#------------------------------------------------------------------------------ #$Date: 2008-03-30 13:21:05 +0300 (Sun, 30 Mar 2008) $ #$Revision: 321 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2203434.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2203434 loop_ _publ_author_name 'Carlos S\'anchez' 'Juan M. Salas' 'Miguel Quir\'os' 'M. Purificaci\'on S\'anchez' _publ_section_title ; trans-Bis(3-amino-1,2,4-triazolium-\kN^1^)dichlorocopper(II) tetrachlorocuprate(II) dihydrate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m370 _journal_page_last m372 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cu Cl2 (C2 H5 N4)2] [Cu Cl4], 2H2 O' _chemical_formula_moiety 'C4 H10 Cl2 Cu N8 2+, Cl4 Cu 2-, 2H2 O' _chemical_formula_sum 'C4 H14 Cl6 Cu2 N8 O2' _chemical_formula_weight 546.01 _chemical_name_systematic ; trans-Bis(3-amino-1,2,4-triazolium-\kN^1^)dichlorocopper(II) tetrachlorocuprate(II) dihydrate ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _cell_angle_alpha 95.0132(15) _cell_angle_beta 99.9045(15) _cell_angle_gamma 110.2812(14) _cell_formula_units_Z 1 _cell_length_a 6.1505(6) _cell_length_b 7.6367(8) _cell_length_c 9.7197(10) _cell_measurement_reflns_used 3558 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.98 _cell_measurement_theta_min 3.62 _cell_volume 416.47(7) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT (Bruker, 1999)' _computing_molecular_graphics ; Xtal_GX (Hall & du Boulay, 1997) and ORTEP-3 (Farrugia, 1997) ; _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 66.06 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.905 _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f' _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 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4759 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.531 _exptl_absorpt_correction_T_max 0.460 _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 270 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.299 _refine_diff_density_min -0.331 _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_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1867 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0177 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^+0.2P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0461 _reflns_number_gt 1800 _reflns_number_total 1867 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hb6014.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu1 0.5000 0.5000 0.0000 0.02586(9) Uani d S 1 Cu Cl1 0.70181(7) 0.54832(5) 0.23901(4) 0.02737(11) Uani d . 1 Cl Cl2 0.77967(7) 0.76437(6) -0.03392(4) 0.02997(11) Uani d . 1 Cl Cu2 0.5000 0.5000 0.5000 0.02415(9) Uani d S 1 Cu Cl3 0.31753(7) 0.70168(5) 0.43559(4) 0.02755(11) Uani d . 1 Cl N1 0.2106(2) 0.27671(18) 0.39413(14) 0.0228(3) Uani d . 1 N N2 0.0043(2) 0.29145(18) 0.32524(14) 0.0233(3) Uani d . 1 N H2 -0.0185 0.3961 0.3220 0.028 Uiso d R 1 H C3 -0.1552(3) 0.1224(2) 0.26424(16) 0.0234(3) Uani d . 1 C N3 -0.3714(3) 0.0830(2) 0.19151(17) 0.0338(3) Uani d . 1 N H31 -0.4240 0.1724 0.1791 0.041 Uiso d R 1 H H32 -0.4607 -0.0321 0.1563 0.041 Uiso d R 1 H N4 -0.0499(2) -0.00194(19) 0.29491(15) 0.0274(3) Uani d . 1 N H4 -0.1124 -0.1226 0.2697 0.033 Uiso d R 1 H C5 0.1719(3) 0.0977(2) 0.37260(18) 0.0268(3) Uani d . 1 C H5 0.2821 0.0447 0.4059 0.032 Uiso d R 1 H O1W 0.2751(2) 0.7072(2) 0.09221(15) 0.0383(3) Uani d D 1 O H1W 0.258(4) 0.672(3) 0.169(2) 0.046 Uiso d D 1 H H2W 0.148(3) 0.708(3) 0.056(2) 0.046 Uiso d D 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.02404(15) 0.02084(15) 0.02380(15) 0.00095(11) -0.00190(11) 0.00270(11) Cl1 0.0289(2) 0.02138(19) 0.0266(2) 0.00780(15) -0.00315(15) 0.00148(14) Cl2 0.0254(2) 0.0263(2) 0.0300(2) 0.00069(15) 0.00337(15) 0.00453(15) Cu2 0.02161(15) 0.01495(14) 0.03194(16) 0.00688(11) -0.00269(11) -0.00035(10) Cl3 0.0283(2) 0.02016(19) 0.0324(2) 0.01148(15) -0.00179(15) 0.00104(15) N1 0.0226(6) 0.0191(6) 0.0250(7) 0.0080(5) 0.0015(5) 0.0012(5) N2 0.0220(6) 0.0174(6) 0.0293(7) 0.0080(5) 0.0016(5) 0.0012(5) C3 0.0255(7) 0.0201(7) 0.0228(7) 0.0075(6) 0.0040(6) 0.0009(6) N3 0.0262(7) 0.0235(7) 0.0437(9) 0.0073(6) -0.0054(6) -0.0016(6) N4 0.0291(7) 0.0150(6) 0.0322(7) 0.0058(5) -0.0013(6) -0.0016(5) C5 0.0285(8) 0.0197(8) 0.0295(8) 0.0095(6) -0.0012(6) 0.0013(6) O1W 0.0312(7) 0.0436(8) 0.0376(7) 0.0109(6) 0.0056(6) 0.0091(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 Cl2 . 2.2467(4) y Cu1 Cl2 2_665 2.2467(4) n Cu1 Cl1 . 2.3695(4) y Cu1 Cl1 2_665 2.3695(4) n Cu2 N1 2_666 2.0233(13) n Cu2 N1 . 2.0233(13) y Cu2 Cl3 . 2.2691(4) y Cu2 Cl3 2_666 2.2691(4) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 Cu1 Cl2 . 2_665 180.0 n Cl2 Cu1 Cl1 . . 89.901(15) y Cl2 Cu1 Cl1 2_665 . 90.099(15) n Cl2 Cu1 Cl1 . 2_665 90.099(15) n Cl2 Cu1 Cl1 2_665 2_665 89.900(15) n Cl1 Cu1 Cl1 . 2_665 180.0 n N1 Cu2 N1 2_666 . 180.0 n N1 Cu2 Cl3 2_666 . 89.47(4) n N1 Cu2 Cl3 . . 90.53(4) y N1 Cu2 Cl3 2_666 2_666 90.53(4) n N1 Cu2 Cl3 . 2_666 89.47(4) n Cl3 Cu2 Cl3 . 2_666 180.0 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_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N2 H2 Cl1 1_455 0.86 2.46 3.2084(14) 146 y N3 H32 O1W 1_445 0.86 2.05 2.892(2) 168 y N4 H4 Cl1 1_445 0.86 2.34 3.1899(14) 170 y O1W H1W Cl3 . 0.828(16) 2.529(18) 3.3078(15) 157(2) y O1W H2W Cl2 1_455 0.806(16) 2.475(17) 3.2728(15) 171(2) y