# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1176

data_aghmt

#====================================================================

# 1. SUBMISSION DETAILS

_publ_contact_author          # Name and address of author for correspondence
;
      Chen, Xiao-Ming
      School of Chemistry and Chemical Engineering
      Zhongshan University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_phone '86-20-84186300 ext 2074'
_publ_contact_author_fax    '86 20 4189173'
_publ_contact_author_email  cedc03@zsu.edu.cn
_publ_requested_joiurnal    ' J. Chem. Soc., Chem. Commun.'
_publ_requested_coeditor_name ?
_publ_contact_letter
;
 
;

#=======================================================================


# 3. TITLE AND AUTHOR LIST

_publ_section_title
;
Two- and three-dimensional non-interpenetrating open-networks 
self-assembled by m4-hexamethanetetraamine (hmt). 
Syntheses and structures of [Ag2(m4-hmt)(SO4)(H2O)](4H2O 
and [Ag2(m4-hmt)(m2-O2CCH3)](CH3CO2)(4.5H2O 
;

loop_
 _publ_author_name
 _publ_author_address
     'Tong, Ming-Liang'
;     School of Chemistry and Chemical Engineering
      Zhongshan University 
      Guangzhou 510275
      P. R. China
;
      'Zheng, Shao-Liang'
;     School of Chemistry and Chemical Engineering
      Zhongshan University 
      Guangzhou 510275
      P. R. China
;
      'Chen, Xiao-Ming '
;     School of Chemistry and Chemical Engineering
      Zhongshan University 
      Guangzhou 510275
      P. R. China
;
#============================================================ 
data_complex1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C6 H22 Ag2 N4 O9 S' 
_chemical_formula_weight          542.08 
 
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' 
 'Ag'  'Ag'  -0.8971   1.1015 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    Cc 
 
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' 
 
