Highly acylated diterpenoids with a new 3,4-secograyanane skeleton from the flower buds of Rhododendron molle.
Wang, Sujuan; Lin, Sheng; Zhu, Chenggen; Yang, Yongchun; Li, Shuai; Zhang, Jianjun; Chen, Xiaoguang; Shi, Jiangong; Organic letters 12 (2010) 1560–1563; doi:10.1021/ol1002797

data_1502898
_publ_section_title
;
 Highly acylated diterpenoids with a new 3,4-secograyanane skeleton from
 the flower buds of Rhododendron molle.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1560
_journal_page_last               1563
_journal_paper_doi               10.1021/ol1002797
_journal_volume                  12
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H42 O13'
_chemical_formula_sum            'C31 H42 O13'
_chemical_formula_weight         622.65
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.15910(10)
_cell_length_b                   15.29610(10)
_cell_length_c                   18.7549(2)
_cell_measurement_reflns_used    4287
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      59.86
_cell_measurement_theta_min      3.73
_cell_volume                     3201.29(5)
_computing_cell_refinement       'SCALE(Otwinowski & Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski & Minor,1997)'
_computing_data_reduction        'SCALE(Otwinowski & Minor,1997)'
_computing_molecular_graphics    PLUTON(Spek,2003)
_computing_publication_material  'SHELXL97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'MAC DIP 2030K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotate anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11060
_diffrn_reflns_theta_full        59.86
_diffrn_reflns_theta_max         59.86
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(17)
_refine_ls_extinction_coef       0.0024(2)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.4966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4213
_reflns_number_total             4287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol1002797_si_002.cif
_cod_data_source_block           a
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_database_code               1502898