#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4300969.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_4300969 _journal_name_full 'Inorganic Chemistry' _journal_year 2005 loop_ _publ_author_name 'Mohamedally Kurmoo 'Claude Estournes' 'Yoshimi Oka' 'Kumagai, Hitoshi' 'Katsuya Inoue _chemical_formula_sum 'C16 H16 N2 O6 Ni ' _chemical_formula_moiety 'C16 H16 N2 O6 Ni ' _chemical_formula_weight 391.01 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 16.812(3) _cell_length_b 5.443(1) _cell_length_c 17.869(4) _cell_angle_alpha 90 _cell_angle_beta 106.229(3) _cell_angle_gamma 90 _cell_volume 1569.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 _exptl_crystal_density_diffrn 1.654 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 1.5000 -0.5000 1.5000 0.0217(3) Uani 1.00 d S . . Ni(2) Ni 1.0000 0.0000 1.0000 0.0202(3) Uani 1.00 d S . . O(1) O 1.1609(3) 0.0612(8) 1.1535(3) 0.038(1) Uani 1.00 d . . . O(2) O 1.0957(2) -0.2083(7) 1.0636(2) 0.027(1) Uani 1.00 d . . . O(3) O 1.6828(3) -0.4874(9) 1.4572(3) 0.044(1) Uani 1.00 d . . . O(4) O 1.6006(2) -0.7305(7) 1.5043(2) 0.026(1) Uani 1.00 d . . . O(6) O 1.0392(2) 0.3092(7) 1.0697(2) 0.028(1) Uani 1.00 d . . . O(7) O 1.5570(2) -0.2117(7) 1.4622(2) 0.029(1) Uani 1.00 d . . . N(1) N 1.4439(3) -0.5851(9) 1.3784(3) 0.027(1) Uani 1.00 d . . . N(2) N 1.0683(3) 0.1024(9) 0.9220(3) 0.027(1) Uani 1.00 d . . . C(1) C 1.3834(5) -0.436(1) 1.3361(3) 0.030(2) Uani 1.00 d . . . C(2) C 1.3388(4) -0.476(1) 1.2581(3) 0.028(2) Uani 1.00 d . . . C(3) C 1.3603(5) -0.682(1) 1.2224(4) 0.033(2) Uani 1.00 d . . . C(4) C 1.4227(4) -0.834(1) 1.2644(3) 0.035(2) Uani 1.00 d . . . C(5) C 1.4633(4) -0.780(1) 1.3424(4) 0.034(2) Uani 1.00 d . . . C(6) C 1.2726(5) -0.303(1) 1.2204(3) 0.032(2) Uani 1.00 d . . . C(7) C 1.2126(5) -0.335(1) 1.1555(3) 0.032(2) Uani 1.00 d . . . C(8) C 1.1522(4) -0.144(1) 1.1222(3) 0.025(2) Uani 1.00 d . . . C(9) C 1.1338(4) 0.243(1) 0.9442(3) 0.028(2) Uani 1.00 d . . . C(10) C 1.1811(5) 0.316(1) 0.8963(4) 0.032(2) Uani 1.00 d . . . C(11) C 1.1585(5) 0.228(1) 0.8206(4) 0.040(2) Uani 1.00 d . . . C(12) C 1.0905(5) 0.085(1) 0.7963(4) 0.045(2) Uani 1.00 d . . . C(13) C 1.0470(4) 0.030(1) 0.8476(4) 0.036(2) Uani 1.00 d . . . C(14) C 1.2510(5) 0.477(1) 0.9245(4) 0.039(2) Uani 1.00 d . . . C(15) C 1.2563(5) 0.662(1) 0.9773(4) 0.033(2) Uani 1.00 d . . . C(16) C 1.6723(5) -0.672(1) 1.4923(4) 0.031(2) Uani 1.00 d . . . H(1) H 1.3655 -0.3017 1.3708 0.0253 Uiso 1.00 calc . . . H(2) H 1.3208 -0.7512 1.1779 0.0253 Uiso 1.00 calc . . . H(3) H 1.4265 -0.9715 1.2243 0.0253 Uiso 1.00 calc . . . H(4) H 1.5156 -0.9263 1.3595 0.0253 