data_shelx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H18 Al0.76 Fe1.49 Mg0.13 Mn0.55 O18 P1.85 Zn0.07' _chemical_formula_weight 505.11 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Zn' 'Zn' 0.2839 1.4301 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.3740(11) _cell_length_b 10.717(3) _cell_length_c 7.2000(14) _cell_angle_alpha 107.60(3) _cell_angle_beta 111.52(3) _cell_angle_gamma 71.651(18) _cell_volume 357.85(15) _cell_formula_units_Z 1 _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 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 256 _exptl_absorpt_coefficient_mu 2.465 _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 0.71000 _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 4461 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 26.34 _reflns_number_total 1331 _reflns_number_gt 1294 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0240P)^2^+0.6700P] 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 0.151(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1331 _refine_ls_number_parameters 155 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.297 _refine_ls_shift/su_mean 0.038 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 1.0000 0.0127(3) Uani 0.854(10) 2 d SP . . Mg1 Mg 0.0000 0.0000 1.0000 0.0127(3) Uani 0.146(10) 2 d SP . . Fe2 Fe 0.0000 0.5000 0.0000 0.0098(3) Uani 0.700(10) 2 d SP . . Al2 Al 0.0000 0.5000 0.0000 0.0098(3) Uani 0.300(10) 2 d SP . . Fe3 Fe 0.0000 0.5000 0.5000 0.0092(3) Uani 0.538(9) 2 d SP . . Al3 Al 0.0000 0.5000 0.5000 0.0092(3) Uani 0.462(9) 2 d SP . . P1 P 0.34520(15) 0.66917(7) 0.92610(12) 0.0113(3) Uani 0.961(6) 1 d P . . O1 O 0.1660(4) 0.6539(2) 0.0417(4) 0.0155(5) Uani 1 1 d . . . O2 O 0.3010(4) 0.5749(2) 0.7112(3) 0.0163(5) Uani 1 1 d . . . O3 O 0.2702(4) 0.8168(2) 0.9039(4) 0.0160(5) Uani 1 1 d . . . O4 O 0.3448(4) 0.3678(2) 0.9510(3) 0.0154(5) Uani 1 1 d . . . O5 O 0.1530(4) 0.5047(2) 0.2969(3) 0.0159(5) Uani 1 1 d D . . O6 O 0.2346(4) 0.3109(2) 0.5435(4) 0.0178(5) Uani 1 1 d D . . O7 O 0.2404(5) 0.0064(2) 0.3215(4) 0.0245(6) Uani 1 1 d D . . O8 O 0.2284(5) 0.1107(2) 0.9465(4) 0.0235(6) Uani 1 1 d D . . O9 O 0.2684(5) 0.8014(2) 0.5087(4) 0.0215(6) Uani 1 1 d D . . H1 H 0.334(4) 0.493(4) 0.323(7) 0.026(11) Uiso 1 1 d D . . H2 H 0.290(8) 0.317(5) 0.680(3) 0.032(12) Uiso 1 1 d D . . H3 H 0.396(6) 0.275(5) 0.512(6) 0.036(12) Uiso 1 1 d D . . H4 H 0.239(12) 0.083(3) 0.423(6) 0.049(15) Uiso 1 1 d D . . H5 H 0.218(14) -0.055(4) 0.374(8) 0.072(19) Uiso 1 1 d D . . H6 H 0.121(8) 0.193(3) 0.974(9) 