Supplementary data for CrystEngComm This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Christoph Janiak' 'Khalid Abu-Shandi' 'Heiner Winkler' 'Biao Wu' _publ_contact_author_name 'Prof Christoph Janiak' _publ_contact_author_address ; Inst. fur Anorgan. u. Analyt. Chemie Universitat Freiburg Albertstr. 21 Freiburg 79104 GERMANY ; _publ_contact_author_email JANIAK@UNI-FREIBURG.DE _publ_section_title ; Open-framework iron phosphates: Syntheses, structures, sorption studies and oxidation catalysis ; data_k8 #No 1 in manuscript _database_code_CSD 207258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexaaquairon(II)-H2piperazinedium-bis(hydrogenphosphate) ; _chemical_name_common Hexaaquairon(ii)-H2piperazinedium-bis(hydrogenphosphate) _chemical_melting_point ? _chemical_formula_moiety 'Fe(H2O)6, C4H12N2, 2(HPO4)' _chemical_formula_sum 'C4 H26 Fe N2 O14 P2' _chemical_formula_weight 444.06 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' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.317(4) _cell_length_b 9.643(5) _cell_length_c 12.877(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.574(9) _cell_angle_gamma 90.00 _cell_volume 783.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7548 _exptl_absorpt_correction_T_max 0.8755 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Bruker AXS CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4479 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.63 _reflns_number_total 1808 _reflns_number_gt 1370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Hydrogen atoms on O for the aqua ligands were found and refined isotropically. Hydrogen atoms on N (NH2) were found and refined with Ueq(H) = -1.5Ueq(N). Hydrogen atoms on carbon of the piperazine moiety were placed in calculated positions with the appropriate riding model AFIX 23 and Ueq(H) = -1.2Ueq(C). ; _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^)+(0.0471P)^2^+0.0000P] 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 1808 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Fe Fe 0.0000 0.0000 0.0000 0.01360(14) Uani 1 2 d S . . O1 O -0.2953(3) 0.0942(2) -0.02336(15) 0.0245(4) Uani 1 1 d . . . H11 H -0.364(6) 0.133(4) 0.025(3) 0.047(11) Uiso 1 1 d . . . H12 H -0.367(5) 0.088(3) -0.079(3) 0.035(9) Uiso 1 1 d . . . O2 O 0.0835(3) 0.1768(2) 0.08921(14) 0.0242(4) Uani 1 1 d . . . H21 H 0.001(6) 0.203(4) 0.148(3) 0.054(11) Uiso 1 1 d . . . H22 H 0.213(6) 0.192(4) 0.105(3) 0.054(11) Uiso 1 1 d . . . O3 O 0.0973(3) 0.1017(2) -0.13332(15) 0.0288(5) Uani 1 1 d . . . H31 H 0.010(6) 0.141(4) -0.177(3) 0.052(11) Uiso 1 1 d . . . H32 H 0.213(7) 0.104(4) -0.161(3) 0.061(13) Uiso 1 1 d . . . P P -0.41649(10) 0.24529(7) -0.26768(5) 0.01850(17) Uani 1 1 d . . . O4 O -0.5079(3) 0.26682(19) -0.37780(13) 0.0241(4) Uani 1 1 d . . . O5 O -0.5091(3) 0.11808(18) -0.21390(13) 0.0216(4) Uani 1 1 d . . . O6 O -0.4874(4) 0.3736(2) -0.19799(14) 0.0325(5) Uani 1 1 d . . . H6 H -0.497(7) 0.460(4) -0.230(3) 0.063(12) Uiso 1 1 d . . . O7 O -0.1749(3) 0.2426(2) -0.26142(15) 0.0320(5) Uani 1 1 d . . . N N -0.0918(5) 0.3850(3) -0.0548(2) 0.0373(6) Uani 1 1 d . . . HN1 H -0.018(6) 0.308(4) -0.008(3) 0.056 Uiso 1 1 d . . . HN2 H -0.186(6) 0.361(4) -0.124(3) 0.056 Uiso 1 1 d . . . C1 C -0.2232(5) 0.4797(3) 0.0065(3) 0.0475(9) Uani 1 1 d . . . H1A H -0.3426 0.4286 0.0339 0.057 Uiso 1 1 calc R . . H1B H -0.2800 0.5545 -0.0380 0.057 Uiso 1 1 calc R . . C2 C 0.0865(7) 0.4598(4) -0.0959(3) 0.0519(10) Uani 1 1 d . . . H2A H 0.0342 0.5345 -0.1417 0.062 Uiso 1 1 calc R . . H2B H 0.1715 0.3966 -0.1366 0.062 Uiso 1 1 calc R . . 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 Fe 0.0121(2) 0.0146(3) 0.0141(2) -0.00016(19) 0.00010(16) 0.00038(19) O1 0.0187(9) 0.0346(11) 0.0201(9) -0.0028(8) -0.0009(8) 0.0049(8) O2 0.0187(10) 0.0309(11) 0.0230(9) -0.0066(8) -0.0001(8) -0.0020(8) O3 0.0200(10) 0.0417(13) 0.0250(10) 0.0120(9) 0.0027(8) 0.0047(9) P 0.0166(3) 0.0199(3) 0.0188(3) 0.0038(2) -0.0012(2) -0.0007(2) O4 0.0205(9) 0.0317(11) 0.0200(9) 0.0043(8) -0.0016(7) 0.0005(8) O5 0.0224(9) 0.0196(9) 0.0229(9) 0.0029(7) 0.0015(7) -0.0010(7) O6 0.0521(14) 0.0201(11) 0.0257(10) 0.0009(8) 0.0053(9) 0.0013(9) O7 0.0162(10) 0.0441(12) 0.0354(11) 0.0183(9) -0.0022(8) -0.0029(8) N 0.0489(16) 0.0276(14) 0.0341(14) -0.0008(11) -0.0118(12) -0.0072(12) C1 0.0209(15) 0.0325(18) 0.090(3) 0.0103(18) 0.0096(16) 0.0004(13) C2 0.082(3) 0.0316(18) 0.045(2) -0.0085(15) 0.037(2) -0.0104(18) _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 Fe O1 2.084(2) 3 ? Fe O1 2.084(2) . ? Fe O3 2.093(2) 3 ? Fe O3 2.093(2) . ? Fe O2 2.110(2) . ? Fe O2 2.110(2) 3 ? O1 H11 0.86(4) . ? O1 H12 0.83(3) . ? O2 H21 0.97(4) . ? O2 H22 0.85(4) . ? O3 H31 0.86(4) . ? O3 H32 0.83(4) . ? P O4 1.5210(19) . ? P O7 1.525(2) . ? P O5 1.5373(19) . ? P O6 1.604(2) . ? O6 H6 0.93(4) . ? N C2 1.456(4) . ? N C1 1.485(4) . ? N HN1 1.05(4) . ? N HN2 1.08(3) . ? C1 C2 1.523(5) 3_565 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C1 1.523(5) 3_565 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? 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 O1 Fe O1 180.00(11) 3 . ? O1 Fe O3 88.36(8) 3 3 ? O1 Fe O3 91.64(8) . 3 ? O1 Fe O3 91.64(8) 3 . ? O1 Fe O3 88.36(8) . . ? O3 Fe O3 180.00(16) 3 . ? O1 Fe O2 94.23(8) 3 . ? O1 Fe O2 85.77(8) . . ? O3 Fe O2 90.43(9) 3 . ? O3 Fe O2 89.57(9) . . ? O1 Fe O2 85.77(8) 3 3 ? O1 Fe O2 94.23(8) . 