# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Stepnicka, Petr' _publ_contact_author_email stepnic@natur.cuni.cz _publ_section_title ; Synthesis, structural characterisation and bonding in an anionic hexavanadate bearing redox-active ferrocenyl groups at the periphery ; loop_ _publ_author_name J.Schulz R.Gyepes I.Cisarova P.Stepnicka # Attachment '- deposit.cif' data_js89 _database_code_depnum_ccdc_archive 'CCDC 779152' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H19 Fe N O4, 0.5 (C4 H8 O2)' _chemical_formula_sum 'C17 H23 Fe N O5' _chemical_formula_weight 377.21 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.2486(4) _cell_length_b 10.19960(10) _cell_length_c 11.81370(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.1641(9) _cell_angle_gamma 90.00 _cell_volume 3431.70(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4149 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type none _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 45736 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3930 _reflns_number_gt 3622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+5.0673P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap+geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3930 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.181994(7) 0.03986(2) 0.221824(18) 0.02026(8) Uani 1 1 d . . . N N 0.13833(4) 0.38804(12) 0.26135(10) 0.0172(2) Uani 1 1 d . . . H1N H 0.1322 0.3885 0.1806 0.021 Uiso 1 1 d R . . O1 O 0.18171(4) 0.31391(11) 0.43395(9) 0.0250(2) Uani 1 1 d . . . O2 O 0.14161(4) 0.51358(12) 0.51720(9) 0.0257(2) Uani 1 1 d . . . H2O H 0.1576 0.4411 0.5140 0.031 Uiso 1 1 d R . . O3 O 0.03735(4) 0.44343(13) 0.39594(9) 0.0278(3) Uani 1 1 d . . . H3O H 0.0489 0.4706 0.4673 0.033 Uiso 1 1 d R . . O4 O 0.05438(4) 0.46651(12) 0.11313(9) 0.0274(3) Uani 1 1 d . . . H4O H 0.0305 0.4529 0.1382 0.033 Uiso 1 1 d R . . C1 C 0.19988(5) 0.22905(14) 0.26443(12) 0.0189(3) Uani 1 1 d . . . C2 C 0.19535(6) 0.20821(15) 0.14195(13) 0.0236(3) Uani 1 1 d . . . H2 H 0.1747 0.2512 0.0820 0.028 Uiso 1 1 calc R . . C3 C 0.22840(6) 0.10946(16) 0.12944(15) 0.0289(3) Uani 1 1 d . . . H3 H 0.2331 0.0767 0.0595 0.035 Uiso 1 1 calc R . . C4 C 0.25289(6) 0.06971(17) 0.24244(16) 0.0296(3) Uani 1 1 d . . . H4 H 0.2763 0.0063 0.2589 0.036 Uiso 1 1 calc R . . C5 C 0.23563(5) 0.14298(16) 0.32557(14) 0.0250(3) Uani 1 1 d . . . H5 H 0.2458 0.1363 0.4059 0.030 Uiso 1 1 calc R . . C6 C 0.11564(6) 0.00618(19) 0.24360(18) 0.0348(4) Uani 1 1 d . . . H6 H 0.0948 0.0694 0.2581 0.042 Uiso 1 1 calc R . . C7 C 0.11974(7) -0.0382(2) 0.13283(18) 0.0448(5) Uani 1 1 d . . . H7 H 0.1020 -0.0095 0.0616 0.054 Uiso 1 1 calc R . . C8 C 0.15565(8) -0.1340(2) 0.1497(2) 0.0495(6) Uani 1 1 d . . . H8 H 0.1656 -0.1795 0.0915 0.059 Uiso 1 1 calc R . . C9 C 0.17363(8) -0.14849(18) 0.2703(2) 0.0459(5) Uani 1 1 d . . . H9 H 0.1977 -0.2048 0.3056 0.055 Uiso 1 1 calc R . . C10 C 0.14875(7) -0.06248(19) 0.32791(17) 0.0377(4) Uani 1 1 d . . . H10 H 0.1534 -0.0528 0.4080 0.045 Uiso 1 1 calc R . . C11 C 0.17232(5) 0.31338(13) 0.32582(12) 0.0173(3) Uani 1 1 d . . . C12 C 0.10474(5) 0.46667(14) 0.30875(12) 0.0171(3) Uani 1 1 d . . . C13 C 0.12910(5) 0.56470(15) 0.40285(13) 0.0233(3) Uani 1 1 d . . . H13A H 0.1573 0.5970 0.3820 0.028 Uiso 1 1 calc R . . H13B H 0.1084 0.6390 0.4025 0.028 Uiso 1 1 calc R . . C14 C 0.07203(5) 0.37269(15) 0.35401(12) 0.0207(3) Uani 1 1 d . . . H14A H 0.0568 0.3145 0.2918 0.025 Uiso 1 1 calc R . . H14B H 0.0903 0.3195 0.4162 0.025 Uiso 1 1 calc R . . C15 C 0.07660(5) 0.54802(16) 0.20784(13) 0.0238(3) Uani 1 1 d . . . H15A H 0.0529 0.5984 0.2345 0.029 Uiso 1 1 calc R . . H15B H 0.0974 0.6092 0.1817 0.029 Uiso 1 1 calc R . . O91 O 0.01434(14) 0.0097(4) 0.3373(3) 0.0644(9) Uiso 0.50 1 d P . . O92 O -0.00678(12) -0.1771(2) 0.2398(4) 0.0419(7) Uiso 0.50 1 d P . . C91 C 0.00597(17) -0.1047(5) 0.3352(5) 0.0378(11) Uiso 0.50 1 d P . . C92 C 0.0048(2) -0.1918(6) 0.4459(5) 0.0569(14) Uiso 0.50 1 d P . . H92A H -0.0029 -0.2798 0.4197 0.085 Uiso 0.50 1 d PR . . H92B H -0.0187 -0.1591 0.4835 0.085 Uiso 0.50 1 d PR . . H92C H 0.0348 -0.1910 0.4999 0.085 Uiso 0.50 1 d PR . . C93 C -0.01064(18) -0.1101(5) 0.1282(5) 0.0439(13) Uiso 0.50 1 d P . . H93B H -0.0342 -0.0417 0.1191 0.053 Uiso 0.50 1 d PR . . H93A H 0.0190 -0.0695 0.1253 0.053 Uiso 0.50 1 d PR . . C94 C -0.0225(2) -0.1968(6) 0.0396(5) 0.0618(15) Uiso 0.50 1 d P . . H94A H -0.0251 -0.1523 -0.0332 0.093 Uiso 0.50 1 d PR . . H94B H -0.0522 -0.2360 0.0417 0.093 Uiso 0.50 1 d PR . . H94C H 0.0011 -0.2637 0.0478 0.093 Uiso 0.50 1 d PR . . 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 0.02065(12) 0.01848(12) 0.02213(12) -0.00109(8) 0.00585(8) 0.00102(8) N 0.0162(5) 0.0226(6) 0.0137(5) -0.0002(4) 0.0050(4) 0.0021(4) O1 0.0277(5) 0.0311(6) 0.0156(5) 0.0018(4) 0.0037(4) 0.0074(4) O2 0.0256(5) 0.0340(6) 0.0172(5) -0.0066(4) 0.0043(4) 0.0017(5) O3 0.0147(5) 0.0527(7) 0.0166(5) -0.0065(5) 0.0048(4) 0.0003(5) O4 0.0153(5) 0.0520(8) 0.0151(5) 0.0042(5) 0.0038(4) -0.0005(5) C1 0.0179(6) 0.0183(7) 0.0211(7) -0.0005(5) 0.0056(5) -0.0001(5) C2 0.0289(8) 0.0218(7) 0.0227(7) 0.0025(6) 0.0114(6) 0.0028(6) C3 0.0310(8) 0.0270(8) 0.0340(8) -0.0046(7) 0.0185(7) -0.0001(7) C4 0.0191(7) 0.0275(8) 0.0428(9) -0.0044(7) 0.0082(6) 0.0041(6) C5 0.0187(7) 0.0258(8) 0.0285(8) -0.0020(6) 0.0011(6) 0.0025(6) C6 0.0243(8) 0.0316(9) 0.0519(11) -0.0032(8) 0.0158(8) -0.0042(7) C7 0.0355(10) 0.0586(13) 0.0373(10) -0.0047(9) 0.0019(8) -0.0207(9) C8 0.0542(12) 0.0367(10) 0.0669(14) -0.0286(10) 0.0330(11) -0.0213(9) C9 0.0447(11) 0.0218(8) 0.0759(15) 0.0093(9) 0.0236(10) 0.0014(8) C10 0.0419(10) 0.0367(9) 0.0383(10) 0.0057(8) 0.0170(8) -0.0084(8) C11 0.0169(6) 0.0171(6) 0.0183(6) 0.0005(5) 0.0048(5) -0.0019(5) C12 0.0151(6) 0.0214(7) 0.0153(6) -0.0002(5) 0.0047(5) 0.0020(5) C13 0.0238(7) 0.0246(7) 0.0220(7) -0.0033(6) 0.0065(6) -0.0017(6) C14 0.0171(6) 0.0299(8) 0.0162(6) -0.0016(6) 0.0056(5) -0.0026(6) C15 0.0214(7) 0.0312(8) 0.0195(7) 0.0042(6) 0.0059(6) 0.0069(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C1 2.0324(14) . ? Fe C9 2.0352(19) . ? Fe C2 2.0394(15) . ? Fe C10 2.0399(18) . ? Fe C8 2.0412(19) . ? Fe C6 2.0442(17) . ? Fe C7 2.0453(19) . ? Fe C5 2.0477(15) . ? Fe C3 2.0523(16) . ? Fe C4 2.0547(16) . ? N C11 1.3428(18) . ? N C12 1.4739(17) . ? N H1N 0.9292 . ? O1 C11 1.2439(17) . ? O2 C13 1.4162(19) . ? O2 H2O 0.8806 . ? O3 C14 1.4225(17) . ? O3 H3O 0.8786 . ? O4 C15 1.4262(19) . ? O4 H4O 0.8303 . ? C1 C5 1.429(2) . ? C1 C2 1.438(2) . ? C1 C11 1.4773(19) . ? C2 C3 1.427(2) . ? C2 H2 0.9300 . ? C3 C4 1.423(3) . ? C3 H3 0.9300 . ? C4 C5 1.416(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.408(3) . ? C6 C7 1.415(3) . ? C6 H6 0.9300 . ? C7 C8 1.415(3) . ? C7 H7 0.9300 . ? C8 C9 1.409(3) . ? C8 H8 0.9300 . ? C9 C10 1.410(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C15 1.5298(19) . ? C12 C14 1.5341(19) . ? C12 C13 1.543(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O91 C91 1.190(6) . ? O92 C91 1.329(6) . ? O92 C93 1.466(6) . ? C91 C92 1.587(8) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 C94 1.353(8) . ? C93 H93B 0.9700 . ? C93 H93A 0.9700 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? 