#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:59:51 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223322 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/16/7701624.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_7701624
loop_
_publ_author_name
'Alderhami, Suliman A.'
'Collison, David'
'Lewis, David J.'
'McNaughter, Paul D.'
'O'Brien, Paul'
'Spencer, Ben F.'
'Vitorica-Yrezabal, Inigo'
'Whitehead, George'
_publ_section_title
;
 Accessing γ-Ga₂S₃ 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         'C9 H15 Ga1 O3 S6'
_chemical_formula_sum            'C9 H15 Ga O3 S6'
_chemical_formula_weight         433.29
_chemical_name_systematic        'Gallium(III) ethylxanthate'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.0276(10)
_cell_length_b                   15.0276(10)
_cell_length_c                   13.1704(8)
_cell_measurement_reflns_used    2280
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.1590
_cell_measurement_theta_min      4.3820
_cell_volume                     2575.8(3)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00 -27.00   1.00    1.00    --   -5.60 -61.00-121.00   40
  2  ω    -35.00  52.00   1.00    1.00    --   -5.60  57.00  90.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0316783000
_diffrn_orient_matrix_UB_12      -0.0078156000
_diffrn_orient_matrix_UB_13      -0.0429035000
_diffrn_orient_matrix_UB_21      0.0415582000
_diffrn_orient_matrix_UB_22      0.0101230000
_diffrn_orient_matrix_UB_23      -0.0326271000
_diffrn_orient_matrix_UB_31      -0.0152678000
_diffrn_orient_matrix_UB_32      -0.0529266000
_diffrn_orient_matrix_UB_33      0.0001008000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3289
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.043
_diffrn_reflns_theta_min         3.492
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41341
_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    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0209
_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/[σ²(Fo²)+(0.0249P)²+3.2591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1199
_reflns_number_total             1267
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02061f2.cif
_cod_data_source_block           s4915r
_cod_original_cell_volume        2575.8(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7701624
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Ga1S6O3C3H9
_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.
;
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_shelx_res_file
;
TITL s4915r R -3 R = 0.02
CELL 0.71073 15.0276 15.0276 13.1704 90 90 120
ZERR 6 0.001 0.001 0.0008 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Ga O S
UNIT 54 90 6 18 36

L.S. 5
PLAN  -20
TEMP -123
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\s4915r.hkl">
REM </olex2.extras>

WGHT    0.024900    3.259100
FVAR       2.30321
GA1   3    0.333333    0.666667    0.466525    10.33333    0.01504    0.01504 =
         0.01999    0.00000    0.00000    0.00752
S1    5    0.399995    0.573672    0.558345    11.00000    0.01895    0.01755 =
         0.01917   -0.00292   -0.00282    0.00985
S2    5    0.289013    0.512744    0.364131    11.00000    0.02094    0.01894 =
         0.02033   -0.00272   -0.00402    0.01071
O1    4    0.353928    0.403942    0.469456    11.00000    0.02529    0.01826 =
         0.02363   -0.00415   -0.00417    0.01319
C1    1    0.347129    0.487539    0.461750    11.00000    0.01355    0.01712 =
         0.02014    0.00048    0.00282    0.00731
C2    1    0.317106    0.329343    0.386203    11.00000    0.03063    0.02062 =
         0.02652   -0.00966   -0.00726    0.01312
AFIX  23
H2A   2    0.366744    0.355008    0.329251    11.00000   -1.20000
H2B   2    0.250048    0.317788    0.361084    11.00000   -1.20000
AFIX   0
C3    1    0.306193    0.231280    0.427158    11.00000    0.03597    0.02061 =
         0.03843   -0.00466   -0.00289    0.01399
AFIX 137
H3A   2    0.282513    0.179713    0.372988    11.00000   -1.50000
H3B   2    0.256104    0.206118    0.482719    11.00000   -1.50000
H3C   2    0.372827    0.243910    0.452539    11.00000   -1.50000
AFIX   0
HKLF 4

REM  s4915r R -3 R = 0.02
REM R1 =  0.0209 for    1199 Fo > 4sig(Fo)  and  0.0226 for all    1267 data
REM     59 parameters refined using      0 restraints

