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#$Date: 2016-03-23 04:03:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179275 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319549.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319549
loop_
_publ_author_name
'Ok-Sang Jung'
'Yun Ju Kim'
'Young-A Lee'
'Hee K. Chae'
'Ho G. Jang'
'Jongki Hong'
_publ_section_title
;
 Structures and Related Properties of AgX Bearing 3,3'-Thiobispyridine
 (X-= NO3-, BF4-, ClO4-, and PF6-)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2105
_journal_page_last               2110
_journal_paper_doi               10.1021/ic001072u
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C10 H8 Ag N3 O3 S'
_chemical_formula_weight         358.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 102.190(10)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            4
_cell_length_a                   8.177(2)
_cell_length_b                   10.2910(10)
_cell_length_c                   14.771(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1214.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.823
_diffrn_measured_fraction_theta_max 0.823
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2094
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    1.833
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²+1.2593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                1925
_reflns_number_total             1956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001072u_1.cif
_cod_data_source_block           '[Ag(Py2S)NO3]'
_cod_database_code               4319549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.96663(4) 0.27307(3) 0.20731(2) 0.04209(12) Uani 1 1 d . . .
S1 S 0.72242(12) 0.25291(9) -0.19653(6) 0.0378(2) Uani 1 1 d . . .
N1 N 0.8465(4) 0.1555(3) 0.0690(2) 0.0443(8) Uani 1 1 d . . .
N2 N 1.2395(4) 0.3311(4) 0.1972(2) 0.0424(8) Uani 1 1 d . . .
N3 N 1.1097(4) 0.0718(3) 0.3579(2) 0.0358(7) Uani 1 1 d . . .
O1 O 1.1304(4) -0.0162(3) 0.41612(19) 0.0479(7) Uani 1 1 d . . .
O2 O 1.1198(4) 0.1866(3) 0.3815(2) 0.0575(8) Uani 1 1 d . . .
O3 O 1.0791(5) 0.0430(3) 0.27394(19) 0.0639(9) Uani 1 1 d . . .
C1 C 0.8109(5) 0.2168(4) -0.0124(3) 0.0398(9) Uani 1 1 d . . .
H1 H 0.8281 0.3061 -0.0131 0.048 Uiso 1 1 calc R . .
C2 C 0.7501(4) 0.1551(4) -0.0954(2) 0.0335(8) Uani 1 1 d . . .
C3 C 0.7233(6) 0.0224(4) -0.0946(3) 0.0533(12) Uani 1 1 d . . .
H3 H 0.6828 -0.0229 -0.1492 0.064 Uiso 1 1 calc R . .
C4 C 0.7581(7) -0.0400(5) -0.0114(3) 0.0618(13) Uani 1 1 d . . .
H4 H 0.7409 -0.1292 -0.0088 0.074 Uiso 1 1 calc R . .
C5 C 0.8183(6) 0.0282(5) 0.0688(3) 0.0514(11) Uani 1 1 d . . .
H5 H 0.8402 -0.0163 0.1249 0.062 Uiso 1 1 calc R . .
C6 C 1.3824(5) 0.2933(4) 0.2533(3) 0.0424(9) Uani 1 1 d . . .
H6 H 1.3771 0.2540 0.3093 0.051 Uiso 1 1 calc R . .
C7 C 1.5379(5) 0.3101(4) 0.2316(2) 0.0344(8) Uani 1 1 d . . .
C8 C 1.5444(5) 0.3668(5) 0.1481(3) 0.0477(10) Uani 1 1 d . . .
H8 H 1.6465 0.3794 0.1312 0.057 Uiso 1 1 calc R . .
C9 C 1.3982(5) 0.4043(5) 0.0903(3) 0.0536(12) Uani 1 1 d . . .
H9 H 1.3999 0.4425 0.0335 0.064 Uiso 1 1 calc R . .
C10 C 1.2500(5) 0.3853(4) 0.1169(3) 0.0450(10) Uani 1 1 d . . .
H10 H 1.1518 0.4115 0.0770 0.054 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ag1 N1 107.36(12) . . ?
N2 Ag1 S1 151.52(8) . 4_566 ?
N1 Ag1 S1 100.55(9) . 4_566 ?
C2 S1 C7 103.73(17) . 4_465 ?
C2 S1 Ag1 114.20(13) . 4_565 ?
C7 S1 Ag1 106.22(13) 4_465 4_565 ?
C1 N1 C5 117.3(3) . . ?
C1 N1 Ag1 120.1(3) . . ?
C5 N1 Ag1 122.5(3) . . ?
C10 N2 C6 117.5(3) . . ?
C10 N2 Ag1 113.9(3) . . ?
C6 N2 Ag1 127.2(3) . . ?
O2 N3 O1 121.1(3) . . ?
O2 N3 O3 119.8(3) . . ?
O1 N3 O3 119.1(3) . . ?
N1 C1 C2 123.6(4) . . ?
C1 C2 C3 118.3(4) . . ?
C1 C2 S1 116.5(3) . . ?
C3 C2 S1 125.1(3) . . ?
C4 C3 C2 118.1(4) . . ?
C3 C4 C5 120.3(4) . . ?
N1 C5 C4 122.3(4) . . ?
N2 C6 C7 122.9(3) . . ?
C8 C7 C6 118.1(3) . . ?
C8 C7 S1 120.2(3) . 4_666 ?
C6 C7 S1 121.5(3) . 4_666 ?
C9 C8 C7 119.0(4) . . ?
C10 C9 C8 119.4(4) . . ?
N2 C10 C9 123.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N2 2.345(3) . ?
Ag1 N1 2.399(3) . ?
Ag1 S1 2.6972(12) 4_566 ?
S1 C2 1.775(4) . ?
S1 C7 1.774(4) 4_465 ?
S1 Ag1 2.6972(12) 4_565 ?
N1 C1 1.333(5) . ?
N1 C5 1.331(6) . ?
N2 C10 1.330(5) . ?
N2 C6 1.340(5) . ?
N3 O2 1.229(4) . ?
N3 O1 1.236(4) . ?
N3 O3 1.248(4) . ?
C1 C2 1.378(5) . ?
C2 C3 1.384(6) . ?
C3 C4 1.362(6) . ?
C4 C5 1.375(6) . ?
C6 C7 1.386(6) . ?
C7 C8 1.375(5) . ?
C7 S1 1.774(4) 4_666 ?
C8 C9 1.370(6) . ?
C9 C10 1.365(6) . ?