_cell_length_a                    6.362(6) 
_cell_length_b                    18.813(13) 
_cell_length_c                    12.552(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.64(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      1501.7(18) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       7.5 
_cell_measurement_theta_max       15 
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.60
_exptl_crystal_size_mid           0.40
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.398 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1072 
_exptl_absorpt_coefficient_mu     2.798 
_exptl_absorpt_correction_type    'y-scans (North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min   0.421 
_exptl_absorpt_correction_T_max   0.991 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Siemens R3m' 
_diffrn_measurement_method        '\w scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  120 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2177 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0150 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          29.06 
_reflns_number_total              2177 
_reflns_number_gt                 2136 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'P3/R3 Nicolet (Nicolet XRD, 1980)'
_computing_cell_refinement        'SHELXTL Plus (Siemens, 1990)'
_computing_data_reduction         'SHELXTL Plus (Siemens, 1990)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Johnson, 1997)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+3.0752P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0094(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.03(4) 
_refine_ls_number_reflns          2177 
_refine_ls_number_parameters      200 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0266 
_refine_ls_R_factor_gt            0.0259 
_refine_ls_wR_factor_ref          0.0662 
_refine_ls_wR_factor_gt           0.0658 
_refine_ls_goodness_of_fit_ref    1.071 
_refine_ls_restrained_S_all       1.070 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
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 -0.00399(5) 0.00861(2) 0.49078(4) 0.02644(12) Uani 1 d . . . 
Ag2 Ag 0.51735(6) -0.22172(2) 0.26771(4) 0.02880(13) Uani 1 d . . . 
S1 S 0.50215(18) 0.07467(7) 0.39203(9) 0.0188(2) Uani 1 d . . . 
O1 O 0.2794(6) 0.0887(3) 0.4118(4) 0.0327(9) Uani 1 d . . . 
O2 O 0.5226(8) 0.0416(3) 0.2869(3) 0.0349(9) Uani 1 d . . . 
O3 O 0.6197(7) 0.1417(2) 0.3979(4) 0.0351(9) Uani 1 d . . . 
O4 O 0.5882(8) 0.0262(3) 0.4720(4) 0.0368(10) Uani 1 d . . . 
N1 N 0.0132(6) -0.0615(2) 0.3420(3) 0.0170(7) Uani 1 d . . . 
N2 N 0.2074(6) -0.1542(2) 0.2546(3) 0.0159(7) Uani 1 d . . . 
N3 N 0.0069(6) -0.0683(2) 0.1488(3) 0.0157(7) Uani 1 d . . . 
N4 N -0.1749(6) -0.1577(2) 0.2524(3) 0.0165(7) Uani 1 d . . . 
C1 C 0.0065(9) -0.0205(3) 0.2412(4) 0.0177(8) Uani 1 d . . . 
H1A H 0.1261 0.0106 0.2392 0.080 Uiso 1 d R . . 
H1B H -0.1182 0.0082 0.2381 0.080 Uiso 1 d R . . 
C2 C -0.1714(7) -0.1086(3) 0.3424(4) 0.0173(8) Uani 1 d . . . 
H2A H -0.2966 -0.0801 0.3392 0.080 Uiso 1 d R . . 
H2B H -0.1709 -0.1351 0.4077 0.080 Uiso 1 d R . . 
C3 C 0.2041(8) -0.1057(3) 0.3451(4) 0.0190(9) Uani 1 d . . . 
H3A H 0.2100 -0.1326 0.4102 0.080 Uiso 1 d R . . 
H3B H 0.3255 -0.0755 0.3443 0.080 Uiso 1 d R . . 
C4 C 0.1985(8) -0.1121(3) 0.1547(4) 0.0180(8) Uani 1 d . . . 
H4A H 0.2003 -0.1438 0.0947 0.080 Uiso 1 d R . . 
H4B H 0.3198 -0.0819 0.1518 0.080 Uiso 1 d R . . 
C5 C -0.1779(8) -0.1158(3) 0.1526(4) 0.0195(9) Uani 1 d . . . 
H5A H -0.1786 -0.1474 0.0926 0.080 Uiso 1 d R . . 
H5B H -0.3039 -0.0877 0.1482 0.080 Uiso 1 d R . . 
C6 C 0.0191(9) -0.1997(2) 0.2562(4) 0.0194(8) Uani 1 d . . . 
H6A H 0.0231 -0.2281 0.3197 0.080 Uiso 1 d R . . 
H6B H 0.0192 -0.2312 0.1960 0.080 Uiso 1 d R . . 
O1W O 0.4815(7) -0.3420(2) 0.2962(3) 0.0275(8) Uani 1 d . . . 
H1WA H 0.3755 -0.3496 0.3172 0.080 Uiso 1 d R . . 
H1WB H 0.5990 -0.3805 0.3201 0.050 Uiso 1 d R . . 
O2W O 0.5638(9) 0.3763(3) 0.5879(4) 0.0444(12) Uani 1 d . . . 
H2WA H 0.5170 0.3730 0.6550 0.080 Uiso 1 d R . . 
H2WB H 0.5960 0.3408 0.6110 0.080 Uiso 1 d R . . 
O3W O 0.4491(11) 0.2373(3) 0.5420(5) 0.0483(14) Uani 1 d . . . 
H3WA H 0.4801 0.2096 0.4959 0.080 Uiso 1 d R . . 
H3WB H 0.5048 0.2742 0.5487 0.080 Uiso 1 d R . . 
O4W O 0.5299(12) -0.2226(3) 0.4871(6) 0.0551(17) Uani 1 d . . . 
H4WA H 0.4187 -0.2034 0.5097 0.080 Uiso 1 d R . . 
H4WB H 0.5377 -0.2652 0.5093 0.080 Uiso 1 d R . . 
O5W O 0.4808(11) 0.0898(3) 0.0875(4) 0.0514(14) Uani 1 d . . . 
H5WA H 0.4977 0.0822 0.0094 0.080 Uiso 1 d R . . 
H5WB H 0.6258 0.1010 0.1028 0.080 Uiso 1 d R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ag1 0.0352(2) 0.0265(2) 0.01770(16) -0.01003(16) 0.00155(13) 0.00010(17) 
Ag2 0.02103(17) 0.02117(19) 0.0442(3) 0.00258(16) 0.00095(15) -0.00146(15) 
S1 0.0177(5) 0.0212(5) 0.0175(5) -0.0011(4) 0.0008(4) -0.0009(4) 
O1 0.0193(17) 0.041(2) 0.038(2) 0.0042(18) 0.0054(16) 0.0010(16) 
O2 0.041(2) 0.040(2) 0.023(2) -0.0061(18) 0.0061(18) 0.001(2) 
O3 0.034(2) 0.026(2) 0.045(3) -0.0033(18) 0.0106(19) -0.0074(18) 
O4 0.035(2) 0.036(2) 0.039(2) 0.0078(19) -0.0071(19) -0.0005(19) 
N1 0.0187(18) 0.0167(18) 0.0155(17) -0.0021(14) 0.0018(14) -0.0010(15) 
N2 0.0174(18) 0.0178(18) 0.0125(17) 0.0017(13) 0.0013(13) 0.0039(14) 
N3 0.0160(18) 0.0179(16) 0.0133(16) 0.0026(13) 0.0028(13) 0.0020(14) 
N4 0.0158(17) 0.0186(18) 0.0150(17) 0.0016(14) -0.0016(13) 0.0011(15) 
C1 0.021(2) 0.016(2) 0.0154(18) 0.0015(19) 0.0008(16) 0.0015(18) 
C2 0.017(2) 0.019(2) 0.016(2) 0.0021(16) 0.0031(16) -0.0001(16) 
C3 0.018(2) 0.022(2) 0.017(2) -0.0009(17) -0.0018(15) 0.0018(17) 
C4 0.019(2) 0.021(2) 0.0143(19) 0.0021(16) 0.0039(15) 0.0038(17) 
C5 0.018(2) 0.022(2) 0.018(2) 0.0024(17) -0.0036(16) -0.0031(17) 
C6 0.0202(18) 0.0183(19) 0.020(2) -0.0004(18) -0.0003(16) 0.001(2) 
O1W 0.028(2) 0.0237(18) 0.031(2) 0.0012(15) 0.0082(15) -0.0027(15) 
O2W 0.065(3) 0.044(3) 0.025(2) -0.0021(19) 0.004(2) -0.002(3) 
O3W 0.073(4) 0.030(2) 0.042(3) -0.003(2) 0.017(3) -0.006(3) 
O4W 0.073(5) 0.041(3) 0.051(3) 0.004(3) 0.003(3) -0.004(3) 
O5W 0.071(4) 0.050(3) 0.033(3) 0.004(2) -0.001(2) 0.017(3) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are 
taken 
 into account individually in the estimation of esds in distances, 
angles 
 and torsion angles; correlations between esds in cell parameters are 
only 
 used when they are defined by crystal symmetry.  An approximate 
(isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. 
planes. 
; 
 
