data_gozaisho _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As3 Ca2 Mg Mn Na O12' _chemical_formula_weight 599.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'y+3/4, x+1/4, -z+1/4' '-y+3/4, -x+3/4, -z+3/4' 'y+1/4, -x+1/4, z+3/4' '-y+1/4, x+3/4, z+1/4' 'x+3/4, z+1/4, -y+1/4' '-x+1/4, z+3/4, y+1/4' '-x+3/4, -z+3/4, -y+3/4' 'x+1/4, -z+1/4, y+3/4' 'z+3/4, y+1/4, -x+1/4' 'z+1/4, -y+1/4, x+3/4' '-z+1/4, y+3/4, x+1/4' '-z+3/4, -y+3/4, -x+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' 'y+5/4, x+3/4, -z+3/4' '-y+5/4, -x+5/4, -z+5/4' 'y+3/4, -x+3/4, z+5/4' '-y+3/4, x+5/4, z+3/4' 'x+5/4, z+3/4, -y+3/4' '-x+3/4, z+5/4, y+3/4' '-x+5/4, -z+5/4, -y+5/4' 'x+3/4, -z+3/4, y+5/4' 'z+5/4, y+3/4, -x+3/4' 'z+3/4, -y+3/4, x+5/4' '-z+3/4, y+5/4, x+3/4' '-z+5/4, -y+5/4, -x+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' '-y-3/4, -x-1/4, z-1/4' 'y-3/4, x-3/4, z-3/4' '-y-1/4, x-1/4, -z-3/4' 'y-1/4, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y-1/4' 'x-1/4, -z-3/4, -y-1/4' 'x-3/4, z-3/4, y-3/4' '-x-1/4, z-1/4, -y-3/4' '-z-3/4, -y-1/4, x-1/4' '-z-1/4, y-1/4, -x-3/4' 'z-1/4, -y-3/4, -x-1/4' 'z-3/4, y-3/4, x-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z, x, y+1/2' 'z, x+1/2, -y' 'z+1/2, -x, y' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z, x' '-y, z, x+1/2' 'y, z+1/2, -x' '-y-1/4, -x+1/4, z+1/4' 'y-1/4, x-1/4, z-1/4' '-y+1/4, x+1/4, -z-1/4' 'y+1/4, -x-1/4, -z+1/4' '-x-1/4, -z+1/4, y+1/4' 'x+1/4, -z-1/4, -y+1/4' 'x-1/4, z-1/4, y-1/4' '-x+1/4, z+1/4, -y-1/4' '-z-1/4, -y+1/4, x+1/4' '-z+1/4, y+1/4, -x-1/4' 'z+1/4, -y-1/4, -x+1/4' 'z-1/4, y-1/4, x-1/4' _cell_length_a 12.4929(2) _cell_length_b 12.4929(2) _cell_length_c 12.4929(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1949.80(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 12.691 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2791 _exptl_absorpt_correction_T_max 0.7854 _exptl_absorpt_process_details ? _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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6753 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0110 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 35.95 _reflns_number_total 388 _reflns_number_gt 339 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0120P)^2^+1.6195P] 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 0.00053(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 388 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0136 _refine_ls_wR_factor_ref 0.0328 _refine_ls_wR_factor_gt 0.0318 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 CaX Ca 0.1250 0.0000 0.2500 0.01113(13) Uani 0.67 4 d SP . . NaX Na 0.1250 0.0000 0.2500 0.01113(13) Uani 0.33 4 d SP . . MnY Mn 0.0000 0.0000 0.0000 0.00945(14) Uani 0.848(5) 6 d SP . . MgY Mg 0.0000 0.0000 0.0000 0.00945(14) Uani 0.152(5) 6 d SP . . AsT As 0.3750 0.0000 0.2500 0.00637(7) Uani 0.963(3) 4 d SP . . O O 0.03973(6) 0.05317(6) 0.65912(6) 0.01104(19) Uani 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 CaX 0.0085(2) 0.01243(16) 0.01243(16) 0.00168(16) 0.000 0.000 NaX 0.0085(2) 0.01243(16) 0.01243(16) 0.00168(16) 0.000 0.000 MnY 0.00945(14) 0.00945(14) 0.00945(14) -0.00048(7) -0.00048(7) -0.00048(7) MgY 0.00945(14) 0.00945(14) 0.00945(14) -0.00048(7) -0.00048(7) -0.00048(7) AsT 0.00621(11) 0.00645(8) 0.00645(8) 0.000 0.000 0.000 O 0.0112(4) 0.0125(4) 0.0094(3) 0.0007(2) -0.0019(2) 0.0016(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 CaX O 2.4424(8) 76_554 ? CaX O 2.4424(8) 67_656 ? CaX O 2.4424(8) 49_556 ? CaX O 2.4424(8) 90_565 ? CaX O 2.5446(8) 70_656 ? CaX O 2.5446(8) 55_556 ? CaX O 2.5446(8) 80_455 ? CaX O 2.5446(8) 93_655 ? CaX AsT 3.1232 . ? CaX AsT 3.1232 50_556 ? CaX MnY 3.4919 . ? MnY O 2.1538(7) 84_545 ? MnY O 2.1538(7) 80_455 ? MnY O 2.1538(7) 76_554 ? MnY O 2.1538(7) 36_454 ? MnY O 2.1538(7) 32_544 ? MnY O 2.1538(7) 28_445 ? MnY CaX 3.4919 57 ? MnY NaX 3.4919 49 ? MnY NaX 3.4919 5 ? MnY NaX 3.4919 53 ? MnY NaX 3.4919 9 ? AsT O 1.6927(7) 27_545 ? AsT O 1.6927(7) 90_565 ? AsT O 1.6927(7) 67_656 ? AsT O 1.6927(7) 2_554 ? AsT CaX 3.1232 50_656 ? AsT NaX 3.1232 50_656 ? O AsT 1.6927(7) 2 ? O MgY 2.1538(7) 28_445 ? O MnY 2.1538(7) 28_445 ? O CaX 2.4424(8) 49_556 ? O NaX 2.4424(8) 49_556 ? O NaX 2.5446(8) 58_566 ? O CaX 2.5446(8) 58_566 ? 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 O CaX O 164.32(4) 76_554 67_656 ? O CaX O 65.17(3) 76_554 49_556 ? O CaX O 117.20(3) 67_656 49_556 ? O CaX O 117.20(3) 76_554 90_565 ? O CaX O 65.17(3) 67_656 90_565 ? O CaX O 164.32(4) 49_556 90_565 ? O CaX O 91.78(2) 76_554 70_656 ? O CaX O 75.22(3) 67_656 70_656 ? O CaX O 71.74(3) 49_556 70_656 ? O CaX O 122.502(15) 90_565 70_656 ? O CaX O 122.502(15) 76_554 55_556 ? O CaX O 71.74(3) 67_656 55_556 ? O CaX O 75.22(3) 49_556 55_556 ? O CaX O 91.78(2) 90_565 55_556 ? O CaX O 113.89(3) 70_656 55_556 ? O CaX O 75.22(3) 76_554 