Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Carty, Arthur' 'Enright, Gary D.' 'Low, Paul J.' 'Udachin, Konstantin A.' _publ_contact_author_name 'Dr Paul J Low' _publ_contact_author_address ; Dr Paul J Low Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'P.J.Low@durham.ac.uk' data_pjl53 _database_code_CSD 155050 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.07 H29.14 Cl0.14 Fe4 O15 P3' _chemical_formula_weight 1107.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 10.9884(5) _cell_length_b 11.1706(5) _cell_length_c 22.0560(10) _cell_angle_alpha 81.6480(10) _cell_angle_beta 75.7140(10) _cell_angle_gamma 61.3590(10) _cell_volume 2301.41(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 1.415 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20767 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8085 _reflns_number_gt 6813 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.1860P] 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 8085 _refine_ls_number_parameters 596 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.914 _refine_ls_shift/su_mean 0.163 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 Fe1 Fe 0.23808(3) 0.22279(3) 0.407081(12) 0.02366(7) Uani 1 d . . . Fe2 Fe 0.22763(2) 0.25641(3) 0.288844(12) 0.02251(6) Uani 1 d . . . Fe3 Fe 0.72851(3) 0.27773(3) 0.207620(13) 0.02787(7) Uani 1 d . . . Fe4 Fe 0.71200(3) 0.19203(3) 0.109135(13) 0.03190(8) Uani 1 d . . . P1 P 0.35454(4) 0.34385(5) 0.36834(2) 0.02214(11) Uani 1 d . . . P2 P 0.64878(5) 0.40707(6) 0.12467(2) 0.03041(13) Uani 1 d . . . P3 P 0.49250(5) -0.03153(5) 0.31168(2) 0.02483(12) Uani 1 d . . . O11 O 0.11899(14) 0.03045(14) 0.43869(7) 0.0396(4) Uani 1 d . . . O12 O -0.04565(15) 0.45682(16) 0.43417(8) 0.0450(5) Uani 1 d . . . O13 O 0.33845(19) 0.1582(2) 0.52459(8) 0.0615(5) Uani 1 d . . . O21 O 0.31737(15) 0.19623(17) 0.15585(7) 0.0449(4) Uani 1 d . . . O22 O 0.02688(16) 0.14666(18) 0.30584(9) 0.0581(5) Uani 1 d . . . O23 O 0.01852(16) 0.54418(16) 0.27679(9) 0.0517(5) Uani 1 d . . . O31 O 0.84913(15) 0.02115(16) 0.28207(9) 0.0498(5) Uani 1 d . . . O32 O 0.6558(2) 0.50439(18) 0.28506(9) 0.0638(5) Uani 1 d . . . O33 O 1.01599(15) 0.2318(2) 0.15115(9) 0.0611(6) Uani 1 d . . . O41 O 0.5324(2) 0.2144(3) 0.02548(10) 0.1171(10) Uani 1 d . . . O42 O 0.82477(19) -0.10045(17) 0.14499(11) 0.0642(6) Uani 1 d . . . O43 O 0.96066(17) 0.15865(19) 0.01100(9) 0.0617(5) Uani 1 d . . . O91 O 0.41808(14) -0.12205(13) 0.33894(7) 0.0342(4) Uani 1 d . . . O92 O 0.62895(13) -0.08334(13) 0.33810(7) 0.0338(4) Uani 1 d . . . O93 O 0.54494(15) -0.06084(14) 0.24057(7) 0.0359(4) Uani 1 d . . . C1 C 0.38508(18) 0.13607(18) 0.32940(9) 0.0234(4) Uani 1 d . . . C2 C 0.41259(17) 0.25186(17) 0.29860(9) 0.0218(4) Uani 1 d . . . C3 C 0.51346(17) 0.24691(18) 0.24171(9) 0.0227(4) Uani 1 d . . . C4 C 0.58436(18) 0.22224(19) 0.18821(10) 0.0277(5) Uani 1 d . . . C11 C 0.1690(2) 0.1026(2) 0.42397(10) 0.0301(5) Uani 1 d . . . C12 C 0.0651(2) 0.3676(2) 0.42438(10) 0.0311(5) Uani 1 d . . . C13 C 0.3015(2) 0.1813(2) 0.47814(10) 0.0361(5) Uani 1 d . . . C21 C 0.28358(18) 0.2197(2) 0.20806(10) 0.0291(5) Uani 1 d . . . C22 C 0.1071(2) 0.1885(2) 0.30053(10) 0.0334(5) Uani 1 d . . . C23 C 0.10216(19) 0.4341(2) 0.28255(10) 0.0328(5) Uani 1 d . . . C31 C 0.80175(19) 0.1220(2) 0.25537(11) 0.0366(5) Uani 1 d . . . C32 C 0.6795(2) 0.4125(2) 0.25822(11) 0.0390(6) Uani 1 d . . . C33 C 0.9020(2) 0.2527(2) 0.17259(11) 0.0413(6) Uani 1 d . . . C41 C 0.6018(2) 0.2066(3) 0.05789(12) 0.0611(8) Uani 1 d . . . C42 C 0.7829(2) 0.0118(2) 0.12977(12) 0.0437(6) Uani 1 d . . . C43 C 0.8640(2) 0.1726(2) 0.04918(11) 0.0427(6) Uani 1 d . . . C51 C 0.26346(18) 0.52794(18) 0.35897(9) 0.0247(4) Uani 1 d . . . C52 C 0.2838(2) 0.5960(2) 0.30297(10) 0.0332(5) Uani 1 d . . . H52 H 0.3482 0.5462 0.2674 0.040 Uiso 1 calc R . . C53 C 0.2096(2) 0.7373(2) 0.29887(11) 0.0424(6) Uani 1 d . . . H53 H 0.2232 0.7840 0.2603 0.051 Uiso 1 calc R . . C54 C 0.1160(2) 0.8105(2) 0.35070(11) 0.0403(6) Uani 1 d . . . H54 H 0.0656 0.9073 0.3476 0.048 Uiso 1 calc R . . C55 C 0.0962(2) 0.7430(2) 0.40681(12) 0.0404(6) Uani 1 d . . . H55 H 0.0322 0.7931 0.4424 0.048 Uiso 1 calc R . . C56 C 0.1695(2) 0.6022(2) 0.41116(10) 0.0324(5) Uani 1 d . . . H56 H 0.1559 0.5557 0.4499 0.039 Uiso 1 calc R . . C61 C 0.50695(18) 0.31041(19) 0.40037(9) 0.0259(5) Uani 1 d . . . C62 C 0.5262(2) 0.4139(2) 0.41734(11) 0.0379(5) Uani 1 d . . . H62 H 0.4574 0.5063 0.4133 0.046 Uiso 1 calc R . . C63 C 0.6456(2) 0.3834(2) 0.44025(12) 0.0454(6) Uani 1 d . . . H63 H 0.6575 0.4554 0.4517 0.055 Uiso 1 calc R . . C64 C 0.7458(2) 0.2512(2) 0.44650(11) 0.0392(6) Uani 1 d . . . H64 H 0.8272 0.2312 0.4619 0.047 Uiso 1 calc R . . C65 C 0.7274(2) 0.1473(2) 0.43023(11) 0.0426(6) Uani 1 d . . . H65 H 0.7968 0.0552 0.4345 0.051 Uiso 1 calc R . . C66 C 0.6086(2) 0.1756(2) 0.40768(11) 0.0359(5) Uani 1 d . . . H66 H 0.5966 0.1029 0.3972 0.043 Uiso 1 calc R . . C71 C 0.4649(2) 0.5393(2) 0.12857(10) 0.0355(6) Uani 1 d . . . C72 C 0.3549(2) 0.5057(3) 0.13663(11) 0.0441(6) Uani 1 d . . . H72 H 0.3737 0.4129 0.1405 0.053 Uiso 1 calc R . . C73 C 0.2165(2) 0.6102(3) 0.13899(12) 0.0552(8) Uani 1 d . . . H73 H 0.1412 0.5876 0.1451 0.066 Uiso 1 calc R . . C74 C 0.1874(3) 0.7443(3) 0.13262(13) 0.0613(9) Uani 1 d . . . H74 H 0.0928 0.8142 0.1344 0.074 Uiso 1 calc R . . C75 C 0.2966(3) 0.7774(3) 0.12366(14) 0.0601(9) Uani 1 d . . . H75 H 0.2772 0.8703 0.1185 0.072 Uiso 1 calc R . . C76 C 0.4332(3) 0.6768(3) 0.12209(12) 0.0472(7) Uani 1 d . . . H76 H 0.5071 0.7011 0.1165 0.057 Uiso 1 calc R . . C81 C 0.7431(2) 0.4965(2) 0.07720(10) 0.0341(5) Uani 1 d . . . C82 C 0.7430(2) 0.5171(3) 0.01335(11) 0.0441(6) Uani 1 d . . . H82 H 0.7053 0.4749 -0.0057 0.053 Uiso 1 calc R . . C83 C 0.7984(2) 0.5998(3) -0.02229(13) 0.0545(7) Uani 1 d . . . H83 H 0.7977 0.6147 -0.0657 0.065 Uiso 1 calc R . . C84 C 0.8543(3) 0.6600(3) 0.00496(14) 0.0587(8) Uani 1 d . . . H84 H 0.8900 0.7178 -0.0196 0.070 Uiso 1 calc R . . C85 C 0.8589(3) 0.6373(3) 0.06783(14) 0.0514(7) Uani 1 d . . . H85 H 0.9007 0.6766 0.0861 0.062 Uiso 1 calc R . . C86 C 0.8019(2) 0.5564(2) 0.10422(12) 0.0421(6) Uani 1 d . . . H86 H 0.8032 0.5419 0.1476 0.051 Uiso 1 calc R . . C91 C 0.4365(3) -0.2034(2) 0.39573(12) 0.0479(7) Uani 1 d . . . H91C H 0.4385 -0.1524 0.4277 0.058 Uiso 1 calc R . . H91B H 0.5259 -0.2879 0.3879 0.058 Uiso 1 calc R . . H91A H 0.3576 -0.2256 0.4104 0.058 Uiso 1 calc R . . C92 C 0.7545(2) -0.2134(2) 0.32164(13) 0.0431(7) Uani 1 d . . . H92C H 0.7881 -0.2158 0.2761 0.052 Uiso 1 calc R . . H92B H 0.7305 -0.2883 0.3358 0.052 Uiso 1 calc R . . H92A H 0.8290 -0.2236 0.3419 0.052 Uiso 1 calc R . . C93 C 0.5001(3) -0.1276(3) 0.20622(14) 0.0663(8) Uani 1 d . . . H93C H 0.3968 -0.0894 0.2173 0.080 Uiso 1 calc R . . H93B H 0.5436 -0.2256 0.2167 0.080 Uiso 1 calc R . . H93A H 0.5294 -0.1131 0.1612 0.080 Uiso 1 calc R . . Cl1A Cl 0.4725(9) 0.0606(9) -0.0517(4) 0.050 Uiso 0.07 d PD A -1 C1A C 0.4039(15) 0.030(3) 0.0277(7) 0.050 Uiso 0.07 d PD A -1 H1A1 H 0.3574 -0.0288 0.0321 0.060 Uiso 0.07 calc PR A -1 H1A2 H 0.3398 0.1149 0.0508 0.060 Uiso 0.07 calc PR A -1 Cl2A Cl 0.5772(8) -0.0587(9) 0.0479(4) 0.050 Uiso 0.07 d PD A -1 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 0.02325(11) 0.02584(11) 0.02086(13) 0.00127(10) -0.00301(10) -0.01177(9) Fe2 0.01918(10) 0.02599(11) 0.02228(13) 0.00103(10) -0.00538(9) -0.01033(9) Fe3 0.02295(11) 0.03850(13) 0.02372(14) 0.00043(11) -0.00595(10) -0.01527(10) Fe4 0.02450(12) 0.04882(15) 0.02343(14) -0.00714(12) 0.00049(11) -0.01868(11) P1 0.02157(18) 0.02337(19) 0.0204(2) -0.00071(17) -0.00365(17) -0.00986(15) P2 0.0245(2) 0.0439(3) 0.0221(2) 0.0027(2) -0.00395(18) -0.01660(18) P3 0.02363(19) 0.02238(19) 0.0279(2) -0.00091(18) -0.00564(18) -0.00996(16) O11 0.0406(6) 0.0396(7) 0.0433(9) 0.0025(6) -0.0024(6) -0.0262(5) O12 0.0291(7) 0.0421(8) 0.0455(9) -0.0069(7) 0.0075(7) -0.0077(6) O13 0.0840(9) 0.0899(11) 0.0327(9) 0.0204(8) -0.0295(7) -0.0554(8) O21 0.0416(7) 0.0680(9) 0.0281(8) -0.0075(7) -0.0065(6) -0.0265(6) O22 0.0646(7) 0.0837(9) 0.0598(10) 0.0261(8) -0.0321(7) -0.0593(6) O23 0.0340(8) 0.0346(8) 0.0656(11) 0.0008(8) -0.0131(8) 0.0014(7) O31 0.0439(7) 0.0487(8) 