#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/52/2235229.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2235229
loop_
_publ_author_name
'Li, Jia-Jia'
'Zhu, Wei-Min'
_publ_section_title
;
 Poly[[{μ₄-2,2'-[butane-1,4-diylbis(sulfanediyl)]bis(1,3,4-thiadiazole)}silver(I)]
 perchlorate sesquihydrate]
;
_journal_coeditor_code           RZ2753
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m845
_journal_paper_doi               10.1107/S1600536812022957
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ag (C8 H10 N4 S4)] Cl O4, 1.5H2 O'
_chemical_formula_moiety         'C8 H10 Ag N4 S4 +, Cl O4 -, 1.5(H2 O)'
_chemical_formula_sum            'C8 H13 Ag Cl N4 O5.5 S4'
_chemical_formula_weight         524.79
_chemical_name_systematic
;
Poly[[{μ₄-2,2'-[butane-1,4-diylbis(sulfanediyl)]bis(1,3,4-
thiadiazole)}silver(I)] perchlorate sesquihydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.02(2)
_cell_angle_beta                 119.727(14)
_cell_angle_gamma                94.20(2)
_cell_formula_units_Z            2
_cell_length_a                   10.076(12)
_cell_length_b                   10.08(2)
_cell_length_c                   10.137(12)
_cell_measurement_reflns_used    954
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      19.49
_cell_measurement_theta_min      2.32
_cell_volume                     889(2)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6708
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.746
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3237
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0596P)²+0.9001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                1834
_reflns_number_total             3237
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2753.cif
_cod_data_source_block           I
_cod_original_cell_volume        889(3)
_cod_database_code               2235229
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
O O5 0.5870(14) 0.9980(12) 0.5479(13) 0.111(3) Uani d PU 0.663(11) 1 . 1
H H1W 0.5826 0.9510 0.4743 0.166 Uiso d PR 0.663(11) 1 . 1
H H2W 0.5493 0.9603 0.5974 0.166 Uiso d PR 0.663(11) 1 . 1
O O5' 0.709(3) 0.984(2) 0.599(3) 0.111(3) Uani d PU 0.337(11) 1 . 2
H H3W 0.6772 0.9410 0.5137 0.166 Uiso d PR 0.337(11) 1 . 2
H H4W 0.6737 0.9609 0.6564 0.166 Uiso d PR 0.337(11) 1 . 2
Cl Cl1 0.6364(2) 0.2700(2) 0.2629(3) 0.0868(8) Uani d PGU 0.640(6) 1 A 1
O O1 0.5621(6) 0.1488(5) 0.2654(8) 0.105(2) Uani d PGU 0.640(6) 1 A 1
O O2 0.7031(8) 0.2400(7) 0.1638(8) 0.107(2) Uani d PGU 0.640(6) 1 A 1
O O3 0.7646(7) 0.3177(6) 0.4046(6) 0.093(2) Uani d PGU 0.640(6) 1 A 1
O O4 0.5392(6) 0.3695(5) 0.1966(8) 0.098(2) Uani d PGU 0.640(6) 1 A 1
Cl Cl1' 0.6364(2) 0.2700(2) 0.2629(3) 0.0868(8) Uani d PGU 0.360(6) 1 A 2
O O1' 0.5900(8) 0.3025(7) 0.3739(8) 0.105(2) Uani d PGU 0.360(6) 1 A 2
O O2' 0.7956(5) 0.2706(6) 0.3363(8) 0.107(2) Uani d PGU 0.360(6) 1 A 2
O O3' 0.5824(7) 0.3645(6) 0.1525(7) 0.093(2) Uani d PGU 0.360(6) 1 A 2
O O4' 0.5605(7) 0.1401(5) 0.1931(7) 0.098(2) Uani d PGU 0.360(6) 1 A 2
Ag Ag1 0.28732(7) 0.49669(7) 0.38379(8) 0.0710(3) Uani d . 1 1 . .
S S1 0.4338(2) 0.2152(2) 0.7857(2) 0.0592(6) Uani d . 1 1 . .
S S2 0.1184(2) 0.28824(19) 0.5359(2) 0.0517(5) Uani d . 1 1 . .
S S3 -0.2397(2) 0.5507(2) 0.0592(2) 0.0525(5) Uani d . 1 1 . .
S S4 -0.1933(2) 0.74107(19) -0.1386(2) 0.0539(5) Uani d . 1 1 . .
N N1 0.5493(7) 0.3652(6) 0.6644(7) 0.0519(16) Uani d . 1 1 . .
N N2 0.3926(6) 0.3663(6) 0.5770(6) 0.0464(15) Uani d . 1 1 . .
N N3 0.0497(7) 0.5526(6) 0.2226(6) 0.0488(15) Uani d . 1 1 . .
N N4 0.0286(6) 0.6374(5) 0.1089(6) 0.0433(14) Uani d . 1 1 . .
C C1 0.5838(9) 0.2893(8) 0.7730(9) 0.057(2) Uani d . 1 1 . .
