# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'U. Siemeling' _publ_contact_author_email SIEMELING@UNI-KASSEL.DE _publ_section_title ; A stable crystalline N-heterocyclic carbene with a 1,1'-ferrocenediyl backbone ; loop_ _publ_author_name 'U. Siemeling' 'Clemens Bruhn' 'Christian Farber' # Attachment 'B813809Erevised1.cif' data_i0450a _database_code_depnum_ccdc_archive 'CCDC 697881' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H39 Fe N2, C H2 Cl2, B F4' _chemical_formula_sum 'C32 H41 B Cl2 F4 Fe N2' _chemical_formula_weight 667.23 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.9008(12) _cell_length_b 18.7777(19) _cell_length_c 10.3761(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.019(13) _cell_angle_gamma 90.00 _cell_volume 1539.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8088 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 25.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 32 _diffrn_source_power 1.60 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 223(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 10075 _diffrn_reflns_av_R_equivalents 0.1268 _diffrn_reflns_av_sigmaI/netI 0.1806 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2819 _reflns_number_gt 1381 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+0.0000P] 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 2819 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 C1 C 0.3204(8) 0.2500 0.5995(6) 0.0298(17) Uani 1 2 d S . . H1A H 0.3448 0.2500 0.6882 0.036 Uiso 1 2 calc SR . . C2 C 0.2808(6) 0.1729(3) 0.4120(4) 0.0265(11) Uani 1 1 d . . . C3 C 0.4090(7) 0.1658(3) 0.3173(4) 0.0336(13) Uani 1 1 d . . . H3A H 0.5262 0.1669 0.3328 0.040 Uiso 1 1 calc R . . C4 C 0.3307(7) 0.1568(3) 0.1955(4) 0.0331(13) Uani 1 1 d . . . H4A H 0.3874 0.1519 0.1163 0.040 Uiso 1 1 calc R . . C5 C 0.1519(6) 0.1566(3) 0.2130(4) 0.0309(13) Uani 1 1 d . . . H5A H 0.0710 0.1516 0.1472 0.037 Uiso 1 1 calc R . . C6 C 0.1158(6) 0.1651(3) 0.3466(4) 0.0305(12) Uani 1 1 d . . . H6A H 0.0083 0.1656 0.3854 0.037 Uiso 1 1 calc R . . C7 C 0.3614(6) 0.1190(3) 0.6232(4) 0.0315(13) Uani 1 1 d . . . H7A H 0.4775 0.1066 0.5950 0.038 Uiso 1 1 calc R . . C8 C 0.2465(6) 0.0561(3) 0.5905(5) 0.0313(12) Uani 1 1 d . . . H8A H 0.2392 0.0507 0.4957 0.038 Uiso 1 1 calc R . . C9 C 0.3243(7) -0.0119(3) 0.6496(5) 0.0384(14) Uani 1 1 d . . . H9B H 0.4372 -0.0200 0.6132 0.046 Uiso 1 1 calc R . . H9A H 0.2535 -0.0531 0.6284 0.046 Uiso 1 1 calc R . . C10 C 0.3375(6) -0.0040(3) 0.7975(5) 0.0344(13) Uani 1 1 d . . . H10A H 0.3899 -0.0472 0.8350 0.041 Uiso 1 1 calc R . . C11 C 0.4477(7) 0.0619(3) 0.8280(5) 0.0377(14) Uani 1 1 d . . . H11B H 0.4600 0.0669 0.9216 0.045 Uiso 1 1 calc R . . H11A H 0.5607 0.0556 0.7908 0.045 Uiso 1 1 calc R . . C12 C 0.3653(6) 0.1292(3) 0.7722(4) 0.0285(12) Uani 1 1 d . . . H12A H 0.4356 0.1712 0.7938 0.034 Uiso 1 1 calc R . . C13 C 0.0705(7) 0.0662(3) 0.6453(5) 0.0421(14) Uani 1 1 d . . . H13A H -0.0009 0.0256 0.6215 0.050 Uiso 1 1 calc R . . H13B H 0.0197 0.1094 0.6090 0.050 Uiso 1 1 calc R . . C14 C 0.1900(7) 0.1392(3) 0.8257(5) 0.0382(14) Uani 1 1 d . . . H14A H 0.1383 0.1817 0.7876 0.046 Uiso 1 1 calc R . . H14B H 0.1962 0.1462 0.9192 0.046 Uiso 1 1 calc R . . C15 C 0.1611(7) 0.0059(3) 0.8518(5) 0.0451(15) Uani 1 1 d . . . H15A H 0.1674 0.0102 0.9458 0.054 Uiso 1 1 calc R . . H15B H 0.0918 -0.0359 0.8313 0.054 Uiso 1 1 calc R . . C16 C 0.0785(7) 0.0727(3) 0.7954(5) 0.0368(13) Uani 1 1 d . . . H16A H -0.0366 0.0790 0.8313 0.044 Uiso 1 1 calc R . . C17 C -0.1608(10) 0.2500 0.9621(7) 0.042(2) Uani 1 2 d S . . H17A H -0.0412 0.2500 0.9872 0.051 Uiso 1 2 calc SR . . H17B H -0.1659 0.2500 0.8678 0.051 Uiso 1 2 calc SR . . B B -0.2261(10) 0.2500 0.5803(8) 0.033(2) Uani 1 2 d S . . N N 0.3061(5) 0.1855(2) 0.5476(3) 0.0307(10) Uani 1 1 d . . . F1 F -0.3343(6) 0.2500 0.6858(4) 0.0668(15) Uani 1 2 d S . . F2 F -0.2601(4) 0.18943(19) 0.5063(3) 0.0659(11) Uani 1 1 d . . . F3 F -0.0606(5) 0.2500 0.6210(4) 0.0454(11) Uani 1 2 d S . . Cl Cl -0.2561(2) 0.17219(9) 1.01985(17) 0.0636(5) Uani 1 1 d . . . Fe Fe 0.25513(13) 0.2500 0.28469(10) 0.0244(3) Uani 1 2 d S . . 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 C1 0.030(4) 0.036(5) 0.024(4) 0.000 0.003(3) 0.000 C2 0.034(3) 0.025(3) 0.021(3) -0.001(2) -0.001(2) -0.003(2) C3 0.037(3) 0.023(3) 0.041(3) -0.004(2) -0.005(2) 0.009(3) C4 0.034(3) 0.037(4) 0.029(3) -0.009(2) -0.002(2) 0.006(3) C5 0.041(3) 0.029(3) 0.023(3) -0.004(2) -0.011(2) -0.006(3) C6 0.031(3) 0.023(3) 0.037(3) 0.001(2) -0.001(2) -0.010(2) C7 0.032(3) 0.024(3) 0.038(3) 0.005(2) -0.002(2) 0.003(2) C8 0.039(3) 0.021(3) 0.034(3) 0.002(2) -0.004(2) -0.002(3) C9 0.052(4) 0.022(3) 0.041(3) 0.000(2) 0.002(3) -0.003(3) C10 0.034(3) 0.029(3) 0.040(3) 0.007(2) -0.004(2) 0.006(3) C11 0.043(3) 0.033(3) 0.037(3) 0.001(2) -0.004(2) 0.005(3) C12 0.030(3) 0.023(3) 0.032(3) 0.001(2) -0.005(2) -0.006(2) C13 0.039(3) 0.038(4) 0.049(4) 0.001(3) -0.014(3) -0.010(3) C14 0.052(4) 0.029(4) 0.034(3) 0.001(2) 0.005(3) 0.009(3) C15 0.054(4) 0.035(4) 0.046(3) 0.010(3) 0.004(3) -0.003(3) C16 0.033(3) 0.035(4) 0.043(3) 0.003(3) 0.002(2) 0.001(3) C17 0.044(5) 0.043(6) 0.040(5) 0.000 -0.001(4) 0.000 B 0.013(4) 0.039(6) 0.047(5) 0.000 0.002(4) 0.000 N 0.038(2) 0.024(3) 0.030(2) -0.0013(19) -0.0055(18) 0.004(2) F1 0.042(3) 0.103(4) 0.056(3) 0.000 0.006(2) 0.000 F2 0.0369(19) 0.069(3) 0.092(3) -0.031(2) -0.0153(17) -0.0020(19) F3 0.029(2) 0.045(3) 0.062(3) 0.000 -0.014(2) 0.000 Cl 0.0461(9) 0.0414(10) 0.1031(13) 0.0163(9) -0.0122(9) -0.0100(8) Fe 0.0249(6) 0.0248(7) 0.0234(5) 0.000 -0.0049(4) 0.000 _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 C1 N 1.331(5) . ? C1 N 1.331(5) 4_565 ? C1 H1A 0.9400 . ? C2 C3 1.418(6) . ? C2 N 1.440(5) . ? C2 C6 1.477(6) . ? C2 Fe 1.971(5) . ? C3 C4 1.417(6) . ? C3 Fe 2.023(5) . ? C3 H3A 0.9400 . ? C4 C5 1.425(6) . ? C4 Fe 2.068(5) . ? C4 H4A 0.9400 . ? C5 C6 1.424(6) . ? C5 Fe 2.073(5) . ? C5 H5A 0.9400 . ? C6 Fe 2.042(5) . ? C6 H6A 0.9400 . ? C7 C8 1.528(6) . ? C7 N 1.538(6) . ? C7 C12 1.559(6) . ? C7 H7A 0.9900 . ? C8 C13 1.515(7) . ? C8 C9 1.544(7) . ? C8 H8A 0.9900 . ? C9 C10 1.545(6) . ? C9 H9B 0.9800 . ? C9 H9A 0.9800 . ? C10 C15 1.515(7) . ? C10 C11 1.546(7) . ? C10 H10A 0.9900 . ? C11 C12 1.535(7) . ? C11 H11B 0.9800 . ? C11 H11A 0.9800 . ? C12 C14 1.505(6) . ? C12 H12A 0.9900 . ? C13 C16 1.563(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C16 1.560(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.530(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9900 . ? C17 Cl 1.750(4) 4_565 ? C17 Cl 1.750(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? B F3 1.374(8) . ? B F1 1.389(9) . ? B F2 1.398(6) . ? B F2 1.398(6) 4_565 ? Fe C2 1.971(5) 4_565 ? Fe C3 2.023(5) 4_565 ? Fe C6 2.042(5) 4_565 ? Fe C4 2.068(5) 4_565 ? Fe C5 2.073(5) 4_565 ? 