Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Daniel J. Price' 'A. K. Powell' 'Paul T. Wood' _publ_contact_author_name 'Dr Daniel J Price' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton Hampshire SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email daniel.price@soton.ac.uk _publ_contact_author_fax 44(0)2380596805 _publ_contact_author_phone 44(0)2380592987 _publ_section_title ; A new series of layered transition metal oxalates: Hydrothermal synthesis, structural and magnetic studies ; #------------------------------------------------------------- data_1 _database_code_CSD 203681 _chemical_name_systematic ; Dibarium bischlorotrisoxalatodimanganese(II) tetrahydrate' ; _chemical_name_common "Dibarium bischlorotrisoxalatodimanganese(ii) tetrahydrate'" _chemical_formula_moiety 'C12 H16 Ba4 Cl4 Mn4 O32' _chemical_formula_structural 'Ba2 Mn2 Cl2 (C2O4)3 (H2O)4' _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 Ba4 Cl4 Mn4 O32' _chemical_formula_weight 1583.17 _chemical_melting_point N/A _chemical_compound_source 'Hydrothermal synthesis' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.916(5) _cell_length_b 8.248(2) _cell_length_c 9.904(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.53(3) _cell_angle_gamma 90.00 _cell_volume 1846.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 126 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 28.28 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.848 _exptl_crystal_density_method ? _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.913 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_detector_area_resol_mean ? _diffrn_detector_crystal_distance '70 mm' _diffrn_measurement_oscillation_angle 5 _diffrn_measurement_frames_number 36 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6319 _diffrn_reflns_av_R_equivalents 0.1098 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2188 _reflns_number_gt 2095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC RaxisII control software' _computing_cell_refinement ; DENZO and SCALEPACK from the HKL programe suite ; _computing_data_reduction SHELX97-SHELXPRO _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. The structure contains some disorder. One of the water molecules in the coordination sphere of the barium is disordered. The occupancy of the two sites was refined isotropically with the thermal parameters constrained to be equal. This gave occupancies of 67% for O9 anem 33% for O10. These occupancies were then constrained and the thermal parameters (constrained to be equal) were refined anisotropically. The hydrogen atoms of these water molecules could not be found and were not included in the model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+3.0367P] 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 0.0087(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2188 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_all 0.0875 _refine_ls_wR_factor_ref 0.0867 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.080 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ba1 Ba 0.395404(8) 0.18524(2) 0.25499(2) 0.02886(14) Uani 1 d . . Mn1 Mn 0.36864(2) 0.34851(7) 0.61774(5) 0.0292(2) Uani 1 d . . Cl1 Cl 0.46675(4) 0.28905(12) 0.55048(9) 0.0354(2) Uani 1 d . . O1 O 0.37623(14) 0.1506(3) 0.7607(3) 0.0369(5) Uani 1 d . . O2 O 0.39471(14) 0.0912(3) 0.9832(3) 