data_x0299 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H20 F8 Fe N5 O' _chemical_formula_sum 'C44 H20 F8 Fe N5 O' _chemical_formula_weight 842.50 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' 'F' 'F' 0.0171 0.0103 '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' 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 12.0504(5) _cell_length_b 12.6148(4) _cell_length_c 12.2383(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.912(5) _cell_angle_gamma 90.00 _cell_volume 1737.84(12) _cell_formula_units_Z 2 _exptl_crystal_description prism _exptl_crystal_colour "dark red" _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_special_details ; two reference frames collected approx. every 50 frames ; _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number ? _diffrn_standards_interval_count 2 _diffrn_standards_interval_time '50' _diffrn_standards_decay_% ? _diffrn_reflns_number 14909 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_resolution_max 0.75 _reflns_number_total 4283 _reflns_number_gt 3015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _computing_structure_solution 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_structure_refinement 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_molecular_graphics 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_publication_material 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The NO group is disordered with the oxygen atoms in two positions. The oxygen atoms, while flagged for being isolated in the checkcif file, are bound to N3 and all bond/angle data are included in this CIF file. sof values for the disordered atoms were refined and then held constant for anisotropic refinement cycles. ; _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^)+(0.0645P)^2^+2.0722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4283 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.41948(17) 0.36133(15) 0.71928(17) 0.0532(5) Uani 1 1 d . . . F2 F 0.81798(16) 0.26722(19) 0.90994(17) 0.0579(6) Uani 1 1 d . . . F3 F 0.45368(17) -0.2647(2) 0.6187(2) 0.0865(9) Uani 1 1 d . . . F4 F 0.13363(15) -0.04497(14) 0.59284(16) 0.0494(5) Uani 1 1 d . . . O1 O 0.2395(7) 0.0483(7) 0.9062(8) 0.0502(19) Uani 0.30 1 d P A 1 O1' O 0.2482(10) 0.0223(11) 0.9784(14) 0.053(3) Uani 0.20 1 d P A 2 N1 N 0.58601(17) 0.13442(16) 1.05862(18) 0.0267(4) Uani 1 1 d . . . N2 N 0.47931(17) 0.04302(17) 0.83738(18) 0.0272(4) Uani 1 1 d . . . N3 N 0.3372(4) 0.0553(4) 0.9717(4) 0.0343(10) Uani 0.50 1 d P . . C1 C 0.6379(2) 0.1659(2) 1.1739(2) 0.0291(5) Uani 1 1 d . . . C2 C 0.6930(2) 0.2682(2) 1.1805(2) 