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_7703837
_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
'C23 H28 Rh S2 Si, 2(C H2 Cl2), C32 H12 B F24'
_chemical_formula_sum            'C57 H44 B Cl4 F24 Rh S2 Si'
_chemical_formula_weight         1532.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                90
_cell_angle_beta                 105.0030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2033(2)
_cell_length_b                   12.75000(10)
_cell_length_c                   38.5848(3)
_cell_measurement_reflns_used    70019
_cell_measurement_temperature    150.01(14)
_cell_measurement_theta_max      76.1980
_cell_measurement_theta_min      3.6180
_cell_volume                     12451.46(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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(14)
_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 0.993
_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    -82.00  41.00   1.00    2.00    --  -42.66   0.00 150.00  123
  2  \w     81.00 124.00   1.00    2.00    --   42.66 178.00 -90.00   43
  3  \w   -121.00 -56.00   1.00    2.00    --  -42.66 178.00-120.00   65
  4  \w    143.00 173.00   1.00    8.00    --  111.00 117.00 -26.00   30
  5  \w     82.00 175.00   1.00    8.00    --  111.00  15.00-180.00   93
  6  \w     84.00 109.00   1.00    8.00    --  111.00 -95.00-120.00   25
  7  \w     93.00 120.00   1.00    8.00    --  111.00-125.00-120.00   27
  8  \w     68.00  94.00   1.00    8.00    --  111.00 -45.00-150.00   26
  9  \w     50.00  91.00   1.00    8.00    --  111.00 -30.00-150.00   41
 10  \w     63.00  94.00   1.00    8.00    --  111.00 -45.00 -60.00   31
 11  \w     50.00  89.00   1.00    8.00    --  111.00 -30.00 -30.00   39
 12  \w     39.00  86.00   1.00    8.00    --  111.00 -30.00  30.00   47
 13  \w     36.00  90.00   1.00    8.00    --  111.00 -30.00  90.00   54
 14  \w     31.00  90.00   1.00    8.00    --  111.00 -95.00   0.00   59
 15  \w     51.00 117.00   1.00    8.00    --  111.00-125.00   0.00   66
 16  \w     40.00  82.00   1.00    8.00    --  111.00-125.00-120.00   42
 17  \w     37.00 124.00   1.00    8.00    --  111.00 -77.00-120.00   87
 18  \w   -111.00 -24.00   1.00    2.00    --  -42.66 -38.00 120.00   87
 19  \w     62.00 119.00   1.00    2.00    --   42.66 178.00   0.00   57
 20  \w     63.00 121.00   1.00    2.00    --   42.66  19.00-150.00   58
 21  \w     60.00 118.00   1.00    2.00    --   42.66-178.00 120.00   58
 22  \w     40.00  90.00   1.00    8.00    --  111.00 -45.00  30.00   50
 23  \w    111.00 142.00   1.00    8.00    --  111.00 -77.00  30.00   31
 24  \w     56.00 109.00   1.00    8.00    --  111.00 -95.00  90.00   53
 25  \w     77.00 155.00   1.00    8.00    --  111.00 -15.00  60.00   78
 26  \w     92.00 121.00   1.00    8.00    --  111.00-125.00  90.00   29
 27  \w     74.00 116.00   1.00    8.00    --  111.00-125.00  60.00   42
 28  \w     93.00 119.00   1.00    8.00    --  111.00  45.00  60.00   26
 29  \w     55.00  83.00   1.00    8.00    --  111.00 -77.00  30.00   28
 30  \w     43.00  69.00   1.00    8.00    --  111.00 -15.00  60.00   26
 31  \w     72.00 121.00   1.00    8.00    --  111.00-125.00-150.00   49
 32  \w     88.00 116.00   1.00    8.00    --  111.00-125.00 -90.00   28
 33  \w     39.00  77.00   1.00    8.00    --  111.00-125.00 -90.00   38
 34  \w     45.00  77.00   1.00    8.00    --  111.00 -45.00  90.00   32
 35  \w     42.00  79.00   1.00    8.00    --  111.00 -15.00-180.00   37
 36  \w     82.00 144.00   1.00    8.00    --  111.00 -15.00-180.00   62
 37  \w     48.00  75.00   1.00    8.00    --  111.00 -77.00-180.00   27
 38  \w     71.00  97.00   1.00    2.00    --   42.66 178.00-180.00   26
 39  \w     50.00  76.00   1.00    8.00    --  111.00 -30.00 -60.00   26
 40  \w    109.00 135.00   1.00    8.00    --  111.00  30.00 120.00   26
 41  \w    124.00 173.00   1.00    8.00    --  111.00  30.00  60.00   49
 42  \w      3.00  28.00   1.00    2.00    --   38.00  89.00-111.29   25
 43  \w      1.00  26.00   1.00    2.00    --   38.00  93.00   7.61   25
 44  \w     -6.00  26.00   1.00    2.00    --  -42.66  57.00 150.00   32
 45  \w   -112.00 -16.00   1.00    2.00    --  -42.66 -57.00   0.00   96
 46  \w    -68.00 -22.00   1.00    2.00    --  -42.66 -38.00  30.00   46
 47  \w     13.00  38.00   1.00    2.00    --   46.00  83.00-178.06   25
 48  \w     14.00  46.00   1.00    2.00    --   46.00  80.00 113.40   32
 49  \w     19.00  44.00   1.00    2.00    --   50.00  81.00 -87.26   25
 50  \w     22.00  47.00   1.00    2.00    --   54.00  78.00 -27.15   25
 51  \w     22.00  47.00   1.00    2.00    --   54.00  78.00  67.57   25
 52  \w     31.00  57.00   1.00    2.00    --   62.00  75.00 115.34   26
 53  \w     34.00  60.00   1.00    2.00    --   62.00  75.00 -26.50   26
 54  \w     77.00 104.00   1.00    2.00    --   62.00  75.00 115.34   27
 55  \w     35.00  66.00   1.00    2.00    --   66.00  75.00  17.96   31
 56  \w     35.00  61.00   1.00    2.00    --   66.00  75.00 161.74   26
