#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013931.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_2013931 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2004 _journal_volume 60 _journal_page_first m177 _journal_page_last m179 _publ_section_title ; [Tris-(4-{pyrazol-3-yl}-3-aza-3-butenyl)amine]iron(II) diperchlorate hydrate ; loop_ _publ_author_name 'Michaele J. Hardie' 'Colin A. Kilner' 'Malcolm A. Halcrow' _chemical_formula_moiety 'C18 H24 Fe N10, 2(Cl O4), H2 O' _chemical_formula_sum 'C18 H26 Cl2 Fe N10 O9' _chemical_formula_weight 653.24 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.40860(10) _cell_length_b 22.5317(4) _cell_length_c 12.7279(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.9858(6) _cell_angle_gamma 90.00 _cell_volume 2639.38(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _exptl_crystal_density_diffrn 1.644 _diffrn_ambient_temperature 100(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 Fe1 0.50212(3) 0.366591(12) 0.25044(2) 0.01882(9) Uani d . 1 . . Fe N2 0.42530(18) 0.26732(7) 0.12636(12) 0.0219(4) Uani d . 1 . . N C3 0.4007(2) 0.21984(9) 0.19870(15) 0.0248(4) Uani d . 1 . . C H3A 0.4267 0.1812 0.1708 0.030 Uiso calc R 1 . . H H3B 0.2965 0.2186 0.2019 0.030 Uiso calc R 1 . . H C4 0.4919(2) 0.22993(9) 0.31113(15) 0.0240(4) Uani d . 1 . . C H4A 0.4648 0.2009 0.3621 0.029 Uiso calc R 1 . . H H4B 0.5963 0.2249 0.3109 0.029 Uiso calc R 1 . . H N5 0.46352(18) 0.29044(7) 0.34325(12) 0.0209(4) Uani d . 1 . . N C6 0.4015(2) 0.29873(9) 0.42240(15) 0.0219(4) Uani d . 1 . . C H6 0.3760 0.2662 0.4622 0.026 Uiso calc R 1 . . H C7 0.3711(2) 0.35947(9) 0.44990(15) 0.0207(4) Uani d . 1 . . C N8 0.40373(18) 0.40215(7) 0.38485(13) 0.0206(4) Uani d . 1 . . N N9 0.36715(18) 0.45327(7) 0.42674(13) 0.0222(4) Uani d . 1 . . N H9 0.3779 0.4885 0.3997 0.027 Uiso calc RD 1 . . H C10 0.3121(2) 0.44404(9) 0.51509(16) 0.0238(4) Uani d . 1 . . C H10 0.2786 0.4737 0.5571 0.029 Uiso calc R 1 . . H C11 0.3131(2) 0.38397(9) 0.53324(15) 0.0228(4) Uani d . 1 . . C H11 0.2816 0.3636 0.5896 0.027 Uiso calc R 1 . . H C12 0.5505(2) 0.25584(9) 0.07622(16) 0.0262(5) Uani d . 1 . . C H12A 0.5175 0.2345 0.0075 0.031 Uiso calc R 1 . . H H12B 0.6218 0.2304 0.1241 0.031 Uiso calc R 1 . . H C13 0.6227(2) 0.31409(9) 0.05553(15) 0.0245(4) Uani d . 1 . . C H13A 0.7098 0.3062 0.0255 0.029 Uiso calc R 1 . . H H13B 0.5543 0.3387 0.0037 0.029 Uiso calc R 1 . . H N14 0.66354(18) 0.34474(7) 0.15855(13) 0.0216(4) Uani d . 1 . . N C15 0.7954(2) 0.35771(9) 0.19791(16) 0.0237(4) Uani d . 1 . . C H15 0.8691 0.3523 0.1578 0.028 Uiso calc R 1 . . H C16 0.8291(2) 0.38135(9) 0.30735(16) 0.0220(4) Uani d . 1 . . C N17 0.71804(18) 0.38498(7) 0.35824(13) 0.0216(4) Uani d . 1 . . N N18 0.77857(18) 0.40390(7) 0.45793(13) 0.0231(4) Uani d . 1 . . N H18 0.7295 0.4103 0.5086 0.028 Uiso calc R 1 . . H C19 0.9228(2) 0.41179(9) 0.47085(17) 0.0268(5) Uani d . 1 . . C H19 0.9871 0.4246 0.5345 0.032 Uiso calc R 1 . . H C20 0.9602(2) 0.39783(10) 0.37475(17) 0.0269(5) Uani d . 