#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318534.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_4318534
loop_
_publ_author_name
'Ming-Liang Tong'
'Yin-Miao Wu'
'Jie Ru'
'Xiao-Ming Chen'
'Ho-Chol Chang'
'Susumu Kitagawa'
_publ_contact_author
;
      Tong, Ming-Liang
      School of Chemistry and Chemical Engineering
      Sun Yat-Sen University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_email       cestml@zsu.edu.cn
_publ_contact_author_fax         '86 20 84112245'
_publ_contact_author_phone       86-20-84113986
_publ_section_title
;
 Pseudo-Polyrotaxane and β-Sheet Layer-Based Three-Dimensional
 Coordination Polymers Constructed with Silver Salts and Flexible
 Pyridyl-Type Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4846
_journal_page_last               4848
_journal_paper_doi               10.1021/ic0256922
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C41 H42 Ag3 N7 O7'
_chemical_formula_weight         1068.43
_chemical_name_systematic
; 
 ? 
;
_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                 94.72(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.619(2)
_cell_length_b                   19.781(4)
_cell_length_c                   26.799(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     4025.2(15)
_computing_cell_refinement       'XSCANS (Siemens, 1990)'
_computing_data_collection       'XSCANS (Siemens, 1990)'
_computing_data_reduction        'XSCANS (Siemens, 1990)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Siemens R3m'
_diffrn_measurement_method       ω-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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11742
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0384
_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)+(0.0408P)²+11.3666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                3412
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic0256922_s1_2.cif
_cod_data_source_block           complex_1
_cod_database_code               4318534
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_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.26099(5) 0.112450(17) 0.442829(11) 0.05422(12) Uani 1 d . . .
Ag2 Ag 0.2500 0.2500 1.0000 0.04698(13) Uani 1 d S . .
O1 O 0.0860(4) 0.21356(15) 0.45919(12) 0.0566(7) Uani 1 d . . .
O2 O 0.0766(4) 0.30745(14) 0.50305(11) 0.0526(7) Uani 1 d . . .
N1 N 0.2491(4) -0.12876(16) 0.86044(11) 0.0429(7) Uani 1 d . . .
N2 N 0.2668(5) 0.03117(17) 0.50041(12) 0.0504(8) Uani 1 d . . .
C1 C 0.2889(5) -0.0797(2) 0.82876(14) 0.0454(9) Uani 1 d . . .
H1A H 0.3186 -0.0359 0.8425 0.080 Uiso 1 d R . .
C2 C 0.2906(5) -0.08869(19) 0.77773(14) 0.0427(8) Uani 1 d . . .
H2A H 0.3171 -0.0512 0.7568 0.080 Uiso 1 d R . .
C3 C 0.2523(5) -0.15138(18) 0.75660(13) 0.0377(8) Uani 1 d . . .
C4 C 0.2078(5) -0.2020(2) 0.78918(14) 0.0449(9) Uani 1 d . . .
H4A H 0.1782 -0.2463 0.7765 0.080 Uiso 1 d R . .
C5 C 0.2081(6) -0.1887(2) 0.83973(15) 0.0479(9) Uani 1 d . . .
H5A H 0.1751 -0.2244 0.8614 0.080 Uiso 1 d R . .
C6 C 0.2624(5) -0.16546(19) 0.70163(14) 0.0440(8) Uani 1 d . . .
H6A H 0.1734 -0.1981 0.6913 0.080 Uiso 1 d R . .
H6B H 0.3747 -0.1856 0.6973 0.080 Uiso 1 d R . .
C7 C 0.2405(5) -0.10457(19) 0.66701(14) 0.0439(8) Uani 1 d . . .
H7A H 0.3278 -0.0712 0.6770 0.080 Uiso 1 d R . .
H7B H 0.1264 -0.0850 0.6698 0.080 Uiso 1 d R . .
C8 C 0.2576(6) -0.12458(19) 0.61258(14) 0.0475(9) Uani 1 d . . .
