# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'G Reid' 'Chitra Gurnani' 'Marek Jura' 'W Levason' 'Raju Ratnani' 'Michael Webster' _publ_contact_author_name 'G Reid' _publ_contact_author_email GR@SOTON.AC.UK _publ_section_title ; Synthesis, characterisation and structures of thio-, seleno- and telluro-ether complexes of indium(III) halides ; # Attachment 'In_all6_3.cif' # Manuscript ref.: # Title: Synthesis, characterisation and structures of thio-, seleno- # and telluro-ether complexes of indium(III) # Authors: C.Gurnani, M.Jura, W.Levason, R.Ratnani, G.Reid and M.Webster # Journal (proposed): Dalton Trans. # CCDC ref. no(s).: # DOI: # ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ### ############################################################################## # This is an electronic "form" for submitting structural details as a # Crystallographic Information File (CIF). # Full details of the format of such files are given in the paper "The # Crystallographic Information File (CIF): a New Standard Archive File for # Crystallography" by S. R. Hall, F. H. Allen and I. D. Brown [Acta Cryst. # (1991), A47, 655-685]. # # The current version of the core CIF dictionary is obtainable from # www.iucr.org as a pdf file. The current version number is 2.3. # # CIFs can be checked for legal syntax and possible errors (ALERTS) by # using checkcif software. # See the web (http://journals.iucr.org/services/cif/checkcif.html). # The website http://checkcif.iucr.org produces o/p in pdf format. # #============================================================================== data_08mj06 _database_code_depnum_ccdc_archive 'CCDC 702284' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-24 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrachlorobis(2,5-diselenahexane-Se,Se')di(mu!2$-chloro)diindium(III) ; # Se ligand. 1,2-bis(methylseleno)ethane ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Cl6 In2 Se4' _chemical_formula_sum 'C8 H20 Cl6 In2 Se4' _chemical_formula_weight 874.42 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' Cl Cl 0.1484 0.1585 '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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.160(3) _cell_length_b 12.463(4) _cell_length_c 9.826(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.00(2) _cell_angle_gamma 90.00 _cell_volume 1113.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 33247 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 9.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6000 # _exptl_absorpt_correction_T_max 0.7456 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14702 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2550 _reflns_number_gt 2249 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+3.0401P] 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 2550 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.06678(3) 0.09263(2) 0.65298(3) 0.01513(8) Uani 1 1 d . . . Cl1 Cl -0.04962(11) 0.11589(7) 0.40610(10) 0.0198(2) Uani 1 1 d . . . Cl2 Cl -0.15785(11) 0.07300(9) 0.75574(11) 0.0270(2) Uani 1 1 d . . . Cl3 Cl 0.10071(11) 0.28645(8) 0.68094(10) 0.0209(2) Uani 1 1 d . . . Se1 Se 0.23974(4) 0.03835(3) 0.89716(4) 0.01980(11) Uani 1 1 d . . . Se2 Se 0.33314(4) 0.06543(4) 0.55883(4) 0.02239(11) Uani 1 1 d . . . C1 C 0.2056(5) 0.1637(3) 1.0092(4) 0.0258(9) Uani 1 1 d . . . H1A H 0.2872 0.1714 1.0829 0.039 Uiso 1 1 calc R . . H1B H 0.1134 0.1544 1.0489 0.039 Uiso 1 1 calc R . . H1C H 0.1992 0.2282 0.9517 0.039 Uiso 1 1 calc R . . C2 C 0.4359(4) 0.0741(4) 0.8471(4) 0.0242(9) Uani 1 1 d . . . H2A H 0.4903 0.1143 0.9241 0.029 Uiso 1 1 calc R . . H2B H 0.4898 0.0062 0.8370 0.029 Uiso 1 1 calc R . . C3 C 0.4395(4) 0.1400(3) 0.7160(4) 0.0227(9) Uani 1 1 d . . . H3A H 0.5429 0.1516 0.6995 0.027 Uiso 1 1 calc R . . H3B H 0.3940 0.2110 0.7270 0.027 Uiso 1 1 calc R . . C4 C 0.3313(5) 0.1822(4) 0.4280(5) 0.0374(12) Uani 1 1 d . . . H4A H 0.3063 0.2493 0.4717 0.056 Uiso 1 1 calc R . . H4B H 0.2579 0.1674 0.3490 0.056 Uiso 1 1 calc R . . H4C H 0.4286 0.1888 0.3971 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.01322(14) 0.01686(15) 0.01506(14) -0.00026(11) 0.00083(10) -0.00041(10) Cl1 0.0232(5) 0.0169(5) 0.0178(5) 0.0016(4) -0.0040(4) 0.0009(4) Cl2 0.0205(5) 0.0324(6) 0.0300(6) -0.0043(5) 0.0104(4) -0.0022(4) Cl3 0.0230(5) 0.0164(5) 0.0226(5) 0.0002(4) -0.0007(4) 0.0003(4) Se1 0.0216(2) 0.0198(2) 0.0174(2) 0.00176(16) -0.00005(16) 0.00056(16) Se2 0.0156(2) 0.0309(2) 0.0213(2) -0.00599(17) 0.00450(16) -0.00198(17) C1 0.034(2) 0.029(2) 0.015(2) -0.0035(17) 0.0017(17) 0.002(2) C2 0.015(2) 0.030(2) 0.026(2) -0.0027(19) -0.0028(16) 0.0007(17) C3 0.0153(19) 0.027(2) 0.025(2) -0.0023(18) 0.0005(16) -0.0034(17) C4 0.035(3) 0.054(3) 0.025(2) 0.009(2) 0.008(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Cl2 2.4124(12) . ? In1 Cl3 2.4466(12) . ? In1 Cl1 2.5447(12) . ? In1 Cl1 2.6633(12) 3_556 ? In1 Se2 2.7339(8) . ? In1 Se1 2.7926(8) . ? Cl1 In1 2.6633(12) 3_556 ? Se1 C1 1.958(4) . ? Se1 C2 1.971(4) . ? Se2 C4 1.941(5) . ? Se2 C3 1.957(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.531(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 In1 Cl3 98.99(4) . . ? Cl2 In1 Cl1 97.52(4) . . ? Cl3 In1 Cl1 91.57(3) . . ? Cl2 In1 Cl1 87.80(4) . 3_556 ? Cl3 In1 Cl1 172.38(3) . 3_556 ? Cl1 In1 Cl1 84.07(3) . 3_556 ? Cl2 In1 Se2 166.16(3) . . ? Cl3 In1 Se2 93.10(3) . . ? Cl1 In1 Se2 88.80(3) . . ? Cl1 In1 Se2 80.60(3) 3_556 . ? Cl2 In1 Se1 92.26(4) . . ? Cl3 In1 Se1 95.26(3) . . ? Cl1 In1 Se1 167.07(3) . . ? Cl1 In1 Se1 87.89(2) 3_556 . ? Se2 In1 Se1 79.89(2) . . ? In1 Cl1 In1 95.93(3) . 3_556 ? C1 Se1 C2 99.96(19) . . ? C1 Se1 In1 100.19(12) . . ? C2 Se1 In1 99.77(12) . . ? C4 Se2 C3 97.5(2) . . ? C4 Se2 In1 101.24(15) . . ? C3 Se2 In1 93.06(13) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Se1 116.4(3) . . ? C3 C2 H2A 108.2 . . ? Se1 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? Se1 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C2 C3 Se2 110.4(3) . . ? C2 C3 H3A 109.6 . . ? Se2 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? Se2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? Se2 C4 H4A 109.5 . . ? Se2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Se2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Cl1 In1 Cl1 In1 0.0 3_556 . . 3_556 ? Cl2 In1 Cl1 In1 -86.98(4) . . . 3_556 ? Cl3 In1 Cl1 In1 173.74(4) . . . 3_556 ? Se2 In1 Cl1 In1 80.67(3) . . . 3_556 ? Se1 In1 Cl1 In1 51.82(13) . . . 3_556 ? Cl2 In1 Se1 C1 -68.27(14) . . . . ? Cl3 In1 Se1 C1 30.97(14) . . . . ? Cl1 In1 Se1 C1 152.54(18) . . . . ? Cl1 In1 Se1 C1 -155.99(14) 3_556 . . . ? Se2 In1 Se1 C1 123.19(14) . . . . ? Cl2 In1 Se1 C2 -170.35(13) . . . . ? Cl3 In1 Se1 C2 -71.10(13) . . . . ? Cl1 In1 Se1 C2 50.46(18) . . . . ? Cl1 In1 Se1 C2 101.94(13) 3_556 . . . ? Se2 In1 Se1 C2 21.12(13) . . . . ? Cl2 In1 Se2 C4 163.50(19) . . . . ? Cl3 In1 Se2 C4 -45.56(16) . . . . ? Cl1 In1 Se2 C4 45.95(16) . . . . ? Cl1 In1 Se2 C4 130.13(16) 3_556 . . . ? Se1 In1 Se2 C4 -140.35(15) . . . . ? Cl2 In1 Se2 C3 -98.26(17) . . . . ? Cl3 In1 Se2 C3 52.69(13) . . . . ? Cl1 In1 Se2 C3 144.19(13) . . . . ? Cl1 In1 Se2 C3 -131.63(13) 3_556 . . . ? Se1 In1 Se2 C3 -42.11(13) . . . . ? C1 Se1 C2 C3 -89.3(3) . . . . ? In1 Se1 C2 C3 13.0(3) . . . . ? Se1 C2 C3 Se2 -57.8(4) . . . . ? C4 Se2 C3 C2 169.9(3) . . . . ? In1 Se2 C3 C2 68.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.331 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.157 #===END OF CIF ============================================================== # 07mfd032 data_07mfd032 _database_code_depnum_ccdc_archive 'CCDC 702285' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-26 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-dichlorobis(2,7-dimethyl-3,6-dithiaoctane)indium(III) tetrachloroindate(III) dichloromethane solvate ; # S ligand: 1,2-bis(i-propylthio)ethane _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 Cl2 In S4 1+, Cl4 In 1-, 0.5(C H2 Cl2)' _chemical_formula_sum 'C16.50 H37 Cl7 In2 S4' _chemical_formula_structural '((C8 H18 S2)2 Cl2 In) (Cl4 In) (C H2 Cl2)0.5' _chemical_formula_weight 841.49 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' S S 0.1246 0.1234 '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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.324(5) _cell_length_b 11.033(2) _cell_length_c 20.679(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.131(7) _cell_angle_gamma 90.00 _cell_volume 6302.5(18) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20131 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 2.