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_4318026
_publ_section_title
;
 Synthesis and Characterization of an Air-Stable Gallium Hydride,
 [t-Bu(H)Ga(\m-NEt2)]2, and Related Chloride Derivatives
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_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_sum            'C16 H40 Ga2 N2'
_chemical_formula_weight         399.94
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.327(2)
_cell_length_b                   11.661(2)
_cell_length_c                   10.229(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      17.1
_cell_measurement_theta_min      11.7
_cell_volume                     1047.0(4)
_computing_cell_refinement       'CAD4 Users Manual (Enraf-Nonius, 1997)'
_computing_data_collection       'CAD4 Users Manual (Enraf-Nonius, 1997)'
_computing_data_reduction        'MolEN (Fair,1990) '
_computing_molecular_graphics    'SHELXTL  (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL  (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXTL  (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL  (Sheldrick, 1995)'
_diffrn_ambient_temperature      210(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'theta-2theta 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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3297
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '120 min'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    2.569
_exptl_absorpt_correction_T_max  0.9972
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.721
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0016(11)
_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_all   1.121
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_obs          0.0382
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.9223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.0972
_reflns_number_observed          1496
_reflns_number_total             1835
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011278a_1.cif
_cod_data_source_block           (1)
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.9223P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.9223P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318026