Synthesis and Characterization of a Coordinated Oxoborane: Lewis Acid Stabilization of a Boron-Oxygen Double Bond
Dragoslav Vidovic; Jennifer A. Moore; Jamie N. Jones; Alan H. Cowley; Journal of the American Chemical Society 127 (2005) 4566–4567; doi:10.1021/ja0507564

data_4111597
_publ_contact_author_address
;
   Department of Chemistry and Biochemistry
   University of Texas-Austin
   1 University Station, A5300
   Austin, TX 78701
   USA
;
_publ_contact_author_email       cowley@mail.utexas.edu
_publ_contact_author_fax         512-471-6822
_publ_contact_author_name
;
Alan H. Cowley
;
_publ_contact_author_phone       512-471-6591
_publ_section_title
;
 Synthesis and Characterization of a Coordinated Oxoborane: Lewis Acid
 Stabilization of a Boron-Oxygen Double Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4566
_journal_page_last               4567
_journal_paper_doi               10.1021/ja0507564
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C23 H12 Al B Cl4 F10 N2'
_chemical_formula_sum            'C23 H12 Al B Cl4 F10 N2'
_chemical_formula_weight         685.94
_chemical_name_systematic        ?
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
manual editing of the .cif file 
created by SHELXTL Ver. 6.10 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.588(5)
_cell_length_b                   15.086(3)
_cell_length_c                   7.1553(14)
_cell_measurement_temperature    153(2)
_cell_volume                     2762.1(9)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;
SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scan
_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  0.1102
_diffrn_reflns_av_unetI/netI     0.1253
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4084
_diffrn_reflns_theta_full        24
_diffrn_reflns_theta_max         24
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.0
_exptl_absorpt_correction_T_min  0.0
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.65
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0055(14)
_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_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1843
_refine_ls_R_factor_gt           0.079
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+5.7949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                1027
_reflns_number_total             2259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0507564si20050204_031017.cif
_cod_data_source_block           ccddvjm001
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'al b c23 cl4 f10 h12 n2' to 'C23 H12 Al B Cl4 F10 N2'.

 Antanas Vaitkus,
 2017-01-04
;
_cod_original_formula_sum        'c23 h12 al b cl4 f10 n2'
_cod_database_code               4111597