# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address 'T. Chivers' 'Department of Chemistry, 2500 University Drive NW, Calgary, AB T2N 1N4' 'May Copsey' 'Department of Chemistry, 2500 University Drive NW, Calgary, AB T2N 1N4' _publ_contact_author_name 'Tristram Chivers' _publ_contact_author_address ; Chemistry University of Calgary 2500 University Drive NW Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email CHIVERS@UCALGARY.CA _publ_section_title ; Formation of Ga2Te2 and M3Te3 (M = Ga, In) rings from reactions of sodium ditelluroimidodiphosphinate with group 13 halides ; _publ_contact_author_fax 403-289-9488 _publ_contact_author_phone 403-220-5741 data_complex2 _database_code_depnum_ccdc_archive 'CCDC 278063' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Ga2 N2 P4 Te4, 2(C4 H8 O)' _chemical_formula_sum 'C32 H72 Ga2 N2 O2 P4 Te4' _chemical_formula_weight 1290.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 13.478(3) _cell_length_b 8.4926(17) _cell_length_c 21.060(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.42(3) _cell_angle_gamma 90.00 _cell_volume 2403.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 3.661 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7110 _exptl_absorpt_correction_T_max 0.9643 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18982 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4221 _reflns_number_gt 3391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; C-C and C-O distances in the lattice thf molecule have been fixed to reasonable values. 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^)+(0.0201P)^2^+4.4028P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4221 _refine_ls_number_parameters 216 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _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 P1 P 1.03522(8) 0.25846(13) 0.22131(5) 0.0291(3) Uani 1 1 d . . . P2 P 0.87535(8) 0.19735(12) 0.12646(5) 0.0238(2) Uani 1 1 d . . . N1 N 0.9222(2) 0.2708(4) 0.19327(16) 0.0275(8) Uani 1 1 d . . . Te1 Te 1.12666(2) 0.04178(4) 0.175536(15) 0.03926(10) Uani 1 1 d . . . Te2 Te 0.94228(2) -0.20943(3) 0.022401(14) 0.03496(10) Uani 1 1 d . . . Ga1 Ga 0.99841(4) 0.05489(5) 0.07358(2) 0.02853(13) Uani 1 1 d . . . C1 C 1.1042(3) 0.4412(5) 0.2098(2) 0.0355(11) Uani 1 1 d . . . H1 H 1.1740 0.4258 0.2284 0.043 Uiso 1 1 calc R . . C2 C 1.1080(4) 0.4750(6) 0.1386(2) 0.0485(13) Uani 1 1 d . . . H2A H 1.0402 0.4892 0.1191 0.073 Uiso 1 1 calc R . . H2B H 1.1396 0.3864 0.1182 0.073 Uiso 1 1 calc R . . H2C H 1.1466 0.5711 0.1330 0.073 Uiso 1 1 calc R . . C3 C 1.0601(5) 0.5793(6) 0.2434(3) 0.0655(17) Uani 1 1 d . . . H3A H 1.0978 0.6750 0.2354 0.098 Uiso 1 1 calc R . . H3B H 1.0634 0.5587 0.2893 0.098 Uiso 1 1 calc R . . H3C H 0.9905 0.5935 0.2273 0.098 Uiso 1 1 calc R . . C4 C 1.0371(4) 0.2293(6) 0.3074(2) 0.0412(12) Uani 1 1 d . . . H4 H 1.0090 0.3269 0.3256 0.049 Uiso 1 1 calc R . . C5 C 1.1418(4) 0.2098(7) 0.3387(2) 0.0574(15) Uani 1 1 d . . . H5A H 1.1392 0.2033 0.3850 0.086 Uiso 1 1 calc R . . H5B H 1.1825 0.3004 0.3282 0.086 Uiso 1 1 calc R . . H5C H 1.1713 0.1131 0.3231 0.086 Uiso 1 1 calc R . . C6 C 0.9693(4) 0.0929(7) 0.3238(3) 0.0650(18) Uani 1 1 d . . . H6A H 0.9927 -0.0047 0.3051 0.098 Uiso 1 1 calc R . . H6B H 0.9011 0.1147 0.3065 0.098 Uiso 1 1 calc R . . H6C H 0.9707 0.0814 0.3701 0.098 Uiso 1 1 calc R . . C7 C 0.7717(3) 0.0653(5) 0.1409(2) 0.0337(10) Uani 1 1 d . . . H7 H 0.7425 0.0276 0.0985 0.040 Uiso 1 1 calc R . . C8 C 0.8099(4) -0.0786(5) 0.1783(2) 0.0476(13) Uani 1 1 d . . . H8A H 0.8351 -0.0465 0.2212 0.071 Uiso 1 1 calc R . . H8B H 0.8637 -0.1276 0.1565 0.071 Uiso 1 1 calc R . . H8C H 0.7556 -0.1543 0.1811 0.071 Uiso 1 1 calc R . . C9 C 0.6883(4) 0.1423(7) 0.1744(3) 0.0622(16) Uani 1 1 d . . . H9A H 0.6392 0.0624 0.1841 0.093 Uiso 1 1 calc R . . H9B H 0.6562 0.2230 0.1467 0.093 Uiso 1 1 calc R . . H9C H 0.7158 0.1911 0.2141 0.093 Uiso 1 1 calc R . . C10 C 0.7748(4) 0.4878(5) 0.1104(2) 0.0440(12) Uani 1 1 d . . . H10A H 0.7682 0.5821 0.0835 0.066 Uiso 1 1 calc R . . H10B H 0.8137 0.5133 0.1503 0.066 Uiso 1 1 calc R . . H10C H 0.7086 0.4510 0.1197 0.066 Uiso 1 1 calc R . . C11 C 0.8276(3) 0.3587(5) 0.0754(2) 0.0308(10) Uani 1 1 d . . . H11 H 0.8876 0.4101 0.0593 0.037 Uiso 1 1 calc R . . C12 C 0.7660(4) 0.2995(6) 0.0161(2) 0.0409(12) Uani 1 1 d . . . H12A H 0.7031 0.2558 0.0286 0.061 Uiso 1 1 calc R . . H12B H 0.8032 0.2176 -0.0046 0.061 Uiso 1 1 calc R . . H12C H 0.7524 0.3872 -0.0135 0.061 Uiso 1 1 calc R . . O1 O 0.9681(6) 0.2466(9) 0.4905(3) 0.149(3) Uani 1 1 d D . . C13 C 0.8954(5) 0.3674(11) 0.4817(4) 0.109(3) Uani 1 1 d D . . H13A H 0.8399 0.3325 0.4514 0.130 Uiso 1 1 calc R . . H13B H 0.9252 0.4634 0.4645 0.130 Uiso 1 1 calc R . . C14 C 0.8581(6) 0.4009(8) 0.5456(4) 0.096(2) Uani 1 1 d D . . H14A H 0.7875 0.4341 0.5419 0.115 Uiso 1 1 calc R . . H14B H 0.8989 0.4818 0.5692 0.115 Uiso 1 1 calc R . . C16 C 0.9497(8) 0.1676(11) 0.5462(4) 0.128(4) Uani 1 1 d D . . H16A H 1.0106 0.1675 0.5756 0.154 Uiso 1 1 calc R . . H16B H 0.9316 0.0568 0.5362 0.154 Uiso 1 1 calc R . . C15 C 0.8713(7) 0.2415(10) 0.5757(4) 0.118(3) Uani 1 1 d D . . H15A H 0.8882 0.2518 0.6221 0.141 Uiso 1 1 calc R . . H15B H 0.8093 0.1792 0.5689 0.141 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 0.0242(6) 0.0351(6) 0.0275(6) 0.0048(5) -0.0018(5) -0.0024(5) P2 0.0215(6) 0.0255(5) 0.0245(6) -0.0011(4) 0.0022(4) 0.0011(4) N1 0.0204(19) 0.0328(18) 0.029(2) -0.0012(15) 0.0018(15) 0.0018(15) Te1 0.03150(19) 0.04106(18) 0.0443(2) 0.00565(14) -0.00293(14) 0.01166(14) Te2 0.0449(2) 0.02633(15) 0.03511(18) 0.00213(12) 0.01260(14) -0.00097(13) Ga1 0.0296(3) 0.0265(2) 0.0302(3) 0.00213(19) 0.0068(2) 0.0048(2) C1 0.028(3) 0.037(2) 0.040(3) 0.006(2) -0.001(2) -0.010(2) C2 0.047(3) 0.048(3) 0.049(3) 0.017(2) -0.001(3) -0.017(2) C3 0.078(4) 0.043(3) 0.078(4) -0.009(3) 0.018(3) -0.020(3) C4 0.038(3) 0.053(3) 0.032(3) 0.005(2) -0.007(2) -0.006(2) C5 0.050(3) 0.078(4) 0.041(3) 0.013(3) -0.016(3) -0.013(3) C6 0.061(4) 0.096(5) 0.037(3) 0.023(3) -0.008(3) -0.031(3) C7 0.029(3) 0.041(2) 0.032(3) -0.004(2) 0.002(2) -0.009(2) C8 0.060(4) 0.042(3) 0.043(3) 0.003(2) 0.017(3) -0.014(3) C9 0.032(3) 0.059(3) 0.100(5) -0.001(3) 0.034(3) -0.009(3) C10 0.041(3) 0.039(3) 0.052(3) 0.001(2) 0.005(2) 0.010(2) C11 0.027(2) 0.030(2) 0.036(3) 0.0037(19) 0.004(2) 0.0048(19) C12 0.036(3) 0.046(3) 0.039(3) 0.002(2) -0.009(2) 0.002(2) O1 0.153(7) 0.172(7) 0.118(6) -0.020(5) -0.015(5) 0.049(5) C13 0.037(4) 0.178(8) 0.105(6) 0.075(6) -0.033(4) -0.012(5) C14 0.068(5) 0.078(5) 0.143(8) -0.005(5) 0.020(5) 0.012(4) C16 0.185(11) 0.107(7) 0.099(7) 0.025(6) 0.040(7) 0.055(7) C15 0.145(9) 0.093(6) 0.121(7) 0.010(5) 0.055(6) 0.033(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 P1 N1 1.594(3) . ? P1 C4 1.829(5) . ? P1 C1 1.835(4) . ? P1 Te1 2.4530(13) . ? P2 N1 1.622(3) . ? P2 C11 1.828(4) . ? P2 C7 1.836(4) . ? P2 Ga1 2.3957(13) . ? Te1 Ga1 2.6532(10) . ? Te2 Ga1 2.5783(7) . ? Te2 Ga1 2.5876(7) 3_755 ? Ga1 Te2 2.5876(7) 3_755 ? C1 C3 1.515(7) . ? C1 C2 1.530(7) . ? C4 C5 1.520(7) . ? C4 C6 1.530(7) . ? C7 C9 1.519(7) . ? C7 C8 1.521(6) . ? C10 C11 1.527(6) . ? C11 C12 1.529(6) . ? O1 C16 1.390(9) . ? O1 C13 1.422(9) . ? C13 C14 1.498(9) . ? C14 C15 1.500(9) . ? C16 C15 1.414(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 C4 108.4(2) . . ? N1 P1 C1 112.01(19) . . ? C4 P1 C1 106.1(2) . . ? N1 P1 Te1 113.47(13) . . ? C4 P1 Te1 108.60(17) . . ? C1 P1 Te1 107.91(16) . . ? N1 P2 C11 108.54(18) . . ? N1 P2 C7 110.0(2) . . ? C11 P2 C7 108.5(2) . . ? N1 P2 Ga1 111.12(13) . . ? C11 P2 Ga1 109.26(15) . . ? C7 P2 Ga1 109.38(15) . . ? P1 N1 P2 126.4(2) . . ? P1 Te1 Ga1 88.33(3) . . ? Ga1 Te2 Ga1 77.68(2) . 