#------------------------------------------------------------------------------
#$Date: 2019-11-05 05:41:22 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223275 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/14/7701475.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_7701475
loop_
_publ_author_name
'Ould, Darren'
'Tran, Thao Thi-Phuong'
'Rawson, Jeremy Michael'
'Melen, Rebecca'
_publ_section_title
;
 Structure-property-reactivity studies on dithiaphospholes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03577J
_journal_year                    2019
_chemical_formula_moiety         'C7 H6 P S2, Cl4 Ga'
_chemical_formula_sum            'C7 H6 Cl4 Ga P S2'
_chemical_formula_weight         396.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-09-03 deposited with the CCDC.	2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0083(16)
_cell_length_b                   9.2891(19)
_cell_length_c                   18.572(4)
_cell_measurement_reflns_used    3320
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.439
_cell_measurement_theta_min      2.206
_cell_volume                     1373.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'DIRDIF (PATTSY)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX II with CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.439
_diffrn_reflns_theta_min         2.206
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.166
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       cube
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0464
_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)+(0.0457P)²+3.9377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2792
_reflns_number_total             3320
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt03577j2.cif
_cod_data_source_block           hklf5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7701475
_shelx_shelxl_version_number     2017/1
_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   0.450
_shelx_estimated_absorpt_t_max   0.450
_exptl_absorpt_special_details
;
sadabs, Bruker AXS, Madison WI USA
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S11 S 0.78539(17) 0.36085(14) 0.07033(7) 0.0231(3) Uani 1 1 d . .
S12 S 0.42848(17) 0.26129(15) 0.01519(7) 0.0237(3) Uani 1 1 d . .
P11 P 0.66906(19) 0.22135(15) -0.00312(8) 0.0264(3) Uani 1 1 d . .
C11 C 0.6178(7) 0.4355(5) 0.1092(3) 0.0195(10) Uani 1 1 d . .
C12 C 0.6408(7) 0.5381(5) 0.1640(3) 0.0235(11) Uani 1 1 d . .
H12A H 0.751081 0.568737 0.181287 0.028 Uiso 1 1 calc R U
C13 C 0.5051(7) 0.5954(5) 0.1932(3) 0.0206(10) Uani 1 1 d . .
C14 C 0.3406(7) 0.5493(6) 0.1672(3) 0.0257(11) Uani 1 1 d . .
H14A H 0.246650 0.588660 0.187473 0.031 Uiso 1 1 calc R U
C15 C 0.3154(7) 0.4479(6) 0.1126(3) 0.0260(11) Uani 1 1 d . .
H15A H 0.205047 0.417943 0.094964 0.031 Uiso 1 1 calc R U
C16 C 0.4538(7) 0.3905(5) 0.0840(3) 0.0208(10) Uani 1 1 d . .
C17 C 0.5284(9) 0.7057(6) 0.2533(3) 0.0331(13) Uani 1 1 d . .
H17A H 0.643514 0.742841 0.257261 0.050 Uiso 1 1 calc R U
H17B H 0.507543 0.660569 0.299217 0.050 Uiso 1 1 calc R U
H17C H 0.449096 0.785141 0.242489 0.050 Uiso 1 1 calc R U
Ga1 Ga 0.05131(7) 0.39287(6) 0.36361(3) 0.02073(16) Uani 1 1 d . .
Cl11 Cl 0.31412(17) 0.46478(15) 0.37794(7) 0.0288(3) Uani 1 1 d . .
Cl12 Cl -0.1111(2) 0.56085(15) 0.39652(9) 0.0385(4) Uani 1 1 d . .
Cl13 Cl -0.0125(2) 0.32671(18) 0.25191(7) 0.0376(4) Uani 1 1 d . .
Cl14 Cl 0.02916(16) 0.20136(13) 0.43156(7) 0.0244(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
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'
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'
P P 0.1023 0.0942 '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
C11 S11 P11 102.41(19)
C16 S12 P11 102.21(19)
S12 P11 S11 98.37(8)
C12 C11 C16 119.4(5)
C12 C11 S11 122.0(4)
C16 C11 S11 118.6(4)
C13 C12 C11 120.4(5)
C13 C12 H12A 119.8
C11 C12 H12A 119.8
C12 C13 C14 119.6(5)
C12 C13 C17 121.0(5)
C14 C13 C17 119.5(5)
C15 C14 C13 120.8(5)
C15 C14 H14A 119.6
C13 C14 H14A 119.6
C14 C15 C16 118.9(5)
C14 C15 H15A 120.5
C16 C15 H15A 120.5
C15 C16 C11 120.9(5)
C15 C16 S12 120.6(4)
C11 C16 S12 118.4(4)
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
Cl12 Ga1 Cl13 112.84(7)
Cl12 Ga1 Cl11 110.13(6)
Cl13 Ga1 Cl11 108.96(7)
Cl12 Ga1 Cl14 109.47(6)
Cl13 Ga1 Cl14 107.10(6)
Cl11 Ga1 Cl14 108.20(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S11 C11 1.736(5)
S11 P11 2.033(2)
S12 C16 1.749(5)
S12 P11 2.027(2)
C11 C12 1.392(7)
C11 C16 1.409(7)
C12 C13 1.374(7)
C12 H12A 0.9500
C13 C14 1.419(8)
C13 C17 1.511(7)
C14 C15 1.383(7)
C14 H14A 0.9500
C15 C16 1.386(7)
C15 H15A 0.9500
C17 H17A 0.9800
C17 H17B 0.9800
C17 H17C 0.9800
Ga1 Cl12 2.1613(16)
Ga1 Cl13 2.1708(16)
Ga1 Cl11 2.1966(15)
Ga1 Cl14 2.1994(14)
