# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #TrackingRef '- Comb CIF.CIF' _publ_contact_author_email chhbsia@chem.iitb.ac.in _publ_contact_author_name 'Prof. Harkesh B. Singh' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Powai, Mumbai-40076 India ; _publ_section_title ; ? ; loop_ _publ_author_name P.Rakesh H.Singh R.Butcher data_5 _database_code_depnum_ccdc_archive 'CCDC 835165' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 Cl3 N O Te' _chemical_formula_sum 'C11 H12 Cl3 N O Te' _chemical_formula_weight 408.17 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8565(2) _cell_length_b 12.1571(3) _cell_length_c 13.2983(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1431.82(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6371 _cell_measurement_theta_min 4.5295 _cell_measurement_theta_max 34.6771 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 2.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58670 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Oxford Diffraction Gemini' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 9905 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 34.76 _reflns_number_total 5448 _reflns_number_gt 4856 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(14) _refine_ls_number_reflns 5448 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0484 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 Cl1 Cl 1.16162(8) 0.84583(5) 0.24953(5) 0.03415(14) Uani 1 1 d . . . Cl2 Cl 0.97636(7) 0.52469(6) 0.05408(5) 0.03112(13) Uani 1 1 d . . . Cl3 Cl 1.20244(8) 0.75979(6) -0.00901(5) 0.03349(14) Uani 1 1 d . . . Te Te 1.055547(15) 0.696484(12) 0.139512(10) 0.01983(3) Uani 1 1 d . . . O O 1.02219(19) 0.51759(16) 0.41370(13) 0.0291(4) Uani 1 1 d . . . N N 0.9665(2) 0.62344(16) 0.28245(13) 0.0222(4) Uani 1 1 d . . . C1 C 1.2395(3) 0.6009(2) 0.19314(17) 0.0213(4) Uani 1 1 d . . . C2 C 1.3789(3) 0.5906(2) 0.1462(2) 0.0295(5) Uani 1 1 d . . . H2A H 1.3995 0.6284 0.0851 0.035 Uiso 1 1 calc R . . C3 C 1.4869(3) 0.5243(3) 0.1902(2) 0.0346(6) Uani 1 1 d . . . H3A H 1.5823 0.5166 0.1583 0.042 Uiso 1 1 calc R . . C4 C 1.4607(3) 0.4689(3) 0.2788(2) 0.0365(6) Uani 1 1 d . . . H4A H 1.5372 0.4237 0.3071 0.044 Uiso 1 1 calc R . . C5 C 1.3219(3) 0.4794(2) 0.3268(2) 0.0307(5) Uani 1 1 d . . . H5A H 1.3029 0.4420 0.3882 0.037 Uiso 1 1 calc R . . C6 C 1.2117(3) 0.5452(2) 0.28347(18) 0.0222(4) Uani 1 1 d . . . C7 C 1.0626(3) 0.56195(18) 0.32725(16) 0.0222(4) Uani 1 1 d . . . C8 C 0.8672(3) 0.5568(2) 0.4332(2) 0.0299(6) Uani 1 1 d . . . H8A H 0.8632 0.5996 0.4965 0.036 Uiso 1 1 calc R . . H8B H 0.7964 0.4941 0.4385 0.036 Uiso 1 1 calc R . . C9 C 0.8262(3) 0.6301(2) 0.34273(17) 0.0247(5) Uani 1 1 d . . . H9A H 0.7398 0.5974 0.3047 0.030 Uiso 1 1 calc R . . C10 C 0.7915(4) 0.7485(2) 0.3709(3) 0.0428(7) Uani 1 1 d . . . H10A H 0.7826 0.7934 0.3091 0.051 Uiso 1 1 calc R . . H10B H 0.8754 0.7786 0.4117 0.051 Uiso 1 1 calc R . . C11 C 0.6447(5) 0.7553(3) 0.4306(3) 0.0703(13) Uani 1 1 d . . . H11A H 0.6297 0.8309 0.4542 0.105 Uiso 1 1 calc R . . H11B H 0.6502 0.7056 0.4886 0.105 Uiso 1 1 calc R . . H11C H 0.5600 0.7338 0.3875 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0407(3) 0.0242(3) 0.0376(3) -0.0059(3) 0.0044(3) -0.0061(3) Cl2 0.0339(3) 0.0281(3) 0.0313(3) -0.0009(3) -0.0068(2) -0.0062(3) Cl3 0.0397(3) 0.0298(3) 0.0309(3) 0.0056(3) 0.0111(2) -0.0030(3) Te 0.01880(5) 0.01967(6) 0.02101(6) 0.00233(6) 0.00137(5) -0.00016(6) O 0.0263(9) 0.0331(10) 0.0279(9) 0.0108(8) 0.0024(7) 0.0017(8) N 0.0183(9) 0.0263(10) 0.0219(9) 0.0019(8) 0.0011(7) -0.0007(8) C1 0.0184(10) 0.0224(11) 0.0232(10) -0.0022(9) -0.0026(8) -0.0003(9) C2 0.0230(10) 0.0399(13) 0.0257(11) -0.0067(12) 0.0016(9) -0.0008(10) C3 0.0197(11) 0.0459(17) 0.0383(14) -0.0105(13) -0.0021(9) 0.0054(11) C4 0.0252(13) 0.0431(15) 0.0413(14) -0.0036(12) -0.0077(11) 0.0115(13) C5 0.0283(13) 0.0323(13) 0.0315(12) 0.0016(11) -0.0065(10) 0.0049(11) C6 0.0170(10) 0.0237(11) 0.0259(11) 0.0002(9) -0.0017(8) -0.0012(9) C7 0.0224(10) 0.0206(10) 0.0237(9) 0.0009(8) -0.0028(9) -0.0025(10) C8 0.0280(13) 0.0295(13) 0.0322(13) 0.0066(11) 0.0095(10) -0.0016(10) C9 0.0192(10) 0.0272(11) 0.0276(12) 0.0020(10) 0.0052(8) -0.0011(9) C10 0.0487(17) 0.0319(14) 0.0480(17) 0.0068(14) 0.0186(15) 0.0109(13) C11 0.069(3) 0.065(2) 0.077(3) 0.017(2) 0.042(2) 0.037(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 Cl1 Te 2.5139(7) . ? Cl2 Te 2.4789(7) . ? Cl3 Te 2.4871(6) . ? Te C1 2.125(2) . ? Te N 2.2414(18) . ? O C7 1.319(3) . ? O C8 1.476(3) . ? N C7 1.280(3) . ? N C9 1.481(3) . ? C1 C2 1.389(3) . ? C1 C6 1.401(3) . ? C2 C3 1.381(4) . ? C2 H2A 0.9500 . ? C3 C4 1.377(4) . ? C3 H3A 0.9500 . ? C4 C5 1.390(4) . ? C4 H4A 0.9500 . ? C5 C6 1.387(3) . ? C5 H5A 0.9500 . ? C6 C7 1.457(3) . ? C8 C9 1.540(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.519(4) . ? C9 H9A 1.0000 . ? C10 C11 1.526(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te N 76.61(8) . . ? C1 Te Cl2 84.83(7) . . ? N Te Cl2 87.44(5) . . ? C1 Te Cl3 91.99(7) . . ? N Te Cl3 168.55(5) . . ? Cl2 Te Cl3 92.57(2) . . ? C1 Te Cl1 85.02(7) . . ? N Te Cl1 85.64(5) . . ? Cl2 Te Cl1 168.81(2) . . ? Cl3 Te Cl1 92.48(2) . . ? C7 O C8 105.87(19) . . ? C7 N C9 109.75(19) . . ? C7 N Te 113.09(16) . . ? C9 N Te 137.11(15) . . ? C2 C1 C6 119.9(2) . . ? C2 C1 Te 125.42(18) . . ? C6 C1 Te 114.66(16) . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C4 C3 C2 122.1(2) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 119.0(3) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C1 120.7(2) . . ? C5 C6 C7 123.5(2) . . ? C1 C6 C7 115.7(2) . . ? N C7 O 117.6(2) . . ? N C7 C6 119.9(2) . . ? O C7 C6 122.5(2) . . ? O C8 C9 105.59(18) . . ? O C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? O C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? N C9 C10 110.8(2) . . ? N C9 C8 101.15(19) . . ? C10 C9 C8 113.8(2) . . ? N C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? C8 C9 H9A 110.3 . . ? C9 C10 C11 110.6(3) . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? 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 . . ? 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 C1 Te N C7 0.15(16) . . . . ? Cl2 Te N C7 85.44(16) . . . . ? Cl3 Te N C7 -4.9(4) . . . . ? Cl1 Te N C7 -85.76(16) . . . . ? C1 Te N C9 177.2(2) . . . . ? Cl2 Te N C9 -97.6(2) . . . . ? Cl3 Te N C9 172.15(19) . . . . ? Cl1 Te N C9 91.2(2) . . . . ? N Te C1 C2 -179.9(2) . . . . ? Cl2 Te C1 C2 91.6(2) . . . . ? Cl3 Te C1 C2 -0.8(2) . . . . ? Cl1 Te C1 C2 -93.2(2) . . . . ? N Te C1 C6 0.27(17) . . . . ? Cl2 Te C1 C6 -88.32(17) . . . . ? Cl3 Te C1 C6 179.28(17) . . . . ? Cl1 Te C1 C6 86.97(17) . . . . ? C6 C1 C2 C3 0.5(4) . . . . ? Te C1 C2 C3 -179.40(19) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C4 C5 C6 C7 -180.0(2) . . . . ? C2 C1 C6 C5 -0.2(4) . . . . ? Te C1 C6 C5 179.73(19) . . . . ? C2 C1 C6 C7 179.5(2) . . . . ? Te C1 C6 C7 -0.6(3) . . . . ? C9 N C7 O 0.3(3) . . . . ? Te N C7 O 178.12(16) . . . . ? C9 N C7 C6 -178.4(2) . . . . ? Te N C7 C6 -0.5(3) . . . . ? C8 O C7 N -0.5(3) . . . . ? C8 O C7 C6 178.1(2) . . . . ? C5 C6 C7 N -179.6(2) . . . . ? C1 C6 C7 N 0.8(3) . . . . ? C5 C6 C7 O 1.8(4) . . . . ? C1 C6 C7 O -177.8(2) . . . . ? C7 O C8 C9 0.5(3) . . . . ? C7 N C9 C10 121.0(3) . . . . ? Te N C9 C10 -56.1(3) . . . . ? C7 N C9 C8 0.1(3) . . . . ? Te N C9 C8 -177.01(18) . . . . ? O C8 C9 N -0.3(2) . . . . ? O C8 C9 C10 -119.2(2) . . . . ? N C9 C10 C11 178.5(3) . . . . ? C8 C9 C10 C11 -68.3(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A Cl1 0.95 2.93 3.684(3) 137.3 3_845 C5 H5A Cl2 0.95 2.98 3.512(3) 117.1 2_765 C5 H5A Cl3 0.95 2.81 3.643(3) 147.1 2_765 C8 H8B Cl2 0.99 2.87 3.581(3) 129.2 2_665 C8 H8B Cl3 0.99 3.00 3.800(3) 138.8 3_745 _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.735 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.091 # ==== data_6 _database_code_depnum_ccdc_archive 'CCDC 835166' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 Br3 N O Te' _chemical_formula_sum 'C11 H12 Br3 N O Te' _chemical_formula_weight 541.55 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.5355(3) _cell_length_b 12.8672(4) _cell_length_c 15.3557(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1488.90(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11098 _cell_measurement_theta_min 4.7490 _cell_measurement_theta_max 34.6862 _exptl_crystal_description 'distorted tetrahedron' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 10.