# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Tatsuro Imakubo' _publ_contact_author_address ; Imakubo Initiative Research Unit RIKEN 2-1 Hirosawa Wako Saitama 351-0198 JAPAN ; _publ_contact_author_email IMAKUBO@RIKEN.JP _publ_section_title ; New organic conductors based on dibromo- and diiodo-TSeFs with magnetic and non-magnetic MX4 counter anions (M = Fe, Ga; X = Cl, Br) ; loop_ _publ_author_name 'Tatsuro Imakubo' 'Tomohito Kawashima' 'Megumi Kibune' 'Mitsuhiko Maesato' 'Gunzi Saito' 'Takashi Shirahata' data_(DBrETSe)2FeCl4 _database_code_depnum_ccdc_archive 'CCDC 604639' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br4 Cl4 Fe S4 Se8' _chemical_formula_weight 1477.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.191(3) _cell_length_b 35.436(14) _cell_length_c 13.048(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3325(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 644 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 25.83 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 14.605 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0968 _exptl_absorpt_correction_T_max 0.8677 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 24 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11830 _diffrn_reflns_av_R_equivalents 0.1779 _diffrn_reflns_av_sigmaI/netI 0.1366 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.43 _reflns_number_total 2168 _reflns_number_gt 818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0978P)^2^+31.3085P] 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 2168 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1630 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 0.796 _refine_ls_restrained_S_all 0.796 _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 Br1 Br 0.1669(2) 0.36564(4) 0.36794(10) 0.0375(4) Uani 1 1 d . . . Se1 Se 0.1571(2) 0.27611(3) 0.37819(8) 0.0292(4) Uani 1 1 d . . . Se2 Se 0.1593(2) 0.18079(3) 0.37905(9) 0.0284(4) Uani 1 1 d . . . S1 S 0.1675(6) 0.09537(10) 0.3654(2) 0.0431(10) Uani 1 1 d . . . C1 C 0.159(3) 0.2478(4) 0.5000 0.023(4) Uani 1 2 d S . . C2 C 0.160(2) 0.2097(4) 0.5000 0.017(3) Uani 1 2 d S . . C3 C 0.1649(18) 0.3220(3) 0.4502(8) 0.025(3) Uani 1 1 d . . . C4 C 0.1658(18) 0.1333(3) 0.4488(8) 0.025(3) Uani 1 1 d . . . C5A C 0.225(4) 0.0555(8) 0.456(2) 0.041(7) Uani 0.50 1 d PD . . H5A1 H 0.2085 0.0314 0.4216 0.049 Uiso 0.50 1 calc PR . . H5A2 H 0.3526 0.0574 0.4786 0.049 Uiso 0.50 1 calc PR . . C5B C 0.092(4) 0.0582(8) 0.452(2) 0.041(7) Uani 0.50 1 d PD . . H5B1 H -0.0326 0.0635 0.4757 0.049 Uiso 0.50 1 calc PR . . H5B2 H 0.0904 0.0343 0.4157 0.049 Uiso 0.50 1 calc PR . . Fe1 Fe 0.5000 0.0000 0.2500 0.0597(15) Uani 1 4 d S . . Cl1 Cl 0.3233(10) 0.03563(13) 0.1566(4) 0.107(2) 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 Br1 0.0414(9) 0.0327(8) 0.0385(8) 0.0118(6) -0.0010(8) 0.0004(7) Se1 0.0399(8) 0.0276(7) 0.0199(6) 0.0011(5) -0.0007(7) 0.0006(6) Se2 0.0388(9) 0.0276(7) 0.0188(6) -0.0012(5) 0.0001(7) -0.0012(6) S1 0.065(3) 0.0317(18) 0.0322(19) -0.0040(15) 0.001(2) -0.004(2) C1 0.037(12) 0.017(8) 0.015(7) 0.000 0.000 0.006(10) C2 0.008(9) 0.027(9) 0.017(8) 0.000 0.000 0.006(8) C3 0.025(7) 0.022(6) 0.029(6) 0.011(5) -0.004(6) -0.008(6) C4 0.029(7) 0.019(6) 0.026(6) 0.010(5) -0.007(6) 0.002(6) C5A 0.07(2) 0.015(8) 0.038(9) 0.009(7) 0.010(19) -0.008(18) C5B 0.07(2) 0.015(8) 0.038(9) 0.009(7) 0.010(19) -0.008(18) Fe1 0.097(4) 0.029(2) 0.053(3) 0.000 0.000 0.000 Cl1 0.172(6) 0.052(3) 0.096(4) 0.005(3) -0.032(4) 0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.882(10) . ? Se1 C3 1.880(11) . ? Se1 C1 1.880(8) . ? Se2 C2 1.881(8) . ? Se2 C4 1.912(10) . ? S1 C4 1.731(11) . ? S1 C5B 1.82(3) . ? S1 C5A 1.89(3) . ? C1 C2 1.35(2) . ? C1 Se1 1.880(8) 10_556 ? C2 Se2 1.881(8) 10_556 ? C3 C3 1.30(2) 10_556 ? C4 C4 1.34(2) 10_556 ? C5A C5B 1.536(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.536(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? Fe1 Cl1 2.167(5) 7_545 ? Fe1 Cl1 2.167(5) 8_445 ? Fe1 Cl1 2.167(5) . ? Fe1 Cl1 2.167(5) 2_655 ? 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 C3 Se1 C1 92.3(5) . . ? C2 Se2 C4 94.5(5) . . ? C4 S1 C5B 99.8(11) . . ? C4 S1 C5A 101.0(10) . . ? C5B S1 C5A 29.8(7) . . ? C2 C1 Se1 122.3(4) . 10_556 ? C2 C1 Se1 122.3(4) . . ? Se1 C1 Se1 115.4(8) 10_556 . ? C1 C2 Se2 123.0(4) . . ? C1 C2 Se2 123.0(4) . 10_556 ? Se2 C2 Se2 114.1(8) . 10_556 ? C3 C3 Se1 120.0(3) 10_556 . ? C3 C3 Br1 124.8(3) 10_556 . ? Se1 C3 Br1 115.2(6) . . ? C4 C4 S1 129.0(3) 10_556 . ? C4 C4 Se2 118.4(3) 10_556 . ? S1 C4 Se2 112.6(6) . . ? C5B C5A S1 108(2) 10_556 . ? C5B C5A H5A1 110.1 10_556 . ? S1 C5A H5A1 110.1 . . ? C5B C5A H5A2 110.1 10_556 . ? S1 C5A H5A2 110.1 . . ? H5A1 C5A H5A2 108.4 . . ? C5A C5B S1 110(2) 10_556 . ? C5A C5B H5B1 109.6 10_556 . ? S1 C5B H5B1 109.6 . . ? C5A C5B H5B2 109.6 10_556 . ? S1 C5B H5B2 109.6 . . ? H5B1 C5B H5B2 108.1 . . ? Cl1 Fe1 Cl1 111.5(3) 7_545 8_445 ? Cl1 Fe1 Cl1 108.7(3) 7_545 . ? Cl1 Fe1 Cl1 108.2(4) 8_445 . ? Cl1 Fe1 Cl1 108.2(4) 7_545 2_655 ? Cl1 Fe1 Cl1 108.7(3) 8_445 2_655 ? Cl1 Fe1 Cl1 111.5(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.128 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.373 # Attachment '6b-revised.cif' data_(DBrETSe)2GaCl4 _database_code_depnum_ccdc_archive 'CCDC 604640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br4 Cl4 Ga S4 Se8' _chemical_formula_weight 1491.