#------------------------------------------------------------------------------ #$Date: 2017-01-11 12:50:15 +0000 (Wed, 11 Jan 2017) $ #$Revision: 190396 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003475.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_2003475 loop_ _publ_author_name 'Cousson, A.' 'Nectoux, F.' 'Robert, F.' 'Rizkalla, E. N.' _publ_section_title ; Sodium Bis(dipicolinato)ferrate(III) Dihydrate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 838 _journal_page_last 840 _journal_paper_doi 10.1107/S0108270194005561 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C14 H10 Fe N2 Na O10' _chemical_formula_weight 445.07 _space_group_IT_number 9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _audit_creation_method CRYSTALS _cell_angle_alpha 90.000 _cell_angle_beta 93.12(2) _cell_angle_gamma 90.000 _cell_formula_units_Z 4 _cell_length_a 14.904(4) _cell_length_b 12.434(2) _cell_length_c 8.645(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 16.8 _cell_measurement_theta_min 15 _cell_volume 1599.7(7) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CRYSTALS (Watkins, Carruthers & Betteridge, 1985)' _computing_molecular_graphics 'CRYSTALS ' _computing_publication_material 'CRYSTALS ' _computing_structure_refinement 'CRYSTALS ' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_measurement_device ' Enraf-nonius CAD4 ' _diffrn_measurement_method \w-2\q _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 0.03 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2151 _diffrn_reflns_theta_max 28 _diffrn_standards_decay_% <0.7 _diffrn_standards_interval_time 60 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_T_max 1.165 _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_type 'empirical (DIFABS; Walker & Stuart, 1983)' _exptl_crystal_colour 'pale green' _exptl_crystal_density_diffrn 1.85 _exptl_crystal_description prism _exptl_crystal_F_000 901.61 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.08 _refine_diff_density_min -0.3 _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_abs_structure_Rogers 1.000 _refine_ls_extinction_coef 621.1(248) _refine_ls_extinction_method 'Larson (1970)' _refine_ls_goodness_of_fit_obs 1.08 _refine_ls_hydrogen_treatment 'One U~eq~ value for all H atoms' _refine_ls_number_parameters 289 _refine_ls_number_reflns 1783 _refine_ls_restrained_S_obs 1.0 _refine_ls_R_factor_obs 0.0306 _refine_ls_shift/esd_max 0.1 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'Chebychev weighting scheme with parameters 6.25' _refine_ls_wR_factor_obs 0.0343 _reflns_number_observed 1783 _reflns_number_total 1934 _reflns_observed_criterion I>=3\s(I) _cod_data_source_file mu1094.cif _cod_data_source_block mu1094a _cod_depositor_comments ; Moving the _atom_type_scat_source data item into the _atom_type loop. All entries of the loop were assumed to have the same _atom_type_scat_source data item value. Antanas