1 . . C H20 1.0539 0.3991 0.3580 0.032 Uiso calc R 1 . . H C21 0.2919(2) 0.28376(9) 0.04891(16) 0.0254(5) Uani d . 1 . . C H21A 0.2325 0.2479 0.0269 0.030 Uiso calc R 1 . . H H21B 0.3176 0.3013 -0.0160 0.030 Uiso calc R 1 . . H C22 0.2045(2) 0.32831(9) 0.09948(16) 0.0259(5) Uani d . 1 . . C H22A 0.1180 0.3414 0.0462 0.031 Uiso calc R 1 . . H H22B 0.1714 0.3100 0.1610 0.031 Uiso calc R 1 . . H N23 0.29967(18) 0.37886(7) 0.13586(13) 0.0219(4) Uani d . 1 . . N C24 0.2685(2) 0.43029(9) 0.09623(16) 0.0236(4) Uani d . 1 . . C H24 0.1777 0.4382 0.0496 0.028 Uiso calc R 1 . . H C25 0.3778(2) 0.47649(9) 0.12542(15) 0.0216(4) Uani d . 1 . . C N26 0.50237(18) 0.46036(7) 0.19068(13) 0.0218(4) Uani d . 1 . . N N27 0.58740(19) 0.50866(7) 0.19898(13) 0.0239(4) Uani d . 1 . . N H27 0.6763 0.5103 0.2380 0.029 Uiso calc R 1 . . H C28 0.5205(2) 0.55426(9) 0.14045(17) 0.0274(5) Uani d . 1 . . C H28 0.5604 0.5925 0.1339 0.033 Uiso calc R 1 . . H C29 0.3841(2) 0.53545(9) 0.09208(17) 0.0282(5) Uani d . 1 . . C H29 0.3102 0.5575 0.0462 0.034 Uiso calc R 1 . . H Cl30 0.96490(6) 0.53235(2) 0.20209(4) 0.02860(13) Uani d . 1 . . Cl O31 0.87955(18) 0.54411(8) 0.28247(13) 0.0412(4) Uani d . 1 . . O O32 1.10489(18) 0.51063(8) 0.25561(15) 0.0435(4) Uani d . 1 . . O O33 0.89253(18) 0.48819(7) 0.12910(12) 0.0345(4) Uani d . 1 . . O O34 0.9830(2) 0.58560(8) 0.14540(15) 0.0525(5) Uani d . 1 . . O Cl35 0.50340(5) 0.71869(2) 0.23985(4) 0.02391(12) Uani d . 1 . . Cl O36 0.40823(18) 0.66807(7) 0.23031(15) 0.0403(4) Uani d . 1 . . O O37 0.62998(17) 0.70271(8) 0.19977(13) 0.0378(4) Uani d . 1 . . O O38 0.5450(2) 0.73624(8) 0.35028(12) 0.0420(4) Uani d . 1 . . O O39 0.42776(18) 0.76658(7) 0.17823(12) 0.0338(4) Uani d . 1 . . O O40 0.34003(17) 0.57388(7) 0.35871(12) 0.0265(3) Uani d D 1 . . O H40A 0.260(2) 0.5725(9) 0.3126(18) 0.048(8) Uiso d D 1 . . H H40B 0.391(3) 0.5997(13) 0.336(2) 0.075(11) 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 Fe1 0.01900(17) 0.02036(16) 0.01707(15) -0.00015(11) 0.00369(11) 0.00102(11) N2 0.0245(9) 0.0242(9) 0.0168(8) -0.0015(7) 0.0040(7) 0.0002(7) C3 0.0328(12) 0.0208(10) 0.0212(10) -0.0048(9) 0.0063(9) -0.0016(8) C4 0.0330(12) 0.0191(10) 0.0200(10) 0.0027(9) 0.0056(9) -0.0001(8) N5 0.0235(9) 0.0215(8) 0.0169(8) 0.0011(7) 0.0022(7) -0.0005(6) C6 0.0250(10) 0.0225(10) 0.0172(9) -0.0027(8) 0.0022(8) 0.0029(8) C7 0.0182(10) 0.0247(10) 0.0185(9) -0.0002(8) 0.0023(8) 0.0017(8) N8 0.0212(9) 0.0209(8) 0.0196(8) 0.0008(7) 0.0038(7) -0.0008(7) N9 0.0237(9) 0.0200(8) 0.0225(8) 0.0006(7) 0.0042(7) -0.0014(7) C10 0.0234(11) 0.0267(11) 0.0222(10) 0.0017(9) 0.0065(8) -0.0025(8) C11 0.0222(10) 0.0277(11) 0.0187(9) 0.0010(9) 0.0047(8) -0.0002(8) C12 0.0336(12) 0.0248(11) 0.0211(10) -0.0022(9) 0.0076(9) -0.0040(8) C13 0.0260(11) 0.0292(11) 0.0185(9) -0.0007(9) 0.0052(8) -0.0041(8) N14 0.0245(9) 0.0222(9) 0.0181(8) 0.0001(7) 0.0043(7) -0.0003(6) C15 0.0235(11) 0.0248(10) 0.0243(10) 0.0010(9) 0.0081(9) 0.0004(8) C16 0.0218(10) 0.0218(10) 0.0219(10) 0.0013(8) 0.0031(8) 0.0000(8) N17 0.0232(9) 0.0225(9) 0.0181(8) -0.0001(7) 0.0022(7) -0.0022(7) N18 0.0260(9) 0.0248(9) 0.0179(8) 0.0024(7) 