# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mark Weller' _publ_contact_author_email MTW@SOTON.AC.UK loop_ _publ_author_name M.Weller K.V.Redrup # Attachment 'Fe2O(HPO4).cif' data_2007kvb0053 _database_code_depnum_ccdc_archive 'CCDC 713718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Fe4 O10 P2' _chemical_formula_weight 447.36 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.927(3) _cell_length_b 6.5566(13) _cell_length_c 9.6670(19) _cell_angle_alpha 90.00 _cell_angle_beta 116.48(3) _cell_angle_gamma 90.00 _cell_volume 733.4(3) _cell_formula_units_Z 4 _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 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 8.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7340 _exptl_absorpt_correction_T_max 0.9221 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _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 3363 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.79 _reflns_number_total 1451 _reflns_number_gt 1047 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+32.8997P] 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 0.39(11) _refine_ls_number_reflns 1451 _refine_ls_number_parameters 85 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 1.073 _refine_ls_shift/su_mean 0.032 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 O1 O 0.0293(16) 0.792(3) 0.628(2) 0.003(4) Uiso 1 1 d . . . O2 O -0.208(2) 0.719(3) 0.358(3) 0.016(5) Uiso 1 1 d . . . O3 O -0.0611(12) 1.161(2) 0.7774(18) 0.000(3) Uiso 1 1 d . . . O4 O -0.1527(14) 1.068(3) 0.409(2) 0.012(4) Uiso 1 1 d . . . O5 O -0.1298(16) 0.645(3) 0.686(2) 0.019(5) Uiso 1 1 d . . . O6 O 0.2350(14) 0.529(3) 0.642(2) 0.013(5) Uiso 1 1 d . . . O7 O 0.0799(14) 0.447(3) 0.347(2) 0.007(4) Uiso 1 1 d . . . O8 O -0.0410(13) 1.424(3) 0.567(2) 0.007(4) Uiso 1 1 d . . . O9 O 0.2103(10) 0.9225(18) 0.4841(15) 0.015(3) Uiso 1 1 d . . . O10 O 0.1575(9) 1.1939(16) 0.6733(12) 0.007(2) Uiso 1 1 d . . . Fe1 Fe 0.0024(3) 1.1053(7) 0.6188(5) 0.0132(11) Uani 1 1 d . . . Fe2 Fe 0.3185(3) 1.1052(7) 0.8640(5) 0.0122(11) Uani 1 1 d . . . Fe3 Fe 0.0999(4) 0.7263(7) 0.4763(6) 0.0163(12) Uani 1 1 d . . . Fe4 Fe 0.2217(4) 1.2747(7) 0.5049(5) 0.0144(11) Uani 1 1 d . . . P1 P 0.3323(6) 1.6027(12) 0.7968(10) 0.0062(17) Uiso 1 1 d . . . P6 P -0.0131(6) 0.6020(12) 0.6854(10) 0.0076(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.024(3) 