Novel C1-Bridged Bisboronate Derivatives by Insertion of Diazoalkanes into Bis(pinacolato)diborane(4)⊥
Abu Ali, Hijazi; Goldberg, Israel; Kaufmann, Dieter; Burmeister, Christian; Srebnik, Morris; Organometallics 21 (2002) 1870–; doi:10.1021/om011012b

data_4076738
_publ_section_title
;
 Novel C1-Bridged Bisboronate Derivatives by Insertion of Diazoalkanes
 into Bis(pinacolato)diborane(4)&#x22A5;
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1870
_journal_paper_doi               10.1021/om011012b
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C22 H34 B2 O4'
_chemical_formula_weight         384.11
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.000(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   53.9430(3)
_cell_length_b                   10.3370(3)
_cell_length_c                   15.7610(6)
_cell_measurement_temperature    110(2)
_cell_volume                     8788.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3658
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.4(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         1920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+6.0496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1698
_reflns_number_total             1920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om011012b.cif
_cod_data_source_block           5b
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4076738