# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Jihong Yu' _publ_contact_author_email JIHONG@MAIL.JLU.EDU.CN _publ_section_title ; Synthesis, structure and magnetic property of a new organo-templated mixed-valent iron (II, III) borophosphate ; _publ_author_name 'Jihong Yu' # Attachment 'FeBPO-CJ28.cif' # 1. SUBMISSION DETAILS data_FeBPO-CJ28 _database_code_depnum_ccdc_archive 'CCDC 706743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'B4 Fe2 P7 O26 (OH)4, (C4 N3 H16) (C4 N3 H15)0.5' _chemical_formula_sum 'C6 H27.50 B4 Fe2 N4.50 O30 P7' _chemical_formula_weight 1014.55 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' B B 0.0013 0.0007 '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 8.9568(3) _cell_length_b 9.8717(3) _cell_length_c 17.9905(5) _cell_angle_alpha 102.510(2) _cell_angle_beta 92.343(2) _cell_angle_gamma 100.403(2) _cell_volume 1522.10(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.31 _exptl_crystal_description rod _exptl_crystal_colour light-brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.449 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11183 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7505 _reflns_number_gt 5703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _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^)+(0.0546P)^2^+2.0586P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7505 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 0.81263(6) 0.73365(5) 0.36089(3) 0.01079(12) Uani 1 1 d . . . Fe2 Fe 1.34922(6) 1.13455(5) 0.29687(3) 0.01020(12) Uani 1 1 d . . . P1 P 1.00277(10) 0.49873(10) 0.27921(5) 0.01139(19) Uani 1 1 d . . . P2 P 0.56393(10) 0.43593(9) 0.30376(5) 0.01011(18) Uani 1 1 d . . . P3 P 1.00724(10) 0.96776(10) 0.28283(5) 0.01192(19) Uani 1 1 d . . . P4 P 0.54796(11) 0.87454(10) 0.29949(5) 0.01217(19) Uani 1 1 d . . . P5 P 1.21031(11) 1.27083(10) 0.45310(5) 0.0136(2) Uani 1 1 d . . . P6 P 0.74579(12) 0.60984(11) 0.06678(6) 0.0180(2) Uani 1 1 d . . . P7 P 1.30706(12) 1.18908(11) 0.12745(5) 0.0156(2) Uani 1 1 d . . . B1 B 0.7559(5) 0.7904(4) 0.2000(2) 0.0117(8) Uani 1 1 d . . . B2 B 0.7501(4) 0.5301(4) 0.1990(2) 0.0109(7) Uani 1 1 d . . . B3 B 1.0563(4) 1.2605(4) 0.3180(2) 0.0112(7) Uani 1 1 d . . . B4 B 1.2614(4) 1.3946(4) 0.2480(2) 0.0101(7) Uani 1 1 d . . . O1 O 1.4375(4) 1.2269(4) 0.07475(18) 0.0336(8) Uani 1 1 d . . . H1 H 1.4066 1.2676 0.0438 0.080 Uiso 1 1 calc . . . O2 O 