80_455 ? O CaX O 91.78(2) 67_656 80_455 ? O CaX O 122.502(16) 49_556 80_455 ? O CaX O 71.74(3) 90_565 80_455 ? O CaX O 69.58(4) 70_656 80_455 ? O CaX O 160.71(3) 55_556 80_455 ? O CaX O 71.74(3) 76_554 93_655 ? O CaX O 122.502(15) 67_656 93_655 ? O CaX O 91.78(2) 49_556 93_655 ? O CaX O 75.22(3) 90_565 93_655 ? O CaX O 160.71(3) 70_656 93_655 ? O CaX O 69.58(4) 55_556 93_655 ? O CaX O 113.89(3) 80_455 93_655 ? O CaX AsT 147.414(17) 76_554 . ? O CaX AsT 32.586(17) 67_656 . ? O CaX AsT 147.414(17) 49_556 . ? O CaX AsT 32.586(17) 90_565 . ? O CaX AsT 99.643(16) 70_656 . ? O CaX AsT 80.357(16) 55_556 . ? O CaX AsT 80.357(16) 80_455 . ? O CaX AsT 99.643(16) 93_655 . ? O CaX AsT 32.586(17) 76_554 50_556 ? O CaX AsT 147.414(17) 67_656 50_556 ? O CaX AsT 32.586(17) 49_556 50_556 ? O CaX AsT 147.414(17) 90_565 50_556 ? O CaX AsT 80.357(16) 70_656 50_556 ? O CaX AsT 99.643(16) 55_556 50_556 ? O CaX AsT 99.643(16) 80_455 50_556 ? O CaX AsT 80.357(16) 93_655 50_556 ? AsT CaX AsT 180.0 . 50_556 ? O CaX MnY 37.571(17) 76_554 . ? O CaX MnY 128.320(18) 67_656 . ? O CaX MnY 92.234(17) 49_556 . ? O CaX MnY 97.676(18) 90_565 . ? O CaX MnY 75.560(17) 70_656 . ? O CaX MnY 159.929(17) 55_556 . ? O CaX MnY 37.866(16) 80_455 . ? O CaX MnY 95.713(17) 93_655 . ? AsT CaX MnY 116.6 . . ? AsT CaX MnY 63.4 50_556 . ? O MnY O 89.95(3) 84_545 80_455 ? O MnY O 89.95(3) 84_545 76_554 ? O MnY O 89.95(3) 80_455 76_554 ? O MnY O 180.00(6) 84_545 36_454 ? O MnY O 90.05(3) 80_455 36_454 ? O MnY O 90.05(3) 76_554 36_454 ? O MnY O 90.05(3) 84_545 32_544 ? O MnY O 180.00(6) 80_455 32_544 ? O MnY O 90.05(3) 76_554 32_544 ? O MnY O 89.95(3) 36_454 32_544 ? O MnY O 90.05(3) 84_545 28_445 ? O MnY O 90.05(3) 80_455 28_445 ? O MnY O 180.00(6) 76_554 28_445 ? O MnY O 89.95(3) 36_454 28_445 ? O MnY O 89.95(3) 32_544 28_445 ? O MnY CaX 93.91(2) 84_545 . ? O MnY CaX 46.48(2) 80_455 . ? O MnY CaX 43.74(2) 76_554 . ? O MnY CaX 86.09(2) 36_454 . ? O MnY CaX 133.52(2) 32_544 . ? O MnY CaX 136.26(2) 28_445 . ? O MnY CaX 136.26(2) 84_545 57 ? O MnY CaX 86.09(2) 80_455 57 ? O MnY CaX 133.52(2) 76_554 57 ? O MnY CaX 43.74(2) 36_454 57 ? O MnY CaX 93.91(2) 32_544 57 ? O MnY CaX 46.48(2) 28_445 57 ? CaX MnY CaX 113.6 . 57 ? O MnY NaX 86.09(2) 84_545 49 ? O MnY NaX 133.52(2) 80_455 49 ? O MnY NaX 136.26(2) 76_554 49 ? O MnY NaX 93.91(2) 36_454 49 ? O MnY NaX 46.48(2) 32_544 49 ? O MnY NaX 43.74(2) 28_445 49 ? CaX MnY NaX 180.0 . 