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_7712136
_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         'C76 H64 N4 O2 P4 Rh2, 2(C4 H10 O)'
_chemical_formula_sum            'C84 H84 N4 O4 P4 Rh2'
_chemical_formula_weight         1543.25
_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             2022-11-25
_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                 115.376(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9934(4)
_cell_length_b                   12.76730(10)
_cell_length_c                   23.3601(4)
_cell_measurement_reflns_used    11117
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7820
_cell_measurement_theta_min      4.0330
_cell_volume                     7273.9(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 32.5190
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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     38.00  68.00   1.00    1.00    --   36.98 -99.00 150.00   30
  2  \w    -13.00  46.00   1.00    1.00    --   36.98 -38.00  90.00   59
  3  \w     27.00  98.00   1.00    1.00    --   36.98  57.00-120.00   71
  4  \w     62.00 108.00   1.00    1.00    --   36.98  19.00  60.00   46
  5  \w    -32.00  54.00   1.00    1.00    --   36.98 -38.00 -60.00   86
  6  \w     28.00  89.00   1.00    1.00    --   36.98-125.00  90.00   61
  7  \w    124.00 150.00   1.00    1.00    --  111.00 111.00 150.00   26
  8  \w    107.00 174.00   1.00    1.00    --  111.00  77.00-180.00   67
  9  \w     91.00 117.00   1.00    1.00    --  111.00 -12.00   0.00   26
 10  \w    152.00 177.00   1.00    1.00    --  111.00  38.00   0.00   25
 11  \w     44.00 128.00   1.00    1.00    --  111.00 -64.00-120.00   84
 12  \w     58.00 106.00   1.00    1.00    --  111.00 -92.00  90.00   48
 13  \w     94.00 120.00   1.00    1.00    --  111.00 -77.00-150.00   26
 14  \w     97.00 130.00   1.00    1.00    --  111.00 -64.00  90.00   33
 15  \w     54.00 103.00   1.00    1.00    --  111.00 -50.00  60.00   49
 16  \w    103.00 129.00   1.00    1.00    --  111.00 -64.00  60.00   26
 17  \w    139.00 177.00   1.00    1.00    --  111.00  12.00 -30.00   38
 18  \w     82.00 124.00   1.00    1.00    --  111.00  12.00 -30.00   42
 19  \w     84.00 111.00   1.00    1.00    --  111.00 -38.00-180.00   27
 20  \w     92.00 133.00   1.00    1.00    --  111.00  38.00   0.00   41
 21  \w     43.00  96.00   1.00    1.00    --  111.00 -92.00-120.00   53
 22  \w     50.00  75.00   1.00    1.00    --  111.00 -38.00-180.00   25
 23  \w     75.00 135.00   1.00    1.00    --  111.00 -25.00   0.00   60
 24  \w     42.00  85.00   1.00    1.00    --  111.00 -38.00  90.00   43
 25  \w     90.00 115.00   1.00    1.00    --  111.00 -38.00  90.00   25
 26  \w     65.00  91.00   1.00    1.00    --  111.00 -77.00-150.00   26
 27  \w     54.00  81.00   1.00    1.00    --  111.00 -64.00  60.00   27
 28  \w     48.00  74.00   1.00    1.00    --  111.00-111.00  90.00   26
 29  \w     46.00  79.00   1.00    1.00    --  111.00 -12.00   0.00   33
;
_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      -0.0474452000
_diffrn_orient_matrix_UB_12      0.0635205000
_diffrn_orient_matrix_UB_13      0.0028277000
_diffrn_orient_matrix_UB_21      -0.0054811000
_diffrn_orient_matrix_UB_22      -0.0817587000
_diffrn_orient_matrix_UB_23      0.0454393000
_diffrn_orient_matrix_UB_31      0.0413578000
_diffrn_orient_matrix_UB_32      0.0620465000
_diffrn_orient_matrix_UB_33      0.0569928000
_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  0.0207
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21222
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.922
_diffrn_reflns_theta_min         3.908
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.929
_exptl_absorpt_correction_T_max  0.68814
_exptl_absorpt_correction_T_min  0.66705
_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            red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       sphere
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.642
_exptl_crystal_size_mid          0.463
_exptl_crystal_size_min          0.286
_exptl_crystal_size_rad          0.226
_refine_diff_density_max         0.419
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+9.3788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             7280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03984b4.cif
_cod_data_source_block           ljw-kc8-2_scale
_cod_depositor_comments
'Adding full bibliography for 7712131--7712137.cif.'
_cod_database_code               7712136
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H60 P4 O2 Rh2'
_chemical_oxdiff_usercomment     'benz/et2o liquid r.t.'
_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:
 C14(H14A,H14B), C2(H2A,H2B), C13(H13A,H13B), C39(H39A,H39B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C00D(H00D), C10(H10), C4(H4), C19(H19), C6(H6), C31(H31), C30(H30),
 C28(H28), C26(H26), C9(H9), C8(H8), C00W(H00W), C34(H34), C5(H5), C35(H35),
 C36(H36), C29(H29), C33(H33), C16(H16), C24(H24), C18(H18), C22(H22), C25(H25),
  C17(H17), C23(H23)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              60652
_shelx_hkl_checksum              57544
_ins_header
;
TITL LJW-KC8-2_scale in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  26.993371  12.767316  23.360090  90.0000 115.3755  90.0000
ZERR    6.00   0.000398   0.000139   0.000378   0.0000   0.0019   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H O P Rh
UNIT 360.00 360.00 12.00 24.00 12.00
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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.785
_publcif_funding_html
;
;