 57  \w     39.00  65.00   1.00    2.00    --   70.00  75.00  65.04   26
 58  \w     39.00  65.00   1.00    2.00    --   70.00  74.00-175.99   26
 59  \w     39.00  65.00   1.00    2.00    --   70.00  77.00-122.29   26
 60  \w    106.00 132.00   1.00    2.00    --   70.00  76.00  -6.00   26
 61  \w     39.00  65.00   1.00    2.00    --   70.00  76.00 -84.58   26
 62  \w     39.00  65.00   1.00    2.00    --   70.00  77.00-150.96   26
 63  \w     39.00  64.00   1.00    2.00    --   70.00  76.00  -6.00   25
 64  \w     43.00  69.00   1.00    2.00    --   74.00  76.00 115.40   26
 65  \w     49.00  74.00   1.00    2.00    --   74.00  69.00  92.65   25
 66  \w     47.00  77.00   1.00    8.00    --   78.00  75.00 -75.87   30
 67  \w     53.00  87.00   1.00    8.00    --   82.00  68.00   8.19   34
 68  \w     55.00  81.00   1.00    8.00    --   82.00  60.00-176.75   26
 69  \w     56.00  83.00   1.00    8.00    --   86.00  73.00-120.24   27
 70  \w     55.00  82.00   1.00    8.00    --   86.00  77.00 121.63   27
 71  \w     60.00  86.00   1.00    8.00    --   86.00  56.00 -19.30   26
 72  \w     58.00 142.00   1.00    8.00    --   86.00  66.00  59.89   84
 73  \w     59.00  86.00   1.00    8.00    --   90.00  77.00 171.96   27
 74  \w     80.00 147.00   1.00    8.00    --  111.00  77.00-120.00   67
 75  \w     80.00 106.00   1.00    8.00    --  111.00  77.00 150.00   26
 76  \w     80.00 111.00   1.00    8.00    --  111.00  77.00  90.00   31
 77  \w     86.00 113.00   1.00    8.00    --  111.00  61.00 120.00   27
 78  \w     80.00 118.00   1.00    8.00    --  111.00  77.00 -90.00   38
 79  \w     83.00 119.00   1.00    8.00    --  111.00  61.00  90.00   36
 80  \w     80.00 121.00   1.00    8.00    --  111.00  77.00   0.00   41
 81  \w     85.00 129.00   1.00    8.00    --  111.00  61.00-180.00   44
 82  \w     83.00 121.00   1.00    8.00    --  111.00  61.00   0.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0416361000
_diffrn_orient_matrix_UB_12      -0.0396911000
_diffrn_orient_matrix_UB_13      -0.0186829000
_diffrn_orient_matrix_UB_21      0.0076511000
_diffrn_orient_matrix_UB_22      0.1126962000
_diffrn_orient_matrix_UB_23      -0.0121644000
_diffrn_orient_matrix_UB_31      0.0437378000
_diffrn_orient_matrix_UB_32      0.0180854000
_diffrn_orient_matrix_UB_33      0.0348124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            127558
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.429
_diffrn_reflns_theta_min         3.493
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       prism
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         12964
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+25.1611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12233
_reflns_number_total             12964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00725k2.cif
_cod_data_source_block           165amm18
_cod_depositor_comments
'Adding full bibliography for 7703836--7703839.cif.'
_cod_original_cell_volume        12451.45(18)
_cod_database_code               7703837
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H70 Rh1 B1 F24 Si1 S2 Cl4'
_shelx_estimated_absorpt_t_max   0.432
_shelx_estimated_absorpt_t_min   0.334
_reflns_odcompleteness_completeness 99.89
_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
 F23-F21 \\sim F23-F22 \\sim F21-F22 \\sim F23A-F22A \\sim F23A-F21A \\sim
F22A-F21A
 with sigma of 0.04
 F10A-F11A \\sim F10A-F12A \\sim F10-F11 \\sim F10-F12 \\sim F11-F12 \\sim
F11A-F12A
 with sigma of 0.04
 C39-F10A \\sim C39-F10 \\sim C39-F11 \\sim C39-F11A \\sim C39-F12 \\sim
C39-F12A
 with sigma of 0.02
 C55-F23 \\sim C55-F21 \\sim C55-F22 \\sim C55-F23A \\sim C55-F22A \\sim
C55-F21A
 with sigma of 0.02
 F2-F3 \\sim F2-F1 \\sim F2A-F3A \\sim F2A-F1A \\sim F3A-F1A \\sim F3-F1
 with sigma of 0.04
 C30-F2 \\sim C30-F2A \\sim C30-F3A \\sim C30-F3 \\sim C30-F1A \\sim C30-F1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39 \\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
C55 \\sim F21 \\sim F22 \\sim F23 \\sim F21A \\sim F22A \\sim F23A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C30 \\sim F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(C30) \\sim
Ueq, Uanis(F1A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2A) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C39, F10, F11, F12, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C55, F21, F22, F23, F21A, F22A, F23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, F1, F2, F3, F1A, F2A, F3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F21A)=Sof(F22A)=Sof(F23A)=1-FVAR(1)
 Sof(F21)=Sof(F22)=Sof(F23)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C56(H56A,H56B), C57(H57A,H57B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C25(H25), C27(H27), C29(H29), C33(H33), C35(H35), C37(H37), C41(H41), C43(H43),
  C45(H45), C49(H49), C51(H51), C53(H53)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              68391
_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 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.664