# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Jiang-Gao Mao.' 'Pei-Xin Li.' _publ_contact_author_name 'Jiang-Gao Mao' _publ_contact_author_email MJG@MS.FJIRSM.AC.CN _publ_section_title ; Hydrothermal synthese, crystal structures and magnetic properties of two new mixed metal copper(I) sulfites ; # Attachment 'lpx-dalton-cif.CIF' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 743942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu H10 Mn2 Na3 O17 S4' _chemical_formula_weight 652.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cu Cu 0.3201 1.2651 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.663(2) _cell_length_b 14.393(3) _cell_length_c 7.799(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.655(3) _cell_angle_gamma 90.00 _cell_volume 845.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2567 _cell_measurement_theta_min 2.7046 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1600 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 3.373 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9324 _exptl_absorpt_correction_T_max 1.0000 _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 Saturn70 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6522 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1985 _reflns_number_gt 1820 _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 ? _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^)+(0.0261P)^2^+0.7572P] 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 0.0017(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1985 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Mn1 Mn 0.23531(4) 0.111002(19) 0.65779(4) 0.01337(10) Uani 1 1 d . . . Cu1 Cu 0.69639(4) 0.2500 0.72264(4) 0.01338(10) Uani 1 2 d S . . Na1 Na 0.52955(16) -0.09733(7) 0.80625(13) 0.0407(3) Uani 1 1 d . . . Na2 Na 0.85762(17) 0.2500 0.21634(15) 0.0243(3) Uani 1 2 d S . . S1 S 0.48668(8) 0.2500 0.47292(8) 0.01073(14) Uani 1 2 d S . . S2 S 0.95273(8) 0.2500 0.61420(8) 0.01080(14) Uani 1 2 d S . . S3 S 0.64835(6) 0.11984(3) 0.87059(6) 0.01106(11) Uani 1 1 d . . . O1 O 0.36706(18) 0.16510(9) 0.46097(18) 0.0177(3) Uani 1 1 d . . . O2 O 0.5598(3) 0.2500 0.3079(2) 0.0167(4) Uani 1 2 d S . . O3 O 0.96699(17) 0.16540(9) 0.50188(18) 0.0156(3) Uani 1 1 d . . . O4 O 1.1308(2) 0.2500 0.7429(2) 0.0156(4) Uani 1 2 d S . . O5 O 0.70909(19) 0.03290(9) 0.79058(18) 0.0180(3) Uani 1 1 d . . . O6 O 0.45140(18) 0.10600(10) 0.87122(18) 0.0192(3) Uani 1 1 d . . . O7 O 0.73538(19) 0.11989(10) 1.05931(17) 0.0175(3) Uani 1 1 d . . . O1W O 0.0775(2) 0.03441(13) 0.8122(2) 0.0312(4) Uani 1 1 d . . . H1WA H 0.122(4) -0.011(2) 0.862(4) 0.036(8) Uiso 1 1 d . . . H1WB H -0.030(4) 0.037(2) 0.801(4) 0.038(8) Uiso 1 1 d . . . O2W O 0.2853(2) -0.02576(11) 0.5562(2) 0.0209(3) Uani 1 1 d . . . H2WA H 0.212(4) -0.065(2) 0.552(3) 0.023(7) Uiso 1 1 d . . . H2WB H 0.298(4) -0.029(2) 0.462(4) 0.037(9) Uiso 1 1 d . . . O3W O 1.1256(5) 0.2500 0.1148(5) 0.115(2) Uani 1 2 d S . . H3WA H 1.1120 0.2500 0.0041 0.138 Uiso 1 2 d SR . . H3WB H 1.1817 0.2029 0.1621 0.138 Uiso 0.50 1 d PR . . 