#------------------------------------------------------------------------------ #$Date: 2014-07-11 19:31:04 +0200 (Fri, 11 Jul 2014) $ #$Revision: 120073 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001489.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4001489 loop_ _publ_author_name 'Herv\'e, Katel' 'Cador, Olivier' 'Golhen, St\'ephane' 'Costuas, Karine' 'Halet, Jean-Fran\,cois' 'Shirahata, Takashi' 'Muto, Tsuyoshi' 'Imakubo, Tatsuro' 'Miyazaki, Akira' 'Ouahab, Lahc\`ene' _publ_section_title ; Iodine Substituted Tetrathiafulvalene Radical Cation Salts with [M(isoq)2(NCS)4]-Anions where M = CrIII, GaIII:  Role of I···S and S···S Contacts on Structural and Magnetic Properties ; _journal_issue 3 _journal_name_full 'Chemistry of Materials' _journal_page_first 790 _journal_volume 18 _journal_year 2006 _chemical_formula_sum 'C38 H22 Ga I4 N6 S16' _chemical_formula_weight 1652.90 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 101.2200(10) _cell_angle_beta 96.7190(10) _cell_angle_gamma 97.5770(10) _cell_formula_units_Z 1 _cell_length_a 10.6730(3) _cell_length_b 11.3330(3) _cell_length_c 11.4010(4) _cell_measurement_reflns_used 5826 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 0.998 _cell_volume 1326.35(7) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10802 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.87 _exptl_absorpt_coefficient_mu 3.513 _exptl_absorpt_correction_type none _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 791 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _refine_diff_density_max 2.877 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.144 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 295 _refine_ls_number_reflns 6054 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0514 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.4557P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1308 _refine_ls_wR_factor_ref 0.1530 _reflns_number_gt 3962 _reflns_number_total 6054 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cm052199qsi20051128_120741.cif _[local]_cod_data_source_block 3b _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'None' changed to 'none' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4001489 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Ga Ga 0.0000 0.0000 0.0000 0.0403(2) Uani 1 2 d S C1 C -0.0822(7) 0.0227(6) 0.2418(6) 0.0442(15) Uani 1 1 d . H1 H 0.0025 0.0598 0.2656 0.053 Uiso 1 1 calc R C2 C -0.1637(6) 0.0151(6) 0.3333(6) 0.0443(15) Uani 