0.0412(6) Uani 1 d . . O3 O 0.37385(12) 0.4089(3) 1.0390(2) 0.0341(5) Uani 1 d . . O4 O 0.37986(11) 0.4695(3) 0.8207(2) 0.0324(5) Uani 1 d . . O5 O 0.31737(11) 0.2297(4) 0.4396(3) 0.0372(5) Uani 1 d . . O6 O 0.22758(12) 0.1255(4) 0.3587(3) 0.0440(6) Uani 1 d . . C1 C 0.3842(2) 0.1882(4) 0.8874(4) 0.0309(7) Uani 1 d . . C2 C 0.37932(14) 0.3716(4) 0.9182(3) 0.0291(6) Uani 1 d . . C3 C 0.2626(2) 0.2084(4) 0.4411(4) 0.0323(7) Uani 1 d . . O7 O 0.5000 0.3860(5) 0.2500 0.0360(7) Uani 1 d S . H7 H 0.4770(36) 0.4401(102) 0.1559(73) 0.111(26) Uiso 1 d . . O8 O 0.5000 0.0084(5) 0.2500 0.0398(9) Uani 1 d S . H8 H 0.5099(28) -0.0336(73) 0.3075(54) 0.056(17) Uiso 1 d . . O9 O 0.2788(7) 0.1230(14) 0.1182(18) 0.062(3) Uani 0.67 d P 1 O10 O 0.2726(17) 0.1740(35) 0.1221(43) 0.062(3) Uani 0.33 d P 1 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 Ba1 0.0319(2) 0.0277(2) 0.0277(2) 0.00058(6) 0.00677(10) 0.00059(6) Mn1 0.0331(3) 0.0283(3) 0.0262(3) 0.0002(2) 0.0052(2) -0.0015(2) Cl1 0.0331(4) 0.0387(4) 0.0345(4) 0.0005(3) 0.0055(3) 0.0014(3) O1 0.056(2) 0.0263(11) 0.0293(12) -0.0035(10) 0.0094(10) 0.0012(12) O2 0.062(2) 0.0298(12) 0.0322(12) 0.0037(10) 0.0079(11) 0.0041(12) O3 0.0487(14) 0.0282(11) 0.0266(10) -0.0023(9) 0.0096(9) 0.0006(10) O4 0.0431(13) 0.0276(11) 0.0267(11) -0.0002(9) 0.0061(9) -0.0024(9) O5 0.0316(12) 0.0485(14) 0.0330(12) -0.0066(12) 0.0098(10) -0.0041(11) O6 0.0350(13) 0.057(2) 0.0414(14) -0.0170(13) 0.0092(10) -0.0079(13) C1 0.037(2) 0.027(2) 0.030(2) -0.0006(11) 0.0090(13) 0.0005(11) C2 0.0334(15) 0.0270(15) 0.0271(14) -0.0022(12) 0.0056(11) -0.0005(12) C3 0.032(2) 0.034(2) 0.032(2) -0.0001(13) 0.0067(13) -0.0006(13) O7 0.036(2) 0.035(2) 0.038(2) 0.000 0.0079(14) 0.000 O8 0.035(2) 0.035(2) 0.049(2) 0.000 0.005(2) 0.000 O9 0.049(4) 0.087(9) 0.052(2) -0.009(6) 0.013(2) -0.004(6) O10 0.049(4) 0.087(9) 0.052(2) -0.009(6) 0.013(2) -0.004(6) _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 Ba1 O5 2.785(2) . ? Ba1 O2 2.799(3) 1_554 ? Ba1 O3 2.805(2) 1_554 ? Ba1 O1 2.807(3) 6 ? Ba1 O8 2.813(2) . ? Ba1 O9 2.83(2) . ? Ba1 O10 2.90(4) . ? Ba1 O7 2.921(2) . ? Ba1 O4 2.956(3) 6_565 ? Ba1 O2 3.212(3) 6 ? Ba1 Cl1 3.2228(13) . ? Ba1 C1 3.374(3) 6 ? Mn1 O1 2.149(3) . ? Mn1 O3 2.158(2) 6_565 ? Mn1 O5 2.184(3) . ? Mn1 O4 2.220(2) . ? Mn1 O6 2.266(3) 7_556 ? Mn1 Cl1 2.4970(12) . ? O1 C1 1.276(4) . ? O1 Ba1 2.807(3) 6_556 ? O2 C1 1.234(4) . ? O2 Ba1 2.799(3) 1_556 ? O2 Ba1 3.212(3) 6_556 ? O3 C2 1.262(4) . ? O3 Mn1 2.158(2) 6_566 ? O3 Ba1 2.805(2) 1_556 ? O4 C2 1.261(4) . ? O4 Ba1 2.956(3) 6_566 ? O5 C3 1.270(5) . ? O6 C3 1.250(5) . ? O6 Mn1 2.266(3) 7_556 ? C1 C2 1.551(4) . ? C1 Ba1 3.374(3) 6_556 ? C3 C3 1.545(7) 7_556 ? O7 Ba1 2.921(2) 2_655 ? O8 Ba1 2.813(2) 2_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 Ba1 O2 139.97(8) . 1_554 ? O5 Ba1 O3 111.27(8) . 1_554 ? O2 Ba1 O3 58.45(7) 1_554 1_554 ? O5 Ba1 O1 89.83(9) . 6 ? O2 Ba1 O1 76.69(8) 1_554 6 ? O3 Ba1 O1 130.98(7) 1_554 6 ? O5 Ba1 O8 136.17(7) . . ? O2 Ba1 O8 73.06(7) 1_554 . ? O3 Ba1 O8 111.74(7) 1_554 . ? O1 Ba1 O8 68.00(10) 6 . ? O5 Ba1 O9 71.4(3) . . ? O2 Ba1 O9 68.6(3) 1_554 . ? O3 Ba1 O9 73.8(3) 1_554 . ? O1 Ba1 O9 72.1(2) 6 . ? O8 Ba1 O9 129.5(2) . . ? O5 Ba1 O10 67.8(7) . . ? O2 Ba1 O10 72.8(7) 1_554 . ? O3 Ba1 O10 68.9(8) 1_554 . ? O1 Ba1 O10 80.5(6) 6 . ? O8 Ba1 O10 137.7(5) . . ? O9 Ba1 O10 8.8(7) . . ? O5 Ba1 O7 123.67(7) . . ? O2 Ba1 O7 90.85(7) 1_554 . ? O3 Ba1 O7 69.86(7) 1_554 . ? O1 Ba1 O7 133.76(9) 6 . ? O8 Ba1 O7 65.77(11) . . ? O9 Ba1 O7 143.7(3) . . ? O10 Ba1 O7 138.3(7) . . ? O5 Ba1 O4 67.34(8) . 