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6689 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30172 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7202 _reflns_number_gt 5278 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+166.7229P] 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 7202 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.125383(17) 0.94885(5) 0.15586(3) 0.01383(13) Uani 1 1 d . . . In2 In 0.161897(19) 0.44703(5) 0.44748(3) 0.01817(14) Uani 1 1 d . . . Cl1 Cl 0.19368(6) 0.87639(18) 0.14205(10) 0.0204(4) Uani 1 1 d . . . Cl2 Cl 0.05772(6) 1.02649(18) 0.17101(10) 0.0188(4) Uani 1 1 d . . . Cl3 Cl 0.16847(7) 0.4673(2) 0.56560(11) 0.0262(5) Uani 1 1 d . . . Cl4 Cl 0.23921(7) 0.4399(2) 0.45630(12) 0.0305(5) Uani 1 1 d . . . Cl5 Cl 0.11493(8) 0.6125(2) 0.37688(12) 0.0293(5) Uani 1 1 d . . . Cl6 Cl 0.11802(7) 0.2727(2) 0.38664(11) 0.0266(4) Uani 1 1 d . . . S1 S 0.16411(6) 0.90211(18) 0.29783(10) 0.0161(4) Uani 1 1 d . . . S2 S 0.17446(6) 1.15673(18) 0.19824(11) 0.0174(4) Uani 1 1 d . . . S3 S 0.08637(6) 0.72801(18) 0.11549(10) 0.0161(4) Uani 1 1 d . . . S4 S 0.07111(7) 0.99928(18) 0.01213(10) 0.0163(4) Uani 1 1 d . . . C1 C 0.2019(3) 0.6832(7) 0.2909(4) 0.0200(17) Uani 1 1 d . . . H1A H 0.2284 0.6247 0.3136 0.030 Uiso 1 1 calc R . . H1B H 0.1929 0.6925 0.2389 0.030 Uiso 1 1 calc R . . H1C H 0.1738 0.6539 0.2954 0.030 Uiso 1 1 calc R . . C2 C 0.2403(3) 0.7915(8) 0.4121(4) 0.0236(18) Uani 1 1 d . . . H2A H 0.2179 0.7470 0.4240 0.035 Uiso 1 1 calc R . . H2B H 0.2466 0.8717 0.4351 0.035 Uiso 1 1 calc R . . H2C H 0.2708 0.7467 0.4304 0.035 Uiso 1 1 calc R . . C3 C 0.2181(3) 0.8058(7) 0.3296(4) 0.0179(16) Uani 1 1 d . . . H3 H 0.2421 0.8441 0.3168 0.022 Uiso 1 1 calc R . . C4 C 0.1885(3) 1.0516(8) 0.3313(4) 0.0213(17) Uani 1 1 d . . . H4A H 0.1616 1.1042 0.3270 0.026 Uiso 1 1 calc R . . H4B H 0.2119 1.0449 0.3841 0.026 Uiso 1 1 calc R . . C5 C 0.2135(3) 1.1140(8) 0.2931(4) 0.0214(17) Uani 1 1 d . . . H5A H 0.2391 1.0595 0.2947 0.026 Uiso 1 1 calc R . . H5B H 0.2296 1.1880 0.3211 0.026 Uiso 1 1 calc R . . C6 C 0.1344(3) 1.2752(7) 0.2038(4) 0.0185(16) Uani 1 1 d . . . H6 H 0.1164 1.2420 0.2290 0.022 Uiso 1 1 calc R . . C7 C 0.0991(3) 1.3061(8) 0.1246(4) 0.0228(18) Uani 1 1 d . . . H7A H 0.0784 1.3736 0.1235 0.034 Uiso 1 1 calc R . . H7B H 0.0789 1.2352 0.1007 0.034 Uiso 1 1 calc R . . H7C H 0.1172 1.3293 0.0987 0.034 Uiso 1 1 calc R . . C8 C 0.1643(3) 1.3829(8) 0.2456(5) 0.029(2) Uani 1 1 d . . . H8A H 0.1827 1.4131 0.2217 0.043 Uiso 1 1 calc R . . H8B H 0.1866 1.3586 0.2960 0.043 Uiso 1 1 calc R . . H8C H 0.1428 1.4470 0.2462 0.043 Uiso 1 1 calc R . . C9 C 0.0367(3) 0.7098(8) 0.1921(4) 0.0251(19) Uani 1 1 d . . . H9A H 0.0061 0.7145 0.1943 0.038 Uiso 1 1 calc R . . H9B H 0.0585 0.7739 0.2226 0.038 Uiso 1 1 calc R . . H9C H 0.0517 0.6306 0.2103 0.038 Uiso 1 1 calc R . . C10 C -0.0051(3) 0.6254(8) 0.0635(5) 0.0262(19) Uani 1 1 d . . . H10A H 0.0112 0.5471 0.0806 0.039 Uiso 1 1 calc R . . H10B H -0.0109 0.6402 0.0133 0.039 Uiso 1 1 calc R . . H10C H -0.0360 0.6243 0.0645 0.039 Uiso 1 1 calc R . . C11 C 0.0268(3) 0.7257(8) 0.1135(4) 0.0190(16) Uani 1 1 d . . . H11 H 0.0104 0.8055 0.0948 0.023 Uiso 1 1 calc R . . C12 C 0.0719(3) 0.7432(7) 0.0199(4) 0.0174(16) Uani 1 1 d . . . H12A H 0.1025 0.7473 0.0171 0.021 Uiso 1 1 calc R . . H12B H 0.0545 0.6694 -0.0066 0.021 Uiso 1 1 calc R . . C13 C 0.0414(3) 0.8528(7) -0.0191(4) 0.0162(15) Uani 1 1 d . . . H13A H 0.0119 0.8518 -0.0130 0.019 Uiso 1 1 calc R . . H13B H 0.0310 0.8450 -0.0721 0.019 Uiso 1 1 calc R . . C14 C 0.1082(3) 1.0112(7) -0.0354(4) 0.0164(16) Uani 1 1 d . . . H14 H 0.1266 0.9340 -0.0282 0.020 Uiso 1 1 calc R . . C15 C 0.0752(3) 1.0299(8) -0.1172(5) 0.027(2) Uani 1 1 d . . . H15A H 0.0556 1.1028 -0.1247 0.041 Uiso 1 1 calc R . . H15B H 0.0539 0.9594 -0.1373 0.041 Uiso 1 1 calc R . . H15C H 0.0949 1.0395 -0.1422 0.041 Uiso 1 1 calc R . . C16 C 0.1432(3) 1.1120(8) -0.0012(5) 0.0273(19) Uani 1 1 d . . . H16A H 0.1626 1.1220 -0.0266 0.041 Uiso 1 1 calc R . . H16B H 0.1645 1.0934 0.0506 0.041 Uiso 1 1 calc R . . H16C H 0.1255 1.1872 -0.0050 0.041 Uiso 1 1 calc R . . Cl7 Cl 0.01701(9) 0.3275(3) 0.19522(14) 0.0483(7) Uani 1 1 d . . . C17 C 0.0000 0.4157(11) 0.2500 0.025(3) Uani 1 2 d S . . H17A H 0.0274 0.4686 0.2820 0.030 Uiso 0.50 1 calc PR . . H17B H -0.0274 0.4686 0.2180 0.030 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0124(2) 0.0153(3) 0.0132(3) 0.0003(2) 0.0056(2) 0.0007(2) In2 0.0180(3) 0.0203(3) 0.0167(3) -0.0009(2) 0.0086(2) -0.0021(2) Cl1 0.0183(8) 0.0238(11) 0.0222(10) 0.0013(8) 0.0122(8) 0.0046(8) Cl2 0.0155(8) 0.0222(11) 0.0198(9) -0.0006(8) 0.0092(7) 0.0014(7) Cl3 0.0275(10) 0.0343(13) 0.0183(10) -0.0025(9) 0.0121(8) -0.0048(9) Cl4 0.0208(9) 0.0458(14) 0.0275(11) -0.0073(10) 0.0136(9) -0.0061(10) Cl5 0.0321(11) 0.0252(11) 0.0260(11) 0.0040(9) 0.0099(9) 0.0056(9) Cl6 0.0290(10) 0.0250(11) 0.0253(11) -0.0052(9) 0.0124(9) -0.0069(9) S1 0.0170(8) 0.0169(10) 0.0146(9) 0.0006(8) 0.0077(7) 0.0019(8) S2 0.0151(8) 0.0165(10) 0.0194(10) 0.0007(8) 0.0071(8) -0.0012(8) S3 0.0152(8) 0.0162(10) 0.0154(9) 0.0011(8) 0.0059(7) -0.0002(7) S4 0.0177(8) 0.0180(10) 0.0144(9) 0.0019(8) 0.0084(7) 0.0024(8) C1 0.021(4) 0.019(4) 0.014(4) 0.004(3) 0.004(3) 0.000(3) C2 0.023(4) 0.018(4) 0.021(4) 0.000(4) 0.003(3) 0.004(3) C3 0.017(3) 0.018(4) 0.021(4) 0.002(3) 0.011(3) 0.002(3) C4 0.023(4) 0.020(4) 0.014(4) 0.005(3) 0.003(3) 0.010(4) C5 0.011(3) 0.017(4) 0.022(4) -0.004(3) -0.004(3) -0.003(3) C6 0.017(4) 0.016(4) 0.019(4) -0.005(3) 0.006(3) -0.001(3) C7 0.023(4) 0.026(5) 0.017(4) 0.006(4) 0.007(3) 0.004(4) C8 0.025(4) 0.024(5) 0.030(5) -0.004(4) 0.006(4) 0.003(4) C9 0.030(4) 0.033(5) 0.017(4) 0.002(4) 0.015(4) -0.002(4) C10 0.027(4) 0.024(5) 0.026(5) -0.005(4) 0.011(4) -0.006(4) C11 0.015(3) 0.023(4) 0.024(4) 0.002(4) 0.013(3) 0.002(3) C12 0.023(4) 0.015(4) 0.015(4) -0.001(3) 0.010(3) -0.001(3) C13 0.018(3) 0.014(4) 0.016(4) 0.002(3) 0.008(3) -0.002(3) C14 0.021(4) 0.017(4) 0.018(4) 0.007(3) 0.015(3) 0.003(3) C15 0.035(5) 0.030(5) 0.026(4) 0.006(4) 0.023(4) 0.003(4) C16 0.026(4) 0.028(5) 0.027(5) -0.002(4) 0.012(4) -0.003(4) Cl7 0.0338(12) 0.074(2) 0.0412(14) -0.0207(14) 0.0211(11) 0.0018(13) C17 0.021(5) 0.026(7) 0.029(7) 0.000 0.013(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Cl1 2.4237(18) . ? In1 Cl2 2.4393(18) . ? In1 S1 2.645(2) . ? In1 S2 2.669(2) . ? In1 S3 2.677(2) . ? In1 S4 2.696(2) . ? In2 Cl4 2.3425(19) . ? In2 Cl6 2.354(2) . ? In2 Cl3 2.3629(19) . ? In2 Cl5 2.367(2) . ? S1 C4 1.812(9) . ? S1 C3 1.837(8) . ? S2 C5 1.818(8) . ? S2 C6 1.852(8) . ? S3 C12 1.815(7) . ? S3 C11 1.848(7) . ? S4 C13 1.825(8) . ? S4 C14 1.848(7) . ? C1 C3 1.532(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.516(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.516(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.507(11) . ? C6 C7 1.521(11) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.516(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.522(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 1.0000 . ? C12 C13 1.516(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.485(11) . ? C14 C15 1.524(11) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Cl7 C17 1.756(7) . ? C17 Cl7 1.756(7) 2 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 In1 Cl2 178.57(7) . . ? Cl1 In1 S1 95.63(6) . . ? Cl2 In1 S1 84.12(6) . . ? Cl1 In1 S2 85.31(6) . . ? Cl2 In1 S2 93.27(6) . . ? S1 In1 S2 84.92(6) . . ? Cl1 In1 S3 87.80(6) . . ? Cl2 In1 S3 93.62(6) . . ? S1 In1 S3 94.11(6) . . ? S2 In1 S3 172.91(6) . . ? Cl1 In1 S4 94.07(6) . . ? Cl2 In1 S4 86.25(6) . . ? S1 In1 S4 169.91(6) . . ? S2 In1 S4 98.68(6) . . ? S3 In1 S4 83.46(6) . . ? Cl4 In2 Cl6 109.62(8) . . ? Cl4 In2 Cl3 109.85(7) . . ? Cl6 In2 Cl3 111.96(7) . . ? Cl4 In2 Cl5 113.15(8) . . ? Cl6 In2 Cl5 105.32(8) . . ? Cl3 In2 Cl5 106.89(8) . . ? C4 S1 C3 103.8(4) . . ? C4 S1 In1 97.9(3) . . ? C3 S1 In1 111.9(2) . . ? C5 S2 C6 104.3(4) . . ? C5 S2 In1 97.0(3) . . ? C6 S2 In1 108.9(3) . . ? C12 S3 C11 104.2(4) . . ? C12 S3 In1 95.7(3) . . ? C11 S3 In1 109.1(3) . . ? C13 S4 C14 102.6(3) . . ? C13 S4 In1 99.1(2) . . ? C14 S4 In1 111.9(2) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 111.1(7) . . ? C2 C3 S1 108.6(5) . . ? C1 C3 S1 107.5(5) . . ? C2 C3 H3 109.9 . . ? C1 C3 H3 109.9 . . ? S1 C3 H3 109.9 . . ? C5 C4 S1 116.3(6) . . ? C5 C4 H4A 108.2 . . ? S1 C4 H4A 108.2 . . ? C5 C4 H4B 108.2 . . ? S1 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? C4 C5 S2 115.5(5) . . ? C4 C5 H5A 108.4 . . ? S2 C5 H5A 108.4 . . ? C4 C5 H5B 108.4 . . ? S2 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C8 C6 C7 112.3(7) . . ? C8 C6 S2 109.7(5) . . ? C7 C6 S2 105.2(5) . . ? C8 C6 H6 109.8 . . ? C7 C6 H6 109.8 . . ? S2 C6 H6 109.