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 'Fe3 H14 O16.50 P2' _chemical_formula_weight 507.60 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' 'P' 'P' 0.1023 0.0942 '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' _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 10.0468(8) _cell_length_b 9.7982(8) _cell_length_c 7.3079(5) _cell_angle_alpha 91.026(6) _cell_angle_beta 96.605(7) _cell_angle_gamma 115.828(8) _cell_volume 641.37(9) _cell_formula_units_Z 2 _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 2.628 _exptl_crystal_F_000 508 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 3.691 _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 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8087 _diffrn_reflns_av_unetI/netI 0.0566 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.368 _diffrn_reflns_theta_max 23.244 _diffrn_reflns_theta_full 23.244 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 1835 _reflns_number_gt 1561 _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^)+(0.0460P)^2^+0.8900P] 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 0.0000(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1835 _refine_ls_number_parameters 247 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 3.185 _refine_ls_shift/su_mean 0.268 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 M1 Fe 0.51204(10) 0.34151(10) 0.25921(13) 0.0212(3) Uani 1 1 d . . . . . Fe1 Fe 0.96886(9) 0.24187(9) 0.13371(11) 0.0167(3) Uani 1 1 d . . . . . Fe2 Fe 0.02610(9) 0.76721(9) 0.36817(11) 0.0168(3) Uani 1 1 d . . . . . P1 P 0.81538(17) 0.47391(17) 0.0708(2) 0.0160(4) Uani 1 1 d . . . . . P2 P 0.19056(17) 0.14678(18) 0.4239(2) 0.0165(4) Uani 1 1 d . . . . . O1 O 0.6519(5) 0.4412(5) 0.0805(6) 0.0238(10) Uani 1 1 d . . . . . O2 O 0.8198(4) 0.3212(5) 0.0353(5) 0.0195(10) Uani 1 1 d . . . . . O3 O 0.9127(4) 0.5541(4) 0.2529(6) 0.0195(10) Uani 1 1 d . . . . . O4 O 0.8607(4) 0.5695(5) 0.9073(6) 0.0216(10) Uani 1 1 d . . . . . O5 O 0.0977(4) 0.1444(5) 0.2385(6) 0.0204(10) Uani 1 1 d . . . . . O6 O 0.1514(5) -0.0179(4) 0.4732(6) 0.0187(10) Uani 1 1 d . . . . . O7 O 0.3571(5) 0.2237(5) 0.4009(6) 0.0242(10) Uani 1 1 d . . . . . O8 O 0.1631(4) 0.2317(5) 0.5815(6) 0.0205(10) Uani 1 1 d . . . . . OH1 O 0.9566(5) 0.3068(5) 0.3853(6) 0.0216(10) Uani 1 1 d D . . . . OH2 O 0.0331(5) 0.8425(5) 0.1159(6) 0.0218(10) Uani 1 1 d D . . . . OW1 O 0.3338(5) 0.2536(5) 0.0113(7) 0.0280(11) Uani 1 1 d D . . . . OW2 O 0.6582(5) 0.4200(5) 0.4766(6) 0.0239(10) Uani 1 1 d D . . . . OW3 O 0.4703(5) 0.5284(5) 0.2578(6) 0.0262(11) Uani 1 1 d D . . . . OW4 O 0.5387(6) 0.1501(6) 0.1956(8) 0.0361(12) Uani 1 1 d D . . . . OW5 O 0.2255(5) 0.7504(5) 0.3350(6) 0.0256(11) Uani 1 1 d D . . . . OW6 O -0.2234(5) 0.0422(5) 0.1696(6) 0.0256(11) Uani 1 1 d D . . . . OW7 O 0.491(3) 0.024(3) 0.529(3) 0.054(5) Uani 0.5 1 d . . P . . H1 H 0.951(9) 0.386(5) 0.376(12) 0.050(8) Uiso 1 1 d D U . . . H2 H 0.042(9) 0.929(4) 0.117(12) 0.050(8) Uiso 1 1 d D U . . . H1A H 0.330(8) 0.302(8) -0.077(8) 0.050(8) Uiso 1 1 d D U . . . H1B H 0.256(5) 0.231(9) 0.054(10) 0.050(8) Uiso 1 1 d D U . . . H2B H 0.728(7) 0.491(7) 0.443(11) 0.050(8) Uiso 1 1 d D U . . . H3A H 0.420(8) 0.529(10) 0.162(7) 0.050(8) Uiso 1 1 d D U . . . H4A H 0.607(7) 0.164(9) 0.138(9) 0.050(8) Uiso 1 1 d D U . . . H4B H 0.547(9) 0.101(9) 0.283(7) 0.050(8) Uiso 1 1 d D U . . . H5A H 0.228(10) 0.737(9) 0.226(4) 0.050(8) Uiso 1 1 d D U . . . H5B H 0.243(9) 0.688(7) 0.390(8) 0.050(8) Uiso 1 1 d D U . . . H6A H -0.229(9) 0.023(8) 0.277(4) 0.050(8) Uiso 1 1 d D U . . . H6B H -0.263(9) -0.037(5) 0.108(8) 0.050(8) 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 M1 0.0195(6) 0.0219(6) 0.0214(6) 0.0029(4) 0.0014(4) 0.0085(4) Fe1 0.0183(5) 0.0170(5) 0.0139(5) 0.0014(4) -0.0011(4) 0.0077(4) Fe2 0.0189(5) 0.0165(5) 0.0132(5) 0.0001(4) -0.0018(4) 0.0071(4) P1 0.0153(9) 0.0172(8) 0.0144(9) 0.0015(6) -0.0012(6) 0.0069(7) P2 0.0169(9) 0.0162(9) 0.0150(9) 0.0024(6) -0.0005(6) 0.0066(7) O1 0.018(2) 0.031(3) 0.024(3) 0.003(2) 0.0022(19) 0.011(2) O2 0.020(2) 0.022(2) 0.016(2) -0.0001(18) -0.0039(18) 0.010(2) O3 0.022(2) 0.017(2) 0.016(2) -0.0013(18) -0.0045(18) 0.0070(19) O4 0.018(2) 0.021(2) 0.020(2) 0.0051(19) 0.0000(18) 0.0044(19) O5 0.021(2) 0.022(2) 0.019(2) 0.0015(18) -0.0005(18) 0.0109(19) O6 0.027(2) 0.015(2) 0.013(2) 0.0021(17) -0.0023(18) 0.0090(19) O7 0.017(2) 0.024(2) 0.029(3) 0.0022(19) 0.0036(19) 0.007(2) O8 0.021(2) 0.022(2) 0.018(2) -0.0005(18) 0.0023(18) 0.009(2) OH1 0.031(3) 