1 C19 1.843(3) . ? P1 C25 1.846(3) . ? P1 In1 2.6109(8) . ? C1 C6 1.370(5) . ? C1 C2 1.380(5) . ? C2 C3 1.397(5) . ? C3 C4 1.370(6) . ? C4 C5 1.364(6) . ? C5 C6 1.388(6) . ? C7 C8 1.377(5) . ? C7 C12 1.379(5) . ? C8 C9 1.386(7) . ? C9 C10 1.355(7) . ? C10 C11 1.359(6) . ? C11 C12 1.384(5) . ? C13 C18 1.374(5) . ? C13 C14 1.379(5) . ? C14 C15 1.390(7) . ? C15 C16 1.354(7) . ? C16 C17 1.347(6) . ? C17 C18 1.371(5) . ? C19 C24 1.514(4) . ? C19 C20 1.527(4) . ? C20 C21 1.522(5) . ? C21 C22 1.502(5) . ? C22 C23 1.493(5) . ? C23 C24 1.531(5) . ? C25 C30 1.527(4) . ? C25 C26 1.528(4) . ? C26 C27 1.523(5) . ? C27 C28 1.510(5) . ? C28 C29 1.515(5) . ? C29 C30 1.520(5) . ? C31 C36 1.532(4) . ? C31 C32 1.533(4) . ? C32 C33 1.520(4) . ? C33 C34 1.510(5) . ? C34 C35 1.508(5) . ? C35 C36 1.522(4) . ? S4 C37 1.782(4) . ? S4 In2 2.4470(10) . ? S5 C43 1.772(4) . ? S5 In2 2.4414(10) . ? S6 C49 1.772(4) . ? S6 In2 2.4411(10) . ? P2 C67 1.837(3) . ? P2 C61 1.852(3) . ? P2 C55 1.853(3) . ? P2 In2 2.6084(8) . ? C37 C38 1.369(5) . ? C37 C42 1.385(5) . ? C38 C39 1.381(6) . ? C39 C40 1.352(7) . ? C40 C41 1.362(7) . ? C41 C42 1.394(6) . ? C43 C44 1.359(5) . ? C43 C48 1.379(6) . ? C44 C45 1.369(6) . ? C45 C46 1.337(7) . ? C46 C47 1.346(8) . ? C47 C48 1.418(7) . ? C49 C50 1.369(5) . ? C49 C54 1.381(5) . ? C50 C51 1.393(6) . ? C51 C52 1.374(7) . ? C52 C53 1.349(7) . ? C53 C54 1.359(7) . ? C55 C60 1.532(4) . ? C55 C56 1.532(4) . ? C56 C57 1.520(5) . ? C57 C58 1.514(5) . ? C58 C59 1.510(5) . ? C59 C60 1.523(5) . ? C61 C62 1.528(5) . ? C61 C66 1.528(5) . ? C62 C63 1.531(5) . ? C63 C64 1.504(6) . ? C64 C65 1.513(6) . ? C65 C66 1.516(5) . ? C67 C68 1.528(5) . ? C67 C72 1.534(4) . ? C68 C69 1.525(5) . ? C69 C70 1.513(5) . ? C70 C71 1.514(6) . ? C71 C72 1.516(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 C1 S1 In1 108.92(12) . . ? C7 S2 In1 110.45(12) . . ? C13 S3 In1 101.50(12) . . ? C31 P1 C19 105.97(13) . . ? C31 P1 C25 110.90(14) . . ? C19 P1 C25 108.12(14) . . ? C31 P1 In1 111.73(10) . . ? C19 P1 In1 107.08(10) . . ? C25 P1 In1 112.68(10) . . ? S3 In1 S1 119.96(4) . . ? S3 In1 S2 105.79(4) . . ? S1 In1 S2 109.48(3) . . ? S3 In1 P1 97.85(3) . . ? S1 In1 P1 112.56(3) . . ? S2 In1 P1 110.48(3) . . ? C6 C1 C2 119.0(3) . . ? C6 C1 S1 123.1(3) . . ? C2 C1 S1 117.8(3) . . ? C1 C2 C3 120.3(4) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 119.6(4) . . ? C4 C5 C6 120.6(5) . . ? C1 C6 C5 120.5(4) . . ? C8 C7 C12 118.0(4) . . ? C8 C7 S2 118.2(3) . . ? C12 C7 S2 123.8(3) . . ? C7 C8 C9 119.9(4) . . ? C10 C9 C8 121.6(5) . . ? C9 C10 C11 119.1(5) . . ? C10 C11 C12 120.2(5) . . ? C7 C12 C11 121.2(4) . . ? C18 C13 C14 117.5(4) . . ? C18 C13 S3 120.4(3) . . ? C14 C13 S3 122.1(3) . . ? C13 C14 C15 120.1(5) . . ? C16 C15 C14 120.7(5) . . ? C17 C16 C15 119.6(5) . . ? C16 C17 C18 120.5(5) . . ? C17 C18 C13 121.5(4) . . ? C24 C19 C20 110.3(3) . . ? C24 C19 P1 115.3(2) . . ? C20 C19 P1 112.7(2) . . ? C21 C20 C19 110.5(3) . . ? C22 C21 C20 111.6(3) . . ? C23 C22 C21 111.5(3) . . ? C22 C23 C24 111.7(3) . . ? C19 C24 C23 109.9(3) . . ? C30 C25 C26 110.3(3) . . ? C30 C25 P1 112.1(2) . . ? C26 C25 P1 116.2(2) . . ? C27 C26 C25 110.8(3) . . ? C28 C27 C26 111.2(3) . . ? C27 C28 C29 110.8(3) . . ? C28 C29 C30 111.3(3) . . ? C29 C30 C25 111.4(3) . . ? C36 C31 C32 