#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012635.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_2012635 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m243 _journal_page_last m245 _publ_section_title ; Tetrakis[1-(3-chloropropyl)-1,2,4-triazole- \kN^4^]bis(tetrafluoroborato)copper(II) ; loop_ _publ_author_name 'Mills, Allison M.' 'Flinzner, Kristel' 'Stassen, Arno F.' 'Haasnoot, Jaap G.' 'Spek, Anthony L.' _chemical_formula_moiety 'C20 H32 B2 Cl4 Cu F8 N12' _chemical_formula_sum 'C20 H32 B2 Cl4 Cu F8 N12' _chemical_formula_iupac '[Cu (B F4)2 (C5 H8 Cl1 N3)4 ]' _chemical_formula_weight 819.54 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8647(2) _cell_length_b 13.3168(3) _cell_length_c 15.1469(4) _cell_angle_alpha 72.1540(8) _cell_angle_beta 78.6200(9) _cell_angle_gamma 88.3480(15) _cell_volume 1667.63(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.632 _diffrn_ambient_temperature 150(2) 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 0.23953(4) 0.25714(3) 0.24702(2) 0.02190(11) Uani d . 1 A . Cu N1 0.5239(3) 0.52248(18) 0.11445(17) 0.0261(5) Uani d . 1 . . N N2 0.3976(3) 0.5621(2) 0.08040(19) 0.0323(6) Uani d . 1 A . N N4 0.3500(3) 0.39680(18) 0.17786(17) 0.0243(5) Uani d . 1 . . N C3 0.2948(4) 0.4843(2) 0.1204(2) 0.0316(7) Uani d . 1 A . C H3 0.1920 0.4884 0.1104 0.038 Uiso calc R 1 . . H C5 0.4948(3) 0.4248(2) 0.1716(2) 0.0273(7) Uani d . 1 A . C H5 0.5668 0.3813 0.2034 0.033 Uiso calc R 1 . . H C6A 0.6648(4) 0.5888(2) 0.0889(2) 0.0358(8) Uani d PDU 0.857(3) A 1 C H6A 0.6857 0.6258 0.0200 0.043 Uiso calc PR 0.857(3) A 1 H H6B 0.7528 0.5435 0.1035 0.043 Uiso calc PR 0.857(3) A 1 H C7A 0.6502(7) 0.6702(3) 0.1428(3) 0.0365(10) Uani d PDU 0.857(3) A 1 C H7A 0.7350 0.7239 0.1130 0.044 Uiso calc PR 0.857(3) A 1 H H7B 0.5519 0.7065 0.1372 0.044 Uiso calc PR 0.857(3) A 1 H C8A 0.6551(4) 0.6220(3) 0.2470(3) 0.0384(10) Uani d PDU 0.857(3) A 1 C H8A 0.5812 0.5610 0.2751 0.046 Uiso calc PR 0.857(3) A 1 H H8B 0.6236 0.6748 0.2804 0.046 Uiso calc PR 0.857(3) A 1 H Cl9A 0.84393(14) 0.57958(11) 0.26284(10) 0.0635(6) Uani d PDU 0.857(3) A 1 Cl C6B 0.6648(4) 0.5888(2) 0.0889(2) 0.0358(8) Uani d PDU 0.143(3) A 2 C H6C 0.6708 0.6406 0.0254 0.043 Uiso calc PR 0.143(3) A 2 H H6D 0.7561 0.5443 0.0868 0.043 Uiso calc PR 0.143(3) A 2 H C7B 0.664(5) 0.6464(19) 0.1617(18) 0.0365(10) Uani d PDU 0.143(3) A 2 C H7C 