0.021(2) 0.015(2) 0.0058(19) 0.0010(19) 0.014(2) OH2 0.031(3) 0.018(2) 0.015(2) 0.0029(19) -0.0016(19) 0.011(2) OW1 0.028(3) 0.029(3) 0.030(3) 0.003(2) 0.003(2) 0.015(2) OW2 0.019(3) 0.026(3) 0.022(3) 0.005(2) -0.0001(19) 0.006(2) OW3 0.031(3) 0.031(3) 0.020(3) 0.003(2) -0.002(2) 0.018(2) OW4 0.038(3) 0.035(3) 0.044(3) 0.012(2) 0.016(2) 0.021(3) OW5 0.026(3) 0.032(3) 0.021(3) 0.001(2) -0.001(2) 0.016(2) OW6 0.026(3) 0.022(2) 0.023(3) 0.0033(19) 0.002(2) 0.005(2) OW7 0.055(8) 0.055(14) 0.049(14) 0.021(10) 0.017(9) 0.020(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 M1 O7 1.917(4) . ? M1 O1 1.977(4) . ? M1 OW4 2.059(5) . ? M1 OW3 2.049(5) . ? M1 OW2 1.925(4) . ? M1 OW1 2.255(5) . ? Fe1 O4 1.954(4) 2_766 ? Fe1 OH1 1.969(4) . ? Fe1 OH2 1.984(4) 2_665 ? Fe1 O5 2.013(4) 1_655 ? Fe1 O2 2.037(4) . ? Fe1 OW6 2.114(4) 1_655 ? Fe2 O8 1.982(4) 2_566 ? Fe2 OH1 1.972(4) 2_666 ? Fe2 OH2 1.995(4) . ? Fe2 O3 2.003(4) 1_455 ? Fe2 O6 2.004(4) 1_565 ? Fe2 OW5 2.121(4) . ? P1 O4 1.518(4) 1_554 ? P1 O1 1.540(4) . ? P1 O2 1.535(4) . ? P1 O3 1.529(4) . ? P2 O7 1.539(4) . ? P2 O8 1.528(4) . ? P2 O6 1.546(4) . ? P2 O5 1.548(4) . ? O3 Fe2 2.003(4) 1_655 ? O4 P1 1.518(4) 1_556 ? O4 Fe1 1.954(4) 2_766 ? O5 Fe1 2.013(4) 1_455 ? O6 Fe2 2.004(4) 1_545 ? O8 Fe2 1.982(4) 2_566 ? OH1 Fe2 1.972(4) 2_666 ? OH1 H1 0.81(2) . ? OH2 Fe1 1.984(4) 2_665 ? OH2 H2 0.81(2) . ? OW1 H1A 0.81(2) . ? OW1 H1B 0.82(2) . ? OW2 H2B 0.81(2) . ? OW3 H3A 0.81(2) . ? OW4 H4A 0.81(2) . ? OW4 H4B 0.82(2) . ? OW5 H5A 0.81(2) . ? OW5 H5B 0.81(2) . ? OW6 Fe1 2.114(4) 1_455 ? OW6 H6A 0.81(2) . ? OW6 H6B 0.80(2) . ? OW7 OW7 0.72(2) 2_656 ? 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 O7 M1 O1 171.19(18) . . ? O7 M1 OW4 89.42(19) . . ? O1 M1 OW4 86.26(19) . . ? O7 M1 OW3 96.24(18) . . ? O1 M1 OW3 86.44(18) . . ? OW4 M1 OW3 166.7(2) . . ? O7 M1 OW2 92.17(18) . . ? O1 M1 OW2 96.06(19) . . ? OW4 M1 OW2 98.5(2) . . ? OW3 M1 OW2 93.32(19) . . ? O7 M1 OW1 86.18(18) . . ? O1 M1 OW1 85.73(17) . . ? OW4 M1 OW1 83.7(2) . . ? OW3 M1 OW1 84.60(17) . . ? OW2 M1 OW1 177.18(17) . . ? O4 Fe1 OH1 95.76(18) 2_766 . ? O4 Fe1 OH2 89.52(17) 2_766 2_665 ? OH1 Fe1 OH2 174.68(17) . 2_665 ? O4 Fe1 O5 93.57(17) 2_766 1_655 ? OH1 Fe1 O5 90.14(17) . 