# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name J.Woollins _publ_contact_author_email jdw3@st-andrews.ac.uk loop_ _publ_author_name F.Knight K.Arachchige R.Randall M.Buhl A.Slawin J.Woollins #============================================================================== data_Ferg-117-B_Off _database_code_depnum_ccdc_archive 'CCDC 850816' #TrackingRef '- 1.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H13 Br I2 Se' _chemical_formula_moiety 'C18 H13 Br I2 Se' _chemical_formula_weight 641.97 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 14.174(7) _cell_length_b 14.165(7) _cell_length_c 9.265(5) _cell_angle_alpha 90.0000 _cell_angle_beta 106.194(10) _cell_angle_gamma 90.0000 _cell_volume 1786.5(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7465 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 29.13 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 2.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184.00 _exptl_absorpt_coefficient_mu 7.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.856 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.257 _diffrn_reflns_number 13238 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3140 _reflns_number_gt 2490 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1936 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3140 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1065P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.810 _refine_diff_density_min -2.050 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Se Se -0.0929 2.2259 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.4742 1.8119 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.82513(5) 0.24505(6) 0.79971(8) 0.0264(3) Uani 1.0 4 d . . . I2 I 0.94094(5) 0.39155(6) 0.96432(8) 0.0303(3) Uani 1.0 4 d . . . Br1 Br 0.60811(8) 0.23355(10) 0.43745(13) 0.0327(4) Uani 1.0 4 d . . . Se1 Se 0.72910(8) 0.07247(9) 0.64783(12) 0.0243(4) Uani 1.0 4 d . . . C1 C 0.6006(8) 0.0533(9) 0.6824(12) 0.023(3) Uani 1.0 4 d . . . C2 C 0.5897(8) -0.0218(10) 0.7715(13) 0.028(3) Uani 1.0 4 d . . . C3 C 0.5027(9) -0.0405(10) 0.8079(13) 0.034(3) Uani 1.0 4 d . . . C4 C 0.4251(8) 0.0170(10) 0.7544(12) 0.026(3) Uani 1.0 4 d . . . C5 C 0.4311(8) 0.0914(9) 0.6623(12) 0.026(3) Uani 1.0 4 d . . . C6 C 0.3428(8) 0.1409(10) 0.6155(12) 0.027(3) Uani 1.0 4 d . . . C7 C 0.3372(8) 0.2183(11) 0.5236(13) 0.031(3) Uani 1.0 4 d . . . C8 C 0.4202(9) 0.2415(9) 0.4737(15) 0.031(3) Uani 1.0 4 d . . . C9 C 0.5054(8) 0.1921(9) 0.5207(12) 0.025(3) Uani 1.0 4 d . . . C10 C 0.5192(8) 0.1127(9) 0.6176(12) 0.023(3) Uani 1.0 4 d . . . C11 C 0.3232(8) 0.0126(10) 0.7777(14) 0.033(3) Uani 1.0 4 d . . . C12 C 0.2679(9) 0.0975(9) 0.6851(13) 0.031(3) Uani 1.0 4 d . . . C13 C 0.8080(7) -0.0082(9) 0.8040(12) 0.024(3) Uani 1.0 4 d . . . C14 C 0.8491(9) -0.0852(10) 0.7610(15) 0.035(3) Uani 1.0 4 d . . . C15 C 0.9044(9) -0.1472(12) 0.8686(15) 0.042(4) Uani 1.0 4 d . . . C16 C 0.9227(9) -0.1227(11) 1.0182(15) 0.043(4) Uani 1.0 4 d . . . C17 C 0.8814(9) -0.0446(10) 1.0613(15) 0.036(4) Uani 1.0 4 d . . . C18 C 0.8244(8) 0.0129(10) 0.9562(13) 0.028(3) Uani 1.0 4 d . . . H2 H 0.6441 -0.0627 0.8097 0.0332 Uiso 1.0 4 calc R . . H3 H 0.4981 -0.0929 0.8695 0.0414 Uiso 1.0 4 calc R . . H7 H 0.2790 0.2553 0.4942 0.0367 Uiso 1.0 4 calc R . . H8 H 0.4162 0.2927 0.4060 0.0369 Uiso 1.0 4 calc R . . H11A H 0.3267 0.0194 0.8854 0.0395 Uiso 1.0 4 calc R . . H11B H 0.2903 -0.0478 0.7400 0.0395 Uiso 1.0 4 calc R . . H12A H 0.2091 0.0758 0.6065 0.0374 Uiso 1.0 4 calc R . . H12B H 0.2473 0.1434 0.7510 0.0374 Uiso 1.0 4 calc R . . H14 H 0.8403 -0.0972 0.6572 0.0421 Uiso 1.0 4 calc R . . H15 H 0.9288 -0.2045 0.8398 0.0509 Uiso 1.0 4 calc R . . H16 H 0.9651 -0.1612 1.0927 0.0514 Uiso 1.0 4 calc R . . H17 H 0.8927 -0.0306 1.1650 0.0428 Uiso 1.0 4 calc R . . H18 H 0.7955 0.0675 0.9858 0.0341 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0208(5) 0.0286(6) 0.0302(5) 0.0003(3) 0.0077(4) -0.0009(4) I2 0.0268(5) 0.0277(6) 0.0351(6) -0.0034(4) 0.0065(4) -0.0023(4) Br1 0.0259(7) 0.0402(9) 0.0308(8) -0.0054(6) 0.0057(6) 0.0100(6) Se1 0.0211(6) 0.0266(8) 0.0251(7) -0.0014(5) 0.0065(5) -0.0019(5) C1 0.024(6) 0.022(7) 0.021(6) 0.001(5) 0.003(5) -0.003(5) C2 0.024(6) 0.029(8) 0.031(7) -0.001(5) 0.008(5) -0.001(6) C3 0.036(7) 0.030(8) 0.030(7) -0.010(6) -0.002(6) 0.013(6) C4 0.025(6) 0.032(8) 0.021(6) 0.001(6) 0.005(5) -0.003(6) C5 0.023(6) 0.027(8) 0.023(6) -0.008(5) -0.003(5) -0.009(6) C6 0.020(5) 0.043(9) 0.015(6) -0.004(6) 0.001(5) -0.015(6) C7 0.022(6) 0.049(9) 0.018(6) 0.009(6) 0.000(5) -0.000(6) C8 0.023(6) 0.027(8) 0.036(8) -0.007(5) -0.004(6) 0.008(6) C9 0.025(6) 0.030(8) 0.023(6) -0.008(6) 0.010(5) -0.005(5) C10 0.021(6) 0.025(8) 0.019(6) -0.005(5) 0.001(5) -0.002(5) C11 0.021(6) 0.041(9) 0.035(7) -0.016(6) 0.007(6) 0.007(6) C12 0.029(6) 0.033(8) 0.029(7) -0.001(6) 0.005(6) -0.009(6) C13 0.013(5) 0.031(8) 0.021(6) -0.002(5) -0.004(5) -0.005(5) C14 0.030(7) 0.038(9) 0.038(7) 0.003(6) 0.011(6) -0.002(7) C15 0.031(7) 0.048(10) 0.049(9) 0.016(7) 0.012(6) 0.012(7) C16 0.024(6) 0.059(11) 0.038(8) 0.008(7) -0.002(6) 0.015(7) C17 0.033(7) 0.039(9) 0.036(8) -0.006(7) 0.012(6) 0.001(7) C18 0.024(6) 0.028(8) 0.031(7) -0.004(6) 0.005(5) 0.003(6) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r6 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r6' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r6' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I1 I2 2.8161(14) yes . . I1 Se1 2.9565(17) yes . . Br1 C9 1.920(13) yes . . Se1 C1 1.954(12) yes . . Se1 C13 1.936(11) yes . . C1 C2 1.382(18) yes . . C1 C10 1.419(15) yes . . C2 C3 1.391(18) yes . . C3 C4 1.346(17) yes . . C4 C5 1.374(18) yes . . C4 C11 1.521(17) yes . . C5 C6 1.394(16) yes . . C5 C10 1.452(17) yes . . C6 C7 1.377(19) yes . . C6 C12 1.518(18) yes . . C7 C8 1.418(19) yes . . C8 C9 1.359(16) yes . . C9 C10 1.418(17) yes . . C11 C12 1.556(18) yes . . C13 C14 1.348(19) yes . . C13 C18 1.396(16) yes . . C14 C15 1.394(19) yes . . C15 C16 1.38(2) yes . . C16 C17 1.36(2) yes . . C17 C18 1.352(17) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I2 I1 Se1 171.32(4) yes . . . I1 Se1 C1 111.3(4) yes . . . I1 Se1 C13 92.2(4) yes . . . C1 Se1 C13 99.6(5) yes . . . Se1 C1 C2 118.0(8) yes . . . Se1 C1 C10 122.3(9) yes . . . C2 C1 C10 119.7(11) yes . . . C1 C2 C3 123.1(11) yes . . . C2 C3 C4 118.9(13) yes . . . C3 C4 C5 120.5(12) yes . . . C3 C4 C11 129.3(12) yes . . . C5 C4 C11 110.2(10) yes . . . C4 C5 C6 111.9(11) yes . . . C4 C5 C10 122.9(10) yes . . . C6 C5 C10 125.1(11) yes . . . C5 C6 C7 119.0(11) yes . . . C5 C6 C12 109.8(11) yes . . . C7 C6 C12 131.2(11) yes . . . C6 C7 C8 118.4(11) yes . . . C7 C8 C9 121.4(12) yes . . . Br1 C9 C8 114.8(10) yes . . . Br1 C9 C10 120.8(9) yes . . . C8 C9 C10 124.4(12) yes . . . C1 C10 C5 114.8(11) yes . . . C1 C10 C9 133.6(11) yes . . . C5 C10 C9 111.6(10) yes . . . C4 C11 C12 104.1(11) yes . . . C6 C12 C11 104.0(10) yes . . . Se1 C13 C14 117.6(9) yes . . . Se1 C13 C18 121.8(10) yes . . . C14 C13 C18 120.5(11) yes . . . C13 C14 C15 120.1(13) yes . . . C14 C15 C16 118.1(14) yes . . . C15 C16 C17 121.5(13) yes . . . C16 C17 C18 119.8(13) yes . . . C13 C18 C17 119.8(13) yes . . . C1 C2 H2 118.453 no . . . C3 C2 H2 118.463 no . . . C2 C3 H3 120.547 no . . . C4 C3 H3 120.548 no . . . C6 C7 H7 120.805 no . . . C8 C7 H7 120.797 no . . . C7 C8 H8 119.308 no . . . C9 C8 H8 119.310 no . . . C4 C11 H11A 110.939 no . . . C4 C11 H11B 110.936 no . . . C12 C11 H11A 110.938 no . . . C12 C11 H11B 110.943 no . . . H11A C11 H11B 108.970 no . . . C6 C12 H12A 110.945 no . . . C6 C12 H12B 110.955 no . . . C11 C12 H12A 110.955 no . . . C11 C12 H12B 110.950 no . . . H12A C12 H12B 108.966 no . . . C13 C14 H14 119.949 no . . . C15 C14 H14 119.964 no . . . C14 C15 H15 120.970 no . . . C16 C15 H15 120.971 no . . . C15 C16 H16 119.275 no . . . C17 C16 H16 119.268 no . . . C16 C17 H17 120.069 no . . . C18 C17 H17 120.084 no . . . C13 C18 H18 120.119 no . . . C17 C18 H18 120.119 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I1 Se1 C1 C2 -111.1(7) no . . . . I1 Se1 C1 C10 70.0(8) no . . . . I1 Se1 C13 C14 -133.8(7) no . . . . I1 Se1 C13 C18 44.8(8) no . . . . C1 Se1 C13 C14 114.2(8) no . . . . C1 Se1 C13 C18 -67.3(9) no . . . . C13 Se1 C1 C2 -14.9(9) no . . . . C13 Se1 C1 C10 166.2(8) no . . . . Se1 C1 C2 C3 177.8(7) no . . . . Se1 C1 C10 C5 -176.6(6) no . . . . Se1 C1 C10 C9 0.6(17) no . . . . C2 C1 C10 C5 4.4(15) no . . . . C2 C1 C10 C9 -178.3(11) no . . . . C10 C1 C2 C3 -3.2(17) no . . . . C1 C2 C3 C4 -0.0(18) no . . . . C2 C3 C4 C5 1.6(17) no . . . . C2 C3 C4 C11 -179.6(10) no . . . . C3 C4 C5 C6 178.4(10) no . . . . C3 C4 C5 C10 0.0(17) no . . . . C3 C4 C11 C12 -179.2(12) no . . . . C5 C4 C11 C12 -0.3(12) no . . . . C11 C4 C5 C6 -0.6(13) no . . . . C11 C4 C5 C10 -179.0(9) no . . . . C4 C5 C6 C7 179.4(9) no . . . . C4 C5 C6 C12 1.3(13) no . . . . C4 C5 C10 C1 -3.0(15) no . . . . C4 C5 C10 C9 179.1(10) no . . . . C6 C5 C10 C1 178.8(10) no . . . . C6 C5 C10 C9 0.9(15) no . . . . C10 C5 C6 C7 -2.3(17) no . . . . C10 C5 C6 C12 179.7(10) no . . . . C5 C6 C7 C8 3.3(16) no . . . . C5 C6 C12 C11 -1.4(12) no . . . . C7 C6 C12 C11 -179.2(12) no . . . . C12 C6 C7 C8 -179.1(10) no . . . . C6 C7 C8 C9 -3.3(18) no . . . . C7 C8 C9 Br1 179.0(10) no . . . . C7 C8 C9 C10 2.1(19) no . . . . Br1 C9 C10 C1 5.1(17) no . . . . Br1 C9 C10 C5 -177.6(6) no . . . . C8 C9 C10 C1 -178.1(11) no . . . . C8 C9 C10 C5 -0.8(16) no . . . . C4 C11 C12 C6 1.0(11) no . . . . Se1 C13 C14 C15 -178.2(8) no . . . . Se1 C13 C18 C17 -178.9(7) no . . . . C14 C13 C18 C17 -0.4(17) no . . . . C18 C13 C14 C15 3.2(18) no . . . . C13 C14 C15 C16 -5.7(19) no . . . . C14 C15 C16 C17 6(2) no . . . . C15 C16 C17 C18 -3(2) no . . . . C16 C17 C18 C13 0.1(19) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 I1 C18 3.595(14) no . . Br1 Se1 3.1753(19) no . . Br1 C1 3.437(12) no . . Se1 C9 3.496(12) no . . C1 C4 2.797(17) no . . C1 C18 3.512(14) no . . C2 C5 2.716(16) no . . C2 C13 3.031(15) no . . C2 C18 3.326(15) no . . C3 C6 3.558(17) no . . C3 C10 2.846(18) no . . C4 C7 3.574(18) no . . C5 C8 2.729(18) no . . C6 C9 2.782(18) no . . C7 C10 2.898(16) no . . C13 C16 2.723(17) no . . C14 C17 2.752(19) no . . C15 C18 2.76(2) no . . I2 I2 3.4731(17) no . 3_767 C2 C9 3.595(17) no . 3_656 C9 C2 3.595(17) no . 3_656 I1 H18 3.1425 no . . Br1 H8 2.7833 no . . Se1 H2 2.8935 no . . Se1 H14 2.8627 no . . Se1 H18 3.0085 no . . C1 H3 3.2886 no . . C1 H18 3.3529 no . . C2 H18 3.2903 no . . C3 H11A 2.9081 no . . C3 H11B 2.9003 no . . C4 H2 3.2061 no . . C4 H12A 3.0996 no . . C4 H12B 3.0856 no . . C5 H3 3.2229 no . . C5 H7 3.2546 no . . C5 H11A 3.0357 no . . C5 H11B 3.0316 no . . C5 H12A 3.0515 no . . C5 H12B 3.0341 no . . C6 H8 3.2556 no . . C6 H11A 3.0967 no . . C6 H11B 3.0829 no . . C7 H12A 2.9556 no . . C7 H12B 2.9475 no . . C9 H7 3.2747 no . . C10 H2 3.2732 no . . C10 H8 3.2986 no . . C11 H3 2.8155 no . . C12 H7 2.8818 no . . C13 H2 2.4631 no . . C13 H15 3.2347 no . . C13 H17 3.2387 no . . C14 H2 3.0792 no . . C14 H16 3.2387 no . . C14 H18 3.2365 no . . C15 H17 3.2489 no . . C16 H14 3.2410 no . . C16 H18 3.2092 no . . C17 H2 3.5276 no . . C17 H15 3.2508 no . . C18 H2 2.7542 no . . C18 H14 3.2418 no . . C18 H16 3.2019 no . . H2 H3 2.3269 no . . H2 H14 3.4878 no . . H2 H18 2.9523 no . . H3 H11A 2.9416 no . . H3 H11B 2.9242 no . . H7 H8 2.3697 no . . H7 H12A 3.0165 no . . H7 H12B 2.9951 no . . H11A H12A 2.7740 no . . H11A H12B 2.2637 no . . H11B H12A 2.2639 no . . H11B H12B 2.7836 no . . H14 H15 2.3587 no . . H15 H16 2.3367 no . . H16 H17 2.3038 no . . H17 H18 2.3045 no . . I1 H11B 3.3303 no . 2_656 I1 H16 3.0975 no . 3_757 I2 H11B 3.4069 no . 2_656 I2 H12A 3.3152 no . 2_656 I2 H14 3.5851 no . 2_756 I2 H15 3.4422 no . 3_757 I2 H17 3.3135 no . 4_554 Br1 H3 3.4547 no . 3_656 Se1 H11B 3.5443 no . 3_656 Se1 H12A 3.4471 no . 3_656 C2 H11A 3.0671 no . 3_657 C3 H3 3.5389 no . 3_657 C3 H8 3.4972 no . 2_646 C3 H11A 3.1904 no . 3_657 C4 H3 3.5173 no . 3_657 C4 H8 3.0592 no . 4_555 C5 H8 2.8473 no . 4_555 C6 H8 2.7658 no . 4_555 C6 H14 3.1383 no . 3_656 C7 H2 3.4429 no . 2_656 C7 H3 3.5062 no . 2_656 C7 H8 3.4092 no . 4_555 C7 H12B 3.1691 no . 4_554 C7 H14 3.1187 no . 3_656 C8 H2 3.5790 no . 3_656 C8 H3 2.8306 no . 2_656 C8 H12B 3.1785 no . 4_554 C9 H3 3.2157 no . 2_656 C11 H8 3.1430 no . 4_555 C11 H17 3.2580 no . 3_657 C11 H18 3.3136 no . 3_657 C12 H7 3.5106 no . 4_555 C12 H8 2.9371 no . 4_555 C12 H14 3.1145 no . 3_656 C12 H17 3.1251 no . 3_657 C14 H7 3.5072 no . 3_656 C14 H12A 3.2748 no . 3_656 C15 H7 3.4829 no . 2_646 C16 H7 3.3158 no . 2_646 C17 H7 3.5804 no . 2_646 C17 H11A 3.1440 no . 3_657 C17 H12B 3.1749 no . 3_657 C18 H11A 2.9497 no . 3_657 H2 C7 3.4429 no . 2_646 H2 C8 3.5790 no . 3_656 H2 H7 3.1677 no . 2_646 H2 H11A 2.8062 no . 3_657 H3 Br1 3.4547 no . 3_656 H3 C3 3.5389 no . 3_657 H3 C4 3.5173 no . 3_657 H3 C7 3.5062 no . 2_646 H3 C8 2.8306 no . 2_646 H3 C9 3.2157 no . 2_646 H3 H3 3.5647 no . 3_657 H3 H8 2.6489 no . 2_646 H3 H11A 3.0436 no . 3_657 H7 C12 3.5106 no . 4_554 H7 C14 3.5072 no . 3_656 H7 C15 3.4829 no . 2_656 H7 C16 3.3158 no . 2_656 H7 C17 3.5804 no . 2_656 H7 H2 3.1677 no . 2_656 H7 H11A 3.4702 no . 4_554 H7 H12B 2.6031 no . 4_554 H7 H14 2.9188 no . 3_656 H7 H16 3.5305 no . 2_656 H8 C3 3.4972 no . 2_656 H8 C4 3.0592 no . 4_554 H8 C5 2.8473 no . 4_554 H8 C6 2.7658 no . 4_554 H8 C7 3.4092 no . 4_554 H8 C11 3.1430 no . 4_554 H8 C12 2.9371 no . 4_554 H8 H3 2.6489 no . 2_656 H8 H11A 2.9319 no . 4_554 H8 H12B 2.5876 no . 4_554 H11A C2 3.0671 no . 3_657 H11A C3 3.1904 no . 3_657 H11A C17 3.1440 no . 3_657 H11A C18 2.9497 no . 3_657 H11A H2 2.8062 no . 3_657 H11A H3 3.0436 no . 3_657 H11A H7 3.4702 no . 4_555 H11A H8 2.9319 no . 4_555 H11A H17 3.0169 no . 3_657 H11A H18 2.6633 no . 3_657 H11B I1 3.3303 no . 2_646 H11B I2 3.4069 no . 2_646 H11B Se1 3.5443 no . 3_656 H11B H17 3.1630 no . 3_657 H11B H18 3.1205 no . 3_657 H12A I2 3.3152 no . 2_646 H12A Se1 3.4471 no . 3_656 H12A C14 3.2748 no . 3_656 H12A H14 2.3660 no . 3_656 H12A H17 2.9459 no . 3_657 H12B C7 3.1691 no . 4_555 H12B C8 3.1785 no . 4_555 H12B C17 3.1749 no . 3_657 H12B H7 2.6031 no . 4_555 H12B H8 2.5876 no . 4_555 H12B H15 3.2261 no . 2_656 H12B H17 2.8203 no . 3_657 H14 I2 3.5851 no . 2_746 H14 C6 3.1383 no . 3_656 H14 C7 3.1187 no . 3_656 H14 C12 3.1145 no . 3_656 H14 H7 2.9188 no . 3_656 H14 H12A 2.3660 no . 3_656 H15 I2 3.4422 no . 3_757 H15 H12B 3.2261 no . 2_646 H15 H16 3.1272 no . 4_544 H16 I1 3.0975 no . 3_757 H16 H7 3.5305 no . 2_646 H16 H15 3.1272 no . 4_545 H17 I2 3.3135 no . 4_555 H17 C11 3.2580 no . 3_657 H17 C12 3.1251 no . 3_657 H17 H11A 3.0169 no . 3_657 H17 H11B 3.1630 no . 3_657 H17 H12A 2.9459 no . 3_657 H17 H12B 2.8203 no . 3_657 H18 C11 3.3136 no . 3_657 H18 H11A 2.6633 no . 3_657 H18 H11B 3.1205 no . 3_657 #============================================================================== data_Ferg99-1 _database_code_depnum_ccdc_archive 'CCDC 850817' #TrackingRef '- 2.cif' # start Validation Reply Form _vrf_PLAT431_I ; PROBLEM: Short Inter HL..A Contact Br2 .. Br5 .. 2.98 Ang. RESPONSE: Guenuine interatomic distance ; # end Validation Reply Form #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 Br6 Se2' _chemical_formula_moiety 'C24 H18 Br6 Se2' _chemical_formula_weight 943.75 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.870(5) _cell_length_b 11.404(6) _cell_length_c 11.938(6) _cell_angle_alpha 106.223(7) _cell_angle_beta 91.894(8) _cell_angle_gamma 108.294(9) _cell_volume 1337.3(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4841 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880.00 _exptl_absorpt_coefficient_mu 11.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.703 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 11213 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_theta_max 26.38 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5355 _reflns_number_gt 3993 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1470 _refine_ls_R_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.3337 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5355 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1594P)^2^+13.3638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 2.460 _refine_diff_density_min -2.400 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Se Se -0.0929 2.2259 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br1 Br 0.2890(3) 0.6472(2) 0.8238(2) 0.0476(6) Uani 1.0 2 d . . . Br2 Br -0.35151(19) 0.8619(2) 0.81853(18) 0.0400(6) Uani 1.0 2 d . . . Br3 Br -0.25060(17) 0.70127(18) 0.85105(15) 0.0327(5) Uani 1.0 2 d . . . Br4 Br -0.1411(2) 0.5426(2) 0.88872(16) 0.0407(6) Uani 1.0 2 d . . . Br5 Br -0.5033(2) 0.2930(3) 0.41994(19) 0.0456(6) Uani 1.0 2 d . . . Br6 Br -0.3890(3) 0.4236(3) 0.6045(2) 0.0550(7) Uani 1.0 2 d . . . Se1 Se 0.12814(17) 0.43835(17) 0.81928(15) 0.0290(5) Uani 1.0 2 d . . . Se2 Se -0.06919(16) 0.22210(18) 0.84185(15) 0.0295(5) Uani 1.0 2 d . . . C1 C 0.2459(18) 0.3414(18) 0.8351(15) 0.030(4) Uani 1.0 2 d . . . C2 C 0.3783(18) 0.4007(19) 0.8447(15) 0.034(5) Uani 1.0 2 d . . . C3 C 0.4665(19) 0.334(3) 0.857(2) 0.048(6) Uani 1.0 2 d . . . C4 C 0.4219(18) 0.2125(19) 0.8580(15) 0.032(4) Uani 1.0 2 d . . . C5 C 0.2808(16) 0.1481(16) 0.8519(15) 0.024(4) Uani 1.0 2 d . . . C6 C 0.2469(19) 0.0249(17) 0.8610(16) 0.031(4) Uani 1.0 2 d . . . C7 C 0.1235(18) -0.0406(18) 0.8662(17) 0.035(5) Uani 1.0 2 d . . . C8 C 0.0250(16) 0.0198(16) 0.8563(15) 0.025(4) Uani 1.0 2 d . . . C9 C 0.0614(17) 0.1441(16) 0.8441(14) 0.025(4) Uani 1.0 2 d . . . C10 C 0.1888(17) 0.2166(17) 0.8419(16) 0.029(4) Uani 1.0 2 d . . . C11 C 0.4872(17) 0.118(2) 0.8764(19) 0.037(5) Uani 1.0 2 d . . . C12 C 0.3721(18) -0.012(2) 0.8640(17) 0.037(5) Uani 1.0 2 d . . . C13 C 0.0875(18) 0.3799(19) 0.6484(18) 0.034(4) Uani 1.0 2 d . . . C14 C -0.0313(15) 0.3810(17) 0.6037(15) 0.026(4) Uani 1.0 2 d . . . C15 C -0.069(3) 0.3377(19) 0.4825(17) 0.040(5) Uani 1.0 2 d . . . C16 C 0.0192(19) 0.3018(17) 0.4083(15) 0.034(5) Uani 1.0 2 d . . . C17 C 0.1328(19) 0.300(2) 0.4539(18) 0.040(5) Uani 1.0 2 d . . . C18 C 0.1739(19) 0.342(2) 0.5777(19) 0.042(5) Uani 1.0 2 d . . . C19 C -0.1613(14) 0.1316(15) 0.6827(16) 0.024(4) Uani 1.0 2 d . . . C20 C -0.122(2) 0.046(3) 0.6046(17) 0.047(6) Uani 1.0 2 d . . . C21 C -0.197(2) -0.018(3) 0.4936(19) 0.045(5) Uani 1.0 2 d . . . C22 C -0.3066(19) 0.014(3) 0.468(2) 0.046(6) Uani 1.0 2 d . . . C23 C -0.3415(15) 0.1055(17) 0.5497(17) 0.029(4) Uani 1.0 2 d . . . C24 C -0.2719(18) 0.1611(19) 0.6617(17) 0.035(5) Uani 1.0 2 d . . . H2 H 0.4119 0.4879 0.8434 0.0411 Uiso 1.0 2 calc R . . H3 H 0.5580 0.3769 0.8639 0.0579 Uiso 1.0 2 calc R . . H7 H 0.1000 -0.1244 0.8760 0.0425 Uiso 1.0 2 calc R . . H8 H -0.0643 -0.0256 0.8582 0.0305 Uiso 1.0 2 calc R . . H11A H 0.5388 0.1513 0.9555 0.0444 Uiso 1.0 2 calc R . . H11B H 0.5460 0.1034 0.8164 0.0444 Uiso 1.0 2 calc R . . H12A H 0.3706 -0.0800 0.7907 0.0439 Uiso 1.0 2 calc R . . H12B H 0.3810 -0.0440 0.9319 0.0439 Uiso 1.0 2 calc R . . H14 H -0.0868 0.4112 0.6556 0.0310 Uiso 1.0 2 calc R . . H15 H -0.1528 0.3327 0.4508 0.0482 Uiso 1.0 2 calc R . . H16 H -0.0016 0.2787 0.3254 0.0410 Uiso 1.0 2 calc R . . H17 H 0.1879 0.2694 0.4019 0.0481 Uiso 1.0 2 calc R . . H18 H 0.2563 0.3446 0.6091 0.0501 Uiso 1.0 2 calc R . . H20 H -0.0447 0.0296 0.6236 0.0559 Uiso 1.0 2 calc R . . H21 H -0.1742 -0.0821 0.4370 0.0535 Uiso 1.0 2 calc R . . H22 H -0.3575 -0.0274 0.3930 0.0550 Uiso 1.0 2 calc R . . H23 H -0.4129 0.1303 0.5296 0.0351 Uiso 1.0 2 calc R . . H24 H -0.2995 0.2178 0.7221 0.0423 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0553(13) 0.0304(11) 0.0514(13) 0.0073(9) -0.0009(10) 0.0126(10) Br2 0.0388(11) 0.0425(12) 0.0393(11) 0.0173(9) -0.0036(8) 0.0103(9) Br3 0.0347(10) 0.0405(11) 0.0233(9) 0.0169(8) 0.0002(7) 0.0060(8) Br4 0.0499(12) 0.0484(12) 0.0299(10) 0.0315(10) 0.0027(8) 0.0047(9) Br5 0.0451(12) 0.0565(14) 0.0449(12) 0.0281(11) 0.0049(9) 0.0179(10) Br6 0.0635(15) 0.0593(15) 0.0426(13) 0.0280(12) 0.0019(11) 0.0083(11) Se1 0.0396(10) 0.0261(10) 0.0241(9) 0.0162(8) 0.0032(7) 0.0062(7) Se2 0.0297(9) 0.0341(10) 0.0264(9) 0.0144(8) 0.0034(7) 0.0077(8) C1 0.037(10) 0.038(10) 0.025(9) 0.029(9) 0.005(7) 0.004(8) C2 0.042(11) 0.030(10) 0.016(9) 0.001(8) -0.003(8) -0.003(7) C3 0.024(10) 0.072(16) 0.073(16) 0.020(10) 0.019(10) 0.054(14) C4 0.038(10) 0.035(10) 0.016(8) 0.004(8) -0.001(7) 0.007(8) C5 0.030(9) 0.022(9) 0.025(9) 0.012(7) 0.005(7) 0.013(7) C6 0.045(11) 0.024(9) 0.027(9) 0.018(8) -0.005(8) 0.007(8) C7 0.040(11) 0.030(10) 0.048(12) 0.027(9) -0.008(9) 0.015(9) C8 0.021(8) 0.023(9) 0.026(9) 0.006(7) -0.010(7) 0.001(7) C9 0.039(10) 0.022(9) 0.021(8) 0.022(8) 0.010(7) 0.003(7) C10 0.032(9) 0.030(10) 0.030(9) 0.016(8) 0.009(7) 0.010(8) C11 0.022(9) 0.046(12) 0.054(12) 0.016(8) 0.002(8) 0.027(10) C12 0.034(10) 0.043(12) 0.032(10) 0.019(9) -0.008(8) 0.005(9) C13 0.037(10) 0.034(10) 0.041(11) 0.020(9) 0.013(8) 0.014(9) C14 0.017(8) 0.035(10) 0.023(9) 0.010(7) 0.002(6) 0.005(8) C15 0.057(13) 0.027(10) 0.034(11) 0.012(9) -0.000(9) 0.007(9) C16 0.050(11) 0.022(9) 0.016(9) 0.009(8) 0.002(8) -0.012(7) C17 0.039(11) 0.036(11) 0.037(11) 0.002(9) 0.001(9) 0.011(9) C18 0.034(10) 0.050(13) 0.044(12) 0.022(10) 0.017(9) 0.010(10) C19 0.014(7) 0.016(8) 0.047(11) 0.002(6) -0.000(7) 0.019(8) C20 0.048(12) 0.059(14) 0.027(10) 0.024(11) -0.005(9) -0.001(10) C21 0.044(12) 0.057(14) 0.039(12) 0.025(11) 0.006(9) 0.015(11) C22 0.031(10) 0.053(14) 0.062(14) 0.029(10) -0.000(10) 0.014(11) C23 0.008(7) 0.034(10) 0.055(12) 0.006(7) 0.002(7) 0.029(9) C24 0.039(11) 0.035(11) 0.034(11) 0.018(9) 0.006(8) 0.008(9) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br1 Se1 2.458(3) yes . . Br2 Br3 2.518(4) yes . . Br3 Br4 2.582(4) yes . . Br5 Br6 2.332(3) yes . . Se1 Se2 2.801(3) yes . . Se1 C1 1.97(3) yes . . Se1 C13 1.95(2) yes . . Se2 C9 1.90(2) yes . . Se2 C19 1.952(17) yes . . C1 C2 1.37(3) yes . . C1 C10 1.39(3) yes . . C2 C3 1.43(4) yes . . C3 C4 1.32(4) yes . . C4 C5 1.47(3) yes . . C4 C11 1.53(4) yes . . C5 C6 1.37(3) yes . . C5 C10 1.47(3) yes . . C6 C7 1.33(3) yes . . C6 C12 1.55(3) yes . . C7 C8 1.46(3) yes . . C8 C9 1.40(3) yes . . C9 C10 1.38(3) yes . . C11 C12 1.57(3) yes . . C13 C14 1.39(3) yes . . C13 C18 1.37(3) yes . . C14 C15 1.39(3) yes . . C15 C16 1.41(3) yes . . C16 C17 1.34(3) yes . . C17 C18 1.43(3) yes . . C19 C20 1.33(3) yes . . C19 C24 1.38(3) yes . . C20 C21 1.40(3) yes . . C21 C22 1.40(4) yes . . C22 C23 1.37(3) yes . . C23 C24 1.39(3) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br2 Br3 Br4 178.19(9) yes . . . Br1 Se1 Se2 171.42(11) yes . . . Br1 Se1 C1 100.2(5) yes . . . Br1 Se1 C13 93.5(6) yes . . . Se2 Se1 C1 84.9(6) yes . . . Se2 Se1 C13 92.6(6) yes . . . C1 Se1 C13 99.1(9) yes . . . Se1 Se2 C9 87.1(5) yes . . . Se1 Se2 C19 104.3(6) yes . . . C9 Se2 C19 101.6(7) yes . . . Se1 C1 C2 119.5(16) yes . . . Se1 C1 C10 117.2(14) yes . . . C2 C1 C10 123(2) yes . . . C1 C2 C3 121(2) yes . . . C2 C3 C4 120.4(18) yes . . . C3 C4 C5 120(2) yes . . . C3 C4 C11 133.7(18) yes . . . C5 C4 C11 106.4(16) yes . . . C4 C5 C6 114.3(19) yes . . . C4 C5 C10 120.5(17) yes . . . C6 C5 C10 125.2(16) yes . . . C5 C6 C7 121(2) yes . . . C5 C6 C12 108.3(16) yes . . . C7 C6 C12 131(2) yes . . . C6 C7 C8 118.1(19) yes . . . C7 C8 C9 120.3(15) yes . . . Se2 C9 C8 118.5(13) yes . . . Se2 C9 C10 118.1(15) yes . . . C8 C9 C10 123.3(19) yes . . . C1 C10 C5 115.0(16) yes . . . C1 C10 C9 132(2) yes . . . C5 C10 C9 112.6(17) yes . . . C4 C11 C12 105.5(15) yes . . . C6 C12 C11 104.5(18) yes . . . Se1 C13 C14 116.3(14) yes . . . Se1 C13 C18 121.1(16) yes . . . C14 C13 C18 122.7(19) yes . . . C13 C14 C15 120.0(18) yes . . . C14 C15 C16 118(2) yes . . . C15 C16 C17 120.4(18) yes . . . C16 C17 C18 123(2) yes . . . C13 C18 C17 116(2) yes . . . Se2 C19 C20 122.3(15) yes . . . Se2 C19 C24 113.4(13) yes . . . C20 C19 C24 124.3(17) yes . . . C19 C20 C21 118(3) yes . . . C20 C21 C22 119(3) yes . . . C21 C22 C23 121.2(19) yes . . . C22 C23 C24 119(2) yes . . . C19 C24 C23 117.8(18) yes . . . C1 C2 H2 119.466 no . . . C3 C2 H2 119.476 no . . . C2 C3 H3 119.778 no . . . C4 C3 H3 119.778 no . . . C6 C7 H7 120.966 no . . . C8 C7 H7 120.971 no . . . C7 C8 H8 119.828 no . . . C9 C8 H8 119.828 no . . . C4 C11 H11A 110.631 no . . . C4 C11 H11B 110.628 no . . . C12 C11 H11A 110.639 no . . . C12 C11 H11B 110.633 no . . . H11A C11 H11B 108.766 no . . . C6 C12 H12A 110.844 no . . . C6 C12 H12B 110.841 no . . . C11 C12 H12A 110.849 no . . . C11 C12 H12B 110.839 no . . . H12A C12 H12B 108.890 no . . . C13 C14 H14 120.029 no . . . C15 C14 H14 120.021 no . . . C14 C15 H15 120.874 no . . . C16 C15 H15 120.867 no . . . C15 C16 H16 119.812 no . . . C17 C16 H16 119.809 no . . . C16 C17 H17 118.720 no . . . C18 C17 H17 118.725 no . . . C13 C18 H18 122.007 no . . . C17 C18 H18 122.006 no . . . C19 C20 H20 120.828 no . . . C21 C20 H20 120.833 no . . . C20 C21 H21 120.723 no . . . C22 C21 H21 120.732 no . . . C21 C22 H22 119.384 no . . . C23 C22 H22 119.379 no . . . C22 C23 H23 120.267 no . . . C24 C23 H23 120.264 no . . . C19 C24 H24 121.090 no . . . C23 C24 H24 121.084 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br1 Se1 C1 C2 0.1(12) no . . . . Br1 Se1 C1 C10 176.9(10) no . . . . Br1 Se1 C13 C14 -105.6(12) no . . . . Br1 Se1 C13 C18 73.2(14) no . . . . Se2 Se1 C1 C2 -172.9(12) no . . . . Se2 Se1 C1 C10 3.9(10) no . . . . C1 Se1 Se2 C9 -3.7(5) no . . . . C1 Se1 Se2 C19 -105.0(5) no . . . . Se2 Se1 C13 C14 68.3(13) no . . . . Se2 Se1 C13 C18 -112.9(14) no . . . . C13 Se1 Se2 C9 95.1(7) no . . . . C13 Se1 Se2 C19 -6.1(7) no . . . . C1 Se1 C13 C14 153.5(13) no . . . . C1 Se1 C13 C18 -27.7(15) no . . . . C13 Se1 C1 C2 95.4(12) no . . . . C13 Se1 C1 C10 -87.9(12) no . . . . Se1 Se2 C9 C8 179.3(10) no . . . . Se1 Se2 C9 C10 3.7(10) no . . . . Se1 Se2 C19 C20 85.7(13) no . . . . Se1 Se2 C19 C24 -96.5(10) no . . . . C9 Se2 C19 C20 -4.3(15) no . . . . C9 Se2 C19 C24 173.5(11) no . . . . C19 Se2 C9 C8 -76.7(12) no . . . . C19 Se2 C9 C10 107.7(11) no . . . . Se1 C1 C2 C3 179.8(10) no . . . . Se1 C1 C10 C5 179.2(9) no . . . . Se1 C1 C10 C9 -3(3) no . . . . C2 C1 C10 C5 -4(3) no . . . . C2 C1 C10 C9 173.9(16) no . . . . C10 C1 C2 C3 3(3) no . . . . C1 C2 C3 C4 0(3) no . . . . C2 C3 C4 C5 -3(3) no . . . . C2 C3 C4 C11 -175.6(16) no . . . . C3 C4 C5 C6 -176.3(17) no . . . . C3 C4 C5 C10 1(3) no . . . . C3 C4 C11 C12 -179(2) no . . . . C5 C4 C11 C12 7.1(18) no . . . . C11 C4 C5 C6 -1.5(18) no . . . . C11 C4 C5 C10 176.1(13) no . . . . C4 C5 C6 C7 174.7(14) no . . . . C4 C5 C6 C12 -5.0(19) no . . . . C4 C5 C10 C1 2(3) no . . . . C4 C5 C10 C9 -176.5(13) no . . . . C6 C5 C10 C1 179.3(15) no . . . . C6 C5 C10 C9 1(3) no . . . . C10 C5 C6 C7 -3(3) no . . . . C10 C5 C6 C12 177.5(14) no . . . . C5 C6 C7 C8 3(3) no . . . . C5 C6 C12 C11 9.0(18) no . . . . C7 C6 C12 C11 -170.5(18) no . . . . C12 C6 C7 C8 -177.6(15) no . . . . C6 C7 C8 C9 -1(3) no . . . . C7 C8 C9 Se2 -176.0(13) no . . . . C7 C8 C9 C10 -1(3) no . . . . Se2 C9 C10 C1 -2(3) no . . . . Se2 C9 C10 C5 176.2(9) no . . . . C8 C9 C10 C1 -177.3(15) no . . . . C8 C9 C10 C5 1(3) no . . . . C4 C11 C12 C6 -9.7(18) no . . . . Se1 C13 C14 C15 -178.5(11) no . . . . Se1 C13 C18 C17 179.3(12) no . . . . C14 C13 C18 C17 -2(3) no . . . . C18 C13 C14 C15 3(3) no . . . . C13 C14 C15 C16 -4(3) no . . . . C14 C15 C16 C17 5(3) no . . . . C15 C16 C17 C18 -5(3) no . . . . C16 C17 C18 C13 3(3) no . . . . Se2 C19 C20 C21 177.5(12) no . . . . Se2 C19 C24 C23 177.6(12) no . . . . C20 C19 C24 C23 -5(3) no . . . . C24 C19 C20 C21 0(4) no . . . . C19 C20 C21 C22 3(4) no . . . . C20 C21 C22 C23 -1(4) no . . . . C21 C22 C23 C24 -4(4) no . . . . C22 C23 C24 C19 6(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br1 C2 3.32(3) no . . C1 C4 2.80(4) no . . C1 C18 3.15(3) no . . C2 C5 2.77(3) no . . C3 C6 3.60(3) no . . C3 C10 2.87(3) no . . C5 C8 2.72(3) no . . C6 C9 2.79(3) no . . C7 C10 2.89(3) no . . C8 C19 3.58(3) no . . C8 C20 3.49(3) no . . C9 C20 3.14(3) no . . C13 C16 2.75(3) no . . C13 C19 3.38(3) no . . C14 C17 2.75(3) no . . C14 C19 3.17(3) no . . C14 C24 3.25(3) no . . C15 C18 2.82(4) no . . C15 C23 3.58(3) no . . C19 C22 2.71(3) no . . C20 C23 2.78(4) no . . C21 C24 2.78(3) no . . Br1 C12 3.59(3) no . 1_565 Br2 Br5 2.976(3) no . 2_466 Br3 Br6 3.530(3) no . . Br3 C5 3.558(16) no . 2_567 Br3 C10 3.505(18) no . 2_567 Br4 Se1 3.530(4) no . . Br4 Se1 3.427(3) no . 2_567 Br4 C1 3.560(18) no . 2_567 Br5 Br2 2.976(3) no . 2_466 Br6 Br3 3.530(3) no . . Se1 Br4 3.530(4) no . . Se1 Br4 3.427(3) no . 2_567 C1 Br4 3.560(18) no . 2_567 C5 Br3 3.558(16) no . 2_567 C10 Br3 3.505(18) no . 2_567 C12 Br1 3.59(3) no . 1_545 C14 C15 3.50(3) no . 2_566 C15 C14 3.50(3) no . 2_566 C15 C15 3.43(3) no . 2_566 C23 C23 3.464(19) no . 2_456 Br1 H2 2.6230 no . . Br1 H18 3.5825 no . . Se1 H2 2.9450 no . . Se1 H14 2.8765 no . . Se1 H18 3.0075 no . . Se2 H8 2.9029 no . . Se2 H14 3.5405 no . . Se2 H20 2.9825 no . . Se2 H24 2.8210 no . . C1 H3 3.2829 no . . C1 H18 2.7135 no . . C2 H18 2.8797 no . . C3 H11A 2.9451 no . . C3 H11B 2.9376 no . . C4 H2 3.2280 no . . C4 H12A 3.0642 no . . C4 H12B 3.1912 no . . C5 H3 3.2765 no . . C5 H7 3.2098 no . . C5 H11A 3.0122 no . . C5 H11B 3.1037 no . . C5 H12A 2.9715 no . . C5 H12B 3.0804 no . . C6 H8 3.2454 no . . C6 H11A 3.0659 no . . C6 H11B 3.1951 no . . C7 H12A 2.9863 no . . C7 H12B 2.8961 no . . C8 H20 2.8968 no . . C9 H7 3.3376 no . . C9 H20 2.6266 no . . C10 H2 3.2720 no . . C10 H8 3.2870 no . . C10 H18 3.4809 no . . C10 H20 3.2929 no . . C11 H3 2.8594 no . . C12 H7 2.8573 no . . C13 H15 3.2671 no . . C13 H17 3.2314 no . . C14 H16 3.2629 no . . C14 H18 3.2812 no . . C14 H24 3.5068 no . . C15 H17 3.2370 no . . C16 H14 3.2666 no . . C16 H18 3.2832 no . . C17 H15 3.2403 no . . C18 H14 3.2670 no . . C18 H16 3.2812 no . . C19 H8 3.4436 no . . C19 H14 3.1462 no . . C19 H21 3.2132 no . . C19 H23 3.2327 no . . C20 H8 3.4379 no . . C20 H22 3.2695 no . . C20 H24 3.2463 no . . C21 H23 3.2710 no . . C22 H15 3.5550 no . . C22 H20 3.2773 no . . C22 H24 3.2432 no . . C23 H14 3.5585 no . . C23 H15 3.2931 no . . C23 H21 3.2701 no . . C24 H14 2.9509 no . . C24 H20 3.2522 no . . C24 H22 3.2365 no . . H2 H3 2.3655 no . . H2 H18 2.9580 no . . H3 H11A 3.0174 no . . H3 H11B 2.9693 no . . H7 H8 2.4230 no . . H7 H12A 3.0819 no . . H7 H12B 2.8949 no . . H8 H20 3.0377 no . . H11A H12A 2.8292 no . . H11A H12B 2.2804 no . . H11B H12A 2.2809 no . . H11B H12B 2.7404 no . . H14 H15 2.3566 no . . H14 H24 2.9559 no . . H15 H16 2.3679 no . . H15 H23 3.3905 no . . H16 H17 2.2704 no . . H17 H18 2.3879 no . . H20 H21 2.3770 no . . H21 H22 2.3522 no . . H22 H23 2.3155 no . . H23 H24 2.3571 no . . Br1 H11A 3.0525 no . 2_667 Br1 H12A 3.0986 no . 1_565 Br1 H12B 3.1989 no . 1_565 Br2 H8 2.9440 no . 1_565 Br2 H11A 3.4416 no . 2_567 Br2 H11B 3.2845 no . 1_465 Br2 H12A 3.3149 no . 1_465 Br2 H12B 3.5845 no . 1_465 Br2 H12B 3.2117 no . 2_567 Br2 H17 3.4798 no . 2_566 Br3 H8 3.1125 no . 1_565 Br3 H16 3.5015 no . 2_566 Br3 H17 3.2018 no . 2_566 Br4 H3 3.1781 no . 1_455 Br4 H14 2.9448 no . . Br4 H24 3.5064 no . . Br5 H17 3.2763 no . 1_455 Br5 H18 3.5897 no . 1_455 Br5 H23 2.9229 no . . Br6 H3 3.3250 no . 1_455 Br6 H14 3.3760 no . . Br6 H15 3.4574 no . . Br6 H17 3.5205 no . 2_566 Br6 H23 3.1342 no . . Br6 H24 3.4082 no . . C1 H21 3.5943 no . 2_556 C2 H3 3.5806 no . 2_667 C3 H2 3.5540 no . 2_667 C3 H24 3.4639 no . 1_655 C4 H22 3.0532 no . 2_556 C4 H24 3.4748 no . 1_655 C5 H21 3.3976 no . 2_556 C5 H22 3.1260 no . 2_556 C6 H22 3.3022 no . 2_556 C7 H8 3.2964 no . 2_557 C7 H16 2.9028 no . 2_556 C8 H7 3.5570 no . 2_557 C8 H8 3.3996 no . 2_557 C8 H16 3.4130 no . 2_556 C9 H21 3.5719 no . 2_556 C10 H21 3.2282 no . 2_556 C11 H12B 3.1004 no . 2_657 C11 H22 3.2135 no . 2_556 C11 H24 3.1416 no . 1_655 C12 H11A 3.2931 no . 2_657 C12 H12B 3.3422 no . 2_657 C12 H22 3.2285 no . 2_556 C14 H15 3.5019 no . 2_566 C16 H7 3.3938 no . 2_556 C16 H14 3.4293 no . 2_566 C17 H20 3.4122 no . 2_556 C17 H21 3.2480 no . 2_556 C18 H21 2.9253 no . 2_556 C19 H11B 3.5718 no . 1_455 C20 H17 3.4214 no . 2_556 C20 H20 3.3824 no . 2_556 C20 H21 3.1875 no . 2_556 C21 H17 3.4582 no . 2_556 C21 H18 3.4173 no . 2_556 C21 H20 3.0398 no . 2_556 C22 H12A 3.4735 no . 2_556 C22 H23 2.9828 no . 2_456 C23 H11B 3.4514 no . 1_455 C23 H22 3.2592 no . 2_456 C23 H23 3.0266 no . 2_456 C24 H11B 2.8040 no . 1_455 H2 C3 3.5540 no . 2_667 H2 H3 3.3606 no . 2_667 H3 Br4 3.1781 no . 1_655 H3 Br6 3.3250 no . 1_655 H3 C2 3.5806 no . 2_667 H3 H2 3.3606 no . 