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 N C1 N 131.1(6) . 4_565 ? N C1 H1A 114.4 . . ? N C1 H1A 114.4 4_565 . ? C3 C2 N 126.4(4) . . ? C3 C2 C6 107.6(4) . . ? N C2 C6 126.0(4) . . ? C3 C2 Fe 71.2(3) . . ? N C2 Fe 123.3(3) . . ? C6 C2 Fe 71.0(3) . . ? C4 C3 C2 108.5(4) . . ? C4 C3 Fe 71.4(3) . . ? C2 C3 Fe 67.3(3) . . ? C4 C3 H3A 125.7 . . ? C2 C3 H3A 125.7 . . ? Fe C3 H3A 127.1 . . ? C3 C4 C5 108.6(4) . . ? C3 C4 Fe 68.0(3) . . ? C5 C4 Fe 70.1(3) . . ? C3 C4 H4A 125.7 . . ? C5 C4 H4A 125.7 . . ? Fe C4 H4A 127.8 . . ? C6 C5 C4 108.8(4) . . ? C6 C5 Fe 68.6(3) . . ? C4 C5 Fe 69.7(3) . . ? C6 C5 H5A 125.6 . . ? C4 C5 H5A 125.6 . . ? Fe C5 H5A 127.7 . . ? C5 C6 C2 106.4(4) . . ? C5 C6 Fe 70.9(3) . . ? C2 C6 Fe 65.9(3) . . ? C5 C6 H6A 126.8 . . ? C2 C6 H6A 126.8 . . ? Fe C6 H6A 127.9 . . ? C8 C7 N 110.2(4) . . ? C8 C7 C12 109.1(4) . . ? N C7 C12 114.3(4) . . ? C8 C7 H7A 107.7 . . ? N C7 H7A 107.7 . . ? C12 C7 H7A 107.7 . . ? C13 C8 C7 111.4(4) . . ? C13 C8 C9 108.7(4) . . ? C7 C8 C9 108.3(4) . . ? C13 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C8 C9 C10 109.9(4) . . ? C8 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? H9B C9 H9A 108.2 . . ? C15 C10 C9 108.7(4) . . ? C15 C10 C11 110.1(4) . . ? C9 C10 C11 108.6(4) . . ? C15 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? C11 C10 H10A 109.8 . . ? C12 C11 C10 110.1(4) . . ? C12 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? C12 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? H11B C11 H11A 108.2 . . ? C14 C12 C11 110.7(4) . . ? C14 C12 C7 111.3(4) . . ? C11 C12 C7 106.3(4) . . ? C14 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C7 C12 H12A 109.5 . . ? C8 C13 C16 110.3(4) . . ? C8 C13 H13A 109.6 . . ? C16 C13 H13A 109.6 . . ? C8 C13 H13B 109.6 . . ? C16 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C12 C14 C16 110.2(4) . . ? C12 C14 H14A 109.6 . . ? C16 C14 H14A 109.6 . . ? C12 C14 H14B 109.6 . . ? C16 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C10 C15 C16 110.5(4) . . ? C10 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 C14 109.8(4) . . ? C15 C16 C13 109.5(4) . . ? C14 C16 C13 106.6(4) . . ? C15 C16 H16A 110.3 . . ? C14 C16 H16A 110.3 . . ? C13 C16 H16A 110.3 . . ? Cl C17 Cl 113.2(4) 4_565 . ? Cl C17 H17A 108.9 4_565 . ? Cl C17 H17A 108.9 . . ? Cl C17 H17B 108.9 4_565 . ? Cl C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? F3 B F1 110.1(6) . . ? F3 B F2 110.6(4) . . ? F1 B F2 108.4(4) . . ? F3 B F2 110.6(4) . 4_565 ? F1 B F2 108.4(4) . 4_565 ? F2 B F2 108.8(7) . 4_565 ? C1 N C2 123.8(4) . . ? C1 N C7 120.6(4) . . ? C2 N C7 113.9(4) . . ? C2 Fe C2 94.6(3) 4_565 . ? C2 Fe C3 41.56(19) 4_565 4_565 ? C2 Fe C3 113.59(19) . 4_565 ? C2 Fe C3 113.59(19) 4_565 . ? C2 Fe C3 41.56(19) . . ? C3 Fe C3 102.8(3) 4_565 . ? C2 Fe C6 114.74(19) 4_565 . ? C2 Fe C6 43.17(18) . . ? C3 Fe C6 151.88(18) 4_565 . ? C3 Fe C6 70.2(2) . . ? C2 Fe C6 43.17(18) 4_565 4_565 ? C2 Fe C6 114.74(19) . 4_565 ? C3 Fe C6 70.2(2) 4_565 4_565 ? C3 Fe C6 151.88(18) . 4_565 ? C6 Fe C6 102.7(3) . 4_565 ? C2 Fe C4 153.15(18) 4_565 . ? C2 Fe C4 69.44(19) . . ? C3 Fe C4 124.2(2) 4_565 . ? C3 Fe C4 40.53(17) . . ? C6 Fe C4 68.6(2) . . ? C6 Fe C4 163.28(18) 4_565 . ? C2 Fe C4 69.44(19) 4_565 4_565 ? C2 Fe C4 153.15(19) . 4_565 ? C3 Fe C4 40.53(17) 4_565 4_565 ? C3 Fe C4 124.2(2) . 4_565 ? C6 Fe C4 163.28(18) . 4_565 ? C6 Fe C4 68.6(2) 4_565 4_565 ? C4 Fe C4 115.6(3) . 4_565 ? C2 Fe C5 154.55(18) 4_565 . ? C2 Fe C5 70.07(18) . . ? C3 Fe C5 163.3(2) 4_565 . ? C3 Fe C5 68.59(19) . . ? C6 Fe C5 40.49(17) . . ? C6 Fe C5 124.2(2) 4_565 . ? C4 Fe C5 40.25(17) . . ? C4 Fe C5 132.01(19) 4_565 . ? C2 Fe C5 70.07(18) 4_565 4_565 ? C2 Fe C5 154.55(18) . 4_565 ? C3 Fe C5 68.59(19) 4_565 4_565 ? C3 Fe C5 163.3(2) . 4_565 ? C6 Fe C5 124.2(2) . 4_565 ? C6 Fe C5 40.49(17) 4_565 4_565 ? C4 Fe C5 132.01(19) . 4_565 ? C4 Fe C5 40.25(17) 4_565 4_565 ? C5 Fe C5 115.7(3) . 4_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.389 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.067 #============================================================================ data_i0480 _database_code_depnum_ccdc_archive 'CCDC 697882' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H50 Cl Fe N2 Rh' _chemical_formula_sum 'C39 H50 Cl Fe N2 Rh' _chemical_formula_weight 741.02 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C c m 21' _symmetry_space_group_name_Hall 'C 2c -2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z+1/2' 'x, -y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 12.8330(12) _cell_length_b 20.430(2) _cell_length_c 12.3078(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3226.