<i>Amaryllidaceae</i> Alkaloids: (+)-Tazettine, (+)-3-<i>O</i>-Demethylcriwelline and (+)-3-Epimacronine at 173 K
Linden, Anthony; Akineri, Gülnur; Noyan, Seda; Gözler, Tekant; Hesse, Manfred; Acta Crystallographica Section C 54 (1998) 1653–1659; doi:10.1107/S0108270198006933

data_2007808
_publ_section_title
;
 <i>Amaryllidaceae</i> Alkaloids: (+)-Tazettine,
 (+)-3-<i>O</i>-Demethylcriwelline and (+)-3-Epimacronine at 173 K
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1653
_journal_page_last               1659
_journal_paper_doi               10.1107/S0108270198006933
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C18 H19 N O5, 0.066H2 O'
_chemical_formula_sum            'C18 H19.132 N O5.066'
_chemical_formula_weight         330.54
_chemical_melting_point          403.0(10)
_chemical_name_common            (+)-3-epimacronine
_chemical_name_systematic
;(+)-(3S,4aS,6aR,13bS)-3-methoxy-5-methyl-3,4,4a,5,6,6a-hexahydro-[1,3]dioxolo[6,
7][2]benzopyrano[3,4-c]indol-8-one
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 95.054(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.176(2)
_cell_length_b                   17.666(2)
_cell_length_c                   11.0743(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      19
_cell_volume                     1593.3(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1991)
;
_computing_data_reduction
'TEXSAN PROCESS (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4033
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             698.64
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.21
_refine_ls_extinction_coef       0.0051(13)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.3026P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.090
_reflns_number_gt                3413
_reflns_number_total             3781
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1465.cif
_cod_data_source_block           III
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-24

The following automatic conversions were performed:

'_chemical_melting_point' value '402-404' was changed to '403.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '402-404' was changed to '403.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1593.3(3)
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2007808