2_667 H3 H24 2.9624 no . 1_655 H7 C8 3.5570 no . 2_557 H7 C16 3.3938 no . 2_556 H7 H8 3.2572 no . 2_557 H7 H16 2.5108 no . 2_556 H8 Br2 2.9440 no . 1_545 H8 Br3 3.1125 no . 1_545 H8 C7 3.2964 no . 2_557 H8 C8 3.3996 no . 2_557 H8 H7 3.2572 no . 2_557 H8 H8 3.4380 no . 2_557 H8 H16 3.3925 no . 2_556 H8 H17 3.4254 no . 2_556 H11A Br1 3.0525 no . 2_667 H11A Br2 3.4416 no . 2_567 H11A C12 3.2931 no . 2_657 H11A H12A 3.5353 no . 2_657 H11A H12B 2.3620 no . 2_657 H11A H24 3.4774 no . 1_655 H11B Br2 3.2845 no . 1_645 H11B C19 3.5718 no . 1_655 H11B C23 3.4514 no . 1_655 H11B C24 2.8040 no . 1_655 H11B H12B 3.3821 no . 2_657 H11B H22 2.9205 no . 2_556 H11B H23 3.5518 no . 1_655 H11B H24 2.3150 no . 1_655 H12A Br1 3.0986 no . 1_545 H12A Br2 3.3149 no . 1_645 H12A C22 3.4735 no . 2_556 H12A H11A 3.5353 no . 2_657 H12A H15 3.5837 no . 2_556 H12A H22 2.8133 no . 2_556 H12B Br1 3.1989 no . 1_545 H12B Br2 3.5845 no . 1_645 H12B Br2 3.2117 no . 2_567 H12B C11 3.1004 no . 2_657 H12B C12 3.3422 no . 2_657 H12B H11A 2.3620 no . 2_657 H12B H11B 3.3821 no . 2_657 H12B H12B 2.7439 no . 2_657 H14 Br4 2.9448 no . . H14 Br6 3.3760 no . . H14 C16 3.4293 no . 2_566 H14 H16 3.3002 no . 2_566 H15 Br6 3.4574 no . . H15 C14 3.5019 no . 2_566 H15 H12A 3.5837 no . 2_556 H16 Br3 3.5015 no . 2_566 H16 C7 2.9028 no . 2_556 H16 C8 3.4130 no . 2_556 H16 H7 2.5108 no . 2_556 H16 H8 3.3925 no . 2_556 H16 H14 3.3002 no . 2_566 H17 Br2 3.4798 no . 2_566 H17 Br3 3.2018 no . 2_566 H17 Br5 3.2763 no . 1_655 H17 Br6 3.5205 no . 2_566 H17 C20 3.4214 no . 2_556 H17 C21 3.4582 no . 2_556 H17 H8 3.4254 no . 2_556 H17 H20 3.1937 no . 2_556 H17 H21 3.2249 no . 2_556 H18 Br5 3.5897 no . 1_655 H18 C21 3.4173 no . 2_556 H18 H21 2.7250 no . 2_556 H20 C17 3.4122 no . 2_556 H20 C20 3.3824 no . 2_556 H20 C21 3.0398 no . 2_556 H20 H17 3.1937 no . 2_556 H20 H20 3.0985 no . 2_556 H20 H21 2.4507 no . 2_556 H21 C1 3.5943 no . 2_556 H21 C5 3.3976 no . 2_556 H21 C9 3.5719 no . 2_556 H21 C10 3.2282 no . 2_556 H21 C17 3.2480 no . 2_556 H21 C18 2.9253 no . 2_556 H21 C20 3.1875 no . 2_556 H21 H17 3.2249 no . 2_556 H21 H18 2.7250 no . 2_556 H21 H20 2.4507 no . 2_556 H22 C4 3.0532 no . 2_556 H22 C5 3.1260 no . 2_556 H22 C6 3.3022 no . 2_556 H22 C11 3.2135 no . 2_556 H22 C12 3.2285 no . 2_556 H22 C23 3.2592 no . 2_456 H22 H11B 2.9205 no . 2_556 H22 H12A 2.8133 no . 2_556 H22 H23 2.7165 no . 2_456 H23 Br5 2.9229 no . . H23 Br6 3.1342 no . . H23 C22 2.9828 no . 2_456 H23 C23 3.0266 no . 2_456 H23 H11B 3.5518 no . 1_455 H23 H22 2.7165 no . 2_456 H23 H23 2.8505 no . 2_456 H24 Br4 3.5064 no . . H24 Br6 3.4082 no . . H24 C3 3.4639 no . 1_455 H24 C4 3.4748 no . 1_455 H24 C11 3.1416 no . 1_455 H24 H3 2.9624 no . 1_455 H24 H11A 3.4774 no . 1_455 H24 H11B 2.3150 no . 1_455 data_Ferg-109-3_off _database_code_depnum_ccdc_archive 'CCDC 850818' #TrackingRef '- 3.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24.25 H18.50 Br4 Cl0.50 S Se' _chemical_formula_moiety 'C24.25 H18.50 Br4 Cl0.50 S Se' _chemical_formula_weight 758.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.822(8) _cell_length_b 11.568(8) _cell_length_c 11.940(10) _cell_angle_alpha 81.42(3) _cell_angle_beta 73.07(3) _cell_angle_gamma 71.07(3) _cell_volume 1350.2(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2100 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 32.58 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 725.00 _exptl_absorpt_coefficient_mu 7.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.528 _exptl_absorpt_correction_T_max 0.799 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku SCX mini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 13.653 _diffrn_reflns_number 11681 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Dichloromethane solvate molecule is disordered and only a partial weight. The C atom was refined isotropically, and H atoms whilst included in the chemical formula have not been included in the refinement DFIX command used w.r.t. Cl-C and Cl-Cl distances. ; _reflns_number_total 4742 _reflns_number_gt 2975 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2791 _refine_ls_number_restraints 3 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4740 _refine_ls_number_parameters 293 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1476P)^2^+10.9173P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.641 _refine_diff_density_min -1.270 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Se Se -0.0929 2.2259 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Br1 Br 0.88298(9) -0.17349(7) 0.33273(9) 0.0601(3) Uani 1.0 2 d . . . Br2 Br 0.40582(9) -0.07592(8) 0.37923(9) 0.0627(3) Uani 1.0 2 d . . . Br3 Br 0.30560(7) -0.23749(7) 0.33717(7) 0.0438(3) Uani 1.0 2 d . . . Br4 Br 0.21111(8) -0.39173(8) 0.29407(9) 0.0611(3) Uani 1.0 2 d . . . Se1 Se 0.70813(7) 0.02278(6) 0.33093(7) 0.0406(2) Uani 1.0 2 d . . . Cl1 Cl -0.12114(8) 0.41172(13) 0.08458(9) 0.108(4) Uani 0.2500 2 d . . . Cl2 Cl 0.10351(17) 0.28182(7) -0.09860(10) 0.129(5) Uani 0.2500 2 d . . . S1 S 0.49800(18) 0.23520(17) 0.34610(19) 0.0441(6) Uani 1.0 2 d . . . C1 C 0.8078(7) 0.1282(6) 0.3510(6) 0.036(2) Uani 1.0 2 d . . . C2 C 0.9421(7) 0.0790(7) 0.3624(8) 0.045(3) Uani 1.0 2 d . . . C3 C 1.0152(8) 0.1528(7) 0.3747(8) 0.051(3) Uani 1.0 2 d . . . C4 C 0.9574(8) 0.2794(7) 0.3731(8) 0.048(3) Uani 1.0 2 d . . . C5 C 0.8212(7) 0.3271(7) 0.3626(7) 0.041(3) Uani 1.0 2 d . . . C6 C 0.7735(9) 0.4556(7) 0.3679(8) 0.053(3) Uani 1.0 2 d . . . C7 C 0.6414(9) 0.5156(7) 0.3621(8) 0.055(3) Uani 1.0 2 d . . . C8 C 0.5589(9) 0.4486(7) 0.3520(8) 0.053(3) Uani 1.0 2 d . . . C9 C 0.6088(7) 0.3206(7) 0.3472(8) 0.043(3) Uani 1.0 2 d . . . C10 C 0.7436(7) 0.2542(7) 0.3522(6) 0.0351(19) Uani 1.0 2 d . . . C11 C 1.0053(9) 0.3828(8) 0.3889(10) 0.065(3) Uani 1.0 2 d . . . C12 C 0.8881(8) 0.4990(7) 0.3791(10) 0.062(3) Uani 1.0 2 d . . . C13 C 0.7415(9) 0.0408(7) 0.1619(8) 0.051(3) Uani 1.0 2 d . . . C14 C 0.6617(11) -0.0050(9) 0.1154(9) 0.072(4) Uani 1.0 2 d . . . C15 C 0.6869(12) 0.0064(12) -0.0074(11) 0.100(5) Uani 1.0 2 d . . . C16 C 0.7765(12) 0.0611(11) -0.0787(10) 0.102(5) Uani 1.0 2 d . . . C17 C 0.8515(11) 0.1032(10) -0.0286(9) 0.082(4) Uani 1.0 2 d . . . C18 C 0.8355(9) 0.0964(9) 0.0967(9) 0.066(4) Uani 1.0 2 d . . . C19 C 0.4619(8) 0.2735(7) 0.2087(8) 0.047(3) Uani 1.0 2 d . . . C20 C 0.3498(9) 0.2480(9) 0.1961(10) 0.066(4) Uani 1.0 2 d . . . C21 C 0.3149(11) 0.2690(11) 0.0952(11) 0.087(4) Uani 1.0 2 d . . . C22 C 0.3951(10) 0.3164(10) -0.0045(11) 0.089(4) Uani 1.0 2 d . . . C23 C 0.5055(10) 0.3455(8) 0.0045(8) 0.061(3) Uani 1.0 2 d . . . C24 C 0.5369(9) 0.3264(7) 0.1132(8) 0.057(3) Uani 1.0 2 d . . . C25 C 0.02547(11) 0.41891(8) -0.02585(12) 0.23(5) Uiso 0.2500 2 d . . . H2 H 0.9831 -0.0071 0.3617 0.0542 Uiso 1.0 2 calc R . . H3 H 1.1043 0.1173 0.3842 0.0609 Uiso 1.0 2 calc R . . H7 H 0.6072 0.6021 0.3650 0.0656 Uiso 1.0 2 calc R . . H8 H 0.4685 0.4898 0.3484 0.0634 Uiso 1.0 2 calc R . . H11A H 1.0885 0.3856 0.3272 0.0779 Uiso 1.0 2 calc R . . H11B H 1.0241 0.3736 0.4666 0.0779 Uiso 1.0 2 calc R . . H12A H 0.8589 0.5462 0.4497 0.0739 Uiso 1.0 2 calc R . . H12B H 0.9163 0.5517 0.3093 0.0739 Uiso 1.0 2 calc R . . H14 H 0.5956 -0.0411 0.1639 0.0864 Uiso 1.0 2 calc R . . H15 H 0.6380 -0.0263 -0.0423 0.1196 Uiso 1.0 2 calc R . . H16 H 0.7872 0.0702 -0.1611 0.1222 Uiso 1.0 2 calc R . . H17 H 0.9174 0.1387 -0.0787 0.0981 Uiso 1.0 2 calc R . . H18 H 0.8861 0.1280 0.1307 0.0793 Uiso 1.0 2 calc R . . H20 H 0.2960 0.2143 0.2621 0.0788 Uiso 1.0 2 calc R . . H21 H 0.2364 0.2521 0.0905 0.1048 Uiso 1.0 2 calc R . . H22 H 0.3732 0.3283 -0.0776 0.1070 Uiso 1.0 2 calc R . . H23 H 0.5597 0.3781 -0.0621 0.0727 Uiso 1.0 2 calc R . . H24 H 0.6101 0.3500 0.1211 0.0683 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0728(5) 0.0244(4) 0.0840(6) -0.0082(4) -0.0343(5) 0.0080(4) Br2 0.0694(5) 0.0620(5) 0.0659(6) -0.0406(4) -0.0127(5) 0.0066(4) Br3 0.0415(4) 0.0392(4) 0.0484(5) -0.0106(3) -0.0145(3) 0.0063(3) Br4 0.0522(4) 0.0453(4) 0.0906(7) -0.0104(4) -0.0299(4) -0.0053(4) Se1 0.0452(4) 0.0279(3) 0.0499(5) -0.0147(3) -0.0137(4) 0.0056(3) Cl1 0.262(8) 0.057(4) 0.059(4) -0.076(5) -0.108(5) 0.030(4) Cl2 0.140(7) 0.117(10) 0.175(11) -0.048(8) -0.110(7) 0.019(8) S1 0.0378(9) 0.0339(9) 0.0562(12) -0.0094(8) -0.0091(9) 0.0013(8) C1 0.040(4) 0.033(4) 0.026(4) -0.015(3) 0.002(3) 0.009(3) C2 0.034(4) 0.033(4) 0.065(6) -0.012(3) -0.009(4) 0.004(4) C3 0.045(4) 0.039(4) 0.072(6) -0.014(4) -0.025(4) 0.005(4) C4 0.047(4) 0.033(4) 0.067(6) -0.021(3) -0.012(4) 0.005(4) C5 0.036(4) 0.031(4) 0.051(5) -0.011(3) -0.007(4) 0.007(4) C6 0.060(5) 0.041(4) 0.059(5) -0.022(4) -0.011(4) -0.004(4) C7 0.058(5) 0.033(4) 0.072(6) -0.010(4) -0.015(4) -0.013(4) C8 0.063(5) 0.036(4) 0.049(5) 0.001(4) -0.016(4) -0.004(4) C9 0.038(4) 0.037(4) 0.054(5) -0.013(3) -0.010(4) 0.001(4) C10 0.035(3) 0.039(4) 0.033(4) -0.012(3) -0.009(3) -0.004(3) C11 0.063(5) 0.053(5) 0.088(7) -0.029(4) -0.023(5) 0.001(5) C12 0.055(5) 0.031(4) 0.101(7) -0.011(4) -0.018(5) -0.019(4) C13 0.055(5) 0.032(4) 0.054(5) 0.006(4) -0.018(4) -0.000(4) C14 0.087(6) 0.058(6) 0.065(6) 0.001(5) -0.034(5) -0.010(5) C15 0.090(7) 0.091(8) 0.084(8) 0.038(7) -0.032(6) -0.030(6) C16 0.095(7) 0.094(8) 0.054(6) 0.056(7) -0.023(6) -0.000(6) C17 0.062(6) 0.070(7) 0.056(6) 0.025(6) 0.008(5) 0.022(5) C18 0.048(5) 0.053(5) 0.062(6) 0.006(5) 0.002(5) 0.021(5) C19 0.032(4) 0.041(4) 0.062(5) -0.003(4) -0.015(4) 0.004(4) C20 0.050(5) 0.051(5) 0.092(7) -0.008(4) -0.019(5) -0.004(5) C21 0.076(6) 0.086(7) 0.109(9) -0.022(6) -0.043(6) 0.001(7) C22 0.081(5) 0.064(6) 0.128(8) 0.021(5) -0.077(5) -0.016(6) C23 0.078(6) 0.048(5) 0.045(5) -0.006(5) -0.023(5) 0.015(4) C24 0.060(5) 0.028(4) 0.073(6) 0.005(4) -0.018(5) -0.013(4) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r6 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r6' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r6' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br1 Se1 2.4409(17) yes . . Br2 Br3 2.614(2) yes . . Br3 Br4 2.502(2) yes . . Se1 C1 1.949(9) yes . . Se1 C13 1.935(9) yes . . Cl1 C25 1.7599(18) yes . . Cl2 C25 1.7600(18) yes . . S1 C9 1.788(10) yes . . S1 C19 1.756(10) yes . . C1 C2 1.418(11) yes . . C1 C10 1.396(9) yes . . C2 C3 1.386(14) yes . . C3 C4 1.393(10) yes . . C4 C5 1.433(12) yes . . C4 C11 1.504(15) yes . . C5 C6 1.411(11) yes . . C5 C10 1.409(13) yes . . C6 C7 1.389(12) yes . . C6 C12 1.526(15) yes . . C7 C8 1.398(15) yes . . C8 C9 1.406(11) yes . . C9 C10 1.425(10) yes . . C11 C12 1.537(11) yes . . C13 C14 1.414(18) yes . . C13 C18 1.367(13) yes . . C14 C15 1.405(16) yes . . C15 C16 1.350(18) yes . . C16 C17 1.37(2) yes . . C17 C18 1.448(15) yes . . C19 C20 1.390(15) yes . . C19 C24 1.382(12) yes . . C20 C21 1.330(19) yes . . C21 C22 1.409(16) yes . . C22 C23 1.377(18) yes . . C23 C24 1.404(15) yes . . C25 C25 1.919(2) yes . 2_565 C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br2 Br3 Br4 179.24(5) yes . . . Br1 Se1 C1 98.5(2) yes . . . Br1 Se1 C13 94.8(2) yes . . . C1 Se1 C13 99.0(4) yes . . . C9 S1 C19 105.1(4) yes . . . Se1 C1 C2 121.2(6) yes . . . Se1 C1 C10 118.0(6) yes . . . C2 C1 C10 120.9(8) yes . . . C1 C2 C3 121.9(7) yes . . . C2 C3 C4 119.6(8) yes . . . C3 C4 C5 117.5(9) yes . . . C3 C4 C11 132.9(8) yes . . . C5 C4 C11 109.4(7) yes . . . C4 C5 C6 111.4(8) yes . . . C4 C5 C10 124.1(7) yes . . . C6 C5 C10 124.5(7) yes . . . C5 C6 C7 118.5(9) yes . . . C5 C6 C12 108.0(7) yes . . . C7 C6 C12 133.5(8) yes . . . C6 C7 C8 120.0(8) yes . . . C7 C8 C9 120.4(8) yes . . . S1 C9 C8 119.8(7) yes . . . S1 C9 C10 117.9(6) yes . . . C8 C9 C10 122.2(9) yes . . . C1 C10 C5 116.0(7) yes . . . C1 C10 C9 129.5(8) yes . . . C5 C10 C9 114.5(7) yes . . . C4 C11 C12 104.8(8) yes . . . C6 C12 C11 106.2(7) yes . . . Se1 C13 C14 115.3(7) yes . . . Se1 C13 C18 120.0(9) yes . . . C14 C13 C18 124.7(9) yes . . . C13 C14 C15 115.5(11) yes . . . C14 C15 C16 123.9(14) yes . . . C15 C16 C17 118.0(12) yes . . . C16 C17 C18 123.4(10) yes . . . C13 C18 C17 114.5(11) yes . . . S1 C19 C20 117.1(7) yes . . . S1 C19 C24 124.7(8) yes . . . C20 C19 C24 118.2(10) yes . . . C19 C20 C21 122.7(10) yes . . . C20 C21 C22 119.6(13) yes . . . C21 C22 C23 119.8(12) yes . . . C22 C23 C24 119.3(9) yes . . . C19 C24 C23 120.3(10) yes . . . Cl1 C25 Cl2 111.51(10) yes . . . Cl1 C25 C25 82.40(8) yes . . 2_565 Cl2 C25 C25 166.06(9) yes . . 2_565 C1 C2 H2 119.035 no . . . C3 C2 H2 119.031 no . . . C2 C3 H3 120.214 no . . . C4 C3 H3 120.209 no . . . C6 C7 H7 120.014 no . . . C8 C7 H7 120.014 no . . . C7 C8 H8 119.811 no . . . C9 C8 H8 119.807 no . . . C4 C11 H11A 110.791 no . . . C4 C11 H11B 110.786 no . . . C12 C11 H11A 110.787 no . . . C12 C11 H11B 110.789 no . . . H11A C11 H11B 108.859 no . . . C6 C12 H12A 110.496 no . . . C6 C12 H12B 110.493 no . . . C11 C12 H12A 110.492 no . . . C11 C12 H12B 110.494 no . . . H12A C12 H12B 108.672 no . . . C13 C14 H14 122.247 no . . . C15 C14 H14 122.245 no . . . C14 C15 H15 118.070 no . . . C16 C15 H15 118.068 no . . . C15 C16 H16 121.004 no . . . C17 C16 H16 121.013 no . . . C16 C17 H17 118.310 no . . . C18 C17 H17 118.314 no . . . C13 C18 H18 122.764 no . . . C17 C18 H18 122.769 no . . . C19 C20 H20 118.654 no . . . C21 C20 H20 118.647 no . . . C20 C21 H21 120.221 no . . . C22 C21 H21 120.224 no . . . C21 C22 H22 120.121 no . . . C23 C22 H22 120.120 no . . . C22 C23 H23 120.339 no . . . C24 C23 H23 120.342 no . . . C19 C24 H24 119.848 no . . . C23 C24 H24 119.848 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br1 Se1 C1 C2 -0.6(5) no . . . . Br1 Se1 C1 C10 178.6(4) no . . . . Br1 Se1 C13 C14 92.4(5) no . . . . Br1 Se1 C13 C18 -88.5(5) no . . . . C1 Se1 C13 C14 -168.1(5) no . . . . C1 Se1 C13 C18 11.0(6) no . . . . C13 Se1 C1 C2 -96.9(5) no . . . . C13 Se1 C1 C10 82.2(5) no . . . . C9 S1 C19 C20 -162.4(5) no . . . . C9 S1 C19 C24 17.8(7) no . . . . C19 S1 C9 C8 69.6(6) no . . . . C19 S1 C9 C10 -115.1(6) no . . . . Se1 C1 C2 C3 178.9(5) no . . . . Se1 C1 C10 C5 -177.8(4) no . . . . Se1 C1 C10 C9 3.9(10) no . . . . C2 C1 C10 C5 1.4(10) no . . . . C2 C1 C10 C9 -176.9(7) no . . . . C10 C1 C2 C3 -0.3(11) no . . . . C1 C2 C3 C4 -1.5(12) no . . . . C2 C3 C4 C5 2.1(12) no . . . . C2 C3 C4 C11 177.0(8) no . . . . C3 C4 C5 C6 177.2(7) no . . . . C3 C4 C5 C10 -1.0(12) no . . . . C3 C4 C11 C12 -178.7(9) no . . . . C5 C4 C11 C12 -3.5(10) no . . . . C11 C4 C5 C6 1.1(10) no . . . . C11 C4 C5 C10 -177.0(7) no . . . . C4 C5 C6 C7 -178.3(7) no . . . . C4 C5 C6 C12 1.8(9) no . . . . C4 C5 C10 C1 -0.8(11) no . . . . C4 C5 C10 C9 177.8(7) no . . . . C6 C5 C10 C1 -178.7(7) no . . . . C6 C5 C10 C9 -0.1(11) no . . . . C10 C5 C6 C7 -0.2(12) no . . . . C10 C5 C6 C12 180.0(7) no . . . . C5 C6 C7 C8 0.3(13) no . . . . C5 C6 C12 C11 -4.0(10) no . . . . C7 C6 C12 C11 176.2(9) no . . . . C12 C6 C7 C8 -179.9(9) no . . . . C6 C7 C8 C9 -0.2(13) no . . . . C7 C8 C9 S1 175.0(7) no . . . . C7 C8 C9 C10 -0.0(12) no . . . . S1 C9 C10 C1 3.4(11) no . . . . S1 C9 C10 C5 -174.9(5) no . . . . C8 C9 C10 C1 178.5(7) no . . . . C8 C9 C10 C5 0.2(11) no . . . . C4 C11 C12 C6 4.5(10) no . . . . Se1 C13 C14 C15 -179.2(5) no . . . . Se1 C13 C18 C17 179.5(4) no . . . . C14 C13 C18 C17 -1.5(11) no . . . . C18 C13 C14 C15 1.8(12) no . . . . C13 C14 C15 C16 -2.5(14) no . . . . C14 C15 C16 C17 3.0(16) no . . . . C15 C16 C17 C18 -2.6(15) no . . . . C16 C17 C18 C13 1.9(13) no . . . . S1 C19 C20 C21 -177.7(6) no . . . . S1 C19 C24 C23 175.4(5) no . . . . C20 C19 C24 C23 -4.4(11) no . . . . C24 C19 C20 C21 2.2(12) no . . . . C19 C20 C21 C22 1.4(15) no . . . . C20 C21 C22 C23 -2.8(15) no . . . . C21 C22 C23 C24 0.5(13) no . . . . C22 C23 C24 C19 3.2(11) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br1 C2 3.274(9) no . . Se1 S1 2.740(3) no . . Se1 C9 3.277(8) no . . S1 C1 3.190(8) no . . S1 C13 3.330(8) no . . C1 C4 2.824(13) no . . C1 C18 3.029(14) no . . C2 C5 2.741(10) no . . C3 C10 2.867(11) no . . C5 C8 2.760(12) no . . C6 C9 2.802(14) no . . C7 C10 2.871(11) no . . C8 C19 3.405(15) no . . C8 C24 3.464(15) no . . C9 C24 3.097(15) no . . C10 C18 3.514(13) no . . C13 C16 2.770(15) no . . C13 C19 3.300(10) no . . C13 C24 3.404(11) no . . C14 C17 2.777(16) no . . C14 C19 3.383(12) no . . C15 C18 2.80(2) no . . C18 C24 3.430(12) no . . C19 C22 2.777(17) no . . C20 C23 2.749(13) no . . C21 C24 2.764(18) no . . Br1 Br4 3.574(3) no . 1_655 Br1 Cl2 3.177(3) no . 2_655 Br2 Se1 3.396(3) no . 2_656 Br2 C1 3.475(7) no . 2_656 Br3 C5 3.571(8) no . 2_656 Br3 C10 3.575(8) no . 2_656 Br4 Br1 3.574(3) no . 1_455 Se1 Br2 3.396(3) no . 2_656 Cl1 C5 3.254(9) no . 1_455 Cl1 C6 3.300(10) no . 1_455 Cl1 C10 3.598(7) no . 1_455 Cl2 Br1 3.177(3) no . 2_655 Cl2 C14 3.371(10) no . 2_655 C1 Br2 3.475(7) no . 2_656 C5 Br3 3.571(8) no . 2_656 C5 Cl1 3.254(9) no . 1_655 C6 Cl1 3.300(10) no . 1_655 C7 C8 3.472(12) no . 2_666 C8 C7 3.472(12) no . 2_666 C10 Br3 3.575(8) no . 2_656 C10 Cl1 3.598(7) no . 1_655 C14 Cl2 3.371(10) no . 2_655 C15 C21 3.51(2) no . 2_655 C17 C17 3.509(15) no . 2_755 C17 C18 3.369(13) no . 2_755 C18 C17 3.369(13) no . 2_755 C21 C15 3.51(2) no . 2_655 C23 C23 3.525(14) no . 2_665 Br1 H2 2.6019 no . . Se1 H2 3.0070 no . . Se1 H14 2.9065 no . . Se1 H18 2.9794 no . . S1 H8 2.8614 no . . S1 H20 2.7456 no . . S1 H24 2.9218 no . . C1 H3 3.3059 no . . C1 H18 2.5175 no . . C2 H18 2.9376 no . . C3 H11A 2.9781 no . . C3 H11B 2.9657 no . . C4 H2 3.2551 no . . C4 H12A 3.1044 no . . C4 H12B 3.0450 no . . C5 H3 3.2853 no . . C5 H7 3.2696 no . . C5 H11A 3.0789 no . . C5 H11B 3.0349 no . . C5 H12A 3.0620 no . . C5 H12B 3.0127 no . . C6 H8 3.2686 no . . C6 H11A 3.1422 no . . C6 H11B 3.0830 no . . C7 H12A 2.9734 no . . C7 H12B 3.0093 no . . C8 H24 2.9746 no . . C9 H7 3.2890 no . . C9 H24 2.6666 no . . C10 H2 3.2944 no . . C10 H8 3.3278 no . . C10 H18 2.9700 no . . C10 H24 3.3614 no . . C11 H3 2.9099 no . . C12 H7 2.9285 no . . C13 H15 3.2438 no . . C13 H17 3.2252 no . . C13 H24 3.4112 no . . C14 H16 3.2854 no . . C14 H18 3.3258 no . . C15 H17 3.1838 no . . C16 H14 3.2856 no . . C16 H18 3.3400 no . . C17 H15 3.1855 no . . C17 H24 3.4837 no . . C18 H14 3.3164 no . . C18 H16 3.3395 no . . C18 H24 3.1369 no . . C19 H8 3.2375 no . . C19 H14 3.5118 no . . C19 H21 3.2425 no . . C19 H23 3.2731 no . . C20 H14 3.5243 no . . C20 H22 3.2205 no . . C20 H24 3.2408 no . . C21 H23 3.2722 no . . C22 H20 3.2235 no . . C22 H24 3.2569 no . . C23 H21 3.2666 no . . C24 H8 3.3872 no . . C24 H20 3.2329 no . . C24 H22 3.2628 no . . H2 H3 2.3251 no . . H2 H18 3.2379 no . . H3 H11A 3.0361 no . . H3 H11B 3.0362 no . . H7 H8 2.3451 no . . H7 H12A 3.0203 no . . H7 H12B 3.0861 no . . H8 H24 3.0998 no . . H11A H12A 2.7325 no . . H11A H12B 2.2358 no . . H11B H12A 2.2361 no . . H11B H12B 2.7745 no . . H14 H15 2.3591 no . . H15 H16 2.2864 no . . H16 H17 2.3113 no . . H17 H18 2.4133 no . . H18 H24 3.2662 no . . H20 H21 2.2638 no . . H21 H22 2.3638 no . . H22 H23 2.3339 no . . H23 H24 2.3574 no . . Br1 H3 3.5852 no . 2_756 Br1 H11B 3.2167 no . 2_756 Br1 H12A 3.3935 no . 1_545 Br1 H12B 3.1263 no . 1_545 Br1 H17 3.2269 no . 2_755 Br2 H3 3.2932 no . 1_455 Br2 H14 2.8537 no . . Br2 H20 3.4080 no . . Br3 H7 3.2756 no . 1_545 Br3 H8 3.0787 no . 1_545 Br3 H16 2.8164 no . 2_655 Br3 H23 3.5808 no . 2_655 Br4 H8 2.8925 no . 1_545 Br4 H11A 3.1873 no . 1_445 Br4 H11B 3.2070 no . 2_656 Br4 H12A 3.3203 no . 2_656 Br4 H12B 3.4088 no . 1_445 Br4 H23 3.1572 no . 2_655 Cl1 H12B 3.5135 no . 1_455 Cl1 H18 3.2254 no . 1_455 Cl1 H22 3.3508 no . 2_565 Cl1 H24 3.1102 no . 1_455 Cl2 H12B 2.9469 no . 2_665 Cl2 H14 3.5007 no . 2_655 Cl2 H17 2.9369 no . 1_455 Cl2 H21 2.9366 no . . Cl2 H22 3.2174 no . . C2 H2 3.5357 no . 2_756 C2 H3 3.5171 no . 2_756 C2 H16 3.3461 no . 2_755 C3 H2 3.3439 no . 2_756 C3 H16 3.5973 no . 2_755 C3 H20 3.2061 no . 1_655 C4 H20 3.3808 no . 1_655 C7 H8 3.3101 no . 2_666 C8 H7 3.3980 no . 2_666 C9 H7 3.5992 no . 2_666 C11 H11B 3.3999 no . 2_766 C11 H12A 3.0739 no . 2_766 C11 H20 3.1810 no . 1_655 C12 H11B 3.0336 no . 2_766 C13 H17 3.5265 no . 2_755 C14 H15 3.4941 no . 2_655 C15 H15 3.3272 no . 2_655 C15 H21 3.0674 no . 2_655 C16 H18 3.5221 no . 2_755 C17 H17 3.4620 no . 2_755 C17 H18 3.2756 no . 2_755 C18 H17 3.1170 no . 2_755 C20 H3 3.5369 no . 1_455 C20 H11A 2.8685 no . 1_455 C20 H15 3.3181 no . 2_655 C21 H11A 3.2425 no . 1_455 C21 H15 2.8198 no . 2_655 C22 H15 3.4356 no . 2_655 C23 H23 3.1792 no . 2_665 C23 H24 3.5888 no . 2_665 C24 H23 3.2528 no . 2_665 C25 H12B 3.2438 no . 2_665 C25 H21 3.0092 no . . C25 H22 3.4525 no . . H2 C2 3.5357 no . 2_756 H2 C3 3.3439 no . 2_756 H2 H2 3.4611 no . 2_756 H2 H3 3.1126 no . 2_756 H2 H16 2.8851 no . 2_755 H3 Br1 3.5852 no . 2_756 H3 Br2 3.2932 no . 1_655 H3 C2 3.5171 no . 2_756 H3 C20 3.5369 no . 1_655 H3 H2 3.1126 no . 2_756 H3 H16 3.3804 no . 2_755 H3 H20 2.6355 no . 1_655 H7 Br3 3.2756 no . 1_565 H7 C8 3.3980 no . 2_666 H7 C9 3.5992 no . 2_666 H7 H8 3.3702 no . 2_666 H7 H22 3.3663 no . 2_665 H8 Br3 3.0787 no . 1_565 H8 Br4 2.8925 no . 1_565 H8 C7 3.3101 no . 2_666 H8 H7 3.3702 no . 2_666 H8 H23 3.5855 no . 2_665 H11A Br4 3.1873 no . 1_665 H11A C20 2.8685 no . 1_655 H11A C21 3.2425 no . 1_655 H11A H12A 3.1369 no . 2_766 H11A H20 2.4759 no . 1_655 H11A H21 3.1623 no . 1_655 H11B Br1 3.2167 no . 2_756 H11B Br4 3.2070 no . 2_656 H11B C11 3.3999 no . 2_766 H11B C12 3.0336 no . 2_766 H11B H11B 2.9864 no . 2_766 H11B H12A 2.2879 no . 2_766 H11B H12B 3.2206 no . 2_766 H11B H20 3.4143 no . 1_655 H12A Br1 3.3935 no . 1_565 H12A Br4 3.3203 no . 2_656 H12A C11 3.0739 no . 2_766 H12A H11A 3.1369 no . 2_766 H12A H11B 2.2879 no . 2_766 H12A H12A 3.3986 no . 2_766 H12B Br1 3.1263 no . 1_565 H12B Br4 3.4088 no . 1_665 H12B Cl1 3.5135 no . 1_655 H12B Cl2 2.9469 no . 2_665 H12B C25 3.2438 no . 2_665 H12B H11B 3.2206 no . 2_766 H14 Br2 2.8537 no . . H14 Cl2 3.5007 no . 2_655 H14 H15 3.1028 no . 2_655 H14 H22 3.5073 no . 2_655 H15 C14 3.4941 no . 2_655 H15 C15 3.3272 no . 2_655 H15 C20 3.3181 no . 2_655 H15 C21 2.8198 no . 2_655 H15 C22 3.4356 no . 2_655 H15 H14 3.1028 no . 2_655 H15 H15 2.7495 no . 2_655 H15 H20 3.4249 no . 2_655 H15 H21 2.5861 no . 2_655 H15 H22 3.5981 no . 2_655 H16 Br3 2.8164 no . 2_655 H16 C2 3.3461 no . 2_755 H16 C3 3.5973 no . 2_755 H16 H2 2.8851 no . 2_755 H16 H3 3.3804 no . 2_755 H17 Br1 3.2269 no . 2_755 H17 Cl2 2.9369 no . 1_655 H17 C13 3.5265 no . 2_755 H17 C17 3.4620 no . 2_755 H17 C18 3.1170 no . 2_755 H17 H18 3.1570 no . 2_755 H18 Cl1 3.2254 no . 1_655 H18 C16 3.5221 no . 2_755 H18 C17 3.2756 no . 2_755 H18 H17 3.1570 no . 2_755 H20 Br2 3.4080 no . . H20 C3 3.2061 no . 1_455 H20 C4 3.3808 no . 1_455 H20 C11 3.1810 no . 1_455 H20 H3 2.6355 no . 1_455 H20 H11A 2.4759 no . 1_455 H20 H11B 3.4143 no . 1_455 H20 H15 3.4249 no . 2_655 H21 Cl2 2.9366 no . . H21 C15 3.0674 no . 2_655 H21 C25 3.0092 no . . H21 H11A 3.1623 no . 1_455 H21 H15 2.5861 no . 2_655 H22 Cl1 3.3508 no . 2_565 H22 Cl2 3.2174 no . . H22 C25 3.4525 no . . H22 H7 3.3663 no . 2_665 H22 H14 3.5073 no . 2_655 H22 H15 3.5981 no . 2_655 H23 Br3 3.5808 no . 2_655 H23 Br4 3.1572 no . 2_655 H23 C23 3.1792 no . 2_665 H23 C24 3.2528 no . 2_665 H23 H8 3.5855 no . 2_665 H23 H23 3.0975 no . 2_665 H23 H24 3.1794 no . 2_665 H24 Cl1 3.1102 no . 1_655 H24 C23 3.5888 no . 2_665 H24 H23 3.1794 no . 2_665 #============================================================================== data__Ferg88-2off _database_code_depnum_ccdc_archive 'CCDC 850819' #TrackingRef '- 4.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 Se2 I2' _chemical_formula_moiety 'C24 H18 Se2 I2' _chemical_formula_weight 718.14 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.555(5) _cell_length_b 8.242(4) _cell_length_c 28.147(14) _cell_angle_alpha 90.0000 _cell_angle_beta 97.390(13) _cell_angle_gamma 90.0000 _cell_volume 2198.4(20) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7869 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 29.13 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.170 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344.00 _exptl_absorpt_coefficient_mu 6.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.290 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 19164 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_theta_max 29.10 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.869 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5470 _reflns_number_gt 3940 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.3043 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5113 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1327P)^2^+20.2076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.290 _refine_diff_density_min -2.480 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Se Se -0.093 2.226 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 I(1) I 0.44033(11) 0.06526(12) 0.18758(4) 0.0309(3) Uani 1.00 4 d . . . I(2) I 0.21132(12) -0.11320(15) 0.21514(4) 0.0401(3) Uani 1.00 4 d . . . Se(1) Se 0.67936(16) 0.2172(2) 0.15150(6) 0.0297(4) Uani 1.00 4 d . . . Se(2) Se 0.91211(16) 0.0505(2) 0.08788(6) 0.0310(4) Uani 1.00 4 d . . . C(1) C 0.5813(17) 0.249(2) 0.0856(6) 0.034(4) Uani 1.00 4 d . . . C(2) C 0.4549(18) 0.3362(19) 0.0826(6) 0.033(4) Uani 1.00 4 d . . . C(3) C 0.3739(15) 0.3652(19) 0.0396(5) 0.028(3) Uani 1.00 4 d . . . C(4) C 0.4138(15) 0.3079(17) -0.0015(6) 0.028(3) Uani 1.00 4 d . . . C(5) C 0.5443(15) 0.220(2) 0.0014(6) 0.030(3) Uani 1.00 4 d . . . C(6) C 0.5709(16) 0.170(2) -0.0457(6) 0.033(4) Uani 1.00 4 d . . . C(7) C 0.6898(18) 0.077(2) -0.0486(6) 0.038(4) Uani 1.00 4 d . . . C(8) C 0.7835(16) 0.0488(18) -0.0088(6) 0.029(3) Uani 1.00 4 d . . . C(9) C 0.7609(16) 0.0988(17) 0.0380(5) 0.025(3) Uani 1.00 4 d . . . C(10) C 0.6340(14) 0.1862(17) 0.0444(5) 0.023(3) Uani 1.00 4 d . . . C(11) C 0.3461(16) 0.3178(20) -0.0528(5) 0.028(3) Uani 1.00 4 d . . . C(12) C 0.4517(15) 0.226(2) -0.0818(6) 0.034(4) Uani 1.00 4 d . . . C(13) C 0.6767(17) 0.440(2) 0.1743(6) 0.034(4) Uani 1.00 4 d . . . C(14) C 0.7915(17) 0.5322(19) 0.1668(6) 0.030(3) Uani 1.00 4 d . . . C(15) C 0.8051(15) 0.684(3) 0.1855(6) 0.042(4) Uani 1.00 4 d . . . C(16) C 0.7030(17) 0.7408(20) 0.2150(6) 0.036(4) Uani 1.00 4 d . . . C(17) C 0.5889(20) 0.641(2) 0.2226(6) 0.039(4) Uani 1.00 4 d . . . C(18) C 0.5760(18) 0.497(2) 0.2029(6) 0.034(4) Uani 1.00 4 d . . . C(19) C 0.9927(17) 0.261(2) 0.0955(6) 0.034(4) Uani 1.00 4 d . . . C(20) C 0.9564(17) 0.386(2) 0.0592(6) 0.033(3) Uani 1.00 4 d . . . C(21) C 1.0221(17) 0.5371(19) 0.0695(6) 0.030(3) Uani 1.00 4 d . . . C(22) C 1.1218(16) 0.572(2) 0.1094(6) 0.039(4) Uani 1.00 4 d . . . C(23) C 1.1513(18) 0.449(2) 0.1432(6) 0.040(4) Uani 1.00 4 d . . . C(24) C 1.0900(19) 0.299(2) 0.1354(7) 0.039(4) Uani 1.00 4 d . . . H(2) H 0.4242 0.3764 0.1112 0.040 Uiso 1.00 4 calc R . . H(3) H 0.2891 0.4260 0.0387 0.033 Uiso 1.00 4 calc R . . H(7) H 0.7064 0.0331 -0.0785 0.045 Uiso 1.00 4 calc R . . H(8) H 0.8683 -0.0073 -0.0124 0.035 Uiso 1.00 4 calc R . . H(11A) H 0.3345 0.4321 -0.0634 0.033 Uiso 1.00 4 calc R . . H(11B) H 0.2526 0.2643 -0.0569 0.033 Uiso 1.00 4 calc R . . H(12A) H 0.4047 0.1323 -0.0991 0.041 Uiso 1.00 4 calc R . . H(12B) H 0.4869 0.2997 -0.1054 0.041 Uiso 1.00 4 calc R . . H(14) H 0.8607 0.4901 0.1487 0.035 Uiso 1.00 4 calc R . . H(15) H 0.8809 0.7523 0.1792 0.050 Uiso 1.00 4 calc R . . H(16) H 0.7126 0.8453 0.2293 0.044 Uiso 1.00 4 calc R . . H(17) H 0.5211 0.6773 0.2421 0.047 Uiso 1.00 4 calc R . . H(18) H 0.4982 0.4298 0.2078 0.041 Uiso 1.00 4 calc R . . H(20) H 0.8934 0.3663 0.0308 0.039 Uiso 1.00 4 calc R . . H(21) H 0.9968 0.6230 0.0476 0.036 Uiso 1.00 4 calc R . . H(22) H 1.1671 0.6742 0.1132 0.047 Uiso 1.00 4 calc R . . H(23) H 1.2140 0.4687 0.1716 0.048 Uiso 1.00 4 calc R . . H(24) H 1.1149 0.2162 0.1585 0.047 Uiso 1.00 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0298(6) 0.0308(6) 0.0321(6) 0.0006(4) 0.0042(4) -0.0001(4) I(2) 0.0386(7) 0.0398(7) 0.0432(7) -0.0079(5) 0.0097(5) -0.0020(5) Se(1) 0.0254(8) 0.0334(9) 0.0305(8) 0.0023(6) 0.0036(6) 0.0003(7) Se(2) 0.0244(8) 0.0338(9) 0.0347(9) 0.0044(6) 0.0031(6) -0.0006(7) C(1) 0.028(8) 0.041(9) 0.034(8) 0.002(7) 0.006(6) -0.016(8) C(2) 0.040(9) 0.023(8) 0.041(9) -0.005(6) 0.016(7) -0.017(7) C(3) 0.021(7) 0.029(8) 0.034(8) 0.006(6) 0.006(6) 0.000(7) C(4) 0.020(7) 0.014(6) 0.048(9) -0.004(5) 0.001(6) 0.006(6) C(5) 0.017(7) 0.037(9) 0.034(8) -0.002(6) -0.001(6) 0.002(7) C(6) 0.023(8) 0.036(9) 0.040(9) -0.007(6) 0.004(6) 0.004(7) C(7) 0.031(9) 0.050(11) 0.032(8) -0.002(7) 0.006(6) 0.014(8) C(8) 0.023(7) 0.022(7) 0.044(9) 0.000(6) 0.010(6) -0.012(7) C(9) 0.032(8) 0.021(7) 0.023(7) 0.002(6) 0.003(6) -0.001(6) C(10) 0.014(6) 0.024(7) 0.032(7) 0.001(5) 0.000(5) 0.001(6) C(11) 0.024(7) 0.032(8) 0.027(7) -0.003(6) 0.003(6) -0.007(7) C(12) 0.019(7) 0.038(9) 0.043(9) 0.009(6) -0.002(6) -0.001(8) C(13) 0.028(8) 0.040(9) 0.033(8) -0.000(7) 0.007(6) 0.011(7) C(14) 0.029(8) 0.025(8) 0.033(8) -0.001(6) 0.001(6) -0.001(7) C(15) 0.008(7) 0.070(13) 0.045(9) -0.001(7) -0.007(6) 0.010(9) C(16) 0.034(9) 0.024(8) 0.045(9) 0.006(6) -0.021(7) 0.006(7) C(17) 0.044(10) 0.033(9) 0.042(9) 0.018(8) 0.007(7) -0.004(8) C(18) 0.036(9) 0.040(9) 0.028(8) 0.005(7) 0.013(6) 0.001(7) C(19) 0.030(8) 0.037(9) 0.034(8) 0.004(7) 0.002(6) 0.006(7) C(20) 0.032(8) 0.032(8) 0.036(8) 0.003(7) 0.011(6) 0.011(7) C(21) 0.031(8) 0.029(8) 0.030(8) -0.001(6) 0.009(6) 0.003(7) C(22) 0.017(7) 0.057(11) 0.046(10) -0.000(7) 0.011(7) 0.005(9) C(23) 0.029(8) 0.052(11) 0.038(9) 0.018(8) -0.004(7) -0.016(8) C(24) 0.046(10) 0.032(9) 0.041(9) 0.004(8) 0.017(8) 0.004(8) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) I(2) 2.8267(19) yes . . I(1) Se(1) 2.901(2) yes . . Se(1) C(1) 1.985(15) yes . . Se(1) C(13) 1.948(17) yes . . Se(2) C(9) 1.922(14) yes . . Se(2) C(19) 1.902(17) yes . . C(1) C(2) 1.40(2) yes . . C(1) C(10) 1.42(2) yes . . C(2) C(3) 1.37(2) yes . . C(3) C(4) 1.35(2) yes . . C(4) C(5) 1.44(2) yes . . C(4) C(11) 1.51(2) yes . . C(5) C(6) 1.44(2) yes . . C(5) C(10) 1.416(20) yes . . C(6) C(7) 1.38(2) yes . . C(6) C(12) 1.50(2) yes . . C(7) C(8) 1.36(2) yes . . C(8) C(9) 1.42(2) yes . . C(9) C(10) 1.44(2) yes . . C(11) C(12) 1.57(2) yes . . C(13) C(14) 1.37(2) yes . . C(13) C(18) 1.41(2) yes . . C(14) C(15) 1.36(3) yes . . C(15) C(16) 1.44(2) yes . . C(16) C(17) 1.41(2) yes . . C(17) C(18) 1.31(2) yes . . C(19) C(20) 1.46(2) yes . . C(19) C(24) 1.40(2) yes . . C(20) C(21) 1.41(2) yes . . C(21) C(22) 1.41(2) yes . . C(22) C(23) 1.39(3) yes . . C(23) C(24) 1.37(3) yes . . C(2) H(2) 0.950 yes . . C(3) H(3) 0.950 yes . . C(7) H(7) 0.950 yes . . C(8) H(8) 0.950 yes . . C(11) H(11A) 0.990 yes . . C(11) H(11B) 0.990 yes . . C(12) H(12A) 0.990 yes . . C(12) H(12B) 0.990 yes . . C(14) H(14) 0.950 yes . . C(15) H(15) 0.950 yes . . C(16) H(16) 0.950 yes . . C(17) H(17) 0.950 yes . . C(18) H(18) 0.950 yes . . C(20) H(20) 0.950 yes . . C(21) H(21) 0.950 yes . . C(22) H(22) 0.950 yes . . C(23) H(23) 0.950 yes . . C(24) H(24) 0.950 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I(2) I(1) Se(1) 173.22(6) yes . . . I(1) Se(1) C(1) 94.9(5) yes . . . I(1) Se(1) C(13) 104.3(5) yes . . . C(1) Se(1) C(13) 99.0(7) yes . . . C(9) Se(2) C(19) 98.5(6) yes . . . Se(1) C(1) C(2) 115.2(12) yes . . . Se(1) C(1) C(10) 122.6(11) yes . . . C(2) C(1) C(10) 122.1(14) yes . . . C(1) C(2) C(3) 121.9(16) yes . . . C(2) C(3) C(4) 120.4(14) yes . . . C(3) C(4) C(5) 117.8(14) yes . . . C(3) C(4) C(11) 132.0(13) yes . . . C(5) C(4) C(11) 110.1(14) yes . . . C(4) C(5) C(6) 110.2(13) yes . . . C(4) C(5) C(10) 125.0(15) yes . . . C(6) C(5) C(10) 124.7(14) yes . . . C(5) C(6) C(7) 117.1(14) yes . . . C(5) C(6) C(12) 109.1(13) yes . . . C(7) C(6) C(12) 133.8(16) yes . . . C(6) C(7) C(8) 120.5(16) yes . . . C(7) C(8) C(9) 123.3(15) yes . . . Se(2) C(9) C(8) 115.2(11) yes . . . Se(2) C(9) C(10) 125.3(11) yes . . . C(8) C(9) C(10) 119.4(13) yes . . . C(1) C(10) C(5) 112.7(13) yes . . . C(1) C(10) C(9) 132.6(13) yes . . . C(5) C(10) C(9) 114.8(13) yes . . . C(4) C(11) C(12) 104.3(12) yes . . . C(6) C(12) C(11) 106.3(13) yes . . . Se(1) C(13) C(14) 115.2(12) yes . . . Se(1) C(13) C(18) 122.6(13) yes . . . C(14) C(13) C(18) 121.5(16) yes . . . C(13) C(14) C(15) 119.2(16) yes . . . C(14) C(15) C(16) 119.0(16) yes . . . C(15) C(16) C(17) 119.7(16) yes . . . C(16) C(17) C(18) 120.0(17) yes . . . C(13) C(18) C(17) 120.5(17) yes . . . Se(2) C(19) C(20) 120.5(11) yes . . . Se(2) C(19) C(24) 120.7(13) yes . . . C(20) C(19) C(24) 118.8(15) yes . . . C(19) C(20) C(21) 114.8(14) yes . . . C(20) C(21) C(22) 125.5(15) yes . . . C(21) C(22) C(23) 117.1(17) yes . . . C(22) C(23) C(24) 120.1(16) yes . . . C(19) C(24) C(23) 123.6(16) yes . . . C(1) C(2) H(2) 119.047 yes . . . C(3) C(2) H(2) 119.054 yes . . . C(2) C(3) H(3) 119.791 yes . . . C(4) C(3) H(3) 119.797 yes . . . C(6) C(7) H(7) 119.758 yes . . . C(8) C(7) H(7) 119.767 yes . . . C(7) C(8) H(8) 118.343 yes . . . C(9) C(8) H(8) 118.333 yes . . . C(4) C(11) H(11A) 110.891 yes . . . C(4) C(11) H(11B) 110.897 yes . . . C(12) C(11) H(11A) 110.888 yes . . . C(12) C(11) H(11B) 110.892 yes . . . H(11A) C(11) H(11B) 108.922 yes . . . C(6) C(12) H(12A) 110.480 yes . . . C(6) C(12) H(12B) 110.476 yes . . . C(11) C(12) H(12A) 110.479 yes . . . C(11) C(12) H(12B) 110.476 yes . . . H(12A) C(12) H(12B) 108.664 yes . . . C(13) C(14) H(14) 120.390 yes . . . C(15) C(14) H(14) 120.387 yes . . . C(14) C(15) H(15) 120.506 yes . . . C(16) C(15) H(15) 120.514 yes . . . C(15) C(16) H(16) 120.162 yes . . . C(17) C(16) H(16) 120.170 yes . . . C(16) C(17) H(17) 120.002 yes . . . C(18) C(17) H(17) 120.005 yes . . . C(13) C(18) H(18) 119.741 yes . . . C(17) C(18) H(18) 119.733 yes . . . C(19) C(20) H(20) 122.606 yes . . . C(21) C(20) H(20) 122.606 yes . . . C(20) C(21) H(21) 117.240 yes . . . C(22) C(21) H(21) 117.243 yes . . . C(21) C(22) H(22) 121.458 yes . . . C(23) C(22) H(22) 121.441 yes . . . C(22) C(23) H(23) 119.966 yes . . . C(24) C(23) H(23) 119.969 yes . . . C(19) C(24) H(24) 118.226 yes . . . C(23) C(24) H(24) 118.223 yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I(1) Se(1) C(1) C(2) 55.8(10) no . . . . I(1) Se(1) C(1) C(10) -123.2(11) no . . . . I(1) Se(1) C(13) C(18) 1.4(11) no . . . . C(1) Se(1) C(13) C(14) -90.4(11) no . . . . C(1) Se(1) C(13) C(18) 98.9(11) no . . . . C(13) Se(1) C(1) C(2) -49.7(12) no . . . . C(13) Se(1) C(1) C(10) 131.4(12) no . . . . C(9) Se(2) C(19) C(20) -15.4(13) no . . . . C(19) Se(2) C(9) C(8) 102.8(10) no . . . . C(19) Se(2) C(9) C(10) -74.1(12) no . . . . Se(1) C(1) C(10) C(9) -3(2) no . . . . C(2) C(1) C(10) C(5) -1(2) no . . . . C(10) C(1) C(2) C(3) 0(2) no . . . . C(1) C(2) C(3) C(4) 1(2) no . . . . C(2) C(3) C(4) C(5) -1(2) no . . . . C(3) C(4) C(5) C(10) 1(2) no . . . . C(5) C(4) C(11) C(12) -0.5(15) no . . . . C(11) C(4) C(5) C(6) 0.7(17) no . . . . C(4) C(5) C(6) C(12) -0.5(17) no . . . . C(4) C(5) C(10) C(1) 0(2) no . . . . C(6) C(5) C(10) C(9) 2(2) no . . . . C(10) C(5) C(6) C(7) 3(2) no . . . . C(5) C(6) C(7) C(8) -6(2) no . . . . C(5) C(6) C(12) C(11) 0.2(17) no . . . . C(6) C(7) C(8) C(9) 5(3) no . . . . C(7) C(8) C(9) C(10) -1(2) no . . . . Se(2) C(9) C(10) C(1) -4(2) no . . . . C(8) C(9) C(10) C(5) -2.5(19) no . . . . C(4) C(11) C(12) C(6) 0.2(15) no . . . . C(14) C(13) C(18) C(17) 1(2) no . . . . C(18) C(13) C(14) C(15) -3(2) no . . . . C(13) C(14) C(15) C(16) 4(2) no . . . . C(14) C(15) C(16) C(17) -2(2) no . . . . C(15) C(16) C(17) C(18) -0(2) no . . . . C(16) C(17) C(18) C(13) 1(2) no . . . . C(20) C(19) C(24) C(23) 2(3) no . . . . C(24) C(19) C(20) C(21) -2(2) no . . . . C(19) C(20) C(21) C(22) 4(2) no . . . . C(20) C(21) C(22) C(23) -4(3) no . . . . C(21) C(22) C(23) C(24) 4(2) no . . . . C(22) C(23) C(24) C(19) -2(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Se(1) Se(2) 3.326(3) yes . . Se(1) C(9) 3.522(15) yes . . Se(1) C(19) 3.577(17) yes . . Se(2) C(1) 3.554(17) yes . . C(1) C(4) 2.79(2) yes . . C(2) C(5) 2.71(2) yes . . C(2) C(13) 3.24(2) yes . . C(3) C(10) 2.88(2) yes . . C(5) C(8) 2.73(2) yes . . C(6) C(9) 2.85(2) yes . . C(7) C(10) 2.88(2) yes . . C(9) C(20) 3.03(2) yes . . C(10) C(19) 3.60(2) yes . . C(10) C(20) 3.47(2) yes . . C(13) C(16) 2.73(2) yes . . C(14) C(17) 2.79(3) yes . . C(15) C(18) 2.77(2) yes . . C(19) C(22) 2.84(3) yes . . C(20) C(23) 2.86(2) yes . . C(21) C(24) 2.72(2) yes . . C(2) C(11) 3.59(2) yes . 