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36655 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Oxford Diffraction Gemini' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 23521 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 34.80 _reflns_number_total 6047 _reflns_number_gt 4353 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+4.2826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(13) _refine_ls_number_reflns 6047 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Te Te -0.09137(5) 0.10740(3) 1.02066(3) 0.02362(9) Uani 1 1 d . . . Br1 Br 0.21554(10) 0.17243(5) 1.08632(5) 0.03606(16) Uani 1 1 d . . . Br2 Br -0.27339(11) 0.16600(6) 1.15842(5) 0.04154(18) Uani 1 1 d . . . Br3 Br -0.37447(10) 0.01491(6) 0.94794(5) 0.04167(19) Uani 1 1 d . . . O1 O 0.1797(7) -0.1277(4) 0.8769(3) 0.0385(12) Uani 1 1 d . . . N1 N 0.0733(7) 0.0260(4) 0.9180(3) 0.0260(10) Uani 1 1 d . . . C1 C -0.0315(8) -0.0412(4) 1.0778(4) 0.0243(12) Uani 1 1 d . . . C2 C -0.0730(9) -0.0690(5) 1.1617(4) 0.0312(13) Uani 1 1 d . . . H2A H -0.1276 -0.0209 1.2003 0.037 Uiso 1 1 calc R . . C3 C -0.0321(9) -0.1712(6) 1.1890(5) 0.0347(15) Uani 1 1 d . . . H3A H -0.0590 -0.1919 1.2469 0.042 Uiso 1 1 calc R . . C4 C 0.0462(10) -0.2414(5) 1.1331(5) 0.0364(16) Uani 1 1 d . . . H4A H 0.0711 -0.3100 1.1524 0.044 Uiso 1 1 calc R . . C5 C 0.0889(11) -0.2120(5) 1.0485(5) 0.0354(15) Uani 1 1 d . . . H5A H 0.1427 -0.2604 1.0099 0.042 Uiso 1 1 calc R . . C6 C 0.0522(8) -0.1111(5) 1.0207(4) 0.0278(12) Uani 1 1 d . . . C7 C 0.1029(10) -0.0705(5) 0.9368(4) 0.0303(13) Uani 1 1 d . . . C8 C 0.2084(13) -0.0596(6) 0.8014(5) 0.047(2) Uani 1 1 d . . . H8A H 0.1452 -0.0868 0.7497 0.057 Uiso 1 1 calc R . . H8B H 0.3365 -0.0545 0.7876 0.057 Uiso 1 1 calc R . . C9 C 0.1335(9) 0.0484(5) 0.8279(4) 0.0294(13) Uani 1 1 d . . . H9A H 0.2306 0.1013 0.8286 0.035 Uiso 1 1 calc R . . C10 C -0.0172(10) 0.0853(6) 0.7724(4) 0.0358(16) Uani 1 1 d . . . H10A H -0.0695 0.1482 0.7992 0.043 Uiso 1 1 calc R . . H10B H -0.1102 0.0309 0.7710 0.043 Uiso 1 1 calc R . . C11 C 0.0385(10) 0.1106(8) 0.6791(5) 0.0448(18) Uani 1 1 d . . . H11A H -0.0651 0.1344 0.6460 0.067 Uiso 1 1 calc R . . H11B H 0.0876 0.0482 0.6516 0.067 Uiso 1 1 calc R . . H11C H 0.1286 0.1655 0.6798 0.067 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 Te 0.02792(18) 0.01838(14) 0.02455(16) -0.00171(15) -0.00201(16) 0.00205(15) Br1 0.0388(4) 0.0336(3) 0.0358(3) 0.0070(3) -0.0074(3) -0.0119(3) Br2 0.0489(4) 0.0329(3) 0.0428(4) -0.0085(3) 0.0124(3) 0.0030(3) Br3 0.0354(4) 0.0401(4) 0.0495(4) -0.0062(3) -0.0093(3) -0.0037(3) O1 0.049(3) 0.029(2) 0.037(3) -0.007(2) 0.007(2) 0.013(2) N1 0.026(3) 0.029(2) 0.023(2) -0.002(2) -0.002(2) 0.006(2) C1 0.024(3) 0.017(2) 0.032(3) 0.000(2) -0.002(2) -0.001(2) C2 0.030(3) 0.032(3) 0.032(3) 0.006(3) -0.001(3) -0.001(3) C3 0.032(3) 0.036(3) 0.036(4) 0.014(3) 0.000(3) -0.006(3) C4 0.036(4) 0.024(3) 0.049(4) 0.012(3) -0.009(3) -0.004(3) C5 0.038(4) 0.025(3) 0.043(4) -0.003(3) -0.012(3) 0.005(3) C6 0.033(3) 0.017(2) 0.033(3) -0.003(3) -0.008(3) 0.002(2) C7 0.029(3) 0.030(3) 0.032(3) -0.011(3) -0.005(3) 0.004(3) C8 0.062(5) 0.046(4) 0.034(4) -0.003(3) 0.004(4) 0.022(4) C9 0.028(3) 0.035(3) 0.024(3) -0.001(3) 0.003(2) 0.000(3) C10 0.034(4) 0.046(4) 0.028(3) 0.011(3) -0.006(3) -0.002(3) C11 0.038(4) 0.065(5) 0.031(3) 0.004(4) -0.003(3) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te C1 2.152(6) . ? Te N1 2.263(5) . ? Te Br2 2.6314(8) . ? Te Br1 2.6581(8) . ? Te Br3 2.6859(8) . ? Te Br1 3.5835(8) 4_457 ? O1 C7 1.312(8) . ? O1 C8 1.469(9) . ? N1 C7 1.294(8) . ? N1 C9 1.485(8) . ? C1 C2 1.373(9) . ? C1 C6 1.406(8) . ? C2 C3 1.415(10) . ? C2 H2A 0.9500 . ? C3 C4 1.379(11) . ? C3 H3A 0.9500 . ? C4 C5 1.390(10) . ? C4 H4A 0.9500 . ? C5 C6 1.395(8) . ? C5 H5A 0.9500 . ? C6 C7 1.442(9) . ? C8 C9 1.554(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.497(9) . ? C9 H9A 1.0000 . ? C10 C11 1.528(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te N1 76.0(2) . . ? C1 Te Br2 92.06(17) . . ? N1 Te Br2 168.03(13) . . ? C1 Te Br1 86.70(16) . . ? N1 Te Br1 86.14(14) . . ? Br2 Te Br1 93.35(3) . . ? C1 Te Br3 86.71(17) . . ? N1 Te Br3 86.61(14) . . ? Br2 Te Br3 92.71(3) . . ? Br1 Te Br3 171.20(3) . . ? C1 Te Br1 167.08(16) . 4_457 ? N1 Te Br1 105.64(13) . 4_457 ? Br2 Te Br1 86.01(2) . 4_457 ? Br1 Te Br1 106.159(17) . 4_457 ? Br3 Te Br1 80.63(2) . 4_457 ? C7 O1 C8 106.5(5) . . ? C7 N1 C9 109.9(5) . . ? C7 N1 Te 112.6(4) . . ? C9 N1 Te 136.6(4) . . ? C2 C1 C6 121.4(6) . . ? C2 C1 Te 124.5(5) . . ? C6 C1 Te 114.1(4) . . ? C1 C2 C3 118.1(6) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 121.2(6) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 119.5(7) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 119.6(6) . . ? C5 C6 C7 123.9(6) . . ? C1 C6 C7 116.4(5) . . ? N1 C7 O1 117.2(6) . . ? N1 C7 C6 120.0(6) . . ? O1 C7 C6 122.7(6) . . ? O1 C8 C9 105.8(5) . . ? O1 C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? O1 C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? N1 C9 C10 111.1(5) . . ? N1 C9 C8 100.5(5) . . ? C10 C9 C8 114.2(6) . . ? N1 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? C9 C10 C11 113.1(6) . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? 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 . . ? 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 C1 Te N1 C7 8.3(5) . . . . ? Br2 Te N1 C7 7.8(10) . . . . ? Br1 Te N1 C7 95.8(5) . . . . ? Br3 Te N1 C7 -79.2(5) . . . . ? Br1 Te N1 C7 -158.5(4) 4_457 . . . ? C1 Te N1 C9 176.1(6) . . . . ? Br2 Te N1 C9 175.7(4) . . . . ? Br1 Te N1 C9 -96.3(6) . . . . ? Br3 Te N1 C9 88.7(6) . . . . ? Br1 Te N1 C9 9.4(6) 4_457 . . . ? N1 Te C1 C2 173.9(6) . . . . ? Br2 Te C1 C2 -6.2(6) . . . . ? Br1 Te C1 C2 87.0(5) . . . . ? Br3 Te C1 C2 -98.8(5) . . . . ? Br1 Te C1 C2 -87.3(9) 4_457 . . . ? N1 Te C1 C6 -7.6(4) . . . . ? Br2 Te C1 C6 172.3(4) . . . . ? Br1 Te C1 C6 -94.5(4) . . . . ? Br3 Te C1 C6 79.7(4) . . . . ? Br1 Te C1 C6 91.2(9) 4_457 . . . ? C6 C1 C2 C3 -1.1(10) . . . . ? Te C1 C2 C3 177.3(5) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C3 C4 C5 C6 0.1(11) . . . . ? C4 C5 C6 C1 -1.6(10) . . . . ? C4 C5 C6 C7 175.2(7) . . . . ? C2 C1 C6 C5 2.2(9) . . . . ? Te C1 C6 C5 -176.4(5) . . . . ? C2 C1 C6 C7 -174.9(6) . . . . ? Te C1 C6 C7 6.6(7) . . . . ? C9 N1 C7 O1 1.2(9) . . . . ? Te N1 C7 O1 172.4(5) . . . . ? C9 N1 C7 C6 -178.8(6) . . . . ? Te N1 C7 C6 -7.7(8) . . . . ? C8 O1 C7 N1 -0.6(9) . . . . ? C8 O1 C7 C6 179.4(7) . . . . ? C5 C6 C7 N1 -175.8(7) . . . . ? C1 C6 C7 N1 1.1(9) . . . . ? C5 C6 C7 O1 4.1(10) . . . . ? C1 C6 C7 O1 -179.0(6) . . . . ? C7 O1 C8 C9 -0.2(8) . . . . ? C7 N1 C9 C10 120.1(7) . . . . ? Te N1 C9 C10 -48.0(9) . . . . ? C7 N1 C9 C8 -1.2(7) . . . . ? Te N1 C9 C8 -169.3(5) . . . . ? O1 C8 C9 N1 0.8(8) . . . . ? O1 C8 C9 C10 -118.2(7) . . . . ? N1 C9 C10 C11 179.3(6) . . . . ? C8 C9 C10 C11 -67.