# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ashok K. S. Chauhan' _publ_contact_author_email akschauhan2003@yahoo.co.in loop_ _publ_author_name S.Misra A.K.S.Chauhan R.C.Srivastava A.Duthie R.J.Butcher # Attachment '- Compond 1.CIF' data_askc-sm3 _database_code_depnum_ccdc_archive 'CCDC 796562' #TrackingRef '- Compond 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H8 Cl2 O Te, C4 H7 N O' _chemical_formula_sum 'C14 H15 Cl2 N O2 Te' _chemical_formula_weight 427.77 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.9609(5) _cell_length_b 7.74529(16) _cell_length_c 23.9193(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.645(3) _cell_angle_gamma 90.00 _cell_volume 3070.95(15) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 20356 _cell_measurement_theta_min 5.0475 _cell_measurement_theta_max 32.7237 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59137 _exptl_absorpt_correction_T_max 1.00000 _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) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 25706 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 5.06 _diffrn_reflns_theta_max 32.79 _reflns_number_total 5313 _reflns_number_gt 5109 _reflns_threshold_expression I>2\s(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 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^)+(0.0139P)^2^+5.2350P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5313 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0446 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _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 0.724626(5) 0.887885(12) 0.405452(4) 0.01329(3) Uani 1 1 d . . . Cl1 Cl 0.84696(2) 0.73247(5) 0.480911(16) 0.01839(7) Uani 1 1 d . . . Cl2 Cl 0.60437(2) 1.02272(5) 0.328949(16) 0.01925(7) Uani 1 1 d . . . O1 O 0.67774(7) 0.67264(16) 0.37491(5) 0.0208(2) Uani 1 1 d . . . H1O H 0.693(2) 0.595(4) 0.4020(14) 0.058(9) Uiso 1 1 d . . . O1A O 0.70683(6) 0.41002(15) 0.44480(5) 0.0192(2) Uani 1 1 d . . . N1A N 0.63428(7) 0.21494(17) 0.47479(6) 0.0153(2) Uani 1 1 d . . . H1N H 0.6756(15) 0.165(3) 0.4966(11) 0.029(6) Uiso 1 1 d . . . C1 C 0.78557(8) 0.90919(18) 0.34559(6) 0.0126(2) Uani 1 1 d . . . C2 C 0.78534(8) 0.76735(19) 0.31127(6) 0.0157(2) Uani 1 1 d . . . H2A H 0.7575 0.6655 0.3140 0.019 Uiso 1 1 calc R . . C3 C 0.82709(9) 0.7740(2) 0.27171(7) 0.0189(3) Uani 1 1 d . . . H3A H 0.8268 0.6765 0.2475 0.023 Uiso 1 1 calc R . . C4 C 0.86783(9) 0.9200(2) 0.26812(7) 0.0191(3) Uani 1 1 d . . . H4A H 0.8960 0.9222 0.2417 0.023 Uiso 1 1 calc R . . C5 C 0.86879(8) 1.0684(2) 0.30319(6) 0.0154(2) Uani 1 1 d . . . C6 C 0.90997(9) 1.2215(2) 0.29947(8) 0.0220(3) Uani 1 1 d . . . H6A H 0.9387 1.2250 0.2734 0.026 Uiso 1 1 calc R . . C7 C 0.90888(10) 1.3642(2) 0.33279(8) 0.0252(3) Uani 1 1 d . . . H7A H 0.9373 1.4652 0.3301 0.030 Uiso 1 1 calc R . . C8 C 0.86566(10) 1.3619(2) 0.37112(8) 0.0221(3) Uani 1 1 d . . . H8A H 0.8646 1.4619 0.3938 0.026 Uiso 1 1 calc R . . C9 C 0.82506(9) 1.21566(19) 0.37582(7) 0.0174(3) Uani 1 1 d . . . H9A H 0.7959 1.2160 0.4016 0.021 Uiso 1 1 calc R . . C10 C 0.82617(8) 1.06483(18) 0.34286(6) 0.0128(2) Uani 1 1 d . . . C1A C 0.64107(8) 0.34841(18) 0.44226(6) 0.0139(2) Uani 1 1 d . . . C2A C 0.55824(8) 0.4108(2) 0.40178(7) 0.0181(3) Uani 1 1 d . . . H2AA H 0.5456 0.3785 0.3590 0.022 Uiso 1 1 calc R . . H2AB H 0.5539 0.5377 0.4045 0.022 Uiso 1 1 calc R . . C3A C 0.50223(9) 0.3183(2) 0.42664(8) 0.0234(3) Uani 1 1 d . . . H3AA H 0.4521 0.2803 0.3932 0.028 Uiso 1 1 calc R . . H3AB H 0.4877 0.3951 0.4540 0.028 Uiso 1 1 calc R . . C4A C 0.55095(9) 0.1622(2) 0.46142(7) 0.0204(3) Uani 1 1 d . . . H4AA H 0.5418 0.1413 0.4991 0.024 Uiso 1 1 calc R . . H4AB H 0.5370 0.0566 0.4362 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Te 0.01242(4) 0.01642(4) 0.01215(4) 0.00294(3) 0.00595(3) 0.00047(3) Cl1 0.01524(14) 0.02368(16) 0.01583(14) 0.00481(12) 0.00551(11) 0.00192(12) Cl2 0.01514(14) 0.02436(17) 0.01872(15) 0.00561(13) 0.00705(12) 0.00478(12) O1 0.0199(5) 0.0190(5) 0.0202(5) 0.0047(4) 0.0041(4) -0.0057(4) O1A 0.0116(4) 0.0185(5) 0.0263(5) 0.0067(4) 0.0060(4) -0.0004(4) N1A 0.0110(5) 0.0177(5) 0.0151(5) 0.0041(4) 0.0029(4) 0.0003(4) C1 0.0116(5) 0.0150(6) 0.0116(5) 0.0012(4) 0.0048(4) 0.0000(4) C2 0.0145(6) 0.0166(6) 0.0146(6) -0.0017(5) 0.0042(5) -0.0003(5) C3 0.0192(6) 0.0232(7) 0.0132(6) -0.0045(5) 0.0051(5) 0.0024(5) C4 0.0173(6) 0.0275(8) 0.0147(6) 0.0017(5) 0.0086(5) 0.0044(5) C5 0.0122(5) 0.0201(6) 0.0140(6) 0.0044(5) 0.0050(5) 0.0014(5) C6 0.0171(6) 0.0256(8) 0.0244(7) 0.0093(6) 0.0093(6) -0.0006(6) C7 0.0204(7) 0.0203(7) 0.0317(8) 0.0077(6) 0.0066(6) -0.0042(6) C8 0.0243(7) 0.0152(7) 0.0232(7) 0.0007(5) 0.0053(6) -0.0015(5) C9 0.0199(6) 0.0156(6) 0.0164(6) -0.0001(5) 0.0065(5) -0.0002(5) C10 0.0114(5) 0.0143(6) 0.0121(5) 0.0024(4) 0.0039(4) 0.0007(4) C1A 0.0117(5) 0.0139(6) 0.0152(6) 0.0006(5) 0.0043(4) 0.0006(4) C2A 0.0106(5) 0.0190(7) 0.0222(7) 0.0060(5) 0.0034(5) 0.0015(5) C3A 0.0119(6) 0.0291(8) 0.0283(8) 0.0086(7) 0.0067(5) 0.0013(6) C4A 0.0126(6) 0.0249(7) 0.0216(7) 0.0073(6) 0.0044(5) -0.0030(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te O1 1.8837(12) . ? Te C1 2.1173(13) . ? Te Cl2 2.4619(4) . ? Te Cl1 2.5457(4) . ? O1 H1O 0.85(3) . ? O1A C1A 1.2535(17) . ? N1A C1A 1.3273(18) . ? N1A C4A 1.4630(19) . ? N1A H1N 0.82(2) . ? C1 C2 1.3705(19) . ? C1 C10 1.4233(19) . ? C2 C3 1.417(2) . ? C2 H2A 0.9500 . ? C3 C4 1.368(2) . ? C3 H3A 0.9500 . ? C4 C5 1.419(2) . ? C4 H4A 0.9500 . ? C5 C6 1.419(2) . ? C5 C10 1.4304(19) . ? C6 C7 1.367(3) . ? C6 H6A 0.9500 . ? C7 C8 1.411(3) . ? C7 H7A 0.9500 . ? C8 C9 1.375(2) . ? C8 H8A 0.9500 . ? C9 C10 1.414(2) . ? C9 H9A 0.9500 . ? C1A C2A 1.5083(19) . ? C2A C3A 1.530(2) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.536(2) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Te C1 94.42(5) . . ? O1 Te Cl2 87.36(4) . . ? C1 Te Cl2 89.90(4) . . ? O1 Te Cl1 89.51(4) . . ? C1 Te Cl1 89.23(4) . . ? Cl2 Te Cl1 176.675(13) . . ? Te O1 H1O 111(2) . . ? C1A N1A C4A 113.98(12) . . ? C1A N1A H1N 118.3(17) . . ? C4A N1A H1N 127.3(17) . . ? C2 C1 C10 122.34(13) . . ? C2 C1 Te 117.35(10) . . ? C10 C1 Te 120.30(10) . . ? C1 C2 C3 119.38(14) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 120.38(14) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 121.16(13) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C6 121.87(14) . . ? C4 C5 C10 119.28(13) . . ? C6 C5 C10 118.85(14) . . ? C7 C6 C5 120.96(15) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 120.24(15) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 120.36(15) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 120.87(14) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C1 123.83(13) . . ? C9 C10 C5 118.70(13) . . ? C1 C10 C5 117.45(13) . . ? O1A C1A N1A 124.45(13) . . ? O1A C1A C2A 125.95(13) . . ? N1A C1A C2A 109.60(12) . . ? C1A C2A C3A 103.53(12) . . ? C1A C2A H2AA 111.1 . . ? C3A C2A H2AA 111.1 . . ? C1A C2A H2AB 111.1 . . ? C3A C2A H2AB 111.1 . . ? H2AA C2A H2AB 109.0 . . ? C2A C3A C4A 104.86(12) . . ? C2A C3A H3AA 110.8 . . ? C4A C3A H3AA 110.8 . . ? C2A C3A H3AB 110.8 . . ? C4A C3A H3AB 110.8 . . ? H3AA C3A H3AB 108.9 . . ? N1A C4A C3A 102.73(12) . . ? N1A C4A H4AA 111.2 . . ? C3A C4A H4AA 111.2 . . ? N1A C4A H4AB 111.2 . . ? C3A C4A H4AB 111.2 . . ? H4AA C4A H4AB 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Te