The absolute configuration of 1-epialexine hemihydrate
Thompson, Amber L.; Watkin, David J.; Gal, Zoltan A.; Jones, Laurence; Hollinshead, Jackie; Jenkinson, Sarah F.; Fleet, George W. J.; Nash, Robert J.; Acta Crystallographica Section C 64 (2008) o649–o652; doi:10.1107/S0108270108037086

data_2016868
_publ_section_title
;
 The absolute configuration of 1-epialexine hemihydrate
;
_journal_coeditor_code           LN3116
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o649
_journal_page_last               o652
_journal_paper_doi               10.1107/S0108270108037086
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C8 H15 N1 O4, 0.5H2 O'
_chemical_formula_moiety         'C8 H15 N1 O4, 0.5(H2 O)'
_chemical_formula_sum            'C8 H16 N O4.5'
_chemical_formula_weight         198.22
_chemical_melting_point_gt       432
_chemical_melting_point_lt       434
_chemical_name_common
;
1-epi-Alexine hemihydrate
;
_chemical_name_systematic
;
(1<i>S</i>,2<i>R</i>,3<i>R</i>,7<i>S</i>,7a<i>S</i>)-1,2,7-trihydroxy-3-
(hydroxymethyl)pyrrolizidine hemihydrate
;
_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
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 93.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4267(3)
_cell_length_b                   7.30208(18)
_cell_length_c                   9.5708(2)
_cell_measurement_reflns_used    5964
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.4819
_cell_measurement_theta_min      5.1926
_cell_volume                     866.51(4)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7771
_diffrn_reflns_theta_full        25.863
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_min         3.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[empirical absorption correction using spherical harmonics (CrysAlis RED)
implementing the SCALE3 ABSPACK scaling algorithm (Oxford Diffraction,
2008)]
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.16
_refine_ls_abs_structure_details 'Flack (1983), 777 Friedel-pairs'
_refine_ls_abs_structure_Flack   -1.5(9)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000984
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.00P]
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0643
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                1402
_reflns_number_total             1724
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ln3116.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C8 H16 N1 O4.50'
_cod_database_code               2016868