Dehydrocoupling of Phosphine-Boranes Using the [RhCp*Me(PMe3)(CH2Cl2)][BArF4] Precatalyst: Stoichiometric and Catalytic Studies
Hooper, Thomas N.; Weller, Andrew; Beattie, Nicholas A.; Macgregor, Stuart Alan; Chem. Sci.  (2015) –; doi:10.1039/C5SC04150C

data_1540713
_publ_section_title
;
 Dehydrocoupling of Phosphine-Boranes Using the
 [RhCp*Me(PMe3)(CH2Cl2)][BArF4] Precatalyst: Stoichiometric and Catalytic
 Studies
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C5SC04150C
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C25 H49 B P2 Rh'
_chemical_formula_sum            'C57 H61 B2 F24 P2 Rh'
_chemical_formula_weight         1388.52
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.155(3)
_cell_length_b                   13.139(3)
_cell_length_c                   35.677(7)
_cell_measurement_reflns_used    14438
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     6139(2)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1310
_diffrn_reflns_av_unetI/netI     0.2008
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            26843
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         5.128
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.938536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       plate
_exptl_crystal_F_000             2816
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane Pentane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.584
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13953
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6203
_reflns_number_total             13953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04150c3.cif
_cod_data_source_block           7
_cod_database_code               1540713
_shelxl_version_number           2014-3
_shelx_res_checksum              9615