C1 C2 -8.87(11) . . . . ? Cl2 Te C1 C2 -96.22(10) . . . . ? Cl1 Te C1 C2 80.57(10) . . . . ? O1 Te C1 C10 172.41(11) . . . . ? Cl2 Te C1 C10 85.07(10) . . . . ? Cl1 Te C1 C10 -98.14(10) . . . . ? C10 C1 C2 C3 0.3(2) . . . . ? Te C1 C2 C3 -178.39(10) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C3 C4 C5 C6 -179.24(14) . . . . ? C3 C4 C5 C10 -0.1(2) . . . . ? C4 C5 C6 C7 178.75(15) . . . . ? C10 C5 C6 C7 -0.4(2) . . . . ? C5 C6 C7 C8 -0.8(2) . . . . ? C6 C7 C8 C9 0.8(3) . . . . ? C7 C8 C9 C10 0.4(2) . . . . ? C8 C9 C10 C1 179.98(14) . . . . ? C8 C9 C10 C5 -1.5(2) . . . . ? C2 C1 C10 C9 177.46(14) . . . . ? Te C1 C10 C9 -3.89(18) . . . . ? C2 C1 C10 C5 -1.0(2) . . . . ? Te C1 C10 C5 177.62(9) . . . . ? C4 C5 C10 C9 -177.64(13) . . . . ? C6 C5 C10 C9 1.5(2) . . . . ? C4 C5 C10 C1 0.94(19) . . . . ? C6 C5 C10 C1 -179.93(13) . . . . ? C4A N1A C1A O1A -177.10(15) . . . . ? C4A N1A C1A C2A 2.00(18) . . . . ? O1A C1A C2A C3A -168.29(15) . . . . ? N1A C1A C2A C3A 12.63(17) . . . . ? C1A C2A C3A C4A -21.30(17) . . . . ? C1A N1A C4A C3A -15.62(18) . . . . ? C2A C3A C4A N1A 22.19(17) . . . . ? 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 O1 H1O O1A 0.85(3) 1.73(3) 2.5557(16) 166(3) . N1A H1N O1A 0.82(2) 2.12(2) 2.9247(16) 168(2) 7_656 C3 H3A Cl2 0.95 2.83 3.6582(15) 145.6 4_645 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.555 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.074 # Attachment '- Compound 2.CIF' data_sm5 _database_code_depnum_ccdc_archive 'CCDC 796563' #TrackingRef '- Compound 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H12 Cl2 O Te, C4 H7 N O' _chemical_formula_sum 'C13 H19 Cl2 N O2 Te' _chemical_formula_weight 419.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 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 13.6291(4) _cell_length_b 6.8780(3) _cell_length_c 19.3019(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.336(4) _cell_angle_gamma 90.00 _cell_volume 1707.33(11) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4264 _cell_measurement_theta_min 5.0988 _cell_measurement_theta_max 32.6078 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53504 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 '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 13068 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 32.68 _reflns_number_total 5677 _reflns_number_gt 2651 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _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^)+(0.0618P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5677 _refine_ls_number_parameters 188 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.917 _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 0.177676(13) 0.69169(4) 0.614732(11) 0.08221(9) Uani 1 1 d . . . Cl1 Cl 0.05280(6) 0.50474(13) 0.65825(5) 0.0925(2) Uani 1 1 d . A . Cl2A Cl 0.31435(10) 0.8704(3) 0.57819(8) 0.1038(5) Uani 0.703(2) 1 d PU A 1 O1AA O 0.2086(3) 0.4870(6) 0.5664(2) 0.1205(12) Uani 0.703(2) 1 d P A 1 H1AB H 0.1843 0.3873 0.5774 0.181 Uiso 0.703(2) 1 calc PR A 1 Cl2B Cl 0.3192(3) 0.7622(7) 0.5711(2) 0.1038(5) Uani 0.297(2) 1 d PU A 2 O1AB O 0.2137(7) 0.3980(18) 0.6017(6) 0.1205(12) Uani 0.297(2) 1 d P A 2 H1AC H 0.1638 0.3459 0.5711 0.181 Uiso 0.297(2) 1 calc PR A 2 O1A O 0.07909(15) 0.2051(3) 0.51130(11) 0.0848(6) Uani 1 1 d . . . N1A N 0.07025(17) -0.0330(4) 0.42895(12) 0.0698(6) Uani 1 1 d . . . H1AA H 0.023(2) -0.100(4) 0.4415(15) 0.074(8) Uiso 1 1 d . . . C1 C 0.28206(18) 0.6946(3) 0.72289(14) 0.0568(6) Uani 1 1 d . A . C2 C 0.3632(2) 0.5620(4) 0.75293(17) 0.0718(8) Uani 1 1 d . . . C3 C 0.4248(2) 0.5912(6) 0.8244(2) 0.0898(10) Uani 1 1 d . A . H3A H 0.4786 0.5035 0.8450 0.108 Uiso 1 1 calc R . . C4 C 0.4127(3) 0.7371(7) 0.8662(2) 0.0987(11) Uani 1 1 d . . . C5 C 0.3326(3) 0.8644(6) 0.8366(2) 0.0996(11) Uani 1 1 d . A . H5A H 0.3226 0.9654 0.8657 0.120 Uiso 1 1 calc R . . C6 C 0.2659(2) 0.8482(4) 0.76520(18) 0.0752(8) Uani 1 1 d . . . C7 C 0.3897(4) 0.3968(7) 0.7119(3) 0.1467(18) Uani 1 1 d . A . H7A H 0.4562 0.3442 0.7401 0.220 Uiso 1 1 calc R . . H7B H 0.3925 0.4428 0.6656 0.220 Uiso 1 1 calc R . . H7C H 0.3376 0.2975 0.7035 0.220 Uiso 1 1 calc R . . C8 C 0.4889(4) 0.7638(10) 0.9451(3) 0.169(3) Uani 1 1 d . A . H8A H 0.5165 0.6397 0.9649 0.254 Uiso 1 1 calc R . . H8B H 0.4527 0.8205 0.9752 0.254 Uiso 1 1 calc R . . H8C H 0.5447 0.8479 0.9443 0.254 Uiso 1 1 calc R . . C9 C 0.1760(4) 0.9896(6) 0.7344(3) 0.1306(16) Uani 1 1 d . A . H9A H 0.1811 1.0922 0.7691 0.196 Uiso 1 1 calc R . . H9B H 0.1113 0.9220 0.7253 0.196 Uiso 1 1 calc R . . H9C H 0.1788 1.0437 0.6892 0.196 Uiso 1 1 calc R . . C1A C 0.10810(19) 0.1284(5) 0.46289(14) 0.0632(7) Uani 1 1 d . . . C2A C 0.1890(2) 0.2078(5) 0.43315(16) 0.0713(8) Uani 1 1 d . . . H2AA H 0.1730 0.3405 0.4161 0.086 Uiso 1 1 calc R . . H2AB H 0.2575 0.2045 0.4702 0.086 Uiso 1 1 calc R . . C3A C 0.1834(3) 0.0750(5) 0.3711(2) 0.1151(10) Uani 1 1 d . . . H3AA H 0.2528 0.0337 0.3740 0.138 Uiso 1 1 calc R . . H3AB H 0.1520 0.1414 0.3247 0.138 Uiso 1 1 calc R . . C4A C 0.1193(2) -0.0974(5) 0.37602(17) 0.0793(8) Uani 1 1 d . . . H4AA H 0.0677 -0.1268 0.3288 0.095 Uiso 1 1 calc R . . H4AB H 0.1624 -0.2111 0.3937 0.095 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 0.05842(11) 0.1201(2) 0.07197(12) -0.00622(11) 0.02672(9) -0.02017(10) Cl1 0.0676(4) 0.0989(5) 0.1192(6) 0.0055(5) 0.0420(4) -0.0159(4) Cl2A 0.0847(5) 0.1377(14) 0.0895(6) 0.0244(9) 0.0297(5) -0.0476(8) O1AA 0.0981(16) 0.160(3) 0.133(3) -0.073(2) 0.0778(17) -0.0633(19) Cl2B 0.0847(5) 0.1377(14) 0.0895(6) 0.0244(9) 0.0297(5) -0.0476(8) O1AB 0.0981(16) 0.160(3) 0.133(3) -0.073(2) 0.0778(17) -0.0633(19) O1A 0.0870(11) 0.1101(15) 0.0784(11) -0.0319(10) 0.0556(9) -0.0353(11) N1A 0.0728(11) 0.0869(15) 0.0669(12) -0.0108(11) 0.0462(10) -0.0214(12) C1 0.0546(11) 0.0578(15) 0.0670(14) -0.0024(12) 0.0321(11) -0.0036(11) C2 0.0616(13) 0.0684(18) 0.0973(19) 0.0030(15) 0.0424(13) 0.0063(14) C3 0.0612(15) 0.116(3) 0.100(2) 0.029(2) 0.0369(15) 0.0076(18) C4 0.0748(18) 0.147(3) 0.082(2) 0.001(2) 0.0365(16) -0.021(2) C5 0.111(2) 0.112(2) 0.091(2) -0.0361(19) 0.0530(19) -0.014(2) C6 0.0800(17) 0.0683(18) 0.0877(19) -0.0084(14) 0.0419(15) 0.0070(14) C7 0.141(3) 0.113(3) 0.205(5) -0.019(3) 0.083(3) 0.053(3) C8 0.133(4) 0.282(7) 0.078(3) -0.003(4) 0.015(3) -0.028(5) C9 0.138(3) 0.093(3) 0.166(4) -0.018(3) 0.059(3) 0.047(2) C1A 0.0543(12) 0.0833(17) 0.0610(14) -0.0041(13) 0.0310(11) -0.0130(13) C2A 0.0627(13) 0.091(2) 0.0741(16) -0.0012(14) 0.0413(12) -0.0140(14) C3A 0.164(2) 0.092(2) 0.148(2) -0.0310(19) 0.1299(19) -0.036(2) C4A 0.0900(16) 0.0843(19) 0.0866(17) -0.0133(16) 0.0604(14) -0.0096(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te O1AA 1.814(4) . ? Te C1 2.101(3) . ? Te O1AB 2.114(12) . ? Te Cl2B 2.397(4) . ? Te Cl1 2.4905(8) . ? Te Cl2A 2.5197(14) . ? O1AA H1AB 0.8200 . ? O1AB H1AC 0.8200 . ? O1A C1A 1.246(3) . ? N1A C1A 1.306(4) . ? N1A C4A 1.463(4) . ? N1A H1AA 0.89(3) . ? C1 C6 1.397(4) . ? C1 C2 1.403(4) . ? C2 C3 1.371(4) . ? C2 C7 1.496(5) . ? C3 C4 1.332(6) . ? C3 H3A 0.9300 . ? C4 C5 1.368(6) . ? C4 C8 1.545(6) . ? C5 C6 1.382(5) . ? C5 H5A 0.9300 . ? C6 C9 1.523(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C1A C2A 1.505(4) . ? C2A C3A 1.489(4) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C4A 1.495(4) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? 