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 Mn1 0.01233(15) 0.01212(15) 0.01617(16) 0.00192(10) 0.00394(11) 0.00117(10) Cu1 0.01416(17) 0.01254(17) 0.01386(17) 0.000 0.00364(12) 0.000 Na1 0.0661(7) 0.0334(5) 0.0289(5) -0.0126(4) 0.0255(5) -0.0285(5) Na2 0.0323(7) 0.0227(6) 0.0169(6) 0.000 0.0015(5) 0.000 S1 0.0113(3) 0.0113(3) 0.0101(3) 0.000 0.0034(2) 0.000 S2 0.0092(3) 0.0101(3) 0.0133(3) 0.000 0.0026(2) 0.000 S3 0.0116(2) 0.0110(2) 0.0107(2) 0.00064(15) 0.00226(15) -0.00003(15) O1 0.0203(7) 0.0161(7) 0.0182(7) -0.0012(5) 0.0074(5) -0.0063(5) O2 0.0194(10) 0.0190(10) 0.0142(9) 0.000 0.0096(8) 0.000 O3 0.0155(6) 0.0118(6) 0.0196(7) -0.0041(5) 0.0038(5) -0.0003(5) O4 0.0132(9) 0.0164(9) 0.0161(9) 0.000 0.0001(7) 0.000 O5 0.0233(7) 0.0131(7) 0.0188(7) -0.0038(5) 0.0072(6) 0.0002(5) O6 0.0110(6) 0.0286(8) 0.0179(7) 0.0043(6) 0.0027(5) -0.0011(5) O7 0.0208(7) 0.0180(7) 0.0121(6) -0.0003(5) -0.0012(5) 0.0015(5) O1W 0.0188(8) 0.0327(9) 0.0453(10) 0.0244(8) 0.0138(7) 0.0086(7) O2W 0.0297(8) 0.0155(7) 0.0199(8) -0.0045(6) 0.0109(6) -0.0066(6) O3W 0.039(2) 0.270(7) 0.0330(18) 0.000 0.0024(15) 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 Mn1 O6 2.1210(15) . ? Mn1 O1 2.1342(14) . ? Mn1 O1W 2.1602(16) . ? Mn1 O2W 2.1819(16) . ? Mn1 O4 2.2981(11) 1_455 ? Mn1 O3 2.3227(14) 1_455 ? Cu1 S3 2.2657(6) 4_565 ? Cu1 S3 2.2657(6) . ? Cu1 S2 2.2778(8) . ? Cu1 S1 2.2843(8) . ? Na1 O5 2.3416(17) . ? Na1 O2 2.4216(13) 3_656 ? Na1 O7 2.4725(18) 3_657 ? Na1 O6 2.4957(19) 3_657 ? Na1 O1 2.5560(18) 3_656 ? Na1 O2W 2.649(2) . ? Na1 S1 3.0797(12) 3_656 ? Na1 S3 3.0961(12) 3_657 ? Na1 S3 3.2681(13) . ? Na1 Na2 3.6699(16) 3_656 ? Na1 Na1 4.206(2) 3_657 ? Na2 O3W 2.333(4) . ? Na2 O7 2.3366(16) 1_554 ? Na2 O7 2.3366(16) 4_564 ? Na2 O2 2.514(2) . ? Na2 O3 2.5404(18) 4_565 ? Na2 O3 2.5404(18) . ? Na2 S2 3.0533(16) . ? Na2 Na1 3.6699(16) 3_656 ? Na2 Na1 3.6699(16) 2_656 ? S1 O2 1.4956(19) . ? S1 O1 1.5201(14) . ? S1 O1 1.5201(14) 4_565 ? S1 Na1 3.0797(12) 2_656 ? S1 Na1 3.0797(12) 3_656 ? S2 O3 1.5156(14) 4_565 ? S2 O3 1.5156(13) . ? S2 O4 1.537(2) . ? S3 O7 1.4994(14) . ? S3 O5 1.5097(14) . ? S3 O6 1.5232(15) . ? S3 Na1 3.0961(12) 3_657 ? O1 Na1 2.5560(18) 3_656 ? O2 Na1 2.4216(13) 2_656 ? O2 Na1 2.4216(13) 3_656 ? O3 Mn1 2.3227(14) 1_655 ? O4 Mn1 2.2981(11) 4_665 ? O4 Mn1 2.2981(11) 1_655 ? O6 Na1 2.4957(19) 3_657 ? O7 Na2 2.3366(16) 1_556 ? O7 Na1 2.4725(18) 3_657 ? O1W H1WA 0.80(3) . ? O1W H1WB 0.81(3) . ? O2W H2WA 0.80(3) . ? O2W H2WB 0.76(3) . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8499 . ? 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 O6 Mn1 O1 99.93(6) . . ? O6 Mn1 O1W 88.93(7) . . ? O1 Mn1 O1W 167.21(7) . . ? O6 Mn1 O2W 95.18(6) . . ? O1 Mn1 O2W 85.98(6) . . ? O1W Mn1 O2W 84.02(7) . . ? O6 Mn1 O4 93.78(6) . 1_455 ? O1 Mn1 O4 97.28(6) . 1_455 ? O1W Mn1 O4 91.28(7) . 1_455 ? O2W Mn1 O4 169.78(6) . 1_455 ? O6 Mn1 O3 155.42(5) . 1_455 ? O1 Mn1 O3 89.50(5) . 1_455 ? O1W Mn1 O3 86.07(6) . 1_455 ? O2W Mn1 O3 108.17(6) . 1_455 ? O4 Mn1 O3 62.34(6) 1_455 1_455 ? S3 Cu1 S3 111.55(3) 4_565 . ? S3 Cu1 S2 114.933(17) 4_565 . ? S3 Cu1 S2 114.933(17) . . ? S3 Cu1 S1 106.22(2) 4_565 . ? S3 Cu1 S1 106.22(2) . . ? S2 Cu1 S1 101.68(3) . . ? O5 Na1 O2 146.72(7) . 3_656 ? O5 Na1 O7 131.58(7) . 3_657 ? O2 Na1 O7 80.69(6) 3_656 3_657 ? O5 Na1 O6 99.62(6) . 3_657 ? O2 Na1 O6 106.56(7) 3_656 3_657 ? O7 Na1 O6 57.70(5) 3_657 3_657 ? O5 Na1 O1 89.38(6) . 3_656 ? O2 Na1 O1 57.53(6) 3_656 3_656 ? O7 Na1 O1 134.29(6) 3_657 3_656 ? O6 Na1 O1 146.46(7) 3_657 3_656 ? O5 Na1 O2W 89.57(6) . . ? O2 Na1 O2W 88.22(6) 3_656 . ? O7 Na1 O2W 80.75(6) 3_657 . ? O6 Na1 O2W 131.53(7) 3_657 . ? O1 Na1 O2W 80.31(6) 3_656 . ? O5 Na1 S1 118.79(5) . 