#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/28/2202865.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_2202865
loop_
_publ_author_name
'Zhu, Hai-Liang'
'Wang, Zao-Gui'
'Lin, Yong-Shan'
'Zou, Ying'
'Tang, Lu-Lu'
'Shao, Si-Chang'
_publ_section_title
;
 Tris(μ-1,6-diaminohexane)diterephthalatotetrasilver(I) dihydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m942
_journal_page_last               m943
_journal_paper_doi               10.1107/S1600536803020373
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ag4 (C8 H4 O4)2 (C6 H14 N2)3], 2H2 O'
_chemical_formula_moiety         'C17 H28 Ag2 N3 O4, H2 O'
_chemical_formula_sum            'C17 H30 Ag2 N3 O5'
_chemical_formula_weight         572.18
_chemical_name_systematic
;
Tris(1,6-diaminohexane)diterephthalatotetrasilver(I) dihydrate
;
_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                110.08(3)
_cell_angle_beta                 98.73(3)
_cell_angle_gamma                96.31(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2200(10)
_cell_length_b                   10.928(2)
_cell_length_c                   13.919(3)
_cell_measurement_reflns_used    4208
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.75
_cell_volume                     1003.9(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4537
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.983
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.949
_refine_ls_extinction_coef       0.0038(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0371
_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)+(0.0429P)²+1.1362P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                3353
_reflns_number_total             3814
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om6175.cif
_cod_data_source_block           I
_cod_original_cell_volume        1003.9(3)
_cod_database_code               2202865
_cod_database_fobs_code          2202865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ag1 0.45582(5) 0.47516(3) 0.32966(2) 0.04479(13) Uani d . 1 . . Ag
Ag2 0.13054(6) 0.37910(4) 0.13754(3) 0.06196(16) Uani d . 1 . . Ag
O3 0.0277(5) 0.1945(3) 0.1412(3) 0.0552(8) Uani d . 1 . . O
O2 -0.0853(5) -0.3665(3) 0.3071(3) 0.0609(9) Uani d . 1 . . O
C10 0.5037(6) 0.1375(4) 0.2084(3) 0.0357(8) Uani d . 1 . . C
H10A 0.4043 0.1649 0.2453 0.080 Uiso d R 1 . . H
H10B 0.6118 0.1381 0.2582 0.080 Uiso d R 1 . . H
C5 -0.0281(5) 0.0475(4) 0.2278(3) 0.0362(8) Uani d . 1 . . C
C4 -0.0158(6) 0.0247(4) 0.3207(3) 0.0398(9) Uani d . 1 . . C
H4A 0.0182 0.0984 0.3861 0.080 Uiso d R 1 . . H
C13 0.3548(6) -0.2465(4) 0.0998(3) 0.0418(9) Uani d . 1 . . C
