#------------------------------------------------------------------------------ #$Date: 2011-01-02 20:00:31 +0000 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203571.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_2203571 loop_ _publ_author_name 'Shan Gao' 'Li-Hua Huo' 'Zhu-Yan Zhang' 'Li-Li Kong' 'Jing-Gui Zhao' _publ_section_title ; Tetraaquabis[(2-oxo-1,2-dihydropyridin-1-yl)acetato]magnesium(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m679 _journal_page_last m681 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Mg (C7 H6 N O3)2 (H2 O)4]' _chemical_formula_moiety 'C14 H20 Mg N2 O10' _chemical_formula_sum 'C14 H20 Mg N2 O10' _chemical_formula_weight 400.63 _chemical_name_systematic ; Tetraaquabis[(2-oxo-1,2-dihydropyridin-1-yl)acetato]magnesium(II) ; _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 113.70(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 10.550(2) _cell_length_b 7.0990(10) _cell_length_c 13.056(3) _cell_measurement_reflns_used 5735 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 3.3 _cell_volume 895.3(4) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC & Rigaku, 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 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scan' _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 0.029 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8176 _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 0.157 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_correction_T_min 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 420 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.35 _refine_diff_density_min -0.27 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2054 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.048 _refine_ls_R_factor_gt 0.043 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.2876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.12 _refine_ls_wR_factor_ref 0.120 _reflns_number_gt 1839 _reflns_number_total 2054 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file ci6369.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. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2203571 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 Mg1 0.0000 0.0000 0.5000 0.0283(2) Uani d S 1 Mg O1 -0.08580(10) 0.5007(2) 0.64772(9) 0.0400(3) Uani d . 1 O O2 -0.25520(10) 0.5467(2) 0.47913(9) 0.0393(3) Uani d . 1 O O3 -0.18480(10) 0.0986(2) 0.49040(10) 0.0534(4) Uani d . 1 O O1W -0.0222(2) 0.1439(2) 0.35680(10) 0.0562(4) Uani d D 1 O O2W -0.09410(10) -0.2399(2) 0.40636(9) 0.0359(3) Uani d D 1 O N1 -0.37970(10) 0.2160(2) 0.49440(10) 0.0313(3) Uani d . 1 N C1 -0.3133(2) 0.1091(2) 0.44290(10) 0.0353(3) Uani d . 1 C C2 -0.3995(2) 0.0214(3) 0.3404(2) 0.0456(4) Uani d . 1 C C3 -0.5392(2) 0.0442(3) 0.2976(2) 0.0528(5) Uani d . 1 C C4 -0.6016(2) 0.1527(3) 0.3544(2) 0.0501(5) Uani d . 1 C C5 -0.5201(2) 0.2352(2) 0.4519(2) 0.0398(4) Uani d . 1 C C6 -0.2900(2) 0.3130(2) 0.59610(10) 0.0364(3) Uani d . 1 C C7 -0.2030(2) 0.4663(2) 0.57080(10) 0.0312(3) Uani d . 1 C H2 -0.3598 -0.0523 0.3023 0.055 Uiso calc R 1 H H3 -0.5940 -0.0127 0.2301 0.063 Uiso calc R 1 H H4 -0.6972 0.1675 0.3254 0.060 Uiso calc R 1 H H5 -0.5604 0.3062 0.4907 0.048 Uiso calc R 1 H H1W1 0.016(3) 0.251(2) 0.359(2) 0.084 Uiso d D 1 H H1W2 -0.039(3) 0.093(3) 0.2930(10) 0.084 Uiso d D 1 H H2W1 -0.042(2) -0.314(2) 0.390(2) 0.054 Uiso d D 1 H H2W2 -0.146(2) -0.304(3) 0.430(2) 0.054 Uiso d D 1 H H6A -0.2287 0.2225 0.6483 0.044 Uiso calc R 1 H H6B -0.3461 0.3705 0.6311 0.044 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 Mg1 0.0280(3) 0.0269(3) 0.0302(3) 0.0002(2) 0.0119(3) -0.0014(2) O1 0.0443(6) 0.0347(6) 0.0348(6) -0.0063(4) 0.0095(5) 0.0005(4) O2 0.0382(6) 0.0396(6) 