Mechanistic Studies of Alkene Isomerization Catalyzed by CCC-Pincer Complexes of Iridium
Knapp, Spring Melody M.; Shaner, Sarah E.; Kim, Daniel; Shopov, Dimitar Y.; Tendler, Jennifer A.; Pudalov, David M.; Chianese, Anthony R.; Organometallics 33 (2014) 473–; doi:10.1021/om400786r

data_4082345
_publ_section_title
;
 Mechanistic Studies of Alkene Isomerization Catalyzed by CCC-Pincer
 Complexes of Iridium
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              473
_journal_paper_doi               10.1021/om400786r
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C47 H42 Ir1 N4'
_chemical_formula_sum            'C47 H42 Ir N4'
_chemical_formula_weight         855.10
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-12
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90.0
_cell_angle_beta                 108.9352(14)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00000
_cell_length_a                   15.04543(17)
_cell_length_b                   15.41690(17)
_cell_length_c                   21.5872(3)
_cell_measurement_reflns_used    21024
_cell_measurement_temperature    109.90(14)
_cell_measurement_theta_max      67.4809
_cell_measurement_theta_min      4.2243
_cell_volume                     4736.27(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      109.90(14)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.3533
_diffrn_detector_type            'Oxford Diffraction Ruby CCD'
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9943
_diffrn_measurement_details
;
  1 omega   16.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.6208   57.0000  150.0000 101

  2 omega   17.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.6208  -46.0000   16.0000 30

  3 omega  -40.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.6208  -37.0000 -150.0000 99

  4 omega  100.00  169.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   30.0000   60.0000 69

  5 omega   28.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -45.0000   30.0000 44

  6 omega   29.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000   60.0000 40

  7 omega   26.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000    0.0000 99

  8 omega  106.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   30.0000   90.0000 71

  9 omega   36.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000  150.0000 26

 10 omega   24.00   56.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -45.0000 -150.0000 32

 11 omega   58.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000  -60.0000 30

 12 omega   27.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -45.0000  150.0000 50

 13 omega   69.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   45.0000  -30.0000 98

 14 omega   20.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000   30.0000 26

 15 omega   91.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000   30.0000 26

 16 omega   25.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000 -150.0000 43

 17 omega  -71.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.6208   57.0000   30.0000 110

 18 omega    6.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.6208   57.0000   30.0000 111

 19 omega    6.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       38.6208   57.0000  -90.0000 111

 20 omega   65.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   45.0000  -90.0000 110

 21 omega   18.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -45.0000  -90.0000 59

 22 omega   18.00  130.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000  150.0000 112

 23 omega   63.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   61.0000    0.0000 60

 24 omega   65.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   45.0000 -180.0000 110

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1077685000
_diffrn_orient_matrix_UB_12      0.0017482000
_diffrn_orient_matrix_UB_13      0.0177421000
_diffrn_orient_matrix_UB_21      -0.0092844000
_diffrn_orient_matrix_UB_22      0.0576286000
_diffrn_orient_matrix_UB_23      -0.0600978000
_diffrn_orient_matrix_UB_31      0.0043699000
_diffrn_orient_matrix_UB_32      0.0816359000
_diffrn_orient_matrix_UB_33      0.0420149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44223
_diffrn_reflns_theta_full        66.4915
_diffrn_reflns_theta_max         67.4809
_diffrn_reflns_theta_min         4.2243
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_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    5.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.2434
_exptl_crystal_size_mid          0.1532
_exptl_crystal_size_min          0.1530
_platon_squeeze_details
;
;
_refine_diff_density_max         4.98
_refine_diff_density_min         -1.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0011519
_refine_ls_shift/su_mean         0.0000188
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 9.30P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1223
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1223
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7764
_reflns_number_total             8483
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0467
_oxford_refine_ls_scale          1.739(9)
_oxford_reflns_number_all        8483
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om400786r_si_002.cif
_cod_data_source_block           arc71
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4736.28(10)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C47 H42 Ir1 N4'
_cod_database_code               4082345
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;