#------------------------------------------------------------------------------
#$Date: 2017-07-22 04:41:50 +0300 (Sat, 22 Jul 2017) $
#$Revision: 198906 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/87/7228714.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_7228714
loop_
_publ_author_name
'Tran, Thao Thi-Phuong'
'Ould, Darren'
'Wilkins, Lewis'
'Wright, Dominic S.'
'Melen, Rebecca'
'Rawson, Jeremy Michael'
_publ_section_title
;
 Supramolecular Aggregation in Dithia-arsoles: Chlorides, Cations and
 N-centered Paddlewheels
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01117B
_journal_year                    2017
_chemical_formula_moiety         'C7 H6 As S2, Cl4 Ga'
_chemical_formula_sum            'C7 H6 As Cl4 Ga S2'
_chemical_formula_weight         440.68
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.483(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.409(4)
_cell_length_b                   7.015(2)
_cell_length_c                   17.742(6)
_cell_measurement_reflns_used    8763
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.35
_cell_volume                     1386.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0385
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15885
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_T_max  0.8999
_exptl_absorpt_correction_T_min  0.2947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
sadabs, Bruker AXS, Madison, WI, UA
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0218
_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)+(0.0237P)²+0.4876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3151
_reflns_number_total             3415
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce01117b2.cif
_cod_data_source_block           TT42
_cod_database_code               7228714
_shelx_shelxl_version_number     2014/7
_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   0.295
_shelx_estimated_absorpt_t_max   0.900
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
As1 As 0.31372(3) 0.7500 0.74010(2) 0.03375(9) Uani 1 2 d S T P
S11 S 0.43691(6) 0.7500 0.84990(4) 0.02276(14) Uani 1 2 d S T P
S12 S 0.45076(7) 0.7500 0.67414(4) 0.02949(16) Uani 1 2 d S T P
C11 C 0.5743(2) 0.7500 0.82366(15) 0.0181(5) Uani 1 2 d S T P
C12 C 0.6798(2) 0.7500 0.88096(15) 0.0222(5) Uani 1 2 d S T P
H12 H 0.6755 0.7500 0.9338 0.027 Uiso 1 2 calc R U P
C13 C 0.7899(3) 0.7500 0.86117(17) 0.0259(6) Uani 1 2 d S T P
C14 C 0.7941(3) 0.7500 0.78263(17) 0.0283(6) Uani 1 2 d S T P
H14 H 0.8700 0.7500 0.7688 0.034 Uiso 1 2 calc R U P
C15 C 0.6925(3) 0.7500 0.72571(16) 0.0256(6) Uani 1 2 d S T P
H15 H 0.6976 0.7500 0.6730 0.031 Uiso 1 2 calc R U P
C16 C 0.5804(2) 0.7500 0.74582(15) 0.0204(5) Uani 1 2 d S T P
C17 C 0.9042(3) 0.7500 0.92275(19) 0.0383(8) Uani 1 2 d S T P
H17A H 0.9371 0.6205 0.9291 0.057 Uiso 0.5 1 calc R U P
H17B H 0.8869 0.7937 0.9717 0.057 Uiso 0.5 1 calc R U P
H17C H 0.9627 0.8358 0.9074 0.057 Uiso 0.5 1 calc R U P
As2 As 0.07875(2) 0.7500 0.41713(2) 0.02204(7) Uani 1 2 d S T P
S21 S 0.01049(6) 0.7500 0.29453(4) 0.02313(14) Uani 1 2 d S T P
S22 S 0.26406(6) 0.7500 0.40871(4) 0.02069(14) Uani 1 2 d S T P
C21 C 0.1407(2) 0.7500 0.25907(15) 0.0177(5) Uani 1 2 d S T P
C22 C 0.1320(2) 0.7500 0.17888(15) 0.0233(6) Uani 1 2 d S T P
H22 H 0.0554 0.7500 0.1447 0.028 Uiso 1 2 calc R U P
C23 C 0.2346(2) 0.7500 0.14978(15) 0.0221(5) Uani 1 2 d S T P
C24 C 0.3470(2) 0.7500 0.20159(15) 0.0236(6) Uani 1 2 d S T P
H24 H 0.4179 0.7500 0.1817 0.028 Uiso 1 2 calc R U P
C25 C 0.3571(2) 0.7500 0.27984(15) 0.0214(5) Uani 1 2 d S T P
H25 H 0.4340 0.7500 0.3137 0.026 Uiso 1 2 calc R U P
C26 C 0.2530(2) 0.7500 0.30967(14) 0.0173(5) Uani 1 2 d S T P
C27 C 0.2270(3) 0.7500 0.06424(16) 0.0332(7) Uani 1 2 d S T P
H27A H 0.2878 0.6635 0.0521 0.050 Uiso 0.5 1 calc R U P
H27B H 0.2413 0.8793 0.0473 0.050 Uiso 0.5 1 calc R U P
H27C H 0.1470 0.7073 0.0375 0.050 Uiso 0.5 1 calc R U P
Ga1 Ga 0.22540(3) 0.2500 0.51627(2) 0.01862(8) Uani 1 2 d S T P
Cl11 Cl 0.41046(7) 0.2500 0.50944(5) 0.0459(2) Uani 1 2 d S T P
Cl12 Cl 0.10686(6) 0.2500 0.40203(4) 0.02375(14) Uani 1 2 d S T P
Cl13 Cl 0.17791(5) 0.50115(6) 0.57557(3) 0.02512(11) Uani 1 1 d . . .
