#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008448.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_2008448 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _journal_page_first 706 _journal_page_last 707 _publ_section_title ; Dichloro(2,3,6,8,11,12,15,17-octamethyl-5,9,14,18-tetraaza- dibenzo[a,h]cyclotetradecene-\k^4^N)zirconium(IV) tetrahydrofuran hemisolvate ; loop_ _publ_author_name 'Corden, Jonathan P' 'Errington, William' 'Moore, Peter' 'Wallbridge, Malcolm G H' _chemical_formula_moiety 'C26 H30 Cl2 N4 Zr, 0.5C4 H8 O' _chemical_formula_sum 'C28 H34 Cl2 N4 O0.5 Zr' _[local]_cod_chemical_formula_sum_orig 'C28 H34 Cl2 N4 O0.50 Zr' _chemical_formula_iupac '[Zr Cl2 (C26 H30 N4)], 0.5C4 H8 O' _chemical_formula_weight 596.71 _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 8.958(5) _cell_length_b 13.258(7) _cell_length_c 14.769(8) _cell_angle_alpha 71.61(5) _cell_angle_beta 88.37(4) _cell_angle_gamma 70.53(4) _cell_volume 1563.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.267 _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 Zr1 .08607(10) .26699(6) .35263(6) .0431(3) Uani d . 1 . . Zr N1 -.0412(8) .2964(5) .4737(4) .0425(18) Uani d . 1 . . N N2 -.1580(8) .3464(5) .2915(4) .0411(17) Uani d . 1 . . N N3 .0426(7) .1548(5) .2851(4) .0394(17) Uani d . 1 . . N N4 .1663(7) .1076(5) .4670(4) .0383(17) Uani d . 1 . . N Cl1 .1100(3) .45752(15) .31739(15) .0591(7) Uani d . 1 . . Cl Cl2 .3564(2) .21420(16) .29232(15) .0620(7) Uani d . 1 . . Cl C1 -.2370(9) .3538(6) .5865(5) .059(3) Uani d . 1 . . C H1A -.1666 .2896 .6352 .089 Uiso calc R 1 . . H H1B -.3440 .3540 .5931 .089 Uiso calc R 1 . . H H1C -.2304 .4220 .5930 .089 Uiso calc R 1 . . H C2 -.1901(10) .3472(6) .4898(6) .042(2) Uani d . 1 . . C C3 -.3120(9) .3924(6) .4165(6) .045(2) Uani d . 1 . . C H3A -.4130 .4270 .4324 .054 Uiso calc R 1 . . H C4 -.3011(10) .3919(6) .3236(6) .046(2) Uani d . 1 . . C C5 -.4529(9) .4352(6) .2569(5) .065(3) Uani d . 1 . . C H5A -.4425 .3874 .2182 .097 Uiso calc R 1 . . H H5B -.4693 .5112 .2162 .097 Uiso calc R 1 . . H H5C -.5420 .4341 .2944 .097 Uiso calc R 1 . . H C6 -.1305(9) .3401(7) .1982(6) .046(2) Uani d D 1 . . C C7 -.1921(9) .4314(6) .1118(6) .053(3) Uani d D 1 . . C H7A -.2628 .5001 .1140 .064 Uiso calc R 1 . . H C8 -.1476(10) .4187(8) .0243(7) .060(3) Uani d D 1 . . C C9 -.2138(11) .5165(7) -.0683(5) .103(4) Uani d . 1 . . C H9A -.2998 .5752 -.0553 .155 Uiso calc R 1 . . H H9B -.2519 .4903 -.1135 .155 Uiso calc R 1 . . H H9C -.1315 .5457 -.0944 .155 Uiso calc R 1 . . H C10 -.0324(11) .3143(8) .0221(6) .060(3) Uani d D 1 . . C C11 .0261(12) .3017(8) -.0749(5) .099(4) Uani d . 1 . . C H11A .1092 .2300 -.0636 .148 Uiso calc R 1 . . H H11B .0661 .3614 -.1069 .148 Uiso calc R 1 . . H H11C -.0607 .3060 -.1142 .148 Uiso calc R 1 . . H C12 .0327(9) .2267(6) .1068(5) .045(2) Uani d D 1 . . C H12A .1140 .1617 .1055 .054 Uiso calc R 1 . . H C13 -.0226(9) .2357(7) .1922(5) .041(2) Uani d D 1 . . C C14 .0694(9) .0444(7) .3096(6) .046(2) Uani d . 