Uiso 1.00 calc . . . H(5) H 1.2808 -0.1489 1.2536 0.0253 Uiso 1.00 calc . . . H(6) H 1.2260 -0.4354 1.1374 0.0253 Uiso 1.00 calc . . . H(7) H 1.1515 0.2903 0.9974 0.0253 Uiso 1.00 calc . . . H(8) H 1.1881 0.2681 0.7827 0.0253 Uiso 1.00 calc . . . H(9) H 1.0709 -0.0309 0.7457 0.0253 Uiso 1.00 calc . . . H(10) H 0.9923 -0.0654 0.8201 0.0253 Uiso 1.00 calc . . . H(11) H 1.3003 0.4543 0.9062 0.0427 Uiso 1.00 calc . . . H(12) H 1.2102 0.6842 0.9952 0.0253 Uiso 1.00 calc . . . H(13) H 1.0560 0.5069 1.0568 0.0253 Uiso 1.00 calc . . . H(14) H 1.0914 0.2939 1.0979 0.0253 Uiso 1.00 calc . . . H(15) H 1.6134 -0.2644 1.4551 0.0253 Uiso 1.00 calc . . . H(16) H 1.5922 -0.1059 1.4997 0.0342 Uiso 1.00 calc . . . H(20) H 1.2550 0.5333 0.9410 0.0367 Uiso 1.00 calc . . . 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(1) 0.0205(5) 0.0184(5) 0.0229(5) 0.0035(5) 0.0005(4) 0.0021(5) Ni(2) 0.0174(5) 0.0184(5) 0.0216(5) -0.0015(5) 0.0001(4) 0.0019(5) O(1) 0.033(2) 0.030(3) 0.037(3) 0.006(2) -0.011(2) -0.005(2) O(2) 0.023(2) 0.021(2) 0.029(2) 0.002(2) -0.004(2) 0.002(2) O(3) 0.045(3) 0.031(3) 0.061(3) 0.010(2) 0.024(2) 0.015(3) O(4) 0.026(2) 0.020(2) 0.029(2) 0.006(2) 0.003(2) 0.000(2) O(6) 0.028(2) 0.023(2) 0.029(2) -0.004(2) 0.000(2) 0.000(2) O(7) 0.030(2) 0.022(2) 0.034(2) -0.002(2) 0.005(2) 0.003(2) N(1) 0.027(3) 0.026(3) 0.024(2) 0.003(2) -0.002(2) 0.000(2) N(2) 0.023(2) 0.026(3) 0.030(3) -0.005(2) 0.006(2) 0.001(2) C(1) 0.038(3) 0.027(3) 0.022(3) 0.006(3) 0.001(3) 0.003(3) C(2) 0.031(3) 0.029(3) 0.022(3) -0.003(3) 0.004(2) -0.002(3) C(3) 0.036(3) 0.030(3) 0.030(3) 0.001(3) 0.004(3) -0.006(3) C(4) 0.039(4) 0.034(4) 0.026(3) 0.008(3) 0.000(3) -0.010(3) C(5) 0.036(3) 0.027(4) 0.035(3) 0.008(3) 0.002(3) 0.008(3) C(6) 0.040(4) 0.026(3) 0.027(3) 0.007(3) 0.003(3) 0.003(3) C(7) 0.038(4) 0.031(3) 0.023(3) 0.001(3) 0.003(3) -0.003(3) C(8) 0.026(3) 0.024(3) 0.027(3) 0.002(3) 0.008(3) 0.006(3) C(9) 0.028(3) 0.030(3) 0.025(3) -0.004(3) 0.004(3) 0.002(3) C(10) 0.032(3) 0.029(3) 0.035(3) -0.010(3) 0.012(3) 0.003(3) C(11) 0.044(4) 0.049(4) 0.032(3) -0.009(4) 0.019(3) -0.001(3) C(12) 0.040(4) 0.056(5) 0.038(4) -0.024(4) 0.009(3) -0.020(4) C(13) 0.029(3) 0.045(4) 0.030(3) -0.017(3) 0.000(3) -0.007(3) C(14) 0.041(4) 0.043(4) 0.038(3) 0.005(4) 0.020(3) -0.001(3) C(15) 0.033(3) 0.028(3) 0.042(4) -0.007(3) 0.018(3) -0.009(3) C(16) 0.036(4) 0.031(4) 0.029(3) 0.003(3) 0.014(3) -0.006(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) O(4) 2.090(4) . . yes Ni(1) O(4) 2.090(4) . 3_848 yes Ni(1) O(7) 2.049(4) . . yes Ni(1) O(7) 2.049(4) . 3_848 yes Ni(1) N(1) 2.163(5) . . yes Ni(1) N(1) 2.163(5) . 