data_tjcag _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex PPh4 3(H2)0 ; _chemical_name_common ? _chemical_formula_moiety 'C19 H24 Fe N4 O5, P C24 H20, 3(H2 O)' _chemical_formula_sum 'C43 H48 Fe N4 O8 P' _chemical_formula_weight 835.67 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8668(3) _cell_length_b 15.9815(4) _cell_length_c 13.1301(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.1060(10) _cell_angle_gamma 90.00 _cell_volume 2062.22(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description 'Thin plate' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 878 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.7627 _exptl_absorpt_correction_T_max 0.9818 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 11294 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6817 _reflns_number_gt 6290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.8802P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.036(12) _refine_ls_number_reflns 6817 _refine_ls_number_parameters 532 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.61997(3) 0.33053(2) 0.17199(3) 0.01596(9) Uani 1 d . . . O1 O 0.7176(2) 0.08892(12) 0.15541(15) 0.0279(5) Uani 1 d . . . O2 O 0.81168(16) 0.33328(15) -0.08879(12) 0.0237(4) Uani 1 d . . . O3 O 0.6776(2) 0.57204(12) 0.09486(16) 0.0295(5) Uani 1 d . . . O4 O 0.5517(2) 0.44042(13) 0.43374(16) 0.0316(5) Uani 1 d . . . O5 O 0.42100(16) 0.33215(15) 0.10098(13) 0.0229(4) Uani 1 d . . . H5A H 0.375(3) 0.293(2) 0.080(2) 0.027 Uiso 1 d . . . H5B H 0.389(3) 0.373(2) 0.056(2) 0.027 Uiso 1 d . . . N1 N 0.6415(2) 0.21714(14) 0.20838(17) 0.0176(5) Uani 1 d . . . N2 N 0.7222(2) 0.30283(13) 0.06172(17) 0.0173(5) Uani 1 d . . . N3 N 0.6511(2) 0.44737(15) 0.17546(17) 0.0177(5) Uani 1 d . . . N4 N 0.5936(2) 0.34343(15) 0.31089(15) 0.0172(5) Uani 1 d . . . C1 C 0.6088(3) 0.19646(17) 0.3083(2) 0.0190(6) Uani 1 d . . . C2 C 0.6984(3) 0.16581(17) 0.1430(2) 0.0195(6) Uani 1 d . . . C3 C 0.7415(3) 0.21003(17) 0.0471(2) 0.0198(6) Uani 1 d . . . C4 C 0.7612(3) 0.35606(16) -0.0086(2) 0.0199(6) Uani 1 d . . . C5 C 0.7468(3) 0.45272(18) 0.0037(2) 0.0207(6) Uani 1 d . . . C6 C 0.6873(3) 0.49347(17) 0.0968(2) 0.0193(6) Uani 1 d . . . C7 C 0.6062(3) 0.48964(17) 0.2682(2) 0.0185(6) Uani 1 d . . . C8 C 0.5814(3) 0.42190(17) 0.3477(2) 0.0194(6) Uani 1 d . . . C9 C 0.5837(3) 0.26808(17) 0.3672(2) 0.0188(6) Uani 1 d . . . C10 C 0.5557(3) 0.26027(18) 0.4682(2) 0.0227(6) Uani 1 d . . . H10A H 0.5414 0.3085 0.5082 0.027 Uiso 1 calc R . . C11 C 0.5490(3) 0.18016(18) 0.5105(2) 0.0258(6) Uani 1 d . . . H11A H 0.5298 0.1741 0.5797 