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 C1 Fe C9 150.14(8) . . ? C1 Fe C2 41.37(6) . . ? C9 Fe C2 166.62(8) . . ? C1 Fe C10 117.74(7) . . ? C9 Fe C10 40.49(8) . . ? C2 Fe C10 152.06(7) . . ? C1 Fe C8 168.47(9) . . ? C9 Fe C8 40.44(10) . . ? C2 Fe C8 129.24(8) . . ? C10 Fe C8 67.93(8) . . ? C1 Fe C6 109.06(7) . . ? C9 Fe C6 68.13(8) . . ? C2 Fe C6 119.15(7) . . ? C10 Fe C6 40.32(8) . . ? C8 Fe C6 68.13(8) . . ? C1 Fe C7 130.22(8) . . ? C9 Fe C7 68.10(9) . . ? C2 Fe C7 109.39(8) . . ? C10 Fe C7 67.88(8) . . ? C8 Fe C7 40.53(9) . . ? C6 Fe C7 40.50(8) . . ? C1 Fe C5 41.00(6) . . ? C9 Fe C5 116.19(8) . . ? C2 Fe C5 69.09(6) . . ? C10 Fe C5 107.61(7) . . ? C8 Fe C5 149.42(9) . . ? C6 Fe C5 129.11(7) . . ? C7 Fe C5 168.12(8) . . ? C1 Fe C3 68.85(6) . . ? C9 Fe C3 127.77(8) . . ? C2 Fe C3 40.81(6) . . ? C10 Fe C3 165.76(8) . . ? C8 Fe C3 108.13(8) . . ? C6 Fe C3 152.49(8) . . ? C7 Fe C3 118.72(8) . . ? C5 Fe C3 68.37(7) . . ? C1 Fe C4 68.54(6) . . ? C9 Fe C4 106.81(8) . . ? C2 Fe C4 68.63(7) . . ? C10 Fe C4 127.76(8) . . ? C8 Fe C4 116.94(8) . . ? C6 Fe C4 166.28(8) . . ? C7 Fe C4 151.04(8) . . ? C5 Fe C4 40.37(6) . . ? C3 Fe C4 40.53(7) . . ? C11 N C12 124.36(11) . . ? C11 N H1N 122.0 . . ? C12 N H1N 113.4 . . ? C13 O2 H2O 107.0 . . ? C14 O3 H3O 110.2 . . ? C15 O4 H4O 95.0 . . ? C5 C1 C2 107.87(13) . . ? C5 C1 C11 121.86(13) . . ? C2 C1 C11 130.12(13) . . ? C5 C1 Fe 70.08(8) . . ? C2 C1 Fe 69.58(8) . . ? C11 C1 Fe 122.41(10) . . ? C3 C2 C1 107.41(13) . . ? C3 C2 Fe 70.08(9) . . ? C1 C2 Fe 69.05(8) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? Fe C2 H2 126.1 . . ? C4 C3 C2 108.19(14) . . ? C4 C3 Fe 69.82(9) . . ? C2 C3 Fe 69.11(9) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.7 . . ? C5 C4 C3 108.51(14) . . ? C5 C4 Fe 69.55(9) . . ? C3 C4 Fe 69.64(9) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.01(14) . . ? C4 C5 Fe 70.08(9) . . ? C1 C5 Fe 68.92(8) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.6 . . ? C10 C6 C7 107.79(18) . . ? C10 C6 Fe 69.68(10) . . ? C7 C6 Fe 69.79(10) . . ? C10 C6 H6 126.1 . . ? C7 C6 H6 126.1 . . ? Fe C6 H6 126.0 . . ? C6 C7 C8 107.88(19) . . ? C6 C7 Fe 69.71(10) . . ? C8 C7 Fe 69.58(11) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? Fe C7 H7 126.2 . . ? C9 C8 C7 107.99(18) . . ? C9 C8 Fe 69.55(11) . . ? C7 C8 Fe 69.89(11) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe C8 H8 126.1 . . ? C8 C9 C10 107.95(18) . . ? C8 C9 Fe 70.01(11) . . ? C10 C9 Fe 69.93(10) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe C9 H9 125.6 . . ? C6 C10 C9 108.38(18) . . ? C6 C10 Fe 70.01(10) . . ? C9 C10 Fe 69.57(11) . . ? C6 C10 H10 125.8 . . ? C9 C10 H10 125.8 . . ? Fe C10 H10 126.2 . . ? O1 C11 N 122.81(13) . . ? O1 C11 C1 119.28(13) . . ? N C11 C1 117.90(12) . . ? N C12 C15 106.61(11) . . ? N C12 C14 108.36(11) . . ? C15 C12 C14 110.05(12) . . ? N C12 C13 112.82(11) . . ? C15 C12 C13 106.75(12) . . ? C14 C12 C13 112.09(11) . . ? O2 C13 C12 115.16(12) . . ? O2 C13 H13A 108.5 . . ? C12 C13 H13A 108.5 . . ? O2 C13 H13B 108.5 . . ? C12 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? O3 C14 C12 110.81(12) . . ? O3 C14 H14A 109.5 . . ? C12 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O4 C15 C12 111.31(12) . . ? O4 C15 H15A 109.4 . . ? C12 C15 H15A 109.4 . . ? O4 C15 H15B 109.4 . . ? C12 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C91 O92 C93 116.9(3) . . ? O91 C91 O92 125.3(5) . . ? O91 C91 C92 125.1(5) . . ? O92 C91 C92 109.5(4) . . ? C91 C92 H92A 107.8 . . ? C91 C92 H92B 109.8 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 110.8 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C94 C93 O92 110.2(5) . . ? C94 C93 H93B 109.4 . . ? O92 C93 H93B 110.0 . . ? C94 C93 H93A 109.0 . . ? O92 C93 H93A 110.2 . . ? O92 C93 H93A 97.1 2 . ? H93B C93 H93A 108.0 . . ? C93 C94 H94A 109.8 . . ? C93 C94 H94B 109.1 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.575 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.054 #===END data_js112 _database_code_depnum_ccdc_archive 'CCDC 779153' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 Fe2 N2 O21 V6, 2(C16 H36 N), 2(C3 H7 N O)' _chemical_formula_sum 'C68 H118 Fe2 N6 O23 V6' _chemical_formula_weight 1805.02 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' V V 0.3005 0.5294 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6480(2) _cell_length_b 15.8602(2) _cell_length_c 20.3923(3) _cell_angle_alpha 84.8847(8) _cell_angle_beta 79.9909(7) _cell_angle_gamma 78.0411(8) _cell_volume 3935.00(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15973 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.37 _exptl_crystal_description fragment _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 105274 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 26.39 _reflns_number_total 16120 _reflns_number_gt 12513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+4.5460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom +difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16120 _refine_ls_number_parameters 963 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.40112(4) 0.48124(3) -0.07727(2) 0.02518(11) Uani 1 1 d . . . V2 V 0.37953(4) 0.46623(3) 0.08661(2) 0.02591(11) Uani 1 1 d . . . V3 V 0.60431(4) 0.36705(3) -0.00469(2) 0.02576(11) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.0000 0.0226(5) Uani 1 2 d S . . O2 O 0.31455(14) 0.44074(11) 0.01070(9) 0.0247(4) Uani 1 1 d . . . O3 O 0.49277(15) 0.36469(11) -0.06690(9) 0.0258(4) Uani 1 1 d . . . O4 O 0.50908(16) 0.51778(12) -0.13227(9) 0.0282(4) Uani 1 1 d . . . O5 O 0.33094(15) 0.59343(11) -0.05253(9) 0.0279(4) Uani 1 1 d . . . O6 O 0.32340(16) 0.45854(12) -0.12465(10) 0.0321(4) Uani 1 1 d . . . O7 O 0.48116(15) 0.34880(11) 0.06562(9) 0.0260(4) Uani 1 1 d . . . O8 O 0.29421(17) 0.42940(13) 0.14397(10) 0.0354(5) Uani 1 1 d . . . O9 O 0.32328(15) 0.57733(12) 0.07955(9) 0.0289(4) Uani 1 1 d . . . O10 O 0.66482(16) 0.26802(12) -0.01177(10) 0.0333(5) Uani 1 1 d . . . Fe1 Fe 0.15328(4) 0.04562(3) 0.06764(2) 0.03828(12) Uani 1 1 d . . . O11 O 0.22152(18) 0.23207(13) -0.07111(11) 0.0394(5) Uani 1 1 d . . . N1 N 0.3268(2) 0.20275(15) 0.01095(13) 0.0326(6) Uani 1 1 d . . . H1N H 0.3582 0.1634 0.0401 0.049(10) Uiso 1 1 d R . . C1 C 0.2379(3) 0.09347(18) -0.01653(15) 0.0335(7) Uani 1 1 d . . . C2 C 0.1429(3) 0.0697(2) -0.03162(16) 0.0391(7) Uani 1 1 d . . . H2 H 0.0864 0.1061 -0.0498 0.047 Uiso 1 1 calc R . . C3 C 0.1495(3) -0.0193(2) -0.01399(17) 0.0456(8) Uani 1 1 d . . . H3 H 0.0973 -0.0513 -0.0181 0.055 Uiso 1 1 calc R . . C4 C 0.2478(3) -0.0516(2) 0.01067(17) 0.0469(9) Uani 1 1 d . . . H4 H 0.2725 -0.1085 0.0249 0.056 Uiso 1 1 calc R . . C5 C 0.3030(3) 0.01776(19) 0.01002(16) 0.0397(7) Uani 1 1 d . . . H5 H 0.3697 0.0146 0.0243 0.048 Uiso 1 1 calc R . . C6 C 0.1060(3) 0.1427(2) 0.13206(16) 0.0436(8) Uani 1 1 d . . . H6 H 0.1168 0.1991 0.1228 0.052 Uiso 1 1 calc R . . C7 C 0.0134(3) 0.1116(2) 0.12187(17) 0.0480(8) Uani 1 1 d . . . H7 H -0.0473 