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C10 112.4(7) . . ? C9 C11 S3 106.5(5) . . ? C10 C11 S3 110.9(5) . . ? C9 C11 H11 109.0 . . ? C10 C11 H11 109.0 . . ? S3 C11 H11 109.0 . . ? C13 C12 S3 115.1(5) . . ? C13 C12 H12A 108.5 . . ? S3 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? S3 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C12 C13 S4 115.5(5) . . ? C12 C13 H13A 108.4 . . ? S4 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? S4 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C16 C14 C15 112.9(7) . . ? C16 C14 S4 107.9(5) . . ? C15 C14 S4 109.4(5) . . ? C16 C14 H14 108.8 . . ? C15 C14 H14 108.8 . . ? S4 C14 H14 108.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl7 C17 Cl7 112.7(7) 2 . ? Cl7 C17 H17A 109.1 2 . ? Cl7 C17 H17A 109.1 . . ? Cl7 C17 H17B 109.1 2 . ? Cl7 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? 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 # S3 In1 S2 C5 -68.8(6) . . . . ? # S3 In1 S2 C6 -176.5(5) . . . . ? # S2 In1 S3 C12 -85.3(5) . . . . ? # S2 In1 S3 C11 167.5(5) . . . . ? Cl1 In1 S1 C4 95.6(3) . . . . ? Cl2 In1 S1 C4 -83.0(3) . . . . ? S2 In1 S1 C4 10.8(3) . . . . ? S3 In1 S1 C4 -176.2(3) . . . . ? S4 In1 S1 C4 -100.5(4) . . . . ? Cl1 In1 S1 C3 -12.8(3) . . . . ? Cl2 In1 S1 C3 168.6(3) . . . . ? S2 In1 S1 C3 -97.6(3) . . . . ? S3 In1 S1 C3 75.4(3) . . . . ? S4 In1 S1 C3 151.1(4) . . . . ? Cl1 In1 S2 C5 -82.4(3) . . . . ? Cl2 In1 S2 C5 97.4(3) . . . . ? S1 In1 S2 C5 13.6(3) . . . . ? S4 In1 S2 C5 -175.9(3) . . . . ? Cl1 In1 S2 C6 169.8(3) . . . . ? Cl2 In1 S2 C6 -10.3(3) . . . . ? S1 In1 S2 C6 -94.1(3) . . . . ? S4 In1 S2 C6 76.4(3) . . . . ? Cl1 In1 S3 C12 -71.7(2) . . . . ? Cl2 In1 S3 C12 108.5(2) . . . . ? S1 In1 S3 C12 -167.2(2) . . . . ? S4 In1 S3 C12 22.7(2) . . . . ? Cl1 In1 S3 C11 -178.8(3) . . . . ? Cl2 In1 S3 C11 1.3(3) . . . . ? S1 In1 S3 C11 85.7(3) . . . . ? S4 In1 S3 C11 -84.5(3) . . . . ? Cl1 In1 S4 C13 89.2(2) . . . . ? Cl2 In1 S4 C13 -92.2(2) . . . . ? S1 In1 S4 C13 -74.7(4) . . . . ? S2 In1 S4 C13 175.1(2) . . . . ? S3 In1 S4 C13 1.9(2) . . . . ? Cl1 In1 S4 C14 -18.5(3) . . . . ? Cl2 In1 S4 C14 160.1(3) . . . . ? S1 In1 S4 C14 177.6(4) . . . . ? S2 In1 S4 C14 67.4(3) . . . . ? S3 In1 S4 C14 -105.8(3) . . . . ? C4 S1 C3 C2 71.1(6) . . . . ? In1 S1 C3 C2 175.6(5) . . . . ? C4 S1 C3 C1 -168.7(5) . . . . ? In1 S1 C3 C1 -64.2(5) . . . . ? C3 S1 C4 C5 71.8(6) . . . . ? In1 S1 C4 C5 -43.1(6) . . . . ? S1 C4 C5 S2 67.1(7) . . . . ? C6 S2 C5 C4 66.4(7) . . . . ? In1 S2 C5 C4 -45.2(6) . . . . ? C5 S2 C6 C8 62.8(6) . . . . ? In1 S2 C6 C8 165.5(5) . . . . ? C5 S2 C6 C7 -176.2(5) . . . . ? In1 S2 C6 C7 -73.5(5) . . . . ? C12 S3 C11 C9 178.5(6) . . . . ? In1 S3 C11 C9 -80.2(6) . . . . ? C12 S3 C11 C10 56.0(6) . . . . ? In1 S3 C11 C10 157.2(5) . . . . ? C11 S3 C12 C13 56.7(6) . . . . ? In1 S3 C12 C13 -54.7(5) . . . . ? S3 C12 C13 S4 67.8(6) . . . . ? C14 S4 C13 C12 80.1(6) . . . . ? In1 S4 C13 C12 -35.0(5) . . . . ? C13 S4 C14 C16 -166.6(6) . . . . ? In1 S4 C14 C16 -61.2(6) . . . . ? C13 S4 C14 C15 70.2(6) . . . . ? In1 S4 C14 C15 175.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.217 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.223 #===END OF CIF ============================================================== # 08cg001 data_08cg001 _database_code_depnum_ccdc_archive 'CCDC 702286' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-07-16 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-dibromobis(2,5-diselenahexane)indium(III) tetrabromoindate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Br2 In Se4 1+, Br4 In 1-' _chemical_formula_sum 'C8 H20 Br6 In2 Se4' _chemical_formula_weight 1141.18 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6920(10) _cell_length_b 16.323(2) _cell_length_c 20.058(3) _cell_angle_alpha 86.925(6) _cell_angle_beta 86.862(10) _cell_angle_gamma 86.979(10) _cell_volume 2507.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10948 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 17.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6339 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35035 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.54 _reflns_number_total 11355 _reflns_number_gt 8202 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+61.5000P] 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 11355 _refine_ls_number_parameters 393 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.52973(10) 0.50186(5) 0.26129(4) 0.02319(19) Uani 1 1 d . . . In2 In 0.49528(10) 1.00221(5) 0.24204(4) 0.02276(19) Uani 1 1 d DU . . In3 In 0.18902(11) 0.72016(6) 0.02896(4) 0.0256(2) Uani 1 1 d . . . In4 In 0.15546(10) 0.74584(5) 0.52781(4) 0.02311(19) Uani 1 1 d . . . Br1 Br 0.33084(17) 0.60729(8) 0.32729(7) 0.0324(3) Uani 1 1 d . . . Br2 Br 0.73605(16) 0.39802(8) 0.19628(7) 0.0315(3) Uani 1 1 d . . . Br3 Br 0.29990(16) 1.12962(8) 0.19942(7) 0.0299(3) Uani 1 1 d . A . Br4 Br 0.68602(17) 0.87495(8) 0.28508(7) 0.0334(3) Uani 1 1 d . A . Br5 Br 0.17661(18) 0.57006(9) 0.05916(8) 0.0388(3) Uani 1 1 d . . . Br6 Br -0.05671(17) 0.76910(11) -0.04081(7) 0.0435(4) Uani 1 1 d . . . Br7 Br 0.14961(18) 0.80316(9) 0.13118(7) 0.0367(3) Uani 1 1 d . . . Br8 Br 0.47503(16) 0.74817(10) -0.02828(7) 0.0374(3) Uani 1 1 d . . . Br9 Br -0.07831(17) 0.82288(10) 0.46417(7) 0.0408(4) Uani 1 1 d . . . Br10 Br 0.44890(16) 0.77949(9) 0.47891(7) 0.0328(3) Uani 1 1 d . . . Br11 Br 0.11217(17) 0.59516(8) 0.53118(7) 0.0340(3) Uani 1 1 d . . . Br12 Br 0.11155(17) 0.79860(8) 0.64305(6) 0.0305(3) Uani 1 1 d . . . Se1 Se 0.22445(16) 0.44801(8) 0.21976(7) 0.0274(3) Uani 1 1 d . . . Se2 Se 0.51064(16) 0.37681(8) 0.36074(6) 0.0272(3) Uani 1 1 d . . . Se3 Se 0.83697(16) 0.55390(8) 0.30447(7) 0.0283(3) Uani 1 1 d . . . Se4 Se 0.55467(16) 0.62391(8) 0.15987(7) 0.0274(3) Uani 1 1 d . . . Se5A Se 0.4347(3) 1.0699(2) 0.36607(11) 0.0262(8) Uani 0.722(10) 1 d PDU A 1 Se5B Se 0.4778(8) 1.0281(6) 0.3775(3) 0.023(2) Uani 0.278(10) 1 d PD A 2 Se6 Se 0.18308(15) 0.93136(7) 0.26562(6) 0.0235(3) Uani 1 1 d . A . Se7A Se 0.5220(2) 0.96786(11) 0.10645(8) 0.0244(6) Uani 0.862(8) 1 d PD A 3 Se7B Se 0.581(2) 0.9360(10) 0.1239(7) 0.065(5) Uiso 0.138(8) 1 d PD A 4 Se8 Se 0.80705(15) 1.07373(7) 0.21893(6) 0.0242(3) Uani 1 1 d . A . C1 C 0.285(2) 0.3647(8) 0.1542(7) 0.044(4) Uani 1 1 d . . . H1A H 0.3806 0.3279 0.1704 0.066 Uiso 1 1 calc R . . H1B H 0.3225 0.3917 0.1114 0.066 Uiso 1 1 calc R . . H1C H 0.1834 0.3328 0.1482 0.066 Uiso 1 1 calc R . . C2 C 0.175(2) 0.3748(11) 0.2982(8) 0.054(5) Uani 1 1 d . . . H2A H 0.1305 0.4090 0.3354 0.065 Uiso 1 1 calc R . . H2B H 0.0797 0.3397 0.2879 0.065 Uiso 1 1 calc R . . C3 C 0.3266(19) 0.3187(9) 0.3230(7) 0.041(4) Uani 1 1 d . . . H3A H 0.3779 0.2874 0.2852 0.049 Uiso 1 1 calc R . . H3B H 0.2804 0.2786 0.3575 0.049 Uiso 1 1 calc R . . C4 C 0.3788(18) 0.4222(10) 0.4382(7) 0.041(4) Uani 1 1 d . . . H4A H 0.3012 0.4682 0.4231 0.061 Uiso 1 1 calc R . . H4B H 0.4601 0.4416 0.4692 0.061 Uiso 1 1 calc R . . H4C H 0.3095 0.3795 0.4611 0.061 Uiso 1 1 calc R . . C5 C 0.788(2) 0.6426(10) 0.3642(8) 0.051(4) Uani 1 1 d . . . H5A H 0.8881 0.6772 0.3632 0.076 Uiso 1 1 calc R . . H5B H 0.7648 0.6197 0.4099 0.076 Uiso 1 1 calc R . . H5C H 0.6851 0.6757 0.3499 0.076 Uiso 1 1 calc R . . C6 C 0.8968(16) 0.6200(9) 0.2232(7) 0.035(3) Uani 1 1 d . . . H6A H 0.9942 0.6543 0.2324 0.042 Uiso 1 1 calc R . . H6B H 0.9399 0.5824 0.1882 0.042 Uiso 1 1 calc R . . C7 C 0.7500(17) 0.6764(8) 0.1951(7) 0.033(3) Uani 1 1 d . . . H7A H 0.8015 0.7125 0.1589 0.040 Uiso 1 1 calc R . . H7B H 0.7032 0.7120 0.2310 0.040 Uiso 1 1 calc R . . C8 C 0.6768(17) 0.5756(9) 0.0840(7) 0.038(3) Uani 1 1 d . . . H8A H 0.7198 0.6192 0.0529 0.058 Uiso 1 1 calc R . . H8B H 0.5972 0.5428 0.0613 0.058 Uiso 1 1 calc R . . H8C H 0.7754 0.5403 0.0992 0.058 Uiso 1 1 calc R . . C9A C 0.616(2) 1.0174(12) 0.4201(9) 0.038(4) Uani 0.722(10) 1 d PDU A 1 H9AA H 0.5884 1.0275 0.4673 0.057 Uiso 0.722(10) 1 calc PR A 1 H9AB H 0.7284 1.0402 0.4061 0.057 Uiso 0.722(10) 1 calc PR A 1 H9AC H 0.6225 0.9581 0.4140 0.057 Uiso 0.722(10) 1 calc PR A 1 C9B C 0.374(6) 1.1394(14) 0.382(2) 0.032(11) Uiso 