#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006211.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_2006211 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 687 _journal_page_last 691 _publ_section_title ; cis- and trans-Diisothiocyanato(1,4,8,11- tetraazacyclotetradecane)chromium(III) Perchlorate ; loop_ _publ_author_name 'Friesen, Duane A. ' 'Quail, J. Wilson ' 'Waltz, William L. ' 'Nashiem, Rodney E.' _chemical_name_common 'cis-diisothiocyanato(cyclam)chromium(III) perchlorate' _chemical_formula_moiety '[Cr(NCS)2 (C10 H24 N4)].(ClO4)' _chemical_formula_sum 'C12 H24 Cl Cr N6 O4 S2' _chemical_formula_weight 467.928 _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 10.975(2) _cell_length_b 8.690(2) _cell_length_c 21.144(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.607(14) _cell_angle_gamma 90.00 _cell_volume 2016.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _exptl_crystal_density_diffrn 1.541 _diffrn_ambient_temperature 123(2) _refine_ls_R_factor_obs .0450 _refine_ls_wR_factor_obs .1172 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 Cr .79090(5) .84208(7) .14397(3) .0211(2) Uani d . 1 . Cr Cl .57355(9) .31502(11) .10763(5) .0314(3) Uani d . 1 . Cl S1 .80522(9) .45855(12) .30540(5) .0324(3) Uani d . 1 . S S2 1.14716(12) .6151(2) .05818(6) .0513(4) Uani d . 1 . S O1 .6906(3) .3872(4) .1027(2) .0696(13) Uani d . 1 . O O2 .5704(4) .2481(5) .1699(2) .0778(14) Uani d . 1 . O O3 .4784(3) .4250(3) .0989(2) .0427(8) Uani d . 1 . O O4 .5680(3) .1954(4) .0620(2) .0566(10) Uani d . 1 . O N1 .8868(3) .9939(4) .2026(2) .0246(7) Uani d . 1 . N N2 .8061(3) 1.0196(4) .07827(15) .0232(7) Uani d . 1 . N N3 .6751(3) .7262(4) .0823(2) .0304(8) Uani d . 1 . N N4 .6288(3) .9197(4) .1826(2) .0258(7) Uani d . 1 . N N5 .7891(3) .6739(4) .2080(2) .0297(8) Uani d . 1 . N N6 .9427(3) .7538(4) .1090(2) .0312(8) Uani d . 1 . N C1 .8940(3) 1.1471(5) .1709(2) .0277(9) Uani d . 1 . C C2 .9079(3) 1.1206(5) .1007(2) .0275(9) Uani d . 1 . C C3 .8257(4) .9735(6) .0113(2) .0347(10) Uani d . 1 . C C4 .7228(4) .8761(6) -.0153(2) .0375(10) Uani d . 1 . C C5 .7094(4) .7198(5) .0145(2) .0365(10) Uani d . 1 . C C6 .5479(4) .7839(5) .0916(2) .0334(10) Uani d . 1 . C C7 .5312(4) .8128(5) .1605(2) .0318(9) Uani d . 1 . C C8 .6253(4) .9388(5) .2527(2) .0297(9) Uani d . 1 . C C9 .7178(4) 1.0527(5) .2779(2) .0342(10) Uani d . 1 . C C10 .8503(4) 1.0063(5) .2694(2) .0308(9) Uani d . 1 . C C11 .7959(3) .5827(4) .2484(2) .0266(9) Uani d . 1 . C C12 1.0285(4) .6944(5) .0879(2) .0299(9) Uani d . 