0.0340(6) Uani 1 1 d . . . H2A H 0.7344 0.3068 1.2497 0.041 Uiso 1 1 calc R . . C3 C 0.6747(2) 0.2985(2) 1.0707(2) 0.0344(6) Uani 1 1 d . A . H3A H 0.6994 0.3635 1.0474 0.041 Uiso 1 1 calc R . . C4 C 0.6109(2) 0.2148(2) 0.9945(2) 0.0296(5) Uani 1 1 d . A . C5 C 0.5814(2) 0.2158(2) 0.8739(2) 0.0304(5) Uani 1 1 d . . . C6 C 0.5206(2) 0.1333(2) 0.8007(2) 0.0289(5) Uani 1 1 d . . . C7 C 0.4906(2) 0.1325(2) 0.6764(2) 0.0313(5) Uani 1 1 d . . . H7A H 0.5102 0.1850 0.6307 0.038 Uiso 1 1 calc R . . C8 C 0.4290(2) 0.0424(2) 0.6370(2) 0.0302(5) Uani 1 1 d . A . H8A H 0.3967 0.0196 0.5579 0.036 Uiso 1 1 calc R . . C9 C 0.4213(2) -0.01265(19) 0.7364(2) 0.0261(5) Uani 1 1 d . A . C10 C 0.3638(2) -0.1091(2) 0.7300(2) 0.0288(5) Uani 1 1 d . . . C11 C 0.6167(3) 0.3107(2) 0.8200(2) 0.0384(6) Uani 1 1 d . . . C12 C 0.5352(3) 0.3817(2) 0.7471(3) 0.0448(7) Uani 1 1 d . . . C13 C 0.5676(4) 0.4716(3) 0.7006(3) 0.0570(9) Uani 1 1 d . . . H13A H 0.5089 0.5174 0.6503 0.068 Uiso 1 1 calc R . . C14 C 0.6854(5) 0.4932(3) 0.7285(4) 0.0682(12) Uani 1 1 d . . . H14A H 0.7084 0.5553 0.6982 0.082 Uiso 1 1 calc R . . C15 C 0.7714(4) 0.4268(3) 0.7997(3) 0.0631(12) Uani 1 1 d . . . H15A H 0.8533 0.4422 0.8192 0.076 Uiso 1 1 calc R . . C16 C 0.7343(3) 0.3357(3) 0.8424(3) 0.0445(7) Uani 1 1 d . . . C17 C 0.2968(2) -0.1528(2) 0.6110(2) 0.0322(6) Uani 1 1 d . . . C18 C 0.3427(3) -0.2276(3) 0.5578(3) 0.0540(9) Uani 1 1 d . . . C19 C 0.2823(3) -0.2684(4) 0.4478(3) 0.0731(13) Uani 1 1 d . . . H19A H 0.3179 -0.3199 0.4141 0.088 Uiso 1 1 calc R . . C20 C 0.1685(3) -0.2318(3) 0.3882(3) 0.0594(10) Uani 1 1 d . . . H20A H 0.1251 -0.2589 0.3126 0.071 Uiso 1 1 calc R . . C21 C 0.1180(2) -0.1581(3) 0.4357(2) 0.0428(7) Uani 1 1 d . . . H21A H 0.0397 -0.1334 0.3943 0.051 Uiso 1 1 calc R . . C22 C 0.1823(2) -0.1196(2) 0.5452(2) 0.0333(6) Uani 1 1 d . . . Fe1 Fe 0.47790(8) 0.00462(17) 0.99512(19) 0.0265(3) Uani 0.50 1 d P . 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 F1 0.0531(11) 0.0429(10) 0.0615(12) 0.0086(9) 0.0180(9) 0.0031(9) F2 0.0368(9) 0.0927(16) 0.0465(10) -0.0222(10) 0.0178(8) -0.0246(10) F3 0.0345(10) 0.126(2) 0.0772(15) -0.0690(15) -0.0064(10) 0.0182(12) F4 0.0360(9) 0.0409(10) 0.0553(11) 0.0002(8) -0.0034(8) 0.0087(8) O1 0.052(5) 0.043(4) 0.050(5) -0.004(4) 0.011(4) 0.014(4) O1' 0.034(6) 0.065(9) 0.066(9) -0.023(7) 0.026(6) 0.001(5) N1 0.0199(9) 0.0277(11) 0.0301(10) -0.0056(8) 0.0061(8) -0.0037(8) N2 0.0210(9) 0.0250(10) 0.0324(11) -0.0071(8) 0.0058(8) -0.0017(8) N3 0.035(2) 0.037(3) 0.030(2) -0.0119(18) 0.0104(19) -0.0094(19) C1 0.0198(10) 0.0310(13) 0.0334(13) -0.0080(10) 