Daphniphyllum and diterpenoid alkaloids from Daphniphyllum longeracemosum.
Li, Chun-Shun; Di, Ying-Tong; Mu, Shu-Zhen; He, Hong-Ping; Zhang, Qiang; Fang, Xin; Zhang, Yu; Li, Shun-Lin; Lu, Yang; Gong, Yan-Qing; Hao, Xiao-Jiang; Journal of natural products 71 (2008) 1202–1206; doi:10.1021/np8001332

data_1504459
_publ_section_title
;
 Daphniphyllum and diterpenoid alkaloids from Daphniphyllum
 longeracemosum.
;
_journal_issue                   7
_journal_name_full               'Journal of natural products'
_journal_page_first              1202
_journal_page_last               1206
_journal_paper_doi               10.1021/np8001332
_journal_volume                  71
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C23 H33 N O4,H2 O'
_chemical_formula_sum            'C23 H35 N O5'
_chemical_formula_weight         405.52
_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                   8.799(2)
_cell_length_b                   14.981(3)
_cell_length_c                   15.655(3)
_cell_measurement_reflns_used    4651
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.88
_cell_volume                     2063.6(7)
_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,1990)
_computing_publication_material  'SHELXL97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17319
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.9(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+0.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                4339
_reflns_number_total             4651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np8001332-file008.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               1504459