#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011456.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_2011456 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first e448 _journal_page_last e449 _publ_section_title ; Low-temperature tris(tert-butyl 3-oxobutanoato)iron(III) ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Urs, Usha K.' 'Shalini, K.' 'Shivashankar, S. A.' 'Guru Row, T. N.' _chemical_formula_sum 'C24 H39 Fe O9' _chemical_formula_iupac '[Fe (C8 H13 O3)3]' _chemical_formula_weight 527.4 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.598(3) _cell_length_b 16.056(4) _cell_length_c 18.112(4) _cell_angle_alpha 90 _cell_angle_beta 100.88(2) _cell_angle_gamma 90 _cell_volume 2741.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _exptl_crystal_density_diffrn 1.278 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 .80599(6) .23407(4) .36506(3) .03710(17) Uani d . 1 . . Fe O7 .7703(3) .14036(19) .42707(16) .0424(7) Uani d . 1 . . O O9 1.2082(3) .1857(2) .49675(16) .0468(8) Uani d . 1 . . O O3 .8416(3) .09677(19) .17076(16) .0440(7) Uani d . 1 . . O O5 .7753(3) .31212(19) .44253(16) .0438(7) Uani d . 1 . . O O4 .8704(3) .33228(18) .30941(15) .0390(7) Uani d . 1 . . O O8 1.0169(3) .22319(19) .41152(15) .0416(7) Uani d . 1 . . O O6 .9472(3) .46255(17) .29270(16) .0431(7) Uani d . 1 . . O O2 .6174(3) .24213(18) .30226(14) .0380(6) Uani d . 1 . . O O1 .8590(3) .15981(18) .28328(16) .0398(7) Uani d . 1 . . O C12 .9721(5) .4433(3) .2163(2) .0396(10) Uani d . 1 . . C C20 1.3070(4) .2398(3) .4636(2) .0400(9) Uani d . 1 . . C C14 .8346(5) .4206(3) .1656(2) .0484(11) Uani d . 1 . . C H14A .7994 .368 .1825 .073 Uiso calc R 1 . . H H14B .8501 .4144 .114 .073 Uiso calc R 1 . . H H14C .7647 .4647 .1674 .073 Uiso calc R 1 . . H C1 .5783(4) .2273(3) .2305(2) .0359(8) Uani d . 1 . . C C2 .6555(4) .1823(3) .1881(2) .0417(10) Uani d . 1 . . C H2 .6174 .1744 .1363 .05 Uiso calc R 1 . . H C7 1.0941(5) .1290(3) .1993(3) .0479(11) Uani d . 1 . . C H7A 1.071 .1672 .1566 .072 Uiso calc R 1 . . H H7B 1.1885 .1051 .2006 .072 Uiso calc R 1 . . H H7C 1.0932 .1595 .2461 .072 Uiso calc R 1 . . H C4 .9856(5) .0600(3) .1911(3) .0411(10) Uani d . 1 . . C C8 .4354(4) .2607(3) .1958(2) .0433(10) Uani d . 1 . . C H8A .3622 .2316 .217 .065 Uiso calc R 1 . . H H8B .4188 .2519 .1413 .065 Uiso calc R 1 . . H H8C .4317 .3204 .2065 .065 Uiso calc R 1 . . H C18 .9926(5) .1279(3) .5085(2) .0449(10) Uani d . 1 . . C H18 1.0421 .1028 .5534 .054 Uiso calc R 1 . . H C3 .7892(4) .1472(3) .2179(2) .0378(9) Uani d . 