data_angarf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H40 Fe15 Mg5 Na2 O96 P16' _chemical_formula_weight 3077.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' 'Mg' 'Mg' 0.0486 0.0363 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, y, -z+1/2' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 12.7997(3) _cell_length_b 17.9081(4) _cell_length_c 8.2112(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1882.16(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 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.353 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4134 _exptl_absorpt_correction_T_max 0.8503 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _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 10527 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2164 _reflns_number_gt 2074 _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^)+(0.0479P)^2^+5.9182P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 2164 _refine_ls_number_parameters 175 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Fe1 Fe 0.11879(4) 0.0000 0.0000 0.0090(2) Uani 0.961(8) 2 d SP . . Mg1 Mg 0.11879(4) 0.0000 0.0000 0.0090(2) Uani 0.039(8) 2 d SP . . Fe2 Fe 0.13261(6) 0.74543(3) 0.81131(8) 0.0108(3) Uani 0.656(7) 1 d P . . Mg2 Mg 0.13261(6) 0.74543(3) 0.81131(8) 0.0108(3) Uani 0.344(7) 1 d P . . Fe3 Fe 0.12964(5) 0.75536(3) 0.20026(7) 0.0124(2) Uani 0.762(7) 1 d P . . Mg3 Mg 0.12964(5) 0.75536(3) 0.20026(7) 0.0124(2) Uani 0.238(7) 1 d P . . P1 P 0.96324(6) 0.84964(4) 0.98805(13) 0.0103(2) Uani 1 1 d . . . P2 P 0.29583(6) 0.14343(4) 0.00075(14) 0.01082(19) Uani 1 1 d . . . Na Na 0.4776(10) 0.0000 0.0000 0.089(5) Uani 0.365(14) 2 d SP . . O1 O 0.8939(2) 0.82487(14) 0.8488(3) 0.0175(6) Uani 1 1 d . . . O2 O 0.9975(2) 0.93072(13) 0.9619(3) 0.0148(5) Uani 1 1 d . . . O3 O 0.9034(2) 0.84281(15) 0.1503(3) 0.0175(6) Uani 1 1 d . . . O4 O 0.06196(16) 0.79926(12) 0.9985(4) 0.0133(4) Uani 1 1 d . . . O5 O 0.22146(19) 0.07858(14) 0.0180(4) 0.0190(5) Uani 1 1 d . . . O6 O 0.40855(18) 0.11783(15) 0.9994(4) 0.0242(5) Uani 1 1 d . . . O7 O 0.2777(2) 0.19970(15) 