110.5(2) . . ? C36 C31 P1 109.9(2) . . ? C32 C31 P1 111.7(2) . . ? C33 C32 C31 111.7(3) . . ? C34 C33 C32 111.6(3) . . ? C35 C34 C33 111.0(3) . . ? C34 C35 C36 111.5(3) . . ? C35 C36 C31 111.3(3) . . ? C37 S4 In2 106.13(13) . . ? C43 S5 In2 101.20(12) . . ? C49 S6 In2 105.94(12) . . ? C67 P2 C61 109.73(15) . . ? C67 P2 C55 105.58(14) . . ? C61 P2 C55 109.28(15) . . ? C67 P2 In2 114.76(11) . . ? C61 P2 In2 110.59(11) . . ? C55 P2 In2 106.63(10) . . ? S6 In2 S5 107.24(4) . . ? S6 In2 S4 108.28(4) . . ? S5 In2 S4 118.36(4) . . ? S6 In2 P2 115.54(4) . . ? S5 In2 P2 99.79(3) . . ? S4 In2 P2 107.82(3) . . ? C38 C37 C42 118.8(4) . . ? C38 C37 S4 122.3(3) . . ? C42 C37 S4 118.7(3) . . ? C37 C38 C39 120.2(4) . . ? C40 C39 C38 121.3(5) . . ? C39 C40 C41 119.5(5) . . ? C40 C41 C42 120.4(5) . . ? C37 C42 C41 119.8(4) . . ? C44 C43 C48 118.2(4) . . ? C44 C43 S5 120.4(3) . . ? C48 C43 S5 121.4(4) . . ? C43 C44 C45 122.1(5) . . ? C46 C45 C44 120.4(5) . . ? C45 C46 C47 119.8(6) . . ? C46 C47 C48 120.8(6) . . ? C43 C48 C47 118.6(5) . . ? C50 C49 C54 117.7(4) . . ? C50 C49 S6 123.9(3) . . ? C54 C49 S6 118.3(4) . . ? C49 C50 C51 120.5(4) . . ? C52 C51 C50 119.8(5) . . ? C53 C52 C51 119.7(5) . . ? C52 C53 C54 120.5(5) . . ? C53 C54 C49 121.8(5) . . ? C60 C55 C56 109.8(3) . . ? C60 C55 P2 116.3(2) . . ? C56 C55 P2 112.1(2) . . ? C57 C56 C55 110.8(3) . . ? C58 C57 C56 112.4(3) . . ? C59 C58 C57 110.6(3) . . ? C58 C59 C60 110.7(3) . . ? C59 C60 C55 110.4(3) . . ? C62 C61 C66 111.2(3) . . ? C62 C61 P2 114.1(2) . . ? C66 C61 P2 113.3(2) . . ? C61 C62 C63 110.5(3) . . ? C64 C63 C62 111.7(3) . . ? C63 C64 C65 111.5(4) . . ? C64 C65 C66 111.5(3) . . ? C65 C66 C61 111.5(3) . . ? C68 C67 C72 109.4(3) . . ? C68 C67 P2 111.8(2) . . ? C72 C67 P2 113.1(2) . . ? C69 C68 C67 110.4(3) . . ? C70 C69 C68 111.0(3) . . ? C69 C70 C71 111.0(3) . . ? C70 C71 C72 111.9(3) . . ? C71 C72 C67 111.3(3) . . ? 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 C13 S3 In1 S1 -76.48(14) . . . . ? C13 S3 In1 S2 47.79(14) . . . . ? C13 S3 In1 P1 161.75(14) . . . . ? C1 S1 In1 S3 -37.06(13) . . . . ? C1 S1 In1 S2 -159.55(12) . . . . ? C1 S1 In1 P1 77.16(13) . . . . ? C7 S2 In1 S3 -178.89(13) . . . . ? C7 S2 In1 S1 -48.30(13) . . . . ? C7 S2 In1 P1 76.22(13) . . . . ? C31 P1 In1 S3 75.41(11) . . . . ? C19 P1 In1 S3 -40.21(10) . . . . ? C25 P1 In1 S3 -158.96(11) . . . . ? C31 P1 In1 S1 -51.70(11) . . . . ? C19 P1 In1 S1 -167.31(10) . . . . ? C25 P1 In1 S1 73.94(11) . . . . ? C31 P1 In1 S2 -174.43(10) . . . . ? C19 P1 In1 S2 69.95(10) . . . . ? C25 P1 In1 S2 -48.79(11) . . . . ? In1 S1 C1 C6 45.0(3) . . . . ? In1 S1 C1 C2 -139.5(2) . . . . ? C6 C1 C2 C3 1.2(5) . . . . ? S1 C1 C2 C3 -174.4(3) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 0.9(7) . . . . ? C2 C1 C6 C5 0.1(6) . . . . ? S1 C1 C6 C5 175.5(3) . . . . ? C4 C5 C6 C1 -1.1(7) . . . . ? In1 S2 C7 C8 -138.3(3) . . . . ? In1 S2 C7 C12 44.5(3) . . . . ? C12 C7 C8 C9 -0.9(6) . . . . ? S2 C7 C8 C9 -178.3(4) . . . . ? C7 C8 C9 C10 0.7(8) . . . . ? C8 C9 C10 C11 0.1(9) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? C8 C7 C12 C11 0.4(6) . . . . ? S2 C7 C12 C11 177.6(3) . . . . ? C10 C11 C12 C7 0.3(7) . . . . ? In1 S3 C13 C18 104.9(3) . . . . ? In1 S3 C13 C14 -75.0(4) . . . . ? C18 C13 C14 C15 0.6(7) . . . . ? S3 C13 C14 