3_848 yes Ni(1) H(1) 2.948 . . no Ni(1) H(1) 2.948 . 3_848 no Ni(1) H(15) 2.603 . . no Ni(1) H(15) 2.603 . 3_848 no Ni(1) H(16) 2.647 . . no Ni(1) H(16) 2.647 . 3_848 no Ni(2) O(2) 2.036(4) . . yes Ni(2) O(2) 2.036(4) . 3_757 yes Ni(2) O(6) 2.087(4) . . yes Ni(2) O(6) 2.087(4) . 3_757 yes Ni(2) N(2) 2.113(5) . . yes Ni(2) N(2) 2.113(5) . 3_757 yes Ni(2) C(8) 2.967(7) . . yes Ni(2) C(8) 2.967(7) . 3_757 yes Ni(2) H(13) 2.999 . . no Ni(2) H(13) 2.930 . 1_545 no Ni(2) H(13) 2.999 . 3_757 no Ni(2) H(13) 2.930 . 3_767 no Ni(2) H(14) 2.545 . . no Ni(2) H(14) 2.545 . 3_757 no O(1) O(2) 2.225(6) . . yes O(1) O(6) 2.557(7) . . yes O(1) C(6) 2.763(9) . . yes O(1) C(7) 2.320(9) . . yes O(1) C(8) 1.239(8) . . yes O(1) H(2) 2.793 . 1_565 no O(1) H(5) 2.560 . . no O(1) H(6) 2.960 . . no O(1) H(6) 2.994 . 1_565 no O(1) H(8) 2.411 . 4_555 no O(1) H(10) 2.746 . 3_757 no O(1) H(14) 1.819 . . no O(2) O(6) 2.984(6) . . yes O(2) O(6) 2.805(6) . 1_545 yes O(2) O(6) 2.846(6) . 3_757 yes O(2) N(2) 2.970(7) . . yes O(2) N(2) 2.898(7) . 3_757 yes O(2) C(7) 2.286(9) . . yes O(2) C(8) 1.251(8) . . yes O(2) H(6) 2.539 . . no O(2) H(12) 2.618 . 1_545 no O(2) H(13) 1.679 . 1_545 no O(2) H(14) 2.807 . . no O(2) H(14) 2.783 . 1_545 no O(3) O(4) 2.240(7) . . yes O(3) O(7) 2.615(7) . . yes O(3) C(15) 2.320(9) . 2_837 yes O(3) C(16) 1.221(8) . . yes O(3) H(2) 2.721 . 2_857 no O(3) H(12) 2.510 . 2_837 no O(3) H(15) 1.677 . . no O(3) H(16) 2.803 . . no O(4) O(7) 2.961(6) . . yes O(4) O(7) 2.767(6) . 1_545 yes O(4) O(7) 2.893(6) . 3_848 yes O(4) N(1) 2.963(7) . 3_848 yes O(4) C(1) 2.932(8) . 3_848 yes O(4) C(14) 2.93(1) . 2_837 yes O(4) C(15) 2.406(10) . 2_837 yes O(4) C(16) 1.322(8) . . yes O(4) H(1) 2.150 . 3_848 no O(4) H(4) 2.795 . . no O(4) H(11) 2.605 . 2_837 no O(4) H(15) 2.713 . . no O(4) H(16) 2.048 . 1_545 no O(4) H(20) 2.678 . 2_837 no O(6) N(2) 2.908(7) . 3_757 yes O(6) C(13) 2.981(8) . 3_757 yes O(6) H(7) 2.570 . . no O(6) H(10) 2.550 . 3_757 no O(6) H(13) 1.152 . . no O(6) H(13) 2.579 . 3_767 no O(6) H(14) 0.885 . . no O(7) N(1) 2.897(7) . . yes O(7) H(4) 2.356 . 1_565 no O(7) H(11) 2.992 . 2_847 no O(7) H(15) 1.032 . . no O(7) H(16) 0.954 . . no N(1) C(1) 1.353(8) . . yes N(1) C(2) 2.444(8) . . yes N(1) C(3) 2.799(8) . . yes N(1) C(4) 2.390(8) . . yes N(1) C(5) 1.327(8) . . yes N(1) H(1) 2.009 . . no N(1) H(4) 2.290 . . no N(1) H(16) 2.946 . 