#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2010576.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_2010576 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first e16 _journal_page_last e18 _publ_section_title ; [Bis(diphenylphosphino)alkane](pentane-2,4-dithionato) complexes of nickel(II) ; _space_group_IT_number 11 _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _[local]_cod_cif_authors_sg_H-M 'P 21/m' loop_ _publ_author_name 'Boyd, Peter D. W.' 'Rickard, Clifton E. F.' 'Cavell, Kingsley J.' _chemical_formula_moiety 'C32 H33 Ni P2 S2, F6 P' _chemical_formula_sum 'C32 H33 F6 Ni P3 S2' _chemical_formula_iupac '[Ni1 (C27 H26 P2) (C5 H7 S2)] P1 F6' _chemical_formula_weight 747.32 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.0345(2) _cell_length_b 15.8632(2) _cell_length_c 10.8058(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.14 _cell_angle_gamma 90.00 _cell_volume 1715.58(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _exptl_crystal_density_diffrn 1.447 _diffrn_ambient_temperature 203(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 Ni .38982(4) .2500 .82875(3) .04148(13) Uani d S 1 . . Ni S1 .31573(7) .35159(4) .93587(6) .05904(18) Uani d . 1 . . S P1 .48000(6) .15051(4) .71370(5) .04412(15) Uani d . 1 . . P C1 .1797(4) .4041(2) 1.1268(4) .0995(12) Uani d . 1 . . C H1A .2089 .4550 1.0870 .149 Uiso calc R 1 . . H H1B .2158 .4030 1.2125 .149 Uiso calc R 1 . . H H1C .0828 .4032 1.1241 .149 Uiso calc R 1 . . H C2 .2287(3) .32782(18) 1.0594(2) .0614(7) Uani d . 1 . . C C3 .1970(4) .2500 1.1021(4) .0701(11) Uani d S 1 . . C H3 .1454 .2500 1.1713 .084 Uiso calc SR 1 . . H C4 .4751(3) .16997(16) .5464(2) .0573(6) Uani d . 1 . . C H4A .5172 .1220 .5074 .069 Uiso calc R 1 . . H H4B .3813 .1714 .5141 .069 Uiso calc R 1 . . H C5 .5420(4) .2500 .5057(3) .0556(8) Uani d S 1 . . C H5A .5422 .2500 .4150 .067 Uiso calc SR 1 . . H H5B .6353 .2500 .5396 .067 Uiso calc SR 1 . . H C11 .4021(2) .04626(15) .7167(2) .0509(5) Uani d . 1 . . C C12 .4656(3) -.02166(17) .7736(3) .0662(7) Uani d . 1 . . C H12A .5515 -.0153 .8134 .079 Uiso calc R 1 . . H C13 .4027(4) -.09994(19) .7725(3) .0842(9) Uani d . 1 . . C H13A .4467 -.1464 .8108 .101 Uiso calc R 1 . . H C14 .2783(4) -.1095(2) .7162(3) .0845(10) Uani d . 1 . . C H14A .2367 -.1626 .7155 .101 Uiso calc R 1 . . H C15 .2135(3) -.0424(2) .6607(3) .0823(9) Uani d . 1 . . C H15A .1270 -.0493 .6225 .099 Uiso calc R 1 . . H C16 .2744(3) .03590(19) .6605(3) .0708(7) Uani d . 