# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12kg28r3 _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-03-14 _audit_update_record ; 2013-11-21 Revised refinement and added comments about working with smaller cell. mw ; _chemical_name_systematic ; (1,2-bis[(ethylthio)methyl]benzene)bis(trichloroaluminium(III)) ; # o-C6H4(CH2SEt)2 = C12H18S2 # 1,2-bis(ethylthiomethyl)benzene # 1,2-bis((ethylthio)methyl)benzene # 1,2-bis[(ethylthio)methyl]benzene (iLab IUPAC defaults) # 1,2-bis[(ethylsulfanyl)methyl]benzene (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 Al2 Cl6 S2' _chemical_formula_sum 'C12 H18 Al2 Cl6 S2' _chemical_formula_structural '(C12 H18 S2) (Al Cl3)2' _chemical_formula_weight 493.04 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' 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 18.7450(16) _cell_length_b 10.810(10) _cell_length_c 13.608(12) _cell_angle_alpha 90.00 _cell_angle_beta 125.7790(10) _cell_angle_gamma 90.00 _cell_volume 2237(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8048 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 31.3 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.473 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7044 _diffrn_reflns_av_R_equivalents 0.0393 # _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1785 _reflns_number_gt 1598 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _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. The original monoclinic cell had b = 32.43(2) Angstrom with layers with k not equal to 3n being very weak. That is k=1,2,4,5, etc being weak. The monoclinic cell used and reported here has b' = b/3 with k != 3n removed and a smaller cell (32.43(2)/3 = 10.81(1) A). 33429 reflections were measured and after removing hkl layers with k != 3n there remained 9449 reflections. We are therefore looking at an averaged structure. It looks like a modulated structure analogous to the reported Ga compound. The largest Q-peak (1.78) is close (0.56 Ang) to Cl1. Regretably the crystal size was not available and attempts to obtain more crystals were not successful. ; _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^)+(0.0038P)^2^+50.1494P] 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 1785 _refine_ls_number_parameters 100 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _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 Al1 Al 0.1304(2) 0.6828(3) 0.2097(3) 0.0613(9) Uani 1 1 d . . . Cl1 Cl 0.2178(3) 0.8098(4) 0.3442(3) 0.147(2) Uani 1 1 d . . . Cl2 Cl 0.17178(13) 0.6162(2) 0.10384(17) 0.0537(6) Uani 1 1 d . . . Cl3 Cl -0.0037(2) 0.7371(2) 0.1038(3) 0.0817(10) Uani 1 1 d . . . S1 S 0.13049(12) 0.5080(2) 0.31442(17) 0.0446(6) Uani 1 1 d . . . C1 C 0.3116(6) 0.4752(16) 0.4577(10) 0.144(8) Uani 1 1 d . . . H1A H 0.3608 0.4214 0.4790 0.216 Uiso 1 1 calc R . . H1B H 0.3121 0.4887 0.5293 0.216 Uiso 1 1 calc R . . H1C H 0.3173 0.5548 0.4285 0.216 Uiso 1 1 calc R . . C2 C 0.2258(5) 0.4145(11) 0.3591(8) 0.070(3) Uani 1 1 d . . . H2A H 0.2210 0.3331 0.3882 0.083 Uiso 1 1 calc R . . H2B H 0.2260 0.3999 0.2874 0.083 Uiso 1 1 calc R . . C3 C 0.0434(4) 0.4166(7) 0.1856(6) 0.041(2) Uani 1 1 d . . . H3A H -0.0106 0.4676 0.1379 0.049 Uiso 1 1 calc R . . H3B H 0.0617 0.3960 0.1325 0.049 Uiso 1 1 calc R . . C4 C 0.0223(5) 0.2989(7) 0.2224(7) 0.053(3) Uani 1 1 d D . . C5 C 0.0449(7) 0.1867(9) 0.1973(8) 0.091(4) Uani 1 1 d D . . H5 H 0.0756 0.1857 0.1613 0.110 Uiso 1 1 calc R . . C6 C 0.0226(11) 0.0763(10) 0.2247(13) 0.158(13) Uani 1 1 d D . . H6 H 0.0389 0.0000 0.2083 0.190 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 Al1 0.091(2) 0.0547(19) 0.0735(19) -0.0401(15) 0.0679(18) -0.0337(15) Cl1 0.241(4) 0.159(3) 0.154(3) -0.135(3) 0.180(3) -0.167(3) Cl2 0.0548(12) 0.0717(16) 0.0412(11) -0.0233(10) 0.0317(10) -0.0042(11) Cl3 0.131(2) 0.0382(16) 0.139(3) 0.0125(15) 0.114(2) 0.0278(14) S1 0.0321(10) 0.0595(15) 0.0363(10) -0.0211(9) 0.0167(8) -0.0122(9) C1 0.038(5) 0.28(2) 0.083(8) -0.114(11) 0.017(5) -0.018(9) C2 0.038(5) 0.110(9) 0.048(5) -0.011(5) 0.018(4) 0.015(5) C3 0.025(4) 0.039(5) 0.037(4) -0.014(3) 0.005(3) 0.005(3) C4 0.038(5) 0.020(5) 0.040(5) -0.006(3) -0.011(3) 0.006(3) C5 0.103(8) 0.034(7) 0.041(5) -0.010(4) -0.011(5) 0.033(6) C6 0.20(2) 0.030(7) 0.062(12) -0.007(6) -0.029(9) 0.041(10) _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 Al1 Cl1 2.100(4) . ? Al1 Cl3 2.122(4) . ? Al1 Cl2 2.122(3) . ? Al1 S1 2.366(4) . ? S1 C2 1.820(9) . ? S1 C3 1.836(7) . ? C1 C2 1.515(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.502(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.392(11) . ? C4 C4 1.414(18) 2 ? C5 C6 1.385(13) . ? C5 H5 0.9500 . ? C6 C6 1.370(18) 2 ? C6 H6 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Al1 Cl3 114.9(2) . . ? Cl1 Al1 Cl2 113.91(16) . . ? Cl3 Al1 Cl2 112.99(17) . . ? Cl1 Al1 S1 105.75(18) . . ? Cl3 Al1 S1 102.32(14) . . ? Cl2 Al1 S1 105.42(15) . . ? C2 S1 C3 99.8(4) . . ? C2 S1 Al1 107.5(4) . . ? C3 S1 Al1 99.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 112.4(8) . . ? C1 C2 H2A 109.1 . . ? S1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? S1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S1 113.4(5) . . ? C4 C3 H3A 108.9 . . ? S1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C4 119.3(7) . 2 ? C5 C4 C3 118.7(9) . . ? C4 C4 C3 122.0(4) 2 . ? C6 C5 C4 120.1(11) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C6 C6 C5 120.5(6) 2 . ? C6 C6 H6 119.7 2 . ? C5 C6 H6 119.7 . . ? 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 C3 S1 C2 C1 173.6(9) . . . . ? Al1 S1 C2 C1 70.1(9) . . . . ? C2 S1 C3 C4 73.8(6) . . . . ? Al1 S1 C3 C4 -176.4(5) . . . . ? S1 C3 C4 C5 -110.7(7) . . . . ? S1 C3 C4 C4 71.6(10) . . . 2 ? C4 C4 C5 C6 0.8(15) 2 . . . ? C3 C4 C5 C6 -176.9(10) . . . . ? C4 C5 C6 C6 1(3) . . . 2 ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.779 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.122 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; #===END OF CIF=============================================================== #===END OF FILE ============================================================= _database_code_depnum_ccdc_archive 'CCDC 966342' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12kg24c _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-06-01 # yyyy-mm-dd _chemical_name_systematic ; dimethylsulfonium tetrachloroaluminate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H7 S 1+, Al Cl4 1-' _chemical_formula_sum 'C2 H7 Al Cl4 S' _chemical_formula_weight 231.92 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.378(3) _cell_length_b 10.908(2) _cell_length_c 12.374(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.260(3) _cell_angle_gamma 90.00 _cell_volume 1940.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8788 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.558 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10988 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4412 _reflns_number_gt 3810 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Shelxl-97. Used DFIX with FVAR 2 to restrain S-H distances to be equal. ; _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^)+(0.0112P)^2^+1.6716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (C-H) difmap (S-H)' _refine_ls_hydrogen_treatment mixed # constr (C-H) refxyz (S-H) _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4412 _refine_ls_number_parameters 152 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.37653(5) 0.72924(7) 0.90013(6) 0.02626(17) Uani 1 1 d . . . Al2 Al 0.12454(5) 0.22953(7) 0.02876(6) 0.02465(16) Uani 1 1 d . . . S1 S 0.40192(5) 0.14094(6) 0.87145(5) 0.03462(16) Uani 1 1 d D . . S2 S 0.13652(6) 0.62087(6) 0.64329(5) 0.03683(17) Uani 1 1 d D . . Cl1 Cl 0.49583(4) 0.84438(6) 0.88012(5) 0.03093(15) Uani 1 1 d . . . Cl2 Cl 0.25590(4) 0.84347(7) 0.90345(6) 0.03739(16) Uani 1 1 d . . . Cl3 Cl 0.38833(7) 0.62811(10) 1.04500(8) 0.0703(3) Uani 1 1 d . . . Cl4 Cl 0.36850(5) 0.60702(7) 0.76565(7) 0.0485(2) Uani 1 1 d . . . Cl5 Cl 0.12945(7) 0.42265(7) 0.04599(7) 0.0528(2) Uani 1 1 d . . . Cl6 Cl 0.24521(4) 0.15030(6) 0.10319(5) 0.03024(15) Uani 1 1 d . . . Cl7 Cl 0.12452(5) 0.18280(8) -0.13918(5) 0.04347(19) Uani 1 1 d . . . Cl8 Cl 0.00220(4) 0.15550(6) 0.10008(5) 0.03141(15) Uani 1 1 d . . . C1 C 0.35672(19) 0.0931(3) 0.7436(2) 0.0330(6) Uani 1 1 d . . . H1A H 0.3704 0.0059 0.7327 0.050 Uiso 1 1 calc R . . H1B H 0.3857 0.1412 0.6860 0.050 Uiso 1 1 calc R . . H1C H 0.2893 0.1058 0.7420 0.050 Uiso 1 1 calc R . . C2 C 0.37079(19) 0.2998(2) 0.8769(2) 0.0330(6) Uani 1 1 d . . . H2A H 0.3929 0.3351 0.9451 0.049 Uiso 1 1 calc R . . H2B H 0.3030 0.3078 0.8724 0.049 Uiso 1 1 calc R . . H2C H 0.3994 0.3432 0.8163 0.049 Uiso 1 1 calc R . . C3 C 0.1249(2) 0.7836(3) 0.6459(2) 0.0361(6) Uani 1 1 d . . . H3A H 0.1405 0.8172 0.5748 0.054 Uiso 1 1 calc R . . H3B H 0.1671 0.8178 0.7005 0.054 Uiso 1 1 calc R . . H3C H 0.0606 0.8053 0.6639 0.054 Uiso 1 1 calc R . . C4 C 0.1062(2) 0.5727(3) 0.7767(2) 0.0338(6) Uani 1 1 d . . . H4A H 0.1110 0.4833 0.7816 0.051 Uiso 1 1 calc R . . H4B H 0.0423 0.5981 0.7924 0.051 Uiso 1 1 calc R . . H4C H 0.1488 0.6104 0.8290 0.051 Uiso 1 1 calc R . . H5 H 0.4886(18) 0.141(3) 0.862(3) 0.050 Uiso 1 1 d D . . H6 H 0.2237(18) 0.614(3) 0.652(3) 0.050 Uiso 1 1 d D . . 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 Al1 0.0242(4) 0.0271(4) 0.0275(4) 0.0032(3) -0.0007(3) -0.0013(3) Al2 0.0237(4) 0.0261(4) 0.0242(3) -0.0001(3) -0.0004(3) 0.0008(3) S1 0.0446(4) 0.0330(3) 0.0262(3) -0.0039(3) -0.0050(3) 0.0088(3) S2 0.0567(5) 0.0277(3) 0.0262(3) 0.0005(2) -0.0001(3) 0.0083(3) Cl1 0.0227(3) 0.0343(3) 0.0358(3) 0.0019(2) 0.0003(2) -0.0035(2) Cl2 0.0244(3) 0.0418(4) 0.0460(4) -0.0045(3) 0.0066(3) 0.0031(3) Cl3 0.0679(6) 0.0858(7) 0.0572(5) 0.0465(5) -0.0113(4) -0.0183(5) Cl4 0.0406(4) 0.0428(4) 0.0620(5) -0.0238(4) -0.0018(3) 0.0003(3) Cl5 0.0733(6) 0.0244(3) 0.0607(5) 0.0042(3) 0.0016(4) 0.0009(4) Cl6 0.0224(3) 0.0348(3) 0.0334(3) 0.0019(2) -0.0036(2) -0.0010(2) Cl7 0.0351(4) 0.0721(5) 0.0232(3) -0.0058(3) 0.0006(3) -0.0028(3) Cl8 0.0223(3) 0.0409(4) 0.0311(3) 0.0004(2) 0.0028(2) -0.0001(3) C1 0.0426(15) 0.0305(14) 0.0260(12) -0.0020(10) -0.0012(11) -0.0009(12) C2 0.0374(15) 0.0270(13) 0.0345(13) -0.0026(10) 0.0006(11) -0.0033(11) C3 0.0440(16) 0.0273(14) 0.0370(14) -0.0014(11) 0.0041(12) -0.0029(12) C4 0.0408(15) 0.0319(14) 0.0289(12) 0.0018(10) 0.0037(11) -0.0023(12) _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 Al1 Cl3 2.1110(11) . ? Al1 Cl4 2.1349(11) . ? Al1 Cl2 2.1361(10) . ? Al1 Cl1 2.1412(10) . ? Al2 Cl5 2.1184(12) . ? Al2 Cl8 2.1305(10) . ? Al2 Cl7 2.1397(10) . ? Al2 Cl6 2.1427(9) . ? S1 C1 1.785(2) . ? S1 C2 1.791(3) . ? S1 H5 1.25(3) . ? S2 C3 1.783(3) . ? S2 C4 1.788(3) . ? S2 H6 1.26(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 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 Cl3 Al1 Cl4 109.85(6) . . ? Cl3 Al1 Cl2 110.52(5) . . ? Cl4 Al1 Cl2 109.77(4) . . ? Cl3 Al1 Cl1 110.08(4) . . ? Cl4 Al1 Cl1 108.46(4) . . ? Cl2 Al1 Cl1 108.12(5) . . ? Cl5 Al2 Cl8 111.25(5) . . ? Cl5 Al2 Cl7 109.54(5) . . ? Cl8 Al2 Cl7 108.40(4) . . ? Cl5 Al2 Cl6 109.34(4) . . ? Cl8 Al2 Cl6 109.73(4) . . ? Cl7 Al2 Cl6 108.54(4) . . ? C1 S1 C2 103.09(12) . . ? C1 S1 H5 105.9(15) . . ? C2 S1 H5 104.8(15) . . ? C3 S2 C4 104.61(13) . . ? C3 S2 H6 98.5(16) . . ? C4 S2 H6 98.6(15) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A S1 H5 Cl4 1.25(3) 2.62(3) 3.7367(13) 147(2) 2_646 S2 H6 Cl4 1.26(3) 2.51(3) 3.6599(12) 151(2) . # S...Cl contacts less than 3.6 Angstrom loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S1 Cl1 3.507(1) . 1_545 ? S1 Cl1 3.405(1) . 3_667 ? S2 Cl2 3.457(1) . 4_575 ? S2 Cl6 3.383(1) . 4_566 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.715 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 966343' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_12kg27ra _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-06-15 _chemical_name_systematic ; trans-dichlorobis(1,2-bis(methylthio)ethane)aluminium tetrachloroaluminate ; # MeSCH2CH2SMe = C4H10S2 # 2,5-dithiahexane # 1,2-bis(methylthio)ethane (iLab name (defaults)) # 1,2-bis(methylsulfanyl)ethane (iLab IUPAC name with selected options) # 1,2-bis(methylsulfanyl)ethane (chemspider) # 1,2-bis(methylthio)ethane & 2,5-dithiahexane (alternatives in chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Al Cl2 S4 1+, Al Cl4 1-' _chemical_formula_sum 'C8 H20 Al2 Cl6 S4' _chemical_formula_weight 511.14 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M '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 6.708(3) _cell_length_b 10.583(5) _cell_length_c 15.383(7) _cell_angle_alpha 90.070(7) _cell_angle_beta 102.422(10) _cell_angle_gamma 96.512(6) _cell_volume 1059.