#------------------------------------------------------------------------------ #$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/02/2200229.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_2200229 loop_ _publ_author_name 'Park, Ki-Min' 'Yoon, Il' 'Seo, Joobeom' 'Lee, Yoon Hee' 'Lee, Shim Sung' _publ_section_title ; A magnesium(II) complex of 1,10-phenanthroline-2,9-dicarboxylate ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m154 _journal_page_last m156 _journal_paper_doi 10.1107/S1600536801004317 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Mg (C14 H6 N2 O4) (H2 O)3], 2H2 O' _chemical_formula_moiety 'C14 H12 Mg N2 O7, 2H2 O' _chemical_formula_sum 'C14 H16 Mg N2 O9' _chemical_formula_weight 380.60 _chemical_name_systematic ; Triaqua(1,10-phenanthroline-2,9-dicarboxylato)magnesium(II) dihydrate ; _space_group_IT_number 70 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-F 2uv 2vw' _symmetry_space_group_name_H-M 'F d d d :2' _audit_creation_method SHELXTL _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 7.4194(12) _cell_length_b 19.044(3) _cell_length_c 46.943(7) _cell_measurement_reflns_used 10406 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.29 _cell_measurement_theta_min 1.74 _cell_volume 6632.8(18) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Siemens, 1996)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .996 _diffrn_measured_fraction_theta_max .996 _diffrn_measurement_device_type 'CCD area detector' _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 .0661 _diffrn_reflns_av_sigmaI/netI .0372 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -62 _diffrn_reflns_number 10406 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 1.74 _exptl_absorpt_coefficient_mu .161 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3168 _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .15 _refine_diff_density_max .323 _refine_diff_density_min -.311 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2063 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all .085 _refine_ls_R_factor_gt .055 _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^)+(0.1026P)^2^+8.6902P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .186 _reflns_number_gt 1385 _reflns_number_total 2063 _reflns_threshold_expression I>2\s(I) _cod_data_source_file tk6009.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 'Orthorhombic' changed to 'orthorhombic' 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_original_sg_symbol_H-M 'F d d d' _cod_database_code 2200229 _cod_database_fobs_code 2200229 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' 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 Mg .3750 .3750 .07737(2) .0375(3) Uani d S 1 . . Mg O1 .6448(2) .42950(10) .08789(3) .0469(5) Uani d . 1 . . O O2 .8903(3) .48671(12) .07265(4) .0602(6) Uani d . 1 . . O O3 .3750 .3750 .12114(5) .0519(7) Uani d S 1 . . O O4 .2576(2) .47404(10) .07751(4) .0478(5) Uani d . 1 . . O N1 .5316(2) .40521(10) .03692(4) .0373(5) Uani d . 1 . . N C1 .7482(3) .45259(13) .06867(5) .0417(6) Uani d . 1 . . C C2 .6882(3) .43836(12) .03842(5) .0394(5) Uani d . 1 . . C C3 .7830(4) .45897(14) .01391(6) .0492(6) Uani d . 1 . . C H3 .8952 .4837 .0156 .059 Uiso calc R 1 . . H C4 .7149(4) .44364(14) -.01242(5) .0522(7) Uani d . 1 . . C H4 .7805 .4564 -.0293 .063 Uiso calc R 1 . . H C5 .5475(4) .40896(13) -.01468(5) .0453(6) Uani d . 