Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name 'Li-Juan Zhang' 'Zhan Shi' 'Tie-Gang Wang' 'Ji-Qing Xu' 'Xiao-Li Zhao' _publ_contact_author_name 'Dr Li-Juan Zhang' _publ_contact_author_address ; Dr Li-Juan Zhang Jilin University Jiefang Road 119 Changchun Jilin 130023 CHINA ; _publ_contact_author_email ZENGZH@MAIL.JL.CN _publ_section_title ; Hydrothermal synthesis and characterization of the first oxalate-bta mixed-ligand three-dimensional frameworks: {[M2(µ8-bta)(µ2-C2O4)]¡¤(H2O)4}n (M = Co¢ó, Fe¢ó ; data_complex_1 _database_code_CSD 183360 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Co O8' _chemical_formula_weight 265.04 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.3343(19) _cell_length_b 13.738(3) _cell_length_c 6.7078(13) _cell_angle_alpha 90.00 _cell_angle_beta 122.60(3) _cell_angle_gamma 90.00 _cell_volume 724.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour mauve _exptl_crystal_size_max 0.267 _exptl_crystal_size_mid 0.146 _exptl_crystal_size_min 0.112 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 2.397 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8666 _exptl_absorpt_correction_T_max 1.0859 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Rugaku _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 828 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.67 _diffrn_reflns_theta_max 27.44 _reflns_number_total 828 _reflns_number_gt 782 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material SHELXL97 _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^)+(0.0492P)^2^+2.0273P] 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 828 _refine_ls_number_parameters 83 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.500 _refine_ls_shift/su_mean 0.006 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.70572(3) 0.5000 0.0123(2) Uani 1 2 d S . . C1 C 0.3329(4) 0.5000 0.8101(6) 0.0126(6) Uani 1 2 d S . . H1 H 0.2202 0.5000 0.6835 0.080 Uiso 1 2 calc S . . C2 C 0.4154(3) 0.58759(17) 0.9028(4) 0.0117(5) Uani 1 1 d . . . C3 C 0.3269(3) 0.67970(18) 0.7772(4) 0.0123(5) Uani 1 1 d . . . C4 C 0.4038(4) 0.5000 0.4061(6) 0.0137(7) Uani 1 2 d S . . O2 O 0.4075(2) 0.73679(13) 0.7274(3) 0.0161(4) Uani 1 1 d . . . O3 O 0.3344(2) 0.58184(14) 0.3387(3) 0.0194(4) Uani 1 1 d . . . O1 O 0.6757(2) 0.80896(14) 0.7233(4) 0.0185(4) Uani 1 1 d . . . OW1 O 0.4960(6) 0.9451(4) 0.7904(9) 0.0107(9) Uani 0.35 1 d PU . . OW1' O 0.5036(4) 0.8916(2) 0.8638(6) 0.0244(7) Uani 0.65 1 d PU . . 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 Co1 0.0098(3) 0.0092(3) 0.0162(3) 0.000 0.0059(2) 0.000 C1 0.0088(14) 0.0131(16) 0.0134(15) 0.000 0.0044(12) 0.000 C2 0.0102(12) 0.0113(11) 0.0134(11) 0.0012(8) 0.0063(10) 0.0018(8) C3 0.0114(10) 0.0111(10) 0.0120(10) -0.0010(8) 0.0048(9) 0.0004(8) C4 0.0121(17) 0.0143(16) 0.0158(16) 0.000 0.0082(14) 0.000 O2 0.0158(9) 0.0128(8) 0.0199(9) 0.0024(7) 0.0097(7) -0.0003(7) O3 0.0159(9) 0.0118(9) 