# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Auban-Senzier, Pascale' 'Avarvari, N.' 'Bertran, J. N.' 'Canadell, Enrique' 'Devic, Thomas' 'Domercq, Benoit' 'Fourmigue, Marc' _publ_contact_author_name 'Dr Marc Fourmigue' _publ_contact_author_address ; Sciences Moleculaires aux Interfaces FRE 2068 CNRS, Institut des Mat Jean Rouxel 2, rue de la Houssiniere Nantes BP32229, F-44322 cedex 3 FRANCE ; _publ_contact_author_email 'FOURMIGUE@CNRS-IMN.FR' _publ_section_title ; Cation Radical Salts of Cyano(ethylenedithio) Tetrathiafulvalene With Halogenated Anions: Annihilation of the CN***Hal Interaction and Stabilisation of Conducting Salt, Antiferromagnetic Square Lattice and Chain ; data_edtcn _database_code_CSD 170662 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4-cyano-4',5'-ethylendithio-tetrathiafulvalene ; _chemical_name_common '(CN)EDT-TTF' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 N S6' _chemical_formula_weight 319.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9395(14) _cell_length_b 7.6083(15) _cell_length_c 12.502(3) _cell_angle_alpha 104.45(3) _cell_angle_beta 93.03(3) _cell_angle_gamma 95.46(3) _cell_volume 634.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3585 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.85 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 324 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_T_max 0.9533 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.9 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5854 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.95 _reflns_number_total 2170 _reflns_number_gt 1501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'SELECT, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.3951P] 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 2170 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.274 _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 S1 S 0.1048(2) 0.7079(2) -0.03905(13) 0.0362(4) Uani 1 1 d . . . S2 S -0.3474(2) 0.6482(3) -0.09296(14) 0.0399(5) Uani 1 1 d . . . S3 S 0.0384(2) 0.9589(2) 0.20370(14) 0.0380(5) Uani 1 1 d . . . S4 S -0.4117(2) 0.9063(3) 0.14824(14) 0.0418(5) Uani 1 1 d . . . S5 S 0.0147(3) 1.2241(3) 0.42181(15) 0.0473(5) Uani 1 1 d . . . S6 S -0.5103(3) 1.1600(3) 0.35123(16) 0.0572(6) Uani 1 1 d . . . N1 N 0.2701(10) 0.4175(9) -0.2977(5) 0.0578(18) Uani 1 1 d . . . C1 C 0.1517(10) 0.4819(10) -0.2405(6) 0.0426(17) Uani 1 1 d . . . C2 C 0.0069(10) 0.5631(8) -0.1670(5) 0.0343(15) Uani 1 1 d . . . C3 C -0.1960(10) 0.5380(10) -0.1896(5) 0.0410(17) Uani 1 1 d . . . H3 H -0.2504 0.4619 -0.2568 0.049 Uiso 1 1 calc R . . C4 C -0.1408(9) 0.7527(8) 0.0042(5) 0.0315(15) Uani 1 1 d . . . C5 C -0.1681(9) 0.8593(9) 0.1047(5) 0.0337(15) Uani 1 1 d . . . C6 C -0.1144(9) 1.0866(9) 0.2995(5) 0.0330(15) Uani 1 1 d . . . C7 C -0.3176(9) 1.0625(9) 0.2744(5) 0.0339(15) Uani 1 1 d . . . C8 C -0.1875(12) 1.2145(15) 0.5125(6) 0.073(3) Uani 1 1 d . . . H8A H -0.2135 1.0892 0.5172 0.087 Uiso 1 1 calc R . . H8B H -0.1420 1.2878 0.5863 0.087 Uiso 1 1 calc R . . C9 C -0.3775(12) 1.2762(15) 0.4810(7) 0.075(3) Uani 1 1 d . . . H9A H -0.3524 1.4041 0.4816 0.090 Uiso 1 1 calc R . . H9B H -0.4626 1.2696 0.5393 0.090 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 S1 0.0302(9) 0.0418(10) 0.0302(9) -0.0036(7) 0.0025(7) 0.0059(8) S2 0.0299(9) 0.0515(11) 0.0293(9) -0.0068(8) -0.0013(7) 0.0069(8) S3 0.0271(9) 0.0456(10) 0.0314(9) -0.0095(8) 0.0011(7) 0.0076(8) S4 0.0276(9) 0.0525(11) 0.0332(9) -0.0112(8) -0.0003(8) 0.0058(8) S5 0.0318(10) 0.0638(12) 0.0309(9) -0.0139(9) 0.0033(8) -0.0015(9) S6 0.0290(10) 0.0937(16) 0.0341(10) -0.0147(10) 0.0037(8) 0.0162(10) N1 0.058(4) 0.069(4) 0.042(4) -0.001(3) 0.019(3) 0.020(4) C1 0.038(4) 0.050(4) 0.035(4) 0.002(3) 0.003(3) 0.008(4) C2 0.044(4) 0.027(3) 0.028(3) 0.000(3) 0.003(3) 0.007(3) C3 0.045(4) 0.046(4) 0.023(3) -0.007(3) -0.002(3) 0.008(4) C4 0.032(4) 0.029(3) 0.030(3) -0.001(3) 0.003(3) 0.004(3) C5 0.032(4) 0.037(4) 0.029(3) 0.001(3) -0.001(3) 0.007(3) C6 0.032(4) 0.035(3) 0.026(3) -0.004(3) 0.007(3) 0.002(3) C7 0.036(4) 0.036(4) 0.026(3) -0.001(3) 0.006(3) 0.005(3) C8 0.054(5) 0.128(8) 0.026(4) 0.000(5) 0.006(4) 0.012(6) C9 0.046(5) 0.125(8) 0.038(4) -0.012(5) 0.009(4) 0.017(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 C2 1.760(7) . ? S1 C4 1.852(6) . ? S2 C3 1.751(6) . ? S2 C4 1.811(7) . ? S3 C6 1.803(6) . ? S3 C5 1.816(7) . ? S4 C7 1.771(7) . ? S4 C5 1.843(6) . ? S5 C6 1.765(7) . ? S5 C8 1.857(8) . ? S6 C7 1.797(6) . ? S6 C9 1.799(9) . ? N1 C1 1.179(8) . ? C1 C2 1.473(9) . ? C2 C3 1.407(9) . ? C4 C5 1.348(8) . ? C6 C7 1.412(9) . ? C8 C9 1.506(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 C2 S1 C4 91.4(3) . . ? C3 S2 C4 91.4(3) . . ? C6 S3 C5 91.7(3) . . ? C7 S4 C5 93.0(3) . . ? C6 S5 C8 95.9(4) . . ? C7 S6 C9 100.4(3) . . ? N1 C1 C2 178.8(8) . . ? C3 C2 C1 126.9(6) . . ? C3 C2 S1 118.4(5) . . ? C1 C2 S1 114.8(5) . . ? C2 C3 S2 120.8(5) . . ? C5 C4 S2 120.1(5) . . ? C5 C4 S1 121.9(5) . . ? S2 C4 S1 118.0(3) . . ? C4 C5 S3 120.2(5) . . ? C4 C5 S4 122.3(5) . . ? S3 C5 S4 117.5(3) . . ? C7 C6 S5 126.9(4) . . ? C7 C6 S3 119.5(5) . . ? S5 C6 S3 113.4(4) . . ? C6 C7 S4 117.9(4) . . ? C6 C7 S6 131.3(5) . . ? S4 C7 S6 110.8(4) . . ? C9 C8 S5 118.5(7) . . ? C8 C9 S6 119.6(6) . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 0.420 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.084 #===END data_EDTCNI3 _database_code_CSD 170663 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis (3-cyano -3',4'-ethylenedithiotetrathiafulvalene, triiodide) ; _chemical_name_common '(EDT-TTF-CN), (I3)' _chemical_melting_point ? _chemical_formula_moiety '(C9H5NS6), (I3)' _chemical_formula_sum 'C9 H5 I3 N S6' _chemical_formula_weight 700.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9359(16) _cell_length_b 9.4229(19) _cell_length_c 11.957(2) _cell_angle_alpha 99.04(3) _cell_angle_beta 94.56(3) _cell_angle_gamma 103.70(3) _cell_volume 851.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5700 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.85 _exptl_crystal_description 'plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.2118 _exptl_crystal_size_mid 0.0962 _exptl_crystal_size_min 0.027 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 6.226 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4517 _exptl_absorpt_correction_T_max 0.8230 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ; _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_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.3' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8345 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.85 _reflns_number_total 3083 _reflns_number_gt 1998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^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 3083 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 0.718 _refine_ls_restrained_S_all 0.718 _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 I1 I 0.20431(5) 0.37968(4) 0.04264(3) 0.03043(10) Uani 1 1 d . . . I2 I 0.08432(6) 0.30538(4) -0.20093(3) 0.04414(13) Uani 1 1 d . . . I3 I 0.34181(6) 0.44971(4) 0.28241(3) 0.04145(13) Uani 1 1 d . . . S1 S 1.29810(19) 0.04108(15) 0.15557(11) 0.0282(3) Uani 1 1 d . . . S2 S 1.4543(2) -0.21298(15) 0.13006(12) 0.0314(4) Uani 1 1 d . . . S3 S 1.16455(19) -0.03440(15) -0.11365(11) 0.0245(3) Uani 1 1 d . . . C1 C 1.3922(8) -0.0006(7) 0.2775(5) 0.0320(13) Uani 1 1 d . . . H1 H 1.3927 0.0550 0.3491 0.038 Uiso 0.393(14) 1 calc PR . . C2 C 1.4643(8) -0.1160(6) 0.2651(5) 0.0360(14) Uani 1 1 d . . . H2 H 1.5181 -0.1426 0.3277 0.043 Uiso 0.607(14) 1 calc PR . . C3 C 1.3389(7) -0.1069(5) 0.0662(4) 0.0212(11) Uani 1 1 d . . . S4 S 1.3206(2) -0.28605(14) -0.13968(12) 0.0277(3) Uani 1 1 d . . . S5 S 1.0218(2) -0.07793(16) -0.35451(12) 0.0325(4) Uani 1 1 d . . . S6 S 1.2212(2) -0.37672(17) -0.38764(12) 0.0399(4) Uani 1 1 d . . . C4 C 1.2804(7) -0.1406(5) -0.0487(4) 0.0218(12) Uani 1 1 d . . . C5 C 1.1400(7) -0.1369(5) -0.2503(4) 0.0211(12) Uani 1 1 d . . . C6 C 1.2144(7) -0.2549(5) -0.2627(4) 0.0237(12) Uani 1 1 d . . . C7 C 0.9827(7) -0.2347(6) -0.4693(4) 0.0306(14) Uani 1 1 d . . . H7A H 0.8987 -0.3174 -0.4499 0.037 Uiso 1 1 calc R . . H7B H 0.9318 -0.2094 -0.5376 0.037 Uiso 1 1 calc R . . C8 C 1.1468(8) -0.2828(6) -0.4945(4) 0.0324(14) Uani 1 1 d . . . H8A H 1.2386 -0.1960 -0.4992 0.039 Uiso 1 1 calc R . . H8B H 1.1243 -0.3485 -0.5681 0.039 Uiso 1 1 calc R . . C9A C 1.3907(13) 0.0737(10) 