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3008 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 31.2 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.920 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9955 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4821 _reflns_number_gt 4210 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4821 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Al1 Al 0.55925(9) 0.47724(6) 0.75653(4) 0.01378(14) Uani 1 1 d . . . Al2 Al 1.0000 0.0000 0.5000 0.01133(19) Uani 1 2 d S . . Al3 Al 1.0000 0.0000 0.0000 0.01312(19) Uani 1 2 d S . . S1 S 0.87546(8) 0.20993(5) 0.49890(4) 0.01414(12) Uani 1 1 d . . . S2 S 1.33159(8) 0.10959(5) 0.47768(3) 0.01299(12) Uani 1 1 d . . . S3 S 0.72423(8) 0.11889(5) 0.02924(4) 0.01720(12) Uani 1 1 d . . . S4 S 1.17003(8) 0.20092(5) -0.04383(4) 0.01639(12) Uani 1 1 d . . . Cl1 Cl 0.36215(8) 0.55324(5) 0.64578(4) 0.02401(14) Uani 1 1 d . . . Cl2 Cl 0.47918(9) 0.52380(5) 0.87835(4) 0.02258(13) Uani 1 1 d . . . Cl3 Cl 0.87127(8) 0.54972(5) 0.76019(4) 0.02224(13) Uani 1 1 d . . . Cl4 Cl 0.52405(8) 0.27451(5) 0.73865(3) 0.01648(12) Uani 1 1 d . . . Cl5 Cl 0.85809(8) -0.01020(5) 0.35594(3) 0.01551(12) Uani 1 1 d . . . Cl6 Cl 1.20163(8) 0.04377(5) 0.13397(3) 0.01889(12) Uani 1 1 d . . . C1 C 0.9284(3) 0.2803(2) 0.60919(14) 0.0215(5) Uani 1 1 d . . . H1A H 1.0709 0.2722 0.6388 0.032 Uiso 1 1 calc R . . H1B H 0.8352 0.2366 0.6435 0.032 Uiso 1 1 calc R . . H1C H 0.9081 0.3706 0.6053 0.032 Uiso 1 1 calc R . . C2 C 1.0693(3) 0.2999(2) 0.45096(14) 0.0169(5) Uani 1 1 d . . . H2A H 1.0402 0.2798 0.3863 0.020 Uiso 1 1 calc R . . H2B H 1.0599 0.3917 0.4586 0.020 Uiso 1 1 calc R . . C3 C 1.2877(3) 0.2731(2) 0.49209(14) 0.0160(5) Uani 1 1 d . . . H3A H 1.3178 0.2948 0.5566 0.019 Uiso 1 1 calc R . . H3B H 1.3848 0.3292 0.4650 0.019 Uiso 1 1 calc R . . C4 C 1.3434(3) 0.1040(2) 0.36186(13) 0.0184(5) Uani 1 1 d . . . H4A H 1.2175 0.1312 0.3256 0.028 Uiso 1 1 calc R . . H4B H 1.3567 0.0168 0.3443 0.028 Uiso 1 1 calc R . . H4C H 1.4624 0.1610 0.3527 0.028 Uiso 1 1 calc R . . C5 C 0.7612(4) 0.1588(2) 0.14609(14) 0.0237(5) Uani 1 1 d . . . H5A H 0.9037 0.1957 0.1690 0.036 Uiso 1 1 calc R . . H5B H 0.7319 0.0818 0.1786 0.036 Uiso 1 1 calc R . . H5C H 0.6680 0.2207 0.1541 0.036 Uiso 1 1 calc R . . C6 C 0.7988(3) 0.2703(2) -0.01522(15) 0.0211(5) Uani 1 1 d . . . H6A H 0.7456 0.2667 -0.0805 0.025 Uiso 1 1 calc R . . H6B H 0.7330 0.3366 0.0100 0.025 Uiso 1 1 calc R . . C7 C 1.0298(3) 0.3095(2) 0.00390(15) 0.0205(5) Uani 1 1 d . . . H7A H 1.0827 0.3152 0.0692 0.025 Uiso 1 1 calc R . . H7B H 1.0562 0.3952 -0.0198 0.025 Uiso 1 1 calc R . . C8 C 1.0812(3) 0.2254(2) -0.16078(14) 0.0201(5) Uani 1 1 d . . . H8A H 0.9315 0.2052 -0.1771 0.030 Uiso 1 1 calc R . . H8B H 1.1450 0.1698 -0.1951 0.030 Uiso 1 1 calc R . . H8C H 1.1188 0.3144 -0.1739 0.030 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 Al1 0.0140(3) 0.0138(3) 0.0136(3) 0.0001(3) 0.0030(3) 0.0015(3) Al2 0.0115(4) 0.0121(4) 0.0104(4) 0.0002(3) 0.0020(4) 0.0020(3) Al3 0.0138(4) 0.0122(4) 0.0124(5) -0.0011(4) 0.0008(4) 0.0017(4) S1 0.0135(3) 0.0135(3) 0.0165(3) 0.0014(2) 0.0049(2) 0.0032(2) S2 0.0120(2) 0.0152(3) 0.0122(3) 0.0006(2) 0.0034(2) 0.0019(2) S3 0.0161(3) 0.0166(3) 0.0195(3) -0.0016(2) 0.0039(2) 0.0041(2) S4 0.0158(3) 0.0146(3) 0.0183(3) 0.0007(2) 0.0029(2) 0.0012(2) Cl1 0.0227(3) 0.0233(3) 0.0240(3) 0.0090(2) -0.0001(2) 0.0037(2) Cl2 0.0280(3) 0.0229(3) 0.0195(3) -0.0040(2) 0.0104(2) 0.0043(2) Cl3 0.0166(3) 0.0231(3) 0.0264(3) -0.0049(2) 0.0068(2) -0.0042(2) Cl4 0.0168(3) 0.0140(2) 0.0184(3) -0.0012(2) 0.0033(2) 0.0018(2) Cl5 0.0169(3) 0.0180(3) 0.0106(2) 0.0002(2) 0.0011(2) 0.0010(2) Cl6 0.0200(3) 0.0199(3) 0.0140(3) -0.0010(2) -0.0020(2) 0.0017(2) C1 0.0274(13) 0.0187(12) 0.0218(12) -0.0043(10) 0.0135(11) 0.0017(10) C2 0.0184(11) 0.0139(11) 0.0203(12) 0.0044(9) 0.0082(10) 0.0017(9) C3 0.0169(11) 0.0150(10) 0.0169(11) -0.0015(9) 0.0070(9) -0.0012(9) C4 0.0191(11) 0.0236(12) 0.0143(11) -0.0014(9) 0.0077(10) 0.0022(10) C5 0.0320(13) 0.0257(13) 0.0178(12) 0.0034(10) 0.0128(11) 0.0077(11) C6 0.0306(13) 0.0184(11) 0.0179(12) 0.0039(9) 0.0093(10) 0.0109(10) C7 0.0319(13) 0.0115(10) 0.0207(12) -0.0021(9) 0.0113(11) 0.0024(9) C8 0.0256(12) 0.0200(12) 0.0172(12) 0.0022(9) 0.0097(10) 0.0031(10) _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 Al1 Cl2 2.1292(12) . ? Al1 Cl3 2.1348(12) . ? Al1 Cl1 2.1385(10) . ? Al1 Cl4 2.1425(13) . ? Al2 Cl5 2.2131(10) 2_756 ? Al2 Cl5 2.2131(11) . ? Al2 S1 2.4595(11) . ? Al2 S1 2.4595(11) 2_756 ? Al2 S2 2.4809(10) 2_756 ? Al2 S2 2.4809(10) . ? Al3 Cl6 2.2243(10) . ? Al3 Cl6 2.2243(10) 2_755 ? Al3 S4 2.4619(10) 2_755 ? Al3 S4 2.4619(10) . ? Al3 S3 2.4682(10) . ? Al3 S3 2.4682(10) 2_755 ? S1 C1 1.799(2) . ? S1 C2 1.810(2) . ? S2 C4 1.802(2) . ? S2 C3 1.809(2) . ? S3 C5 1.804(2) . ? S3 C6 1.804(2) . ? S4 C8 1.798(2) . ? S4 C7 1.812(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.524(3) . ? 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 1.522(3) . ? 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 . ? 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 Al1 Cl3 109.94(4) . . ? Cl2 Al1 Cl1 110.95(5) . . ? Cl3 Al1 Cl1 109.68(4) . . ? Cl2 Al1 Cl4 109.13(3) . . ? Cl3 Al1 Cl4 109.12(4) . . ? Cl1 Al1 Cl4 107.98(4) . . ? Cl5 Al2 Cl5 180.0 2_756 . ? Cl5 Al2 S1 94.50(2) 2_756 . ? Cl5 Al2 S1 85.50(2) . . ? Cl5 Al2 S1 85.50(2) 2_756 2_756 ? Cl5 Al2 S1 94.50(2) . 2_756 ? S1 Al2 S1 180.0 . 2_756 ? Cl5 Al2 S2 93.51(3) 2_756 2_756 ? Cl5 Al2 S2 86.49(3) . 2_756 ? S1 Al2 S2 92.08(3) . 2_756 ? S1 Al2 S2 87.92(3) 2_756 2_756 ? Cl5 Al2 S2 86.49(3) 2_756 . ? Cl5 Al2 S2 93.51(3) . . ? S1 Al2 S2 87.92(3) . . ? S1 Al2 S2 92.08(3) 2_756 . ? S2 Al2 S2 180.0 2_756 . ? Cl6 Al3 Cl6 180.00(3) . 2_755 ? Cl6 Al3 S4 94.58(3) . 2_755 ? Cl6 Al3 S4 85.42(3) 2_755 2_755 ? Cl6 Al3 S4 85.42(3) . . ? Cl6 Al3 S4 94.58(3) 2_755 . ? S4 Al3 S4 180.00(3) 2_755 . ? Cl6 Al3 S3 94.20(3) . . ? Cl6 Al3 S3 85.80(3) 2_755 . ? S4 Al3 S3 91.57(4) 2_755 . ? S4 Al3 S3 88.43(4) . . ? Cl6 Al3 S3 85.80(3) . 2_755 ? Cl6 Al3 S3 94.20(3) 2_755 2_755 ? S4 Al3 S3 88.43(4) 2_755 2_755 ? S4 Al3 S3 91.57(4) . 2_755 ? S3 Al3 S3 180.00(3) . 2_755 ? C1 S1 C2 101.47(11) . . ? C1 S1 Al2 111.37(8) . . ? C2 S1 Al2 98.76(8) . . ? C4 S2 C3 101.52(10) . . ? C4 S2 Al2 110.77(7) . . ? C3 S2 Al2 99.62(7) . . ? C5 S3 C6 101.65(11) . . ? C5 S3 Al3 111.39(8) . . ? C6 S3 Al3 99.41(8) . . ? C8 S4 C7 101.07(11) . . ? C8 S4 Al3 110.55(8) . . ? C7 S4 Al3 98.19(8) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 113.66(14) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 S2 113.73(14) . . ? C2 C3 H3A 108.8 . . ? S2 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? S2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 S3 114.27(15) . . ? C7 C6 H6A 108.7 . . ? S3 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? S3 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 S4 113.71(15) . . ? C6 C7 H7A 108.8 . . ? S4 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? S4 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 S1 C2 C3 68.38(18) . . . . ? Al2 S1 C2 C3 -45.66(16) . . . . ? S1 C2 C3 S2 61.78(19) . . . . ? C4 S2 C3 C2 74.62(17) . . . . ? Al2 S2 C3 C2 -39.05(16) . . . . ? C5 S3 C6 C7 75.49(18) . . . . ? Al3 S3 C6 C7 -38.81(17) . . . . ? S3 C6 C7 S4 61.6(2) . . . . ? C8 S4 C7 C6 67.65(17) . . . . ? Al3 S4 C7 C6 -45.28(16) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.383 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.079 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if needed. ; _database_code_depnum_ccdc_archive 'CCDC 966344' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg01r _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-06-15 _chemical_name_systematic ; trans-dichlorobis(2,5-diselenahexane)aluminium tetrachloroaluminate ; # MeSeCH2CH2SeMe = C4H10Se2 # 2,5-diselenahexane # 1,2-bis(methylseleno)ethane (I-Lab name (defaults)) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Al Cl2 Se4 1+, Al Cl4 1-' _chemical_formula_sum 'C8 H20 Al2 Cl6 Se4' _chemical_formula_weight 698.74 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.122(4) _cell_length_b 17.744(8) _cell_length_c 17.582(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.169(8) _cell_angle_gamma 90.00 _cell_volume 2218.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4428 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 31.3 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 7.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.683 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10277 _diffrn_reflns_av_R_equivalents 0.1141 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5039 _reflns_number_gt 4183 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5039 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2070 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 Al1 Al 0.0614(4) 0.23889(13) 0.26907(13) 0.0276(5) Uani 1 1 d . . . Al2 Al 0.5000 0.5000 0.5000 0.0197(6) Uani 1 2 d S . . Al3 Al 0.5000 0.5000 0.0000 0.0296(8) Uani 1 2 d S . . Cl1 Cl 0.0274(4) 0.13056(13) 0.31739(17) 0.0584(8) Uani 1 1 d . . . Cl2 Cl -0.1734(4) 0.26784(14) 0.19450(13) 0.0479(6) Uani 1 1 d . . . Cl3 Cl 0.0861(4) 0.31778(15) 0.35971(15) 0.0544(7) Uani 1 1 d . . . Cl4 Cl 0.3105(5) 0.2372(2) 0.20922(17) 0.0789(11) Uani 1 1 d . . . Cl5 Cl 0.4497(3) 0.37714(10) 0.49371(11) 0.0300(4) Uani 1 1 d . . . Cl6 Cl 0.4021(3) 0.50688(11) -0.12213(11) 0.0338(5) Uani 1 1 d . . . Se1 Se 0.36408(12) 0.49155(5) 0.63366(4) 0.0285(2) Uani 1 1 d . . . Se2 Se 0.83657(11) 0.48464(4) 0.56661(4) 0.0219(2) Uani 1 1 d . . . Se3 Se 0.17846(12) 0.43272(4) 0.02202(4) 0.0297(2) Uani 1 1 d . . . Se4 Se 0.64683(13) 0.36642(5) -0.01189(5) 0.0327(2) Uani 1 1 d . . . C1 C 0.3867(16) 0.5909(5) 0.6812(5) 0.046(3) Uani 1 1 d . . . H1A H 0.3979 0.5852 0.7367 0.070 Uiso 1 1 calc R . . H1B H 0.2748 0.6209 0.6668 0.070 Uiso 1 1 calc R . . H1C H 0.4988 0.6163 0.6639 0.070 Uiso 1 1 calc R . . C2 C 0.5843(12) 0.4439(4) 0.6856(4) 0.0288(17) Uani 1 1 d . . . H2A H 0.5652 0.4421 0.7409 0.035 Uiso 1 1 calc R . . H2B H 0.5939 0.3914 0.6673 0.035 Uiso 1 1 calc R . . C3 C 0.7682(12) 0.4841(5) 0.6734(4) 0.0331(19) Uani 1 1 d . . . H3A H 0.8701 0.4594 0.7048 0.040 Uiso 1 1 calc R . . H3B H 0.7585 0.5368 0.6912 0.040 Uiso 1 1 calc R . . C4 C 0.9114(12) 0.3792(4) 0.5579(5) 0.0314(18) Uani 1 1 d . . . H4A H 1.0142 0.3683 0.5956 0.047 Uiso 1 1 calc R . . H4B H 0.9537 0.3699 0.5066 0.047 Uiso 1 1 calc R . . H4C H 0.8039 0.3466 0.5670 0.047 Uiso 1 1 calc R . . C5 C 0.1380(14) 0.4387(5) 0.1314(5) 0.041(2) Uani 1 1 d . . . H5A H 0.0395 0.4029 0.1441 0.062 Uiso 1 1 calc R . . H5B H 0.0991 0.4899 0.1442 0.062 Uiso 1 1 calc R . . H5C H 0.2551 0.4261 0.1606 0.062 Uiso 1 1 calc R . . C6 C 0.2651(13) 0.3278(4) 0.0222(5) 0.0335(19) Uani 1 1 d . . . H6A H 0.1831 0.2977 0.0542 0.040 Uiso 1 1 calc R . . H6B H 0.2497 0.3080 -0.0304 0.040 Uiso 1 1 calc R . . C7 C 0.4641(12) 0.3165(4) 0.0505(4) 0.0294(17) Uani 1 1 d . . . H7A H 0.4913 0.2618 0.0519 0.035 Uiso 1 1 calc R . . H7B H 0.4799 0.3359 0.1032 0.035 Uiso 1 1 calc R . . C8 C 0.5585(17) 0.3243(6) -0.1112(5) 0.050(3) Uani 1 1 d . . . H8A H 0.5509 0.2693 -0.1074 0.075 Uiso 1 1 calc R . . H8B H 0.6468 0.3380 -0.1497 0.075 Uiso 1 1 calc R . . H8C H 0.4338 0.3447 -0.1258 0.075 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 Al1 0.0406(14) 0.0219(11) 0.0204(11) 0.0012(9) 0.0017(10) 0.0014(10) Al2 0.0307(17) 0.0163(14) 0.0119(14) 0.0003(11) 0.0000(12) -0.0011(12) Al3 0.044(2) 0.0266(18) 0.0185(16) 0.0040(13) 0.0044(15) 0.0015(15) Cl1 0.080(2) 0.0289(12) 0.0629(17) 0.0154(11) -0.0273(15) -0.0195(12) Cl2 0.0638(16) 0.0443(14) 0.0336(12) -0.0108(10) -0.0153(11) 0.0166(12) Cl3 0.0603(16) 0.0464(14) 0.0542(15) -0.0303(12) -0.0188(13) 0.0045(13) Cl4 0.076(2) 0.107(3) 0.0580(17) 0.0522(17) 0.0413(15) 0.0507(19) Cl5 0.0418(11) 0.0185(9) 0.0287(10) 0.0009(7) -0.0060(8) -0.0014(8) Cl6 0.0590(14) 0.0255(10) 0.0168(9) 0.0030(7) 0.0019(8) 0.0010(9) Se1 0.0299(4) 0.0400(5) 0.0158(4) 0.0054(3) 0.0028(3) 0.0031(3) Se2 0.0267(4) 0.0229(4) 0.0158(4) 0.0026(3) -0.0002(3) 0.0010(3) Se3 0.0443(5) 0.0230(4) 0.0220(4) 0.0026(3) 0.0034(3) 0.0043(3) Se4 0.0475(6) 0.0253(4) 0.0261(4) 0.0034(3) 0.0079(4) 0.0061(4) C1 0.082(8) 0.039(5) 0.018(4) -0.003(4) 0.000(4) 0.023(5) C2 0.044(5) 0.026(4) 0.017(4) 0.001(3) 0.003(3) 0.009(4) C3 0.036(5) 0.049(5) 0.014(4) 0.001(3) -0.002(3) 0.008(4) C4 0.029(4) 0.027(4) 0.038(5) 0.009(4) 0.002(3) 0.006(3) C5 0.060(6) 0.036(5) 0.029(5) -0.004(4) 0.012(4) 0.001(4) C6 0.053(5) 0.019(4) 0.029(4) -0.002(3) 0.012(4) 0.007(4) C7 0.048(5) 0.018(4) 0.022(4) 0.000(3) 0.005(3) 0.000(3) C8 0.084(8) 0.053(6) 0.015(4) -0.009(4) 0.016(4) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Cl4 2.112(4) . ? Al1 Cl1 2.121(3) . ? Al1 Cl3 2.121(3) . ? Al1 Cl2 2.130(3) . ? Al2 Cl5 2.211(2) . ? Al2 Cl5 2.211(2) 3_666 ? Al2 Se1 2.5950(13) 3_666 ? Al2 Se1 2.5950(13) . ? Al2 Se2 2.6232(13) 3_666 ? Al2 Se2 2.6232(13) . ? Al3 Cl6 2.224(2) . ? Al3 Cl6 2.224(2) 3_665 ? Al3 Se4 2.6037(13) . ? Al3 Se4 2.6037(13) 3_665 ? Al3 Se3 2.6300(13) . ? Al3 Se3 2.6300(13) 3_665 ? Se1 C1 1.953(9) . ? Se1 C2 1.962(8) . ? Se2 C4 1.953(8) . ? Se2 C3 1.965(8) . ? Se3 C6 1.961(8) . ? Se3 C5 1.964(9) . ? Se4 C7 1.959(8) . ? Se4 C8 1.970(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.517(12) . ? 