1.1719(4) 1.0946(3) 0.07996(19) 0.0349(8) Uani 1 1 d . . . O3 O 1.3100(4) 1.4221(3) 0.48354(17) 0.0322(8) Uani 1 1 d . . . H3 H 1.3437 1.4529 0.4475 0.080 Uiso 1 1 calc . . . O4 O 0.9056(3) 0.6254(4) 0.04442(18) 0.0302(7) Uani 1 1 d . . . O5 O 0.6304(3) 0.5631(3) -0.00338(16) 0.0258(7) Uani 1 1 d . . . H5 H 0.6435 0.6223 -0.0294 0.080 Uiso 1 1 calc . . . O6 O 0.9903(3) 0.6167(3) 0.34476(15) 0.0194(6) Uani 1 1 d . . . O7 O 0.4095(3) 0.7495(3) 0.26980(18) 0.0265(7) Uani 1 1 d . . . H7 H 0.4405 0.6753 0.2572 0.080 Uiso 1 1 calc . . . O8 O 0.8519(3) 0.7865(3) 0.48144(14) 0.0184(6) Uani 1 1 d . . . O9 O 1.2687(3) 1.3347(3) 0.16622(15) 0.0218(6) Uani 1 1 d . . . O10 O 1.0746(3) 1.2911(3) 0.40196(15) 0.0225(6) Uani 1 1 d . . . O11 O 1.1673(3) 0.5042(3) 0.25431(15) 0.0138(5) Uani 1 1 d . . . O12 O 0.9679(3) 1.1172(3) 0.28749(16) 0.0181(6) Uani 1 1 d . . . O13 O 0.7077(3) 0.4980(3) 0.11588(14) 0.0148(5) Uani 1 1 d . . . O14 O 0.9541(3) 0.3503(3) 0.29594(15) 0.0150(5) Uani 1 1 d . . . O15 O 1.3014(3) 1.1746(3) 0.40528(15) 0.0190(6) Uani 1 1 d . . . O16 O 0.7111(3) 0.7485(3) 0.11720(14) 0.0159(5) Uani 1 1 d . . . O17 O 1.4862(3) 1.0094(3) 0.31587(16) 0.0187(6) Uani 1 1 d . . . O18 O 0.4108(3) 0.4796(3) 0.28311(16) 0.0168(6) Uani 1 1 d . . . O19 O 1.2048(3) 1.2827(3) 0.28709(14) 0.0115(5) Uani 1 1 d . . . O20 O 1.5309(3) 1.2917(3) 0.32200(15) 0.0147(5) Uani 1 1 d . . . O21 O 0.6513(3) 0.8855(3) 0.23259(15) 0.0185(6) Uani 1 1 d . . . O22 O 0.6522(3) 0.4229(3) 0.23017(14) 0.0142(5) Uani 1 1 d . . . O23 O 1.3806(3) 1.1258(3) 0.18567(15) 0.0190(6) Uani 1 1 d . . . O24 O 0.9632(3) 0.9148(3) 0.35235(15) 0.0198(6) Uani 1 1 d . . . O25 O 0.6525(3) 0.5506(3) 0.36763(14) 0.0160(5) Uani 1 1 d . . . O26 O 0.6333(3) 0.8500(3) 0.36709(15) 0.0194(6) Uani 1 1 d . . . O27 O 1.1740(3) 0.9778(3) 0.26812(16) 0.0175(6) Uani 1 1 d . . . O28 O 0.7419(3) 0.6718(3) 0.23627(13) 0.0105(5) Uani 1 1 d . . . O29 O 0.9126(3) 0.8735(3) 0.20884(15) 0.0169(6) Uani 1 1 d . . . O30 O 0.9093(3) 0.5023(3) 0.20608(14) 0.0140(5) Uani 1 1 d . . . C1 C 0.7323(7) 0.2422(7) -0.1160(3) 0.0518(15) Uani 1 1 d . . . H1A H 0.6304 0.2312 -0.1398 0.080 Uiso 1 1 calc . . . H1B H 0.7819 0.1732 -0.1472 0.080 Uiso 1 1 calc . . . C2 C 0.7201(6) 0.2101(6) -0.0405(3) 0.0362(11) Uani 1 1 d . . . H2A H 0.6372 0.1301 -0.0441 0.080 Uiso 1 1 calc . . . H2B H 0.6940 0.2905 -0.0057 0.080 Uiso 1 1 calc . . . C3 C 0.8618(5) 0.1983(5) 0.0765(3) 0.0288(10) Uani 