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_7028389
_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         'C15 H15 Ag N3 O3, C F3 O3 S'
_chemical_formula_sum            'C16 H15 Ag F3 N3 O6 S'
_chemical_formula_weight         542.24
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.9649(5)
_cell_length_b                   25.9649(5)
_cell_length_c                   11.8154(3)
_cell_measurement_reflns_used    12255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9700
_cell_measurement_theta_min      3.2970
_cell_volume                     7965.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 0.9981
_diffrn_measured_fraction_theta_max 0.8944
_diffrn_measurement_details
;
  1 omega   -8.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -99.0000   90.0000 30

  2 omega  -89.00  -25.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  154.0000  141.0000 64

  3 omega   -2.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701    0.0000  -90.0000 93

  4 omega  -70.00  -44.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513 -178.0000   30.0000 26

  5 omega   -3.00   38.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   38.0000   30.0000 41
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0202426000
_diffrn_orient_matrix_UB_12      0.0141466000
_diffrn_orient_matrix_UB_13      -0.0256817000
_diffrn_orient_matrix_UB_21      -0.0103845000
_diffrn_orient_matrix_UB_22      0.0232058000
_diffrn_orient_matrix_UB_23      0.0220563000
_diffrn_orient_matrix_UB_31      0.0151125000
_diffrn_orient_matrix_UB_32      -0.0030077000
_diffrn_orient_matrix_UB_33      0.0495257000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19449
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0195P)^2^+14.3198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0512
_reflns_number_gt                3749
_reflns_number_total             4065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52416g.txt
_cod_data_source_block           kb2011
_cod_original_cell_volume        7965.6(3)
_cod_database_code               7028389
_chemical_oxdiff_formula         'Ag C30 H30 N8 O8 C F3 S O3'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C12(H12), C11(H11), C23(H23), C21(H21), C17(H17), C20(H20),
 C24(H24), C19(H19), C15(H15), C13(H13), C16(H16), C18(H18), C22(H22), C14(H14)
;