# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/138 #============================================================================ data_global _publ_contact_author # Name and address of author for correspondence ; Dr. Aravinda M. Kini Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439-4831, USA ; _publ_contact_author_phone '(630) 252-3468' _publ_contact_author_fax '(630) 252-9151' _publ_contact_author_email 'amkini@anl.gov' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Tetraalkyl and Dialkyl-substituted BEDT-TTF Derivatives and their Cation-Radical Salts: Synthesis, Structure and Properties ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Kini, Aravinda M.' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Parakka, James P.' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Geiser, Urs' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Wang, Hsien-Hau' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Rivas, Felix' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'DiNino, Ernest' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Thomas, Seddon' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Dudek, James D.' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; 'Williams, Jack M.' ; Chemistry and Materials Science Divisions Argonne National Laboratory 9700 South Cass Avenue Argonne, IL 60439, USA ; #============================================================================ data_teet _audit_creation_method SHELXL _chemical_name_systematic ; Bis(1,2-diethyl-ethylenedithio)tetrathiafulvalene ; _chemical_name_common 'Tetraethyl-ET' _chemical_formula_sum 'C18 H24 S8' _chemical_formula_weight 496.85 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' 'y, x, -z' '-y, -x, -z+1/2' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' _cell_length_a 13.9032(5) _cell_length_b 13.9032(5) _cell_length_c 23.9326(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4626.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.863 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6.053 cm. Coverage of the unique set is over 98% complete to at least 28.29\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART diffractometer' _diffrn_measurement_method 'Area detector \w-scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 27762 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5555 _reflns_number_observed 3947 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.04 (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+2.1830P] 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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef 0.0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(20) _refine_ls_number_reflns 5555 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_obs 0.0501 _refine_ls_wR_factor_all 0.1002 _refine_ls_wR_factor_obs 0.0898 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.160 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.160 _refine_ls_shift/su_max -0.075 _refine_ls_shift/esd_mean 0.015 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 1.01853(8) 1.18356(8) 0.06092(3) 0.0590(3) Uani 1 d . . S2 S 1.02381(7) 1.18715(8) -0.06235(3) 0.0583(3) Uani 1 d . . S3 S 0.87488(9) 1.33750(10) 0.07209(4) 0.0718(3) Uani 1 d . . S4 S 0.88066(9) 1.33957(9) -0.07530(4) 0.0697(3) Uani 1 d . . C1 C 1.0707(2) 1.1390(2) -0.00044(13) 0.0432(7) Uani 1 d . . C2 C 0.9432(3) 1.2660(3) 0.02683(13) 0.0493(8) Uani 1 d . . C3 C 0.9468(3) 1.2690(3) -0.02867(13) 0.0476(9) Uani 1 d . . C4 C 0.7857(3) 1.3845(3) 0.0238(2) 0.0657(12) Uani 1 d . . H4 H 0.7531(3) 1.4370(3) 0.0435(2) 0.079 Uiso 1 calc R . C5 C 0.8316(3) 1.4297(3) -0.0281(2) 0.0657(11) Uani 1 d . . H5 H 0.7791(3) 1.4609(3) -0.0486(2) 0.079 Uiso 1 calc R . C6 C 0.7076(3) 1.3116(3) 0.0091(2) 0.0837(13) Uani 1 d . . H6A H 0.6601(3) 1.3430(3) -0.0143(2) 0.100 Uiso 1 calc R . H6B H 0.7365(3) 1.2604(3) -0.0128(2) 0.100 Uiso 1 calc R . C7 C 0.6571(4) 1.2675(5) 0.0583(2) 0.123(2) Uani 1 d . . H7A H 0.6050(21) 1.2280(26) 0.0453(2) 0.185 Uiso 1 calc R . H7B H 0.6322(28) 1.3176(5) 0.0818(10) 0.185 Uiso 1 calc R . H7C H 0.7016(9) 1.2289(26) 0.0791(11) 0.185 Uiso 1 calc R . C8 C 0.9047(4) 1.5094(4) -0.0153(2) 0.092(2) Uani 1 d . . H8A H 0.8739(4) 1.5571(4) 0.0082(2) 0.110 Uiso 1 calc R . H8B H 0.9573(4) 1.4817(4) 0.0058(2) 0.110 Uiso 1 calc R . C9 C 0.9458(5) 1.5597(4) -0.0662(2) 0.127(2) Uani 1 d . . H9A H 0.9906(25) 1.6082(23) -0.0544(3) 0.190 Uiso 1 calc R . H9B H 0.8946(6) 1.5892(28) -0.0870(11) 0.190 Uiso 1 calc R . H9C H 0.9782(29) 1.5136(7) -0.0894(10) 0.190 Uiso 1 calc R . S11 S 0.51908(8) 0.51812(8) -0.06170(3) 0.0617(3) Uani 1 d . . S12 S 0.67869(8) 0.68709(8) -0.06145(3) 0.0587(3) Uani 1 d . . S13 S 0.37002(10) 0.37062(9) -0.07357(4) 0.0758(3) Uani 1 d . . S14 S 0.82670(10) 0.83647(9) -0.07360(4) 0.0733(3) Uani 1 d . . C11 C 0.5666(2) 0.5666(2) 0.0000 0.0443(10) Uani 1 d S . C12 C 0.6350(2) 0.6350(2) 0.0000 0.0451(10) Uani 1 d S . C13 C 0.4393(3) 0.4391(3) -0.02827(12) 0.0521(9) Uani 1 d . . C14 C 0.7604(3) 0.7643(3) -0.02806(12) 0.0524(8) Uani 1 d . . C15 C 0.3237(3) 0.2788(3) -0.0260(2) 0.0714(13) Uani 1 d . . H15 H 0.2709(3) 0.2473(3) -0.0459(2) 0.086 Uiso 1 calc R . C16 C 0.8761(3) 0.9243(3) -0.0245(2) 0.0750(14) Uani 1 d . . H16 H 0.9276(3) 0.9574(3) -0.0448(2) 0.090 Uiso 1 calc R . C17 C 0.3973(4) 0.2007(3) -0.0145(2) 0.0930(15) Uani 1 d . . H17A H 0.4501(4) 0.2286(3) 0.0064(2) 0.112 Uiso 1 calc R . H17B H 0.3677(4) 0.1522(3) 0.0090(2) 0.112 Uiso 1 calc R . C18 C 0.4374(4) 0.1522(4) -0.0655(2) 0.120(2) Uani 1 d . . H18A H 0.4831(25) 0.1041(23) -0.0544(3) 0.181 Uiso 1 calc R . H18B H 0.4687(28) 0.1991(7) -0.0886(9) 0.181 Uiso 1 calc R . H18C H 0.3861(6) 0.1225(28) -0.0860(10) 0.181 Uiso 1 calc R . C19 C 0.8040(4) 1.0022(4) -0.0089(2) 0.093(2) Uani 1 d . . H19A H 0.7530(4) 0.9729(4) 0.0129(2) 0.112 Uiso 1 calc R . H19B H 0.8361(4) 1.0486(4) 0.0150(2) 0.112 Uiso 1 calc R . C20 C 0.7595(5) 1.0550(4) -0.0569(2) 0.140(3) Uani 1 d . . H20A H 0.7121(27) 1.0992(27) -0.0430(3) 0.210 Uiso 1 calc R . H20B H 0.7294(33) 1.0098(5) -0.0817(12) 0.210 Uiso 1 calc R . H20C H 0.8084(8) 1.0898(30) -0.0767(13) 0.210 Uiso 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 S1 0.0620(6) 0.0737(7) 0.0413(4) -0.0058(5) -0.0002(5) 0.0322(5) S2 0.0651(6) 0.0678(7) 0.0419(4) -0.0095(5) -0.0004(5) 0.0289(5) S3 0.0767(7) 0.0907(8) 0.0481(5) -0.0177(6) -0.0043(5) 0.0466(6) S4 0.0876(8) 0.0728(7) 0.0486(5) -0.0050(5) -0.0087(5) 0.0384(6) C1 0.043(2) 0.043(2) 0.044(2) -0.006(2) 0.002(2) 0.0076(13) C2 0.048(2) 0.051(2) 0.049(2) -0.009(2) 0.001(2) 0.019(2) C3 0.046(2) 0.053(2) 0.044(2) -0.009(2) -0.003(2) 0.018(2) C4 0.065(3) 0.071(3) 0.062(2) -0.014(2) -0.008(2) 0.035(2) C5 0.074(3) 0.059(2) 0.064(2) -0.009(2) -0.006(2) 0.031(2) C6 0.076(3) 0.103(3) 0.072(3) -0.001(3) -0.004(3) 0.020(2) C7 0.095(4) 0.169(6) 0.106(4) 0.006(4) 0.011(3) 0.002(4) C8 0.105(4) 0.079(3) 0.090(4) -0.018(3) -0.005(3) 0.011(3) C9 0.143(5) 0.098(4) 0.139(5) 0.001(4) 0.020(5) -0.010(4) S11 0.0727(7) 0.0671(7) 0.0454(4) 0.0106(5) -0.0082(5) -0.0337(5) S12 0.0681(7) 0.0620(6) 0.0461(4) 0.0000(5) -0.0017(5) -0.0300(5) S13 0.1013(9) 0.0714(7) 0.0546(5) 0.0136(5) -0.0254(6) -0.0454(6) S14 0.0879(8) 0.0820(8) 0.0500(5) 0.0076(6) -0.0018(6) -0.0477(6) C11 0.042(2) 0.042(2) 0.048(2) 0.004(2) -0.004(2) -0.007(2) C12 0.044(2) 0.044(2) 0.046(2) 0.004(2) -0.004(2) -0.008(2) C13 0.059(3) 0.048(2) 0.049(2) 0.011(2) -0.011(2) -0.019(2) C14 0.056(2) 0.049(2) 0.052(2) -0.002(2) 0.003(2) -0.022(2) C15 0.074(3) 0.066(3) 0.074(2) 0.018(2) -0.019(2) -0.035(2) C16 0.089(3) 0.076(3) 0.060(2) 0.003(2) 0.005(2) -0.048(3) C17 0.100(4) 0.078(3) 0.101(4) 0.021(3) -0.012(3) -0.015(3) C18 0.127(5) 0.088(4) 0.147(5) 0.012(4) 0.020(4) 0.004(4) C19 0.119(4) 0.080(3) 0.081(3) 0.008(3) 0.004(3) -0.026(3) C20 0.211(8) 0.092(4) 0.117(4) 