data_[Fe(H2O)6][1]2.14H2O _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H22 F Fe2 N2 O13), Fe H12 O6, 14(H2 O)' _chemical_formula_sum 'C32 H84 F2 Fe5 N4 O46' _chemical_formula_weight 1578.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 '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' 'N' 'N' 0.0061 0.0033 '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' 'F' 'F' 0.0171 0.0103 '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 10.8238(3) _cell_length_b 11.3967(3) _cell_length_c 13.4092(4) _cell_angle_alpha 92.709(2) _cell_angle_beta 113.420(3) _cell_angle_gamma 90.301(2) _cell_volume 1515.61(8) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 17362 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.69 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_F_000 820 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_absorpt_coefficient_mu 1.290 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_standards_number '.' _diffrn_standards_interval_time '.' _diffrn_standards_decay_% '.' _diffrn_reflns_number 27964 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.657 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.004 _diffrn_measured_fraction_theta_full 1.004 _diffrn_reflns_Laue_measured_fraction_max 1.004 _diffrn_reflns_Laue_measured_fraction_full 1.004 _diffrn_reflns_point_group_measured_fraction_max 1.004 _diffrn_reflns_point_group_measured_fraction_full 1.004 _reflns_number_total 6967 _reflns_number_gt 6627 _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 ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXTL v6.10 (Sheldrick, 2008)' _computing_publication_material 'SHELXTL v6.10 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.0223P)^2^+2.0226P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6967 _refine_ls_number_parameters 488 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.050 _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_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 Fe1 Fe 0.68199(3) 0.74448(3) 0.33774(2) 0.00962(7) Uani 1 1 d . . . . . O1W O 0.82159(18) 0.88482(16) 0.39056(14) 0.0172(4) Uani 1 1 d D . . . . H1W1 H 0.850(3) 0.906(3) 0.4539(18) 0.026 Uiso 1 1 d D U . . . H1W2 H 0.881(3) 0.891(3) 0.368(2) 0.026 Uiso 1 1 d D U . . . O2W O 0.70549(19) 0.72460(17) 0.18331(14) 0.0178(4) Uani 1 1 d D . . . . H2W1 H 0.777(2) 0.712(3) 0.180(2) 0.027 Uiso 1 1 d D U . . . H2W2 H 0.653(3) 0.746(3) 0.124(2) 0.027 Uiso 1 1 d D U . . . Fe2 Fe 0.83655(3) 0.76504(3) 0.64675(2) 0.00939(7) Uani 1 1 d . . . . . O3W O 1.00918(18) 0.77776(16) 0.80319(14) 0.0171(4) Uani 1 1 d D . . . . H3W1 H 1.019(3) 0.748(3) 0.860(2) 0.026 Uiso 1 1 d D U . . . H3W2 H 1.080(3) 0.801(3) 0.806(2) 0.026 Uiso 1 1 d D U . . . O4W O 0.92291(18) 0.62365(16) 0.59790(14) 0.0178(4) Uani 1 1 d D . . . . H4W1 H 1.005(2) 0.609(3) 0.624(2) 0.027 Uiso 1 1 d D U . . . H4W2 H 0.896(3) 0.608(3) 0.5314(18) 0.027 Uiso 1 1 d D U . . . C1 C 0.7484(2) 0.4984(2) 0.31896(18) 0.0115(4) Uani 1 1 d . . . . . C2 C 0.5975(2) 0.4986(2) 0.25202(19) 0.0135(5) Uani 1 1 d . . . . . H2A H 0.5806 0.5040 0.1742 0.016 Uiso 1 1 calc R U . . . H2B H 0.5563 0.4237 0.2600 0.016 Uiso 1 1 calc R U . . . C3 C 0.4113(2) 0.6364(2) 0.19775(18) 0.0124(4) Uani 1 1 d . . . . . H3A H 0.3315 0.6058 0.2079 0.015 Uiso 1 1 calc R U . . . H3B H 0.4083 0.6017 0.1277 0.015 Uiso 1 1 calc R U . . . C4 C 0.4022(2) 0.7696(2) 0.19112(18) 0.0122(4) Uani 1 1 d . . . . . C5 C 0.5054(2) 0.5623(2) 0.38134(18) 0.0124(4) Uani 1 1 d . . . . . H5A H 0.5880 0.5292 0.4353 0.015 Uiso 1 1 calc R U . . . H5B H 0.4347 0.4994 0.3563 0.015 Uiso 1 1 calc R U . . . C6 C 0.4605(2) 0.6612(2) 0.43669(18) 0.0118(4) Uani 1 1 d . . . . . C7 C 0.3330(2) 0.6585(2) 0.43826(18) 0.0145(5) Uani 1 1 d . . . . . H7 H 0.2692 0.5984 0.3979 0.017 Uiso 1 1 calc R U . . . C8 C 0.3002(2) 0.7441(2) 0.4991(2) 0.0151(5) Uani 1 1 d . . . . . C9 C 0.3894(2) 0.8333(2) 0.55870(18) 0.0145(5) Uani 1 1 d . . . . . H9 H 0.3642 0.8905 0.6005 0.017 Uiso 1 1 calc R U . . . C10 C 0.5173(2) 0.8381(2) 0.55655(18) 0.0125(4) Uani 1 1 d . . . . . C11 C 0.5537(2) 0.7520(2) 0.49500(18) 0.0106(4) Uani 1 1 d . . . . . C12 C 0.6142(2) 0.9388(2) 0.61365(18) 0.0124(4) Uani 1 1 d . . . . . H12A H 0.6422 0.9759 0.5604 0.015 Uiso 1 1 calc R U . . . H12B H 0.5672 0.9984 0.6407 0.015 