Xylogranatins A-D: novel tetranortriterpenoids with an unusual 9,10-seco scaffold from marine mangrove Xylocarpus granatum.
Yin, Sheng; Fan, Cheng-Qi; Wang, Xiao-Ning; Lin, Li-Ping; Ding, Jian; Yue, Jian-Min; Organic letters 8 (2006) 4935–4938; doi:10.1021/ol062101t

data_1506258
_publ_section_title
;
 Xylogranatins A-D: novel tetranortriterpenoids with an unusual 9,10-seco
 scaffold from marine mangrove Xylocarpus granatum.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              4935
_journal_page_last               4938
_journal_paper_doi               10.1021/ol062101t
_journal_volume                  8
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety         C34H42O12,C4H8O2
_chemical_formula_sum            'C38 H50 O14'
_chemical_formula_weight         730.78
_chemical_melting_point          450
_chemical_name_common
;
xylogranatin A 
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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            6
_cell_length_a                   23.446(16)
_cell_length_b                   23.446(16)
_cell_length_c                   14.036(14)
_cell_measurement_reflns_used    4337
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.636
_cell_measurement_theta_min      4.527
_cell_volume                     6682(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36628
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79609
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2340
_exptl_crystal_preparation       'ethyl acetate'
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.289
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(15)
_refine_ls_extinction_coef       0.0105(11)
_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   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8324
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.120
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                4968
_reflns_number_total             8324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol062101tsi20060825_030627.cif
_cod_data_source_block           cd25487
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P6(5)
_cod_database_code               1506258