data_erk4197 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Fe Li N' _chemical_formula_weight 225.10 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' 'Li' 'Li' -0.0003 0.0001 '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 7.4443(1) _cell_length_b 9.2993(2) _cell_length_c 9.9602(3) _cell_angle_alpha 95.318(1) _cell_angle_beta 108.510(1) _cell_angle_gamma 102.226(2) _cell_volume 629.43(2) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 1532 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7196 _exptl_absorpt_correction_T_max 0.8916 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5795 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.26 _reflns_number_total 3013 _reflns_number_gt 2587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000) & SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0310P)^2^+0.3841P] 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 'riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3013 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Li1 Li -0.0574(5) 0.3859(4) 0.0371(4) 0.0276(7) Uani 1 1 d . . . Fe Fe 0.31262(4) 0.76368(3) 0.24742(3) 0.01983(9) Uani 1 1 d . . . C1 C 0.5472(3) 0.7081(2) 0.2231(2) 0.0257(4) Uani 1 1 d . . . C2 C 0.6093(3) 0.8384(2) 0.3307(3) 0.0328(5) Uani 1 1 d . . . H2 H 0.6910 0.8475 0.4278 0.039 Uiso 1 1 calc R . . C3 C 0.5280(3) 0.9529(2) 0.2677(3) 0.0370(6) Uani 1 1 d . . . H3 H 0.5438 1.0501 0.3161 0.044 Uiso 1 1 calc R . . C4 C 0.4198(3) 0.8954(3) 0.1205(3) 0.0350(5) Uani 1 1 d . . . H4 H 0.3498 0.9471 0.0526 0.042 Uiso 1 1 calc R . . C5 C 0.4348(3) 0.7457(2) 0.0924(2) 0.0291(4) Uani 1 1 d . . . H5 H 0.3791 0.6817 0.0016 0.035 Uiso 1 1 calc R . . C6 C 0.5812(3) 0.5575(2) 0.2473(3) 0.0297(5) Uani 1 1 d . . . H6A H 0.6465 0.5617 0.3516 0.036 Uiso 1 1 calc R . . H6B H 0.6718 0.5359 0.1985 0.036 Uiso 1 1 calc R . . C8 C 0.3951(3) 0.4284(2) 0.1937(2) 0.0257(4) Uani 1 1 d . . . H8A H 0.4342 0.3330 0.1942 0.031 Uiso 1 1 calc R . . H8B H 0.3210 0.4325 0.0927 0.031 Uiso 1 1 calc R . . C9 C 0.2572(3) 0.4272(2) 0.2814(2) 0.0208(4) Uani 1 1 d . . . H9 H 0.3281 0.4139 0.3812 0.025 Uiso 1 1 calc R . . C10 C 0.1857(3) 0.5678(2) 0.2899(2) 0.0189(4) Uani 1 1 d . . . C11 C 0.2472(3) 0.6826(2) 0.4136(2) 0.0251(4) Uani 1 1 d . . . H11 H 0.3373 0.6833 0.5061 0.030 Uiso 1 1 calc R . . C12 C 0.1481(3) 0.7952(2) 0.3722(2) 0.0276(4) Uani 1 1 d . . . H12 H 0.1620 0.8861 0.4310 0.033 Uiso 1 1 calc R . . C13 C 0.0249(3) 0.7461(2) 0.2266(2) 0.0243(4) Uani 1 1 d . . . H13 H -0.0586 0.8008 0.1732 0.029 Uiso 1 1 calc R . . C14 C 0.0409(3) 0.6033(2) 0.1690(2) 0.0202(4) Uani 1 1 d . . . N1 N 0.0783(2) 0.29939(17) 0.21559(19) 0.0238(4) Uani 1 1 d . . . C15 C 0.1244(4) 0.1545(2) 0.1926(3) 0.0388(6) Uani 1 1 d . . . H15A H 0.2163 0.1397 0.2824 0.058 Uiso 1 1 calc R . . H15B H 0.1839 0.1535 0.1178 0.058 Uiso 1 1 calc R . . H15C H 0.0037 0.0740 0.1623 0.058 Uiso 1 1 calc R . . C16 C -0.0388(3) 0.2882(2) 0.3107(3) 0.0339(5) Uani 1 1 d . . . H16A H -0.1583 0.2070 0.2661 0.051 Uiso 1 1 