1 1 d . . . H3A H 0.8373 0.2903 0.0968 0.080 Uiso 1 1 calc . . . H3B H 0.9629 0.1989 0.0983 0.080 Uiso 1 1 calc . . . C4 C 0.7496(6) 0.0875(5) 0.1012(3) 0.0358(12) Uani 1 1 d . . . H4A H 0.6556 0.0658 0.0685 0.080 Uiso 1 1 calc . . . H4B H 0.7903 0.0016 0.0961 0.080 Uiso 1 1 calc . . . N1 N 0.8168(5) 0.3847(6) -0.1158(3) 0.0487(12) Uani 1 1 d . . . H1C H 0.8196 0.3956 -0.1636 0.080 Uiso 1 1 calc . . . H1D H 0.9114 0.3955 -0.0951 0.080 Uiso 1 1 calc . . . H1E H 0.7705 0.4492 -0.0887 0.080 Uiso 1 1 calc . . . N2 N 0.8638(4) 0.1763(4) -0.0068(2) 0.0278(8) Uani 1 1 d . . . H2C H 0.8695 0.0858 -0.0272 0.080 Uiso 1 1 calc . . . H2D H 0.9463 0.2325 -0.0183 0.080 Uiso 1 1 calc . . . N3 N 0.7180(4) 0.1380(4) 0.1820(2) 0.0221(7) Uani 1 1 d . . . H3C H 0.6513 0.0715 0.1958 0.080 Uiso 1 1 calc . . . H3D H 0.6797 0.2163 0.1865 0.080 Uiso 1 1 calc . . . H3E H 0.8042 0.1567 0.2119 0.080 Uiso 1 1 calc . . . N4 N 0.4830(9) 1.0416(8) 0.4968(4) 0.0252(16) Uiso 0.50 1 d P . . N5 N 0.1519(9) 0.9210(8) 0.5094(4) 0.0283(16) Uiso 0.50 1 d P A -1 C5 C 0.4226(11) 0.8897(9) 0.4968(5) 0.0241(18) Uiso 0.50 1 d P . -1 C6 C 0.2595(13) 0.8450(12) 0.4631(6) 0.039(2) Uiso 0.50 1 d P A -1 N5' N 0.1667(13) 0.6846(12) 0.4864(6) 0.060(3) Uiso 0.50 1 d P B -2 C5' C 0.3504(12) 0.9097(10) 0.4857(5) 0.029(2) Uiso 0.50 1 d P . -2 C6' C 0.3173(16) 0.7546(15) 0.4941(8) 0.057(3) Uiso 0.50 1 d P B -2 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 0.0124(3) 0.0091(2) 0.0113(2) 0.00310(19) 0.00218(19) 0.00188(19) Fe2 0.0103(2) 0.0084(2) 0.0131(2) 0.00432(19) 0.00292(19) 0.00218(19) P1 0.0103(4) 0.0093(4) 0.0157(4) 0.0043(3) 0.0021(3) 0.0027(3) P2 0.0100(4) 0.0075(4) 0.0126(4) 0.0028(3) 0.0014(3) 0.0005(3) P3 0.0116(4) 0.0074(4) 0.0167(5) 0.0042(3) 0.0022(3) -0.0001(3) P4 0.0122(4) 0.0089(4) 0.0168(5) 0.0042(3) 0.0023(3) 0.0038(3) P5 0.0157(5) 0.0149(5) 0.0107(4) 0.0038(3) 0.0022(3) 0.0025(4) P6 0.0202(5) 0.0177(5) 0.0151(5) 0.0039(4) 0.0000(4) 0.0011(4) P7 0.0213(5) 0.0149(5) 0.0110(4) 0.0016(4) 0.0029(4) 0.0057(4) B1 0.0140(19) 0.0107(19) 0.0111(18) 0.0039(14) 0.0016(15) 0.0021(15) B2 0.0103(18) 0.0088(18) 0.0142(19) 0.0036(14) 0.0013(15) 0.0019(14) B3 0.0105(18) 0.0101(18) 0.0140(19) 0.0053(15) 0.0009(15) 0.0019(15) B4 0.0125(18) 0.0065(17) 0.0135(18) 0.0053(14) 0.0040(15) 0.0034(14) O1 0.046(2) 0.038(2) 0.0285(17) 0.0196(15) 0.0225(15) 0.0203(16) O2 0.0348(18) 0.0240(17) 0.0389(19) -0.0050(14) -0.0150(15) 0.0060(14) O3 