#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203612.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_2203612 loop_ _publ_author_name 'Zhu-Yan Zhang' 'Shan Gao' 'Li-Hua Huo' 'Hui Zhao' 'Jing-Gui Zhao' 'Ng, Seik Weng' _publ_section_title ; 'Hexaaquanickel(II) bis[(4-oxo-4H-pyridin-1-yl)acetate] dihydrate' ; _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m544 _journal_page_last m545 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Ni(H2 O)6] (C7 H6 N O3)2 , 2H2 O' _chemical_formula_moiety 'H12 Ni O6, 2(C7 H6 N O3), 2(H2 O)' _chemical_formula_sum 'C14 H28 N2 Ni O14' _chemical_formula_weight 507.07 _chemical_name_systematic ; 'Hexaaquanickel(II) bis[(4-oxo-4H-pyridin-1-yl)acetate] dihydrate' ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 98.42(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.387(3) _cell_length_b 12.816(3) _cell_length_c 6.7660(10) _cell_measurement_reflns_used 6398 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 3.6 _cell_volume 1062.6(4) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.016 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 10195 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.99 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Green _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 532 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.35 _refine_diff_density_min -0.77 _refine_ls_extinction_coef 0.370(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 2423 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.033 _refine_ls_R_factor_gt 0.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.2260P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.076 _refine_ls_wR_factor_ref 0.078 _reflns_number_gt 2237 _reflns_number_total 2423 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hg6034.cif _[local]_cod_cif_authors_sg_H-M 'P 21/c' _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. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' 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 ; _cod_database_code 2203612 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' 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_type_symbol Ni1 0.0000 0.5000 0.0000 0.02160(10) Uani d S 1 Ni O1 0.25666(8) 0.79125(8) 0.5949(2) 0.0325(2) Uani d . 1 O O2 0.10136(8) 0.69862(8) 0.5417(2) 0.0306(2) Uani d . 1 O O3 0.71588(9) 0.61907(9) 0.6729(2) 0.0400(3) Uani d . 