0.055(16) Uiso 1 1 d D . . H7 H 0.398(5) 0.119(5) 0.974(8) 0.040(13) Uiso 1 1 d D . . H8 H 0.252(13) 0.810(6) 0.633(4) 0.061(18) Uiso 1 1 d D . . H9 H 0.180(10) 0.740(4) 0.422(6) 0.048(15) Uiso 1 1 d 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 0.0101(4) 0.0090(4) 0.0182(5) 0.0014(3) 0.0045(3) -0.0020(2) Mg1 0.0101(4) 0.0090(4) 0.0182(5) 0.0014(3) 0.0045(3) -0.0020(2) Fe2 0.0078(4) 0.0091(4) 0.0126(4) 0.0011(3) 0.0033(3) -0.0030(2) Al2 0.0078(4) 0.0091(4) 0.0126(4) 0.0011(3) 0.0033(3) -0.0030(2) Fe3 0.0071(4) 0.0095(4) 0.0110(5) 0.0013(3) 0.0024(3) -0.0034(3) Al3 0.0071(4) 0.0095(4) 0.0110(5) 0.0013(3) 0.0024(3) -0.0034(3) P1 0.0096(4) 0.0091(4) 0.0146(5) 0.0015(3) 0.0035(3) -0.0025(3) O1 0.0128(10) 0.0138(10) 0.0194(12) 0.0023(9) 0.0045(8) -0.0039(8) O2 0.0152(10) 0.0155(10) 0.0186(12) 0.0027(9) 0.0049(9) -0.0052(8) O3 0.0136(10) 0.0119(10) 0.0212(12) 0.0026(9) 0.0054(9) -0.0020(8) O4 0.0128(10) 0.0156(10) 0.0176(12) 0.0037(9) 0.0033(9) -0.0044(8) O5 0.0132(10) 0.0161(10) 0.0172(12) 0.0023(9) 0.0048(8) -0.0027(8) O6 0.0145(10) 0.0193(11) 0.0180(12) 0.0009(9) 0.0058(9) -0.0034(8) O7 0.0219(12) 0.0212(12) 0.0269(14) 0.0042(10) 0.0040(10) -0.0050(9) O8 0.0150(11) 0.0155(11) 0.0413(16) 0.0059(10) 0.0111(10) -0.0021(9) O9 0.0192(11) 0.0218(12) 0.0242(14) 0.0038(10) 0.0079(10) -0.0049(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 O3 2.136(2) 2_567 ? Mn1 O3 2.136(2) 1_545 ? Mn1 O8 2.145(2) 2_557 ? Mn1 O8 2.145(2) . ? Mn1 O7 2.190(3) 2_556 ? Mn1 O7 2.190(3) 1_556 ? Fe2 O5 1.980(2) . ? Fe2 O5 1.980(2) 2_565 ? Fe2 O1 2.009(2) . ? Fe2 O1 2.009(2) 2_565 ? Fe2 O4 2.022(2) 1_554 ? Fe2 O4 2.022(2) 2_566 ? Fe3 O5 1.942(2) 2_566 ? Fe3 O5 1.942(2) . ? Fe3 O2 1.962(2) 2_566 ? Fe3 O2 1.962(2) . ? Fe3 O6 2.069(2) 2_566 ? Fe3 O6 2.069(2) . ? P1 O3 1.547(2) . ? P1 O2 1.551(2) . ? P1 O1 1.555(2) 1_556 ? P1 O4 1.559(2) 2_667 ? O1 P1 1.555(2) 1_554 ? O3 Mg1 2.136(2) 1_565 ? O3 Mn1 2.136(2) 1_565 ? O4 P1 1.559(2) 2_667 ? O4 Fe2 2.022(2) 1_556 ? O4 Al2 2.022(2) 1_556 ? O5 H1 0.892(19) . ? O6 H2 0.903(19) . ? O6 H3 0.911(19) . ? O7 Mg1 2.190(3) 1_554 ? O7 Mn1 2.190(3) 1_554 ? O7 H4 0.916(19) . ? O7 H5 0.91(2) . ? O8 H6 0.897(19) . ? O8 H7 0.888(19) . ? O9 H8 0.90(2) . ? O9 H9 0.886(19) . ? 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 Mn1 O3 180.000(1) 2_567 1_545 ? O3 Mn1 O8 89.50(9) 2_567 2_557 ? O3 Mn1 O8 90.50(9) 1_545 2_557 ? O3 Mn1 O8 90.50(9) 2_567 . ? O3 Mn1 O8 89.50(9) 1_545 . ? O8 Mn1 O8 180.0 2_557 . ? O3 Mn1 O7 91.76(10) 2_567 2_556 ? O3 Mn1 O7 88.24(10) 1_545 2_556 ? O8 Mn1 O7 94.85(10) 2_557 2_556 ? O8 Mn1 O7 85.15(10) . 