0.5582 0.6656 0.1851 0.044 Uiso calc PR 0.143(3) A 2 H H7D 0.7306 0.7112 0.1344 0.044 Uiso calc PR 0.143(3) A 2 H C8B 0.727(4) 0.5666(14) 0.2414(14) 0.056(5) Uani d PDU 0.143(3) A 2 C H8C 0.8214 0.5354 0.2153 0.067 Uiso calc PR 0.143(3) A 2 H H8D 0.6496 0.5091 0.2772 0.067 Uiso calc PR 0.143(3) A 2 H Cl9B 0.7687(14) 0.6376(7) 0.3162(7) 0.087(4) Uani d PDU 0.143(3) A 2 Cl N11 -0.0419(3) -0.00986(19) 0.39190(17) 0.0264(5) Uani d . 1 . . N N12 0.0950(3) -0.0574(2) 0.3911(2) 0.0349(6) Uani d . 1 . . N N14 0.1296(3) 0.11551(18) 0.31373(17) 0.0242(5) Uani d . 1 . . N C13 0.1941(4) 0.0207(2) 0.3430(2) 0.0338(7) Uani d . 1 A . C H13 0.3020 0.0115 0.3299 0.041 Uiso calc R 1 . . H C15 -0.0204(3) 0.0928(2) 0.3454(2) 0.0265(6) Uani d . 1 A . C H15 -0.0998 0.1422 0.3363 0.032 Uiso calc R 1 . . H C16 -0.1858(4) -0.0705(2) 0.4397(2) 0.0335(7) Uani d . 1 . . C H16A -0.2624 -0.0233 0.4615 0.040 Uiso calc R 1 . . H H16B -0.1671 -0.1269 0.4963 0.040 Uiso calc R 1 . . H C17 -0.2525(4) -0.1204(2) 0.3774(2) 0.0339(7) Uani d . 1 . . C H17A -0.1697 -0.1544 0.3436 0.041 Uiso calc R 1 . . H H17B -0.3307 -0.1757 0.4174 0.041 Uiso calc R 1 . . H C18 -0.3257(4) -0.0389(3) 0.3063(2) 0.0388(8) Uani d . 1 . . C H18A -0.2454 0.0123 0.2622 0.047 Uiso calc R 1 . . H H18B -0.4009 0.0001 0.3398 0.047 Uiso calc R 1 . . H Cl19 -0.42204(11) -0.09895(7) 0.23996(7) 0.0491(2) Uani d . 1 . . Cl N21 0.5502(3) 0.13428(19) 0.06715(17) 0.0257(5) Uani d . 1 . . N N22 0.4190(3) 0.1150(2) 0.04015(19) 0.0319(6) Uani d . 1 . . N N24 0.3664(3) 0.19370(18) 0.15412(17) 0.0228(5) Uani d . 1 . . N C23 0.3120(3) 0.1519(2) 0.0947(2) 0.0297(7) Uani d . 1 A . C H23 0.2058 0.1494 0.0927 0.036 Uiso calc R 1 . . H C25 0.5176(3) 0.1813(2) 0.1339(2) 0.0266(6) Uani d . 1 A . C H25 0.5912 0.2028 0.1629 0.032 Uiso calc R 1 . . H C26 0.7002(3) 0.1029(2) 0.0244(2) 0.0284(7) Uani d . 1 . . C H26A 0.6872 0.0361 0.0104 0.034 Uiso calc R 1 . . H H26B 0.7706 0.0905 0.0697 0.034 Uiso calc R 1 . . H C27 0.7700(4) 0.1878(3) -0.0660(3) 0.0414(8) Uani d . 1 . . C H27A 0.7088 0.1910 -0.1148 0.050 Uiso calc R 1 . . H H27B 0.7644 0.2570 -0.0541 0.050 Uiso calc R 1 . . H C28 0.9360(4) 0.1682(3) -0.1031(3) 0.0431(9) Uani d . 1 . . C H28A 0.9957 0.1604 -0.0528 0.052 Uiso calc R 1 . . H H28B 0.9797 0.2303 -0.1571 0.052 Uiso calc R 1 . . H Cl29 0.95614(11) 0.05301(8) -0.14080(7) 0.0520(3) Uani d . 