Uiso 1 1 calc R U . . . C13 C 0.7023(2) 0.8565(2) 0.79353(18) 0.0127(4) Uani 1 1 d . . . . . H13A H 0.6126 0.8845 0.7856 0.015 Uiso 1 1 calc R U . . . H13B H 0.7688 0.8880 0.8648 0.015 Uiso 1 1 calc R U . . . C14 C 0.7006(2) 0.7227(2) 0.79246(18) 0.0107(4) Uani 1 1 d . . . . . C15 C 0.8332(2) 1.0034(2) 0.74448(19) 0.0138(5) Uani 1 1 d . . . . . H15A H 0.8933 0.9947 0.8217 0.017 Uiso 1 1 calc R U . . . H15B H 0.7837 1.0771 0.7401 0.017 Uiso 1 1 calc R U . . . C16 C 0.9181(2) 1.0116(2) 0.67730(18) 0.0122(4) Uani 1 1 d . . . . . N1 N 0.53344(19) 0.59751(16) 0.28625(15) 0.0104(4) Uani 1 1 d . . . . . N2 N 0.7361(2) 0.90330(16) 0.70624(15) 0.0104(4) Uani 1 1 d . . . . . O1 O 0.80483(16) 0.59082(14) 0.37634(13) 0.0123(3) Uani 1 1 d . . . . . O2 O 0.80917(17) 0.40842(14) 0.30991(14) 0.0161(4) Uani 1 1 d . . . . . O3 O 0.50696(17) 0.83303(14) 0.24458(13) 0.0128(3) Uani 1 1 d . . . . . O4 O 0.29197(17) 0.80708(15) 0.12898(14) 0.0157(3) Uani 1 1 d . . . . . O5 O 0.67712(15) 0.75586(14) 0.49308(13) 0.0109(3) Uani 1 1 d . . . . . O6 O 0.74769(17) 0.66649(14) 0.73168(13) 0.0126(3) Uani 1 1 d . . . . . O7 O 0.65760(17) 0.67559(15) 0.85539(13) 0.0147(3) Uani 1 1 d . . . . . O8 O 0.91928(17) 0.92213(14) 0.61615(13) 0.0122(3) Uani 1 1 d . . . . . O9 O 0.98629(18) 1.10325(14) 0.68899(13) 0.0153(3) Uani 1 1 d . . . . . F1 F 0.17437(14) 0.74093(15) 0.50059(13) 0.0216(3) Uani 1 1 d . . . . . Fe3 Fe 0.0000 0.5000 0.0000 0.01085(10) Uani 1 2 d S . P . . O5W O 0.09298(19) 0.51076(15) 0.16890(13) 0.0163(3) Uani 1 1 d D . . . . H5W1 H 0.060(3) 0.545(2) 0.209(2) 0.024 Uiso 1 1 d D U . . . H5W2 H 0.139(3) 0.458(2) 0.202(2) 0.024 Uiso 1 1 d D U . . . O6W O 0.18244(17) 0.46231(15) -0.01487(14) 0.0151(3) Uani 1 1 d D . . . . H6W1 H 0.222(3) 0.515(2) -0.031(2) 0.023 Uiso 1 1 d D U . . . H6W2 H 0.235(3) 0.429(2) 0.038(2) 0.023 Uiso 1 1 d D U . . . O7W O -0.04462(18) 0.31037(14) -0.00541(14) 0.0137(3) Uani 1 1 d D . . . . H7W1 H 0.001(3) 0.269(2) -0.028(2) 0.021 Uiso 1 1 d D U . . . H7W2 H -0.124(2) 0.285(3) -0.038(2) 0.021 Uiso 1 1 d D U . . . O8W O 0.5788(2) 0.02288(16) 0.14186(14) 0.0206(4) Uani 1 1 d D . . . . H8W1 H 0.554(3) -0.033(2) 0.167(2) 0.031 Uiso 1 1 d D U . . . H8W2 H 0.641(3) 0.057(3) 0.194(2) 0.031 Uiso 1 1 d D U . . . O9W O 0.46975(19) 0.22152(16) 0.02329(14) 0.0177(4) Uani 1 1 d D . . . . H9W1 H 0.430(3) 0.251(2) 0.061(2) 0.027 Uiso 1 1 d D U . . . H9W2 H 0.485(3) 0.152(2) 0.043(2) 0.027 Uiso 1 1 d D U . . . O10W O 0.98565(19) 0.65045(15) 0.27888(14) 0.0168(4) Uani 1 1 d D . . . . H0W3 H 1.020(3) 0.716(2) 0.301(2) 0.025 Uiso 1 1 d D U . . . H0W4 H 0.961(3) 0.627(2) 0.326(2) 0.025 Uiso 1 1 d D U . . . O11W O 0.8994(2) 0.82809(16) 0.08204(15) 0.0215(4) Uani 1 1 d D . . . . H1W3 H 0.863(3) 0.889(2) 0.058(2) 0.032 Uiso 1 1 d D U . . . H1W4 H 0.938(3) 0.835(3) 0.1474(18) 0.032 Uiso 1 1 d D U . . . O12W O 0.7099(2) 0.35618(17) 0.08021(15) 0.0216(4) Uani 1 1 d D . . . . H2W3 H 0.746(3) 0.358(3) 0.1477(18) 0.032 Uiso 1 1 d D U . . . H2W4 H 0.641(3) 0.312(3) 0.062(2) 0.032 Uiso 1 1 d D U . . . O13W O 0.79827(19) 0.15502(16) 0.28337(15) 0.0201(4) Uani 1 1 d D . . . . H3W3 H 0.794(3) 0.224(2) 0.305(3) 0.030 Uiso 1 1 d D U . . . H3W4 H 0.860(3) 0.125(3) 0.332(2) 0.030 Uiso 1 1 d D U . . . O14W O 0.7601(2) 0.02842(19) 0.03001(18) 0.0301(5) Uani 1 1 d D . . . . H4W3 H 0.693(3) 0.022(3) 0.044(3) 0.045 Uiso 1 1 d D U . . . H4W4 H 0.736(4) 0.070(3) -0.023(2) 0.045 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 Fe1 0.01022(16) 0.00933(14) 0.00851(14) -0.00153(11) 0.00312(12) 0.00031(12) O1W 0.0182(9) 0.0221(9) 0.0125(8) -0.0052(7) 0.0082(7) -0.0073(7) O2W 0.0132(9) 0.0289(10) 0.0121(8) 0.0014(7) 0.0059(7) 0.0054(8) Fe2 0.01096(16) 0.00854(14) 0.00850(14) -0.00141(11) 0.00389(13) 0.00045(12) O3W 0.0129(9) 0.0258(9) 0.0117(8) 0.0024(7) 0.0040(7) -0.0031(7) O4W 0.0148(9) 0.0227(9) 0.0114(8) -0.0048(7) 0.0011(7) 0.0076(7) C1 0.0131(11) 0.0139(11) 0.0075(10) 0.0006(8) 0.0041(9) 0.0005(9) C2 0.0118(11) 0.0117(10) 0.0142(10) -0.0052(8) 0.0030(9) 0.0003(9) C3 0.0103(11) 0.0130(11) 0.0114(10) -0.0020(8) 0.0020(9) -0.0004(9) C4 0.0134(11) 0.0157(11) 0.0097(10) -0.0006(8) 0.0071(9) 0.0015(9) C5 0.0125(11) 0.0129(10) 0.0115(10) -0.0002(8) 0.0046(9) -0.0013(9) C6 0.0117(11) 0.0138(11) 0.0094(10) 0.0018(8) 0.0035(9) 0.0000(9) C7 0.0131(11) 