6_565 ? O2 Ba1 O4 119.80(7) 1_554 6_565 ? O3 Ba1 O4 61.44(6) 1_554 6_565 ? O1 Ba1 O4 157.14(7) 6 6_565 ? O8 Ba1 O4 129.60(9) . 6_565 ? O9 Ba1 O4 98.1(2) . 6_565 ? O10 Ba1 O4 89.3(5) . 6_565 ? O7 Ba1 O4 65.58(8) . 6_565 ? O5 Ba1 O2 63.46(8) . 6 ? O2 Ba1 O2 118.69(3) 1_554 6 ? O3 Ba1 O2 169.20(8) 1_554 6 ? O1 Ba1 O2 42.80(7) 6 6 ? O8 Ba1 O2 75.40(8) . 6 ? O9 Ba1 O2 95.4(3) . 6 ? O10 Ba1 O2 100.3(8) . 6 ? O7 Ba1 O2 120.94(7) . 6 ? O4 Ba1 O2 120.94(7) 6_565 6 ? O5 Ba1 Cl1 69.72(6) . . ? O2 Ba1 Cl1 150.25(7) 1_554 . ? O3 Ba1 Cl1 121.09(6) 1_554 . ? O1 Ba1 Cl1 107.55(6) 6 . ? O8 Ba1 Cl1 81.26(4) . . ? O9 Ba1 Cl1 141.1(3) . . ? O10 Ba1 Cl1 136.7(7) . . ? O7 Ba1 Cl1 64.55(3) . . ? O4 Ba1 Cl1 66.78(5) 6_565 . ? O2 Ba1 Cl1 67.08(5) 6 . ? O5 Ba1 C1 76.52(9) . 6 ? O2 Ba1 C1 97.59(8) 1_554 6 ? O3 Ba1 C1 151.81(8) 1_554 6 ? O1 Ba1 C1 21.41(8) 6 6 ? O8 Ba1 C1 69.71(10) . 6 ? O9 Ba1 C1 83.9(3) . 6 ? O10 Ba1 C1 91.0(7) . 6 ? O7 Ba1 C1 129.75(9) . 6 ? O4 Ba1 C1 140.75(7) 6_565 6 ? O2 Ba1 C1 21.41(8) 6 6 ? Cl1 Ba1 C1 87.09(7) . 6 ? O1 Mn1 O3 159.90(10) . 6_565 ? O1 Mn1 O5 99.53(11) . . ? O3 Mn1 O5 100.30(11) 6_565 . ? O1 Mn1 O4 76.15(10) . . ? O3 Mn1 O4 84.55(9) 6_565 . ? O5 Mn1 O4 154.07(9) . . ? O1 Mn1 O6 88.75(12) . 7_556 ? O3 Mn1 O6 93.57(11) 6_565 7_556 ? O5 Mn1 O6 73.92(10) . 7_556 ? O4 Mn1 O6 80.39(10) . 7_556 ? O1 Mn1 Cl1 92.77(9) . . ? O3 Mn1 Cl1 88.84(7) 6_565 . ? O5 Mn1 Cl1 94.82(7) . . ? O4 Mn1 Cl1 110.82(8) . . ? O6 Mn1 Cl1 168.73(8) 7_556 . ? O1 Mn1 Ba1 109.27(7) . . ? O3 Mn1 Ba1 87.80(6) 6_565 . ? O5 Mn1 Ba1 42.36(6) . . ? O4 Mn1 Ba1 163.24(7) . . ? O6 Mn1 Ba1 115.04(8) 7_556 . ? Cl1 Mn1 Ba1 54.01(3) . . ? Mn1 Cl1 Ba1 87.17(4) . . ? C1 O1 Mn1 116.5(2) . . ? C1 O1 Ba1 105.2(2) . 6_556 ? Mn1 O1 Ba1 137.09(11) . 6_556 ? C1 O2 Ba1 121.9(2) . 1_556 ? C1 O2 Ba1 86.7(2) . 6_556 ? Ba1 O2 Ba1 150.86(10) 1_556 6_556 ? C2 O3 Mn1 126.0(2) . 6_566 ? C2 O3 Ba1 122.0(2) . 1_556 ? Mn1 O3 Ba1 110.34(9) 6_566 1_556 ? C2 O4 Mn1 113.0(2) . . ? C2 O4 Ba1 143.4(2) . 6_566 ? Mn1 O4 Ba1 103.53(8) . 6_566 ? C3 O5 Mn1 116.9(2) . . ? C3 O5 Ba1 137.1(2) . . ? Mn1 O5 Ba1 105.75(10) . . ? C3 O6 Mn1 114.3(2) . 7_556 ? O2 C1 O1 125.2(3) . . ? O2 C1 C2 119.5(3) . . ? O1 C1 C2 115.3(3) . . ? O2 C1 Ba1 71.9(2) . 6_556 ? O1 C1 Ba1 53.4(2) . 6_556 ? C2 C1 Ba1 168.4(2) . 6_556 ? O4 C2 O3 125.9(3) . . ? O4 C2 C1 117.6(3) . . ? O3 C2 C1 116.5(3) . . ? O6 C3 O5 126.7(3) . . ? O6 C3 C3 117.1(4) . 7_556 ? O5 C3 C3 116.2(4) . 7_556 ? Ba1 O7 Ba1 110.91(13) . 2_655 ? Ba1 O8 Ba1 117.5(2) . 2_655 ? _refine_diff_density_max 1.882 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.188 #==END #------------------------------------------------------------------ data_2 _database_code_CSD 203682 _chemical_name_systematic ; Dibarium bischlorotrisoxalatodiiron(II) tetrahydrate' ; _chemical_name_common "Dibarium bischlorotrisoxalatodiiron(ii) tetrahydrate'" _chemical_formula_moiety 'C12 H16, Ba4, Cl4 Fe4 O32' _chemical_formula_structural 'Ba2 Fe2 Cl2 (C2O4)3 (H2O)4' _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 Ba4 Cl4 Fe4 O32' _chemical_formula_weight 1586.82 _chemical_melting_point n/a _chemical_compound_source 'hydrothermal synthesis' 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.798(5) _cell_length_b 8.297(2) _cell_length_c 9.849(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.90(3) _cell_angle_gamma 90.00 _cell_volume 1835.