1 . . Cl N31 -0.0595(3) 0.36817(18) 0.44066(17) 0.0231(5) Uani d . 1 . . N N32 0.0702(3) 0.3713(2) 0.47541(18) 0.0282(6) Uani d . 1 . . N N34 0.1214(3) 0.31735(18) 0.34562(17) 0.0227(5) Uani d . 1 . . N C33 0.1767(3) 0.3410(2) 0.4151(2) 0.0261(6) Uani d . 1 A . C H33 0.2821 0.3361 0.4197 0.031 Uiso calc R 1 . . H C35 -0.0281(3) 0.3364(2) 0.3644(2) 0.0259(6) Uani d . 1 A . C H35 -0.1010 0.3284 0.3285 0.031 Uiso calc R 1 . . H C36 -0.2087(3) 0.3940(2) 0.4884(2) 0.0278(6) Uani d . 1 . . C H36A -0.2797 0.4121 0.4434 0.033 Uiso calc R 1 . . H H36B -0.1954 0.4566 0.5086 0.033 Uiso calc R 1 . . H C37 -0.2795(4) 0.3027(3) 0.5745(2) 0.0330(7) Uani d . 1 . . C H37A -0.3891 0.3170 0.5942 0.040 Uiso calc R 1 . . H H37B -0.2762 0.2378 0.5554 0.040 Uiso calc R 1 . . H C38 -0.2037(4) 0.2819(3) 0.6583(2) 0.0395(8) Uani d . 1 . . C H38A -0.0922 0.2729 0.6386 0.047 Uiso calc R 1 . . H H38B -0.2478 0.2157 0.7069 0.047 Uiso calc R 1 . . H Cl39 -0.23119(11) 0.38936(7) 0.70862(6) 0.0457(2) Uani d . 1 . . Cl F1 0.0335(2) 0.31776(15) 0.16409(15) 0.0453(5) Uani d . 1 . . F F2 0.0295(3) 0.3126(2) 0.01767(16) 0.0681(7) Uani d . 1 . . F F3 -0.0958(2) 0.18615(16) 0.14357(16) 0.0504(5) Uani d . 1 . . F F4 -0.1866(2) 0.34998(18) 0.10698(17) 0.0578(6) Uani d . 1 . . F B1 -0.0564(4) 0.2938(3) 0.1070(3) 0.0293(8) Uani d . 1 A . B F11 0.4293(2) 0.18958(15) 0.35275(14) 0.0396(5) Uani d . 1 . . F F13 0.5805(3) 0.13003(18) 0.46161(15) 0.0565(6) Uani d . 1 . . F F14 0.5304(2) 0.30392(17) 0.41066(18) 0.0551(6) Uani d . 1 . . F F12 0.6834(2) 0.22866(19) 0.31270(16) 0.0576(6) Uani d . 1 . . F B11 0.5557(4) 0.2129(3) 0.3859(3) 0.0304(8) Uani d . 1 . . B 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 0.01794(19) 0.02215(19) 0.0253(2) -0.00251(13) -0.00073(14) -0.00883(14) N1 0.0246(13) 0.0239(12) 0.0272(13) -0.0041(10) -0.0017(10) -0.0056(10) N2 0.0351(15) 0.0250(13) 0.0367(15) 0.0012(11) -0.0108(12) -0.0070(11) N4 0.0229(12) 0.0211(12) 0.0285(14) -0.0020(10) -0.0019(10) -0.0089(10) C3 0.0305(17) 0.0263(16) 0.0398(19) 0.0021(13) -0.0087(14) -0.0118(14) C5 0.0249(15) 0.0222(14) 0.0295(16) -0.0029(12) -0.0018(12) -0.0019(12) C6A 0.0283(17) 0.0299(16) 0.0412(19) -0.0101(13) 0.0023(14) -0.0042(14) C7A 0.037(2) 0.029(2) 0.037(2) -0.010(2) -0.0096(18) 0.001(2) C8A 0.034(2) 0.037(2) 0.044(2) -0.0041(17) -0.0092(18) -0.0104(18) Cl9A 0.0478(7) 0.0626(9) 0.0609(9) -0.0042(6) -0.0222(6) 0.0164(7) C6B 