#------------------------------------------------------------------------------ #$Date: 2012-02-28 12:14:52 +0000 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100148.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_1100148 _journal_name_full 'Acta Crystallographica Section E' _journal_volume 59 loop_ _publ_author_name 'Mohammad Abul-Haj' 'Miguel Quiros' 'Juan M. Salas' _publ_section_title ; Diaquabis(nitrato-O)bis(4,7-dihydro-1,2,4-triazolo [1,5-a]pyrimidine-7-one-N^3^)copper(II). ; _journal_page_first m903 _journal_page_last m905 _journal_year 2003 _publ_section_exptl_refinement ; Hydrogen atoms of the organic moiety were idealized. Those of water molecule were located in the \DF map and refined with restrained O-H distance (0.86 \%A). Isotropic thermal parameters of all hydrogen atoms fixed to 1.2 times the Ueq of their parent atoms. ; _chemical_formula_sum 'C10 H12 Cu N10 O10' _chemical_formula_moiety 'C10 H12 Cu N10 O10' _chemical_formula_weight 495.84 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.4717(5) _cell_length_b 6.4247(2) _cell_length_c 18.4846(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1718.63(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 17.6 _exptl_crystal_description 'brick-shaped' _exptl_crystal_colour blue _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.383 _exptl_crystal_size_min 0.250 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5692 _exptl_absorpt_correction_T_max 0.7036 _exptl_absorpt_process_details 'X-RED (Stoe, 1996)' _diffrn_ambient_temperature 295(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 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (\w) = 1.05 - 1.25, scan ratio 2\q:\w = 1.00 ; _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.0 _diffrn_reflns_number 3096 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 32.45 _reflns_number_total 3096 _reflns_number_gt 2141 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+3.5000P] 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 SHELXL _refine_ls_extinction_coef 0.0078(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3092 _refine_ls_number_parameters 149 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_goodness_of_fit_gt 1.113 _refine_ls_restrained_S_all 1.088 _refine_ls_restrained_S_gt 1.113 _refine_ls_shift/su_max 0.002 _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_group Cu Cu 0.5000 0.5000 0.5000 0.0276(2) Uani 1 d S . N1 N 0.5490(2) 0.0712(4) 0.33448(14) 0.0393(6) Uani 1 d . . C2 C 0.5189(2) 0.1410(5) 0.3969(2) 0.0375(6) Uani 1 d . . H2 H 0.4894 0.0560 0.4304 0.045 Uiso 1 calc RT . N3 N 0.5341(2) 0.3490(4) 0.40906(12) 0.0307(5) Uani 1 d . . C3A C 0.5769(2) 0.4102(4) 0.34914(15) 0.0311(5) Uani 1 d . . N4 N 0.6091(2) 0.5978(4) 0.3301(2) 0.0415(6) Uani 1 d . . H4 H 0.6048 0.7019 0.3592 0.050 Uiso 1 calc RT . C5 C 0.6487(2) 0.6202(6) 0.2636(2) 0.0456(8) Uani 1 d . . H5 H 0.6712 0.7502 0.2502 0.055 Uiso 1 calc RT . C6 C 0.6564(3) 0.4609(6) 0.2165(2) 0.0451(7) Uani 1 d . . H6 H 0.6849 0.4838 0.1721 0.054 Uiso 1 calc RT . C7 C 0.6220(2) 0.2581(5) 0.2329(2) 0.0354(6) Uani 1 d . . O7 O 0.6210(2) 0.1020(4) 0.19453(12) 0.0458(6) Uani 1 d . . N8 N 0.5860(2) 0.2468(4) 0.30352(12) 0.0317(5) Uani 1 d . . N1N N 0.3085(2) 0.2281(5) 0.5033(2) 0.0455(7) Uani 1 d . . O1N O 0.3890(2) 0.2359(4) 0.53173(13) 0.0403(5) Uani 1 d . . O2N O 0.2998(2) 0.2337(6) 0.4369(2) 0.0764(10) Uani 1 d . . O3N O 0.2405(2) 0.2160(6) 0.5432(2) 0.0724(10) Uani 1 d . . O1W O 0.59055(15) 0.3231(4) 0.55131(12) 0.0359(5) Uani 1 d D . H11W H 0.6388(19) 0.2951(66) 0.5275(19) 0.043 Uiso 1 d DT . H12W H 0.6026(27) 0.3639(60) 0.5942(12) 0.043 Uiso 1 d DT . 