Acetylcholinesterase Inhibitory Alkaloids from the Whole Plants of Zephyranthes carinata.
Zhan, Guanqun; Zhou, Junfei; Liu, Junjun; Huang, Jinfeng; Zhang, Hanqi; Liu, Rong; Yao, Guangmin; Journal of natural products 80 (2017) 2462–2471; doi:10.1021/acs.jnatprod.7b00301

data_1547128
_publ_section_title
;
 Acetylcholinesterase Inhibitory Alkaloids from the Whole Plants of
 Zephyranthes carinata.
;
_journal_issue                   9
_journal_name_full               'Journal of natural products'
_journal_page_first              2462
_journal_page_last               2471
_journal_paper_doi               10.1021/acs.jnatprod.7b00301
_journal_volume                  80
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H21 N O5, 1.5(H2 O) '
_chemical_formula_sum            'C17 H24 N O6.5'
_chemical_formula_weight         346.37
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 103.780(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.998(2)
_cell_length_b                   12.1491(11)
_cell_length_c                   11.3547(11)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      56.49
_cell_measurement_theta_min      2.62
_cell_volume                     3483.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17506
_diffrn_reflns_theta_full        57.49
_diffrn_reflns_theta_max         57.49
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.9051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881;
Flack  parameter = 0.1(3), 2068 Friedel pairs.
Hooft <i>et al.</i> (2010) and Spek (2009);
Hooft parameter = 0.1(1), 2068 Bijvoet pairs.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+2.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4159
_reflns_number_total             4530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np7b00301_si_003.cif
_cod_data_source_block           t
_cod_depositor_comments
;
Adding full bibliography for 1547128--1547129.cif.

2019-08-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_Hall     'c 2y'
_cod_original_sg_symbol_H-M      'c 2'
_cod_original_formula_moiety     '2(C17 H21 N O5), 3(H2 O) '
_cod_original_formula_sum        'C34 H48 N2 O13'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     692.74
_cod_database_code               1547128