#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2014692.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_2014692 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2005 _journal_volume 61 _journal_page_first o188 _journal_page_last o192 _publ_section_title ; A new phase of 7,16-dibenzyl-1,4,10,13-tetraoxo-7,16-diazacyclooctadecane, and 7,16-dibenzyl-1,4,10,13-tetraoxo-7,16-diazoniacyclooctadecane bis(tetrafluoroborate) monohydrate, both determined at 123 K ; loop_ _publ_author_name 'Basok, Stepan S.' 'Croitoru Lilia' 'Fonari, Marina S.' 'Ganin, Eduard V.' 'Gelmboldt, Vladimir O.' 'Lipkowski, Janusz' 'Simonov, Yurii A.' _chemical_name_common ; N,N'-dibenzyl-1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane bis tetrafluoroborate monohydrate ; _chemical_formula_moiety 'C26 H40 N2 O4, 2B F4, H2 O' _chemical_formula_sum 'C26 H40 B2 F8 N2 O4.2' _[local]_cod_chemical_formula_sum_orig 'C26 H40 B2 F8 N2 O4.20' _chemical_formula_iupac 'C26 H40 N2 O4 2+, 2B F4 -, H2 O' _chemical_formula_weight 621.48 _chemical_melting_point 168--170 _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9290(6) _cell_length_b 9.3870(6) _cell_length_c 11.6070(7) _cell_angle_alpha 69.342(4) _cell_angle_beta 72.226(4) _cell_angle_gamma 81.480(4) _cell_volume 768.98(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _exptl_crystal_density_diffrn 1.342 _diffrn_ambient_temperature 123(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 N1 0.63995(18) 0.00507(14) -0.26512(13) 0.0255(3) Uani d . 1 . . N H1N 0.599(2) -0.008(2) -0.1798(19) 0.038 Uiso d . 1 . . H C2 0.3942(2) 0.13891(18) 0.28211(16) 0.0309(4) Uani d . 1 . . C H2A 0.3304 0.1384 0.3701 0.037 Uiso calc R 1 . . H H2B 0.5226 0.1431 0.2705 0.037 Uiso calc R 1 . . H C3 0.3336(2) 0.27758(18) 0.18699(15) 0.0296(4) Uani d . 1 . . C H3A 0.2026 0.2854 0.2075 0.036 Uiso calc R 1 . . H H3B 0.3753 0.3713 0.1882 0.036 Uiso calc R 1 . . H O4 0.40852(15) 0.25841(12) 0.06524(10) 0.0308(3) Uani d . 1 . . O C5 0.3292(2) 0.36037(18) -0.03014(15) 0.0311(4) Uani d . 1 . . C H5A 0.3513 0.4670 -0.0438 0.037 Uiso calc R 1 . . H H5B 0.1994 0.3487 -0.0019 0.037 Uiso calc R 1 . . H C6 0.4078(2) 0.32474(18) -0.15215(16) 0.0326(4) Uani d . 1 . . C H6A 0.3621 0.4001 -0.2215 0.039 Uiso calc R 1 . . H H6B 0.5384 0.3296 -0.1774 0.039 Uiso calc R 1 . . H O7 0.36008(15) 0.17417(12) -0.13226(10) 0.0317(3) Uani d . 1 . . O C8 0.3523(2) 0.1520(2) -0.24600(16) 0.0348(4) Uani d . 1 . . C H8A 0.2846 0.2389 -0.2924 0.042 Uiso calc R 1 . . H H8B 0.2891 0.0581 -0.2227 0.042 Uiso calc R 1 . . H C9 0.5357(2) 0.13856(18) -0.33235(15) 0.0307(4) Uani d . 1 . . C H9A 0.5264 0.1253 -0.4111 0.037 Uiso calc R 1 . . H H9B 0.5981 0.2333 -0.3575 0.037 Uiso calc R 1 . . H C10 0.8355(2) 0.03204(17) -0.30300(15) 0.0270(4) Uani d . 1 . . C H10A 0.9002 -0.0650 -0.2690 0.032 Uiso calc R 1 . . H H10B 0.8808 0.0672 -0.3975 0.032 Uiso calc R 1 . . H C11 0.8701(2) 0.14913(17) -0.25252(14) 0.0247(4) Uani d . 1 . . C C12 0.9169(2) 0.29523(18) -0.33387(15) 0.0312(4) Uani d . 1 . . C H12A 0.9283 0.3218 -0.4227 0.037 Uiso calc R 1 . . H C13 0.9470(2) 0.40214(18) -0.28615(17) 0.0347(4) Uani d . 