2_556 ? O3 Mn1 O7 88.24(10) 2_567 1_556 ? O3 Mn1 O7 91.76(10) 1_545 1_556 ? O8 Mn1 O7 85.15(10) 2_557 1_556 ? O8 Mn1 O7 94.85(10) . 1_556 ? O7 Mn1 O7 180.000(1) 2_556 1_556 ? O5 Fe2 O5 180.00(13) . 2_565 ? O5 Fe2 O1 89.46(10) . . ? O5 Fe2 O1 90.54(10) 2_565 . ? O5 Fe2 O1 90.54(10) . 2_565 ? O5 Fe2 O1 89.46(10) 2_565 2_565 ? O1 Fe2 O1 180.00(14) . 2_565 ? O5 Fe2 O4 90.92(10) . 1_554 ? O5 Fe2 O4 89.08(10) 2_565 1_554 ? O1 Fe2 O4 90.12(9) . 1_554 ? O1 Fe2 O4 89.88(9) 2_565 1_554 ? O5 Fe2 O4 89.08(10) . 2_566 ? O5 Fe2 O4 90.92(10) 2_565 2_566 ? O1 Fe2 O4 89.88(9) . 2_566 ? O1 Fe2 O4 90.12(9) 2_565 2_566 ? O4 Fe2 O4 180.00(13) 1_554 2_566 ? O5 Fe3 O5 180.000(1) 2_566 . ? O5 Fe3 O2 88.19(9) 2_566 2_566 ? O5 Fe3 O2 91.81(9) . 2_566 ? O5 Fe3 O2 91.81(9) 2_566 . ? O5 Fe3 O2 88.19(9) . . ? O2 Fe3 O2 180.0 2_566 . ? O5 Fe3 O6 94.94(10) 2_566 2_566 ? O5 Fe3 O6 85.06(10) . 2_566 ? O2 Fe3 O6 87.99(9) 2_566 2_566 ? O2 Fe3 O6 92.01(9) . 2_566 ? O5 Fe3 O6 85.06(10) 2_566 . ? O5 Fe3 O6 94.94(10) . . ? O2 Fe3 O6 92.01(9) 2_566 . ? O2 Fe3 O6 87.99(9) . . ? O6 Fe3 O6 180.0 2_566 . ? O3 P1 O2 109.39(13) . . ? O3 P1 O1 109.49(12) . 1_556 ? O2 P1 O1 111.16(12) . 1_556 ? O3 P1 O4 108.73(13) . 2_667 ? O2 P1 O4 108.23(12) . 2_667 ? O1 P1 O4 109.80(13) 1_556 2_667 ? P1 O1 Fe2 129.63(13) 1_554 . ? P1 O2 Fe3 137.17(13) . . ? P1 O3 Mg1 136.29(13) . 1_565 ? P1 O3 Mn1 136.29(13) . 1_565 ? Mg1 O3 Mn1 0.0 1_565 1_565 ? P1 O4 Fe2 137.21(13) 2_667 1_556 ? P1 O4 Al2 137.21(13) 2_667 1_556 ? Fe2 O4 Al2 0.0 1_556 1_556 ? Fe3 O5 Fe2 133.28(12) . . ? Fe3 O5 H1 121(3) . . ? Fe2 O5 H1 104(3) . . ? Fe3 O6 H2 105(3) . . ? Fe3 O6 H3 122(3) . . ? H2 O6 H3 103(3) . . ? Mg1 O7 Mn1 0.0 1_554 1_554 ? Mg1 O7 H4 124(3) 1_554 . ? Mn1 O7 H4 124(3) 1_554 . ? Mg1 O7 H5 113(4) 1_554 . ? Mn1 O7 H5 113(4) 1_554 . ? H4 O7 H5 104(3) . . ? Mn1 O8 H6 97(3) . . ? Mn1 O8 H7 142(3) . . ? H6 O8 H7 108(3) . . ? H8 O9 H9 107(3) . . ? 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 H1 O2 0.892(19) 1.95(2) 2.804(3) 160(4) 2_666 O6 H2 O4 0.903(19) 1.80(2) 2.684(3) 167(4) . O6 H3 O9 0.911(19) 1.77(2) 2.676(3) 171(4) 2_666 O7 H4 O6 0.916(19) 2.33(3) 3.166(4) 151(4) . O7 H5 O9 0.91(2) 1.95(3) 2.846(4) 166(6) 1_545 O8 H6 O1 0.897(19) 1.87(2) 2.739(3) 164(5) 2_566 O8 H7 O3 0.888(19) 1.92(2) 2.776(3) 162(4) 2_667 O9 H8 O3 0.90(2) 1.90(2) 2.797(4) 172(6) . O9 H9 O5 0.886(19) 2.44(3) 3.231(3) 149(4) . _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.486 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.133