A Key Intermediate in the Synthesis of (+)-Hernandulcin
Zukerman-Schpector, J.; Caracelli, I.; de Oliveira, S. Ma.; Faria de Medeiros, E.; Brocksom, T. J.; Acta Crystallographica Section C 52 (1996) 1579–1581; doi:10.1107/S010827019600008X

data_2005030
_publ_contact_author
;
    Prof. J. Zukerman-Schpector
    Departamento Qu\'imica
    Universidade Federal de S\~ao Carlos
    Caixa Postal 676
    13565-905 S\~ao Carlos
    SP
    Brazil
;
_publ_section_title
;
 A Key Intermediate in the Synthesis of (+)-Hernandulcin
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1579
_journal_page_last               1581
_journal_paper_doi               10.1107/S010827019600008X
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C14 H23 N O3'
_chemical_formula_sum            'C14 H23 N O3'
_chemical_formula_weight         253.341
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           'manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.742(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5380(10)
_cell_length_b                   8.8950(10)
_cell_length_c                   16.0310(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.79
_cell_measurement_theta_min      9.00
_cell_volume                     1465.7(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_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  0.0285
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2667
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        -1.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.127
_refine_ls_goodness_of_fit_obs   1.154
_refine_ls_hydrogen_treatment    'refxyz, one common U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2571
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.154
_refine_ls_R_factor_all          0.1881
_refine_ls_R_factor_obs          0.0535
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.8671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1715
_refine_ls_wR_factor_obs         0.1048
_reflns_number_observed          1052
_reflns_number_total             2571
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1142.cif
_cod_data_source_block           default
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.8671P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.8671P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2005030