#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2009088.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_2009088 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _journal_page_first 1800 _journal_page_last 1802 _publ_section_title ; Bis(pyrimidine-2-thiolato-N,S)bis(trimethyl phosphite-P)cobalt(III) hexafluorophosphate ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Ye-Xiang Tong' 'Cheng-Yong Su' 'Bei-Sheng Kang' 'Xiao-Lan Yu' 'Xiao-Ming Chen' _chemical_formula_moiety 'C14 H24 Co F6 N4 O6 P3 S2' _chemical_formula_sum 'C14 H24 Co F6 N4 O6 P3 S2' _chemical_formula_iupac '[Co (C4 H3 N2 S1)2 (C3 H9 O3 P1)2] P1 F6' _chemical_formula_weight 674.33 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.194(3) _cell_length_b 11.059(2) _cell_length_c 16.262(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.19(3) _cell_angle_gamma 90.00 _cell_volume 2670.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.677 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .067 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 Co1 .35111(6) .21719(8) .12958(6) .0422(3) Uani d . 1 . . Co S1 .36646(15) .01846(17) .16759(12) .0573(5) Uani d . 1 . . S N1 .3286(4) .2025(5) .2445(3) .0459(14) Uani d . 1 . . N N2 .3497(5) .0271(6) .3316(4) .0641(18) Uani d . 1 . . N C1 .3125(5) .2718(8) .3071(5) .064(2) Uani d . 1 . . C H1A .3010 .3566 .2980 .080 Uiso d R 1 . . H C2 .3137(6) .2184(9) .3852(5) .076(3) Uani d . 1 . . C H2A .3029 .2653 .4318 .080 Uiso d R 1 . . H C3 .3317(6) .0971(9) .3928(5) .071(3) Uani d . 1 . . C H3A .3299 .0585 .4453 .080 Uiso d R 1 . . H C4 .3462(5) .0843(7) .2593(4) .0501(18) Uani d . 1 . . C S2 .35670(14) .42295(17) .12484(13) .0575(5) Uani d . 1 . . S N3 .4730(4) .2677(6) .1864(3) .0486(14) Uani d . 1 . . N N4 .5274(5) .4694(7) .2127(4) .0695(19) Uani d . 1 . . N C5 .5500(5) .2226(8) .2312(4) .059(2) Uani d . 1 . . C H5A .5567 .1367 .2384 .080 Uiso d R 1 . . H C6 .6186(6) .2997(11) .2668(6) .081(3) Uani d . 1 . . C H6A .6747 .2698 .2990 .080 Uiso d R 1 . . H C7 .6034(7) .4218(11) .2545(6) .085(3) Uani d . 1 . . C H7A .6516 .4763 .2774 .080 Uiso d R 1 . . H C8 .4646(5) .3892(7) .1804(5) .0536(19) Uani d . 1 . . C P1 .39021(13) .19997(18) .00882(11) .0484(5) Uani d . 1 . . P O1 .3946(4) .0629(5) -.0145(3) .0612(14) Uani d . 1 . . O O2 .3291(3) .2542(5) -.0735(3) .0597(14) Uani d . 1 . . O O3 .4867(3) .2564(5) .0160(3) .0639(15) Uani d . 1 . . O C9 .3786(7) .0109(9) -.0976(5) .091(3) Uani d . 1 . . C H9A .3859 -.0752 -.0928 .080 Uiso d R 1 . . H H9B .3185 .0294 -.1272 .080 Uiso d R 1 . . H H9C .4211 .0433 -.1279 .080 Uiso d R 1 . . H C10 .3212(7) .3799(8) -.0955(6) .084(3) Uani d . 1 . . C H10A .2804 .3890 -.1489 .080 Uiso d R 1 . . H H10B .2984 .4231 -.0532 .080 Uiso d R 1 . . H H10C .3791 .4118 -.0989 .080 Uiso d R 1 . . H C11 .5351(6) .2562(10) -.0518(5) .090(3) Uani d . 1 . . C H11A .5921 .2957 -.0332 .080 Uiso d R 1 . . H H11B .5448 .1742 -.0672 .080 Uiso d R 1 . . H H11C .5009 .2983 -.0996 .080 Uiso d R 1 . . H P2 .20995(13) .18884(18) .07196(12) .0498(5) Uani d . 1 . . P O4 .1655(3) .3113(4) .0353(3) .0565(13) Uani d . 1 . . O O5 .1918(4) .0985(6) -.0056(4) .0788(18) Uani d . 1 . . O O6 .1485(3) .1309(5) .1288(3) .0655(15) Uani d . 1 . . O C12 .0716(5) .3242(9) -.0054(6) .083(3) Uani d . 