0.0283(17) 0.0299(16) 0.0412(19) -0.0101(13) 0.0023(14) -0.0042(14) C7B 0.037(2) 0.029(2) 0.037(2) -0.010(2) -0.0096(18) 0.001(2) C8B 0.051(9) 0.051(9) 0.064(9) -0.006(8) -0.023(8) -0.004(9) Cl9B 0.143(9) 0.061(5) 0.070(6) -0.015(5) -0.048(6) -0.021(4) N11 0.0233(13) 0.0246(12) 0.0292(14) -0.0011(10) -0.0052(10) -0.0051(10) N12 0.0274(14) 0.0251(13) 0.0504(18) 0.0030(11) -0.0127(13) -0.0058(12) N14 0.0203(12) 0.0228(12) 0.0294(13) -0.0008(9) -0.0057(10) -0.0073(10) C13 0.0233(16) 0.0301(16) 0.047(2) 0.0026(13) -0.0076(14) -0.0109(15) C15 0.0214(15) 0.0234(14) 0.0307(16) -0.0002(11) -0.0027(12) -0.0039(12) C16 0.0293(17) 0.0301(16) 0.0321(17) -0.0066(13) -0.0012(13) 0.0010(13) C17 0.0312(17) 0.0293(16) 0.0367(18) -0.0076(13) -0.0040(14) -0.0045(14) C18 0.0399(19) 0.0323(17) 0.042(2) -0.0047(14) -0.0116(16) -0.0056(15) Cl19 0.0550(6) 0.0443(5) 0.0471(5) -0.0105(4) -0.0187(4) -0.0063(4) N21 0.0209(12) 0.0278(13) 0.0288(14) -0.0007(10) -0.0044(10) -0.0096(11) N22 0.0287(14) 0.0360(14) 0.0384(16) 0.0027(11) -0.0109(12) -0.0196(12) N24 0.0199(12) 0.0224(12) 0.0261(13) -0.0010(9) -0.0008(10) -0.0098(10) C23 0.0252(16) 0.0307(16) 0.0369(18) 0.0003(12) -0.0068(13) -0.0151(14) C25 0.0230(15) 0.0302(15) 0.0286(16) -0.0033(12) -0.0028(12) -0.0128(13) C26 0.0233(15) 0.0296(16) 0.0313(17) 0.0016(12) -0.0012(13) -0.0109(13) C27 0.042(2) 0.0306(17) 0.042(2) 0.0052(15) 0.0036(16) -0.0052(15) C28 0.0341(19) 0.0381(19) 0.050(2) -0.0036(15) 0.0069(16) -0.0124(16) Cl29 0.0429(5) 0.0517(5) 0.0593(6) -0.0035(4) 0.0120(4) -0.0272(5) N31 0.0199(12) 0.0246(12) 0.0242(13) 0.0007(9) -0.0033(10) -0.0073(10) N32 0.0255(13) 0.0330(14) 0.0288(14) 0.0000(10) -0.0057(11) -0.0131(11) N34 0.0203(12) 0.0212(12) 0.0260(13) -0.0001(9) -0.0016(10) -0.0081(10) C33 0.0225(15) 0.0278(15) 0.0296(16) -0.0021(12) -0.0053(12) -0.0110(13) C35 0.0251(15) 0.0273(15) 0.0265(16) 0.0005(12) -0.0055(12) -0.0098(12) C36 0.0235(15) 0.0315(16) 0.0278(16) 0.0018(12) -0.0016(12) -0.0105(13) C37 0.0324(17) 0.0348(17) 0.0298(17) -0.0026(14) -0.0010(14) -0.0099(14) C38 0.046(2) 0.0374(18) 0.0324(18) 0.0035(15) -0.0029(15) -0.0094(15) Cl39 0.0532(5) 0.0497(5) 0.0355(5) 0.0018(4) -0.0054(4) -0.0171(4) F1 0.0452(12) 0.0439(11) 0.0589(13) 0.0015(9) -0.0314(10) -0.0200(10) F2 0.0555(14) 0.101(2) 0.0418(13) -0.0244(13) 0.0128(11) -0.0247(13) F3 0.0550(13) 0.0391(11) 0.0603(14) -0.0087(10) -0.0177(11) -0.0148(10) F4 