0.031 Uiso 1 calc R . . C12 C 0.5700(3) 0.10945(18) 0.4526(2) 0.0265(6) Uani 1 d . . . H12A H 0.5633 0.0555 0.4821 0.032 Uiso 1 calc R . . C13 C 0.6008(3) 0.11702(17) 0.3513(2) 0.0229(6) Uani 1 d . . . H13A H 0.6161 0.0685 0.3121 0.027 Uiso 1 calc R . . C14 C 0.8888(3) 0.18595(19) 0.0353(2) 0.0268(7) Uani 1 d . . . H14A H 0.9192 0.2134 -0.0253 0.040 Uiso 1 calc R . . H14B H 0.8954 0.1251 0.0277 0.040 Uiso 1 calc R . . H14C H 0.9464 0.2038 0.0961 0.040 Uiso 1 calc R . . C15 C 0.6460(3) 0.17730(18) -0.0419(2) 0.0262(6) Uani 1 d . . . H15A H 0.6688 0.2037 -0.1056 0.039 Uiso 1 calc R . . H15B H 0.5518 0.1907 -0.0301 0.039 Uiso 1 calc R . . H15C H 0.6563 0.1165 -0.0472 0.039 Uiso 1 calc R . . C16 C 0.8944(3) 0.4884(2) 0.0045(3) 0.0333(8) Uani 1 d . . . H16A H 0.9493 0.4684 0.0655 0.050 Uiso 1 calc R . . H16B H 0.8912 0.5497 0.0053 0.050 Uiso 1 calc R . . H16C H 0.9352 0.4694 -0.0569 0.050 Uiso 1 calc R . . C17 C 0.6624(4) 0.4850(2) -0.0926(2) 0.0340(7) Uani 1 d . . . H17A H 0.5697 0.4626 -0.0944 0.051 Uiso 1 calc R . . H17B H 0.7045 0.4665 -0.1536 0.051 Uiso 1 calc R . . H17C H 0.6593 0.5462 -0.0911 0.051 Uiso 1 calc R . . C18 C 0.4708(3) 0.53658(18) 0.2449(2) 0.0241(6) Uani 1 d . . . H18A H 0.4822 0.5803 0.1941 0.036 Uiso 1 calc R . . H18B H 0.4436 0.5621 0.3078 0.036 Uiso 1 calc R . . H18C H 0.4004 0.4972 0.2180 0.036 Uiso 1 calc R . . C19 C 0.7174(3) 0.54775(17) 0.3174(2) 0.0243(6) Uani 1 d . . . H19A H 0.7367 0.5918 0.2687 0.036 Uiso 1 calc R . . H19B H 0.8003 0.5153 0.3358 0.036 Uiso 1 calc R . . H19C H 0.6861 0.5733 0.3790 0.036 Uiso 1 calc R . . P P 1.06365(6) 0.33689(6) 0.58103(5) 0.02049(15) Uani 1 d . . . C21 C 0.9726(3) 0.24321(19) 0.6046(2) 0.0229(7) Uani 1 d . . . C22 C 0.9840(3) 0.17415(19) 0.5399(2) 0.0310(7) Uani 1 d . . . H22A H 1.0299 0.1797 0.4797 0.037 Uiso 1 calc R . . C23 C 0.9285(3) 0.0979(2) 0.5639(3) 0.0370(8) Uani 1 d . . . H23A H 0.9374 0.0511 0.5204 0.044 Uiso 1 calc R . . C24 C 0.8603(3) 0.0896(2) 0.6505(3) 0.0347(8) Uani 1 d . . . H24A H 0.8216 0.0373 0.6664 0.042 Uiso 1 calc R . . C25 C 0.8484(3) 0.1573(2) 0.7138(3) 0.0382(8) Uani 1 d . . . H25A H 0.8019 0.1511 0.7737 0.046 Uiso 1 calc R . . C26 C 0.9032(3) 0.2346(2) 0.6917(2) 0.0314(7) Uani 1 d . . . H26A H 0.8933 0.2811 0.7355 0.038 Uiso 1 calc R . . C31 C 0.9741(3) 0.42702(19) 0.6231(2) 0.0214(6) Uani 1 d . . . C32 C 0.8371(3) 0.43973(19) 0.5873(2) 0.0267(6) Uani 1 d . . . H32A H 0.7902 0.3986 0.5455 0.032 Uiso 1 calc R . . C33 C 0.7705(3) 0.51166(19) 0.6128(2) 0.0306(7) Uani 1 d . . . H33A H 0.6790 0.5211 0.5863 0.037 Uiso 1 calc R . . C34 C 0.8375(4) 