0.031(4) -0.020(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.751(3) . ? S1 C2 1.754(3) . ? S2 C1 1.752(3) . ? S2 C3 1.758(3) . ? S3 C2 1.751(3) . ? S3 C4 1.816(4) . ? S4 C3 1.748(3) . ? S4 C5 1.819(4) . ? C1 C1 1.343(5) 5 ? C2 C3 1.330(4) . ? C4 C6 1.526(6) . ? C4 C5 1.534(6) . ? C5 C8 1.533(6) . ? C6 C7 1.501(6) . ? C8 C9 1.516(6) . ? S11 C11 1.753(2) . ? S11 C13 1.755(3) . ? S12 C12 1.748(2) . ? S12 C14 1.755(3) . ? S13 C13 1.735(3) . ? S13 C15 1.828(4) . ? S14 C14 1.745(3) . ? S14 C16 1.829(4) . ? C11 C12 1.344(5) . ? C11 S11 1.753(2) 5 ? C12 S12 1.748(2) 5 ? C13 C13 1.353(6) 5 ? C14 C14 1.345(6) 5 ? C15 C17 1.517(6) . ? C15 C15 1.524(8) 5 ? C16 C16 1.507(8) 5 ? C16 C19 1.521(6) . ? C17 C18 1.501(6) . ? C19 C20 1.498(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 95.08(14) . . ? C1 S2 C3 94.95(14) . . ? C2 S3 C4 100.5(2) . . ? C3 S4 C5 100.8(2) . . ? C1 C1 S1 122.0(3) 5 . ? C1 C1 S2 123.1(3) 5 . ? S1 C1 S2 114.8(2) . . ? C3 C2 S3 128.4(3) . . ? C3 C2 S1 117.6(3) . . ? S3 C2 S1 114.0(2) . . ? C2 C3 S4 129.5(3) . . ? C2 C3 S2 117.4(3) . . ? S4 C3 S2 113.0(2) . . ? C6 C4 C5 112.4(3) . . ? C6 C4 S3 113.2(3) . . ? C5 C4 S3 112.2(3) . . ? C8 C5 C4 114.2(4) . . ? C8 C5 S4 111.9(3) . . ? C4 C5 S4 112.1(3) . . ? C7 C6 C4 115.0(4) . . ? C9 C8 C5 115.0(4) . . ? C11 S11 C13 95.46(15) . . ? C12 S12 C14 95.46(14) . . ? C13 S13 C15 100.9(2) . . ? C14 S14 C16 100.4(2) . . ? C12 C11 S11 122.59(12) . . ? C12 C11 S11 122.59(12) . 5 ? S11 C11 S11 114.8(2) . 5 ? C11 C12 S12 122.59(11) . 5 ? C11 C12 S12 122.59(11) . . ? S12 C12 S12 114.8(2) 5 . ? C13 C13 S13 128.68(10) 5 . ? C13 C13 S11 117.13(10) 5 . ? S13 C13 S11 114.2(2) . . ? C14 C14 S14 128.72(10) 5 . ? C14 C14 S12 117.13(10) 5 . ? S14 C14 S12 114.2(2) . . ? C17 C15 C15 115.0(4) . 5 ? C17 C15 S13 112.1(3) . . ? C15 C15 S13 111.5(3) 5 . ? C16 C16 C19 114.8(5) 5 . ? C16 C16 S14 111.7(3) 5 . ? C19 C16 S14 112.7(3) . . ? C18 C17 C15 115.1(4) . . ? C20 C19 C16 115.7(4) . . ? _refine_diff_density_max 0.216 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.043 #============================================================================ data_teetaucl _audit_creation_method SHELXL _chemical_name_systematic ; Bis(1,2-diethyl-ethylenedithio)tetrathiafulvalenium tetrachloroaurate(III) dichloroaurate(I) (1:1:1) ; _chemical_formula_moiety '(C18 H32 S8)2+ (Au Cl4)- (AuCl2)-' _chemical_formula_sum 'C18 H32 Au2 Cl6 S8' _chemical_formula_weight 1111.55 _chemical_compound_source 'grown by electrocrystallization' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-x, -y, -z' 'x, y, -z-1/2' '-x, y, -z-1/2' 'x, -y, -z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' '-x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.619(2) _cell_length_b 19.864(2) _cell_length_c 8.4853(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3138.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 2621 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.353 _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 10.394 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3887 _exptl_absorpt_correction_T_max 0.6661 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6.053 cm. Coverage of the unique set is over 98% complete to at least 25.0\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART diffractometer' _diffrn_measurement_method 'area detector \w scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 7582 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1530 _reflns_number_observed 1206 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.04 (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+51.5603P] 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 omitted _refine_ls_extinction_method none _refine_ls_number_reflns 1530 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_obs 0.0590 _refine_ls_wR_factor_all 0.1232 _refine_ls_wR_factor_obs 0.1131 _refine_ls_goodness_of_fit_all 1.155 _refine_ls_goodness_of_fit_obs 1.201 _refine_ls_restrained_S_all 1.155 _refine_ls_restrained_S_obs 1.201 _refine_ls_shift/su_max 0.009 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 0.41351(14) 0.1305(2) 0.4181(4) 0.0596(8) Uani 1 d . . S2 S 0.2576(2) 0.1198(2) 0.4566(5) 0.0838(12) Uani 1 d . . C1 C 0.4614(7) 0.1324(7) 0.2500 0.043(4) Uani 1 d S . C2 C 0.3303(5) 0.1249(5) 0.3288(15) 0.054(3) Uani 1 d . . C3 C 0.1830(13) 0.1069(13) 0.3186(29) 0.067(7) Uiso 0.50 d P . C4 C 0.1863(13) 0.1492(12) 0.1761(29) 0.060(6) Uiso 0.50 d P . C5 C 0.1722(12) 0.0309(10) 0.2869(34) 0.069(7) Uiso 0.50 d P . C6 C 0.0990(14) 0.0161(13) 0.2119(43) 0.094(10) Uiso 0.50 d P . C7 C 0.1952(13) 0.2249(12) 0.1859(28) 0.066(7) Uiso 0.50 d P . C8 C 0.1394(14) 0.2628(13) 0.2500 0.106(8) Uiso 1 d S . Au1 Au 0.5000 0.32163(4) 0.2500 0.0494(3) Uani 1 d S . Cl1 Cl 0.5000 0.3222(5) -0.0137(8) 0.168(4) Uani 1 d S . Cl2 Cl 0.3778(2) 0.3193(3) 0.2500 0.0768(14) Uani 1 d S . Au2 Au 0.5000 -0.04099(5) 0.2500 0.0690(4) Uani 1 d S . Cl3 Cl 0.6214(3) -0.0415(2) 0.2500 0.0805(15) Uani 1 d S . 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 S1 0.0326(13) 0.083(2) 0.064(2) -0.007(2) 0.0010(13) -0.0038(14) S2 0.037(2) 0.139(4) 0.076(3) -0.014(2) 0.010(2) -0.010(2) C1 0.030(7) 0.037(8) 0.062(10) 0.000 0.000 -0.014(6) C2 0.033(5) 0.062(7) 0.067(7) -0.001(6) 0.002(5) -0.003(5) Au1 0.0355(5) 0.0503(6) 0.0626(6) 0.000 0.000 0.000 Cl1 0.055(3) 0.384(14) 0.063(4) -0.001(6) 0.000 0.000 Cl2 0.036(2) 0.110(4) 0.084(3) 0.000 0.000 -0.008(2) Au2 0.0752(7) 0.0515(6) 0.0803(9) 0.000 0.000 0.000 Cl3 0.076(3) 0.068(3) 0.097(4) 0.000 0.000 -0.014(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 S1 C1 1.682(8) . ? S1 C2 1.729(11) . ? S2 C2 1.737(11) . ? S2 C4 1.84(2) 10_556 ? S2 C3 1.83(2) . ? C1 C1 1.44(3) 11_656 ? C2 C2 1.34(2) 10_556 ? C3 C4 1.47(3) . ? C3 C5 1.55(3) . ? C4 C7 1.51(3) . ? C5 C6 1.53(3) . ? C7 C8 1.39(3) . ? Au1 Cl1 2.238(6) . ? Au1 Cl2 2.276(4) . ? Au2 Cl3 2.260(5) 11_656 ? 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 S1 C2 96.0(6) . . ? C2 S2 C4 99.3(9) . 10_556 ? C2 S2 C3 101.5(9) . . ? C1 C1 S1 122.0(4) 11_656 . ? S1 C1 S1 116.0(8) 10_556 . ? C2 C2 S1 116.0(4) 10_556 . ? C2 C2 S2 128.6(4) 10_556 . ? S1 C2 S2 115.4(7) . . ? C4 C3 C5 114.8(20) . . ? C4 C3 S2 114.4(18) . . ? C5 C3 S2 110.2(17) . . ? C7 C4 C3 121.7(20) . . ? C7 C4 S2 105.8(17) . 10_556 ? C3 C4 S2 110.6(17) . 10_556 ? C3 C5 C6 112.0(20) . . ? C8 C7 C4 118.4(21) . . ? Cl1 Au1 Cl1 179.4(6) . 10_556 ? Cl1 Au1 Cl2 90.006(6) . . ? Cl1 Au1 Cl2 90.006(5) . 11_656 ? Cl2 Au1 Cl2 177.7(3) . 11_656 ? Cl3 Au2 Cl3 179.4(2) 11_656 . ? _refine_diff_density_max 0.874 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.157 #============================================================================ data_teetibr2 _audit_creation_method SHELXL _chemical_name_systematic ; Bis(1,2-diethyl-ethylenedithio)tetrathiafulvalenium dibromoiodate (1:2) ; _chemical_formula_moiety '(C18 H24 S8)2+ 2(I Br2)-' _chemical_formula_sum 'C18 H24 Br4 I2 S8' _chemical_formula_weight 1070.29 _chemical_compound_source 'grown by electrocrystallization' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.190(3) _cell_length_b 18.925(4) _cell_length_c 6.5035(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.19(3) _cell_angle_gamma 90.00 _cell_volume 1606.