Daphlongeranines A and B, two novel alkaloids possessing unprecedented skeletons from Daphniphyllum longeracemosum.
Li, Chun-Shun; Di, Ying-Tong; He, Hong-Ping; Gao, Suo; Wang, Yue-Hu; Lu, Yang; Zhong, Jia-Liang; Hao, Xiao-Jiang; Organic letters 9 (2007) 2509–2512; doi:10.1021/ol070942+

data_1516653
_publ_section_title
;
 Daphlongeranines A and B, two novel alkaloids possessing unprecedented
 skeletons from Daphniphyllum longeracemosum.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2509
_journal_page_last               2512
_journal_paper_doi               10.1021/ol070942+
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C24 H31 N O5,H2 0 '
_chemical_formula_sum            'C24 H33 N O6'
_chemical_formula_weight         431.51
_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                 109.89(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.576(1)
_cell_length_b                   8.049(1)
_cell_length_c                   10.772(1)
_cell_measurement_reflns_used    2124
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.96
_cell_volume                     1106.9(2)
_computing_cell_refinement       'SCALE(Otwinowski & Minor,1996)'
_computing_data_collection       'DENZO(Otwinowski & Minor,1996)'
_computing_data_reduction        'SCALE(Otwinowski & Minor,1996)'
_computing_molecular_graphics    'ORTEPII(Johnson,1976) and PLUTON(Spek,1990)'
_computing_publication_material  'SHELXL97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'MAC DIP 2030K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotate anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2124
_diffrn_reflns_theta_full        25.55
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.080(9)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2124
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                2093
_reflns_number_total             2124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070942%2Brom20070422_022513.cif
_cod_data_source_block           d4857
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1516653