Steric Effects on Acetate-Assisted Cyclometallation of meta-substituted N-phenyl and N-benzyl imidazolium salts at [MCl2Cp*]2 (M = Ir, Rh).
Davies, David L.; Singh, Kuldip; Tamosiunaite, Neringa; Dalton Transactions  (2021) –; doi:10.1039/D1DT02677A

data_7708157
_publ_section_title
;
 Steric Effects on Acetate-Assisted Cyclometallation of meta-substituted
 N-phenyl and N-benzyl imidazolium salts at [MCl2Cp*]2 (M = Ir, Rh).
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02677A
_journal_year                    2021
_chemical_formula_moiety         'C22 H29 Cl2 Ir N2 O'
_chemical_formula_sum            'C22 H29 Cl2 Ir N2 O'
_chemical_formula_weight         600.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-24 deposited with the CCDC.	2021-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.248(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.369(6)
_cell_length_b                   8.613(5)
_cell_length_c                   12.615(7)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.005
_cell_measurement_theta_min      2.964
_cell_volume                     1117.3(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8857
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.981
_exptl_absorpt_coefficient_mu    6.229
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absoprtion correction based on 7497 reflections(SADABS);Rint 0.1553 before
correction and 0.0683 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.707
_refine_diff_density_min         -1.876
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.035(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4624
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0518P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                4390
_reflns_number_total             4624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02677a2.cif
_cod_data_source_block           18022
_cod_original_cell_volume        1117.2(11)
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7708157
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              89044
_shelx_hkl_checksum              1899