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 1.489(12) . ? 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 . ? 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 Cl4 Al1 Cl1 107.73(17) . . ? Cl4 Al1 Cl3 110.28(19) . . ? Cl1 Al1 Cl3 107.68(16) . . ? Cl4 Al1 Cl2 110.44(15) . . ? Cl1 Al1 Cl2 111.22(15) . . ? Cl3 Al1 Cl2 109.45(15) . . ? Cl5 Al2 Cl5 180.000(1) . 3_666 ? Cl5 Al2 Se1 94.54(6) . 3_666 ? Cl5 Al2 Se1 85.46(6) 3_666 3_666 ? Cl5 Al2 Se1 85.46(6) . . ? Cl5 Al2 Se1 94.54(6) 3_666 . ? Se1 Al2 Se1 180.000(1) 3_666 . ? Cl5 Al2 Se2 86.47(6) . 3_666 ? Cl5 Al2 Se2 93.53(6) 3_666 3_666 ? Se1 Al2 Se2 88.11(4) 3_666 3_666 ? Se1 Al2 Se2 91.89(4) . 3_666 ? Cl5 Al2 Se2 93.53(6) . . ? Cl5 Al2 Se2 86.47(6) 3_666 . ? Se1 Al2 Se2 91.89(4) 3_666 . ? Se1 Al2 Se2 88.11(4) . . ? Se2 Al2 Se2 180.0 3_666 . ? Cl6 Al3 Cl6 180.0 . 3_665 ? Cl6 Al3 Se4 94.50(6) . . ? Cl6 Al3 Se4 85.50(6) 3_665 . ? Cl6 Al3 Se4 85.50(6) . 3_665 ? Cl6 Al3 Se4 94.50(6) 3_665 3_665 ? Se4 Al3 Se4 180.0 . 3_665 ? Cl6 Al3 Se3 86.44(6) . . ? Cl6 Al3 Se3 93.56(6) 3_665 . ? Se4 Al3 Se3 87.45(4) . . ? Se4 Al3 Se3 92.55(4) 3_665 . ? Cl6 Al3 Se3 93.56(6) . 3_665 ? Cl6 Al3 Se3 86.44(6) 3_665 3_665 ? Se4 Al3 Se3 92.55(4) . 3_665 ? Se4 Al3 Se3 87.45(4) 3_665 3_665 ? Se3 Al3 Se3 180.00(3) . 3_665 ? C1 Se1 C2 98.3(4) . . ? C1 Se1 Al2 108.0(3) . . ? C2 Se1 Al2 96.8(2) . . ? C4 Se2 C3 98.8(4) . . ? C4 Se2 Al2 108.1(3) . . ? C3 Se2 Al2 99.1(3) . . ? C6 Se3 C5 96.5(4) . . ? C6 Se3 Al3 98.9(3) . . ? C5 Se3 Al3 107.2(3) . . ? C7 Se4 C8 97.7(4) . . ? C7 Se4 Al3 94.8(2) . . ? C8 Se4 Al3 107.8(3) . . ? 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 113.9(5) . . ? C3 C2 H2A 108.8 . . ? Se1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? Se1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 Se2 113.5(5) . . ? C2 C3 H3A 108.9 . . ? Se2 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? Se2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? 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 115.0(6) . . ? C7 C6 H6A 108.5 . . ? Se3 C6 H6A 108.5 . . ? C7 C6 H6B 108.5 . . ? Se3 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C6 C7 Se4 113.7(5) . . ? C6 C7 H7A 108.8 . . ? Se4 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? Se4 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Se1 C2 C3 -58.4(6) . . . . ? Al2 Se1 C2 C3 51.0(6) . . . . ? Se1 C2 C3 Se2 -63.4(7) . . . . ? C4 Se2 C3 C2 -73.4(6) . . . . ? Al2 Se2 C3 C2 36.7(6) . . . . ? C5 Se3 C6 C7 -78.6(7) . . . . ? Al3 Se3 C6 C7 30.1(6) . . . . ? Se3 C6 C7 Se4 -62.7(7) . . . . ? C8 Se4 C7 C6 -52.7(6) . . . . ? Al3 Se4 C7 C6 56.1(5) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se2 Se2 3.436(2) . 3_766 ? Se3 Se3 3.542(2) . 3_565 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.639 _refine_diff_density_min -2.819 _refine_diff_density_rms 0.259 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if needed. ; _database_code_depnum_ccdc_archive 'CCDC 966345' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg01ka _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-05-18 _chemical_name_systematic ; trichloro(dimethylselenide)aluminium ; # Me2Se = C2H6Se # dimethylselenide (chemspider) # methylselanylmethane (chemspider IUPAC name) # dimethyl selenide (chemspider) # (methylseleno)methane (iLab (defaults)) # dimethyl selenide (iLab (defaults)) (two names from iLab) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Al Cl3 Se' _chemical_formula_sum 'C2 H6 Al Cl3 Se' _chemical_formula_weight 242.36 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c m' _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 6.205(4) _cell_length_b 12.603(8) _cell_length_c 10.479(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 819.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2496 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 31.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 5.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.739 # _exptl_absorpt_correction_T_max 1.000 # _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4140 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.49 _reflns_number_total 984 _reflns_number_gt 914 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0405P)^2^+0.0977P] 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 984 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Se1 Se 0.36460(8) 0.86829(4) 0.7500 0.01973(19) Uani 1 2 d S . . Cl1 Cl 0.78567(17) 1.07244(9) 0.7500 0.0217(3) Uani 1 2 d S . . Cl2 Cl 0.31244(16) 1.12338(7) 0.57966(8) 0.0262(2) Uani 1 1 d . . . Al1 Al 0.4446(2) 1.06161(11) 0.7500 0.0171(3) Uani 1 2 d S . . C1 C 0.1561(6) 0.8588(3) 0.8887(3) 0.0255(8) Uani 1 1 d . . . H1A H 0.0504 0.9162 0.8805 0.038 Uiso 1 1 calc R . . H1B H 0.2311 0.8653 0.9706 0.038 Uiso 1 1 calc R . . H1C H 0.0821 0.7902 0.8847 0.038 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 Se1 0.0221(3) 0.0142(3) 0.0229(3) 0.000 0.000 0.00016(17) Cl1 0.0183(6) 0.0218(6) 0.0252(6) 0.000 0.000 -0.0005(4) Cl2 0.0279(5) 0.0250(5) 0.0258(5) 0.0083(3) -0.0063(4) -0.0010(3) Al1 0.0193(7) 0.0157(7) 0.0163(7) 0.000 0.000 0.0007(5) C1 0.037(2) 0.0238(19) 0.0157(18) 0.0032(13) 0.0033(15) -0.0067(14) _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 Se1 C1 1.950(4) 6_557 ? Se1 C1 1.950(4) . ? Se1 Al1 2.486(2) . ? Cl1 Al1 2.121(2) . ? Cl2 Al1 2.1130(14) . ? Al1 Cl2 2.1130(14) 6_557 ? 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 C1 Se1 C1 96.4(2) 6_557 . ? C1 Se1 Al1 101.10(11) 6_557 . ? C1 Se1 Al1 101.10(11) . . ? Cl2 Al1 Cl2 115.30(9) 6_557 . ? Cl2 Al1 Cl1 111.32(5) 6_557 . ? Cl2 Al1 Cl1 111.32(5) . . ? Cl2 Al1 Se1 106.47(5) 6_557 . ? Cl2 Al1 Se1 106.47(5) . . ? Cl1 Al1 Se1 105.20(6) . . ? 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 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.637 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.144 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 966346' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg03r _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-05-18 _audit_update_record ;2013-06-17 Revised atom labelling and moved some atoms to get better connectivity. M. Webster ; _chemical_name_systematic ; catena-[(1,1,1-tris[(methylsulfanyl)methyl]ethane)-trichloroaluminium] ; # MeC(CH2SMe)3 = C8H18S3 # 2-methyl-1,3-bis(methylsulfanyl)-2-[(methylsulfanyl)methyl]propane # (I-Lab2, defaults) # 1,1,1-tris[(methylsulfanyl)methyl]ethane (mw) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 Al2 Cl6 S6' _chemical_formula_sum 'C16 H36 Al2 Cl6 S6' _chemical_formula_structural '2(C8 H18 S3) 2(Al Cl3)' _chemical_formula_weight 687.47 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.131(7) _cell_length_b 8.310(3) _cell_length_c 24.976(11) _cell_angle_alpha 90.00 _cell_angle_beta 107.156(8) _cell_angle_gamma 90.00 _cell_volume 3199(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5733 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.6 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11255 _diffrn_reflns_av_R_equivalents 0.1340 _diffrn_reflns_av_sigmaI/netI 0.1305 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5251 _reflns_number_gt 4229 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+4.2040P] 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 5251 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2207 _refine_ls_wR_factor_gt 0.2045 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _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 Al1 Al -0.18107(14) 0.4869(3) 0.37272(8) 0.0204(5) Uani 1 1 d . . . Al2 Al 0.32647(14) 0.4938(3) 0.33820(8) 0.0216(5) Uani 1 1 d . . . Cl1 Cl -0.09815(13) 0.6046(3) 0.44564(8) 0.0326(5) Uani 1 1 d . . . Cl2 Cl -0.28460(12) 0.3410(2) 0.38443(8) 0.0288(5) Uani 1 1 d . . . Cl3 Cl -0.15734(13) 0.5236(3) 0.29311(7) 0.0304(5) Uani 1 1 d . . . Cl4 Cl 0.21319(12) 0.6284(3) 0.29110(7) 0.0286(5) Uani 1 1 d . . . Cl5 Cl 0.36423(12) 0.4948(2) 0.42859(7) 0.0278(5) Uani 1 1 d . . . Cl6 Cl 0.40589(12) 0.3573(2) 0.29841(7) 0.0255(5) Uani 1 1 d . . . S1 S 0.12528(17) -0.0123(3) 0.43060(10) 0.0435(6) Uani 1 1 d . . . S2 S -0.08982(12) 0.2411(2) 0.38178(7) 0.0214(4) Uani 1 1 d . . . S3 S 0.22913(12) 0.2595(2) 0.32880(7) 0.0223(4) Uani 1 1 d . . . S4 S -0.37532(13) 1.0495(3) 0.48392(7) 0.0291(5) Uani 1 1 d . . . S5 S -0.28520(12) 0.7124(3) 0.34604(7) 0.0225(4) Uani 1 1 d . . . S6 S -0.58921(12) 0.7448(2) 0.33885(7) 0.0237(5) Uani 1 1 d . . . C1 C 0.0686(5) 0.2363(9) 0.3526(3) 0.0194(16) Uani 1 1 d . . . C2 C 0.0229(5) 0.2765(12) 0.2915(3) 0.035(2) Uani 1 1 d . . . H2A H 0.0507 0.2182 0.2674 0.052 Uiso 1 1 calc R . . H2B H 0.0267 0.3925 0.2856 0.052 Uiso 1 1 calc R . . H2C H -0.0382 0.2447 0.2823 0.052 Uiso 1 1 calc R . . C3 C 0.0744(5) 0.0521(10) 0.3593(3) 0.0287(19) Uani 1 1 d . . . H3A H 0.1077 0.0085 0.3351 0.034 Uiso 1 1 calc R . . H3B H 0.0152 0.0064 0.3463 0.034 Uiso 1 1 calc R . . C4 C 0.1367(10) -0.2249(13) 0.4193(6) 0.088(5) Uani 1 1 d . . . H4A H 0.0793 -0.2753 0.4075 0.132 Uiso 1 1 calc R . . H4B H 0.1718 -0.2748 0.4542 0.132 Uiso 1 1 calc R . . H4C H 0.1653 -0.2399 0.3901 0.132 Uiso 1 1 calc R . . C5 C 0.0203(4) 0.3142(10) 0.3913(3) 0.0198(16) Uani 1 1 d . . . H5A H 0.0179 0.4319 0.3850 0.024 Uiso 1 1 calc R . . H5B H 0.0548 0.2952 0.4308 0.024 Uiso 1 1 calc R . . C6 C -0.0821(5) 0.1616(11) 0.4504(3) 0.032(2) Uani 1 1 d . . . H6A H -0.0451 0.0657 0.4573 0.048 Uiso 1 1 calc R . . H6B H -0.1401 0.1329 0.4522 0.048 Uiso 1 1 calc R . . H6C H -0.0569 0.2432 0.4789 0.048 Uiso 1 1 calc R . . C7 C 0.1596(5) 0.3140(10) 0.3715(3) 0.0243(17) Uani 1 1 d . . . H7A H 0.1886 0.2821 0.4108 0.029 Uiso 1 1 calc R . . H7B H 0.1528 0.4325 0.3708 0.029 Uiso 1 1 calc R . . C8 C 0.2962(6) 0.0994(11) 0.3674(4) 0.038(2) Uani 1 1 d . . . H8A H 0.3230 0.1338 0.4062 0.057 Uiso 1 1 calc R . . H8B H 0.3417 0.0737 0.3500 0.057 Uiso 1 1 calc R . . H8C H 0.2605 0.0038 0.3670 0.057 Uiso 1 1 calc R . . C9 C -0.4147(5) 0.8295(9) 0.3922(3) 0.0199(16) Uani 1 1 d . . . C10 C -0.4259(5) 0.9714(9) 0.3518(3) 0.0208(16) Uani 1 1 d . . . H10A H -0.4836 1.0185 0.3457 0.031 Uiso 1 1 calc R . . H10B H -0.4197 0.9339 0.3160 0.031 Uiso 1 1 calc R . . H10C H -0.3816 1.0528 0.3678 0.031 Uiso 1 1 calc R . . C11 C -0.4330(5) 0.8750(10) 0.4473(3) 0.0273(18) Uani 1 1 d . . . H11A H -0.4184 0.7814 0.4729 0.033 Uiso 1 1 calc R . . H11B H -0.4960 0.8948 0.4391 0.033 Uiso 1 1 calc R . . C12 C -0.4499(6) 1.2107(11) 0.4536(3) 0.036(2) Uani 1 1 d . . . H12A H -0.4488 1.2308 0.4152 0.054 Uiso 1 1 calc R . . H12B H -0.4327 1.3085 0.4760 0.054 Uiso 1 1 calc R . . H12C H -0.5087 1.1799 0.4533 0.054 Uiso 1 1 calc R . . C13 C -0.3199(4) 0.7625(9) 0.4069(3) 0.0191(16) Uani 1 1 d . . . H13A H -0.3156 0.6650 0.4303 0.023 Uiso 1 1 calc R . . H13B H -0.2796 0.8439 0.4295 0.023 Uiso 1 1 calc R . . C14 C -0.2206(5) 0.8830(9) 0.3399(3) 0.0293(19) Uani 1 1 d . . . H14A H -0.2561 0.9806 0.3348 0.044 Uiso 1 1 calc R . . H14B H -0.1989 0.8686 0.3074 0.044 Uiso 1 1 calc R . . H14C H -0.1715 0.8929 0.3739 0.044 Uiso 1 1 calc R . . C15 C -0.4750(4) 0.6880(9) 0.3657(3) 0.0228(17) Uani 1 1 d . . . H15A H -0.4691 0.6026 0.3942 0.027 Uiso 1 1 calc R . . H15B H -0.4560 0.6426 0.3347 0.027 Uiso 1 1 calc R . . C16 C -0.6018(5) 0.7812(11) 0.2655(3) 0.0305(19) Uani 1 1 d . . . H16A H -0.5673 0.8752 0.2618 0.046 Uiso 1 1 calc R . . H16B H -0.6631 0.8013 0.2458 0.046 Uiso 1 1 calc R . . H16C H -0.5819 0.6868 0.2493 0.046 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 Al1 0.0217(12) 0.0286(13) 0.0110(10) 0.0007(8) 