3_755 ? P2 Ga1 Te2 116.28(3) . . ? P2 Ga1 Te2 111.94(4) . 3_755 ? Te2 Ga1 Te2 102.32(2) . 3_755 ? P2 Ga1 Te1 94.37(3) . . ? Te2 Ga1 Te1 116.98(2) . . ? Te2 Ga1 Te1 115.61(2) 3_755 . ? C3 C1 C2 110.9(4) . . ? C3 C1 P1 111.8(3) . . ? C2 C1 P1 110.1(3) . . ? C5 C4 C6 111.8(4) . . ? C5 C4 P1 112.7(4) . . ? C6 C4 P1 111.3(3) . . ? C9 C7 C8 109.8(4) . . ? C9 C7 P2 114.4(3) . . ? C8 C7 P2 110.1(3) . . ? C10 C11 C12 112.7(4) . . ? C10 C11 P2 114.2(3) . . ? C12 C11 P2 112.2(3) . . ? C16 O1 C13 107.0(7) . . ? O1 C13 C14 107.2(6) . . ? C13 C14 C15 99.9(6) . . ? O1 C16 C15 110.2(7) . . ? C16 C15 C14 106.4(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.939 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.101 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 278064' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 In3 N3 P6 Te9, 0.75(C4 H8 O)' _chemical_formula_sum 'C39 H90 In3 N3 O0.75 P6 Te9' _chemical_formula_weight 2291.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.423(3) _cell_length_b 17.204(3) _cell_length_c 27.475(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.31(3) _cell_angle_gamma 90.00 _cell_volume 7763(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4224 _exptl_absorpt_coefficient_mu 4.348 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5252 _exptl_absorpt_correction_T_max 0.6703 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78175 _diffrn_reflns_av_R_equivalents 0.078 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15838 _reflns_number_gt 11660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The lattice thf molecule has been modelled with a four part positional disorder. One of these quarter molecules of thf is further disordered into two positions related by rotation (eg. the oxygen atom occupies two separate positions in the ring). While only three quarters of a thf molecule have been located in the final answer, there is evidence for further disordered solvent, however no suitable model could be refined. All C-C, C-O and cross-molecule distances in the lattice thf have been fixed to reasonable values. 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^)+(0.0492P)^2^+46.1026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15838 _refine_ls_number_parameters 611 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1206 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.007 _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 0.23368(3) 0.91919(3) 0.42495(2) 0.03451(13) Uani 1 1 d . . . In2 In 0.18237(3) 0.82379(3) 0.29805(2) 0.03282(13) Uani 1 1 d . . . In3 In 0.32067(3) 0.99819(3) 0.30096(2) 0.03206(13) Uani 1 1 d . . . P1 P 0.17059(15) 0.84956(14) 0.55708(8) 0.0439(5) Uani 1 1 d . . . P2 P 0.25410(17) 1.00542(17) 0.55954(8) 0.0537(7) Uani 1 1 d . . . P3 P 0.06738(13) 0.61640(13) 0.29864(9) 0.0407(5) Uani 1 1 d . . . P4 P 0.24598(12) 0.59892(11) 0.32423(8) 0.0319(4) Uani 1 1 d . . . P5 P 0.41424(13) 1.20518(13) 0.25575(9) 0.0419(5) Uani 1 1 d . . . P6 P 0.28155(14) 1.22458(12) 0.33184(9) 0.0415(5) Uani 1 1 d . . . N1 N 0.2130(5) 0.9271(5) 0.5767(3) 0.053(2) Uani 1 1 d . A . N2 N 0.1522(4) 0.5809(4) 0.3142(2) 0.0367(15) Uani 1 1 d . . . N3 N 0.3514(4) 1.2408(4) 0.2939(3) 0.0428(17) Uani 1 1 d . . . Te1 Te 0.22755(4) 0.78739(3) 0.48485(2) 0.04761(16) Uani 1 1 d . A . Te2 Te 0.22061(4) 1.05717(3) 0.47898(2) 0.04557(15) Uani 1 1 d . A . Te3 Te 0.06813(4) 0.73275(3) 0.24741(2) 0.04345(15) Uani 1 1 d . . . Te4 Te 0.29467(3) 0.72914(3) 0.348481(19) 0.03278(12) Uani 1 1 d . . . Te5 Te 0.46194(4) 1.07264(3) 0.26714(3) 0.04815(16) Uani 1 1 d . . . Te6 Te 0.20131(3) 1.10385(3) 0.33118(2) 0.03701(13) Uani 1 1 d . . . Te7 Te 0.38142(3) 0.91553(3) 0.379058(19) 0.03514(13) Uani 1 1 d . . . Te8 Te 0.10318(3) 0.91914(3) 0.36277(2) 0.03594(13) Uani 1 1 d . . . Te9 Te 0.25670(4) 0.90991(3) 0.227054(19) 0.03840(13) Uani 1 1 d . . . C1 C 0.0609(7) 0.8629(8) 0.5475(4) 0.078(4) Uani 0.60 1 d P A 1 H1 H 0.0409 0.8101 0.5378 0.094 Uiso 0.60 1 calc PR A 1 C2 C 0.0160(8) 0.8806(9) 0.5945(5) 0.094(5) Uani 0.60 1 d P A 1 H2A H 0.0350 0.8453 0.6202 0.141 Uiso 0.60 1 calc PR A 1 H2B H -0.0426 0.8733 0.5894 0.141 Uiso 0.60 1 calc PR A 1 H2C H 0.0266 0.9344 0.6042 0.141 Uiso 0.60 1 calc PR A 1 C3 C 0.0366(12) 0.9089(11) 0.5112(8) 0.070(5) Uani 0.60 1 d P A 1 H3A H 0.0600 0.8906 0.4806 0.105 Uiso 0.60 1 calc PR A 1 H3B H 0.0549 0.9622 0.5176 0.105 Uiso 0.60 1 calc PR A 1 H3C H -0.0229 0.9079 0.5089 0.105 Uiso 0.60 1 calc PR A 1 C1A C 0.0609(7) 0.8629(8) 0.5475(4) 0.078(4) Uani 0.40 1 d P A 2 H1A H 0.0630 0.9172 0.5346 0.094 Uiso 0.40 1 calc PR A 2 C2A C 0.0160(8) 0.8806(9) 0.5945(5) 0.094(5) Uani 0.40 1 d P A 2 H2D H 0.0531 0.9064 0.6174 0.141 Uiso 0.40 1 calc PR A 2 H2E H -0.0037 0.8320 0.6089 0.141 Uiso 0.40 1 calc PR A 2 H2F H -0.0304 0.9147 0.5875 0.141 Uiso 0.40 1 calc PR A 2 C3A C 0.0235(16) 0.8278(15) 0.5062(9) 0.059(7) Uani 0.40 1 d P A 2 H3D H -0.0244 0.8582 0.4966 0.088 Uiso 0.40 1 calc PR A 2 H3E H 0.0068 0.7747 0.5144 0.088 Uiso 0.40 1 calc PR A 2 H3F H 0.0623 0.8263 0.4793 0.088 Uiso 0.40 1 calc PR A 2 C4 C 0.1819(7) 0.7793(7) 0.6060(4) 0.066(3) Uani 1 1 d . A . H4 H 0.1600 0.8044 0.6360 0.079 Uiso 1 1 calc R . . C5 C 0.2710(9) 0.7635(7) 0.6155(4) 0.086(4) Uani 1 1 d . . . H5A H 0.2771 0.7344 0.6459 0.128 Uiso 1 1 calc R A . H5B H 0.3005 0.8129 0.6180 0.128 Uiso 1 1 calc R . . H5C H 0.2934 0.7329 0.5886 0.128 Uiso 1 1 calc R . . C6 C 0.1345(8) 0.7068(7) 0.5984(5) 0.080(4) Uani 1 1 d . . . H6A H 0.1524 0.6814 0.5684 0.120 Uiso 1 1 calc R A . H6B H 0.0764 0.7194 0.5958 0.120 Uiso 1 1 calc R . . H6C H 0.1434 0.6717 0.6260 0.120 Uiso 1 1 calc R . . C7 C 0.2256(8) 1.0806(7) 0.6036(4) 0.073(3) Uani 1 1 d . A . H7 H 0.2371 1.0586 0.6366 0.087 Uiso 1 1 calc R . . C8 C 0.1367(10) 1.0943(8) 0.6011(5) 0.097(5) Uani 1 1 d . . . H8A H 0.1228 1.1395 0.6211 0.146 Uiso 1 1 calc R A . H8B H 0.1079 1.0484 0.6132 0.146 Uiso 1 1 calc R . . H8C H 0.1206 1.1042 0.5672 0.146 Uiso 1 1 calc R . . C9 C 0.2781(14) 1.1521(10) 0.5988(7) 0.162(9) Uani 1 1 d . . . H9A H 0.2504 1.1903 0.5780 0.243 Uiso 1 1 calc R A . H9B H 0.3303 1.1378 0.5842 0.243 Uiso 1 1 calc R . . H9C H 0.2877 1.1747 0.6311 0.243 Uiso 1 1 calc R . . C10 C 0.3654(7) 1.0006(8) 0.5649(4) 0.079(4) Uani 1 1 d D A . H10 H 0.3877 1.0532 0.5572 0.095 Uiso 1 1 calc R . . C11 C 0.4027(9) 0.9442(10) 0.5313(4) 0.105(5) Uani 1 1 d D . . H11A H 0.4594 0.9349 0.5410 0.158 Uiso 1 1 calc R A . H11B H 0.4012 0.9650 0.4981 0.158 Uiso 1 1 calc R . . H11C H 0.3724 0.8951 0.5324 0.158 Uiso 1 1 calc R . . C12 C 0.3934(10) 0.9788(12) 0.6169(4) 0.159(9) Uani 1 