data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H Al Ca Ce Fe2 O13 Si3' _chemical_formula_weight 612.16 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' 'H' 'H' 0.0000 0.0000 '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' '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 '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, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.9393(2) _cell_length_b 5.81580(10) _cell_length_c 10.1643(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.8240(10) _cell_angle_gamma 90.00 _cell_volume 479.607(16) _cell_formula_units_Z 2 _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 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 8.737 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3743 _exptl_absorpt_correction_T_max 0.7213 _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 12238 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 36.38 _reflns_number_total 2465 _reflns_number_gt 2367 _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^)+(0.0161P)^2^+0.3456P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2465 _refine_ls_number_parameters 125 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0368 _refine_ls_wR_factor_gt 0.0365 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.002 _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 Ca1 Ca 0.75946(5) 0.7500 0.15168(4) 0.01143(10) Uani 1.003(3) 2 d SP . . Ce2 Ce 0.594052(13) 0.7500 0.429063(10) 0.00866(3) Uani 0.958(2) 2 d SP . . Ca2 Ca 0.594052(13) 0.7500 0.429063(10) 0.00866(3) Uani 0.042(2) 2 d SP . . Al1 Al 0.0000 0.0000 0.0000 0.00669(8) Uani 0.267(4) 2 d SP . . Fe1 Fe 0.0000 0.0000 0.0000 0.00669(8) Uani 0.733(4) 2 d SP . . Al2 Al 0.0000 0.0000 0.5000 0.00675(13) Uani 0.817(3) 2 d SP . . Fe2 Fe 0.0000 0.0000 0.5000 0.00675(13) Uani 0.183(3) 2 d SP . . Fe3 Fe 0.30527(3) 0.2500 0.21529(3) 0.00884(8) Uani 0.966(4) 2 d SP . . Al3 Al 0.30527(3) 0.2500 0.21529(3) 0.00884(8) Uani 0.034(4) 2 d SP . . Si1 Si 0.34128(6) 0.7500 0.03697(5) 0.00648(9) Uani 1 2 d S . . Si2 Si 0.68609(6) 0.2500 0.27869(5) 0.00684(9) Uani 1 2 d S . . Si3 Si 0.19065(6) 0.7500 0.32616(5) 0.00636(9) Uani 1 2 d S . . O1 O 0.23700(12) 0.98635(17) 0.02529(10) 0.00948(17) Uani 1 1 d . . . O2 O 0.31524(12) 0.96881(17) 0.36745(10) 0.00943(16) Uani 1 1 d . . . O3 O 0.79535(12) 0.01642(17) 0.33526(10) 0.01045(17) Uani 1 1 d . . . O4 O 0.06058(17) 0.2500 0.13633(15) 0.0108(2) Uani 1 2 d S . . O5 O 0.05198(17) 0.7500 0.15525(14) 0.0092(2) Uani 1 2 d S . . O6 O 0.07001(17) 0.7500 0.41144(15) 0.0107(2) Uani 1 2 d S . . O7 O 0.51035(17) 0.7500 0.17923(14) 0.0111(2) Uani 1 2 d S . . O8 O 0.54263(18) 0.2500 0.33314(15) 0.0159(3) Uani 1 2 d S . . O9 O 0.60762(19) 0.2500 0.10080(15) 0.0129(3) Uani 1 2 d S . . O10 O 0.08891(17) 0.2500 0.42996(14) 0.0108(2) Uani 1 2 d SD . . H10 H 0.070(5) 0.2500 0.3281(16) 0.050 Uiso 1 2 d SD . . 