Ph2P(BH3)Li: From Ditopicity to Dual Reactivity
Gabriella Barozzino Consiglio; Pierre Queval; Anne Harrison-Marchand; Alessandro Mordini; Jean-François Lohier; Olivier Delacroix; Annie-Claude Gaumont; Hélène Gérard; Jacques Maddaluno; Hassan Oulyadi; Journal of the American Chemical Society 133 (2011) 6472–6480; doi:10.1021/ja201760c

data_4106056
_publ_contact_author_address
;     
Laboratoire de Chimie Mol\'eculaire et Thio-organique,
UMR CNRS 6507, FR CNRS 3038 INC3M,
ENSICAEN - Universit\'e de Caen, 14050 Caen, France

;
_publ_contact_author_email       annie-claude.gaumont@ensicaen.fr
_publ_contact_author_fax         '332 31 45 28 77'
_publ_contact_author_name        'Gaumont, Annie-Claude'
_publ_contact_author_phone       '332 31 45 28 73'
_publ_section_title
;
 Ph2P(BH3)Li: From Ditopicity to Dual Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6472
_journal_page_last               6480
_journal_paper_doi               10.1021/ja201760c
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C20 H19 B N O P'
_chemical_formula_sum            'C20 H19 B N O P'
_chemical_formula_weight         331.14
_chemical_name_systematic
; 
 1-Hydroxy-1-(4-cyanophenyl))methyldiphenylphosphine-borane 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.140(2)
_cell_angle_beta                 82.4840(10)
_cell_angle_gamma                80.8710(10)
_cell_formula_units_Z            4
_cell_length_a                   9.8401(3)
_cell_length_b                   13.3270(4)
_cell_length_c                   13.9118(4)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      2.43
_cell_volume                     1781.98(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48093
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.5576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                8552
_reflns_number_total             9969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201760c_si_001.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4106056