0.0180(11) 0.0103(10) 0.0021(9) 0.0023(9) -0.0012(9) C8 0.0083(10) 0.0251(12) 0.0127(10) 0.0045(9) 0.0044(9) 0.0027(10) C9 0.0145(12) 0.0198(12) 0.0108(10) 0.0026(9) 0.0066(9) 0.0055(9) C10 0.0142(11) 0.0136(11) 0.0099(10) 0.0016(8) 0.0049(9) 0.0018(9) C11 0.0095(10) 0.0130(10) 0.0087(10) 0.0025(8) 0.0026(9) 0.0019(9) C12 0.0146(11) 0.0111(10) 0.0120(10) 0.0001(8) 0.0059(9) 0.0030(9) C13 0.0169(12) 0.0133(11) 0.0099(10) -0.0003(8) 0.0076(9) 0.0006(9) C14 0.0077(10) 0.0136(11) 0.0081(10) 0.0008(8) 0.0002(8) -0.0009(8) C15 0.0172(12) 0.0115(10) 0.0150(11) -0.0038(8) 0.0093(10) -0.0024(9) C16 0.0124(11) 0.0126(10) 0.0095(10) -0.0001(8) 0.0022(9) 0.0004(9) N1 0.0098(9) 0.0115(9) 0.0086(9) -0.0007(7) 0.0025(7) 0.0015(7) N2 0.0125(9) 0.0085(8) 0.0106(9) -0.0011(7) 0.0054(8) -0.0008(7) O1 0.0120(8) 0.0127(8) 0.0104(7) -0.0018(6) 0.0027(6) 0.0006(6) O2 0.0151(8) 0.0141(8) 0.0165(8) -0.0034(6) 0.0041(7) 0.0027(7) O3 0.0121(8) 0.0110(7) 0.0139(8) 0.0000(6) 0.0038(7) 0.0009(6) O4 0.0121(8) 0.0170(8) 0.0155(8) 0.0010(7) 0.0027(7) 0.0042(7) O5 0.0096(7) 0.0140(7) 0.0092(7) -0.0013(6) 0.0040(6) 0.0002(6) O6 0.0142(8) 0.0116(8) 0.0134(8) 0.0000(6) 0.0071(7) 0.0011(6) O7 0.0147(8) 0.0164(8) 0.0153(8) 0.0025(6) 0.0081(7) -0.0003(7) O8 0.0156(8) 0.0109(7) 0.0118(8) -0.0029(6) 0.0076(7) -0.0012(6) O9 0.0183(9) 0.0123(8) 0.0170(8) -0.0032(6) 0.0093(7) -0.0043(7) F1 0.0102(7) 0.0377(9) 0.0188(7) -0.0013(6) 0.0082(6) -0.0007(7) Fe3 0.0120(2) 0.0108(2) 0.0094(2) -0.00109(16) 0.00407(18) 0.00086(18) O5W 0.0212(10) 0.0157(8) 0.0113(8) 0.0006(6) 0.0056(7) 0.0075(7) O6W 0.0134(8) 0.0161(8) 0.0164(8) 0.0042(7) 0.0062(7) 0.0022(7) O7W 0.0124(8) 0.0135(8) 0.0147(8) -0.0004(6) 0.0049(7) 0.0019(7) O8W 0.0219(10) 0.0172(9) 0.0202(9) 0.0014(7) 0.0057(8) -0.0031(8) O9W 0.0207(9) 0.0176(9) 0.0185(9) 0.0018(7) 0.0117(8) 0.0019(7) O10W 0.0194(9) 0.0148(8) 0.0187(9) -0.0040(7) 0.0106(8) -0.0023(7) O11W 0.0240(10) 0.0209(9) 0.0159(9) -0.0035(7) 0.0045(8) 0.0057(8) O12W 0.0256(10) 0.0235(10) 0.0153(9) -0.0019(7) 0.0083(8) -0.0061(8) O13W 0.0216(10) 0.0176(9) 0.0201(9) -0.0039(7) 0.0079(8) 0.0005(8) O14W 0.0347(12) 0.0310(11) 0.0325(12) 0.0143(9) 0.0201(10) 0.0150(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 Fe1 O1W 2.0880(17) . ? Fe1 O5 2.1025(16) . ? Fe1 O3 2.1039(17) . ? Fe1 O1 2.1599(16) . ? Fe1 O2W 2.1861(17) . ? Fe1 N1 2.2016(19) . ? O1W H1W1 0.80(2) . ? O1W H1W2 0.81(2) . ? O2W H2W1 0.81(2) . ? O2W H2W2 0.82(2) . ? Fe2 O4W 2.0742(17) . ? Fe2 O5 2.0943(16) . ? Fe2 O6 2.1127(16) . ? Fe2 O8 2.1260(16) . ? Fe2 O3W 2.1829(17) . ? Fe2 N2 2.2113(19) . ? O3W H3W1 0.82(2) . ? O3W H3W2 0.80(2) . ? O4W H4W1 0.83(2) . ? O4W H4W2 0.83(2) . ? C1 O2 1.248(3) . ? C1 O1 1.272(3) . ? C1 C2 1.519(3) . ? C2 N1 1.474(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.470(3) . ? C3 C4 1.526(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.244(3) . ? C4 O3 1.273(3) . ? C5 N1 1.495(3) . ? C5 C6 1.507(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.389(3) . ? C6 C11 1.409(3) . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 F1 1.370(2) . ? C8 C9 1.380(4) . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 C11 1.409(3) . ? C10 C12 1.506(3) . ? C11 O5 1.347(3) . ? C12 N2 1.482(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N2 1.479(3) . ? C13 C14 1.523(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O7 1.253(3) . ? C14 O6 1.272(3) . ? C15 N2 1.474(3) . ? C15 C16 1.526(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O9 1.243(3) . ? C16 O8 1.282(3) . ? Fe3 O5W 2.0778(16) 2_565 ? Fe3 O5W 2.0779(16) . ? Fe3 O6W 2.1065(17) 2_565 ? Fe3 O6W 2.1065(17) . ? Fe3 O7W 2.2035(16) . ? Fe3 O7W 2.2035(16) 2_565 ? O5W H5W1 0.84(2) . ? O5W H5W2 0.81(2) . ? O6W H6W1 0.82(2) . ? O6W H6W2 0.82(2) . ? O7W H7W1 0.81(2) . ? O7W H7W2 0.83(2) . ? O8W H8W1 0.83(2) . ? O8W H8W2 0.83(2) . ? O9W H9W1 0.85(2) . ? O9W H9W2 0.84(2) . ? O10W H0W3 0.82(2) . ? O10W H0W4 0.83(2) . ? O11W H1W3 0.81(2) . ? O11W H1W4 0.81(2) . ? O12W H2W3 0.83(2) . ? O12W H2W4 0.84(2) . ? O13W H3W3 0.84(2) . ? O13W H3W4 0.82(2) . ? O14W H4W3 0.83(2) . ? O14W H4W4 0.83(2) . ? 