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 Ca1 0.0173(2) 0.00900(17) 0.01156(16) 0.000 0.00951(14) 0.000 Ce2 0.00735(5) 0.01107(5) 0.00665(4) 0.000 0.00204(3) 0.000 Ca2 0.00735(5) 0.01107(5) 0.00665(4) 0.000 0.00204(3) 0.000 Al1 0.00595(14) 0.00660(14) 0.00719(12) 0.00049(9) 0.00243(10) -0.00012(9) Fe1 0.00595(14) 0.00660(14) 0.00719(12) 0.00049(9) 0.00243(10) -0.00012(9) Al2 0.0053(2) 0.0066(2) 0.00717(19) -0.00095(14) 0.00150(15) 0.00069(14) Fe2 0.0053(2) 0.0066(2) 0.00717(19) -0.00095(14) 0.00150(15) 0.00069(14) Fe3 0.00610(12) 0.00970(13) 0.00856(12) 0.000 0.00095(9) 0.000 Al3 0.00610(12) 0.00970(13) 0.00856(12) 0.000 0.00095(9) 0.000 Si1 0.0065(2) 0.0064(2) 0.00610(18) 0.000 0.00222(16) 0.000 Si2 0.0065(2) 0.0073(2) 0.00684(19) 0.000 0.00293(17) 0.000 Si3 0.0056(2) 0.0070(2) 0.00627(18) 0.000 0.00233(16) 0.000 O1 0.0092(4) 0.0075(4) 0.0120(4) 0.0007(3) 0.0047(3) 0.0013(3) O2 0.0086(4) 0.0088(4) 0.0098(4) 0.0001(3) 0.0028(3) -0.0017(3) O3 0.0101(4) 0.0069(4) 0.0116(4) -0.0008(3) 0.0018(3) 0.0006(3) O4 0.0082(6) 0.0112(6) 0.0114(5) 0.000 0.0026(5) 0.000 O5 0.0082(6) 0.0110(6) 0.0068(5) 0.000 0.0015(4) 0.000 O6 0.0092(6) 0.0139(6) 0.0106(5) 0.000 0.0056(5) 0.000 O7 0.0088(6) 0.0147(6) 0.0073(5) 0.000 0.0009(5) 0.000 O8 0.0074(6) 0.0318(9) 0.0090(5) 0.000 0.0041(5) 0.000 O9 0.0129(6) 0.0187(7) 0.0081(5) 0.000 0.0055(5) 0.000 O10 0.0093(6) 0.0138(6) 0.0092(5) 0.000 0.0040(5) 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 Ca1 O3 2.3415(10) 1_565 ? Ca1 O3 2.3415(10) 4_565 ? Ca1 O7 2.3581(15) . ? Ca1 O1 2.3739(10) 2_645 ? Ca1 O1 2.3739(10) 3_675 ? Ca1 O5 2.5999(15) 1_655 ? Ca1 O6 2.9195(15) 1_655 ? Ca1 Si2 3.3561(3) . ? Ca1 Si2 3.3561(3) 1_565 ? Ca1 Si1 3.3902(3) 3_665 ? Ca1 Si1 3.3902(3) 3_675 ? Ca1 Si1 3.4167(7) . ? Ce2 O7 2.3265(13) . ? Ce2 O2 2.4902(10) 3_676 ? Ce2 O2 2.4902(10) 2_646 ? Ce2 O10 2.5837(14) 3_666 ? Ce2 O2 2.6293(10) 4_575 ? Ce2 O2 2.6293(10) . ? Ce2 O3 2.8264(10) 1_565 ? Ce2 O3 2.8264(10) 4_565 ? Ce2 Si3 3.3063(5) . ? Ce2 Fe3 3.3386(3) 3_666 ? Ce2 Al3 3.3386(3) 3_666 ? Al1 O4 1.9228(9) . ? Al1 O4 1.9228(9) 3 ? Al1 O1 2.0257(10) 3_565 ? Al1 O1 2.0257(10) 1_545 ? Al1 O5 2.0504(9) 3_565 ? Al1 O5 2.0504(9) 1_545 ? Al1 Al1 2.9079 2 ? Al1 Fe1 2.9079 2 ? Al1 Al1 2.9079 2_545 ? Al1 Fe1 2.9079 2_545 ? Al1 Ca1 3.4494(3) 3_665 ? Al1 Ca1 3.4494(3) 1_445 ? Al2 O3 1.8941(10) 3_656 ? Al2 O3 1.8941(10) 1_455 ? Al2 O10 1.9307(9) . ? Al2 O10 1.9307(9) 3_556 ? Al2 O6 1.9465(9) 3_566 ? Al2 O6 1.9465(9) 1_545 ? Al2 Al2 2.9079 2_546 ? Al2 Al2 2.9079 2_556 ? Al2 Fe2 2.9079 2_546 ? Al2 Fe2 2.9079 2_556 ? Al2 Ca1 3.5889(4) 1_445 ? Al2 