Spectroscopic and Structural Characterization of the CyNHC Adduct of B2pin2 in Solution and in the Solid State
Christian Kleeberg; Andrew G. Crawford; Andrei S. Batsanov; Paul Hodgkinson; David C. Apperley; Man Sing Cheung; Zhenyang Lin; Todd B. Marder; Journal of Organic Chemistry 77 (2012) 785–789; doi:10.1021/jo202127c

data_4026864
_publ_contact_author_address
;
 Durham University
 Department of Chemistry
 South Road, Durham, DH1 3LE
 UK
;
_publ_contact_author_email       todd.marder@durham.ac.uk
_publ_contact_author_fax         '+44 (0) 191 38 44737'
_publ_contact_author_name        'Todd B. Marder'
_publ_contact_author_phone       '+44 (0) 191 33 42037'
_publ_section_title
;
 Spectroscopic and Structural Characterization of the CyNHC Adduct of
 B2pin2 in Solution and in the Solid State
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              785
_journal_page_last               789
_journal_paper_doi               10.1021/jo202127c
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C12 H24 B2 O4'
_chemical_formula_sum            'C12 H24 B2 O4'
_chemical_formula_weight         253.93
_chemical_melting_point          411
_chemical_name_common            bis(pinacolate)diborane(4)
_chemical_name_systematic
; 
4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl-4',4',5',
5'-tetramethyl-1',3',2'-dioxaborolane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 110.478(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2834(9)
_cell_length_b                   7.4809(6)
_cell_length_c                   10.1672(8)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.42
_cell_volume                     732.73(11)
_computing_cell_refinement       'SAINT version 7.46A (Bruker, 2007)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 7.46A (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL version 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area detector'
_diffrn_measurement_method       '\w 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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13019
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         3.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2006/1 (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       tablet
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0789P)^2^+0.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                1842
_reflns_number_total             2143
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo202127c_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        732.73(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4026864