0.0055(9) -0.0028(9) C2 0.0259(12) 0.0347(14) 0.0378(14) -0.0101(11) 0.0069(10) -0.0098(10) C3 0.0323(13) 0.0326(14) 0.0389(14) -0.0098(11) 0.0134(11) -0.0116(11) C4 0.0240(11) 0.0279(12) 0.0374(13) -0.0079(10) 0.0113(10) -0.0079(10) C5 0.0269(12) 0.0305(13) 0.0354(13) -0.0064(10) 0.0130(10) -0.0054(10) C6 0.0239(11) 0.0280(13) 0.0333(13) -0.0044(10) 0.0084(9) -0.0010(9) C7 0.0292(12) 0.0296(13) 0.0325(13) -0.0003(10) 0.0079(10) 0.0007(10) C8 0.0255(12) 0.0312(13) 0.0274(12) -0.0035(10) 0.0016(9) 0.0025(10) C9 0.0179(10) 0.0274(12) 0.0280(12) -0.0038(9) 0.0020(9) 0.0026(9) C10 0.0185(10) 0.0322(13) 0.0297(12) -0.0069(10) 0.0013(9) -0.0001(9) C11 0.0478(16) 0.0373(15) 0.0354(14) -0.0147(12) 0.0212(12) -0.0179(13) C12 0.0622(19) 0.0303(15) 0.0437(16) -0.0042(12) 0.0212(14) -0.0067(14) C13 0.089(3) 0.0321(16) 0.058(2) -0.0041(14) 0.0362(19) -0.0137(17) C14 0.117(4) 0.0410(19) 0.058(2) -0.0169(17) 0.046(2) -0.035(2) C15 0.078(2) 0.075(3) 0.050(2) -0.0354(19) 0.0397(19) -0.054(2) C16 0.0439(16) 0.0562(19) 0.0350(15) -0.0173(13) 0.0161(13) -0.0210(15) C17 0.0246(11) 0.0368(14) 0.0294(13) -0.0061(10) 0.0027(10) -0.0091(10) C18 0.0276(14) 0.081(3) 0.0445(17) -0.0317(17) 0.0015(12) -0.0047(15) C19 0.0416(18) 0.116(4) 0.053(2) -0.052(2) 0.0057(16) -0.009(2) C20 0.0436(17) 0.096(3) 0.0316(15) -0.0220(17) 0.0046(13) -0.0276(19) C21 0.0301(13) 0.0579(19) 0.0310(14) 0.0078(13) -0.0005(11) -0.0137(13) C22 0.0277(12) 0.0338(14) 0.0327(13) 0.0046(11) 0.0038(10) -0.0084(11) Fe1 0.0264(8) 0.0248(5) 0.0279(4) -0.0089(3) 0.0093(8) -0.0085(8) _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 F1 C12 1.337(4) . ? F2 C16 1.360(4) . ? F3 C18 1.361(4) . ? F4 C22 1.347(3) . ? O1 N3 1.167(9) . ? O1' N3 1.180(13) . ? N1 C4 1.379(3) . ? N1 C1 1.381(3) . ? N1 Fe1 1.934(3) 3_657 ? N1 Fe1 2.064(3) . ? N2 C9 1.375(3) . ? N2 C6 1.380(3) . ? N2 Fe1 1.996(3) . ? N2 Fe1 2.019(3) 3_657 ? N3 Fe1 1.738(5) . ? N3 Fe1 2.249(5) 3_657 ? C1 C10 1.384(4) 3_657 ? C1 C2 1.440(4) . ? C2 C3 1.337(4) . ? C2 H2A 0.9500 . ? C3 C4 1.438(3) . ? C3 H3A 0.9500 . ? C4 C5 1.389(4) . ? C5 C6 1.398(3) . ? C5 C11 1.500(4) . ? C6 C7 1.433(4) . ? C7 C8 1.349(4) . ? C7 H7A 0.9500 . ? C8 C9 1.433(4) . ? C8 H8A 0.9500 . ? C9 C10 1.389(4) . ? C10 C1 1.384(4) 3_657 ? C10 C17 1.495(3) . ? C11 C16 1.380(4) . ? C11 C12 1.392(5) . ? C12 C13 1.386(4) . ? C13 C14 1.363(6) . ? C13 H13A 0.9500 . ? C14 C15 1.375(6) . ? C14 H14A 0.9500 . ? C15 C16 1.401(5) . ? C15 H15A 0.9500 . ? C17 C18 1.370(4) . ? C17 C22 1.390(3) . ? C18 C19 1.382(4) . ? C19 C20 1.382(5) . ? C19 H19A 0.9500 . ? C20 C21 1.351(5) . ? C20 H20A 0.9500 . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? Fe1 Fe1 0.5159(16) 3_657 ? Fe1 N1 1.934(3) 3_657 ? Fe1 N2 2.019(3) 3_657 ? Fe1 N3 2.249(5) 3_657 ? 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 C4 N1 C1 105.0(2) . . ? C4 N1 Fe1 127.89(18) . 3_657 ? C1 N1 Fe1 126.00(19) . 3_657 ? C4 N1 Fe1 127.24(17) . . ? C1 N1 Fe1 127.38(18) . . ? C9 N2 C6 104.8(2) . . ? C9 N2 Fe1 124.59(18) . . ? C6 N2 Fe1 130.03(17) . . ? C9 N2 Fe1 128.60(18) . 3_657 ? C6 N2 Fe1 125.79(17) . 3_657 ? O1 N3 O1' 45.8(7) . . ? O1 N3 Fe1 140.4(5) . . ? O1' N3 Fe1 135.7(8) . . ? O1 N3 Fe1 142.1(5) . 3_657 ? O1' N3 Fe1 137.3(8) . 3_657 ? N1 C1 C10 125.5(2) . 3_657 ? N1 C1 C2 110.3(2) . . ? C10 C1 C2 124.2(2) 3_657 . ? C3 C2 C1 107.0(2) . . ? C3 C2 H2A 126.5 . . ? C1 C2 H2A 126.5 . . ? C2 C3 C4 107.4(2) . . ? C2 C3 H3A 126.3 . . ? C4 C3 H3A 126.3 . . ? N1 C4 C5 125.9(2) . . ? N1 C4 C3 110.2(2) . . ? C5 C4 C3 123.9(2) . . ? C4 C5 C6 123.4(2) . . ? C4 C5 C11 118.0(2) . . ? C6 C5 C11 118.6(2) . . ? N2 C6 C5 125.0(2) . . ? N2 C6 C7 110.8(2) . . ? C5 C6 C7 124.2(2) . . ? C8 C7 C6 106.5(2) . . ? C8 C7 H7A 126.8 . . ? C6 C7 H7A 126.8 . . ? C7 C8 C9 107.4(2) . . ? C7 C8 H8A 126.3 . . ? C9 C8 H8A 126.3 . . ? N2 C9 C10 125.6(2) . . ? N2 C9 C8 110.5(2) . . ? C10 C9 C8 123.9(2) . . ? C1 C10 C9 124.3(2) 3_657 . ? C1 C10 C17 118.1(2) 3_657 . ? C9 C10 C17 117.6(2) . . ? C16 C11 C12 114.8(3) . . ? C16 C11 C5 121.8(3) . . ? C12 C11 C5 123.4(3) . . ? F1 C12 C13 118.3(3) . . ? F1 C12 C11 118.2(3) . . ? C13 C12 C11 123.5(3) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 121.3(3) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C16 117.9(3) . . ? C14 C15 H15A 121.0 . . ? C16 C15 H15A 121.0 . . ? F2 C16 C11 117.5(3) . . ? F2 C16 C15 118.8(3) . . ? C11 C16 C15 123.7(4) . . ? C18 C17 C22 114.7(2) . . ? C18 C17 C10 123.2(2) . . ? C22 C17 C10 122.2(2) . . ? F3 C18 C17 117.5(2) . . ? F3 C18 C19 118.6(3) . . ? C17 C18 C19 123.9(3) . . ? C18 C19 C20 117.9(3) . . ? C18 C19 H19A 121.1 . . ? C20 C19 H19A 121.1 . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 118.6(3) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? F4 C22 C21 119.2(2) . . ? F4 C22 C17 117.1(2) . . ? C21 C22 C17 123.7(3) . . ? Fe1 Fe1 N3 170.9(6) 3_657 . ? Fe1 Fe1 N1 97.3(5) 3_657 3_657 ? N3 Fe1 N1 91.78(17) . 3_657 ? Fe1 Fe1 N2 85.1(5) 3_657 . ? N3 Fe1 N2 95.50(18) . . ? N1 Fe1 N2 91.78(12) 3_657 . ? Fe1 Fe1 N2 80.2(5) 3_657 3_657 ? N3 Fe1 N2 99.06(18) . 3_657 ? N1 Fe1 N2 90.10(13) 3_657 3_657 ? N2 Fe1 N2 165.25(5) . 3_657 ? Fe1 Fe1 N1 68.4(5) 3_657 . ? N3 Fe1 N1 102.57(18) . . ? N1 Fe1 N1 165.64(6) 3_657 . ? N2 Fe1 N1 87.10(12) . . ? N2 Fe1 N1 87.46(11) 3_657 . ? Fe1 Fe1 N3 7.0(4) 3_657 3_657 ? N3 Fe1 N3 177.92(13) . 