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_7225708
_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         'C6 H11 N O2 S2, H2 O'
_chemical_formula_sum            'C6 H13 N O3 S2'
_chemical_formula_weight         211.29
_chemical_name_systematic        '2-(1,5,3-dithiazepan-3-yl)acetic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
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_atom_sites_solution_primary     direct
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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.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.507(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.6882(3)
_cell_length_b                   8.6039(4)
_cell_length_c                   8.0793(4)
_cell_measurement_reflns_used    1280
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.1197
_cell_measurement_theta_min      2.5237
_cell_volume                     463.48(4)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
_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  -48.00   50.00   1.0000    1.2600
omega____ theta____ kappa____ phi______ frames
    -       24.2348  -38.0000  -30.0000 98

  2 omega   53.00   96.00   1.0000    1.2600
omega____ theta____ kappa____ phi______ frames
    -       24.2348  178.0000  -90.0000 43

  3 omega  -19.00   67.00   1.0000    1.2600
omega____ theta____ kappa____ phi______ frames
    -       24.2348  -19.0000   30.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
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_diffrn_orient_matrix_UB_12      -0.0627213000
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_diffrn_orient_matrix_UB_21      -0.0910382000
_diffrn_orient_matrix_UB_22      -0.0126711000
_diffrn_orient_matrix_UB_23      0.0374140000
_diffrn_orient_matrix_UB_31      -0.0499039000
_diffrn_orient_matrix_UB_32      0.0520848000
_diffrn_orient_matrix_UB_33      -0.0573142000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0084
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_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2436
_diffrn_reflns_point_group_measured_fraction_full 0.840
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.189
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84544
_exptl_absorpt_correction_type   multi-scan
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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    1.514
_exptl_crystal_F_000             224.0
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.13(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2054
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.752
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.010
_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          0.0865
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.462
_reflns_Friedel_fraction_full    0.677
_reflns_Friedel_fraction_max     0.459
_reflns_number_gt                1990
_reflns_number_total             2054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00708b2.cif
_cod_data_source_block           compound_2a
_cod_depositor_comments
'Adding full bibliography for 7225700--7225708.cif.'
_cod_database_code               7225708
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_date_sample_data_collection 1386301073.56
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              31533
_shelxl_version_number           2013-4