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.838 _refine_diff_density_min -2.002 _refine_diff_density_rms 0.202 # ==== data_7 _database_code_depnum_ccdc_archive 'CCDC 835167' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_absolute_configuration ad _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 I3 N O Te' _chemical_formula_sum 'C11 H12 I3 N O Te' _chemical_formula_weight 682.52 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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.79100(10) _cell_length_b 13.6338(2) _cell_length_c 15.5148(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1648.00(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19180 _cell_measurement_theta_min 4.6630 _cell_measurement_theta_max 37.4626 _exptl_crystal_description chunk _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 7.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.29377 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 34752 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.67 _diffrn_reflns_theta_max 37.58 _reflns_number_total 8380 _reflns_number_gt 7351 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 8380 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0447 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 I1 I 0.76900(2) 0.325576(13) 1.083486(10) 0.03026(4) Uani 1 1 d . . . I2 I 1.39199(3) 0.494010(15) 0.940356(13) 0.03662(5) Uani 1 1 d . . . I3 I 1.27665(3) 0.330649(14) 1.166903(11) 0.03320(4) Uani 1 1 d . . . Te Te 1.09304(2) 0.398106(11) 1.020017(9) 0.01991(3) Uani 1 1 d . . . O O 0.8234(3) 0.62040(16) 0.87866(13) 0.0368(5) Uani 1 1 d . . . N N 0.9323(3) 0.47604(16) 0.91772(13) 0.0248(4) Uani 1 1 d . . . C1 C 1.0346(3) 0.53865(17) 1.07606(16) 0.0231(4) Uani 1 1 d . . . C2 C 1.0810(4) 0.5670(2) 1.15784(17) 0.0294(5) Uani 1 1 d . . . H2A H 1.1358 0.5224 1.1960 0.035 Uiso 1 1 calc R . . C3 C 1.0453(4) 0.6637(2) 1.1836(2) 0.0374(6) Uani 1 1 d . . . H3A H 1.0749 0.6842 1.2402 0.045 Uiso 1 1 calc R . . C4 C 0.9692(5) 0.7286(2) 1.1289(2) 0.0386(7) Uani 1 1 d . . . H4A H 0.9483 0.7938 1.1478 0.046 Uiso 1 1 calc R . . C5 C 0.9216(5) 0.7013(2) 1.04640(19) 0.0353(6) Uani 1 1 d . . . H5A H 0.8698 0.7472 1.0084 0.042 Uiso 1 1 calc R . . C6 C 0.9516(3) 0.60421(18) 1.02005(17) 0.0257(4) Uani 1 1 d . . . C7 C 0.9015(4) 0.56640(19) 0.93706(16) 0.0270(5) Uani 1 1 d . . . C8 C 0.7987(5) 0.5583(2) 0.80355(18) 0.0373(7) Uani 1 1 d . . . H8A H 0.8636 0.5841 0.7536 0.045 Uiso 1 1 calc R . . H8B H 0.6756 0.5547 0.7880 0.045 Uiso 1 1 calc R . . C9 C 0.8674(4) 0.4549(2) 0.83010(16) 0.0278(5) Uani 1 1 d . . . H9A H 0.7709 0.4066 0.8328 0.033 Uiso 1 1 calc R . . C10 C 1.0105(4) 0.4161(2) 0.77289(16) 0.0325(6) Uani 1 1 d . . . H10A H 1.0588 0.3558 0.7990 0.039 Uiso 1 1 calc R . . H10B H 1.1034 0.4655 0.7696 0.039 Uiso 1 1 calc R . . C11 C 0.9470(5) 0.3928(3) 0.68139(18) 0.0440(8) Uani 1 1 d . . . H11A H 1.0393 0.3611 0.6487 0.066 Uiso 1 1 calc R . . H11B H 0.9133 0.4537 0.6525 0.066 Uiso 1 1 calc R . . H11C H 0.8480 0.3486 0.6846 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02900(8) 0.03135(8) 0.03044(7) -0.00616(6) 0.00620(6) -0.00940(7) I2 0.02850(9) 0.04111(10) 0.04025(9) 0.00764(8) 0.00765(7) -0.00544(8) I3 0.03580(9) 0.03137(8) 0.03244(8) 0.00757(7) -0.00817(7) 0.00140(8) Te 0.02172(6) 0.01833(6) 0.01969(5) 0.00115(5) 0.00240(5) 0.00188(5) O 0.0435(13) 0.0338(11) 0.0331(9) 0.0106(8) -0.0044(8) 0.0131(9) N 0.0264(11) 0.0270(9) 0.0211(8) 0.0028(7) -0.0014(8) 0.0031(8) C1 0.0238(11) 0.0177(10) 0.0278(11) -0.0015(8) 0.0030(9) 0.0002(8) C2 0.0277(13) 0.0292(12) 0.0312(12) -0.0067(10) -0.0015(10) 0.0018(10) C3 0.0375(16) 0.0336(14) 0.0411(15) -0.0152(12) 0.0003(12) -0.0030(13) C4 0.0411(17) 0.0225(13) 0.0523(18) -0.0118(12) 0.0078(14) 0.0016(12) C5 0.0416(17) 0.0217(11) 0.0425(14) 0.0049(10) 0.0059(13) 0.0059(12) C6 0.0272(11) 0.0189(9) 0.0311(10) 0.0002(10) 0.0059(10) 0.0004(9) C7 0.0267(12) 0.0262(11) 0.0281(10) 0.0082(9) 0.0040(10) 0.0033(10) C8 0.0363(16) 0.0466(17) 0.0290(12) 0.0102(12) -0.0017(11) 0.0074(14) C9 0.0273(13) 0.0335(13) 0.0227(10) 0.0051(9) 0.0012(9) -0.0021(10) C10 0.0297(14) 0.0431(17) 0.0246(11) -0.0009(11) 0.0038(10) -0.0033(12) C11 0.0463(19) 0.060(2) 0.0262(12) -0.0023(14) 0.0009(12) -0.0032(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Te 2.8847(2) . ? I2 Te 2.9431(2) . ? I3 Te 2.8435(2) . ? Te C1 2.153(2) . ? Te N 2.284(2) . ? Te I1 3.7092(2) 4_557 ? O C7 1.317(3) . ? O C8 1.453(4) . ? N C7 1.290(3) . ? N C9 1.479(3) . ? C1 C2 1.375(4) . ? C1 C6 1.404(4) . ? C2 C3 1.406(4) . ? C2 H2A 0.9500 . ? C3 C4 1.361(5) . ? C3 H3A 0.9500 . ? C4 C5 1.384(4) . ? C4 H4A 0.9500 . ? C5 C6 1.405(4) . ? C5 H5A 0.9500 . ? C6 C7 1.441(4) . ? C8 C9 1.563(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.520(4) . ? C9 H9A 1.0000 . ? C10 C11 1.537(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te N 75.56(9) . . ? C1 Te I3 94.05(7) . . ? N Te I3 169.50(6) . . ? C1 Te I1 88.97(7) . . ? N Te I1 85.23(6) . . ? I3 Te I1 93.200(7) . . ? C1 Te I2 86.65(7) . . ? N Te I2 86.30(6) . . ? I3 Te I2 94.713(8) . . ? I1 Te I2 171.208(8) . . ? C1 Te I1 169.99(7) . 4_557 ? N Te I1 106.52(5) . 4_557 ? I3 Te I1 83.980(6) . 4_557 ? I1 Te I1 100.918(5) . 4_557 ? I2 Te I1 83.742(6) . 4_557 ? C7 O C8 106.7(2) . . ? C7 N C9 109.6(2) . . ? C7 N Te 112.61(17) . . ? C9 N Te 137.36(17) . . ? C2 C1 C6 120.9(2) . . ? C2 C1 Te 124.57(19) . . ? C6 C1 Te 114.46(18) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C6 118.6(3) . . ? C4 C5 H5A 120.7 . . ? C6 C5 H5A 120.7 . . ? C1 C6 C5 119.8(2) . . ? C1 C6 C7 116.7(2) . . ? C5 C6 C7 123.5(2) . . ? N C7 O 117.4(2) . . ? N C7 C6 119.9(2) . . ? O C7 C6 122.7(2) . . ? O C8 C9 105.6(2) . . ? O C8 H8A 110.6 . . ? C9 C8 H8A 110.6 . . ? O C8 H8B 110.6 . . ? C9 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? N C9 C10 110.7(2) . . ? N C9 C8 100.6(2) . . ? C10 C9 C8 114.3(2) . . ? N C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? C8 C9 H9A 110.3 . . ? C9 C10 C11 112.1(3) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? 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 . . ? 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 C1 Te N C7 7.15(19) . . . . ? I3 Te N C7 15.5(5) . . . . ? I1 Te N C7 97.32(19) . . . . ? I2 Te N C7 -80.34(19) . . . . ? I1 Te N C7 -162.69(18) 4_557 . . . ? C1 Te N C9 179.1(3) . . . . ? I3 Te N C9 -172.5(2) . . . . ? I1 Te N C9 -90.7(2) . . . . ? I2 Te N C9 91.6(2) . . . . ? I1 Te N C9 9.2(3) 4_557 . . . ? N Te C1 C2 176.9(3) . . . . ? I3 Te C1 C2 -1.6(2) . . . . ? I1 Te C1 C2 91.5(2) . . . . ? I2 Te C1 C2 -96.1(2) . . . . ? I1 Te C1 C2 -79.9(5) 4_557 . . . ? N Te C1 C6 -6.79(18) . . . . ? I3 Te C1 C6 174.73(18) . . . . ? I1 Te C1 C6 -92.13(19) . . . . ? I2 Te C1 C6 80.24(18) . . . . ? I1 Te C1 C6 96.5(4) 4_557 . . . ? C6 C1 C2 C3 -0.8(4) . . . . ? Te C1 C2 C3 175.3(2) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C2 C1 C6 C5 2.6(4) . . . . ? Te C1 C6 C5 -173.9(2) . . . . ? C2 C1 C6 C7 -177.4(3) . . . . ? Te C1 C6 C7 6.1(3) . . . . ? C4 C5 C6 C1 -2.5(4) . . . . ? C4 C5 C6 C7 177.5(3) . . . . ? C9 N C7 O -0.3(4) . . . . ? Te N C7 O 173.9(2) . . . . ? C9 N C7 C6 179.3(2) . . . . ? Te N C7 C6 -6.4(3) . . . . ? C8 O C7 N -2.0(4) . . . . ? C8 O C7 C6 178.4(3) . . . . ? C1 C6 C7 N 0.6(4) . . . . ? C5 C6 C7 N -179.5(3) . . . . ? C1 C6 C7 O -179.8(3) . . . . ? C5 C6 C7 O 0.2(4) . . . . ? C7 O C8 C9 3.2(3) . . . . ? C7 N C9 C10 123.4(3) . . . . ? Te N C9 C10 -48.6(3) . . . . ? C7 N C9 C8 2.2(3) . . . . ? Te N C9 C8 -169.8(2) . . . . ? O C8 C9 N -3.2(3) . . . . ? O C8 C9 C10 -121.9(3) . . . . ? N C9 C10 C11 179.7(3) . . . . ? C8 C9 C10 C11 -67.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A I2 0.95 3.23 3.977(3) 137.0 4_467 C8 H8A I1 0.99 3.09 3.800(3) 129.7 2_664 C9 H9A I3 1.00 3.24 3.957(3) 130.4 4_457 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.118 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.122 # ==== data_8 _database_code_depnum_ccdc_archive 'CCDC 835168' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H11 Br N O Te' _chemical_formula_sum 'C11 H11 Br N O Te' _chemical_formula_weight 380.72 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 1 2/m 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.6722(3) _cell_length_b 6.9965(2) _cell_length_c 15.7268(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.463(3) _cell_angle_gamma 90.00 _cell_volume 1231.67(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5773 _cell_measurement_theta_min 4.5481 _cell_measurement_theta_max 34.7001 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 5.