3 ? O3 Fe O2 89.57(9) 3 3 ? O3 Fe O2 90.43(9) . 3 ? O2 Fe O2 180.00(8) . 3 ? Fe O1 H11 124(2) . . ? Fe O1 H12 123(2) . . ? H11 O1 H12 112(3) . . ? Fe O2 H21 120(2) . . ? Fe O2 H22 119(2) . . ? H21 O2 H22 108(3) . . ? Fe O3 H31 123(2) . . ? Fe O3 H32 132(3) . . ? H31 O3 H32 104(3) . . ? O4 P O7 112.86(11) . . ? O4 P O5 113.13(10) . . ? O7 P O5 111.29(11) . . ? O4 P O6 108.21(11) . . ? O7 P O6 106.70(12) . . ? O5 P O6 104.00(11) . . ? P O6 H6 118(3) . . ? C2 N C1 110.4(2) . . ? C2 N HN1 103(2) . . ? C1 N HN1 111.9(19) . . ? C2 N HN2 102.5(19) . . ? C1 N HN2 105.7(19) . . ? HN1 N HN2 123(3) . . ? N C1 C2 109.0(3) . 3_565 ? N C1 H1A 109.9 . . ? C2 C1 H1A 109.9 3_565 . ? N C1 H1B 109.9 . . ? C2 C1 H1B 109.9 3_565 . ? H1A C1 H1B 108.3 . . ? N C2 C1 109.7(3) . 3_565 ? N C2 H2A 109.7 . . ? C1 C2 H2A 109.7 3_565 . ? N C2 H2B 109.7 . . ? C1 C2 H2B 109.7 3_565 . ? H2A C2 H2B 108.2 . . ? 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 C2 N C1 C2 -59.4(4) . . . 3_565 ? C1 N C2 C1 59.8(4) . . . 3_565 ? 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 O1 H11 O4 0.86(4) 1.85(4) 2.709(3) 174(3) 4_566 O1 H12 O5 0.83(3) 1.94(3) 2.757(3) 166(3) . O2 H21 O7 0.97(4) 1.73(4) 2.692(3) 171(3) 4_566 O2 H22 O4 0.85(4) 1.81(4) 2.653(3) 173(3) 4_666 O3 H31 O7 0.86(4) 1.84(4) 2.697(3) 174(3) . O3 H32 O5 0.83(4) 1.92(4) 2.741(3) 174(4) 1_655 O6 H6 O5 0.93(4) 1.69(4) 2.616(3) 175(4) 2_454 N HN1 O2 1.05(4) 1.88(4) 2.917(3) 172(3) . N HN2 O6 1.08(3) 2.09(4) 3.040(4) 146(3) . N HN2 O7 1.08(3) 2.11(3) 3.018(3) 141(3) . _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.63 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.593 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.085 data_k2 #No 2 in manuscript _database_code_CSD 207259 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ammonium-[aqua(µ3-hydroxo)bis(µ4-phosphato)diferrate(III)]-hydrate ; _chemical_name_common ;Ammonium-(aqua(µ3-hydroxo)bis(µ4-phosphato)diferrate(iii))- hydrate ; _chemical_melting_point ? _chemical_formula_moiety 'Fe2, (PO4)2, OH, NH4, (H2O)2' _chemical_formula_sum 'H9 Fe2 N O11 P2' _chemical_formula_weight 372.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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 9.815(2) _cell_length_b 9.7225(19) _cell_length_c 9.877(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.87(3) _cell_angle_gamma 90.00 _cell_volume 918.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square plate' _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 3.562 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5360 _exptl_absorpt_correction_T_max 0.7171 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker AXS CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4945 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 26.06 _reflns_number_total 1808 _reflns_number_gt 1585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The hydrogen atoms on the hydroxy group (O9), aqua ligand (O10), the water molecule of crystallization (O11) and the ammonium moiety (N1) were found from the difference Fourier map and their position could be freely refined with Ueq(H) = -1.5Ueq(O,N). ; _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^)+(0.0632P)^2^+0.5522P] 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 1808 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 -0.60191(5) -0.26719(5) 0.18679(5) 0.00741(18) Uani 1 1 d . . . Fe2 Fe -0.38675(5) 0.04474(5) 0.12955(5) 0.00740(18) Uani 1 1 d . . . P1 P -0.29232(8) -0.18231(9) 0.36910(8) 0.0075(2) Uani 1 1 d . . . P2 P -0.70365(9) 0.03630(9) 0.14766(9) 0.0075(2) Uani 1 1 d . . . O1 O -0.2377(2) -0.1683(3) 0.5254(2) 0.0110(5) Uani 1 1 d . . . O2 O -0.2059(3) -0.2843(3) 0.3050(3) 0.0125(5) Uani 1 1 d . . . O3 O -0.4456(2) -0.2258(3) 0.3428(3) 0.0117(5) Uani 1 1 d . . . O4 O -0.2804(3) -0.0398(3) 0.3014(3) 0.0103(5) Uani 1 1 d . . . O5 O -0.7374(2) 0.0201(3) -0.0122(2) 0.0098(5) Uani 1 1 d . . . O6 O -0.8117(2) 0.1333(3) 0.1831(2) 0.0102(5) Uani 1 1 d . . . O7 O -0.5542(2) 0.0928(3) 0.1985(2) 0.0094(5) Uani 1 1 d . . . O8 O -0.7149(2) -0.1055(3) 0.2146(2) 0.0107(5) Uani 1 1 d . . . O9 O -0.5014(3) -0.1413(3) 0.0600(2) 0.0094(5) Uani 1 1 d . . . H9 H -0.451(5) -0.187(5) 0.042(5) 0.014 Uiso 1 1 d . . . O10 O -0.4946(3) -0.4459(3) 0.1572(3) 0.0182(6) Uani 1 1 d . . . H10A H -0.428(6) -0.478(6) 0.181(6) 0.027 Uiso 1 1 d . . . H10B H -0.534(6) -0.504(6) 0.120(6) 0.027 Uiso 1 1 d . . . O11 O -0.6784(3) -0.6471(3) 0.0354(3) 0.0203(6) Uani 1 1 d . . . H11A H -0.737(6) -0.599(6) -0.038(6) 0.030 Uiso 1 1 d . . . H11B H -0.711(6) -0.647(6) 0.094(6) 0.030 Uiso 1 1 d . . . N1 N -0.4904(4) 0.3088(4) 0.3980(4) 0.0188(7) Uani 1 1 d . . . H1A H -0.491(6) 0.254(6) 0.352(6) 0.028 Uiso 1 1 d . . . H1B H -0.424(6) 0.347(6) 0.402(6) 0.028 Uiso 1 1 d . . . H1C H -0.549(6) 0.370(6) 0.369(5) 0.028 Uiso 1 1 d . . . H1D H -0.489(5) 0.276(5) 0.482(6) 0.028 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 0.0032(3) 0.0096(3) 0.0082(3) 0.00008(18) -0.00137(19) -0.00057(18) Fe2 0.0032(3) 0.0091(3) 0.0087(3) -0.00047(17) -0.00123(19) -0.00015(18) P1 0.0029(4) 0.0096(5) 0.0083(4) 0.0004(3) -0.0024(3) -0.0004(3) P2 0.0033(4) 0.0093(5) 0.0090(4) -0.0007(3) -0.0004(3) 