Synthesis of the 6,6,5,7-tetracyclic core of daphnilongeranin B
Xiaochun Xiong; Yong Li; Zhaoyong Lu; Ming Wan; Jun Deng; Shuhang Wu; Huawu Shao; Ang Li; Chem.Commun. 50 (2014) 5294–; doi:10.1039/C3CC47873D

data_7112630
_publ_section_title
;
 Synthesis of the 6,6,5,7-tetracyclic core of daphnilongeranin B
;
_journal_name_full               Chem.Commun.
_journal_page_first              5294
_journal_paper_doi               10.1039/C3CC47873D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C23 H29 N O7'
_chemical_formula_weight         431.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.029(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2542(9)
_cell_length_b                   26.236(3)
_cell_length_c                   10.2531(12)
_cell_measurement_reflns_used    1308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      40.559
_cell_measurement_theta_min      5.139
_cell_volume                     2154.2(4)
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11005
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.6358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.2123
_reflns_number_gt                2414
_reflns_number_total             3990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47873d.txt
_cod_data_source_block           cd211492
_cod_original_cell_volume        2154.1(4)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7112630