#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012471.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_2012471 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2002 _journal_volume 58 _journal_page_first m70 _journal_page_last m73 _publ_section_title ; Two new [Ni(tren)~2~]^2+^ complexes: [Ni(tren)~2~]Cl~2~ and [Ni(tren)~2~]WS~4~ ; loop_ _publ_author_name 'Ellermeier, Jan' 'St\"ahler, Ralph' 'Bensch, Wolfgang' _chemical_formula_moiety ' C12 H36 N8 Ni 2+ , W S4 2- ' _chemical_formula_sum 'C12 H36 N8 Ni S4 W' _chemical_formula_iupac '[Ni(C6 H18 N4)2] W S4' _chemical_formula_weight 663.29 _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 10.147(2) _cell_length_b 11.852(2) _cell_length_c 19.122(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.44(3) _cell_angle_gamma 90.00 _cell_volume 2227.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.978 _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_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 W .208831(12) .263872(10) .639058(6) .02600(4) Uani d . 1 . . W Ni .69114(3) .25185(3) .381889(18) .02017(7) Uani d . 1 . . Ni S1 .01227(10) .18292(9) .61700(5) .0498(2) Uani d . 1 . . S S2 .22893(10) .37285(8) .73337(5) .0411(2) Uani d . 1 . . S S3 .37402(9) .13706(7) .66069(5) .0444(2) Uani d . 1 . . S S4 .21983(10) .36718(7) .54555(5) .0417(2) Uani d . 1 . . S N1 .7978(3) .1048(2) .42911(15) .0299(5) Uani d . 1 . . N H1N .793(3) .092(3) .474(2) .036 Uiso d . 1 . . H H2N .765(4) .048(3) .4057(19) .036 Uiso d . 1 . . H N2 .8559(2) .2631(2) .33040(13) .0243(5) Uani d . 1 . . N N3 .5992(3) .1667(2) .28322(14) .0287(5) Uani d . 1 . . N H3N .595(3) .093(3) .2907(18) .034 Uiso d . 1 . . H H4N .521(4) .190(3) .2664(19) .034 Uiso d . 1 . . H N4 1.1187(3) .5000(3) .3448(2) .0507(8) Uani d . 1 . . N H5N 1.148(4) .491(4) .392(2) .061 Uiso d . 1 . . H H6N 1.062(4) .553(4) .346(2) .061 Uiso d . 1 . . H N5 .5928(3) .4036(2) .33604(14) .0287(5) Uani d . 1 . . N H7N .647(3) .464(3) .3365(18) .034 Uiso d . 1 . . H H8N .558(4) .392(3) .291(2) .034 Uiso d . 1 . . H N6 .5187(2) .2402(2) .42811(13) .0248(5) Uani d . 1 . . N N7 .7791(3) .3383(2) .48101(14) .0284(5) Uani d . 1 . . N H9N .850(4) .305(3) .5061(19) .034 Uiso d . 1 . . H H10N .799(3) .403(3) .4761(19) .034 Uiso d . 1 . . H N8 .2772(4) -.0069(3) .4206(2) .0484(8) Uani d . 1 . . N H11N .297(4) -.029(4) .379(2) .058 Uiso d . 1 . . H H12N .197(4) -.009(4) .400(2) .058 Uiso d . 1 . . H C1 .9396(3) .1191(3) .42383(19) .0349(7) Uani d . 1 . . C H1C .996(4) .048(3) .4361(19) .042 Uiso d . 1 . . H H2C .984(4) .175(3) .4580(19) .042 Uiso d . 1 . . H C2 .9370(3) .1575(3) .34778(19) .0331(7) Uani d . 1 . . C H3C 1.023(4) .176(3) .3394(19) .040 Uiso d . 1 . . H H4C .894(3) .099(3) .3124(19) .040 Uiso d . 1 . . H C3 .6805(3) .1805(3) .22942(18) .0361(7) Uani d . 1 . . C H5C .623(4) .205(3) .187(2) .043 Uiso d . 1 . . H H6C .721(4) .114(3) .2233(19) .043 Uiso d . 1 . . H C4 .7894(3) .2705(3) .25226(16) .0322(6) Uani d . 1 . . C H7C .852(4) .265(3) .223(2) .039 Uiso d . 1 . . H H8C .751(4) .342(3) .2403(19) .039 Uiso d . 1 . . H C5 .9393(3) .3646(3) .35566(17) .0282(6) Uani d . 1 . . C H9C .995(3) .352(3) .4084(19) .034 Uiso d . 1 . . H H10C .879(3) .427(3) .3526(18) .034 Uiso d . 1 . . H C6 1.0417(4) .4006(3) .3134(2) .0392(8) Uani d . 1 . . C H11C 1.107(4) .345(3) .308(2) .047 Uiso d . 1 . . H H12C .997(4) .423(3) .265(2) .047 Uiso d . 1 . . H C7 .4840(4) .4312(3) .3716(2) .0369(7) Uani d . 1 . . C H13C .411(4) .467(3) .342(2) .044 Uiso d . 1 . . H H14C .525(4) .480(3) .413(2) .044 Uiso d . 1 . . H C8 .4189(3) .3245(3) .39028(19) .0327(7) Uani d . 1 . . C H15C .352(4) .343(3) .4167(19) .039 Uiso d . 