Connecting Main-Group Metals (Al, Ga, In) and Tungsten(0) Carbonyls via the N2S2 Metallo-Ligand Strategy
Yang, X.; Lunsford, A.; Darensbourg, M.Y.; Inorganics 7 (2019) 115–; doi:10.3390/inorganics7090115

data_1556434
_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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0829P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            GaClN2S2.cif
_cod_data_source_block           cu_062517
_cod_database_code               1556434
_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)
;
_shelx_res_checksum              16054
_shelx_hkl_checksum              67667
_olex2_diffrn_ambient_temperature_device 'Oxford 700'
_olex2_submission_special_instructions 'No special instructions were received'