H H1 0.6850 0.2755 0.8411 0.069 Uiso calc R 1 1 . .
C C2 0.3171(8) 0.2935(7) 0.6263(8) 0.0424(17) Uani d . 1 1 . .
C C3 0.0689(9) 0.1618(8) 0.6326(9) 0.054(2) Uani d . 1 1 . .
H H3A 0.1430 0.1754 0.7408 0.065 Uiso calc R 1 1 . .
H H3B -0.0309 0.1755 0.6198 0.065 Uiso calc R 1 1 . .
C C4 0.0641(9) 0.0183(8) 0.5792(8) 0.055(2) Uani d . 1 1 . .
H H4A 0.1607 0.0053 0.5839 0.065 Uiso calc R 1 1 . .
H H4B 0.0524 -0.0404 0.6473 0.065 Uiso calc R 1 1 . .
C C5 -0.0794(9) 0.5012(8) 0.2069(9) 0.0518(19) Uani d . 1 1 . .
H H5 -0.0839 0.4410 0.2724 0.062 Uiso calc R 1 1 . .
C C6 -0.1156(8) 0.6454(6) 0.0185(7) 0.0401(16) Uani d . 1 1 . .
C C7 -0.0201(9) 0.8336(8) -0.1127(9) 0.060(2) Uani d . 1 1 . .
H H7A 0.0559 0.7718 -0.0924 0.072 Uiso calc R 1 1 . .
H H7B -0.0431 0.8718 -0.2073 0.072 Uiso calc R 1 1 . .
C C8 0.0493(10) 0.9440(8) 0.0136(10) 0.068(2) Uani d . 1 1 . .
H H8A 0.0685 0.9068 0.1077 0.082 Uiso calc R 1 1 . .
H H8B 0.1475 0.9798 0.0268 0.082 Uiso calc R 1 1 . .
O O6 0.337(2) 0.974(2) 0.981(2) 0.169(8) Uani d PU 0.50 1 . .
H H5W 0.4339 0.9960 1.0303 0.254 Uiso d PR 0.50 1 . .
H H6W 0.3215 0.9007 0.9296 0.254 Uiso d PR 0.50 1 . .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O5 O5 H1W 2_676 . 88.4
O5 O5 H2W 2_676 . 74.1
H1W O5 H2W . . 116.5
O5 O5 H3W 2_676 . 129.1
H2W O5 H3W . . 121.9
O5 O5 H4W 2_676 . 139.9
H1W O5 H4W . . 108.3
H2W O5 H4W . . 65.8
H3W O5 H4W . . 75.3
H1W O5' H4W . . 94.7
H3W O5' H4W . . 120.0
O1 Cl1 O4 . . 114.6
O1 Cl1 O3 . . 114.0
O4 Cl1 O3 . . 111.4
O1 Cl1 O2 . . 105.0
O4 Cl1 O2 . . 106.5
O3 Cl1 O2 . . 104.3
O2' Cl1' O3' . . 112.2
O2' Cl1' O4' . . 111.4
O3' Cl1' O4' . . 109.7
O2' Cl1' O1' . . 109.6
O3' Cl1' O1' . . 107.8
O4' Cl1' O1' . . 105.9
N2 Ag1 N3 . . 136.8(2)
N2 Ag1 N1 . 2_666 118.1(2)
N3 Ag1 N1 . 2_666 104.8(2)
C1 S1 C2 . . 86.5(4)
C2 S2 C3 . . 102.5(3)
C5 S3 C6 . . 86.1(4)
C6 S4 C7 . . 100.3(3)
C1 N1 N2 . . 111.0(6)
C1 N1 Ag1 . 2_666 128.6(5)
N2 N1 Ag1 . 2_666 120.1(4)
C2 N2 N1 . . 113.0(6)
C2 N2 Ag1 . . 125.1(5)
N1 N2 Ag1 . . 121.7(4)
C5 N3 N4 . . 112.3(6)
C5 N3 Ag1 . . 127.3(5)
N4 N3 Ag1 . . 119.7(4)
C6 N4 N3 . . 110.5(5)
N1 C1 S1 . . 116.1(6)
N1 C1 H1 . . 122.0
S1 C1 H1 . . 122.0
N2 C2 S1 . . 113.4(5)
N2 C2 S2 . . 119.8(5)
S1 C2 S2 . . 126.8(4)
C4 C3 S2 . . 115.7(6)
C4 C3 H3A . . 108.4
S2 C3 H3A . . 108.4
C4 C3 H3B . . 108.4
S2 C3 H3B . . 108.4
H3A C3 H3B . . 107.4
C4 C4 C3 2_556 . 112.3(8)
C4 C4 H4A 2_556 . 109.1
C3 C4 H4A . . 109.1
C4 C4 H4B 2_556 . 109.1
C3 C4 H4B . . 109.1
H4A C4 H4B . . 107.9
N3 C5 S3 . . 115.6(6)
N3 C5 H5 . . 122.2
S3 C5 H5 . . 122.2
N4 C6 S3 . . 115.6(5)
N4 C6 S4 . . 125.7(5)
S3 C6 S4 . . 118.7(4)
