#------------------------------------------------------------------------------ #$Date: 2009-05-14 15:03:35 +0100 (Thu, 14 May 2009) $ #$Revision: 725 $ #$URL: svn://www.crystallography.net/cod/cif/7/7051240.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_7051240 _journal_name_full 'New Journal of Chemistry' _journal_year 2000 loop_ _publ_author_name 'Ch. Schmidt' 'E. F. Paulus' 'V. Boehmer' 'W. Vogt' _chemical_formula_sum 'C85.50 H126.50 Cl N4.50 O12' _chemical_formula_weight 1444.86 _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 22.03610(10) _cell_length_b 22.03610(10) _cell_length_c 17.0005(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8255.27(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.163 _diffrn_ambient_temperature 293(2) loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 0.35033(9) 0.18914(9) 0.43742(11) 0.0515(5) Uani 1 1 d . . . C02 C 0.39554(9) 0.22636(9) 0.46711(12) 0.0522(5) Uani 1 1 d . . . C03 C 0.42914(9) 0.20444(10) 0.53107(13) 0.0573(6) Uani 1 1 d . . . C04 C 0.41988(10) 0.14628(10) 0.56233(12) 0.0581(6) Uani 1 1 d . . . C05 C 0.37364(9) 0.11081(9) 0.52938(12) 0.0567(5) Uani 1 1 d . . . C06 C 0.33824(9) 0.13113(9) 0.46596(11) 0.0519(5) Uani 1 1 d . . . C07 C 0.40852(9) 0.28849(9) 0.43057(13) 0.0561(6) Uani 1 1 d . . . C08 C 0.40527(11) 0.28740(11) 0.33947(13) 0.0661(6) Uani 1 1 d . . . C09 C 0.44628(13) 0.24060(13) 0.29941(15) 0.0835(8) Uani 1 1 d . . . C10 C 0.51291(15) 0.24843(18) 0.3137(2) 0.1126(11) Uani 1 1 d . . . C11 C 0.54949(18) 0.2004(3) 0.2677(4) 0.213(3) Uani 1 1 d . . . H11A H 0.5450 0.1625 0.2960 0.320 Uiso 1 1 calc R . . H11B H 0.5292 0.1951 0.2176 0.320 Uiso 1 1 calc R . . C12 C 0.5988(5) 0.2055(4) 0.2546(6) 0.470(5) Uani 1 1 d . . . H12A H 0.6082 0.2477 0.2479 0.705 Uiso 1 1 calc R . . H12B H 0.6084 0.1838 0.2072 0.705 Uiso 1 1 calc R . . H12C H 0.6221 0.1894 0.2975 0.705 Uiso 1 1 calc R . . C13 C 0.45561(11) 0.12561(11) 0.63410(14) 0.0709(7) Uani 1 1 d . . . C14 C 0.49234(12) 0.02169(12) 0.63599(17) 0.0852(8) Uani 1 1 d . . . C15 C 0.54247(14) -0.02517(14) 0.6373(2) 0.1159(12) Uani 1 1 d . . . H15A H 0.5266 -0.0631 0.6558 0.174 Uiso 1 1 calc R . . H15B H 0.5743 -0.0118 0.6717 0.174 Uiso 1 1 calc R . . H15C H 0.5584 -0.0303 0.5851 0.174 Uiso 1 1 calc R . . C16 C 0.56522(12) 0.09996(14) 0.59325(19) 0.0902(9) Uani 1 1 d . . . C17 C 0.56854(17) 0.1052(2) 0.5073(2) 0.1368(15) Uani 1 1 d . . . H17A H 0.5395 0.1354 0.4899 0.205 Uiso 1 1 calc R . . H17B H 0.5571 0.0666 0.4841 0.205 Uiso 1 1 calc R . . C18 C 0.6317(2) 0.1228(3) 0.4779(3) 0.211(2) Uani 1 1 d . . . H18A H 0.6588 0.0884 0.4833 