0.1436 0.1050 0.058 Uiso 1 1 calc R . . C8 C 0.0303(4) 0.0228(3) 0.1421(2) 0.0638(12) Uani 1 1 d . . . H8 H -0.0174 -0.0142 0.1406 0.077 Uiso 1 1 calc R . . C9 C 0.1310(5) 0.0003(3) 0.16475(19) 0.0740(15) Uani 1 1 d . . . H9 H 0.1615 -0.0542 0.1812 0.089 Uiso 1 1 calc R . . C10 C 0.1788(4) 0.0745(2) 0.15837(18) 0.0574(10) Uani 1 1 d . . . H10 H 0.2461 0.0774 0.1696 0.069 Uiso 1 1 calc R . . C11 C 0.2611(2) 0.18236(18) -0.02816(15) 0.0316(6) Uani 1 1 d . . . C12 C 0.3683(2) 0.28349(17) 0.00583(14) 0.0290(6) Uani 1 1 d . . . C13 C 0.2739(2) 0.36266(17) 0.01242(15) 0.0287(6) Uani 1 1 d . . . H13A H 0.2324 0.3656 -0.0238 0.034 Uiso 1 1 calc R . . H13B H 0.2251 0.3566 0.0541 0.034 Uiso 1 1 calc R . . C14 C 0.4442(2) 0.29021(17) -0.06120(14) 0.0286(6) Uani 1 1 d . . . H14A H 0.5015 0.2389 -0.0654 0.034 Uiso 1 1 calc R . . H14B H 0.4025 0.2929 -0.0973 0.034 Uiso 1 1 calc R . . C15 C 0.4327(2) 0.27599(17) 0.06395(14) 0.0300(6) Uani 1 1 d . . . H15A H 0.3838 0.2698 0.1056 0.036 Uiso 1 1 calc R . . H15B H 0.4896 0.2245 0.0601 0.036 Uiso 1 1 calc R . . V21 V -0.11122(4) 0.62586(3) 0.52547(2) 0.02445(11) Uani 1 1 d . . . V22 V 0.08683(4) 0.55229(3) 0.40524(2) 0.02406(11) Uani 1 1 d . . . V23 V 0.12585(4) 0.51528(3) 0.56200(2) 0.02466(11) Uani 1 1 d . . . O21 O 0.0000 0.5000 0.5000 0.0218(5) Uani 1 2 d S . . O22 O -0.00850(14) 0.65912(11) 0.44253(9) 0.0242(4) Uani 1 1 d . . . O23 O 0.01589(14) 0.63030(11) 0.56966(9) 0.0243(4) Uani 1 1 d . . . O24 O -0.16524(15) 0.56099(12) 0.59366(9) 0.0274(4) Uani 1 1 d . . . O25 O -0.18767(15) 0.58919(12) 0.46586(10) 0.0282(4) Uani 1 1 d . . . O26 O -0.17819(15) 0.72185(12) 0.53951(10) 0.0321(5) Uani 1 1 d . . . O27 O 0.17991(14) 0.57035(11) 0.47453(9) 0.0238(4) Uani 1 1 d . . . O28 O 0.15426(16) 0.59808(12) 0.34270(9) 0.0315(4) Uani 1 1 d . . . O29 O -0.02245(16) 0.52638(12) 0.37213(9) 0.0277(4) Uani 1 1 d . . . O30 O 0.21052(16) 0.53898(12) 0.60410(10) 0.0323(4) Uani 1 1 d . . . Fe21 Fe 0.33613(4) 0.96691(3) 0.42896(2) 0.03615(11) Uani 1 1 d . . . O31 O 0.26631(17) 0.77746(13) 0.56553(11) 0.0379(5) Uani 1 1 d . . . N21 N 0.15345(19) 0.80808(15) 0.48709(12) 0.0302(5) Uani 1 1 d . . . H21N H 0.1318 0.8455 0.4512 0.033(8) Uiso 1 1 d R . . C21 C 0.2495(3) 0.91639(18) 0.51190(15) 0.0337(7) Uani 1 1 d . . . C22 C 0.1859(3) 0.99408(19) 0.48637(17) 0.0396(7) Uani 1 1 d . . . H22 H 0.1192 0.9992 0.4716 0.048 Uiso 1 1 calc R . . C23 C 0.2433(3) 1.0616(2) 0.48786(18) 0.0473(9) Uani 1 1 d . . . H23 H 0.2202 1.1192 0.4746 0.057 Uiso 1 1 calc R . . C24 C 0.3413(3) 1.0266(2) 0.51286(17) 0.0457(8) Uani 1 1 d . . . H24 H 0.3942 1.0571 0.5184 0.055 Uiso 1 1 calc R . . C25 C 0.3456(3) 0.9376(2) 0.52808(16) 0.0388(7) Uani 1 1 d . . . H25 H 0.4014 0.8995 0.5456 0.047 Uiso 1 1 calc R . . C26 C 0.3737(3) 0.8785(2) 0.35838(18) 0.0541(10) Uani 1 1 d . . . H26 H 0.3550 0.8243 0.3636 0.065 Uiso 1 1 calc R . . C27 C 0.3102(3) 0.9553(3) 0.33500(19) 0.0627(11) Uani 1 1 d . . . H27 H 0.2421 0.9611 0.3218 0.075 Uiso 1 1 calc R . . C28 C 0.3684(4) 1.0216(3) 0.3353(2) 0.0613(11) Uani 1 1 d . . . H28 H 0.3455 1.0792 0.3221 0.074 Uiso 1 1 calc R . . C29 C 0.4659(3) 0.9868(3) 0.35854(19) 0.0535(9) Uani 1 1 d . . . H29 H 0.5192 1.0171 0.3639 0.064 Uiso 1 1 calc R . . C30 C 0.4704(3) 0.8983(2) 0.37251(18) 0.0509(9) Uani 1 1 d . . . H30 H 0.5274 0.8594 0.3884 0.061 Uiso 1 1 calc R . . C31 C 0.2242(2) 0.82756(18) 0.52333(15) 0.0315(6) Uani 1 1 d . . . C32 C 0.1165(2) 0.72501(17) 0.49235(14) 0.0266(6) Uani 1 1 d . . . C33 C 0.0356(2) 0.73465(16) 0.44304(14) 0.0275(6) Uani 1 1 d . . . H33A H -0.0239 0.7830 0.4547 0.033 Uiso 1 1 calc R . . H33B H 0.0725 0.7475 0.3986 0.033 Uiso 1 1 calc R . . C34 C 0.0584(2) 0.70824(17) 0.56348(14) 0.0279(6) Uani 1 1 d . . . H34A H 0.1097 0.7040 0.5945 0.033 Uiso 1 1 calc R . . H34B H -0.0011 0.7565 0.5751 0.033 Uiso 1 1 calc R . . C35 C 0.2142(2) 0.65094(17) 0.47297(14) 0.0269(6) Uani 1 1 d . . . H35A H 0.2510 0.6638 0.4285 0.032 Uiso 1 1 calc R . . H35B H 0.2661 0.6466 0.5036 0.032 Uiso 1 1 calc R . . N40 N 0.0008(2) 0.37258(16) 0.82440(12) 0.0332(6) Uani 1 1 d . . . C41 C 0.0145(3) 0.3703(2) 0.89757(14) 0.0389(7) Uani 1 1 d . . . H41A H 0.0240 0.3107 0.9150 0.047 Uiso 1 1 calc R . . H41B H 0.0812 0.3904 0.8997 0.047 Uiso 1 1 calc R . . C42 C -0.0789(3) 0.4234(2) 0.94241(15) 0.0369(7) Uani 1 1 d . . . H42A H -0.1473 0.4073 0.9383 0.044 Uiso 1 1 calc R . . H42B H -0.0840 0.4841 0.9289 0.044 Uiso 1 1 calc R . . C43 C -0.0598(3) 0.4081(2) 1.01494(16) 0.0420(8) Uani 1 1 d . . . H43A H 0.0110 0.4209 1.0178 0.050 Uiso 1 1 calc R . . H43B H -0.1151 0.4480 1.0421 0.050 Uiso 1 1 calc R . . C44 C -0.0630(3) 0.3176(2) 1.04333(18) 0.0541(9) Uani 1 1 d . . . H44A H -0.1282 0.3012 1.0349 0.081 Uiso 1 1 calc R . . H44B H -0.0630 0.3152 1.0905 0.081 Uiso 1 1 calc R . . H44C H 0.0001 0.2787 1.0226 0.081 Uiso 1 1 calc R . . C45 C -0.1051(2) 0.34567(19) 0.81720(15) 0.0340(7) Uani 1 1 d . . . H45A H -0.1658 0.3894 0.8359 0.041 Uiso 1 1 calc R . . H45B H -0.1081 0.3456 0.7700 0.041 Uiso 1 1 calc R . . C46 C -0.1231(3) 0.2587(2) 0.84924(16) 0.0455(8) Uani 1 1 d . . . H46A H -0.1314 0.2599 0.8974 0.055 Uiso 1 1 calc R . . H46B H -0.0601 0.2144 0.8345 0.055 Uiso 1 1 calc R . . C47 C -0.2252(3) 0.2379(2) 0.82988(17) 0.0497(9) Uani 1 1 d . . . H47A H -0.2853 0.2865 0.8394 0.060 Uiso 1 1 calc R . . H47B H -0.2442 0.1885 0.8575 0.060 Uiso 1 1 calc R . . C48 C -0.2137(4) 0.2183(2) 0.75705(18) 0.0603(11) Uani 1 1 d . . . H48A H -0.2098 0.2702 0.7295 0.091 Uiso 1 1 calc R . . H48B H -0.2758 0.1960 0.7504 0.091 Uiso 1 1 calc R . . H48C H -0.1481 0.1762 0.7453 0.091 Uiso 1 1 calc R . . C49 C 0.1004(3) 0.3111(2) 0.79173(16) 0.0441(8) Uani 1 1 d . . . H49A H 0.1652 0.3309 0.7983 0.053 Uiso 1 1 calc R . . H49B H 0.1020 0.2548 0.8149 0.053 Uiso 1 1 calc R . . C50 C 0.1081(3) 0.3001(2) 0.71834(16) 0.0466(9) Uani 1 1 d . . . H50A H 0.1193 0.3533 0.6933 0.056 Uiso 1 1 calc R . . H50B H 0.0405 0.2869 0.7097 0.056 Uiso 1 1 calc R . . C51 C 0.2036(3) 0.2270(2) 0.69631(19) 0.0547(10) Uani 1 1 d . . . H51A H 0.2687 0.2374 0.7107 0.066 Uiso 1 1 calc R . . H51B H 0.1877 0.1733 0.7186 0.066 Uiso 1 1 calc R . . C52 C 0.2265(3) 0.2169(3) 0.6250(2) 0.0614(10) Uani 1 1 d . . . H52A H 0.1621 0.2078 0.6099 0.092 Uiso 1 1 calc R . . H52B H 0.2849 0.1682 0.6152 0.092 Uiso 1 1 calc R . . H52C H 0.2478 0.2681 0.6025 0.092 Uiso 1 1 calc R . . C53 C -0.0064(2) 0.46303(19) 0.79192(15) 0.0323(6) Uani 1 1 d . . . H53A H -0.0215 0.4616 0.7470 0.039 Uiso 1 1 calc R . . H53B H -0.0687 0.5003 0.8163 0.039 Uiso 1 1 calc R . . C54 C 0.0924(3) 0.5036(2) 0.78775(17) 0.0415(8) Uani 1 1 d . . . H54A H 0.1526 0.4734 0.7570 0.050 Uiso 1 1 calc R . . H54B H 0.1148 0.4992 0.8313 0.050 Uiso 1 1 calc R . . C55 C 0.0648(3) 0.5981(2) 0.76393(18) 0.0439(8) Uani 1 1 d . . . H55A H 0.0381 0.6019 0.7217 0.053 Uiso 1 1 calc R . . H55B H 0.0064 0.6281 0.7960 0.053 Uiso 1 1 calc R . . C56 C 0.1613(3) 0.6423(3) 0.7551(2) 0.0617(11) Uani 1 1 d . . . H56A H 0.1915 0.6352 0.7958 0.093 Uiso 1 1 calc R . . H56B H 0.1379 0.7027 0.7442 0.093 Uiso 1 1 calc R . . H56C H 0.2161 0.6172 0.7198 0.093 Uiso 1 1 calc R . . N60 