Preparation of polynuclear NHC complexes by post-synthetic modification of half-sandwich rhodium and iridium complexes bearing C-azolato ligands.
Aznarez, Francisco; Gao, Wen-Xi; Lin, Yue-Jian; Hahn, F. Ekkehardt; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9442–9452; doi:10.1039/c8dt02212g

data_7046850
_publ_section_title
;
 Preparation of polynuclear NHC complexes by post-synthetic modification
 of half-sandwich rhodium and iridium complexes bearing C-azolato ligands.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9442
_journal_page_last               9452
_journal_paper_doi               10.1039/c8dt02212g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C29 H33 Br3 Cl6 F N4 O Rh'
_chemical_formula_weight         1027.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-20 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                72.454(2)
_cell_angle_beta                 86.588(2)
_cell_angle_gamma                60.740(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8662(13)
_cell_length_b                   11.9461(13)
_cell_length_c                   15.5287(17)
_cell_measurement_reflns_used    6818
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.29
_cell_volume                     1820.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12432
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.030
_exptl_absorpt_coefficient_mu    4.237
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       stick
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_refine_diff_density_max         3.013
_refine_diff_density_min         -3.775
_refine_diff_density_rms         0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0763
_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^)+(0.2000P)^2^+3.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.2958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6308
_reflns_number_total             7740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02212g2.cif
_cod_data_source_block           5Br
_cod_depositor_comments
'Adding full bibliography for 7046846--7046852.cif.'
_cod_database_code               7046850
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.282
_shelx_estimated_absorpt_t_max   0.516
_shelx_res_checksum              15508