0.1426(3) 0.0141(6) Uani 1 1 d . . . O8 O 0.2712(2) 0.18688(15) 0.8404(3) 0.0148(6) Uani 1 1 d . . . OH1 O 0.0000 0.6997(2) 0.2500 0.0168(8) Uani 1 2 d SD . . H1 H -0.007(9) 0.658(3) 0.186(9) 0.020 Uiso 0.50 1 d PD . . OH2 O 0.0000 0.6900(2) 0.7500 0.0201(9) Uani 1 2 d SD . . H2 H -0.036(7) 0.676(5) 0.840(8) 0.024 Uiso 0.50 1 d PD . . OH3 O 0.1702(2) 0.68182(14) 0.0128(4) 0.0225(6) Uani 1 1 d D . . H3 H 0.237(2) 0.669(2) 0.002(8) 0.027 Uiso 1 1 d D . . OW1 O 0.1272(2) 0.98473(13) 0.2488(3) 0.0180(5) Uani 1 1 d D . . HW1A H 0.102(3) 1.0160(17) 0.315(5) 0.022 Uiso 1 1 d D . . HW1B H 0.112(4) 0.9381(14) 0.268(6) 0.022 Uiso 1 1 d D . . OW2A O 0.6548(13) 0.0335(8) 0.136(2) 0.092(7) Uiso 0.50(3) 1 d P . . OW2B O 0.604(2) 0.0076(14) 0.214(3) 0.177(11) Uiso 0.50(3) 1 d P . . 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 Fe1 0.0089(3) 0.0080(3) 0.0100(3) 0.0002(2) 0.000 0.000 Mg1 0.0089(3) 0.0080(3) 0.0100(3) 0.0002(2) 0.000 0.000 Fe2 0.0114(4) 0.0122(4) 0.0089(4) 0.00018(19) 0.0011(2) 0.0035(3) Mg2 0.0114(4) 0.0122(4) 0.0089(4) 0.00018(19) 0.0011(2) 0.0035(3) Fe3 0.0107(4) 0.0161(4) 0.0105(3) 0.00245(19) -0.0004(2) 0.0024(3) Mg3 0.0107(4) 0.0161(4) 0.0105(3) 0.00245(19) -0.0004(2) 0.0024(3) P1 0.0097(3) 0.0092(3) 0.0119(4) -0.0011(3) 0.0006(4) -0.0012(3) P2 0.0109(3) 0.0108(4) 0.0109(4) -0.0003(4) 0.0003(4) -0.0016(3) Na 0.114(10) 0.017(4) 0.135(11) 0.012(6) 0.000 0.000 O1 0.0162(14) 0.0172(12) 0.0189(12) -0.0035(9) -0.0053(12) 0.0008(10) O2 0.0132(10) 0.0091(10) 0.0220(14) 0.0001(9) -0.0010(9) -0.0014(9) O3 0.0170(14) 0.0188(12) 0.0169(12) -0.0016(10) 0.0041(11) 0.0004(11) O4 0.0125(9) 0.0139(10) 0.0136(10) 0.0006(11) -0.0001(12) 0.0034(8) O5 0.0213(11) 0.0139(11) 0.0217(13) 0.0008(12) 0.0026(12) -0.0061(9) O6 0.0155(11) 0.0289(13) 0.0281(13) 0.0000(14) -0.0005(17) 0.0048(10) O7 0.0153(14) 0.0145(12) 0.0124(12) -0.0016(10) -0.0010(10) -0.0025(10) O8 0.0166(14) 0.0156(12) 0.0121(12) 0.0014(10) 0.0022(10) -0.0010(11) OH1 0.016(2) 0.0150(18) 0.0196(19) 0.000 0.0041(16) 0.000 OH2 0.018(2) 0.0205(19) 0.021(2) 0.000 -0.0011(17) 0.000 OH3 0.0290(13) 0.0198(12) 0.0187(13) -0.0025(12) 