N 0.46216(19) 0.38684(16) 0.31811(12) 0.0318(5) Uani 1 1 d . . . C61 C 0.4302(2) 0.3877(2) 0.39376(14) 0.0377(7) Uani 1 1 d . . . H61A H 0.3696 0.4356 0.4043 0.045 Uiso 1 1 calc R . . H61B H 0.4045 0.3349 0.4098 0.045 Uiso 1 1 calc R . . C62 C 0.5213(3) 0.3956(2) 0.43128(16) 0.0416(8) Uani 1 1 d . . . H62A H 0.5444 0.4502 0.4186 0.050 Uiso 1 1 calc R . . H62B H 0.5839 0.3494 0.4204 0.050 Uiso 1 1 calc R . . C63 C 0.4781(3) 0.3903(2) 0.50668(16) 0.0444(8) Uani 1 1 d . . . H63A H 0.5284 0.4093 0.5304 0.053 Uiso 1 1 calc R . . H63B H 0.4079 0.4294 0.5156 0.053 Uiso 1 1 calc R . . C64 C 0.4648(4) 0.3013(3) 0.53281(18) 0.0631(11) Uani 1 1 d . . . H64A H 0.4070 0.2855 0.5146 0.095 Uiso 1 1 calc R . . H64B H 0.4469 0.3000 0.5806 0.095 Uiso 1 1 calc R . . H64C H 0.5319 0.2612 0.5201 0.095 Uiso 1 1 calc R . . C65 C 0.3598(2) 0.3867(2) 0.28815(15) 0.0340(7) Uani 1 1 d . . . H65A H 0.3020 0.4327 0.3067 0.041 Uiso 1 1 calc R . . H65B H 0.3753 0.3996 0.2405 0.041 Uiso 1 1 calc R . . C66 C 0.3183(2) 0.3026(2) 0.29998(15) 0.0366(7) Uani 1 1 d . . . H66A H 0.3132 0.2842 0.3469 0.044 Uiso 1 1 calc R . . H66B H 0.3694 0.2582 0.2746 0.044 Uiso 1 1 calc R . . C67 C 0.2060(3) 0.3146(2) 0.27873(16) 0.0393(7) Uani 1 1 d . . . H67A H 0.1548 0.3580 0.3050 0.047 Uiso 1 1 calc R . . H67B H 0.2111 0.3352 0.2323 0.047 Uiso 1 1 calc R . . C68 C 0.1630(3) 0.2311(2) 0.28764(18) 0.0496(9) Uani 1 1 d . . . H68A H 0.2107 0.1893 0.2592 0.074 Uiso 1 1 calc R . . H68B H 0.0908 0.2418 0.2761 0.074 Uiso 1 1 calc R . . H68C H 0.1602 0.2095 0.3333 0.074 Uiso 1 1 calc R . . C69 C 0.5486(2) 0.3083(2) 0.30024(15) 0.0368(7) Uani 1 1 d . . . H69A H 0.5220 0.2578 0.3214 0.044 Uiso 1 1 calc R . . H69B H 0.6130 0.3119 0.3188 0.044 Uiso 1 1 calc R . . C70 C 0.5826(3) 0.2949(2) 0.22621(16) 0.0386(7) Uani 1 1 d . . . H70A H 0.6190 0.3407 0.2050 0.046 Uiso 1 1 calc R . . H70B H 0.5184 0.2965 0.2057 0.046 Uiso 1 1 calc R . . C71 C 0.6601(3) 0.2075(2) 0.21663(17) 0.0459(8) Uani 1 1 d . . . H71A H 0.7192 0.2037 0.2420 0.055 Uiso 1 1 calc R . . H71B H 0.6206 0.1618 0.2339 0.055 Uiso 1 1 calc R . . C72 C 0.7073(3) 0.1944(2) 0.14450(19) 0.0553(10) Uani 1 1 d . . . H72A H 0.6489 0.2008 0.1189 0.083 Uiso 1 1 calc R . . H72B H 0.7514 0.1375 0.1402 0.083 Uiso 1 1 calc R . . H72C H 0.7517 0.2364 0.1283 0.083 Uiso 1 1 calc R . . C73 C 0.5069(3) 0.4673(2) 0.29011(15) 0.0371(7) Uani 1 1 d . . . H73A H 0.5770 0.4636 0.3045 0.044 Uiso 1 1 calc R . . H73B H 0.5203 0.4667 0.2418 0.044 Uiso 1 1 calc R . . C74 C 0.4353(3) 0.5529(2) 0.30951(18) 0.0455(8) Uani 1 1 d . . . H74A H 0.4326 0.5594 0.3567 0.055 Uiso 1 1 calc R . . H74B H 0.3614 0.5542 0.3019 0.055 Uiso 1 1 calc R . . C75 C 0.4801(4) 0.6293(3) 0.2682(3) 0.0763(13) Uani 1 1 d . . . H75A H 0.4728 0.6259 0.2220 0.092 Uiso 1 1 calc R . . H75B H 0.4336 0.6828 0.2837 0.092 Uiso 1 1 calc R . . C76 C 0.5922(5) 0.6343(4) 0.2704(3) 0.0978(18) Uani 1 1 d . . . H76A H 0.6030 0.6320 0.3161 0.147 Uiso 1 1 calc R . . H76B H 0.6074 0.6876 0.2484 0.147 Uiso 1 1 calc R . . H76C H 0.6405 0.5867 0.2483 0.147 Uiso 1 1 calc R . . O80 O 0.4470(3) 1.07123(19) 0.10947(18) 0.0803(10) Uani 1 1 d . . . N80 N 0.5465(3) 0.9608(2) 0.16241(17) 0.0637(9) Uani 1 1 d . . . C81 C 0.5276(4) 1.0390(3) 0.1321(2) 0.0785(14) Uani 1 1 d . . . H81 H 0.5821 1.0713 0.1282 0.094 Uiso 1 1 calc R . . C82 C 0.6464(5) 0.9322(5) 0.1890(3) 0.122(3) Uani 1 1 d . . . H82A H 0.6910 0.9752 0.1784 0.183 Uiso 1 1 calc R . . H82B H 0.6852 0.8791 0.1699 0.183 Uiso 1 1 calc R . . H82C H 0.6301 0.9230 0.2366 0.183 Uiso 1 1 calc R . . C83 C 0.4693(5) 0.9076(3) 0.1698(3) 0.101(2) Uani 1 1 d . . . H83A H 0.4286 0.9105 0.2142 0.152 Uiso 1 1 calc R . . H83B H 0.5062 0.8492 0.1622 0.152 Uiso 1 1 calc R . . H83C H 0.4202 0.9267 0.1381 0.152 Uiso 1 1 calc R . . O90 O 1.0481(2) -0.06609(18) 0.38457(15) 0.0654(8) Uani 1 1 d . . . N90 N 0.9211(3) 0.0232(2) 0.33408(17) 0.0588(8) Uani 1 1 d . . . C91 C 0.9629(4) -0.0498(3) 0.3646(2) 0.0692(12) Uani 1 1 d . . . H91 H 0.9216 -0.0929 0.3710 0.083 Uiso 1 1 calc R . . C92 C 0.8161(4) 0.0342(4) 0.3117(3) 0.0930(17) Uani 1 1 d . . . H92A H 0.7873 -0.0176 0.3227 0.139 Uiso 1 1 calc R . . H92B H 0.8253 0.0460 0.2643 0.139 Uiso 1 1 calc R . . H92C H 0.7663 0.0816 0.3333 0.139 Uiso 1 1 calc R . . C93 C 0.9714(5) 0.0928(3) 0.3235(2) 0.0809(15) Uani 1 1 d . . . H93A H 1.0337 0.0819 0.3462 0.121 Uiso 1 1 calc R . . H93B H 0.9208 0.1431 0.3402 0.121 Uiso 1 1 calc R . . H93C H 0.9950 0.1024 0.2766 0.121 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0288(2) 0.0232(2) 0.0243(2) 0.00105(18) -0.00916(19) -0.00379(19) V2 0.0283(2) 0.0258(2) 0.0230(2) -0.00085(18) -0.00243(19) -0.00533(19) V3 0.0245(2) 0.0201(2) 0.0318(3) -0.00152(18) -0.00687(19) -0.00020(18) O1 0.0245(13) 0.0210(12) 0.0220(13) -0.0002(10) -0.0044(10) -0.0031(10) O2 0.0255(9) 0.0215(9) 0.0281(10) -0.0011(7) -0.0066(8) -0.0048(7) O3 0.0279(10) 0.0215(9) 0.0283(10) -0.0032(8) -0.0054(8) -0.0036(8) O4 0.0358(11) 0.0271(10) 0.0221(10) 0.0002(8) -0.0062(8) -0.0064(8) O5 0.0280(10) 0.0231(9) 0.0334(11) 0.0010(8) -0.0111(8) -0.0025(8) O6 0.0347(11) 0.0323(11) 0.0325(11) 0.0003(8) -0.0150(9) -0.0067(9) O7 0.0298(10) 0.0222(9) 0.0280(10) 0.0025(8) -0.0088(8) -0.0074(8) O8 0.0381(12) 0.0410(12) 0.0276(11) 0.0007(9) -0.0013(9) -0.0132(9) O9 0.0264(10) 0.0282(10) 0.0307(10) -0.0054(8) -0.0021(8) -0.0028(8) O10 0.0322(11) 0.0234(10) 0.0429(12) -0.0032(9) -0.0091(9) 0.0013(8) Fe1 0.0511(3) 0.0261(2) 0.0376(3) -0.00430(18) -0.0045(2) -0.0085(2) O11 0.0443(13) 0.0314(11) 0.0473(13) 0.0051(10) -0.0211(11) -0.0099(9) N1 0.0380(14) 0.0235(12) 0.0408(15) 0.0040(11) -0.0166(12) -0.0101(10) C1 0.0412(17) 0.0278(15) 0.0337(16) -0.0037(12) -0.0080(13) -0.0089(13) C2 0.0463(19) 0.0375(17) 0.0374(17) -0.0049(14) -0.0102(14) -0.0133(14) C3 0.057(2) 0.0396(18) 0.046(2) -0.0115(15) -0.0039(17) -0.0221(16) C4 0.066(2) 0.0247(15) 0.047(2) -0.0084(14) 0.0016(17) -0.0073(15) C5 0.0438(18) 0.0287(16) 0.0453(19) -0.0051(14) -0.0075(15) -0.0022(14) C6 0.055(2) 0.0329(17) 0.0419(19) -0.0104(14) -0.0037(16) -0.0052(15) C7 0.049(2) 0.049(2) 0.043(2) -0.0075(16) 0.0046(16) -0.0115(16) C8 0.089(3) 0.049(2) 0.051(2) -0.0078(18) 0.017(2) -0.030(2) C9 0.127(4) 0.039(2) 0.039(2) 0.0003(17) 0.004(2) 0.007(2) C10 0.069(3) 0.057(2) 0.043(2) -0.0161(18) -0.0180(19) 0.008(2) C11 0.0307(15) 0.0270(14) 0.0379(17) -0.0040(13) -0.0066(13) -0.0051(12) C12 0.0323(15) 0.0209(13) 0.0356(16) 0.0011(11) -0.0098(12) -0.0069(11) C13 0.0287(14) 0.0257(14) 0.0340(16) 0.0007(12) -0.0082(12) -0.0091(11) C14 0.0322(15) 0.0227(13) 0.0331(15) -0.0042(11) -0.0104(12) -0.0046(11) C15 0.0354(16) 0.0218(13) 0.0345(16) 0.0052(11) -0.0111(13) -0.0077(12) V21 0.0210(2) 0.0210(2) 0.0293(3) -0.00195(18) -0.00115(18) -0.00134(18) V22 0.0264(2) 0.0244(2) 0.0204(2) -0.00023(18) -0.00084(18) -0.00550(18) V23 0.0252(2) 0.0240(2) 0.0254(2) 0.00191(18) -0.00772(19) -0.00446(18) O21 0.0215(13) 0.0214(12) 0.0217(13) -0.0010(10) -0.0035(10) -0.0019(10) O22 0.0247(9) 0.0212(9) 0.0269(10) 0.0011(7) -0.0054(8) -0.0050(7) O23 0.0264(10) 0.0232(9) 0.0236(9) -0.0028(7) -0.0028(8) -0.0058(8) O24 0.0246(10) 0.0271(10) 