Rapid intramolecular heterolytic dihydrogen activation by a four-membered heterocyclic phosphane-borane adduct.
Spies, Patrick; Erker, Gerhard; Kehr, Gerald; Bergander, Klaus; Fröhlich, Roland; Grimme, Stefan; Stephan, Douglas W; Chemical communications (Cambridge, England)  (2007) 5072–5074; doi:10.1039/b710475h

data_7102324
_publ_section_title
;
 Rapid intramolecular heterolytic dihydrogen activation by a
 four-membered heterocyclic phosphane-borane adduct.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5072
_journal_page_last               5074
_journal_paper_doi               10.1039/b710475h
_journal_year                    2007
_chemical_formula_sum            'C39 H34 B F10 O P'
_chemical_formula_weight         750.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'at P from difmap, other geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.669(3)
_cell_angle_beta                 100.577(5)
_cell_angle_gamma                100.279(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1089(8)
_cell_length_b                   12.7662(10)
_cell_length_c                   12.8752(8)
_cell_measurement_reflns_used    5261
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1839.0(2)
_computing_cell_refinement       'Collect (Nonius B.V., 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinwoski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.078
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20114
_diffrn_reflns_theta_full        67.93
_diffrn_reflns_theta_max         67.93
_diffrn_reflns_theta_min         4.36
_exptl_absorpt_coefficient_mu    1.385
_exptl_absorpt_correction_T_max  0.9340
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0774
_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^)+(0.0947P)^2^+3.3191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2265
_reflns_number_gt                4081
_reflns_number_total             6171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710475h.txt
_cod_data_source_block           erk4157b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102324