Activation of B-H, Si-H, and C-F Bonds with Tp'Rh(PMe3) Complexes: Kinetics, Mechanism, and Selectivity.
Procacci, Barbara; Jiao, Yunzhe; Evans, Meagan E.; Jones, William D.; Perutz, Robin N.; Whitwood, Adrian C.; Journal of the American Chemical Society 137 (2015) 1258–1272; doi:10.1021/ja5113172

data_4123234
_publ_section_title
;
 Activation of B-H, Si-H, and C-F Bonds with Tp'Rh(PMe3) Complexes:
 Kinetics, Mechanism, and Selectivity.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1258
_journal_page_last               1272
_journal_paper_doi               10.1021/ja5113172
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C22 H43 B N6 P Rh Si'
_chemical_formula_sum            'C22 H43 B N6 P Rh Si'
_chemical_formula_weight         564.40
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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             2011-03-28
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                65.602(8)
_cell_angle_beta                 72.784(7)
_cell_angle_gamma                65.226(7)
_cell_formula_units_Z            2
_cell_length_a                   10.8404(7)
_cell_length_b                   11.5332(9)
_cell_length_c                   13.5457(11)
_cell_measurement_reflns_used    6104
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.8569
_cell_measurement_theta_min      3.1806
_cell_volume                     1384.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9943
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
  1 omega  -45.00   46.00   1.0000    7.2100
omega____ theta____ kappa____ phi______ frames
    -      -14.9940   77.0000  -60.0000 91

  2 omega  -12.00   82.00   1.0000    7.2100
omega____ theta____ kappa____ phi______ frames
    -       16.3221   77.0000 -180.0000 94

  3 omega  -51.00   43.00   1.0000    7.2100
omega____ theta____ kappa____ phi______ frames
    -       16.3221  -77.0000   60.0000 94

  4 omega  -87.00   11.00   1.0000    7.2100
omega____ theta____ kappa____ phi______ frames
    -      -14.9940  -37.0000  150.0000 98

  5 omega  -45.00   30.00   1.0000    7.2100
omega____ theta____ kappa____ phi______ frames
    -      -14.9940   77.0000   90.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0301706000
_diffrn_orient_matrix_UB_12      -0.0396638000
_diffrn_orient_matrix_UB_13      -0.0349437000
_diffrn_orient_matrix_UB_21      0.0659751000
_diffrn_orient_matrix_UB_22      -0.0038001000
_diffrn_orient_matrix_UB_23      0.0025440000
_diffrn_orient_matrix_UB_31      0.0055832000
_diffrn_orient_matrix_UB_32      -0.0596726000
_diffrn_orient_matrix_UB_33      0.0463337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12496
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.2635
_exptl_crystal_size_mid          0.1224
_exptl_crystal_size_min          0.0927
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0240P)^2^+0.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                4898
_reflns_number_total             5656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5113172_si_002.cif
_cod_data_source_block           rnp1109
_cod_depositor_comments
'Adding full bibliography for 4123232--4123234.cif.'
_cod_database_code               4123234
_chemical_oxdiff_formula         'C22H43B N6P Rh Si'
_chemical_oxdiff_usercomment     Rh1Et2SiH2-Barby`s
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.01