β-Hydride Elimination and C-H Activation by an Iridium Acetate Complex, Catalyzed by Lewis Acids. Alkane Dehydrogenation Co-Catalyzed by Lewis Acids and (Phebox)Ir.
Gao, Yang; Guan, Changjian; Zhou, Meng; Kumar, Akshai; Emge, Thomas J.; Wright, Ashley M.; Goldberg, Karen I.; Krogh-Jespersen, Karsten; Goldman, Alan S.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.6b12995

data_4126008
_publ_section_title
;
 \b-Hydride Elimination and C-H Activation by an Iridium Acetate Complex,
 Catalyzed by Lewis Acids. Alkane Dehydrogenation Co-Catalyzed by Lewis
 Acids and (Phebox)Ir.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.6b12995
_journal_year                    2017
_chemical_formula_sum            'C22 H31 Ir N2 O2'
_chemical_formula_weight         547.69
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                111.002(2)
_cell_angle_beta                 109.988(2)
_cell_angle_gamma                120.760(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3340(10)
_cell_length_b                   11.4364(12)
_cell_length_c                   15.3376(16)
_cell_measurement_reflns_used    6180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.03
_cell_measurement_theta_min      2.56
_cell_volume                     993.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21258
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.039
_diffrn_reflns_theta_min         1.881
_exptl_absorpt_coefficient_mu    6.743
_exptl_absorpt_correction_T_max  0.4334
_exptl_absorpt_correction_T_min  0.2536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (TWINABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       lathe
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.045
_refine_diff_density_max         3.701
_refine_diff_density_min         -4.885
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         21258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19055
_reflns_number_total             21258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12995_si_005.cif
_cod_data_source_block           twin5
_cod_original_cell_volume        992.95(18)
_cod_database_code               4126008
_shelx_estimated_absorpt_t_min   0.377
_shelx_estimated_absorpt_t_max   0.751
_shelxl_version_number           2013-4
_shelx_res_checksum              30376
_shelx_hkl_checksum              5502