Amplification of asymmetric induction in sequential reactions of bis-diazoacetates catalyzed by chiral dirhodium(II) carboxamidates.
Doyle, Michael P.; Wang, Yuanhua; Ghorbani, Pejman; Bappert, Erhard; Organic letters 7 (2005) 5035–5038; doi:10.1021/ol0520121

data_1506735
_publ_section_title
;
 Amplification of asymmetric induction in sequential reactions of
 bis-diazoacetates catalyzed by chiral dirhodium(II) carboxamidates.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5035
_journal_page_last               5038
_journal_paper_doi               10.1021/ol0520121
_journal_volume                  7
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C10 H12 O4'
_chemical_formula_sum            'C10 H12 O4'
_chemical_formula_weight         196.20
_chemical_name_common            MPPIM-B
_chemical_name_systematic
;
MPPIM-B
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.6310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0222(4)
_cell_length_b                   12.2044(6)
_cell_length_c                   10.4549(6)
_cell_measurement_reflns_used    6754
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.6
_cell_volume                     891.68(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Platon (Spek, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      NFRAMES=606,606,606,50,923
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.1012566
_diffrn_orient_matrix_UB_12      0.0558815
_diffrn_orient_matrix_UB_13      -0.0110871
_diffrn_orient_matrix_UB_21      -0.0308896
_diffrn_orient_matrix_UB_22      -0.0034215
_diffrn_orient_matrix_UB_23      -0.0953521
_diffrn_orient_matrix_UB_31      -0.0962927
_diffrn_orient_matrix_UB_32      0.0598354
_diffrn_orient_matrix_UB_33      0.0049118
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10653
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.96
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.27
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_id                'Doyle/YuanhuaWang MPPIM-B'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_coef       0.059(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         2143
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.012P)^2^+0.2915P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2046
_reflns_number_total             2143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0520121si20050819_025449.cif
_cod_data_source_block           1247
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1506735
_diffrn_measurement_total_frames-ccd 2791
_diffrn_measurement_frame_width-ccd 0.3
_diffrn_detector_distance-ccd    4.99
_diffrn_measurement_frame_time-ccd 15
_diffrn_measurement_total_time-ccd 17.2
_diffrn_measurement_frame_size-ccd 512