#------------------------------------------------------------------------------
#$Date: 2019-11-22 22:54:17 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231497 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/32/4003293.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_4003293
loop_
_publ_author_name
'Kawaguchi, Genta'
'Maesato, Mitsuhiko'
'Komatsu, Tokutaro'
'Imakubo, Tatsuro'
'Kiswandhi, Andhika'
'Graf, David'
'Kitagawa, Hiroshi'
_publ_section_title
;
 Use of Halogen Bonding in a Molecular Solid Solution to Simultaneously
 Control Spin and Charge
;
_journal_issue                   20
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7276
_journal_paper_doi               10.1021/acs.chemmater.6b02495
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         '2(C8 H4 I2 S2 Se4), Cl4 Ga'
_chemical_formula_sum            'C16 H8 Cl4 Ga I4 S4 Se8'
_chemical_formula_weight         1679.26
_chemical_name_common            (DIETSe)2GaCl4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.339(2)
_cell_length_b                   35.846(11)
_cell_length_c                   13.576(4)
_cell_measurement_reflns_used    4316
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.27
_cell_volume                     3571.5(18)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9856
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.551
_diffrn_reflns_theta_min         1.136
_diffrn_source                   'rotating anode with a mirror focusing unit'
_exptl_absorpt_coefficient_mu    12.928
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3004
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0401P)²+8.0461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1803
_reflns_number_total             2248
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm6b02495_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3571.4(19)
_cod_database_code               4003293
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, 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
I1 I 0.17943(3) 0.36731(2) 0.36395(2) 0.03789(10) Uani 1 1 d . . .
Se1 Se 0.16802(5) 0.27401(2) 0.38281(3) 0.03309(12) Uani 1 1 d . . .
Se2 Se 0.17220(5) 0.17938(2) 0.38308(3) 0.03256(12) Uani 1 1 d . . .
Ga1 Ga 0.5000 0.0000 0.2500 0.0634(3) Uani 1 4 d S T P
Cl1 Cl 0.3258(3) 0.03494(4) 0.16030(15) 0.1016(6) Uani 1 1 d . . .
S1 S 0.17225(14) 0.09443(3) 0.37104(7) 0.0422(2) Uani 1 1 d . . .
C1 C 0.1692(6) 0.24551(14) 0.5000 0.0299(10) Uani 1 2 d S T P
C2 C 0.1708(6) 0.20751(13) 0.5000 0.0285(10) Uani 1 2 d S T P
C3 C 0.1744(4) 0.31986(9) 0.4505(2) 0.0282(7) Uani 1 1 d . . .
C4 C 0.1746(4) 0.13290(9) 0.4508(3) 0.0315(7) Uani 1 1 d . . .
C5A C 0.1038(17) 0.0570(3) 0.4551(8) 0.062(3) Uani 0.5 1 d . . P
C5B C 0.2238(19) 0.0561(3) 0.4556(9) 0.067(3) Uani 0.5 1 d . . P
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'
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
C3 Se1 C1 93.49(16) . .
C2 Se2 C4 93.56(17) . .
Cl1 Ga1 Cl1 109.30(10) . 3_655
Cl1 Ga1 Cl1 107.60(11) . 4
Cl1 Ga1 Cl1 111.54(11) 3_655 4
Cl1 Ga1 Cl1 111.54(11) . 2_655
Cl1 Ga1 Cl1 107.60(11) 3_655 2_655
Cl1 Ga1 Cl1 109.30(10) 4 2_655
C4 S1 C5B 101.6(4) . .
C4 S1 C5A 101.2(4) . .
C5B S1 C5A 27.9(4) . .
C2 C1 Se1 122.70(13) . 10_556
C2 C1 Se1 122.70(13) . .
Se1 C1 Se1 114.6(3) 10_556 .
C1 C2 Se2 122.43(12) . 10_556
C1 C2 Se2 122.43(12) . .
Se2 C2 Se2 115.1(2) 10_556 .
C3 C3 Se1 119.19(10) 10_556 .
C3 C3 I1 124.62(9) 10_556 .
Se1 C3 I1 116.19(16) . .
C4 C4 S1 128.13(12) 10_556 .
C4 C4 Se2 118.87(11) 10_556 .
S1 C4 Se2 113.0(2) . .
C5B C5A C5A 89.6(13) . 10_556
C5B C5A C5B 53.6(15) . 10_556
C5A C5A C5B 36.0(5) 10_556 10_556
C5B C5A S1 75.9(11) . .
C5A C5A S1 128.5(3) 10_556 .
C5B C5A S1 111.0(7) 10_556 .
C5A C5B C5B 90.4(13) . 10_556
C5A C5B C5A 54.4(14) . 10_556
C5B C5B C5A 36.0(5) 10_556 10_556
C5A C5B S1 76.2(12) . .
C5B C5B S1 128.8(3) 10_556 .
C5A C5B S1 111.7(8) 10_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 C3 2.067(3) .
Se1 C3 1.883(3) .
Se1 C1 1.891(3) .
Se2 C2 1.881(3) .
Se2 C4 1.903(3) .
Ga1 Cl1 2.1647(16) .
Ga1 Cl1 2.1647(16) 3_655
Ga1 Cl1 2.1647(16) 4
Ga1 Cl1 2.1647(16) 2_655
S1 C4 1.753(4) .
S1 C5B 1.829(11) .
S1 C5A 1.831(11) .
C1 C2 1.362(7) .
C1 Se1 1.891(3) 10_556
C2 Se2 1.881(3) 10_556
C3 C3 1.345(7) 10_556
C4 C4 1.337(7) 10_556
C5A C5B 0.881(14) .
C5A C5A 1.22(2) 10_556
C5A C5B 1.500(12) 10_556
C5B C5B 1.21(2) 10_556
C5B C5A 1.500(12) 10_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C3 Se1 C1 C2 -178.1(4) . .
C3 Se1 C1 Se1 1.8(2) . 10_556
Se1 C1 C2 Se2 -0.1(6) 10_556 10_556
Se1 C1 C2 Se2 179.9(2) . 10_556
Se1 C1 C2 Se2 -179.9(2) 10_556 .
Se1 C1 C2 Se2 0.1(6) . .
C4 Se2 C2 C1 179.8(4) . .
C4 Se2 C2 Se2 0.0(2) . 10_556
C1 Se1 C3 C3 -1.14(15) . 10_556
C1 Se1 C3 I1 179.21(18) . .
C5B S1 C4 C4 -12.8(4) . 10_556
C5A S1 C4 C4 15.7(4) . 10_556
C5B S1 C4 Se2 168.5(4) . .
C5A S1 C4 Se2 -163.0(4) . .
C4 S1 C5A C5B -93.7(12) . .
C4 S1 C5A C5A -15.8(4) . 10_556
C5B S1 C5A C5A 77.9(12) . 10_556
C4 S1 C5A C5B -52.4(8) . 10_556
C5B S1 C5A C5B 41.2(11) . 10_556
C5A C5A C5B C5B -0.009(3) 10_556 10_556
S1 C5A C5B C5B 130.09(19) . 10_556
C5B C5A C5B C5A 0.009(5) 10_556 10_556
S1 C5A C5B C5A 130.10(19) . 10_556
C5A C5A C5B S1 -130.10(19) 10_556 .
C5B C5A C5B S1 -130.09(19) 10_556 .
C4 S1 C5B C5A 92.1(12) . .
C4 S1 C5B C5B 12.9(4) . 10_556
C5A S1 C5B C5B -79.2(11) . 10_556
C4 S1 C5B C5A 50.0(8) . 10_556
C5A S1 C5B C5A -42.1(10) . 10_556