3_657 ? N1 Fe1 N3 90.29(15) 3_657 3_657 ? N2 Fe1 N3 84.62(14) . 3_657 ? N2 Fe1 N3 80.74(14) 3_657 3_657 ? N1 Fe1 N3 75.35(13) . 3_657 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C10 -179.7(2) . . . 3_657 ? Fe1 N1 C1 C10 -10.9(3) 3_657 . . 3_657 ? Fe1 N1 C1 C10 6.9(4) . . . 3_657 ? C4 N1 C1 C2 1.4(3) . . . . ? Fe1 N1 C1 C2 170.16(17) 3_657 . . . ? Fe1 N1 C1 C2 -171.99(17) . . . . ? N1 C1 C2 C3 0.1(3) . . . . ? C10 C1 C2 C3 -178.9(2) 3_657 . . . ? C1 C2 C3 C4 -1.4(3) . . . . ? C1 N1 C4 C5 176.7(2) . . . . ? Fe1 N1 C4 C5 8.2(4) 3_657 . . . ? Fe1 N1 C4 C5 -10.0(4) . . . . ? C1 N1 C4 C3 -2.3(3) . . . . ? Fe1 N1 C4 C3 -170.77(17) 3_657 . . . ? Fe1 N1 C4 C3 171.11(17) . . . . ? C2 C3 C4 N1 2.4(3) . . . . ? C2 C3 C4 C5 -176.6(3) . . . . ? N1 C4 C5 C6 0.4(4) . . . . ? C3 C4 C5 C6 179.2(2) . . . . ? N1 C4 C5 C11 -179.8(2) . . . . ? C3 C4 C5 C11 -1.0(4) . . . . ? C9 N2 C6 C5 177.3(2) . . . . ? Fe1 N2 C6 C5 5.8(4) . . . . ? Fe1 N2 C6 C5 -12.1(3) 3_657 . . . ? C9 N2 C6 C7 -1.4(3) . . . . ? Fe1 N2 C6 C7 -172.99(17) . . . . ? Fe1 N2 C6 C7 169.06(17) 3_657 . . . ? C4 C5 C6 N2 2.1(4) . . . . ? C11 C5 C6 N2 -177.8(2) . . . . ? C4 C5 C6 C7 -179.3(2) . . . . ? C11 C5 C6 C7 0.8(4) . . . . ? N2 C6 C7 C8 1.1(3) . . . . ? C5 C6 C7 C8 -177.7(2) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C6 N2 C9 C10 -179.3(2) . . . . ? Fe1 N2 C9 C10 -7.1(3) . . . . ? Fe1 N2 C9 C10 10.6(3) 3_657 . . . ? C6 N2 C9 C8 1.3(3) . . . . ? Fe1 N2 C9 C8 173.41(16) . . . . ? Fe1 N2 C9 C8 -168.87(16) 3_657 . . . ? C7 C8 C9 N2 -0.7(3) . . . . ? C7 C8 C9 C10 179.9(2) . . . . ? N2 C9 C10 C1 -3.5(4) . . . 3_657 ? C8 C9 C10 C1 175.9(2) . . . 3_657 ? N2 C9 C10 C17 174.8(2) . . . . ? C8 C9 C10 C17 -5.8(3) . . . . ? C4 C5 C11 C16 65.5(4) . . . . ? C6 C5 C11 C16 -114.6(3) . . . . ? C4 C5 C11 C12 -112.6(3) . . . . ? C6 C5 C11 C12 67.2(4) . . . . ? C16 C11 C12 F1 178.5(3) . . . . ? C5 C11 C12 F1 -3.3(4) . . . . ? C16 C11 C12 C13 -0.7(4) . . . . ? C5 C11 C12 C13 177.5(3) . . . . ? F1 C12 C13 C14 179.9(3) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C12 C11 C16 F2 -177.8(2) . . . . ? C5 C11 C16 F2 4.0(4) . . . . ? C12 C11 C16 C15 2.2(4) . . . . ? C5 C11 C16 C15 -176.1(3) . . . . ? C14 C15 C16 F2 178.0(3) . . . . ? C14 C15 C16 C11 -2.0(5) . . . . ? C1 C10 C17 C18 -83.9(4) 3_657 . . . ? C9 C10 C17 C18 97.7(4) . . . . ? C1 C10 C17 C22 96.5(3) 3_657 . . . ? C9 C10 C17 C22 -81.9(3) . . . . ? C22 C17 C18 F3 -178.8(3) . . . . ? C10 C17 C18 F3 1.6(5) . . . . ? C22 C17 C18 C19 -0.1(6) . . . . ? C10 C17 C18 C19 -179.6(4) . . . . ? F3 C18 C19 C20 178.4(4) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C18 C19 C20 C21 0.3(7) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 F4 179.0(3) . . . . ? C20 C21 C22 C17 -0.5(5) . . . . ? C18 C17 C22 F4 -179.0(3) . . . . ? C10 C17 C22 F4 0.5(4) . . . . ? C18 C17 C22 C21 0.5(4) . . . . ? C10 C17 C22 C21 -179.9(3) . . . . ? O1 N3 Fe1 N1 -37.1(10) . . . 