0.5700(2) 0.6770(3) 0.0345(8) Uani 1 d . . . H34A H 0.7910 0.6191 0.6954 0.041 Uiso 1 calc R . . C35 C 0.9702(3) 0.5576(2) 0.7144(2) 0.0344(7) Uani 1 d . . . H35A H 1.0148 0.5979 0.7588 0.041 Uiso 1 calc R . . C36 C 1.0401(3) 0.48623(19) 0.6876(2) 0.0284(7) Uani 1 d . . . H36A H 1.1323 0.4780 0.7133 0.034 Uiso 1 calc R . . C41 C 1.2291(2) 0.3323(2) 0.64979(18) 0.0208(5) Uani 1 d . . . C42 C 1.3289(3) 0.39138(19) 0.6311(2) 0.0275(6) Uani 1 d . . . H42A H 1.3091 0.4344 0.5821 0.033 Uiso 1 calc R . . C43 C 1.4563(3) 0.38690(19) 0.6839(2) 0.0274(6) Uani 1 d . . . H43A H 1.5239 0.4269 0.6711 0.033 Uiso 1 calc R . . C44 C 1.4860(3) 0.3244(2) 0.7555(2) 0.0273(6) Uani 1 d . . . H44A H 1.5740 0.3210 0.7910 0.033 Uiso 1 calc R . . C45 C 1.3866(3) 0.26665(19) 0.7751(2) 0.0279(7) Uani 1 d . . . H45A H 1.4065 0.2243 0.8250 0.033 Uiso 1 calc R . . C46 C 1.2584(3) 0.27036(18) 0.7225(2) 0.0238(6) Uani 1 d . . . H46A H 1.1908 0.2306 0.7363 0.029 Uiso 1 calc R . . C51 C 1.0851(2) 0.34229(19) 0.4458(2) 0.0227(6) Uani 1 d . . . C52 C 0.9749(3) 0.3601(2) 0.3759(2) 0.0361(8) Uani 1 d . . . H52A H 0.8889 0.3725 0.3996 0.043 Uiso 1 calc R . . C53 C 0.9892(3) 0.3600(2) 0.2731(3) 0.0435(9) Uani 1 d . . . H53A H 0.9132 0.3729 0.2262 0.052 Uiso 1 calc R . . C54 C 1.1129(3) 0.3413(3) 0.2369(2) 0.0346(7) Uani 1 d . . . H54A H 1.1222 0.3415 0.1655 0.041 Uiso 1 calc R . . C55 C 1.2225(3) 0.3223(3) 0.3055(2) 0.0400(8) Uani 1 d . . . H55A H 1.3079 0.3092 0.2812 0.048 Uiso 1 calc R . . C56 C 1.2091(3) 0.3223(3) 0.4092(2) 0.0380(8) Uani 1 d . . . H56A H 1.2849 0.3085 0.4559 0.046 Uiso 1 calc R . . O7 O 0.0909(2) 0.32062(19) -0.0886(2) 0.0517(7) Uani 1 d . . . H7A H 0.014(4) 0.330(3) -0.082(3) 0.062 Uiso 1 d . . . H7B H 0.137(4) 0.364(3) -0.080(3) 0.062 Uiso 1 d . . . O6 O 0.2641(2) 0.20720(15) 0.02362(19) 0.0343(5) Uani 1 d . . . H6A H 0.283(3) 0.165(2) -0.018(3) 0.041 Uiso 1 d . . . H6B H 0.220(4) 0.231(3) -0.012(3) 0.041 Uiso 1 d . . . O8 O 0.3011(3) 0.43899(18) -0.0571(3) 0.0821(12) Uani 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 Fe 0.01921(16) 0.01137(16) 0.01758(17) -0.00017(17) 0.00321(13) 0.00049(19) O1 0.0416(12) 0.0122(10) 0.0311(11) 0.0013(9) 0.0094(9) 0.0052(9) O2 0.0276(9) 0.0238(9) 0.0211(9) 0.0023(11) 0.0092(7) -0.0002(11) O3 0.0410(12) 0.0142(10) 0.0350(12) 0.0028(9) 0.0123(10) 0.0017(9) O4 0.0523(14) 0.0195(11) 0.0241(11) -0.0025(9) 0.0093(10) 0.0014(10) O5 0.0226(9) 0.0160(9) 0.0293(10) 0.0004(11) -0.0016(7) -0.0022(11) N1 0.0226(12) 0.0116(11) 0.0193(12) 0.0001(9) 0.0055(10) 0.0031(9) N2 0.0214(12) 0.0124(11) 0.0183(12) 0.0003(8) 0.0035(9) 0.0010(8) N3 