0.0012(14) -0.0009(10) OW1 0.0238(12) 0.0158(12) 0.0144(12) 0.0032(10) 0.0040(10) 0.0018(11) _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 Fe1 O5 1.931(2) . ? Fe1 O5 1.931(2) 2 ? Fe1 O2 2.012(2) 1_444 ? Fe1 O2 2.012(2) 2_466 ? Fe1 OW1 2.064(3) 1_545 ? Fe1 OW1 2.064(3) 2_565 ? Fe2 O1 1.966(3) 3_656 ? Fe2 O4 2.027(3) . ? Fe2 OH2 2.030(2) . ? Fe2 O8 2.042(3) 7_556 ? Fe2 OH3 2.065(3) 1_556 ? Fe2 O7 2.135(3) 2_566 ? Fe2 Mg3 3.1768(7) 8_565 ? Fe2 Mg3 3.1989(8) 1_556 ? Fe3 OH1 1.978(2) . ? Fe3 O7 2.016(3) 7 ? Fe3 O4 2.028(3) 1_554 ? Fe3 O3 2.034(3) 3_655 ? Fe3 OH3 2.091(3) . ? Fe3 O8 2.113(3) 2_566 ? Fe3 Mg2 3.1768(7) 8_564 ? Fe3 Mg2 3.1989(8) 1_554 ? P1 O1 1.514(3) . ? P1 O2 1.532(2) . ? P1 O3 1.541(3) 1_556 ? P1 O4 1.555(2) 1_655 ? P2 O5 1.508(2) . ? P2 O6 1.514(2) 1_554 ? P2 O7 1.558(3) . ? P2 O8 1.561(3) 1_554 ? Na O6 2.287(6) 2_556 ? Na O6 2.287(6) 1_554 ? Na OW2B 2.39(2) . ? Na OW2B 2.39(2) 2 ? Na OW2B 2.57(3) 4_654 ? Na OW2B 2.57(3) 3_655 ? Na OW2A 2.598(19) 2 ? Na OW2A 2.598(19) . ? Na Na 4.146(4) 3_655 ? Na Na 4.146(4) 3_654 ? O1 Mg2 1.966(3) 3_656 ? O1 Fe2 1.966(3) 3_656 ? O2 Mg1 2.012(2) 1_666 ? O2 Fe1 2.012(2) 1_666 ? O3 P1 1.541(3) 1_554 ? O3 Fe3 2.034(3) 3_655 ? O3 Mg3 2.034(3) 3_655 ? O4 P1 1.555(2) 1_455 ? O4 Fe3 2.028(3) 1_556 ? O4 Mg3 2.028(3) 1_556 ? O6 P2 1.514(2) 1_556 ? O6 Na 2.288(6) 1_556 ? O7 Mg3 2.016(3) 7_545 ? O7 Fe3 2.016(3) 7_545 ? O7 Fe2 2.135(3) 2_566 ? O7 Mg2 2.135(3) 2_566 ? O8 P2 1.561(3) 1_556 ? O8 Fe2 2.042(3) 7_546 ? O8 Mg2 2.042(3) 7_546 ? O8 Fe3 2.113(3) 2_566 ? O8 Mg3 2.113(3) 2_566 ? OH1 Mg3 1.978(2) 3 ? OH1 Fe3 1.978(2) 3 ? OH1 H1 0.91(3) . ? OH2 Mg2 2.030(2) 3_556 ? OH2 Fe2 2.030(2) 3_556 ? OH2 H2 0.91(3) . ? OH3 Mg2 2.065(3) 1_554 ? OH3 Fe2 2.065(3) 1_554 ? OH3 H3 0.89(3) . ? OW1 Mg1 2.064(3) 1_565 ? OW1 Fe1 2.064(3) 1_565 ? OW1 HW1A 0.85(2) . ? OW1 HW1B 0.87(2) . ? OW2A OW2B 1.03(3) . ? OW2B Na 2.57(3) 3_655 ? 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 Fe1 O5 94.23(15) . 2 ? O5 Fe1 O2 170.56(11) . 1_444 ? O5 Fe1 O2 93.66(10) 2 1_444 ? O5 Fe1 O2 93.66(10) . 2_466 ? O5 Fe1 O2 170.56(11) 2 2_466 ? O2 Fe1 O2 78.99(14) 1_444 2_466 ? O5 Fe1 OW1 89.16(12) . 