0.0279(10) -0.0048(8) 0.0029(8) -0.0036(8) O25 0.0242(10) 0.0248(9) 0.0353(11) 0.0023(8) -0.0094(8) -0.0020(8) O26 0.0282(10) 0.0243(10) 0.0395(12) -0.0036(8) -0.0013(9) 0.0018(8) O27 0.0223(9) 0.0216(9) 0.0268(10) -0.0007(7) -0.0029(7) -0.0042(7) O28 0.0345(11) 0.0335(11) 0.0260(10) 0.0021(8) -0.0001(8) -0.0106(9) O29 0.0342(11) 0.0288(10) 0.0212(9) 0.0029(8) -0.0059(8) -0.0093(8) O30 0.0327(11) 0.0329(11) 0.0339(11) 0.0006(9) -0.0123(9) -0.0077(9) Fe21 0.0381(2) 0.0298(2) 0.0417(3) -0.00267(19) -0.0062(2) -0.00915(19) O31 0.0383(12) 0.0349(11) 0.0434(13) 0.0005(10) -0.0125(10) -0.0100(9) N21 0.0309(13) 0.0248(12) 0.0363(14) 0.0011(10) -0.0069(11) -0.0086(10) C21 0.0384(17) 0.0280(15) 0.0360(17) -0.0068(12) -0.0017(13) -0.0104(13) C22 0.0358(17) 0.0315(16) 0.050(2) -0.0082(14) -0.0013(14) -0.0048(13) C23 0.056(2) 0.0252(16) 0.059(2) -0.0118(15) -0.0001(17) -0.0076(15) C24 0.053(2) 0.0388(18) 0.051(2) -0.0126(15) -0.0060(17) -0.0195(16) C25 0.0431(18) 0.0366(17) 0.0410(18) -0.0068(14) -0.0086(14) -0.0140(14) C26 0.070(3) 0.052(2) 0.043(2) -0.0161(17) 0.0055(18) -0.023(2) C27 0.049(2) 0.099(3) 0.042(2) -0.009(2) -0.0123(17) -0.013(2) C28 0.072(3) 0.049(2) 0.054(2) 0.0125(18) -0.002(2) -0.004(2) C29 0.053(2) 0.059(2) 0.051(2) -0.0014(18) -0.0002(18) -0.0258(19) C30 0.046(2) 0.055(2) 0.042(2) 0.0003(16) 0.0030(16) 0.0005(17) C31 0.0286(15) 0.0279(15) 0.0371(17) -0.0042(13) -0.0020(13) -0.0048(12) C32 0.0270(14) 0.0206(13) 0.0322(15) -0.0008(11) -0.0047(12) -0.0050(11) C33 0.0296(14) 0.0201(13) 0.0322(15) 0.0044(11) -0.0069(12) -0.0040(11) C34 0.0294(14) 0.0237(13) 0.0312(15) -0.0053(11) -0.0042(12) -0.0054(11) C35 0.0257(14) 0.0256(14) 0.0286(15) 0.0000(11) -0.0017(11) -0.0062(11) N40 0.0321(13) 0.0376(14) 0.0256(13) 0.0013(10) -0.0068(10) 0.0035(11) C41 0.0345(17) 0.0507(19) 0.0284(16) 0.0039(14) -0.0099(13) 0.0005(14) C42 0.0356(16) 0.0423(17) 0.0324(16) -0.0033(13) -0.0121(13) -0.0004(14) C43 0.0387(18) 0.053(2) 0.0347(17) -0.0040(15) -0.0101(14) -0.0051(15) C44 0.053(2) 0.063(2) 0.041(2) 0.0082(17) -0.0094(17) -0.0006(18) C45 0.0344(16) 0.0341(16) 0.0313(16) -0.0015(12) -0.0047(13) -0.0021(13) C46 0.061(2) 0.0367(17) 0.0332(17) 0.0031(14) -0.0052(16) -0.0022(16) C47 0.072(3) 0.0372(18) 0.0401(19) -0.0028(15) -0.0001(17) -0.0184(17) C48 0.092(3) 0.050(2) 0.045(2) 0.0008(17) -0.009(2) -0.031(2) C49 0.0382(18) 0.0461(19) 0.0367(18) 0.0041(14) -0.0030(14) 0.0125(15) C50 0.0458(19) 0.0466(19) 0.0361(18) 0.0004(15) -0.0034(15) 0.0129(16) C51 0.048(2) 0.051(2) 0.058(2) -0.0154(18) -0.0069(18) 0.0100(17) C52 0.052(2) 0.062(2) 0.065(3) -0.006(2) -0.0056(19) -0.0001(19) C53 0.0283(15) 0.0372(16) 0.0289(15) 0.0012(12) -0.0079(12) 0.0010(12) C54 0.0302(16) 0.052(2) 0.0427(19) -0.0008(15) -0.0100(14) -0.0060(14) C55 0.0369(18) 0.050(2) 0.048(2) -0.0053(16) -0.0097(15) -0.0114(15) C56 0.054(2) 0.070(3) 0.069(3) -0.008(2) -0.011(2) -0.027(2) N60 0.0251(12) 0.0434(14) 0.0264(13) -0.0036(11) -0.0035(10) -0.0051(11) C61 0.0314(16) 0.054(2) 0.0278(16) -0.0017(14) -0.0056(12) -0.0073(14) C62 0.0372(17) 0.0504(19) 0.0389(18) -0.0048(15) -0.0133(14) -0.0052(15) C63 0.0408(18) 0.059(2) 0.0345(17) -0.0091(15) -0.0162(14) -0.0004(16) C64 0.078(3) 0.069(3) 0.0334(19) 0.0046(18) -0.0039(19) 0.000(2) C65 0.0268(15) 0.0467(18) 0.0289(15) -0.0019(13) -0.0072(12) -0.0060(13) C66 0.0326(16) 0.0452(18) 0.0322(16) -0.0015(13) -0.0053(13) -0.0076(14) C67 0.0359(17) 0.0505(19) 0.0360(17) -0.0021(14) -0.0097(14) -0.0156(15) C68 0.049(2) 0.052(2) 0.051(2) -0.0022(17) -0.0107(17) -0.0147(17) C69 0.0310(16) 0.0406(17) 0.0373(17) -0.0033(14) -0.0074(13) -0.0011(13) C70 0.0325(16) 0.0443(18) 0.0381(18) -0.0046(14) -0.0041(13) -0.0057(14) C71 0.0426(19) 0.0433(19) 0.051(2) -0.0071(16) -0.0087(16) -0.0029(15) C72 0.046(2) 0.056(2) 0.058(2) -0.0075(18) 0.0016(18) -0.0024(17) C73 0.0337(16) 0.0456(18) 0.0323(16) -0.0020(14) -0.0039(13) -0.0099(14) C74 0.0418(19) 0.047(2) 0.047(2) -0.0046(16) -0.0087(15) -0.0063(15) C75 0.071(3) 0.051(2) 0.105(4) -0.022(2) -0.002(3) -0.009(2) C76 0.100(4) 0.094(4) 0.102(4) -0.033(3) 0.016(3) -0.040(3) O80 0.087(2) 0.0546(17) 0.109(3) 0.0221(17) -0.051(2) -0.0173(16) N80 0.071(2) 0.064(2) 0.050(2) 0.0067(16) -0.0123(17) -0.0002(18) C81 0.091(4) 0.070(3) 0.083(3) 0.013(3) -0.039(3) -0.022(3) C82 0.105(5) 0.169(6) 0.068(3) -0.012(4) -0.032(3) 0.043(4) C83 0.162(6) 0.055(3) 0.078(4) -0.003(2) 0.009(4) -0.029(3) O90 0.0557(17) 0.0575(17) 0.088(2) 0.0089(15) -0.0271(16) -0.0146(13) N90 0.065(2) 0.0504(19) 0.060(2) 0.0051(16) -0.0116(17) -0.0107(16) C91 0.070(3) 0.064(3) 0.076(3) 0.009(2) -0.026(2) -0.012(2) C92 0.080(3) 0.111(4) 0.091(4) 0.020(3) -0.038(3) -0.016(3) C93 0.118(4) 0.046(2) 0.071(3) -0.002(2) 0.001(3) -0.012(3) _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 V1 O6 1.6027(19) . ? V1 O4 1.7714(19) . ? V1 O5 1.8863(18) . ? V1 O3 1.9832(18) . ? V1 O2 2.0574(19) . ? V1 O1 2.2490(5) . ? V1 V2 3.0287(7) 2_665 ? V1 V3 3.0324(7) 2_665 ? V2 O8 1.605(2) . ? V2 O9 1.7613(19) . ? V2 O4 1.8874(19) 2_665 ? V2 O2 1.9816(18) . ? V2 O7 2.0648(18) . ? V2 O1 2.2275(5) . ? V2 V3 3.0236(6) 2_665 ? V2 V1 3.0287(7) 2_665 ? V3 O10 1.6054(18) . ? V3 O5 1.7607(19) 2_665 ? V3 O9 1.886(2) 2_665 ? V3 O7 1.9754(19) . ? V3 O3 2.0625(19) . ? V3 O1 2.2440(4) . ? V3 V2 3.0235(6) 2_665 ? V3 V1 3.0324(7) 2_665 ? O1 V2 2.2275(5) 2_665 ? O1 V3 2.2440(4) 2_665 ? O1 V1 2.2490(5) 2_665 ? O2 C13 1.431(3) . ? O3 C14 1.427(3) . ? O4 V2 1.8874(19) 2_665 ? O5 V3 1.7607(19) 2_665 ? O7 C15 1.421(3) . ? O9 V3 1.886(2) 2_665 ? Fe1 C1 2.033(3) . ? Fe1 C5 2.033(3) . ? Fe1 C9 2.038(4) . ? Fe1 C10 2.039(4) . ? Fe1 C6 2.040(3) . ? Fe1 C8 2.043(4) . ? Fe1 C3 2.047(3) . ? Fe1 C2 2.048(3) . ? Fe1 C7 2.051(3) . ? Fe1 C4 2.057(3) . ? O11 C11 1.227(3) . ? N1 C11 1.349(4) . ? N1 C12 1.471(3) . ? N1 H1N 0.9022 . ? C1 C2 1.421(4) . ? C1 C5 1.429(4) . ? C1 C11 1.489(4) . ? C2 C3 1.414(4) . ? C2 H2 0.9300 . ? C3 C4 1.403(5) . ? C3 H3 0.9300 . ? C4 C5 1.418(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.400(5) . ? C6 C7 1.414(5) . ? C6 H6 0.9300 . ? C7 C8 1.416(5) . ? C7 H7 0.9300 . ? C8 C9 1.396(7) . ? C8 H8 0.9300 . ? C9 C10 1.417(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C15 1.533(4) . ? C12 C14 1.536(4) . ? C12 C13 1.541(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? V21 O26 1.6050(18) . ? V21 O24 1.7791(19) . ? V21 O25 1.8758(19) . ? V21 O23 1.9909(18) . ? V21 O22 2.0464(18) . ? V21 O21 2.2362(4) . ? V21 V22 3.0256(6) 2_566 ? V21 V23 3.0374(7) 2_566 ? V22 O28 1.6107(19) . ? V22 O29 1.7732(19) . ? V22 O24 1.8638(18) 2_566 ? V22 O22 1.9918(18) . ? V22 O27 2.0627(18) . ? V22 O21 2.2321(4) . ? V22 V21 3.0256(6) 2_566 ? V22 V23 3.0452(6) 2_566 ? V23 O30 1.6028(19) . ? V23 O25 1.7767(19) 2_566 ? V23 O29 1.8816(19) 2_566 ? V23 O27 1.9895(18) . ? V23 O23 2.0518(18) . ? V23 O21 2.2595(5) . ? V23 V21 3.0374(7) 2_566 ? V23 V22 3.0452(6) 2_566 ? O21 V22 2.2321(4) 2_566 ? O21 V21 2.2362(4) 2_566 ? O21 V23 2.2595(5) 2_566 ? O22 C33 1.424(3) . ? O23 C34 1.434(3) . ? O24 V22 1.8639(18) 2_566 ? O25 V23 1.7767(19) 2_566 ? O27 C35 1.429(3) . ? O29 V23 1.8816(19) 2_566 ? Fe21 C26 