0.0047(8) -0.0018(11) Al2 0.0220(12) 0.0317(14) 0.0104(10) -0.0008(9) 0.0036(8) -0.0012(11) Cl1 0.0308(11) 0.0420(13) 0.0189(9) -0.0100(8) -0.0023(7) 0.0018(10) Cl2 0.0269(11) 0.0325(12) 0.0294(10) 0.0016(8) 0.0117(8) -0.0044(10) Cl3 0.0386(12) 0.0405(12) 0.0162(9) 0.0080(8) 0.0144(8) 0.0082(10) Cl4 0.0229(10) 0.0386(12) 0.0216(9) 0.0080(8) 0.0027(7) 0.0032(10) Cl5 0.0342(11) 0.0370(11) 0.0104(8) -0.0020(7) 0.0037(7) -0.0040(10) Cl6 0.0263(10) 0.0338(11) 0.0178(9) -0.0032(7) 0.0089(7) 0.0002(9) S1 0.0624(16) 0.0392(14) 0.0390(13) 0.0170(10) 0.0303(12) 0.0161(13) S2 0.0230(10) 0.0296(11) 0.0118(8) 0.0002(7) 0.0056(7) -0.0039(9) S3 0.0221(10) 0.0309(11) 0.0146(8) -0.0032(7) 0.0062(7) -0.0001(9) S4 0.0289(11) 0.0420(13) 0.0128(9) -0.0046(8) 0.0007(7) 0.0006(10) S5 0.0240(10) 0.0307(11) 0.0132(8) 0.0016(7) 0.0061(7) 0.0013(9) S6 0.0226(10) 0.0294(11) 0.0184(9) 0.0015(7) 0.0051(7) 0.0021(9) C1 0.021(4) 0.030(4) 0.009(3) 0.001(3) 0.007(3) 0.007(4) C2 0.026(4) 0.068(7) 0.008(3) -0.005(4) 0.000(3) -0.007(5) C3 0.037(5) 0.026(5) 0.028(4) -0.012(3) 0.016(3) -0.007(4) C4 0.160(14) 0.044(7) 0.095(10) 0.027(6) 0.091(10) 0.046(8) C5 0.018(4) 0.029(4) 0.012(3) -0.004(3) 0.003(3) 0.000(4) C6 0.033(5) 0.046(6) 0.014(4) 0.003(3) 0.003(3) -0.003(4) C7 0.030(4) 0.033(5) 0.009(3) -0.004(3) 0.004(3) 0.006(4) C8 0.030(5) 0.037(6) 0.051(6) 0.007(4) 0.020(4) 0.000(5) C9 0.019(4) 0.022(4) 0.018(4) 0.000(3) 0.005(3) -0.004(4) C10 0.024(4) 0.024(4) 0.013(3) 0.000(3) 0.003(3) -0.002(4) C11 0.035(5) 0.038(5) 0.008(3) 0.002(3) 0.004(3) -0.001(4) C12 0.050(5) 0.043(5) 0.015(4) -0.011(3) 0.008(4) -0.004(5) C13 0.016(4) 0.028(4) 0.014(3) 0.002(3) 0.005(3) 0.003(3) C14 0.037(5) 0.026(5) 0.029(4) 0.008(3) 0.016(4) 0.003(4) C15 0.020(4) 0.029(4) 0.020(4) 0.001(3) 0.008(3) -0.003(4) C16 0.029(4) 0.044(5) 0.016(4) 0.009(3) 0.002(3) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Cl1 2.151(3) . ? Al1 Cl2 2.152(3) . ? Al1 Cl3 2.154(3) . ? Al1 S5 2.473(3) . ? Al1 S2 2.489(3) . ? Al2 Cl5 2.158(3) . ? Al2 Cl6 2.160(3) . ? Al2 Cl4 2.169(3) . ? Al2 S3 2.469(3) . ? Al2 S6 2.488(3) 1_655 ? S1 C4 1.807(11) . ? S1 C3 1.807(8) . ? S2 C6 1.806(7) . ? S2 C5 1.826(7) . ? S3 C8 1.804(9) . ? S3 C7 1.819(7) . ? S4 C12 1.810(9) . ? S4 C11 1.818(8) . ? S5 C14 1.793(8) . ? S5 C13 1.816(7) . ? S6 C16 1.808(7) . ? S6 C15 1.826(7) . ? S6 Al2 2.488(3) 1_455 ? C1 C2 1.522(9) . ? C1 C3 1.540(11) . ? C1 C7 1.544(10) . ? C1 C5 1.551(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.527(10) . ? C9 C11 1.537(9) . ? C9 C15 1.545(10) . ? C9 C13 1.566(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 Cl1 Al1 Cl2 117.05(12) . . ? Cl1 Al1 Cl3 118.80(13) . . ? Cl2 Al1 Cl3 124.15(13) . . ? Cl1 Al1 S5 94.98(11) . . ? Cl2 Al1 S5 88.33(11) . . ? Cl3 Al1 S5 86.31(10) . . ? Cl1 Al1 S2 95.32(11) . . ? Cl2 Al1 S2 89.27(11) . . ? Cl3 Al1 S2 86.49(10) . . ? S5 Al1 S2 169.38(11) . . ? Cl5 Al2 Cl6 117.44(13) . . ? Cl5 Al2 Cl4 119.86(12) . . ? Cl6 Al2 Cl4 122.70(12) . . ? Cl5 Al2 S3 94.48(10) . . ? Cl6 Al2 S3 89.38(11) . . ? Cl4 Al2 S3 86.84(11) . . ? Cl5 Al2 S6 90.27(10) . 1_655 ? Cl6 Al2 S6 92.63(10) . 1_655 ? Cl4 Al2 S6 86.71(11) . 1_655 ? S3 Al2 S6 173.30(12) . 1_655 ? C4 S1 C3 100.0(5) . . ? C6 S2 C5 101.9(3) . . ? C6 S2 Al1 105.1(3) . . ? C5 S2 Al1 105.4(3) . . ? C8 S3 C7 104.3(4) . . ? C8 S3 Al2 105.4(3) . . ? C7 S3 Al2 103.5(3) . . ? C12 S4 C11 101.6(4) . . ? C14 S5 C13 102.8(4) . . ? C14 S5 Al1 104.9(3) . . ? C13 S5 Al1 107.5(2) . . ? C16 S6 C15 102.4(4) . . ? C16 S6 Al2 103.6(3) . 1_455 ? C15 S6 Al2 106.0(3) . 1_455 ? C2 C1 C3 108.9(6) . . ? C2 C1 C7 110.6(6) . . ? C3 C1 C7 111.1(6) . . ? C2 C1 C5 110.5(6) . . ? C3 C1 C5 111.8(6) . . ? C7 C1 C5 103.9(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 S1 113.4(5) . . ? C1 C3 H3A 108.9 . . ? S1 C3 H3A 108.9 . . ? C1 C3 H3B 108.9 . . ? S1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? S1 C4 H4A 109.5 . . ? S1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C5 S2 115.3(5) . . ? C1 C5 H5A 108.4 . . ? S2 C5 H5A 108.4 . . ? C1 C5 H5B 108.4 . . ? S2 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 S3 114.3(5) . . ? C1 C7 H7A 108.7 . . ? S3 C7 H7A 108.7 . . ? C1 C7 H7B 108.7 . . ? S3 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? S3 C8 H8A 109.5 . . ? S3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 112.6(6) . . ? C10 C9 C15 111.6(6) . . ? C11 C9 C15 107.9(6) . . ? C10 C9 C13 110.2(6) . . ? C11 C9 C13 108.1(6) . . ? C15 C9 C13 106.2(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 S4 116.2(5) . . ? C9 C11 H11A 108.2 . . ? S4 C11 H11A 108.2 . . ? C9 C11 H11B 108.2 . . ? S4 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? S4 C12 H12A 109.5 . . ? S4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 S5 114.0(4) . . ? C9 C13 H13A 108.8 . . ? S5 C13 H13A 108.8 . . ? C9 C13 H13B 108.8 . . ? S5 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? S5 C14 H14A 109.5 . . ? S5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 S6 113.6(5) . . ? C9 C15 H15A 108.8 . . ? S6 C15 H15A 108.8 . . ? C9 C15 H15B 108.8 . . ? S6 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? S6 C16 H16A 109.5 . . ? S6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S6 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 C2 C1 C3 S1 -178.6(5) . . . . ? C7 C1 C3 S1 59.4(7) . . . . ? C5 C1 C3 S1 -56.2(7) . . . . ? C4 S1 C3 C1 -170.6(7) . . . . ? C2 C1 C5 S2 63.9(8) . . . . ? C3 C1 C5 S2 -57.6(7) . . . . ? C7 C1 C5 S2 -177.5(5) . . . . ? C6 S2 C5 C1 120.2(6) . . . . ? Al1 S2 C5 C1 -130.3(5) . . . . ? C2 C1 C7 S3 -56.1(8) . . . . ? C3 C1 C7 S3 65.0(7) . . . . ? C5 C1 C7 S3 -174.6(5) . . . . ? C8 S3 C7 C1 -97.8(6) . . . . ? Al2 S3 C7 C1 152.1(5) . . . . ? C10 C9 C11 S4 -51.9(8) . . . . ? C15 C9 C11 S4 -175.5(5) . . . . ? C13 C9 C11 S4 70.1(8) . . . . ? C12 S4 C11 C9 89.9(6) . . . . ? C10 C9 C13 S5 -53.5(7) . . . . ? C11 C9 C13 S5 -176.9(5) . . . . ? C15 C9 C13 S5 67.6(7) . . . . ? C14 S5 C13 C9 100.4(6) . . . . ? Al1 S5 C13 C9 -149.2(5) . . . . ? C10 C9 C15 S6 -54.1(7) . . . . ? C11 C9 C15 S6 70.1(7) . . . . ? C13 C9 C15 S6 -174.2(4) . . . . ? C16 S6 C15 C9 95.6(6) . . . . ? Al2 S6 C15 C9 -156.0(4) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.834 _refine_diff_density_max 0.604 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.139 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if needed. ; _database_code_depnum_ccdc_archive 'CCDC 966347' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg06r _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-06-18 _chemical_name_systematic ; 2-methyl-1,3-dihydro-2-benzoselenophenium tetrachloroaluminate ; # [C9H11Se]+ # 2-methyl-1,3-dihydro-2-benzoselenophenium (iLab defaults) # 2-methyl-1,3-dihydro-2-benzoselenophenium (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H11 Se 1+, Al Cl4 1-' _chemical_formula_sum 'C9 H11 Al Cl4 Se' _chemical_formula_weight 366.92 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4218(19) _cell_length_b 14.027(3) _cell_length_c 13.481(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.415(6) _cell_angle_gamma 90.00 _cell_volume 1399.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4133 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 34.5 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 3.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.827 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8131 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3200 _reflns_number_gt 2847 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0356P)^2^+0.7540P] 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 3200 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Al1 Al 0.09007(12) 0.30564(7) 0.02797(6) 0.0177(2) Uani 1 1 d . . . Cl1 Cl 0.09021(11) 0.17028(6) 0.10111(6) 0.02691(18) Uani 1 1 d . . . Cl2 Cl 0.35093(9) 0.37089(5) 0.05319(5) 0.02200(17) Uani 1 1 d . . . Cl3 Cl 0.03597(10) 0.28208(5) -0.12839(5) 0.02267(17) Uani 1 1 d . . . Cl4 Cl -0.11066(11) 0.39390(7) 0.08467(7) 0.0346(2) Uani 1 1 d . . . Se1 Se 0.61454(4) 0.37332(2) 0.83473(2) 0.02062(10) Uani 1 1 d . . . C1 C 0.7547(4) 0.4597(2) 0.7572(2) 0.0214(6) Uani 1 1 d . . . H1A H 0.8276 0.5037 0.8015 0.026 Uiso 1 1 calc R . . H1B H 0.8367 0.4234 0.7166 0.026 Uiso 1 1 calc R . . C2 C 0.6165(4) 0.5144(2) 0.6912(2) 0.0200(6) Uani 1 1 d . . . C3 C 0.6632(4) 0.5691(2) 0.6116(2) 0.0249(7) Uani 1 1 d . . . H3 H 0.7857 0.5733 0.5963 0.030 Uiso 1 1 calc R . . C4 C 0.5309(5) 0.6175(2) 0.5550(2) 0.0277(7) Uani 1 1 d . . . H4 H 0.5631 0.6557 0.5009 0.033 Uiso 1 1 calc R . . C5 C 0.3511(5) 0.6113(2) 0.5757(2) 0.0262(7) Uani 1 1 d . . . H5 H 0.2609 0.6446 0.5355 0.031 Uiso 1 1 calc R . . C6 C 0.3031(4) 0.5563(2) 0.6553(2) 0.0236(7) Uani 1 1 d . . . H6 H 0.1802 0.5516 0.6699 0.028 Uiso 1 1 calc R . . C7 C 0.4372(4) 0.5080(2) 0.7134(2) 0.0186(6) Uani 1 1 d . . . C8 C 0.3980(4) 0.4486(2) 0.8026(2) 0.0214(6) Uani 1 1 d . . . H8A H 0.2926 0.4066 0.7865 0.026 Uiso 1 1 calc R . . H8B H 0.3722 0.4899 0.8593 0.026 Uiso 1 1 calc R . . C9 C 0.5701(5) 0.2781(2) 0.7330(2) 0.0334(8) Uani 1 1 d . . . H9A H 0.4771 0.2338 0.7526 0.050 Uiso 1 1 calc R . . H9B H 0.6820 0.2429 0.7244 0.050 Uiso 1 1 calc R . . H9C H 0.5287 0.3091 0.6701 0.050 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 Al1 0.0149(4) 0.0221(5) 0.0161(4) 0.0002(4) 0.0020(3) 0.0021(4) Cl1 0.0287(4) 0.0302(4) 0.0221(4) 0.0095(3) 0.0037(3) -0.0019(3) Cl2 0.0173(3) 0.0267(4) 0.0219(4) 0.0002(3) 0.0007(3) -0.0019(3) Cl3 0.0227(4) 0.0290(4) 0.0161(3) 0.0032(3) 0.0001(3) -0.0003(3) Cl4 0.0215(4) 0.0421(5) 0.0407(5) -0.0131(4) 0.0044(3) 0.0082(4) Se1 0.02012(17) 0.02652(18) 0.01509(15) 0.00150(13) 0.00055(11) 0.00148(13) C1 0.0183(14) 0.0215(15) 0.0246(15) -0.0003(13) 0.0028(12) 0.0002(13) C2 0.0219(15) 0.0180(14) 0.0203(14) -0.0059(13) 0.0025(12) 0.0007(12) C3 0.0264(16) 0.0232(16) 0.0256(16) -0.0014(14) 0.0059(13) -0.0048(14) C4 0.0376(19) 0.0222(16) 0.0236(16) 0.0029(14) 0.0034(14) -0.0036(14) C5 0.0342(18) 0.0189(15) 0.0243(16) 0.0001(13) -0.0053(14) 0.0033(14) C6 0.0217(15) 0.0218(15) 0.0275(16) -0.0060(14) 0.0027(12) -0.0004(13) C7 0.0219(15) 0.0147(13) 0.0193(14) -0.0029(12) 0.0022(12) -0.0003(12) C8 0.0152(13) 0.0246(15) 0.0249(15) -0.0004(14) 0.0043(12) 0.0029(13) C9 0.047(2) 0.0256(17) 0.0258(17) 0.0008(15) -0.0073(15) 0.0081(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 Cl4 2.1240(12) . ? Al1 Cl1 2.1393(13) . ? Al1 Cl3 2.1409(12) . ? Al1 Cl2 2.1448(12) . ? Se1 C9 1.925(3) . ? Se1 C8 1.944(3) . ? Se1 C1 1.952(3) . ? C1 C2 1.513(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.385(4) . ? C2 C7 1.389(4) . ? C3 C4 1.375(5) . ? C3 H3 0.9500 . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.394(4) . ? C6 H6 0.9500 . ? C7 C8 1.510(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 Cl4 Al1 Cl1 109.08(5) . . ? Cl4 Al1 Cl3 111.14(5) . . ? Cl1 Al1 Cl3 108.07(5) . . ? Cl4 Al1 Cl2 110.11(5) . . ? Cl1 Al1 Cl2 109.71(5) . . ? Cl3 Al1 Cl2 108.69(5) . . ? C9 Se1 C8 97.15(14) . . ? C9 Se1 C1 96.79(15) . . ? C8 Se1 C1 90.51(13) . . ? C2 C1 Se1 105.3(2) . . ? C2 C1 H1A 110.7 . . ? Se1 C1 H1A 110.7 . . ? C2 C1 H1B 110.7 . . ? Se1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C3 C2 C7 120.2(3) . . ? C3 C2 C1 122.5(3) . . ? C7 C2 C1 117.3(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 119.3(3) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C2 C7 C6 120.2(3) . . ? C2 C7 C8 117.0(3) . . ? C6 C7 C8 122.9(3) . . ? C7 C8 Se1 105.71(19) . . ? C7 C8 H8A 110.6 . . ? Se1 C8 H8A 110.6 . . ? C7 C8 H8B 110.6 . . ? Se1 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? Se1 C9 H9A 109.5 . . ? Se1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Se1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.112 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.097 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if tequired. ; _database_code_depnum_ccdc_archive 'CCDC 966348' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg09ra _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-6-19 _chemical_name_systematic ; [(Methyltellanyl)methane]trichloroaluminium(III) ; # Me2Te = C2H6Te # (Methyltellanyl)methane (Chemspider IUPAC) # dimethyl telluride (Chemspider alternative) # dimethyltelluride (Chemspider alternative) # (methyltellanyl)methane (ACD I-Lab2) # dimethyl telluride (ACD I-Lab2) # dimethyltellane (? mw. See Red book) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Al Cl3 Te' _chemical_formula_sum 'C2 H6 Al Cl3 Te' _chemical_formula_weight 291.00 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c m' _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 6.2476(13) _cell_length_b 13.114(3) _cell_length_c 10.514(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 861.