High current density electrodeposition of silver from silver-containing liquid metal salts with pyridine-N-oxide ligands.
Sniekers, Jeroen; Brooks, Neil R.; Schaltin, Stijn; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1589–1598; doi:10.1039/c3dt52416g

data_7028388
_publ_section_title
;
 High current density electrodeposition of silver from silver-containing
 liquid metal salts with pyridine-N-oxide ligands.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1589
_journal_page_last               1598
_journal_paper_doi               10.1039/c3dt52416g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C11 H13 Ag N2 O5 S'
_chemical_formula_sum            'C11 H13 Ag N2 O5 S'
_chemical_formula_weight         393.16
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.866(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6002(2)
_cell_length_b                   6.90176(12)
_cell_length_c                   17.1007(4)
_cell_measurement_reflns_used    3386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0130
_cell_measurement_theta_min      3.6320
_cell_volume                     1323.29(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8547
_diffrn_measurement_details
;
  1 omega  -17.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -99.0000  -30.0000 33

  2 omega  -88.00   44.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513    0.0000 -150.0000 132

  3 omega  -26.00   26.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513   57.0000 -120.0000 52
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0452835000
_diffrn_orient_matrix_UB_12      0.0511630000
_diffrn_orient_matrix_UB_13      0.0124651000
_diffrn_orient_matrix_UB_21      0.0270019000
_diffrn_orient_matrix_UB_22      -0.0251386000
_diffrn_orient_matrix_UB_23      0.0407820000
_diffrn_orient_matrix_UB_31      0.0349925000
_diffrn_orient_matrix_UB_32      0.0855496000
_diffrn_orient_matrix_UB_33      0.0044740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5428
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+0.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0444
_reflns_number_gt                2504
_reflns_number_total             2707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52416g.txt
_cod_data_source_block           kb2015
_cod_original_cell_volume        1323.28(4)
_cod_database_code               7028388
_chemical_oxdiff_formula         'Ag C15 H15 N3 O3 C H3 S O3'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C19(H19), C17(H17), C18(H18), C14(H14), C20(H20),
 C11(H11), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;