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.205(3) _cell_length_b 35.506(15) _cell_length_c 13.063(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3342(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1056 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.21 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2716 _exptl_absorpt_coefficient_mu 14.902 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0944 _exptl_absorpt_correction_T_max 0.8653 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 27 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11566 _diffrn_reflns_av_R_equivalents 0.1842 _diffrn_reflns_av_sigmaI/netI 0.1226 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2176 _reflns_number_gt 877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1123P)^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 2176 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 0.789 _refine_ls_restrained_S_all 0.789 _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 Br1 Br 0.16583(18) 0.36548(3) 0.36814(8) 0.0413(4) Uani 1 1 d . . . Se1 Se 0.15707(16) 0.27600(3) 0.37831(6) 0.0318(3) Uani 1 1 d . . . Se2 Se 0.15914(18) 0.18089(3) 0.37890(6) 0.0317(3) Uani 1 1 d . . . S1 S 0.1664(5) 0.09551(8) 0.36627(19) 0.0442(8) Uani 1 1 d . . . C1 C 0.157(2) 0.2470(3) 0.5000 0.023(3) Uani 1 2 d S . . C2 C 0.158(2) 0.2096(4) 0.5000 0.024(3) Uani 1 2 d S . . C3 C 0.1637(15) 0.3221(2) 0.4486(6) 0.028(2) Uani 1 1 d . . . C4 C 0.1642(14) 0.1342(2) 0.4490(7) 0.030(2) Uani 1 1 d . . . C5A C 0.213(4) 0.0554(9) 0.452(3) 0.052(7) Uani 0.50 1 d PD . . H5A1 H 0.1860 0.0319 0.4169 0.062 Uiso 0.50 1 calc PR . . H5A2 H 0.3434 0.0552 0.4712 0.062 Uiso 0.50 1 calc PR . . C5B C 0.092(4) 0.0590(9) 0.452(2) 0.052(7) Uani 0.50 1 d PD . . H5B1 H -0.0350 0.0641 0.4732 0.062 Uiso 0.50 1 calc PR . . H5B2 H 0.0922 0.0351 0.4160 0.062 Uiso 0.50 1 calc PR . . Ga1 Ga 0.5000 0.0000 0.2500 0.0707(11) Uani 1 4 d S . . Cl1 Cl 0.3252(8) 0.03552(12) 0.1579(3) 0.1035(16) 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 Br1 0.0509(8) 0.0393(7) 0.0338(6) 0.0108(5) -0.0014(6) 0.0004(6) Se1 0.0463(7) 0.0341(6) 0.0151(5) 0.0009(4) -0.0006(5) 0.0003(5) Se2 0.0455(8) 0.0338(6) 0.0156(5) -0.0008(4) 0.0000(5) -0.0004(5) S1 0.069(2) 0.0355(16) 0.0287(14) -0.0056(11) 0.0020(17) -0.0017(16) C1 0.044(9) 0.020(7) 0.006(5) 0.000 0.000 -0.002(8) C2 0.030(8) 0.032(8) 0.011(6) 0.000 0.000 0.008(7) C3 0.040(6) 0.030(5) 0.015(4) 0.011(4) -0.005(5) -0.009(5) C4 0.037(6) 0.025(5) 0.028(5) -0.005(4) -0.001(5) -0.003(5) C5A 0.09(2) 0.025(9) 0.039(6) 0.003(6) 0.02(2) -0.009(19) C5B 0.09(2) 0.025(9) 0.039(6) 0.003(6) 0.02(2) -0.009(19) Ga1 0.112(3) 0.0483(18) 0.0516(17) 0.000 0.000 0.000 Cl1 0.159(4) 0.062(3) 0.089(3) 0.002(2) -0.032(3) 0.023(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 Br1 C3 1.866(8) . ? Se1 C3 1.876(9) . ? Se1 C1 1.894(7) . ? Se2 C2 1.883(7) . ? Se2 C4 1.893(9) . ? S1 C4 1.749(9) . ? S1 C5B 1.80(3) . ? S1 C5A 1.84(3) . ? C1 C2 1.328(18) . ? C1 Se1 1.894(7) 10_556 ? C2 Se2 1.883(7) 10_556 ? C3 C3 1.344(16) 10_556 ? C4 C4 1.332(17) 10_556 ? C5A C5B 1.534(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.534(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? Ga1 Cl1 2.151(4) 7_545 ? Ga1 Cl1 2.151(4) 8_445 ? Ga1 Cl1 2.151(4) . ? Ga1 Cl1 2.151(4) 2_655 ? 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 C3 Se1 C1 93.6(4) . . ? C2 Se2 C4 93.9(4) . . ? C4 S1 C5B 100.3(11) . . ? C4 S1 C5A 103.6(11) . . ? C5B S1 C5A 28.1(7) . . ? C2 C1 Se1 122.9(3) . 10_556 ? C2 C1 Se1 122.9(3) . . ? Se1 C1 Se1 114.2(6) 10_556 . ? C1 C2 Se2 122.8(3) . . ? C1 C2 Se2 122.8(3) . 10_556 ? Se2 C2 Se2 114.4(7) . 10_556 ? C3 C3 Br1 124.3(3) 10_556 . ? C3 C3 Se1 119.3(2) 10_556 . ? Br1 C3 Se1 116.4(4) . . ? C4 C4 S1 128.2(3) 10_556 . ? C4 C4 Se2 118.9(3) 10_556 . ? S1 C4 Se2 112.9(5) . . ? C5B C5A S1 109(2) 10_556 . ? C5B C5A H5A1 109.9 10_556 . ? S1 C5A H5A1 109.9 . . ? C5B C5A H5A2 109.9 10_556 . ? S1 C5A H5A2 109.9 . . ? H5A1 C5A H5A2 108.3 . . ? C5A C5B S1 114(3) 10_556 . ? C5A C5B H5B1 108.9 10_556 . ? S1 C5B H5B1 108.9 . . ? C5A C5B H5B2 108.9 10_556 . ? S1 C5B H5B2 108.9 . . ? H5B1 C5B H5B2 107.7 . . ? Cl1 Ga1 Cl1 111.9(3) 7_545 8_445 ? Cl1 Ga1 Cl1 108.2(2) 7_545 . ? Cl1 Ga1 Cl1 108.3(3) 8_445 . ? Cl1 Ga1 Cl1 108.3(3) 7_545 2_655 ? Cl1 Ga1 Cl1 108.2(2) 8_445 2_655 ? Cl1 Ga1 Cl1 111.9(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.854 _refine_diff_density_min -1.905 _refine_diff_density_rms 0.402 # Attachment '6c-revised.cif' data_(DBrETSe)2FeBr4 _database_code_depnum_ccdc_archive 'CCDC 604641' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br8 Fe S4 Se8' _chemical_formula_weight 1655.