#------------------------------------------------------------------------------
#$Date: 2020-06-05 12:51:43 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252709 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/62/7126288.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_7126288
loop_
_publ_author_name
'Chakraborty, Poulami'
'Das, Bikash'
'Pal, Pulak'
'Datta, Subhadeep'
'Bera, Sourabh'
'Dastidar, Parthasarathi'
_publ_section_title
;
 A supramolecular hydrogel derived from a simple organic salt capable of
 proton conduction.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5251
_journal_page_last               5254
_journal_paper_doi               10.1039/d0cc01467b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C10 H7 O3 S, C7 H10 N'
_chemical_formula_sum            'C17 H17 N O3 S'
_chemical_formula_weight         315.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-09 deposited with the CCDC.	2020-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.376(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.352(19)
_cell_length_b                   10.823(12)
_cell_length_c                   9.736(11)
_cell_measurement_reflns_used    6727
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.28
_cell_volume                     1661(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21873
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.862
_diffrn_reflns_theta_min         1.291
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1487 before and 0.0403 after correction. The Ratio of minimum to maximum transmission is 0.9267. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0399
_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)+(0.0820P)²+0.1315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2877
_reflns_number_total             4088
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc01467b3.cif
_cod_data_source_block           N2SBA
_cod_depositor_comments
'Adding full bibliography for 7126286--7126291.cif.'
_cod_database_code               7126288
_shelx_shelxl_version_number     2016/6
_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_max   0.964
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C17(H17), C8(H8), C13(H13), C3(H3), C7(H7), C16(H16), C14(H14),
 C15(H15), C6(H6), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.38197(2) 0.60048(4) 0.15596(4) 0.05132(16) Uani 1 1 d . . . . .
O2 O 0.41672(8) 0.72546(12) 0.16281(16) 0.0691(4) Uani 1 1 d . . . . .
O3 O 0.39158(9) 0.53830(15) 0.02729(16) 0.0808(4) Uani 1 1 d . . . . .
N1 N 0.51982(8) 0.80490(14) 0.43340(17) 0.0603(4) Uani 1 1 d . . . . .
H1A H 0.546156 0.871703 0.413146 0.090 Uiso 1 1 calc GR . . . .
H1B H 0.481417 0.827370 0.478460 0.090 Uiso 1 1 calc GR . . . .
H1C H 0.494178 0.765899 0.353045 0.090 Uiso 1 1 calc GR . . . .
O1 O 0.41570(8) 0.53003(18) 0.28480(17) 0.0969(6) Uani 1 1 d . . . . .
C2 C 0.23093(9) 0.55447(15) 0.21987(16) 0.0478(4) Uani 1 1 d . . . . .
H2 H 0.262630 0.504221 0.292026 0.057 Uiso 1 1 calc R . . . .
C1 C 0.27009(9) 0.61613(14) 0.13268(17) 0.0457(3) Uani 1 1 d . . . . .
C9 C 0.14111(10) 0.56665(16) 0.20098(17) 0.0507(4) Uani 1 1 d . . . . .
C12 C 0.64688(10) 0.67167(16) 0.45202(17) 0.0514(4) Uani 1 1 d . . . . .
C10 C 0.09439(10) 0.64680(18) 0.0909(2) 0.0594(4) Uani 1 1 d . . . . .
C17 C 0.71375(11) 0.74573(18) 0.4352(2) 0.0618(5) Uani 1 1 d . . . . .
H17 H 0.720077 0.825841 0.471034 0.074 Uiso 1 1 calc R . . . .
C8 C 0.22329(11) 0.69360(18) 0.0205(2) 0.0635(5) Uani 1 1 d . . . . .
H8 H 0.250661 0.733811 -0.039190 0.076 Uiso 1 1 calc R . . . .
C13 C 0.63887(11) 0.55143(18) 0.39778(19) 0.0601(4) Uani 1 1 d . . . . .
H13 H 0.594397 0.502028 0.408315 0.072 Uiso 1 1 calc R . . . .
C3 C 0.09713(12) 0.5025(2) 0.2868(2) 0.0690(5) Uani 1 1 d . . . . .
H3 H 0.126526 0.449352 0.357875 0.083 Uiso 1 1 calc R . . . .
C7 C 0.13768(11) 0.7083(2) 0.0013(2) 0.0740(6) Uani 1 1 d . . . . .
H7 H 0.107347 0.759215 -0.071438 0.089 Uiso 1 1 calc R . . . .
C11 C 0.58325(12) 0.7203(2) 0.5268(2) 0.0704(5) Uani 1 1 d . . . . .
H11A H 0.553762 0.651336 0.555668 0.085 Uiso 1 1 calc R . . . .