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 O1W Fe1 O5 87.33(7) . . ? O1W Fe1 O3 100.24(7) . . ? O5 Fe1 O3 101.99(6) . . ? O1W Fe1 O1 103.96(7) . . ? O5 Fe1 O1 91.78(6) . . ? O3 Fe1 O1 152.63(6) . . ? O1W Fe1 O2W 91.37(7) . . ? O5 Fe1 O2W 174.55(7) . . ? O3 Fe1 O2W 83.44(7) . . ? O1 Fe1 O2W 83.40(7) . . ? O1W Fe1 N1 178.33(7) . . ? O5 Fe1 N1 91.04(7) . . ? O3 Fe1 N1 79.73(7) . . ? O1 Fe1 N1 76.45(7) . . ? O2W Fe1 N1 90.29(7) . . ? Fe1 O1W H1W1 117(2) . . ? Fe1 O1W H1W2 122(2) . . ? H1W1 O1W H1W2 110(3) . . ? Fe1 O2W H2W1 122(2) . . ? Fe1 O2W H2W2 127(2) . . ? H2W1 O2W H2W2 109(3) . . ? O4W Fe2 O5 89.37(7) . . ? O4W Fe2 O6 96.02(7) . . ? O5 Fe2 O6 98.98(6) . . ? O4W Fe2 O8 108.10(7) . . ? O5 Fe2 O8 93.17(6) . . ? O6 Fe2 O8 153.09(6) . . ? O4W Fe2 O3W 89.68(7) . . ? O5 Fe2 O3W 177.17(7) . . ? O6 Fe2 O3W 83.77(7) . . ? O8 Fe2 O3W 84.60(7) . . ? O4W Fe2 N2 174.40(7) . . ? O5 Fe2 N2 91.30(7) . . ? O6 Fe2 N2 78.39(7) . . ? O8 Fe2 N2 77.41(7) . . ? O3W Fe2 N2 89.90(7) . . ? Fe2 O3W H3W1 129(2) . . ? Fe2 O3W H3W2 119(2) . . ? H3W1 O3W H3W2 110(3) . . ? Fe2 O4W H4W1 125(2) . . ? Fe2 O4W H4W2 117(2) . . ? H4W1 O4W H4W2 105(3) . . ? O2 C1 O1 124.5(2) . . ? O2 C1 C2 117.14(19) . . ? O1 C1 C2 118.2(2) . . ? N1 C2 C1 111.79(18) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 114.01(18) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.6 . . ? O4 C4 O3 125.1(2) . . ? O4 C4 C3 116.1(2) . . ? O3 C4 C3 118.7(2) . . ? N1 C5 C6 114.21(19) . . ? N1 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? N1 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C11 120.0(2) . . ? C7 C6 C5 120.7(2) . . ? C11 C6 C5 119.0(2) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? F1 C8 C7 119.1(2) . . ? F1 C8 C9 118.5(2) . . ? C7 C8 C9 122.5(2) . . ? C8 C9 C10 118.9(2) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 120.0(2) . . ? C9 C10 C12 120.7(2) . . ? C11 C10 C12 119.2(2) . . ? O5 C11 C6 120.4(2) . . ? O5 C11 C10 120.2(2) . . ? C6 C11 C10 119.4(2) . . ? N2 C12 C10 113.59(18) . . ? N2 C12 H12A 108.8 . . ? C10 C12 H12A 108.8 . . ? N2 C12 H12B 108.8 . . ? C10 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N2 C13 C14 113.29(18) . . ? N2 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N2 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? O7 C14 O6 124.3(2) . . ? O7 C14 C13 117.3(2) . . ? O6 C14 C13 118.4(2) . . ? N2 C15 C16 111.93(18) . . ? N2 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? N2 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O9 C16 O8 124.1(2) . . ? O9 C16 C15 117.7(2) . . ? O8 C16 C15 118.2(2) . . ? C3 N1 C2 113.05(17) . . ? C3 N1 C5 111.74(18) . . ? C2 N1 C5 108.28(18) . . ? C3 N1 Fe1 107.90(13) . . ? C2 N1 Fe1 106.29(14) . . ? C5 N1 Fe1 109.40(13) . . ? C15 N2 C13 113.03(17) . . ? C15 N2 C12 109.01(18) . . ? C13 N2 C12 111.68(18) . . ? C15 N2 Fe2 105.47(13) . . ? C13 N2 Fe2 108.65(13) . . ? C12 N2 Fe2 108.75(13) . . ? C1 O1 Fe1 114.30(14) . . ? C4 O3 Fe1 116.67(15) . . ? C11 O5 Fe2 114.62(14) . . ? C11 O5 Fe1 115.74(14) . . ? Fe2 O5 Fe1 129.58(7) . . ? C14 O6 Fe2 117.70(14) . . ? C16 O8 Fe2 114.50(14) . . ? O5W Fe3 O5W 180.00(10) 2_565 . ? O5W Fe3 O6W 92.18(7) 2_565 2_565 ? O5W Fe3 O6W 87.82(7) . 2_565 ? O5W Fe3 O6W 87.82(7) 2_565 . ? O5W Fe3 O6W 92.18(7) . . ? O6W Fe3 O6W 180.0 2_565 . ? O5W Fe3 O7W 87.40(6) 2_565 . ? O5W Fe3 O7W 92.61(6) . . ? O6W Fe3 O7W 90.09(7) 2_565 . ? O6W Fe3 O7W 89.91(7) . . ? O5W Fe3 O7W 92.60(6) 2_565 2_565 ? O5W Fe3 O7W 87.39(6) . 2_565 ? O6W Fe3 O7W 89.91(7) 2_565 2_565 ? O6W Fe3 O7W 90.09(7) . 2_565 ? O7W Fe3 O7W 180.00(9) . 2_565 ? Fe3 O5W H5W1 124(2) . . ? Fe3 O5W H5W2 121(2) . . ? H5W1 O5W H5W2 108(3) . . ? Fe3 O6W H6W1 119(2) . . ? Fe3 O6W H6W2 112(2) . . ? H6W1 O6W H6W2 110(3) . . ? Fe3 O7W H7W1 114(2) . . ? Fe3 O7W H7W2 119(2) . . ? H7W1 O7W H7W2 107(2) . . ? H8W1 O8W H8W2 106(3) . . ? H9W1 O9W H9W2 104(2) . . ? H0W3 O10W H0W4 106(3) . . ? H1W3 O11W H1W4 110(3) . . ? H2W3 O12W H2W4 106(3) . . ? H3W3 O13W H3W4 107(3) . . ? H4W3 O14W H4W4 105(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 N1 168.2(2) . . . . ? O1 C1 C2 N1 -14.8(3) . . . . ? N1 C3 C4 O4 -169.26(19) . . . . ? N1 C3 C4 O3 13.7(3) . . . . ? N1 C5 C6 C7 116.4(2) . . . . ? N1 C5 C6 C11 -68.9(3) . . . . ? C11 C6 C7 C8 -1.3(3) . . . . ? C5 C6 C7 C8 173.3(2) . . . . ? C6 C7 C8 F1 -179.9(2) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? F1 C8 C9 C10 -179.2(2) . . . . ? C7 C8 C9 C10 0.7(4) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? C8 C9 C10 C12 