1_545 ? O5 Fe1 OW1 86.77(12) 2 1_545 ? O2 Fe1 OW1 96.46(10) 1_444 1_545 ? O2 Fe1 OW1 88.17(10) 2_466 1_545 ? O5 Fe1 OW1 86.77(12) . 2_565 ? O5 Fe1 OW1 89.16(12) 2 2_565 ? O2 Fe1 OW1 88.17(10) 1_444 2_565 ? O2 Fe1 OW1 96.46(10) 2_466 2_565 ? OW1 Fe1 OW1 174.01(15) 1_545 2_565 ? O1 Fe2 O4 94.93(12) 3_656 . ? O1 Fe2 OH2 92.52(12) 3_656 . ? O4 Fe2 OH2 92.73(8) . . ? O1 Fe2 O8 93.87(12) 3_656 7_556 ? O4 Fe2 O8 167.43(12) . 7_556 ? OH2 Fe2 O8 95.84(11) . 7_556 ? O1 Fe2 OH3 167.07(12) 3_656 1_556 ? O4 Fe2 OH3 76.05(12) . 1_556 ? OH2 Fe2 OH3 97.09(11) . 1_556 ? O8 Fe2 OH3 93.74(12) 7_556 1_556 ? O1 Fe2 O7 86.30(11) 3_656 2_566 ? O4 Fe2 O7 91.99(9) . 2_566 ? OH2 Fe2 O7 175.22(9) . 2_566 ? O8 Fe2 O7 79.63(11) 7_556 2_566 ? OH3 Fe2 O7 84.80(11) 1_556 2_566 ? O1 Fe2 Mg3 88.65(10) 3_656 8_565 ? O4 Fe2 Mg3 130.32(7) . 8_565 ? OH2 Fe2 Mg3 136.69(6) . 8_565 ? O8 Fe2 Mg3 40.96(8) 7_556 8_565 ? OH3 Fe2 Mg3 90.26(8) 1_556 8_565 ? O7 Fe2 Mg3 38.71(7) 2_566 8_565 ? O1 Fe2 Mg3 128.70(8) 3_656 1_556 ? O4 Fe2 Mg3 37.94(8) . 1_556 ? OH2 Fe2 Mg3 105.36(3) . 1_556 ? O8 Fe2 Mg3 130.17(9) 7_556 1_556 ? OH3 Fe2 Mg3 39.98(8) 1_556 1_556 ? O7 Fe2 Mg3 78.91(7) 2_566 1_556 ? Mg3 Fe2 Mg3 107.35(3) 8_565 1_556 ? OH1 Fe3 O7 96.44(10) . 7 ? OH1 Fe3 O4 90.33(8) . 1_554 ? O7 Fe3 O4 164.94(11) 7 1_554 ? OH1 Fe3 O3 95.10(12) . 3_655 ? O7 Fe3 O3 96.71(11) 7 3_655 ? O4 Fe3 O3 96.06(11) 1_554 3_655 ? OH1 Fe3 OH3 92.44(11) . . ? O7 Fe3 OH3 90.80(12) 7 . ? O4 Fe3 OH3 75.44(12) 1_554 . ? O3 Fe3 OH3 168.69(12) 3_655 . ? OH1 Fe3 O8 176.92(8) . 2_566 ? O7 Fe3 O8 80.72(11) 7 2_566 ? O4 Fe3 O8 92.71(10) 1_554 2_566 ? O3 Fe3 O8 84.09(11) 3_655 2_566 ? OH3 Fe3 O8 88.81(11) . 2_566 ? OH1 Fe3 Mg2 137.89(7) . 8_564 ? O7 Fe3 Mg2 41.46(8) 7 8_564 ? O4 Fe3 Mg2 130.19(7) 1_554 8_564 ? O3 Fe3 Mg2 91.69(9) 3_655 8_564 ? OH3 Fe3 Mg2 88.34(8) . 8_564 ? O8 Fe3 Mg2 39.30(7) 2_566 8_564 ? OH1 Fe3 Mg2 100.84(3) . 1_554 ? O7 Fe3 Mg2 127.19(8) 7 1_554 ? O4 Fe3 Mg2 37.91(7) 1_554 1_554 ? O3 Fe3 Mg2 130.36(8) 3_655 1_554 ? OH3 Fe3 Mg2 39.38(9) . 