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 O1AA Te C1 108.80(14) . . ? O1AA Te O1AB 25.1(3) . . ? C1 Te O1AB 91.2(3) . . ? O1AA Te Cl2B 67.99(16) . . ? C1 Te Cl2B 89.32(12) . . ? O1AB Te Cl2B 84.6(3) . . ? O1AA Te Cl1 94.23(12) . . ? C1 Te Cl1 89.05(7) . . ? O1AB Te Cl1 76.0(3) . . ? Cl2B Te Cl1 160.50(12) . . ? O1AA Te Cl2A 85.16(12) . . ? C1 Te Cl2A 87.32(7) . . ? O1AB Te Cl2A 102.2(2) . . ? Cl2B Te Cl2A 17.64(12) . . ? Cl1 Te Cl2A 175.91(4) . . ? Te O1AA H1AB 109.5 . . ? Te O1AB H1AC 109.5 . . ? C1A N1A C4A 114.3(2) . . ? C1A N1A H1AA 120.2(19) . . ? C4A N1A H1AA 125(2) . . ? C6 C1 C2 120.4(3) . . ? C6 C1 Te 113.71(19) . . ? C2 C1 Te 125.9(2) . . ? C3 C2 C1 117.2(3) . . ? C3 C2 C7 118.0(3) . . ? C1 C2 C7 124.8(3) . . ? C4 C3 C2 124.2(3) . . ? C4 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C3 C4 C5 118.2(3) . . ? C3 C4 C8 120.6(4) . . ? C5 C4 C8 121.2(4) . . ? C4 C5 C6 122.3(3) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C9 121.1(3) . . ? C1 C6 C9 121.1(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1A C1A N1A 124.4(2) . . ? O1A C1A C2A 126.0(3) . . ? N1A C1A C2A 109.6(2) . . ? C3A C2A C1A 103.6(2) . . ? C3A C2A H2AA 111.0 . . ? C1A C2A H2AA 111.0 . . ? C3A C2A H2AB 111.0 . . ? C1A C2A H2AB 111.0 . . ? H2AA C2A H2AB 109.0 . . ? C2A C3A C4A 108.1(2) . . ? C2A C3A H3AA 110.1 . . ? C4A C3A H3AA 110.1 . . ? C2A C3A H3AB 110.1 . . ? C4A C3A H3AB 110.1 . . ? H3AA C3A H3AB 108.4 . . ? N1A C4A C3A 102.5(2) . . ? N1A C4A H4AA 111.3 . . ? C3A C4A H4AA 111.3 . . ? N1A C4A H4AB 111.3 . . ? C3A C4A H4AB 111.3 . . ? H4AA C4A H4AB 109.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1AA Te C1 C6 179.5(2) . . . . ? O1AB Te C1 C6 -162.4(3) . . . . ? Cl2B Te C1 C6 113.1(2) . . . . ? Cl1 Te C1 C6 -86.4(2) . . . . ? Cl2A Te C1 C6 95.5(2) . . . . ? O1AA Te C1 C2 0.7(3) . . . . ? O1AB Te C1 C2 18.8(3) . . . . ? Cl2B Te C1 C2 -65.8(3) . . . . ? Cl1 Te C1 C2 94.8(2) . . . . ? Cl2A Te C1 C2 -83.3(2) . . . . ? C6 C1 C2 C3 -0.4(4) . . . . ? Te C1 C2 C3 178.4(2) . . . . ? C6 C1 C2 C7 -177.8(3) . . . . ? Te C1 C2 C7 1.0(4) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C7 C2 C3 C4 177.1(4) . . . . ? C2 C3 C4 C5 1.2(6) . . . . ? C2 C3 C4 C8 -177.3(4) . . . . ? C3 C4 C5 C6 -1.2(6) . . . . ? C8 C4 C5 C6 177.4(4) . . . . ? C4 C5 C6 C1 0.3(5) . . . . ? C4 C5 C6 C9 178.7(4) . . . . ? C2 C1 C6 C5 0.4(4) . . . . ? Te C1 C6 C5 -178.5(3) . . . . ? C2 C1 C6 C9 -177.9(3) . . . . ? Te C1 C6 C9 3.2(4) . . . . ? C4A N1A C1A O1A -178.1(3) . . . . ? C4A N1A C1A C2A 3.4(3) . . . . ? O1A C1A C2A C3A -173.0(3) . . . . ? N1A C1A C2A C3A 5.6(3) . . . . ? C1A C2A C3A C4A -12.0(4) . . . . ? C1A N1A C4A C3A -10.7(4) . . . . ? C2A C3A C4A N1A 13.6(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 O1AA H1AB O1A 0.82 2.01 2.600(4) 128.4 . O1AB H1AC O1A 0.82 1.65 2.459(9) 168.8 . N1A H1AA O1A 0.89(3) 2.03(3) 2.903(3) 167(3) 3_556 C3 H3A Cl2A 0.93 2.87 3.748(3) 158.2 2_646 _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.660 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.066 # Attachment '- Compound 4.CIF' data_aksc-sm7 _database_code_depnum_ccdc_archive 'CCDC 825838' #TrackingRef '- Compound 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H14 Br6 Te2' _chemical_formula_sum 'C20 H14 Br6 Te2' _chemical_formula_weight 988.97 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' 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 20.3174(8) _cell_length_b 7.3678(3) _cell_length_c 17.7571(8) _cell_angle_alpha 90.00 _cell_angle_beta 115.656(5) _cell_angle_gamma 90.00 _cell_volume 2396.07(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9457 _cell_measurement_theta_min 5.0088 _cell_measurement_theta_max 32.6448 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.8730 _exptl_crystal_size_mid 0.2593 _exptl_crystal_size_min 0.1639 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 12.447 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.026 _exptl_absorpt_correction_T_max 0.173 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) 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 123(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 '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 20066 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 32.72 _reflns_number_total 8027 _reflns_number_gt 6196 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _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^)+(0.1004P)^2^+20.1563P] 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 8027 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1942 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.09050(3) 0.38490(9) 0.30063(4) 0.01310(15) Uani 1 1 d . . . Te2 Te 0.59146(3) 0.36766(9) 0.78909(4) 0.01308(14) Uani 1 1 d . . . Br11 Br 0.01117(7) 0.0831(2) 0.33397(8) 0.0298(3) Uani 1 1 d . . . Br12 Br 0.18289(6) 0.58877(19) 0.28432(9) 0.0299(3) Uani 1 1 d . . . Br21 Br 0.49107(7) 0.57284(19) 0.82357(8) 0.0296(3) Uani 1 1 d . . . Br13 Br 0.19480(6) 0.2181(2) 0.41802(8) 0.0311(3) Uani 1 1 d . . . Br22 Br 0.69414(7) 0.1912(2) 0.77596(10) 0.0339(3) Uani 1 1 d . . . Br23 Br 0.68646(7) 0.5709(2) 0.89526(9) 0.0325(3) Uani 1 1 d . . . C10B C 0.5012(6) 0.5706(15) 0.6195(6) 0.0164(19) Uani 1 1 d . . . C10A C -0.0002(6) 0.5837(15) 0.3826(7) 0.018(2) Uani 1 1 d . . . C9A C -0.0654(5) 0.5090(14) 0.3189(6) 0.0151(18) Uani 1 1 d . . . H9AA H -0.0625 0.4335 0.2770 0.018 Uiso 1 1 calc R . . C6B C 0.4280(7) 0.7313(15) 0.4896(7) 0.024(2) Uani 1 1 d . . . H6BA H 0.4248 0.8118 0.4463 0.029 Uiso 1 1 calc R . . C1A C 0.0714(5) 0.5547(14) 0.3862(6) 0.0145(18) Uani 1 1 d . . . C5A C -0.0064(7) 0.6957(15) 0.4427(7) 0.020(2) Uani 1 1 d . . . C5B C 0.4972(6) 0.6900(15) 0.5546(6) 0.019(2) Uani 1 1 d . . . C1B C 0.5726(6) 0.5380(15) 0.6857(7) 0.0165(19) Uani 1 1 d . . . C2A C 0.1310(7) 0.6392(16) 0.4473(7) 0.024(2) Uani 1 1 d . . . H2AA H 0.1778 0.6232 0.4485 0.029 Uiso 1 1 calc R . . C9B C 0.4367(6) 0.4962(15) 0.6152(6) 0.0167(19) Uani 1 1 d . . . H9BA H 0.4385 0.4139 0.6572 0.020 Uiso 1 1 calc R . . C8B C 0.3695(6) 0.5404(17) 0.5503(7) 0.021(2) Uani 1 1 d . . . H8BA H 0.3261 0.4895 0.5490 0.025 Uiso 1 1 calc R . . C3A C 0.1240(7) 0.7474(18) 0.5074(7) 0.025(2) Uani 1 1 d . . . H3AA H 0.1658 0.8039 0.5494 0.030 Uiso 1 1 calc R . . C4A C 0.0580(7) 0.7721(17) 0.5060(7) 0.026(2) Uani 1 1 d . . . H4AA H 0.0542 0.8430 0.5486 0.031 Uiso 1 1 calc R . . C6A C -0.0765(7) 0.7311(15) 0.4394(8) 0.024(2) Uani 1 1 d . . . H6AA H -0.0803 0.8070 0.4806 0.028 Uiso 1 1 calc R . . C4B C 0.5608(7) 0.7656(16) 0.5542(7) 0.023(2) Uani 1 1 d . . . H4BA H 0.5568 0.8398 0.5087 0.027 Uiso 1 1 calc R . . C2B C 0.6348(6) 0.6181(17) 0.6851(8) 0.023(2) Uani 1 1 d . . . H2BA H 0.6815 0.5950 0.7294 0.027 Uiso 1 1 calc R . . C3B C 0.6279(8) 0.7340(19) 0.6182(9) 0.033(3) Uani 1 1 d . . . H3BA H 0.6700 0.7896 0.6179 0.040 Uiso 1 1 calc R . . C7A C -0.1380(7) 0.6586(17) 0.3786(9) 0.029(3) Uani 1 1 d . . . H7AA H -0.1844 0.6837 0.3771 0.035 Uiso 1 1 calc R . . C8A C -0.1322(6) 0.5457(16) 0.3177(8) 0.023(2) Uani 1 1 d . . . H8AA H -0.1751 0.4941 0.2752 0.028 Uiso 1 1 calc R . . C7B C 0.3655(8) 0.6577(18) 0.4877(8) 0.031(3) Uani 1 1 d . . . H7BA H 0.3195 0.6871 0.4435 0.037 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 0.0098(3) 0.0147(3) 0.0152(3) 0.0008(2) 0.0058(2) 0.0005(2) Te2 0.0110(3) 0.0122(3) 0.0151(3) 0.0004(2) 0.0048(2) 