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#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/28/8102860.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_8102860
loop_
_publ_author_name
'Guang-Yi Wang'
'Zhen Ma'
'Bing Liu'
'Cun-Yuan Cao'
_publ_section_title
;
 Crystal structure of
 aqua(hexamethylenetetraamine)-(pyrazine-2,3-dicarboxylato)disilver(I)
 dihydrate, Ag2(H2O)(C6H2N2O4)(C6H12N4) · 2H2O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              771
_journal_volume                  225
_journal_year                    2010
_chemical_formula_moiety         'C12 H14 Ag2 N6 O5, 2(O)'
_chemical_formula_sum            'C12 H20 Ag2 N6 O7'
_chemical_formula_weight         576.08
_chemical_name_systematic
;
aqua[pyrazine-2,3-dicarboxyliato-disilver(I)-hexamethylenetetraamine] 
dihydrate, C₁₂H₂₀Ag₂N₆O₇
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   20.769(5)
_cell_length_b                   6.405(5)
_cell_length_c                   12.187(5)
_cell_measurement_reflns_used    3026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      1.96
_cell_volume                     1621.2(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8394
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.471
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3026
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0219
_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)+(0.0413P)²+0.7324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                2968
_reflns_number_total             3026
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            1267-3204.cff
_cod_data_source_block           bb
_cod_database_code               8102860
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'
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
C1 C 0.40922(19) 0.9742(6) 0.7299(3) 0.0130(7) Uani 1 1 d . . .
C2 C 0.34283(19) 0.9441(5) 0.7283(3) 0.0105(7) Uani 1 1 d . . .
C3 C 0.40734(19) 0.9553(6) 0.9177(3) 0.0143(8) Uani 1 1 d . . .
H3 H 0.4288 0.9549 0.9847 0.017 Uiso 1 1 calc R . .
C4 C 0.3410(2) 0.9274(5) 0.9152(4) 0.0163(8) Uani 1 1 d . . .
H4 H 0.3188 0.9114 0.9809 0.020 Uiso 1 1 calc R . .
C5 C 0.44789(17) 1.0031(7) 0.6243(3) 0.0166(7) Uani 1 1 d . . .
C6 C 0.30225(17) 0.9439(5) 0.6244(3) 0.0116(7) Uani 1 1 d . . .
C7 C 0.56591(17) 0.5739(5) 0.8017(3) 0.0112(8) Uani 1 1 d . . .
H7A H 0.5329 0.5728 0.7454 0.013 Uiso 1 1 calc R . .
H7B H 0.5447 0.5781 0.8726 0.013 Uiso 1 1 calc R . .
C8 C 0.65638(17) 0.7590(5) 0.8751(3) 0.0121(7) Uani 1 1 d . . .
H8A H 0.6830 0.8828 0.8684 0.015 Uiso 1 1 calc R . .
H8B H 0.6358 0.7623 0.9466 0.015 Uiso 1 1 calc R . .
C9 C 0.65523(17) 0.3879(6) 0.8799(3) 0.0102(7) Uani 1 1 d . . .
H9A H 0.6348 0.3922 0.9514 0.012 Uiso 1 1 calc R . .
H9B H 0.6810 0.2619 0.8760 0.012 Uiso 1 1 calc R . .
C10 C 0.72677(18) 0.5644(5) 0.7569(3) 0.0115(8) Uani 1 1 d . . .
H10A H 0.7532 0.4401 0.7510 0.014 Uiso 1 1 calc R . .
H10B H 0.7545 0.6849 0.7476 0.014 Uiso 1 1 calc R . .
C11 C 0.63776(16) 0.7516(5) 0.6805(3) 0.0119(7) Uani 1 1 d . . .
H11A H 0.6050 0.7526 0.6237 0.014 Uiso 1 1 calc R . .
H11B H 0.6645 0.8742 0.6706 0.014 Uiso 1 1 calc R . .
C12 C 0.63667(17) 0.3790(6) 0.6851(3) 0.0119(7) Uani 1 1 d . . .
H12A H 0.6627 0.2537 0.6787 0.014 Uiso 1 1 calc R . .
H12B H 0.6041 0.3747 0.6282 0.014 Uiso 1 1 calc R . .
N1 N 0.44056(14) 0.9825(5) 0.8253(3) 0.0141(6) Uani 1 1 d . . .
N2 N 0.30822(15) 0.9230(4) 0.8206(3) 0.0139(6) Uani 1 1 d . . .
N3 N 0.60652(13) 0.7612(4) 0.7887(2) 0.0117(6) Uani 1 1 d . . .
N4 N 0.60503(14) 0.3817(5) 0.7935(2) 0.0113(6) Uani 1 1 d . . .
N5 N 0.69725(16) 0.5717(4) 0.8670(3) 0.0098(6) Uani 1 1 d . . .
N6 N 0.67766(15) 0.5628(4) 0.6686(3) 0.0093(6) Uani 1 1 d . . .
O1 O 0.49587(12) 1.1210(5) 0.6280(3) 0.0224(6) Uani 1 1 d . . .
O2 O 0.42767(14) 0.9049(4) 0.5428(2) 0.0201(6) Uani 1 1 d . . .
O3 O 0.28946(14) 1.1210(4) 0.5871(2) 0.0170(6) Uani 1 1 d . . .
O4 O 0.28187(12) 0.7711(4) 0.5919(2) 0.0176(6) Uani 1 1 d . . .
O1W O 0.87778(15) 0.5531(4) 0.8919(3) 0.0245(7) Uani 1 1 d . . .
