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_7244802
_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, 3(C10 H12 O), 2(C H6 N3)'
_chemical_formula_sum            'C44 H56 N6 O9 S2'
_chemical_formula_weight         877.06
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-06
_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                90
_cell_angle_beta                 94.659(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6608(5)
_cell_length_b                   10.9150(7)
_cell_length_c                   27.573(2)
_cell_measurement_reflns_used    3315
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.0820
_cell_measurement_theta_min      2.8310
_cell_volume                     2298.0(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_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 0.999
_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     -6.00  82.00   1.00    5.00    --   11.74  37.00  60.00   88
  2  \w    -50.00  40.00   1.00    5.00    --   11.74 -57.00-120.00   90
;
_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      0.0325803000
_diffrn_orient_matrix_UB_12      -0.0602927000
_diffrn_orient_matrix_UB_13      -0.0024481000
_diffrn_orient_matrix_UB_21      0.0061518000
_diffrn_orient_matrix_UB_22      0.0101396000
_diffrn_orient_matrix_UB_23      -0.0252197000
_diffrn_orient_matrix_UB_31      0.0868251000
_diffrn_orient_matrix_UB_32      0.0218512000
_diffrn_orient_matrix_UB_33      0.0049701000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9072
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.383
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44803
_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    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.074
_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     329
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0301P)^2^+6.4266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3409
_reflns_number_total             4031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00228k3.cif
_cod_data_source_block           c1b+i
_cod_database_code               7244802
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C4B-C8B
 1.5 with sigma of 0.02
 O1B-C7B
 1.45 with sigma of 0.02
 C8B-C9B
 1.33 with sigma of 0.02
 C9B-C10B
 1.52 with sigma of 0.02
 C1B-O1B
 1.48 with sigma of 0.02
 C5B-C4B \\sim C5B-C6B \\sim C6B-C1B \\sim C2B-C1B \\sim C2B-C3B \\sim C4B-C3B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O1B, C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O1B(0.5) C1B(0.5) C2B(0.5) H2B(0.5) C3B(0.5) H3B(0.5) C4B(0.5)
 C5B(0.5) H5B(0.5) C6B(0.5) H6B(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5)
 C8B(0.5) H8B(0.5) C9B(0.5) H9B(0.5) C10B(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A),
 C8A(H8A), C9A(H9A), C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C8B(H8B), C9B(H9B)
5.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2C,H2D), N3(H3C,H3D)
5.c Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C10A(H10A,H10B,H10C), C7B(H7BA,H7BB,H7BC), C10B(H10D,
 H10E,H10F)
;
_shelx_res_checksum              10003
_shelx_hkl_checksum              42700
_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 1.726
_oxdiff_exptl_absorpt_empirical_full_min 0.473