0.0221(13) 0.0151(12) 0.0164(12) -0.0011(9) 0.0034(10) 0.0010(9) N4 0.0206(10) 0.0142(13) 0.0169(10) 0.0023(10) 0.0025(8) 0.0027(10) C1 0.0199(14) 0.0161(14) 0.0213(15) 0.0027(12) 0.0037(11) 0.0002(11) C2 0.0195(13) 0.0160(15) 0.0230(15) -0.0023(12) 0.0016(12) 0.0027(11) C3 0.0230(15) 0.0147(14) 0.0216(15) -0.0008(12) 0.0015(12) 0.0036(11) C4 0.0157(12) 0.0242(16) 0.0193(14) -0.0002(11) 0.0000(11) 0.0019(10) C5 0.0205(14) 0.0163(14) 0.0257(15) 0.0014(12) 0.0047(12) -0.0019(11) C6 0.0215(14) 0.0128(14) 0.0235(15) 0.0016(12) 0.0017(12) -0.0015(11) C7 0.0209(14) 0.0141(13) 0.0201(14) -0.0024(11) -0.0009(11) 0.0032(11) C8 0.0209(15) 0.0175(14) 0.0196(15) -0.0045(12) 0.0007(11) 0.0024(12) C9 0.0200(14) 0.0159(13) 0.0203(15) 0.0039(11) 0.0006(11) 0.0001(12) C10 0.0238(14) 0.0206(15) 0.0239(16) 0.0003(12) 0.0031(12) 0.0009(12) C11 0.0272(15) 0.0267(15) 0.0241(15) 0.0074(13) 0.0060(12) 0.0024(12) C12 0.0295(16) 0.0183(14) 0.0322(16) 0.0097(12) 0.0053(12) -0.0007(12) C13 0.0265(15) 0.0157(14) 0.0269(15) 0.0007(12) 0.0046(12) 0.0002(11) C14 0.0298(17) 0.0196(15) 0.0322(16) 0.0025(13) 0.0088(13) 0.0081(13) C15 0.0346(17) 0.0175(14) 0.0260(15) -0.0038(12) -0.0006(13) 0.0007(13) C16 0.0259(17) 0.0273(17) 0.048(2) -0.0030(15) 0.0124(15) -0.0081(13) C17 0.047(2) 0.0246(16) 0.0294(17) 0.0001(14) -0.0044(15) 0.0071(14) C18 0.0254(14) 0.0195(14) 0.0276(15) -0.0013(12) 0.0028(12) 0.0057(12) C19 0.0312(16) 0.0154(13) 0.0257(15) -0.0036(11) -0.0005(12) -0.0015(12) P 0.0186(3) 0.0203(3) 0.0224(3) -0.0003(4) 0.0009(2) 0.0006(4) C21 0.0182(16) 0.0253(16) 0.0246(16) -0.0015(13) -0.0020(12) 0.0005(12) C22 0.0343(16) 0.0274(17) 0.0326(17) -0.0064(14) 0.0108(13) -0.0033(13) C23 0.0443(19) 0.0267(17) 0.0412(19) -0.0095(14) 0.0101(15) -0.0029(15) C24 0.0357(19) 0.0259(17) 0.043(2) -0.0007(15) 0.0071(15) -0.0087(14) C25 0.0380(18) 0.043(2) 0.0362(18) -0.0029(15) 0.0159(15) -0.0125(15) C26 0.0315(17) 0.0316(17) 0.0322(17) -0.0073(14) 0.0086(13) -0.0093(14) C31 0.0218(16) 0.0174(14) 0.0257(15) 0.0016(12) 0.0055(12) 0.0016(12) C32 0.0248(15) 0.0304(16) 0.0251(15) -0.0026(12) 0.0030(12) 0.0010(13) C33 0.0262(16) 0.0314(17) 0.0347(17) 0.0053(13) 0.0062(13) 0.0085(13) C34 0.042(2) 0.0269(18) 0.0363(18) -0.0014(15) 0.0116(15) 0.0102(15) C35 0.0435(19) 0.0291(17) 0.0312(17) -0.0075(13) 0.0062(15) 0.0026(14) C36 0.0276(16) 0.0298(16) 0.0275(15) -0.0009(13) -0.0002(12) 0.0021(13) C41 0.0202(11) 0.0178(12) 0.0245(12) -0.0035(15) 0.0026(9) 0.0021(15) C42 0.0315(16) 0.0235(14) 0.0268(15) 0.0062(13) -0.0020(12) -0.0013(13) C43 0.0249(15) 0.0252(15) 0.0316(16) -0.0033(13) 