3_848 no N(2) C(9) 1.309(8) . . yes N(2) C(10) 2.377(9) . . yes N(2) C(11) 2.756(9) . . yes N(2) C(12) 2.380(9) . . yes N(2) C(13) 1.338(8) . . yes N(2) H(7) 1.940 . . no N(2) H(10) 2.118 . . no C(1) C(2) 1.402(9) . . yes C(1) C(3) 2.372(9) . . yes C(1) C(4) 2.691(10) . . yes C(1) C(5) 2.286(10) . . yes C(1) C(6) 2.474(10) . . yes C(1) H(1) 1.056 . . no C(1) H(5) 2.486 . . no C(2) C(3) 1.389(9) . . yes C(2) C(4) 2.392(10) . . yes C(2) C(5) 2.762(10) . . yes C(2) C(6) 1.47(1) . . yes C(2) C(7) 2.51(1) . . yes C(2) H(1) 2.155 . . no C(2) H(2) 2.038 . . no C(2) H(5) 2.019 . . no C(2) H(6) 2.452 . . no C(3) C(4) 1.382(10) . . yes C(3) C(5) 2.41(1) . . yes C(3) C(6) 2.53(1) . . yes C(3) H(2) 0.959 . . no C(3) H(3) 1.924 . . no C(3) H(5) 2.995 . 1_545 no C(3) H(6) 2.699 . . no C(4) C(5) 1.401(9) . . yes C(4) H(2) 2.011 . . no C(4) H(3) 1.049 . . no C(4) H(4) 2.024 . . no C(4) H(5) 2.899 . 1_545 no C(5) H(3) 2.279 . . no C(5) H(3) 2.984 . 2_857 no C(5) H(4) 1.163 . . no C(6) C(7) 1.318(10) . . yes C(6) C(8) 2.44(1) . . yes C(6) H(1) 2.705 . . no C(6) H(2) 2.742 . . no C(6) H(5) 1.015 . . no C(6) H(6) 1.637 . . no C(7) C(8) 1.46(1) . . yes C(7) H(2) 2.864 . . no C(7) H(5) 2.070 . . no C(7) H(6) 0.705 . . no C(7) H(12) 2.855 . 1_545 no C(7) H(13) 2.862 . 1_545 no C(7) H(14) 2.851 . 1_545 no C(8) H(5) 2.711 . . no C(8) H(6) 1.985 . . no C(8) H(12) 2.866 . 1_545 no C(8) H(13) 2.557 . 1_545 no C(8) H(14) 2.581 . . no C(9) C(10) 1.379(9) . . yes C(9) C(11) 2.360(9) . . yes C(9) C(12) 2.679(9) . . yes C(9) C(13) 2.248(9) . . yes C(9) C(14) 2.45(1) . . yes C(9) H(7) 0.949 . . no C(9) H(12) 2.753 . . no C(9) H(20) 2.589 . . no C(10) C(11) 1.385(10) . . yes C(10) C(12) 2.36(1) . . yes C(10) C(13) 2.68(1) . . yes C(10) C(14) 1.44(1) . . yes C(10) C(15) 2.49(1) . . yes C(10) H(7) 2.009 . . no C(10) H(8) 2.082 . . no C(10) H(11) 2.100 . . no C(10) H(12) 2.626 . . no C(10) H(20) 1.739 . . no C(11) C(12) 1.35(1) . . yes C(11) C(13) 2.33(1) . . yes C(11) C(14) 2.47(1) . . yes C(11) H(8) 0.970 . . no C(11) H(9) 2.201 . . no C(11) H(11) 2.738 . . no C(11) H(20) 2.841 . . no C(12) C(13) 1.36(1) . . yes C(12) H(8) 1.992 . . no C(12) H(9) 1.076 . . no C(12) H(10) 1.992 . . no C(12) H(10) 2.876 . 2_756 no C(13) H(9) 1.998 . . no C(13) H(10) 1.050 . . no C(14) C(15) 1.366(9) . . yes C(14) C(16) 2.54(1) . 2_867 yes C(14) H(1) 2.963 . 4_554 no C(14) H(7) 2.597 . . no C(14) H(8) 2.709 . . no C(14) H(11) 0.979 . . no C(14) H(12) 1.955 . . no C(14) H(15) 2.967 . 2_857 no C(14) H(16) 2.643 . 2_857 no C(14) H(20) 0.417 . . no C(15) C(16) 1.48(1) . 2_867 yes C(15) H(7) 2.773 . . no C(15) H(11) 1.991 . . no C(15) H(12) 0.926 . . no C(15) H(16) 2.864 . 2_857 no C(15) H(20) 0.951 . . no C(16) H(1) 2.699 . 3_848 no C(16) H(11) 2.679 . 2_837 no C(16) H(12) 2.078 . 2_837 no C(16) H(15) 2.443 . . no C(16) H(16) 2.742 . 1_545 no C(16) H(20) 2.163 . 2_837 no