0.3876(8) 0.030(3) Uani 0.607(14) 1 d P . . N1A N 1.3913(14) 0.1358(11) 0.4777(12) 0.043(3) Uani 0.607(14) 1 d P . . C9B C 1.545(2) -0.1343(16) 0.3702(13) 0.033(5) Uani 0.393(14) 1 d P . . N1B N 1.605(2) -0.1546(19) 0.4531(19) 0.048(5) Uani 0.393(14) 1 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 0.0363(2) 0.02547(19) 0.0297(2) 0.00440(15) 0.00342(18) 0.00877(17) I2 0.0656(3) 0.0334(2) 0.0287(2) 0.00222(17) -0.0085(2) 0.0103(2) I3 0.0546(3) 0.0463(3) 0.0268(2) 0.00500(19) 0.0047(2) 0.0206(2) S1 0.0299(9) 0.0360(8) 0.0183(7) -0.0008(6) 0.0003(7) 0.0122(7) S2 0.0403(10) 0.0288(7) 0.0258(8) 0.0056(6) -0.0042(7) 0.0123(7) S3 0.0288(8) 0.0280(7) 0.0173(7) 0.0011(6) -0.0002(7) 0.0114(6) C1 0.025(3) 0.050(4) 0.012(3) -0.001(2) -0.003(3) -0.001(3) C2 0.032(4) 0.050(4) 0.019(3) 0.008(3) -0.004(3) -0.002(3) C3 0.019(3) 0.024(3) 0.016(3) 0.001(2) 0.000(3) 0.000(2) S4 0.0390(10) 0.0225(7) 0.0210(7) 0.0000(6) -0.0029(7) 0.0110(7) S5 0.0456(10) 0.0330(8) 0.0201(7) -0.0004(6) -0.0060(7) 0.0190(7) S6 0.0618(12) 0.0391(8) 0.0216(7) -0.0056(6) -0.0062(8) 0.0291(8) C4 0.015(3) 0.021(3) 0.026(3) 0.007(2) 0.001(3) 0.000(2) C5 0.022(3) 0.025(3) 0.014(3) 0.002(2) -0.004(2) 0.005(2) C6 0.026(3) 0.027(3) 0.016(3) 0.006(2) -0.002(3) 0.004(3) C7 0.033(4) 0.039(3) 0.016(3) -0.005(2) -0.003(3) 0.009(3) C8 0.040(4) 0.036(3) 0.017(3) -0.007(2) 0.002(3) 0.009(3) C9A 0.029(6) 0.037(6) 0.025(6) 0.000(4) 0.000(5) 0.015(5) N1A 0.047(7) 0.064(6) 0.019(6) 0.000(5) -0.005(6) 0.026(5) C9B 0.032(10) 0.037(9) 0.027(10) -0.003(7) 0.009(8) 0.008(7) N1B 0.049(11) 0.077(11) 0.020(10) 0.017(10) 0.000(9) 0.018(9) _geom_special_details ; The cyano group is disordered on two positions, occupancy parameter refinement converged to a 60:40 distribution. 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 I3 2.9002(10) . ? I1 I2 2.9121(10) . ? S1 C1 1.727(6) . ? S1 C3 1.730(5) . ? S2 C2 1.712(6) . ? S2 C3 1.727(5) . ? S3 C5 1.734(5) . ? S3 C4 1.736(5) . ? C1 C2 1.338(7) . ? C3 C4 1.377(7) . ? S4 C4 1.720(5) . ? S4 C6 1.737(5) . ? S5 C5 1.738(5) . ? S5 C7 1.800(5) . ? S6 C6 1.748(5) . ? S6 C8 1.802(5) . ? C5 C6 1.371(6) . ? C7 C8 1.514(7) . ? C9A N1A 1.141(15) . ? C9A N1B 1.93(2) 2_856 ? N1A N1B 0.815(15) 2_856 ? N1A C9B 1.85(2) 2_856 ? C9B N1B 1.13(2) . ? C9B N1A 1.85(2) 2_856 ? N1B N1A 0.815(15) 2_856 ? N1B C9A 1.93(2) 2_856 ? 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 I3 I1 I2 176.83(2) . . ? C1 S1 C3 94.1(3) . . ? C2 S2 C3 94.6(3) . . ? C5 S3 C4 96.2(2) . . ? C2 C1 S1 117.5(4) . . ? C1 C2 S2 117.7(4) . . ? C4 C3 S2 121.7(4) . . ? C4 C3 S1 122.3(4) . . ? S2 C3 S1 116.0(3) . . ? C4 S4 C6 96.3(2) . . ? C5 S5 C7 100.9(2) . . ? C6 S6 C8 101.0(2) . . ? C3 C4 S4 123.3(4) . . ? C3 C4 S3 122.0(4) . . ? S4 C4 S3 114.8(3) . . ? C6 C5 S3 116.3(4) . . ? C6 C5 S5 128.1(4) . . ? S3 C5 S5 115.7(3) . . ? C5 C6 S4 116.4(4) . . ? C5 C6 S6 128.4(4) . . ? S4 C6 S6 115.2(3) . . ? C8 C7 S5 113.1(4) . . ? C7 C8 S6 112.7(4) . . ? N1A C9A N1B 7.7(8) . 2_856 ? N1B N1A C9A 161.4(19) 2_856 . ? N1B N1A C9B 21.1(13) 2_856 2_856 ? C9A N1A C9B 142.3(9) . 2_856 ? N1B C9B N1A 15.0(10) . 2_856 ? N1A N1B C9B 144(2) 2_856 . ? N1A N1B C9A 10.9(11) 2_856 2_856 ? C9B N1B C9A 134.7(15) . 2_856 ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.675 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.112 #===END data_edtcn2I3 _database_code_CSD 170664 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(3-cyano -3',4'-ethylenedithiotetrathiafulvalene), triiodide ; _chemical_name_common '(EDT-TTF-CN)2, (I3)' _chemical_melting_point ? _chemical_formula_moiety '(C9H5NS6)2, (I3)' _chemical_formula_sum 'C18 H10 I3 N2 S12' _chemical_formula_weight 1019.7 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0545(16) _cell_length_b 8.0611(16) _cell_length_c 23.587(5) _cell_angle_alpha 86.78(3) _cell_angle_beta 86.82(3) _cell_angle_gamma 76.11(3) _cell_volume 1482.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.8 _exptl_crystal_description 'plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 4.023 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3314 _exptl_absorpt_correction_T_max 0.8061 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; The triclinic unit cell allows for a monoclinic C-centered transformation. Attempts to refine the structure in the monoclinic C2/c space group led to a much higher R(F) value. In the triclinic P-1 refinement, the two crystallographically independent donor molecules do correspond through a pseudo inversion center but the two crystallographically independent I3- anions do not. ; _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_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.0' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12816 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.77 _reflns_number_total 5233 _reflns_number_gt 2659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5233 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 0.697 _refine_ls_restrained_S_all 0.697 _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 I1 I 0.0000 0.0000 0.5000 0.0497(2) Uani 1 2 d S . . I2 I -0.09176(8) -0.11042(9) 0.61437(2) 0.0778(2) Uani 1 1 d . . . I3 I 0.0000 0.0000 0.0000 0.0496(2) Uani 1 2 d S . . I4 I -0.11109(8) -0.09159(9) 0.11430(2) 0.0777(2) Uani 1 1 d . . . S1 S -0.5769(3) 0.7349(3) 0.57362(8) 0.0590(6) Uani 1 1 d . . . S2 S -0.2703(2) 0.4496(3) 0.57429(8) 0.0601(6) Uani 1 1 d . . . S3 S -0.4748(3) 0.8394(3) 0.44392(8) 0.0542(6) Uani 1 1 d . . . S4 S -0.1695(2) 0.5551(3) 0.44602(8) 0.0572(6) Uani 1 1 d . . . S5 S -0.4220(3) 0.9471(3) 0.32419(8) 0.0682(7) Uani 1 1 d . . . S6 S -0.0567(2) 0.6086(3) 0.32703(8) 0.0705(7) Uani 1 1 d . . . C8 C -0.0934(18) 0.819(2) 0.2852(7) 0.053(5) Uiso 0.55(3) 1 d P . . C8' C -0.130(2) 0.751(3) 0.2694(9) 0.057(6) Uiso 0.45(3) 1 d P . . C1 C -0.5335(11) 0.6151(12) 0.6369(3) 0.063(2) Uani 1 1 d . . . C2 C -0.3938(10) 0.4859(12) 0.6360(3) 0.061(2) Uani 1 1 d . . . C3 C -0.3950(8) 0.6239(9) 0.5372(3) 0.0433(17) Uani 1 1 d . . . C4 C -0.3510(8) 0.6684(9) 0.4822(3) 0.0421(17) Uani 1 1 d . . . C5 C -0.3480(8) 0.8026(9) 0.3808(3) 0.0421(17) Uani 1 1 d . . . C6 C -0.2097(8) 0.6755(9) 0.3819(3) 0.0420(18) Uani 1 1 d . . . C7 C -0.2891(18) 0.8492(19) 0.2643(6) 0.050(5) Uiso 0.55(3) 1 d P . . C7' C -0.229(2) 0.913(3) 0.2777(8) 0.055(6) Uiso 0.45(3) 1 d P . . C9A C -0.6192(16) 0.644(2) 0.6881(6) 0.049(4) Uani 0.50 1 d P . . N1A N -0.6965(19) 0.673(2) 0.7293(6) 0.075(5) Uani 0.50 1 d P . . C9B C -0.3676(19) 0.399(2) 0.6856(8) 0.063(5) Uani 0.50 1 d P . . N1B N -0.334(2) 0.319(2) 0.7296(9) 0.077(5) Uani 0.50 1 d P . . S11 S -0.7348(2) 0.5775(3) 0.92660(8) 0.0591(6) Uani 1 1 d . . . S12 S -0.4501(3) 0.2707(3) 0.92554(8) 0.0594(6) Uani 1 1 d . . . S13 S -0.8394(2) 0.4746(3) 1.05607(8) 0.0544(6) Uani 1 1 d . . . S14 S -0.5554(3) 0.1697(3) 1.05394(8) 0.0564(6) Uani 1 1 d . . . S15 S -0.9479(3) 0.4216(3) 1.17562(8) 0.0687(7) Uani 1 1 d . . . S16 S -0.6088(3) 0.0569(3) 1.17279(9) 0.0715(7) Uani 1 1 d . . . C11 C -0.6165(10) 0.5348(12) 0.8637(3) 0.061(2) Uani 1 1 d . . . C12 C -0.4878(11) 0.3953(11) 0.8637(3) 0.061(2) Uani 1 1 d . . . C13 C -0.6240(8) 0.3954(9) 0.9632(3) 0.0439(18) Uani 1 1 d . . . C14 C -0.6686(8) 0.3513(9) 1.0177(3) 0.0428(17) Uani 1 1 d . . . C15 C -0.8058(8) 0.3497(10) 1.1185(3) 0.0459(19) Uani 1 1 d . . . C16 C -0.6757(9) 0.2082(10) 1.1177(3) 0.0465(18) Uani 1 1 d . . . C17 C -0.920(3) 0.221(3) 1.2201(9) 0.055(7) Uiso 0.40(3) 1 d P . . C18 C -0.744(3) 0.137(3) 1.2310(8) 0.050(6) Uiso 0.40(3) 1 d P . . C17' C -0.8570(15) 0.2843(18) 1.2350(5) 0.047(4) Uiso 0.60(3) 1 d P . . C18' C -0.8148(17) 0.0948(19) 1.2164(6) 0.052(4) Uiso 0.60(3) 1 d P . . C19A C -0.3990(18) 0.368(2) 0.8129(7) 0.051(4) Uani 0.50 1 d P . . N11A N -0.322(2) 0.334(2) 0.7703(9) 0.076(5) Uani 0.50 1 d P . . C19B C -0.6422(19) 0.6225(19) 0.8123(6) 0.054(4) Uani 0.50 1 d P . . N11B N -0.672(2) 0.693(2) 0.7698(7) 0.081(5) Uani 0.50 1 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 0.0515(4) 0.0546(5) 0.0353(4) 0.0026(3) 0.0025(3) 0.0006(3) I2 0.0896(4) 0.0990(5) 0.0369(4) 0.0127(3) 0.0099(3) -0.0133(4) I3 0.0541(4) 0.0517(5) 0.0358(4) 0.0021(3) 0.0023(3) 0.0000(3) I4 0.0973(5) 0.0905(5) 0.0373(4) 0.0104(3) 0.0123(3) -0.0133(4) S1 0.0776(13) 0.0538(13) 0.0399(11) 0.0042(9) 0.0188(9) -0.0107(10) S2 0.0499(10) 0.0850(16) 0.0416(11) 0.0190(10) 0.0021(8) -0.0141(10) S3 0.0732(12) 0.0497(12) 0.0334(10) 0.0044(8) 0.0155(8) -0.0076(10) S4 0.0450(10) 0.0870(16) 0.0335(10) 0.0170(9) 