0.278(10) 1 d PD A 2 H9BA H 0.3391 1.1502 0.4286 0.048 Uiso 0.278(10) 1 calc PR A 2 H9BB H 0.2719 1.1453 0.3549 0.048 Uiso 0.278(10) 1 calc PR A 2 H9BC H 0.4599 1.1788 0.3651 0.048 Uiso 0.278(10) 1 calc PR A 2 C10 C 0.2472(11) 0.9940(7) 0.3983(6) 0.030(3) Uani 1 1 d DU . . H10A H 0.2997 0.9382 0.4076 0.036 Uiso 1 1 calc R A 1 H10B H 0.1901 1.0135 0.4404 0.036 Uiso 1 1 calc R A 1 C11 C 0.1119(16) 0.9908(8) 0.3460(6) 0.029(3) Uani 1 1 d . A . H11A H 0.0759 1.0480 0.3317 0.034 Uiso 1 1 calc R . . H11B H 0.0078 0.9652 0.3676 0.034 Uiso 1 1 calc R . . C12 C 0.2275(17) 0.8217(7) 0.3057(7) 0.030(3) Uani 1 1 d . . . H12A H 0.3050 0.8244 0.3426 0.045 Uiso 1 1 calc R A . H12B H 0.2829 0.7861 0.2720 0.045 Uiso 1 1 calc R . . H12C H 0.1171 0.7992 0.3227 0.045 Uiso 1 1 calc R . . C13A C 0.6465(18) 0.8609(6) 0.1046(8) 0.032(4) Uani 0.862(8) 1 d PD A 3 H13A H 0.7025 0.8538 0.0601 0.047 Uiso 0.862(8) 1 calc PR A 3 H13B H 0.5641 0.8176 0.1149 0.047 Uiso 0.862(8) 1 calc PR A 3 H13C H 0.7355 0.8574 0.1379 0.047 Uiso 0.862(8) 1 calc PR A 3 C13B C 0.368(5) 0.971(4) 0.079(4) 0.040 Uiso 0.138(8) 1 d PD A 4 H13D H 0.3367 1.0286 0.0886 0.060 Uiso 0.138(8) 1 calc PR A 4 H13E H 0.2734 0.9365 0.0963 0.060 Uiso 0.138(8) 1 calc PR A 4 H13F H 0.3875 0.9660 0.0311 0.060 Uiso 0.138(8) 1 calc PR A 4 C14 C 0.7231(15) 1.0296(8) 0.0849(7) 0.042(4) Uani 1 1 d D . . H14A H 0.7745 1.0111 0.0416 0.050 Uiso 1 1 calc R A 3 H14B H 0.6819 1.0877 0.0772 0.050 Uiso 1 1 calc R A 3 C15 C 0.8640(17) 1.0285(8) 0.1306(7) 0.034(3) Uani 1 1 d . A . H15A H 0.9599 1.0597 0.1084 0.040 Uiso 1 1 calc R . . H15B H 0.9087 0.9709 0.1378 0.040 Uiso 1 1 calc R . . C16 C 0.7511(16) 1.1873(7) 0.1917(6) 0.024(3) Uani 1 1 d . . . H16A H 0.8525 1.2106 0.1674 0.036 Uiso 1 1 calc R A . H16B H 0.7200 1.2185 0.2314 0.036 Uiso 1 1 calc R . . H16C H 0.6525 1.1901 0.1626 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0204(4) 0.0181(4) 0.0305(5) -0.0017(4) 0.0044(3) -0.0014(3) In2 0.0216(4) 0.0199(4) 0.0262(5) 0.0000(3) 0.0012(3) -0.0001(3) In3 0.0199(4) 0.0354(5) 0.0215(5) 0.0002(4) 0.0002(3) -0.0056(4) In4 0.0207(4) 0.0266(5) 0.0223(4) -0.0007(4) -0.0001(3) -0.0055(3) Br1 0.0318(6) 0.0234(6) 0.0411(8) -0.0070(6) 0.0075(6) 0.0024(5) Br2 0.0298(6) 0.0200(6) 0.0434(8) -0.0040(6) 0.0072(6) 0.0032(5) Br3 0.0265(6) 0.0238(6) 0.0382(8) 0.0050(6) -0.0007(5) 0.0027(5) Br4 0.0298(6) 0.0217(6) 0.0483(9) 0.0019(6) -0.0047(6) 0.0026(5) Br5 0.0391(7) 0.0347(8) 0.0428(9) -0.0059(6) 0.0060(6) -0.0080(6) Br6 0.0206(6) 0.0754(11) 0.0341(8) 0.0054(7) -0.0060(5) -0.0035(7) Br7 0.0345(7) 0.0378(8) 0.0393(8) -0.0138(6) -0.0034(6) -0.0016(6) Br8 0.0188(6) 0.0638(10) 0.0288(7) 0.0086(7) -0.0001(5) -0.0056(6) Br9 0.0236(6) 0.0597(10) 0.0380(8) 0.0085(7) -0.0044(6) 0.0002(6) Br10 0.0208(6) 0.0386(8) 0.0376(8) 0.0098(6) 0.0009(5) -0.0047(5) Br11 0.0338(7) 0.0299(7) 0.0392(8) -0.0104(6) 0.0065(6) -0.0110(6) Br12 0.0388(7) 0.0263(7) 0.0270(7) -0.0086(5) -0.0026(5) 0.0001(6) Se1 0.0232(6) 0.0272(7) 0.0320(7) -0.0016(5) 0.0013(5) -0.0042(5) Se2 0.0270(6) 0.0247(7) 0.0290(7) 0.0008(5) 0.0024(5) 0.0005(5) Se3 0.0249(6) 0.0296(7) 0.0304(7) -0.0022(6) 0.0017(5) -0.0054(5) Se4 0.0251(6) 0.0223(6) 0.0334(7) 0.0036(5) 0.0022(5) 0.0005(5) Se5A 0.0319(11) 0.0211(18) 0.0259(10) -0.0033(9) -0.0042(8) -0.0009(11) Se5B 0.026(3) 0.017(4) 0.025(3) 0.001(2) -0.0016(19) 0.002(3) Se6 0.0225(6) 0.0196(6) 0.0282(7) -0.0006(5) -0.0009(5) -0.0002(5) Se7A 0.0219(8) 0.0265(10) 0.0251(9) -0.0044(6) -0.0034(6) 0.0022(6) Se8 0.0225(6) 0.0188(6) 0.0316(7) -0.0008(5) -0.0026(5) -0.0017(5) C1 0.072(11) 0.022(7) 0.041(9) -0.014(6) -0.014(8) 0.000(7) C2 0.043(9) 0.065(11) 0.053(10) 0.033(9) -0.005(7) -0.029(8) C3 0.051(9) 0.036(8) 0.035(8) 0.017(7) -0.001(7) -0.026(7) C4 0.034(7) 0.057(10) 0.030(8) -0.007(7) 0.011(6) 0.010(7) C5 0.050(9) 0.054(10) 0.051(10) -0.027(8) 0.004(8) -0.006(8) C6 0.027(6) 0.043(8) 0.034(8) 0.000(6) 0.010(6) -0.006(6) C7 0.042(8) 0.028(7) 0.030(7) -0.004(6) -0.002(6) -0.003(6) C8 0.029(7) 0.045(9) 0.038(8) 0.013(7) 0.002(6) 0.007(6) C9A 0.032(8) 0.045(12) 0.039(9) -0.010(9) -0.013(8) -0.004(8) C10 0.023(6) 0.035(7) 0.033(7) -0.012(6) -0.001(5) -0.005(5) C11 0.033(7) 0.023(7) 0.031(7) -0.011(6) 0.000(6) -0.007(5) C12 0.039(7) 0.018(6) 0.032(7) 0.005(5) 0.000(6) -0.006(5) C13A 0.035(8) 0.018(7) 0.042(9) -0.016(7) 0.012(7) -0.002(6) C14 0.037(8) 0.051(9) 0.040(9) -0.020(7) 0.007(6) -0.019(7) C15 0.041(7) 0.024(7) 0.038(8) -0.019(6) 0.018(6) -0.018(6) C16 0.041(7) 0.010(5) 0.023(6) -0.003(5) -0.014(5) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Br1 2.6076(15) . ? In1 Br2 2.6113(15) . ? In1 Se1 2.7370(16) . ? In1 Se3 2.7516(16) . ? In1 Se4 2.7762(15) . ? In1 Se2 2.7802(15) . ? In2 Br4 2.6150(15) . ? In2 Br3 2.6334(14) . ? In2 Se7B 2.691(13) . ? In2 Se6 2.7272(15) . ? In2 Se8 2.7284(15) . ? In2 Se5B 2.767(5) . ? In2 Se5A 2.782(2) . ? In2 Se7A 2.8006(18) . ? In3 Br8 2.4779(15) . ? In3 Br6 2.4859(16) . ? In3 Br5 2.4977(18) . ? In3 Br7 2.5135(17) . ? In4 Br10 2.4877(15) . ? In4 Br11 2.4962(17) . ? In4 Br9 2.5070(16) . ? In4 Br12 2.5091(16) . ? Se1 C2 1.958(14) . ? Se1 C1 1.964(13) . ? Se2 C3 1.952(14) . ? Se2 C4 1.966(12) . ? Se3 C5 1.938(14) . ? Se3 C6 1.953(13) . ? Se4 C8 1.927(14) . ? Se4 C7 1.951(14) . ? Se5A C9A 1.947(9) . ? Se5A C10 2.007(7) . ? Se5B C10 1.905(7) . ? Se5B C9B 1.950(10) . ? Se6 C12 1.944(11) . ? Se6 C11 1.964(12) . ? Se7A C14 1.908(8) . ? Se7A C13A 1.948(8) . ? Se7B C13B 1.952(10) . ? Se7B C14 2.025(9) . ? Se8 C16 1.937(11) . ? Se8 C15 1.975(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.53(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.531(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? C10 C11 1.523(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14 C15 1.456(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # Se5B C10 Se5A 22.5(2) . . ? # Se7A C14 Se7B 21.9(6) . . ? Br1 In1 Br2 178.50(6) . . ? Br1 In1 Se1 85.22(5) . . ? Br2 In1 Se1 96.28(5) . . ? Br1 In1 Se3 94.98(5) . . ? Br2 In1 Se3 83.53(5) . . ? Se1 In1 Se3 179.09(5) . . ? Br1 In1 Se4 86.54(5) . . ? Br2 In1 Se4 93.28(5) . . ? Se1 In1 Se4 93.79(5) . . ? Se3 In1 Se4 87.10(5) . . ? Br1 In1 Se2 95.03(5) . . ? Br2 In1 Se2 85.15(5) . . ? Se1 In1 Se2 86.35(5) . . ? Se3 In1 Se2 92.75(5) . . ? Se4 In1 Se2 178.43(5) . . ? Br4 In2 Br3 179.32(6) . . ? Br4 In2 Se7B 81.3(5) . . ? Br3 In2 Se7B 99.0(5) . . ? Br4 In2 Se6 95.80(5) . . ? Br3 In2 Se6 83.55(4) . . ? Se7B In2 Se6 97.1(3) . . ? Br4 In2 Se8 84.35(5) . . ? Br3 In2 Se8 96.30(5) . . ? Se7B In2 Se8 83.2(3) . . ? Se6 In2 Se8 179.69(6) . . ? Br4 In2 Se5B 80.1(2) . . ? Br3 In2 Se5B 99.7(2) . . ? Se7B In2 Se5B 161.3(5) . . ? Se6 In2 Se5B 85.78(10) . . ? Se8 In2 Se5B 93.97(10) . . ? Br4 In2 Se5A 95.85(10) . . ? Br3 In2 Se5A 83.92(10) . . ? Se7B In2 Se5A 175.5(4) . . ? Se6 In2 Se5A 86.66(5) . . ? Se8 In2 Se5A 93.05(6) . . ? Se5B In2 Se5A 15.98(15) . . ? Br4 In2 Se7A 96.89(6) . . ? Br3 In2 Se7A 83.36(5) . . ? Se7B In2 Se7A 15.7(5) . . ? Se6 In2 Se7A 94.18(5) . . ? Se8 In2 Se7A 86.07(5) . . ? Se5B In2 Se7A 176.9(2) . . ? Se5A In2 Se7A 167.08(10) . . ? Br8 In3 Br6 111.65(6) . . ? Br8 In3 Br5 109.51(6) . . ? Br6 In3 Br5 111.05(6) . . ? Br8 In3 Br7 108.91(6) . . ? Br6 In3 Br7 104.50(6) . . ? Br5 In3 Br7 111.13(6) . . ? Br10 In4 Br11 111.87(5) . . ? Br10 In4 Br9 110.49(6) . . ? Br11 In4 Br9 110.39(6) . . ? Br10 In4 Br12 110.02(6) . . ? Br11 In4 Br12 110.23(6) . . ? Br9 In4 Br12 103.52(6) . . ? C2 Se1 C1 98.8(7) . . ? C2 Se1 In1 96.4(5) . . ? C1 Se1 In1 107.4(5) . . ? C3 Se2 C4 99.5(7) . . ? C3 Se2 In1 96.7(4) . . ? C4 Se2 In1 107.3(5) . . ? C5 Se3 C6 98.3(7) . . ? C5 Se3 In1 109.7(5) . . ? C6 Se3 In1 95.7(4) . . ? C8 Se4 C7 98.4(6) . . ? C8 Se4 In1 107.4(4) . . ? C7 Se4 In1 95.8(4) . . ? C9A Se5A C10 96.1(7) . . ? C9A Se5A In2 104.0(6) . . ? C10 Se5A In2 95.3(4) . . ? C10 Se5B C9B 85.3(15) . . ? C10 Se5B In2 98.3(4) . . ? C9B Se5B In2 103.3(15) . . ? C12 Se6 C11 100.1(6) . . ? C12 Se6 In2 108.0(4) . . ? C11 Se6 In2 96.0(4) . . ? C14 Se7A C13A 95.3(6) . . ? C14 Se7A In2 95.7(4) . . ? C13A Se7A In2 104.2(5) . . ? C13B Se7B C14 95.7(10) . . ? C13B Se7B In2 98(3) . . ? C14 Se7B In2 96.3(6) . . ? C16 Se8 C15 99.9(6) . . ? C16 Se8 In2 105.9(4) . . ? C15 Se8 In2 96.5(4) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Se1 116.9(10) . . ? C3 C2 H2A 108.1 . . ? Se1 C2 H2A 108.1 . . ? C3 C2 H2B 108.1 . . ? Se1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C2 C3 Se2 114.1(11) . . ? C2 C3 H3A 108.7 . . ? Se2 C3 H3A 108.7 . . ? C2 C3 H3B 108.7 . . ? Se2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? Se2 C4 H4A 109.5 . . ? Se2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Se2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Se3 C5 H5A 109.5 . . ? Se3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Se3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 Se3 116.3(9) . . ? C7 C6 H6A 108.2 . . ? Se3 C6 H6A 108.2 . . ? C7 C6 H6B 108.2 . . ? Se3 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? C6 C7 Se4 117.2(10) . . ? C6 C7 H7A 108.0 . . ? Se4 C7 H7A 108.0 . . ? C6 C7 H7B 108.0 . . ? Se4 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? Se4 C8 H8A 109.5 . . ? Se4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Se4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Se5B C9B H9BA 109.5 . . ? Se5B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? Se5B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C11 C10 Se5B 123.0(9) . . ? C11 C10 Se5A 110.6(8) . . ? C11 C10 H10A 109.5 . . ? Se5B C10 H10A 87.1 . . ? Se5A C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? Se5B C10 H10B 116.1 . . ? Se5A C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 Se6 116.7(8) . . ? C10 C11 H11A 108.1 . . ? Se6 C11 H11A 108.1 . . ? C10 C11 H11B 108.1 . . ? Se6 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? Se6 C12 H12A 109.5 . . ? Se6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Se6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C14 Se7A 120.7(9) . . ? C15 C14 Se7B 101.9(11) . . ? C15 C14 H14A 107.1 . . ? Se7A C14 H14A 107.1 . . ? Se7B C14 H14A 105.6 . . ? C15 C14 H14B 107.1 . . ? Se7A C14 H14B 107.1 . . ? Se7B C14 H14B 126.9 . . ? H14A C14 H14B 106.8 . . ? C14 C15 Se8 116.8(9) . . ? C14 C15 H15A 108.1 . . ? Se8 C15 H15A 108.1 . . ? C14 C15 H15B 108.1 . . ? Se8 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? Se8 C16 H16A 109.5 . . ? Se8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Se8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.220 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.313 #===END OF CIF ============================================================== # 08mj05 data_08mj05 _database_code_depnum_ccdc_archive 'CCDC 702287' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-05-09 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-dibromobis(2,7-dimethyl-3,6-dithiaoctane-S,S')indium(III) tetrabromoindate ; # S ligand 1,2-bis(i-propylthio)ethane _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 Br2 In S4 1+, Br4 In 1-' _chemical_formula_sum 'C16 H36 Br6 In2 S4' _chemical_formula_structural '((C8 H18 S2)2 In Br2) (Br4 In)' _chemical_formula_weight 1065.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_IT_number 19 # New _space_group_name_Hall 'P 2ac 2ab' # New loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.4407(10) _cell_length_b 12.9075(12) _cell_length_c 21.6066(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3190.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17067 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 9.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7862 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22267 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7294 _reflns_number_gt 6702 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.338(5) _chemical_absolute_configuration ad _refine_ls_number_reflns 7294 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0477 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.43235(2) 0.30916(2) 0.131341(12) 0.01336(6) Uani 1 1 d . . . In2 In 0.44603(2) 0.67909(2) 0.873620(12) 0.01655(7) Uani 1 1 d . . . Br1 Br 0.50212(4) 0.33695(3) 0.018429(17) 0.01775(10) Uani 1 1 d . . . Br2 Br 0.36606(3) 0.28509(4) 0.244441(18) 0.02175(11) Uani 1 1 d . . . Br3 Br 0.43264(4) 0.86088(4) 0.83487(2) 0.02634(11) Uani 1 1 d . . . Br4 Br 0.27795(4) 0.64187(4) 0.94385(2) 0.03225(13) Uani 1 1 d . . . Br5 Br 0.63441(4) 0.66725(5) 0.93197(2) 0.03453(13) Uani 1 1 d . . . Br6 Br 0.44639(5) 0.54654(4) 0.789477(19) 0.03087(12) Uani 1 1 d . . . S1 S 0.22052(9) 0.33152(9) 0.08335(4) 0.0155(2) Uani 1 1 d . . . S2 S 0.41717(9) 0.51346(8) 0.15461(4) 0.0175(2) Uani 1 1 d . . . S3 S 0.42947(10) 0.10161(8) 0.12303(5) 0.0194(2) Uani 1 1 d . . . S4 S 0.66022(9) 0.28220(9) 0.15458(5) 0.0184(2) Uani 1 1 d . . . C1 C -0.0069(4) 0.3525(4) 0.12394(19) 0.0249(10) Uani 1 1 d . . . H1A H -0.0319 0.3195 0.0853 0.037 Uiso 1 1 calc R . . H1B H 0.0010 0.4273 0.1175 0.037 Uiso 1 1 calc R . . H1C H -0.0652 0.3394 0.1562 0.037 Uiso 1 1 calc R . . C2 C 0.1063(4) 0.1899(4) 0.15291(18) 0.0224(10) Uani 1 1 d . . . H2A H 0.0523 0.1731 0.1867 0.034 Uiso 1 1 calc R . . H2B H 0.1846 0.1644 0.1632 0.034 Uiso 1 1 calc R . . H2C H 0.0792 0.1569 0.1147 0.034 Uiso 1 1 calc R . . C3 C 0.1104(3) 0.3077(3) 0.14389(17) 0.0162(9) Uani 1 1 d . . . H3 H 0.1359 0.3414 0.1833 0.019 Uiso 1 1 calc R . . C4 C 0.2261(4) 0.4718(3) 0.07635(19) 0.0204(10) Uani 1 1 d . . . H4A H 0.2808 0.4895 0.0425 0.024 Uiso 1 1 calc R . . H4B H 0.1476 0.4967 0.0641 0.024 Uiso 1 1 calc R . . C5 C 0.2635(4) 0.5300(4) 0.1339(2) 0.0265(11) Uani 1 1 d . . . H5A H 0.2146 0.5067 0.1691 0.032 Uiso 1 1 calc R . . H5B H 0.2480 0.6047 0.1276 0.032 Uiso 1 1 calc R . . C6 C 0.4962(4) 0.5862(3) 0.09443(18) 0.0163(9) Uani 1 1 d . . . H6 H 0.4779 0.5559 0.0530 0.020 Uiso 1 1 calc R . . C7 C 0.6257(4) 0.5702(4) 0.10860(19) 0.0224(10) Uani 1 1 d . . . H7A H 0.6729 0.6067 0.0777 0.034 Uiso 1 1 calc R . . H7B H 0.6439 0.4961 0.1074 0.034 Uiso 1 1 calc R . . H7C H 0.6433 0.5977 0.1498 0.034 Uiso 1 1 calc R . . C8 C 0.4639(4) 0.6993(3) 0.09468(18) 0.0196(10) Uani 1 1 d . . . H8A H 0.4757 0.7278 0.1362 0.029 Uiso 1 1 calc R . . H8B H 0.3817 0.7070 0.0828 0.029 Uiso 1 1 calc R . . H8C H 0.5133 0.7366 0.0651 0.029 Uiso 1 1 calc R . . C9 C 0.3184(4) 0.0891(3) 0.0126(2) 0.0231(11) Uani 1 1 d . . . H9A H 0.3154 0.0640 -0.0302 0.035 Uiso 1 1 calc R . . H9B H 0.3083 0.1645 0.0131 0.035 Uiso 1 1 calc R . . H9C H 0.2557 0.0566 0.0367 0.035 Uiso 1 1 calc R . . C10 C 0.4609(4) -0.0536(3) 0.0368(2) 0.0273(11) Uani 1 1 d . . . H10A H 0.4014 -0.0918 0.0601 0.041 Uiso 1 1 calc R . . H10B H 0.5383 -0.0683 0.0541 0.041 Uiso 1 1 calc R . . H10C H 0.4588 -0.0752 -0.0067 0.041 Uiso 1 1 calc R . . C11 C 0.4364(4) 0.0613(3) 0.04111(17) 0.0172(9) Uani 1 1 d . . . H11 H 0.4998 0.1006 0.0196 0.021 Uiso 1 1 calc R . . C12 C 0.5752(4) 0.0754(3) 0.15278(19) 0.0238(10) Uani 1 1 d . . . H12A H 0.5728 0.0793 0.1985 0.029 Uiso 1 1 calc R . . H12B H 0.5969 0.0036 0.1415 0.029 Uiso 1 1 calc R . . C13 C 0.6705(3) 0.1486(3) 0.1294(2) 0.0225(10) Uani 1 1 d . . . H13A H 0.6694 0.1475 0.0835 0.027 Uiso 1 1 calc R . . H13B H 0.7472 0.1210 0.1427 0.027 Uiso 1 1 calc R . . C14 C 0.6791(3) 0.2772(4) 0.23881(18) 0.0202(10) Uani 1 1 d . . . H14 H 0.6126 0.2380 0.2576 0.024 Uiso 1 1 calc R . . C15 C 0.7937(4) 0.2256(4) 0.25667(18) 0.0227(11) Uani 1 1 d . . . H15A H 0.8590 0.2638 0.2382 0.034 Uiso 1 1 calc R . . H15B H 0.7942 0.1540 0.2415 0.034 Uiso 1 1 calc R . . H15C H 0.8018 0.2257 0.3018 0.034 Uiso 1 1 calc R . . C16 C 0.6750(4) 0.3893(4) 0.2608(2) 0.0348(13) Uani 1 1 d . . . H16A H 0.6841 0.3914 0.3059 0.052 Uiso 1 1 calc R . . H16B H 0.5998 0.4201 0.2493 0.052 Uiso 1 1 calc R . . H16C H 0.7385 0.4285 0.2413 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.01260(13) 0.01348(16) 0.01401(14) 0.00122(12) 0.00081(12) 0.00142(13) In2 0.01513(14) 0.01682(16) 0.01770(15) 0.00061(13) 0.00101(12) -0.00108(14) Br1 0.0209(2) 0.0164(2) 0.0160(2) -0.00093(18) 0.00495(17) -0.00158(19) Br2 0.0181(2) 0.0323(3) 0.0149(2) 0.00488(19) 0.00128(17) 0.0012(2) Br3 0.0278(3) 0.0168(2) 0.0345(3) 0.0029(2) 0.0078(2) 0.0000(2) Br4 0.0198(2) 0.0437(4) 0.0332(3) 0.0149(2) 0.0070(2) -0.0026(2) Br5 0.0186(2) 0.0586(4) 0.0264(3) 0.0052(2) -0.0044(2) -0.0002(3) Br6 0.0496(3) 0.0188(3) 0.0243(3) -0.00390(19) -0.0079(2) 0.0066(3) S1 0.0128(5) 0.0180(6) 0.0156(5) 0.0007(5) 0.0013(4) -0.0006(5) S2 0.0205(6) 0.0146(6) 0.0173(6) -0.0018(4) 0.0020(4) -0.0011(5) S3 0.0222(6) 0.0131(6) 0.0228(6) 0.0036(5) 0.0011(5) -0.0007(5) S4 0.0144(5) 0.0223(7) 0.0185(6) 0.0025(5) -0.0007(4) 0.0007(5) C1 0.022(2) 0.025(3) 0.027(2) 0.000(2) 0.007(2) 0.000(2) C2 0.023(2) 0.025(3) 0.019(2) 0.011(2) 0.0003(18) -0.002(2) C3 0.016(2) 0.019(3) 0.013(2) -0.0012(18) 0.0063(16) 0.0012(19) C4 0.018(2) 0.017(3) 0.026(2) 0.0065(19) -0.0020(19) 0.001(2) C5 0.019(2) 0.019(3) 0.042(3) -0.004(2) 0.005(2) 0.002(2) C6 0.018(2) 0.014(2) 0.016(2) -0.0024(18) 0.0004(18) -0.006(2) C7 0.020(2) 0.014(3) 0.033(3) 0.0038(19) 