END

WGHT      0.0255      3.2393

REM Highest difference peak  0.402,  deepest hole -0.274,  1-sigma level  0.057
Q1    1   0.2961  0.6994  0.4375  11.00000  0.05    0.40
Q2    1   0.3272  0.4943  0.4029  11.00000  0.05    0.36
Q3    1   0.3188  0.5807  0.3861  11.00000  0.05    0.34
Q4    1   0.3710  0.5176  0.5198  11.00000  0.05    0.33
Q5    1   0.2705  0.6311  0.4950  11.00000  0.05    0.30
Q6    1   0.4648  0.6039  0.5335  11.00000  0.05    0.27
Q7    1   0.3363  0.5335  0.5898  11.00000  0.05    0.26
Q8    1   0.3410  0.3717  0.4235  11.00000  0.05    0.23
Q9    1   0.4298  0.5474  0.5919  11.00000  0.05    0.23
Q10   1   0.2568  0.4518  0.3345  11.00000  0.05    0.22
Q11   1   0.3865  0.7611  0.5356  11.00000  0.05    0.22
Q12   1   0.3603  0.5609  0.3327  11.00000  0.05    0.21
Q13   1   0.3262  0.3430  0.3301  11.00000  0.05    0.21
Q14   1   0.3333  0.6667  0.3914  10.33333  0.05    0.21
Q15   1   0.3147  0.2773  0.4008  11.00000  0.05    0.20
Q16   1   0.2204  0.4785  0.3953  11.00000  0.05    0.19
Q17   1   0.2754  0.7118  0.4827  11.00000  0.05    0.18
Q18   1   0.2834  0.3465  0.3345  11.00000  0.05    0.17
Q19   1   0.2973  0.3836  0.5009  11.00000  0.05    0.17
Q20   1   0.3333  0.6667  0.5400  10.33333  0.05    0.17
;
_shelx_res_checksum              24849
_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 2.023
_oxdiff_exptl_absorpt_empirical_full_min 0.681
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ga1 Ga 0.3333 0.6667 0.46652(2) 0.01669(10) Uani 1 3 d S T P
S1 S 0.40000(3) 0.57367(3) 0.55834(3) 0.01824(11) Uani 1 1 d . . .
S2 S 0.28901(3) 0.51274(3) 0.36413(3) 0.01974(11) Uani 1 1 d . . .
O1 O 0.35393(9) 0.40394(8) 0.46946(8) 0.0214(2) Uani 1 1 d . . .
C1 C 0.34713(11) 0.48754(12) 0.46175(11) 0.0171(3) Uani 1 1 d . . .
C2 C 0.31711(14) 0.32934(13) 0.38620(13) 0.0258(4) Uani 1 1 d . . .
H2A H 0.3667 0.3550 0.3293 0.031 Uiso 1 1 calc R . .
H2B H 0.2500 0.3178 0.3611 0.031 Uiso 1 1 calc R . .
C3 C 0.30619(16) 0.23128(14) 0.42716(15) 0.0317(4) Uani 1 1 d . . .
H3A H 0.2825 0.1797 0.3730 0.048 Uiso 1 1 calc GR . .
H3B H 0.2561 0.2061 0.4827 0.048 Uiso 1 1 calc GR . .
H3C H 0.3728 0.2439 0.4525 0.048 Uiso 1 1 calc GR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.01504(12) 0.01504(12) 0.01999(16) 0.000 0.000 0.00752(6)
S1 0.0190(2) 0.0176(2) 0.01917(19) -0.00292(14) -0.00282(14) 0.00985(15)
S2 0.0209(2) 0.0189(2) 0.02033(19) -0.00272(14) -0.00402(15) 0.01071(16)
O1 0.0253(6) 0.0183(5) 0.0236(5) -0.0041(4) -0.0042(5) 0.0132(5)
C1 0.0135(7) 0.0171(7) 0.0201(7) 0.0005(6) 0.0028(6) 0.0073(6)
C2 0.0306(9) 0.0206(8) 0.0265(8) -0.0097(7) -0.0073(7) 0.0131(7)
C3 0.0360(10) 0.0206(8) 0.0384(10) -0.0047(7) -0.0029(8) 0.0140(8)
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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Ga1 S1 97.068(14) 3_565 2_665
S1 Ga1 S1 97.064(14) 3_565 .
S1 Ga1 S1 97.065(14) 2_665 .
S1 Ga1 S2 97.969(14) . 2_665
S1 Ga1 S2 74.108(13) 2_665 2_665
S1 Ga1 S2 97.970(14) 2_665 3_565
S1 Ga1 S2 163.388(13) 2_665 .
S1 Ga1 S2 163.391(13) 3_565 2_665
S1 Ga1 S2 163.389(13) . 3_565
S1 Ga1 S2 74.108(13) . .
S1 Ga1 S2 97.968(14) 3_565 .
S1 Ga1 S2 74.110(13) 3_565 3_565
S2 Ga1 S2 92.907(15) 3_565 2_665
S2 Ga1 S2 92.908(15) 3_565 .
S2 Ga1 S2 92.907(15) 2_665 .
C1 S1 Ga1 83.96(5) . .
C1 S2 Ga1 82.38(5) . .
C1 O1 C2 119.58(12) . .
S2 C1 S1 119.49(9) . .
O1 C1 S1 116.07(11) . .
O1 C1 S2 124.44(11) . .
O1 C2 H2A 110.3 . .
O1 C2 H2B 110.3 . .
O1 C2 C3 107.27(13) . .
H2A C2 H2B 108.5 . .
C3 C2 H2A 110.3 . .
C3 C2 H2B 110.3 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 S1 2.4122(4) 3_565
Ga1 S1 2.4122(4) 2_665
Ga1 S1 2.4122(4) .
Ga1 S2 2.4642(4) .
Ga1 S2 2.4642(4) 3_565
Ga1 S2 2.4642(4) 2_665
S1 C1 1.7020(15) .
S2 C1 1.7000(15) .
O1 C1 1.3143(19) .
O1 C2 1.4645(19) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.499(2) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Ga1 S1 C1 S2 2.41(8)
Ga1 S1 C1 O1 -176.94(12)
Ga1 S2 C1 S1 -2.37(8)
Ga1 S2 C1 O1 176.93(13)
C1 O1 C2 C3 -163.98(14)
C2 O1 C1 S1 -175.60(11)
C2 O1 C1 S2 5.1(2)