0.0334(11) 0.0586(14) 0.0758(16) 0.0143(10) -0.0140(11) -0.0116(12) B1 0.0195(17) 0.038(2) 0.0297(19) -0.0028(14) -0.0032(14) -0.0105(15) F11 0.0288(10) 0.0482(11) 0.0501(12) 0.0012(8) -0.0159(9) -0.0221(10) F13 0.0655(15) 0.0547(13) 0.0454(13) 0.0109(11) -0.0228(11) -0.0033(10) F14 0.0400(12) 0.0519(13) 0.0935(18) 0.0104(10) -0.0338(12) -0.0393(13) F12 0.0256(10) 0.0846(17) 0.0532(14) 0.0021(10) 0.0000(10) -0.0124(12) B11 0.0198(17) 0.040(2) 0.0318(19) 0.0015(14) -0.0064(14) -0.0102(16) 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 N4 . 2.005(2) yes Cu1 N14 . 2.019(2) yes Cu1 N24 . 2.002(2) yes Cu1 N34 . 2.009(2) yes Cu1 F1 . 2.4009(18) yes Cu1 F11 . 2.5096(18) yes N1 C5 . 1.323(4) ? N1 N2 . 1.350(3) ? N1 C6A . 1.467(4) ? N2 C3 . 1.313(4) ? N4 C5 . 1.324(4) ? N4 C3 . 1.367(4) ? C3 H3 . 0.9500 ? C5 H5 . 0.9500 ? C6A C7A . 1.534(5) ? C6A H6A . 0.9900 ? C6A H6B . 0.9900 ? C7A C8A . 1.520(5) ? C7A H7A . 0.9900 ? C7A H7B . 0.9900 ? C8A Cl9A . 1.789(4) ? C8A H8A . 0.9900 ? C8A H8B . 0.9900 ? C7B C8B . 1.531(11) ? C7B H7C . 0.9900 ? C7B H7D . 0.9900 ? C8B Cl9B . 1.776(10) ? C8B H8C . 0.9900 ? C8B H8D . 0.9900 ? N11 C15 . 1.332(4) ? N11 N12 . 1.353(3) ? N11 C16 . 1.462(4) ? N12 C13 . 1.310(4) ? N14 C15 . 1.331(4) ? N14 C13 . 1.354(4) ? C13 H13 . 0.9500 ? C15 H15 . 0.9500 ? C16 C17 . 1.520(5) ? C16 H16A . 0.9900 ? C16 H16B . 0.9900 ? C17 C18 . 1.508(4) ? C17 H17A . 0.9900 ? C17 H17B . 0.9900 ? C18 Cl19 . 1.803(3) ? C18 H18A . 0.9900 ? C18 H18B . 0.9900 ? N21 C25 . 1.326(4) ? N21 N22 . 1.362(3) ? N21 C26 . 1.468(4) ? N22 C23 . 1.318(4) ? N24 C25 . 1.332(4) ? N24 C23 . 1.358(4) ? C23 H23 . 0.9500 ? C25 H25 . 0.9500 ? C26 C27 . 1.514(4) ? C26 H26A . 0.9900 ? C26 H26B . 0.9900 ? C27 C28 . 1.513(5) ? C27 H27A . 0.9900 ? C27 H27B . 0.9900 ? C28 Cl29 . 1.787(4) ? C28 H28A . 0.9900 ? C28 H28B . 0.9900 ? N31 C35 . 1.326(4) ? N31 N32 . 1.363(3) ? N31 C36 . 1.462(4) ? N32 C33 . 1.324(4) ? N34 C35 . 1.333(4) ? N34 C33 . 1.364(4) ? C33 H33 . 0.9500 ? C35 H35 . 0.9500 ? C36 C37 . 1.523(4) ? C36 H36A . 0.9900 ? C36 H36B . 0.9900 ? C37 C38 . 1.501(5) ? C37 H37A . 0.9900 ? C37 H37B . 0.9900 ? C38 Cl39 . 1.805(4) ? C38 H38A . 0.9900 ? C38 H38B . 0.9900 ? F1 B1 . 1.393(4) ? F2 B1 . 1.368(4) ? F3 B1 . 1.396(4) ? F4 B1 . 1.357(4) ? F11 B11 . 1.393(4) ? F13 B11 . 1.375(4) ? F14 B11 . 1.375(4) ? F12 B11 . 1.389(4) ? _cod_database_code 2012635