#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012337.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_2012337 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 1274 _journal_page_last 1276 _publ_section_title ; A nitronyl nitroxide complex of a late transition metal ion with nitrate as a ligand ; loop_ _publ_author_name 'Yoshida, Takafumi' 'Suzuki, Takayoshi' 'Kaizaki, Sumio' _chemical_name_common '[Ni(NO~3~)(tmen)(NIT2py)]PF6.CH2Cl2' _chemical_formula_moiety 'C18 H32 N6 Ni O5 1+, F6 P 1-, C H2 Cl2' _chemical_formula_sum 'C19 H34 Cl2 F6 N6 Ni O5 P' _chemical_formula_iupac '[Ni (N O3) (C6 H16 N2) (C12 H16 N3 O2)] P F6, C H2 Cl2' _chemical_formula_weight 701.08 _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 8.6307(18) _cell_length_b 26.690(6) _cell_length_c 13.119(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.305(15) _cell_angle_gamma 90.00 _cell_volume 2952.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _exptl_crystal_density_diffrn 1.577 _diffrn_ambient_temperature 296(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 .41129(5) .410130(15) .66249(3) .03195(11) Uani d . 1 . . Ni Cl1 .6878(2) .70824(5) .74479(10) .0886(4) Uani d . 1 . . Cl Cl2 .89180(19) .62099(6) .77924(13) .0982(5) Uani d . 1 . . Cl P .14341(16) .73457(5) .09915(10) .0674(4) Uani d . 1 . . P F1 .1098(4) .79279(12) .1031(3) .1081(11) Uani d . 1 . . F F2 .3162(5) .74151(18) .1505(4) .174(2) Uani d . 1 . . F F3 .0941(6) .72666(16) .2033(3) .160(2) Uani d . 1 . . F F4 .1807(6) .74055(15) -.0121(3) .1473(17) Uani d . 1 . . F F5 -.0333(5) .72698(16) .0408(4) .1541(18) Uani d . 1 . . F F6 .1799(5) .67706(12) .0953(3) .1212(13) Uani d . 1 . . F O1 .4495(3) .36687(8) .79122(16) .0394(5) Uani d . 1 . . O O2 .7405(4) .46434(12) 1.0546(2) .0701(9) Uani d . 1 . . O O3 .3417(3) .47299(9) .56337(19) .0471(6) Uani d . 1 . . O O4 .2691(3) .46675(9) .71039(19) .0457(6) Uani d . 1 . . O O5 .1911(4) .53047(11) .6093(3) .0810(10) Uani d . 1 . . O N1 .5019(3) .38735(10) .88158(19) .0327(6) Uani d . 1 . . N N2 .6435(4) .43159(12) 1.0072(2) .0457(7) Uani d . 1 . . N N3 .6205(3) .45047(10) .7323(2) .0352(6) Uani d . 1 . . N N4 .2051(3) .36722(11) .5914(2) .0399(7) Uani d . 1 . . N N5 .5331(3) .36274(10) .5786(2) .0391(6) Uani d . 1 . . N N6 .2643(4) .49164(11) .6277(3) .0491(8) Uani d . 1 . . N C1 .6182(4) .42088(12) .9043(2) .0358(7) Uani d . 1 . . C C2 .4257(4) .37535(13) .9721(3) .0388(7) Uani d . 1 . . C C3 .5479(4) .39892(14) 1.0646(3) .0444(8) Uani d . 1 . . C C4 .2654(5) .40188(17) .9493(3) .0610(11) Uani d . 1 . . C H4A .2814 .4374 .9455 .075 Uiso calc R 1 . . H H4B .2104 .3948 1.0040 .075 Uiso calc R 1 . . H H4C .2034 .3902 .8840 .075 Uiso calc R 1 . . H C5 .4050(6) .31903(14) .9780(3) .0589(11) Uani d . 1 . . C H5A .3688 .3108 1.0403 .073 Uiso calc R 1 . . H H5B .5046 .3028 .9793 .073 Uiso calc R 1 . . H H5C .3284 .3079 .9181 .073 Uiso calc R 1 . . H C6 .4795(6) .43214(19) 1.1380(4) .0762(14) Uani d . 