#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011520.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_2011520 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1296 _journal_page_last 1297 _publ_section_title ; Bis(di-tert-butylthiophosphinic isopropylamidato-N,S)nickel(II) ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Kuchen, Wilhelm' 'Wunderlich, Hartmut' _chemical_formula_moiety 'C22 H50 N2 Ni P2 S2' _chemical_formula_sum 'C22 H50 N2 Ni P2 S2' _chemical_formula_weight 527.41 _chemical_melting_point 407 _symmetry_cell_setting monoclinic 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 16.123(2) _cell_length_b 11.6840(10) _cell_length_c 15.815(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.740(10) _cell_angle_gamma 90.00 _cell_volume 2979.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _exptl_crystal_density_diffrn 1.176 _diffrn_ambient_temperature 300(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 .251038(18) .11069(2) .178323(18) .03863(11) Uani d . 1 . . Ni S1 .38047(4) .17682(6) .23412(5) .0580(2) Uani d . 1 . . S S2 .12902(5) .10909(6) .26158(5) .0627(2) Uani d . 1 . . S P1 .35848(4) .28310(5) .13636(4) .04049(16) Uani d . 1 . . P P2 .14585(4) -.05723(5) .23521(4) .04095(16) Uani d . 1 . . P N1 .27274(12) .23254(16) .09830(12) .0401(4) Uani d . 1 . . N N2 .22661(12) -.05205(16) .17676(12) .0413(4) Uani d . 1 . . N C1 .22290(16) .2724(2) .02567(16) .0542(6) Uani d . 1 . . C H1 .2510 .3379 .0000 .081 Uiso calc R 1 . . H C2 .27440(18) -.1451(2) .1372(2) .0604(7) Uani d . 1 . . C H2 .2473 -.2183 .1494 .091 Uiso calc R 1 . . H C3 .13709(19) .3095(4) .0522(2) .0856(11) Uani d . 1 . . C H3A .1062 .3350 .0034 .128 Uiso calc R 1 . . H H3B .1417 .3710 .0922 .128 Uiso calc R 1 . . H H3C .1090 .2461 .0777 .128 Uiso calc R 1 . . H C4 .2148(2) .1778(4) -.0403(2) .0887(11) Uani d . 1 . . C H4A .1821 .2048 -.0874 .133 Uiso calc R 1 . . H H4B .1882 .1125 -.0156 .133 Uiso calc R 1 . . H H4C .2689 .1564 -.0594 .133 Uiso calc R 1 . . H C5 .2754(3) -.1274(4) .0417(2) .1010(14) Uani d . 1 . . C H5A .3067 -.1877 .0160 .152 Uiso calc R 1 . . H H5B .3007 -.0550 .0293 .152 Uiso calc R 1 . . H H5C .2196 -.1283 .0199 .152 Uiso calc R 1 . . H C6 .3624(2) -.1488(3) .1718(3) .0819(10) Uani d . 1 . . C H6A .3921 -.2097 .1451 .123 Uiso calc R 1 . . H H6B .3614 -.1616 .2317 .123 Uiso calc R 1 . . H H6C .3894 -.0773 .1605 .123 Uiso calc R 1 . . H C11 .44588(16) .2715(3) .0598(2) .0614(7) Uani d . 1 . . C C12 .5287(2) .3056(4) .1008(3) .1073(15) Uani d . 1 . . C H12A .5270 .3850 .1163 .161 Uiso calc R 1 . . H H12B .5726 .2934 .0614 .161 Uiso calc R 1 . . H H12C .5384 .2599 .1503 .161 Uiso calc R 1 . . H C13 .4514(2) .1444(3) .0357(3) .1011(14) Uani d . 1 . . C H13A .4000 .1206 .0098 .152 Uiso calc R 1 . . H H13B .4618 .0996 .0856 .152 Uiso calc R 1 . . H H13C .4957 .1335 -.0034 .152 Uiso calc R 1 . . H C14 .4311(2) .3420(4) -.0206(2) .0939(12) Uani d . 1 . . C H14A .3790 .3205 -.0460 .141 Uiso calc R 1 . . H H14B .4750 .3278 -.0597 .141 Uiso calc R 1 . . H H14C .4299 .4219 -.0065 .141 Uiso calc R 1 . . H C15 .3461(2) .4310(2) .1799(2) .0612(7) Uani d . 1 . . C C16 .2714(3) .4251(3) .2385(3) .0944(13) Uani d . 1 . . C H16A .2233 .4008 .2069 .142 Uiso calc R 1 . . H H16B .2615 .4994 .2623 .142 Uiso calc R 1 . . H H16C .2826 .3714 .2832 .142 Uiso calc R 1 . . H C17 .4218(3) .4692(4) .2316(3) .1245(18) Uani d . 1 . . C H17A .4692 .4733 .1956 .187 Uiso calc R 1 . . H H17B .4323 .4151 .2762 .187 Uiso calc R 1 . . H H17C .4114 .5432 .2556 .187 Uiso calc R 1 . . H C18 .3276(3) .5193(3) .1110(3) .0989(13) Uani d . 1 . . C H18A .3738 .5240 .0735 .148 Uiso calc R 1 . . H H18B .3184 .5927 .1365 .148 Uiso calc R 1 . . H H18C .2789 .4968 .0796 .148 Uiso calc R 1 . . H C21 .05239(18) -.1130(3) .17779(19) .0646(8) Uani d . 