data_shelx _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.94 H17.70 Fe1.39 Mg0.27 Mn0.37 O17.60 P1.91 Zn0.03' _chemical_formula_weight 490.44 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.3160(10) _cell_length_b 10.620(3) _cell_length_c 7.1180(10) _cell_angle_alpha 107.33(3) _cell_angle_beta 111.33(3) _cell_angle_gamma 72.22(2) _cell_volume 348.45(16) _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_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_F_000 249 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 2.230 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.710 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4231 _diffrn_reflns_av_unetI/netI 0.0465 _diffrn_reflns_av_R_equivalents 0.0472 _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 4.102 _diffrn_reflns_theta_max 26.343 _diffrn_reflns_theta_full 25.214 _diffrn_measured_fraction_theta_max 0.893 _diffrn_measured_fraction_theta_full 0.889 _diffrn_reflns_Laue_measured_fraction_max 0.893 _diffrn_reflns_Laue_measured_fraction_full 0.889 _diffrn_reflns_point_group_measured_fraction_max 0.893 _diffrn_reflns_point_group_measured_fraction_full 0.889 _reflns_number_total 1271 _reflns_number_gt 1226 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.7130P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.184(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1271 _refine_ls_number_parameters 146 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.003 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.0000 1.0000 0.0151(3) Uani 0.37 2 d S . P . . Mg1 Mg 0.0000 0.0000 1.0000 0.0151(3) Uani 0.27 2 d S . P . . Fe1 Fe 0.0000 0.0000 1.0000 0.0151(3) Uani 0.33 2 d S . P . . Zn1 Zn 0.0000 0.0000 1.0000 0.0151(3) Uani 0.03 2 d S . P . . Fe2 Fe 0.0000 0.5000 0.0000 0.0120(3) Uani 0.593(7) 2 d S . P . . Al2 Al 0.0000 0.5000 0.0000 0.0120(3) Uani 0.407(7) 2 d S . P . . Fe3 Fe 0.0000 0.5000 0.5000 0.0127(3) Uani 0.425(7) 2 d S . P . . Al3 Al 0.0000 0.5000 0.5000 0.0127(3) Uani 0.575(7) 2 d S . P . . P1 P 0.34452(13) 0.66876(7) 0.92555(11) 0.0129(3) Uani 0.973(5) 1 d . . . . . O1 O 0.1663(4) 0.6530(2) 0.0430(3) 0.0169(5) Uani 1 1 d . . . . . O2 O 0.2989(4) 0.5752(2) 0.7096(3) 0.0166(5) Uani 1 1 d . . . . . O3 O 0.2701(4) 0.81683(19) 0.9046(3) 0.0177(5) Uani 