C8 C7 S4 . . 115.0(6)
C8 C7 H7A . . 108.5
S4 C7 H7A . . 108.5
C8 C7 H7B . . 108.5
S4 C7 H7B . . 108.5
H7A C7 H7B . . 107.5
C8 C8 C7 2_575 . 114.0(9)
C8 C8 H8A 2_575 . 108.8
C7 C8 H8A . . 108.8
C8 C8 H8B 2_575 . 108.8
C7 C8 H8B . . 108.8
H8A C8 H8B . . 107.6
H5W O6 H6W . . 107.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O5 O5 2_676 1.53(2)
O5 H1W . 0.8502
O5 H2W . 0.8498
O5 H3W . 1.2854
O5 H4W . 1.1129
O5' H1W . 1.2852
O5' H3W . 0.8500
O5' H4W . 0.8500
Cl1 O1 . 1.393(5)
Cl1 O4 . 1.398(5)
Cl1 O3 . 1.408(4)
Cl1 O2 . 1.494(5)
Cl1' O2' . 1.394(4)
Cl1' O3' . 1.415(5)
Cl1' O4' . 1.433(5)
Cl1' O1' . 1.452(4)
Ag1 N2 . 2.239(6)
Ag1 N3 . 2.259(6)
Ag1 N1 2_666 2.323(6)
S1 C1 . 1.701(8)
S1 C2 . 1.720(7)
S2 C2 . 1.736(7)
S2 C3 . 1.821(7)
S3 C5 . 1.695(8)
S3 C6 . 1.735(7)
S4 C6 . 1.750(7)
S4 C7 . 1.810(8)
N1 C1 . 1.280(9)
N1 N2 . 1.376(8)
N1 Ag1 2_666 2.323(6)
N2 C2 . 1.300(8)
N3 C5 . 1.296(9)
N3 N4 . 1.398(8)
N4 C6 . 1.288(8)
C1 H1 . 0.9300
C3 C4 . 1.516(11)
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 C4 2_556 1.487(14)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 H5 . 0.9300
C7 C8 . 1.505(11)
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 C8 2_575 1.501(15)
C8 H8A . 0.9700
C8 H8B . 0.9700
O6 H5W . 0.8500
O6 H6W . 0.8498
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O6 H6W O4' 2_666 0.85 2.15 2.71(3) 123 y
O6 H6W O2 2_666 0.85 1.61 2.46(4) 178 y
O6 H5W O1 1_566 0.85 2.47 3.02(6) 123 y
O6 H5W O6 2_677 0.85 2.36 3.10(4) 146 y
O6 H5W O4' 1_566 0.85 1.98 2.62(6) 131 y
O5 H2W O1 2_666 0.85 2.42 3.27(4) 179 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C1 N1 N2 C2 . . 1.4(9)
Ag1 N1 N2 C2 2_666 . -173.9(5)
C1 N1 N2 Ag1 . . 176.4(5)
Ag1 N1 N2 Ag1 2_666 . 1.1(7)
N3 Ag1 N2 C2 . . 1.4(8)
N1 Ag1 N2 C2 2_666 . 173.3(6)
N3 Ag1 N2 N1 . . -173.0(4)
N1 Ag1 N2 N1 2_666 . -1.0(7)
N2 Ag1 N3 C5 . . -8.1(8)
N1 Ag1 N3 C5 2_666 . 179.3(6)
N2 Ag1 N3 N4 . . -177.8(4)
N1 Ag1 N3 N4 2_666 . 9.6(5)
C5 N3 N4 C6 . . 1.6(8)
Ag1 N3 N4 C6 . . 172.7(5)
N2 N1 C1 S1 . . -1.8(9)
Ag1 N1 C1 S1 2_666 . 173.0(4)
C2 S1 C1 N1 . . 1.3(7)
N1 N2 C2 S1 . . -0.5(8)
Ag1 N2 C2 S1 . . -175.2(3)
N1 N2 C2 S2 . . 177.2(5)
Ag1 N2 C2 S2 . . 2.4(9)
C1 S1 C2 N2 . . -0.4(6)
C1 S1 C2 S2 . . -177.8(5)
C3 S2 C2 N2 . . 174.1(6)
C3 S2 C2 S1 . . -8.6(6)
C2 S2 C3 C4 . . -80.2(6)
S2 C3 C4 C4 . 2_556 -67.4(10)
N4 N3 C5 S3 . . -1.7(8)
Ag1 N3 C5 S3 . . -172.0(3)
C6 S3 C5 N3 . . 1.0(6)
N3 N4 C6 S3 . . -0.8(8)
N3 N4 C6 S4 . . 179.6(5)
C5 S3 C6 N4 . . 0.0(6)
C5 S3 C6 S4 . . 179.6(5)
C7 S4 C6 N4 . . -7.9(7)
C7 S4 C6 S3 . . 172.5(4)
C6 S4 C7 C8 . . -74.4(6)
S4 C7 C8 C8 . 2_575 -65.6(11)