3_656 ? O2 Na1 S1 28.47(4) 3_656 3_656 ? O7 Na1 S1 106.09(5) 3_657 3_656 ? O6 Na1 S1 131.61(5) 3_657 3_656 ? O1 Na1 S1 29.47(3) 3_656 3_656 ? O2W Na1 S1 80.00(5) . 3_656 ? O5 Na1 S3 118.53(5) . 3_657 ? O2 Na1 S3 93.85(5) 3_656 3_657 ? O7 Na1 S3 28.53(3) 3_657 3_657 ? O6 Na1 S3 29.17(3) 3_657 3_657 ? O1 Na1 S3 150.85(5) 3_656 3_657 ? O2W Na1 S3 106.40(6) . 3_657 ? S1 Na1 S3 122.31(4) 3_656 3_657 ? O5 Na1 S3 24.88(4) . . ? O2 Na1 S3 167.43(6) 3_656 . ? O7 Na1 S3 106.72(5) 3_657 . ? O6 Na1 S3 86.01(4) 3_657 . ? O1 Na1 S3 111.75(4) 3_656 . ? O2W Na1 S3 83.11(5) . . ? S1 Na1 S3 139.88(3) 3_656 . ? S3 Na1 S3 97.30(3) 3_657 . ? O5 Na1 Na2 162.62(6) . 3_656 ? O2 Na1 Na2 42.94(5) 3_656 3_656 ? O7 Na1 Na2 38.91(4) 3_657 3_656 ? O6 Na1 Na2 85.10(4) 3_657 3_656 ? O1 Na1 Na2 95.86(5) 3_656 3_656 ? O2W Na1 Na2 75.08(5) . 3_656 ? S1 Na1 Na2 67.18(3) 3_656 3_656 ? S3 Na1 Na2 60.18(3) 3_657 3_656 ? S3 Na1 Na2 141.24(4) . 3_656 ? O5 Na1 Na1 69.31(4) . 3_657 ? O2 Na1 Na1 143.88(6) 3_656 3_657 ? O7 Na1 Na1 64.97(4) 3_657 3_657 ? O6 Na1 Na1 45.83(4) 3_657 3_657 ? O1 Na1 Na1 158.56(5) 3_656 3_657 ? O2W Na1 Na1 96.58(6) . 3_657 ? S1 Na1 Na1 170.94(5) 3_656 3_657 ? S3 Na1 Na1 50.41(2) 3_657 3_657 ? S3 Na1 Na1 46.89(2) . 3_657 ? Na2 Na1 Na1 103.88(4) 3_656 3_657 ? O3W Na2 O7 96.59(7) . 1_554 ? O3W Na2 O7 96.59(7) . 4_564 ? O7 Na2 O7 106.53(8) 1_554 4_564 ? O3W Na2 O2 176.72(11) . . ? O7 Na2 O2 81.48(6) 1_554 . ? O7 Na2 O2 81.48(6) 4_564 . ? O3W Na2 O3 97.42(9) . 4_565 ? O7 Na2 O3 151.51(6) 1_554 4_565 ? O7 Na2 O3 96.35(5) 4_564 4_565 ? O2 Na2 O3 85.45(6) . 4_565 ? O3W Na2 O3 97.42(9) . . ? O7 Na2 O3 96.35(5) 1_554 . ? O7 Na2 O3 151.51(6) 4_564 . ? O2 Na2 O3 85.45(6) . . ? O3 Na2 O3 57.28(7) 4_565 . ? O3W Na2 S2 106.58(10) . . ? O7 Na2 S2 122.00(4) 1_554 . ? O7 Na2 S2 122.00(4) 4_564 . ? O2 Na2 S2 76.71(6) . . ? O3 Na2 S2 29.67(3) 4_565 . ? O3 Na2 S2 29.67(3) . . ? O3W Na2 Na1 137.56(5) . 3_656 ? O7 Na2 Na1 41.65(4) 1_554 3_656 ? O7 Na2 Na1 102.27(6) 4_564 3_656 ? O2 Na2 Na1 41.01(3) . 3_656 ? O3 Na2 Na1 117.50(5) 4_565 3_656 ? O3 Na2 Na1 83.56(4) . 3_656 ? S2 Na2 Na1 95.03(3) . 3_656 ? O3W Na2 Na1 137.56(5) . 2_656 ? O7 Na2 Na1 102.27(6) 1_554 2_656 ? O7 Na2 Na1 41.65(4) 4_564 2_656 ? O2 Na2 Na1 41.01(3) . 2_656 ? O3 Na2 Na1 83.56(4) 4_565 2_656 ? O3 Na2 Na1 117.50(5) . 2_656 ? S2 Na2 Na1 95.03(3) . 2_656 ? Na1 Na2 Na1 73.56(5) 3_656 2_656 ? O2 S1 O1 105.36(7) . . ? O2 S1 O1 105.36(7) . 4_565 ? O1 S1 O1 107.01(12) . 4_565 ? O2 S1 Cu1 114.67(9) . . ? O1 S1 Cu1 111.93(6) . . ? O1 S1 Cu1 111.93(6) 4_565 . ? O2 S1 Na1 50.52(4) . 2_656 ? O1 S1 Na1 125.82(7) . 2_656 ? O1 S1 Na1 55.80(6) 4_565 2_656 ? Cu1 S1 Na1 122.20(3) . 2_656 ? O2 S1 Na1 50.52(4) . 3_656 ? O1 S1 Na1 55.80(6) . 3_656 ? O1 S1 Na1 125.82(7) 4_565 3_656 ? Cu1 S1 Na1 122.20(3) . 3_656 ? Na1 S1 Na1 91.04(5) 2_656 3_656 ? O3 S2 O3 106.90(11) 4_565 . ? O3 S2 O4 103.14(7) 4_565 . ? O3 S2 O4 103.14(7) . . ? O3 S2 Cu1 111.95(6) 4_565 . ? O3 S2 Cu1 111.95(6) . . ? O4 S2 Cu1 118.67(8) . . ? O3 S2 Na2 56.07(6) 4_565 . ? O3 S2 Na2 56.07(6) . . ? O4 S2 Na2 132.84(8) . . ? Cu1 S2 Na2 108.49(4) . . ? O7 S3 O5 106.92(8) . . ? O7 S3 O6 104.95(8) . . ? O5 S3 O6 105.92(8) . . ? O7 S3 Cu1 114.51(6) . . ? O5 S3 Cu1 112.54(6) . . ? O6 S3 Cu1 111.35(6) . . ? O7 S3 Na1 51.96(6) . 3_657 ? O5 S3 Na1 117.75(6) . 3_657 ? O6 S3 Na1 52.99(6) . 3_657 ? Cu1 S3 Na1 129.68(3) . 