Vaitkus, 2017-01-11 Moving the _atom_type_scat_dispersion_real and _atom_type_scat_dispersion_imag data items into the _atom_type loop. Antanas Vaitkus, 2017-01-11 ; _cod_original_cell_volume 1599.69 _cod_original_sg_symbol_H-M 'C c' _cod_original_formula_sum 'C14 H10 Fe1 N2 Na1 O10' _cod_database_code 2003475 loop_ _symmetry_equiv_pos_as_xyz X,Y,Z X+1/2,Y+1/2,Z X,-Y,Z+1/2 X+1/2,-Y+1/2,Z+1/2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Fe(1) 0.0203(2) -0.0016(1) 0.0009(1) 0.0153(2) 0.0012(1) 0.0203(2) Na(1) 0.0284(6) 0.0013(5) -0.0007(4) 0.0324(6) -0.0072(5) 0.0246(6) C(1) 0.019(1) 0.002(1) 0.0037(9) 0.024(1) 0.000(1) 0.013(1) C(2) 0.017(1) -0.0007(9) 0.0048(9) 0.022(1) -0.0003(9) 0.012(1) C(3) 0.025(1) 0.002(1) 0.006(1) 0.021(1) 0.003(1) 0.023(1) C(4) 0.031(2) -0.007(1) 0.006(1) 0.019(1) -0.002(1) 0.027(1) C(5) 0.024(1) -0.009(1) 0.003(1) 0.026(1) -0.004(1) 0.025(1) C(6) 0.014(1) -0.003(1) 0.0047(9) 0.024(1) 0.002(1) 0.016(1) C(7) 0.017(1) -0.001(1) 0.0038(9) 0.028(1) 0.004(1) 0.018(1) C(8) 0.020(1) 0.000(1) -0.0021(9) 0.024(1) -0.003(1) 0.018(1) C(9) 0.017(1) -0.002(1) -0.0008(9) 0.027(1) -0.001(1) 0.016(1) C(10) 0.022(1) -0.005(1) 0.005(1) 0.027(1) 0.002(1) 0.026(1) C(11) 0.031(2) -0.006(1) -0.001(1) 0.020(1) 0.002(1) 0.029(2) C(12) 0.023(1) 0.001(1) -0.003(1) 0.020(1) -0.002(1) 0.025(2) C(13) 0.018(1) 0.002(1) -0.0016(9) 0.023(1) 0.0003(9) 0.015(1) C(14) 0.016(1) 0.001(1) -0.0003(9) 0.025(1) 0.002(1) 0.017(1) N(1) 0.018(1) -0.0027(8) 0.0045(8) 0.020(1) -0.0006(8) 0.018(1) N(2) 0.017(1) -0.0007(9) 0.0019(8) 0.017(1) 0.0011(9) 0.020(1) O(1) 0.026(1) 0.0005(8) -0.0056(8) 0.022(1) -0.0024(8) 0.022(1) O(2) 0.029(1) 0.0043(9) -0.0074(8) 0.030(1) -0.0003(9) 0.024(1) O(3) 0.024(1) -0.0069(9) -0.0069(8) 0.042(1) 0.010(1) 0.028(1) O(4) 0.030(1) -0.0002(8) -0.008(1) 0.024(1) 0.0067(8) 0.032(1) O(5) 0.024(1) -0.0002(7) 0.0079(9) 0.022(1) -0.0053(8) 0.030(1) O(6) 0.024(1) -0.003(1) 0.0109(9) 0.038(1) -0.009(1) 0.034(1) O(7) 0.025(1) -0.0011(8) 0.0097(8) 0.024(1) 0.0032(8) 0.028(1) O(8) 0.031(1) 0.0051(9) 0.014(1) 0.031(1) 0.001(1) 0.034(1) O(9) 0.052(1) 0.013(1) -0.006(1) 0.041(1) -0.004(1) 0.024(1) O(10) 0.057(2) -0.035(2) -0.003(1) 0.075(2) -0.007(1) 0.025(1) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Fe(1) 1.0000 -0.00007(6) 0.24700(3) -0.0001(1) 0.0184 Uani Na(1) 1.0000 0.2406(1) 0.1333(1) 0.7506(2) 0.0277 Uani C(1) 1.0000 0.0864(2) 0.0712(2) 0.1637(3) 0.0178 Uani C(2) 1.0000 0.0189(2) 0.0165(2) 0.0525(3) 0.0158 Uani C(3) 1.0000 0.0048(2) -0.0933(2) 0.0322(3) 0.0223 Uani C(4) 1.0000 -0.0636(2) -0.1252(2) -0.0731(4) 0.0239 Uani C(5) 1.0000 -0.1153(2) -0.0491(2) -0.1560(3) 0.0231 Uani C(6) 1.0000 -0.0964(2) 0.0588(2) -0.1295(3) 0.0169 Uani C(7) 1.0000 -0.1399(2) 0.1565(2) -0.2065(3) 0.0198 Uani C(8) 1.0000 0.1438(2) 0.3284(2) -0.1796(3) 0.0203 Uani C(9) 1.0000 0.1063(2) 0.4284(2) -0.1078(3) 0.0192 Uani C(10) 1.0000 0.1313(2) 0.5343(2) -0.1295(4) 0.0242 Uani