calc R . . H16B H -0.0741 0.3826 0.3258 0.051 Uiso 1 1 calc R . . H16C H 0.0381 0.2675 0.4033 0.051 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 Li1 0.0308(17) 0.0189(16) 0.0278(19) 0.0061(14) 0.0062(15) 0.0004(14) Fe 0.01818(14) 0.01479(14) 0.02432(16) 0.00226(10) 0.00776(11) -0.00053(10) C1 0.0150(8) 0.0259(10) 0.0384(12) 0.0072(9) 0.0134(8) 0.0026(8) C2 0.0181(9) 0.0258(11) 0.0442(14) 0.0031(10) 0.0039(9) -0.0038(8) C3 0.0270(11) 0.0193(10) 0.0615(17) 0.0068(10) 0.0183(11) -0.0051(8) C4 0.0305(11) 0.0332(12) 0.0510(15) 0.0234(11) 0.0237(11) 0.0067(9) C5 0.0263(10) 0.0336(11) 0.0316(11) 0.0090(9) 0.0177(9) 0.0031(9) C6 0.0207(10) 0.0292(11) 0.0414(13) 0.0055(9) 0.0132(9) 0.0075(8) C8 0.0266(10) 0.0203(9) 0.0321(11) 0.0041(8) 0.0114(9) 0.0078(8) C9 0.0230(9) 0.0163(9) 0.0219(10) 0.0057(7) 0.0058(8) 0.0044(7) C10 0.0202(8) 0.0148(8) 0.0223(10) 0.0046(7) 0.0102(7) 0.0008(7) C11 0.0335(10) 0.0229(10) 0.0189(10) 0.0034(8) 0.0112(8) 0.0042(8) C12 0.0361(11) 0.0195(9) 0.0318(11) 0.0000(8) 0.0203(9) 0.0051(8) C13 0.0200(9) 0.0195(9) 0.0357(12) 0.0036(8) 0.0139(8) 0.0038(7) C14 0.0151(8) 0.0156(9) 0.0278(10) 0.0033(7) 0.0077(7) -0.0008(7) N1 0.0259(8) 0.0130(7) 0.0312(9) 0.0066(7) 0.0097(7) 0.0011(6) C15 0.0438(13) 0.0161(10) 0.0538(16) 0.0073(10) 0.0132(12) 0.0070(9) C16 0.0329(11) 0.0292(11) 0.0418(14) 0.0153(10) 0.0171(10) 0.0020(9) _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 Li1 N1 2.073(4) . ? Li1 C14 2.105(4) 2_565 ? Li1 C14 2.150(4) . ? Li1 Li1 2.388(7) 2_565 ? Li1 C5 2.647(4) 2_565 ? Li1 C9 2.717(4) . ? Li1 C10 2.738(4) . ? Li1 Fe 2.882(3) 2_565 ? Fe C1 2.0005(18) . ? Fe C10 2.0142(18) . ? Fe C2 2.032(2) . ? Fe C11 2.033(2) . ? Fe C5 2.036(2) . ? Fe C12 2.0447(19) . ? Fe C13 2.0547(18) . ? Fe C3 2.059(2) . ? Fe C4 2.061(2) . ? Fe C14 2.1041(18) . ? Fe Li1 2.882(3) 2_565 ? C1 C5 1.425(3) . ? C1 C2 1.427(3) . ? C1 C6 1.503(3) . ? C2 C3 1.431(3) . ? C3 C4 1.417(4) . ? C4 C5 1.429(3) . ? C5 Li1 2.647(4) 2_565 ? C6 C8 1.534(3) . ? C8 C9 1.544(3) . ? C9 N1 1.499(2) . ? C9 C10 1.518(2) . ? C10 C11 1.434(3) . ? C10 C14 1.457(3) . ? C11 C12 1.423(3) . ? C12 C13 1.417(3) . ? C13 C14 1.440(3) . ? C14 Li1 2.105(4) 2_565 ? N1 C16 1.474(3) . ? N1 C15 1.475(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 N1 Li1 C14 136.93(19) . 2_565 ? N1 Li1 C14 89.09(15) . . ? C14 Li1 C14 111.72(16) 2_565 . ? N1 Li1 Li1 129.0(2) . 2_565 ? C14 Li1 Li1 56.75(15) 2_565 2_565 ? C14 Li1 Li1 54.97(14) . 2_565 ? N1 Li1 C5 114.31(15) . 2_565 ? C14 Li1 C5 87.21(14) 2_565 2_565 ? C14 Li1 C5 121.48(16) . 2_565 ? Li1 Li1 C5 115.3(2) 2_565 2_565 ? N1 Li1 C9 33.14(8) . . ? C14 Li1 C9 124.59(16) 2_565 . ? C14 Li1 C9 63.79(11) . . ? Li1 Li1 C9 95.90(19) 2_565 . ? C5 Li1 C9 145.17(15) 2_565 . ? N1 Li1 C10 58.45(10) . . ? C14 Li1 C10 127.14(16) 2_565 . ? C14 Li1 C10 31.87(8) . . ? Li1 Li1 C10 76.57(17) 2_565 . ? C5 Li1 C10 138.80(15) 2_565 . ? C9 Li1 C10 32.31(7) . . ? N1 Li1 Fe 130.31(15) . 2_565 ? C14 Li1 Fe 46.77(8) 2_565 2_565 ? C14 Li1 Fe 140.00(16) . 