175.5(2) . . . . ? C7 C6 C11 O5 -179.4(2) . . . . ? C5 C6 C11 O5 5.9(3) . . . . ? C7 C6 C11 C10 1.4(3) . . . . ? C5 C6 C11 C10 -173.3(2) . . . . ? C9 C10 C11 O5 -179.6(2) . . . . ? C12 C10 C11 O5 4.2(3) . . . . ? C9 C10 C11 C6 -0.5(3) . . . . ? C12 C10 C11 C6 -176.6(2) . . . . ? C9 C10 C12 N2 114.5(2) . . . . ? C11 C10 C12 N2 -69.4(3) . . . . ? N2 C13 C14 O7 -171.83(19) . . . . ? N2 C13 C14 O6 11.0(3) . . . . ? N2 C15 C16 O9 167.6(2) . . . . ? N2 C15 C16 O8 -15.4(3) . . . . ? C4 C3 N1 C2 -135.6(2) . . . . ? C4 C3 N1 C5 101.9(2) . . . . ? C4 C3 N1 Fe1 -18.4(2) . . . . ? C1 C2 N1 C3 151.82(19) . . . . ? C1 C2 N1 C5 -83.8(2) . . . . ? C1 C2 N1 Fe1 33.6(2) . . . . ? C6 C5 N1 C3 -64.3(2) . . . . ? C6 C5 N1 C2 170.60(19) . . . . ? C6 C5 N1 Fe1 55.2(2) . . . . ? C16 C15 N2 C13 151.60(19) . . . . ? C16 C15 N2 C12 -83.6(2) . . . . ? C16 C15 N2 Fe2 33.0(2) . . . . ? C14 C13 N2 C15 -135.8(2) . . . . ? C14 C13 N2 C12 100.8(2) . . . . ? C14 C13 N2 Fe2 -19.1(2) . . . . ? C10 C12 N2 C15 170.86(18) . . . . ? C10 C12 N2 C13 -63.5(2) . . . . ? C10 C12 N2 Fe2 56.4(2) . . . . ? O2 C1 O1 Fe1 163.02(18) . . . . ? C2 C1 O1 Fe1 -13.8(3) . . . . ? O4 C4 O3 Fe1 -177.20(18) . . . . ? C3 C4 O3 Fe1 -0.4(3) . . . . ? C6 C11 O5 Fe2 -126.03(19) . . . . ? C10 C11 O5 Fe2 53.1(3) . . . . ? C6 C11 O5 Fe1 51.5(3) . . . . ? C10 C11 O5 Fe1 -129.37(19) . . . . ? O7 C14 O6 Fe2 -172.60(17) . . . . ? C13 C14 O6 Fe2 4.4(3) . . . . ? O9 C16 O8 Fe2 163.76(19) . . . . ? C15 C16 O8 Fe2 -13.0(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 O1W H1W1 O8 0.80(2) 2.00(2) 2.789(2) 168(3) . O1W H1W2 O9 0.81(2) 1.88(2) 2.693(2) 176(3) 2_776 O2W H2W1 O10W 0.81(2) 2.25(2) 2.931(3) 142(3) . O2W H2W1 O11W 0.81(2) 2.60(3) 3.167(3) 128(3) . O2W H2W2 O9W 0.82(2) 1.95(2) 2.765(3) 174(3) 2_665 O3W H3W1 O7W 0.82(2) 2.00(2) 2.818(2) 175(3) 2_666 O3W H3W2 O13W 0.80(2) 2.18(2) 2.875(3) 147(3) 2_766 O4W H4W1 O2 0.83(2) 1.87(2) 2.697(2) 174(3) 2_766 O4W H4W2 O1 0.83(2) 1.92(2) 2.733(2) 169(3) . O5W H5W1 O10W 0.84(2) 1.86(2) 2.687(2) 166(3) 1_455 O5W H5W2 O6 0.81(2) 1.89(2) 2.701(2) 174(3) 2_666 O6W H6W1 O12W 0.82(2) 1.90(2) 2.713(3) 172(3) 2_665 O6W H6W2 O7 0.82(2) 1.92(2) 2.728(2) 169(3) 2_666 O7W H7W1 O11W 0.81(2) 1.86(2) 2.679(2) 178(3) 2_665 O7W H7W2 O4 0.83(2) 2.00(2) 2.816(2) 165(3) 2_565 O8W H8W1 O3 0.83(2) 2.06(2) 2.881(2) 174(3) 1_545 O8W H8W2 O13W 0.83(2) 1.95(2) 2.761(3) 164(3) . O9W H9W1 O7 0.85(2) 1.90(2) 2.746(2) 177(3) 2_666 O9W H9W2 O8W 0.84(2) 2.02(2) 2.815(3) 157(3) . O10W H0W3 F1 0.82(2) 2.53(3) 2.989(2) 117(2) 1_655 O10W H0W4 O1 0.83(2) 2.10(2) 2.847(2) 150(3) . O11W H1W3 O14W 0.81(2) 1.91(2) 2.706(3) 166(3) 1_565 O11W H1W4 O9 0.81(2) 2.10(2) 2.883(2) 164(3) 2_776 O12W H2W3 O2 0.83(2) 2.05(2) 2.861(2) 164(3) . O12W H2W4 O9W 0.84(2) 1.99(2) 2.822(3) 174(3) . O13W H3W3 O2 0.84(2) 2.10(2) 2.889(2) 156(3) . O13W H3W3 F1 0.84(2) 2.50(3) 2.979(2) 118(3) 2_666 O13W H3W4 O8 0.82(2) 2.28(3) 2.967(3) 142(3) 2_766 O14W H4W3 O8W 0.83(2) 2.12(2) 2.907(3) 158(4) . O14W H4W4 O4 0.83(2) 1.98(2) 2.795(3) 168(4) 2_665 _refine_diff_density_max 0.932 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.066 _shelxl_version_number 2013-2 _shelx_res_file ; TITL xs0625a CELL 0.71073 10.8238 11.3967 13.4092 92.709 113.420 90.301 ZERR 1 0.0003 0.0003 0.0004 0.002 0.003 0.002 LATT 1 SFAC C H N O F FE UNIT 32 84 4 46 2 5 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 55 OMIT 1 -8 7 rem restraints DFIX 0.84 0.03 O1W H1W1 O1W H1W2 DFIX 1.33 0.03 H1W1 H1W2 DFIX 0.84 0.03 O2W H2W1 O2W H2W2 DFIX 1.33 0.03 H2W1 H2W2 DFIX 0.84 0.03 O3W H3W1 O3W H3W2 DFIX 1.33 0.03 H3W1 H3W2 DFIX 0.84 0.03 O4W H4W1 O4W H4W2 DFIX 1.33 0.03 H4W1 H4W2 DFIX 0.84 0.03 O5W H5W1 O5W H5W2 DFIX 1.33 0.03 H5W1 H5W2 DFIX 0.84 0.03 O6W H6W1 O6W H6W2 DFIX 1.33 0.03 H6W1 H6W2 DFIX 0.84 0.03 O7W H7W1 O7W H7W2 DFIX 1.33 0.03 H7W1 H7W2 DFIX 0.84 0.03 O8W H8W1 O8W H8W2 DFIX 1.33 0.03 H8W1 H8W2 DFIX 0.84 0.03 O9W H9W1 O9W H9W2 DFIX 1.33 0.03 H9W1 H9W2 DFIX 0.84 0.03 O10W H0W3 O10W H0W4 DFIX 1.33 0.03 H0W3 H0W4 DFIX 0.84 0.03 O11W H1W3 O11W H1W4 DFIX 1.33 0.03 H1W3 H1W4 DFIX 0.84 0.03 O12W H2W3 O12W H2W4 DFIX 1.33 0.03 H2W3 H2W4 DFIX 0.84 0.03 O13W H3W3 O13W H3W4 DFIX 1.33 0.03 H3W3 H3W4 DFIX 0.84 0.03 O14W H4W3 O14W H4W4 DFIX 1.33 0.03 H4W3 H4W4 EQIV $1 -x+2, -y+2, -z+1 EQIV $2 -x+1, -y+1, -z EQIV $3 -x+1, -y+1, -z+1 