0.0658(10) 0.0201(7) -0.0314(7) -0.0249(6) O32 0.0871(10) 0.0666(9) 0.0490(11) -0.0179(8) 0.0029(9) -0.0480(8) O33 0.0290(7) 0.1009(13) 0.0521(11) 0.0106(9) -0.0072(7) -0.0329(7) O41 0.0705(10) 0.259(3) 0.0432(11) -0.0197(14) -0.0173(9) -0.0866(13) O42 0.0507(9) 0.0424(8) 0.0888(15) -0.0165(9) 0.0096(9) -0.0205(7) O43 0.0492(8) 0.0765(10) 0.0571(11) -0.0231(8) 0.0237(8) -0.0376(7) O91 0.0377(6) 0.0291(6) 0.0404(8) 0.0054(6) -0.0113(6) -0.0193(5) O92 0.0243(6) 0.0262(6) 0.0478(8) -0.0055(6) -0.0124(6) -0.0059(5) O93 0.0418(7) 0.0344(6) 0.0291(7) -0.0082(6) 0.0000(6) -0.0172(5) C1 0.0237(7) 0.0219(8) 0.0229(9) 0.0002(7) -0.0075(7) -0.0082(6) C2 0.0195(7) 0.0233(7) 0.0218(9) -0.0030(7) -0.0030(6) -0.0092(6) C3 0.0187(7) 0.0256(8) 0.0247(9) 0.0003(7) -0.0066(6) -0.0102(6) C4 0.0223(7) 0.0336(9) 0.0288(10) -0.0022(7) -0.0076(7) -0.0128(7) C11 0.0267(8) 0.0347(9) 0.0272(10) 0.0003(8) -0.0044(7) -0.0137(7) C12 0.0313(8) 0.0342(9) 0.0255(10) -0.0024(8) 0.0030(8) -0.0170(7) C13 0.0412(9) 0.0411(9) 0.0313(11) 0.0049(8) -0.0069(8) -0.0252(8) C21 0.0220(7) 0.0408(9) 0.0293(10) 0.0014(8) -0.0080(7) -0.0177(7) C22 0.0355(8) 0.0411(9) 0.0311(10) 0.0071(8) -0.0128(8) -0.0230(7) C23 0.0248(8) 0.0391(9) 0.0340(11) 0.0017(8) -0.0057(8) -0.0153(7) C31 0.0280(8) 0.0513(10) 0.0388(11) 0.0006(9) -0.0115(8) -0.0232(7) C32 0.0436(9) 0.0509(11) 0.0283(11) 0.0020(9) -0.0023(8) -0.0297(8) C33 0.0362(9) 0.0577(12) 0.0321(11) 0.0061(9) -0.0139(8) -0.0222(9) C41 0.0380(11) 0.118(2) 0.0270(12) -0.0145(12) 0.0038(10) -0.0379(12) C42 0.0317(9) 0.0556(12) 0.0435(13) -0.0197(10) 0.0083(9) -0.0225(9) C43 0.0389(9) 0.0548(11) 0.0381(12) -0.0137(9) 0.0047(9) -0.0272(8) C51 0.0222(7) 0.0240(8) 0.0264(9) -0.0006(7) -0.0061(7) -0.0091(6) C52 0.0408(9) 0.0299(9) 0.0294(11) 0.0016(8) -0.0074(8) -0.0174(7) C53 0.0568(11) 0.0348(10) 0.0387(12) 0.0110(9) -0.0212(9) -0.0216(8) C54 0.0448(10) 0.0243(9) 0.0547(13) 0.0026(9) -0.0266(9) -0.0117(8) C55 0.0351(10) 0.0322(10) 0.0469(13) -0.0118(9) -0.0073(9) -0.0078(8) C56 0.0338(9) 0.0291(9) 0.0290(10) -0.0029(8) -0.0033(8) -0.0113(7) C61 0.0270(8) 0.0302(8) 0.0211(9) -0.0004(7) -0.0045(7) -0.0141(6) C62 0.0422(9) 0.0351(9) 0.0443(12) 0.0019(9) -0.0191(9) -0.0200(8) C63 0.0473(9) 0.0527(11) 0.0525(13) -0.0022(10) -0.0230(9) -0.0297(8) C64 0.0311(8) 0.0569(12) 0.0342(11) 0.0001(9) -0.0109(8) -0.0225(8) C65 0.0339(10) 0.0432(11) 0.0448(13) -0.0045(10) -0.0171(9) -0.0081(9) C66 0.0335(9) 0.0343(9) 0.0433(12) -0.0016(9) -0.0171(8) -0.0140(7) C71 0.0280(8) 0.0544(11) 0.0192(9) 0.0032(8) -0.0050(7) -0.0163(8) C72 0.0348(9) 0.0629(13) 0.0337(12) 0.0125(10) -0.0125(9) -0.0231(9) C73 0.0273(10) 0.0887(18) 0.0386(13) 0.0096(12) -0.0116(9) -0.0192(11) C74 0.0336(12) 0.0763(18) 0.0461(14) -0.0042(14) -0.0122(10) -0.0010(12) C75 0.0467(13) 0.0559(15) 0.0568(17) -0.0092(13) -0.0078(12) -0.0066(12) C76 0.0407(11) 0.0546(13) 0.0379(13) -0.0072(10) -0.0029(10) -0.0163(10) C81 0.0277(8) 0.0430(10) 0.0291(11) -0.0006(8) -0.0013(8) -0.0165(8) C82 0.0378(9) 0.0686(13) 0.0291(11) 0.0080(10) -0.0057(9) -0.0301(9) C83 0.0478(11) 0.0768(14) 0.0411(14) 0.0184(11) -0.0086(10) -0.0361(10) C84 0.0570(12) 0.0674(14) 0.0571(17) 0.0148(12) -0.0039(12) -0.0411(10) C85 0.0499(11) 0.0558(12) 0.0588(16) -0.0045(11) -0.0063(11) -0.0340(9) C86 0.0373(10) 0.0528(11) 0.0369(12) -0.0027(10) -0.0022(9) -0.0234(9) C91 0.0467(11) 0.0424(11) 0.0483(14) 0.0187(10) -0.0097(10) -0.0210(9) C92 0.0252(9) 0.0251(10) 0.0663(16) -0.0039(10) -0.0107(10) -0.0004(8) C93 0.1080(17) 0.0637(13) 0.0444(15) -0.0120(11) -0.0168(13) -0.0499(12) _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 C13 1.782(2) . ? Fe1 C11 1.792(2) . ? Fe1 C12 1.8023(18) . ? Fe1 C1 2.0247(17) . ? Fe1 P1 2.2316(6) . ? Fe1 Fe2 2.6033(4) . ? Fe2 C22 1.770(2) . ? Fe2 C21 1.775(2) . ? Fe2 C23 1.8034(19) . ? Fe2 C1 1.9456(18) . ? Fe2 C2 2.0721(19) . ? Fe3 C33 1.770(2) . ? Fe3 C32 1.794(2) . ? Fe3 C31 1.824(2) . ? Fe3 C4 2.105(2) . ? Fe3 P2 2.2388(6) . ? Fe3 C3 2.4689(19) . ? Fe3 Fe4 2.5754(4) . ? Fe4 C41 1.790(3) . ? Fe4 C43 1.798(2) . ? Fe4 C42 1.809(2) . ? Fe4 C4 1.9061(19) . ? Fe4 P2 2.2118(7) . ? P1 C2 1.7819(19) . ? P1 C51 1.8107(18) . ? P1 C61 1.831(2) . ? P2 C81 1.822(2) . ? P2 C71 1.8331(19) . ? P3 O93 1.5561(15) . ? P3 O92 1.5569(15) . ? P3 O91 1.5576(16) . ? P3 C1 1.7081(17) . ? O11 C11 1.147(3) . ? O12 C12 1.136(2) . ? O13 C13 1.144(3) . ? O21 C21 1.147(3) . ? O22 C22 1.157(3) . ? O23 C23 1.141(2) . ? O31 C31 1.133(3) . ? O32 C32 1.147(3) . ? O33 C33 1.143(3) . ? O41 C41 1.134(4) . ? O42 C42 1.139(3) . ? O43 C43 1.140(3) . ? O91 C91 1.433(3) . ? O92 C92 1.460(2) . ? O93 C93 1.440(4) . ? C1 C2 1.498(3) . ? C2 C3 1.443(2) . ? C3 C4 1.229(3) . ? C51 C52 1.381(3) . ? C51 C56 1.396(3) . ? C52 C53 1.387(3) . ? C53 C54 1.386(3) . ? C54 C55 1.379(3) . ? C55 C56 1.383(3) . ? C61 C62 1.385(3) . ? C61 C66 1.396(3) . ? C62 C63 1.394(3) . ? C63 C64 1.367(3) . ? C64 C65 1.378(4) . ? C65 C66 1.389(3) . ? C71 C76 1.396(4) . ? C71 C72 1.395(4) . ? C72 C73 1.398(3) . ? C73 C74 1.367(5) . ? C74 C75 1.378(5) . ? C75 C76 1.373(3) . ? C81 C86 1.393(4) . ? C81 C82 1.394(3) . ? C82 C83 1.390(4) . ? C83 C84 1.373(5) . ? C84 C85 1.382(4) . ? C85 C86 1.392(4) . ? Cl1A C1A 1.781(15) . ? C1A Cl2A 1.814(15) . ? 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 C13 Fe1 C11 92.93(10) . . ? C13 Fe1 C12 105.18(9) . . ? C11 Fe1 C12 93.27(9) . . ? C13 Fe1 C1 115.77(8) . . ? C11 Fe1 C1 97.92(8) . . ? C12 Fe1 C1 136.71(8) . . ? C13 Fe1 P1 92.79(8) . . ? C11 Fe1 P1 167.50(6) . . ? C12 Fe1 P1 95.94(7) . . ? C1 Fe1 P1 69.59(6) . . ? C13 Fe1 Fe2 162.43(7) . . ? C11 Fe1 Fe2 95.46(7) . . ? C12 Fe1 Fe2 89.75(7) . . ? C1 Fe1 Fe2 47.73(5) . . ? P1 Fe1 Fe2 76.187(16) . . ? C22 Fe2 C21 92.26(10) . . ? C22 Fe2 C23 97.71(9) . . ? C21 Fe2 C23 98.60(9) . . ? C22 Fe2 C1 109.46(9) . . ? C21 Fe2 C1 107.62(8) . . ? C23 Fe2 C1 140.88(10) . . ? C22 Fe2 C2 153.09(8) . . ? C21 Fe2 C2 96.05(8) . . ? C23 Fe2 C2 106.24(9) . . ? C1 Fe2 C2 43.64(8) . . ? C22 Fe2 Fe1 91.80(7) . . ? C21 Fe2 Fe1 157.47(6) . . ? C23 Fe2 Fe1 102.80(7) . . ? C1 Fe2 Fe1 50.36(5) . . ? C2 Fe2 Fe1 71.32(5) . . ? C33 Fe3 C32 98.13(11) . . ? C33 Fe3 C31 89.93(10) . . ? C32 Fe3 C31 104.47(10) . . ? C33 Fe3 C4 136.03(10) . . ? C32 Fe3 C4 124.07(9) . . ? C31 Fe3 C4 90.72(9) . . ? C33 Fe3 P2 90.06(7) . . ? C32 Fe3 P2 98.08(7) . . ? C31 Fe3 P2 157.22(8) . . ? C4 Fe3 P2 73.72(6) . . ? C33 Fe3 C3 162.78(10) . . ? C32 Fe3 C3 98.64(8) . . ? C31 Fe3 C3 82.09(8) . . ? C4 Fe3 C3 29.84(7) . . ? P2 Fe3 C3 91.46(5) . . ? C33 Fe3 Fe4 90.52(8) . . ? C32 Fe3 Fe4 151.09(7) . . ? C31 Fe3 Fe4 103.07(8) . . ? C4 Fe3 Fe4 46.74(5) . . ? P2 Fe3 Fe4 54.156(18) . . ? C3 Fe3 Fe4 76.58(5) . . ? C41 Fe4 C43 96.67(11) . . ? C41 Fe4 C42 100.10(14) . . ? C43 Fe4 C42 94.42(10) . . ? C41 Fe4 C4 101.27(10) . . ? C43 Fe4 C4 161.51(11) . . ? C42 Fe4 C4 86.81(9) . . ? C41 Fe4 P2 103.12(11) . . ? C43 Fe4 P2 93.52(8) . . ? C42 Fe4 P2 154.37(9) . . ? C4 Fe4 P2 78.19(6) . . ? C41 Fe4 Fe3 147.00(8) . . ? C43 Fe4 Fe3 108.20(9) . . ? C42 Fe4 Fe3 99.25(9) . . ? C4 Fe4 Fe3 53.53(7) . . ? P2 Fe4 Fe3 55.135(17) . . ? C2 P1 C51 115.58(9) . . ? C2 P1 C61 110.08(8) . . ? C51 P1 C61 103.93(9) . . ? C2 P1 Fe1 86.10(7) . . ? C51 P1 Fe1 121.97(6) . . ? C61 P1 Fe1 118.44(7) . . ? C81 P2 C71 100.53(10) . . ? C81 P2 Fe4 121.94(7) . . ? C71 P2 Fe4 120.87(9) . . ? C81 P2 Fe3 119.72(7) . . ? C71 P2 Fe3 123.18(7) . . ? Fe4 P2 Fe3 70.71(2) . . ? O93 P3 O92 105.53(8) . . ? O93 P3 O91 105.07(9) . . ? O92 P3 O91 109.81(8) . . ? O93 P3 C1 115.31(9) . . ? O92 P3 C1 108.69(9) . . ? O91 P3 C1 112.14(8) . . ? C91 O91 P3 124.95(16) . . ? C92 O92 P3 123.13(16) . . ? C93 O93 P3 125.75(16) . . ? C2 C1 P3 124.64(13) . . ? C2 C1 Fe2 72.68(10) . . ? P3 C1 Fe2 123.27(11) . . ? C2 C1 Fe1 102.09(11) . . ? P3 C1 Fe1 130.77(11) . . ? Fe2 C1 Fe1 81.92(6) . . ? C3 C2 C1 126.50(15) . . ? C3 C2 P1 131.78(16) . . ? C1 C2 P1 95.46(12) . . ? C3 C2 Fe2 116.67(14) . . ? C1 C2 Fe2 63.68(10) . . ? P1 C2 Fe2 101.83(8) . . ? C4 C3 C2 162.2(2) . . ? C4 C3 Fe3 58.44(13) . . ? C2 C3 Fe3 138.56(14) . . ? C3 C4 Fe4 171.46(19) . . ? C3 C4 Fe3 91.72(15) . . ? Fe4 C4 Fe3 79.73(7) . . ? O11 C11 Fe1 175.07(17) . . ? O12 C12 Fe1 177.6(2) . . ? O13 C13 Fe1 177.84(18) . . ? O21 C21 