0.005(3) 0.014(3) -0.006(2) 0.011(2) -0.003(2) Fe2 0.018(2) 0.009(3) 0.011(3) -0.002(2) 0.008(2) -0.001(2) Fe3 0.012(2) 0.021(3) 0.013(3) -0.001(2) 0.003(2) 0.013(2) Fe4 0.017(2) 0.021(3) 0.004(2) -0.003(2) 0.0036(19) 0.008(2) _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 O1 P6 1.56(2) . ? O1 Fe1 2.078(18) . ? O1 Fe3 2.09(2) . ? O2 P1 1.50(2) 4_474 ? O2 Fe4 2.03(2) 3_445 ? O2 Fe2 2.15(2) 4_464 ? O3 P1 1.519(16) 3_445 ? O3 Fe1 2.070(16) . ? O3 Fe3 2.238(15) 2_575 ? O4 P1 1.51(2) 4_474 ? O4 Fe1 2.135(17) . ? O4 Fe2 2.19(2) 4_474 ? O5 P6 1.54(2) . ? O5 Fe4 2.12(2) 3_445 ? O5 Fe2 2.12(2) 3_445 ? O6 P1 1.54(2) 1_545 ? O6 Fe4 2.090(19) 1_545 ? O6 Fe3 2.191(18) . ? O7 P6 1.52(2) 2_564 ? O7 Fe4 2.113(18) 1_545 ? O7 Fe3 2.164(19) . ? O8 P6 1.56(2) 1_565 ? O8 Fe2 2.002(16) 4_474 ? O8 Fe1 2.164(19) . ? O9 Fe3 1.897(13) . ? O9 Fe2 2.186(13) 2_574 ? O9 Fe4 2.317(12) . ? O10 Fe1 1.921(11) . ? O10 Fe2 2.156(12) . ? O10 Fe4 2.196(11) . ? Fe2 O8 2.002(16) 4_575 ? Fe2 O5 2.12(2) 3 ? Fe2 O2 2.15(2) 4_565 ? Fe2 O4 2.19(2) 4_575 ? Fe2 O9 2.186(13) 2_575 ? Fe3 O3 2.238(15) 2_574 ? Fe4 O2 2.03(2) 3 ? Fe4 O6 2.090(19) 1_565 ? Fe4 O7 2.113(18) 1_565 ? Fe4 O5 2.12(2) 3 ? P1 O2 1.50(2) 4_575 ? P1 O4 1.51(2) 4_575 ? P1 O3 1.519(16) 3 ? P1 O6 1.54(2) 1_565 ? P6 O7 1.52(2) 2_565 ? P6 O8 1.56(2) 1_545 ? 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 P6 O1 Fe1 136.4(12) . . ? P6 O1 Fe3 114.8(11) . . ? Fe1 O1 Fe3 107.0(9) . . ? P1 O2 Fe4 118.6(13) 4_474 3_445 ? P1 O2 Fe2 134.2(15) 4_474 4_464 ? Fe4 O2 Fe2 105.9(11) 3_445 4_464 ? P1 O3 Fe1 136.8(10) 3_445 . ? P1 O3 Fe3 121.6(10) 3_445 2_575 ? Fe1 O3 Fe3 99.8(6) . 2_575 ? P1 O4 Fe1 122.2(11) 4_474 . ? P1 O4 Fe2 128.7(12) 4_474 4_474 ? Fe1 O4 Fe2 94.6(8) . 4_474 ? P6 O5 Fe4 126.9(13) . 3_445 ? P6 O5 Fe2 130.2(13) . 3_445 ? Fe4 O5 Fe2 102.9(8) 3_445 3_445 ? P1 O6 Fe4 131.8(10) 1_545 1_545 ? P1 O6 Fe3 124.4(10) 1_545 . ? Fe4 O6 Fe3 101.1(8) 1_545 . ? P6 O7 Fe4 131.4(11) 2_564 1_545 ? P6 O7 Fe3 127.4(10) 2_564 . ? Fe4 O7 Fe3 101.3(8) 1_545 . ? P6 O8 Fe2 127.1(11) 1_565 4_474 ? P6 O8 Fe1 127.0(11) 1_565 . ? Fe2 O8 Fe1 99.4(7) 4_474 . ? Fe3 O9 Fe2 124.8(6) . 