#------------------------------------------------------------------------------ #$Date: 2015-01-27 19:58:39 +0000 (Tue, 27 Jan 2015) $ #$Revision: 130149 $ #$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 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_name_full 'Acta Crystallographica Section E' _journal_page_first m903 _journal_page_last m905 _journal_paper_doi 10.1107/S1600536803019974 _journal_volume 59 _journal_year 2003 _chemical_formula_moiety 'C10 H12 Cu N10 O10' _chemical_formula_sum 'C10 H12 Cu N10 O10' _chemical_formula_weight 495.84 _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.4717(5) _cell_length_b 6.4247(2) _cell_length_c 18.4846(6) _cell_measurement_reflns_used 40 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.6 _cell_measurement_theta_min 12.7 _cell_volume 1718.63(10) _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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_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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3096 _diffrn_reflns_theta_full 32.45 _diffrn_reflns_theta_max 32.45 _diffrn_reflns_theta_min 2.20 _diffrn_standards_decay_% 4.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_T_max 0.7036 _exptl_absorpt_correction_T_min 0.5692 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'X-RED (Stoe, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.916 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description brick-shaped _exptl_crystal_F_000 1004 _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.383 _exptl_crystal_size_min 0.250 _refine_diff_density_max 0.941 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.106 _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_extinction_method SHELXL _refine_ls_goodness_of_fit_gt 1.113 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 149 _refine_ls_number_reflns 3092 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.088 _refine_ls_restrained_S_gt 1.113 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0570 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.1398 _refine_ls_wR_factor_ref 0.1658 _reflns_number_gt 2141 _reflns_number_total 3096 _reflns_threshold_expression >2sigma(I) _cod_duplicate_entry 2202376 _cod_database_code 1100148 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' 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) 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' 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_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_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