3_657 ? O7 S3 Na1 102.24(6) . . ? O5 S3 Na1 40.74(6) . . ? O6 S3 Na1 68.12(6) . . ? Cu1 S3 Na1 141.21(3) . . ? Na1 S3 Na1 82.69(3) 3_657 . ? S1 O1 Mn1 127.54(8) . . ? S1 O1 Na1 94.73(7) . 3_656 ? Mn1 O1 Na1 134.94(7) . 3_656 ? S1 O2 Na1 101.01(6) . 2_656 ? S1 O2 Na1 101.01(6) . 3_656 ? Na1 O2 Na1 130.30(10) 2_656 3_656 ? S1 O2 Na2 138.46(12) . . ? Na1 O2 Na2 96.05(6) 2_656 . ? Na1 O2 Na2 96.05(6) 3_656 . ? S2 O3 Mn1 96.87(7) . 1_655 ? S2 O3 Na2 94.26(7) . . ? Mn1 O3 Na2 137.49(7) 1_655 . ? S2 O4 Mn1 97.24(6) . 4_665 ? S2 O4 Mn1 97.24(6) . 1_655 ? Mn1 O4 Mn1 121.04(9) 4_665 1_655 ? S3 O5 Na1 114.38(8) . . ? S3 O6 Mn1 128.55(8) . . ? S3 O6 Na1 97.84(7) . 3_657 ? Mn1 O6 Na1 133.19(7) . 3_657 ? S3 O7 Na2 125.27(8) . 1_556 ? S3 O7 Na1 99.51(8) . 3_657 ? Na2 O7 Na1 99.44(6) 1_556 3_657 ? Mn1 O1W H1WA 117(2) . . ? Mn1 O1W H1WB 125(2) . . ? H1WA O1W H1WB 115(3) . . ? Mn1 O2W Na1 103.36(6) . . ? Mn1 O2W H2WA 119.6(19) . . ? Na1 O2W H2WA 98.4(19) . . ? Mn1 O2W H2WB 118(2) . . ? Na1 O2W H2WB 119(2) . . ? H2WA O2W H2WB 97(3) . . ? Na2 O3W H3WA 113.2 . . ? Na2 O3W H3WB 105.0 . . ? H3WA O3W H3WB 113.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O7 0.80(3) 1.95(3) 2.731(2) 167(3) 3_657 O1W H1WB O5 0.81(3) 1.99(3) 2.797(2) 174(3) 1_455 O2W H2WA O3 0.80(3) 1.98(3) 2.767(2) 170(3) 3_656 O2W H2WB O5 0.76(3) 1.96(3) 2.715(2) 171(3) 3_656 O3W H3WA O4 0.85 2.07 2.908(4) 169.2 1_554 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.140 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.071 #===end data_compound2 _database_code_depnum_ccdc_archive 'CCDC 743943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cu H6 Mn4 Na O18 S5' _chemical_formula_weight 760.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' S S 0.1246 0.1234 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.821(4) _cell_length_b 11.020(3) _cell_length_c 13.097(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.903(6) _cell_angle_gamma 90.00 _cell_volume 1656.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 3.2046 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.981 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7910 _exptl_absorpt_correction_T_max 1.0000 _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 'Rigaku Mercury CCD' _diffrn_measurement_method 'narrow frame method' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 12603 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3788 _reflns_number_gt 3240 _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 ? _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^)+(0.0433P)^2^+7.5673P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3788 _refine_ls_number_parameters 266 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.025 _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 Na1 Na 0.6657(2) 1.0618(2) 0.48709(19) 0.0269(5) Uani 1 1 d . . . Cu1 Cu 0.49735(5) 0.69602(5) 0.22589(5) 0.01419(16) Uani 1 1 d . . . Mn1 Mn 0.55119(7) 0.70872(7) 0.54957(6) 0.01338(18) Uani 1 1 d . . . Mn2 Mn 0.74817(6) 0.55375(7) 0.74015(6) 0.01325(18) Uani 1 1 d . . . Mn3 Mn 0.81890(6) 0.89226(7) 0.34127(6) 0.01439(18) Uani 1 1 d . . . Mn4 Mn 0.75974(7) 0.43589(8) 0.46110(7) 0.0193(2) Uani 1 1 d . . . S1 S 0.69452(11) 0.30169(11) 0.62728(10) 0.0127(3) Uani 1 1 d . . . S2 S 0.65463(11) 0.69939(11) 0.15465(10) 0.0130(3) Uani 1 1 d . . . S3 S 0.53930(10) 