2_574 ? Fe3 O9 Fe4 134.1(6) . . ? Fe2 O9 Fe4 95.6(5) 2_574 . ? Fe1 O10 Fe2 130.1(6) . . ? Fe1 O10 Fe4 124.2(5) . . ? Fe2 O10 Fe4 99.2(4) . . ? O10 Fe1 O3 117.0(6) . . ? O10 Fe1 O1 98.8(7) . . ? O3 Fe1 O1 105.0(7) . . ? O10 Fe1 O4 136.0(6) . . ? O3 Fe1 O4 102.0(7) . . ? O1 Fe1 O4 89.6(8) . . ? O10 Fe1 O8 84.4(5) . . ? O3 Fe1 O8 81.6(6) . . ? O1 Fe1 O8 170.1(8) . . ? O4 Fe1 O8 81.7(7) . . ? O8 Fe2 O5 109.3(7) 4_575 3 ? O8 Fe2 O2 89.8(9) 4_575 4_565 ? O5 Fe2 O2 101.8(8) 3 4_565 ? O8 Fe2 O10 166.4(6) 4_575 . ? O5 Fe2 O10 78.8(6) 3 . ? O2 Fe2 O10 99.3(7) 4_565 . ? O8 Fe2 O4 84.2(7) 4_575 4_575 ? O5 Fe2 O4 87.4(7) 3 4_575 ? O2 Fe2 O4 170.3(9) 4_565 4_575 ? O10 Fe2 O4 85.4(6) . 4_575 ? O8 Fe2 O9 89.3(6) 4_575 2_575 ? O5 Fe2 O9 161.4(6) 3 2_575 ? O2 Fe2 O9 78.4(7) 4_565 2_575 ? O10 Fe2 O9 82.8(5) . 2_575 ? O4 Fe2 O9 93.8(6) 4_575 2_575 ? O9 Fe3 O1 112.9(7) . . ? O9 Fe3 O7 119.4(6) . . ? O1 Fe3 O7 126.9(7) . . ? O9 Fe3 O6 91.8(6) . . ? O1 Fe3 O6 93.7(8) . . ? O7 Fe3 O6 76.9(6) . . ? O9 Fe3 O3 101.9(6) . 2_574 ? O1 Fe3 O3 90.2(7) . 2_574 ? O7 Fe3 O3 87.6(6) . 2_574 ? O6 Fe3 O3 163.1(7) . 2_574 ? O2 Fe4 O6 130.7(8) 3 1_565 ? O2 Fe4 O7 96.0(8) 3 1_565 ? O6 Fe4 O7 80.2(6) 1_565 1_565 ? O2 Fe4 O5 89.1(9) 3 3 ? O6 Fe4 O5 90.4(7) 1_565 3 ? O7 Fe4 O5 170.6(8) 1_565 3 ? O2 Fe4 O10 155.5(7) 3 . ? O6 Fe4 O10 70.9(6) 1_565 . ? O7 Fe4 O10 99.8(5) 1_565 . ? O5 Fe4 O10 78.1(6) 3 . ? O2 Fe4 O9 77.9(7) 3 . ? O6 Fe4 O9 146.6(7) 1_565 . ? O7 Fe4 O9 118.0(6) 1_565 . ? O5 Fe4 O9 70.8(6) 3 . ? O10 Fe4 O9 78.1(5) . . ? O2 P1 O4 104.3(13) 4_575 4_575 ? O2 P1 O3 110.4(11) 4_575 3 ? O4 P1 O3 116.3(11) 4_575 3 ? O2 P1 O6 110.3(12) 4_575 1_565 ? O4 P1 O6 104.7(11) 4_575 1_565 ? O3 P1 O6 110.6(11) 3 1_565 ? O7 P6 O5 111.1(12) 2_565 . ? O7 P6 O8 114.5(11) 2_565 1_545 ? O5 P6 O8 103.5(11) . 1_545 ? O7 P6 O1 107.1(10) 2_565 . ? O5 P6 O1 110.8(11) . . ? O8 P6 O1 109.7(12) 1_545 . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.586 _refine_diff_density_min -1.335 _refine_diff_density_rms 0.374 # Attachment 'Fe3(HPO4)6(NH4)2(NH4).cif' data_2007kvb0051 _database_code_depnum_ccdc_archive 'CCDC 713719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H Fe N0 O P' _chemical_formula_weight 115.84 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1290(3) _cell_length_b 8.8372(3) _cell_length_c 9.4621(3) _cell_angle_alpha 64.649(2) _cell_angle_beta 70.328(2) _cell_angle_gamma 69.541(2) _cell_volume 492.27(3) _cell_formula_units_Z 5 _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 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 4.