Ca1 3.5889(4) 3_666 ? Fe3 O8 1.9501(15) . ? Fe3 O4 1.9887(14) . ? Fe3 O2 2.2268(10) 4_575 ? Fe3 O2 2.2268(10) 1_545 ? Fe3 O1 2.3374(10) 1_545 ? Fe3 O1 2.3374(10) 4_575 ? Fe3 Ce2 3.3386(3) 3_666 ? Fe3 Ca2 3.3386(3) 3_666 ? Fe3 Ca1 3.5264(5) 3_665 ? Si1 O7 1.5938(14) . ? Si1 O1 1.6370(10) 4_575 ? Si1 O1 1.6370(10) . ? Si1 O9 1.6452(14) 3_665 ? Si1 Ca1 3.3902(3) 3_665 ? Si1 Ca1 3.3902(3) 3_675 ? Si2 O8 1.5960(15) . ? Si2 O3 1.6305(10) . ? Si2 O3 1.6305(10) 4_565 ? Si2 O9 1.6420(14) . ? Si2 Ca1 3.3561(3) 1_545 ? Si2 Ca2 3.5391(3) 1_545 ? Si3 O2 1.6259(10) . ? Si3 O2 1.6259(10) 4_575 ? Si3 O6 1.6430(14) . ? Si3 O5 1.6572(14) . ? Si3 Ca1 3.5019(7) 1_455 ? O1 Fe1 2.0258(10) 1_565 ? O1 Al1 2.0258(10) 1_565 ? O1 Al3 2.3374(10) 1_565 ? O1 Fe3 2.3374(10) 1_565 ? O1 Ca1 2.3739(10) 3_675 ? O2 Al3 2.2268(10) 1_565 ? O2 Fe3 2.2268(10) 1_565 ? O2 Ca2 2.4903(10) 3_676 ? O2 Ce2 2.4903(10) 3_676 ? O3 Fe2 1.8941(10) 1_655 ? O3 Al2 1.8941(10) 1_655 ? O3 Ca1 2.3415(10) 1_545 ? O3 Ca2 2.8264(10) 1_545 ? O3 Ce2 2.8264(10) 1_545 ? O4 Fe1 1.9228(9) 2 ? O4 Al1 1.9228(9) 2 ? O5 Fe1 2.0504(9) 2 ? O5 Al1 2.0504(9) 2 ? O5 Fe1 2.0504(9) 1_565 ? O5 Al1 2.0504(9) 1_565 ? O5 Ca1 2.6000(15) 1_455 ? O6 Fe2 1.9465(9) 1_565 ? O6 Al2 1.9465(9) 1_565 ? O6 Fe2 1.9465(9) 2_556 ? O6 Al2 1.9465(9) 2_556 ? O6 Ca1 2.9195(15) 1_455 ? O8 Ca2 3.0400(4) 1_545 ? O9 Si1 1.6451(14) 3_665 ? O10 Fe2 1.9307(9) 2_556 ? O10 Al2 1.9307(9) 2_556 ? O10 Ce2 2.5836(14) 3_666 ? O10 Ca2 2.5836(14) 3_666 ? O10 H10 0.975(10) . ? 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 O3 Ca1 O3 82.86(5) 1_565 4_565 ? O3 Ca1 O7 74.08(4) 1_565 . ? O3 Ca1 O7 74.08(4) 4_565 . ? O3 Ca1 O1 172.00(4) 1_565 2_645 ? O3 Ca1 O1 97.79(3) 4_565 2_645 ? O7 Ca1 O1 113.81(4) . 2_645 ? O3 Ca1 O1 97.79(3) 1_565 3_675 ? O3 Ca1 O1 172.00(4) 4_565 3_675 ? O7 Ca1 O1 113.81(4) . 3_675 ? O1 Ca1 O1 80.47(5) 2_645 3_675 ? O3 Ca1 O5 100.86(4) 1_565 1_655 ? O3 Ca1 O5 100.86(4) 4_565 1_655 ? O7 Ca1 O5 173.09(5) . 1_655 ? O1 Ca1 O5 71.17(3) 2_645 1_655 ? O1 Ca1 O5 71.17(3) 3_675 1_655 ? O3 Ca1 O6 61.26(3) 1_565 1_655 ? O3 Ca1 O6 61.26(3) 4_565 1_655 ? O7 Ca1 O6 118.65(4) . 1_655 ? O1 Ca1 O6 112.03(3) 2_645 1_655 ? O1 Ca1 O6 112.03(3) 3_675 1_655 ? O5 Ca1 O6 54.44(4) 1_655 1_655 ? O3 Ca1 Si2 104.50(3) 1_565 . ? O3 Ca1 Si2 26.32(3) 4_565 . ? O7 Ca1 Si2 66.893(15) . . ? O1 Ca1 Si2 78.39(2) 2_645 . ? O1 Ca1 Si2 156.64(3) 3_675 . ? O5 Ca1 Si2 110.637(15) 1_655 . ? O6 Ca1 Si2 85.257(17) 1_655 . ? O3 Ca1 Si2 26.32(3) 1_565 1_565 ? O3 Ca1 Si2 104.50(3) 4_565 1_565 ? O7 Ca1 Si2 66.892(15) . 1_565 ? O1 Ca1 Si2 156.64(3) 2_645 1_565 ? O1 Ca1 Si2 78.39(2) 3_675 1_565 ? O5 Ca1 Si2 110.638(16) 1_655 1_565 ? O6 Ca1 Si2 85.257(17) 1_655 1_565 ? Si2 Ca1 Si2 120.098(18) . 