Catalysis of Enantioselective [2+1]-Cycloaddition Reactions of Ethyl Diazoacetate and Terminal Acetylenes Using Mixed-Ligand Complexes of the Series Rh2(RCO2)n(L*4-n). Stereochemical Heuristics for Ligand Exchange and Catalyst Synthesis
Yan Lou; Travis P. Remarchuk; E. J. Corey; Journal of the American Chemical Society 127 (2005) 14223–14230; doi:10.1021/ja052254w

data_4111989
_publ_section_title
;
 Catalysis of Enantioselective [2+1]-Cycloaddition Reactions of Ethyl
 Diazoacetate and Terminal Acetylenes Using Mixed-Ligand Complexes of the
 Series Rh2(RCO2)n(L*4-n). Stereochemical Heuristics for Ligand Exchange
 and Catalyst Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14223
_journal_page_last               14230
_journal_paper_doi               10.1021/ja052254w
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C57 H50 Cl2 F9 N9 O11 Rh2 S3'
_chemical_formula_weight         1580.96
_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                 108.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5313(13)
_cell_length_b                   19.398(3)
_cell_length_c                   16.449(2)
_cell_measurement_temperature    193(2)
_cell_volume                     3194.9(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      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23235
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_refine_diff_density_max         0.984
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.039(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         13533
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0563P)^2^+0.6622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                13233
_reflns_number_total             13533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052254wsi20050407_035743.cif
_cod_data_source_block           rak22
_cod_original_cell_volume        3194.8(7)
_cod_database_code               4111989