EQIV $4 -x+2, -y+1, -z+1 EQIV $6 x-1, y, z EQIV $8 -x, -y+1, -z EQIV $10 x, y-1, z EQIV $12 x+1, y, z EQIV $13 x, y+1, z HTAB O1W O8 HTAB O1W O9_$1 HTAB O2W O10W HTAB O2W O11W HTAB O2W O9W_$2 HTAB O3W O7W_$3 HTAB O3W O13W_$4 HTAB O4W O2_$4 HTAB O4W O1 HTAB O5W O10W_$6 HTAB O5W O6_$3 HTAB O6W O12W_$2 HTAB O6W O7_$3 HTAB O7W O11W_$2 HTAB O7W O4_$8 HTAB O8W O3_$10 HTAB O8W O13W HTAB O9W O7_$3 HTAB O9W O8W HTAB O10W F1_$12 HTAB O10W O1 HTAB O11W O14W_$13 HTAB O11W O9_$1 HTAB O12W O2 HTAB O12W O9W HTAB O13W O2 HTAB O13W F1_$3 HTAB O13W O8_$4 HTAB O14W O8W HTAB O14W O4_$2 TWIN 1 0 0 0 -1 0 -1 0 -1 WGHT 0.022300 2.022600 BASF 0.13306 FVAR 5.38349 PART 0 rem Fe1-Fe2 complex FE1 6 0.681994 0.744475 0.337739 11.00000 0.01022 0.00933 = 0.00851 -0.00153 0.00312 0.00031 O1W 4 0.821592 0.884819 0.390564 11.00000 0.01824 0.02207 = 0.01247 -0.00523 0.00825 -0.00734 H1W1 2 0.849694 0.905664 0.453877 11.00000 -1.50000 H1W2 2 0.881281 0.890995 0.368459 11.00000 -1.50000 O2W 4 0.705492 0.724599 0.183310 11.00000 0.01320 0.02885 = 0.01207 0.00142 0.00586 0.00539 H2W1 2 0.777140 0.711565 0.180170 11.00000 -1.50000 H2W2 2 0.653209 0.745799 0.123740 11.00000 -1.50000 FE2 6 0.836553 0.765042 0.646754 11.00000 0.01096 0.00854 = 0.00850 -0.00141 0.00389 0.00045 O3W 4 1.009176 0.777761 0.803187 11.00000 0.01292 0.02581 = 0.01174 0.00240 0.00400 -0.00307 H3W1 2 1.019049 0.747816 0.860320 11.00000 -1.50000 H3W2 2 1.079973 0.801064 0.806068 11.00000 -1.50000 O4W 4 0.922908 0.623653 0.597896 11.00000 0.01484 0.02274 = 0.01145 -0.00477 0.00115 0.00763 H4W1 2 1.004606 0.609196 0.623629 11.00000 -1.50000 H4W2 2 0.896450 0.608374 0.531445 11.00000 -1.50000 C1 1 0.748379 0.498381 0.318963 11.00000 0.01305 0.01395 = 0.00750 0.00058 0.00407 0.00051 C2 1 0.597480 0.498623 0.252022 11.00000 0.01181 0.01172 = 0.01418 -0.00522 0.00297 0.00026 AFIX 23 H2A 2 0.580579 0.504001 0.174219 11.00000 -1.20000 H2B 2 0.556339 0.423743 0.259953 11.00000 -1.20000 AFIX 0 C3 1 0.411272 0.636382 0.197752 11.00000 0.01026 0.01299 = 0.01141 -0.00204 0.00203 -0.00044 AFIX 23 H3A 2 0.331482 0.605800 0.207862 11.00000 -1.20000 H3B 2 0.408298 0.601687 0.127715 11.00000 -1.20000 AFIX 0 C4 1 0.402169 0.769569 0.191122 11.00000 0.01341 0.01573 = 0.00970 -0.00059 0.00708 0.00154 C5 1 0.505398 0.562298 0.381342 11.00000 0.01249 0.01287 = 0.01146 -0.00015 0.00457 -0.00132 AFIX 23 H5A 2 0.587984 0.529181 0.435288 11.00000 -1.20000 H5B 2 0.434654 0.499394 0.356348 11.00000 -1.20000 AFIX 0 C6 1 0.460538 0.661246 0.436689 11.00000 0.01175 0.01375 = 0.00940 0.00179 0.00349 0.00001 C7 1 0.333050 0.658510 0.438262 11.00000 0.01306 0.01801 = 0.01029 0.00213 0.00227 -0.00120 AFIX 43 H7 2 0.269221 0.598379 0.397912 11.00000 -1.20000 AFIX 0 C8 1 0.300160 0.744065 0.499057 11.00000 0.00833 0.02505 = 0.01267 0.00448 0.00441 0.00268 C9 1 0.389356 0.833328 0.558704 11.00000 0.01450 0.01985 = 0.01080 0.00265 0.00663 0.00547 AFIX 43 H9 2 0.364186 0.890544 0.600516 11.00000 -1.20000 AFIX 0 C10 1 0.517258 0.838103 0.556546 11.00000 0.01421 0.01361 = 0.00990 0.00164 0.00495 0.00177 C11 1 0.553676 0.752048 0.494997 11.00000 0.00953 0.01297 = 0.00867 0.00249 0.00257 0.00187 C12 1 0.614209 0.938772 0.613646 11.00000 0.01457 0.01112 = 0.01198 0.00008 0.00590 0.00303 AFIX 23 H12A 2 0.642192 0.975925 0.560393 11.00000 -1.20000 H12B 2 0.567153 0.998408 0.640697 11.00000 -1.20000 AFIX 0 C13 1 0.702283 0.856463 0.793525 11.00000 0.01694 0.01332 = 0.00995 -0.00035 0.00761 0.00065 AFIX 23 H13A 2 0.612595 0.884470 0.785614 11.00000 -1.20000 H13B 2 0.768843 0.888025 0.864848 11.00000 -1.20000 AFIX 0 C14 1 0.700624 0.722730 0.792461 11.00000 0.00768 0.01360 = 0.00813 0.00083 0.00025 -0.00088 C15 1 0.833167 1.003382 0.744477 11.00000 0.01717 0.01150 = 0.01495 -0.00376 0.00929 -0.00238 AFIX 23 H15A 2 0.893305 0.994732 0.821696 11.00000 -1.20000 H15B 2 0.783693 1.077088 0.740064 11.00000 -1.20000 AFIX 0 C16 1 0.918066 1.011633 0.677295 11.00000 0.01236 0.01264 = 0.00949 -0.00012 0.00224 0.00042 N1 3 0.533442 0.597513 0.286247 11.00000 0.00978 0.01152 = 0.00863 -0.00070 0.00250 0.00146 N2 3 0.736105 0.903297 0.706243 11.00000 0.01248 0.00854 = 0.01062 -0.00110 0.00535 -0.00077 O1 4 0.804828 0.590817 0.376337 11.00000 0.01203 0.01269 = 0.01040 -0.00182 0.00271 0.00065 O2 4 0.809166 0.408423 0.309914 11.00000 