3_665 C(4) C(8) 3.52(2) yes . 3_655 C(6) C(10) 3.53(2) yes . 3_655 C(8) C(4) 3.52(2) yes . 3_655 C(10) C(6) 3.53(2) yes . 3_655 C(11) C(2) 3.59(2) yes . 3_665 C(11) C(14) 3.53(2) yes . 3_665 C(13) C(16) 3.58(2) yes . 2_645 C(14) C(11) 3.53(2) yes . 3_665 C(16) C(13) 3.58(2) yes . 2_655 I(1) H(2) 3.3379 yes . . I(1) H(18) 3.0949 yes . . Se(1) H(2) 2.8711 yes . . Se(1) H(14) 2.8465 yes . . Se(1) H(18) 3.0468 yes . . Se(2) H(8) 2.8406 yes . . Se(2) H(20) 3.0511 yes . . Se(2) H(24) 2.9290 yes . . C(1) H(3) 3.2724 yes . . C(2) H(18) 3.5786 yes . . C(3) H(11A) 2.9266 yes . . C(3) H(11B) 2.9329 yes . . C(4) H(2) 3.2098 yes . . C(4) H(12A) 3.0969 yes . . C(4) H(12B) 3.0941 yes . . C(5) H(3) 3.2543 yes . . C(5) H(7) 3.2761 yes . . C(5) H(11A) 3.0761 yes . . C(5) H(11B) 3.0697 yes . . C(5) H(12A) 3.0562 yes . . C(5) H(12B) 3.0581 yes . . C(5) H(20) 3.5430 yes . . C(6) H(8) 3.2254 yes . . C(6) H(11A) 3.1188 yes . . C(6) H(11B) 3.1162 yes . . C(7) H(12A) 2.9413 yes . . C(7) H(12B) 2.9796 yes . . C(8) H(20) 2.9818 yes . . C(9) H(7) 3.2991 yes . . C(9) H(20) 2.5630 yes . . C(10) H(2) 3.3141 yes . . C(10) H(8) 3.3211 yes . . C(10) H(20) 2.9552 yes . . C(11) H(3) 2.8452 yes . . C(12) H(7) 2.8985 yes . . C(13) H(2) 2.8553 yes . . C(13) H(15) 3.2207 yes . . C(13) H(17) 3.2245 yes . . C(14) H(16) 3.2655 yes . . C(14) H(18) 3.2753 yes . . C(15) H(17) 3.3176 yes . . C(16) H(14) 3.2773 yes . . C(16) H(18) 3.2154 yes . . C(17) H(15) 3.3164 yes . . C(18) H(2) 2.9638 yes . . C(18) H(14) 3.2845 yes . . C(18) H(16) 3.2036 yes . . C(19) H(14) 2.8066 yes . . C(19) H(21) 3.2740 yes . . C(19) H(23) 3.2886 yes . . C(20) H(14) 2.9186 yes . . C(20) H(22) 3.3510 yes . . C(20) H(24) 3.3116 yes . . C(21) H(14) 2.8964 yes . . C(21) H(23) 3.2542 yes . . C(22) H(14) 2.9348 yes . . C(22) H(15) 3.5422 yes . . C(22) H(20) 3.3580 yes . . C(22) H(24) 3.2431 yes . . C(23) H(14) 2.8225 yes . . C(23) H(21) 3.2353 yes . . C(24) H(14) 2.7630 yes . . C(24) H(20) 3.3293 yes . . C(24) H(22) 3.2595 yes . . H(2) H(3) 2.3051 yes . . H(2) H(18) 2.7560 yes . . H(3) H(11A) 2.9618 yes . . H(3) H(11B) 2.9837 yes . . H(7) H(8) 2.2859 yes . . H(7) H(12A) 2.9806 yes . . H(7) H(12B) 3.0646 yes . . H(8) H(20) 3.3087 yes . . H(11A) H(12A) 2.7818 yes . . H(11A) H(12B) 2.2697 yes . . H(11B) H(12A) 2.2698 yes . . H(11B) H(12B) 2.7835 yes . . H(14) H(15) 2.3240 yes . . H(14) H(20) 3.5236 yes . . H(14) H(21) 3.4574 yes . . H(14) H(22) 3.5540 yes . . H(14) H(23) 3.3598 yes . . H(14) H(24) 3.3018 yes . . H(15) H(16) 2.3960 yes . . H(15) H(22) 3.5580 yes . . H(16) H(17) 2.3589 yes . . H(17) H(18) 2.2549 yes . . H(20) H(21) 2.3572 yes . . H(21) H(22) 2.3379 yes . . H(22) H(23) 2.3634 yes . . H(23) H(24) 2.2966 yes . . I(1) H(7) 3.3074 yes . 3_655 I(1) H(12A) 3.4634 yes . 3_655 I(1) H(16) 3.2630 yes . 1_545 I(1) H(17) 3.5876 yes . 1_545 I(1) H(24) 3.3518 yes . 1_455 I(2) H(15) 3.3760 yes . 1_445 I(2) H(17) 3.4268 yes . 1_545 I(2) H(17) 3.5782 yes . 2_545 I(2) H(18) 3.1556 yes . 2_545 I(2) H(22) 3.3425 yes . 1_445 I(2) H(23) 3.2469 yes . 2_645 I(2) H(24) 3.2226 yes . 1_455 Se(1) H(12A) 3.2888 yes . 3_655 Se(1) H(16) 3.5424 yes . 2_645 Se(2) H(8) 3.1919 yes . 3_755 Se(2) H(11B) 3.1013 yes . 3_655 Se(2) H(12A) 3.4325 yes . 3_655 Se(2) H(15) 3.5978 yes . 1_545 C(1) H(7) 3.5876 yes . 3_655 C(1) H(11A) 2.8398 yes . 3_665 C(1) H(12A) 3.1695 yes . 3_655 C(2) H(7) 3.4072 yes . 3_655 C(2) H(11A) 2.8754 yes . 3_665 C(2) H(12B) 3.1036 yes . 3_665 C(3) H(7) 3.5754 yes . 3_655 C(3) H(11A) 3.2439 yes . 3_665 C(3) H(12B) 3.4920 yes . 3_665 C(4) H(11A) 3.5469 yes . 3_665 C(5) H(3) 3.5758 yes . 3_665 C(5) H(11A) 3.4763 yes . 3_665 C(6) H(3) 3.5841 yes . 3_665 C(6) H(22) 3.5692 yes . 3_765 C(7) H(22) 3.1636 yes . 3_765 C(8) H(8) 3.3217 yes . 3_755 C(8) H(11B) 3.2188 yes . 3_655 C(9) H(11B) 3.0457 yes . 3_655 C(9) H(12A) 3.1290 yes . 3_655 C(10) H(11A) 3.1992 yes . 3_665 C(10) H(12A) 3.0903 yes . 3_655 C(11) H(14) 3.5107 yes . 3_665 C(11) H(20) 3.5728 yes . 3_665 C(11) H(21) 3.3349 yes . 3_665 C(13) H(11A) 3.2834 yes . 3_665 C(13) H(12B) 3.1654 yes . 3_665 C(13) H(16) 2.8907 yes . 2_645 C(14) H(11A) 3.0181 yes . 3_665 C(14) H(11B) 3.4963 yes . 3_665 C(14) H(12B) 3.2861 yes . 3_665 C(14) H(16) 3.3103 yes . 2_645 C(15) H(12A) 3.3113 yes . 3_665 C(15) H(12B) 3.3571 yes . 3_665 C(16) H(12A) 3.4542 yes . 3_665 C(16) H(12B) 3.3887 yes . 3_665 C(17) H(12B) 3.3221 yes . 3_665 C(17) H(16) 3.2699 yes . 2_645 C(18) H(12B) 3.2057 yes . 3_665 C(18) H(16) 2.8797 yes . 2_645 C(18) H(23) 3.4652 yes . 1_455 C(19) H(8) 3.5239 yes . 3_755 C(20) H(3) 3.3199 yes . 1_655 C(20) H(11A) 3.1750 yes . 3_665 C(20) H(11B) 3.5040 yes . 3_665 C(20) H(21) 3.0953 yes . 3_765 C(21) H(3) 2.9438 yes . 1_655 C(21) H(11A) 3.3991 yes . 3_665 C(21) H(11B) 3.0745 yes . 3_665 C(21) H(20) 3.1379 yes . 3_765 C(21) H(21) 3.5314 yes . 3_765 C(22) H(2) 3.3016 yes . 1_655 C(22) H(3) 2.9613 yes . 1_655 C(23) H(2) 2.9272 yes . 1_655 C(23) H(3) 3.3775 yes . 1_655 C(23) H(18) 3.5730 yes . 1_655 C(24) H(2) 3.4111 yes . 1_655 H(2) C(22) 3.3016 yes . 1_455 H(2) C(23) 2.9272 yes . 1_455 H(2) C(24) 3.4111 yes . 1_455 H(2) H(11A) 3.2271 yes . 3_665 H(2) H(12B) 2.8124 yes . 3_665 H(2) H(22) 3.4783 yes . 1_455 H(2) H(23) 2.8952 yes . 1_455 H(3) C(5) 3.5758 yes . 3_665 H(3) C(6) 3.5841 yes . 3_665 H(3) C(20) 3.3199 yes . 1_455 H(3) C(21) 2.9438 yes . 1_455 H(3) C(22) 2.9613 yes . 1_455 H(3) C(23) 3.3775 yes . 1_455 H(3) H(12B) 3.4897 yes . 3_665 H(3) H(20) 2.9876 yes . 3_665 H(3) H(21) 3.2678 yes . 1_455 H(3) H(21) 3.4378 yes . 3_665 H(3) H(22) 3.2502 yes . 1_455 H(7) I(1) 3.3074 yes . 3_655 H(7) C(1) 3.5876 yes . 3_655 H(7) C(2) 3.4072 yes . 3_655 H(7) C(3) 3.5754 yes . 3_655 H(7) H(22) 2.9215 yes . 3_765 H(8) Se(2) 3.1919 yes . 3_755 H(8) C(8) 3.3217 yes . 3_755 H(8) C(19) 3.5239 yes . 3_755 H(8) H(8) 2.5273 yes . 3_755 H(8) H(11B) 3.1949 yes . 3_655 H(11A) C(1) 2.8398 yes . 3_665 H(11A) C(2) 2.8754 yes . 3_665 H(11A) C(3) 3.2439 yes . 3_665 H(11A) C(4) 3.5469 yes . 3_665 H(11A) C(5) 3.4763 yes . 3_665 H(11A) C(10) 3.1992 yes . 3_665 H(11A) C(13) 3.2834 yes . 3_665 H(11A) C(14) 3.0181 yes . 3_665 H(11A) C(20) 3.1750 yes . 3_665 H(11A) C(21) 3.3991 yes . 3_665 H(11A) H(2) 3.2271 yes . 3_665 H(11A) H(14) 2.9167 yes . 3_665 H(11A) H(20) 2.9758 yes . 3_665 H(11A) H(21) 3.2850 yes . 3_665 H(11B) Se(2) 3.1013 yes . 3_655 H(11B) C(8) 3.2188 yes . 3_655 H(11B) C(9) 3.0457 yes . 3_655 H(11B) C(14) 3.4963 yes . 3_665 H(11B) C(20) 3.5040 yes . 3_665 H(11B) C(21) 3.0745 yes . 3_665 H(11B) H(8) 3.1949 yes . 3_655 H(11B) H(14) 3.3506 yes . 3_665 H(11B) H(15) 3.5179 yes . 3_665 H(11B) H(20) 3.4663 yes . 3_665 H(11B) H(21) 2.6019 yes . 3_665 H(12A) I(1) 3.4634 yes . 3_655 H(12A) Se(1) 3.2888 yes . 3_655 H(12A) Se(2) 3.4325 yes . 3_655 H(12A) C(1) 3.1695 yes . 3_655 H(12A) C(9) 3.1290 yes . 3_655 H(12A) C(10) 3.0903 yes . 3_655 H(12A) C(15) 3.3113 yes . 3_665 H(12A) C(16) 3.4542 yes . 3_665 H(12A) H(15) 3.4433 yes . 3_665 H(12B) C(2) 3.1036 yes . 3_665 H(12B) C(3) 3.4920 yes . 3_665 H(12B) C(13) 3.1654 yes . 3_665 H(12B) C(14) 3.2861 yes . 3_665 H(12B) C(15) 3.3571 yes . 3_665 H(12B) C(16) 3.3887 yes . 3_665 H(12B) C(17) 3.3221 yes . 3_665 H(12B) C(18) 3.2057 yes . 3_665 H(12B) H(2) 2.8124 yes . 3_665 H(12B) H(3) 3.4897 yes . 3_665 H(12B) H(22) 3.3482 yes . 3_765 H(14) C(11) 3.5107 yes . 3_665 H(14) H(11A) 2.9167 yes . 3_665 H(14) H(11B) 3.3506 yes . 3_665 H(15) I(2) 3.3760 yes . 1_665 H(15) Se(2) 3.5978 yes . 1_565 H(15) H(11B) 3.5179 yes . 3_665 H(15) H(12A) 3.4433 yes . 3_665 H(15) H(18) 3.5554 yes . 2_655 H(16) I(1) 3.2630 yes . 1_565 H(16) Se(1) 3.5424 yes . 2_655 H(16) C(13) 2.8907 yes . 2_655 H(16) C(14) 3.3103 yes . 2_655 H(16) C(17) 3.2699 yes . 2_655 H(16) C(18) 2.8797 yes . 2_655 H(16) H(18) 3.1621 yes . 2_655 H(17) I(1) 3.5876 yes . 1_565 H(17) I(2) 3.4268 yes . 1_565 H(17) I(2) 3.5782 yes . 2_555 H(17) H(24) 3.2494 yes . 2_655 H(18) I(2) 3.1556 yes . 2_555 H(18) C(23) 3.5730 yes . 1_455 H(18) H(15) 3.5554 yes . 2_645 H(18) H(16) 3.1621 yes . 2_645 H(18) H(23) 2.7931 yes . 1_455 H(20) C(11) 3.5728 yes . 3_665 H(20) C(21) 3.1379 yes . 3_765 H(20) H(3) 2.9876 yes . 3_665 H(20) H(11A) 2.9758 yes . 3_665 H(20) H(11B) 3.4663 yes . 3_665 H(20) H(20) 3.5965 yes . 3_765 H(20) H(21) 2.5639 yes . 3_765 H(21) C(11) 3.3349 yes . 3_665 H(21) C(20) 3.0953 yes . 3_765 H(21) C(21) 3.5314 yes . 3_765 H(21) H(3) 3.2678 yes . 1_655 H(21) H(3) 3.4378 yes . 3_665 H(21) H(11A) 3.2850 yes . 3_665 H(21) H(11B) 2.6019 yes . 3_665 H(21) H(20) 2.5639 yes . 3_765 H(21) H(21) 3.3653 yes . 3_765 H(22) I(2) 3.3425 yes . 1_665 H(22) C(6) 3.5692 yes . 3_765 H(22) C(7) 3.1636 yes . 3_765 H(22) H(2) 3.4783 yes . 1_655 H(22) H(3) 3.2502 yes . 1_655 H(22) H(7) 2.9215 yes . 3_765 H(22) H(12B) 3.3482 yes . 3_765 H(23) I(2) 3.2469 yes . 2_655 H(23) C(18) 3.4652 yes . 1_655 H(23) H(2) 2.8952 yes . 1_655 H(23) H(18) 2.7931 yes . 1_655 H(24) I(1) 3.3518 yes . 1_655 H(24) I(2) 3.2226 yes . 1_655 H(24) H(17) 3.2494 yes . 2_645 #============================================================================== data_Ferg-115-B_off _database_code_depnum_ccdc_archive 'CCDC 850820' #TrackingRef '- 5.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 I2 S Se' _chemical_formula_moiety 'C24 H18 I2 S Se' _chemical_formula_weight 671.24 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.578(4) _cell_length_b 8.184(3) _cell_length_c 28.084(10) _cell_angle_alpha 90.0000 _cell_angle_beta 96.485(9) _cell_angle_gamma 90.0000 _cell_volume 2187.4(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9329 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 29.13 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272.00 _exptl_absorpt_coefficient_mu 4.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.448 _exptl_absorpt_correction_T_max 0.911 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.257 _diffrn_reflns_number 15951 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3848 _reflns_number_gt 3502 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1625 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3848 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.660 _refine_diff_density_min -1.760 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Se Se -0.0929 2.2259 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.4742 1.8119 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.44017(4) 0.44093(5) 0.187097(16) 0.0251(2) Uani 1.0 4 d . . . I2 I 0.21441(5) 0.62232(6) 0.215994(19) 0.0345(3) Uani 1.0 4 d . . . Se1 Se 0.67832(7) 0.28576(8) 0.14957(3) 0.0254(3) Uani 1.0 4 d . . . S1 S 0.90026(16) 0.44059(18) 0.08252(6) 0.0206(4) Uani 1.0 4 d . . . C1 C 0.5835(7) 0.2502(8) 0.0853(3) 0.0205(14) Uani 1.0 4 d . . . C2 C 0.4563(7) 0.1682(9) 0.0834(3) 0.0253(15) Uani 1.0 4 d . . . C3 C 0.3707(7) 0.1374(9) 0.0407(3) 0.0288(17) Uani 1.0 4 d . . . C4 C 0.4143(7) 0.1942(8) -0.0015(3) 0.0241(15) Uani 1.0 4 d . . . C5 C 0.5437(7) 0.2792(8) 0.0002(3) 0.0185(14) Uani 1.0 4 d . . . C6 C 0.5684(7) 0.3305(8) -0.0459(3) 0.0224(15) Uani 1.0 4 d . . . C7 C 0.6901(7) 0.4141(9) -0.0516(3) 0.0272(16) Uani 1.0 4 d . . . C8 C 0.7846(7) 0.4465(8) -0.0104(3) 0.0234(15) Uani 1.0 4 d . . . C9 C 0.7623(7) 0.3953(8) 0.0352(3) 0.0228(15) Uani 1.0 4 d . . . C10 C 0.6347(7) 0.3104(8) 0.0433(3) 0.0201(14) Uani 1.0 4 d . . . C11 C 0.3474(8) 0.1843(9) -0.0520(3) 0.0273(16) Uani 1.0 4 d . . . C12 C 0.4499(8) 0.2730(9) -0.0824(3) 0.0277(16) Uani 1.0 4 d . . . C13 C 0.6765(7) 0.0649(8) 0.1745(3) 0.0243(15) Uani 1.0 4 d . . . C14 C 0.5762(8) 0.0099(9) 0.2031(3) 0.0333(18) Uani 1.0 4 d . . . C15 C 0.5867(7) -0.1293(10) 0.2241(3) 0.0308(18) Uani 1.0 4 d . . . C16 C 0.7038(9) -0.2397(10) 0.2156(3) 0.038(2) Uani 1.0 4 d . . . C17 C 0.8039(7) -0.1788(9) 0.1860(3) 0.0233(15) Uani 1.0 4 d . . . C18 C 0.7913(7) -0.0370(10) 0.1673(3) 0.0327(18) Uani 1.0 4 d . . . C19 C 0.9823(7) 0.2426(9) 0.0909(3) 0.0238(15) Uani 1.0 4 d . . . C20 C 1.0758(7) 0.2259(10) 0.1318(3) 0.0311(17) Uani 1.0 4 d . . . C21 C 1.1439(8) 0.0734(11) 0.1411(3) 0.036(2) Uani 1.0 4 d . . . C22 C 1.1171(8) -0.0542(10) 0.1105(3) 0.0341(18) Uani 1.0 4 d . . . C23 C 1.0225(8) -0.0357(9) 0.0698(3) 0.0298(16) Uani 1.0 4 d . . . C24 C 0.9553(7) 0.1136(9) 0.0594(3) 0.0266(16) Uani 1.0 4 d . . . H2 H 0.4266 0.1320 0.1120 0.0303 Uiso 1.0 4 calc R . . H3 H 0.2868 0.0802 0.0407 0.0345 Uiso 1.0 4 calc R . . H7 H 0.7095 0.4482 -0.0817 0.0327 Uiso 1.0 4 calc R . . H8 H 0.8659 0.5051 -0.0141 0.0281 Uiso 1.0 4 calc R . . H11A H 0.2564 0.2378 -0.0554 0.0328 Uiso 1.0 4 calc R . . H11B H 0.3349 0.0713 -0.0620 0.0328 Uiso 1.0 4 calc R . . H12A H 0.4845 0.1988 -0.1053 0.0332 Uiso 1.0 4 calc R . . H12B H 0.4041 0.3648 -0.0995 0.0332 Uiso 1.0 4 calc R . . H14 H 0.4994 0.0761 0.2070 0.0399 Uiso 1.0 4 calc R . . H15 H 0.5213 -0.1606 0.2444 0.0370 Uiso 1.0 4 calc R . . H16 H 0.7118 -0.3437 0.2289 0.0451 Uiso 1.0 4 calc R . . H17 H 0.8797 -0.2440 0.1802 0.0280 Uiso 1.0 4 calc R . . H18 H 0.8591 0.0002 0.1487 0.0392 Uiso 1.0 4 calc R . . H20 H 1.0938 0.3131 0.1528 0.0373 Uiso 1.0 4 calc R . . H21 H 1.2074 0.0607 0.1685 0.0438 Uiso 1.0 4 calc R . . H22 H 1.1622 -0.1538 0.1169 0.0409 Uiso 1.0 4 calc R . . H23 H 1.0036 -0.1237 0.0491 0.0357 Uiso 1.0 4 calc R . . H24 H 0.8932 0.1260 0.0317 0.0319 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0274(3) 0.0242(4) 0.0245(4) -0.00113(17) 0.0060(3) -0.00058(16) I2 0.0347(4) 0.0340(4) 0.0365(4) 0.0082(2) 0.0118(3) 0.0009(2) Se1 0.0240(4) 0.0275(5) 0.0255(5) -0.0032(3) 0.0064(3) -0.0013(3) S1 0.0153(8) 0.0203(9) 0.0266(10) -0.0060(6) 0.0045(7) 0.0002(7) C1 0.021(3) 0.019(3) 0.021(4) 0.003(3) 0.001(3) -0.004(3) C2 0.023(4) 0.030(4) 0.025(4) -0.002(3) 0.010(3) -0.000(3) C3 0.020(4) 0.031(4) 0.036(5) -0.002(3) 0.008(4) -0.000(3) C4 0.024(4) 0.016(3) 0.033(5) -0.004(3) 0.004(3) -0.005(3) C5 0.016(3) 0.017(4) 0.023(4) 0.001(3) 0.005(3) -0.001(3) C6 0.023(4) 0.019(3) 0.024(4) 0.003(3) 0.001(3) 0.002(3) C7 0.027(4) 0.034(4) 0.022(5) 0.001(3) 0.009(3) 0.009(3) C8 0.016(3) 0.025(4) 0.030(5) -0.002(3) 0.009(3) 0.006(3) C9 0.021(4) 0.019(3) 0.029(5) -0.002(3) 0.005(3) -0.003(3) C10 0.018(3) 0.016(3) 0.028(4) -0.001(3) 0.010(3) -0.002(3) C11 0.027(4) 0.029(4) 0.024(5) 0.001(3) -0.002(3) -0.004(3) C12 0.033(4) 0.027(4) 0.023(5) 0.002(3) 0.002(4) -0.000(3) C13 0.028(4) 0.026(4) 0.018(4) -0.005(3) -0.000(3) -0.002(3) C14 0.025(4) 0.033(4) 0.042(5) -0.002(4) 0.007(4) -0.011(4) C15 0.019(4) 0.060(6) 0.014(4) -0.018(4) 0.002(3) 0.003(4) C16 0.048(5) 0.036(4) 0.025(5) -0.006(4) -0.013(4) 0.006(4) C17 0.010(3) 0.038(4) 0.021(4) 0.005(3) -0.004(3) -0.009(3) C18 0.021(4) 0.052(5) 0.026(5) -0.002(4) 0.007(3) -0.011(4) C19 0.012(3) 0.034(4) 0.026(4) -0.005(3) 0.002(3) 0.004(3) C20 0.021(4) 0.046(5) 0.026(5) -0.011(4) 0.003(3) -0.001(4) C21 0.016(4) 0.061(6) 0.033(5) 0.001(4) 0.003(4) 0.012(4) C22 0.023(4) 0.042(5) 0.039(5) 0.005(4) 0.009(4) 0.007(4) C23 0.028(4) 0.035(4) 0.028(5) 0.002(4) 0.008(4) 0.004(4) C24 0.019(4) 0.035(4) 0.026(5) 0.002(3) 0.005(3) 0.005(3) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r6 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r6' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r6' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I1 I2 2.8168(10) yes . . I1 Se1 2.9102(12) yes . . Se1 C1 1.949(7) yes . . Se1 C13 1.939(7) yes . . S1 C9 1.803(7) yes . . S1 C19 1.804(7) yes . . C1 C2 1.387(9) yes . . C1 C10 1.416(10) yes . . C2 C3 1.398(10) yes . . C3 C4 1.381(11) yes . . C4 C5 1.418(9) yes . . C4 C11 1.491(10) yes . . C5 C6 1.406(10) yes . . C5 C10 1.431(9) yes . . C6 C7 1.376(10) yes . . C6 C12 1.517(9) yes . . C7 C8 1.410(10) yes . . C8 C9 1.388(11) yes . . C9 C10 1.446(9) yes . . C11 C12 1.551(11) yes . . C13 C14 1.394(11) yes . . C13 C18 1.412(10) yes . . C14 C15 1.282(11) yes . . C15 C16 1.480(11) yes . . C16 C17 1.428(11) yes . . C17 C18 1.274(11) yes . . C19 C20 1.381(10) yes . . C19 C24 1.383(10) yes . . C20 C21 1.419(11) yes . . C21 C22 1.359(12) yes . . C22 C23 1.385(11) yes . . C23 C24 1.397(10) yes . . C2 H2 0.930 no . . C3 H3 0.930 no . . C7 H7 0.930 no . . C8 H8 0.930 no . . C11 H11A 0.970 no . . C11 H11B 0.970 no . . C12 H12A 0.970 no . . C12 H12B 0.970 no . . C14 H14 0.930 no . . C15 H15 0.930 no . . C16 H16 0.930 no . . C17 H17 0.930 no . . C18 H18 0.930 no . . C20 H20 0.930 no . . C21 H21 0.930 no . . C22 H22 0.930 no . . C23 H23 0.930 no . . C24 H24 0.930 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I2 I1 Se1 173.16(3) yes . . . I1 Se1 C1 95.65(19) yes . . . I1 Se1 C13 103.7(3) yes . . . C1 Se1 C13 99.9(3) yes . . . C9 S1 C19 100.6(3) yes . . . Se1 C1 C2 115.0(5) yes . . . Se1 C1 C10 123.4(5) yes . . . C2 C1 C10 121.5(6) yes . . . C1 C2 C3 123.2(7) yes . . . C2 C3 C4 118.1(7) yes . . . C3 C4 C5 118.9(7) yes . . . C3 C4 C11 131.3(6) yes . . . C5 C4 C11 109.8(7) yes . . . C4 C5 C6 110.6(6) yes . . . C4 C5 C10 124.3(7) yes . . . C6 C5 C10 125.1(6) yes . . . C5 C6 C7 119.2(6) yes . . . C5 C6 C12 109.8(6) yes . . . C7 C6 C12 130.9(7) yes . . . C6 C7 C8 118.2(7) yes . . . C7 C8 C9 123.3(6) yes . . . S1 C9 C8 116.2(5) yes . . . S1 C9 C10 123.1(6) yes . . . C8 C9 C10 120.7(6) yes . . . C1 C10 C5 114.0(6) yes . . . C1 C10 C9 132.5(6) yes . . . C5 C10 C9 113.5(6) yes . . . C4 C11 C12 105.5(6) yes . . . C6 C12 C11 104.2(6) yes . . . Se1 C13 C14 122.9(6) yes . . . Se1 C13 C18 117.4(6) yes . . . C14 C13 C18 119.3(7) yes . . . C13 C14 C15 121.9(7) yes . . . C14 C15 C16 119.3(7) yes . . . C15 C16 C17 116.8(7) yes . . . C16 C17 C18 121.3(7) yes . . . C13 C18 C17 121.2(7) yes . . . S1 C19 C20 115.4(6) yes . . . S1 C19 C24 123.7(5) yes . . . C20 C19 C24 120.9(7) yes . . . C19 C20 C21 118.8(7) yes . . . C20 C21 C22 120.6(7) yes . . . C21 C22 C23 119.8(7) yes . . . C22 C23 C24 120.8(7) yes . . . C19 C24 C23 119.1(7) yes . . . C1 C2 H2 118.393 no . . . C3 C2 H2 118.393 no . . . C2 C3 H3 120.925 no . . . C4 C3 H3 120.957 no . . . C6 C7 H7 120.923 no . . . C8 C7 H7 120.921 no . . . C7 C8 H8 118.361 no . . . C9 C8 H8 118.364 no . . . C4 C11 H11A 110.650 no . . . C4 C11 H11B 110.659 no . . . C12 C11 H11A 110.641 no . . . C12 C11 H11B 110.631 no . . . H11A C11 H11B 108.767 no . . . C6 C12 H12A 110.909 no . . . C6 C12 H12B 110.918 no . . . C11 C12 H12A 110.902 no . . . C11 C12 H12B 110.906 no . . . H12A C12 H12B 108.943 no . . . C13 C14 H14 119.036 no . . . C15 C14 H14 119.057 no . . . C14 C15 H15 120.340 no . . . C16 C15 H15 120.337 no . . . C15 C16 H16 121.568 no . . . C17 C16 H16 121.594 no . . . C16 C17 H17 119.367 no . . . C18 C17 H17 119.358 no . . . C13 C18 H18 119.386 no . . . C17 C18 H18 119.390 no . . . C19 C20 H20 120.567 no . . . C21 C20 H20 120.590 no . . . C20 C21 H21 119.679 no . . . C22 C21 H21 119.696 no . . . C21 C22 H22 120.108 no . . . C23 C22 H22 120.087 no . . . C22 C23 H23 119.613 no . . . C24 C23 H23 119.604 no . . . C19 C24 H24 120.467 no . . . C23 C24 H24 120.469 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I1 Se1 C1 C2 -53.4(4) no . . . . I1 Se1 C1 C10 123.2(4) no . . . . I1 Se1 C13 C14 0.6(5) no . . . . I1 Se1 C13 C18 -172.3(4) no . . . . C1 Se1 C13 C14 -97.8(5) no . . . . C1 Se1 C13 C18 89.3(5) no . . . . C13 Se1 C1 C2 51.6(5) no . . . . C13 Se1 C1 C10 -131.8(5) no . . . . C9 S1 C19 C20 -167.2(5) no . . . . C9 S1 C19 C24 12.4(6) no . . . . C19 S1 C9 C8 -103.1(5) no . . . . C19 S1 C9 C10 76.7(5) no . . . . Se1 C1 C2 C3 177.4(5) no . . . . Se1 C1 C10 C5 -176.1(4) no . . . . Se1 C1 C10 C9 5.0(10) no . . . . C2 C1 C10 C5 0.3(9) no . . . . C2 C1 C10 C9 -178.6(6) no . . . . C10 C1 C2 C3 0.7(10) no . . . . C1 C2 C3 C4 -1.2(10) no . . . . C2 C3 C4 C5 0.7(9) no . . . . C2 C3 C4 C11 -178.9(6) no . . . . C3 C4 C5 C6 -178.6(6) no . . . . C3 C4 C5 C10 0.3(9) no . . . . C3 C4 C11 C12 179.7(7) no . . . . C5 C4 C11 C12 0.1(7) no . . . . C11 C4 C5 C6 1.1(7) no . . . . C11 C4 C5 C10 180.0(5) no . . . . C4 C5 C6 C7 -179.4(5) no . . . . C4 C5 C6 C12 -1.8(7) no . . . . C4 C5 C10 C1 -0.8(9) no . . . . C4 C5 C10 C9 178.4(5) no . . . . C6 C5 C10 C1 178.0(6) no . . . . C6 C5 C10 C9 -2.9(9) no . . . . C10 C5 C6 C7 1.7(10) no . . . . C10 C5 C6 C12 179.3(5) no . . . . C5 C6 C7 C8 -0.8(9) no . . . . C5 C6 C12 C11 1.7(7) no . . . . C7 C6 C12 C11 179.0(7) no . . . . C12 C6 C7 C8 -177.8(6) no . . . . C6 C7 C8 C9 1.4(10) no . . . . C7 C8 C9 S1 177.0(6) no . . . . C7 C8 C9 C10 -2.8(10) no . . . . S1 C9 C10 C1 2.5(10) no . . . . S1 C9 C10 C5 -176.5(4) no . . . . C8 C9 C10 C1 -177.7(6) no . . . . C8 C9 C10 C5 3.3(9) no . . . . C4 C11 C12 C6 -1.0(7) no . . . . Se1 C13 C14 C15 -171.1(5) no . . . . Se1 C13 C18 C17 174.1(5) no . . . . C14 C13 C18 C17 1.0(11) no . . . . C18 C13 C14 C15 1.7(11) no . . . . C13 C14 C15 C16 -3.7(11) no . . . . C14 C15 C16 C17 3.4(10) no . . . . C15 C16 C17 C18 -0.9(10) no . . . . C16 C17 C18 C13 -1.2(11) no . . . . S1 C19 C20 C21 179.5(5) no . . . . S1 C19 C24 C23 -178.7(5) no . . . . C20 C19 C24 C23 0.9(11) no . . . . C24 C19 C20 C21 -0.1(11) no . . . . C19 C20 C21 C22 -0.3(11) no . . . . C20 C21 C22 C23 -0.0(12) no . . . . C21 C22 C23 C24 0.8(12) no . . . . C22 C23 C24 C19 -1.2(11) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Se1 S1 3.252(2) no . . Se1 C9 3.514(8) no . . Se1 C19 3.522(7) no . . S1 C1 3.419(7) no . . C1 C4 2.809(10) no . . C2 C5 2.725(11) no . . C2 C13 3.238(10) no . . C3 C10 2.892(10) no . . C5 C8 2.728(9) no . . C6 C9 2.821(9) no . . C7 C10 2.901(11) no . . C9 C24 2.985(9) no . . C10 C19 3.489(9) no . . C10 C24 3.451(9) no . . C13 C16 2.747(11) no . . C14 C17 2.758(10) no . . C15 C18 2.767(11) no . . C19 C22 2.778(10) no . . C20 C23 2.770(11) no . . C21 C24 2.776(11) no . . C4 C4 3.575(9) no . 3_655 C4 C8 3.540(9) no . 3_665 C6 C10 3.530(9) no . 3_665 C8 C4 3.540(9) no . 3_665 C10 C6 3.530(9) no . 3_665 C11 C18 3.568(11) no . 3_655 C13 C16 3.550(11) no . 2_655 C14 C16 3.574(11) no . 2_655 C16 C13 3.550(11) no . 2_645 C16 C14 3.574(11) no . 2_645 C18 C11 3.568(11) no . 3_655 I1 H2 3.2860 no . . I1 H14 3.0782 no . . Se1 H2 2.8174 no . . Se1 H14 3.0168 no . . Se1 H18 2.9101 no . . S1 H8 2.7460 no . . S1 H20 2.7551 no . . S1 H24 2.9410 no . . C1 H3 3.2828 no . . C2 H14 3.5287 no . . C3 H11A 2.9141 no . . C3 H11B 2.9172 no . . C4 H2 3.2172 no . . C4 H12A 3.0646 no . . C4 H12B 3.0782 no . . C5 H3 3.2607 no . . C5 H7 3.2489 no . . C5 H11A 3.0258 no . . C5 H11B 3.0266 no . . C5 H12A 3.0257 no . . C5 H12B 3.0464 no . . C5 H24 3.5894 no . . C6 H8 3.2222 no . . C6 H11A 3.0656 no . . C6 H11B 3.0792 no . . C7 H12A 2.9308 no . . C7 H12B 2.9411 no . . C8 H24 3.0131 no . . C9 H7 3.2944 no . . C9 H24 2.5431 no . . C10 H2 3.2710 no . . C10 H8 3.2925 no . . C10 H24 2.9481 no . . C11 H3 2.8616 no . . C12 H7 2.8692 no . . C13 H2 2.8572 no . . C13 H15 3.1835 no . . C13 H17 3.1831 no . . C14 H2 2.9604 no . . C14 H16 3.2218 no . . C14 H18 3.2579 no . . C15 H17 3.3254 no . . C16 H14 3.2350 no . . C16 H18 3.1986 no . . C17 H15 3.3232 no . . C18 H14 3.2582 no . . C18 H16 3.1898 no . . C19 H18 2.8979 no . . C19 H21 3.2484 no . . C19 H23 3.2342 no . . C20 H18 2.8580 no . . C20 H22 3.2552 no . . C20 H24 3.2429 no . . C21 H18 2.8240 no . . C21 H23 3.2096 no . . C22 H17 3.5242 no . . C22 H18 2.8383 no . . C22 H20 3.2494 no . . C22 H24 3.2571 no . . C23 H18 2.8695 no . . C23 H21 3.2143 no . . C24 H18 2.9193 no . . C24 H20 3.2437 no . . C24 H22 3.2565 no . . H2 H3 2.3180 no . . H2 H14 2.7182 no . . H3 H11A 2.9762 no . . H3 H11B 2.9736 no . . H7 H8 2.3297 no . . H7 H12A 2.9881 no . . H7 H12B 2.9907 no . . H8 H24 3.3562 no . . H11A H12A 2.7438 no . . H11A H12B 2.2391 no . . H11B H12A 2.2389 no . . H11B H12B 2.7344 no . . H14 H15 2.2041 no . . H15 H16 2.4375 no . . H16 H17 2.3715 no . . H17 H18 2.1860 no . . H17 H22 3.4808 no . . H18 H20 3.4007 no . . H18 H21 3.3562 no . . H18 H22 3.3767 no . . H18 H23 3.4122 no . . H18 H24 3.4939 no . . H20 H21 2.3529 no . . H21 H22 2.2860 no . . H22 H23 2.3113 no . . H23 H24 2.3277 no . . I1 H7 3.2680 no . 3_665 I1 H12B 3.4099 no . 3_665 I1 H16 3.2504 no . 1_565 I1 H20 3.5085 no . 1_455 I2 H14 3.1654 no . 2_555 I2 H15 3.4503 no . 1_565 I2 H15 3.5019 no . 2_555 I2 H17 3.4291 no . 1_465 I2 H20 3.2293 no . 1_455 I2 H21 3.2857 no . 2_655 I2 H22 3.3226 no . 1_465 Se1 H12B 3.2446 no . 3_665 S1 H8 3.1438 no . 3_765 S1 H11A 3.0828 no . 3_665 S1 H12B 3.4028 no . 3_665 C1 H11B 2.8418 no . 3_655 C1 H12B 3.1769 no . 3_665 C2 H7 3.5162 no . 3_665 C2 H11B 2.9108 no . 3_655 C2 H12A 3.1054 no . 3_655 C3 H11B 3.2929 no . 3_655 C3 H12A 3.4951 no . 3_655 C4 H11B 3.5654 no . 3_655 C5 H11B 3.4838 no . 3_655 C7 H22 3.2388 no . 3_755 C8 H8 3.3636 no . 3_765 C8 H11A 3.2272 no . 3_665 C8 H23 3.5738 no . 3_755 C9 H11A 3.0648 no . 3_665 C9 H12B 3.2103 no . 3_665 C10 H11B 3.1756 no . 3_655 C10 H12B 3.1364 no . 3_665 C11 H18 3.5135 no . 3_655 C11 H23 3.4085 no . 3_655 C11 H24 3.5191 no . 3_655 C13 H11B 3.3390 no . 3_655 C13 H12A 3.1832 no . 3_655 C13 H16 2.8990 no . 2_655 C14 H12A 3.2297 no . 3_655 C14 H16 2.8862 no . 2_655 C14 H21 3.5803 no . 1_455 C15 H12A 3.3764 no . 3_655 C15 H16 3.2179 no . 2_655 C16 H12A 3.4202 no . 3_655 C16 H12B 3.4610 no . 3_655 C17 H12A 3.3728 no . 3_655 C17 H12B 3.3294 no . 3_655 C18 H11A 3.5307 no . 3_655 C18 H11B 3.0789 no . 3_655 C18 H12A 3.2757 no . 3_655 C18 H16 3.3174 no . 2_655 C19 H8 3.4263 no . 3_765 C20 H2 3.5510 no . 1_655 C21 H2 2.9547 no . 1_655 C21 H3 3.2712 no . 1_655 C22 H2 3.3286 no . 1_655 C22 H3 2.9006 no . 1_655 C23 H3 2.9049 no . 1_655 C23 H11A 3.1294 no . 3_655 C23 H11B 3.4182 no . 3_655 C23 H23 3.5656 no . 3_755 C23 H24 3.1357 no . 3_755 C24 H3 3.2880 no . 1_655 C24 H11A 3.5129 no . 3_655 C24 H11B 3.1724 no . 3_655 C24 H23 3.1160 no . 3_755 H2 C20 3.5510 no . 1_455 H2 C21 2.9547 no . 1_455 H2 C22 3.3286 no . 1_455 H2 H11B 3.2681 no . 3_655 H2 H12A 2.8507 no . 3_655 H2 H21 2.8310 no . 1_455 H2 H22 3.4608 no . 1_455 H3 C21 3.2712 no . 1_455 H3 C22 2.9006 no . 1_455 H3 C23 2.9049 no . 1_455 H3 C24 3.2880 no . 1_455 H3 H12A 3.5217 no . 3_655 H3 H22 3.2007 no . 1_455 H3 H23 3.2156 no . 1_455 H3 H23 3.5552 no . 3_655 H3 H24 3.0266 no . 3_655 H7 I1 3.2680 no . 3_665 H7 C2 3.5162 no . 3_665 H7 H20 3.4926 no . 3_765 H7 H22 2.9267 no . 3_755 H8 S1 3.1438 no . 3_765 H8 C8 3.3636 no . 3_765 H8 C19 3.4263 no . 3_765 H8 H8 2.6016 no . 3_765 H8 H11A 3.1819 no . 3_665 H8 H23 3.5428 no . 3_755 H11A S1 3.0828 no . 3_665 H11A C8 3.2272 no . 3_665 H11A C9 3.0648 no . 3_665 H11A C18 3.5307 no . 3_655 H11A C23 3.1294 no . 3_655 H11A C24 3.5129 no . 3_655 H11A H8 3.1819 no . 3_665 H11A H17 3.5983 no . 3_655 H11A H18 3.3502 no . 3_655 H11A H23 2.6845 no . 3_655 H11A H24 3.4026 no . 3_655 H11B C1 2.8418 no . 3_655 H11B C2 2.9108 no . 3_655 H11B C3 3.2929 no . 3_655 H11B C4 3.5654 no . 3_655 H11B C5 3.4838 no . 3_655 H11B C10 3.1756 no . 3_655 H11B C13 3.3390 no . 3_655 H11B C18 3.0789 no . 3_655 H11B C23 3.4182 no . 3_655 H11B C24 3.1724 no . 3_655 H11B H2 3.2681 no . 3_655 H11B H18 2.9486 no . 3_655 H11B H23 3.3307 no . 3_655 H11B H24 2.9200 no . 3_655 H12A C2 3.1054 no . 3_655 H12A C3 3.4951 no . 3_655 H12A C13 3.1832 no . 3_655 H12A C14 3.2297 no . 3_655 H12A C15 3.3764 no . 3_655 H12A C16 3.4202 no . 3_655 H12A C17 3.3728 no . 3_655 H12A C18 3.2757 no . 3_655 H12A H2 2.8507 no . 3_655 H12A H3 3.5217 no . 3_655 H12A H22 3.4552 no . 3_755 H12B I1 3.4099 no . 3_665 H12B Se1 3.2446 no . 3_665 H12B S1 3.4028 no . 3_665 H12B C1 3.1769 no . 3_665 H12B C9 3.2103 no . 3_665 H12B C10 3.1364 no . 3_665 H12B C16 3.4610 no . 3_655 H12B C17 3.3294 no . 3_655 H12B H17 3.4788 no . 3_655 H14 I2 3.1654 no . 2_545 H14 H16 3.1931 no . 2_655 H14 H17 3.5671 no . 2_655 H14 H21 2.8854 no . 1_455 H15 I2 3.4503 no . 1_545 H15 I2 3.5019 no . 2_545 H15 H20 3.2112 no . 2_645 H16 I1 3.2504 no . 1_545 H16 C13 2.8990 no . 2_645 H16 C14 2.8862 no . 2_645 H16 C15 3.2179 no . 2_645 H16 C18 3.3174 no . 2_645 H16 H14 3.1931 no . 2_645 H17 I2 3.4291 no . 1_645 H17 H11A 3.5983 no . 3_655 H17 H12B 3.4788 no . 3_655 H17 H14 3.5671 no . 2_645 H18 C11 3.5135 no . 3_655 H18 H11A 3.3502 no . 3_655 H18 H11B 2.9486 no . 3_655 H20 I1 3.5085 no . 1_655 H20 I2 3.2293 no . 1_655 H20 H7 3.4926 no . 3_765 H20 H15 3.2112 no . 2_655 H21 I2 3.2857 no . 2_645 H21 C14 3.5803 no . 1_655 H21 H2 2.8310 no . 1_655 H21 H14 2.8854 no . 1_655 H22 I2 3.3226 no . 1_645 H22 C7 3.2388 no . 3_755 H22 H2 3.4608 no . 1_655 H22 H3 3.2007 no . 1_655 H22 H7 2.9267 no . 3_755 H22 H12A 3.4552 no . 3_755 H23 C8 3.5738 no . 3_755 H23 C11 3.4085 no . 3_655 H23 C23 3.5656 no . 3_755 H23 C24 3.1160 no . 3_755 H23 H3 3.2156 no . 1_655 H23 H3 3.5552 no . 3_655 H23 H8 3.5428 no . 3_755 H23 H11A 2.6845 no . 3_655 H23 H11B 3.3307 no . 3_655 H23 H23 3.4144 no . 3_755 H23 H24 2.5744 no . 3_755 H24 C11 3.5191 no . 3_655 H24 C23 3.1357 no . 3_755 H24 H3 3.0266 no . 3_655 H24 H11A 3.4026 no . 3_655 H24 H11B 2.9200 no . 3_655 H24 H23 2.5744 no . 3_755 H24 H24 3.5260 no . 3_755 #============================================================================== data__Ferg80-2 _database_code_depnum_ccdc_archive 'CCDC 850821' #TrackingRef '- 6.