Iridium Complexes of the Doubly Cyclometalated NHC Ligand IMes''
Janeth Navarro; Olga Torres; Marta Martín; Eduardo Sola; Journal of the American Chemical Society 133 (2011) 9738–9740; doi:10.1021/ja204522e

data_4106334
_publ_contact_author_address
;
  Dr. Marta Mart\'in
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       martam@unizar.es
_publ_contact_author_fax         '+34 956 761187'
_publ_contact_author_name        'Dr. Marta Mart\'in'
_publ_contact_author_phone       '+34 976 762026'
_publ_section_title
;
 Iridium Complexes of the Doubly Cyclometalated NHC Ligand IMes''
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9738
_journal_page_last               9740
_journal_paper_doi               10.1021/ja204522e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C45 H42 B Ir N2, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C46.5 H45 B Cl3 Ir N2'
_chemical_formula_weight         941.21
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.968(6)
_cell_angle_beta                 87.718(6)
_cell_angle_gamma                74.061(6)
_cell_formula_units_Z            2
_cell_length_a                   11.062(4)
_cell_length_b                   13.329(5)
_cell_length_c                   13.883(5)
_cell_measurement_reflns_used    3380
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      21.87
_cell_measurement_theta_min      2.37
_cell_volume                     1966.6(12)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.1270
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23684
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.635
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.455
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                7136
_reflns_number_total             9419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204522e_si_002_1.cif
_cod_data_source_block           mar170as
_cod_original_cell_volume        1966.7(11)
_cod_original_formula_sum        'C46.50 H45 B Cl3 Ir N2'
_cod_database_code               4106334