Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal OSciety of Chemistry 2002 data_{K[Fe(1,3,5-triazine-2,4,6-tricarboxilate)(H2O)2]}.2H2O_(1) _database_code_CSD 173765 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Dunbar, K.' 'Juan-Modesto Clemente-Juan' 'Jose-Ramon Galan-Mascaros' _publ_contact_author_name 'Prof K Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A & M University College Station Texas TX77842-3012 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DUNBAR@MAIL.CHEM.TAMU.EDU' _publ_section_title ; Synthesis, structure and magnetic properties of the one-dimensional chain compound {K[Fe(1,3,5-triazine-2,4,6-tricarboxylate)(H2O)2]} ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; {K[Fe(1,3,5-triazine-2,4,6-tricarboxilate)(H2O)2]}.2H2O ; _chemical_formula_sum 'C6 H8 Fe1 K1 N3 O10' _chemical_formula_weight 377.1 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 7.0800(14) _cell_length_b 8.828(2) _cell_length_c 10.299(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.24(3) _cell_angle_gamma 90.00 _cell_volume 618.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.026 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.617 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4749 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1475 _reflns_number_gt 1191 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.2587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1475 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 3.479 _refine_ls_shift/su_mean 0.031 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.5000 -0.43403(5) 0.7500 0.01729(18) Uani 1 2 d S . . K K 1.0000 -0.56645(8) 0.7500 0.0220(2) Uani 1 2 d S . . N1 N 0.5000 -0.1939(3) 0.7500 0.0174(6) Uani 1 2 d S . . N2 N 0.6088(3) 0.0368(2) 0.6802(2) 0.0189(4) Uani 1 1 d . . . O1 O 0.7056(2) -0.35139(18) 0.62627(17) 0.0202(4) Uani 1 1 d . . . O2 O 0.8010(3) -0.1424(2) 0.5344(2) 0.0298(4) Uani 1 1 d . . . O3 O 0.3967(2) -0.65439(18) 0.81341(17) 0.0206(4) Uani 1 1 d . . . O4 O 0.2522(3) -0.4540(2) 0.5791(2) 0.0218(4) Uani 1 1 d . . . O5 O 0.1120(3) -0.2086(2) 0.4405(2) 0.0279(4) Uani 1 1 d . . . C1 C 0.6026(3) -0.1141(2) 0.6831(2) 0.0181(5) Uani 1 1 d . . . C2 C 0.5000 0.1060(4) 0.7500 0.0174(6) Uani 1 2 d S . . C3 C 0.7160(3) -0.2094(3) 0.6072(3) 0.0205(5) Uani 1 1 d . . . C4 C 0.5000 -0.7204(4) 0.7500 0.0156(6) Uani 1 2 d S . . H1 H 1.264(4) -0.493(4) 1.025(3) 0.021(8) Uiso 1 1 d . . . H2 H 1.217(5) -0.623(4) 1.037(4) 0.037(9) Uiso 1 1 d . . . H3 H 1.164(5) -0.853(4) 0.914(3) 0.033(9) Uiso 1 1 d . . . H4 H 1.017(6) -0.834(4) 0.966(4) 0.051(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0200(3) 0.0153(3) 0.0196(3) 0.000 0.01063(19) 0.000 