1_655 ? OH2 Fe1 O5 88.88(17) 2_665 1_655 ? O4 Fe1 O2 92.43(17) 2_766 . ? OH1 Fe1 O2 88.52(17) . . ? OH2 Fe1 O2 91.91(17) 2_665 . ? O5 Fe1 O2 173.95(16) 1_655 . ? O4 Fe1 OW6 176.80(18) 2_766 1_655 ? OH1 Fe1 OW6 84.76(18) . 1_655 ? OH2 Fe1 OW6 90.01(17) 2_665 1_655 ? O5 Fe1 OW6 89.58(17) 1_655 1_655 ? O2 Fe1 OW6 84.42(17) . 1_655 ? O8 Fe2 OH1 88.34(17) 2_566 2_666 ? O8 Fe2 OH2 98.79(18) 2_566 . ? OH1 Fe2 OH2 172.87(17) 2_666 . ? O8 Fe2 O3 90.16(16) 2_566 1_455 ? OH1 Fe2 O3 91.37(17) 2_666 1_455 ? OH2 Fe2 O3 89.00(17) . 1_455 ? O8 Fe2 O6 93.63(17) 2_566 1_565 ? OH1 Fe2 O6 90.29(17) 2_666 1_565 ? OH2 Fe2 O6 88.89(17) . 1_565 ? O3 Fe2 O6 175.91(16) 1_455 1_565 ? O8 Fe2 OW5 174.26(18) 2_566 . ? OH1 Fe2 OW5 86.32(18) 2_666 . ? OH2 Fe2 OW5 86.58(18) . . ? O3 Fe2 OW5 87.89(17) 1_455 . ? O6 Fe2 OW5 88.49(18) 1_565 . ? O4 P1 O1 105.8(2) 1_554 . ? O4 P1 O2 110.1(2) 1_554 . ? O1 P1 O2 107.8(2) . . ? O4 P1 O3 112.9(2) 1_554 . ? O1 P1 O3 110.2(2) . . ? O2 P1 O3 109.8(2) . . ? O7 P2 O8 109.5(2) . . ? O7 P2 O6 107.5(2) . . ? O8 P2 O6 109.3(2) . . ? O7 P2 O5 108.8(2) . . ? O8 P2 O5 112.0(2) . . ? O6 P2 O5 109.7(2) . . ? P1 O1 M1 133.2(3) . . ? P1 O2 Fe1 132.0(2) . . ? P1 O3 Fe2 137.7(3) . 1_655 ? P1 O4 Fe1 135.0(3) 1_556 2_766 ? P2 O5 Fe1 138.6(2) . 1_455 ? P2 O6 Fe2 140.2(3) . 1_545 ? P2 O7 M1 149.6(3) . . ? P2 O8 Fe2 129.0(3) . 2_566 ? Fe1 OH1 Fe2 134.8(2) . 2_666 ? Fe1 OH1 H1 106(6) . . ? Fe2 OH1 H1 119(6) 2_666 . ? Fe1 OH2 Fe2 134.8(2) 2_665 . ? Fe1 OH2 H2 113(6) 2_665 . ? Fe2 OH2 H2 112(6) . . ? M1 OW1 H1A 125(6) . . ? M1 OW1 H1B 105(6) . . ? H1A OW1 H1B 106(3) . . ? M1 OW2 H2B 104(6) . . ? M1 OW3 H3A 112(6) . . ? M1 OW4 H4A 115(6) . . ? M1 OW4 H4B 116(6) . . ? H4A OW4 H4B 107(3) . . ? Fe2 OW5 H5A 110(6) . . ? Fe2 OW5 H5B 119(6) . . ? H5A OW5 H5B 108(3) . . ? Fe1 OW6 H6A 113(5) 1_455 . ? Fe1 OW6 H6B 129(5) 1_455 . ? H6A OW6 H6B 107(4) . . ? 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 O3 0.81(2) 2.05(4) 2.814(6) 158(8) . OH2 H2 O5 0.81(2) 2.08(4) 2.841(6) 155(8) 1_565 OW1 H1B O5 0.82(2) 2.10(3) 2.878(6) 158(7) . OW1 H1A OW3 0.81(2) 2.51(5) 3.112(7) 131(6) 2_665 OW2 H2B O8 0.81(2) 2.47(6) 3.153(6) 143(8) 2_666 OW3 H3A O1 0.81(2) 1.92(3) 2.712(6) 166(9) 2_665 OW4 H4A O2 0.81(2) 2.24(5) 2.977(6) 151(8) . OW4 H4B OW7 0.82(2) 2.01(4) 2.75(3) 149(7) . OW4 H4A OW6 