Catalytic Activation of Remote Alkenes through Silyl-Rhodium(III) Complexes
Prieto-Pascual, Unai; Martínez de Morentin, Aitor; Choquesillo-Lazarte, Duane; Rodríguez Diéguez, Antonio; Freixa, Zoraida; Huertos, Miguel A. A.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00624G

data_7713217
_publ_section_title
;
 Catalytic Activation of Remote Alkenes through Silyl-Rhodium(III)
 Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00624G
_journal_year                    2023
_chemical_formula_moiety         'C30 H30 Cl N P Rh Si'
_chemical_formula_sum            'C30 H30 Cl N P Rh Si'
_chemical_formula_weight         601.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-25 deposited with the CCDC.	2023-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                87.968(3)
_cell_angle_beta                 77.527(3)
_cell_angle_gamma                86.993(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8377(3)
_cell_length_b                   9.9596(3)
_cell_length_c                   13.8627(4)
_cell_measurement_reflns_used    14176
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.2540
_cell_measurement_theta_min      2.1060
_cell_volume                     1323.97(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25 122.08  104
  2  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25-135.92  104
  3  \w    -92.33  -0.33   1.00   69.00    --  -51.02  94.56 -34.84   92
  4  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25  20.08  104
  5  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25 173.08  104
  6  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25  71.08  104
  7  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25 -84.92  104
  8  \w    -72.51   6.49   1.00   69.00    --  -34.01  89.85  69.33   79
  9  \w    -72.51   6.49   1.00   69.00    --  -34.01  89.85-137.67   79
 10  \w    242.30 346.30   1.00   69.00    --  -34.01 -59.25 -33.92  104
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0080865000
_diffrn_orient_matrix_UB_12      -0.0218922000
_diffrn_orient_matrix_UB_13      -0.0491336000
_diffrn_orient_matrix_UB_21      -0.0458444000
_diffrn_orient_matrix_UB_22      -0.0525020000
_diffrn_orient_matrix_UB_23      0.0171930000
_diffrn_orient_matrix_UB_31      -0.0574212000
_diffrn_orient_matrix_UB_32      0.0430503000
_diffrn_orient_matrix_UB_33      -0.0061678000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33125
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.048
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0247P)^2^+1.5466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5819
_reflns_number_total             6562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00624g2.cif
_cod_data_source_block           1_L2
_cod_database_code               7713217
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              12719
_shelx_hkl_checksum              35342
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.380
_oxdiff_exptl_absorpt_empirical_full_min 0.780