#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/08/2200858.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_2200858 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2002 _journal_volume 58 _journal_page_first m74 _journal_page_last m76 _publ_section_title ; Further refinement of diaqua(1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane- N,N',N'',N''')nickel(II) dichloride ; _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 'Kuksa, Vladimir A.' 'Wardell, Solange M. S. V' 'Lin, Paul Kong Thoo' 'Howie, R. Alan' _chemical_formula_moiety 'C12 H32 N4 Ni O6 2+, 2Cl 1-' _chemical_formula_sum 'C12 H32 Cl2 N4 Ni O6' _chemical_formula_iupac '[Ni (C12 H28 N4 O4) (H2 O)2] Cl2' _chemical_formula_weight 458.03 _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 7.4288(3) _cell_length_b 13.1426(5) _cell_length_c 10.2527(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.2480(18) _cell_angle_gamma 90.00 _cell_volume 978.22(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.555 _diffrn_ambient_temperature 150(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 Ni1 .23391(3) .2500 .24285(2) .01320(10) Uani d S 1 . . Ni Cl1 .73803(4) .07626(3) .24487(3) .01941(11) Uani d . 1 . . Cl O1W .51256(19) .2500 .35069(15) .0182(3) Uani d S 1 . . O H1W .568(3) .2013(14) .3345(18) .036(5) Uiso d . 1 . . H O2W -.04151(19) .2500 .13598(14) .0180(3) Uani d S 1 . . O H2W -.096(3) .2002(14) .1564(18) .034(5) Uiso d . 1 . . H O1 .15440(12) .05709(8) .11108(10) .0204(2) Uani d . 1 . . O O2 .33653(13) .06625(8) .38171(10) .0206(2) Uani d . 1 . . O N1 .29493(16) .13413(9) .11811(12) .0170(2) Uani d . 1 . . N H1N .396(2) .1059(13) .1653(16) .022(4) Uiso d . 1 . . H N2 .17873(16) .13271(9) .36923(12) .0170(3) Uani d . 1 . . N H2N .085(2) .0976(13) .3214(15) .017(4) Uiso d . 1 . . H C1 .4252(3) .2500 -.0275(2) .0249(5) Uani d S 1 . . C H1A .5352 .2500 .0465 .030 Uiso calc SR 1 . . H H1B .4685 .2500 -.1124 .030 Uiso calc SR 1 . . H C2 .3158(2) .15393(13) -.01978(14) .0263(3) Uani d . 1 . . C H2A .1924 .1606 -.0790 .032 Uiso calc R 1 . . H H2B .3790 .0956 -.0515 .032 Uiso calc R 1 . . H C3 .2234(2) -.04547(11) .12978(15) .0230(3) Uani d . 1 . . C H3A .3583 -.0467 .1363 .028 Uiso calc PR .74 A 1 H H3B .1639 -.0892 .0542 .028 Uiso calc PR .74 A 1 H H3C .2953 -.0576 .0603 .028 Uiso calc PR .26 A 2 H H3D .1149 -.0909 .1087 .028 Uiso calc PR .26 A 2 H C4 .1765(3) -.08232(16) .2592(2) .0232(4) Uani d P .74 B 1 C H4A .0463 -.0650 .2575 .028 Uiso calc PR .74 B 1 H H4B .1871 -.1574 .2625 .028 Uiso calc PR .74 B 1 H C4A .3383(8) -.0822(4) .2574(6) .0224(12) Uani d P .26 B 2 C H4C .4685 -.0656 .2580 .027 Uiso calc PR .26 B 2 H H4D .3282 -.1573 .2596 .027 Uiso calc PR .26 B 2 H C5 .2923(2) -.04018(12) .38390(15) .0248(3) Uani d . 