2_565 ? Li1 Li1 Fe 94.92(19) 2_565 2_565 ? C5 Li1 Fe 42.96(7) 2_565 2_565 ? C9 Li1 Fe 154.13(14) . 2_565 ? C10 Li1 Fe 171.13(14) . 2_565 ? C1 Fe C10 98.11(8) . . ? C1 Fe C2 41.45(9) . . ? C10 Fe C2 118.37(8) . . ? C1 Fe C11 112.08(9) . . ? C10 Fe C11 41.51(7) . . ? C2 Fe C11 102.34(9) . . ? C1 Fe C5 41.34(9) . . ? C10 Fe C5 114.95(8) . . ? C2 Fe C5 68.56(9) . . ? C11 Fe C5 148.85(9) . . ? C1 Fe C12 150.22(9) . . ? C10 Fe C12 69.06(8) . . ? C2 Fe C12 120.03(9) . . ? C11 Fe C12 40.84(8) . . ? C5 Fe C12 168.44(9) . . ? C1 Fe C13 159.20(8) . . ? C10 Fe C13 67.67(8) . . ? C2 Fe C13 158.71(9) . . ? C11 Fe C13 67.95(8) . . ? C5 Fe C13 129.51(9) . . ? C12 Fe C13 40.45(8) . . ? C1 Fe C3 69.74(9) . . ? C10 Fe C3 158.26(9) . . ? C2 Fe C3 40.96(9) . . ? C11 Fe C3 125.02(9) . . ? C5 Fe C3 68.27(9) . . ? C12 Fe C3 112.37(9) . . ? C13 Fe C3 128.45(8) . . ? C1 Fe C4 69.72(9) . . ? C10 Fe C4 153.48(9) . . ? C2 Fe C4 68.47(10) . . ? C11 Fe C4 164.70(9) . . ? C5 Fe C4 40.82(9) . . ? C12 Fe C4 132.26(9) . . ? C13 Fe C4 116.14(9) . . ? C3 Fe C4 40.23(10) . . ? C1 Fe C14 118.91(8) . . ? C10 Fe C14 41.35(7) . . ? C2 Fe C14 156.15(8) . . ? C11 Fe C14 70.10(8) . . ? C5 Fe C14 105.71(8) . . ? C12 Fe C14 69.66(8) . . ? C13 Fe C14 40.50(7) . . ? C3 Fe C14 160.38(9) . . ? C4 Fe C14 123.21(9) . . ? C1 Fe Li1 93.46(9) . 2_565 ? C10 Fe Li1 79.08(9) . 2_565 ? C2 Fe Li1 130.54(10) . 2_565 ? C11 Fe Li1 116.20(9) . 2_565 ? C5 Fe Li1 62.35(9) . 2_565 ? C12 Fe Li1 109.42(9) . 2_565 ? C13 Fe Li1 69.56(9) . 2_565 ? C3 Fe Li1 118.53(10) . 2_565 ? C4 Fe Li1 78.30(10) . 2_565 ? C14 Fe Li1 46.80(9) . 2_565 ? C5 C1 C2 106.87(18) . . ? C5 C1 C6 127.05(19) . . ? C2 C1 C6 125.9(2) . . ? C5 C1 Fe 70.67(11) . . ? C2 C1 Fe 70.45(11) . . ? C6 C1 Fe 120.34(13) . . ? C1 C2 C3 108.6(2) . . ? C1 C2 Fe 68.10(11) . . ? C3 C2 Fe 70.54(12) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 Fe 69.98(12) . . ? C2 C3 Fe 68.50(11) . . ? C3 C4 C5 107.7(2) . . ? C3 C4 Fe 69.79(13) . . ? C5 C4 Fe 68.65(12) . . ? C1 C5 C4 108.9(2) . . ? C1 C5 Fe 67.98(11) . . ? C4 C5 Fe 70.53(12) . . ? C1 C5 Li1 121.70(15) . 2_565 ? C4 C5 Li1 98.33(15) . 2_565 ? Fe C5 Li1 74.69(10) . 2_565 ? C1 C6 C8 114.67(17) . . ? C6 C8 C9 115.27(16) . . ? N1 C9 C10 106.65(14) . . ? N1 C9 C8 110.19(15) . . ? C10 C9 C8 114.15(15) . . ? N1 C9 Li1 49.12(11) . . ? C10 C9 Li1 74.63(12) . . ? C8 C9 Li1 91.08(14) . . ? C11 C10 C14 110.60(16) . . ? C11 C10 C9 126.29(17) . . ? C14 C10 C9 123.11(16) . . ? C11 C10 Fe 69.96(11) . . ? C14 C10 Fe 72.64(10) . . ? C9 C10 Fe 124.39(12) . . ? C11 C10 Li1 158.20(16) . . ? C14 C10 Li1 51.19(11) . . ? C9 C10 Li1 73.05(12) . . ? Fe C10 Li1 109.24(10) . . ? C12 C11 C10 107.27(17) . . ? C12 C11 Fe 70.00(12) . . ? C10 C11 Fe 68.53(11) . . ? C13 C12 C11 107.10(17) . . ? C13 C12 Fe 70.15(11) . . ? C11 C12 Fe 69.16(11) . . ? C12 C13 C14 112.07(18) . . ? C12 C13 Fe 69.39(11) . . ? C14 C13 Fe 71.60(10) . . ? C13 C14 C10 102.93(16) . . ? C13 C14 Fe 67.90(10) . . ? C10 C14 Fe 66.01(10) . . ? C13 C14 Li1 108.14(16) . 2_565 ? C10 C14 Li1 126.09(16) . 