0.0000(2) Br11 0.0301(6) 0.0340(7) 0.0267(6) -0.0013(5) 0.0134(5) -0.0046(5) Br12 0.0183(5) 0.0318(7) 0.0396(7) 0.0067(5) 0.0125(5) -0.0036(5) Br21 0.0338(6) 0.0300(7) 0.0278(6) 0.0024(5) 0.0161(5) 0.0036(5) Br13 0.0190(5) 0.0369(8) 0.0318(6) 0.0082(5) 0.0057(4) 0.0054(5) Br22 0.0229(5) 0.0298(7) 0.0526(8) 0.0040(6) 0.0196(6) 0.0053(5) Br23 0.0225(5) 0.0336(7) 0.0313(6) -0.0082(5) 0.0022(5) -0.0063(5) C10B 0.026(5) 0.013(5) 0.013(4) 0.001(4) 0.010(4) 0.003(4) C10A 0.021(5) 0.013(5) 0.026(5) 0.001(4) 0.014(4) 0.002(4) C9A 0.013(4) 0.014(5) 0.019(4) -0.001(4) 0.008(3) 0.001(4) C6B 0.045(7) 0.009(5) 0.017(5) -0.002(4) 0.012(5) 0.002(5) C1A 0.014(4) 0.015(5) 0.014(4) -0.003(4) 0.006(3) -0.003(4) C5A 0.036(6) 0.010(5) 0.016(4) 0.000(4) 0.015(4) 0.003(4) C5B 0.036(6) 0.011(5) 0.015(4) -0.001(4) 0.016(4) 0.005(4) C1B 0.022(5) 0.010(4) 0.019(4) 0.001(4) 0.011(4) -0.001(4) C2A 0.023(5) 0.021(6) 0.023(5) 0.002(4) 0.006(4) -0.005(4) C9B 0.018(4) 0.013(5) 0.017(4) -0.004(4) 0.006(4) -0.001(4) C8B 0.014(4) 0.023(6) 0.019(5) 0.003(4) 0.000(4) 0.002(4) C3A 0.031(6) 0.026(6) 0.011(4) 0.000(4) 0.003(4) -0.003(5) C4A 0.042(7) 0.021(6) 0.015(5) -0.003(4) 0.012(5) -0.008(5) C6A 0.038(6) 0.011(5) 0.032(6) 0.005(4) 0.025(5) 0.009(5) C4B 0.039(6) 0.013(5) 0.025(5) 0.004(4) 0.022(5) -0.001(5) C2B 0.018(5) 0.024(6) 0.028(5) 0.000(5) 0.012(4) -0.001(4) C3B 0.049(8) 0.021(6) 0.051(8) 0.002(6) 0.041(7) -0.004(6) C7A 0.034(6) 0.020(6) 0.048(8) 0.005(5) 0.032(6) 0.002(5) C8A 0.021(5) 0.018(5) 0.040(7) 0.004(5) 0.022(5) 0.001(4) C7B 0.038(7) 0.019(6) 0.021(5) -0.003(5) 0.000(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 C1A 2.130(10) . ? Te1 Br12 2.5168(14) . ? Te1 Br13 2.5537(13) . ? Te1 Br11 2.7997(14) 2 ? Te1 Br11 2.9526(15) . ? Te2 C1B 2.118(11) . ? Te2 Br23 2.5240(14) . ? Te2 Br22 2.5529(14) . ? Te2 Br21 2.8110(15) . ? Te2 Br21 2.9373(15) 2_646 ? Br11 Te1 2.7997(14) 2_545 ? Br21 Te2 2.9373(15) 2_656 ? C10B C9B 1.392(15) . ? C10B C5B 1.424(14) . ? C10B C1B 1.438(15) . ? C10A C5A 1.398(15) . ? C10A C9A 1.428(15) . ? C10A C1A 1.444(14) . ? C9A C8A 1.376(14) . ? C9A H9AA 0.9500 . ? C6B C7B 1.367(19) . ? C6B C5B 1.414(16) . ? C6B H6BA 0.9500 . ? C1A C2A 1.376(14) . ? C5A C4A 1.420(16) . ? C5A C6A 1.422(16) . ? C5B C4B 1.409(16) . ? C1B C2B 1.398(15) . ? C2A C3A 1.386(17) . ? C2A H2AA 0.9500 . ? C9B C8B 1.390(14) . ? C9B H9BA 0.9500 . ? C8B C7B 1.382(17) . ? C8B H8BA 0.9500 . ? C3A C4A 1.343(18) . ? C3A H3AA 0.9500 . ? C4A H4AA 0.9500 . ? C6A C7A 1.358(19) . ? C6A H6AA 0.9500 . ? C4B C3B 1.36(2) . ? C4B H4BA 0.9500 . ? C2B C3B 1.420(18) . ? C2B H2BA 0.9500 . ? C3B H3BA 0.9500 . ? C7A C8A 1.409(18) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C7B H7BA 0.9500 . ? 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 Br12 96.1(3) . . ? C1A Te1 Br13 92.5(3) . . ? Br12 Te1 Br13 89.12(5) . . ? C1A Te1 Br11 90.4(3) . 2 ? Br12 Te1 Br11 84.37(5) . 2 ? Br13 Te1 Br11 173.11(5) . 2 ? C1A Te1 Br11 90.9(3) . . ? Br12 Te1 Br11 166.30(5) . . ? Br13 Te1 Br11 78.81(4) . . ? Br11 Te1 Br11 107.39(3) 2 . ? C1B Te2 Br23 95.1(3) . . ? C1B Te2 Br22 94.0(3) . . ? Br23 Te2 Br22 88.82(5) . . ? C1B Te2 Br21 89.7(3) . . ? Br23 Te2 Br21 84.87(5) . . ? Br22 Te2 Br21 172.94(5) . . ? C1B Te2 Br21 90.7(3) . 2_646 ? Br23 Te2 Br21 166.87(5) . 2_646 ? Br22 Te2 Br21 79.01(5) . 2_646 ? Br21 Te2 Br21 106.98(3) . 2_646 ? Te1 Br11 Te1 119.13(5) 2_545 . ? Te2 Br21 Te2 120.23(5) . 2_656 ? C9B C10B C5B 118.5(10) . . ? C9B C10B C1B 124.9(10) . . ? C5B C10B C1B 116.6(10) . . ? C5A C10A C9A 118.3(10) . . ? C5A C10A C1A 118.5(10) . . ? C9A C10A C1A 123.2(10) . . ? C8A C9A C10A 120.4(10) . . ? C8A C9A H9AA 119.8 . . ? C10A C9A H9AA 119.8 . . ? C7B C6B C5B 121.3(11) . . ? C7B C6B H6BA 119.4 . . ? C5B C6B H6BA 119.4 . . ? C2A C1A C10A 119.5(10) . . ? C2A C1A Te1 117.3(8) . . ? C10A C1A Te1 123.2(7) . . ? C10A C5A C4A 118.7(11) . . ? C10A C5A C6A 119.7(11) . . ? C4A C5A C6A 121.5(10) . . ? C4B C5B C6B 120.0(10) . . ? C4B C5B C10B 121.2(10) . . ? C6B C5B C10B 118.8(11) . . ? C2B C1B C10B 121.3(10) . . ? C2B C1B Te2 115.6(8) . . ? C10B C1B Te2 123.1(8) . . ? C1A C2A C3A 121.3(11) . . ? C1A C2A H2AA 119.4 . . ? C3A C2A H2AA 119.4 . . ? C8B C9B C10B 121.1(10) . . ? C8B C9B H9BA 119.5 . . ? C10B C9B H9BA 119.5 . . ? C7B C8B C9B 120.5(11) . . ? C7B C8B H8BA 119.8 . . ? C9B C8B H8BA 119.8 . . ? C4A C3A C2A 119.8(11) . . ? C4A C3A H3AA 120.1 . . ? C2A C3A H3AA 120.1 . . ? C3A C4A C5A 122.1(11) . . ? C3A C4A H4AA 118.9 . . ? C5A C4A H4AA 118.9 . . ? C7A C6A C5A 121.4(11) . . ? C7A C6A H6AA 119.3 . . ? C5A C6A H6AA 119.3 . . ? C3B C4B C5B 121.1(10) . . ? C3B C4B H4BA 119.5 . . ? C5B C4B H4BA 119.5 . . ? C1B C2B C3B 119.9(11) . . ? C1B C2B H2BA 120.1 . . ? C3B C2B H2BA 120.1 . . ? C4B C3B C2B 120.0(11) . . ? C4B C3B H3BA 120.0 . . ? C2B C3B H3BA 120.0 . . ? C6A C7A C8A 119.3(11) . . ? C6A C7A H7AA 120.4 . . ? C8A C7A H7AA 120.4 . . ? C9A C8A C7A 120.9(11) . . ? C9A C8A H8AA 119.5 . . ? C7A C8A H8AA 119.5 . . ? C6B C7B C8B 119.9(11) . . ? C6B C7B H7BA 120.1 . . ? C8B C7B H7BA 120.1 . . ? 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 Br11 Te1 134.6(3) . . . 2_545 ? Br12 Te1 Br11 Te1 -104.5(2) . . . 2_545 ? Br13 Te1 Br11 Te1 -133.05(6) . . . 2_545 ? Br11 Te1 Br11 Te1 43.85(7) 2 . . 2_545 ? C1B Te2 Br21 Te2 4.3(3) . . . 2_656 ? Br23 Te2 Br21 Te2 99.46(6) . . . 2_656 ? Br22 Te2 Br21 Te2 126.3(4) . . . 2_656 ? Br21 Te2 Br21 Te2 -86.31(8) 2_646 . . 2_656 ? C5A C10A C9A C8A -0.7(16) . . . . ? C1A C10A C9A C8A -178.3(11) . . . . ? C5A C10A C1A C2A -0.9(16) . . . . ? C9A C10A C1A C2A 176.7(11) . . . . ? C5A C10A C1A Te1 179.0(8) . . . . ? C9A C10A C1A Te1 -3.4(15) . . . . ? Br12 Te1 C1A C2A -40.3(9) . . . . ? Br13 Te1 C1A C2A 49.1(8) . . . . ? Br11 Te1 C1A C2A -124.7(8) 2 . . . ? Br11 Te1 C1A C2A 127.9(8) . . . . ? Br12 Te1 C1A C10A 139.7(8) . . . . ? Br13 Te1 C1A C10A -130.9(9) . . . . ? Br11 Te1 C1A C10A 55.4(9) 2 . . . ? Br11 Te1 C1A C10A -52.0(9) . . . . ? C9A C10A C5A C4A -179.4(10) . . . . ? C1A C10A C5A C4A -1.7(16) . . . . ? C9A C10A C5A C6A 0.5(16) . . . . ? C1A C10A C5A C6A 178.2(10) . . . . ? C7B C6B C5B C4B 179.0(11) . . . . ? C7B C6B C5B C10B -0.6(16) . . . . ? C9B C10B C5B C4B -178.2(10) . . . . ? C1B C10B C5B C4B 2.5(15) . . . . ? C9B C10B C5B C6B 1.4(15) . . . . ? C1B C10B C5B C6B -177.9(10) . . . . ? C9B C10B C1B C2B 179.9(11) . . . . ? C5B C10B C1B C2B -0.9(15) . . . . ? C9B C10B C1B Te2 0.1(15) . . . . ? C5B C10B C1B Te2 179.4(7) . . . . ? Br23 Te2 C1B C2B 40.4(8) . . . . ? Br22 Te2 C1B C2B -48.8(8) . . . . ? Br21 Te2 C1B C2B 125.2(8) . . . . ? Br21 Te2 C1B C2B -127.8(8) 2_646 . . . ? Br23 Te2 C1B C10B -139.8(8) . . . . ? Br22 Te2 C1B C10B 131.0(8) . . . . ? Br21 Te2 C1B C10B -55.0(9) . . . . ? Br21 Te2 C1B C10B 52.0(9) 2_646 . . . ? C10A C1A C2A C3A 2.1(17) . . . . ? Te1 C1A C2A C3A -177.9(9) . . . . ? C5B C10B C9B C8B -1.6(15) . . . . ? C1B C10B C9B C8B 177.7(11) . . . . ? C10B C9B C8B C7B 1.0(17) . . . . ? C1A C2A C3A C4A -0.5(19) . . . . ? C2A C3A C4A C5A -2.2(19) . . . . ? C10A C5A C4A C3A 3.3(17) . . . . ? C6A C5A C4A C3A -176.5(12) . . . . ? C10A C5A C6A C7A -0.2(17) . . . . ? C4A C5A C6A C7A 179.6(11) . . . . ? C6B C5B C4B C3B 177.1(11) . . . . ? C10B C5B C4B C3B -3.3(17) . . . . ? C10B C1B C2B C3B -0.1(17) . . . . ? Te2 C1B C2B C3B 179.7(9) . . . . ? C5B C4B C3B C2B 2.3(19) . . . . ? C1B C2B C3B C4B -0.6(19) . . . . ? C5A C6A C7A C8A 0.2(18) . . . . ? C10A C9A C8A C7A 0.6(17) . . . . ? C6A C7A C8A C9A -0.4(18) . . . . ? C5B C6B C7B C8B -0.1(18) . . . . ? C9B C8B C7B C6B -0.1(18) . . . . ? 