0.0034(7) -0.0094(10) S5 0.0826(13) 0.0677(15) 0.0373(11) 0.0117(9) 0.0130(9) 0.0087(11) S6 0.0589(11) 0.0963(18) 0.0379(11) 0.0173(11) 0.0134(8) 0.0092(11) C1 0.082(6) 0.074(6) 0.038(5) 0.005(4) 0.012(4) -0.036(5) C2 0.073(5) 0.090(7) 0.030(4) 0.012(4) 0.005(3) -0.044(5) C3 0.051(4) 0.051(5) 0.034(4) 0.001(3) 0.001(3) -0.024(3) C4 0.049(4) 0.050(5) 0.031(4) 0.004(3) 0.003(3) -0.021(3) C5 0.054(4) 0.050(5) 0.024(4) 0.001(3) 0.005(3) -0.019(3) C6 0.045(4) 0.058(5) 0.023(4) 0.006(3) 0.005(3) -0.016(3) C9A 0.045(7) 0.073(11) 0.027(8) 0.011(7) 0.012(6) -0.015(7) N1A 0.093(10) 0.099(13) 0.027(8) 0.024(8) 0.019(8) -0.019(8) C9B 0.059(9) 0.068(12) 0.053(11) 0.012(9) 0.020(8) -0.005(8) N1B 0.082(11) 0.078(12) 0.070(13) -0.007(11) 0.019(10) -0.021(8) S11 0.0541(10) 0.0785(15) 0.0393(11) 0.0186(10) 0.0035(8) -0.0114(10) S12 0.0841(13) 0.0499(13) 0.0398(11) 0.0020(9) 0.0186(9) -0.0130(10) S13 0.0484(10) 0.0743(14) 0.0347(10) 0.0174(9) 0.0042(7) -0.0088(9) S14 0.0853(13) 0.0440(12) 0.0347(11) 0.0030(8) 0.0171(9) -0.0108(10) S15 0.0658(12) 0.0846(16) 0.0377(11) 0.0133(10) 0.0126(9) 0.0106(11) S16 0.0975(15) 0.0608(14) 0.0368(11) 0.0148(9) 0.0167(10) 0.0109(12) C11 0.065(5) 0.084(7) 0.040(5) 0.019(4) 0.000(4) -0.034(5) C12 0.091(6) 0.070(6) 0.035(5) -0.002(4) 0.021(4) -0.045(5) C13 0.051(4) 0.054(5) 0.031(4) 0.007(3) -0.002(3) -0.022(3) C14 0.049(4) 0.048(5) 0.037(4) 0.000(3) 0.001(3) -0.022(3) C15 0.052(4) 0.055(5) 0.032(4) 0.006(3) 0.002(3) -0.017(3) C16 0.063(4) 0.051(5) 0.029(4) 0.000(3) 0.006(3) -0.023(4) C19A 0.056(9) 0.053(10) 0.041(10) 0.001(7) 0.006(7) -0.008(7) N11A 0.077(10) 0.067(12) 0.080(14) -0.002(10) -0.004(10) -0.011(8) C19B 0.082(10) 0.043(9) 0.030(9) 0.012(7) 0.010(7) -0.008(8) N11B 0.102(11) 0.094(12) 0.036(9) 0.027(9) 0.019(8) -0.017(9) _geom_special_details ; Two crystallographically independent molecules, each of them with a CN group disordered on two positions as well as a disordered ethylene group. Accordingly, hydrogen atoms were not introduced. Occupation parameters of the disordered cyano groups converged in both cases to a 50:50 distribution and final refinement was performed anisotropically with a fixed 50:50 distribution. The carbon atoms of the ethylenic groups were refined isotropically and their occupation parameters were also refined. 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 2.9051(9) 2_556 ? I1 I2 2.9052(9) . ? I3 I4 2.9050(9) 2 ? I3 I4 2.9050(9) . ? S1 C3 1.733(7) . ? S1 C1 1.737(8) . ? S2 C2 1.715(8) . ? S2 C3 1.741(7) . ? S3 C4 1.734(7) . ? S3 C5 1.756(6) . ? S4 C4 1.734(7) . ? S4 C6 1.754(6) . ? S5 C5 1.753(6) . ? S5 C7 1.821(13) . ? S5 C7' 1.825(17) . ? S6 C6 1.751(6) . ? S6 C8' 1.760(18) . ? S6 C8 1.884(15) . ? C8 C8' 0.80(2) . ? C8 C7' 1.19(2) . ? C8 C7 1.64(2) . ? C8' C7 1.34(2) . ? C8' C7' 1.38(3) . ? C1 C2 1.338(11) . ? C1 C9A 1.360(15) . ? C2 C9B 1.329(18) . ? C3 C4 1.377(9) . ? C5 C6 1.320(8) . ? C7 C7' 0.87(2) . ? C9A N1A 1.130(19) . ? N1A N11B 1.017(19) . ? C9B N1B 1.20(2) . ? N1B N11A 0.99(2) . ? S11 C11 1.723(8) . ? S11 C13 1.734(7) . ? S12 C12 1.722(8) . ? S12 C13 1.745(7) . ? S13 C15 1.732(7) . ? S13 C14 1.733(7) . ? S14 C14 1.734(7) . ? S14 C16 1.745(7) . ? S15 C15 1.749(7) . ? S15 C17' 1.809(12) . ? S15 C17 1.85(2) . ? S16 C16 1.746(7) . ? S16 C18 1.756(18) . ? S16 C18' 1.873(13) . ? C11 C12 1.333(11) . ? C11 C19B 1.370(15) . ? C12 C19A 1.362(17) . ? C13 C14 1.368(9) . ? C15 C16 1.351(9) . ? C17 C17' 0.90(2) . ? C17 C18' 1.16(2) . ? C17 C18 1.45(3) . ? C18 C18' 0.83(2) . ? C18 C17' 1.31(2) . ? C17' C18' 1.57(2) . ? C19A N11A 1.16(2) . ? C19B N11B 1.132(19) . ? 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 2_556 . ? I4 I3 I4 180.000(1) 2 . ? C3 S1 C1 94.7(4) . . ? C2 S2 C3 93.9(4) . . ? C4 S3 C5 94.8(3) . . ? C4 S4 C6 95.0(3) . . ? C5 S5 C7 102.2(5) . . ? C5 S5 C7' 100.1(6) . . ? C7 S5 C7' 27.6(7) . . ? C6 S6 C8' 103.9(6) . . ? C6 S6 C8 96.9(5) . . ? C8' S6 C8 25.2(7) . . ? C8' C8 C7' 86(2) . . ? C8' C8 C7 54.9(18) . . ? C7' C8 C7 30.9(13) . . ? C8' C8 S6 68.8(19) . . ? C7' C8 S6 125.2(16) . . ? C7 C8 S6 103.8(12) . . ? C8 C8' C7 96(2) . . ? C8 C8' C7' 59(2) . . ? C7 C8' C7' 37.1(10) . . ? C8 C8' S6 86(2) . . ? C7 C8' S6 126.0(13) . . ? C7' C8' S6 121.4(16) . . ? C2 C1 C9A 116.2(8) . . ? C2 C1 S1 116.2(6) . . ? C9A C1 S1 127.5(8) . . ? C9B C2 C1 113.4(9) . . ? C9B C2 S2 127.4(9) . . ? C1 C2 S2 119.2(6) . . ? C4 C3 S1 122.7(5) . . ? C4 C3 S2 121.5(5) . . ? S1 C3 S2 115.8(4) . . ? C3 C4 S4 122.2(5) . . ? C3 C4 S3 122.3(5) . . ? S4 C4 S3 115.4(4) . . ? C6 C5 S5 128.4(5) . . ? C6 C5 S3 117.4(5) . . ? S5 C5 S3 114.1(4) . . ? C5 C6 S6 128.6(5) . . ? C5 C6 S4 117.2(5) . . ? S6 C6 S4 114.2(4) . . ? C7' C7 C8' 74(2) . . ? C7' C7 C8 44.7(16) . . ? C8' C7 C8 29.3(11) . . ? C7' C7 S5 76.5(16) . . ? C8' C7 S5 123.5(14) . . ? C8 C7 S5 104.1(11) . . ? C7 C7' C8 104(3) . . ? C7 C7' C8' 69(2) . . ? C8 C7' C8' 35.5(11) . . ? C7 C7' S5 75.9(16) . . ? C8 C7' S5 128.5(14) . . ? C8' C7' S5 120.9(16) . . ? N1A C9A C1 176.7(16) . . ? N11B N1A C9A 136(2) . . ? N1B C9B C2 176.2(16) . . ? N11A N1B C9B 141(2) . . ? C11 S11 C13 94.9(4) . . ? C12 S12 C13 93.9(4) . . ? C15 S13 C14 95.5(3) . . ? C14 S14 C16 95.2(3) . . ? C15 S15 C17' 103.6(4) . . ? C15 S15 C17 99.9(7) . . ? C17' S15 C17 28.4(7) . . ? C16 S16 C18 103.6(7) . . ? C16 S16 C18' 98.0(5) . . ? C18 S16 C18' 26.3(7) . . ? C12 C11 C19B 115.0(9) . . ? C12 C11 S11 116.9(5) . . ? C19B C11 S11 128.0(8) . . ? C11 C12 C19A 114.3(9) . . ? C11 C12 S12 118.7(5) . . ? C19A C12 S12 126.9(9) . . ? C14 C13 S11 122.8(5) . . ? C14 C13 S12 121.8(5) . . ? S11 C13 S12 115.4(4) . . ? C13 C14 S13 122.5(5) . . ? C13 C14 S14 122.2(5) . . ? S13 C14 S14 115.2(4) . . ? C16 C15 S13 117.2(5) . . ? C16 C15 S15 127.3(5) . . ? S13 C15 S15 115.5(4) . . ? C15 C16 S14 116.7(5) . . ? C15 C16 S16 128.6(5) . . ? S14 C16 S16 114.7(4) . . ? C17' C17 C18' 98(2) . . ? C17' C17 C18 63(2) . . ? C18' C17 C18 35.1(12) . . ? C17' C17 S15 73.0(16) . . ? C18' C17 S15 129.1(16) . . ? C18 C17 S15 114.4(17) . . ? C18' C18 C17' 91(2) . . ? C18' C18 C17 53(2) . . ? C17' C18 C17 37.6(10) . . ? C18' C18 S16 84.7(19) . . ? C17' C18 S16 129.3(14) . . ? C17 C18 S16 117.7(17) . . ? C17 C17' C18 79(2) . . ? C17 C17' C18' 47.0(16) . . ? C18 C17' C18' 32.1(11) . . ? C17 C17' S15 78.6(15) . . ? C18 C17' S15 125.3(13) . . ? C18' C17' S15 108.1(10) . . ? C18 C18' C17 92(3) . . ? C18 C18' C17' 57.1(18) . . ? C17 C18' C17' 34.6(14) . . ? C18 C18' S16 69.0(16) . . ? C17 C18' S16 128.2(16) . . ? C17' C18' S16 107.6(11) . . ? N11A C19A C12 175.9(17) . . ? N1B N11A C19A 143(2) . . ? N11B C19B C11 176.4(19) . . ? N1A N11B C19B 141(2) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.929 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.094 #===END data_tde120absm _database_code_CSD 170665 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-cyano -3',4'-ethylenedithiotetrathiafulvalene, tetrabromoindate (III) ; _chemical_name_common '(EDT-TTF-CN), InBr4' _chemical_melting_point ? _chemical_formula_moiety 'C9H5NS6, InBr4' _chemical_formula_sum 'C9 H5 Br4 In N S6' _chemical_formula_weight 753.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.3990(13) _cell_length_b 28.687(6) _cell_length_c 11.222(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.13(3) _cell_angle_gamma 90.00 _cell_volume 1978.