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5013 _exptl_absorpt_correction_T_max 0.8248 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _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 5764 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.58 _reflns_number_total 2240 _reflns_number_gt 2072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0068P)^2^+1.3200P] 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_number_reflns 2240 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 3.817 _refine_ls_shift/su_mean 0.082 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 O1 O 0.1587(3) 0.7611(2) 0.1124(2) 0.0067(4) Uani 1 1 d . . . O2 O 0.2635(3) 1.0414(2) -0.1422(2) 0.0086(4) Uani 1 1 d . . . O3 O 0.4053(3) 0.8730(3) 0.2391(2) 0.0099(4) Uani 1 1 d . . . O4 O 0.0557(3) 1.0867(2) 0.1467(2) 0.0080(4) Uani 1 1 d . . . O5 O -0.1056(3) 0.5858(3) 0.2502(2) 0.0093(4) Uani 1 1 d . . . O6 O 0.0260(3) 0.6819(2) 0.4099(2) 0.0079(4) Uani 1 1 d . . . O7 O 0.4353(3) 0.1257(2) 0.2857(2) 0.0069(4) Uani 1 1 d . . . O8 O -0.2815(3) 1.2970(2) 0.2146(2) 0.0083(4) Uani 1 1 d . . . O9 O 0.0146(3) 0.2589(2) 0.3105(2) 0.0076(4) Uani 1 1 d . . . O10 O 0.1671(3) -0.0173(2) 0.5720(2) 0.0073(4) Uani 1 1 d . . . O11 O 0.4048(3) 0.1884(2) 0.5636(2) 0.0073(4) Uani 1 1 d . . . O12 O 0.2540(3) 0.4537(2) 0.2942(2) 0.0066(4) Uani 1 1 d . . . N1 N 0.3811(5) 1.3349(4) -0.0311(3) 0.0141(5) Uani 1 1 d . . . N2 N 0.5000 0.5000 0.5000 0.0195(10) Uani 1 2 d S . . H1 H -0.084(5) 0.500(5) 0.267(4) 0.008(9) Uiso 1 1 d . . . H2 H 0.514(8) 1.299(6) -0.064(6) 0.050 Uiso 1 1 d . . . H3 H 0.340(7) 1.297(6) 0.079(6) 0.045 Uiso 1 1 d . . . H4 H 0.310(7) 0.929(6) 0.220(5) 0.029(12) Uiso 1 1 d . . . H5 H -0.366(7) 1.261(5) 0.229(5) 0.030(12) Uiso 1 1 d . . . H6 H 0.348(7) 1.447(6) -0.075(5) 0.038(12) Uiso 1 1 d . . . H7 H 0.324(7) 1.294(6) -0.055(5) 0.029(12) Uiso 1 1 d . . . H9 H 0.52(6) 0.28(5) 0.42(5) 0.9(3) Uiso 1 1 d . . . H8 H 0.09(7) 0.66(5) 0.42(5) 0.5(4) Uiso 1 1 d . . . H10 H 0.487(16) 0.437(9) 0.525(10) 0.17(3) Uiso 1 1 d . . . H11 H 0.57(5) 0.46(6) 0.47(4) 0.27(19) Uiso 1 1 d . . . Fe1 Fe 0.0000 1.0000 0.0000 0.00514(13) Uani 1 2 d S . . Fe2 Fe 0.20344(6) 0.21676(5) 0.44977(4) 0.00526(11) Uani 1 1 d . . . P3 P -0.08951(10) 1.15543(8) 0.27900(8) 0.00546(15) Uani 1 1 d . . . P4 P 0.45262(10) 1.05503(9) -0.27791(8) 0.00549(15) Uani 1 1 d . . . P5 P 0.08655(10) 0.62240(8) 0.26849(8) 0.00571(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0078(9) 