#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006591.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_2006591 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1484 _journal_page_last 1486 _publ_section_title ; 1:1 Molecular Complex Between Water and a Macrocyclic Crown-Phosphonamide ; loop_ _publ_author_name 'Declercq, Jean-Paul' 'Delangle, Pascale' 'Dutasta, Jean-Pierre' 'Van Oostenryck, Luc' 'Tinant, Bernard' _chemical_formula_moiety 'C21 H29 N2 O4 P S, H2 O' _chemical_formula_sum 'C21 H31 N2 O5 P S' _chemical_formula_weight 454.52 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.766(2) _cell_length_b 10.825(2) _cell_length_c 11.857(3) _cell_angle_alpha 71.88(2) _cell_angle_beta 63.47(2) _cell_angle_gamma 73.18(2) _cell_volume 1156.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.305 _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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 .5679(2) .7969(2) .2324(2) .0378(5) Uani d . 1 . C N2 .5262(2) .7133(2) .1906(2) .0379(4) Uani d . 1 . N H2 .530(3) .741(3) .123(3) .071(2) Uiso d . 1 . H P3 .47227(5) .57095(5) .26988(5) .03058(14) Uani d . 1 . P N4 .6051(2) .4550(2) .2895(2) .0421(4) Uani d . 1 . N H4 .599(3) .429(3) .364(3) .071(2) Uiso d . 1 . H C5 .7359(2) .4050(2) .1994(2) .0347(4) Uani d . 1 . C C6 .8219(3) .3003(2) .2479(2) .0422(5) Uani d . 1 . C H6 .795(3) .267(3) .335(3) .071(2) Uiso d . 1 . H C7 .9509(3) .2470(2) .1642(3) .0500(6) Uani d . 1 . C H7 1.006(3) .180(3) .195(3) .071(2) Uiso d . 1 . H C8 .9944(2) .2944(2) .0331(3) .0462(5) Uani d . 1 . C H8 1.082(3) .257(3) -.025(3) .071(2) Uiso d . 1 . H C9 .9096(2) .3988(2) -.0177(2) .0361(4) Uani d . 1 . C C10 .9631(3) .4450(2) -.1612(2) .0460(5) Uani d . 1 . C H10A 1.054(3) .466(3) -.192(3) .071(2) Uiso d . 1 . H H10B .980(3) .371(3) -.205(3) .071(2) Uiso d . 1 . H O11 .87528(15) .55694(15) -.20383(13) .0415(4) Uani d . 1 . O C12 .9282(3) .5893(3) -.3415(2) .0519(6) Uani d . 1 . C H12A .928(3) .510(3) -.373(3) .071(2) Uiso d . 1 . H H12B 1.026(3) .602(3) -.373(3) .071(2) Uiso d . 1 . H C13 .8424(3) .7129(3) -.3882(3) .0540(6) Uani d . 1 . C H13A .870(3) .720(3) -.476(3) .071(2) Uiso d . 1 . H H13B .744(3) .707(3) -.341(3) .071(2) Uiso d . 1 . H O14 .8715(2) .8239(2) -.3707(2) .0503(4) Uani d . 1 . O C15 .7782(3) .9424(3) -.3946(3) .0620(7) Uani d . 1 . C H15A .676(3) .928(3) -.338(3) .071(2) Uiso d . 1 . H H15B .783(3) .969(3) -.490(3) .071(2) Uiso d . 1 . H C16 .8153(4) 1.0523(3) -.3729(3) .0678(8) Uani d . 