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.489(13) _cell_length_b 7.207(2) _cell_length_c 13.080(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.405(8) _cell_angle_gamma 90.00 _cell_volume 3422.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1044 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 25.77 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 18.549 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.0718 _exptl_absorpt_correction_T_max 0.8362 _exptl_absorpt_process_details ; XPREP; Bruker AXS 2003 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 33 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 12551 _diffrn_reflns_av_R_equivalents 0.1077 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.52 _reflns_number_total 4307 _reflns_number_gt 1792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0683P)^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 4307 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _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 Br1 Br 0.13643(4) 0.3271(2) 0.26651(12) 0.0353(4) Uani 1 1 d . . . Br2 Br 0.13758(4) 0.3327(2) 0.00453(11) 0.0349(4) Uani 1 1 d . . . Se1 Se 0.22394(4) 0.3390(2) 0.34538(10) 0.0272(4) Uani 1 1 d . . . Se2 Se 0.22496(4) 0.34099(19) 0.10275(10) 0.0269(4) Uani 1 1 d . . . Se3 Se 0.31725(4) 0.33941(19) 0.43864(10) 0.0256(4) Uani 1 1 d . . . Se4 Se 0.31818(4) 0.33394(19) 0.19756(10) 0.0260(4) Uani 1 1 d . . . S1 S 0.40021(11) 0.3349(6) 0.5351(3) 0.0357(9) Uani 1 1 d . . . S2 S 0.40150(11) 0.3220(6) 0.2683(3) 0.0361(10) Uani 1 1 d . . . C1 C 0.2527(5) 0.3381(18) 0.2539(10) 0.029(3) Uani 1 1 d . . . C2 C 0.2892(4) 0.3383(17) 0.2870(10) 0.025(3) Uani 1 1 d . . . C3 C 0.1780(4) 0.3317(17) 0.2274(10) 0.021(3) Uani 1 1 d . . . C4 C 0.1797(4) 0.3375(16) 0.1293(9) 0.021(3) Uani 1 1 d . . . C5 C 0.3633(4) 0.3331(16) 0.4157(9) 0.020(3) Uani 1 1 d . . . C6 C 0.3639(4) 0.3269(17) 0.3140(11) 0.025(3) Uani 1 1 d . . . C7 C 0.4380(5) 0.395(3) 0.4858(12) 0.055(5) Uani 1 1 d . . . H7A H 0.4357 0.5231 0.4626 0.066 Uiso 1 1 calc R . . H7B H 0.4613 0.3804 0.5440 0.066 Uiso 1 1 calc R . . C8 C 0.4375(5) 0.271(2) 0.3919(13) 0.055(5) Uani 1 1 d . . . H8A H 0.4350 0.1428 0.4115 0.066 Uiso 1 1 calc R . . H8B H 0.4610 0.2819 0.3799 0.066 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5425(4) 0.7500 0.0364(8) Uani 1 2 d S . . Br3 Br 0.03684(6) 0.7348(3) 0.68550(17) 0.0620(6) Uani 1 1 d . . . Br4 Br -0.03757(6) 0.3564(3) 0.61444(16) 0.0643(6) 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 Br1 0.0264(9) 0.0380(9) 0.0491(9) 0.0005(7) 0.0225(8) 0.0011(7) Br2 0.0265(9) 0.0383(9) 0.0324(8) 0.0004(7) -0.0005(7) 0.0005(7) Se1 0.0240(9) 0.0372(8) 0.0219(7) -0.0006(6) 0.0099(7) -0.0004(7) Se2 0.0216(9) 0.0388(8) 0.0207(7) 0.0005(6) 0.0074(6) 0.0014(7) Se3 0.0215(9) 0.0358(8) 0.0200(7) 0.0001(6) 0.0077(6) -0.0001(7) Se4 0.0227(9) 0.0356(8) 0.0216(7) -0.0020(6) 0.0098(7) -0.0009(7) S1 0.023(2) 0.057(3) 0.0237(18) 0.0001(18) 0.0030(17) 0.000(2) S2 0.021(2) 0.056(3) 0.034(2) -0.0022(19) 0.0135(19) 0.0002(19) C1 0.041(10) 0.034(8) 0.024(7) 0.001(6) 0.026(7) 0.003(8) C2 0.036(10) 0.024(7) 0.018(7) 0.000(6) 0.015(7) -0.006(7) C3 0.015(7) 0.026(7) 0.020(7) -0.009(6) 0.001(6) -0.003(6) C4 0.018(8) 0.022(7) 0.014(6) -0.001(5) -0.008(6) 0.000(6) C5 0.015(7) 0.020(7) 0.019(6) -0.005(6) -0.002(6) -0.010(6) C6 0.019(8) 0.022(7) 0.033(8) 0.006(6) 0.008(7) 0.004(6) C7 0.025(10) 0.109(15) 0.027(8) 0.006(9) 0.004(8) -0.012(10) C8 0.048(13) 0.067(12) 0.051(11) 0.001(9) 0.019(10) 0.015(10) Fe1 0.024(2) 0.052(2) 0.0310(16) 0.000 0.0052(15) 0.000 Br3 0.0488(14) 0.0750(14) 0.0683(12) 0.0135(10) 0.0276(11) -0.0116(11) Br4 0.0481(14) 0.0737(14) 0.0642(12) -0.0258(10) 0.0095(11) -0.0092(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.833(13) . ? Br2 C4 1.881(12) . ? Se1 C1 1.880(13) . ? Se1 C3 1.924(13) . ? Se2 C4 1.885(14) . ? Se2 C1 1.909(14) . ? Se3 C5 1.894(13) . ? Se3 C2 1.917(13) . ? Se4 C2 1.867(13) . ? Se4 C6 1.906(14) . ? S1 C5 1.727(13) . ? S1 C7 1.826(16) . ? S2 C6 1.742(14) . ? S2 C8 1.784(17) . ? C1 C2 1.33(2) . ? C3 C4 1.308(16) . ? C5 C6 1.339(16) . ? C7 C8 1.51(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? Fe1 Br4 2.309(3) . ? Fe1 Br4 2.309(3) 2_556 ? Fe1 Br3 2.332(3) 2_556 ? Fe1 Br3 2.332(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 C1 Se1 C3 93.9(6) . . ? C4 Se2 C1 92.4(6) . . ? C5 Se3 C2 94.1(6) . . ? C2 Se4 C6 94.9(6) . . ? C5 S1 C7 101.2(7) . . ? C6 S2 C8 100.2(7) . . ? C2 C1 Se1 125.1(10) . . ? C2 C1 Se2 120.4(9) . . ? Se1 C1 Se2 114.5(9) . . ? C1 C2 Se4 125.7(10) . . ? C1 C2 Se3 120.7(9) . . ? Se4 C2 Se3 113.6(8) . . ? C4 C3 Br1 127.5(11) . . ? C4 C3 Se1 116.9(10) . . ? Br1 C3 Se1 115.6(6) . . ? C3 C4 Br2 122.6(11) . . ? C3 C4 Se2 122.2(10) . . ? Br2 C4 Se2 115.1(6) . . ? C6 C5 S1 128.2(11) . . ? C6 C5 Se3 118.9(10) . . ? S1 C5 Se3 112.9(6) . . ? C5 C6 S2 129.2(11) . . ? C5 C6 Se4 118.6(10) . . ? S2 C6 Se4 112.2(7) . . ? C8 C7 S1 110.6(12) . . ? C8 C7 H7A 109.5 . . ? S1 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? S1 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 S2 114.2(12) . . ? C7 C8 H8A 108.7 . . ? S2 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? S2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? Br4 Fe1 Br4 108.94(16) . 