#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011105.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_2011105 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 749 _journal_page_last 757 _publ_section_title ; Polymorphs and pseudo-polymorphs of \m-oxo-bis{[bis(salicylidene)-propane-1,3-diamine]oxorhenium(V)} ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Kooijman, Huub' 'Bommel, Kjeld J. C. van' 'Verboom, Willem' 'Reinhoudt, David N.' 'Kroon, Jan' 'Spek, Anthony L.' _chemical_formula_moiety 'C34 H32 N4 O7 Re2, 4(C H Cl3)' _chemical_formula_sum 'C38 H36 Cl12 N4 O7 Re2' _chemical_formula_iupac '[Re2 O (C17 H16 N2 O3)2] , 4C H Cl3' _chemical_formula_weight 1458.53 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 10.137(10) _cell_length_b 18.733(15) _cell_length_c 16.131(11) _cell_angle_alpha 90 _cell_angle_beta 126.43(6) _cell_angle_gamma 90 _cell_volume 2465(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _exptl_crystal_density_diffrn 1.965 _diffrn_ambient_temperature 150 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_occupancy _atom_site_type_symbol Re1 .21608(7) .03730(3) .09915(5) .0261(2) Uani 1.000 Re O1 .1976(12) .0948(5) -.0132(8) .028(3) Uani 1.000 O O2 .1150(12) .1269(5) .1099(8) .031(3) Uani 1.000 O O3 .4150(12) .0536(5) .1976(8) .032(3) Uani 1.000 O O4 0 0 0 .029(4) Uani 1.000 O N1 .2910(14) -.0548(6) .0578(9) .026(3) Uani 1.000 N N2 .1940(15) -.0147(6) .2082(9) .029(3) Uani 1.000 N C1 .2301(17) .0746(8) -.0779(11) .027(4) Uani 1.000 C C2 .201(2) .1239(9) -.1509(12) .037(5) Uani 1.000 C C3 .2255(19) .1079(9) -.2247(11) .035(4) Uani 1.000 C C4 .2780(19) .0392(9) -.2292(12) .039(5) Uani 1.000 C C5 .3066(19) -.0102(8) -.1567(12) .034(4) Uani 1.000 C C6 .2805(18) .0042(8) -.0808(11) .029(4) Uani 1.000 C C7 .3042(17) -.0538(7) -.0154(12) .029(4) Uani 1.000 C C8 .3256(18) -.1198(7) .1154(11) .032(4) Uani 1.000 C C9 .2145(19) -.1350(8) .1493(13) .038(4) Uani 1.000 C C10 .252(2) -.0913(7) .2385(13) .036(4) Uani 1.000 C C11 .1316(19) .0158(8) .2493(12) .031(4) Uani 1.000 C C12 .0777(18) .0890(8) .2378(11) .030(4) Uani 1.000 C C13 .021(2) .1086(10) .2983(13) .043(5) Uani 1.000 C C14 -.044(2) .1734(9) .2869(12) .042(5) Uani 1.000 C C15 -.064(2) .2232(9) .2136(14) .044(5) Uani 1.000 C C16 -.0054(19) .2055(8) .1579(13) .034(4) Uani 1.000 C C17 .0613(18) .1392(8) .1660(12) .032(4) Uani 1.000 C Cl1 .4329(6) .2306(2) .2493(3) .0474(14) Uani 1.000 Cl Cl2 .2757(7) .3180(3) .0671(4) .0620(19) Uani 1.000 Cl Cl3 .5301(7) .2194(3) .1140(5) .0622(19) Uani 1.000 Cl C18 .362(2) .2351(8) .1217(12) .038(4) Uani 1.000 C Cl4 .6516(9) -.0009(3) .4612(4) .081(2) Uani 1.000 Cl Cl5 .5839(10) .1440(3) .4817(5) .091(3) Uani 1.000 Cl Cl6 .8584(9) .1138(5) .4787(6) .113(3) Uani 1.000 Cl C19 .659(2) .0870(10) .4309(13) .049(5) Uani 1.000 C H2 .16350 .17020 -.15030 .0450 Uiso 1.000 H H3 .20660 .14350 -.27270 .0420 Uiso 1.000 H H4 .29310 .02740 -.28030 .0470 Uiso 1.000 H H5 .34560 -.05610 -.15740 .0410 Uiso 1.000 H H7 .33430 -.09790 -.02890 .0360 Uiso 1.000 H H8A .44080 -.11800 .17770 .0380 Uiso 1.000 H H8B .31630 -.16040 .07290 .0380 Uiso 1.000 H H9A .09920 -.12630 .09000 .0460 Uiso 1.000 H H9B .22450 -.18610 .16770 .0460 Uiso 1.000 H H10A .37130 -.09170 .29330 .0440 Uiso 1.000 H H10B .19730 -.11320 .26700 .0440 Uiso 