C15 -179.6(4) . . . . ? C13 C14 C15 C16 0.5(8) . . . . ? C14 C15 C16 C17 -1.1(9) . . . . ? C15 C16 C17 C18 0.4(8) . . . . ? C16 C17 C18 C13 0.7(7) . . . . ? C14 C13 C18 C17 -1.2(6) . . . . ? S3 C13 C18 C17 178.9(3) . . . . ? C31 P1 C19 C24 55.5(3) . . . . ? C25 P1 C19 C24 -63.5(3) . . . . ? In1 P1 C19 C24 174.9(2) . . . . ? C31 P1 C19 C20 -176.7(2) . . . . ? C25 P1 C19 C20 64.3(3) . . . . ? In1 P1 C19 C20 -57.3(2) . . . . ? C24 C19 C20 C21 -57.1(4) . . . . ? P1 C19 C20 C21 172.4(3) . . . . ? C19 C20 C21 C22 55.5(4) . . . . ? C20 C21 C22 C23 -54.8(5) . . . . ? C21 C22 C23 C24 55.5(5) . . . . ? C20 C19 C24 C23 57.4(4) . . . . ? P1 C19 C24 C23 -173.6(3) . . . . ? C22 C23 C24 C19 -57.0(5) . . . . ? C31 P1 C25 C30 93.4(2) . . . . ? C19 P1 C25 C30 -150.9(2) . . . . ? In1 P1 C25 C30 -32.7(2) . . . . ? C31 P1 C25 C26 -34.8(3) . . . . ? C19 P1 C25 C26 81.0(3) . . . . ? In1 P1 C25 C26 -160.9(2) . . . . ? C30 C25 C26 C27 55.7(4) . . . . ? P1 C25 C26 C27 -175.3(3) . . . . ? C25 C26 C27 C28 -57.0(4) . . . . ? C26 C27 C28 C29 56.8(5) . . . . ? C27 C28 C29 C30 -56.2(4) . . . . ? C28 C29 C30 C25 55.8(4) . . . . ? C26 C25 C30 C29 -55.4(4) . . . . ? P1 C25 C30 C29 173.4(2) . . . . ? C19 P1 C31 C36 58.4(2) . . . . ? C25 P1 C31 C36 175.5(2) . . . . ? In1 P1 C31 C36 -57.9(2) . . . . ? C19 P1 C31 C32 -178.6(2) . . . . ? C25 P1 C31 C32 -61.5(2) . . . . ? In1 P1 C31 C32 65.1(2) . . . . ? C36 C31 C32 C33 -53.8(4) . . . . ? P1 C31 C32 C33 -176.5(2) . . . . ? C31 C32 C33 C34 55.0(4) . . . . ? C32 C33 C34 C35 -56.0(4) . . . . ? C33 C34 C35 C36 56.6(4) . . . . ? C34 C35 C36 C31 -56.1(4) . . . . ? C32 C31 C36 C35 54.2(4) . . . . ? P1 C31 C36 C35 177.9(2) . . . . ? C49 S6 In2 S5 177.59(14) . . . . ? C49 S6 In2 S4 -53.63(14) . . . . ? C49 S6 In2 P2 67.37(14) . . . . ? C43 S5 In2 S6 36.93(15) . . . . ? C43 S5 In2 S4 -85.81(14) . . . . ? C43 S5 In2 P2 157.70(14) . . . . ? C37 S4 In2 S6 -172.10(13) . . . . ? C37 S4 In2 S5 -49.89(14) . . . . ? C37 S4 In2 P2 62.23(13) . . . . ? C67 P2 In2 S6 -58.71(12) . . . . ? C61 P2 In2 S6 66.07(12) . . . . ? C55 P2 In2 S6 -175.23(11) . . . . ? C67 P2 In2 S5 -173.28(12) . . . . ? C61 P2 In2 S5 -48.50(12) . . . . ? C55 P2 In2 S5 70.21(11) . . . . ? C67 P2 In2 S4 62.54(12) . . . . ? C61 P2 In2 S4 -172.68(12) . . . . ? C55 P2 In2 S4 -53.98(11) . . . . ? In2 S4 C37 C38 59.1(3) . . . . ? In2 S4 C37 C42 -125.2(3) . . . . ? C42 C37 C38 C39 -0.9(6) . . . . ? S4 C37 C38 C39 174.8(3) . . . . ? C37 C38 C39 C40 0.1(7) . . . . ? C38 C39 C40 C41 0.8(8) . . . . ? C39 C40 C41 C42 -0.7(8) . . . . ? C38 C37 C42 C41 0.9(6) . . . . ? S4 C37 C42 C41 -175.0(3) . . . . ? C40 C41 C42 C37 -0.1(7) . . . . ? In2 S5 C43 C44 100.3(3) . . . . ? In2 S5 C43 C48 -80.3(4) . . . . ? C48 C43 C44 C45 -0.5(7) . . . . ? S5 C43 C44 C45 178.8(3) . . . . ? C43 C44 C45 C46 2.0(7) . . . . ? C44 C45 C46 C47 -1.4(9) . . . . ? C45 C46 C47 C48 -0.5(10) . . . . ? C44 C43 C48 C47 -1.4(8) . . . . ? S5 C43 C48 C47 179.3(4) . . . . ? C46 C47 C48 C43 1.9(10) . . . . ? In2 S6 C49 C50 55.8(3) . . . . ? In2 S6 C49 C54 -127.8(3) . . . . ? C54 C49 C50 C51 1.2(6) . . . . ? S6 C49 C50 C51 177.7(3) . . . . ? C49 C50 C51 C52 -0.5(6) . . . . ? C50 C51 C52 C53 -0.2(7) . . . . ? C51 C52 C53 C54 0.2(8) . . . . ? C52 C53 C54 C49 0.5(8) . . . . ? C50 C49 C54 C53 -1.2(6) . . . . ? S6 C49 C54 