K 0.0207(4) 0.0217(4) 0.0252(4) 0.000 0.0090(3) 0.000 N1 0.0199(12) 0.0184(13) 0.0177(14) 0.000 0.0116(11) 0.000 N2 0.0211(9) 0.0177(9) 0.0213(11) 0.0000(7) 0.0115(8) -0.0002(7) O1 0.0258(8) 0.0154(7) 0.0228(9) -0.0003(6) 0.0126(7) 0.0008(6) O2 0.0387(10) 0.0210(9) 0.0410(11) 0.0029(8) 0.0298(9) 0.0016(8) O3 0.0240(8) 0.0169(7) 0.0255(9) -0.0007(6) 0.0144(7) 0.0006(6) O4 0.0273(9) 0.0192(9) 0.0204(10) -0.0020(7) 0.0094(7) 0.0020(7) O5 0.0329(10) 0.0213(9) 0.0370(12) 0.0041(8) 0.0219(9) 0.0027(8) C1 0.0179(10) 0.0176(11) 0.0207(12) 0.0001(9) 0.0088(9) 0.0002(8) C2 0.0181(14) 0.0161(14) 0.0199(17) 0.000 0.0083(12) 0.000 C3 0.0216(11) 0.0188(11) 0.0238(13) 0.0004(9) 0.0111(9) 0.0015(9) C4 0.0157(13) 0.0188(14) 0.0139(15) 0.000 0.0067(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O4 2.117(2) 2_656 ? Fe O4 2.117(2) . ? Fe N1 2.120(3) . ? Fe O3 2.2389(17) . ? Fe O3 2.2390(17) 2_656 ? Fe O1 2.3049(17) 2_656 ? Fe O1 2.3050(17) . ? Fe K 3.7280(7) . ? Fe K 3.7280(7) 1_455 ? K O5 2.748(2) 3_646 ? K O5 2.748(2) 4_646 ? K O3 2.8092(17) 1_655 ? K O3 2.8092(17) 2_656 ? K O1 2.8437(18) . ? K O1 2.8438(18) 2_756 ? K O4 3.0045(19) 1_655 ? K O4 3.0046(19) 2_656 ? K O4 3.365(2) 3_646 ? K O4 3.365(2) 4_646 ? K Fe 3.7280(7) 1_655 ? N1 C1 1.333(3) 2_656 ? N1 C1 1.333(3) . ? N2 C1 1.334(3) . ? N2 C2 1.339(2) . ? O1 C3 1.274(3) . ? O2 C3 1.236(3) . ? O3 C4 1.252(2) . ? O3 K 2.8092(17) 1_455 ? O4 K 3.0046(19) 1_455 ? O4 K 3.365(2) 3_646 ? O5 K 2.748(2) 3_646 ? C1 C3 1.521(3) . ? C2 N2 1.339(2) 2_656 ? C2 C4 1.532(4) 1_565 ? C4 O3 1.252(2) 2_656 ? C4 C2 1.532(4) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Fe O4 170.45(11) 2_656 . ? O4 Fe N1 94.77(5) 2_656 . ? O4 Fe N1 94.77(5) . . ? O4 Fe O3 87.00(7) 2_656 . ? O4 Fe O3 84.71(7) . . ? N1 Fe O3 150.33(4) . . ? O4 Fe O3 84.71(7) 2_656 2_656 ? O4 Fe O3 87.00(7) . 2_656 ? N1 Fe O3 150.33(4) . 2_656 ? O3 Fe O3 59.35(8) . 2_656 ? O4 Fe O1 94.11(7) 2_656 2_656 ? O4 Fe O1 88.92(7) . 2_656 ? N1 Fe O1 71.55(4) . 2_656 ? O3 Fe O1 78.78(6) . 2_656 ? O3 Fe O1 138.13(6) 2_656 2_656 ? O4 Fe O1 88.92(7) 2_656 . ? O4 Fe O1 94.10(7) . . ? N1 Fe O1 71.55(4) . . ? O3 Fe O1 138.13(6) . . ? O3 Fe O1 78.78(6) 2_656 . ? O1 Fe O1 143.09(8) 2_656 . ? O4 Fe K 53.66(5) 2_656 . ? O4 Fe K 122.71(6) . . ? N1 Fe K 108.274(13) . . ? O3 Fe K 96.62(4) . . ? O3 Fe K 48.69(4) 2_656 . ? O1 Fe K 147.76(4) 2_656 . ? O1 Fe K 49.66(4) . . ? O4 Fe K 122.71(6) 2_656 1_455 ? O4 Fe K 53.67(5) . 1_455 ? N1 Fe K 108.274(13) . 1_455 ? O3 Fe K 48.69(4) . 1_455 ? O3 Fe K 96.62(4) 2_656 1_455 ? O1 Fe K 49.66(4) 2_656 1_455 ? O1 Fe K 147.76(4) . 1_455 ? K Fe K 143.45(3) . 