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_4111993
_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            'C78 H69 F12 N15 O12 Rh2 S4'
_chemical_formula_weight         1970.54
_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                 102.554(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.513(2)
_cell_length_b                   17.419(2)
_cell_length_c                   17.740(3)
_cell_measurement_temperature    213(2)
_cell_volume                     4377.5(11)
_computing_cell_refinement       'SMART (BRUKER, V5.625, 2001)'
_computing_data_collection       'ASTRO (BRUKER, V5.007, 1997)'
_computing_data_reduction        'SAINT (BRUKER, V6.22, 2001)'
_computing_molecular_graphics    'SHELXTL (BRUKER, 2000, V6.1)'
_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      213(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker 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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28372
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9151
_exptl_absorpt_correction_T_min  0.8859
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         19540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+1.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                17597
_reflns_number_total             19540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052254wsi20050413_123036.cif
_cod_data_source_block           ejc74t
_cod_original_cell_volume        4377.6(11)
_cod_database_code               4111993