0.0000(12) -0.0059(13) C44 0.0230(12) 0.0280(15) 0.0296(14) -0.0050(15) -0.0043(10) 0.0036(15) C45 0.0308(16) 0.0220(14) 0.0297(17) 0.0019(13) -0.0039(13) 0.0063(13) C46 0.0241(14) 0.0181(13) 0.0291(16) 0.0020(12) 0.0018(12) 0.0018(12) C51 0.0229(12) 0.0200(16) 0.0253(13) -0.0021(13) 0.0020(10) 0.0001(13) C52 0.0237(15) 0.057(2) 0.0280(16) 0.0006(14) 0.0025(13) 0.0105(14) C53 0.0327(17) 0.066(3) 0.0308(17) 0.0026(15) -0.0013(14) 0.0106(16) C54 0.0331(14) 0.047(2) 0.0243(14) 0.0032(16) 0.0043(11) -0.0042(17) C55 0.0218(13) 0.069(3) 0.0302(15) -0.0054(19) 0.0071(11) 0.0042(19) C56 0.0210(13) 0.066(2) 0.0262(14) 0.0029(18) 0.0010(11) 0.0038(18) O7 0.0245(11) 0.0438(17) 0.0879(19) -0.0083(15) 0.0109(12) 0.0007(13) O6 0.0313(12) 0.0226(12) 0.0484(15) -0.0094(11) 0.0008(10) 0.0030(9) O8 0.0527(18) 0.0378(16) 0.148(3) 0.0470(19) -0.0335(19) -0.0146(14) _geom_special_details ; ? ; 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 N4 1.876(2) . ? Fe N1 1.881(2) . ? Fe N2 1.889(2) . ? Fe N3 1.892(2) . ? Fe O5 2.0972(17) . ? O1 C2 1.252(3) . ? O2 C4 1.258(3) . ? O3 C6 1.259(3) . ? O4 C8 1.229(4) . ? N1 C2 1.346(3) . ? N1 C1 1.418(3) . ? N2 C4 1.337(3) . ? N2 C3 1.510(3) . ? N3 C6 1.342(4) . ? N3 C7 1.494(3) . ? N4 C8 1.353(3) . ? N4 C9 1.421(4) . ? C1 C13 1.395(4) . ? C1 C9 1.415(4) . ? C2 C3 1.536(4) . ? C3 C14 1.525(4) . ? C3 C15 1.527(4) . ? C4 C5 1.561(4) . ? C5 C17 1.540(4) . ? C5 C6 1.546(4) . ? C5 C16 1.563(4) . ? C7 C19 1.535(4) . ? C7 C18 1.539(4) . ? C7 C8 1.538(4) . ? C9 C10 1.385(4) . ? C10 C11 1.399(4) . ? C11 C12 1.388(4) . ? C12 C13 1.396(4) . ? P C21 1.787(3) . ? P C41 1.796(2) . ? P C31 1.802(3) . ? P C51 1.809(3) . ? C21 C26 1.391(4) . ? C21 C22 1.403(4) . ? C22 C23 1.384(4) . ? C23 C24 1.379(5) . ? C24 C25 1.376(5) . ? C25 C26 1.389(4) . ? C31 C36 1.393(4) . ? C31 C32 1.406(4) . ? C32 C33 1.380(4) . ? C33 C34 1.385(5) . ? C34 C35 1.371(5) . ? C35 C36 1.394(4) . ? C41 C46 1.389(4) . ? C41 C42 1.401(4) . ? C42 C43 1.383(4) . ? C43 C44 1.385(4) . ? C44 C45 1.387(4) . ? C45 C46 1.387(4) . ? C51 C52 1.388(4) . ? C51 C56 1.390(4) . ? C52 C53 1.370(4) . ? C53 C54 1.381(4) . ? C54 C55 1.378(4) . ? C55 C56 1.381(4) . ? 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 N4 Fe N1 83.18(10) . . ? N4 Fe N2 154.19(9) . . ? N1 Fe N2 85.00(9) . . ? N4 Fe N3 84.51(10) . . ? N1 Fe N3 158.44(9) . . ? N2 Fe N3 98.81(9) . . ? N4 Fe O5 103.03(8) . . ? N1 Fe O5 101.83(10) . . ? N2 Fe O5 101.81(8) . . ? N3 Fe O5 98.16(10) . . ? C2 N1 C1 126.2(2) . . ? C2 N1 Fe 117.99(19) . . ? C1 N1 Fe 115.44(17) . . ? C4 N2 C3 119.3(2) . . ? C4 N2 Fe 125.90(17) . . ? C3 