1_554 ? O8 Fe3 Mg2 81.90(8) 2_566 1_554 ? Mg2 Fe3 Mg2 105.96(2) 8_564 1_554 ? O1 P1 O2 109.86(15) . . ? O1 P1 O3 109.76(15) . 1_556 ? O2 P1 O3 109.80(15) . 1_556 ? O1 P1 O4 110.37(16) . 1_655 ? O2 P1 O4 108.96(13) . 1_655 ? O3 P1 O4 108.06(17) 1_556 1_655 ? O5 P2 O6 111.65(15) . 1_554 ? O5 P2 O7 109.51(16) . . ? O6 P2 O7 110.07(17) 1_554 . ? O5 P2 O8 109.61(17) . 1_554 ? O6 P2 O8 109.72(18) 1_554 1_554 ? O7 P2 O8 106.13(13) . 1_554 ? O6 Na O6 134.6(6) 2_556 1_554 ? O6 Na OW2B 108.2(7) 2_556 . ? O6 Na OW2B 102.1(6) 1_554 . ? O6 Na OW2B 102.1(6) 2_556 2 ? O6 Na OW2B 108.2(7) 1_554 2 ? OW2B Na OW2B 95.0(16) . 2 ? O6 Na OW2B 78.3(6) 2_556 4_654 ? O6 Na OW2B 83.7(6) 1_554 4_654 ? OW2B Na OW2B 161.3(8) . 4_654 ? OW2B Na OW2B 66.4(11) 2 4_654 ? O6 Na OW2B 83.7(6) 2_556 3_655 ? O6 Na OW2B 78.3(6) 1_554 3_655 ? OW2B Na OW2B 66.4(11) . 3_655 ? OW2B Na OW2B 161.3(8) 2 3_655 ? OW2B Na OW2B 132.4(12) 4_654 3_655 ? O6 Na OW2A 97.2(3) 2_556 2 ? O6 Na OW2A 123.3(4) 1_554 2 ? OW2B Na OW2A 74.8(10) . 2 ? OW2B Na OW2A 23.3(7) 2 2 ? OW2B Na OW2A 87.1(7) 4_654 2 ? OW2B Na OW2A 139.2(6) 3_655 2 ? O6 Na OW2A 123.3(4) 2_556 . ? O6 Na OW2A 97.2(3) 1_554 . ? OW2B Na OW2A 23.3(7) . . ? OW2B Na OW2A 74.8(10) 2 . ? OW2B Na OW2A 139.2(6) 4_654 . ? OW2B Na OW2A 87.1(7) 3_655 . ? OW2A Na OW2A 58.3(8) 2 . ? O6 Na Na 92.95(13) 2_556 3_655 ? O6 Na Na 93.18(13) 1_554 3_655 ? OW2B Na Na 34.8(8) . 3_655 ? OW2B Na Na 129.3(10) 2 3_655 ? OW2B Na Na 163.8(8) 4_654 3_655 ? OW2B Na Na 32.0(5) 3_655 3_655 ? OW2A Na Na 107.7(6) 2 3_655 ? OW2A Na Na 56.9(5) . 3_655 ? O6 Na Na 93.18(13) 2_556 3_654 ? O6 Na Na 92.95(13) 1_554 3_654 ? OW2B Na Na 129.4(10) . 3_654 ? OW2B Na Na 34.8(8) 2 3_654 ? OW2B Na Na 32.0(5) 4_654 3_654 ? OW2B Na Na 163.8(8) 3_655 3_654 ? OW2A Na Na 56.9(5) 2 3_654 ? OW2A Na Na 107.7(6) . 3_654 ? Na Na Na 164.1(7) 3_655 3_654 ? P1 O1 Mg2 144.87(18) . 3_656 ? P1 O1 Fe2 144.87(18) . 3_656 ? Mg2 O1 Fe2 0.00(5) 3_656 3_656 ? P1 O2 Mg1 141.60(16) . 1_666 ? P1 O2 Fe1 141.60(16) . 1_666 ? Mg1 O2 Fe1 0.0 1_666 1_666 ? P1 O3 Fe3 133.31(17) 1_554 3_655 ? P1 O3 Mg3 133.31(17) 1_554 3_655 ? Fe3 O3 Mg3 0.00(4) 3_655 3_655 ? P1 O4 Fe2 126.64(18) 1_455 . ? P1 O4 Fe3 128.09(18) 1_455 1_556 ? Fe2 O4 Fe3 104.15(9) . 