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53482 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 10225 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 34.85 _reflns_number_total 2722 _reflns_number_gt 2292 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+27.8155P] 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 2722 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1353 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te Te 0.42230(5) 0.0000 0.11875(4) 0.02564(13) Uani 1 2 d S . . Br Br 0.28066(9) 0.0000 -0.05175(7) 0.0514(3) Uani 1 2 d S . . O O 0.4660(6) 0.0000 0.3962(4) 0.0427(18) Uani 1 2 d S . . N N 0.4999(6) 0.0000 0.2639(5) 0.0370(19) Uani 1 2 d S . . C1 C 0.2722(7) 0.0000 0.1687(6) 0.0287(16) Uani 1 2 d S . . C2 C 0.1538(8) 0.0000 0.1184(6) 0.0337(18) Uani 1 2 d S . . H2A H 0.1343 0.0000 0.0555 0.040 Uiso 1 2 calc SR . . C3 C 0.0620(8) 0.0000 0.1608(8) 0.045(3) Uani 1 2 d S . . H3A H -0.0194 0.0000 0.1265 0.054 Uiso 1 2 calc SR . . C4 C 0.0912(9) 0.0000 0.2527(7) 0.041(2) Uani 1 2 d S . . H4A H 0.0295 0.0000 0.2811 0.050 Uiso 1 2 calc SR . . C5 C 0.2082(9) 0.0000 0.3027(7) 0.038(2) Uani 1 2 d S . . H5A H 0.2276 0.0000 0.3656 0.046 Uiso 1 2 calc SR . . C6 C 0.2987(7) 0.0000 0.2611(6) 0.0302(17) Uani 1 2 d S . . C7 C 0.4238(8) 0.0000 0.3084(6) 0.0335(18) Uani 1 2 d S . . C8 C 0.5964(8) 0.0000 0.4167(6) 0.044(3) Uani 1 2 d S . . H8A H 0.6283 -0.1237 0.4371 0.053 Uiso 0.50 1 d PR . . C9 C 0.6229(9) 0.0531(19) 0.3270(7) 0.033(3) Uani 0.50 1 d P . . H9A H 0.6433 0.1852 0.3234 0.040 Uiso 0.50 1 d PR . . C10 C 0.7159(11) -0.083(2) 0.3083(9) 0.038(3) Uani 0.50 1 d P . . H10A H 0.7162 -0.0773 0.2473 0.046 Uiso 0.50 1 d PR . . H10B H 0.7016 -0.2126 0.3230 0.046 Uiso 0.50 1 d PR . . C11 C 0.8388(10) 0.0000 0.3737(10) 0.088(7) Uani 1 2 d S . . H11A H 0.9048 -0.0757 0.3680 0.132 Uiso 0.50 1 d PR . . H11B H 0.8495 0.1301 0.3582 0.132 Uiso 0.50 1 d PR . . H11C H 0.8350 0.0000 0.4338 0.132 Uiso 1 2 d SR . . 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 Te 0.0241(2) 0.0289(2) 0.0263(2) 0.000 0.01088(17) 0.000 Br 0.0354(5) 0.0908(10) 0.0273(4) 0.000 0.0076(4) 0.000 O 0.036(3) 0.071(5) 0.026(3) 0.000 0.017(3) 0.000 N 0.020(3) 0.067(6) 0.024(3) 0.000 0.005(2) 0.000 C1 0.023(3) 0.036(4) 0.031(4) 0.000 0.013(3) 0.000 C2 0.028(4) 0.037(5) 0.039(5) 0.000 0.013(3) 0.000 C3 0.017(3) 0.059(7) 0.058(6) 0.000 0.010(4) 0.000 C4 0.035(4) 0.046(6) 0.054(6) 0.000 0.030(4) 0.000 C5 0.036(4) 0.047(6) 0.040(5) 0.000 0.024(4) 0.000 C6 0.026(4) 0.037(5) 0.031(4) 0.000 0.015(3) 0.000 C7 0.031(4) 0.043(5) 0.030(4) 0.000 0.014(3) 0.000 C8 0.030(4) 0.075(8) 0.029(4) 0.000 0.011(3) 0.000 C9 0.026(4) 0.048(9) 0.025(4) 0.001(4) 0.007(4) -0.003(4) C10 0.037(6) 0.046(7) 0.038(6) 0.006(6) 0.019(5) 0.005(6) C11 0.028(5) 0.17(2) 0.061(8) 0.000 0.014(5) 0.000 _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 Te C1 2.113(7) . ? Te N 2.204(7) . ? Te Br 2.7224(11) . ? O C7 1.328(11) . ? O C8 1.464(11) . ? N C7 1.278(11) . ? N C9 1.542(12) . ? N C9 1.542(12) 6 ? C1 C2 1.385(12) . ? C1 C6 1.397(12) . ? C2 C3 1.414(13) . ? C2 H2A 0.9500 . ? C3 C4 1.388(15) . ? C3 H3A 0.9500 . ? C4 C5 1.370(14) . ? C4 H4A 0.9500 . ? C5 C6 1.391(11) . ? C5 H5A 0.9500 . ? C6 C7 1.439(12) . ? C8 C9 1.572(14) 6 ? C8 C9 1.572(14) . ? C8 H8A 0.9600 . ? C9 C9 0.74(3) 6 ? C9 C10 1.221(15) 6 ? C9 C10 1.535(17) . ? C9 H9A 0.9600 . ? C10 C10 1.16(3) 6 ? C10 C9 1.221(15) 6 ? C10 C11 1.619(17) . ? C10 H10A 0.9601 . ? C10 H10B 0.9600 . ? C11 C10 1.619(17) 6 ? C11 H11A 0.9599 . ? C11 H11B 0.9601 . ? C11 H11C 0.9593 . ? 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 Te N 75.9(3) . . ? C1 Te Br 91.7(2) . . ? N Te Br 167.60(18) . . ? C7 O C8 106.6(6) . . ? C7 N C9 108.2(7) . . ? C7 N C9 108.2(7) . 6 ? C9 N C9 27.9(10) . 6 ? C7 N Te 115.0(6) . . ? C9 N Te 134.6(6) . . ? C9 N Te 134.6(6) 6 . ? C2 C1 C6 119.0(7) . . ? C2 C1 Te 125.8(6) . . ? C6 C1 Te 115.1(6) . . ? C1 C2 C3 119.8(9) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 119.7(9) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 119.7(9) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C1 121.1(8) . . ? C5 C6 C7 123.4(8) . . ? C1 C6 C7 115.5(7) . . ? N C7 O 117.4(8) . . ? N C7 C6 118.6(8) . . ? O C7 C6 124.1(7) . . ? O C8 C9 105.0(7) . 6 ? O C8 C9 105.0(7) . . ? C9 C8 C9 27.3(10) 6 . ? O C8 H8A 110.7 . . ? C9 C8 H8A 86.0 6 . ? C9 C8 H8A 110.9 . . ? C9 C9 C10 100.0(10) 6 6 ? C9 C9 C10 51.6(7) 6 . ? C10 C9 C10 48.4(13) 6 . ? C9 C9 N 76.1(5) 6 . ? C10 C9 N 128.0(11) 6 . ? C10 C9 N 107.8(9) . . ? C9 C9 C8 76.3(5) 6 . ? C10 C9 C8 132.2(11) 6 . ? C10 C9 C8 110.8(9) . . ? N C9 C8 97.9(7) . . ? C9 C9 H9A 164.3 6 . ? C10 C9 H9A 64.4 6 . ? C10 C9 H9A 112.7 . . ? N C9 H9A 113.3 . . ? C8 C9 H9A 113.3 . . ? C10 C10 C9 80.0(10) 6 6 ? C10 C10 C9 51.6(7) 6 . ? C9 C10 C9 28.5(11) 6 . ? C10 C10 C11 68.9(5) 6 . ? C9 C10 C11 118.2(12) 6 . ? C9 C10 C11 101.7(10) . . ? C10 C10 H10A 87.5 6 . ? C9 C10 H10A 119.2 6 . ? C9 C10 H10A 111.6 . . ? C11 C10 H10A 111.4 . . ? C10 C10 H10B 160.5 6 . ? C9 C10 H10B 83.0 6 . ? C9 C10 H10B 111.0 . . ? C11 C10 H10B 111.7 . . ? H10A C10 H10B 109.3 . . ? C10 C11 C10 42.2(11) 6 . ? C10 C11 H11A 136.8 6 . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 69.7 6 . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 110.3 6 . ? C10 C11 H11C 110.3 . . ? H11A C11 H11C 110.8 . . ? H11B C11 H11C 107.3 . . ? 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 C1 Te N C7 0.0 . . . . ? Br Te N C7 0.000(2) . . . . ? C1 Te N C9 -160.2(7) . . . . ? Br Te N C9 -160.2(7) . . . . ? C1 Te N C9 160.2(7) . . . 6 ? Br Te N C9 160.2(7) . . . 6 ? N Te C1 C2 180.0 . . . . ? Br Te C1 C2 0.0 . . . . ? N Te C1 C6 0.0 . . . . ? Br Te C1 C6 180.0 . . . . ? C6 C1 C2 C3 0.0 . . . . ? Te C1 C2 C3 180.0 . . . . ? C1 C2 C3 C4 0.000(1) . . . . ? C2 C3 C4 C5 0.000(1) . . . . ? C3 C4 C5 C6 0.000(2) . . . . ? C4 C5 C6 C1 0.000(2) . . . . ? C4 C5 C6 C7 180.000(2) . . . . ? C2 C1 C6 C5 0.000(2) . . . . ? Te C1 C6 C5 180.000(1) . . . . ? C2 C1 C6 C7 180.000(1) . . . . ? Te C1 C6 C7 0.0 . . . . ? C9 N C7 O -14.7(5) . . . . ? C9 N C7 O 14.7(5) 6 . . . ? Te N C7 O 180.000(1) . . . . ? C9 N C7 C6 165.3(5) . . . . ? C9 N C7 C6 -165.3(5) 6 . . . ? Te N C7 C6 0.000(1) . . . . ? C8 O C7 N 0.000(1) . . . . ? C8 O C7 C6 180.000(2) . . . . ? C5 C6 C7 N 180.000(1) . . . . ? C1 C6 C7 N 0.000(1) . . . . ? C5 C6 C7 O 0.000(1) . . . . ? C1 C6 C7 O 180.000(1) . . . . ? C7 O C8 C9 -14.2(5) . . . 6 ? C7 O C8 C9 14.2(5) . . . . ? C7 N C9 C9 94.7(3) . . . 6 ? Te N C9 C9 -104.1(6) . . . 6 ? C7 N C9 C10 -173.5(14) . . . 6 ? C9 N C9 C10 91.8(15) 6 . . 6 ? Te N C9 C10 -12.3(19) . . . 6 ? C7 N C9 C10 135.9(7) . . . . ? C9 N C9 C10 41.2(9) 6 . . . ? Te N C9 C10 -63.0(11) . . . . ? C7 N C9 C8 20.9(7) . . . . ? C9 N C9 C8 -73.7(6) 6 . . . ? Te N C9 C8 -177.9(2) . . . . ? O C8 C9 C9 -93.7(2) . . . 6 ? O C8 C9 C10 175.1(15) . . . 6 ? C9 C8 C9 C10 -91.1(16) 6 . . 6 ? O C8 C9 C10 -132.8(8) . . . . ? C9 C8 C9 C10 -39.1(9) 6 . . . ? O C8 C9 N -20.2(7) . . . . ? C9 C8 C9 N 73.5(6) 6 . . . ? C9 C9 C10 C10 180.000(3) 6 . . 6 ? N C9 C10 C10 125.3(10) . . . 6 ? C8 C9 C10 C10 -128.6(11) . . . 6 ? C10 C9 C10 C9 180.000(4) 6 . . 6 ? N C9 C10 C9 -54.7(10) . . . 6 ? C8 C9 C10 C9 51.4(11) . . . 6 ? C9 C9 C10 C11 -129.2(10) 6 . . . ? C10 C9 C10 C11 50.8(10) 6 . . . ? N C9 C10 C11 176.1(8) . . . . ? C8 C9 C10 C11 -77.8(11) . . . . ? C9 C10 C11 C10 -65.4(14) 6 . . 6 ? C9 C10 C11 C10 -40.6(9) . . . 6 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.143 _refine_diff_density_min -2.177 _refine_diff_density_rms 0.230 # ==== data_9 _database_code_depnum_ccdc_archive 'CCDC 835169' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 Br4 O5 Te2' _chemical_formula_sum 'C16 H14 Br4 O5 Te2' _chemical_formula_weight 861.