#------------------------------------------------------------------------------ #$Date: 2015-12-13 20:06:19 +0000 (Sun, 13 Dec 2015) $ #$Revision: 171491 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/08/4300864.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_4300864 loop_ _publ_author_name 'Richard T. Oakley' 'Robert W. Reed' 'Craig M. Robertson' 'John F. Richardson' _publ_section_title ; Naphthalene-1,2,3-Dithiazolyl and Its Selenium-Containing Variants ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1837 _journal_page_last 1845 _journal_paper_doi 10.1021/ic048534e _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C10 H6 Cl4 Ga N Se2' _chemical_formula_sum 'C10 H6 Cl4 Ga N Se2' _chemical_formula_weight 509.60 _chemical_name_common 'Se-Se-N gallate' _chemical_name_systematic ; 3H-naphtho[1,2-d][1,2,3]diselenazolylium tetrachlorogallate ; _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 100.530(7) _cell_angle_beta 104.778(8) _cell_angle_gamma 92.760(8) _cell_formula_units_Z 2 _cell_length_a 7.790(4) _cell_length_b 10.009(5) _cell_length_c 10.109(5) _cell_measurement_reflns_used 2318 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25.29 _cell_measurement_theta_min 2.65 _cell_volume 745.6(7) _computing_cell_refinement 'SAINT 6.22 (Bruker, 2001)' _computing_data_collection 'SMART 5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT 6.22 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-90 (Sheldrick, 1990)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.907 _diffrn_measured_fraction_theta_max 0.907 _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6767 _diffrn_reflns_theta_full 28.54 _diffrn_reflns_theta_max 28.54 _diffrn_reflns_theta_min 2.08 _diffrn_standards_decay_% <0.1 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.429 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_correction_T_min 0.406 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (George Sheldrick)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.069 _exptl_crystal_size_min 0.036 _refine_diff_density_max 0.614 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.115 _refine_ls_extinction_coef 0.0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 3453 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0444 _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^)+(0.0211P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.1117 _reflns_number_gt 2364 _reflns_number_total 3453 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048534esi20041220_010846_1.cif _[local]_cod_data_source_block rto10rt _[local]_cod_cif_authors_sg_Hall P-1 _cod_original_cell_volume 745.5(7) _cod_database_code 4300864 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 _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.12531(7) 0.20525(5) 0.40611(5) 0.04681(17) Uani 1 1 d . . . Se1 Se 0.55527(7) 0.33832(5) 0.28310(5) 0.05188(17) Uani 1 1 d . . . Se2 Se 0.57778(7) 0.11943(5) 0.17777(5) 0.05374(17) Uani 1 1 d . . . Cl2 Cl -0.10467(19) 0.18266(16) 0.48720(16) 0.0681(4) Uani 1 1 d . . . Cl1 Cl 0.35928(19) 0.13256(16) 0.52453(17) 0.0763(5) Uani 1 1 d . . . Cl4 Cl 0.0663(2) 0.09424(15) 0.19138(14) 0.0692(4) Uani 1 1 d . . . Cl3 Cl 0.1812(2) 0.42245(13) 0.41535(15) 0.0660(4) Uani 1 1 d . . . N1 N 0.4361(5) 0.1332(4) 0.0148(4) 0.0505(10) Uani 1 1 d . . . C4 C 0.1865(6) 0.3841(6) -0.1436(5) 0.0524(13) Uani 1 1 d . . . H4 H 0.1142 0.3924 -0.2298 0.063 Uiso 1 1 calc R . . C6 C 0.3336(6) 0.4907(5) 0.1028(5) 0.0428(11) Uani 1 1 d . . . C5 C 0.2231(6) 0.4986(5) -0.0297(5) 