data_2011734 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 26 _journal_page_last 27 _publ_section_title ; Tris{bis[N-(2-aminoethyl)-1,2-ethanediamine-\k^3^N]nickel(II)} bis(tetrathioantimonate) ; loop_ _publ_author_name 'St\"ahler, Ralph' 'N\"ather, Christian' 'Bensch, Wolfgang' _chemical_name_common ; Tris{bis[N-(2-aminoethyl)-1,2-ethanediamine-\k^3^N]nickel(II)} bis(tetrathioantimonate) ; _chemical_formula_moiety '3C8 H26 N6 Ni1 2+, 2S4 Sb1 3-' _chemical_formula_sum 'C24 H78 N18 Ni3 S8 Sb2' _chemical_formula_iupac '[Ni (C4 H13 N2)2]3 [Sb1 S4]2' _chemical_formula_weight 1295.19 _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 7.5259(15) _cell_length_b 14.250(3) _cell_length_c 14.565(3) _cell_angle_alpha 111.79(3) _cell_angle_beta 90.72(3) _cell_angle_gamma 90.92(3) _cell_volume 1450.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.483 _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 Sb1 .857195(17) .805903(10) .200520(10) .02672(4) Uani d . 1 . . Sb S1 .99745(8) .95855(4) .29879(4) .03653(12) Uani d . 1 . . S S2 .59471(8) .84297(5) .13708(5) .04119(13) Uani d . 1 . . S S3 1.03208(9) .71683(5) .06747(5) .04234(14) Uani d . 1 . . S S4 .79343(10) .70958(5) .29461(5) .04316(14) Uani d . 1 . . S Ni1 1.0000 1.0000 .0000 .03548(9) Uani d S 1 . . Ni N1 1.2026(3) .96153(19) .08280(19) .0497(6) Uani d . 1 . . N H1N 1.1532 .9391 .1270 .060 Uiso calc R 1 . . H H2N 1.2695 .9121 .0420 .060 Uiso calc R 1 . . H C1 1.3096(5) 1.0486(3) .1323(4) .0901(15) Uani d . 1 . . C H1A 1.4327 1.0288 .1219 .108 Uiso calc R 1 . . H H1B 1.2888 1.0688 .2026 .108 Uiso calc R 1 . . H C2 1.2899(5) 1.1355(3) .1077(3) .0767(11) Uani d . 1 . . C H2A 1.3744 1.1325 .0570 .092 Uiso calc R 1 . . H H2B 1.3197 1.1951 .1657 .092 Uiso calc R 1 . . H N2 1.1112(3) 1.14692(16) .07216(17) .0452(5) Uani d . 1 B . N H3N 1.1217 1.1768 .0270 .054 Uiso calc R 1 . . H C3 .9935(5) 1.2074(2) .1501(3) .0690(9) Uani d . 1 . . C H3A 1.0669 1.2574 .2005 .083 Uiso calc R 1 A 1 H H3B .9163 1.2438 .1217 .083 Uiso calc R 1 A 1 H C4 .8818(17) 1.1576(5) .1992(10) .061(3) Uani d P .488(19) B 1 C H4A .7731 1.1946 .2200 .074 Uiso calc PR .488(19) B 1 H H4B .9432 1.1559 .2575 .074 Uiso calc PR .488(19) B 1 H C4' .8249(10) 1.1542(5) .1505(8) .051(2) Uani d P .512(19) B 2 C H4C .7739 1.1844 .2155 .061 Uiso calc PR .512(19) B 2 H H4D .7433 1.1649 .1034 .061 Uiso calc PR .512(19) B 2 H N3 .8376(3) 1.04909(18) .12719(19) .0504(5) Uani d . 