#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012241.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_2012241 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 1135 _journal_page_last 1137 _publ_section_title ; Tricarbonyl[1,1',1''-ethylidynetris(pyrazole-\kN^2^)]rhenium(I) bromide and tricarbonyl[methylidynetris(pyrazole-\kN^2^)]rhenium(I) iodide ethanol hemisolvate ; _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Gibson, Dorothy H.' 'Mashuta, Mark S.' 'He, Haiyang' _chemical_name_common ; tricarbonyl-tris(pyrazol-1-yl)methane rhenium(I) bromide ; _chemical_formula_moiety 'C13 H10 N6 O3 Re 1+, Br 1-' _chemical_formula_sum 'C13 H10 Br N6 O3 Re' _chemical_formula_iupac '[Re (C10 H10 N6) (C O)3] Br' _chemical_formula_weight 564.38 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.565(4) _cell_length_b 9.002(2) _cell_length_c 18.396(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.93(3) _cell_angle_gamma 90.00 _cell_volume 3434.0(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.183 _diffrn_ambient_temperature 293(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 Re .330173(9) .88021(2) .200909(10) .03940(9) Uani d . 1 . . Re Br .41970(3) .30361(6) .03315(3) .05823(16) Uani d . 1 . . Br N1 .37570(19) .6766(4) .2542(2) .0392(8) Uani d . 1 . . N O1 .4131(3) 1.0946(6) .3166(3) .0975(19) Uani d . 1 . . O C1 .3828(3) 1.0137(6) .2729(3) .0608(15) Uani d . 1 . . C C2 .2659(3) .8897(6) .2546(3) .0513(13) Uani d . 1 . . C O2 .2253(2) .8932(6) .2839(3) .0786(15) Uani d . 1 . . O N2 .39157(18) .5692(4) .2103(2) .0385(8) Uani d . 1 . . N N3 .4001(2) .8491(4) .1368(2) .0419(9) Uani d . 1 . . N O3 .2657(3) 1.1480(5) .1075(3) .0898(17) Uani d . 1 . . O C3 .2899(3) 1.0497(7) .1431(3) .0567(14) Uani d . 1 . . C N4 .40772(19) .7119(4) .1092(2) .0426(9) Uani d . 1 . . N C4 .3749(2) .5861(5) .1292(3) .0410(10) Uani d . 1 . . C H4A .3885 .4966 .1074 .049 Uiso calc R 1 . . H N5 .27532(18) .7188(5) .1207(2) .0417(9) Uani d . 1 . . N C5 .3949(3) .6235(6) .3244(3) .0488(12) Uani d . 1 . . C H5A .3906 .6731 .3671 .059 Uiso calc R 1 . . H N6 .30618(19) .6022(4) .0992(2) .0396(9) Uani d . 1 . . N C6 .4224(3) .4825(6) .3249(3) .0579(14) Uani d . 1 . . C H6A .4393 .4228 .3670 .070 Uiso calc R 1 . . H C7 .4197(2) .4504(6) .2525(3) .0478(12) Uani d . 1 . . C H7A .4342 .3640 .2348 .057 Uiso calc R 1 . . H C8 .4393(3) .9367(7) .1121(3) .0551(13) Uani d . 1 . . C H8A .4444 1.0380 .1219 .066 Uiso calc R 1 . . H C9 .4718(3) .8564(6) .0695(4) .0585(15) Uani d . 1 . . C H9A .5016 .8930 .0459 .070 Uiso calc R 1 . . H C10 .4518(2) .7169(6) .0691(3) .0507(13) Uani d . 1 . . C H10A .4655 .6369 .0455 .061 Uiso calc R 1 . . H C11 .2646(3) .5066(6) .0549(3) .0511(13) Uani d . 1 . . C H11A .2747 .4186 .0343 .061 Uiso calc R 1 . . H C12 .2043(3) .5642(8) .0463(3) .0636(15) Uani d . 1 . . C H12A .1654 .5242 .0179 .076 Uiso calc R 1 . . H C13 .2128(3) .6945(7) .0884(3) .0546(13) Uani d . 1 . . C H13A .1795 .7561 .0933 .066 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 Re .04381(13) .03421(12) .04082(12) .00841(8) .01270(8) -.00313(8) Br .0784(4) .0437(3) .0612(3) .0076(3) .0336(3) -.0052(2) N1 .040(2) .036(2) .041(2) .0048(17) .0114(17) -.0002(17) O1 .100(4) .062(3) .103(4) -.005(3) -.017(3) -.029(3) C1 .064(4) .043(3) .069(4) .009(3) .007(3) -.007(3) C2 .054(3) .057(3) .042(2) .019(3) .011(2) -.002(2) O2 .073(3) .113(4) .061(3) .034(3) .037(2) .006(2) N2 .039(2) .0323(19) .046(2) .0009(16) .0143(17) .0026(16) N3 .042(2) .030(2) .058(2) .0004(16) .0207(18) .0045(17) O3 .137(5) .056(3) .064(3) .040(3) .007(3) .007(2) C3 .073(4) .047(3) .048(3) .019(3) .013(3) -.007(2) N4 .046(2) .033(2) .056(2) .0020(17) .0268(19) .0012(17) C4 .046(3) .035(2) .048(3) .004(2) .023(2) -.0002(19) N5 .040(2) .046(2) .0386(19) .0029(18) .0108(16) -.0032(17) C5 .046(3) .055(3) .039(2) -.002(2) .002(2) .001(2) N6 .047(2) .037(2) .0385(19) .0011(17) .0177(17) -.0009(16) C6 .058(3) .054(3) .053(3) .001(3) .000(3) .017(3) C7 .040(3) .036(3) .066(3) .006(2) .012(2) .009(2) C8 .052(3) .040(3) .075(4) .000(2) .020(3) .012(3) C9 .053(3) .059(4) .073(4) .005(3) .034(3) .019(3) C10 .049(3) .051(3) .061(3) .012(3) .030(2) .012(3) C11 .063(3) .051(3) .036(2) -.009(3) .009(2) -.005(2) C12 .058(3) .075(4) .050(3) -.013(3) .001(3) -.002(3) C13 .040(3) .072(4) .049(3) .002(3) .008(2) -.003(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 Re C1 . 1.913(6) yes Re C2 . 1.911(5) yes Re C3 . 1.925(6) yes Re N1 . 2.181(4) yes Re N3 . 2.172(4) yes Re N5 . 2.175(4) yes N1 C5 . 1.333(6) no N1 N2 . 1.361(5) no O1 C1 . 1.146(7) no C2 O2 . 1.150(7) no N2 C7 . 1.362(6) no N2 C4 . 1.444(6) no N3 C8 . 1.326(7) no N3 N4 . 1.362(5) no O3 C3 . 1.139(7) no N4 C10 . 1.354(6) no N4 C4 . 1.436(6) no C4 N6 . 1.439(6) no C4 H4A . .98 no N5 C13 . 1.335(6) no N5 N6 . 1.359(5) no C5 C6 . 1.400(8) no C5 H5A . .93 no N6 C11 . 1.345(6) no C6 C7 . 1.349(8) no C6 H6A . .93 no C7 H7A . .93 no C8 C9 . 1.388(8) no C8 H8A . .93 no C9 C10 . 1.327(8) no C9 H9A . .93 no C10 H10A . .93 no C11 C12 . 1.367(8) no C11 H11A . .93 no C12 C13 . 1.389(9) no C12 H12A . .93 no C13 H13A . .93 no _cod_database_code 2012241