1 d D . . H12A H 0.3741 0.9264 0.6248 0.238 Uiso 1 1 calc R A . H12B H 0.3708 1.0160 0.6402 0.238 Uiso 1 1 calc R . . H12C H 0.4530 0.9800 0.6187 0.238 Uiso 1 1 calc R . . C20 C 0.0150(6) 0.5419(5) 0.2616(4) 0.061(3) Uani 1 1 d . . . H20 H -0.0367 0.5652 0.2490 0.073 Uiso 1 1 calc R . . C21 C -0.0070(7) 0.4722(6) 0.2918(5) 0.077(4) Uani 1 1 d . . . H21A H -0.0307 0.4320 0.2708 0.116 Uiso 1 1 calc R . . H21B H -0.0466 0.4873 0.3166 0.116 Uiso 1 1 calc R . . H21C H 0.0421 0.4517 0.3077 0.116 Uiso 1 1 calc R . . C22 C 0.0675(8) 0.5204(7) 0.2180(4) 0.076(3) Uani 1 1 d . . . H22A H 0.1193 0.4987 0.2294 0.114 Uiso 1 1 calc R . . H22B H 0.0779 0.5669 0.1984 0.114 Uiso 1 1 calc R . . H22C H 0.0389 0.4816 0.1981 0.114 Uiso 1 1 calc R . . C23 C 0.0057(5) 0.6336(6) 0.3518(4) 0.051(2) Uani 1 1 d . . . H23 H 0.0041 0.5837 0.3704 0.061 Uiso 1 1 calc R . . C24 C -0.0837(6) 0.6550(8) 0.3392(5) 0.079(4) Uani 1 1 d . . . H24A H -0.1163 0.6549 0.3690 0.118 Uiso 1 1 calc R . . H24B H -0.1059 0.6168 0.3162 0.118 Uiso 1 1 calc R . . H24C H -0.0854 0.7068 0.3244 0.118 Uiso 1 1 calc R . . C25 C 0.0438(7) 0.6944(6) 0.3853(4) 0.063(3) Uani 1 1 d . . . H25A H 0.0380 0.7460 0.3706 0.094 Uiso 1 1 calc R . . H25B H 0.1017 0.6827 0.3901 0.094 Uiso 1 1 calc R . . H25C H 0.0161 0.6936 0.4169 0.094 Uiso 1 1 calc R . . C26 C 0.2771(6) 0.5332(5) 0.3733(3) 0.047(2) Uani 1 1 d . . . H26 H 0.2633 0.4793 0.3624 0.056 Uiso 1 1 calc R . . C27 C 0.2276(7) 0.5491(6) 0.4188(4) 0.068(3) Uani 1 1 d . . . H27A H 0.2462 0.5148 0.4451 0.101 Uiso 1 1 calc R . . H27B H 0.1699 0.5392 0.4120 0.101 Uiso 1 1 calc R . . H27C H 0.2349 0.6034 0.4286 0.101 Uiso 1 1 calc R . . C28 C 0.3684(6) 0.5346(6) 0.3837(4) 0.066(3) Uani 1 1 d . . . H28A H 0.3844 0.5866 0.3948 0.099 Uiso 1 1 calc R . . H28B H 0.3981 0.5217 0.3539 0.099 Uiso 1 1 calc R . . H28C H 0.3815 0.4964 0.4090 0.099 Uiso 1 1 calc R . . C29 C 0.2875(6) 0.6216(6) 0.2281(3) 0.055(2) Uani 1 1 d . . . H29A H 0.3264 0.6111 0.2020 0.082 Uiso 1 1 calc R . . H29B H 0.2902 0.6766 0.2371 0.082 Uiso 1 1 calc R . . H29C H 0.2324 0.6090 0.2167 0.082 Uiso 1 1 calc R . . C30 C 0.3082(5) 0.5723(5) 0.2717(3) 0.043(2) Uani 1 1 d . . . H30 H 0.3661 0.5838 0.2805 0.051 Uiso 1 1 calc R . . C31 C 0.3037(7) 0.4869(5) 0.2591(4) 0.060(3) Uani 1 1 d . . . H31A H 0.2473 0.4730 0.2511 0.089 Uiso 1 1 calc R . . H31B H 0.3224 0.4560 0.2869 0.089 Uiso 1 1 calc R . . H31C H 0.3384 0.4763 0.2309 0.089 Uiso 1 1 calc R . . C40 C 0.5061(5) 1.2641(5) 0.2572(4) 0.052(2) Uani 1 1 d . . . H40 H 0.5455 1.2420 0.2332 0.063 Uiso 1 1 calc R . . C41 C 0.5459(6) 1.2628(6) 0.3071(4) 0.070(3) Uani 1 1 d . . . H41A H 0.5959 1.2938 0.3064 0.104 Uiso 1 1 calc R . . H41B H 0.5591 1.2091 0.3159 0.104 Uiso 1 1 calc R . . H41C H 0.5083 1.2846 0.3310 0.104 Uiso 1 1 calc R . . C42 C 0.4860(6) 1.3483(5) 0.2418(5) 0.066(3) Uani 1 1 d . . . H42A H 0.4445 1.3697 0.2635 0.099 Uiso 1 1 calc R . . H42B H 0.4654 1.3485 0.2082 0.099 Uiso 1 1 calc R . . H42C H 0.5354 1.3801 0.2438 0.099 Uiso 1 1 calc R . . C43 C 0.3728(6) 1.2124(6) 0.1947(3) 0.054(2) Uani 1 1 d . . . H43 H 0.3528 1.2669 0.1905 0.065 Uiso 1 1 calc R . . C44 C 0.4366(7) 1.1987(8) 0.1554(4) 0.077(3) Uani 1 1 d . . . H44A H 0.4542 1.1443 0.1563 0.116 Uiso 1 1 calc R . . H44B H 0.4835 1.2327 0.1613 0.116 Uiso 1 1 calc R . . H44C H 0.4130 1.2103 0.1234 0.116 Uiso 1 1 calc R . . C45 C 0.2995(6) 1.1592(7) 0.1880(4) 0.064(3) Uani 1 1 d . . . H45A H 0.2725 1.1709 0.1569 0.096 Uiso 1 1 calc R . . H45B H 0.2611 1.1674 0.2147 0.096 Uiso 1 1 calc R . . H45C H 0.3176 1.1049 0.1880 0.096 Uiso 1 1 calc R . . C46 C 0.3224(7) 1.2350(6) 0.3934(4) 0.055(3) Uani 1 1 d . . . H46 H 0.2774 1.2240 0.4168 0.067 Uiso 1 1 calc R . . C47 C 0.3902(7) 1.1746(6) 0.4020(4) 0.060(3) Uani 1 1 d . . . H47A H 0.4359 1.1856 0.3803 0.090 Uiso 1 1 calc R . . H47B H 0.3690 1.1225 0.3953 0.090 Uiso 1 1 calc R . . H47C H 0.4088 1.1775 0.4359 0.090 Uiso 1 1 calc R . . C48 C 0.3532(8) 1.3181(6) 0.4030(5) 0.079(4) Uani 1 1 d . . . H48A H 0.3753 1.3215 0.4361 0.119 Uiso 1 1 calc R . . H48B H 0.3079 1.3548 0.3993 0.119 Uiso 1 1 calc R . . H48C H 0.3959 1.3309 0.3795 0.119 Uiso 1 1 calc R . . C49 C 0.2072(5) 1.3036(5) 0.3233(4) 0.051(2) Uani 1 1 d . . . H49 H 0.2362 1.3541 0.3284 0.061 Uiso 1 1 calc R . . C50 C 0.1749(6) 1.3024(6) 0.2708(4) 0.067(3) Uani 1 1 d . . . H50A H 0.1481 1.2525 0.2644 0.101 Uiso 1 1 calc R . . H50B H 0.2204 1.3091 0.2482 0.101 Uiso 1 1 calc R . . H50C H 0.1357 1.3447 0.2662 0.101 Uiso 1 1 calc R . . C51 C 0.1384(7) 1.2995(7) 0.3592(5) 0.083(4) Uani 1 1 d . . . H51A H 0.1023 1.3443 0.3546 0.125 Uiso 1 1 calc R . . H51B H 0.1606 1.3001 0.3924 0.125 Uiso 1 1 calc R . . H51C H 0.1076 1.2514 0.3540 0.125 Uiso 1 1 calc R . . O1 O 0.462(2) 0.2248(14) 0.5318(14) 0.072(10) Uiso 0.12 1 d PD B 1 C60 C 0.4169(16) 0.2908(17) 0.5284(13) 0.070(10) Uiso 0.12 1 d PD B 1 H60A H 0.3842 0.2966 0.5584 0.084 Uiso 0.12 1 calc PR B 1 H60B H 0.3787 0.2860 0.5006 0.084 Uiso 0.12 1 calc PR B 1 C61 C 0.464(2) 0.3558(15) 0.5223(18) 0.081(14) Uiso 0.12 1 d PD B 1 H61A H 0.4645 0.3875 0.5524 0.097 Uiso 0.12 1 calc PR B 1 H61B H 0.4423 0.3880 0.4952 0.097 Uiso 0.12 1 calc PR B 1 C62 C 0.546(2) 0.326(2) 0.511(2) 0.12(2) Uiso 0.12 1 d PD B 1 H62A H 0.5656 0.3456 0.4791 0.147 Uiso 0.12 1 calc PR B 1 H62B H 0.5863 0.3409 0.5366 0.147 Uiso 0.12 1 calc PR B 1 C63 C 0.532(2) 0.242(2) 0.510(2) 0.12(2) Uiso 0.12 1 d PD B 1 H63A H 0.5309 0.2238 0.4759 0.146 Uiso 0.12 1 calc PR B 1 H63B H 0.5776 0.2153 0.5271 0.146 Uiso 0.12 1 calc PR B 1 O1A O 0.4169(16) 0.2908(17) 0.5284(13) 0.070(10) Uiso 0.13 1 d PD C 2 C60A C 0.464(2) 0.3558(15) 0.5223(18) 0.081(14) Uiso 0.13 1 d PD C 2 H60C H 0.4645 0.3875 0.5524 0.097 Uiso 0.13 1 calc PR C 2 H60D H 0.4423 0.3880 0.4952 0.097 Uiso 0.13 1 calc PR C 2 C61A C 0.546(2) 0.326(2) 0.511(2) 0.12(2) Uiso 0.13 1 d P C 2 H61C H 0.5656 0.3456 0.4791 0.147 Uiso 0.13 1 calc PR C 2 H61D H 0.5863 0.3409 0.5366 0.147 Uiso 0.13 1 calc PR C 2 C62A C 0.532(2) 0.242(2) 0.510(2) 0.12(2) Uiso 0.13 1 d P C 2 H62C H 0.5309 0.2238 0.4759 0.146 Uiso 0.13 1 calc PR C 2 H62D H 0.5776 0.2153 0.5271 0.146 Uiso 0.13 1 calc PR C 2 C63A C 0.462(2) 0.2248(14) 0.5318(14) 0.072(10) Uiso 0.13 1 d P C 2 H63C H 0.4708 0.2103 0.5663 0.086 Uiso 0.13 1 calc PR C 2 H63D H 0.4341 0.1812 0.5150 0.086 Uiso 0.13 1 calc PR C 2 O2 O 0.606(2) 0.465(2) 0.3938(9) 0.101(13) Uani 0.25 1 d PD D 3 C66 C 0.682(2) 0.483(3) 0.4148(13) 0.068(12) Uiso 0.25 1 d PD D 3 H66A H 0.6961 0.5380 0.4093 0.082 Uiso 0.25 1 calc PR D 3 H66B H 0.7250 0.4496 0.4008 0.082 Uiso 0.25 1 calc PR D 3 C67 C 0.673(3) 0.467(4) 0.4664(13) 0.14(3) Uiso 0.25 1 d PD D 3 H67A H 0.6560 0.5150 0.4839 0.165 Uiso 0.25 1 calc PR D 3 H67B H 0.7244 0.4482 0.4806 0.165 Uiso 0.25 1 calc PR D 3 C68 C 0.609(3) 0.408(3) 0.4694(14) 0.11(2) Uiso 0.25 1 d PD D 3 H68A H 0.5803 0.4099 0.5009 0.132 Uiso 0.25 1 calc PR D 3 H68B H 0.6316 0.3550 0.4643 0.132 Uiso 0.25 1 calc PR D 3 C69 C 0.558(2) 0.433(3) 0.4289(15) 0.11(2) Uiso 0.25 1 d PD D 3 H69A H 0.5280 0.3880 0.4152 0.136 Uiso 0.25 1 calc PR D 3 H69B H 0.5176 0.4717 0.4403 0.136 Uiso 0.25 1 calc PR D 3 C72 C 0.941(3) 0.590(2) 0.502(2) 0.102(18) Uiso 