Fe2 178.74(18) . . ? O22 C22 Fe2 177.2(2) . . ? O23 C23 Fe2 175.8(2) . . ? O31 C31 Fe3 176.1(2) . . ? O32 C32 Fe3 172.3(2) . . ? O33 C33 Fe3 177.4(2) . . ? O41 C41 Fe4 179.3(3) . . ? O42 C42 Fe4 177.5(2) . . ? O43 C43 Fe4 179.1(2) . . ? C52 C51 C56 119.63(17) . . ? C52 C51 P1 122.73(14) . . ? C56 C51 P1 117.64(15) . . ? C51 C52 C53 119.78(19) . . ? C54 C53 C52 120.4(2) . . ? C55 C54 C53 119.96(19) . . ? C54 C55 C56 119.9(2) . . ? C55 C56 C51 120.3(2) . . ? C62 C61 C66 118.5(2) . . ? C62 C61 P1 122.59(14) . . ? C66 C61 P1 118.95(17) . . ? C61 C62 C63 120.48(19) . . ? C64 C63 C62 120.8(2) . . ? C63 C64 C65 119.3(2) . . ? C64 C65 C66 120.7(2) . . ? C65 C66 C61 120.2(2) . . ? C76 C71 C72 118.6(2) . . ? C76 C71 P2 119.98(19) . . ? C72 C71 P2 121.38(19) . . ? C71 C72 C73 119.2(3) . . ? C74 C73 C72 121.3(3) . . ? C73 C74 C75 119.4(2) . . ? C76 C75 C74 120.5(3) . . ? C75 C76 C71 121.0(3) . . ? C86 C81 C82 119.5(2) . . ? C86 C81 P2 121.49(18) . . ? C82 C81 P2 118.7(2) . . ? C83 C82 C81 119.7(3) . . ? C84 C83 C82 120.4(3) . . ? C83 C84 C85 120.6(3) . . ? C84 C85 C86 119.6(3) . . ? C81 C86 C85 120.2(2) . . ? Cl1A C1A Cl2A 93.5(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.412 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.120 #===END data_p47 _database_code_CSD 155051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H62 Fe8 N2 O24 P4' _chemical_formula_weight 2102.08 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 39.793(4) _cell_length_b 11.6394(12) _cell_length_c 19.5520(19) _cell_angle_alpha 90.00 _cell_angle_beta 102.081(2) _cell_angle_gamma 90.00 _cell_volume 8855.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33404 _diffrn_reflns_av_R_equivalents 0.1178 _diffrn_reflns_av_sigmaI/netI 0.1130 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 21.50 _reflns_number_total 10058 _reflns_number_gt 6687 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+24.9712P] 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 10058 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.424 _refine_ls_shift/su_mean 0.045 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 Fe1 Fe 0.33840(3) -0.20971(11) 0.23512(7) 0.0232(4) Uani 1 d . . . Fe2 Fe 0.39571(3) -0.09056(11) 0.23651(7) 0.0208(4) Uani 1 d . . . Fe3 Fe 0.36860(3) 0.08051(11) 0.00161(7) 0.0191(3) Uani 1 d . . . Fe4 Fe 0.42357(3) -0.03686(11) 0.03005(7) 0.0202(4) Uani 1 d . . . P1 P 0.32879(6) -0.1177(2) 0.13265(12) 0.0185(6) Uani 1 d . . . P2 P 0.42034(6) 0.1512(2) 0.04484(13) 0.0207(6) Uani 1 d . . . O11 O 0.2945(2) -0.0536(6) 0.2966(4) 0.047(2) Uani 1 d . . . O12 O 0.3671(2) -0.2925(7) 0.3766(4) 0.049(2) Uani 1 d . . . O13 O 0.2861(2) -0.3923(7) 0.2060(4) 0.053(2) Uani 1 d . . . O21 O 0.46184(19) 0.0206(6) 0.2430(4) 0.0347(18) Uani 1 d . . . O22 O 0.43813(19) -0.2182(6) 0.3518(4) 0.040(2) Uani 1 d . . . O23 O 0.36954(18) 0.0734(6) 0.3276(4) 0.042(2) Uani 1 d . . . O31 O 0.33081(18) 0.2757(6) 0.0416(4) 0.0383(19) Uani 1 d . . . O32 O 0.31171(19) -0.0619(6) -0.0752(4) 0.041(2) Uani 1 d . . . O33 O 0.3703(2) 0.1686(7) -0.1394(4) 0.0601(18) Uani 1 d . . . O41 O 0.41380(19) -0.2853(6) 0.0048(3) 0.038(2) Uani 1 d . . . O42 O 0.4391(2) -0.0148(6) -0.1112(4) 0.043(2) Uani 1 d . . . O43 O 0.48996(19) -0.0567(7) 0.1258(4) 0.049(2) Uani 1 d . . . N1 N 0.3869(2) -0.3886(6) 0.1990(4) 0.025(2) Uani 1 d . . . C1 C 0.3753(2) -0.2810(7) 0.1917(5) 0.022(2) Uani 1 d . . . C01 C 0.4160(2) -0.4295(8) 0.1676(5) 0.028(3) Uani 1 d . . . H01A H 0.4146 -0.5141 0.1628 0.034 Uiso 1 calc R . . H01B H 0.4134 -0.3964 0.1202 0.034 Uiso 1 calc R . . C2 C 0.3924(2) -0.2009(7) 0.1548(4) 0.017(2) Uani 1 d . . . H2 H 0.4136 -0.2247 0.1389 0.021 Uiso 1 calc R . . C02 C 0.4505(3) -0.3985(8) 0.2092(5) 0.038(3) Uani 1 d . . . H02A H 0.4520 -0.3150 0.2153 0.057 Uiso 1 calc R . . H02B H 0.4682 -0.4244 0.1846 0.057 Uiso 1 calc R . . H02C H 0.4541 -0.4357 0.2551 0.057 Uiso 1 calc R . . C3 C 0.3729(2) -0.1009(8) 0.1234(4) 0.018(2) Uani 1 d . . . C4 C 0.3847(2) -0.0316(8) 0.0751(5) 0.0255(18) Uani 1 d . . . C11 C 0.3116(3) -0.1141(9) 0.2717(5) 0.029(3) Uani 1 d . . . C12 C 0.3569(2) -0.2623(9) 0.3205(7) 0.034(3) Uani 1 d . . . C13 C 0.3060(3) -0.3208(10) 0.2145(5) 0.030(3) Uani 1 d . . . C21 C 0.4353(3) -0.0188(8) 0.2336(5) 0.026(3) Uani 1 d . . . C22 C 0.4203(3) -0.1722(9) 0.3073(6) 0.027(3) Uani 1 d . . . C23 C 0.3793(3) 0.0119(10) 0.2899(6) 0.036(3) Uani 1 d . . . C31 C 0.3447(3) 0.1953(9) 0.0284(5) 0.026(3) Uani 1 d . . . C32 C 0.3347(3) -0.0107(9) -0.0405(6) 0.031(3) Uani 1 d . . . C33 C 0.3704(2) 0.1372(8) -0.0845(6) 0.025(2) Uani 1 d . . . C41 C 0.4166(2) -0.1875(10) 0.0146(5) 0.027(3) Uani 1 d . . . C42 C 0.4348(3) -0.0223(8) -0.0556(6) 0.029(3) Uani 1 d . . . C43 C 0.4633(3) -0.0504(9) 0.0906(5) 0.030(3) Uani 1 d . . . C51 C 0.3044(2) 0.0162(8) 0.1173(5) 0.023(2) Uani 1 d . . . C52 C 0.3086(2) 0.1017(8) 0.1688(5) 0.027(3) Uani 1 d . . . H52 H 0.3253 0.0926 0.2110 0.033 Uiso 1 calc R . . C53 C 0.2885(3) 0.1990(8) 0.1581(6) 0.029(3) Uani 1 d . . . H53 H 0.2916 0.2568 0.1932 0.035 Uiso 1 calc R . . C54 C 0.2643(3) 0.2139(9) 0.0984(6) 0.037(3) Uani 1 d . . . H54 H 0.2509 0.2822 0.0923 0.044 Uiso 1 calc R . . C55 C 0.2589(2) 0.1326(9) 0.0472(5) 0.032(3) Uani 1 d . . . H55 H 0.2417 0.1429 0.0060 0.038 Uiso 1 calc R . . C56 C 0.2793(3) 0.0337(9) 0.0567(5) 0.033(3) Uani 1 d . . . H56 H 0.2759 -0.0230 0.0209 0.040 Uiso 1 calc R . . C61 C 0.3074(3) -0.2154(8) 0.0637(5) 0.0294(18) Uani 1 d . . . C62 C 0.2731(3) -0.2434(9) 0.0610(6) 0.044(3) Uani 1 d . . . H62 H 0.2607 -0.2062 0.0912 0.053 Uiso 1 calc R . . C63 C 0.2572(3) -0.3258(10) 0.0139(7) 0.059(4) Uani 1 d . . . H63 H 0.2335 -0.3427 0.0108 0.071 Uiso 1 calc R . . C64 C 0.2751(4) -0.3832(11) -0.0283(7) 0.065(4) Uani 1 d . . . H64 H 0.2642 -0.4409 -0.0596 0.078 Uiso 1 calc R . . C65 C 0.3098(4) -0.3554(10) -0.0244(6) 0.058(4) Uani 1 d . . . H65 H 0.3223 -0.3942 -0.0539 0.069 Uiso 1 calc R . . C66 C 0.3260(3) -0.2741(9) 0.0209(5) 0.033(3) Uani 1 d . . . H66 H 0.3496 -0.2573 0.0234 0.040 Uiso 1 calc R . . C71 C 0.4408(3) 0.2526(8) -0.0036(5) 0.023(2) Uani 1 d . . . C72 C 0.4710(3) 0.2315(9) -0.0237(5) 0.035(3) Uani 1 d . . . H72 H 0.4812 0.1576 -0.0160 0.042 Uiso 1 calc R . . C73 C 0.4871(3) 0.3166(10) -0.0555(5) 0.037(3) Uani 1 d . . . H73 H 0.5087 0.3010 -0.0672 0.044 Uiso 1 calc R . . C74 C 0.4722(3) 0.4224(10) -0.0699(5) 0.044(3) Uani 1 d . . . H74 H 0.4825 0.4788 -0.0941 0.053 Uiso 1 calc R . . C75 C 0.4423(3) 0.4453(10) -0.0490(6) 0.041(3) Uani 1 d . . . H75 H 0.4321 0.5193 -0.0570 0.049 Uiso 1 calc R . . C76 C 0.4265(3) 0.3613(8) -0.0162(5) 0.033(3) Uani 1 d . . . H76 H 0.4057 0.3785 -0.0021 0.040 Uiso 1 calc R . . C81 C 0.4308(2) 0.2139(7) 0.1307(5) 0.019(2) Uani 1 d . . . C82 C 0.4628(2) 0.2592(8) 0.1583(5) 0.028(3) Uani 1 d . . . H82 H 0.4792 0.2609 0.1294 0.033 Uiso 1 calc R . . C83 C 0.4724(3) 0.3024(8) 0.2258(5) 0.031(3) Uani 1 d . . . H83 H 0.4947 0.3326 0.2427 0.037 Uiso 1 calc R . . C84 C 0.4488(3) 0.3001(8) 0.2668(6) 0.035(3) Uani 1 d . . . H84 H 0.4549 0.3292 0.3131 0.042 Uiso 1 calc R . . C85 C 0.4165(3) 0.2568(8) 0.2432(5) 0.030(3) Uani 1 d . . . H85 H 0.4004 0.2564 0.2729 0.035 Uiso 1 calc R . . C86 C 0.4073(3) 0.2135(8) 0.1755(5) 0.023(2) Uani 1 d . . . H86 H 0.3849 0.1832 0.1593 0.027 Uiso 1 calc R . . C91 C 0.3726(3) -0.4792(8) 0.2351(5) 0.031(3) Uani 1 d . . . H91A H 0.3594 -0.4447 0.2675 0.037 Uiso 1 calc R . . H91B H 0.3915 -0.5251 0.2631 0.037 Uiso 1 calc R . . C92 C 0.3492(3) -0.5575(9) 0.1839(6) 0.052(3) Uani 1 d . . . H92A H 0.3302 -0.5125 0.1568 0.078 Uiso 1 calc R . . H92B H 0.3400 -0.6179 0.2098 0.078 Uiso 1 calc R . . H92C H 0.3623 -0.5926 0.1521 0.078 Uiso 1 calc R . . Fe1A Fe 0.06744(4) 0.90588(14) 0.10945(8) 0.0433(5) Uani 1 d . . . Fe2A Fe 0.08594(4) 0.68455(15) 0.10463(9) 0.0521(5) Uani 1 d . . . Fe3A Fe 0.12980(4) 0.51719(13) 0.30648(8) 0.0363(4) Uani 1 d . . . Fe4A Fe 0.17894(4) 0.65423(13) 0.30408(8) 0.0361(4) Uani 1 d . . . P1A P 0.11252(7) 0.8821(3) 0.19741(15) 0.0355(8) Uani 1 d . . . P2A P 0.17622(7) 0.4756(3) 0.26444(15) 0.0358(8) Uani 1 d . . . O11A O 0.1063(2) 1.0375(9) 0.0254(5) 0.086(3) Uani 1 d . . . O12A O 0.0152(3) 0.8855(8) -0.0198(5) 0.082(3) Uani 1 d . . . O13A O 0.0411(3) 1.1128(9) 