0.0057(9) 0.0046(9) -0.0004(7) -0.0009(7) -0.0013(7) O2 0.0092(9) 0.0079(9) 0.0068(9) -0.0029(7) 0.0007(7) -0.0019(7) O3 0.0084(10) 0.0089(10) 0.0157(10) -0.0059(8) -0.0064(8) -0.0003(8) O4 0.0091(9) 0.0088(9) 0.0067(9) -0.0044(7) -0.0008(7) -0.0017(7) O5 0.0086(10) 0.0047(10) 0.0164(11) -0.0038(8) -0.0059(8) -0.0007(8) O6 0.0078(9) 0.0084(9) 0.0077(9) -0.0040(7) -0.0010(7) -0.0013(7) O7 0.0080(9) 0.0050(9) 0.0064(9) -0.0021(7) -0.0011(7) -0.0005(7) O8 0.0054(10) 0.0079(9) 0.0107(10) -0.0022(8) -0.0024(7) -0.0013(8) O9 0.0088(9) 0.0065(9) 0.0083(9) -0.0029(7) -0.0024(7) -0.0020(7) O10 0.0084(9) 0.0052(9) 0.0071(9) -0.0004(7) -0.0014(7) -0.0030(7) O11 0.0079(9) 0.0073(9) 0.0065(9) -0.0021(7) -0.0028(7) -0.0009(7) O12 0.0047(9) 0.0051(8) 0.0074(9) -0.0014(7) -0.0007(7) 0.0001(7) N1 0.0163(14) 0.0129(13) 0.0106(13) -0.0037(11) -0.0033(10) -0.0009(11) N2 0.025(3) 0.026(3) 0.013(2) -0.004(2) -0.0022(17) -0.016(2) Fe1 0.0057(3) 0.0049(3) 0.0048(3) -0.0018(2) -0.00101(19) -0.0011(2) Fe2 0.0058(2) 0.00497(19) 0.00488(19) -0.00178(15) -0.00107(14) -0.00119(14) P3 0.0060(3) 0.0050(3) 0.0057(3) -0.0022(3) -0.0013(2) -0.0013(2) P4 0.0053(3) 0.0058(3) 0.0054(3) -0.0022(3) -0.0010(2) -0.0011(2) P5 0.0064(3) 0.0045(3) 0.0060(3) -0.0021(3) -0.0014(2) -0.0008(2) _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 O1 P5 1.5257(19) . ? O1 Fe1 2.0211(18) . ? O2 P4 1.5153(19) . ? O2 Fe1 1.9573(19) . ? O3 P4 1.571(2) 2_675 ? O4 P3 1.5316(19) . ? O4 Fe1 2.0412(18) . ? O5 P5 1.590(2) . ? O6 P5 1.5194(19) . ? O6 Fe2 1.9423(19) 2_566 ? O7 P4 1.5374(19) 2_665 ? O7 Fe2 2.0496(18) . ? O8 P3 1.588(2) . ? O9 P3 1.5274(19) 1_545 ? O9 Fe2 2.0276(19) . ? O10 P3 1.5021(19) 2_566 ? O10 Fe2 1.9515(18) . ? O11 P4 1.5176(19) 1_546 ? O11 Fe2 1.9600(19) . ? O12 P5 1.5321(19) . ? O12 Fe2 2.0524(18) . ? Fe1 O2 1.9573(19) 2_575 ? Fe1 O1 2.0211(18) 2_575 ? Fe1 O4 2.0412(18) 2_575 ? Fe2 O6 1.9423(19) 2_566 ? P3 O10 1.5021(19) 2_566 ? P3 O9 1.5274(19) 1_565 ? P4 O11 1.5176(19) 1_564 ? P4 O7 1.5374(19) 2_665 ? P4 O3 1.571(2) 2_675 ? 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 P5 O1 Fe1 129.39(11) . . ? P4 O2 Fe1 164.83(13) . . ? P3 O4 Fe1 131.08(12) . . ? P5 O6 Fe2 144.42(13) . 2_566 ? P4 O7 Fe2 134.33(11) 2_665 . ? P3 O9 Fe2 138.45(12) 1_545 . ? P3 O10 Fe2 153.25(12) 2_566 . ? P4 O11 Fe2 130.28(12) 1_546 . ? P5 O12 Fe2 124.21(11) . . ? O2 Fe1 O2 180.0 . 