# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2164 data_440-a _audit_creation_method 'SHELXL + manual editing' _chemical_name_systematic ; Disodium dicobalto(2+)tris[ethandioate(2-)] dihydrate ; _chemical_name_common 'Sodium cobalt oxalate' _chemical_formula_moiety 'Na2 Co2 C6 O14 H4' _chemical_formula_structural 'Na2 Co2 (C2O4)3 (H2O)2' _chemical_formula_analytical 'Na2 Co2 C6 O14 H4' _chemical_formula_sum 'C3 H2 Co Na O7' _chemical_formula_weight 231.97 _chemical_melting_point 'n/a' _chemical_compound_source 'Hydrothermal synthesis djp440bi' 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' 'Na' 'Na' 0.0362 0.0249 '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' '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 P2(1)/c 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' _cell_length_a 5.864(4) _cell_length_b 15.723(6) _cell_length_c 6.963(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.36(4) _cell_angle_gamma 90.00 _cell_volume 631.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.26 _cell_measurement_theta_max 14.50 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.440 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 2.780 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_process_details ; Measured with MSC's Diffraction Control Software PSI subroutine and applied to the data with TEXSAN ; _exptl_absorpt_correction_T_min 0.9338 _exptl_absorpt_correction_T_max 0.9950 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MSC AFCR7 4-circle difractometer' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 256 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 1215 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1104 _reflns_number_observed 886 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MSC Control Software' _computing_cell_refinement 'MSC Control Software' _computing_data_reduction 'TEXSAN' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL+XP' _computing_publication_material 'SHELXTL+XCIF' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.1951P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0268(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1104 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_obs 0.0211 _refine_ls_wR_factor_all 0.0579 _refine_ls_wR_factor_obs 0.0526 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.029 _refine_ls_restrained_S_obs 1.059 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.76949(6) 0.10033(2) 0.21577(5) 0.0157(2) Uani 1 d . . Na1 Na 0.9662(2) 0.31659(7) 0.3076(2) 0.0227(3) Uani 1 d . . O1 O 0.8985(4) 0.10338(12) 0.5163(3) 0.0244(5) Uani 1 d . . O7 O 0.6795(4) 0.08595(14) -0.0861(3) 0.0200(5) Uani 1 d . . O3 O 1.0821(3) 0.15893(12) 0.1741(3) 0.0236(5) Uani 1 d . . C1 C 1.0044(5) 0.0363(2) 0.5749(4) 0.0180(6) Uani 1 d . . O6 O 1.3501(3) 0.29823(12) 0.2836(3) 0.0282(5) Uani 1 d . . C2 C 1.2977(5) 0.1494(2) 0.2145(4) 0.0176(6) Uani 1 d . . O2 O 1.1161(3) 0.02355(12) 0.7438(3) 0.0214(4) Uani 1 d . . O4 O 1.4071(3) 0.08047(12) 0.2304(3) 0.0222(5) Uani 1 d . . C3 C 1.4444(4) 0.2315(2) 0.2460(4) 0.0179(6) Uani 1 d . . O5 O 1.6549(3) 0.22301(12) 0.2329(3) 0.0218(5) Uani 1 d . . H2 H 0.6719(56) 0.0377(23) -0.1379(49) 0.028(10) Uiso 1 d . . H1 H 0.5722(77) 0.1099(26) -0.1316(61) 0.055(14) Uiso 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 Co1 0.0136(2) 0.0133(2) 0.0198(2) 0.0002(2) 0.0018(2) 0.00143(14) Na1 0.0178(6) 0.0246(6) 0.0258(6) 0.0027(5) 0.0039(5) -0.0004(5) O1 0.0330(12) 0.0178(11) 0.0209(10) -0.0021(9) 0.0005(9) 0.0088(9) O7 0.0184(11) 0.0176(11) 0.0229(11) -0.0014(9) 0.0007(9) 0.0014(9) O3 0.0117(10) 0.0252(11) 0.0342(12) 0.0016(9) 0.0046(8) -0.0022(8) C1 0.0180(13) 0.0146(14) 0.0221(14) -0.0015(12) 0.0057(11) -0.0004(11) O6 0.0183(10) 0.0179(11) 0.0481(13) -0.0075(9) 0.0049(10) 0.0022(9) C2 0.0169(13) 0.0205(15) 0.0161(13) 0.0006(12) 0.0047(11) 0.0003(12) O2 0.0282(11) 0.0164(10) 0.0179(10) 0.0002(8) -0.0005(8) 0.0029(8) O4 0.0157(9) 0.0164(10) 0.0347(12) -0.0013(9) 0.0048(9) -0.0011(8) C3 0.0158(14) 0.0164(14) 0.0200(13) -0.0018(11) -0.0001(11) 0.0026(11) O5 0.0139(9) 0.0148(10) 0.0366(12) -0.0015(9) 0.0045(9) 0.0001(8) _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 O5 2.053(2) 1_455 ? Co1 O2 2.063(2) 3_756 ? Co1 O7 2.086(2) . ? Co1 O1 2.094(2) . ? Co1 O3 2.118(2) . ? Co1 O4 2.168(2) 1_455 ? Co1 Na1 3.5061(14) 4_565 ? Na1 O6 2.305(2) . ? Na1 O5 2.329(2) 1_455 ? Na1 O1 2.359(2) 4_565 ? Na1 O7 2.484(2) 4_566 ? Na1 O3 2.549(2) 4_566 ? Na1 O2 2.725(2) 4_565 ? Na1 O3 2.774(2) . ? Na1 C1 2.857(3) 4_565 ? Na1 Co1 3.5062(14) 4_566 ? Na1 Na1 4.0626(13) 4_565 ? Na1 Na1 4.0627(13) 4_566 ? O1 C1 1.255(3) . ? O1 Na1 2.359(2) 4_566 ? O7 Na1 2.484(2) 4_565 ? O3 C2 1.254(3) . ? O3 Na1 2.549(2) 4_565 ? C1 O2 1.255(3) . ? C1 C1 1.540(5) 3_756 ? C1 Na1 2.857(3) 4_566 ? O6 C3 1.235(3) . ? C2 O4 1.254(3) . ? C2 C3 1.545(4) . ? O2 Co1 2.063(2) 3_756 ? O2 Na1 2.726(2) 4_566 ? O4 Co1 2.168(2) 1_655 ? C3 O5 1.261(3) . ? O5 Co1 2.053(2) 1_655 ? O5 Na1 2.329(2) 1_655 ? 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 O5 Co1 O2 168.81(8) 1_455 3_756 ? O5 Co1 O7 97.72(9) 1_455 . ? O2 Co1 O7 93.00(8) 3_756 . ? O5 Co1 O1 89.06(8) 1_455 . ? O2 Co1 O1 80.51(7) 3_756 . ? O7 Co1 O1 172.00(8) . . ? O5 Co1 O3 84.23(8) 1_455 . ? O2 Co1 O3 99.28(8) 3_756 . ? O7 Co1 O3 88.72(8) . . ? O1 Co1 O3 87.75(9) . . ? O5 Co1 O4 78.40(7) 1_455 1_455 ? O2 Co1 O4 98.91(8) 3_756 1_455 ? O7 Co1 O4 87.66(9) . 1_455 ? O1 Co1 O4 97.90(9) . 1_455 ? O3 Co1 O4 161.61(8) . 1_455 ? O5 Co1 Na1 81.71(6) 1_455 4_565 ? O2 Co1 Na1 108.43(6) 3_756 4_565 ? O7 Co1 Na1 44.27(6) . 4_565 ? O1 Co1 Na1 133.56(6) . 