Complex formation of silver(I) ions with a glucosinolate derivative: structural and mechanistic insights into myrosinase-mimicking C-S bond cleavage.
Alba, Laurenzo D. V.; Hatanaka, Tsubasa; Franco, Francisco C.; Nojiri, Masaki; Noel, Marissa G.; Funahashi, Yasuhiro; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8292–8296; doi:10.1039/d1dt00695a

data_7707259
_publ_section_title
;
 Complex formation of silver(I) ions with a glucosinolate derivative:
 structural and mechanistic insights into myrosinase-mimicking C-S bond
 cleavage.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8292
_journal_page_last               8296
_journal_paper_doi               10.1039/d1dt00695a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C18 H24 K N O13 S2'
_chemical_formula_sum            'C18 H24 K N O13 S2'
_chemical_formula_weight         565.60
_chemical_name_systematic        O-acetylsinigrin
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-30 deposited with the CCDC.	2021-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.321(2)
_cell_angle_beta                 110.969(2)
_cell_angle_gamma                97.225(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0195(2)
_cell_length_b                   12.3261(4)
_cell_length_c                   12.5871(3)
_cell_measurement_reflns_used    14835
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.0900
_cell_measurement_theta_min      1.7860
_cell_volume                     1251.57(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.837
_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     -7.00  29.00   0.50    1.84    --   12.33  57.00 150.00   72
  2  \w     60.00  85.00   0.50    1.84    --   12.33  57.00 150.00   50
  3  \w    -47.00 -20.00   0.50    1.84    --   12.33 -19.00-180.00   54
  4  \w    -11.00  52.00   0.50    1.84    --   12.33 -99.00  60.00  126
  5  \w      9.00  46.00   0.50    1.84    --   12.33-100.00 116.00   74
  6  \w    -76.00  16.00   0.50    1.84    --   -7.01 -57.00 150.00  184
  7  \w    -46.00   3.00   0.50    1.84    --   -7.01 100.00-137.00   98
  8  \w    -29.00  63.00   0.50    1.84    --   -7.01  57.00 -60.00  184
  9  \w    -17.00  14.00   0.50    1.84    --   -7.01 -77.00-120.00   62
 10  \w    -65.00 -26.00   0.50    1.84    --   -7.01 -77.00-120.00   78
 11  \w     -1.00  24.00   0.50    1.82    --   -7.17 -19.00  30.00   50
 12  \w    -45.00 -20.00   0.50    1.84    --   -7.17 100.00-137.00   50
 13  \w    -24.00  22.00   0.50    1.84    --   -7.17 -77.00-150.00   92
 14  \w    -73.00 -47.00   0.50    1.84    --   -7.17 -77.00-150.00   52
 15  \w    -11.00  16.00   0.50    1.84    --   12.33 -99.00 -30.00   54
 16  \w    -10.00  88.00   0.50    1.84    --   12.33  37.00  60.00  196
 17  \w    -15.00  11.00   0.50    1.84    --   12.33  77.00  60.00   52
 18  \w     21.00  52.00   0.50    1.84    --   12.33 -99.00 -30.00   62
 19  \w      5.00  90.00   0.50    1.84    --   12.33  37.00 -30.00  170
 20  \w     46.00  87.00   0.50    1.84    --   12.33  77.00  60.00   82
 21  \w     24.00  60.00   0.50    1.84    --   14.00-110.00 164.62   72
 22  \w     22.00  48.00   0.50    1.84    --   14.00 -87.00-166.39   52
 23  \w     17.00  57.00   0.50    1.84    --   14.00-106.00 -92.47   80
 24  \w     -4.00  21.00   0.50    1.84    --   12.33-100.00 116.00   50
 25  \w     27.00  52.00   0.50    1.84    --   12.33-100.00 116.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0124554000
_diffrn_orient_matrix_UB_12      0.0562017000
_diffrn_orient_matrix_UB_13      0.0065318000
_diffrn_orient_matrix_UB_21      -0.0451688000
_diffrn_orient_matrix_UB_22      -0.0102639000
_diffrn_orient_matrix_UB_23      0.0343236000
_diffrn_orient_matrix_UB_31      0.0723741000
_diffrn_orient_matrix_UB_32      0.0185883000
_diffrn_orient_matrix_UB_33      0.0518286000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37676
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.125
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 4138 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         12544
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0441
_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/[\s^2^(Fo^2^)+(0.0556P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.720
_reflns_number_gt                10295
_reflns_number_total             12544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00695a2.cif
_cod_data_source_block           alba200805
_cod_depositor_comments
'Adding full bibliography for 7707258--7707259.cif.'
_cod_database_code               7707259
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H28 K N O13 S2 '
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.825
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C2B(H2B), C2(H2), C1B(H1B), C1(H1), C4(H4), C3B(H3B), C4B(H4B),
 C5B(H5B), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C6B(H6BA,H6BB), C6(H6A,H6B), C14B(H14C,H14D)
2.c Aromatic/amide H refined with riding coordinates:
 C15B(H15B), C15(H15)
2.d X=CH2 refined with riding coordinates:
 C16B(H16A,H16B), C16(H16C,H16D)
2.e Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C31B(H31A,H31B,H31C), C31(H31D,
 H31E,H31F), C28(H28A,H28B,H28C), C28B(H28D,H28E,H28F), C25B(H25A,H25B,H25C),
 C25(H25D,H25E,H25F)
;
_shelx_res_checksum              28746
_olex2_exptl_crystal_mounting_method loop
_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 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.604