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_4331811
_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         'C28 H30 Ir N4, B F4'
_chemical_formula_sum            'C28 H30 B F4 Ir N4'
_chemical_formula_weight         701.57
_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             2012-04-05
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 20 2012 17:37:33, GUI svn.r4124)
;
_cell_angle_alpha                82.3830(10)
_cell_angle_beta                 84.2520(10)
_cell_angle_gamma                85.7140(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9633(2)
_cell_length_b                   11.9394(2)
_cell_length_c                   12.6935(2)
_cell_measurement_reflns_used    5962
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      3.74
_cell_volume                     1337.05(4)
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8056
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.6
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.121
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0811 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.6532.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.026
_refine_diff_density_max         2.153
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                3905
_reflns_number_total             4431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302589b_si_004_4.cif
_cod_data_source_block           x1204001
_cod_database_code               4331811