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 14.8602(11) _cell_length_b 17.5288(8) _cell_length_c 8.9476(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.740(7) _cell_angle_gamma 90.00 _cell_volume 2273.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.6437 _cell_measurement_theta_max 32.6062 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4871 _exptl_crystal_size_mid 0.4097 _exptl_crystal_size_min 0.0279 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 9.620 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.061 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15286 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1474 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.65 _diffrn_reflns_theta_max 32.69 _reflns_number_total 7284 _reflns_number_gt 4268 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+69.1150P] 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 7284 _refine_ls_number_parameters 246 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1641 _refine_ls_R_factor_gt 0.0977 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.33660(6) -0.04788(4) 1.42775(8) 0.01248(18) Uani 1 1 d . . . Te2 Te 0.18229(6) 0.04948(4) 1.60131(8) 0.01195(18) Uani 1 1 d . . . Br11 Br 0.43197(10) 0.05006(7) 1.30448(15) 0.0202(3) Uani 1 1 d . . . Br12 Br 0.21986(11) -0.14615(7) 1.52198(15) 0.0205(3) Uani 1 1 d . . . Br21 Br 0.03583(10) 0.07443(7) 1.37494(14) 0.0157(3) Uani 1 1 d . . . Br22 Br 0.34186(10) 0.03828(7) 1.80687(15) 0.0205(3) Uani 1 1 d . . . O O 0.2486(6) 0.0344(4) 1.4381(9) 0.0125(18) Uani 1 1 d . . . O1A O 0.4196(7) -0.2129(5) 1.1066(11) 0.022(2) Uani 1 1 d . . . O2A O 0.4225(7) -0.1527(5) 1.3303(10) 0.019(2) Uani 1 1 d . . . O1B O 0.0309(7) 0.2329(5) 1.7803(11) 0.020(2) Uani 1 1 d . . . O2B O 0.0842(7) 0.1141(5) 1.7597(11) 0.021(2) Uani 1 1 d . . . C1A C 0.2629(9) -0.0719(6) 1.2009(14) 0.013(2) Uani 1 1 d U . . C2A C 0.1813(10) -0.0329(7) 1.1350(15) 0.019(3) Uani 1 1 d . . . H2AA H 0.1568 0.0050 1.1906 0.023 Uiso 1 1 calc R . . C3A C 0.1374(10) -0.0516(7) 0.9858(15) 0.020(3) Uani 1 1 d . . . H3AA H 0.0828 -0.0250 0.9386 0.024 Uiso 1 1 calc R . . C4A C 0.1708(10) -0.1075(7) 0.9045(14) 0.019(3) Uani 1 1 d U . . H4AA H 0.1374 -0.1206 0.8046 0.022 Uiso 1 1 calc R . . C5A C 0.2527(11) -0.1448(8) 0.9672(15) 0.023(3) Uani 1 1 d . . . H5AA H 0.2772 -0.1815 0.9089 0.027 Uiso 1 1 calc R . . C6A C 0.2987(9) -0.1278(7) 1.1164(14) 0.012(2) Uani 1 1 d U . . C7A C 0.3854(10) -0.1645(7) 1.1952(15) 0.018(3) Uani 1 1 d . . . C1B C 0.2089(9) 0.1683(6) 1.5944(13) 0.013(2) Uani 1 1 d U . . C2B C 0.2765(9) 0.1958(7) 1.5236(14) 0.014(2) Uani 1 1 d U . . H2BA H 0.3123 0.1617 1.4779 0.016 Uiso 1 1 calc R . . C3B C 0.2913(10) 0.2756(7) 1.5208(14) 0.017(3) Uani 1 1 d U . . H3BA H 0.3387 0.2952 1.4758 0.021 Uiso 1 1 calc R . . C4B C 0.2367(9) 0.3255(7) 1.5835(14) 0.015(3) Uani 1 1 d . . . H4BA H 0.2452 0.3790 1.5777 0.018 Uiso 1 1 calc R . . C5B C 0.1707(9) 0.2973(7) 1.6535(15) 0.015(3) Uani 1 1 d . . . H5BA H 0.1345 0.3315 1.6982 0.018 Uiso 1 1 calc R . . C6B C 0.1559(9) 0.2186(6) 1.6601(13) 0.012(3) Uani 1 1 d . . . C7B C 0.0873(9) 0.1839(7) 1.7362(14) 0.013(2) Uani 1 1 d . . . C8B C -0.0372(11) 0.2025(9) 1.8579(18) 0.026(3) Uani 1 1 d . . . H8BA H -0.0709 0.2447 1.8923 0.039 Uiso 1 1 calc R . . H8BB H -0.0062 0.1724 1.9466 0.039 Uiso 1 1 calc R . . H8BC H -0.0805 0.1699 1.7872 0.039 Uiso 1 1 calc R . . C8A C 0.5028(11) -0.2521(8) 1.1801(17) 0.026(3) Uani 1 1 d . . . H8AA H 0.5227 -0.2856 1.1058 0.039 Uiso 1 1 calc R . . H8AB H 0.4911 -0.2826 1.2655 0.039 Uiso 1 1 calc R . . H8AC H 0.5514 -0.2147 1.2188 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0216(4) 0.0083(3) 0.0085(3) -0.0010(3) 0.0055(3) 0.0011(3) Te2 0.0212(4) 0.0067(3) 0.0093(3) -0.0012(3) 0.0065(3) -0.0007(3) Br11 0.0219(7) 0.0164(6) 0.0233(7) 0.0029(5) 0.0075(5) -0.0028(6) Br12 0.0362(9) 0.0116(6) 0.0173(6) 0.0003(5) 0.0137(6) -0.0034(6) Br21 0.0195(7) 0.0130(5) 0.0153(6) 0.0012(5) 0.0051(5) -0.0009(5) Br22 0.0276(8) 0.0161(6) 0.0162(6) -0.0001(5) 0.0015(5) 0.0029(5) O 0.026(5) 0.007(4) 0.006(4) 0.000(3) 0.007(3) 0.001(3) O1A 0.023(5) 0.020(5) 0.025(5) -0.006(4) 0.009(4) 0.013(4) O2A 0.033(6) 0.013(4) 0.011(4) -0.002(3) 0.003(4) 0.012(4) O1B 0.029(6) 0.013(4) 0.024(5) -0.001(4) 0.017(4) 0.004(4) O2B 0.030(6) 0.018(5) 0.021(5) 0.001(4) 0.020(4) 0.007(4) C1A 0.021(6) 0.004(4) 0.011(5) 0.002(4) 0.000(4) -0.005(4) C2A 0.030(8) 0.016(6) 0.013(6) 0.004(5) 0.008(6) -0.010(6) C3A 0.024(7) 0.017(6) 0.023(7) 0.011(5) 0.015(6) 0.004(6) C4A 0.025(6) 0.022(6) 0.009(5) -0.006(4) 0.003(5) -0.003(5) C5A 0.041(10) 0.016(6) 0.017(7) 0.003(5) 0.018(6) 0.002(6) C6A 0.015(4) 0.011(4) 0.012(4) -0.003(3) 0.005(3) 0.002(3) C7A 0.031(8) 0.010(6) 0.017(6) -0.001(5) 0.012(6) -0.002(5) C1B 0.025(6) 0.006(4) 0.006(5) 0.003(4) -0.002(4) -0.001(4) C2B 0.020(6) 0.006(4) 0.015(5) -0.001(4) 0.006(4) 0.004(4) C3B 0.025(6) 0.019(5) 0.009(5) 0.006(4) 0.007(5) 0.000(5) C4B 0.015(7) 0.009(5) 0.016(6) 0.000(5) -0.005(5) -0.001(5) C5B 0.011(6) 0.014(6) 0.020(7) -0.006(5) 0.004(5) -0.002(5) C6B 0.023(7) 0.007(5) 0.006(5) 0.001(4) 0.002(5) -0.007(5) C7B 0.011(6) 0.016(6) 0.013(6) 0.004(5) 0.003(5) 0.001(5) C8B 0.030(9) 0.026(7) 0.030(8) -0.006(6) 0.022(7) -0.008(7) C8A 0.020(8) 0.022(7) 0.033(8) -0.010(6) 0.002(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 Te1 O 1.963(8) . ? Te1 C1A 2.125(12) . ? Te1 O2A 2.501(9) . ? Te1 Br11 2.6195(16) . ? Te1 Br12 2.7080(16) . ? Te2 O 1.951(8) . ? Te2 C1B 2.123(11) . ? Te2 O2B 2.516(9) . ? Te2 Br21 2.6621(16) . ? Te2 Br22 2.6685(16) . ? O1A C7A 1.335(15) . ? O1A C8A 1.441(17) . ? O2A C7A 1.230(15) . ? O1B C7B 1.320(15) . ? O1B C8B 1.449(17) . ? O2B C7B 1.243(15) . ? C1A C2A 1.404(19) . ? C1A C6A 1.412(17) . ? C2A C3A 1.389(19) . ? C2A H2AA 0.9500 . ? C3A C4A 1.376(18) . ? C3A H3AA 0.9500 . ? C4A C5A 1.39(2) . ? C4A H4AA 0.9500 . ? C5A C6A 1.391(18) . ? C5A H5AA 0.9500 . ? C6A C7A 1.474(19) . ? C1B C2B 1.387(19) . ? C1B C6B 1.396(18) . ? C2B C3B 1.418(17) . ? C2B H2BA 0.9500 . ? C3B C4B 1.392(19) . ? C3B H3BA 0.9500 . ? C4B C5B 1.367(19) . ? C4B H4BA 0.9500 . ? C5B C6B 1.400(16) . ? C5B H5BA 0.9500 . ? C6B C7B 1.476(18) . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Te1 C1A 89.0(4) . . ? O Te1 O2A 162.3(3) . . ? C1A Te1 O2A 73.5(4) . . ? O Te1 Br11 88.1(2) . . ? C1A Te1 Br11 86.6(3) . . ? O2A Te1 Br11 88.3(2) . . ? O Te1 Br12 88.5(3) . . ? C1A Te1 Br12 86.6(3) . . ? O2A Te1 Br12 93.0(2) . . ? Br11 Te1 Br12 172.41(5) . . ? O Te2 C1B 89.0(4) . . ? O Te2 O2B 159.0(3) . . ? C1B Te2 O2B 73.1(4) . . ? O Te2 Br21 85.2(3) . . ? C1B Te2 Br21 86.7(3) . . ? O2B Te2 Br21 82.9(2) . . ? O Te2 Br22 89.3(3) . . ? C1B Te2 Br22 87.1(3) . . ? O2B Te2 Br22 100.5(2) . . ? Br21 Te2 Br22 171.76(5) . . ? Te2 O Te1 125.9(4) . . ? C7A O1A C8A 115.6(11) . . ? C7A O2A Te1 108.3(8) . . ? C7B O1B C8B 117.4(10) . . ? C7B O2B Te2 107.5(8) . . ? C2A C1A C6A 120.3(11) . . ? C2A C1A Te1 121.4(9) . . ? C6A C1A Te1 118.3(9) . . ? C3A C2A C1A 117.9(13) . . ? C3A C2A H2AA 121.0 . . ? C1A C2A H2AA 121.0 . . ? C4A C3A C2A 121.9(13) . . ? C4A C3A H3AA 119.1 . . ? C2A C3A H3AA 119.1 . . ? C3A C4A C5A 120.5(12) . . ? C3A C4A H4AA 119.7 . . ? C5A C4A H4AA 119.7 . . ? C4A C5A C6A 119.3(12) . . ? C4A C5A H5AA 120.3 . . ? C6A C5A H5AA 120.3 . . ? C5A C6A C1A 119.9(12) . . ? C5A C6A C7A 124.0(11) . . ? C1A C6A C7A 116.1(11) . . ? O2A C7A O1A 123.0(13) . . ? O2A C7A C6A 123.5(12) . . ? O1A C7A C6A 113.6(11) . . ? C2B C1B C6B 120.4(10) . . ? C2B C1B Te2 120.8(9) . . ? C6B C1B Te2 118.8(9) . . ? C1B C2B C3B 118.8(12) . . ? C1B C2B H2BA 120.6 . . ? C3B C2B H2BA 120.6 . . ? C4B C3B C2B 120.4(13) . . ? C4B C3B H3BA 119.8 . . ? C2B C3B H3BA 119.8 . . ? C5B C4B C3B 119.9(12) . . ? C5B C4B H4BA 120.1 . . ? C3B C4B H4BA 120.1 . . ? C4B C5B C6B 120.7(12) . . ? C4B C5B H5BA 