#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/23/2232336.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_2232336
loop_
_publ_author_name
'Hu, Xiao-Ming'
'Li, Fu-An'
_publ_section_title
;
 catena-Poly[[tris[silver(I)-μ-4,4'-bipyridine-κ²N:N']]
 tris(perchlorate) dihydrate]
;
_journal_coeditor_code           HY2472
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1505
_journal_paper_doi               10.1107/S1600536811040153
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ag3 (C10 H8 N2)3] (Cl O4)3, 2H2 O'
_chemical_formula_moiety         '(C30 H24 Ag3 N6 3+), 3(Cl O4 -), 2(H2 O)'
_chemical_formula_sum            'C30 H28 Ag3 Cl3 N6 O14'
_chemical_formula_weight         1126.54
_chemical_name_systematic
;
catena-Poly[tris[silver(I)-μ-4,4'-bipyridine-κ²N:N']
tris(perchlorate) dihydrate]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 148.768(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.259(2)
_cell_length_b                   15.7647(17)
_cell_length_c                   20.949(3)
_cell_measurement_reflns_used    2263
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      3.12
_cell_volume                     3640.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7095
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.7147
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.870
_refine_diff_density_min         -1.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0615
_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/[σ²(Fo²)+(0.0911P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                2229
_reflns_number_total             3145
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2472.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232336
_cod_database_fobs_code          2232336
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Ag Ag1 0.0000 0.45375(5) -0.2500 0.0566(3) Uani d S 1 2
Ag Ag2 0.59795(4) 0.05250(4) 0.68999(4) 0.0558(3) Uani d . 1 1
O O1 0.9612(11) 0.3396(11) 0.2576(10) 0.320(11) Uani d . 1 1
O O2 1.0878(12) 0.2447(7) 0.3549(11) 0.225(6) Uani d . 1 1
O O3 0.2999(8) 0.2382(7) 0.1888(9) 0.183(5) Uani d . 1 1
O O4 0.4471(17) 0.2642(6) 0.3825(14) 0.279(8) Uani d . 1 1
O O5 0.4822(10) 0.2063(8) 0.3197(13) 0.240(6) Uani d . 1 1
O O6 0.3993(6) 0.1309(6) 0.3237(6) 0.147(3) Uani d . 1 1
O O1W 0.1272(4) 0.2966(4) 0.1401(5) 0.0789(16) Uani d . 1 1
H H1WB 0.0798 0.2751 0.0713 0.118 Uiso d R 1 1
H H1WA 0.2000 0.2788 0.2016 0.118 Uiso d R 1 1
N N1 0.1878(5) 0.4546(3) -0.0596(5) 0.0465(14) Uani d . 1 1
N N2 0.4098(5) 0.0531(3) 0.4983(5) 0.0404(12) Uani d . 1 1
N N3 -0.2117(4) 0.0492(3) -0.1224(5) 0.0410(13) Uani d . 1 1