1_565 ? O3 Ca1 Si1 158.95(3) 1_565 3_665 ? O3 Ca1 Si1 78.35(3) 4_565 3_665 ? O7 Ca1 Si1 91.57(2) . 3_665 ? O1 Ca1 Si1 26.14(2) 2_645 3_665 ? O1 Ca1 Si1 102.14(3) 3_675 3_665 ? O5 Ca1 Si1 91.987(19) 1_655 3_665 ? O6 Ca1 Si1 115.940(13) 1_655 3_665 ? Si2 Ca1 Si1 54.968(11) . 3_665 ? Si2 Ca1 Si1 155.831(18) 1_565 3_665 ? O3 Ca1 Si1 78.35(3) 1_565 3_675 ? O3 Ca1 Si1 158.95(3) 4_565 3_675 ? O7 Ca1 Si1 91.57(2) . 3_675 ? O1 Ca1 Si1 102.14(3) 2_645 3_675 ? O1 Ca1 Si1 26.14(2) 3_675 3_675 ? O5 Ca1 Si1 91.987(19) 1_655 3_675 ? O6 Ca1 Si1 115.940(13) 1_655 3_675 ? Si2 Ca1 Si1 155.831(18) . 3_675 ? Si2 Ca1 Si1 54.968(11) 1_565 3_675 ? Si1 Ca1 Si1 118.126(18) 3_665 3_675 ? O3 Ca1 Si1 92.07(3) 1_565 . ? O3 Ca1 Si1 92.07(3) 4_565 . ? O7 Ca1 Si1 24.23(3) . . ? O1 Ca1 Si1 95.86(3) 2_645 . ? O1 Ca1 Si1 95.86(3) 3_675 . ? O5 Ca1 Si1 162.68(3) 1_655 . ? O6 Ca1 Si1 142.88(3) 1_655 . ? Si2 Ca1 Si1 76.631(12) . . ? Si2 Ca1 Si1 76.631(12) 1_565 . ? Si1 Ca1 Si1 79.294(13) 3_665 . ? Si1 Ca1 Si1 79.294(13) 3_675 . ? O7 Ce2 O2 138.58(2) . 3_676 ? O7 Ce2 O2 138.58(2) . 2_646 ? O2 Ce2 O2 82.10(4) 3_676 2_646 ? O7 Ce2 O10 112.37(5) . 3_666 ? O2 Ce2 O10 68.93(3) 3_676 3_666 ? O2 Ce2 O10 68.93(3) 2_646 3_666 ? O7 Ce2 O2 84.36(4) . 4_575 ? O2 Ce2 O2 117.466(18) 3_676 4_575 ? O2 Ce2 O2 79.95(3) 2_646 4_575 ? O10 Ce2 O2 147.30(2) 3_666 4_575 ? O7 Ce2 O2 84.36(4) . . ? O2 Ce2 O2 79.95(3) 3_676 . ? O2 Ce2 O2 117.466(19) 2_646 . ? O10 Ce2 O2 147.30(3) 3_666 . ? O2 Ce2 O2 57.89(4) 4_575 . ? O7 Ce2 O3 65.82(3) . 1_565 ? O2 Ce2 O3 83.61(3) 3_676 1_565 ? O2 Ce2 O3 127.50(3) 2_646 1_565 ? O10 Ce2 O3 58.78(3) 3_666 1_565 ? O2 Ce2 O3 149.22(3) 4_575 1_565 ? O2 Ce2 O3 109.17(3) . 1_565 ? O7 Ce2 O3 65.82(3) . 4_565 ? O2 Ce2 O3 127.50(3) 3_676 4_565 ? O2 Ce2 O3 83.61(3) 2_646 4_565 ? O10 Ce2 O3 58.78(3) 3_666 4_565 ? O2 Ce2 O3 109.17(3) 4_575 4_565 ? O2 Ce2 O3 149.21(3) . 4_565 ? O3 Ce2 O3 66.49(4) 1_565 4_565 ? O7 Ce2 Si3 81.17(4) . . ? O2 Ce2 Si3 101.21(2) 3_676 . ? O2 Ce2 Si3 101.21(2) 2_646 . ? O10 Ce2 Si3 166.46(3) 3_666 . ? O2 Ce2 Si3 29.04(2) 4_575 . ? O2 Ce2 Si3 29.04(2) . . ? O3 Ce2 Si3 131.12(2) 1_565 . ? O3 Ce2 Si3 131.12(2) 4_565 . ? O7 Ce2 Fe3 177.19(4) . 3_666 ? O2 Ce2 Fe3 41.84(2) 3_676 3_666 ? O2 Ce2 Fe3 41.84(2) 2_646 3_666 ? O10 Ce2 Fe3 70.44(3) 3_666 3_666 ? O2 Ce2 Fe3 93.18(2) 4_575 3_666 ? O2 Ce2 Fe3 93.18(2) . 3_666 ? O3 Ce2 Fe3 116.42(2) 1_565 3_666 ? O3 Ce2 Fe3 116.42(2) 4_565 3_666 ? Si3 Ce2 Fe3 96.024(10) . 3_666 ? O7 Ce2 Al3 177.19(4) . 3_666 ? O2 Ce2 Al3 41.84(2) 3_676 3_666 ? O2 Ce2 Al3 41.84(2) 2_646 3_666 ? O10 Ce2 Al3 70.44(3) 3_666 3_666 ? O2 Ce2 Al3 93.18(2) 4_575 3_666 ? O2 Ce2 Al3 93.18(2) . 3_666 ? O3 Ce2 Al3 116.42(2) 1_565 3_666 ? O3 Ce2 Al3 116.42(2) 4_565 3_666 ? Si3 Ce2 Al3 96.024(10) . 