Relative and Absolute Configuration of Aloperine
Brosius, Arthur D.; Ziller, Joseph W.; Zhang, Qiming; Acta Crystallographica Section C 53 (1997) 1510–1512; doi:10.1107/S0108270197009244

data_2006624
_publ_section_title
;
 Relative and Absolute Configuration of Aloperine
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1510
_journal_page_last               1512
_journal_paper_doi               10.1107/S0108270197009244
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C15 H24 N2'
_chemical_formula_sum            'C15 H24 N2'
_chemical_formula_weight         232.27
_chemical_melting_point          344.5(6)
_chemical_name_common            Aloperine
_chemical_name_systematic
;
(6R,7R,9R,11S)--16,17-Didehydro--9--de--2--piperidinylormosanine
;
_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                90.00
_cell_angle_beta                 97.415(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.006(2)
_cell_length_b                   6.6905(13)
_cell_length_c                   10.963(2)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    158
_cell_measurement_theta_max      13.85
_cell_measurement_theta_min      3.76
_cell_volume                     655.0(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'CARESS (Broach, 1978)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick 1994)'
_diffrn_ambient_temperature      158
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         rotating-anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1747
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.160
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.(4)
_refine_ls_extinction_coef       0.012(6)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_hydrogen_treatment    'H atoms refined isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         1641
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_obs          .0383
_refine_ls_shift/esd_max         '< 0.001'
_refine_ls_shift/esd_mean        '< 0.001'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1015
_refine_ls_wR_factor_obs         .0931
_reflns_number_observed          1335
_reflns_number_total             1641
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sx1032.cif
_cod_data_source_block           1
_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:

'_chemical_melting_point' value '70.8--72.0 \%C' was changed to
'344.5(6)' - it was converted from degrees Celsius(C) to Kelvins(K),
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 '70.8--72.0 \%C' was changed to
'344.5(6)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_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 

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^)+(0.0523P)^2^+0.1282P] 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^)+(0.0523P)^2^+0.1282P] 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'
_cod_database_code               2006624