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_7712137
_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         'C42 H31 N2 P2 Rh Si, 1.5(C6 H6)'
_chemical_formula_sum            'C51 H40 N2 P2 Rh Si'
_chemical_formula_weight         873.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-18
_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                90
_cell_angle_beta                 95.3060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.59280(10)
_cell_length_b                   22.3888(2)
_cell_length_c                   20.17120(10)
_cell_measurement_reflns_used    23686
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.8270
_cell_measurement_theta_min      4.3730
_cell_volume                     4313.63(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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 (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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      8.00  42.00   1.00    5.00    --   36.95  81.00 167.95   34
  2  \w     11.00  42.00   1.00    5.00    --   36.95  76.00 100.80   31
  3  \w      7.00  42.00   1.00    5.00    --   36.95  82.00  46.68   35
  4  \w     27.00  90.00   1.00    5.00    --   36.95-125.00 -90.00   63
  5  \w    -32.00  56.00   1.00    5.00    --   36.95 -38.00  90.00   88
  6  \w     20.00 104.00   1.00    5.00    --   36.95  57.00 -30.00   84
  7  \w      6.00  76.00   1.00    5.00    --   36.95 -99.00   0.00   70
  8  \w     27.00  90.00   1.00    5.00    --   36.95-125.00 120.00   63
  9  \w      9.00  42.00   1.00    5.00    --   36.95  80.00-157.95   33
 10  \w    -30.00  54.00   1.00    5.00    --   36.95 -57.00  90.00   84
 11  \w    103.00 178.00   1.00   20.00    --  111.00  77.00 -60.00   75
 12  \w     42.00 130.00   1.00   20.00    --  111.00 -38.00-180.00   88
 13  \w     41.00 109.00   1.00   20.00    --  111.00-111.00 120.00   68
 14  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00-120.00   64
 15  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00 -30.00   64
 16  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00 150.00   64
 17  \w     94.00 178.00   1.00   20.00    --  111.00  50.00   0.00   84
 18  \w    103.00 178.00   1.00   20.00    --  111.00  77.00-150.00   75
 19  \w     43.00 128.00   1.00   20.00    --  111.00 -50.00 -90.00   85
 20  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00-180.00   64
 21  \w     41.00 109.00   1.00   20.00    --  111.00-111.00-150.00   68
 22  \w     42.00 106.00   1.00   20.00    --  111.00 -92.00 -90.00   64
 23  \w     94.00 178.00   1.00   20.00    --  111.00  50.00  60.00   84
 24  \w     86.00 178.00   1.00   20.00    --  111.00  25.00  90.00   92
 25  \w     41.00 109.00   1.00   20.00    --  111.00-111.00 150.00   68
 26  \w     46.00 116.00   1.00   20.00    --  111.00 -50.00   0.00   70
 27  \w    150.00 178.00   1.00   20.00    --  111.00  25.00 120.00   28
 28  \w    121.00 169.00   1.00   20.00    --  111.00  64.00  90.00   48
 29  \w    138.00 163.00   1.00   20.00    --  111.00  50.00  30.00   25
 30  \w    126.00 155.00   1.00   20.00    --  111.00  42.00-130.70   29
 31  \w     82.00 115.00   1.00   20.00    --  111.00 -50.00 150.00   33
 32  \w     80.00 131.00   1.00   20.00    --  111.00 -25.00 150.00   51
 33  \w     95.00 135.00   1.00   20.00    --  111.00  50.00  30.00   40
 34  \w    115.00 171.00   1.00   20.00    --  111.00  77.00 -90.00   56
 35  \w    103.00 128.00   1.00   20.00    --  111.00  38.00  90.00   25
 36  \w     71.00 101.00   1.00   20.00    --  111.00 -77.00  90.00   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      0.0227616000
_diffrn_orient_matrix_UB_12      0.0381263000
_diffrn_orient_matrix_UB_13      -0.0616715000
_diffrn_orient_matrix_UB_21      -0.1077430000
_diffrn_orient_matrix_UB_22      0.0457436000
_diffrn_orient_matrix_UB_23      0.0208348000
_diffrn_orient_matrix_UB_31      0.1177465000
_diffrn_orient_matrix_UB_32      0.0344769000
_diffrn_orient_matrix_UB_33      0.0406222000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44676
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.980
_diffrn_reflns_theta_min         3.949
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.450
_exptl_absorpt_correction_T_max  0.70019
_exptl_absorpt_correction_T_min  0.68041
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.049
_exptl_crystal_size_rad          0.047
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0577P)^2^+3.0738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7986
_reflns_number_total             8691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03984b4.cif
_cod_data_source_block           ljw-361-a_scale
_cod_depositor_comments
'Adding full bibliography for 7712131--7712137.cif.'
_cod_database_code               7712137
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H41 N2 P2 Si Rh'
_chemical_oxdiff_usercomment     'benzene standing'
_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. Others
 Fixed Sof: C18A(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C17A(0.5) H17A(0.5)
 H17B(0.5) H17C(0.5) C17B(0.5) H17D(0.5) H17E(0.5) H17F(0.5) C18B(0.5)
 H18D(0.5) H18E(0.5) H18F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C33(H33), C11(H11), C8(H8), C12(H12), C9(H9), C34(H34),
 C42(H42), C20(H20), C38(H38), C39(H39), C41(H41), C40(H40), C35(H35), C36(H36),
  C22(H22), C24(H24), C21(H21), C44(H44), C23(H23), C43(H43), C45(H45),
 C48(H48), C46(H46), C47(H47), C49(H49), C51(H51), C50(H50)
3.c Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C17A(H17A,H17B,H17C), C16(H16A,H16B,H16C), C17B(H17D,
 H17E,H17F), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              87525
_shelx_hkl_checksum              46322
_ins_header
;
TITL LJW-361-a_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   9.592846  22.388752  20.171152  90.0000  95.3064  90.0000
ZERR    5.00   0.000061   0.000150   0.000146   0.0000   0.0006   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N Si P Rh
UNIT 230.00 205.00 10.00 5.00 10.00 5.00
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 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.834
_publcif_funding_html
;
;