3_666 ? Fe3 Ce2 Al3 0.000(10) 3_666 3_666 ? O7 Ce2 Ca1 38.28(4) . . ? O2 Ce2 Ca1 122.62(2) 3_676 . ? O2 Ce2 Ca1 122.62(2) 2_646 . ? O10 Ce2 Ca1 74.09(3) 3_666 . ? O2 Ce2 Ca1 117.49(2) 4_575 . ? O2 Ce2 Ca1 117.49(2) . . ? O3 Ce2 Ca1 39.35(2) 1_565 . ? O3 Ce2 Ca1 39.35(2) 4_565 . ? Si3 Ce2 Ca1 119.448(11) . . ? Fe3 Ce2 Ca1 144.529(9) 3_666 . ? Al3 Ce2 Ca1 144.529(9) 3_666 . ? O4 Al1 O4 180.00(9) . 3 ? O4 Al1 O1 91.43(5) . 3_565 ? O4 Al1 O1 88.57(5) 3 3_565 ? O4 Al1 O1 88.57(5) . 1_545 ? O4 Al1 O1 91.43(5) 3 1_545 ? O1 Al1 O1 180.00(8) 3_565 1_545 ? O4 Al1 O5 85.57(4) . 3_565 ? O4 Al1 O5 94.43(4) 3 3_565 ? O1 Al1 O5 89.29(5) 3_565 3_565 ? O1 Al1 O5 90.71(5) 1_545 3_565 ? O4 Al1 O5 94.43(4) . 1_545 ? O4 Al1 O5 85.57(4) 3 1_545 ? O1 Al1 O5 90.71(5) 3_565 1_545 ? O1 Al1 O5 89.29(5) 1_545 1_545 ? O5 Al1 O5 180.00(8) 3_565 1_545 ? O4 Al1 Al1 40.87(3) . 2 ? O4 Al1 Al1 139.13(3) 3 2 ? O1 Al1 Al1 87.75(3) 3_565 2 ? O1 Al1 Al1 92.25(3) 1_545 2 ? O5 Al1 Al1 44.84(3) 3_565 2 ? O5 Al1 Al1 135.16(3) 1_545 2 ? O4 Al1 Fe1 40.87(3) . 2 ? O4 Al1 Fe1 139.13(3) 3 2 ? O1 Al1 Fe1 87.75(3) 3_565 2 ? O1 Al1 Fe1 92.25(3) 1_545 2 ? O5 Al1 Fe1 44.84(3) 3_565 2 ? O5 Al1 Fe1 135.16(3) 1_545 2 ? Al1 Al1 Fe1 0.0 2 2 ? O4 Al1 Al1 139.13(3) . 2_545 ? O4 Al1 Al1 40.87(3) 3 2_545 ? O1 Al1 Al1 92.25(3) 3_565 2_545 ? O1 Al1 Al1 87.75(3) 1_545 2_545 ? O5 Al1 Al1 135.16(3) 3_565 2_545 ? O5 Al1 Al1 44.84(3) 1_545 2_545 ? Al1 Al1 Al1 180.0 2 2_545 ? Fe1 Al1 Al1 180.0 2 2_545 ? O4 Al1 Fe1 139.13(3) . 2_545 ? O4 Al1 Fe1 40.87(3) 3 2_545 ? O1 Al1 Fe1 92.25(3) 3_565 2_545 ? O1 Al1 Fe1 87.75(3) 1_545 2_545 ? O5 Al1 Fe1 135.16(3) 3_565 2_545 ? O5 Al1 Fe1 44.84(3) 1_545 2_545 ? Al1 Al1 Fe1 180.0 2 2_545 ? Fe1 Al1 Fe1 180.0 2 2_545 ? Al1 Al1 Fe1 0.0 2_545 2_545 ? O4 Al1 Ca1 87.91(4) . 3_665 ? O4 Al1 Ca1 92.09(4) 3 3_665 ? O1 Al1 Ca1 137.88(3) 3_565 3_665 ? O1 Al1 Ca1 42.12(3) 1_545 3_665 ? O5 Al1 Ca1 48.66(4) 3_565 3_665 ? O5 Al1 Ca1 131.34(4) 1_545 3_665 ? Al1 Al1 Ca1 65.070(3) 2 3_665 ? Fe1 Al1 Ca1 65.070(3) 2 3_665 ? Al1 Al1 Ca1 114.930(3) 2_545 3_665 ? Fe1 Al1 Ca1 114.930(3) 2_545 3_665 ? O4 Al1 Ca1 92.09(4) . 1_445 ? O4 Al1 Ca1 87.91(4) 3 1_445 ? O1 Al1 Ca1 42.12(3) 3_565 1_445 ? O1 Al1 Ca1 137.88(3) 1_545 1_445 ? O5 Al1 Ca1 131.34(4) 3_565 1_445 ? O5 Al1 Ca1 48.66(4) 1_545 1_445 ? Al1 Al1 Ca1 114.930(3) 2 1_445 ? Fe1 Al1 Ca1 114.930(3) 2 1_445 ? Al1 Al1 Ca1 65.070(3) 2_545 1_445 ? Fe1 Al1 Ca1 65.070(3) 2_545 1_445 ? Ca1 Al1 Ca1 180.0 3_665 1_445 ? O3 Al2 O3 180.0 3_656 1_455 ? O3 Al2 O10 88.26(5) 3_656 . ? O3 Al2 O10 91.74(5) 1_455 . ? O3 Al2 O10 91.74(5) 3_656 3_556 ? O3 Al2 O10 88.26(5) 1_455 3_556 ? O10 Al2 O10 180.0 . 3_556 ? O3 Al2 O6 90.43(5) 3_656 3_566 ? O3 Al2 O6 89.57(5) 1_455 3_566 ? O10 Al2 O6 82.53(4) . 