2_556 ? Br4 Fe1 Br3 108.80(8) . 2_556 ? Br4 Fe1 Br3 111.62(8) 2_556 2_556 ? Br4 Fe1 Br3 111.62(8) . . ? Br4 Fe1 Br3 108.80(8) 2_556 . ? Br3 Fe1 Br3 107.09(16) 2_556 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.450 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.421 # Attachment '6d-revised.cif' data_(DBrETSe)2GaBr4 _database_code_depnum_ccdc_archive 'CCDC 604642' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br8 Ga S4 Se8' _chemical_formula_weight 1669.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.506(11) _cell_length_b 7.214(2) _cell_length_c 13.084(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.567(6) _cell_angle_gamma 90.00 _cell_volume 3424.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1414 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 26.10 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 18.898 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.0732 _exptl_absorpt_correction_T_max 0.8335 _exptl_absorpt_process_details ; XPREP; Bruker AXS 2003 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 42 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 12276 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.1054 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.41 _reflns_number_total 4260 _reflns_number_gt 1948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1139P)^2^+17.4987P] 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 4260 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2690 _refine_ls_wR_factor_gt 0.2490 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Br1 Br 0.13670(5) 0.3286(3) 0.26733(15) 0.0366(5) Uani 1 1 d . . . Br2 Br 0.13750(5) 0.3338(3) 0.00494(14) 0.0376(5) Uani 1 1 d . . . Se1 Se 0.22407(5) 0.3402(3) 0.34540(12) 0.0290(4) Uani 1 1 d . . . Se2 Se 0.22476(5) 0.3418(3) 0.10270(12) 0.0294(4) Uani 1 1 d . . . Se3 Se 0.31728(4) 0.3402(2) 0.43824(12) 0.0279(4) Uani 1 1 d . . . Se4 Se 0.31797(4) 0.3355(3) 0.19734(12) 0.0278(4) Uani 1 1 d . . . S1 S 0.40027(13) 0.3351(7) 0.5352(3) 0.0372(11) Uani 1 1 d . . . S2 S 0.40111(13) 0.3235(7) 0.2679(4) 0.0391(12) Uani 1 1 d . . . C1 C 0.2524(4) 0.342(2) 0.2518(11) 0.025(4) Uani 1 1 d . . . C2 C 0.2902(4) 0.340(2) 0.2916(12) 0.024(4) Uani 1 1 d . . . C3 C 0.1786(5) 0.327(2) 0.2282(13) 0.031(4) Uani 1 1 d . . . C4 C 0.1785(5) 0.339(2) 0.1276(12) 0.029(4) Uani 1 1 d . . . C5 C 0.3633(4) 0.334(2) 0.4165(12) 0.027(4) Uani 1 1 d . . . C6 C 0.3630(4) 0.335(2) 0.3125(12) 0.022(3) Uani 1 1 d . . . C7 C 0.4369(6) 0.405(4) 0.4848(17) 0.078(8) Uani 1 1 d . . . H7A H 0.4328 0.5316 0.4590 0.093 Uiso 1 1 calc R . . H7B H 0.4604 0.3991 0.5432 0.093 Uiso 1 1 calc R . . C8 C 0.4378(6) 0.276(3) 0.3916(16) 0.063(7) Uani 1 1 d . . . H8A H 0.4360 0.1484 0.4124 0.075 Uiso 1 1 calc R . . H8B H 0.4612 0.2913 0.3798 0.075 Uiso 1 1 calc R . . Ga1 Ga 0.0000 0.5369(5) 0.7500 0.0508(10) Uani 1 2 d S . . Br3 Br 0.03699(7) 0.7274(4) 0.6873(2) 0.0705(8) Uani 1 1 d . . . Br4 Br -0.03700(7) 0.3530(4) 0.6142(2) 0.0754(9) 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 Br1 0.0281(10) 0.0403(11) 0.0473(11) -0.0005(9) 0.0204(8) 0.0005(8) Br2 0.0286(10) 0.0431(11) 0.0311(9) -0.0002(9) -0.0034(7) 0.0005(9) Se1 0.0250(9) 0.0407(10) 0.0213(8) 0.0006(8) 0.0081(7) -0.0003(8) Se2 0.0246(9) 0.0419(11) 0.0206(8) -0.0014(8) 0.0059(7) -0.0003(8) Se3 0.0238(9) 0.0392(10) 0.0202(8) 0.0008(8) 0.0067(7) 0.0004(8) Se4 0.0246(9) 0.0370(10) 0.0219(8) -0.0013(8) 0.0080(7) 0.0001(8) S1 0.026(2) 0.054(3) 0.026(2) 0.000(2) 0.0009(17) 0.002(2) S2 0.026(2) 0.057(3) 0.037(2) -0.006(2) 0.015(2) -0.004(2) C1 0.019(8) 0.043(10) 0.013(7) 0.010(7) 0.007(6) 0.006(8) C2 0.019(8) 0.027(9) 0.025(8) -0.004(7) 0.005(6) -0.012(7) C3 0.027(9) 0.040(11) 0.030(9) -0.005(8) 0.016(7) -0.011(8) C4 0.035(10) 0.033(10) 0.019(8) -0.005(8) 0.008(7) 0.005(8) C5 0.031(9) 0.020(9) 0.030(9) -0.013(7) 0.011(7) -0.021(8) C6 0.017(8) 0.019(8) 0.027(8) -0.001(7) 0.001(6) -0.009(7) C7 0.032(13) 0.15(3) 0.047(13) 0.012(15) 0.006(10) -0.003(15) C8 0.043(14) 0.096(19) 0.041(12) 0.007(12) 0.004(10) 0.007(13) Ga1 0.0288(17) 0.083(3) 0.0395(17) 0.000 0.0102(13) 0.000 Br3 0.0514(16) 0.087(2) 0.0762(17) 0.0092(14) 0.0253(13) -0.0106(14) Br4 0.0505(16) 0.091(2) 0.0729(17) -0.0263(15) 0.0055(12) -0.0083(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 Br1 C3 1.848(16) . ? Br2 C4 1.837(16) . ? Se1 C1 1.894(15) . ? Se1 C3 1.905(16) . ? Se2 C1 1.884(14) . ? Se2 C4 1.915(17) . ? Se3 C2 1.851(14) . ? Se3 C5 1.888(17) . ? Se4 C6 1.877(14) . ? Se4 C2 1.883(15) . ? S1 C5 1.719(16) . ? S1 C7 1.81(2) . ? S2 C6 1.755(16) . ? S2 C8 1.789(19) . ? C1 C2 1.37(2) . ? C3 C4 1.32(2) . ? C5 C6 1.36(2) . ? C7 C8 