0.81(2) 2.47(6) 3.027(6) 127(6) 1_655 OW4 H4B OW7 0.82(2) 1.82(4) 2.62(3) 164(8) 2_656 OW5 H5A O2 0.81(2) 1.93(3) 2.719(6) 165(9) 2_665 OW5 H5B OW2 0.81(2) 1.94(3) 2.731(6) 164(9) 2_666 OW6 H6A O6 0.81(2) 1.91(4) 2.670(6) 155(8) 2_556 OW6 H6B OW1 0.80(2) 2.06(3) 2.847(6) 167(8) 2 _refine_diff_density_max 1.034 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.155 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL Znferristrunz used for ferristrunz REM transformed to space group : CELL 0.71075 10.0468 9.7982 7.3079 91.026 96.605 115.828 ZERR 2 0.0008 0.0008 0.0005 0.006 0.007 0.008 LATT 1 SFAC O H P FE UNIT 33 28 4 6 MERG 2 SHEL 999 0.9 L.S. 4 BOND FMAP 2 PLAN 60 DFIX 0.82 0.02 OH1 H1 OH2 H2 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.02 OW4 H4A OW4 H4B OW5 H5a OW5 H5b OW6 H6a OW6 H6b DFIX 0.82 0.02 OW7 H7A OW7 H7B DFIX 1.30 0.02 H1a H1b H2a H2b H3a H3b H4a H4b H5a H5b H6a H6b H7A H7B BOND $H EQIV $1 x, y+1, z EQIV $2 -x+1, -y+1,-z EQIV $3 -x+1, -y+1, -z+1 EQIV $4 -x, -y,-z+1 EQIV $5 -x, -y, -z EQIV $6 x+1, y, z EQIV $7 -x+1, -y, -z+1 HTAB 2.5 HTAB OH1 O3 HTAB OH2 O5_$1 HTAB OW1 O5 HTAB OW1 OW3_$2 HTAB OW2 O8_$3 HTAB OW3 O1_$2 HTAB OW4 O2 HTAB OW4 OW7 HTAB OW4 OW6_$6 HTAB OW4 OW7_$7 HTAB OW5 O2_$2 HTAB OW5 OW2_$3 HTAB OW6 O6_$4 HTAB OW6 OW1_$5 ACTA WGHT 0.046000 0.890000 EXTI 0.000000 FVAR 2.12855 0.05033 0.05000 0.05000 0.05000 0.05000 0.05000 FVAR 0.05000 0.05000 0.05000 0.05000 0.05000 M1 4 0.512043 0.341507 0.259213 11.00000 0.01948 0.02189 = 0.02135 0.00293 0.00135 0.00852 FE1 4 0.968861 0.241867 0.133711 11.00000 0.01831 0.01698 = 0.01390 0.00137 -0.00110 0.00766 FE2 4 0.026097 0.767213 0.368170 11.00000 0.01892 0.01645 = 0.01317 0.00008 -0.00179 0.00710 P1 3 0.815385 0.473913 0.070763 11.00000 0.01534 0.01720 = 0.01442 0.00146 -0.00124 0.00687 P2 3 0.190564 0.146784 0.423925 11.00000 0.01687 0.01624 = 0.01500 0.00242 -0.00049 0.00658 O1 1 0.651945 0.441177 0.080496 11.00000 0.01758 0.03055 = 0.02377 0.00319 0.00221 0.01128 O2 1 0.819756 0.321163 0.035342 11.00000 0.01962 0.02200 = 0.01635 -0.00011 -0.00386 0.01019 O3 1 0.912651 0.554111 0.252930 11.00000 0.02240 0.01678 = 0.01566 -0.00125 -0.00448 0.00695 O4 1 0.860704 0.569500 0.907338 11.00000 0.01789 0.02146 = 0.02020 0.00513 -0.00005 