0.1651(5) 0.086(3) Uani 1 d . . . O21A O 0.0959(2) 0.4364(8) 0.0960(4) 0.061(2) Uani 1 d . . . O22A O 0.0220(3) 0.6277(9) 0.0071(6) 0.123(5) Uani 1 d . . . O23A O 0.1257(3) 0.7382(9) -0.0012(6) 0.105(4) Uani 1 d . . . O31A O 0.0772(2) 0.6225(7) 0.3717(5) 0.071(3) Uani 1 d . . . O32A O 0.0817(3) 0.3495(9) 0.2285(5) 0.097(4) Uani 1 d . . . O33A O 0.1590(2) 0.4085(7) 0.4425(4) 0.0601(18) Uani 1 d . . . O41A O 0.2265(3) 0.5738(8) 0.4286(6) 0.105(4) Uani 1 d . . . O42A O 0.1726(2) 0.8558(8) 0.3893(4) 0.062(3) Uani 1 d . . . O43A O 0.2270(2) 0.7412(7) 0.2231(5) 0.078(3) Uani 1 d . . . N1A N 0.0147(2) 0.7806(11) 0.1719(6) 0.075(4) Uani 1 d . . . C1A C 0.0475(3) 0.7897(11) 0.1638(7) 0.061(4) Uani 1 d . . . C2A C 0.0708(3) 0.7063(10) 0.1972(6) 0.048(3) Uani 1 d . . . H2A H 0.0621 0.6389 0.2201 0.058 Uiso 1 calc R . . C3A C 0.1083(2) 0.7307(9) 0.2114(5) 0.032(3) Uani 1 d . . . C4A C 0.1324(2) 0.6561(8) 0.2521(5) 0.0255(18) Uani 1 d . . . C11A C 0.0919(3) 0.9831(11) 0.0592(6) 0.049(3) Uani 1 d . . . C12A C 0.0348(3) 0.8914(11) 0.0320(7) 0.057(4) Uani 1 d . . . C13A C 0.0504(3) 1.0324(14) 0.1421(7) 0.060(4) Uani 1 d . . . C21A C 0.0932(3) 0.5345(12) 0.1059(7) 0.056(4) Uani 1 d . . . C22A C 0.0471(4) 0.6548(11) 0.0454(8) 0.075(4) Uani 1 d . . . C23A C 0.1110(4) 0.7209(11) 0.0417(8) 0.071(4) Uani 1 d . . . C31A C 0.0988(3) 0.5832(10) 0.3465(7) 0.054(4) Uani 1 d . . . C32A C 0.1014(3) 0.4169(11) 0.2574(7) 0.050(3) Uani 1 d . . . C33A C 0.1478(3) 0.4468(10) 0.3880(7) 0.053(4) Uani 1 d . . . C41A C 0.2089(3) 0.6057(11) 0.3797(7) 0.057(4) Uani 1 d . . . C42A C 0.1735(3) 0.7796(11) 0.3530(6) 0.043(3) Uani 1 d . . . C43A C 0.2075(3) 0.7095(10) 0.2547(7) 0.054(4) Uani 1 d . . . C51A C 0.1069(2) 0.9580(10) 0.2758(6) 0.035(3) Uani 1 d . . . C52A C 0.0944(3) 0.8985(11) 0.3275(6) 0.050(3) Uani 1 d . . . H52A H 0.0898 0.8185 0.3227 0.060 Uiso 1 calc R . . C53A C 0.0889(4) 0.9578(13) 0.3863(7) 0.073(5) Uani 1 d . . . H53A H 0.0801 0.9170 0.4209 0.087 Uiso 1 calc R . . C54A C 0.0955(3) 1.0703(12) 0.3955(7) 0.057(4) Uani 1 d . . . H54A H 0.0922 1.1075 0.4369 0.069 Uiso 1 calc R . . C55A C 0.1072(3) 1.1328(12) 0.3442(7) 0.056(4) Uani 1 d . . . H55A H 0.1121 1.2126 0.3500 0.067 Uiso 1 calc R . . C56A C 0.1117(3) 1.0743(10) 0.2833(6) 0.043(3) Uani 1 d . . . H56A H 0.1181 1.1167 0.2466 0.052 Uiso 1 calc R . . C61A C 0.1547(3) 0.9259(8) 0.1873(5) 0.0294(18) Uani 1 d . . . C62A C 0.1784(3) 0.9785(10) 0.2419(6) 0.042(3) Uani 1 d . . . H62A H 0.1728 0.9876 0.2865 0.051 Uiso 1 calc R . . C63A C 0.2098(3) 1.0172(9) 0.2311(6) 0.045(3) Uani 1 d . . . H63A H 0.2248 1.0571 0.2675 0.054 Uiso 1 calc R . . C64A C 0.2195(3) 0.9991(10) 0.1694(7) 0.053(3) Uani 1 d . . . H64A H 0.2413 1.0246 0.1630 0.063 Uiso 1 calc R . . C65A C 0.1975(3) 0.9437(11) 0.1169(7) 0.053(3) Uani 1 d . . . H65A H 0.2044 0.9291 0.0740 0.064 Uiso 1 calc R . . C66A C 0.1656(3) 0.9086(10) 0.1254(6) 0.050(3) Uani 1 d . . . H66A H 0.1506 0.8716 0.0876 0.060 Uiso 1 calc R . . C71A C 0.1744(3) 0.4409(12) 0.1738(6) 0.050(3) Uani 1 d . . . C72A C 0.1736(3) 0.3239(12) 0.1538(6) 0.058(4) Uani 1 d . . . H72A H 0.1742 0.2661 0.1883 0.069 Uiso 1 calc R . . C73A C 0.1721(3) 0.2923(15) 0.0852(8) 0.078(5) Uani 1 d . . . H73A H 0.1713 0.2134 0.0727 0.093 Uiso 1 calc R . . C74A C 0.1717(3) 0.3734(19) 0.0365(9) 0.084(5) Uani 1 d . . . H74A H 0.1697 0.3505 -0.0109 0.100 Uiso 1 calc R . . C75A C 0.1742(3) 0.4893(17) 0.0524(7) 0.077(5) Uani 1 d . . . H75A H 0.1752 0.5449 0.0173 0.092 Uiso 1 calc R . . C76A C 0.1754(3) 0.5230(14) 0.1230(7) 0.072(5) Uani 1 d . . . H76A H 0.1769 0.6022 0.1353 0.087 Uiso 1 calc R . . C81A C 0.2085(3) 0.3710(9) 0.3074(5) 0.034(3) Uani 1 d . . . C82A C 0.2428(3) 0.3916(10) 0.3070(6) 0.045(3) Uani 1 d . . . H82A H 0.2491 0.4574 0.2839 0.054 Uiso 1 calc R . . C83A C 0.2677(3) 0.3158(12) 0.3404(7) 0.062(4) Uani 1 d . . . H83A H 0.2911 0.3279 0.3382 0.075 Uiso 1 calc R . . C84A C 0.2590(3) 0.2233(11) 0.3767(7) 0.053(3) Uani 1 d . . . H84A H 0.2765 0.1742 0.4014 0.064 Uiso 1 calc R . . C85A C 0.2251(4) 0.2011(10) 0.3778(6) 0.051(3) Uani 1 d . . . H85A H 0.2187 0.1359 0.4014 0.061 Uiso 1 calc R . . C86A C 0.2006(3) 0.2772(10) 0.3431(6) 0.043(3) Uani 1 d . . . H86A H 0.1771 0.2637 0.3442 0.051 Uiso 1 calc R . . C91A C 0.0043(4) 0.6895(18) 0.2145(11) 0.135(9) Uani 1 d . . . H91C H -0.0175 0.7119 0.2274 0.162 Uiso 1 calc R . . H91D H 0.0219 0.6819 0.2583 0.162 Uiso 1 calc R . . C92A C -0.0005(4) 0.5726(17) 0.1778(11) 0.148(10) Uani 1 d . . . H92D H -0.0178 0.5793 0.1342 0.222 Uiso 1 calc R . . H92E H -0.0083 0.5162 0.2084 0.222 Uiso 1 calc R . . H92F H 0.0214 0.5474 0.1674 0.222 Uiso 1 calc R . . C01A C -0.0137(4) 0.8653(15) 0.1402(9) 0.114(7) Uani 1 d . . . H01C H -0.0237 0.8977 0.1783 0.137 Uiso 1 calc R . . H01D H -0.0032 0.9296 0.1187 0.137 Uiso 1 calc R . . C02A C -0.0403(4) 0.8178(14) 0.0894(12) 0.157(10) Uani 1 d . . . H02D H -0.0305 0.7688 0.0579 0.236 Uiso 1 calc R . . H02E H -0.0536 0.8797 0.0625 0.236 Uiso 1 calc R . . H02F H -0.0553 0.7718 0.1124 0.236 Uiso 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 0.0258(9) 0.0245(8) 0.0197(8) 0.0023(7) 0.0059(7) -0.0015(7) Fe2 0.0230(8) 0.0201(8) 0.0177(8) 0.0010(7) 0.0011(6) 0.0003(7) Fe3 0.0229(8) 0.0194(8) 0.0144(8) 0.0020(6) 0.0024(6) 0.0019(7) Fe4 0.0253(8) 0.0197(8) 0.0166(8) -0.0008(7) 0.0067(6) 0.0012(7) P1 0.0211(15) 0.0179(14) 0.0149(14) 0.0030(12) 0.0000(11) -0.0008(12) P2 0.0236(15) 0.0200(15) 0.0186(15) -0.0005(12) 0.0045(12) 0.0011(12) O11 0.053(5) 0.048(5) 0.045(5) 0.009(4) 0.024(4) 0.017(4) O12 0.055(6) 0.055(6) 0.037(5) 0.018(5) 0.005(4) 0.004(4) O13 0.036(5) 0.039(5) 0.083(7) 0.008(5) 0.010(5) -0.011(4) O21 0.030(5) 0.036(5) 0.034(5) -0.001(4) -0.002(4) -0.002(4) O22 0.044(5) 0.040(5) 0.028(5) 0.006(4) -0.012(4) 0.008(4) O23 0.035(5) 0.045(5) 0.043(5) -0.017(4) 0.005(4) 0.005(4) O31 0.040(5) 0.036(5) 0.040(5) -0.005(4) 0.011(4) 0.009(4) O32 0.032(5) 0.050(5) 0.040(5) -0.002(4) 0.006(4) -0.009(4) O33 0.084(5) 0.077(5) 0.025(3) 0.020(3) 0.024(3) 0.017(4) O41 0.064(6) 0.024(5) 0.027(5) -0.005(4) 0.010(4) 0.001(4) O42 0.069(6) 0.051(5) 0.016(4) 0.003(4) 0.025(4) 0.005(4) O43 0.027(5) 0.071(6) 0.045(5) -0.008(4) -0.004(4) 0.016(4) N1 0.029(5) 0.017(5) 0.029(5) 0.006(4) 0.005(4) 0.003(4) C1 0.027(6) 0.004(6) 0.025(6) -0.001(5) -0.016(5) 0.001(5) C01 0.036(7) 0.017(6) 0.031(6) 0.013(5) 0.004(5) 0.003(5) C2 0.027(6) 0.012(5) 0.013(5) -0.002(5) 0.005(5) -0.002(5) C02 0.044(7) 0.026(6) 0.041(7) 0.006(6) 0.002(6) 0.006(6) C3 0.027(6) 0.018(5) 0.009(5) 0.004(5) 0.006(4) 0.007(5) C4 0.030(4) 0.026(4) 0.020(4) -0.013(4) 0.005(3) 0.003(4) C11 0.036(7) 0.035(7) 0.017(6) 0.009(5) 0.009(5) 0.000(6) C12 0.012(6) 0.039(7) 0.051(8) 0.003(7) 0.009(6) -0.002(5) C13 0.029(7) 0.040(7) 0.020(6) 0.004(6) 0.007(5) 0.008(6) C21 0.044(8) 0.007(6) 0.023(6) 0.004(5) -0.003(6) 0.010(5) C22 0.027(6) 0.030(7) 0.024(7) -0.004(6) 0.007(5) -0.005(5) C23 0.033(7) 0.049(8) 0.023(7) 0.012(6) 0.003(6) 0.005(6) C31 0.030(7) 0.033(7) 0.016(6) 0.005(5) 0.007(5) -0.006(6) C32 0.027(7) 0.039(7) 0.032(7) 0.018(6) 0.015(6) 0.017(6) C33 0.024(6) 0.013(5) 0.037(7) -0.009(5) 0.006(5) -0.005(5) C41 0.020(6) 0.047(8) 0.013(6) 0.001(6) 0.006(5) 0.005(6) C42 0.031(7) 0.016(6) 0.036(7) -0.008(6) -0.003(6) -0.004(5) C43 0.035(7) 0.031(7) 0.026(7) 0.003(5) 0.014(6) 0.008(6) C51 0.020(6) 0.022(6) 0.028(7) 0.005(5) 0.006(5) -0.004(5) C52 0.015(6) 0.030(7) 0.032(7) -0.005(6) -0.006(5) -0.009(5) C53 0.030(6) 0.017(6) 0.039(7) 0.003(5) 0.004(6) 0.008(5) C54 0.043(8) 0.024(7) 0.048(8) 0.015(7) 0.022(7) 0.016(6) C55 0.019(6) 0.042(7) 0.030(7) 0.009(6) -0.004(5) 0.015(6) C56 0.035(7) 0.038(7) 0.026(7) 0.004(5) 0.004(6) 0.003(6) C61 0.028(5) 0.030(4) 0.029(5) 0.011(4) 0.002(4) 0.003(4) C62 0.047(8) 0.041(7) 0.041(8) 0.002(6) -0.002(6) -0.023(6) C63 0.052(8) 0.047(9) 0.069(10) -0.007(8) -0.009(8) -0.019(7) C64 0.085(12) 0.054(9) 0.051(9) -0.024(8) 0.001(8) -0.029(9) C65 0.074(10) 0.050(8) 0.055(9) -0.025(7) 0.027(8) -0.020(8) C66 0.046(7) 0.032(7) 0.024(6) -0.002(6) 0.012(6) -0.004(6) C71 0.026(6) 0.012(6) 0.030(6) -0.002(5) 0.007(5) -0.012(5) C72 0.045(8) 0.020(6) 0.040(7) -0.004(5) 0.007(6) -0.003(6) C73 0.028(7) 0.043(8) 0.047(8) -0.014(6) 0.027(6) -0.017(6) C74 0.070(9) 