0.0478(12) Uani 1 1 d . . . C3 C 0.2534(6) 0.2651(5) -0.1297(5) 0.0510(12) Uani 1 1 d . . . H3 H 0.2259 0.1919 -0.2054 0.061 Uiso 1 1 calc R . . C2 C 0.3690(6) 0.2503(5) 0.0037(5) 0.0470(11) Uani 1 1 d . . . C1 C 0.4061(6) 0.3644(5) 0.1181(5) 0.0434(11) Uani 1 1 d . . . C7 C 0.3661(7) 0.6063(5) 0.2129(5) 0.0495(12) Uani 1 1 d . . . H7 H 0.4406 0.6028 0.3000 0.059 Uiso 1 1 calc R . . C8 C 0.2893(7) 0.7221(5) 0.1923(6) 0.0554(13) Uani 1 1 d . . . H8 H 0.3083 0.7965 0.2662 0.066 Uiso 1 1 calc R . . C10 C 0.1503(7) 0.6223(6) -0.0466(6) 0.0554(13) Uani 1 1 d . . . H10 H 0.0790 0.6298 -0.1335 0.066 Uiso 1 1 calc R . . C9 C 0.1822(7) 0.7306(6) 0.0613(6) 0.0578(14) Uani 1 1 d . . . H9 H 0.1322 0.8113 0.0480 0.069 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 Ga1 0.0461(3) 0.0446(3) 0.0475(3) 0.0046(2) 0.0116(2) 0.0068(2) Se1 0.0557(3) 0.0522(3) 0.0425(3) 0.0046(2) 0.0065(2) 0.0104(2) Se2 0.0538(3) 0.0514(3) 0.0533(3) 0.0080(2) 0.0101(2) 0.0118(2) Cl2 0.0595(8) 0.0777(10) 0.0761(9) 0.0217(8) 0.0296(7) 0.0094(7) Cl1 0.0587(9) 0.0767(10) 0.0817(10) 0.0154(8) -0.0034(7) 0.0158(8) Cl4 0.0826(10) 0.0638(9) 0.0516(8) -0.0052(6) 0.0106(7) 0.0182(7) Cl3 0.0803(10) 0.0455(7) 0.0731(9) 0.0039(6) 0.0287(8) 0.0016(7) N1 0.047(2) 0.055(3) 0.045(2) 0.0015(19) 0.0104(18) 0.009(2) C4 0.040(3) 0.069(4) 0.047(3) 0.008(3) 0.010(2) 0.012(3) C6 0.041(2) 0.047(3) 0.042(2) 0.006(2) 0.016(2) 0.004(2) C5 0.034(2) 0.059(3) 0.055(3) 0.018(2) 0.017(2) 0.006(2) C3 0.041(3) 0.061(3) 0.046(3) 0.001(2) 0.011(2) 0.005(2) C2 0.041(3) 0.057(3) 0.043(3) 0.005(2) 0.014(2) 0.003(2) C1 0.036(2) 0.052(3) 0.042(2) 0.006(2) 0.014(2) 0.004(2) C7 0.047(3) 0.052(3) 0.049(3) 0.009(2) 0.012(2) 0.004(2) C8 0.059(3) 0.042(3) 0.064(3) 0.002(2) 0.021(3) 0.005(2) C10 0.047(3) 0.066(4) 0.057(3) 0.019(3) 0.014(2) 0.017(3) C9 0.046(3) 0.061(3) 0.077(4) 0.026(3) 0.025(3) 0.016(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' N N 0.0061 0.0033 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ga1 Cl2 113.21(7) . . no Cl1 Ga1 Cl4 108.01(7) . . no Cl2 Ga1 Cl4 110.15(7) . . no Cl1 Ga1 Cl3 108.60(7) . . no Cl2 Ga1 Cl3 106.88(6) . . no Cl4 Ga1 Cl3 109.96(6) . . no C1 Se1 Se2 89.77(15) . . no N1 Se2 Se1 94.01(14) . . no C2 N1 Se2 118.0(3) . . no C3 C4 C5 121.9(5) . . no C3 C4 H4 119.1 . . no C5 C4 H4 119.1 . . no C5 C6 C7 119.1(5) . . no C5 C6 C1 117.5(4) . . no C7 C6 C1 123.4(4) . . no C10 C5 C6 118.3(5) . . no C10 C5 C4 120.8(5) . . no C6 C5 C4 120.9(5) . . no C4 C3 C2 120.1(5) . . no C4 C3 H3 120.0 . . no C2 C3 H3 120.0 . . no N1 C2 C1 122.4(4) . . no N1 C2 C3 119.2(4) . . no C1 C2 C3 118.3(5) . . no C6 C1 C2 121.3(4) . . no C6 C1 Se1 122.9(3) . . no C2 C1 Se1 115.8(4) . . no C8 C7 C6 120.3(5) . . no C8 C7 H7 119.8 . . no C6 C7 H7 119.8 . . no C7 C8 C9 120.6(5) . . no C7 C8 H8 119.7 . . no C9 C8 H8 119.7 . . no C9 C10 C5 121.2(5) . . no C9 C10 H10 119.4 . . no C5 C10 H10 119.4 . . no C10 C9 C8 120.5(5) . . no C10 C9 H9 119.8 . . no C8 C9 H9 119.8 . . no 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 Ga1 Cl1 2.1487(16) . no Ga1 Cl2 2.1703(17) . no Ga1 Cl4 2.1721(16) . no Ga1 Cl3 2.1767(18) . no Se1 C1 1.844(5) . no Se1 Se2 2.2900(12) . no Se2 N1 1.767(4) . no N1 C2 1.318(6) . no C4 C3 1.338(7) . no C4 C5 1.428(7) . no C4 H4 0.9300 . no C6 C5 1.413(6) . no C6 C7 1.414(6) . no C6 C1 1.427(7) . no C5 C10 1.407(7) . no C3 C2 1.456(7) . no C3 H3 0.9300 . no C2 C1 1.428(6) . no C7 C8 1.355(7) . no C7 H7 0.9300 . no C8 C9 1.394(7) . no C8 H8 0.9300 . no C10 C9 1.353(7) . no C10 H10 0.9300 . no C9 H9 0.9300 . no