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 N3 2.279(4) 2 ? 
Ag1 N1 2.292(4) . ? 
Ag1 O1 2.571(5) . ? 
Ag2 O1W 2.303(4) . ? 
Ag2 N4 2.311(4) 1_655 ? 
Ag2 N2 2.347(4) . ? 
S1 O4 1.452(5) . ? 
S1 O3 1.467(4) . ? 
S1 O2 1.468(4) . ? 
S1 O1 1.469(4) . ? 
N1 C2 1.471(6) . ? 
N1 C3 1.471(6) . ? 
N1 C1 1.481(6) . ? 
N2 C3 1.459(6) . ? 
N2 C6 1.472(7) . ? 
N2 C4 1.483(6) . ? 
N3 C1 1.468(6) . ? 
N3 C4 1.472(6) . ? 
N3 C5 1.478(6) . ? 
N3 Ag1 2.279(4) 2_554 ? 
N4 C2 1.459(6) . ? 
N4 C6 1.465(6) . ? 
N4 C5 1.480(6) . ? 
N4 Ag2 2.311(4) 1_455 ? 
O1W O3 2.681(6) 3_445 ? 
O1W O1 2.691(7) 3_545 ? 
O2 O5W 2.669(7) . ? 
O3 O3W 2.792(8) . ? 
O2W O1W 2.758(6) 2 ? 
O2W O3W 2.770(8) . ? 
O4W O5W 2.818(8) 2 ? 
O4W O3W 2.838(10) 3_545 ? 
O5W O4 2.718(8) 2_554 ? 
O5W O2W 2.728(9) 4_454 ? 
 
