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_7225707
_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         'C7 H12 N O2 S2'
_chemical_formula_sum            'C7 H12 N O2 S2'
_chemical_formula_weight         206.30
_chemical_name_systematic        '3-(1,5,3-dithiazepan-3-yl)propanoic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.709(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.9212(5)
_cell_length_b                   30.519(2)
_cell_length_c                   6.7336(4)
_cell_measurement_reflns_used    1205
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.1397
_cell_measurement_theta_min      1.9978
_cell_volume                     982.51(14)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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   59.00   98.00   1.0000   11.2700
omega____ theta____ kappa____ phi______ frames
    -       24.0786  178.0000 -120.0000 39

  2 omega  -49.00   62.00   1.0000   11.2700
omega____ theta____ kappa____ phi______ frames
    -       24.0786  -19.0000  -60.0000 111

  3 omega   -7.00   -5.00   1.0000   11.2700
omega____ theta____ kappa____ phi______ frames
    -       24.0786  -99.0000 -101.0000 2
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0148444000
_diffrn_orient_matrix_UB_12      -0.0146958000
_diffrn_orient_matrix_UB_13      -0.0784075000
_diffrn_orient_matrix_UB_21      0.0509083000
_diffrn_orient_matrix_UB_22      -0.0163258000
_diffrn_orient_matrix_UB_23      0.0744052000
_diffrn_orient_matrix_UB_31      -0.1385986000
_diffrn_orient_matrix_UB_32      -0.0075663000
_diffrn_orient_matrix_UB_33      -0.0085488000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.878
_diffrn_reflns_Laue_measured_fraction_max 0.717
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3485
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.717
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.210
_diffrn_reflns_theta_min         2.670
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76538
_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    1.395
_exptl_crystal_F_000             436.0
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.6655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1850
_reflns_number_total             2291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00708b2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 7225700--7225708.cif.'
_cod_original_cell_volume        982.53(14)
_cod_database_code               7225707
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 81.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=1-FVAR(1)
 Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C8(H8A,H8B), C4(H4A,H4B), C7A(H7AA,H7AB), C7B(H7BA,
 H7BB)
;
_olex2_date_sample_data_collection 1384406396.26
_olex2_submission_special_instructions 'No special instructions were received'