0.0260(10) 0.0016(7) 0.0082(8) 0.0021(7) O1 0.0126(9) 0.0171(9) 0.0256(10) -0.0080(7) 0.0101(8) -0.0055(7) OW1 0.0040(18) 0.008(2) 0.021(2) -0.0044(17) 0.0071(16) 0.0006(15) OW1' 0.0400(17) 0.0102(14) 0.0384(16) -0.0114(12) 0.0314(14) -0.0078(12) _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 Co1 O1 2.073(2) . ? Co1 O1 2.073(2) 2_656 ? Co1 O3 2.158(2) . ? Co1 O3 2.158(2) 2_656 ? Co1 O2 2.1621(18) 2_656 ? Co1 O2 2.1621(18) . ? C1 C2 1.383(3) . ? C1 C2 1.383(3) 6_565 ? C2 C2 1.406(5) 2_657 ? C2 C3 1.498(3) . ? C3 O2 1.250(3) . ? C3 O1 1.264(3) 8_465 ? C4 O3 1.254(2) 6_565 ? C4 O3 1.254(2) . ? C4 C4 1.540(7) 5_666 ? O1 C3 1.264(3) 8_565 ? OW1 OW1' 0.865(6) . ? OW1 OW1 1.509(10) 6_575 ? 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 O1 Co1 O1 93.67(12) . 2_656 ? O1 Co1 O3 167.47(8) . . ? O1 Co1 O3 95.92(8) 2_656 . ? O1 Co1 O3 95.92(8) . 2_656 ? O1 Co1 O3 167.47(8) 2_656 2_656 ? O3 Co1 O3 75.85(10) . 2_656 ? O1 Co1 O2 85.04(8) . 2_656 ? O1 Co1 O2 79.43(8) 2_656 2_656 ? O3 Co1 O2 104.63(7) . 2_656 ? O3 Co1 O2 93.37(7) 2_656 2_656 ? O1 Co1 O2 79.43(8) . . ? O1 Co1 O2 85.04(8) 2_656 . ? O3 Co1 O2 93.37(7) . . ? O3 Co1 O2 104.63(7) 2_656 . ? O2 Co1 O2 157.23(10) 2_656 . ? C2 C1 C2 121.0(3) . 6_565 ? C1 C2 C2 119.50(16) . 2_657 ? C1 C2 C3 118.5(2) . . ? C2 C2 C3 121.67(14) 2_657 . ? O2 C3 O1 125.9(2) . 8_465 ? O2 C3 C2 116.9(2) . . ? O1 C3 C2 117.2(2) 8_465 . ? O3 C4 O3 127.4(3) 6_565 . ? O3 C4 C4 116.31(16) 6_565 5_666 ? O3 C4 C4 116.31(16) . 5_666 ? C3 O2 Co1 126.23(16) . . ? C4 O3 Co1 115.77(19) . . ? C3 O1 Co1 128.15(17) 8_565 . ? OW1' OW1 OW1 148.1(4) . 6_575 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.938 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.093 #==END#============================================== data_complex_2 _database_code_CSD 183361 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 Fe O8' _chemical_formula_weight 261.96 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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.3825(19) _cell_length_b 13.791(3) _cell_length_c 6.7346(13) _cell_angle_alpha 90.00 _cell_angle_beta 122.37(3) _cell_angle_gamma 90.00 _cell_volume 736.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour brown _exptl_crystal_size_max 0.212 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.114 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 2.078 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1960 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.95 _reflns_number_total 759 _reflns_number_gt 719 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material SHELXL97 _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^)+(0.0478P)^2^+0.1002P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 759 _refine_ls_number_parameters 82 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.20736(3) 1.0000 0.0152(2) Uani 1 2 d S . . C1 C 0.1657(4) 1.0000 0.6888(6) 0.0160(7) Uani 