data_Mn-bloedite _audit_update_record ; 2013-03-18 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common Mn-bloedite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Co0.14 Mg0.29 Mn0.44 Na1.96 Ni0.06 O12 S2.03' _chemical_formula_weight 353.20 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 21/a' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 11.137(2) _cell_length_b 8.2790(10) _cell_length_c 5.5381(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.423(13) _cell_angle_gamma 90.00 _cell_volume 502.20(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2708 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 43.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 1.559 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'X-Red, X-Shape' _exptl_special_details ? _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2708 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1498 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 43.00 _reflns_number_total 2708 _reflns_number_gt 1115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis CCD' _computing_cell_refinement 'Crysalis RED' _computing_data_reduction 'Crysalis RED' _computing_structure_solution 'SHELXS-97' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics ? _computing_publication_material 'publCIF' _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 [0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0359P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2708 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _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 0.0000 0.0000 0.0000 0.01783(19) Uani 0.45 2 d SP . . Mg1 Mg 0.0000 0.0000 0.0000 0.01783(19) Uani 0.29 2 d SP . . Ni1 Ni 0.0000 0.0000 0.0000 0.01783(19) Uani 0.06 2 d SP . . Co1 Co 0.0000 0.0000 0.0000 0.01783(19) Uani 0.14 2 d SP . . S1 S 0.13613(6) 0.29031(9) 0.37014(13) 0.01383(14) Uani 1 1 d . . . Na1 Na 0.36212(11) 0.07065(16) 0.1298(2) 0.0222(3) Uani 1 1 d . . . O1 O 0.26526(19) 0.2728(3) 0.3466(4) 0.0223(5) Uani 1 1 d . . . O2 O 0.07933(19) 0.4193(3) 0.2078(4) 0.0233(5) Uani 1 1 d . . . O3 O 0.0713(2) 0.1369(3) 0.3118(4) 0.0227(5) Uani 1 1 d . . . O4 O 0.1319(2) 0.3304(3) 0.6293(4) 0.0223(5) Uani 1 1 d . . . O5 O 0.16225(19) 0.0390(3) 0.8708(4) 0.0196(5) Uani 1 1 d . . . O6 O 0.0814(2) 0.7876(3) 0.1799(4) 0.0208(5) Uani 1 1 d . . . H5A H 0.179(5) 0.145(7) 0.758(9) 0.080 Uiso 1 1 d . . . H5B H 0.180(4) -0.050(6) 0.747(9) 0.080 Uiso 1 1 d . . . H6A H 0.024(5) 0.713(6) 0.222(9) 0.080 Uiso 1 1 d . . . H6B H 0.099(6) 0.783(7) 0.310(10) 0.080 