1.54(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? Ga1 Br4 2.292(3) . ? Ga1 Br4 2.292(3) 2_556 ? Ga1 Br3 2.318(3) . ? Ga1 Br3 2.318(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 C3 93.1(6) . . ? C1 Se2 C4 93.4(6) . . ? C2 Se3 C5 94.3(7) . . ? C6 Se4 C2 92.8(7) . . ? C5 S1 C7 100.4(9) . . ? C6 S2 C8 101.7(9) . . ? C2 C1 Se2 123.6(12) . . ? C2 C1 Se1 121.5(11) . . ? Se2 C1 Se1 114.9(8) . . ? C1 C2 Se3 123.4(12) . . ? C1 C2 Se4 121.0(11) . . ? Se3 C2 Se4 115.6(8) . . ? C4 C3 Br1 124.5(14) . . ? C4 C3 Se1 119.6(13) . . ? Br1 C3 Se1 115.4(8) . . ? C3 C4 Br2 125.8(14) . . ? C3 C4 Se2 118.7(13) . . ? Br2 C4 Se2 115.3(8) . . ? C6 C5 S1 129.4(13) . . ? C6 C5 Se3 117.1(12) . . ? S1 C5 Se3 113.5(9) . . ? C5 C6 S2 127.2(12) . . ? C5 C6 Se4 120.1(12) . . ? S2 C6 Se4 112.5(8) . . ? C8 C7 S1 110.3(17) . . ? C8 C7 H7A 109.6 . . ? S1 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? S1 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 S2 112.4(16) . . ? C7 C8 H8A 109.1 . . ? S2 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? S2 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? Br4 Ga1 Br4 109.3(2) . 2_556 ? Br4 Ga1 Br3 111.40(11) . . ? Br4 Ga1 Br3 108.77(10) 2_556 . ? Br4 Ga1 Br3 108.77(10) . 2_556 ? Br4 Ga1 Br3 111.40(11) 2_556 2_556 ? Br3 Ga1 Br3 107.3(2) . 2_556 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.208 _refine_diff_density_min -1.618 _refine_diff_density_rms 0.407 # Attachment '7a-revised.cif' data_(DIETSe)2FeCl4 _database_code_depnum_ccdc_archive 'CCDC 604643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Cl4 Fe I4 S4 Se8' _chemical_formula_weight 1665.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.3104(15) _cell_length_b 35.755(8) _cell_length_c 13.552(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3542.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 2440 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.85 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 12.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2521 _exptl_absorpt_correction_T_max 0.8836 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 69 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12642 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2303 _reflns_number_gt 1711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0723P)^2^+2.1799P] 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 2303 _refine_ls_number_parameters 97 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.18043(5) 0.367402(12) 0.36391(3) 0.03489(17) Uani 1 1 d . . . Se1 Se 0.16846(8) 0.273964(16) 0.38284(4) 0.03060(18) Uani 1 1 d . . . Se2 Se 0.17285(8) 0.179269(16) 0.38308(4) 0.03022(18) Uani 1 1 d . . . S1 S 0.1734(2) 0.09447(5) 0.37110(11) 0.0395(4) Uani 1 1 d . . . C1 C 0.1709(10) 0.2450(2) 0.5000 0.0267(16) Uani 1 2 d S . . C2 C 0.1708(9) 0.2074(2) 0.5000 0.0269(16) Uani 1 2 d S . . C3 C 0.1751(6) 0.31982(15) 0.4506(4) 0.0251(11) Uani 1 1 d . . . C4 C 0.1746(7) 0.13274(15) 0.4502(4) 0.0290(12) Uani 1 1 d . . . C5A C 0.223(2) 0.0563(4) 0.4535(11) 0.056(4) Uani 0.50 1 d PD . . H5A1 H 0.2031 0.0328 0.4194 0.068 Uiso 0.50 1 calc PR . . H5A2 H 0.3506 0.0574 0.4728 0.068 Uiso 0.50 1 calc PR . . C5B C 0.103(2) 0.0578(4) 0.4544(10) 0.049(4) Uani 0.50 1 d PD . . H5B1 H -0.0235 0.0620 0.4738 0.058 Uiso 0.50 1 calc PR . . H5B2 H 0.1086 0.0339 0.4205 0.058 Uiso 0.50 1 calc PR . . Fe1 Fe 0.5000 0.0000 0.2500 0.0631(6) Uani 1 4 d S . . Cl1 Cl 0.3234(4) 0.03526(8) 0.1605(2) 0.1021(10) 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 I1 0.0388(3) 0.0281(3) 0.0378(3) 0.01105(16) -0.00331(16) 0.00007(15) Se1 0.0459(4) 0.0234(4) 0.0225(3) -0.0003(2) -0.0008(2) 0.0004(2) Se2 0.0414(4) 0.0227(3) 0.0266(3) -0.0011(2) 0.0011(2) -0.0006(2) S1 0.0550(10) 0.0244(8) 0.0391(8) -0.0072(6) 0.0046(7) -0.0017(7) C1 0.030(4) 0.025(4) 0.025(4) 0.000 0.000 0.000(3) C2 0.026(4) 0.027(4) 0.028(4) 0.000 0.000 -0.001(3) C3 0.026(3) 0.022(3) 0.027(3) 0.002(2) 0.000(2) -0.001(2) C4 0.035(3) 0.018(3) 0.033(3) 0.004(2) 0.003(2) 0.000(2) C5A 0.075(11) 0.023(7) 0.071(10) 0.011(6) 0.023(10) 0.006(8) C5B 0.077(10) 0.021(7) 0.047(7) 0.003(5) -0.003(8) -0.020(8) Fe1 0.0873(16) 0.0228(10) 0.0793(16) 0.000 0.000 0.000 Cl1 0.134(3) 0.0467(15) 0.126(2) 0.0148(15) -0.0331(18) 0.0127(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 I1 C3 2.068(5) . ? Se1 C3 1.880(5) . ? Se1 C1 1.895(4) . ? Se2 C2 1.877(4) . ? Se2 C4 1.896(5) . ? S1 C4 1.738(6) . ? S1 C5A 1.799(15) . ? S1 C5B 1.806(13) . ? C1 C2 1.345(12) . ? C1 Se1 1.895(4) 10_556 ? C2 Se2 1.877(4) 10_556 ? C3 C3 1.340(10) 10_556 ? C4 C4 1.349(11) 10_556 ? C5A C5B 1.530(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.530(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? Fe1 Cl1 2.174(3) 7_545 ? Fe1 Cl1 2.174(3) . ? Fe1 Cl1 2.174(3) 2_655 ? Fe1 Cl1 2.174(3) 8_445 ? 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 C3 Se1 C1 93.8(3) . . ? C2 Se2 C4 93.8(3) . . ? C4 S1 C5A 102.3(5) . . ? C4 S1 C5B 100.8(5) . . ? C5A S1 C5B 28.3(5) . . ? C2 C1 Se1 123.1(2) . 