14-Electron Rh and Ir silylphosphine complexes and their catalytic activity in alkene functionalization with hydrosilanes.
Abeynayake, Niroshani S.; Zamora-Moreno, Julio; Gorla, Saidulu; Donnadieu, Bruno; Muñoz-Hernández, Miguel A; Montiel-Palma, Virginia; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11783–11792; doi:10.1039/d1dt00677k

data_7707935
_publ_section_title
;
 14-Electron Rh and Ir silylphosphine complexes and their catalytic
 activity in alkene functionalization with hydrosilanes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11783
_journal_page_last               11792
_journal_paper_doi               10.1039/d1dt00677k
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H45 Br P Rh Si2'
_chemical_formula_sum            'C32 H45 Br P Rh Si2'
_chemical_formula_weight         699.65
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-09-08 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4574(11)
_cell_length_b                   11.4574(11)
_cell_length_c                   24.066(4)
_cell_measurement_reflns_used    1105
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.572
_cell_measurement_theta_min      1.969
_cell_volume                     3159.2(7)
_computing_cell_refinement       'APEX3 v2019.1.0'
_computing_data_collection       'APEX3 v2019.1.0'
_computing_data_reduction        'Saint, APEX v2019.1.0.'
_computing_molecular_graphics    'Mercury V.4.2.0,POV-Ray v 3.7'
_computing_publication_material  'APEX3 v2019.1.0'
_computing_structure_refinement  SHELXTL-2018/3
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS D8 Venture  '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40461
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         1.969
_exptl_absorpt_coefficient_mu    1.952
_exptl_absorpt_correction_T_max  0.599
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.579
_exptl_crystal_size_mid          0.452
_exptl_crystal_size_min          0.293
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.052(6)
_refine_ls_extinction_coef       0.0030(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6936
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+0.2739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.883
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                6838
_reflns_number_total             6936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00677k2.cif
_cod_data_source_block           Rh3
_cod_depositor_comments
'Adding full bibliography for 7707933--7707936.cif.'
_cod_original_cell_volume        3159.3(8)
_cod_database_code               7707935
_shelx_estimated_absorpt_t_min   0.398
_shelx_estimated_absorpt_t_max   0.599
_shelx_res_checksum              71669
_shelx_hkl_checksum              48476