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 24.01 _exptl_crystal_description 'diamond shaped plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.871 _exptl_crystal_density_method ? _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 6.153 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2724 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 24.69 _reflns_number_total 1481 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'msc RaxisII control software' _computing_cell_refinement ; DENZO and SCALEPACK from the HKL programe suite ; _computing_data_reduction SHELX97-SHELXPRO _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 1 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^)+(0.0281P)^2^+2.8513P] 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 0.0017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1480 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_all 0.0839 _refine_ls_wR_factor_ref 0.0495 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.797 _refine_ls_restrained_S_obs 1.075 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ba1 Ba 0.104812(7) 0.18354(2) 0.74825(2) 0.01415(12) Uani 1 d . . Fe1 Fe 0.13355(2) 0.35300(5) 0.38590(4) 0.01419(14) Uani 1 d . . Cl1 Cl 0.03551(3) 0.29385(9) 0.44854(8) 0.0208(2) Uani 1 d . . O1 O 0.12617(11) 0.1548(2) 0.2486(2) 0.0224(5) Uani 1 d . . O2 O 0.10552(10) 0.0927(2) 0.0244(2) 0.0259(5) Uani 1 d . . O3 O 0.12846(9) 0.4118(2) -0.0323(2) 0.0182(4) Uani 1 d . . O4 O 0.12015(8) 0.4719(2) 0.1864(2) 0.0178(4) Uani 1 d . . O5 O 0.18288(8) 0.2325(3) 0.5617(2) 0.0217(4) Uani 1 d . . O6 O 0.27204(9) 0.1193(3) 0.6386(2) 0.0267(5) Uani 1 d . . C1 C 0.11708(13) 0.1910(3) 0.1204(3) 0.0160(6) Uani 1 d . . C2 C 0.12202(11) 0.3750(3) 0.0885(3) 0.0141(5) Uani 1 d . . C3 C 0.23716(13) 0.2069(3) 0.5584(3) 0.0160(6) Uani 1 d . . O7 O 0.0000 0.3816(4) 0.7500 0.0226(7) Uani 1 d S . H7 H 0.0062(20) 0.4431(56) 0.8119(44) 0.051(13) Uiso 1 d . . O8 O 0.0000 0.0033(4) 0.7500 0.0254(7) Uani 1 d S . H8 H -0.0124(18) -0.0575(53) 0.6790(42) 0.043(12) Uiso 1 d . . O9 O 0.2222(17) 0.1198(43) 0.8711(32) 0.043(4) Uani 0.53 d P 1 O10 O 0.2255(20) 0.1536(51) 0.8949(38) 0.043(4) Uani 0.47 d P 1 H9A H 0.2442(36) 0.1041(99) 0.9583(99) 0.142(32) Uiso 1 d . . H9B H 0.2419(35) 0.1287(98) 0.8299(82) 0.114(30) 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 Ba1 0.0174(2) 0.0104(2) 0.0153(2) -0.00058(5) 0.00462(9) -0.00050(5) Fe1 0.0187(2) 0.0115(2) 0.0126(2) 0.0000(2) 0.0032(2) 0.0015(2) Cl1 0.0195(4) 0.0213(4) 0.0214(4) -0.0010(3) 0.0031(3) -0.0015(3) O1 0.0379(12) 0.0120(9) 0.0180(12) 0.0027(8) 0.0070(9) -0.0009(9) O2 0.0463(13) 0.0138(10) 0.0180(11) -0.0041(9) 0.0065(10) -0.0050(9) O3 0.0300(10) 0.0134(9) 0.0118(10) 0.0019(8) 0.0056(8) 0.0006(8) O4 0.0272(10) 0.0110(9) 0.0151(11) -0.0016(8) 0.0034(8) 0.0035(8) O5 0.0169(10) 0.0283(11) 0.0209(11) 0.0069(9) 0.0056(8) 0.0031(9) O6 0.0206(10) 0.0333(12) 0.0270(12) 0.0161(10) 0.0066(9) 0.0078(10) C1 0.0207(15) 0.0112(14) 0.018(2) 0.0011(11) 0.0077(13) -0.0005(10) C2 0.0139(12) 0.0115(13) 0.0170(14) 0.0008(12) 0.0026(10) 0.0002(10) C3 0.0163(14) 0.0166(13) 0.015(2) -0.0015(12) 0.0040(12) -0.0013(11) O7 0.026(2) 0.016(2) 0.026(2) 0.000 0.0066(14) 