1 1 d . . . . . O4 O 0.3438(4) 0.3684(2) 0.9523(3) 0.0165(5) Uani 1 1 d . . . . . O5 O 0.1502(4) 0.5041(2) 0.2965(3) 0.0171(5) Uani 1 1 d D . . . . O6 O 0.2329(4) 0.3127(2) 0.5431(3) 0.0193(5) Uani 1 1 d D . . . . O7 O 0.2412(5) 0.0069(2) 0.3207(4) 0.0254(5) Uani 1 1 d D . . . . O8 O 0.2268(4) 0.1099(2) 0.9442(4) 0.0254(6) Uani 1 1 d D . . . . O9 O 0.2679(4) 0.8026(2) 0.5079(3) 0.0219(5) Uani 1 1 d D . . . . H5 H 0.335(4) 0.481(5) 0.322(8) 0.046(4) Uiso 1 1 d D U . . . H6A H 0.290(9) 0.327(5) 0.682(3) 0.046(4) Uiso 1 1 d D U . . . H6B H 0.390(6) 0.280(5) 0.507(6) 0.046(4) Uiso 1 1 d D U . . . H7A H 0.249(10) 0.084(3) 0.418(6) 0.046(4) Uiso 1 1 d D U . . . H7B H 0.209(10) -0.050(4) 0.376(6) 0.046(4) Uiso 1 1 d D U . . . H8A H 0.118(7) 0.192(3) 0.951(7) 0.046(4) Uiso 1 1 d D U . . . H8B H 0.401(4) 0.117(4) 0.986(7) 0.046(4) Uiso 1 1 d D U . . . H9A H 0.257(10) 0.816(5) 0.636(4) 0.046(4) Uiso 1 1 d D U . . . H9B H 0.177(9) 0.738(4) 0.427(6) 0.046(4) Uiso 1 1 d D U . . . 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 0.0117(4) 0.0140(4) 0.0184(4) 0.0024(3) 0.0034(3) -0.0033(2) Mg1 0.0117(4) 0.0140(4) 0.0184(4) 0.0024(3) 0.0034(3) -0.0033(2) Fe1 0.0117(4) 0.0140(4) 0.0184(4) 0.0024(3) 0.0034(3) -0.0033(2) Zn1 0.0117(4) 0.0140(4) 0.0184(4) 0.0024(3) 0.0034(3) -0.0033(2) Fe2 0.0094(4) 0.0141(4) 0.0120(4) 0.0028(3) 0.0021(3) -0.0033(2) Al2 0.0094(4) 0.0141(4) 0.0120(4) 0.0028(3) 0.0021(3) -0.0033(2) Fe3 0.0096(4) 0.0146(5) 0.0128(5) 0.0021(3) 0.0018(3) -0.0040(3) Al3 0.0096(4) 0.0146(5) 0.0128(5) 0.0021(3) 0.0018(3) -0.0040(3) P1 0.0106(4) 0.0135(4) 0.0136(5) 0.0027(3) 0.0020(3) -0.0035(2) O1 0.0139(9) 0.0189(10) 0.0171(10) 0.0034(8) 0.0033(8) -0.0045(7) O2 0.0162(9) 0.0182(10) 0.0154(10) 0.0025(8) 0.0036(8) -0.0062(7) O3 0.0161(9) 0.0155(10) 0.0212(11) 0.0036(8) 0.0047(8) -0.0043(7) O4 0.0129(9) 0.0191(10) 0.0171(10) 0.0051(8) 0.0023(8) -0.0041(7) O5 0.0127(9) 0.0213(10) 0.0163(10) 0.0034(8) 0.0033(7) -0.0041(7) O6 0.0147(9) 0.0228(11) 0.0188(11) 0.0014(8) 0.0045(8) -0.0056(8) O7 0.0224(11) 0.0234(11) 0.0250(12) 0.0033(9) 0.0023(9) -0.0053(9) O8 0.0163(10) 0.0189(11) 0.0410(14) 0.0066(9) 0.0078(9) -0.0044(8) O9 0.0202(10) 0.0264(11) 0.0203(11) 0.0054(9) 0.0064(9) -0.0060(8) _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 O8 