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H13 Br3 Te' _chemical_formula_moiety 'C18 H13 Br3 Te' _chemical_formula_weight 596.61 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,+Z 3 +X,-Y,1/2+Z 4 1/2-X,1/2-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,-Z 7 -X,+Y,1/2-Z 8 1/2+X,1/2+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 15.745(7) _cell_length_b 10.066(4) _cell_length_c 22.162(9) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3512(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 12120 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description chip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.256 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224.00 _exptl_absorpt_coefficient_mu 8.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.308 _exptl_absorpt_correction_T_max 0.599 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 26879 _diffrn_reflns_av_R_equivalents 0.1228 _diffrn_reflns_theta_max 26.32 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3659 _reflns_number_gt 3224 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0801 _refine_ls_R_factor_all 0.0988 _refine_ls_wR_factor_ref 0.2488 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3563 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.405 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1031P)^2^+29.8563P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.390 _refine_diff_density_min -1.620 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.531 1.675 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Te 0.84780(5) 0.24810(9) 0.06487(4) 0.0266(3) Uani 1.00 8 d . . . Br(1) Br 0.71864(8) 0.19985(15) 0.14213(6) 0.0326(4) Uani 1.00 8 d . . . Br(2) Br 0.98242(9) 0.27397(15) -0.00656(7) 0.0335(4) Uani 1.00 8 d . . . Br(3) Br 0.94741(9) 0.46749(14) 0.14657(7) 0.0343(4) Uani 1.00 8 d . . . C(1) C 0.9286(8) 0.1321(14) 0.1220(6) 0.028(3) Uani 1.00 8 d . . . C(2) C 0.9163(9) -0.0057(14) 0.1206(7) 0.033(3) Uani 1.00 8 d . . . C(3) C 0.9736(9) -0.0984(17) 0.1458(6) 0.034(3) Uani 1.00 8 d . . . C(4) C 1.0448(8) -0.0453(14) 0.1750(6) 0.027(3) Uani 1.00 8 d . . . C(5) C 1.0552(8) 0.0931(14) 0.1804(6) 0.028(3) Uani 1.00 8 d . . . C(6) C 1.1316(8) 0.1245(15) 0.2109(6) 0.029(3) Uani 1.00 8 d . . . C(7) C 1.1516(8) 0.2583(16) 0.2197(6) 0.033(3) Uani 1.00 8 d . . . C(8) C 1.0943(9) 0.3562(15) 0.1984(7) 0.035(3) Uani 1.00 8 d . . . C(9) C 1.0228(8) 0.3251(14) 0.1670(6) 0.028(3) Uani 1.00 8 d . . . C(10) C 0.9979(8) 0.1885(14) 0.1556(5) 0.024(3) Uani 1.00 8 d . . . C(11) C 1.1197(9) -0.1149(15) 0.2030(6) 0.032(3) Uani 1.00 8 d . . . C(12) C 1.1770(8) 0.0015(16) 0.2290(7) 0.034(3) Uani 1.00 8 d . . . C(13) C 0.7978(8) 0.0952(14) 0.0072(6) 0.026(3) Uani 1.00 8 d . . . C(14) C 0.7119(9) 0.1041(14) -0.0058(6) 0.028(3) Uani 1.00 8 d . . . C(15) C 0.6788(9) 0.0145(15) -0.0479(6) 0.034(3) Uani 1.00 8 d . . . C(16) C 0.7291(9) -0.0815(16) -0.0751(6) 0.034(3) Uani 1.00 8 d . . . C(17) C 0.8126(9) -0.0889(14) -0.0621(6) 0.033(3) Uani 1.00 8 d . . . C(18) C 0.8498(8) 0.0008(15) -0.0209(7) 0.032(3) Uani 1.00 8 d . . . H(2) H 0.8665 -0.0388 0.1015 0.039 Uiso 1.00 8 calc R . . H(3) H 0.9643 -0.1915 0.1432 0.041 Uiso 1.00 8 calc R . . H(7) H 1.2026 0.2832 0.2395 0.039 Uiso 1.00 8 calc R . . H(8) H 1.1063 0.4470 0.2064 0.041 Uiso 1.00 8 calc R . . H(11A) H 1.1511 -0.1670 0.1724 0.038 Uiso 1.00 8 calc R . . H(11B) H 1.1011 -0.1752 0.2357 0.038 Uiso 1.00 8 calc R . . H(12A) H 1.1817 -0.0047 0.2735 0.041 Uiso 1.00 8 calc R . . H(12B) H 1.2347 -0.0012 0.2113 0.041 Uiso 1.00 8 calc R . . H(14) H 0.6769 0.1685 0.0132 0.034 Uiso 1.00 8 calc R . . H(15) H 0.6203 0.0196 -0.0582 0.040 Uiso 1.00 8 calc R . . H(16) H 0.7047 -0.1422 -0.1030 0.041 Uiso 1.00 8 calc R . . H(17) H 0.8466 -0.1551 -0.0808 0.039 Uiso 1.00 8 calc R . . H(18) H 0.9089 -0.0027 -0.0125 0.038 Uiso 1.00 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te(1) 0.0207(5) 0.0281(5) 0.0309(5) 0.0007(3) -0.0010(3) 0.0031(3) Br(1) 0.0234(7) 0.0396(8) 0.0347(8) 0.0006(6) 0.0031(5) 0.0008(6) Br(2) 0.0248(7) 0.0362(8) 0.0396(8) -0.0006(6) 0.0034(5) 0.0053(6) Br(3) 0.0322(8) 0.0276(8) 0.0431(9) 0.0020(6) -0.0049(6) -0.0002(6) C(1) 0.028(7) 0.032(7) 0.025(7) -0.001(6) 0.003(5) 0.004(5) C(2) 0.023(7) 0.034(8) 0.042(8) -0.003(6) -0.004(6) -0.004(6) C(3) 0.027(7) 0.044(9) 0.031(8) -0.001(6) -0.000(5) 0.001(6) C(4) 0.019(6) 0.034(8) 0.028(7) -0.004(5) 0.002(5) -0.003(5) C(5) 0.023(6) 0.031(7) 0.029(7) -0.002(5) 0.013(5) 0.006(5) C(6) 0.018(6) 0.037(8) 0.032(7) 0.005(5) 0.002(5) 0.004(6) C(7) 0.022(7) 0.047(9) 0.029(7) -0.012(6) 0.002(5) 0.001(6) C(8) 0.031(7) 0.030(7) 0.043(8) -0.003(6) -0.006(6) -0.002(6) C(9) 0.014(6) 0.032(7) 0.039(8) -0.002(5) 0.005(5) -0.001(6) C(10) 0.018(6) 0.031(7) 0.024(6) 0.002(5) -0.003(5) 0.003(5) C(11) 0.034(7) 0.041(8) 0.022(7) 0.011(6) -0.005(5) 0.005(6) C(12) 0.014(6) 0.040(9) 0.049(9) -0.003(6) 0.002(6) -0.000(6) C(13) 0.022(6) 0.035(7) 0.022(6) -0.011(5) -0.001(5) 0.002(5) C(14) 0.031(7) 0.032(7) 0.022(6) 0.001(6) -0.002(5) -0.001(5) C(15) 0.029(7) 0.037(8) 0.034(8) -0.008(6) -0.002(6) 0.010(6) C(16) 0.032(8) 0.046(9) 0.024(7) -0.015(7) 0.000(5) -0.006(6) C(17) 0.043(8) 0.026(7) 0.030(7) -0.004(6) 0.010(6) 0.007(6) C(18) 0.018(6) 0.040(9) 0.036(8) -0.008(6) -0.007(5) -0.001(6) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Te(1) Br(1) 2.7025(17) yes . . Te(1) Br(2) 2.6583(19) yes . . Te(1) C(1) 2.141(13) yes . . Te(1) C(13) 2.150(13) yes . . Br(3) C(9) 1.915(14) yes . . C(1) C(2) 1.40(2) yes . . C(1) C(10) 1.438(18) yes . . C(2) C(3) 1.41(2) yes . . C(3) C(4) 1.401(19) yes . . C(4) C(5) 1.41(2) yes . . C(4) C(11) 1.506(19) yes . . C(5) C(6) 1.416(18) yes . . C(5) C(10) 1.427(19) yes . . C(6) C(7) 1.40(2) yes . . C(6) C(12) 1.49(2) yes . . C(7) C(8) 1.42(2) yes . . C(8) C(9) 1.361(19) yes . . C(9) C(10) 1.452(20) yes . . C(11) C(12) 1.59(2) yes . . C(13) C(14) 1.385(18) yes . . C(13) C(18) 1.401(19) yes . . C(14) C(15) 1.399(20) yes . . C(15) C(16) 1.39(2) yes . . C(16) C(17) 1.35(2) yes . . C(17) C(18) 1.41(2) yes . . C(2) H(2) 0.950 yes . . C(3) H(3) 0.950 yes . . C(7) H(7) 0.950 yes . . C(8) H(8) 0.950 yes . . C(11) H(11A) 0.990 yes . . C(11) H(11B) 0.990 yes . . C(12) H(12A) 0.990 yes . . C(12) H(12B) 0.990 yes . . C(14) H(14) 0.950 yes . . C(15) H(15) 0.950 yes . . C(16) H(16) 0.950 yes . . C(17) H(17) 0.950 yes . . C(18) H(18) 0.950 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Te(1) Br(2) 174.23(6) yes . . . Br(1) Te(1) C(1) 88.5(4) yes . . . Br(1) Te(1) C(13) 88.4(3) yes . . . Br(2) Te(1) C(1) 86.1(4) yes . . . Br(2) Te(1) C(13) 90.5(3) yes . . . C(1) Te(1) C(13) 100.3(5) yes . . . Te(1) C(1) C(2) 116.4(10) yes . . . Te(1) C(1) C(10) 122.8(10) yes . . . C(2) C(1) C(10) 120.5(12) yes . . . C(1) C(2) C(3) 123.8(13) yes . . . C(2) C(3) C(4) 116.2(14) yes . . . C(3) C(4) C(5) 120.7(13) yes . . . C(3) C(4) C(11) 129.8(13) yes . . . C(5) C(4) C(11) 109.6(11) yes . . . C(4) C(5) C(6) 111.1(12) yes . . . C(4) C(5) C(10) 124.1(12) yes . . . C(6) C(5) C(10) 124.8(13) yes . . . C(5) C(6) C(7) 118.2(12) yes . . . C(5) C(6) C(12) 110.6(12) yes . . . C(7) C(6) C(12) 131.2(12) yes . . . C(6) C(7) C(8) 118.8(12) yes . . . C(7) C(8) C(9) 122.4(14) yes . . . Br(3) C(9) C(8) 117.5(11) yes . . . Br(3) C(9) C(10) 120.0(9) yes . . . C(8) C(9) C(10) 122.1(13) yes . . . C(1) C(10) C(5) 114.4(12) yes . . . C(1) C(10) C(9) 132.0(12) yes . . . C(5) C(10) C(9) 113.5(11) yes . . . C(4) C(11) C(12) 104.6(12) yes . . . C(6) C(12) C(11) 104.1(11) yes . . . Te(1) C(13) C(14) 115.8(10) yes . . . Te(1) C(13) C(18) 122.4(9) yes . . . C(14) C(13) C(18) 121.4(12) yes . . . C(13) C(14) C(15) 117.5(13) yes . . . C(14) C(15) C(16) 121.7(13) yes . . . C(15) C(16) C(17) 120.2(13) yes . . . C(16) C(17) C(18) 120.5(13) yes . . . C(13) C(18) C(17) 118.6(12) yes . . . C(1) C(2) H(2) 118.119 yes . . . C(3) C(2) H(2) 118.104 yes . . . C(2) C(3) H(3) 121.889 yes . . . C(4) C(3) H(3) 121.883 yes . . . C(6) C(7) H(7) 120.596 yes . . . C(8) C(7) H(7) 120.595 yes . . . C(7) C(8) H(8) 118.778 yes . . . C(9) C(8) H(8) 118.775 yes . . . C(4) C(11) H(11A) 110.840 yes . . . C(4) C(11) H(11B) 110.834 yes . . . C(12) C(11) H(11A) 110.842 yes . . . C(12) C(11) H(11B) 110.832 yes . . . H(11A) C(11) H(11B) 108.893 yes . . . C(6) C(12) H(12A) 110.934 yes . . . C(6) C(12) H(12B) 110.934 yes . . . C(11) C(12) H(12A) 110.942 yes . . . C(11) C(12) H(12B) 110.932 yes . . . H(12A) C(12) H(12B) 108.952 yes . . . C(13) C(14) H(14) 121.276 yes . . . C(15) C(14) H(14) 121.272 yes . . . C(14) C(15) H(15) 119.135 yes . . . C(16) C(15) H(15) 119.134 yes . . . C(15) C(16) H(16) 119.909 yes . . . C(17) C(16) H(16) 119.918 yes . . . C(16) C(17) H(17) 119.737 yes . . . C(18) C(17) H(17) 119.743 yes . . . C(13) C(18) H(18) 120.682 yes . . . C(17) C(18) H(18) 120.675 yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Te(1) C(1) C(2) 73.4(8) no . . . . Br(1) Te(1) C(1) C(10) -113.0(8) no . . . . Br(1) Te(1) C(13) C(14) 49.9(8) no . . . . Br(1) Te(1) C(13) C(18) -136.8(9) no . . . . Br(2) Te(1) C(1) C(2) -104.5(8) no . . . . Br(2) Te(1) C(1) C(10) 69.2(8) no . . . . Br(2) Te(1) C(13) C(14) -135.7(8) no . . . . Br(2) Te(1) C(13) C(18) 37.5(9) no . . . . C(1) Te(1) C(13) C(14) 138.2(8) no . . . . C(1) Te(1) C(13) C(18) -48.6(10) no . . . . C(13) Te(1) C(1) C(2) -14.7(9) no . . . . C(13) Te(1) C(1) C(10) 158.9(9) no . . . . Te(1) C(1) C(10) C(9) 9.8(18) no . . . . C(2) C(1) C(10) C(5) 6.4(17) no . . . . C(10) C(1) C(2) C(3) -7(2) no . . . . C(1) C(2) C(3) C(4) 1.8(20) no . . . . C(2) C(3) C(4) C(5) 2.6(18) no . . . . C(3) C(4) C(5) C(10) -2.3(19) no . . . . C(5) C(4) C(11) C(12) 2.1(13) no . . . . C(11) C(4) C(5) C(6) -0.8(14) no . . . . C(4) C(5) C(6) C(12) -1.0(14) no . . . . C(4) C(5) C(10) C(1) -2.2(17) no . . . . C(6) C(5) C(10) C(9) -2.8(17) no . . . . C(10) C(5) C(6) C(7) 2.4(19) no . . . . C(5) C(6) C(7) C(8) 0.8(18) no . . . . C(5) C(6) C(12) C(11) 2.2(14) no . . . . C(6) C(7) C(8) C(9) -4(2) no . . . . C(7) C(8) C(9) C(10) 3(2) no . . . . Br(3) C(9) C(10) C(1) 11.0(18) no . . . . C(8) C(9) C(10) C(5) -0.0(18) no . . . . C(4) C(11) C(12) C(6) -2.5(13) no . . . . C(14) C(13) C(18) C(17) -1.7(20) no . . . . C(18) C(13) C(14) C(15) 0.4(19) no . . . . C(13) C(14) C(15) C(16) 1.2(20) no . . . . C(14) C(15) C(16) C(17) -1(2) no . . . . C(15) C(16) C(17) C(18) -0(2) no . . . . C(16) C(17) C(18) C(13) 2(2) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Te(1) Br(3) 3.2581(19) yes . . Br(1) C(14) 3.418(13) yes . . Br(2) C(18) 3.467(15) yes . . Br(3) C(1) 3.433(14) yes . . C(1) C(4) 2.813(19) yes . . C(2) C(5) 2.744(19) yes . . C(2) C(13) 3.290(19) yes . . C(2) C(18) 3.31(2) yes . . C(3) C(10) 2.92(2) yes . . C(5) C(8) 2.75(2) yes . . C(6) C(9) 2.820(19) yes . . C(7) C(10) 2.892(18) yes . . C(13) C(16) 2.768(19) yes . . C(14) C(17) 2.801(20) yes . . C(15) C(18) 2.761(19) yes . . Br(1) Br(3) 3.509(2) yes . 2_645 Br(3) Br(1) 3.509(2) yes . 2_655 C(5) C(17) 3.347(19) yes . 5_755 C(6) C(17) 3.432(19) yes . 5_755 C(8) C(9) 3.521(20) yes . 7_755 C(9) C(8) 3.521(20) yes . 7_755 C(14) C(17) 3.36(2) yes . 2_655 C(17) C(5) 3.347(19) yes . 5_755 C(17) C(6) 3.432(19) yes . 5_755 C(17) C(14) 3.36(2) yes . 2_645 Te(1) H(2) 3.0142 yes . . Te(1) H(14) 3.0321 yes . . Te(1) H(18) 3.1996 yes . . Br(1) H(2) 3.4642 yes . . Br(1) H(14) 2.9485 yes . . Br(2) H(18) 3.0189 yes . . Br(3) H(8) 2.8395 yes . . C(1) H(3) 3.3379 yes . . C(1) H(18) 3.2893 yes . . C(2) H(18) 2.9511 yes . . C(3) H(11A) 2.9397 yes . . C(3) H(11B) 2.9325 yes . . C(4) H(2) 3.2459 yes . . C(4) H(12A) 3.0946 yes . . C(4) H(12B) 3.1277 yes . . C(5) H(3) 3.3066 yes . . C(5) H(7) 3.2812 yes . . C(5) H(11A) 3.0287 yes . . C(5) H(11B) 3.0541 yes . . C(5) H(12A) 3.0328 yes . . C(5) H(12B) 3.0595 yes . . C(6) H(8) 3.2718 yes . . C(6) H(11A) 3.0716 yes . . C(6) H(11B) 3.1045 yes . . C(7) H(12A) 2.9424 yes . . C(7) H(12B) 2.9278 yes . . C(9) H(7) 3.2824 yes . . C(10) H(2) 3.3090 yes . . C(10) H(8) 3.3097 yes . . C(11) H(3) 2.8881 yes . . C(12) H(7) 2.8736 yes . . C(13) H(2) 2.7127 yes . . C(13) H(15) 3.2383 yes . . C(13) H(17) 3.2777 yes . . C(14) H(16) 3.2863 yes . . C(14) H(18) 3.2853 yes . . C(15) H(17) 3.2287 yes . . C(16) H(14) 3.2930 yes . . C(16) H(18) 3.2504 yes . . C(17) H(15) 3.2186 yes . . C(18) H(2) 2.7557 yes . . C(18) H(14) 3.2912 yes . . C(18) H(16) 3.2553 yes . . H(2) H(3) 2.3634 yes . . H(2) H(18) 2.6384 yes . . H(3) H(11A) 3.0224 yes . . H(3) H(11B) 2.9788 yes . . H(7) H(8) 2.3569 yes . . H(7) H(12A) 3.0122 yes . . H(7) H(12B) 2.9734 yes . . H(11A) H(12A) 2.8132 yes . . H(11A) H(12B) 2.2928 yes . . H(11B) H(12A) 2.2929 yes . . H(11B) H(12B) 2.7904 yes . . H(14) H(15) 2.3551 yes . . H(15) H(16) 2.3238 yes . . H(16) H(17) 2.2916 yes . . H(17) H(18) 2.3677 yes . . Br(1) H(2) 3.0869 yes . 2_655 Br(1) H(3) 3.0815 yes . 2_655 Br(1) H(7) 3.0205 yes . 7_755 Br(1) H(11B) 3.5119 yes . 8_455 Br(1) H(12A) 3.1938 yes . 7_755 Br(1) H(12A) 3.5611 yes . 8_455 Br(2) H(3) 3.2492 yes . 5_755 Br(2) H(14) 3.1197 yes . 6_555 Br(2) H(15) 3.1684 yes . 2_655 Br(2) H(15) 3.3309 yes . 6_555 Br(2) H(17) 3.5253 yes . 5_755 Br(2) H(18) 3.2501 yes . 5_755 Br(3) H(3) 3.4440 yes . 1_565 Br(3) H(8) 3.3722 yes . 7_755 Br(3) H(15) 3.3565 yes . 6_555 C(1) H(12A) 3.2060 yes . 7_755 C(2) H(12A) 2.8100 yes . 7_755 C(3) H(11B) 2.9789 yes . 7_755 C(3) H(12A) 3.1731 yes . 7_755 C(4) H(11B) 3.3024 yes . 7_755 C(4) H(17) 3.3682 yes . 5_755 C(5) H(17) 2.7653 yes . 5_755 C(6) H(16) 3.5210 yes . 5_755 C(6) H(17) 2.9199 yes . 5_755 C(7) H(11A) 3.3631 yes . 2_755 C(7) H(12B) 3.0170 yes . 2_755 C(7) H(17) 3.2479 yes . 5_755 C(8) H(12B) 3.0639 yes . 2_755 C(8) H(15) 3.3748 yes . 6_555 C(8) H(17) 3.4291 yes . 5_755 C(9) H(15) 3.2584 yes . 6_555 C(9) H(17) 3.2870 yes . 5_755 C(10) H(17) 2.9759 yes . 5_755 C(11) H(7) 3.0872 yes . 2_745 C(11) H(16) 3.5616 yes . 6_545 C(12) H(7) 2.9110 yes . 2_745 C(12) H(8) 3.4913 yes . 2_745 C(13) H(16) 3.5991 yes . 2_655 C(14) H(16) 3.5900 yes . 2_655 C(14) H(17) 3.0812 yes . 2_655 C(15) H(17) 3.4284 yes . 2_655 C(16) H(11A) 3.5449 yes . 6_445 C(16) H(12B) 3.1815 yes . 5_755 C(16) H(14) 3.5146 yes . 2_645 C(17) H(11A) 3.5972 yes . 5_755 C(17) H(12B) 3.5074 yes . 5_755 C(17) H(14) 2.9626 yes . 2_645 C(18) H(14) 3.4553 yes . 2_645 H(2) Br(1) 3.0869 yes . 2_645 H(2) H(12A) 2.8933 yes . 7_755 H(3) Br(1) 3.0815 yes . 2_645 H(3) Br(2) 3.2492 yes . 5_755 H(3) Br(3) 3.4440 yes . 1_545 H(3) H(11B) 2.8798 yes . 7_755 H(3) H(12A) 3.4980 yes . 7_755 H(7) Br(1) 3.0205 yes . 7_755 H(7) C(11) 3.0872 yes . 2_755 H(7) C(12) 2.9110 yes . 2_755 H(7) H(11A) 2.7859 yes . 2_755 H(7) H(11B) 3.1196 yes . 2_755 H(7) H(12A) 2.9054 yes . 2_755 H(7) H(12B) 2.4649 yes . 2_755 H(8) Br(3) 3.3722 yes . 7_755 H(8) C(12) 3.4913 yes . 2_755 H(8) H(12B) 2.5593 yes . 2_755 H(8) H(15) 3.3096 yes . 6_555 H(8) H(16) 3.3932 yes . 6_555 H(11A) C(7) 3.3631 yes . 2_745 H(11A) C(16) 3.5449 yes . 6_545 H(11A) C(17) 3.5972 yes . 5_755 H(11A) H(7) 2.7859 yes . 2_745 H(11A) H(16) 2.6016 yes . 6_545 H(11B) Br(1) 3.5119 yes . 8_545 H(11B) C(3) 2.9789 yes . 7_755 H(11B) C(4) 3.3024 yes . 7_755 H(11B) H(3) 2.8798 yes . 7_755 H(11B) H(7) 3.1196 yes . 2_745 H(11B) H(11B) 3.2463 yes . 7_755 H(12A) Br(1) 3.1938 yes . 7_755 H(12A) Br(1) 3.5611 yes . 8_545 H(12A) C(1) 3.2060 yes . 7_755 H(12A) C(2) 2.8100 yes . 7_755 H(12A) C(3) 3.1731 yes . 7_755 H(12A) H(2) 2.8933 yes . 7_755 H(12A) H(3) 3.4980 yes . 7_755 H(12A) H(7) 2.9054 yes . 2_745 H(12B) C(7) 3.0170 yes . 2_745 H(12B) C(8) 3.0639 yes . 2_745 H(12B) C(16) 3.1815 yes . 5_755 H(12B) C(17) 3.5074 yes . 5_755 H(12B) H(7) 2.4649 yes . 2_745 H(12B) H(8) 2.5593 yes . 2_745 H(12B) H(16) 2.9584 yes . 5_755 H(12B) H(17) 3.5316 yes . 5_755 H(14) Br(2) 3.1197 yes . 6_455 H(14) C(16) 3.5146 yes . 2_655 H(14) C(17) 2.9626 yes . 2_655 H(14) C(18) 3.4553 yes . 2_655 H(14) H(17) 2.7628 yes . 2_655 H(15) Br(2) 3.1684 yes . 2_645 H(15) Br(2) 3.3309 yes . 6_455 H(15) Br(3) 3.3565 yes . 6_455 H(15) C(8) 3.3748 yes . 6_455 H(15) C(9) 3.2584 yes . 6_455 H(15) H(8) 3.3096 yes . 6_455 H(15) H(17) 3.3539 yes . 2_655 H(16) C(6) 3.5210 yes . 5_755 H(16) C(11) 3.5616 yes . 6_445 H(16) C(13) 3.5991 yes . 2_645 H(16) C(14) 3.5900 yes . 2_645 H(16) H(8) 3.3932 yes . 6_455 H(16) H(11A) 2.6016 yes . 6_445 H(16) H(12B) 2.9584 yes . 5_755 H(17) Br(2) 3.5253 yes . 5_755 H(17) C(4) 3.3682 yes . 5_755 H(17) C(5) 2.7653 yes . 5_755 H(17) C(6) 2.9199 yes . 5_755 H(17) C(7) 3.2479 yes . 5_755 H(17) C(8) 3.4291 yes . 5_755 H(17) C(9) 3.2870 yes . 5_755 H(17) C(10) 2.9759 yes . 5_755 H(17) C(14) 3.0812 yes . 2_645 H(17) C(15) 3.4284 yes . 2_645 H(17) H(12B) 3.5316 yes . 5_755 H(17) H(14) 2.7628 yes . 2_645 H(17) H(15) 3.3539 yes . 2_645 H(18) Br(2) 3.2501 yes . 5_755 H(18) H(18) 2.9225 yes . 5_755 #============================================================================== data__Ferg78-4 _database_code_depnum_ccdc_archive 'CCDC 850822' #TrackingRef '- 7.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H13 Br I2 Te' _chemical_formula_moiety 'C18 H13 Br I2 Te' _chemical_formula_weight 690.61 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 26.071(7) _cell_length_b 9.378(2) _cell_length_c 15.682(4) _cell_angle_alpha 90.0000 _cell_angle_beta 105.281(5) _cell_angle_gamma 90.0000 _cell_volume 3698.4(16) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7604 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange/Red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512.00 _exptl_absorpt_coefficient_mu 7.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 0.808 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 15059 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3967 _reflns_number_gt 3559 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1490 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3729 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0954P)^2^+2.6044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.670 _refine_diff_density_min -2.880 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.531 1.675 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 I(1) I 0.275619(15) 0.33761(4) 0.21498(3) 0.02555(17) Uani 1.00 8 d . . . I(2) I 0.073242(15) 0.07095(4) 0.22310(3) 0.02691(17) Uani 1.00 8 d . . . Te(1) Te 0.172315(14) 0.21800(4) 0.22536(2) 0.01843(17) Uani 1.00 8 d . . . Br(1) Br 0.15460(3) 0.10333(7) 0.02717(4) 0.0343(2) Uani 1.00 8 d . . . C(1) C 0.1282(2) 0.3853(6) 0.1467(4) 0.0196(11) Uani 1.00 8 d . . . C(2) C 0.1177(2) 0.5051(6) 0.1914(4) 0.0221(12) Uani 1.00 8 d . . . C(3) C 0.0887(3) 0.6249(6) 0.1477(4) 0.0248(12) Uani 1.00 8 d . . . C(4) C 0.0685(2) 0.6187(6) 0.0581(4) 0.0217(11) Uani 1.00 8 d . . . C(5) C 0.0776(2) 0.4967(6) 0.0117(4) 0.0205(11) Uani 1.00 8 d . . . C(6) C 0.0545(2) 0.5102(7) -0.0800(4) 0.0256(13) Uani 1.00 8 d . . . C(7) C 0.0598(3) 0.4012(8) -0.1350(4) 0.0298(14) Uani 1.00 8 d . . . C(8) C 0.0894(3) 0.2803(8) -0.0989(5) 0.0312(14) Uani 1.00 8 d . . . C(9) C 0.1130(2) 0.2697(7) -0.0088(4) 0.0244(13) Uani 1.00 8 d . . . C(10) C 0.1080(2) 0.3762(6) 0.0523(4) 0.0180(11) Uani 1.00 8 d . . . C(11) C 0.0367(3) 0.7268(7) -0.0079(5) 0.0306(14) Uani 1.00 8 d . . . C(12) C 0.0262(3) 0.6519(7) -0.0980(4) 0.0281(13) Uani 1.00 8 d . . . C(13) C 0.1823(2) 0.3070(6) 0.3549(4) 0.0196(11) Uani 1.00 8 d . . . C(14) C 0.2057(2) 0.4391(6) 0.3789(4) 0.0225(12) Uani 1.00 8 d . . . C(15) C 0.2138(2) 0.4835(6) 0.4664(4) 0.0249(12) Uani 1.00 8 d . . . C(16) C 0.2009(2) 0.3957(7) 0.5282(4) 0.0276(13) Uani 1.00 8 d . . . C(17) C 0.1782(3) 0.2631(7) 0.5034(4) 0.0247(12) Uani 1.00 8 d . . . C(18) C 0.1681(3) 0.2185(6) 0.4173(4) 0.0244(13) Uani 1.00 8 d . . . H(2) H 0.1304 0.5072 0.2540 0.027 Uiso 1.00 8 calc R . . H(3) H 0.0836 0.7069 0.1800 0.030 Uiso 1.00 8 calc R . . H(7) H 0.0436 0.4072 -0.1967 0.036 Uiso 1.00 8 calc R . . H(8) H 0.0933 0.2045 -0.1368 0.037 Uiso 1.00 8 calc R . . H(11A) H 0.0573 0.8156 -0.0074 0.037 Uiso 1.00 8 calc R . . H(11B) H 0.0028 0.7506 0.0062 0.037 Uiso 1.00 8 calc R . . H(12A) H -0.0124 0.6377 -0.1238 0.034 Uiso 1.00 8 calc R . . H(12B) H 0.0405 0.7092 -0.1396 0.034 Uiso 1.00 8 calc R . . H(14) H 0.2159 0.4979 0.3368 0.027 Uiso 1.00 8 calc R . . H(15) H 0.2284 0.5753 0.4836 0.030 Uiso 1.00 8 calc R . . H(16) H 0.2076 0.4261 0.5879 0.033 Uiso 1.00 8 calc R . . H(17) H 0.1697 0.2027 0.5464 0.030 Uiso 1.00 8 calc R . . H(18) H 0.1516 0.1289 0.4000 0.029 Uiso 1.00 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0246(3) 0.0222(3) 0.0296(3) -0.00069(13) 0.00676(19) -0.00029(15) I(2) 0.0243(3) 0.0220(3) 0.0321(3) -0.00234(14) 0.00332(19) 0.00128(16) Te(1) 0.0207(3) 0.0144(3) 0.0186(3) 0.00192(12) 0.00223(18) 0.00116(13) Br(1) 0.0440(4) 0.0278(4) 0.0280(4) 0.0128(3) 0.0038(3) -0.0091(3) C(1) 0.016(2) 0.019(3) 0.021(3) 0.003(2) 0.001(2) 0.005(2) C(2) 0.026(3) 0.021(3) 0.017(3) 0.004(2) 0.002(2) 0.004(2) C(3) 0.029(3) 0.018(3) 0.027(3) 0.002(2) 0.006(3) 0.004(2) C(4) 0.026(3) 0.016(3) 0.023(3) 0.003(2) 0.008(2) 0.008(2) C(5) 0.018(3) 0.025(3) 0.020(3) 0.001(2) 0.007(2) 0.006(2) C(6) 0.023(3) 0.032(3) 0.019(3) 0.001(2) 0.002(2) 0.009(3) C(7) 0.029(3) 0.045(4) 0.014(3) 0.001(3) 0.003(2) 0.005(3) C(8) 0.029(3) 0.039(4) 0.024(3) -0.001(3) 0.005(3) -0.011(3) C(9) 0.026(3) 0.027(3) 0.022(3) 0.000(2) 0.009(2) 0.000(2) C(10) 0.019(3) 0.016(3) 0.018(3) -0.002(2) 0.004(2) 0.002(2) C(11) 0.032(3) 0.027(3) 0.031(3) 0.008(3) 0.004(3) 0.012(3) C(12) 0.023(3) 0.034(3) 0.026(3) 0.005(2) 0.005(3) 0.012(3) C(13) 0.024(3) 0.019(3) 0.013(3) 0.001(2) 0.000(2) 0.001(2) C(14) 0.020(3) 0.021(3) 0.023(3) 0.006(2) -0.000(2) 0.002(2) C(15) 0.025(3) 0.018(3) 0.030(3) 0.002(2) 0.004(2) -0.006(2) C(16) 0.023(3) 0.035(3) 0.024(3) 0.006(3) 0.004(2) -0.004(3) C(17) 0.028(3) 0.024(3) 0.023(3) 0.007(2) 0.009(2) 0.004(2) C(18) 0.031(3) 0.019(3) 0.023(3) 0.005(2) 0.006(3) 0.000(2) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Te(1) 2.9613(8) yes . . I(2) Te(1) 2.9199(8) yes . . Te(1) C(1) 2.135(5) yes . . Te(1) C(13) 2.147(6) yes . . Br(1) C(9) 1.900(6) yes . . C(1) C(2) 1.389(9) yes . . C(1) C(10) 1.436(8) yes . . C(2) C(3) 1.424(8) yes . . C(3) C(4) 1.365(9) yes . . C(4) C(5) 1.409(9) yes . . C(4) C(11) 1.528(8) yes . . C(5) C(6) 1.410(8) yes . . C(5) C(10) 1.431(8) yes . . C(6) C(7) 1.367(10) yes . . C(6) C(12) 1.510(9) yes . . C(7) C(8) 1.403(9) yes . . C(8) C(9) 1.389(9) yes . . C(9) C(10) 1.412(9) yes . . C(11) C(12) 1.537(10) yes . . C(13) C(14) 1.389(8) yes . . C(13) C(18) 1.405(9) yes . . C(14) C(15) 1.396(9) yes . . C(15) C(16) 1.379(10) yes . . C(16) C(17) 1.389(9) yes . . C(17) C(18) 1.371(9) yes . . C(2) H(2) 0.950 yes . . C(3) H(3) 0.950 yes . . C(7) H(7) 0.950 yes . . C(8) H(8) 0.950 yes . . C(11) H(11A) 0.990 yes . . C(11) H(11B) 0.990 yes . . C(12) H(12A) 0.990 yes . . C(12) H(12B) 0.990 yes . . C(14) H(14) 0.950 yes . . C(15) H(15) 0.950 yes . . C(16) H(16) 0.950 yes . . C(17) H(17) 0.950 yes . . C(18) H(18) 0.950 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I(1) Te(1) I(2) 173.039(19) yes . . . I(1) Te(1) C(1) 92.81(16) yes . . . I(1) Te(1) C(13) 91.14(16) yes . . . I(2) Te(1) C(1) 90.00(16) yes . . . I(2) Te(1) C(13) 94.65(16) yes . . . C(1) Te(1) C(13) 100.0(2) yes . . . Te(1) C(1) C(2) 116.8(4) yes . . . Te(1) C(1) C(10) 123.2(4) yes . . . C(2) C(1) C(10) 120.0(5) yes . . . C(1) C(2) C(3) 123.0(5) yes . . . C(2) C(3) C(4) 118.3(6) yes . . . C(3) C(4) C(5) 119.6(5) yes . . . C(3) C(4) C(11) 131.5(6) yes . . . C(5) C(4) C(11) 108.9(5) yes . . . C(4) C(5) C(6) 111.7(5) yes . . . C(4) C(5) C(10) 124.0(5) yes . . . C(6) C(5) C(10) 124.2(6) yes . . . C(5) C(6) C(7) 119.3(6) yes . . . C(5) C(6) C(12) 109.0(5) yes . . . C(7) C(6) C(12) 131.7(6) yes . . . C(6) C(7) C(8) 119.0(6) yes . . . C(7) C(8) C(9) 121.1(6) yes . . . Br(1) C(9) C(8) 115.2(5) yes . . . Br(1) C(9) C(10) 121.8(4) yes . . . C(8) C(9) C(10) 123.0(6) yes . . . C(1) C(10) C(5) 114.9(5) yes . . . C(1) C(10) C(9) 131.8(5) yes . . . C(5) C(10) C(9) 113.3(5) yes . . . C(4) C(11) C(12) 104.6(5) yes . . . C(6) C(12) C(11) 105.7(5) yes . . . Te(1) C(13) C(14) 122.6(5) yes . . . Te(1) C(13) C(18) 116.2(4) yes . . . C(14) C(13) C(18) 121.0(5) yes . . . C(13) C(14) C(15) 118.4(6) yes . . . C(14) C(15) C(16) 120.7(6) yes . . . C(15) C(16) C(17) 120.2(6) yes . . . C(16) C(17) C(18) 120.5(6) yes . . . C(13) C(18) C(17) 119.2(5) yes . . . C(1) C(2) H(2) 118.493 yes . . . C(3) C(2) H(2) 118.489 yes . . . C(2) C(3) H(3) 120.871 yes . . . C(4) C(3) H(3) 120.862 yes . . . C(6) C(7) H(7) 120.477 yes . . . C(8) C(7) H(7) 120.481 yes . . . C(7) C(8) H(8) 119.435 yes . . . C(9) C(8) H(8) 119.438 yes . . . C(4) C(11) H(11A) 110.824 yes . . . C(4) C(11) H(11B) 110.830 yes . . . C(12) C(11) H(11A) 110.832 yes . . . C(12) C(11) H(11B) 110.832 yes . . . H(11A) C(11) H(11B) 108.893 yes . . . C(6) C(12) H(12A) 110.600 yes . . . C(6) C(12) H(12B) 110.585 yes . . . C(11) C(12) H(12A) 110.591 yes . . . C(11) C(12) H(12B) 110.590 yes . . . H(12A) C(12) H(12B) 108.728 yes . . . C(13) C(14) H(14) 120.807 yes . . . C(15) C(14) H(14) 120.813 yes . . . C(14) C(15) H(15) 119.643 yes . . . C(16) C(15) H(15) 119.647 yes . . . C(15) C(16) H(16) 119.918 yes . . . C(17) C(16) H(16) 119.916 yes . . . C(16) C(17) H(17) 119.772 yes . . . C(18) C(17) H(17) 119.775 yes . . . C(13) C(18) H(18) 120.398 yes . . . C(17) C(18) H(18) 120.394 yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I(1) Te(1) C(1) C(2) -90.2(4) no . . . . I(1) Te(1) C(1) C(10) 92.1(4) no . . . . I(1) Te(1) C(13) C(14) 36.8(4) no . . . . I(1) Te(1) C(13) C(18) -137.7(3) no . . . . I(2) Te(1) C(1) C(2) 96.2(4) no . . . . I(2) Te(1) C(1) C(10) -81.5(4) no . . . . I(2) Te(1) C(13) C(14) -147.1(4) no . . . . I(2) Te(1) C(13) C(18) 38.4(3) no . . . . C(1) Te(1) C(13) C(14) -56.2(4) no . . . . C(1) Te(1) C(13) C(18) 129.2(3) no . . . . C(13) Te(1) C(1) C(2) 1.5(4) no . . . . Te(1) C(1) C(10) C(9) -3.0(9) no . . . . C(2) C(1) C(10) C(5) -0.1(8) no . . . . C(10) C(1) C(2) C(3) -2.2(9) no . . . . C(1) C(2) C(3) C(4) 2.9(9) no . . . . C(2) C(3) C(4) C(5) -1.2(9) no . . . . C(3) C(4) C(5) C(10) -1.1(9) no . . . . C(5) C(4) C(11) C(12) 2.1(7) no . . . . C(11) C(4) C(5) C(6) -0.6(7) no . . . . C(4) C(5) C(6) C(12) -1.3(7) no . . . . C(4) C(5) C(10) C(1) 1.8(8) no . . . . C(6) C(5) C(10) C(9) -0.2(8) no . . . . C(10) C(5) C(6) C(7) 1.9(9) no . . . . C(5) C(6) C(7) C(8) -1.9(10) no . . . . C(5) C(6) C(12) C(11) 2.6(7) no . . . . C(6) C(7) C(8) C(9) 0.4(10) no . . . . C(7) C(8) C(9) C(10) 1.4(10) no . . . . Br(1) C(9) C(10) C(1) -3.0(9) no . . . . C(8) C(9) C(10) C(5) -1.5(9) no . . . . C(4) C(11) C(12) C(6) -2.8(6) no . . . . C(14) C(13) C(18) C(17) -1.0(8) no . . . . C(18) C(13) C(14) C(15) -1.3(8) no . . . . C(13) C(14) C(15) C(16) 2.6(8) no . . . . C(14) C(15) C(16) C(17) -1.8(9) no . . . . C(15) C(16) C(17) C(18) -0.5(9) no . . . . C(16) C(17) C(18) C(13) 1.8(9) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Te(1) Br(1) 3.2050(11) yes . . Br(1) C(1) 3.414(6) yes . . C(1) C(4) 2.829(8) yes . . C(2) C(5) 2.737(8) yes . . C(2) C(13) 3.253(8) yes . . C(2) C(14) 3.276(8) yes . . C(3) C(10) 2.885(9) yes . . C(5) C(8) 2.738(10) yes . . C(6) C(9) 2.785(9) yes . . C(7) C(10) 2.884(8) yes . . C(13) C(16) 2.761(9) yes . . C(14) C(17) 2.790(9) yes . . C(15) C(18) 2.776(8) yes . . Br(1) C(15) 3.587(7) yes . 6_545 Br(1) C(17) 3.528(6) yes . 4_554 Br(1) C(18) 3.538(6) yes . 4_554 C(2) C(7) 3.554(10) yes . 4_565 C(4) C(6) 3.528(9) yes . 3_565 C(4) C(17) 3.383(10) yes . 4_564 C(5) C(16) 3.315(9) yes . 4_564 C(5) C(17) 3.487(9) yes . 4_564 C(6) C(4) 3.528(9) yes . 3_565 C(7) C(2) 3.554(10) yes . 4_564 C(9) C(15) 3.599(9) yes . 4_564 C(10) C(16) 3.326(9) yes . 4_564 C(15) Br(1) 3.587(7) yes . 6_555 C(15) C(9) 3.599(9) yes . 4_565 C(15) C(17) 3.577(9) yes . 7_556 C(16) C(5) 3.315(9) yes . 4_565 C(16) C(10) 3.326(9) yes . 4_565 C(16) C(18) 3.465(9) yes . 7_556 C(17) Br(1) 3.528(6) yes . 4_555 C(17) C(4) 3.383(10) yes . 4_565 C(17) C(5) 3.487(9) yes . 4_565 C(17) C(15) 3.577(9) yes . 7_556 C(18) Br(1) 3.538(6) yes . 4_555 C(18) C(16) 3.465(9) yes . 7_556 I(1) H(14) 3.1475 yes . . I(2) H(18) 3.0291 yes . . Te(1) H(2) 3.0016 yes . . Te(1) H(14) 3.1917 yes . . Te(1) H(18) 3.0448 yes . . Br(1) H(8) 2.8107 yes . . C(1) H(3) 3.3232 yes . . C(1) H(14) 3.4114 yes . . C(2) H(14) 2.9463 yes . . C(3) H(11A) 2.9552 yes . . C(3) H(11B) 2.9516 yes . . C(4) H(2) 3.2431 yes . . C(4) H(12A) 3.0731 yes . . C(4) H(12B) 3.1104 yes . . C(5) H(3) 3.2651 yes . . C(5) H(7) 3.2616 yes . . C(5) H(11A) 3.0378 yes . . C(5) H(11B) 3.0638 yes . . C(5) H(12A) 3.0217 yes . . C(5) H(12B) 3.0536 yes . . C(6) H(8) 3.2422 yes . . C(6) H(11A) 3.0754 yes . . C(6) H(11B) 3.1121 yes . . C(7) H(12A) 2.9425 yes . . C(7) H(12B) 2.9293 yes . . C(9) H(7) 3.2873 yes . . C(10) H(2) 3.2986 yes . . C(10) H(8) 3.3070 yes . . C(11) H(3) 2.8833 yes . . C(12) H(7) 2.8697 yes . . C(13) H(2) 2.5939 yes . . C(13) H(15) 3.2509 yes . . C(13) H(17) 3.2555 yes . . C(14) H(2) 2.4637 yes . . C(14) H(16) 3.2673 yes . . C(14) H(18) 3.2872 yes . . C(15) H(2) 3.4724 yes . . C(15) H(17) 3.2538 yes . . C(16) H(14) 3.2702 yes . . C(16) H(18) 3.2551 yes . . C(17) H(15) 3.2543 yes . . C(18) H(14) 3.2920 yes . . C(18) H(16) 3.2496 yes . . H(2) H(3) 2.3655 yes . . H(2) H(14) 2.2663 yes . . H(3) H(11A) 3.0137 yes . . H(3) H(11B) 3.0017 yes . . H(7) H(8) 2.3522 yes . . H(7) H(12A) 2.9978 yes . . H(7) H(12B) 2.9777 yes . . H(11A) H(12A) 2.7690 yes . . H(11A) H(12B) 2.2376 yes . . H(11B) H(12A) 2.2374 yes . . H(11B) H(12B) 2.7430 yes . . H(14) H(15) 2.3526 yes . . H(15) H(16) 2.3228 yes . . H(16) H(17) 2.3342 yes . . H(17) H(18) 2.3234 yes . . I(1) H(14) 3.3098 yes . 6_545 I(1) H(16) 3.1879 yes . 4_564 I(2) H(3) 3.5043 yes . 1_545 I(2) H(8) 3.3415 yes . 4_555 I(2) H(12A) 3.3331 yes . 3_565 I(2) H(12B) 3.5650 yes . 3_565 I(2) H(12B) 3.2536 yes . 4_565 Br(1) H(15) 3.1113 yes . 6_545 Br(1) H(17) 2.9018 yes . 4_554 Br(1) H(18) 2.9400 yes . 4_554 C(1) H(12A) 2.9539 yes . 3_565 C(1) H(16) 3.0439 yes . 4_564 C(2) H(7) 3.0450 yes . 4_565 C(2) H(12A) 2.9866 yes . 3_565 C(2) H(16) 3.2476 yes . 4_564 C(3) H(7) 2.9906 yes . 4_565 C(3) H(12A) 3.1259 yes . 3_565 C(3) H(16) 3.4983 yes . 4_564 C(3) H(17) 3.3707 yes . 4_564 C(4) H(12A) 3.1266 yes . 3_565 C(4) H(16) 3.5565 yes . 4_564 C(4) H(17) 3.1708 yes . 4_564 C(5) H(11B) 3.0884 yes . 3_565 C(5) H(12A) 3.0238 yes . 3_565 C(5) H(16) 3.3628 yes . 4_564 C(6) H(11B) 3.2355 yes . 3_565 C(7) H(2) 2.9743 yes . 4_564 C(7) H(3) 3.2839 yes . 4_564 C(7) H(7) 3.2387 yes . 2_554 C(7) H(11B) 3.2412 yes . 3_565 C(8) H(2) 3.4254 yes . 4_564 C(8) H(3) 3.4325 yes . 4_564 C(8) H(11B) 3.1332 yes . 3_565 C(9) H(11B) 3.0352 yes . 3_565 C(9) H(15) 3.3718 yes . 4_564 C(10) H(11B) 3.0346 yes . 3_565 C(10) H(12A) 2.9948 yes . 3_565 C(10) H(16) 3.1182 yes . 4_564 C(11) H(17) 3.4105 yes . 4_564 C(13) H(16) 3.5312 yes . 7_556 C(14) H(17) 3.4203 yes . 7_556 C(15) H(17) 3.5554 yes . 7_556 C(17) H(11A) 3.1981 yes . 4_565 C(18) H(11A) 3.4104 yes . 4_565 C(18) H(12B) 3.2791 yes . 4_565 C(18) H(16) 3.5351 yes . 7_556 H(2) C(7) 2.9743 yes . 4_565 H(2) C(8) 3.4254 yes . 4_565 H(2) H(7) 2.6982 yes . 4_565 H(2) H(8) 3.4706 yes . 4_565 H(2) H(12A) 3.4883 yes . 3_565 H(3) I(2) 3.5043 yes . 1_565 H(3) C(7) 3.2839 yes . 4_565 H(3) C(8) 3.4325 yes . 4_565 H(3) H(7) 3.5602 yes . 3_565 H(3) H(7) 2.6523 yes . 4_565 H(3) H(8) 2.9360 yes . 4_565 H(3) H(17) 3.5532 yes . 4_564 H(7) C(2) 3.0450 yes . 4_564 H(7) C(3) 2.9906 yes . 4_564 H(7) C(7) 3.2387 yes . 2_554 H(7) H(2) 2.6982 yes . 4_564 H(7) H(3) 3.5602 yes . 3_565 H(7) H(3) 2.6523 yes . 4_564 H(7) H(7) 2.4423 yes . 2_554 H(7) H(12A) 3.4716 yes . 2_554 H(8) I(2) 3.3415 yes . 4_554 H(8) H(2) 3.4706 yes . 4_564 H(8) H(3) 2.9360 yes . 4_564 H(8) H(18) 3.4573 yes . 4_554 H(11A) C(17) 3.1981 yes . 4_564 H(11A) C(18) 3.4104 yes . 4_564 H(11A) H(17) 2.8323 yes . 4_564 H(11A) H(18) 3.2096 yes . 4_564 H(11B) C(5) 3.0884 yes . 3_565 H(11B) C(6) 3.2355 yes . 3_565 H(11B) C(7) 3.2412 yes . 3_565 H(11B) C(8) 3.1332 yes . 3_565 H(11B) C(9) 3.0352 yes . 3_565 H(11B) C(10) 3.0346 yes . 3_565 H(12A) I(2) 3.3331 yes . 3_565 H(12A) C(1) 2.9539 yes . 3_565 H(12A) C(2) 2.9866 yes . 3_565 H(12A) C(3) 3.1259 yes . 3_565 H(12A) C(4) 3.1266 yes . 3_565 H(12A) C(5) 3.0238 yes . 3_565 H(12A) C(10) 2.9948 yes . 3_565 H(12A) H(2) 3.4883 yes . 3_565 H(12A) H(7) 3.4716 yes . 2_554 H(12B) I(2) 3.5650 yes . 3_565 H(12B) I(2) 3.2536 yes . 4_564 H(12B) C(18) 3.2791 yes . 4_564 H(12B) H(12B) 3.5485 yes . 2_554 H(12B) H(18) 3.1831 yes . 4_564 H(14) I(1) 3.3098 yes . 6_555 H(14) H(17) 3.5940 yes . 7_556 H(15) Br(1) 3.1113 yes . 6_555 H(15) C(9) 3.3718 yes . 4_565 H(15) H(15) 3.4601 yes . 