Boronation of 1,8-Bis(diphenylphosphino)naphthalene: Formation of Cyclic Boronium Salts⊥
Owsianik, Krzysztof; Chauvin, Remi; Balińska, Agnieszka; Wieczorek, Michał; Cypryk, Marek; Mikołajczyk, Marian; Organometallics 28 (2009) 4929–; doi:10.1021/om900017n

data_4069091
_publ_section_title
;
 Boronation of 1,8-Bis(diphenylphosphino)naphthalene: Formation of Cyclic
 Boronium Salts&#x22A5;
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4929
_journal_paper_doi               10.1021/om900017n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C34 H28 B P2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C35 H30 B Cl2 F6 P3'
_chemical_formula_weight         739.21
_chemical_name_systematic
;
[1,8-Bis(diphenylphosphanyl)naphthalene]dihydroboron Hexafluorophosphate
;
_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_date             2006-01-16T13:39:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.72(3)
_cell_angle_beta                 85.66(3)
_cell_angle_gamma                72.35(3)
_cell_formula_units_Z            2
_cell_length_a                   11.964(3)
_cell_length_b                   12.191(3)
_cell_length_c                   12.717(3)
_cell_measurement_reflns_used    18111
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      38.74
_cell_measurement_theta_min      4.45
_cell_volume                     1667.8(8)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'PLATON (Spek,2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur PX CCD \k-geometry diffractometer'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37897
_diffrn_reflns_theta_full        35
_diffrn_reflns_theta_max         35
_diffrn_reflns_theta_min         4.45
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         14518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                10106
_reflns_number_total             14518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900017n_si_001.cif
_cod_data_source_block           bal0dc
_cod_database_code               4069091