Rhodium-Catalyzed Dehydrocoupling of the Sterically Encumbered Phosphine-Borane Adduct tBu2PH.BH3: Synthesis of the Linear Dimers tBu2PH-BH2-tBu2P-BH3 and tBu2PH-BH2-tBu2P-BH2Cl
Hendrik Dorn; Emira Vejzovic; Alan J. Lough; Ian Manners; Inorganic Chemistry 40 (2001) 4327–4331; doi:10.1021/ic0100626

data_4320056
_publ_section_title
;
 Rhodium-Catalyzed Dehydrocoupling of the Sterically Encumbered
 Phosphine-Borane Adduct tBu2PH.BH3: Synthesis of the Linear Dimers
 tBu2PH-BH2-tBu2P-BH3 and tBu2PH-BH2-tBu2P-BH2Cl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4327
_journal_page_last               4331
_journal_paper_doi               10.1021/ic0100626
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C16 H41.21 B2 Cl0.79 P2'
_chemical_formula_weight         345.18
_chemical_name_systematic
;
  ?
;
_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                 101.857(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7446(3)
_cell_length_b                   24.6411(9)
_cell_length_c                   10.4574(5)
_cell_measurement_reflns_used    6348
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.59
_cell_volume                     2205.25(15)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'Bruker SHELXTL V5.1'
_computing_structure_solution    'Bruker SHELXTL V5.1'
_diffrn_ambient_temperature      240(1)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.028
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16496
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9397
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowki & Minor, 1997)'
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0570P)^2^+0.4946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                4182
_reflns_number_total             6348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100626_3.cif
_cod_data_source_block           k00109ra
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C16 H3 H38.21 B2 Cl0.79 P2'
_cod_database_code               4320056