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.3157 _exptl_crystal_size_mid 0.1156 _exptl_crystal_size_min 0.0770 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 9.894 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2170 _exptl_absorpt_correction_T_max 0.4950 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_type ?area_detector _diffrn_measurement_method 'rotation, phi incr. 0.8' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15693 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.90 _reflns_number_total 3702 _reflns_number_gt 2399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3702 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.771 _refine_ls_restrained_S_all 0.771 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.11188(6) 0.382465(12) 0.16858(3) 0.03926(10) Uani 1 1 d . . . Br2 Br 0.04789(10) 0.297203(19) 0.19284(5) 0.05321(16) Uani 1 1 d . . . Br3 Br 0.07599(9) 0.42515(2) 0.35581(5) 0.05227(16) Uani 1 1 d . . . Br4 Br 0.49635(10) 0.38553(2) 0.16063(7) 0.0722(2) Uani 1 1 d . . . Br5 Br -0.11543(11) 0.41825(3) -0.02487(5) 0.0688(2) Uani 1 1 d . . . S1 S -0.2643(2) 0.28373(5) 0.39880(12) 0.0463(3) Uani 1 1 d . . . S2 S -0.5766(2) 0.23531(5) 0.50231(13) 0.0501(4) Uani 1 1 d . . . S3 S 0.6464(2) 0.37880(5) 0.52622(12) 0.0447(3) Uani 1 1 d . . . S4 S 0.3080(2) 0.33353(4) 0.61063(12) 0.0421(3) Uani 1 1 d . . . S5 S 0.6327(2) 0.46739(5) 0.65331(13) 0.0524(4) Uani 1 1 d . . . S6 S 0.2222(3) 0.41246(5) 0.75600(13) 0.0560(4) Uani 1 1 d . . . C1 C -0.2893(8) 0.22332(17) 0.3799(4) 0.0393(12) Uani 1 1 d . . . C2 C -0.4327(9) 0.20221(18) 0.4257(4) 0.0465(13) Uani 1 1 d . . . H2 H -0.4551 0.1702 0.4168 0.056 Uiso 1 1 calc R . . C3 C -0.4528(8) 0.28709(16) 0.4822(4) 0.0365(11) Uani 1 1 d . . . C4 C 0.5010(8) 0.32902(16) 0.5316(4) 0.0378(12) Uani 1 1 d . . . C5 C 0.5349(8) 0.41066(16) 0.6239(4) 0.0374(12) Uani 1 1 d . . . C6 C 0.3752(8) 0.39006(16) 0.6636(4) 0.0379(12) Uani 1 1 d . . . C7 C 0.3951(11) 0.4930(2) 0.6824(6) 0.0651(17) Uani 1 1 d . . . H7A H 0.4220 0.5259 0.6998 0.078 Uiso 1 1 calc R . . H7B H 0.2745 0.4904 0.6079 0.078 Uiso 1 1 calc R . . C8 C 0.3318(10) 0.4713(2) 0.7869(5) 0.0628(17) Uani 1 1 d . . . H8A H 0.2237 0.4909 0.8080 0.075 Uiso 1 1 calc R . . H8B H 0.4584 0.4703 0.8585 0.075 Uiso 1 1 calc R . . C9 C -0.1509(10) 0.20041(17) 0.3184(5) 0.0473(14) Uani 1 1 d . . . N1 N -0.0366(9) 0.18364(17) 0.2680(5) 0.0670(14) Uani 1 1 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 In1 0.0375(2) 0.0383(2) 0.0442(2) -0.00113(17) 0.01496(16) 0.00021(17) Br2 0.0619(4) 0.0399(3) 0.0640(3) 0.0008(3) 0.0279(3) -0.0029(3) Br3 0.0518(3) 0.0549(4) 0.0497(3) -0.0111(3) 0.0137(3) 0.0050(3) Br4 0.0444(3) 0.0778(5) 0.1037(5) -0.0306(4) 0.0363(3) -0.0110(3) Br5 0.0698(4) 0.0856(5) 0.0534(3) 0.0224(3) 0.0209(3) 0.0162(4) S1 0.0549(8) 0.0337(7) 0.0610(8) -0.0050(6) 0.0338(7) -0.0020(6) S2 0.0549(9) 0.0420(8) 0.0620(8) -0.0045(7) 0.0308(7) -0.0092(7) S3 0.0494(8) 0.0371(7) 0.0550(8) -0.0006(6) 0.0268(7) -0.0018(6) S4 0.0449(8) 0.0372(7) 0.0506(7) -0.0025(6) 0.0236(6) -0.0013(6) S5 0.0618(9) 0.0331(7) 0.0625(9) -0.0013(6) 0.0177(7) -0.0031(7) S6 0.0679(10) 0.0493(9) 0.0621(9) -0.0098(7) 0.0369(8) 0.0029(7) C1 0.048(3) 0.032(3) 0.040(3) -0.008(2) 0.015(2) -0.003(2) C2 0.061(4) 0.034(3) 0.045(3) -0.007(2) 0.016(3) -0.001(3) C3 0.041(3) 0.030(3) 0.042(3) 0.000(2) 0.016(2) 0.001(2) C4 0.037(3) 0.033(3) 0.045(3) 0.002(2) 0.014(2) 0.002(2) C5 0.041(3) 0.028(3) 0.040(3) 0.001(2) 0.007(2) 0.001(2) C6 0.047(3) 0.034(3) 0.034(2) 0.000(2) 0.013(2) 0.006(2) C7 0.085(5) 0.033(3) 0.080(4) -0.007(3) 0.028(4) 0.008(3) C8 0.071(4) 0.050(4) 0.070(4) -0.015(3) 0.024(3) 0.008(3) C9 0.062(4) 0.026(3) 0.054(3) -0.006(2) 0.016(3) -0.004(3) N1 0.085(4) 0.040(3) 0.091(4) -0.013(3) 0.049(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 Br5 2.4755(10) . ? In1 Br4 2.4880(9) . ? In1 Br3 2.4969(7) . ? In1 Br2 2.5072(8) . ? S1 C3 1.723(5) . ? S1 C1 1.748(5) . ? S2 C2 1.711(5) . ? S2 C3 1.728(5) . ? S3 C4 1.715(5) . ? S3 C5 1.726(5) . ? S4 C4 1.713(5) . ? S4 C6 1.739(5) . ? S5 C5 1.742(5) . ? S5 C7 1.799(7) . ? S6 C6 1.735(5) . ? S6 C8 1.824(6) . ? C1 C2 1.317(7) . ? C1 C9 1.426(8) . ? C3 C4 1.390(6) 1_455 ? C4 C3 1.390(6) 1_655 ? C5 C6 1.358(7) . ? C7 C8 1.481(8) . ? C9 N1 1.147(7) . ? 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 Br5 In1 Br4 107.45(4) . . ? Br5 In1 Br3 111.44(3) . . ? Br4 In1 Br3 109.62(3) . . ? Br5 In1 Br2 115.21(3) . . ? Br4 In1 Br2 103.37(3) . . ? Br3 In1 Br2 109.34(3) . . ? C3 S1 C1 93.8(2) . . ? C2 S2 C3 94.7(3) . . ? C4 S3 C5 95.4(2) . . ? C4 S4 C6 95.8(2) . . ? C5 S5 C7 98.0(3) . . ? C6 S6 C8 101.8(3) . . ? C2 C1 C9 124.8(5) . . ? C2 C1 S1 117.3(4) . . ? C9 C1 S1 117.9(4) . . ? C1 C2 S2 118.1(4) . . ? C4 C3 S1 121.6(4) 1_455 . ? C4 C3 S2 122.4(4) 1_455 . ? S1 C3 S2 116.0(3) . . ? C3 C4 S4 122.4(4) 1_655 . ? C3 C4 S3 121.9(4) 1_655 . ? S4 C4 S3 115.6(3) . . ? C6 C5 S3 117.3(4) . . ? C6 C5 S5 127.4(4) . . ? S3 C5 S5 115.1(3) . . ? C5 C6 S6 129.5(4) . . ? C5 C6 S4 115.5(4) . . ? S6 C6 S4 115.0(3) . . ? C8 C7 S5 113.7(4) . . ? C7 C8 S6 114.5(4) . . ? N1 C9 C1 177.3(6) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.994 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.105 #===END data_tde41cm _database_code_CSD 170666 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-cyano -3',4'-ethylenedithiotetrathiafulvalene, tetrabromoferrate (III) ; _chemical_name_common 'EDT-TTF-CN, FeBr4' _chemical_melting_point ? _chemical_formula_moiety 'C9H5NS6, FeBr4' _chemical_formula_sum 'C9 H5 Br4 Fe N S6' _chemical_formula_weight 694.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.2930(13) _cell_length_b 28.506(6) _cell_length_c 11.126(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.52(3) _cell_angle_gamma 90.00 _cell_volume 1913.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.31 _cell_measurement_theta_max 17.89 _exptl_crystal_description 'prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 9.785 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.03499 _exptl_absorpt_correction_T_max 0.12123 _exptl_absorpt_process_details 'SHELXTL' _exptl_special_details ; ? ; _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_type 'Enraf Nonius CAD4' _diffrn_measurement_method w--2q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3859 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.97 _reflns_number_total 3757 _reflns_number_gt 2124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 [Harms, 1993)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3757 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.637 _refine_ls_restrained_S_all 1.637 _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 Fe1 Fe 0.11211(17) 0.38033(4) 0.16910(10) 0.0443(3) Uani 1 1 d . . . Br2 Br 0.04323(14) 0.30027(3) 0.18986(8) 0.0582(3) Uani 1 1 d . . . Br3 Br 0.07612(13) 0.42107(3) 0.34469(8) 0.0564(2) Uani 1 1 d . . . Br4 Br 0.47607(14) 0.38333(3) 0.16052(10) 0.0726(3) Uani 1 1 d . . . Br5 Br -0.11124(15) 0.41420(4) -0.01258(9) 0.0713(3) Uani 1 1 d . . . S1 S -0.2633(3) 0.28517(7) 0.3983(2) 0.0507(5) Uani 1 1 d . . . S2 S -0.5836(3) 0.23781(7) 0.5021(2) 0.0526(5) Uani 1 1 d . . . C1 C -0.2917(12) 0.2250(2) 0.3783(7) 0.0417(18) Uani 1 1 d . . . C2 C -0.4408(12) 0.2038(3) 0.4231(7) 0.0472(19) Uani 1 1 d . . . H2 H -0.4673 0.1718 0.4123 0.057 Uiso 1 1 calc R . . C3 C -0.4555(11) 0.2893(2) 0.4807(7) 0.0422(18) Uani 1 1 d . . . C9 C -0.1501(12) 0.2007(3) 0.3181(7) 0.0470(19) Uani 1 1 d . . . N1 N -0.0350(12) 0.1833(2) 0.2693(7) 0.065(2) Uani 1 1 d . . . S3 S -0.3492(3) 0.38129(7) 0.52785(19) 0.0465(5) Uani 1 1 d . . . S4 S -0.6955(3) 0.33599(7) 0.61070(19) 0.0463(5) Uani 1 1 d . . . S5 S -0.3583(4) 0.46978(7) 0.6584(2) 0.0579(6) Uani 1 1 d . . . S6 S -0.7776(4) 0.41513(7) 0.7596(2) 0.0612(6) Uani 1 1 d . . . C4 C -0.4973(10) 0.3307(2) 0.5303(6) 0.0351(17) Uani 1 1 d . . . C5 C -0.4601(11) 0.4136(2) 0.6287(7) 0.0421(18) Uani 1 1 d . . . C6 C -0.6247(11) 0.3920(2) 0.6645(7) 0.0410(18) Uani 1 1 d . . . C7 C -0.6003(14) 0.4966(3) 0.6868(9) 0.067(3) Uani 1 1 d . . . H7A H -0.5693 0.5295 0.7070 0.081 Uiso 1 1 calc R . . H7B H -0.7224 0.4950 0.6106 0.081 Uiso 1 1 calc R . . C8 C -0.6685(15) 0.4738(3) 0.7906(9) 0.069(3) Uani 1 1 d . . . H8A H -0.7801 0.4933 0.8107 0.082 Uiso 1 1 calc R . . H8B H -0.5411 0.4728 0.8642 0.082 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 Fe1 0.0426(6) 0.0481(6) 0.0461(7) -0.0007(6) 0.0188(5) -0.0005(5) Br2 0.0670(5) 0.0516(5) 0.0623(6) -0.0004(4) 0.0288(4) -0.0045(4) Br3 0.0571(5) 0.0621(5) 0.0519(5) -0.0090(4) 0.0188(4) 0.0058(4) Br4 0.0517(5) 0.0789(6) 0.0979(8) -0.0249(6) 0.0383(5) -0.0102(5) Br5 0.0741(6) 0.0888(7) 0.0531(6) 0.0184(5) 0.0215(5) 0.0136(5) S1 0.0572(12) 0.0451(11) 0.0599(14) -0.0075(10) 0.0329(11) -0.0027(10) S2 0.0611(13) 0.0457(12) 0.0602(14) -0.0069(11) 0.0322(11) -0.0094(10) C1 0.058(5) 0.026(4) 0.044(5) 0.001(4) 0.020(4) 0.005(4) C2 0.056(5) 0.046(5) 0.036(4) -0.005(4) 0.007(4) -0.002(4) C3 0.042(4) 0.041(4) 0.049(5) 0.002(4) 0.020(4) 0.010(3) C9 0.044(4) 0.051(5) 0.041(5) 0.005(4) 0.004(4) 0.000(4) N1 0.081(5) 0.048(4) 0.083(6) -0.003(4) 0.052(5) 0.009(4) S3 0.0488(11) 0.0428(11) 0.0537(13) -0.0012(10) 0.0238(10) -0.0009(9) S4 0.0527(12) 0.0436(11) 0.0501(13) -0.0042(10) 0.0268(10) 0.0000(9) S5 0.0673(14) 0.0428(12) 0.0671(16) -0.0034(11) 0.0247(12) -0.0045(10) S6 0.0754(14) 0.0560(13) 0.0646(15) -0.0105(12) 0.0402(12) 0.0020(12) C4 0.027(3) 0.053(5) 0.026(4) 0.011(3) 0.009(3) 0.006(3) C5 0.040(4) 0.047(4) 0.040(4) 0.004(4) 0.011(3) 0.000(4) C6 0.039(4) 0.050(5) 0.031(4) -0.005(4) 0.007(3) 0.006(3) C7 0.081(6) 0.038(5) 0.090(8) -0.004(5) 0.036(6) 0.005(4) C8 0.084(7) 0.056(5) 0.076(7) -0.022(5) 0.039(5) 0.004(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 Fe1 Br5 2.3190(15) . ? Fe1 Br4 2.3209(14) . ? Fe1 Br3 2.3383(14) . ? Fe1 Br2 2.3467(14) . ? Br2 N1 3.518(7) . ? S1 C3 1.717(7) . ? S1 C1 1.732(7) . ? S2 C2 1.722(7) . ? S2 C3 1.724(7) . ? C1 C2 1.327(9) . ? C1 C9 1.436(10) . ? C3 C4 1.358(9) . ? C9 N1 1.136(9) . ? S3 C4 1.722(7) . ? S3 C5 1.743(8) . ? S4 C6 1.720(7) . ? S4 C4 1.736(7) . ? S5 C5 1.722(7) . ? S5 C7 1.810(8) . ? S6 C6 1.748(7) . ? S6 C8 1.802(8) . ? C5 C6 1.358(10) . ? C7 C8 1.492(11) . ? 