Entrapment oftert-Butyllithium and Lithiumtert-Butylamide Monomers by Partially Lithiated Derivatives of Aluminum and Gallium Primary Amide Complexes
Brask, Justin K.; Chivers, Tristram; Schatte, Gabriele; Yap, Glenn P. A.; Organometallics 19 (2000) 5683–; doi:10.1021/om000603j

data_4077610
_publ_section_title
;
 Entrapment oftert-Butyllithium and Lithiumtert-Butylamide Monomers by
 Partially Lithiated Derivatives of Aluminum and Gallium Primary Amide
 Complexes
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5683
_journal_paper_doi               10.1021/om000603j
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C28 H68 Ga2 Li3 N7'
_chemical_formula_sum            'C28 H68 Ga2 Li3 N7'
_chemical_formula_weight         663.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9693(17)
_cell_length_b                   10.8903(10)
_cell_length_c                   18.7885(17)
_cell_measurement_reflns_used    7135
_cell_measurement_temperature    193(2)
_cell_volume                     3881.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (1.05) in WinGX-1.62'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14656
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  0.6606
_exptl_absorpt_correction_T_min  0.5214
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
  Corrections; Bruker AXS Inc., Madison, WI, 2000. 
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.355(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7180
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0393P)^2^+0.9975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                5577
_reflns_number_total             7180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000603j.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4077610