1 . . C H16A .2292 .0820 .6224 .085 Uiso calc R 1 . . H C21 .6545(2) .13424(15) .7651(3) .0541(6) Uani d U 1 . . C C22 .6943(3) .1442(2) .8880(4) .0965(12) Uani d U 1 . . C H22A .6305 .1570 .9447 .116 Uiso calc R 1 . . H C23 .8272(4) .1356(3) .9300(5) .141(2) Uani d U 1 . . C H23A .8535 .1422 1.0147 .170 Uiso calc R 1 . . H C24 .9187(4) .1175(3) .8481(6) .131(2) Uani d U 1 . . C H24A 1.0093 .1130 .8761 .157 Uiso calc R 1 . . H C25 .8824(4) .1061(4) .7281(6) .142(2) Uani d U 1 . . C H25A .9470 .0928 .6724 .170 Uiso calc R 1 . . H C26 .7489(3) .1139(3) .6855(4) .1076(14) Uani d U 1 . . C H26A .7235 .1051 .6011 .129 Uiso calc R 1 . . H P2 .05592(9) .2500 .45600(9) .0620(3) Uani d S 1 . . P F1 -.0151(2) .2500 .3197(2) .1001(10) Uani d S 1 . . F F2 -.0847(3) .2500 .5091(3) .1087(10) Uani d S 1 . . F F3 .1291(3) .2500 .5914(2) .0930(8) Uani d S 1 . . F F4 .1976(2) .2500 .4005(2) .1244(13) Uani d S 1 . . F F5 .0568(2) .15064(14) .4566(3) .1275(9) Uani d . 1 . . F 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 Ni .0358(2) .0466(2) .0424(2) .000 .00536(16) .000 S1 .0621(4) .0539(4) .0640(4) -.0058(3) .0244(3) -.0084(3) P1 .0391(3) .0472(3) .0464(3) .0010(2) .0057(2) -.0009(2) C1 .110(3) .085(2) .110(3) -.018(2) .059(2) -.040(2) C2 .0597(15) .0711(17) .0552(14) -.0074(13) .0157(12) -.0153(13) C3 .077(3) .078(3) .059(2) .000 .0291(19) .000 C4 .0658(15) .0615(15) .0450(13) -.0015(12) .0061(11) -.0054(11) C5 .060(2) .065(2) .0423(17) .000 .0093(15) .000 C11 .0500(13) .0496(13) .0540(13) -.0025(10) .0104(10) -.0055(11) C12 .0674(16) .0549(16) .0757(18) -.0021(13) .0028(14) .0038(13) C13 .098(2) .0538(17) .102(2) -.0060(16) .0096(19) .0056(16) C14 .096(2) .0600(19) .100(2) -.0255(18) .022(2) -.0142(17) C15 .0680(18) .082(2) .097(2) -.0243(17) .0032(17) -.0141(18) C16 .0554(15) .0674(18) .088(2) -.0092(13) -.0026(14) -.0030(15) C21 .0400(12) .0479(13) .0752(16) .0014(10) .0087(11) .0090(12) C22 .0629(18) .112(3) .110(3) .0295(18) -.0289(18) -.046(2) C23 .085(3) .138(4) .190(5) .042(3) -.069(3) -.069(4) C24 .047(2) .104(3) .236(6) -.0044(19) -.017(3) .051(4) C25 .062(2) .193(5) .178(5) .047(3) .058(3) .119(4) C26 .0673(19) .159(4) .100(2) .047(2) .0360(18) .062(2) P2 .0480(5) .0877(7) .0500(5) .000 .0014(4) .000 F1 .0494(12) .196(3) .0543(13) .000 -.0042(10) .000 F2 .0692(16) .177(3) .0839(18) .000 .0311(14) .000 F3 .1046(19) .119(2) .0529(13) .000 -.0154(13) .000 F4 .0436(13) .255(4) .0738(16) .000 .0017(12) .000 F5 .1328(19) .0891(15) .153(2) .0085(13) -.0389(16) -.0239(14) 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 Ni S1 . 2.1479(7) ? Ni S1 4_565 2.1479(7) ? Ni P1 . 2.2401(6) ? Ni P1 4_565 2.2401(6) ? S1 C2 . 1.690(3) ? S1 P1 4_565 3.0088(8) ? S1 S1 4_565 3.2230(13) ? P1 C21 . 1.816(2) ? P1 C11 . 1.830(2) ? P1 C4 . 1.832(2) ? P1 P1 4_565 3.1565(12) ? C1 C2 . 1.513(4) ? C2 C3 . 1.364(3) ? C3 C2 4_565 1.364(3) ? C4 C5 . 1.516(3) ? C5 C4 4_565 1.516(3) ? C11 C12 . 1.375(4) ? C11 C16 . 1.388(3) ? C12 C13 . 1.393(4) ? C13 C14 . 1.357(5) ? C14 C15 . 1.364(5) ? C15 C16 . 1.384(4) ? C21 C26 . 1.363(4) ? C21 C22 . 1.368(4) ? C22 C23 . 1.384(5) ? C23 C24 . 1.352(7) ? C24 C25 . 1.334(7) ? C25 C26 . 1.391(5) ? P2 F2 . 1.561(3) ? P2 F5 4_565 1.576(2) ? P2 F5 . 1.576(2) ? P2 F4 . 1.582(3) ? P2 F3 . 1.589(2) ? P2 F1 . 1.589(2) ? _cod_database_code 2010576