H13A 0.4556 -0.2673 0.0624 0.080 Uiso d R 1 . . H
H13B 0.2420 -0.2539 0.0503 0.080 Uiso d R 1 . . H
N1 0.6357(5) 0.3690(3) 0.2367(3) 0.0425(8) Uani d . 1 . . N
H1A 0.7361 0.3622 0.2804 0.080 Uiso d R 1 . . H
H1B 0.6807 0.4189 0.2028 0.080 Uiso d R 1 . . H
N3 0.2685(5) 0.5793(3) 0.4171(3) 0.0450(8) Uani d . 1 . . N
H3B 0.2205 0.5298 0.4504 0.080 Uiso d R 1 . . H
H3C 0.1708 0.5859 0.3716 0.080 Uiso d R 1 . . H
C6 -0.0808(6) -0.0600(4) 0.1339(3) 0.0393(9) Uani d . 1 . . C
H6A -0.0897 -0.0457 0.0692 0.080 Uiso d R 1 . . H
C7 -0.1220(6) -0.1863(4) 0.1337(3) 0.0396(9) Uani d . 1 . . C
H7A -0.1616 -0.2594 0.0682 0.080 Uiso d R 1 . . H
C3 -0.0523(6) -0.1025(4) 0.3196(3) 0.0389(9) Uani d . 1 . . C
H3A -0.0405 -0.1167 0.3844 0.080 Uiso d R 1 . . H
C12 0.4085(6) -0.1061(4) 0.1781(3) 0.0376(9) Uani d . 1 . . C
H12A 0.5242 -0.0985 0.2256 0.080 Uiso d R 1 . . H
H12B 0.3104 -0.0877 0.2177 0.080 Uiso d R 1 . . H
C16 0.4073(6) 0.8096(4) 0.4454(3) 0.0440(10) Uani d . 1 . . C
H16A 0.5097 0.7819 0.4113 0.080 Uiso d R 1 . . H
H16B 0.3027 0.8085 0.3933 0.080 Uiso d R 1 . . H
O1 -0.2176(6) -0.4402(3) 0.1402(2) 0.0682(10) Uani d . 1 . . O
C17 0.4709(7) 0.9501(4) 0.5241(3) 0.0482(10) Uani d . 1 . . C
H17A 0.5776 0.9512 0.5749 0.080 Uiso d R 1 . . H
H17B 0.3697 0.9762 0.5598 0.080 Uiso d R 1 . . H
C2 -0.1057(5) -0.2098(4) 0.2257(3) 0.0348(8) Uani d . 1 . . C
C9 0.5581(6) 0.2347(4) 0.1580(3) 0.0399(9) Uani d . 1 . . C
H9A 0.4479 0.2386 0.1116 0.080 Uiso d R 1 . . H
H9B 0.6514 0.2042 0.1173 0.080 Uiso d R 1 . . H
C8 0.0173(6) 0.1861(4) 0.2290(4) 0.0425(9) Uani d . 1 . . C
C15 0.3453(7) 0.7136(4) 0.4955(3) 0.0471(10) Uani d . 1 . . C
H15A 0.4530 0.7088 0.5431 0.080 Uiso d R 1 . . H
H15B 0.2510 0.7457 0.5349 0.080 Uiso d R 1 . . H
O4 0.0377(6) 0.2814(3) 0.3106(3) 0.0660(10) Uani d . 1 . . O
C11 0.4361(6) -0.0031(4) 0.1285(3) 0.0382(9) Uani d . 1 . . C
H11A 0.5276 -0.0251 0.0848 0.080 Uiso d R 1 . . H
H11B 0.3178 -0.0061 0.0849 0.080 Uiso d R 1 . . H
C14 0.3193(7) -0.3442(4) 0.1527(3) 0.0471(10) Uani d . 1 . . C
H14A 0.2141 -0.3248 0.1867 0.080 Uiso d R 1 . . H
H14B 0.4294 -0.3303 0.2059 0.080 Uiso d R 1 . . H
C1 -0.1397(6) -0.3493(4) 0.2246(3) 0.0416(9) Uani d . 1 . . C
N2 0.2714(12) -0.4793(4) 0.0868(4) 0.127(3) Uani d . 1 . . N
H2A 0.3834 -0.5044 0.0758 0.080 Uiso d R 1 . . H
H2B 0.2041 -0.4862 0.0246 0.080 Uiso d R 1 . . H
O1W -0.2084(5) -0.3810(4) 0.4810(3) 0.0776(11) Uani d . 1 . . O
H1WA -0.1693 -0.3764 0.4172 0.080 Uiso d R 1 . . H
H1WB -0.1662 -0.3273 0.5476 0.080 Uiso d R 1 . . H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N3 Ag1 N1 . . 177.80(13)
N3 Ag1 Ag2 . . 87.93(10)
N1 Ag1 Ag2 . . 89.89(10)
O3 Ag2 N2 . 1_565 158.96(18)
