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#$Date: 2019-11-25 13:40:15 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240994 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/05/4130594.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_4130594
loop_
_publ_author_name
'Postulka, Lars'
'Winter, Stephen M.'
'Mihailov, Adam G.'
'Mailman, Aaron'
'Assoud, Abdeljalil'
'Robertson, Craig M.'
'Wolf, Bernd'
'Lang, Michael'
'Oakley, Richard T.'
_publ_section_title
;
 Spin Frustration in an Organic Radical Ion Salt Based on a Kagome-Coupled
 Chain Structure.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10738
_journal_page_last               10741
_journal_paper_doi               10.1021/jacs.6b05079
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C6 Cl2 N2 S4, Ga Br4'
_chemical_formula_sum            'C6 Br4 Cl2 Ga N2 S4'
_chemical_formula_weight         688.58
_chemical_name_common            '[QT][GaBr4]'
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.6489(4)
_cell_length_b                   13.6489(4)
_cell_length_c                   7.9023(3)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      1.5
_cell_volume                     1274.91(7)
_computing_cell_refinement       'SMART, 'Bruker APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'SAINT, 'Bruker APEX II'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEX II'
_diffrn_measurement_method       'Omega scan'
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16656
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         1.723
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.811
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.691
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             957
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 1230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.078(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0123P)²+4.4021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                3060
_reflns_number_total             4045
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b05079_si_003.cif
_cod_data_source_block           '[Kagome][GaBr4]100k'
_cod_original_cell_volume        1274.91(9)
_cod_database_code               4130594
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.452
_shelx_estimated_absorpt_t_max   0.798
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br6 Br 0.58355(11) 0.14731(11) 1.20066(17) 0.0512(4) Uani 1 1 d . . .
Br2 Br 0.3333 0.6667 0.3704(3) 0.0497(5) Uani 1 3 d S T P
Br3 Br 0.0000 0.0000 -0.5827(3) 0.0522(6) Uani 1 3 d S T P
Br5 Br 0.6667 0.3333 1.5838(3) 0.0579(6) Uani 1 3 d S T P
Br4 Br 0.07842(12) 0.18591(12) -0.1981(2) 0.0587(4) Uani 1 1 d . . .
Br1 Br 0.17273(13) 0.50676(13) -0.0248(2) 0.0702(4) Uani 1 1 d . . .
Ga3 Ga 0.6667 0.3333 1.2929(3) 0.0380(5) Uani 1 3 d S T P
Ga2 Ga 0.0000 0.0000 -0.2892(3) 0.0399(5) Uani 1 3 d S T P
Ga1 Ga 0.3333 0.6667 0.0746(3) 0.0397(5) Uani 1 3 d S T P
Cl2 Cl 0.4321(3) 0.1666(3) 0.8587(5) 0.0637(9) Uani 1 1 d . . .
Cl1 Cl 0.2389(3) 0.2283(3) 0.1727(4) 0.0599(9) Uani 1 1 d . . .
S2 S 0.4074(3) 0.3833(3) 0.7932(4) 0.0569(9) Uani 1 1 d . . .
S3 S 0.2677(3) 0.0143(3) 0.2335(5) 0.0625(10) Uani 1 1 d . . .
S1 S 0.3557(3) 0.4678(3) 0.6326(5) 0.0588(9) Uani 1 1 d . . .
S4 S 0.3226(4) -0.0685(3) 0.3961(6) 0.0751(12) Uani 1 1 d . . .
N1 N 0.3171(8) 0.3882(9) 0.4758(13) 0.042(2) Uani 1 1 d . . .
N2 N 0.3590(10) 0.0066(11) 0.5526(15) 0.063(3) Uani 1 1 d . . .
C1 C 0.3239(9) 0.2943(10) 0.4898(15) 0.039(3) Uani 1 1 d . . .
