Hydrolytically Stable Tricoordinate Chiral Bicyclo[4.4.0]diboronic Ester: Synthesis, Structural Characterization, and Theoretical Investigation†
Zhou, Yan; Shan, Zixing; Wang, Baoshan; Xie, Peng; Organometallics 25 (2006) 4917–; doi:10.1021/om060559t

data_4074336
_publ_section_title
;
 Hydrolytically Stable Tricoordinate Chiral Bicyclo[4.4.0]diboronic
 Ester:&#x00A0; Synthesis, Structural Characterization, and Theoretical
 Investigation&#x2020;
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4917
_journal_paper_doi               10.1021/om060559t
_journal_volume                  25
_journal_year                    2006
_chemical_absolute_configuration 4aR,8aR
_chemical_formula_moiety         'C40 H32 B2 O4, O'
_chemical_formula_sum            'C40 H32 B2 O5'
_chemical_formula_weight         614.28
_chemical_melting_point          537(8)
_chemical_name_systematic
; 
(4aR,8aR)-tetrahydro-2,4,4,6,8,8-hexaphenyl-[1,3,2]dioxaborinino
[5,4-d][1,3,2]dioxaborinine 
;
_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-97
_cell_angle_alpha                111.552(2)
_cell_angle_beta                 90.165(2)
_cell_angle_gamma                108.708(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6051(13)
_cell_length_b                   9.9781(13)
_cell_length_c                   10.4687(14)
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.11
_cell_volume                     875.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5740
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9922
_exptl_absorpt_correction_T_min  0.9680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(13)
_refine_ls_extinction_coef       0.038(7)
_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   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+0.0504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                3688
_reflns_number_total             4840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060559tsi20060626_113242.cif
_cod_data_source_block           60215zy2_0m
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4074336