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3180 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.212 _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 7.460 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.281 _exptl_absorpt_correction_T_max 0.641 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6.053 cm. Coverage of the unique set is over 98% complete to at least 25.0\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART diffractometer' _diffrn_measurement_method 'area detector \w scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 5572 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1943 _reflns_number_observed 1640 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.04 (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+13.2497P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1943 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_obs 0.0504 _refine_ls_wR_factor_all 0.1247 _refine_ls_wR_factor_obs 0.1174 _refine_ls_goodness_of_fit_all 1.128 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.159 _refine_ls_shift/su_max -0.030 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I1 I -0.20347(4) 0.5000 0.83764(9) 0.0401(2) Uani 1 d S . Br1 Br -0.19662(6) 0.35808(3) 0.84508(13) 0.0569(3) Uani 1 d . . S1 S -0.08380(13) 0.41402(7) 0.3348(3) 0.0412(4) Uani 1 d . . S2 S -0.10447(14) 0.26006(7) 0.2994(3) 0.0514(5) Uani 1 d . . C1 C 0.0000 0.4625(4) 0.5000 0.0292(15) Uani 1 d S . C2 C -0.0411(4) 0.3319(3) 0.4228(10) 0.0354(12) Uani 1 d . . C3 C -0.0551(6) 0.1868(3) 0.4698(14) 0.064(2) Uani 1 d . . H3 H -0.0710(6) 0.1435(3) 0.3886(14) 0.077 Uiso 1 calc R . C4 C -0.1108(7) 0.1790(4) 0.6695(18) 0.078(3) Uani 1 d . . H4A H -0.0759(7) 0.2079(4) 0.7810(18) 0.093 Uiso 1 calc R . H4B H -0.1808(7) 0.1958(4) 0.6379(18) 0.093 Uiso 1 calc R . C5 C -0.1111(9) 0.1040(6) 0.7385(18) 0.090(3) Uani 1 d . . H5A H -0.1694(38) 0.0958(13) 0.8086(122) 0.135 Uiso 1 calc R . H5B H -0.0494(33) 0.0943(13) 0.8317(104) 0.135 Uiso 1 calc R . H5C H -0.1147(66) 0.0734(6) 0.6198(21) 0.135 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0485(4) 0.0339(3) 0.0370(3) 0.000 0.0031(2) 0.000 Br1 0.0770(5) 0.0313(3) 0.0600(5) -0.0086(3) 0.0014(4) -0.0051(3) S1 0.0494(8) 0.0194(6) 0.0480(9) 0.0002(5) -0.0161(7) 0.0004(5) S2 0.0603(10) 0.0217(6) 0.0624(11) -0.0012(6) -0.0245(8) -0.0036(6) C1 0.034(4) 0.023(3) 0.030(4) 0.000 0.003(3) 0.000 C2 0.039(3) 0.023(2) 0.041(3) -0.001(2) -0.006(2) 0.000(2) C3 0.084(5) 0.026(3) 0.071(5) -0.003(3) -0.024(4) 0.000(3) C4 0.081(6) 0.053(4) 0.109(8) -0.003(5) 0.046(6) -0.002(4) C5 0.097(7) 0.089(7) 0.092(8) 0.031(6) 0.043(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 I1 Br1 2.6876(8) . ? I1 Br1 2.6876(8) 6_565 ? S1 C1 1.697(4) . ? S1 C2 1.722(5) . ? S2 C2 1.733(5) . ? S2 C3 1.836(7) . ? C1 C1 1.420(13) 5_566 ? C1 S1 1.697(4) 2_556 ? C2 C2 1.368(11) 2_556 ? C3 C3 1.45(2) 2_556 ? C3 C4 1.587(13) . ? C4 C5 1.489(12) . ? 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 I1 Br1 175.90(4) . 6_565 ? C1 S1 C2 97.1(3) . . ? C2 S2 C3 102.0(3) . . ? C1 C1 S1 122.7(2) 5_566 . ? C1 C1 S1 122.7(2) 5_566 2_556 ? S1 C1 S1 114.6(4) . 2_556 ? C2 C2 S1 115.6(2) 2_556 . ? C2 C2 S2 128.3(2) 2_556 . ? S1 C2 S2 116.1(3) . . ? C3 C3 C4 109.9(9) 2_556 . ? C3 C3 S2 114.8(6) 2_556 . ? C4 C3 S2 113.5(6) . . ? C5 C4 C3 110.9(7) . . ? _refine_diff_density_max 1.216 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.202 #============================================================================ data_teeti3 _audit_creation_method SHELXL _chemical_name_systematic ; Bis(1,2-diethyl-ethylenedithio)tetrathiafulvalenium triiodide solvate with 1,1,2-trichloroethane (1:1:ca.1) ; _chemical_formula_moiety '(C18 H24 S8)+ (I3)- (C2 H3 Cl3)' _chemical_formula_sum 'C20 H27 Cl3 I3 S8' _chemical_formula_weight 1010.99 _chemical_compound_source 'diffusion-controlled chemical oxidation' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 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 39.754(2) _cell_length_b 13.8902(7) _cell_length_c 11.4853(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.7220(10) _cell_angle_gamma 90.00 _cell_volume 6335.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'slanted octagonal prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 2.120 _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 3.707 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.55938 _exptl_absorpt_correction_T_max 0.75979 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6.053 cm. Coverage of the unique set is over 98% complete to at least 28.29\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. The composition dependent parameters, chemical_formula_weight, exptl_crystal_density_diffrn, exptl_crystal_F_000, exptl_absorpt_coefficient_mu, are based on the idealized composition with one TCE solvent molecule per formula unit. The corresponding values for the effectively refined model, containing a solvent model of incomplete composition (C 1 CL 1.08) are: chemical_formula_weight=927.88, exptl_crystal_density_diffrn=1.946, exptl_crystal_F_000=3546, exptl_absorpt_coefficient_mu=3.539. The values based on the idealized composition were used for the absorption correction. (leading _ omitted in this paragraph for seamless CIF processing). ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART diffractometer' _diffrn_measurement_method 'area detector \w scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 23609 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7369 _reflns_number_observed 5087 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.04 (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+74.0512P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7369 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1273 _refine_ls_R_factor_obs 0.0849 _refine_ls_wR_factor_all 0.1761 _refine_ls_wR_factor_obs 0.1591 _refine_ls_goodness_of_fit_all 1.247 _refine_ls_goodness_of_fit_obs 1.363 _refine_ls_restrained_S_all 1.247 _refine_ls_restrained_S_obs 1.363 _refine_ls_shift/su_max 1.088 _refine_ls_shift/esd_mean 0.044 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I1 I 0.2500 0.2500 0.0000 0.0619(3) Uani 1 d S . I2 I 0.28337(2) 0.20503(6) 0.22480(7) 0.0837(3) Uani 1 d . . I3 I 0.0000 0.23348(8) 0.2500 0.0747(3) Uani 1 d S . I4 I 0.05645(2) 0.23766(8) 0.09689(9) 0.0990(3) Uani 1 d . . S1 S 0.31127(6) -0.0493(2) 0.4307(2) 0.0532(6) Uani 1 d . . S2 S 0.30101(6) 0.1027(2) 0.5990(2) 0.0564(6) Uani 1 d . . S3 S 0.23382(5) -0.0234(2) 0.3312(2) 0.0496(5) Uani 1 d . . S4 S 0.22436(6) 0.1255(2) 0.5040(2) 0.0506(6) Uani 1 d . . S5 S 0.38188(6) -0.0877(2) 0.5042(2) 0.0540(6) Uani 1 d . . S6 S 0.36964(6) 0.0984(2) 0.7044(2) 0.0619(7) Uani 1 d . . S7 S 0.16421(6) -0.0169(2) 0.2312(2) 0.0574(6) Uani 1 d . . S8 S 0.15416(7) 0.1656(3) 0.4365(2) 0.0753(9) Uani 1 d . . C1 C 0.2840(2) 0.0317(6) 0.4874(7) 0.045(2) Uani 1 d . . C2 C 0.2509(2) 0.0428(6) 0.4461(7) 0.043(2) Uani 1 d . . C3 C 0.3458(2) -0.0194(6) 0.5213(7) 0.041(2) Uani 1 d . . C4 C 0.3411(2) 0.0514(6) 0.5985(7) 0.044(2) Uani 1 d . . C5 C 0.1943(2) 0.0272(6) 0.3325(7) 0.042(2) Uani 1 d . . C6 C 0.1895(2) 0.0953(7) 0.4123(7) 0.049(2) Uani 1 d . . C7 C 0.4027(2) -0.0697(7) 0.6476(9) 0.063(3) Uani 1 d . . H7 H 0.4250(2) -0.0995(7) 0.6454(9) 0.075 Uiso 1 calc R . C8 C 0.4082(2) 0.0343(8) 0.6741(9) 0.066(3) Uani 1 d . . H8 H 0.4221(2) 0.0363(8) 0.7467(9) 0.079 Uiso 1 calc R . C9 C 0.1382(2) 0.0923(7) 0.2152(8) 0.053(2) Uani 1 d . . H9 H 0.1192(2) 0.0745(7) 0.1622(8) 0.064 Uiso 1 calc R . C10 C 0.1228(2) 0.1207(7) 0.3283(8) 0.056(2) Uani 1 d . . H10 H 0.1081(2) 0.1756(7) 0.3089(8) 0.067 Uiso 1 calc R . C11 C 0.3836(3) -0.1214(9) 0.7483(10) 0.081(3) Uiso 1 d . . H11A H 0.3926(3) -0.0984(9) 0.8232(10) 0.097 Uiso 1 calc R . H11B H 0.3599(3) -0.1048(9) 0.7414(10) 0.097 Uiso 1 calc R . C12 C 0.3873(4) -0.2294(11) 0.7433(14) 0.112(5) Uiso 1 d . . H12A H 0.3755(4) -0.2582(11) 0.8054(14) 0.169 Uiso 1 calc R . H12B H 0.4107(4) -0.2462(11) 0.7515(14) 0.169 Uiso 1 calc R . H12C H 0.3781(4) -0.2526(11) 0.6698(14) 0.169 Uiso 1 calc R . C13 C 0.4282(3) 0.0892(9) 0.5831(11) 0.082(3) Uiso 1 d . . H13A H 0.4147(3) 0.0920(9) 0.5106(11) 0.098 Uiso 1 calc R . H13B H 0.4317(3) 0.1548(9) 0.6100(11) 0.098 Uiso 1 calc R . C14 C 0.4620(4) 0.0459(13) 0.5590(15) 0.137(6) Uiso 1 d . . H14A H 0.4727(4) 0.0841(13) 0.5018(15) 0.206 Uiso 1 