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_4068093
_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 syn
_chemical_formula_moiety         'C27 H39 B N2 O2'
_chemical_formula_sum            'C27 H39 B N2 O2'
_chemical_formula_weight         434.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-03-18
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2010.12.31 svn.r1581, GUI svn.r3426)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7154(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.55564(15)
_cell_length_b                   14.24537(18)
_cell_length_c                   14.6874(2)
_cell_measurement_reflns_used    13782
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      73.8704
_cell_measurement_theta_min      3.0414
_cell_volume                     2596.65(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -65.00   30.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075   38.0000  -30.0000 95

  2 omega -104.00  -10.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075  -38.0000  150.0000 94

  3 omega -120.00  -94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075  -87.0000 -118.0000 26

  4 omega  -10.00   16.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9075  -87.0000   61.0000 26

  5 omega  -61.00  -35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   45.0000  -60.0000 26

  6 omega   33.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  -45.0000  -60.0000 44

  7 omega   94.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  125.0000    0.0000 78

  8 omega   33.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  -45.0000    0.0000 34

  9 omega   35.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  -45.0000   30.0000 30

 10 omega   95.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  125.0000   30.0000 71

 11 omega  111.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  125.0000  -60.0000 64

 12 omega  118.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289   45.0000  -60.0000 44

 13 omega   38.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  -45.0000  -90.0000 26

 14 omega   47.00   75.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  -45.0000 -120.0000 28

 15 omega  105.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289  125.0000 -120.0000 67

 16 omega -116.00  -10.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075  -38.0000  -60.0000 106

 17 omega -116.00  -10.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075  -38.0000   30.0000 106

 18 omega -120.00   -4.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9075  -77.0000  -90.0000 116

 19 omega  -43.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9075  -77.0000   90.0000 117

 20 omega   32.00  162.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289   15.0000    0.0000 130

 21 omega   32.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5289   15.0000 -150.0000 146
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0549981000
_diffrn_orient_matrix_UB_12      0.0483704000
_diffrn_orient_matrix_UB_13      0.0744328000
_diffrn_orient_matrix_UB_21      0.0775608000
_diffrn_orient_matrix_UB_22      0.0838536000
_diffrn_orient_matrix_UB_23      0.0006889000
_diffrn_orient_matrix_UB_31      -0.0797142000
_diffrn_orient_matrix_UB_32      0.0481127000
_diffrn_orient_matrix_UB_33      -0.0757601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20141
_diffrn_reflns_theta_full        74.03
_diffrn_reflns_theta_max         74.03
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
In the absence of significant anomalous scattering, Friedel pairs were merged
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         5393
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0910P)^2^+0.1012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                4814
_reflns_number_total             5393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201087n_si_002.cif
_cod_data_source_block           db6082
_cod_database_code               4068093
_chemical_oxdiff_formula         'C27 B1 N2 O2 H36'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97