0.0006(3) O1 0.0072(11) 0.0143(13) 0.0095(11) -0.0007(10) -0.0028(9) 0.0004(10) O2 0.0114(12) 0.0117(13) 0.0132(12) 0.0008(10) 0.0001(10) 0.0034(10) O3 0.0059(11) 0.0164(14) 0.0116(12) 0.0005(10) -0.0008(9) -0.0027(10) O4 0.0067(12) 0.0110(13) 0.0119(12) 0.0008(9) -0.0009(9) 0.0002(10) O5 0.0048(11) 0.0136(13) 0.0102(12) -0.0012(10) 0.0001(9) 0.0013(10) O6 0.0051(11) 0.0141(13) 0.0107(11) -0.0024(9) -0.0003(9) 0.0034(10) O7 0.0039(12) 0.0122(13) 0.0114(12) -0.0009(10) -0.0001(9) -0.0022(10) O8 0.0096(12) 0.0088(13) 0.0139(12) 0.0017(10) 0.0028(9) 0.0011(10) O9 0.0063(12) 0.0090(13) 0.0122(12) 0.0011(9) 0.0009(9) 0.0018(10) O10 0.0075(13) 0.0157(15) 0.0276(15) -0.0064(12) -0.0043(11) 0.0046(11) O11 0.0230(15) 0.0179(15) 0.0208(15) 0.0037(12) 0.0067(12) 0.0013(12) N1 0.0127(17) 0.027(2) 0.0155(18) -0.0042(15) 0.0001(14) -0.0018(16) _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 O1 1.940(3) 4 ? Fe1 O6 1.948(2) 2_345 ? Fe1 O3 1.959(3) . ? Fe1 O8 1.978(3) . ? Fe1 O10 2.086(3) . ? Fe1 O9 2.142(2) . ? Fe2 O2 1.935(3) 2_455 ? Fe2 O5 1.964(2) 3_455 ? Fe2 O4 1.964(3) . ? Fe2 O7 1.970(2) . ? Fe2 O9 2.160(3) . ? Fe2 O9 2.162(3) 3_455 ? P1 O1 1.523(2) . ? P1 O3 1.528(2) . ? P1 O2 1.531(3) . ? P1 O4 1.554(3) . ? P2 O6 1.517(2) . ? P2 O7 1.542(2) . ? P2 O8 1.544(3) . ? P2 O5 1.547(2) . ? O1 Fe1 1.940(3) 4_656 ? O2 Fe2 1.935(3) 2_445 ? O5 Fe2 1.964(2) 3_455 ? O6 Fe1 1.948(2) 2_355 ? O9 Fe2 2.162(3) 3_455 ? O9 H9 0.72(5) . ? O10 H10A 0.71(6) . ? O10 H10B 0.74(6) . ? O11 H11A 0.94(6) . ? O11 H11B 0.72(6) . ? N1 H1A 0.70(6) . ? N1 H1B 0.74(6) . ? N1 H1C 0.84(6) . ? N1 H1D 0.89(6) . ? 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 O1 Fe1 O6 93.52(10) 4 2_345 ? O1 Fe1 O3 170.77(11) 4 . ? O6 Fe1 O3 87.88(10) 2_345 . ? O1 Fe1 O8 93.86(10) 4 . ? O6 Fe1 O8 87.89(10) 2_345 . ? O3 Fe1 O8 95.31(11) . . ? O1 Fe1 O10 83.77(11) 4 . ? O6 Fe1 O10 89.22(12) 2_345 . ? O3 Fe1 O10 87.13(12) . . ? O8 Fe1 O10 176.14(12) . . ? O1 Fe1 O9 91.48(10) 4 . ? O6 Fe1 O9 173.97(10) 2_345 . ? O3 Fe1 O9 87.72(10) . . ? O8 Fe1 O9 88.42(10) . . ? O10 Fe1 O9 94.67(12) . . ? O2 Fe2 O5 99.55(10) 2_455 3_455 ? O2 Fe2 O4 87.20(11) 2_455 . ? O5 Fe2 O4 95.49(10) 3_455 . ? O2 Fe2 O7 92.67(11) 2_455 . ? O5 Fe2 O7 162.83(10) 3_455 . ? O4 Fe2 O7 97.12(10) . . ? O2 Fe2 O9 176.50(10) 2_455 . ? O5 Fe2 O9 83.76(10) 3_455 . ? O4 Fe2 O9 93.63(10) . . ? O7 Fe2 O9 83.85(10) . . ? O2 Fe2 O9 91.51(11) 2_455 3_455 ? O5 Fe2 O9 83.69(10) 3_455 3_455 ? O4 Fe2 O9 178.35(10) . 3_455 ? O7 Fe2 O9 83.97(10) . 3_455 ? O9 Fe2 O9 87.71(10) . 3_455 ? O1 P1 O3 107.95(14) . . ? O1 P1 O2 111.98(14) . . ? O3 P1 O2 111.46(15) . . ? O1 P1 O4 108.24(14) . . ? O3 P1 O4 109.81(14) . . ? O2 P1 O4 107.34(14) . . ? O6 P2 O7 111.51(14) . . ? O6 P2 O8 109.62(14) . . ? O7 P2 O8 109.42(14) . . ? O6 P2 O5 107.25(14) . . ? O7 P2 O5 109.90(13) . . ? O8 P2 O5 109.09(14) . . ? P1 O1 Fe1 145.71(16) . 4_656 ? P1 O2 Fe2 132.92(16) . 2_445 ? P1 O3 Fe1 139.43(16) . . ? P1 O4 Fe2 131.95(15) . . ? P2 O5 Fe2 127.96(14) . 3_455 ? P2 O6 Fe1 152.93(16) . 2_355 ? P2 O7 Fe2 127.51(15) . . ? P2 O8 Fe1 123.66(14) . . ? Fe1 O9 Fe2 124.60(12) . . ? Fe1 O9 Fe2 122.91(11) . 3_455 ? Fe2 O9 Fe2 92.29(10) . 3_455 ? Fe1 O9 H9 103(4) . . ? Fe2 O9 H9 105(4) . . ? Fe2 O9 H9 107(4) 3_455 . ? Fe1 O10 H10A 140(5) . . ? Fe1 O10 H10B 119(4) . . ? H10A O10 H10B 100(6) . . ? H11A O11 H11B 108(5) . . ? H1A N1 H1B 107(6) . . ? H1A N1 H1C 114(6) . . ? H1B N1 H1C 101(5) . . ? H1A N1 H1D 109(6) . . ? H1B N1 H1D 108(5) . . ? H1C N1 H1D 117(5) . . ? 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 O3 P1 O1 Fe1 119.7(3) . . . 4_656 ? O2 P1 O1 Fe1 -3.3(3) . . . 4_656 ? O4 P1 O1 Fe1 -121.5(3) . . . 4_656 ? O1 P1 O2 Fe2 36.0(3) . . . 2_445 ? O3 P1 O2 Fe2 -85.1(2) . . . 2_445 ? O4 P1 O2 Fe2 154.63(19) . . . 2_445 ? O1 P1 O3 Fe1 179.3(2) . . . . ? O2 P1 O3 Fe1 -57.3(3) . . . . ? O4 P1 O3 Fe1 61.5(3) . . . . ? O1 Fe1 O3 P1 60.9(8) 4 . . . ? O6 Fe1 O3 P1 159.8(3) 2_345 . . . ? O8 Fe1 O3 P1 -112.5(3) . . . . ? O10 Fe1 O3 P1 70.5(3) . . . . ? O9 Fe1 O3 P1 -24.3(3) . . . . ? O1 P1 O4 Fe2 -152.87(18) . . . . ? O3 P1 O4 Fe2 -35.2(2) . . . . ? O2 P1 O4 Fe2 86.1(2) . . . . ? O2 Fe2 O4 P1 169.1(2) 2_455 . . . ? O5 Fe2 O4 P1 -91.5(2) 3_455 . . . ? O7 Fe2 O4 P1 76.8(2) . . . . ? O9 Fe2 O4 P1 -7.5(2) . . . . ? O9 Fe2 O4 P1 -152(3) 3_455 . . . ? O6 P2 O5 Fe2 160.77(17) . . . 3_455 ? O7 P2 O5 Fe2 39.4(2) . . . 3_455 ? O8 P2 O5 Fe2 -80.6(2) . . . 3_455 ? O7 P2 O6 Fe1 -62.4(4) . . . 2_355 ? O8 P2 O6 Fe1 58.9(4) . . . 2_355 ? O5 P2 O6 Fe1 177.2(3) . . . 2_355 ? O6 P2 O7 Fe2 -157.90(16) . . . . ? O8 P2 O7 Fe2 80.66(19) . . . . ? O5 P2 O7 Fe2 -39.1(2) . . . . ? O2 Fe2 O7 P2 156.84(19) 2_455 . . . ? O5 Fe2 O7 P2 21.3(5) 3_455 . . . ? O4 Fe2 O7 P2 -115.65(19) . . . . ? O9 Fe2 O7 P2 -22.74(18) . . . . ? O9 Fe2 O7 P2 65.60(18) 3_455 . . . ? O6 P2 O8 Fe1 176.22(15) . . . . ? O7 P2 O8 Fe1 -61.21(19) . . . . ? O5 P2 O8 Fe1 59.1(2) . . . . ? O1 Fe1 O8 P2 -90.08(18) 4 . . . ? O6 Fe1 O8 P2 176.53(18) 2_345 . . . ? O3 Fe1 O8 P2 88.86(18) . . . . ? O10 Fe1 O8 P2 -142.0(16) . . . . ? O9 Fe1 O8 P2 1.30(17) . . . . ? O1 Fe1 O9 Fe2 152.71(15) 4 . . . ? O6 Fe1 O9 Fe2 6.7(10) 2_345 . . . ? O3 Fe1 O9 Fe2 -36.49(15) . . . . ? O8 Fe1 O9 Fe2 58.89(15) . . . . ? O10 Fe1 O9 Fe2 -123.43(15) . . . . ? O1 Fe1 O9 Fe2 32.42(15) 4 . . 3_455 ? O6 Fe1 O9 Fe2 -113.6(9) 2_345 . . 