Neogenkwanines A–H: Daphnane-Type Diterpenes Containing 4,7 or 4,6-Ether Group from the Flower Bud of Daphne genkwa
Li, Lingzhi; Song, shao-jiang; gao, pinyi; Li, Feifei; Wang, Lihui; liu, Qingbo; Huang, Xiaoxiao; Li, Danqi; Sun, Yu; RSC Adv.  (2014) –; doi:10.1039/C4RA13167C

data_7219030
_publ_section_title
;
 Neogenkwanines A--H: Daphnane-Type Diterpenes Containing 4,7 or 4,6-Ether
 Group from the Flower Bud of Daphne genkwa
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA13167C
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H36 O9, C4 H8 O2'
_chemical_formula_sum            'C31 H44 O11'
_chemical_formula_weight         592.66
_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
_audit_update_record
;
2014-10-25 deposited with the CCDC.
2014-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7035(7)
_cell_length_b                   12.7664(9)
_cell_length_c                   21.1157(14)
_cell_measurement_reflns_used    5361
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      59.74
_cell_measurement_theta_min      3.78
_cell_volume                     3154.9(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9697
_diffrn_reflns_theta_full        59.94
_diffrn_reflns_theta_max         59.94
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.9620
_exptl_absorpt_correction_T_min  0.7995
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plane
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_coef       0.0040(3)
_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   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.5284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                4183
_reflns_number_total             4408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra13167c2.cif
_cod_data_source_block           s079
_cod_database_code               7219030