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5695 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.076 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6727 _exptl_absorpt_correction_T_max 0.8832 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 173(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 10266 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1546 _reflns_number_gt 1204 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The displacement ellipsoid of C9 is notably elongated orthogonally to its C-C bond axes, which might indicate a minor disorder problem. ; _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^)+(0.0240P)^2^+0.0000P] 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_abs_structure_details # 'Flack H D (1983), Acta Cryst. A39, 876-881' # _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 1546 _refine_ls_number_parameters 205 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _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 C1 C 0.7978(7) 0.0000 0.2623(8) 0.030(2) Uani 1 2 d S . . C2 C 0.7160(5) -0.0696(3) 0.1164(6) 0.0295(15) Uani 1 1 d . . . C3 C 0.6056(5) -0.0793(3) 0.1144(6) 0.0367(18) Uani 1 1 d . . . H3A H 0.5608 -0.0804 0.1759 0.044 Uiso 1 1 calc R . . C4 C 0.5747(5) -0.0871(4) 0.0041(6) 0.0382(19) Uani 1 1 d . . . H4A H 0.5054 -0.0930 -0.0211 0.046 Uiso 1 1 calc R . . C5 C 0.6644(5) -0.0845(3) -0.0612(6) 0.0365(17) Uani 1 1 d . . . H5A H 0.6657 -0.0886 -0.1380 0.044 Uiso 1 1 calc R . . C6 C 0.7532(5) -0.0747(3) 0.0065(6) 0.0321(16) Uani 1 1 d . . . H6A H 0.8237 -0.0721 -0.0166 0.039 Uiso 1 1 calc R . . C7 C 0.7007(5) -0.0344(3) 0.4756(5) 0.0356(16) Uani 1 1 d . . . H7A H 0.6960 -0.0565 0.4079 0.043 Uiso 1 1 calc R . . C8 C 0.7078(6) -0.0750(4) 0.5785(6) 0.0407(18) Uani 1 1 d . . . H8B H 0.6532 -0.0598 0.6294 0.049 Uiso 1 1 calc R . . H8A H 0.6916 -0.1210 0.5598 0.049 Uiso 1 1 calc R . . C9 C 0.8089(7) -0.0738(6) 0.6362(8) 0.081(4) Uani 1 1 d . . . H9B H 0.8345 -0.1194 0.6420 0.097 Uiso 1 1 calc R . . H9A H 0.7964 -0.0578 0.7110 0.097 Uiso 1 1 calc R . . C10 C 0.8936(5) -0.0333(3) 0.5873(5) 0.0387(18) Uani 1 1 d . . . H10A H 0.9507 -0.0553 0.5544 0.046 Uiso 1 1 calc R . . C11 C 0.8180(4) -0.1189(3) 0.2701(5) 0.0287(15) Uani 1 1 d . . . H11A H 0.8240 -0.1058 0.3481 0.034 Uiso 1 1 calc R . . C12 C 0.9298(5) -0.1398(3) 0.2366(5) 0.0302(16) Uani 1 1 d . . . H12A H 0.9744 -0.0999 0.2294 0.036 Uiso 1 1 calc R . . C13 C 0.9311(5) -0.1773(3) 0.1301(6) 0.0368(17) Uani 1 1 d . . . H13A H 1.0038 -0.1887 0.1109 0.044 Uiso 1 1 calc R . . H13B H 0.9024 -0.1495 0.0715 0.044 Uiso 1 1 calc R . . C14 C 0.8658(6) -0.2401(3) 0.1403(5) 0.0385(19) Uani 1 1 d . . . H14A H 0.8686 -0.2653 0.0707 0.046 Uiso 1 1 calc R . . C15 C 0.7520(6) -0.2194(4) 0.1647(6) 0.0386(17) Uani 1 1 d . . . H15A H 0.7248 -0.1926 0.1039 0.046 Uiso 1 1 calc R . . H15B H 0.7076 -0.2588 0.1715 0.046 Uiso 1 1 calc R . . C16 C 0.7475(5) -0.1797(3) 0.2707(5) 0.0323(16) Uani 1 1 d . . . H16A H 0.6740 -0.1666 0.2865 0.039 Uiso 1 1 calc R . . C17 C 0.9077(6) -0.2822(4) 0.2334(6) 0.0454(19) Uani 1 1 d . . . H17A H 0.9807 -0.2950 0.2179 0.054 Uiso 1 1 calc R . . H17B H 0.8657 -0.3226 0.2398 0.054 Uiso 1 1 calc R . . C18 C 0.9718(5) -0.1824(3) 0.3291(6) 0.0358(17) Uani 1 1 d . . . H18A H 0.9712 -0.1572 0.3979 0.043 Uiso 1 1 calc R . . H18B H 1.0446 -0.1953 0.3133 0.043 Uiso 1 1 calc R . . C19 C 0.7894(6) -0.2237(4) 0.3630(6) 0.0417(18) Uani 1 1 d . . . H19B H 0.7856 -0.1998 0.4329 0.050 Uiso 1 1 calc R . . H19A H 0.7455 -0.2634 0.3691 0.050 Uiso 1 1 calc R . . C20 C 0.9032(7) -0.2439(4) 0.3408(6) 0.0402(17) Uani 1 1 d . . . H20A H 0.9296 -0.2718 0.4016 0.048 Uiso 1 1 calc R . . N N 0.7764(4) -0.0585(2) 0.2127(5) 0.0230(14) Uani 1 1 d . . . Cl Cl 1.02846(17) 0.0000 0.37020(19) 0.0348(6) Uani 1 2 d S . . Fe Fe 0.65256(13) 0.0000 0.02833(9) 0.0323(4) Uani 1 2 d S . . Rh Rh 0.84939(6) 0.0000 0.42315(5) 0.02512(19) Uani 1 2 d S . . 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 C1 0.021(5) 0.031(6) 0.038(6) 0.000 0.008(4) 0.000 C2 0.024(4) 0.027(4) 0.037(4) -0.002(3) -0.005(3) -0.004(3) C3 0.031(4) 0.039(4) 0.040(4) 0.003(4) -0.001(3) -0.002(3) C4 0.029(4) 0.042(4) 0.044(5) -0.008(3) -0.010(3) -0.003(3) C5 0.050(4) 0.032(3) 0.027(5) 0.003(3) -0.007(4) -0.001(3) C6 0.033(4) 0.030(4) 0.034(4) 0.001(3) -0.006(3) -0.007(3) C7 0.030(4) 0.040(4) 0.037(4) -0.001(3) 0.009(3) 0.000(3) C8 0.041(4) 0.044(4) 0.037(4) 0.006(4) 0.007(4) -0.005(4) C9 0.054(6) 0.118(9) 0.071(7) 0.068(7) -0.014(5) -0.020(6) C10 0.036(4) 0.049(4) 0.031(4) 0.016(3) -0.004(3) -0.001(3) C11 0.028(4) 0.030(4) 0.029(4) -0.001(3) -0.001(3) -0.003(3) C12 0.026(4) 0.027(4) 0.037(4) -0.001(3) -0.003(3) 0.002(3) C13 0.035(4) 0.035(4) 0.041(4) 0.002(4) 0.005(3) 0.007(3) C14 0.049(5) 0.031(4) 0.036(4) -0.006(3) -0.002(3) 0.006(3) C15 0.046(5) 0.026(4) 0.044(4) 0.001(4) -0.008(4) -0.004(4) C16 0.035(4) 0.024(4) 0.038(4) 0.005(3) 0.004(4) -0.006(3) C17 0.060(5) 0.027(4) 0.049(5) 0.003(4) -0.006(4) 0.005(4) C18 0.035(4) 0.034(4) 0.039(4) 0.001(3) -0.008(3) 0.005(3) C19 0.049(5) 0.035(4) 0.042(4) 0.004(4) 0.008(4) -0.008(4) C20 0.054(4) 0.030(4) 0.037(3) 0.004(4) -0.010(4) 0.002(3) N 0.025(4) 0.019(3) 0.025(3) 0.002(3) 0.001(3) 0.003(2) Cl 0.0215(12) 0.0436(14) 0.0395(14) 0.000 0.0000(10) 0.000 Fe 0.0287(8) 0.0327(9) 0.0356(9) 0.000 -0.0057(8) 0.000 Rh 0.0232(4) 0.0252(4) 0.0269(4) 0.000 0.0004(6) 0.000 _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 C1 N 1.369(7) . ? C1 N 1.369(7) 4 ? C1 Rh 2.088(10) . ? C2 C3 1.432(9) . ? C2 N 1.434(9) . ? C2 C6 1.437(10) . ? C2 Fe 1.965(7) . ? C3 C4 1.423(10) . ? C3 Fe 2.028(7) . ? C3 H3A 0.9500 . ? C4 C5 1.405(10) . ? C4 Fe 2.062(7) . ? C4 H4A 0.9500 . ? C5 C6 1.425(9) . ? C5 Fe 2.053(6) . ? C5 H5A 0.9500 . ? C6 Fe 2.018(7) . ? C6 H6A 0.9500 . ? C7 C7 1.405(13) 4 ? C7 C8 1.517(9) . ? C7 Rh 2.133(6) . ? C7 H7A 0.9500 . ? C8 C9 1.479(11) . ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C9 C10 1.492(11) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 C10 1.363(14) 4 ? C10 Rh 2.207(6) . ? C10 H10A 0.9500 . ? C11 N 1.519(8) . ? C11 C16 1.536(9) . ? C11 C12 1.553(8) . ? C11 H11A 1.0000 . ? C12 C13 1.518(9) . ? C12 C18 1.530(9) . ? C12 H12A 1.0000 . ? C13 C14 1.538(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C17 1.531(9) . ? C14 C15 1.550(10) . ? C14 H14A 1.0000 . ? C15 C16 1.538(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C19 1.546(10) . ? C16 H16A 1.0000 . ? C17 C20 1.537(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.542(10) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.541(10) . ? C19 H19B 0.9900 . ? C19 H19A 0.9900 . ? C20 H20A 1.0000 . ? Cl Rh 2.389(2) . ? Fe C2 1.965(7) 4 ? Fe C6 2.018(7) 4 ? Fe C3 2.028(7) 4 ? Fe C5 2.053(6) 4 ? Fe C4 2.062(7) 4 ? Rh C7 2.133(6) 4 ? Rh C10 2.207(6) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N C1 N 121.5(9) . 