Stabilized alpha-helix-catalyzed enantioselective epoxidation of alpha,beta-unsaturated ketones.
Nagano, Masanobu; Doi, Mitsunobu; Kurihara, Masaaki; Suemune, Hiroshi; Tanaka, Masakazu; Organic letters 12 (2010) 3564–3566; doi:10.1021/ol101435w

data_1503120
_publ_section_title
;
 Stabilized alpha-helix-catalyzed enantioselective epoxidation of
 alpha,beta-unsaturated ketones.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3564
_journal_page_last               3566
_journal_paper_doi               10.1021/ol101435w
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C44 H78 N6 O11 '
_chemical_formula_sum            'C44 H78 N6 O11'
_chemical_formula_weight         867.12
_chemical_melting_point          209
_chemical_name_systematic
; 
 Boc-(Leu-Leu-Ac5c[OMe])2-OMe 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   21.328(3)
_cell_length_b                   21.328(3)
_cell_length_c                   29.108(6)
_cell_measurement_reflns_used    73389
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11467(3)
_computing_cell_refinement       'RIGAKU Software'
_computing_data_collection       'RIGAKU Software'
_computing_data_reduction        'RIGAKU Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Seldrick & Gould, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID'
_diffrn_measurement_method       \w
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            87127
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1.3(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1648
_refine_ls_number_reflns         13014
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1944P)^2^+8.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2649
_refine_ls_wR_factor_ref         0.2788
_reflns_number_gt                11176
_reflns_number_total             13014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol101435w_si_002.cif
_cod_data_source_block           nag7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 32'
_cod_original_sg_symbol_H-M      'P3(2)   '
_cod_database_code               1503120