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 Br5 Fe1 Br4 108.02(6) . . ? Br5 Fe1 Br3 110.05(6) . . ? Br4 Fe1 Br3 110.32(6) . . ? Br5 Fe1 Br2 114.05(6) . . ? Br4 Fe1 Br2 104.59(5) . . ? Br3 Fe1 Br2 109.65(5) . . ? Fe1 Br2 N1 171.48(13) . . ? C3 S1 C1 94.3(4) . . ? C2 S2 C3 94.4(4) . . ? C2 C1 C9 123.7(7) . . ? C2 C1 S1 117.4(6) . . ? C9 C1 S1 118.9(6) . . ? C1 C2 S2 117.6(6) . . ? C4 C3 S1 121.6(5) . . ? C4 C3 S2 122.0(5) . . ? S1 C3 S2 116.3(4) . . ? N1 C9 C1 177.0(9) . . ? C9 N1 Br2 82.0(5) . . ? C4 S3 C5 96.6(3) . . ? C6 S4 C4 96.2(3) . . ? C5 S5 C7 98.1(4) . . ? C6 S6 C8 102.7(4) . . ? C3 C4 S3 123.5(5) . . ? C3 C4 S4 122.4(5) . . ? S3 C4 S4 114.0(4) . . ? C6 C5 S5 129.6(6) . . ? C6 C5 S3 115.4(6) . . ? S5 C5 S3 114.8(4) . . ? C5 C6 S4 117.5(6) . . ? C5 C6 S6 127.2(6) . . ? S4 C6 S6 115.3(4) . . ? C8 C7 S5 113.1(6) . . ? C7 C8 S6 115.7(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.931 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.197 #===END data_tde297absm _database_code_CSD 170667 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3-cyano -3',4'-ethylenedithiotetrathiafulvalene, tetrabromoaurate (III) ; _chemical_name_common 'EDT-TTF-CN, AuBr4' _chemical_melting_point ? _chemical_formula_moiety 'C9H5NS6, AuBr4' _chemical_formula_sum 'C9 H5 Au Br4 N S6' _chemical_formula_weight 836.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7596(16) _cell_length_b 8.3250(17) _cell_length_c 16.245(3) _cell_angle_alpha 93.98(3) _cell_angle_beta 93.63(3) _cell_angle_gamma 114.98(3) _cell_volume 944.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5982 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.75 _exptl_crystal_description 'prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 16.911 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0943 _exptl_absorpt_correction_T_max 0.2197 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_type area_detector _diffrn_measurement_method 'rotation, phi incr. 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9269 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.83 _reflns_number_total 3409 _reflns_number_gt 2363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^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 3409 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _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 Au1 Au 0.5000 0.0000 0.5000 0.03117(18) Uani 1 2 d S . . Br1 Br 0.5065(2) 0.28600(17) 0.47430(9) 0.0518(4) Uani 1 1 d . . . Br2 Br 0.81297(17) 0.09041(17) 0.45325(9) 0.0506(4) Uani 1 1 d . . . Au2 Au 0.5000 0.5000 0.0000 0.03242(19) Uani 1 2 d S . . Br3 Br 0.2748(2) 0.4100(2) 0.10230(10) 0.0651(4) Uani 1 1 d . . . Br4 Br 0.5814(3) 0.2564(2) 0.02325(11) 0.0718(5) Uani 1 1 d . . . S1 S -0.0013(4) 0.5695(4) 0.3817(2) 0.0457(8) Uani 1 1 d . . . S2 S -0.3152(4) 0.4296(4) 0.2490(2) 0.0447(8) Uani 1 1 d . . . S3 S 0.1372(4) 0.2701(4) 0.3116(2) 0.0390(7) Uani 1 1 d . . . S4 S -0.1881(4) 0.1311(4) 0.1868(2) 0.0466(8) Uani 1 1 d . . . S5 S 0.2638(5) -0.0124(5) 0.2668(2) 0.0481(8) Uani 1 1 d . . . S6 S -0.1216(5) -0.1678(5) 0.1184(3) 0.0767(15) Uani 1 1 d . . . C1 C -0.1521(17) 0.6708(16) 0.3771(9) 0.044(3) Uani 1 1 d . . . H1 H -0.1350 0.7657 0.4155 0.053 Uiso 1 1 calc R . . C2 C -0.2957(16) 0.6089(15) 0.3162(8) 0.039(3) Uani 1 1 d . . . C3 C -0.1188(16) 0.4170(15) 0.2965(7) 0.036(3) Uani 1 1 d . . . C4 C -0.0604(16) 0.2879(15) 0.2688(8) 0.038(3) Uani 1 1 d . . . C5 C 0.1011(15) 0.0758(15) 0.2509(8) 0.038(3) Uani 1 1 d . . . C6 C -0.0526(17) 0.0142(16) 0.1919(8) 0.043(3) Uani 1 1 d . . . C7 C 0.255(2) -0.110(3) 0.1632(9) 0.068(5) Uani 1 1 d . . . C8 C 0.068(3) -0.241(3) 0.1286(15) 0.058(8) Uiso 0.74(5) 1 d P . . C80 C 0.097(7) -0.148(8) 0.096(4) 0.05(2) Uiso 0.26(5) 1 d P . . C9 C -0.4292(18) 0.6793(17) 0.3040(8) 0.048(3) Uani 1 1 d . . . N1 N -0.5399(19) 0.7370(19) 0.2915(9) 0.074(4) Uani 1 1 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 Au1 0.0354(3) 0.0291(3) 0.0307(4) 0.0000(3) 0.0008(3) 0.0163(3) Br1 0.0672(8) 0.0391(7) 0.0596(9) 0.0122(6) 0.0120(7) 0.0311(6) Br2 0.0416(6) 0.0442(7) 0.0654(9) -0.0016(7) 0.0136(6) 0.0177(5) Au2 0.0377(3) 0.0341(3) 0.0252(3) 0.0006(3) 0.0029(3) 0.0156(3) Br3 0.0777(10) 0.0625(9) 0.0614(10) 0.0161(8) 0.0397(8) 0.0304(8) Br4 0.1134(13) 0.0786(11) 0.0627(10) 0.0291(9) 0.0329(9) 0.0723(10) S1 0.0435(16) 0.0414(17) 0.055(2) -0.0080(16) -0.0053(15) 0.0245(14) S2 0.0493(17) 0.0445(18) 0.0477(19) -0.0044(15) -0.0032(15) 0.0298(15) S3 0.0405(15) 0.0403(16) 0.0402(17) -0.0040(14) -0.0005(13) 0.0230(13) S4 0.0453(16) 0.0457(18) 0.054(2) -0.0085(16) -0.0075(15) 0.0286(14) S5 0.0557(19) 0.0521(19) 0.050(2) -0.0016(16) -0.0001(16) 0.0380(16) S6 0.055(2) 0.062(2) 0.106(3) -0.046(2) -0.027(2) 0.0319(19) C1 0.049(7) 0.028(6) 0.059(9) 0.001(6) 0.006(7) 0.020(5) C2 0.042(6) 0.026(6) 0.053(8) 0.008(6) 0.011(6) 0.017(5) C3 0.043(6) 0.036(6) 0.031(6) 0.004(5) 0.005(5) 0.019(5) C4 0.040(6) 0.034(6) 0.040(7) 0.005(5) 0.006(5) 0.018(5) C5 0.039(6) 0.029(6) 0.053(8) 0.009(6) 0.015(6) 0.019(5) C6 0.047(7) 0.030(6) 0.046(8) -0.006(6) 0.006(6) 0.011(5) C7 0.073(10) 0.109(13) 0.038(8) -0.012(9) 0.005(8) 0.056(10) C9 0.052(7) 0.047(7) 0.051(8) -0.007(6) 0.000(6) 0.031(6) N1 0.080(8) 0.087(10) 0.076(9) -0.005(8) -0.006(7) 0.061(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 Au1 Br2 2.4103(15) 2_656 ? Au1 Br2 2.4103(15) . ? Au1 Br1 2.4259(14) . ? Au1 Br1 2.4259(14) 2_656 ? Au2 Br3 2.4106(17) . ? Au2 Br3 2.4106(17) 2_665 ? Au2 Br4 2.4107(15) 2_665 ? Au2 Br4 2.4107(15) . ? S1 C1 1.708(12) . ? S1 C3 1.726(11) . ? S2 C3 1.711(11) . ? S2 C2 1.734(12) . ? S3 C4 1.711(11) . ? S3 C5 1.741(12) . ? S4 C6 1.711(13) . ? S4 C4 1.720(12) . ? S5 C5 1.722(11) . ? S5 C7 1.801(14) . ? S6 C80 1.70(5) . ? S6 C6 1.729(12) . ? S6 C8 1.82(2) . ? C1 C2 1.338(16) . ? C2 C9 1.400(16) . ? C3 C4 1.390(15) . ? C5 C6 1.369(16) . ? C7 C8 1.44(2) . ? C7 C80 1.50(5) . ? C8 C80 0.92(6) . ? C9 N1 1.161(16) . ? 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 Au1 Br2 180.0 2_656 . ? Br2 Au1 Br1 89.87(6) 2_656 . ? Br2 Au1 Br1 90.13(6) . . ? Br2 Au1 Br1 90.13(6) 2_656 2_656 ? Br2 Au1 Br1 89.87(6) . 2_656 ? Br1 Au1 Br1 180.0 . 2_656 ? Br3 Au2 Br3 180.0 . 2_665 ? Br3 Au2 Br4 89.75(6) . 2_665 ? Br3 Au2 Br4 90.25(6) 2_665 2_665 ? Br3 Au2 Br4 90.25(6) . . ? Br3 Au2 Br4 89.75(6) 2_665 . ? Br4 Au2 Br4 180.0 2_665 . ? C1 S1 C3 94.6(6) . . ? C3 S2 C2 94.3(5) . . ? C4 S3 C5 96.4(5) . . ? C6 S4 C4 95.9(5) . . ? C5 S5 C7 100.1(7) . . ? C80 S6 C6 99.7(18) . . ? C80 S6 C8 30(2) . . ? C6 S6 C8 105.2(8) . . ? C2 C1 S1 117.7(9) . . ? C1 C2 C9 124.3(11) . . ? C1 C2 S2 117.0(9) . . ? C9 C2 S2 118.7(9) . . ? C4 C3 S2 121.5(8) . . ? C4 C3 S1 122.1(8) . . ? S2 C3 S1 116.4(7) . . ? C3 C4 S3 124.2(9) . . ? C3 C4 S4 120.8(8) . . ? S3 C4 S4 115.1(7) . . ? C6 C5 S5 127.0(9) . . ? C6 C5 S3 114.8(9) . . ? S5 C5 S3 118.2(7) . . ? C5 C6 S4 117.7(9) . . ? C5 C6 S6 126.7(10) . . ? S4 C6 S6 115.6(7) . . ? C8 C7 C80 36(2) . . ? C8 C7 S5 114.7(14) . . ? C80 C7 S5 124(2) . . ? C80 C8 C7 75(4) . . ? C80 C8 S6 68(4) . . ? C7 C8 S6 117.3(16) . . ? C8 C80 C7 68(4) . . ? C8 C80 S6 82(4) . . ? C7 C80 S6 121(4) . . ? N1 C9 C2 178.2(15) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 2.534 _refine_diff_density_min -3.349 _refine_diff_density_rms 0.322 #===END data_tde5absm _database_code_CSD 170668 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis (3-cyano -3',4'-ethylenedithiotetrathiafulvalene), hexabromo-octa-mu3-bromohexamolybdate (II), acetonitrile solvate ; _chemical_name_common '(EDT-TTF-CN)2, Mo6Br14, (CH3CN)4' _chemical_melting_point ? _chemical_formula_moiety '2(C9H5NS6), Mo6Br14, 4(C2H3N1)' _chemical_formula_sum 'C26 H22 Br14 Mo6 N6 S12' _chemical_formula_weight 2497.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.191(2) _cell_length_b 11.443(2) _cell_length_c 13.372(3) _cell_angle_alpha 102.05(3) _cell_angle_beta 103.82(3) _cell_angle_gamma 93.63(3) _cell_volume 1470.