4 ? N C1 Rh 119.1(4) . . ? N C1 Rh 119.1(4) 4 . ? C3 C2 N 124.8(7) . . ? C3 C2 C6 107.6(6) . . ? N C2 C6 127.6(6) . . ? C3 C2 Fe 71.4(4) . . ? N C2 Fe 124.4(4) . . ? C6 C2 Fe 70.8(4) . . ? C4 C3 C2 107.9(7) . . ? C4 C3 Fe 70.9(4) . . ? C2 C3 Fe 66.6(4) . . ? C4 C3 H3A 126.1 . . ? C2 C3 H3A 126.1 . . ? Fe C3 H3A 127.9 . . ? C5 C4 C3 108.3(6) . . ? C5 C4 Fe 69.7(4) . . ? C3 C4 Fe 68.4(4) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Fe C4 H4A 127.6 . . ? C4 C5 C6 109.0(7) . . ? C4 C5 Fe 70.4(4) . . ? C6 C5 Fe 68.2(4) . . ? C4 C5 H5A 125.5 . . ? C6 C5 H5A 125.5 . . ? Fe C5 H5A 127.5 . . ? C5 C6 C2 107.2(6) . . ? C5 C6 Fe 70.9(4) . . ? C2 C6 Fe 66.9(4) . . ? C5 C6 H6A 126.4 . . ? C2 C6 H6A 126.4 . . ? Fe C6 H6A 127.4 . . ? C7 C7 C8 123.2(4) 4 . ? C7 C7 Rh 70.78(18) 4 . ? C8 C7 Rh 112.3(4) . . ? C7 C7 H7A 118.4 4 . ? C8 C7 H7A 118.4 . . ? Rh C7 H7A 87.0 . . ? C9 C8 C7 116.3(6) . . ? C9 C8 H8B 108.2 . . ? C7 C8 H8B 108.2 . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8A 108.2 . . ? H8B C8 H8A 107.4 . . ? C8 C9 C10 117.1(7) . . ? C8 C9 H9B 108.0 . . ? C10 C9 H9B 108.0 . . ? C8 C9 H9A 108.0 . . ? C10 C9 H9A 108.0 . . ? H9B C9 H9A 107.3 . . ? C10 C10 C9 123.6(6) 4 . ? C10 C10 Rh 72.02(18) 4 . ? C9 C10 Rh 110.6(5) . . ? C10 C10 H10A 118.2 4 . ? C9 C10 H10A 118.2 . . ? Rh C10 H10A 87.3 . . ? N C11 C16 116.9(5) . . ? N C11 C12 115.2(5) . . ? C16 C11 C12 108.8(5) . . ? N C11 H11A 104.9 . . ? C16 C11 H11A 104.9 . . ? C12 C11 H11A 104.9 . . ? C13 C12 C18 110.6(6) . . ? C13 C12 C11 112.2(5) . . ? C18 C12 C11 106.5(6) . . ? C13 C12 H12A 109.1 . . ? C18 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C12 C13 C14 110.2(6) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C17 C14 C13 109.8(6) . . ? C17 C14 C15 109.9(6) . . ? C13 C14 C15 107.5(5) . . ? C17 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? C16 C15 C14 110.1(6) . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C11 C16 C15 113.6(5) . . ? C11 C16 C19 105.6(5) . . ? C15 C16 C19 107.6(5) . . ? C11 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? C19 C16 H16A 109.9 . . ? C14 C17 C20 110.1(6) . . ? C14 C17 H17A 109.6 . . ? C20 C17 H17A 109.6 . . ? C14 C17 H17B 109.6 . . ? C20 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C12 C18 C20 109.4(6) . . ? C12 C18 H18A 109.8 . . ? C20 C18 H18A 109.8 . . ? C12 C18 H18B 109.8 . . ? C20 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? C20 C19 C16 110.8(6) . . ? C20 C19 H19B 109.5 . . ? C16 C19 H19B 109.5 . . ? C20 C19 H19A 109.5 . . ? C16 C19 H19A 109.5 . . ? H19B C19 H19A 108.1 . . ? C17 C20 C19 109.0(6) . . ? C17 C20 C18 108.2(6) . . ? C19 C20 C18 109.8(6) . . ? C17 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? C18 C20 H20A 109.9 . . ? C1 N C2 127.9(6) . . ? C1 N C11 115.6(6) . . ? C2 N C11 116.4(5) . . ? C2 Fe C2 92.7(4) 4 . ? C2 Fe C6 42.3(3) 4 4 ? C2 Fe C6 110.8(3) . 4 ? C2 Fe C6 110.8(3) 4 . ? C2 Fe C6 42.3(3) . . ? C6 Fe C6 98.4(4) 4 . ? C2 Fe C3 42.0(3) 4 4 ? C2 Fe C3 114.4(3) . 4 ? C6 Fe C3 69.8(3) 4 4 ? C6 Fe C3 149.8(3) . 4 ? C2 Fe C3 114.4(3) 4 . ? C2 Fe C3 42.0(3) . . ? C6 Fe C3 149.8(3) 4 . ? C6 Fe C3 69.8(3) . . ? C3 Fe C3 106.1(4) 4 . ? C2 Fe C5 150.9(3) 4 . ? C2 Fe C5 69.9(3) . . ? C6 Fe C5 121.2(3) 4 . ? C6 Fe C5 41.0(2) . . ? C3 Fe C5 166.9(3) 4 . ? C3 Fe C5 68.3(3) . . ? C2 Fe C5 69.9(3) 4 4 ? C2 Fe C5 150.9(3) . 4 ? C6 Fe C5 41.0(2) 4 4 ? C6 Fe C5 121.2(3) . 4 ? C3 Fe C5 68.3(3) 4 4 ? C3 Fe C5 166.9(3) . 4 ? C5 Fe C5 114.4(4) . 4 ? C2 Fe C4 154.8(3) 4 . ? C2 Fe C4 69.9(3) . . ? C6 Fe C4 160.7(3) 4 . ? C6 Fe C4 68.8(3) . . ? C3 Fe C4 128.4(3) 4 . ? C3 Fe C4 40.7(3) . . ? C5 Fe C4 39.9(3) . . ? C5 Fe C4 133.1(3) 4 . ? C2 Fe C4 69.9(3) 4 4 ? C2 Fe C4 154.8(3) . 4 ? C6 Fe C4 68.8(3) 4 4 ? C6 Fe C4 160.7(3) . 4 ? C3 Fe C4 40.7(3) 4 4 ? C3 Fe C4 128.4(3) . 4 ? C5 Fe C4 133.1(3) . 4 ? C5 Fe C4 39.9(3) 4 4 ? C4 Fe C4 119.3(4) . 4 ? C1 Rh C7 90.2(3) . . ? C1 Rh C7 90.2(3) . 4 ? C7 Rh C7 38.4(4) . 4 ? C1 Rh C10 161.81(18) . 4 ? C7 Rh C10 93.1(3) . 4 ? C7 Rh C10 81.4(3) 4 4 ? C1 Rh C10 161.81(18) . . ? C7 Rh C10 81.4(3) . . ? C7 Rh C10 93.1(3) 4 . ? C10 Rh C10 36.0(4) 4 . ? C1 Rh Cl 92.6(3) . . ? C7 Rh Cl 160.57(18) . . ? C7 Rh Cl 160.57(18) 4 . ? C10 Rh Cl 90.14(19) 4 . ? C10 Rh Cl 90.14(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.514 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.072 #==================================================================== data_i0482 _database_code_depnum_ccdc_archive 'CCDC 697883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H38 Fe Mo N2 O4' _chemical_formula_sum 'C35 H38 Fe Mo N2 O4' _chemical_formula_weight 702.46 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 13.549(2) _cell_length_b 20.097(5) _cell_length_c 11.2263(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3056.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1814 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 23.23 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8167 _exptl_absorpt_correction_T_max 0.8969 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 173(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 71 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 7347 _diffrn_reflns_av_R_equivalents 0.1785 _diffrn_reflns_av_sigmaI/netI 0.2630 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2583 _reflns_number_gt 812 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.0000P] 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 2583 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2096 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 0.748 _refine_ls_restrained_S_all 0.748 _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 C1 C 0.3272(6) 0.2500 0.2782(6) 0.038(3) Uani 1 2 d S . . C2 C 0.3399(5) 0.1793(4) 0.4636(5) 0.046(2) Uani 1 1 d . . . C3 C 0.4246(6) 0.1743(5) 0.5357(5) 0.069(3) Uani 1 1 d . . . H3A H 0.4916 0.1773 0.5111 0.083 Uiso 1 1 calc R . . C4 C 0.3888(8) 0.1640(6) 0.6520(6) 0.095(4) Uani 1 1 d . . . H4A H 0.4289 0.1572 0.7204 0.114 Uiso 1 1 calc R . . C5 C 0.2842(8) 0.1653(6) 0.6519(6) 0.099(4) Uani 1 1 d . . . H5A H 0.2419 0.1623 0.7192 0.119 Uiso 1 1 calc R . . C6 C 0.2557(6) 0.1717(5) 0.5329(5) 0.069(3) Uani 1 1 d . . . H6A H 0.1897 