1 . . C C15 .0150(10) -.0053(6) .2423(5) .065(3) Uani d . 1 . . C H15A -.0770 .0505 .2021 .098 Uiso calc R 1 . . H H15B -.0112 -.0701 .2790 .098 Uiso calc R 1 . . H H15C .0988 -.0276 .2031 .098 Uiso calc R 1 . . H C16 .1441(9) -.0300(6) .4010(5) .042(2) Uani d . 1 . . C H16A .1654 -.1068 .4121 .051 Uiso calc R 1 . . H C17 .1885(9) -.0007(6) .4753(6) .038(2) Uani d . 1 . . C C18 .2627(9) -.0957(5) .5668(5) .055(3) Uani d . 1 . . C H18A .2369 -.0685 .6203 .082 Uiso calc R 1 . . H H18B .3760 -.1231 .5649 .082 Uiso calc R 1 . . H H18C .2223 -.1560 .5734 .082 Uiso calc R 1 . . H C19 .2062(10) .1473(6) .5392(5) .038(2) Uani d D 1 . . C C20 .3469(9) .0992(6) .5992(5) .044(2) Uani d D 1 . . C H20A .4213 .0318 .5968 .052 Uiso calc R 1 . . H C21 .3780(9) .1497(6) .6620(5) .039(2) Uani d D 1 . . C C22 .5264(9) .0960(7) .7272(5) .060(3) Uani d . 1 . . C H22A .5806 .0214 .7243 .090 Uiso calc R 1 . . H H22B .5004 .0914 .7916 .090 Uiso calc R 1 . . H H22C .5940 .1407 .7077 .090 Uiso calc R 1 . . H C23 .2694(11) .2533(7) .6626(5) .044(2) Uani d D 1 . . C C24 .3034(10) .3154(7) .7257(6) .070(3) Uani d . 1 . . C H24A .2115 .3803 .7220 .105 Uiso calc R 1 . . H H24B .3919 .3394 .7041 .105 Uiso calc R 1 . . H H24C .3281 .2658 .7907 .105 Uiso calc R 1 . . H C25 .1304(10) .3054(7) .6019(5) .045(2) Uani d D 1 . . C H25A .0620 .3764 .6005 .054 Uiso calc R 1 . . H C26 .0935(9) .2509(6) .5429(5) .038(2) Uani d D 1 . . C O1S .282(6) .831(3) .036(3) .17(2) Uiso d PDU .25 A 1 O C1S .280(4) .938(2) .020(2) .049(9) Uiso d PDU .25 A 1 C H1SA .3397 .9442 .0704 .059 Uiso calc PR .25 A 1 H H1SB .1735 .9925 .0086 .059 Uiso calc PR .25 A 1 H C2S .362(4) .944(2) -.0668(19) .062(12) Uiso d PDU .25 A 1 C H2SA .2926 .9511 -.1196 .074 Uiso calc PR .25 A 1 H H2SB .4009 1.0066 -.0845 .074 Uiso calc PR .25 A 1 H C3S .490(3) .839(2) -.041(3) .069(12) Uiso d PDU .25 A 1 C H3SA .5701 .8355 .0032 .083 Uiso calc PR .25 A 1 H H3SB .5387 .8228 -.0971 .083 Uiso calc PR .25 A 1 H C4S .403(6) .762(3) .004(3) .091(16) Uiso d PDU .25 A 1 C H4SA .3650 .7353 -.0415 .109 Uiso calc PR .25 A 1 H H4SB .4678 .6975 .0566 .109 Uiso calc PR .25 A 1 H O2S .370(3) .761(2) .0717(19) .098(10) Uiso d PDU .25 B 2 O C5S .482(4) .757(3) .014(2) .084(16) Uiso d PDU .25 B 2 C H5S1 .5256 .6817 .0076 .101 Uiso calc PR .25 B 2 H H5S2 .5673 .7750 .0362 .101 Uiso calc PR .25 B 2 H C6S .404(4) .841(3) -.0774(17) .059(11) Uiso d PDU .25 B 2 C H6S1 .4791 .8657 -.1192 .070 Uiso calc PR .25 B 2 H H6S2 .3421 .8131 -.1104 .070 Uiso calc PR .25 B 2 H C7S .303(6) .930(2) -.042(3) .13(2) Uiso d PDU .25 B 2 C H7S1 .3596 .9762 -.0318 .150 Uiso calc PR .25 B 2 H H7S2 .2085 .9772 -.0857 .150 Uiso calc PR .25 B 2 H C8S .264(5) .862(3) .047(3) .091(19) Uiso d PDU .25 B 2 C H8S1 .2630 .8965 .0959 .109 Uiso calc PR .25 B 2 H H8S2 .1593 .8581 .0385 .109 Uiso calc PR .25 B 2 