Monoclinic modification of <i>N</i>-[(1,1-dimethylethoxy)carbonyl]-3-[(<i>R</i>)-prop-2-en-1-ylsulfinyl]-(<i>R</i>)-alanine ethyl ester at 200(1) K
Singh, Suneel P.; Verdu, Marcus J.; Lough, Alan J.; Schwan, Adrian L.; Acta Crystallographica Section E 65 (2009) o1385–o1386; doi:10.1107/S1600536809019023

data_2222032
_publ_section_title
;Monoclinic modification of
 <i>N</i>-[(1,1-dimethylethoxy)carbonyl]-3-[(<i>R</i>)-prop-2-en-1-ylsulfinyl]-(<i>R</i>)-alanine
 ethyl ester at 200(1) K
;
_journal_coeditor_code           HB2978
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1385
_journal_page_last               o1386
_journal_paper_doi               10.1107/S1600536809019023
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C13 H23 N O5 S'
_chemical_formula_moiety         'C13 H23 N O5 S'
_chemical_formula_sum            'C13 H23 N O5 S'
_chemical_formula_weight         305.38
_chemical_name_systematic
;<i>N</i>-[(1,1-dimethylethoxy)carbonyl]-3-[(<i>R</i>)-prop-2-en-1-ylsulfinyl]-
(<i>R</i>)-alanine
 ethyl ester
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.396(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.1859(6)
_cell_length_b                   11.5202(18)
_cell_length_c                   14.009(2)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    200.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.9
_cell_volume                     831.7(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3908
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.9
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.224
_refine_ls_abs_structure_details 'Flack (1983), 898 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.08(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.1385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                1844
_reflns_number_total             2397
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2978.cif
_cod_data_source_block           I
_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      'P 21'
_cod_database_code               2222032
_cod_database_fobs_code          2222032