Synthesis and Characterization of an Air-Stable Gallium Hydride, [t-Bu(H)Ga(μ-NEt2)]2, and Related Chloride Derivatives
Luke Grocholl; Scott A. Cullison; Jianjun Wang; Dale C. Swenson; Edward G. Gillan; Inorganic Chemistry 41 (2002) 2920–2926; doi:10.1021/ic011278a

data_4318028
_publ_section_title
;
 Synthesis and Characterization of an Air-Stable Gallium Hydride,
 [t-Bu(H)Ga(\m-NEt2)]2, and Related Chloride Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2920
_journal_page_last               2926
_journal_paper_doi               10.1021/ic011278a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C12 H29 Cl3 Ga2 N2'
_chemical_formula_sum            'C12 H29 Cl3 Ga2 N2'
_chemical_formula_weight         447.16
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.83(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.625(2)
_cell_length_b                   12.122(3)
_cell_length_c                   16.540(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      13.9
_cell_volume                     1922.9(8)
_computing_cell_refinement       'CAD4 Users Manual (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 Users Manual (Enraf-Nonius, 1977)'
_computing_data_reduction        'MoLEN (Fair, 1990)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\q-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7145
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  7200
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    3.210
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.7163
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details   'MoLEN (Fair, 1990)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.534
_exptl_crystal_size_min          0.452
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+1.3964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                4032
_reflns_number_total             4382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011278a_3.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318028