0.044(2) 0.0213(16) 0.0258(16) 0.0077(13) -0.0010(14) -0.0110(14) O4 0.0262(16) 0.0358(19) 0.0295(17) 0.0098(14) 0.0081(13) 0.0046(14) O5 0.0302(16) 0.0295(17) 0.0161(14) 0.0117(12) -0.0062(12) -0.0042(13) O6 0.0185(14) 0.0196(15) 0.0198(14) 0.0015(11) 0.0012(11) 0.0066(11) O7 0.0193(14) 0.0138(14) 0.0454(19) 0.0098(13) -0.0081(13) -0.0010(12) O8 0.0207(14) 0.0215(15) 0.0115(12) 0.0048(11) 0.0032(10) -0.0012(11) O9 0.0404(18) 0.0152(14) 0.0122(13) 0.0040(10) 0.0060(12) 0.0099(13) O10 0.0222(15) 0.0370(18) 0.0128(13) 0.0064(12) 0.0047(11) 0.0162(13) O11 0.0111(12) 0.0111(12) 0.0227(14) 0.0089(10) 0.0044(10) 0.0043(10) O12 0.0113(12) 0.0092(13) 0.0337(16) 0.0051(11) 0.0015(11) 0.0016(10) O13 0.0213(14) 0.0117(13) 0.0102(12) 0.0025(10) -0.0011(10) 0.0008(11) O14 0.0112(12) 0.0126(13) 0.0240(14) 0.0092(10) 0.0032(10) 0.0032(10) O15 0.0203(14) 0.0265(16) 0.0145(13) 0.0076(11) 0.0049(11) 0.0113(12) O16 0.0215(14) 0.0141(13) 0.0128(12) 0.0048(10) -0.0011(10) 0.0035(11) O17 0.0167(13) 0.0129(13) 0.0286(15) 0.0050(11) 0.0046(11) 0.0078(11) O18 0.0097(12) 0.0106(13) 0.0307(15) 0.0066(11) 0.0006(11) 0.0011(10) O19 0.0108(12) 0.0098(12) 0.0163(12) 0.0066(10) 0.0037(10) 0.0032(10) O20 0.0140(12) 0.0098(12) 0.0218(14) 0.0081(10) 0.0007(10) 0.0005(10) O21 0.0271(15) 0.0131(13) 0.0207(14) 0.0088(11) 0.0099(11) 0.0100(11) O22 0.0177(13) 0.0090(12) 0.0154(13) 0.0022(10) 0.0072(10) 0.0006(10) O23 0.0207(14) 0.0195(14) 0.0191(14) 0.0062(11) 0.0060(11) 0.0066(12) O24 0.0237(15) 0.0171(14) 0.0173(14) 0.0075(11) 0.0023(11) -0.0033(11) O25 0.0196(13) 0.0115(13) 0.0139(13) 0.0007(10) 0.0005(10) -0.0021(10) O26 0.0225(14) 0.0221(15) 0.0176(14) 0.0060(11) 0.0028(11) 0.0128(12) O27 0.0113(12) 0.0132(13) 0.0276(15) 0.0039(11) 0.0036(11) 0.0015(10) O28 0.0137(12) 0.0075(12) 0.0112(12) 0.0037(9) 0.0004(9) 0.0023(9) O29 0.0174(13) 0.0148(13) 0.0155(13) 0.0023(10) 0.0026(10) -0.0033(11) O30 0.0130(12) 0.0169(13) 0.0149(13) 0.0062(10) 0.0035(10) 0.0063(10) C1 0.055(4) 0.059(4) 0.041(3) 0.016(3) 0.000(3) 0.004(3) C2 0.032(3) 0.038(3) 0.043(3) 0.018(2) 0.001(2) 0.005(2) C3 0.034(2) 0.024(2) 0.026(2) 0.0036(18) 0.0047(19) 0.0024(19) C4 0.056(3) 0.022(2) 0.026(2) 0.0046(19) 0.008(2) 0.000(2) N1 0.040(3) 0.065(3) 0.052(3) 0.037(3) 0.007(2) 0.009(2) N2 0.034(2) 0.0198(19) 0.029(2) 0.0049(15) 0.0109(16) 0.0039(16) N3 0.0228(18) 0.0196(18) 0.0249(18) 0.0094(14) 0.0003(14) 0.0023(14) _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 