119.6 . . ? C6B C5B H5BA 119.6 . . ? C1B C6B C5B 119.7(12) . . ? C1B C6B C7B 116.4(10) . . ? C5B C6B C7B 123.8(12) . . ? O2B C7B O1B 122.7(12) . . ? O2B C7B C6B 122.6(12) . . ? O1B C7B C6B 114.7(11) . . ? O1B C8B H8BA 109.5 . . ? O1B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? O1B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? O1A C8A H8AA 109.5 . . ? O1A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? O1A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1B Te2 O Te1 137.7(6) . . . . ? O2B Te2 O Te1 169.0(7) . . . . ? Br21 Te2 O Te1 -135.5(5) . . . . ? Br22 Te2 O Te1 50.6(5) . . . . ? C1A Te1 O Te2 129.3(6) . . . . ? O2A Te1 O Te2 137.8(9) . . . . ? Br11 Te1 O Te2 -144.1(5) . . . . ? Br12 Te1 O Te2 42.7(5) . . . . ? O Te1 O2A C7A -4.1(17) . . . . ? C1A Te1 O2A C7A 4.7(9) . . . . ? Br11 Te1 O2A C7A -82.2(9) . . . . ? Br12 Te1 O2A C7A 90.3(9) . . . . ? O Te2 O2B C7B -22.0(15) . . . . ? C1B Te2 O2B C7B 10.8(9) . . . . ? Br21 Te2 O2B C7B -77.9(8) . . . . ? Br22 Te2 O2B C7B 94.5(8) . . . . ? O Te1 C1A C2A -4.1(10) . . . . ? O2A Te1 C1A C2A 178.6(11) . . . . ? Br11 Te1 C1A C2A -92.2(10) . . . . ? Br12 Te1 C1A C2A 84.5(10) . . . . ? O Te1 C1A C6A 175.2(10) . . . . ? O2A Te1 C1A C6A -2.1(9) . . . . ? Br11 Te1 C1A C6A 87.1(9) . . . . ? Br12 Te1 C1A C6A -96.3(9) . . . . ? C6A C1A C2A C3A 0.4(18) . . . . ? Te1 C1A C2A C3A 179.7(9) . . . . ? C1A C2A C3A C4A 1.4(19) . . . . ? C2A C3A C4A C5A -3(2) . . . . ? C3A C4A C5A C6A 3(2) . . . . ? C4A C5A C6A C1A -1(2) . . . . ? C4A C5A C6A C7A 179.2(13) . . . . ? C2A C1A C6A C5A -0.3(19) . . . . ? Te1 C1A C6A C5A -179.6(10) . . . . ? C2A C1A C6A C7A 179.1(11) . . . . ? Te1 C1A C6A C7A -0.2(15) . . . . ? Te1 O2A C7A O1A 174.3(10) . . . . ? Te1 O2A C7A C6A -6.7(15) . . . . ? C8A O1A C7A O2A 1.0(19) . . . . ? C8A O1A C7A C6A -178.0(12) . . . . ? C5A C6A C7A O2A -175.2(13) . . . . ? C1A C6A C7A O2A 5.5(19) . . . . ? C5A C6A C7A O1A 3.9(19) . . . . ? C1A C6A C7A O1A -175.5(11) . . . . ? O Te2 C1B C2B -16.8(10) . . . . ? O2B Te2 C1B C2B 174.4(11) . . . . ? Br21 Te2 C1B C2B -102.0(10) . . . . ? Br22 Te2 C1B C2B 72.5(10) . . . . ? O Te2 C1B C6B 162.1(10) . . . . ? O2B Te2 C1B C6B -6.7(9) . . . . ? Br21 Te2 C1B C6B 76.9(9) . . . . ? Br22 Te2 C1B C6B -108.6(9) . . . . ? C6B C1B C2B C3B 0.6(18) . . . . ? Te2 C1B C2B C3B 179.5(9) . . . . ? C1B C2B C3B C4B -2.1(19) . . . . ? C2B C3B C4B C5B 2.5(19) . . . . ? C3B C4B C5B C6B -1.4(19) . . . . ? C2B C1B C6B C5B 0.5(18) . . . . ? Te2 C1B C6B C5B -178.4(9) . . . . ? C2B C1B C6B C7B -178.5(11) . . . . ? Te2 C1B C6B C7B 2.6(14) . . . . ? C4B C5B C6B C1B -0.1(19) . . . . ? C4B C5B C6B C7B 178.8(12) . . . . ? Te2 O2B C7B O1B 167.7(10) . . . . ? Te2 O2B C7B C6B -13.8(14) . . . . ? C8B O1B C7B O2B -0.5(19) . . . . ? C8B O1B C7B C6B -179.1(11) . . . . ? C1B C6B C7B O2B 9.4(18) . . . . ? C5B C6B C7B O2B -169.5(12) . . . . ? C1B C6B C7B O1B -172.0(11) . . . . ? C5B C6B C7B O1B 9.1(18) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 4.837 _refine_diff_density_min -2.385 _refine_diff_density_rms 0.400 # ==== data_12a _database_code_depnum_ccdc_archive 'CCDC 835171' #TrackingRef '- Comb CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 0.79(C9 H12 Br3 N Te), 0.21(C9 H12 Cl3 N Te) ; _chemical_formula_sum 'C9 H12 Br2.37 Cl0.63 N Te' _chemical_formula_weight 473.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 14.7827(8) _cell_length_b 12.0157(5) _cell_length_c 15.8651(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.130(5) _cell_angle_gamma 90.00 _cell_volume 2662.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5674 _cell_measurement_theta_min 4.8518 _cell_measurement_theta_max 73.7704 _exptl_crystal_description 'thick needle' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.8151 _exptl_crystal_size_mid 0.3205 _exptl_crystal_size_min 0.1647 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1749 _exptl_absorpt_coefficient_mu 26.859 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.007 _exptl_absorpt_correction_T_max 0.120 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9770 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.85 _diffrn_reflns_theta_max 73.87 _reflns_number_total 5118 _reflns_number_gt 3902 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.1966P)^2^+6.3038P] 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 5118 _refine_ls_number_parameters 281 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.2705 _refine_ls_wR_factor_gt 0.2428 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Te1 Te 0.81699(5) 0.51634(6) 0.24658(4) 0.0368(3) Uani 1 1 d D . . Te2 Te 0.68502(5) 0.21391(6) 0.25890(4) 0.0368(3) Uani 1 1 d D . . Br1A Br 0.9647(3) 0.5991(5) 0.37579(17) 0.0605(9) Uani 0.748(11) 1 d PD A 1 Br2A Br 0.7036(3) 0.5830(6) 0.3311(3) 0.0565(10) Uani 0.748(11) 1 d PD A 1 Br3A Br 0.65428(19) 0.4488(2) 0.11729(15) 0.0445(7) Uani 0.748(11) 1 d PD A 1 Br1B Br 0.84847(16) 0.27342(18) 0.39025(15) 0.0507(6) Uani 0.832(11) 1 d PD A 1 Br2B Br 0.5298(2) 0.1408(3) 0.13069(19) 0.0550(7) Uani 0.832(11) 1 d PD A 1 Br3B Br 0.7918(3) 0.1446(3) 0.1654(2) 0.0541(7) Uani 0.832(11) 1 d PD A 1 Cl1A Cl 0.965(2) 0.592(4) 0.3575(18) 0.0605(9) Uani 0.252(11) 1 d PD A 2 Cl2A Cl 0.724(3) 0.580(5) 0.342(2) 0.0565(10) Uani 0.252(11) 1 d PD A 2 Cl3A Cl 0.6599(16) 0.453(2) 0.1408(12) 0.0445(7) Uani 0.252(11) 1 d PD A 2 Cl1B Cl 0.831(2) 0.268(3) 0.3633(19) 0.0507(6) Uani 0.168(11) 1 d PD A 2 Cl2B Cl 0.549(3) 0.156(4) 0.143(3) 0.0550(7) Uani 0.168(11) 1 d PD A 2 Cl3B Cl 0.780(4) 0.162(5) 0.173(4) 0.0541(7) Uani 0.168(11) 1 d PD A 2 N1A N 0.9215(8) 0.4801(9) 0.1601(7) 0.046(2) Uani 1 1 d . A . N1B N 0.5865(8) 0.2449(9) 0.3498(6) 0.043(2) Uani 1 1 d . A . C1A C 0.8089(9) 0.6659(10) 0.1734(7) 0.038(2) Uani 1 1 d . A . C2A C 0.7361(13) 0.7414(12) 0.1619(9) 0.054(3) Uani 1 1 d . . . H2AA H 0.6859 0.7281 0.1837 0.065 Uiso 1 1 calc R A . C3A C 0.7410(11) 0.8413(12) 0.1149(9) 0.053(3) Uani 1 1 d . A . H3AA H 0.6965 0.8975 0.1108 0.063 Uiso 1 1 calc R . . C4A C 0.8093(12) 0.8554(11) 0.0760(8) 0.055(4) Uani 1 1 d . . . H4AA H 0.8093 0.9198 0.0436 0.066 Uiso 1 1 calc R A . C5A C 0.8781(10) 0.7767(10) 0.0837(8) 0.043(3) Uani 1 1 d . A . H5AA H 0.9246 0.7881 0.0569 0.051 Uiso 1 1 calc R . . C6A C 0.8790(10) 0.6759(10) 0.1332(8) 0.042(3) Uani 1 1 d . . . C7A C 0.9567(11) 0.5902(10) 0.1489(9) 0.047(3) Uani 1 1 d . A . H7AA H 0.9804 0.5895 0.0986 0.056 Uiso 1 1 calc R . . H7AB H 1.0096 0.6097 0.2019 0.056 Uiso 1 1 calc R . . C8A C 0.8697(11) 0.4311(13) 0.0721(7) 0.050(3) Uani 1 1 d . . . H8AA H 0.9148 0.4079 0.0438 0.074 Uiso 1 1 calc R A . H8AB H 0.8271 0.4856 0.0356 0.074 Uiso 1 1 calc R . . H8AC H 0.8334 0.3679 0.0799 0.074 Uiso 1 1 calc R . . C9A C 0.9984(12) 0.4058(14) 0.2102(10) 0.060(4) Uani 1 1 d . . . H9AA H 1.0475 0.4482 0.2527 0.090 Uiso 1 1 calc R A . H9AB H 1.0248 0.3690 0.1699 0.090 Uiso 1 1 calc R . . H9AC H 0.9733 0.3513 0.2409 0.090 Uiso 1 1 calc R . . C1B C 0.6898(9) 0.0597(9) 0.3241(6) 0.034(2) Uani 1 1 d . A . C2B C 0.7570(10) -0.0196(11) 0.3300(8) 0.046(3) Uani 1 1 d . . . H2BA H 0.8049 -0.0069 0.3050 0.055 Uiso 1 1 calc R A . C3B C 0.7546(12) -0.1203(11) 0.3732(9) 0.055(3) Uani 1 1 d . A . H3BA H 0.7995 -0.1755 0.3755 0.066 Uiso 1 1 calc R . . C4B C 0.6854(10) -0.1371(9) 0.4126(8) 0.046(3) Uani 1 1 d . . . H4BA H 0.6847 -0.2035 0.4425 0.056 Uiso 1 1 calc R A . C5B C 0.6165(9) -0.0570(10) 0.4083(6) 0.037(2) Uani 1 1 d . A . H5BA H 0.5693 -0.0696 0.4341 0.045 Uiso 1 1 calc R . . C6B C 0.6197(9) 0.0446(9) 0.3640(6) 0.038(2) Uani 1 1 d . . . C7B C 0.5447(10) 0.1357(10) 0.3559(8) 0.043(3) Uani 1 1 d . A . H7BA H 0.4896 0.1229 0.3032 0.052 Uiso 1 1 calc R . . H7BB H 0.5234 0.1338 0.4076 0.052 Uiso 1 1 calc R . . C8B C 0.6418(12) 0.2851(13) 0.4395(8) 0.056(4) Uani 1 1 d . . . H8BA H 0.6024 0.2829 0.4771 0.084 Uiso 1 1 calc R A . H8BB H 0.6623 0.3601 0.4356 0.084 Uiso 1 1 calc R . . H8BC H 0.6968 0.2383 0.4644 0.084 Uiso 