The first limonoid peroxide in the Meliaceae family: walsuronoid A from Walsura robusta.
Yin, Sheng; Wang, Xiao-Ning; Fan, Cheng-Qi; Liao, Shang-Gao; Yue, Jian-Min; Organic letters 9 (2007) 2353–2356; doi:10.1021/ol070735+

data_1516662
_publ_section_title
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 The first limonoid peroxide in the Meliaceae family: walsuronoid A from
 Walsura robusta.
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_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              2353
_journal_page_last               2356
_journal_paper_doi               10.1021/ol070735+
_journal_volume                  9
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_sum            'C32 H44 O11'
_chemical_formula_weight         604.67
_chemical_melting_point          465
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.478(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2919(8)
_cell_length_b                   18.2388(18)
_cell_length_c                   10.7413(10)
_cell_measurement_reflns_used    3810
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.834
_cell_measurement_theta_min      4.542
_cell_volume                     1557.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1380
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9186
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75521
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             648
_exptl_crystal_preparation       acetone
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.465
_exptl_crystal_size_min          0.312
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         3500
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                2859
_reflns_number_total             3500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070735%2Bsi20070325_105514.cif
_cod_data_source_block           cd26319
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'ad_' changed to 'ad'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
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_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1516662