0.00442 O5 1 0.097731 0.144371 0.238525 11.00000 0.02103 0.02165 = 0.01919 0.00154 -0.00049 0.01089 O6 1 0.151449 -0.017921 0.473212 11.00000 0.02685 0.01497 = 0.01268 0.00212 -0.00234 0.00899 O7 1 0.357148 0.223740 0.400919 11.00000 0.01680 0.02445 = 0.02891 0.00224 0.00363 0.00675 O8 1 0.163122 0.231702 0.581543 11.00000 0.02059 0.02192 = 0.01820 -0.00052 0.00225 0.00894 OH1 1 0.956581 0.306774 0.385262 11.00000 0.03132 0.02084 = 0.01541 0.00584 0.00097 0.01437 OH2 1 0.033141 0.842505 0.115943 11.00000 0.03082 0.01844 = 0.01538 0.00292 -0.00163 0.01125 OW1 1 0.333764 0.253627 0.011320 11.00000 0.02766 0.02858 = 0.02973 0.00309 0.00254 0.01462 OW2 1 0.658190 0.420014 0.476629 11.00000 0.01894 0.02642 = 0.02172 0.00485 -0.00010 0.00619 OW3 1 0.470304 0.528379 0.257766 11.00000 0.03096 0.03101 = 0.02039 0.00295 -0.00221 0.01840 OW4 1 0.538675 0.150056 0.195648 11.00000 0.03768 0.03531 = 0.04360 0.01162 0.01597 0.02097 OW5 1 0.225499 0.750370 0.334999 11.00000 0.02640 0.03235 = 0.02068 0.00082 -0.00062 0.01636 OW6 1 -0.223422 0.042176 0.169638 11.00000 0.02576 0.02233 = 0.02251 0.00330 0.00202 0.00525 OW7 1 0.491342 0.024090 0.529105 10.50000 0.05536 0.05468 = 0.04900 0.02056 0.01749 0.01976 H1 2 0.950611 0.386173 0.376427 11.00000 21.00000 H2 2 0.042118 0.929070 0.117288 11.00000 21.00000 H1A 2 0.330023 0.301809 -0.077261 11.00000 21.00000 H1B 2 0.255605 0.230605 0.053611 11.00000 21.00000 H2B 2 0.728128 0.490592 0.442708 11.00000 21.00000 H3A 2 0.420109 0.528701 0.162478 11.00000 21.00000 H4A 2 0.607095 0.164481 0.137657 11.00000 21.00000 H4B 2 0.547139 0.101365 0.282754 11.00000 21.00000 H5A 2 0.228333 0.736510 0.226225 11.00000 21.00000 H5B 2 0.243494 0.687686 0.389760 11.00000 21.00000 H6A 2 -0.229043 0.022962 0.276842 11.00000 21.00000 H6B 2 -0.262944 -0.037220 0.107980 11.00000 21.00000 HKLF 4 REM Znferristrunz used for ferristrunz REM R1 = 0.0412 for 1561 Fo > 4sig(Fo) and 0.0489 for all 1835 data REM 247 parameters refined using 16 restraints END WGHT 0.0630 1.2396 REM Instructions for potential hydrogen bonds HTAB OH1 O3 EQIV $8 -x+2, -y+1, -z+1 HTAB OH1 OH1_$8 HTAB OH2 O5_$1 EQIV $9 -x, -y+2, -z HTAB OH2 OH2_$9 HTAB OW1 O1_$2 EQIV $10 x, y, z-1 HTAB OW1 O8_$10 HTAB OW1 OW3_$2 HTAB OW1 O4_$3 HTAB OW1 O5 