3_455 ? O3 Fe1 O9 Fe2 -156.78(15) . . . 3_455 ? O8 Fe1 O9 Fe2 -61.40(15) . . . 3_455 ? O10 Fe1 O9 Fe2 116.29(15) . . . 3_455 ? O2 Fe2 O9 Fe1 -56.2(17) 2_455 . . . ? O5 Fe2 O9 Fe1 142.62(15) 3_455 . . . ? O4 Fe2 O9 Fe1 47.48(15) . . . . ? O7 Fe2 O9 Fe1 -49.30(14) . . . . ? O9 Fe2 O9 Fe1 -133.48(18) 3_455 . . . ? O2 Fe2 O9 Fe2 77.3(17) 2_455 . . 3_455 ? O5 Fe2 O9 Fe2 -83.90(10) 3_455 . . 3_455 ? O4 Fe2 O9 Fe2 -179.04(9) . . . 3_455 ? O7 Fe2 O9 Fe2 84.18(10) . . . 3_455 ? O9 Fe2 O9 Fe2 0.0 3_455 . . 3_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 O9 H9 O11 0.72(5) 2.29(5) 2.997(4) 171(5) 3_445 O10 H10A O4 0.71(6) 2.10(6) 2.792(4) 162(6) 2_445 O10 H10B O11 0.74(6) 2.03(6) 2.750(4) 167(6) . O11 H11A O4 0.94(6) 2.06(6) 2.935(4) 155(4) 4 O11 H11B O8 0.72(6) 2.21(6) 2.917(4) 168(6) 2_345 N1 H1A O7 0.70(6) 2.17(6) 2.851(5) 164(6) . N1 H1B O5 0.74(6) 2.25(6) 2.956(5) 159(5) 4_666 N1 H1C O8 0.84(6) 2.29(6) 2.977(5) 140(5) 2_355 N1 H1D O3 0.89(6) 2.04(6) 2.885(5) 160(5) 3_456 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.198 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.168 data_k3 #No 3 in manuscript _database_code_CSD 207260 _audit_creation_method SHELXL-97 _chemical_name_systematic ; H2piperazinedium-(aqua)(µ3-hydrogenphosphato)(tris-µ4-phosphato)- tri-iron(III)-0.25hydrate ; _chemical_name_common ; H2piperazinedium-(aqua)(µ3-hydrogenphosphato)(tris-µ4- phosphato)-tri-iron(iii)-0.25hydrate ; _chemical_melting_point ? _chemical_formula_moiety '3Fe, (C4N2H12), 3(PO4), HPO4, 1.25H2O' _chemical_formula_sum 'C4 H13 Fe3 N2 O17.25 P4' _chemical_formula_weight 656.59 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' 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 6.3554(16) _cell_length_b 9.166(2) _cell_length_c 15.311(4) _cell_angle_alpha 90.270(4) _cell_angle_beta 91.338(4) _cell_angle_gamma 106.594(4) _cell_volume 854.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 2.988 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6153 _exptl_absorpt_correction_T_max 0.8181 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Bruker AXS CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7722 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.77 _reflns_number_total 4000 _reflns_number_gt 2917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker 1997)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The hydrogen atoms on piperazinedium were calculated with appropriate riding models (AFIX 23) and Ueq(H) = 1.2 Ueq(C,N). The hydrogen atom on HPO4 was placed in a position calculated for an appropriate hydrogen bond to O1 with Ueq(H) = 1.5 Ueq(O). One HPO4 ligand was assumed because of electroneutrality for all Fe in the formal +3 oxidation state. Oxygen atom O8 was chosen for the hydrogen atom since it is the only O atom with no bond to Fe. The phosphato groups of P2 and P3 were subject to disorder coupled together with the aqua ligand (O21, O21') on Fe2. As part of the disorder around P2 a water molecule of crystallization (O31, not fully occupied) could be located. O8’ was refined with an isotropic thermal parameter. The hydrogen atoms of the water molecules were neither found nor calculated, hence there is a deviation in the chemical formula moiety composition and the chemical formula sum by 2.5 hydrogen atoms. ; _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^)+(0.0522P)^2^+0.0000P] 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 4000 _refine_ls_number_parameters 330 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1054 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 -0.23468(9) 0.03711(6) 0.38230(4) 0.00907(14) Uani 1 1 d . . . Fe2 Fe -0.25269(10) 0.04156(8) 0.12640(4) 0.01779(17) Uani 1 1 d . . . Fe3 Fe -0.87048(9) -0.31140(6) 0.24959(4) 0.00899(14) Uani 1 1 d . . . P1 P -0.34494(17) -0.22356(12) 0.27779(7) 0.0101(2) Uani 1 1 d . . . O1 O -0.1736(5) -0.2939(4) 0.2421(2) 0.0276(8) Uani 1 1 d . . . O2 O -0.3194(4) -0.1937(3) 0.37748(18) 0.0112(6) Uani 1 1 d . . . O3 O -0.3072(5) -0.0585(3) 0.24361(19) 0.0188(7) Uani 1 1 d . . . O4 O -0.5678(5) -0.3289(3) 0.25099(19) 0.0148(6) Uani 1 1 d . . . O5 O -0.1581(5) 0.2429(3) 0.33639(18) 0.0159(6) Uani 1 1 d . . . O6 O 0.0224(5) 0.4736(3) 0.2530(2) 0.0190(7) Uani 1 1 d . . . P2 P -0.1787(2) 0.33615(15) 0.25889(9) 0.0188(4) Uani 0.867(4) 1 d P A 1 O7 O -0.2635(11) 0.2540(7) 0.1767(4) 0.0128(13) Uani 0.50 1 d P A 1 O31 O 0.269(3) 0.2165(16) 0.2386(9) 0.026(3) Uani 0.25 1 d P B 1 O8 O -0.3835(7) 0.3966(5) 0.2721(5) 0.076(2) Uani 0.867(4) 1 d P A 1 H8A H -0.3168 0.4967 0.2612 0.115 Uiso 0.50 1 d P C 1 H8B H -0.4882 0.3470 0.2420 0.115 Uiso 0.50 1 d P D 1 P2' P -0.0275(15) 0.3035(9) 0.2540(5) 0.013(3) Uani 0.133(4) 1 d PD A 2 O7' O -0.1537(12) 0.2330(7) 0.1716(4) 0.0153(14) Uani 0.50 1 d P A 2 O8' O 0.197(4) 0.257(3) 0.2621(17) 0.017(6) Uiso 0.133(4) 1 d PD A 2 P3 P -0.6645(4) -0.1253(3) 0.07954(14) 0.0112(4) Uani 0.50 1 d P . 3 O12 O -0.4485(9) -0.1691(7) 0.0683(4) 0.0146(12) Uani 0.50 1 d P . 3 O21 O 0.0718(9) 0.1126(7) 0.1796(4) 0.0165(13) Uani 0.50 1 d P A 3 P3' P -0.8030(4) -0.0934(2) 0.07929(13) 0.0101(4) Uani 0.50 1 d P . 4 O12' O -0.9574(10) -0.0024(7) 0.1083(4) 0.0180(13) Uani 0.50 1 d P . 4 O21' O -0.2041(9) -0.1508(7) 0.0772(4) 0.0145(12) Uani 0.50 1 d P . 