3_657 ? O1' N3 Fe1 N1 33.7(11) . . . 3_657 ? Fe1 N3 Fe1 N1 175(4) 3_657 . . 3_657 ? O1 N3 Fe1 N2 54.8(10) . . . . ? O1' N3 Fe1 N2 125.7(11) . . . . ? Fe1 N3 Fe1 N2 -93(4) 3_657 . . . ? O1 N3 Fe1 N2 -127.5(10) . . . 3_657 ? O1' N3 Fe1 N2 -56.6(11) . . . 3_657 ? Fe1 N3 Fe1 N2 84(4) 3_657 . . 3_657 ? O1 N3 Fe1 N1 143.1(10) . . . . ? O1' N3 Fe1 N1 -146.0(11) . . . . ? Fe1 N3 Fe1 N1 -5(4) 3_657 . . . ? C9 N2 Fe1 Fe1 110.9(5) . . . 3_657 ? C6 N2 Fe1 Fe1 -79.0(5) . . . 3_657 ? C9 N2 Fe1 N3 -78.2(2) . . . . ? C6 N2 Fe1 N3 91.9(3) . . . . ? Fe1 N2 Fe1 N3 170.9(6) 3_657 . . . ? C9 N2 Fe1 N1 13.8(2) . . . 3_657 ? C6 N2 Fe1 N1 -176.2(2) . . . 3_657 ? Fe1 N2 Fe1 N1 -97.2(5) 3_657 . . 3_657 ? C9 N2 Fe1 N2 110.9(5) . . . 3_657 ? C6 N2 Fe1 N2 -79.0(5) . . . 3_657 ? Fe1 N2 Fe1 N2 0.0 3_657 . . 3_657 ? C9 N2 Fe1 N1 179.44(19) . . . . ? C6 N2 Fe1 N1 -10.5(2) . . . . ? Fe1 N2 Fe1 N1 68.5(5) 3_657 . . . ? C9 N2 Fe1 N3 103.9(2) . . . 3_657 ? C6 N2 Fe1 N3 -86.1(2) . . . 3_657 ? Fe1 N2 Fe1 N3 -7.0(4) 3_657 . . 3_657 ? C4 N1 Fe1 Fe1 98.1(5) . . . 3_657 ? C1 N1 Fe1 Fe1 -89.9(5) . . . 3_657 ? C4 N1 Fe1 N3 -82.7(3) . . . . ? C1 N1 Fe1 N3 89.2(3) . . . . ? Fe1 N1 Fe1 N3 179.2(6) 3_657 . . . ? C4 N1 Fe1 N1 98.1(5) . . . 3_657 ? C1 N1 Fe1 N1 -89.9(5) . . . 3_657 ? Fe1 N1 Fe1 N1 0.0 3_657 . . 3_657 ? C4 N1 Fe1 N2 12.3(2) . . . . ? C1 N1 Fe1 N2 -175.8(2) . . . . ? Fe1 N1 Fe1 N2 -85.8(5) 3_657 . . . ? C4 N1 Fe1 N2 178.6(2) . . . 3_657 ? C1 N1 Fe1 N2 -9.5(2) . . . 3_657 ? Fe1 N1 Fe1 N2 80.4(5) 3_657 . . 3_657 ? C4 N1 Fe1 N3 97.5(2) . . . 3_657 ? C1 N1 Fe1 N3 -90.6(2) . . . 3_657 ? Fe1 N1 Fe1 N3 -0.7(5) 3_657 . . 3_657 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.622 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.066 _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -14.00 1.00 14.00 0.2569 11.00 3.00 -16.00 0.1835 -11.00 12.00 -2.00 0.2959 -5.00 11.00 -10.00 0.2961 14.00 -2.00 -14.00 0.2280 11.00 -12.00 2.00 0.2977 11.00 12.00 2.00 0.3302 -11.00 0.00 -8.00 0.3269 -11.00 7.00 -6.00 0.3169 -6.00 2.00 17.00 0.1969 -13.00 11.00 3.00 0.3035 16.00 5.00 -3.00 0.3526 -5.00 -4.00 -13.00 0.3193 13.00 -11.00 -1.00 0.2942 13.00 1.00 -15.00 0.1816 -1.00 1.00 17.00 0.1657 -15.00 -4.00 12.00 0.2840 -11.00 -11.00 -2.00 0.2763 _audit_creation_date ; 'Tue Oct 10 14:03:45 2006' ; _audit_creation_method_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_collection_reference ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinment_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _cell_measurement_reflns_used 7010 _cell_measurement_theta_min 3.9051 _cell_measurement_theta_max 28.4993 _cell_measurement_resolution_max 0.74 _cell_measurement_temperature 110 _exptl_crystal_size_max 0.8256 _exptl_crystal_size_mid 0.6226 _exptl_crystal_size_min 0.4507 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_detector_area_resol_mean 15.9890 _diffrn_orient_matrix_UB_11 -0.0203115457 _diffrn_orient_matrix_UB_12 0.0521286036 _diffrn_orient_matrix_UB_13 -0.0173932361 _diffrn_orient_matrix_UB_21 0.0030937910 _diffrn_orient_matrix_UB_22 -0.0095825456 _diffrn_orient_matrix_UB_23 -0.0558448940 _diffrn_orient_matrix_UB_31 -0.0593856888 _diffrn_orient_matrix_UB_32 -0.0183284196 _diffrn_orient_matrix_UB_33 -0.0202493456 _diffrn_measurement_details 'see scan set' loop_ _diffrn_scan_number _diffrn_scan_type _diffrn_scan_start _diffrn_scan_end _diffrn_scan_width _diffrn_scan_exptime _diffrn_scan_omega _diffrn_scan_theta _diffrn_scan_kappa _diffrn_scan_phi _diffrn_scan_omega1 _diffrn_scan_theta1 _diffrn_scan_frames 1 omega -30.00 11.00 1.00 4.00 - 24.85 116.00 328.00 0.00 0.00 41 2 omega 45.00 97.00 1.00 4.00 - 24.85 75.00 120.00 0.00 0.00 52 3 omega 45.00 97.00 1.00 4.00 - 24.85 76.00 -23.00 0.00 0.00 52 4 omega -3.00 41.00 1.00 4.00 - 24.85 -125.00 326.00 0.00 0.00 44 5 phi -179.00 -120.00 1.00 4.00 -40.00 -25.62 0.00 - 0.00 0.00 59 6 omega -16.94 83.06 1.00 4.00 - 32.00 -109.00 140.00 0.00 0.00 100 7 omega -0.52 94.48 1.00 4.00 - 32.00 -129.00 50.00 0.00 0.00 95 8 omega -3.00 25.00 1.00 4.00 - -25.62 45.00 120.00 0.00 0.00 28 _diffrn_measurement_method ' omega phi scans' _JHU_your_name_here 'Dr. Amy A Sarjeant' _JHU_your_lab_here 'NCB 240' _JHU_your_phone_number_here 'x6-8569' _JHU_your_email_here 'xray@jhu.edu' _JHU_Institutional_Source 'Karlin Lab' _JHU_Submitting_Scientist 'Jun Wang' _JHU_Scientist_Phone 'x6-7937' _JHU_Scientist_EMail 'jun.wang@jhu.edu' _JHU_identifying_number 'x0299' _JHU_xray_labbook 'II-33' _JHU_crystalization_labbook '20061010_2' _JHU_crystalization_solvent 'Methylene Chloride, Hexane, Methanol' _JHU_crystalization_method '' _diffrn_source_power '2' _diffrn_source_voltage '50' _diffrn_source_current '40' _diffrn_measurement_device 'Kappa' _diffrn_measurement_device_type 'Xcalibur3' _diffrn_ambient_temperature 110 _JHU_diffraction_detector_distance '50' _JHU_quality_factor '2'