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_7028392
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 H40 Ag3 N8 O8, 3(C F3 O3 S)'
_chemical_formula_sum            'C43 H40 Ag3 F9 N8 O17 S3'
_chemical_formula_weight         1531.62
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.519(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0275(3)
_cell_length_b                   25.8608(10)
_cell_length_c                   14.6674(4)
_cell_measurement_reflns_used    8184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1360
_cell_measurement_theta_min      2.9950
_cell_volume                     2665.50(17)
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.6850
_diffrn_measurement_details
;
  1 omega  -76.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513 -178.0000  -30.0000 37

  2 omega  -51.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -77.0000 -120.0000 100

  3 omega   10.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000   30.0000 72

  4 omega  -20.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1513  -99.0000  -30.0000 25

  5 omega   11.00   36.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000 -120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1000549000
_diffrn_orient_matrix_UB_12      0.0030107000
_diffrn_orient_matrix_UB_13      -0.0033052000
_diffrn_orient_matrix_UB_21      -0.0123388000
_diffrn_orient_matrix_UB_22      0.0267510000
_diffrn_orient_matrix_UB_23      -0.0088017000
_diffrn_orient_matrix_UB_31      0.0055720000
_diffrn_orient_matrix_UB_32      0.0051963000
_diffrn_orient_matrix_UB_33      0.0474425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13133
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81739
_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    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         9023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0173P)^2^+1.0040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                8638
_reflns_number_total             9023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52416g.txt
_cod_data_source_block           kb2010
_cod_original_cell_volume        2665.49(16)
_cod_database_code               7028392
_chemical_oxdiff_formula         'Ag C16 H15 F3 S O3 N3'
_reflns_odcompleteness_completeness 99.84
_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:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56)
;