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_4121315
_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            'C50 H67 Ir Li O4 P'
_chemical_formula_weight         962.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 89.94(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.87(3)
_cell_length_b                   18.89(4)
_cell_length_c                   19.99(3)
_cell_measurement_reflns_used    313
_cell_measurement_temperature    243.1500
_cell_measurement_theta_max      23.3782
_cell_measurement_theta_min      3.3622
_cell_volume                     4860(17)
_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      243(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17537
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  0.8719
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       Block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                4841
_reflns_number_total             8306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409672w_si_002_1.cif
_cod_data_source_block           3a1
_cod_original_cell_volume        4862(16)
_cod_database_code               4121315