0.037(8) 0.027(7) 0.017(6) 0.012(6) -0.024(7) C75 0.044(8) 0.039(7) 0.039(7) 0.000(6) 0.008(6) -0.009(6) C76 0.046(7) 0.019(6) 0.037(7) 0.001(5) 0.016(6) 0.006(6) C81 0.026(6) 0.011(5) 0.021(6) 0.006(5) 0.002(5) 0.008(5) C82 0.018(6) 0.027(6) 0.036(7) 0.012(5) 0.001(5) 0.000(5) C83 0.043(7) 0.029(6) 0.016(6) -0.013(5) -0.003(6) -0.006(5) C84 0.047(8) 0.027(6) 0.027(7) -0.013(5) -0.004(6) -0.007(6) C85 0.057(8) 0.014(6) 0.022(7) -0.005(5) 0.018(6) -0.003(6) C86 0.033(6) 0.020(6) 0.011(6) 0.001(5) -0.005(5) 0.008(5) C91 0.033(7) 0.022(6) 0.041(7) 0.010(6) 0.013(6) -0.004(5) C92 0.041(7) 0.034(7) 0.077(10) 0.002(7) 0.002(7) 0.005(6) Fe1A 0.0326(10) 0.0554(11) 0.0393(10) 0.0113(9) 0.0017(8) 0.0059(9) Fe2A 0.0508(12) 0.0532(12) 0.0428(11) 0.0012(9) -0.0120(9) -0.0038(9) Fe3A 0.0318(10) 0.0383(10) 0.0365(10) 0.0063(8) 0.0024(8) 0.0011(8) Fe4A 0.0303(9) 0.0367(10) 0.0364(10) 0.0024(8) -0.0043(7) 0.0018(8) P1A 0.0279(17) 0.0454(19) 0.0321(18) 0.0071(15) 0.0042(14) 0.0016(15) P2A 0.0368(18) 0.0388(18) 0.0292(18) 0.0003(15) 0.0007(14) -0.0029(15) O11A 0.065(7) 0.125(9) 0.069(7) 0.046(7) 0.015(6) -0.001(6) O12A 0.081(7) 0.090(8) 0.061(7) -0.006(6) -0.018(6) 0.003(6) O13A 0.073(7) 0.107(9) 0.072(7) -0.007(6) 0.005(6) 0.041(7) O21A 0.054(6) 0.057(6) 0.065(6) 0.000(5) -0.005(5) -0.001(5) O22A 0.112(9) 0.084(8) 0.125(10) -0.013(7) -0.083(8) -0.004(7) O23A 0.183(12) 0.080(8) 0.064(8) -0.017(6) 0.055(8) -0.046(8) O31A 0.070(7) 0.062(6) 0.089(7) 0.014(5) 0.039(6) 0.022(5) O32A 0.103(8) 0.081(8) 0.086(8) 0.019(6) -0.025(6) -0.041(7) O33A 0.084(5) 0.077(5) 0.025(3) 0.020(3) 0.024(3) 0.017(4) O41A 0.114(9) 0.064(7) 0.105(9) -0.012(7) -0.049(7) 0.023(6) O42A 0.068(6) 0.067(7) 0.040(6) -0.008(5) -0.014(5) 0.019(5) O43A 0.071(7) 0.053(6) 0.128(9) 0.013(6) 0.061(7) 0.013(5) N1A 0.019(6) 0.126(10) 0.075(8) 0.056(8) -0.002(5) 0.000(6) C1A 0.015(7) 0.081(10) 0.082(10) 0.017(8) -0.002(6) -0.008(7) C2A 0.047(8) 0.041(7) 0.052(8) 0.007(7) -0.002(6) -0.010(7) C3A 0.017(6) 0.054(8) 0.023(6) 0.000(6) -0.001(5) -0.001(5) C4A 0.030(4) 0.026(4) 0.020(4) -0.013(4) 0.005(3) 0.003(4) C11A 0.041(8) 0.064(9) 0.040(8) 0.006(7) 0.002(6) 0.008(7) C12A 0.065(9) 0.055(9) 0.044(9) 0.014(7) -0.008(8) -0.002(7) C13A 0.046(9) 0.097(12) 0.037(8) 0.019(8) 0.007(7) 0.034(8) C21A 0.045(8) 0.051(9) 0.063(10) 0.004(8) -0.010(7) -0.008(7) C22A 0.088(11) 0.051(9) 0.066(10) 0.001(8) -0.027(9) 0.017(8) C23A 0.110(13) 0.048(9) 0.045(10) 0.000(8) -0.005(9) -0.033(9) C31A 0.053(9) 0.047(8) 0.055(9) 0.032(7) -0.004(7) 0.009(7) C32A 0.043(8) 0.046(8) 0.060(9) 0.015(7) 0.012(7) -0.007(7) C33A 0.055(8) 0.059(9) 0.053(9) 0.011(7) 0.031(7) 0.023(7) C41A 0.050(8) 0.042(8) 0.063(10) -0.003(7) -0.024(7) 0.018(7) C42A 0.022(7) 0.054(9) 0.044(9) 0.007(7) -0.011(6) 0.010(6) C43A 0.032(8) 0.044(8) 0.084(11) 0.007(7) 0.009(7) 0.011(6) C51A 0.010(6) 0.057(9) 0.039(7) 0.008(7) 0.003(5) -0.001(6) C52A 0.048(8) 0.057(8) 0.050(8) 0.013(7) 0.021(7) 0.031(7) C53A 0.106(12) 0.063(10) 0.066(11) 0.039(9) 0.057(9) 0.039(9) C54A 0.066(9) 0.066(10) 0.043(8) 0.014(8) 0.021(7) 0.029(8) C55A 0.040(8) 0.067(9) 0.059(9) -0.022(8) 0.005(7) -0.003(7) C56A 0.048(8) 0.041(8) 0.046(8) 0.005(7) 0.018(6) 0.000(6) C61A 0.028(5) 0.030(4) 0.029(5) 0.011(4) 0.002(4) 0.003(4) C62A 0.025(7) 0.060(8) 0.035(7) 0.006(6) -0.010(6) -0.003(6) C63A 0.033(8) 0.040(7) 0.056(9) -0.014(6) -0.004(6) -0.005(6) C64A 0.045(8) 0.059(9) 0.060(9) -0.005(7) 0.024(8) -0.012(7) C65A 0.043(8) 0.071(9) 0.053(9) -0.008(8) 0.027(7) -0.010(7) C66A 0.050(8) 0.058(8) 0.037(8) -0.007(7) 0.001(6) -0.018(7) C71A 0.047(8) 0.082(11) 0.019(7) 0.006(7) 0.001(6) 0.004(7) C72A 0.058(9) 0.078(11) 0.037(9) 0.003(8) 0.009(7) 0.023(8) C73A 0.066(10) 0.112(14) 0.045(10) -0.030(10) -0.012(8) 0.027(10) C74A 0.021(8) 0.162(19) 0.064(12) -0.028(13) 0.001(8) 0.004(10) C75A 0.055(10) 0.138(16) 0.037(10) 0.019(10) 0.006(7) -0.026(10) C76A 0.033(8) 0.141(14) 0.037(9) -0.006(10) -0.004(6) -0.028(8) C81A 0.026(7) 0.038(7) 0.037(7) -0.022(6) 0.004(5) -0.002(6) C82A 0.058(9) 0.044(8) 0.033(7) 0.004(6) 0.009(6) 0.003(7) C83A 0.040(8) 0.064(10) 0.076(10) -0.014(9) -0.006(8) 0.018(8) C84A 0.051(10) 0.048(9) 0.056(9) -0.003(7) 0.001(7) 0.020(7) C85A 0.072(10) 0.034(8) 0.048(8) -0.002(6) 0.012(7) 0.006(7) C86A 0.033(7) 0.044(8) 0.049(8) 0.001(7) 0.005(6) 0.003(7) C91A 0.037(10) 0.20(2) 0.17(2) 0.13(2) 0.026(11) -0.001(13) C92A 0.066(12) 0.143(18) 0.20(2) 0.112(18) -0.038(13) -0.050(13) C01A 0.055(11) 0.150(17) 0.126(15) 0.087(14) -0.007(10) -0.005(11) C02A 0.054(11) 0.110(15) 0.27(3) 0.100(16) -0.051(14) -0.051(10) _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 C12 1.786(13) . ? Fe1 C11 1.791(12) . ? Fe1 C13 1.812(12) . ? Fe1 C1 2.020(9) . ? Fe1 P1 2.233(3) . ? Fe1 Fe2 2.6645(19) . ? Fe2 C22 1.791(12) . ? Fe2 C23 1.794(13) . ? Fe2 C21 1.793(12) . ? Fe2 C2 2.033(9) . ? Fe2 C3 2.212(9) . ? Fe2 C1 2.458(9) . ? Fe3 C32 1.778(13) . ? Fe3 C31 1.782(12) . ? Fe3 C33 1.823(11) . ? Fe3 C4 1.947(10) . ? Fe3 P2 2.214(3) . ? Fe3 Fe4 2.5399(18) . ? Fe4 C43 1.771(12) . ? Fe4 C41 1.792(12) . ? Fe4 C42 1.829(12) . ? Fe4 C4 1.933(9) . ? Fe4 P2 2.216(3) . ? P1 C3 1.813(9) . ? P1 C51 1.826(10) . ? P1 C61 1.831(10) . ? P2 C81 1.798(9) . ? P2 C71 1.809(9) . ? O11 C11 1.153(11) . ? O12 C12 1.143(12) . ? O13 C13 1.136(11) . ? O21 C21 1.132(11) . ? O22 C22 1.136(11) . ? O23 C23 1.154(11) . ? O31 C31 1.142(11) . ? O32 C32 1.180(12) . ? O33 C33 1.134(10) . ? O41 C41 1.155(11) . ? O42 C42 1.137(11) . ? O43 C43 1.141(11) . ? N1 C1 1.333(11) . ? N1 C91 1.449(11) . ? N1 C01 1.498(11) . ? C1 C2 1.434(12) . ? C01 C02 1.485(13) . ? C2 C3 1.461(12) . ? C3 C4 1.396(12) . ? C51 C56 1.398(13) . ? C51 C52 1.400(13) . ? C52 C53 1.377(13) . ? C53 C54 1.361(14) . ? C54 C55 1.361(13) . ? C55 C56 1.398(13) . ? C61 C62 1.395(14) . ? C61 C66 1.404(13) . ? C62 C63 1.388(15) . ? C63 C64 1.371(17) . ? C64 C65 1.406(17) . ? C65 C66 1.361(14) . ? C71 C72 1.362(13) . ? C71 C76 1.388(13) . ? C72 C73 1.396(13) . ? C73 C74 1.371(14) . ? C74 C75 1.364(14) . ? C75 C76 1.389(13) . ? C81 C82 1.379(13) . ? C81 C86 1.409(12) . ? C82 C83 1.389(13) . ? C83 C84 1.354(13) . ? C84 C85 1.369(14) . ? C85 C86 1.391(12) . ? C91 C92 1.519(14) . ? Fe1A C11A 1.766(14) . ? Fe1A C12A 1.785(14) . ? Fe1A C13A 1.794(15) . ? Fe1A C1A 1.984(12) . ? Fe1A P1A 2.227(3) . ? Fe1A Fe2A 2.686(2) . ? Fe2A C22A 1.762(15) . ? Fe2A C21A 1.769(14) . ? Fe2A C23A 1.790(17) . ? Fe2A C2A 2.039(12) . ? Fe2A C3A 2.159(10) . ? Fe2A C1A 2.432(13) . ? Fe3A C32A 1.763(14) . ? Fe3A C31A 1.768(15) . ? Fe3A C33A 1.802(13) . ? Fe3A C4A 1.950(10) . ? Fe3A P2A 2.227(3) . ? Fe3A Fe4A 2.532(2) . ? Fe4A C43A 1.759(14) . ? Fe4A C42A 1.783(14) . ? Fe4A C41A 1.786(14) . ? Fe4A C4A 1.916(10) . ? Fe4A P2A 2.214(3) . ? P1A C3A 1.797(11) . ? P1A C61A 1.804(10) . ? P1A C51A 1.824(11) . ? P2A C71A 1.803(12) . ? P2A C81A 1.841(11) . ? O11A C11A 1.150(13) . ? O12A C12A 1.143(13) . ? O13A C13A 1.134(14) . ? O21A C21A 1.167(13) . ? O22A C22A 1.159(15) . ? O23A C23A 1.136(15) . ? O31A C31A 1.169(13) . ? O32A C32A 1.167(13) . ? O33A C33A 1.154(12) . ? O41A C41A 1.122(13) . ? O42A C42A 1.141(12) . ? O43A C43A 1.150(13) . ? N1A C1A 1.352(13) . ? N1A C91A 1.461(17) . ? N1A C01A 1.530(17) . ? C1A C2A 1.405(15) . ? C2A C3A 1.487(14) . ? C3A C4A 1.410(13) . ? C51A C56A 1.370(14) . ? C51A C52A 1.400(14) . ? C52A C53A 1.396(16) . ? C53A C54A 1.341(17) . ? C54A C55A 1.397(16) . ? C55A C56A 1.415(15) . ? C61A C66A 1.384(14) . ? C61A C62A 1.407(14) . ? C62A C63A 1.384(14) . ? C63A C64A 1.357(15) . ? C64A C65A 1.362(16) . ? C65A C66A 1.379(15) . ? C71A C76A 1.385(17) . ? C71A C72A 1.415(16) . ? C72A C73A 1.380(17) . ? C73A C74A 1.34(2) . ? C74A C75A 1.38(2) . ? C75A C76A 1.427(18) . ? C81A C86A 1.368(14) . ? C81A C82A 1.385(14) . ? C82A C83A 1.385(15) . ? C83A C84A 1.374(16) . ? C84A C85A 1.377(16) . ? C85A C86A 1.385(15) . ? C91A C92A 1.53(3) . ? C01A C02A 1.40(2) . ? 