1 1 d . C3 C -0.1191(7) 0.0670(7) 0.4541(7) 0.0543(17) Uani 1 1 d . H3 H -0.0361 0.1086 0.4781 0.065 Uiso 1 1 calc R C4 C -0.2025(8) 0.0549(7) 0.5395(7) 0.063(2) Uani 1 1 d . H4 H -0.1748 0.0880 0.6212 0.075 Uiso 1 1 calc R C5 C -0.3281(8) -0.0077(8) 0.5005(8) 0.064(2) Uani 1 1 d . H5 H -0.3822 -0.0163 0.5576 0.076 Uiso 1 1 calc R C6 C -0.3727(8) -0.0559(7) 0.3814(8) 0.062(2) Uani 1 1 d . H6 H -0.4565 -0.0953 0.3578 0.075 Uiso 1 1 calc R C7 C -0.2902(7) -0.0454(6) 0.2941(6) 0.0467(16) Uani 1 1 d . C8 C -0.3306(7) -0.0923(6) 0.1681(7) 0.0513(17) Uani 1 1 d . H8 H -0.4136 -0.1323 0.1398 0.062 Uiso 1 1 calc R C9 C -0.2465(7) -0.0777(6) 0.0903(7) 0.0500(16) Uani 1 1 d . H9 H -0.2740 -0.1079 0.0081 0.060 Uiso 1 1 calc R C10 C -0.2054(6) 0.1308(6) -0.1213(6) 0.0432(14) Uani 1 1 d . C11 C -0.1071(6) -0.2643(6) -0.1555(6) 0.0426(14) Uani 1 1 d . C12 C -0.6972(7) -0.3262(6) 0.6090(6) 0.0472(16) Uani 1 1 d . C13 C -0.5975(7) -0.2861(6) 0.6925(6) 0.0478(15) Uani 1 1 d . C14 C -0.5027(7) -0.3410(6) 0.4963(6) 0.0509(16) Uani 1 1 d . C15 C -0.4238(7) -0.3597(6) 0.4098(6) 0.0496(16) Uani 1 1 d . C16 C -0.3282(7) -0.3902(6) 0.2107(6) 0.0513(17) Uani 1 1 d . C17 C -0.2284(7) -0.3475(6) 0.2970(6) 0.0474(16) Uani 1 1 d . C18 C -0.1661(8) -0.4682(8) 0.0672(7) 0.066(2) Uani 1 1 d . H18A H -0.1677 -0.5346 0.1097 0.079 Uiso 1 1 calc R H18B H -0.1483 -0.4990 -0.0136 0.079 Uiso 1 1 calc R C19 C -0.0585(8) -0.3685(9) 0.1312(8) 0.072(2) Uani 1 1 d . H19A H -0.0555 -0.3031 0.0874 0.087 Uiso 1 1 calc R H19B H 0.0213 -0.4004 0.1277 0.087 Uiso 1 1 calc R I1 I -0.88707(4) -0.36062(4) 0.63891(4) 0.05180(16) Uani 1 1 d . I2 I -0.60341(5) -0.23619(5) 0.87729(4) 0.05936(17) Uani 1 1 d . S1 S -0.3052(2) 0.2162(2) -0.16349(19) 0.0675(6) Uani 1 1 d . S2 S -0.1530(2) -0.39912(18) -0.23907(19) 0.0643(5) Uani 1 1 d . S3 S -0.66830(19) -0.37226(18) 0.46000(16) 0.0554(5) Uani 1 1 d . S4 S -0.44647(19) -0.28340(19) 0.64814(17) 0.0593(5) Uani 1 1 d . S5 S -0.47866(18) -0.41936(18) 0.25743(17) 0.0541(4) Uani 1 1 d . S6 S -0.25734(19) -0.33127(17) 0.44750(16) 0.0534(4) Uani 1 1 d . S7 S -0.3218(2) -0.42411(19) 0.05532(18) 0.0611(5) Uani 1 1 d . S8 S -0.0683(2) -0.3064(2) 0.2843(2) 0.0688(6) Uani 1 1 d . N1 N -0.1227(5) -0.0206(5) 0.1263(5) 0.0420(12) Uani 1 1 d . N2 N -0.1333(6) 0.0708(5) -0.0924(5) 0.0520(14) Uani 1 1 d . N3 N -0.0742(6) -0.1674(5) -0.0950(5) 0.0532(15) 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 Ga 0.0472(6) 0.0407(5) 0.0336(5) 0.0046(4) 0.0107(4) 0.0094(4) C1 