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_4107753
_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         'C27 H40 Ir N O P2, C6 H6'
_chemical_formula_sum            'C33 H46 Ir N O P2'
_chemical_formula_weight         726.85
_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                 95.130(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1315(15)
_cell_length_b                   9.6222(12)
_cell_length_c                   27.912(3)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.98
_cell_measurement_theta_min      2.33
_cell_volume                     3245.2(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            256669
_diffrn_reflns_theta_full        45.08
_diffrn_reflns_theta_max         45.08
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.238
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.092
_refine_diff_density_max         2.998
_refine_diff_density_min         -1.889
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.685
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         26785
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.711
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_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          0.0487
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                20862
_reflns_number_total             26785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801865c-file003_1.cif
_cod_data_source_block           mtw78abs
_cod_original_cell_volume        3245.1(7)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4107753