0.317 Uiso 1 1 calc R . . H18B H 0.6294 0.1331 0.4225 0.317 Uiso 1 1 calc R . . C19 C 0.6552(3) 0.1717(3) 0.5191(6) 0.288(5) Uani 1 1 d . . . H19A H 0.6327 0.2076 0.5034 0.432 Uiso 1 1 calc R . . H19B H 0.6968 0.1774 0.5020 0.432 Uiso 1 1 calc R . . C20 C 0.65505(19) 0.1691(3) 0.6057(4) 0.209(3) Uani 1 1 d . . . H20A H 0.6666 0.2083 0.6267 0.314 Uiso 1 1 calc R . . H20B H 0.6846 0.1395 0.6233 0.314 Uiso 1 1 calc R . . C21 C 0.59182(17) 0.1517(2) 0.6369(3) 0.1593(18) Uani 1 1 d . . . H21A H 0.5950 0.1411 0.6921 0.239 Uiso 1 1 calc R . . H21B H 0.5650 0.1864 0.6326 0.239 Uiso 1 1 calc R . . H01 H 0.3232(9) 0.2036(9) 0.3946(12) 0.061(6) Uiso 1 1 d . . . H07 H 0.4515(9) 0.2978(8) 0.4459(10) 0.052(5) Uiso 1 1 d . . . H081 H 0.4126(10) 0.3273(11) 0.3184(13) 0.075(7) Uiso 1 1 d . . . H082 H 0.3612(10) 0.2810(10) 0.3237(12) 0.065(6) Uiso 1 1 d . . . H091 H 0.4429(12) 0.2374(13) 0.2360(18) 0.112(9) Uiso 1 1 d . . . H092 H 0.4399(13) 0.1949(13) 0.3177(16) 0.105(9) Uiso 1 1 d . . . H101 H 0.5305(19) 0.3013(19) 0.303(3) 0.180(16) Uiso 1 1 d . . . H102 H 0.5157(16) 0.2344(16) 0.364(2) 0.134(12) Uiso 1 1 d . . . H131 H 0.4742(11) 0.1630(12) 0.6593(14) 0.088(8) Uiso 1 1 d . . . H132 H 0.4260(12) 0.1040(12) 0.6751(16) 0.095(8) Uiso 1 1 d . . . H16 H 0.6035(18) 0.0796(18) 0.631(2) 0.169(15) Uiso 1 1 d . . . H1 H 0.4612(13) 0.2827(13) 0.5628(16) 0.106(9) Uiso 1 1 d . . . H2 H 0.3908(14) 0.0413(13) 0.6005(18) 0.119(10) Uiso 1 1 d . . . N1 N 0.50490(9) 0.08072(9) 0.62179(12) 0.0729(6) Uani 1 1 d . . . O1 O 0.47363(7) 0.23909(8) 0.56601(10) 0.0783(5) Uani 1 1 d . . . O2 O 0.35997(7) 0.05395(7) 0.55879(10) 0.0741(5) Uani 1 1 d . . . O3 O 0.44008(9) 0.00480(9) 0.64930(15) 0.1102(7) Uani 1 1 d . . . C1 C 0.2500 0.2500 0.1075(4) 0.160(4) Uani 0.526(5) 4 d SP A 1 C2 C 0.2500 0.2500 0.1900(6) 0.084(3) Uani 0.526(5) 4 d SP A 1 N2 N 0.2500 0.2500 0.2546(6) 0.119(4) Uani 0.526(5) 4 d SP A 1 C3 C 0.2500 0.2500 0.1075(4) 0.160(4) Uani 0.474(5) 4 d SP . 2 Cl1 Cl 0.3074(3) 0.2250(5) 0.1666(4) 0.233(4) Uani 0.237(3) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.0489(10) 0.0551(11) 0.0507(10) 0.0030(9) 0.0014(9) 0.0059(9) C02 0.0463(10) 0.0548(11) 0.0554(10) 0.0019(9) 0.0026(9) 0.0035(9) C03 0.0514(11) 0.0595(12) 0.0610(12) -0.0042(10) -0.0033(10) 0.0059(9) C04 0.0568(11) 0.0593(12) 0.0582(11) -0.0003(10) -0.0026(10) 0.0108(10) C05 0.0564(11) 0.0517(11) 0.0619(11) 0.0071(10) 0.0045(10) 0.0073(9) C06 0.0485(10) 0.0517(11) 0.0554(10) 0.0001(9) 0.0041(9) 0.0052(9) C07 0.0456(10) 0.0560(11) 0.0666(12) 0.0023(10) 0.0016(9) -0.0033(9) C08 0.0690(13) 0.0661(13) 0.0630(13) 0.0055(11) 