Synthesis and Characterization of Dialkylmetal Boryloxides [(μ-9-BBN-9-O)MMe2]2, M = Al, Ga, In
Romana Anulewicz-Ostrowska; Sergiusz Luliński; Janusz Serwatowski; Inorganic Chemistry 38 (1999) 3796–3800; doi:10.1021/ic981454o

data_4322209
_publ_contact_author
;
   Sergiusz Lulinski
   Department of Chemistry
   Technical University of Warsaw
   Noakowskiego 3,
   PL-00-664 Warszawa
   Poland
;
_publ_contact_author_email       serek@ch.pw.edu.pl
_publ_contact_author_fax         '048 22 6282741'
_publ_contact_author_phone       '048 22 6607273'
_publ_section_title
;
 Synthesis and Characterization of Dialkylmetal Boryloxides
 [(\m-9-BBN-9-O)MMe2]2, M = Al, Ga, In
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3796
_journal_page_last               3800
_journal_paper_doi               10.1021/ic981454o
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     '[(1,5-C8H14)BOGa(C4H9)2]2'
_chemical_formula_sum            'C32 H64 B2 Ga2 O2'
_chemical_formula_weight         641.90
_chemical_melting_point          563
_chemical_name_systematic
bis((m2-cyclooctane-1,5-diyl-borane-oxo)bis(tert-butyl)gallium)
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.55(3)
_cell_angle_beta                 67.75(3)
_cell_angle_gamma                77.23(3)
_cell_formula_units_Z            1
_cell_length_a                   9.209(2)
_cell_length_b                   10.184(2)
_cell_length_c                   10.503(2)
_cell_measurement_temperature    293(2)
_cell_volume                     849.7(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3959
_diffrn_reflns_theta_max         79.39
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    2.117
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(5)
_refine_ls_extinction_coef       0.0058(10)
_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   1.036
_refine_ls_goodness_of_fit_obs   1.039
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         3959
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_obs          0.0533
_refine_ls_shift/esd_max         2.600
_refine_ls_shift/esd_mean        0.113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+0.1863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1472
_refine_ls_wR_factor_obs         0.1375
_reflns_number_observed          3480
_reflns_number_total             3959
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981454o_4.cif
_cod_data_source_block           B-O-Ga-t-Bu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1226P)^2^+0.1863P] 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^)+(0.1226P)^2^+0.1863P] where P=(Fo^2^+2Fc^2^)/3'.

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

2020-09-22
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z            2
_cod_original_cell_volume        849.7(3)
_cod_database_code               4322209