Structure determination of liquid molecules by encapsulation in an aromatic cavity with hydrogen bonding and enhanced C–H⋯π interactions
Qin, Shu-Qin; Xu, Wei; Ye, Wen-Cai; Jiang, Ren-Wang; CrystEngComm  (2022) –; doi:10.1039/D2CE01033J

data_7245785
_publ_section_title
;
 Structure determination of liquid molecules by encapsulation in an
 aromatic cavity with hydrogen bonding and enhanced C--H&#x22EF;\p
 interactions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01033J
_journal_year                    2022
_chemical_formula_moiety         'C5 H3 O3 S, C H6 N3, 2(H2 O)'
_chemical_formula_sum            'C6 H13 N3 O5 S'
_chemical_formula_weight         239.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-18
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-23 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                92.107(12)
_cell_angle_beta                 94.692(12)
_cell_angle_gamma                112.190(16)
_cell_formula_units_Z            2
_cell_length_a                   7.5403(12)
_cell_length_b                   8.1374(15)
_cell_length_c                   9.2100(11)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.9260
_cell_measurement_theta_min      6.3440
_cell_volume                     520.10(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  51.00   1.00    1.00    --   40.73 -99.00 -60.00   50
  2  \w     32.00  68.00   1.00    1.00    --   40.73-125.00-120.00   36
  3  \w      5.00  33.00   1.00    1.00    --   40.73-104.00-133.00   28
  4  \w     44.00 127.00   1.00    1.20    --  107.58 -30.00-150.00   83
  5  \w     80.00 177.00   1.00    1.20    --  107.58  30.00-180.00   97
  6  \w     96.00 121.00   1.00    1.20    --  107.58 125.00-120.00   25
  7  \w    101.00 163.00   1.00    1.20    --  107.58  30.00  60.00   62
  8  \w     69.00 110.00   1.00    1.20    --  107.58 -95.00  60.00   41
  9  \w     51.00  95.00   1.00    1.20    --  107.58 -95.00 150.00   44
 10  \w     50.00 128.00   1.00    1.20    --  107.58 -45.00 120.00   78
 11  \w     52.00 127.00   1.00    1.20    --  107.58 -45.00   0.00   75
 12  \w     46.00  94.00   1.00    1.00    --   40.73-125.00  30.00   48
 13  \w     29.00  74.00   1.00    1.20    --  107.58 -95.00  30.00   45
 14  \w     46.00 114.00   1.00    1.20    --  107.58-125.00  30.00   68
 15  \w     69.00 132.00   1.00    1.20    --  107.58 -77.00-180.00   63
 16  \w   -114.00 -24.00   1.00    1.00    --  -40.73 -38.00 -30.00   90
 17  \w   -112.00 -19.00   1.00    1.00    --  -40.73 -38.00  60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0649820000
_diffrn_orient_matrix_UB_12      0.2014782000
_diffrn_orient_matrix_UB_13      -0.0161557000
_diffrn_orient_matrix_UB_21      -0.0305427000
_diffrn_orient_matrix_UB_22      0.0287852000
_diffrn_orient_matrix_UB_23      0.1608370000
_diffrn_orient_matrix_UB_31      0.2099043000
_diffrn_orient_matrix_UB_32      0.0246409000
_diffrn_orient_matrix_UB_33      0.0468001000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3166
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.535
_diffrn_reflns_theta_min         4.831
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1298P)^2^+1.5729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1669
_reflns_number_total             1998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01033j2.cif
_cod_data_source_block           GNPS
_cod_database_code               7245785
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5)
2.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B)
;
_shelx_res_checksum              76820
_shelx_hkl_checksum              10437
_olex2_date_sample_data_collection 2020-10-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.397