A Catalytic Cycle for Oxidation of tert-Butyl Methyl Ether by a Double C-H Activation-Group Transfer Process
Matthew T. Whited; Robert H. Grubbs; Journal of the American Chemical Society 130 (2008) 16476–16477; doi:10.1021/ja8071385

data_4108804
_publ_contact_author_address
;1200 E. California Blvd.
Pasadena, CA 91125
;
_publ_contact_author_email       rhg@caltech.edu
_publ_contact_author_fax         626-564-9297
_publ_contact_author_name        'Robert H. Grubbs'
_publ_contact_author_phone       626-395-6003
_publ_section_title
;
 A Catalytic Cycle for Oxidation of tert-Butyl Methyl Ether by a Double
 C-H Activation-Group Transfer Process
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16476
_journal_page_last               16477
_journal_paper_doi               10.1021/ja8071385
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C26 H40 Ir N3 P2'
_chemical_formula_sum            'C26 H40 Ir N3 P2'
_chemical_formula_weight         648.75
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4977(10)
_cell_length_b                   30.723(4)
_cell_length_c                   9.5901(11)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.20
_cell_measurement_theta_min      2.23
_cell_volume                     2798.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36987
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         35.91
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    4.903
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.946
_refine_diff_density_min         -2.394
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack (1983), 4537 Friedel pairs'
_refine_ls_abs_structure_Flack   0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         11069
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                7090
_reflns_number_total             11069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8071385_si_002.cif
_cod_data_source_block           mtw102abs
_cod_original_cell_volume        2798.3(6)
_cod_database_code               4108804