0.25 1 d PD . . H72A H 0.9409 0.5533 0.5294 0.122 Uiso 0.25 1 calc PR . . H72B H 0.9937 0.5846 0.4842 0.122 Uiso 0.25 1 calc PR . . C71 C 0.872(4) 0.576(3) 0.469(3) 0.15(3) Uiso 0.25 1 d PD . . H71A H 0.8470 0.5243 0.4743 0.176 Uiso 0.25 1 calc PR . . H71B H 0.8873 0.5812 0.4342 0.176 Uiso 0.25 1 calc PR . . O3 O 0.869(3) 0.704(2) 0.491(2) 0.18(2) Uiso 0.25 1 d PD . . C70 C 0.815(2) 0.642(3) 0.485(2) 0.12(2) Uiso 0.25 1 d PD . . H70A H 0.7731 0.6536 0.4602 0.141 Uiso 0.25 1 calc PR . . H70B H 0.7882 0.6297 0.5163 0.141 Uiso 0.25 1 calc PR . . C73 C 0.929(3) 0.669(3) 0.5181(18) 0.098(17) Uiso 0.25 1 d PD . . H73A H 0.9140 0.6694 0.5529 0.118 Uiso 0.25 1 calc PR . . H73B H 0.9808 0.6989 0.5147 0.118 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0350(3) 0.0384(3) 0.0302(3) 0.0004(2) 0.0005(2) -0.0004(2) In2 0.0315(3) 0.0298(3) 0.0371(3) -0.0007(2) -0.0016(2) 0.0004(2) In3 0.0307(3) 0.0299(3) 0.0356(3) 0.0003(2) 0.0015(2) -0.0015(2) P1 0.0445(13) 0.0544(14) 0.0328(12) 0.0024(10) 0.0031(10) -0.0025(11) P2 0.0568(16) 0.0733(18) 0.0309(12) -0.0049(12) 0.0022(11) -0.0189(13) P3 0.0300(11) 0.0358(11) 0.0561(14) 0.0022(10) -0.0074(10) -0.0038(9) P4 0.0295(11) 0.0255(9) 0.0405(11) 0.0007(8) -0.0026(9) -0.0001(8) P5 0.0312(12) 0.0378(12) 0.0566(14) 0.0118(10) 0.0033(10) -0.0028(9) P6 0.0421(13) 0.0276(11) 0.0550(14) 0.0010(10) 0.0077(11) -0.0013(9) N1 0.060(5) 0.066(5) 0.033(4) -0.001(4) 0.001(4) -0.012(4) N2 0.035(4) 0.035(4) 0.041(4) 0.004(3) -0.003(3) -0.006(3) N3 0.035(4) 0.035(4) 0.059(5) 0.007(3) 0.004(3) -0.004(3) Te1 0.0622(4) 0.0417(3) 0.0390(3) 0.0053(3) 0.0070(3) 0.0067(3) Te2 0.0547(4) 0.0419(3) 0.0402(3) -0.0059(3) 0.0019(3) -0.0002(3) Te3 0.0433(3) 0.0398(3) 0.0471(3) 0.0030(3) -0.0140(3) -0.0033(3) Te4 0.0298(3) 0.0280(2) 0.0405(3) -0.0016(2) -0.0038(2) 0.0006(2) Te5 0.0332(3) 0.0369(3) 0.0745(4) 0.0089(3) 0.0107(3) -0.0004(2) Te6 0.0336(3) 0.0283(3) 0.0493(3) 0.0017(2) 0.0060(2) -0.0006(2) Te7 0.0305(3) 0.0359(3) 0.0390(3) 0.0019(2) -0.0015(2) 0.0001(2) Te8 0.0303(3) 0.0350(3) 0.0425(3) -0.0029(2) -0.0010(2) 0.0046(2) Te9 0.0429(3) 0.0400(3) 0.0324(3) -0.0023(2) 0.0007(2) -0.0029(2) C1 0.055(7) 0.112(10) 0.068(8) -0.045(8) -0.011(6) 0.015(7) C2 0.064(8) 0.126(12) 0.094(10) -0.045(9) 0.023(7) -0.008(8) C3 0.057(12) 0.075(13) 0.079(13) 0.011(11) 0.012(10) 0.001(10) C1A 0.055(7) 0.112(10) 0.068(8) -0.045(8) -0.011(6) 0.015(7) C2A 0.064(8) 0.126(12) 0.094(10) -0.045(9) 0.023(7) -0.008(8) C3A 0.055(16) 0.057(15) 0.064(16) -0.013(13) 0.007(13) 0.000(13) C4 0.083(8) 0.070(7) 0.043(6) 0.016(5) 0.000(5) -0.009(6) C5 0.114(11) 0.075(8) 0.067(8) 0.023(6) -0.033(7) 0.003(8) C6 0.093(10) 0.075(8) 0.073(8) 0.008(6) 0.003(7) -0.018(7) C7 0.083(9) 0.083(8) 0.053(6) -0.020(6) 0.008(6) -0.031(7) C8 0.130(14) 0.082(9) 0.079(9) -0.025(7) 0.024(9) -0.025(9) C9 0.24(2) 0.105(13) 0.143(16) -0.035(12) 0.015(16) -0.097(15) C10 0.070(8) 0.113(10) 0.055(7) 0.027(7) -0.011(6) -0.022(7) C11 0.076(10) 0.168(15) 0.072(9) -0.011(10) -0.019(7) 0.019(10) C12 0.093(12) 0.27(3) 0.111(13) 0.085(15) -0.031(10) -0.085(15) C20 0.055(6) 0.040(5) 0.087(8) 0.002(5) -0.028(6) -0.012(5) C21 0.066(8) 0.043(6) 0.124(11) -0.007(6) -0.017(7) -0.007(5) C22 0.093(9) 0.068(7) 0.067(7) -0.021(6) -0.027(7) -0.017(7) C23 0.034(5) 0.059(6) 0.060(6) 0.011(5) 0.011(4) 0.006(4) C24 0.040(6) 0.100(9) 0.097(9) 0.017(7) 0.009(6) 0.012(6) C25 0.069(7) 0.066(7) 0.053(6) -0.005(5) 0.019(5) 0.000(6) C26 0.049(5) 0.031(4) 0.060(6) 0.013(4) -0.012(4) -0.003(4) C27 0.089(9) 0.064(7) 0.050(6) 0.020(5) -0.009(6) -0.005(6) C28 0.061(7) 0.057(6) 0.079(7) 0.008(5) -0.039(6) 0.011(5) C29 0.069(7) 0.057(6) 0.038(5) 0.000(4) 0.011(5) 0.006(5) C30 0.039(5) 0.039(5) 0.050(5) -0.010(4) 0.015(4) 0.003(4) C31 0.059(7) 0.047(6) 0.073(7) -0.011(5) 0.009(5) 0.007(5) C40 0.033(5) 0.043(5) 0.080(7) 0.008(5) 0.015(5) -0.009(4) C41 0.048(6) 0.059(6) 0.101(9) 0.007(6) -0.008(6) -0.022(5) C42 0.036(5) 0.047(6) 0.116(9) 0.030(6) 0.003(6) -0.006(4) C43 0.050(6) 0.066(6) 0.047(5) 0.013(5) 0.006(4) 0.003(5) C44 0.067(8) 0.103(9) 0.062(7) 0.005(7) 0.009(6) -0.012(7) C45 0.042(6) 0.083(8) 0.067(7) 0.006(6) -0.005(5) -0.006(5) C46 0.065(7) 0.047(5) 0.055(6) -0.007(5) 0.005(5) -0.007(5) C47 0.071(7) 0.052(6) 0.057(6) 0.008(5) -0.003(5) -0.005(5) C48 0.097(10) 0.046(6) 0.096(9) -0.021(6) -0.003(7) -0.008(6) C49 0.039(5) 0.029(4) 0.084(7) 0.006(4) 0.011(5) 0.001(4) C50 0.040(6) 0.049(6) 0.113(10) 0.014(6) -0.010(6) 0.004(5) C51 0.077(8) 0.062(7) 0.111(10) 0.016(7) 0.037(8) 0.035(6) O2 0.12(3) 0.10(3) 0.09(2) 0.00(2) 0.06(2) 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Te8 2.7334(11) . ? In1 Te7 2.7413(11) . ? In1 Te1 2.8040(9) . ? In1 Te2 2.8085(9) . ? In2 Te9 2.7416(9) . ? In2 Te8 2.7513(9) . ? In2 Te3 2.8072(10) . ? In2 Te4 2.8187(9) . ? In3 Te9 2.7404(9) . ? In3 Te7 2.7566(9) . ? In3 Te6 2.8026(9) . ? In3 Te5 2.8126(10) . ? P1 N1 1.597(8) . ? P1 C4 1.816(10) . ? P1 C1 1.833(12) . ? P1 Te1 2.445(2) . ? P2 N1 1.580(8) . ? P2 C7 1.834(11) . ? P2 C10 1.834(12) . ? P2 Te2 2.446(3) . ? P3 N2 1.578(7) . ? P3 C23 1.806(9) . ? P3 C20 1.846(10) . ? P3 Te3 2.447(2) . ? P4 N2 1.593(7) . ? P4 C26 1.830(8) . ? P4 C30 1.832(8) . ? P4 Te4 2.469(2) . ? P5 N3 1.598(7) . ? P5 C43 1.812(10) . ? P5 C40 1.818(9) . ? P5 Te5 2.431(2) . ? P6 N3 1.578(7) . ? P6 C46 1.825(10) . ? P6 C49 1.842(9) . ? P6 Te6 2.460(2) . ? C1 C3 1.33(2) . ? C1 C2 1.522(15) . ? C4 C6 1.485(15) . ? C4 C5 1.510(17) . ? C7 C8 1.480(19) . ? C7 C9 1.508(17) . ? C10 C11 1.476(13) . ? C10 C12 1.545(13) . ? C20 C21 1.504(15) . ? C20 C22 1.526(16) . ? C23 C25 1.526(14) . ? C23 C24 1.551(13) . ? C26 C27 1.519(14) . ? C26 C28 1.526(13) . ? C29 C30 1.504(13) . ? C30 C31 1.512(12) . ? C40 C41 1.515(15) . ? C40 C42 1.544(12) . ? C43 C45 1.524(14) . ? C43 C44 1.526(13) . ? C46 C48 1.539(13) . ? C46 C47 1.540(14) . ? C49 C51 1.505(13) . ? C49 C50 1.535(15) . ? O1 C63 1.341(18) . ? O1 C60 1.355(16) . ? C60 C61 1.368(17) . ? C61 C62 1.486(18) . ? C62 C63 1.466(18) . ? O2 C69 1.372(19) . ? O2 C66 1.394(19) . ? C66 C67 1.450(18) . ? C67 C68 1.460(19) . ? C68 C69 1.462(19) . ? C72 C73 1.450(18) . ? C72 C71 1.474(19) . ? C71 C70 1.54(5) . ? O3 C73 1.386(19) . ? O3 C70 1.388(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 Te8 In1 Te7 113.92(3) . . ? Te8 In1 Te1 109.63(3) . . ? Te7 In1 Te1 106.62(3) . . ? Te8 In1 Te2 105.58(3) . . ? Te7 In1 Te2 109.45(3) . . ? Te1 In1 Te2 111.73(3) . . ? Te9 In2 Te8 110.58(3) . . ? Te9 In2 Te3 104.35(3) . . ? Te8 In2 Te3 109.63(3) . . ? Te9 In2 Te4 111.67(3) . . ? Te8 In2 Te4 109.70(3) . . ? Te3 In2 Te4 110.80(3) . . ? Te9 In3 Te7 115.24(3) . . ? Te9 In3 Te6 108.25(3) . . ? Te7 In3 Te6 110.78(3) . . ? Te9 In3 Te5 108.74(3) . . ? Te7 In3 Te5 101.33(3) . . ? Te6 In3 Te5 112.46(3) . . ? N1 P1 C4 105.3(5) . . ? N1 P1 C1 111.8(5) . . ? C4 P1 C1 106.6(6) . . ? N1 P1 Te1 118.1(3) . . ? C4 P1 Te1 105.7(4) . . ? C1 P1 Te1 108.5(3) . . ? N1 P2 C7 107.1(5) . . ? N1 P2 C10 111.4(5) . . ? C7 P2 C10 103.7(6) . . ? N1 P2 Te2 119.1(3) . . ? C7 P2 Te2 106.4(4) . . ? C10 P2 Te2 108.0(3) . . ? N2 P3 C23 110.0(4) . . ? N2 P3 C20 106.8(4) . . ? C23 P3 C20 107.3(5) . . ? N2 P3 Te3 117.7(3) . . ? C23 P3 Te3 