7_566 H(16) I(1) 3.1879 yes . 4_565 H(16) C(1) 3.0439 yes . 4_565 H(16) C(2) 3.2476 yes . 4_565 H(16) C(3) 3.4983 yes . 4_565 H(16) C(4) 3.5565 yes . 4_565 H(16) C(5) 3.3628 yes . 4_565 H(16) C(10) 3.1182 yes . 4_565 H(16) C(13) 3.5312 yes . 7_556 H(16) C(18) 3.5351 yes . 7_556 H(17) Br(1) 2.9018 yes . 4_555 H(17) C(3) 3.3707 yes . 4_565 H(17) C(4) 3.1708 yes . 4_565 H(17) C(11) 3.4105 yes . 4_565 H(17) C(14) 3.4203 yes . 7_556 H(17) C(15) 3.5554 yes . 7_556 H(17) H(3) 3.5532 yes . 4_565 H(17) H(11A) 2.8323 yes . 4_565 H(17) H(14) 3.5940 yes . 7_556 H(18) Br(1) 2.9400 yes . 4_555 H(18) H(8) 3.4573 yes . 4_555 H(18) H(11A) 3.2096 yes . 4_565 H(18) H(12B) 3.1831 yes . 4_565 #============================================================================== data_Ferg110-3 _database_code_depnum_ccdc_archive 'CCDC 850823' #TrackingRef '- 8.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 Br2 S Te' _chemical_formula_moiety 'C24 H18 Br2 S Te' _chemical_formula_weight 625.87 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.516(5) _cell_length_b 12.616(5) _cell_length_c 14.436(6) _cell_angle_alpha 90.0000 _cell_angle_beta 112.682(8) _cell_angle_gamma 90.0000 _cell_volume 2103.0(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6951 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description chunk _exptl_crystal_colour paleYellow _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200.00 _exptl_absorpt_coefficient_mu 5.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.852 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.257 _diffrn_reflns_number 15439 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3693 _reflns_number_gt 3138 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0950 _refine_ls_wR_factor_ref 0.2857 _refine_ls_number_restraints 12 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3692 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1143P)^2^+31.5372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 2.000 _refine_diff_density_min -2.240 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.5308 1.6751 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.64934(6) 0.03009(6) 0.96766(5) 0.0208(2) Uani 1.0 4 d . . . Br1 Br 0.55990(10) 0.22579(10) 0.94092(9) 0.0275(4) Uani 1.0 4 d . . . Br2 Br 0.73336(11) -0.16740(10) 0.97870(9) 0.0298(4) Uani 1.0 4 d . . . S1 S 0.4495(3) -0.1167(3) 0.8133(2) 0.0227(8) Uani 1.0 4 d . . . C1 C 0.6667(10) 0.0444(10) 0.8249(9) 0.022(3) Uani 1.0 4 d . . . C2 C 0.7465(10) 0.1170(10) 0.8229(10) 0.027(4) Uani 1.0 4 d . . . C3 C 0.7797(11) 0.1289(11) 0.7397(10) 0.031(4) Uani 1.0 4 d . . . C4 C 0.7317(11) 0.0543(11) 0.6628(10) 0.029(4) Uani 1.0 4 d . . . C5 C 0.6531(11) -0.0200(10) 0.6652(10) 0.026(4) Uani 1.0 4 d . . . C6 C 0.6154(9) -0.0851(9) 0.5818(9) 0.0197(8) Uani 1.0 4 d . . . C7 C 0.5348(10) -0.1668(11) 0.5716(9) 0.026(4) Uani 1.0 4 d . . . C8 C 0.4908(11) -0.1728(10) 0.6476(9) 0.027(4) Uani 1.0 4 d . . . C9 C 0.5257(10) -0.1039(10) 0.7289(9) 0.024(3) Uani 1.0 4 d . . . C10 C 0.6102(10) -0.0278(9) 0.7437(9) 0.022(3) Uani 1.0 4 d . . . C11 C 0.7575(11) 0.0364(11) 0.5681(10) 0.030(4) Uani 1.0 4 d . . . C12 C 0.6789(10) -0.0572(10) 0.5169(9) 0.025(4) Uani 1.0 4 d . . . C13 C 0.8181(9) 0.0944(9) 1.0608(8) 0.0159(8) Uani 1.0 4 d . . . C14 C 0.8217(12) 0.1881(11) 1.1136(10) 0.033(4) Uani 1.0 4 d . . . C15 C 0.9319(11) 0.2256(11) 1.1778(10) 0.030(4) Uani 1.0 4 d . . . C16 C 1.0314(11) 0.1729(11) 1.1842(10) 0.032(4) Uani 1.0 4 d . . . C17 C 1.0257(12) 0.0816(12) 1.1347(11) 0.036(4) Uani 1.0 4 d . . . C18 C 0.9209(11) 0.0392(11) 1.0687(10) 0.031(4) Uani 1.0 4 d . . . C19 C 0.3171(9) -0.0446(9) 0.7476(8) 0.017(3) Uani 1.0 4 d . . . C20 C 0.3042(10) 0.0572(11) 0.7784(10) 0.026(4) Uani 1.0 4 d . . . C21 C 0.2005(10) 0.1114(11) 0.7335(10) 0.027(4) Uani 1.0 4 d . . . C22 C 0.1083(11) 0.0653(11) 0.6536(10) 0.029(4) Uani 1.0 4 d . . . C23 C 0.1229(11) -0.0361(10) 0.6237(10) 0.028(4) Uani 1.0 4 d . . . C24 C 0.2236(11) -0.0914(12) 0.6693(10) 0.033(4) Uani 1.0 4 d . . . H2 H 0.7815 0.1616 0.8796 0.0318 Uiso 1.0 4 calc R . . H3 H 0.8306 0.1834 0.7365 0.0373 Uiso 1.0 4 calc R . . H7 H 0.5115 -0.2149 0.5167 0.0316 Uiso 1.0 4 calc R . . H8 H 0.4352 -0.2259 0.6431 0.0322 Uiso 1.0 4 calc R . . H11A H 0.7378 0.0999 0.5244 0.0359 Uiso 1.0 4 calc R . . H11B H 0.8401 0.0185 0.5857 0.0359 Uiso 1.0 4 calc R . . H12A H 0.6240 -0.0369 0.4489 0.0303 Uiso 1.0 4 calc R . . H12B H 0.7256 -0.1181 0.5108 0.0303 Uiso 1.0 4 calc R . . H14 H 0.7529 0.2250 1.1067 0.0391 Uiso 1.0 4 calc R . . H15 H 0.9377 0.2876 1.2169 0.0360 Uiso 1.0 4 calc R . . H16 H 1.1049 0.2016 1.2243 0.0385 Uiso 1.0 4 calc R . . H17 H 1.0955 0.0446 1.1448 0.0432 Uiso 1.0 4 calc R . . H18 H 0.9181 -0.0232 1.0310 0.0374 Uiso 1.0 4 calc R . . H20 H 0.3670 0.0900 0.8308 0.0317 Uiso 1.0 4 calc R . . H21 H 0.1917 0.1800 0.7568 0.0328 Uiso 1.0 4 calc R . . H22 H 0.0377 0.1027 0.6209 0.0343 Uiso 1.0 4 calc R . . H23 H 0.0612 -0.0682 0.5698 0.0336 Uiso 1.0 4 calc R . . H24 H 0.2303 -0.1615 0.6481 0.0398 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te1 0.0236(4) 0.0196(4) 0.0165(4) -0.0004(3) 0.0049(3) 0.0004(3) Br1 0.0296(6) 0.0234(7) 0.0238(6) 0.0048(5) 0.0042(5) -0.0020(5) Br2 0.0351(7) 0.0208(6) 0.0272(6) 0.0029(5) 0.0050(6) 0.0020(5) S1 0.0283(14) 0.0204(15) 0.0190(14) -0.0033(12) 0.0086(12) 0.0018(12) C1 0.025(6) 0.021(6) 0.018(6) -0.001(5) 0.007(5) 0.001(5) C2 0.025(6) 0.027(7) 0.023(6) 0.000(6) 0.005(5) -0.001(6) C3 0.034(7) 0.028(7) 0.033(7) 0.002(6) 0.014(6) 0.003(6) C4 0.028(6) 0.028(7) 0.030(7) 0.002(6) 0.010(5) 0.004(6) C5 0.025(6) 0.023(7) 0.028(6) 0.002(5) 0.007(5) 0.000(6) C6 0.0186(10) 0.0205(10) 0.0155(11) 0.0084(8) 0.0015(7) 0.0059(8) C7 0.027(6) 0.029(7) 0.026(6) 0.000(6) 0.014(5) 0.004(6) C8 0.029(6) 0.025(7) 0.027(6) 0.001(6) 0.012(5) 0.004(6) C9 0.025(6) 0.023(6) 0.023(6) 0.005(5) 0.009(5) -0.002(5) C10 0.023(6) 0.017(6) 0.022(6) 0.005(5) 0.005(5) 0.001(5) C11 0.031(6) 0.030(7) 0.027(7) -0.001(6) 0.009(6) -0.001(6) C12 0.022(6) 0.024(6) 0.025(6) 0.000(5) 0.004(5) -0.002(6) C13 0.0149(10) 0.0151(10) 0.0124(11) -0.0057(8) -0.0004(7) 0.0041(8) C14 0.033(7) 0.035(8) 0.028(7) -0.000(6) 0.009(6) -0.002(6) C15 0.035(7) 0.029(7) 0.024(6) -0.000(6) 0.010(6) -0.001(6) C16 0.029(7) 0.032(7) 0.033(7) -0.005(6) 0.010(6) -0.002(6) C17 0.037(7) 0.034(8) 0.033(7) 0.008(6) 0.010(6) -0.005(6) C18 0.028(6) 0.027(7) 0.032(7) -0.005(6) 0.005(6) -0.003(6) C19 0.022(5) 0.016(6) 0.016(5) 0.001(5) 0.010(5) 0.005(5) C20 0.023(6) 0.030(7) 0.027(6) -0.008(6) 0.010(5) -0.003(6) C21 0.027(6) 0.025(7) 0.027(7) 0.003(5) 0.007(6) -0.002(6) C22 0.029(6) 0.027(7) 0.026(7) -0.000(6) 0.006(6) 0.002(6) C23 0.030(6) 0.024(7) 0.025(6) -0.005(6) 0.006(5) -0.002(6) C24 0.039(7) 0.033(8) 0.029(7) -0.002(6) 0.014(6) -0.002(6) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Te1 Br1 2.6766(17) yes . . Te1 Br2 2.6850(17) yes . . Te1 C1 2.161(14) yes . . Te1 C13 2.176(10) yes . . S1 C9 1.821(15) yes . . S1 C19 1.806(11) yes . . C1 C2 1.364(19) yes . . C1 C10 1.438(16) yes . . C2 C3 1.42(3) yes . . C3 C4 1.402(18) yes . . C4 C5 1.369(19) yes . . C4 C11 1.54(3) yes . . C5 C6 1.382(17) yes . . C5 C10 1.43(3) yes . . C6 C7 1.409(18) yes . . C6 C12 1.49(2) yes . . C7 C8 1.41(3) yes . . C8 C9 1.389(18) yes . . C9 C10 1.382(17) yes . . C11 C12 1.532(17) yes . . C13 C14 1.398(18) yes . . C13 C18 1.429(18) yes . . C14 C15 1.415(17) yes . . C15 C16 1.38(2) yes . . C16 C17 1.34(2) yes . . C17 C18 1.397(17) yes . . C19 C20 1.389(18) yes . . C19 C24 1.406(15) yes . . C20 C21 1.387(16) yes . . C21 C22 1.405(16) yes . . C22 C23 1.384(19) yes . . C23 C24 1.366(18) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br1 Te1 Br2 175.49(5) yes . . . Br1 Te1 C1 88.6(4) yes . . . Br1 Te1 C13 89.8(3) yes . . . Br2 Te1 C1 87.3(4) yes . . . Br2 Te1 C13 92.6(3) yes . . . C1 Te1 C13 97.3(5) yes . . . C9 S1 C19 102.4(6) yes . . . Te1 C1 C2 114.9(9) yes . . . Te1 C1 C10 121.8(10) yes . . . C2 C1 C10 122.8(13) yes . . . C1 C2 C3 123.0(12) yes . . . C2 C3 C4 115.0(13) yes . . . C3 C4 C5 122.2(15) yes . . . C3 C4 C11 129.1(13) yes . . . C5 C4 C11 108.7(12) yes . . . C4 C5 C6 113.1(14) yes . . . C4 C5 C10 124.0(12) yes . . . C6 C5 C10 122.8(12) yes . . . C5 C6 C7 121.1(13) yes . . . C5 C6 C12 108.8(11) yes . . . C7 C6 C12 130.0(11) yes . . . C6 C7 C8 116.0(12) yes . . . C7 C8 C9 122.4(12) yes . . . S1 C9 C8 115.8(10) yes . . . S1 C9 C10 121.7(10) yes . . . C8 C9 C10 122.5(14) yes . . . C1 C10 C5 112.7(11) yes . . . C1 C10 C9 132.2(14) yes . . . C5 C10 C9 115.1(11) yes . . . C4 C11 C12 103.1(12) yes . . . C6 C12 C11 106.2(11) yes . . . Te1 C13 C14 118.2(9) yes . . . Te1 C13 C18 119.8(8) yes . . . C14 C13 C18 122.0(10) yes . . . C13 C14 C15 117.3(13) yes . . . C14 C15 C16 120.5(13) yes . . . C15 C16 C17 121.1(12) yes . . . C16 C17 C18 122.3(14) yes . . . C13 C18 C17 116.6(13) yes . . . S1 C19 C20 119.6(8) yes . . . S1 C19 C24 121.4(10) yes . . . C20 C19 C24 118.9(10) yes . . . C19 C20 C21 120.6(10) yes . . . C20 C21 C22 120.3(12) yes . . . C21 C22 C23 118.2(11) yes . . . C22 C23 C24 122.0(11) yes . . . C19 C24 C23 120.0(13) yes . . . C1 C2 H2 118.498 no . . . C3 C2 H2 118.489 no . . . C2 C3 H3 122.524 no . . . C4 C3 H3 122.517 no . . . C6 C7 H7 122.015 no . . . C8 C7 H7 122.016 no . . . C7 C8 H8 118.812 no . . . C9 C8 H8 118.816 no . . . C4 C11 H11A 111.149 no . . . C4 C11 H11B 111.144 no . . . C12 C11 H11A 111.144 no . . . C12 C11 H11B 111.143 no . . . H11A C11 H11B 109.089 no . . . C6 C12 H12A 110.494 no . . . C6 C12 H12B 110.500 no . . . C11 C12 H12A 110.498 no . . . C11 C12 H12B 110.494 no . . . H12A C12 H12B 108.668 no . . . C13 C14 H14 121.350 no . . . C15 C14 H14 121.348 no . . . C14 C15 H15 119.731 no . . . C16 C15 H15 119.735 no . . . C15 C16 H16 119.469 no . . . C17 C16 H16 119.469 no . . . C16 C17 H17 118.844 no . . . C18 C17 H17 118.844 no . . . C13 C18 H18 121.691 no . . . C17 C18 H18 121.696 no . . . C19 C20 H20 119.701 no . . . C21 C20 H20 119.704 no . . . C20 C21 H21 119.856 no . . . C22 C21 H21 119.851 no . . . C21 C22 H22 120.897 no . . . C23 C22 H22 120.897 no . . . C22 C23 H23 118.989 no . . . C24 C23 H23 118.989 no . . . C19 C24 H24 120.024 no . . . C23 C24 H24 120.020 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br1 Te1 C1 C2 67.8(7) no . . . . Br1 Te1 C1 C10 -120.6(8) no . . . . Br1 Te1 C13 C14 28.3(7) no . . . . Br1 Te1 C13 C18 -153.5(8) no . . . . Br2 Te1 C1 C2 -114.1(7) no . . . . Br2 Te1 C1 C10 57.5(7) no . . . . Br2 Te1 C13 C14 -155.5(7) no . . . . Br2 Te1 C13 C18 22.7(8) no . . . . C1 Te1 C13 C14 116.9(8) no . . . . C1 Te1 C13 C18 -64.9(8) no . . . . C13 Te1 C1 C2 -21.9(8) no . . . . C13 Te1 C1 C10 149.7(8) no . . . . C9 S1 C19 C20 -102.3(10) no . . . . C9 S1 C19 C24 81.4(10) no . . . . C19 S1 C9 C8 -80.3(8) no . . . . C19 S1 C9 C10 97.6(8) no . . . . Te1 C1 C2 C3 172.5(7) no . . . . Te1 C1 C10 C5 -166.7(6) no . . . . Te1 C1 C10 C9 11.4(17) no . . . . C2 C1 C10 C5 4.3(15) no . . . . C2 C1 C10 C9 -177.6(11) no . . . . C10 C1 C2 C3 1.0(18) no . . . . C1 C2 C3 C4 -5.2(17) no . . . . C2 C3 C4 C5 4.0(17) no . . . . C2 C3 C4 C11 -173.2(10) no . . . . C3 C4 C5 C6 179.3(10) no . . . . C3 C4 C5 C10 1.5(18) no . . . . C3 C4 C11 C12 179.0(11) no . . . . C5 C4 C11 C12 1.4(12) no . . . . C11 C4 C5 C6 -3.0(13) no . . . . C11 C4 C5 C10 179.2(9) no . . . . C4 C5 C6 C7 179.6(9) no . . . . C4 C5 C6 C12 3.3(13) no . . . . C4 C5 C10 C1 -5.6(16) no . . . . C4 C5 C10 C9 176.0(10) no . . . . C6 C5 C10 C1 176.9(10) no . . . . C6 C5 C10 C9 -1.5(16) no . . . . C10 C5 C6 C7 -2.6(16) no . . . . C10 C5 C6 C12 -178.9(9) no . . . . C5 C6 C7 C8 3.9(15) no . . . . C5 C6 C12 C11 -2.2(11) no . . . . C7 C6 C12 C11 -178.0(10) no . . . . C12 C6 C7 C8 179.2(10) no . . . . C6 C7 C8 C9 -1.1(16) no . . . . C7 C8 C9 S1 174.7(9) no . . . . C7 C8 C9 C10 -3.2(17) no . . . . S1 C9 C10 C1 8.5(17) no . . . . S1 C9 C10 C5 -173.4(7) no . . . . C8 C9 C10 C1 -173.7(10) no . . . . C8 C9 C10 C5 4.4(16) no . . . . C4 C11 C12 C6 0.5(11) no . . . . Te1 C13 C14 C15 176.8(8) no . . . . Te1 C13 C18 C17 -176.1(8) no . . . . C14 C13 C18 C17 2.0(19) no . . . . C18 C13 C14 C15 -1.4(19) no . . . . C13 C14 C15 C16 2(2) no . . . . C14 C15 C16 C17 -4(3) no . . . . C15 C16 C17 C18 5(3) no . . . . C16 C17 C18 C13 -4(3) no . . . . S1 C19 C20 C21 -175.7(9) no . . . . S1 C19 C24 C23 177.5(10) no . . . . C20 C19 C24 C23 1(2) no . . . . C24 C19 C20 C21 1(2) no . . . . C19 C20 C21 C22 -2(2) no . . . . C20 C21 C22 C23 2(2) no . . . . C21 C22 C23 C24 -0(3) no . . . . C22 C23 C24 C19 -1(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Te1 S1 3.218(3) no . . Br1 C14 3.298(12) no . . Br2 S1 3.491(3) no . . Br2 C10 3.599(12) no . . Br2 C18 3.412(13) no . . S1 C1 3.346(13) no . . C1 C4 2.76(2) no . . C2 C5 2.735(17) no . . C2 C13 3.210(17) no . . C2 C18 3.514(17) no . . C3 C10 2.917(19) no . . C5 C8 2.740(19) no . . C6 C9 2.77(2) no . . C7 C10 2.885(17) no . . C8 C19 3.44(2) no . . C9 C24 3.544(19) no . . C13 C16 2.759(15) no . . C14 C17 2.80(2) no . . C15 C18 2.80(2) no . . C19 C22 2.803(16) no . . C20 C23 2.759(16) no . . C21 C24 2.77(2) no . . Br1 C15 3.560(13) no . 4_454 C3 C17 3.587(18) no . 3_757 C11 C24 3.59(3) no . 3_656 C15 Br1 3.560(13) no . 4_555 C17 C3 3.587(18) no . 3_757 C17 C18 3.59(3) no . 3_757 C18 C17 3.59(3) no . 3_757 C18 C18 3.44(3) no . 3_757 C24 C11 3.59(3) no . 3_656 Te1 H2 2.9541 no . . Te1 H14 3.1224 no . . Te1 H18 3.1988 no . . Te1 H20 3.4026 no . . Br1 H2 3.3210 no . . Br1 H14 2.6652 no . . Br1 H20 2.8860 no . . Br2 H18 2.8071 no . . S1 H8 2.7609 no . . S1 H20 2.8523 no . . S1 H24 2.9131 no . . C1 H3 3.3064 no . . C1 H18 3.5013 no . . C2 H18 3.4336 no . . C3 H11A 2.9684 no . . C3 H11B 2.9575 no . . C4 H2 3.2415 no . . C4 H12A 3.0768 no . . C4 H12B 3.0707 no . . C5 H3 3.2887 no . . C5 H7 3.2935 no . . C5 H11A 3.0337 no . . C5 H11B 3.0164 no . . C5 H12A 3.0081 no . . C5 H12B 2.9813 no . . C6 H8 3.2499 no . . C6 H11A 3.0760 no . . C6 H11B 3.0820 no . . C7 H12A 2.9312 no . . C7 H12B 2.9107 no . . C8 H24 3.2662 no . . C9 H7 3.3099 no . . C9 H24 3.4976 no . . C10 H2 3.3034 no . . C10 H8 3.2704 no . . C11 H3 2.9107 no . . C12 H7 2.8878 no . . C13 H2 2.6161 no . . C13 H15 3.2643 no . . C13 H17 3.2670 no . . C14 H2 3.2354 no . . C14 H16 3.2834 no . . C14 H18 3.3309 no . . C15 H17 3.2221 no . . C16 H14 3.2907 no . . C16 H18 3.2560 no . . C17 H15 3.2219 no . . C18 H2 3.0338 no . . C18 H14 3.3331 no . . C18 H16 3.2495 no . . C19 H8 3.3780 no . . C19 H21 3.2657 no . . C19 H23 3.2548 no . . C20 H22 3.2821 no . . C20 H24 3.2662 no . . C21 H23 3.2519 no . . C22 H20 3.2773 no . . C22 H24 3.2587 no . . C23 H21 3.2540 no . . C24 H8 3.2874 no . . C24 H20 3.2669 no . . C24 H22 3.2617 no . . H2 H3 2.3870 no . . H2 H14 3.5251 no . . H2 H18 3.2017 no . . H3 H11A 3.0150 no . . H3 H11B 3.0458 no . . H7 H8 2.3677 no . . H7 H12A 3.0065 no . . H7 H12B 2.9754 no . . H8 H24 2.7170 no . . H11A H12A 2.2361 no . . H11A H12B 2.7579 no . . H11B H12A 2.7537 no . . H11B H12B 2.2360 no . . H14 H15 2.3805 no . . H15 H16 2.3222 no . . H16 H17 2.2692 no . . H17 H18 2.3551 no . . H20 H21 2.3311 no . . H21 H22 2.3658 no . . H22 H23 2.3327 no . . H23 H24 2.3022 no . . Te1 H20 3.3558 no . 3_657 Br1 H12B 3.1818 no . 2_656 Br1 H15 3.0025 no . 4_454 Br1 H16 3.5060 no . 4_454 Br1 H22 3.4739 no . 4_555 Br1 H23 2.9826 no . 2_556 Br2 H3 3.4523 no . 2_646 Br2 H8 3.0334 no . 4_545 Br2 H11A 2.9600 no . 2_646 Br2 H20 3.5717 no . 3_657 Br2 H21 3.5669 no . 3_657 Br2 H24 3.2727 no . 4_545 S1 H14 3.4454 no . 3_657 S1 H21 3.0570 no . 2_546 C1 H15 3.4193 no . 4_454 C1 H16 3.4796 no . 4_454 C1 H17 3.0512 no . 3_757 C2 H16 2.9083 no . 4_454 C2 H17 2.7518 no . 3_757 C3 H16 3.0051 no . 4_454 C3 H17 2.8289 no . 3_757 C4 H17 3.0519 no . 3_757 C5 H12A 3.2944 no . 3_656 C5 H17 3.2961 no . 3_757 C6 H2 3.4107 no . 2_646 C6 H12A 3.2438 no . 3_656 C7 H2 3.0369 no . 2_646 C7 H3 3.2381 no . 2_646 C7 H11A 3.2596 no . 3_656 C7 H12A 3.1920 no . 3_656 C8 H3 2.8643 no . 2_646 C8 H11A 3.1172 no . 3_656 C8 H12A 3.0760 no . 3_656 C9 H3 3.1609 no . 2_646 C9 H12A 3.0901 no . 3_656 C10 H12A 3.2718 no . 3_656 C10 H17 3.4107 no . 3_757 C11 H22 3.3937 no . 1_655 C11 H23 3.5714 no . 3_656 C11 H24 3.5523 no . 3_656 C12 H14 3.5546 no . 2_646 C14 H7 3.5251 no . 2_656 C14 H12B 2.9549 no . 2_656 C14 H21 3.5042 no . 4_555 C15 H7 3.2375 no . 2_656 C15 H12A 3.4381 no . 2_656 C15 H12B 3.3233 no . 2_656 C15 H20 3.5114 no . 4_555 C16 H7 3.0831 no . 2_656 C17 H7 3.2862 no . 2_656 C17 H18 2.8377 no . 3_757 C18 H7 3.5589 no . 2_656 C18 H17 3.1897 no . 3_757 C18 H18 2.8995 no . 3_757 C19 H12A 3.3555 no . 3_656 C19 H14 3.4339 no . 3_657 C19 H21 3.4765 no . 2_546 C20 H14 3.5884 no . 4_454 C20 H15 2.9259 no . 4_454 C21 H8 3.5505 no . 2_556 C21 H14 2.9937 no . 4_454 C21 H15 3.3238 no . 4_454 C21 H24 3.2771 no . 2_556 C22 H11B 3.1683 no . 1_455 C22 H14 3.4169 no . 4_454 C22 H23 3.1018 no . 3_556 C23 H11A 3.3359 no . 3_656 C23 H11B 3.4370 no . 1_455 C23 H11B 3.2372 no . 3_656 C23 H22 3.4264 no . 3_556 C23 H23 3.1426 no . 3_556 C24 H11A 3.0175 no . 3_656 C24 H11B 3.5733 no . 3_656 C24 H12A 3.4181 no . 3_656 C24 H14 3.5563 no . 3_657 C24 H21 3.1156 no . 2_546 H2 C6 3.4107 no . 2_656 H2 C7 3.0369 no . 2_656 H2 H7 2.8962 no . 2_656 H2 H12B 3.2166 no . 2_656 H2 H16 3.0115 no . 4_454 H2 H17 3.1110 no . 3_757 H3 Br2 3.4523 no . 2_656 H3 C7 3.2381 no . 2_656 H3 C8 2.8643 no . 2_656 H3 C9 3.1609 no . 2_656 H3 H7 3.5795 no . 2_656 H3 H8 2.9990 no . 2_656 H3 H16 3.1195 no . 4_454 H3 H17 3.2926 no . 3_757 H7 C14 3.5251 no . 2_646 H7 C15 3.2375 no . 2_646 H7 C16 3.0831 no . 2_646 H7 C17 3.2862 no . 2_646 H7 C18 3.5589 no . 2_646 H7 H2 2.8962 no . 2_646 H7 H3 3.5795 no . 2_646 H7 H11A 3.2813 no . 3_656 H7 H16 3.3805 no . 2_646 H7 H18 3.5378 no . 4_444 H8 Br2 3.0334 no . 4_444 H8 C21 3.5505 no . 2_546 H8 H3 2.9990 no . 2_646 H8 H11A 3.0038 no . 3_656 H8 H12A 3.5422 no . 3_656 H8 H18 3.5239 no . 4_444 H8 H21 2.7915 no . 2_546 H11A Br2 2.9600 no . 2_656 H11A C7 3.2596 no . 3_656 H11A C8 3.1172 no . 3_656 H11A C23 3.3359 no . 3_656 H11A C24 3.0175 no . 3_656 H11A H7 3.2813 no . 3_656 H11A H8 3.0038 no . 3_656 H11A H22 3.4640 no . 1_655 H11A H23 3.3134 no . 3_656 H11A H24 2.7804 no . 3_656 H11B C22 3.1683 no . 1_655 H11B C23 3.4370 no . 1_655 H11B C23 3.2372 no . 3_656 H11B C24 3.5733 no . 3_656 H11B H22 2.5565 no . 1_655 H11B H23 3.0654 no . 1_655 H11B H23 3.0166 no . 3_656 H12A C5 3.2944 no . 3_656 H12A C6 3.2438 no . 3_656 H12A C7 3.1920 no . 3_656 H12A C8 3.0760 no . 3_656 H12A C9 3.0901 no . 3_656 H12A C10 3.2718 no . 3_656 H12A C15 3.4381 no . 2_646 H12A C19 3.3555 no . 3_656 H12A C24 3.4181 no . 3_656 H12A H8 3.5422 no . 3_656 H12A H15 3.1299 no . 2_646 H12B Br1 3.1818 no . 2_646 H12B C14 2.9549 no . 2_646 H12B C15 3.3233 no . 2_646 H12B H2 3.2166 no . 2_646 H12B H14 2.6862 no . 2_646 H12B H15 3.3480 no . 2_646 H14 S1 3.4454 no . 3_657 H14 C12 3.5546 no . 2_656 H14 C19 3.4339 no . 3_657 H14 C20 3.5884 no . 4_555 H14 C21 2.9937 no . 4_555 H14 C22 3.4169 no . 4_555 H14 C24 3.5563 no . 3_657 H14 H12B 2.6862 no . 2_656 H14 H21 2.8273 no . 4_555 H14 H22 3.5275 no . 4_555 H14 H24 3.5552 no . 3_657 H15 Br1 3.0025 no . 4_555 H15 C1 3.4193 no . 4_555 H15 C20 2.9259 no . 4_555 H15 C21 3.3238 no . 4_555 H15 H12A 3.1299 no . 2_656 H15 H12B 3.3480 no . 2_656 H15 H20 2.6448 no . 4_555 H15 H21 3.3686 no . 4_555 H16 Br1 3.5060 no . 4_555 H16 C1 3.4796 no . 4_555 H16 C2 2.9083 no . 4_555 H16 C3 3.0051 no . 4_555 H16 H2 3.0115 no . 4_555 H16 H3 3.1195 no . 4_555 H16 H7 3.3805 no . 2_656 H17 C1 3.0512 no . 3_757 H17 C2 2.7518 no . 3_757 H17 C3 2.8289 no . 3_757 H17 C4 3.0519 no . 3_757 H17 C5 3.2961 no . 3_757 H17 C10 3.4107 no . 3_757 H17 C18 3.1897 no . 3_757 H17 H2 3.1110 no . 3_757 H17 H3 3.2926 no . 3_757 H17 H18 2.4924 no . 3_757 H18 C17 2.8377 no . 3_757 H18 C18 2.8995 no . 3_757 H18 H7 3.5378 no . 4_545 H18 H8 3.5239 no . 4_545 H18 H17 2.4924 no . 3_757 H18 H18 2.5999 no . 3_757 H20 Te1 3.3558 no . 3_657 H20 Br2 3.5717 no . 3_657 H20 C15 3.5114 no . 4_454 H20 H15 2.6448 no . 4_454 H20 H24 3.4185 no . 2_556 H21 Br2 3.5669 no . 3_657 H21 S1 3.0570 no . 2_556 H21 C14 3.5042 no . 4_454 H21 C19 3.4765 no . 2_556 H21 C24 3.1156 no . 2_556 H21 H8 2.7915 no . 2_556 H21 H14 2.8273 no . 4_454 H21 H15 3.3686 no . 4_454 H21 H24 2.4089 no . 2_556 H22 Br1 3.4739 no . 4_454 H22 C11 3.3937 no . 1_455 H22 C23 3.4264 no . 3_556 H22 H11A 3.4640 no . 1_455 H22 H11B 2.5565 no . 1_455 H22 H14 3.5275 no . 4_454 H22 H23 2.5833 no . 3_556 H23 Br1 2.9826 no . 2_546 H23 C11 3.5714 no . 3_656 H23 C22 3.1018 no . 3_556 H23 C23 3.1426 no . 3_556 H23 H11A 3.3134 no . 3_656 H23 H11B 3.0654 no . 1_455 H23 H11B 3.0166 no . 3_656 H23 H22 2.5833 no . 3_556 H23 H23 2.6426 no . 3_556 H24 Br2 3.2727 no . 4_444 H24 C11 3.5523 no . 3_656 H24 C21 3.2771 no . 2_546 H24 H11A 2.7804 no . 3_656 H24 H14 3.5552 no . 3_657 H24 H20 3.4185 no . 2_546 H24 H21 2.4089 no . 2_546 #============================================================================== data__Ferg75-2 _database_code_depnum_ccdc_archive 'CCDC 850824' #TrackingRef '- 9.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 Br2 Se Te' _chemical_formula_moiety 'C24 H18 Br2 Se Te' _chemical_formula_weight 672.77 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.680(4) _cell_length_b 12.776(3) _cell_length_c 14.386(4) _cell_angle_alpha 90.0000 _cell_angle_beta 113.068(6) _cell_angle_gamma 90.0000 _cell_volume 2144.2(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8312 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272.00 _exptl_absorpt_coefficient_mu 6.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.419 _exptl_absorpt_correction_T_max 0.664 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 17275 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4526 _reflns_number_gt 4024 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1624 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4324 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1007P)^2^+4.6380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.580 _refine_diff_density_min -1.790 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Se Se -0.093 2.226 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.531 1.675 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(2) Te 0.84159(3) 0.97065(3) 0.02939(3) 0.02386(17) Uani 1.00 4 d . . . Br(1) Br 0.75636(6) 1.16474(5) 0.01537(5) 0.0333(2) Uani 1.00 4 d . . . Br(2) Br 0.93553(6) 0.77874(5) 0.05896(5) 0.0306(2) Uani 1.00 4 d . . . Se(1) Se 1.04217(5) 1.12606(5) 0.17774(5) 0.0260(2) Uani 1.00 4 d . . . C(1) C 0.8257(6) 0.9586(5) 0.1723(5) 0.0256(13) Uani 1.00 4 d . . . C(2) C 0.7504(5) 0.8815(5) 0.1773(5) 0.0253(13) Uani 1.00 4 d . . . C(3) C 0.7196(6) 0.8714(5) 0.2611(5) 0.0307(15) Uani 1.00 4 d . . . C(4) C 0.7632(6) 0.9431(5) 0.3386(5) 0.0272(13) Uani 1.00 4 d . . . C(5) C 0.8434(5) 1.0185(5) 0.3353(5) 0.0241(12) Uani 1.00 4 d . . . C(6) C 0.8792(5) 1.0827(5) 0.4207(5) 0.0273(13) Uani 1.00 4 d . . . C(7) C 0.9598(6) 1.1600(5) 0.4312(5) 0.0273(13) Uani 1.00 4 d . . . C(8) C 1.0018(6) 1.1702(5) 0.3549(5) 0.0279(13) Uani 1.00 4 d . . . C(9) C 0.9653(5) 1.1066(5) 0.2695(5) 0.0242(12) Uani 1.00 4 d . . . C(10) C 0.8806(5) 1.0280(5) 0.2546(4) 0.0220(12) Uani 1.00 4 d . . . C(11) C 0.7422(7) 0.9584(6) 0.4339(6) 0.0351(16) Uani 1.00 4 d . . . C(12) C 0.8188(6) 1.0513(6) 0.4893(5) 0.0299(14) Uani 1.00 4 d . . . C(13) C 0.6744(5) 0.9050(5) -0.0628(5) 0.0255(13) Uani 1.00 4 d . . . C(14) C 0.5767(6) 0.9572(6) -0.0716(6) 0.0377(16) Uani 1.00 4 d . . . C(15) C 0.4695(6) 0.9132(7) -0.1340(6) 0.0422(18) Uani 1.00 4 d . . . C(16) C 0.4661(6) 0.8231(6) -0.1868(5) 0.0358(16) Uani 1.00 4 d . . . C(17) C 0.5662(7) 0.7728(6) -0.1766(5) 0.0366(16) Uani 1.00 4 d . . . C(18) C 0.6721(6) 0.8130(6) -0.1139(5) 0.0292(14) Uani 1.00 4 d . . . C(19) C 1.1823(5) 1.0483(5) 0.2510(5) 0.0258(13) Uani 1.00 4 d . . . C(20) C 1.2746(6) 1.0968(6) 0.3273(5) 0.0300(14) Uani 1.00 4 d . . . C(21) C 1.3774(7) 1.0417(6) 0.3753(6) 0.0351(16) Uani 1.00 4 d . . . C(22) C 1.3875(6) 0.9407(6) 0.3459(6) 0.0366(16) Uani 1.00 4 d . . . C(23) C 1.2959(6) 0.8943(6) 0.2687(6) 0.0349(16) Uani 1.00 4 d . . . C(24) C 1.1929(6) 0.9468(6) 0.2214(5) 0.0298(14) Uani 1.00 4 d . . . H(2) H 0.7187 0.8342 0.1224 0.030 Uiso 1.00 4 calc R . . H(3) H 0.6702 0.8168 0.2641 0.037 Uiso 1.00 4 calc R . . H(7) H 0.9859 1.2047 0.4886 0.033 Uiso 1.00 4 calc R . . H(8) H 1.0574 1.2227 0.3617 0.034 Uiso 1.00 4 calc R . . H(11A) H 0.7632 0.8946 0.4763 0.042 Uiso 1.00 4 calc R . . H(11B) H 0.6604 0.9745 0.4175 0.042 Uiso 1.00 4 calc R . . H(12A) H 0.7721 1.1098 0.4977 0.036 Uiso 1.00 4 calc R . . H(12B) H 0.8749 1.0298 0.5566 0.036 Uiso 1.00 4 calc R . . H(14) H 0.5806 1.0212 -0.0369 0.045 Uiso 1.00 4 calc R . . H(15) H 0.4002 0.9462 -0.1391 0.051 Uiso 1.00 4 calc R . . H(16) H 0.3944 0.7952 -0.2306 0.043 Uiso 1.00 4 calc R . . H(17) H 0.5627 0.7099 -0.2128 0.044 Uiso 1.00 4 calc R . . H(18) H 0.7411 0.7781 -0.1065 0.035 Uiso 1.00 4 calc R . . H(20) H 1.2677 1.1667 0.3467 0.036 Uiso 1.00 4 calc R . . H(21) H 1.4400 1.0739 0.4280 0.042 Uiso 1.00 4 calc R . . H(22) H 1.4570 0.9031 0.3784 0.044 Uiso 1.00 4 calc R . . H(23) H 1.3039 0.8252 0.2478 0.042 Uiso 1.00 4 calc R . . H(24) H 1.1304 0.9138 0.1693 0.036 Uiso 1.00 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te(2) 0.0251(3) 0.0225(3) 0.0219(3) -0.00030(15) 0.00699(19) -0.00002(15) Br(1) 0.0366(4) 0.0231(4) 0.0333(4) 0.0046(3) 0.0063(3) 0.0023(3) Br(2) 0.0330(4) 0.0254(4) 0.0301(4) 0.0049(3) 0.0088(3) -0.0011(3) Se(1) 0.0276(4) 0.0241(4) 0.0255(4) -0.0034(2) 0.0095(3) 0.0022(2) C(1) 0.033(3) 0.024(3) 0.023(3) 0.004(2) 0.015(3) 0.004(2) C(2) 0.024(3) 0.023(3) 0.025(3) -0.001(2) 0.005(3) 0.001(2) C(3) 0.033(3) 0.024(3) 0.038(4) -0.008(3) 0.016(3) -0.001(3) C(4) 0.030(3) 0.027(3) 0.028(3) 0.001(3) 0.015(3) 0.001(3) C(5) 0.022(3) 0.020(3) 0.028(3) 0.003(2) 0.007(3) 0.002(2) C(6) 0.026(3) 0.028(3) 0.026(3) 0.007(3) 0.008(2) 0.002(3) C(7) 0.028(3) 0.026(3) 0.025(3) 0.004(3) 0.007(3) -0.005(3) C(8) 0.026(3) 0.025(3) 0.028(3) -0.002(2) 0.005(3) -0.001(3) C(9) 0.022(3) 0.024(3) 0.024(3) 0.003(2) 0.007(2) 0.001(2) C(10) 0.022(3) 0.021(3) 0.018(3) 0.005(2) 0.003(2) 0.003(2) C(11) 0.040(4) 0.033(4) 0.038(4) -0.007(3) 0.021(3) -0.004(3) C(12) 0.026(3) 0.037(4) 0.027(3) 0.003(3) 0.011(3) -0.003(3) C(13) 0.022(3) 0.028(3) 0.023(3) -0.004(2) 0.005(2) 0.003(3) C(14) 0.035(4) 0.033(4) 0.039(4) 0.003(3) 0.009(3) -0.007(3) C(15) 0.023(3) 0.049(5) 0.045(4) -0.000(3) 0.004(3) -0.013(4) C(16) 0.025(3) 0.044(4) 0.031(4) -0.007(3) 0.003(3) -0.001(3) C(17) 0.042(4) 0.035(4) 0.028(3) -0.010(3) 0.009(3) -0.007(3) C(18) 0.028(3) 0.031(3) 0.025(3) -0.001(3) 0.006(3) -0.004(3) C(19) 0.028(3) 0.027(3) 0.025(3) -0.002(3) 0.012(3) 0.005(3) C(20) 0.032(3) 0.032(3) 0.024(3) -0.005(3) 0.009(3) 0.000(3) C(21) 0.038(4) 0.034(4) 0.033(4) -0.009(3) 0.013(3) 0.000(3) C(22) 0.029(3) 0.043(4) 0.035(4) 0.003(3) 0.009(3) 0.007(3) C(23) 0.034(4) 0.025(3) 0.042(4) 0.002(3) 0.011(3) -0.008(3) C(24) 0.026(3) 0.030(3) 0.034(3) -0.005(3) 0.013(3) -0.001(3) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Te(2) Br(1) 2.6808(9) yes . . Te(2) Br(2) 2.6859(9) yes . . Te(2) C(1) 2.148(7) yes . . Te(2) C(13) 2.180(6) yes . . Se(1) C(9) 1.940(8) yes . . Se(1) C(19) 1.946(6) yes . . C(1) C(2) 1.392(10) yes . . C(1) C(10) 1.423(8) yes . . C(2) C(3) 1.412(12) yes . . C(3) C(4) 1.380(9) yes . . C(4) C(5) 1.414(10) yes . . C(4) C(11) 1.508(12) yes . . C(5) C(6) 1.397(9) yes . . C(5) C(10) 1.420(11) yes . . C(6) C(7) 1.386(10) yes . . C(6) C(12) 1.521(11) yes . . C(7) C(8) 1.401(12) yes . . C(8) C(9) 1.393(9) yes . . C(9) C(10) 1.425(9) yes . . C(11) C(12) 1.544(10) yes . . C(13) C(14) 1.368(11) yes . . C(13) C(18) 1.381(10) yes . . C(14) C(15) 1.419(10) yes . . C(15) C(16) 1.371(12) yes . . C(16) C(17) 1.377(11) yes . . C(17) C(18) 1.390(9) yes . . C(19) C(20) 1.397(8) yes . . C(19) C(24) 1.387(10) yes . . C(20) C(21) 1.402(10) yes . . C(21) C(22) 1.379(11) yes . . C(22) C(23) 1.387(9) yes . . C(23) C(24) 1.387(9) yes . . C(2) H(2) 0.950 yes . . C(3) H(3) 0.950 yes . . C(7) H(7) 0.950 yes . . C(8) H(8) 0.950 yes . . C(11) H(11A) 0.990 yes . . C(11) H(11B) 0.990 yes . . C(12) H(12A) 0.990 yes . . C(12) H(12B) 0.990 yes . . C(14) H(14) 0.950 yes . . C(15) H(15) 0.950 yes . . C(16) H(16) 0.950 yes . . C(17) H(17) 0.950 yes . . C(18) H(18) 0.950 yes . . C(20) H(20) 0.950 yes . . C(21) H(21) 0.950 yes . . C(22) H(22) 0.950 yes . . C(23) H(23) 0.950 yes . . C(24) H(24) 0.950 yes . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Te(2) Br(2) 175.54(3) yes . . . Br(1) Te(2) C(1) 87.27(17) yes . . . Br(1) Te(2) C(13) 92.46(18) yes . . . Br(2) Te(2) C(1) 89.13(17) yes . . . Br(2) Te(2) C(13) 90.58(17) yes . . . C(1) Te(2) C(13) 96.9(3) yes . . . C(9) Se(1) C(19) 99.3(3) yes . . . Te(2) C(1) C(2) 115.0(4) yes . . . Te(2) C(1) C(10) 123.6(5) yes . . . C(2) C(1) C(10) 121.2(7) yes . . . C(1) C(2) C(3) 122.3(6) yes . . . C(2) C(3) C(4) 118.2(7) yes . . . C(3) C(4) C(5) 119.4(7) yes . . . C(3) C(4) C(11) 131.5(7) yes . . . C(5) C(4) C(11) 109.1(6) yes . . . C(4) C(5) C(6) 111.2(7) yes . . . C(4) C(5) C(10) 124.0(6) yes . . . C(6) C(5) C(10) 124.8(6) yes . . . C(5) C(6) C(7) 119.2(7) yes . . . C(5) C(6) C(12) 110.1(6) yes . . . C(7) C(6) C(12) 130.8(6) yes . . . C(6) C(7) C(8) 118.1(6) yes . . . C(7) C(8) C(9) 122.7(6) yes . . . Se(1) C(9) C(8) 116.4(5) yes . . . Se(1) C(9) C(10) 122.6(5) yes . . . C(8) C(9) C(10) 120.9(7) yes . . . C(1) C(10) C(5) 114.6(6) yes . . . C(1) C(10) C(9) 131.1(7) yes . . . C(5) C(10) C(9) 114.2(5) yes . . . C(4) C(11) C(12) 105.6(7) yes . . . C(6) C(12) C(11) 104.0(6) yes . . . Te(2) C(13) C(14) 119.9(5) yes . . . Te(2) C(13) C(18) 117.6(5) yes . . . C(14) C(13) C(18) 122.4(6) yes . . . C(13) C(14) C(15) 118.3(7) yes . . . C(14) C(15) C(16) 119.8(7) yes . . . C(15) C(16) C(17) 120.3(6) yes . . . C(16) C(17) C(18) 120.8(7) yes . . . C(13) C(18) C(17) 118.2(7) yes . . . Se(1) C(19) C(20) 120.3(5) yes . . . Se(1) C(19) C(24) 119.3(4) yes . . . C(20) C(19) C(24) 120.2(6) yes . . . C(19) C(20) C(21) 119.7(6) yes . . . C(20) C(21) C(22) 119.9(6) yes . . . C(21) C(22) C(23) 119.8(6) yes . . . C(22) C(23) C(24) 121.2(7) yes . . . C(19) C(24) C(23) 119.2(6) yes . . . C(1) C(2) H(2) 118.874 yes . . . C(3) C(2) H(2) 118.876 yes . . . C(2) C(3) H(3) 120.917 yes . . . C(4) C(3) H(3) 120.900 yes . . . C(6) C(7) H(7) 120.967 yes . . . C(8) C(7) H(7) 120.975 yes . . . C(7) C(8) H(8) 118.636 yes . . . C(9) C(8) H(8) 118.637 yes . . . C(4) C(11) H(11A) 110.620 yes . . . C(4) C(11) H(11B) 110.610 yes . . . C(12) C(11) H(11A) 110.615 yes . . . C(12) C(11) H(11B) 110.615 yes . . . H(11A) C(11) H(11B) 108.745 yes . . . C(6) C(12) H(12A) 110.946 yes . . . C(6) C(12) H(12B) 110.955 yes . . . C(11) C(12) H(12A) 110.947 yes . . . C(11) C(12) H(12B) 110.946 yes . . . H(12A) C(12) H(12B) 108.970 yes . . . C(13) C(14) H(14) 120.843 yes . . . C(15) C(14) H(14) 120.839 yes . . . C(14) C(15) H(15) 120.102 yes . . . C(16) C(15) H(15) 120.103 yes . . . C(15) C(16) H(16) 119.832 yes . . . C(17) C(16) H(16) 119.822 yes . . . C(16) C(17) H(17) 119.583 yes . . . C(18) C(17) H(17) 119.581 yes . . . C(13) C(18) H(18) 120.895 yes . . . C(17) C(18) H(18) 120.887 yes . . . C(19) C(20) H(20) 120.158 yes . . . C(21) C(20) H(20) 120.159 yes . . . C(20) C(21) H(21) 120.037 yes . . . C(22) C(21) H(21) 120.036 yes . . . C(21) C(22) H(22) 120.114 yes . . . C(23) C(22) H(22) 120.117 yes . . . C(22) C(23) H(23) 119.403 yes . . . C(24) C(23) H(23) 119.416 yes . . . C(19) C(24) H(24) 120.398 yes . . . C(23) C(24) H(24) 120.404 yes . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Te(2) C(1) C(2) 117.2(4) no . . . . Br(1) Te(2) C(1) C(10) -58.4(4) no . . . . Br(1) Te(2) C(13) C(14) -22.0(5) no . . . . Br(1) Te(2) C(13) C(18) 155.2(4) no . . . . Br(2) Te(2) C(1) C(2) -65.5(4) no . . . . Br(2) Te(2) C(1) C(10) 119.0(4) no . . . . Br(2) Te(2) C(13) C(14) 154.7(4) no . . . . Br(2) Te(2) C(13) C(18) -28.1(4) no . . . . C(1) Te(2) C(13) C(14) 65.5(5) no . . . . C(1) Te(2) C(13) C(18) -117.2(4) no . . . . C(13) Te(2) C(1) C(2) 25.0(4) no . . . . C(13) Te(2) C(1) C(10) -150.5(4) no . . . . C(9) Se(1) C(19) C(20) -85.2(5) no . . . . C(9) Se(1) C(19) C(24) 99.7(5) no . . . . C(19) Se(1) C(9) C(8) 79.0(4) no . . . . C(19) Se(1) C(9) C(10) -97.6(4) no . . . . Te(2) C(1) C(10) C(9) -9.6(9) no . . . . C(2) C(1) C(10) C(5) -6.0(8) no . . . . C(10) C(1) C(2) C(3) 3.4(9) no . . . . C(1) C(2) C(3) C(4) 2.2(9) no . . . . C(2) C(3) C(4) C(5) -4.8(9) no . . . . C(3) C(4) C(5) C(10) 2.0(9) no . . . . C(5) C(4) C(11) C(12) -0.3(7) no . . . . C(11) C(4) C(5) C(6) 0.6(7) no . . . . C(4) C(5) C(6) C(12) -0.7(7) no . . . . C(4) C(5) C(10) C(1) 3.4(8) no . . . . C(6) C(5) C(10) C(9) 3.6(8) no . . . . C(10) C(5) C(6) C(7) -2.2(9) no . . . . C(5) C(6) C(7) C(8) 0.1(8) no . . . . C(5) C(6) C(12) C(11) 0.5(6) no . . . . C(6) C(7) C(8) C(9) 0.4(9) no . . . . C(7) C(8) C(9) C(10) 1.2(9) no . . . . Se(1) C(9) C(10) C(1) -7.6(8) no . . . . C(8) C(9) C(10) C(5) -3.0(8) no . . . . C(4) C(11) C(12) C(6) -0.1(6) no . . . . C(14) C(13) C(18) C(17) 0.1(11) no . . . . C(18) C(13) C(14) C(15) 1.5(11) no . . . . C(13) C(14) C(15) C(16) -2.8(12) no . . . . C(14) C(15) C(16) C(17) 2.5(12) no . . . . C(15) C(16) C(17) C(18) -0.9(12) no . . . . C(16) C(17) C(18) C(13) -0.4(11) no . . . . C(20) C(19) C(24) C(23) 0.2(11) no . . . . C(24) C(19) C(20) C(21) -1.2(11) no . . . . C(19) C(20) C(21) C(22) 1.0(12) no . . . . C(20) C(21) C(22) C(23) 0.3(13) no . . . . C(21) C(22) C(23) C(24) -1.3(13) no . . . . C(22) C(23) C(24) C(19) 1.0(13) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Te(2) Se(1) 3.2729(8) yes . . Br(1) Se(1) 3.4930(12) yes . . Br(1) C(14) 3.399(7) yes . . Br(2) C(18) 3.320(6) yes . . Se(1) C(1) 3.456(7) yes . . C(1) C(4) 2.807(11) yes . . C(2) C(5) 2.742(9) yes . . C(2) C(13) 3.215(9) yes . . C(2) C(14) 3.525(9) yes . . C(3) C(10) 2.885(10) yes . . C(5) C(8) 2.726(9) yes . . C(6) C(9) 2.806(11) yes . . C(7) C(10) 2.883(9) yes . . C(8) C(19) 3.548(11) yes . . C(13) C(16) 2.749(8) yes . . C(14) C(17) 2.772(11) yes . . C(15) C(18) 2.783(11) yes . . C(19) C(22) 2.782(9) yes . . C(20) C(23) 2.767(10) yes . . C(21) C(24) 2.790(9) yes . . Br(2) C(17) 3.566(7) yes . 4_565 C(11) C(20) 3.594(12) yes . 3_776 C(17) Br(2) 3.566(7) yes . 4_464 C(18) C(20) 3.583(11) yes . 3_775 C(20) C(11) 3.594(12) yes . 3_776 C(20) C(18) 3.583(11) yes . 3_775 Te(2) H(2) 2.9817 yes . . Te(2) H(14) 3.1315 yes . . Te(2) H(18) 3.0892 yes . . Te(2) H(24) 3.4949 yes . . Br(1) H(14) 2.7535 yes . . Br(2) H(2) 3.2951 yes . . Br(2) H(18) 2.6727 yes . . Br(2) H(24) 2.9203 yes . . Se(1) H(8) 2.8582 yes . . Se(1) H(20) 2.9847 yes . . Se(1) H(24) 2.9544 yes . . C(1) H(3) 3.3097 yes . . C(1) H(14) 3.4682 yes . . C(2) H(14) 3.4807 yes . . C(3) H(11A) 2.9387 yes . . C(3) H(11B) 2.9467 yes . . C(4) H(2) 3.2487 yes . . C(4) H(12A) 3.0961 yes . . C(4) H(12B) 3.0972 yes . . C(5) H(3) 3.2778 yes . . C(5) H(7) 3.2663 yes . . C(5) H(11A) 3.0439 yes . . C(5) H(11B) 3.0399 yes . . C(5) H(12A) 3.0477 yes . . C(5) H(12B) 3.0534 yes . . C(6) H(8) 3.2439 yes . . C(6) H(11A) 3.0824 yes . . C(6) H(11B) 3.0834 yes . . C(7) H(12A) 2.9616 yes . . C(7) H(12B) 2.9501 yes . . C(8) H(20) 3.4207 yes . . C(9) H(7) 3.3060 yes . . C(10) H(2) 3.3012 yes . . C(10) H(8) 3.2993 yes . . C(11) H(3) 2.8859 yes . . C(12) H(7) 2.8885 yes . . C(13) H(2) 2.6560 yes . . C(13) H(15) 3.2518 yes . . C(13) H(17) 3.2378 yes . . C(14) H(2) 3.0923 yes . . C(14) H(16) 3.2735 yes . . C(14) H(18) 3.2635 yes . . C(15) H(17) 3.2378 yes . . C(16) H(14) 3.2727 yes . . C(16) H(18) 3.2663 yes . . C(17) H(15) 3.2417 yes . . C(18) H(2) 3.2255 yes . . C(18) H(14) 3.2649 yes . . C(18) H(16) 3.2615 yes . . C(19) H(8) 3.4630 yes . . C(19) H(21) 3.2787 yes . . C(19) H(23) 3.2493 yes . . C(20) H(8) 3.3894 yes . . C(20) H(22) 3.2677 yes . . C(20) H(24) 3.2743 yes . . C(21) H(23) 3.2468 yes . . C(22) H(20) 3.2646 yes . . C(22) H(24) 3.2730 yes . . C(23) H(21) 3.2521 yes . . C(24) H(20) 3.2713 yes . . C(24) H(22) 3.2710 yes . . H(2) H(3) 2.3588 yes . . H(2) H(14) 3.2990 yes . . H(2) H(18) 3.4882 yes . . H(3) H(11A) 2.9796 yes . . H(3) H(11B) 3.0269 yes . . H(7) H(8) 2.3451 yes . . H(7) H(12A) 3.0184 yes . . H(7) H(12B) 3.0021 yes . . H(8) H(20) 2.8503 yes . . H(11A) H(12A) 2.7642 yes . . H(11A) H(12B) 2.2461 yes . . H(11B) H(12A) 2.2461 yes . . H(11B) H(12B) 2.7634 yes . . H(14) H(15) 2.3825 yes . . H(15) H(16) 2.3202 yes . . H(16) H(17) 2.3189 yes . . H(17) H(18) 2.3469 yes . . H(20) H(21) 2.3550 yes . . H(21) H(22) 2.3312 yes . . H(22) H(23) 2.3304 yes . . H(23) H(24) 2.3344 yes . . Te(2) H(24) 3.3576 yes . 3_775 Br(1) H(3) 3.5206 yes . 2_655 Br(1) H(8) 2.9915 yes . 4_474 Br(1) H(11A) 2.9537 yes . 2_655 Br(1) H(15) 3.4481 yes . 3_675 Br(1) H(20) 3.2894 yes . 4_474 Br(1) H(23) 3.5591 yes . 3_775 Br(2) H(12A) 3.2515 yes . 2_645 Br(2) H(16) 3.4005 yes . 4_565 Br(2) H(17) 3.0419 yes . 4_565 Br(2) H(21) 3.0231 yes . 2_745 Br(2) H(22) 3.5736 yes . 4_464 Se(1) H(18) 3.5084 yes . 3_775 Se(1) H(23) 3.1293 yes . 2_755 C(1) H(15) 2.9749 yes . 3_675 C(1) H(16) 3.5022 yes . 4_565 C(1) H(17) 3.5351 yes . 4_565 C(2) H(15) 2.8243 yes . 3_675 C(2) H(16) 2.8793 yes . 4_565 C(3) H(15) 2.9549 yes . 3_675 C(3) H(16) 3.0414 yes . 4_565 C(4) H(15) 3.1423 yes . 3_675 C(5) H(12B) 3.3478 yes . 3_776 C(5) H(15) 3.2986 yes . 3_675 C(6) H(2) 3.4126 yes . 2_655 C(6) H(12B) 3.3311 yes . 3_776 C(7) H(2) 3.0504 yes . 2_655 C(7) H(3) 3.3159 yes . 2_655 C(7) H(11A) 3.3067 yes . 3_776 C(7) H(12B) 3.1648 yes . 3_776 C(8) H(3) 2.8754 yes . 2_655 C(8) H(11A) 3.1300 yes . 3_776 C(8) H(12B) 3.0058 yes . 3_776 C(9) H(3) 3.1225 yes . 2_655 C(9) H(12B) 3.0701 yes . 3_776 C(10) H(12B) 3.3070 yes . 3_776 C(10) H(15) 3.3033 yes . 3_675 C(11) H(20) 3.5845 yes . 3_776 C(11) H(22) 3.4571 yes . 1_455 C(12) H(17) 3.5934 yes . 2_655 C(12) H(18) 3.5801 yes . 2_655 C(14) H(14) 2.9885 yes . 3_675 C(14) H(15) 3.1791 yes . 3_675 C(15) H(7) 3.2959 yes . 2_645 C(15) H(14) 2.8929 yes . 3_675 C(16) H(7) 3.0706 yes . 2_645 C(17) H(7) 3.1473 yes . 2_645 C(17) H(12A) 3.3209 yes . 2_645 C(17) H(12B) 3.4874 yes . 2_645 C(17) H(24) 3.5605 yes . 4_464 C(18) H(7) 3.4653 yes . 2_645 C(18) H(12A) 3.0175 yes . 2_645 C(18) H(23) 3.5322 yes . 4_464 C(19) H(12B) 3.2796 yes . 3_776 C(19) H(18) 3.4300 yes . 3_775 C(19) H(23) 3.5420 yes . 2_755 C(20) H(11A) 3.0470 yes . 3_776 C(20) H(11B) 3.5518 yes . 3_776 C(20) H(12B) 3.3874 yes . 3_776 C(20) H(18) 3.4922 yes . 3_775 C(20) H(23) 3.1361 yes . 2_755 C(21) H(11A) 3.3739 yes . 3_776 C(21) H(11B) 3.5040 yes . 1_655 C(21) H(11B) 3.2068 yes . 3_776 C(21) H(21) 3.2278 yes . 3_876 C(21) H(22) 3.4102 yes . 3_876 C(22) H(11B) 3.2294 yes . 1_655 C(22) H(18) 3.5678 yes . 4_565 C(22) H(21) 3.1347 yes . 3_876 C(23) H(17) 3.3478 yes . 4_565 C(23) H(18) 3.0885 yes . 4_565 C(23) H(20) 3.2875 yes . 2_745 C(24) H(17) 2.9763 yes . 4_565 H(2) C(6) 3.4126 yes . 2_645 H(2) C(7) 3.0504 yes . 2_645 H(2) H(7) 2.9612 yes . 2_645 H(2) H(12A) 3.3717 yes . 2_645 H(2) H(15) 3.2395 yes . 3_675 H(2) H(16) 2.9110 yes . 4_565 H(3) Br(1) 3.5206 yes . 2_645 H(3) C(7) 3.3159 yes . 2_645 H(3) C(8) 2.8754 yes . 2_645 H(3) C(9) 3.1225 yes . 2_645 H(3) H(8) 2.9926 yes . 2_645 H(3) H(15) 3.4560 yes . 3_675 H(3) H(16) 3.1566 yes . 4_565 H(7) C(15) 3.2959 yes . 2_655 H(7) C(16) 3.0706 yes . 2_655 H(7) C(17) 3.1473 yes . 2_655 H(7) C(18) 3.4653 yes . 2_655 H(7) H(2) 2.9612 yes . 2_655 H(7) H(11A) 3.2761 yes . 3_776 H(7) H(16) 3.4095 yes . 2_655 H(7) H(17) 3.5139 yes . 2_655 H(8) Br(1) 2.9915 yes . 4_575 H(8) H(3) 2.9926 yes . 2_655 H(8) H(11A) 2.9498 yes . 3_776 H(8) H(12B) 3.4256 yes . 3_776 H(8) H(14) 3.5468 yes . 4_575 H(8) H(23) 3.0764 yes . 2_755 H(11A) Br(1) 2.9537 yes . 2_645 H(11A) C(7) 3.3067 yes . 3_776 H(11A) C(8) 3.1300 yes . 3_776 H(11A) C(20) 3.0470 yes . 3_776 H(11A) C(21) 3.3739 yes . 3_776 H(11A) H(7) 3.2761 yes . 3_776 H(11A) H(8) 2.9498 yes . 3_776 H(11A) H(20) 2.8349 yes . 3_776 H(11A) H(21) 3.3884 yes . 3_776 H(11A) H(22) 3.5753 yes . 1_455 H(11B) C(20) 3.5518 yes . 3_776 H(11B) C(21) 3.5040 yes . 1_455 H(11B) C(21) 3.2068 yes . 3_776 H(11B) C(22) 3.2294 yes . 1_455 H(11B) H(21) 3.1266 yes . 1_455 H(11B) H(21) 3.0284 yes . 3_776 H(11B) H(22) 2.5822 yes . 1_455 H(12A) Br(2) 3.2515 yes . 2_655 H(12A) C(17) 3.3209 yes . 2_655 H(12A) C(18) 3.0175 yes . 2_655 H(12A) H(2) 3.3717 yes . 2_655 H(12A) H(17) 3.2434 yes . 2_655 H(12A) H(18) 2.7029 yes . 2_655 H(12B) C(5) 3.3478 yes . 3_776 H(12B) C(6) 3.3311 yes . 3_776 H(12B) C(7) 3.1648 yes . 3_776 H(12B) C(8) 3.0058 yes . 3_776 H(12B) C(9) 3.0701 yes . 3_776 H(12B) C(10) 3.3070 yes . 3_776 H(12B) C(17) 3.4874 yes . 2_655 H(12B) C(19) 3.2796 yes . 3_776 H(12B) C(20) 3.3874 yes . 3_776 H(12B) H(8) 3.4256 yes . 3_776 H(12B) H(17) 3.0937 yes . 2_655 H(14) C(14) 2.9885 yes . 3_675 H(14) C(15) 2.8929 yes . 3_675 H(14) H(8) 3.5468 yes . 4_474 H(14) H(14) 2.7012 yes . 3_675 H(14) H(15) 2.4820 yes . 3_675 H(15) Br(1) 3.4481 yes . 3_675 H(15) C(1) 2.9749 yes . 3_675 H(15) C(2) 2.8243 yes . 3_675 H(15) C(3) 2.9549 yes . 3_675 H(15) C(4) 3.1423 yes . 3_675 H(15) C(5) 3.2986 yes . 3_675 H(15) C(10) 3.3033 yes . 3_675 H(15) C(14) 3.1791 yes . 3_675 H(15) H(2) 3.2395 yes . 3_675 H(15) H(3) 3.4560 yes . 3_675 H(15) H(14) 2.4820 yes . 3_675 H(16) Br(2) 3.4005 yes . 4_464 H(16) C(1) 3.5022 yes . 4_464 H(16) C(2) 2.8793 yes . 4_464 H(16) C(3) 3.0414 yes . 4_464 H(16) H(2) 2.9110 yes . 4_464 H(16) H(3) 3.1566 yes . 4_464 H(16) H(7) 3.4095 yes . 2_645 H(17) Br(2) 3.0419 yes . 4_464 H(17) C(1) 3.5351 yes . 4_464 H(17) C(12) 3.5934 yes . 2_645 H(17) C(23) 3.3478 yes . 4_464 H(17) C(24) 2.9763 yes . 4_464 H(17) H(7) 3.5139 yes . 2_645 H(17) H(12A) 3.2434 yes . 2_645 H(17) H(12B) 3.0937 yes . 2_645 H(17) H(23) 3.3524 yes . 4_464 H(17) H(24) 2.6924 yes . 4_464 H(18) Se(1) 3.5084 yes . 3_775 H(18) C(12) 3.5801 yes . 2_645 H(18) C(19) 3.4300 yes . 3_775 H(18) C(20) 3.4922 yes . 3_775 H(18) C(22) 3.5678 yes . 4_464 H(18) C(23) 3.0885 yes . 4_464 H(18) H(12A) 2.7029 yes . 2_645 H(18) H(20) 3.4855 yes . 3_775 H(18) H(23) 2.8426 yes . 4_464 H(20) Br(1) 3.2894 yes . 4_575 H(20) C(11) 3.5845 yes . 3_776 H(20) C(23) 3.2875 yes . 2_755 H(20) H(11A) 2.8349 yes . 3_776 H(20) H(18) 3.4855 yes . 3_775 H(20) H(23) 2.4096 yes . 2_755 H(20) H(24) 3.4522 yes . 2_755 H(21) Br(2) 3.0231 yes . 2_755 H(21) C(21) 3.2278 yes . 3_876 H(21) C(22) 3.1347 yes . 3_876 H(21) H(11A) 3.3884 yes . 3_776 H(21) H(11B) 3.1266 yes . 1_655 H(21) H(11B) 3.0284 yes . 3_776 H(21) H(21) 2.7762 yes . 3_876 H(21) H(22) 2.5883 yes . 3_876 H(22) Br(2) 3.5736 yes . 4_565 H(22) C(11) 3.4571 yes . 1_655 H(22) C(21) 3.4102 yes . 3_876 H(22) H(11A) 3.5753 yes . 1_655 H(22) H(11B) 2.5822 yes . 1_655 H(22) H(21) 2.5883 yes . 3_876 H(23) Br(1) 3.5591 yes . 3_775 H(23) Se(1) 3.1293 yes . 2_745 H(23) C(18) 3.5322 yes . 4_565 H(23) C(19) 3.5420 yes . 2_745 H(23) C(20) 3.1361 yes . 2_745 H(23) H(8) 3.0764 yes . 2_745 H(23) H(17) 3.3524 yes . 4_565 H(23) H(18) 2.8426 yes . 4_565 H(23) H(20) 2.4096 yes . 2_745 H(24) Te(2) 3.3576 yes . 3_775 H(24) C(17) 3.5605 yes . 4_565 H(24) H(17) 2.6924 yes . 4_565 H(24) H(20) 3.4522 yes . 2_745 #============================================================================== data_Ferg-108 _database_code_depnum_ccdc_archive 'CCDC 850825' #TrackingRef '- 10.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H18 I2 S Te' _chemical_formula_moiety 'C24 H18 I2 S Te' _chemical_formula_weight 719.88 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.129(6) _cell_length_b 16.603(9) _cell_length_c 12.582(7) _cell_angle_alpha 90.0000 _cell_angle_beta 102.416(10) _cell_angle_gamma 90.0000 _cell_volume 2270(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8991 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 26.37 _cell_measurement_temperature 125 #------------------------------------------------------------------------------ _exptl_crystal_description chunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344.00 _exptl_absorpt_coefficient_mu 4.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.208 _exptl_absorpt_correction_T_max 0.921 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 125 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 29.257 _diffrn_reflns_number 18531 _diffrn_reflns_av_R_equivalents 0.1020 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4609 _reflns_number_gt 4006 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2488 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4609 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1125P)^2^+9.5559P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.940 _refine_diff_density_min -2.590 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; I I -0.4742 1.8119 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.5308 1.6751 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.59588(8) 0.15040(5) 0.30364(7) 0.0313(3) Uani 1.0 4 d . . . I2 I 0.62308(8) 0.06121(5) -0.14034(7) 0.0306(3) Uani 1.0 4 d . . . Te1 Te 0.60397(7) 0.10626(5) 0.08344(6) 0.0249(3) Uani 1.0 4 d . . . S1 S 0.4058(3) 0.21332(19) -0.0685(3) 0.0284(7) Uani 1.0 4 d . . . C1 C 0.7004(11) 0.2139(7) 0.0691(10) 0.024(3) Uani 1.0 4 d . . . C2 C 0.8185(11) 0.2228(7) 0.1247(11) 0.026(3) Uani 1.0 4 d . . . C3 C 0.8930(12) 0.2885(8) 0.1200(11) 0.029(3) Uani 1.0 4 d . . . C4 C 0.8439(12) 0.3509(7) 0.0564(10) 0.024(3) Uani 1.0 4 d . . . C5 C 0.7190(12) 0.3483(8) 0.0014(11) 0.029(3) Uani 1.0 4 d . . . C6 C 0.6803(13) 0.4213(9) -0.0548(10) 0.033(3) Uani 1.0 4 d . . . C7 C 0.5618(14) 0.4302(8) -0.1066(12) 0.036(4) Uani 1.0 4 d . . . C8 C 0.4806(13) 0.3644(8) -0.1071(11) 0.032(3) Uani 1.0 4 d . . . C9 C 0.5176(12) 0.2931(8) -0.0536(11) 0.030(3) Uani 1.0 4 d . . . C10 C 0.6434(11) 0.2830(7) 0.0053(10) 0.024(3) Uani 1.0 4 d . . . C11 C 0.8972(13) 0.4317(8) 0.0287(13) 0.038(4) Uani 1.0 4 d . . . C12 C 0.7907(13) 0.4784(9) -0.0417(12) 0.039(4) Uani 1.0 4 d . . . C13 C 0.7587(12) 0.0281(8) 0.1399(11) 0.028(3) Uani 1.0 4 d . . . C14 C 0.7419(12) -0.0341(8) 0.2084(10) 0.029(3) Uani 1.0 4 d . . . C15 C 0.8256(12) -0.0959(9) 0.2314(12) 0.036(4) Uani 1.0 4 d . . . C16 C 0.9302(13) -0.0953(9) 0.1895(11) 0.036(3) Uani 1.0 4 d . . . C17 C 0.9539(12) -0.0303(9) 0.1241(12) 0.037(4) Uani 1.0 4 d . . . C18 C 0.8685(11) 0.0301(9) 0.0996(11) 0.033(3) Uani 1.0 4 d . . . C19 C 0.3345(10) 0.2289(8) 0.0441(10) 0.024(3) Uani 1.0 4 d . . . C20 C 0.2736(12) 0.1607(9) 0.0731(12) 0.034(3) Uani 1.0 4 d . . . C21 C 0.2164(12) 0.1643(9) 0.1591(12) 0.035(4) Uani 1.0 4 d . . . C22 C 0.2200(12) 0.2355(10) 0.2171(12) 0.039(4) Uani 1.0 4 d . . . C23 C 0.2808(13) 0.3006(11) 0.1887(12) 0.047(4) Uani 1.0 4 d . . . C24 C 0.3388(12) 0.3003(10) 0.1021(14) 0.043(4) Uani 1.0 4 d . . . H2 H 0.8531 0.1797 0.1710 0.0310 Uiso 1.0 4 calc R . . H3 H 0.9758 0.2898 0.1601 0.0352 Uiso 1.0 4 calc R . . H7 H 0.5334 0.4793 -0.1418 0.0434 Uiso 1.0 4 calc R . . H8 H 0.3977 0.3696 -0.1457 0.0388 Uiso 1.0 4 calc R . . H11A H 0.9318 0.4621 0.0961 0.0458 Uiso 1.0 4 calc R . . H11B H 0.9633 0.4227 -0.0115 0.0458 Uiso 1.0 4 calc R . . H12A H 0.8089 0.4916 -0.1133 0.0466 Uiso 1.0 4 calc R . . H12B H 0.7748 0.5290 -0.0054 0.0466 Uiso 1.0 4 calc R . . H14 H 0.6716 -0.0341 0.2400 0.0344 Uiso 1.0 4 calc R . . H15 H 0.8113 -0.1391 0.2765 0.0433 Uiso 1.0 4 calc R . . H16 H 0.9868 -0.1388 0.2045 0.0431 Uiso 1.0 4 calc R . . H17 H 1.0277 -0.0285 0.0978 0.0445 Uiso 1.0 4 calc R . . H18 H 0.8829 0.0738 0.0551 0.0397 Uiso 1.0 4 calc R . . H20 H 0.2722 0.1121 0.0329 0.0406 Uiso 1.0 4 calc R . . H21 H 0.1747 0.1185 0.1787 0.0424 Uiso 1.0 4 calc R . . H22 H 0.1801 0.2390 0.2766 0.0474 Uiso 1.0 4 calc R . . H23 H 0.2834 0.3485 0.2304 0.0562 Uiso 1.0 4 calc R . . H24 H 0.3797 0.3467 0.0832 0.0517 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0365(5) 0.0325(5) 0.0269(5) 0.0003(4) 0.0114(4) -0.0004(4) I2 0.0369(5) 0.0300(5) 0.0267(5) -0.0011(4) 0.0110(4) -0.0005(4) Te1 0.0282(5) 0.0230(5) 0.0249(5) -0.0018(4) 0.0087(4) 0.0012(3) S1 0.0278(15) 0.0279(16) 0.0292(17) -0.0014(13) 0.0060(12) -0.0032(13) C1 0.035(6) 0.017(6) 0.020(6) 0.002(5) 0.007(5) -0.007(5) C2 0.025(6) 0.019(6) 0.034(7) -0.001(5) 0.008(5) 0.004(5) C3 0.028(6) 0.026(7) 0.033(8) 0.004(6) 0.005(5) 0.003(6) C4 0.038(7) 0.021(6) 0.018(6) -0.012(6) 0.020(5) -0.006(5) C5 0.038(7) 0.024(7) 0.027(7) 0.002(6) 0.009(6) 0.006(5) C6 0.043(8) 0.047(8) 0.011(6) -0.015(7) 0.014(5) 0.007(6) C7 0.053(9) 0.025(7) 0.029(8) 0.003(7) 0.005(6) 0.013(6) C8 0.036(7) 0.032(7) 0.026(7) 0.006(6) -0.002(6) 0.006(6) C9 0.031(7) 0.036(7) 0.024(7) 0.004(6) 0.011(5) 0.003(6) C10 0.029(6) 0.024(6) 0.018(6) -0.004(5) 0.004(5) -0.000(5) C11 0.040(8) 0.026(7) 0.048(9) -0.010(6) 0.008(7) -0.003(7) C12 0.047(8) 0.037(8) 0.029(8) -0.008(7) -0.001(6) 0.007(6) C13 0.038(7) 0.021(6) 0.027(7) 0.007(6) 0.009(6) 0.001(5) C14 0.034(7) 0.028(7) 0.025(7) -0.002(6) 0.010(5) -0.002(6) C15 0.033(7) 0.046(8) 0.034(8) -0.008(7) 0.016(6) 0.005(7) C16 0.036(7) 0.039(8) 0.030(8) 0.001(7) -0.000(6) -0.001(6) C17 0.030(7) 0.042(8) 0.043(9) 0.006(7) 0.015(6) -0.008(7) C18 0.029(7) 0.041(8) 0.030(7) -0.008(6) 0.008(5) 0.007(6) C19 0.025(6) 0.030(6) 0.018(6) 0.006(6) 0.007(5) 0.006(5) C20 0.039(7) 0.031(7) 0.032(8) -0.004(6) 0.009(6) 0.005(6) C21 0.031(7) 0.042(8) 0.033(8) -0.004(6) 0.008(6) 0.016(7) C22 0.030(7) 0.053(9) 0.034(8) 0.005(7) 0.003(6) 0.006(7) C23 0.039(8) 0.072(11) 0.028(8) 0.017(8) 0.004(6) -0.012(8) C24 0.025(7) 0.045(9) 0.057(10) 0.004(7) 0.004(7) -0.017(8) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I1 Te1 2.8860(19) yes . . I2 Te1 2.9648(19) yes . . Te1 C1 2.112(12) yes . . Te1 C13 2.151(12) yes . . S1 C9 1.800(14) yes . . S1 C19 1.785(14) yes . . C1 C2 1.358(16) yes . . C1 C10 1.465(16) yes . . C2 C3 1.379(18) yes . . C3 C4 1.351(17) yes . . C4 C5 1.414(17) yes . . C4 C11 1.536(19) yes . . C5 C6 1.422(19) yes . . C5 C10 1.380(18) yes . . C6 C7 1.347(19) yes . . C6 C12 1.53(2) yes . . C7 C8 1.42(2) yes . . C8 C9 1.380(19) yes . . C9 C10 1.446(16) yes . . C11 C12 1.529(19) yes . . C13 C14 1.384(19) yes . . C13 C18 1.42(2) yes . . C14 C15 1.373(19) yes . . C15 C16 1.38(2) yes . . C16 C17 1.42(2) yes . . C17 C18 1.371(19) yes . . C19 C20 1.408(19) yes . . C19 C24 1.39(2) yes . . C20 C21 1.37(3) yes . . C21 C22 1.39(3) yes . . C22 C23 1.36(3) yes . . C23 C24 1.38(3) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 I1 Te1 I2 177.73(4) yes . . . I1 Te1 C1 89.3(4) yes . . . I1 Te1 C13 91.4(4) yes . . . I2 Te1 C1 89.5(4) yes . . . I2 Te1 C13 86.9(4) yes . . . C1 Te1 C13 98.8(5) yes . . . C9 S1 C19 103.1(6) yes . . . Te1 C1 C2 120.1(9) yes . . . Te1 C1 C10 122.8(8) yes . . . C2 C1 C10 117.0(11) yes . . . C1 C2 C3 126.0(11) yes . . . C2 C3 C4 117.5(11) yes . . . C3 C4 C5 119.8(12) yes . . . C3 C4 C11 132.6(11) yes . . . C5 C4 C11 107.6(10) yes . . . C4 C5 C6 112.3(11) yes . . . C4 C5 C10 123.3(11) yes . . . C6 C5 C10 124.4(12) yes . . . C5 C6 C7 119.6(13) yes . . . C5 C6 C12 108.8(11) yes . . . C7 C6 C12 131.5(13) yes . . . C6 C7 C8 118.4(13) yes . . . C7 C8 C9 122.4(12) yes . . . S1 C9 C8 117.0(9) yes . . . S1 C9 C10 122.7(10) yes . . . C8 C9 C10 120.2(12) yes . . . C1 C10 C5 116.1(10) yes . . . C1 C10 C9 129.0(11) yes . . . C5 C10 C9 114.9(11) yes . . . C4 C11 C12 106.6(11) yes . . . C6 C12 C11 104.6(12) yes . . . Te1 C13 C14 116.8(10) yes . . . Te1 C13 C18 123.8(10) yes . . . C14 C13 C18 118.8(12) yes . . . C13 C14 C15 120.8(14) yes . . . C14 C15 C16 120.3(14) yes . . . C15 C16 C17 120.4(13) yes . . . C16 C17 C18 118.8(14) yes . . . C13 C18 C17 120.7(13) yes . . . S1 C19 C20 114.1(10) yes . . . S1 C19 C24 124.8(11) yes . . . C20 C19 C24 121.0(13) yes . . . C19 C20 C21 120.0(13) yes . . . C20 C21 C22 119.2(14) yes . . . C21 C22 C23 119.9(15) yes . . . C22 C23 C24 123.2(16) yes . . . C19 C24 C23 116.7(15) yes . . . C1 C2 H2 116.975 no . . . C3 C2 H2 116.975 no . . . C2 C3 H3 121.261 no . . . C4 C3 H3 121.250 no . . . C6 C7 H7 120.815 no . . . C8 C7 H7 120.816 no . . . C7 C8 H8 118.808 no . . . C9 C8 H8 118.792 no . . . C4 C11 H11A 110.410 no . . . C4 C11 H11B 110.414 no . . . C12 C11 H11A 110.409 no . . . C12 C11 H11B 110.408 no . . . H11A C11 H11B 108.619 no . . . C6 C12 H12A 110.823 no . . . C6 C12 H12B 110.823 no . . . C11 C12 H12A 110.831 no . . . C11 C12 H12B 110.835 no . . . H12A C12 H12B 108.894 no . . . C13 C14 H14 119.577 no . . . C15 C14 H14 119.587 no . . . C14 C15 H15 119.829 no . . . C16 C15 H15 119.834 no . . . C15 C16 H16 119.822 no . . . C17 C16 H16 119.816 no . . . C16 C17 H17 120.586 no . . . C18 C17 H17 120.587 no . . . C13 C18 H18 119.658 no . . . C17 C18 H18 119.649 no . . . C19 C20 H20 119.975 no . . . C21 C20 H20 119.984 no . . . C20 C21 H21 120.403 no . . . C22 C21 H21 120.398 no . . . C21 C22 H22 120.074 no . . . C23 C22 H22 120.067 no . . . C22 C23 H23 118.426 no . . . C24 C23 H23 118.413 no . . . C19 C24 H24 121.662 no . . . C23 C24 H24 121.649 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 I1 Te1 C1 C2 70.5(9) no . . . . I1 Te1 C1 C10 -106.2(9) no . . . . I1 Te1 C13 C14 59.3(8) no . . . . I1 Te1 C13 C18 -129.7(8) no . . . . I2 Te1 C1 C2 -107.6(9) no . . . . I2 Te1 C1 C10 75.7(9) no . . . . I2 Te1 C13 C14 -122.2(8) no . . . . I2 Te1 C13 C18 48.9(8) no . . . . C1 Te1 C13 C14 148.8(8) no . . . . C1 Te1 C13 C18 -40.1(9) no . . . . C13 Te1 C1 C2 -20.8(10) no . . . . C13 Te1 C1 C10 162.5(9) no . . . . C9 S1 C19 C20 -159.7(7) no . . . . C9 S1 C19 C24 18.8(10) no . . . . C19 S1 C9 C8 -91.5(10) no . . . . C19 S1 C9 C10 92.4(11) no . . . . Te1 C1 C2 C3 177.8(9) no . . . . Te1 C1 C10 C5 -178.4(7) no . . . . Te1 C1 C10 C9 2.5(18) no . . . . C2 C1 C10 C5 4.8(17) no . . . . C2 C1 C10 C9 -174.3(12) no . . . . C10 C1 C2 C3 -5(2) no . . . . C1 C2 C3 C4 2(2) no . . . . C2 C3 C4 C5 2.6(19) no . . . . C2 C3 C4 C11 -178.4(12) no . . . . C3 C4 C5 C6 175.4(11) no . . . . C3 C4 C5 C10 -3(2) no . . . . C3 C4 C11 C12 -175.8(14) no . . . . C5 C4 C11 C12 3.3(15) no . . . . C11 C4 C5 C6 -3.9(15) no . . . . C11 C4 C5 C10 178.0(12) no . . . . C4 C5 C6 C7 -176.4(11) no . . . . C4 C5 C6 C12 2.9(15) no . . . . C4 C5 C10 C1 -1.1(19) no . . . . C4 C5 C10 C9 178.1(11) no . . . . C6 C5 C10 C1 -179.0(12) no . . . . C6 C5 C10 C9 0.3(19) no . . . . C10 C5 C6 C7 2(2) no . . . . C10 C5 C6 C12 -179.1(12) no . . . . C5 C6 C7 C8 -3(2) no . . . . C5 C6 C12 C11 -0.6(15) no . . . . C7 C6 C12 C11 178.6(14) no . . . . C12 C6 C7 C8 178.1(13) no . . . . C6 C7 C8 C9 2(2) no . . . . C7 C8 C9 S1 -176.6(12) no . . . . C7 C8 C9 C10 -0(2) no . . . . S1 C9 C10 C1 -5.7(19) no . . . . S1 C9 C10 C5 175.1(8) no . . . . C8 C9 C10 C1 178.3(12) no . . . . C8 C9 C10 C5 -0.9(18) no . . . . C4 C11 C12 C6 -1.6(15) no . . . . Te1 C13 C14 C15 167.1(7) no . . . . Te1 C13 C18 C17 -168.0(8) no . . . . C14 C13 C18 C17 2.8(18) no . . . . C18 C13 C14 C15 -4.4(17) no . . . . C13 C14 C15 C16 2.3(19) no . . . . C14 C15 C16 C17 1.3(19) no . . . . C15 C16 C17 C18 -2.8(19) no . . . . C16 C17 C18 C13 0.7(19) no . . . . S1 C19 C20 C21 179.2(8) no . . . . S1 C19 C24 C23 -178.4(7) no . . . . C20 C19 C24 C23 0.0(17) no . . . . C24 C19 C20 C21 0.6(17) no . . . . C19 C20 C21 C22 -0.4(18) no . . . . C20 C21 C22 C23 -0.5(18) no . . . . C21 C22 C23 C24 1(2) no . . . . C22 C23 C24 C19 -1(2) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Te1 S1 3.141(4) no . . Te1 C9 3.579(13) no . . Te1 C19 3.570(12) no . . S1 C1 3.363(12) no . . C1 C4 2.804(17) no . . C1 C18 3.557(18) no . . C2 C5 2.691(17) no . . C2 C13 3.314(17) no . . C2 C18 3.273(19) no . . C3 C10 2.843(16) no . . C5 C8 2.723(18) no . . C6 C9 2.80(2) no . . C7 C10 2.867(18) no . . C8 C19 3.557(19) no . . C8 C24 3.51(3) no . . C9 C24 3.08(3) no . . C13 C16 2.779(19) no . . C14 C17 2.79(2) no . . C15 C18 2.77(2) no . . C19 C22 2.75(2) no . . C20 C23 2.73(3) no . . C21 C24 2.81(3) no . . S1 C15 3.517(14) no . 3_655 C11 C11 3.41(2) no . 3_765 C15 S1 3.517(14) no . 3_655 I1 H14 3.3209 no . . I2 H18 3.3751 no . . Te1 H2 3.0123 no . . Te1 H14 3.0397 no . . Te1 H18 3.2443 no . . S1 H8 2.7644 no . . S1 H20 2.7346 no . . S1 H24 2.9777 no . . C1 H3 3.2837 no . . C1 H18 3.1178 no . . C2 H18 2.7688 no . . C3 H11A 2.9388 no . . C3 H11B 2.9781 no . . C4 H2 3.1793 no . . C4 H12A 3.1323 no . . C4 H12B 3.1107 no . . C5 H3 3.2619 no . . C5 H7 3.2621 no . . C5 H11A 3.0623 no . . C5 H11B 3.0208 no . . C5 H12A 3.0601 no . . C5 H12B 3.0674 no . . C6 H8 3.2235 no . . C6 H11A 3.1004 no . . C6 H11B 3.0785 no . . C7 H12A 2.9517 no . . C7 H12B 2.9383 no . . C8 H24 2.8700 no . . C9 H7 3.3025 no . . C9 H24 2.6922 no . . C10 H2 3.2626 no . . C10 H8 3.3039 no . . C10 H24 3.4536 no . . C11 H3 2.9023 no . . C12 H7 2.8698 no . . C13 H2 2.7233 no . . C13 H15 3.2520 no . . C13 H17 3.2881 no . . C14 H16 3.2416 no . . C14 H18 3.2697 no . . C15 H17 3.2807 no . . C16 H14 3.2406 no . . C16 H18 3.2615 no . . C17 H15 3.2819 no . . C18 H2 2.6593 no . . C18 H14 3.2741 no . . C18 H16 3.2555 no . . C19 H8 3.5168 no . . C19 H21 3.2687 no . . C19 H23 3.2144 no . . C20 H22 3.2362 no . . C20 H24 3.2984 no . . C21 H23 3.2292 no . . C22 H20 3.2381 no . . C22 H24 3.2696 no . . C23 H21 3.2380 no . . C24 H8 3.5137 no . . C24 H20 3.2851 no . . C24 H22 3.2621 no . . H2 H3 2.3035 no . . H2 H18 2.3530 no . . H3 H11A 2.9823 no . . H3 H11B 3.0684 no . . H7 H8 2.3611 no . . H7 H12A 3.0162 no . . H7 H12B 2.9767 no . . H8 H24 2.9534 no . . H11A H12A 2.7394 no . . H11A H12B 2.2265 no . . H11B H12A 2.2262 no . . H11B H12B 2.7546 no . . H14 H15 2.3150 no . . H15 H16 2.3229 no . . H16 H17 2.3723 no . . H17 H18 2.3240 no . . H20 H21 2.3252 no . . H21 H22 2.3428 no . . H22 H23 2.2914 no . . H23 H24 2.3313 no . . I1 H8 3.2976 no . 4_555 I1 H11A 3.4109 no . 2_645 I1 H11B 3.2459 no . 4_455 I1 H12B 3.3178 no . 2_645 I2 H11A 3.5558 no . 4_454 I2 H12A 3.5386 no . 2_644 I2 H14 3.2808 no . 3_655 I2 H20 3.2846 no . 3_655 I2 H22 3.5758 no . 4_554 I2 H23 3.0532 no . 4_554 S1 H15 3.3884 no . 3_655 C1 H15 3.1387 no . 2_655 C2 H8 3.2224 no . 4_555 C2 H15 3.1085 no . 2_655 C3 H14 3.5838 no . 2_655 C3 H15 3.0954 no . 2_655 C3 H22 3.4723 no . 1_655 C4 H14 3.2299 no . 2_655 C4 H15 2.9989 no . 2_655 C5 H15 2.8940 no . 2_655 C5 H22 3.1246 no . 4_554 C6 H21 3.4052 no . 4_554 C6 H22 3.4031 no . 4_554 C7 H21 3.3157 no . 4_554 C7 H22 3.5519 no . 4_554 C8 H2 2.9398 no . 4_454 C8 H22 3.3789 no . 4_554 C9 H2 3.5822 no . 4_454 C9 H22 3.1274 no . 4_554 C10 H15 2.9779 no . 2_655 C10 H22 3.0146 no . 4_554 C11 H11A 3.2378 no . 3_765 C11 H11B 2.9066 no . 3_765 C11 H12A 3.4573 no . 3_765 C11 H14 3.2153 no . 2_655 C12 H11A 3.4477 no . 3_765 C12 H11B 3.1387 no . 3_765 C12 H24 3.4468 no . 3_665 C13 H8 3.2811 no . 4_555 C13 H20 3.1536 no . 3_655 C14 H7 3.5033 no . 4_555 C14 H8 3.5314 no . 4_555 C14 H11A 3.4407 no . 2_645 C14 H20 3.2740 no . 3_655 C15 H7 3.1701 no . 4_555 C15 H20 3.2811 no . 3_655 C16 H7 2.9126 no . 4_555 C16 H20 3.2054 no . 3_655 C16 H23 3.2653 no . 2_645 C16 H24 3.3136 no . 2_645 C17 H7 3.0082 no . 4_555 C17 H17 3.0064 no . 3_755 C17 H18 3.2666 no . 3_755 C17 H20 3.1535 no . 3_655 C17 H21 3.4480 no . 1_655 C18 H7 3.3783 no . 4_555 C18 H8 3.5649 no . 4_555 C18 H17 2.9556 no . 3_755 C18 H20 3.1120 no . 3_655 C21 H3 3.3953 no . 1_455 C22 H3 2.8062 no . 1_455 C23 H3 3.3406 no . 1_455 C23 H16 2.8306 no . 2_655 C24 H12B 3.2335 no . 3_665 C24 H16 2.9456 no . 2_655 H2 C8 2.9398 no . 4_555 H2 C9 3.5822 no . 4_555 H2 H8 2.3969 no . 4_555 H3 C21 3.3953 no . 1_655 H3 C22 2.8062 no . 1_655 H3 C23 3.3406 no . 1_655 H3 H21 3.5809 no . 1_655 H3 H22 2.5691 no . 1_655 H3 H23 3.4856 no . 1_655 H7 C14 3.5033 no . 4_454 H7 C15 3.1701 no . 4_454 H7 C16 2.9126 no . 4_454 H7 C17 3.0082 no . 4_454 H7 C18 3.3783 no . 4_454 H7 H16 3.2540 no . 4_454 H7 H17 3.3639 no . 4_454 H7 H21 3.4262 no . 4_554 H7 H24 3.0855 no . 3_665 H8 I1 3.2976 no . 4_454 H8 C2 3.2224 no . 4_454 H8 C13 3.2811 no . 4_454 H8 C14 3.5314 no . 4_454 H8 C18 3.5649 no . 4_454 H8 H2 2.3969 no . 4_454 H8 H12B 3.4209 no . 3_665 H11A I1 3.4109 no . 2_655 H11A I2 3.5558 no . 4_555 H11A C11 3.2378 no . 3_765 H11A C12 3.4477 no . 3_765 H11A C14 3.4407 no . 2_655 H11A H11A 3.3635 no . 3_765 H11A H11B 2.5869 no . 3_765 H11A H12A 2.9484 no . 3_765 H11A H14 2.5706 no . 2_655 H11B I1 3.2459 no . 4_554 H11B C11 2.9066 no . 3_765 H11B C12 3.1387 no . 3_765 H11B H11A 2.5869 no . 3_765 H11B H11B 2.6912 no . 3_765 H11B H12A 3.0340 no . 3_765 H11B H12B 2.9863 no . 3_765 H12A I2 3.5386 no . 2_654 H12A C11 3.4573 no . 3_765 H12A H11A 2.9484 no . 3_765 H12A H11B 3.0340 no . 3_765 H12A H21 3.2779 no . 4_554 H12A H23 3.1016 no . 3_665 H12A H24 3.4785 no . 3_665 H12B I1 3.3178 no . 2_655 H12B C24 3.2335 no . 3_665 H12B H8 3.4209 no . 3_665 H12B H11B 2.9863 no . 3_765 H12B H14 3.4277 no . 2_655 H12B H23 3.4332 no . 3_665 H12B H24 2.7305 no . 3_665 H14 I2 3.2808 no . 3_655 H14 C3 3.5838 no . 2_645 H14 C4 3.2299 no . 2_645 H14 C11 3.2153 no . 2_645 H14 H11A 2.5706 no . 2_645 H14 H12B 3.4277 no . 2_645 H15 S1 3.3884 no . 3_655 H15 C1 3.1387 no . 2_645 H15 C2 3.1085 no . 2_645 H15 C3 3.0954 no . 2_645 H15 C4 2.9989 no . 2_645 H15 C5 2.8940 no . 2_645 H15 C10 2.9779 no . 2_645 H15 H24 3.5200 no . 2_645 H16 C23 2.8306 no . 2_645 H16 C24 2.9456 no . 2_645 H16 H7 3.2540 no . 4_555 H16 H23 2.5211 no . 2_645 H16 H24 2.7736 no . 2_645 H17 C17 3.0064 no . 3_755 H17 C18 2.9556 no . 3_755 H17 H7 3.3639 no . 4_555 H17 H17 2.5849 no . 3_755 H17 H18 2.4657 no . 3_755 H17 H21 2.9931 no . 1_655 H17 H23 3.3623 no . 2_645 H18 C17 3.2666 no . 3_755 H18 H17 2.4657 no . 3_755 H18 H20 3.5927 no . 3_655 H18 H21 3.3687 no . 1_655 H20 I2 3.2846 no . 3_655 H20 C13 3.1536 no . 3_655 H20 C14 3.2740 no . 3_655 H20 C15 3.2811 no . 3_655 H20 C16 3.2054 no . 3_655 H20 C17 3.1535 no . 3_655 H20 C18 3.1120 no . 3_655 H20 H18 3.5927 no . 3_655 H21 C6 3.4052 no . 4_455 H21 C7 3.3157 no . 4_455 H21 C17 3.4480 no . 1_455 H21 H3 3.5809 no . 1_455 H21 H7 3.4262 no . 4_455 H21 H12A 3.2779 no . 4_455 H21 H17 2.9931 no . 1_455 H21 H18 3.3687 no . 1_455 H22 I2 3.5758 no . 4_455 H22 C3 3.4723 no . 1_455 H22 C5 3.1246 no . 4_455 H22 C6 3.4031 no . 4_455 H22 C7 3.5519 no . 4_455 H22 C8 3.3789 no . 4_455 H22 C9 3.1274 no . 4_455 H22 C10 3.0146 no . 4_455 H22 H3 2.5691 no . 1_455 H23 I2 3.0532 no . 4_455 H23 C16 3.2653 no . 2_655 H23 H3 3.4856 no . 1_455 H23 H12A 3.1016 no . 3_665 H23 H12B 3.4332 no . 3_665 H23 H16 2.5211 no . 2_655 H23 H17 3.3623 no . 2_655 H24 C12 3.4468 no . 3_665 H24 C16 3.3136 no . 2_655 H24 H7 3.0855 no . 3_665 H24 H12A 3.4785 no . 3_665 H24 H12B 2.7305 no . 3_665 H24 H15 3.5200 no . 2_655 H24 H16 2.7736 no . 2_655 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment '- new11.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 850826' #TrackingRef '- new11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24.05 H18.10 Cl0.10 I2 Se Te' _chemical_formula_weight 770.99 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.079(3) _cell_length_b 14.105(4) _cell_length_c 16.134(5) _cell_angle_alpha 82.21(2) _cell_angle_beta 78.41(2) _cell_angle_gamma 77.42(2) _cell_volume 2399.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9615 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 26.37 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 5.