# 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_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Richard Walton' _publ_contact_author_email R.I.WALTON@WARWICK.AC.UK _publ_section_title ; Polymorphism and variable structural dimensionality in the iron(III) phosphate oxalate system: a new polymorph of 3D [Fe2(HPO4)2(C2O4)(H2O)2].2H2O and the layered material [Fe2(HPO4)2(C2O4)(H2O)2] ; loop_ _publ_author_name 'Richard Walton' 'Guy J. Clarkson' 'Zoe A. D. Lethbridge' 'Scott Turner' # Attachment 'B911757A-I.cif' data_zl1 _database_code_depnum_ccdc_archive 'CCDC 736331' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H5 Fe O8 P' _chemical_formula_weight 231.87 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1041(3) _cell_length_b 6.6254(2) _cell_length_c 12.0431(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.423(2) _cell_angle_gamma 90.00 _cell_volume 613.49(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4750 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour light_brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 2.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5880 _exptl_absorpt_correction_T_max 0.8989 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; We are greatful to the EPSRC crystallographic service for recording the data for ZL1. Crystal decay was found to be negligible by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. The hydrogens on O1 and the waters O7 and O8 were found in a difference map. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameters equal to 1.5 times the displacement parameter of the oxygen atom to which they are attached. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 6105 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1402 _reflns_number_gt 1322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0126P)^2^+1.5819P] 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 1402 _refine_ls_number_parameters 115 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.77404(4) 0.18152(5) 0.59523(3) 0.00604(11) Uani 1 1 d . . . P1 P 1.01365(7) 0.42453(9) 0.82646(5) 0.00622(14) Uani 1 1 d . . . O1 O 1.1566(2) 0.5467(3) 0.79206(15) 0.0113(3) Uani 1 1 d D . . H1A H 1.160(4) 0.669(2) 0.813(3) 0.017 Uiso 1 1 d D . . O2 O 1.0869(2) 0.3465(3) 0.94998(14) 0.0101(3) Uani 1 1 d . . . O3 O 0.8603(2) 0.5683(2) 0.81152(13) 0.0083(3) Uani 1 1 d . . . O4 O 0.9633(2) 0.2471(2) 0.74104(13) 0.0080(3) Uani 1 1 d . . . C1 C 1.0164(3) 0.1015(3) 0.47453(19) 0.0079(4) Uani 1 1 d . . . O5 O 0.9412(2) 0.2523(3) 0.49823(14) 0.0097(3) Uani 1 1 d . . . O6 O 1.1194(2) 0.0977(2) 0.41483(14) 0.0091(3) Uani 1 1 d . . . O7 O 0.6937(2) 0.4734(3) 0.58613(14) 0.0114(3) Uani 1 1 d D . . H7A H 0.682(4) 0.525(4) 0.5207(14) 0.017 Uiso 1 1 d D . . H7B H 0.731(4) 0.558(4) 0.6391(17) 0.017 Uiso 1 1 d D . . O8 O 1.3279(2) 0.4170(3) 0.63545(15) 0.0119(4) Uani 1 1 d D . . H8A H 1.242(2) 0.468(4) 0.649(3) 0.018 Uiso 1 1 d D . . H8B H 1.414(2) 0.488(4) 0.673(2) 0.018 Uiso 1 1 d 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 0.00649(18) 0.00650(19) 0.00474(17) -0.00018(11) 0.00122(13) -0.00052(11) P1 0.0059(3) 0.0069(3) 0.0055(3) -0.0005(2) 0.0013(2) -0.0001(2) O1 0.0116(8) 0.0083(8) 0.0159(8) -0.0020(7) 0.0070(7) -0.0027(7) O2 0.0106(8) 0.0115(8) 0.0065(8) -0.0003(6) 0.0006(6) 0.0014(7) O3 0.0080(8) 0.0103(8) 0.0066(7) 0.0006(6) 0.0022(6) 0.0029(6) O4 0.0081(7) 0.0084(8) 0.0063(7) -0.0010(6) 0.0006(6) -0.0003(6) C1 0.0066(10) 0.0098(12) 0.0053(10) -0.0005(8) -0.0013(8) -0.0002(9) O5 