0.001(2) -0.003(2) C8 0.022(2) 0.014(2) 0.023(2) 0.0040(18) -0.0018(18) -0.001(2) C9 0.023(3) 0.015(3) 0.031(3) -0.001(2) -0.004(2) 0.002(2) C10 0.024(3) 0.017(3) 0.041(3) -0.008(2) 0.000(2) 0.001(2) C11 0.015(2) 0.011(2) 0.025(2) 0.0003(18) 0.0018(19) 0.000(2) C12 0.028(3) 0.016(2) 0.027(2) 0.0039(19) -0.011(2) 0.004(2) C13 0.019(2) 0.024(3) 0.025(2) -0.009(2) -0.0062(19) 0.008(2) C14 0.017(2) 0.026(3) 0.018(2) 0.0008(19) -0.0013(18) -0.001(2) C15 0.020(2) 0.029(3) 0.019(2) 0.008(2) 0.0011(19) 0.004(2) C16 0.036(3) 0.034(3) 0.035(3) -0.008(2) -0.010(2) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Br2 2.5775(5) . ? In1 Br1 2.5918(5) . ? In1 S1 2.6518(10) . ? In1 S4 2.6775(11) . ? In1 S3 2.6852(11) . ? In1 S2 2.6901(11) . ? In2 Br4 2.4963(5) . ? In2 Br3 2.4962(6) . ? In2 Br6 2.4965(5) . ? In2 Br5 2.5015(5) . ? S1 C4 1.818(4) . ? S1 C3 1.842(4) . ? S2 C5 1.827(4) . ? S2 C6 1.841(4) . ? S3 C12 1.819(4) . ? S3 C11 1.847(4) . ? S4 C13 1.812(4) . ? S4 C14 1.834(4) . ? C1 C3 1.524(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.533(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.515(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C8 1.506(6) . ? C6 C7 1.526(5) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.527(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.513(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 1.0000 . ? C12 C13 1.530(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.521(5) . ? C14 C16 1.523(6) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br2 In1 Br1 178.653(19) . . ? Br2 In1 S1 96.60(2) . . ? Br1 In1 S1 84.16(2) . . ? Br2 In1 S4 95.34(2) . . ? Br1 In1 S4 83.95(2) . . ? S1 In1 S4 167.76(3) . . ? Br2 In1 S3 86.53(3) . . ? Br1 In1 S3 94.53(3) . . ? S1 In1 S3 94.08(4) . . ? S4 In1 S3 83.96(3) . . ? Br2 In1 S2 85.52(2) . . ? Br1 In1 S2 93.45(2) . . ? S1 In1 S2 84.69(3) . . ? S4 In1 S2 98.93(3) . . ? S3 In1 S2 171.76(3) . . ? Br4 In2 Br3 109.727(19) . . ? Br4 In2 Br6 108.18(2) . . ? Br3 In2 Br6 113.582(18) . . ? Br4 In2 Br5 110.215(19) . . ? Br3 In2 Br5 106.22(2) . . ? Br6 In2 Br5 108.89(2) . . ? C4 S1 C3 104.5(2) . . ? C4 S1 In1 96.24(14) . . ? C3 S1 In1 109.21(13) . . ? C5 S2 C6 103.9(2) . . ? C5 S2 In1 97.53(15) . . ? C6 S2 In1 109.63(14) . . ? C12 S3 C11 104.29(19) . . ? C12 S3 In1 98.68(15) . . ? C11 S3 In1 110.15(13) . . ? C13 S4 C14 104.9(2) . . ? C13 S4 In1 97.51(13) . . ? C14 S4 In1 107.77(13) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 C2 112.6(3) . . ? C1 C3 S1 109.8(3) . . ? C2 C3 S1 106.1(3) . . ? C1 C3 H3 109.4 . . ? C2 C3 H3 109.4 . . ? S1 C3 H3 109.4 . . ? C5 C4 S1 115.9(3) . . ? C5 C4 H4A 108.3 . . ? S1 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? S1 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 S2 114.5(3) . . ? C4 C5 H5A 108.6 . . ? S2 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? S2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C8 C6 C7 111.6(3) . . ? C8 C6 S2 111.8(3) . . ? C7 C6 S2 105.4(3) . . ? C8 C6 H6 109.3 . . ? C7 C6 H6 109.3 . . ? S2 C6 H6 109.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C10 C11 C9 111.6(4) . . ? C10 C11 S3 110.1(3) . . ? C9 C11 S3 106.4(3) . . ? C10 C11 H11 109.6 . . ? C9 C11 H11 109.6 . . ? S3 C11 H11 109.6 . . ? C13 C12 S3 114.9(3) . . ? C13 C12 H12A 108.5 . . ? S3 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? S3 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C12 C13 S4 116.2(3) . . ? C12 C13 H13A 108.2 . . ? S4 C13 H13A 108.2 . . ? C12 C13 H13B 108.2 . . ? S4 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C16 111.3(4) . . ? C15 C14 S4 111.6(3) . . ? C16 C14 S4 105.8(3) . . ? C15 C14 H14 109.3 . . ? C16 C14 H14 109.3 . . ? S4 C14 H14 109.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # S3 In1 S2 C5 -73.1(3) . . . . ? # S3 In1 S2 C6 179.1(3) . . . . ? # S2 In1 S3 C12 -100.7(3) . . . . ? # S2 In1 S3 C11 150.5(3) . . . . ? Br2 In1 S1 C4 101.50(13) . . . . ? Br1 In1 S1 C4 -77.39(13) . . . . ? S4 In1 S1 C4 -91.2(2) . . . . ? S3 In1 S1 C4 -171.53(14) . . . . ? S2 In1 S1 C4 16.64(14) . . . . ? Br2 In1 S1 C3 -6.21(15) . . . . ? Br1 In1 S1 C3 174.91(15) . . . . ? S4 In1 S1 C3 161.1(2) . . . . ? S3 In1 S1 C3 80.76(15) . . . . ? S2 In1 S1 C3 -91.07(15) . . . . ? Br2 In1 S2 C5 -88.45(15) . . . . ? Br1 In1 S2 C5 92.42(15) . . . . ? S1 In1 S2 C5 8.62(15) . . . . ? S4 In1 S2 C5 176.83(15) . . . . ? Br2 In1 S2 C6 163.82(14) . . . . ? Br1 In1 S2 C6 -15.31(14) . . . . ? S1 In1 S2 C6 -99.11(14) . . . . ? S4 In1 S2 C6 69.10(14) . . . . ? Br2 In1 S3 C12 -85.43(14) . . . . ? Br1 In1 S3 C12 93.73(14) . . . . ? S1 In1 S3 C12 178.19(14) . . . . ? S4 In1 S3 C12 10.32(14) . . . . ? Br2 In1 S3 C11 165.79(14) . . . . ? Br1 In1 S3 C11 -15.05(15) . . . . ? S1 In1 S3 C11 69.40(15) . . . . ? S4 In1 S3 C11 -98.47(15) . . . . ? Br2 In1 S4 C13 100.35(14) . . . . ? Br1 In1 S4 C13 -80.80(14) . . . . ? S1 In1 S4 C13 -67.0(2) . . . . ? S3 In1 S4 C13 14.42(15) . . . . ? S2 In1 S4 C13 -173.36(14) . . . . ? Br2 In1 S4 C14 -8.01(16) . . . . ? Br1 In1 S4 C14 170.83(16) . . . . ? S1 In1 S4 C14 -175.3(2) . . . . ? S3 In1 S4 C14 -93.94(16) . . . . ? S2 In1 S4 C14 78.28(16) . . . . ? C4 S1 C3 C1 60.1(3) . . . . ? In1 S1 C3 C1 162.1(3) . . . . ? C4 S1 C3 C2 -178.0(3) . . . . ? In1 S1 C3 C2 -75.9(3) . . . . ? C3 S1 C4 C5 61.5(3) . . . . ? In1 S1 C4 C5 -50.2(3) . . . . ? S1 C4 C5 S2 69.7(4) . . . . ? C6 S2 C5 C4 71.0(4) . . . . ? In1 S2 C5 C4 -41.5(3) . . . . ? C5 S2 C6 C8 60.9(3) . . . . ? In1 S2 C6 C8 164.3(2) . . . . ? C5 S2 C6 C7 -177.6(3) . . . . ? In1 S2 C6 C7 -74.2(3) . . . . ? C12 S3 C11 C10 62.9(3) . . . . ? In1 S3 C11 C10 167.9(3) . . . . ? C12 S3 C11 C9 -176.0(3) . . . . ? In1 S3 C11 C9 -71.0(3) . . . . ? C11 S3 C12 C13 71.6(4) . . . . ? In1 S3 C12 C13 -41.9(3) . . . . ? S3 C12 C13 S4 67.0(4) . . . . ? C14 S4 C13 C12 64.0(3) . . . . ? In1 S4 C13 C12 -46.7(3) . . . . ? C13 S4 C14 C15 56.8(4) . . . . ? In1 S4 C14 C15 159.9(3) . . . . ? C13 S4 C14 C16 178.1(3) . . . . ? In1 S4 C14 C16 -78.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.598 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.114 #===END OF CIF ============================================================== # 08mj13 data_08mj13 _database_code_depnum_ccdc_archive 'CCDC 702288' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-05-21 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dichloro(1,4,8,11-tetrathiacyclotetradecane)indium(III) tetrachloroindate ; # 1,4,8,11-tetrathiacyclotetradecane = [14]aneS4 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Cl2 In S4 1+, Cl4 In 1-' _chemical_formula_sum 'C10 H20 Cl6 In2 S4' _chemical_formula_weight 710.84 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' S S 0.1246 0.1234 '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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic # Superceded ** _symmetry_space_group_name_H-M 'P -1' # Superceded ** # _space_group_crystal_system triclinic # _space_group_name_H-M_alt 'P -1' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.758(5) _cell_length_b 12.416(5) _cell_length_c 15.640(7) _cell_angle_alpha 92.10(2) _cell_angle_beta 90.46(2) _cell_angle_gamma 93.36(2) _cell_volume 2277.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 81711 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 3.