N2 Fe 114.17(16) . . ? C6 N3 C7 119.8(2) . . ? C6 N3 Fe 125.23(19) . . ? C7 N3 Fe 113.99(17) . . ? C8 N4 C9 126.0(2) . . ? C8 N4 Fe 118.23(19) . . ? C9 N4 Fe 115.73(18) . . ? C13 C1 C9 119.8(2) . . ? C13 C1 N1 127.8(3) . . ? C9 C1 N1 112.5(2) . . ? O1 C2 N1 125.6(3) . . ? O1 C2 C3 120.6(2) . . ? N1 C2 C3 113.8(2) . . ? N2 C3 C14 113.1(2) . . ? N2 C3 C15 111.0(2) . . ? C14 C3 C15 111.4(2) . . ? N2 C3 C2 107.5(2) . . ? C14 C3 C2 107.6(2) . . ? C15 C3 C2 105.8(2) . . ? O2 C4 N2 123.6(2) . . ? O2 C4 C5 114.8(2) . . ? N2 C4 C5 121.6(2) . . ? C17 C5 C6 107.0(2) . . ? C17 C5 C4 107.1(2) . . ? C6 C5 C4 122.9(2) . . ? C17 C5 C16 108.6(3) . . ? C6 C5 C16 105.1(2) . . ? C4 C5 C16 105.5(2) . . ? O3 C6 N3 122.6(3) . . ? O3 C6 C5 115.9(2) . . ? N3 C6 C5 121.5(2) . . ? N3 C7 C19 111.3(2) . . ? N3 C7 C18 111.9(2) . . ? C19 C7 C18 111.3(2) . . ? N3 C7 C8 108.1(2) . . ? C19 C7 C8 107.0(2) . . ? C18 C7 C8 106.9(2) . . ? O4 C8 N4 126.0(3) . . ? O4 C8 C7 121.3(2) . . ? N4 C8 C7 112.7(2) . . ? C10 C9 C1 120.6(3) . . ? C10 C9 N4 127.1(3) . . ? C1 C9 N4 112.2(2) . . ? C9 C10 C11 118.9(3) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C13 120.5(3) . . ? C1 C13 C12 119.3(3) . . ? C21 P C41 109.13(15) . . ? C21 P C31 110.40(11) . . ? C41 P C31 109.09(14) . . ? C21 P C51 108.34(14) . . ? C41 P C51 108.35(11) . . ? C31 P C51 111.48(14) . . ? C26 C21 C22 119.5(3) . . ? C26 C21 P 121.1(2) . . ? C22 C21 P 119.0(2) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C26 121.1(3) . . ? C25 C26 C21 119.3(3) . . ? C36 C31 C32 119.3(3) . . ? C36 C31 P 120.9(2) . . ? C32 C31 P 119.7(2) . . ? C33 C32 C31 120.3(3) . . ? C32 C33 C34 119.7(3) . . ? C35 C34 C33 120.6(3) . . ? C34 C35 C36 120.4(3) . . ? C31 C36 C35 119.6(3) . . ? C46 C41 C42 119.7(2) . . ? C46 C41 P 119.9(2) . . ? C42 C41 P 120.4(2) . . ? C43 C42 C41 119.9(3) . . ? C42 C43 C44 120.4(3) . . ? C45 C44 C43 119.7(2) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 119.8(3) . . ? C52 C51 C56 118.7(3) . . ? C52 C51 P 120.3(2) . . ? C56 C51 P 120.7(2) . . ? C53 C52 C51 120.5(3) . . ? C52 C53 C54 120.7(3) . . ? C55 C54 C53 119.3(3) . . ? C54 C55 C56 120.4(3) . . ? C55 C56 C51 120.4(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O6 0.80(3) 1.87(3) 2.671(3) 176(3) . O5 H5B O8 0.92(3) 1.96(3) 2.861(4) 167(3) . O7 H7B O8 0.84(4) 2.01(4) 2.811(4) 160(4) . O7 H7A O2 0.79(4) 1.99(4) 2.762(3) 167(5) 1_455 O6 H6B O7 0.72(4) 2.11(4) 2.816(4) 166(4) . O6 H6A O3 0.90(4) 1.85(4) 2.752(3) 176(3) 2_645 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.663 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.045