#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100154.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_1100154 _journal_name_full 'Acta Crystallographica Section E' _journal_volume 60 loop_ _publ_author_name 'Carlos Sanchez' 'Juan M. Salas' 'Miguel Quiros' 'M. Purificacion Sanchez' _publ_section_title ; trans-Dichloro bis(3-amino-1,2,4-triazolium-N^1^) copper(II) tetrachlorocuprate(II) dihydrate. ; _journal_page_first m370 _journal_page_last m372 _journal_year 2004 _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_name_systematic ; trans-Dichloro bis(3-amino-1,2,4-triazolium-N^1^) copper(II) tetrachlorocuprate(II) dihydrate. ; _chemical_formula_moiety 'C4 H10 Cl2 Cu N8 2+, Cl4 Cu 2-, 2(H2 O)' _chemical_formula_sum 'C4 H14 Cl6 Cu2 N8 O2' _chemical_formula_weight 546.01 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' 'Cl' 'Cl' 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1505(6) _cell_length_b 7.6367(8) _cell_length_c 9.7197(10) _cell_angle_alpha 95.0132(15) _cell_angle_beta 99.9045(15) _cell_angle_gamma 110.2812(14) _cell_volume 416.47(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3558 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 27.98 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 270 _exptl_absorpt_coefficient_mu 3.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4216 _exptl_absorpt_correction_T_max 0.5105 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _diffrn_ambient_temperature 100(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 4759 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.28 _reflns_number_total 1867 _reflns_number_gt 1800 _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^)+(0.0200P)^2^+0.2000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.079(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1867 _refine_ls_number_parameters 110 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.086 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.0000 0.02586(9) Uani 1 2 d S . . Cl1 Cl 0.70181(7) 0.54832(5) 0.23901(4) 0.02737(11) Uani 1 1 d . . . Cl2 Cl 0.77967(7) 0.76437(6) -0.03392(4) 0.02997(11) Uani 1 1 d . . . Cu2 Cu 0.5000 0.5000 0.5000 0.02415(9) Uani 1 2 d S . . Cl3 Cl 0.31753(7) 0.70168(5) 0.43559(4) 0.02755(11) Uani 1 1 d . . . N1 N 0.2106(2) 0.27671(18) 0.39413(14) 0.0228(3) Uani 1 1 d . . . N2 N 0.0043(2) 0.29145(18) 0.32524(14) 0.0233(3) Uani 1 1 d . . . H2 H -0.0185 0.3961 0.3220 0.028 Uiso 1 1 d R . . C3 C -0.1552(3) 0.1224(2) 0.26424(16) 0.0234(3) Uani 1 1 d . . . N3 N -0.3714(3) 0.0830(2) 0.19151(17) 0.0338(3) Uani 1 1 d . . . H31 H -0.4240 0.1724 0.1791 0.041 Uiso 1 1 d R . . H32 H -0.4607 -0.0321 0.1563 0.041 Uiso 1 1 d R . . N4 N -0.0499(2) -0.00194(19) 0.29491(15) 0.0274(3) Uani 1 1 d . . . H4 H -0.1124 -0.1226 0.2697 0.033 Uiso 1 1 d R . . C5 C 0.1719(3) 0.0977(2) 0.37260(18) 0.0268(3) Uani 1 1 d . . . H5 H 0.2821 0.0447 0.4059 0.032 Uiso 1 1 d