1 . C H1 .9663(3) .9570(4) .2038(2) .030 Uiso calc R 1 . H H2 .7346(3) 1.0770(4) .07960(15) .028 Uiso calc R 1 . H H3 .6747(3) .6245(4) .0961(2) .037 Uiso calc R 1 . H H4 .6123(3) 1.0154(4) .1648(2) .031 Uiso calc R 1 . H H1A .9646(3) 1.2058(5) .1876(2) .033 Uiso calc R 1 . H H1B .8190(3) 1.2070(5) .1790(2) .033 Uiso calc R 1 . H H2A .9054(3) 1.2202(5) .0780(2) .033 Uiso calc R 1 . H H2B .9872(3) 1.0708(5) .0923(2) .033 Uiso calc R 1 . H H3A .9028(4) .9149(6) .0086(2) .042 Uiso calc R 1 . H H3B .8342(4) 1.0672(6) -.0149(2) .042 Uiso calc R 1 . H H4A .6454(4) .9331(6) -.0102(2) .045 Uiso calc R 1 . H H4B .7358(4) .8623(6) -.0613(2) .045 Uiso calc R 1 . H H5A .6464(4) .6611(5) -.0091(2) .044 Uiso calc R 1 . H H5B .7874(4) .6635(5) .0108(2) .044 Uiso calc R 1 . H H6A .5350(4) .8802(5) .0674(2) .040 Uiso calc R 1 . H H6B .4883(4) .7065(5) .0763(2) .040 Uiso calc R 1 . H H7A .4501(4) .8590(5) .1679(2) .038 Uiso calc R 1 . H H7B .5362(4) .7147(5) .1842(2) .038 Uiso calc R 1 . H H8A .6401(4) .8376(5) .2729(2) .036 Uiso calc R 1 . H H8B .5428(4) .9733(5) .2648(2) .036 Uiso calc R 1 . H H9A .7031(4) 1.0682(5) .3236(2) .041 Uiso calc R 1 . H H9B .7044(4) 1.1527(5) .2565(2) .041 Uiso calc R 1 . H H10A .9030(4) 1.0831(5) .2908(2) .037 Uiso calc R 1 . H H10B .8641(4) .9059(5) .2904(2) .037 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 Cr .0186(3) .0206(3) .0240(3) .0028(2) -.0015(2) -.0010(3) Cl .0394(6) .0211(5) .0337(6) .0055(4) -.0024(4) .0000(4) S1 .0264(5) .0310(6) .0399(6) -.0021(4) -.0041(4) .0072(5) S2 .0475(7) .0662(9) .0402(7) .0315(7) .0062(5) -.0039(6) O1 .042(2) .035(2) .131(4) -.004(2) -.022(2) .006(2) O2 .111(3) .068(3) .054(3) .053(3) .029(2) .028(2) O3 .047(2) .029(2) .052(2) .0157(14) -.009(2) -.0020(15) O4 .051(2) .048(2) .070(3) .021(2) -.028(2) -.030(2) N1 .021(2) .026(2) .026(2) .0022(14) -.0012(13) .0006(14) N2 .0198(15) .027(2) .022(2) .0026(13) .0011(12) -.0017(14) N3 .027(2) .021(2) .042(2) .0040(14) -.0089(15) -.002(2) N4 .019(2) .023(2) .036(2) .0007(13) .0056(13) .0060(15) N5 .034(2) .024(2) .031(2) .0057(15) -.0005(14) .006(2) N6 .025(2) .037(2) .031(2) .011(2) -.0025(14) -.004(2) C1 .024(2) .026(2) .034(2) -.002(2) -.001(2) .001(2) C2 .024(2) .032(2) .026(2) -.004(2) .005(2) .001(2) C3 .032(2) .047(3) .025(2) .004(2) .001(2) .000(2) C4 .035(2) .050(3) .027(2) .002(2) -.006(2) -.006(2) C5 .037(2) .035(2) .037(3) .009(2) -.009(2) -.012(2) C6 .024(2) .024(2) .053(3) .000(2) -.005(2) .003(2) C7 .023(2) .028(2) .044(3) -.002(2) -.001(2) .008(2) C8 .032(2) .032(2) .025(2) .005(2) .009(2) .002(2) C9 .038(2) .038(2) .028(2) .005(2) .010(2) -.001(2) C10 .036(2) .033(2) .024(2) .001(2) -.002(2) -.002(2) C11 .014(2) .023(2) .043(3) -.003(2) -.004(2) -.009(2) C12 .033(2) .034(2) .022(2) .009(2) -.006(2) -.004(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 Cr N1 . 2.088(3) ? Cr N2 . 2.084(3) ? Cr N3 . 2.073(3) ? Cr N4 . 2.078(3) ? Cr N5 . 1.992(3) ? Cr N6 . 1.984(3) ? Cl O1 . 1.434(4) ? Cl O2 . 1.440(4) ? Cl O3 . 1.426(3) ? Cl O4 . 1.419(3) ? S1 C11 . 1.620(4) ? S2 C12 . 1.607(4) ? N1 C1 . 1.494(5) ? N1 C10 . 1.476(5) ? N2 C2 . 1.495(5) ? N2 C3 . 1.490(5) ? N3 C5 . 1.486(6) ? N3 C6 . 1.498(5) ? N4 C7 . 1.489(5) ? N4 C8 . 1.491(5) ? N5 C11 . 1.167(5) ? N6 C12 . 1.167(5) ? C1 C2 . 1.510(6) ? C3 C4 . 1.515(6) ? C4 C5 . 1.506(7) ? C6 C7 . 1.493(6) ? C8 C9 . 1.511(6) ? C9 C10 . 1.521(6) ?