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0169(4) 0.0177(4) 0.0193(4) -0.0010(3) 0.0046(3) -0.0012(3) Mg1 0.0169(4) 0.0177(4) 0.0193(4) -0.0010(3) 0.0046(3) -0.0012(3) Ni1 0.0169(4) 0.0177(4) 0.0193(4) -0.0010(3) 0.0046(3) -0.0012(3) Co1 0.0169(4) 0.0177(4) 0.0193(4) -0.0010(3) 0.0046(3) -0.0012(3) S1 0.0128(3) 0.0154(3) 0.0130(3) 0.0004(3) 0.0018(2) -0.0009(3) Na1 0.0193(6) 0.0222(7) 0.0245(6) -0.0009(6) 0.0022(5) 0.0003(5) O1 0.0144(10) 0.0238(12) 0.0291(12) 0.0028(10) 0.0048(9) 0.0022(9) O2 0.0187(10) 0.0253(12) 0.0256(12) 0.0109(10) 0.0033(9) 0.0030(9) O3 0.0297(12) 0.0222(11) 0.0166(10) -0.0053(9) 0.0054(9) -0.0111(10) O4 0.0309(13) 0.0225(12) 0.0143(10) -0.0051(9) 0.0062(9) -0.0014(10) O5 0.0189(10) 0.0213(11) 0.0199(11) 0.0006(9) 0.0075(9) 0.0011(8) O6 0.0209(11) 0.0193(11) 0.0202(11) 0.0010(10) -0.0017(9) -0.0014(9) _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 O5 2.085(2) 1_554 ? Mn1 O5 2.085(2) 3_556 ? Mn1 O3 2.097(2) . ? Mn1 O3 2.097(2) 3 ? Mn1 O6 2.140(2) 1_545 ? Mn1 O6 2.140(2) 3_565 ? S1 O2 1.464(2) . ? S1 O3 1.468(2) . ? S1 O1 1.474(2) . ? S1 O4 1.482(2) . ? S1 Na1 3.3075(15) 4_565 ? Na1 O2 2.381(2) 4_665 ? Na1 O4 2.389(2) 2_546 ? Na1 O1 2.424(3) . ? Na1 O5 2.434(2) 1_554 ? Na1 O2 2.435(2) 2_545 ? Na1 O6 2.638(3) 2_545 ? Na1 S1 3.3075(15) 4_665 ? Na1 Na1 3.804(2) 3_655 ? O2 Na1 2.381(2) 4_565 ? O2 Na1 2.435(2) 2 ? O4 Na1 2.389(2) 2_556 ? O5 Co1 2.085(2) 1_556 ? O5 Mn1 2.085(2) 1_556 ? O5 Mg1 2.085(2) 1_556 ? O5 Ni1 2.085(2) 1_556 ? O5 Na1 2.434(2) 1_556 ? O5 H5A 1.11(5) . ? O5 H5B 1.05(5) . ? O6 Co1 2.140(2) 1_565 ? O6 Mn1 2.140(2) 1_565 ? O6 Mg1 2.140(2) 1_565 ? O6 Ni1 2.140(2) 1_565 ? O6 Na1 2.638(3) 2 ? O6 H6A 0.95(6) . ? O6 H6B 0.71(5) . ? 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 Mn1 O5 180.00(13) 1_554 3_556 ? O5 Mn1 O3 88.64(8) 1_554 . ? O5 Mn1 O3 91.36(8) 3_556 . ? O5 Mn1 O3 91.36(8) 1_554 3 ? O5 Mn1 O3 88.64(8) 3_556 3 ? O3 Mn1 O3 180.00(7) . 3 ? O5 Mn1 O6 88.11(9) 1_554 1_545 ? O5 Mn1 O6 91.89(9) 3_556 1_545 ? O3 Mn1 O6 89.73(9) . 1_545 ? O3 Mn1 O6 90.27(9) 3 1_545 ? O5 Mn1 O6 91.89(9) 1_554 3_565 ? O5 Mn1 O6 88.11(9) 3_556 3_565 ? O3 Mn1 O6 90.27(9) . 3_565 ? O3 Mn1 O6 89.73(9) 3 3_565 ? O6 Mn1 O6 180.00(14) 1_545 3_565 ? O2 S1 O3 110.81(13) . . ? O2 S1 O1 109.72(13) . . ? O3 S1 O1 110.14(13) . . ? O2 S1 O4 110.22(13) . . ? O3 S1 O4 107.83(12) . . ? O1 S1 O4 108.06(13) . . ? O2 S1 Na1 40.04(9) . 4_565 ? O3 S1 Na1 80.28(10) . 4_565 ? O1 S1 Na1 147.39(10) . 4_565 ? O4 S1 Na1 97.07(10) . 4_565 ? O2 Na1 O4 90.17(9) 4_665 2_546 ? O2 Na1 O1 114.51(9) 4_665 . ? O4 Na1 O1 105.56(9) 2_546 . ? O2 Na1 O5 154.35(9) 4_665 1_554 ? O4 Na1 O5 99.77(9) 2_546 1_554 ? O1 Na1 O5 85.68(8) . 