Synthesis, Structure, and Reactivity of Iridium(III) Complexes Containing a 4,6-Dimethyl-1,3-benzenediphenylimine Pincer Ligand
Leah A. Wingard; Mathew C. Finniss; Michael Norris; Peter S. White; Maurice Brookhart; Joseph L. Templeton; Inorganic Chemistry 52 (2013) 515–526; doi:10.1021/ic302589b

data_4331809
_publ_contact_author_name
;
;
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Iridium(III) Complexes Containing
 a 4,6-Dimethyl-1,3-benzenediphenylimine Pincer Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              515
_journal_page_last               526
_journal_paper_doi               10.1021/ic302589b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C26 H27 Ir N2 O2'
_chemical_formula_sum            'C26 H27 Ir N2 O2'
_chemical_formula_weight         591.70
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-29
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Dec 16 2011 16:06:37, GUI svn.r3983)
;
_cell_angle_alpha                73.8230(10)
_cell_angle_beta                 83.5340(10)
_cell_angle_gamma                62.6830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3583(2)
_cell_length_b                   10.4763(2)
_cell_length_c                   12.0455(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.01
_cell_measurement_theta_min      3.82
_cell_volume                     1115.21(4)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12793
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.57
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.784
_exptl_absorpt_correction_T_max  0.4225
_exptl_absorpt_correction_T_min  0.1657
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0652 before and 0.0375 after correction.
The Ratio of minimum to maximum transmission is 0.3922.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.6671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                3730
_reflns_number_total             3770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302589b_si_004_3.cif
_cod_data_source_block           x1112012
_cod_database_code               4331809