Si-C(sp<sup>3</sup>) bond activation through oxidative addition at a Rh(i) centre.
Azpeitia, S.; Martínez-Martínez, A J; Garralda, M. A.; Weller, A. S.; Huertos, M. A.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5416–5419; doi:10.1039/d0dt00725k

data_7703838
_publ_section_title
;
 Si-C(sp<sup>3</sup>) bond activation through oxidative addition at a
 Rh(i) centre.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5416
_journal_page_last               5419
_journal_paper_doi               10.1039/d0dt00725k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H32 Rh S2 Si, C32 H12 B F24, C H2 Cl2'
_chemical_formula_sum            'C57 H46 B Cl2 F24 Rh S2 Si'
_chemical_formula_weight         1463.77
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                99.872(2)
_cell_angle_beta                 101.171(2)
_cell_angle_gamma                97.292(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4418(3)
_cell_length_b                   12.9564(3)
_cell_length_c                   20.2172(6)
_cell_measurement_reflns_used    17089
_cell_measurement_temperature    150.00(16)
_cell_measurement_theta_max      76.1320
_cell_measurement_theta_min      3.7540
_cell_volume                     3106.40(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -111.00 -20.00   1.00    5.00    --  -42.66 -38.00 120.00   91
  2  \w    -21.00  14.00   1.00    5.00    --  -42.66  38.00 120.00   35
  3  \w   -113.00 -19.00   1.00    5.00    --  -42.66 -57.00-120.00   94
  4  \w    -67.00  27.00   1.00    5.00    --  -42.66  57.00  30.00   94
  5  \w     52.00  79.00   1.00    5.00    --   42.66 -99.00  30.00   27
  6  \w     75.00 123.00   1.00    5.00    --   42.66 178.00 -90.00   48
  7  \w     42.00 113.00   1.00   20.00    --  111.00-125.00   0.00   71
  8  \w    121.00 178.00   1.00   20.00    --  111.00  61.00  30.00   57
  9  \w    115.00 141.00   1.00   20.00    --  111.00  45.00 150.00   26
 10  \w     87.00 150.00   1.00   20.00    --  111.00  77.00 -90.00   63
 11  \w     60.00  91.00   1.00   20.00    --  111.00 -30.00 120.00   31
 12  \w     44.00  96.00   1.00   20.00    --  111.00-125.00-180.00   52
 13  \w     82.00 121.00   1.00   20.00    --  111.00-125.00  30.00   39
 14  \w     65.00  98.00   1.00   20.00    --  111.00 -45.00-180.00   33
 15  \w     75.00 112.00   1.00   20.00    --  111.00-125.00-150.00   37
 16  \w    111.00 138.00   1.00   20.00    --  111.00 -77.00-180.00   27
 17  \w     46.00 120.00   1.00   20.00    --  111.00-125.00 150.00   74
 18  \w     99.00 169.00   1.00   20.00    --  111.00 125.00 150.00   70
 19  \w     61.00 105.00   1.00   20.00    --  111.00 -95.00   0.00   44
 20  \w    127.00 178.00   1.00   20.00    --  111.00 125.00-180.00   51
 21  \w     79.00 105.00   1.00   20.00    --  111.00 -95.00-120.00   26
 22  \w     87.00 174.00   1.00   20.00    --  111.00  45.00 -30.00   87
 23  \w     78.00 121.00   1.00   20.00    --  111.00-125.00 -90.00   43
 24  \w     66.00  92.00   1.00   20.00    --  111.00  15.00 -60.00   26
 25  \w    128.00 176.00   1.00   20.00    --  111.00  15.00 -60.00   48
 26  \w     40.00  94.00   1.00   20.00    --  111.00 -45.00 120.00   54
 27  \w     75.00 100.00   1.00   20.00    --  111.00 -95.00-180.00   25
 28  \w     81.00 163.00   1.00   20.00    --  111.00  77.00-150.00   82
 29  \w     83.00 133.00   1.00   20.00    --  111.00  61.00   0.00   50
 30  \w     59.00  90.00   1.00   20.00    --  111.00 -30.00  30.00   31
 31  \w     51.00  87.00   1.00   20.00    --  111.00 -45.00   0.00   36
 32  \w     30.00  56.00   1.00   20.00    --  111.00 -95.00   0.00   26
 33  \w     53.00  78.00   1.00   20.00    --  111.00 -77.00-180.00   25
 34  \w     94.00 177.00   1.00   20.00    --  111.00 125.00-150.00   83
 35  \w      2.00  32.00   1.00    5.00    --   38.00  90.00  58.65   30
 36  \w      7.00  33.00   1.00    5.00    --   42.00  88.00 -24.47   26
 37  \w      8.00  33.00   1.00    5.00    --   42.00  86.00-132.37   25
 38  \w   -113.00 -21.00   1.00    5.00    --  -42.66 -38.00 -30.00   92
 39  \w    -42.00 -16.00   1.00    5.00    --  -42.66 -57.00  30.00   26
 40  \w    -73.00 -60.00   1.00    5.00    --  -42.66  77.00 -90.00   13
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469697000
_diffrn_orient_matrix_UB_12      0.0551836000
_diffrn_orient_matrix_UB_13      0.0758180000
_diffrn_orient_matrix_UB_21      0.0241018000
_diffrn_orient_matrix_UB_22      -0.1069671000
_diffrn_orient_matrix_UB_23      0.0177296000
_diffrn_orient_matrix_UB_31      0.1165857000
_diffrn_orient_matrix_UB_32      0.0221412000
_diffrn_orient_matrix_UB_33      -0.0150147000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37489
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.274
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         12840
_refine_ls_number_restraints     1258
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0681P)^2^+2.9596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11306
_reflns_number_total             12840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00725k2.cif
_cod_data_source_block           164amm18
_cod_depositor_comments
'Adding full bibliography for 7703836--7703839.cif.'