1 1 calc R . . C9B C 0.5098(12) 0.3249(14) 0.3055(11) 0.061(4) Uani 1 1 d . . . H9BA H 0.4831 0.3546 0.3484 0.091 Uiso 1 1 calc R A . H9BB H 0.4606 0.2877 0.2590 0.091 Uiso 1 1 calc R . . H9BC H 0.5358 0.3844 0.2802 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te1 0.0499(5) 0.0362(4) 0.0176(4) 0.0043(2) 0.0016(3) -0.0014(3) Te2 0.0468(5) 0.0371(4) 0.0211(4) 0.0099(2) 0.0038(3) 0.0013(3) Br1A 0.0687(12) 0.0783(15) 0.0200(15) -0.0034(15) -0.0053(11) -0.0129(10) Br2A 0.075(3) 0.0594(11) 0.0338(16) -0.0028(14) 0.0151(18) 0.003(2) Br3A 0.0611(11) 0.0466(8) 0.0155(12) -0.0004(10) -0.0016(10) -0.0044(7) Br1B 0.0546(12) 0.0504(9) 0.0326(12) 0.0068(9) -0.0057(9) -0.0053(8) Br2B 0.0570(16) 0.0720(16) 0.0251(12) 0.0055(9) -0.0014(9) -0.0116(11) Br3B 0.0700(17) 0.0569(18) 0.0374(11) 0.0083(11) 0.0202(8) 0.0087(11) Cl1A 0.0687(12) 0.0783(15) 0.0200(15) -0.0034(15) -0.0053(11) -0.0129(10) Cl2A 0.075(3) 0.0594(11) 0.0338(16) -0.0028(14) 0.0151(18) 0.003(2) Cl3A 0.0611(11) 0.0466(8) 0.0155(12) -0.0004(10) -0.0016(10) -0.0044(7) Cl1B 0.0546(12) 0.0504(9) 0.0326(12) 0.0068(9) -0.0057(9) -0.0053(8) Cl2B 0.0570(16) 0.0720(16) 0.0251(12) 0.0055(9) -0.0014(9) -0.0116(11) Cl3B 0.0700(17) 0.0569(18) 0.0374(11) 0.0083(11) 0.0202(8) 0.0087(11) N1A 0.050(6) 0.049(6) 0.027(5) 0.005(4) -0.006(4) -0.013(5) N1B 0.052(6) 0.048(5) 0.016(4) 0.001(4) -0.004(4) -0.006(5) C1A 0.053(6) 0.040(5) 0.013(4) -0.001(4) -0.002(4) -0.003(5) C2A 0.082(10) 0.042(6) 0.036(6) 0.008(5) 0.015(7) 0.011(7) C3A 0.067(8) 0.043(6) 0.037(6) 0.007(5) 0.002(6) 0.006(6) C4A 0.090(10) 0.039(6) 0.021(5) 0.013(4) -0.004(6) -0.011(6) C5A 0.055(7) 0.041(6) 0.027(5) 0.008(4) 0.005(5) -0.009(5) C6A 0.053(7) 0.037(6) 0.031(5) -0.001(5) 0.008(5) -0.008(5) C7A 0.062(8) 0.031(5) 0.037(6) 0.000(5) 0.003(6) 0.000(5) C8A 0.070(9) 0.061(8) 0.018(5) -0.005(5) 0.013(5) 0.000(7) C9A 0.060(8) 0.058(8) 0.048(8) 0.010(6) 0.000(7) 0.023(7) C1B 0.046(6) 0.038(5) 0.009(4) 0.002(3) -0.005(4) -0.003(5) C2B 0.057(7) 0.045(6) 0.034(6) 0.009(5) 0.012(5) 0.015(6) C3B 0.078(10) 0.036(6) 0.039(6) 0.002(5) 0.001(6) 0.006(6) C4B 0.067(8) 0.029(5) 0.027(5) 0.008(4) -0.006(5) -0.009(5) C5B 0.050(6) 0.040(5) 0.014(4) 0.004(4) 0.000(4) -0.009(5) C6B 0.058(7) 0.032(5) 0.017(4) 0.005(4) 0.003(4) -0.007(5) C7B 0.058(7) 0.042(6) 0.032(5) 0.007(5) 0.018(5) 0.011(5) C8B 0.077(10) 0.060(8) 0.023(6) -0.009(5) 0.005(6) -0.009(7) C9B 0.067(9) 0.056(8) 0.050(8) 0.017(7) 0.008(7) 0.020(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 Te1 C1A 2.121(12) . ? Te1 N1A 2.418(12) . ? Te1 Cl2A 2.48(2) . ? Te1 Cl1A 2.49(2) . ? Te1 Cl3A 2.499(19) . ? Te1 Br2A 2.592(3) . ? Te1 Br1A 2.651(3) . ? Te1 Br3A 2.723(3) . ? Te1 Cl1B 3.48(3) . ? Te1 Br1B 3.638(2) . ? Te2 C1B 2.112(10) . ? Te2 Cl3B 2.34(2) . ? Te2 Cl1B 2.34(2) . ? Te2 Cl2B 2.34(2) . ? Te2 N1B 2.391(11) . ? Te2 Br3B 2.630(2) . ? Te2 Br2B 2.668(2) . ? Te2 Br1B 2.719(2) . ? Te2 Cl3A 3.38(2) . ? Te2 Br3A 3.543(3) . ? N1A C7A 1.453(16) . ? N1A C9A 1.459(17) . ? N1A C8A 1.476(15) . ? N1B C7B 1.467(16) . ? N1B C8B 1.471(14) . ? N1B C9B 1.477(17) . ? C1A C2A 1.37(2) . ? C1A C6A 1.390(19) . ? C2A C3A 1.427(19) . ? C2A H2AA 0.9300 . ? C3A C4A 1.36(2) . ? C3A H3AA 0.9300 . ? C4A C5A 1.37(2) . ? C4A H4AA 0.9300 . ? C5A C6A 1.441(16) . ? C5A H5AA 0.9300 . ? C6A C7A 1.502(19) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C8A H8AA 0.9600 . ? C8A H8AB 0.9600 . ? C8A H8AC 0.9600 . ? C9A H9AA 0.9600 . ? C9A H9AB 0.9600 . ? C9A H9AC 0.9600 . ? C1B C2B 1.357(17) . ? C1B C6B 1.392(17) . ? C2B C3B 1.397(18) . ? C2B H2BA 0.9300 . ? C3B C4B 1.38(2) . ? C3B H3BA 0.9300 . ? C4B C5B 1.386(19) . ? C4B H4BA 0.9300 . ? C5B C6B 1.417(14) . ? C5B H5BA 0.9300 . ? C6B C7B 1.534(17) . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C9B H9BA 0.9600 . ? C9B H9BB 0.9600 . ? C9B H9BC 0.9600 . ? 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 C1A Te1 N1A 77.0(4) . . ? C1A Te1 Cl2A 97.4(14) . . ? N1A Te1 Cl2A 171.2(14) . . ? C1A Te1 Cl1A 87.5(11) . . ? N1A Te1 Cl1A 83.6(9) . . ? Cl2A Te1 Cl1A 89.5(14) . . ? C1A Te1 Cl3A 91.1(6) . . ? N1A Te1 Cl3A 100.9(6) . . ? Cl2A Te1 Cl3A 85.8(12) . . ? Cl1A Te1 Cl3A 174.8(12) . . ? C1A Te1 Br2A 95.2(4) . . ? N1A Te1 Br2A 172.1(3) . . ? Cl2A Te1 Br2A 6.2(10) . . ? Cl1A Te1 Br2A 95.2(9) . . ? Cl3A Te1 Br2A 80.0(6) . . ? C1A Te1 Br1A 89.4(3) . . ? N1A Te1 Br1A 89.4(3) . . ? Cl2A Te1 Br1A 83.8(11) . . ? Cl1A Te1 Br1A 5.8(9) . . ? Cl3A Te1 Br1A 169.5(6) . . ? Br2A Te1 Br1A 89.59(13) . . ? C1A Te1 Br3A 87.9(3) . . ? N1A Te1 Br3A 95.1(2) . . ? Cl2A Te1 Br3A 91.3(11) . . ? Cl1A Te1 Br3A 175.3(10) . . ? Cl3A Te1 Br3A 6.1(5) . . ? Br2A Te1 Br3A 85.42(11) . . ? Br1A Te1 Br3A 174.07(13) . . ? C1A Te1 Cl1B 179.0(6) . . ? N1A Te1 Cl1B 102.2(6) . . ? Cl2A Te1 Cl1B 83.5(15) . . ? Cl1A Te1 Cl1B 93.0(11) . . ? Cl3A Te1 Cl1B 88.5(7) . . ? Br2A Te1 Cl1B 85.7(6) . . ? Br1A Te1 Cl1B 91.1(4) . . ? Br3A Te1 Cl1B 91.7(4) . . ? C1A Te1 Br1B 174.4(3) . . ? N1A Te1 Br1B 103.7(3) . . ? Cl2A Te1 Br1B 81.3(13) . . ? Cl1A Te1 Br1B 87.0(10) . . ? Cl3A Te1 Br1B 94.3(6) . . ? Br2A Te1 Br1B 84.00(16) . . ? Br1A Te1 Br1B 85.00(12) . . ? Br3A Te1 Br1B 97.64(7) . . ? Cl1B Te1 Br1B 6.4(4) . . ? C1B Te2 Cl3B 97.0(14) . . ? C1B Te2 Cl1B 91.3(8) . . ? Cl3B Te2 Cl1B 84.1(19) . . ? C1B Te2 Cl2B 90.4(13) . . ? Cl3B Te2 Cl2B 89(2) . . ? Cl1B Te2 Cl2B 173.5(16) . . ? C1B Te2 N1B 76.7(4) . . ? Cl3B Te2 N1B 173.6(14) . . ? Cl1B Te2 N1B 97.5(9) . . ? Cl2B Te2 N1B 89.0(14) . . ? C1B Te2 Br3B 93.9(3) . . ? Cl3B Te2 Br3B 3.1(15) . . ? Cl1B Te2 Br3B 84.5(9) . . ? Cl2B Te2 Br3B 89.1(14) . . ? N1B Te2 Br3B 170.4(3) . . ? C1B Te2 Br2B 88.1(3) . . ? Cl3B Te2 Br2B 90.0(16) . . ? Cl1B Te2 Br2B 173.9(9) . . ? Cl2B Te2 Br2B 2.3(13) . . ? N1B Te2 Br2B 88.3(2) . . ? Br3B Te2 Br2B 89.47(13) . . ? C1B Te2 Br1B 88.7(3) . . ? Cl3B Te2 Br1B 87.9(16) . . ? Cl1B Te2 Br1B 4.4(8) . . ? Cl2B Te2 Br1B 177.1(14) . . ? N1B Te2 Br1B 93.5(2) . . ? Br3B Te2 Br1B 88.21(12) . . ? Br2B Te2 Br1B 175.88(10) . . ? C1B Te2 Cl3A 175.0(4) . . ? Cl3B Te2 Cl3A 83.1(14) . . ? Cl1B Te2 Cl3A 93.7(8) . . ? Cl2B Te2 Cl3A 84.6(13) . . ? N1B Te2 Cl3A 103.0(5) . . ? Br3B Te2 Cl3A 86.2(4) . . ? Br2B Te2 Cl3A 86.9(3) . . ? Br1B Te2 Cl3A 96.3(3) . . ? C1B Te2 Br3A 170.5(3) . . ? Cl3B Te2 Br3A 79.5(13) . . ? Cl1B Te2 Br3A 97.1(8) . . ? Cl2B Te2 Br3A 80.8(13) . . ? N1B Te2 Br3A 106.4(3) . . ? Br3B Te2 Br3A 82.56(9) . . ? Br2B Te2 Br3A 83.08(9) . . ? Br1B Te2 Br3A 100.00(6) . . ? Cl3A Te2 Br3A 5.3(3) . . ? Te1 Br3A Te2 82.05(6) . . ? Te2 Br1B Te1 80.31(5) . . ? Te1 Cl3A Te2 88.8(6) . . ? Te2 Cl1B Te1 89.0(8) . . ? C7A N1A C9A 112.1(12) . . ? C7A N1A C8A 110.1(10) . . ? C9A N1A C8A 109.9(12) . . ? C7A N1A Te1 103.1(9) . . ? C9A N1A Te1 109.2(9) . . ? C8A N1A Te1 112.2(8) . . ? C7B N1B C8B 110.0(10) . . ? C7B N1B C9B 109.8(11) . . ? C8B N1B C9B 110.1(12) . . ? C7B N1B Te2 104.7(7) . . ? C8B N1B Te2 112.3(9) . . ? C9B N1B Te2 109.8(8) . . ? C2A C1A C6A 123.4(12) . . ? C2A C1A Te1 122.3(10) . . ? C6A C1A Te1 114.1(9) . . ? C1A C2A C3A 117.1(15) . . ? C1A C2A H2AA 121.5 . . ? C3A C2A H2AA 121.5 . . ? C4A C3A C2A 121.0(14) . . ? C4A C3A H3AA 119.5 . . ? C2A C3A H3AA 119.5 . . ? C3A C4A C5A 121.2(11) . . ? C3A C4A H4AA 119.4 . . ? C5A C4A H4AA 119.4 . . ? C4A C5A C6A 120.3(12) . . ? C4A C5A H5AA 119.8 . . ? C6A C5A H5AA 119.8 . . ? C1A C6A C5A 116.6(12) . . ? C1A C6A C7A 120.7(11) . . ? C5A C6A C7A 122.4(12) . . ? N1A C7A C6A 111.0(12) . . ? N1A C7A H7AA 109.4 . . ? C6A C7A H7AA 109.4 . . ? N1A C7A H7AB 109.4 . . ? C6A C7A H7AB 109.4 . . ? H7AA C7A H7AB 108.0 . . ? N1A C8A H8AA 109.5 . . ? N1A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? N1A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? N1A C9A H9AA 109.5 . . ? N1A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? N1A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C2B C1B C6B 120.9(11) . . ? C2B C1B Te2 123.8(9) . . ? C6B C1B Te2 115.2(8) . . ? C1B C2B C3B 120.4(13) . . ? C1B C2B H2BA 119.8 . . ? C3B C2B H2BA 119.8 . . ? C4B C3B C2B 119.5(14) . . ? C4B C3B H3BA 120.3 . . ? C2B C3B H3BA 120.3 . . ? C3B C4B C5B 121.2(11) . . ? C3B C4B H4BA 119.4 . . ? C5B C4B H4BA 119.4 . . ? C4B C5B C6B 118.6(11) . . ? C4B C5B H5BA 120.7 . . ? C6B C5B H5BA 120.7 . . ? C1B C6B C5B 119.3(12) . . ? C1B C6B C7B 119.6(10) . . ? C5B C6B C7B 121.0(11) . . ? N1B C7B C6B 109.6(11) . . ? N1B C7B H7BA 109.8 . . ? C6B C7B H7BA 109.8 . . ? N1B C7B H7BB 109.8 . . ? C6B C7B H7BB 109.8 . . ? H7BA C7B H7BB 108.2 . . ? N1B C8B H8BA 109.5 . . ? N1B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? N1B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? N1B C9B H9BA 109.5 . . ? N1B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? N1B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1A Te1 Br3A Te2 -178.3(3) . . . . ? N1A Te1 Br3A Te2 105.0(3) . . . . ? Cl2A Te1 Br3A Te2 -80.9(14) . . . . ? Cl1A Te1 Br3A Te2 179(84) . . . . ? Cl3A Te1 Br3A Te2 -56(6) . . . . ? Br2A Te1 Br3A Te2 -82.87(17) . . . . ? Br1A Te1 Br3A Te2 -115.7(9) . . . . ? Cl1B Te1 Br3A Te2 2.7(6) . . . . ? Br1B Te1 Br3A Te2 0.44(6) . . . . ? C1B Te2 Br3A Te1 -156(2) . . . . ? Cl3B Te2 Br3A Te1 -86.6(17) . . . . ? Cl1B Te2 Br3A Te1 -4.0(9) . . . . ? Cl2B Te2 Br3A Te1 -177.7(14) . . . . ? N1B Te2 Br3A Te1 96.1(2) . . . . ? Br3B Te2 Br3A Te1 -87.44(12) . . . . ? Br2B Te2 Br3A Te1 -177.81(10) . . . . ? Br1B Te2 Br3A Te1 -0.59(8) . . . . ? Cl3A Te2 Br3A Te1 46(5) . . . . ? C1B Te2 Br1B Te1 176.5(3) . . . . ? Cl3B Te2 Br1B Te1 79.4(14) . . . . ? Cl1B Te2 Br1B Te1 50(11) . . . . ? Cl2B Te2 Br1B Te1 106(24) . . . . ? N1B Te2 Br1B Te1 -106.8(3) . . . . ? Br3B Te2 Br1B Te1 82.57(8) . . . . ? Br2B Te2 Br1B Te1 138.4(13) . . . . ? Cl3A Te2 Br1B Te1 -3.4(4) . . . . ? Br3A Te2 Br1B Te1 0.45(6) . . . . ? C1A Te1 Br1B Te2 166(4) . . . . ? N1A Te1 Br1B Te2 -97.8(3) . . . . ? Cl2A Te1 Br1B Te2 89.6(11) . . . . ? Cl1A Te1 Br1B Te2 179.6(9) . . . . ? Cl3A Te1 Br1B Te2 4.6(6) . . . . ? Br2A Te1 Br1B Te2 83.97(13) . . . . ? Br1A Te1 Br1B Te2 174.08(11) . . . . ? Br3A Te1 Br1B Te2 -0.58(7) . . . . ? Cl1B Te1 Br1B Te2 -21(5) . . . . ? C1A Te1 Cl3A Te2 178.2(5) . . . . ? N1A Te1 Cl3A Te2 101.2(5) . . . . ? Cl2A Te1 Cl3A Te2 -84.5(14) . . . . ? Cl1A Te1 Cl3A Te2 -108(12) . . . . ? Br2A Te1 Cl3A Te2 -86.7(4) . . . . ? Br1A Te1 Cl3A Te2 -89(3) . . . . ? Br3A Te1 Cl3A Te2 120(6) . . . . ? Cl1B Te1 Cl3A Te2 -0.9(7) . . . . ? Br1B Te1 Cl3A Te2 -3.6(4) . . . . ? C1B Te2 Cl3A Te1 -174(6) . . . . ? Cl3B Te2 Cl3A Te1 -82.3(18) . . . . ? Cl1B Te2 Cl3A Te1 1.3(10) . . . . ? Cl2B Te2 Cl3A Te1 -172.4(15) . . . . ? N1B Te2 Cl3A Te1 99.9(6) . . . . ? Br3B Te2 Cl3A Te1 -82.9(6) . . . . ? Br2B Te2 Cl3A Te1 -172.6(6) . . . . ? Br1B Te2 Cl3A Te1 4.9(6) . . . . ? Br3A Te2 Cl3A Te1 -129(5) . . . . ? C1B Te2 Cl1B Te1 178.7(6) . . . . ? Cl3B Te2 Cl1B Te1 81.7(15) . . . . ? Cl2B Te2 Cl1B Te1 74(14) . . . . ? N1B Te2 Cl1B Te1 -104.5(6) . . . . ? Br3B Te2 Cl1B Te1 84.9(6) . . . . ? Br2B Te2 Cl1B Te1 94(7) . . . . ? Br1B Te2 Cl1B Te1 -128(11) . . . . ? Cl3A Te2 Cl1B Te1 -0.9(7) . . . . ? Br3A Te2 Cl1B Te1 3.1(7) . . . . ? C1A Te1 Cl1B Te2 -68(32) . . . . ? N1A Te1 Cl1B Te2 -99.6(9) . . . . ? Cl2A Te1 Cl1B Te2 87.2(14) . . . . ? Cl1A Te1 Cl1B Te2 176.3(12) . . . . ? Cl3A Te1 Cl1B Te2 1.3(10) . . . . ? Br2A Te1 Cl1B Te2 81.3(9) . . . . ? Br1A Te1 Cl1B Te2 170.8(9) . . . . ? Br3A Te1 Cl1B Te2 -4.0(9) . . . . ? Br1B Te1 Cl1B Te2 156(6) . . . . ? C1A Te1 N1A C7A 29.2(8) . . . . ? Cl2A Te1 N1A C7A -22(7) . . . . ? Cl1A Te1 N1A C7A -59.7(13) . . . . ? Cl3A Te1 N1A C7A 117.8(9) . . . . ? Br2A Te1 N1A C7A 22(2) . . . . ? Br1A Te1 N1A C7A -60.3(7) . . . . ? Br3A Te1 N1A C7A 115.8(7) . . . . ? Cl1B Te1 N1A C7A -151.3(8) . . . . ? Br1B Te1 N1A C7A -145.0(7) . . . . ? C1A Te1 N1A C9A 148.6(10) . . . . ? Cl2A Te1 N1A C9A 98(7) . . . . ? Cl1A Te1 N1A C9A 59.7(15) . . . . ? Cl3A Te1 N1A C9A -122.8(11) . . . . ? Br2A Te1 N1A C9A 141.5(17) . . . . ? Br1A Te1 N1A C9A 59.1(9) . . . . ? Br3A Te1 N1A C9A -124.8(9) . . . . ? Cl1B Te1 N1A C9A -31.9(10) . . . . ? Br1B Te1 N1A C9A -25.6(10) . . . . ? C1A Te1 N1A C8A -89.2(9) . . . . ? Cl2A Te1 N1A C8A -140(7) . . . . ? Cl1A Te1 N1A C8A -178.1(14) . . . . ? Cl3A Te1 N1A C8A -0.6(11) . . . . ? Br2A Te1 N1A C8A -96(2) . . . . ? Br1A Te1 N1A C8A -178.8(9) . . . . ? Br3A Te1 N1A C8A -2.6(9) . . . . ? Cl1B Te1 N1A C8A 90.2(9) . . . . ? Br1B Te1 N1A C8A 96.5(8) . . . . ? C1B Te2 N1B C7B -30.5(7) . . . . ? Cl3B Te2 N1B C7B -16(14) . . . . ? Cl1B Te2 N1B C7B -120.1(11) . . . . ? Cl2B Te2 N1B C7B 60.1(15) . . . . ? Br3B Te2 N1B C7B -18(2) . . . . ? Br2B Te2 N1B C7B 58.0(7) . . . . ? Br1B Te2 N1B C7B -118.3(7) . . . . ? Cl3A Te2 N1B C7B 144.4(8) . . . . ? Br3A Te2 N1B C7B 140.3(7) . . . . ? C1B Te2 N1B C8B 88.9(9) . . . . ? Cl3B Te2 N1B C8B 103(14) . . . . ? Cl1B Te2 N1B C8B -0.7(12) . . . . ? Cl2B Te2 N1B C8B 179.5(16) . . . . ? Br3B Te2 N1B C8B 101.0(17) . . . . ? Br2B Te2 N1B C8B 177.3(9) . . . . ? Br1B Te2 N1B C8B 1.1(9) . . . . ? Cl3A Te2 N1B C8B -96.2(9) . . . . ? Br3A Te2 N1B C8B -100.4(9) . . . . ? C1B Te2 N1B C9B -148.3(10) . . . . ? Cl3B Te2 N1B C9B -134(14) . . . . ? Cl1B Te2 N1B C9B 122.1(12) . . . . ? Cl2B Te2 N1B C9B -57.7(16) . . . . ? Br3B Te2 N1B C9B -136.2(15) . . . . ? Br2B Te2 N1B C9B -59.8(9) . . . . ? Br1B Te2 N1B C9B 123.9(9) . . . . ? Cl3A Te2 N1B C9B 26.6(10) . . . . ? Br3A Te2 N1B C9B 22.5(10) . . . . ? N1A Te1 C1A C2A 161.8(11) . . . . ? Cl2A Te1 C1A C2A -25.1(15) . . . . ? Cl1A Te1 C1A C2A -114.2(13) . . . . ? Cl3A Te1 C1A C2A 60.8(12) . . . . ? Br2A Te1 C1A C2A -19.2(10) . . . . ? Br1A Te1 C1A C2A -108.7(10) . . . . ? Br3A Te1 C1A C2A 66.0(10) . . . . ? Cl1B Te1 C1A C2A 130(31) . . . . ? Br1B Te1 C1A C2A -101(4) . . . . ? N1A Te1 C1A C6A -13.6(8) . . . . ? Cl2A Te1 C1A C6A 159.5(13) . . . . ? Cl1A Te1 C1A C6A 70.4(12) . . . . ? Cl3A Te1 C1A C6A -114.6(10) . . . . ? Br2A Te1 C1A C6A 165.4(8) . . . . ? Br1A Te1 C1A C6A 75.9(8) . . . . ? Br3A Te1 C1A C6A -109.4(8) . . . . ? Cl1B Te1 C1A C6A -46(32) . . . . ? Br1B Te1 C1A C6A 84(4) . . . . ? C6A C1A C2A C3A -8(2) . . . . ? Te1 C1A C2A C3A 177.2(9) . . . . ? C1A C2A C3A C4A 6(2) . . . . ? C2A C3A C4A C5A -3(2) . . . . ? C3A C4A C5A C6A 0.4(19) . . . . ? C2A C1A C6A C5A 5.7(18) . . . . ? Te1 C1A C6A C5A -179.0(8) . . . . ? C2A C1A C6A C7A 179.9(12) . . . . ? Te1 C1A C6A C7A -4.8(14) . . . . ? C4A C5A C6A C1A -1.7(17) . . . . ? C4A C5A C6A C7A -175.8(12) . . . . ? C9A N1A C7A C6A -156.3(11) . . . . ? C8A N1A C7A C6A 81.0(14) . . . . ? Te1 N1A C7A C6A -38.9(11) . . . . ? C1A C6A C7A N1A 33.5(16) . . . . ? C5A C6A C7A N1A -152.6(11) . . . . ? Cl3B Te2 C1B C2B 19.0(19) . . . . ? Cl1B Te2 C1B C2B -65.2(13) . . . . ? Cl2B Te2 C1B C2B 108.5(17) . . . . ? N1B Te2 C1B C2B -162.6(10) . . . . ? Br3B Te2 C1B C2B 19.4(10) . . . . ? Br2B Te2 C1B C2B 108.7(10) . . . . ? Br1B Te2 C1B C2B -68.7(10) . . . . ? Cl3A Te2 C1B C2B 110(6) . . . . ? Br3A Te2 C1B C2B 87(2) . . . . ? Cl3B Te2 C1B C6B -162.7(18) . . . . ? Cl1B Te2 C1B C6B 113.1(11) . . . . ? Cl2B Te2 C1B C6B -73.2(16) . . . . ? N1B Te2 C1B C6B 15.7(7) . . . . ? Br3B Te2 C1B C6B -162.3(7) . . . . ? Br2B Te2 C1B C6B -73.0(7) . . . . ? Br1B Te2 C1B C6B 109.6(7) . . . . ? Cl3A Te2 C1B C6B -72(6) . . . . ? Br3A Te2 C1B C6B -95(2) . . . . ? C6B C1B C2B C3B 2.7(18) . . . . ? Te2 C1B C2B C3B -179.1(10) . . . . ? C1B C2B C3B C4B -2(2) . . . . ? C2B C3B C4B C5B 1.4(19) . . . . ? C3B C4B C5B C6B -1.3(17) . . . . ? C2B C1B C6B C5B -2.5(16) . . . . ? Te2 C1B C6B C5B 179.2(7) . . . . ? C2B C1B C6B C7B -179.9(11) . . . . ? Te2 C1B C6B C7B 1.8(13) . . . . ? C4B C5B C6B C1B 1.7(15) . . . . ? C4B C5B C6B C7B 179.1(10) . . . . ? C8B N1B C7B C6B -82.3(13) . . . . ? C9B N1B C7B C6B 156.3(10) . . . . ? Te2 N1B C7B C6B 38.6(10) . . . . ? C1B C6B C7B N1B -30.6(14) . . . . ? C5B C6B C7B N1B 152.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.432 _refine_diff_density_min -2.885 _refine_diff_density_rms 0.389 #===END