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_4068091
_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         'C27 H39 B N2'
_chemical_formula_sum            'C27 H39 B N2'
_chemical_formula_weight         402.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-03-15
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2010.12.31 svn.r1581, GUI svn.r3426)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.669(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   46.4335(19)
_cell_length_b                   7.3273(2)
_cell_length_c                   23.5143(10)
_cell_measurement_reflns_used    44112
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.54
_cell_volume                     7485.4(5)
_computing_data_collection       'STOE X-AREA'
_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
'SUPERFLIP : Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.'
_diffrn_ambient_temperature      180.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27046
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.53
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           35
_diffrn_source_power             1.93
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.028
_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   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0512P)^2^+2.0265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6997
_reflns_number_total             7932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201087n_si_002.cif
_cod_data_source_block           db5064
_cod_database_code               4068091