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_4322206
_publ_contact_author
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   Sergiusz Lulinski
   Department of Chemistry
   Technical University of Warsaw
   Noakowskiego 3,
   PL-00-664 Warszawa
   Poland
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_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
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 Synthesis and Characterization of Dialkylmetal Boryloxides
 [(\m-9-BBN-9-O)MMe2]2, M = Al, Ga, In
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_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)BOAl(CH3)2]2'
_chemical_formula_sum            'C20 H40 Al2 B2 O2'
_chemical_formula_weight         388.10
_chemical_melting_point          483
_chemical_name_systematic
'bis((m2-cyclooctane-1,5-diyl-borane-oxo) dimethylaluminum)'
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.142(4)
_cell_length_b                   9.876(2)
_cell_length_c                   12.846(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2428.5(9)
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1511
_diffrn_reflns_theta_max         78.79
_diffrn_reflns_theta_min         4.62
_exptl_absorpt_coefficient_mu    1.146
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(12)
_refine_ls_extinction_coef       0.0111(9)
_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   1.082
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1365
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_restrained_S_obs      1.121
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_obs          0.0568
_refine_ls_shift/esd_max         0.381
_refine_ls_shift/esd_mean        0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+1.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1567
_refine_ls_wR_factor_obs         0.1437
_reflns_number_observed          1127
_reflns_number_total             1367
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981454o_1.cif
_cod_data_source_block           B-O-Al
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+1.1872P] 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^)+(0.0909P)^2^+1.1872P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322206