O24 2.075(3) . ? Fe1 O8 2.117(3) . ? Fe1 O6 2.123(3) . ? Fe1 O25 2.124(3) . ? Fe1 O26 2.130(3) . ? Fe1 O28 2.225(2) . ? Fe2 O27 1.958(3) . ? Fe2 O17 1.961(3) . ? Fe2 O15 1.985(3) . ? Fe2 O20 1.996(3) . ? Fe2 O23 2.017(3) . ? Fe2 O19 2.149(2) . ? P1 O6 1.491(3) . ? P1 O30 1.541(3) . ? P1 O14 1.549(3) . ? P1 O11 1.553(3) . ? P2 O25 1.506(3) . ? P2 O20 1.510(3) 1_445 ? P2 O22 1.563(3) . ? P2 O18 1.564(3) . ? P3 O24 1.497(3) . ? P3 O27 1.517(3) . ? P3 O29 1.563(3) . ? P3 O12 1.563(3) . ? P4 O26 1.497(3) . ? P4 O17 1.508(3) 1_455 ? P4 O21 1.558(3) . ? P4 O7 1.566(3) . ? P5 O8 1.499(3) 2_776 ? P5 O15 1.513(3) . ? P5 O10 1.562(3) . ? P5 O3 1.566(3) . ? P6 O4 1.493(3) . ? P6 O5 1.531(3) . ? P6 O13 1.558(3) . ? P6 O16 1.559(3) . ? P7 O2 1.493(3) . ? P7 O23 1.516(3) . ? P7 O9 1.560(3) . ? P7 O1 1.578(3) . ? B1 O28 1.449(5) . ? B1 O16 1.474(5) . ? B1 O29 1.476(5) . ? B1 O21 1.493(5) . ? B2 O28 1.430(5) . ? B2 O22 1.472(5) . ? B2 O13 1.478(5) . ? B2 O30 1.505(5) . ? B3 O19 1.461(4) . ? B3 O12 1.468(5) . ? B3 O10 1.471(5) . ? B3 O14 1.481(5) 1_565 ? B4 O19 1.461(4) . ? B4 O9 1.472(5) . ? B4 O11 1.475(4) 1_565 ? B4 O18 1.480(5) 1_665 ? O1 H1 0.8200 . ? O3 H3 0.8200 . ? O5 H5 0.8200 . ? O7 H7 0.8200 . ? O8 P5 1.499(3) 2_776 ? O11 B4 1.475(4) 1_545 ? O14 B3 1.481(5) 1_545 ? O17 P4 1.508(3) 1_655 ? O18 B4 1.480(5) 1_445 ? O20 P2 1.510(3) 1_665 ? C1 C2 1.463(7) . ? C1 N1 1.472(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.522(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.469(6) . ? C3 C4 1.501(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.487(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8901 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? N3 H3E 0.8900 . ? N4 N4 0.952(14) 2_676 ? N4 C5 0.969(11) 2_676 ? N4 C5 1.499(12) . ? N4 C5' 1.481(13) 2_676 ? N5 C6 1.496(13) . ? C5 N4 0.969(11) 2_676 ? C5 C6 1.508(14) . ? N5' C6' 1.387(17) . ? C5' N4 1.481(13) 2_676 ? C5' C6' 1.548(17) . ? 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 O24 Fe1 O8 91.38(10) . . ? O24 Fe1 O6 90.10(11) . . ? O8 Fe1 O6 93.96(11) . . ? O24 Fe1 O25 178.00(11) . . ? O8 Fe1 O25 89.67(10) . . ? O6 Fe1 O25 91.52(11) . . ? O24 Fe1 O26 88.85(11) . . ? O8 Fe1 O26 90.72(11) . . ? O6 Fe1 O26 175.23(10) . . ? O25 Fe1 O26 89.45(11) . . ? O24 Fe1 O28 93.49(10) . . ? O8 Fe1 O28 173.15(10) . . ? O6 Fe1 O28 90.84(10) . . ? O25 Fe1 O28 85.32(9) . . ? O26 Fe1 O28 84.58(10) . . ? O27 