O3 Ag2 Ag1 . . 98.98(10)
N2 Ag2 Ag1 1_565 . 87.55(18)
C8 O3 Ag2 . . 118.5(3)
C9 C10 C11 . . 112.2(3)
C9 C10 H10A . . 109.2
C11 C10 H10A . . 109.3
C9 C10 H10B . . 109.1
C11 C10 H10B . . 109.0
H10A C10 H10B . . 108.0
C6 C5 C4 . . 118.7(4)
C6 C5 C8 . . 120.7(4)
C4 C5 C8 . . 120.6(4)
C3 C4 C5 . . 120.6(4)
C3 C4 H4A . . 119.9
C5 C4 H4A . . 119.5
C12 C13 C14 . . 111.5(3)
C12 C13 H13A . . 109.2
C14 C13 H13A . . 109.4
C12 C13 H13B . . 109.4
C14 C13 H13B . . 109.2
H13A C13 H13B . . 108.1
C9 N1 Ag1 . . 119.4(3)
C9 N1 H1A . . 107.4
Ag1 N1 H1A . . 107.5
C9 N1 H1B . . 107.4
Ag1 N1 H1B . . 107.5
H1A N1 H1B . . 107.0
C15 N3 Ag1 . . 118.1(3)
C15 N3 H3B . . 107.6
Ag1 N3 H3B . . 107.8
C15 N3 H3C . . 107.8
Ag1 N3 H3C . . 107.8
H3B N3 H3C . . 107.2
C7 C6 C5 . . 120.2(4)
C7 C6 H6A . . 120.2
C5 C6 H6A . . 119.6
C6 C7 C2 . . 121.3(4)
C6 C7 H7A . . 119.3
C2 C7 H7A . . 119.4
C4 C3 C2 . . 120.6(4)
C4 C3 H3A . . 119.6
C2 C3 H3A . . 119.8
C13 C12 C11 . . 113.6(3)
C13 C12 H12A . . 108.9
C11 C12 H12A . . 108.8
C13 C12 H12B . . 108.7
C11 C12 H12B . . 108.8
H12A C12 H12B . . 107.8
C15 C16 C17 . . 112.4(3)
C15 C16 H16A . . 109.4
C17 C16 H16A . . 109.3
C15 C16 H16B . . 108.9
C17 C16 H16B . . 108.8
H16A C16 H16B . . 108.0
C17 C17 C16 2_676 . 113.8(4)
C17 C17 H17A 2_676 . 108.4
C16 C17 H17A . . 108.4
C17 C17 H17B 2_676 . 109.3
C16 C17 H17B . . 108.9
H17A C17 H17B . . 107.8
C7 C2 C3 . . 118.5(3)
C7 C2 C1 . . 120.9(4)
C3 C2 C1 . . 120.6(3)
N1 C9 C10 . . 111.8(3)
N1 C9 H9A . . 109.2
C10 C9 H9A . . 109.1
N1 C9 H9B . . 109.5
C10 C9 H9B . . 109.2
H9A C9 H9B . . 108.0
O4 C8 O3 . . 124.3(4)
O4 C8 C5 . . 120.2(4)
O3 C8 C5 . . 115.5(4)
N3 C15 C16 . . 111.9(3)
N3 C15 H15A . . 108.7
C16 C15 H15A . . 108.9
N3 C15 H15B . . 109.9
C16 C15 H15B . . 109.3
H15A C15 H15B . . 108.0
C12 C11 C10 . . 113.3(3)
C12 C11 H11A . . 108.8
C10 C11 H11A . . 109.0
C12 C11 H11B . . 108.9
C10 C11 H11B . . 108.9
H11A C11 H11B . . 107.9
N2 C14 C13 . . 116.3(4)
N2 C14 H14A . . 106.0
C13 C14 H14A . . 108.3
N2 C14 H14B . . 110.3
C13 C14 H14B . . 108.0
H14A C14 H14B . . 107.5
O2 C1 O1 . . 124.2(4)
O2 C1 C2 . . 117.8(4)
O1 C1 C2 . . 118.0(4)
C14 N2 Ag2 . 1_545 120.5(3)
C14 N2 H2A . . 104.9
Ag2 N2 H2A 1_545 . 105.9
C14 N2 H2B . . 109.0
Ag2 N2 H2B 1_545 . 108.7
H2A N2 H2B . . 107.2
H1WA O1W H1WB . . 129.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag1 N3 . 2.120(4) ?
Ag1 N1 . 2.125(3) ?
Ag1 Ag2 . 3.0646(14) ?
Ag2 O3 . 2.092(3) ?
Ag2 N2 1_565 2.133(4) ?
O3 C8 . 1.269(5) ?
O2 C1 . 1.240(5) ?
C10 C9 . 1.510(5) ?
C10 C11 . 1.527(5) ?
C10 H10A . 0.9600 ?
C10 H10B . 0.9600 ?
C5 C6 . 1.389(5) ?
C5 C4 . 1.390(6) ?
C5 C8 . 1.508(5) ?
C4 C3 . 1.381(6) ?
C4 H4A . 0.9600 ?