1.000 H H11 .11960 -.01340 .29260 .0380 Uiso 1.000 H H13 .03020 .07570 .34620 .0530 Uiso 1.000 H H14 -.07740 .18630 .32880 .0510 Uiso 1.000 H H15 -.11640 .26780 .20320 .0520 Uiso 1.000 H H16 -.01110 .23990 .11260 .0400 Uiso 1.000 H H18 .27770 .19720 .08160 .0460 Uiso 1.000 H H19 .58720 .09210 .35420 .0590 Uiso 1.000 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 Re1 .0248(3) .0253(3) .0276(3) -.0010(3) .0152(2) -.0006(3) O1 .029(5) .023(5) .031(5) .005(4) .017(4) .003(4) O2 .035(6) .023(4) .043(6) .002(4) .027(5) .006(4) O3 .031(5) .035(6) .033(5) -.010(4) .020(4) -.008(4) O4 .033(6) .033(7) .033(6) -.004(5) .026(5) -.003(6) N1 .025(6) .029(5) .020(5) -.004(4) .011(5) -.008(4) N2 .025(6) .033(5) .028(6) .010(5) .015(5) .010(4) C1 .022(7) .032(6) .028(7) -.008(6) .016(6) -.001(5) C2 .043(9) .039(7) .040(8) -.001(7) .030(8) -.001(6) C3 .037(8) .046(7) .021(7) .000(7) .016(6) .007(6) C4 .036(8) .050(8) .038(8) .006(8) .026(7) .002(7) C5 .035(8) .032(6) .038(8) -.010(6) .024(7) -.012(5) C6 .026(7) .028(6) .035(7) -.015(6) .019(6) -.012(5) C7 .026(7) .027(6) .036(7) -.001(5) .019(6) -.008(5) C8 .032(8) .023(6) .025(7) -.006(6) .009(6) -.008(5) C9 .032(8) .022(6) .055(9) .003(6) .023(7) .005(6) C10 .043(9) .027(6) .044(8) .003(6) .029(8) .012(6) C11 .037(8) .037(6) .028(7) .000(6) .024(7) .002(6) C12 .033(8) .035(6) .029(7) -.011(6) .022(6) -.016(5) C13 .043(9) .062(8) .032(8) .003(8) .026(7) -.013(7) C14 .039(9) .059(9) .031(8) -.009(7) .022(7) -.031(6) C15 .032(8) .045(8) .059(10) -.007(7) .030(8) -.021(6) C16 .036(8) .024(6) .048(9) -.011(6) .029(7) -.010(6) C17 .030(8) .031(6) .039(8) -.005(6) .022(6) -.010(5) Cl1 .050(3) .039(2) .043(2) -.0126(19) .022(2) -.0076(18) Cl2 .071(4) .046(3) .066(3) .011(2) .039(3) .016(2) Cl3 .061(3) .056(3) .090(4) -.007(2) .056(3) -.012(3) C18 .033(9) .037(7) .033(7) -.005(6) .014(7) -.006(6) Cl4 .108(5) .053(3) .054(3) -.006(3) .033(3) .004(3) Cl5 .133(6) .078(4) .063(4) .031(4) .058(4) .001(3) Cl6 .073(4) .165(7) .084(5) -.046(5) .037(4) -.021(5) C19 .048(9) .055(8) .023(9) -.005(8) .009(8) -.004(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 O1 . . 2.019(11) yes Re1 O2 . . 2.027(11) yes Re1 O3 . . 1.696(12) yes Re1 O4 . . 1.919(2) yes Re1 N1 . . 2.145(13) yes Re1 N2 . . 2.136(14) yes Cl1 C18 . . 1.733(17) no Cl2 C18 . . 1.743(17) no Cl3 C18 . . 1.80(2) no Cl4 C19 . . 1.73(2) no Cl5 C19 . . 1.77(2) no Cl6 C19 . . 1.76(2) no O1 C1 . . 1.32(2) no O2 C17 . . 1.32(2) no N1 C8 . . 1.443(18) no N1 C7 . . 1.26(2) no N2 C10 . . 1.517(18) no N2 C11 . . 1.29(3) no C1 C2 . . 1.38(2) no C1 C6 . . 1.43(2) no C2 C3 . . 1.39(3) no C3 C4 . . 1.41(3) no C4 C5 . . 1.38(2) no C5 C6 . . 1.42(3) no C6 C7 . . 1.43(2) no C8 C9 . . 1.54(3) no C9 C10 . . 1.50(2) no C11 C12 . . 1.45(2) no C12 C13 . . 1.44(3) no C12 C17 . . 1.42(2) no C13 C14 . . 1.34(3) no C14 C15 . . 1.42(3) no C15 C16 . . 1.38(3) no C16 C17 . . 1.38(2) no C2 H2 . . .9493 no C3 H3 . . .9512 no C4 H4 . . .9495 no C5 H5 . . .9492 no C7 H7 . . .9497 no C8 H8B . . .9902 no C8 H8A . . .9904 no C9 H9A . . .9898 no C9 H9B . . .9894 no C10 H10A . . .9871 no C10 H10B . . .9949 no C11 H11 . . .9502 no C13 H13 . . .9487 no C14 H14 . . .9495 no C15 H15 . . .9500 no C16 H16 . . .9500 no C18 H18 . . .9981 no C19 H19 . . 1.0001 no _cod_database_code 2011105