calc R . H14B H 0.4588(4) -0.0185(13) 0.5301(15) 0.206 Uiso 1 calc R . H14C H 0.4759(4) 0.0445(13) 0.6297(15) 0.206 Uiso 1 calc R . C15 C 0.1561(2) 0.1737(7) 0.1546(8) 0.053(2) Uiso 1 d . . H15A H 0.1432(2) 0.2326(7) 0.1620(8) 0.064 Uiso 1 calc R . H15B H 0.1780(2) 0.1837(7) 0.1934(8) 0.064 Uiso 1 calc R . C16 C 0.1606(3) 0.1543(9) 0.0273(10) 0.083(3) Uiso 1 d . . H16A H 0.1720(3) 0.2077(9) -0.0064(10) 0.125 Uiso 1 calc R . H16B H 0.1390(3) 0.1458(9) -0.0120(10) 0.125 Uiso 1 calc R . H16C H 0.1738(3) 0.0969(9) 0.0193(10) 0.125 Uiso 1 calc R . C17 C 0.0998(3) 0.0431(10) 0.3744(11) 0.092(4) Uiso 1 d . . H17A H 0.0851(3) 0.0202(10) 0.3106(11) 0.111 Uiso 1 calc R . H17B H 0.1136(3) -0.0108(10) 0.4015(11) 0.111 Uiso 1 calc R . C18 C 0.0787(4) 0.0749(13) 0.4710(15) 0.138(6) Uiso 1 d . . H18A H 0.0651(4) 0.0222(13) 0.4950(15) 0.207 Uiso 1 calc R . H18B H 0.0645(4) 0.1271(13) 0.4447(15) 0.207 Uiso 1 calc R . H18C H 0.0931(4) 0.0959(13) 0.5357(15) 0.207 Uiso 1 calc R . Cl1 Cl 0.0000 0.3272(12) 0.7500 0.186(9) Uani 0.50 d SP . Cl2 Cl 0.0086(8) 0.0388(15) 0.6881(32) 0.206(16) Uani 0.25 d P . Cl3 Cl 0.0218(10) 0.1185(48) 0.6576(43) 0.179(21) Uani 0.13 d P . Cl4 Cl 0.0250(7) 0.2352(59) 0.6483(38) 0.315(39) Uani 0.20 d P . C21 C -0.0052(17) 0.2046(48) 0.6802(54) 0.185(24) Uiso 0.50 d P . C22 C -0.0093(32) 0.1423(75) 0.7981(94) 0.306(57) Uiso 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0734(6) 0.0483(5) 0.0643(6) -0.0078(4) 0.0068(5) 0.0019(5) I2 0.1144(7) 0.0746(5) 0.0621(4) 0.0101(4) 0.0050(4) 0.0014(5) I3 0.0517(5) 0.0704(7) 0.0999(8) 0.000 -0.0169(5) 0.000 I4 0.0608(5) 0.1280(8) 0.1073(7) 0.0303(6) -0.0046(4) -0.0068(5) S1 0.0408(11) 0.064(2) 0.0536(13) -0.0154(11) -0.0094(10) 0.0070(11) S2 0.0441(12) 0.069(2) 0.0547(13) -0.0166(12) -0.0080(10) 0.0109(11) S3 0.0400(11) 0.0517(13) 0.0563(13) -0.0094(11) -0.0080(9) 0.0065(10) S4 0.0433(12) 0.0643(15) 0.0434(11) -0.0102(10) -0.0047(9) 0.0062(11) S5 0.0459(12) 0.065(2) 0.0502(12) -0.0131(11) -0.0089(10) 0.0141(11) S6 0.0490(13) 0.073(2) 0.0623(14) -0.0238(13) -0.0163(11) 0.0117(12) S7 0.0483(13) 0.0552(14) 0.0668(15) -0.0103(12) -0.0168(11) 0.0045(11) S8 0.0511(14) 0.109(2) 0.065(2) -0.028(2) -0.0100(12) 0.0302(15) C1 0.042(5) 0.050(5) 0.044(4) 0.001(4) -0.004(4) 0.006(4) C2 0.044(5) 0.047(5) 0.040(4) -0.002(4) 0.003(4) 0.003(4) C3 0.034(4) 0.050(5) 0.039(4) 0.000(4) -0.006(3) 0.008(4) C4 0.035(4) 0.052(5) 0.044(4) -0.001(4) -0.007(3) 0.009(4) C5 0.038(4) 0.050(5) 0.039(4) -0.005(4) -0.002(3) -0.002(4) C6 0.041(5) 0.061(6) 0.044(5) 0.004(4) -0.003(4) 0.004(4) C7 0.049(5) 0.064(6) 0.072(6) -0.010(5) -0.024(5) 0.020(5) C8 0.051(6) 0.081(8) 0.063(6) -0.011(5) -0.027(5) 0.011(5) C9 0.042(5) 0.058(6) 0.058(5) -0.002(4) -0.010(4) 0.013(4) C10 0.042(5) 0.060(6) 0.065(6) 0.004(5) -0.003(4) 0.004(4) Cl1 0.211(20) 0.125(12) 0.212(18) 0.000 -0.110(17) 0.000 Cl2 0.170(28) 0.082(12) 0.366(54) -0.011(18) 0.011(25) 0.003(15) Cl3 0.099(24) 0.279(56) 0.164(34) -0.113(38) 0.070(23) -0.001(28) Cl4 0.076(18) 0.645(117) 0.217(38) 0.180(55) -0.052(20) -0.088(36) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 I2 2.9139(8) . ? I1 I2 2.9139(8) 7 ? I3 I4 2.9165(9) 2 ? I3 I4 2.9165(9) . ? S1 C1 1.712(9) . ? S1 C3 1.732(8) . ? S2 C1 1.730(9) . ? S2 C4 1.747(8) . ? S3 C2 1.721(8) . ? S3 C5 1.723(8) . ? S4 C2 1.714(8) . ? S4 C6 1.753(8) . ? S5 C3 1.739(8) . ? S5 C7 1.825(9) . ? S6 C4 1.749(8) . ? S6 C8 1.819(10) . ? S7 C5 1.738(8) . ? S7 C9 1.840(9) . ? S8 C6 1.743(9) . ? S8 C10 1.829(9) . ? C1 C2 1.386(11) . ? C3 C4 1.343(11) . ? C5 C6 1.337(12) . ? C7 C8 1.491(14) . ? C7 C11 1.58(2) . ? C8 C13 1.55(2) . ? C9 C10 1.514(13) . ? C9 C15 1.522(13) . ? C10 C17 1.52(2) . ? C11 C12 1.51(2) . ? C13 C14 1.51(2) . ? C15 C16 1.505(14) . ? C17 C18 1.49(2) . ? Cl1 C21 1.89(6) . ? Cl1 C21 1.89(6) 2_556 ? Cl1 Cl4 2.02(8) 2_556 ? Cl1 Cl4 2.02(8) . ? Cl2 Cl3 1.28(6) . ? Cl2 Cl2 1.61(7) 2_556 ? Cl2 C22 1.45(10) 2_556 ? Cl2 C22 2.06(9) . ? Cl2 Cl3 2.46(7) 2_556 ? Cl3 C22 0.80(11) 2_556 ? Cl3 C21 1.64(9) . ? Cl3 Cl4 1.63(8) . ? Cl3 C22 2.11(11) . ? Cl3 Cl2 2.46(7) 2_556 ? Cl4 C21 1.34(7) . ? Cl4 C22 1.57(11) 2_556 ? Cl4 C21 2.20(8) 2_556 ? C21 C22 1.06(12) 2_556 ? C21 C22 1.62(9) . ? C21 C21 1.64(12) 2_556 ? C21 Cl4 2.20(8) 2_556 ? C22 C22 1.36(21) 2_556 ? C22 C21 1.06(12) 2_556 ? C22 Cl3 0.80(11) 2_556 ? C22 Cl2 1.45(10) 2_556 ? C22 Cl4 1.57(11) 2_556 ? 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 I2 I1 I2 180.0 . 7 ? I4 I3 I4 177.72(6) 2 . ? C1 S1 C3 96.5(4) . . ? C1 S2 C4 95.2(4) . . ? C2 S3 C5 95.8(4) . . ? C2 S4 C6 95.1(4) . . ? C3 S5 C7 99.5(4) . . ? C4 S6 C8 102.0(4) . . ? C5 S7 C9 98.1(4) . . ? C6 S8 C10 103.2(4) . . ? C2 C1 S1 123.5(7) . . ? C2 C1 S2 121.4(7) . . ? S1 C1 S2 115.0(5) . . ? C1 C2 S4 122.2(6) . . ? C1 C2 S3 122.3(6) . . ? S4 C2 S3 115.4(5) . . ? C4 C3 S1 116.2(6) . . ? C4 C3 S5 127.9(6) . . ? S1 C3 S5 115.9(5) . . ? C3 C4 S2 117.1(6) . . ? C3 C4 S6 128.8(6) . . ? S2 C4 S6 114.0(5) . . ? C6 C5 S3 117.0(6) . . ? C6 C5 S7 126.3(7) . . ? S3 C5 S7 116.7(5) . . ? C5 C6 S8 130.4(7) . . ? C5 C6 S4 116.6(7) . . ? S8 C6 S4 112.9(5) . . ? C8 C7 C11 111.1(9) . . ? C8 C7 S5 111.9(7) . . ? C11 C7 S5 112.6(7) . . ? C7 C8 C13 114.5(9) . . ? C7 C8 S6 113.4(7) . . ? C13 C8 S6 110.8(8) . . ? C10 C9 C15 114.6(8) . . ? C10 C9 S7 112.2(6) . . ? C15 C9 S7 112.7(6) . . ? C9 C10 C17 112.8(9) . . ? C9 C10 S8 112.4(6) . . ? C17 C10 S8 113.9(8) . . ? C12 C11 C7 111.9(11) . . ? C14 C13 C8 114.8(11) . . ? C16 C15 C9 113.0(8) . . ? C18 C17 C10 114.6(12) . . ? C21 Cl1 C21 51.3(40) . 2_556 ? C21 Cl1 Cl4 68.2(24) . 2_556 ? C21 Cl1 Cl4 40.0(25) 2_556 2_556 ? C21 Cl1 Cl4 40.0(25) . . ? C21 Cl1 Cl4 68.2(24) 2_556 . ? Cl4 Cl1 Cl4 101.7(31) 2_556 . ? Cl3 Cl2 Cl2 116.0(25) . 2_556 ? Cl3 Cl2 C22 33.4(40) . 2_556 ? Cl2 Cl2 C22 84.8(45) 2_556 2_556 ? Cl3 Cl2 C22 73.9(39) . . ? Cl2 Cl2 C22 44.3(30) 2_556 . ? C22 Cl2 C22 41.0(67) 2_556 . ? Cl3 Cl2 Cl3 91.7(27) . 2_556 ? Cl2 Cl2 Cl3 28.0(11) 2_556 2_556 ? C22 Cl2 Cl3 58.7(48) 2_556 2_556 ? C22 Cl2 Cl3 17.8(35) . 2_556 ? C22 Cl3 Cl2 84.8(94) 2_556 . ? C22 Cl3 C21 33.4(98) 2_556 . ? Cl2 Cl3 C21 107.9(37) . . ? C22 Cl3 Cl4 71.6(94) 2_556 . ? Cl2 Cl3 Cl4 155.8(35) . . ? C21 Cl3 Cl4 48.6(27) . . ? C22 Cl3 C22 16.6(80) 2_556 . ? Cl2 Cl3 C22 70.3(42) . . ? C21 Cl3 C22 49.4(32) . . ? Cl4 Cl3 C22 86.9(36) . . ? C22 Cl3 Cl2 52.1(94) 2_556 2_556 ? Cl2 Cl3 Cl2 36.0(23) . 2_556 ? C21 Cl3 Cl2 82.3(30) . 2_556 ? Cl4 Cl3 Cl2 122.6(26) . 2_556 ? C22 Cl3 Cl2 36.0(33) . 2_556 ? C21 Cl4 Cl3 66.0(45) . . ? C21 Cl4 C22 41.9(47) . 2_556 ? Cl3 Cl4 C22 28.8(44) . 2_556 ? C21 Cl4 Cl1 64.6(41) . . ? Cl3 Cl4 Cl1 123.2(24) . . ? C22 Cl4 Cl1 94.4(51) 2_556 . ? C21 Cl4 C21 47.9(42) . 2_556 ? Cl3 Cl4 C21 73.5(27) . 2_556 ? C22 Cl4 C21 47.4(42) 2_556 2_556 ? Cl1 Cl4 C21 53.0(24) . 2_556 ? C22 C21 Cl4 80.7(80) 2_556 . ? C22 C21 C22 56.3(96) 2_556 . ? Cl4 C21 C22 121.6(71) . . ? C22 C21 Cl3 24.4(69) 2_556 . ? Cl4 C21 Cl3 65.5(45) . . ? C22 C21 Cl3 80.5(53) . . ? C22 C21 C21 70.2(79) 2_556 2_556 ? Cl4 C21 C21 94.5(56) . 2_556 ? C22 C21 C21 38.1(44) . 2_556 ? Cl3 C21 C21 91.0(43) . 2_556 ? C22 C21 Cl1 125.9(92) 2_556 . ? Cl4 C21 Cl1 75.5(50) . . ? C22 C21 Cl1 98.1(46) . . ? Cl3 C21 Cl1 131.8(40) . . ? C21 C21 Cl1 64.3(20) 2_556 . ? C22 C21 Cl4 99.3(91) 2_556 2_556 ? Cl4 C21 Cl4 123.2(53) . 2_556 ? C22 C21 Cl4 45.6(41) . 2_556 ? Cl3 C21 Cl4 123.4(51) . 2_556 ? C21 C21 Cl4 37.5(34) 2_556 2_556 ? Cl1 C21 Cl4 58.8(28) . 2_556 ? C22 C22 C21 83.1(99) 2_556 2_556 ? C22 C22 Cl3 153.8(100) 2_556 2_556 ? C21 C22 Cl3 122.2(100) 2_556 2_556 ? C22 C22 C21 40.6(50) 2_556 . ? C21 C22 C21 71.7(91) 2_556 . ? Cl3 C22 C21 147.5(100) 2_556 . ? C22 C22 Cl2 94.6(46) 2_556 2_556 ? C21 C22 Cl2 140.8(100) 2_556 2_556 ? Cl3 C22 Cl2 61.9(93) 2_556 2_556 ? C21 C22 Cl2 128.3(68) . 2_556 ? C22 C22 Cl4 124.1(55) 2_556 2_556 ? C21 C22 Cl4 57.5(63) 2_556 2_556 ? Cl3 C22 Cl4 79.6(99) 2_556 2_556 ? C21 C22 Cl4 87.0(67) . 