C(11) 1.0000 0.0834(2) 0.6141(2) -0.0575(4) 0.0252 Uani C(12) 1.0000 0.0130(2) 0.5874(2) 0.0342(3) 0.0225 Uani C(13) 1.0000 -0.0070(2) 0.4791(2) 0.0520(3) 0.0185 Uani C(14) 1.0000 -0.0787(2) 0.4288(2) 0.1465(3) 0.0188 Uani N(1) 1.0000 -0.0308(2) 0.0874(2) -0.0266(3) 0.0180 Uani N(2) 1.0000 0.0393(2) 0.4045(2) -0.0189(3) 0.0181 Uani O(1) 1.0000 0.0789(1) 0.1742(2) 0.1644(2) 0.0231 Uani O(2) 1.0000 0.1396(2) 0.0180(2) 0.2452(3) 0.0267 Uani O(3) 1.0000 -0.2032(2) 0.1459(2) -0.3016(3) 0.0285 Uani O(4) 1.0000 -0.1039(2) 0.2453(2) -0.1621(3) 0.0269 Uani O(5) 1.0000 0.0986(2) 0.2424(2) -0.1534(3) 0.0242 Uani O(6) 1.0000 0.2101(2) 0.3309(2) -0.2552(3) 0.0292 Uani O(7) 1.0000 -0.0773(2) 0.3258(2) 0.1465(3) 0.0242 Uani O(8) 1.0000 -0.1308(2) 0.4851(2) 0.2140(3) 0.0293 Uani O(9) 1.0000 0.2876(2) 0.1573(3) 0.0099(3) 0.0360 Uani O(10) 1.0000 0.2309(3) 0.1449(4) 0.4774(3) 0.0416 Uani H(3) 1.0000 0.035(3) -0.138(4) 0.087(5) 0.031(3) Uiso H(4) 1.0000 -0.074(3) -0.201(4) -0.085(5) 0.031(3) Uiso H(5) 1.0000 -0.166(3) -0.073(4) -0.218(5) 0.031(3) Uiso H(10) 1.0000 0.179(3) 0.552(4) -0.176(5) 0.031(3) Uiso H(11) 1.0000 0.104(3) 0.687(4) -0.063(5) 0.031(3) Uiso H(12) 1.0000 -0.018(3) 0.643(4) 0.071(5) 0.031(3) Uiso H(91) 1.0000 0.307(3) 0.123(4) 0.068(6) 0.031(3) Uiso H(92) 1.0000 0.284(3) 0.218(4) 0.060(5) 0.031(3) Uiso H(101) 1.0000 0.262(3) 0.177(4) 0.442(5) 0.031(3) Uiso H(102) 1.0000 0.214(3) 0.106(4) 0.439(6) 0.031(3) Uiso loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C ' 0.0020 0.0020 'IntTabIV Table 2.2B' 'H ' 0.0000 0.0000 'IntTabIV Table 2.2B' 'O ' 0.0080 0.0060 'IntTabIV Table 2.2B' 'N ' 0.0040 0.0030 'IntTabIV Table 2.2B' 'Na ' 0.0300 0.0250 'IntTabIV Table 2.2B' 'Fe ' 0.3010 0.8450 'IntTabIV Table 2.2B' 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 N(1) Fe(1) N(2) . . 168.26(9) yes N(1) Fe(1) O(1) . . 76.20(9) yes N(2) Fe(1) O(1) . . 109.04(9) yes N(1) Fe(1) O(4) . . 75.82(9) yes N(2) Fe(1) O(4) . . 99.57(9) yes O(1) Fe(1) O(4) . . 151.39(9) yes N(1) Fe(1) O(5) . . 93.74(9) yes N(2) Fe(1) O(5) . . 75.82(9) yes O(1) Fe(1) O(5) . . 91.83(9) yes O(4) Fe(1) O(5) . . 95.80(10) yes N(1) Fe(1) O(7) . . 114.22(9) yes N(2) Fe(1) O(7) . . 76.20(9) yes O(1) Fe(1) O(7) . . 96.13(9) yes O(4) Fe(1) O(7) . . 89.90(10) yes O(5) Fe(1) O(7) . . 152.00(8) yes C(2) C(1) O(1) . . 113.3(2) yes C(2) C(1) O(2) . . 120.6(2) yes O(1) C(1) O(2) . . 126.1(3) yes C(1) C(2) C(3) . . 127.7(2) yes C(1) C(2) N(1) . . 111.4(2) yes C(3) C(2) N(1) . . 120.9(3) yes C(2) C(3) C(4) . . 117.7(3) yes C(2) C(3) H(3) . . 120.(3) no C(4) C(3) H(3) . . 122.(3) no C(3) C(4) C(5) . . 120.6(3) yes C(3) C(4) H(4) . . 117.(3) no C(5) C(4) H(4) . . 122.(3) no C(4) C(5) C(6) . . 118.0(3) yes C(4) C(5) H(5) . . 118.(3) no C(6) C(5) H(5) . . 123.(3) no C(5) C(6) C(7) . . 128.7(3) yes C(5) C(6) N(1) . . 120.2(3) yes C(7) C(6) N(1) . . 111.1(2) yes C(6) C(7) O(3) . . 120.4(3) yes C(6) C(7) O(4) . . 113.5(2) yes O(3) C(7) O(4) . . 