Synthesis of New Iridium N-Heterocyclic Carbene Complexes and Facile Intramolecular Alkyl C−H Bond Activation Reactions of the Carbene Ligand
Hanasaka, Fumihiro; Tanabe, Yusuke; Fujita, Ken-ichi; Yamaguchi, Ryohei; Organometallics 25 (2006) 826–; doi:10.1021/om050723x

data_4074656
_publ_section_title
;
 Synthesis of New Iridium N-Heterocyclic Carbene Complexes and Facile
 Intramolecular Alkyl C&#x2212;H Bond Activation Reactions of the Carbene
 Ligand
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              826
_journal_paper_doi               10.1021/om050723x
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C21 H34 Cl Ir N2 '
_chemical_formula_sum            'C21 H34 Cl Ir N2'
_chemical_formula_weight         542.19
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.612(3)
_cell_length_b                   16.459(2)
_cell_length_c                   8.331(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.4
_cell_volume                     4334.6(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows version 1.06'
_computing_publication_material  'teXsan for Windows version 1.06'
_computing_structure_refinement  'teXsan for Windows version 1.06'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      291.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.02602
_diffrn_orient_matrix_UB_12      -0.00249
_diffrn_orient_matrix_UB_13      0.06807
_diffrn_orient_matrix_UB_21      -0.01781
_diffrn_orient_matrix_UB_22      0.00492
_diffrn_orient_matrix_UB_23      0.09872
_diffrn_orient_matrix_UB_31      -0.00252
_diffrn_orient_matrix_UB_32      -0.06051
_diffrn_orient_matrix_UB_33      0.00522
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5592
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        -0.62
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type
;
PSI scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2144.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.85
_refine_diff_density_min         -1.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.457
_refine_ls_goodness_of_fit_ref   1.460
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0350
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                3205
_reflns_number_total             5592
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            om050723xsi20051217_125838.cif
_cod_data_source_block           '_Complex_2_____'
_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        4335(1)
_cod_original_sg_symbol_H-M      'P b c a    '
_cod_original_formula_sum        'C21 H34 Cl Ir N2 '
_cod_database_code               4074656