1 . . C H6A .5643 .4459 1.1899 .095 Uiso calc R 1 . . H H6B .4111 .4126 1.1714 .095 Uiso calc R 1 . . H H6C .4200 .4589 1.0991 .095 Uiso calc R 1 . . H C7 .6658(6) .36214(19) 1.1267(4) .0728(14) Uani d . 1 . . C H7A .6104 .3382 1.1603 .089 Uiso calc R 1 . . H H7B .7411 .3800 1.1784 .089 Uiso calc R 1 . . H H7C .7205 .3450 1.0805 .089 Uiso calc R 1 . . H C8 .7016(4) .44415(12) .8315(2) .0350(7) Uani d . 1 . . C C9 .8576(4) .46030(15) .8645(3) .0481(9) Uani d . 1 . . C H9 .9125 .4542 .9324 .059 Uiso calc R 1 . . H C10 .9295(5) .48525(15) .7958(3) .0534(10) Uani d . 1 . . C H10 1.0337 .4963 .8167 .063 Uiso calc R 1 . . H C11 .8467(4) .49380(14) .6966(3) .0488(9) Uani d . 1 . . C H11 .8927 .5112 .6492 .060 Uiso calc R 1 . . H C12 .6926(4) .47600(13) .6680(3) .0426(8) Uani d . 1 . . C H12 .6365 .4821 .6004 .052 Uiso calc R 1 . . H C13 .2621(5) .33203(16) .5203(4) .0640(12) Uani d . 1 . . C H13A .2523 .3476 .4524 .077 Uiso calc R 1 . . H H13B .1965 .3022 .5116 .077 Uiso calc R 1 . . H C14 .4305(5) .31769(14) .5617(4) .0606(11) Uani d . 1 . . C H14A .4393 .2999 .6271 .074 Uiso calc R 1 . . H H14B .4657 .2955 .5127 .074 Uiso calc R 1 . . H C15 .0731(5) .39703(16) .5283(3) .0615(11) Uani d . 1 . . C H15A .0304 .4190 .5733 .075 Uiso calc R 1 . . H H15B -.0085 .3748 .4932 .075 Uiso calc R 1 . . H H15C .1124 .4165 .4776 .075 Uiso calc R 1 . . H C16 .1372(5) .33916(17) .6686(3) .0598(11) Uani d . 1 . . C H16A .0971 .3623 .7127 .075 Uiso calc R 1 . . H H16B .2180 .3187 .7104 .075 Uiso calc R 1 . . H H16C .0523 .3182 .6329 .075 Uiso calc R 1 . . H C17 .5530(6) .38405(17) .4787(3) .0645(12) Uani d . 1 . . C H17A .6287 .4109 .4917 .077 Uiso calc R 1 . . H H17B .4530 .3966 .4408 .077 Uiso calc R 1 . . H H17C .5903 .3585 .4383 .077 Uiso calc R 1 . . H C18 .6906(5) .34657(17) .6376(4) .0646(12) Uani d . 1 . . C H18A .6827 .3365 .7066 .082 Uiso calc R 1 . . H H18B .7642 .3739 .6422 .082 Uiso calc R 1 . . H H18C .7273 .3189 .6025 .082 Uiso calc R 1 . . H C19 .8837(7) .6864(2) .7862(4) .0911(17) Uani d . 1 . . C H19A .9497 .7009 .7426 .108 Uiso calc R 1 . . H H19B .9251 .6971 .8574 .108 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 .0309(2) .03157(19) .03237(19) -.00208(19) .00456(14) .00162(18) Cl1 .1133(12) .0825(9) .0734(8) -.0056(8) .0277(8) -.0089(7) Cl2 .0929(11) .0907(10) .1147(12) -.0056(8) .0306(9) .0051(9) P .0641(8) .0749(8) .0668(7) .0291(6) .0214(6) .0230(6) F1 .124(3) .078(2) .120(3) .033(2) .023(2) .0144(19) F2 .073(3) .164(4) .258(6) .014(3) -.022(3) -.003(4) F3 .235(5) .157(4) .124(3) .113(4) .120(3) .064(3) F4 .242(5) .120(3) .102(3) .045(3) .085(3) .042(2) F5 .097(3) .129(3) .211(5) .012(3) -.023(3) .035(3) F6 .165(4) .081(2) .129(3) .056(2) .056(3) .033(2) O1 .0483(14) .0348(12) .0321(11) -.0095(11) .0022(10) .0012(9) O2 .080(2) .080(2) .0486(16) -.0380(17) .0088(15) -.0193(15) O3 .0457(15) .0488(15) .0465(14) .0007(12) .0093(12) .0142(12) O4 .0493(15) .0428(13) .0476(14) .0029(11) .0164(12) .0018(11) O5 .069(2) .0481(17) .127(3) .0233(16) .024(2) .0252(18) N1 .0332(14) .0317(13) .0320(13) -.0013(11) .0043(11) .0011(11) N2 .0452(17) .0511(17) .0384(15) -.0122(15) .0035(13) -.0060(13) N3 .0332(14) .0340(14) .0388(15) -.0046(11) .0085(12) .0028(12) N4 .0306(14) .0433(16) .0434(16) -.0055(12) .0028(12) -.0031(13) N5 .0398(16) .0391(15) .0394(15) .0017(13) .0106(12) -.0015(12) N6 .0380(17) .0390(17) .067(2) -.0002(14) .0043(16) .0057(15) C1 .0345(17) .0346(17) .0379(16) -.0038(13) .0072(14) -.0010(13) C2 .0424(19) .0405(18) .0363(17) -.0024(15) .0146(15) .0011(14) C3 .049(2) .051(2) .0344(17) -.0002(16) .0103(15) -.0004(15) C4 .047(2) .081(3) .058(2) .002(2) .0170(19) -.007(2) C5 .088(3) .044(2) .048(2) -.018(2) .023(2) .0007(17) C6 .073(3) .094(4) .065(3) -.010(3) .024(2) -.036(3) C7 .064(3) .085(3) .060(3) -.005(3) -.007(2) .022(2) C8 .0342(17) .0338(16) .0366(17) -.0017(14) .0063(13) -.0018(13) C9 .0366(19) .056(2) .050(2) -.0051(17) .0053(16) .0013(18) C10 .034(2) .058(2) .067(3) -.0100(18) .0097(18) -.006(2) C11 .044(2) .047(2) .058(2) -.0149(17) .0153(18) .0060(18) C12 .041(2) .044(2) .0427(19) -.0058(16) .0087(15) .0066(16) C13 .055(3) .063(3) .072(3) -.018(2) .011(2) -.030(2) C14 .061(3) .040(2) .086(3) -.0011(19) .025(2) -.016(2) C15 .042(2) .060(3) .071(3) -.0073(19) -.0140(19) .008(2) C16 .045(2) .070(3) .062(3) -.021(2) .0075(19) .009(2) C17 .083(3) .062(3) .054(2) -.008(2) .028(2) -.002(2) C18 .052(3) .066(3) .073(3) .024(2) .006(2) -.008(2) C19 .091(4) .093(4) .088(4) -.037(3) .016(3) -.010(3) 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 O1 . 2.014(2) yes Ni O3 . 2.129(2) yes Ni O4 . 2.125(2) yes Ni N3 . 2.134(3) yes Ni N4 . 2.154(3) yes Ni N5 . 2.100(3) yes Cl1 C19 . 1.761(6) no Cl2 C19 . 1.750(6) no P F2 . 1.512(4) no P F3 . 1.530(3) no P F5 . 1.567(4) no P F4 . 1.569(4) no P F6 . 1.570(3) no P F1 . 1.584(3) no O1 N1 . 1.296(3) yes O2 N2 . 1.276(4) yes O3 N6 . 1.283(4) yes O4 N6 . 1.265(4) yes O5 N6 . 1.211(4) yes N1 C1 . 1.330(4) no N1 C2 . 1.509(4) no N2 C1 . 1.351(4) no N2 C3 . 1.508(5) no N3 C12 . 1.337(4) no N3 C8 . 1.351(4) no N4 C16 . 1.478(5) no N4 C13 . 1.480(5) no N4 C15 . 1.488(5) no N5 C17 . 1.472(5) no N5 C18 . 1.479(5) no N5 C14 . 1.481(5) no C1 C8 . 1.452(4) no C2 C5 . 1.518(5) no C2 C4 . 1.526(5) no C2 C3 . 1.561(5) no C3 C6 . 1.518(5) no C3 C7 . 1.520(6) no C4 H4A . .9600 no C4 H4B . .9600 no C4 H4C . .9600 no C5 H5A . .9600 no C5 H5B . .9600 no C5 H5C . .9600 no C6 H6A . .9600 no C6 H6B . .9600 no C6 H6C . .9600 no C7 H7A . .9600 no C7 H7B . .9600 no C7 H7C . .9600 no C8 C9 . 1.392(5) no C9 C10 . 1.370(5) no C9 H9 . .9300 no C10 C11 . 1.364(5) no C10 H10 . .9300 no C11 C12 . 1.387(5) no C11 H11 . .9300 no C12 H12 . .9300 no C13 C14 . 1.490(6) no C13 H13A . .9700 no C13 H13B . .9700 no C14 H14A . .9700 no C14 H14B . .9700 no C15 H15A . .9600 no C15 H15B . .9600 no C15 H15C . .9600 no C16 H16A . .9600 no C16 H16B . .9600 no C16 H16C . .9600 no C17 H17A . .9600 no C17 H17B . .9600 no C17 H17C . .9600 no C18 H18A . .9600 no C18 H18B . .9600 no C18 H18C . .9600 no C19 H19A . .9700 no C19 H19B . .9700 no