0.01510 0.01405 = 0.01654 -0.00336 0.00412 0.00271 O3 4 0.506958 0.833028 0.244576 11.00000 0.01211 0.01104 = 0.01392 0.00004 0.00385 0.00093 O4 4 0.291974 0.807077 0.128979 11.00000 0.01211 0.01703 = 0.01550 0.00100 0.00274 0.00420 O5 4 0.677124 0.755859 0.493081 11.00000 0.00960 0.01399 = 0.00924 -0.00127 0.00395 0.00018 O6 4 0.747690 0.666488 0.731676 11.00000 0.01420 0.01160 = 0.01338 -0.00002 0.00705 0.00110 O7 4 0.657602 0.675589 0.855388 11.00000 0.01469 0.01639 = 0.01529 0.00252 0.00805 -0.00035 O8 4 0.919281 0.922126 0.616152 11.00000 0.01562 0.01090 = 0.01182 -0.00290 0.00759 -0.00124 O9 4 0.986291 1.103246 0.688993 11.00000 0.01832 0.01229 = 0.01698 -0.00319 0.00934 -0.00433 F1 5 0.174374 0.740932 0.500587 11.00000 0.01019 0.03767 = 0.01881 -0.00129 0.00816 -0.00071 rem cation FE3 6 0.000000 0.500000 0.000000 10.50000 0.01204 0.01081 = 0.00936 -0.00109 0.00407 0.00086 O5W 4 0.092981 0.510760 0.168895 11.00000 0.02118 0.01565 = 0.01128 0.00060 0.00559 0.00753 H5W1 2 0.059576 0.544644 0.208897 11.00000 -1.50000 H5W2 2 0.139259 0.458449 0.202273 11.00000 -1.50000 O6W 4 0.182437 0.462309 -0.014869 11.00000 0.01338 0.01614 = 0.01644 0.00418 0.00624 0.00217 H6W1 2 0.222279 0.514693 -0.030645 11.00000 -1.50000 H6W2 2 0.234855 0.428861 0.037629 11.00000 -1.50000 O7W 4 -0.044620 0.310373 -0.005410 11.00000 0.01235 0.01347 = 0.01475 -0.00040 0.00495 0.00190 H7W1 2 0.001369 0.269315 -0.027675 11.00000 -1.50000 H7W2 2 -0.123894 0.285303 -0.037664 11.00000 -1.50000 O8W 4 0.578779 0.022883 0.141858 11.00000 0.02188 0.01721 = 0.02021 0.00143 0.00573 -0.00305 H8W1 2 0.554174 -0.033387 0.166898 11.00000 -1.50000 H8W2 2 0.641135 0.057231 0.193940 11.00000 -1.50000 O9W 4 0.469752 0.221520 0.023294 11.00000 0.02074 0.01759 = 0.01851 0.00181 0.01169 0.00185 H9W1 2 0.429852 0.250834 0.061251 11.00000 -1.50000 H9W2 2 0.484581 0.152441 0.043474 11.00000 -1.50000 O10W 4 0.985653 0.650451 0.278878 11.00000 0.01937 0.01476 = 0.01867 -0.00403 0.01057 -0.00235 H0W3 2 1.020402 0.715520 0.301434 11.00000 -1.50000 H0W4 2 0.960785 0.627040 0.325869 11.00000 -1.50000 O11W 4 0.899367 0.828091 0.082038 11.00000 0.02397 0.02088 = 0.01591 -0.00351 0.00448 0.00569 H1W3 2 0.863009 0.888809 0.058477 11.00000 -1.50000 H1W4 2 0.937916 0.834690 0.147449 11.00000 -1.50000 O12W 4 0.709928 0.356182 0.080209 11.00000 0.02555 0.02352 = 0.01532 -0.00187 0.00826 -0.00609 H2W3 2 0.745760 0.358285 0.147656 11.00000 -1.50000 H2W4 2 0.641470 0.311944 0.061611 11.00000 -1.50000 O13W 4 0.798274 0.155020 0.283373 11.00000 0.02160 0.01762 = 0.02013 -0.00388 0.00792 0.00050 H3W3 2 0.793527 0.224386 0.305411 11.00000 -1.50000 H3W4 2 0.859985 0.124692 0.332017 11.00000 -1.50000 O14W 4 0.760055 0.028424 0.030011 11.00000 0.03471 0.03096 = 0.03249 0.01433 0.02012 0.01498 H4W3 2 0.692621 0.022212 0.044347 11.00000 -1.50000 H4W4 2 0.736223 0.069574 -0.023406 11.00000 -1.50000 HKLF 4 REM xs0625a REM R1 = 0.0310 for 6627 Fo > 4sig(Fo) and 0.0339 for all 6967 data REM 488 parameters refined using 42 restraints END WGHT 0.0224 2.0223 REM Instructions for potential hydrogen bonds HTAB O1W O8 HTAB O1W O9_$1 HTAB O2W O10W HTAB O2W O11W HTAB O2W O9W_$2 HTAB O3W O7W_$3 HTAB O3W O13W_$4 HTAB O4W O2_$4 HTAB O4W O1 HTAB C2 O7_$3 HTAB C3 O5W HTAB C3 O12W_$2 HTAB C5 O6_$3 EQIV $14 -x+1, -y+2, -z+1 HTAB C15 O4_$14 HTAB O5W O10W_$6 HTAB O5W O6_$3 HTAB O6W O12W_$2 HTAB O6W O7_$3 HTAB O7W O11W_$2 HTAB O7W O4_$8 HTAB O8W O3_$10 HTAB O8W O13W HTAB O9W O7_$3 HTAB O9W O8W HTAB O10W O9_$1 HTAB O10W F1_$12 HTAB O10W O1 HTAB O11W O14W_$13 HTAB O11W O9_$1 HTAB O12W O2 HTAB O12W O9W HTAB O13W O2 HTAB O13W F1_$3 HTAB O13W O8_$4 HTAB O14W O8W HTAB O14W O4_$2 REM Highest difference peak 0.932, deepest hole -0.618, 1-sigma level 0.066 Q1 1 0.5000 0.0000 0.0000 10.50000 0.05 0.93 Q2 1 0.6195 0.7217 0.3604 11.00000 0.05 0.43 Q3 1 0.7176 0.6757 0.3821 11.00000 0.05 0.37 Q4 1 0.7662 0.7337 0.6640 11.00000 0.05 0.37 Q5 1 0.4770 0.6185 0.4010 11.00000 0.05 0.36 Q6 1 0.8770 1.0056 0.7140 11.00000 0.05 0.35 Q7 1 0.7408 0.7390 0.3189 11.00000 0.05 0.32 Q8 1 0.4997 0.7155 0.4552 11.00000 0.05 0.30 Q9 1 0.5679 0.8774 0.5844 11.00000 0.05 0.30 Q10 1 0.4094 0.6988 0.1955 11.00000 0.05 0.30 ; _shelx_res_checksum 48656 _shelx_hkl_file ; 0 0 -1 129900. 