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_7225705
_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_formula_moiety         'C8 H15 N O2 S2'
_chemical_formula_sum            'C8 H15 N O2 S2'
_chemical_formula_weight         221.33
_chemical_name_systematic        '2-(1,5,3-dithiazepan-3-yl)butanoic acid'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-28
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                78.801(5)
_cell_angle_beta                 87.344(5)
_cell_angle_gamma                69.141(5)
_cell_formula_units_Z            2
_cell_length_a                   5.0968(3)
_cell_length_b                   6.7869(3)
_cell_length_c                   16.6360(10)
_cell_measurement_reflns_used    2049
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.9914
_cell_measurement_theta_min      2.4919
_cell_volume                     527.34(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
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
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 16.1709
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -97.00  -29.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -      -23.4536  154.0000  131.0000 68

  2 omega   10.00   83.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       24.0786   57.0000  150.0000 73

  3 omega   37.00   78.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       24.0786 -121.0000   69.0000 41

  4 omega  -39.00   40.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       24.0786  -57.0000  -90.0000 79

  5 omega  -18.00   95.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       24.0786   19.0000   90.0000 113
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1371008000
_diffrn_orient_matrix_UB_12      0.0374676000
_diffrn_orient_matrix_UB_13      0.0156566000
_diffrn_orient_matrix_UB_21      -0.0579967000
_diffrn_orient_matrix_UB_22      0.0253979000
_diffrn_orient_matrix_UB_23      -0.0402698000
_diffrn_orient_matrix_UB_31      -0.0057248000
_diffrn_orient_matrix_UB_32      -0.1045469000
_diffrn_orient_matrix_UB_33      0.0048484000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4589
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.061
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             236.0
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_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          0.1190
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2551
_reflns_number_total             3000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00708b2.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 7225700--7225708.cif.'
_cod_original_cell_volume        527.34(6)
_cod_database_code               7225705
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_date_sample_data_collection 2014-03-27
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              19372
_shelxl_version_number           2013-4