#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100137.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_1100137 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Sawsan Salameh' 'Mohammad Abul-Haj' 'Miguel Quiros' 'Juan M. Salas' _journal_name_full 'Inorganica Chimica Acta' _journal_volume 358 _journal_page_first 824 _journal_page_last 827 _journal_year 2005 _chemical_name_systematic ; Di(nitrate)bis(mu-7,8-dihydro-7-oxo-1,2,4-triazolo[4,3-a]pyrimidine-N1,N2) disilver(I) dihydrate ; _chemical_formula_sum 'C10 H12 Ag2 N10 O10' _chemical_formula_weight 648.04 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 monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5297(6) _cell_length_b 12.6897(8) _cell_length_c 6.9432(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.7820(10) _cell_angle_gamma 90.00 _cell_volume 924.51(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3774 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.01 _exptl_crystal_description 'trapezoidal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 2.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4965 _exptl_absorpt_correction_T_max 0.6930 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 298(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 66.06 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5595 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.14 _reflns_number_total 2080 _reflns_number_gt 1912 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2080 _refine_ls_number_parameters 151 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag -0.034602(16) 0.366253(14) 0.47882(3) 0.04028(9) Uani 1 1 d . . . N1 N 0.15620(17) 0.41571(14) 0.3890(3) 0.0311(4) Uani 1 1 d . . . N2 N 0.18306(18) 0.52354(15) 0.4143(3) 0.0345(4) Uani 1 1 d . . . C3 C 0.2960(2) 0.54148(17) 0.3607(3) 0.0323(5) Uani 1 1 d . . . H3 H 0.3362 0.6068 0.3644 0.039 Uiso 1 1 calc R . . N4 N 0.34725(17) 0.44956(13) 0.2983(3) 0.0278(4) Uani 1 1 d . . . C5 C 0.4636(2) 0.42561(18) 0.2279(3) 0.0326(5) Uani 1 1 d . . . H5 H 0.5234 0.4780 0.2104 0.039 Uiso 1 1 calc R . . C6 C 0.4873(2) 0.32501(19) 0.1866(4) 0.0351(5) Uani 1 1 d . . . H6 H 0.5644 0.3079 0.1381 0.042 Uiso 1 1 calc R . . C7 C 0.3965(2) 0.24136(17) 0.2140(3) 0.0299(4) Uani 1 1 d . . . O7 O 0.41724(18) 0.14841(12) 0.1839(3) 0.0391(4) Uani 1 1 d . . . N8 N 0.28107(17) 0.27263(14) 0.2769(3) 0.0299(4) Uani 1 1 d . . . H8 H 0.2228 0.2261 0.2885 0.036 Uiso 1 1 calc R . . C8A C 0.2569(2) 0.37471(15) 0.3210(3) 0.0263(4) Uani 1 1 d . . . N1N N -0.18750(19) 0.16666(16) 0.5373(3) 0.0340(4) Uani 1 1 d . . . O1N O -0.07156(17) 0.18332(16) 0.5922(3) 0.0480(4) Uani 1 1 d . . . O2N O -0.24949(19) 0.23627(14) 0.4477(3) 0.0484(4) Uani 1 1 d . . . O3N O -0.2380(2) 0.08141(14) 0.5736(3) 0.0508(5) Uani 1 1 d . . . O1W O 0.1119(2) 0.11319(15) 0.3519(3) 0.0483(5) Uani 1 1 d D . . H11W H 0.059(3) 0.115(3) 0.438(4) 0.058 Uiso 1 1 d D . . H12W H 0.142(3) 0.0506(13) 0.369(5) 0.058 Uiso 1 1 d D . . 