Hybrid interaction network of guanidinium-biphenyldisulfonic acid for the structure determination of liquid molecules
Qin, Shu-Qin; Gan, Qian-Ying; Xu, Wei; Jiang, Ren-Wang; CrystEngComm  (2022) –; doi:10.1039/D2CE00228K

data_7244801
_publ_section_title
;
 Hybrid interaction network of guanidinium-biphenyldisulfonic acid for the
 structure determination of liquid molecules
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00228K
_journal_year                    2022
_chemical_formula_moiety         'C12 H8 O6 S2, C8 H8 O2, 2(C H6 N3)'
_chemical_formula_sum            'C22 H28 N6 O8 S2'
_chemical_formula_weight         568.62
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-17 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                69.146(5)
_cell_angle_beta                 86.884(4)
_cell_angle_gamma                77.000(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4141(3)
_cell_length_b                   12.8303(7)
_cell_length_c                   15.1362(9)
_cell_measurement_reflns_used    5910
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.7840
_cell_measurement_theta_min      3.7600
_cell_volume                     1310.50(13)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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      9.00  49.00   1.00    1.00    --   40.73 -99.00 120.00   40
  2  \w     29.00 108.00   1.00    1.50    --  107.58 -94.00   0.00   79
  3  \w     65.00 138.00   1.00    1.50    --  107.58 -77.00  90.00   73
  4  \w     57.00 170.00   1.00    1.50    --  107.58  15.00  90.00  113
  5  \w    119.00 174.00   1.00    1.50    --  107.58 125.00  60.00   55
  6  \w     94.00 126.00   1.00    1.50    --  107.58 131.00  82.00   32
  7  \w     83.00 166.00   1.00    1.50    --  107.58  45.00 150.00   83
  8  \w     37.00  65.00   1.00    1.50    --  107.58 -94.00 150.00   28
  9  \w     32.00 114.00   1.00    1.50    --  107.58 -30.00 120.00   82
 10  \w     36.00 127.00   1.00    1.50    --  107.58 -61.00   0.00   91
 11  \w     47.00  96.00   1.00    1.00    --   40.73-125.00-150.00   49
 12  \w     36.00 118.00   1.00    1.50    --  107.58-125.00 -60.00   82
 13  \w    -25.00  51.00   1.00    1.00    --   40.73 -37.00 150.00   76
 14  \w    -28.00  -2.00   1.00    1.00    --  -40.73 125.00  30.00   26
 15  \w   -105.00 -30.00   1.00    1.00    --  -40.73 -37.00-120.00   75
 16  \w   -117.00 -15.00   1.00    1.00    --  -40.73 -77.00   0.00  102
 17  \w    108.00 133.00   1.00    1.50    --  107.58 125.00-120.00   25
;
_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      0.0591068000
_diffrn_orient_matrix_UB_12      -0.1209776000
_diffrn_orient_matrix_UB_13      0.0744431000
_diffrn_orient_matrix_UB_21      -0.0550014000
_diffrn_orient_matrix_UB_22      0.0487534000
_diffrn_orient_matrix_UB_23      0.0794988000
_diffrn_orient_matrix_UB_31      -0.1974716000
_diffrn_orient_matrix_UB_32      -0.0184315000
_diffrn_orient_matrix_UB_33      -0.0031875000
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8801
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.940
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82541
_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    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.4026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4704
_reflns_number_total             5127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00228k3.cif
_cod_data_source_block           1-k_2
_cod_database_code               7244801
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.96
_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 C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              59597
_shelx_hkl_checksum              30530
_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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.664