#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:00:59 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 233540 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/90/4349009.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_4349009
loop_
_publ_author_name
'Nie, Lina'
'Zhang, Yu'
'Xiong, Wei-Wei'
'Lim, Teik-Thye'
'Xu, Rong'
'Yan, Qingyu'
'Zhang, Qichun'
_publ_section_title
;
 A surfactant-thermal method to prepare crystalline thioantimonate for
 high-performance lithium-ion batteries
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              111
_journal_paper_doi               10.1039/C5QI00194C
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C2 H7 N O0 S8 Sb4'
_chemical_formula_weight         788.57
_space_group_IT_number           40
_space_group_name_Hall           'A 2 -2a'
_space_group_name_H-M_alt        'A m a 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'A m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1k04tj
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-08 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0371(4)
_cell_length_b                   26.6752(13)
_cell_length_c                   5.9349(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1589.02(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    7.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73481
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.191
_refine_diff_density_min         -3.125
_refine_diff_density_rms         0.356
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1335
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0948P)²+69.7501P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                1293
_reflns_number_total             1335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5qi00194c2.cif
_cod_data_source_block           c
_cod_original_sg_symbol_H-M      Ama2
_cod_database_code               4349009
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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
Sb1 Sb 0.05226(9) 0.42968(4) 1.31284(17) 0.0248(3) Uani 1 1 d .
Sb2 Sb 0.2500 0.49087(7) 0.8582(3) 0.0350(5) Uani 1 2 d S
Sb3 Sb -0.2500 0.37448(12) 1.5593(6) 0.0712(9) Uani 1 2 d S
S1 S 0.2500 0.3766(2) 1.3726(11) 0.0281(13) Uani 1 2 d S
S2 S 0.0632(5) 0.43027(18) 0.8982(9) 0.0319(11) Uani 1 1 d .
S3 S -0.2500 0.2976(6) 1.794(2) 0.091(4) Uani 1 2 d S
S4 S -0.2500 0.3755(2) 1.0683(11) 0.0248(13) Uani 1 2 d S
S5 S -0.0707(4) 0.34889(17) 1.3126(12) 0.0390(11) Uani 1 1 d .
S6 S 0.2500 0.5162(3) 1.2447(12) 0.0331(15) Uani 1 2 d S
N1 N 0.2500 0.3175(11) 0.858(7) 0.066(9) Uani 1 2 d S
H1A H 0.2500 0.3474 0.9120 0.079 Uiso 1 2 calc SR
C1 C 0.126(2) 0.2912(9) 0.811(6) 0.065(7) Uani 1 1 d .
H1B H 0.0522 0.3121 0.8522 0.097 Uiso 1 1 calc R
H1C H 0.1233 0.2607 0.8961 0.097 Uiso 1 1 calc R
H1D H 0.1214 0.2836 0.6529 0.097 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
Sb1 0.0203(5) 0.0310(6) 0.0230(6) -0.0005(5) -0.0003(5) 0.0011(4)
Sb2 0.0426(9) 0.0375(9) 0.0248(8) 0.0054(8) 0.000 0.000
Sb3 0.0461(15) 0.0632(19) 0.104(2) -0.0175(16) 0.000 0.000
S1 0.019(2) 0.035(3) 0.030(3) 0.007(3) 0.000 0.000
S2 0.033(2) 0.041(3) 0.022(2) -0.001(2) -0.0075(17) 0.0015(17)
S3 0.060(5) 0.144(11) 0.068(7) 0.035(8) 0.000 0.000
S4 0.013(3) 0.027(3) 0.034(3) 0.018(3) 0.000 0.000
S5 0.0233(17) 0.033(2) 0.061(3) 0.006(3) 0.002(2) -0.0055(15)
S6 0.024(3) 0.042(4) 0.033(4) -0.004(3) 0.000 0.000
N1 0.053(15) 0.062(18) 0.08(2) -0.044(18) 0.000 0.000
C1 0.064(13) 0.051(12) 0.079(18) 0.012(15) 0.024(17) -0.001(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 '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
S2 Sb1 S1 96.4(2) . .
S2 Sb1 S5 91.5(2) . .
S1 Sb1 S5 84.33(15) . .
S6 Sb2 S2 95.30(17) . .
S6 Sb2 S2 95.30(17) . 4
S2 Sb2 S2 97.9(2) . 4
S5 Sb3 S5 96.2(3) 4_455 .
S5 Sb3 S3 96.2(3) 4_455 .
S5 Sb3 S3 96.2(3) . .
S5 Sb3 S4 52.94(17) 4_455 .
S5 Sb3 S4 52.94(17) . .
S3 Sb3 S4 124.8(4) . .
Sb1 S1 Sb1 107.3(2) 4 .
Sb1 S2 Sb2 97.64(18) . .
S5 S4 S5 96.2(3) . 4_455
S5 S4 Sb3 52.96(19) . .
S5 S4 Sb3 52.96(19) 4_455 .
S4 S5 Sb3 74.10(19) . .
S4 S5 Sb1 96.6(2) . .
Sb3 S5 Sb1 97.2(2) . .
C1 N1 C1 118(3) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 S2 2.464(5) .
Sb1 S1 2.464(4) .
Sb1 S5 2.483(4) .
Sb2 S6 2.391(7) .
Sb2 S2 2.487(5) .
Sb2 S2 2.487(5) 4
Sb3 S5 2.419(6) 4_455
Sb3 S5 2.419(6) .
Sb3 S3 2.480(14) .
Sb3 S4 2.915(7) .
S1 Sb1 2.464(4) 4
S4 S5 2.418(7) .
S4 S5 2.418(7) 4_455
N1 C1 1.45(3) .
N1 C1 1.45(3) 4
