#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006363.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_2006363 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1004 _journal_page_last 1006 _publ_section_title ; K^+^~2~(18-crown-6-K^+^)~2~Sn~2~Se~6~^4-^.4en: An [Sn~2~Se~6~]^4-^ Anion with a Short Sn...Sn Distance ; loop_ _publ_author_name 'Borrmann, Horst' 'Pirani, Ayaaz M.' 'Schrobilgen, Gary J.' _chemical_formula_sum 'C32 H80 K4 N8 O12 Se6 Sn2' _chemical_formula_iupac '[K]2 [K(C12 H24 O6)]2 [Sn2 Se6] , 4C2 H8 N2' _chemical_formula_weight 1636.58 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 15.634(2) _cell_length_b 8.4790(10) _cell_length_c 23.404(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.600(10) _cell_angle_gamma 90.00 _cell_volume 2940.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.848 _diffrn_ambient_temperature 150(2) _refine_ls_R_factor_obs .0298 _refine_ls_wR_factor_obs .0753 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 Sn1 .606520(10) .58420(2) .013180(10) .01411(5) Uani d . 1 . Sn Se1 .65022(2) .83161(3) .070530(10) .01900(6) Uani d . 1 . Se Se2 .71568(2) .46461(3) -.029960(10) .02071(7) Uani d . 1 . Se Se3 .54618(2) .37177(3) .070340(10) .01831(6) Uani d . 1 . Se K1 .13731(4) .39529(7) .87592(3) .02054(11) Uani d . 1 . K O100 .19839(13) .3607(2) .76530(9) .0219(4) Uani d . 1 . O C101 .2047(2) .1959(3) .75598(12) .0229(5) Uani d . 1 . C C102 .1113(2) .1279(3) .73961(12) .0229(5) Uani d . 1 . C O103 .08111(13) .1379(2) .79075(8) .0210(4) Uani d . 1 . O C104 -.0055(2) .0658(3) .77889(13) .0233(5) Uani d . 1 . C C105 -.0338(2) .0814(3) .83407(13) .0237(5) Uani d . 1 . C O106 -.04926(14) .2439(2) .84316(8) .0222(4) Uani d . 1 . O C107 -.0774(2) .2616(4) .89500(12) .0246(5) Uani d . 1 . C C108 -.0908(2) .4340(4) .90463(13) .0229(5) Uani d . 1 . C O109 -.00634(12) .5127(2) .91642(8) .0208(4) Uani d . 1 . O C110 -.0155(2) .6757(3) .92783(12) .0208(5) Uani d . 1 . C C111 .0738(2) .7552(3) .93891(11) .0201(5) Uani d . 1 . C O112 .10014(12) .7433(2) .88589(8) .0202(4) Uani d . 1 . O C113 .1852(2) .8219(3) .89532(12) .0220(5) Uani d . 1 . C C114 .2148(2) .7981(3) .84116(13) .0225(5) Uani d . 1 . C O115 .23026(13) .6344(2) .83415(8) .0197(4) Uani d . 1 . O C116 .2695(2) .6097(3) .78805(12) .0212(5) Uani d . 1 . C C117 .2843(2) .4366(4) .78273(12) .0228(5) Uani d . 1 . C H10A .231(2) .182(4) .7254(16) .026(9) Uiso d . 1 . H H10B .244(2) .141(4) .7906(16) .025(9) Uiso d . 1 . H H10C .070(3) .183(5) .7042(17) .033(10) Uiso d . 1 . H H10D .107(2) .023(4) .7270(16) .025(9) Uiso d . 1 . H H10E -.004(2) -.051(4) .7670(15) .017(8) Uiso d . 1 . H H10F -.046(3) .106(5) .7455(19) .040(11) Uiso d . 1 . H H10G .015(2) .052(4) .8693(16) .024(8) Uiso d . 1 . H H10H -.089(2) .010(4) .8292(16) .028(9) Uiso d . 1 . H H10I -.134(2) .210(4) .8875(15) .019(8) Uiso d . 