0.0097(11) -0.0051(11) C09 0.0938(17) 0.0815(16) 0.0752(15) -0.0045(14) 0.0240(14) -0.0013(14) C10 0.092(2) 0.125(3) 0.121(2) -0.008(2) 0.0230(19) 0.0140(19) C11 0.101(2) 0.281(6) 0.258(5) -0.068(5) 0.061(3) 0.066(3) C12 0.672(12) 0.351(9) 0.388(10) 0.113(8) 0.325(9) 0.314(9) C13 0.0746(14) 0.0730(14) 0.0650(13) 0.0013(12) -0.0104(12) 0.0186(12) C14 0.0793(16) 0.0767(16) 0.0995(18) 0.0146(14) -0.0170(15) 0.0157(13) C15 0.099(2) 0.0831(18) 0.165(3) 0.012(2) -0.029(2) 0.0296(16) C16 0.0697(15) 0.104(2) 0.0969(19) 0.0073(17) -0.0105(15) 0.0026(15) C17 0.118(3) 0.191(4) 0.102(2) 0.018(3) 0.032(2) 0.021(3) C18 0.145(3) 0.297(6) 0.193(4) 0.096(4) 0.076(3) 0.064(4) C19 0.157(4) 0.150(5) 0.557(13) 0.042(7) 0.139(6) -0.004(4) C20 0.079(2) 0.192(5) 0.356(8) -0.040(6) -0.029(4) -0.018(3) C21 0.099(2) 0.162(3) 0.217(4) -0.061(3) -0.019(3) -0.024(3) N1 0.0664(11) 0.0751(12) 0.0772(12) 0.0075(10) -0.0093(10) 0.0146(10) O1 0.0731(9) 0.0663(10) 0.0953(11) -0.0010(9) -0.0316(9) 0.0005(8) O2 0.0711(10) 0.0634(9) 0.0879(11) 0.0219(8) -0.0087(9) 0.0018(8) O3 0.0838(12) 0.0901(12) 0.1567(18) 0.0492(12) -0.0177(12) 0.0088(10) C1 0.201(5) 0.201(5) 0.078(4) 0.000 0.000 0.000 C2 0.095(4) 0.095(4) 0.061(5) 0.000 0.000 0.000 N2 0.141(5) 0.141(5) 0.077(6) 0.000 0.000 0.000 C3 0.201(5) 0.201(5) 0.078(4) 0.000 0.000 0.000 Cl1 0.185(6) 0.346(10) 0.168(5) -0.021(7) 0.009(5) 0.087(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C01 C02 1.386(3) . ? C01 C06 1.393(3) . ? C01 H01 0.99(2) . ? C02 C03 1.401(3) . ? C02 C07 1.530(3) . ? C03 O1 1.377(3) . ? C03 C04 1.402(3) . ? C04 C05 1.401(3) . ? C04 C13 1.522(3) . ? C05 O2 1.382(3) . ? C05 C06 1.404(3) . ? C06 C07 1.525(3) 4 ? C07 C06 1.525(3) 3 ? C07 C08 1.551(3) . ? C07 H07 1.005(19) . ? C08 C09 1.531(4) . ? C08 H081 0.96(2) . ? C08 H082 1.02(2) . ? C09 C10 1.498(4) . ? C09 H091 1.08(3) . ? C09 H092 1.06(3) . ? C10 C11 1.543(6) . ? C10 H101 1.24(4) . ? C10 H102 0.91(3) . ? C11 C12 1.114(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N1 1.484(3) . ? C13 H131 1.02(3) . ? C13 H132 1.07(3) . ? C14 O3 1.231(3) . ? C14 N1 1.352(3) . ? C14 C15 1.512(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.467(5) . ? C16 N1 1.477(3) . ? C16 C21 1.481(5) . ? C16 H16 1.15(4) . ? C17 C18 1.529(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.384(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.474(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.539(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? O1 H1 1.00(3) . ? O2 H2 1.02(3) . ? C1 C2 1.403(12) . ? C2 N2 1.099(13) . ? Cl1 Cl1 1.952(10) 4 ? Cl1 Cl1 1.952(10) 3 ?