126.2(3) yes C(9) C(8) O(5) . . 113.7(2) yes C(9) C(8) O(6) . . 122.0(3) yes O(5) C(8) O(6) . . 124.3(3) yes C(8) C(9) C(10) . . 128.3(3) yes C(8) C(9) N(2) . . 111.1(2) yes C(10) C(9) N(2) . . 120.5(3) yes C(9) C(10) C(11) . . 118.1(3) yes C(9) C(10) H(10) . . 123.(3) no C(11) C(10) H(10) . . 119.(3) no C(10) C(11) C(12) . . 120.5(3) yes C(10) C(11) H(11) . . 118.(3) no C(12) C(11) H(11) . . 121.(3) no C(11) C(12) C(13) . . 117.9(3) yes C(11) C(12) H(12) . . 116.(3) no C(13) C(12) H(12) . . 126.(3) no C(12) C(13) C(14) . . 128.4(3) yes C(12) C(13) N(2) . . 120.5(3) yes C(14) C(13) N(2) . . 111.1(2) yes C(13) C(14) O(7) . . 113.6(2) yes C(13) C(14) O(8) . . 120.5(3) yes O(7) C(14) O(8) . . 125.9(3) yes Fe(1) N(1) C(2) . . 118.3(2) yes Fe(1) N(1) C(6) . . 119.0(2) yes C(2) N(1) C(6) . . 122.6(3) yes Fe(1) N(2) C(9) . . 119.1(2) yes Fe(1) N(2) C(13) . . 118.2(2) yes C(9) N(2) C(13) . . 122.5(2) yes Fe(1) O(1) C(1) . . 119.5(2) yes Fe(1) O(4) C(7) . . 120.6(2) yes Fe(1) O(5) C(8) . . 119.6(2) yes Fe(1) O(7) C(14) . . 119.8(2) yes H(91) O(9) H(92) . . 101.(5) no H(101) O(10) H(102) . . 117.(6) no O(2) Na(1) O(5) 3 1_556 84.14(8) yes O(2) Na(1) O(6) 3 1_556 130.90(10) yes O(5) Na(1) O(6) 1_556 1_556 50.43(7) yes O(2) Na(1) O(8) 3 4_555 91.20(9) yes O(5) Na(1) O(8) 1_556 4_555 168.30(10) yes O(6) Na(1) O(8) 1_556 4_555 136.99(9) yes O(2) Na(1) O(9) 3 1_556 105.90(10) yes O(5) Na(1) O(9) 1_556 1_556 80.70(10) yes O(6) Na(1) O(9) 1_556 1_556 86.50(10) yes O(8) Na(1) O(9) 4_555 1_556 90.30(10) yes O(2) Na(1) O(10) 3 . 91.40(10) yes O(5) Na(1) O(10) 1_556 . 105.70(10) yes O(6) Na(1) O(10) 1_556 . 85.30(10) yes O(8) Na(1) O(10) 4_555 . 85.00(10) yes O(9) Na(1) O(10) 1_556 . 162.20(10) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe(1) N(1) 2.047(2) yes Fe(1) N(2) 2.053(2) yes Fe(1) O(1) 2.012(2) yes Fe(1) O(4) 2.030(2) yes Fe(1) O(5) 2.034(2) yes Fe(1) O(7) 2.013(2) yes C(1) C(2) 1.515(4) yes C(1) O(1) 1.285(4) yes C(1) O(2) 1.225(4) yes C(2) C(3) 1.392(4) yes C(2) N(1) 1.318(4) yes C(3) C(4) 1.386(4) yes C(3) H(3) 0.85(5) no C(4) C(5) 1.394(5) yes C(4) H(4) 0.96(5) no C(5) C(6) 1.387(4) yes C(5) H(5) 0.95(5) no C(6) C(7) 1.514(4) yes C(6) N(1) 1.333(4) yes C(7) O(3) 1.225(4) yes C(7) O(4) 1.277(4) yes C(8) C(9) 1.510(4) yes C(8) O(5) 1.290(4) yes C(8) O(6) 1.214(4) yes C(9) C(10) 1.384(4) yes C(9) N(2) 1.327(4) yes C(10) C(11) 1.389(5) yes C(10) H(10) 0.86(5) no C(11) C(12) 1.390(5) yes C(11) H(11) 0.96(4) no C(12) C(13) 1.389(4) yes C(12) H(12) 0.90(5) no C(13) C(14) 1.516(4) yes C(13) N(2) 1.327(4) yes C(14) O(7) 1.281(4) yes C(14) O(8) 1.218(4) yes O(9) H(91) 0.71(5) no O(9) H(92) 0.88(5) no O(10) H(101) 0.70(5) no O(10) H(102) 0.63(5) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag Na(1) O(2) 2.409(3) 3 yes Na(1) O(5) 2.683(3) 1_556 yes Na(1) O(6) 2.500(3) 1_556 yes Na(1) O(8) 2.450(3) 4_555 yes Na(1) O(9) 2.331(3) 1_556 yes Na(1) O(10) 2.363(3) . yes