#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:44:48 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262565 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/19/7241975.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7241975
loop_
_publ_author_name
'Abe, Haruka'
'Kobayashi, Takahiro'
'Hoshino, Norihisa'
'Takeda, Takashi'
'Suzuki, Yasutaka'
'Kawamata, Jun'
'Akutagawa, Tomoyuki'
_publ_section_title
;
 Dynamic structural reconstruction of
 (guanidinium+)2(benzene-1,4-disulfonate2−) host crystal by guest
 adsorption
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1149
_journal_page_last               1157
_journal_paper_doi               10.1039/D0CE01616K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '2(C H6 N3)+, (C6 H4 O6 S2)2-, 3(C4 H4 S)'
_chemical_formula_sum            'C20 H28 N6 O6 S5'
_chemical_formula_weight         608.78
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-29 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.488(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6230(3)
_cell_length_b                   16.8745(8)
_cell_length_c                   11.8090(6)
_cell_measurement_reflns_used    10020
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.75
_cell_volume                     1518.99(12)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2011)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2011)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2011)'
_computing_molecular_graphics    'Mercury (CCDC, 2016)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16375
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         4.570
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       needle
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1849P)²+1.1864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2899
_refine_ls_wR_factor_ref         0.3084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2043
_reflns_number_total             2751
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01616k2.cif
_cod_data_source_block           p21n_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7241968--7241975.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241975
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.697
_shelx_estimated_absorpt_t_max   0.962
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.46946(15) 0.18512(7) 0.01995(10) 0.0567(4) Uani 1 1 d . . . . .
O1 O 0.4665(4) 0.2162(2) -0.0946(3) 0.0608(8) Uani 1 1 d . . . . .
O2 O 0.6264(4) 0.2084(2) 0.0826(3) 0.0603(9) Uani 1 1 d . . . . .
O3 O 0.3101(4) 0.2019(2) 0.0813(3) 0.0606(9) Uani 1 1 d . . . . .
N1 N 0.4676(5) 0.2778(2) 0.4809(3) 0.0587(10) Uani 1 1 d . . . . .
H1 H 0.567968 0.284881 0.516852 0.070 Uiso 1 1 calc R U . . .
H2 H 0.368034 0.283974 0.517081 0.070 Uiso 1 1 calc R U . . .
N2 N 0.6166(5) 0.2485(2) 0.3175(4) 0.0656(11) Uani 1 1 d . . . . .
H3 H 0.717064 0.255561 0.353363 0.079 Uiso 1 1 calc R U . . .
H4 H 0.615749 0.235246 0.245382 0.079 Uiso 1 1 calc R U . . .
N3 N 0.3136(5) 0.2448(2) 0.3188(4) 0.0616(11) Uani 1 1 d . . . . .
H5 H 0.214401 0.249406 0.355725 0.074 Uiso 1 1 calc R U . . .
H6 H 0.312371 0.231502 0.246693 0.074 Uiso 1 1 calc R U . . .
C1 C 0.4082(6) 0.0335(3) 0.0920(4) 0.0594(12) Uani 1 1 d . . . . .
H7 H 0.346613 0.056781 0.153167 0.071 Uiso 1 1 calc R U . . .
C2 C 0.5720(6) 0.0479(3) -0.0845(4) 0.0582(12) Uani 1 1 d . . . . .
H8 H 0.619853 0.081184 -0.141319 0.070 Uiso 1 1 calc R U . . .
C3 C 0.4823(5) 0.0811(3) 0.0058(4) 0.0523(11) Uani 1 1 d . . . . .
C4 C 0.4663(6) 0.2578(3) 0.3721(4) 0.0543(11) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 O1 112.9(2) . . ?
O3 S1 O2 112.5(2) . . ?
O1 S1 O2 112.5(2) . . ?
O3 S1 C3 106.8(2) . . ?
O1 S1 C3 105.7(2) . . ?
O2 S1 C3 105.7(2) . . ?
C4 N1 H1 120.0 . . ?
C4 N1 H2 120.0 . . ?
H1 N1 H2 120.0 . . ?
C4 N2 H3 120.0 . . ?
C4 N2 H4 120.0 . . ?
H3 N2 H4 120.0 . . ?
C4 N3 H5 120.0 . . ?
C4 N3 H6 120.0 . . ?
H5 N3 H6 120.0 . . ?
C2 C1 C3 118.1(4) 3_655 . ?
C2 C1 H7 120.9 3_655 . ?
C3 C1 H7 120.9 . . ?
C1 C2 C3 120.2(4) 3_655 . ?
C1 C2 H8 119.9 3_655 . ?
C3 C2 H8 119.9 . . ?
C2 C3 C1 121.6(5) . . ?
C2 C3 S1 120.1(4) . . ?
C1 C3 S1 118.2(4) . . ?
N1 C4 N2 120.0(4) . . ?
N1 C4 N3 119.8(4) . . ?
N2 C4 N3 120.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O3 1.448(3) . ?
S1 O1 1.451(4) . ?
S1 O2 1.455(4) . ?
S1 C3 1.766(5) . ?
N1 C4 1.328(6) . ?
N1 H1 0.8800 . ?
N1 H2 0.8800 . ?
N2 C4 1.330(6) . ?
N2 H3 0.8800 . ?
N2 H4 0.8800 . ?
N3 C4 1.337(6) . ?
N3 H5 0.8800 . ?
N3 H6 0.8800 . ?
C1 C2 1.385(7) 3_655 ?
C1 C3 1.419(6) . ?
C1 H7 0.9500 . ?
C2 C3 1.389(6) . ?
C2 H8 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C1 -0.3(8) 3_655 . . . ?
C1 C2 C3 S1 175.9(4) 3_655 . . . ?
C2 C1 C3 C2 0.3(8) 3_655 . . . ?
C2 C1 C3 S1 -176.0(4) 3_655 . . . ?
O3 S1 C3 C2 153.1(4) . . . . ?
O1 S1 C3 C2 32.5(4) . . . . ?
O2 S1 C3 C2 -86.9(4) . . . . ?
O3 S1 C3 C1 -30.6(4) . . . . ?
O1 S1 C3 C1 -151.1(4) . . . . ?
O2 S1 C3 C1 89.4(4) . . . . ?