109.6(3) . . ? C20 P3 Te3 104.8(3) . . ? N2 P4 C26 105.8(4) . . ? N2 P4 C30 111.0(4) . . ? C26 P4 C30 105.8(4) . . ? N2 P4 Te4 122.3(3) . . ? C26 P4 Te4 105.8(3) . . ? C30 P4 Te4 105.0(3) . . ? N3 P5 C43 109.9(4) . . ? N3 P5 C40 108.1(4) . . ? C43 P5 C40 106.8(5) . . ? N3 P5 Te5 119.0(3) . . ? C43 P5 Te5 107.6(4) . . ? C40 P5 Te5 104.7(3) . . ? N3 P6 C46 109.3(5) . . ? N3 P6 C49 105.6(4) . . ? C46 P6 C49 106.6(5) . . ? N3 P6 Te6 122.4(3) . . ? C46 P6 Te6 106.5(3) . . ? C49 P6 Te6 105.5(3) . . ? P2 N1 P1 142.9(5) . . ? P3 N2 P4 145.4(4) . . ? P6 N3 P5 147.1(5) . . ? P1 Te1 In1 97.92(6) . . ? P2 Te2 In1 98.81(7) . . ? P3 Te3 In2 100.18(6) . . ? P4 Te4 In2 100.45(5) . . ? P5 Te5 In3 101.76(6) . . ? P6 Te6 In3 100.04(6) . . ? In1 Te7 In3 91.64(3) . . ? In1 Te8 In2 91.85(3) . . ? In3 Te9 In2 86.72(3) . . ? C3 C1 C2 111.8(13) . . ? C3 C1 P1 118.2(12) . . ? C2 C1 P1 112.5(8) . . ? C6 C4 C5 112.3(10) . . ? C6 C4 P1 113.8(8) . . ? C5 C4 P1 110.1(8) . . ? C8 C7 C9 115.5(14) . . ? C8 C7 P2 109.7(8) . . ? C9 C7 P2 111.7(10) . . ? C11 C10 C12 107.3(11) . . ? C11 C10 P2 113.4(9) . . ? C12 C10 P2 112.1(9) . . ? C21 C20 C22 112.2(9) . . ? C21 C20 P3 111.3(8) . . ? C22 C20 P3 109.8(7) . . ? C25 C23 C24 110.9(9) . . ? C25 C23 P3 111.8(6) . . ? C24 C23 P3 113.1(8) . . ? C27 C26 C28 111.9(9) . . ? C27 C26 P4 110.3(7) . . ? C28 C26 P4 113.5(7) . . ? C29 C30 C31 110.8(8) . . ? C29 C30 P4 111.2(6) . . ? C31 C30 P4 113.4(6) . . ? C41 C40 C42 110.6(9) . . ? C41 C40 P5 111.4(7) . . ? C42 C40 P5 110.0(7) . . ? C45 C43 C44 111.6(9) . . ? C45 C43 P5 111.3(7) . . ? C44 C43 P5 112.8(7) . . ? C48 C46 C47 111.3(9) . . ? C48 C46 P6 111.6(8) . . ? C47 C46 P6 109.7(7) . . ? C51 C49 C50 111.1(9) . . ? C51 C49 P6 112.4(7) . . ? C50 C49 P6 109.5(7) . . ? C63 O1 C60 104.7(15) . . ? O1 C60 C61 112.9(14) . . ? C60 C61 C62 105.1(10) . . ? C63 C62 C61 101.3(11) . . ? O1 C63 C62 110.5(15) . . ? C69 O2 C66 108.4(12) . . ? O2 C66 C67 105.6(15) . . ? C66 C67 C68 105.2(16) . . ? C67 C68 C69 99.1(14) . . ? O2 C69 C68 108.6(17) . . ? C73 C72 C71 103.8(12) . . ? C72 C71 C70 100(2) . . ? C73 O3 C70 100.4(17) . . ? O3 C70 C71 102(3) . . ? O3 C73 C72 109.6(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.302 _refine_diff_density_min -1.324 _refine_diff_density_rms 0.174 #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 278065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 Ga3 N3 P6 Te9, C4 H8 O' _chemical_formula_sum 'C40 H92 Ga3 N3 O P6 Te9' _chemical_formula_weight 2174.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.634(3) _cell_length_b 16.349(3) _cell_length_c 16.396(3) _cell_angle_alpha 78.16(3) _cell_angle_beta 85.85(3) _cell_angle_gamma 79.27(3) _cell_volume 3512.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 4.972 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6362 _exptl_absorpt_correction_T_max 0.7223 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55031 _diffrn_reflns_av_R_equivalents 0.125 _diffrn_reflns_av_sigmaI/netI 0.1277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 24.98 _reflns_number_total 12287 _reflns_number_gt 6614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The lattice thf molecule has been modelled to a six-part disorder. The molecule is split over two positions in space (50 % each). Each half of the thf molecule has been modeled over three rotational positions (0.16, 0.17 and 0.17 % occupancy). All C-C, C-O and cross-molecule distances have been fixed to reasonable values. 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^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12287 _refine_ls_number_parameters 578 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1353 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.992 _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 N1 N 0.3411(6) 0.9473(5) 0.4644(6) 0.039(2) Uani 1 1 d . . . P1 P 0.4095(2) 0.85693(18) 0.4744(2) 0.0399(8) Uani 1 1 d . . . P2 P 0.2312(2) 0.99453(17) 0.43193(18) 0.0351(7) Uani 1 1 d . . . P3 P 0.3360(3) 0.8725(2) -0.0252(2) 0.0571(10) Uani 1 1 d . . . P4 P 0.1775(3) 0.7889(2) -0.0783(2) 0.0494(9) Uani 1 1 d . . . P5 P -0.1010(2) 0.54559(18) 0.21877(19) 0.0408(8) Uani 1 1 d . B . P6 P -0.2573(2) 0.59105(18) 0.3474(2) 0.0406(8) Uani 1 1 d . . . N2 N 0.2699(8) 0.8379(6) -0.0807(6) 0.056(3) Uani 1 1 d . . . N3 N -0.1991(6) 0.5469(5) 0.2764(6) 0.041(2) Uani 1 1 d . . . Te1 Te 0.33033(6) 0.73112(5) 0.50349(5) 0.0484(2) Uani 1 1 d . . . Te2 Te 0.14414(6) 0.93953(4) 0.33296(5) 0.0391(2) Uani 1 1 d . . . Te3 Te 0.26088(7) 0.91323(5) 0.10365(5) 0.0574(3) Uani 1 1 d . . . Te4 Te 0.13890(7) 0.69466(5) 0.05154(5) 0.0489(2) Uani 1 1 d . . . Te5 Te 0.04756(6) 0.58916(4) 0.26247(5) 0.0384(2) Uani 1 1 d . . . Te6 Te -0.23193(6) 0.73581(5) 0.34697(5) 0.0450(2) Uani 1 1 d . . . Ga1 Ga 0.18934(9) 0.77336(7) 0.39144(8) 0.0381(3) Uani 1 1 d . . . Ga2 Ga 0.16045(10) 0.78761(8) 0.16212(8) 0.0431(3) Uani 1 1 d . . . Ga3 Ga -0.03518(9) 0.72532(7) 0.32369(7) 0.0353(3) Uani 1 1 d . . . Te7 Te 0.26133(6) 0.68473(5) 0.27978(5) 0.0432(2) Uani 1 1 d . . . Te8 Te -0.01179(6) 0.85945(4) 0.21218(5) 0.0403(2) Uani 1 1 d . . . Te9 Te 0.03393(6) 0.72211(5) 0.46660(5) 0.0409(2) Uani 1 1 d . . . C1 C 0.4871(8) 0.8451(7) 0.5639(7) 0.045(3) Uani 1 1 d . . . H1 H 0.5203 0.8960 0.5545 0.055 Uiso 1 1 calc R . . C2 C 0.4242(9) 0.8459(8) 0.6425(8) 0.059(4) Uani 1 1 d . . . H2A H 0.3998 0.7921 0.6594 0.088 Uiso 1 1 calc R . . H2B H 0.3674 0.8928 0.6330 0.088 Uiso 1 1 calc R . . H2C H 0.4644 0.8535 0.6867 0.088 Uiso 1 1 calc R . . C3 C 0.5710(9) 0.7667(8) 0.5720(8) 0.059(4) Uani 1 1 d . . . H3A H 0.6068 0.7610 0.6232 0.088 Uiso 1 1 calc R . . H3B H 0.6176 0.7735 0.5238 0.088 Uiso 1 1 calc R . . H3C H 0.5419 0.7157 0.5744 0.088 Uiso 1 1 calc R . . C4 C 0.4971(8) 0.8514(7) 0.3848(7) 0.041(3) Uani 1 1 d . . . H4 H 0.5412 0.7944 0.3961 0.050 Uiso 1 1 calc R . . C5 C 0.5635(9) 0.9176(7) 0.3784(8) 0.054(3) Uani 1 1 d . . . H5A H 0.6211 0.9049 0.3409 0.081 Uiso 1 1 calc R . . H5B H 0.5867 0.9167 0.4338 0.081 Uiso 1 1 calc R . . H5C H 0.5254 0.9739 0.3564 0.081 Uiso 1 1 calc R . . C6 C 0.4456(9) 0.8584(8) 0.3038(7) 0.053(3) Uani 1 1 d . . . H6A H 0.3967 0.9113 0.2935 0.079 Uiso 1 1 calc R . . H6B H 0.4114 0.8100 0.3080 0.079 Uiso 1 1 calc R . . H6C H 0.4954 0.8587 0.2576 0.079 Uiso 1 1 calc R . . C7 C 0.2444(9) 1.1023(7) 0.3779(7) 0.044(3) Uani 1 1 d . . . H7 H 0.2776 1.1267 0.4174 0.053 Uiso 1 1 calc R . . C8 C 0.1478(9) 1.1621(7) 0.3567(8) 0.059(4) Uani 1 1 d . . . H8A H 0.1618 1.2156 0.3228 0.088 Uiso 1 1 calc R . . H8B H 0.1114 1.1730 0.4083 0.088 Uiso 1 1 calc R . . H8C H 0.1071 1.1365 0.3254 0.088 Uiso 1 1 calc R . . C9 C 0.3158(9) 1.1004(7) 0.3001(7) 0.050(3) Uani 1 1 d . . . H9A H 0.2846 1.0802 0.2577 0.075 Uiso 1 1 calc R . . H9B H 0.3787 1.0620 0.3159 0.075 Uiso 1 1 calc R . . H9C H 0.3293 1.1577 0.2774 0.075 Uiso 1 1 calc R . . C10 C 0.1430(8) 1.0076(7) 0.5217(6) 0.036(3) Uani 1 1 d . . . H10 H 0.0782 1.0417 0.4998 0.043 Uiso 1 1 calc R . . C11 C 0.1828(9) 1.0555(7) 0.5798(7) 0.048(3) Uani 1 1 d . . . H11A H 0.1332 1.0649 0.6247 0.072 Uiso 1 1 calc R . . H11B H 0.1958 1.1104 0.5480 0.072 Uiso 1 1 calc R . . H11C