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_T_max 0.852 _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.944 _diffrn_reflns_number 19966 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0880 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _reflns_number_total 9555 _reflns_number_gt 7698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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. Disorderd dichloromethane solvate, DFIX, instruction used for Cl-C and Cl-Cl distances ISOR and PART commands used to deal with disorder ; _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^)+(0.1295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9555 _refine_ls_number_parameters 516 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2394 _refine_ls_wR_factor_gt 0.1888 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.096 _refine_ls_shift/su_mean 0.001 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 0.88989(7) 0.58331(6) 0.17106(5) 0.0311(2) Uani 1 1 d . . . I2 I 1.21850(7) 0.86365(6) 0.03789(6) 0.0322(2) Uani 1 1 d . . . I3 I 0.65550(7) 0.29364(6) 0.26720(5) 0.0318(2) Uani 1 1 d . . . I4 I 1.09732(8) 0.00087(6) 0.33242(6) 0.0339(2) Uani 1 1 d . . . Te1 Te 1.06117(7) 0.72177(5) 0.10539(5) 0.0237(2) Uani 1 1 d . . . Te2 Te 0.87855(7) 0.14648(5) 0.29620(5) 0.0242(2) Uani 1 1 d . . . Se1 Se 1.15067(11) 0.60786(9) 0.27971(8) 0.0266(3) Uani 1 1 d . . . Se2 Se 0.85761(11) -0.03950(9) 0.20098(8) 0.0292(3) Uani 1 1 d . . . C1 C 1.2066(10) 0.6041(7) 0.0646(8) 0.023(2) Uani 1 1 d . . . C2 C 1.2541(11) 0.6082(8) -0.0235(8) 0.027(3) Uani 1 1 d . . . H2A H 1.2281 0.6659 -0.0585 0.032 Uiso 1 1 calc R . . C3 C 1.3389(11) 0.5294(9) -0.0612(9) 0.030(3) Uani 1 1 d . . . H3A H 1.3711 0.5344 -0.1205 0.036 Uiso 1 1 calc R . . C4 C 1.3742(11) 0.4449(8) -0.0106(8) 0.025(2) Uani 1 1 d . . . C5 C 1.3285(9) 0.4438(8) 0.0782(7) 0.020(2) Uani 1 1 d . . . C6 C 1.3743(11) 0.3522(8) 0.1192(8) 0.024(2) Uani 1 1 d . . . C7 C 1.3407(11) 0.3366(8) 0.2065(8) 0.028(3) Uani 1 1 d . . . H7A H 1.3681 0.2747 0.2354 0.034 Uiso 1 1 calc R . . C8 C 1.2646(12) 0.4141(9) 0.2527(8) 0.029(3) Uani 1 1 d . . . H8A H 1.2427 0.4047 0.3128 0.035 Uiso 1 1 calc R . . C9 C 1.2225(11) 0.5035(8) 0.2097(7) 0.023(2) Uani 1 1 d . . . C10 C 1.2500(10) 0.5193(7) 0.1191(7) 0.020(2) Uani 1 1 d . . . C11 C 1.4546(13) 0.2842(9) 0.0544(8) 0.032(3) Uani 1 1 d . . . H11A H 1.4172 0.2266 0.0544 0.039 Uiso 1 1 calc R . . H11B H 1.5410 0.2619 0.0665 0.039 Uiso 1 1 calc R . . C12 C 1.4546(11) 0.3498(9) -0.0331(8) 0.026(2) Uani 1 1 d . . . H12A H 1.5409 0.3578 -0.0597 0.031 Uiso 1 1 calc R . . H12B H 1.4192 0.3205 -0.0729 0.031 Uiso 1 1 calc R . . C13 C 0.9832(11) 0.7482(8) -0.0093(8) 0.026(2) Uani 1 1 d U . . C14 C 0.9692(11) 0.6719(8) -0.0516(8) 0.025(2) Uani 1 1 d . . . H14A H 0.9978 0.6061 -0.0309 0.030 Uiso 1 1 calc R . . C15 C 0.9149(12) 0.6916(9) -0.1223(9) 0.031(3) Uani 1 1 d . . . H15A H 0.9096 0.6397 -0.1525 0.037 Uiso 1 1 calc R . . C16 C 0.8665(11) 0.7892(10) -0.1507(8) 0.029(3) Uani 1 1 d . . . H16A H 0.8257 0.8025 -0.1986 0.035 Uiso 1 1 calc R . . C17 C 0.8781(12) 0.8653(9) -0.1092(8) 0.030(3) Uani 1 1 d . . . H17A H 0.8467 0.9309 -0.1290 0.036 Uiso 1 1 calc R . . C18 C 0.9362(11) 0.8453(9) -0.0378(8) 0.027(3) Uani 1 1 d . . . H18A H 0.9440 0.8973 -0.0087 0.032 Uiso 1 1 calc R . . C19 C 1.3042(12) 0.6506(10) 0.2794(8) 0.030(3) Uani 1 1 d . . . C20 C 1.3019(14) 0.7470(11) 0.2790(9) 0.041(3) Uani 1 1 d . . . H20A H 1.2245 0.7922 0.2797 0.049 Uiso 1 1 calc R . . C21 C 1.4104(19) 0.7804(14) 0.2777(10) 0.058(5) Uani 1 1 d . . . H21A H 1.4066 0.8485 0.2767 0.069 Uiso 1 1 calc R . . C22 C 1.5200(17) 0.7194(13) 0.2777(10) 0.051(4) Uani 1 1 d . . . H22A H 1.5929 0.7441 0.2786 0.061 Uiso 1 1 calc R . . C23 C 1.5294(14) 0.6197(14) 0.2764(11) 0.052(4) Uani 1 1 d . . . H23A H 1.6086 0.5764 0.2731 0.063 Uiso 1 1 calc R . . C24 C 1.4196(11) 0.5849(10) 0.2800(9) 0.034(3) Uani 1 1 d . . . H24A H 1.4228 0.5167 0.2828 0.040 Uiso 1 1 calc R . . C25 C 0.6798(12) -0.0998(9) 0.1197(8) 0.032(3) Uani 1 1 d . . . H25A H 0.7473 -0.1512 0.1018 0.038 Uiso 1 1 calc R . . C26 C 0.5612(13) -0.0914(11) 0.0972(9) 0.042(4) Uani 1 1 d . . . H26A H 0.5480 -0.1395 0.0659 0.051 Uiso 1 1 calc R . . C27 C 0.4650(12) -0.0157(10) 0.1192(9) 0.036(3) Uani 1 1 d . . . H27A H 0.3863 -0.0100 0.1022 0.044 Uiso 1 1 calc R . . C28 C 0.4836(13) 0.0526(9) 0.1667(9) 0.036(3) Uani 1 1 d . . . H28A H 0.4165 0.1051 0.1828 0.043 Uiso 1 1 calc R . . C29 C 0.5986(12) 0.0461(8) 0.1915(8) 0.031(3) Uani 1 1 d . . . H29A H 0.6102 0.0941 0.2237 0.037 Uiso 1 1 calc R . . C30 C 0.6959(12) -0.0308(9) 0.1689(8) 0.031(3) Uani 1 1 d . . . C31 C 0.7665(11) 0.0656(9) 0.3902(7) 0.029(3) Uani 1 1 d . . . C32 C 0.7032(9) 0.1128(9) 0.4591(7) 0.022(2) Uani 1 1 d . . . H32A H 0.7010 0.1806 0.4581 0.027 Uiso 1 1 calc R . . C33 C 0.6389(12) 0.0630(10) 0.5342(8) 0.033(3) Uani 1 1 d . . . H33A H 0.5924 0.0971 0.5810 0.040 Uiso 1 1 calc R . . C34 C 0.6484(11) -0.0345(10) 0.5342(8) 0.031(3) Uani 1 1 d . . . C35 C 0.7075(10) -0.0836(9) 0.4616(7) 0.024(2) Uani 1 1 d . . . C36 C 0.7003(12) -0.1818(10) 0.4740(8) 0.032(3) Uani 1 1 d . . . C37 C 0.7492(11) -0.2389(8) 0.4067(9) 0.031(3) Uani 1 1 d . . . H37A H 0.7477 -0.3066 0.4125 0.037 Uiso 1 1 calc R . . C38 C 0.8011(12) -0.1911(9) 0.3292(8) 0.030(3) Uani 1 1 d . . . H38A H 0.8355 -0.2294 0.2829 0.036 Uiso 1 1 calc R . . C39 C 0.8055(10) -0.0943(9) 0.3160(7) 0.024(2) Uani 1 1 d . . . C40 C 0.7648(10) -0.0342(8) 0.3855(7) 0.023(2) Uani 1 1 d . . . C41 C 0.5988(14) -0.1086(11) 0.6041(9) 0.042(3) Uani 1 1 d . . . H41A H 0.5061 -0.0914 0.6196 0.050 Uiso 1 1 calc R . . H41B H 0.6358 -0.1113 0.6555 0.050 Uiso 1 1 calc R . . C42 C 0.6400(14) -0.2068(10) 0.5646(9) 0.043(3) Uani 1 1 d . . . H42A H 0.7008 -0.2527 0.5955 0.051 Uiso 1 1 calc R . . H42B H 0.5667 -0.2369 0.5663 0.051 Uiso 1 1 calc R . . C43 C 0.9197(11) 0.2382(9) 0.3807(8) 0.029(3) Uani 1 1 d . . . C44 C 0.9461(12) 0.2007(9) 0.4588(8) 0.031(3) Uani 1 1 d . . . H44A H 0.9406 0.1352 0.4795 0.037 Uiso 1 1 calc R . . C45 C 0.9816(13) 0.2612(11) 0.5082(8) 0.038(3) Uani 1 1 d . . . H45A H 0.9990 0.2369 0.5633 0.045 Uiso 1 1 calc R . . C46 C 0.9912(16) 0.3561(12) 0.4768(10) 0.051(4) Uani 1 1 d . . . H46A H 1.0149 0.3966 0.5108 0.061 Uiso 1 1 calc R . . C47 C 0.9667(14) 0.3927(11) 0.3966(10) 0.047(4) Uani 1 1 d . . . H47A H 0.9747 0.4576 0.3751 0.056 Uiso 1 1 calc R . . C48 C 0.9298(12) 0.3330(9) 0.3469(9) 0.034(3) Uani 1 1 d . . . H48A H 0.9123 0.3568 0.2917 0.041 Uiso 1 1 calc R . . C49 C 0.478(3) 0.467(2) 0.495(9) 0.100 Uiso 0.10 1 d PD A -1 H49A H 0.5051 0.4309 0.5474 0.120 Uiso 0.10 1 calc PR A -1 H49B H 0.5490 0.4618 0.4461 0.120 Uiso 0.10 1 calc PR A -1 Cl1 Cl 0.345(5) 0.441(4) 0.474(4) 0.079(14) Uiso 0.10 1 d PD A -1 Cl2 Cl 0.395(3) 0.582(2) 0.507(2) 0.041(7) Uiso 0.10 1 d PD A -1 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 0.0225(4) 0.0282(4) 0.0413(5) -0.0015(3) -0.0048(3) -0.0045(3) I2 0.0245(4) 0.0238(4) 0.0474(5) -0.0038(3) -0.0049(4) -0.0038(3) I3 0.0256(4) 0.0301(4) 0.0370(5) 0.0034(3) -0.0114(4) 0.0015(3) I4 0.0228(4) 0.0326(4) 0.0421(5) 0.0053(4) -0.0096(4) 0.0016(3) Te1 0.0197(4) 0.0196(4) 0.0302(4) -0.0024(3) -0.0056(3) 0.0009(3) Te2 0.0198(4) 0.0241(4) 0.0279(4) 0.0006(3) -0.0066(3) -0.0023(3) Se1 0.0220(6) 0.0285(6) 0.0277(6) -0.0064(5) -0.0042(5) 0.0008(5) Se2 0.0240(6) 0.0331(6) 0.0302(7) -0.0040(5) -0.0042(5) -0.0046(5) C1 0.015(5) 0.015(5) 0.037(7) -0.001(4) -0.010(5) 0.008(4) C2 0.019(6) 0.021(5) 0.036(7) -0.004(5) -0.001(5) 0.002(5) C3 0.019(6) 0.028(6) 0.043(8) -0.013(5) -0.007(5) 0.000(5) C4 0.024(6) 0.025(6) 0.027(6) -0.002(5) -0.007(5) -0.001(5) C5 0.008(5) 0.023(5) 0.029(6) -0.009(4) -0.007(4) 0.005(4) C6 0.021(6) 0.014(5) 0.033(7) 0.005(4) -0.005(5) -0.001(4) C7 0.020(6) 0.022(5) 0.037(7) 0.001(5) -0.009(5) 0.007(5) C8 0.030(7) 0.036(6) 0.019(6) 0.009(5) -0.008(5) -0.008(5) C9 0.022(6) 0.021(5) 0.025(6) -0.005(4) -0.005(5) 0.002(5) C10 0.017(5) 0.011(5) 0.038(7) -0.001(4) -0.017(5) -0.006(4) C11 0.033(7) 0.027(6) 0.033(7) 0.001(5) -0.009(6) 0.003(5) C12 0.015(5) 0.030(6) 0.028(6) -0.007(5) -0.001(5) 0.006(5) C13 0.026(3) 0.026(3) 0.026(3) -0.0023(10) -0.0046(11) -0.0046(11) C14 0.025(6) 0.024(6) 0.029(6) -0.005(5) -0.004(5) -0.007(5) C15 0.028(7) 0.024(6) 0.043(8) -0.004(5) -0.008(6) -0.010(5) C16 0.020(6) 0.046(7) 0.023(6) 0.004(5) -0.003(5) -0.012(5) C17 0.032(7) 0.024(6) 0.029(7) 0.000(5) -0.007(5) 0.006(5) C18 0.019(6) 0.026(6) 0.036(7) -0.008(5) -0.005(5) -0.001(5) C19 0.026(6) 0.043(7) 0.023(6) -0.008(5) -0.009(5) -0.006(6) C20 0.042(8) 0.039(7) 0.045(8) -0.002(6) -0.015(7) -0.011(7) C21 0.090(14) 0.060(10) 0.042(9) 0.000(8) -0.023(9) -0.048(11) C22 0.054(10) 0.063(11) 0.048(9) -0.012(8) -0.014(8) -0.029(9) C23 0.027(8) 0.074(11) 0.056(10) -0.008(8) -0.005(7) -0.011(8) C24 0.012(6) 0.035(7) 0.047(8) -0.008(6) 0.004(5) 0.003(5) C25 0.024(6) 0.033(6) 0.036(7) -0.012(5) 0.000(5) 0.000(5) C26 0.035(8) 0.054(9) 0.041(8) -0.026(7) -0.002(6) -0.008(7) C27 0.025(7) 0.032(7) 0.052(9) -0.004(6) -0.011(6) -0.002(5) C28 0.031(7) 0.031(7) 0.042(8) 0.000(6) -0.007(6) 0.002(6) C29 0.035(7) 0.018(5) 0.037(7) -0.002(5) -0.007(6) 0.004(5) C30 0.030(7) 0.025(6) 0.039(7) -0.004(5) -0.002(6) -0.009(5) C31 0.027(6) 0.038(7) 0.020(6) 0.010(5) -0.012(5) -0.004(5) C32 0.007(5) 0.030(6) 0.027(6) -0.004(5) 0.003(4) -0.003(4) C33 0.031(7) 0.047(8) 0.022(6) -0.005(5) -0.001(5) -0.011(6) C34 0.021(6) 0.042(7) 0.028(7) 0.006(5) -0.008(5) -0.008(5) C35 0.013(5) 0.033(6) 0.026(6) -0.003(5) -0.005(4) -0.004(5) C36 0.031(7) 0.038(7) 0.028(7) 0.011(5) -0.010(5) -0.013(6) C37 0.025(6) 0.017(5) 0.051(8) 0.007(5) -0.011(6) -0.010(5) C38 0.032(7) 0.032(6) 0.030(7) 0.004(5) -0.012(5) -0.012(5) C39 0.010(5) 0.036(6) 0.022(6) -0.009(5) -0.002(4) 0.005(5) C40 0.019(5) 0.023(5) 0.028(6) 0.000(5) -0.007(5) -0.006(4) C41 0.032(7) 0.052(8) 0.038(8) 0.011(6) -0.011(6) -0.009(7) C42 0.035(8) 0.040(8) 0.048(9) 0.010(6) 0.001(7) -0.011(6) C43 0.021(6) 0.038(7) 0.032(7) -0.005(5) -0.006(5) -0.008(5) C44 0.030(7) 0.031(6) 0.036(7) 0.006(5) -0.016(6) -0.011(5) C45 0.035(7) 0.058(9) 0.024(7) -0.005(6) -0.012(6) -0.011(7) C46 0.056(10) 0.059(10) 0.048(9) -0.030(8) -0.005(8) -0.020(8) C47 0.049(9) 0.035(7) 0.064(10) -0.002(7) 0.001(8) -0.033(7) C48 0.035(7) 0.024(6) 0.039(7) -0.001(5) -0.006(6) -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 I1 Te1 2.9636(13) . ? I2 Te1 2.8973(13) . ? I3 Te2 2.9328(14) . ? I4 Te2 2.9172(14) . ? Te1 C1 2.118(10) . ? Te1 C13 2.151(12) . ? Te2 C31 2.129(12) . ? Te2 C43 2.175(12) . ? Se1 C9 1.912(11) . ? Se1 C19 1.923(12) . ? Se2 C30 1.937(13) . ? Se2 C39 1.937(12) . ? C1 C2 1.411(17) . ? C1 C10 1.439(15) . ? C2 C3 1.410(15) . ? C2 H2A 0.9500 . ? C3 C4 1.380(18) . ? C3 H3A 0.9500 . ? C4 C5 1.419(16) . ? C4 C12 1.486(15) . ? C5 C10 1.372(14) . ? C5 C6 1.408(15) . ? C6 C7 1.382(17) . ? C6 C11 1.527(17) . ? C7 C8 1.425(17) . ? C7 H7A 0.9500 . ? C8 C9 1.387(16) . ? C8 H8A 0.9500 . ? C9 C10 1.429(16) . ? C11 C12 1.579(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.401(16) . ? C13 C18 1.405(16) . ? C14 C15 1.363(18) . ? C14 H14A 0.9500 . ? C15 C16 1.414(18) . ? C15 H15A 0.9500 . ? C16 C17 1.382(17) . ? C16 H16A 0.9500 . ? C17 C18 1.396(18) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.353(19) . ? C19 C24 1.408(17) . ? C20 C21 1.38(2) . ? C20 H20A 0.9500 . ? C21 C22 1.33(3) . ? C21 H21A 0.9500 . ? C22 C23 1.39(2) . ? C22 H22A 0.9500 . ? C23 C24 1.395(19) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.397(17) . ? C25 C26 1.410(19) . ? C25 H25A 0.9500 . ? C26 C27 1.362(19) . ? C26 H26A 0.9500 . ? C27 C28 1.381(19) . ? C27 H27A 0.9500 . ? C28 C29 1.392(19) . ? C28 H28A 0.9500 . ? C29 C30 1.383(17) . ? C29 H29A 0.9500 . ? C31 C32 1.363(16) . ? C31 C40 1.424(17) . ? C32 C33 1.451(16) . ? C32 H32A 0.9500 . ? C33 C34 1.356(19) . ? C33 H33A 0.9500 . ? C34 C35 1.413(17) . ? C34 C41 1.532(18) . ? C35 C36 1.390(17) . ? C35 C40 1.429(16) . ? C36 C37 1.390(18) . ? C36 C42 1.509(18) . ? C37 C38 1.414(17) . ? C37 H37A 0.9500 . ? C38 C39 1.363(17) . ? C38 H38A 0.9500 . ? C39 C40 1.438(16) . ? C41 C42 1.54(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.361(18) . ? C43 C48 1.393(18) . ? C44 C45 1.405(17) . ? C44 H44A 0.9500 . ? C45 C46 1.38(2) . ? C45 H45A 0.9500 . ? C46 C47 1.38(2) . ? C46 H46A 0.9500 . ? C47 C48 1.407(19) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 Cl2 1.7000(12) . ? C49 Cl1 1.7000(11) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? Cl1 Cl2 2.32(6) . ? 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 Te1 C13 95.7(4) . . ? C1 Te1 I2 92.3(3) . . ? C13 Te1 I2 90.0(3) . . ? C1 Te1 I1 89.8(3) . . ? C13 Te1 I1 87.9(3) . . ? I2 Te1 I1 177.17(4) . . ? C31 Te2 C43 97.3(5) . . ? C31 Te2 I4 87.7(3) . . ? C43 Te2 I4 88.5(3) . . ? C31 Te2 I3 90.9(3) . . ? C43 Te2 I3 89.9(3) . . ? I4 Te2 I3 177.68(4) . . ? C9 Se1 C19 97.0(5) . . ? C30 Se2 C39 94.0(5) . . ? C2 C1 C10 119.6(10) . . ? C2 C1 Te1 115.8(8) . . ? C10 C1 Te1 124.3(9) . . ? C3 C2 C1 122.1(11) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? C4 C3 C2 118.8(12) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 117.9(10) . . ? C3 C4 C12 130.6(11) . . ? C5 C4 C12 111.5(10) . . ? C10 C5 C6 124.2(11) . . ? C10 C5 C4 126.0(11) . . ? C6 C5 C4 109.8(9) . . ? C7 C6 C5 118.7(10) . . ? C7 C6 C11 130.8(10) . . ? C5 C6 C11 110.5(10) . . ? C6 C7 C8 119.4(10) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 119.9(11) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.5(10) . . ? C8 C9 Se1 115.4(9) . . ? C10 C9 Se1 122.3(8) . . ? C5 C10 C9 116.0(10) . . ? C5 C10 C1 115.3(10) . . ? C9 C10 C1 128.7(10) . . ? C6 C11 C12 103.6(9) . . ? C6 C11 H11A 111.0 . . ? C12 C11 H11A 111.0 . . ? C6 C11 H11B 111.0 . . ? C12 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? C4 C12 C11 104.6(9) . . ? C4 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? C4 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.9 . . ? C14 C13 C18 119.8(11) . . ? C14 C13 Te1 122.0(9) . . ? C18 C13 Te1 118.0(8) . . ? C15 C14 C13 120.3(11) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 120.0(11) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 120.5(12) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 119.5(11) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C13 119.8(11) . . ? C17 C18 H18A 120.1 . . ? C13 C18 H18A 120.1 . . ? C20 C19 C24 118.5(12) . . ? C20 C19 Se1 119.3(10) . . ? C24 C19 Se1 122.2(10) . . ? C19 C20 C21 120.9(15) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C22 C21 C20 121.3(16) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 120.7(15) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C22 C23 C24 118.3(15) . . ? C22 C23 H23A 120.8 . . ? C24 C23 H23A 120.8 . . ? C23 C24 C19 120.1(13) . . ? C23 C24 H24A 119.9 . . ? C19 C24 H24A 119.9 . . ? C30 C25 C26 118.5(12) . . ? C30 C25 H25A 120.8 . . ? C26 C25 H25A 120.8 . . ? C27 C26 C25 121.4(12) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 119.1(13) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C27 C28 C29 121.3(12) . . ? C27 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C30 C29 C28 119.3(12) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C29 C30 C25 120.3(12) . . ? C29 C30 Se2 119.9(9) . . ? C25 C30 Se2 119.8(9) . . ? C32 C31 C40 121.3(10) . . ? C32 C31 Te2 115.9(9) . . ? C40 C31 Te2 122.7(9) . . ? C31 C32 C33 122.3(11) . . ? C31 C32 H32A 118.8 . . ? C33 C32 H32A 118.8 . . ? C34 C33 C32 116.8(11) . . ? C34 C33 H33A 121.6 . . ? C32 C33 H33A 121.6 . . ? C33 C34 C35 121.6(11) . . ? C33 C34 C41 130.0(12) . . ? C35 C34 C41 108.4(11) . . ? C36 C35 C34 111.9(11) . . ? C36 C35 C40 126.2(11) . . ? C34 C35 C40 121.9(11) . . ? C37 C36 C35 118.6(11) . . ? C37 C36 C42 131.6(12) . . ? C35 C36 C42 109.7(11) . . ? C36 C37 C38 116.6(11) . . ? C36 C37 H37A 121.7 . . ? C38 C37 H37A 121.7 . . ? C39 C38 C37 125.0(12) . . ? C39 C38 H38A 117.5 . . ? C37 C38 H38A 117.5 . . ? C38 C39 C40 120.2(11) . . ? C38 C39 Se2 118.3(8) . . ? C40 C39 Se2 121.5(9) . . ? C31 C40 C35 115.5(10) . . ? C31 C40 C39 131.4(11) . . ? C35 C40 C39 113.0(10) . . ? C34 C41 C42 104.5(11) . . ? C34 C41 H41A 110.8 . . ? C42 C41 H41A 110.8 . . ? C34 C41 H41B 110.8 . . ? C42 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? C36 C42 C41 105.1(11) . . ? C36 C42 H42A 110.7 . . ? C41 C42 H42A 110.7 . . ? C36 C42 H42B 110.7 . . ? C41 C42 H42B 110.7 . . ? H42A C42 H42B 108.8 . . ? C44 C43 C48 122.8(11) . . ? C44 C43 Te2 120.8(9) . . ? C48 C43 Te2 116.1(9) . . ? C43 C44 C45 118.5(12) . . ? C43 C44 H44A 120.8 . . ? C45 C44 H44A 120.8 . . ? C46 C45 C44 120.2(13) . . ? C46 C45 H45A 119.9 . . ? C44 C45 H45A 119.9 . . ? C45 C46 C47 120.7(12) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C47 C48 119.5(13) . . ? C46 C47 H47A 120.2 . . ? C48 C47 H47A 120.2 . . ? C43 C48 C47 118.3(13) . . ? C43 C48 H48A 120.9 . . ? C47 C48 H48A 120.9 . . ? Cl2 C49 Cl1 86(3) . . ? Cl2 C49 H49A 114.2 . . ? Cl1 C49 H49A 114.2 . . ? Cl2 C49 H49B 114.4 . . ? Cl1 C49 H49B 114.4 . . ? H49A C49 H49B 111.4 . . ? C49 Cl1 Cl2 46.9(13) . . ? C49 Cl2 Cl1 46.9(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Te1 C1 C2 31.2(9) . . . . ? I2 Te1 C1 C2 -59.0(8) . . . . ? I1 Te1 C1 C2 119.1(8) . . . . ? C13 Te1 C1 C10 -143.3(9) . . . . ? I2 Te1 C1 C10 126.5(9) . . . . ? I1 Te1 C1 C10 -55.4(9) . . . . ? C10 C1 C2 C3 3.3(17) . . . . ? Te1 C1 C2 C3 -171.5(9) . . . . ? C1 C2 C3 C4 1.4(17) . . . . ? C2 C3 C4 C5 -3.5(17) . . . . ? C2 C3 C4 C12 175.9(12) . . . . ? C3 C4 C5 C10 1.0(17) . . . . ? C12 C4 C5 C10 -178.5(10) . . . . ? C3 C4 C5 C6 -180.0(10) . . . . ? C12 C4 C5 C6 0.5(13) . . . . ? C10 C5 C6 C7 -1.2(17) . . . . ? C4 C5 C6 C7 179.7(10) . . . . ? C10 C5 C6 C11 177.6(10) . . . . ? C4 C5 C6 C11 -1.4(13) . . . . ? C5 C6 C7 C8 -2.1(17) . . . . ? C11 C6 C7 C8 179.3(12) . . . . ? C6 C7 C8 C9 1.6(18) . . . . ? C7 C8 C9 C10 2.2(17) . . . . ? C7 C8 C9 Se1 -168.0(9) . . . . ? C19 Se1 C9 C8 88.6(10) . . . . ? C19 Se1 C9 C10 -81.5(10) . . . . ? C6 C5 C10 C9 4.7(15) . . . . ? C4 C5 C10 C9 -176.3(11) . . . . ? C6 C5 C10 C1 -175.4(10) . . . . ? C4 C5 C10 C1 3.5(16) . . . . ? C8 C9 C10 C5 -5.1(16) . . . . ? Se1 C9 C10 C5 164.4(8) . . . . ? C8 C9 C10 C1 175.0(11) . . . . ? Se1 C9 C10 C1 -15.5(16) . . . . ? C2 C1 C10 C5 -5.5(15) . . . . ? Te1 C1 C10 C5 168.8(7) . . . . ? C2 C1 C10 C9 174.4(11) . . . . ? Te1 C1 C10 C9 -11.3(16) . . . . ? C7 C6 C11 C12 -179.6(12) . . . . ? C5 C6 C11 C12 1.7(13) . . . . ? C3 C4 C12 C11 -178.9(13) . . . . ? C5 C4 C12 C11 0.5(13) . . . . ? C6 C11 C12 C4 -1.3(13) . . . . ? C1 Te1 C13 C14 41.7(10) . . . . ? I2 Te1 C13 C14 133.9(9) . . . . ? I1 Te1 C13 C14 -47.9(9) . . . . ? C1 Te1 C13 C18 -143.4(9) . . . . ? I2 Te1 C13 C18 -51.2(9) . . . . ? I1 Te1 C13 C18 126.9(9) . . . . ? C18 C13 C14 C15 2.6(17) . . . . ? Te1 C13 C14 C15 177.4(9) . . . . ? C13 C14 C15 C16 -3.3(18) . . . . ? C14 C15 C16 C17 2.5(18) . . . . ? C15 C16 C17 C18 -1.1(18) . . . . ? C16 C17 C18 C13 0.5(18) . . . . ? C14 C13 C18 C17 -1.2(17) . . . . ? Te1 C13 C18 C17 -176.2(9) . . . . ? C9 Se1 C19 C20 144.3(11) . . . . ? C9 Se1 C19 C24 -36.0(11) . . . . ? C24 C19 C20 C21 1(2) . . . . ? Se1 C19 C20 C21 -179.2(11) . . . . ? C19 C20 C21 C22 -1(2) . . . . ? C20 C21 C22 C23 2(3) . . . . ? C21 C22 C23 C24 -4(2) . . . . ? C22 C23 C24 C19 4(2) . . . . ? C20 C19 C24 C23 -3(2) . . . . ? Se1 C19 C24 C23 177.5(11) . . . . ? C30 C25 C26 C27 3(2) . . . . ? C25 C26 C27 C28 -2(2) . . . . ? C26 C27 C28 C29 1(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C25 1.7(19) . . . . ? C28 C29 C30 Se2 178.8(10) . . . . ? C26 C25 C30 C29 -3(2) . . . . ? C26 C25 C30 Se2 -179.8(11) . . . . ? C39 Se2 C30 C29 80.3(11) . . . . ? C39 Se2 C30 C25 -102.5(11) . . . . ? C43 Te2 C31 C32 28.7(10) . . . . ? I4 Te2 C31 C32 117.0(9) . . . . ? I3 Te2 C31 C32 -61.2(9) . . . . ? C43 Te2 C31 C40 -146.3(10) . . . . ? I4 Te2 C31 C40 -58.1(9) . . . . ? I3 Te2 C31 C40 123.7(9) . . . . ? C40 C31 C32 C33 4.9(18) . . . . ? Te2 C31 C32 C33 -170.2(9) . . . . ? C31 C32 C33 C34 2.4(18) . . . . ? C32 C33 C34 C35 -6.0(18) . . . . ? C32 C33 C34 C41 176.4(12) . . . . ? C33 C34 C35 C36 -176.5(12) . . . . ? C41 C34 C35 C36 1.5(15) . . . . ? C33 C34 C35 C40 2.5(19) . . . . ? C41 C34 C35 C40 -179.4(11) . . . . ? C34 C35 C36 C37 177.0(11) . . . . ? C40 C35 C36 C37 -2.0(19) . . . . ? C34 C35 C36 C42 -4.5(15) . . . . ? C40 C35 C36 C42 176.4(12) . . . . ? C35 C36 C37 C38 -1.1(18) . . . . ? C42 C36 C37 C38 -179.2(14) . . . . ? C36 C37 C38 C39 -0.6(19) . . . . ? C37 C38 C39 C40 5.3(19) . . . . ? C37 C38 C39 Se2 -170.9(10) . . . . ? C30 Se2 C39 C38 78.7(10) . . . . ? C30 Se2 C39 C40 -97.4(9) . . . . ? C32 C31 C40 C35 -8.1(17) . . . . ? Te2 C31 C40 C35 166.7(8) . . . . ? C32 C31 C40 C39 168.5(12) . . . . ? Te2 C31 C40 C39 -16.6(18) . . . . ? C36 C35 C40 C31 -176.5(12) . . . . ? C34 C35 C40 C31 4.6(16) . . . . ? C36 C35 C40 C39 6.2(17) . . . . ? C34 C35 C40 C39 -172.7(11) . . . . ? C38 C39 C40 C31 175.8(12) . . . . ? Se2 C39 C40 C31 -8.2(18) . . . . ? C38 C39 C40 C35 -7.5(16) . . . . ? Se2 C39 C40 C35 168.6(8) . . . . ? C33 C34 C41 C42 179.8(14) . . . . ? C35 C34 C41 C42 1.9(14) . . . . ? C37 C36 C42 C41 -176.3(14) . . . . ? C35 C36 C42 C41 5.5(15) . . . . ? C34 C41 C42 C36 -4.3(15) . . . . ? C31 Te2 C43 C44 40.4(11) . . . . ? I4 Te2 C43 C44 -47.1(10) . . . . ? I3 Te2 C43 C44 131.3(10) . . . . ? C31 Te2 C43 C48 -145.9(10) . . . . ? I4 Te2 C43 C48 126.7(9) . . . . ? I3 Te2 C43 C48 -55.0(9) . . . . ? C48 C43 C44 C45 1.8(19) . . . . ? Te2 C43 C44 C45 175.1(9) . . . . ? C43 C44 C45 C46 -1(2) . . . . ? C44 C45 C46 C47 0(2) . . . . ? C45 C46 C47 C48 1(2) . . . . ? C44 C43 C48 C47 -1(2) . . . . ? Te2 C43 C48 C47 -174.8(10) . . . . ? C46 C47 C48 C43 0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.595 _refine_diff_density_min -3.214 _refine_diff_density_rms 0.637 #============================================================================== data_FK140DMF _database_code_depnum_ccdc_archive 'CCDC 850827' #TrackingRef '- 12.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C25.50 H21.50 Br2 N0.50 O1.50 Te2' _chemical_formula_moiety 'C25.50 H21.50 Br2 N0.50 O1.50 Te2' _chemical_formula_weight 773.96 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.599(3) _cell_length_b 23.952(6) _cell_length_c 17.983(4) _cell_angle_alpha 90.0000 _cell_angle_beta 95.095(7) _cell_angle_gamma 90.0000 _cell_volume 4976.3(18) _cell_formula_units_Z 8 _cell_measurement_reflns_used 17583 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 25.35 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912.00 _exptl_absorpt_coefficient_mu 5.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.433 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_reflns_number 31149 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9013 _reflns_number_gt 7872 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0692 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 9013 _refine_ls_number_parameters 568 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.950 _refine_diff_density_min -0.760 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Te Te -0.5308 1.6751 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.35437(2) -0.049317(13) 0.966033(14) 0.01231(8) Uani 1.0 4 d . . . Te2 Te 0.53572(2) -0.033852(12) 0.833576(14) 0.01129(8) Uani 1.0 4 d . . . Te3 Te 0.53370(3) 0.150922(13) 0.783412(15) 0.01502(8) Uani 1.0 4 d . . . Te4 Te 0.72241(3) 0.150357(13) 0.650241(15) 0.01580(8) Uani 1.0 4 d . . . Br1 Br 0.19307(4) 0.00449(2) 1.05072(2) 0.01792(11) Uani 1.0 4 d . . . Br2 Br 0.66053(4) 0.03069(2) 0.73146(3) 0.02141(12) Uani 1.0 4 d . . . Br3 Br 0.40841(4) 0.08515(2) 0.89511(2) 0.01675(11) Uani 1.0 4 d . . . Br4 Br 0.85970(4) 0.09860(2) 0.55267(3) 0.02850(13) Uani 1.0 4 d . . . O1 O 0.4619(3) -0.08685(13) 0.90036(14) 0.0152(7) Uani 1.0 4 d . . . O2 O 0.6250(3) 0.19462(13) 0.71911(15) 0.0201(8) Uani 1.0 4 d . . . O3 O 0.9445(3) 0.17614(15) 0.73638(18) 0.0343(10) Uani 1.0 4 d . . . N1 N 1.0515(4) 0.13420(17) 0.8327(2) 0.0205(10) Uani 1.0 4 d . . . C1 C 0.2333(4) -0.04593(19) 0.8693(3) 0.0134(10) Uani 1.0 4 d . . . C2 C 0.1195(4) -0.0555(2) 0.8822(3) 0.0171(11) Uani 1.0 4 d . . . C3 C 0.0283(4) -0.0563(2) 0.8252(3) 0.0229(12) Uani 1.0 4 d . . . C4 C 0.0534(4) -0.0460(2) 0.7538(3) 0.0182(11) Uani 1.0 4 d . . . C5 C 0.1692(4) -0.03681(18) 0.7398(3) 0.0133(10) Uani 1.0 4 d . . . C6 C 0.1791(4) -0.02873(19) 0.6626(3) 0.0163(11) Uani 1.0 4 d . . . C7 C 0.2848(4) -0.02254(19) 0.6371(3) 0.0165(11) Uani 1.0 4 d . . . C8 C 0.3831(4) -0.02336(19) 0.6897(3) 0.0164(11) Uani 1.0 4 d . . . C9 C 0.3756(4) -0.02978(18) 0.7653(2) 0.0098(10) Uani 1.0 4 d . . . C10 C 0.2654(4) -0.03713(18) 0.7944(3) 0.0136(10) Uani 1.0 4 d . . . C11 C -0.0240(4) -0.0440(3) 0.6814(3) 0.0265(13) Uani 1.0 4 d . . . C12 C 0.0582(4) -0.0290(3) 0.6226(3) 0.0234(12) Uani 1.0 4 d . . . C13 C 0.2943(4) -0.1298(2) 0.9971(3) 0.0184(11) Uani 1.0 4 d . . . C14 C 0.2422(4) -0.1377(3) 1.0624(3) 0.0226(12) Uani 1.0 4 d . . . C15 C 0.2016(5) -0.1902(3) 1.0783(3) 0.0293(13) Uani 1.0 4 d . . . C16 C 0.2133(5) -0.2349(3) 1.0307(3) 0.0353(14) Uani 1.0 4 d . . . C17 C 0.2657(5) -0.2266(3) 0.9660(3) 0.0362(15) Uani 1.0 4 d . . . C18 C 0.3060(5) -0.1740(2) 0.9485(3) 0.0282(13) Uani 1.0 4 d . . . C19 C 0.6031(4) -0.10374(19) 0.7802(2) 0.0128(10) Uani 1.0 4 d . . . C20 C 0.5306(5) -0.1459(2) 0.7530(3) 0.0208(12) Uani 1.0 4 d . . . C21 C 0.5795(5) -0.1942(2) 0.7265(3) 0.0289(14) Uani 1.0 4 d . . . C22 C 0.6990(5) -0.1993(3) 0.7281(3) 0.0271(13) Uani 1.0 4 d . . . C23 C 0.7713(5) -0.1566(2) 0.7550(3) 0.0225(12) Uani 1.0 4 d . . . C24 C 0.7219(4) -0.1085(2) 0.7809(3) 0.0181(11) Uani 1.0 4 d . . . C31 C 0.4174(4) 0.1296(2) 0.6893(3) 0.0169(11) Uani 1.0 4 d . . . C32 C 0.3026(4) 0.12387(19) 0.7031(3) 0.0168(11) Uani 1.0 4 d . . . C33 C 0.2125(4) 0.1147(2) 0.6468(3) 0.0217(12) Uani 1.0 4 d . . . C34 C 0.2415(4) 0.1096(2) 0.5755(3) 0.0195(11) Uani 1.0 4 d . . . C35 C 0.3585(4) 0.11425(19) 0.5608(3) 0.0162(11) Uani 1.0 4 d . . . C36 C 0.3713(4) 0.1070(2) 0.4831(3) 0.0212(12) Uani 1.0 4 d . . . C37 C 0.4779(5) 0.1123(3) 0.4577(3) 0.0249(13) Uani 1.0 4 d . . . C38 C 0.5730(4) 0.1234(2) 0.5099(3) 0.0201(12) Uani 1.0 4 d . . . C39 C 0.5638(4) 0.1296(2) 0.5855(3) 0.0153(11) Uani 1.0 4 d . . . C40 C 0.4521(4) 0.12488(19) 0.6154(3) 0.0143(11) Uani 1.0 4 d . . . C41 C 0.1672(5) 0.0974(3) 0.5034(3) 0.0330(15) Uani 1.0 4 d . . . C42 C 0.2543(5) 0.0947(3) 0.4425(3) 0.0309(14) Uani 1.0 4 d . . . C43 C 0.4424(4) 0.2240(2) 0.8085(3) 0.0194(11) Uani 1.0 4 d . . . C44 C 0.4268(5) 0.2371(3) 0.8824(3) 0.0319(14) Uani 1.0 4 d . . . C45 C 0.3722(6) 0.2863(3) 0.8975(3) 0.0477(18) Uani 1.0 4 d . . . C46 C 0.3313(6) 0.3221(3) 0.8406(3) 0.0396(15) Uani 1.0 4 d . . . C47 C 0.3474(5) 0.3094(3) 0.7673(3) 0.0355(14) Uani 1.0 4 d . . . C48 C 0.4034(5) 0.2602(3) 0.7509(3) 0.0278(13) Uani 1.0 4 d . . . C49 C 0.7402(4) 0.2288(2) 0.5969(3) 0.0190(11) Uani 1.0 4 d . . . C50 C 0.6421(5) 0.2590(2) 0.5765(3) 0.0241(12) Uani 1.0 4 d . . . C51 C 0.6507(5) 0.3129(3) 0.5496(3) 0.0314(14) Uani 1.0 4 d . . . C52 C 0.7586(6) 0.3348(3) 0.5430(3) 0.0341(14) Uani 1.0 4 d . . . C53 C 0.8582(5) 0.3041(3) 0.5639(3) 0.0317(14) Uani 1.0 4 d . . . C54 C 0.8496(5) 0.2510(3) 0.5914(3) 0.0252(13) Uani 1.0 4 d . . . C55 C 0.9674(5) 0.1355(3) 0.7765(3) 0.0268(13) Uani 1.0 4 d . . . C56 C 1.1235(4) 0.1831(2) 0.8495(3) 0.0223(12) Uani 1.0 4 d . . . C57 C 1.0660(5) 0.0865(3) 0.8828(3) 0.0390(15) Uani 1.0 4 d . . . H2 H 0.1018 -0.0618 0.9321 0.0205 Uiso 1.0 4 calc R . . H3 H -0.0488 -0.0638 0.8361 0.0275 Uiso 1.0 4 calc R . . H7 H 0.2928 -0.0178 0.5854 0.0198 Uiso 1.0 4 calc R . . H8 H 0.4575 -0.0193 0.6722 0.0197 Uiso 1.0 4 calc R . . H11A H -0.0850 -0.0153 0.6836 0.0318 Uiso 1.0 4 calc R . . H11B H -0.0611 -0.0807 0.6704 0.0318 Uiso 1.0 4 calc R . . H12A H 0.0527 -0.0570 0.5819 0.0281 Uiso 1.0 4 calc R . . H12B H 0.0388 0.0081 0.6009 0.0281 Uiso 1.0 4 calc R . . H14 H 0.2345 -0.1075 1.0959 0.0271 Uiso 1.0 4 calc R . . H15 H 0.1648 -0.1958 1.1229 0.0352 Uiso 1.0 4 calc R . . H16 H 0.1855 -0.2709 1.0426 0.0424 Uiso 1.0 4 calc R . . H17 H 0.2744 -0.2569 0.9330 0.0435 Uiso 1.0 4 calc R . . H18 H 0.3416 -0.1684 0.9035 0.0339 Uiso 1.0 4 calc R . . H20 H 0.4490 -0.1421 0.7524 0.0249 Uiso 1.0 4 calc R . . H21 H 0.5310 -0.2237 0.7072 0.0347 Uiso 1.0 4 calc R . . H22 H 0.7315 -0.2326 0.7105 0.0325 Uiso 1.0 4 calc R . . H23 H 0.8530 -0.1601 0.7557 0.0270 Uiso 1.0 4 calc R . . H24 H 0.7700 -0.0786 0.7993 0.0217 Uiso 1.0 4 calc R . . H32 H 0.2836 0.1263 0.7533 0.0202 Uiso 1.0 4 calc R . . H33 H 0.1343 0.1122 0.6581 0.0261 Uiso 1.0 4 calc R . . H37 H 0.4879 0.1085 0.4061 0.0299 Uiso 1.0 4 calc R . . H38 H 0.6474 0.1268 0.4921 0.0242 Uiso 1.0 4 calc R . . H41A H 0.1097 0.1275 0.4922 0.0396 Uiso 1.0 4 calc R . . H41B H 0.1258 0.0615 0.5067 0.0396 Uiso 1.0 4 calc R . . H42A H 0.2536 0.0573 0.4192 0.0371 Uiso 1.0 4 calc R . . H42B H 0.2347 0.1229 0.4030 0.0371 Uiso 1.0 4 calc R . . H44 H 0.4532 0.2124 0.9216 0.0383 Uiso 1.0 4 calc R . . H45 H 0.3624 0.2958 0.9478 0.0572 Uiso 1.0 4 calc R . . H46 H 0.2923 0.3555 0.8521 0.0475 Uiso 1.0 4 calc R . . H47 H 0.3202 0.3341 0.7283 0.0427 Uiso 1.0 4 calc R . . H48 H 0.4150 0.2513 0.7007 0.0333 Uiso 1.0 4 calc R . . H50 H 0.5681 0.2429 0.5807 0.0289 Uiso 1.0 4 calc R . . H51 H 0.5832 0.3343 0.5360 0.0377 Uiso 1.0 4 calc R . . H52 H 0.7655 0.3715 0.5238 0.0409 Uiso 1.0 4 calc R . . H53 H 0.9322 0.3200 0.5592 0.0381 Uiso 1.0 4 calc R . . H54 H 0.9170 0.2299 0.6062 0.0303 Uiso 1.0 4 calc R . . H55 H 0.9224 0.1026 0.7671 0.0322 Uiso 1.0 4 calc R . . H56A H 1.0745 0.2146 0.8618 0.0268 Uiso 1.0 4 calc R . . H56B H 1.1646 0.1927 0.8059 0.0268 Uiso 1.0 4 calc R . . H56C H 1.1797 0.1751 0.8921 0.0268 Uiso 1.0 4 calc R . . H57A H 1.0810 0.0529 0.8539 0.0468 Uiso 1.0 4 calc R . . H57B H 0.9953 0.0812 0.9080 0.0468 Uiso 1.0 4 calc R . . H57C H 1.1314 0.0932 0.9200 0.0468 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te1 0.01015(16) 0.01589(18) 0.01084(15) -0.00134(13) 0.00060(12) -0.00009(12) Te2 0.00811(15) 0.01375(18) 0.01193(15) 0.00008(12) 0.00052(12) -0.00090(11) Te3 0.01530(17) 0.01823(19) 0.01175(15) -0.00310(13) 0.00235(13) -0.00059(12) Te4 0.01289(16) 0.02084(19) 0.01367(15) -0.00353(13) 0.00121(13) 0.00250(12) Br1 0.0150(3) 0.0231(3) 0.0159(3) 0.0015(2) 0.00284(19) -0.00338(19) Br2 0.0179(3) 0.0207(3) 0.0261(3) -0.0007(2) 0.0049(2) 0.0055(2) Br3 0.0174(3) 0.0164(3) 0.0171(3) -0.0003(2) 0.00526(19) -0.00097(19) Br4 0.0226(3) 0.0362(4) 0.0277(3) 0.0072(3) 0.0079(3) 0.0010(3) O1 0.0147(17) 0.0185(19) 0.0132(15) 0.0042(14) 0.0051(13) 0.0015(13) O2 0.0222(19) 0.022(2) 0.0168(16) -0.0079(15) 0.0091(14) -0.0045(14) O3 0.039(3) 0.029(3) 0.032(2) -0.0023(19) -0.0177(18) 0.0045(17) N1 0.017(3) 0.019(3) 0.026(3) 0.0033(19) -0.0008(19) 0.0030(18) C1 0.010(3) 0.017(3) 0.012(3) -0.001(2) -0.0028(19) -0.0033(19) C2 0.013(3) 0.024(3) 0.015(3) -0.002(3) 0.003(2) -0.005(2) C3 0.009(3) 0.040(4) 0.021(3) -0.002(3) 0.005(2) -0.009(3) C4 0.009(3) 0.023(3) 0.022(3) 0.000(2) -0.002(2) -0.006(2) C5 0.014(3) 0.011(3) 0.015(3) 0.001(2) -0.002(2) -0.0010(18) C6 0.015(3) 0.018(3) 0.015(3) 0.002(3) -0.002(2) -0.0021(19) C7 0.020(3) 0.019(3) 0.010(3) -0.001(3) -0.003(2) 0.0039(19) C8 0.013(3) 0.015(3) 0.022(3) 0.002(2) 0.003(2) -0.002(2) C9 0.009(3) 0.006(3) 0.015(3) 0.0013(19) -0.0003(19) 0.0002(17) C10 0.017(3) 0.008(3) 0.016(3) -0.004(2) -0.000(2) -0.0035(18) C11 0.016(3) 0.045(4) 0.018(3) -0.005(3) -0.001(3) -0.007(3) C12 0.012(3) 0.040(4) 0.018(3) 0.002(3) -0.003(2) -0.007(3) C13 0.014(3) 0.020(3) 0.021(3) -0.004(2) -0.002(2) 0.003(2) C14 0.022(3) 0.027(4) 0.019(3) 0.002(3) 0.004(3) 0.003(3) C15 0.031(4) 0.028(4) 0.031(3) 0.000(3) 0.012(3) 0.016(3) C16 0.036(4) 0.022(4) 0.048(4) -0.011(3) 0.009(3) 0.007(3) C17 0.055(4) 0.019(4) 0.036(3) -0.015(3) 0.010(3) -0.004(3) C18 0.038(4) 0.021(4) 0.027(3) -0.010(3) 0.010(3) -0.003(3) C19 0.016(3) 0.016(3) 0.007(2) 0.004(2) 0.0037(19) -0.0008(18) C20 0.019(3) 0.020(3) 0.022(3) -0.001(3) -0.005(3) -0.001(2) C21 0.041(4) 0.018(4) 0.026(3) -0.005(3) -0.007(3) -0.002(3) C22 0.040(4) 0.020(4) 0.021(3) 0.013(3) 0.003(3) -0.004(3) C23 0.021(3) 0.031(4) 0.017(3) 0.009(3) 0.006(3) -0.000(3) C24 0.014(3) 0.023(3) 0.017(3) -0.000(3) 0.000(2) 0.001(2) C31 0.017(3) 0.018(3) 0.016(3) -0.002(2) -0.001(2) -0.0005(19) C32 0.019(3) 0.016(3) 0.016(3) 0.002(3) 0.004(2) 0.000(2) C33 0.013(3) 0.022(3) 0.031(3) 0.000(3) 0.005(3) 0.003(3) C34 0.015(3) 0.021(3) 0.022(3) -0.004(3) -0.002(3) 0.008(2) C35 0.016(3) 0.018(3) 0.014(3) 0.000(3) -0.000(2) -0.002(2) C36 0.019(3) 0.026(4) 0.017(3) -0.004(3) -0.004(3) -0.000(2) C37 0.027(3) 0.040(4) 0.008(3) -0.001(3) 0.002(3) 0.001(3) C38 0.014(3) 0.029(4) 0.019(3) -0.002(3) 0.009(2) -0.002(2) C39 0.013(3) 0.018(3) 0.015(3) 0.002(2) -0.001(2) -0.0008(19) C40 0.013(3) 0.016(3) 0.014(3) -0.003(2) 0.001(2) 0.0008(19) C41 0.020(3) 0.052(5) 0.026(3) -0.003(3) -0.004(3) 0.009(3) C42 0.027(3) 0.047(4) 0.017(3) -0.009(3) -0.007(3) 0.003(3) C43 0.020(3) 0.013(3) 0.026(3) -0.006(3) 0.010(3) -0.001(2) C44 0.049(4) 0.030(4) 0.018(3) 0.003(3) 0.011(3) -0.005(3) C45 0.089(6) 0.025(4) 0.033(3) -0.004(4) 0.029(4) -0.007(3) C46 0.066(5) 0.013(4) 0.043(4) -0.000(3) 0.022(3) -0.005(3) C47 0.048(4) 0.022(4) 0.039(3) 0.007(3) 0.014(3) 0.006(3) C48 0.037(4) 0.024(4) 0.023(3) 0.000(3) 0.006(3) -0.001(3) C49 0.026(3) 0.019(3) 0.013(3) -0.002(3) 0.003(2) 0.001(2) C50 0.026(3) 0.025(4) 0.021(3) -0.005(3) 0.002(3) 0.003(3) C51 0.044(4) 0.027(4) 0.024(3) 0.001(3) 0.008(3) 0.002(3) C52 0.060(5) 0.022(4) 0.021(3) -0.006(3) 0.012(3) 0.001(3) C53 0.048(4) 0.034(4) 0.015(3) -0.021(3) 0.013(3) -0.000(3) C54 0.027(3) 0.037(4) 0.012(3) -0.012(3) 0.004(3) -0.003(3) C55 0.019(3) 0.032(4) 0.029(3) -0.001(3) 0.001(3) -0.009(3) C56 0.015(3) 0.024(4) 0.028(3) 0.003(3) 0.002(3) -0.000(3) C57 0.028(4) 0.039(4) 0.049(4) -0.004(3) -0.003(3) 0.015(3) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 rc13' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc13' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Te1 Br1 2.8261(7) yes . . Te1 O1 2.005(3) yes . . Te1 C1 2.137(4) yes . . Te1 C13 2.140(5) yes . . Te2 Br2 2.8862(7) yes . . Te2 O1 1.992(3) yes . . Te2 C9 2.135(4) yes . . Te2 C19 2.113(5) yes . . Te3 O2 1.942(3) yes . . Te3 C31 2.131(5) yes . . Te3 C43 2.114(5) yes . . Te4 Br4 2.7654(7) yes . . Te4 O2 2.045(3) yes . . Te4 C39 2.146(5) yes . . Te4 C49 2.128(5) yes . . O3 C55 1.227(7) yes . . N1 C55 1.341(6) yes . . N1 C56 1.455(7) yes . . N1 C57 1.455(7) yes . . C1 C2 1.380(7) yes . . C1 C10 1.444(6) yes . . C2 C3 1.407(6) yes . . C3 C4 1.362(7) yes . . C4 C5 1.406(7) yes . . C4 C11 1.516(6) yes . . C5 C6 1.416(6) yes . . C5 C10 1.420(6) yes . . C6 C7 