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 
N3 Ag1 N1 172.81(15) 2 . ? 
N3 Ag1 O1 92.44(15) 2 . ? 
N1 Ag1 O1 88.44(16) . . ? 
O1W Ag2 N4 127.80(15) . 1_655 ? 
O1W Ag2 N2 117.09(15) . . ? 
N4 Ag2 N2 115.10(14) 1_655 . ? 
O4 S1 O3 108.9(3) . . ? 
O4 S1 O2 108.3(3) . . ? 
O3 S1 O2 110.6(3) . . ? 
O4 S1 O1 110.0(3) . . ? 
O3 S1 O1 109.2(3) . . ? 
O2 S1 O1 109.8(3) . . ? 
S1 O1 Ag1 130.6(3) . . ? 
S1 O2 O5W 133.6(3) . . ? 
S1 O3 O3W 112.3(3) . . ? 
C2 N1 C3 108.5(4) . . ? 
C2 N1 C1 108.3(4) . . ? 
C3 N1 C1 108.7(4) . . ? 
C2 N1 Ag1 106.7(3) . . ? 
C3 N1 Ag1 111.2(3) . . ? 
C1 N1 Ag1 113.3(3) . . ? 
C3 N2 C6 108.8(4) . . ? 
C3 N2 C4 108.9(4) . . ? 
C6 N2 C4 108.1(4) . . ? 
C3 N2 Ag2 108.3(3) . . ? 
C6 N2 Ag2 111.6(3) . . ? 
C4 N2 Ag2 111.1(3) . . ? 
C1 N3 C4 108.9(4) . . ? 
C1 N3 C5 109.0(4) . . ? 
C4 N3 C5 108.6(4) . . ? 
C1 N3 Ag1 112.6(3) . 2_554 ? 
C4 N3 Ag1 108.9(3) . 2_554 ? 
C5 N3 Ag1 108.8(3) . 2_554 ? 
C2 N4 C6 108.8(4) . . ? 
C2 N4 C5 108.5(4) . . ? 
C6 N4 C5 107.7(4) . . ? 
C2 N4 Ag2 105.1(3) . 1_455 ? 
C6 N4 Ag2 115.5(3) . 1_455 ? 
C5 N4 Ag2 111.0(3) . 1_455 ? 
N3 C1 N1 110.8(4) . . ? 
N4 C2 N1 111.9(4) . . ? 
N2 C3 N1 111.3(4) . . ? 
N3 C4 N2 110.7(4) . . ? 
N3 C5 N4 111.0(4) . . ? 
N4 C6 N2 111.8(4) . . ? 
Ag2 O1W O3 106.06(18) . 3_445 ? 
Ag2 O1W O1 119.2(2) . 3_545 ? 
O3 O1W O1 106.8(2) 3_445 3_545 ? 
O1W O2W O3W 85.4(2) 2 . ? 
O2W O3W O3 129.6(3) . . ? 
O5W O4W O3W 104.0(3) 2 3_545 ? 
O2 O5W O4 101.9(2) . 2_554 ? 
O2 O5W O2W 98.6(2) . 4_454 ? 
O4 O5W O2W 116.6(3) 2_554 4_454 ? 
 
