Triclinic 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 120(1) K
Singh, Suneel P.; Verdu, Marcus J.; Lough, Alan J.; Schwan, Adrian L.; Acta Crystallographica Section E 65 (2009) o1387–; doi:10.1107/S1600536809019011

data_2222033
_publ_section_title
;Triclinic 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 120(1) K
;
_journal_coeditor_code           HB2979
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1387
_journal_paper_doi               10.1107/S1600536809019011
_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           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.884(6)
_cell_angle_beta                 82.681(8)
_cell_angle_gamma                87.306(8)
_cell_formula_units_Z            2
_cell_length_a                   5.1483(5)
_cell_length_b                   11.6600(15)
_cell_length_c                   13.6510(19)
_cell_measurement_reflns_used    4279
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     811.81(17)
_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 <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.12
_diffrn_reflns_av_sigmaI/netI    0.0878
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4279
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_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         0.761
_refine_diff_density_min         -0.495
_refine_ls_abs_structure_details 'Flack (1983), 1709 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.12(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1506P)^2^+0.8783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2437
_refine_ls_wR_factor_ref         0.2607
_reflns_number_gt                3526
_reflns_number_total             4279
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2979.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_database_code               2222033
_cod_database_fobs_code          2222033