2_556 ? Cl2 C22 Cl4 141.2(93) 2_556 2_556 ? C22 C22 Cl3 9.7(49) 2_556 . ? C21 C22 Cl3 88.6(91) 2_556 . ? Cl3 C22 Cl3 145.9(100) 2_556 . ? C21 C22 Cl3 50.0(38) . . ? Cl2 C22 Cl3 85.3(58) 2_556 . ? Cl4 C22 Cl3 133.5(84) 2_556 . ? C22 C22 Cl2 44.4(31) 2_556 . ? C21 C22 Cl2 120.8(100) 2_556 . ? Cl3 C22 Cl2 110.1(100) 2_556 . ? C21 C22 Cl2 79.0(40) . . ? Cl2 C22 Cl2 50.8(39) 2_556 . ? Cl4 C22 Cl2 165.3(77) 2_556 . ? Cl3 C22 Cl2 35.8(25) . . ? 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 C1 C2 178.8(8) . . . . ? C3 S1 C1 S2 0.6(6) . . . . ? C4 S2 C1 C2 -178.4(8) . . . . ? C4 S2 C1 S1 -0.3(6) . . . . ? S1 C1 C2 S4 -179.3(5) . . . . ? S2 C1 C2 S4 -1.3(11) . . . . ? S1 C1 C2 S3 -0.8(11) . . . . ? S2 C1 C2 S3 177.2(5) . . . . ? C6 S4 C2 C1 -179.1(8) . . . . ? C6 S4 C2 S3 2.3(6) . . . . ? C5 S3 C2 C1 179.5(8) . . . . ? C5 S3 C2 S4 -1.9(6) . . . . ? C1 S1 C3 C4 -0.9(8) . . . . ? C1 S1 C3 S5 177.1(5) . . . . ? C7 S5 C3 C4 21.0(9) . . . . ? C7 S5 C3 S1 -156.7(5) . . . . ? S1 C3 C4 S2 0.9(10) . . . . ? S5 C3 C4 S2 -176.8(5) . . . . ? S1 C3 C4 S6 178.5(5) . . . . ? S5 C3 C4 S6 0.8(13) . . . . ? C1 S2 C4 C3 -0.4(8) . . . . ? C1 S2 C4 S6 -178.4(5) . . . . ? C8 S6 C4 C3 5.0(10) . . . . ? C8 S6 C4 S2 -177.3(5) . . . . ? C2 S3 C5 C6 0.6(8) . . . . ? C2 S3 C5 S7 -178.3(5) . . . . ? C9 S7 C5 C6 29.2(9) . . . . ? C9 S7 C5 S3 -152.0(5) . . . . ? S3 C5 C6 S8 177.0(6) . . . . ? S7 C5 C6 S8 -4.2(14) . . . . ? S3 C5 C6 S4 0.9(10) . . . . ? S7 C5 C6 S4 179.7(5) . . . . ? C10 S8 C6 C5 2.5(10) . . . . ? C10 S8 C6 S4 178.7(5) . . . . ? C2 S4 C6 C5 -2.0(8) . . . . ? C2 S4 C6 S8 -178.7(5) . . . . ? C3 S5 C7 C8 -56.9(8) . . . . ? C3 S5 C7 C11 69.1(8) . . . . ? C11 C7 C8 C13 177.1(9) . . . . ? S5 C7 C8 C13 -56.1(10) . . . . ? C11 C7 C8 S6 -54.5(9) . . . . ? S5 C7 C8 S6 72.3(9) . . . . ? C4 S6 C8 C7 -41.7(8) . . . . ? C4 S6 C8 C13 88.6(8) . . . . ? C5 S7 C9 C10 -62.3(7) . . . . ? C5 S7 C9 C15 68.7(7) . . . . ? C15 C9 C10 C17 169.5(9) . . . . ? S7 C9 C10 C17 -60.5(10) . . . . ? C15 C9 C10 S8 -60.1(9) . . . . ? S7 C9 C10 S8 70.0(8) . . . . ? C6 S8 C10 C9 -35.6(8) . . . . ? C6 S8 C10 C17 94.3(8) . . . . ? C8 C7 C11 C12 -162.1(10) . . . . ? S5 C7 C11 C12 71.5(12) . . . . ? C7 C8 C13 C14 -54.8(14) . . . . ? S6 C8 C13 C14 175.5(10) . . . . ? C10 C9 C15 C16 -160.4(8) . . . . ? S7 C9 C15 C16 69.7(10) . . . . ? C9 C10 C17 C18 -168.1(11) . . . . ? S8 C10 C17 C18 62.3(14) . . . . ? Cl2 Cl2 Cl3 C22 -22.5(120) 2_556 . . 2_556 ? C22 Cl2 Cl3 C22 0.00(2) 2_556 . . 2_556 ? C22 Cl2 Cl3 C22 -8.3(142) . . . 2_556 ? Cl3 Cl2 Cl3 C22 -8.2(105) 2_556 . . 2_556 ? Cl2 Cl2 Cl3 C21 -46.8(57) 2_556 . . . ? C22 Cl2 Cl3 C21 -24.3(106) 2_556 . . . ? C22 Cl2 Cl3 C21 -32.7(47) . . . . ? Cl3 Cl2 Cl3 C21 -32.5(31) 2_556 . . . ? Cl2 Cl2 Cl3 Cl4 -34.5(135) 2_556 . . . ? C22 Cl2 Cl3 Cl4 -12.0(109) 2_556 . . . ? C22 Cl2 Cl3 Cl4 -20.3(121) . . . . ? Cl3 Cl2 Cl3 Cl4 -20.1(106) 2_556 . . . ? Cl2 Cl2 Cl3 C22 -14.2(50) 2_556 . . . ? C22 Cl2 Cl3 C22 8.3(142) 2_556 . . . ? C22 Cl2 Cl3 C22 0.000(11) . . . . ? Cl3 Cl2 Cl3 C22 0.2(40) 2_556 . . . ? Cl2 Cl2 Cl3 Cl2 0.000(5) 2_556 . . 2_556 ? C22 Cl2 Cl3 Cl2 22.5(120) 2_556 . . 2_556 ? C22 Cl2 Cl3 Cl2 14.2(50) . . . 2_556 ? Cl3 Cl2 Cl3 Cl2 14.4(33) 2_556 . . 2_556 ? C22 Cl3 Cl4 C21 -28.3(120) 2_556 . . . ? Cl2 Cl3 Cl4 C21 -15.8(115) . . . . ? C21 Cl3 Cl4 C21 0.000(7) . . . . ? C22 Cl3 Cl4 C21 -34.9(41) . . . . ? Cl2 Cl3 Cl4 C21 -39.0(41) 2_556 . . . ? C22 Cl3 Cl4 C22 0.00(3) 2_556 . . 2_556 ? Cl2 Cl3 Cl4 C22 12.6(116) . . . 2_556 ? C21 Cl3 Cl4 C22 28.3(121) . . . 2_556 ? C22 Cl3 Cl4 C22 -6.5(142) . . . 2_556 ? Cl2 Cl3 Cl4 C22 -10.7(101) 2_556 . . 2_556 ? C22 Cl3 Cl4 Cl1 3.1(122) 2_556 . . . ? Cl2 Cl3 Cl4 Cl1 15.7(128) . . . . ? C21 Cl3 Cl4 Cl1 31.4(34) . . . . ? C22 Cl3 Cl4 Cl1 -3.4(40) . . . . ? Cl2 Cl3 Cl4 Cl1 -7.6(45) 2_556 . . . ? C22 Cl3 Cl4 C21 22.4(111) 2_556 . . 2_556 ? Cl2 Cl3 Cl4 C21 35.0(110) . . . 2_556 ? C21 Cl3 Cl4 C21 50.7(43) . . . 2_556 ? C22 Cl3 Cl4 C21 15.9(40) . . . 2_556 ? Cl2 Cl3 Cl4 C21 11.7(31) 2_556 . . 2_556 ? C21 Cl1 Cl4 C21 0.000(2) . . . . ? C21 Cl1 Cl4 C21 55.2(54) 2_556 . . . ? Cl4 Cl1 Cl4 C21 33.0(34) 2_556 . . . ? C21 Cl1 Cl4 Cl3 -31.8(42) . . . . ? C21 Cl1 Cl4 Cl3 23.4(34) 2_556 . . . ? Cl4 Cl1 Cl4 Cl3 1.2(25) 2_556 . . . ? C21 Cl1 Cl4 C22 -30.3(58) . . . 2_556 ? C21 Cl1 Cl4 C22 24.9(54) 2_556 . . 2_556 ? Cl4 Cl1 Cl4 C22 2.7(48) 2_556 . . 2_556 ? C21 Cl1 Cl4 C21 -55.2(54) . . . 2_556 ? C21 Cl1 Cl4 C21 0.00(2) 2_556 . . 2_556 ? Cl4 Cl1 Cl4 C21 -22.2(23) 2_556 . . 2_556 ? Cl3 Cl4 C21 C22 20.1(79) . . . 2_556 ? C22 Cl4 C21 C22 0.000(11) 2_556 . . 2_556 ? Cl1 Cl4 C21 C22 -131.0(88) . . . 2_556 ? C21 Cl4 C21 C22 -69.0(79) 2_556 . . 2_556 ? Cl3 Cl4 C21 C22 60.5(64) . . . . ? C22 Cl4 C21 C22 40.4(88) 2_556 . . . ? Cl1 Cl4 C21 C22 -90.6(63) . . . . ? C21 Cl4 C21 C22 -28.6(60) 2_556 . . . ? Cl3 Cl4 C21 Cl3 0.000(6) . . . . ? C22 Cl4 C21 Cl3 -20.1(79) 2_556 . . . ? Cl1 Cl4 C21 Cl3 -151.1(33) . . . . ? C21 Cl4 C21 Cl3 -89.1(31) 2_556 . . . ? Cl3 Cl4 C21 C21 89.1(31) . . . 2_556 ? C22 Cl4 C21 C21 69.0(79) 2_556 . . 2_556 ? Cl1 Cl4 C21 C21 -62.0(18) . . . 2_556 ? C21 Cl4 C21 C21 0.000(7) 2_556 . . 2_556 ? Cl3 Cl4 C21 Cl1 151.1(33) . . . . ? C22 Cl4 C21 Cl1 131.0(88) 2_556 . . . ? Cl1 Cl4 C21 Cl1 0.000(1) . . . . ? C21 Cl4 C21 Cl1 62.0(18) 2_556 . . . ? Cl3 Cl4 C21 Cl4 115.1(79) . . . 2_556 ? C22 Cl4 C21 Cl4 95.0(110) 2_556 . . 2_556 ? Cl1 Cl4 C21 Cl4 -36.0(59) . . . 2_556 ? C21 Cl4 C21 Cl4 26.0(59) 2_556 . . 2_556 ? C22 Cl3 C21 C22 0.00(6) 2_556 . . 2_556 ? Cl2 Cl3 C21 C22 48.3(182) . . . 2_556 ? Cl4 Cl3 C21 C22 -125.0(194) . . . 2_556 ? C22 Cl3 C21 C22 6.3(202) . . . 2_556 ? Cl2 Cl3 C21 C22 22.6(178) 2_556 . . 2_556 ? C22 Cl3 C21 Cl4 125.0(194) 2_556 . . . ? Cl2 Cl3 C21 Cl4 173.3(49) . . . . ? Cl4 Cl3 C21 Cl4 0.000(7) . . . . ? C22 Cl3 C21 Cl4 131.3(55) . . . . ? Cl2 Cl3 C21 Cl4 147.6(35) 2_556 . . . ? C22 Cl3 C21 C22 -6.3(202) 2_556 . . . ? Cl2 Cl3 C21 C22 42.0(65) . . . . ? Cl4 Cl3 C21 C22 -131.3(55) . . . . ? C22 Cl3 C21 C22 0.00(3) . . . . ? Cl2 Cl3 C21 C22 16.4(50) 2_556 . . . ? C22 Cl3 C21 C21 30.5(181) 2_556 . . 2_556 ? Cl2 Cl3 C21 C21 78.8(50) . . . 2_556 ? Cl4 Cl3 C21 C21 -94.5(47) . . . 2_556 ? C22 Cl3 C21 C21 36.8(50) . . . 2_556 ? Cl2 Cl3 C21 C21 53.1(36) 2_556 . . 2_556 ? C22 Cl3 C21 Cl1 86.1(195) 2_556 . . . ? Cl2 Cl3 C21 Cl1 134.4(51) . . . . ? Cl4 Cl3 C21 Cl1 -38.9(53) . . . . ? C22 Cl3 C21 Cl1 92.4(78) . . . . ? Cl2 Cl3 C21 Cl1 108.7(54) 2_556 . . . ? C22 Cl3 C21 Cl4 10.2(177) 2_556 . . 2_556 ? Cl2 Cl3 C21 Cl4 58.4(56) . . . 2_556 ? Cl4 Cl3 C21 Cl4 -114.9(60) . . . 2_556 ? C22 Cl3 C21 Cl4 16.4(63) . . . 2_556 ? Cl2 Cl3 C21 Cl4 32.8(45) 2_556 . . 2_556 ? C21 Cl1 C21 C22 -35.7(86) 2_556 . . 2_556 ? Cl4 Cl1 C21 C22 -78.1(110) 2_556 . . 2_556 ? Cl4 Cl1 C21 C22 66.8(102) . . . 2_556 ? C21 Cl1 C21 Cl4 -102.4(57) 2_556 . . . ? Cl4 Cl1 C21 Cl4 -144.9(39) 2_556 . . . ? Cl4 Cl1 C21 Cl4 0.000(2) . . . . ? C21 Cl1 C21 C22 18.2(52) 2_556 . . . ? Cl4 Cl1 C21 C22 -24.2(47) 2_556 . . . ? Cl4 Cl1 C21 C22 120.7(69) . . . . ? C21 Cl1 C21 Cl3 -66.2(60) 2_556 . . . ? Cl4 Cl1 C21 Cl3 -108.7(64) 2_556 . . . ? Cl4 Cl1 C21 Cl3 36.2(45) . . . . ? C21 Cl1 C21 C21 0.00(2) 2_556 . . 2_556 ? Cl4 Cl1 C21 C21 -42.5(38) 2_556 . . 2_556 ? Cl4 Cl1 C21 C21 102.4(57) . . . 2_556 ? C21 Cl1 C21 Cl4 42.5(38) 2_556 . . 2_556 ? Cl4 Cl1 C21 Cl4 0.000(8) 2_556 . . 2_556 ? Cl4 Cl1 C21 Cl4 144.9(39) . . . 2_556 ? C22 C21 C22 C22 0.00(4) 2_556 . . 2_556 ? Cl4 C21 C22 C22 -50.3(102) . . . 2_556 ? Cl3 C21 C22 C22 3.1(100) . . . 2_556 ? C21 C21 C22 C22 -100.9(167) 2_556 . . 2_556 ? Cl1 C21 C22 C22 -128.1(108) . . . 2_556 ? Cl4 C21 C22 C22 -157.6(151) 2_556 . . 2_556 ? C22 C21 C22 C21 100.9(167) 2_556 . . 2_556 ? Cl4 C21 C22 C21 50.7(116) . . . 2_556 ? Cl3 C21 C22 C21 104.0(89) . . . 2_556 ? C21 C21 C22 C21 0.00(2) 2_556 . . 