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6879 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36707 _diffrn_reflns_av_R_equivalents 0.1024 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8916 _reflns_number_gt 5804 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+71.5279P] 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 8916 _refine_ls_number_parameters 396 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.007 _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 In1 In 0.27094(9) 0.98047(8) 0.38956(7) 0.0288(3) Uani 1 1 d . . . In2 In 0.78892(9) 0.53354(8) 0.84569(7) 0.0288(3) Uani 1 1 d . A . In3 In 0.29005(10) 0.95820(9) 0.88616(8) 0.0349(3) Uani 1 1 d . . . In4 In 0.24503(9) 0.43215(9) 0.66615(7) 0.0321(3) Uani 1 1 d . . . Cl1 Cl 0.3964(4) 1.0825(3) 0.2966(3) 0.0460(11) Uani 1 1 d . . . Cl2 Cl 0.2508(3) 1.1183(3) 0.4997(3) 0.0394(10) Uani 1 1 d . . . Cl3 Cl 0.6423(4) 0.4032(3) 0.8896(3) 0.0466(11) Uani 1 1 d . . . Cl4 Cl 0.9372(3) 0.4158(3) 0.8031(3) 0.0353(9) Uani 1 1 d . . . Cl5 Cl 0.3203(4) 0.7920(3) 0.9479(3) 0.0461(11) Uani 1 1 d . . . Cl6 Cl 0.4482(4) 1.0803(4) 0.8894(4) 0.0634(14) Uani 1 1 d . . . Cl7 Cl 0.2166(5) 0.9153(4) 0.7473(3) 0.0577(13) Uani 1 1 d . . . Cl8 Cl 0.1404(4) 1.0353(4) 0.9639(3) 0.0465(11) Uani 1 1 d . . . Cl9 Cl 0.4010(4) 0.4578(4) 0.5724(3) 0.0491(11) Uani 1 1 d . . . Cl10 Cl 0.0812(3) 0.4497(3) 0.5815(3) 0.0348(9) Uani 1 1 d . . . Cl11 Cl 0.2519(4) 0.2620(3) 0.7259(3) 0.0430(10) Uani 1 1 d . . . Cl12 Cl 0.2592(4) 0.5724(4) 0.7700(3) 0.0501(12) Uani 1 1 d . . . S1 S 0.1130(3) 0.8570(3) 0.4746(3) 0.0322(9) Uani 1 1 d . . . S2 S 0.0850(3) 1.0224(3) 0.3060(3) 0.0310(9) Uani 1 1 d . . . S3 S 0.2830(3) 0.8050(3) 0.2857(3) 0.0318(9) Uani 1 1 d . . . S4 S 0.4326(3) 0.8812(3) 0.4634(3) 0.0376(10) Uani 1 1 d . . . S5 S 0.6502(3) 0.6930(3) 0.8724(3) 0.0363(10) Uani 1 1 d D A . S6 S 0.6980(4) 0.5323(3) 0.6934(3) 0.0364(10) Uani 1 1 d . . . S7 S 0.9213(3) 0.7097(3) 0.8123(3) 0.0325(9) Uani 1 1 d . A . S8 S 0.8775(4) 0.5786(4) 0.9972(3) 0.0522(13) Uani 1 1 d D . . C1 C 0.0169(13) 0.8240(13) 0.3843(11) 0.035(4) Uani 1 1 d . . . H1A H 0.0568 0.7817 0.3402 0.042 Uiso 1 1 calc R . . H1B H -0.0495 0.7788 0.4036 0.042 Uiso 1 1 calc R . . C2 C -0.0244(12) 0.9257(13) 0.3454(12) 0.038(4) Uani 1 1 d . . . H2A H -0.0694 0.9637 0.3891 0.045 Uiso 1 1 calc R . . H2B H -0.0767 0.9034 0.2972 0.045 Uiso 1 1 calc R . . C3 C 0.1013(15) 0.9895(12) 0.1928(10) 0.039(4) Uani 1 1 d . . . H3A H 0.0270 0.9985 0.1645 0.047 Uiso 1 1 calc R . . H3B H 0.1562 1.0443 0.1698 0.047 Uiso 1 1 calc R . . C4 C 0.1404(15) 0.8778(13) 0.1645(11) 0.041(4) Uani 1 1 d . . . H4A H 0.0940 0.8226 0.1951 0.050 Uiso 1 1 calc R . . H4B H 0.1232 0.8663 0.1027 0.050 Uiso 1 1 calc R . . C5 C 0.2659(16) 0.8579(13) 0.1791(11) 0.045(5) Uani 1 1 d . . . H5A H 0.3128 0.9263 0.1745 0.054 Uiso 1 1 calc R . . H5B H 0.2914 0.8055 0.1352 0.054 Uiso 1 1 calc R . . C6 C 0.4348(15) 0.7893(15) 0.2980(11) 0.044(4) Uani 1 1 d . . . H6A H 0.4572 0.7268 0.2622 0.053 Uiso 1 1 calc R . . H6B H 0.4779 0.8547 0.2787 0.053 Uiso 1 1 calc R . . C7 C 0.4617(18) 0.7727(19) 0.3875(16) 0.076(7) Uani 1 1 d . . . H7A H 0.5437 0.7592 0.3918 0.092 Uiso 1 1 calc R . . H7B H 0.4184 0.7064 0.4049 0.092 Uiso 1 1 calc R . . C8 C 0.3629(19) 0.830(2) 0.5549(15) 0.074(7) Uani 1 1 d . . . H8A H 0.4233 0.8120 0.5957 0.089 Uiso 1 1 calc R . . H8B H 0.3227 0.8897 0.5818 0.089 Uiso 1 1 calc R . . C9 C 0.2808(15) 0.7354(14) 0.5490(12) 0.046(4) Uani 1 1 d . . . H9A H 0.2491 0.7264 0.6070 0.055 Uiso 1 1 calc R . . H9B H 0.3251 0.6715 0.5362 0.055 Uiso 1 1 calc R . . C10 C 0.1773(16) 0.7286(13) 0.4853(12) 0.047(5) Uani 1 1 d . . . H10A H 0.1189 0.6747 0.5053 0.057 Uiso 1 1 calc R . . H10B H 0.2031 0.7030 0.4284 0.057 Uiso 1 1 calc R . . C11 C 0.5426(15) 0.6461(15) 0.7937(12) 0.050(5) Uani 1 1 d . . . H11A H 0.5100 0.5738 0.8081 0.060 Uiso 1 1 calc R . . H11B H 0.4802 0.6963 0.7934 0.060 Uiso 1 1 calc R . . C12 C 0.5981(16) 0.6406(14) 0.7051(11) 0.045(5) Uani 1 1 d . . . H12A H 0.6394 0.7107 0.6950 0.053 Uiso 1 1 calc R . . H12B H 0.5376 0.6290 0.6608 0.053 Uiso 1 1 calc R . . C13 C 0.8047(16) 0.5825(16) 0.6198(13) 0.055(5) Uani 1 1 d . . . H13A H 0.8568 0.5239 0.6088 0.066 Uiso 1 1 calc R . . H13B H 0.7650 0.5937 0.5650 0.066 Uiso 1 1 calc R . . C14 C 0.8789(14) 0.6854(13) 0.6412(11) 0.039(4) Uani 1 1 d . . . H14A H 0.8292 0.7415 0.6633 0.047 Uiso 1 1 calc R . . H14B H 0.9131 0.7115 0.5875 0.047 Uiso 1 1 calc R . . C15 C 0.9768(14) 0.6742(13) 0.7076(10) 0.037(4) Uani 1 1 d . . . H15A H 1.0433 0.7231 0.6943 0.045 Uiso 1 1 calc R . . H15B H 1.0011 0.5991 0.7062 0.045 Uiso 1 1 calc R . . C16 C 1.0329(15) 0.6831(13) 0.8869(11) 0.042(4) Uani 1 1 d . . . H16A H 1.0622 0.6114 0.8732 0.051 Uiso 1 1 calc R A . H16B H 1.0967 0.7383 0.8827 0.051 Uiso 1 1 calc R . . C17 C 0.9844(17) 0.6858(13) 0.9780(13) 0.053(5) Uani 1 1 d . A . H17A H 0.9506 0.7561 0.9890 0.064 Uiso 1 1 calc R . . H17B H 1.0479 0.6810 1.0194 0.064 Uiso 1 1 calc R . . C18A C 0.760(3) 0.604(4) 1.069(2) 0.064(16) Uiso 0.43(4) 1 d PD A 1 H18A H 0.7134 0.5360 1.0745 0.076 Uiso 0.43(4) 1 calc PR A 1 H18B H 0.7917 0.6263 1.1258 0.076 Uiso 0.43(4) 1 calc PR A 1 C19A C 0.681(2) 0.692(3) 1.040(2) 0.030(10) Uiso 0.43(4) 1 d PD A 1 H19A H 0.6457 0.7221 1.0917 0.036 Uiso 0.43(4) 1 calc PR A 1 H19B H 0.7301 0.7504 1.0156 0.036 Uiso 0.43(4) 1 calc PR A 1 C18B C 0.779(2) 0.672(2) 1.050(2) 0.054(11) Uiso 0.57(4) 1 d PD A 2 H18C H 0.8037 0.6879 1.1098 0.064 Uiso 0.57(4) 1 calc PR A 2 H18D H 0.7819 0.7412 1.0198 0.064 Uiso 0.57(4) 1 calc PR A 2 C19B C 0.655(2) 0.623(3) 1.0481(18) 0.051(10) Uiso 0.57(4) 1 d PD A 2 H19C H 0.6569 0.5430 1.0435 0.061 Uiso 0.57(4) 1 calc PR A 2 H19D H 0.6183 0.6418 1.1027 0.061 Uiso 0.57(4) 1 calc PR A 2 C20 C 0.5860(14) 0.6608(13) 0.9748(9) 0.048(5) Uani 1 1 d D . . H20A H 0.5187 0.7034 0.9858 0.057 Uiso 1 1 calc R A 1 H20B H 0.5626 0.5830 0.9765 0.057 Uiso 1 1 calc R 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 In1 0.0279(6) 0.0198(5) 0.0387(7) -0.0033(5) -0.0007(5) 0.0041(4) In2 0.0306(6) 0.0223(5) 0.0343(6) 0.0017(5) 0.0018(5) 0.0069(5) In3 0.0345(6) 0.0313(6) 0.0389(7) -0.0018(5) 0.0002(5) 0.0048(5) In4 0.0296(6) 0.0311(6) 0.0357(7) -0.0029(5) -0.0005(5) 0.0062(5) Cl1 0.045(2) 0.024(2) 0.068(3) 0.002(2) 0.014(2) -0.0030(18) Cl2 0.039(2) 0.030(2) 0.048(3) -0.0132(18) -0.0034(19) 0.0070(18) Cl3 0.052(3) 0.0226(19) 0.066(3) 0.0034(19) 0.019(2) 0.0023(18) Cl4 0.035(2) 0.0253(19) 0.047(2) -0.0026(17) 0.0051(18) 0.0124(16) Cl5 0.046(3) 0.036(2) 0.057(3) 0.003(2) -0.015(2) 0.0089(19) Cl6 0.050(3) 0.066(3) 0.071(4) -0.006(3) 0.019(3) -0.016(3) Cl7 0.074(3) 0.056(3) 0.044(3) -0.004(2) -0.014(2) 0.022(3) Cl8 0.041(2) 0.046(3) 0.054(3) -0.003(2) 0.012(2) 0.012(2) Cl9 0.032(2) 0.059(3) 0.055(3) -0.007(2) 0.011(2) 0.003(2) Cl10 0.034(2) 0.037(2) 0.034(2) 0.0013(17) -0.0025(17) 0.0044(17) Cl11 0.052(3) 0.031(2) 0.046(3) 0.0011(19) -0.010(2) 0.0042(19) Cl12 0.035(2) 0.046(3) 0.067(3) -0.027(2) 0.000(2) 0.005(2) S1 0.032(2) 0.029(2) 0.036(2) 0.0002(17) 0.0036(17) 0.0073(17) S2 0.032(2) 0.0264(19) 0.035(2) 0.0005(17) -0.0054(17) 0.0081(16) S3 0.037(2) 0.0198(18) 0.039(2) -0.0019(16) 0.0020(18) 0.0059(16) S4 0.031(2) 0.031(2) 0.051(3) -0.0075(19) -0.0090(19) 0.0077(17) S5 0.029(2) 0.025(2) 0.055(3) -0.0008(19) -0.0024(19) 0.0045(17) S6 0.042(2) 0.026(2) 0.042(3) -0.0028(18) -0.0075(19) 0.0062(18) S7 0.036(2) 0.0238(19) 0.038(2) -0.0014(17) 0.0013(18) 0.0020(16) S8 0.054(3) 0.067(3) 0.038(3) 0.008(2) -0.002(2) 0.021(3) C1 0.025(8) 0.035(9) 0.044(10) -0.001(8) -0.001(7) 0.000(7) C2 0.015(7) 0.037(9) 0.060(12) -0.004(8) -0.014(7) -0.010(7) C3 0.054(11) 0.027(8) 0.038(10) 0.015(7) 0.014(8) 0.003(8) C4 0.059(11) 0.029(9) 0.034(10) -0.005(7) -0.010(8) -0.002(8) C5 0.068(13) 0.031(9) 0.037(10) -0.003(8) 0.001(9) 0.018(9) C6 0.046(10) 0.048(11) 0.037(10) -0.015(8) 0.003(8) 0.009(9) C7 0.039(12) 0.078(16) 0.11(2) -0.021(15) -0.009(12) 0.019(11) C8 0.056(14) 0.093(18) 0.076(17) 0.012(14) -0.014(12) 0.019(13) C9 0.048(11) 0.042(10) 0.050(12) 0.006(9) -0.002(9) 0.009(9) C10 0.062(12) 0.028(9) 0.051(12) 0.004(8) 0.000(9) 0.002(8) C11 0.039(10) 0.050(11) 0.063(13) 0.013(10) -0.004(9) 0.019(9) C12 0.061(12) 0.041(10) 0.034(10) 0.001(8) -0.011(8) 0.026(9) C13 0.050(12) 0.059(12) 0.056(13) 0.009(10) -0.022(10) 0.008(10) C14 0.042(10) 0.041(10) 0.034(10) 0.010(8) -0.014(8) -0.012(8) C15 0.046(10) 0.037(9) 0.029(9) -0.003(7) 0.009(7) 0.001(8) C16 0.045(10) 0.029(9) 0.052(12) -0.001(8) 0.000(8) -0.001(8) C17 0.072(13) 0.029(9) 0.060(13) -0.004(9) -0.007(10) 0.023(9) C20 0.054(11) 0.029(9) 0.062(13) 0.007(8) 0.020(9) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Cl2 2.406(4) . ? In1 Cl1 2.418(4) . ? In1 S4 2.610(4) . ? In1 S2 2.626(4) . ? In1 S3 2.681(4) . ? In1 S1 2.725(4) . ? In2 Cl3 2.416(4) . ? In2 Cl4 2.421(4) . ? In2 S6 2.602(4) . ? In2 S8 2.609(5) . ? In2 S5 2.662(4) . ? In2 S7 2.679(4) . ? In3 Cl6 2.328(5) . ? In3 Cl5 2.355(4) . ? In3 Cl7 2.361(5) . ? In3 Cl8 2.375(4) . ? In4 Cl12 2.336(4) . ? In4 Cl11 2.347(4) . ? In4 Cl10 2.354(4) . ? In4 Cl9 2.372(4) . ? S1 C10 1.817(17) . ? S1 C1 1.822(16) . ? S2 C3 1.816(17) . ? S2 C2 1.834(16) . ? S3 C6 1.815(18) . ? S3 C5 1.829(17) . ? S4 C8 1.78(2) . ? S4 C7 1.81(2) . ? S5 C11 1.815(19) . ? S5 C20 1.823(13) . ? S6 C13 1.81(2) . ? S6 C12 1.842(16) . ? S7 C16 1.801(18) . ? S7 C15 1.817(16) . ? S8 C17 1.81(2) . ? S8 C18A 1.818(19) . ? S8 C18B 1.864(17) . ? C1 C2 1.52(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.54(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.53(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.46(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.47(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.56(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.54(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.53(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.56(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.54(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18A