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_7701627
_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         'C6 H9 Ga O3 S6'
_chemical_formula_sum            'C6 H9 Ga O3 S6'
_chemical_formula_weight         391.21
_chemical_name_systematic        'Gallium(III) methylxanthate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-28
_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                 107.382(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5526(2)
_cell_length_b                   13.9797(3)
_cell_length_c                   11.1352(3)
_cell_measurement_reflns_used    11496
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      26.3250
_cell_measurement_theta_min      2.3920
_cell_volume                     1419.12(6)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -24.00   4.00   1.00    1.00    --    5.00 -57.00  60.00   28
  2  \w    -81.00 -37.00   1.00    1.00    --    5.00 -57.00  60.00   44
  3  \w    -95.00  26.00   1.00    1.00    --   -7.70 -57.00 -30.00  121
  4  \w    -85.00 -28.00   1.00    1.00    --   -7.70 -57.00 120.00   57
  5  \w    -23.00  26.00   1.00    1.00    --   -7.70 -57.00 120.00   49
  6  \w    -97.00   2.00   1.00    1.00    --   -7.70 -19.00-120.00   99
  7  \w     23.00  48.00   1.00    1.00    --   -7.70 -19.00-120.00   25
  8  \w    -96.00 -22.00   1.00    1.00    --   -7.70 -38.00-180.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0102295000
_diffrn_orient_matrix_UB_12      -0.0500895000
_diffrn_orient_matrix_UB_13      -0.0031260000
_diffrn_orient_matrix_UB_21      0.0770446000
_diffrn_orient_matrix_UB_22      0.0064220000
_diffrn_orient_matrix_UB_23      0.0234827000
_diffrn_orient_matrix_UB_31      -0.0036124000
_diffrn_orient_matrix_UB_32      -0.0049250000
_diffrn_orient_matrix_UB_33      0.0624015000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.407
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72266
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0167
_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/[\s^2^(Fo^2^)+(0.0113P)^2^+0.6059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2784
_reflns_number_total             2892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02061f2.cif
_cod_data_source_block           s5050r
_cod_database_code               7701627
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.413
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              85482
_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 1.534
_oxdiff_exptl_absorpt_empirical_full_min 0.748