A New Chiral Rh(II) Catalyst for Enantioselective [2 + 1]-Cycloaddition. Mechanistic Implications and Applications
Yan Lou; Manabu Horikawa; Robin A. Kloster; Natalie A. Hawryluk; E. J. Corey; Journal of the American Chemical Society 126 (2004) 8916–8918; doi:10.1021/ja047064k

data_4112774
_publ_section_title
;
 A New Chiral Rh(II) Catalyst for Enantioselective [2 + 1]-Cycloaddition.
 Mechanistic Implications and Applications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8916
_journal_page_last               8918
_journal_paper_doi               10.1021/ja047064k
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C84 H70 F12 N10 O12 Rh2 S4'
_chemical_formula_weight         1973.56
_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                 90.439(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2670(17)
_cell_length_b                   21.482(3)
_cell_length_c                   16.249(2)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      2.34
_cell_volume                     4630.9(10)
_computing_cell_refinement       'SMART (BRUKER, V5.054, 1998)'
_computing_data_collection       'ASTRO (BRUKER, V5.007, 1997)'
_computing_data_reduction        'SAINT (BRUKER, V6.01, 1999)'
_computing_molecular_graphics    'SHELXTL (BRUKER, 1998, V5.1)'
_computing_publication_material  'XCIF (Sheldrick and BRUKER, 1997, V5.1)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w, 0.3 deg'
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31049
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9389
_exptl_absorpt_correction_type   'Semi-empirical, SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         20829
_refine_ls_number_restraints     481
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0758
_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^)+(0.0941P)^2^+4.1931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1846
_reflns_number_gt                18972
_reflns_number_total             20829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047064ksi20040519_112103.cif
_cod_data_source_block           ejc38t
_cod_original_cell_volume        4630.8(10)
_cod_database_code               4112774