1 . . N H4N .7230 1.0456 .1074 .060 Uiso calc R 1 B 1 H H5N .8502 1.0066 .1595 .060 Uiso calc R 1 B 1 H Ni2 .5000 .5000 .0000 .02827(8) Uani d S 1 . . Ni N4 .7465(3) .49477(14) .07239(15) .0367(4) Uani d . 1 . . N H6N .8263 .4604 .0274 .044 Uiso calc R 1 . . H H7N .7900 .5579 .1047 .044 Uiso calc R 1 . . H C5 .7158(3) .44471(19) .1423(2) .0432(5) Uani d . 1 . . C H5A .6777 .4937 .2048 .052 Uiso calc R 1 . . H H5B .8254 .4157 .1540 .052 Uiso calc R 1 . . H C6 .5737(4) .36181(18) .1005(2) .0445(6) Uani d . 1 . . C H6A .6234 .3057 .0470 .053 Uiso calc R 1 . . H H6B .5390 .3374 .1518 .053 Uiso calc R 1 . . H N5 .4152(3) .39640(14) .06345(15) .0359(4) Uani d . 1 . . N H8N .3629 .3422 .0150 .043 Uiso calc R 1 . . H C7 .2797(4) .4464(2) .1359(2) .0478(6) Uani d . 1 . . C H7A .2649 .4104 .1803 .057 Uiso calc R 1 . . H H7B .1671 .4426 .1014 .057 Uiso calc R 1 . . H C8 .3260(4) .5571(2) .1968(2) .0489(6) Uani d . 1 . . C H8A .2195 .5915 .2274 .059 Uiso calc R 1 . . H H8B .4105 .5610 .2489 .059 Uiso calc R 1 . . H N6 .4024(3) .60801(14) .13483(15) .0368(4) Uani d . 1 . . N H9N .4920 .6498 .1682 .044 Uiso calc R 1 . . H H10N .3189 .6454 .1207 .044 Uiso calc R 1 . . H Ni3 .5000 .0000 .5000 .03448(9) Uani d S 1 . . Ni N7 .2853(3) .09136(18) .48989(16) .0472(5) Uani d . 1 . . N H11N .1942 .0516 .4555 .057 Uiso calc R 1 . . H H12N .2474 .1279 .5509 .057 Uiso calc R 1 . . H C9 .3417(5) .1589(3) .4410(2) .0620(8) Uani d . 1 . . C H9A .3737 .2247 .4903 .074 Uiso calc R 1 . . H H9B .2443 .1675 .4008 .074 Uiso calc R 1 . . H C10 .5002(6) .1161(3) .3762(3) .0719(10) Uani d . 1 . . C H10A .4596 .0608 .3169 .086 Uiso calc R 1 . . H H10B .5521 .1682 .3562 .086 Uiso calc R 1 . . H N8 .6368(3) .07957(18) .42620(18) .0513(6) Uani d . 1 . . N H13N .7042 .0349 .3791 .062 Uiso calc R 1 . . H C11 .7572(4) .1549(3) .4976(3) .0682(9) Uani d . 1 . . C H11A .7829 .2087 .4738 .082 Uiso calc R 1 . . H H11B .8685 .1231 .5017 .082 Uiso calc R 1 . . H C12 .6800(4) .2001(2) .6002(2) .0601(8) Uani d . 1 . . C H12A .7727 .2364 .6475 .072 Uiso calc R 1 . . H H12B .5890 .2477 .6008 .072 Uiso calc R 1 . . H N9 .6036(3) .12051(17) .62835(16) .0484(5) Uani d . 1 . . N H14N .5159 .1456 .6715 .058 Uiso calc R 1 . . H H15N .6875 .0968 .6582 .058 Uiso calc R 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 Sb1 .02564(7) .02224(6) .02859(7) -.00025(4) .00112(5) .00518(5) S1 .0362(3) .0303(3) .0364(3) -.0079(2) -.0062(2) .0051(2) S2 .0292(3) .0369(3) .0551(4) .0001(2) -.0073(2) .0145(3) S3 .0451(3) .0361(3) .0431(3) .0140(2) .0154(3) .0105(2) S4 .0583(4) .0339(3) .0370(3) -.0074(3) .0023(3) .0131(2) Ni1 .03042(19) .0346(2) .0476(2) -.00614(16) -.00727(17) .02295(18) N1 .0392(11) .0563(14) .0668(15) -.0041(10) -.0085(10) .0387(12) C1 .0534(19) .073(2) .153(4) -.0180(17) -.056(2) .055(3) C2 .0563(19) .077(2) .110(3) -.0339(17) -.035(2) .052(2) N2 .0489(12) .0413(11) .0530(13) -.0112(9) -.0096(10) .0272(10) C3 .085(2) .0430(16) .067(2) -.0097(16) .0067(18) .0067(14) C4 .079(6) .037(3) .067(6) .012(3) .022(5) .017(3) C4' .057(4) .043(3) .053(5) .017(3) .006(3) .017(3) N3 .0459(12) .0506(13) .0616(14) -.0076(10) -.0014(11) .0293(12) Ni2 .02789(17) .01989(16) .03364(19) .00024(13) .00098(14) .00602(14) N4 .0321(9) .0254(8) .0472(11) .0004(7) -.0010(8) .0074(8) C5 .0457(13) .0353(12) .0468(13) .0032(10) -.0096(11) .0134(10) C6 .0534(15) .0289(11) .0528(15) .0005(10) -.0027(12) .0173(10) N5 .0405(10) .0242(8) .0379(10) -.0058(7) .0002(8) .0058(7) C7 .0475(14) .0389(13) .0538(15) -.0082(11) .0120(12) .0137(11) C8 .0541(15) .0410(13) .0434(13) -.0002(11) .0128(12) .0060(11) N6 .0357(10) .0250(8) .0425(10) .0002(7) .0020(8) .0041(7) Ni3 .02723(18) .0374(2) .02894(19) .00137(15) .00012(14) .00080(16) N7 .0382(11) .0524(13) .0378(11) .0081(9) -.0037(9) .0014(9) C9 .069(2) .0608(19) .0551(17) .0181(16) -.0031(15) .0194(15) C10 .095(3) .074(2) .0512(18) .018(2) .0174(18) .0282(17) N8 .0486(13) .0488(13) .0485(13) .0061(10) .0166(10) .0082(10) C11 .0522(17) .0530(18) .087(2) -.0113(14) .0176(17) .0117(17) C12 .0478(15) .0429(15) .0671(19) -.0031(12) -.0033(14) -.0054(13) N9 .0357(10) .0517(13) .0385(11) .0046(9) .0000(9) -.0058(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 Sb1 S4 . 2.3205(8) Y Sb1 S2 . 2.3206(8) Y Sb1 S3 . 2.3218(11) Y Sb1 S1 . 2.3389(11) Y Ni1 N2 . 2.116(2) Y Ni1 N2 2_775 2.116(2) N Ni1 N3 2_775 2.130(3) N Ni1 N3 . 2.130(3) Y Ni1 N1 . 2.133(2) Y Ni1 N1 2_775 2.133(2) N N1 C1 . 1.412(4) N C1 C2 . 1.421(5) N C2 N2 . 1.468(4) N N2 C3 . 1.462(4) N C3 C4 . 1.447(8) N C3 C4' . 1.469(8) N C4 N3 . 1.540(9) N C4' N3 . 1.413(7) N Ni2 N5 . 2.107(2) Y Ni2 N5 2_665 2.107(2) N Ni2 N4 2_665 2.138(2) N Ni2 N4 . 2.138(2) Y Ni2 N6 . 2.143(2) Y Ni2 N6 2_665 2.143(2) N N4 C5 . 1.462(3) N C5 C6 . 1.523(3) N C6 N5 . 1.469(3) N N5 C7 . 1.468(3) N C7 C8 . 1.527(4) N C8 N6 . 1.468(3) N Ni3 N8 2_656 2.097(2) N Ni3 N8 . 2.097(2) Y Ni3 N7 . 2.129(2) Y Ni3 N7 2_656 2.129(2) N Ni3 N9 2_656 2.142(2) N Ni3 N9 . 2.142(2) Y N7 C9 . 1.454(4) N C9 C10 . 1.520(5) N C10 N8 . 1.462(5) N N8 C11 . 1.474(4) N C11 C12 . 1.518(5) N C12 N9 . 1.454(4) N