H11B H 0.613091 0.764506 0.612090 0.085 Uiso 1 1 calc R . . . .
C16 C 0.77095(11) 0.6986(2) 0.3643(2) 0.0760(6) Uani 1 1 d . . . . .
H16 H 0.815147 0.747715 0.352063 0.091 Uiso 1 1 calc R . . . .
C14 C 0.69597(13) 0.5046(2) 0.3287(2) 0.0691(5) Uani 1 1 d . . . . .
H14 H 0.690139 0.424248 0.293594 0.083 Uiso 1 1 calc R . . . .
C15 C 0.76182(13) 0.5784(2) 0.3121(2) 0.0765(6) Uani 1 1 d . . . . .
H15 H 0.800320 0.547264 0.265722 0.092 Uiso 1 1 calc R . . . .
C6 C 0.00480(12) 0.6615(2) 0.0726(3) 0.0843(7) Uani 1 1 d . . . . .
H6 H -0.026151 0.713838 0.001971 0.101 Uiso 1 1 calc R . . . .
C5 C -0.03517(13) 0.5993(3) 0.1581(3) 0.0936(8) Uani 1 1 d . . . . .
H5 H -0.093101 0.610130 0.145675 0.112 Uiso 1 1 calc R . . . .
C4 C 0.01043(14) 0.5188(3) 0.2649(3) 0.0874(7) Uani 1 1 d . . . . .
H4 H -0.017871 0.476195 0.321431 0.105 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O2 S1 O3 109.58(10) . . ?
O2 S1 C1 106.85(8) . . ?
O3 S1 C1 105.81(8) . . ?
O1 S1 O2 113.20(11) . . ?
O1 S1 O3 113.35(14) . . ?
O1 S1 C1 107.54(8) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C11 N1 H1A 109.5 . . ?
C11 N1 H1B 109.5 . . ?
C11 N1 H1C 109.5 . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C9 120.50(15) . . ?
C9 C2 H2 119.8 . . ?
C2 C1 S1 120.45(12) . . ?
C2 C1 C8 121.21(16) . . ?
C8 C1 S1 118.33(13) . . ?
C10 C9 C2 118.41(15) . . ?
C3 C9 C2 122.68(17) . . ?
C3 C9 C10 118.91(17) . . ?
C17 C12 C11 120.98(19) . . ?
C13 C12 C17 119.14(18) . . ?
C13 C12 C11 119.88(17) . . ?
C9 C10 C6 118.96(18) . . ?
C7 C10 C9 119.19(16) . . ?
C7 C10 C6 121.84(18) . . ?
C12 C17 H17 120.2 . . ?
C16 C17 C12 119.6(2) . . ?
C16 C17 H17 120.2 . . ?
C1 C8 H8 120.2 . . ?
C7 C8 C1 119.52(17) . . ?
C7 C8 H8 120.2 . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.14(18) . . ?
C14 C13 H13 119.4 . . ?
C9 C3 H3 119.9 . . ?
C4 C3 C9 120.3(2) . . ?
C4 C3 H3 119.9 . . ?
C10 C7 H7 119.4 . . ?
C8 C7 C10 121.14(17) . . ?
C8 C7 H7 119.4 . . ?
N1 C11 C12 111.98(16) . . ?
N1 C11 H11A 109.2 . . ?
N1 C11 H11B 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C17 C16 H16 120.0 . . ?
C15 C16 C17 120.06(19) . . ?
C15 C16 H16 120.0 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C16 C15 H15 119.7 . . ?
C14 C15 C16 120.6(2) . . ?
C14 C15 H15 119.7 . . ?
C10 C6 H6 119.8 . . ?
C5 C6 C10 120.5(2) . . ?
C5 C6 H6 119.8 . . ?
C6 C5 H5 119.7 . . ?
C6 C5 C4 120.7(2) . . ?
C4 C5 H5 119.7 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
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 O2 1.462(2) . ?
S1 O3 1.4668(19) . ?
S1 O1 1.4465(18) . ?
S1 C1 1.791(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C11 1.497(3) . ?
C2 H2 0.9300 . ?
C2 C1 1.365(2) . ?
C2 C9 1.437(3) . ?
C1 C8 1.428(2) . ?
C9 C10 1.432(3) . ?
C9 C3 1.420(3) . ?
C12 C17 1.400(3) . ?
C12 C13 1.397(3) . ?
C12 C11 1.514(3) . ?
C10 C7 1.426(3) . ?
C10 C6 1.437(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.398(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.372(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.384(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.388(3) . ?
C7 H7 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C16 H16 0.9300 . ?
C16 C15 1.390(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.384(3) . ?
C15 H15 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.364(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.409(4) . ?
C4 H4 0.9300 . ?
