#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006413.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_2006413 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1036 _journal_page_last 1037 _publ_section_title ; A Tetrahydrofuran Ring-Opening Product: trans-Tetrachloro{4-[2-(phenylamino)pyridinio]butoxido-O}(tetrahydrofuran-O) zirconium(IV) ; loop_ _publ_author_name 'Polamo, Mika' 'Mutikainen, Ilpo' 'Leskel\"a, Markku' _chemical_formula_sum '[ZrCl4 (C4 H8 O)(C15 H18 N2 O)]' _chemical_formula_structural '[Zr Cl4 (C4 H8 O) (C15 H18 N1 O1)' _chemical_formula_weight 547.44 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.251(5) _cell_length_b 11.548(5) _cell_length_c 14.280(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.89(3) _cell_angle_gamma 90.00 _cell_volume 2315.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193.0(10) _exptl_crystal_density_diffrn 1.571 _diffrn_ambient_temperature 193.0(10) _refine_ls_R_factor_obs .0435 _refine_ls_wR_factor_obs .0994 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Zr1 .25243(2) .24733(3) .36527(2) .03647(14) Uani d . 1 . Zr Cl1 .35443(8) .40199(9) .31638(8) .0466(3) Uani d . 1 . Cl Cl2 .16540(7) .40190(9) .44123(8) .0431(3) Uani d . 1 . Cl Cl3 .16276(8) .10127(9) .44306(7) .0433(3) Uani d . 1 . Cl Cl4 .35480(9) .09502(10) .31699(9) .0541(3) Uani d . 1 . Cl O1 .3573(2) .2430(2) .5052(2) .0461(7) Uani d . 1 . O C2 .4038(4) .3418(4) .5586(3) .0572(13) Uani d . 1 . C H2A .3568(4) .3879(4) .5864(3) .074 Uiso calc R 1 . H H2B .4341(4) .3925(4) .5165(3) .074 Uiso calc R 1 . H C3 .4781(3) .2913(5) .6363(3) .0603(13) Uani d . 1 . C H3A .5390(3) .3340(5) .6413(3) .078 Uiso calc R 1 . H H3B .4563(3) .2945(5) .6984(3) .078 Uiso calc R 1 . H C4 .4897(3) .1678(5) .6065(4) .0639(14) Uani d . 1 . C H4A .5365(3) .1618(5) .5630(4) .083 Uiso calc R 1 . H H4B .5100(3) .1173(5) .6623(4) .083 Uiso calc R 1 . H C5 .3913(4) .1372(4) .5568(4) .0614(14) Uani d . 1 . C H5A .3932(4) .0717(4) .5124(4) .080 Uiso calc R 1 . H H5B .3499(4) .1160(4) .6032(4) .080 Uiso calc R 1 . H O6 .1648(2) .2481(2) .2492(2) .0449(7) Uani d . 1 . O C7 .1047(3) .2670(4) .1616(3) .0486(11) Uani d . 1 . C H7A .0619(3) .1997(4) .1456(3) .063 Uiso calc R 1 . H H7B .1432(3) .2764(4) .1106(3) .063 Uiso calc R 1 . H C8 .0463(3) .3755(4) .1691(3) .0496(11) Uani d . 1 . C H8A .0149(3) .3687(4) .2255(3) .065 Uiso calc R 1 . H H8B -.0043(3) .3805(4) .1123(3) .065 Uiso calc R 1 . H C9 .1047(3) .4874(3) .1770(3) .0435(10) Uani d . 1 . C H9A .1687(3) .4727(3) .2147(3) .057 Uiso calc R 1 . H H9B .1130(3) .5130(3) .1128(3) .057 Uiso calc R 1 . H C10 .0557(3) .5823(3) .2242(3) .0427(10) Uani d . 1 . C H10A -.0121(3) .5867(3) .1937(3) .055 Uiso calc R 1 . H H10B .0579(3) .5627(3) .2921(3) .055 Uiso calc R 1 . H N11 .1014(2) .6962(3) .2169(2) .0402(8) Uani d . 1 . N C12 .1730(3) .7363(3) .2845(3) .0392(9) Uani d . 1 . C C13 .2128(3) .8445(3) .2692(3) .0469(11) Uani d . 1 . C H13A .2634(3) .8742(3) .3150(3) .061 Uiso calc R 1 . H C14 .1799(3) .9073(4) .1899(3) .0527(12) Uani d . 1 . C H14A .2071(3) .9808(4) .1812(3) .068 Uiso calc R 1 . H C15 .1063(3) .8649(4) .1208(3) .0514(11) Uani d . 