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 C9A H9AA Br11 0.95 2.82 3.386(10) 118.9 2 C9B H9BA Br21 0.95 2.84 3.419(11) 120.4 2_646 C4A H4AA Br11 0.95 2.97 3.827(12) 151.2 3_566 C4B H4BA Br21 0.95 3.03 3.895(11) 151.6 4_575 C8A H8AA Br22 0.95 2.99 3.712(11) 133.6 4_465 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.068 _refine_diff_density_min -3.872 _refine_diff_density_rms 0.379 # Attachment '- Compound 5.CIF' data_aksc-sm6 _database_code_depnum_ccdc_archive 'CCDC 825839' #TrackingRef '- Compound 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Cl4 Te, 2(C5 H9 N O)' _chemical_formula_sum 'C20 H25 Cl4 N2 O2 Te' _chemical_formula_weight 594.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0476(4) _cell_length_b 10.8133(3) _cell_length_c 11.8837(5) _cell_angle_alpha 91.270(3) _cell_angle_beta 112.652(4) _cell_angle_gamma 95.227(3) _cell_volume 1184.28(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9702 _cell_measurement_theta_min 5.1380 _cell_measurement_theta_max 32.7130 _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47400 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 '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 16082 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.15 _diffrn_reflns_theta_max 32.79 _reflns_number_total 7808 _reflns_number_gt 6384 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _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^)+(0.0283P)^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 SHELXL _refine_ls_extinction_coef 0.0024(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7808 _refine_ls_number_parameters 395 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 Te Te 0.345692(10) 0.058956(8) 0.337104(9) 0.01720(3) Uani 1 1 d . . . Cl1 Cl 0.36045(5) -0.01576(4) 0.14126(4) 0.03310(10) Uani 1 1 d . . . Cl2 Cl 0.12826(4) -0.10011(3) 0.29308(4) 0.02612(8) Uani 1 1 d . . . Cl3 Cl 0.32607(4) 0.12386(3) 0.53682(4) 0.02478(8) Uani 1 1 d . . . Cl4 Cl 0.55922(4) 0.21727(4) 0.37029(4) 0.02624(8) Uani 1 1 d . . . C1 C 0.19912(15) 0.19118(13) 0.23798(14) 0.0179(3) Uani 1 1 d . . . C2 C 0.09401(17) 0.14231(15) 0.12889(15) 0.0232(3) Uani 1 1 d . . . H2A H 0.0897 0.0571 0.1051 0.028 Uiso 1 1 calc R . . C3 C -0.00770(18) 0.21658(17) 0.05160(15) 0.0270(4) Uani 1 1 d . . . H3A H -0.0803 0.1812 -0.0231 0.032 Uiso 1 1 calc R . . C4 C -0.00150(17) 0.33864(16) 0.08422(15) 0.0257(3) Uani 1 1 d . . . H4A H -0.0693 0.3885 0.0313 0.031 Uiso 1 1 calc R . . C5 C 0.10449(16) 0.39286(15) 0.19602(14) 0.0210(3) Uani 1 1 d . . . C6 C 0.10946(18) 0.52138(15) 0.22937(16) 0.0263(3) Uani 1 1 d . . . H6A H 0.0418 0.5706 0.1752 0.032 Uiso 1 1 calc R . . C7 C 0.20898(18) 0.57470(15) 0.33695(16) 0.0263(3) Uani 1 1 d . . . H7A H 0.2107 0.6604 0.3574 0.032 Uiso 1 1 calc R . . C8 C 0.30958(17) 0.50286(14) 0.41818(15) 0.0217(3) Uani 1 1 d . . . H8A H 0.3781 0.5403 0.4938 0.026 Uiso 1 1 calc R . . C9 C 0.30962(15) 0.37889(13) 0.38902(14) 0.0178(3) Uani 1 1 d . . . H9A H 0.3789 0.3323 0.4449 0.021 Uiso 1 1 calc R . . C10 C 0.20847(15) 0.31926(13) 0.27727(14) 0.0171(3) Uani 1 1 d . . . O1A O 0.62259(16) 0.38769(15) -0.00516(14) 0.0333(4) Uani 0.7996(16) 1 d PD A 1 N1A N 0.4129(2) 0.37227(17) -0.17357(16) 0.0267(4) Uani 0.7996(16) 1 d PD A 1 C1A C 0.4873(2) 0.3544(2) -0.05877(19) 0.0255(4) Uani 0.7996(16) 1 d PD A 1 C2A C 0.3907(3) 0.2873(3) -0.0044(2) 0.0342(6) Uani 0.7996(16) 1 d PD A 1 H2AA H 0.4069 0.3263 0.0767 0.041 Uiso 0.7996(16) 1 calc PR A 1 H2AB H 0.4074 0.1986 0.0042 0.041 Uiso 0.7996(16) 1 calc PR A 1 C3A C 0.2394(2) 0.3014(2) -0.0965(2) 0.0362(6) Uani 0.7996(16) 1 d PD A 1 H3AA H 0.1993 0.3724 -0.0712 0.043 Uiso 0.7996(16) 1 calc PR A 1 H3AB H 0.1732 0.2248 -0.1058 0.043 Uiso 0.7996(16) 1 calc PR A 1 C4A C 0.2600(2) 0.3250(2) -0.2155(2) 0.0291(5) Uani 0.7996(16) 1 d PD A 1 H4AA H 0.2384 0.2471 -0.2676 0.035 Uiso 0.7996(16) 1 calc PR A 1 H4AB H 0.1971 0.3871 -0.2619 0.035 Uiso 0.7996(16) 1 calc PR A 1 C5A C 0.4764(3) 0.4258(3) -0.2554(2) 0.0371(6) Uani 0.7996(16) 1 d PD A 1 H5AA H 0.5809 0.4474 -0.2104 0.056 Uiso 0.7996(16) 1 calc PR A 1 H5AB H 0.4311 0.5009 -0.2877 0.056 Uiso 0.7996(16) 1 calc PR A 1 H5AC H 0.4600 0.3651 -0.3231 0.056 Uiso 0.7996(16) 1 calc PR A 1 O1D O 0.2728(7) 0.4894(5) -0.1150(6) 0.0357(16) Uani 0.2004(16) 1 d PD A 2 N1D N 0.3931(7) 0.3201(6) -0.0798(6) 0.0227(15) Uani 0.2004(16) 1 d PD A 2 C1D C 0.3600(8) 0.4202(7) -0.1336(8) 0.0245(18) Uani 0.2004(16) 1 d PD A 2 C2D C 0.4377(11) 0.4409(10) -0.2190(9) 0.035(2) Uani 0.2004(16) 1 d PD A 2 H2DA H 0.3695 0.4234 -0.3051 0.042 Uiso 0.2004(16) 1 calc PR A 2 H2DB H 0.4833 0.5277 -0.2086 0.042 Uiso 0.2004(16) 1 calc PR A 2 C3D C 0.5500(10) 0.3520(9) -0.1840(10) 0.039(2) Uani 0.2004(16) 1 d PD A 2 H3DA H 0.6449 0.3928 -0.1264 0.047 Uiso 0.2004(16) 1 calc PR A 2 H3DB H 0.5615 0.3161 -0.2567 0.047 Uiso 0.2004(16) 1 calc PR A 2 C4D C 0.4871(10) 0.2524(8) -0.1228(8) 0.034(2) Uani 0.2004(16) 1 d PD A 2 H4DA H 0.4304 0.1825 -0.1820 0.041 Uiso 0.2004(16) 1 calc PR A 2 H4DB H 0.5650 0.2197 -0.0537 0.041 Uiso 0.2004(16) 1 calc PR A 2 C5D C 0.3239(14) 0.2621(10) -0.0031(12) 0.047(3) Uani 0.2004(16) 1 d PD A 2 H5DA H 0.2577 0.3174 0.0088 0.070 Uiso 0.2004(16) 1 calc PR A 2 H5DB H 0.3984 0.2475 0.0763 0.070 Uiso 0.2004(16) 1 calc PR A 2 H5DC H 0.2693 0.1827 -0.0431 0.070 Uiso 0.2004(16) 1 calc PR A 2 O1B O 0.76281(17) 0.37188(14) 0.21068(15) 0.0234(4) Uani 0.766(2) 1 d PD B 1 N1B N 0.88767(19) 0.23746(17) 0.34781(17) 0.0220(4) Uani 0.766(2) 1 d PD B 1 C1B C 0.7901(3) 0.2599(3) 0.2428(3) 0.0172(6) Uani 0.766(2) 1 d PD B 1 C2B C 0.7182(2) 0.1421(2) 0.1662(2) 0.0232(5) Uani 0.766(2) 1 d PD B 1 H2BA H 0.7278 0.1433 0.0864 0.028 Uiso 0.766(2) 1 calc PR B 1 H2BB H 0.6140 0.1295 0.1520 0.028 Uiso 0.766(2) 1 calc PR B 1 C3B C 0.7993(5) 0.0421(3) 0.2418(4) 0.0347(9) Uani 0.766(2) 1 d PD B 1 H3BA H 0.8603 0.0066 0.2034 0.042 Uiso 0.766(2) 1 calc PR B 1 H3BB H 0.7305 -0.0256 0.2492 0.042 Uiso 0.766(2) 1 calc PR B 1 C4B C 0.8945(3) 0.1052(2) 0.3681(2) 0.0282(5) Uani 0.766(2) 1 d PD B 1 H4BA H 0.8551 0.0807 0.4299 0.034 Uiso 0.766(2) 1 calc PR B 1 H4BB H 0.9954 0.0837 0.3950 0.034 Uiso 0.766(2) 1 calc PR B 1 C5B C 0.9694(3) 0.3317(3) 0.4444(2) 0.0325(6) Uani 0.766(2) 1 d PD B 1 H5BA H 0.9573 0.4143 0.4119 0.049 Uiso 0.766(2) 1 calc PR B 1 H5BB H 1.0724 0.3187 0.4762 0.049 Uiso 0.766(2) 1 calc PR B 1 H5BC H 0.9339 0.3258 0.5104 0.049 Uiso 0.766(2) 1 calc PR B 1 O1C O 0.7277(7) 0.3031(8) 0.1676(7) 0.0502(19) Uani 0.234(2) 1 d PD B 2 N1C N 0.8390(6) 0.1564(6) 0.2953(6) 0.0299(16) Uani 0.234(2) 1 d PD B 2 C1C C 0.8213(14) 0.2711(11) 0.2736(11) 0.046(4) Uani 0.234(2) 1 d PD B 2 C2C C 0.8956(9) 0.3585(7) 0.3842(8) 0.035(2) Uani 0.234(2) 1 d PD B 2 H2CA H 0.8247 0.3921 0.4127 0.042 Uiso 0.234(2) 1 calc PR B 2 H2CB H 0.9552 0.4284 0.3681 0.042 Uiso 0.234(2) 1 calc PR B 2 C3C C 0.9915(9) 0.2730(8) 0.4780(8) 0.035(2) Uani 0.234(2) 1 d PD B 2 H3CA H 1.0941 0.2890 0.4879 0.042 Uiso 0.234(2) 1 calc PR B 2 H3CB H 0.9856 0.2860 0.5586 0.042 Uiso 0.234(2) 1 calc PR B 2 C4C C 0.9289(9) 0.1430(7) 0.4233(7) 0.0299(19) Uani 0.234(2) 1 d PD B 2 H4CA H 1.0073 0.0908 0.4304 0.036 Uiso 0.234(2) 1 calc PR B 2 H4CB H 0.8697 0.1039 0.4657 0.036 Uiso 0.234(2) 1 calc PR