Formation of an Endoperoxide upon Chromium-Catalyzed Allylic Oxidation of a Triterpene by Oxygen.
Chung, Abbie; Miner, Matthew R.; Richert, Kathleen J.; Rieder, Curtis J.; Woerpel, K. A.; The Journal of organic chemistry 80 (2014) 266–; doi:10.1021/jo502344x

data_4030295
_publ_section_title
;
 Formation of an Endoperoxide upon Chromium-Catalyzed Allylic Oxidation of
 a Triterpene by Oxygen.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              266
_journal_paper_doi               10.1021/jo502344x
_journal_volume                  80
_journal_year                    2014
_chemical_absolute_configuration SN
_chemical_formula_sum            'C31 H44 O4'
_chemical_formula_weight         480.66
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_symmetry_space_group_name_H-M   'P 1 21 1'
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_cell_length_b                   7.2755(2)
_cell_length_c                   31.2394(10)
_cell_measurement_reflns_used    9720
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_cell_measurement_theta_min      2.42
_cell_volume                     2690.00(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            65960
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_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_correction_T_min  0.9606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.152
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
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_refine_ls_number_parameters     647
_refine_ls_number_reflns         7205
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.4208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                6865
_reflns_number_total             7205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502344x_si_004.cif
_cod_data_source_block           11kaw9h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4030293--4030296.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               4030295