2.111(2) 2_557 ? Mn1 O8 2.111(2) . ? Mn1 O3 2.127(2) 1_545 ? Mn1 O3 2.127(2) 2_567 ? Mn1 O7 2.165(2) 1_556 ? Mn1 O7 2.165(2) 2_556 ? Fe2 O5 1.958(2) . ? Fe2 O5 1.958(2) 2_565 ? Fe2 O1 1.975(2) 2_565 ? Fe2 O1 1.975(2) . ? Fe2 O4 2.004(2) 1_554 ? Fe2 O4 2.004(2) 2_566 ? Fe3 O5 1.908(2) 2_566 ? Fe3 O5 1.908(2) . ? Fe3 O2 1.931(2) . ? Fe3 O2 1.931(2) 2_566 ? Fe3 O6 2.041(2) 2_566 ? Fe3 O6 2.041(2) . ? P1 O3 1.539(2) . ? P1 O2 1.541(2) . ? P1 O1 1.543(2) 1_556 ? P1 O4 1.554(2) 2_667 ? O1 P1 1.543(2) 1_554 ? O3 Zn1 2.127(2) 1_565 ? O3 Mn1 2.127(2) 1_565 ? O3 Mg1 2.127(2) 1_565 ? O3 Fe1 2.127(2) 1_565 ? O4 P1 1.554(2) 2_667 ? O4 Fe2 2.004(2) 1_556 ? O4 Al2 2.004(2) 1_556 ? O5 H5 0.90(2) . ? O6 H6A 0.903(19) . ? O6 H6B 0.900(19) . ? O7 Zn1 2.165(2) 1_554 ? O7 Mn1 2.165(2) 1_554 ? O7 Mg1 2.165(2) 1_554 ? O7 Fe1 2.165(2) 1_554 ? O7 H7A 0.902(19) . ? O7 H7B 0.893(19) . ? O8 H8A 0.889(19) . ? O8 H8B 0.887(19) . ? O9 H9A 0.904(19) . ? O9 H9B 0.891(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 O8 Mn1 O8 180.0 2_557 . ? O8 Mn1 O3 90.48(8) 2_557 1_545 ? O8 Mn1 O3 89.52(8) . 1_545 ? O8 Mn1 O3 89.52(8) 2_557 2_567 ? O8 Mn1 O3 90.48(8) . 2_567 ? O3 Mn1 O3 180.00(12) 1_545 2_567 ? O8 Mn1 O7 85.09(10) 2_557 1_556 ? O8 Mn1 O7 94.91(10) . 1_556 ? O3 Mn1 O7 91.49(9) 1_545 1_556 ? O3 Mn1 O7 88.51(9) 2_567 1_556 ? O8 Mn1 O7 94.91(10) 2_557 2_556 ? O8 Mn1 O7 85.09(10) . 2_556 ? O3 Mn1 O7 88.51(9) 1_545 2_556 ? O3 Mn1 O7 91.49(9) 2_567 2_556 ? O7 Mn1 O7 180.0 1_556 2_556 ? O5 Fe2 O5 180.0 . 2_565 ? O5 Fe2 O1 90.56(9) . 2_565 ? O5 Fe2 O1 89.45(9) 2_565 2_565 ? O5 Fe2 O1 89.45(9) . . ? O5 Fe2 O1 90.55(9) 2_565 . ? O1 Fe2 O1 180.00(5) 2_565 . ? O5 Fe2 O4 90.81(9) . 1_554 ? O5 Fe2 O4 89.19(9) 2_565 1_554 ? O1 Fe2 O4 89.51(8) 2_565 1_554 ? O1 Fe2 O4 90.49(8) . 1_554 ? O5 Fe2 O4 89.19(9) . 2_566 ? O5 Fe2 O4 90.81(9) 2_565 2_566 ? O1 Fe2 O4 90.49(8) 2_565 2_566 ? O1 Fe2 O4 89.51(8) . 2_566 ? O4 Fe2 O4 180.00(12) 1_554 2_566 ? O5 Fe3 O5 180.0 2_566 . ? O5 Fe3 O2 91.36(9) 2_566 . ? O5 Fe3 O2 88.64(9) . . ? O5 Fe3 O2 88.64(9) 2_566 2_566 ? O5 Fe3 O2 91.36(9) . 2_566 ? O2 Fe3 O2 180.0 . 2_566 ? O5 Fe3 O6 94.57(9) 2_566 2_566 ? O5 Fe3 O6 85.43(9) . 2_566 ? O2 Fe3 O6 91.96(9) . 