0.000 O8 0.0216(15) 0.0146(15) 0.038(2) 0.000 0.0003(14) 0.000 O9 0.033(4) 0.074(14) 0.019(9) -0.017(6) 0.001(6) 0.006(7) O10 0.033(4) 0.074(14) 0.019(9) -0.017(6) 0.001(6) 0.006(7) _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 Ba1 O9 2.79(4) . ? Ba1 O5 2.799(2) . ? Ba1 O2 2.819(2) 1_556 ? Ba1 O8 2.822(2) . ? Ba1 O1 2.849(2) 6_556 ? Ba1 O3 2.854(2) 1_556 ? Ba1 O10 2.89(4) . ? Ba1 O7 2.903(2) . ? Ba1 O4 2.956(2) 6_566 ? Ba1 O2 3.183(2) 6_556 ? Ba1 Cl1 3.2317(12) . ? Ba1 C1 3.383(3) 6_556 ? Fe1 O1 2.118(2) . ? Fe1 O3 2.122(2) 6_566 ? Fe1 O5 2.143(2) . ? Fe1 O4 2.173(2) . ? Fe1 O6 2.219(2) 7_556 ? Fe1 Cl1 2.4679(9) . ? O1 C1 1.280(4) . ? O1 Ba1 2.849(2) 6 ? O2 C1 1.242(4) . ? O2 Ba1 2.819(2) 1_554 ? O2 Ba1 3.183(2) 6 ? O3 C2 1.262(3) . ? O3 Fe1 2.122(2) 6_565 ? O3 Ba1 2.854(2) 1_554 ? O4 C2 1.262(3) . ? O4 Ba1 2.956(2) 6_565 ? O5 C3 1.262(4) . ? O6 C3 1.252(4) . ? O6 Fe1 2.219(2) 7_556 ? C1 C2 1.566(3) . ? C1 Ba1 3.383(3) 6 ? C3 C3 1.552(6) 7_556 ? O7 Ba1 2.903(2) 2_556 ? O8 Ba1 2.822(2) 2_556 ? 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 O9 Ba1 O5 69.0(8) . . ? O9 Ba1 O2 71.6(8) . 1_556 ? O5 Ba1 O2 140.64(6) . 1_556 ? O9 Ba1 O8 130.3(9) . . ? O5 Ba1 O8 135.70(5) . . ? O2 Ba1 O8 73.55(5) 1_556 . ? O9 Ba1 O1 70.2(7) . 6_556 ? O5 Ba1 O1 90.91(6) . 6_556 ? O2 Ba1 O1 76.29(6) 1_556 6_556 ? O8 Ba1 O1 67.82(7) . 6_556 ? O9 Ba1 O3 75.8(4) . 1_556 ? O5 Ba1 O3 110.00(6) . 1_556 ? O2 Ba1 O3 58.54(6) 1_556 1_556 ? O8 Ba1 O3 113.40(5) . 1_556 ? O1 Ba1 O3 130.01(6) 6_556 1_556 ? O9 Ba1 O10 7.1(10) . . ? O5 Ba1 O10 71.5(9) . . ? O2 Ba1 O10 69.4(9) 1_556 . ? O8 Ba1 O10 133.3(10) . . ? O1 Ba1 O10 76.5(8) 6_556 . ? O3 Ba1 O10 68.8(6) 1_556 . ? O9 Ba1 O7 146.5(4) . . ? O5 Ba1 O7 122.60(6) . . ? O2 Ba1 O7 90.80(5) 1_556 . ? O8 Ba1 O7 66.50(8) . . ? O1 Ba1 O7 134.31(7) 6_556 . ? O3 Ba1 O7 70.64(5) 1_556 . ? O10 Ba1 O7 139.4(6) . . ? O9 Ba1 O4 97.7(8) . 6_566 ? O5 Ba1 O4 67.24(6) . 6_566 ? O2 Ba1 O4 118.43(6) 1_556 6_566 ? O8 Ba1 O4 130.10(6) . 6_566 ? O1 Ba1 O4 157.94(6) 6_556 6_566 ? O3 Ba1 O4 60.06(5) 1_556 6_566 ? O10 Ba1 O4 92.9(9) . 6_566 ? O7 Ba1 O4 65.19(6) . 6_566 ? O9 Ba1 O2 92.6(4) . 6_556 ? O5 Ba1 O2 64.54(6) . 6_556 ? O2 Ba1 O2 118.42(3) 1_556 6_556 ? O8 Ba1 O2 74.20(6) . 6_556 ? O1 Ba1 O2 43.10(6) 6_556 6_556 ? O3 Ba1 O2 168.42(6) 1_556 6_556 ? O10 Ba1 O2 99.6(6) . 6_556 ? O7 Ba1 O2 120.94(6) . 6_556 ? O4 Ba1 O2 122.60(5) 6_566 6_556 ? O9 Ba1 Cl1 137.0(8) . . ? O5 Ba1 Cl1 68.00(5) . . ? O2 Ba1 Cl1 151.36(5) 1_556 . ? O8 Ba1 Cl1 82.77(3) . . ? O1 Ba1 Cl1 109.67(5) 6_556 . ? O3 Ba1 Cl1 120.18(4) 1_556 . ? O10 Ba1 Cl1 139.0(9) . . ? O7 Ba1 Cl1 64.62(2) . . ? O4 Ba1 Cl1 66.07(4) 6_566 . ? O2 Ba1 Cl1 68.35(4) 6_556 . ? O9 Ba1 C1 81.5(5) . 6_556 ? O5 Ba1 C1 77.66(7) . 6_556 ? O2 Ba1 C1 97.26(7) 1_556 6_556 ? O8 Ba1 C1 68.88(7) . 6_556 ? O1 Ba1 C1 21.59(7) 6_556 6_556 ? O3 Ba1 C1 150.98(7) 1_556 6_556 ? O10 Ba1 C1 88.5(7) . 6_556 ? O7 Ba1 C1 130.03(7) . 6_556 ? O4 Ba1 C1 142.31(6) 6_566 6_556 ? O2 Ba1 C1 21.54(7) 6_556 6_556 ? Cl1 Ba1 C1 88.79(6) . 6_556 ? O1 Fe1 O3 162.39(8) . 6_566 ? O1 Fe1 O5 97.29(9) . . ? O3 Fe1 O5 100.24(8) 6_566 . ? O1 Fe1 O4 77.98(7) . . ? O3 Fe1 O4 85.24(8) 6_566 . ? O5 Fe1 O4 156.22(7) . . ? O1 Fe1 O6 89.01(9) . 7_556 ? O3 Fe1 O6 93.64(8) 6_566 7_556 ? O5 Fe1 O6 75.64(8) . 7_556 ? O4 Fe1 O6 80.95(8) . 