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_7028391
_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         'C45 H45 Ag3 N9 O9, 3(C2 F6 N O4 S2)'
_chemical_formula_sum            'C51 H45 Ag3 F18 N12 O21 S6'
_chemical_formula_weight         2019.93
_chemical_name_common
;
tris(pyridine-N-oxide) silver bistriflimide
;
_chemical_name_systematic
;
tris(pyridine-N-oxide) silver bis(trifluoromethylsulfonyl)imide
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   25.5554(4)
_cell_length_b                   25.5554(4)
_cell_length_c                   56.4189(11)
_cell_measurement_reflns_used    40166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1457
_cell_measurement_theta_min      2.6840
_cell_volume                     31909.5(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
XS, 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -78.00   -1.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -57.0000 -120.0000 154

  2 omega  -32.00   52.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513   57.0000  150.0000 168

  3 omega   -8.00   23.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -99.0000  150.0000 62

  4 omega   -9.00   55.00   0.5000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -99.0000   90.0000 128
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0317519000
_diffrn_orient_matrix_UB_12      -0.0171552000
_diffrn_orient_matrix_UB_13      -0.0016300000
_diffrn_orient_matrix_UB_21      -0.0008878000
_diffrn_orient_matrix_UB_22      0.0270306000
_diffrn_orient_matrix_UB_23      -0.0016025000
_diffrn_orient_matrix_UB_31      0.0043237000
_diffrn_orient_matrix_UB_32      -0.0012861000
_diffrn_orient_matrix_UB_33      -0.0123658000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            53899
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             18036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         14480
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+190.5742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                12956
_reflns_number_total             14480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52416g.txt
_cod_data_source_block           kb2002
_cod_database_code               7028391
_chemical_oxdiff_formula         'Ag C2 F6 S2 O4 N C10 H10 O2 N2'
_reflns_odcompleteness_completeness 99.85
_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. Uiso/Uaniso restraints and constraints
Uanis(O5) = Uanis(O5')
Uanis(N14) = Uanis(N14')
Uanis(C39) = Uanis(C39')
Uanis(C40) = Uanis(C40')
Uanis(C41) = Uanis(C41')
Uanis(C42) = Uanis(C42')
Uanis(C43) = Uanis(C43')
Uanis(S72) = Uanis(S72')
Uanis(O73) = Uanis(O73')
Uanis(O74) = Uanis(O74')
Uanis(C75) = Uanis(C75')
Uanis(F76) = Uanis(F76')
Uanis(F77) = Uanis(F77')
Uanis(F78) = Uanis(F78')
3. Same fragment restrains
{O5, N14, C39, C40, C41, C42, C43}
as
{O5', N14', C39', C40', C41', C42', C43'}
{S72, O73, O74, C75, F76, F77, F78}
as
{S72', O73', O74', C75', F76', F77', F78'}
4. Others
 Sof(S72')=Sof(O73')=Sof(O74')=Sof(C75')=Sof(F76')=Sof(F77')=Sof(F78')=1-FVAR(1)
 Sof(S72)=Sof(O73)=Sof(O74)=Sof(C75)=Sof(F76)=Sof(F77)=Sof(F78)=FVAR(1)
 Sof(O5')=Sof(N14')=Sof(C39')=Sof(H39')=Sof(C40')=Sof(H40')=Sof(C41')=
 Sof(H41')=Sof(C42')=Sof(H42')=Sof(C43')=Sof(H43')=1-FVAR(2)
 Sof(O5)=Sof(N14)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=
 Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=FVAR(2)
5.a Riding coordinates:
 C21(H21)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C39'(H39'), C40'(H40'), C41'(H41'), C42'(H42'), C43'(H43'),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
;