Molecular and crystalline structures of three (<i>S</i>)-4-alkoxycarbonyl-2-azetidinones containing long alkyl side chains from synchrotron X-ray powder diffraction data
Seijas, Luis E.; Mora, Asiloé J.; Delgado, Gerzon E.; López-Carrasquero, Francisco; Báez, María E.; Brunelli, Michela; Fitch, Andrew N.; Acta Crystallographica Section B 65 (2009) 724–730; doi:10.1107/S0108768109036386

data_2104632
_publ_section_title
;
 Molecular and crystalline structures of three
 (<i>S</i>)-4-alkoxycarbonyl-2-azetidinones containing long alkyl side
 chains from synchrotron X-ray powder diffraction data
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              724
_journal_page_last               730
_journal_paper_doi               10.1107/S0108768109036386
_journal_volume                  65
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source        'via synthetic'
_chemical_formula_analytical     'C20 H37 N O3'
_chemical_formula_moiety         'C20 H37 N O3'
_chemical_formula_structural     'C20 H37 N O3'
_chemical_formula_sum            'C20 H37 N O3'
_chemical_formula_weight         339.52
_chemical_melting_point          349
_chemical_name_systematic        ' (S)-4-hexadecyloxycarbonyl-2-azetidinone'
_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                90.0
_cell_angle_beta                 92.1693(6)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   37.15863(33)
_cell_length_b                   5.35911(5)
_cell_length_c                   5.30974(5)
_cell_measurement_temperature    298
_cell_volume                     1056.609(17)
_computing_molecular_graphics
'PLATON (Spek, 2003) and DIAMOND 2.1e (Brandenburg, 2001)'
_computing_publication_material
;GSAS2CIF (Toby et al., 2003), PLATON (Spek, 2003), and publCIF (Westrip,
 2009)
;
_computing_structure_refinement  GSAS
_computing_structure_solution
'FOX; Favre-Nicolin, V. & \^Cern\'y, R. (2002). J. Appl. Cryst. 35, 734--743.'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type
' High Resolution Diffractometer ID31, ESRF, Grenoble, France.'
_diffrn_radiation_monochromator  'Double crystal Si 111'
_diffrn_radiation_polarisn_ratio 1.0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.850227
_diffrn_source                   synchrotron
_diffrn_source_type              'Beamline ID31'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             376
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     needles
_pd_instr_location
' High Resolution Diffractometer ID31, ESRF, Grenoble, France.'
_pd_meas_2theta_range_inc        0.005
_pd_meas_2theta_range_max        32.065
_pd_meas_2theta_range_min        0.505
_pd_meas_number_of_points        7493
_pd_meas_scan_method             cont
_pd_phase_name
'from C:/gsas/MyWork/L_16_BDD_080709/L_16_4_H1.cif'
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.005
_pd_proc_2theta_range_max        32.06859
_pd_proc_2theta_range_min        0.50859
_pd_proc_info_datetime           2009-07-28T09:58:45
_pd_proc_info_excluded_regions
' The region 1.725 to 1.765 correspond to peak of an unidentified phase'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 16 terms.
 Shifted Chebyshev function of 1st kind
      1:    174.731     2:   -69.0201     3:    29.5791     4:   -27.7684    
      5:    27.0858     6:   -27.6400     7:   -5.19894     8:    24.4862    
      9:   -20.0027    10:   -7.46537    11:    9.13741    12:    7.24856    
     13:   -7.66897    14:    3.46197    15:    10.3473    16:   -4.77013    
;
_pd_proc_ls_peak_cutoff          0.00010
_pd_proc_ls_profile_function
;CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients
 as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl.
 Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P.
 Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W.
 Stephens, (1999). J. Appl. Cryst.,32,281-289. Peak tails are ignored where
 the intensity is below 0.0001 times the peak Aniso. broadening axis 0.0 0.0
 1.0
;
_pd_proc_ls_prof_R_factor        0.0783
_pd_proc_ls_prof_wR_expected     0.0485
_pd_proc_ls_prof_wR_factor       0.1066
_pd_proc_number_of_points        6312
_pd_proc_wavelength              0.850227
_pd_spec_mounting                ' borosilicate glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              40
_pd_spec_size_equat              1.0
_pd_spec_size_thick              1.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.22
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     256
_refine_ls_number_restraints     185
_refine_ls_R_Fsqd_factor         0.06998
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        1.543
_reflns_d_resolution_low         37.132
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              3
_reflns_limit_k_min              0
_reflns_limit_l_max              3
_reflns_limit_l_min              -3
_reflns_number_total             373
_cod_data_source_file            kd5033.cif
_cod_data_source_block           KD5033_L_16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (84
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (118 times).

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

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (84
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (118 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1056.608(16)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               2104632