7_556 ? O1 Fe1 Cl1 91.68(7) . . ? O3 Fe1 Cl1 88.69(6) 6_566 . ? O5 Fe1 Cl1 94.43(6) . . ? O4 Fe1 Cl1 108.89(6) . . ? O6 Fe1 Cl1 170.05(6) 7_556 . ? Fe1 Cl1 Ba1 87.89(3) . . ? C1 O1 Fe1 115.4(2) . . ? C1 O1 Ba1 103.4(2) . 6 ? Fe1 O1 Ba1 139.53(9) . 6 ? C1 O2 Ba1 121.6(2) . 1_554 ? C1 O2 Ba1 88.3(2) . 6 ? Ba1 O2 Ba1 149.43(7) 1_554 6 ? C2 O3 Fe1 127.1(2) . 6_565 ? C2 O3 Ba1 121.1(2) . 1_554 ? Fe1 O3 Ba1 109.79(8) 6_565 1_554 ? C2 O4 Fe1 112.5(2) . . ? C2 O4 Ba1 142.6(2) . 6_565 ? Fe1 O4 Ba1 104.83(7) . 6_565 ? C3 O5 Fe1 116.0(2) . . ? C3 O5 Ba1 136.9(2) . . ? Fe1 O5 Ba1 107.07(7) . . ? C3 O6 Fe1 113.2(2) . 7_556 ? O2 C1 O1 125.0(2) . . ? O2 C1 C2 120.0(3) . . ? O1 C1 C2 114.9(2) . . ? O2 C1 Ba1 70.12(15) . 6 ? O1 C1 Ba1 55.00(13) . 6 ? C2 C1 Ba1 169.5(2) . 6 ? O4 C2 O3 126.3(2) . . ? O4 C2 C1 117.1(2) . . ? O3 C2 C1 116.7(2) . . ? O6 C3 O5 126.9(3) . . ? O6 C3 C3 117.1(3) . 7_556 ? O5 C3 C3 116.0(3) . 7_556 ? Ba1 O7 Ba1 111.03(10) . 2_556 ? Ba1 O8 Ba1 115.98(11) . 2_556 ? _refine_diff_density_max 0.702 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.125 #==END #--------------------------------------------------------------------- data_3 _database_code_CSD 203683 _chemical_name_systematic ; Dibarium bischlorotrisoxalatodicobalt(II) tetrahydrate ; _chemical_name_common 'Dibarium bischlorotrisoxalatodicobalt(ii) tetrahydrate' _chemical_formula_moiety 'C12 H16 Ba4 Cl4 Co4 O32' _chemical_formula_structural 'Ba2 Co2 Cl2 (C2O4)3(H2O)4' _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 Ba4 Cl4 Co4 O32' _chemical_formula_weight 1599.13 _chemical_melting_point N/A _chemical_compound_source 'Hydrothermal synthesis' 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' Cl Cl 0.1484 0.1585 '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' Ba Ba -0.3244 2.2819 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.675(5) _cell_length_b 8.230(2) _cell_length_c 9.757(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.00(3) _cell_angle_gamma 90.00 _cell_volume 1793.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.126 _exptl_crystal_size_mid 0.084 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.962 _exptl_crystal_density_method ? _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 6.529 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 R-axis IIc' _diffrn_measurement_method 'image plate oscillation photographs' _diffrn_detector_area_resol_mean ? _diffrn_detector_crystal_distance '70 mm' _diffrn_measurement_oscillation_angle 5 _diffrn_measurement_frames_number 45 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7235 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2195 _reflns_number_gt 1853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC RaxisII control software' _computing_cell_refinement ; DENZO and SCALEPACK from The HKL Programe suite ; _computing_data_reduction SHELX97-SHELXPRO _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. The structure contains some disorder. One of the water molecules in the coordination sphere of the barium is disordered. The occupancy of the two sites was refined isotropically with the thermal parameters constrained to be equal. This gave occupancies of 50% for O9 anem 50% for O10. These occupancies were then constrained and the thermal parameters (constrained to be equal) were refined anisotropically. The hydrogen atoms of these water molecules could not be found and were not included in the