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_7703839
_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         'C20 H26 N2 Rh S2 Si, C32 H12 B F24'
_chemical_formula_sum            'C52 H38 B F24 N2 Rh S2 Si'
_chemical_formula_weight         1352.77
_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                64.937(3)
_cell_angle_beta                 82.448(3)
_cell_angle_gamma                74.530(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0258(4)
_cell_length_b                   14.6748(5)
_cell_length_c                   16.5971(6)
_cell_measurement_reflns_used    15479
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.8160
_cell_measurement_theta_min      2.9370
_cell_volume                     2769.10(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_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     44.00  91.00   1.00    1.50    --    0.00  57.00-150.00   47
  2  \w     11.00  40.00   1.00    1.50    --    0.00 -99.00-150.00   29
  3  \w    -93.00 -36.00   1.00    1.50    --    0.00-178.00 -60.00   57
  4  \w    -29.00  35.00   1.00    1.50    --    0.00  57.00-150.00   64
  5  \w    -97.00 -68.00   1.00    6.00    --  -59.95  77.00-150.00   29
  6  \w    -23.00  18.00   1.00    6.00    --  -59.95  77.00-150.00   41
  7  \w    -56.00  10.00   1.00    6.00    --  -59.95  45.00-150.00   66
  8  \w   -159.00  24.00   1.00    6.00    --  -59.95  15.00 120.00  183
  9  \w    105.00 133.00   1.00    6.00    --   59.95 125.00-120.00   28
 10  \w    103.00 135.00   1.00    6.00    --   59.95 125.00  60.00   32
 11  \w    110.00 150.00   1.00    6.00    --   59.95 125.00 120.00   40
 12  \w     94.00 152.00   1.00    6.00    --   59.95 125.00  30.00   58
 13  \w    112.00 151.00   1.00    6.00    --   59.95 125.00-180.00   39
 14  \w     44.00 118.00   1.00    6.00    --   59.95-125.00-120.00   74
 15  \w     71.00 112.00   1.00    9.00    --  119.91-111.00 -60.00   41
 16  \w    100.00 126.00   1.00    9.00    --  119.91 111.00  60.00   26
 17  \w     63.00  89.00   1.00    9.00    --  119.91-111.00   0.00   26
 18  \w     29.00  81.00   1.00    9.00    --  119.91 -37.00 120.00   52
 19  \w     25.00 177.00   1.00    9.00    --  119.91   0.00  60.00  152
 20  \w     30.00 102.00   1.00    9.00    --  119.91 -50.00-180.00   72
 21  \w     50.00  87.00   1.00    9.00    --  119.91 -25.00  30.00   37
 22  \w     34.00  92.00   1.00    9.00    --  119.91 -37.00 -30.00   58
 23  \w     29.00 112.00   1.00    9.00    --  119.91-111.00-180.00   83
 24  \w     41.00  66.00   1.00    9.00    --  119.91 -25.00-180.00   25
 25  \w     64.00  98.00   1.00    9.00    --  119.91-111.00-120.00   34
 26  \w     67.00  93.00   1.00    9.00    --  119.91 -50.00  60.00   26
 27  \w     66.00  91.00   1.00    9.00    --  119.91 -50.00 120.00   25
 28  \w     99.00 177.00   1.00    9.00    --  119.91  63.00  60.00   78
 29  \w     30.00  92.00   1.00    9.00    --  119.91 -37.00 -90.00   62
 30  \w     86.00 112.00   1.00    9.00    --  119.91-111.00  30.00   26
 31  \w     66.00 104.00   1.00    9.00    --  119.91-111.00 120.00   38
 32  \w    143.00 176.00   1.00    9.00    --  119.91 111.00  60.00   33
 33  \w     43.00 151.00   1.00    9.00    --  119.91 -77.00 -30.00  108
 34  \w    -95.00 -63.00   1.00    1.50    --    0.00 -66.00  49.00   32
 35  \w    -54.00  33.00   1.00    1.50    --    0.00 -66.00  49.00   87
 36  \w      5.00  51.00   1.00    1.50    --    0.00 -99.00  90.00   46
 37  \w    -40.00  -8.00   1.00    1.50    --   22.00 122.00 174.71   32
 38  \w     -1.00  26.00   1.00    6.00    --   46.00  94.00 -25.50   27
 39  \w      2.00  27.00   1.00    6.00    --   50.00  92.00 107.04   25
 40  \w      3.00  31.00   1.00    6.00    --   50.00  90.00 -83.83   28
 41  \w   -140.00  43.00   1.00    6.00    --  -59.95 -15.00 -60.00  183
 42  \w     16.00  41.00   1.00    6.00    --   59.95  81.00 118.98   25
 43  \w     16.00  41.00   1.00    6.00    --   59.95  81.00 -24.55   25
 44  \w     17.00  43.00   1.00    6.00    --   59.95  82.00-136.99   26
 45  \w     18.00  43.00   1.00    6.00    --   62.00  82.00  28.62   25
 46  \w     18.00  43.00   1.00    6.00    --   62.00  80.00  64.85   25
 47  \w     18.00  43.00   1.00    6.00    --   62.00  80.00 -69.98   25
 48  \w     19.00  45.00   1.00    6.00    --   62.00  82.00-179.93   26
 49  \w     18.00  43.00   1.00    6.00    --   62.00  80.00 156.87   25
 50  \w     30.00  89.00   1.00    6.00    --   74.00  64.00-158.84   59
 51  \w     30.00  65.00   1.00    6.00    --   74.00  77.00 -20.29   35
 52  \w     35.00  65.00   1.00    6.00    --   78.00  75.00-120.24   30
 53  \w     34.00  81.00   1.00    6.00    --   78.00  77.00 -70.05   47
 54  \w     40.00  67.00   1.00    6.00    --   82.00  67.00  88.33   27
 55  \w     43.00  69.00   1.00    6.00    --   86.00  71.00  52.90   26