H 0.2450 1.0219 0.6037 0.072 Uiso 1 1 calc R . . C12 C 0.1237(9) 0.9216(7) 0.5698(7) 0.047(3) Uani 1 1 d . . . H12A H 0.1871 0.8863 0.5893 0.070 Uiso 1 1 calc R . . H12B H 0.0933 0.8936 0.5332 0.070 Uiso 1 1 calc R . . H12C H 0.0784 0.9297 0.6178 0.070 Uiso 1 1 calc R . . C13 C 0.4533(10) 0.7937(9) 0.0005(10) 0.074(4) Uani 1 1 d . . . H13 H 0.4839 0.7793 -0.0533 0.088 Uiso 1 1 calc R . . C14 C 0.4306(11) 0.7136(10) 0.0538(10) 0.087(5) Uani 1 1 d . . . H14A H 0.4932 0.6745 0.0691 0.131 Uiso 1 1 calc R . . H14B H 0.3904 0.6872 0.0229 0.131 Uiso 1 1 calc R . . H14C H 0.3933 0.7263 0.1044 0.131 Uiso 1 1 calc R . . C15 C 0.5304(13) 0.8286(11) 0.0398(12) 0.112(6) Uani 1 1 d . . . H15A H 0.5028 0.8440 0.0926 0.168 Uiso 1 1 calc R . . H15B H 0.5474 0.8791 0.0018 0.168 Uiso 1 1 calc R . . H15C H 0.5907 0.7853 0.0504 0.168 Uiso 1 1 calc R . . C16 C 0.3750(13) 0.9687(9) -0.0872(9) 0.079(5) Uani 1 1 d . . . H16 H 0.4144 0.9924 -0.0513 0.095 Uiso 1 1 calc R . . C17 C 0.2843(13) 1.0337(9) -0.1148(10) 0.089(5) Uani 1 1 d . . . H17A H 0.3044 1.0888 -0.1370 0.133 Uiso 1 1 calc R . . H17B H 0.2373 1.0386 -0.0672 0.133 Uiso 1 1 calc R . . H17C H 0.2520 1.0162 -0.1584 0.133 Uiso 1 1 calc R . . C18 C 0.4411(16) 0.9465(12) -0.1605(11) 0.134(8) Uani 1 1 d . . . H18A H 0.4005 0.9334 -0.2014 0.201 Uiso 1 1 calc R . . H18B H 0.4924 0.8971 -0.1412 0.201 Uiso 1 1 calc R . . H18C H 0.4732 0.9948 -0.1864 0.201 Uiso 1 1 calc R . . C19 C 0.2090(12) 0.7182(9) -0.1553(8) 0.069(4) Uani 1 1 d . . . H19 H 0.1548 0.6836 -0.1508 0.082 Uiso 1 1 calc R . . C20 C 0.3023(11) 0.6593(9) -0.1388(10) 0.083(5) Uani 1 1 d . . . H20A H 0.3075 0.6150 -0.1718 0.124 Uiso 1 1 calc R . . H20B H 0.3041 0.6334 -0.0793 0.124 Uiso 1 1 calc R . . H20C H 0.3583 0.6900 -0.1540 0.124 Uiso 1 1 calc R . . C21 C 0.2085(14) 0.7725(11) -0.2456(8) 0.105(6) Uani 1 1 d . . . H21A H 0.2375 0.8232 -0.2459 0.157 Uiso 1 1 calc R . . H21B H 0.1397 0.7897 -0.2642 0.157 Uiso 1 1 calc R . . H21C H 0.2481 0.7388 -0.2834 0.157 Uiso 1 1 calc R . . C22 C 0.0655(11) 0.8644(8) -0.1120(8) 0.059(4) Uani 1 1 d . . . H22 H 0.0825 0.9014 -0.1658 0.070 Uiso 1 1 calc R . . C23 C 0.0297(10) 0.9202(8) -0.0506(8) 0.064(4) Uani 1 1 d . . . H23A H -0.0264 0.9638 -0.0733 0.096 Uiso 1 1 calc R . . H23B H 0.0842 0.9475 -0.0394 0.096 Uiso 1 1 calc R . . H23C H 0.0077 0.8859 0.0015 0.096 Uiso 1 1 calc R . . C24 C -0.0218(12) 0.8216(10) -0.1274(9) 0.085(5) Uani 1 1 d . . . H24A H -0.0366 0.7817 -0.0766 0.128 Uiso 1 1 calc R . . H24B H -0.0029 0.7909 -0.1732 0.128 Uiso 1 1 calc R . . H24C H -0.0811 0.8651 -0.1420 0.128 Uiso 1 1 calc R . . C25 C -0.1306(10) 0.6050(8) 0.1109(7) 0.053(3) Uani 1 1 d . . . H25 H -0.0663 0.6007 0.0774 0.063 Uiso 1 1 calc R . . C26 C -0.1657(10) 0.6982(7) 0.1120(8) 0.060(4) Uani 1 1 d . . . H26A H -0.1770 0.7298 0.0549 0.090 Uiso 1 1 calc R . . H26B H -0.1146 0.7199 0.1364 0.090 Uiso 1 1 calc R . . H26C H -0.2281 0.7053 0.1455 0.090 Uiso 1 1 calc R . . C27 C -0.2013(11) 0.5654(9) 0.0688(8) 0.073(4) Uani 1 1 d . . . H27A H -0.2590 0.5554 0.1064 0.110 Uiso 1 1 calc R . . H27B H -0.1661 0.5114 0.0559 0.110 Uiso 1 1 calc R . . H27C H -0.2242 0.6041 0.0172 0.110 Uiso 1 1 calc R . . C28 C -0.0610(10) 0.4338(8) 0.2093(8) 0.060(4) Uani 1 1 d D . . H28 H -0.1165 0.4150 0.1854 0.072 Uiso 1 1 calc R A 1 C29 C -0.0381(11) 0.3778(7) 0.2929(8) 0.068(4) Uani 1 1 d . B . H29A H -0.0280 0.3182 0.2876 0.101 Uiso 1 1 calc R . . H29B H -0.0940 0.3892 0.3324 0.101 Uiso 1 1 calc R . . H29C H 0.0227 0.3896 0.3132 0.101 Uiso 1 1 calc R . . C30 C 0.0353(19) 0.413(2) 0.1573(18) 0.053(9) Uiso 0.50 1 d PD B 1 H30A H 0.0900 0.4324 0.1791 0.080 Uiso 0.50 1 calc PR B 1 H30B H 0.0253 0.4413 0.0991 0.080 Uiso 0.50 1 calc PR B 1 H30C H 0.0520 0.3513 0.1606 0.080 Uiso 0.50 1 calc PR B 1 C30A C 0.014(2) 0.431(3) 0.1329(19) 0.084(13) Uiso 0.50 1 d PD B 2 H30D H -0.0095 0.4780 0.0872 0.125 Uiso 0.50 1 calc PR B 2 H30E H 0.0184 0.3770 0.1147 0.125 Uiso 0.50 1 calc PR B 2 H30F H 0.0800 0.4364 0.1489 0.125 Uiso 0.50 1 calc PR B 2 C31 C -0.2287(9) 0.5259(7) 0.4518(7) 0.046(3) Uani 1 1 d . . . H31 H -0.2352 0.4663 0.4503 0.055 Uiso 1 1 calc R . . C32 C -0.3020(10) 0.5553(8) 0.5200(7) 0.065(4) Uani 1 1 d . . . H32A H -0.2892 0.5151 0.5729 0.097 Uiso 1 1 calc R . . H32B H -0.3707 0.5579 0.5042 0.097 Uiso 1 1 calc R . . H32C H -0.2930 0.6118 0.5264 0.097 Uiso 1 1 calc R . . C33 C -0.1230(10) 0.5248(7) 0.4727(7) 0.055(4) Uani 1 1 d . . . H33A H -0.1167 0.5807 0.4826 0.083 Uiso 1 1 calc R . . H33B H -0.0779 0.5112 0.4262 0.083 Uiso 1 1 calc R . . H33C H -0.1054 0.4817 0.5230 0.083 Uiso 1 1 calc R . . C34 C -0.3908(9) 0.6003(8) 0.3332(8) 0.056(4) Uani 1 1 d . . . H34 H -0.4276 0.6311 0.3761 0.067 Uiso 1 1 calc R . . C35 C -0.4220(10) 0.5125(8) 0.3470(10) 0.079(5) Uani 1 1 d . . . H35A H -0.4938 0.5197 0.3387 0.118 Uiso 1 1 calc R . . H35B H -0.4071 0.4820 0.4039 0.118 Uiso 1 1 calc R . . H35C H -0.3850 0.4800 0.3071 0.118 Uiso 1 1 calc R . . C36 C -0.4201(9) 0.6527(9) 0.2474(9) 0.069(4) Uani 1 1 d . . . H36A H -0.3915 0.6208 0.2042 0.103 Uiso 1 1 calc R . . H36B H -0.3945 0.7062 0.2384 0.103 Uiso 1 1 calc R . . H36C H -0.4930 0.6649 0.2444 0.103 Uiso 1 1 calc R . . C43 C 0.334(5) 0.448(3) 0.102(2) 0.24(3) Uiso 0.17 1 d PD C 1 H43A H 0.2691 0.4781 0.0779 0.291 Uiso 0.17 1 calc PR C 1 H43B H 0.3871 0.4553 0.0575 0.291 Uiso 0.17 1 calc PR C 1 O1 O 0.353(4) 0.481(2) 0.169(3) 0.19(2) Uiso 0.17 1 d PD C 1 C40 C 0.322(4) 0.427(3) 0.239(2) 0.148(17) Uiso 0.17 1 d PD C 1 H40A H 0.2528 0.4504 0.2559 0.177 Uiso 0.17 1 calc PR C 1 H40B H 0.3661 0.4215 0.2855 0.177 Uiso 0.17 1 calc PR C 1 C41 C 0.326(3) 0.3501(19) 0.216(2) 0.143(14) Uiso 0.17 1 d PD C 1 H41A H 0.3848 0.3096 0.2394 0.172 Uiso 0.17 1 calc PR C 1 H41B H 0.2650 0.3263 0.2374 0.172 Uiso 0.17 1 calc PR C 1 C42 C 0.331(4) 0.363(2) 0.131(2) 0.171(18) Uiso 0.17 1 d PD C 1 H42A H 0.2725 0.3478 0.1100 0.205 Uiso 0.17 1 calc PR C 1 H42B H 0.3923 0.3281 0.1121 0.205 Uiso 0.17 1 calc PR C 1 C41A C 0.334(5) 0.448(3) 0.102(2) 0.24(3) Uiso 0.16 1 d P D 2 H41C H 0.2691 0.4781 0.0779 0.291 Uiso 0.16 1 calc PR D 2 H41D H 0.3871 0.4553 0.0575 0.291 Uiso 0.16 1 calc PR D 2 C42A C 0.353(4) 0.481(2) 0.169(3) 0.19(2) Uiso 0.16 1 d PD D 2 H42C H 0.4258 0.4810 0.1710 0.227 Uiso 0.16 1 calc PR D 2 H42D H 0.3166 0.5393 0.1658 0.227 Uiso 0.16 1 calc PR D 2 C43A C 0.322(4) 0.427(3) 0.239(2) 0.148(17) Uiso 0.16 1 d PD D 2 H43C H 0.2528 0.4504 0.2559 0.177 Uiso 0.16 1 calc PR D 2 H43D H 0.3661 0.4215 0.2855 0.177 Uiso 0.16 1 calc PR D 2 O1A O 0.326(3) 0.3501(19) 0.216(2) 0.143(14) Uiso 0.16 1 d PD D 2 C40A C 0.331(4) 0.363(2) 0.131(2) 0.171(18) Uiso 0.16 1 d PD D 2 H40C H 0.2725 0.3478 0.1100 0.205 Uiso 0.16 1 calc PR D 2 H40D H 0.3923 0.3281 0.1121 0.205 Uiso 0.16 1 calc PR D 2 C40B C 0.334(5) 0.448(3) 0.102(2) 0.24(3) Uiso 0.17 1 d PD E 3 H40E H 0.2691 0.4781 0.0779 0.291 Uiso 0.17 1 calc PR E 3 H40F H 0.3871 0.4553 0.0575 0.291 Uiso 0.17 1 calc PR E 3 C41B C 0.353(4) 0.481(2) 0.169(3) 0.19(2) Uiso 0.17 1 d PD E 3 H41E H 0.4258 0.4810 0.1710 0.227 Uiso 0.17 1 calc PR E 3 H41F H 0.3166 0.5393 0.1658 0.227 Uiso 0.17 1 calc PR E 3 C42B C 0.322(4) 0.427(3) 0.239(2) 0.148(17) Uiso 