Synthesis and Reactivity of New Bis(N-heterocyclic carbene) Iridium(I) Complexes
David J. Nelson; Byron J. Truscott; Alexandra M. Z. Slawin; Steven P. Nolan; Inorganic Chemistry 52 (2013) 12674–12681; doi:10.1021/ic4018773

data_4336599
_publ_section_title
;
 Synthesis and Reactivity of New Bis(N-heterocyclic carbene) Iridium(I)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12674
_journal_page_last               12681
_journal_paper_doi               10.1021/ic4018773
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C40.50 H68 Cl Ir N4'
_chemical_formula_sum            'C40.5 H68 Cl Ir N4'
_chemical_formula_weight         838.68
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.5268(18)
_cell_length_b                   26.589(5)
_cell_length_c                   15.428(2)
_cell_measurement_reflns_used    13406
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.47
_cell_volume                     4318.3(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25479
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.192
_exptl_absorpt_correction_T_max  0.528
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.020
_refine_diff_density_min         -3.720
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3300 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.476(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     443
_refine_ls_number_reflns         25479
_refine_ls_number_restraints     65
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0556P)^2^+9.7656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                20096
_reflns_number_total             25479
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic4018773_si_002_4.cif
_cod_data_source_block           8D
_cod_original_formula_sum        'C40.50 H68 Cl Ir N4'
_cod_database_code               4336599