model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] 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 0.00156(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2195 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_all 0.0784 _refine_ls_wR_factor_ref 0.0760 _refine_ls_goodness_of_fit_all 0.989 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 0.989 _refine_ls_restrained_S_obs 1.049 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ba1 Ba 0.105139(11) 0.18198(3) 0.25112(2) 0.02334(11) Uani 1 d . . Co1 Co 0.13500(3) 0.35627(6) -0.11155(6) 0.02292(15) Uani 1 d . . Cl1 Cl 0.03749(5) 0.29620(13) -0.05218(11) 0.0296(2) Uani 1 d . . O1 O 0.1275(2) 0.1574(3) -0.2448(3) 0.0296(7) Uani 1 d . . O2 O 0.1059(2) 0.0941(4) -0.4695(3) 0.0339(7) Uani 1 d . . O3 O 0.13013(13) 0.4128(3) -0.5284(3) 0.0264(6) Uani 1 d . . O4 O 0.12028(14) 0.4744(3) -0.3084(3) 0.0249(6) Uani 1 d . . O5 O 0.18269(13) 0.2328(4) 0.0641(3) 0.0295(6) Uani 1 d . . O6 O 0.27205(14) 0.1159(4) 0.1378(3) 0.0352(7) Uani 1 d . . C1 C 0.1181(2) 0.1930(5) -0.3733(5) 0.0250(8) Uani 1 d . . C2 C 0.1230(2) 0.3767(5) -0.4060(4) 0.0223(8) Uani 1 d . . C3 C 0.2369(2) 0.2062(5) 0.0585(4) 0.0248(8) Uani 1 d . . O7 O 0.0000 0.3789(6) 0.2500 0.0330(10) Uani 1 d S . H7 H 0.0001(31) 0.4338(69) 0.3102(61) 0.049(19) Uiso 1 d . . O8 O 0.0000 0.0005(6) 0.2500 0.0337(10) Uani 1 d S . H8 H -0.0117(28) -0.0499(70) 0.1769(59) 0.046(17) Uiso 1 d . . O9 O 0.2286(14) 0.1541(32) 0.3920(35) 0.041(3) Uani 0.50 d P 1 O10 O 0.2209(14) 0.1119(32) 0.3767(35) 0.041(3) Uani 0.50 d P 1 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 Ba1 0.0261(2) 0.0238(2) 0.0206(2) -0.00046(8) 0.00517(10) -0.00060(9) Co1 0.0268(3) 0.0240(3) 0.0180(3) 0.0001(2) 0.0039(2) 0.0010(2) Cl1 0.0284(5) 0.0339(5) 0.0261(5) -0.0008(4) 0.0035(4) -0.0014(4) O1 0.048(2) 0.0210(14) 0.020(2) 0.0013(10) 0.0067(13) -0.0016(13) O2 0.054(2) 0.0248(14) 0.024(2) -0.0043(12) 0.0078(15) -0.0036(14) O3 0.037(2) 0.0243(14) 0.0189(14) 0.0012(11) 0.0066(12) -0.0017(12) O4 0.0343(15) 0.0216(13) 0.0184(14) -0.0006(10) 0.0030(12) 0.0035(12) O5 0.0256(15) 0.040(2) 0.023(2) 0.0079(12) 0.0063(12) 0.0057(13) O6 0.026(2) 0.045(2) 0.036(2) 0.0159(15) 0.0076(14) 0.0059(14) C1 0.031(2) 0.021(2) 0.025(2) 0.0016(15) 0.010(2) -0.001(2) C2 0.025(2) 0.024(2) 0.017(2) 0.0022(14) 0.0033(15) 0.001(2) C3 0.025(2) 0.027(2) 0.022(2) 0.001(2) 0.004(2) 0.000(2) O7 0.033(2) 0.031(2) 0.036(3) 0.000 0.009(2) 0.000 O8 0.030(2) 0.029(2) 0.041(3) 0.000 0.005(2) 0.000 O9 0.033(7) 0.057(12) 0.029(6) -0.012(7) -0.003(5) -0.011(6) O10 0.033(7) 0.057(12) 0.029(6) -0.012(7) -0.003(5) -0.011(6) _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 Ba1 O10 2.76(3) . ? Ba1 O5 2.777(3) . ? Ba1 O8 2.812(3) . ? Ba1 O2 2.818(3) 1_556 ? Ba1 O1 2.838(3) 6_556 ? Ba1 O3 2.852(3) 1_556 ? Ba1 O7 2.881(3) . ? Ba1 O9 2.90(3) . ? Ba1 O4 2.919(3) 6_566 ? Ba1 O2 3.132(3) 6_556 ? Ba1 Cl1 3.2277(14) . ? Ba1 C1 3.348(4) 6_556 ? Co1 O3 2.077(3) 6_566 ? Co1 O1 2.079(3) . ? Co1 O5 2.120(3) . ? Co1 O4 2.126(3) . ? Co1 O6 2.179(3) 7 ? Co1 Cl1 2.4318(13) . ? O1 C1 1.269(5) . ? O1 Ba1 2.838(3) 6 ? O2 C1 1.237(5) . ? O2 Ba1 2.817(3) 1_554 ? O2 Ba1 3.132(3) 6 ? O3 C2 1.268(5) . ? O3 Co1 2.077(3) 6_565 ? O3 Ba1 2.852(3) 1_554 ? O4 C2 1.256(5) . ? O4 Ba1 2.919(3) 6_565 ? O5 C3 1.259(5) . ? O6 C3 1.254(5) . ? O6 Co1 2.179(3) 7 ? C1 C2 1.553(5) . ? C1 Ba1 3.347(4) 6 ? C3 C3 1.553(8) 7 ? O7 Ba1 2.881(3) 2 ? O8 Ba1 2.812(3) 2 ? 