10_556 ? C2 C1 Se1 123.1(2) . . ? Se1 C1 Se1 113.8(4) 10_556 . ? C1 C2 Se2 122.4(2) . . ? C1 C2 Se2 122.4(2) . 10_556 ? Se2 C2 Se2 115.1(4) . 10_556 ? C3 C3 Se1 119.23(15) 10_556 . ? C3 C3 I1 124.61(14) 10_556 . ? Se1 C3 I1 116.2(2) . . ? C4 C4 S1 128.09(19) 10_556 . ? C4 C4 Se2 118.67(18) 10_556 . ? S1 C4 Se2 113.2(3) . . ? C5B C5A S1 111.4(10) 10_556 . ? C5B C5A H5A1 109.3 10_556 . ? S1 C5A H5A1 109.3 . . ? C5B C5A H5A2 109.3 10_556 . ? S1 C5A H5A2 109.3 . . ? H5A1 C5A H5A2 108.0 . . ? C5A C5B S1 111.7(10) 10_556 . ? C5A C5B H5B1 109.3 10_556 . ? S1 C5B H5B1 109.3 . . ? C5A C5B H5B2 109.3 10_556 . ? S1 C5B H5B2 109.3 . . ? H5B1 C5B H5B2 107.9 . . ? Cl1 Fe1 Cl1 109.11(16) 7_545 . ? Cl1 Fe1 Cl1 107.13(17) 7_545 2_655 ? Cl1 Fe1 Cl1 112.22(18) . 2_655 ? Cl1 Fe1 Cl1 112.22(18) 7_545 8_445 ? Cl1 Fe1 Cl1 107.13(17) . 8_445 ? Cl1 Fe1 Cl1 109.11(16) 2_655 8_445 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.347 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.296 # Attachment '7b-revised.cif' data_(DIETSe)2GaCl4 _database_code_depnum_ccdc_archive 'CCDC 604644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Cl4 Ga I4 S4 Se8' _chemical_formula_weight 1679.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.313(3) _cell_length_b 35.766(13) _cell_length_c 13.558(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3546(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 859 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.48 _exptl_crystal_description plate _exptl_crystal_colour browny _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3004 _exptl_absorpt_coefficient_mu 13.020 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1116 _exptl_absorpt_correction_T_max 0.8808 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 19 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12459 _diffrn_reflns_av_R_equivalents 0.1577 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2310 _reflns_number_gt 1113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0876P)^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 2310 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1482 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.859 _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 I1 I 0.17974(12) 0.36733(2) 0.36375(6) 0.0359(3) Uani 1 1 d . . . Se1 Se 0.1680(2) 0.27395(3) 0.38306(8) 0.0320(4) Uani 1 1 d . . . Se2 Se 0.1720(2) 0.17946(3) 0.38339(8) 0.0313(4) Uani 1 1 d . . . S1 S 0.1735(6) 0.09447(10) 0.3713(2) 0.0416(9) Uani 1 1 d . . . C1 C 0.171(3) 0.2452(5) 0.5000 0.032(4) Uani 1 2 d S . . C2 C 0.167(2) 0.2077(4) 0.5000 0.021(3) Uani 1 2 d S . . C3 C 0.1752(17) 0.3199(3) 0.4511(7) 0.024(3) Uani 1 1 d . . . C4 C 0.1706(15) 0.1326(3) 0.4506(8) 0.029(3) Uani 1 1 d . . . C5A C 0.220(4) 0.0562(9) 0.453(2) 0.042(6) Uani 0.50 1 d PD . . H5A1 H 0.1962 0.0327 0.4196 0.051 Uiso 0.50 1 calc PR . . H5A2 H 0.3481 0.0566 0.4720 0.051 Uiso 0.50 1 calc PR . . C5B C 0.101(4) 0.0587(9) 0.454(2) 0.042(6) Uani 0.50 1 d PD . . H5B1 H -0.0248 0.0635 0.4732 0.051 Uiso 0.50 1 calc PR . . H5B2 H 0.1037 0.0348 0.4198 0.051 Uiso 0.50 1 calc PR . . Ga1 Ga 0.5000 0.0000 0.2500 0.0577(11) Uani 1 4 d S . . Cl1 Cl 0.3267(8) 0.03493(13) 0.1613(4) 0.0960(18) 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 I1 0.0399(5) 0.0321(5) 0.0358(5) 0.0111(4) -0.0032(5) 0.0002(5) Se1 0.0473(9) 0.0267(7) 0.0220(6) -0.0007(5) -0.0006(6) 0.0006(7) Se2 0.0431(9) 0.0244(7) 0.0264(6) -0.0013(5) 0.0014(6) 0.0002(7) S1 0.060(3) 0.0240(16) 0.0409(18) -0.0054(14) 0.006(2) -0.0009(18) C1 0.046(13) 0.024(9) 0.027(8) 0.000 0.000 0.000(10) C2 0.024(10) 0.021(8) 0.017(7) 0.000 0.000 -0.005(8) C3 0.034(7) 0.018(6) 0.019(5) -0.001(4) 0.006(6) 0.004(6) C4 0.030(7) 0.024(6) 0.034(6) -0.002(5) 0.014(6) -0.006(6) C5A 0.051(17) 0.034(9) 0.042(9) 0.015(8) 0.013(16) 0.000(17) C5B 0.051(17) 0.034(9) 0.042(9) 0.015(8) 0.013(16) 0.000(17) Ga1 0.078(3) 0.0248(17) 0.070(2) 0.000 0.000 0.000 Cl1 0.132(5) 0.050(3) 0.106(4) 0.012(3) -0.033(4) 0.012(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 I1 C3 2.068(10) . ? Se1 C1 1.890(9) . ? Se1 C3 1.886(10) . ? Se2 C2 1.877(8) . ? Se2 C4 1.908(11) . ? S1 C4 1.736(11) . ? S1 C5B 1.78(3) . ? S1 C5A 1.80(3) . ? C1 C2 1.34(2) . ? C1 Se1 1.890(9) 10_556 ? C2 Se2 1.877(8) 10_556 ? C3 C3 1.33(2) 10_556 ? C4 C4 1.34(2) 10_556 ? C5A C5B 1.535(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.535(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? Ga1 Cl1 2.148(5) 7_545 ? Ga1 Cl1 2.148(5) 2_655 ? Ga1 Cl1 2.148(5) . ? Ga1 Cl1 2.148(5) 8_445 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Se1 C3 93.7(5) . . ? C2 Se2 C4 94.1(5) . . ? C4 S1 C5B 99.9(11) . . ? C4 S1 C5A 102.6(11) . . ? C5B S1 C5A 28.4(8) . . ? C2 C1 Se1 122.9(4) . 10_556 ? C2 C1 Se1 122.9(4) . . ? Se1 C1 Se1 114.0(9) 10_556 . ? C1 C2 Se2 122.5(4) . . ? C1 C2 Se2 122.5(4) . 10_556 ? Se2 C2 Se2 114.8(8) . 