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 Cu 0.0306(3) 0.0281(2) 0.0242(2) -0.0024(2) 0.0003(2) 0.0033(2) N1 0.056(2) 0.0270(11) 0.0348(12) -0.0016(10) 0.0075(11) -0.0019(11) C2 0.052(2) 0.0283(13) 0.0324(13) 0.0012(11) 0.0044(12) 0.0004(12) N3 0.0363(11) 0.0272(10) 0.0286(10) -0.0008(8) 0.0026(9) 0.0014(9) C3A 0.0369(13) 0.0254(11) 0.0311(12) -0.0015(10) -0.0003(10) -0.0006(10) N4 0.0485(15) 0.0299(12) 0.0462(14) -0.0032(11) 0.0080(12) -0.0062(11) C5 0.047(2) 0.038(2) 0.052(2) 0.0102(14) 0.0090(15) -0.0041(14) C6 0.049(2) 0.049(2) 0.037(2) 0.0069(14) 0.0081(14) -0.0034(15) C7 0.0393(14) 0.040(2) 0.0265(11) 0.0006(11) -0.0001(10) 0.0033(12) O7 0.063(2) 0.0453(13) 0.0295(10) -0.0071(9) 0.0037(10) 0.0042(12) N8 0.0403(12) 0.0282(10) 0.0266(10) -0.0017(8) 0.0056(9) 0.0017(10) N1N 0.0356(13) 0.0348(13) 0.066(2) -0.0082(13) -0.0011(13) -0.0054(11) O1N 0.0351(10) 0.0405(12) 0.0454(12) -0.0002(10) -0.0016(9) -0.0035(9) O2N 0.071(2) 0.100(3) 0.058(2) -0.009(2) -0.023(2) -0.006(2) O3N 0.048(2) 0.085(2) 0.084(2) -0.012(2) 0.015(2) -0.012(2) O1W 0.0361(10) 0.0394(11) 0.0321(10) -0.0022(9) -0.0018(8) 0.0065(9) _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 Cu O1W 1.977(2) . y Cu N3 2.003(2) . y Cu O1N 2.410(2) . y N1 C2 1.312(4) . n N1 N8 1.374(4) . n C2 N3 1.373(4) . n C2 H2 0.9300 . n N3 C3A 1.328(4) . n C3A N4 1.339(4) . n C3A N8 1.353(4) . n N4 C5 1.364(4) . n N4 H4 0.8600 . n C5 C6 1.348(5) . n C5 H5 0.9300 . n C6 C7 1.427(5) . n C6 H6 0.9300 . n C7 O7 1.228(4) . n C7 N8 1.408(4) . n N1N O3N 1.232(4) . n N1N O2N 1.234(4) . n N1N O1N 1.278(4) . n O1W H11W 0.844(18) . n O1W H12W 0.853(18) . n 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 O1W Cu N3 87.75(9) . . y O1W Cu O1N 85.44(9) . . y N3 Cu O1N 91.59(9) . . y C2 N1 N8 102.4(2) . . n N1 C2 N3 115.1(3) . . n N1 C2 H2 122.5 . . n N3 C2 H2 122.4 . . n C3A N3 C2 103.1(2) . . n C3A N3 Cu 132.2(2) . . n C2 N3 Cu 124.7(2) . . n N3 C3A N4 130.4(3) . . n N3 C3A N8 109.6(2) . . n N4 C3A N8 120.0(3) . . n C3A N4 C5 118.6(3) . . n C3A N4 H4 120.7 . . n C5 N4 H4 120.7 . . n C6 C5 N4 122.4(3) . . n C6 C5 H5 118.7 . . n N4 C5 H5 118.8 . . n C5 C6 C7 121.8(3) . . n C5 C6 H6 119.1 . . n C7 C6 H6 119.0 . . n O7 C7 N8 119.3(3) . . n O7 C7 C6 128.9(3) . . n N8 C7 C6 111.9(3) . . n C3A N8 N1 109.9(2) . . n C3A N8 C7 125.0(3) . . n N1 N8 C7 125.0(2) . . n O3N N1N O2N 121.0(3) . . n O3N N1N O1N 119.0(3) . . n O2N N1N O1N 120.1(3) . . n N1N O1N Cu 122.3(2) . . y Cu O1W H11W 115(3) . . n Cu O1W H12W 114(3) . . n H11W O1W H12W 113(4) . . n 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 _geom_hbond_publ_flag N4 H4 O1N 0.86 2.06 2.769(4) 139.5(2) 5_666 n O1W H11W O3N 0.84(2) 1.97(2) 2.797(4) 166(3) 4_556 n O1W H12W O7 0.85(2) 1.89(1) 2.727(3) 168(4) 7_566 n _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 32.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.941 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.106 _cod_database_code 1100148