0.0382(6) -0.0012(4) 0.0134(5) 0.0080(5) O3 0.0321(6) 0.0529(8) 0.0748(9) 0.0030(5) 0.0210(6) -0.0175(7) O1W 0.0940(10) 0.0389(7) 0.0329(6) -0.0205(7) 0.0224(6) -0.0034(5) O2W 0.0363(5) 0.0319(5) 0.0419(6) -0.0038(4) 0.0182(5) -0.0053(4) N1 0.0304(6) 0.0276(6) 0.0369(6) 0.0009(4) 0.0146(5) 0.0016(5) C1 0.0334(7) 0.0308(7) 0.0433(8) 0.0008(6) 0.0171(6) -0.0015(6) C2 0.0580(10) 0.0387(8) 0.0423(9) -0.0058(7) 0.0217(8) -0.0067(7) C3 0.0580(10) 0.0445(9) 0.0398(9) -0.0131(8) 0.0030(8) 0.0024(8) C4 0.0299(7) 0.0453(9) 0.0620(10) -0.0009(7) 0.0052(7) 0.0149(8) C5 0.0333(7) 0.0315(7) 0.0580(10) 0.0047(6) 0.0215(7) 0.0096(7) C6 0.0434(8) 0.0325(7) 0.0351(7) -0.0032(6) 0.0178(6) 0.0002(6) C7 0.0358(7) 0.0257(6) 0.0341(7) 0.0026(5) 0.0161(6) -0.0019(5) 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' 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 O3 Mg1 O1W . . 90.97(7) yes O3 Mg1 O1W . 3_556 89.03(7) yes O3 Mg1 O2W . 3_556 88.51(5) yes O3 Mg1 O2W . . 91.49(5) yes O1W Mg1 O2W . . 91.08(5) yes O1W Mg1 O2W . 3_556 88.92(5) yes N1 C6 C7 . . 111.30(10) yes O3 Mg1 O3 3_556 . 180.0 no O3 Mg1 O1W 3_556 . 89.03(7) no O3 Mg1 O1W 3_556 3_556 90.97(7) no O3 Mg1 O2W 3_556 3_556 91.49(5) no O3 Mg1 O2W 3_556 . 88.51(5) no O1W Mg1 O1W . 3_556 180.0 no O1W Mg1 O2W 3_556 . 88.92(5) no O1W Mg1 O2W 3_556 3_556 91.08(5) no O2W Mg1 O2W . 3_556 180.00(3) no Mg1 O1W H1W1 . . 122(2) no Mg1 O1W H1W2 . . 125(2) no Mg1 O2W H2W1 . . 117.0(10) no Mg1 O2W H2W2 . . 116.0(10) no O1 C7 C6 . . 116.30(10) no O2 C7 O1 . . 126.30(10) no O2 C7 C6 . . 117.40(10) no O3 C1 N1 . . 117.10(10) no O3 C1 C2 . . 126.7(2) no N1 C1 C2 . . 116.20(10) no N1 C5 H5 . . 119.5 no N1 C6 H6A . . 109.4 no N1 C6 H6B . . 109.4 no C1 O3 Mg1 . . 151.50(10) no C1 N1 C6 . . 115.70(10) no C1 C2 H2 . . 119.6 no C2 C3 C4 . . 120.6(2) no C2 C3 H3 . . 119.7 no C3 C2 C1 . . 120.8(2) no C3 C2 H2 . . 119.6 no C3 C4 H4 . . 120.6 no C4 C3 H3 . . 119.7 no C4 C5 N1 . . 121.0(2) no C4 C5 H5 . . 119.5 no C5 N1 C1 . . 122.60(10) no C5 N1 C6 . . 121.70(10) no C5 C4 C3 . . 118.8(2) no C5 C4 H4 . . 120.6 no C7 C6 H6A . . 109.4 no C7 C6 H6B . . 109.4 no H1W1 O1W H1W2 . . 109.0(10) no H2W1 O2W H2W2 . . 110.0(10) no H6A C6 H6B . . 108.0 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 Mg1 O1W . 2.0600(10) yes Mg1 O2W . 2.0990(10) yes Mg1 O3 . 2.0270(10) yes O3 C1 . 1.246(2) yes C2 C3 . 1.360(3) yes C4 C5 . 1.351(3) yes Mg1 O1W 3_556 2.0600(10) no Mg1 O2W 3_556 2.0990(10) no Mg1 O3 3_556 2.0270(10) no O1W H1W1 . 0.86(2) no O1W H1W2 . 0.86(2) no O2W H2W1 . 0.86(2) no O2W H2W2 . 0.86(2) no O1 C7 . 1.265(2) no O2 C7 . 1.238(2) no N1 C5 . 1.364(2) no N1 C1 . 1.378(2) no N1 C6 . 1.457(2) no C1 C2 . 1.423(2) no C2 H2 . 0.93 no C3 C4 . 1.402(3) no C3 H3 . 0.93 no C4 H4 . 0.93 no C5 H5 . 0.93 no C6 C7 . 1.542(2) no C6 H6A . 0.97 no C6 H6B . 0.97 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 O1 4_565 0.86(2) 1.880(10) 2.735(2) 175(3) yes O1W H1W1 O1 3_566 0.86(2) 1.930(10) 2.779(2) 175(3) yes O2W H2W2 O2 1_545 0.86(2) 1.860(10) 2.717(2) 177(2) yes O2W H2W1 O1 3_556 0.86(2) 2.09(2) 2.933(2) 179(2) 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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag Mg1 O3 C1 N1 . 178.2(2) no Mg1 O3 C1 C2 . -1.6(4) no O3 C1 C2 C3 . 179.8(2) no O1W Mg1 O3 C1 . 65.2(3) no O1W Mg1 O3 C1 3_556 -114.8(3) no O2W Mg1 O3 C1 . -25.9(3) no O2W Mg1 O3 C1 3_556 154.1(3) no N1 C6 C7 O2 . 31.6(2) no N1 C6 C7 O1 . -150.00(10) no N1 C1 C2 C3 . 0.0(2) no C1 N1 C6 C7 . 66.39(18) no C1 C2 C3 C4 . -0.8(3) no C1 N1 C5 C4 . -1.7(2) no C2 C3 C4 C5 . 0.5(3) no C3 C4 C5 N1 . 0.8(2) no C5 N1 C1 O3 . -178.60(10) no C5 N1 C6 C7 . -111.80(10) no C5 N1 C1 C2 . 1.2(2) no C6 N1 C1 C2 . -176.90(10) no C6 N1 C1 O3 . 3.2(2) no C6 N1 C5 C4 . 176.40(10) no