1 . H H10J -.031(2) .210(4) .9296(16) .025(8) Uiso d . 1 . H H10K -.134(2) .474(4) .8694(15) .016(7) Uiso d . 1 . H H10L -.114(3) .439(5) .9407(19) .045(12) Uiso d . 1 . H H11A -.034(2) .683(4) .9643(14) .016(7) Uiso d . 1 . H H11B -.060(2) .726(4) .8924(14) .014(7) Uiso d . 1 . H H11C .120(3) .707(5) .9722(17) .034(10) Uiso d . 1 . H H11D .072(2) .864(4) .9493(14) .015(7) Uiso d . 1 . H H11E .227(3) .774(5) .9321(17) .034(10) Uiso d . 1 . H H11F .179(3) .939(4) .9048(16) .028(9) Uiso d . 1 . H H11G .273(2) .852(4) .8478(14) .017(7) Uiso d . 1 . H H11H .171(2) .838(4) .8053(15) .021(8) Uiso d . 1 . H H11I .327(2) .666(4) .8006(14) .014(7) Uiso d . 1 . H H11J .230(2) .655(4) .7506(15) .019(8) Uiso d . 1 . H H11K .313(2) .417(4) .7525(15) .020(8) Uiso d . 1 . H H11L .324(2) .388(4) .8196(15) .019(8) Uiso d . 1 . H K2 .42176(4) .87940(8) .04533(3) .02983(14) Uani d . 1 . K N200 .4760(2) .7390(4) .1640(2) .0424(7) Uani d . 1 . N C201 .4044(3) .7139(4) .1911(2) .0366(7) Uani d . 1 . C C202 .4134(4) .5663(5) .2296(2) .0521(11) Uani d . 1 . C N203 .4119(3) .4171(4) .1969(2) .0512(9) Uani d . 1 . N H20A .475(3) .645(6) .140(2) .056(14) Uiso d . 1 . H H20B .535(4) .750(7) .198(3) .084(18) Uiso d . 1 . H H20C .404(3) .812(5) .2158(17) .030(9) Uiso d . 1 . H H20D .344(3) .716(6) .162(2) .052(13) Uiso d . 1 . H H20E .365(3) .569(5) .243(2) .044(12) Uiso d . 1 . H H20F .469(3) .571(6) .269(2) .058(14) Uiso d . 1 . H H20G .466(4) .403(7) .186(3) .08(2) Uiso d . 1 . H H20H .368(4) .434(7) .162(3) .083(19) Uiso d . 1 . H N300 .3386(2) .1102(3) .10056(12) .0266(5) Uani d . 1 . N C301 .2480(2) .1039(4) .10580(13) .0257(6) Uani d . 1 . C C302 .1790(2) .0548(3) .04667(13) .0230(5) Uani d . 1 . C N303 .1697(2) .1618(3) -.00462(11) .0232(5) Uani d . 1 . N H30G .215(3) .147(5) -.0213(17) .030(9) Uiso d . 1 . H H30H .174(3) .253(5) .0077(17) .032(10) Uiso d . 1 . H H30A .345(3) .180(6) .076(2) .061(15) Uiso d . 1 . H H30B .373(4) .131(6) .129(3) .066(17) Uiso d . 1 . H H30C .235(2) .203(4) .1204(14) .016(7) Uiso d . 1 . H H30D .247(2) .025(4) .1385(16) .025(9) Uiso d . 1 . H H30E .120(3) .042(4) .0502(16) .027(9) Uiso d . 1 . H H30F .197(3) -.047(5) .0356(16) .028(9) 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 Sn1 .00997(8) .01565(9) .01552(8) -.00135(5) .00238(6) .00096(6) Se1 .01876(12) .01777(12) .01963(12) -.00353(9) .00494(9) -.00238(9) Se2 .01728(12) .02091(14) .02592(13) .00251(9) .00968(10) .00097(10) Se3 .01286(11) .02172(13) .01715(11) -.00184(9) .00029(9) .00625(9) K1 .0191(2) .0212(3) .0211(2) -.0013(2) .0062(2) -.0008(2) O100 .0191(9) .0189(9) .0264(9) .0022(7) .0054(7) .0012(7) C101 .0285(13) .0226(13) .0188(11) .0067(11) .0093(10) .0003(10) C102 .0344(14) .0184(12) .0137(11) .0008(11) .0047(10) -.0010(9) O103 .0230(9) .0219(9) .0153(8) -.0034(8) .0024(7) -.0033(7) C104 .0210(12) .0193(12) .0236(13) -.0023(10) -.0013(10) -.0041(10) C105 .0229(13) .0176(12) .0267(13) -.0019(10) .0022(11) .0017(10) O106 .0288(10) .0187(9) .0202(9) -.0023(8) .0093(8) .0022(7) C107 .0277(13) .0272(14) .0208(12) -.0084(11) .0101(11) .0048(11) C108 .0192(11) .0287(14) .0226(12) -.0014(10) .0094(10) .0026(11) O109 .0187(8) .0196(9) .0257(9) -.0010(7) .0093(7) -.0039(7) C110 .0211(12) .0235(13) .0174(11) .0055(10) .0053(9) -.0013(10) C111 .0242(12) .0182(12) .0160(11) .0026(10) .0035(9) -.0009(9) O112 .0203(9) .0205(9) .0185(8) -.0035(7) .0043(7) -.0029(7) C113 .0214(12) .0168(12) .0236(12) -.0042(9) .0013(10) -.0015(10) C114 .0236(12) .0152(11) .0281(13) -.0027(10) .0072(11) .0041(10) O115 .0223(9) .0175(9) .0212(9) -.0018(7) .0094(7) .0025(7) C116 .0205(12) .0263(13) .0171(11) -.0043(10) .0063(10) .0033(10) C117 .0178(11) .0304(14) .0203(12) .0011(10) .0063(10) .0028(11) K2 .0265(3) .0305(3) .0359(3) .0026(2) .0148(3) -.0003(3) N200 .044(2) .043(2) .046(2) .0022(14) .0216(15) -.0007(14) C201 .045(2) .033(2) .036(2) .0015(15) .0187(15) -.0060(14) C202 .088(3) .037(2) .037(2) -.011(2) .028(2) -.004(2) N203 .069(3) .038(2) .043(2) -.002(2) .012(2) -.0005(15) N300 .0249(12) .0301(13) .0217(11) .0003(10) .0031(10) .0002(10) C301 .0305(14) .0284(14) .0204(12) -.0044(11) .0113(11) -.0039(11) C302 .0247(13) .0204(12) .0249(13) -.0054(10) .0095(11) -.0004(10) N303 .0211(11) .0263(13) .0234(11) -.0025(9) .0086(9) -.0003(10) 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 Sn1 Sn1 3_665 3.4930(9) yes Sn1 Se1 . 2.4665(4) yes Sn1 Se2 . 2.4616(4) yes Sn1 Se3 . 2.5941(4) yes Sn1 Se3 3_665 2.5852(5) yes Sn1 K1 3_666 4.0218(8) yes Sn1 K2 . 4.0695(8) yes Sn1 K2 3_665 4.1397(8) yes Se1 K1 3_666 3.6946(7) yes Se1 K2 . 3.4534(8) yes Se1 K2 3_675 3.5604(8) yes Se2 K1 3_666 3.7952(8) yes Se2 K2 3_665 3.5723(8) yes Se3 K2 3_665 3.6030(8) yes K1 O100 . 3.046(2) yes K1 O103 . 2.897(2) yes K1 O106 . 3.052(2) yes K1 O109 . 2.879(2) yes K1 O112 . 3.030(2) yes K1 O115 . 2.843(2) yes K1 N303 1_556 3.330(3) yes K1 Se1 3_666 3.6946(7) no K1 Se2 3_666 3.7953(8) no K1 Sn1 3_666 4.0218(8) no O100 C101 . 1.423(3) no O100 C117 . 1.427(3) no C101 C102 . 1.501(4) no C102 O103 . 1.422(3) no O103 C104 . 1.429(3) no C104 C105 . 1.499(4) no C105 O106 . 1.426(3) no O106 C107 . 1.425(3) no C107 C108 . 1.504(4) no C108 O109 . 1.426(3) no O109 C110 . 1.423(3) no C110 C111 . 1.497(4) no C111 O112 . 1.430(3) no O112 C113 . 1.440(3) no C113 C114 . 1.495(4) no C114 O115 . 1.427(3) no O115 C116 . 1.417(3) no C116 C117 . 1.497(4) no K2 N200 . 2.890(4) yes K2 N300 1_565 2.874(3) yes K2 Se1 3_675 3.5603(8) no K2 Se2 3_665 3.5723(8) no K2 Se3 3_665 3.6030(8) no K2 Sn1 3_665 4.1396(8) no K2 K2 3_675 4.2403(14) yes N200 C201 . 1.467(5) no C201 C202 . 1.522(6) no C202 N203 . 1.475(5) no N300 C301 . 1.462(4) no N300 K2 1_545 2.874(3) no C301 C302 . 1.516(4) no C302 N303 . 1.474(4) no N303 K1 1_554 3.330(3) no