_diffrn_measured_fraction_theta_max    0.500 
_diffrn_reflns_theta_full              29.06 
_diffrn_measured_fraction_theta_full   0.500 
_refine_diff_density_max    0.896 
_refine_diff_density_min   -0.666 
_refine_diff_density_rms    0.126 
#============================================================END
 
data_complex2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C10 H27 Ag2 N4 O8.50' 
_chemical_formula_weight          555.10 
 
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' 
 
_symmetry_cell_setting            Orthorhmobic 
_symmetry_space_group_name_H-M    Pbcn 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-x, y, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y-1/2, -z-1/2' 
 'x, -y, z-1/2' 
 '-x-1/2, y-1/2, z' 
 
_cell_length_a                    22.7015(3) 
_cell_length_b                    12.1200(2) 
_cell_length_c                    12.9889(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3573.79(9) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       7.5 
_cell_measurement_theta_max       15 
 
_exptl_crystal_description        polyhedral 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.46 
_exptl_crystal_size_mid           0.36 
_exptl_crystal_size_min           0.22 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.063 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2216 
_exptl_absorpt_coefficient_mu     2.240 
_exptl_absorpt_correction_type    'y-scans (North, Phillips & Mathews, 1968)'
_exptl_absorpt_correction_T_min   0.622
_exptl_absorpt_correction_T_max   0.884
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Siemens R3m' 
_diffrn_measurement_method        '\w scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  120 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3180 
_diffrn_reflns_av_R_equivalents   0.0307 
_diffrn_reflns_av_sigmaI/netI     0.0286 
_diffrn_reflns_limit_h_min        -20 
_diffrn_reflns_limit_h_max        27 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          1.79 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              3147 
_reflns_number_gt                 2567 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'P3/R3 Nicolet (Nicolet XRD, 1980)'
_computing_cell_refinement        'SHELXTL Plus (Siemens, 1990)'
_computing_data_reduction         'SHELXTL Plus (Siemens, 1990)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Johnson, 1997)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+13.1038P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3147 
_refine_ls_number_parameters      235 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0617 
_refine_ls_R_factor_gt            0.0487 
_refine_ls_wR_factor_ref          0.1335 
_refine_ls_wR_factor_gt           0.1251 
_refine_ls_goodness_of_fit_ref    1.076 
_refine_ls_restrained_S_all       1.076 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 0.058106(18) 0.50977(3) 0.04679(3) 0.02783(18) Uani 1 d . . . 
Ag2 Ag 0.24843(2) 0.24992(4) 0.29954(5) 0.0509(2) Uani 1 d . . . 
O11 O 0.01205(19) 0.6814(3) 0.0795(3) 0.0421(10) Uani 1 d . . . 
O12 O -0.0171(2) 0.6680(4) -0.0820(4) 0.0493(12) Uani 1 d . . . 
N1 N 0.11572(19) 0.5039(3) 0.2021(3) 0.0210(9) Uani 1 d . . . 
N2 N 0.19059(19) 0.3996(4) 0.2966(3) 0.0244(10) Uani 1 d . . . 
N3 N 0.11393(18) 0.5008(3) 0.3899(3) 0.0222(9) Uani 1 d . . . 
N4 N 0.19128(18) 0.6021(4) 0.2988(3) 0.0226(10) Uani 1 d . . . 
C1 C 0.1530(2) 0.4043(4) 0.2033(4) 0.0222(12) Uani 1 d . . . 
H1C H 0.1779 0.4038 0.1425 0.080 Uiso 1 d R . . 
H1D H 0.1282 0.3393 0.2009 0.080 Uiso 1 d R . . 
C2 C 0.1516(2) 0.4013(4) 0.3875(4) 0.0249(12) Uani 1 d . . . 
H2C H 0.1754 0.3989 0.4495 0.080 Uiso 1 d R . . 
H2D H 0.1267 0.3362 0.3868 0.080 Uiso 1 d R . . 
C3 C 0.0782(2) 0.5028(4) 0.2952(4) 0.0231(11) Uani 1 d . . . 
H3C H 0.0533 0.5679 0.2954 0.080 Uiso 1 d R . . 
H3D H 0.0528 0.4384 0.2936 0.080 Uiso 1 d R . . 