10_556 ? C3 C3 Se1 119.3(3) 10_556 . ? C3 C3 I1 124.9(3) 10_556 . ? Se1 C3 I1 115.8(5) . . ? C4 C4 S1 128.3(4) 10_556 . ? C4 C4 Se2 118.5(3) 10_556 . ? S1 C4 Se2 113.2(6) . . ? C5B C5A S1 111(2) 10_556 . ? C5B C5A H5A1 109.5 10_556 . ? S1 C5A H5A1 109.5 . . ? C5B C5A H5A2 109.5 10_556 . ? S1 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 108.1 . . ? C5A C5B S1 113(2) 10_556 . ? C5A C5B H5B1 109.0 10_556 . ? S1 C5B H5B1 109.0 . . ? C5A C5B H5B2 109.0 10_556 . ? S1 C5B H5B2 109.0 . . ? H5B1 C5B H5B2 107.8 . . ? Cl1 Ga1 Cl1 107.7(3) 7_545 2_655 ? Cl1 Ga1 Cl1 108.9(3) 7_545 . ? Cl1 Ga1 Cl1 111.9(3) 2_655 . ? Cl1 Ga1 Cl1 111.9(3) 7_545 8_445 ? Cl1 Ga1 Cl1 108.9(3) 2_655 8_445 ? Cl1 Ga1 Cl1 107.7(3) . 8_445 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.027 _refine_diff_density_min -1.325 _refine_diff_density_rms 0.390 # Attachment '7c-revised.cif' data_(DIETSe)2FeBr4 _database_code_depnum_ccdc_archive 'CCDC 604645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br4 Fe I4 S4 Se8' _chemical_formula_weight 1843.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.317(2) _cell_length_b 36.582(12) _cell_length_c 13.569(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3632(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1820 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 26.32 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 16.476 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0687 _exptl_absorpt_correction_T_max 0.8526 _exptl_absorpt_process_details ; XPREP; Bruker AXS, 2003 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 47 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12816 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2352 _reflns_number_gt 1523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0800P)^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 2352 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.006 _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 0.18348(9) 0.364680(18) 0.36386(5) 0.0333(2) Uani 1 1 d . . . Se1 Se 0.17036(14) 0.27338(3) 0.38298(7) 0.0298(3) Uani 1 1 d . . . Se2 Se 0.17611(15) 0.18090(2) 0.38322(7) 0.0286(3) Uani 1 1 d . . . S1 S 0.1778(4) 0.09802(7) 0.37134(19) 0.0376(6) Uani 1 1 d . . . C1 C 0.1748(19) 0.2451(4) 0.5000 0.028(3) Uani 1 2 d S . . C2 C 0.1721(17) 0.2082(3) 0.5000 0.023(3) Uani 1 2 d S . . C3 C 0.1774(12) 0.3183(2) 0.4505(6) 0.0218(18) Uani 1 1 d . . . C4 C 0.1761(12) 0.1350(2) 0.4507(7) 0.0265(19) Uani 1 1 d . . . C5A C 0.231(3) 0.0605(7) 0.4517(17) 0.047(5) Uani 0.50 1 d PD . . H5A1 H 0.2116 0.0377 0.4169 0.056 Uiso 0.50 1 calc PR . . H5A2 H 0.3582 0.0618 0.4707 0.056 Uiso 0.50 1 calc PR . . C5B C 0.111(3) 0.0612(7) 0.4554(17) 0.047(5) Uani 0.50 1 d PD . . H5B1 H -0.0161 0.0644 0.4743 0.056 Uiso 0.50 1 calc PR . . H5B2 H 0.1211 0.0379 0.4216 0.056 Uiso 0.50 1 calc PR . . Fe1 Fe 0.5000 0.0000 0.2500 0.0621(11) Uani 1 4 d S . . Br1 Br 0.3115(3) 0.03670(5) 0.15444(14) 0.1021(7) 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 I1 0.0378(4) 0.0251(4) 0.0371(4) 0.0118(3) -0.0027(3) 0.0004(3) Se1 0.0474(6) 0.0208(5) 0.0212(5) -0.0009(3) -0.0006(4) 0.0002(5) Se2 0.0407(6) 0.0196(5) 0.0256(5) -0.0014(3) 0.0010(4) -0.0003(4) S1 0.0558(17) 0.0191(12) 0.0379(13) -0.0055(10) 0.0054(13) -0.0016(12) C1 0.036(8) 0.023(7) 0.024(6) 0.000 0.000 -0.005(6) C2 0.029(7) 0.017(6) 0.022(6) 0.000 0.000 0.002(6) C3 0.028(5) 0.011(4) 0.027(4) 0.004(3) 0.007(4) 0.000(4) C4 0.028(5) 0.014(4) 0.037(5) 0.000(4) 0.007(4) 0.004(4) C5A 0.066(14) 0.028(7) 0.048(8) 0.010(6) -0.002(13) 0.003(14) C5B 0.066(14) 0.028(7) 0.048(8) 0.010(6) -0.002(13) 0.003(14) Fe1 0.107(3) 0.0199(16) 0.059(2) 0.000 0.000 0.000 Br1 0.1625(19) 0.0403(8) 0.1035(14) 0.0144(9) -0.0349(13) 0.0086(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 C3 2.065(8) . ? Se1 C3 1.883(8) . ? Se1 C1 1.895(7) . ? Se2 C2 1.873(6) . ? Se2 C4 1.911(9) . ? S1 C4 1.731(9) . ? S1 C5A 1.79(2) . ? S1 C5B 1.83(2) . ? C1 C2 1.352(18) . ? C1 Se1 1.895(7) 10_556 ? C2 Se2 1.873(6) 10_556 ? C3 C3 1.342(17) 10_556 ? C4 C4 1.337(18) 10_556 ? C5A C5B 1.535(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.535(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? Fe1 Br1 2.3209(18) 7_545 ? Fe1 Br1 2.3209(18) 2_655 ? Fe1 Br1 2.3209(18) . ? Fe1 Br1 2.3209(18) 8_445 ? 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 C3 Se1 C1 93.9(4) . . ? C2 Se2 C4 93.6(4) . . ? C4 S1 C5A 102.8(9) . . ? C4 S1 C5B 100.7(8) . . ? C5A S1 C5B 28.0(7) . . ? C2 C1 Se1 123.0(3) . 10_556 ? C2 C1 Se1 123.0(3) . . ? Se1 C1 Se1 113.9(7) 10_556 . ? C1 C2 Se2 122.2(3) . . ? C1 C2 Se2 122.2(3) . 10_556 ? Se2 C2 Se2 115.6(6) . 10_556 ? C3 C3 Se1 119.1(2) 10_556 . ? C3 C3 I1 124.7(2) 10_556 . ? Se1 C3 I1 116.1(4) . . ? C4 C4 S1 128.5(3) 10_556 . ? C4 C4 Se2 118.6(3) 10_556 . ? S1 C4 Se2 112.9(5) . . ? C5B C5A S1 111.4(18) 10_556 . ? C5B C5A H5A1 109.3 10_556 . ? S1 C5A H5A1 109.3 . . ? C5B C5A H5A2 109.3 10_556 . ? S1 C5A H5A2 109.3 . . ? H5A1 C5A H5A2 108.0 . . ? C5A C5B S1 111.6(19) 10_556 . ? C5A C5B H5B1 109.3 10_556 . ? S1 C5B H5B1 109.3 . . ? C5A C5B H5B2 109.3 10_556 . ? S1 C5B H5B2 109.3 . . ? H5B1 C5B H5B2 108.0 . . ? Br1 Fe1 Br1 107.08(11) 7_545 2_655 ? Br1 Fe1 Br1 109.31(10) 7_545 . ? Br1 Fe1 Br1 112.07(11) 2_655 . ? Br1 Fe1 Br1 112.07(11) 7_545 8_445 ? Br1 Fe1 Br1 109.31(10) 2_655 8_445 ? Br1 Fe1 Br1 107.08(11) . 