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_7046852
_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            'C53 H60 Br6 Cl10 F2 Ir2 N8 O3'
_chemical_formula_weight         2113.45
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 91.462(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5068(16)
_cell_length_b                   14.4057(13)
_cell_length_c                   27.924(3)
_cell_measurement_reflns_used    8104
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      2.29
_cell_volume                     7442.2(12)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52245
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.197
_diffrn_reflns_theta_min         1.924
_exptl_absorpt_coefficient_mu    7.201
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         16423
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9606
_reflns_number_total             16423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02212g2.cif
_cod_data_source_block           11Br2
_cod_depositor_comments
'Adding full bibliography for 7046846--7046852.cif.'
_cod_original_cell_volume        7442.3(11)
_cod_database_code               7046852
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.455
_shelx_estimated_absorpt_t_max   0.505
_shelx_res_checksum              36130
_shelx_fab_checksum              34870