1 . . C C22 -.0266(2) -.1002(4) .2286(3) .0925(12) Uani d . 1 . . C H22A -.0222 -.1453 .2792 .139 Uiso calc R 1 . . H H22B -.0732 -.1259 .1953 .139 Uiso calc R 1 . . H H22C -.0342 -.0212 .2433 .139 Uiso calc R 1 . . H C23 .0614(2) -.2377(4) .1512(2) .0944(13) Uani d . 1 . . C H23A .0670 -.2849 .2007 .142 Uiso calc R 1 . . H H23B .1098 -.2460 .1170 .142 Uiso calc R 1 . . H H23C .0132 -.2608 .1194 .142 Uiso calc R 1 . . H C24 .0438(2) -.0401(5) .0981(3) .130(2) Uani d . 1 . . C H24A .0932 -.0471 .0651 .194 Uiso calc R 1 . . H H24B .0360 .0385 .1136 .194 Uiso calc R 1 . . H H24C -.0031 -.0659 .0653 .194 Uiso calc R 1 . . H C25 .1664(2) -.1351(3) .33711(18) .0668(8) Uani d . 1 . . C C26 .2419(3) -.0788(4) .3762(2) .0969(13) Uani d . 1 . . C H26A .2878 -.0859 .3386 .145 Uiso calc R 1 . . H H26B .2553 -.1154 .4290 .145 Uiso calc R 1 . . H H26C .2305 .0007 .3859 .145 Uiso calc R 1 . . H C27 .0953(3) -.1205(5) .3987(3) .134(2) Uani d . 1 . . C H27A .0460 -.1552 .3755 .201 Uiso calc R 1 . . H H27B .0856 -.0405 .4081 .201 Uiso calc R 1 . . H H27C .1095 -.1567 .4514 .201 Uiso calc R 1 . . H C28 .1864(4) -.2616(3) .3223(3) .139(2) Uani d . 1 . . C H28A .1392 -.2988 .2969 .209 Uiso calc R 1 . . H H28B .1996 -.2975 .3754 .209 Uiso calc R 1 . . H H28C .2330 -.2677 .2854 .209 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 Ni .04046(17) .03194(16) .0436(2) -.00542(12) .00397(12) .00163(12) S1 .0592(4) .0533(4) .0608(4) -.0119(3) -.0195(3) .0138(3) S2 .0620(4) .0412(3) .0856(6) .0044(3) .0314(4) .0015(3) P1 .0397(3) .0360(3) .0458(4) -.0071(2) .0018(2) .0013(3) P2 .0439(3) .0367(3) .0422(4) -.0074(3) .0010(2) .0055(2) N1 .0403(10) .0412(10) .0388(10) -.0058(8) -.0011(8) .0058(8) N2 .0421(10) .0312(10) .0506(11) -.0045(8) .0021(8) -.0046(8) C1 .0513(14) .0633(17) .0480(14) -.0076(13) -.0049(11) .0168(13) C2 .0642(17) .0350(13) .082(2) -.0019(12) .0106(15) -.0182(13) C3 .0535(18) .105(3) .098(3) .0106(18) -.0118(17) .027(2) C4 .096(3) .115(3) .0553(18) .001(2) -.0227(18) -.010(2) C5 .115(3) .112(3) .076(2) .006(3) .023(2) -.048(2) C6 .0601(19) .067(2) .119(3) .0173(16) .0071(19) -.019(2) C11 .0432(14) .0669(19) .0746(18) -.0122(13) .0166(13) -.0029(15) C12 .0465(18) .151(4) .124(3) -.024(2) .012(2) -.010(3) C13 .081(2) .082(3) .142(4) -.003(2) .057(3) -.030(2) C14 .089(3) .123(3) .070(2) -.013(2) .0343(19) .014(2) C15 .0753(19) .0394(14) .0690(18) -.0108(13) .0072(15) -.0062(13) C16 .130(3) .061(2) .094(3) -.004(2) .044(2) -.0289(19) C17 .116(3) .081(3) .175(5) -.020(3) -.038(3) -.057(3) C18 .145(4) .0401(18) .112(3) .009(2) .027(3) .0143(18) C21 .0521(15) .081(2) .0604(17) -.0282(15) -.0067(13) .0144(15) C22 .0496(18) .105(3) .123(3) -.0177(18) .0040(19) .006(2) C23 .084(2) .108(3) .091(3) -.045(2) .001(2) -.034(2) C24 .088(3) .200(5) .099(3) -.063(3) -.052(2) .077(3) C25 .092(2) .0617(18) .0470(15) -.0068(16) -.0073(15) .0125(13) C26 .113(3) .116(3) .061(2) -.002(3) -.032(2) .002(2) C27 .125(4) .206(6) .072(3) -.015(4) .027(3) .055(3) C28 .273(7) .054(2) .088(3) .008(3) -.043(4) .027(2) 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 N1 . 1.9397(18) Yes Ni N2 . 1.9419(19) Yes Ni S2 . 2.3814(8) Yes Ni S1 . 2.3839(8) Yes S1 P1 . 2.0109(9) Yes S2 P2 . 2.0067(10) Yes P1 N1 . 1.6126(19) Yes P1 C15 . 1.871(3) ? P1 C11 . 1.875(3) ? P2 N2 . 1.608(2) Yes P2 C21 . 1.867(3) ? P2 C25 . 1.877(3) ? N1 C1 . 1.469(3) ? N2 C2 . 1.476(3) ? C1 C3 . 1.514(4) ? C1 C4 . 1.524(4) ? C2 C6 . 1.514(4) ? C2 C5 . 1.525(5) ? C11 C14 . 1.531(5) ? C11 C12 . 1.529(4) ? C11 C13 . 1.536(5) ? C15 C17 . 1.527(5) ? C15 C18 . 1.528(5) ? C15 C16 . 1.531(5) ? C21 C22 . 1.522(5) ? C21 C24 . 1.527(5) ? C21 C23 . 1.523(5) ? C25 C26 . 1.509(5) ? C25 C27 . 1.524(5) ? C25 C28 . 1.531(5) ? _cod_database_code 2011520