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 Ag 0.03116(12) 0.03170(12) 0.05990(15) -0.00673(8) 0.01517(9) -0.00173(7) N1 0.0279(9) 0.0223(9) 0.0441(11) -0.0045(8) 0.0088(8) -0.0015(7) N2 0.0322(9) 0.0231(9) 0.0493(12) -0.0051(8) 0.0099(8) 0.0014(7) C3 0.0317(11) 0.0210(10) 0.0448(13) -0.0012(9) 0.0064(9) 0.0011(8) N4 0.0260(9) 0.0212(8) 0.0368(10) 0.0014(7) 0.0062(7) -0.0001(7) C5 0.0262(11) 0.0298(11) 0.0432(13) 0.0015(9) 0.0107(9) -0.0021(8) C6 0.0276(11) 0.0353(12) 0.0438(13) -0.0030(10) 0.0116(9) 0.0020(9) C7 0.0308(11) 0.0269(10) 0.0321(11) -0.0018(8) 0.0037(9) 0.0050(8) O7 0.0421(10) 0.0262(8) 0.0494(10) -0.0063(7) 0.0059(8) 0.0080(7) N8 0.0287(9) 0.0209(8) 0.0408(10) -0.0032(7) 0.0070(7) -0.0016(7) C8A 0.0263(10) 0.0221(10) 0.0310(11) 0.0003(8) 0.0047(8) -0.0006(7) N1N 0.0350(10) 0.0288(9) 0.0395(11) -0.0023(8) 0.0112(8) 0.0003(8) O1N 0.0328(9) 0.0547(12) 0.0571(12) -0.0004(9) 0.0074(8) -0.0028(8) O2N 0.0527(11) 0.0334(9) 0.0587(12) 0.0067(8) 0.0027(9) 0.0060(8) O3N 0.0523(11) 0.0296(9) 0.0721(13) 0.0072(9) 0.0143(10) -0.0054(8) O1W 0.0492(11) 0.0317(9) 0.0674(13) 0.0017(9) 0.0251(10) -0.0025(8) _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 Ag N1 2.2423(18) . ? Ag N2 2.2680(19) 3_566 ? Ag O1N 2.492(2) . ? N1 C8A 1.304(3) . ? N1 N2 1.405(3) . ? N2 C3 1.295(3) . ? N2 Ag 2.2679(19) 3_566 ? C3 N4 1.371(3) . ? C3 H3 0.9300 . ? N4 C8A 1.363(3) . ? N4 C5 1.390(3) . ? C5 C6 1.336(3) . ? C5 H5 0.9300 . ? C6 C7 1.451(3) . ? C6 H6 0.9300 . ? C7 O7 1.221(3) . ? C7 N8 1.384(3) . ? N8 C8A 1.360(3) . ? N8 H8 0.8600 . ? N1N O2N 1.235(3) . ? N1N O3N 1.240(3) . ? N1N O1N 1.266(3) . ? O1W H11W 0.856(10) . ? O1W H12W 0.860(10) . ? 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 Ag N2 125.20(6) . 3_566 ? N1 Ag O1N 121.04(6) . . ? N2 Ag O1N 109.94(7) 3_566 . ? C8A N1 N2 105.80(17) . . ? C8A N1 Ag 139.76(15) . . ? N2 N1 Ag 114.42(13) . . ? C3 N2 N1 108.38(18) . . ? C3 N2 Ag 131.29(15) . 3_566 ? N1 N2 Ag 120.28(14) . 3_566 ? N2 C3 N4 109.65(19) . . ? N2 C3 H3 125.1 . . ? N4 C3 H3 125.2 . . ? C8A N4 C3 105.04(17) . . ? C8A N4 C5 122.17(18) . . ? C3 N4 C5 132.78(19) . . ? C6 C5 N4 118.0(2) . . ? C6 C5 H5 121.0 . . ? N4 C5 H5 121.0 . . ? C5 C6 C7 122.3(2) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 118.7 . . ? O7 C7 N8 120.3(2) . . ? O7 C7 C6 123.7(2) . . ? N8 C7 C6 115.91(19) . . ? C8A N8 C7 122.00(18) . . ? C8A N8 H8 119.0 . . ? C7 N8 H8 119.0 . . ? N1 C8A N8 129.4(2) . . ? N1 C8A N4 111.12(18) . . ? N8 C8A N4 119.50(19) . . ? O2N N1N O3N 120.6(2) . . ? O2N N1N O1N 119.2(2) . . ? O3N N1N O1N 120.2(2) . . ? N1N O1N Ag 103.45(15) . . ? H11W O1W H12W 101(3) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.599 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.073 _cod_database_code 1100137