1 . C H15A .0833(3) .9082(4) .0650(3) .067 Uiso calc R 1 . H C16 .0688(3) .7594(4) .1362(3) .0467(10) Uani d . 1 . C H16A .0189(3) .7287(4) .0901(3) .061 Uiso calc R 1 . H N17 .2033(2) .6710(3) .3626(2) .0465(9) Uani d . 1 . N H17A .1860(2) .5977(3) .3603(2) .060 Uiso calc R 1 . H C18 .2611(3) .7110(3) .4487(3) .0411(10) Uani d . 1 . C C19 .2434(3) .8141(4) .4891(3) .0493(11) Uani d . 1 . C H19A .1932(3) .8625(4) .4591(3) .064 Uiso calc R 1 . H C20 .2986(3) .8474(4) .5737(3) .0558(12) Uani d . 1 . C H20A .2870(3) .9197(4) .6015(3) .073 Uiso calc R 1 . H C21 .3701(3) .7772(4) .6180(3) .0602(13) Uani d . 1 . C H21A .4087(3) .8010(4) .6758(3) .078 Uiso calc R 1 . H C22 .3856(3) .6718(4) .5781(4) .0609(13) Uani d . 1 . C H22A .4336(3) .6217(4) .6100(4) .079 Uiso calc R 1 . H C23 .3325(3) .6378(4) .4926(3) .0481(11) Uani d . 1 . C H23A .3445(3) .5660(4) .4644(3) .063 Uiso calc R 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 Zr1 .0396(2) .0309(2) .0370(2) .0000(2) .00105(15) .0018(2) Cl1 .0473(7) .0430(6) .0498(7) -.0059(5) .0087(5) .0031(5) Cl2 .0437(6) .0333(5) .0523(7) .0030(4) .0083(5) .0001(5) Cl3 .0467(7) .0357(6) .0465(6) -.0013(5) .0051(5) .0053(5) Cl4 .0579(8) .0416(6) .0653(8) .0038(5) .0175(6) -.0059(5) O1 .051(2) .0357(15) .0461(15) .0023(15) -.0062(12) .0051(14) C2 .070(3) .046(3) .050(3) .006(2) -.008(2) -.005(2) C3 .045(3) .081(4) .051(3) -.001(2) -.002(2) -.003(2) C4 .053(3) .073(4) .062(3) .011(3) -.002(2) .018(3) C5 .068(4) .045(3) .064(3) .010(2) -.009(3) .013(2) O6 .056(2) .0384(15) .0372(14) -.0068(15) -.0003(12) .0005(14) C7 .060(3) .041(2) .040(2) -.008(2) -.005(2) -.002(2) C8 .048(3) .039(2) .060(3) -.010(2) .003(2) .001(2) C9 .045(2) .037(2) .049(2) -.001(2) .007(2) -.001(2) C10 .040(2) .040(2) .048(3) -.003(2) .007(2) .001(2) N11 .038(2) .035(2) .047(2) .001(2) .005(2) .000(2) C12 .039(2) .031(2) .047(2) .006(2) .006(2) .001(2) C13 .044(3) .035(2) .060(3) -.002(2) .004(2) -.001(2) C14 .058(3) .038(2) .063(3) -.001(2) .016(2) .003(2) C15 .061(3) .045(3) .048(3) .003(2) .008(2) .006(2) C16 .049(2) .045(2) .044(2) .011(2) .003(2) .003(2) N17 .048(2) .030(2) .056(2) -.003(2) -.007(2) .004(2) C18 .036(2) .036(2) .049(2) -.003(2) .001(2) .000(2) C19 .045(3) .038(2) .062(3) .001(2) .004(2) -.001(2) C20 .061(3) .043(3) .063(3) -.010(2) .011(3) -.009(2) C21 .052(3) .072(4) .052(3) -.019(3) -.002(2) -.003(2) C22 .046(3) .061(3) .071(3) .006(2) -.004(3) .012(3) C23 .041(2) .045(3) .055(3) .002(2) .002(2) .002(2) 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 Zr1 O6 . 1.896(3) y Zr1 O1 . 2.281(3) y Zr1 Cl4 . 2.4581(12) y Zr1 Cl1 . 2.4777(12) y Zr1 Cl3 . 2.4899(12) y Zr1 Cl2 . 2.5226(11) y O1 C5 . 1.466(5) n O1 C2 . 1.466(5) n C2 C3 . 1.513(6) n C3 C4 . 1.505(7) n C4 C5 . 1.500(6) n O6 C7 . 1.407(5) n C7 C8 . 1.518(6) n C8 C9 . 1.531(5) n C9 C10 . 1.518(5) n C10 N11 . 1.480(5) n N11 C12 . 1.359(5) n N11 C16 . 1.375(5) n C12 N17 . 1.354(5) n C12 C13 . 1.405(5) n C13 C14 . 1.359(6) n C14 C15 . 1.398(6) n C15 C16 . 1.364(6) n N17 C18 . 1.435(5) n C18 C19 . 1.365(6) n C18 C23 . 1.387(6) n C19 C20 . 1.378(6) n C20 C21 . 1.369(6) n C21 C22 . 1.378(7) n C22 C23 . 1.379(6) n