0.17 1 d P E 3 H42E H 0.2528 0.4504 0.2559 0.177 Uiso 0.17 1 calc PR E 3 H42F H 0.3661 0.4215 0.2855 0.177 Uiso 0.17 1 calc PR E 3 C43B C 0.326(3) 0.3501(19) 0.216(2) 0.143(14) Uiso 0.17 1 d PD E 3 H43E H 0.3848 0.3096 0.2394 0.172 Uiso 0.17 1 calc PR E 3 H43F H 0.2650 0.3263 0.2374 0.172 Uiso 0.17 1 calc PR E 3 O1B O 0.331(4) 0.363(2) 0.131(2) 0.171(18) Uiso 0.17 1 d PD E 3 C52 C 0.423(3) 0.4799(17) 0.160(2) 0.107(12) Uiso 0.17 1 d PD F 4 H52A H 0.4900 0.4953 0.1568 0.128 Uiso 0.17 1 calc PR F 4 H52B H 0.3725 0.5303 0.1671 0.128 Uiso 0.17 1 calc PR F 4 C51 C 0.415(4) 0.414(2) 0.2257(17) 0.188(19) Uiso 0.17 1 d PD F 4 H51A H 0.3566 0.4296 0.2621 0.226 Uiso 0.17 1 calc PR F 4 H51B H 0.4760 0.4013 0.2591 0.226 Uiso 0.17 1 calc PR F 4 C50 C 0.405(4) 0.3445(18) 0.193(2) 0.147(17) Uiso 0.17 1 d PD F 4 H50A H 0.4631 0.2982 0.2084 0.177 Uiso 0.17 1 calc PR F 4 H50B H 0.3436 0.3235 0.2165 0.177 Uiso 0.17 1 calc PR F 4 O2 O 0.402(3) 0.3697(18) 0.1087(19) 0.121(12) Uiso 0.17 1 d PD F 4 C53 C 0.406(3) 0.4541(19) 0.0883(15) 0.131(13) Uiso 0.17 1 d PD F 4 H53A H 0.3431 0.4866 0.0640 0.157 Uiso 0.17 1 calc PR F 4 H53B H 0.4615 0.4638 0.0468 0.157 Uiso 0.17 1 calc PR F 4 O2A O 0.415(4) 0.414(2) 0.2257(17) 0.188(19) Uiso 0.17 1 d PD G 5 C50A C 0.423(3) 0.4799(17) 0.160(2) 0.107(12) Uiso 0.17 1 d PD G 5 H50C H 0.4900 0.4953 0.1568 0.128 Uiso 0.17 1 calc PR G 5 H50D H 0.3725 0.5303 0.1671 0.128 Uiso 0.17 1 calc PR G 5 C51A C 0.406(3) 0.4541(19) 0.0883(15) 0.131(13) Uiso 0.17 1 d P G 5 H51C H 0.3431 0.4866 0.0640 0.157 Uiso 0.17 1 calc PR G 5 H51D H 0.4615 0.4638 0.0468 0.157 Uiso 0.17 1 calc PR G 5 C52A C 0.402(3) 0.3697(18) 0.1087(19) 0.121(12) Uiso 0.17 1 d P G 5 H52C H 0.4582 0.3367 0.0814 0.146 Uiso 0.17 1 calc PR G 5 H52D H 0.3386 0.3595 0.0893 0.146 Uiso 0.17 1 calc PR G 5 C53A C 0.405(4) 0.3445(18) 0.193(2) 0.147(17) Uiso 0.17 1 d PD G 5 H53C H 0.4631 0.2982 0.2084 0.177 Uiso 0.17 1 calc PR G 5 H53D H 0.3436 0.3235 0.2165 0.177 Uiso 0.17 1 calc PR G 5 C53B C 0.423(3) 0.4799(17) 0.160(2) 0.107(12) Uiso 0.16 1 d PD H 6 H53E H 0.4900 0.4953 0.1568 0.128 Uiso 0.16 1 calc PR H 6 H53F H 0.3725 0.5303 0.1671 0.128 Uiso 0.16 1 calc PR H 6 C52B C 0.415(4) 0.414(2) 0.2257(17) 0.188(19) Uiso 0.16 1 d PD H 6 H52E H 0.3566 0.4296 0.2621 0.226 Uiso 0.16 1 calc PR H 6 H52F H 0.4760 0.4013 0.2591 0.226 Uiso 0.16 1 calc PR H 6 C51B C 0.405(4) 0.3445(18) 0.193(2) 0.147(17) Uiso 0.16 1 d P H 6 H51E H 0.4631 0.2982 0.2084 0.177 Uiso 0.16 1 calc PR H 6 H51F H 0.3436 0.3235 0.2165 0.177 Uiso 0.16 1 calc PR H 6 C50B C 0.402(3) 0.3697(18) 0.1087(19) 0.121(12) Uiso 0.16 1 d PD H 6 H50E H 0.4582 0.3367 0.0814 0.146 Uiso 0.16 1 calc PR H 6 H50F H 0.3386 0.3595 0.0893 0.146 Uiso 0.16 1 calc PR H 6 O2B O 0.406(3) 0.4541(19) 0.0883(15) 0.131(13) Uiso 0.16 1 d PD H 6 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 N1 0.025(5) 0.037(5) 0.057(6) -0.019(5) 0.001(5) 0.001(4) P1 0.0343(19) 0.0380(17) 0.051(2) -0.0157(15) -0.0041(15) -0.0064(14) P2 0.0322(18) 0.0329(16) 0.0425(18) -0.0127(14) -0.0033(14) -0.0052(14) P3 0.067(3) 0.065(2) 0.050(2) -0.0198(18) 0.0050(19) -0.030(2) P4 0.062(2) 0.0494(19) 0.042(2) -0.0106(16) 0.0034(17) -0.0233(18) P5 0.044(2) 0.0412(17) 0.0429(19) -0.0140(15) -0.0050(16) -0.0131(15) P6 0.0329(18) 0.0367(17) 0.052(2) -0.0086(15) -0.0041(16) -0.0060(14) N2 0.059(7) 0.052(6) 0.063(7) -0.013(5) -0.012(6) -0.023(6) N3 0.029(6) 0.041(5) 0.055(6) -0.010(5) -0.002(5) -0.012(4) Te1 0.0485(5) 0.0414(5) 0.0573(5) -0.0066(4) -0.0149(4) -0.0114(4) Te2 0.0398(5) 0.0401(4) 0.0411(5) -0.0139(4) -0.0047(4) -0.0089(4) Te3 0.0687(7) 0.0605(5) 0.0518(6) -0.0183(4) 0.0073(5) -0.0293(5) Te4 0.0638(6) 0.0459(5) 0.0409(5) -0.0104(4) 0.0006(4) -0.0177(4) Te5 0.0364(5) 0.0382(4) 0.0431(5) -0.0138(4) -0.0020(4) -0.0066(4) Te6 0.0326(5) 0.0355(4) 0.0668(6) -0.0121(4) 0.0007(4) -0.0041(4) Ga1 0.0352(8) 0.0407(7) 0.0421(8) -0.0147(6) -0.0044(6) -0.0080(6) Ga2 0.0447(9) 0.0475(8) 0.0400(8) -0.0125(6) 0.0018(7) -0.0125(7) Ga3 0.0320(8) 0.0363(7) 0.0391(7) -0.0094(6) -0.0011(6) -0.0076(6) Te7 0.0385(5) 0.0455(5) 0.0487(5) -0.0181(4) -0.0026(4) -0.0053(4) Te8 0.0438(5) 0.0374(4) 0.0400(5) -0.0062(4) -0.0027(4) -0.0088(4) Te9 0.0433(5) 0.0444(4) 0.0376(5) -0.0097(4) -0.0012(4) -0.0128(4) C1 0.027(7) 0.056(8) 0.057(8) -0.019(6) -0.012(6) -0.006(6) C2 0.040(8) 0.080(9) 0.064(9) -0.029(7) -0.011(7) -0.009(7) C3 0.044(9) 0.067(9) 0.068(9) -0.017(7) -0.020(7) -0.007(7) C4 0.037(7) 0.035(6) 0.052(8) -0.014(6) 0.002(6) 0.002(6) C5 0.038(8) 0.051(8) 0.072(9) -0.018(7) 0.002(7) 0.001(6) C6 0.044(8) 0.060(8) 0.061(9) -0.028(7) 0.007(7) -0.015(7) C7 0.048(8) 0.040(7) 0.046(7) -0.022(6) 0.007(6) -0.001(6) C8 0.051(9) 0.053(8) 0.071(9) -0.022(7) -0.008(7) 0.009(7) C9 0.047(8) 0.045(7) 0.057(8) -0.010(6) 0.004(7) -0.012(6) C10 0.017(6) 0.054(7) 0.040(7) -0.027(6) -0.003(5) 0.005(5) C11 0.045(8) 0.060(8) 0.046(8) -0.032(6) 0.010(6) -0.009(6) C12 0.045(8) 0.049(7) 0.049(8) -0.005(6) -0.007(6) -0.017(6) C13 0.042(9) 0.081(10) 0.101(12) -0.027(9) -0.006(8) -0.009(8) C14 0.059(11) 0.096(12) 0.102(13) -0.020(10) -0.015(9) 0.005(9) C15 0.084(14) 0.109(13) 0.153(18) -0.023(13) -0.009(13) -0.040(11) C16 0.089(13) 0.084(11) 0.068(10) -0.012(9) 0.020(10) -0.036(10) C17 0.103(14) 0.063(10) 0.095(13) 0.007(9) -0.004(11) -0.025(10) C18 0.18(2) 0.137(16) 0.098(14) -0.020(12) 0.066(15) -0.098(16) C19 0.093(13) 0.074(10) 0.050(9) -0.022(7) 0.004(8) -0.034(9) C20 0.076(12) 0.068(10) 0.101(12) -0.046(9) 0.016(10) 0.020(9) C21 0.151(18) 0.151(16) 0.041(9) -0.043(10) 0.024(10) -0.083(14) C22 0.085(11) 0.054(8) 0.038(8) 0.003(6) -0.019(7) -0.023(8) C23 0.074(11) 0.056(8) 0.060(9) -0.010(7) -0.016(8) -0.003(7) C24 0.086(13) 0.093(11) 0.079(11) -0.022(9) -0.014(9) -0.010(10) C25 0.056(9) 0.066(9) 0.040(8) -0.006(6) -0.005(7) -0.024(7) C26 0.064(10) 0.051(8) 0.065(9) -0.001(7) -0.016(7) -0.012(7) C27 0.086(12) 0.094(11) 0.055(9) -0.010(8) -0.022(8) -0.049(9) C28 0.066(10) 0.058(8) 0.068(9) -0.032(7) 0.012(8) -0.026(7) C29 0.090(11) 0.038(7) 0.077(10) -0.021(7) -0.019(9) 0.001(7) C31 0.040(8) 0.029(6) 0.068(9) -0.013(6) 0.012(7) -0.006(6) C32 0.072(10) 0.068(9) 0.045(8) -0.006(7) 0.002(7) 0.005(8) C33 0.066(10) 0.044(7) 0.050(8) 0.000(6) -0.007(7) -0.004(7) C34 0.031(8) 0.070(9) 0.065(9) -0.013(7) 0.008(7) -0.009(7) C35 0.049(9) 0.072(9) 0.129(14) -0.024(9) -0.016(9) -0.037(8) C36 0.022(7) 0.098(11) 0.082(11) -0.028(9) -0.007(7) 0.011(7) _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 N1 P1 1.578(9) . ? N1 P2 1.624(9) . ? P1 C1 1.828(12) . ? P1 C4 1.831(11) . ? P1 Te1 2.444(3) . ? P2 C7 1.837(11) . ? P2 C10 1.854(10) . ? P2 Te2 2.475(3) . ? P3 N2 1.575(10) . ? P3 C16 1.834(13) . ? P3 C13 1.872(14) . ? P3 Te3 2.442(4) . ? P4 N2 1.609(10) . ? P4 C22 1.817(14) . ? P4 C19 1.858(13) . ? P4 Te4 2.444(3) . ? P5 N3 1.581(9) . ? P5 C28 1.843(12) . ? P5 C25 1.867(12) . ? P5 Te5 2.466(3) . ? P6 N3 1.583(9) . ? P6 C34 1.825(12) . ? P6 C31 1.847(12) . ? P6 Te6 2.453(3) . ? Te1 Ga1 2.6540(18) . ? Te2 Ga1 2.6596(16) . ? Te3 Ga2 2.6573(16) . ? Te4 Ga2 2.6566(17) . ? Te5 Ga3 2.6559(16) . ? Te6 Ga3 2.6605(15) . ? Ga1 Te9 2.5631(16) . ? Ga1 Te7 2.5911(17) . ? Ga2 