Synthesis of new asymmetric substituted boron amidines - reactions with CO and transfer hydrogenations of phenylacetylene.
Cabrera, Alan R.; Rojas, Rene S.; Valderrama, Mauricio; Plüss, Pascal; Berke, Heinz; Daniliuc, Constantin G.; Kehr, Gerald; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19606–19614; doi:10.1039/c5dt01966d

data_7035706
_publ_section_title
;
 Synthesis of new asymmetric substituted boron amidines - reactions with
 CO and transfer hydrogenations of phenylacetylene.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19606
_journal_page_last               19614
_journal_paper_doi               10.1039/c5dt01966d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C33 H26 B F10 N3'
_chemical_formula_weight         665.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'at N and B from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc148pgk
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-24 deposited with the CCDC.
2015-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4308(2)
_cell_length_b                   18.9125(2)
_cell_length_c                   15.1079(2)
_cell_measurement_reflns_used    5959
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     3547.62(8)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_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  0.060
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29690
_diffrn_reflns_theta_full        67.01
_diffrn_reflns_theta_max         67.01
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_correction_T_min  0.8310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 A badly disordered half hexane molecule was found in the 
 asymmetrical unit and could not be satisfactorily refined. The program 
 SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) was therefore used
 to remove mathematically the effect of the solvent.
 The quoted formula and derived parameters are not included the squeezed
 solvent molecule. 
;
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+1.1709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                4294
_reflns_number_total             6109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01966d2.cif
_cod_data_source_block           erk6293
_cod_depositor_comments
'Adding full bibliography for 7035706--7035708.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7035706