2_575 ? O2 Fe1 O1 86.76(8) . . ? O2 Fe1 O1 93.24(8) 2_575 . ? O2 Fe1 O1 93.24(8) . 2_575 ? O2 Fe1 O1 86.76(8) 2_575 2_575 ? O1 Fe1 O1 180.00(11) . 2_575 ? O2 Fe1 O4 87.32(8) . . ? O2 Fe1 O4 92.68(8) 2_575 . ? O1 Fe1 O4 88.87(7) . . ? O1 Fe1 O4 91.13(7) 2_575 . ? O2 Fe1 O4 92.68(8) . 2_575 ? O2 Fe1 O4 87.32(8) 2_575 2_575 ? O1 Fe1 O4 91.13(7) . 2_575 ? O1 Fe1 O4 88.87(7) 2_575 2_575 ? O4 Fe1 O4 180.0 . 2_575 ? O6 Fe2 O10 94.19(8) 2_566 . ? O6 Fe2 O11 93.47(8) 2_566 . ? O10 Fe2 O11 93.53(8) . . ? O6 Fe2 O9 90.26(8) 2_566 . ? O10 Fe2 O9 90.93(8) . . ? O11 Fe2 O9 173.97(8) . . ? O6 Fe2 O7 175.16(8) 2_566 . ? O10 Fe2 O7 88.93(8) . . ? O11 Fe2 O7 90.03(8) . . ? O9 Fe2 O7 85.98(7) . . ? O6 Fe2 O12 92.23(8) 2_566 . ? O10 Fe2 O12 172.23(8) . . ? O11 Fe2 O12 90.45(8) . . ? O9 Fe2 O12 84.66(7) . . ? O7 Fe2 O12 84.39(7) . . ? O10 P3 O9 113.28(11) 2_566 1_565 ? O10 P3 O4 113.26(11) 2_566 . ? O9 P3 O4 109.04(11) 1_565 . ? O10 P3 O8 108.30(11) 2_566 . ? O9 P3 O8 102.73(11) 1_565 . ? O4 P3 O8 109.66(11) . . ? O2 P4 O11 112.77(11) . 1_564 ? O2 P4 O7 108.95(11) . 2_665 ? O11 P4 O7 113.51(10) 1_564 2_665 ? O2 P4 O3 107.38(11) . 2_675 ? O11 P4 O3 104.13(11) 1_564 2_675 ? O7 P4 O3 109.83(11) 2_665 2_675 ? O6 P5 O1 110.95(11) . . ? O6 P5 O12 110.78(11) . . ? O1 P5 O12 110.29(10) . . ? O6 P5 O5 110.07(11) . . ? O1 P5 O5 107.40(11) . . ? O12 P5 O5 107.23(11) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.542 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.112 data_2007kvb0045 _database_code_depnum_ccdc_archive 'CCDC 713720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H2 Fe1.50 O5 P' _chemical_formula_weight 196.76 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 5.2061(3) _cell_length_b 5.2061(3) _cell_length_c 12.9609(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 351.29(4) _cell_formula_units_Z 4 _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 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 6.614 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5576 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _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 1338 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 27.52 _reflns_number_total 128 _reflns_number_gt 111 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.1051P] 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_number_reflns 