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.95 _exptl_crystal_description 'plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.308 _exptl_crystal_size_mid 0.2118 _exptl_crystal_size_min 0.0424 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 _exptl_absorpt_coefficient_mu 11.210 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1169 _exptl_absorpt_correction_T_max 0.6212 _exptl_absorpt_process_details 'FACEIT, Stoe-IPDS' _exptl_special_details ; ? ; _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_type area_detector _diffrn_measurement_method 'rotation, phi incr. 1.5' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17757 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 28.12 _reflns_number_total 6538 _reflns_number_gt 3838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6538 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 0.709 _refine_ls_restrained_S_all 0.709 _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 Mo1 Mo 0.07834(4) 0.87576(4) 0.05470(3) 0.02504(10) Uani 1 1 d . . . Mo2 Mo -0.02433(4) 1.07090(4) 0.13197(3) 0.02479(10) Uani 1 1 d . . . Mo3 Mo 0.17112(4) 1.08812(4) 0.03509(3) 0.02474(10) Uani 1 1 d . . . Br1 Br 0.18557(7) 0.70103(6) 0.12915(5) 0.05034(16) Uani 1 1 d . . . Br2 Br -0.06331(7) 1.16363(6) 0.31421(4) 0.04553(15) Uani 1 1 d . . . Br3 Br 0.40866(6) 1.21219(5) 0.07992(4) 0.04187(14) Uani 1 1 d . . . Br4 Br 0.22209(5) 1.03616(5) 0.22024(4) 0.03639(13) Uani 1 1 d . . . Br5 Br 0.26979(5) 0.89539(5) -0.04071(4) 0.03372(12) Uani 1 1 d . . . Br6 Br -0.07104(5) 0.71992(5) -0.11222(4) 0.03413(13) Uani 1 1 d . . . Br7 Br -0.11411(6) 0.86127(5) 0.14982(4) 0.03578(13) Uani 1 1 d . . . S1 S -0.57223(17) 1.28051(14) 0.46915(11) 0.0468(4) Uani 1 1 d . . . S2 S -0.74753(16) 1.45933(15) 0.40218(11) 0.0469(4) Uani 1 1 d . . . S3 S -0.36756(15) 1.36421(13) 0.33411(10) 0.0414(3) Uani 1 1 d . . . S4 S -0.55443(15) 1.53120(14) 0.26825(11) 0.0437(4) Uani 1 1 d . . . S5 S -0.17242(18) 1.42074(15) 0.21707(13) 0.0549(4) Uani 1 1 d . . . S6 S -0.40287(17) 1.62056(14) 0.13353(12) 0.0496(4) Uani 1 1 d . . . C1 C -0.7214(7) 1.2926(6) 0.5117(4) 0.0495(16) Uani 1 1 d . . . C2 C -0.8006(7) 1.3741(6) 0.4810(4) 0.0478(15) Uani 1 1 d . . . C3 C -0.6012(6) 1.3913(5) 0.3985(4) 0.0411(14) Uani 1 1 d . . . C4 C -0.5154(6) 1.4241(5) 0.3405(4) 0.0408(14) Uani 1 1 d . . . C5 C -0.3221(6) 1.4500(5) 0.2510(4) 0.0370(13) Uani 1 1 d . . . C6 C -0.4115(6) 1.5276(5) 0.2200(4) 0.0395(13) Uani 1 1 d . . . C7 C -0.1498(7) 1.5386(6) 0.1485(5) 0.0562(17) Uani 1 1 d . . . H7A H -0.1172 1.6143 0.2001 0.067 Uiso 1 1 calc R . . H7B H -0.0812 1.5203 0.1102 0.067 Uiso 1 1 calc R . . C8 C -0.2809(6) 1.5523(6) 0.0715(4) 0.0527(17) Uani 1 1 d . . . H8A H -0.3216 1.4734 0.0284 0.063 Uiso 1 1 calc R . . H8B H -0.2591 1.6005 0.0246 0.063 Uiso 1 1 calc R . . C9A C -0.7701(12) 1.2155(11) 0.5694(8) 0.051(3) Uani 0.550(7) 1 d P . . N1A N -0.8167(14) 1.1494(10) 0.6131(8) 0.071(4) Uani 0.550(7) 1 d P . . C9B C -0.9088(13) 1.3920(12) 0.5116(9) 0.038(3) Uani 0.450(7) 1 d P . . N1B N -1.0005(15) 1.4158(12) 0.5420(9) 0.064(4) Uani 0.450(7) 1 d P . . C10 C 0.5718(8) 0.9666(8) 0.2295(6) 0.083(2) Uani 1 1 d . . . H10A H 0.5195 1.0310 0.2155 0.124 Uiso 1 1 calc R . . H10B H 0.5548 0.9039 0.1662 0.124 Uiso 1 1 calc R . . H10C H 0.6669 0.9964 0.2522 0.124 Uiso 1 1 calc R . . C11 C 0.5327(9) 0.9189(8) 0.3122(7) 0.081(2) Uani 1 1 d . . . N2 N 0.5003(9) 0.8834(10) 0.3741(7) 0.144(4) Uani 1 1 d . . . C12A C -1.164(2) 1.1093(18) 0.5587(14) 0.077(6) Uiso 0.550(7) 1 d P . . C13A C -1.1216(14) 1.2421(13) 0.5738(9) 0.063(4) Uiso 0.550(7) 1 d P . . N3A N -1.0772(13) 1.3397(13) 0.5756(9) 0.083(4) Uiso 0.550(7) 1 d P . . C12B C -1.180(2) 1.147(2) 0.5754(17) 0.077(7) Uiso 0.450(7) 1 d P . . C13B C -1.035(3) 1.1405(19) 0.5886(15) 0.091(6) Uiso 0.450(7) 1 d P . . N3B N -0.920(3) 1.1510(17) 0.6092(13) 0.099(6) Uiso 0.450(7) 1 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 Mo1 0.0240(2) 0.0252(2) 0.0268(2) 0.00683(17) 0.00682(17) 0.00573(19) Mo2 0.0241(2) 0.0265(2) 0.0241(2) 0.00428(17) 0.00782(16) 0.00392(19) Mo3 0.0205(2) 0.0262(2) 0.0268(2) 0.00445(17) 0.00634(16) 0.00266(18) Br1 0.0555(4) 0.0461(4) 0.0568(4) 0.0240(3) 0.0140(3) 0.0226(3) Br2 0.0580(4) 0.0479(4) 0.0302(3) 0.0013(2) 0.0181(2) 0.0031(3) Br3 0.0265(3) 0.0420(3) 0.0527(3) 0.0065(3) 0.0075(2) -0.0030(3) Br4 0.0313(3) 0.0442(3) 0.0305(3) 0.0085(2) 0.0017(2) 0.0052(3) Br5 0.0265(3) 0.0365(3) 0.0398(3) 0.0066(2) 0.0123(2) 0.0091(2) Br6 0.0345(3) 0.0273(3) 0.0395(3) 0.0024(2) 0.0123(2) 0.0035(2) Br7 0.0381(3) 0.0361(3) 0.0375(3) 0.0122(2) 0.0150(2) 0.0037(3) S1 0.0529(10) 0.0408(9) 0.0491(8) 0.0148(7) 0.0139(7) 0.0049(8) S2 0.0419(9) 0.0523(10) 0.0489(8) 0.0156(7) 0.0119(7) 0.0090(8) S3 0.0434(9) 0.0375(8) 0.0447(8) 0.0135(6) 0.0097(6) 0.0078(7) S4 0.0424(9) 0.0436(9) 0.0507(8) 0.0180(7) 0.0145(7) 0.0123(7) S5 0.0542(11) 0.0465(10) 0.0771(11) 0.0232(8) 0.0306(8) 0.0195(8) S6 0.0551(11) 0.0445(9) 0.0597(9) 0.0238(7) 0.0223(7) 0.0149(8) C1 0.056(4) 0.047(4) 0.037(3) 0.002(3) 0.008(3) -0.007(3) C2 0.047(4) 0.046(4) 0.047(3) 0.008(3) 0.011(3) -0.008(3) C3 0.042(4) 0.040(3) 0.038(3) 0.007(2) 0.006(2) 0.002(3) C4 0.043(4) 0.039(3) 0.040(3) 0.011(3) 0.008(2) 0.000(3) C5 0.045(4) 0.026(3) 0.040(3) 0.004(2) 0.013(2) 0.004(3) C6 0.042(4) 0.035(3) 0.042(3) 0.011(2) 0.011(2) 0.004(3) C7 0.059(5) 0.041(4) 0.082(4) 0.023(3) 0.036(4) 0.011(3) C8 0.068(5) 0.042(4) 0.056(4) 0.017(3) 0.026(3) 0.012(3) C9A 0.049(8) 0.050(8) 0.053(7) 0.019(6) 0.003(5) 0.017(6) N1A 0.082(9) 0.081(8) 0.076(7) 0.065(7) 0.028(6) 0.031(7) C9B 0.025(8) 0.041(8) 0.050(7) 0.009(6) 0.018(6) -0.005(6) N1B 0.065(10) 0.053(9) 0.067(8) 0.002(6) 0.019(7) -0.003(7) C10 0.062(5) 0.100(7) 0.107(6) 0.046(5) 0.038(4) 0.035(5) C11 0.068(6) 0.095(7) 0.085(6) 0.044(5) 0.013(4) 0.010(5) N2 0.110(7) 0.216(11) 0.152(8) 0.128(8) 0.042(6) 0.033(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Br7 2.5942(10) . ? Mo1 Br5 2.5957(9) . ? Mo1 Br1 2.6021(10) . ? Mo1 Br4 2.6131(14) . ? Mo1 Br6 2.6173(14) . ? Mo1 Mo2 2.6323(8) 2_575 ? Mo1 Mo3 2.6377(10) 2_575 ? Mo1 Mo3 2.6383(9) . ? Mo1 Mo2 2.6451(10) . ? Mo2 Br2 2.5804(10) . ? Mo2 Br7 2.5910(10) . ? Mo2 Br5 2.5992(10) 2_575 ? Mo2 Br4 2.6007(10) . ? Mo2 Br6 2.6144(10) 2_575 ? Mo2 Mo3 2.6269(13) 2_575 ? Mo2 Mo1 2.6323(8) 2_575 ? Mo2 Mo3 2.6407(9) . ? Mo3 Br5 2.5953(10) . ? Mo3 Br7 2.5964(9) 2_575 ? Mo3 Br3 2.5982(11) . ? Mo3 Br6 2.6016(10) 2_575 ? Mo3 Br4 2.6063(9) . ? Mo3 Mo2 2.6269(13) 2_575 ? Mo3 Mo1 2.6376(10) 2_575 ? Br5 Mo2 2.5992(10) 2_575 ? Br6 Mo3 2.6016(10) 2_575 ? Br6 Mo2 2.6144(10) 2_575 ? Br7 Mo3 2.5964(9) 2_575 ? S1 C3 1.732(5) . ? S1 C1 1.750(7) . ? S2 C2 1.729(6) . ? S2 C3 1.732(6) . ? S3 C4 1.707(6) . ? S3 C5 1.748(5) . ? S4 C4 1.722(5) . ? S4 C6 1.727(6) . ? S5 C5 1.726(6) . ? S5 C7 1.815(6) . ? S6 C6 1.740(5) . ? S6 C8 1.786(6) . ? C1 C2 1.336(8) . ? C1 C9A 1.426(13) . ? C2 C9B 1.278(14) . ? C3 C4 1.382(8) . ? C5 C6 1.366(7) . ? C7 C8 1.519(8) . ? C9A N1A 1.187(15) . ? C9A N3B 1.89(3) . ? N1A N3B 1.05(2) . ? C9B N1B 1.132(17) . ? N1B N3A 1.347(17) . ? C10 C11 1.454(10) . ? C11 N2 1.102(10) . ? C12A C13B 1.29(3) . ? C12A C13A 1.51(3) . ? C13A N3A 1.172(17) . ? C13A C12B 1.21(3) . ? C13A C13B 1.52(2) . ? C12B C13B 1.45(3) . ? C13B N3B 1.12(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 Br7 Mo1 Br5 178.65(3) . . ? Br7 Mo1 Br1 90.70(3) . . ? Br5 Mo1 Br1 90.56(3) . . ? Br7 Mo1 Br4 89.47(3) . . ? Br5 Mo1 Br4 90.01(3) . . ? Br1 Mo1 Br4 91.60(3) . . ? Br7 Mo1 Br6 89.85(3) . . ? Br5 Mo1 Br6 90.63(3) . . ? Br1 Mo1 Br6 90.05(3) . . ? Br4 Mo1 Br6 178.22(3) . . ? Br7 Mo1 Mo2 119.64(3) . 2_575 ? Br5 Mo1 Mo2 59.62(3) . 2_575 ? Br1 Mo1 Mo2 134.56(3) . 2_575 ? Br4 Mo1 Mo2 119.29(3) . 2_575 ? Br6 Mo1 Mo2 59.74(3) . 2_575 ? Br7 Mo1 Mo3 59.50(2) . 2_575 ? Br5 Mo1 Mo3 119.76(3) . 2_575 ? Br1 Mo1 Mo3 134.60(3) . 2_575 ? Br4 Mo1 Mo3 118.92(4) . 2_575 ? Br6 Mo1 Mo3 59.35(3) . 2_575 ? Mo2 Mo1 Mo3 60.14(3) 2_575 2_575 ? Br7 Mo1 Mo3 119.24(3) . . ? Br5 Mo1 Mo3 59.45(3) . . ? Br1 Mo1 Mo3 135.61(3) . . ? Br4 Mo1 Mo3 59.51(3) . . ? Br6 Mo1 Mo3 119.52(3) . . ? Mo2 Mo1 Mo3 59.79(3) 2_575 . ? Mo3 Mo1 Mo3 89.79(3) 2_575 . ? Br7 Mo1 Mo2 59.27(3) . . ? Br5 Mo1 Mo2 119.42(3) . . ? Br1 Mo1 Mo2 135.62(3) . . ? Br4 Mo1 Mo2 59.28(3) . . ? Br6 Mo1 Mo2 118.99(3) . . ? Mo2 Mo1 Mo2 89.82(3) 2_575 . ? Mo3 Mo1 Mo2 59.64(3) 2_575 . ? Mo3 Mo1 Mo2 59.97(2) . . ? Br2 Mo2 Br7 88.94(4) . . ? Br2 Mo2 Br5 89.82(4) . 2_575 ? Br7 Mo2 Br5 90.34(4) . 2_575 ? Br2 Mo2 Br4 91.11(4) . . ? Br7 Mo2 Br4 89.81(4) . . ? Br5 Mo2 Br4 179.06(3) 2_575 . ? Br2 Mo2 Br6 92.08(4) . 