2_566 ? O2 Fe3 O6 88.04(9) 2_566 2_566 ? O5 Fe3 O6 85.43(9) 2_566 . ? O5 Fe3 O6 94.57(9) . . ? O2 Fe3 O6 88.04(9) . . ? O2 Fe3 O6 91.96(9) 2_566 . ? O6 Fe3 O6 180.0 2_566 . ? O3 P1 O2 109.49(12) . . ? O3 P1 O1 109.11(12) . 1_556 ? O2 P1 O1 111.59(12) . 1_556 ? O3 P1 O4 108.83(12) . 2_667 ? O2 P1 O4 108.00(11) . 2_667 ? O1 P1 O4 109.78(12) 1_556 2_667 ? P1 O1 Fe2 129.09(12) 1_554 . ? P1 O2 Fe3 137.27(13) . . ? P1 O3 Zn1 136.88(13) . 1_565 ? P1 O3 Mn1 136.88(13) . 1_565 ? Zn1 O3 Mn1 0.0 1_565 1_565 ? P1 O3 Mg1 136.88(13) . 1_565 ? Zn1 O3 Mg1 0.0 1_565 1_565 ? Mn1 O3 Mg1 0.0 1_565 1_565 ? P1 O3 Fe1 136.88(13) . 1_565 ? Zn1 O3 Fe1 0.0 1_565 1_565 ? Mn1 O3 Fe1 0.0 1_565 1_565 ? Mg1 O3 Fe1 0.0 1_565 1_565 ? P1 O4 Fe2 137.77(13) 2_667 1_556 ? P1 O4 Al2 137.77(13) 2_667 1_556 ? Fe2 O4 Al2 0.0 1_556 1_556 ? Fe3 O5 Fe2 134.07(11) . . ? Fe3 O5 H5 118(3) . . ? Fe2 O5 H5 105(3) . . ? Fe3 O6 H6A 101(3) . . ? Fe3 O6 H6B 120(3) . . ? H6A O6 H6B 105(3) . . ? Zn1 O7 Mn1 0.0 1_554 1_554 ? Zn1 O7 Mg1 0.0 1_554 1_554 ? Mn1 O7 Mg1 0.0 1_554 1_554 ? Zn1 O7 Fe1 0.0 1_554 1_554 ? Mn1 O7 Fe1 0.0 1_554 1_554 ? Mg1 O7 Fe1 0.0 1_554 1_554 ? Zn1 O7 H7A 124(3) 1_554 . ? Mn1 O7 H7A 124(3) 1_554 . ? Mg1 O7 H7A 124(3) 1_554 . ? Fe1 O7 H7A 124(3) 1_554 . ? Zn1 O7 H7B 113(3) 1_554 . ? Mn1 O7 H7B 113(3) 1_554 . ? Mg1 O7 H7B 113(3) 1_554 . ? Fe1 O7 H7B 113(3) 1_554 . ? H7A O7 H7B 105(3) . . ? Mn1 O8 H8A 102(3) . . ? Mn1 O8 H8B 137(3) . . ? H8A O8 H8B 109(3) . . ? H9A O9 H9B 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 H5 O2 0.90(2) 1.93(2) 2.802(3) 163(5) 2_666 O6 H6A O4 0.903(19) 1.774(19) 2.668(3) 170(4) . O6 H6B O9 0.900(19) 1.79(2) 2.669(3) 166(4) 2_666 O7 H7A O6 0.902(19) 2.31(2) 3.155(3) 156(4) . O7 H7B O9 0.893(19) 1.95(2) 2.811(3) 161(4) 1_545 O8 H8A O1 0.889(19) 1.86(2) 2.739(3) 168(4) 2_566 O8 H8B O3 0.887(19) 1.89(2) 2.756(3) 164(4) 2_667 O9 H9A O3 0.904(19) 1.88(2) 2.778(3) 171(5) . O9 H9B O5 0.891(19) 2.41(3) 3.223(3) 152(4) . _refine_diff_density_max 0.359 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.095 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL IG1 in P-1 REM transformed to laueite cell : CELL 0.71000 5.3160 10.620 7.1180 107.33 111.33 72.22 ZERR 1 0.001 0.003 0.001 0.03 0.03 0.02 LATT 1 SFAC O AL P MN FE MG ZN H UNIT 17.6 0.94 1.91 0.37 1.39 0.27 0.03 17.7 MERG 2 SHEL 20 0.8 FMAP 2 PLAN 25 FMAP 2 BOND $H DFIX 0.90 0.02 O5 H5 