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_7712131
_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         'C45 H35 N2 P2 Rh, C6 H6'
_chemical_formula_sum            'C51 H41 N2 P2 Rh'
_chemical_formula_weight         846.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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
;
2022-11-24 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.81730(10)
_cell_length_b                   25.6987(3)
_cell_length_c                   16.1102(2)
_cell_measurement_reflns_used    18307
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5450
_cell_measurement_theta_min      4.8480
_cell_volume                     4033.99(8)
_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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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   -103.00 -77.00   1.00    1.00    --  -36.95 -38.00  60.00   26
  2  \w    -44.00 -18.00   1.00    1.00    --  -36.95 -38.00  60.00   26
  3  \w      9.00  76.00   1.00    1.00    --   36.95 -99.00-150.00   67
  4  \w     65.00  90.00   1.00    1.00    --   36.95-125.00-180.00   25
  5  \w     20.00 104.00   1.00    1.00    --   36.95  38.00  30.00   84
  6  \w     35.00  99.00   1.00    1.00    --   36.95  57.00 -60.00   64
  7  \w     39.00  64.00   1.00    1.00    --   36.95 -77.00 150.00   25
  8  \w     39.00  86.00   1.00    1.00    --   36.95-125.00  90.00   47
  9  \w     51.00  76.00   1.00    1.00    --   36.95 -99.00  60.00   25
 10  \w     10.00  36.00   1.00    1.00    --   36.95 -99.00  60.00   26
 11  \w    -15.00  23.00   1.00    1.00    --   36.95 -77.00 150.00   38
 12  \w    101.00 144.00   1.00    2.50    --  111.00 178.00 120.00   43
 13  \w     66.00  94.00   1.00    2.50    --  111.00 178.00 120.00   28
 14  \w     41.00 135.00   1.00    2.50    --  111.00 -25.00   0.00   94
 15  \w    115.00 141.00   1.00    2.50    --  111.00 111.00 -90.00   26
 16  \w     43.00 105.00   1.00    2.50    --  111.00 -50.00   0.00   62
 17  \w    105.00 162.00   1.00    2.50    --  111.00  77.00   0.00   57
 18  \w     61.00  87.00   1.00    2.50    --  111.00 -92.00 120.00   26
 19  \w     72.00 172.00   1.00    2.50    --  111.00  12.00   0.00  100
 20  \w    119.00 149.00   1.00    2.50    --  111.00 -12.00 -60.00   30
 21  \w    118.00 157.00   1.00    2.50    --  111.00  25.00  60.00   39
 22  \w     54.00  81.00   1.00    2.50    --  111.00 -50.00-120.00   27
 23  \w     54.00  80.00   1.00    2.50    --  111.00 -12.00 -60.00   26
 24  \w     46.00  81.00   1.00    2.50    --  111.00 -92.00  30.00   35
 25  \w    150.00 178.00   1.00    2.50    --  111.00  38.00  30.00   28
 26  \w    152.00 177.00   1.00    2.50    --  111.00 111.00 -90.00   25
 27  \w     99.00 124.00   1.00    2.50    --  111.00  38.00  30.00   25
 28  \w     92.00 125.00   1.00    2.50    --  111.00 -38.00-150.00   33
 29  \w     56.00  82.00   1.00    2.50    --  111.00 -92.00 -60.00   26
 30  \w     64.00 100.00   1.00    2.50    --  111.00 -92.00  60.00   36
 31  \w     45.00  70.00   1.00    2.50    --  111.00 -12.00 120.00   25
 32  \w     75.00 100.00   1.00    2.50    --  111.00 -56.00-164.00   25
 33  \w    119.00 145.00   1.00    2.50    --  111.00 178.00-120.00   26
 34  \w     43.00  79.00   1.00    2.50    --  111.00 -38.00-150.00   36
 35  \w    118.00 143.00   1.00    2.50    --  111.00 -12.00 120.00   25
 36  \w     81.00 106.00   1.00    2.50    --  111.00-111.00   0.00   25
 37  \w    149.00 174.00   1.00    2.50    --  111.00 111.00  90.00   25
 38  \w     85.00 127.00   1.00    2.50    --  111.00 178.00 -30.00   42
 39  \w     44.00 104.00   1.00    2.50    --  111.00 -92.00-150.00   60
 40  \w    102.00 140.00   1.00    2.50    --  111.00  38.00 -60.00   38
;
_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      -0.1031547000
_diffrn_orient_matrix_UB_12      0.0028005000
_diffrn_orient_matrix_UB_13      0.0646718000
_diffrn_orient_matrix_UB_21      0.0916280000
_diffrn_orient_matrix_UB_22      0.0404136000
_diffrn_orient_matrix_UB_23      0.0505221000
_diffrn_orient_matrix_UB_31      -0.0772678000
_diffrn_orient_matrix_UB_32      0.0441700000
_diffrn_orient_matrix_UB_33      -0.0504845000
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29666
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0536P)^2^+6.1365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7547
_reflns_number_total             7932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03984b4.cif
_cod_data_source_block           ljw-378_scale
_cod_depositor_comments
'Adding full bibliography for 7712131--7712137.cif.'
_cod_database_code               7712131
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H41 N2 P2 Rh'
_chemical_oxdiff_usercomment     benzene/pent
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C49) = Uanis(C48) = Uanis(C47) = Uanis(C46) = Uanis(C51) = Uanis(C50)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C41(H41), C19(H19), C18(H18), C23(H23), C27(H27), C14(H14),
 C15(H15), C24(H24), C11(H11), C29(H29), C39(H39), C9(H9), C37(H37), C33(H33),
 C7(H7), C17(H17), C25(H25), C38(H38), C45(H45), C42(H42), C10(H10), C26(H26),
 C35(H35), C43(H43), C44(H44), C36(H36), C8(H8), C32(H32), C30(H30), C31(H31),
 C48(H48), C51(H51), C47(H47), C46(H46), C49(H49), C50(H50)
;
_shelx_res_checksum              84958
_shelx_hkl_checksum              92958
_ins_header
;
TITL LJW-378_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.817271  25.698731  16.110162  90.0000  97.0220  90.0000
ZERR    4.00   0.000100   0.000260   0.000174   0.0000   0.0010   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N P Rh
UNIT 200.00 164.00 8.00 8.00 4.00
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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.678
_publcif_funding_html
;
;