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_7701625
_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         'C12 H21 Ga O3 S6'
_chemical_formula_sum            'C12 H21 Ga O3 S6'
_chemical_formula_weight         475.37
_chemical_name_systematic        'Gallium(III) i-propylxanthate'
_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             2017-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2019-02-27 deposited with the CCDC.	2019-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.135(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8900(4)
_cell_length_b                   10.9162(5)
_cell_length_c                   18.9067(7)
_cell_measurement_reflns_used    5492
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      28.7010
_cell_measurement_theta_min      2.2880
_cell_volume                     2039.77(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.845
_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    -42.00 -17.00   1.00    1.50    --    5.00 -31.00 -65.00   25
  2  \w     27.00  52.00   1.00    1.50    --    5.00  31.00  94.00   25
  3  \w      2.00  29.00   1.00    1.50    --    5.00  38.00-150.00   27
  4  \w     33.00  76.00   1.00    1.50    --   -5.50  38.00 -30.00   43
  5  \w     -5.00  83.00   1.00    1.50    --   -5.50  57.00 -30.00   88
  6  \w    -41.00  11.00   1.00    1.50    --   -5.50  38.00 -30.00   52
  7  \w    -92.00   9.00   1.00    1.50    --   -5.50 -57.00  90.00  101
;
_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      -0.0641896000
_diffrn_orient_matrix_UB_12      -0.0252093000
_diffrn_orient_matrix_UB_13      -0.0096688000
_diffrn_orient_matrix_UB_21      -0.0145554000
_diffrn_orient_matrix_UB_22      -0.0063313000
_diffrn_orient_matrix_UB_23      0.0362670000
_diffrn_orient_matrix_UB_31      -0.0286155000
_diffrn_orient_matrix_UB_32      0.0595626000
_diffrn_orient_matrix_UB_33      -0.0002468000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21645
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27091
_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    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+3.1574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3658
_reflns_number_total             4661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02061f2.cif
_cod_data_source_block           s4917r
_cod_database_code               7701625
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Ga1S6C12O3H20
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C6(H6), C10(H10)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              73362
_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 2.304
_oxdiff_exptl_absorpt_empirical_full_min 0.460