Synthesis of Bis(imino)aryl Iridium Pincer Complexes and Demonstration of Catalytic Hydrogen-Transfer Activity
Oakley, Sarah H.; Coogan, Michael P.; Arthur, Richard J.; Organometallics 26 (2007) 2285–; doi:10.1021/om070059f

data_4073087
_publ_section_title
;
 Synthesis of Bis(imino)aryl Iridium Pincer Complexes and Demonstration of
 Catalytic Hydrogen-Transfer Activity
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2285
_journal_paper_doi               10.1021/om070059f
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         PhNCNPhIrBr2
_chemical_formula_sum            'C22 H18 Br2 Ir N3'
_chemical_formula_weight         676.41
_chemical_melting_point          200+
_chemical_name_common            PhNCNPhIrBr2
_chemical_name_systematic
; 
 1,3bisphenylcarbaldimino-2-phenyliridiumdibromide 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.434(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.5949(9)
_cell_length_b                   10.5989(5)
_cell_length_c                   16.8333(9)
_cell_measurement_reflns_used    10245
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4408.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12327
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    9.694
_exptl_absorpt_correction_T_max  0.2190
_exptl_absorpt_correction_T_min  0.2190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blesing, 1995)'
_exptl_crystal_colour            claret
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2862
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.693
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                3245
_reflns_number_total             5026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070059fsi20070119_100155.cif
_cod_data_source_block           C22H18Br2IrN3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4408.6(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4073087