_cod_original_cell_volume        3106.41(15)
_cod_database_code               7703838
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H66 Rh1 B1 F24 Si S2'
_shelx_estimated_absorpt_t_max   0.699
_shelx_estimated_absorpt_t_min   0.552
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F11-F10 \\sim F11-F12 \\sim F10-F12 \\sim F10A-F11A \\sim F10A-F12A \\sim
F11A-F12A
 with sigma of 0.04
 C40-F11 \\sim C40-F10 \\sim C40-F12 \\sim C40-F10A \\sim C40-F11A \\sim
C40-F12A
 with sigma of 0.02
 F16-F18 \\sim F16-F17 \\sim F18-F17 \\sim F18A-F17A \\sim F18A-F16A \\sim
F17A-F16A
 with sigma of 0.04
 C48-F16 \\sim C48-F18 \\sim C48-F17 \\sim C48-F18A \\sim C48-F17A \\sim
C48-F16A
 with sigma of 0.02
 F23-F24 \\sim F23-F22 \\sim F24-F22 \\sim F24A-F23A \\sim F24A-F22A \\sim
F23A-F22A
 with sigma of 0.04
 C56-F23 \\sim C56-F24 \\sim C56-F22 \\sim C56-F24A \\sim C56-F23A \\sim
C56-F22A
 with sigma of 0.02
 F15-F14 \\sim F15-F13 \\sim F14-F13 \\sim F14A-F13A \\sim F14A-F15A \\sim
F13A-F15A
 with sigma of 0.04
 C47-F15 \\sim C47-F14 \\sim C47-F13 \\sim C47-F14A \\sim C47-F13A \\sim
C47-F15A
 with sigma of 0.02
 F6-F5 \\sim F6-F4 \\sim F5-F4 \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.04
 C32-F6 \\sim C32-F5 \\sim C32-F4 \\sim C32-F4A \\sim C32-F5A \\sim C32-F6A
 with sigma of 0.02
 Si1-C9A \\sim Si1-C9
 with sigma of 0.02
 S2A-C8A \\sim S2-C8
 with sigma of 0.02
 S2A-C14A \\sim S2-C14
 with sigma of 0.02
 F19-F20 \\sim F19-F21 \\sim F20-F21 \\sim F21A-F20A \\sim F21A-F19A \\sim
F20A-F19A
 with sigma of 0.04
 C55-F19 \\sim C55-F20 \\sim C55-F21 \\sim C55-F21A \\sim C55-F20A \\sim
C55-F19A
 with sigma of 0.02
 Cl1-C57 \\sim Cl2A-C57A \\sim Cl1A-C57A \\sim Cl2-C57
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
3. Rigid bond restraints
 Cl1A, Cl2A, C57A, H57A, H57B, Cl1, Cl2, C57, H57C, H57D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S2 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
S2A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
H44 \\sim C48 \\sim F16 \\sim F17 \\sim F18 \\sim F16A \\sim F17A \\sim F18A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C32 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C56 \\sim F22 \\sim F23 \\sim F24 \\sim F22A \\sim F23A \\sim F24A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C55 \\sim F19 \\sim F20 \\sim F21 \\sim F19A \\sim F20A \\sim F21A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C40 \\sim F10 \\sim F11 \\sim F12 \\sim F10A \\sim F11A \\sim F12A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C48 \\sim F16 \\sim F17 \\sim F18 \\sim F16A \\sim F17A \\sim F18A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C47 \\sim F13 \\sim F14 \\sim F15 \\sim F13A \\sim F14A \\sim F15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
Cl1 \\sim Cl2 \\sim C57: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Cl1A \\sim Cl2A \\sim C57A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(Cl2) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(Cl1A)
\\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(C57A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C40, F10, F11, F12, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, F16, F17, F18, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, F22, F23, F24, F22A, F23A, F24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, C8, C9, C10, C11, C12, C13, C14, S2A, C8A, C9A, C10A, C11A, C12A, C13A,
 C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, F19, F20, F21, F19A, F20A, F21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl2, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1A, Cl2A, C57A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(4)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(5)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(5)
 Sof(S2A)=Sof(C8A)=Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(6)
 Sof(S2)=Sof(C8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(6)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(7)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(7)
 Fixed Sof: Cl1A(0.25) Cl2A(0.25) C57A(0.25) H57A(0.25) H57B(0.25) Cl1(0.75)
 Cl2(0.75) C57(0.75) H57C(0.75) H57D(0.75)
7.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C21(H21), C22(H22)
7.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B), C57A(H57A,
 H57B), C57(H57C,H57D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C26(H26), C28(H28), C30(H30),
 C34(H34), C36(H36), C38(H38), C42(H42), C44(H44), C46(H46), C50(H50), C52(H52),
  C54(H54)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C14(H14A,H14B,
 H14C), C14A(H14D,H14E,H14F)
;
_shelx_res_checksum              27448
_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 1.726
_oxdiff_exptl_absorpt_empirical_full_min 0.731