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_7712135
_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 Cl2 N4 O2 P4 Rh2'
_chemical_formula_sum            'C76 H64 Cl2 N4 O2 P4 Rh2'
_chemical_formula_weight         1465.91
_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             2022-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                108.38(3)
_cell_angle_beta                 106.46(3)
_cell_angle_gamma                93.84(3)
_cell_formula_units_Z            1
_cell_length_a                   11.403(2)
_cell_length_b                   12.569(3)
_cell_length_c                   12.798(3)
_cell_measurement_reflns_used    305
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      19.1
_cell_measurement_theta_min      1.86
_cell_volume                     1644.5(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'SHELXLE (H\~A\#188;bschle, 2011)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_detector_type            'Dectris Eiger 16M'
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.740
_diffrn_measurement_device_type  'Australian Synchrotron'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.740
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30342
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.102
_diffrn_reflns_theta_min         1.733
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.4344
_exptl_absorpt_correction_T_min  0.2826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.6506.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0854P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6274
_reflns_number_total             8517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03984b4.cif
_cod_data_source_block           rh_sadabss
_cod_depositor_comments
'Adding full bibliography for 7712131--7712137.cif.'
_cod_original_cell_volume        1644.5(7)
_cod_database_code               7712135
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C32(H32), C28(H28), C31(H31), C10(H10), C17(H17), C38(H38),
 C26(H26), C11(H11), C22(H22), C29(H29), C34(H34), C23(H23), C35(H35), C16(H16),
  C8(H8), C36(H36), C20(H20), C7(H7), C6(H6), C25(H25), C24(H24), C37(H37),
 C30(H30), C18(H18), C19(H19)
;
_shelx_res_checksum              96067
_shelx_hkl_checksum              37466
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;