1 2 d S . . H1 H 0.2772 1.0000 0.8149 0.080 Uiso 1 2 calc S . . C2 C 0.0839(3) 1.08743(17) 0.5963(4) 0.0142(5) Uani 1 1 d . . . C3 C 0.1718(3) 1.17930(18) 0.7200(4) 0.0158(5) Uani 1 1 d . . . C4 C 0.0951(4) 1.0000 1.0953(6) 0.0170(7) Uani 1 2 d S . . O1 O 0.1779(2) 1.31005(14) 1.2260(4) 0.0225(4) Uani 1 1 d . . . O2 O 0.0924(2) 1.23740(14) 0.7686(3) 0.0198(4) Uani 1 1 d . . . O3 O 0.1640(2) 1.08163(13) 1.1638(4) 0.0229(4) Uani 1 1 d . . . OW1 O -0.0067(5) 1.3904(3) 0.6278(7) 0.0319(8) Uani 0.61 1 d PU . . OW1' O -0.0047(6) 1.4462(4) 1.2883(9) 0.0242(11) Uani 0.39 1 d P . . 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 Fe1 0.0124(3) 0.0117(3) 0.0181(3) 0.000 0.0059(2) 0.000 C1 0.0119(15) 0.0172(16) 0.0153(14) 0.000 0.0048(12) 0.000 C2 0.0122(11) 0.0147(11) 0.0146(10) -0.0009(8) 0.0064(10) -0.0011(8) C3 0.0147(11) 0.0136(11) 0.0149(10) 0.0021(8) 0.0053(9) 0.0003(8) C4 0.0185(18) 0.0143(16) 0.0200(16) 0.000 0.0115(15) 0.000 O1 0.0153(9) 0.0219(9) 0.0292(10) -0.0087(7) 0.0111(8) -0.0062(7) O2 0.0183(9) 0.0163(8) 0.0226(8) -0.0028(7) 0.0095(7) 0.0004(7) O3 0.0187(10) 0.0147(9) 0.0289(10) -0.0006(7) 0.0086(8) -0.0029(6) OW1 0.059(2) 0.0110(15) 0.0470(18) 0.0136(14) 0.0424(16) 0.0119(13) OW1' 0.013(2) 0.027(3) 0.033(3) -0.009(2) 0.013(2) 0.0050(19) _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 Fe1 O1 2.095(2) . ? Fe1 O1 2.0946(19) 2_557 ? Fe1 O3 2.1847(19) 2_557 ? Fe1 O3 2.1847(19) . ? Fe1 O2 2.1907(18) 2_557 ? Fe1 O2 2.1907(18) . ? C1 C2 1.385(3) 6_575 ? C1 C2 1.385(3) . ? C2 C2 1.405(5) 2_556 ? C2 C3 1.498(3) . ? C3 O2 1.251(3) . ? C3 O1 1.262(3) 7_577 ? C4 O3 1.256(2) . ? C4 O3 1.256(2) 6_575 ? C4 C4 1.542(7) 5_577 ? O1 C3 1.262(3) 7_577 ? OW1 OW1' 0.926(6) 2_557 ? OW1 OW1 1.791(7) 2_556 ? OW1' OW1 0.926(6) 2_557 ? OW1' OW1' 1.485(12) 6_585 ? 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 O1 Fe1 O1 94.92(12) . 2_557 ? O1 Fe1 O3 167.22(8) . 2_557 ? O1 Fe1 O3 95.62(8) 2_557 2_557 ? O1 Fe1 O3 95.62(8) . . ? O1 Fe1 O3 167.22(8) 2_557 . ? O3 Fe1 O3 74.94(10) 2_557 . ? O1 Fe1 O2 79.64(7) . 2_557 ? O1 Fe1 O2 85.66(7) 2_557 2_557 ? O3 Fe1 O2 93.98(8) 2_557 2_557 ? O3 Fe1 O2 103.34(7) . 2_557 ? O1 Fe1 O2 85.65(7) . . ? O1 Fe1 O2 79.64(7) 2_557 . ? O3 Fe1 O2 103.34(7) 2_557 . ? O3 Fe1 O2 93.98(8) . . ? O2 Fe1 O2 158.20(10) 2_557 . ? C2 C1 C2 121.0(3) 6_575 . ? C1 C2 C2 119.49(15) . 2_556 ? C1 C2 C3 118.6(2) . . ? C2 C2 C3 121.65(13) 2_556 . ? O2 C3 O1 125.5(2) . 7_577 ? O2 C3 C2 117.3(2) . . ? O1 C3 C2 117.1(2) 7_577 . ? O3 C4 O3 127.3(3) . 6_575 ? O3 C4 C4 116.37(16) . 5_577 ? O3 C4 C4 116.37(16) 6_575 5_577 ? C3 O1 Fe1 128.36(17) 7_577 . ? C3 O2 Fe1 125.64(17) . . ? C4 O3 Fe1 116.16(19) . . ? OW1' OW1 OW1 122.8(4) 2_557 2_556 ? OW1 OW1' OW1' 146.1(4) 2_557 6_585 ? _diffrn_measured_fraction_theta_max 0.825 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.825 _refine_diff_density_max 0.852 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.090