R . . O1W O 0.2751(2) 0.7072(2) 0.09221(15) 0.0383(3) Uani 1 1 d D . . H1W H 0.258(4) 0.672(3) 0.169(2) 0.046 Uiso 1 1 d D . . H2W H 0.148(3) 0.708(3) 0.056(2) 0.046 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 Cu1 0.02404(15) 0.02084(15) 0.02380(15) 0.00270(11) -0.00190(11) 0.00095(11) Cl1 0.0289(2) 0.02138(19) 0.0266(2) 0.00148(14) -0.00315(15) 0.00780(15) Cl2 0.0254(2) 0.0263(2) 0.0300(2) 0.00453(15) 0.00337(15) 0.00069(15) Cu2 0.02161(15) 0.01495(14) 0.03194(16) -0.00035(10) -0.00269(11) 0.00688(11) Cl3 0.0283(2) 0.02016(19) 0.0324(2) 0.00104(15) -0.00179(15) 0.01148(15) N1 0.0226(6) 0.0191(6) 0.0250(7) 0.0012(5) 0.0015(5) 0.0080(5) N2 0.0220(6) 0.0174(6) 0.0293(7) 0.0012(5) 0.0016(5) 0.0080(5) C3 0.0255(7) 0.0201(7) 0.0228(7) 0.0009(6) 0.0040(6) 0.0075(6) N3 0.0262(7) 0.0235(7) 0.0437(9) -0.0016(6) -0.0054(6) 0.0073(6) N4 0.0291(7) 0.0150(6) 0.0322(7) -0.0016(5) -0.0013(6) 0.0058(5) C5 0.0285(8) 0.0197(8) 0.0295(8) 0.0013(6) -0.0012(6) 0.0095(6) O1W 0.0312(7) 0.0436(8) 0.0376(7) 0.0091(6) 0.0056(6) 0.0109(6) _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 Cu1 Cl2 2.2467(4) . y Cu1 Cl2 2.2467(4) 2_665 n Cu1 Cl1 2.3695(4) . y Cu1 Cl1 2.3695(4) 2_665 n Cu2 N1 2.0233(13) 2_666 n Cu2 N1 2.0233(13) . y Cu2 Cl3 2.2691(4) . y Cu2 Cl3 2.2691(4) 2_666 n N1 C5 1.295(2) . y N1 N2 1.3749(18) . y N2 C3 1.330(2) . y N2 H2 0.8600 . n C3 N3 1.312(2) . y C3 N4 1.349(2) . y N3 H31 0.8600 . n N3 H32 0.8600 . n N4 C5 1.355(2) . y N4 H4 0.8600 . n C5 H5 0.9300 . n O1W H1W 0.828(16) . n O1W H2W 0.806(16) . 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 Cl2 Cu1 Cl2 180.0 . 2_665 n Cl2 Cu1 Cl1 89.901(15) . . y Cl2 Cu1 Cl1 90.099(15) 2_665 . n Cl2 Cu1 Cl1 90.099(15) . 2_665 n Cl2 Cu1 Cl1 89.900(15) 2_665 2_665 n Cl1 Cu1 Cl1 180.0 . 2_665 n N1 Cu2 N1 180.0 2_666 . n N1 Cu2 Cl3 89.47(4) 2_666 . n N1 Cu2 Cl3 90.53(4) . . y N1 Cu2 Cl3 90.53(4) 2_666 2_666 n N1 Cu2 Cl3 89.47(4) . 2_666 n Cl3 Cu2 Cl3 180.0 . 2_666 n C5 N1 N2 104.80(13) . . y C5 N1 Cu2 131.20(11) . . y N2 N1 Cu2 124.00(10) . . y C3 N2 N1 110.98(13) . . y C3 N2 H2 124.5 . . n N1 N2 H2 124.5 . . n N3 C3 N2 127.60(15) . . y N3 C3 N4 126.81(15) . . y N2 C3 N4 105.58(13) . . y C3 N3 H31 119.9 . . n C3 N3 H32 120.1 . . n H31 N3 H32 120.0 . . n C3 N4 C5 107.61(13) . . y C3 N4 H4 126.1 . . n C5 N4 H4 126.2 . . n N1 C5 N4 111.03(14) . . y N1 C5 H5 124.4 . . n N4 C5 H5 124.6 . . n H1W O1W H2W 105(2) . . 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 N2 H2 Cl1 0.86 2.46 3.2084(14) 146.4 1_455 y N3 H32 O1W 0.86 2.05 2.892(2) 167.8 1_445 y N4 H4 Cl1 0.86 2.34 3.1899(14) 170.3 1_445 y O1W H1W Cl3 0.828(16) 2.529(18) 3.3078(15) 157(2) . y O1W H2W Cl2 0.806(16) 2.475(17) 3.2728(15) 171(2) 1_455 y _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.299 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.062 _cod_database_code 1100154 _cod_duplicate_entry 2203434 _journal_paper_doi 10.1107/S1600536804003812