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 .0381(6) .0361(5) .0507(5) -.0098(4) .0021(4) -.0113(4) N1 .035(5) .027(4) .056(4) -.003(3) .002(4) -.009(3) N2 .046(5) .038(4) .039(4) -.014(4) .001(4) -.012(3) N3 .033(4) .031(4) .048(4) -.006(3) .003(3) -.009(3) N4 .034(4) .032(4) .047(4) -.007(3) .003(3) -.015(3) Cl1 .0642(17) .0404(13) .0770(15) -.0201(12) .0189(13) -.0238(11) Cl2 .0404(15) .0515(13) .0890(17) -.0090(11) .0149(13) -.0238(12) C1 .056(6) .063(6) .061(6) -.017(5) .017(5) -.028(5) C2 .036(6) .033(5) .053(6) -.009(4) -.001(5) -.013(4) C3 .031(5) .045(5) .058(6) -.009(4) .007(5) -.021(5) C4 .036(6) .027(5) .062(6) .001(4) .001(5) -.009(4) C5 .045(6) .069(6) .072(6) -.023(5) -.006(5) -.007(5) C6 .040(6) .047(5) .049(6) -.019(5) .000(4) -.012(5) C7 .039(6) .052(6) .058(6) -.006(5) -.013(5) -.011(5) C8 .049(6) .074(7) .050(6) -.029(6) -.013(5) .001(6) C9 .125(10) .097(8) .053(6) -.039(7) -.001(6) .024(6) C10 .066(7) .073(7) .056(6) -.038(6) .008(5) -.025(6) C11 .106(9) .145(10) .041(6) -.039(7) .011(6) -.028(6) C12 .054(6) .049(5) .034(5) -.018(5) .006(5) -.017(5) C13 .041(6) .048(5) .037(5) -.018(5) -.007(4) -.013(5) C14 .033(6) .056(6) .047(5) -.012(5) .005(4) -.018(5) C15 .083(8) .059(6) .066(6) -.031(5) -.013(5) -.028(5) C16 .037(5) .035(5) .053(5) -.012(4) -.006(4) -.009(4) C17 .027(5) .032(5) .054(6) -.012(4) .007(4) -.010(4) C18 .064(6) .029(5) .061(6) -.017(4) -.006(5) .001(4) C19 .041(6) .033(5) .039(5) -.015(4) .006(4) -.010(4) C20 .040(6) .036(5) .044(5) -.010(4) .014(5) -.002(4) C21 .034(6) .037(5) .040(5) -.007(4) .001(4) -.009(4) C22 .041(6) .084(7) .062(6) -.023(5) -.009(5) -.029(5) C23 .048(6) .054(6) .044(5) -.031(5) .012(5) -.020(5) C24 .066(7) .075(7) .077(6) -.029(6) -.005(5) -.029(6) C25 .047(6) .045(5) .045(5) -.017(5) .006(5) -.016(4) C26 .029(5) .038(5) .042(5) -.010(4) .012(4) -.007(4) 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 N4 . 2.154(5) y Zr1 N1 . 2.163(6) y Zr1 N2 . 2.164(6) y Zr1 N3 . 2.168(6) y Zr1 Cl1 . 2.495(2) y Zr1 Cl2 . 2.508(3) y N1 C2 . 1.331(9) ? N1 C26 . 1.436(9) ? N2 C4 . 1.364(9) ? N2 C6 . 1.417(9) ? N3 C14 . 1.330(9) ? N3 C13 . 1.441(8) ? N4 C17 . 1.347(8) ? N4 C19 . 1.429(9) ? C1 C2 . 1.497(9) ? C2 C3 . 1.395(9) ? C3 C4 . 1.374(9) ? C4 C5 . 1.533(9) ? C6 C7 . 1.421(9) ? C6 C13 . 1.428(10) ? C7 C8 . 1.385(10) ? C8 C10 . 1.434(11) ? C8 C9 . 1.522(9) ? C10 C12 . 1.388(10) ? C10 C11 . 1.551(10) ? C12 C13 . 1.367(9) ? C14 C16 . 1.420(9) ? C14 C15 . 1.522(10) ? C16 C17 . 1.382(9) ? C17 C18 . 1.508(8) ? C19 C20 . 1.397(10) ? C19 C26 . 1.424(10) ? C20 C21 . 1.385(10) ? C21 C23 . 1.397(10) ? C21 C22 . 1.486(9) ? C23 C25 . 1.389(10) ? C23 C24 . 1.518(10) ? C25 C26 . 1.401(10) ? O1S C1S . 1.347(16) ? O1S C4S . 1.348(16) ? C1S C2S . 1.449(16) ? C2S C3S . 1.422(19) ? C3S C4S . 1.468(16) ? O2S C5S . 1.297(16) ? O2S C8S . 1.302(16) ? C5S C6S . 1.462(16) ? C6S C7S . 1.46(2) ? C7S C8S . 1.444(16) ? _cod_database_code 2008448