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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/4/31/95/4319551.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_4319551
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 Cl N2 O4 S'
_chemical_formula_weight         395.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.780(10)
_cell_angle_gamma                90.010(10)
_cell_formula_units_Z            4
_cell_length_a                   8.8840(10)
_cell_length_b                   14.305(3)
_cell_length_c                   10.1100(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1230.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.838
_diffrn_measured_fraction_theta_max 0.838
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2149
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    2.035
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0662P)²+1.0318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                1976
_reflns_number_total             2014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001072u_3.cif
_cod_data_source_block           '[Ag(Py2S)]ClO4'
_cod_database_code               4319551
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Ag Ag 0.15719(4) 0.94517(2) 0.02168(4) 0.04079(16) Uani 1 1 d . . .
Cl Cl 0.67864(15) 1.43651(8) -0.15280(11) 0.0408(3) Uani 1 1 d . . .
S S 0.63322(17) 1.24185(10) 0.12475(13) 0.0495(4) Uani 1 1 d . . .
N1 N 0.2991(4) 1.0488(2) -0.0409(4) 0.0304(7) Uani 1 1 d . . .
N2 N 0.0326(4) 0.8256(3) 0.0686(4) 0.0313(7) Uani 1 1 d . . .
O1 O 0.7394(5) 1.3452(3) -0.1529(6) 0.0701(13) Uani 1 1 d . . .
O2 O 0.7663(9) 1.4983(3) -0.2165(5) 0.0871(17) Uani 1 1 d . . .
O3 O 0.6950(7) 1.4693(4) -0.0192(4) 0.0815(15) Uani 1 1 d . . .
O4 O 0.5206(6) 1.4362(5) -0.2315(7) 0.113(3) Uani 1 1 d . . .
C1 C 0.3943(5) 1.1071(3) 0.0491(4) 0.0290(9) Uani 1 1 d . . .
H1 H 0.3893 1.1082 0.1397 0.035 Uiso 1 1 calc R . .
C2 C 0.4995(5) 1.1653(3) 0.0129(4) 0.0299(8) Uani 1 1 d . . .
C3 C 0.5075(5) 1.1636(3) -0.1227(4) 0.0317(9) Uani 1 1 d . . .
H3 H 0.5770 1.2023 -0.1502 0.038 Uiso 1 1 calc R . .
C4 C 0.4104(5) 1.1033(3) -0.2153(4) 0.0351(10) Uani 1 1 d . . .
H4 H 0.4149 1.1000 -0.3060 0.042 Uiso 1 1 calc R . .
C5 C 0.3069(5) 1.0479(3) -0.1725(5) 0.0340(9) Uani 1 1 d . . .
H5 H 0.2401 1.0085 -0.2362 0.041 Uiso 1 1 calc R . .
C6 C 0.0056(5) 0.8140(3) 0.1914(4) 0.0319(9) Uani 1 1 d . . .
H6 H 0.0479 0.8569 0.2614 0.038 Uiso 1 1 calc R . .
C7 C -0.0825(5) 0.7409(3) 0.2175(4) 0.0341(9) Uani 1 1 d . . .
C8 C -0.1449(5) 0.6767(3) 0.1138(5) 0.0386(10) Uani 1 1 d . . .
H8 H -0.2066 0.6274 0.1282 0.046 Uiso 1 1 calc R . .
C9 C -0.1141(6) 0.6871(3) -0.0104(5) 0.0413(11) Uani 1 1 d . . .
H9 H -0.1516 0.6438 -0.0808 0.050 Uiso 1 1 calc R . .
C10 C -0.0265(5) 0.7627(3) -0.0295(4) 0.0352(10) Uani 1 1 d . . .
H10 H -0.0080 0.7701 -0.1149 0.042 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'
Cl Cl 0.1484 0.1585 '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
N1 Ag N2 170.99(14) . . ?
N1 Ag Ag 100.87(10) . 3_575 ?
N2 Ag Ag 86.25(10) . 3_575 ?
O3 Cl O4 111.0(4) . . ?
O3 Cl O1 112.2(3) . . ?
O4 Cl O1 108.5(3) . . ?
O3 Cl O2 107.8(3) . . ?
O4 Cl O2 109.2(5) . . ?
O1 Cl O2 108.0(3) . . ?
C2 S C7 105.8(2) . 2 ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Ag 122.4(3) . . ?
C5 N1 Ag 118.9(3) . . ?
C10 N2 C6 118.0(4) . . ?
C10 N2 Ag 119.2(3) . . ?
C6 N2 Ag 122.7(3) . . ?
N1 C1 C2 122.7(4) . . ?
C1 C2 C3 118.8(4) . . ?
C1 C2 S 126.0(3) . . ?
C3 C2 S 115.2(3) . . ?
C4 C3 C2 118.7(4) . . ?
C5 C4 C3 119.4(4) . . ?
N1 C5 C4 122.2(4) . . ?
N2 C6 C7 122.4(4) . . ?
C8 C7 C6 119.0(4) . . ?
C8 C7 S 122.3(4) . 2_545 ?
C6 C7 S 118.2(4) . 2_545 ?
C9 C8 C7 118.7(4) . . ?
C8 C9 C10 119.0(4) . . ?
N2 C10 C9 122.9(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
Ag N1 2.156(4) . ?
Ag N2 2.163(4) . ?
Ag Ag 3.1221(8) 3_575 ?
Cl O3 1.397(4) . ?
Cl O4 1.400(5) . ?
Cl O1 1.414(4) . ?
Cl O2 1.447(5) . ?
S C2 1.764(4) . ?
S C7 1.778(4) 2 ?
N1 C1 1.339(6) . ?
N1 C5 1.352(6) . ?
N2 C10 1.330(6) . ?
N2 C6 1.341(6) . ?
C1 C2 1.378(6) . ?
C2 C3 1.393(6) . ?
C3 C4 1.378(6) . ?
C4 C5 1.375(7) . ?
C6 C7 1.376(6) . ?
C7 C8 1.384(7) . ?
C7 S 1.778(4) 2_545 ?
C8 C9 1.368(7) . ?
C9 C10 1.378(7) . ?