0.052(4) 0.041(3) 0.041(4) 0.007(3) 0.013(3) 0.008(3) C2 0.051(4) 0.040(3) 0.046(4) 0.008(3) 0.018(3) 0.015(3) C3 0.052(4) 0.065(4) 0.048(4) 0.009(3) 0.015(3) 0.014(4) C4 0.080(6) 0.070(5) 0.041(4) 0.005(4) 0.019(4) 0.022(4) C5 0.063(5) 0.076(5) 0.063(5) 0.020(4) 0.038(4) 0.017(4) C6 0.062(5) 0.065(5) 0.068(5) 0.017(4) 0.029(4) 0.016(4) C7 0.052(4) 0.041(3) 0.051(4) 0.007(3) 0.018(3) 0.015(3) C8 0.038(4) 0.059(4) 0.052(4) 0.004(3) 0.004(3) 0.003(3) C9 0.046(4) 0.053(4) 0.047(4) 0.000(3) 0.006(3) 0.009(3) C10 0.045(4) 0.054(4) 0.030(3) 0.006(3) 0.009(3) 0.008(3) C11 0.041(4) 0.047(4) 0.040(3) 0.008(3) 0.012(3) 0.007(3) C12 0.055(4) 0.047(4) 0.043(4) 0.008(3) 0.017(3) 0.017(3) C13 0.054(4) 0.054(4) 0.035(3) 0.006(3) 0.011(3) 0.008(3) C14 0.067(5) 0.052(4) 0.034(3) 0.006(3) 0.011(3) 0.011(3) C15 0.057(4) 0.046(4) 0.046(4) 0.005(3) 0.012(3) 0.012(3) C16 0.060(4) 0.051(4) 0.042(4) 0.006(3) 0.012(3) 0.006(3) C17 0.055(4) 0.049(4) 0.041(4) 0.009(3) 0.018(3) 0.010(3) C18 0.080(6) 0.072(5) 0.052(4) 0.010(4) 0.029(4) 0.026(4) C19 0.064(5) 0.088(6) 0.078(6) 0.033(5) 0.033(5) 0.016(5) I1 0.0508(3) 0.0520(3) 0.0543(3) 0.0105(2) 0.0123(2) 0.0114(2) I2 0.0667(3) 0.0705(3) 0.0392(3) 0.0029(2) 0.0106(2) 0.0156(3) S1 0.0672(13) 0.0898(15) 0.0525(12) 0.0188(11) 0.0066(10) 0.0338(12) S2 0.0645(13) 0.0573(11) 0.0582(12) -0.0105(9) 0.0097(10) -0.0035(9) S3 0.0597(11) 0.0666(11) 0.0371(9) 0.0025(8) 0.0103(8) 0.0102(9) S4 0.0530(11) 0.0765(13) 0.0458(10) 0.0051(9) 0.0116(9) 0.0093(10) S5 0.0540(11) 0.0646(11) 0.0441(10) 0.0053(8) 0.0126(8) 0.0153(9) S6 0.0573(11) 0.0611(10) 0.0424(9) 0.0067(8) 0.0115(8) 0.0135(9) S7 0.0660(13) 0.0719(12) 0.0448(10) 0.0081(9) 0.0088(9) 0.0142(10) S8 0.0643(13) 0.0687(12) 0.0652(13) 0.0005(10) 0.0192(10) -0.0071(10) N1 0.046(3) 0.045(3) 0.034(3) 0.006(2) 0.007(2) 0.007(2) N2 0.057(4) 0.061(4) 0.041(3) 0.012(3) 0.012(3) 0.016(3) N3 0.064(4) 0.046(3) 0.050(3) 0.005(3) 0.019(3) 0.007(3) 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' Ga Ga 0.2307 1.6083 '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' 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' 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 N3 Ga N3 180.0(4) . 2 N3 Ga N2 89.6(3) . 2 N3 Ga N2 90.4(3) 2 2 N3 Ga N2 90.4(3) . . N3 Ga N2 89.6(3) 2 . N2 Ga N2 180.0(4) 2 . N3 Ga N1 90.2(2) . 2 N3 Ga N1 89.8(2) 2 2 N2 Ga N1 89.2(2) 2 2 N2 Ga N1 90.8(2) . 