B 2 C5C C 0.7662(17) 0.0509(14) 0.2132(15) 0.052(5) Uani 0.234(2) 1 d PD B 2 H5CA H 0.7223 0.0779 0.1299 0.079 Uiso 0.234(2) 1 calc PR B 2 H5CB H 0.6903 0.0104 0.2367 0.079 Uiso 0.234(2) 1 calc PR B 2 H5CC H 0.8361 -0.0080 0.2167 0.079 Uiso 0.234(2) 1 calc PR B 2 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 0.01682(5) 0.01616(5) 0.01804(5) -0.00043(3) 0.00613(4) 0.00220(3) Cl1 0.0304(2) 0.0410(2) 0.0289(2) -0.01403(18) 0.01535(18) -0.00474(18) Cl2 0.02646(19) 0.01669(16) 0.0325(2) 0.00235(15) 0.00917(17) -0.00068(14) Cl3 0.0348(2) 0.02160(17) 0.02034(18) 0.00301(14) 0.01362(16) 0.00144(15) Cl4 0.01841(17) 0.02715(19) 0.0342(2) -0.00611(16) 0.01256(16) -0.00102(15) C1 0.0168(6) 0.0193(7) 0.0175(7) 0.0042(5) 0.0062(6) 0.0024(5) C2 0.0224(7) 0.0251(8) 0.0192(7) 0.0017(6) 0.0055(6) 0.0000(6) C3 0.0203(7) 0.0390(9) 0.0177(7) 0.0044(7) 0.0038(6) 0.0001(7) C4 0.0186(7) 0.0386(9) 0.0211(8) 0.0127(7) 0.0075(6) 0.0081(7) C5 0.0181(7) 0.0267(8) 0.0218(7) 0.0099(6) 0.0101(6) 0.0072(6) C6 0.0273(8) 0.0259(8) 0.0328(9) 0.0141(7) 0.0165(7) 0.0130(7) C7 0.0320(8) 0.0179(7) 0.0374(9) 0.0069(7) 0.0215(8) 0.0080(6) C8 0.0208(7) 0.0188(7) 0.0280(8) 0.0018(6) 0.0126(6) 0.0008(6) C9 0.0162(6) 0.0173(7) 0.0209(7) 0.0044(6) 0.0082(6) 0.0021(5) C10 0.0162(6) 0.0190(7) 0.0191(7) 0.0051(5) 0.0096(6) 0.0032(5) O1A 0.0242(8) 0.0397(9) 0.0292(8) 0.0117(7) 0.0041(6) -0.0035(7) N1A 0.0283(9) 0.0313(9) 0.0180(8) 0.0025(7) 0.0068(7) 0.0008(8) C1A 0.0267(11) 0.0249(10) 0.0226(10) 0.0047(8) 0.0070(9) 0.0030(9) C2A 0.0290(12) 0.0409(14) 0.0273(12) 0.0116(10) 0.0066(10) -0.0043(11) C3A 0.0254(11) 0.0436(14) 0.0369(13) -0.0008(11) 0.0103(10) -0.0014(10) C4A 0.0258(10) 0.0286(11) 0.0261(11) 0.0002(9) 0.0032(9) 0.0015(9) C5A 0.0425(14) 0.0487(15) 0.0223(12) 0.0049(11) 0.0160(11) -0.0008(12) O1D 0.046(4) 0.029(3) 0.053(4) 0.022(3) 0.037(3) 0.021(3) N1D 0.024(3) 0.023(3) 0.027(4) 0.005(3) 0.015(3) 0.005(3) C1D 0.028(4) 0.021(4) 0.030(4) 0.008(3) 0.019(4) -0.002(3) C2D 0.043(5) 0.049(6) 0.026(5) 0.013(5) 0.026(4) 0.003(5) C3D 0.037(5) 0.041(5) 0.043(6) -0.008(5) 0.022(5) 0.000(4) C4D 0.037(5) 0.041(5) 0.029(5) -0.006(4) 0.016(4) 0.012(4) C5D 0.058(7) 0.033(6) 0.071(8) 0.019(5) 0.046(7) 0.015(5) O1B 0.0234(8) 0.0179(7) 0.0247(8) 0.0014(6) 0.0051(7) 0.0007(6) N1B 0.0179(8) 0.0289(10) 0.0192(9) 0.0033(8) 0.0075(7) 0.0016(7) C1B 0.0130(12) 0.0199(11) 0.0206(12) 0.0019(9) 0.0086(10) 0.0009(9) C2B 0.0222(10) 0.0240(10) 0.0222(10) -0.0022(8) 0.0085(8) -0.0016(8) C3B 0.0394(19) 0.0203(14) 0.049(2) 0.0064(13) 0.0208(15) 0.0073(12) C4B 0.0271(12) 0.0310(13) 0.0310(14) 0.0154(11) 0.0137(11) 0.0120(10) C5B 0.0262(13) 0.0457(16) 0.0198(12) -0.0058(11) 0.0046(10) -0.0030(12) O1C 0.043(4) 0.076(6) 0.046(4) 0.016(4) 0.030(3) 0.021(4) N1C 0.019(3) 0.042(4) 0.032(4) -0.001(3) 0.015(3) 0.001(3) C1C 0.017(5) 0.072(9) 0.055(10) 0.014(7) 0.023(6) 0.003(5) C2C 0.037(4) 0.021(4) 0.060(6) 0.010(4) 0.033(4) 0.001(3) C3C 0.026(4) 0.051(6) 0.033(5) 0.010(4) 0.017(4) 0.010(4) C4C 0.029(4) 0.033(5) 0.030(5) 0.009(4) 0.013(4) 0.008(4) C5C 0.036(7) 0.068(10) 0.052(8) -0.041(7) 0.022(6) -0.014(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 Te C1 2.1732(14) . ? Te Cl1 2.5091(4) . ? Te Cl4 2.5176(4) . ? Te Cl2 2.5298(4) . ? Te Cl3 2.5448(4) . ? C1 C2 1.374(2) . ? C1 C10 1.435(2) . ? C2 C3 1.411(2) . ? C2 H2A 0.9500 . ? C3 C4 1.357(2) . ? C3 H3A 0.9500 . ? C4 C5 1.416(2) . ? C4 H4A 0.9500 . ? C5 C6 1.428(2) . ? C5 C10 1.437(2) . ? C6 C7 1.358(2) . ? C6 H6A 0.9500 . ? C7 C8 1.408(2) . ? C7 H7A 0.9500 . ? C8 C9 1.377(2) . ? C8 H8A 0.9500 . ? C9 C10 1.420(2) . ? C9 H9A 0.9500 . ? O1A C1A 1.271(3) . ? N1A C1A 1.308(3) . ? N1A C5A 1.457(3) . ? N1A C4A 1.458(3) . ? C1A C2A 1.504(3) . ? C2A C3A 1.517(3) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.529(3) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? O1D C1D 1.280(9) . ? N1D C1D 1.274(9) . ? N1D C5D 1.462(10) . ? N1D C4D 1.473(9) . ? C1D C2D 1.509(10) . ? C2D C3D 1.491(12) . ? C2D H2DA 0.9900 . ? C2D H2DB 0.9900 . ? C3D C4D 1.534(11) . ? C3D H3DA 0.9900 . ? C3D H3DB 0.9900 . ? C4D H4DA 0.9900 . ? C4D H4DB 0.9900 . ? C5D H5DA 0.9800 . ? C5D H5DB 0.9800 . ? C5D H5DC 0.9800 . ? O1B C1B 1.299(3) . ? N1B C1B 1.301(3) . ? N1B C5B 1.449(3) . ? N1B C4B 1.459(3) . ? C1B C2B 1.498(4) . ? C2B C3B 1.510(4) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.537(5) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C4B H4BA 0.9900 . ? C4B H4BB 0.9900 . ? C5B H5BA 0.9800 . ? C5B H5BB 0.9800 . ? C5B H5BC 0.9800 . ? O1C C1C 1.325(11) . ? N1C C1C 1.287(12) . ? N1C C5C 1.427(12) . ? N1C C4C 1.458(9) . ? C1C C2C 1.497(13) . ? C2C C3C 1.552(10) . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C4C 1.509(11) . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C H4CA 0.9900 . ? C4C H4CB 0.9900 . ? C5C H5CA 0.9800 . ? C5C H5CB 0.9800 . ? C5C H5CC 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 Cl1 89.58(4) . . ? C1 Te Cl4 89.97(4) . . ? Cl1 Te Cl4 88.658(14) . . ? C1 Te Cl2 88.83(4) . . ? Cl1 Te Cl2 88.924(14) . . ? Cl4 Te Cl2 177.308(14) . . ? C1 Te Cl3 91.89(4) . . ? Cl1 Te Cl3 177.178(13) . . ? Cl4 Te Cl3 93.753(14) . . ? Cl2 Te Cl3 88.696(14) . . ? C2 C1 C10 121.04(14) . . ? C2 C1 Te 113.82(11) . . ? C10 C1 Te 125.13(11) . . ? C1 C2 C3 121.11(15) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C4 C3 C2 119.86(15) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 120.99(15) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 120.39(14) . . ? C4 C5 C10 120.43(15) . . ? C6 C5 C10 119.18(15) . . ? C7 C6 C5 121.29(15) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C8 119.96(15) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.65(15) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 121.46(14) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C9 C10 C1 125.98(13) . . ? C9 C10 C5 117.45(13) . . ? C1 C10 C5 116.57(14) . . ? C1A N1A C5A 124.02(19) . . ? C1A N1A C4A 113.40(18) . . ? C5A N1A C4A 122.44(18) . . ? O1A C1A N1A 123.2(2) . . ? O1A C1A C2A 126.7(2) . . ? N1A C1A C2A 110.1(2) . . ? C1A C2A C3A 103.2(2) . . ? C1A C2A H2AA 111.1 . . ? C3A C2A H2AA 111.1 . . ? C1A C2A H2AB 111.1 . . ? C3A C2A H2AB 111.1 . . ? H2AA C2A H2AB 109.1 . . ? C2A C3A C4A 104.31(19) . . ? C2A C3A H3AA 110.9 . . ? C4A C3A H3AA 110.9 . . ? C2A C3A H3AB 110.9 . . ? C4A C3A H3AB 110.9 . . ? H3AA C3A H3AB 108.9 . . ? N1A C4A C3A 103.22(18) . . ? N1A C4A H4AA 111.1 . . ? C3A C4A H4AA 111.1 . . ? N1A C4A H4AB 111.1 . . ? C3A C4A H4AB 111.1 . . ? H4AA C4A H4AB 109.1 . . ? C1D N1D C5D 124.9(7) . . ? C1D N1D C4D 112.7(7) . . ? C5D N1D C4D 121.2(7) . . ? N1D C1D O1D 122.9(7) . . ? N1D C1D C2D 109.9(7) . . ? O1D C1D C2D 127.2(7) . . ? C3D C2D C1D 104.9(7) . . ? C3D C2D H2DA 110.8 . . ? C1D C2D H2DA 110.8 . . ? C3D C2D H2DB 110.8 . . ? C1D C2D H2DB 110.8 . . ? H2DA C2D H2DB 108.8 . . ? C2D C3D C4D 102.4(7) . . ? C2D C3D H3DA 111.3 . . ? C4D C3D H3DA 111.3 . . ? C2D C3D H3DB 111.3 . . ? C4D C3D H3DB 111.3 . . ? H3DA C3D H3DB 109.2 . . ? N1D C4D C3D 103.3(7) . . ? N1D C4D H4DA 111.1 . . ? C3D C4D H4DA 111.1 . . ? N1D C4D H4DB 111.1 . . ? C3D C4D H4DB 111.1 . . ? H4DA C4D H4DB 109.1 . . ? N1D C5D H5DA 109.5 . . ? N1D C5D H5DB 109.5 . . ? H5DA C5D H5DB 109.5 . . ? N1D C5D H5DC 109.5 . . ? H5DA C5D H5DC 109.5 . . ? H5DB C5D H5DC 109.5 . . ? C1B N1B C5B 124.5(2) . . ? C1B N1B C4B 113.6(2) . . ? C5B N1B C4B 121.3(2) . . ? O1B