Fe2 O17 92.60(11) . . ? O27 Fe2 O15 92.10(12) . . ? O17 Fe2 O15 91.92(11) . . ? O27 Fe2 O20 177.65(11) . . ? O17 Fe2 O20 86.86(11) . . ? O15 Fe2 O20 90.20(11) . . ? O27 Fe2 O23 90.30(11) . . ? O17 Fe2 O23 98.47(11) . . ? O15 Fe2 O23 169.21(11) . . ? O20 Fe2 O23 87.52(11) . . ? O27 Fe2 O19 90.30(10) . . ? O17 Fe2 O19 174.56(11) . . ? O15 Fe2 O19 83.37(10) . . ? O20 Fe2 O19 90.43(10) . . ? O23 Fe2 O19 86.11(10) . . ? O6 P1 O30 112.61(15) . . ? O6 P1 O14 113.50(16) . . ? O30 P1 O14 107.93(15) . . ? O6 P1 O11 113.21(15) . . ? O30 P1 O11 103.55(14) . . ? O14 P1 O11 105.28(14) . . ? O25 P2 O20 114.06(15) . 1_445 ? O25 P2 O22 110.41(15) . . ? O20 P2 O22 107.63(15) 1_445 . ? O25 P2 O18 108.51(15) . . ? O20 P2 O18 109.57(14) 1_445 . ? O22 P2 O18 106.39(15) . . ? O24 P3 O27 115.07(16) . . ? O24 P3 O29 111.74(15) . . ? O27 P3 O29 106.98(15) . . ? O24 P3 O12 110.65(16) . . ? O27 P3 O12 107.68(15) . . ? O29 P3 O12 104.05(15) . . ? O26 P4 O17 113.82(16) . 1_455 ? O26 P4 O21 111.57(16) . . ? O17 P4 O21 105.60(15) 1_455 . ? O26 P4 O7 110.13(17) . . ? O17 P4 O7 107.35(16) 1_455 . ? O21 P4 O7 108.09(17) . . ? O8 P5 O15 112.41(16) 2_776 . ? O8 P5 O10 108.69(16) 2_776 . ? O15 P5 O10 109.58(15) . . ? O8 P5 O3 109.95(16) 2_776 . ? O15 P5 O3 110.32(18) . . ? O10 P5 O3 105.66(18) . . ? O4 P6 O5 111.45(18) . . ? O4 P6 O13 112.81(17) . . ? O5 P6 O13 106.60(15) . . ? O4 P6 O16 113.12(17) . . ? O5 P6 O16 108.03(17) . . ? O13 P6 O16 104.34(14) . . ? O2 P7 O23 115.25(18) . . ? O2 P7 O9 110.99(18) . . ? O23 P7 O9 110.79(15) . . ? O2 P7 O1 109.9(2) . . ? O23 P7 O1 104.69(17) . . ? O9 P7 O1 104.44(17) . . ? O28 B1 O16 113.4(3) . . ? O28 B1 O29 112.8(3) . . ? O16 B1 O29 106.3(3) . . ? O28 B1 O21 109.8(3) . . ? O16 B1 O21 105.3(3) . . ? O29 B1 O21 108.9(3) . . ? O28 B2 O22 113.0(3) . . ? O28 B2 O13 112.9(3) . . ? O22 B2 O13 107.2(3) . . ? O28 B2 O30 111.9(3) . . ? O22 B2 O30 106.4(3) . . ? O13 B2 O30 105.0(3) . . ? O19 B3 O12 112.4(3) . . ? O19 B3 O10 110.4(3) . . ? O12 B3 O10 110.3(3) . . ? O19 B3 O14 113.2(3) . 1_565 ? O12 B3 O14 102.4(3) . 1_565 ? O10 B3 O14 107.7(3) . 1_565 ? O19 B4 O9 110.4(3) . . ? O19 B4 O11 113.8(3) . 1_565 ? O9 B4 O11 107.6(3) . 1_565 ? O19 B4 O18 112.3(3) . 1_665 ? O9 B4 O18 110.9(3) . 