Syntheses and Structures of Quinuclidine-Stabilized Amido- and Azidogallanes
Bing Luo; Victor G. Young; Wayne L. Gladfelter; Inorganic Chemistry 39 (2000) 1705–1709; doi:10.1021/ic9910110

data_4320870
_publ_section_title
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 Syntheses and Structures of Quinuclidine-Stabilized Amido- and
 Azidogallanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1705
_journal_page_last               1709
_journal_paper_doi               10.1021/ic9910110
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'B. Luo / Prof. W. Gladfelter'
_chemical_formula_sum            'C31 H50 Ga N3'
_chemical_formula_weight         534.46
_chemical_name_common            98291a
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.650(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7610(1)
_cell_length_b                   19.4052(3)
_cell_length_c                   14.3919(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2978.56(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19309
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       'Irregular plate'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0008(2)
_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   1.079
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_obs          0.0281
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.1238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0649
_refine_ls_wR_factor_obs         0.0630
_reflns_number_observed          4889
_reflns_number_total             5250
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9910110_3.cif
_cod_data_source_block           98294a_Compound3:HGa[NH(2,6-i-Pr2C6H3)]2(quin)
_cod_depositor_comments
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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^)+(0.0206P)^2^+2.1238P] 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^)+(0.0206P)^2^+2.1238P] 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               4320870