2_565 ? Fe C14 Li1 86.43(11) . 2_565 ? C13 C14 Li1 156.65(17) . . ? C10 C14 Li1 96.93(15) . . ? Fe C14 Li1 132.77(13) . . ? Li1 C14 Li1 68.28(16) 2_565 . ? C16 N1 C15 107.88(17) . . ? C16 N1 C9 109.39(15) . . ? C15 N1 C9 113.10(15) . . ? C16 N1 Li1 109.85(16) . . ? C15 N1 Li1 118.42(17) . . ? C9 N1 Li1 97.73(14) . . ? 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 C10 Fe C1 C5 118.89(12) . . . . ? C2 Fe C1 C5 -116.80(18) . . . . ? C11 Fe C1 C5 159.56(12) . . . . ? C12 Fe C1 C5 -179.64(15) . . . . ? C13 Fe C1 C5 73.8(3) . . . . ? C3 Fe C1 C5 -79.75(14) . . . . ? C4 Fe C1 C5 -36.74(13) . . . . ? C14 Fe C1 C5 80.84(14) . . . . ? Li1 Fe C1 C5 39.44(13) 2_565 . . . ? C10 Fe C1 C2 -124.31(13) . . . . ? C11 Fe C1 C2 -83.64(14) . . . . ? C5 Fe C1 C2 116.80(18) . . . . ? C12 Fe C1 C2 -62.8(2) . . . . ? C13 Fe C1 C2 -169.4(2) . . . . ? C3 Fe C1 C2 37.05(14) . . . . ? C4 Fe C1 C2 80.06(14) . . . . ? C14 Fe C1 C2 -162.36(13) . . . . ? Li1 Fe C1 C2 156.24(14) 2_565 . . . ? C10 Fe C1 C6 -3.43(18) . . . . ? C2 Fe C1 C6 120.9(2) . . . . ? C11 Fe C1 C6 37.25(19) . . . . ? C5 Fe C1 C6 -122.3(2) . . . . ? C12 Fe C1 C6 58.0(3) . . . . ? C13 Fe C1 C6 -48.6(3) . . . . ? C3 Fe C1 C6 157.9(2) . . . . ? C4 Fe C1 C6 -159.1(2) . . . . ? C14 Fe C1 C6 -41.5(2) . . . . ? Li1 Fe C1 C6 -82.88(18) 2_565 . . . ? C5 C1 C2 C3 2.6(2) . . . . ? C6 C1 C2 C3 -172.94(18) . . . . ? Fe C1 C2 C3 -59.07(15) . . . . ? C5 C1 C2 Fe 61.66(13) . . . . ? C6 C1 C2 Fe -113.87(19) . . . . ? C10 Fe C2 C1 68.33(15) . . . . ? C11 Fe C2 C1 109.48(13) . . . . ? C5 Fe C2 C1 -39.31(13) . . . . ? C12 Fe C2 C1 149.31(12) . . . . ? C13 Fe C2 C1 169.7(2) . . . . ? C3 Fe C2 C1 -120.4(2) . . . . ? C4 Fe C2 C1 -83.33(14) . . . . ? C14 Fe C2 C1 41.0(3) . . . . ? Li1 Fe C2 C1 -31.96(18) 2_565 . . . ? C1 Fe C2 C3 120.4(2) . . . . ? C10 Fe C2 C3 -171.23(13) . . . . ? C11 Fe C2 C3 -130.09(14) . . . . ? C5 Fe C2 C3 81.13(15) . . . . ? C12 Fe C2 C3 -90.26(16) . . . . ? C13 Fe C2 C3 -69.9(3) . . . . ? C4 Fe C2 C3 37.10(14) . . . . ? C14 Fe C2 C3 161.42(19) . . . . ? Li1 Fe C2 C3 88.47(17) 2_565 . . . ? C1 C2 C3 C4 -1.5(2) . . . . ? Fe C2 C3 C4 -59.08(15) . . . . ? C1 C2 C3 Fe 57.57(14) . . . . ? C1 Fe C3 C4 82.19(14) . . . . ? C10 Fe C3 C4 140.9(2) . . . . ? C2 Fe C3 C4 119.7(2) . . . . ? C11 Fe C3 C4 -174.47(12) . . . . ? C5 Fe C3 C4 37.79(13) . . . . ? C12 Fe C3 C4 -129.75(13) . . . . ? C13 Fe C3 C4 -86.13(16) . . . . ? C14 Fe C3 C4 -37.8(3) . . . . ? Li1 Fe C3 C4 -0.48(16) 2_565 . . . ? C1 Fe C3 C2 -37.48(14) . . . . ? C10 Fe C3 C2 21.2(3) . . . . ? C11 Fe C3 C2 65.86(17) . . . . ? C5 Fe C3 C2 -81.88(15) . . . . ? C12 Fe C3 C2 110.58(15) . . . . ? C13 Fe C3 C2 154.20(14) . . . . ? C4 Fe C3 C2 -119.7(2) . . . . ? C14 Fe C3 C2 -157.4(2) . . . . ? Li1 Fe C3 C2 -120.16(15) 2_565 . . . ? C2 C3 C4 C5 -0.2(2) . . . . ? Fe C3 C4 C5 -58.35(14) . . . . ? C2 C3 C4 Fe 58.16(15) . . . . ? C1 Fe C4 C3 -82.26(14) . . . . ? C10 Fe C4 C3 -148.46(17) . . . . ? C2 Fe C4 C3 -37.75(13) . . . . ? C11 Fe C4 C3 17.4(4) . . . . ? C5 Fe