C C1 0.2488(6) 0.5264(4) -0.0009(6) 0.0390(14) Uani d . 1 1
H H1 0.2081 0.5774 -0.0424 0.047 Uiso calc R 1 1
C C2 0.3715(6) 0.5285(4) 0.1205(6) 0.0386(14) Uani d . 1 1
H H2 0.4115 0.5803 0.1582 0.046 Uiso calc R 1 1
C C3 0.4347(5) 0.4539(4) 0.1856(5) 0.0318(13) Uani d . 1 1
C C4 0.3680(6) 0.3788(4) 0.1220(7) 0.0522(17) Uani d . 1 1
H H4 0.4053 0.3266 0.1612 0.063 Uiso calc R 1 1
C C5 0.2469(6) 0.3825(5) 0.0010(6) 0.0560(19) Uani d . 1 1
H H5 0.2044 0.3319 -0.0402 0.067 Uiso calc R 1 1
C C6 0.3549(6) -0.0171(4) 0.4321(6) 0.0480(16) Uani d . 1 1
H H6 0.3989 -0.0675 0.4706 0.058 Uiso calc R 1 1
C C7 0.2379(5) -0.0197(4) 0.3112(5) 0.0459(16) Uani d . 1 1
H H7 0.2051 -0.0703 0.2679 0.055 Uiso calc R 1 1
C C8 0.1676(5) 0.0518(3) 0.2521(5) 0.0295(13) Uani d . 1 1
C C9 0.2230(6) 0.1252(4) 0.3215(6) 0.0461(16) Uani d . 1 1
H H9 0.1792 0.1755 0.2862 0.055 Uiso calc R 1 1
C C10 0.3441(6) 0.1232(4) 0.4441(6) 0.0524(17) Uani d . 1 1
H H10 0.3805 0.1729 0.4900 0.063 Uiso calc R 1 1
C C11 0.0359(5) 0.0509(3) 0.1213(5) 0.0279(12) Uani d . 1 1
C C12 -0.0267(5) -0.0238(4) 0.0584(5) 0.0318(13) Uani d . 1 1
H H12 0.0135 -0.0754 0.0971 0.038 Uiso calc R 1 1
C C13 -0.1494(5) -0.0225(4) -0.0625(5) 0.0382(14) Uani d . 1 1
H H13 -0.1898 -0.0737 -0.1032 0.046 Uiso calc R 1 1
C C14 -0.1510(6) 0.1215(4) -0.0627(6) 0.0534(18) Uani d . 1 1
H H14 -0.1926 0.1725 -0.1033 0.064 Uiso calc R 1 1
C C15 -0.0293(5) 0.1237(4) 0.0570(6) 0.0490(17) Uani d . 1 1
H H15 0.0094 0.1759 0.0948 0.059 Uiso calc R 1 1
Cl Cl1 1.0000 0.28764(14) 0.2500 0.0493(6) Uani d S 1 2
Cl Cl2 0.41235(16) 0.21081(11) 0.30907(16) 0.0539(5) Uani d . 1 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'
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'
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'
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
N1 Ag1 N1 . 2_554 179.3(3)
N3 Ag2 N2 1_656 . 176.36(19)
H1WB O1W H1WA . . 115.0
C1 N1 C5 . . 118.1(6)
C1 N1 Ag1 . . 121.3(4)
C5 N1 Ag1 . . 120.5(5)
C6 N2 C10 . . 117.6(6)
C6 N2 Ag2 . . 121.2(4)
C10 N2 Ag2 . . 121.1(4)
C13 N3 C14 . . 117.3(5)
C13 N3 Ag2 . 1_454 123.0(4)
C14 N3 Ag2 . 1_454 119.7(4)
N1 C1 C2 . . 122.4(6)
N1 C1 H1 . . 118.8
C2 C1 H1 . . 118.8
C3 C2 C1 . . 120.4(6)
C3 C2 H2 . . 119.8
C1 C2 H2 . . 119.8
C2 C3 C4 . . 116.2(6)
C2 C3 C3 . 2_655 121.7(4)
C4 C3 C3 . 2_655 122.1(4)
C5 C4 C3 . . 119.6(6)
C5 C4 H4 . . 120.2
C3 C4 H4 . . 120.2
N1 C5 C4 . . 123.3(6)
N1 C5 H5 . . 118.4
C4 C5 H5 . . 118.4
N2 C6 C7 . . 123.4(6)
N2 C6 H6 . . 118.3
C7 C6 H6 . . 118.3
C6 C7 C8 . . 120.5(6)
C6 C7 H7 . . 119.8
C8 C7 H7 . . 119.8
C7 C8 C9 . . 116.7(6)
C7 C8 C11 . . 122.5(5)
C9 C8 C11 . . 120.8(5)
C8 C9 C10 . . 119.5(6)
C8 C9 H9 . . 120.3