C13 C12 . 1.512(5) ?
C13 C14 . 1.512(5) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
N1 C9 . 1.483(5) ?
N1 H1A . 0.8999 ?
N1 H1B . 0.9000 ?
N3 C15 . 1.480(5) ?
N3 H3B . 0.9001 ?
N3 H3C . 0.9000 ?
C6 C7 . 1.378(5) ?
C6 H6A . 0.9600 ?
C7 C2 . 1.382(5) ?
C7 H7A . 0.9600 ?
C3 C2 . 1.388(5) ?
C3 H3A . 0.9600 ?
C12 C11 . 1.518(5) ?
C12 H12A . 0.9600 ?
C12 H12B . 0.9600 ?
C16 C15 . 1.510(6) ?
C16 C17 . 1.518(6) ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
O1 C1 . 1.247(5) ?
C17 C17 2_676 1.517(8) ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C2 C1 . 1.511(5) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C8 O4 . 1.225(5) ?
C15 H15A . 0.9601 ?
C15 H15B . 0.9600 ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C14 N2 . 1.415(6) ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
N2 Ag2 1_545 2.133(4) ?
N2 H2A . 0.9000 ?
N2 H2B . 0.9000 ?
O1W H1WA . 0.9876 ?
O1W H1WB . 0.8931 ?
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
N1 H1A O4 1_655 0.90 2.47 3.283(5) 151
N1 H1B O1 1_665 0.90 2.13 3.023(5) 172
N1 H1B O2 1_665 0.90 2.55 3.090(5) 119
N3 H3B O1W 2_556 0.90 2.15 2.998(5) 157
N3 H3C O2 1_565 0.90 2.13 2.997(5) 163
N2 H2B O1 2_545 0.90 2.18 2.924(6) 140
O1W H1WA O2 . 0.99 1.76 2.749(5) 177
O1W H1WB O4 2_556 0.89 1.92 2.751(5) 155
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
N3 Ag1 Ag2 O3 . . -96.44(14)
N1 Ag1 Ag2 O3 . . 83.88(13)
N3 Ag1 Ag2 N2 . 1_565 103.7(2)
N1 Ag1 Ag2 N2 . 1_565 -76.0(2)
N2 Ag2 O3 C8 1_565 . 147.7(6)
Ag1 Ag2 O3 C8 . . 40.8(3)
C6 C5 C4 C3 . . 1.1(6)
C8 C5 C4 C3 . . -178.2(4)
N3 Ag1 N1 C9 . . -49(3)
Ag2 Ag1 N1 C9 . . -41.2(3)
N1 Ag1 N3 C15 . . -131(3)
Ag2 Ag1 N3 C15 . . -139.6(3)
C4 C5 C6 C7 . . 0.7(6)
C8 C5 C6 C7 . . 180.0(4)
C5 C6 C7 C2 . . -2.3(6)
C5 C4 C3 C2 . . -1.3(6)
C14 C13 C12 C11 . . -177.1(4)
C15 C16 C17 C17 . 2_676 -178.4(5)
C6 C7 C2 C3 . . 2.0(6)
C6 C7 C2 C1 . . -176.3(4)
C4 C3 C2 C7 . . -0.2(6)
C4 C3 C2 C1 . . 178.1(4)
Ag1 N1 C9 C10 . . -65.5(4)
C11 C10 C9 N1 . . -176.2(3)
Ag2 O3 C8 O4 . . 10.9(6)
Ag2 O3 C8 C5 . . -170.7(2)
C6 C5 C8 O4 . . 169.8(4)
C4 C5 C8 O4 . . -11.0(6)
C6 C5 C8 O3 . . -8.7(6)
C4 C5 C8 O3 . . 170.6(4)
Ag1 N3 C15 C16 . . 64.9(4)
C17 C16 C15 N3 . . 175.2(4)
C13 C12 C11 C10 . . -176.0(3)
C9 C10 C11 C12 . . 171.4(3)
C12 C13 C14 N2 . . -178.8(5)
C7 C2 C1 O2 . . 165.2(4)
C3 C2 C1 O2 . . -13.0(6)
C7 C2 C1 O1 . . -13.6(6)
C3 C2 C1 O1 . . 168.2(4)
C13 C14 N2 Ag2 . 1_545 -159.7(4)
