#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/00/2200077.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200077 loop_ _publ_author_name 'Batten, Stuart R.' 'Harris, Alexander R.' _publ_section_title ; trans-Tetraaquabis(pyridine-3-carboxylate-\kN)nickel(II) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m9 _journal_page_last m11 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ni (C6 H4 N O2)2 (H2 O)4]' _chemical_formula_moiety 'C12 H16 N2 Ni O8' _chemical_formula_sum 'C12 H16 N2 Ni O8' _chemical_formula_weight 374.98 _chemical_name_common ; trans-Bis(pyridine-3-carboxylate)tetraaquonickel(II) ; _chemical_name_systematic ; trans-Bis(pyridine-3-carboxylate)tetraaquonickel(II) ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _cell_angle_alpha 90.00 _cell_angle_beta 118.137(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 14.0549(7) _cell_length_b 6.8170(2) _cell_length_c 8.4359(4) _cell_measurement_reflns_used 5663 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.83 _cell_measurement_theta_min 2.74 _cell_volume 712.74(5) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0504 _diffrn_reflns_av_sigmaI/netI .0397 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 5664 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.83 _diffrn_reflns_theta_min 2.74 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type none _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 388 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .025 _refine_diff_density_max .373 _refine_diff_density_min -.341 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 916 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all .040 _refine_ls_R_factor_gt .032 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0108P)^2^+1.0314P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .058 _reflns_number_gt 843 _reflns_number_total 916 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6008.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/m' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200077 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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 .0000 .0000 .5000 .01259(14) Uani d S 1 . . Ni O1 .05577(10) .2183(2) .39281(17) .0189(3) Uani d . 1 . . O H1A .096(2) .161(4) .341(3) .051(8) Uiso d . 1 . . H H1B .096(2) .297(4) .468(4) .045(8) Uiso d . 1 . . H N1 .14602(16) .0000 .7405(3) .0145(4) Uani d S 1 . . N C2 .1462(2) .0000 .8993(3) .0150(5) Uani d S 1 . . C H2A .0787 .0000 .8996 .018 Uiso calc SR 1 . . H C3 .2395(2) .0000 1.0634(3) .0146(5) Uani d S 1 . . C C4 .3381(2) .0000 1.0642(3) .0188(5) Uani d S 1 . . C H4A .4035 .0000 1.1742 .023 Uiso calc SR 1 . . H C5 .3393(2) .0000 .9000(3) .0206(6) Uani d S 1 . . C H5A .4058 .0000 .8963 .025 Uiso calc SR 1 . . H C6 .2428(2) .0000 .7429(3) .0176(5) Uani d S 1 . . C H6A .2445 .0000 .6316 .021 Uiso calc SR 1 . . H C7 .2301(2) .0000 1.2347(3) .0180(5) Uani d S 1 . . C O2 .13636(16) .0000 1.2175(2) .0263(4) Uani d S 1 . . O O3 .31551(15) .0000 1.3817(2) .0234(4) Uani d S 1 . . O 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 .0109(2) .0136(2) .0092(2) .000 .00141(18) .000 O1 .0185(7) .0198(7) .0153(7) -.0041(5) .0055(6) -.0011(5) N1 .0149(11) .0140(10) .0117(10) .000 .0038(8) .000 C2 .0142(12) .0139(12) .0145(12) .000 .0049(10) .000 C3 .0183(13) .0082(11) .0130(12) .000 .0039(10) .000 C4 .0145(13) .0176(12) .0163(12) .000 .0007(10) .000 C5 .0127(13) .0252(14) .0220(14) .000 .0067(11) .000 C6 .0165(13) .0194(12) .0159(12) .000 .0068(11) .000 C7 .0253(15) .0111(11) .0138(12) .000 .0060(11) .000 O2 .0265(11) .0341(11) .0203(10) .000 .0127(9) .000 O3 .0277(11) .0196(9) .0119(9) .000 .0003(8) .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 O1 6 2.0775(12) no Ni1 O1 2_556 2.0775(12) no Ni1 O1 5_556 2.0775(13) no Ni1 O1 . 2.0775(12) yes Ni1 N1 . 2.098(2) yes Ni1 N1 5_556 2.098(2) no O1 H1A . .95(3) no O1 H1B . .82(3) no N1 C2 . 1.339(3) no N1 C6 . 1.351(3) no C2 C3 . 1.387(3) no C3 C4 . 1.382(4) no C3 C7 . 1.512(3) no C4 C5 . 1.394(4) no C5 C6 . 1.378(4) no C7 O3 . 1.255(3) no C7 O2 . 1.256(3) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Ni1 O1 6 2_556 180.0(8) no O1 Ni1 O1 6 5_556 88.48(8) no O1 Ni1 O1 2_556 5_556 91.52(8) no O1 Ni1 N1 . . 91.32(5) yes O1 Ni1 O1 . 6 91.52(8) yes O1 Ni1 O1 2_556 . 88.48(8) no O1 Ni1 O1 5_556 . 180.00(6) no O1 Ni1 N1 6 . 91.32(5) no O1 Ni1 N1 2_556 . 88.68(5) no O1 Ni1 N1 5_556 . 88.68(5) no O1 Ni1 N1 6 5_556 88.68(5) no O1 Ni1 N1 2_556 5_556 91.32(5) no O1 Ni1 N1 5_556 5_556 91.32(5) no O1 Ni1 N1 . 5_556 88.68(5) no N1 Ni1 N1 . 5_556 180.0 no Ni1 O1 H1A . . 109.7(16) no Ni1 O1 H1B . . 113.4(18) no H1A O1 H1B . . 106(2) no C2 N1 C6 . . 117.3(2) no C2 N1 Ni1 . . 120.46(17) no C6 N1 Ni1 . . 122.25(16) no N1 C2 C3 . . 123.6(2) no C4 C3 C2 . . 118.6(2) no C4 C3 C7 . . 122.3(2) no C2 C3 C7 . . 119.1(2) no C3 C4 C5 . . 118.5(2) no C6 C5 C4 . . 119.2(2) no N1 C6 C5 . . 122.8(2) no O3 C7 O2 . . 125.2(2) no O3 C7 C3 . . 118.0(2) no O2 C7 C3 . . 116.7(2) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1A O2 1_554 .95(3) 1.77(3) 2.696(2) 161(2) yes O1 H1B O3 7_557 .82(3) 1.89(3) 2.708(2) 173(3) yes _cod_database_fobs_code 2200077 _journal_paper_doi 10.1107/S1600536800018742