C19A 1.542(19) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A C20 1.529(18) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C18B C19B 1.543(19) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B C20 1.509(18) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # C18A S8 C18B 28.9(14) . . ? # C18B C19B H19C 109.1 . . ? # C19B C20 C19A 34.7(15) . . ? Cl2 In1 Cl1 98.17(15) . . ? Cl2 In1 S4 97.30(14) . . ? Cl1 In1 S4 95.28(15) . . ? Cl2 In1 S2 94.86(13) . . ? Cl1 In1 S2 94.25(15) . . ? S4 In1 S2 163.31(13) . . ? Cl2 In1 S3 170.97(15) . . ? Cl1 In1 S3 90.29(14) . . ? S4 In1 S3 78.67(13) . . ? S2 In1 S3 87.62(13) . . ? Cl2 In1 S1 87.26(14) . . ? Cl1 In1 S1 172.19(15) . . ? S4 In1 S1 89.56(14) . . ? S2 In1 S1 79.63(13) . . ? S3 In1 S1 84.65(13) . . ? Cl3 In2 Cl4 100.84(14) . . ? Cl3 In2 S6 90.36(16) . . ? Cl4 In2 S6 94.06(14) . . ? Cl3 In2 S8 96.96(18) . . ? Cl4 In2 S8 93.95(15) . . ? S6 In2 S8 167.95(15) . . ? Cl3 In2 S5 90.62(14) . . ? Cl4 In2 S5 167.88(14) . . ? S6 In2 S5 81.83(13) . . ? S8 In2 S5 88.51(15) . . ? Cl3 In2 S7 167.34(13) . . ? Cl4 In2 S7 91.65(13) . . ? S6 In2 S7 90.83(14) . . ? S8 In2 S7 79.95(16) . . ? S5 In2 S7 77.08(13) . . ? Cl6 In3 Cl5 114.68(19) . . ? Cl6 In3 Cl7 114.0(2) . . ? Cl5 In3 Cl7 106.01(17) . . ? Cl6 In3 Cl8 108.93(18) . . ? Cl5 In3 Cl8 106.52(17) . . ? Cl7 In3 Cl8 106.13(18) . . ? Cl12 In4 Cl11 112.20(18) . . ? Cl12 In4 Cl10 109.11(15) . . ? Cl11 In4 Cl10 113.34(15) . . ? Cl12 In4 Cl9 107.45(17) . . ? Cl11 In4 Cl9 108.92(17) . . ? Cl10 In4 Cl9 105.44(16) . . ? C10 S1 C1 100.4(8) . . ? C10 S1 In1 104.5(6) . . ? C1 S1 In1 97.3(5) . . ? C3 S2 C2 106.6(8) . . ? C3 S2 In1 109.7(6) . . ? C2 S2 In1 104.4(5) . . ? C6 S3 C5 105.2(9) . . ? C6 S3 In1 97.3(6) . . ? C5 S3 In1 103.2(5) . . ? C8 S4 C7 110.7(12) . . ? C8 S4 In1 102.1(7) . . ? C7 S4 In1 103.8(7) . . ? C11 S5 C20 104.3(9) . . ? C11 S5 In2 96.8(6) . . ? C20 S5 In2 102.8(5) . . ? C13 S6 C12 105.0(9) . . ? C13 S6 In2 108.6(6) . . ? C12 S6 In2 101.8(6) . . ? C16 S7 C15 105.0(8) . . ? C16 S7 In2 95.5(6) . . ? C15 S7 In2 101.9(6) . . ? C17 S8 C18A 119.6(18) . . ? C17 S8 C18B 93.2(11) . . ? C17 S8 In2 103.4(7) . . ? C18A S8 In2 106.9(16) . . ? C18B S8 In2 105.0(11) . . ? C2 C1 S1 111.3(11) . . ? C2 C1 H1A 109.4 . . ? S1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? S1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 S2 116.9(10) . . ? C1 C2 H2A 108.1 . . ? S2 C2 H2A 108.1 . . ? C1 C2 H2B 108.1 . . ? S2 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C4 C3 S2 119.5(11) . . ? C4 C3 H3A 107.4 . . ? S2 C3 H3A 107.4 . . ? C4 C3 H3B 107.4 . . ? S2 C3 H3B 107.4 . . ? H3A C3 H3B 107.0 . . ? C5 C4 C3 116.8(14) . . ? C5 C4 H4A 108.1 . . ? C3 C4 H4A 108.1 . . ? C5 C4 H4B 108.1 . . ? C3 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C5 S3 108.8(12) . . ? C4 C5 H5A 109.9 . . ? S3 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 . . ? S3 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C7 C6 S3 109.7(13) . . ? C7 C6 H6A 109.7 . . ? S3 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? S3 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 C7 S4 116.7(15) . . ? C6 C7 H7A 108.1 . . ? S4 C7 H7A 108.1 . . ? C6 C7 H7B 108.1 . . ? S4 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C9 C8 S4 122.1(17) . . ? C9 C8 H8A 106.8 . . ? S4 C8 H8A 106.8 . . ? C9 C8 H8B 106.8 . . ? S4 C8 H8B 106.8 . . ? H8A C8 H8B 106.7 . . ? C8 C9 C10 122.2(16) . . ? C8 C9 H9A 106.8 . . ? C10 C9 H9A 106.8 . . ? C8 C9 H9B 106.8 . . ? C10 C9 H9B 106.8 . . ? H9A C9 H9B 106.6 . . ? C9 C10 S1 113.0(12) . . ? C9 C10 H10A 109.0 . . ? S1 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? S1 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 S5 108.8(13) . . ? C12 C11 H11A 109.9 . . ? S5 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? S5 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 S6 113.1(11) . . ? C11 C12 H12A 109.0 . . ? S6 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? S6 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 S6 121.2(14) . . ? C14 C13 H13A 107.0 . . ? S6 C13 H13A 107.0 . . ? C14 C13 H13B 107.0 . . ? S6 C13 H13B 107.0 . . ? H13A C13 H13B 106.8 . . ? C13 C14 C15 115.8(14) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 S7 107.1(11) . . ? C14 C15 H15A 110.3 . . ? S7 C15 H15A 110.3 . . ? C14 C15 H15B 110.3 . . ? S7 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C17 C16 S7 108.8(12) . . ? C17 C16 H16A 109.9 . . ? S7 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? S7 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C16 C17 S8 114.2(13) . . ? C16 C17 H17A 108.7 . . ? S8 C17 H17A 108.7 . . ? C16 C17 H17B 108.7 . . ? S8 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C19A C18A S8 115(2) . . ? C19A C18A H18A 108.5 . . ? S8 C18A H18A 108.5 . . ? C19A C18A H18B 108.5 . . ? S8 C18A H18B 108.5 . . ? H18A C18A H18B 107.5 . . ? C20 C19A C18A 119(3) . . ? C20 C19A H19A 107.5 . . ? C18A C19A H19A 107.5 . . ? C20 C19A H19B 107.5 . . ? C18A C19A H19B 107.5 . . ? H19A C19A H19B 107.0 . . ? C19B C18B S8 111.0(19) . . ? C19B C18B H18C 109.4 . . ? S8 C18B H18C 109.4 . . ? C19B C18B H18D 109.4 . . ? S8 C18B H18D 109.4 . . ? H18C C18B H18D 108.0 . . ? C20 C19B C18B 113(2) . . ? C20 C19B H19C 109.1 . . ? C20 C19B H19D 109.1 . . ? C18B C19B H19D 109.1 . . ? H19C C19B H19D 107.8 . . ? C19B C20 S5 121.8(15) . . ? C19A C20 S5 103.6(17) . . ? C19B C20 H20A 120.6 . . ? C19A C20 H20A 111.0 . . ? S5 C20 H20A 111.0 . . ? C19B C20 H20B 76.6 . . ? C19A C20 H20B 111.0 . . ? S5 C20 H20B 111.0 . . ? H20A C20 H20B 109.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.636 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.244 #===END OF CIF ============================================================== # 08mj34 data_08mj34 _database_code_depnum_ccdc_archive 'CCDC 702289' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-08-04 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tribromo(dimethylselenide-Se)indium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Br3 In Se' _chemical_formula_sum 'C2 H6 Br3 In Se' _chemical_formula_weight 463.58 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 13.449(5) _cell_length_b 10.233(3) _cell_length_c 6.787(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 934.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6074 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 19.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4513 # 0.3365 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6608 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1126 _reflns_number_gt 927 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+1.0749P] 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 1126 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.23521(4) 0.2500 0.16899(8) 0.01517(16) Uani 1 2 d S . . Br1 Br 0.42030(5) 0.2500 0.15896(12) 0.0199(2) Uani 1 2 d S . . Br2 Br 0.17107(3) 0.45311(5) 0.32882(8) 0.01873(17) Uani 1 1 d . . . Se1 Se 0.16410(5) 0.2500 -0.19445(11) 0.01499(19) Uani 1 2 d S . . C1 C 0.0685(4) 0.3913(5) -0.1720(8) 0.0222(12) Uani 1 1 d . . . H1A H 0.0300 0.3976 -0.2942 0.033 Uiso 1 1 calc R . . H1B H 0.1038 0.4737 -0.1490 0.033 Uiso 1 1 calc R . . H1C H 0.0235 0.3739 -0.0615 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.0145(3) 0.0161(3) 0.0149(3) 0.000 -0.0009(2) 0.000 Br1 0.0138(4) 0.0206(4) 0.0253(5) 0.000 -0.0004(3) 0.000 Br2 0.0190(3) 0.0189(3) 0.0183(3) -0.00297(19) 0.0011(2) 0.00049(19) Se1 0.0158(4) 0.0161(4) 0.0131(4) 0.000 0.0002(3) 0.000 C1 0.024(3) 0.020(3) 0.023(3) -0.002(2) -0.005(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Br1 2.4901(12) . ? In1 Br2 2.4981(7) . ? In1 Br2 2.4981(7) 7_565 ? In1 Se1 2.6455(11) . ? Se1 C1 1.941(5) 7_565 ? Se1 C1 1.941(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 In1 Br2 110.92(2) . . ? Br1 In1 Br2 110.92(2) . 7_565 ? Br2 In1 Br2 112.61(4) . 7_565 ? Br1 In1 Se1 109.63(3) . . ? Br2 In1 Se1 106.26(2) . . ? Br2 In1 Se1 106.26(2) 7_565 . ? C1 Se1 C1 96.3(3) 7_565 . ? C1 Se1 In1 99.58(17) 7_565 . ? C1 Se1 In1 99.58(17) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.054 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.260 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================