C4 C3 -119.45(19) . . . . ? C12 Fe C4 C3 73.86(17) . . . . ? C13 Fe C4 C3 119.49(13) . . . . ? C14 Fe C4 C3 165.77(12) . . . . ? Li1 Fe C4 C3 179.57(15) 2_565 . . . ? C1 Fe C4 C5 37.19(13) . . . . ? C10 Fe C4 C5 -29.0(2) . . . . ? C2 Fe C4 C5 81.70(14) . . . . ? C11 Fe C4 C5 136.9(3) . . . . ? C12 Fe C4 C5 -166.69(13) . . . . ? C13 Fe C4 C5 -121.06(13) . . . . ? C3 Fe C4 C5 119.45(19) . . . . ? C14 Fe C4 C5 -74.78(15) . . . . ? Li1 Fe C4 C5 -60.98(14) 2_565 . . . ? C2 C1 C5 C4 -2.7(2) . . . . ? C6 C1 C5 C4 172.75(18) . . . . ? Fe C1 C5 C4 58.79(14) . . . . ? C2 C1 C5 Fe -61.52(13) . . . . ? C6 C1 C5 Fe 113.96(19) . . . . ? C2 C1 C5 Li1 -115.75(18) . . . 2_565 ? C6 C1 C5 Li1 59.7(3) . . . 2_565 ? Fe C1 C5 Li1 -54.23(15) . . . 2_565 ? C3 C4 C5 C1 1.8(2) . . . . ? Fe C4 C5 C1 -57.24(13) . . . . ? C3 C4 C5 Fe 59.07(14) . . . . ? C3 C4 C5 Li1 129.51(17) . . . 2_565 ? Fe C4 C5 Li1 70.44(10) . . . 2_565 ? C10 Fe C5 C1 -72.95(13) . . . . ? C2 Fe C5 C1 39.41(12) . . . . ? C11 Fe C5 C1 -38.7(2) . . . . ? C12 Fe C5 C1 179.1(4) . . . . ? C13 Fe C5 C1 -153.77(12) . . . . ? C3 Fe C5 C1 83.61(13) . . . . ? C4 Fe C5 C1 120.87(18) . . . . ? C14 Fe C5 C1 -116.13(12) . . . . ? Li1 Fe C5 C1 -134.29(15) 2_565 . . . ? C1 Fe C5 C4 -120.87(18) . . . . ? C10 Fe C5 C4 166.18(13) . . . . ? C2 Fe C5 C4 -81.46(14) . . . . ? C11 Fe C5 C4 -159.59(16) . . . . ? C12 Fe C5 C4 58.2(4) . . . . ? C13 Fe C5 C4 85.36(15) . . . . ? C3 Fe C5 C4 -37.26(13) . . . . ? C14 Fe C5 C4 123.00(13) . . . . ? Li1 Fe C5 C4 104.84(16) 2_565 . . . ? C1 Fe C5 Li1 134.29(15) . . . 2_565 ? C10 Fe C5 Li1 61.35(11) . . . 2_565 ? C2 Fe C5 Li1 173.70(11) . . . 2_565 ? C11 Fe C5 Li1 95.57(17) . . . 2_565 ? C12 Fe C5 Li1 -46.6(4) . . . 2_565 ? C13 Fe C5 Li1 -19.48(13) . . . 2_565 ? C3 Fe C5 Li1 -142.10(12) . . . 2_565 ? C4 Fe C5 Li1 -104.84(16) . . . 2_565 ? C14 Fe C5 Li1 18.16(10) . . . 2_565 ? C5 C1 C6 C8 -49.4(3) . . . . ? C2 C1 C6 C8 125.2(2) . . . . ? Fe C1 C6 C8 38.4(3) . . . . ? C1 C6 C8 C9 -70.8(2) . . . . ? C6 C8 C9 N1 178.04(16) . . . . ? C6 C8 C9 C10 58.1(2) . . . . ? C6 C8 C9 Li1 131.71(17) . . . . ? C14 Li1 C9 N1 -124.5(2) 2_565 . . . ? C14 Li1 C9 N1 136.18(18) . . . . ? Li1 Li1 C9 N1 -177.8(3) 2_565 . . . ? C5 Li1 C9 N1 28.0(2) 2_565 . . . ? C10 Li1 C9 N1 129.11(17) . . . . ? Fe Li1 C9 N1 -63.5(3) 2_565 . . . ? N1 Li1 C9 C10 -129.11(17) . . . . ? C14 Li1 C9 C10 106.4(2) 2_565 . . . ? C14 Li1 C9 C10 7.07(11) . . . . ? Li1 Li1 C9 C10 53.12(19) 2_565 . . . ? C5 Li1 C9 C10 -101.1(3) 2_565 . . . ? Fe Li1 C9 C10 167.4(3) 2_565 . . . ? N1 Li1 C9 C8 116.11(16) . . . . ? C14 Li1 C9 C8 -8.4(2) 2_565 . . . ? C14 Li1 C9 C8 -107.71(14) . . . . ? Li1 Li1 C9 C8 -61.7(2) 2_565 . . . ? C5 Li1 C9 C8 144.1(3) 2_565 . . . ? C10 Li1 C9 C8 -114.78(15) . . . . ? Fe Li1 C9 C8 52.6(3) 2_565 . . . ? N1 C9 C10 C11 130.89(19) . . . . ? C8 C9 C10 C11 -107.2(2) . . . . ? Li1 C9 C10 C11 168.7(2) . . . . ? N1 C9 C10 C14 -49.0(2) . . . . ? C8 C9 C10 C14 72.9(2) . . . . ? Li1 C9 C10 C14 -11.22(17) . . . . ? N1 C9 C10 Fe -139.82(14) . . . . ? C8 