3_566 ? O10 Al2 O6 97.47(4) 3_556 3_566 ? O3 Al2 O6 89.57(5) 3_656 1_545 ? O3 Al2 O6 90.43(5) 1_455 1_545 ? O10 Al2 O6 97.47(4) . 1_545 ? O10 Al2 O6 82.53(4) 3_556 1_545 ? O6 Al2 O6 180.0 3_566 1_545 ? O3 Al2 Al2 87.11(3) 3_656 2_546 ? O3 Al2 Al2 92.89(3) 1_455 2_546 ? O10 Al2 Al2 138.86(3) . 2_546 ? O10 Al2 Al2 41.14(3) 3_556 2_546 ? O6 Al2 Al2 138.33(3) 3_566 2_546 ? O6 Al2 Al2 41.67(3) 1_545 2_546 ? O3 Al2 Al2 92.89(3) 3_656 2_556 ? O3 Al2 Al2 87.11(3) 1_455 2_556 ? O10 Al2 Al2 41.14(3) . 2_556 ? O10 Al2 Al2 138.86(3) 3_556 2_556 ? O6 Al2 Al2 41.67(3) 3_566 2_556 ? O6 Al2 Al2 138.33(3) 1_545 2_556 ? Al2 Al2 Al2 180.0 2_546 2_556 ? O3 Al2 Fe2 87.11(3) 3_656 2_546 ? O3 Al2 Fe2 92.89(3) 1_455 2_546 ? O10 Al2 Fe2 138.86(3) . 2_546 ? O10 Al2 Fe2 41.14(3) 3_556 2_546 ? O6 Al2 Fe2 138.33(3) 3_566 2_546 ? O6 Al2 Fe2 41.67(3) 1_545 2_546 ? Al2 Al2 Fe2 0.0 2_546 2_546 ? Al2 Al2 Fe2 180.0 2_556 2_546 ? O3 Al2 Fe2 92.89(3) 3_656 2_556 ? O3 Al2 Fe2 87.11(3) 1_455 2_556 ? O10 Al2 Fe2 41.14(3) . 2_556 ? O10 Al2 Fe2 138.86(3) 3_556 2_556 ? O6 Al2 Fe2 41.67(3) 3_566 2_556 ? O6 Al2 Fe2 138.33(3) 1_545 2_556 ? Al2 Al2 Fe2 180.0 2_546 2_556 ? Al2 Al2 Fe2 0.0 2_556 2_556 ? Fe2 Al2 Fe2 180.0 2_546 2_556 ? O3 Al2 Ca1 143.90(3) 3_656 1_445 ? O3 Al2 Ca1 36.10(3) 1_455 1_445 ? O10 Al2 Ca1 96.33(4) . 1_445 ? O10 Al2 Ca1 83.67(4) 3_556 1_445 ? O6 Al2 Ca1 125.66(4) 3_566 1_445 ? O6 Al2 Ca1 54.34(4) 1_545 1_445 ? Al2 Al2 Ca1 66.101(3) 2_546 1_445 ? Al2 Al2 Ca1 113.899(3) 2_556 1_445 ? Fe2 Al2 Ca1 66.101(3) 2_546 1_445 ? Fe2 Al2 Ca1 113.899(3) 2_556 1_445 ? O3 Al2 Ca1 36.10(3) 3_656 3_666 ? O3 Al2 Ca1 143.90(3) 1_455 3_666 ? O10 Al2 Ca1 83.67(4) . 3_666 ? O10 Al2 Ca1 96.33(4) 3_556 3_666 ? O6 Al2 Ca1 54.34(4) 3_566 3_666 ? O6 Al2 Ca1 125.66(4) 1_545 3_666 ? Al2 Al2 Ca1 113.899(3) 2_546 3_666 ? Al2 Al2 Ca1 66.101(3) 2_556 3_666 ? Fe2 Al2 Ca1 113.899(3) 2_546 3_666 ? Fe2 Al2 Ca1 66.101(3) 2_556 3_666 ? Ca1 Al2 Ca1 180.000(9) 1_445 3_666 ? O8 Fe3 O4 167.60(6) . . ? O8 Fe3 O2 81.80(4) . 4_575 ? O4 Fe3 O2 89.82(4) . 4_575 ? O8 Fe3 O2 81.80(4) . 1_545 ? O4 Fe3 O2 89.82(4) . 1_545 ? O2 Fe3 O2 94.51(5) 4_575 1_545 ? O8 Fe3 O1 110.30(4) . 1_545 ? O4 Fe3 O1 78.76(4) . 1_545 ? O2 Fe3 O1 167.43(4) 4_575 1_545 ? O2 Fe3 O1 90.72(3) 1_545 1_545 ? O8 Fe3 O1 110.30(4) . 4_575 ? O4 Fe3 O1 78.76(4) . 4_575 ? O2 Fe3 O1 90.72(3) 4_575 4_575 ? O2 Fe3 O1 167.43(4) 1_545 4_575 ? O1 Fe3 O1 81.99(5) 1_545 4_575 ? O8 Fe3 Ce2 66.78(4) . 3_666 ? O4 Fe3 Ce2 100.82(4) . 3_666 ? O2 Fe3 Ce2 48.24(3) 4_575 3_666 ? O2 Fe3 Ce2 48.24(3) 1_545 3_666 ? O1 Fe3 Ce2 138.83(2) 1_545 3_666 ? O1 Fe3 Ce2 138.83(2) 4_575 3_666 ? O8 Fe3 Ca2 66.78(4) . 3_666 ? O4 Fe3 Ca2 100.82(4) . 3_666 ? O2 Fe3 Ca2 48.24(3) 4_575 3_666 ? O2 Fe3 Ca2 48.24(3) 1_545 3_666 ? O1 Fe3 Ca2 138.83(2) 1_545 3_666 ? O1 Fe3 Ca2 138.83(2) 4_575 3_666 ? Ce2 Fe3 Ca2 0.000(4) 3_666 3_666 ? O8 Fe3 Ca1 107.63(4) . 