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3088 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 34.6 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 4.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.778 # _exptl_absorpt_correction_T_max 1.000 # _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3839 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 29.97 _reflns_number_total 1312 _reflns_number_gt 1194 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1312 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0353 _refine_ls_wR_factor_gt 0.0342 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.54039(12) 0.43573(5) 0.2500 0.01317(15) Uani 1 2 d S . . Cl1 Cl 0.20082(9) 0.42169(4) 0.2500 0.01742(12) Uani 1 2 d S . . Cl2 Cl 0.67397(7) 0.37693(3) 0.07969(4) 0.02111(10) Uani 1 1 d . . . Te1 Te 0.62427(2) 0.636690(12) 0.2500 0.01562(5) Uani 1 2 d S . . C1 C 0.8594(3) 0.63865(14) 0.39652(17) 0.0225(4) Uani 1 1 d . . . H1A H 0.9531 0.5792 0.3876 0.034 Uiso 1 1 calc R . . H1B H 0.7885 0.6366 0.4796 0.034 Uiso 1 1 calc R . . H1C H 0.9447 0.7011 0.3898 0.034 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 Al1 0.0127(3) 0.0128(3) 0.0140(3) 0.000 0.000 -0.0010(3) Cl1 0.0128(3) 0.0204(3) 0.0191(3) 0.000 0.000 -0.0006(2) Cl2 0.0204(2) 0.0216(2) 0.0214(2) -0.00715(18) 0.00571(17) -0.00174(16) Te1 0.01650(8) 0.01113(8) 0.01923(8) 0.000 0.000 0.00067(6) C1 0.0295(10) 0.0243(9) 0.0137(7) -0.0031(8) -0.0011(7) -0.0069(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 Al1 Cl2 2.1207(6) . ? Al1 Cl2 2.1207(6) 6_556 ? Al1 Cl1 2.1295(10) . ? Al1 Te1 2.6871(9) . ? Te1 C1 2.1287(18) . ? Te1 C1 2.1287(18) 6_556 ? 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 Cl2 Al1 Cl2 115.20(4) . 6_556 ? Cl2 Al1 Cl1 111.14(3) . . ? Cl2 Al1 Cl1 111.14(3) 6_556 . ? Cl2 Al1 Te1 106.25(2) . . ? Cl2 Al1 Te1 106.25(2) 6_556 . ? Cl1 Al1 Te1 106.21(3) . . ? C1 Te1 C1 92.72(10) . 6_556 ? C1 Te1 Al1 98.42(5) . . ? C1 Te1 Al1 98.42(5) 6_556 . ? Te1 C1 H1A 109.5 . . ? Te1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Te1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.658 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.100 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 966349' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg25ra _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-7-18 _chemical_name_systematic ; [(Methyltellanyl)methane]tribromoaluminium(III) ; # Me2Te = C2H6Te # (Methyltellanyl)methane (Chemspider IUPAC) # dimethyl telluride (Chemspider alternative) # dimethyltelluride (Chemspider alternative) # (methyltellanyl)methane (ACD I-Lab2) # dimethyl telluride (ACD I-Lab2) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Al Br3 Te' _chemical_formula_sum 'C2 H6 Al Br3 Te' _chemical_formula_weight 424.38 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c m' _space_group_IT_number 57 _space_group_name_Hall '-P 2c 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 6.562(3) _cell_length_b 13.400(5) _cell_length_c 10.724(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 943.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3222 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 34.7 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 15.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8126 _diffrn_reflns_av_R_equivalents 0.2969 # _diffrn_reflns_av_sigmaI/netI 0.1318 _diffrn_reflns_av_unetI/netI 0.1318 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1140 _reflns_number_gt 1066 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _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^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1140 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Al1 Al 0.4562(5) 0.4431(2) 0.7500 0.0155(6) Uani 1 2 d S . . Br1 Br 0.80297(16) 0.42680(9) 0.7500 0.0191(3) Uani 1 2 d S . . Br2 Br 0.31725(14) 0.37987(6) 0.57114(7) 0.0220(3) Uani 1 1 d . . . Te1 Te 0.37910(11) 0.64046(5) 0.7500 0.0179(3) Uani 1 2 d S . . C1 C 0.1537(13) 0.6441(6) 0.8944(8) 0.0216(17) Uani 1 1 d . . . H1A H 0.0695 0.7040 0.8850 0.032 Uiso 1 1 calc R . . H1B H 0.2212 0.6453 0.9759 0.032 Uiso 1 1 calc R . . H1C H 0.0674 0.5846 0.8884 0.032 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 Al1 0.0235(16) 0.0085(15) 0.0146(13) 0.000 0.000 0.0018(12) Br1 0.0214(6) 0.0166(7) 0.0194(5) 0.000 0.000 -0.0001(4) Br2 0.0286(5) 0.0185(5) 0.0190(5) -0.0057(3) -0.0038(3) 0.0001(3) Te1 0.0263(5) 0.0087(5) 0.0187(4) 0.000 0.000 -0.0002(2) C1 0.028(4) 0.024(5) 0.013(4) -0.004(3) 0.006(3) 0.005(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 Al1 Br1 2.286(3) . ? Al1 Br2 2.287(2) . ? Al1 Br2 2.287(2) 6_557 ? Al1 Te1 2.692(4) . ? Te1 C1 2.142(8) 6_557 ? Te1 C1 2.142(8) . ? 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 Al1 Br2 111.19(9) . . ? Br1 Al1 Br2 111.19(9) . 6_557 ? Br2 Al1 Br2 114.01(15) . 6_557 ? Br1 Al1 Te1 106.34(12) . . ? Br2 Al1 Te1 106.80(9) . . ? Br2 Al1 Te1 106.80(9) 6_557 . ? C1 Te1 C1 92.6(5) 6_557 . ? C1 Te1 Al1 98.7(2) 6_557 . ? C1 Te1 Al1 98.7(2) . . ? Te1 C1 H1A 109.5 . . ? Te1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Te1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.904 _refine_diff_density_min -2.392 _refine_diff_density_rms 0.426 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 966350' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_13kg03kb _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-08-25 # yyyy-mm-dd _chemical_name_systematic ; bis(1,2-bis(methylthio)ethane)diiodoaluminium tetraiodoaluminate ; # MeSCH2CH2SMe = C4H10S2 # 2,5-dithiahexane # 1,2-bis(methylthio)ethane (iLab name (defaults)) # 1,2-bis(methylsulfanyl)ethane (iLab IUPAC name with selected options) # 1,2-bis(methylsulfanyl)ethane (chemspider) # 1,2-bis(methylthio)ethane & 2,5-dithiahexane (alternatives in chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Al I2 S4 1+, Al I4 1-' _chemical_formula_sum 'C8 H20 Al2 I6 S4' _chemical_formula_weight 1059.84 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' Al Al 0.0645 0.0514 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.825(3) _cell_length_b 12.181(2) _cell_length_c 15.150(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.449(8) _cell_angle_gamma 90.00 _cell_volume 2595.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16847 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 7.563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.489 # Expt'l Tmin & Tmax _exptl_absorpt_correction_T_max 1.000 # scaled to Tmax=1.0 _exptl_absorpt_process_details ; Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, HF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ SuperBright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24085 _diffrn_reflns_av_R_equivalents 0.1524 # _diffrn_reflns_av_sigmaI/netI 0.2641 _diffrn_reflns_av_unetI/netI 0.2641 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5928 _reflns_number_gt 2983 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _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^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5928 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1353 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _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 Al1 Al 0.3367(3) 0.7367(3) 0.4061(2) 0.0273(8) Uani 1 1 d . . . Al2 Al 0.1467(3) 0.2390(3) 0.1903(2) 0.0287(9) Uani 1 1 d . . . I1 I 0.40538(6) 0.57074(7) 0.33872(5) 0.0354(2) Uani 1 1 d . . . I2 I 0.39418(6) 0.89298(7) 0.31611(5) 0.0339(2) Uani 1 1 d . . . I3 I 0.12326(7) 0.26988(7) 0.34650(5) 0.0372(2) Uani 1 1 d . . . I4 I 0.03371(7) 0.36299(8) 0.07291(6) 0.0456(3) Uani 1 1 d . . . I5 I 0.11278(6) 0.03723(7) 0.14822(5) 0.0369(2) Uani 1 1 d . . . I6 I 0.31569(6) 0.28125(7) 0.19294(5) 0.0375(2) Uani 1 1 d . . . S1 S 0.1748(2) 0.7349(3) 0.29990(19) 0.0307(7) Uani 1 1 d . . . S2 S 0.2672(2) 0.6159(3) 0.50549(19) 0.0315(7) Uani 1 1 d . . . S3 S 0.2733(2) 0.8726(3) 0.4985(2) 0.0331(8) Uani 1 1 d . . . S4 S 0.4714(2) 0.7265(2) 0.54989(19) 0.0298(7) Uani 1 1 d . . . C1 C 0.1793(10) 0.7084(11) 0.1837(7) 0.044(4) Uani 1 1 d . . . H1A H 0.2218 0.6463 0.1853 0.067 Uiso 1 1 calc R . . H1B H 0.2032 0.7737 0.1604 0.067 Uiso 1 1 calc R . . H1C H 0.1153 0.6909 0.1424 0.067 Uiso 1 1 calc R . . C2 C 0.1368(9) 0.6017(12) 0.3284(8) 0.047(4) Uani 1 1 d . . . H2A H 0.0702 0.5878 0.2897 0.057 Uiso 1 1 calc R . . H2B H 0.1773 0.5435 0.3151 0.057 Uiso 1 1 calc R . . C3 C 0.1446(8) 0.5992(11) 0.4320(8) 0.037(3) Uani 1 1 d . . . H3A H 0.1197 0.5284 0.4466 0.045 Uiso 1 1 calc R . . H3B H 0.1053 0.6588 0.4452 0.045 Uiso 1 1 calc R . . C4 C 0.3117(10) 0.4790(10) 0.5130(8) 0.047(4) Uani 1 1 d . . . H4A H 0.2836 0.4348 0.5517 0.071 Uiso 1 1 calc R . . H4B H 0.3810 0.4800 0.5410 0.071 Uiso 1 1 calc R . . H4C H 0.2949 0.4471 0.4505 0.071 Uiso 1 1 calc R . . C5 C 0.2256(11) 0.9903(10) 0.4351(8) 0.046(4) Uani 1 1 d . . . H5A H 0.2228 1.0494 0.4780 0.069 Uiso 1 1 calc R . . H5B H 0.1613 0.9744 0.3936 0.069 Uiso 1 1 calc R . . H5C H 0.2659 1.0130 0.3980 0.069 Uiso 1 1 calc R . . C6 C 0.3900(8) 0.9224(10) 0.5733(7) 0.031(3) Uani 1 1 d . . . H6A H 0.4244 0.9576 0.5344 0.037 Uiso 1 1 calc R . . H6B H 0.3809 0.9779 0.6174 0.037 Uiso 1 1 calc R . . C7 C 0.4471(9) 0.8285(11) 0.6259(8) 0.039(3) Uani 1 1 d . . . H7A H 0.4120 0.7936 0.6643 0.047 Uiso 1 1 calc R . . H7B H 0.5080 0.8566 0.6684 0.047 Uiso 1 1 calc R . . C8 C 0.5747(8) 0.7799(11) 0.5253(8) 0.038(3) Uani 1 1 d . . . H8A H 0.5661 0.8586 0.5117 0.058 Uiso 1 1 calc R . . H8B H 0.5826 0.7415 0.4713 0.058 Uiso 1 1 calc R . . H8C H 0.6313 0.7685 0.5794 0.058 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 Al1 0.028(2) 0.025(2) 0.0268(17) -0.0009(14) 0.0070(16) 0.0006(16) Al2 0.029(2) 0.034(2) 0.0229(17) -0.0005(14) 0.0070(16) 0.0026(17) I1 0.0457(5) 0.0308(5) 0.0298(4) -0.0035(3) 0.0119(4) 0.0053(4) I2 0.0375(5) 0.0312(5) 0.0322(4) 0.0060(3) 0.0099(4) -0.0023(4) I3 0.0523(6) 0.0353(5) 0.0258(4) -0.0008(3) 0.0152(4) 0.0032(4) I4 0.0491(6) 0.0490(6) 0.0371(5) 0.0161(4) 0.0114(4) 0.0129(5) I5 0.0371(5) 0.0327(5) 0.0402(5) -0.0085(3) 0.0112(4) -0.0012(4) I6 0.0348(5) 0.0412(5) 0.0357(4) -0.0016(4) 0.0102(4) -0.0072(4) S1 0.0310(17) 0.0346(18) 0.0231(14) 0.0025(12) 0.0038(13) -0.0011(14) S2 0.0326(17) 0.0363(19) 0.0252(15) 0.0024(12) 0.0087(13) -0.0009(15) S3 0.0397(19) 0.0268(18) 0.0323(16) 0.0024(12) 0.0108(14) 0.0056(14) S4 0.0321(17) 0.0263(17) 0.0296(15) -0.0038(12) 0.0076(13) 0.0007(14) C1 0.054(9) 0.050(9) 0.023(6) 0.002(6) 0.004(6) -0.008(7) C2 0.029(7) 0.062(10) 0.042(8) 0.002(6) -0.001(6) -0.004(7) C3 0.027(7) 0.051(9) 0.036(7) 0.014(6) 0.013(6) 0.013(6) C4 0.046(9) 0.040(9) 0.043(8) 0.017(6) -0.004(7) -0.002(7) C5 0.071(10) 0.026(8) 0.038(7) 0.010(5) 0.011(7) 0.009(7) C6 0.028(7) 0.031(7) 0.027(6) -0.002(5) 0.001(5) 0.011(6) C7 0.047(8) 0.043(8) 0.025(6) -0.004(5) 0.007(6) 0.012(7) C8 0.023(7) 0.049(9) 0.040(7) 0.002(6) 0.006(6) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 S1 2.431(4) . ? Al1 S4 2.448(4) . ? Al1 S3 2.533(5) . ? Al1 S2 2.546(5) . ? Al1 I1 2.612(4) . ? Al1 I2 2.635(4) . ? Al2 I4 2.523(3) . ? Al2 I3 2.526(4) . ? Al2 I6 2.546(4) . ? Al2 I5 2.549(4) . ? S1 C1 1.812(12) . ? S1 C2 1.814(14) . ? S2 C4 1.783(13) . ? S2 C3 1.817(12) . ? S3 C5 1.745(11) . ? S3 C6 1.845(11) . ? S4 C7 1.806(12) . ? S4 C8 1.807(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.539(16) . ? 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 1.495(15) . ? 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 . ? 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 S1 Al1 S4 160.9(2) . . ? S1 Al1 S3 84.84(15) . . ? S4 Al1 S3 83.28(14) . . ? S1 Al1 S2 83.46(15) . . ? S4 Al1 S2 79.24(14) . . ? S3 Al1 S2 76.13(15) . . ? S1 Al1 I1 99.17(14) . . ? S4 Al1 I1 89.96(14) . . ? S3 Al1 I1 168.65(17) . . ? S2 Al1 I1 93.69(14) . . ? S1 Al1 I2 94.43(13) . . ? S4 Al1 I2 101.02(15) . . ? S3 Al1 I2 92.95(14) . . ? S2 Al1 I2 169.01(18) . . ? I1 Al1 I2 97.30(13) . . ? I4 Al2 I3 108.30(14) . . ? I4 Al2 I6 108.68(14) . . ? I3 Al2 I6 112.43(12) . . ? I4 Al2 I5 111.51(12) . . ? I3 Al2 I5 107.67(14) . . ? I6 Al2 I5 108.29(14) . . ? C1 S1 C2 100.4(6) . . ? C1 S1 Al1 108.2(5) . . ? C2 S1 Al1 99.6(4) . . ? C4 S2 C3 102.3(6) . . ? C4 S2 Al1 111.6(5) . . ? C3 S2 Al1 102.5(4) . . ? C5 S3 C6 101.9(6) . . ? C5 S3 Al1 112.9(5) . . ? C6 S3 Al1 96.5(4) . . ? C7 S4 C8 103.7(7) . . ? C7 S4 Al1 105.1(4) . . ? C8 S4 Al1 107.7(4) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 109.4(9) . . ? C3 C2 H2A 109.8 . . ? S1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? S1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C2 C3 S2 111.1(9) . . ? C2 C3 H3A 109.4 . . ? S2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? S2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 S3 109.8(9) . . ? 