data_gold _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.13 Ca3 Cr0.13 Mn0.13 O12 Si3 V2' _chemical_formula_weight 515.13 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' 'Si' 'Si' 0.0817 0.0704 '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' 'V' 'V' 0.3005 0.5294 '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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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 12.0279(9) _cell_length_b 12.0279(9) _cell_length_c 12.0279(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1740.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2014 _exptl_absorpt_coefficient_mu 4.744 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 2711 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 8.66 _diffrn_reflns_theta_max 34.95 _reflns_number_total 320 _reflns_number_gt 248 _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^)+(0.0175P)^2^+3.4874P] 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 0.00041(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 320 _refine_ls_number_parameters 23 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0510 _refine_ls_wR_factor_gt 0.0455 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.066 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.1250 0.0000 0.2500 0.00736(14) Uani 0.927(1) 4 d SP . . Mn Mn 0.1250 0.0000 0.2500 0.00736(14) Uani 0.057(1) 4 d SP . . V V 0.0000 0.0000 0.0000 0.00539(14) Uani 0.810(1) 6 d SP . . Al Al 0.0000 0.0000 0.0000 0.00539(14) Uani 0.110(1) 6 d SP . . Cr Cr 0.0000 0.0000 0.0000 0.00539(14) Uani 0.080(1) 6 d SP . . Si Si 0.3750 0.0000 0.2500 0.00559(16) Uani 1 4 d S . . O O 0.03916(8) 0.04789(8) 0.65493(8) 0.0084(2) 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 Ca 0.0053(2) 0.00840(17) 0.00840(17) 0.00141(17) 0.000 0.000 Mn 0.0053(2) 0.00840(17) 0.00840(17) 0.00141(17) 0.000 0.000 V 0.00539(14) 0.00539(14) 0.00539(14) 0.00009(10) 0.00009(10) 0.00009(10) Al 0.00539(14) 0.00539(14) 0.00539(14) 0.00009(10) 0.00009(10) 0.00009(10) Cr 0.00539(14) 0.00539(14) 0.00539(14) 0.00009(10) 0.00009(10) 0.00009(10) Si 0.0060(3) 0.0054(2) 0.0054(2) 0.000 0.000 0.000 O 0.0085(4) 0.0087(4) 0.0080(4) 0.0000(3) -0.0004(3) 0.0002(3) _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 Ca O 2.3533(10) 90_565 ? Ca O 2.3533(10) 76_554 ? Ca O 2.3533(10) 67_656 ? Ca O 2.3533(10) 49_556 ? Ca O 2.5022(10) 70_656 ? Ca O 2.5022(10) 55_556 ? Ca O 2.5022(10) 80_455 ? Ca O 2.5022(10) 93_655 ? Ca Si 3.0070(2) . ? Ca Si 3.0070(2) 50_556 ? Ca V 3.3619(3) . ? V O 2.0065(10) 80_455 ? V O 2.0065(10) 32_544 ? V O 2.0065(10) 76_554 ? V O 2.0065(10) 28_445 ? V O 2.0065(10) 84_545 ? V O 2.0065(10) 36_454 ? V Ca 3.3619(3) 9 ? V Ca 3.3619(3) 53 ? V Ca 3.3619(3) 5 ? V Ca 3.3619(3) 49 ? V Ca 3.3619(3) 57 ? Si O 1.6449(10) 27_545 ? Si O 1.6449(10) 67_656 ? Si O 1.6449(10) 2_554 ? Si O 1.6449(10) 90_565 ? Si Ca 3.0070(2) 50_656 ? Si Mn 3.0070(2) 50_656 ? O Si 1.6449(10) 2 ? O Cr 2.0065(10) 28_445 ? O Al 2.0065(10) 28_445 ? O V 2.0065(10) 28_445 ? O Ca 2.3533(10) 49_556 ? O Mn 2.3533(10) 49_556 ? O Mn 2.5022(10) 58_566 ? O Ca 2.5022(10) 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 Ca O 117.78(5) 90_565 76_554 ? O Ca O 65.93(5) 90_565 67_656 ? O Ca O 160.36(5) 76_554 67_656 ? O Ca O 160.36(5) 90_565 49_556 ? O Ca O 65.93(5) 76_554 49_556 ? O Ca O 117.78(5) 67_656 49_556 ? O Ca O 123.14(2) 90_565 70_656 ? O Ca O 91.47(3) 76_554 70_656 ? O Ca O 72.22(5) 67_656 70_656 ? O Ca O 74.51(4) 49_556 70_656 ? O Ca O 91.47(3) 90_565 55_556 ? O Ca O 123.14(2) 76_554 55_556 ? O Ca O 74.51(4) 67_656 55_556 ? O Ca O 72.22(5) 49_556 55_556 ? O Ca O 112.73(5) 70_656 55_556 ? O Ca O 74.51(4) 90_565 80_455 ? O Ca O 72.22(5) 76_554 80_455 ? O Ca O 91.47(3) 67_656 80_455 ? O Ca O 123.14(2) 49_556 80_455 ? O Ca O 69.82(5) 70_656 80_455 ? O Ca O 163.46(5) 55_556 80_455 ? O Ca O 72.22(5) 90_565 93_655 ? O Ca O 74.51(4) 76_554 93_655 ? O Ca O 123.14(2) 67_656 93_655 ? O Ca O 91.47(3) 49_556 93_655 ? O Ca O 163.46(4) 70_656 93_655 ? O Ca O 69.82(5) 55_556 93_655 ? O Ca O 112.73(5) 80_455 93_655 ? O Ca Si 32.96(2) 90_565 . ? O Ca Si 147.04(2) 76_554 . ? O Ca Si 32.96(2) 67_656 . ? O Ca Si 147.04(2) 49_556 . ? O Ca Si 98.27(2) 70_656 . ? O Ca Si 81.73(2) 55_556 . ? O Ca Si 81.73(2) 80_455 . ? O Ca Si 98.27(2) 93_655 . ? O Ca Si 147.04(2) 90_565 50_556 ? O Ca Si 32.96(2) 76_554 50_556 ? O Ca Si 147.04(2) 67_656 50_556 ? O Ca Si 32.96(2) 49_556 50_556 ? O Ca Si 81.73(2) 70_656 50_556 ? O Ca Si 98.27(2) 55_556 50_556 ? O Ca Si 98.27(2) 80_455 50_556 ? O Ca Si 81.73(2) 93_655 50_556 ? Si Ca Si 180.0 . 50_556 ? O Ca V 98.99(2) 90_565 . ? O Ca V 35.92(2) 76_554 . ? O Ca V 126.45(2) 67_656 . ? O Ca V 93.41(2) 49_556 . ? O Ca V 76.54(2) 70_656 . ? O Ca V 158.96(2) 55_556 . ? O Ca V 36.43(2) 80_455 . ? O Ca V 95.97(2) 93_655 . ? Si Ca V 116.6 . . ? Si Ca V 63.4 50_556 . ? O V O 180.00(8) 80_455 32_544 ? O V O 91.07(4) 80_455 76_554 ? O V O 88.93(4) 32_544 76_554 ? O V O 88.93(4) 80_455 28_445 ? O V O 91.07(4) 32_544 28_445 ? O V O 180.00(6) 76_554 28_445 ? O V O 91.07(4) 80_455 84_545 ? O V O 88.93(4) 32_544 84_545 ? O V O 91.07(4) 76_554 84_545 ? O V O 88.93(4) 28_445 84_545 ? O V O 88.93(4) 80_455 36_454 ? O V O 91.07(4) 32_544 36_454 ? O V O 88.93(4) 76_554 36_454 ? O V O 91.07(4) 28_445 36_454 ? O V O 180.00(6) 84_545 36_454 ? O V Ca 94.68(3) 80_455 9 ? O V Ca 85.32(3) 32_544 9 ? O V Ca 47.77(3) 76_554 9 ? O V Ca 132.23(3) 28_445 9 ? O V Ca 43.47(3) 84_545 9 ? O V Ca 136.53(3) 36_454 9 ? O V Ca 136.53(3) 80_455 53 ? O V Ca 43.47(3) 32_544 53 ? O V Ca 