EQIV $11 -x, -y+1, -z HTAB OW1 OH2_$11 HTAB OW2 O3 HTAB OW2 O8_$3 HTAB OW2 OH1_$8 HTAB OW3 O1_$2 HTAB OW3 O4_$3 HTAB OW4 O2 HTAB OW4 OW6_$6 HTAB OW4 OW7 HTAB OW4 OW7_$7 HTAB OW5 O2_$2 HTAB OW5 O4_$3 HTAB OW5 OW2_$3 HTAB OW6 O6_$4 HTAB OW6 O8_$4 HTAB OW6 OW7_$4 HTAB OW6 OW1_$5 HTAB OW6 OW4_$5 REM Highest difference peak 1.034, deepest hole -0.701, 1-sigma level 0.155 Q1 1 0.6177 0.3682 0.1469 11.00000 0.05 1.03 Q2 1 0.4008 0.2578 0.2198 11.00000 0.05 0.76 Q3 1 0.3549 0.2854 0.3180 11.00000 0.05 0.73 Q4 1 0.4248 0.5567 0.3794 11.00000 0.05 0.67 Q5 1 0.1135 0.2816 0.5676 11.00000 0.05 0.66 Q6 1 0.0539 0.1276 0.5002 11.00000 0.05 0.64 Q7 1 0.9256 0.6686 0.8580 11.00000 0.05 0.64 Q8 1 0.8778 0.6995 0.9307 11.00000 0.05 0.62 Q9 1 0.1693 0.8233 0.3247 11.00000 0.05 0.59 Q10 1 0.2468 0.3512 0.5648 11.00000 0.05 0.58 Q11 1 0.9089 0.2994 0.1094 11.00000 0.05 0.57 Q12 1 0.1493 0.1584 0.3098 11.00000 0.05 0.57 Q13 1 0.7115 0.4011 0.0558 11.00000 0.05 0.56 Q14 1 0.8506 0.5184 0.1769 11.00000 0.05 0.56 Q15 1 0.8682 0.1536 0.1397 11.00000 0.05 0.54 Q16 1 0.6393 0.4736 0.1403 11.00000 0.05 0.53 Q17 1 1.0244 0.1738 0.1517 11.00000 0.05 0.53 Q18 1 0.8087 0.6339 0.9247 11.00000 0.05 0.51 Q19 1 0.9957 0.5988 0.2399 11.00000 0.05 0.50 Q20 1 0.0763 0.7059 0.3840 11.00000 0.05 0.49 Q21 1 0.5115 0.2847 0.1528 11.00000 0.05 0.49 Q22 1 0.2947 0.2453 0.4331 11.00000 0.05 0.47 Q23 1 -0.2524 0.1193 0.1769 11.00000 0.05 0.47 Q24 1 0.0962 0.0004 0.5075 11.00000 0.05 0.47 Q25 1 -0.0228 0.8371 0.3599 11.00000 0.05 0.47 Q26 1 0.8903 0.3872 -0.0067 11.00000 0.05 0.47 Q27 1 0.9547 0.5100 0.9767 11.00000 0.05 0.45 Q28 1 0.2692 0.8924 0.2896 11.00000 0.05 0.44 Q29 1 0.2420 0.2191 0.3289 11.00000 0.05 0.43 Q30 1 0.1453 0.1839 0.1504 11.00000 0.05 0.42 Q31 1 0.6416 0.4365 0.3003 11.00000 0.05 0.42 Q32 1 0.4339 0.0782 0.7358 11.00000 0.05 0.41 Q33 1 0.4156 -0.0409 0.2928 11.00000 0.05 0.40 Q34 1 0.9992 0.5937 0.4031 11.00000 0.05 0.40 Q35 1 0.9014 0.4452 0.7948 11.00000 0.05 0.39 Q36 1 0.2774 0.3985 0.0543 11.00000 0.05 0.38 Q37 1 0.9230 0.2574 0.3764 11.00000 0.05 0.37 Q38 1 0.8203 0.2383 0.2028 11.00000 0.05 0.37 Q39 1 -0.0393 0.0814 0.1272 11.00000 0.05 0.36 Q40 1 0.1608 0.2186 0.4437 11.00000 0.05 0.36 Q41 1 0.8242 0.2344 0.3716 11.00000 0.05 0.36 