Iridium Complexes of Bulky CCC-Pincer N-Heterocyclic Carbene Ligands: Steric Control of Coordination Number and Catalytic Alkene Isomerization
Chianese, Anthony R.; Shaner, Sarah E.; Tendler, Jennifer A.; Pudalov, David M.; Shopov, Dimitar Y.; Kim, Daniel; Rogers, Scott L.; Mo, Allen; Organometallics 31 (2012) 7359–; doi:10.1021/om300468d

data_4079081
_publ_section_title
;
 Iridium Complexes of Bulky CCC-Pincer N-Heterocyclic Carbene Ligands:
 Steric Control of Coordination Number and Catalytic Alkene Isomerization
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7359
_journal_paper_doi               10.1021/om300468d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C40 H42 Cl1 Ir1 N4'
_chemical_formula_sum            'C40 H42 Cl Ir N4'
_chemical_formula_weight         806.47
_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
_audit_creation_date             12-02-25
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90.0
_cell_angle_beta                 97.3868(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00000
_cell_length_a                   14.0985(2)
_cell_length_b                   15.2590(2)
_cell_length_c                   15.0008(2)
_cell_measurement_reflns_used    19978
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.4774
_cell_measurement_theta_min      3.6230
_cell_volume                     3200.32(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.3533
_diffrn_detector_type            'Oxford Diffraction Ruby CCD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega   -6.00   20.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   69.0000  177.0000 26

  2 omega  -87.00   12.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208  -37.0000  -90.0000 99

  3 omega  -37.00   51.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   37.0000   90.0000 88

  4 omega  -65.00  -40.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000 -180.0000 25

  5 omega  -88.00   14.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208  -37.0000  120.0000 102

  6 omega  -44.00   64.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   69.0000 -105.0000 108

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0100424000
_diffrn_orient_matrix_UB_12      -0.0398552000
_diffrn_orient_matrix_UB_13      0.0212179000
_diffrn_orient_matrix_UB_21      0.0287682000
_diffrn_orient_matrix_UB_22      -0.0230666000
_diffrn_orient_matrix_UB_23      -0.0276243000
_diffrn_orient_matrix_UB_31      0.0405286000
_diffrn_orient_matrix_UB_32      0.0064324000
_diffrn_orient_matrix_UB_33      0.0325834000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38298
_diffrn_reflns_theta_full        26.588
_diffrn_reflns_theta_max         29.4774
_diffrn_reflns_theta_min         3.6230
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.1993
_exptl_crystal_size_mid          0.1124
_exptl_crystal_size_min          0.0967
_refine_diff_density_max         1.61
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0229
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.0028803
_refine_ls_shift/su_mean         0.0000414
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 6.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0569
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0569
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7325
_reflns_number_total             8180
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.17
_oxford_diffrn_Wilson_scale      4.28
_oxford_refine_ls_r_factor_ref   0.0357
_oxford_refine_ls_scale          0.5500(4)
_oxford_reflns_number_all        8180
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om300468d_si_002.cif
_cod_data_source_block           arc54b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_diffrn_radiation_probe' value 'X-ray' changed to
'x-ray' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3200.33(14)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C40 H42 Cl1 Ir1 N4'
_cod_database_code               4079081