H8A H 0.1631 -0.1550 0.6024 0.080 Uiso 1 d R . .
H8B H 0.3659 -0.1491 0.6114 0.080 Uiso 1 d R . .
C9 C 0.2569(5) -0.06821(19) 0.57516(14) 0.0415(8) Uani 1 d . . .
C10 C 0.1908(7) -0.0796(2) 0.52651(16) 0.0585(11) Uani 1 d . . .
H10A H 0.1378 -0.1224 0.5175 0.080 Uiso 1 d R . .
C11 C 0.1996(7) -0.0298(2) 0.49082(15) 0.0630(12) Uani 1 d . . .
H11A H 0.1546 -0.0396 0.4571 0.080 Uiso 1 d R . .
C12 C 0.3238(7) -0.0045(2) 0.58509(16) 0.0609(12) Uani 1 d . . .
H12A H 0.3692 0.0066 0.6186 0.080 Uiso 1 d R . .
C13 C 0.3272(7) 0.0426(2) 0.54763(17) 0.0597(11) Uani 1 d . . .
H13A H 0.3746 0.0865 0.5559 0.080 Uiso 1 d R . .
N3 N 0.1714(4) 0.19881(17) 0.92800(11) 0.0429(7) Uani 1 d . . .
C14 C 0.2967(5) 0.1761(2) 0.90043(14) 0.0515(10) Uani 1 d . . .
H14A H 0.4167 0.1880 0.9103 0.080 Uiso 1 d R . .
C15 C 0.2625(6) 0.1377(2) 0.85811(15) 0.0545(10) Uani 1 d . . .
H15A H 0.3575 0.1220 0.8397 0.080 Uiso 1 d R . .
C16 C -0.0360(6) 0.1451(3) 0.86966(16) 0.0636(13) Uani 1 d . . .
H16A H -0.1571 0.1346 0.8600 0.080 Uiso 1 d R . .
C17 C 0.0085(6) 0.1841(3) 0.91160(17) 0.0676(14) Uani 1 d . . .
H17A H -0.0851 0.2018 0.9296 0.080 Uiso 1 d R . .
C18 C 0.0923(5) 0.12099(18) 0.84220(13) 0.0412(8) Uani 1 d . . .
C19 C 0.0476(6) 0.0795(2) 0.79567(13) 0.0486(9) Uani 1 d . . .
H19A H -0.0505 0.0507 0.8010 0.080 Uiso 1 d R . .
H19B H 0.1461 0.0513 0.7895 0.080 Uiso 1 d R . .
C20 C 0.0000 0.1232(3) 0.7500 0.0414(12) Uani 1 d S . .
H20A H 0.0983 0.1517 0.7441 0.080 Uiso 1 d R . .
C21 C 0.1522(4) 0.25626(18) 0.48878(13) 0.0370(8) Uani 1 d . . .
N4 N 0.5000 0.0879(3) 0.7500 0.0533(12) Uani 1 d S . .
O3 O 0.5000 0.1496(2) 0.7500 0.0911(18) Uani 1 d S . .
O4 O 0.5594(5) 0.0556(2) 0.78722(14) 0.0831(11) Uani 1 d . . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 N2 142.10(12) 6 . ?
N1 Ag1 O2 118.49(11) 6 7_556 ?
N2 Ag1 O2 94.44(12) . 7_556 ?
N1 Ag1 O1 94.62(11) 6 . ?
N2 Ag1 O1 116.31(12) . . ?
O2 Ag1 O1 67.59(9) 7_556 . ?
N3 Ag2 N3 180.000(1) . 7_557 ?
C21 O1 Ag1 118.1(2) . . ?
C21 O2 Ag1 119.5(2) . 7_556 ?
C5 N1 C1 115.9(3) . . ?
C5 N1 Ag1 122.0(2) . 6_556 ?
C1 N1 Ag1 122.0(3) . 6_556 ?
