Acceptorless Alkane Dehydrogenation Catalyzed by Iridium CCC-Pincer Complexes
Chianese, Anthony R.; Drance, Myles J.; Jensen, Kelsey H.; McCollom, Samuel P.; Yusufova, Nevin; Shaner, Sarah E.; Shopov, Dimitar Y.; Tendler, Jennifer A.; Organometallics 33 (2014) 457–; doi:10.1021/om4006577

data_4082320
_publ_section_title
;
 Acceptorless Alkane Dehydrogenation Catalyzed by Iridium CCC-Pincer
 Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              457
_journal_paper_doi               10.1021/om4006577
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C39 H35 Cl3 Ir1 N4'
_chemical_formula_sum            'C39 H35 Cl3 Ir N4'
_chemical_formula_weight         858.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-10
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                77.741(6)
_cell_angle_beta                 74.571(6)
_cell_angle_gamma                74.955(7)
_cell_formula_units_Z            2.00000
_cell_length_a                   9.6026(8)
_cell_length_b                   14.5545(11)
_cell_length_c                   15.2620(11)
_cell_measurement_reflns_used    10984
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      67.7293
_cell_measurement_theta_min      4.0464
_cell_volume                     1962.0(3)
_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      109.95(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.3533
_diffrn_detector_type            'Oxford Diffraction Ruby CCD'
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details
;
  1 omega    1.00   95.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958 -125.0000 -150.0000 47

  2 omega   -3.00   25.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958 -125.0000  -90.0000 14

  3 omega  -41.00   55.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958  -37.0000  -90.0000 48

  4 omega   13.00  105.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958   57.0000   60.0000 46

  5 omega -158.00 -112.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  179.0000    0.0000 23

  6 omega   20.00   46.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -91.0000   98.0000 13

  7 omega   94.00  120.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -93.0000   57.0000 13

  8 omega   19.00   63.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -92.0000 -167.0000 22

  9 omega   67.00  177.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000    0.0000  120.0000 55

 10 omega    5.00   57.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000    0.0000  120.0000 26

 11 omega   25.00   57.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000 -150.0000 16

 12 omega   20.00   46.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000 -111.0000 -180.0000 13

 13 omega   31.00   67.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000   90.0000 18

 14 omega   15.00   45.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000  -60.0000 15

 15 omega   25.00   51.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -93.0000   57.0000 13

 16 omega   18.00   82.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -94.0000   30.0000 32

 17 omega   18.00  130.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000   90.0000 56

 18 omega   26.00  126.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -91.0000 -110.0000 50

 19 omega   25.00   69.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000  150.0000 22

 20 omega   15.00   57.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -30.0000    0.0000 21

 21 omega   40.00   66.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000 -120.0000 13

 22 omega   81.00  127.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -61.0000 -120.0000 23

 23 omega   41.00   77.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -45.0000 -120.0000 18

 24 omega   55.00  109.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -91.0000   98.0000 27

 25 omega   70.00  108.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -92.0000 -167.0000 19

 26 omega   94.00  130.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -93.0000  -28.0000 18

 27 omega   64.00  114.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   61.0000   90.0000 25

 28 omega   21.00   47.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000  -93.0000  -28.0000 13

 29 omega    2.00  122.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958   77.0000  150.0000 60

 30 omega   -3.00   95.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958 -125.0000   90.0000 49

 31 omega    6.00  116.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958   57.0000  -90.0000 55

 32 omega    7.00  117.00   2.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       38.4958   37.0000   30.0000 55

 33 omega   60.00  178.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   77.0000   60.0000 59

 34 omega   63.00  175.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   61.0000  -30.0000 56

 35 omega   65.00  175.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   45.0000 -180.0000 55

 36 omega   60.00  178.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   77.0000  120.0000 59

 37 omega   59.00  177.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   30.0000  -90.0000 59

 38 omega   60.00  178.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   77.0000 -150.0000 59

 39 omega   60.00  178.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   77.0000  -90.0000 59

 40 omega   63.00  175.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   61.0000    0.0000 56

 41 omega   60.00  178.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   77.0000 -180.0000 59

 42 omega   63.00  175.00   2.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -       96.5000   61.0000   30.0000 56

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0331691000
_diffrn_orient_matrix_UB_12      -0.0852036000
_diffrn_orient_matrix_UB_13      -0.0300257000
_diffrn_orient_matrix_UB_21      -0.1667214000
_diffrn_orient_matrix_UB_22      0.0454492000
_diffrn_orient_matrix_UB_23      0.0228400000
_diffrn_orient_matrix_UB_31      0.0123719000
_diffrn_orient_matrix_UB_32      0.0545829000
_diffrn_orient_matrix_UB_33      -0.0990358000
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33792
_diffrn_reflns_theta_full        66.4915
_diffrn_reflns_theta_max         67.7293
_diffrn_reflns_theta_min         4.0464
_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    8.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82637
_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            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.0587
_exptl_crystal_size_mid          0.0550
_exptl_crystal_size_min          0.0226
_platon_squeeze_details
;
;
_refine_diff_density_max         1.46
_refine_diff_density_min         -1.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0197
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.0007079
_refine_ls_shift/su_mean         0.0000108
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ +14.02P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0949
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0949
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6258
_reflns_number_total             7017
_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   0.0415
_oxford_refine_ls_scale          2.011(8)
_oxford_reflns_number_all        7017
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om4006577_si_002.cif
_cod_data_source_block           arc62
_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        1962.0(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C39 H35 Cl3 Ir1 N4'
_cod_database_code               4082320
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;