1_554 ? O2 Na1 O2 75.68(9) 4_665 2_545 ? O4 Na1 O2 90.92(9) 2_546 2_545 ? O1 Na1 O2 160.12(10) . 2_545 ? O5 Na1 O2 80.54(8) 1_554 2_545 ? O2 Na1 O6 74.92(8) 4_665 2_545 ? O4 Na1 O6 160.79(9) 2_546 2_545 ? O1 Na1 O6 91.83(9) . 2_545 ? O5 Na1 O6 89.45(8) 1_554 2_545 ? O2 Na1 O6 73.88(8) 2_545 2_545 ? O2 Na1 S1 23.31(5) 4_665 4_665 ? O4 Na1 S1 97.73(7) 2_546 4_665 ? O1 Na1 S1 91.22(6) . 4_665 ? O5 Na1 S1 162.42(8) 1_554 4_665 ? O2 Na1 S1 97.60(7) 2_545 4_665 ? O6 Na1 S1 73.34(6) 2_545 4_665 ? O2 Na1 Na1 38.34(6) 4_665 3_655 ? O4 Na1 Na1 90.69(7) 2_546 3_655 ? O1 Na1 Na1 149.52(8) . 3_655 ? O5 Na1 Na1 117.32(7) 1_554 3_655 ? O2 Na1 Na1 37.33(6) 2_545 3_655 ? O6 Na1 Na1 70.09(6) 2_545 3_655 ? S1 Na1 Na1 60.65(4) 4_665 3_655 ? S1 O1 Na1 129.81(13) . . ? S1 O2 Na1 116.66(12) . 4_565 ? S1 O2 Na1 134.49(13) . 2 ? Na1 O2 Na1 104.32(9) 4_565 2 ? S1 O3 Mn1 138.30(13) . . ? S1 O4 Na1 136.41(14) . 2_556 ? Co1 O5 Mn1 0.0 1_556 1_556 ? Co1 O5 Mg1 0.0 1_556 1_556 ? Mn1 O5 Mg1 0.0 1_556 1_556 ? Co1 O5 Ni1 0.0 1_556 1_556 ? Mn1 O5 Ni1 0.0 1_556 1_556 ? Mg1 O5 Ni1 0.0 1_556 1_556 ? Co1 O5 Na1 124.83(10) 1_556 1_556 ? Mn1 O5 Na1 124.83(10) 1_556 1_556 ? Mg1 O5 Na1 124.83(10) 1_556 1_556 ? Ni1 O5 Na1 124.83(10) 1_556 1_556 ? Co1 O5 H5A 124(3) 1_556 . ? Mn1 O5 H5A 124(3) 1_556 . ? Mg1 O5 H5A 124(3) 1_556 . ? Ni1 O5 H5A 124(3) 1_556 . ? Na1 O5 H5A 91(3) 1_556 . ? Co1 O5 H5B 113(3) 1_556 . ? Mn1 O5 H5B 113(3) 1_556 . ? Mg1 O5 H5B 113(3) 1_556 . ? Ni1 O5 H5B 113(3) 1_556 . ? Na1 O5 H5B 102(3) 1_556 . ? H5A O5 H5B 97(3) . . ? Co1 O6 Mn1 0.0 1_565 1_565 ? Co1 O6 Mg1 0.0 1_565 1_565 ? Mn1 O6 Mg1 0.0 1_565 1_565 ? Co1 O6 Ni1 0.0 1_565 1_565 ? Mn1 O6 Ni1 0.0 1_565 1_565 ? Mg1 O6 Ni1 0.0 1_565 1_565 ? Co1 O6 Na1 112.80(9) 1_565 2 ? Mn1 O6 Na1 112.80(9) 1_565 2 ? Mg1 O6 Na1 112.80(9) 1_565 2 ? Ni1 O6 Na1 112.80(9) 1_565 2 ? Co1 O6 H6A 114(3) 1_565 . ? Mn1 O6 H6A 114(3) 1_565 . ? Mg1 O6 H6A 114(3) 1_565 . ? Ni1 O6 H6A 114(3) 1_565 . ? Na1 O6 H6A 88(3) 2 . ? Co1 O6 H6B 122(5) 1_565 . ? Mn1 O6 H6B 122(5) 1_565 . ? Mg1 O6 H6B 122(5) 1_565 . ? Ni1 O6 H6B 122(5) 1_565 . ? Na1 O6 H6B 124(5) 2 . ? H6A O6 H6B 78(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 O5 H5A O4 1.11(5) 1.73(5) 2.749(3) 149(4) . O5 H5B O1 1.05(5) 1.70(5) 2.704(3) 158(4) 2_546 O6 H6A O4 0.95(6) 2.08(6) 2.936(3) 149(4) 3_566 O6 H6B O1 0.71(5) 2.21(6) 2.861(3) 154(7) 2_556 _diffrn_measured_fraction_theta_max 0.728 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.715 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.134