0.1711 0.5041 0.083 Uiso 1 1 calc R . . C7 C 0.3928(8) 0.2500 -0.0050(9) 0.077(5) Uani 1 2 d S . . C8 C 0.1396(8) 0.2500 0.1809(9) 0.073(4) Uani 1 2 d S . . C9 C 0.2126(6) 0.3129(6) -0.0134(6) 0.075(2) Uiso 1 1 d . . . C10 C 0.3352(4) 0.1297(4) 0.2523(5) 0.0353(18) Uani 1 1 d . . . H10A H 0.2909 0.1425 0.1849 0.042 Uiso 1 1 calc R . . C11 C 0.2898(4) 0.0683(4) 0.3048(4) 0.040(2) Uani 1 1 d . . . H11A H 0.2272 0.0795 0.3475 0.048 Uiso 1 1 calc R . . C12 C 0.3607(5) 0.0293(4) 0.3879(5) 0.050(2) Uani 1 1 d . . . H12A H 0.3738 0.0557 0.4605 0.060 Uiso 1 1 calc R . . H12B H 0.3292 -0.0131 0.4123 0.060 Uiso 1 1 calc R . . C13 C 0.4558(5) 0.0149(5) 0.3257(6) 0.059(3) Uani 1 1 d . . . H13A H 0.5017 -0.0080 0.3821 0.071 Uiso 1 1 calc R . . C14 C 0.5023(4) 0.0770(5) 0.2821(5) 0.057(3) Uani 1 1 d . . . H14B H 0.5643 0.0660 0.2397 0.069 Uiso 1 1 calc R . . H14A H 0.5190 0.1058 0.3507 0.069 Uiso 1 1 calc R . . C15 C 0.4320(5) 0.1150(4) 0.1966(5) 0.047(2) Uani 1 1 d . . . H15A H 0.4638 0.1569 0.1677 0.056 Uiso 1 1 calc R . . C16 C 0.2688(5) 0.0202(4) 0.1984(5) 0.049(2) Uani 1 1 d . . . H16A H 0.2376 -0.0211 0.2284 0.059 Uiso 1 1 calc R . . H16B H 0.2224 0.0417 0.1420 0.059 Uiso 1 1 calc R . . C17 C 0.4140(5) 0.0661(4) 0.0909(5) 0.050(2) Uani 1 1 d . . . H17A H 0.3721 0.0879 0.0300 0.060 Uiso 1 1 calc R . . H17B H 0.4778 0.0545 0.0533 0.060 Uiso 1 1 calc R . . C18 C 0.3636(5) 0.0034(4) 0.1347(6) 0.047(2) Uani 1 1 d . . . H18A H 0.3486 -0.0260 0.0651 0.056 Uiso 1 1 calc R . . C19 C 0.4328(5) -0.0326(5) 0.2180(5) 0.058(3) Uani 1 1 d . . . H19B H 0.4947 -0.0443 0.1759 0.070 Uiso 1 1 calc R . . H19A H 0.4018 -0.0742 0.2469 0.070 Uiso 1 1 calc R . . N N 0.3399(4) 0.1915(3) 0.3332(4) 0.0397(16) Uani 1 1 d . . . O1 O 0.4652(5) 0.2500 -0.0584(6) 0.094(4) Uani 1 2 d S . . O2 O 0.0644(5) 0.2500 0.2340(7) 0.077(3) Uani 1 2 d S . . O3 O 0.1762(5) 0.3540(4) -0.0745(7) 0.116(3) Uani 1 1 d . . . Fe Fe 0.33814(11) 0.2500 0.57895(11) 0.0549(5) Uani 1 2 d S . . Mo Mo 0.26502(6) 0.2500 0.09128(8) 0.0796(5) Uani 1 2 d S . . 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 C1 0.041(5) 0.047(8) 0.026(4) 0.000 -0.008(4) 0.000 C2 0.066(4) 0.031(5) 0.042(3) 0.011(3) 0.001(3) -0.002(4) C3 0.077(5) 0.078(9) 0.052(4) -0.006(4) -0.013(4) 0.012(5) C4 0.185(9) 0.060(9) 0.039(4) 0.010(4) -0.019(5) 0.017(8) C5 0.172(8) 0.082(10) 0.044(4) -0.002(5) 0.047(5) -0.012(8) C6 0.103(6) 0.057(8) 0.047(3) -0.003(4) 0.016(4) -0.023(6) C7 0.073(7) 0.101(15) 0.056(6) 0.000 -0.012(5) 0.000 C8 0.074(7) 0.072(12) 0.073(6) 0.000 -0.037(5) 0.000 C10 0.053(4) 0.016(5) 0.037(3) 0.007(3) 0.003(3) 0.001(4) C11 0.046(4) 0.037(6) 0.037(3) -0.022(3) 0.001(3) -0.004(4) C12 0.090(4) 0.016(5) 0.046(4) 0.006(3) -0.002(3) 0.005(4) C13 0.073(5) 0.055(7) 0.049(4) 0.004(4) -0.001(3) 0.008(5) C14 0.047(4) 0.081(8) 0.044(4) -0.022(4) -0.003(3) -0.001(5) C15 0.066(4) 0.036(6) 0.037(3) -0.002(3) 0.002(3) 0.002(4) C16 0.059(4) 0.022(6) 0.065(4) -0.011(3) -0.003(4) -0.009(4) C17 0.077(4) 0.035(5) 0.039(3) -0.017(4) 0.004(4) 0.017(4) C18 0.064(4) 0.021(6) 0.056(4) -0.014(3) -0.012(3) 0.008(4) C19 0.081(4) 0.040(7) 0.054(4) -0.018(4) 0.002(4) 0.021(5) N 0.055(3) 0.042(4) 0.021(2) 0.000(2) -0.003(2) 0.018(3) O1 0.082(5) 0.119(10) 0.081(5) 0.000 0.031(4) 0.000 O2 0.057(4) 0.042(8) 0.131(6) 0.000 0.043(4) 0.000 O3 0.136(4) 0.065(6) 0.147(5) 0.007(5) 0.043(5) 0.014(4) Fe 0.0990(10) 0.0317(11) 0.0340(6) 0.000 0.0037(8) 0.000 Mo 0.0519(5) 0.1494(13) 0.0374(4) 0.000 -0.0040(5) 0.000 _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 C1 N 1.340(6) 8_565 ? C1 N 1.340(6) . ? C1 Mo 2.262(7) . ? C2 C6 1.389(9) . ? C2 C3 1.408(9) . ? C2 N 1.484(7) . ? C2 Fe 1.923(7) . ? C3 C4 1.408(9) . ? C3 Fe 1.980(9) . ? C3 H3A 0.9500 . ? C4 C5 1.419(13) . ? C4 Fe 2.032(10) . ? C4 H4A 0.9500 . ? C5 C6 1.397(9) . ? C5 Fe 2.026(11) . ? C5 H5A 0.9500 . ? C6 Fe 1.998(9) . ? C6 H6A 0.9500 . ? C7 O1 1.149(11) . ? C7 Mo 2.041(11) . ? C8 O2 1.181(12) . ? C8 Mo 1.975(11) . ? C9 O3 1.183(11) . ? C9 Mo 1.866(10) . ? C10 C15 1.483(9) . ? C10 C11 1.500(10) . ? C10 N 1.540(9) . ? C10 H10A 1.0000 . ? C11 C12 1.551(9) . ? C11 C16 1.563(9) . ? C11 H11A 1.0000 . ? C12 C13 1.493(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.482(12) . ? C13 C19 1.572(11) . ? C13 H13A 1.0000 . ? C14 C15 1.553(10) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C17 1.561(10) . ? C15 H15A 1.0000 . ? C16 C18 1.509(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.516(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.508(10) . ? C18 H18A 1.0000 . ? C19 H19B 0.9900 . ? C19 H19A 0.9900 . ? Fe C2 1.923(7) 8_565 ? Fe C3 1.980(9) 8_565 ? Fe C6 1.998(9) 8_565 ? Fe C5 2.026(11) 8_565 ? Fe C4 2.032(10) 8_565 ? Mo C9 1.866(10) 8_565 ? 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 N C1 N 122.8(7) 8_565 . ? N C1 Mo 118.4(3) 8_565 . ? N C1 Mo 118.4(3) . . ? C6 C2 C3 109.9(5) . . ? C6 C2 N 124.8(6) . . ? C3 C2 N 125.3(6) . . ? C6 C2 Fe 72.1(5) . . ? C3 C2 Fe 71.0(5) . . ? N C2 Fe 122.8(5) . . ? C4 C3 C2 105.3(7) . . ? C4 C3 Fe 71.5(6) . . ? C2 C3 Fe 66.7(5) . . ? C4 C3 H3A 127.4 . . ? C2 C3 H3A 127.4 . . ? Fe C3 H3A 126.0 . . ? C3 C4 C5 109.9(7) . . ? C3 C4 Fe 67.5(5) . . ? C5 C4 Fe 69.3(6) . . ? C3 C4 H4A 125.0 . . ? C5 C4 H4A 125.0 . . ? Fe C4 H4A 129.9 . . ? C6 C5 C4 106.2(7) . . ? C6 C5 Fe 68.6(5) . . ? C4 C5 Fe 69.8(6) . . ? C6 C5 H5A 126.9 . . ? C4 C5 H5A 126.9 . . ? Fe C5 H5A 126.3 . . ? C2 C6 C5 108.6(7) . . ? C2 C6 Fe 66.4(5) . . ? C5 C6 Fe 70.8(6) . . ? C2 C6 H6A 125.7 . . ? C5 C6 H6A 125.7 . . ? Fe C6 H6A 128.7 . . ? O1 C7 Mo 179.4(8) . . ? O2 C8 Mo 179.7(9) . . ? O3 C9 Mo 176.3(8) . . ? C15 C10 C11 111.4(6) . . ? C15 C10 N 111.9(5) . . ? C11 C10 N 116.6(4) . . ? C15 C10 H10A 105.3 . . ? C11 C10 H10A 105.3 . . ? N C10 H10A 105.3 . . ? C10 C11 C12 113.5(5) . . ? C10 C11 C16 106.4(5) . . ? C12 C11 C16 105.1(6) . . ? C10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? C16 C11 H11A 110.5 . . ? C13 C12 C11 110.6(5) . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 111.0(7) . . ? C14 C13 C19 109.9(6) . . ? C12 C13 C19 107.8(6) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C19 C13 H13A 109.3 . . ? C13 C14 C15 111.0(6) . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? H14B C14 H14A 108.0 . . ? C10 C15 C14 112.3(5) . . ? C10 C15 C17 107.9(5) . . ? C14 C15 C17 104.8(6) . . ? C10 C15 H15A 110.5 . . ? C14 C15 H15A 110.5 . . ? C17 C15 H15A 110.5 . . ? C18 C16 C11 110.2(5) . . ? C18 C16 H16A 109.6 . . ? C11 C16 H16A 109.6 . . ? C18 C16 H16B 109.6 . . ? C11 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C15 110.3(5) . . ? C18 C17 H17A 109.6 . . ? C15 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C15 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C19 C18 C16 110.1(5) . . ? C19 C18 C17 108.7(6) . . ? C16 C18 C17 110.5(6) . . ? C19 C18 H18A 109.2 . . ? C16 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C18 C19 C13 108.0(7) . . ? C18 C19 H19B 110.1 . . ? C13 C19 H19B 110.1 . . ? C18 C19 H19A 110.1 . . ? C13 C19 H19A 110.1 . . ? H19B C19 H19A 108.4 . . ? C1 N C2 126.8(6) . . ? C1 N C10 115.5(4) . . ? C2 N C10 116.7(5) . . ? C2 Fe C2 95.3(4) . 8_565 ? C2 Fe C3 113.3(3) . 8_565 ? C2 Fe C3 42.3(3) 8_565 8_565 ? C2 Fe C3 42.3(3) . . ? C2 Fe C3 113.3(3) 8_565 . ? C3 Fe C3 100.4(5) 8_565 . ? C2 Fe C6 41.4(3) . . ? C2 Fe C6 114.5(3) 8_565 . ? C3 Fe C6 150.7(3) 8_565 . ? C3 Fe C6 70.3(4) . . ? C2 Fe C6 114.5(3) . 8_565 ? C2 Fe C6 41.4(3) 8_565 8_565 ? C3 Fe C6 70.3(4) 8_565 8_565 ? C3 Fe C6 150.7(3) . 8_565 ? C6 Fe C6 103.9(5) . 8_565 ? C2 Fe C5 153.9(3) . 8_565 ? C2 Fe C5 69.9(3) 8_565 8_565 ? C3 Fe C5 70.6(4) 8_565 8_565 ? C3 Fe C5 163.4(4) . 8_565 ? C6 Fe C5 124.4(4) . 8_565 ? C6 Fe C5 40.6(3) 8_565 8_565 ? C2 Fe C5 69.9(3) . . ? C2 Fe C5 153.9(3) 8_565 . ? C3 Fe C5 163.4(4) 8_565 . ? C3 Fe C5 70.6(4) . . ? C6 Fe C5 40.6(3) . . ? C6 Fe C5 124.4(4) 8_565 . ? C5 Fe C5 114.4(5) 8_565 . ? C2 Fe C4 153.6(3) . 8_565 ? C2 Fe C4 68.9(3) 8_565 8_565 ? C3 Fe C4 41.1(3) 8_565 8_565 ? C3 Fe C4 123.5(4) . 8_565 ? C6 Fe C4 164.4(4) . 8_565 ? C6 Fe C4 67.9(4) 8_565 8_565 ? C5 Fe C4 40.9(4) 8_565 8_565 ? C5 Fe C4 132.3(3) . 8_565 ? C2 Fe C4 68.9(3) . . ? C2 Fe C4 153.6(3) 8_565 . ? C3 Fe C4 123.5(4) 8_565 . ? C3 Fe C4 41.1(3) . . ? C6 Fe C4 67.9(4) . . ? C6 Fe C4 164.4(4) 8_565 . ? C5 Fe C4 132.3(3) 8_565 . ? C5 Fe C4 40.9(4) . . ? C4 Fe C4 116.5(5) 8_565 . ? C9 Mo C9 85.2(6) 8_565 . ? C9 Mo C8 89.6(3) 8_565 . ? C9 Mo C8 89.6(3) . . ? C9 Mo C7 89.4(3) 8_565 . ? C9 Mo C7 89.4(3) . . ? C8 Mo C7 178.7(4) . . ? C9 Mo C1 136.6(3) 8_565 . ? C9 Mo C1 136.6(3) . . ? C8 Mo C1 81.2(3) . . ? C7 Mo C1 100.1(3) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.794 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.083 #================================================================= data_i0495 _database_code_depnum_ccdc_archive 'CCDC 697884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C31 H38 Fe N2), C7 H8' _chemical_formula_sum 'C32.75 H40 Fe N2' _chemical_formula_weight 517.52 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.763(3) _cell_length_b 16.153(5) _cell_length_c 16.339(5) _cell_angle_alpha 71.83(2) _cell_angle_beta 70.42(2) _cell_angle_gamma 81.36(2) _cell_volume 2539.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2488 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 23.79 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1106 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9056 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details 'X-red ver 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 213(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 11413 _diffrn_reflns_av_R_equivalents 0.1921 _diffrn_reflns_av_sigmaI/netI 0.4045 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6269 _reflns_number_gt 1750 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The carbon atoms of the disordered solvent molecule had to be refined isotropically as a consequence of the low data/parameter ratio. ; _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^)+(0.0248P)^2^+0.0000P] 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 6269 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2322 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 0.737 _refine_ls_restrained_S_all 0.737 _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 C1 C 0.1576(5) 1.1700(3) 0.1751(3) 0.056(4) Uani 1 1 d . . . C2 C 0.1864(5) 1.3342(3) 0.1197(3) 0.045(4) Uani 1 1 d R . . C3 C 0.2507(5) 1.3835(3) 0.1505(3) 0.057(4) Uani 1 1 d R . . H3 H 0.2519 1.3725 0.2102 0.069 Uiso 1 1 calc R . . C4 C 0.3126(5) 1.4525(3) 0.0753(3) 0.061(5) Uani 1 1 d R . . H4 H 0.3621 1.4951 0.0765 0.073 Uiso 1 1 calc R . . C5 C 0.2867(5) 1.4458(3) -0.0020(3) 0.054(4) Uani 1 1 d R . . H5 H 0.3160 1.4832 -0.0610 0.064 Uiso 1 1 calc R . . C6 C 0.2087(5) 1.3726(3) 0.0255(3) 0.067(5) Uani 1 1 d R . . H6 H 0.1773 1.3531 -0.0122 0.080 Uiso 1 1 calc R . . C7 C 0.3984(5) 1.2041(3) 0.0963(3) 0.041(4) Uani 1 1 d R . . C8 C 0.4708(5) 1.2425(3) 0.1323(3) 0.052(4) Uani 1 1 d R . . H8 H 0.4587 1.2340 0.1940 0.062 Uiso 1 1 calc R . . C9 C 0.5647(5) 1.2961(3) 0.0586(3) 0.051(4) Uani 1 1 d R . . H9 H 0.6256 1.3293 0.0630 0.061 Uiso 1 1 calc R . . C10 C 0.5503(5) 1.2907(3) -0.0229(3) 0.044(4) Uani 1 1 d R . . H10 H 0.6001 1.3198 -0.0819 0.053 Uiso 1 1 calc R . . C11 C 0.4476(5) 1.2339(3) 0.0005(3) 0.053(4) Uani 1 1 d R . . H11 H 0.4174 1.2186 -0.0404 0.063 Uiso 1 1 calc R . . C12 C -0.0310(16) 1.2718(9) 0.1929(9) 0.054(4) Uani 1 1 d . . . H12A H -0.0519 1.2813 0.1360 0.065 Uiso 1 1 calc R . . C13 C -0.1139(17) 1.1948(11) 0.2634(10) 0.059(5) Uani 1 1 d . . . H13A H -0.0836 1.1398 0.2463 0.071 Uiso 1 1 calc R . . C14 C -0.0846(17) 1.3532(9) 0.2247(10) 0.057(4) Uani 1 1 d . . . H14A H -0.0340 1.4033 0.1802 0.068 Uiso 1 1 calc R . . C15 C -0.1007(17) 1.1864(10) 0.3570(11) 0.066(5) Uani 1 1 d . . . H15A H -0.1519 1.1379 0.4024 0.079 Uiso 1 1 calc R . . H15B H -0.0080 1.1733 0.3549 0.079 Uiso 1 1 calc R . . C16 C -0.2532(17) 1.2155(11) 0.2711(12) 0.069(5) Uani 1 1 d . . . H16A H -0.2644 1.2212 0.2124 0.083 Uiso 1 1 calc R . . H16B H -0.3034 1.1660 0.3150 0.083 Uiso 1 1 calc R . . C17 C -0.2250(19) 1.3717(11) 0.2290(12) 0.087(6) Uani 1 1 d . . . H17B H -0.2334 1.3822 0.1687 0.105 Uiso 1 1 calc R . . H17A H -0.2582 1.4245 0.2487 0.105 Uiso 