1 . . C C6 .4568(4) .39108(14) -.04074(5) .0567(7) Uani d . 1 . . C H6 .5132 .4021 -.0586 .068 Uiso calc R 1 . . H C7 .4614(3) .39150(12) .01097(4) .0386(5) Uani d . 1 . . C O5 .4235(18) .5506(3) .12298(12) .061(2) Uani d P .69(4) . . O O5' .327(9) .5534(8) .1265(4) .100(10) Uani d P .31(4) . . O H3A .2856 .3532 .1341 .050 Uiso d . 1 . . H H4A .1426 .4775 .0769 .050 Uiso d . 1 . . H H4B .2937 .4967 .0939 .050 Uiso d . 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 Mg .0400(6) .0452(6) .0273(5) .0001(5) .000 .000 O1 .0417(10) .0646(12) .0345(9) -.0086(8) -.0030(7) .0076(7) O2 .0427(10) .0702(13) .0677(13) -.0095(9) -.0055(9) .0103(10) O3 .0543(15) .0739(17) .0276(11) -.0216(13) .000 .000 O4 .0427(9) .0532(10) .0475(10) .0020(8) .0007(7) -.0011(8) N1 .0371(10) .0446(10) .0304(9) .0039(8) .0015(7) .0030(8) C1 .0314(11) .0484(13) .0454(13) .0018(10) -.0024(9) .0080(10) C2 .0381(12) .0423(12) .0376(11) .0056(9) .0044(9) .0071(9) C3 .0463(14) .0521(15) .0491(15) .0012(12) .0115(11) .0105(11) C4 .0635(17) .0546(15) .0385(13) .0087(13) .0172(11) .0113(11) C5 .0612(16) .0431(13) .0315(11) .0127(12) .0074(10) .0060(9) C6 .084(2) .0564(17) .0297(11) .0152(14) .0076(11) .0045(10) C7 .0470(13) .0394(12) .0294(10) .0102(9) .0030(9) .0028(8) O5 .070(5) .0518(19) .060(2) .003(2) .006(2) -.0002(17) O5' .14(3) .063(6) .096(8) -.017(9) .001(11) -.028(6) 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' Mg Mg .0486 .0363 '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 Mg O4 . 2 89.81(5) ? O3 Mg O4 . . 89.81(5) y O4 Mg O4 2 . 179.63(11) y O3 Mg N1 . . 145.68(5) ? O4 Mg N1 2 . 91.03(7) ? O4 Mg N1 . . 89.28(7) y O3 Mg N1 . 2 145.68(5) ? O4 Mg N1 2 2 89.28(7) ? O4 Mg N1 . 2 91.03(7) ? N1 Mg N1 . 2 68.64(10) y O3 Mg O1 . 2 77.65(5) ? O4 Mg O1 2 2 87.41(7) ? O4 Mg O1 . 2 92.51(7) ? N1 Mg O1 . 2 136.66(7) ? N1 Mg O1 2 2 68.03(6) ? O3 Mg O1 . . 77.65(5) y O4 Mg O1 2 . 92.51(7) ? O4 Mg O1 . . 87.41(7) y N1 Mg O1 . . 68.04(6) y N1 Mg O1 2 . 136.66(7) ? O1 Mg O1 2 . 155.30(9) ? C1 O1 Mg . . 122.05(15) ? C2 N1 C7 . . 118.61(19) ? C2 N1 Mg . . 121.23(14) ? C7 N1 Mg . . 120.12(15) ? O2 C1 O1 . . 125.8(2) ? O2 C1 C2 . . 118.7(2) ? O1 C1 C2 . . 115.4(2) ? N1 C2 C3 . . 121.9(2) ? N1 C2 C1 . . 113.18(18) ? C3 C2 C1 . . 124.9(2) ? C4 C3 C2 . . 119.7(3) ? C3 C4 C5 . . 119.6(2) ? C7 C5 C4 . . 116.6(2) ? C7 C5 C6 . . 117.5(3) ? C4 C5 C6 . . 125.9(2) ? C6 C6 C5 2 . 121.63(16) ? N1 C7 C5 . . 123.6(2) ? N1 C7 C7 . 2 115.56(13) ? C5 C7 C7 . 2 120.87(15) ? 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 Mg O3 . 2.055(2) y Mg O4 2 2.0777(18) ? Mg O4 . 2.0777(18) y Mg N1 . 2.2994(19) y Mg N1 2 2.2994(19) ? Mg O1 2 2.3080(16) ? Mg O1 . 2.3080(17) y O1 C1 . 1.263(3) ? O2 C1 . 1.252(3) ? N1 C2 . 1.324(3) ? N1 C7 . 1.350(3) ? C1 C2 . 1.513(3) ? C2 C3 . 1.405(3) ? C3 C4 . 1.367(4) ? C4 C5 . 1.411(4) ? C5 C7 . 1.403(3) ? C5 C6 . 1.437(4) ? C6 C6 2 1.360(6) ? C7 C7 2 1.428(5) ? O5 O5' . .74(5) ? 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 O3 H3A O1 12_454 .9910(10) 1.791(2) 2.774(2) 170.60(10) y O4 H4A O2 1_455 .856(2) 1.891(2) 2.745(3) 175.80(10) y O4 H4B O5 1_555 .922(2) 1.960(7) 2.863(6) 165.7(4) y O4 H4B O5' 1_555 .922(2) 1.890(10) 2.800(10) 169(2) y O5 . O2 11_554 . . 2.866(7) . y O5' . O2 11_554 . . 2.71(2) . y O5 . O5 8_554 . . 2.840(10) . y O5' . O5' 8_554 . . 2.73(3) . y 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 O1 C1 C2 N1 1.9(3) O2 C1 C2 C3 1.9(4)