C1B N1B 122.7(3) . . ? O1B C1B C2B 125.7(3) . . ? N1B C1B C2B 111.6(2) . . ? C1B C2B C3B 103.6(2) . . ? C1B C2B H2BA 111.0 . . ? C3B C2B H2BA 111.0 . . ? C1B C2B H2BB 111.0 . . ? C3B C2B H2BB 111.0 . . ? H2BA C2B H2BB 109.0 . . ? C2B C3B C4B 106.4(3) . . ? C2B C3B H3BA 110.5 . . ? C4B C3B H3BA 110.5 . . ? C2B C3B H3BB 110.5 . . ? C4B C3B H3BB 110.5 . . ? H3BA C3B H3BB 108.6 . . ? N1B C4B C3B 103.2(2) . . ? N1B C4B H4BA 111.1 . . ? C3B C4B H4BA 111.1 . . ? N1B C4B H4BB 111.1 . . ? C3B C4B H4BB 111.1 . . ? H4BA C4B H4BB 109.1 . . ? C1C N1C C5C 126.3(10) . . ? C1C N1C C4C 111.4(8) . . ? C5C N1C C4C 121.7(9) . . ? N1C C1C O1C 121.5(11) . . ? N1C C1C C2C 113.4(9) . . ? O1C C1C C2C 124.3(10) . . ? C1C C2C C3C 102.1(7) . . ? C1C C2C H2CA 111.4 . . ? C3C C2C H2CA 111.4 . . ? C1C C2C H2CB 111.4 . . ? C3C C2C H2CB 111.4 . . ? H2CA C2C H2CB 109.2 . . ? C4C C3C C2C 104.1(6) . . ? C4C C3C H3CA 110.9 . . ? C2C C3C H3CA 110.9 . . ? C4C C3C H3CB 110.9 . . ? C2C C3C H3CB 110.9 . . ? H3CA C3C H3CB 108.9 . . ? N1C C4C C3C 106.0(6) . . ? N1C C4C H4CA 110.5 . . ? C3C C4C H4CA 110.5 . . ? N1C C4C H4CB 110.5 . . ? C3C C4C H4CB 110.5 . . ? H4CA C4C H4CB 108.7 . . ? N1C C5C H5CA 109.5 . . ? N1C C5C H5CB 109.5 . . ? H5CA C5C H5CB 109.5 . . ? N1C C5C H5CC 109.5 . . ? H5CA C5C H5CC 109.5 . . ? H5CB C5C H5CC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Te C1 C2 43.62(11) . . . . ? Cl4 Te C1 C2 132.28(11) . . . . ? Cl2 Te C1 C2 -45.31(11) . . . . ? Cl3 Te C1 C2 -133.97(11) . . . . ? Cl1 Te C1 C10 -134.98(12) . . . . ? Cl4 Te C1 C10 -46.33(12) . . . . ? Cl2 Te C1 C10 136.08(12) . . . . ? Cl3 Te C1 C10 47.43(12) . . . . ? C10 C1 C2 C3 0.3(2) . . . . ? Te C1 C2 C3 -178.32(12) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C2 C3 C4 C5 -1.0(2) . . . . ? C3 C4 C5 C6 -179.80(14) . . . . ? C3 C4 C5 C10 0.3(2) . . . . ? C4 C5 C6 C7 179.07(15) . . . . ? C10 C5 C6 C7 -1.0(2) . . . . ? C5 C6 C7 C8 -0.2(2) . . . . ? C6 C7 C8 C9 0.9(2) . . . . ? C7 C8 C9 C10 -0.4(2) . . . . ? C8 C9 C10 C1 179.96(14) . . . . ? C8 C9 C10 C5 -0.7(2) . . . . ? C2 C1 C10 C9 178.29(14) . . . . ? Te C1 C10 C9 -3.2(2) . . . . ? C2 C1 C10 C5 -1.0(2) . . . . ? Te C1 C10 C5 177.49(10) . . . . ? C4 C5 C10 C9 -178.64(14) . . . . ? C6 C5 C10 C9 1.4(2) . . . . ? C4 C5 C10 C1 0.7(2) . . . . ? C6 C5 C10 C1 -179.22(13) . . . . ? C5A N1A C1A O1A 3.5(4) . . . . ? C4A N1A C1A O1A 179.3(2) . . . . ? C5A N1A C1A C2A -174.9(2) . . . . ? C4A N1A C1A C2A 0.8(3) . . . . ? O1A C1A C2A C3A 166.2(2) . . . . ? N1A C1A C2A C3A -15.4(3) . . . . ? C1A C2A C3A C4A 22.8(3) . . . . ? C1A N1A C4A C3A 14.0(3) . . . . ? C5A N1A C4A C3A -170.1(2) . . . . ? C2A C3A C4A N1A -22.4(2) . . . . ? C5D N1D C1D O1D 8.3(15) . . . . ? C4D N1D C1D O1D 175.9(8) . . . . ? C5D N1D C1D C2D -171.5(10) . . . . ? C4D N1D C1D C2D -3.8(10) . . . . ? N1D C1D C2D C3D -13.4(11) . . . . ? O1D C1D C2D C3D 166.9(9) . . . . ? C1D C2D C3D C4D 23.4(10) . . . . ? C1D N1D C4D C3D 18.9(10) . . . . ? C5D N1D C4D C3D -173.0(9) . . . . ? C2D C3D C4D N1D -25.2(10) . . . . ? C5B N1B C1B O1B 4.8(5) . . . . ? C4B N1B C1B O1B 176.5(3) . . . . ? C5B N1B C1B C2B -176.2(2) . . . . ? C4B N1B C1B C2B -4.5(4) . . . . ? O1B C1B C2B C3B 174.9(4) . . . . ? N1B C1B C2B C3B -4.1(4) . . . . ? C1B C2B C3B C4B 10.3(4) . . . . ? C1B N1B C4B C3B 10.8(4) . . . . ? C5B N1B C4B C3B -177.2(3) . . . . ? C2B C3B C4B N1B -12.6(4) . . . . ? C5C N1C C1C O1C 1(2) . . . . ? C4C N1C C1C O1C -170.7(11) . . . . ? C5C N1C C1C C2C 170.8(11) . . . . ? C4C N1C C1C C2C -0.5(14) . . . . ? N1C C1C C2C C3C 10.9(13) . . . . ? O1C C1C C2C C3C -179.3(12) . . . . ? C1C C2C C3C C4C -16.0(10) . . . . ? C1C N1C C4C C3C -10.5(11) . . . . ? C5C N1C C4C C3C 177.6(10) . . . . ? C2C C3C C4C N1C 16.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.621 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.081 # Attachment '- Compound 6.CIF' data_aksc-sm4 _database_code_depnum_ccdc_archive 'CCDC 825840' #TrackingRef '- Compound 6.CIF' _audit_creation_method 'Created with Diamond (www.crystalimpact.com)' _audit_creation_date 11-01-31 _audit_update_record 11-01-31 _chemical_formula_sum 'C12 H16 Br2 N2 O4 Te' _chemical_formula_weight 539.690 _refine_ls_R_factor_all 0.054 _cell_length_a 28.4093(10) _cell_length_b 9.5781(2) _cell_length_c 13.1483(4) _cell_angle_alpha 90.000 _cell_angle_beta 112.596(4) _cell_angle_gamma 90.000 _cell_volume 3303.1(2) _cell_formula_units_Z 8 _symmetry_int_tables_number 15 _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -C_2yc loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x, y, z' 2 '-x, y, 0.500-z' 3 '-x, -y, -z' 4 'x, -y, 0.500+z' 5 '0.500+x, 0.500+y, z' 6 '0.500-x, 0.500+y, 0.500-z' 7 '0.500-x, 0.500-y, -z' 8 '0.500+x, 0.500-y, 0.500+z' loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_radius_bond Te ? 1.200 Br ? 1.200 O ? 1.200 N ? 1.200 C ? 1.200 H ? 1.200 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_attached_hydrogens _atom_site_calc_flag _atom_site_thermal_displace_type _atom_site_u_iso_or_equiv Te Te 0.6377(0) 0.2104(0) 0.3594(0) 1.000 8 f ? d Uani 0.01973(6) Br1 Br 0.6985(0) 0.4045(0) 0.4866(0) 1.000 8 f ? d Uani 0.03094(8) Br2 Br 0.5713(0) 0.0281(0) 0.2249(0) 1.000 8 f ? d Uani 0.03978(9) O1A O 0.5988(1) 0.3691(2) 0.5913(2) 1.000 8 f ? d Uani 0.0315(4) O2A O 0.6817(1) 0.0349(2) 0.5531(2) 1.000 8 f ? d Uani 0.0252(4) O1B O 0.5098(1) 0.3760(3) 0.1394(2) 1.000 8 f ? d Uani 0.0601(8) O2B O 0.6556(1) 0.2782(2) 0.1679(2) 1.000 8 f ? d Uani 0.0305(4) N1A N 0.6583(1) 0.2015(2) 0.6516(2) 1.000 8 f ? d Uani 0.0199(4) N1B N 0.5693(1) 0.3153(2) 0.0740(2) 1.000 8 f ? d Uani 0.0258(5) C1A C 0.5938(1) 0.1926(3) 0.4611(2) 1.000 8 f ? d Uani 0.0232(5) H1AA H 0.5595 0.2323 0.4204 1.000 8 f ? calc Uiso 0.02800 H1AB H 0.5894 0.0923 0.4735 1.000 8 f ? calc Uiso 0.02800 C2A C 0.6167(1) 0.2639(3) 0.5709(2) 1.000 8 f ? d Uani 0.0220(5) C3A C 0.6879(1) 0.0922(3) 0.6394(2) 1.000 8 f ? d Uani 0.0214(5) C4A C 0.7292(1) 0.0638(3) 0.7496(2) 1.000 8 f ? d Uani 0.0280(6) H4AA H 0.7629 0.0898 0.7493 1.000 8 f ? calc Uiso 0.03400 H4AB H 0.7299 -0.0365 0.7684 1.000 8 f ? calc Uiso 0.03400 C5A C 0.7168(1) 0.1530(3) 0.8326(2) 1.000 8 f ? d Uani 0.0344(7) H5AA H 0.7019 0.0949 0.8749 1.000 8 f ? calc Uiso 0.04100 H5AB H 0.7479 0.1990 0.8847 1.000 8 f ? calc Uiso 0.04100 C6A C 0.6783(1) 0.2615(3) 0.7634(2) 1.000 8 f ? d Uani 0.0261(6) H6AA H 0.6507 0.2750 0.7908 1.000 8 f ? calc Uiso 0.03100 H6AB H 0.6952 0.3524 0.7646 1.000 8 f ? calc Uiso 0.03100 C1B C 0.5939(1) 0.3843(3) 0.2689(2) 1.000 8 f ? d Uani 0.0256(6) H1BA H 0.5772 0.4284 0.3144 1.000 8 f ? calc Uiso 0.03100 H1BB H 0.6179 0.4537 0.2602 1.000 8 f ? calc Uiso 0.03100 C2B C 0.5539(1) 0.3565(3) 0.1579(2) 1.000 8 f ? d Uani 0.0302(6) C3B C 0.6178(1) 0.2857(3) 0.0818(2) 1.000 8 f ? d Uani 0.0248(5) C4B C 0.6159(1) 0.2635(3) -0.0323(2) 1.000 8 f ? d Uani 0.0314(6) H4BA H 0.6296 0.1704 -0.0388 1.000 8 f ? calc Uiso 0.03800 H4BB H 0.6362 0.3356 -0.0511 1.000 8 f ? calc Uiso 0.03800 C5B C 0.5605(1) 0.2740(4) -0.1072(3) 1.000 8 f ? d Uani 0.0451(8) H5BA H 0.5555 0.3510 -0.1606 1.000 8 f ? calc Uiso 0.05400 H5BB H 0.5491 0.1859 -0.1488 1.000 8 f ? calc Uiso 0.05400 C6B C 0.5315(1) 0.3006(6) -0.0393(3) 1.000 8 f ? d Uani 0.0644(13) H6BA H 0.5081 0.2220 -0.0443 1.000 8 f ? calc Uiso 0.07700 H6BB H 0.5112 0.3872 -0.0632 1.000 8 f ? calc Uiso 0.07700 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te 