#------------------------------------------------------------------------------ #$Date: 2019-07-12 11:11:15 +0300 (Fri, 12 Jul 2019) $ #$Revision: 216971 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552094.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_1552094 loop_ _publ_author_name 'Jack Rumble' 'Paz Vaqueiro' _publ_section_title ; Na5(Ga4S)(GaS4)3 6H2O: A three-dimensional gallium sulphide containing a novel octahedral building block ; _journal_name_full 'Solid State Sciences' _journal_page_first 1137 _journal_page_last 1142 _journal_paper_doi 10.1016/j.solidstatesciences.2011.01.003 _journal_volume 13 _journal_year 2011 _chemical_absolute_configuration ad _chemical_formula_moiety 'Ga7 H12 Na5 O6 S13' _chemical_formula_sum 'Ga7 H12 Na5 O6 S13' _chemical_formula_weight 1127.94 _space_group_IT_number 219 _space_group_name_Hall 'F -4a 2 3' _space_group_name_H-M_alt 'F -4 3 c' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F -4 3 c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.577(4) _cell_length_b 17.577(4) _cell_length_c 17.577(4) _cell_measurement_reflns_used 0 _cell_measurement_temperature 290 _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _cell_volume 5430(2) _computing_cell_refinement 'APEX 2 (Bruker, 2005)' _computing_data_collection 'APEX 2 (Bruker, 2005)' _computing_data_reduction 'APEX 2 (Bruker, 2005)' _computing_molecular_graphics 'ATOMS (Dowty, 2000)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 290 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type ; Bruker-Nonius APEX-2 CCD area-detector diffractometer ; _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 2205 _diffrn_reflns_theta_full 25.882 _diffrn_reflns_theta_max 26.410 _diffrn_reflns_theta_min 3.278 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.940 _exptl_absorpt_correction_T_max 0.8532 _exptl_absorpt_correction_T_min 0.7880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.759 _exptl_crystal_description block _exptl_crystal_F_000 4320.000 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.20 _refine_diff_density_min -1.47 _refine_ls_abs_structure_details 'Flack, 195 Friedel-pairs' _refine_ls_abs_structure_Flack 0.07(5) _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.1206 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.000030 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.300 -0.749E-02 0.967E-01 -0.995E-02 0.527E-01 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0639 _refine_ls_wR_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0313 _reflns_limit_h_max 12 _reflns_limit_h_min -12 _reflns_limit_k_max 14 _reflns_limit_k_min 0 _reflns_limit_l_max 21 _reflns_limit_l_min 2 _reflns_number_gt 277 _reflns_number_total 472 _reflns_threshold_expression I>2.00u(I) _oxford_diffrn_Wilson_B_factor 1.50 _oxford_diffrn_Wilson_scale 2138.21 _oxford_refine_ls_scale 0.02258(8) _cod_data_source_file Solid-State-Science-2011-13-1137.cif _cod_data_source_block CRYSTALS_cif _cod_depositor_comments ; The following automatic conversions were performed: data item '_symmetry_cell_setting' value 'Cubic' was changed to 'cubic' in accordance with the built-in table derived from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated on 2014-11-21. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_sg_symbol_H-M 'F -4 3 c ' _cod_database_code 1552094 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,y+1/2,z+1/2 x+1/2,y,z+1/2 x+1/2,y+1/2,z y,z,x y,z+1/2,x+1/2 y+1/2,z,x+1/2 y+1/2,z+1/2,x z,x,y z,x+1/2,y+1/2 z+1/2,x,y+1/2 z+1/2,x+1/2,y y+1/2,-x+1/2,-z+1/2 y+1/2,-x+1,-z+1 y+1,-x+1/2,-z+1 y+1,-x+1,-z+1/2 z+1/2,-y+1/2,-x+1/2 z+1/2,-y+1,-x+1 z+1,-y+1/2,-x+1 z+1,-y+1,-x+1/2 x+1/2,-z+1/2,-y+1/2 x+1/2,-z+1,-y+1 x+1,-z+1/2,-y+1 x+1,-z+1,-y+1/2 -x,-y,z -x,-y+1/2,z+1/2 -x+1/2,-y,z+1/2 -x+1/2,-y+1/2,z -z,x,-y -z,x+1/2,-y+1/2 -z+1/2,x,-y+1/2 -z+1/2,x+1/2,-y -x,y,-z -x,y+1/2,-z+1/2 -x+1/2,y,-z+1/2 -x+1/2,y+1/2,-z -y,-z,x -y,-z+1/2,x+1/2 -y+1/2,-z,x+1/2 -y+1/2,-z+1/2,x -z,-x,y -z,-x+1/2,y+1/2 -z+1/2,-x,y+1/2 -z+1/2,-x+1/2,y -y+1/2,x+1/2,-z+1/2 -y+1/2,x+1,-z+1 -y+1,x+1/2,-z+1 -y+1,x+1,-z+1/2 -z+1/2,y+1/2,-x+1/2 -z+1/2,y+1,-x+1 -z+1,y+1/2,-x+1 -z+1,y+1,-x+1/2 -x+1/2,z+1/2,-y+1/2 -x+1/2,z+1,-y+1 -x+1,z+1/2,-y+1 -x+1,z+1,-y+1/2 -y,z,-x -y,z+1/2,-x+1/2 -y+1/2,z,-x+1/2 -y+1/2,z+1/2,-x z+1/2,y+1/2,x+1/2 z+1/2,y+1,x+1 z+1,y+1/2,x+1 z+1,y+1,x+1/2 x+1/2,z+1/2,y+1/2 x+1/2,z+1,y+1 x+1,z+1/2,y+1 x+1,z+1,y+1/2 y+1/2,x+1/2,z+1/2 y+1/2,x+1,z+1 y+1,x+1/2,z+1 y+1,x+1,z+1/2 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+1/2,-x+1/2,z+1/2 -y+1/2,-x+1,z+1 -y+1,-x+1/2,z+1 -y+1,-x+1,z+1/2 -z+1/2,-y+1/2,x+1/2 -z+1/2,-y+1,x+1 -z+1,-y+1/2,x+1 -z+1,-y+1,x+1/2 -x+1/2,-z+1/2,y+1/2 -x+1/2,-z+1,y+1 -x+1,-z+1/2,y+1 -x+1,-z+1,y+1/2 x,-y,-z x,-y+1/2,-z+1/2 x+1/2,-y,-z+1/2 x+1/2,-y+1/2,-z z,-x,-y z,-x+1/2,-y+1/2 z+1/2,-x,-y+1/2 z+1/2,-x+1/2,-y 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ga1 Ga 0.0000 0.2500 0.2500 0.0145 1.0000 Uani S T . . . . Ga2 Ga 0.17157(6) 0.17157(6) 0.32843(6) 0.0136 1.0000 Uani S T . . . . S3 S 0.06842(15) 0.14021(14) 0.25982(15) 0.0162 1.0000 Uani . . . . . . S4 S 0.2500 0.2500 0.2500 0.0148 1.0000 Uani S T . . . . Na5 Na 0.1057(2) 0.1057(2) 0.1057(2) 0.0390 1.0000 Uani S T . . . . Na6 Na 0.0000 0.0000 0.0000 0.0234 1.0000 Uani S T . . . . O7 O 0.0000 0.0000 0.1326(6) 0.0333 1.0000 Uani S T . . . . H8 H -0.0158 0.0410 0.1579 0.0500 1.0000 Uiso 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 0.0115(10) 0.0160(6) 0.0160(6) 0.0000 0.0000 0.0000 Ga2 0.0136(4) 0.0136(4) 0.0136(4) -0.0001(5) -0.0001(5) 0.0001(5) S3 0.0122(13) 0.0138(13) 0.0227(16) -0.0017(11) -0.0035(13) 0.0014(9) S4 0.0148(15) 0.0148(15) 0.0148(15) 0.0000 0.0000 0.0000 Na5 0.039(2) 0.039(2) 0.039(2) -0.007(2) -0.007(2) -0.007(2) Na6 0.023(3) 0.023(3) 0.023(3) 0.0000 0.0000 0.0000 O7 0.068(15) 0.010(9) 0.022(6) 0.0000 0.0000 0.012(5) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S3 56_445 Ga1 . S3 90_555 106.15(6) yes S3 56_445 Ga1 . S3 87_454 116.34(14) yes S3 90_555 Ga1 . S3 87_454 106.15(6) yes S3 56_445 Ga1 . S3 . 106.15(7) yes S3 90_555 Ga1 . S3 . 116.34(14) yes S3 87_454 Ga1 . S3 . 106.15(6) yes S3 31_555 Ga2 . S3 74_555 111.53(7) yes S3 31_555 Ga2 . S3 . 111.53(7) yes S3 74_555 Ga2 . S3 . 111.53(7) yes S3 31_555 Ga2 . S4 . 107.32(8) yes S3 74_555 Ga2 . S4 . 107.32(8) yes S3 . Ga2 . S4 . 107.32(8) yes Ga1 . S3 . Ga2 . 104.99(10) yes Ga2 44_555 S4 . Ga2 9_555 109.471(16) yes Ga2 44_555 S4 . Ga2 . 109.471(16) yes Ga2 9_555 S4 . Ga2 . 109.471(16) yes Ga2 44_555 S4 . Ga2 28_555 109.471(16) yes Ga2 9_555 S4 . Ga2 28_555 109.471(16) yes Ga2 . S4 . Ga2 28_555 109.471(16) yes H8 25_555 O7 . H8 . 120.123 no loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . S3 56_445 2.280(2) yes Ga1 . S3 90_555 2.280(2) yes Ga1 . S3 87_454 2.280(2) yes Ga1 . S3 . 2.280(2) yes Ga2 . S3 31_555 2.246(3) yes Ga2 . S3 74_555 2.246(3) yes Ga2 . S3 . 2.246(3) yes Ga2 . S4 . 2.3877(18) yes O7 . H8 25_555 0.891 no O7 . H8 . 0.891 no