1 . . H H16C .369(4) .287(3) .345(2) .039 Uiso d . 1 . . H C9 .6793(4) .3488(4) .5246(2) .0480(9) Uani d . 1 . . C H17C .611(4) .417(4) .508(2) .058 Uiso d . 1 . . H H18C .729(4) .337(4) .574(2) .058 Uiso d . 1 . . H C10 .5700(4) .2620(3) .50690(18) .0401(8) Uani d . 1 . . C H19C .495(4) .272(3) .531(2) .048 Uiso d . 1 . . H H20C .625(4) .187(3) .529(2) .048 Uiso d . 1 . . H C11 .4579(3) .1257(3) .41681(19) .0315(6) Uani d . 1 . . C H21C .528(3) .068(3) .4366(18) .038 Uiso d . 1 . . H H22C .438(3) .108(3) .3657(19) .038 Uiso d . 1 . . H C12 .3276(4) .1064(3) .4406(2) .0428(8) Uani d . 1 . . C H23C .349(4) .111(3) .491(2) .051 Uiso d . 1 . . H H24C .261(4) .166(4) .420(2) .051 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 W .03021(7) .02242(6) .02403(6) -.00081(5) .00424(4) .00048(4) Ni .02156(16) .01876(17) .02060(16) .00015(12) .00602(13) -.00127(12) S1 .0450(5) .0585(6) .0450(5) -.0151(4) .0097(4) -.0015(4) S2 .0533(5) .0360(4) .0313(4) .0021(4) .0058(4) -.0045(3) S3 .0456(5) .0314(4) .0478(5) .0097(4) -.0042(4) -.0051(4) S4 .0613(6) .0329(4) .0341(4) -.0009(4) .0179(4) .0061(3) N1 .0369(14) .0209(12) .0324(14) .0017(10) .0097(12) .0020(10) N2 .0253(11) .0243(12) .0246(11) -.0023(9) .0085(9) -.0027(9) N3 .0259(12) .0313(14) .0284(13) -.0047(11) .0061(10) -.0049(10) N4 .0438(19) .0419(19) .071(2) -.0165(14) .0227(18) -.0084(17) N5 .0320(13) .0245(13) .0307(13) .0010(10) .0097(11) .0048(10) N6 .0252(11) .0261(12) .0240(11) -.0004(9) .0079(9) .0008(9) N7 .0302(13) .0280(13) .0265(12) -.0035(11) .0061(10) -.0029(10) N8 .0417(17) .0440(18) .060(2) -.0126(15) .0135(16) .0036(15) C1 .0335(17) .0298(16) .0389(17) .0066(13) .0043(14) .0030(13) C2 .0307(16) .0270(15) .0447(18) .0036(12) .0151(14) -.0035(13) C3 .0323(17) .048(2) .0289(15) -.0036(14) .0099(13) -.0125(14) C4 .0317(15) .0420(18) .0248(14) -.0061(14) .0106(12) -.0034(13) C5 .0255(14) .0276(15) .0316(15) -.0049(12) .0076(12) -.0032(12) C6 .0324(17) .043(2) .046(2) -.0110(15) .0169(15) -.0059(16) C7 .0351(17) .0291(16) .049(2) .0092(13) .0148(15) .0055(14) C8 .0252(15) .0334(17) .0417(18) .0057(12) .0124(14) .0052(14) C9 .047(2) .065(3) .0340(18) -.0135(19) .0145(16) -.0162(18) C10 .0391(17) .058(2) .0263(15) -.0104(16) .0144(13) -.0049(15) C11 .0303(16) .0277(15) .0384(17) -.0015(12) .0123(13) .0025(13) C12 .0405(19) .0385(19) .054(2) -.0077(15) .0212(17) .0025(17) 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 W S1 . 2.1580(10) y W S2 . 2.1860(9) y W S3 . 2.2122(9) y W S4 . 2.1929(9) y Ni N1 . 2.130(3) y Ni N2 . 2.146(2) y Ni N3 . 2.138(3) y Ni N5 . 2.136(3) y Ni N6 . 2.152(2) y Ni N7 . 2.143(3) y N1 C1 . 1.477(4) n N1 H1N . .87(4) n N1 H2N . .83(4) n N2 C5 . 1.480(4) n N2 C4 . 1.481(4) n N2 C2 . 1.489(4) n N3 C3 . 1.480(4) n N3 H3N . .89(4) n N3 H4N . .83(4) n N4 C6 . 1.457(5) n N4 H5N . .88(4) n N4 H6N . .86(4) n N5 C7 . 1.471(4) n N5 H7N . .90(4) n N5 H8N . .86(4) n N6 C8 . 1.477(4) n N6 C11 . 1.485(4) n N6 C10 . 1.489(4) n N7 C9 . 1.468(4) n N7 H9N . .86(4) n N7 H10N . .80(4) n N8 C12 . 1.454(5) n N8 H11N . .91(4) n N8 H12N . .81(4) n C1 C2 . 1.518(5) n C1 H1C . 1.01(4) n C1 H2C . .96(4) n C2 H3C . .95(4) n C2 H4C . .99(4) n C3 C4 . 1.519(5) n C3 H5C . .93(4) n C3 H6C . .91(4) n C4 H7C . .95(4) n C4 H8C . .94(4) n C5 C6 . 1.528(4) n C5 H9C . 1.04(3) n C5 H10C . .95(3) n C6 H11C . .96(4) n C6 H12C . .97(4) n C7 C8 . 1.510(5) n C7 H13C . .91(4) n C7 H14C . .98(4) n C8 H15C . .97(4) n C8 H16C . .99(4) n C9 C10 . 1.488(5) n C9 H17C . 1.06(4) n C9 H18C . .96(4) n C10 H19C . .99(4) n C10 H20C . 1.08(4) n C11 C12 . 1.519(4) n C11 H21C . .99(4) n C11 H22C . .97(3) n C12 H23C . .94(4) n C12 H24C . .99(4) n