Accessing γ-Ga<sub>2</sub>S<sub>3</sub> by solventless thermolysis of gallium xanthates: a low-temperature limit for crystalline products.
Alderhami, Suliman A.; Collison, David; Lewis, David J.; McNaughter, Paul D.; O'Brien, Paul; Spencer, Ben F.; Vitorica-Yrezabal, Inigo; Whitehead, George; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15605–15612; doi:10.1039/c9dt02061f

data_7701626
_publ_section_title
;
 Accessing \g-Ga<sub>2</sub>S<sub>3</sub> by solventless thermolysis of
 gallium xanthates: a low-temperature limit for crystalline products.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15605
_journal_page_last               15612
_journal_paper_doi               10.1039/c9dt02061f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C15 H24 Ga O3 S6'
_chemical_formula_sum            'C15 H24 Ga O3 S6'
_chemical_formula_weight         514.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-02-27 deposited with the CCDC.	2019-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4378(6)
_cell_length_b                   11.5173(4)
_cell_length_c                   20.0826(5)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    200.08(10)
_cell_measurement_theta_max      71.7500
_cell_measurement_theta_min      4.3300
_cell_volume                     4727.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.08(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00 -33.00   1.00    1.00    --    0.00  60.00-120.00   26
  2  \w    -14.00  87.00   1.00    1.00    --    0.00  29.00   0.00  101
  3  \w    -82.00 -40.00   1.00    1.00    --    0.00  29.00   0.00   42
  4  \w     -4.00 143.00   1.00    1.00    --   55.00  60.00-120.00  147
  5  \w    -12.00  47.00   1.00    1.00    --   55.00  43.00 -90.00   59
  6  \w    -31.00 132.00   1.00    1.00    --   55.00  60.00-150.00  163
  7  \w    102.00 137.00   1.00    1.00    --   55.00  43.00 -90.00   35
  8  \w     84.00 110.00   1.00    5.00    --  110.00  60.00 150.00   26
  9  \w     51.00  77.00   1.00    5.00    --  110.00  60.00 150.00   26
 10  \w     22.00 199.00   1.00    5.00    --  110.00  23.00-120.00  177
 11  \w    139.00 193.00   1.00    5.00    --  110.00  60.00-150.00   54
 12  \w    152.00 195.00   1.00    5.00    --  110.00  60.00-120.00   43
 13  \w     74.00 103.00   1.00    5.00    --  110.00  60.00-120.00   29
 14  \w     57.00  96.00   1.00    5.00    --  110.00  60.00-180.00   39
 15  \w     99.00 180.00   1.00    5.00    --  110.00  60.00-180.00   81
 16  \w    133.00 158.00   1.00    5.00    --  110.00  60.00 150.00   25
 17  \w     82.00 108.00   1.00    5.00    --  110.00  60.00-150.00   26
 18  \w     21.00  46.00   1.00    5.00    --  110.00  60.00  30.00   25
 19  \w    126.00 199.00   1.00    5.00    --  110.00  60.00  30.00   73
 20  \w     91.00 192.00   1.00    5.00    --  110.00  23.00   0.00  101
 21  \w     64.00  90.00   1.00    5.00    --  110.00  23.00   0.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0527805000
_diffrn_orient_matrix_UB_12      -0.0331680000
_diffrn_orient_matrix_UB_13      0.0513694000
_diffrn_orient_matrix_UB_21      -0.0204391000
_diffrn_orient_matrix_UB_22      0.1284444000
_diffrn_orient_matrix_UB_23      0.0055082000
_diffrn_orient_matrix_UB_31      -0.0497380000
_diffrn_orient_matrix_UB_32      -0.0174741000
_diffrn_orient_matrix_UB_33      -0.0567207000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24488
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.346
_diffrn_reflns_theta_min         4.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0580
_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/[\s^2^(Fo^2^)+20.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4164
_reflns_number_total             4612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02061f2.cif
_cod_data_source_block           s4946l
_cod_database_code               7701626
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.435
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C3 \\sim C5-C4A
 with sigma of 0.02
 C9A-C10 \\sim C9-C8A
 with sigma of 0.02
 C8A-C7 \\sim C8-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4A \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9A \\sim C9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C8A \\sim C8: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 C4A, C5, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9A, C10, C7, C8A, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=FVAR(1)
 Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(2)
 Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7B), C7(H7A), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C8(H8A,H8B)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C4(H4A,H4B,H4C), C8A(H8AA,H8AB,H8AC),
  C9A(H9AA,H9AB,H9AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              51867
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.763
_oxdiff_exptl_absorpt_empirical_full_min 0.616