#------------------------------------------------------------------------------
#$Date: 2019-12-06 11:37:00 +0200 (Fri, 06 Dec 2019) $
#$Revision: 244931 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556434.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_1556434
loop_
_publ_author_name
'Yang, X.'
'Lunsford, A.'
'Darensbourg, M.Y.'
_publ_section_title
;
 Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via
 the N2S2 Metallo-Ligand Strategy
;
_journal_name_full               Inorganics
_journal_page_first              115
_journal_paper_doi               10.3390/inorganics7090115
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C9 H18 Cl Ga N2 S2'
_chemical_formula_sum            'C9 H18 Cl Ga N2 S2'
_chemical_formula_weight         323.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                94.557(2)
_cell_angle_beta                 98.228(2)
_cell_angle_gamma                114.796(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3341(5)
_cell_length_b                   7.6637(5)
_cell_length_c                   12.6658(9)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    100
_cell_measurement_theta_max      61.26
_cell_measurement_theta_min      3.57
_cell_volume                     631.86(8)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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_temperature      100
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Micro-Source CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11060
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        61.257
_diffrn_reflns_theta_max         61.257
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.767
_exptl_absorpt_correction_T_max  0.1560
_exptl_absorpt_correction_T_min  0.0487
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       needle
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.417
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0498
_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)+(0.0829P)²+2.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1851
_reflns_number_total             1862
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            GaClN2S2.cif
_cod_data_source_block           cu_062517
_cod_database_code               1556434
_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_max   0.926
_shelx_estimated_absorpt_t_min   0.511
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
;
_olex2_diffrn_ambient_temperature_device 'Oxford 700'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.37598(9) 0.31177(8) 0.24390(5) 0.0309(3) Uani 1 1 d . . . . .
Cl1 Cl 0.2803(2) 0.06378(19) 0.10966(11) 0.0416(4) Uani 1 1 d . . . . .
S1 S 0.5374(2) 0.2440(2) 0.39286(11) 0.0380(4) Uani 1 1 d . . . . .
S2 S 0.6382(2) 0.5795(2) 0.20713(12) 0.0408(4) Uani 1 1 d . . . . .
N1 N 0.1044(6) 0.1924(6) 0.3136(3) 0.0316(9) Uani 1 1 d . . . . .
N2 N 0.1808(7) 0.4374(6) 0.1783(4) 0.0364(10) Uani 1 1 d . . . . .
C1 C 0.3121(8) 0.0968(8) 0.4468(5) 0.0383(12) Uani 1 1 d . . . . .
H1A H 0.326053 -0.018310 0.469641 0.046 Uiso 1 1 calc R . . . .
H1B H 0.305818 0.174260 0.511346 0.046 Uiso 1 1 calc R . . . .
C2 C 0.1153(9) 0.0296(8) 0.3652(5) 0.0380(12) Uani 1 1 d . . . . .
H2A H 0.106117 -0.072857 0.309039 0.046 Uiso 1 1 calc R . . . .
H2B H -0.002603 -0.027505 0.401573 0.046 Uiso 1 1 calc R . . . .
C3 C -0.0722(8) 0.1269(8) 0.2250(5) 0.0386(12) Uani 1 1 d . . . . .
H3A H -0.194664 0.114371 0.254079 0.046 Uiso 1 1 calc R . . . .
H3B H -0.099885 -0.002481 0.187255 0.046 Uiso 1 1 calc R . . . .
C4 C -0.0287(9) 0.2768(8) 0.1431(5) 0.0408(13) Uani 1 1 d . . . . .
H4A H -0.042140 0.209983 0.070278 0.049 Uiso 1 1 calc R . . . .
H4B H -0.130519 0.330529 0.139146 0.049 Uiso 1 1 calc R . . . .
C5 C 0.1099(9) 0.3449(8) 0.3960(4) 0.0381(12) Uani 1 1 d . . . . .
H5A H 0.247429 0.408473 0.443064 0.046 Uiso 1 1 calc R . . . .
H5B H 0.009138 0.282622 0.441681 0.046 Uiso 1 1 calc R . . . .
C6 C 0.0627(9) 0.4981(8) 0.3465(5) 0.0412(13) Uani 1 1 d . . . . .
H6A H 0.087616 0.603806 0.405025 0.049 Uiso 1 1 calc R . . . .
H6B H -0.084595 0.439327 0.313091 0.049 Uiso 1 1 calc R . . . .
C7 C 0.1856(9) 0.5864(8) 0.2622(5) 0.0396(12) Uani 1 1 d . . . . .
