Formation of Chlorosilyl Pincer-Type Rhodium Complexes by Multiple Si–H Activations of Bis(phosphine)/Dihydrosilyl Ligands
Whited, Matthew T.; Deetz, Alexander M.; Boerma, Joseph W.; DeRosha, Daniel E.; Janzen, Daron E.; Organometallics 33 (2014) 5070–; doi:10.1021/om5006319

data_4084701
_publ_section_title
;
 Formation of Chlorosilyl Pincer-Type Rhodium Complexes by Multiple Si--H
 Activations of Bis(phosphine)/Dihydrosilyl Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5070
_journal_paper_doi               10.1021/om5006319
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C36 H30 P2 Si'
_chemical_formula_sum            'C36 H30 P2 Si'
_chemical_formula_weight         552.63
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                110.145(8)
_cell_angle_beta                 90.794(6)
_cell_angle_gamma                101.593(7)
_cell_formula_units_Z            2
_cell_length_a                   10.0297(10)
_cell_length_b                   11.3624(12)
_cell_length_c                   14.2414(15)
_cell_measurement_reflns_used    12757
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.10
_cell_volume                     1486.5(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13'
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.060
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.7656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                5168
_reflns_number_total             6795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5006319_si_002.cif
_cod_data_source_block           scu1229_compound1
_cod_database_code               4084701
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              7927
_shelx_hkl_checksum              50484