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 C12 Fe1 C11 90.2(4) . . ? C12 Fe1 C13 95.6(4) . . ? C11 Fe1 C13 94.4(4) . . ? C12 Fe1 C1 93.4(4) . . ? C11 Fe1 C1 165.6(4) . . ? C13 Fe1 C1 99.2(4) . . ? C12 Fe1 P1 164.4(3) . . ? C11 Fe1 P1 93.2(3) . . ? C13 Fe1 P1 99.3(3) . . ? C1 Fe1 P1 79.8(3) . . ? C12 Fe1 Fe2 89.1(3) . . ? C11 Fe1 Fe2 104.6(3) . . ? C13 Fe1 Fe2 160.4(3) . . ? C1 Fe1 Fe2 61.5(2) . . ? P1 Fe1 Fe2 75.23(8) . . ? C22 Fe2 C23 96.3(4) . . ? C22 Fe2 C21 86.0(4) . . ? C23 Fe2 C21 97.9(5) . . ? C22 Fe2 C2 102.0(4) . . ? C23 Fe2 C2 154.8(4) . . ? C21 Fe2 C2 100.5(4) . . ? C22 Fe2 C3 141.9(4) . . ? C23 Fe2 C3 119.7(4) . . ? C21 Fe2 C3 99.9(4) . . ? C2 Fe2 C3 40.0(3) . . ? C22 Fe2 C1 83.3(4) . . ? C23 Fe2 C1 132.3(4) . . ? C21 Fe2 C1 129.5(4) . . ? C2 Fe2 C1 35.7(3) . . ? C3 Fe2 C1 63.8(3) . . ? C22 Fe2 Fe1 93.4(3) . . ? C23 Fe2 Fe1 86.4(3) . . ? C21 Fe2 Fe1 175.7(3) . . ? C2 Fe2 Fe1 75.4(3) . . ? C3 Fe2 Fe1 77.9(2) . . ? C1 Fe2 Fe1 46.2(2) . . ? C32 Fe3 C31 100.5(4) . . ? C32 Fe3 C33 87.8(4) . . ? C31 Fe3 C33 97.3(4) . . ? C32 Fe3 C4 92.4(4) . . ? C31 Fe3 C4 113.6(4) . . ? C33 Fe3 C4 148.5(4) . . ? C32 Fe3 P2 162.5(3) . . ? C31 Fe3 P2 96.9(3) . . ? C33 Fe3 P2 90.3(3) . . ? C4 Fe3 P2 80.3(3) . . ? C32 Fe3 Fe4 108.4(3) . . ? C31 Fe3 Fe4 145.9(3) . . ? C33 Fe3 Fe4 101.5(3) . . ? C4 Fe3 Fe4 48.9(3) . . ? P2 Fe3 Fe4 55.04(8) . . ? C43 Fe4 C41 96.4(4) . . ? C43 Fe4 C42 105.4(4) . . ? C41 Fe4 C42 89.7(4) . . ? C43 Fe4 C4 112.6(4) . . ? C41 Fe4 C4 89.8(4) . . ? C42 Fe4 C4 141.8(4) . . ? C43 Fe4 P2 93.9(3) . . ? C41 Fe4 P2 168.0(3) . . ? C42 Fe4 P2 93.5(3) . . ? C4 Fe4 P2 80.5(3) . . ? C43 Fe4 Fe3 143.2(3) . . ? C41 Fe4 Fe3 113.2(3) . . ? C42 Fe4 Fe3 96.6(3) . . ? C4 Fe4 Fe3 49.4(3) . . ? P2 Fe4 Fe3 54.99(8) . . ? C3 P1 C51 112.5(4) . . ? C3 P1 C61 107.7(4) . . ? C51 P1 C61 105.1(5) . . ? C3 P1 Fe1 98.9(3) . . ? C51 P1 Fe1 122.8(3) . . ? C61 P1 Fe1 109.2(3) . . ? C81 P2 C71 100.5(4) . . ? C81 P2 Fe3 121.5(3) . . ? C71 P2 Fe3 121.8(3) . . ? C81 P2 Fe4 121.0(3) . . ? C71 P2 Fe4 122.1(3) . . ? Fe3 P2 Fe4 69.97(9) . . ? C1 N1 C91 125.0(8) . . ? C1 N1 C01 122.4(8) . . ? C91 N1 C01 112.5(7) . . ? N1 C1 C2 118.2(8) . . ? N1 C1 Fe1 127.4(7) . . ? C2 C1 Fe1 114.0(6) . . ? N1 C1 Fe2 136.6(6) . . ? C2 C1 Fe2 55.8(4) . . ? Fe1 C1 Fe2 72.3(3) . . ? C02 C01 N1 113.8(8) . . ? C1 C2 C3 117.6(8) . . ? C1 C2 Fe2 88.6(5) . . ? C3 C2 Fe2 76.6(5) . . ? C4 C3 C2 121.4(8) . . ? C4 C3 P1 126.9(7) . . ? C2 C3 P1 108.1(6) . . ? C4 C3 Fe2 121.3(7) . . ? C2 C3 Fe2 63.4(4) . . ? P1 C3 Fe2 96.2(4) . . ? C3 C4 Fe4 134.8(7) . . ? C3 C4 Fe3 141.3(7) . . ? Fe4 C4 Fe3 81.8(4) . . ? O11 C11 Fe1 178.5(8) . . ? O12 C12 Fe1 175.8(9) . . ? O13 C13 Fe1 175.5(9) . . ? O21 C21 Fe2 168.4(9) . . ? O22 C22 Fe2 174.3(9) . . ? O23 C23 Fe2 175.9(9) . . ? O31 C31 Fe3 173.3(8) . . ? O32 C32 Fe3 171.7(9) . . ? O33 C33 Fe3 176.7(9) . . ? O41 C41 Fe4 176.6(9) . . ? O42 C42 Fe4 174.4(9) . . ? O43 C43 Fe4 175.0(9) . . ? C56 C51 C52 117.6(9) . . ? C56 C51 P1 121.7(8) . . ? C52 C51 P1 120.6(7) . . ? C53 C52 C51 119.9(9) . . ? C54 C53 C52 121.3(10) . . ? C55 C54 C53 121.1(10) . . ? C54 C55 C56 118.5(10) . . ? C51 C56 C55 121.6(10) . . ? C62 C61 C66 119.8(10) . . ? C62 C61 P1 118.2(8) . . ? C66 C61 P1 121.3(8) . . ? C61 C62 C63 119.6(11) . . ? C64 C63 C62 120.9(12) . . ? C63 C64 C65 119.0(12) . . ? C66 C65 C64 121.4(11) . . ? C65 C66 C61 119.3(10) . . ? C72 C71 C76 117.7(9) . . ? C72 C71 P2 123.7(8) . . ? C76 C71 P2 118.4(8) . . ? C71 C72 C73 121.1(10) . . ? C74 C73 C72 120.6(10) . . ? C75 C74 C73 118.8(10) . . ? C74 C75 C76 120.5(10) . . ? C75 C76 C71 121.2(10) . . ? C82 C81 C86 115.9(9) . . ? C82 C81 P2 122.2(7) . . ? C86 C81 P2 121.7(7) . . ? C81 C82 C83 123.8(9) . . ? C84 C83 C82 117.9(10) . . ? C83 C84 C85 121.8(10) . . ? C84 C85 C86 119.7(9) . . ? C85 C86 C81 120.9(9) . . ? N1 C91 C92 111.4(9) . . ? C11A Fe1A C12A 87.9(6) . . ? C11A Fe1A C13A 94.2(6) . . ? C12A Fe1A C13A 96.8(6) . . ? C11A Fe1A C1A 166.6(5) . . ? C12A Fe1A C1A 95.1(5) . . ? C13A Fe1A C1A 98.4(6) . . ? C11A Fe1A P1A 92.5(4) . . ? C12A Fe1A P1A 165.7(4) . . ? C13A Fe1A P1A 97.5(4) . . ? C1A Fe1A P1A 81.3(4) . . ? C11A Fe1A Fe2A 106.4(4) . . ? C12A Fe1A Fe2A 92.1(4) . . ? C13A Fe1A Fe2A 157.9(4) . . ? C1A Fe1A Fe2A 60.6(4) . . ? P1A Fe1A Fe2A 74.08(9) . . ? C22A Fe2A C21A 86.2(6) . . ? C22A Fe2A C23A 97.7(7) . . ? C21A Fe2A C23A 97.5(6) . . ? C22A Fe2A C2A 103.1(6) . . ? C21A Fe2A C2A 100.8(5) . . ? C23A Fe2A C2A 153.1(5) . . ? C22A Fe2A C3A 144.3(6) . . ? C21A Fe2A C3A 101.5(5) . . ? C23A Fe2A C3A 115.5(5) . . ? C2A Fe2A C3A 41.4(4) . . ? C22A Fe2A C1A 81.9(6) . . ? C21A Fe2A C1A 127.4(5) . . ? C23A Fe2A C1A 134.8(6) . . ? C2A Fe2A C1A 35.3(4) . . ? C3A Fe2A C1A 65.6(4) . . ? C22A Fe2A Fe1A 90.1(4) . . ? C21A Fe2A Fe1A 172.3(4) . . ? C23A Fe2A Fe1A 89.6(5) . . ? C2A Fe2A Fe1A 73.5(3) . . ? C3A Fe2A Fe1A 77.8(3) . . ? C1A Fe2A Fe1A 45.3(3) . . ? C32A Fe3A C31A 95.8(6) . . ? C32A Fe3A C33A 105.8(6) . . ? C31A Fe3A C33A 89.5(5) . . ? C32A Fe3A C4A 110.7(5) . . ? C31A Fe3A C4A 90.2(4) . . ? C33A Fe3A C4A 143.4(5) . . ? C32A Fe3A P2A 98.2(4) . . ? C31A Fe3A P2A 165.2(4) . . ? C33A Fe3A P2A 91.2(3) . . ? C4A Fe3A P2A 80.5(3) . . ? C32A Fe3A Fe4A 144.8(4) . . ? C31A Fe3A Fe4A 110.3(4) . . ? C33A Fe3A Fe4A 97.9(4) . . ? C4A Fe3A Fe4A 48.5(3) . . ? P2A Fe3A Fe4A 55.01(9) . . ? C43A Fe4A C42A 99.2(5) . . ? C43A Fe4A C41A 100.1(6) . . ? C42A Fe4A C41A 87.1(5) . . ? C43A Fe4A C4A 111.5(5) . . ? C42A Fe4A C4A 93.6(4) . . ? C41A Fe4A C4A 147.8(5) . . ? C43A Fe4A P2A 98.1(4) . . ? C42A Fe4A P2A 162.6(4) . . ? C41A Fe4A P2A 88.2(4) . . ? C4A Fe4A P2A 81.6(3) . . ? C43A Fe4A Fe3A 146.1(4) . . ? C42A Fe4A Fe3A 108.9(4) . . ? C41A Fe4A Fe3A 99.8(4) . . ? C4A Fe4A Fe3A 49.7(3) . . ? P2A Fe4A Fe3A 55.48(9) . . ? C3A P1A C61A 114.3(4) . . ? C3A P1A C51A 108.4(5) . . ? C61A P1A C51A 103.7(5) . . ? C3A P1A Fe1A 98.8(3) . . ? C61A P1A Fe1A 119.9(3) . . ? C51A P1A Fe1A 111.6(3) . . ? C71A P2A C81A 100.4(5) . . ? C71A P2A Fe4A 122.9(5) . . ? C81A P2A Fe4A 118.9(3) . . ? C71A P2A Fe3A 123.1(4) . . ? C81A P2A Fe3A 122.0(4) . . ? Fe4A P2A Fe3A 69.51(10) . . ? C1A N1A C91A 121.3(11) . . ? C1A N1A C01A 123.5(11) . . ? C91A N1A C01A 115.2(11) . . ? N1A C1A C2A 116.8(11) . . ? N1A C1A Fe1A 128.3(10) . . ? C2A C1A Fe1A 114.9(8) . . ? N1A C1A Fe2A 137.3(10) . . ? C2A C1A Fe2A 56.9(7) . . ? Fe1A C1A Fe2A 74.2(4) . . ? C1A C2A C3A 119.5(10) . . ? C1A C2A Fe2A 87.8(8) . . ? C3A C2A Fe2A 73.6(6) . . ? C4A C3A C2A 121.7(9) . . ? C4A C3A P1A 128.0(8) . . ? C2A C3A P1A 106.3(7) . . ? C4A C3A Fe2A 119.1(7) . . ? C2A C3A Fe2A 65.0(6) . . ? P1A C3A Fe2A 97.4(5) . . ? C3A C4A Fe4A 140.7(8) . . ? C3A C4A Fe3A 135.2(7) . . ? Fe4A C4A Fe3A 81.8(4) . . ? O11A C11A Fe1A 176.2(11) . . ? O12A C12A Fe1A 175.7(12) . . ? O13A C13A Fe1A 176.8(12) . . ? O21A C21A Fe2A 169.7(12) . . ? O22A C22A Fe2A 175.5(13) . . ? O23A C23A Fe2A 175.2(12) . . ? O31A C31A Fe3A 176.6(12) . . ? O32A C32A Fe3A 175.9(11) . . ? O33A C33A Fe3A 175.4(11) . . ? O41A C41A Fe4A 176.8(14) . . ? O42A C42A Fe4A 173.2(10) . . ? O43A C43A Fe4A 176.9(10) . . ? C56A C51A C52A 118.4(11) . . ? C56A C51A P1A 121.9(9) . . ? C52A C51A P1A 119.5(9) . . ? C53A C52A C51A 119.3(12) . . ? C54A C53A C52A 122.3(12) . . ? C53A C54A C55A 119.8(12) . . ? C54A C55A C56A 118.3(12) . . ? C51A C56A C55A 121.7(11) . . ? C66A C61A C62A 116.4(10) . . ? C66A C61A P1A 121.5(8) . . ? C62A C61A P1A 122.1(8) . . ? C63A C62A C61A 120.5(10) . . ? C64A C63A C62A 121.3(11) . . ? C63A C64A C65A 119.0(11) . . ? C64A C65A C66A 120.8(11) . . ? C65A C66A C61A 121.8(11) . . ? C76A C71A C72A 117.9(12) . . ? C76A C71A P2A 123.3(11) . . ? C72A C71A P2A 118.7(10) . . ? C73A C72A C71A 121.3(13) . . ? C74A C73A C72A 119.7(16) . . ? C73A C74A C75A 122.5(16) . . ? C74A C75A C76A 118.2(15) . . ? C71A C76A C75A 120.2(15) . . ? C86A C81A C82A 118.3(10) . . ? C86A C81A P2A 123.1(8) . . ? C82A C81A P2A 118.4(9) . . ? C81A C82A C83A 119.7(11) . . ? C84A C83A C82A 120.6(12) . . ? C85A C84A C83A 120.5(12) . . ? C84A C85A C86A 117.7(11) . . ? C81A C86A C85A 123.1(11) . . ? N1A C91A C92A 113.6(17) . . ? C02A C01A N1A 114.6(16) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 21.50 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.775 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.098 #===END data_pjl44 _database_code_CSD 155052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H31 Fe4 N O12 P2' _chemical_formula_weight 1051.