C53 -177.9(4) . . . . ? C67 P2 C55 C60 41.0(3) . . . . ? C61 P2 C55 C60 -77.0(3) . . . . ? In2 P2 C55 C60 163.4(2) . . . . ? C67 P2 C55 C56 168.5(2) . . . . ? C61 P2 C55 C56 50.5(3) . . . . ? In2 P2 C55 C56 -69.0(2) . . . . ? C60 C55 C56 C57 -55.6(4) . . . . ? P2 C55 C56 C57 173.5(3) . . . . ? C55 C56 C57 C58 54.8(5) . . . . ? C56 C57 C58 C59 -55.2(5) . . . . ? C57 C58 C59 C60 56.9(4) . . . . ? C58 C59 C60 C55 -59.0(4) . . . . ? C56 C55 C60 C59 58.0(4) . . . . ? P2 C55 C60 C59 -173.4(2) . . . . ? C67 P2 C61 C62 -39.8(3) . . . . ? C55 P2 C61 C62 75.5(3) . . . . ? In2 P2 C61 C62 -167.4(2) . . . . ? C67 P2 C61 C66 88.8(3) . . . . ? C55 P2 C61 C66 -155.9(2) . . . . ? In2 P2 C61 C66 -38.8(3) . . . . ? C66 C61 C62 C63 54.5(4) . . . . ? P2 C61 C62 C63 -175.9(3) . . . . ? C61 C62 C63 C64 -55.5(5) . . . . ? C62 C63 C64 C65 56.0(6) . . . . ? C63 C64 C65 C66 -55.5(5) . . . . ? C64 C65 C66 C61 54.8(5) . . . . ? C62 C61 C66 C65 -54.7(4) . . . . ? P2 C61 C66 C65 175.2(3) . . . . ? C61 P2 C67 C68 174.9(2) . . . . ? C55 P2 C67 C68 57.2(3) . . . . ? In2 P2 C67 C68 -59.9(2) . . . . ? C61 P2 C67 C72 -61.2(3) . . . . ? C55 P2 C67 C72 -178.8(2) . . . . ? In2 P2 C67 C72 64.1(3) . . . . ? C72 C67 C68 C69 58.1(4) . . . . ? P2 C67 C68 C69 -175.9(2) . . . . ? C67 C68 C69 C70 -58.4(4) . . . . ? C68 C69 C70 C71 56.0(5) . . . . ? C69 C70 C71 C72 -54.5(5) . . . . ? C70 C71 C72 C67 55.3(5) . . . . ? C68 C67 C72 C71 -56.6(4) . . . . ? P2 C67 C72 C71 178.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.548 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.070 data_compound13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 In P Se3' _chemical_formula_weight 863.41 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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 10.4085(7) _cell_length_b 11.6417(9) _cell_length_c 15.5724(11) _cell_angle_alpha 85.84(3) _cell_angle_beta 82.96(3) _cell_angle_gamma 70.98(3) _cell_volume 1769.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 3.822 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.4100 _exptl_absorpt_correction_T_max 0.4883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 cad4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7434 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.29 _reflns_number_total 7159 _reflns_number_gt 5451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.3005P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7159 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Se1 Se 0.67817(4) 0.78889(3) 0.38013(2) 0.02891(10) Uani 1 1 d . . . Se2 Se 0.67307(4) 0.82797(3) 0.10886(2) 0.02571(10) Uani 1 1 d . . . Se3 Se 0.62405(4) 0.50980(3) 0.25633(2) 0.02175(9) Uani 1 1 d . . . In1 In 0.58029(2) 0.73968(2) 0.248428(15) 0.01745(7) Uani 1 1 d . . . P1 P 0.31525(9) 0.81154(8) 0.28727(5) 0.01627(18) Uani 1 1 d . . . C1 C 0.7079(4) 0.9409(3) 0.3418(2) 0.0246(8) Uani 1 1 d . . . C2 C 0.7944(4) 0.9489(4) 0.2689(3) 0.0298(9) Uani 1 1 d . . . H2 H 0.8399 0.8805 0.2367 0.036 Uiso 1 1 calc R . . C3 C 0.8132(4) 1.0602(4) 0.2434(3) 0.0401(11) Uani 1 1 d . . . H3 H 0.8714 1.0658 0.1941 0.048 Uiso 1 1 calc R . . C4 C 0.7468(5) 1.1613(4) 0.2905(3) 0.0438(12) Uani 1 1 d . . . H4 H 0.7602 1.2350 0.2732 0.053 Uiso 1 1 calc R . . C5 C 0.6604(5) 1.1541(4) 0.3630(3) 