DFIX 0.90 0.02 O6 H6A DFIX 0.90 0.02 O6 H6B DFIX 0.90 0.02 O7 H7A DFIX 0.90 0.02 O7 H7B DFIX 0.90 0.02 O8 H8A DFIX 0.90 0.02 O8 H8B DFIX 0.90 0.02 O9 H9A DFIX 0.90 0.02 O9 H9B DANG 1.45 0.03 H6A H6B DANG 1.45 0.03 H7A H7B DANG 1.45 0.03 H8A H8B DANG 1.45 0.03 H9A H9B EQIV $1 1-X, 1-Y, 1-Z EQIV $2 X, Y-1, Z EQIV $3 -X, 1-Y, 1-Z EQIV $4 1-X, 1-Y, 2-Z ACTA HTAB HTAB O5 O2_$1 HTAB O6 O4 HTAB O6 O9_$1 HTAB O7 O6 HTAB O7 O9_$2 HTAB O8 O1_$3 HTAB O8 O3_$4 HTAB O9 O3 HTAB O9 O5 L.S. 6 EADP FE3 AL3 EXYZ FE3 AL3 EADP MN1 MG1 FE1 ZN1 EXYZ MN1 MG1 FE1 ZN1 EADP FE2 AL2 EXYZ FE2 AL2 ACTA WGHT 0.022000 0.713000 EXTI 0.183837 FVAR 1.61510 0.59329 0.42492 0.76538 0.04590 0.03000 0.03000 FVAR 0.03000 0.03000 MN1 4 0.000000 0.000000 1.000000 10.18500 0.01166 0.01401 = 0.01835 0.00239 0.00341 -0.00332 MG1 6 0.000000 0.000000 1.000000 10.13500 0.01166 0.01401 = 0.01835 0.00239 0.00341 -0.00332 FE1 5 0.000000 0.000000 1.000000 10.16500 0.01166 0.01401 = 0.01835 0.00239 0.00341 -0.00332 ZN1 7 0.000000 0.000000 1.000000 10.01500 0.01166 0.01401 = 0.01835 0.00239 0.00341 -0.00332 FE2 5 0.000000 0.500000 0.000000 20.50000 0.00945 0.01410 = 0.01199 0.00282 0.00208 -0.00325 AL2 2 0.000000 0.500000 0.000000 -20.50000 0.00945 0.01410 = 0.01199 0.00282 0.00208 -0.00325 FE3 5 0.000000 0.500000 0.500000 30.50000 0.00960 0.01462 = 0.01280 0.00211 0.00179 -0.00403 AL3 2 0.000000 0.500000 0.500000 -30.50000 0.00960 0.01462 = 0.01280 0.00211 0.00179 -0.00403 P1 3 0.344522 0.668757 0.925554 0.97259 0.01056 0.01351 = 0.01362 0.00266 0.00201 -0.00348 O1 1 0.166283 0.653041 0.042970 11.00000 0.01387 0.01886 = 0.01714 0.00336 0.00330 -0.00452 O2 1 0.298915 0.575244 0.709608 11.00000 0.01620 0.01819 = 0.01542 0.00253 0.00362 -0.00624 O3 1 0.270066 0.816832 0.904555 11.00000 0.01605 0.01552 = 0.02116 0.00360 0.00467 -0.00433 O4 1 0.343759 0.368364 0.952344 11.00000 0.01289 0.01908 = 0.01705 0.00513 0.00233 -0.00413 O5 1 0.150168 0.504128 0.296461 11.00000 0.01270 0.02130 = 0.01631 0.00342 0.00333 -0.00413 O6 1 0.232914 0.312738 0.543109 11.00000 0.01475 0.02277 = 0.01877 0.00136 0.00449 -0.00565 O7 1 0.241241 0.006924 0.320679 11.00000 0.02241 0.02343 = 0.02498 0.00334 0.00230 -0.00534 O8 1 0.226788 0.109885 0.944168 11.00000 0.01632 0.01887 = 0.04097 0.00662 0.00778 -0.00437 O9 1 