Experimental and theoretical mechanistic investigation of the iridium-catalyzed dehydrogenative decarbonylation of primary alcohols.
Olsen, Esben P. K.; Singh, Thishana; Harris, Pernille; Andersson, Pher G.; Madsen, Robert; Journal of the American Chemical Society 137 (2015) 834–842; doi:10.1021/ja5106943

data_4123290
_publ_section_title
;
 Experimental and theoretical mechanistic investigation of the
 iridium-catalyzed dehydrogenative decarbonylation of primary alcohols.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              834
_journal_page_last               842
_journal_paper_doi               10.1021/ja5106943
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C45 H33 Cl2 Ir O P2, C H2 Cl2'
_chemical_formula_sum            'C46 H35 Cl4 Ir O P2'
_chemical_formula_weight         999.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-24
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Olex2 1.2
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   21.1066(3)
_cell_measurement_reflns_used    24666
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.4030
_cell_measurement_theta_min      2.8470
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
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_diffrn_measurement_details
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  1 omega  -35.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8919   38.0000  120.0000 89

  2 omega  -55.00  -28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8919  -57.0000  -30.0000 27

  3 omega  -15.00   15.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8919  -57.0000  -30.0000 30

  4 omega  -37.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8919   57.0000 -150.0000 61

  5 omega  -22.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.2669   77.0000  150.0000 108

  6 omega  -70.00  -45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.2669  -19.0000  150.0000 25

  7 omega  -20.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.2669  -99.0000    0.0000 71
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_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
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_diffrn_orient_matrix_UB_32      0.0451077000
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.714
_diffrn_reflns_theta_min         2.676
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.760
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_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
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Empirical absorption correction using spherical harmonics,
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_exptl_crystal_colour            yellow
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_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.33
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 Flack x determined using 4063 quotients [(I+)-(I-)]/[(I+)+(I-)]
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_refine_ls_number_reflns         10155
_refine_ls_number_restraints     0
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_refine_ls_structure_factor_coef Fsqd
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 w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+3.1284P]
 where P=(Fo^2^+2Fc^2^)/3
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5106943_si_001.cif
_cod_data_source_block           IrH(Cl)2(CO)BINAP
_cod_depositor_comments
'Adding full bibliography for 4123286--4123290.cif.'
_cod_original_cell_volume        3959.12(12)
_cod_database_code               4123290
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'Ir1 Cl2 P2 C45 H33'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C6(H6), C13(H13), C38(H38), C14(H14), C44(H44), C3(H3),
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