C-H activation in bimetallic rhodium complexes to afford N-heterocyclic carbene pincer complexes.
Watson, Lachlan J.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2164–2174; doi:10.1039/d2dt03984b

data_7712132
_publ_section_title
;
 C-H activation in bimetallic rhodium complexes to afford N-heterocyclic
 carbene pincer complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2164
_journal_page_last               2174
_journal_paper_doi               10.1039/d2dt03984b
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C86 H82 N4 O2 P4 Rh2 Si2, 2(C6 H6)'
_chemical_formula_sum            'C98 H94 N4 O2 P4 Rh2 Si2'
_chemical_formula_weight         1745.65
_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             2022-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-25 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                64.079(4)
_cell_angle_beta                 66.091(4)
_cell_angle_gamma                74.274(4)
_cell_formula_units_Z            1
_cell_length_a                   12.7185(5)
_cell_length_b                   14.3038(6)
_cell_length_c                   14.4821(6)
_cell_measurement_reflns_used    6886
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3940
_cell_measurement_theta_min      3.9560
_cell_volume                     2152.08(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_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   -100.00 -20.00   1.00    5.00    --  -36.95 -57.00  30.00   80
  2  \w    -86.00 -20.00   1.00    5.00    --  -36.95 125.00  90.00   66
  3  \w     24.00 106.00   1.00    5.00    --   36.95  38.00   0.00   82
  4  \w     35.00 106.00   1.00    5.00    --   36.95  19.00-120.00   71
  5  \w     38.00  89.00   1.00    5.00    --   36.95-125.00  30.00   51
  6  \w    -30.00  47.00   1.00    5.00    --   36.95 -57.00-120.00   77
  7  \w     37.00  81.00   1.00    5.00    --   36.95-125.00-120.00   44
  8  \w     23.00  95.00   1.00    5.00    --   36.95  38.00 150.00   72
  9  \w     97.00 177.00   1.00   20.00    --  111.00  38.00-120.00   80
 10  \w     70.00 105.00   1.00   20.00    --  111.00-111.00 -90.00   35
 11  \w     65.00 128.00   1.00   20.00    --  111.00 -38.00 -90.00   63
 12  \w    109.00 154.00   1.00   20.00    --  111.00  77.00   0.00   45
 13  \w     42.00  70.00   1.00   20.00    --  111.00-111.00 120.00   28
 14  \w     84.00 109.00   1.00   20.00    --  111.00-111.00 120.00   25
 15  \w     93.00 178.00   1.00   20.00    --  111.00  64.00 -30.00   85
 16  \w    106.00 137.00   1.00   20.00    --  111.00  77.00 120.00   31
 17  \w     55.00  99.00   1.00   20.00    --  111.00 -92.00 150.00   44
 18  \w    111.00 178.00   1.00   20.00    --  111.00  77.00  90.00   67
 19  \w     43.00 109.00   1.00   20.00    --  111.00 -50.00-180.00   66
 20  \w     49.00 109.00   1.00   20.00    --  111.00-111.00-150.00   60
 21  \w     42.00 119.00   1.00   20.00    --  111.00 -38.00  60.00   77
 22  \w     48.00 109.00   1.00   20.00    --  111.00-111.00 -30.00   61
 23  \w     52.00 133.00   1.00   20.00    --  111.00 -77.00   0.00   81
 24  \w    140.00 175.00   1.00   20.00    --  111.00  64.00  60.00   35
 25  \w     57.00 108.00   1.00   20.00    --  111.00-111.00   0.00   51
 26  \w    119.00 158.00   1.00   20.00    --  111.00 111.00-180.00   39
 27  \w     97.00 127.00   1.00   20.00    --  111.00  64.00  60.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0546133000
_diffrn_orient_matrix_UB_12      -0.0600115000
_diffrn_orient_matrix_UB_13      0.1229228000
_diffrn_orient_matrix_UB_21      0.0369676000
_diffrn_orient_matrix_UB_22      0.0784284000
_diffrn_orient_matrix_UB_23      0.0244588000
_diffrn_orient_matrix_UB_31      -0.1159231000
_diffrn_orient_matrix_UB_32      0.0691169000
_diffrn_orient_matrix_UB_33      -0.0023330000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16125
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.694
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0290P)^2^+0.2104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             8522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03984b4.cif
_cod_data_source_block           ljw-rhtmsdimer_scale
_cod_depositor_comments
'Adding full bibliography for 7712131--7712137.cif.'
_cod_database_code               7712132
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P Si Rh'
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C39(H39), C27(H27), C16(H16), C43(H43), C31(H31), C15(H15),
 C14(H14), C37(H37), C35(H35), C10(H10), C25(H25), C22(H22), C30(H30), C28(H28),
  C12(H12), C42(H42), C29(H29), C11(H11), C40(H40), C41(H41), C23(H23),
 C33(H33), C36(H36), C24(H24), C34(H34), C45(H45), C49(H49), C46(H46), C44(H44),
  C48(H48), C47(H47)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              93664
_shelx_hkl_checksum              82496
_ins_header
;
TITL LJW-RhTMSdimer_scale in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  12.718500  14.303772  14.482125  64.0791  66.0910  74.2738
ZERR   20.00   0.000488   0.000635   0.000583   0.0042   0.0038   0.0036
LATT -1
SFAC C H N O Si P Rh
UNIT 20.00 20.00 20.00 20.00 20.00 20.00 20.00
TREF
HKLF 4
END
;
_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 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.874
_publcif_funding_html
;
;