0.53162(10) 0.33164(10) 0.0108(2) Uani 1 1 d . . . S4 S 0.31999(10) 0.68643(11) 0.11132(10) 0.0112(2) Uani 1 1 d . . . S5 S 0.52991(10) 0.86653(11) 0.32775(10) 0.0125(3) Uani 1 1 d . . . O1 O 0.7695(3) 0.1884(3) 0.6443(3) 0.0174(8) Uani 1 1 d . . . O2 O 0.7781(3) 0.4100(3) 0.6335(3) 0.0159(7) Uani 1 1 d . . . O3 O 0.6375(3) 0.3013(3) 0.5079(3) 0.0183(8) Uani 1 1 d . . . O4 O 0.6348(3) 0.7947(3) 0.0691(3) 0.0207(8) Uani 1 1 d . . . O5 O 0.6729(3) 0.5814(3) 0.1014(3) 0.0187(8) Uani 1 1 d . . . O6 O 0.7683(3) 0.7304(4) 0.2322(3) 0.0204(8) Uani 1 1 d . . . O7 O 0.6354(3) 0.4541(3) 0.3060(3) 0.0159(7) Uani 1 1 d . . . O8 O 0.4406(3) 0.4452(3) 0.3359(3) 0.0157(8) Uani 1 1 d . . . O9 O 0.5950(3) 0.5693(3) 0.4441(3) 0.0167(8) Uani 1 1 d . . . O10 O 0.2372(3) 0.7898(3) 0.1238(3) 0.0149(7) Uani 1 1 d . . . O11 O 0.3244(3) 0.6895(3) -0.0020(3) 0.0192(8) Uani 1 1 d . . . O12 O 0.2595(3) 0.5710(3) 0.1290(3) 0.0195(8) Uani 1 1 d . . . O13 O 0.5345(3) 0.8610(3) 0.4445(3) 0.0213(8) Uani 1 1 d . . . O14 O 0.4318(3) 0.9542(3) 0.2826(3) 0.0190(8) Uani 1 1 d . . . O15 O 0.6385(3) 0.9336(3) 0.3186(3) 0.0195(8) Uani 1 1 d . . . O1W O 0.8766(6) 0.5729(7) 0.4552(6) 0.0303(15) Uiso 0.581(4) 1 d P . . O1WA O 0.8670(15) 0.5603(16) 0.3819(15) 0.0303(15) Uiso 0.248(7) 1 d P . . O1WB O 0.936(2) 0.529(2) 0.569(2) 0.0303(15) Uiso 0.171(7) 1 d P . . O2W O 0.4892(4) 0.8189(4) 0.6657(3) 0.0264(9) Uani 1 1 d . . . H2WA H 0.5489 0.8713 0.7070 0.032 Uiso 1 1 calc R . . H2WB H 0.4527 0.7711 0.7111 0.032 Uiso 1 1 calc R . . O3W O 0.9968(4) 0.8297(5) 0.3816(4) 0.0437(14) Uani 1 1 d . . . H3WA H 1.0422 0.8904 0.3950 0.066 Uiso 1 1 d R . . H3WB H 1.0072 0.7843 0.4355 0.066 Uiso 1 1 d R . . 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 Na1 0.0318(13) 0.0226(12) 0.0251(13) -0.0031(10) 0.0046(10) 0.0008(10) Cu1 0.0126(3) 0.0127(3) 0.0171(3) 0.0004(2) 0.0034(3) 0.0003(2) Mn1 0.0115(4) 0.0133(4) 0.0144(4) 0.0004(3) 0.0012(3) 0.0009(3) Mn2 0.0117(4) 0.0116(4) 0.0153(4) -0.0008(3) 0.0010(3) -0.0001(3) Mn3 0.0123(4) 0.0157(4) 0.0154(4) 0.0010(3) 0.0038(3) 0.0001(3) Mn4 0.0202(4) 0.0224(4) 0.0156(4) 0.0043(3) 0.0047(3) 0.0057(3) S1 0.0138(6) 0.0114(6) 0.0136(6) 0.0001(5) 0.0050(5) 0.0001(4) S2 0.0129(6) 0.0116(6) 0.0154(6) -0.0003(5) 0.0053(5) -0.0004(4) S3 0.0104(5) 0.0098(5) 0.0120(6) 0.0008(4) 0.0023(5) 0.0014(4) S4 0.0102(6) 0.0110(6) 0.0119(6) -0.0011(4) 0.0015(5) 0.0005(4) S5 0.0105(6) 0.0111(6) 0.0152(6) 0.0001(5) 0.0017(5) 0.0001(4) O1 0.0160(18) 0.0149(18) 0.020(2) 0.0032(15) 0.0016(16) 0.0022(14) O2 0.0167(18) 0.0120(17) 0.0183(19) -0.0022(15) 0.0028(15) -0.0036(14) O3 0.0135(18) 0.021(2) 0.0170(19) 0.0024(15) -0.0020(15) -0.0024(14) O4 0.021(2) 0.0173(19) 0.025(2) 0.0059(16) 0.0076(17) -0.0020(15) O5 0.022(2) 0.0149(18) 0.020(2) -0.0018(15) 0.0062(16) 0.0025(15) O6 0.0142(18) 0.023(2) 0.023(2) -0.0065(17) 0.0039(16) -0.0033(15) O7 0.0144(17) 0.0205(19) 0.0132(18) -0.0004(15) 0.0041(15) 0.0076(14) O8 0.0129(17) 0.0127(17) 0.020(2) 0.0054(15) 0.0008(15) -0.0054(13) O9 0.0210(19) 0.0153(18) 0.0129(18) -0.0056(14) 0.0024(15) 0.0000(14) O10 0.0121(17) 0.0137(17) 0.0166(19) -0.0029(15) -0.0008(15) 0.0023(13) O11 0.0212(19) 0.024(2) 0.0128(19) -0.0018(15) 0.0054(16) 0.0011(15) O12 0.0177(19) 0.0162(18) 0.023(2) 0.0014(16) 0.0016(16) -0.0063(14) O13 0.028(2) 0.0185(19) 0.018(2) 0.0013(16) 0.0050(17) -0.0030(16) O14 0.0102(17) 0.0152(18) 0.029(2) 