85.32(3) 76_554 53 ? O V Ca 94.68(3) 28_445 53 ? O V Ca 132.23(3) 84_545 53 ? O V Ca 47.77(3) 36_454 53 ? Ca V Ca 113.6 9 53 ? O V Ca 43.47(3) 80_455 5 ? O V Ca 136.53(3) 32_544 5 ? O V Ca 94.68(3) 76_554 5 ? O V Ca 85.32(3) 28_445 5 ? O V Ca 47.77(3) 84_545 5 ? O V Ca 132.23(3) 36_454 5 ? Ca V Ca 66.4 9 5 ? Ca V Ca 180.0 53 5 ? O V Ca 132.23(3) 80_455 49 ? O V Ca 47.77(3) 32_544 49 ? O V Ca 136.53(3) 76_554 49 ? O V Ca 43.47(3) 28_445 49 ? O V Ca 85.32(3) 84_545 49 ? O V Ca 94.68(3) 36_454 49 ? Ca V Ca 113.6 9 49 ? Ca V Ca 66.4 53 49 ? Ca V Ca 113.6 5 49 ? O V Ca 47.77(3) 80_455 . ? O V Ca 132.23(3) 32_544 . ? O V Ca 43.47(3) 76_554 . ? O V Ca 136.53(3) 28_445 . ? O V Ca 94.68(3) 84_545 . ? O V Ca 85.32(3) 36_454 . ? Ca V Ca 66.4 9 . ? Ca V Ca 113.6 53 . ? Ca V Ca 66.4 5 . ? Ca V Ca 180.0 49 . ? O V Ca 85.32(3) 80_455 57 ? O V Ca 94.68(3) 32_544 57 ? O V Ca 132.23(3) 76_554 57 ? O V Ca 47.77(3) 28_445 57 ? O V Ca 136.53(3) 84_545 57 ? O V Ca 43.47(3) 36_454 57 ? Ca V Ca 180.0 9 57 ? Ca V Ca 66.4 53 57 ? Ca V Ca 113.6 5 57 ? Ca V Ca 66.4 49 57 ? Ca V Ca 113.6 . 57 ? O Si O 113.21(4) 27_545 67_656 ? O Si O 102.23(7) 27_545 2_554 ? O Si O 113.21(4) 67_656 2_554 ? O Si O 113.21(4) 27_545 90_565 ? O Si O 102.23(7) 67_656 90_565 ? O Si O 113.21(4) 2_554 90_565 ? O Si Ca 51.12(3) 27_545 50_656 ? O Si Ca 128.88(3) 67_656 50_656 ? O Si Ca 51.12(3) 2_554 50_656 ? O Si Ca 128.88(3) 90_565 50_656 ? O Si Ca 128.88(3) 27_545 . ? O Si Ca 51.12(3) 67_656 . ? O Si Ca 128.88(3) 2_554 . ? O Si Ca 51.12(3) 90_565 . ? Ca Si Ca 180.0 50_656 . ? O Si Mn 51.12(3) 27_545 50_656 ? O Si Mn 128.88(3) 67_656 50_656 ? O Si Mn 51.12(3) 2_554 50_656 ? O Si Mn 128.88(3) 90_565 50_656 ? Ca Si Mn 0.0 50_656 50_656 ? Ca Si Mn 180.0 . 50_656 ? Si O Cr 133.83(6) 2 28_445 ? Si O Al 133.83(6) 2 28_445 ? Cr O Al 0.0 28_445 28_445 ? Si O V 133.83(6) 2 28_445 ? Cr O V 0.0 28_445 28_445 ? Al O V 0.0 28_445 28_445 ? Si O Ca 95.92(4) 2 49_556 ? Cr O Ca 100.61(4) 28_445 49_556 ? Al O Ca 100.61(4) 28_445 49_556 ? V O Ca 100.61(4) 28_445 49_556 ? Si O Mn 95.92(4) 2 49_556 ? Cr O Mn 100.61(4) 28_445 49_556 ? Al O Mn 100.61(4) 28_445 49_556 ? V O Mn 100.61(4) 28_445 49_556 ? Ca O Mn 0.0 49_556 49_556 ? Si O Mn 123.94(5) 2 58_566 ? Cr O Mn 95.80(4) 28_445 58_566 ? Al O Mn 95.80(4) 28_445 58_566 ? V O Mn 95.80(4) 28_445 58_566 ? Ca O Mn 98.61(4) 49_556 58_566 ? Mn O Mn 98.61(4) 49_556 58_566 ? Si O Ca 123.94(5) 2 58_566 ? Cr O Ca 95.80(4) 28_445 58_566 ? Al O Ca 95.80(4) 28_445 58_566 ? V O Ca 95.80(4) 28_445 58_566 ? Ca O Ca 98.61(4) 49_556 58_566 ? Mn O Ca 98.61(4) 49_556 58_566 ? Mn O Ca 0.0 58_566 58_566 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 34.95 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.351 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.088