1 . . C H12A .0595 .4068 -.0222 .080 Uiso d R 1 . . H H12B .0591 .2731 -.0542 .080 Uiso d R 1 . . H H12C .0340 .3009 .0326 .080 Uiso d R 1 . . H C13 .1694(14) -.0202(18) -.0160(12) .078(5) Uiso d P .50 A 1 C C13' .1128(14) .0104(18) -.0245(11) .076(5) Uiso d P .50 A 2 C C14 .1119(6) .1953(9) .1912(5) .082(3) Uani d . 1 . . C H14A .0773 .1408 .2177 .080 Uiso d R 1 . . H H14B .1600 .2288 .2329 .080 Uiso d R 1 . . H H14C .0738 .2594 .1643 .080 Uiso d R 1 . . H P3 .34621(15) .1669(2) .65461(13) .0610(6) Uani d . 1 . . P F1 .3973(4) .2463(6) .5984(3) .110(2) Uani d . 1 . . F F2 .3058(6) .2826(7) .6856(6) .169(3) Uani d . 1 . . F F3 .2639(4) .1571(7) .5799(4) .137(3) Uani d . 1 . . F F4 .3859(6) .0523(7) .6227(5) .166(3) Uani d . 1 . . F F5 .2958(4) .0869(6) .7093(3) .117(2) Uani d . 1 . . F F6 .4298(4) .1770(8) .7293(4) .145(3) 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 Co1 .0418(5) .0472(5) .0389(5) .0034(4) .0115(4) .0002(4) S1 .0735(14) .0493(11) .0539(12) .0086(10) .0244(10) .0020(9) N1 .047(3) .058(4) .035(3) .000(3) .013(3) -.001(3) N2 .081(5) .074(4) .042(4) -.004(4) .024(3) .016(3) C1 .067(5) .069(5) .059(5) -.006(4) .023(4) -.014(4) C2 .087(7) .099(7) .046(5) -.020(6) .026(5) -.020(5) C3 .067(6) .102(8) .045(5) -.017(5) .018(4) .011(5) C4 .042(4) .057(5) .053(5) -.004(3) .012(3) .005(4) S2 .0508(12) .0508(11) .0695(13) .0025(9) .0094(10) .0026(10) N3 .040(3) .067(4) .040(3) .004(3) .013(3) .008(3) N4 .058(5) .077(5) .073(5) -.015(4) .013(4) -.001(4) C5 .046(5) .089(6) .043(4) .011(4) .012(4) .007(4) C6 .043(5) .125(9) .069(6) .003(6) .001(4) .005(6) C7 .058(6) .117(9) .079(7) -.030(6) .012(5) -.013(6) C8 .044(4) .066(5) .052(5) -.005(4) .014(4) -.001(4) P1 .0471(11) .0600(12) .0403(10) .0102(9) .0143(8) .0068(9) O1 .082(4) .061(3) .044(3) .020(3) .020(3) .002(2) O2 .068(3) .065(3) .045(3) .014(3) .008(3) .012(3) O3 .050(3) .094(4) .051(3) .001(3) .020(2) .007(3) C9 .120(9) .100(7) .048(5) .027(7) .006(5) -.018(5) C10 .101(8) .078(6) .070(6) .012(6) .007(6) .020(5) C11 .079(7) .127(9) .076(6) .004(6) .046(5) .017(6) P2 .0457(11) .0539(11) .0501(11) -.0028(9) .0108(9) -.0047(9) O4 .043(3) .063(3) .061(3) .003(2) .007(2) .004(3) O5 .070(4) .087(4) .080(4) -.014(3) .018(3) -.033(3) O6 .053(3) .068(3) .081(4) -.004(3) .026(3) .006(3) C12 .055(5) .086(7) .101(7) .015(5) -.004(5) .005(6) C14 .056(5) .120(8) .078(6) .007(5) .030(5) .014(6) P3 .0659(14) .0692(14) .0494(12) -.0115(11) .0152(11) .0006(10) F1 .095(4) .141(5) .095(4) -.024(4) .026(3) .047(4) F2 .203(8) .110(6) .217(9) .000(6) .095(7) -.055(6) F3 .094(5) .218(8) .081(4) -.041(5) -.025(3) .020(5) F4 .208(9) .110(5) .205(8) .036(6) .101(7) -.017(6) F5 .125(5) .157(6) .075(4) -.064(4) .035(3) .012(4) F6 .112(5) .228(9) .076(4) -.061(6) -.021(4) .038(5) 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 Co1 N3 . 1.968(6) ? Co1 N1 . 1.976(5) ? Co1 P2 . 2.174(2) ? Co1 P1 . 2.177(2) ? Co1 S2 . 2.279(2) ? Co1 S1 . 2.282(2) ? S1 C4 . 1.745(7) ? N1 C1 . 1.337(9) ? N1 C4 . 1.346(9) ? N2 C4 . 1.326(9) ? N2 C3 . 1.333(10) ? C1 C2 . 1.397(11) ? C2 C3 . 1.370(12) ? S2 C8 . 1.736(8) ? N3 C5 . 1.338(8) ? N3 C8 . 1.351(9) ? N4 C7 . 1.320(11) ? N4 C8 . 1.327(9) ? C5 C6 . 1.376(11) ? C6 C7 . 1.378(14) ? P1 O1 . 1.567(5) ? P1 O3 . 1.575(5) ? P1 O2 . 1.578(5) ? O1 C9 . 1.441(8) ? O2 C10 . 1.434(9) ? O3 C11 . 1.449(8) ? P2 O4 . 1.573(5) ? P2 O6 . 1.581(5) ? P2 O5 . 1.588(6) ? O4 C12 . 1.448(8) ? O5 C13 . 1.36(2) ? O5 C13' . 1.525(19) ? O6 C14 . 1.444(9) ? P3 F4 . 1.540(7) ? P3 F2 . 1.549(7) ? P3 F3 . 1.552(6) ? P3 F5 . 1.564(5) ? P3 F6 . 1.564(6) ? P3 F1 . 1.584(5) ?