Oxygen-Atom Transfer from Carbon Dioxide to a Fischer Carbene at (PNP)Ir
Matthew T. Whited; Robert H. Grubbs; Journal of the American Chemical Society 130 (2008) 5874–5875; doi:10.1021/ja801865c

data_4107754
_publ_contact_author_email       rhg@caltech.edu
_publ_contact_author_name        'Robert H. Grubbs'
_publ_section_title
;
 Oxygen-Atom Transfer from Carbon Dioxide to a Fischer Carbene at (PNP)Ir
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5874
_journal_page_last               5875
_journal_paper_doi               10.1021/ja801865c
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C31 H50 Ir N O P2'
_chemical_formula_sum            'C31 H50 Ir N O P2'
_chemical_formula_weight         706.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.557(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.554(4)
_cell_length_b                   11.303(3)
_cell_length_c                   18.303(4)
_cell_measurement_reflns_used    6128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.90
_cell_measurement_theta_min      2.48
_cell_volume                     3216.6(14)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1062
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            75382
_diffrn_reflns_theta_full        33.55
_diffrn_reflns_theta_max         38.44
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.273
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.092
_refine_diff_density_max         6.866
_refine_diff_density_min         -4.075
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         16906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0526
_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          0.0888
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                10359
_reflns_number_total             16906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801865c-file003_2.cif
_cod_data_source_block           mtw67abs
_cod_original_cell_volume        3216.6(13)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4107754