8_445 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.646 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.294 # Attachment '7d-revised.cif' data_(DIETSe)2GaBr4 _database_code_depnum_ccdc_archive 'CCDC 604646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H8 Br4 Fe I4 S4 Se8' _chemical_formula_weight 1843.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ibam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' _cell_length_a 7.3241(17) _cell_length_b 36.602(9) _cell_length_c 13.580(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3640.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 2193 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 26.30 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 16.438 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0835 _exptl_absorpt_correction_T_max 0.8529 _exptl_absorpt_process_details ; XPREP; Bruker AXS, 2003 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number 81 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13002 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.37 _reflns_number_total 2369 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0800P)^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 2369 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 0.18204(7) 0.364608(15) 0.36401(4) 0.0372(2) Uani 1 1 d . . . Se1 Se 0.17000(11) 0.27339(2) 0.38297(6) 0.0326(2) Uani 1 1 d . . . Se2 Se 0.17534(11) 0.18092(2) 0.38324(6) 0.0317(2) Uani 1 1 d . . . S1 S 0.1758(3) 0.09791(6) 0.37133(16) 0.0395(5) Uani 1 1 d . . . C1 C 0.1715(14) 0.2450(3) 0.5000 0.031(2) Uani 1 2 d S . . C2 C 0.1735(13) 0.2086(3) 0.5000 0.028(2) Uani 1 2 d S . . C3 C 0.1759(9) 0.31821(18) 0.4513(5) 0.0246(16) Uani 1 1 d . . . C4 C 0.1761(9) 0.1354(2) 0.4511(6) 0.0313(17) Uani 1 1 d . . . C5A C 0.234(3) 0.0609(7) 0.4548(15) 0.057(5) Uani 0.50 1 d PD . . H5A1 H 0.2153 0.0377 0.4217 0.068 Uiso 0.50 1 calc PR . . H5A2 H 0.3626 0.0626 0.4720 0.068 Uiso 0.50 1 calc PR . . C5B C 0.119(3) 0.0619(7) 0.4507(18) 0.057(5) Uani 0.50 1 d PD . . H5B1 H -0.0087 0.0641 0.4686 0.068 Uiso 0.50 1 calc PR . . H5B2 H 0.1345 0.0390 0.4158 0.068 Uiso 0.50 1 calc PR . . GA1 Fe 0.5000 0.0000 0.2500 0.0418(6) Uani 1 4 d S . . Br1 Br 0.3129(2) 0.03652(4) 0.15454(12) 0.1033(6) 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 I1 0.0416(3) 0.0288(3) 0.0413(3) 0.0113(2) -0.0032(2) 0.0003(2) Se1 0.0491(5) 0.0233(4) 0.0254(4) -0.0007(3) -0.0004(3) 0.0001(4) Se2 0.0431(5) 0.0226(4) 0.0295(4) -0.0006(3) 0.0010(3) -0.0006(3) S1 0.0545(13) 0.0235(10) 0.0404(11) -0.0055(9) 0.0044(10) -0.0023(10) C1 0.034(6) 0.032(6) 0.028(5) 0.000 0.000 0.000(5) C2 0.033(6) 0.023(6) 0.029(5) 0.000 0.000 0.006(5) C3 0.028(4) 0.018(4) 0.028(4) 0.004(3) 0.003(3) -0.004(3) C4 0.036(4) 0.020(4) 0.038(4) 0.005(3) 0.003(3) 0.002(3) C5A 0.093(16) 0.024(6) 0.052(7) 0.009(5) -0.023(14) -0.002(13) C5B 0.093(16) 0.024(6) 0.052(7) 0.009(5) -0.023(14) -0.002(13) GA1 0.0782(18) 0.0078(10) 0.0395(13) 0.000 0.000 0.000 Br1 0.1621(15) 0.0434(7) 0.1044(12) 0.0140(8) -0.0378(10) 0.0072(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 I1 C3 2.071(7) . ? Se1 C3 1.885(7) . ? Se1 C1 1.899(7) . ? Se2 C2 1.882(6) . ? Se2 C4 1.905(7) . ? S1 C4 1.747(8) . ? S1 C5B 1.75(2) . ? S1 C5A 1.82(2) . ? C1 C2 1.333(16) . ? C1 Se1 1.899(7) 10_556 ? C2 Se2 1.882(6) 10_556 ? C3 C3 1.324(14) 10_556 ? C4 C4 1.329(16) 10_556 ? C5A C5B 1.537(7) 10_556 ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C5B C5A 1.537(7) 10_556 ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? GA1 Br1 2.3117(14) 7_545 ? GA1 Br1 2.3117(14) 8_445 ? GA1 Br1 2.3117(14) . ? GA1 Br1 2.3117(14) 2_655 ? 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 C3 Se1 C1 93.7(4) . . ? C2 Se2 C4 93.7(4) . . ? C4 S1 C5B 102.1(9) . . ? C4 S1 C5A 101.4(8) . . ? C5B S1 C5A 27.4(7) . . ? C2 C1 Se1 123.2(3) . 10_556 ? C2 C1 Se1 123.2(3) . . ? Se1 C1 Se1 113.7(6) 10_556 . ? C1 C2 Se2 122.6(3) . 10_556 ? C1 C2 Se2 122.6(3) . . ? Se2 C2 Se2 114.8(6) 10_556 . ? C3 C3 Se1 119.5(2) 10_556 . ? C3 C3 I1 124.9(2) 10_556 . ? Se1 C3 I1 115.6(3) . . ? C4 C4 S1 128.3(3) 10_556 . ? C4 C4 Se2 118.9(2) 10_556 . ? S1 C4 Se2 112.8(4) . . ? C5B C5A S1 111.9(18) 10_556 . ? C5B C5A H5A1 109.2 10_556 . ? S1 C5A H5A1 109.2 . . ? C5B C5A H5A2 109.2 10_556 . ? S1 C5A H5A2 109.2 . . ? H5A1 C5A H5A2 107.9 . . ? C5A C5B S1 113.7(18) 10_556 . ? C5A C5B H5B1 108.8 10_556 . ? S1 C5B H5B1 108.8 . . ? C5A C5B H5B2 108.8 10_556 . ? S1 C5B H5B2 108.8 . . ? H5B1 C5B H5B2 107.7 . . ? Br1 GA1 Br1 111.78(9) 7_545 8_445 ? Br1 GA1 Br1 109.35(8) 7_545 . ? Br1 GA1 Br1 107.31(9) 8_445 . ? Br1 GA1 Br1 107.31(9) 7_545 2_655 ? Br1 GA1 Br1 109.35(8) 8_445 2_655 ? Br1 GA1 Br1 111.78(9) . 2_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.625 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.246