1 O O1W -0.02773(9) 0.56660(9) 0.2646(2) 0.0361(3) Uani d D 1 O H1W1 -0.0878(9) 0.597(2) 0.269(3) 0.054 Uiso d D 1 H H1W2 0.0230(10) 0.600(2) 0.338(3) 0.054 Uiso d D 1 H O2W 0.16549(9) 0.51745(9) 0.0696(2) 0.0337(3) Uani d D 1 O H2W1 0.196(2) 0.5762(8) 0.086(3) 0.051 Uiso d D 1 H H2W2 0.204(2) 0.4720(10) 0.136(3) 0.051 Uiso d D 1 H O3W 0.01496(8) 0.35815(8) 0.1413(2) 0.0293(2) Uani d D 1 O H3W1 -0.008(2) 0.362(2) 0.253(2) 0.044 Uiso d D 1 H H3W2 -0.0210(10) 0.3110(10) 0.070(2) 0.044 Uiso d D 1 H O4W 0.21710(10) 0.16630(10) 0.1937(2) 0.0555(4) Uani d D 1 O H4W1 0.221(2) 0.155(2) 0.070(2) 0.083 Uiso d D 1 H H4W2 0.223(2) 0.2316(9) 0.214(4) 0.083 Uiso d D 1 H N1 0.38350(10) 0.61411(9) 0.6404(2) 0.0272(3) Uani d . 1 N C1 0.20360(10) 0.70860(10) 0.5826(2) 0.0234(3) Uani d . 1 C C2 0.26420(10) 0.60490(10) 0.6221(2) 0.0298(3) Uani d . 1 C H2A 0.2455 0.5749 0.7443 0.036 Uiso calc R 1 H H2B 0.2390 0.5572 0.5139 0.036 Uiso calc R 1 H C3 0.43010(10) 0.63180(10) 0.4744(2) 0.0314(3) Uani d . 1 C H3 0.3855 0.6415 0.3527 0.038 Uiso calc R 1 H C4 0.54010(10) 0.63570(10) 0.4808(2) 0.0318(3) Uani d . 1 C H4 0.5692 0.6482 0.3639 0.038 Uiso calc R 1 H C5 0.61210(10) 0.62080(10) 0.6643(2) 0.0290(3) Uani d . 1 C C6 0.55940(10) 0.60800(10) 0.8362(2) 0.0346(3) Uani d . 1 C H6 0.6013 0.6016 0.9615 0.041 Uiso calc R 1 H C7 0.44860(10) 0.60480(10) 0.8195(2) 0.0333(3) Uani d . 1 C H7 0.4164 0.5960 0.9342 0.040 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 Ni1 0.0204(2) 0.0195(2) 0.0243(2) -0.00179(7) 0.00113(9) -0.00067(7) O1 0.0278(5) 0.0235(5) 0.0446(6) 0.0010(4) -0.0003(4) -0.0021(4) O2 0.0229(5) 0.0306(5) 0.0376(6) 0.0022(4) 0.0020(4) 0.0008(4) O3 0.0250(5) 0.0441(6) 0.0499(7) 0.0040(4) 0.0018(5) 0.0085(5) O1W 0.0319(6) 0.0420(6) 0.0337(6) 0.0013(5) 0.0028(4) -0.0134(5) O2W 0.0233(5) 0.0260(5) 0.0487(7) -0.0036(4) -0.0050(5) 0.0063(4) O3W 0.0317(5) 0.0250(5) 0.0312(5) -0.0031(4) 0.0043(4) 0.0017(4) O4W 0.0575(8) 0.0474(8) 0.0682(9) -0.0129(6) 0.0312(7) -0.0079(6) N1 0.0253(6) 0.0242(6) 0.0322(6) 0.0059(4) 0.0040(5) 0.0032(4) C1 0.0248(6) 0.0240(6) 0.0213(6) 0.0035(5) 0.0032(5) -0.0007(4) C2 0.0257(7) 0.0234(6) 0.0406(8) 0.0024(5) 0.0062(6) 0.0024(5) C3 0.0313(7) 0.0330(7) 0.0289(7) 0.0049(6) 0.0010(6) 0.0063(5) C4 0.0307(7) 0.0338(7) 0.0313(7) 0.0038(6) 0.0056(6) 0.0073(6) C5 0.0271(7) 0.0218(6) 0.0373(8) 0.0027(5) 0.0020(6) 0.0021(5) C6 0.0346(8) 0.0398(8) 0.0275(7) 0.0049(6) -0.0016(6) 0.0004(6) C7 0.0361(8) 0.0364(7) 0.0279(7) 0.0070(6) 0.0066(6) 0.0018(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 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 O2W Ni1 O2W . 3_565 180.00(2) no O2W Ni1 O3W . . 88.31(4) yes O2W Ni1 O3W 3_565 . 91.69(4) no O2W Ni1 O3W . 3_565 91.69(4) yes O2W Ni1 O3W 3_565 3_565 88.31(4) no O3W Ni1 O3W . 3_565 180.00(3) no O2W Ni1 O1W . 3_565 87.50(6) yes O2W Ni1 O1W 3_565 3_565 92.50(5) no O3W Ni1 O1W . 3_565 91.29(5) yes O3W Ni1 O1W 3_565 3_565 88.71(5) no O2W Ni1 O1W . . 92.50(6) yes O2W Ni1 O1W 3_565 . 