The Unusual Role of CO Transfer in Molybdenum-Catalyzed Asymmetric Alkylations
Shane W. Krska; David L. Hughes; Robert A. Reamer; David J. Mathre; Yongkui Sun; Barry M. Trost; Journal of the American Chemical Society 124 (2002) 12656–12657; doi:10.1021/ja028035h

data_4115233
_publ_section_title
;
 The Unusual Role of CO Transfer in Molybdenum-Catalyzed Asymmetric
 Alkylations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12656
_journal_page_last               12657
_journal_paper_doi               10.1021/ja028035h
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C30 H29 Mo N3 O4, C4 H8 O, C4 H8, O'
_chemical_formula_sum            'C38 H45 Mo N3 O6'
_chemical_formula_weight         735.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.515(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4824(9)
_cell_length_b                   25.322(2)
_cell_length_c                   13.7540(12)
_cell_measurement_reflns_used    5577
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.61
_cell_measurement_theta_min      2.57
_cell_volume                     3534.3(5)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20981
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                11333
_reflns_number_total             13987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028035h_s2.cif
_cod_data_source_block           djm2063m
_cod_database_code               4115233