4 O9 O -0.5745(5) 0.0201(4) 0.1087(3) 0.0421(11) Uani 1 1 d . . . O10 O -0.8181(6) -0.1324(4) -0.0120(2) 0.0263(8) Uani 1 1 d . . . O11 O -0.8360(5) -0.2406(3) 0.13311(19) 0.0183(7) Uani 1 1 d . . . P4 P -0.77599(17) -0.05024(12) 0.40192(7) 0.0102(2) Uani 1 1 d . A . O13 O -0.8145(5) -0.2051(4) 0.3563(2) 0.0220(7) Uani 1 1 d . . . O14 O -0.5386(5) 0.0478(3) 0.3909(2) 0.0168(7) Uani 1 1 d . . . O15 O -0.9248(5) 0.0387(3) 0.3629(2) 0.0166(7) Uani 1 1 d . . . O16 O -0.8262(5) -0.0848(4) 0.49774(19) 0.0191(7) Uani 1 1 d . . . N1 N -0.5124(7) 0.3464(5) 0.4750(3) 0.0246(9) Uani 1 1 d . . . H1A H -0.5593 0.2943 0.5247 0.030 Uiso 1 1 calc R . . H1B H -0.4960 0.2786 0.4340 0.030 Uiso 1 1 calc R . . C2 C -0.2964(8) 0.4610(6) 0.4932(3) 0.0277(12) Uani 1 1 d . . . H2C H -0.2383 0.5099 0.4385 0.033 Uiso 1 1 calc R . . H2D H -0.1920 0.4097 0.5168 0.033 Uiso 1 1 calc R . . C1 C -0.6818(8) 0.4204(6) 0.4430(3) 0.0301(12) Uani 1 1 d . . . H1C H -0.6392 0.4675 0.3864 0.036 Uiso 1 1 calc R . . H1D H -0.8237 0.3430 0.4350 0.036 Uiso 1 1 calc R . . N2 N -0.5027(8) -0.3703(5) -0.0505(3) 0.0432(13) Uani 1 1 d . . . H2A H -0.5287 -0.3293 -0.1023 0.052 Uiso 1 1 calc R . . H2B H -0.4581 -0.2934 -0.0104 0.052 Uiso 1 1 calc R . . C4 C -0.6714(11) -0.5558(7) 0.0610(4) 0.0454(17) Uani 1 1 d . . . H4A H -0.6296 -0.4795 0.1081 0.054 Uiso 1 1 calc R . . H4B H -0.8073 -0.6318 0.0771 0.054 Uiso 1 1 calc R . . C3 C -0.7093(9) -0.4812(7) -0.0215(6) 0.059(2) Uani 1 1 d . . . H3A H -0.8209 -0.4280 -0.0125 0.071 Uiso 1 1 calc R . . H3B H -0.7647 -0.5588 -0.0672 0.071 Uiso 1 1 calc R . . 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 0.0071(3) 0.0097(3) 0.0106(3) 0.0004(2) 0.0006(2) 0.0026(2) Fe2 0.0111(3) 0.0244(4) 0.0127(3) 0.0078(3) -0.0022(2) -0.0033(3) Fe3 0.0075(3) 0.0087(3) 0.0105(3) -0.0001(2) 0.0007(2) 0.0017(2) P1 0.0077(5) 0.0110(5) 0.0115(5) -0.0010(4) 0.0016(4) 0.0024(4) O1 0.0109(16) 0.044(2) 0.0303(19) -0.0241(17) -0.0087(14) 0.0131(15) O2 0.0107(14) 0.0100(14) 0.0125(15) 0.0001(11) 0.0026(11) 0.0024(11) O3 0.0271(18) 0.0120(16) 0.0123(16) 0.0014(12) -0.0005(13) -0.0023(13) O4 0.0079(14) 0.0133(15) 0.0220(16) -0.0044(12) -0.0020(12) 0.0012(12) O5 0.0215(16) 0.0121(15) 0.0122(15) 0.0033(12) -0.0001(12) 0.0016(13) O6 0.0172(16) 0.0089(15) 0.0289(18) 0.0017(13) 0.0048(13) 0.0000(12) P2 0.0213(9) 0.0108(7) 0.0184(7) 0.0044(5) -0.0083(6) -0.0043(6) O7 0.019(4) 0.010(3) 0.009(3) -0.001(2) 0.001(3) 0.003(3) O31 0.038(9) 0.023(8) 0.014(7) 0.010(6) -0.001(6) 0.005(7) O8 0.014(2) 0.021(3) 0.191(7) 0.037(3) -0.018(3) 0.001(2) P2' 0.016(5) 0.008(4) 0.011(4) 0.003(3) 0.005(3) -0.001(3) O7' 0.020(4) 0.011(3) 0.013(3) -0.004(2) 0.001(3) 0.002(3) P3 0.0083(11) 0.0163(11) 0.0096(10) 0.0018(8) 0.0013(8) 0.0041(9) O12 0.009(3) 0.019(3) 0.015(3) 0.000(2) 0.002(2) 0.002(2) O21 0.010(3) 0.024(4) 0.015(3) 0.001(3) -0.001(2) 0.004(3) P3' 0.0087(11) 0.0134(11) 0.0087(10) 0.0023(8) 0.0023(8) 0.0039(9) O12' 0.015(3) 0.022(3) 0.019(3) 0.000(3) 0.004(2) 0.008(3) O21' 0.013(3) 0.015(3) 0.017(3) 0.003(2) 0.003(2) 0.005(2) O9 0.0103(17) 0.035(2) 0.074(3) 0.032(2) -0.0129(18) -0.0046(15) O10 0.042(2) 0.0221(18) 0.0178(17) 0.0103(14) 0.0148(15) 0.0119(16) O11 0.0204(17) 0.0208(17) 0.0140(15) 0.0082(13) 0.0051(13) 0.0058(14) P4 0.0076(5) 0.0134(5) 0.0100(5) -0.0012(4) 0.0009(4) 0.0038(4) O13 0.0169(17) 0.0280(19) 0.0226(17) -0.0160(14) -0.0074(13) 0.0100(14) O14 0.0099(15) 0.0176(16) 0.0244(17) 0.0012(13) 0.0043(12) 0.0058(12) O15 0.0088(14) 0.0185(16) 0.0242(17) 0.0086(13) 0.0040(12) 0.0064(12) O16 0.0176(16) 0.0263(18) 0.0120(15) -0.0005(13) 0.0003(12) 0.0038(14) N1 0.027(2) 0.025(2) 0.018(2) 0.0074(17) 0.0023(17) 0.0025(18) C2 0.016(2) 0.035(3) 0.031(3) 0.014(2) 0.004(2) 0.004(2) C1 0.021(3) 0.034(3) 0.030(3) 0.012(2) -0.002(2) 0.000(2) N2 0.046(3) 0.025(3) 0.050(3) 0.015(2) -0.026(2) -0.002(2) C4 0.057(4) 0.031(3) 0.041(4) -0.010(3) 0.033(3) -0.003(3) C3 0.016(3) 0.028(3) 0.129(7) 0.017(4) -0.018(3) 0.002(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 Fe1 O16 1.891(3) 2_456 ? Fe1 O5 1.947(3) . ? Fe1 O14 1.969(3) . ? Fe1 O15 1.994(3) 1_655 ? Fe1 O2 2.029(3) . ? Fe1 O3 2.279(3) . ? Fe1 P1 2.7775(13) . ? Fe2 O7' 1.814(6) . ? Fe2 O10 1.950(3) 2_455 ? Fe2 O9 2.010(3) . ? Fe2 O3 2.011(3) . ? Fe2 O21' 2.020(6) . ? Fe2 O12' 2.053(6) 1_655 ? Fe2 O7 2.110(6) . ? Fe2 O21 2.119(6) . ? Fe2 O12 2.151(6) . ? Fe2 P3 2.705(2) . ? Fe3 O13 1.873(3) . ? Fe3 O6 1.893(3) 1_445 ? Fe3 O11 1.897(3) . ? Fe3 O4 1.975(3) . ? Fe3 O1 1.979(3) 1_455 ? P1 O4 1.515(3) . ? P1 O1 1.525(3) . ? P1 O2 1.546(3) . ? P1 O3 1.558(3) . ? O1 Fe3 1.979(3) 1_655 ? O5 P2 1.491(3) . ? O5 P2' 1.543(8) . ? O6 P2' 1.500(8) . ? O6 P2 1.522(3) . ? O6 Fe3 1.893(3) 1_665 ? P2 O7 1.473(6) . ? P2 O8 1.570(5) . ? P2 H8A 1.9170 . ? O8 H8A 0.9120 . ? O8 H8B 0.8204 . ? P2' O7' 1.516(11) . ? P2' O8' 1.61(3) . ? P3 O9 1.360(5) . ? P3 O11 1.539(3) . ? P3 O12 1.549(6) . ? P3 O10 1.679(4) . ? P3' O10 1.435(4) . ? P3' O12' 1.530(6) . ? P3' O11 1.549(4) . ? P3' O9 1.580(4) . ? O12' O21' 1.810(8) 1_455 ? O12' Fe2 2.053(6) 1_455 ? O21' O12' 1.810(8) 1_655 ? O10 Fe2 1.950(3) 2_455 ? P4 O16 1.524(3) . ? P4 O15 1.528(3) . ? P4 O13 1.531(3) . ? P4 O14 1.533(3) . ? O15 Fe1 1.994(3) 1_455 ? O16 Fe1 1.891(3) 2_456 ? N1 C2 1.490(6) . ? N1 C1 1.501(6) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? C2 C1 1.495(7) 2_466 ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C1 C2 1.495(7) 2_466 ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? N2 C4 1.464(8) 2_445 ? N2 C3 1.491(7) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? C4 N2 1.464(8) 2_445 ? C4 C3 1.486(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? 