128 _refine_ls_number_parameters 20 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.240 _refine_ls_shift/su_max 0.749 _refine_ls_shift/su_mean 0.202 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 O3 O 0.0000 0.7500 0.1250 0.022(2) Uani 1 8 d S . . H H 0.0000 0.87(3) 0.091(11) 0.00(5) Uiso 0.33 2 d SP . . P3 P 0.5000 0.2500 0.1250 0.0135(7) Uani 1 8 d S . . Fe2 Fe 0.0000 0.467(2) 0.0040(15) 0.0093(17) Uani 0.33 2 d SP . . O1 O 0.2575(9) 0.2500 0.0580(3) 0.0217(10) Uani 1 2 d S . . 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 O3 0.023(3) 0.023(3) 0.018(5) 0.000 0.000 0.000 P3 0.0129(10) 0.0129(10) 0.0148(14) 0.000 0.000 0.000 Fe2 0.0094(9) 0.012(5) 0.007(3) 0.015(4) 0.000 0.000 O1 0.021(2) 0.024(2) 0.020(2) 0.000 -0.009(2) 0.000 _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 O3 Fe2 2.02(2) 12_454 ? O3 Fe2 2.02(2) 3 ? O3 Fe2 2.02(2) 17_565 ? O3 Fe2 2.02(2) 26 ? O3 Fe2 2.150(19) 20_666 ? O3 Fe2 2.150(19) . ? O3 Fe2 2.150(19) 27_465 ? O3 Fe2 2.150(19) 10_464 ? P3 O1 1.533(4) 27_565 ? P3 O1 1.533(4) . ? P3 O1 1.533(4) 20_656 ? P3 O1 1.533(4) 10_554 ? Fe2 Fe2 0.354(19) 17_565 ? Fe2 O1 1.889(8) 10_454 ? Fe2 O1 1.889(8) . ? Fe2 O3 2.02(2) 17_565 ? Fe2 O1 2.146(8) 26 ? Fe2 O1 2.146(8) 17_565 ? Fe2 Fe2 2.26(2) 10_454 ? Fe2 Fe2 2.6051(15) 26 ? Fe2 Fe2 2.6051(15) 26_545 ? Fe2 Fe2 2.94(2) 10_464 ? O1 Fe2 1.889(8) 10_454 ? O1 Fe2 2.146(8) 26_545 ? O1 Fe2 2.146(8) 17_565 ? 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 Fe2 O3 Fe2 68.2(6) 12_454 3 ? Fe2 O3 Fe2 133.3(4) 12_454 17_565 ? Fe2 O3 Fe2 133.3(4) 3 17_565 ? Fe2 O3 Fe2 133.3(4) 12_454 26 ? Fe2 O3 Fe2 133.3(4) 3 26 ? Fe2 O3 Fe2 68.2(6) 17_565 26 ? Fe2 O3 Fe2 9.1(6) 12_454 20_666 ? Fe2 O3 Fe2 77.27(8) 3 20_666 ? Fe2 O3 Fe2 127.15(8) 17_565 20_666 ? Fe2 O3 Fe2 127.15(8) 26 20_666 ? Fe2 O3 Fe2 127.15(8) 12_454 . ? Fe2 O3 Fe2 127.15(8) 3 . ? Fe2 O3 Fe2 9.1(6) 17_565 . ? Fe2 O3 Fe2 77.27(8) 26 . ? Fe2 O3 Fe2 122.1(4) 20_666 . ? Fe2 O3 Fe2 77.27(8) 12_454 27_465 ? Fe2 O3 Fe2 9.1(6) 3 27_465 ? Fe2 O3 Fe2 127.15(8) 17_565 27_465 ? Fe2 O3 Fe2 127.15(8) 26 27_465 ? Fe2 O3 Fe2 86.3(6) 20_666 27_465 ? Fe2 O3 Fe2 122.1(4) . 27_465 ? Fe2 O3 Fe2 127.15(8) 12_454 10_464 ? Fe2 O3 Fe2 127.15(8) 3 10_464 ? Fe2 O3 Fe2 77.27(8) 17_565 10_464 ? Fe2 O3 Fe2 9.1(6) 26 10_464 ? Fe2 O3 Fe2 122.1(4) 20_666 10_464 ? Fe2 O3 Fe2 86.3(6) . 