C4 C 0.1541(2) 0.6025(4) 0.2055(4) 0.0255(12) Uani 1 d . . . 
H4A H 0.1790 0.6039 0.1448 0.080 Uiso 1 d R . . 
H4B H 0.1299 0.6685 0.2049 0.080 Uiso 1 d R . . 
C5 C 0.2280(2) 0.5012(4) 0.2985(4) 0.0266(12) Uani 1 d . . . 
H5A H 0.2526 0.5002 0.3595 0.080 Uiso 1 d R . . 
H5B H 0.2535 0.5018 0.2386 0.080 Uiso 1 d R . . 
C6 C 0.1526(2) 0.6000(4) 0.3912(4) 0.0226(11) Uani 1 d . . . 
H6A H 0.1766 0.5993 0.4529 0.080 Uiso 1 d R . . 
H6B H 0.1284 0.6661 0.3926 0.080 Uiso 1 d R . . 
C11 C -0.0078(2) 0.7220(5) -0.0012(5) 0.0317(13) Uani 1 d . . . 
C12 C -0.0222(3) 0.8434(5) -0.0039(5) 0.0502(17) Uani 1 d . . . 
H12A H -0.0369 0.8626 -0.0708 0.080 Uiso 1 d R . . 
H12B H 0.0128 0.8853 0.0102 0.080 Uiso 1 d R . . 
H12C H -0.0515 0.8597 0.0472 0.080 Uiso 1 d R . . 
C21 C 0.2978(3) 0.6310(6) 0.5431(6) 0.0484(17) Uani 1 d . . . 
C22 C 0.3625(3) 0.6194(7) 0.5367(7) 0.066(2) Uani 1 d . . . 
H22A H 0.3731 0.5435 0.5473 0.080 Uiso 1 d R . . 
H22B H 0.3807 0.6642 0.5886 0.080 Uiso 1 d R . . 
H22C H 0.3758 0.6427 0.4699 0.080 Uiso 1 d R . . 
O21 O 0.2662(2) 0.5434(4) 0.5480(4) 0.0516(12) Uani 1 d . . . 
O22 O 0.2753(3) 0.7203(5) 0.5321(10) 0.157(5) Uani 1 d . . . 
O1W O 0.1435(3) 0.1239(6) 0.2551(6) 0.105(2) Uani 1 d . . . 
H1WA H 0.1001 0.1198 0.2592 0.080 Uiso 1 d R . . 
H1WB H 0.1496 0.1492 0.1743 0.080 Uiso 1 d R . . 
O2W O 0.1808(3) 0.1511(5) 0.0426(7) 0.115(3) Uani 1 d . . . 
H2WA H 0.1989 0.1653 0.1158 0.080 Uiso 1 d R . . 
H2WB H 0.2089 0.1730 -0.0033 0.080 Uiso 1 d R . . 
O3W O 0.1461(3) 0.8742(6) 0.3232(6) 0.104(2) Uani 1 d . . . 
H3WA H 0.1194 0.8369 0.2894 0.080 Uiso 1 d R . . 
H3WB H 0.1302 0.9401 0.3259 0.080 Uiso 1 d R . . 
O4W O 0.0289(4) 0.8013(8) 0.2510(8) 0.061(3) Uani 0.50 d P . . 
O5W O 0.0277(5) 0.2113(8) 0.2568(8) 0.067(3) Uani 0.50 d P . . 
O6W O 0.0385(10) 0.0086(12) 0.258(2) 0.141(7) Uani 0.50 d P . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ag1 0.0284(3) 0.0311(3) 0.0240(3) 0.00013(17) -0.00356(16) 0.00058(16) 
Ag2 0.0478(3) 0.0373(3) 0.0675(4) -0.0074(2) -0.0113(2) 0.0246(2) 
O11 0.049(3) 0.034(2) 0.043(3) 0.002(2) 0.001(2) 0.0067(19) 
O12 0.071(3) 0.034(2) 0.043(3) 0.000(2) 0.003(2) -0.010(2) 
N1 0.021(2) 0.020(2) 0.022(2) -0.0004(16) -0.0003(16) 0.0011(17) 
N2 0.024(2) 0.021(2) 0.027(3) -0.0006(17) -0.0027(17) 0.0014(18) 
N3 0.022(2) 0.023(2) 0.022(2) 0.0044(16) 0.0020(17) 0.0010(17) 
N4 0.021(2) 0.024(2) 0.023(2) 0.0004(17) -0.0004(17) -0.0043(17) 
C1 0.026(3) 0.023(3) 0.017(3) -0.006(2) -0.0022(19) 0.000(2) 
C2 0.031(3) 0.023(3) 0.021(3) 0.005(2) -0.001(2) 0.002(2) 
C3 0.020(2) 0.033(3) 0.016(3) -0.004(2) -0.0033(19) 0.004(2) 
C4 0.025(3) 0.022(3) 0.029(3) 0.005(2) -0.003(2) -0.006(2) 
C5 0.022(3) 0.028(3) 0.029(3) -0.004(2) -0.001(2) 0.002(2) 
C6 0.024(3) 0.024(3) 0.020(3) -0.001(2) 0.003(2) -0.002(2) 
C11 0.032(3) 0.029(3) 0.035(3) -0.003(3) 0.002(3) -0.003(2) 
C12 0.064(4) 0.036(4) 0.051(4) 0.002(3) -0.007(3) 0.012(3) 
C21 0.038(4) 0.040(4) 0.067(5) 0.001(3) -0.004(3) 0.000(3) 
C22 0.042(4) 0.058(5) 0.098(7) 0.008(4) -0.007(4) -0.004(3) 
O21 0.042(3) 0.051(3) 0.061(3) 0.003(2) 0.003(2) -0.001(2) 
O22 0.054(4) 0.041(3) 0.375(15) 0.027(6) -0.004(6) 0.004(3) 
O1W 0.081(5) 0.113(6) 0.120(6) -0.022(5) -0.031(4) 0.023(4) 
O2W 0.078(5) 0.067(4) 0.200(9) 0.002(5) 0.016(5) -0.011(4) 
O3W 0.077(5) 0.086(5) 0.150(7) -0.026(5) 0.026(4) -0.014(4) 
O4W 0.087(7) 0.056(6) 0.040(6) -0.001(5) 0.012(6) -0.017(5) 
O5W 0.101(8) 0.051(6) 0.049(6) 0.006(5) 0.004(7) 0.023(5) 
O6W 0.150(16) 0.097(13) 0.175(18) 0.024(11) 0.032(18) 0.002(10) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are 
taken 
 into account individually in the estimation of esds in distances, 
angles 
 and torsion angles; correlations between esds in cell parameters are 
only 
 used when they are defined by crystal symmetry.  An approximate 
(isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. 
planes. 
; 
 