1 . . C H5A .2279 -.0520 .4577 .030 Uiso calc PR .74 C 1 H H5B .4091 -.0791 .4047 .030 Uiso calc PR .74 C 1 H H5C .1602 -.0500 .3839 .030 Uiso calc PR .26 C 2 H H5D .3671 -.0738 .4637 .030 Uiso calc PR .26 C 2 H C6 .1419(2) .15349(13) .50294(15) .0268(3) Uani d . 1 . . C H6A .1880 .0957 .5627 .032 Uiso calc PR .81 D 1 H H6B .0071 .1581 .4957 .032 Uiso calc PR .81 D 1 H H6C .0613 .0988 .5244 .032 Uiso calc PR .19 D 2 H H6D .2601 .1492 .5689 .032 Uiso calc PR .19 D 2 H C7 .2304(4) .2500 .5643(2) .0237(6) Uani d SP .81 . 1 C H7A .3612 .2500 .5570 .028 Uiso calc SPR .81 . 1 H H7B .2279 .2500 .6604 .028 Uiso calc SPR .81 . 1 H C7A .0573(15) .2500 .5204(10) .022(2) Uani d SP .19 . 2 C H7C .0343 .2500 .6121 .026 Uiso calc SPR .19 . 2 H H7D -.0649 .2500 .4589 .026 Uiso calc SPR .19 . 2 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 Ni1 .01242(14) .01446(15) .01340(15) .000 .00427(9) .000 Cl1 .01442(18) .0204(2) .0240(2) .00084(12) .00530(14) -.00023(13) O1W .0153(7) .0164(8) .0234(8) .000 .0051(6) .000 O2W .0149(7) .0172(8) .0218(8) .000 .0033(6) .000 O1 .0132(5) .0175(5) .0294(6) -.0017(4) .0021(4) -.0033(4) O2 .0135(5) .0183(5) .0275(6) .0021(4) -.0012(4) .0022(4) N1 .0125(5) .0202(6) .0185(6) -.0022(5) .0035(4) -.0031(5) N2 .0129(6) .0197(6) .0182(6) .0013(5) .0030(4) .0018(5) C1 .0225(11) .0354(13) .0189(10) .000 .0092(8) .000 C2 .0304(8) .0322(9) .0184(7) -.0031(7) .0096(6) -.0063(6) C3 .0238(7) .0179(7) .0272(8) .0018(6) .0047(6) -.0045(6) C4 .0225(10) .0163(10) .0294(11) -.0009(8) .0026(8) -.0002(8) C4A .019(3) .015(3) .035(3) -.002(2) .007(2) -.001(2) C5 .0288(8) .0175(8) .0277(8) .0018(6) .0048(6) .0051(6) C6 .0319(8) .0308(9) .0205(7) -.0014(7) .0120(6) .0048(7) C7 .0254(13) .0318(15) .0129(12) .000 .0021(10) .000 C7A .024(6) .031(6) .013(5) .000 .013(4) .000 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 Ni1 N1 . 2.0990(12) yes Ni1 O2W . 2.1061(14) yes Ni1 N2 . 2.1091(12) yes Ni1 O1W . 2.1299(14) yes O1W H1W 4_565 .796(18) ? O1W H1W . .796(18) ? O2W H2W 4_565 .820(18) ? O2W H2W . .820(18) ? O1 C3 . 1.4404(17) yes O1 N1 . 1.4451(14) yes O2 C5 . 1.4381(18) yes O2 N2 . 1.4457(14) yes N1 C2 . 1.4776(18) yes N1 H1N . .883(18) ? N2 C6 . 1.4792(18) yes N2 H2N . .890(17) ? C1 C2 . 1.5130(19) yes C1 H1A . .990 ? C1 H1B . .990 ? C2 H2A . .990 ? C2 H2B . .990 ? C3 C4A . 1.484(6) yes C3 C4 . 1.521(2) yes C3 H3A . .990 ? C3 H3B . .990 ? C3 H3C . .990 ? C3 H3D . .990 ? C4 C5 . 1.488(2) yes C4 H4A . .990 ? C4 H4B . .990 ? C4A C5 . 1.514(6) yes C4A H4C . .990 ? C4A H4D . .990 ? C5 H5A . .990 ? C5 H5B . .990 ? C5 H5C . .990 ? C5 H5D . .990 ? C6 C7A . 1.443(5) yes C6 C7 . 1.504(2) yes C6 H6A . .990 ? C6 H6B . .990 ? C6 H6C . .990 ? C6 H6D . .990 ? C7 H7A . .990 ? C7 H7B . .990 ? C7A H7C . .990 ? C7A H7D . .990 ? _cod_database_code 2200858