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_7244805
_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, C11 H14 O2, 2(C H6 N3)'
_chemical_formula_sum            'C25 H34 N6 O8 S2'
_chemical_formula_weight         610.70
_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
_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                101.192(4)
_cell_angle_beta                 90.032(4)
_cell_angle_gamma                93.056(4)
_cell_formula_units_Z            1
_cell_length_a                   6.1959(3)
_cell_length_b                   7.1931(3)
_cell_length_c                   14.6132(6)
_cell_measurement_reflns_used    4375
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.6390
_cell_measurement_theta_min      6.1570
_cell_volume                     637.94(5)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       multi-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5959
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.737
_diffrn_reflns_theta_min         3.083
_exptl_absorpt_coefficient_mu    2.458
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.331
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.400
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0959
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2744
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5306
_reflns_number_total             5959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00228k3.cif
_cod_data_source_block           12345
_cod_database_code               7244805
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.403(3)
 0.597(3)
2. 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
3. Restrained distances
 C2-O4
 1.38 with sigma of 0.02
 C4-C7
 1.5 with sigma of 0.02
 O5-C1
 1.38 with sigma of 0.02
 O4-C11
 1.4 with sigma of 0.02
 C6-O5
 2.3 with sigma of 0.02
 O4-C3
 2.3 with sigma of 0.02
 O5-C10
 1.4 with sigma of 0.02
 C8-C9
 1.55 with sigma of 0.02
 C7-C9
 2.5 with sigma of 0.02
 C7-C8
 1.37 with sigma of 0.02
 C11-C3
 2.4 with sigma of 0.02
 C6B-C1A \\sim C6B-C5B \\sim C5B-C4A \\sim C3B-C4A \\sim C3B-C2B \\sim C2B-C1A
 with sigma of 0.02
 C2A-C1A \\sim C2A-C3A \\sim C3A-C4A \\sim C5A-C4A \\sim C6A-C5A \\sim C6A-C1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1A, C2B, C3B, C4A, C5B, C6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O4, O5, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=1-
 FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=FVAR(1)
 Fixed Sof: O4(0.5) O5(0.5) C3(0.5) H3(0.5) C4(0.5) C5(0.5) H5(0.5) C6(0.5)
 H6(0.5) C1(0.5) C2(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C2A(H2A), C2B(H2B), C3A(H3A),
 C3B(H3B), C5A(H5A), C5B(H5B), C6A(H6A), C6B(H6B)
7.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C1,C2)
7.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2C,H2D), N3(H3C,H3D)
7.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              70690
_shelx_hkl_checksum              59218
_olex2_submission_special_instructions 'No special instructions were received'