Acceptorless Dehydrogenation of C-C Single Bonds Adjacent to Functional Groups by Metal-Ligand Cooperation
Shuhei Kusumoto; Midori Akiyama; Kyoko Nozaki; Journal of the American Chemical Society 135 (2013) 18726–18729; doi:10.1021/ja409672w

data_4121316
_publ_section_title
;
 Acceptorless Dehydrogenation of C-C Single Bonds Adjacent to Functional
 Groups by Metal-Ligand Cooperation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18726
_journal_page_last               18729
_journal_paper_doi               10.1021/ja409672w
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C46 H60 Ir O3 P'
_chemical_formula_weight         884.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.334(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.051(7)
_cell_length_b                   12.151(2)
_cell_length_c                   24.288(5)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    93.1500
_cell_measurement_theta_max      28.1320
_cell_measurement_theta_min      2.2382
_cell_volume                     7989(3)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'RIGAKU/MSCIO Saturn CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25932
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  0.7259
_exptl_absorpt_correction_T_min  0.7259
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       Block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.434
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7022
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+141.8840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                5971
_reflns_number_total             7022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409672w_si_002_2.cif
_cod_data_source_block           4a1
_cod_database_code               4121316