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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 14.4035(10) _cell_length_b 21.8794(15) _cell_length_c 14.4482(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.52(5) _cell_angle_gamma 90.00 _cell_volume 4387.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37566 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10107 _reflns_number_gt 7001 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+2.9523P] 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 10107 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.417 _refine_ls_shift/su_mean 0.064 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 Fe1 Fe 0.34365(3) 0.75685(2) 0.05142(3) 0.02229(12) Uani 1 d . . . Fe2 Fe 0.26390(3) 0.91451(2) 0.07195(3) 0.02022(11) Uani 1 d . . . Fe3 Fe 0.14989(3) 0.96172(2) 0.18747(3) 0.02066(11) Uani 1 d . . . Fe4 Fe 0.28144(3) 0.92671(2) 0.33731(3) 0.02213(12) Uani 1 d . . . P1 P 0.36440(6) 0.85705(4) 0.00937(6) 0.02167(19) Uani 1 d . . . P2 P 0.13092(6) 0.89331(4) 0.29529(6) 0.02149(19) Uani 1 d . . . O5 O 0.39598(18) 0.79322(12) 0.25367(17) 0.0326(6) Uani 1 d . . . O11 O 0.54963(19) 0.73781(13) 0.14537(19) 0.0395(7) Uani 1 d . . . O12 O 0.2899(2) 0.64546(13) 0.1381(2) 0.0431(7) Uani 1 d . . . O13 O 0.3811(2) 0.71011(13) -0.12783(19) 0.0448(7) Uani 1 d . . . O21 O 0.1551(2) 0.96929(13) -0.11047(18) 0.0411(7) Uani 1 d . . . O22 O 0.40945(19) 1.01068(13) 0.1062(2) 0.0461(7) Uani 1 d . . . O31 O 0.2262(2) 1.07443(13) 0.1249(2) 0.0487(8) Uani 1 d . . . O32 O 0.0539(2) 1.05344(12) 0.27746(19) 0.0388(7) Uani 1 d . . . O33 O -0.01950(19) 0.93182(13) 0.02980(19) 0.0395(7) Uani 1 d . . . O41 O 0.4569(2) 0.99046(16) 0.3245(2) 0.0608(9) Uani 1 d . . . O42 O 0.3642(2) 0.82643(14) 0.4669(2) 0.0465(7) Uani 1 d . . . O43 O 0.2656(2) 1.01046(13) 0.49165(19) 0.0413(7) Uani 1 d . . . N1 N 0.1292(2) 0.75377(13) -0.04770(19) 0.0236(6) Uani 1 d . . . C1 C 0.2038(2) 0.78029(15) 0.0129(2) 0.0220(7) Uani 1 d . . . C2 C 0.1849(2) 0.83280(15) 0.0672(2) 0.0210(7) Uani 1 d . . . H2 H 0.124(2) 0.8428(15) 0.065(2) 0.018(9) Uiso 1 d . . . C3 C 0.2557(2) 0.84277(15) 0.1568(2) 0.0200(7) Uani 1 d . . . C4 C 0.2546(2) 0.89673(15) 0.2074(2) 0.0197(7) Uani 1 d . . . C5 C 0.3399(2) 0.79862(15) 0.1760(2) 0.0227(7) Uani 1 d . . . C11 C 0.4707(3) 0.74593(16) 0.1073(3) 0.0286(8) Uani 1 d . . . C12 C 0.3107(3) 0.68723(18) 0.1025(3) 0.0290(8) Uani 1 d . . . C13 C 0.3620(3) 0.72786(17) -0.0621(3) 0.0293(8) Uani 1 d . . . C21 C 0.1981(3) 0.94661(16) -0.0412(3) 0.0268(8) Uani 1 d . . . C22 C 0.3522(3) 0.97328(18) 0.0961(3) 0.0297(8) Uani 1 d . . . C31 C 0.2022(3) 1.02820(18) 0.1460(3) 0.0323(9) Uani 1 d . . . C32 C 0.0904(3) 1.01656(16) 0.2441(2) 0.0256(8) Uani 1 d . . . C33 C 0.0487(3) 0.94343(16) 0.0894(2) 0.0266(8) Uani 1 d . . . C41 C 0.3878(3) 0.96616(19) 0.3282(3) 0.0340(9) Uani 1 d . . . C42 C 0.3340(3) 0.86475(18) 0.4132(3) 0.0296(8) Uani 1 d . . . C43 C 0.2679(2) 0.97765(17) 0.4309(3) 0.0280(8) Uani 1 d . . . C51 C 0.3381(2) 0.87371(16) -0.1196(2) 0.0245(7) Uani 1 d . . . C52 C 0.3804(3) 0.92427(17) -0.1496(2) 0.0292(8) Uani 1 d . . . H52 H 0.4246 0.9485 -0.1036 0.035 Uiso 1 calc R . . C53 C 0.3588(3) 0.93969(19) -0.2461(3) 0.0371(9) Uani 1 d . . . H53 H 0.3883 0.9743 -0.2660 0.044 Uiso 1 calc R . . C54 C 0.2945(3) 0.9048(2) -0.3128(3) 0.0396(10) Uani 1 d . . . H54 H 0.2808 0.9150 -0.3790 0.047 Uiso 1 calc R . . C55 C 0.2499(3) 0.85551(19) -0.2847(3) 0.0353(9) Uani 1 d . . . H55 H 0.2043 0.8323 -0.3311 0.042 Uiso 1 calc R . . C56 C 0.2719(3) 0.83950(17) -0.1874(2) 0.0282(8) Uani 1 d . . . H56 H 0.2414 0.8052 -0.1678 0.034 Uiso 1 calc R . . C61 C 0.4948(2) 0.87212(16) 0.0513(3) 0.0273(8) Uani 1 d . . . C62 C 0.5364(3) 0.89052(17) 0.1451(3) 0.0338(9) Uani 1 d . . . H62 H 0.4964 0.9010 0.1854 0.041 Uiso 1 calc R . . C63 C 0.6362(3) 0.8937(2) 0.1807(3) 0.0464(11) Uani 1 d . . . H63 H 0.6641 0.9066 0.2449 0.056 Uiso 1 calc R . . C64 C 0.6945(3) 0.8782(2) 0.1223(4) 0.0549(13) Uani 1 d . . . H64 H 0.7626 0.8806 0.1463 0.066 Uiso 1 calc R . . C65 C 0.6539(3) 0.8594(2) 0.0296(3) 0.0492(12) Uani 1 d . . . H65 H 0.6943 0.8487 -0.0102 0.059 Uiso 1 calc R . . C66 C 0.5552(3) 0.85578(19) -0.0065(3) 0.0375(9) Uani 1 d . . . H66 H 0.5280 0.8422 -0.0705 0.045 Uiso 1 calc R . . C71 C 0.0493(2) 0.90911(15) 0.3698(2) 0.0232(7) Uani 1 d . . . C72 C -0.0418(2) 0.93442(16) 0.3332(2) 0.0275(8) Uani 1 d . . . H72 H -0.0630 0.9448 0.2670 0.033 Uiso 1 calc R . . C73 C -0.1016(3) 0.94464(17) 0.3922(3) 0.0331(9) Uani 1 d . . . H73 H -0.1636 0.9620 0.3666 0.040 Uiso 1 calc R . . C74 C -0.0709(3) 0.92948(17) 0.4886(3) 0.0360(9) Uani 1 d . . . H74 H -0.1121 0.9363 0.5292 0.043 Uiso 1 calc R . . C75 C 0.0195(3) 0.90440(17) 0.5261(3) 0.0313(8) Uani 1 d . . . H75 H 0.0408 0.8943 0.5924 0.038 Uiso 1 calc R . . C76 C 0.0789(3) 0.89404(16) 0.4665(2) 0.0276(8) Uani 1 d . . . H76 H 0.1407 0.8764 0.4922 0.033 Uiso 1 calc R . . C81 C 0.0978(3) 0.81410(16) 0.2614(2) 0.0261(8) Uani 1 d . . . C82 C 0.0036(3) 0.80207(19) 0.2078(3) 0.0373(9) Uani 1 d . . . H82 H -0.0406 0.8348 0.1880 0.045 Uiso 1 calc R . . C83 C -0.0258(4) 0.7423(2) 0.1832(3) 0.0531(13) Uani 1 d . . . H83 H -0.0903 0.7346 0.1476 0.064 Uiso 1 calc R . . C84 C 0.0369(4) 0.6948(2) 0.2097(3) 0.0564(13) Uani 1 d . . . H84 H 0.0164 0.6542 0.1914 0.068 Uiso 1 calc R . . C85 C 0.1305(4) 0.7058(2) 0.2632(3) 0.0510(12) Uani 1 d . . . H85 H 0.1741 0.6727 0.2824 0.061 Uiso 1 calc R . . C86 C 0.1610(3) 0.76521(18) 0.2889(3) 0.0376(9) Uani 1 d . . . H86 H 0.2253 0.7725 0.3256 0.045 Uiso 1 calc R . . C91 C 0.1363(3) 0.69889(17) -0.1053(3) 0.0340(9) Uani 1 d . . . H91B H 0.2046 0.6920 -0.1037 0.041 Uiso 1 calc R . . H91A H 0.0999 0.7061 -0.1730 0.041 Uiso 1 calc R . . C92 C 0.0971(3) 0.64246(18) -0.0685(3) 0.0451(11) Uani 1 d . . . H92C H 0.0272 0.6464 -0.0797 0.068 Uiso 1 calc R . . H92B H 0.1273 0.6380 0.0006 0.068 Uiso 1 calc R . . H92A H 0.1115 0.6064 -0.1023 0.068 Uiso 1 calc R . . C101 C 0.0280(2) 0.77647(17) -0.0658(3) 0.0287(8) Uani 1 d . . . H10B H 0.0165 0.7894 -0.0041 0.034 Uiso 1 calc R . . H10A H -0.0171 0.7427 -0.0921 0.034 Uiso 1 calc R . . C102 C 0.0076(3) 0.82975(18) -0.1354(3) 0.0368(9) Uani 1 d . . . H10E H 0.0204 0.8175 -0.1960 0.055 Uiso 1 calc R . . H10D H 0.0494 0.8642 -0.1078 0.055 Uiso 1 calc R . . H10C H -0.0600 0.8420 -0.1472 0.055 Uiso 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 0.0207(3) 0.0238(3) 0.0225(2) 0.0007(2) 0.0060(2) 0.0028(2) Fe2 0.0185(2) 0.0211(3) 0.0209(2) 0.00142(19) 0.00499(19) -0.0003(2) Fe3 0.0193(2) 0.0207(3) 0.0216(2) 0.0009(2) 0.00472(19) 0.0010(2) Fe4 0.0189(2) 0.0258(3) 0.0205(2) -0.0012(2) 0.00313(19) 0.0004(2) P1 0.0188(4) 0.0249(5) 0.0209(4) 0.0014(4) 0.0046(3) -0.0001(4) P2 0.0198(4) 0.0228(5) 0.0217(4) 0.0004(4) 0.0052(3) -0.0002(4) O5 0.0298(14) 0.0391(16) 0.0246(13) -0.0003(11) -0.0001(11) 0.0107(12) O11 0.0231(14) 0.0444(17) 0.0480(17) 0.0052(13) 0.0045(13) 0.0079(13) O12 0.0499(18) 0.0303(16) 0.0514(18) 0.0119(14) 0.0174(14) 0.0022(14) O13 0.060(2) 0.0459(18) 0.0357(15) -0.0006(13) 0.0247(14) 0.0128(15) O21 0.0413(16) 0.0490(18) 0.0305(14) 0.0127(13) 0.0049(12) 0.0090(14) O22 0.0305(15) 0.0351(17) 0.073(2) 0.0044(15) 0.0146(15) -0.0090(13) O31 0.0536(19) 0.0244(16) 0.079(2) 0.0042(15) 0.0358(17) -0.0022(14) O32 0.0492(17) 0.0304(16) 0.0412(16) -0.0002(12) 0.0200(13) 0.0063(13) O33 0.0314(15) 0.0405(17) 0.0382(15) -0.0066(13) -0.0051(13) 0.0064(13) O41 0.0402(19) 0.082(3) 0.061(2) -0.0025(18) 0.0164(16) -0.0267(18) O42 0.0473(18) 0.0504(19) 0.0374(16) 0.0145(14) 0.0038(13) 0.0180(15) O43 0.0437(17) 0.0434(18) 0.0374(15) -0.0146(13) 0.0122(13) -0.0015(14) N1 0.0211(15) 0.0234(16) 0.0250(14) 0.0002(12) 0.0040(12) -0.0008(12) C1 0.0242(18) 0.0225(18) 0.0192(16) 0.0051(14) 0.0056(14) 0.0013(14) C2 0.0189(17) 0.0223(19) 0.0217(16) -0.0002(14) 0.0051(14) -0.0002(14) C3 0.0174(16) 0.0230(18) 0.0186(16) 0.0036(13) 0.0033(13) -0.0015(14) C4 0.0174(17) 0.0224(18) 0.0192(15) 0.0012(13) 0.0046(13) 0.0013(13) C5 0.0232(18) 0.0223(19) 0.0224(17) 0.0004(14) 0.0057(14) -0.0030(14) C11 0.031(2) 0.024(2) 0.0313(19) 0.0011(15) 0.0099(16) 0.0039(16) C12 0.0245(19) 0.032(2) 0.0299(19) 0.0013(17) 0.0063(16) 0.0057(16) C13 0.030(2) 0.027(2) 0.031(2) 0.0035(16) 0.0070(16) 0.0027(16) C21 0.0261(19) 0.028(2) 0.0279(19) 0.0008(16) 0.0092(15) 0.0010(16) C22 0.0217(18) 