2_556 ? Cl1 C21 C22 C21 -27.2(69) . . . 2_556 ? Cl4 C21 C22 C21 -56.7(62) 2_556 . . 2_556 ? C22 C21 C22 Cl3 -137.2(274) 2_556 . . 2_556 ? Cl4 C21 C22 Cl3 172.5(244) . . . 2_556 ? Cl3 C21 C22 Cl3 -134.1(249) . . . 2_556 ? C21 C21 C22 Cl3 121.8(274) 2_556 . . 2_556 ? Cl1 C21 C22 Cl3 94.6(251) . . . 2_556 ? Cl4 C21 C22 Cl3 65.2(227) 2_556 . . 2_556 ? C22 C21 C22 Cl2 -40.2(65) 2_556 . . 2_556 ? Cl4 C21 C22 Cl2 -90.5(106) . . . 2_556 ? Cl3 C21 C22 Cl2 -37.1(104) . . . 2_556 ? C21 C21 C22 Cl2 -141.1(161) 2_556 . . 2_556 ? Cl1 C21 C22 Cl2 -168.3(100) . . . 2_556 ? Cl4 C21 C22 Cl2 162.2(155) 2_556 . . 2_556 ? C22 C21 C22 Cl4 157.6(151) 2_556 . . 2_556 ? Cl4 C21 C22 Cl4 107.3(99) . . . 2_556 ? Cl3 C21 C22 Cl4 160.7(65) . . . 2_556 ? C21 C21 C22 Cl4 56.7(62) 2_556 . . 2_556 ? Cl1 C21 C22 Cl4 29.5(62) . . . 2_556 ? Cl4 C21 C22 Cl4 0.00(3) 2_556 . . 2_556 ? C22 C21 C22 Cl3 -3.1(100) 2_556 . . . ? Cl4 C21 C22 Cl3 -53.4(62) . . . . ? Cl3 C21 C22 Cl3 0.00(2) . . . . ? C21 C21 C22 Cl3 -104.0(89) 2_556 . . . ? Cl1 C21 C22 Cl3 -131.2(40) . . . . ? Cl4 C21 C22 Cl3 -160.7(65) 2_556 . . . ? C22 C21 C22 Cl2 -26.9(85) 2_556 . . . ? Cl4 C21 C22 Cl2 -77.1(66) . . . . ? Cl3 C21 C22 Cl2 -23.8(29) . . . . ? C21 C21 C22 Cl2 -127.8(96) 2_556 . . . ? Cl1 C21 C22 Cl2 -155.0(36) . . . . ? Cl4 C21 C22 Cl2 175.5(79) 2_556 . . . ? C22 Cl3 C22 C22 0.00(14) 2_556 . . 2_556 ? Cl2 Cl3 C22 C22 -149.6(471) . . . 2_556 ? C21 Cl3 C22 C22 -12.2(433) . . . 2_556 ? Cl4 Cl3 C22 C22 22.2(444) . . . 2_556 ? Cl2 Cl3 C22 C22 -163.8(503) 2_556 . . 2_556 ? C22 Cl3 C22 C21 -55.0(386) 2_556 . . 2_556 ? Cl2 Cl3 C22 C21 155.4(99) . . . 2_556 ? C21 Cl3 C22 C21 -67.2(90) . . . 2_556 ? Cl4 Cl3 C22 C21 -32.8(79) . . . 2_556 ? Cl2 Cl3 C22 C21 141.2(127) 2_556 . . 2_556 ? C22 Cl3 C22 Cl3 148.7(685) 2_556 . . 2_556 ? Cl2 Cl3 C22 Cl3 -1.0(216) . . . 2_556 ? C21 Cl3 C22 Cl3 136.5(256) . . . 2_556 ? Cl4 Cl3 C22 Cl3 170.8(243) . . . 2_556 ? Cl2 Cl3 C22 Cl3 -15.2(184) 2_556 . . 2_556 ? C22 Cl3 C22 C21 12.2(434) 2_556 . . . ? Cl2 Cl3 C22 C21 -137.5(59) . . . . ? C21 Cl3 C22 C21 0.00(3) . . . . ? Cl4 Cl3 C22 C21 34.4(37) . . . . ? Cl2 Cl3 C22 C21 -151.6(83) 2_556 . . . ? C22 Cl3 C22 Cl2 163.8(503) 2_556 . . 2_556 ? Cl2 Cl3 C22 Cl2 14.2(51) . . . 2_556 ? C21 Cl3 C22 Cl2 151.6(83) . . . 2_556 ? Cl4 Cl3 C22 Cl2 -174.0(64) . . . 2_556 ? Cl2 Cl3 C22 Cl2 0.00(2) 2_556 . . 2_556 ? C22 Cl3 C22 Cl4 -14.9(362) 2_556 . . 2_556 ? Cl2 Cl3 C22 Cl4 -164.5(117) . . . 2_556 ? C21 Cl3 C22 Cl4 -27.1(84) . . . 2_556 ? Cl4 Cl3 C22 Cl4 7.3(97) . . . 2_556 ? Cl2 Cl3 C22 Cl4 -178.7(151) 2_556 . . 2_556 ? C22 Cl3 C22 Cl2 149.6(471) 2_556 . . . ? Cl2 Cl3 C22 Cl2 0.000(15) . . . . ? C21 Cl3 C22 Cl2 137.5(59) . . . . ? Cl4 Cl3 C22 Cl2 171.8(48) . . . . ? Cl2 Cl3 C22 Cl2 -14.2(51) 2_556 . . . ? Cl3 Cl2 C22 C22 7.0(121) . . . 2_556 ? Cl2 Cl2 C22 C22 168.6(168) 2_556 . . 2_556 ? C22 Cl2 C22 C22 0.00(3) 2_556 . . 2_556 ? Cl3 Cl2 C22 C22 -172.5(247) 2_556 . . 2_556 ? Cl3 Cl2 C22 C21 -29.0(115) . . . 2_556 ? Cl2 Cl2 C22 C21 132.7(147) 2_556 . . 2_556 ? C22 Cl2 C22 C21 -36.0(86) 2_556 . . 2_556 ? Cl3 Cl2 C22 C21 151.6(231) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl3 179.4(129) . . . 2_556 ? Cl2 Cl2 C22 Cl3 -18.9(95) 2_556 . . 2_556 ? C22 Cl2 C22 Cl3 172.5(247) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl3 0.00(3) 2_556 . . 2_556 ? Cl3 Cl2 C22 C21 31.9(51) . . . . ? Cl2 Cl2 C22 C21 -166.5(87) 2_556 . . . ? C22 Cl2 C22 C21 24.9(90) 2_556 . . . ? Cl3 Cl2 C22 C21 -147.6(163) 2_556 . . . ? Cl3 Cl2 C22 Cl2 -161.6(66) . . . 2_556 ? Cl2 Cl2 C22 Cl2 0.00(2) 2_556 . . 2_556 ? C22 Cl2 C22 Cl2 -168.6(168) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl2 18.9(96) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl4 49.7(349) . . . 2_556 ? Cl2 Cl2 C22 Cl4 -148.7(385) 2_556 . . 2_556 ? C22 Cl2 C22 Cl4 42.7(261) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl4 -129.8(446) 2_556 . . 2_556 ? Cl3 Cl2 C22 Cl3 0.00(2) . . . . ? Cl2 Cl2 C22 Cl3 161.6(66) 2_556 . . . ? C22 Cl2 C22 Cl3 -7.0(121) 2_556 . . . ? Cl3 Cl2 C22 Cl3 -179.4(129) 2_556 . . . ? _refine_diff_density_max 0.843 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.132 #============================================================================ data_deetibr2 _audit_creation_method SHELXL _chemical_name_systematic ; (1,2-diethyl-ethylenedithio)tetrathiafulvalenium dibromoiodate (2:3) ; _chemical_formula_moiety '2(C14 H16 S8)1.5+ 3(I Br2)-' _chemical_formula_sum 'C28 H32 Br6 I3 S16' _chemical_formula_weight 1741.66 _chemical_compound_source 'crystal grown by electrocrystallization' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 35.639(2) _cell_length_b 9.4278(4) _cell_length_c 14.7617(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.4560(10) _cell_angle_gamma 90.00 _cell_volume 4944.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.15 _cell_measurement_theta_max 28.30 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.339 _exptl_crystal_F_000 3300 _exptl_absorpt_coefficient_mu 7.446 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.051 _exptl_absorpt_correction_T_max 0.341 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6.053 cm. Coverage of the unique set is over 98% complete to at least 28.29\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. No statistically significant decay was found. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART diffractometer' _diffrn_measurement_method 'area detector \w scans' _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 27146 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.1089 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11276 _reflns_number_observed 5596 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens/Bruker 1994)' _computing_cell_refinement 'SAINT (Siemens/Bruker 1994)' _computing_data_reduction 'SAINT (Siemens/Bruker 1994)' _computing_structure_solution 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_molecular_graphics 'SHELXTL 5.04 (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.04 (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. This structure exhibits a distinct pseudotranslation 0.5a + 0.5c (intensity ratio ca. 10:1). However, the reflections with h+l=2n+1 are clearly present by inspection of the raw data. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+40.5127P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11275 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1597 _refine_ls_R_factor_obs 0.0761 _refine_ls_wR_factor_all 0.1978 _refine_ls_wR_factor_obs 0.1646 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.352 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.352 _refine_ls_shift/su_max -0.115 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I1 I 0.47985(2) 0.69143(8) 0.08470(5) 0.0400(2) Uani 1 d . . Br1 Br 0.55596(4) 0.6900(2) 0.11430(11) 0.0591(4) Uani 1 d . . Br2 Br 0.40499(4) 0.6957(2) 0.06048(10) 0.0551(4) Uani 1 d . . I2 I -0.01800(2) 0.67891(8) 0.58149(5) 0.0409(2) Uani 1 d . . Br3 Br 0.05755(4) 0.6768(2) 0.61626(11) 0.0606(4) Uani 1 d . . Br4 Br -0.09282(4) 0.6861(2) 0.54963(10) 0.0606(4) Uani 1 d . . I3A I 0.26221(3) 0.59417(11) 0.17752(8) 0.0651(3) Uani 0.902(2) d P 1 Br5A Br 0.23836(5) 0.4406(2) 0.32036(13) 0.0883(6) Uani 0.902(2) d P 1 Br6A Br 0.28695(5) 0.7366(2) 0.0332(2) 0.0863(7) Uani 0.902(2) d P 1 I3B I 0.23836(5) 0.4406(2) 0.32036(13) 0.0883(6) Uani 0.098(2) d P 2 Br5B Br 0.2120(5) 0.2641(22) 0.4723(14) 0.0863(7) Uani 0.098(2) d P 2 Br6B Br 0.26221(3) 0.59417(11) 0.17752(8) 0.0651(3) Uani 0.098(2) d P 2 S1 S 0.02464(8) 0.0417(3) 0.6357(2) 0.0407(8) Uani 1 d . . S2 S 0.02453(8) 0.3395(3) 0.6818(2) 0.0372(7) Uani 1 d . . S3 S -0.06573(8) 0.0470(3) 0.5998(2) 0.0434(8) Uani 1 d . . S4 S -0.06663(8) 0.3437(3) 0.6486(2) 0.0443(8) Uani 1 d . . S5 S 0.10628(9) 0.0050(4) 0.6556(3) 0.0532(10) Uani 1 d . . S6 S 0.10600(9) 