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 O11 2.366(4) . ? 
Ag1 O12 2.391(4) 5_565 ? 
Ag1 N3 2.403(4) 7_565 ? 
Ag1 N1 2.405(4) . ? 
Ag1 Ag1 2.9144(8) 5_565 ? 
Ag2 N2 2.240(4) . ? 
Ag2 N4 2.254(4) 8_655 ? 
O11 C11 1.243(7) . ? 
O12 C11 1.255(7) . ? 
O12 Ag1 2.391(4) 5_565 ? 
N1 C1 1.475(6) . ? 
N1 C3 1.479(6) . ? 
N1 C4 1.480(6) . ? 
N2 C2 1.477(6) . ? 
N2 C1 1.483(6) . ? 
N2 C5 1.495(7) . ? 
N3 C3 1.475(6) . ? 
N3 C2 1.478(6) . ? 
N3 C6 1.489(6) . ? 
N3 Ag1 2.403(4) 7_566 ? 
N4 C4 1.477(6) . ? 
N4 C5 1.480(7) . ? 
N4 C6 1.487(6) . ? 
N4 Ag2 2.254(4) 8_665 ? 
C11 C12 1.508(8) . ? 
C21 O22 1.205(9) . ? 
C21 O21 1.283(8) . ? 
C21 C22 1.479(10) . ? 
O1W O6W 2.76(2) . ? 
O1W O5W 2.835(12) . ? 
O1W O2W 2.905(12) . ? 
O2W O22 2.655(9) 7_565 ? 
O3W O4W 2.956(12) . ? 
O3W O6W 3.06(2) 1_565 ? 
O3W O1W 3.154(12) 1_565 ? 