1 1 calc R . . C18 C -0.0713(18) 1.3443(12) 0.3170(10) 0.077(6) Uani 1 1 d . . . H18B H 0.0218 1.3337 0.3147 0.092 Uiso 1 1 calc R . . H18A H -0.1045 1.3982 0.3345 0.092 Uiso 1 1 calc R . . C19 C -0.1494(17) 1.2695(12) 0.3846(10) 0.067(5) Uani 1 1 d . . . H19A H -0.1396 1.2620 0.4447 0.080 Uiso 1 1 calc R . . C20 C -0.2893(18) 1.2872(14) 0.3903(11) 0.087(6) Uani 1 1 d . . . H20A H -0.3205 1.3425 0.4051 0.104 Uiso 1 1 calc R . . H20B H -0.3414 1.2408 0.4387 0.104 Uiso 1 1 calc R . . C21 C -0.3101(19) 1.2922(11) 0.2974(11) 0.071(5) Uani 1 1 d . . . H21A H -0.4043 1.3025 0.3003 0.085 Uiso 1 1 calc R . . C22 C 0.3250(13) 1.0548(8) 0.1475(8) 0.038(3) Uani 1 1 d . . . H22A H 0.3237 1.0517 0.0883 0.045 Uiso 1 1 calc R . . C23 C 0.2302(15) 0.9886(9) 0.2175(9) 0.050(4) Uani 1 1 d . . . H23A H 0.1396 1.0078 0.2147 0.060 Uiso 1 1 calc R . . C24 C 0.4646(15) 1.0232(8) 0.1514(9) 0.048(4) Uani 1 1 d . . . H24A H 0.5287 1.0647 0.1042 0.058 Uiso 1 1 calc R . . C25 C 0.2639(15) 0.8990(9) 0.2025(10) 0.050(4) Uani 1 1 d . . . H25A H 0.2560 0.9014 0.1437 0.060 Uiso 1 1 calc R . . H25B H 0.2007 0.8580 0.2495 0.060 Uiso 1 1 calc R . . C26 C 0.2364(15) 0.9833(9) 0.3123(8) 0.054(4) Uani 1 1 d . . . H26A H 0.1727 0.9425 0.3591 0.065 Uiso 1 1 calc R . . H26B H 0.2144 1.0409 0.3232 0.065 Uiso 1 1 calc R . . C27 C 0.4744(15) 1.0162(10) 0.2439(9) 0.052(4) Uani 1 1 d . . . H27A H 0.5651 0.9982 0.2450 0.062 Uiso 1 1 calc R . . H27B H 0.4526 1.0734 0.2557 0.062 Uiso 1 1 calc R . . C28 C 0.4976(16) 0.9337(9) 0.1361(9) 0.053(4) Uani 1 1 d . . . H28A H 0.5873 0.9145 0.1389 0.063 Uiso 1 1 calc R . . H28B H 0.4963 0.9377 0.0753 0.063 Uiso 1 1 calc R . . C29 C 0.3813(17) 0.9510(9) 0.3159(9) 0.052(4) Uani 1 1 d . . . H29A H 0.3877 0.9470 0.3761 0.062 Uiso 1 1 calc R . . C30 C 0.4028(17) 0.8662(9) 0.2047(9) 0.050(4) Uani 1 1 d . . . H30A H 0.4256 0.8084 0.1928 0.060 Uiso 1 1 calc R . . C31 C 0.4093(17) 0.8627(10) 0.2997(10) 0.059(5) Uani 1 1 d . . . H31B H 0.3448 0.8225 0.3467 0.071 Uiso 1 1 calc R . . H31A H 0.4973 0.8402 0.3042 0.071 Uiso 1 1 calc R . . C32 C 0.0141(5) 0.7050(4) 0.3472(3) 0.055(4) Uani 1 1 d . . . C33 C 0.0833(5) 0.6482(4) 0.2084(3) 0.040(4) Uani 1 1 d R . . C34 C 0.1177(5) 0.7097(4) 0.1216(3) 0.057(4) Uani 1 1 d R . . H34 H 0.1544 0.7637 0.1067 0.069 Uiso 1 1 calc R . . C35 C 0.0870(5) 0.6752(4) 0.0610(3) 0.076(6) Uani 1 1 d R . . H35 H 0.0998 0.7024 -0.0009 0.091 Uiso 1 1 calc R . . C36 C 0.0336(5) 0.5925(4) 0.1104(3) 0.055(4) Uani 1 1 d R . . H36 H 0.0048 0.5553 0.0870 0.066 Uiso 1 1 calc R . . C37 C 0.0313(5) 0.5758(4) 0.2015(3) 0.062(5) Uani 1 1 d R . . H37 H 0.0007 0.5256 0.2490 0.074 Uiso 1 1 calc R . . C38 C -0.1606(5) 0.7434(4) 0.2649(3) 0.050(4) Uani 1 1 d R . . C39 C -0.2406(5) 0.6761(4) 0.2735(3) 0.073(5) Uani 1 1 d R . . H39 H -0.2671 0.6271 0.3234 0.087 Uiso 1 1 calc R . . C40 C -0.2718(5) 0.6984(4) 0.1910(3) 0.062(5) Uani 1 1 d R . . H40 H -0.3207 0.6651 0.1759 0.074 Uiso 1 1 calc R . . C41 C -0.2174(5) 0.7781(4) 0.1360(3) 0.063(5) Uani 1 1 d R . . H41 H -0.2244 0.8082 0.0783 0.075 Uiso 1 1 calc R . . C42 C -0.1504(5) 0.8048(4) 0.1831(3) 0.061(5) Uani 1 1 d R . . H42 H -0.1056 0.8567 0.1620 0.073 Uiso 1 1 calc R . . C43 C 0.2344(14) 0.6319(8) 0.2992(8) 0.035(3) Uani 1 1 d . . . H43A H 0.2960 0.6735 0.2497 0.042 Uiso 1 1 calc R . . C44 C 0.2796(14) 0.5399(10) 0.2870(8) 0.052(4) Uani 1 1 d . . . H44A H 0.2677 0.5367 0.2306 0.062 Uiso 1 1 calc R . . C45 C 0.2499(14) 0.6339(10) 0.3899(9) 0.047(4) Uani 1 1 d . . . H45A H 0.2177 0.6917 0.4001 0.057 Uiso 1 1 calc R . . C46 C 0.4291(13) 0.5261(9) 0.2797(8) 0.042(4) Uani 1 1 d . . . H46A H 0.4625 0.4693 0.2691 0.050 Uiso 1 1 calc R . . H46B H 0.4785 0.5713 0.2280 0.050 Uiso 1 1 calc R . . C47 C 0.2013(14) 0.4711(8) 0.3666(8) 0.046(4) Uani 1 1 d . . . H47A H 0.2294 0.4131 0.3577 0.055 Uiso 1 1 calc R . . H47B H 0.1071 0.4815 0.3725 0.055 Uiso 1 1 calc R . . C48 C 0.1771(14) 0.5655(8) 0.4673(8) 0.041(4) Uani 1 1 d . . . H48A H 0.0828 0.5741 0.4733 0.049 Uiso 1 1 calc R . . H48B H 0.1886 0.5693 0.5230 0.049 Uiso 1 1 calc R . . C49 C 0.4003(14) 0.6212(9) 0.3770(8) 0.043(4) Uani 1 1 d . . . H49A H 0.4472 0.6659 0.3234 0.051 Uiso 1 1 calc R . . H49B H 0.4177 0.6278 0.4297 0.051 Uiso 1 1 calc R . . C50 C 0.4509(14) 0.5301(9) 0.3654(9) 0.043(4) Uani 1 1 d . . . H50A H 0.5461 0.5210 0.3599 0.051 Uiso 1 1 calc R . . C51 C 0.2266(15) 0.4763(10) 0.4545(8) 0.047(4) Uani 1 1 d . . . H51A H 0.1766 0.4312 0.5073 0.057 Uiso 1 1 calc R . . C52 C 0.3738(14) 0.4590(10) 0.4438(9) 0.054(4) Uani 1 1 d . . . H52A H 0.3899 0.4580 0.4997 0.064 Uiso 1 1 calc R . . H52B H 0.4031 0.4021 0.4324 0.064 Uiso 1 1 calc R . . C53 C -0.213(3) 0.7697(11) 0.4155(13) 0.117(9) Uani 1 1 d . . . H53A H -0.2821 0.7267 0.4422 0.140 Uiso 1 1 calc R . . C54 C -0.2705(14) 0.8576(8) 0.3780(9) 0.046(4) Uani 1 1 d . . . H54A H -0.3034 0.8540 0.3295 0.055 Uiso 1 1 calc R . . C55 C -0.1519(14) 0.7732(10) 0.4934(11) 0.055(4) Uani 1 1 d . . . H55A H -0.1062 0.7177 0.5176 0.066 Uiso 1 1 calc R . . C56 C -0.388(2) 0.876(2) 0.4533(14) 0.187(16) Uani 1 1 d . . . H56A H -0.4501 0.8297 0.4754 0.224 Uiso 1 1 calc R . . H56B H -0.4334 0.9313 0.4302 0.224 Uiso 1 1 calc R . . C57 C -0.179(2) 0.9271(16) 0.3397(11) 0.131(11) Uani 1 1 d . . . H57A H -0.2236 0.9824 0.3158 0.158 Uiso 1 1 calc R . . H57B H -0.1049 0.9143 0.2899 0.158 Uiso 1 1 calc R . . C58 C -0.273(2) 0.7933(11) 0.5587(11) 0.104(8) Uani 1 1 d . . . H58A H -0.2544 0.7828 0.6160 0.125 Uiso 1 1 calc R . . H58B H -0.3370 0.7510 0.5691 0.125 Uiso 1 1 calc R . . C59 C -0.0644(17) 0.8457(11) 0.4469(9) 0.067(5) Uani 1 1 d . . . H59A H -0.0041 0.8344 0.3910 0.081 Uiso 1 1 calc R . . H59B H -0.0105 0.8448 0.4851 0.081 Uiso 1 1 calc R . . C60 C -0.3392(18) 0.8821(11) 0.5387(12) 0.066(5) Uani 1 1 d . . . H60A H -0.4120 0.8939 0.5906 0.079 Uiso 1 1 calc R . . C61 C -0.1233(16) 0.9344(11) 0.4229(14) 0.092(7) Uani 1 1 d . . . H61A H -0.0588 0.9801 0.4018 0.110 Uiso 1 1 calc R . . C62 C -0.2478(17) 0.9535(11) 0.4886(9) 0.064(5) Uani 1 1 d . . . H62B H -0.2951 1.0024 0.4562 0.077 Uiso 1 1 calc R . . H62A H -0.2261 0.9734 0.5328 0.077 Uiso 1 1 calc R . . C63 C -0.156(5) 1.085(2) 