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_4082319
_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         'C41 H35 Cl1 F3 Ir1 N5'
_chemical_formula_sum            'C41 H35 Cl F3 Ir N5'
_chemical_formula_weight         882.43
_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             13-05-23
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                72.1088(14)
_cell_angle_beta                 67.2559(15)
_cell_angle_gamma                89.7454(15)
_cell_formula_units_Z            2.00000
_cell_length_a                   12.6114(2)
_cell_length_b                   13.0423(2)
_cell_length_c                   15.2552(2)
_cell_measurement_reflns_used    28003
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      29.4209
_cell_measurement_theta_min      3.6878
_cell_volume                     2183.42(7)
_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      110.00(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.3533
_diffrn_detector_type            'Oxford Diffraction Ruby CCD'
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9698
_diffrn_measurement_details
;
  1 omega   -7.00   70.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000  -60.0000 77

  2 omega  -18.00   80.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000 -180.0000 98

  3 omega   10.00   48.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176   57.0000    0.0000 38

  4 omega  -59.00   30.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -57.0000   30.0000 89

  5 omega  -63.00   41.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -57.0000 -180.0000 104

  6 omega  -65.00   37.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2176  -37.0000 -120.0000 102

  7 omega  -42.00   62.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   57.0000   30.0000 104

  8 omega  -88.00   14.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208  -37.0000  -30.0000 102

  9 omega  -42.00  -17.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   57.0000  -30.0000 25

 10 omega  -42.00   62.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9208   57.0000  150.0000 104

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0463534000
_diffrn_orient_matrix_UB_12      -0.0283753000
_diffrn_orient_matrix_UB_13      -0.0020735000
_diffrn_orient_matrix_UB_21      0.0325402000
_diffrn_orient_matrix_UB_22      -0.0440023000
_diffrn_orient_matrix_UB_23      -0.0046143000
_diffrn_orient_matrix_UB_31      -0.0239973000
_diffrn_orient_matrix_UB_32      -0.0241025000
_diffrn_orient_matrix_UB_33      0.0531926000
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48962
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.4209
_diffrn_reflns_theta_min         3.6878
_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    3.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95259
_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            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.1471
_exptl_crystal_size_mid          0.1205
_exptl_crystal_size_min          0.0796
_platon_squeeze_details
;
;
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0027
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10984
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.0004377
_refine_ls_shift/su_mean         0.0000219
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 3.04P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0681
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0681
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                9985
_reflns_number_total             10984
_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   0.0333
_oxford_refine_ls_scale          0.9788(13)
_oxford_reflns_number_all        10984
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om4006577_si_002.cif
_cod_data_source_block           arc61
_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        2183.41(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C41 H35 Cl1 F3 Ir1 N5'
_cod_database_code               4082319
_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                                                                             
;