3_665 ? O4 Fe3 Ca1 84.77(4) . 3_665 ? O2 Fe3 Ca1 132.50(3) 4_575 3_665 ? O2 Fe3 Ca1 132.50(3) 1_545 3_665 ? O1 Fe3 Ca1 41.94(2) 1_545 3_665 ? O1 Fe3 Ca1 41.94(2) 4_575 3_665 ? Ce2 Fe3 Ca1 174.403(12) 3_666 3_665 ? Ca2 Fe3 Ca1 174.403(12) 3_666 3_665 ? O7 Si1 O1 111.10(4) . 4_575 ? O7 Si1 O1 111.10(4) . . ? O1 Si1 O1 114.22(8) 4_575 . ? O7 Si1 O9 106.01(8) . 3_665 ? O1 Si1 O9 106.95(5) 4_575 3_665 ? O1 Si1 O9 106.94(5) . 3_665 ? O7 Si1 Ca1 116.020(19) . 3_665 ? O1 Si1 Ca1 39.72(4) 4_575 3_665 ? O1 Si1 Ca1 132.17(4) . 3_665 ? O9 Si1 Ca1 67.75(2) 3_665 3_665 ? O7 Si1 Ca1 116.020(19) . 3_675 ? O1 Si1 Ca1 132.17(4) 4_575 3_675 ? O1 Si1 Ca1 39.72(4) . 3_675 ? O9 Si1 Ca1 67.75(2) 3_665 3_675 ? Ca1 Si1 Ca1 118.126(18) 3_665 3_675 ? O7 Si1 Ca1 37.39(5) . . ? O1 Si1 Ca1 122.20(4) 4_575 . ? O1 Si1 Ca1 122.20(4) . . ? O9 Si1 Ca1 68.62(6) 3_665 . ? Ca1 Si1 Ca1 100.706(12) 3_665 . ? Ca1 Si1 Ca1 100.706(12) 3_675 . ? O8 Si2 O3 109.10(5) . . ? O8 Si2 O3 109.10(5) . 4_565 ? O3 Si2 O3 112.85(7) . 4_565 ? O8 Si2 O9 110.36(8) . . ? O3 Si2 O9 107.70(5) . . ? O3 Si2 O9 107.70(5) 4_565 . ? O8 Si2 Ca1 116.657(17) . 1_545 ? O3 Si2 Ca1 39.55(4) . 1_545 ? O3 Si2 Ca1 132.28(4) 4_565 1_545 ? O9 Si2 Ca1 68.81(2) . 1_545 ? O8 Si2 Ca1 116.657(17) . . ? O3 Si2 Ca1 132.28(4) . . ? O3 Si2 Ca1 39.55(4) 4_565 . ? O9 Si2 Ca1 68.81(2) . . ? Ca1 Si2 Ca1 120.099(18) 1_545 . ? O8 Si2 Ca2 58.926(17) . 1_545 ? O3 Si2 Ca2 51.43(4) . 1_545 ? O3 Si2 Ca2 138.22(4) 4_565 1_545 ? O9 Si2 Ca2 113.97(3) . 1_545 ? Ca1 Si2 Ca2 64.697(6) 1_545 1_545 ? Ca1 Si2 Ca2 175.177(15) . 1_545 ? O2 Si3 O2 103.01(8) . 4_575 ? O2 Si3 O6 113.20(5) . . ? O2 Si3 O6 113.20(5) 4_575 . ? O2 Si3 O5 113.61(5) . . ? O2 Si3 O5 113.61(5) 4_575 . ? O6 Si3 O5 100.68(7) . . ? O2 Si3 Ce2 51.71(4) . . ? O2 Si3 Ce2 51.71(4) 4_575 . ? O6 Si3 Ce2 134.70(5) . . ? O5 Si3 Ce2 124.62(5) . . ? O2 Si3 Ca1 128.30(4) . 1_455 ? O2 Si3 Ca1 128.30(4) 4_575 1_455 ? O6 Si3 Ca1 55.97(5) . 1_455 ? O5 Si3 Ca1 44.70(5) . 1_455 ? Ce2 Si3 Ca1 169.323(17) . 1_455 ? Si1 O1 Fe1 125.13(6) . 1_565 ? Si1 O1 Al1 125.13(6) . 1_565 ? Fe1 O1 Al1 0.0 1_565 1_565 ? Si1 O1 Al3 123.21(5) . 1_565 ? Fe1 O1 Al3 88.60(4) 1_565 1_565 ? Al1 O1 Al3 88.60(4) 1_565 1_565 ? Si1 O1 Fe3 123.21(5) . 1_565 ? Fe1 O1 Fe3 88.60(4) 1_565 1_565 ? Al1 O1 Fe3 88.60(4) 1_565 1_565 ? Al3 O1 Fe3 0.000(14) 1_565 1_565 ? Si1 O1 Ca1 114.14(5) . 3_675 ? Fe1 O1 Ca1 102.97(4) 1_565 3_675 ? Al1 O1 Ca1 102.97(4) 1_565 3_675 ? Al3 O1 Ca1 96.92(4) 1_565 3_675 ? Fe3 O1 Ca1 96.92(4) 1_565 3_675 ? Si3 O2 Al3 124.90(5) . 1_565 ? Si3 O2 Fe3 124.90(5) . 1_565 ? Al3 O2 Fe3 0.000(11) 1_565 1_565 ? Si3 O2 Ca2 132.63(5) . 3_676 ? Al3 O2 Ca2 89.93(3) 1_565 3_676 ? Fe3 O2 Ca2 89.93(3) 1_565 3_676 ? Si3 O2 Ce2 132.63(5) . 