Vesicles, fibres, films and crystals: A low-molecular-weight-gelator [Au(6-thioguanosine)<sub>2</sub>]Cl which exhibits a co-operative anion-induced transition from vesicles to a fibrous metallo-hydrogel.
McGarry, Liam F.; El-Zubir, Osama; Waddell, Paul G.; Cucinotta, Fabio; Houlton, Andrew; Horrocks, Benjamin R.; Soft matter 19 (2023) 8386–8402; doi:10.1039/d3sm01006f

data_1570154
_publ_section_title
;
 Vesicles, fibres, films and crystals: A low-molecular-weight-gelator
 [Au(6-thioguanosine)<sub>2</sub>]Cl which exhibits a co-operative
 anion-induced transition from vesicles to a fibrous metallo-hydrogel.
;
_journal_issue                   43
_journal_name_full               'Soft matter'
_journal_page_first              8386
_journal_page_last               8402
_journal_paper_doi               10.1039/d3sm01006f
_journal_volume                  19
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C20 H24 Au N10 O8 S2, Cl, 3(H2 O)'
_chemical_formula_sum            'C20 H32 Au Cl N10 O11 S2'
_chemical_formula_weight         885.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-17 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.962(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3414(3)
_cell_length_b                   13.5389(5)
_cell_length_c                   14.8400(6)
_cell_measurement_reflns_used    5062
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66.7520
_cell_measurement_theta_min      4.4130
_cell_volume                     1442.98(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -99.00 -18.00   1.00    2.00    --  -41.59 125.00 -30.00   81
  2  \w    -37.00  75.00   1.00    2.00    --   41.59 -77.00  90.00  112
  3  \w     15.00 117.00   1.00    2.00    --   41.59  38.00 -30.00  102
  4  \w     12.00 116.00   1.00    2.00    --   41.59  57.00-150.00  104
  5  \w     66.00 168.00   1.00    8.00    --   93.50  45.00 -90.00  102
  6  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00 120.00   74
  7  \w     63.00 168.00   1.00    8.00    --   93.50  61.00-180.00  105
  8  \w     19.00  96.00   1.00    8.00    --   93.50-125.00-150.00   77
  9  \w     63.00 171.00   1.00    8.00    --   93.50  30.00  30.00  108
 10  \w     73.00 168.00   1.00    8.00    --   93.50 125.00  60.00   95
 11  \w     66.00 168.00   1.00    8.00    --   93.50  45.00 -30.00  102
 12  \w      9.00  83.00   1.00    8.00    --   93.50 -94.00-150.00   74
 13  \w     60.00 172.00   1.00    8.00    --   93.50  77.00 120.00  112
 14  \w     19.00  96.00   1.00    8.00    --   93.50-125.00  90.00   77
 15  \w     19.00 124.00   1.00    8.00    --   93.50 -61.00-120.00  105
 16  \w     60.00 172.00   1.00    8.00    --   93.50  77.00-180.00  112
 17  \w     31.00  57.00   1.00    8.00    --   93.50 -89.00  98.00   26
 18  \w     63.00 111.00   1.00    8.00    --   93.50 -89.00  98.00   48
 19  \w     92.00 145.00   1.00    8.00    --   93.50  61.00-150.00   53
 20  \w    110.00 168.00   1.00    8.00    --   93.50 125.00 -30.00   58
 21  \w    116.00 147.00   1.00    8.00    --   93.50 125.00 -60.00   31
 22  \w     35.00  86.00   1.00    8.00    --   93.50-125.00 -90.00   51
 23  \w     65.00 118.00   1.00    8.00    --   93.50  61.00 150.00   53
 24  \w     19.00  58.00   1.00    8.00    --   93.50 -45.00 -90.00   39
 25  \w     75.00 108.00   1.00    8.00    --   93.50 -45.00 -90.00   33
 26  \w     58.00 124.00   1.00    8.00    --   93.50 -61.00  30.00   66
 27  \w    106.00 167.00   1.00    8.00    --   93.50  45.00 -60.00   61
 28  \w     75.00 123.00   1.00    8.00    --   93.50 -30.00  30.00   48
 29  \w     54.00  83.00   1.00    8.00    --   93.50 -94.00 -60.00   29
 30  \w     19.00  49.00   1.00    8.00    --   93.50 -30.00  30.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0409121000
_diffrn_orient_matrix_UB_12      0.0945616000
_diffrn_orient_matrix_UB_13      0.0500882000
_diffrn_orient_matrix_UB_21      0.1119015000
_diffrn_orient_matrix_UB_22      -0.0416167000
_diffrn_orient_matrix_UB_23      0.0915595000
_diffrn_orient_matrix_UB_31      0.1782653000
_diffrn_orient_matrix_UB_32      0.0477249000
_diffrn_orient_matrix_UB_33      -0.0194326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20519
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.108
_diffrn_reflns_theta_max         67.108
_diffrn_reflns_theta_min         4.466
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (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    2.037
_exptl_crystal_description       needle
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 1956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.042(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5112
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                4572
_reflns_number_total             5112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sm01006f2.cif
_cod_data_source_block           aho200014
_cod_depositor_comments          'Adding full bibliography for 1570154.cif.'
_cod_database_code               1570154
_chemical_oxdiff_formula         'C20 H24 N120 O6 S2 Au1'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H7'_$1-O12_$3
 2.1 with sigma of 0.02
 H10D-N7_$4
 2 with sigma of 0.02
 H10C-O3'
 2 with sigma of 0.02
 H11C-O2'_$5
 2 with sigma of 0.02
 H11D-O10_$6
 2 with sigma of 0.02
 H3'-O12_$7
 2 with sigma of 0.02
3.a Free rotating group:
 O10(H10C,H10D), O11(H11C,H11D), O12(H12A,H12B)
3.b Ternary CH refined with riding coordinates:
 C1'(H1'), C2'(H2'A), C3'(H3'A), C4'(H4'), C6'(H6'), C7'(H7'A), C8'(H8'A),
 C9'(H9'A)
3.c Secondary CH2 refined with riding coordinates:
 C5'(H5'A,H5'B), C10'(H10A,H10B)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C17(H17)
3.e X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N11(H11A,H11B)
3.f Idealised tetrahedral OH refined as rotating group:
 O2'(H2'), O3'(H3'), O5'(H5'), O7'(H7'), O8'(H8'), O9'(H9')
;
_shelx_res_checksum              54637
_shelx_hkl_checksum              70240
_shelx_shelxl_version_number     2018/3
_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 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.752