1 . . C C17 .8514(5) .1097(3) .4859(2) .0390(9) Uani d . 1 . . C C10 .8793(5) .4339(3) .4057(2) .0433(10) Uani d . 1 . . C H10 .9095 .4889 .4202 .052 Uiso calc R 1 . . H C19 1.0691(4) .1820(3) .4685(2) .0374(9) Uani d . 1 . . C C13 1.0846(5) .3762(3) .2201(3) .0514(12) Uani d . 1 . . C H13A 1.1636 .3884 .2614 .077 Uiso calc R 1 . . H H13B 1.1193 .3748 .1726 .077 Uiso calc R 1 . . H H13C 1.0435 .322 .2287 .077 Uiso calc R 1 . . H C21 1.3078(5) .2154(4) .3840(3) .0649(15) Uani d . 1 . . C H21A 1.3196 .1549 .381 .097 Uiso calc R 1 . . H H21B 1.3864 .2434 .3666 .097 Uiso calc R 1 . . H H21C 1.2178 .2318 .3521 .097 Uiso calc R 1 . . H C11 .8986(4) .4050(3) .3346(2) .0392(9) Uani d . 1 . . C C16 .7988(6) .4231(3) .5290(3) .0523(12) Uani d . 1 . . C H16A .6995 .4166 .5341 .078 Uiso calc R 1 . . H H16B .8232 .4825 .5307 .078 Uiso calc R 1 . . H H16C .8603 .3941 .5703 .078 Uiso calc R 1 . . H C5 .9941(5) .0072(4) .1226(3) .0636(15) Uani d . 1 . . C H5A .9225 -.037 .1177 .095 Uiso calc R 1 . . H H5B 1.0887 -.0177 .1283 .095 Uiso calc R 1 . . H H5C .9764 .0423 .0775 .095 Uiso calc R 1 . . H C22 1.2692(6) .3291(3) .4708(3) .0604(13) Uani d . 1 . . C H22A 1.1799 .3412 .4364 .091 Uiso calc R 1 . . H H22B 1.3446 .3644 .4583 .091 Uiso calc R 1 . . H H22C 1.2582 .3403 .5226 .091 Uiso calc R 1 . . H C24 .7791(5) .0521(3) .5319(3) .0512(12) Uani d . 1 . . C H24A .7034 .0821 .5502 .077 Uiso calc R 1 . . H H24B .8484 .0315 .5749 .077 Uiso calc R 1 . . H H24C .7384 .0049 .5008 .077 Uiso calc R 1 . . H C15 1.0252(6) .5251(3) .1916(3) .0557(13) Uani d . 1 . . C H15A .9521 .5678 .1909 .084 Uiso calc R 1 . . H H15B 1.0466 .519 .1411 .084 Uiso calc R 1 . . H H15C 1.1113 .5415 .2268 .084 Uiso calc R 1 . . H C9 .8190(5) .3869(3) .4553(2) .0392(9) Uani d . 1 . . C C6 .9989(6) .0061(3) .2594(4) .0711(17) Uani d . 1 . . C H6A .9909 .0405 .3031 .107 Uiso calc R 1 . . H H6B 1.0913 -.0219 .2682 .107 Uiso calc R 1 . . H H6C .9231 -.0358 .2517 .107 Uiso calc R 1 . . H C23 1.4496(5) .2195(4) .5133(3) .0674(15) Uani d . 1 . . C H23A 1.4444 .2298 .566 .101 Uiso calc R 1 . . H H23B 1.5234 .2547 .4989 .101 Uiso calc R 1 . . H H23C 1.4726 .1608 .5068 .101 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 Fe1 .0346(3) .0435(3) .0344(3) -.0002(3) .0096(2) .0023(3) O7 .0386(17) .0480(18) .0414(16) -.0057(14) .0094(13) .0079(14) O9 .0346(16) .056(2) .0481(17) -.0070(15) .0023(13) .0123(15) O3 .0320(15) .0563(19) .0435(17) .0059(14) .0064(13) -.0144(14) O5 .0460(18) .0499(19) .0384(15) -.0042(15) .0155(13) -.0053(14) O4 .0438(17) .0340(16) .0419(16) .0018(13) .0149(13) .0008(12) O8 .0362(16) .0508(18) .0375(14) -.0020(14) .0060(12) .0080(14) O6 .055(2) .0369(16) .0400(15) -.0039(14) .0151(14) -.0027(13) O2 .0324(14) .0447(17) .0375(14) .0020(13) .0077(11) -.0018(13) O1 .0363(16) .0447(17) .0372(15) .0066(13) .0042(12) -.0017(13) C12 .040(2) .038(2) .043(2) -.0009(19) .0115(19) .0026(18) C20 .032(2) .049(3) .0380(19) -.0028(19) .0054(16) .0045(19) C14 .043(3) .062(3) .040(2) -.004(2) .008(2) -.001(2) C1 .0305(19) .037(2) .041(2) -.0022(18) .0085(16) .0044(19) C2 .035(2) .052(3) .038(2) .005(2) .0082(18) .004(2) C7 .038(2) .050(3) .056(3) -.001(2) .009(2) -.004(2) C4 .031(2) .041(2) .052(2) .0033(18) .0093(19) -.002(2) C8 .034(2) .048(3) .047(2) .004(2) .0072(17) .002(2) C18 .045(3) .050(3) .039(2) -.003(2) .0063(19) .008(2) C3 .031(2) .039(2) .044(2) -.0004(18) .0096(18) .0006(18) C17 .036(2) .040(2) .042(2) .0016(19) .0132(18) .0047(19) C10 .049(3) .037(2) .044(2) -.002(2) .011(2) -.0020(19) C19 .037(2) .041(2) .033(2) .0008(19) .0054(17) -.0008(18) C13 .046(3) .052(3) .059(3) .008(2) .019(2) .005(2) C21 .047(3) .094(4) .058(3) -.005(3) .021(2) -.021(3) C11 .032(2) .042(2) .045(2) .0051(18) .0093(18) .0077(19) C16 .059(3) .056(3) .044(3) .001(2) .015(2) -.004(2) C5 .043(3) .073(4) .077(4) -.001(3) .017(3) -.033(3) C22 .063(3) .050(3) .067(3) -.011(3) .010(3) -.003(3) C24 .050(3) .052(3) .054(3) -.004(2) .016(2) .015(2) C15 .066(3) .045(3) .062(3) -.007(2) .025(3) .005(2) C9 .040(2) .043(2) .037(2) .008(2) .0094(18) -.0045(19) C6 .068(4) .054(3) .100(4) .018(3) .039(3) .030(3) C23 .037(3) .091(4) .069(3) -.008(3) -.001(2) .021(3) 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 O5 . 1.945(3) yes Fe1 O7 . 1.946(3) yes Fe1 O2 . 1.952(3) yes Fe1 O4 . 2.030(3) yes Fe1 O1 . 2.039(3) yes Fe1 O8 . 2.048(3) yes O7 C17 . 1.292(5) no O9 C19 . 1.338(5) no O9 C20 . 1.493(5) no O3 C3 . 1.341(5) no O3 C4 . 1.483(5) no O5 C9 . 1.278(5) no O4 C11 . 1.265(5) no O8 C19 . 1.249(5) no O6 C11 . 1.334(5) no O6 C12 . 1.481(5) no O2 C1 . 1.305(4) no O1 C3 . 1.263(5) no C12 C14 . 1.503(6) no C12 C15 . 1.506(6) no C12 C13 . 1.518(6) no C20 C22 . 1.491(7) no C20 C21 . 1.496(6) no C20 C23 . 1.524(6) no C1 C2 . 1.368(5) no C1 C8 . 1.496(6) no C2 C3 . 1.412(6) no C7 C4 . 1.508(6) no C4 C6 . 1.496(7) no C4 C5 . 1.518(6) no C18 C17 . 1.371(6) no C18 C19 . 1.421(6) no C17 C24 . 1.500(6) no C10 C9 . 1.382(6) no C10 C11 . 1.413(6) no C16 C9 . 1.502(6) no _cod_database_code 2011456