0.267923 0.802553 0.507898 11.00000 0.02018 0.02644 = 0.02033 0.00537 0.00640 -0.00596 H5 8 0.334780 0.481145 0.322470 11.00000 51.00000 H6A 8 0.290410 0.327072 0.682165 11.00000 51.00000 H6B 8 0.389875 0.279750 0.506859 11.00000 51.00000 H7A 8 0.248567 0.084195 0.417550 11.00000 51.00000 H7B 8 0.209381 -0.049805 0.375869 11.00000 51.00000 H8A 8 0.117912 0.192381 0.950794 11.00000 51.00000 H8B 8 0.401489 0.117169 0.986035 11.00000 51.00000 H9A 8 0.257243 0.815678 0.636433 11.00000 51.00000 H9B 8 0.177210 0.738256 0.427436 11.00000 51.00000 HKLF 4 REM IG1 in P-1 REM R1 = 0.0317 for 1226 Fo > 4sig(Fo) and 0.0325 for all 1271 data REM 146 parameters refined using 13 restraints END WGHT 0.0219 0.7152 REM Instructions for potential hydrogen bonds HTAB O5 O2_$1 HTAB O6 O4 HTAB O6 O9_$1 HTAB O7 O6 HTAB O7 O9_$2 HTAB O8 O1_$3 HTAB O8 O4 HTAB O8 O3_$4 EQIV $5 -x+1, -y, -z+2 HTAB O8 O8_$5 HTAB O9 O3 HTAB O9 O1 HTAB O9 O5 HTAB O9 O6_$3 REM Highest difference peak 0.359, deepest hole -0.390, 1-sigma level 0.095 Q1 1 0.3250 0.7461 0.9320 11.00000 0.05 0.36 Q2 1 0.0940 0.0993 0.1973 11.00000 0.05 0.35 Q3 1 0.0754 0.8596 0.5688 11.00000 0.05 0.35 Q4 1 0.1353 0.5920 0.6790 11.00000 0.05 0.34 Q5 1 0.2079 0.4385 0.9968 11.00000 0.05 0.34 Q6 1 0.1986 0.3969 0.5485 11.00000 0.05 0.34 Q7 1 0.2146 -0.0049 0.8441 11.00000 0.05 0.33 Q8 1 0.1971 0.5551 -0.0802 11.00000 0.05 0.31 Q9 1 0.2345 0.1386 1.0660 11.00000 0.05 0.31 Q10 1 0.0748 0.5908 0.1927 11.00000 0.05 0.30 Q11 1 0.4779 0.6652 0.9970 11.00000 0.05 0.30 Q12 1 0.1917 0.5868 0.0809 11.00000 0.05 0.30 Q13 1 0.4312 0.4498 1.1332 11.00000 0.05 0.29 Q14 1 -0.0856 0.8199 0.4199 11.00000 0.05 0.29 Q15 1 0.1216 -0.0791 0.1599 11.00000 0.05 0.29 Q16 1 0.3448 0.4595 0.5864 11.00000 0.05 0.29 Q17 1 0.0436 0.2942 0.9780 11.00000 0.05 0.28 Q18 1 0.0872 0.2896 0.4518 11.00000 0.05 0.28 Q19 1 -0.0261 0.5665 0.3352 11.00000 0.05 0.28 Q20 1 0.5000 0.5000 0.5000 10.50000 0.05 0.27 Q21 1 0.0651 0.8589 0.4047 11.00000 0.05 0.27 Q22 1 0.2614 0.1803 0.6674 11.00000 0.05 0.27 Q23 1 0.0040 0.0388 0.3036 11.00000 0.05 0.26 Q24 1 0.3884 0.8324 0.8846 11.00000 0.05 0.26 Q25 1 0.3479 0.3298 0.1953 11.00000 0.05 0.26 ; _shelx_res_checksum 74953 _shelx_hkl_file ; 3 0 0 5248.88 404.16 4 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