Ga2 Ga 1.28118(3) 0.2500 0.86116(2) 0.02282(8) Uani 1 2 d S T P
Cl21 Cl 1.44677(7) 0.2500 0.94638(4) 0.0542(3) Uani 1 2 d S T P
Cl22 Cl 1.32549(6) 0.2500 0.74769(4) 0.02637(15) Uani 1 2 d S T P
Cl23 Cl 1.17415(5) 0.49964(7) 0.87164(3) 0.03629(13) 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
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'
As As 0.0499 2.0058 '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
S11 As1 S12 94.81(4) . .
C11 S11 As1 102.12(9) . .
C16 S12 As1 101.95(10) . .
C12 C11 C16 120.0(2) . .
C12 C11 S11 119.5(2) . .
C16 C11 S11 120.5(2) . .
C13 C12 C11 120.3(2) . .
C13 C12 H12 119.8 . .
C11 C12 H12 119.8 . .
C12 C13 C14 118.8(3) . .
C12 C13 C17 120.6(3) . .
C14 C13 C17 120.6(3) . .
C15 C14 C13 121.9(3) . .
C15 C14 H14 119.0 . .
C13 C14 H14 119.0 . .
C14 C15 C16 119.3(3) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
C15 C16 C11 119.7(2) . .
C15 C16 S12 119.7(2) . .
C11 C16 S12 120.6(2) . .
C13 C17 H17A 109.5 . .
C13 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C13 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
S21 As2 S22 94.38(3) . .
C21 S21 As2 102.48(9) . .
C26 S22 As2 102.28(9) . .
C26 C21 C22 120.4(2) . .
C26 C21 S21 120.37(19) . .
C22 C21 S21 119.3(2) . .
C23 C22 C21 120.0(3) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C22 C23 C24 118.9(2) . .
C22 C23 C27 120.7(3) . .
C24 C23 C27 120.3(3) . .
C25 C24 C23 121.8(3) . .
C25 C24 H24 119.1 . .
C23 C24 H24 119.1 . .
C24 C25 C26 119.4(2) . .
C24 C25 H25 120.3 . .
C26 C25 H25 120.3 . .
C21 C26 C25 119.5(2) . .
C21 C26 S22 120.49(19) . .
C25 C26 S22 120.0(2) . .
C23 C27 H27A 109.5 . .
C23 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C23 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
Cl11 Ga1 Cl12 111.63(4) . .
Cl11 Ga1 Cl13 112.24(2) . .
Cl12 Ga1 Cl13 106.25(2) . .
Cl11 Ga1 Cl13 112.24(2) . 4_565
Cl12 Ga1 Cl13 106.25(2) . 4_565
Cl13 Ga1 Cl13 107.86(4) . 4_565
Cl21 Ga2 Cl23 111.46(2) . 4_565
Cl21 Ga2 Cl23 111.46(2) . .
Cl23 Ga2 Cl23 107.92(4) 4_565 .
Cl21 Ga2 Cl22 107.80(4) . .
Cl23 Ga2 Cl22 109.09(2) 4_565 .
Cl23 Ga2 Cl22 109.09(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 S11 2.1416(9) .
As1 S12 2.1459(9) .
S11 C11 1.729(3) .
S12 C16 1.730(3) .
C11 C12 1.398(4) .
C11 C16 1.398(3) .
C12 C13 1.375(4) .
C12 H12 0.9500 .
C13 C14 1.405(4) .
C13 C17 1.509(4) .
C14 C15 1.363(4) .
C14 H14 0.9500 .
C15 C16 1.400(4) .
C15 H15 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
As2 S21 2.1460(10) .
As2 S22 2.1514(10) .
S21 C21 1.734(3) .
S22 C26 1.734(3) .
C21 C26 1.396(3) .
C21 C22 1.405(4) .
C22 C23 1.377(4) .
C22 H22 0.9500 .
C23 C24 1.408(4) .
C23 C27 1.501(4) .
C24 C25 1.368(4) .
C24 H24 0.9500 .
C25 C26 1.401(4) .
C25 H25 0.9500 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
Ga1 Cl11 2.1408(11) .
Ga1 Cl12 2.1798(9) .
Ga1 Cl13 2.1797(7) .
Ga1 Cl13 2.1797(7) 4_565
Ga2 Cl21 2.1494(10) .
Ga2 Cl23 2.1657(8) 4_565
Ga2 Cl23 2.1658(8) .
Ga2 Cl22 2.1792(9) .