C9 C10 Fe -17.9(2) . . . . ? Li1 C9 C10 Fe -102.06(15) . . . . ? N1 C9 C10 Li1 -37.76(14) . . . . ? C8 C9 C10 Li1 84.16(16) . . . . ? C1 Fe C10 C11 114.33(12) . . . . ? C2 Fe C10 C11 75.90(14) . . . . ? C5 Fe C10 C11 153.96(12) . . . . ? C12 Fe C10 C11 -37.82(12) . . . . ? C13 Fe C10 C11 -81.47(12) . . . . ? C3 Fe C10 C11 60.3(3) . . . . ? C4 Fe C10 C11 174.43(17) . . . . ? C14 Fe C10 C11 -120.43(15) . . . . ? Li1 Fe C10 C11 -153.70(13) 2_565 . . . ? C1 Fe C10 C14 -125.25(11) . . . . ? C2 Fe C10 C14 -163.67(11) . . . . ? C11 Fe C10 C14 120.43(15) . . . . ? C5 Fe C10 C14 -85.61(12) . . . . ? C12 Fe C10 C14 82.60(12) . . . . ? C13 Fe C10 C14 38.96(11) . . . . ? C3 Fe C10 C14 -179.3(2) . . . . ? C4 Fe C10 C14 -65.1(2) . . . . ? Li1 Fe C10 C14 -33.27(12) 2_565 . . . ? C1 Fe C10 C9 -6.59(17) . . . . ? C2 Fe C10 C9 -45.02(19) . . . . ? C11 Fe C10 C9 -120.9(2) . . . . ? C5 Fe C10 C9 33.04(19) . . . . ? C12 Fe C10 C9 -158.74(18) . . . . ? C13 Fe C10 C9 157.62(18) . . . . ? C3 Fe C10 C9 -60.7(3) . . . . ? C4 Fe C10 C9 53.5(3) . . . . ? C14 Fe C10 C9 118.7(2) . . . . ? Li1 Fe C10 C9 85.39(17) 2_565 . . . ? C1 Fe C10 Li1 -88.82(12) . . . . ? C2 Fe C10 Li1 -127.25(12) . . . . ? C11 Fe C10 Li1 156.85(16) . . . . ? C5 Fe C10 Li1 -49.19(13) . . . . ? C12 Fe C10 Li1 119.03(12) . . . . ? C13 Fe C10 Li1 75.38(12) . . . . ? C3 Fe C10 Li1 -142.9(2) . . . . ? C4 Fe C10 Li1 -28.7(2) . . . . ? C14 Fe C10 Li1 36.42(12) . . . . ? Li1 Fe C10 Li1 3.15(16) 2_565 . . . ? N1 Li1 C10 C11 -124.9(4) . . . . ? C14 Li1 C10 C11 107.5(4) 2_565 . . . ? C14 Li1 C10 C11 37.4(4) . . . . ? Li1 Li1 C10 C11 80.2(4) 2_565 . . . ? C5 Li1 C10 C11 -33.0(5) 2_565 . . . ? C9 Li1 C10 C11 -154.7(4) . . . . ? Fe Li1 C10 C11 63.5(11) 2_565 . . . ? N1 Li1 C10 C14 -162.22(19) . . . . ? C14 Li1 C10 C14 70.2(2) 2_565 . . . ? Li1 Li1 C10 C14 42.81(16) 2_565 . . . ? C5 Li1 C10 C14 -70.4(2) 2_565 . . . ? C9 Li1 C10 C14 167.92(19) . . . . ? Fe Li1 C10 C14 26.1(9) 2_565 . . . ? N1 Li1 C10 C9 29.86(11) . . . . ? C14 Li1 C10 C9 -97.7(2) 2_565 . . . ? C14 Li1 C10 C9 -167.92(19) . . . . ? Li1 Li1 C10 C9 -125.1(2) 2_565 . . . ? C5 Li1 C10 C9 121.7(2) 2_565 . . . ? Fe Li1 C10 C9 -141.8(10) 2_565 . . . ? N1 Li1 C10 Fe 151.13(11) . . . . ? C14 Li1 C10 Fe 23.5(2) 2_565 . . . ? C14 Li1 C10 Fe -46.65(13) . . . . ? Li1 Li1 C10 Fe -3.84(19) 2_565 . . . ? C5 Li1 C10 Fe -117.0(2) 2_565 . . . ? C9 Li1 C10 Fe 121.27(13) . . . . ? Fe Li1 C10 Fe -20.5(10) 2_565 . . . ? C14 C10 C11 C12 -2.0(2) . . . . ? C9 C10 C11 C12 178.09(17) . . . . ? Fe C10 C11 C12 59.53(14) . . . . ? Li1 C10 C11 C12 -32.4(5) . . . . ? C14 C10 C11 Fe -61.55(13) . . . . ? C9 C10 C11 Fe 118.56(18) . . . . ? Li1 C10 C11 Fe -91.9(4) . . . . ? C1 Fe C11 C12 164.35(12) . . . . ? C10 Fe C11 C12 -118.86(17) . . . . ? C2 Fe C11 C12 122.02(13) . . . . ? C5 Fe C11 C12 -169.16(15) . . . . ? C13 Fe C11 C12 -38.11(12) . . . . ? C3 Fe C11 C12 84.26(15) . . . . ? C4 Fe C11 C12 70.6(3) . . . . ? C14 Fe C11 C12 -81.57(12) . . . . ? Li1 Fe C11 C12 -89.85(14) 2_565 . . . ? C1 Fe C11 C10 -76.78(13) . . . . ? C2 Fe C11 C10 -119.12(12) . . . . ? C5 Fe C11 C10 -50.3(2) . . . . ? C12 Fe C11 C10 118.86(17) . . . . ? C13 Fe C11 C10 80.75(12) . . . . ? C3 Fe C11 C10 -156.88(11) . . . . ? C4 Fe C11 C10 -170.5(3) . . . . ? C14 Fe C11 C10 37.29(11) . . . . ? Li1 Fe C11 C10 29.01(14) 2_565 . . . ? C10 C11 C12 C13 1.6(2) . . . . ? Fe C11 C12 C13 60.19(14) . . . . ? C10 C11 C12 Fe -58.59(13) . . . . ? C1 Fe C12 C13 -148.36(15) . . . . ? C10 Fe C12 C13 -79.73(12) . . . . ? C2 Fe C12 C13 168.77(12) . . . . ? C11 Fe C12 C13 -118.16(17) . . . . ? C5 Fe C12 C13 32.8(4) . . . . ? C3 Fe C12 C13 123.63(13) . . . . ? C4 Fe C12 C13 81.49(16) . . . . ? C14 Fe C12 C13 -35.40(11) . . . . ? Li1 Fe C12 C13 -10.22(14) 2_565 . . . ? C1 Fe C12 C11 -30.2(2) . . . . ? C10 Fe C12 C11 38.42(11) . . . . ? C2 Fe C12 C11 -73.08(14) . . . . ? C5 Fe C12 C11 151.0(4) . . . . ? C13 Fe C12 C11 118.16(17) . . . . ? C3 Fe C12 C11 -118.22(13) . . . . ? C4 Fe C12 C11 -160.35(13) . . . . ? C14 Fe C12 C11 82.75(12) . . . . ? Li1 Fe C12 C11 107.94(13) 2_565 . . . ? C11 C12 C13 C14 -0.6(2) . . . . ? Fe C12 C13 C14 58.91(14) . . . . ? C11 C12 C13 Fe -59.55(14) . . . . ? C1 Fe C13 C12 132.8(2) . . . . ? C10 Fe C13 C12 83.47(12) . . . . ? C2 Fe C13 C12 -27.7(3) . . . . ? C11 Fe C13 C12 38.47(12) . . . . ? C5 Fe C13 C12 -171.91(12) . . . . ? C3 Fe C13 C12 -79.49(16) . . . . ? C4 Fe C13 C12 -125.37(13) . . . . ? C14 Fe C13 C12 123.24(17) . . . . ? Li1 Fe C13 C12 169.72(14) 2_565 . . . ? C1 Fe C13 C14 9.6(3) . . . . ? C10 Fe C13 C14 -39.77(11) . . . . ? C2 Fe C13 C14 -150.9(2) . . . . ? C11 Fe C13 C14 -84.77(12) . . . . ? C5 Fe C13 C14 64.86(15) . . . . ? C12 Fe C13 C14 -123.24(17) . . . . ? C3 Fe C13 C14 157.27(13) . . . . ? C4 Fe C13 C14 111.39(13) . . . . ? Li1 Fe C13 C14 46.48(12) 2_565 . . . ? C12 C13 C14 C10 -0.6(2) . . . . ? Fe C13 C14 C10 57.09(12) . . . . ? C12 C13 C14 Fe -57.65(14) . . . . ? C12 C13 C14 Li1 -135.89(17) . . . 2_565 ? Fe C13 C14 Li1 -78.24(13) . . . 2_565 ? C12 C13 C14 Li1 147.0(4) . . . . ? Fe C13 C14 Li1 -155.3(4) . . . . ? C11 C10 C14 C13 1.6(2) . . . . ? C9 C10 C14 C13 -178.54(16) . . . . ? Fe C10 C14 C13 -58.36(12) . . . . ? Li1 C10 C14 C13 167.64(19) . . . . ? C11 C10 C14 Fe 59.93(13) . . . . ? C9 C10 C14 Fe -120.17(17) . . . . ? Li1 C10 C14 Fe -134.00(12) . . . . ? C11 C10 C14 Li1 125.81(19) . . . 2_565 ? C9 C10 C14 Li1 -54.3(3) . . . 2_565 ? Fe C10 C14 Li1 65.87(17) . . . 2_565 ? Li1 C10 C14 Li1 -68.1(2) . . . 2_565 ? C11 C10 C14 Li1 -166.07(16) . . . . ? C9 C10 C14 Li1 13.8(2) . . . . ? Fe C10 C14 Li1 134.00(13) . . . . ? C1 Fe C14 C13 -176.13(12) . . . . ? C10 Fe C14 C13 116.42(16) . . . . ? C2 Fe C14 C13 154.1(2) . . . . ? C11 Fe C14 C13 78.99(13) . . . . ? C5 Fe C14 C13 -133.48(13) . . . . ? C12 Fe C14 C13 35.37(12) . . . . ? C3 Fe C14 C13 -64.3(3) . . . . ? C4 Fe C14 C13 -92.55(14) . . . . ? Li1 Fe C14 C13 -111.22(16) 2_565 . . . ? C1 Fe C14 C10 67.45(13) . . . . ? C2 Fe C14 C10 37.7(3) . . . . ? C11 Fe C14 C10 -37.43(11) . . . . ? C5 Fe C14 C10 110.10(11) . . . . ? C12 Fe C14 C10 -81.05(12) . . . . ? C13 Fe C14 C10 -116.42(16) . . . . ? C3 Fe C14 C10 179.2(2) . . . . ? C4 Fe C14 C10 151.04(11) . . . . ? Li1 Fe C14 C10 132.36(15) 2_565 . . . ? C1 Fe C14 Li1 -64.91(13) . . . 