Supercritical and Liquid Solvent Effects on the Enantioselectivity of Asymmetric Cyclopropanation with Tetrakis[1-[(4-tert-butylphenyl)- sulfonyl]-(2S)-pyrrolidinecarboxylate]dirhodium(II)
Dolores C. Wynne; Marilyn M. Olmstead; Philip G. Jessop; Journal of the American Chemical Society 122 (2000) 7638–7647; doi:10.1021/ja000894n

data_4116119
_publ_section_title
;
 Supercritical and Liquid Solvent Effects on the Enantioselectivity of
 Asymmetric Cyclopropanation with Tetrakis[1-[(4-tert-butylphenyl)-
 sulfonyl]-(2S)-pyrrolidinecarboxylate]dirhodium(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7638
_journal_page_last               7647
_journal_paper_doi               10.1021/ja000894n
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C72 H104 N6 O18 Rh2 S4'
_chemical_formula_weight         1675.67
_chemical_name_common            '[Rh2(TBSP)4(DMF)2].0.5toluene.0.5n-pentane'
_chemical_name_systematic
; 
 tetrakis[1-[(4-tert-butylphenyl)sulfonyl]
-(2S)-pyrrolidinecarboxylate]dirhodium(II) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6911(5)
_cell_length_b                   24.4434(11)
_cell_length_c                   29.7425(13)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      60.23
_cell_measurement_theta_min      4.38
_cell_volume                     7772.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.1144
_diffrn_reflns_av_sigmaI/netI    0.1650
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            76290
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8169
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.850
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         24884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1310
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                13770
_reflns_number_total             24884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000894n.cif
_cod_data_source_block           mn1028
_cod_database_code               4116119