3_676 ? Al3 O2 Ce2 89.93(3) 1_565 3_676 ? Fe3 O2 Ce2 89.93(3) 1_565 3_676 ? Ca2 O2 Ce2 0.000(5) 3_676 3_676 ? Si3 O2 Ce2 99.25(5) . . ? Al3 O2 Ce2 106.16(4) 1_565 . ? Fe3 O2 Ce2 106.16(4) 1_565 . ? Ca2 O2 Ce2 100.05(3) 3_676 . ? Ce2 O2 Ce2 100.05(3) 3_676 . ? Si2 O3 Fe2 124.54(6) . 1_655 ? Si2 O3 Al2 124.54(6) . 1_655 ? Fe2 O3 Al2 0.0 1_655 1_655 ? Si2 O3 Ca1 114.14(5) . 1_545 ? Fe2 O3 Ca1 115.43(5) 1_655 1_545 ? Al2 O3 Ca1 115.43(5) 1_655 1_545 ? Si2 O3 Ca2 101.76(5) . 1_545 ? Fe2 O3 Ca2 100.93(4) 1_655 1_545 ? Al2 O3 Ca2 100.93(4) 1_655 1_545 ? Ca1 O3 Ca2 90.71(3) 1_545 1_545 ? Si2 O3 Ce2 101.76(5) . 1_545 ? Fe2 O3 Ce2 100.93(4) 1_655 1_545 ? Al2 O3 Ce2 100.93(4) 1_655 1_545 ? Ca1 O3 Ce2 90.71(3) 1_545 1_545 ? Ca2 O3 Ce2 0.000(3) 1_545 1_545 ? Al1 O4 Fe1 98.25(6) . 2 ? Al1 O4 Al1 98.25(6) . 2 ? Fe1 O4 Al1 0.0 2 2 ? Al1 O4 Fe3 102.71(5) . . ? Fe1 O4 Fe3 102.71(5) 2 . ? Al1 O4 Fe3 102.71(5) 2 . ? Si3 O5 Fe1 129.41(4) . 2 ? Si3 O5 Al1 129.41(4) . 2 ? Fe1 O5 Al1 0.0 2 2 ? Si3 O5 Fe1 129.41(4) . 1_565 ? Fe1 O5 Fe1 90.32(5) 2 1_565 ? Al1 O5 Fe1 90.32(5) 2 1_565 ? Si3 O5 Al1 129.41(4) . 1_565 ? Fe1 O5 Al1 90.32(5) 2 1_565 ? Al1 O5 Al1 90.32(5) 2 1_565 ? Fe1 O5 Al1 0.0 1_565 1_565 ? Si3 O5 Ca1 108.66(6) . 1_455 ? Fe1 O5 Ca1 95.03(4) 2 1_455 ? Al1 O5 Ca1 95.03(4) 2 1_455 ? Fe1 O5 Ca1 95.03(4) 1_565 1_455 ? Al1 O5 Ca1 95.03(4) 1_565 1_455 ? Si3 O6 Fe2 130.82(3) . 1_565 ? Si3 O6 Al2 130.82(3) . 1_565 ? Fe2 O6 Al2 0.0 1_565 1_565 ? Si3 O6 Fe2 130.82(3) . 2_556 ? Fe2 O6 Fe2 96.65(6) 1_565 2_556 ? Al2 O6 Fe2 96.65(6) 1_565 2_556 ? Si3 O6 Al2 130.82(3) . 2_556 ? Fe2 O6 Al2 96.65(6) 1_565 2_556 ? Al2 O6 Al2 96.65(6) 1_565 2_556 ? Fe2 O6 Al2 0.0 2_556 2_556 ? Si3 O6 Ca1 96.23(6) . 1_455 ? Fe2 O6 Ca1 92.86(5) 1_565 1_455 ? Al2 O6 Ca1 92.86(5) 1_565 1_455 ? Fe2 O6 Ca1 92.86(5) 2_556 1_455 ? Al2 O6 Ca1 92.86(5) 2_556 1_455 ? Si1 O7 Ce2 137.58(8) . . ? Si1 O7 Ca1 118.38(7) . . ? Ce2 O7 Ca1 104.04(5) . . ? Si2 O8 Fe3 127.77(8) . . ? Si2 O8 Ca2 94.35(3) . 1_545 ? Fe3 O8 Ca2 100.14(3) . 1_545 ? Si2 O9 Si1 142.59(10) . 3_665 ? Al2 O10 Fe2 97.71(6) . 2_556 ? Al2 O10 Al2 97.71(6) . 2_556 ? Fe2 O10 Al2 0.0 2_556 2_556 ? Al2 O10 Ce2 108.72(5) . 3_666 ? Fe2 O10 Ce2 108.72(5) 2_556 3_666 ? Al2 O10 Ce2 108.72(5) 2_556 3_666 ? Al2 O10 Ca2 108.72(5) . 3_666 ? Fe2 O10 Ca2 108.72(5) 2_556 3_666 ? Al2 O10 Ca2 108.72(5) 2_556 3_666 ? Ce2 O10 Ca2 0.000(3) 3_666 3_666 ? Al2 O10 H10 118.3(13) . . ? Fe2 O10 H10 118.3(13) 2_556 . ? Al2 O10 H10 118.3(13) 2_556 . ? Ce2 O10 H10 105(2) 3_666 . ? Ca2 O10 H10 105(2) 3_666 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 36.38 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.995 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.132