1 . . C H13A 0.9785 0.5019 -0.3421 0.042 Uiso calc R 1 . . H C14 0.9311(2) 0.36360(19) -0.15688(17) 0.0338(4) Uani d . 1 . . C H14A 0.9528 0.4367 -0.1242 0.041 Uiso calc R 1 . . H C15 0.8839(2) 0.2191(2) -0.07526(16) 0.0338(4) Uani d . 1 . . C H15A 0.8720 0.1931 0.0136 0.041 Uiso calc R 1 . . H C16 0.8539(2) 0.11163(18) -0.12296(15) 0.0291(4) Uani d . 1 . . C H16A 0.8221 0.0120 -0.0667 0.035 Uiso calc R 1 . . H B1 0.7890(3) 0.2304(2) 0.33341(18) 0.0291(4) Uani d . 1 . . B F1 0.86572(15) 0.26613(14) 0.20294(9) 0.0513(3) Uani d . 1 . . F F2 0.63511(14) 0.31951(11) 0.35620(10) 0.0448(3) Uani d . 1 . . F F3 0.74774(14) 0.07671(10) 0.38617(10) 0.0418(3) Uani d . 1 . . F F4 0.90924(14) 0.25270(11) 0.39029(9) 0.0382(3) Uani d . 1 . . F O1W 0.372(2) 0.4751(17) 0.5008(14) 0.064(7) Uiso d P 0.102(6) A -1 O 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 N1 0.0273(8) 0.0249(7) 0.0253(7) -0.0001(6) -0.0062(6) -0.0107(6) C2 0.0332(10) 0.0306(9) 0.0347(9) -0.0047(7) -0.0096(7) -0.0161(7) C3 0.0328(10) 0.0272(8) 0.0313(9) -0.0038(7) -0.0054(7) -0.0142(7) O4 0.0301(7) 0.0311(6) 0.0287(6) 0.0047(5) -0.0054(5) -0.0114(5) C5 0.0330(10) 0.0248(8) 0.0313(9) 0.0017(7) -0.0057(7) -0.0082(7) C6 0.0358(10) 0.0240(8) 0.0316(9) -0.0006(7) -0.0040(7) -0.0063(7) O7 0.0359(7) 0.0277(6) 0.0300(6) -0.0026(5) -0.0037(5) -0.0116(5) C8 0.0328(11) 0.0394(10) 0.0359(9) 0.0048(8) -0.0111(8) -0.0177(8) C9 0.0336(10) 0.0304(9) 0.0277(9) 0.0049(7) -0.0101(7) -0.0103(7) C10 0.0244(9) 0.0257(8) 0.0302(8) -0.0008(7) -0.0028(7) -0.0123(7) C11 0.0206(9) 0.0246(8) 0.0288(8) 0.0008(6) -0.0034(6) -0.0122(7) C12 0.0343(10) 0.0285(9) 0.0288(9) -0.0021(7) -0.0046(7) -0.0102(7) C13 0.0377(11) 0.0226(8) 0.0434(10) -0.0019(7) -0.0098(8) -0.0109(7) C14 0.0304(10) 0.0331(9) 0.0473(11) 0.0046(7) -0.0130(8) -0.0247(8) C15 0.0328(10) 0.0420(10) 0.0307(9) 0.0034(8) -0.0102(7) -0.0173(8) C16 0.0270(10) 0.0270(8) 0.0310(9) -0.0013(7) -0.0057(7) -0.0084(7) B1 0.0309(11) 0.0293(10) 0.0298(10) -0.0024(8) -0.0052(8) -0.0154(8) F1 0.0532(8) 0.0721(8) 0.0283(6) 0.0016(6) -0.0084(5) -0.0203(5) F2 0.0420(7) 0.0322(6) 0.0514(6) 0.0076(5) -0.0057(5) -0.0130(5) F3 0.0384(7) 0.0283(5) 0.0654(7) -0.0016(4) -0.0191(5) -0.0190(5) F4 0.0471(7) 0.0388(6) 0.0351(5) -0.0129(5) -0.0120(5) -0.0147(4) 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 N1 C9 . 1.503(2) no N1 C2 2_655 1.506(2) no N1 C10 . 1.511(2) no N1 H1N . 0.911(19) no C2 C3 . 1.506(2) no C2 N1 2_655 1.506(2) no C2 H2A . 0.9900 no C2 H2B . 0.9900 no C3 O4 . 1.4204(18) no C3 H3A . 0.9900 no C3 H3B . 0.9900 no O4 C5 . 1.427(2) no C5 C6 . 1.497(2) no C5 H5A . 0.9900 no C5 H5B . 0.9900 no C6 O7 . 1.4384(19) no C6 H6A . 0.9900 no C6 H6B . 0.9900 no O7 C8 . 1.428(2) no C8 C9 . 1.510(2) no C8 H8A . 0.9900 no C8 H8B . 0.9900 no C9 H9A . 0.9900 no C9 H9B . 0.9900 no C10 C11 . 1.506(2) no C10 H10A . 0.9900 no C10 H10B . 0.9900 no C11 C16 . 1.387(2) no C11 C12 . 1.390(2) no C12 C13 . 1.384(2) no C12 H12A . 0.9500 no C13 C14 . 1.383(3) no C13 H13A . 0.9500 no C14 C15 . 1.380(2) no C14 H14A . 0.9500 no C15 C16 . 1.388(2) no C15 H15A . 0.9500 no C16 H16A . 0.9500 no B1 F2 . 1.384(2) no B1 F1 . 1.384(2) no B1 F4 . 1.389(2) no B1 F3 . 1.399(2) no