10_464 ? Fe2 O3 Fe2 122.1(4) 27_465 10_464 ? O1 P3 O1 108.74(16) 27_565 . ? O1 P3 O1 110.9(3) 27_565 20_656 ? O1 P3 O1 108.74(16) . 20_656 ? O1 P3 O1 108.74(16) 27_565 10_554 ? O1 P3 O1 110.9(3) . 10_554 ? O1 P3 O1 108.74(16) 20_656 10_554 ? Fe2 Fe2 O1 133.0(18) 17_565 10_454 ? Fe2 Fe2 O1 133.0(18) 17_565 . ? O1 Fe2 O1 90.4(5) 10_454 . ? Fe2 Fe2 O3 107(7) 17_565 17_565 ? O1 Fe2 O3 88.3(6) 10_454 17_565 ? O1 Fe2 O3 88.3(6) . 17_565 ? Fe2 Fe2 O1 40.1(15) 17_565 26 ? O1 Fe2 O1 173.1(4) 10_454 26 ? O1 Fe2 O1 96.1(2) . 26 ? O3 Fe2 O1 94.3(7) 17_565 26 ? Fe2 Fe2 O1 40.1(15) 17_565 17_565 ? O1 Fe2 O1 96.1(2) 10_454 17_565 ? O1 Fe2 O1 173.1(4) . 17_565 ? O3 Fe2 O1 94.3(7) 17_565 17_565 ? O1 Fe2 O1 77.3(4) 26 17_565 ? Fe2 Fe2 O3 64(6) 17_565 . ? O1 Fe2 O3 98.0(7) 10_454 . ? O1 Fe2 O3 98.0(7) . . ? O3 Fe2 O3 170.9(6) 17_565 . ? O1 Fe2 O3 78.7(4) 26 . ? O1 Fe2 O3 78.7(4) 17_565 . ? Fe2 Fe2 Fe2 163(7) 17_565 10_454 ? O1 Fe2 Fe2 53.2(4) 10_454 10_454 ? O1 Fe2 Fe2 53.2(4) . 10_454 ? O3 Fe2 Fe2 55.9(3) 17_565 10_454 ? O1 Fe2 Fe2 133.3(4) 26 10_454 ? O1 Fe2 Fe2 133.3(4) 17_565 10_454 ? O3 Fe2 Fe2 133.2(3) . 10_454 ? Fe2 Fe2 Fe2 15(6) 17_565 26 ? O1 Fe2 Fe2 127.9(7) 10_454 26 ? O1 Fe2 Fe2 127.9(7) . 26 ? O3 Fe2 Fe2 121.8(10) 17_565 26 ? O1 Fe2 Fe2 45.6(2) 26 26 ? O1 Fe2 Fe2 45.6(2) 17_565 26 ? O3 Fe2 Fe2 49.1(6) . 26 ? Fe2 Fe2 Fe2 177.7(8) 10_454 26 ? Fe2 Fe2 Fe2 161(7) 17_565 26_545 ? O1 Fe2 Fe2 54.3(3) 10_454 26_545 ? O1 Fe2 Fe2 54.3(3) . 26_545 ? O3 Fe2 Fe2 53.6(7) 17_565 26_545 ? O1 Fe2 Fe2 132.1(8) 26 26_545 ? O1 Fe2 Fe2 132.1(8) 17_565 26_545 ? O3 Fe2 Fe2 135.4(11) . 26_545 ? Fe2 Fe2 Fe2 2.3(8) 10_454 26_545 ? Fe2 Fe2 Fe2 175.4(17) 26 26_545 ? Fe2 Fe2 Fe2 17(7) 17_565 10_464 ? O1 Fe2 Fe2 126.8(4) 10_454 10_464 ? O1 Fe2 Fe2 126.8(4) . 10_464 ? O3 Fe2 Fe2 124.1(3) 17_565 10_464 ? O1 Fe2 Fe2 46.7(4) 26 10_464 ? O1 Fe2 Fe2 46.7(4) 17_565 10_464 ? O3 Fe2 Fe2 46.8(3) . 10_464 ? Fe2 Fe2 Fe2 180.000(1) 10_454 10_464 ? Fe2 Fe2 Fe2 2.3(8) 26 10_464 ? Fe2 Fe2 Fe2 177.7(8) 26_545 10_464 ? P3 O1 Fe2 142.6(5) . 10_454 ? P3 O1 Fe2 142.6(5) . . ? Fe2 O1 Fe2 73.7(8) 10_454 . ? P3 O1 Fe2 136.6(4) . 26_545 ? Fe2 O1 Fe2 6.9(4) 10_454 26_545 ? Fe2 O1 Fe2 80.15(18) . 26_545 ? P3 O1 Fe2 136.6(4) . 17_565 ? Fe2 O1 Fe2 80.15(18) 10_454 17_565 ? Fe2 O1 Fe2 6.9(4) . 17_565 ? Fe2 O1 Fe2 86.5(7) 26_545 17_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.557 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.140