87.50(6) no O3W Ni1 O1W . . 88.71(5) yes O3W Ni1 O1W 3_565 . 91.29(5) no O1W Ni1 O1W 3_565 . 180.00(6) no Ni1 O1W H1W1 . . 118.0(10) no Ni1 O1W H1W2 . . 121.0(10) no H1W1 O1W H1W2 . . 109.0(10) no Ni1 O2W H2W1 . . 123.0(10) no Ni1 O2W H2W2 . . 121.0(10) no H2W1 O2W H2W2 . . 110.0(10) no Ni1 O3W H3W1 . . 111.0(10) no Ni1 O3W H3W2 . . 111.0(10) no H3W1 O3W H3W2 . . 109.0(10) no H4W1 O4W H4W2 . . 108(2) no C3 N1 C7 . . 119.00(10) no C3 N1 C2 . . 119.20(10) no C7 N1 C2 . . 121.70(10) no O1 C1 O2 . . 127.20(10) no O1 C1 C2 . . 119.20(10) no O2 C1 C2 . . 113.60(10) no N1 C2 C1 . . 114.00(10) yes N1 C2 H2A . . 108.8 no C1 C2 H2A . . 108.8 no N1 C2 H2B . . 108.8 no C1 C2 H2B . . 108.8 no H2A C2 H2B . . 107.6 no N1 C3 C4 . . 121.80(10) no N1 C3 H3 . . 119.1 no C4 C3 H3 . . 119.1 no C3 C4 C5 . . 121.20(10) no C3 C4 H4 . . 119.4 no C5 C4 H4 . . 119.4 no O3 C5 C6 . . 122.60(10) no O3 C5 C4 . . 122.50(10) no C6 C5 C4 . . 115.00(10) no C7 C6 C5 . . 120.80(10) no C7 C6 H6 . . 119.6 no C5 C6 H6 . . 119.6 no N1 C7 C6 . . 122.10(10) no N1 C7 H7 . . 119.0 no C6 C7 H7 . . 119.0 no 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 O2W . 2.0470(10) yes Ni1 O2W 3_565 2.0470(10) no Ni1 O3W . 2.0500(10) yes Ni1 O3W 3_565 2.0500(10) no Ni1 O1W 3_565 2.0570(10) no Ni1 O1W . 2.0570(10) yes O1 C1 . 1.243(2) yes O2 C1 . 1.263(2) yes O3 C5 . 1.278(2) yes O1W H1W1 . 0.841(9) no O1W H1W2 . 0.856(19) no O2W H2W1 . 0.843(9) no O2W H2W2 . 0.840(19) no O3W H3W1 . 0.847(9) no O3W H3W2 . 0.850(9) no O4W H4W1 . 0.857(9) no O4W H4W2 . 0.850(9) no N1 C3 . 1.355(2) no N1 C7 . 1.358(2) no N1 C2 . 1.470(2) no C1 C2 . 1.530(2) no C2 H2A . 0.9700 no C2 H2B . 0.9700 no C3 C4 . 1.358(2) yes C3 H3 . 0.9300 no C4 C5 . 1.431(2) no C4 H4 . 0.9300 no C5 C6 . 1.425(2) no C6 C7 . 1.362(2) yes C6 H6 . 0.9300 no C7 H7 . 0.9300 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 O1W H1W2 O2 . 0.856(19) 2.020(10) 2.839(2) 162(2) yes O1W H1W1 O4W 2 0.841(9) 1.880(10) 2.722(2) 174(2) yes O2W H2W1 O1 4_575 0.843(9) 1.854(9) 2.694(2) 174(2) yes O2W H2W2 O3 3_666 0.840(19) 1.900(10) 2.739(2) 170(2) yes O3W H3W1 O2 3_566 0.847(9) 2.080(10) 2.848(2) 150(2) yes O3W H3W2 O2 2_545 0.850(9) 1.860(10) 2.696(2) 170(2) yes O4W H4W1 O3 2_645 0.857(9) 1.980(10) 2.795(2) 159(3) yes O4W H4W2 O3 3_666 0.850(9) 2.160(10) 2.975(2) 162(3) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag C3 N1 C2 C1 -73.2(2) no C7 N1 C2 C1 107.2(2) no O1 C1 C2 N1 -9.2(2) no O2 C1 C2 N1 171.40(10) no C7 N1 C3 C4 3.1(2) no C2 N1 C3 C4 -176.60(10) no N1 C3 C4 C5 0.2(2) no C3 C4 C5 O3 176.60(10) no C3 C4 C5 C6 -3.4(2) no O3 C5 C6 C7 -176.60(10) no C4 C5 C6 C7 3.4(2) no C3 N1 C7 C6 -3.1(2) no C2 N1 C7 C6 176.60(10) no C5 C6 C7 N1 -0.3(2) no