Te7 2.5755(18) . ? Ga2 Te8 2.5802(17) . ? Ga3 Te9 2.5753(16) . ? Ga3 Te8 2.6047(16) . ? C1 C2 1.497(15) . ? C1 C3 1.540(16) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.519(15) . ? C4 C6 1.522(16) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.503(15) . ? C7 C9 1.550(14) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.523(14) . ? C10 C11 1.534(14) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.489(18) . ? C13 C15 1.52(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.50(2) . ? C16 C18 1.51(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.451(19) . ? C19 C21 1.562(18) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.492(17) . ? C22 C24 1.547(18) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.514(16) . ? C25 C27 1.527(16) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.501(17) . ? C28 C30 1.536(17) . ? C28 C30A 1.561(18) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31 C33 1.500(16) . ? C31 C32 1.537(15) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.528(17) . ? C34 C35 1.539(16) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C43 C42 1.379(17) . ? C43 O1 1.384(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O1 C40 1.378(18) . ? C40 C41 1.381(17) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.362(16) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C52 C51 1.369(16) . ? C52 C53 1.372(16) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C51 C50 1.382(16) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C50 O2 1.369(16) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O2 C53 1.364(16) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 N1 P2 139.3(6) . . ? N1 P1 C1 107.1(5) . . ? N1 P1 C4 110.7(5) . . ? C1 P1 C4 105.4(5) . . ? N1 P1 Te1 118.8(3) . . ? C1 P1 Te1 104.6(4) . . ? C4 P1 Te1 109.2(4) . . ? N1 P2 C7 106.6(5) . . ? N1 P2 C10 110.3(5) . . ? C7 P2 C10 106.0(5) . . ? N1 P2 Te2 121.4(3) . . ? C7 P2 Te2 104.6(4) . . ? C10 P2 Te2 106.8(3) . . ? N2 P3 C16 108.3(7) . . ? N2 P3 C13 109.6(6) . . ? C16 P3 C13 106.2(7) . . ? N2 P3 Te3 118.2(4) . . ? C16 P3 Te3 105.3(5) . . ? C13 P3 Te3 108.5(5) . . ? N2 P4 C22 110.0(6) . . ? N2 P4 C19 106.7(6) . . ? C22 P4 C19 107.6(7) . . ? N2 P4 Te4 118.3(4) . . ? C22 P4 Te4 109.2(4) . . ? C19 P4 Te4 104.5(4) . . ? N3 P5 C28 105.1(5) . . ? N3 P5 C25 110.4(5) . . ? C28 P5 C25 105.5(6) . . ? N3 P5 Te5 120.5(4) . . ? C28 P5 Te5 105.5(4) . . ? C25 P5 Te5 108.7(4) . . ? N3 P6 C34 107.6(6) . . ? N3 P6 C31 111.2(5) . . ? C34 P6 C31 107.8(5) . . ? N3 P6 Te6 116.2(3) . . ? C34 P6 Te6 105.3(4) . . ? C31 P6 Te6 108.3(4) . . ? P3 N2 P4 143.9(7) . . ? P5 N3 P6 142.0(6) . . ? P1 Te1 Ga1 101.54(9) . . ? P2 Te2 Ga1 100.72(8) . . ? P3 Te3 Ga2 101.05(9) . . ? P4 Te4 Ga2 100.62(9) . . ? P5 Te5 Ga3 101.21(8) . . ? P6 Te6 Ga3 103.30(9) . . ? Te9 Ga1 Te7 111.06(5) . . ? Te9 Ga1 Te1 105.85(5) . . ? Te7 Ga1 Te1 102.88(6) . . ? Te9 Ga1 Te2 108.68(6) . . ? Te7 Ga1 Te2 114.38(6) . . ? Te1 Ga1 Te2 113.60(6) . . ? Te7 Ga2 Te8 113.51(6) . . ? Te7 Ga2 Te4 105.60(5) . . ? Te8 Ga2 Te4 110.36(6) . . ? Te7 Ga2 Te3 107.73(6) . . ? Te8 Ga2 Te3 105.48(6) . . ? Te4 Ga2 Te3 114.34(5) . . ? Te9 Ga3 Te8 113.87(5) . . ? Te9 Ga3 Te5 111.53(6) . . ? Te8 Ga3 Te5 108.08(5) . . ? Te9 Ga3 Te6 106.42(6) . . ? Te8 Ga3 Te6 104.98(6) . . ? Te5 Ga3 Te6 111.82(5) . . ? Ga2 Te7 Ga1 93.53(5) . . ? Ga2 Te8 Ga3 92.60(5) . . ? Ga1 Te9 Ga3 88.98(5) . . ? C2 C1 C3 111.9(10) . . ? C2 C1 P1 110.9(8) . . ? C3 C1 P1 113.0(8) . . ? C2 C1 H1 106.9 . . ? C3 C1 H1 106.9 . . ? P1 C1 H1 106.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 112.2(9) . . ? C5 C4 P1 109.6(8) . . ? C6 C4 P1 113.0(8) . . ? C5 C4 H4 107.2 . . ? C6 C4 H4 107.2 . . ? P1 C4 H4 107.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 111.2(10) . . ? C8 C7 P2 115.1(8) . . ? C9 C7 P2 111.3(7) . . ? C8 C7 H7 106.2 . . ? C9 C7 H7 106.2 . . ? P2 C7 H7 106.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.3(9) . . ? C12 C10 P2 110.6(7) . . ? C11 C10 P2 110.9(7) . . ? C12 C10 H10 108.3 . . ? C11 C10 H10 108.3 . . ? P2 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.1(14) . . ? C14 C13 P3 110.9(10) . . ? C15 C13 P3 113.1(11) . . ? C14 C13 H13 107.1 . . ? C15 C13 H13 107.1 . . ? P3 C13 H13 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 111.7(15) . . ? C17 C16 P3 109.6(10) . . ? C18 C16 P3 109.7(11) . . ? C17 C16 H16 108.6 . . ? C18 C16 H16 108.6 . . ? P3 C16 H16 108.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 112.0(13) . . ? C20 C19 P4 112.7(10) . . ? C21 C19 P4 109.9(10) . . ? C20 C19 H19 107.3 . . ? C21 C19 H19 107.3 . . ? P4 C19 H19 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 108.1(12) . . ? C23 C22 P4 111.7(9) . . ? C24 C22 P4 113.2(9) . . ? C23 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? P4 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 114.2(11) . . ? C26 C25 P5 109.6(8) . . ? C27 C25 P5 112.6(8) . . ? C26 C25 H25 106.6 . . ? C27 C25 H25 106.6 . . ? P5 C25 H25 106.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 102.9(16) . . ? C29 C28 C30A 121.9(19) . . ? C29 C28 P5 111.1(8) . . ? C30 C28 P5 116.8(14) . . ? C30A C28 P5 108.1(17) . . ? C29 C28 H28 108.6 . . ? C30 C28 H28 108.6 . . ? C30A C28 H28 97.3 . . ? P5 C28 H28 108.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? C28 C30A H30D 109.5 . . ? C28 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C28 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C33 C31 C32 110.6(11) . . ? C33 C31 P6 110.9(8) . . ? C32 C31 P6 112.3(8) . . ? C33 C31 H31 107.6 . . ? C32 C31 H31 107.6 . . ? P6 C31 H31 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C35 111.2(12) . . ? C36 C34 P6 110.8(8) . . ? C35 C34 P6 111.6(9) . . ? C36 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? P6 C34 H34 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C43 O1 106.2(12) . . ? C42 C43 H43A 110.5 . . ? O1 C43 H43A 110.5 . . ? C42 C43 H43B 110.5 . . ? O1 C43 H43B 110.5 . . ? H43A C43 H43B 108.7 . . ? C40 O1 C43 105.8(13) . . ? O1 C40 C41 106.3(11) . . ? O1 C40 H40A 110.5 . . ? C41 C40 H40A 110.5 . . ? O1 C40 H40B 110.5 . . ? C41 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? C42 C41 C40 107.5(9) . . ? C42 C41 H41A 110.2 . . ? C40 C41 H41A 110.2 . . ? C42 C41 H41B 110.2 . . ? C40 C41 H41B 110.2 . . ? H41A C41 H41B 108.5 . . ? C41 C42 C43 107.9(9) . . ? C41 C42 H42A 110.1 . . ? C43 C42 H42A 110.1 . . ? C41 C42 H42B 110.1 . . ? C43 C42 H42B 110.1 . . ? H42A C42 H42B 108.4 . . ? C51 C52 C53 108.0(9) . . ? C51 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? C51 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C51 C50 107.7(8) . . ? C52 C51 H51A 110.2 . . ? C50 C51 H51A 110.2 . . ? C52 C51 H51B 110.2 . . ? C50 C51 H51B 110.2 . . ? H51A C51 H51B 108.5 . . ? O2 C50 C51 107.5(8) . . ? O2 C50 H50A 110.2 . . ? C51 C50 H50A 110.2 . . ? O2 C50 H50B 110.2 . . ? C51 C50 H50B 110.2 . . ? H50A C50 H50B 108.5 . . ? C53 O2 C50 108.5(8) . . ? O2 C53 C52 107.8(8) . . ? O2 C53 H53A 110.2 . . ? C52 C53 H53A 110.2 . . ? O2 C53 H53B 110.2 . . ? C52 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.573 _refine_diff_density_min -1.207 _refine_diff_density_rms 0.181