2_575 ? Br7 Mo2 Br6 178.60(3) . 2_575 ? Br5 Mo2 Br6 90.62(4) 2_575 2_575 ? Br4 Mo2 Br6 89.21(4) . 2_575 ? Br2 Mo2 Mo3 133.27(3) . 2_575 ? Br7 Mo2 Mo3 59.68(3) . 2_575 ? Br5 Mo2 Mo3 59.55(3) 2_575 2_575 ? Br4 Mo2 Mo3 119.79(4) . 2_575 ? Br6 Mo2 Mo3 120.06(3) 2_575 2_575 ? Br2 Mo2 Mo1 135.43(3) . 2_575 ? Br7 Mo2 Mo1 119.89(4) . 2_575 ? Br5 Mo2 Mo1 59.49(3) 2_575 2_575 ? Br4 Mo2 Mo1 119.66(3) . 2_575 ? Br6 Mo2 Mo1 59.85(3) 2_575 2_575 ? Mo3 Mo2 Mo1 60.22(3) 2_575 2_575 ? Br2 Mo2 Mo3 136.75(3) . . ? Br7 Mo2 Mo3 119.27(3) . . ? Br5 Mo2 Mo3 119.51(3) 2_575 . ? Br4 Mo2 Mo3 59.63(2) . . ? Br6 Mo2 Mo3 59.35(3) 2_575 . ? Mo3 Mo2 Mo3 89.97(3) 2_575 . ? Mo1 Mo2 Mo3 60.03(3) 2_575 . ? Br2 Mo2 Mo1 134.35(3) . . ? Br7 Mo2 Mo1 59.39(2) . . ? Br5 Mo2 Mo1 119.59(4) 2_575 . ? Br4 Mo2 Mo1 59.75(4) . . ? Br6 Mo2 Mo1 119.23(3) 2_575 . ? Mo3 Mo2 Mo1 60.04(3) 2_575 . ? Mo1 Mo2 Mo1 90.18(3) 2_575 . ? Mo3 Mo2 Mo1 59.89(3) . . ? Br5 Mo3 Br7 90.31(3) . 2_575 ? Br5 Mo3 Br3 90.33(4) . . ? Br7 Mo3 Br3 89.41(4) 2_575 . ? Br5 Mo3 Br6 179.40(3) . 2_575 ? Br7 Mo3 Br6 90.15(3) 2_575 2_575 ? Br3 Mo3 Br6 90.07(4) . 2_575 ? Br5 Mo3 Br4 90.17(3) . . ? Br7 Mo3 Br4 178.62(3) 2_575 . ? Br3 Mo3 Br4 91.89(4) . . ? Br6 Mo3 Br4 89.37(3) 2_575 . ? Br5 Mo3 Mo2 59.69(3) . 2_575 ? Br7 Mo3 Mo2 59.47(3) 2_575 2_575 ? Br3 Mo3 Mo2 133.92(3) . 2_575 ? Br6 Mo3 Mo2 120.26(3) 2_575 2_575 ? Br4 Mo3 Mo2 119.75(3) . 2_575 ? Br5 Mo3 Mo1 120.01(4) . 2_575 ? Br7 Mo3 Mo1 59.42(3) 2_575 2_575 ? Br3 Mo3 Mo1 133.98(3) . 2_575 ? Br6 Mo3 Mo1 59.94(3) 2_575 2_575 ? Br4 Mo3 Mo1 119.25(3) . 2_575 ? Mo2 Mo3 Mo1 60.32(3) 2_575 2_575 ? Br5 Mo3 Mo1 59.46(2) . . ? Br7 Mo3 Mo1 119.46(4) 2_575 . ? Br3 Mo3 Mo1 135.79(3) . . ? Br6 Mo3 Mo1 119.96(3) 2_575 . ? Br4 Mo3 Mo1 59.76(3) . . ? Mo2 Mo3 Mo1 59.99(3) 2_575 . ? Mo1 Mo3 Mo1 90.21(4) 2_575 . ? Br5 Mo3 Mo2 119.60(3) . . ? Br7 Mo3 Mo2 119.24(3) 2_575 . ? Br3 Mo3 Mo2 136.03(3) . . ? Br6 Mo3 Mo2 59.82(3) 2_575 . ? Br4 Mo3 Mo2 59.42(3) . . ? Mo2 Mo3 Mo2 90.03(3) 2_575 . ? Mo1 Mo3 Mo2 59.83(2) 2_575 . ? Mo1 Mo3 Mo2 60.14(3) . . ? Mo2 Br4 Mo3 60.95(3) . . ? Mo2 Br4 Mo1 60.97(3) . . ? Mo3 Br4 Mo1 60.73(3) . . ? Mo3 Br5 Mo1 61.10(3) . . ? Mo3 Br5 Mo2 60.76(4) . 2_575 ? Mo1 Br5 Mo2 60.89(2) . 2_575 ? Mo3 Br6 Mo2 60.83(2) 2_575 2_575 ? Mo3 Br6 Mo1 60.71(3) 2_575 . ? Mo2 Br6 Mo1 60.42(3) 2_575 . ? Mo2 Br7 Mo1 61.34(3) . . ? Mo2 Br7 Mo3 60.85(4) . 2_575 ? Mo1 Br7 Mo3 61.08(3) . 2_575 ? C3 S1 C1 94.1(3) . . ? C2 S2 C3 94.9(3) . . ? C4 S3 C5 96.0(3) . . ? C4 S4 C6 96.0(3) . . ? C5 S5 C7 101.3(3) . . ? C6 S6 C8 99.6(3) . . ? C2 C1 C9A 117.5(7) . . ? C2 C1 S1 117.5(5) . . ? C9A C1 S1 124.7(6) . . ? C9B C2 C1 121.7(8) . . ? C9B C2 S2 120.9(7) . . ? C1 C2 S2 117.4(5) . . ? C4 C3 S2 120.7(4) . . ? C4 C3 S1 123.2(4) . . ? S2 C3 S1 116.2(3) . . ? C3 C4 S3 124.0(4) . . ? C3 C4 S4 120.4(4) . . ? S3 C4 S4 115.5(3) . . ? C6 C5 S5 129.4(4) . . ? C6 C5 S3 115.7(4) . . ? S5 C5 S3 114.9(3) . . ? C5 C6 S4 116.7(4) . . ? C5 C6 S6 128.0(5) . . ? S4 C6 S6 115.2(3) . . ? C8 C7 S5 112.3(5) . . ? C7 C8 S6 114.1(4) . . ? N1A C9A C1 176.5(12) . . ? N1A C9A N3B 29.9(8) . . ? C1 C9A N3B 147.5(10) . . ? N3B N1A C9A 115.7(14) . . ? N1B C9B C2 175.2(15) . . ? C9B N1B N3A 124.4(14) . . ? N2 C11 C10 178.5(10) . . ? C13B C12A C13A 65.3(14) . . ? N3A C13A C12B 173(2) . . ? N3A C13A C12A 170.3(16) . . ? C12B C13A C12A 16.7(15) . . ? N3A C13A C13B 123.7(16) . . ? C12B C13A C13B 63.0(16) . . ? C12A C13A C13B 50.3(11) . . ? C13A N3A N1B 151.0(15) . . ? C13A C12B C13B 69.0(17) . . ? N3B C13B C12A 170(3) . . ? N3B C13B C12B 170(3) . . ? C12A C13B C12B 19.6(15) . . ? N3B C13B C13A 125(2) . . ? C12A C13B C13A 64.4(15) . . ? C12B C13B C13A 48.0(12) . . ? N1A N3B C13B 168(2) . . ? N1A N3B C9A 34.4(9) . . ? C13B N3B C9A 142.1(18) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.576 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.118 #===END data_tde18absm _database_code_CSD 170669 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis (3-cyano -3',4'-ethylenedithiotetrathiafulvalene), hexabromo-octa-mu3-chlorohexamolybdate (II), acetonitrile solvate ; _chemical_name_common '(EDT-TTF-CN)2, Mo6Cl8Br6, (CH3CN)4' _chemical_melting_point ? _chemical_formula_moiety '2(C9H5NS6), Mo6Cl8Br6, 4(C2H3N1)' _chemical_formula_sum 'C13 H11 Br3 Cl4 Mo3 N3 S6' _chemical_formula_weight 1070.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9799(10) _cell_length_b 11.3713(10) _cell_length_c 13.3427(10) _cell_angle_alpha 101.938(10) _cell_angle_beta 104.094(10) _cell_angle_gamma 93.366(10) _cell_volume 1427.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.773 _cell_measurement_theta_max 11.589 _exptl_crystal_description 'plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 6.322 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.514 _exptl_absorpt_process_details 'SHELXTL' _exptl_special_details ; ? ; _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_type 'Enraf Nonius CAD4' _diffrn_measurement_method w--2q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6520 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.1265 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5531 _reflns_number_gt 2926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 [Harms, 1993)' _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 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5531 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1705 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1788 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _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 Mo1 Mo 0.41922(13) 0.12401(11) 0.44698(9) 0.0274(3) Uani 1 1 d . . . Mo2 Mo 0.32765(13) -0.08826(11) 0.46504(9) 0.0272(3) Uani 1 1 d . . . Mo3 Mo 0.47678(13) 0.06838(11) 0.63171(9) 0.0271(3) Uani 1 1 d . . . Br1 Br 0.3081(2) 0.29814(16) 0.37426(14) 0.0509(5) Uani 1 1 d . . . Br2 Br 0.08772(17) -0.21214(15) 0.42071(14) 0.0451(4) Uani 1 1 d . . . Br3 Br 0.4388(2) 0.15790(16) 0.81377(12) 0.0486(5) Uani 1 1 d . . . Cl1 Cl 0.2386(4) 0.0975(3) 0.5410(3) 0.0361(8) Uani 1 1 d . . . Cl2 Cl 0.5671(4) 0.2662(3) 0.6088(3) 0.0365(9) Uani 1 1 d . . . Cl3 Cl 0.6078(4) 0.1361(3) 0.3587(3) 0.0334(8) Uani 1 1 d . . . Cl4 Cl 0.2815(4) -0.0325(3) 0.2920(3) 0.0365(8) Uani 1 1 d . . . S1 S -0.2492(5) 0.4554(4) 0.9013(4) 0.0473(11) Uani 1 1 d . . . S2 S -0.0664(5) 0.2781(4) 0.9699(3) 0.0460(10) Uani 1 1 d . . . S3 S -0.0530(5) 0.5288(4) 0.7674(3) 0.0443(10) Uani 1 1 d . . . S4 S 0.1412(5) 0.3629(4) 0.8349(3) 0.0426(10) Uani 1 1 d . . . S5 S 0.0992(5) 0.6194(4) 0.6325(4) 0.0490(11) Uani 1 1 d . . . S6 S 0.3364(5) 0.4204(4) 0.7171(4) 0.0554(12) Uani 1 1 d . . . C1 C -0.2975(15) 0.3678(14) 0.9796(12) 0.035(3) Uani 1 1 d . . . C2 C -0.2139(17) 0.2880(13) 1.0132(12) 0.037(4) Uani 1 1 d . . . C3 C -0.0992(18) 0.3864(15) 0.8980(13) 0.047(4) Uani 1 1 d . . . C4 C -0.0120(15) 0.4226(13) 0.8416(12) 0.034(3) Uani 1 1 d . . . C5 C 0.0950(17) 0.5280(13) 0.7203(11) 0.035(4) Uani 1 1 d . . . C6 C 0.1826(17) 0.4488(13) 0.7485(12) 0.042(4) Uani 1 1 d . . . C7 C 0.226(2) 0.5549(17) 0.5720(15) 0.062(5) Uani 1 1 d . . . H7A H 0.1869 0.4759 0.5271 0.074 Uiso 1 1 calc R . . H7B H 0.2497 0.6056 0.5270 0.074 Uiso 1 1 calc R . . C8 C 0.355(2) 0.5418(17) 0.6504(14) 0.058(5) Uani 1 1 d . . . H8A H 0.3843 0.6173 0.7033 0.070 Uiso 1 1 calc R . . H8B H 0.4281 0.5272 0.6143 0.070 Uiso 1 1 calc R . . C9B C -0.262(4) 0.220(3) 1.076(3) 0.039(9) Uiso 0.44(2) 1 d P . . N1B N -0.310(5) 0.145(3) 1.115(3) 0.061(10) Uiso 0.44(2) 1 d P . . C9A C -0.401(3) 0.379(3) 1.011(2) 0.045(8) Uiso 0.56(2) 1 d P . . N1A N -0.507(4) 0.405(3) 1.039(3) 0.077(10) Uiso 0.56(2) 1 d P . . C12A C -0.657(5) 0.137(4) 1.085(4) 0.065(13) Uiso 0.56(2) 1 d P . . C13A C -0.511(5) 0.139(4) 1.096(3) 0.083(13) Uiso 0.56(2) 1 d P . . N3A N -0.393(6) 0.153(4) 1.126(3) 0.101(13) Uiso 0.56(2) 1 d P . . C12B C -0.690(6) 0.105(5) 1.054(5) 0.067(17) Uiso 0.44(2) 1 d P . . C13B C -0.631(4) 0.236(4) 1.071(3) 0.047(10) Uiso 0.44(2) 1 d P . . N3B N -0.582(4) 0.341(3) 1.076(3) 0.060(11) Uiso 0.44(2) 1 d P . . C10 C 0.072(2) 0.9588(19) 0.7260(16) 0.073(6) Uani 1 1 d . . . H10A H 0.0778 0.8904 0.6721 0.110 Uiso 1 1 calc R . . H10B H 0.1601 1.0076 0.7528 0.110 Uiso 1 1 calc R . . H10C H 0.0025 1.0061 0.6962 0.110 Uiso 1 1 calc R . . C11 C 0.036(2) 0.920(2) 0.8058(17) 0.077(7) Uani 1 1 d . . . N2 N -0.003(2) 0.885(2) 0.8692(19) 0.113(8) Uani 1 1 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 Mo1 0.0249(7) 0.0308(7) 0.0280(6) 