Ag-Induced metallogel based on cyclooctatetrathiophene: structural characterization and stimuli-responsive properties.
Tian, Yu; Wang, Chenglong; Wang, Guangxia; Xu, Li; Wang, Hua; Soft matter 17 (2021) 341–345; doi:10.1039/d0sm01957g

data_1559863
_publ_section_title
;
 Ag-Induced metallogel based on cyclooctatetrathiophene: structural
 characterization and stimuli-responsive properties.
;
_journal_issue                   2
_journal_name_full               'Soft matter'
_journal_page_first              341
_journal_page_last               345
_journal_paper_doi               10.1039/d0sm01957g
_journal_volume                  17
_journal_year                    2021
_chemical_formula_moiety         'C32 H30 N2 S4 Si2'
_chemical_formula_sum            'C32 H30 N2 S4 Si2'
_chemical_formula_weight         627.00
_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     direct
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2020-07-20 deposited with the CCDC.	2020-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                86.414(5)
_cell_angle_beta                 81.109(6)
_cell_angle_gamma                77.472(6)
_cell_formula_units_Z            4
_cell_length_a                   10.1836(8)
_cell_length_b                   16.2598(12)
_cell_length_c                   23.1451(14)
_cell_measurement_reflns_used    5728
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.7590
_cell_measurement_theta_min      3.9030
_cell_volume                     3694.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.8662
_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    -25.00  34.00   0.50    3.00    --   -1.40  57.00 -30.00  118
  2  \w     17.00  88.00   0.50    3.00    --   -1.40  49.00 146.00  142
  3  \w    -21.00  40.00   0.50    3.00    --   -1.40  38.00 -60.00  122
  4  \w    -46.00 -21.00   0.50    3.00    --   -1.40 -77.00 -60.00   50
  5  \w    -23.00   4.00   0.50    3.00    --   -1.40  49.00 146.00   54
  6  \w    -31.00  -5.00   0.50    3.00    --   -1.40 -82.00  30.00   52
  7  \w    -29.00   9.00   0.50    3.00    --   -1.40 -82.00 -30.00   76
  8  \w    -32.00  11.00   0.50    3.00    --   -1.40 -82.00 150.00   86
  9  \w    -33.00  17.00   0.50    3.00    --   -1.40 -82.00-180.00  100
 10  \w    -71.00 -45.00   0.50    3.00    --    1.70 -38.00  90.00   52
 11  \w     -8.00  17.00   0.50    3.00    --    1.70 -57.00 150.00   50
 12  \w    -79.00 -50.00   0.50    3.00    --    1.70 -57.00 150.00   58
 13  \w    -33.00  33.00   0.50    3.00    --    1.70 -82.00  90.00  132
 14  \w    -23.00   2.00   0.50    3.00    --    1.70 -82.00 -90.00   50
 15  \w    -65.00 -39.00   0.50    3.00    --    1.70 -38.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0243247000
_diffrn_orient_matrix_UB_12      0.0436859000
_diffrn_orient_matrix_UB_13      -0.0052969000
_diffrn_orient_matrix_UB_21      -0.0448889000
_diffrn_orient_matrix_UB_22      -0.0094693000
_diffrn_orient_matrix_UB_23      -0.0179756000
_diffrn_orient_matrix_UB_31      -0.0509222000
_diffrn_orient_matrix_UB_32      0.0007861000
_diffrn_orient_matrix_UB_33      0.0247354000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1207
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89991
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.623
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         14336
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0805
_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^)+(0.0955P)^2^+3.4245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.2044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9454
_reflns_number_total             14336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sm01957g2.cif
_cod_data_source_block           exp_791-sr
_cod_depositor_comments
'Adding full bibliography for 1559863--1559864.cif.'
_cod_database_code               1559863
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.950
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.005
Uanis(C17) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.008
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C14(H14), C16(H16), C21(H21), C22(H22), C23(H23),
 C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C42(H42), C44(H44), C46(H46),
  C48(H48), C53(H53), C54(H54), C55(H55), C56(H56), C61(H61), C62(H62),
 C63(H63), C64(H64)
3.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C25(H25a,H25b,
 H25c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C49(H49a,H49b,H49c), C50(H50a,
 H50b,H50c), C51(H51a,H51b,H51c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c),
 C59(H59a,H59b,H59c)
;
_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 2.061
_oxdiff_exptl_absorpt_empirical_full_min 0.569