0.3668(4) 0.7162(2) 0.0496(9) Uani 1 d . . S7 S -0.14803(9) 0.0145(4) 0.5740(3) 0.0591(11) Uani 1 d . . S8 S -0.14942(9) 0.3707(4) 0.6341(3) 0.0580(10) Uani 1 d . . C1 C -0.0008(3) 0.1933(10) 0.6493(7) 0.027(2) Uani 1 d . . C2 C -0.0407(3) 0.1951(11) 0.6363(8) 0.032(3) Uani 1 d . . C3 C 0.0683(3) 0.1182(13) 0.6618(8) 0.036(3) Uani 1 d . . C4 C 0.0690(3) 0.2600(12) 0.6857(8) 0.037(3) Uani 1 d . . C5 C -0.1097(3) 0.1232(12) 0.6021(8) 0.039(3) Uani 1 d . . C6 C -0.1099(3) 0.2620(13) 0.6259(8) 0.038(3) Uani 1 d . . C7 C 0.1446(3) 0.1289(13) 0.6634(10) 0.052(4) Uani 1 d . . H7A H 0.1680(3) 0.0764(13) 0.6715(10) 0.062 Uiso 1 calc R . H7B H 0.1446(3) 0.1798(13) 0.6062(10) 0.062 Uiso 1 calc R . C8 C 0.1436(3) 0.2373(12) 0.7405(8) 0.042(3) Uani 1 d . . H8A H 0.1676(3) 0.2861(12) 0.7482(8) 0.051 Uiso 1 calc R . H8B H 0.1396(3) 0.1884(12) 0.7967(8) 0.051 Uiso 1 calc R . C9A C -0.1891(4) 0.1344(17) 0.5701(11) 0.045(3) Uiso 0.84(2) d P 1 H9A H -0.2072(4) 0.0964(17) 0.5229(11) 0.054 Uiso 0.84(2) calc PR 1 C10A C -0.1794(4) 0.2833(17) 0.5391(11) 0.045(3) Uiso 0.84(2) d P 1 H10A H -0.2032(4) 0.3359(17) 0.5336(11) 0.054 Uiso 0.84(2) calc PR 1 C11 C -0.2091(5) 0.1295(20) 0.6596(12) 0.093(6) Uani 1 d . 1 H11A H -0.1906(5) 0.1397(20) 0.7110(12) 0.112 Uiso 1 calc R 1 H11B H -0.2267(5) 0.2079(20) 0.6609(12) 0.112 Uiso 1 calc R 1 C12 C -0.2302(5) -0.0111(29) 0.6674(16) 0.154(11) Uani 1 d . 1 H12A H -0.2424(5) -0.0124(29) 0.7231(16) 0.231 Uiso 1 calc R 1 H12B H -0.2127(5) -0.0885(29) 0.6670(16) 0.231 Uiso 1 calc R 1 H12C H -0.2487(5) -0.0204(29) 0.6170(16) 0.231 Uiso 1 calc R 1 C13A C -0.1657(5) 0.2841(20) 0.4498(12) 0.057(5) Uiso 0.84(2) d P 1 H13A H -0.1391(5) 0.2603(20) 0.4540(12) 0.068 Uiso 0.84(2) calc PR 1 H13B H -0.1791(5) 0.2141(20) 0.4116(12) 0.068 Uiso 0.84(2) calc PR 1 C14 C -0.1713(7) 0.4233(21) 0.4108(14) 0.151(11) Uani 1 d . 1 H14A H -0.1621(7) 0.4248(21) 0.3513(14) 0.226 Uiso 1 calc R 1 H14B H -0.1578(7) 0.4920(21) 0.4487(14) 0.226 Uiso 1 calc R 1 H14C H -0.1976(7) 0.4458(21) 0.4064(14) 0.226 Uiso 1 calc R 1 C9B C -0.1791(23) 0.1742(93) 0.5221(60) 0.045(3) Uiso 0.16(2) d P 2 C10B C -0.1869(22) 0.2622(90) 0.5906(62) 0.045(3) Uiso 0.16(2) d P 2 C13B C -0.1572(28) 0.3467(126) 0.4645(70) 0.057(5) Uiso 0.16(2) d P 2 S9 S 0.52462(8) 0.0553(3) 0.1365(2) 0.0382(7) Uani 1 d . 1 S10 S 0.52507(8) 0.3548(3) 0.1782(2) 0.0359(7) Uani 1 d . 1 S11 S 0.43404(8) 0.0611(3) 0.1041(2) 0.0408(8) Uani 1 d . 1 S12 S 0.43393(8) 0.3587(3) 0.1520(2) 0.0414(8) Uani 1 d . 1 S13 S 0.60666(8) 0.0184(3) 0.1501(2) 0.0459(8) Uani 1 d . 1 S14 S 0.60698(8) 0.3836(3) 0.2044(2) 0.0437(8) Uani 1 d . 1 S15 S 0.35104(9) 0.0347(4) 0.0833(3) 0.0567(10) Uani 1 d . 1 S16 S 0.35021(9) 0.3823(4) 0.1405(2) 0.0482(9) Uani 1 d . 1 C15 C 0.4988(3) 0.2083(11) 0.1534(7) 0.033(3) Uani 1 d . 1 C16 C 0.4598(3) 0.2093(11) 0.1381(7) 0.031(3) Uani 1 d . 1 C17 C 0.5683(3) 0.1306(13) 0.1572(8) 0.038(3) Uani 1 d . 1 C18 C 0.5684(3) 0.2721(12) 0.1791(8) 0.034(3) Uani 1 d . 1 C19 C 0.3902(3) 0.1384(13) 0.1084(8) 0.040(3) Uani 1 d . 1 C20 C 0.3906(3) 0.2793(13) 0.1332(8) 0.039(3) Uani 1 d . 1 C21 C 0.6453(3) 0.1431(13) 0.1533(9) 0.044(3) Uani 1 d . 1 H21A H 0.6688(3) 0.0910(13) 0.1607(9) 0.053 Uiso 1 calc R 1 H21B H 0.6446(3) 0.1925(13) 0.0956(9) 0.053 Uiso 1 calc R 1 C22 C 0.6446(3) 0.2520(13) 0.2291(9) 0.049(3) Uani 1 d . 1 H22A H 0.6687(3) 0.3000(13) 0.2363(9) 0.059 Uiso 1 calc R 1 H22B H 0.6407(3) 0.2041(13) 0.2858(9) 0.059 Uiso 1 calc R 1 C23 C 0.3132(3) 0.1660(15) 0.0492(10) 0.058(4) Uani 1 d . 1 H23 H 0.3016(3) 0.1342(15) -0.0098(10) 0.069 Uiso 1 calc R 1 C24 C 0.3248(4) 0.3098(14) 0.0366(10) 0.058(4) Uani 1 d . 1 H24 H 0.3016(4) 0.3656(14) 0.0266(10) 0.070 Uiso 1 calc R 1 C25 C 0.2819(4) 0.1496(19) 0.1189(12) 0.087(6) Uani 1 d . 1 H25A H 0.2799(4) 0.0509(19) 0.1364(12) 0.104 Uiso 1 calc R 1 H25B H 0.2889(4) 0.2045(19) 0.1731(12) 0.104 Uiso 1 calc R 1 C26 C 0.2428(4) 0.2023(19) 0.0752(13) 0.094(6) Uani 1 d . 1 H26A H 0.2242(4) 0.1918(19) 0.1182(13) 0.141 Uiso 1 calc R 1 H26B H 0.2357(4) 0.1471(19) 0.0220(13) 0.141 Uiso 1 calc R 1 H26C H 0.2447(4) 0.3004(19) 0.0587(13) 0.141 Uiso 1 calc R 1 C27 C 0.3468(4) 0.3345(19) -0.0454(10) 0.077(5) Uani 1 d . 1 H27A H 0.3606(4) 0.4224(19) -0.0355(10) 0.093 Uiso 1 calc R 1 H27B H 0.3652(4) 0.2591(19) -0.0469(10) 0.093 Uiso 1 calc R 1 C28 C 0.3278(5) 0.3420(24) -0.1315(13) 0.121(8) Uani 1 d . 1 H28A H 0.3455(5) 0.3579(24) -0.1761(13) 0.181 Uiso 1 calc R 1 H28B H 0.3100(5) 0.4187(24) -0.1331(13) 0.181 Uiso 1 calc R 1 H28C H 0.3147(5) 0.2545(24) -0.1445(13) 0.181 Uiso 1 calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0465(5) 0.0346(5) 0.0388(5) 0.0014(4) 0.0039(4) 0.0001(4) Br1 0.0416(8) 0.0553(9) 0.0805(11) 0.0038(8) 0.0059(7) -0.0035(7) Br2 0.0455(8) 0.0603(9) 0.0585(9) 0.0011(7) -0.0022(7) 0.0026(7) I2 0.0543(5) 0.0344(5) 0.0343(4) -0.0010(3) 0.0050(4) 0.0003(4) Br3 0.0506(9) 0.0551(9) 0.0763(11) -0.0038(8) 0.0053(8) -0.0054(7) Br4 0.0523(9) 0.0686(10) 0.0598(9) -0.0019(8) -0.0029(7) 0.0060(7) I3A 0.0383(5) 0.0686(7) 0.0853(8) -0.0237(6) -0.0144(5) 0.0100(5) Br5A 0.0769(12) 0.0951(14) 0.0904(13) -0.0077(11) -0.0094(10) 0.0259(10) Br6A 0.0620(12) 0.0919(15) 0.104(2) -0.0046(12) 0.0009(11) -0.0208(11) I3B 0.0769(12) 0.0951(14) 0.0904(13) -0.0077(11) -0.0094(10) 0.0259(10) Br5B 0.0620(12) 0.0919(15) 0.104(2) -0.0046(12) 0.0009(11) -0.0208(11) Br6B 0.0383(5) 0.0686(7) 0.0853(8) -0.0237(6) -0.0144(5) 0.0100(5) S1 0.032(2) 0.035(2) 0.055(2) -0.0004(15) -0.0012(15) 0.0006(13) S2 0.035(2) 0.033(2) 0.043(2) -0.0011(14) -0.0016(14) 0.0028(13) S3 0.031(2) 0.034(2) 0.064(2) -0.004(2) -0.003(2) 0.0023(13) S4 0.030(2) 0.034(2) 0.069(2) -0.003(2) -0.001(2) 0.0016(13) S5 0.031(2) 0.039(2) 0.089(3) -0.005(2) 0.002(2) 0.0044(14) S6 0.037(2) 0.047(2) 0.064(2) -0.009(2) -0.006(2) -0.004(2) S7 0.031(2) 0.042(2) 0.102(3) -0.007(2) -0.012(2) -0.0013(15) S8 0.031(2) 0.046(2) 0.096(3) -0.018(2) -0.004(2) 0.008(2) C1 0.025(6) 0.017(5) 0.038(6) 0.007(5) -0.005(5) -0.002(4) C2 0.029(6) 0.022(6) 0.044(7) 0.003(5) 0.004(5) 0.003(5) C3 0.026(6) 0.040(7) 0.042(7) 0.003(6) 0.005(5) -0.004(5) C4 0.037(7) 0.037(7) 0.036(7) 0.004(6) -0.002(5) -0.004(6) C5 0.040(7) 0.023(6) 0.053(8) 0.014(6) 0.004(6) 0.003(5) C6 0.024(6) 0.045(8) 0.045(7) 0.009(6) -0.001(5) -0.002(5) C7 0.024(7) 0.047(8) 0.082(10) 0.001(7) -0.007(7) -0.005(6) C8 0.037(7) 0.036(7) 0.054(8) -0.002(6) 0.002(6) -0.002(6) C11 0.092(13) 0.097(14) 0.097(14) 0.030(12) 0.051(11) 0.014(11) C12 0.080(15) 0.237(31) 0.147(22) -0.014(22) 0.019(14) -0.057(18) C14 0.247(30) 0.083(16) 0.113(18) 0.019(14) -0.045(19) 0.034(17) S9 0.024(2) 0.033(2) 0.057(2) 0.0018(14) 0.0006(14) 0.0002(12) S10 0.028(2) 0.029(2) 0.050(2) 0.0013(14) -0.0011(14) 0.0006(12) S11 0.027(2) 0.031(2) 0.064(2) -0.0023(15) -0.0011(15) 0.0005(13) S12 0.028(2) 0.030(2) 0.066(2) -0.0044(15) 0.001(2) 0.0029(13) S13 0.027(2) 0.040(2) 0.071(2) -0.003(2) 0.004(2) 0.0049(14) S14 0.029(2) 0.036(2) 0.065(2) -0.004(2) -0.0051(15) -0.0016(13) S15 0.032(2) 0.036(2) 0.099(3) 0.005(2) -0.011(2) -0.0024(15) S16 0.032(2) 0.042(2) 0.070(2) -0.010(2) 0.004(2) 0.0055(15) C15 0.035(7) 0.028(6) 0.037(7) 0.009(5) 0.001(5) -0.004(5) C16 0.030(6) 0.032(6) 0.031(6) 0.005(5) 0.002(5) -0.001(5) C17 0.025(6) 0.040(7) 0.051(8) 0.012(6) 0.006(6) 0.007(5) C18 0.025(6) 0.035(7) 0.041(7) -0.004(5) -0.006(5) 0.001(5) C19 0.033(7) 0.041(8) 0.046(8) 0.001(6) -0.004(6) 0.002(5) C20 0.025(6) 0.047(8) 0.045(7) -0.002(6) -0.004(5) -0.006(5) C21 0.022(6) 0.049(8) 0.060(8) -0.002(7) 0.001(6) 0.001(5) C22 0.045(8) 0.045(8) 0.056(8) 0.007(7) -0.004(7) -0.006(6) C23 0.030(7) 0.072(10) 0.069(10) -0.018(8) -0.015(7) 0.010(7) C24 0.045(8) 0.037(8) 0.090(11) 0.010(7) -0.006(8) 0.025(6) C25 0.053(10) 0.098(14) 0.114(15) 0.007(11) 0.035(10) 0.002(9) C26 0.024(8) 0.105(15) 0.155(18) -0.032(13) 0.019(9) -0.010(8) C27 0.072(12) 0.102(14) 