0.0022(16) 0.0005(16) 0.0012(14) O15 0.0089(17) 0.0171(19) 0.033(2) 0.0038(17) 0.0060(16) -0.0001(14) O2W 0.030(2) 0.019(2) 0.033(2) -0.0122(18) 0.0128(19) -0.0075(17) O3W 0.020(2) 0.084(4) 0.028(3) 0.018(3) 0.007(2) 0.012(2) _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 Na1 O12 2.416(4) 4_676 ? Na1 O5 2.468(4) 2_655 ? Na1 O1 2.546(4) 1_565 ? Na1 O15 2.574(5) . ? Na1 O13 2.682(5) . ? Na1 O3 2.683(4) 1_565 ? Na1 O2W 2.707(5) 3_676 ? Na1 O13 2.855(5) 3_676 ? Na1 S5 3.154(3) . ? Na1 S1 3.190(3) 1_565 ? Na1 Mn2 3.473(3) 2_656 ? Na1 Mn3 3.475(3) . ? Cu1 S3 2.2618(14) . ? Cu1 S4 2.2687(15) . ? Cu1 S2 2.2721(15) . ? Cu1 S5 2.2829(14) . ? Mn1 O13 2.149(4) . ? Mn1 O3 2.179(4) 3_666 ? Mn1 O10 2.180(4) 4_676 ? Mn1 O2W 2.204(4) . ? Mn1 O9 2.209(4) . ? Mn1 O8 2.251(4) 3_666 ? Mn1 Na1 3.551(3) 3_676 ? Mn2 O14 2.109(4) 4_676 ? Mn2 O1 2.165(4) 2_656 ? Mn2 O2 2.197(4) . ? Mn2 O8 2.214(4) 3_666 ? Mn2 O12 2.216(4) 3_666 ? Mn2 O10 2.284(4) 4_676 ? Mn2 Na1 3.473(3) 2_646 ? Mn3 O15 2.130(4) . ? Mn3 O3W 2.155(4) . ? Mn3 O5 2.210(4) 2_655 ? Mn3 O11 2.228(4) 4_676 ? Mn3 O7 2.231(4) 2_655 ? Mn3 O6 2.273(4) . ? Mn4 O1W 2.060(8) . ? Mn4 O4 2.090(4) 2_645 ? Mn4 O7 2.211(4) . ? Mn4 O2 2.234(4) . ? Mn4 O3 2.256(4) . ? Mn4 O1WA 2.279(18) . ? Mn4 O9 2.408(4) . ? Mn4 O1WB 2.45(3) . ? Mn4 S1 2.8853(16) . ? S1 O1 1.516(4) . ? S1 O2 1.539(4) . ? S1 O3 1.546(4) . ? S1 Na1 3.190(3) 1_545 ? S2 O4 1.513(4) . ? S2 O5 1.515(4) . ? S2 O6 1.516(4) . ? S3 O8 1.517(3) . ? S3 O9 1.520(4) . ? S3 O7 1.522(3) . ? S4 O11 1.498(4) . ? S4 O12 1.504(4) . ? S4 O10 1.536(4) . ? S5 O15 1.511(4) . ? S5 O14 1.516(4) . ? S5 O13 1.517(4) . ? O1 Mn2 2.165(4) 2_646 ? O1 Na1 2.546(4) 1_545 ? O3 Mn1 2.179(4) 3_666 ? O3 Na1 2.683(4) 1_545 ? O4 Mn4 2.090(4) 2_655 ? O5 Mn3 2.210(4) 2_645 ? O5 Na1 2.468(4) 2_645 ? O7 Mn3 2.231(4) 2_645 ? O8 Mn2 2.214(4) 3_666 ? O8 Mn1 2.251(4) 3_666 ? O10 Mn1 2.180(4) 4_575 ? O10 Mn2 2.284(4) 4_575 ? O11 Mn3 2.228(4) 4_575 ? O12 Mn2 2.216(4) 3_666 ? O12 Na1 2.416(4) 4_575 ? O13 Na1 2.855(5) 3_676 ? O14 Mn2 2.109(4) 4_575 ? O1W O1WA 0.949(18) . ? O1W O1WB 1.57(3) . ? O2W Na1 2.707(5) 3_676 ? 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 O12 Na1 O5 98.68(15) 4_676 2_655 ? O12 Na1 O1 70.53(14) 4_676 1_565 ? O5 Na1 O1 93.14(15) 2_655 1_565 ? O12 Na1 O15 105.48(15) 4_676 . ? O5 Na1 O15 66.24(13) 2_655 . ? O1 Na1 O15 158.57(16) 1_565 . ? O12 Na1 O13 78.23(14) 4_676 . ? O5 Na1 O13 116.62(15) 2_655 . ? O1 Na1 O13 139.72(15) 1_565 . ? O15 Na1 O13 54.70(12) . . ? O12 Na1 O3 124.26(15) 4_676 1_565 ? O5 Na1 O3 95.19(14) 2_655 1_565 ? O1 Na1 O3 54.96(12) 1_565 1_565 ? O15 Na1 O3 129.36(15) . 1_565 ? O13 Na1 O3 138.85(15) . 1_565 ? O12 Na1 O2W 165.25(16) 4_676 3_676 ? O5 Na1 O2W 94.16(15) 2_655 3_676 ? O1 Na1 O2W 116.14(14) 1_565 3_676 ? O15 Na1 O2W 73.15(13) . 3_676 ? O13 Na1 O2W 89.56(14) . 3_676 ? O3 Na1 O2W 61.21(12) 1_565 3_676 ? O12 Na1 O13 101.57(15) 4_676 3_676 ? O5 Na1 O13 156.07(15) 2_655 3_676 ? O1 Na1 O13 81.81(13) 1_565 3_676 ? O15 Na1 O13 119.38(14) . 3_676 ? O13 Na1 O13 80.20(14) . 3_676 ? O3 Na1 O13 62.75(12) 1_565 3_676 ? O2W Na1 O13 67.82(13) 3_676 3_676 ? O12 Na1 S5 99.35(12) 4_676 . ? O5 Na1 S5 94.43(12) 2_655 . ? O1 Na1 S5 168.21(13) 1_565 . ? O15 Na1 S5 28.34(8) . . ? O13 Na1 S5 28.71(9) . . ? O3 Na1 S5 133.03(12) 1_565 . ? O2W Na1 S5 72.30(10) 3_676 . ? O13 Na1 S5 94.73(11) 3_676 . ? O12 Na1 S1 95.36(12) 4_676 1_565 ? O5 Na1 S1 102.11(12) 2_655 1_565 ? O1 Na1 S1 27.87(8) 1_565 1_565 ? O15 Na1 S1 157.25(13) . 