1.355(7) yes . . C6 C12 1.518(6) yes . . C7 C8 1.415(6) yes . . C8 C9 1.379(6) yes . . C9 C10 1.434(6) yes . . C11 C12 1.528(7) yes . . C13 C14 1.381(7) yes . . C13 C18 1.388(7) yes . . C14 C15 1.382(8) yes . . C15 C16 1.385(8) yes . . C16 C17 1.375(8) yes . . C17 C18 1.388(8) yes . . C19 C20 1.375(7) yes . . C19 C24 1.382(7) yes . . C20 C21 1.392(7) yes . . C21 C22 1.389(8) yes . . C22 C23 1.382(7) yes . . C23 C24 1.385(7) yes . . C31 C32 1.383(7) yes . . C31 C40 1.427(6) yes . . C32 C33 1.407(6) yes . . C33 C34 1.359(7) yes . . C34 C35 1.411(7) yes . . C34 C41 1.520(7) yes . . C35 C36 1.429(6) yes . . C35 C40 1.420(6) yes . . C36 C37 1.361(7) yes . . C36 C42 1.512(7) yes . . C37 C38 1.409(7) yes . . C38 C39 1.382(6) yes . . C39 C40 1.451(7) yes . . C41 C42 1.556(7) yes . . C43 C44 1.393(7) yes . . C43 C48 1.395(7) yes . . C44 C45 1.376(9) yes . . C45 C46 1.386(8) yes . . C46 C47 1.382(8) yes . . C47 C48 1.389(8) yes . . C49 C50 1.371(7) yes . . C49 C54 1.387(7) yes . . C50 C51 1.385(8) yes . . C51 C52 1.372(9) yes . . C52 C53 1.392(8) yes . . C53 C54 1.372(8) yes . . C2 H2 0.950 no . . C3 H3 0.950 no . . C7 H7 0.950 no . . C8 H8 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C14 H14 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C32 H32 0.950 no . . C33 H33 0.950 no . . C37 H37 0.950 no . . C38 H38 0.950 no . . C41 H41A 0.990 no . . C41 H41B 0.990 no . . C42 H42A 0.990 no . . C42 H42B 0.990 no . . C44 H44 0.950 no . . C45 H45 0.950 no . . C46 H46 0.950 no . . C47 H47 0.950 no . . C48 H48 0.950 no . . C50 H50 0.950 no . . C51 H51 0.950 no . . C52 H52 0.950 no . . C53 H53 0.950 no . . C54 H54 0.950 no . . C55 H55 0.950 no . . C56 H56A 0.980 no . . C56 H56B 0.980 no . . C56 H56C 0.980 no . . C57 H57A 0.980 no . . C57 H57B 0.980 no . . C57 H57C 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br1 Te1 O1 176.46(8) yes . . . Br1 Te1 C1 90.16(12) yes . . . Br1 Te1 C13 91.35(13) yes . . . O1 Te1 C1 86.32(14) yes . . . O1 Te1 C13 89.08(16) yes . . . C1 Te1 C13 92.36(17) yes . . . Br2 Te2 O1 172.52(9) yes . . . Br2 Te2 C9 93.99(12) yes . . . Br2 Te2 C19 84.78(12) yes . . . O1 Te2 C9 88.69(14) yes . . . O1 Te2 C19 87.99(15) yes . . . C9 Te2 C19 96.49(16) yes . . . O2 Te3 C31 89.80(15) yes . . . O2 Te3 C43 89.46(16) yes . . . C31 Te3 C43 94.25(18) yes . . . Br4 Te4 O2 175.41(9) yes . . . Br4 Te4 C39 93.79(13) yes . . . Br4 Te4 C49 91.45(13) yes . . . O2 Te4 C39 87.45(15) yes . . . O2 Te4 C49 84.05(15) yes . . . C39 Te4 C49 94.18(18) yes . . . Te1 O1 Te2 113.11(15) yes . . . Te3 O2 Te4 116.17(16) yes . . . C55 N1 C56 120.2(4) yes . . . C55 N1 C57 121.3(5) yes . . . C56 N1 C57 118.2(4) yes . . . Te1 C1 C2 115.2(3) yes . . . Te1 C1 C10 124.0(3) yes . . . C2 C1 C10 120.7(4) yes . . . C1 C2 C3 123.2(4) yes . . . C2 C3 C4 118.4(5) yes . . . C3 C4 C5 119.0(4) yes . . . C3 C4 C11 130.9(5) yes . . . C5 C4 C11 110.0(4) yes . . . C4 C5 C6 111.1(4) yes . . . C4 C5 C10 125.4(4) yes . . . C6 C5 C10 123.5(4) yes . . . C5 C6 C7 120.1(4) yes . . . C5 C6 C12 108.2(4) yes . . . C7 C6 C12 131.8(4) yes . . . C6 C7 C8 118.2(4) yes . . . C7 C8 C9 122.9(5) yes . . . Te2 C9 C8 116.4(3) yes . . . Te2 C9 C10 122.9(3) yes . . . C8 C9 C10 120.6(4) yes . . . C1 C10 C5 113.2(4) yes . . . C1 C10 C9 132.1(4) yes . . . C5 C10 C9 114.7(4) yes . . . C4 C11 C12 104.1(4) yes . . . C6 C12 C11 106.3(4) yes . . . Te1 C13 C14 121.5(4) yes . . . Te1 C13 C18 118.1(4) yes . . . C14 C13 C18 120.3(5) yes . . . C13 C14 C15 119.0(5) yes . . . C14 C15 C16 121.4(5) yes . . . C15 C16 C17 119.1(6) yes . . . C16 C17 C18 120.5(5) yes . . . C13 C18 C17 119.7(5) yes . . . Te2 C19 C20 120.2(4) yes . . . Te2 C19 C24 118.1(4) yes . . . C20 C19 C24 121.3(5) yes . . . C19 C20 C21 118.5(5) yes . . . C20 C21 C22 120.1(5) yes . . . C21 C22 C23 121.1(5) yes . . . C22 C23 C24 118.4(5) yes . . . C19 C24 C23 120.6(5) yes . . . Te3 C31 C32 115.6(3) yes . . . Te3 C31 C40 123.2(4) yes . . . C32 C31 C40 121.1(4) yes . . . C31 C32 C33 123.4(4) yes . . . C32 C33 C34 117.7(5) yes . . . C33 C34 C35 119.5(4) yes . . . C33 C34 C41 130.8(5) yes . . . C35 C34 C41 109.7(4) yes . . . C34 C35 C36 111.0(4) yes . . . C34 C35 C40 125.0(4) yes . . . C36 C35 C40 124.0(4) yes . . . C35 C36 C37 119.5(4) yes . . . C35 C36 C42 109.3(4) yes . . . C37 C36 C42 131.3(4) yes . . . C36 C37 C38 118.4(4) yes . . . C37 C38 C39 123.5(5) yes . . . Te4 C39 C38 114.9(4) yes . . . Te4 C39 C40 124.6(3) yes . . . C38 C39 C40 120.3(4) yes . . . C31 C40 C35 113.3(4) yes . . . C31 C40 C39 132.3(4) yes . . . C35 C40 C39 114.3(4) yes . . . C34 C41 C42 104.8(4) yes . . . C36 C42 C41 105.2(4) yes . . . Te3 C43 C44 120.0(4) yes . . . Te3 C43 C48 119.5(4) yes . . . C44 C43 C48 120.5(5) yes . . . C43 C44 C45 118.8(5) yes . . . C44 C45 C46 121.3(5) yes . . . C45 C46 C47 120.0(6) yes . . . C46 C47 C48 119.7(5) yes . . . C43 C48 C47 119.8(5) yes . . . Te4 C49 C50 118.4(4) yes . . . Te4 C49 C54 119.8(4) yes . . . C50 C49 C54 121.4(5) yes . . . C49 C50 C51 120.1(5) yes . . . C50 C51 C52 118.8(5) yes . . . C51 C52 C53 121.1(5) yes . . . C52 C53 C54 120.1(6) yes . . . C49 C54 C53 118.5(5) yes . . . O3 C55 N1 124.5(5) yes . . . C1 C2 H2 118.386 no . . . C3 C2 H2 118.376 no . . . C2 C3 H3 120.820 no . . . C4 C3 H3 120.823 no . . . C6 C7 H7 120.913 no . . . C8 C7 H7 120.922 no . . . C7 C8 H8 118.529 no . . . C9 C8 H8 118.537 no . . . C4 C11 H11A 110.937 no . . . C4 C11 H11B 110.937 no . . . C12 C11 H11A 110.930 no . . . C12 C11 H11B 110.942 no . . . H11A C11 H11B 108.952 no . . . C6 C12 H12A 110.457 no . . . C6 C12 H12B 110.475 no . . . C11 C12 H12A 110.467 no . . . C11 C12 H12B 110.482 no . . . H12A C12 H12B 108.658 no . . . C13 C14 H14 120.521 no . . . C15 C14 H14 120.523 no . . . C14 C15 H15 119.282 no . . . C16 C15 H15 119.278 no . . . C15 C16 H16 120.472 no . . . C17 C16 H16 120.470 no . . . C16 C17 H17 119.776 no . . . C18 C17 H17 119.761 no . . . C13 C18 H18 120.127 no . . . C17 C18 H18 120.127 no . . . C19 C20 H20 120.741 no . . . C21 C20 H20 120.718 no . . . C20 C21 H21 119.956 no . . . C22 C21 H21 119.951 no . . . C21 C22 H22 119.466 no . . . C23 C22 H22 119.459 no . . . C22 C23 H23 120.799 no . . . C24 C23 H23 120.800 no . . . C19 C24 H24 119.708 no . . . C23 C24 H24 119.726 no . . . C31 C32 H32 118.293 no . . . C33 C32 H32 118.298 no . . . C32 C33 H33 121.165 no . . . C34 C33 H33 121.182 no . . . C36 C37 H37 120.785 no . . . C38 C37 H37 120.791 no . . . C37 C38 H38 118.265 no . . . C39 C38 H38 118.278 no . . . C34 C41 H41A 110.801 no . . . C34 C41 H41B 110.796 no . . . C42 C41 H41A 110.786 no . . . C42 C41 H41B 110.794 no . . . H41A C41 H41B 108.862 no . . . C36 C42 H42A 110.700 no . . . C36 C42 H42B 110.693 no . . . C41 C42 H42A 110.709 no . . . C41 C42 H42B 110.697 no . . . H42A C42 H42B 108.807 no . . . C43 C44 H44 120.589 no . . . C45 C44 H44 120.605 no . . . C44 C45 H45 119.377 no . . . C46 C45 H45 119.366 no . . . C45 C46 H46 120.017 no . . . C47 C46 H46 120.009 no . . . C46 C47 H47 120.154 no . . . C48 C47 H47 120.143 no . . . C43 C48 H48 120.106 no . . . C47 C48 H48 120.103 no . . . C49 C50 H50 119.954 no . . . C51 C50 H50 119.943 no . . . C50 C51 H51 120.624 no . . . C52 C51 H51 120.599 no . . . C51 C52 H52 119.461 no . . . C53 C52 H52 119.466 no . . . C52 C53 H53 119.966 no . . . C54 C53 H53 119.946 no . . . C49 C54 H54 120.733 no . . . C53 C54 H54 120.723 no . . . O3 C55 H55 117.762 no . . . N1 C55 H55 117.764 no . . . N1 C56 H56A 109.476 no . . . N1 C56 H56B 109.468 no . . . N1 C56 H56C 109.470 no . . . H56A C56 H56B 109.474 no . . . H56A C56 H56C 109.472 no . . . H56B C56 H56C 109.467 no . . . N1 C57 H57A 109.465 no . . . N1 C57 H57B 109.485 no . . . N1 C57 H57C 109.474 no . . . H57A C57 H57B 109.462 no . . . H57A C57 H57C 109.468 no . . . H57B C57 H57C 109.475 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br1 Te1 C1 C2 -38.7(3) no . . . . Br1 Te1 C1 C10 144.2(3) no . . . . Br1 Te1 C13 C14 -25.6(3) no . . . . Br1 Te1 C13 C18 152.6(3) no . . . . O1 Te1 C1 C2 141.5(3) no . . . . O1 Te1 C1 C10 -35.5(3) no . . . . C1 Te1 O1 Te2 77.22(17) no . . . . O1 Te1 C13 C14 157.9(3) no . . . . O1 Te1 C13 C18 -23.9(3) no . . . . C13 Te1 O1 Te2 169.64(17) no . . . . C1 Te1 C13 C14 -115.8(3) no . . . . C1 Te1 C13 C18 62.4(3) no . . . . C13 Te1 C1 C2 52.6(3) no . . . . C13 Te1 C1 C10 -124.5(4) no . . . . Br2 Te2 C9 C8 26.9(3) no . . . . Br2 Te2 C9 C10 -157.4(3) no . . . . Br2 Te2 C19 C20 -128.7(3) no . . . . Br2 Te2 C19 C24 58.2(3) no . . . . O1 Te2 C9 C8 -146.1(3) no . . . . O1 Te2 C9 C10 29.6(3) no . . . . C9 Te2 O1 Te1 -75.67(16) no . . . . O1 Te2 C19 C20 53.2(3) no . . . . O1 Te2 C19 C24 -119.9(3) no . . . . C19 Te2 O1 Te1 -172.21(16) no . . . . C9 Te2 C19 C20 -35.3(3) no . . . . C9 Te2 C19 C24 151.6(3) no . . . . C19 Te2 C9 C8 -58.3(3) no . . . . C19 Te2 C9 C10 117.4(3) no . . . . O2 Te3 C31 C32 -145.9(3) no . . . . O2 Te3 C31 C40 30.1(4) no . . . . C31 Te3 O2 Te4 -73.23(18) no . . . . O2 Te3 C43 C44 -131.7(3) no . . . . O2 Te3 C43 C48 45.1(3) no . . . . C43 Te3 O2 Te4 -167.48(18) no . . . . C31 Te3 C43 C44 138.6(4) no . . . . C31 Te3 C43 C48 -44.6(4) no . . . . C43 Te3 C31 C32 -56.4(4) no . . . . C43 Te3 C31 C40 119.5(4) no . . . . Br4 Te4 C39 C38 -27.9(3) no . . . . Br4 Te4 C39 C40 155.3(3) no . . . . Br4 Te4 C49 C50 130.0(3) no . . . . Br4 Te4 C49 C54 -57.4(3) no . . . . O2 Te4 C39 C38 147.7(3) no . . . . O2 Te4 C39 C40 -29.1(4) no . . . . C39 Te4 O2 Te3 72.56(18) no . . . . O2 Te4 C49 C50 -50.9(3) no . . . . O2 Te4 C49 C54 121.7(3) no . . . . C49 Te4 O2 Te3 167.03(18) no . . . . C39 Te4 C49 C50 36.1(3) no . . . . C39 Te4 C49 C54 -151.3(3) no . . . . C49 Te4 C39 C38 63.8(3) no . . . . C49 Te4 C39 C40 -112.9(4) no . . . . C56 N1 C55 O3 -0.2(8) no . . . . C57 N1 C55 O3 173.6(5) no . . . . Te1 C1 C2 C3 -178.4(3) no . . . . Te1 C1 C10 C5 179.8(3) no . . . . Te1 C1 C10 C9 1.1(7) no . . . . C2 C1 C10 C5 2.8(6) no . . . . C2 C1 C10 C9 -175.8(4) no . . . . C10 C1 C2 C3 -1.2(7) no . . . . C1 C2 C3 C4 -1.4(7) no . . . . C2 C3 C4 C5 2.0(7) no . . . . C2 C3 C4 C11 179.9(4) no . . . . C3 C4 C5 C6 178.0(4) no . . . . C3 C4 C5 C10 -0.1(7) no . . . . C3 C4 C11 C12 178.7(5) no . . . . C5 C4 C11 C12 -3.3(5) no . . . . C11 C4 C5 C6 -0.2(6) no . . . . C11 C4 C5 C10 -178.4(4) no . . . . C4 C5 C6 C7 -176.1(4) no . . . . C4 C5 C6 C12 3.8(5) no . . . . C4 C5 C10 C1 -2.3(7) no . . . . C4 C5 C10 C9 176.6(4) no . . . . C6 C5 C10 C1 179.8(4) no . . . . C6 C5 C10 C9 -1.3(6) no . . . . C10 C5 C6 C7 2.1(7) no . . . . C10 C5 C6 C12 -178.0(4) no . . . . C5 C6 C7 C8 -1.2(7) no . . . . C5 C6 C12 C11 -5.7(5) no . . . . C7 C6 C12 C11 174.1(5) no . . . . C12 C6 C7 C8 179.0(5) no . . . . C6 C7 C8 C9 -0.4(7) no . . . . C7 C8 C9 Te2 177.0(4) no . . . . C7 C8 C9 C10 1.2(7) no . . . . Te2 C9 C10 C1 2.8(7) no . . . . Te2 C9 C10 C5 -175.9(3) no . . . . C8 C9 C10 C1 178.3(4) no . . . . C8 C9 C10 C5 -0.3(6) no . . . . C4 C11 C12 C6 5.3(5) no . . . . Te1 C13 C14 C15 177.8(3) no . . . . Te1 C13 C18 C17 -178.5(3) no . . . . C14 C13 C18 C17 -0.3(7) no . . . . C18 C13 C14 C15 -0.4(7) no . . . . C13 C14 C15 C16 0.8(7) no . . . . C14 C15 C16 C17 -0.6(8) no . . . . C15 C16 C17 C18 -0.1(8) no . . . . C16 C17 C18 C13 0.6(8) no . . . . Te2 C19 C20 C21 -172.3(3) no . . . . Te2 C19 C24 C23 172.1(3) no . . . . C20 C19 C24 C23 -1.0(6) no . . . . C24 C19 C20 C21 0.6(6) no . . . . C19 C20 C21 C22 0.3(7) no . . . . C20 C21 C22 C23 -0.8(7) no . . . . C21 C22 C23 C24 0.4(7) no . . . . C22 C23 C24 C19 0.4(6) no . . . . Te3 C31 C32 C33 174.3(3) no . . . . Te3 C31 C40 C35 -175.7(3) no . . . . Te3 C31 C40 C39 3.4(7) no . . . . C32 C31 C40 C35 0.1(7) no . . . . C32 C31 C40 C39 179.2(4) no . . . . C40 C31 C32 C33 -1.7(7) no . . . . C31 C32 C33 C34 2.1(7) no . . . . C32 C33 C34 C35 -0.8(7) no . . . . C32 C33 C34 C41 177.4(4) no . . . . C33 C34 C35 C36 179.3(4) no . . . . C33 C34 C35 C40 -0.8(7) no . . . . C33 C34 C41 C42 -177.8(5) no . . . . C35 C34 C41 C42 0.5(6) no . . . . C41 C34 C35 C36 0.7(6) no . . . . C41 C34 C35 C40 -179.4(4) no . . . . C34 C35 C36 C37 177.4(4) no . . . . C34 C35 C36 C42 -1.8(6) no . . . . C34 C35 C40 C31 1.2(7) no . . . . C34 C35 C40 C39 -178.1(4) no . . . . C36 C35 C40 C31 -178.9(4) no . . . . C36 C35 C40 C39 1.8(7) no . . . . C40 C35 C36 C37 -2.5(7) no . . . . C40 C35 C36 C42 178.3(4) no . . . . C35 C36 C37 C38 1.6(7) no . . . . C35 C36 C42 C41 2.0(6) no . . . . C37 C36 C42 C41 -177.1(5) no . . . . C42 C36 C37 C38 -179.4(5) no . . . . C36 C37 C38 C39 -0.4(8) no . . . . C37 C38 C39 Te4 -177.1(4) no . . . . C37 C38 C39 C40 -0.2(8) no . . . . Te4 C39 C40 C31 -3.0(7) no . . . . Te4 C39 C40 C35 176.1(3) no . . . . C38 C39 C40 C31 -179.6(5) no . . . . C38 C39 C40 C35 -0.5(7) no . . . . C34 C41 C42 C36 -1.5(6) no . . . . Te3 C43 C44 C45 176.7(3) no . . . . Te3 C43 C48 C47 -177.5(3) no . . . . C44 C43 C48 C47 -0.7(7) no . . . . C48 C43 C44 C45 -0.0(8) no . . . . C43 C44 C45 C46 1.1(9) no . . . . C44 C45 C46 C47 -1.5(9) no . . . . C45 C46 C47 C48 0.7(9) no . . . . C46 C47 C48 C43 0.3(8) no . . . . Te4 C49 C50 C51 172.5(3) no . . . . Te4 C49 C54 C53 -173.2(3) no . . . . C50 C49 C54 C53 -0.8(7) no . . . . C54 C49 C50 C51 0.0(7) no . . . . C49 C50 C51 C52 0.9(7) no . . . . C50 C51 C52 C53 -1.1(7) no . . . . C51 C52 C53 C54 0.3(7) no . . . . C52 C53 C54 C49 0.6(7) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br1 C2 3.393(5) no . . Br1 C14 3.457(6) no . . Br2 C8 3.488(5) no . . Br2 C24 3.508(5) no . . Br4 C38 3.398(5) no . . O1 C10 3.077(5) no . . O1 C18 2.942(6) no . . O1 C20 3.167(6) no . . O2 C40 3.103(5) no . . O2 C48 3.108(6) no . . O2 C50 3.015(6) no . . O3 C56 2.779(6) no . . O3 C57 3.587(7) no . . C1 C4 2.811(6) no . . C1 C18 3.455(7) no . . C2 C5 2.712(6) no . . C2 C13 3.287(7) no . . C3 C6 3.598(7) no . . C3 C10 2.890(7) no . . C4 C7 3.596(7) no . . C5 C8 2.732(7) no . . C6 C9 2.804(6) no . . C7 C10 2.879(6) no . . C8 C19 3.483(6) no . . C8 C20 3.534(7) no . . C9 C20 3.329(7) no . . C13 C16 2.774(8) no . . C14 C17 2.774(8) no . . C15 C18 2.751(8) no . . C19 C22 2.745(7) no . . C20 C23 2.801(7) no . . C21 C24 2.758(7) no . . C31 C34 2.800(6) no . . C31 C48 3.328(7) no . . C32 C35 2.706(6) no . . C32 C43 3.380(7) no . . C32 C48 3.548(7) no . . C33 C40 2.894(7) no . . C35 C38 2.735(7) no . . C36 C39 2.819(6) no . . C37 C40 2.892(6) no . . C38 C49 3.470(7) no . . C38 C50 3.529(7) no . . C39 C50 3.238(7) no . . C43 C46 2.767(8) no . . C44 C47 2.791(8) no . . C45 C48 2.763(8) no . . C49 C52 2.733(8) no . . C50 C53 2.757(8) no . . C51 C54 2.788(8) no . . Te1 Br3 3.5404(9) no . . Te2 Br3 3.4380(8) no . . Te3 Br2 3.4021(8) no . . Te3 Br3 3.0244(7) no . . Te4 Br2 3.3242(8) no . . Te4 O3 2.950(4) no . . Te4 C55 3.494(5) no . . Br2 Te3 3.4021(8) no . . Br2 Te4 3.3242(8) no . . Br3 Te1 3.5404(9) no . . Br3 Te2 3.4380(8) no . . Br3 Te3 3.0244(7) no . . O1 C53 3.369(7) no . 2_646 O2 C22 3.345(6) no . 2_656 O3 Te4 2.950(4) no . . O3 C21 3.194(7) no . 2_656 O3 C22 3.503(7) no . 2_656 O3 C49 3.527(6) no . . O3 C54 3.274(6) no . . C2 C57 3.456(8) no . 1_455 C3 C57 3.588(8) no . 1_455 C6 C33 3.472(7) no . . C6 C46 3.574(8) no . 2_546 C7 C33 3.401(7) no . . C7 C34 3.375(7) no . . C11 C42 3.537(7) no . 3_556 C19 C53 3.564(7) no . 2_646 C21 O3 3.194(7) no . 2_646 C21 C54 3.558(7) no . 2_646 C22 O2 3.345(6) no . 2_646 C22 O3 3.503(7) no . 2_646 C22 C54 3.550(7) no . 2_646 C24 C52 3.435(7) no . 2_646 C33 C6 3.472(7) no . . C33 C7 3.401(7) no . . C34 C7 3.375(7) no . . C42 C11 3.537(7) no . 3_556 C44 C53 3.567(7) no . 4_455 C46 C6 3.574(8) no . 2_556 C49 O3 3.527(6) no . . C51 C56 3.586(7) no . 4_454 C52 C24 3.435(7) no . 2_656 C53 O1 3.369(7) no . 2_656 C53 C19 3.564(7) no . 2_656 C53 C44 3.567(7) no . 4_554 C54 O3 3.274(6) no . . C54 C21 3.558(7) no . 2_656 C54 C22 3.550(7) no . 2_656 C55 Te4 3.494(5) no . . C56 C51 3.586(7) no . 4_555 C57 C2 3.456(8) no . 1_655 C57 C3 3.588(8) no . 1_655 Te1 H2 2.9537 no . . Te1 H14 3.1485 no . . Te1 H18 3.0642 no . . Te2 H8 2.9840 no . . Te2 H20 3.0984 no . . Te2 H24 3.0355 no . . Te3 H32 2.9632 no . . Te3 H44 3.1036 no . . Te3 H48 3.0860 no . . Te4 H38 2.9529 no . . Te4 H50 3.0473 no . . Te4 H54 3.1088 no . . Br1 H2 2.7910 no . . Br1 H14 2.8324 no . . Br2 H8 2.7699 no . . Br2 H24 3.1108 no . . Br4 H38 2.6889 no . . Br4 H54 3.3377 no . . O1 H18 2.4040 no . . O1 H20 2.9632 no . . O2 H48 2.7818 no . . O2 H50 2.7702 no . . O3 H56A 2.7576 no . . O3 H56B 2.7700 no . . C1 H3 3.3020 no . . C1 H18 3.2277 no . . C3 H11A 2.9282 no . . C3 H11B 2.9410 no . . C4 H2 3.2277 no . . C4 H12A 3.1025 no . . C4 H12B 3.0309 no . . C5 H3 3.2540 no . . C5 H7 3.2676 no . . C5 H11A 3.0742 no . . C5 H11B 3.0339 no . . C5 H12A 3.0723 no . . C5 H12B 3.0014 no . . C6 H8 3.2264 no . . C6 H11A 3.1361 no . . C6 H11B 3.0658 no . . C7 H12A 2.9054 no . . C7 H12B 2.9622 no . . C8 H20 3.1283 no . . C9 H7 3.3055 no . . C9 H20 2.8367 no . . C10 H2 3.3040 no . . C10 H8 3.2938 no . . C10 H20 3.4218 no . . C11 H3 2.8616 no . . C12 H7 2.8719 no . . C13 H2 2.9218 no . . C13 H15 3.2372 no . . C13 H17 3.2575 no . . C14 H2 3.2820 no . . C14 H16 3.2696 no . . C14 H18 3.2588 no . . C15 H17 3.2387 no . . C16 H14 3.2703 no . . C16 H18 3.2542 no . . C17 H15 3.2342 no . . C18 H2 3.5773 no . . C18 H14 3.2622 no . . C18 H16 3.2584 no . . C19 H8 3.1841 no . . C19 H21 3.2387 no . . C19 H23 3.2632 no . . C20 H8 3.4360 no . . C20 H22 3.2636 no . . C20 H24 3.2540 no . . C21 H23 3.2726 no . . C22 H20 3.2709 no . . C22 H24 3.2376 no . . C23 H21 3.2663 no . . C24 H20 3.2614 no . . C24 H22 3.2365 no . . C31 H33 3.3083 no . . C31 H48 2.9227 no . . C32 H48 3.3207 no . . C33 H41A 2.9424 no . . C33 H41B 2.9204 no . . C34 H32 3.2170 no . . C34 H42A 3.0920 no . . C34 H42B 3.1118 no . . C35 H33 3.2621 no . . C35 H37 3.2788 no . . C35 H41A 3.0532 no . . C35 H41B 3.0596 no . . C35 H42A 3.0465 no . . C35 H42B 3.0712 no . . C36 H38 3.2282 no . . C36 H41A 3.0921 no . . C36 H41B 3.1119 no . . C37 H42A 2.9440 no . . C37 H42B 2.9153 no . . C38 H50 3.1365 no . . C39 H37 3.3068 no . . C39 H50 2.7169 no . . C40 H32 3.2924 no . . C40 H38 3.3075 no . . C40 H48 3.4380 no . . C40 H50 3.2160 no . . C41 H33 2.8647 no . . C42 H37 2.8625 no . . C43 H32 3.0871 no . . C43 H45 3.2423 no . . C43 H47 3.2676 no . . C44 H46 3.2601 no . . C44 H48 3.2764 no . . C45 H47 3.2561 no . . C46 H44 3.2651 no . . C46 H48 3.2548 no . . C47 H45 3.2506 no . . C48 H32 3.4978 no . . C48 H44 3.2794 no . . C48 H46 3.2553 no . . C49 H38 3.2107 no . . C49 H51 3.2477 no . . C49 H53 3.2348 no . . C50 H38 3.5125 no . . C50 H52 3.2319 no . . C50 H54 3.2616 no . . C51 H53 3.2591 no . . C52 H50 3.2330 no . . C52 H54 3.2578 no . . C53 H51 3.2659 no . . C54 H50 3.2593 no . . C54 H52 3.2474 no . . C55 H56A 2.6735 no . . C55 H56B 2.6787 no . . C55 H56C 3.2207 no . . C55 H57A 2.6944 no . . C55 H57B 2.6926 no . . C55 H57C 3.2297 no . . C56 H55 3.2758 no . . C56 H57A 3.1595 no . . C56 H57B 3.0921 no . . C56 H57C 2.4971 no . . C57 H55 2.5746 no . . C57 H56A 3.0940 no . . C57 H56B 3.1577 no . . C57 H56C 2.4964 no . . H2 H3 2.3455 no . . H2 H14 3.3822 no . . H3 H11A 2.9727 no . . H3 H11B 2.9976 no . . H7 H8 2.3571 no . . H7 H12A 2.9340 no . . H7 H12B 3.0473 no . . H8 H20 3.2809 no . . H11A H12A 2.7229 no . . H11A H12B 2.2290 no . . H11B H12A 2.2296 no . . H11B H12B 2.7726 no . . H14 H15 2.3297 no . . H15 H16 2.3315 no . . H16 H17 2.3284 no . . H17 H18 2.3363 no . . H18 H20 3.1522 no . . H20 H21 2.3512 no . . H21 H22 2.3311 no . . H22 H23 2.3357 no . . H23 H24 2.3426 no . . H32 H33 2.3489 no . . H32 H48 3.5278 no . . H33 H41A 2.9954 no . . H33 H41B 2.9752 no . . H37 H38 2.3451 no . . H37 H42A 3.0109 no . . H37 H42B 2.9530 no . . H38 H50 3.3733 no . . H41A H42A 2.7793 no . . H41A H42B 2.2571 no . . H41B H42A 2.2573 no . . H41B H42B 2.7657 no . . H44 H45 2.3255 no . . H45 H46 2.3278 no . . H46 H47 2.3343 no . . H47 H48 2.3426 no . . H48 H50 2.9189 no . . H50 H51 2.3428 no . . H51 H52 2.3232 no . . H52 H53 2.3337 no . . H53 H54 2.3317 no . . H55 H56A 3.5585 no . . H55 H56B 3.5607 no . . H55 H57A 2.5938 no . . H55 H57B 2.6481 no . . H55 H57C 3.5069 no . . H56A H57B 3.4475 no . . H56A H57C 3.1399 no . . H56B H57C 3.1902 no . . H56C H57A 3.1940 no . . H56C H57B 3.1348 no . . H56C H57C 2.1122 no . . Te3 H14 3.4616 no . 3_657 Te4 H55 3.2004 no . . Br1 H3 3.0926 no . 3_557 Br1 H24 3.2260 no . 3_657 Br1 H52 3.1368 no . 4_455 Br1 H57B 3.1338 no . 3_657 Br1 H57C 3.2021 no . 1_455 Br2 H11A 3.3340 no . 1_655 Br2 H55 3.5021 no . . Br3 H32 2.9851 no . . Br3 H44 3.1222 no . . Br3 H52 3.1405 no . 4_455 Br3 H56C 3.4140 no . 1_455 Br3 H57C 3.2895 no . 1_455 Br4 H7 3.5011 no . 3_656 Br4 H12A 2.8841 no . 3_656 Br4 H12B 3.0732 no . 1_655 Br4 H33 3.5738 no . 1_655 Br4 H41A 3.2608 no . 1_655 Br4 H41B 3.3847 no . 1_655 Br4 H45 3.1567 no . 4_554 O1 H52 3.4772 no . 2_646 O1 H53 2.6181 no . 2_646 O2 H15 3.5761 no . 3_657 O2 H22 2.6530 no . 2_656 O2 H23 3.5146 no . 2_656 O3 H15 2.9669 no . 3_657 O3 H21 2.6098 no . 2_656 O3 H22 3.1943 no . 2_656 O3 H33 3.1182 no . 1_655 O3 H54 2.6649 no . . N1 H15 3.0772 no . 3_657 N1 H21 3.5900 no . 2_656 N1 H32 3.1618 no . 1_655 N1 H33 3.4039 no . 1_655 C1 H47 3.3964 no . 2_546 C1 H57A 2.9525 no . 1_455 C2 H47 3.4189 no . 2_546 C2 H57A 2.6752 no . 1_455 C3 H23 3.3818 no . 1_455 C3 H24 3.0380 no . 1_455 C3 H47 3.3483 no . 2_546 C3 H57A 2.7247 no . 1_455 C4 H23 3.5906 no . 1_455 C4 H24 3.5430 no . 1_455 C4 H47 3.2283 no . 2_546 C4 H57A 2.9755 no . 1_455 C5 H46 3.1163 no . 2_546 C5 H47 3.1456 no . 2_546 C5 H57A 3.2021 no . 1_455 C6 H33 3.4152 no . . C6 H41B 3.5501 no . . C6 H46 2.8077 no . 2_546 C7 H37 3.4871 no . 3_656 C7 H38 3.5478 no . 3_656 C7 H41B 3.4905 no . . C7 H46 3.0661 no . 2_546 C8 H37 3.1352 no . 3_656 C8 H46 3.5847 no . 2_546 C10 H47 3.2554 no . 2_546 C10 H57A 3.2834 no . 1_455 C11 H23 3.4489 no . 1_455 C11 H24 3.4328 no . 1_455 C11 H41B 3.5073 no . 3_556 C11 H42A 3.0990 no . 3_556 C11 H42B 3.3443 no . 3_556 C12 H33 3.5399 no . . C12 H41A 3.5917 no . 3_556 C12 H41B 3.1550 no . . C12 H41B 3.1126 no . 3_556 C12 H46 3.2742 no . 2_546 C14 H57B 3.1574 no . 3_657 C15 H22 3.0056 no . 4_445 C15 H56A 3.5175 no . 3_657 C15 H57B 3.4932 no . 3_657 C16 H22 3.3129 no . 4_445 C17 H48 3.5413 no . 2_546 C18 H44 3.5964 no . 3_657 C18 H47 3.3866 no . 2_546 C18 H53 3.0545 no . 2_646 C19 H37 3.4249 no . 3_656 C19 H53 3.4712 no . 2_646 C20 H37 2.9881 no . 3_656 C20 H53 3.4635 no . 2_646 C21 H15 3.4236 no . 4_544 C21 H37 3.1898 no . 3_656 C21 H54 3.5127 no . 2_646 C21 H56A 3.1593 no . 2_646 C22 H15 3.1496 no . 4_544 C22 H16 3.4015 no . 4_544 C22 H42B 3.1340 no . 3_656 C23 H3 3.2989 no . 1_655 C23 H11B 3.1498 no . 1_655 C23 H42B 2.9490 no . 3_656 C24 H3 2.9565 no . 1_655 C24 H11B 3.4083 no . 1_655 C24 H42B 3.4071 no . 3_656 C24 H52 3.5352 no . 2_646 C32 H56B 3.0363 no . 1_455 C33 H7 3.5124 no . . C33 H12B 3.3103 no . . C33 H17 3.4019 no . 2_556 C33 H56B 3.5029 no . 1_455 C34 H7 3.1099 no . . C34 H12B 3.4388 no . . C34 H17 3.2061 no . 2_556 C35 H7 3.2923 no . . C35 H16 3.3351 no . 2_556 C35 H17 3.4556 no . 2_556 C36 H16 3.0262 no . 2_556 C37 H8 3.3595 no . 3_656 C37 H16 3.3807 no . 2_556 C38 H7 3.4975 no . 3_656 C41 H7 3.3959 no . . C41 H11B 3.2799 no . 3_556 C41 H12A 3.0168 no . 3_556 C41 H12B 3.2151 no . . C42 H11A 3.4383 no . 3_556 C42 H11B 2.9059 no . 3_556 C42 H16 3.2998 no . 2_556 C43 H56B 3.3049 no . 1_455 C44 H53 3.4567 no . 4_455 C44 H56B 3.3948 no . 1_455 C44 H56C 3.2459 no . 1_455 C45 H56B 3.5818 no . 1_455 C45 H56C 3.4713 no . 1_455 C46 H11B 3.5574 no . 2_556 C46 H12A 3.4347 no . 2_556 C48 H23 3.4208 no . 2_656 C48 H56B 3.4278 no . 1_455 C49 H22 3.5727 no . 2_656 C49 H45 3.1972 no . 4_554 C50 H23 3.5828 no . 2_656 C51 H23 3.5652 no . 2_656 C51 H56A 3.4771 no . 4_454 C51 H56C 2.8964 no . 4_454 C51 H57C 3.2319 no . 4_454 C52 H24 3.5542 no . 2_656 C52 H44 3.4655 no . 4_554 C52 H56C 2.7960 no . 4_454 C52 H57C 3.0759 no . 4_454 C53 H18 3.5416 no . 2_656 C53 H44 2.9016 no . 4_554 C53 H45 3.1801 no . 4_554 C53 H56C 3.5985 no . 4_454 C54 H44 3.4900 no . 4_554 C54 H45 2.8307 no . 4_554 C55 H14 3.4849 no . 3_657 C55 H15 2.8645 no . 3_657 C55 H21 3.3850 no . 2_656 C55 H33 3.0531 no . 1_655 C56 H15 3.4371 no . 3_657 C56 H21 2.9834 no . 2_656 C56 H32 2.9770 no . 1_655 C56 H51 3.4521 no . 4_555 C57 H14 3.5752 no . 3_657 C57 H51 3.3372 no . 4_555 C57 H52 3.4292 no . 4_555 H2 H51 3.3688 no . 2_546 H2 H57A 3.0864 no . 1_455 H2 H57B 3.2137 no . 3_657 H3 Br1 3.0926 no . 3_557 H3 C23 3.2989 no . 1_455 H3 C24 2.9565 no . 1_455 H3 H23 2.9025 no . 1_455 H3 H24 2.1755 no . 1_455 H3 H51 3.4031 no . 2_546 H3 H57A 3.1775 no . 1_455 H7 Br4 3.5011 no . 3_656 H7 C33 3.5124 no . . H7 C34 3.1099 no . . H7 C35 3.2923 no . . H7 C38 3.4975 no . 3_656 H7 C41 3.3959 no . . H7 H37 3.3390 no . 3_656 H7 H38 3.0691 no . 3_656 H7 H41B 2.9783 no . . H7 H42A 3.4827 no . . H7 H46 3.4125 no . 2_546 H8 C37 3.3595 no . 3_656 H8 H37 2.6660 no . 3_656 H11A Br2 3.3340 no . 1_455 H11A C42 3.4383 no . 3_556 H11A H24 3.1733 no . 1_455 H11A H41B 3.5882 no . 3_556 H11A H42A 2.7581 no . 3_556 H11A H42B 3.4060 no . 3_556 H11A H55 3.1971 no . 1_455 H11B C23 3.1498 no . 1_455 H11B C24 3.4083 no . 1_455 H11B C41 3.2799 no . 3_556 H11B C42 2.9059 no . 3_556 H11B C46 3.5574 no . 2_546 H11B H23 2.6903 no . 1_455 H11B H24 3.1643 no . 1_455 H11B H41A 3.1352 no . 3_556 H11B H41B 3.2396 no . 3_556 H11B H42A 2.6933 no . 3_556 H11B H42B 2.5194 no . 3_556 H11B H46 3.5277 no . 2_546 H12A Br4 2.8841 no . 3_656 H12A C41 3.0168 no . 3_556 H12A C46 3.4347 no . 2_546 H12A H12B 3.5621 no . 3_556 H12A H41A 2.7800 no . 3_556 H12A H41B 3.2875 no . . H12A H41B 2.5007 no . 3_556 H12A H42A 3.5505 no . 3_556 H12A H46 2.9416 no . 2_546 H12B Br4 3.0732 no . 1_455 H12B C33 3.3103 no . . H12B C34 3.4388 no . . H12B C41 3.2151 no . . H12B H12A 3.5621 no . 3_556 H12B H33 2.8797 no . . H12B H41B 2.4142 no . . H12B H41B 3.0858 no . 3_556 H14 Te3 3.4616 no . 3_657 H14 C55 3.4849 no . 3_657 H14 C57 3.5752 no . 3_657 H14 H55 3.1915 no . 3_657 H14 H57B 2.7336 no . 3_657 H15 O2 3.5761 no . 3_657 H15 O3 2.9669 no . 3_657 H15 N1 3.0772 no . 3_657 H15 C21 3.4236 no . 4_445 H15 C22 3.1496 no . 4_445 H15 C55 2.8645 no . 3_657 H15 C56 3.4371 no . 3_657 H15 H21 2.9731 no . 4_445 H15 H22 2.4085 no . 4_445 H15 H55 3.2048 no . 3_657 H15 H56A 2.8500 no . 3_657 H15 H57B 3.3340 no . 3_657 H16 C22 3.4015 no . 4_445 H16 C35 3.3351 no . 2_546 H16 C36 3.0262 no . 2_546 H16 C37 3.3807 no . 2_546 H16 C42 3.2998 no . 2_546 H16 H21 3.5963 no . 4_445 H16 H22 3.0191 no . 4_445 H16 H41A 3.4957 no . 2_546 H16 H42B 2.8506 no . 2_546 H16 H50 3.5392 no . 2_546 H17 C33 3.4019 no . 2_546 H17 C34 3.2061 no . 2_546 H17 C35 3.4556 no . 2_546 H17 H41A 3.3111 no . 2_546 H17 H48 3.1145 no . 2_546 H18 C53 3.5416 no . 2_646 H18 H47 2.8903 no . 2_546 H18 H53 2.6645 no . 2_646 H20 H37 3.1109 no . 3_656 H20 H46 3.2303 no . 2_546 H20 H47 3.2234 no . 2_546 H21 O3 2.6098 no . 2_646 H21 N1 3.5900 no . 2_646 H21 C55 3.3850 no . 2_646 H21 C56 2.9834 no . 2_646 H21 H15 2.9731 no . 4_544 H21 H16 3.5963 no . 4_544 H21 H37 3.4258 no . 3_656 H21 H54 3.5349 no . 2_646 H21 H56A 2.2249 no . 2_646 H21 H56B 3.0191 no . 2_646 H22 O2 2.6530 no . 2_646 H22 O3 3.1943 no . 2_646 H22 C15 3.0056 no . 4_544 H22 C16 3.3129 no . 4_544 H22 C49 3.5727 no . 2_646 H22 H15 2.4085 no . 4_544 H22 H16 3.0191 no . 4_544 H22 H42B 3.3716 no . 3_656 H23 O2 3.5146 no . 2_646 H23 C3 3.3818 no . 1_655 H23 C4 3.5906 no . 1_655 H23 C11 3.4489 no . 1_655 H23 C48 3.4208 no . 2_646 H23 C50 3.5828 no . 2_646 H23 C51 3.5652 no . 2_646 H23 H3 2.9025 no . 1_655 H23 H11B 2.6903 no . 1_655 H23 H42B 3.0759 no . 3_656 H23 H48 3.4617 no . 2_646 H24 Br1 3.2260 no . 3_657 H24 C3 3.0380 no . 1_655 H24 C4 3.5430 no . 1_655 H24 C11 3.4328 no . 1_655 H24 C52 3.5542 no . 2_646 H24 H3 2.1755 no . 1_655 H24 H11A 3.1733 no . 1_655 H24 H11B 3.1643 no . 1_655 H24 H52 3.4583 no . 2_646 H32 Br3 2.9851 no . . H32 N1 3.1618 no . 1_455 H32 C56 2.9770 no . 1_455 H32 H56B 2.3580 no . 1_455 H32 H56C 3.0944 no . 1_455 H32 H57A 3.5545 no . 1_455 H33 Br4 3.5738 no . 1_455 H33 O3 3.1182 no . 1_455 H33 N1 3.4039 no . 1_455 H33 C6 3.4152 no . . H33 C12 3.5399 no . . H33 C55 3.0531 no . 1_455 H33 H12B 2.8797 no . . H33 H55 3.2843 no . 1_455 H33 H56B 3.2766 no . 1_455 H37 C7 3.4871 no . 3_656 H37 C8 3.1352 no . 3_656 H37 C19 3.4249 no . 3_656 H37 C20 2.9881 no . 3_656 H37 C21 3.1898 no . 3_656 H37 H7 3.3390 no . 3_656 H37 H8 2.6660 no . 3_656 H37 H20 3.1109 no . 3_656 H37 H21 3.4258 no . 3_656 H38 C7 3.5478 no . 3_656 H38 H7 3.0691 no . 3_656 H38 H45 3.2618 no . 4_554 H38 H46 3.1776 no . 4_554 H41A Br4 3.2608 no . 1_455 H41A C12 3.5917 no . 3_556 H41A H11B 3.1352 no . 3_556 H41A H12A 2.7800 no . 3_556 H41A H16 3.4957 no . 2_556 H41A H17 3.3111 no . 2_556 H41A H45 3.4395 no . 4_454 H41B Br4 3.3847 no . 1_455 H41B C6 3.5501 no . . H41B C7 3.4905 no . . H41B C11 3.5073 no . 3_556 H41B C12 3.1550 no . . H41B C12 3.1126 no . 3_556 H41B H7 2.9783 no . . H41B H11A 3.5882 no . 3_556 H41B H11B 3.2396 no . 3_556 H41B H12A 3.2875 no . . H41B H12A 2.5007 no . 3_556 H41B H12B 2.4142 no . . H41B H12B 3.0858 no . 3_556 H42A C11 3.0990 no . 3_556 H42A H7 3.4827 no . . H42A H11A 2.7581 no . 3_556 H42A H11B 2.6933 no . 3_556 H42A H12A 3.5505 no . 3_556 H42B C11 3.3443 no . 3_556 H42B C22 3.1340 no . 3_656 H42B C23 2.9490 no . 3_656 H42B C24 3.4071 no . 3_656 H42B H11A 3.4060 no . 3_556 H42B H11B 2.5194 no . 3_556 H42B H16 2.8506 no . 2_556 H42B H22 3.3716 no . 3_656 H42B H23 3.0759 no . 3_656 H44 Br3 3.1222 no . . H44 C18 3.5964 no . 3_657 H44 C52 3.4655 no . 4_455 H44 C53 2.9016 no . 4_455 H44 C54 3.4900 no . 4_455 H44 H52 3.5869 no . 4_455 H44 H53 2.6249 no . 4_455 H44 H56C 3.2943 no . 1_455 H45 Br4 3.1567 no . 4_455 H45 C49 3.1972 no . 4_455 H45 C53 3.1801 no . 4_455 H45 C54 2.8307 no . 4_455 H45 H38 3.2618 no . 4_455 H45 H41A 3.4395 no . 4_555 H45 H53 3.4757 no . 4_455 H45 H54 2.9290 no . 4_455 H46 C5 3.1163 no . 2_556 H46 C6 2.8077 no . 2_556 H46 C7 3.0661 no . 2_556 H46 C8 3.5847 no . 2_556 H46 C12 3.2742 no . 2_556 H46 H7 3.4125 no . 2_556 H46 H11B 3.5277 no . 2_556 H46 H12A 2.9416 no . 2_556 H46 H20 3.2303 no . 2_556 H46 H38 3.1776 no . 4_455 H47 C1 3.3964 no . 2_556 H47 C2 3.4189 no . 2_556 H47 C3 3.3483 no . 2_556 H47 C4 3.2283 no . 2_556 H47 C5 3.1456 no . 2_556 H47 C10 3.2554 no . 2_556 H47 C18 3.3866 no . 2_556 H47 H18 2.8903 no . 2_556 H47 H20 3.2234 no . 2_556 H48 C17 3.5413 no . 2_556 H48 H17 3.1145 no . 2_556 H48 H23 3.4617 no . 2_656 H50 H16 3.5392 no . 2_556 H51 C56 3.4521 no . 4_454 H51 C57 3.3372 no . 4_454 H51 H2 3.3688 no . 2_556 H51 H3 3.4031 no . 2_556 H51 H56A 3.3371 no . 4_454 H51 H56C 2.9179 no . 4_454 H51 H57B 3.1662 no . 4_454 H51 H57C 2.8077 no . 4_454 H52 Br1 3.1368 no . 4_554 H52 Br3 3.1405 no . 4_554 H52 O1 3.4772 no . 2_656 H52 C24 3.5352 no . 2_656 H52 C57 3.4292 no . 4_454 H52 H24 3.4583 no . 2_656 H52 H44 3.5869 no . 4_554 H52 H56C 2.7250 no . 4_454 H52 H57C 2.4700 no . 4_454 H53 O1 2.6181 no . 2_656 H53 C18 3.0545 no . 2_656 H53 C19 3.4712 no . 2_656 H53 C20 3.4635 no . 2_656 H53 C44 3.4567 no . 4_554 H53 H18 2.6645 no . 2_656 H53 H44 2.6249 no . 4_554 H53 H45 3.4757 no . 4_554 H54 O3 2.6649 no . . H54 C21 3.5127 no . 2_656 H54 H21 3.5349 no . 2_656 H54 H45 2.9290 no . 4_554 H55 Te4 3.2004 no . . H55 Br2 3.5021 no . . H55 H11A 3.1971 no . 1_655 H55 H14 3.1915 no . 3_657 H55 H15 3.2048 no . 3_657 H55 H33 3.2843 no . 1_655 H56A C15 3.5175 no . 3_657 H56A C21 3.1593 no . 2_656 H56A C51 3.4771 no . 4_555 H56A H15 2.8500 no . 3_657 H56A H21 2.2249 no . 2_656 H56A H51 3.3371 no . 4_555 H56B C32 3.0363 no . 1_655 H56B C33 3.5029 no . 1_655 H56B C43 3.3049 no . 1_655 H56B C44 3.3948 no . 1_655 H56B C45 3.5818 no . 1_655 H56B C48 3.4278 no . 1_655 H56B H21 3.0191 no . 2_656 H56B H32 2.3580 no . 1_655 H56B H33 3.2766 no . 1_655 H56C Br3 3.4140 no . 1_655 H56C C44 3.2459 no . 1_655 H56C C45 3.4713 no . 1_655 H56C C51 2.8964 no . 4_555 H56C C52 2.7960 no . 4_555 H56C C53 3.5985 no . 4_555 H56C H32 3.0944 no . 1_655 H56C H44 3.2943 no . 1_655 H56C H51 2.9179 no . 4_555 H56C H52 2.7250 no . 4_555 H57A C1 2.9525 no . 1_655 H57A C2 2.6752 no . 1_655 H57A C3 2.7247 no . 1_655 H57A C4 2.9755 no . 1_655 H57A C5 3.2021 no . 1_655 H57A C10 3.2834 no . 1_655 H57A H2 3.0864 no . 1_655 H57A H3 3.1775 no . 1_655 H57A H32 3.5545 no . 1_655 H57B Br1 3.1338 no . 3_657 H57B C14 3.1574 no . 3_657 H57B C15 3.4932 no . 3_657 H57B H2 3.2137 no . 3_657 H57B H14 2.7336 no . 3_657 H57B H15 3.3340 no . 3_657 H57B H51 3.1662 no . 4_555 H57C Br1 3.2021 no . 1_655 H57C Br3 3.2895 no . 1_655 H57C C51 3.2319 no . 4_555 H57C C52 3.0759 no . 4_555 H57C H51 2.8077 no . 4_555 H57C H52 2.4700 no . 4_555 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================