0.0110(8) 0.0090(8) 0.0104(8) 0.0002(6) 0.0054(7) 0.0011(6) O6 0.0111(8) 0.0089(8) 0.0088(7) 0.0007(6) 0.0051(6) 0.0011(6) O7 0.0148(9) 0.0091(8) 0.0080(8) -0.0011(6) 0.0002(7) 0.0012(7) O8 0.0110(8) 0.0099(9) 0.0152(8) -0.0018(6) 0.0045(7) -0.0007(7) _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 O2 1.9283(16) 4_565 ? Fe1 O3 1.9450(16) 2_646 ? Fe1 O4 1.9804(16) . ? Fe1 O7 2.0322(17) . ? Fe1 O6 2.0615(16) 3_756 ? Fe1 O5 2.1025(16) . ? P1 O2 1.5080(16) . ? P1 O4 1.5300(17) . ? P1 O3 1.5303(16) . ? P1 O1 1.5720(17) . ? O1 H1A 0.846(14) . ? O2 Fe1 1.9283(16) 4_666 ? O3 Fe1 1.9450(16) 2_656 ? C1 O5 1.249(3) . ? C1 O6 1.262(3) . ? C1 C1 1.536(4) 3_756 ? O6 Fe1 2.0615(16) 3_756 ? O7 H7A 0.836(14) . ? O7 H7B 0.831(14) . ? O8 H8A 0.836(14) . ? O8 H8B 0.844(14) . ? 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 O2 Fe1 O3 93.62(7) 4_565 2_646 ? O2 Fe1 O4 172.85(7) 4_565 . ? O3 Fe1 O4 89.46(7) 2_646 . ? O2 Fe1 O7 84.04(7) 4_565 . ? O3 Fe1 O7 99.78(7) 2_646 . ? O4 Fe1 O7 89.08(7) . . ? O2 Fe1 O6 94.83(7) 4_565 3_756 ? O3 Fe1 O6 90.53(7) 2_646 3_756 ? O4 Fe1 O6 91.59(7) . 3_756 ? O7 Fe1 O6 169.67(7) . 3_756 ? O2 Fe1 O5 88.72(7) 4_565 . ? O3 Fe1 O5 169.60(7) 2_646 . ? O4 Fe1 O5 89.39(6) . . ? O7 Fe1 O5 90.53(7) . . ? O6 Fe1 O5 79.16(6) 3_756 . ? O2 P1 O4 109.77(10) . . ? O2 P1 O3 112.39(9) . . ? O4 P1 O3 111.39(9) . . ? O2 P1 O1 110.08(10) . . ? O4 P1 O1 106.30(9) . . ? O3 P1 O1 106.69(10) . . ? P1 O1 H1A 112(2) . . ? P1 O2 Fe1 151.57(11) . 4_666 ? P1 O3 Fe1 138.95(10) . 2_656 ? P1 O4 Fe1 137.07(10) . . ? O5 C1 O6 127.2(2) . . ? O5 C1 C1 116.8(2) . 3_756 ? O6 C1 C1 116.0(2) . 3_756 ? C1 O5 Fe1 113.27(15) . . ? C1 O6 Fe1 114.60(14) . 3_756 ? Fe1 O7 H7A 112(2) . . ? Fe1 O7 H7B 124(2) . . ? H7A O7 H7B 111(2) . . ? H8A O8 H8B 106(2) . . ? 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 O7 H7B O3 0.831(14) 2.01(2) 2.696(2) 140(3) . O8 H8A O1 0.836(14) 2.11(2) 2.807(2) 140(3) . O7 H7A O8 0.836(14) 1.896(14) 2.717(2) 167(3) 3_766 O8 H8B O4 0.844(14) 2.088(19) 2.876(2) 155(3) 2_756 O1 H1A O8 0.846(14) 1.749(15) 2.594(2) 177(3) 2_756 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.345 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.106 # Attachment 'II.cif' data_zl3 _database_code_depnum_ccdc_archive 'CCDC 736332' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H3 Fe O7 P' _chemical_formula_weight 213.85 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0365(3) _cell_length_b 7.6400(5) _cell_length_c 7.6678(6) _cell_angle_alpha 97.292(6) _cell_angle_beta 101.847(6) _cell_angle_gamma 106.380(6) _cell_volume 271.62(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1980 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 28.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 212 _exptl_absorpt_coefficient_mu 3.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; A crystal was glued to a glass fibre and the data ecorded at 296K. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Anisotropic displacement parameters were used for all non-H atoms; The hydrogens on O3 and O6 were located in a difference map and allowed to refine freely. OH-hydrogen atoms were given isotropic displacement parameters equal to 1.5 times the equivalent isotropic displacement parameter of the oxygen to which they are attached. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2581 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 28.95 _reflns_number_total 1277 _reflns_number_gt 1193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0265P)^2^+0.1073P] 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 1277 _refine_ls_number_parameters 100 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.04690(5) 0.26153(3) 0.29469(3) 0.00860(9) Uani 1 1 d . . . P1 P -0.35395(9) 0.54238(6) 0.29005(6) 0.00838(12) Uani 1 1 d . . . O1 O 0.1939(3) -0.15197(18) -0.02586(18) 0.0129(3) Uani 1 1 d . . . C1 C 0.1226(4) -0.0277(2) 0.0545(3) 0.0101(4) Uani 1 1 d . . . O2 O 0.2281(3) 0.05927(17) 0.21597(18) 0.0120(3) Uani 1 1 d . . . O3 O -0.2400(3) 0.0503(2) 0.3708(2) 0.0171(3) Uani 1 1 d . . . H3A H -0.231(5) -0.052(4) 0.364(4) 0.026 Uiso 1 1 d . . . H3B H -0.415(6) 0.050(3) 0.330(4) 0.026 Uiso 1 1 d . . . O4 O -0.2012(3) 0.40141(18) 0.32140(19) 0.0157(3) Uani 1 1 d . . . O5 O -0.2967(3) 0.68519(18) 0.46209(18) 0.0121(3) Uani 1 1 d . . . O6 O -0.2382(3) 0.6627(2) 0.1553(2) 0.0197(3) Uani 1 1 d D . . H6 H -0.247(5) 0.608(3) 0.054(3) 0.029 Uiso 1 1 d D . . O7 O -0.6748(3) 0.44552(17) 0.20709(18) 0.0118(3) 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 Fe1 0.00846(14) 0.00876(14) 0.00732(15) -0.00128(10) 0.00103(10) 0.00271(10) P1 0.0092(2) 0.0082(2) 0.0062(2) -0.00071(17) 0.00120(17) 0.00166(16) O1 0.0131(6) 0.0136(6) 0.0101(7) -0.0035(5) 0.0006(5) 0.0057(5) C1 0.0088(8) 0.0088(8) 0.0114(9) 0.0005(7) 0.0025(7) 0.0016(6) O2 0.0114(6) 0.0117(6) 0.0099(7) -0.0036(5) -0.0005(5) 0.0040(5) O3 0.0125(7) 0.0127(7) 0.0257(8) 0.0073(6) 0.0032(6) 0.0032(5) O4 0.0156(6) 0.0150(7) 0.0163(7) -0.0019(6) 0.0021(5) 0.0082(5) O5 0.0148(6) 0.0111(6) 0.0087(7) -0.0019(5) -0.0001(5) 0.0054(5) O6 0.0239(7) 0.0168(7) 0.0117(7) 0.0023(6) 0.0060(6) -0.0045(6) O7 0.0098(6) 0.0133(6) 0.0091(7) 0.0013(5) 0.0004(5) 0.0008(5) _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 O4 1.8835(13) . ? Fe1 O5 1.9446(13) 2_566 ? Fe1 O7 1.9765(12) 1_655 ? Fe1 O3 2.0745(14) . ? Fe1 O2 2.0905(13) . ? Fe1 O1 2.0937(13) 2 ? P1 O4 1.5056(14) . ? P1 O5 1.5214(13) . ? P1 O7 1.5322(13) . ? P1 O6 1.5616(15) . ? O1 C1 1.243(2) . ? O1 Fe1 2.0937(13) 2 ? C1 O2 1.257(2) . ? C1 C1 1.538(4) 2 ? O3 H3A 0.79(3) . ? O3 H3B 0.87(3) . ? O5 Fe1 1.9446(13) 2_566 ? O6 H6 0.819(17) . ? O7 Fe1 1.9765(12) 1_455 ? 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 O4 Fe1 O5 103.08(6) . 2_566 ? O4 Fe1 O7 97.57(6) . 1_655 ? O5 Fe1 O7 93.55(6) 2_566 1_655 ? O4 Fe1 O3 86.48(6) . . ? O5 Fe1 O3 88.50(6) 2_566 . ? O7 Fe1 O3 174.92(5) 1_655 . ? O4 Fe1 O2 165.15(5) . . ? O5 Fe1 O2 89.43(5) 2_566 . ? O7 Fe1 O2 89.49(5) 1_655 . ? O3 Fe1 O2 85.88(5) . . ? O4 Fe1 O1 88.66(6) . 2 ? O5 Fe1 O1 167.38(5) 2_566 2 ? O7 Fe1 O1 89.41(5) 1_655 2 ? O3 Fe1 O1 87.61(6) . 2 ? O2 Fe1 O1 78.33(5) . 2 ? O4 P1 O5 112.07(8) . . ? O4 P1 O7 110.66(7) . . ? O5 P1 O7 111.86(7) . . ? O4 P1 O6 111.13(9) . . ? O5 P1 O6 103.46(8) . . ? O7 P1 O6 107.36(8) . . ? C1 O1 Fe1 114.39(12) . 2 ? O1 C1 O2 127.52(17) . . ? O1 C1 C1 117.0(2) . 2 ? O2 C1 C1 115.53(19) . 2 ? C1 O2 Fe1 114.79(12) . . ? Fe1 O3 H3A 123.0(18) . . ? Fe1 O3 H3B 110.7(17) . . ? H3A O3 H3B 112(2) . . ? P1 O4 Fe1 159.13(10) . . ? P1 O5 Fe1 134.38(8) . 2_566 ? P1 O6 H6 117.4(19) . . ? P1 O7 Fe1 129.69(8) . 1_455 ? 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 O3 H3A O5 0.79(3) 2.20(3) 2.912(2) 151(2) 1_545 O3 H3A O6 0.79(3) 2.52(3) 3.205(2) 146(3) 1_545 O3 H3B O2 0.87(3) 1.85(3) 2.722(2) 172(2) 1_455 O6 H6 O7 0.819(17) 1.93(2) 2.704(2) 158(3) 2_465 _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.335 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.107