C4 C 0.3504(10) 0.1032(10) 0.5371(17) 0.043(3) Uani 1 1 d . . .
C6 C 0.3698(10) 0.2745(11) 0.6452(16) 0.043(3) Uani 1 1 d . . .
C5 C 0.3778(10) 0.1814(11) 0.6663(15) 0.042(3) Uani 1 1 d . . .
C2 C 0.2911(9) 0.2099(10) 0.3597(14) 0.036(3) Uani 1 1 d . . .
C3 C 0.3029(9) 0.1179(10) 0.3813(15) 0.038(3) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br5 Ga3 Br6 108.31(7) . .
Br5 Ga3 Br6 108.31(7) . 2_655
Br6 Ga3 Br6 110.61(6) . 2_655
Br5 Ga3 Br6 108.31(7) . 3_665
Br6 Ga3 Br6 110.61(6) . 3_665
Br6 Ga3 Br6 110.61(6) 2_655 3_665
Br3 Ga2 Br4 108.06(7) . 2
Br3 Ga2 Br4 108.06(7) . 3
Br4 Ga2 Br4 110.85(7) 2 3
Br3 Ga2 Br4 108.06(7) . .
Br4 Ga2 Br4 110.85(7) 2 .
Br4 Ga2 Br4 110.84(7) 3 .
Br1 Ga1 Br1 109.18(7) 3_565 2_665
Br1 Ga1 Br1 109.18(7) 3_565 .
Br1 Ga1 Br1 109.18(7) 2_665 .
Br1 Ga1 Br2 109.76(7) 3_565 .
Br1 Ga1 Br2 109.76(7) 2_665 .
Br1 Ga1 Br2 109.76(7) . .
C6 S2 S1 91.5(5) . .
C3 S3 S4 89.9(4) . .
N1 S1 S2 101.0(4) . .
N2 S4 S3 102.7(5) . .
C1 N1 S1 116.3(9) . .
C4 N2 S4 114.4(10) . .
N1 C1 C2 124.5(11) . .
N1 C1 C6 119.2(11) . .
C2 C1 C6 116.2(10) . .
C5 C4 N2 123.2(12) . .
C5 C4 C3 119.1(10) . .
N2 C4 C3 117.5(12) . .
C5 C6 C1 121.7(12) . .
C5 C6 S2 126.3(10) . .
C1 C6 S2 112.0(9) . .
C6 C5 C4 121.3(11) . .
C6 C5 Cl2 117.3(10) . .
C4 C5 Cl2 121.2(10) . .
C3 C2 C1 121.3(10) . .
C3 C2 Cl1 119.7(10) . .
C1 C2 Cl1 119.0(9) . .
C2 C3 C4 120.2(11) . .
C2 C3 S3 124.5(10) . .
C4 C3 S3 115.2(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br6 Ga3 2.3205(15) .
Br2 Ga1 2.337(3) .
Br3 Ga2 2.319(3) .
Br5 Ga3 2.298(4) .
Br4 Ga2 2.3208(16) .
Br1 Ga1 2.3242(16) .
Ga3 Br6 2.3205(15) 2_655
Ga3 Br6 2.3205(15) 3_665
Ga2 Br4 2.3207(16) 2
Ga2 Br4 2.3207(16) 3
Ga1 Br1 2.3242(16) 3_565
Ga1 Br1 2.3242(16) 2_665
Cl2 C5 1.747(12) .
Cl1 C2 1.712(11) .
S2 C6 1.753(13) .
S2 S1 2.063(5) .
S3 C3 1.707(12) .
S3 S4 2.083(6) .
S1 N1 1.556(11) .
S4 N2 1.523(14) .
N1 C1 1.335(14) .
N2 C4 1.388(17) .
C1 C2 1.439(16) .
C1 C6 1.464(17) .
C4 C5 1.386(17) .
C4 C3 1.451(17) .
C6 C5 1.339(17) .
C2 C3 1.354(16) .
