Dehydrogenation reactivity of a frustrated carbene–borane Lewis pair
Holschumacher, Dirk; Taouss, Christina; Bannenberg, Thomas; Hrib, Cristian G.; Daniliuc, Constantin G.; Jones, Peter G.; Tamm, M.; Dalton Transactions  (2009) 6927–; doi:10.1039/b908074k

data_7001970
_publ_section_title
;
 Dehydrogenation reactivity of a frustrated carbene--borane Lewis pair
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              6927
_journal_paper_doi               10.1039/b908074k
_journal_year                    2009
_chemical_formula_sum            'C29 H24 B F15 N2'
_chemical_formula_weight         696.31
_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                 106.959(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3321(4)
_cell_length_b                   9.7938(2)
_cell_length_c                   19.7688(4)
_cell_measurement_reflns_used    11028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1737
_cell_measurement_theta_min      2.0711
_cell_volume                     2839.39(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.36 (release 29-09-2008 CrysAlis171 .NET)
(compiled Sep 29 2008,12:11:20)
;
_computing_data_collection
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.36 (release 29-09-2008 CrysAlis171 .NET)
(compiled Sep 29 2008,12:11:20)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.36 (release 29-09-2008 CrysAlis171 .NET)
(compiled Sep 29 2008,12:11:20)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53738
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.36 (release 29-09-2008 CrysAlis171 .NET)
(compiled Sep 29 2008,12:11:20)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment
;
H1, H2 free refined but thermal parameter were fixed,
rigid methyls, others riding
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                3357
_reflns_number_total             5800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908074k.txt
_cod_data_source_block           dhol40
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001970