1 . C H16A .911(3) 1.064(3) -.414(3) .071(2) Uiso d . 1 . H H16B .767(3) 1.135(3) -.399(3) .071(2) Uiso d . 1 . H O17 .7942(2) 1.0310(2) -.2416(2) .0556(4) Uani d . 1 . O C18 .8594(3) 1.1151(3) -.2234(3) .0624(7) Uani d . 1 . C H18A .831(3) 1.208(3) -.260(3) .071(2) Uiso d . 1 . H H18B .962(3) 1.091(3) -.268(3) .071(2) Uiso d . 1 . H C19 .8244(3) 1.0981(3) -.0836(3) .0585(7) Uani d . 1 . C H19A .843(3) 1.003(3) -.035(3) .071(2) Uiso d . 1 . H H19B .887(3) 1.137(3) -.067(3) .071(2) Uiso d . 1 . H O20 .6821(2) 1.15633(15) -.0229(2) .0499(4) Uani d . 1 . O C21 .6413(4) 1.1481(2) .1105(3) .0581(7) Uani d . 1 . C H21A .550(3) 1.206(3) .135(3) .071(2) Uiso d . 1 . H H21B .714(3) 1.177(3) .117(3) .071(2) Uiso d . 1 . H C22 .6263(3) 1.0103(2) .1925(2) .0476(6) Uani d . 1 . C C23 .6502(4) .9709(3) .3043(3) .0757(10) Uani d . 1 . C H23 .675(3) 1.021(3) .328(3) .071(2) Uiso d . 1 . H C24 .6309(5) .8470(3) .3802(3) .0866(12) Uani d . 1 . C H24 .649(3) .814(3) .452(3) .071(2) Uiso d . 1 . H C25 .5932(3) .7589(3) .3446(3) .0608(8) Uani d . 1 . C H25 .583(3) .677(3) .392(3) .071(2) Uiso d . 1 . H C26 .5840(2) .9236(2) .1574(2) .0380(5) Uani d . 1 . C H26 .564(3) .948(3) .080(3) .071(2) Uiso d . 1 . H C27 .7811(2) .4553(2) .0662(2) .0359(4) Uani d . 1 . C H27 .731(3) .527(3) .030(3) .071(2) Uiso d . 1 . H C28 .4283(3) .5351(2) .1559(2) .0413(5) Uani d . 1 . C H28A .398(3) .462(3) .186(3) .071(2) Uiso d . 1 . H H28B .501(3) .531(3) .078(3) .071(2) Uiso d . 1 . H H28C .357(3) .589(3) .140(3) .071(2) Uiso d . 1 . H S29 .31925(6) .56977(6) .43978(5) .0445(2) Uani d . 1 . S OW1 .6764(2) .7828(2) -.0902(2) .0707(6) Uani d . 1 . O HW1 .774(3) .721(3) -.135(3) .071(2) Uiso d . 1 . H HW2 .701(3) .872(3) -.147(3) .071(2) Uiso d . 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 C1 .0466(12) .0332(10) .0357(10) -.0109(9) -.0191(9) -.0022(8) N2 .0580(11) .0286(8) .0292(8) -.0131(8) -.0202(8) .0010(7) P3 .0376(3) .0259(2) .0262(2) -.0058(2) -.0122(2) -.0030(2) N4 .0479(11) .0395(10) .0308(9) .0036(8) -.0180(8) -.0032(7) C5 .0375(10) .0295(9) .0402(11) -.0040(8) -.0184(9) -.0086(8) C6 .0506(13) .0336(10) .0482(12) -.0016(9) -.0283(11) -.0079(9) C7 .0511(14) .0387(12) .067(2) .0051(10) -.0363(13) -.0122(11) C8 .0378(12) .0397(12) .0621(15) .0025(9) -.0209(11) -.0188(11) C9 .0344(10) .0329(10) .0455(11) -.0074(8) -.0159(9) -.0126(9) C10 .0384(12) .0415(12) .0487(13) -.0051(10) -.0086(10) -.0121(10) O11 .0379(8) .0466(8) .0347(8) -.0050(6) -.0095(6) -.0114(6) C12 .059(2) .0518(14) .0375(12) -.0140(12) -.0065(11) -.0152(10) C13 .064(2) .063(2) .0397(13) -.0205(13) -.0209(12) -.0077(11) O14 .0477(9) .0477(9) .0508(9) -.0061(7) -.0188(8) -.0073(7) C15 .060(2) .065(2) .0453(14) .0072(13) -.0201(13) -.0099(12) C16 .079(2) .0466(14) .0484(15) .0023(14) -.0132(14) -.0024(12) O17 .0606(11) .0458(9) .0469(9) -.0112(8) -.0109(8) -.0058(7) C18 .058(2) .0436(14) .068(2) -.0132(12) -.0135(14) -.0014(13) C19 .060(2) .0446(14) .073(2) -.0138(12) -.0317(14) -.0018(13) O20 .0628(11) .0327(8) .0530(10) -.0089(7) -.0261(8) -.0015(7) C21 .088(2) .0361(12) .062(2) -.0171(13) -.039(2) -.0066(11) C22 .065(2) .0373(11) .0518(13) -.0154(11) -.0311(12) -.0061(10) C23 .130(3) .062(2) .075(2) -.045(2) -.069(2) .0035(14) C24 .154(4) .077(2) .078(2) -.056(2) -.089(2) .019(2) C25 .099(2) .0470(14) .058(2) -.0306(14) -.054(2) .0123(12) C26 .0502(13) .0312(10) .0358(11) -.0072(9) -.0221(10) -.0034(8) C27 .0345(10) .0314(10) .0414(11) -.0025(8) -.0168(9) -.0074(8) C28 .0490(13) .0420(12) .0397(12) -.0124(10) -.0202(10) -.0093(10) S29 .0446(3) .0470(3) .0294(3) -.0055(2) -.0081(2) -.0039(2) OW1 .0705(13) .0677(13) .0454(10) -.0059(11) -.0068(9) -.0048(9) 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 C1 C25 . 1.390(3) no C1 C26 . 1.393(3) no C1 N2 . 1.407(3) yes N2 P3 . 1.651(2) yes N2 H2 . .75(3) ? P3 N4 . 1.659(2) yes P3 C28 . 1.790(2) yes P3 S29 . 1.9503(9) yes N4 C5 . 1.411(3) yes N4 H4 . .82(3) ? C5 C6 . 1.391(3) no C5 C27 . 1.400(3) no C6 C7 . 1.382(3) no C6 H6 . .91(3) ? C7 C8 . 1.375(4) no C7 H7 . .89(3) ? C8 C9 . 1.394(3) no C8 H8 . .95(3) ? C9 C27 . 1.391(3) no C9 C10 . 1.496(3) no C10 O11 . 1.415(3) no C10 H10A . .95(3) ? C10 H10B . 1.01(3) ? O11 C12 . 1.428(3) no C12 C13 . 1.494(4) no C12 H12A . 1.04(3) ? C12 H12B . .98(3) ? C13 O14 . 1.420(3) no C13 H13A . .93(3) ? C13 H13B . .96(3) ? O14 C15 . 1.420(3) no C15 C16 . 1.483(5) no C15 H15A . 1.03(3) ? C15 H15B . 1.06(3) ? C16 O17 . 1.422(3) no C16 H16A . .95(3) ? C16 H16B . .93(3) ? O17 C18 . 1.413(4) no C18 C19 . 1.488(4) no C18 H18A . .98(3) ? C18 H18B . .98(3) ? C19 O20 . 1.414(3) no C19 H19A . 1.02(3) ? C19 H19B . 1.00(3) ? O20 C21 . 1.420(3) no C21 C22 . 1.514(3) no C21 H21A . .97(3) ? C21 H21B . .96(3) ? C22 C23 . 1.376(4) no C22 C26 . 1.386(3) no C23 C24 . 1.376(4) no C23 H23 . .83(3) ? C24 C25 . 1.372(4) no C24 H24 . .90(3) ? C25 H25 . .90(3) ? C26 H26 . .98(3) ? C27 H27 . .92(3) ? C28 H28A . .85(3) ? C28 H28B . .91(3) ? C28 H28C . .87(3) ? OW1 HW1 . 1.07(3) ? OW1 HW2 . 1.02(3) ? _cod_database_code 2006591