0.059(10) 0.024(10) 0.014(9) 0.015(10) C28 0.077(14) 0.164(22) 0.120(18) 0.050(16) -0.001(13) -0.011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Br2 2.665(2) . ? I1 Br1 2.714(2) . ? I2 Br4 2.672(2) . ? I2 Br3 2.702(2) . ? I3A Br6A 2.722(2) . ? I3A Br5A 2.746(2) . ? I3B Br6B 2.746(2) . ? S1 C1 1.713(10) . ? S1 C3 1.732(11) . ? S2 C1 1.696(10) . ? S2 C4 1.751(12) . ? S3 C2 1.721(11) . ? S3 C5 1.725(12) . ? S4 C2 1.696(11) . ? S4 C6 1.734(11) . ? S5 C3 1.731(12) . ? S5 C7 1.793(12) . ? S6 C4 1.691(12) . ? S6 C8 1.826(12) . ? S7 C5 1.734(12) . ? S7 C9A 1.847(15) . ? S7 C9B 1.99(8) . ? S8 C6 1.753(12) . ? S8 C10B 1.76(8) . ? S8 C10A 1.89(2) . ? C1 C2 1.420(14) . ? C3 C4 1.38(2) . ? C5 C6 1.35(2) . ? C7 C8 1.53(2) . ? C9A C10A 1.52(2) . ? C9A C11 1.55(2) . ? C10A C13A 1.44(2) . ? C11 C12 1.53(3) . ? C13A C14 1.44(2) . ? C9B C10B 1.35(12) . ? C9B C13B 2.02(14) . ? S9 C17 1.715(12) . ? S9 C15 1.739(11) . ? S10 C15 1.694(11) . ? S10 C18 1.728(11) . ? S11 C16 1.724(11) . ? S11 C19 1.731(12) . ? S12 C16 1.704(11) . ? S12 C20 1.720(11) . ? S13 C17 1.739(11) . ? S13 C21 1.807(11) . ? S14 C18 1.749(11) . ? S14 C22 1.842(12) . ? S15 C19 1.720(12) . ? S15 C23 1.871(13) . ? S16 C20 1.746(12) . ? S16 C24 1.851(15) . ? C15 C16 1.391(14) . ? C17 C18 1.37(2) . ? C19 C20 1.38(2) . ? C21 C22 1.52(2) . ? C23 C24 1.43(2) . ? C23 C25 1.58(2) . ? C24 C27 1.51(2) . ? C25 C26 1.57(2) . ? C27 C28 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br2 I1 Br1 178.34(6) . . ? Br4 I2 Br3 178.69(6) . . ? Br6A I3A Br5A 177.72(7) . . ? C1 S1 C3 95.8(5) . . ? C1 S2 C4 97.0(5) . . ? C2 S3 C5 96.0(5) . . ? C2 S4 C6 95.6(6) . . ? C3 S5 C7 100.9(6) . . ? C4 S6 C8 101.5(6) . . ? C5 S7 C9A 104.7(6) . . ? C5 S7 C9B 92.8(25) . . ? C6 S8 C10B 103.0(27) . . ? C6 S8 C10A 96.0(7) . . ? C2 C1 S2 122.3(8) . . ? C2 C1 S1 121.8(8) . . ? S2 C1 S1 115.9(6) . . ? C1 C2 S4 122.9(8) . . ? C1 C2 S3 121.5(8) . . ? S4 C2 S3 115.5(6) . . ? C4 C3 S5 127.7(9) . . ? C4 C3 S1 117.2(9) . . ? S5 C3 S1 115.1(7) . . ? C3 C4 S6 129.9(9) . . ? C3 C4 S2 114.0(8) . . ? S6 C4 S2 116.0(7) . . ? C6 C5 S3 115.6(9) . . ? C6 C5 S7 127.7(9) . . ? S3 C5 S7 116.7(7) . . ? C5 C6 S4 117.0(9) . . ? C5 C6 S8 127.2(9) . . ? S4 C6 S8 115.7(7) . . ? C8 C7 S5 114.9(9) . . ? C7 C8 S6 111.0(8) . . ? C10A C9A C11 114.4(14) . . ? C10A C9A S7 112.1(11) . . ? C11 C9A S7 111.8(11) . . ? C13A C10A C9A 112.4(15) . . ? C13A C10A S8 117.6(13) . . ? C9A C10A S8 107.9(11) . . ? C12 C11 C9A 110.5(17) . . ? C14 C13A C10A 108.9(17) . . ? C10B C9B C13B 85.9(67) . . ? C10B C9B S7 108.5(64) . . ? C13B C9B S7 123.4(51) . . ? C9B C10B S8 115.7(66) . . ? C17 S9 C15 96.6(5) . . ? C15 S10 C18 96.4(5) . . ? C16 S11 C19 96.3(5) . . ? C16 S12 C20 96.2(6) . . ? C17 S13 C21 101.8(6) . . ? C18 S14 C22 100.7(6) . . ? C19 S15 C23 103.8(6) . . ? C20 S16 C24 95.5(6) . . ? C16 C15 S10 124.0(9) . . ? C16 C15 S9 121.1(8) . . ? S10 C15 S9 114.7(6) . . ? C15 C16 S12 121.9(8) . . ? C15 C16 S11 122.9(9) . . ? S12 C16 S11 115.1(6) . . ? C18 C17 S9 115.4(8) . . ? C18 C17 S13 128.1(9) . . ? S9 C17 S13 116.4(7) . . ? C17 C18 S10 116.8(8) . . ? C17 C18 S14 128.5(9) . . ? S10 C18 S14 114.7(7) . . ? C20 C19 S15 126.7(9) . . ? C20 C19 S11 115.1(9) . . ? S15 C19 S11 118.2(7) . . ? C19 C20 S12 117.0(9) . . ? C19 C20 S16 124.1(9) . . ? S12 C20 S16 118.8(7) . . ? C22 C21 S13 113.8(8) . . ? C21 C22 S14 111.2(8) . . ? C24 C23 C25 113.6(13) . . ? C24 C23 S15 116.8(9) . . ? C25 C23 S15 106.9(11) . . ? C23 C24 C27 115.0(13) . . ? C23 C24 S16 111.7(10) . . ? C27 C24 S16 110.9(11) . . ? C26 C25 C23 110.5(13) . . ? C28 C27 C24 119.5(15) . . ? 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 C4 S2 C1 C2 179.0(9) . . . . ? C4 S2 C1 S1 0.6(8) . . . . ? C3 S1 C1 C2 -179.7(9) . . . . ? C3 S1 C1 S2 -1.3(8) . . . . ? S2 C1 C2 S4 2.0(14) . . . . ? S1 C1 C2 S4 -179.6(6) . . . . ? S2 C1 C2 S3 177.9(6) . . . . ? S1 C1 C2 S3 -3.8(14) . . . . ? C6 S4 C2 C1 -178.5(10) . . . . ? C6 S4 C2 S3 5.4(8) . . . . ? C5 S3 C2 C1 178.8(9) . . . . ? C5 S3 C2 S4 -5.0(8) . . . . ? C7 S5 C3 C4 -11.9(13) . . . . ? C7 S5 C3 S1 168.6(7) . . . . ? C1 S1 C3 C4 1.9(10) . . . . ? C1 S1 C3 S5 -178.6(7) . . . . ? S5 C3 C4 S6 -0.3(18) . . . . ? S1 C3 C4 S6 179.1(7) . . . . ? S5 C3 C4 S2 178.8(7) . . . . ? S1 C3 C4 S2 -1.8(13) . . . . ? C8 S6 C4 C3 -15.1(13) . . . . ? C8 S6 C4 S2 165.8(7) . . . . ? C1 S2 C4 C3 0.7(10) . . . . ? C1 S2 C4 S6 180.0(7) . . . . ? C2 S3 C5 C6 2.3(11) . . . . ? C2 S3 C5 S7 -177.7(7) . . . . ? C9A S7 C5 C6 6.6(14) . . . . ? C9B S7 C5 C6 31.0(29) . . . . ? C9A S7 C5 S3 -173.4(8) . . . . ? C9B S7 C5 S3 -149.0(26) . . . . ? S3 C5 C6 S4 1.0(13) . . . . ? S7 C5 C6 S4 -179.0(7) . . . . ? S3 C5 C6 S8 179.6(7) . . . . ? S7 C5 C6 S8 -0.4(18) . . . . ? C2 S4 C6 C5 -3.9(11) . . . . ? C2 S4 C6 S8 177.4(7) . . . . ? C10B S8 C6 C5 -7.1(33) . . . . ? C10A S8 C6 C5 -33.2(13) . . . . ? C10B S8 C6 S4 171.4(31) . . . . ? C10A S8 C6 S4 145.3(8) . . . . ? C3 S5 C7 C8 48.2(10) . . . . ? S5 C7 C8 S6 -71.3(11) . . . . ? C4 S6 C8 C7 48.7(10) . . . . ? C5 S7 C9A C10A 31.9(13) . . . . ? C9B S7 C9A C10A -34.1(54) . . . . ? C5 S7 C9A C11 -98.0(13) . . . . ? C9B S7 C9A C11 -164.0(60) . . . . ? C11 C9A C10A C13A -172.1(14) . . . . ? S7 C9A C10A C13A 59.4(16) . . . . ? C11 C9A C10A S8 56.6(15) . . . . ? S7 C9A C10A S8 -71.9(13) . . . . ? C6 S8 C10A C13A -60.0(14) . . . . ? C10B S8 C10A C13A -167.1(68) . . . . ? C6 S8 C10A C9A 68.4(11) . . . . ? C10B S8 C10A C9A -38.7(61) . . . . ? C10A C9A C11 C12 159.3(16) . . . . ? S7 C9A C11 C12 -72.0(18) . . . . ? C9A C10A C13A C14 157.4(16) . . . . ? S8 C10A C13A C14 -76.4(19) . . . . ? C5 S7 C9B C10B -68.2(64) . . . . ? C9A S7 C9B C10B 49.6(60) . . . . ? C5 S7 C9B C13B 29.4(62) . . . . ? C9A S7 C9B C13B 147.2(101) . . . . ? C13B C9B C10B S8 -49.0(68) . . . . ? S7 C9B C10B S8 74.9(79) . . . . ? C6 S8 C10B C9B -34.8(78) . . . . ? C10A S8 C10B C9B 42.4(63) . . . . ? C18 S10 C15 C16 -176.1(10) . . . . ? C18 S10 C15 S9 -2.4(8) . . . . ? C17 S9 C15 C16 175.2(9) . . . . ? C17 S9 C15 S10 1.4(8) . . . . ? S10 C15 C16 S12 -5.4(14) . . . . ? S9 C15 C16 S12 -178.7(6) . . . . ? S10 C15 C16 S11 174.7(6) . . . . ? S9 C15 C16 S11 1.4(14) . . . . ? C20 S12 C16 C15 -174.6(9) . . . . ? C20 S12 C16 S11 5.3(8) . . . . ? C19 S11 C16 C15 175.6(10) . . . . ? C19 S11 C16 S12 -4.4(8) . . . . ? C15 S9 C17 C18 0.7(11) . . . . ? C15 S9 C17 S13 179.5(7) . . . . ? C21 S13 C17 C18 -12.4(13) . . . . ? C21 S13 C17 S9 169.1(7) . . . . ? S9 C17 C18 S10 -2.5(13) . . . . ? S13 C17 C18 S10 178.9(7) . . . . ? S9 C17 C18 S14 179.9(7) . . . . ? S13 C17 C18 S14 1.3(18) . . . . ? C15 S10 C18 C17 3.0(11) . . . . ? C15 S10 C18 S14 -179.1(7) . . . . ? C22 S14 C18 C17 -17.1(13) . . . . ? C22 S14 C18 S10 165.3(7) . . . . ? C23 S15 C19 C20 23.2(13) . . . . ? C23 S15 C19 S11 -157.5(8) . . . . ? C16 S11 C19 C20 1.3(11) . . . . ? C16 S11 C19 S15 -178.1(7) . . . . ? S15 C19 C20 S12 -178.4(7) . . . . ? S11 C19 C20 S12 2.2(14) . . . . ? S15 C19 C20 S16 -1.9(18) . . . . ? S11 C19 C20 S16 178.7(7) . . . . ? C16 S12 C20 C19 -4.5(11) . . . . ? C16 S12 C20 S16 178.8(7) . . . . ? C24 S16 C20 C19 -40.7(12) . . . . ? C24 S16 C20 S12 135.7(8) . . . . ? C17 S13 C21 C22 48.5(10) . . . . ? S13 C21 C22 S14 -72.7(10) . . . . ? C18 S14 C22 C21 51.2(10) . . . . ? C19 S15 C23 C24 9.9(13) . . . . ? C19 S15 C23 C25 -118.7(11) . . . . ? C25 C23 C24 C27 -165.1(12) . . . . ? S15 C23 C24 C27 69.7(15) . . . . ? C25 C23 C24 S16 67.4(13) . . . . ? S15 C23 C24 S16 -57.8(13) . . . . ? C20 S16 C24 C23 70.7(10) . . . . ? C20 S16 C24 C27 -59.0(10) . . . . ? C24 C23 C25 C26 74.0(17) . . . . ? S15 C23 C25 C26 -155.7(11) . . . . ? C23 C24 C27 C28 77.8(20) . . . . ? S16 C24 C27 C28 -154.3(16) . . . . ? _refine_diff_density_max 1.284 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.166 #===END ############################## End of CIF file ##############################