O2W O 0.50840(15) 0.5394(4) 0.5322(3) 0.0258(7) Uani 1 1 d . . .
O3W O 0.37241(14) 1.4515(4) 0.6560(3) 0.0243(7) Uani 1 1 d . . .
Ag1 Ag 0.774850(13) 0.56477(3) 0.99864(2) 0.01387(8) Uani 1 1 d . . .
Ag2 Ag 0.546314(13) 1.07727(4) 0.82291(3) 0.01633(9) Uani 1 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 C1 C2 120.0(4) . . ?
N1 C1 C5 118.2(3) . . ?
C2 C1 C5 121.7(3) . . ?
N2 C2 C1 122.2(4) . . ?
N2 C2 C6 113.6(3) . . ?
C1 C2 C6 124.1(4) . . ?
N1 C3 C4 120.8(4) . . ?
N1 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N2 C4 C3 121.7(4) . . ?
N2 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
O2 C5 O1 126.9(4) . . ?
O2 C5 C1 115.6(4) . . ?
O1 C5 C1 117.5(4) . . ?
O4 C6 O3 128.0(4) . . ?
O4 C6 C2 116.9(3) . . ?
O3 C6 C2 114.8(3) . . ?
N3 C7 N4 110.8(3) . . ?
N3 C7 H7A 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N5 C8 N3 111.3(3) . . ?
N5 C8 H8A 109.4 . . ?
N3 C8 H8A 109.4 . . ?
N5 C8 H8B 109.4 . . ?
N3 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N5 C9 N4 111.2(3) . . ?
N5 C9 H9A 109.4 . . ?
N4 C9 H9A 109.4 . . ?
N5 C9 H9B 109.4 . . ?
N4 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N5 C10 N6 112.0(3) . . ?
N5 C10 H10A 109.2 . . ?
N6 C10 H10A 109.2 . . ?
N5 C10 H10B 109.2 . . ?
N6 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N6 C11 N3 111.7(3) . . ?
N6 C11 H11A 109.3 . . ?
N3 C11 H11A 109.3 . . ?
N6 C11 H11B 109.3 . . ?
N3 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
N6 C12 N4 111.8(3) . . ?
N6 C12 H12A 109.2 . . ?
N4 C12 H12A 109.2 . . ?
N6 C12 H12B 109.2 . . ?
N4 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C1 N1 C3 118.6(3) . . ?
C1 N1 Ag2 118.0(3) . . ?
C3 N1 Ag2 123.0(3) . . ?
C4 N2 C2 116.5(3) . . ?
C11 N3 C7 108.4(3) . . ?
C11 N3 C8 109.2(3) . . ?
C7 N3 C8 108.4(3) . . ?
C11 N3 Ag2 114.7(2) . . ?
C7 N3 Ag2 111.5(2) . . ?
C8 N3 Ag2 104.34(19) . . ?
C7 N4 C12 108.4(3) . . ?
C7 N4 C9 108.4(3) . . ?
C12 N4 C9 108.8(3) . . ?
C7 N4 Ag2 113.5(2) . 1_545 ?
C12 N4 Ag2 111.2(2) . 1_545 ?
C9 N4 Ag2 106.4(2) . 1_545 ?
C8 N5 C9 107.6(3) . . ?
C8 N5 C10 109.0(3) . . ?
C9 N5 C10 108.5(3) . . ?
C8 N5 Ag1 112.1(2) . . ?
C9 N5 Ag1 109.2(2) . . ?
C10 N5 Ag1 110.3(2) . . ?
C12 N6 C11 108.6(3) . . ?
C12 N6 C10 107.8(3) . . ?
C11 N6 C10 108.0(3) . . ?
C12 N6 Ag1 112.2(2) . 3_654 ?
C11 N6 Ag1 109.0(2) . 3_654 ?
C10 N6 Ag1 111.1(2) . 3_654 ?
N5 Ag1 N6 160.32(11) . 3_655 ?
N5 Ag1 O1W 103.82(12) . . ?
N6 Ag1 O1W 95.85(11) 3_655 . ?
N1 Ag2 N4 136.89(11) . 1_565 ?
N1 Ag2 N3 106.13(11) . . ?
N4 Ag2 N3 113.85(12) 1_565 . ?
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
C1 N1 1.334(5) . ?
C1 C2 1.392(5) . ?
C1 C5 1.528(5) . ?
C2 N2 1.341(6) . ?
C2 C6 1.521(6) . ?
C3 N1 1.332(5) . ?
C3 C4 1.389(6) . ?
C3 H3 0.9300 . ?
C4 N2 1.340(6) . ?
C4 H4 0.9300 . ?
C5 O2 1.249(5) . ?
C5 O1 1.251(5) . ?
C6 O4 1.249(4) . ?
C6 O3 1.250(5) . ?
C7 N3 1.475(4) . ?
C7 N4 1.478(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N5 1.473(4) . ?
C8 N3 1.477(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.474(5) . ?
C9 N4 1.482(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N5 1.475(5) . ?
C10 N6 1.483(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N6 1.473(4) . ?
C11 N3 1.471(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N6 1.467(5) . ?
C12 N4 1.475(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N1 Ag2 2.279(3) . ?
N3 Ag2 2.416(3) . ?
N4 Ag2 2.328(3) 1_545 ?
N5 Ag1 2.274(3) . ?
N6 Ag1 2.294(3) 3_654 ?
O1W Ag1 2.504(3) . ?
Ag1 N6 2.294(3) 3_655 ?
Ag2 N4 2.328(3) 1_565 ?