1_565 ? O13 Na1 S1 141.24(13) . 1_565 ? O3 Na1 S1 28.92(9) 1_565 1_565 ? O2W Na1 S1 88.99(11) 3_676 1_565 ? O13 Na1 S1 63.52(9) 3_676 1_565 ? S5 Na1 S1 155.92(9) . 1_565 ? O12 Na1 Mn2 39.29(10) 4_676 2_656 ? O5 Na1 Mn2 114.61(12) 2_655 2_656 ? O1 Na1 Mn2 38.43(9) 1_565 2_656 ? O15 Na1 Mn2 144.41(12) . 2_656 ? O13 Na1 Mn2 101.84(11) . 2_656 ? O3 Na1 Mn2 86.17(10) 1_565 2_656 ? O2W Na1 Mn2 138.75(12) 3_676 2_656 ? O13 Na1 Mn2 75.21(10) 3_676 2_656 ? S5 Na1 Mn2 129.79(8) . 2_656 ? S1 Na1 Mn2 57.63(5) 1_565 2_656 ? O12 Na1 Mn3 83.92(11) 4_676 . ? O5 Na1 Mn3 39.24(9) 2_655 . ? O1 Na1 Mn3 121.71(12) 1_565 . ? O15 Na1 Mn3 37.65(9) . . ? O13 Na1 Mn3 78.10(10) . . ? O3 Na1 Mn3 132.74(12) 1_565 . ? O2W Na1 Mn3 101.79(11) 3_676 . ? O13 Na1 Mn3 156.01(11) 3_676 . ? S5 Na1 Mn3 61.28(5) . . ? S1 Na1 Mn3 139.83(8) 1_565 . ? Mn2 Na1 Mn3 119.27(7) 2_656 . ? S3 Cu1 S4 113.55(5) . . ? S3 Cu1 S2 100.60(5) . . ? S4 Cu1 S2 116.52(6) . . ? S3 Cu1 S5 108.66(6) . . ? S4 Cu1 S5 115.09(5) . . ? S2 Cu1 S5 100.76(5) . . ? O13 Mn1 O3 83.67(14) . 3_666 ? O13 Mn1 O10 101.95(14) . 4_676 ? O3 Mn1 O10 173.50(14) 3_666 4_676 ? O13 Mn1 O2W 91.00(16) . . ? O3 Mn1 O2W 77.53(15) 3_666 . ? O10 Mn1 O2W 98.93(15) 4_676 . ? O13 Mn1 O9 98.16(15) . . ? O3 Mn1 O9 97.05(14) 3_666 . ? O10 Mn1 O9 85.48(14) 4_676 . ? O2W Mn1 O9 168.82(15) . . ? O13 Mn1 O8 176.21(14) . 3_666 ? O3 Mn1 O8 93.93(13) 3_666 3_666 ? O10 Mn1 O8 80.28(13) 4_676 3_666 ? O2W Mn1 O8 85.61(15) . 3_666 ? O9 Mn1 O8 85.03(14) . 3_666 ? O13 Mn1 Na1 53.51(11) . 3_676 ? O3 Mn1 Na1 48.97(11) 3_666 3_676 ? O10 Mn1 Na1 132.31(11) 4_676 3_676 ? O2W Mn1 Na1 49.62(12) . 3_676 ? O9 Mn1 Na1 132.92(11) . 3_676 ? O8 Mn1 Na1 122.74(10) 3_666 3_676 ? O14 Mn2 O1 96.34(14) 4_676 2_656 ? O14 Mn2 O2 79.90(14) 4_676 . ? O1 Mn2 O2 175.05(14) 2_656 . ? O14 Mn2 O8 168.76(15) 4_676 3_666 ? O1 Mn2 O8 93.12(14) 2_656 3_666 ? O2 Mn2 O8 90.97(14) . 3_666 ? O14 Mn2 O12 90.05(14) 4_676 3_666 ? O1 Mn2 O12 81.73(15) 2_656 3_666 ? O2 Mn2 O12 94.99(14) . 3_666 ? O8 Mn2 O12 97.30(13) 3_666 3_666 ? O14 Mn2 O10 95.58(14) 4_676 4_676 ? O1 Mn2 O10 87.11(14) 2_656 4_676 ? O2 Mn2 O10 96.43(14) . 4_676 ? O8 Mn2 O10 78.83(13) 3_666 4_676 ? O12 Mn2 O10 167.99(14) 3_666 4_676 ? O14 Mn2 Na1 72.61(12) 4_676 2_646 ? O1 Mn2 Na1 46.94(11) 2_656 2_646 ? O2 Mn2 Na1 128.34(11) . 2_646 ? O8 Mn2 Na1 118.50(11) 3_666 2_646 ? O12 Mn2 Na1 43.66(11) 3_666 2_646 ? O10 Mn2 Na1 128.53(10) 4_676 2_646 ? O15 Mn3 O3W 171.04(17) . . ? O15 Mn3 O5 78.85(14) . 2_655 ? O3W Mn3 O5 104.96(19) . 2_655 ? O15 Mn3 O11 91.24(15) . 4_676 ? O3W Mn3 O11 80.44(16) . 4_676 ? O5 Mn3 O11 94.53(14) 2_655 4_676 ? O15 Mn3 O7 104.86(14) . 2_655 ? O3W Mn3 O7 83.39(16) . 2_655 ? O5 Mn3 O7 90.35(14) 2_655 2_655 ? O11 Mn3 O7 163.81(14) 4_676 2_655 ? O15 Mn3 O6 88.67(14) . . ? O3W Mn3 O6 89.81(18) . . ? O5 Mn3 O6 159.55(15) 2_655 . ? O11 Mn3 O6 101.94(15) 4_676 . ? O7 Mn3 O6 77.15(14) 2_655 . ? O15 Mn3 Na1 47.58(12) . . ? O3W Mn3 Na1 130.10(15) . . ? O5 Mn3 Na1 44.96(10) 2_655 . ? O11 Mn3 Na1 67.35(11) 4_676 . ? O7 Mn3 Na1 125.27(11) 2_655 . ? O6 Mn3 Na1 132.37(10) . . ? O1W Mn4 O4 95.9(2) . 