1_665 ? O11 B4 O18 101.5(3) 1_565 1_665 ? P7 O1 H1 109.5 . . ? P5 O3 H3 109.5 . . ? P6 O5 H5 109.5 . . ? P1 O6 Fe1 127.63(16) . . ? P4 O7 H7 109.5 . . ? P5 O8 Fe1 136.89(17) 2_776 . ? B4 O9 P7 128.5(2) . . ? B3 O10 P5 127.3(2) . . ? B4 O11 P1 128.7(2) 1_545 . ? B3 O12 P3 132.1(2) . . ? B2 O13 P6 122.6(2) . . ? B3 O14 P1 126.7(2) 1_545 . ? P5 O15 Fe2 135.44(17) . . ? B1 O16 P6 121.4(2) . . ? P4 O17 Fe2 154.44(19) 1_655 . ? B4 O18 P2 131.7(2) 1_445 . ? B3 O19 B4 125.4(3) . . ? B3 O19 Fe2 117.3(2) . . ? B4 O19 Fe2 117.3(2) . . ? P2 O20 Fe2 132.28(16) 1_665 . ? B1 O21 P4 128.5(2) . . ? B2 O22 P2 131.5(2) . . ? P7 O23 Fe2 131.44(16) . . ? P3 O24 Fe1 129.53(16) . . ? P2 O25 Fe1 128.88(15) . . ? P4 O26 Fe1 124.79(16) . . ? P3 O27 Fe2 131.77(16) . . ? B2 O28 B1 125.2(3) . . ? B2 O28 Fe1 115.7(2) . . ? B1 O28 Fe1 113.7(2) . . ? B1 O29 P3 129.1(2) . . ? B2 O30 P1 127.8(2) . . ? C2 C1 N1 115.0(5) . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? N1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 N2 114.5(4) . . ? C1 C2 H2A 108.6 . . ? N2 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? N2 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N2 C3 C4 113.5(4) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 110.4(4) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C1 N1 H1E 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C3 N2 C2 109.9(4) . . ? C3 N2 H2C 109.7 . . ? C2 N2 H2C 109.7 . . ? C3 N2 H2D 109.7 . . ? C2 N2 H2D 109.7 . . ? H2C N2 H2D 108.2 . . ? C4 N3 H3C 109.5 . . ? C4 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C4 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? N4 N4 C5 102.6(12) 2_676 2_676 ? N4 N4 C5 39.1(8) 2_676 . ? C5 N4 C5 141.7(8) 2_676 . ? N4 N4 C5' 76.8(10) 2_676 2_676 ? C5 N4 C5' 25.9(7) 2_676 2_676 ? C5 N4 C5' 115.9(6) . 2_676 ? N4 C5 N4 38.3(8) 2_676 . ? N4 C5 C6 147.3(11) 2_676 . ? N4 C5 C6 110.8(8) . . ? N5 C6 C5 113.4(8) . . ? N4 C5' C6' 105.4(9) 2_676 . ? N5' C6' C5' 118.1(11) . . ? 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 H1 O5 0.82 2.03 2.804(4) 156.1 2_775 O5 H5 O1 0.82 2.07 2.804(4) 149.1 2_775 O7 H7 O18 0.82 2.06 2.728(4) 138.8 . N1 H1C O11 0.89 2.08 2.930(5) 159.5 2_765 N1 H1D O4 0.89 1.91 2.780(6) 165.6 2_765 N1 H1E O5 0.89 2.26 3.127(6) 163.9 . N2 H2C O2 0.90 1.79 2.668(5) 163.6 2_765 N2 H2D O4 0.90 1.90 2.790(5) 169.0 2_765 N3 H3C O21 0.89 2.08 2.809(4) 138.3 1_545 N3 H3D O22 0.89 2.08 2.932(4) 158.8 . N3 H3E O12 0.89 2.10 2.940(4) 156.4 1_545 N3 H3E O14 0.89 2.32 3.041(4) 137.8 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.338 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.121