0.032(2) 0.035(2) 0.0035(17) 0.0066(16) 0.0027(17) C31 0.028(2) 0.034(2) 0.039(2) 0.0041(17) 0.0155(17) 0.0047(17) C32 0.0267(19) 0.0241(19) 0.0242(17) 0.0038(15) 0.0034(15) 0.0031(15) C33 0.028(2) 0.0216(19) 0.0296(19) 0.0012(15) 0.0061(16) 0.0061(15) C41 0.0242(19) 0.047(3) 0.0282(19) -0.0020(18) 0.0024(16) -0.0043(18) C42 0.0240(19) 0.039(2) 0.0259(18) -0.0055(17) 0.0070(15) 0.0020(17) C43 0.0220(18) 0.030(2) 0.0300(19) 0.0001(16) 0.0045(15) -0.0010(15) C51 0.0208(17) 0.031(2) 0.0216(17) 0.0017(15) 0.0054(14) 0.0036(15) C52 0.0258(19) 0.033(2) 0.0274(18) -0.0007(16) 0.0046(15) -0.0057(16) C53 0.035(2) 0.043(2) 0.035(2) 0.0091(18) 0.0114(17) -0.0073(19) C54 0.043(2) 0.052(3) 0.0225(19) 0.0078(18) 0.0067(17) -0.007(2) C55 0.033(2) 0.043(2) 0.0243(18) 0.0006(17) -0.0016(16) -0.0061(18) C56 0.0274(19) 0.028(2) 0.0294(19) 0.0037(15) 0.0078(15) -0.0005(16) C61 0.0215(18) 0.026(2) 0.0331(19) 0.0064(16) 0.0052(15) -0.0003(15) C62 0.027(2) 0.030(2) 0.042(2) -0.0018(18) 0.0044(17) 0.0001(17) C63 0.032(2) 0.046(3) 0.052(3) 0.004(2) -0.005(2) -0.008(2) C64 0.021(2) 0.072(4) 0.066(3) 0.015(3) 0.002(2) -0.003(2) C65 0.028(2) 0.069(3) 0.056(3) 0.020(2) 0.020(2) 0.006(2) C66 0.027(2) 0.052(3) 0.035(2) 0.0094(19) 0.0118(17) 0.0041(19) C71 0.0209(17) 0.0212(18) 0.0279(18) 0.0003(14) 0.0075(14) -0.0037(14) C72 0.0257(19) 0.030(2) 0.0254(18) -0.0018(15) 0.0040(15) -0.0013(16) C73 0.0223(19) 0.032(2) 0.046(2) -0.0005(18) 0.0108(17) 0.0039(16) C74 0.043(2) 0.034(2) 0.040(2) -0.0059(18) 0.0256(19) 0.0001(18) C75 0.036(2) 0.032(2) 0.0283(19) 0.0009(16) 0.0133(17) -0.0030(17) C76 0.028(2) 0.025(2) 0.0288(19) 0.0027(15) 0.0055(15) -0.0008(15) C81 0.034(2) 0.0255(19) 0.0231(17) -0.0019(15) 0.0143(15) -0.0059(16) C82 0.034(2) 0.040(2) 0.041(2) -0.0088(19) 0.0148(18) -0.0089(18) C83 0.055(3) 0.055(3) 0.056(3) -0.022(2) 0.026(2) -0.028(3) C84 0.084(4) 0.033(3) 0.062(3) -0.015(2) 0.037(3) -0.023(3) C85 0.076(4) 0.027(2) 0.056(3) 0.003(2) 0.028(3) 0.003(2) C86 0.044(2) 0.033(2) 0.038(2) 0.0022(18) 0.0139(19) 0.0007(19) C91 0.033(2) 0.033(2) 0.033(2) -0.0113(17) 0.0043(17) -0.0044(17) C92 0.041(2) 0.028(2) 0.060(3) -0.009(2) 0.003(2) -0.0010(19) C101 0.0212(18) 0.030(2) 0.0307(19) -0.0064(16) -0.0008(15) -0.0032(15) C102 0.034(2) 0.034(2) 0.035(2) -0.0004(17) -0.0038(17) 0.0007(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 Fe1 C12 1.810(4) . ? Fe1 C11 1.807(4) . ? Fe1 C13 1.843(4) . ? Fe1 C1 2.008(3) . ? Fe1 C5 2.032(3) . ? Fe1 P1 2.3155(10) . ? Fe2 C22 1.777(4) . ? Fe2 C21 1.799(4) . ? Fe2 C3 2.015(3) . ? Fe2 C4 2.034(3) . ? Fe2 C2 2.110(3) . ? Fe2 P1 2.2790(11) . ? Fe2 Fe3 2.8313(10) . ? Fe3 C33 1.786(4) . ? Fe3 C32 1.793(4) . ? Fe3 C31 1.812(4) . ? Fe3 C4 2.036(3) . ? Fe3 P2 2.2291(10) . ? Fe3 Fe4 2.5823(15) . ? Fe4 C42 1.780(4) . ? Fe4 C41 1.794(4) . ? Fe4 C43 1.802(4) . ? Fe4 C4 1.928(3) . ? Fe4 P2 2.2132(11) . ? P1 C51 1.836(3) . ? P1 C61 1.843(4) . ? P2 C71 1.827(3) . ? P2 C81 1.829(4) . ? O5 C5 1.201(4) . ? O11 C11 1.137(4) . ? O12 C12 1.128(4) . ? O13 C13 1.126(4) . ? O21 C21 1.140(4) . ? O22 C22 1.143(4) . ? O31 C31 1.136(4) . ? O32 C32 1.139(4) . ? O33 C33 1.148(4) . ? O41 C41 1.142(4) . ? O42 C42 1.146(4) . ? O43 C43 1.142(4) . ? N1 C1 1.324(4) . ? N1 C91 1.480(4) . ? N1 C101 1.495(4) . ? C1 C2 1.457(5) . ? C2 C3 1.434(4) . ? C3 C4 1.390(5) . ? C3 C5 1.518(5) . ? C51 C52 1.387(5) . ? C51 C56 1.389(5) . ? C52 C53 1.386(5) . ? C53 C54 1.375(5) . ? C54 C55 1.371(5) . ? C55 C56 1.400(5) . ? C61 C62 1.386(5) . ? C61 C66 1.404(5) . ? C62 C63 1.393(5) . ? C63 C64 1.382(6) . ? C64 C65 1.374(6) . ? C65 C66 1.379(5) . ? C71 C76 1.386(5) . ? C71 C72 1.392(5) . ? C72 C73 1.383(5) . ? C73 C74 1.385(5) . ? C74 C75 1.383(5) . ? C75 C76 1.386(5) . ? C81 C86 1.392(5) . ? C81 C82 1.395(5) . ? C82 C83 1.390(6) . ? C83 C84 1.364(7) . ? C84 C85 1.385(7) . ? C85 C86 1.390(6) . ? C91 C92 1.512(5) . ? C101 C102 1.516(5) . ? 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 C12 Fe1 C11 92.96(16) . . ? C12 Fe1 C13 100.89(16) . . ? C11 Fe1 C13 89.00(16) . . ? C12 Fe1 C1 88.54(15) . . ? C11 Fe1 C1 168.08(15) . . ? C13 Fe1 C1 102.34(15) . . ? C12 Fe1 C5 86.88(15) . . ? C11 Fe1 C5 85.85(15) . . ? C13 Fe1 C5 170.89(15) . . ? C1 Fe1 C5 82.42(14) . . ? C12 Fe1 P1 165.90(11) . . ? C11 Fe1 P1 93.21(12) . . ? C13 Fe1 P1 91.88(12) . . ? C1 Fe1 P1 82.87(10) . . ? C5 Fe1 P1 80.93(10) . . ? C22 Fe2 C21 94.09(17) . . ? C22 Fe2 C3 126.87(15) . . ? C21 Fe2 C3 139.01(15) . . ? C22 Fe2 C4 100.24(15) . . ? C21 Fe2 C4 142.61(14) . . ? C3 Fe2 C4 40.16(13) . . ? C22 Fe2 C2 166.18(15) . . ? C21 Fe2 C2 98.79(15) . . ? C3 Fe2 C2 40.61(13) . . ? C4 Fe2 C2 72.28(13) . . ? C22 Fe2 P1 88.82(12) . . ? C21 Fe2 P1 95.24(11) . . ? C3 Fe2 P1 87.65(10) . . ? C4 Fe2 P1 119.23(10) . . ? C2 Fe2 P1 85.05(10) . . ? C22 Fe2 Fe3 96.79(12) . . ? C21 Fe2 Fe3 98.36(11) . . ? C3 Fe2 Fe3 77.72(9) . . ? C4 Fe2 Fe3 45.96(9) . . ? C2 Fe2 Fe3 86.31(9) . . ? P1 Fe2 Fe3 164.86(3) . . ? C33 Fe3 C32 97.11(16) . . ? C33 Fe3 C31 103.95(16) . . ? C32 Fe3 C31 84.57(16) . . ? C33 Fe3 C4 111.85(14) . . ? C32 Fe3 C4 145.97(14) . . ? C31 Fe3 C4 104.42(15) . . ? C33 Fe3 P2 100.22(12) . . ? C32 Fe3 P2 88.15(11) . . ? C31 Fe3 P2 155.43(13) . . ? C4 Fe3 P2 69.96(9) . . ? C33 Fe3 Fe4 149.21(12) . . ? C32 Fe3 Fe4 98.56(11) . . ? C31 Fe3 Fe4 103.79(12) . . ? C4 Fe3 Fe4 47.55(9) . . ? P2 Fe3 Fe4 54.17(3) . . ? C33 Fe3 Fe2 85.96(11) . . ? C32 Fe3 Fe2 159.37(11) . . ? C31 Fe3 Fe2 74.92(12) . . ? C4 Fe3 Fe2 45.89(9) . . ? P2 Fe3 Fe2 111.46(3) . . ? Fe4 Fe3 Fe2 88.56(2) . . ? C42 Fe4 C41 100.42(17) . . ? C42 Fe4 C43 97.01(16) . . ? C41 Fe4 C43 91.31(17) . . ? C42 Fe4 C4 106.41(15) . . ? C41 Fe4 C4 92.58(15) . . ? C43 Fe4 C4 155.12(15) . . ? C42 Fe4 P2 98.13(12) . . ? C41 Fe4 P2 158.76(12) . . ? C43 Fe4 P2 96.64(12) . . ? C4 Fe4 P2 72.19(11) . . ? C42 Fe4 Fe3 146.93(12) . . ? C41 Fe4 Fe3 104.21(12) . . ? C43 Fe4 Fe3 104.07(12) . . ? C4 Fe4 Fe3 51.21(10) . . ? P2 Fe4 Fe3 54.75(4) . . ? C51 P1 C61 102.33(16) . . ? C51 P1 Fe2 108.22(12) . . ? C61 P1 Fe2 118.07(12) . . ? C51 P1 Fe1 116.64(12) . . ? C61 P1 Fe1 105.96(12) . . ? Fe2 P1 Fe1 106.14(4) . . ? C71 P2 C81 100.02(15) . . ? C71 P2 Fe4 120.88(11) . . ? C81 P2 Fe4 123.54(12) . . ? C71 P2 Fe3 120.22(12) . . ? C81 P2 Fe3 121.40(11) . . ? Fe4 P2 Fe3 71.08(5) . . ? C1 N1 C91 124.2(3) . . ? C1 N1 C101 123.4(3) . . ? C91 N1 C101 112.5(3) . . ? N1 C1 C2 117.8(3) . . ? N1 C1 Fe1 130.3(3) . . ? C2 C1 Fe1 111.7(2) . . ? C3 C2 C1 114.6(3) . . ? C3 C2 Fe2 66.12(18) . . ? C1 C2 Fe2 120.6(2) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C5 124.5(3) . . ? C2 C3 C5 114.1(3) . . ? C4 C3 Fe2 70.66(19) . . ? C2 C3 Fe2 73.27(18) . . ? C5 C3 Fe2 115.6(2) . . ? C3 C4 Fe4 140.6(2) . . ? C3 C4 Fe2 69.19(18) . . ? Fe4 C4 Fe2 145.50(18) . . ? C3 C4 Fe3 129.1(2) . . ? Fe4 C4 Fe3 81.24(13) . . ? Fe2 C4 Fe3 88.15(13) . . ? O5 C5 C3 122.5(3) . . ? O5 C5 Fe1 127.8(3) . . ? C3 C5 Fe1 109.6(2) . . ? O11 C11 Fe1 177.2(3) . . ? O12 C12 Fe1 176.6(3) . . ? O13 C13 Fe1 174.3(3) . . ? O21 C21 Fe2 176.6(3) . . ? O22 C22 Fe2 176.0(3) . . ? O31 C31 Fe3 170.4(3) . . ? O32 C32 Fe3 176.8(3) . . ? O33 C33 Fe3 176.2(3) . . ? O41 C41 Fe4 178.2(4) . . ? O42 C42 Fe4 174.8(3) . . ? O43 C43 Fe4 175.7(3) . . ? C52 C51 C56 119.0(3) . . ? C52 C51 P1 119.1(3) . . ? C56 C51 P1 121.7(3) . . ? C53 C52 C51 120.6(3) . . ? C54 C53 C52 119.9(4) . . ? C53 C54 C55 120.6(3) . . ? C54 C55 C56 119.7(3) . . ? C51 C56 C55 120.1(3) . . ? C62 C61 C66 118.8(3) . . ? C62 C61 P1 120.6(3) . . ? C66 C61 P1 119.8(3) . . ? C61 C62 C63 120.5(4) . . ? C64 C63 C62 119.9(4) . . ? C65 C64 C63 119.9(4) . . ? C64 C65 C66 120.9(4) . . ? C65 C66 C61 120.0(4) . . ? C76 C71 C72 118.8(3) . . ? C76 C71 P2 118.4(3) . . ? C72 C71 P2 122.7(3) . . ? C73 C72 C71 120.6(3) . . ? C72 C73 C74 119.8(3) . . ? C75 C74 C73 120.2(3) . . ? C74 C75 C76 119.7(3) . . ? C75 C76 C71 120.9(3) . . ? C86 C81 C82 118.6(4) . . ? C86 C81 P2 123.2(3) . . ? C82 C81 P2 118.2(3) . . ? C83 C82 C81 120.2(4) . . ? C84 C83 C82 120.8(5) . . ? C83 C84 C85 119.8(4) . . ? C84 C85 C86 120.2(4) . . ? C81 C86 C85 120.5(4) . . ? N1 C91 C92 112.1(3) . . ? N1 C101 C102 112.2(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.699 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.090 #===END