0.0406(11) Uani 1 1 d . . . H5 H 0.6151 1.2232 0.3947 0.049 Uiso 1 1 calc R . . C6 C 0.6399(4) 1.0439(4) 0.3898(3) 0.0315(9) Uani 1 1 d . . . H6 H 0.5815 1.0391 0.4391 0.038 Uiso 1 1 calc R . . C7 C 0.6076(4) 0.7671(3) 0.0168(2) 0.0218(8) Uani 1 1 d . . . C8 C 0.6109(4) 0.6467(3) 0.0141(2) 0.0272(8) Uani 1 1 d . . . H8 H 0.6399 0.5921 0.0598 0.033 Uiso 1 1 calc R . . C9 C 0.5702(4) 0.6092(4) -0.0579(3) 0.0322(9) Uani 1 1 d . . . H9 H 0.5707 0.5294 -0.0595 0.039 Uiso 1 1 calc R . . C10 C 0.5291(4) 0.6881(4) -0.1267(3) 0.0302(9) Uani 1 1 d . . . H10 H 0.5039 0.6612 -0.1749 0.036 Uiso 1 1 calc R . . C11 C 0.5256(4) 0.8068(4) -0.1241(2) 0.0291(9) Uani 1 1 d . . . H11 H 0.4969 0.8607 -0.1702 0.035 Uiso 1 1 calc R . . C12 C 0.5648(4) 0.8466(3) -0.0525(2) 0.0251(8) Uani 1 1 d . . . H12 H 0.5623 0.9270 -0.0511 0.030 Uiso 1 1 calc R . . C13 C 0.8131(4) 0.4613(3) 0.2082(2) 0.0219(8) Uani 1 1 d . . . C14 C 0.9096(4) 0.4983(4) 0.2418(3) 0.0319(9) Uani 1 1 d . . . H14 H 0.8840 0.5498 0.2882 0.038 Uiso 1 1 calc R . . C15 C 1.0440(4) 0.4585(4) 0.2061(3) 0.0393(10) Uani 1 1 d . . . H15 H 1.1086 0.4845 0.2281 0.047 Uiso 1 1 calc R . . C16 C 1.0833(4) 0.3808(5) 0.1385(3) 0.0478(12) Uani 1 1 d . . . H16 H 1.1742 0.3539 0.1151 0.057 Uiso 1 1 calc R . . C17 C 0.9892(5) 0.3435(5) 0.1058(3) 0.0526(13) Uani 1 1 d . . . H17 H 1.0162 0.2907 0.0601 0.063 Uiso 1 1 calc R . . C18 C 0.8534(4) 0.3831(4) 0.1398(3) 0.0372(10) Uani 1 1 d . . . H18 H 0.7895 0.3574 0.1168 0.045 Uiso 1 1 calc R . . C19 C 0.2780(3) 0.6856(3) 0.3539(2) 0.0188(7) Uani 1 1 d . . . H19 H 0.3271 0.6119 0.3219 0.023 Uiso 1 1 calc R . . C20 C 0.1284(4) 0.6878(3) 0.3690(2) 0.0261(8) Uani 1 1 d . . . H20A H 0.0751 0.7556 0.4047 0.031 Uiso 1 1 calc R . . H20B H 0.0904 0.6986 0.3140 0.031 Uiso 1 1 calc R . . C21 C 0.1210(4) 0.5691(4) 0.4138(3) 0.0307(9) Uani 1 1 d . . . H21A H 0.1680 0.5025 0.3757 0.037 Uiso 1 1 calc R . . H21B H 0.0261 0.5724 0.4248 0.037 Uiso 1 1 calc R . . C22 C 0.1848(4) 0.5445(4) 0.4990(3) 0.0314(9) Uani 1 1 d . . . H22A H 0.1311 0.6053 0.5400 0.038 Uiso 1 1 calc R . . H22B H 0.1843 0.4654 0.5232 0.038 Uiso 1 1 calc R . . C23 C 0.3309(4) 0.5476(3) 0.4853(2) 0.0277(8) Uani 1 1 d . . . H23A H 0.3869 0.4799 0.4504 0.033 Uiso 1 1 calc R . . H23B H 0.3670 0.5380 0.5408 0.033 Uiso 1 1 calc R . . C24 C 0.3397(4) 0.6665(3) 0.4404(2) 0.0231(8) Uani 1 1 d . . . H24A H 0.4344 0.6637 0.4303 0.028 Uiso 1 1 calc R . . H24B H 0.2905 0.7339 0.4773 0.028 Uiso 1 1 calc R . . C25 C 0.2575(4) 0.9507(3) 0.3503(2) 0.0208(7) Uani 1 1 d . . . H25 H 0.2867 0.9258 0.4081 0.025 Uiso 1 1 calc R . . C26 C 0.1023(4) 1.0101(3) 0.3632(3) 0.0287(9) Uani 1 1 d . . . H26A H 0.0682 1.0385 0.3077 0.034 Uiso 1 1 calc R . . H26B H 0.0600 0.9507 0.3881 0.034 Uiso 1 1 calc R . . C27 C 0.0649(4) 1.1166(4) 0.4230(3) 0.0366(10) Uani 1 1 d . . . H27A H -0.0335 1.1549 0.4291 0.044 Uiso 1 1 calc R . . H27B H 0.0926 1.0867 0.4798 0.044 Uiso 1 1 calc R . . C28 C 0.1331(4) 1.2104(4) 0.3885(3) 0.0374(10) Uani 1 1 d . . . H28A H 0.0980 1.2470 0.3346 0.045 Uiso 1 1 calc R . . H28B H 0.1115 1.2743 0.4298 0.045 Uiso 1 1 calc R . . C29 C 0.2866(4) 1.1523(3) 0.3733(3) 0.0311(9) Uani 1 1 d . . . H29A H 0.3226 1.1252 0.4285 0.037 Uiso 1 1 calc R . . H29B H 0.3270 1.2125 0.3475 0.037 Uiso 1 1 calc R . . C30 C 0.3272(4) 1.0444(3) 