2_645 ? O1W Mn4 O7 101.7(2) . . ? O4 Mn4 O7 100.88(14) 2_645 . ? O1W Mn4 O2 103.2(2) . . ? O4 Mn4 O2 100.27(15) 2_645 . ? O7 Mn4 O2 145.25(13) . . ? O1W Mn4 O3 166.2(3) . . ? O4 Mn4 O3 90.70(15) 2_645 . ? O7 Mn4 O3 88.94(14) . . ? O2 Mn4 O3 63.53(13) . . ? O1W Mn4 O1WA 24.6(5) . . ? O4 Mn4 O1WA 86.5(5) 2_645 . ? O7 Mn4 O1WA 81.2(5) . . ? O2 Mn4 O1WA 127.4(5) . . ? O3 Mn4 O1WA 169.1(5) . . ? O1W Mn4 O9 94.8(2) . . ? O4 Mn4 O9 160.60(14) 2_645 . ? O7 Mn4 O9 61.02(12) . . ? O2 Mn4 O9 92.95(13) . . ? O3 Mn4 O9 82.50(13) . . ? O1WA Mn4 O9 96.7(4) . . ? O1W Mn4 O1WB 39.5(6) . . ? O4 Mn4 O1WB 87.7(6) 2_645 . ? O7 Mn4 O1WB 141.2(6) . . ? O2 Mn4 O1WB 66.8(6) . . ? O3 Mn4 O1WB 129.1(6) . . ? O1WA Mn4 O1WB 61.4(8) . . ? O9 Mn4 O1WB 110.7(6) . . ? O1W Mn4 S1 135.0(2) . . ? O4 Mn4 S1 92.34(12) 2_645 . ? O7 Mn4 S1 120.01(11) . . ? O2 Mn4 S1 31.88(9) . . ? O3 Mn4 S1 32.14(10) . . ? O1WA Mn4 S1 158.5(5) . . ? O9 Mn4 S1 91.46(10) . . ? O1WB Mn4 S1 97.1(6) . . ? O1 S1 O2 106.5(2) . . ? O1 S1 O3 104.1(2) . . ? O2 S1 O3 100.0(2) . . ? O1 S1 Mn4 106.26(15) . . ? O2 S1 Mn4 50.04(14) . . ? O3 S1 Mn4 50.90(14) . . ? O1 S1 Na1 51.70(15) . 1_545 ? O2 S1 Na1 130.63(16) . 1_545 ? O3 S1 Na1 57.03(15) . 1_545 ? Mn4 S1 Na1 90.09(6) . 1_545 ? O4 S2 O5 105.6(2) . . ? O4 S2 O6 107.1(2) . . ? O5 S2 O6 107.5(2) . . ? O4 S2 Cu1 108.62(16) . . ? O5 S2 Cu1 113.34(15) . . ? O6 S2 Cu1 114.20(16) . . ? O8 S3 O9 107.1(2) . . ? O8 S3 O7 106.1(2) . . ? O9 S3 O7 101.2(2) . . ? O8 S3 Cu1 117.89(15) . . ? O9 S3 Cu1 110.81(15) . . ? O7 S3 Cu1 112.35(15) . . ? O11 S4 O12 107.6(2) . . ? O11 S4 O10 105.3(2) . . ? O12 S4 O10 105.8(2) . . ? O11 S4 Cu1 114.05(16) . . ? O12 S4 Cu1 109.61(16) . . ? O10 S4 Cu1 113.99(15) . . ? O15 S5 O14 104.0(2) . . ? O15 S5 O13 105.9(2) . . ? O14 S5 O13 104.9(2) . . ? O15 S5 Cu1 112.54(16) . . ? O14 S5 Cu1 106.90(16) . . ? O13 S5 Cu1 121.05(16) . . ? O15 S5 Na1 53.97(17) . . ? O14 S5 Na1 92.50(16) . . ? O13 S5 Na1 58.10(16) . . ? Cu1 S5 Na1 159.31(7) . . ? S1 O1 Mn2 121.0(2) . 2_646 ? S1 O1 Na1 100.43(19) . 1_545 ? Mn2 O1 Na1 94.63(14) 2_646 1_545 ? S1 O2 Mn2 113.1(2) . . ? S1 O2 Mn4 98.08(18) . . ? Mn2 O2 Mn4 123.99(17) . . ? S1 O3 Mn1 120.7(2) . 3_666 ? S1 O3 Mn4 96.95(18) . . ? Mn1 O3 Mn4 127.51(17) 3_666 . ? S1 O3 Na1 94.05(18) . 1_545 ? Mn1 O3 Na1 93.25(14) 3_666 1_545 ? Mn4 O3 Na1 121.04(17) . 1_545 ? S2 O4 Mn4 131.6(2) . 2_655 ? S2 O5 Mn3 130.7(2) . 2_645 ? S2 O5 Na1 120.2(2) . 2_645 ? Mn3 O5 Na1 95.80(14) 2_645 2_645 ? S2 O6 Mn3 130.9(2) . . ? S3 O7 Mn4 102.42(19) . . ? S3 O7 Mn3 135.3(2) . 2_645 ? Mn4 O7 Mn3 121.40(15) . 2_645 ? S3 O8 Mn2 132.9(2) . 3_666 ? S3 O8 Mn1 125.9(2) . 3_666 ? Mn2 O8 Mn1 100.43(13) 3_666 3_666 ? S3 O9 Mn1 133.2(2) . . ? S3 O9 Mn4 94.30(17) . . ? Mn1 O9 Mn4 132.29(17) . . ? S4 O10 Mn1 124.0(2) . 4_575 ? S4 O10 Mn2 134.0(2) . 4_575 ? Mn1 O10 Mn2 100.45(14) 4_575 4_575 ? S4 O11 Mn3 154.6(2) . 4_575 ? S4 O12 Mn2 138.9(2) . 3_666 ? S4 O12 Na1 122.7(2) . 4_575 ? Mn2 O12 Na1 97.05(15) 3_666 4_575 ? S5 O13 Mn1 130.7(2) . . ? S5 O13 Na1 93.19(18) . . ? Mn1 O13 Na1 123.45(17) . . ? S5 O13 Na1 118.2(2) . 3_676 ? Mn1 O13 Na1 89.25(14) . 3_676 ? Na1 O13 Na1 99.80(14) . 3_676 ? S5 O14 Mn2 136.0(2) . 4_575 ? S5 O15 Mn3 136.5(2) . . ? S5 O15 Na1 97.7(2) . . ? Mn3 O15 Na1 94.78(15) . . ? O1WA O1W O1WB 146.9(16) . . ? O1WA O1W Mn4 90.7(12) . . ? O1WB O1W Mn4 83.7(10) . . ? O1W O1WA Mn4 64.7(11) . . ? O1W O1WB Mn4 56.8(8) . . ? Mn1 O2W Na1 92.05(16) . 3_676 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.202 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.184 #===end