H7A H 0.130607 0.669957 0.227261 0.048 Uiso 1 1 calc R . . . .
H7B H 0.329455 0.669871 0.298196 0.048 Uiso 1 1 calc R . . . .
C8 C 0.2642(9) 0.5286(8) 0.0868(5) 0.0402(13) Uani 1 1 d . . . . .
H8A H 0.183365 0.595357 0.056600 0.048 Uiso 1 1 calc R . . . .
H8B H 0.251517 0.426454 0.029323 0.048 Uiso 1 1 calc R . . . .
C9 C 0.4860(9) 0.6734(8) 0.1215(5) 0.0397(13) Uani 1 1 d . . . . .
H9A H 0.494160 0.793391 0.161748 0.048 Uiso 1 1 calc R . . . .
H9B H 0.545609 0.708074 0.056484 0.048 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
Cl1 Ga1 S1 107.76(5) . .
Cl1 Ga1 S2 109.29(6) . .
S2 Ga1 S1 101.37(5) . .
N1 Ga1 Cl1 97.19(12) . .
N1 Ga1 S1 85.80(12) . .
N1 Ga1 S2 148.54(12) . .
N2 Ga1 Cl1 98.33(13) . .
N2 Ga1 S1 148.60(13) . .
N2 Ga1 S2 85.69(13) . .
N2 Ga1 N1 73.65(16) . .
C1 S1 Ga1 98.85(18) . .
C9 S2 Ga1 98.78(18) . .
C2 N1 Ga1 105.6(3) . .
C2 N1 C5 110.3(4) . .
C3 N1 Ga1 107.1(3) . .
C3 N1 C2 112.3(4) . .
C3 N1 C5 112.2(4) . .
C5 N1 Ga1 109.0(3) . .
C4 N2 Ga1 107.2(3) . .
C7 N2 Ga1 109.3(3) . .
C7 N2 C4 111.3(4) . .
C8 N2 Ga1 106.6(3) . .
C8 N2 C4 112.1(4) . .
C8 N2 C7 110.2(4) . .
C2 C1 S1 112.4(4) . .
N1 C2 C1 111.4(4) . .
N1 C3 C4 109.9(4) . .
N2 C4 C3 110.2(4) . .
N1 C5 C6 112.8(4) . .
C5 C6 C7 115.0(5) . .
N2 C7 C6 112.7(5) . .
N2 C8 C9 111.3(5) . .
C8 C9 S2 112.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 Cl1 2.2409(14) .
Ga1 S1 2.2942(14) .
Ga1 S2 2.2855(15) .
Ga1 N1 2.164(4) .
Ga1 N2 2.147(4) .
S1 C1 1.831(5) .
S2 C9 1.842(5) .
N1 C2 1.479(7) .
N1 C3 1.462(7) .
N1 C5 1.487(7) .
N2 C4 1.485(8) .
N2 C7 1.483(7) .
N2 C8 1.476(7) .
C1 C2 1.511(8) .
C3 C4 1.572(8) .
C5 C6 1.512(8) .
C6 C7 1.512(8) .
C8 C9 1.508(8) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Ga1 S1 C1 C2 15.3(4) . . . .
Ga1 S2 C9 C8 -12.7(4) . . . .
Ga1 N1 C2 C1 56.5(5) . . . .
Ga1 N1 C3 C4 -39.7(5) . . . .
Ga1 N1 C5 C6 74.4(5) . . . .
Ga1 N2 C4 C3 37.6(5) . . . .
Ga1 N2 C7 C6 -75.3(5) . . . .
Ga1 N2 C8 C9 -55.7(5) . . . .
S1 C1 C2 N1 -48.5(6) . . . .
N1 C3 C4 N2 1.6(6) . . . .
N1 C5 C6 C7 -50.6(7) . . . .
N2 C8 C9 S2 45.5(6) . . . .
C2 N1 C3 C4 -155.2(4) . . . .
C2 N1 C5 C6 -170.1(5) . . . .
C3 N1 C2 C1 172.9(4) . . . .
C3 N1 C5 C6 -44.0(6) . . . .
C4 N2 C7 C6 43.0(6) . . . .
C4 N2 C8 C9 -172.7(4) . . . .
C5 N1 C2 C1 -61.2(6) . . . .
C5 N1 C3 C4 79.9(5) . . . .
C5 C6 C7 N2 50.6(7) . . . .
C7 N2 C4 C3 -81.9(5) . . . .
C7 N2 C8 C9 62.8(6) . . . .
C8 N2 C4 C3 154.2(4) . . . .
C8 N2 C7 C6 167.9(4) . . . .