2.027(3) . ? Fe21 C27 2.029(4) . ? Fe21 C22 2.036(3) . ? Fe21 C28 2.037(4) . ? Fe21 C29 2.042(4) . ? Fe21 C30 2.042(3) . ? Fe21 C23 2.044(3) . ? Fe21 C24 2.045(3) . ? Fe21 C21 2.045(3) . ? Fe21 C25 2.052(3) . ? O31 C31 1.232(3) . ? N21 C31 1.352(4) . ? N21 C32 1.476(3) . ? N21 H21N 0.9420 . ? C21 C25 1.424(4) . ? C21 C22 1.434(4) . ? C21 C31 1.498(4) . ? C22 C23 1.418(5) . ? C22 H22 0.9300 . ? C23 C24 1.410(5) . ? C23 H23 0.9300 . ? C24 C25 1.409(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C30 1.405(5) . ? C26 C27 1.407(6) . ? C26 H26 0.9300 . ? C27 C28 1.404(6) . ? C27 H27 0.9300 . ? C28 C29 1.388(6) . ? C28 H28 0.9300 . ? C29 C30 1.398(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C32 C33 1.532(4) . ? C32 C34 1.535(4) . ? C32 C35 1.541(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? N40 C49 1.515(4) . ? N40 C53 1.517(4) . ? N40 C45 1.522(4) . ? N40 C41 1.528(4) . ? C41 C42 1.513(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.530(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.505(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.516(4) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.520(5) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.521(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.506(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.526(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.450(5) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.507(4) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.521(5) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.508(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? N60 C69 1.503(4) . ? N60 C65 1.525(4) . ? N60 C61 1.526(4) . ? N60 C73 1.527(4) . ? C61 C62 1.520(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.541(4) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.496(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.517(4) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.526(4) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.517(5) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.517(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.530(4) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.504(5) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.511(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.561(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.445(7) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? O80 C81 1.192(5) . ? N80 C81 1.329(5) . ? N80 C83 1.398(6) . ? N80 C82 1.434(6) . ? C81 H81 0.9300 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? O90 C91 1.188(5) . ? N90 C91 1.319(5) . ? N90 C93 1.368(5) . ? N90 C92 1.449(6) . ? C91 H91 0.9300 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? 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 O6 V1 O4 105.08(10) . . ? O6 V1 O5 102.58(9) . . ? O4 V1 O5 93.59(9) . . ? O6 V1 O3 98.44(9) . . ? O4 V1 O3 91.46(8) . . ? O5 V1 O3 156.27(8) . . ? O6 V1 O2 95.88(9) . . ? O4 V1 O2 158.75(8) . . ? O5 V1 O2 85.10(8) . . ? O3 V1 O2 81.88(7) . . ? O6 V1 O1 171.89(8) . . ? O4 V1 O1 82.37(6) . . ? O5 V1 O1 79.81(6) . . ? O3 V1 O1 77.90(5) . . ? O2 V1 O1 76.51(5) . . ? O6 V1 V2 140.01(8) . 2_665 ? O4 V1 V2 35.38(6) . 2_665 ? O5 V1 V2 89.27(6) . 2_665 ? O3 V1 V2 81.54(6) . 2_665 ? O2 V1 V2 123.37(5) . 2_665 ? O1 V1 V2 47.125(12) . 2_665 ? O6 V1 V3 134.95(7) . 2_665 ? O4 V1 V3 86.22(6) . 2_665 ? O5 V1 V3 32.45(6) . 2_665 ? O3 V1 V3 125.19(6) . 2_665 ? O2 V1 V3 81.33(5) . 2_665 ? O1 V1 V3 47.481(12) . 2_665 ? V2 V1 V3 65.847(15) 2_665 2_665 ? O8 V2 O9 103.60(10) . . ? O8 V2 O4 103.69(9) . 2_665 ? O9 V2 O4 93.80(9) . 2_665 ? O8 V2 O2 96.06(9) . . ? O9 V2 O2 92.81(8) . . ? O4 V2 O2 157.03(8) 2_665 . ? O8 V2 O7 96.39(9) . . ? O9 V2 O7 159.81(8) . . ? O4 V2 O7 84.06(8) 2_665 . ? O2 V2 O7 82.18(7) . . ? O8 V2 O1 171.87(8) . . ? O9 V2 O1 82.87(6) . . ? O4 V2 O1 80.51(6) 2_665 . ? O2 V2 O1 78.52(5) . . ? O7 V2 O1 76.98(5) . . ? O8 V2 V3 138.22(8) . 2_665 ? O9 V2 V3 35.34(6) . 2_665 ? O4 V2 V3 90.09(6) 2_665 2_665 ? O2 V2 V3 82.71(5) . 2_665 ? O7 V2 V3 124.48(5) . 2_665 ? O1 V2 V3 47.684(12) . 2_665 ? O8 V2 V1 136.56(8) . 2_665 ? O9 V2 V1 86.51(6) . 2_665 ? O4 V2 V1 32.92(6) 2_665 2_665 ? O2 V2 V1 125.96(6) . 2_665 ? O7 V2 V1 80.82(5) . 2_665 ? O1 V2 V1 47.724(12) . 2_665 ? V3 V2 V1 66.430(15) 2_665 2_665 ? O10 V3 O5 104.97(9) . 2_665 ? O10 V3 O9 102.32(9) . 2_665 ? O5 V3 O9 94.05(9) 2_665 2_665 ? O10 V3 O7 98.17(9) . . ? O5 V3 O7 91.61(8) 2_665 . ? O9 V3 O7 156.51(8) 2_665 . ? O10 V3 O3 95.89(9) . . ? O5 V3 O3 158.99(8) 2_665 . ? O9 V3 O3 83.73(8) 2_665 . ? O7 V3 O3 82.86(7) . . ? O10 V3 O1 171.88(8) . . ? O5 V3 O1 82.58(6) 2_665 . ? O9 V3 O1 79.78(6) 2_665 . ? O7 V3 O1 78.38(5) . . ? O3 V3 O1 76.46(5) . . ? O10 V3 V2 134.96(8) . 2_665 ? O5 V3 V2 86.38(6) 2_665 2_665 ? O9 V3 V2 32.70(6) 2_665 2_665 ? O7 V3 V2 125.41(5) . 2_665 ? O3 V3 V2 80.51(5) . 2_665 ? O1 V3 V2 47.225(12) . 2_665 ? O10 V3 V1 139.65(8) . 2_665 ? O5 V3 V1 35.09(6) 2_665 2_665 ? O9 V3 V1 89.59(6) 2_665 2_665 ? O7 V3 V1 82.05(5) . 2_665 ? O3 V3 V1 123.90(5) . 2_665 ? O1 V3 V1 47.622(12) . 2_665 ? V2 V3 V1 65.959(15) 2_665 2_665 ? V2 O1 V2 180.000(18) . 2_665 ? V2 O1 V3 94.908(17) . . ? V2 O1 V3 85.092(17) 2_665 . ? V2 O1 V3 85.092(17) . 2_665 ? V2 O1 V3 94.908(17) 2_665 2_665 ? V3 O1 V3 180.00(2) . 2_665 ? V2 O1 V1 85.151(17) . 2_665 ? V2 O1 V1 94.849(17) 2_665 2_665 ? V3 O1 V1 84.897(17) . 2_665 ? V3 O1 V1 95.103(17) 2_665 2_665 ? V2 O1 V1 94.849(17) . . ? V2 O1 V1 85.151(17) 2_665 . ? V3 O1 V1 95.103(17) . . ? V3 O1 V1 84.897(17) 2_665 . ? V1 O1 V1 180.0 2_665 . ? C13 O2 V2 120.18(16) . . ? C13 O2 V1 118.46(16) . . ? V2 O2 V1 109.39(8) . . ? C14 O3 V1 119.81(16) . . ? C14 O3 V3 117.37(15) . . ? V1 O3 V3 110.05(8) . . ? V1 O4 V2 111.70(10) . 2_665 ? V3 O5 V1 112.46(9) 2_665 . ? C15 O7 V3 118.98(17) . . ? C15 O7 V2 118.37(16) . . ? V3 O7 V2 109.23(8) . . ? V2 O9 V3 111.95(10) . 2_665 ? C1 Fe1 C5 41.15(12) . . ? C1 Fe1 C9 154.95(19) . . ? C5 Fe1 C9 120.34(18) . . ? C1 Fe1 C10 119.28(16) . . ? C5 Fe1 C10 106.73(16) . . ? C9 Fe1 C10 40.67(18) . . ? C1 Fe1 C6 106.87(13) . . ? C5 Fe1 C6 124.62(14) . . ? C9 Fe1 C6 67.64(15) . . ? C10 Fe1 C6 40.15(14) . . ? C1 Fe1 C8 162.80(17) . . ? C5 Fe1 C8 155.34(16) . . ? C9 Fe1 C8 40.00(19) . . ? C10 Fe1 C8 68.04(18) . . ? C6 Fe1 C8 67.87(15) . . ? C1 Fe1 C3 68.31(13) . . ? C5 Fe1 C3 68.04(14) . . ? C9 Fe1 C3 126.58(16) . . ? C10 Fe1 C3 162.86(15) . . ? C6 Fe1 C3 156.21(15) . . ? C8 Fe1 C3 109.47(16) . . ? C1 Fe1 C2 40.75(12) . . ? C5 Fe1 C2 68.55(13) . . ? C9 Fe1 C2 163.27(18) . . ? C10 Fe1 C2 154.70(15) . . ? C6 Fe1 C2 120.74(13) . . ? C8 Fe1 C2 126.55(17) . . ? C3 Fe1 C2 40.42(13) . . ? C1 Fe1 C7 125.05(13) . . ? C5 Fe1 C7 162.03(13) . . ? C9 Fe1 C7 67.64(17) . . ? C10 Fe1 C7 67.97(16) . . ? C6 Fe1 C7 40.44(14) . . ? C8 Fe1 C7 40.47(15) . . ? C3 Fe1 C7 121.97(15) . . ? C2 Fe1 C7 108.44(14) . . ? C1 Fe1 C4 68.47(13) . . ? C5 Fe1 C4 40.55(13) . . ? C9 Fe1 C4 108.76(15) . . ? C10 Fe1 C4 125.62(15) . . ? C6 Fe1 C4 161.98(15) . . ? C8 Fe1 C4 121.58(15) . . ? C3 Fe1 C4 40.00(14) . . ? C2 Fe1 C4 67.87(14) . . ? C7 Fe1 C4 156.33(15) . . ? C11 N1 C12 126.1(2) . . ? C11 N1 H1N 121.5 . . ? C12 N1 H1N 111.8 . . ? C2 C1 C5 107.5(3) . . ? C2 C1 C11 124.0(3) . . ? C5 C1 C11 128.5(3) . . ? C2 C1 Fe1 70.18(18) . . ? C5 C1 Fe1 69.43(18) . . ? C11 C1 Fe1 126.1(2) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 Fe1 69.74(19) . . ? C1 C2 Fe1 69.07(18) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe1 C2 H2 126.6 . . ? C4 C3 C2 108.8(3) . . ? C4 C3 Fe1 70.39(19) . . ? C2 C3 Fe1 69.84(18) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 125.8 . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Fe1 69.62(19) . . ? C5 C4 Fe1 68.84(18) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 127.1 . . ? C4 C5 C1 107.9(3) . . ? C4 C5 Fe1 70.61(19) . . ? C1 C5 Fe1 69.42(18) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe1 C5 H5 125.5 . . ? C10 C6 C7 108.7(3) . . ? C10 C6 Fe1 69.90(19) . . ? C7 C6 Fe1 70.23(19) . . ? C10 C6 H6 125.7 . . ? C7 C6 H6 125.7 . . ? Fe1 C6 H6 125.8 . . ? C6 C7 C8 107.3(4) . . ? C6 C7 Fe1 69.33(19) . . ? C8 C7 Fe1 69.4(2) . . ? C6 C7 H7 126.4 . . ? C8 C7 H7 126.4 . . ? Fe1 C7 H7 126.4 . . ? C9 C8 C7 108.1(4) . . ? C9 C8 Fe1 69.8(2) . . ? C7 C8 Fe1 70.1(2) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? Fe1 C8 H8 125.7 . . ? C8 C9 C10 108.6(4) . . ? C8 C9 Fe1 70.2(2) . . ? C10 C9 Fe1 69.7(2) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 126.0 . . ? C6 C10 C9 107.4(4) . . ? C6 C10 Fe1 69.9(2) . . ? C9 C10 Fe1 69.6(2) . . ? C6 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Fe1 C10 H10 125.7 . . ? O11 C11 N1 123.9(3) . . ? O11 C11 C1 120.4(3) . . ? N1 C11 C1 115.7(3) . . ? N1 C12 C15 105.0(2) . . ? N1 C12 C14 109.4(2) . . ? C15 C12 C14 110.6(2) . . ? N1 C12 C13 111.3(2) . . ? C15 C12 C13 110.2(2) . . ? C14 C12 C13 110.2(2) . . ? O2 C13 C12 111.1(2) . . ? O2 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? O2 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? O3 C14 C12 111.7(2) . . ? O3 C14 H14A 109.3 . . ? C12 C14 H14A 109.3 . . ? O3 C14 H14B 109.3 . . ? C12 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? O7 C15 C12 112.5(2) . . ? O7 C15 H15A 109.1 . . ? C12 C15 H15A 109.1 . . ? O7 C15 H15B 109.1 . . ? C12 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? O26 V21 O24 104.21(9) . . ? O26 V21 O25 102.79(9) . . ? O24 V21 O25 93.31(9) . . ? O26 V21 O23 97.74(9) . . ? O24 V21 O23 91.01(8) . . ? O25 V21 O23 157.26(8) . . ? O26 V21 O22 96.42(9) . . ? O24 V21 O22 158.98(8) . . ? O25 V21 O22 85.95(8) . . ? O23 V21 O22 82.12(7) . . ? O26 V21 O21 172.70(8) . . ? O24 V21 O21 81.98(6) . . ? O25 V21 O21 80.45(6) . . ? O23 V21 O21 78.07(5) . . ? O22 V21 O21 77.18(5) . . ? O26 V21 V22 138.52(7) . 2_566 ? O24 V21 V22 34.75(6) . 2_566 ? O25 V21 V22 89.12(6) . 2_566 ? O23 V21 V22 81.80(5) . 2_566 ? O22 V21 V22 124.26(5) . 2_566 ? O21 V21 V22 47.324(12) . 2_566 ? O26 V21 V23 135.44(8) . 2_566 ? O24 V21 V23 86.19(6) . 2_566 ? O25 V21 V23 32.71(5) . 2_566 ? O23 V21 V23 125.71(5) . 2_566 ? O22 V21 V23 81.88(5) . 2_566 ? O21 V21 V23 47.821(12) . 2_566 ? V22 V21 V23 65.991(15) 2_566 2_566 ? O28 V22 O29 103.93(9) . . ? O28 V22 O24 102.83(9) . 2_566 ? O29 V22 O24 94.02(9) . 2_566 ? O28 V22 O22 97.40(9) . . ? O29 V22 O22 91.57(8) . . ? O24 V22 O22 157.01(8) 2_566 . ? O28 V22 O27 96.13(9) . . ? O29 V22 O27 159.58(8) . . ? O24 V22 O27 85.11(8) 2_566 . ? O22 V22 O27 81.96(7) . . ? O28 V22 O21 172.65(8) . . ? O29 V22 O21 82.32(6) . . ? O24 V22 O21 80.31(6) 2_566 . ? O22 V22 O21 78.38(5) . . ? O27 V22 O21 77.41(5) . . ? O28 V22 V21 135.74(7) . 2_566 ? O29 V22 V21 86.73(6) . 2_566 ? O24 V22 V21 32.96(6) 2_566 2_566 ? O22 V22 V21 125.55(5) . 2_566 ? O27 V22 V21 81.48(5) . 2_566 ? O21 V22 V21 47.438(12) . 2_566 ? O28 V22 V23 138.23(7) . 2_566 ? O29 V22 V23 34.72(6) . 2_566 ? O24 V22 V23 89.50(6) 2_566 2_566 ? O22 V22 V23 82.50(5) . 2_566 ? O27 V22 V23 124.89(5) . 2_566 ? O21 V22 V23 47.693(12) . 2_566 ? V21 V22 V23 66.181(15) 2_566 2_566 ? O30 V23 O25 104.54(9) . 2_566 ? O30 V23 O29 103.32(9) . 2_566 ? O25 V23 O29 93.47(9) 2_566 2_566 ? O30 V23 O27 98.05(9) . . ? O25 V23 O27 91.34(8) 2_566 . ? O29 V23 O27 156.12(8) 2_566 . ? O30 V23 O23 97.10(9) . . ? O25 V23 O23 158.12(8) 2_566 . ? O29 V23 O23 84.53(8) 2_566 . ? O27 V23 O23 82.37(7) . . ? O30 V23 O21 172.77(7) . . ? O25 V23 O21 81.88(6) 2_566 . ? O29 V23 O21 79.31(6) 2_566 . ? O27 V23 O21 78.24(5) . . ? O23 V23 O21 76.33(5) . . ? O30 V23 V21 138.97(7) . 2_566 ? O25 V23 V21 34.79(6) 2_566 2_566 ? O29 V23 V21 88.43(6) 2_566 2_566 ? O27 V23 V21 82.27(5) . 2_566 ? O23 V23 V21 123.34(5) . 2_566 ? O21 V23 V21 47.174(12) . 2_566 ? O30 V23 V22 135.71(8) . 2_566 ? O25 V23 V22 86.24(6) 2_566 2_566 ? O29 V23 V22 32.46(6) 2_566 2_566 ? O27 V23 V22 124.94(6) . 2_566 ? O23 V23 V22 80.40(5) . 2_566 ? O21 V23 V22 46.937(12) . 2_566 ? V21 V23 V22 65.446(15) 2_566 2_566 ? V22 O21 V22 180.00(2) . 2_566 ? V22 O21 V21 94.762(16) . . ? V22 O21 V21 85.238(16) 2_566 . ? V22 O21 V21 85.238(16) . 2_566 ? V22 O21 V21 94.762(16) 2_566 2_566 ? V21 O21 V21 180.00(2) . 2_566 ? V22 O21 V23 94.630(17) . . ? V22 O21 V23 85.370(17) 2_566 . ? V21 O21 V23 94.995(17) . . ? V21 O21 V23 85.005(17) 2_566 . ? V22 O21 V23 85.370(17) . 2_566 ? V22 O21 V23 94.630(17) 2_566 2_566 ? V21 O21 V23 85.005(17) . 2_566 ? V21 O21 V23 94.995(17) 2_566 2_566 ? V23 O21 V23 180.000(1) . 2_566 ? C33 O22 V22 119.96(16) . . ? C33 O22 V21 118.27(16) . . ? V22 O22 V21 109.02(8) . . ? C34 O23 V21 119.47(16) . . ? C34 O23 V23 117.88(15) . . ? V21 O23 V23 110.13(8) . . ? V21 O24 V22 112.29(9) . 2_566 ? V23 O25 V21 112.50(9) 2_566 . ? C35 O27 V23 119.17(16) . . ? C35 O27 V22 119.02(15) . . ? V23 O27 V22 109.12(8) . . ? V22 O29 V23 112.82(9) . 2_566 ? C26 Fe21 C27 40.60(16) . . ? C26 Fe21 C22 122.67(15) . . ? C27 Fe21 C22 106.63(15) . . ? C26 Fe21 C28 67.77(16) . . ? C27 Fe21 C28 40.39(17) . . ? C22 Fe21 C28 122.25(15) . . ? C26 Fe21 C29 67.72(15) . . ? C27 Fe21 C29 67.66(16) . . ? C22 Fe21 C29 158.07(14) . . ? C28 Fe21 C29 39.78(16) . . ? C26 Fe21 C30 40.41(15) . . ? C27 Fe21 C30 67.86(16) . . ? C22 Fe21 C30 159.55(14) . . ? C28 Fe21 C30 67.19(15) . . ? C29 Fe21 C30 40.02(15) . . ? C26 Fe21 C23 158.44(16) . . ? C27 Fe21 C23 122.08(17) . . ? C22 Fe21 C23 40.67(13) . . ? C28 Fe21 C23 107.37(16) . . ? C29 Fe21 C23 122.92(15) . . ? C30 Fe21 C23 159.07(16) . . ? C26 Fe21 C24 160.00(16) . . ? C27 Fe21 C24 158.06(17) . . ? C22 Fe21 C24 68.39(14) . . ? C28 Fe21 C24 122.83(16) . . ? C29 Fe21 C24 108.53(15) . . ? C30 Fe21 C24 124.11(15) . . ? C23 Fe21 C24 40.35(14) . . ? C26 Fe21 C21 108.09(14) . . ? C27 Fe21 C21 122.99(16) . . ? C22 Fe21 C21 41.15(12) . . ? C28 Fe21 C21 158.95(16) . . ? C29 Fe21 C21 159.75(14) . . ? C30 Fe21 C21 123.99(13) . . ? C23 Fe21 C21 68.44(13) . . ? C24 Fe21 C21 68.21(13) . . ? C26 Fe21 C25 124.21(15) . . ? C27 Fe21 C25 159.84(16) . . ? C22 Fe21 C25 68.67(13) . . ? C28 Fe21 C25 158.72(16) . . ? C29 Fe21 C25 123.95(15) . . ? C30 Fe21 C25 109.31(14) . . ? C23 Fe21 C25 67.95(14) . . ? C24 Fe21 C25 40.24(13) . . ? C21 Fe21 C25 40.69(12) . . ? C31 N21 C32 125.1(2) . . ? C31 N21 H21N 120.2 . . ? C32 N21 H21N 114.1 . . ? C25 C21 C22 107.5(3) . . ? C25 