1_455 ? O5 K O5 87.46(9) 3_646 4_646 ? O5 K O3 92.08(6) 3_646 1_655 ? O5 K O3 64.17(6) 4_646 1_655 ? O5 K O3 64.17(6) 3_646 2_656 ? O5 K O3 92.08(6) 4_646 2_656 ? O3 K O3 147.91(7) 1_655 2_656 ? O5 K O1 97.68(6) 3_646 . ? O5 K O1 146.23(5) 4_646 . ? O3 K O1 148.05(5) 1_655 . ? O3 K O1 61.35(5) 2_656 . ? O5 K O1 146.23(5) 3_646 2_756 ? O5 K O1 97.68(6) 4_646 2_756 ? O3 K O1 61.35(5) 1_655 2_756 ? O3 K O1 148.05(5) 2_656 2_756 ? O1 K O1 96.23(7) . 2_756 ? O5 K O4 85.44(6) 3_646 1_655 ? O5 K O4 123.85(6) 4_646 1_655 ? O3 K O4 60.55(5) 1_655 1_655 ? O3 K O4 132.40(5) 2_656 1_655 ? O1 K O4 89.89(5) . 1_655 ? O1 K O4 63.94(5) 2_756 1_655 ? O5 K O4 123.85(6) 3_646 2_656 ? O5 K O4 85.44(6) 4_646 2_656 ? O3 K O4 132.40(5) 1_655 2_656 ? O3 K O4 60.55(5) 2_656 2_656 ? O1 K O4 63.94(5) . 2_656 ? O1 K O4 89.89(5) 2_756 2_656 ? O4 K O4 141.41(8) 1_655 2_656 ? O5 K O4 49.74(5) 3_646 3_646 ? O5 K O4 136.37(6) 4_646 3_646 ? O3 K O4 117.60(5) 1_655 3_646 ? O3 K O4 64.30(5) 2_656 3_646 ? O1 K O4 52.91(5) . 3_646 ? O1 K O4 122.10(5) 2_756 3_646 ? O4 K O4 68.10(6) 1_655 3_646 ? O4 K O4 109.73(5) 2_656 3_646 ? O5 K O4 136.37(6) 3_646 4_646 ? O5 K O4 49.74(5) 4_646 4_646 ? O3 K O4 64.30(5) 1_655 4_646 ? O3 K O4 117.60(5) 2_656 4_646 ? O1 K O4 122.10(5) . 4_646 ? O1 K O4 52.92(5) 2_756 4_646 ? O4 K O4 109.73(5) 1_655 4_646 ? O4 K O4 68.10(6) 2_656 4_646 ? O4 K O4 173.86(7) 3_646 4_646 ? O5 K Fe 108.11(5) 3_646 1_655 ? O5 K Fe 98.18(5) 4_646 1_655 ? O3 K Fe 36.78(3) 1_655 1_655 ? O3 K Fe 166.98(3) 2_656 1_655 ? O1 K Fe 111.57(4) . 1_655 ? O1 K Fe 38.16(3) 2_756 1_655 ? O4 K Fe 34.58(4) 1_655 1_655 ? O4 K Fe 128.04(4) 2_656 1_655 ? O4 K Fe 102.68(4) 3_646 1_655 ? O4 K Fe 75.34(4) 4_646 1_655 ? O5 K Fe 98.18(5) 3_646 . ? O5 K Fe 108.11(5) 4_646 . ? O3 K Fe 166.98(3) 1_655 . ? O3 K Fe 36.78(3) 2_656 . ? O1 K Fe 38.16(3) . . ? O1 K Fe 111.57(4) 2_756 . ? O4 K Fe 128.04(4) 1_655 . ? O4 K Fe 34.58(4) 2_656 . ? O4 K Fe 75.34(4) 3_646 . ? O4 K Fe 102.68(4) 4_646 . ? Fe K Fe 143.45(3) 1_655 . ? C1 N1 C1 116.2(3) 2_656 . ? C1 N1 Fe 121.88(13) 2_656 . ? C1 N1 Fe 121.88(13) . . ? C1 N2 C2 114.6(2) . . ? C3 O1 Fe 117.97(14) . . ? C3 O1 K 131.25(15) . . ? Fe O1 K 92.18(6) . . ? C4 O3 Fe 88.07(15) . . ? C4 O3 K 134.36(11) . 1_455 ? Fe O3 K 94.53(6) . 1_455 ? Fe O4 K 91.76(7) . 1_455 ? Fe O4 K 156.34(8) . 3_646 ? K O4 K 111.90(6) 1_455 3_646 ? N1 C1 N2 124.4(2) . . ? N1 C1 C3 114.57(19) . . ? N2 C1 C3 121.00(19) . . ? N2 C2 N2 125.7(3) . 2_656 ? N2 C2 C4 117.15(14) . 1_565 ? N2 C2 C4 117.15(14) 2_656 1_565 ? O2 C3 O1 128.5(2) . . ? O2 C3 C1 117.67(19) . . ? O1 C3 C1 113.8(2) . . ? O3 C4 O3 124.5(3) 2_656 . ? O3 C4 C2 117.75(15) 2_656 1_545 ? O3 C4 C2 117.75(15) . 1_545 ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.239 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.110