0.0107(5) 0.0057(5) 0.0074(5) Mo2 0.0242(6) 0.0307(7) 0.0261(6) 0.0075(5) 0.0038(5) 0.0061(5) Mo3 0.0283(7) 0.0321(7) 0.0219(6) 0.0063(5) 0.0073(5) 0.0076(5) Br1 0.0549(11) 0.0495(10) 0.0554(10) 0.0277(8) 0.0109(9) 0.0222(9) Br2 0.0318(9) 0.0479(10) 0.0519(10) 0.0117(8) 0.0056(7) -0.0016(7) Br3 0.0630(12) 0.0531(10) 0.0299(8) 0.0048(7) 0.0162(8) 0.0070(9) Cl1 0.032(2) 0.043(2) 0.0380(19) 0.0108(16) 0.0136(16) 0.0163(17) Cl2 0.038(2) 0.0320(19) 0.040(2) 0.0065(15) 0.0114(17) 0.0080(16) Cl3 0.0326(19) 0.040(2) 0.0306(18) 0.0128(15) 0.0106(15) 0.0044(16) Cl4 0.033(2) 0.046(2) 0.0301(18) 0.0125(16) 0.0021(16) 0.0110(17) S1 0.039(2) 0.059(3) 0.051(3) 0.021(2) 0.015(2) 0.020(2) S2 0.048(3) 0.048(2) 0.050(2) 0.022(2) 0.018(2) 0.014(2) S3 0.041(2) 0.050(2) 0.047(2) 0.0238(19) 0.007(2) 0.019(2) S4 0.045(2) 0.040(2) 0.046(2) 0.0175(18) 0.010(2) 0.0149(19) S5 0.060(3) 0.052(3) 0.051(2) 0.025(2) 0.030(2) 0.024(2) S6 0.046(3) 0.051(3) 0.078(3) 0.022(2) 0.022(2) 0.020(2) C1 0.020(7) 0.044(9) 0.044(9) 0.012(7) 0.012(7) -0.006(7) C2 0.045(10) 0.026(8) 0.036(8) -0.006(6) 0.015(7) 0.011(7) C3 0.050(11) 0.045(9) 0.039(9) 0.011(7) -0.007(8) 0.009(8) C4 0.027(8) 0.036(8) 0.045(9) 0.031(7) 0.004(7) 0.002(6) C5 0.052(10) 0.039(8) 0.032(8) 0.027(7) 0.021(7) 0.022(8) C6 0.049(10) 0.029(8) 0.047(9) 0.002(7) 0.022(8) 0.000(7) C7 0.058(13) 0.061(12) 0.061(12) 0.015(10) -0.001(10) 0.026(10) C8 0.061(13) 0.072(13) 0.059(11) 0.019(10) 0.047(10) 0.007(10) C10 0.062(14) 0.094(17) 0.070(14) 0.020(12) 0.025(11) 0.024(12) C11 0.075(16) 0.13(2) 0.058(12) 0.055(13) 0.039(12) 0.040(15) N2 0.051(12) 0.18(2) 0.108(18) 0.059(17) 0.007(12) -0.003(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 Mo1 Cl3 2.463(4) . ? Mo1 Cl1 2.471(4) . ? Mo1 Cl4 2.477(4) . ? Mo1 Cl2 2.486(4) . ? Mo1 Br1 2.573(2) . ? Mo1 Mo2 2.6074(17) 2_656 ? Mo1 Mo3 2.6083(17) . ? Mo1 Mo2 2.6093(18) . ? Mo1 Mo3 2.6102(17) 2_656 ? Mo2 Cl1 2.460(4) . ? Mo2 Cl4 2.463(4) . ? Mo2 Cl3 2.465(4) 2_656 ? Mo2 Cl2 2.469(4) 2_656 ? Mo2 Br2 2.576(2) . ? Mo2 Mo3 2.6022(17) . ? Mo2 Mo1 2.6074(17) 2_656 ? Mo2 Mo3 2.6120(18) 2_656 ? Mo3 Cl3 2.466(4) 2_656 ? Mo3 Cl1 2.466(4) . ? Mo3 Cl4 2.472(4) 2_656 ? Mo3 Cl2 2.479(4) . ? Mo3 Br3 2.5594(19) . ? Mo3 Mo1 2.6102(17) 2_656 ? Mo3 Mo2 2.6121(18) 2_656 ? Cl2 Mo2 2.469(4) 2_656 ? Cl3 Mo2 2.465(4) 2_656 ? Cl3 Mo3 2.466(4) 2_656 ? Cl4 Mo3 2.472(4) 2_656 ? S1 C1 1.713(15) . ? S1 C3 1.736(18) . ? S2 C2 1.709(16) . ? S2 C3 1.712(17) . ? S3 C4 1.721(13) . ? S3 C5 1.740(16) . ? S4 C4 1.723(15) . ? S4 C6 1.762(16) . ? S5 C5 1.727(13) . ? S5 C7 1.777(19) . ? S6 C6 1.718(16) . ? S6 C8 1.814(18) . ? C1 C9A 1.21(3) . ? C1 C2 1.34(2) . ? C2 C9B 1.40(4) . ? C3 C4 1.38(2) . ? C5 C6 1.34(2) . ? C7 C8 1.48(2) . ? C9B N1B 1.22(5) . ? C9B N3A 1.80(6) . ? N1B N3A 0.88(5) . ? N1B C13A 1.96(6) . ? C9A N1A 1.24(4) . ? N1A N3B 1.27(4) . ? C12A C12B 0.52(7) . ? C12A C13B 1.20(5) . ? C12A C13A 1.43(6) . ? C13A N3A 1.14(6) . ? C13A C13B 1.69(6) . ? C13A C12B 1.73(8) . ? C12B C13B 1.53(7) . ? C13B N3B 1.24(5) . ? C10 C11 1.35(3) . ? C11 N2 1.14(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 Cl3 Mo1 Cl1 175.19(13) . . ? Cl3 Mo1 Cl4 90.07(13) . . ? Cl1 Mo1 Cl4 89.52(13) . . ? Cl3 Mo1 Cl2 89.70(13) . . ? Cl1 Mo1 Cl2 90.29(13) . . ? Cl4 Mo1 Cl2 174.91(13) . . ? Cl3 Mo1 Br1 92.23(10) . . ? Cl1 Mo1 Br1 92.57(10) . . ? Cl4 Mo1 Br1 93.07(10) . . ? Cl2 Mo1 Br1 92.02(10) . . ? Cl3 Mo1 Mo2 58.08(9) . 2_656 ? Cl1 Mo1 Mo2 118.10(10) . 2_656 ? Cl4 Mo1 Mo2 117.88(10) . 2_656 ? Cl2 Mo1 Mo2 57.94(9) . 2_656 ? Br1 Mo1 Mo2 134.65(7) . 2_656 ? Cl3 Mo1 Mo3 118.17(10) . . ? Cl1 Mo1 Mo3 58.02(9) . . ? Cl4 Mo1 Mo3 117.67(10) . . ? Cl2 Mo1 Mo3 58.19(9) . . ? Br1 Mo1 Mo3 134.74(7) . . ? Mo2 Mo1 Mo3 60.11(5) 2_656 . ? Cl3 Mo1 Mo2 118.11(10) . . ? Cl1 Mo1 Mo2 57.85(9) . . ? Cl4 Mo1 Mo2 57.86(9) . . ? Cl2 Mo1 Mo2 118.00(10) . . ? Br1 Mo1 Mo2 135.44(7) . . ? Mo2 Mo1 Mo2 89.91(5) 2_656 . ? Mo3 Mo1 Mo2 59.83(5) . . ? Cl3 Mo1 Mo3 58.07(9) . 2_656 ? Cl1 Mo1 Mo3 117.89(10) . 2_656 ? Cl4 Mo1 Mo3 58.08(9) . 2_656 ? Cl2 Mo1 Mo3 117.76(10) . 2_656 ? Br1 Mo1 Mo3 135.31(7) . 2_656 ? Mo2 Mo1 Mo3 59.83(5) 2_656 2_656 ? Mo3 Mo1 Mo3 89.94(5) . 2_656 ? Mo2 Mo1 Mo3 60.06(5) . 2_656 ? Cl1 Mo2 Cl4 90.08(13) . . ? Cl1 Mo2 Cl3 90.09(13) . 2_656 ? Cl4 Mo2 Cl3 175.56(14) . 2_656 ? Cl1 Mo2 Cl2 175.98(14) . 2_656 ? Cl4 Mo2 Cl2 89.47(13) . 2_656 ? Cl3 Mo2 Cl2 90.05(13) 2_656 2_656 ? Cl1 Mo2 Br2 91.88(11) . . ? Cl4 Mo2 Br2 93.46(11) . . ? Cl3 Mo2 Br2 90.97(10) 2_656 . ? Cl2 Mo2 Br2 92.13(11) 2_656 . ? Cl1 Mo2 Mo3 58.23(10) . . ? Cl4 Mo2 Mo3 118.43(11) . . ? Cl3 Mo2 Mo3 58.16(9) 2_656 . ? Cl2 Mo2 Mo3 118.68(10) 2_656 . ? Br2 Mo2 Mo3 133.77(7) . . ? Cl1 Mo2 Mo1 118.35(10) . 2_656 ? Cl4 Mo2 Mo1 118.17(11) . 2_656 ? Cl3 Mo2 Mo1 58.03(9) 2_656 2_656 ? Cl2 Mo2 Mo1 58.56(10) 2_656 2_656 ? Br2 Mo2 Mo1 134.14(7) . 2_656 ? Mo3 Mo2 Mo1 60.14(5) . 2_656 ? Cl1 Mo2 Mo1 58.24(10) . . ? Cl4 Mo2 Mo1 58.38(10) . . ? Cl3 Mo2 Mo1 118.20(10) 2_656 . ? Cl2 Mo2 Mo1 118.31(11) 2_656 . ? Br2 Mo2 Mo1 135.74(7) . . ? Mo3 Mo2 Mo1 60.06(5) . . ? Mo1 Mo2 Mo1 90.10(5) 2_656 . ? Cl1 Mo2 Mo3 118.22(11) . 2_656 ? Cl4 Mo2 Mo3 58.22(10) . 2_656 ? Cl3 Mo2 Mo3 117.97(10) 2_656 2_656 ? Cl2 Mo2 Mo3 58.33(10) 2_656 2_656 ? Br2 Mo2 Mo3 136.18(7) . 2_656 ? Mo3 Mo2 Mo3 90.04(5) . 2_656 ? Mo1 Mo2 Mo3 59.96(5) 2_656 2_656 ? Mo1 Mo2 Mo3 59.99(5) . 2_656 ? Cl3 Mo3 Cl1 89.93(13) 2_656 . ? Cl3 Mo3 Cl4 90.13(13) 2_656 2_656 ? Cl1 Mo3 Cl4 175.25(13) . 2_656 ? Cl3 Mo3 Cl2 175.36(13) 2_656 . ? Cl1 Mo3 Cl2 90.54(13) . . ? Cl4 Mo3 Cl2 89.02(13) 2_656 . ? Cl3 Mo3 Br3 90.76(10) 2_656 . ? Cl1 Mo3 Br3 91.56(10) . . ? Cl4 Mo3 Br3 93.19(10) 2_656 . ? Cl2 Mo3 Br3 93.84(10) . . ? Cl3 Mo3 Mo2 58.13(9) 2_656 . ? Cl1 Mo3 Mo2 58.00(9) . . ? Cl4 Mo3 Mo2 118.27(10) 2_656 . ? Cl2 Mo3 Mo2 118.50(10) . . ? Br3 Mo3 Mo2 133.26(7) . . ? Cl3 Mo3 Mo1 118.21(10) 2_656 . ? Cl1 Mo3 Mo1 58.19(9) . . ? Cl4 Mo3 Mo1 117.80(10) 2_656 . ? Cl2 Mo3 Mo1 58.43(9) . . ? Br3 Mo3 Mo1 135.53(7) . . ? Mo2 Mo3 Mo1 60.10(5) . . ? Cl3 Mo3 Mo1 57.98(9) 2_656 2_656 ? Cl1 Mo3 Mo1 118.01(10) . 2_656 ? Cl4 Mo3 Mo1 58.26(9) 2_656 2_656 ? Cl2 Mo3 Mo1 117.90(10) . 2_656 ? Br3 Mo3 Mo1 134.37(7) . 2_656 ? Mo2 Mo3 Mo1 60.03(5) . 2_656 ? Mo1 Mo3 Mo1 90.05(5) . 2_656 ? Cl3 Mo3 Mo2 117.92(10) 2_656 2_656 ? Cl1 Mo3 Mo2 118.09(10) . 2_656 ? Cl4 Mo3 Mo2 57.88(9) 2_656 2_656 ? Cl2 Mo3 Mo2 57.95(9) . 2_656 ? Br3 Mo3 Mo2 136.78(7) . 2_656 ? Mo2 Mo3 Mo2 89.96(5) . 2_656 ? Mo1 Mo3 Mo2 59.93(5) . 2_656 ? Mo1 Mo3 Mo2 59.96(5) 2_656 2_656 ? Mo2 Cl1 Mo3 63.77(9) . . ? Mo2 Cl1 Mo1 63.90(9) . . ? Mo3 Cl1 Mo1 63.79(10) . . ? Mo2 Cl2 Mo3 63.72(9) 2_656 . ? Mo2 Cl2 Mo1 63.50(9) 2_656 . ? Mo3 Cl2 Mo1 63.38(9) . . ? Mo1 Cl3 Mo2 63.89(9) . 2_656 ? Mo1 Cl3 Mo3 63.95(10) . 2_656 ? Mo2 Cl3 Mo3 63.71(10) 2_656 2_656 ? Mo2 Cl4 Mo3 63.91(10) . 2_656 ? Mo2 Cl4 Mo1 63.76(9) . . ? Mo3 Cl4 Mo1 63.65(10) 2_656 . ? C1 S1 C3 92.8(8) . . ? C2 S2 C3 94.8(8) . . ? C4 S3 C5 96.7(7) . . ? C4 S4 C6 95.5(7) . . ? C5 S5 C7 99.9(8) . . ? C6 S6 C8 99.3(8) . . ? C9A C1 C2 118(2) . . ? C9A C1 S1 122.8(19) . . ? C2 C1 S1 119.3(12) . . ? C1 C2 C9B 115.2(19) . . ? C1 C2 S2 116.3(12) . . ? C9B C2 S2 128.4(18) . . ? C4 C3 S2 123.6(13) . . ? C4 C3 S1 119.7(12) . . ? S2 C3 S1 116.7(11) . . ? C3 C4 S3 121.5(12) . . ? C3 C4 S4 123.7(11) . . ? S3 C4 S4 114.7(8) . . ? C6 C5 S5 128.7(13) . . ? C6 C5 S3 116.1(11) . . ? S5 C5 S3 114.8(8) . . ? C5 C6 S6 129.7(13) . . ? C5 C6 S4 116.8(12) . . ? S6 C6 S4 113.4(10) . . ? C8 C7 S5 112.9(13) . . ? C7 C8 S6 114.0(14) . . ? N1B C9B C2 169(4) . . ? N1B C9B N3A 26(2) . . ? C2 C9B N3A 155(3) . . ? N3A N1B C9B 117(6) . . ? N3A N1B C13A 16(4) . . ? C9B N1B C13A 114(3) . . ? C1 C9A N1A 171(4) . . ? C9A N1A N3B 127(4) . . ? C12B C12A C13B 119(10) . . ? C12B C12A C13A 118(10) . . ? C13B C12A C13A 80(4) . . ? N3A C13A C12A 166(5) . . ? N3A C13A C13B 132(5) . . ? C12A C13A C13B 44(3) . . ? N3A C13A C12B 175(5) . . ? C12A C13A C12B 15(3) . . ? C13B C13A C12B 53(3) . . ? N3A C13A N1B 12(3) . . ? C12A C13A N1B 179(4) . . ? C13B C13A N1B 135(3) . . ? C12B C13A N1B 166(3) . . ? N1B N3A C13A 151(7) . . ? N1B N3A C9B 37(4) . . ? C13A N3A C9B 132(4) . . ? C12A C12B C13B 44(9) . . ? C12A C12B C13A 47(9) . . ? C13B C12B C13A 62(3) . . ? C12A C13B N3B 167(5) . . ? C12A C13B C12B 17(3) . . ? N3B C13B C12B 174(4) . . ? C12A C13B C13A 56(3) . . ? N3B C13B C13A 115(4) . . ? C12B C13B C13A 65(3) . . ? C13B N3B N1A 145(4) . . ? N2 C11 C10 175(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.798 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.287