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 O16 Fe1 O5 99.02(13) 2_456 . ? O16 Fe1 O14 92.32(13) 2_456 . ? O5 Fe1 O14 87.85(13) . . ? O16 Fe1 O15 91.62(13) 2_456 1_655 ? O5 Fe1 O15 87.46(12) . 1_655 ? O14 Fe1 O15 174.30(13) . 1_655 ? O16 Fe1 O2 103.94(13) 2_456 . ? O5 Fe1 O2 156.75(12) . . ? O14 Fe1 O2 94.73(12) . . ? O15 Fe1 O2 88.31(12) 1_655 . ? O16 Fe1 O3 170.86(13) 2_456 . ? O5 Fe1 O3 89.76(11) . . ? O14 Fe1 O3 90.51(12) . . ? O15 Fe1 O3 86.22(12) 1_655 . ? O2 Fe1 O3 67.14(11) . . ? O16 Fe1 P1 136.87(10) 2_456 . ? O5 Fe1 P1 123.68(9) . . ? O14 Fe1 P1 94.81(9) . . ? O15 Fe1 P1 85.10(10) 1_655 . ? O2 Fe1 P1 33.10(8) . . ? O3 Fe1 P1 34.11(8) . . ? O7' Fe2 O10 87.0(2) . 2_455 ? O7' Fe2 O9 101.4(3) . . ? O10 Fe2 O9 92.60(15) 2_455 . ? O7' Fe2 O3 94.4(2) . . ? O10 Fe2 O3 175.84(14) 2_455 . ? O9 Fe2 O3 90.98(15) . . ? O7' Fe2 O21' 152.2(3) . . ? O10 Fe2 O21' 87.78(19) 2_455 . ? O9 Fe2 O21' 106.2(2) . . ? O3 Fe2 O21' 89.19(19) . . ? O7' Fe2 O12' 99.4(3) . 1_655 ? O10 Fe2 O12' 80.3(2) 2_455 1_655 ? O9 Fe2 O12' 157.6(2) . 1_655 ? O3 Fe2 O12' 95.61(19) . 1_655 ? O21' Fe2 O12' 52.8(2) . 1_655 ? O7' Fe2 O7 21.3(2) . . ? O10 Fe2 O7 89.86(19) 2_455 . ? O9 Fe2 O7 80.2(2) . . ? O3 Fe2 O7 92.83(19) . . ? O21' Fe2 O7 173.3(3) . . ? O12' Fe2 O7 120.6(3) 1_655 . ? O7' Fe2 O21 62.1(3) . . ? O10 Fe2 O21 96.30(19) 2_455 . ? O9 Fe2 O21 160.6(2) . . ? O3 Fe2 O21 80.91(18) . . ? O21' Fe2 O21 91.4(2) . . ? O12' Fe2 O21 41.7(2) 1_655 . ? O7 Fe2 O21 82.6(3) . . ? O7' Fe2 O12 165.0(3) . . ? O10 Fe2 O12 91.63(19) 2_455 . ? O9 Fe2 O12 63.7(2) . . ? O3 Fe2 O12 88.07(18) . . ? O21' Fe2 O12 42.5(2) . . ? O12' Fe2 O12 95.1(2) 1_655 . ? O7 Fe2 O12 143.9(2) . . ? O21 Fe2 O12 132.9(2) . . ? O7' Fe2 P3 130.3(2) . . ? O10 Fe2 P3 95.26(12) 2_455 . ? O9 Fe2 P3 29.02(13) . . ? O3 Fe2 P3 86.86(10) . . ? O21' Fe2 P3 77.39(17) . . ? O12' Fe2 P3 129.95(18) 1_655 . ? O7 Fe2 P3 109.1(2) . . ? O21 Fe2 P3 163.55(17) . . ? O12 Fe2 P3 34.90(16) . . ? O13 Fe3 O6 117.69(15) . 1_445 ? O13 Fe3 O11 130.82(15) . . ? O6 Fe3 O11 111.49(14) 1_445 . ? O13 Fe3 O4 90.44(13) . . ? O6 Fe3 O4 89.12(13) 1_445 . ? O11 Fe3 O4 89.82(13) . . ? O13 Fe3 O1 91.91(13) . 1_455 ? O6 Fe3 O1 90.99(14) 1_445 1_455 ? O11 Fe3 O1 87.62(14) . 1_455 ? O4 Fe3 O1 177.29(13) . 1_455 ? O4 P1 O1 106.80(18) . . ? O4 P1 O2 112.75(16) . . ? O1 P1 O2 113.00(17) . . ? O4 P1 O3 113.01(17) . . ? O1 P1 O3 110.6(2) . . ? O2 P1 O3 100.80(16) . . ? O4 P1 Fe1 130.36(12) . . ? O1 P1 Fe1 122.67(13) . . ? O2 P1 Fe1 45.79(11) . . ? O3 P1 Fe1 55.14(11) . . ? P1 O1 Fe3 148.2(2) . 1_655 ? P1 O2 Fe1 101.11(14) . . ? P1 O3 Fe2 135.29(19) . . ? P1 O3 Fe1 90.75(14) . . ? Fe2 O3 Fe1 131.79(14) . . ? P1 O4 Fe3 134.42(18) . . ? P2 O5 P2' 42.0(3) . . ? P2 O5 Fe1 144.35(19) . . ? P2' O5 Fe1 128.1(4) . . ? P2' O6 P2 42.2(4) . . ? P2' O6 Fe3 171.5(4) . 1_665 ? P2 O6 Fe3 146.3(2) . 1_665 ? O7 P2 O5 117.3(3) . . ? O7 P2 O6 116.8(3) . . ? O5 P2 O6 110.50(19) . . ? O7 P2 O8 94.9(4) . . ? O5 P2 O8 107.6(3) . . ? O6 P2 O8 107.7(2) . . ? O7 P2 H8A 103.5 . . ? O5 P2 H8A 123.7 . . ? O6 P2 H8A 80.0 . . ? O8 P2 H8A 28.1 . . ? P2 O7 Fe2 132.3(4) . . ? P2 O8 H8A 97.6 . . ? P2 O8 H8B 110.3 . . ? H8A O8 H8B 121.3 . . ? O6 P2' O7' 110.8(6) . . ? O6 P2' O5 108.9(5) . . ? O7' P2' O5 111.2(6) . . ? O6 P2' O8' 109.8(10) . . ? O7' P2' O8' 109.6(11) . . ? O5 P2' O8' 106.4(10) . . ? P2' O7' Fe2 135.1(5) . . ? O9 P3 O11 121.1(3) . . ? O9 P3 O12 98.0(3) . . ? O11 P3 O12 113.6(3) . . ? O9 P3 O10 111.9(2) . . ? O11 P3 O10 97.9(2) . . ? O12 P3 O10 115.5(3) . . ? O9 P3 Fe2 45.82(16) . . ? O11 P3 Fe2 129.50(16) . . ? O12 P3 Fe2 52.6(2) . . ? O10 P3 Fe2 132.55(16) . . ? P3 O12 Fe2 92.5(3) . . ? O10 P3' O12' 115.0(3) . . ? O10 P3' O11 108.9(2) . . ? O12' P3' O11 111.3(3) . . ? O10 P3' O9 113.6(3) . . ? O12' P3' O9 100.0(3) . . ? O11 P3' O9 107.7(2) . . ? P3' O12' O21' 94.0(4) . 1_455 ? P3' O12' Fe2 156.7(4) . 1_455 ? O21' O12' Fe2 62.7(3) 1_455 1_455 ? O12' O21' Fe2 64.6(3) 1_655 . ? P3 O9 P3' 39.04(15) . . ? P3 O9 Fe2 105.2(2) . . ? P3' O9 Fe2 144.2(3) . . ? P3' O10 P3 36.56(14) . . ? P3' O10 Fe2 141.5(2) . 2_455 ? P3 O10 Fe2 131.8(2) . 2_455 ? P3 O11 P3' 37.93(13) . . ? P3 O11 Fe3 138.3(2) . . ? P3' O11 Fe3 141.3(2) . . ? O16 P4 O15 110.70(17) . . ? O16 P4 O13 105.83(19) . . ? O15 P4 O13 111.42(18) . . ? O16 P4 O14 111.43(18) . . ? O15 P4 O14 106.91(17) . . ? O13 P4 O14 110.63(18) . . ? P4 O13 Fe3 145.7(2) . . ? P4 O14 Fe1 142.87(19) . . ? P4 O15 Fe1 133.68(18) . 1_455 ? P4 O16 Fe1 150.5(2) . 2_456 ? C2 N1 C1 111.5(4) . . ? C2 N1 H1A 109.3 . . ? C1 N1 H1A 109.3 . . ? C2 N1 H1B 109.3 . . ? C1 N1 H1B 109.3 . . ? H1A N1 H1B 108.0 . . ? N1 C2 C1 111.1(4) . 2_466 ? N1 C2 H2C 109.4 . . ? C1 C2 H2C 109.4 2_466 . ? N1 C2 H2D 109.4 . . ? C1 C2 H2D 109.4 2_466 . ? H2C C2 H2D 108.0 . . ? C2 C1 N1 110.7(4) 2_466 . ? C2 C1 H1C 109.5 2_466 . ? N1 C1 H1C 109.5 . . ? C2 C1 H1D 109.5 2_466 . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? C4 N2 C3 111.1(4) 2_445 . ? C4 N2 H2A 109.4 2_445 . ? C3 N2 H2A 109.4 . . ? C4 N2 H2B 109.4 2_445 . ? C3 N2 H2B 109.4 . . ? H2A N2 H2B 108.0 . . ? N2 C4 C3 110.5(5) 2_445 . ? N2 C4 H4A 109.6 2_445 . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 2_445 . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C3 N2 111.1(5) . . ? C4 C3 H3A 109.4 . . ? N2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? N2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? 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 O16 Fe1 P1 O4 90.5(2) 2_456 . . . ? O5 Fe1 P1 O4 -98.7(2) . . . . ? O14 Fe1 P1 O4 -8.11(19) . . . . ? O15 Fe1 P1 O4 177.62(19) 1_655 . . . ? O2 Fe1 P1 O4 83.2(2) . . . . ? O3 Fe1 P1 O4 -91.9(2) . . . . ? O16 Fe1 P1 O1 -84.1(2) 2_456 . . . ? O5 Fe1 P1 O1 86.7(2) . . . . ? O14 Fe1 P1 O1 177.4(2) . . . . ? O15 Fe1 P1 O1 3.1(2) 1_655 . . . ? O2 Fe1 P1 O1 -91.4(2) . . . . ? O3 Fe1 P1 O1 93.6(2) . . . . ? O16 Fe1 P1 O2 7.3(2) 2_456 . . . ? O5 Fe1 P1 O2 178.09(18) . . . . ? O14 Fe1 P1 O2 -91.30(17) . . . . ? O15 Fe1 P1 O2 94.43(17) 1_655 . . . ? O3 Fe1 P1 O2 -175.1(2) . . . . ? O16 Fe1 P1 O3 -177.6(2) 2_456 . . . ? O5 Fe1 P1 O3 -6.83(19) . . . . ? O14 Fe1 P1 O3 83.79(17) . . . . ? O15 Fe1 P1 O3 -90.49(17) 1_655 . . . ? O2 Fe1 P1 O3 175.1(2) . . . . ? O4 P1 O1 Fe3 -157.3(4) . . . 1_655 ? O2 P1 O1 Fe3 -32.7(5) . . . 1_655 ? O3 P1 O1 Fe3 79.4(5) . . . 1_655 ? Fe1 P1 O1 Fe3 18.4(5) . . . 1_655 ? O4 P1 O2 Fe1 -124.86(15) . . . . ? O1 P1 O2 Fe1 113.91(19) . . . . ? O3 P1 O2 Fe1 -4.10(18) . . . . ? O16 Fe1 O2 P1 -174.87(14) 2_456 . . . ? O5 Fe1 O2 P1 -4.0(4) . . . . ? O14 Fe1 O2 P1 91.55(15) . . . . ? O15 Fe1 O2 P1 -83.62(15) 1_655 . . . ? O3 Fe1 O2 P1 2.99(13) . . . . ? O4 P1 O3 Fe2 -72.0(3) . . . . ? O1 P1 O3 Fe2 47.7(3) . . . . ? O2 P1 O3 Fe2 167.5(2) . . . . ? Fe1 P1 O3 Fe2 163.9(3) . . . . ? O4 P1 O3 Fe1 124.16(15) . . . . ? O1 P1 O3 Fe1 -116.18(15) . . . . ? O2 P1 O3 Fe1 3.59(15) . . . . ? O7' Fe2 O3 P1 -163.5(4) . . . . ? O10 Fe2 O3 P1 -55(2) 2_455 . . . ? O9 Fe2 O3 P1 95.0(3) . . . . ? O21' Fe2 O3 P1 -11.2(3) . . . . ? O12' Fe2 O3 P1 -63.6(3) 1_655 . . . ? O7 Fe2 O3 P1 175.2(3) . . . . ? O21 Fe2 O3 P1 -102.7(3) . . . . ? O12 Fe2 O3 P1 31.3(3) . . . . ? P3 Fe2 O3 P1 66.2(3) . . . . ? O7' Fe2 O3 Fe1 -5.4(3) . . . . ? O10 Fe2 O3 Fe1 103.5(19) 2_455 . . . ? O9 Fe2 O3 Fe1 -106.9(2) . . . . ? O21' Fe2 O3 Fe1 146.9(3) . . . . ? O12' Fe2 O3 Fe1 94.5(3) 1_655 . . . ? O7 Fe2 O3 Fe1 -26.7(3) . . . . ? O21 Fe2 O3 Fe1 55.4(2) . . . . ? O12 Fe2 O3 Fe1 -170.6(2) . . . . ? P3 Fe2 O3 Fe1 -135.6(2) . . . . ? O16 Fe1 O3 P1 10.3(9) 2_456 . . . ? O5 Fe1 O3 P1 174.32(15) . . . . ? O14 Fe1 O3 P1 -97.83(15) . . . . ? O15 Fe1 O3 P1 86.85(15) 1_655 . . . ? O2 Fe1 O3 P1 -2.91(13) . . . . ? O16 Fe1 O3 Fe2 -154.6(7) 2_456 . . . ? O5 Fe1 O3 Fe2 9.5(2) . . . . ? O14 Fe1 O3 Fe2 97.4(2) . . . . ? O15 Fe1 O3 Fe2 -78.0(2) 1_655 . . . ? O2 Fe1 O3 Fe2 -167.7(2) . . . . ? P1 Fe1 O3 Fe2 -164.8(3) . . . . ? O1 P1 O4 Fe3 -166.8(2) . . . . ? O2 P1 O4 Fe3 68.5(3) . . . . ? O3 P1 O4 Fe3 -45.0(3) . . . . ? Fe1 P1 O4 Fe3 18.0(3) . . . . ? O13 Fe3 O4 P1 -39.1(3) . . . . ? O6 Fe3 O4 P1 -156.8(3) 1_445 . . . ? O11 Fe3 O4 P1 91.7(3) . . . . ? O1 Fe3 O4 P1 111(3) 1_455 . . . ? O16 Fe1 O5 P2 -164.5(3) 2_456 . . . ? O14 Fe1 O5 P2 -72.5(4) . . . . ? O15 Fe1 O5 P2 104.2(4) 1_655 . . . ? O2 Fe1 O5 P2 24.5(6) . . . . ? O3 Fe1 O5 P2 18.0(4) . . . . ? P1 Fe1 O5 P2 21.8(4) . . . . ? O16 Fe1 O5 P2' 137.2(5) 2_456 . . . ? O14 Fe1 O5 P2' -130.8(5) . . . . ? O15 Fe1 O5 P2' 45.9(5) 1_655 . . . ? O2 Fe1 O5 P2' -33.8(6) . . . . ? O3 Fe1 O5 P2' -40.3(5) . . . . ? P1 Fe1 O5 P2' -36.5(5) . . . . ? P2' O5 P2 O7 80.6(6) . . . . ? Fe1 O5 P2 O7 -11.5(5) . . . . ? P2' O5 P2 O6 -56.6(5) . . . . ? Fe1 O5 P2 O6 -148.7(3) . . . . ? P2' O5 P2 O8 -174.0(5) . . . . ? Fe1 O5 P2 O8 93.9(4) . . . . ? P2' O6 P2 O7 -78.6(6) . . . . ? Fe3 O6 P2 O7 100.8(5) 1_665 . . . ? P2' O6 P2 O5 58.9(5) . . . . ? Fe3 O6 P2 O5 -121.7(4) 1_665 . . . ? P2' O6 P2 O8 176.2(6) . . . . ? Fe3 O6 P2 O8 -4.4(5) 1_665 . . . ? O5 P2 O7 Fe2 -27.9(7) . . . . ? O6 P2 O7 Fe2 106.7(5) . . . . ? O8 P2 O7 Fe2 -140.6(5) . . . . ? O7' Fe2 O7 P2 -55.1(8) . . . . ? O10 Fe2 O7 P2 -137.1(5) 2_455 . . . ? O9 Fe2 O7 P2 130.2(6) . . . . ? O3 Fe2 O7 P2 39.7(5) . . . . ? O21' Fe2 O7 P2 -68(2) . . . . ? O12' Fe2 O7 P2 -58.5(6) 1_655 . . . ? O21 Fe2 O7 P2 -40.7(5) . . . . ? O12 Fe2 O7 P2 130.3(5) . . . . ? P3 Fe2 O7 P2 127.4(5) . . . . ? P2 O6 P2' O7' 67.7(6) . . . . ? Fe3 O6 P2' O7' -110(3) 1_665 . . . ? P2 O6 P2' O5 -54.9(4) . . . . ? Fe3 O6 P2' O5 127(2) 1_665 . . . ? P2 O6 P2' O8' -171.0(12) . . . . ? Fe3 O6 P2' O8' 11(3) 1_665 . . . ? P2 O5 P2' O6 57.0(4) . . . . ? Fe1 O5 P2' O6 -170.8(3) . . . . ? P2 O5 P2' O7' -65.4(6) . . . . ? Fe1 O5 P2' O7' 66.8(7) . . . . ? P2 O5 P2' O8' 175.3(12) . . . . ? Fe1 O5 P2' O8' -52.5(11) . . . . ? O6 P2' O7' Fe2 175.9(5) . . . . ? O5 P2' O7' Fe2 -62.9(10) . . . . ? O8' P2' O7' Fe2 54.5(13) . . . . ? O10 Fe2 O7' P2' -143.5(8) 2_455 . . . ? O9 Fe2 O7' P2' 124.5(8) . . . . ? O3 Fe2 O7' P2' 32.6(8) . . . . ? O21' Fe2 O7' P2' -64.0(10) . . . . ? O12' Fe2 O7' P2' -63.8(8) 1_655 . . . ? O7 Fe2 O7' P2' 119.2(13) . . . . ? O21 Fe2 O7' P2' -44.7(7) . . . . ? O12 Fe2 O7' P2' 131.5(10) . . . . ? P3 Fe2 O7' P2' 122.2(7) . . . . ? O7' Fe2 P3 O9 4.6(4) . . . . ? O10 Fe2 P3 O9 -85.9(3) 2_455 . . . ? O3 Fe2 P3 O9 97.7(3) . . . . ? O21' Fe2 P3 O9 -172.4(3) . . . . ? O12' Fe2 P3 O9 -167.6(3) 1_655 . . . ? O7 Fe2 P3 O9 5.8(3) . . . . ? O21 Fe2 P3 O9 139.6(6) . . . . ? O12 Fe2 P3 O9 -171.2(4) . . . . ? O7' Fe2 P3 O11 -92.9(3) . . . . ? O10 Fe2 P3 O11 176.6(2) 2_455 . . . ? O9 Fe2 P3 O11 -97.6(3) . . . . ? O3 Fe2 P3 O11 0.1(2) . . . . ? O21' Fe2 P3 O11 90.0(3) . . . . ? O12' Fe2 P3 O11 94.8(3) 1_655 . . . ? O7 Fe2 P3 O11 -91.8(3) . . . . ? O21 Fe2 P3 O11 42.0(7) . . . . ? O12 Fe2 P3 O11 91.3(3) . . . . ? O7' Fe2 P3 O12 175.8(4) . . . . ? O10 Fe2 P3 O12 85.3(3) 2_455 . . . ? O9 Fe2 P3 O12 171.2(4) . . . . ? O3 Fe2 P3 O12 -91.1(3) . . . . ? O21' Fe2 P3 O12 -1.2(3) . . . . ? O12' Fe2 P3 O12 3.6(4) 1_655 . . . ? O7 Fe2 P3 O12 177.0(3) . . . . ? O21 Fe2 P3 O12 -49.2(7) . . . . ? O7' Fe2 P3 O10 83.8(4) . . . . ? O10 Fe2 P3 O10 -6.7(3) 2_455 . . . ? O9 Fe2 P3 O10 79.2(3) . . . . ? O3 Fe2 P3 O10 176.9(2) . . . . ? O21' Fe2 P3 O10 -93.2(3) . . . . ? O12' Fe2 P3 O10 -88.4(3) 1_655 . . . ? O7 Fe2 P3 O10 85.0(3) . . . . ? O21 Fe2 P3 O10 -141.2(6) . . . . ? O12 Fe2 P3 O10 -92.0(3) . . . . ? O9 P3 O12 Fe2 6.4(3) . . . . ? O11 P3 O12 Fe2 -122.7(2) . . . . ? O10 P3 O12 Fe2 125.3(2) . . . . ? O7' Fe2 O12 P3 -12.4(11) . . . . ? O10 Fe2 O12 P3 -96.9(3) 2_455 . . . ? O9 Fe2 O12 P3 -4.8(2) . . . . ? O3 Fe2 O12 P3 87.3(3) . . . . ? O21' Fe2 O12 P3 178.2(5) . . . . ? O12' Fe2 O12 P3 -177.3(3) 1_655 . . . ? O7 Fe2 O12 P3 -4.9(5) . . . . ? O21 Fe2 O12 P3 163.0(2) . . . . ? O10 P3' O12' O21' 61.5(4) . . . 1_455 ? O11 P3' O12' O21' -62.9(4) . . . 1_455 ? O9 P3' O12' O21' -176.4(3) . . . 1_455 ? O10 P3' O12' Fe2 58.4(10) . . . 1_455 ? O11 P3' O12' Fe2 -66.0(10) . . . 1_455 ? O9 P3' O12' Fe2 -179.6(9) . . . 1_455 ? O7' Fe2 O21' O12' 0.2(7) . . . 1_655 ? O10 Fe2 O21' O12' 79.5(3) 2_455 . . 1_655 ? O9 Fe2 O21' O12' 171.5(3) . . . 1_655 ? O3 Fe2 O21' O12' -97.7(3) . . . 1_655 ? O7 Fe2 O21' O12' 10(2) . . . 1_655 ? O21 Fe2 O21' O12' -16.8(3) . . . 1_655 ? O12 Fe2 O21' O12' 174.3(4) . . . 1_655 ? P3 Fe2 O21' O12' 175.4(3) . . . 1_655 ? O11 P3 O9 P3' -63.1(2) . . . . ? O12 P3 O9 P3' 173.1(3) . . . . ? O10 P3 O9 P3' 51.4(2) . . . . ? Fe2 P3 O9 P3' -179.8(2) . . . . ? O11 P3 O9 Fe2 116.7(2) . . . . ? O12 P3 O9 Fe2 -7.1(3) . . . . ? O10 P3 O9 Fe2 -128.8(2) . . . . ? O10 P3' O9 P3 -67.9(3) . . . . ? O12' P3' O9 P3 169.1(3) . . . . ? O11 P3' O9 P3 52.8(2) . . . . ? O10 P3' O9 Fe2 -68.2(5) . . . . ? O12' P3' O9 Fe2 168.7(4) . . . . ? O11 P3' O9 Fe2 52.4(5) . . . . ? O7' Fe2 O9 P3 -176.4(3) . . . . ? O10 Fe2 O9 P3 96.2(2) 2_455 . . . ? O3 Fe2 O9 P3 -81.7(2) . . . . ? O21' Fe2 O9 P3 7.7(3) . . . . ? O12' Fe2 O9 P3 25.6(6) 1_655 . . . ? O7 Fe2 O9 P3 -174.4(3) . . . . ? O21 Fe2 O9 P3 -146.4(5) . . . . ? O12 Fe2 O9 P3 5.6(2) . . . . ? O7' Fe2 O9 P3' -176.2(5) . . . . ? O10 Fe2 O9 P3' 96.4(4) 2_455 . . . ? O3 Fe2 O9 P3' -81.5(4) . . . . ? O21' Fe2 O9 P3' 7.9(5) . . . . ? O12' Fe2 O9 P3' 25.8(8) 1_655 . . . ? O7 Fe2 O9 P3' -174.2(5) . . . . ? O21 Fe2 O9 P3' -146.2(6) . . . . ? O12 Fe2 O9 P3' 5.8(4) . . . . ? P3 Fe2 O9 P3' 0.2(3) . . . . ? O12' P3' O10 P3 166.9(4) . . . . ? O11 P3' O10 P3 -67.4(2) . . . . ? O9 P3' O10 P3 52.5(2) . . . . ? O12' P3' O10 Fe2 71.0(5) . . . 2_455 ? O11 P3' O10 Fe2 -163.3(3) . . . 2_455 ? O9 P3' O10 Fe2 -43.4(5) . . . 2_455 ? O9 P3 O10 P3' -65.5(3) . . . . ? O11 P3 O10 P3' 62.6(2) . . . . ? O12 P3 O10 P3' -176.5(4) . . . . ? Fe2 P3 O10 P3' -114.9(3) . . . . ? O9 P3 O10 Fe2 58.3(4) . . . 2_455 ? O11 P3 O10 Fe2 -173.6(2) . . . 2_455 ? O12 P3 O10 Fe2 -52.7(4) . . . 2_455 ? Fe2 P3 O10 Fe2 8.9(4) . . . 2_455 ? O9 P3 O11 P3' 68.7(3) . . . . ? O12 P3 O11 P3' -175.2(3) . . . . ? O10 P3 O11 P3' -52.8(2) . . . . ? Fe2 P3 O11 P3' 124.8(3) . . . . ? O9 P3 O11 Fe3 -49.3(4) . . . . ? O12 P3 O11 Fe3 66.9(4) . . . . ? O10 P3 O11 Fe3 -170.8(3) . . . . ? Fe2 P3 O11 Fe3 6.8(4) . . . . ? O10 P3' O11 P3 77.4(2) . . . . ? O12' P3' O11 P3 -154.8(4) . . . . ? O9 P3' O11 P3 -46.1(2) . . . . ? O10 P3' O11 Fe3 -172.6(3) . . . . ? O12' P3' O11 Fe3 -44.9(5) . . . . ? O9 P3' O11 Fe3 63.8(4) . . . . ? O13 Fe3 O11 P3 44.5(4) . . . . ? O6 Fe3 O11 P3 -134.9(3) 1_445 . . . ? O4 Fe3 O11 P3 -45.9(3) . . . . ? O1 Fe3 O11 P3 135.0(3) 1_455 . . . ? O13 Fe3 O11 P3' -15.8(4) . . . . ? O6 Fe3 O11 P3' 164.8(3) 1_445 . . . ? O4 Fe3 O11 P3' -106.2(3) . . . . ? O1 Fe3 O11 P3' 74.7(3) 1_455 . . . ? O16 P4 O13 Fe3 159.5(3) . . . . ? O15 P4 O13 Fe3 39.1(4) . . . . ? O14 P4 O13 Fe3 -79.7(4) . . . . ? O6 Fe3 O13 P4 -162.9(3) 1_445 . . . ? O11 Fe3 O13 P4 17.7(4) . . . . ? O4 Fe3 O13 P4 107.9(4) . . . . ? O1 Fe3 O13 P4 -70.8(4) 1_455 . . . ? O16 P4 O14 Fe1 83.4(3) . . . . ? O15 P4 O14 Fe1 -155.5(3) . . . . ? O13 P4 O14 Fe1 -34.1(4) . . . . ? O16 Fe1 O14 P4 -97.1(3) 2_456 . . . ? O5 Fe1 O14 P4 164.0(3) . . . . ? O15 Fe1 O14 P4 129.2(12) 1_655 . . . ? O2 Fe1 O14 P4 7.1(3) . . . . ? O3 Fe1 O14 P4 74.2(3) . . . . ? P1 Fe1 O14 P4 40.4(3) . . . . ? O16 P4 O15 Fe1 -34.1(3) . . . 1_455 ? O13 P4 O15 Fe1 83.4(3) . . . 1_455 ? O14 P4 O15 Fe1 -155.7(2) . . . 1_455 ? O15 P4 O16 Fe1 -96.5(4) . . . 2_456 ? O13 P4 O16 Fe1 142.6(4) . . . 2_456 ? O14 P4 O16 Fe1 22.3(5) . . . 2_456 ? C1 N1 C2 C1 56.1(6) . . . 2_466 ? C2 N1 C1 C2 -55.9(5) . . . 2_466 ? N2 C4 C3 N2 -56.3(7) 2_445 . . . ? C4 N2 C3 C4 56.6(8) 2_445 . . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 1.307 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.159