Chiral N-Heterocyclic Carbene Borane Complexes: Synthesis and Structural Analysis
Banerjee, Dipshikha; Besnard, Céline; Kündig, E. Peter; Organometallics 31 (2012) 709–; doi:10.1021/om201087n

data_4068094
_publ_section_title
;
 Chiral N-Heterocyclic Carbene Borane Complexes: Synthesis and Structural
 Analysis
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              709
_journal_paper_doi               10.1021/om201087n
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C39 H47 B N2 O2'
_chemical_formula_sum            'C39 H47 B N2 O2'
_chemical_formula_weight         586.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-03-17
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2010.12.31 svn.r1581, GUI svn.r3426)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4531(6)
_cell_length_b                   17.8577(5)
_cell_length_c                   26.0300(15)
_cell_measurement_reflns_used    4678
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      73.2276
_cell_measurement_theta_min      2.4735
_cell_volume                     3464.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -48.00   22.20   0.6000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6678   38.0000 -150.0000 117

  2 omega  -51.00   -4.80   0.6000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6678  -44.0000   -8.0000 77

  3 omega    8.00   69.80   0.6000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6678  -38.0000 -180.0000 103

  4 omega   31.00   70.60   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  -45.0000   60.0000 66

  5 omega   30.00   66.00   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  -45.0000 -120.0000 60

  6 omega   40.00   69.40   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  -45.0000   90.0000 49

  7 omega  110.00  172.40   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  106.0000    3.0000 104

  8 omega  143.00  169.40   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  111.0000 -180.0000 44

  9 omega   84.00  175.20   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686   45.0000 -180.0000 152

 10 omega   43.00   68.80   0.6000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7686  -45.0000  150.0000 43
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0427269000
_diffrn_orient_matrix_UB_12      0.0577514000
_diffrn_orient_matrix_UB_13      -0.0424084000
_diffrn_orient_matrix_UB_21      0.1038440000
_diffrn_orient_matrix_UB_22      -0.0602904000
_diffrn_orient_matrix_UB_23      -0.0299762000
_diffrn_orient_matrix_UB_31      -0.1735844000
_diffrn_orient_matrix_UB_32      -0.0218729000
_diffrn_orient_matrix_UB_33      -0.0284421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            8958
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         73.29
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  1.325
_exptl_absorpt_correction_T_min  1.124
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.6505
_exptl_crystal_size_mid          0.0409
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
In the absence of anomalous scatterine, Friedel pairs were merged
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         3829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0398
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3485
_reflns_number_total             3829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201087n_si_002.cif
_cod_data_source_block           db6084
_cod_original_cell_volume        3464.5(3)
_cod_database_code               4068094
_chemical_oxdiff_formula         'C38 B1 N2 O2'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97