Intermolecular interactions and chiral crystallization effects in (1,5,3-dithiazepan-3-yl)-alkanoic acids
Tulyabaev, Arthur R.; Mescheryakova, Ekaterina S.; Khabibullina, Guzel R.; Khalilov, Leonard M.; CrystEngComm 18 (2016) 5686–; doi:10.1039/C6CE00708B

data_7225706
_publ_section_title
;
 Intermolecular interactions and chiral crystallization effects in
 (1,5,3-dithiazepan-3-yl)-alkanoic acids
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5686
_journal_paper_doi               10.1039/C6CE00708B
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C7 H13 N O3 S2'
_chemical_formula_sum            'C7 H13 N O3 S2'
_chemical_formula_weight         223.30
_chemical_name_systematic
'(S)-(+)-2-(1,5,3-dithiazepan-3-yl)-3-hydroxypropanoic acid'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
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  Olex2 1.2-ac2
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2016-05-17 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
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_cell_length_a                   6.8616(11)
_cell_length_b                   8.8688(8)
_cell_length_c                   8.9458(10)
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_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.9270
_cell_measurement_theta_min      2.5140
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
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_computing_structure_solution
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SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      200(2)
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_diffrn_measurement_details
;
  1 omega  -60.00  -35.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -      -23.4536 -178.0000   30.0000 25

  2 omega   -5.00   46.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       24.0786   82.0000  140.0000 51

  3 omega   38.00   64.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       24.0786  -99.0000  -90.0000 26

  4 omega   -1.00   97.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       24.0786   38.0000  -60.0000 98

  5 omega   -6.00   93.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       24.0786   77.0000   30.0000 99

  6 omega  -48.00   64.00   1.0000    3.8900
omega____ theta____ kappa____ phi______ frames
    -       24.0786  -19.0000   90.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0288510000
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_diffrn_orient_matrix_UB_13      -0.0880862000
_diffrn_orient_matrix_UB_21      -0.0496962000
_diffrn_orient_matrix_UB_22      0.0751863000
_diffrn_orient_matrix_UB_23      -0.0170416000
_diffrn_orient_matrix_UB_31      0.0939471000
_diffrn_orient_matrix_UB_32      0.0422953000
_diffrn_orient_matrix_UB_33      -0.0180450000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.938
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_number            4183
_diffrn_reflns_point_group_measured_fraction_full 0.638
_diffrn_reflns_point_group_measured_fraction_max 0.546
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.919
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             236.0
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
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_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.12(9)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3248
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_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.0524
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_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                2873
_reflns_number_total             3248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00708b2.cif
_cod_data_source_block           compound_6
_cod_depositor_comments
'Adding full bibliography for 7225700--7225708.cif.'
_cod_original_cell_volume        470.11(11)
_cod_database_code               7225706
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_date_sample_data_collection 2014-10-27
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              38508
_shelxl_version_number           2013-4