1_556 ? P1 O4 Mg3 128.09(18) 1_455 1_556 ? Fe2 O4 Mg3 104.15(9) . 1_556 ? Fe3 O4 Mg3 0.00(3) 1_556 1_556 ? P2 O5 Fe1 169.5(2) . . ? P2 O6 Na 130.3(3) 1_556 1_556 ? P2 O7 Mg3 135.30(17) . 7_545 ? P2 O7 Fe3 135.30(17) . 7_545 ? Mg3 O7 Fe3 0.00(4) 7_545 7_545 ? P2 O7 Fe2 124.06(15) . 2_566 ? Mg3 O7 Fe2 99.83(11) 7_545 2_566 ? Fe3 O7 Fe2 99.83(11) 7_545 2_566 ? P2 O7 Mg2 124.06(15) . 2_566 ? Mg3 O7 Mg2 99.83(11) 7_545 2_566 ? Fe3 O7 Mg2 99.83(11) 7_545 2_566 ? Fe2 O7 Mg2 0.00(2) 2_566 2_566 ? P2 O8 Fe2 130.45(18) 1_556 7_546 ? P2 O8 Mg2 130.45(18) 1_556 7_546 ? Fe2 O8 Mg2 0.00(4) 7_546 7_546 ? P2 O8 Fe3 123.40(16) 1_556 2_566 ? Fe2 O8 Fe3 99.74(12) 7_546 2_566 ? Mg2 O8 Fe3 99.74(12) 7_546 2_566 ? P2 O8 Mg3 123.40(16) 1_556 2_566 ? Fe2 O8 Mg3 99.74(12) 7_546 2_566 ? Mg2 O8 Mg3 99.74(12) 7_546 2_566 ? Fe3 O8 Mg3 0.000(19) 2_566 2_566 ? Mg3 OH1 Fe3 0.00(4) 3 3 ? Mg3 OH1 Fe3 119.47(19) 3 . ? Fe3 OH1 Fe3 119.47(19) 3 . ? Mg3 OH1 H1 117(7) 3 . ? Fe3 OH1 H1 117(7) 3 . ? Fe3 OH1 H1 112(7) . . ? Mg2 OH2 Fe2 0.00(2) 3_556 3_556 ? Mg2 OH2 Fe2 121.4(2) 3_556 . ? Fe2 OH2 Fe2 121.4(2) 3_556 . ? Mg2 OH2 H2 85(6) 3_556 . ? Fe2 OH2 H2 85(6) 3_556 . ? Fe2 OH2 H2 111(7) . . ? Mg2 OH3 Fe2 0.00(5) 1_554 1_554 ? Mg2 OH3 Fe3 100.64(11) 1_554 . ? Fe2 OH3 Fe3 100.64(11) 1_554 . ? Mg2 OH3 H3 106(4) 1_554 . ? Fe2 OH3 H3 106(4) 1_554 . ? Fe3 OH3 H3 118(4) . . ? Mg1 OW1 Fe1 0.00(3) 1_565 1_565 ? Mg1 OW1 HW1A 122(3) 1_565 . ? Fe1 OW1 HW1A 122(3) 1_565 . ? Mg1 OW1 HW1B 107(3) 1_565 . ? Fe1 OW1 HW1B 107(3) 1_565 . ? HW1A OW1 HW1B 116(3) . . ? OW2B OW2A Na 66.8(16) . . ? OW2A OW2B Na 89.9(19) . . ? OW2A OW2B Na 148(2) . 3_655 ? Na OW2B Na 113.3(12) . 3_655 ? 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 OH1 H1 O6 0.91(3) 2.01(7) 2.784(4) 141(8) 5_454 OH2 H2 O6 0.91(3) 1.81(4) 2.690(4) 162(9) 5_455 OH3 H3 O1 0.89(3) 2.35(5) 3.083(4) 139(5) 6_466 OW1 HW1A O2 0.85(2) 2.00(3) 2.811(3) 162(4) 4_674 OW1 HW1B O3 0.87(2) 1.84(3) 2.702(4) 167(5) 3_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.925 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.156