0.02748(10) 0.01669(9) 0.01669(9) 0.00226(7) 0.01036(7) -0.00110(6) Br1 0.02900(15) 0.03599(17) 0.02336(14) -0.00889(12) 0.00511(11) -0.00441(11) Br2 0.0685(2) 0.02435(16) 0.02948(16) -0.01947(15) 0.02220(15) -0.00993(12) O1A 0.0346(11) 0.0296(11) 0.029(1) 0.0135(9) 0.0107(8) -0.0039(8) O2A 0.0295(10) 0.0222(10) 0.027(1) 0.0066(8) 0.0142(8) 0.0014(8) O1B 0.0253(11) 0.122(2) 0.0333(13) -0.0017(13) 0.0118(10) -0.0069(14) O2B 0.0243(9) 0.0393(12) 0.0268(10) -0.0012(9) 0.0085(8) 0.0006(9) N1A 0.0238(10) 0.0229(11) 0.0141(10) 0.0031(9) 0.0083(8) 0.0019(8) N1B 0.0245(11) 0.0352(14) 0.015(1) -0.003(1) 0.0046(9) 0.0019(9) C1A 0.0248(13) 0.0279(14) 0.0190(12) 0.0034(11) 0.0105(10) -0.0002(10) C2A 0.0220(12) 0.0264(14) 0.0205(12) 0.004(1) 0.0114(10) 0.0009(10) C3A 0.0217(12) 0.0207(13) 0.0255(13) 0.0003(10) 0.013(1) 0.0047(10) C4A 0.0241(13) 0.0330(15) 0.0250(14) 0.0065(12) 0.0074(11) 0.0051(11) C5A 0.0320(15) 0.0461(19) 0.0202(14) 0.0066(14) 0.0045(11) 0.0047(13) C6A 0.0304(14) 0.0306(14) 0.0188(12) -0.0019(12) 0.0111(11) -0.0016(11) C1B 0.0323(14) 0.0203(13) 0.0204(13) 0.0006(11) 0.0061(11) 0.0012(10) C2B 0.0273(14) 0.0415(17) 0.0207(13) -0.0009(13) 0.0080(11) 0.0050(12) C3B 0.0317(14) 0.0203(13) 0.0238(13) -0.0052(11) 0.0121(11) 0.0032(10) C4B 0.0399(16) 0.0356(16) 0.0228(14) 0.0018(13) 0.0165(12) 0.0027(12) C5B 0.057(2) 0.050(2) 0.0262(16) 0.0113(17) 0.0139(15) -0.0056(14) C6B 0.0326(17) 0.133(4) 0.0213(16) 0.007(2) 0.0027(13) -0.005(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Te C1B . . 2.145(3) no Te C1A . . 2.159(2) no Te Br1 . . 2.6488(3) no Te Br2 . . 2.6784(3) no Te O2B . . 2.8291(19) no Te O2A . . 2.9036(18) no O1A C2A . . 1.205(3) no O2A C3A . . 1.211(3) no O1B C2B . . 1.196(3) no O2B C3B . . 1.227(3) no N1A C2A . . 1.384(3) no N1A C3A . . 1.390(3) no N1A C6A . . 1.475(3) no N1B C3B . . 1.372(3) no N1B C2B . . 1.391(4) no N1B C6B . . 1.470(4) no C1A C2A . . 1.501(3) no C1A H1AA . . 0.9900 no C1A H1AB . . 0.9900 no C3A C4A . . 1.498(4) no C4A C5A . . 1.530(4) no C4A H4AA . . 0.9900 no C4A H4AB . . 0.9900 no C5A C6A . . 1.529(4) no C5A H5AA . . 0.9900 no C5A H5AB . . 0.9900 no C6A H6AA . . 0.9900 no C6A H6AB . . 0.9900 no C1B C2B . . 1.489(4) no C1B H1BA . . 0.9900 no C1B H1BB . . 0.9900 no C3B C4B . . 1.495(4) no C4B C5B . . 1.505(4) no C4B H4BA . . 0.9900 no C4B H4BB . . 0.9900 no C5B C6B . . 1.452(5) no C5B H5BA . . 0.9900 no C5B H5BB . . 0.9900 no C6B H6BA . . 0.9900 no C6B H6BB . . 0.9900 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1B Te C1A . . . 93.12(11) no C1B Te Br1 . . . 84.50(7) no C1A Te Br1 . . . 93.22(7) no C1B Te Br2 . . . 91.63(7) no C1A Te Br2 . . . 85.93(7) no Br1 Te Br2 . . . 175.99(1) no C1B Te O2B . . . 65.96(9) no C1A Te O2B . . . 156.06(8) no Br1 Te O2B . . . 96.02(4) no Br2 Te O2B . . . 83.32(4) no C1B Te O2A . . . 153.97(8) no C1A Te O2A . . . 64.35(8) no Br1 Te O2A . . . 84.01(4) no Br2 Te O2A . . . 99.12(4) no O2B Te O2A . . . 138.58(5) no C3A O2A Te . . . 114.73(16) no C3B O2B Te . . . 116.22(17) no C2A N1A C3A . . . 127.8(2) no C2A N1A C6A . . . 119.0(2) no C3A N1A C6A . . . 112.9(2) no C3B N1B C2B . . . 127.7(2) no C3B N1B C6B . . . 112.2(2) no C2B N1B C6B . . . 120.1(2) no C2A C1A Te . . . 114.80(17) no C2A C1A H1AA . . . 108.60 no Te C1A H1AA . . . 108.60 no C2A C1A H1AB . . . 108.60 no Te C1A H1AB . . . 108.60 no H1AA C1A H1AB . . . 107.50 no O1A C2A N1A . . . 120.0(2) no O1A C2A C1A . . . 122.0(2) no N1A C2A C1A . . . 117.9(2) no O2A C3A N1A . . . 125.0(2) no O2A C3A C4A . . . 127.0(2) no N1A C3A C4A . . . 108.0(2) no C3A C4A C5A . . . 106.2(2) no C3A C4A H4AA . . . 110.50 no C5A C4A H4AA . . . 110.50 no C3A C4A H4AB . . . 110.50 no C5A C4A H4AB . . . 110.50 no H4AA C4A H4AB . . . 108.70 no C6A C5A C4A . . . 105.3(2) no C6A C5A H5AA . . . 110.70 no C4A C5A H5AA . . . 110.70 no C6A C5A H5AB . . . 110.70 no C4A C5A H5AB . . . 110.70 no H5AA C5A H5AB . . . 108.80 no N1A C6A C5A . . . 104.0(2) no N1A C6A H6AA . . . 111.00 no C5A C6A H6AA . . . 111.00 no N1A C6A H6AB . . . 111.00 no C5A C6A H6AB . . . 111.00 no H6AA C6A H6AB . . . 109.00 no C2B C1B Te . . . 117.79(19) no C2B C1B H1BA . . . 107.90 no Te C1B H1BA . . . 107.90 no C2B C1B H1BB . . . 107.90 no Te C1B H1BB . . . 107.90 no H1BA C1B H1BB . . . 107.20 no O1B C2B N1B . . . 120.4(3) no O1B C2B C1B . . . 121.1(3) no N1B C2B C1B . . . 118.3(2) no O2B C3B N1B . . . 125.4(2) no O2B C3B C4B . . . 126.8(3) no N1B C3B C4B . . . 107.8(2) no C3B C4B C5B . . . 105.8(2) no C3B C4B H4BA . . . 110.60 no C5B C4B H4BA . . . 110.60 no C3B C4B H4BB . . . 110.60 no C5B C4B H4BB . . . 110.60 no H4BA C4B H4BB . . . 108.70 no C6B C5B C4B . . . 107.9(3) no C6B C5B H5BA . . . 110.10 no C4B C5B H5BA . . . 110.10 no C6B C5B H5BB . . . 110.10 no C4B C5B H5BB . . . 110.10 no H5BA C5B H5BB . . . 108.40 no C5B C6B N1B . . . 105.9(3) no C5B C6B H6BA . . . 110.60 no N1B C6B H6BA . . . 110.60 no C5B C6B H6BB . . . 110.60 no N1B C6B H6BB . . . 110.60 no H6BA C6B H6BB . . . 108.70 no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C1B Te O2A C3A . . . . -24.1(3) no C1A Te O2A C3A . . . . -56.36(18) no Br1 Te O2A C3A . . . . 40.13(17) no Br2 Te O2A C3A . . . . -137.34(17) no O2B Te O2A C3A . . . . 132.45(17) no C1B Te O2B C3B . . . . -53.0(2) no C1A Te O2B C3B . . . . -22.1(3) no Br1 Te O2B C3B . . . . -134.23(19) no Br2 Te O2B C3B . . . . 41.79(19) no O2A Te O2B C3B . . . . 138.01(18) no C1B Te C1A C2A . . . . -96.48(19) no Br1 Te C1A C2A . . . . -11.82(18) no Br2 Te C1A C2A . . . . 172.11(19) no O2B Te C1A C2A . . . . -124.5(2) no O2A Te C1A C2A . . . . 69.96(18) no C3A N1A C2A O1A . . . . -170.7(3) no C6A N1A C2A O1A . . . . 3.2(4) no C3A N1A C2A C1A . . . . 12.2(4) no C6A N1A C2A C1A . . . . -173.9(2) no Te C1A C2A O1A . . . . 108.5(3) no Te C1A C2A N1A . . . . -74.5(3) no Te O2A C3A N1A . . . . 29.1(3) no Te O2A C3A C4A . . . . -148.0(2) no C2A N1A C3A O2A . . . . 1.0(4) no C6A N1A C3A O2A . . . . -173.1(2) no C2A N1A C3A C4A . . . . 178.6(2) no C6A N1A C3A C4A . . . . 4.4(3) no O2A C3A C4A C5A . . . . -174.5(3) no N1A C3A C4A C5A . . . . 8.0(3) no C3A C4A C5A C6A . . . . -16.7(3) no C2A N1A C6A C5A . . . . 170.4(2) no C3A N1A C6A C5A . . . . -14.9(3) no C4A C5A C6A N1A . . . . 18.7(3) no C1A Te C1B C2B . . . . -100.6(2) no Br1 Te C1B C2B . . . . 166.5(2) no Br2 Te C1B C2B . . . . -14.6(2) no O2B Te C1B C2B . . . . 67.4(2) no O2A Te C1B C2B . . . . -129.4(2) no C3B N1B C2B O1B . . . . -178.4(3) no C6B N1B C2B O1B . . . . 2.3(5) no C3B N1B C2B C1B . . . . 5.6(4) no C6B N1B C2B C1B . . . . -173.8(3) no Te C1B C2B O1B . . . . 116.1(3) no Te C1B C2B N1B . . . . -67.9(3) no Te O2B C3B N1B . . . . 25.4(3) no Te O2B C3B C4B . . . . -154.1(2) no C2B N1B C3B O2B . . . . 7.3(4) no C6B N1B C3B O2B . . . . -173.3(3) no C2B N1B C3B C4B . . . . -173.2(3) no C6B N1B C3B C4B . . . . 6.2(4) no O2B C3B C4B C5B . . . . 175.9(3) no N1B C3B C4B C5B . . . . -3.6(3) no C3B C4B C5B C6B . . . . -0.3(4) no C4B C5B C6B N1B . . . . 3.7(4) no C3B N1B C6B C5B . . . . -6.3(4) no C2B N1B C6B C5B . . . . 173.1(3) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C1A H1AA O1B . . 2_655 0.9900 2.2800 3.241(4) 163.40 no C4A H4AA O2B . . 7_656 0.9900 2.4900 3.383(3) 149.60 no C4B H4BA O2A . . 4_554 0.9900 2.4800 3.363(4) 148.60 no C5B H5BB Br2 . . 4_554 0.9900 2.8600 3.723(3) 146.40 no C6B H6BB O1B . . 3_665 0.9900 2.4600 3.394(6) 157.30 no