 56  \w     42.00  68.00   1.00    6.00    --   86.00  77.00  94.93   26
 57  \w     51.00  78.00   1.00    9.00    --   94.00  74.00   5.11   27
 58  \w     52.00  77.00   1.00    9.00    --   94.00  62.00 143.15   25
 59  \w     51.00  78.00   1.00    9.00    --   94.00  74.00  97.91   27
 60  \w     55.00  91.00   1.00    9.00    --   98.00  70.00-110.55   36
 61  \w     60.00  95.00   1.00    9.00    --  102.00  66.00 143.17   35
 62  \w     59.00  93.00   1.00    9.00    --  102.00  76.00-149.63   34
 63  \w     71.00  97.00   1.00    9.00    --  114.00  69.00 -41.42   26
 64  \w     76.00 111.00   1.00    9.00    --  119.91  77.00  30.00   35
 65  \w     76.00 123.00   1.00    9.00    --  119.91  63.00 -60.00   47
 66  \w     77.00 102.00   1.00    9.00    --  119.91  63.00 -90.00   25
 67  \w     76.00 146.00   1.00    9.00    --  119.91  77.00 150.00   70
 68  \w     76.00 110.00   1.00    9.00    --  119.91  77.00 -90.00   34
;
_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      -0.0926613000
_diffrn_orient_matrix_UB_12      0.0964147000
_diffrn_orient_matrix_UB_13      -0.0350729000
_diffrn_orient_matrix_UB_21      0.0227939000
_diffrn_orient_matrix_UB_22      0.0348752000
_diffrn_orient_matrix_UB_23      0.0699576000
_diffrn_orient_matrix_UB_31      0.0772034000
_diffrn_orient_matrix_UB_32      0.0608638000
_diffrn_orient_matrix_UB_33      -0.0661867000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34308
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.970
_diffrn_reflns_theta_min         2.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.626
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         11318
_refine_ls_number_restraints     950
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0899P)^2^+4.9989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10301
_reflns_number_total             11318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00725k2.cif
_cod_data_source_block           172amm18re
_cod_depositor_comments
'Adding full bibliography for 7703836--7703839.cif.'
_cod_database_code               7703839
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H66 Ir S2 N2 B1 F24'
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.533
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Restrained distances
 F17-F16 \\sim F17-F18 \\sim F17A-F16A \\sim F17A-F18A \\sim F16A-F18A \\sim
F16-F18
 with sigma of 0.04
 F4-F6 \\sim F4-F5 \\sim F4A-F6A \\sim F4A-F5A \\sim F6A-F5A \\sim F6-F5
 with sigma of 0.04
 C52-F17 \\sim C52-F17A \\sim C52-F16A \\sim C52-F16 \\sim C52-F18A \\sim
C52-F18
 with sigma of 0.02
 C28-F4 \\sim C28-F4A \\sim C28-F6A \\sim C28-F6 \\sim C28-F5 \\sim C28-F5A
 with sigma of 0.02
 F11A-F12A \\sim F11A-F10A \\sim F11-F12 \\sim F11-F10 \\sim F12-F10 \\sim
F12A-F10A
 with sigma of 0.04
 C36-F11A \\sim C36-F11 \\sim C36-F12 \\sim C36-F12A \\sim C36-F10A \\sim
C36-F10
 with sigma of 0.02
 S2A-C14A \\sim S2-C14
 with sigma of 0.02
 Rh1-S2A \\sim Rh1-S2
 with sigma of 0.02
 S2A-C8A \\sim S2-C8
 with sigma of 0.02
 C9A-C8A \\sim C9-C8 \\sim C13-C8 \\sim C13A-C8A \\sim C13A-C12A \\sim C13-C12
\\sim C12A-C11A \\sim C12-
 C11 \\sim C11-C10 \\sim C11A-C10A \\sim C10A-C9A \\sim C10-C9
 with sigma of 0.02
 Si1-C9 \\sim Si1-C9A
 with sigma of 0.02
 F22-F24 \\sim F22-F23 \\sim F22A-F24A \\sim F22A-F23A \\sim F24A-F23A \\sim
F24-F23
 with sigma of 0.04
 C44-F22 \\sim C44-F22A \\sim C44-F24A \\sim C44-F24 \\sim C44-F23 \\sim
C44-F23A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C52 \\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
C28 \\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
C36 \\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
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
C44 \\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
4. Rigid body (RIGU) restrains
 C52, F16, F17, F18, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, F10, F11, F12, F10A, F11A, F12A
 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
 C44, F22, F23, F24, F22A, F23A, F24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(1)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 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(H14F)=Sof(H14E)=1-FVAR(4)
 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(H14B)=Sof(H14C)=Sof(H14A)=FVAR(4)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(5)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(5)
6.a 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), C22(H22), C24(H24), C26(H26),
 C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42), C46(H46), C48(H48),
  C50(H50)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C14(H14B,H14C,H14A), C14A(H14D,H14F,H14E)
;
_shelx_res_checksum              52309
_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 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.693