Stepwise synthesis of a hydrido, N-heterocyclic dicarbene iridium(III) pincer complex featuring mixed NHC/abnormal NHC ligands.
Zuo, Weiwei; Braunstein, Pierre; Dalton transactions (Cambridge, England : 2003) 41 (2012) 636–643; doi:10.1039/c1dt11511a

data_7017836
_publ_section_title
;
 Stepwise synthesis of a hydrido, N-heterocyclic dicarbene iridium(III)
 pincer complex featuring mixed NHC/abnormal NHC ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              636
_journal_page_last               643
_journal_paper_doi               10.1039/c1dt11511a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C50 H66 Cl0.25 I1.75 Ir2 N4'
_chemical_formula_sum            'C50 H66 Cl0.25 I1.75 Ir2 N4'
_chemical_formula_weight         1338.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.637(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3334(5)
_cell_length_b                   17.8209(8)
_cell_length_c                   19.0291(5)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     4657.2(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17895
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.922
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.636
_refine_diff_density_min         -2.783
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         10267
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                5824
_reflns_number_total             10267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11511a.txt
_cod_data_source_block           PBZW100412
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017836