2_565 ? C10 Fe C14 Li1 -132.36(15) . . . 2_565 ? C2 Fe C14 Li1 -94.6(2) . . . 2_565 ? C11 Fe C14 Li1 -169.79(13) . . . 2_565 ? C5 Fe C14 Li1 -22.26(13) . . . 2_565 ? C12 Fe C14 Li1 146.59(13) . . . 2_565 ? C13 Fe C14 Li1 111.22(16) . . . 2_565 ? C3 Fe C14 Li1 46.9(3) . . . 2_565 ? C4 Fe C14 Li1 18.68(14) . . . 2_565 ? C1 Fe C14 Li1 -9.2(2) . . . . ? C10 Fe C14 Li1 -76.61(19) . . . . ? C2 Fe C14 Li1 -38.9(3) . . . . ? C11 Fe C14 Li1 -114.04(19) . . . . ? C5 Fe C14 Li1 33.5(2) . . . . ? C12 Fe C14 Li1 -157.7(2) . . . . ? C13 Fe C14 Li1 167.0(2) . . . . ? C3 Fe C14 Li1 102.6(3) . . . . ? C4 Fe C14 Li1 74.4(2) . . . . ? Li1 Fe C14 Li1 55.8(2) 2_565 . . . ? N1 Li1 C14 C13 -133.2(4) . . . . ? C14 Li1 C14 C13 85.6(5) 2_565 . . . ? Li1 Li1 C14 C13 85.6(5) 2_565 . . . ? C5 Li1 C14 C13 -14.9(5) 2_565 . . . ? C9 Li1 C14 C13 -155.4(4) . . . . ? C10 Li1 C14 C13 -148.2(5) . . . . ? Fe Li1 C14 C13 37.8(6) 2_565 . . . ? N1 Li1 C14 C10 15.09(16) . . . . ? C14 Li1 C14 C10 -126.18(18) 2_565 . . . ? Li1 Li1 C14 C10 -126.18(18) 2_565 . . . ? C5 Li1 C14 C10 133.32(17) 2_565 . . . ? C9 Li1 C14 C10 -7.16(11) . . . . ? Fe Li1 C14 C10 -173.9(2) 2_565 . . . ? N1 Li1 C14 Fe 78.64(19) . . . . ? C14 Li1 C14 Fe -62.6(2) 2_565 . . . ? Li1 Li1 C14 Fe -62.6(2) 2_565 . . . ? C5 Li1 C14 Fe -163.13(13) 2_565 . . . ? C9 Li1 C14 Fe 56.39(16) . . . . ? C10 Li1 C14 Fe 63.55(15) . . . . ? Fe Li1 C14 Fe -110.4(2) 2_565 . . . ? N1 Li1 C14 Li1 141.3(2) . . . 2_565 ? C14 Li1 C14 Li1 0.0 2_565 . . 2_565 ? C5 Li1 C14 Li1 -100.5(2) 2_565 . . 2_565 ? C9 Li1 C14 Li1 119.01(17) . . . 2_565 ? C10 Li1 C14 Li1 126.18(18) . . . 2_565 ? Fe Li1 C14 Li1 -47.76(18) 2_565 . . 2_565 ? C10 C9 N1 C16 -62.93(19) . . . . ? C8 C9 N1 C16 172.68(16) . . . . ? Li1 C9 N1 C16 -114.28(18) . . . . ? C10 C9 N1 C15 176.80(17) . . . . ? C8 C9 N1 C15 52.4(2) . . . . ? Li1 C9 N1 C15 125.5(2) . . . . ? C10 C9 N1 Li1 51.35(18) . . . . ? C8 C9 N1 Li1 -73.04(18) . . . . ? C14 Li1 N1 C16 -162.8(2) 2_565 . . . ? C14 Li1 N1 C16 75.50(17) . . . . ? Li1 Li1 N1 C16 116.8(3) 2_565 . . . ? C5 Li1 N1 C16 -49.0(2) 2_565 . . . ? C9 Li1 N1 C16 113.90(17) . . . . ? C10 Li1 N1 C16 84.78(14) . . . . ? Fe Li1 N1 C16 -96.9(2) 2_565 . . . ? C14 Li1 N1 C15 -38.3(3) 2_565 . . . ? C14 Li1 N1 C15 -159.99(16) . . . . ? Li1 Li1 N1 C15 -118.7(3) 2_565 . . . ? C5 Li1 N1 C15 75.5(2) 2_565 . . . ? C9 Li1 N1 C15 -121.6(2) . . . . ? C10 Li1 N1 C15 -150.71(17) . . . . ? Fe Li1 N1 C15 27.6(3) 2_565 . . . ? C14 Li1 N1 C9 83.2(3) 2_565 . . . ? C14 Li1 N1 C9 -38.41(15) . . . . ? Li1 Li1 N1 C9 2.9(3) 2_565 . . . ? C5 Li1 N1 C9 -162.87(15) 2_565 . . . ? C10 Li1 N1 C9 -29.13(10) . . . . ? Fe Li1 N1 C9 149.19(18) 2_565 . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.458 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.065