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 112.3(8) . . ? C6 C7 H7A 109.1 . . ? S4 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? S4 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 S1 C2 C3 170.4(9) . . . . ? Al1 S1 C2 C3 59.6(9) . . . . ? S1 C2 C3 S2 -63.0(11) . . . . ? C4 S2 C3 C2 -84.6(10) . . . . ? Al1 S2 C3 C2 31.1(10) . . . . ? C5 S3 C6 C7 -173.4(9) . . . . ? Al1 S3 C6 C7 -58.3(9) . . . . ? S3 C6 C7 S4 62.0(11) . . . . ? C8 S4 C7 C6 83.5(10) . . . . ? Al1 S4 C7 C6 -29.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.731 _refine_diff_density_min -1.516 _refine_diff_density_rms 0.283 _iucr_refine_instruction_details ; Add final .res file here for Acta Cryst publications or if required. ; _database_code_depnum_ccdc_archive 'CCDC 966351' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2013kg27rml _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2013-08-05 _chemical_name_systematic ; 1,3-di-tert-butyl-3-[3-(tert-butyltellanyl)propyl]-1\l^4^,2,3-tritelluran-1-ium tetrachloroaluminate ; # [C18H39Te4]+ # 1,3-di-tert-butyl-3-[3-(tert-butyltellanyl)propyl]-1l4,2,3-tritelluran-1-ium # '1l4' is 1 lambda superscript 4 (cif 1\l^4^) (ACD I-Lab2 (defaults)) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H39 Te4 1+, Al Cl4 1-' _chemical_formula_sum 'C18 H39 Al Cl4 Te4' _chemical_formula_weight 934.67 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _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 10.0158(11) _cell_length_b 12.5236(15) _cell_length_c 14.0488(15) _cell_angle_alpha 113.209(8) _cell_angle_beta 90.417(6) _cell_angle_gamma 105.465(7) _cell_volume 1548.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5064 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 34.8 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 4.109 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8209 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details ;Jacobson, R.A. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator ? _diffrn_radiation_collimation 'Confocal mirrors, VHF VariMax ' _diffrn_source 'Rotating anode X-ray tube' _diffrn_source_type 'Rigaku FR-E+ Superbright' _diffrn_measurement_device 'Four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 ' _diffrn_measurement_method 'Profile data from \w-scans' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 20728 # Is this correct? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11817 _diffrn_reflns_av_R_equivalents 0.1494 _diffrn_reflns_av_sigmaI/netI 0.2522 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5448 _reflns_number_gt 2446 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5448 _refine_ls_number_parameters 253 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.919 _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 C1 C 0.8148(18) 0.1858(17) 1.0714(13) 0.036(4) Uani 1 1 d U . . C2 C 0.6659(17) 0.1386(16) 1.0243(12) 0.036(4) Uani 1 1 d U . . H2A H 0.6155 0.1958 1.0640 0.054 Uiso 1 1 calc R . . H2B H 0.6235 0.0595 1.0263 0.054 Uiso 1 1 calc R . . H2C H 0.6608 0.1295 0.9517 0.054 Uiso 1 1 calc R . . C3 C 0.8913(17) 0.0930(16) 1.0139(13) 0.040(4) Uani 1 1 d U . . H3A H 0.8579 0.0215 1.0296 0.061 Uiso 1 1 calc R . . H3B H 0.9919 0.1294 1.0366 0.061 Uiso 1 1 calc R . . H3C H 0.8731 0.0686 0.9385 0.061 Uiso 1 1 calc R . . C4 C 0.8273(17) 0.2201(17) 1.1891(12) 0.042(5) Uani 1 1 d U . . H4A H 0.7576 0.2615 1.2194 0.062 Uiso 1 1 calc R . . H4B H 0.9210 0.2744 1.2215 0.062 Uiso 1 1 calc R . . H4C H 0.8113 0.1464 1.2017 0.062 Uiso 1 1 calc R . . C5 C 0.7617(18) 0.4435(17) 1.0856(13) 0.042(4) Uani 1 1 d U . . H5A H 0.7146 0.4309 1.1437 0.050 Uiso 1 1 calc R . . H5B H 0.8052 0.5319 1.1083 0.050 Uiso 1 1 calc R . . C6 C 0.6525(16) 0.3967(16) 0.9904(12) 0.036(4) Uani 1 1 d U . . H6A H 0.5977 0.3125 0.9766 0.043 Uiso 1 1 calc R . . H6B H 0.5874 0.4469 1.0082 0.043 Uiso 1 1 calc R . . C7 C 0.7086(18) 0.3969(17) 0.8904(13) 0.041(4) Uani 1 1 d U . . H7A H 0.7633 0.4809 0.9034 0.049 Uiso 1 1 calc R . . H7B H 0.6288 0.3716 0.8364 0.049 Uiso 1 1 calc R . . C8 C 0.882(2) 0.3144(17) 0.5600(13) 0.044(4) Uani 1 1 d U . . C9 C 0.8558(18) 0.2611(15) 0.4415(12) 0.036(4) Uani 1 1 d U . . H9A H 0.9118 0.3195 0.4164 0.054 Uiso 1 1 calc R . . H9B H 0.7565 0.2440 0.4193 0.054 Uiso 1 1 calc R . . H9C H 0.8821 0.1857 0.4124 0.054 Uiso 1 1 calc R . . C10 C 1.0201(19) 0.3186(19) 0.5980(15) 0.058(6) Uani 1 1 d U . . H10A H 1.0261 0.2356 0.5764 0.088 Uiso 1 1 calc R . . H10B H 1.0354 0.3600 0.6744 0.088 Uiso 1 1 calc R . . H10C H 1.0914 0.3630 0.5688 0.088 Uiso 1 1 calc R . . C11 C 0.865(2) 0.4450(16) 0.6052(13) 0.049(5) Uani 1 1 d U . . H11A H 0.9397 0.4987 0.5860 0.074 Uiso 1 1 calc R . . H11B H 0.8713 0.4759 0.6815 0.074 Uiso 1 1 calc R . . H11C H 0.7743 0.4423 0.5767 0.074 Uiso 1 1 calc R . . C12 C 0.7649(17) 0.0491(16) 0.5533(13) 0.037(4) Uani 1 1 d U . . H12A H 0.7633 0.0216 0.4768 0.044 Uiso 1 1 calc R . . H12B H 0.8613 0.0644 0.5835 0.044 Uiso 1 1 calc R . . C13 C 0.6663(19) -0.0511(17) 0.5766(14) 0.040(4) Uani 1 1 d U . . H13A H 0.5734 -0.0785 0.5358 0.048 Uiso 1 1 calc R . . H13B H 0.6549 -0.0203 0.6518 0.048 Uiso 1 1 calc R . . C14 C 0.7292(18) -0.1570(16) 0.5468(13) 0.039(4) Uani 1 1 d U . . H14A H 0.8152 -0.1314 0.5952 0.046 Uiso 1 1 calc R . . H14B H 0.7558 -0.1767 0.4755 0.046 Uiso 1 1 calc R . . C15 C 0.6336(19) -0.2765(16) 0.7199(13) 0.036(4) Uani 1 1 d U . . C16 C 0.597(2) -0.1616(17) 0.7825(13) 0.053(5) Uani 1 1 d U . . H16A H 0.6449 -0.0977 0.7605 0.079 Uiso 1 1 calc R . . H16B H 0.6263 -0.1358 0.8569 0.079 Uiso 1 1 calc R . . H16C H 0.4958 -0.1766 0.7710 0.079 Uiso 1 1 calc R . . C17 C 0.543(2) -0.3824(17) 0.7353(14) 0.052(6) Uani 1 1 d U . . H17A H 0.5575 -0.4574 0.6843 0.078 Uiso 1 1 calc R . . H17B H 0.4451 -0.3853 0.7258 0.078 Uiso 1 1 calc R . . H17C H 0.5675 -0.3742 0.8061 0.078 Uiso 1 1 calc R . . C18 C 0.7861(17) -0.2567(18) 0.7439(13) 0.046(5) Uani 1 1 d U . . H18A H 0.8081 -0.2376 0.8179 0.069 Uiso 1 1 calc R . . H18B H 0.8400 -0.1891 0.7284 0.069 Uiso 1 1 calc R . . H18C H 0.8104 -0.3306 0.7011 0.069 Uiso 1 1 calc R . . Al1 Al 0.2722(5) 0.1743(5) 0.8015(4) 0.0334(14) Uani 1 1 d U . . Cl1 Cl 0.2608(5) 0.2567(5) 0.9648(4) 0.0506(15) Uani 1 1 d U . . Cl2 Cl 0.4141(5) 0.0686(5) 0.7700(4) 0.0520(14) Uani 1 1 d U . . Cl3 Cl 0.0689(5) 0.0598(5) 0.7246(4) 0.0526(15) Uani 1 1 d U . . Cl4 Cl 0.3442(5) 0.3120(5) 0.7455(3) 0.0429(13) Uani 1 1 d U . . Te1 Te 0.92233(12) 0.35351(11) 1.05372(9) 0.0341(4) Uani 1 1 d U . . Te2 Te 0.83863(12) 0.27923(12) 0.83079(9) 0.0344(4) Uani 1 1 d U . . Te3 Te 0.70919(13) 0.21394(12) 0.61529(9) 0.0367(4) Uani 1 1 d U . . Te4 Te 0.58738(13) -0.31980(12) 0.55155(9) 0.0421(4) Uani 1 1 d U . . 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 C1 0.032(8) 0.041(9) 0.033(8) 0.015(8) -0.001(7) 0.010(7) C2 0.037(8) 0.039(11) 0.037(10) 0.021(9) 0.000(7) 0.011(7) C3 0.023(9) 0.038(8) 0.050(11) 0.015(9) 0.001(8) -0.001(8) C4 0.023(10) 0.058(13) 0.033(8) 0.020(8) -0.005(7) -0.007(10) C5 0.041(10) 0.043(11) 0.037(7) 0.010(9) 0.005(7) 0.016(9) C6 0.021(8) 0.030(10) 0.044(9) 0.001(8) 0.006(6) 0.012(8) C7 0.038(11) 0.050(12) 0.051(7) 0.028(8) 0.016(7) 0.025(9) C8 0.050(9) 0.039(8) 0.035(7) 0.015(8) -0.006(8) 0.003(9) C9 0.050(12) 0.012(9) 0.040(7) 0.008(7) 0.005(7) 0.005(9) C10 0.038(8) 0.066(15) 0.063(13) 0.030(12) -0.003(9) -0.002(10) C11 0.059(13) 0.034(8) 0.039(11) 0.009(8) 0.010(10) 0.000(9) C12 0.028(10) 0.041(7) 0.036(8) 0.015(7) -0.017(8) 0.001(7) C13 0.043(11) 0.051(8) 0.045(11) 0.037(9) 0.001(9) 0.016(8) C14 0.043(11) 0.043(9) 0.033(10) 0.016(9) 0.012(8) 0.016(7) C15 0.037(9) 0.026(9) 0.042(8) 0.015(8) 0.002(8) 0.007(8) C16 0.074(14) 0.037(10) 0.033(8) -0.002(8) -0.012(10) 0.020(10) C17 0.050(11) 0.040(10) 0.045(11) 0.016(9) -0.004(10) -0.018(9) C18 0.034(8) 0.063(14) 0.044(11) 0.030(11) -0.005(8) 0.007(9) Al1 0.027(3) 0.035(3) 0.034(3) 0.009(3) 0.001(2) 0.011(3) Cl1 0.047(3) 0.062(4) 0.037(3) 0.018(3) 0.007(2) 0.011(3) Cl2 0.040(3) 0.050(3) 0.076(4) 0.030(3) 0.012(3) 0.023(3) Cl3 0.029(3) 0.051(3) 0.060(3) 0.009(3) -0.006(2) 0.007(2) Cl4 0.046(3) 0.049(3) 0.042(3) 0.024(3) 0.004(2) 0.019(3) Te1 0.0276(7) 0.0388(8) 0.0329(7) 0.0132(6) 0.0010(5) 0.0072(6) Te2 0.0301(7) 0.0396(8) 0.0348(7) 0.0160(6) 0.0040(6) 0.0113(6) Te3 0.0348(8) 0.0422(8) 0.0356(7) 0.0204(6) 0.0001(6) 0.0086(7) Te4 0.0467(9) 0.0378(8) 0.0358(7) 0.0154(6) -0.0060(6) 0.0024(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.49(2) . ? C1 C3 1.53(2) . ? C1 C4 1.53(2) . ? C1 Te1 2.200(19) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.53(2) . ? C5 Te1 2.154(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.52(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 Te2 2.153(17) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.46(2) . ? C8 C9 1.52(2) . ? C8 C11 1.56(3) . ? C8 Te3 2.193(19) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.52(2) . ? C12 Te3 2.130(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.53(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 Te4 2.177(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.49(2) . ? C15 C18 1.50(2) . ? C15 C16 1.51(2) . ? C15 Te4 2.223(17) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Al1 Cl2 2.125(7) . ? Al1 Cl4 2.128(8) . ? Al1 Cl1 2.131(7) . ? Al1 Cl3 2.136(7) . ? Te1 Te2 2.9370(17) . ? Te2 Te3 2.9903(17) . ? 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 C2 C1 C3 109.5(14) . . ? C2 C1 C4 111.3(14) . . ? C3 C1 C4 112.7(16) . . ? C2 C1 Te1 111.2(13) . . ? C3 C1 Te1 106.4(11) . . ? C4 C1 Te1 105.6(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Te1 112.5(11) . . ? C6 C5 H5A 109.1 . . ? Te1 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? Te1 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 116.1(14) . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C5 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 Te2 114.0(12) . . ? C6 C7 H7A 108.8 . . ? Te2 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? Te2 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C10 C8 C9 112.4(17) . . ? C10 C8 C11 109.8(16) . . ? C9 C8 C11 109.2(15) . . ? C10 C8 Te3 114.2(13) . . ? C9 C8 Te3 108.1(11) . . ? C11 C8 Te3 102.7(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 Te3 112.2(12) . . ? C13 C12 H12A 109.2 . . ? Te3 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? Te3 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 108.1(15) . . ? C12 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? C12 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? C13 C14 Te4 113.3(12) . . ? C13 C14 H14A 108.9 . . ? Te4 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? Te4 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C17 C15 C18 113.4(17) . . ? C17 C15 C16 111.6(16) . . ? C18 C15 C16 109.6(15) . . ? C17 C15 Te4 105.3(11) . . ? C18 C15 Te4 108.5(12) . . ? C16 C15 Te4 108.1(13) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Cl2 Al1 Cl4 108.1(3) . . ? Cl2 Al1 Cl1 111.0(3) . . ? Cl4 Al1 Cl1 109.4(3) . . ? Cl2 Al1 Cl3 109.3(3) . . ? Cl4 Al1 Cl3 110.5(3) . . ? Cl1 Al1 Cl3 108.4(3) . . ? C5 Te1 C1 100.1(7) . . ? C5 Te1 Te2 87.6(5) . . ? C1 Te1 Te2 100.5(4) . . ? C7 Te2 Te1 82.8(5) . . ? C7 Te2 Te3 88.4(5) . . ? Te1 Te2 Te3 170.33(6) . . ? C12 Te3 C8 94.6(7) . . ? C12 Te3 Te2 92.4(4) . . ? C8 Te3 Te2 100.3(5) . . ? C14 Te4 C15 99.0(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.499 _refine_diff_density_min -1.578 _refine_diff_density_rms 0.272 _database_code_depnum_ccdc_archive 'CCDC 966352' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2013kg16R _audit_creation_method SHELXL-2013 # start Validation Reply Form _vrf_RINTA01_2013kg16R ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: The crystal produced poor and weak diffraction. ; _vrf_PLAT019_2013kg16R ; PROBLEM: Check _diffrn_measured_fraction_theta_full/_max 0.976 RESPONSE: Some diffraction frames were omitted from the scaling to improve the statistics. ; _vrf_PLAT020_2013kg16R ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.241 RESPONSE: The crystal produced poor and weak diffraction. ; _vrf_PLAT026_2013kg16R ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 36 % RESPONSE: The crystal produced poor and weak diffraction. ; _vrf_PLAT340_2013kg16R ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0102 Ang. RESPONSE: The crystal produced poor and weak diffraction. ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Al Cl2 S4, Al Cl4' _chemical_formula_sum 'C30 H60 Al6 Cl18 S12' _chemical_formula_weight 1605.48 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' Al Al 0.0645 0.0514 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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 21.8492(16) _cell_length_b 11.8690(9) _cell_length_c 26.0539(19) _cell_angle_alpha 90.000 _cell_angle_beta 100.82(6) _cell_angle_gamma 90 _cell_volume 6636.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_F_000 3264 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 1.226 _shelx_estimated_absorpt_T_min 0.953 _shelx_estimated_absorpt_T_max 0.988 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_process_details ; Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_source_power 2.475 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_source 'Rotating Anode' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation 'Confocal mirrors, VHF Varimax ' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_device 'four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 (Right)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen MicroMesh' _diffrn_reflns_number 29678 _diffrn_reflns_av_unetI/netI 0.3112 _diffrn_reflns_av_R_equivalents 0.2407 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.949 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_Laue_measured_fraction_full 0.961 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_point_group_measured_fraction_full 0.961 _reflns_number_total 11544 _reflns_number_gt 4131 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; ? ; _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^)+(0.0873P)^2^+97.7842P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11544 _refine_ls_number_parameters 644 _refine_ls_number_restraints 994 _refine_ls_R_factor_all 0.3050 _refine_ls_R_factor_gt 0.1227 _refine_ls_wR_factor_ref 0.3354 _refine_ls_wR_factor_gt 0.2363 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.00731(11) -0.08200(18) 0.28746(8) 0.0799(7) Uani 1 1 d . U . . . Cl2 Cl 0.01456(9) -0.36101(19) 0.28644(7) 0.0601(6) Uani 1 1 d . U . . . S1 S -0.09949(9) -0.38525(16) 0.35653(7) 0.0433(5) Uani 1 1 d . U . . . S2 S -0.12554(10) -0.25271(19) 0.24399(7) 0.0549(6) Uani 1 1 d . U . . . S3 S -0.11181(10) -0.12718(17) 0.36616(8) 0.0524(6) Uani 1 1 d . U . . . S4 S 0.03105(9) -0.2224(2) 0.39986(8) 0.0610(7) Uani 1 1 d . U . . . Al1 Al -0.04356(9) -0.23567(17) 0.31808(7) 0.0316(5) Uani 1 1 d . U . . . C1 C -0.1408(4) -0.4481(7) 0.2952(3) 0.063(2) Uani 1 1 d . U . . . H1A H -0.1107 -0.4803 0.2752 0.076 Uiso 1 1 calc R U . . . H1B H -0.1689 -0.5090 0.3026 0.076 Uiso 1 1 calc R U . . . C2 C -0.1788(4) -0.3527(7) 0.2637(3) 0.0667(19) Uani 1 1 d . U . . . H2A H -0.2052 -0.3148 0.2855 0.080 Uiso 1 1 calc R U . . . H2B H -0.2063 -0.3844 0.2325 0.080 Uiso 1 1 calc R U . . . C3 C -0.1701(5) -0.1244(8) 0.2344(4) 0.104(2) Uani 1 1 d . U . . . H3A H -0.1448 -0.0686 0.2192 0.125 Uiso 1 1 calc R U . . . H3B H -0.2075 -0.1398 0.2074 0.125 Uiso 1 1 calc R U . . . C4 C -0.1917(5) -0.0684(8) 0.2788(4) 0.113(2) Uani 1 1 d . U . . . H4A H -0.2155 -0.1248 0.2951 0.136 Uiso 1 1 calc R U . . . H4B H -0.2214 -0.0085 0.2641 0.136 Uiso 1 1 calc R U . . . C5 C -0.1437(5) -0.0153(8) 0.3227(4) 0.092(2) Uani 1 1 d . U . . . H5A H -0.1639 0.0417 0.3417 0.110 Uiso 1 1 calc R U . . . H5B H -0.1103 0.0220 0.3080 0.110 Uiso 1 1 calc R U . . . C6 C -0.0543(4) -0.0602(7) 0.4144(3) 0.067(2) Uani 1 1 d . U . . . H6A H -0.0297 -0.0062 0.3976 0.080 Uiso 1 1 calc R U . . . H6B H -0.0745 -0.0185 0.4396 0.080 Uiso 1 1 calc R U . . . C7 C -0.0116(4) -0.1535(8) 0.4428(3) 0.0734(19) Uani 1 1 d . U . . . H7A H -0.0372 -0.2097 0.4572 0.088 Uiso 1 1 calc R U . . . H7B H 0.0180 -0.1200 0.4723 0.088 Uiso 1 1 calc R U . . . C8 C 0.0504(4) -0.3641(8) 0.4259(3) 0.075(2) Uani 1 1 d . U . . . H8A H 0.0756 -0.4015 0.4030 0.090 Uiso 1 1 calc R U . . . H8B H 0.0774 -0.3558 0.4607 0.090 Uiso 1 1 calc R U . . . C9 C -0.0031(4) -0.4436(8) 0.4317(3) 0.075(2) Uani 1 1 d . U . . . H9A H 0.0148 -0.5083 0.4535 0.090 Uiso 1 1 calc R U . . . H9B H -0.0310 -0.4031 0.4513 0.090 Uiso 1 1 calc R U . . . C10 C -0.0425(4) -0.4897(7) 0.3823(3) 0.072(2) Uani 1 1 d . U . . . H10A H -0.0634 -0.5600 0.3900 0.086 Uiso 1 1 calc R U . . . H10B H -0.0159 -0.5070 0.3564 0.086 Uiso 1 1 calc R U . . . Cl3A Cl 0.1071(4) 0.3868(6) 0.4819(3) 0.0578(6) Uani 0.1117(14) 1 d D U P A 1 Cl4A Cl 0.0755(3) 0.1164(6) 0.4527(4) 0.0999(9) Uani 0.1117(14) 1 d D U P A 1 S5A S 0.2124(3) 0.1924(5) 0.5256(2) 0.0556(6) Uani 0.1117(14) 1 d D U P A 1 S6A S 0.2083(3) 0.1012(5) 0.40555(19) 0.0526(6) Uani 0.1117(14) 1 d D U P A 1 S7A S 0.0909(3) 0.3025(5) 0.3590(2) 0.0805(7) Uani 0.1117(14) 1 d D U P A 1 S8A S 0.2310(3) 0.3580(5) 0.4205(2) 0.0412(5) Uani 0.1117(14) 1 d D U P A 1 Al2A Al 0.14705(9) 0.24471(17) 0.44464(7) 0.0405(6) Uani 0.1117(14) 1 d D U P A 1 C11A C 0.2605(4) 0.0792(6) 0.5084(3) 0.0736(16) Uani 0.1117(14) 1 d D U P A 1 H11A H 0.2985 0.1112 0.4984 0.088 Uiso 0.1117(14) 1 calc R U P A 1 H11B H 0.2735 0.0295 0.5390 0.088 Uiso 0.1117(14) 1 calc R U P A 1 C12A C 0.2248(7) 0.0109(6) 0.4630(2) 0.0741(19) Uani 0.1117(14) 1 d D U P A 1 H12A H 0.1854 -0.0172 0.4718 0.089 Uiso 0.1117(14) 1 calc R U P A 1 H12B H 0.2499 -0.0547 0.4560 0.089 Uiso 0.1117(14) 1 calc R U P A 1 C13A C 0.1548(5) 0.0285(7) 0.3559(3) 0.0787(17) Uani 0.1117(14) 1 d D U P A 1 H13A H 0.1758 -0.0373 0.3435 0.094 Uiso 0.1117(14) 1 calc R U P A 1 H13B H 0.1190 0.0006 0.3706 0.094 Uiso 0.1117(14) 1 calc R U P A 1 C14A C 0.1318(4) 0.1062(6) 0.3106(3) 0.0921(18) Uani 0.1117(14) 1 d D U P A 1 H14A H 0.1184 0.0590 0.2792 0.111 Uiso 0.1117(14) 1 calc R U P A 1 H14B H 0.1676 0.1519 0.3044 0.111 Uiso 0.1117(14) 1 calc R U P A 1 C15A C 0.0788(4) 0.1866(5) 0.3146(3) 0.0939(16) Uani 0.1117(14) 1 d D U P A 1 H15A H 0.0443 0.1410 0.3236 0.113 Uiso 0.1117(14) 1 calc R U P A 1 H15B H 0.0637 0.2179 0.2793 0.113 Uiso 0.1117(14) 1 calc R U P A 1 C16A C 0.1449(4) 0.3953(7) 0.3335(3) 0.0714(15) Uani 0.1117(14) 1 d D U P A 1 H16A H 0.1725 0.3499 0.3156 0.086 Uiso 0.1117(14) 1 calc R U P A 1 H16B H 0.1211 0.4480 0.3078 0.086 Uiso 0.1117(14) 1 calc R U P A 1 C17A C 0.1842(4) 0.4621(6) 0.3781(3) 0.0679(15) Uani 0.1117(14) 1 d D U P A 1 H17A H 0.1571 0.5045 0.3978 0.081 Uiso 0.1117(14) 1 calc R U P A 1 H17B H 0.2115 0.5162 0.3642 0.081 Uiso 0.1117(14) 1 calc R U P A 1 C18A C 0.2686(5) 0.4345(7) 0.4772(3) 0.0655(15) Uani 0.1117(14) 1 d D U P A 1 H18A H 0.2965 0.4927 0.4670 0.079 Uiso 0.1117(14) 1 calc R U P A 1 H18B H 0.2370 0.4725 0.4938 0.079 Uiso 0.1117(14) 1 calc R U P A 1 C19A C 0.3053(4) 0.3532(5) 0.5146(3) 0.0702(16) Uani 0.1117(14) 1 d D U P A 1 H19A H 0.3420 0.3923 0.5348 0.084 Uiso 0.1117(14) 1 calc R U P A 1 H19B H 0.3205 0.2917 0.4946 0.084 Uiso 0.1117(14) 1 calc R U P A 1 C20A C 0.2674(4) 0.3027(6) 0.5522(3) 0.0591(15) Uani 0.1117(14) 1 d D U P A 1 H20A H 0.2439 0.3642 0.5654 0.071 Uiso 0.1117(14) 1 calc R U P A 1 H20B H 0.2966 0.2714 0.5825 0.071 Uiso 0.1117(14) 1 calc R U P A 1 Cl3B Cl 0.13603(10) 0.37973(19) 0.50069(8) 0.0578(6) Uani 0.8883(14) 1 d D U P A 2 Cl4B Cl 0.05291(10) 0.1782(3) 0.43029(9) 0.0999(9) Uani 0.8883(14) 1 d D U P A 2 S5B S 0.18716(11) 0.11743(18) 0.51447(8) 0.0556(6) Uani 0.8883(14) 1 d D U P A 2 S6B S 0.18424(10) 0.09977(17) 0.38818(8) 0.0526(6) Uani 0.8883(14) 1 d D U P A 2 S7B S 0.12487(12) 0.3721(2) 0.36927(9) 0.0805(7) Uani 0.8883(14) 1 d D U P A 2 S8B S 0.25571(9) 0.30648(17) 0.44441(7) 0.0412(5) Uani 0.8883(14) 1 d D U P A 2 Al2B Al 0.14705(9) 0.24471(17) 0.44464(7) 0.0405(6) Uani 0.8883(14) 1 d D U P A 2 C11B C 0.2276(3) 0.0098(5) 0.4839(2) 0.0736(16) Uani 0.8883(14) 1 d D U P A 2 H11C H 0.2681 0.0387 0.4777 0.088 Uiso 0.8883(14) 1 calc R U P A 2 H11D H 0.2352 -0.0578 0.5065 0.088 Uiso 0.8883(14) 1 calc R U P A 2 C12B C 0.1848(4) -0.0186(5) 0.4323(2) 0.0741(19) Uani 0.8883(14) 1 d D U P A 2 H12C H 0.1420 -0.0334 0.4382 0.089 Uiso 0.8883(14) 1 calc R U P A 2 H12D H 0.2000 -0.0870 0.4169 0.089 Uiso 0.8883(14) 1 calc R U P A 2 C13B C 0.1232(4) 0.0838(5) 0.3327(2) 0.0787(17) Uani 0.8883(14) 1 d D U P A 2 H13C H 0.1308 0.0152 0.3131 0.094 Uiso 0.8883(14) 1 calc R U P A 2 H13D H 0.0830 0.0745 0.3444 0.094 Uiso 0.8883(14) 1 calc R U P A 2 C14B C 0.1200(4) 0.1848(5) 0.2974(2) 0.0921(18) Uani 0.8883(14) 1 d D U P A 2 H14C H 0.0963 0.1618 0.2628 0.111 Uiso 0.8883(14) 1 calc R U P A 2 H14D H 0.1630 0.2011 0.2927 0.111 Uiso 0.8883(14) 1 calc R U P A 2 C15B C 0.0923(4) 0.2947(5) 0.3114(2) 0.0939(16) Uani 0.8883(14) 1 d D U P A 2 H15C H 0.0483 0.2793 0.3132 0.113 Uiso 0.8883(14) 1 calc R U P A 2 H15D H 0.0919 0.3463 0.2815 0.113 Uiso 0.8883(14) 1 calc R U P A 2 C16B C 0.2012(2) 0.4165(7) 0.3582(2) 0.0714(15) Uani 0.8883(14) 1 d D U P A 2 H16C H 0.2205 0.3557 0.3406 0.086 Uiso 0.8883(14) 1 calc R U P A 2 H16D H 0.1970 0.4842 0.3356 0.086 Uiso 0.8883(14) 1 calc R U P A 2 C17B C 0.2417(3) 0.4430(5) 0.4113(2) 0.0679(15) Uani 0.8883(14) 1 d D U P A 2 H17C H 0.2197 0.4948 0.4315 0.081 Uiso 0.8883(14) 1 calc R U P A 2 H17D H 0.2815 0.4781 0.4069 0.081 Uiso 0.8883(14) 1 calc R U P A 2 C18B C 0.2884(4) 0.3408(5) 0.51091(19) 0.0655(15) Uani 0.8883(14) 1 d D U P A 2 H18C H 0.3269 0.3857 0.5123 0.079 Uiso 0.8883(14) 1 calc R U P A 2 H18D H 0.2584 0.3864 0.5262 0.079 Uiso 0.8883(14) 1 calc R U P A 2 C19B C 0.3031(3) 0.2356(5) 0.5414(2) 0.0702(16) Uani 0.8883(14) 1 d D U P A 2 H19C H 0.3371 0.2515 0.5714 0.084 Uiso 0.8883(14) 1 calc R U P A 2 H19D H 0.3189 0.1794 0.5190 0.084 Uiso 0.8883(14) 1 calc R U P A 2 C20B C 0.2492(2) 0.1839(6) 0.5619(2) 0.0591(15) Uani 0.8883(14) 1 d D U P A 2 H20C H 0.2301 0.2436 0.5803 0.071 Uiso 0.8883(14) 1 calc R U P A 2 H20D H 0.2663 0.1265 0.5883 0.071 Uiso 0.8883(14) 1 calc R U P A 2 Cl5 Cl 0.43639(8) 0.39430(14) 0.46270(7) 0.0455(5) Uani 1 1 d D U . . . Cl6 Cl 0.40399(8) 0.11765(14) 0.45536(6) 0.0383(5) Uani 1 1 d D U . . . S9 S 0.55214(8) 0.20743(16) 0.48015(7) 0.0466(6) Uani 1 1 d D U . . . S10 S 0.49642(8) 0.09536(14) 0.36616(7) 0.0417(5) Uani 1 1 d D U . . . S11 S 0.36845(8) 0.27793(15) 0.34939(6) 0.0365(5) Uani 1 1 d D U . . . S12 S 0.51400(8) 0.35702(14) 0.36292(7) 0.0384(5) Uani 1 1 d D U . . . Al3 Al 0.45680(8) 0.24366(15) 0.41900(7) 0.0290(5) Uani 1 1 d D U . . . C21 C 0.5904(2) 0.0977(4) 0.4500(2) 0.0525(18) Uani 1 1 d D U . . . H21A H 0.6150 0.1317 0.4257 0.063 Uiso 1 1 calc R U . . . H21B H 0.6193 0.0558 0.4772 0.063 Uiso 1 1 calc R U . . . C22 C 0.5425(3) 0.0171(4) 0.4201(2) 0.0562(19) Uani 1 1 d D U . . . H22A H 0.5153 -0.0126 0.4434 0.067 Uiso 1 1 calc R U . . . H22B H 0.5637 -0.0472 0.4066 0.067 Uiso 1 1 calc R U . . . C23 C 0.4311(2) 0.0049(4) 0.3406(2) 0.0504(18) Uani 1 1 d D U . . . H23A H 0.4462 -0.0628 0.3246 0.061 Uiso 1 1 calc R U . . . H23B H 0.4107 -0.0201 0.3696 0.061 Uiso 1 1 calc R U . . . C24 C 0.3847(3) 0.0666(5) 0.3004(2) 0.057(2) Uani 1 1 d D U . . . H24A H 0.3594 0.0094 0.2783 0.069 Uiso 1 1 calc R U . . . H24B H 0.4084 0.1083 0.2776 0.069 Uiso 1 1 calc R U . . . C25 C 0.3399(3) 0.1494(4) 0.3185(2) 0.0521(19) Uani 1 1 d D U . . . H25A H 0.3182 0.1086 0.3429 0.062 Uiso 1 1 calc R U . . . H25B H 0.3081 0.1693 0.2875 0.062 Uiso 1 1 calc R U . . . C26 C 0.4007(2) 0.3578(4) 0.3007(2) 0.0439(17) Uani 1 1 d D U . . . H26A H 0.4204 0.3056 0.2791 0.053 Uiso 1 1 calc R U . . . H26B H 0.3668 0.3986 0.2775 0.053 Uiso 1 1 calc R U . . . C27 C 0.4493(2) 0.4422(4) 0.3283(2) 0.0450(18) Uani 1 1 d D U . . . H27A H 0.4314 0.4893 0.3532 0.054 Uiso 1 1 calc R U . . . H27B H 0.4636 0.4921 0.3025 0.054 Uiso 1 1 calc R U . . . C28 C 0.5633(2) 0.4523(4) 0.4066(2) 0.0475(18) Uani 1 1 d D U . . . H28A H 0.5795 0.5123 0.3864 0.057 Uiso 1 1 calc R U . . . H28B H 0.5392 0.4882 0.4308 0.057 Uiso 1 1 calc R U . . . C29 C 0.6161(3) 0.3856(4) 0.4369(2) 0.0574(19) Uani 1 1 d D U . . . H29A H 0.6525 0.4362 0.4465 0.069 Uiso 1 1 calc R U . . . H29B H 0.6277 0.3264 0.4137 0.069 Uiso 1 1 calc R U . . . C30 C 0.6036(3) 0.3296(4) 0.4863(2) 0.0579(18) Uani 1 1 d D U . . . H30A H 0.5860 0.3874 0.5068 0.070 Uiso 1 1 calc R U . . . H30B H 0.6442 0.3065 0.5073 0.070 Uiso 1 1 calc R U . . . Al4 Al -0.29585(9) -0.21699(17) 0.06975(8) 0.0334(6) Uani 1 1 d . U . . . Cl7 Cl -0.39079(9) -0.26600(18) 0.06430(8) 0.0570(6) Uani 1 1 d . U . . . Cl8 Cl -0.27678(9) -0.20243(16) -0.00747(6) 0.0449(5) Uani 1 1 d . U . . . Cl9 Cl -0.27634(9) -0.06139(15) 