4_565 ? O3 Co1 Na1 46.20(6) . 4_565 ? O4 Co1 Na1 124.04(6) 1_455 4_565 ? O6 Na1 O5 129.86(9) . 1_455 ? O6 Na1 O1 91.15(9) . 4_565 ? O5 Na1 O1 98.10(8) 1_455 4_565 ? O6 Na1 O7 145.18(9) . 4_566 ? O5 Na1 O7 84.89(8) 1_455 4_566 ? O1 Na1 O7 84.76(8) 4_565 4_566 ? O6 Na1 O3 90.19(8) . 4_566 ? O5 Na1 O3 112.09(8) 1_455 4_566 ? O1 Na1 O3 138.90(8) 4_565 4_566 ? O7 Na1 O3 71.43(7) 4_566 4_566 ? O6 Na1 O2 75.87(7) . 4_565 ? O5 Na1 O2 143.99(8) 1_455 4_565 ? O1 Na1 O2 51.49(6) 4_565 4_565 ? O7 Na1 O2 74.64(8) 4_566 4_565 ? O3 Na1 O2 89.32(7) 4_566 4_565 ? O6 Na1 O3 64.06(7) . . ? O5 Na1 O3 65.80(7) 1_455 . ? O1 Na1 O3 101.66(8) 4_565 . ? O7 Na1 O3 150.54(8) 4_566 . ? O3 Na1 O3 115.65(7) 4_566 . ? O2 Na1 O3 131.59(7) 4_565 . ? O6 Na1 C1 83.30(8) . 4_565 ? O5 Na1 C1 121.54(9) 1_455 4_565 ? O1 Na1 C1 25.64(7) 4_565 4_565 ? O7 Na1 C1 78.20(8) 4_566 4_565 ? O3 Na1 C1 114.31(8) 4_566 4_565 ? O2 Na1 C1 25.86(7) 4_565 4_565 ? O3 Na1 C1 119.00(8) . 4_565 ? O6 Na1 Co1 124.98(7) . 4_566 ? O5 Na1 Co1 93.30(6) 1_455 4_566 ? O1 Na1 Co1 117.98(7) 4_565 4_566 ? O7 Na1 Co1 35.88(5) 4_566 4_566 ? O3 Na1 Co1 36.84(4) 4_566 4_566 ? O2 Na1 Co1 87.21(5) 4_565 4_566 ? O3 Na1 Co1 137.77(6) . 4_566 ? C1 Na1 Co1 103.23(6) 4_565 4_566 ? O6 Na1 Na1 73.91(6) . 4_565 ? O5 Na1 Na1 66.66(6) 1_455 4_565 ? O1 Na1 Na1 64.16(5) 4_565 4_565 ? O7 Na1 Na1 132.65(6) 4_566 4_565 ? O3 Na1 Na1 153.45(6) 4_566 4_565 ? O2 Na1 Na1 106.62(5) 4_565 4_565 ? O3 Na1 Na1 38.25(5) . 4_565 ? C1 Na1 Na1 85.37(6) 4_565 4_565 ? Co1 Na1 Na1 159.61(3) 4_566 4_565 ? O6 Na1 Na1 98.51(7) . 4_566 ? O5 Na1 Na1 75.23(7) 1_455 4_566 ? O1 Na1 Na1 170.32(6) 4_565 4_566 ? O7 Na1 Na1 87.62(6) 4_566 4_566 ? O3 Na1 Na1 42.36(5) 4_566 4_566 ? O2 Na1 Na1 131.66(5) 4_565 4_566 ? O3 Na1 Na1 82.20(6) . 4_566 ? C1 Na1 Na1 156.30(7) 4_565 4_566 ? Co1 Na1 Na1 56.41(2) 4_566 4_566 ? Na1 Na1 Na1 117.95(6) 4_565 4_566 ? C1 O1 Co1 112.0(2) . . ? C1 O1 Na1 99.9(2) . 4_566 ? Co1 O1 Na1 147.80(10) . 4_566 ? Co1 O7 Na1 99.85(9) . 4_565 ? C2 O3 Co1 141.3(2) . . ? C2 O3 Na1 108.6(2) . 4_565 ? Co1 O3 Na1 96.96(8) . 4_565 ? C2 O3 Na1 109.2(2) . . ? Co1 O3 Na1 94.17(7) . . ? Na1 O3 Na1 99.39(7) 4_565 . ? O1 C1 O2 125.7(2) . . ? O1 C1 C1 116.6(3) . 3_756 ? O2 C1 C1 117.7(3) . 3_756 ? O1 C1 Na1 54.45(13) . 4_566 ? O2 C1 Na1 71.23(15) . 4_566 ? C1 C1 Na1 170.9(3) 3_756 4_566 ? C3 O6 Na1 127.0(2) . . ? O3 C2 O4 127.0(3) . . ? O3 C2 C3 116.4(2) . . ? O4 C2 C3 116.5(2) . . ? C1 O2 Co1 112.4(2) . 3_756 ? C1 O2 Na1 82.9(2) . 4_566 ? Co1 O2 Na1 162.76(9) 3_756 4_566 ? C2 O4 Co1 111.2(2) . 1_655 ? O6 C3 O5 126.0(3) . . ? O6 C3 C2 118.7(2) . . ? O5 C3 C2 115.3(2) . . ? C3 O5 Co1 116.0(2) . 1_655 ? C3 O5 Na1 130.9(2) . 1_655 ? Co1 O5 Na1 110.80(9) 1_655 1_655 ? _refine_diff_density_max 0.309 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.075 #===END