0.3143(2) 0.0246(8) Uani 1 1 d . . . H30A H 0.4256 1.0065 0.3095 0.030 Uiso 1 1 calc R . . H30B H 0.3010 1.0727 0.2569 0.030 Uiso 1 1 calc R . . C31 C 0.2157(4) 0.8335(3) 0.1941(2) 0.0197(7) Uani 1 1 d . . . H31 H 0.1188 0.8570 0.2162 0.024 Uiso 1 1 calc R . . C32 C 0.2360(4) 0.9336(3) 0.1300(2) 0.0255(8) Uani 1 1 d . . . H32A H 0.2072 1.0102 0.1590 0.031 Uiso 1 1 calc R . . H32B H 0.3323 0.9144 0.1095 0.031 Uiso 1 1 calc R . . C33 C 0.1539(4) 0.9463(3) 0.0529(2) 0.0274(8) Uani 1 1 d . . . H33A H 0.0571 0.9754 0.0726 0.033 Uiso 1 1 calc R . . H33B H 0.1738 1.0060 0.0113 0.033 Uiso 1 1 calc R . . C34 C 0.1876(4) 0.8257(4) 0.0090(2) 0.0304(9) Uani 1 1 d . . . H34A H 0.1294 0.8358 -0.0370 0.037 Uiso 1 1 calc R . . H34B H 0.2817 0.8013 -0.0167 0.037 Uiso 1 1 calc R . . C35 C 0.1667(4) 0.7271(4) 0.0734(2) 0.0306(9) Uani 1 1 d . . . H35A H 0.0710 0.7481 0.0955 0.037 Uiso 1 1 calc R . . H35B H 0.1923 0.6506 0.0444 0.037 Uiso 1 1 calc R . . C36 C 0.2522(4) 0.7129(3) 0.1478(2) 0.0241(8) Uani 1 1 d . . . H36A H 0.3483 0.6871 0.1260 0.029 Uiso 1 1 calc R . . H36B H 0.2367 0.6507 0.1886 0.029 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 Se1 0.0423(2) 0.0254(2) 0.0252(2) 0.00227(16) -0.01331(17) -0.01639(18) Se2 0.0322(2) 0.0289(2) 0.02119(19) 0.00190(15) -0.00239(15) - 0.01757(17) Se3 0.02294(19) 0.01574(18) 0.0259(2) -0.00266(14) 0.00251(15) - 0.00667(14) In1 0.01935(13) 0.01557(12) 0.01744(13) -0.00173(9) -0.00120(9) - 0.00564(10) P1 0.0177(4) 0.0163(4) 0.0146(4) -0.0014(3) -0.0012(3) -0.0051(4) C1 0.0238(19) 0.0215(19) 0.031(2) -0.0014(16) -0.0105(16) -0.0081(15) C2 0.026(2) 0.035(2) 0.030(2) -0.0016(17) -0.0065(17) -0.0105(17) C3 0.034(2) 0.051(3) 0.042(3) 0.012(2) -0.010(2) -0.022(2) C4 0.049(3) 0.026(2) 0.063(3) 0.013(2) -0.023(2) -0.019(2) C5 0.044(3) 0.026(2) 0.053(3) -0.011(2) -0.019(2) -0.006(2) C6 0.031(2) 0.031(2) 0.033(2) -0.0048(18) -0.0057(18) -0.0098(18) C7 0.0222(19) 0.0221(18) 0.0217(18) -0.0027(15) 0.0017(15) -0.0090(15) C8 0.033(2) 0.0232(19) 0.023(2) 0.0006(16) 0.0043(16) -0.0083(17) C9 0.041(2) 0.025(2) 0.033(2) -0.0078(17) 0.0066(18) -0.0168(18) C10 0.031(2) 0.036(2) 0.026(2) -0.0070(17) -0.0011(17) -0.0152(18) C11 0.032(2) 0.033(2) 0.023(2) 0.0037(16) -0.0016(16) -0.0134(18) C12 0.030(2) 0.0225(19) 0.0236(19) -0.0015(15) 0.0006(16) -0.0105(16) C13 0.0221(19) 0.0189(18) 0.0226(19) 0.0021(14) -0.0011(15) -0.0045(15) C14 0.032(2) 0.031(2) 0.032(2) -0.0096(17) -0.0020(18) -0.0080(18) C15 0.031(2) 0.048(3) 0.043(3) -0.010(2) -0.0053(19) -0.016(2) C16 0.023(2) 0.073(3) 0.043(3) -0.013(2) 0.008(2) -0.011(2) C17 0.039(3) 0.070(4) 0.046(3) -0.034(3) 0.005(2) -0.011(2) C18 0.028(2) 0.047(3) 0.037(2) -0.018(2) -0.0058(18) -0.0081(19) C19 0.0199(18) 0.0186(17) 0.0157(17) 0.0013(14) 0.0020(14) -0.0048(14) C20 0.0197(19) 0.031(2) 0.028(2) 0.0022(16) -0.0037(16) -0.0089(16) C21 0.024(2) 0.034(2) 0.038(2) 0.0046(18) -0.0031(17) -0.0149(17) C22 0.025(2) 0.035(2) 0.033(2) 0.0124(18) 0.0001(17) -0.0126(18) C23 0.029(2) 0.030(2) 0.025(2) 0.0101(16) -0.0081(16) -0.0100(17) C24 0.0241(19) 0.0255(19) 0.0210(18) 0.0042(15) -0.0049(15) -0.0098(15) C25 0.0274(19) 0.0195(18) 0.0131(16) -0.0006(14) -0.0014(14) -0.0047(15) C26 0.026(2) 0.0220(19) 0.036(2) -0.0079(17) 0.0081(17) -0.0070(16) C27 0.030(2) 0.030(2) 0.043(3) -0.0127(19) 