C21 C31 123.2(3) . . ? C22 C21 C31 129.3(3) . . ? C25 C21 Fe21 69.91(18) . . ? C22 C21 Fe21 69.09(18) . . ? C31 C21 Fe21 127.8(2) . . ? C23 C22 C21 107.5(3) . . ? C23 C22 Fe21 69.96(19) . . ? C21 C22 Fe21 69.77(17) . . ? C23 C22 H22 126.3 . . ? C21 C22 H22 126.3 . . ? Fe21 C22 H22 125.6 . . ? C24 C23 C22 108.4(3) . . ? C24 C23 Fe21 69.86(19) . . ? C22 C23 Fe21 69.37(18) . . ? C24 C23 H23 125.8 . . ? C22 C23 H23 125.8 . . ? Fe21 C23 H23 126.5 . . ? C25 C24 C23 108.5(3) . . ? C25 C24 Fe21 70.14(18) . . ? C23 C24 Fe21 69.8(2) . . ? C25 C24 H24 125.7 . . ? C23 C24 H24 125.7 . . ? Fe21 C24 H24 125.9 . . ? C24 C25 C21 108.1(3) . . ? C24 C25 Fe21 69.62(19) . . ? C21 C25 Fe21 69.40(18) . . ? C24 C25 H25 126.0 . . ? C21 C25 H25 126.0 . . ? Fe21 C25 H25 126.6 . . ? C30 C26 C27 107.8(3) . . ? C30 C26 Fe21 70.4(2) . . ? C27 C26 Fe21 69.8(2) . . ? C30 C26 H26 126.1 . . ? C27 C26 H26 126.1 . . ? Fe21 C26 H26 125.3 . . ? C28 C27 C26 107.4(4) . . ? C28 C27 Fe21 70.1(2) . . ? C26 C27 Fe21 69.6(2) . . ? C28 C27 H27 126.3 . . ? C26 C27 H27 126.3 . . ? Fe21 C27 H27 125.6 . . ? C29 C28 C27 108.6(4) . . ? C29 C28 Fe21 70.3(2) . . ? C27 C28 Fe21 69.5(2) . . ? C29 C28 H28 125.7 . . ? C27 C28 H28 125.7 . . ? Fe21 C28 H28 126.0 . . ? C28 C29 C30 108.3(4) . . ? C28 C29 Fe21 69.9(2) . . ? C30 C29 Fe21 70.0(2) . . ? C28 C29 H29 125.9 . . ? C30 C29 H29 125.9 . . ? Fe21 C29 H29 125.8 . . ? C29 C30 C26 108.0(3) . . ? C29 C30 Fe21 70.0(2) . . ? C26 C30 Fe21 69.2(2) . . ? C29 C30 H30 126.0 . . ? C26 C30 H30 126.0 . . ? Fe21 C30 H30 126.4 . . ? O31 C31 N21 123.8(3) . . ? O31 C31 C21 119.1(3) . . ? N21 C31 C21 117.1(3) . . ? N21 C32 C33 105.8(2) . . ? N21 C32 C34 109.9(2) . . ? C33 C32 C34 109.9(2) . . ? N21 C32 C35 110.4(2) . . ? C33 C32 C35 109.9(2) . . ? C34 C32 C35 110.7(2) . . ? O22 C33 C32 112.7(2) . . ? O22 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? O22 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? O23 C34 C32 111.6(2) . . ? O23 C34 H34A 109.3 . . ? C32 C34 H34A 109.3 . . ? O23 C34 H34B 109.3 . . ? C32 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? O27 C35 C32 111.6(2) . . ? O27 C35 H35A 109.3 . . ? C32 C35 H35A 109.3 . . ? O27 C35 H35B 109.3 . . ? C32 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C49 N40 C53 111.5(2) . . ? C49 N40 C45 111.7(2) . . ? C53 N40 C45 105.5(2) . . ? C49 N40 C41 105.2(2) . . ? C53 N40 C41 111.7(2) . . ? C45 N40 C41 111.4(2) . . ? C42 C41 N40 115.6(2) . . ? C42 C41 H41A 108.4 . . ? N40 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? N40 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 110.0(2) . . ? C41 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? C41 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 114.0(3) . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N40 117.0(2) . . ? C46 C45 H45A 108.1 . . ? N40 C45 H45A 108.1 . . ? C46 C45 H45B 108.1 . . ? N40 C45 H45B 108.1 . . ? H45A C45 H45B 107.3 . . ? C45 C46 C47 109.6(3) . . ? C45 C46 H46A 109.8 . . ? C47 C46 H46A 109.8 . . ? C45 C46 H46B 109.8 . . ? C47 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C46 C47 C48 114.3(3) . . ? C46 C47 H47A 108.7 . . ? C48 C47 H47A 108.7 . . ? C46 C47 H47B 108.7 . . ? C48 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N40 116.8(2) . . ? C50 C49 H49A 108.1 . . ? N40 C49 H49A 108.1 . . ? C50 C49 H49B 108.1 . . ? N40 C49 H49B 108.1 . . ? H49A C49 H49B 107.3 . . ? C49 C50 C51 109.5(3) . . ? C49 C50 H50A 109.8 . . ? C51 C50 H50A 109.8 . . ? C49 C50 H50B 109.8 . . ? C51 C50 H50B 109.8 . . ? H50A C50 H50B 108.2 . . ? C52 C51 C50 114.2(3) . . ? C52 C51 H51A 108.7 . . ? C50 C51 H51A 108.7 . . ? C52 C51 H51B 108.7 . . ? C50 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N40 116.9(2) . . ? C54 C53 H53A 108.1 . . ? N40 C53 H53A 108.1 . . ? C54 C53 H53B 108.1 . . ? N40 C53 H53B 108.1 . . ? H53A C53 H53B 107.3 . . ? C53 C54 C55 109.7(2) . . ? C53 C54 H54A 109.7 . . ? C55 C54 H54A 109.7 . . ? C53 C54 H54B 109.7 . . ? C55 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C56 C55 C54 112.9(3) . . ? C56 C55 H55A 109.0 . . ? C54 C55 H55A 109.0 . . ? C56 C55 H55B 109.0 . . ? C54 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C69 N60 C65 111.0(2) . . ? C69 N60 C61 109.5(2) . . ? C65 N60 C61 108.3(2) . . ? C69 N60 C73 108.9(2) . . ? C65 N60 C73 108.3(2) . . ? C61 N60 C73 110.9(2) . . ? C62 C61 N60 115.1(2) . . ? C62 C61 H61A 108.5 . . ? N60 C61 H61A 108.5 . . ? C62 C61 H61B 108.5 . . ? N60 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? C61 C62 C63 108.6(3) . . ? C61 C62 H62A 110.0 . . ? C63 C62 H62A 110.0 . . ? C61 C62 H62B 110.0 . . ? C63 C62 H62B 110.0 . . ? H62A C62 H62B 108.3 . . ? C64 C63 C62 113.0(3) . . ? C64 C63 H63A 109.0 . . ? C62 C63 H63A 109.0 . . ? C64 C63 H63B 109.0 . . ? C62 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N60 114.7(2) . . ? C66 C65 H65A 108.6 . . ? N60 C65 H65A 108.6 . . ? C66 C65 H65B 108.6 . . ? N60 C65 H65B 108.6 . . ? H65A C65 H65B 107.6 . . ? C65 C66 C67 110.1(3) . . ? C65 C66 H66A 109.6 . . ? C67 C66 H66A 109.6 . . ? C65 C66 H66B 109.6 . . ? C67 C66 H66B 109.6 . . ? H66A C66 H66B 108.2 . . ? C68 C67 C66 111.8(3) . . ? C68 C67 H67A 109.2 . . ? C66 C67 H67A 109.2 . . ? C68 C67 H67B 109.2 . . ? C66 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N60 C69 C70 115.6(2) . . ? N60 C69 H69A 108.4 . . ? C70 C69 H69A 108.4 . . ? N60 C69 H69B 108.4 . . ? C70 C69 H69B 108.4 . . ? H69A C69 H69B 107.4 . . ? C69 C70 C71 109.2(3) . . ? C69 C70 H70A 109.8 . . ? C71 C70 H70A 109.8 . . ? C69 C70 H70B 109.8 . . ? C71 C70 H70B 109.8 . . ? H70A C70 H70B 108.3 . . ? C72 C71 C70 112.0(3) . . ? C72 C71 H71A 109.2 . . ? C70 C71 H71A 109.2 . . ? C72 C71 H71B 109.2 . . ? C70 C71 H71B 109.2 . . ? H71A C71 H71B 107.9 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 N60 116.2(3) . . ? C74 C73 H73A 108.2 . . ? N60 C73 H73A 108.2 . . ? C74 C73 H73B 108.2 . . ? N60 C73 H73B 108.2 . . ? H73A C73 H73B 107.4 . . ? C73 C74 C75 111.0(3) . . ? C73 C74 H74A 109.4 . . ? C75 C74 H74A 109.4 . . ? C73 C74 H74B 109.4 . . ? C75 C74 H74B 109.4 . . ? H74A C74 H74B 108.0 . . ? C76 C75 C74 117.0(4) . . ? C76 C75 H75A 108.0 . . ? C74 C75 H75A 108.0 . . ? C76 C75 H75B 108.0 . . ? C74 C75 H75B 108.0 . . ? H75A C75 H75B 107.3 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C81 N80 C83 120.9(4) . . ? C81 N80 C82 119.1(5) . . ? C83 N80 C82 120.0(5) . . ? O80 C81 N80 125.8(5) . . ? O80 C81 H81 117.1 . . ? N80 C81 H81 117.1 . . ? N80 C82 H82A 109.5 . . ? N80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N80 C83 H83A 109.5 . . ? N80 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N80 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C91 N90 C93 122.7(4) . . ? C91 N90 C92 120.8(4) . . ? C93 N90 C92 116.4(4) . . ? O90 C91 N90 126.6(5) . . ? O90 C91 H91 116.7 . . ? N90 C91 H91 116.7 . . ? N90 C92 H92A 109.5 . . ? N90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N90 C93 H93A 109.5 . . ? N90 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N90 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.815 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.073 #===END