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_4079082
_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         'C47 H51 Cl3 Ir1 N5'
_chemical_formula_sum            'C47 H51 Cl3 Ir N5'
_chemical_formula_weight         984.53
_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             11-07-01
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90.0
_cell_angle_beta                 113.0013(18)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00000
_cell_length_a                   14.9067(2)
_cell_length_b                   19.6272(2)
_cell_length_c                   16.3925(2)
_cell_measurement_reflns_used    25468
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.3484
_cell_measurement_theta_min      3.6952
_cell_volume                     4414.76(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
  1 omega  -15.00   74.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   37.0000  -30.0000 89

  2 omega   -8.00   20.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000  -60.0000 28

  3 omega  -65.00   28.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000  150.0000 93

  4 omega  -65.00   28.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000    0.0000 93

  5 omega  -15.00   87.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   37.0000  150.0000 102

  6 omega  -38.00    3.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   37.0000  -90.0000 41

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0015663000
_diffrn_orient_matrix_UB_12      -0.0071191000
_diffrn_orient_matrix_UB_13      0.0418338000
_diffrn_orient_matrix_UB_21      0.0231939000
_diffrn_orient_matrix_UB_22      0.0315718000
_diffrn_orient_matrix_UB_23      0.0164269000
_diffrn_orient_matrix_UB_31      -0.0461840000
_diffrn_orient_matrix_UB_32      0.0160842000
_diffrn_orient_matrix_UB_33      -0.0137258000
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51560
_diffrn_reflns_theta_full        26.472
_diffrn_reflns_theta_max         29.3484
_diffrn_reflns_theta_min         3.6952
_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    3.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.2178
_exptl_crystal_size_mid          0.0719
_exptl_crystal_size_min          0.0579
_refine_diff_density_max         2.08
_refine_diff_density_min         -1.81
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9670
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.0028863
_refine_ls_shift/su_mean         0.0000354
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 131. 121. 66.3 22.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0563
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0563
_reflns_limit_h_max              18
_reflns_limit_h_min              -20
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                9879
_reflns_number_total             10888
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.01
_oxford_diffrn_Wilson_scale      3.46
_oxford_refine_ls_r_factor_ref   0.0499
_oxford_refine_ls_scale          0.5577(3)
_oxford_reflns_number_all        10888
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om300468d_si_002.cif
_cod_data_source_block           arc54e
_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        4414.76(13)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C47 H51 Cl3 Ir1 N5'
_cod_database_code               4079082