0.10927(7) 0.0452(6) Uani 1 1 d . U . . . Cl10 Cl -0.23714(9) -0.34514(16) 0.11156(7) 0.0506(6) Uani 1 1 d . U . . . Al5 Al -0.10432(11) 0.26396(17) 0.20458(8) 0.0445(7) Uani 1 1 d . U . . . Cl11 Cl -0.13647(10) 0.42708(15) 0.17490(7) 0.0502(6) Uani 1 1 d . U . . . Cl12 Cl -0.17275(10) 0.14348(18) 0.17322(9) 0.0659(7) Uani 1 1 d . U . . . Cl13 Cl -0.01969(10) 0.22721(17) 0.17862(10) 0.0683(7) Uani 1 1 d . U . . . Cl14 Cl -0.08942(14) 0.26276(18) 0.28789(8) 0.0837(9) Uani 1 1 d . U . . . Al6 Al 0.26927(10) -0.24146(18) 0.33398(9) 0.0421(7) Uani 1 1 d . U . . . Cl15 Cl 0.17683(8) -0.27699(17) 0.34244(7) 0.0486(6) Uani 1 1 d . U . . . Cl16 Cl 0.26234(11) -0.1326(2) 0.26709(8) 0.0710(7) Uani 1 1 d . U . . . Cl17 Cl 0.31823(12) -0.1532(3) 0.39993(8) 0.1034(9) Uani 1 1 d . U . . . Cl18 Cl 0.31410(14) -0.3912(2) 0.31896(16) 0.1482(13) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1274(15) 0.0586(11) 0.0680(11) -0.0188(10) 0.0548(10) -0.0561(11) Cl2 0.0579(11) 0.0746(13) 0.0522(10) -0.0176(10) 0.0217(8) 0.0004(11) S1 0.0551(10) 0.0399(9) 0.0363(9) -0.0001(8) 0.0121(8) -0.0118(9) S2 0.0590(12) 0.0660(12) 0.0361(9) 0.0036(10) -0.0004(9) -0.0049(10) S3 0.0612(11) 0.0427(10) 0.0577(10) -0.0086(9) 0.0225(8) 0.0035(10) S4 0.0404(10) 0.0899(14) 0.0519(10) -0.0239(11) 0.0064(9) -0.0092(11) Al1 0.0371(10) 0.0320(10) 0.0265(9) -0.0071(8) 0.0082(8) -0.0100(9) C1 0.065(4) 0.066(3) 0.057(3) -0.011(3) 0.006(3) -0.040(3) C2 0.064(3) 0.091(3) 0.040(3) -0.013(3) -0.004(3) -0.031(3) C3 0.116(5) 0.091(3) 0.089(3) 0.027(3) -0.027(3) 0.031(3) C4 0.113(5) 0.081(4) 0.128(4) 0.015(3) -0.023(3) 0.065(3) C5 0.097(5) 0.071(4) 0.104(3) 0.013(3) 0.013(3) 0.042(3) C6 0.085(4) 0.069(4) 0.053(3) -0.033(2) 0.030(3) -0.008(3) C7 0.072(4) 0.098(4) 0.049(3) -0.040(3) 0.008(2) -0.003(3) C8 0.050(3) 0.113(3) 0.059(4) -0.003(3) -0.001(3) 0.027(2) C9 0.087(4) 0.078(3) 0.058(4) 0.027(3) 0.007(3) 0.034(3) C10 0.090(4) 0.056(3) 0.068(4) 0.029(3) 0.010(3) 0.005(3) Cl3A 0.0615(12) 0.0781(12) 0.0334(9) -0.0066(10) 0.0074(8) 0.0314(11) Cl4A 0.0493(10) 0.193(2) 0.0624(13) -0.0498(14) 0.0241(9) -0.0491(13) S5A 0.0878(13) 0.0395(11) 0.0457(9) 0.0058(9) 0.0285(9) 0.0007(10) S6A 0.0646(11) 0.0486(10) 0.0515(9) -0.0282(8) 0.0286(8) -0.0224(10) S7A 0.0839(13) 0.1155(15) 0.0406(10) 0.0008(10) 0.0076(10) 0.0489(12) S8A 0.0505(10) 0.0424(10) 0.0337(9) -0.0075(8) 0.0157(7) -0.0119(9) Al2A 0.0365(10) 0.0597(11) 0.0262(8) -0.0099(8) 0.0084(8) 0.0072(9) C11A 0.104(4) 0.054(2) 0.066(2) 0.0065(19) 0.023(2) 0.025(2) C12A 0.109(4) 0.039(2) 0.080(2) -0.0113(17) 0.030(3) -0.005(3) C13A 0.073(4) 0.103(2) 0.060(2) -0.0453(17) 0.013(2) -0.008(3) C14A 0.090(4) 0.134(3) 0.052(3) -0.0333(19) 0.011(3) 0.006(3) C15A 0.099(3) 0.139(2) 0.037(2) -0.010(2) -0.003(3) 0.024(2) C16A 0.099(3) 0.080(3) 0.039(2) 0.010(2) 0.0211(19) 0.046(2) C17A 0.095(3) 0.065(3) 0.051(2) 0.011(2) 0.031(2) 0.022(2) C18A 0.058(3) 0.106(3) 0.036(2) -0.0170(18) 0.018(2) -0.026(2) C19A 0.047(3) 0.122(3) 0.042(3) -0.015(2) 0.009(2) -0.003(2) C20A 0.055(3) 0.078(3) 0.042(2) 0.0011(18) 0.0032(18) 0.013(2) Cl3B 0.0615(12) 0.0781(12) 0.0334(9) -0.0066(10) 0.0074(8) 0.0314(11) Cl4B 0.0493(10) 0.193(2) 0.0624(13) -0.0498(14) 0.0241(9) -0.0491(13) S5B 0.0878(13) 0.0395(11) 0.0457(9) 0.0058(9) 0.0285(9) 0.0007(10) S6B 0.0646(11) 0.0486(10) 0.0515(9) -0.0282(8) 0.0286(8) -0.0224(10) S7B 0.0839(13) 0.1155(15) 0.0406(10) 0.0008(10) 0.0076(10) 0.0489(12) S8B 0.0505(10) 0.0424(10) 0.0337(9) -0.0075(8) 0.0157(7) -0.0119(9) Al2B 0.0365(10) 0.0597(11) 0.0262(8) -0.0099(8) 0.0084(8) 0.0072(9) C11B 0.104(4) 0.054(2) 0.066(2) 0.0065(19) 0.023(2) 0.025(2) C12B 0.109(4) 0.039(2) 0.080(2) -0.0113(17) 0.030(3) -0.005(3) C13B 0.073(4) 0.103(2) 0.060(2) -0.0453(17) 0.013(2) -0.008(3) C14B 0.090(4) 0.134(3) 0.052(3) -0.0333(19) 0.011(3) 0.006(3) C15B 0.099(3) 0.139(2) 0.037(2) -0.010(2) -0.003(3) 0.024(2) C16B 0.099(3) 0.080(3) 0.039(2) 0.010(2) 0.0211(19) 0.046(2) C17B 0.095(3) 0.065(3) 0.051(2) 0.011(2) 0.031(2) 0.022(2) C18B 0.058(3) 0.106(3) 0.036(2) -0.0170(18) 0.018(2) -0.026(2) C19B 0.047(3) 0.122(3) 0.042(3) -0.015(2) 0.009(2) -0.003(2) C20B 0.055(3) 0.078(3) 0.042(2) 0.0011(18) 0.0032(18) 0.013(2) Cl5 0.0505(10) 0.0375(9) 0.0511(10) -0.0088(8) 0.0159(8) -0.0057(9) Cl6 0.0462(9) 0.0317(8) 0.0413(8) 0.0049(8) 0.0197(7) -0.0046(8) S9 0.0336(9) 0.0537(11) 0.0493(10) 0.0123(9) -0.0002(8) -0.0047(9) S10 0.0467(9) 0.0333(9) 0.0516(9) 0.0018(8) 0.0261(7) -0.0008(8) S11 0.0348(9) 0.0412(9) 0.0339(8) 0.0075(8) 0.0073(7) -0.0043(8) S12 0.0355(8) 0.0357(9) 0.0460(9) 0.0085(8) 0.0133(7) -0.0061(8) Al3 0.0308(9) 0.0255(9) 0.0319(9) 0.0012(8) 0.0091(8) -0.0043(8) C21 0.029(3) 0.046(3) 0.085(4) 0.032(3) 0.017(3) 0.003(2) C22 0.055(3) 0.041(3) 0.074(4) 0.017(3) 0.014(3) 0.009(3) C23 0.067(3) 0.031(3) 0.060(4) -0.008(3) 0.028(3) -0.014(2) C24 0.068(3) 0.045(3) 0.057(4) -0.014(3) 0.008(3) -0.035(3) C25 0.057(3) 0.039(3) 0.052(4) 0.013(3) -0.011(3) -0.022(2) C26 0.046(3) 0.040(3) 0.045(3) 0.016(2) 0.004(2) -0.008(2) C27 0.044(3) 0.038(3) 0.053(3) 0.017(2) 0.009(3) -0.003(2) C28 0.036(3) 0.039(3) 0.066(4) 0.004(3) 0.005(3) -0.005(2) C29 0.038(3) 0.064(4) 0.067(3) 0.016(3) 0.001(2) -0.012(3) C30 0.047(3) 0.062(3) 0.060(3) 0.011(3) -0.002(3) -0.019(3) Al4 0.0338(10) 0.0342(11) 0.0296(10) 0.0006(9) -0.0003(9) -0.0013(10) Cl7 0.0418(10) 0.0684(13) 0.0596(11) 0.0013(11) 0.0064(9) -0.0182(10) Cl8 0.0581(11) 0.0457(10) 0.0324(8) -0.0011(8) 0.0119(8) 0.0031(10) Cl9 0.0560(11) 0.0385(9) 0.0379(9) -0.0010(8) 0.0007(9) -0.0023(9) Cl10 0.0610(11) 0.0455(10) 0.0435(10) 0.0096(9) 0.0052(9) 0.0151(10) Al5 0.0638(14) 0.0272(11) 0.0386(11) -0.0023(10) -0.0003(11) -0.0037(11) Cl11 0.0676(12) 0.0408(10) 0.0376(9) 0.0002(9) -0.0017(9) 0.0113(10) Cl12 0.0701(13) 0.0526(11) 0.0701(13) -0.0083(11) 0.0008(11) -0.0227(11) Cl13 0.0597(11) 0.0459(11) 0.0979(15) -0.0096(12) 0.0108(11) 0.0091(10) Cl14 0.150(2) 0.0471(12) 0.0458(11) -0.0008(10) -0.0029(13) -0.0018(15) Al6 0.0383(11) 0.0399(12) 0.0473(12) 0.0021(10) 0.0060(10) -0.0044(10) Cl15 0.0395(9) 0.0546(11) 0.0515(10) -0.0083(10) 0.0083(8) -0.0043(9) Cl16 0.0781(14) 0.0840(14) 0.0469(11) 0.0098(11) 0.0016(10) -0.0225(13) Cl17 0.0962(15) 0.163(2) 0.0407(11) 0.0196(13) -0.0140(11) -0.0824(14) Cl18 0.1202(16) 0.0692(15) 0.286(3) 0.0283(18) 0.1163(17) 0.0370(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Al1 2.197(3) . ? Cl2 Al1 2.213(3) . ? S1 C10 1.795(9) . ? S1 C1 1.839(8) . ? S1 Al1 2.472(3) . ? S2 C3 1.799(10) . ? S2 C2 1.804(9) . ? S2 Al1 2.383(3) . ? S3 C6 1.788(8) . ? S3 C5 1.798(10) . ? S3 Al1 2.480(3) . ? S4 C7 1.782(9) . ? S4 C8 1.833(10) . ? S4 Al1 2.433(3) . ? C1 C2 1.546(11) . ? C3 C4 1.488(16) . ? C4 C5 1.534(14) . ? C6 C7 1.545(12) . ? C8 C9 1.532(13) . ? C9 C10 1.511(12) . ? Cl3A Al2A 2.206(7) . ? Cl4A Al2A 2.220(7) . ? S5A C11A 1.813(9) . ? S5A C20A 1.823(8) . ? S5A Al2A 2.397(5) . ? S6A C13A 1.793(9) . ? S6A C12A 1.822(8) . ? S6A Al2A 2.498(6) . ? S7A C15A 1.784(9) . ? S7A C16A 1.826(9) . ? S7A Al2A 2.435(5) . ? S8A C18A 1.795(8) . ? S8A C17A 1.836(9) . ? S8A Al2A 2.450(6) . ? C11A C12A 1.521(10) . ? C13A C14A 1.508(10) . ? C14A C15A 1.519(10) . ? C16A C17A 1.530(9) . ? C18A C19A 1.493(9) . ? C19A C20A 1.521(10) . ? S5B C11B 1.819(7) . ? S5B C20B 1.833(6) . ? S6B C13B 1.783(6) . ? S6B C12B 1.814(6) . ? S7B C15B 1.795(6) . ? S7B C16B 1.823(6) . ? S8B C18B 1.793(5) . ? S8B C17B 1.834(6) . ? C11B C12B 1.525(8) . ? C13B C14B 1.504(8) . ? C14B C15B 1.511(8) . ? C16B C17B 1.529(7) . ? C18B C19B 1.482(8) . ? C19B C20B 1.511(8) . ? Cl5 Al3 2.210(3) . ? Cl6 Al3 2.208(2) . ? S9 C21 1.806(6) . ? S9 C30 1.823(6) . ? S9 Al3 2.412(2) . ? S10 C23 1.810(5) . ? S10 C22 1.823(5) . ? S10 Al3 2.488(3) . ? S11 C25 1.782(5) . ? S11 C26 1.827(6) . ? S11 Al3 2.422(2) . ? S12 C28 1.810(5) . ? S12 C27 1.832(5) . ? S12 Al3 2.489(3) . ? C21 C22 1.518(7) . ? C23 C24 1.505(7) . ? C24 C25 1.522(8) . ? C26 C27 1.537(7) . ? C28 C29 1.496(7) . ? C29 C30 1.520(7) . ? Al4 Cl9 2.118(3) . ? Al4 Cl7 2.133(3) . ? Al4 Cl8 2.137(3) . ? Al4 Cl10 2.150(3) . ? Al5 Cl12 2.119(3) . ? Al5 Cl13 2.130(3) . ? Al5 Cl14 2.134(3) . ? Al5 Cl11 2.153(3) . ? Al6 Cl18 2.102(4) . ? Al6 Cl15 2.115(3) . ? Al6 Cl17 2.122(3) . ? Al6 Cl16 2.152(3) . ? 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 C10 S1 C1 103.7(4) . . ? C10 S1 Al1 106.6(3) . . ? C1 S1 Al1 98.0(3) . . ? C3 S2 C2 103.7(5) . . ? C3 S2 Al1 110.2(3) . . ? C2 S2 Al1 104.6(3) . . ? C6 S3 C5 104.6(4) . . ? C6 S3 Al1 100.2(3) . . ? C5 S3 Al1 105.3(4) . . ? C7 S4 C8 107.5(4) . . ? C7 S4 Al1 103.7(3) . . ? C8 S4 Al1 109.5(3) . . ? Cl1 Al1 Cl2 98.72(12) . . ? Cl1 Al1 S2 92.51(10) . . ? Cl2 Al1 S2 92.17(10) . . ? Cl1 Al1 S4 92.07(10) . . ? Cl2 Al1 S4 91.88(10) . . ? S2 Al1 S4 173.36(12) . . ? Cl1 Al1 S1 169.37(13) . . ? Cl2 Al1 S1 91.72(10) . . ? S2 Al1 S1 85.05(9) . . ? S4 Al1 S1 89.58(9) . . ? Cl1 Al1 S3 92.54(11) . . ? Cl2 Al1 S3 168.08(12) . . ? S2 Al1 S3 91.23(10) . . ? S4 Al1 S3 83.77(9) . . ? S1 Al1 S3 77.19(9) . . ? C2 C1 S1 106.9(5) . . ? C1 C2 S2 108.8(6) . . ? C4 C3 S2 120.8(7) . . ? C3 C4 C5 119.4(9) . . ? C4 C5 S3 107.2(6) . . ? C7 C6 S3 107.4(6) . . ? C6 C7 S4 111.6(6) . . ? C9 C8 S4 118.3(6) . . ? C10 C9 C8 117.5(8) . . ? C9 C10 S1 108.2(6) . . ? C11A S5A C20A 104.8(5) . . ? C11A S5A Al2A 104.5(3) . . ? C20A S5A Al2A 112.9(4) . . ? C13A S6A C12A 108.2(5) . . ? C13A S6A Al2A 107.3(4) . . ? C12A S6A Al2A 96.0(4) . . ? C15A S7A C16A 105.0(5) . . ? C15A S7A Al2A 111.4(4) . . ? C16A S7A Al2A 104.7(3) . . ? C18A S8A C17A 105.8(4) . . ? C18A S8A Al2A 108.4(4) . . ? C17A S8A Al2A 99.4(4) . . ? Cl3A Al2A Cl4A 98.0(3) . . ? Cl3A Al2A S5A 91.7(2) . . ? Cl4A Al2A S5A 93.0(3) . . ? Cl3A Al2A S7A 90.9(3) . . ? Cl4A Al2A S7A 92.1(3) . . ? S5A Al2A S7A 173.8(2) . . ? Cl3A Al2A S8A 94.1(3) . . ? Cl4A Al2A S8A 167.2(3) . . ? S5A Al2A S8A 91.0(2) . . ? S7A Al2A S8A 83.3(2) . . ? Cl3A Al2A S6A 170.8(3) . . ? Cl4A Al2A S6A 90.6(3) . . ? S5A Al2A S6A 84.62(19) . . ? S7A Al2A S6A 91.96(19) . . ? S8A Al2A S6A 77.6(2) . . ? C12A C11A S5A 110.5(7) . . ? C11A C12A S6A 108.5(6) . . ? C14A C13A S6A 110.3(6) . . ? C13A C14A C15A 118.5(8) . . ? C14A C15A S7A 120.4(6) . . ? C17A C16A S7A 110.3(6) . . ? C16A C17A S8A 106.1(5) . . ? C19A C18A S8A 108.4(5) . . ? C18A C19A C20A 112.6(7) . . ? C19A C20A S5A 115.9(5) . . ? C11B S5B C20B 103.8(3) . . ? C13B S6B C12B 110.2(3) . . ? C15B S7B C16B 104.1(3) . . ? C18B S8B C17B 104.8(3) . . ? C12B C11B S5B 105.9(5) . . ? C11B C12B S6B 108.5(4) . . ? C14B C13B S6B 110.7(5) . . ? C13B C14B C15B 121.1(6) . . ? C14B C15B S7B 122.1(5) . . ? C17B C16B S7B 107.9(4) . . ? C16B C17B S8B 105.2(4) . . ? C19B C18B S8B 109.5(4) . . ? C18B C19B C20B 115.3(5) . . ? C19B C20B S5B 117.5(4) . . ? C21 S9 C30 106.5(3) . . ? C21 S9 Al3 104.71(19) . . ? C30 S9 Al3 111.00(19) . . ? C23 S10 C22 105.3(3) . . ? C23 S10 Al3 106.9(2) . . ? C22 S10 Al3 97.6(2) . . ? C25 S11 C26 106.1(3) . . ? C25 S11 Al3 110.89(19) . . ? C26 S11 Al3 104.47(18) . . ? C28 S12 C27 106.1(2) . . ? C28 S12 Al3 105.9(2) . . ? C27 S12 Al3 99.3(2) . . ? Cl6 Al3 Cl5 98.90(10) . . ? Cl6 Al3 S9 92.98(9) . . ? Cl5 Al3 S9 92.11(9) . . ? Cl6 Al3 S11 91.59(8) . . ? Cl5 Al3 S11 92.32(9) . . ? S9 Al3 S11 173.08(11) . . ? Cl6 Al3 S10 91.28(9) . . ? Cl5 Al3 S10 169.23(11) . . ? S9 Al3 S10 83.82(8) . . ? S11 Al3 S10 90.89(8) . . ? Cl6 Al3 S12 168.11(10) . . ? Cl5 Al3 S12 92.14(9) . . ? S9 Al3 S12 91.01(8) . . ? S11 Al3 S12 83.51(8) . . ? S10 Al3 S12 78.01(8) . . ? C22 C21 S9 110.3(4) . . ? C21 C22 S10 107.6(4) . . ? C24 C23 S10 110.4(4) . . ? C23 C24 C25 119.2(5) . . ? C24 C25 S11 120.1(4) . . ? C27 C26 S11 109.7(4) . . ? C26 C27 S12 105.7(3) . . ? C29 C28 S12 108.0(4) . . ? C28 C29 C30 115.7(5) . . ? C29 C30 S9 118.6(4) . . ? Cl9 Al4 Cl7 111.99(12) . . ? Cl9 Al4 Cl8 109.27(12) . . ? Cl7 Al4 Cl8 108.57(11) . . ? Cl9 Al4 Cl10 108.91(10) . . ? Cl7 Al4 Cl10 108.73(12) . . ? Cl8 Al4 Cl10 109.32(12) . . ? Cl12 Al5 Cl13 109.34(13) . . ? Cl12 Al5 Cl14 110.46(14) . . ? Cl13 Al5 Cl14 110.24(14) . . ? Cl12 Al5 Cl11 108.03(12) . . ? Cl13 Al5 Cl11 108.32(13) . . ? Cl14 Al5 Cl11 110.39(12) . . ? Cl18 Al6 Cl15 109.78(14) . . ? Cl18 Al6 Cl17 112.76(15) . . ? Cl15 Al6 Cl17 111.11(14) . . ? Cl18 Al6 Cl16 108.76(17) . . ? Cl15 Al6 Cl16 106.30(12) . . ? Cl17 Al6 Cl16 107.88(13) . . ? _refine_diff_density_max 1.212 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.157 #===END OF CIF ============================================================== #===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 ============================================================= _database_code_depnum_ccdc_archive 'CCDC 966353'