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 O10 Ba1 O5 70.2(8) . . ? O10 Ba1 O8 129.2(6) . . ? O5 Ba1 O8 135.29(8) . . ? O10 Ba1 O2 70.8(8) . 1_556 ? O5 Ba1 O2 140.95(10) . 1_556 ? O8 Ba1 O2 74.33(8) . 1_556 ? O10 Ba1 O1 68.5(4) . 6_556 ? O5 Ba1 O1 91.47(10) . 6_556 ? O8 Ba1 O1 68.06(11) . 6_556 ? O2 Ba1 O1 76.28(9) 1_556 6_556 ? O10 Ba1 O3 75.8(5) . 1_556 ? O5 Ba1 O3 109.26(9) . 1_556 ? O8 Ba1 O3 114.46(8) . 1_556 ? O2 Ba1 O3 58.27(8) 1_556 1_556 ? O1 Ba1 O3 129.29(9) 6_556 1_556 ? O10 Ba1 O7 147.4(5) . . ? O5 Ba1 O7 122.05(8) . . ? O8 Ba1 O7 66.31(12) . . ? O2 Ba1 O7 90.79(8) 1_556 . ? O1 Ba1 O7 134.37(12) 6_556 . ? O3 Ba1 O7 71.59(8) 1_556 . ? O10 Ba1 O9 7.6(9) . . ? O5 Ba1 O9 69.8(7) . . ? O8 Ba1 O9 134.9(6) . . ? O2 Ba1 O9 71.3(7) 1_556 . ? O1 Ba1 O9 76.1(5) 6_556 . ? O3 Ba1 O9 69.3(5) 1_556 . ? O7 Ba1 O9 140.8(5) . . ? O10 Ba1 O4 98.9(5) . 6_566 ? O5 Ba1 O4 67.28(9) . 6_566 ? O8 Ba1 O4 130.00(10) . 6_566 ? O2 Ba1 O4 117.37(8) 1_556 6_566 ? O1 Ba1 O4 158.35(9) 6_556 6_566 ? O3 Ba1 O4 59.33(8) 1_556 6_566 ? O7 Ba1 O4 65.17(10) . 6_566 ? O9 Ba1 O4 91.9(6) . 6_566 ? O10 Ba1 O2 92.0(5) . 6_556 ? O5 Ba1 O2 65.05(9) . 6_556 ? O8 Ba1 O2 73.59(9) . 6_556 ? O2 Ba1 O2 118.61(4) 1_556 6_556 ? O1 Ba1 O2 43.39(8) 6_556 6_556 ? O3 Ba1 O2 167.84(9) 1_556 6_556 ? O7 Ba1 O2 120.56(9) . 6_556 ? O9 Ba1 O2 98.5(5) . 6_556 ? O4 Ba1 O2 123.47(8) 6_566 6_556 ? O10 Ba1 Cl1 137.1(8) . . ? O5 Ba1 Cl1 66.92(7) . . ? O8 Ba1 Cl1 83.31(5) . . ? O2 Ba1 Cl1 152.10(8) 1_556 . ? O1 Ba1 Cl1 110.79(7) 6_556 . ? O3 Ba1 Cl1 119.88(6) 1_556 . ? O7 Ba1 Cl1 64.63(3) . . ? O9 Ba1 Cl1 136.2(7) . . ? O4 Ba1 Cl1 65.74(6) 6_566 . ? O2 Ba1 Cl1 68.87(6) 6_556 . ? O10 Ba1 C1 80.3(4) . 6_556 ? O5 Ba1 C1 78.17(10) . 6_556 ? O8 Ba1 C1 68.70(11) . 6_556 ? O2 Ba1 C1 97.36(9) 1_556 6_556 ? O1 Ba1 C1 21.73(10) 6_556 6_556 ? O3 Ba1 C1 150.34(10) 1_556 6_556 ? O7 Ba1 C1 129.93(11) . 6_556 ? O9 Ba1 C1 87.7(5) . 6_556 ? O4 Ba1 C1 143.15(9) 6_566 6_556 ? O2 Ba1 C1 21.68(9) 6_556 6_556 ? Cl1 Ba1 C1 89.64(8) . 6_556 ? O3 Co1 O1 163.88(12) 6_566 . ? O3 Co1 O5 100.20(13) 6_566 . ? O1 Co1 O5 95.91(13) . . ? O3 Co1 O4 85.63(11) 6_566 . ? O1 Co1 O4 79.18(11) . . ? O5 Co1 O4 157.99(12) . . ? O3 Co1 O6 93.90(13) 6_566 7 ? O1 Co1 O6 89.14(14) . 7 ? O5 Co1 O6 77.14(11) . 7 ? O4 Co1 O6 81.32(12) . 7 ? O3 Co1 Cl1 88.89(9) 6_566 . ? O1 Co1 Cl1 90.56(11) . . ? O5 Co1 Cl1 93.86(9) . . ? O4 Co1 Cl1 107.54(9) . . ? O6 Co1 Cl1 170.91(9) 7 . ? Co1 Cl1 Ba1 88.31(4) . . ? C1 O1 Co1 114.7(3) . . ? C1 O1 Ba1 102.4(2) . 6 ? Co1 O1 Ba1 141.16(14) . 6 ? C1 O2 Ba1 121.9(3) . 1_554 ? C1 O2 Ba1 89.0(2) . 6 ? Ba1 O2 Ba1 148.35(11) 1_554 6 ? C2 O3 Co1 127.3(3) . 6_565 ? C2 O3 Ba1 120.9(2) . 1_554 ? Co1 O3 Ba1 109.38(11) 6_565 1_554 ? C2 O4 Co1 111.8(2) . . ? C2 O4 Ba1 142.5(2) . 6_565 ? Co1 O4 Ba1 105.59(10) . 6_565 ? C3 O5 Co1 114.4(3) . . ? C3 O5 Ba1 137.4(3) . . ? Co1 O5 Ba1 108.12(11) . . ? C3 O6 Co1 112.9(3) . 7 ? O2 C1 O1 125.1(4) . . ? O2 C1 C2 119.9(4) . . ? O1 C1 C2 115.0(3) . . ? O2 C1 Ba1 69.3(2) . 6 ? O1 C1 Ba1 55.9(2) . 6 ? C2 C1 Ba1 170.3(3) . 6 ? O4 C2 O3 126.5(4) . . ? O4 C2 C1 116.9(3) . . ? O3 C2 C1 116.6(3) . . ? O6 C3 O5 126.7(4) . . ? O6 C3 C3 116.4(4) . 7 ? O5 C3 C3 116.9(5) . 7 ? Ba1 O7 Ba1 111.6(2) . 2 ? Ba1 O8 Ba1 115.8(2) . 2 ? _refine_diff_density_max 1.264 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.172 #==END