0.0029(7) -0.0030(7) C19 0.0250(11) 0.0280(11) 0.0246(10) -0.0022(9) -0.0010(8) -0.0028(8) C20 0.0205(10) 0.0307(11) 0.0288(11) 0.0003(9) 0.0035(9) -0.0021(9) C21 0.0265(11) 0.0275(11) 0.0202(10) -0.0064(9) 0.0002(8) -0.0012(8) C22 0.0234(11) 0.0289(11) 0.0235(10) -0.0041(9) 0.0005(8) 0.0026(8) N23 0.0215(9) 0.0249(9) 0.0190(8) -0.0036(7) 0.0037(7) -0.0010(7) C24 0.0217(10) 0.0282(11) 0.0202(10) 0.0028(9) 0.0028(8) 0.0031(8) C25 0.0229(10) 0.0233(10) 0.0193(9) 0.0004(8) 0.0058(8) 0.0002(8) N26 0.0228(9) 0.0228(9) 0.0200(8) -0.0029(7) 0.0051(7) -0.0005(7) N27 0.0234(9) 0.0255(9) 0.0229(9) -0.0044(7) 0.0052(7) -0.0018(7) C28 0.0328(12) 0.0211(10) 0.0295(11) -0.0004(9) 0.0093(9) 0.0013(8) C29 0.0300(12) 0.0241(11) 0.0296(11) 0.0024(9) 0.0046(9) 0.0024(9) Cl30 0.0260(3) 0.0301(3) 0.0283(3) -0.0040(2) 0.0023(2) -0.0015(2) O31 0.0294(9) 0.0597(12) 0.0342(9) -0.0028(8) 0.0063(7) -0.0178(8) O32 0.0253(9) 0.0500(11) 0.0510(11) -0.0012(8) -0.0018(8) 0.0030(9) O33 0.0373(9) 0.0349(9) 0.0300(8) -0.0085(7) 0.0042(7) -0.0078(7) O34 0.0712(14) 0.0317(10) 0.0505(11) -0.0119(9) 0.0036(10) 0.0095(8) Cl35 0.0304(3) 0.0218(2) 0.0210(2) 0.0003(2) 0.0089(2) -0.00018(18) O36 0.0387(10) 0.0283(9) 0.0586(11) -0.0065(7) 0.0206(8) 0.0012(8) O37 0.0300(9) 0.0482(10) 0.0395(9) -0.0008(8) 0.0168(7) -0.0046(8) O38 0.0658(12) 0.0397(10) 0.0182(8) 0.0187(9) 0.0033(8) -0.0022(7) O39 0.0468(10) 0.0296(8) 0.0234(8) 0.0057(7) 0.0041(7) 0.0062(6) O40 0.0264(8) 0.0281(8) 0.0252(8) -0.0032(7) 0.0054(7) 0.0011(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 Fe1 N2 . 2.7468(17) yes Fe1 N5 . 2.1563(16) yes Fe1 N8 . 2.2547(16) yes Fe1 N14 . 2.1575(17) yes Fe1 N17 . 2.2413(17) yes Fe1 N23 . 2.1628(17) yes Fe1 N26 . 2.2457(16) yes N2 C3 . 1.461(2) ? N2 C21 . 1.473(3) ? N2 C12 . 1.475(3) ? C3 C4 . 1.525(3) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 N5 . 1.464(2) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? N5 C6 . 1.278(3) ? C6 C7 . 1.456(3) ? C6 H6 . 0.9500 ? C7 N8 . 1.345(2) ? C7 C11 . 1.403(3) ? N8 N9 . 1.344(2) ? N9 C10 . 1.349(3) ? N9 H9 . 0.8800 ? C10 C11 . 1.373(3) ? C10 H10 . 0.9500 ? C11 H11 . 0.9500 ? C12 C13 . 1.526(3) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 N14 . 1.461(2) ? C13 H13A . 0.9900 ? C13 H13B . 0.9900 ? N14 C15 . 1.272(3) ? C15 C16 . 1.463(3) ? C15 H15 . 0.9500 ? C16 N17 . 1.341(3) ? C16 C20 . 1.398(3) ? N17 N18 . 1.348(2) ? N18 C19 . 1.344(3) ? N18 H18 . 0.8800 ? C19 C20 . 1.377(3) ? C19 H19 . 0.9500 ? C20 H20 . 0.9500 ? C21 C22 . 1.522(3) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C22 N23 . 1.463(3) ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? N23 C24 . 1.273(3) ? C24 C25 . 1.456(3) ? C24 H24 . 0.9500 ? C25 N26 . 1.339(3) ? C25 C29 . 1.400(3) ? N26 N27 . 1.342(2) ? N27 C28 . 1.346(3) ? N27 H27 . 0.8800 ? C28 C29 . 1.370(3) ? C28 H28 . 0.9500 ? C29 H29 . 0.9500 ? Cl30 O34 . 1.4282(17) ? Cl30 O33 . 1.4332(15) ? Cl30 O32 . 1.4372(17) ? Cl30 O31 . 1.4502(17) ? Cl35 O39 . 1.4332(15) ? Cl35 O38 . 1.4341(16) ? Cl35 O37 . 1.4355(16) ? Cl35 O36 . 1.4394(16) ? O40 H40A . 0.854(19) ? O40 H40B . 0.84(2) ?