1311.19 1 0 0 2 71704.1 1305.18 7 0 0 2 71744.2 1117.98 6 0 0 -2 73845.3 1397.25 1 0 0 -2 69378.2 1123.33 6 0 0 -3 350275. 2999.70 6 0 0 3 340521. 3495.00 7 0 0 3 337275. 2991.10 6 0 0 -3 348917. 3736.11 1 0 0 4 2040.20 278.927 6 0 0 -4 1897.48 282.637 6 0 0 -4 2041.61 340.942 1 0 0 4 2039.95 319.375 7 0 0 -5 20018.6 1161.60 1 0 0 5 19464.2 1171.77 1 0 0 5 20809.8 1112.16 7 0 0 5 19372.9 898.687 6 0 0 -5 20218.2 951.445 6 0 0 6 395037. 5347.68 7 0 0 6 379561. 5696.57 1 0 0 -6 388302. 5602.69 1 0 0 6 390564. 4441.59 6 0 0 -6 393958. 4514.90 6 0 0 7 3626.62 615.881 1 0 0 7 2541.55 468.806 7 0 0 7 3283.36 454.109 6 0 0 -7 3721.39 604.739 1 0 0 -7 3022.05 449.511 6 0 0 8 34127.4 1514.95 6 0 0 -8 33564.9 1923.99 1 0 0 -8 32646.6 1524.28 6 0 0 -8 32922.6 1793.80 7 0 0 8 32458.2 1962.34 1 0 0 -9 3888.39 705.128 7 0 0 9 4653.86 799.677 1 0 0 9 3723.36 536.838 6 0 0 10 8091.89 1126.09 1 0 0 10 7392.46 791.514 6 0 0 -10 7283.85 1013.77 7 0 0 -10 7729.31 843.931 5 0 0 -11 21625.3 1470.50 5 0 0 11 22032.2 1926.37 1 0 0 -11 21007.3 1743.35 7 0 0 11 20868.1 1382.77 6 0 0 12 25061.4 1932.74 4 0 0 -12 26573.5 1699.15 5 0 0 -12 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11362.8 1204.19 7 2 -5 -9 1671.94 489.362 6 2 -5 -9 1838.68 443.017 7 -2 5 9 1296.74 446.607 3 -2 5 9 2075.56 624.022 4 2 -5 -8 1047.43 474.473 6 -2 5 8 642.695 387.413 4 -2 5 8 538.171 292.119 3 2 -5 -8 668.211 279.977 7 -2 5 7 11808.4 1173.56 3 2 -5 -7 13679.5 1308.14 6 -2 5 7 14235.6 1103.42 7 -2 5 7 12807.4 1218.76 4 2 -5 -7 12528.7 1033.63 7 -2 5 6 2067.85 459.740 4 2 -5 -6 2737.67 565.815 1 2 -5 -6 1834.25 452.026 6 -2 5 6 2291.66 489.666 3 2 -5 -6 2255.77 399.871 7 -2 5 6 1968.46 385.581 7 -2 5 6 2164.94 490.490 6 2 -5 -5 3312.60 572.446 3 -2 5 5 5610.03 721.395 4 -2 5 5 5015.59 703.659 6 -2 5 5 5329.59 563.544 7 2 -5 -5 3425.30 450.671 7 2 -5 -5 4311.94 684.317 1 2 -5 -4 27953.6 1117.13 7 2 -5 -4 28830.4 1616.70 3 -2 5 4 27128.3 1540.02 6 -2 5 4 26234.4 1417.24 4 -2 5 4 25726.3 1081.38 7 2 -5 -3 61117.3 2294.32 6 -2 5 3 67700.2 2117.79 4 -2 5 3 63889.7 2307.13 6 2 -5 -3 51231.8 1328.99 7 2 -5 -3 50927.6 2059.47 3 2 -5 -2 303092. 2427.20 7 -2 5 2 291263. 4586.60 6 2 -5 -2 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2898.36 6 -2 4 13 40241.1 2857.19 3 -2 4 13 47359.0 3007.19 1 -2 4 13 46415.7 3035.67 4 2 -4 -12 5492.37 992.579 5 -2 4 12 5795.84 1052.50 4 2 -4 -12 5425.73 1013.88 6 -2 4 12 5507.82 989.609 1 2 -4 -12 4419.42 880.062 7 -2 4 12 4902.37 970.384 3 -2 4 11 8475.35 1204.26 3 -2 4 11 9765.15 1235.38 1 2 -4 -11 9194.81 1136.77 7 2 -4 -11 11279.7 1310.33 6 2 -4 -10 85776.0 3268.29 7 -2 4 10 83097.8 3537.42 3 2 -4 -10 87117.6 3538.30 6 -2 4 10 86461.3 3494.14 1 2 -4 -9 2502.37 504.678 7 -2 4 9 2379.73 601.876 3 2 -4 -9 1703.17 536.499 6 2 -4 -8 17359.2 1460.75 6 -2 4 8 16948.3 1444.87 3 2 -4 -8 16459.6 1266.97 7 -2 4 8 17891.4 1305.94 7 2 -4 -7 268889. 4687.79 7 2 -4 -7 278207. 5551.71 6 2 -4 -7 286133. 5549.33 1 -2 4 7 274866. 4764.99 7 -2 4 7 267010. 5314.38 3 -2 4 7 280339. 5433.66 6 2 -4 -6 55639.6 1966.26 7 -2 4 6 55133.2 2314.24 6 -2 4 6 53696.0 1936.59 7 2 -4 -6 59173.5 2374.81 1 -2 4 5 2297.36 367.987 7 2 -4 -5 2463.88 366.702 7 2 -4 -5 3369.67 540.258 1 2 -4 -5 2698.90 493.988 3 -2 4 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546.844 370.560 3 8 -8 -1 146078. 4918.01 1 8 -8 -1 155315. 3577.49 5 -8 8 1 154269. 5262.30 3 8 -8 0 46276.8 2846.43 1 8 -8 0 47350.5 1799.92 5 -8 8 0 48745.1 3006.98 3 8 -8 1 63767.7 3466.96 1 -8 8 -1 59151.1 3375.97 3 8 -8 2 4904.88 1030.62 1 8 -8 3 948.742 496.280 1 8 -8 4 19966.9 2188.81 1 8 -8 5 9398.25 1578.14 1 8 -8 6 231.475 221.431 1 -8 7 14 15406.9 1618.53 2 8 -7 -14 13278.5 1580.79 7 -8 7 14 13669.6 1757.48 3 8 -7 -14 14252.3 1788.24 5 -8 7 13 5280.08 940.175 2 8 -7 -13 5389.88 974.957 7 -8 7 13 4643.08 1090.57 3 8 -7 -13 5297.33 1112.97 5 -8 7 12 7668.48 1049.71 2 8 -7 -12 8589.07 1172.68 7 -8 7 12 8346.53 1323.99 3 8 -7 -12 10209.1 1451.36 5 -8 7 11 19136.4 1560.61 2 8 -7 -11 19479.9 1667.66 7 -8 7 11 19825.4 1945.06 3 8 -7 -11 18161.9 1845.66 5 -8 7 10 2048.24 484.612 2 8 -7 -10 2029.53 539.556 7 -8 7 10 2478.79 688.795 3 8 -7 -10 2465.48 670.700 5 -8 7 9 11672.7 1088.53 2 8 -7 -9 10855.3 1100.60 7 -8 7 9 10613.4 1347.66 3 8 -7 -9 11209.5 1342.54 5 -8 7 8 6357.28 786.523 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