2 N3 Ga N1 89.8(2) . . N3 Ga N1 90.2(2) 2 . N2 Ga N1 90.8(2) 2 . N2 Ga N1 89.2(2) . . N1 Ga N1 180.0(3) 2 . N1 C1 C2 122.6(6) . . N1 C1 H1 118.7 . . C2 C1 H1 118.7 . . C3 C2 C7 122.0(6) . . C3 C2 C1 121.0(6) . . C7 C2 C1 117.0(6) . . C2 C3 C4 118.4(7) . . C2 C3 H3 120.8 . . C4 C3 H3 120.8 . . C3 C4 C5 119.5(7) . . C3 C4 H4 120.2 . . C5 C4 H4 120.2 . . C6 C5 C4 121.9(7) . . C6 C5 H5 119.0 . . C4 C5 H5 119.0 . . C5 C6 C7 119.5(8) . . C5 C6 H6 120.3 . . C7 C6 H6 120.3 . . C2 C7 C6 118.6(7) . . C2 C7 C8 118.8(6) . . C6 C7 C8 122.5(7) . . C9 C8 C7 119.0(6) . . C9 C8 H8 120.5 . . C7 C8 H8 120.5 . . C8 C9 N1 123.3(7) . . C8 C9 H9 118.3 . . N1 C9 H9 118.3 . . N2 C10 S1 178.9(6) . . N3 C11 S2 179.8(7) . . C13 C12 S3 117.2(5) . . C13 C12 I1 125.9(5) . . S3 C12 I1 116.5(4) . . C12 C13 S4 118.0(5) . . C12 C13 I2 125.3(5) . . S4 C13 I2 116.6(4) . . C15 C14 S4 123.2(6) . . C15 C14 S3 121.9(6) . . S4 C14 S3 114.9(4) . . C14 C15 S5 123.7(6) . . C14 C15 S6 121.6(6) . . S5 C15 S6 114.6(4) . . C17 C16 S7 125.5(6) . . C17 C16 S5 117.1(5) . . S7 C16 S5 117.3(4) . . C16 C17 S8 129.6(6) . . C16 C17 S6 117.1(5) . . S8 C17 S6 113.3(4) . . C19 C18 S7 115.2(6) . . C19 C18 H18A 108.5 . . S7 C18 H18A 108.5 . . C19 C18 H18B 108.5 . . S7 C18 H18B 108.5 . . H18A C18 H18B 107.5 . . C18 C19 S8 115.4(5) . . C18 C19 H19A 108.4 . . S8 C19 H19A 108.4 . . C18 C19 H19B 108.4 . . S8 C19 H19B 108.4 . . H19A C19 H19B 107.5 . . C14 S3 C12 94.9(3) . . C14 S4 C13 95.1(3) . . C15 S5 C16 94.9(3) . . C15 S6 C17 94.6(3) . . C16 S7 C18 96.1(4) . . C17 S8 C19 104.0(4) . . C1 N1 C9 119.2(6) . . C1 N1 Ga 120.0(4) . . C9 N1 Ga 120.8(4) . . C10 N2 Ga 164.5(6) . . C11 N3 Ga 173.6(6) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ga N3 2.001(6) . Ga N3 2.001(6) 2 Ga N2 2.014(6) 2 Ga N2 2.014(6) . Ga N1 2.081(5) 2 Ga N1 2.081(5) . C1 N1 1.312(8) . C1 C2 1.443(9) . C1 H1 0.9300 . C2 C3 1.388(10) . C2 C7 1.410(10) . C3 C4 1.408(10) . C3 H3 0.9300 . C4 C5 1.410(11) . C4 H4 0.9300 . C5 C6 1.363(11) . C5 H5 0.9300 . C6 C7 1.416(10) . C6 H6 0.9300 . C7 C8 1.425(9) . C8 C9 1.350(10) . C8 H8 0.9300 . C9 N1 1.370(8) . C9 H9 0.9300 . C10 N2 1.152(8) . C10 S1 1.624(7) . C11 N3 1.163(8) . C11 S2 1.616(7) . C12 C13 1.308(10) . C12 S3 1.752(7) . C12 I1 2.093(7) . C13 S4 1.743(7) . C13 I2 2.084(6) . C14 C15 1.373(9) . C14 S4 1.731(7) . C14 S3 1.740(8) . C15 S5 1.737(7) . C15 S6 1.750(8) . C16 C17 1.330(10) . C16 S7 1.750(7) . C16 S5 1.761(7) . C17 S8 1.740(7) . C17 S6 1.758(7) . C18 C19 1.507(12) . C18 S7 1.794(8) . C18 H18A 0.9700 . C18 H18B 0.9700 . C19 S8 1.772(9) . C19 H19A 0.9700 . C19 H19B 0.9700 . _journal_paper_doi 10.1021/cm052199q