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_4073088
_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         C28H30Br2IrN3
_chemical_formula_sum            'C28 H30 Br2 Ir N3'
_chemical_formula_weight         760.57
_chemical_melting_point          234
_chemical_name_common            MesNCNIrBr2
_chemical_name_systematic
; 
 1,3bismesitylcarbaldimino-2-phenyliridiumdibromide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.337(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3368(2)
_cell_length_b                   17.4467(5)
_cell_length_c                   18.0171(6)
_cell_measurement_reflns_used    22320
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2618.40(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20659
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    8.173
_exptl_absorpt_correction_T_max  0.2917
_exptl_absorpt_correction_T_min  0.2917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blesing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.773
_refine_diff_density_min         -3.041
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+9.5319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1439
_reflns_number_gt                4458
_reflns_number_total             5971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070059fsi20070228_104410.cif
_cod_data_source_block           C28H30Br2IrN3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measure' 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_sg_symbol_H-M      P21/n
_cod_database_code               4073088