Q42 1 0.4498 0.4107 0.2353 11.00000 0.05 0.36 Q43 1 0.4163 0.1047 0.5511 11.00000 0.05 0.35 Q44 1 0.5600 0.3640 0.0102 11.00000 0.05 0.35 Q45 1 0.8601 0.4076 0.0644 11.00000 0.05 0.35 Q46 1 0.5793 0.3689 0.4017 11.00000 0.05 0.34 Q47 1 0.8169 0.4998 0.0032 11.00000 0.05 0.34 Q48 1 0.5568 0.4333 0.4210 11.00000 0.05 0.33 Q49 1 0.4653 0.3380 0.5054 11.00000 0.05 0.33 Q50 1 0.4580 0.1010 0.3101 11.00000 0.05 0.33 Q51 1 0.3847 0.1226 0.4014 11.00000 0.05 0.32 Q52 1 0.9665 0.4211 0.1679 11.00000 0.05 0.32 Q53 1 0.6061 0.4324 0.0062 11.00000 0.05 0.32 Q54 1 0.3791 0.8225 0.2630 11.00000 0.05 0.32 Q55 1 0.3527 0.3263 0.1091 11.00000 0.05 0.31 Q56 1 0.1107 -0.0548 0.3847 11.00000 0.05 0.31 Q57 1 0.8089 0.5595 0.8541 11.00000 0.05 0.30 Q58 1 0.8727 0.5888 0.4470 11.00000 0.05 0.30 Q59 1 0.4399 0.0130 0.0894 11.00000 0.05 0.30 Q60 1 0.3745 0.4014 -0.1932 11.00000 0.05 0.30 ; _shelx_res_checksum 54976 _shelx_hkl_file ; 1 0 -1 70.76 24.39 1 0 -1 28.72 35.54 -1 0 1 65.17 65.99 1 0 -1 23.41 35.54 -1 0 1 83.20 33.77 0 1 -1 1067.14 121.75 0 -1 1 938.45 180.72 0 -1 1 941.90 62.99 0 1 -1 1063.32 102.71 0 1 -1 1068.63 95.02 -1 1 1 2275.41 139.94 1 -1 -1 2357.77 236.65 -1 1 1 2181.49 152.34 1 -1 -1 2242.23 156.79 1 -1 -1 2557.34 136.43 0 1 181792.64 7760.66 0 -1 -192388.53 8420.93 0 -1 -181250.92 7925.70 0 1 191298.41 8412.02 -1 1 -167390.28 5718.00 1 -1 164514.64 5530.67 1 0 1 808.67 123.62 1 0 1 740.94 99.52 -1 0 -1 886.56 164.74 -1 0 -1 970.62 129.36 -1 -1 010368.94 584.73 1 1 011064.80 872.77 -1 -1 0 9837.68 725.64 1 1 0 9159.83 480.37 2 -1 0 5517.86 342.13 -2 1 0 6809.09 400.85 2 -1 0 6627.76 523.71 -2 1 0 6296.12 355.08 -2 1 0 5766.06 366.70 2 -1 0 7051.96 596.64 -1 2 0 5853.28 337.19 -1 2 0 6710.21 451.43 1 -2 0 6568.67 453.94 1 -2 0 6514.52 567.29 1 -2 0 5872.96 525.46 -1 2 0 6104.01 357.80 1 1 -1 1924.42 297.39 1 1 -1 1624.96 118.13 -1 -1 1 1741.38 185.66 -1 -1 1 1998.40 280.10 1 1 -1 1809.07 58.32 -2 0 036744.57 2638.37 2 0 036462.07 2951.36 2 0 039602.75 2673.32 -2 0 039616.23 2715.32 -2 0 035743.78 2494.26 0 2 043263.00 2919.56 0 2 042747.36 3633.11 0 -2 043409.05 3415.48 0 -2 042864.94 3307.34 0 -2 040692.85 3521.42 0 2 043744.22 3282.44 -2 1 1 804.20 64.68 2 -1 -1 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