Highly stereoselective epoxidation with H2O2 catalyzed by electron-rich aminopyridine manganese catalysts.
Cussó, Olaf; Garcia-Bosch, Isaac; Font, David; Ribas, Xavi; Lloret-Fillol, Julio; Costas, Miquel; Organic letters 15 (2013) 6158–6161; doi:10.1021/ol403018x

data_1556253
_publ_section_title
;
 Highly stereoselective epoxidation with H2O2 catalyzed by electron-rich
 aminopyridine manganese catalysts.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6158
_journal_page_last               6161
_journal_paper_doi               10.1021/ol403018x
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H36 F6 Mn N6 O6 S2'
_chemical_formula_sum            'C26 H36 F6 Mn N6 O6 S2'
_chemical_formula_weight         761.67
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90.00
_cell_angle_beta                 103.655(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1618(2)
_cell_length_b                   9.79637(18)
_cell_length_c                   16.8542(4)
_cell_measurement_reflns_used    8381
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9412
_cell_measurement_theta_min      4.4702
_cell_volume                     1630.39(6)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21c (release 23-05-2012 CrysAlis171 .NET)
(compiled May 23 2012,12:53:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21c (release 23-05-2012 CrysAlis171 .NET)
(compiled May 23 2012,12:53:54)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21c (release 23-05-2012 CrysAlis171 .NET)
(compiled May 23 2012,12:53:54)
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_computing_molecular_graphics    Shelxtl
_computing_publication_material  Shelxtl
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16314
_diffrn_reflns_theta_full        73.13
_diffrn_reflns_theta_max         73.13
_diffrn_reflns_theta_min         4.48
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21c (release 23-05-2012 CrysAlis171 .NET)
(compiled May 23 2012,12:53:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fiber
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.4813
_exptl_crystal_size_mid          0.0418
_exptl_crystal_size_min          0.0228
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         5896
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.4414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                5356
_reflns_number_total             5896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol403018x_si_001.cif
_cod_data_source_block           ocnmebpbp
_cod_original_cell_volume        1630.38(6)
_cod_database_code               1556253