0.0103(19) -0.0027(18) C28 0.039(2) 0.021(2) 0.049(3) -0.0125(19) 0.002(2) -0.0060(18) C29 0.037(2) 0.0211(19) 0.039(2) -0.0083(17) -0.0043(18) -0.0128(17) C30 0.027(2) 0.0210(19) 0.0255(19) -0.0045(15) -0.0024(16) -0.0062(16) C31 0.0190(18) 0.0220(18) 0.0165(17) -0.0037(14) 0.0000(14) -0.0046(14) C32 0.031(2) 0.028(2) 0.0185(18) 0.0005(15) -0.0048(16) -0.0103(17) C33 0.029(2) 0.030(2) 0.0194(19) 0.0037(16) -0.0061(16) -0.0033(17) C34 0.029(2) 0.038(2) 0.0210(19) -0.0071(17) -0.0044(16) -0.0039(18) C35 0.031(2) 0.033(2) 0.028(2) -0.0084(17) -0.0083(17) -0.0081(18) C36 0.031(2) 0.0213(19) 0.0202(18) -0.0034(15) -0.0039(16) -0.0079(16) _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 Se1 C1 1.934(4) . ? Se1 In1 2.5760(7) . ? Se2 C7 1.929(4) . ? Se2 In1 2.5537(8) . ? Se3 C13 1.931(4) . ? Se3 In1 2.5604(5) . ? In1 P1 2.6145(11) . ? P1 C31 1.840(3) . ? P1 C25 1.844(3) . ? P1 C19 1.852(3) . ? C1 C2 1.378(5) . ? C1 C6 1.394(5) . ? C2 C3 1.395(6) . ? C3 C4 1.367(6) . ? C4 C5 1.371(7) . ? C5 C6 1.394(6) . ? C7 C12 1.388(5) . ? C7 C8 1.394(5) . ? C8 C9 1.391(5) . ? C9 C10 1.374(6) . ? C10 C11 1.374(5) . ? C11 C12 1.390(5) . ? C13 C14 1.383(5) . ? C13 C18 1.386(5) . ? C14 C15 1.381(6) . ? C15 C16 1.373(6) . ? C16 C17 1.356(6) . ? C17 C18 1.385(6) . ? C19 C24 1.533(5) . ? C19 C20 1.537(5) . ? C20 C21 1.523(5) . ? C21 C22 1.523(5) . ? C22 C23 1.521(5) . ? C23 C24 1.529(5) . ? C25 C26 1.530(5) . ? C25 C30 1.535(5) . ? C26 C27 1.523(5) . ? C27 C28 1.520(6) . ? C28 C29 1.514(5) . ? C29 C30 1.525(5) . ? C31 C32 1.530(5) . ? C31 C36 1.539(5) . ? C32 C33 1.528(5) . ? C33 C34 1.524(5) . ? C34 C35 1.521(5) . ? C35 C36 1.513(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 C1 Se1 In1 101.50(11) . . ? C7 Se2 In1 105.21(10) . . ? C13 Se3 In1 97.49(11) . . ? Se2 In1 Se3 116.76(3) . . ? Se2 In1 Se1 110.736(19) . . ? Se3 In1 Se1 106.60(3) . . ? Se2 In1 P1 117.28(4) . . ? Se3 In1 P1 98.66(4) . . ? Se1 In1 P1 105.47(3) . . ? C31 P1 C25 109.89(16) . . ? C31 P1 C19 105.39(16) . . ? C25 P1 C19 109.65(16) . . ? C31 P1 In1 114.81(12) . . ? C25 P1 In1 111.16(12) . . ? C19 P1 In1 105.62(11) . . ? C2 C1 C6 119.8(4) . . ? C2 C1 Se1 121.5(3) . . ? C6 C1 Se1 118.7(3) . . ? C1 C2 C3 119.7(4) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 120.1(4) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 119.3(4) . . ? C12 C7 C8 119.3(3) . . ? C12 C7 Se2 117.1(3) . . ? C8 C7 Se2 123.4(3) . . ? C9 C8 C7 119.2(4) . . ? C10 C9 C8 121.2(4) . . ? C9 C10 C11 119.7(4) . . ? C10 C11 C12 120.2(4) . . ? C7 C12 C11 120.4(3) . . ? C14 C13 C18 119.4(3) . . ? C14 C13 Se3 122.1(3) . . ? C18 C13 Se3 118.4(3) . . ? C15 C14 C13 119.7(4) . . ? C16 C15 C14 120.7(4) . . ? C17 C16 C15 119.8(4) . . ? C16 C17 C18 120.7(4) . . ? C17 C18 C13 119.7(4) . . ? C24 C19 C20 110.1(3) . . ? C24 C19 P1 111.8(2) . . ? C20 C19 P1 117.6(2) . . ? C21 C20 C19 109.7(3) . . ? C20 C21 C22 112.2(3) . . ? C23 C22 C21 110.7(3) . . ? C22 C23 C24 112.0(3) . . ? C23 C24 C19 110.0(3) . . ? C26 C25 C30 110.6(3) . . ? C26 C25 P1 114.4(2) . . ? C30 C25 P1 112.7(2) . . ? C27 C26 C25 110.2(3) . . ? C28 C27 C26 111.8(3) . . ? C29 C28 C27 110.8(3) . . ? C28 C29 C30 112.1(3) . . ? C29 C30 C25 110.7(3) . . ? C32 C31 C36 110.2(3) . . ? C32 C31 P1 113.0(2) . . ? C36 C31 P1 109.8(2) . . ? C33 C32 C31 111.0(3) . . ? C34 C33 C32 111.6(3) . . ? C35 C34 C33 111.1(3) . . ? C36 C35 C34 110.5(3) . . ? C35 C36 C31 110.9(3) . . ? 