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 
O11 Ag1 O12 125.84(17) . 5_565 ? 
O11 Ag1 N3 115.61(14) . 7_565 ? 
O12 Ag1 N3 108.63(14) 5_565 7_565 ? 
O11 Ag1 N1 96.64(15) . . ? 
O12 Ag1 N1 91.41(15) 5_565 . ? 
N3 Ag1 N1 115.01(15) 7_565 . ? 
O11 Ag1 Ag1 75.31(11) . 5_565 ? 
O12 Ag1 Ag1 69.77(12) 5_565 5_565 ? 
N3 Ag1 Ag1 96.86(10) 7_565 5_565 ? 
N1 Ag1 Ag1 147.10(10) . 5_565 ? 
N2 Ag2 N4 178.08(15) . 8_655 ? 
C11 O11 Ag1 110.9(4) . . ? 
C11 O12 Ag1 112.1(4) . 5_565 ? 
C1 N1 C3 108.4(4) . . ? 
C1 N1 C4 108.8(4) . . ? 
C3 N1 C4 108.8(4) . . ? 
C1 N1 Ag1 110.2(3) . . ? 
C3 N1 Ag1 111.9(3) . . ? 
C4 N1 Ag1 108.7(3) . . ? 
C2 N2 C1 108.0(4) . . ? 
C2 N2 C5 108.4(4) . . ? 
C1 N2 C5 107.9(4) . . ? 
C2 N2 Ag2 110.5(3) . . ? 
C1 N2 Ag2 112.4(3) . . ? 
C5 N2 Ag2 109.5(3) . . ? 
C3 N3 C2 108.3(4) . . ? 
C3 N3 C6 108.7(4) . . ? 
C2 N3 C6 108.6(4) . . ? 
C3 N3 Ag1 114.7(3) . 7_566 ? 
C2 N3 Ag1 106.2(3) . 7_566 ? 
C6 N3 Ag1 110.2(3) . 7_566 ? 
C4 N4 C5 108.7(4) . . ? 
C4 N4 C6 109.0(4) . . ? 
C5 N4 C6 108.7(4) . . ? 
C4 N4 Ag2 110.4(3) . 8_665 ? 
C5 N4 Ag2 108.4(3) . 8_665 ? 
C6 N4 Ag2 111.7(3) . 8_665 ? 
N1 C1 N2 111.7(4) . . ? 
N2 C2 N3 112.0(4) . . ? 
N3 C3 N1 111.4(4) . . ? 
N4 C4 N1 111.0(4) . . ? 
N4 C5 N2 111.2(4) . . ? 
N4 C6 N3 110.7(4) . . ? 
O11 C11 O12 124.0(6) . . ? 
O11 C11 C12 119.0(5) . . ? 
O12 C11 C12 116.9(6) . . ? 
O22 C21 O21 120.9(7) . . ? 
O22 C21 C22 119.9(7) . . ? 
O21 C21 C22 118.6(6) . . ? 
O6W O1W O5W 52.3(4) . . ? 
O6W O1W O2W 108.8(6) . . ? 
O5W O1W O2W 103.6(4) . . ? 
O22 O2W O1W 110.6(4) 7_565 . ? 
O4W O3W O6W 49.6(4) . 1_565 ? 
O4W O3W O1W 100.5(3) . 1_565 ? 
O6W O3W O1W 52.9(4) 1_565 1_565 ? 
O4W O4W O3W 155.0(7) 3 . ? 
O5W O5W O1W 156.6(5) 3 . ? 
O6W O6W O1W 148.7(7) 3 . ? 
 
_diffrn_measured_fraction_theta_max    0.884 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.884 
_refine_diff_density_max    1.816 
_refine_diff_density_min   -0.768 
_refine_diff_density_rms    0.135 

#_eof
#End of Crystallographic Information File