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_7001971
_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            'C33 H30 B F15 N2 O'
_chemical_formula_weight         766.40
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.3740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.16670(10)
_cell_length_b                   20.9206(3)
_cell_length_c                   15.2247(2)
_cell_measurement_reflns_used    15114
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2314
_cell_measurement_theta_min      1.9414
_cell_volume                     3211.41(7)
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67546
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96601
_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            clourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                3855
_reflns_number_total             6570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b908074k.txt
_cod_data_source_block           dhol41
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7001971