49 ? CaX MnY NaX 66.4 57 49 ? O MnY NaX 46.48(2) 84_545 5 ? O MnY NaX 43.74(2) 80_455 5 ? O MnY NaX 93.91(2) 76_554 5 ? O MnY NaX 133.52(2) 36_454 5 ? O MnY NaX 136.26(2) 32_544 5 ? O MnY NaX 86.09(2) 28_445 5 ? CaX MnY NaX 66.4 . 5 ? CaX MnY NaX 113.6 57 5 ? NaX MnY NaX 113.6 49 5 ? O MnY NaX 133.52(2) 84_545 53 ? O MnY NaX 136.26(2) 80_455 53 ? O MnY NaX 86.09(2) 76_554 53 ? O MnY NaX 46.48(2) 36_454 53 ? O MnY NaX 43.74(2) 32_544 53 ? O MnY NaX 93.91(2) 28_445 53 ? CaX MnY NaX 113.6 . 53 ? CaX MnY NaX 66.4 57 53 ? NaX MnY NaX 66.4 49 53 ? NaX MnY NaX 180.0 5 53 ? O MnY NaX 43.74(2) 84_545 9 ? O MnY NaX 93.91(2) 80_455 9 ? O MnY NaX 46.48(2) 76_554 9 ? O MnY NaX 136.26(2) 36_454 9 ? O MnY NaX 86.09(2) 32_544 9 ? O MnY NaX 133.52(2) 28_445 9 ? CaX MnY NaX 66.4 . 9 ? CaX MnY NaX 180.0 57 9 ? NaX MnY NaX 113.6 49 9 ? NaX MnY NaX 66.4 5 9 ? NaX MnY NaX 113.6 53 9 ? O AsT O 113.33(3) 27_545 90_565 ? O AsT O 113.33(3) 27_545 67_656 ? O AsT O 101.99(5) 90_565 67_656 ? O AsT O 101.99(5) 27_545 2_554 ? O AsT O 113.33(3) 90_565 2_554 ? O AsT O 113.33(3) 67_656 2_554 ? O AsT CaX 51.00(3) 27_545 50_656 ? O AsT CaX 129.00(3) 90_565 50_656 ? O AsT CaX 129.00(3) 67_656 50_656 ? O AsT CaX 51.00(3) 2_554 50_656 ? O AsT NaX 51.00(3) 27_545 50_656 ? O AsT NaX 129.00(3) 90_565 50_656 ? O AsT NaX 129.00(3) 67_656 50_656 ? O AsT NaX 51.00(3) 2_554 50_656 ? CaX AsT NaX 0.0 50_656 50_656 ? O AsT CaX 129.00(3) 27_545 . ? O AsT CaX 51.00(3) 90_565 . ? O AsT CaX 51.00(3) 67_656 . ? O AsT CaX 129.00(3) 2_554 . ? CaX AsT CaX 180.0 50_656 . ? NaX AsT CaX 180.0 50_656 . ? AsT O MgY 130.02(4) 2 28_445 ? AsT O MnY 130.02(4) 2 28_445 ? MgY O MnY 0.0 28_445 28_445 ? AsT O CaX 96.42(3) 2 49_556 ? MgY O CaX 98.69(3) 28_445 49_556 ? MnY O CaX 98.69(3) 28_445 49_556 ? AsT O NaX 96.42(3) 2 49_556 ? MgY O NaX 98.69(3) 28_445 49_556 ? MnY O NaX 98.69(3) 28_445 49_556 ? CaX O NaX 0.0 49_556 49_556 ? AsT O NaX 127.90(4) 2 58_566 ? MgY O NaX 95.65(3) 28_445 58_566 ? MnY O NaX 95.65(3) 28_445 58_566 ? CaX O NaX 100.16(3) 49_556 58_566 ? NaX O NaX 100.16(3) 49_556 58_566 ? AsT O CaX 127.90(4) 2 58_566 ? MgY O CaX 95.65(3) 28_445 58_566 ? MnY O CaX 95.65(3) 28_445 58_566 ? CaX O CaX 100.16(3) 49_556 58_566 ? NaX O CaX 100.16(3) 49_556 58_566 ? NaX O CaX 0.0 58_566 58_566 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 35.95 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.211 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.069