C10 C9 H9 . . 120.3
N2 C10 C9 . . 122.4(6)
N2 C10 H10 . . 118.8
C9 C10 H10 . . 118.8
C15 C11 C12 . . 116.1(6)
C15 C11 C8 . . 122.1(5)
C12 C11 C8 . . 121.7(5)
C11 C12 C13 . . 120.3(6)
C11 C12 H12 . . 119.9
C13 C12 H12 . . 119.9
N3 C13 C12 . . 122.5(6)
N3 C13 H13 . . 118.7
C12 C13 H13 . . 118.7
N3 C14 C15 . . 122.5(6)
N3 C14 H14 . . 118.8
C15 C14 H14 . . 118.8
C11 C15 C14 . . 121.2(6)
C11 C15 H15 . . 119.4
C14 C15 H15 . . 119.4
O1 Cl1 O1 2_755 . 99.3(17)
O1 Cl1 O2 2_755 2_755 105.5(7)
O1 Cl1 O2 . 2_755 113.2(9)
O1 Cl1 O2 2_755 . 113.2(9)
O1 Cl1 O2 . . 105.5(7)
O2 Cl1 O2 2_755 . 118.6(12)
O4 Cl2 O5 . . 115.0(10)
O4 Cl2 O6 . . 110.4(7)
O5 Cl2 O6 . . 109.2(6)
O4 Cl2 O3 . . 107.5(9)
O5 Cl2 O3 . . 105.6(7)
O6 Cl2 O3 . . 108.9(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ag1 N1 . 2.149(6)
Ag1 N1 2_554 2.149(6)
Ag2 N3 1_656 2.151(5)
Ag2 N2 . 2.158(6)
O1 Cl1 . 1.27(3)
O2 Cl1 . 1.325(9)
O3 Cl2 . 1.396(8)
O4 Cl2 . 1.295(10)
O5 Cl2 . 1.30(3)
O6 Cl2 . 1.379(8)
O1W H1WB . 0.8500
O1W H1WA . 0.8500
N1 C1 . 1.323(8)
N1 C5 . 1.324(9)
N2 C6 . 1.320(8)
N2 C10 . 1.323(8)
N3 C13 . 1.328(8)
N3 C14 . 1.329(8)
C1 C2 . 1.389(9)
C1 H1 . 0.9300
C2 C3 . 1.383(8)
C2 H2 . 0.9300
C3 C4 . 1.400(8)
C3 C3 2_655 1.475(12)
C4 C5 . 1.378(10)
C4 H4 . 0.9300
C5 H5 . 0.9300
C6 C7 . 1.353(8)
C6 H6 . 0.9300
C7 C8 . 1.368(8)
C7 H7 . 0.9300
C8 C9 . 1.383(8)
C8 C11 . 1.492(8)
C9 C10 . 1.385(9)
C9 H9 . 0.9300
C10 H10 . 0.9300
C11 C15 . 1.364(8)
C11 C12 . 1.377(8)
C12 C13 . 1.386(7)
C12 H12 . 0.9300
C13 H13 . 0.9300
C14 C15 . 1.374(8)
C14 H14 . 0.9300
C15 H15 . 0.9300
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
O1W H1WB O4 8_455 0.85 2.21 3.060(15) 173
O1W H1WA O3 . 0.85 2.44 2.99(3) 123
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
C5 N1 C1 C2 . . 0.5(10)
Ag1 N1 C1 C2 . . -177.1(4)
N1 C1 C2 C3 . . -0.8(9)
C1 C2 C3 C4 . . 0.2(9)
C1 C2 C3 C3 . 2_655 179.6(6)
C2 C3 C4 C5 . . 0.8(10)
C3 C3 C4 C5 2_655 . -178.7(7)
C1 N1 C5 C4 . . 0.5(11)
Ag1 N1 C5 C4 . . 178.1(6)
C3 C4 C5 N1 . . -1.1(11)
C10 N2 C6 C7 . . 4.0(10)
Ag2 N2 C6 C7 . . -178.7(5)
N2 C6 C7 C8 . . -3.6(11)
C6 C7 C8 C9 . . 1.2(9)
C6 C7 C8 C11 . . -175.4(6)
C7 C8 C9 C10 . . 0.5(9)
C11 C8 C9 C10 . . 177.2(6)
C6 N2 C10 C9 . . -2.1(10)
Ag2 N2 C10 C9 . . -179.5(5)
C8 C9 C10 N2 . . -0.1(10)
C7 C8 C11 C15 . . -169.4(6)
C9 C8 C11 C15 . . 14.1(9)
C7 C8 C11 C12 . . 10.0(9)
C9 C8 C11 C12 . . -166.5(5)
C15 C11 C12 C13 . . -1.4(8)
C8 C11 C12 C13 . . 179.1(5)
C14 N3 C13 C12 . . 1.3(9)
Ag2 N3 C13 C12 1_454 . 179.9(4)
C11 C12 C13 N3 . . -0.1(9)
C13 N3 C14 C15 . . -1.0(10)
Ag2 N3 C14 C15 1_454 . -179.7(5)
C12 C11 C15 C14 . . 1.7(9)
C8 C11 C15 C14 . . -178.8(6)
N3 C14 C15 C11 . . -0.5(11)