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 C7 Se2 In1 Se3 51.24(11) . . . . ? C7 Se2 In1 Se1 173.44(11) . . . . ? C7 Se2 In1 P1 -65.49(11) . . . . ? C13 Se3 In1 Se2 44.01(11) . . . . ? C13 Se3 In1 Se1 -80.33(11) . . . . ? C13 Se3 In1 P1 170.59(11) . . . . ? C1 Se1 In1 Se2 29.32(12) . . . . ? C1 Se1 In1 Se3 157.28(11) . . . . ? C1 Se1 In1 P1 -98.51(12) . . . . ? Se2 In1 P1 C31 37.48(13) . . . . ? Se3 In1 P1 C31 -88.74(13) . . . . ? Se1 In1 P1 C31 161.27(12) . . . . ? Se2 In1 P1 C25 -88.02(12) . . . . ? Se3 In1 P1 C25 145.75(12) . . . . ? Se1 In1 P1 C25 35.76(12) . . . . ? Se2 In1 P1 C19 153.13(11) . . . . ? Se3 In1 P1 C19 26.90(11) . . . . ? Se1 In1 P1 C19 -83.09(12) . . . . ? In1 Se1 C1 C2 -60.1(3) . . . . ? In1 Se1 C1 C6 120.0(3) . . . . ? C6 C1 C2 C3 0.0(6) . . . . ? Se1 C1 C2 C3 -179.9(3) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C4 C5 C6 C1 -0.2(6) . . . . ? C2 C1 C6 C5 0.0(6) . . . . ? Se1 C1 C6 C5 179.9(3) . . . . ? In1 Se2 C7 C12 140.6(3) . . . . ? In1 Se2 C7 C8 -44.3(3) . . . . ? C12 C7 C8 C9 -0.5(5) . . . . ? Se2 C7 C8 C9 -175.5(3) . . . . ? C7 C8 C9 C10 1.1(6) . . . . ? C8 C9 C10 C11 -1.2(6) . . . . ? C9 C10 C11 C12 0.7(6) . . . . ? C8 C7 C12 C11 0.0(5) . . . . ? Se2 C7 C12 C11 175.3(3) . . . . ? C10 C11 C12 C7 -0.1(6) . . . . ? In1 Se3 C13 C14 54.1(3) . . . . ? In1 Se3 C13 C18 -128.3(3) . . . . ? C18 C13 C14 C15 0.9(6) . . . . ? Se3 C13 C14 C15 178.5(3) . . . . ? C13 C14 C15 C16 -1.1(7) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C15 C16 C17 C18 0.2(8) . . . . ? C16 C17 C18 C13 -0.4(8) . . . . ? C14 C13 C18 C17 -0.2(6) . . . . ? Se3 C13 C18 C17 -177.8(4) . . . . ? C31 P1 C19 C24 -172.9(2) . . . . ? C25 P1 C19 C24 -54.6(3) . . . . ? In1 P1 C19 C24 65.2(2) . . . . ? C31 P1 C19 C20 -44.1(3) . . . . ? C25 P1 C19 C20 74.1(3) . . . . ? In1 P1 C19 C20 -166.1(2) . . . . ? C24 C19 C20 C21 -58.4(4) . . . . ? P1 C19 C20 C21 172.0(3) . . . . ? C19 C20 C21 C22 57.0(4) . . . . ? C20 C21 C22 C23 -54.8(4) . . . . ? C21 C22 C23 C24 54.5(4) . . . . ? C22 C23 C24 C19 -56.7(4) . . . . ? C20 C19 C24 C23 58.3(4) . . . . ? P1 C19 C24 C23 -169.0(2) . . . . ? C31 P1 C25 C26 42.5(3) . . . . ? C19 P1 C25 C26 -72.9(3) . . . . ? In1 P1 C25 C26 170.7(2) . . . . ? C31 P1 C25 C30 -84.9(3) . . . . ? C19 P1 C25 C30 159.7(2) . . . . ? In1 P1 C25 C30 43.3(3) . . . . ? C30 C25 C26 C27 -56.9(4) . . . . ? P1 C25 C26 C27 174.6(3) . . . . ? C25 C26 C27 C28 57.1(5) . . . . ? C26 C27 C28 C29 -55.7(5) . . . . ? C27 C28 C29 C30 54.7(5) . . . . ? C28 C29 C30 C25 -55.2(4) . . . . ? C26 C25 C30 C29 56.0(4) . . . . ? P1 C25 C30 C29 -174.6(3) . . . . ? C25 P1 C31 C32 63.1(3) . . . . ? C19 P1 C31 C32 -178.8(2) . . . . ? In1 P1 C31 C32 -63.1(3) . . . . ? C25 P1 C31 C36 -173.5(2) . . . . ? C19 P1 C31 C36 -55.4(3) . . . . ? In1 P1 C31 C36 60.4(3) . . . . ? C36 C31 C32 C33 55.5(4) . . . . ? P1 C31 C32 C33 178.7(2) . . . . ? C31 C32 C33 C34 -54.8(4) . . . . ? C32 C33 C34 C35 55.3(4) . . . . ? C33 C34 C35 C36 -56.9(4) . . . . ? C34 C35 C36 C31 58.2(4) . . . . ? C32 C31 C36 C35 -57.6(4) . . . . ? P1 C31 C36 C35 177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.687 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.107