C11 N2 C13 115.9(3) . . ?
C11 N2 Ag1 122.4(3) . . ?
C13 N2 Ag1 121.5(3) . . ?
N1 C1 C2 123.7(4) . . ?
C1 C2 C3 120.1(3) . . ?
C2 C3 C4 116.3(3) . . ?
C2 C3 C6 122.6(3) . . ?
C4 C3 C6 121.0(3) . . ?
C5 C4 C3 119.9(4) . . ?
N1 C5 C4 124.0(4) . . ?
C3 C6 C7 116.0(3) . . ?
C6 C7 C8 111.3(3) . . ?
C9 C8 C7 116.8(3) . . ?
C12 C9 C10 115.7(4) . . ?
C12 C9 C8 124.8(4) . . ?
C10 C9 C8 119.5(4) . . ?
C9 C10 C11 120.4(4) . . ?
N2 C11 C10 123.7(4) . . ?
C13 C12 C9 120.6(4) . . ?
N2 C13 C12 123.8(4) . . ?
C17 N3 C14 116.1(3) . . ?
C17 N3 Ag2 124.9(3) . . ?
C14 N3 Ag2 118.8(2) . . ?
N3 C14 C15 123.3(4) . . ?
C18 C15 C14 120.0(4) . . ?
C18 C16 C17 119.8(4) . . ?
N3 C17 C16 123.9(4) . . ?
C16 C18 C15 116.8(4) . . ?
C16 C18 C19 121.0(4) . . ?
C15 C18 C19 122.1(4) . . ?
C18 C19 C20 112.3(3) . . ?
C19 C20 C19 110.5(4) 2_556 . ?
O1 C21 O2 125.4(3) . . ?
O1 C21 C21 117.3(4) . 7_556 ?
O2 C21 C21 117.3(4) . 7_556 ?
O3 N4 O4 121.0(3) . 2_656 ?
O3 N4 O4 121.0(3) . . ?
O4 N4 O4 117.9(6) 2_656 . ?
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 N1 2.226(3) 6 ?
Ag1 N2 2.226(3) . ?
Ag1 O2 2.419(3) 7_556 ?
Ag1 O1 2.463(3) . ?
Ag2 N3 2.217(3) . ?
Ag2 N3 2.217(3) 7_557 ?
O1 C21 1.237(4) . ?
O2 C21 1.241(4) . ?
O2 Ag1 2.419(3) 7_556 ?
N1 C5 1.336(5) . ?
N1 C1 1.341(5) . ?
N1 Ag1 2.226(3) 6_556 ?
N2 C11 1.326(6) . ?
N2 C13 1.330(5) . ?
C1 C2 1.380(5) . ?
C2 C3 1.384(5) . ?
C3 C4 1.389(5) . ?
C3 C6 1.507(5) . ?
C4 C5 1.380(5) . ?
C6 C7 1.521(5) . ?
C7 C8 1.527(5) . ?
C8 C9 1.499(5) . ?
C9 C12 1.377(6) . ?
C9 C10 1.377(5) . ?
C10 C11 1.379(6) . ?
C12 C13 1.372(6) . ?
N3 C17 1.315(5) . ?
N3 C14 1.332(5) . ?
C14 C15 1.372(5) . ?
C15 C18 1.372(6) . ?
C16 C18 1.358(6) . ?
C16 C17 1.382(6) . ?
C18 C19 1.508(5) . ?
C19 C20 1.518(5) . ?
C20 C19 1.518(5) 2_556 ?
C21 C21 1.580(7) 7_556 ?
N4 O3 1.221(7) . ?
N4 O4 1.238(4) 2_656 ?
N4 O4 1.238(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4A O3 0.96 2.53 3.457(6) 161.0 3_445
C10 H10A O1 0.96 2.59 3.428(6) 145.6 5_556
C15 H15A O4 0.96 2.54 3.474(5) 165.9 .