0.087(3) 0.070(13) Uiso 0.50 1 d P . . C64 C 0.074(3) 1.0156(13) 0.0367(15) 0.042(10) Uiso 0.50 1 d PG . . C65 C -0.056(2) 1.0273(14) 0.0357(15) 0.054(8) Uiso 0.50 1 d PG . . C66 C -0.096(2) 0.9890(17) -0.0162(19) 0.085(18) Uiso 0.50 1 d PG . . C67 C -0.005(4) 0.9390(16) -0.0670(16) 0.084(11) Uiso 0.50 1 d PG . . C68 C 0.125(3) 0.9273(15) -0.0660(17) 0.13(3) Uiso 0.50 1 d PG . . C69 C 0.1647(19) 0.9656(16) -0.014(2) 0.076(10) Uiso 0.50 1 d PG . . N1 N 0.1180(12) 1.2559(7) 0.1701(7) 0.048(3) Uani 1 1 d . . . N2 N 0.2934(11) 1.1468(6) 0.1461(7) 0.038(3) Uani 1 1 d . . . N3 N 0.0972(11) 0.6595(6) 0.2911(5) 0.035(3) Uani 1 1 d . . . N4 N -0.0999(13) 0.7432(9) 0.3342(7) 0.063(4) Uani 1 1 d . . . Fe1 Fe 0.3764(2) 1.33302(13) 0.05649(13) 0.0438(6) Uani 1 1 d . . . Fe2 Fe -0.0711(2) 0.68900(13) 0.16828(12) 0.0404(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(11) 0.075(11) 0.061(9) -0.035(8) -0.022(8) 0.027(9) C2 0.052(11) 0.044(9) 0.025(7) -0.012(7) 0.001(7) 0.011(8) C3 0.059(12) 0.054(10) 0.055(10) -0.021(8) -0.015(8) 0.016(9) C4 0.045(11) 0.046(10) 0.068(11) -0.007(8) 0.007(8) -0.013(8) C5 0.069(13) 0.042(9) 0.035(8) -0.016(7) -0.001(8) 0.014(8) C6 0.062(13) 0.090(13) 0.056(10) -0.032(9) -0.032(9) 0.033(10) C7 0.029(9) 0.052(9) 0.029(7) -0.009(7) 0.005(6) -0.001(8) C8 0.046(11) 0.051(9) 0.040(8) -0.004(7) 0.005(8) -0.010(8) C9 0.056(12) 0.046(9) 0.049(9) -0.007(8) -0.017(8) -0.009(8) C10 0.037(10) 0.037(8) 0.058(9) -0.006(7) -0.018(7) -0.004(8) C11 0.057(12) 0.058(10) 0.044(9) -0.028(8) -0.013(8) 0.019(9) C12 0.066(13) 0.068(10) 0.037(8) -0.023(8) -0.025(8) 0.009(9) C13 0.051(13) 0.075(12) 0.067(11) -0.053(10) -0.019(9) 0.022(10) C14 0.049(13) 0.044(9) 0.058(9) -0.012(8) 0.002(8) 0.006(8) C15 0.049(12) 0.064(11) 0.089(12) -0.015(10) -0.033(10) 0.002(10) C16 0.046(14) 0.079(13) 0.095(13) -0.050(11) -0.025(10) 0.021(10) C17 0.067(16) 0.077(13) 0.094(13) -0.023(11) -0.006(11) 0.021(11) C18 0.086(15) 0.106(14) 0.054(10) -0.046(10) -0.011(9) -0.026(12) C19 0.046(13) 0.106(15) 0.056(10) -0.050(10) 0.000(8) -0.006(11) C20 0.041(13) 0.136(17) 0.067(12) -0.032(11) 0.012(9) -0.014(12) C21 0.059(13) 0.057(11) 0.084(13) -0.008(10) -0.020(10) 0.002(10) C22 0.034(10) 0.052(9) 0.027(7) -0.011(6) -0.014(6) 0.009(8) C23 0.038(10) 0.061(10) 0.051(9) -0.011(8) -0.014(7) -0.016(9) C24 0.038(11) 0.018(7) 0.072(10) 0.003(7) -0.011(8) 0.001(7) C25 0.044(12) 0.045(9) 0.068(10) -0.024(8) -0.016(8) -0.009(8) C26 0.059(12) 0.039(9) 0.040(8) 0.003(7) -0.001(7) 0.004(8) C27 0.051(11) 0.062(10) 0.059(9) -0.023(8) -0.035(8) 0.002(9) C28 0.057(12) 0.050(10) 0.048(9) -0.017(8) -0.013(8) 0.003(8) C29 0.078(14) 0.048(9) 0.036(8) -0.022(7) -0.026(8) 0.015(9) C30 0.081(14) 0.030(8) 0.051(9) -0.033(7) -0.021(8) 0.008(8) C31 0.046(11) 0.057(10) 0.072(11) -0.010(9) -0.021(8) -0.004(9) C32 0.055(12) 0.094(12) 0.022(7) -0.041(8) -0.008(7) 0.019(10) C33 0.037(10) 0.048(9) 0.027(7) -0.012(7) -0.007(6) 0.018(7) C34 0.043(11) 0.078(11) 0.040(8) -0.022(8) 0.000(7) 0.014(9) C35 0.057(13) 0.130(16) 0.042(9) -0.044(10) -0.019(8) 0.049(11) C36 0.040(11) 0.061(11) 0.077(12) -0.044(9) -0.032(9) 0.042(8) C37 0.099(15) 0.035(9) 0.058(10) -0.009(8) -0.037(9) 0.002(9) C38 0.043(10) 0.072(11) 0.038(8) -0.022(8) -0.012(7) -0.002(9) C39 0.030(11) 0.143(16) 0.031(8) -0.018(9) -0.005(7) 0.009(11) C40 0.051(12) 0.088(12) 0.052(9) -0.026(9) -0.013(8) -0.012(10) C41 0.055(12) 0.082(12) 0.057(10) -0.020(9) -0.029(9) 0.008(10) C42 0.076(14) 0.060(10) 0.052(9) -0.016(8) -0.044(9) 0.042(9) C43 0.031(10) 0.041(8) 0.035(7) -0.016(6) -0.012(6) 0.010(7) C44 0.042(11) 0.087(12) 0.030(8) -0.009(8) -0.018(7) -0.014(9) C45 0.038(11) 0.065(10) 0.052(9) -0.029(8) -0.016(7) -0.014(9) C46 0.016(9) 0.064(10) 0.034(7) -0.008(7) -0.003(6) 0.009(7) C47 0.047(10) 0.028(8) 0.068(10) -0.025(7) -0.013(8) -0.004(7) C48 0.049(10) 0.032(8) 0.048(8) -0.025(7) -0.012(7) 0.003(7) C49 0.048(11) 0.053(9) 0.031(7) -0.015(7) -0.019(7) 0.011(8) C50 0.020(9) 0.041(9) 0.058(9) -0.007(7) -0.008(7) 0.001(7) C51 0.048(12) 0.074(11) 0.019(7) 0.000(7) -0.019(7) -0.008(9) C52 0.039(11) 0.069(10) 0.054(9) -0.018(8) -0.016(8) -0.005(9) C53 0.23(3) 0.045(12) 0.090(15) -0.007(11) -0.073(18) -0.036(15) C54 0.043(11) 0.033(8) 0.045(8) 0.000(7) -0.004(7) 0.003(7) C55 0.012(9) 0.051(10) 0.096(12) -0.036(9) 0.000(8) 0.013(8) C56 0.077(18) 0.42(5) 0.118(17) -0.18(2) -0.070(14) 0.14(2) C57 0.16(2) 0.21(3) 0.060(12) -0.027(14) -0.039(13) -0.11(2) C58 0.15(2) 0.059(12) 0.050(10) 0.004(9) 0.019(12) 0.011(13) C59 0.082(14) 0.079(12) 0.038(8) -0.025(8) -0.017(9) 0.017(11) C60 0.064(13) 0.057(11) 0.081(12) -0.030(10) -0.024(10) 0.014(10) C61 0.025(11) 0.052(11) 0.18(2) -0.055(12) 0.015(11) -0.006(9) C62 0.079(14) 0.070(12) 0.040(8) -0.030(8) -0.017(9) 0.036(10) N1 0.039(9) 0.048(7) 0.051(7) -0.022(6) -0.008(6) 0.018(6) N2 0.046(8) 0.022(6) 0.046(6) -0.012(5) -0.011(6) 0.001(6) N3 0.037(8) 0.045(7) 0.014(5) 0.000(5) 0.001(5) -0.011(6) N4 0.046(9) 0.107(11) 0.048(7) -0.052(7) -0.023(6) 0.043(8) Fe1 0.0426(16) 0.0447(14) 0.0365(12) -0.0100(10) -0.0070(10) 0.0052(12) Fe2 0.0357(15) 0.0495(14) 0.0356(11) -0.0137(10) -0.0122(10) 0.0059(11) _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 C1 N1 1.375(12) . ? C1 N2 1.408(12) . ? C1 Fe1 3.444(5) . ? C2 C6 1.4200 . ? C2 C3 1.4200 . ? C2 N1 1.429 . ? C2 Fe1 1.957 . ? C3 C4 1.4200 . ? C3 Fe1 1.978 . ? C3 H3 0.9400 . ? C4 C5 1.4200 . ? C4 Fe1 2.030 . ? C4 H4 0.9400 . ? C5 C6 1.4200 . ? C5 Fe1 2.041 . ? C5 H5 0.9400 . ? C6 Fe1 1.997 . ? C6 H6 0.9400 . ? C7 C11 1.4200 . ? C7 C8 1.4200 . ? C7 N2 1.424 . ? C7 Fe1 1.982 . ? C8 C9 1.4200 . ? C8 Fe1 1.992 . ? C8 H8 0.9400 . ? C9 C10 1.4200 . ? C9 Fe1 2.034 . ? C9 H9 0.9400 . ? C10 C11 1.4200 . ? C10 Fe1 2.048 . ? C10 H10 0.9400 . ? C11 Fe1 2.016 . ? C11 H11 0.9400 . ? C12 N1 1.521(18) . ? C12 C14 1.526(19) . ? C12 C13 1.56(2) . ? C12 H12A 0.9900 . ? C13 C16 1.46(2) . ? C13 C15 1.55(2) . ? C13 H13A 0.9900 . ? C14 C17 1.48(2) . ? C14 C18 1.52(2) . ? C14 H14A 0.9900 . ? C15 C19 1.51(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C21 1.42(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C21 1.58(2) . ? C17 H17B 0.9800 . ? C17 H17A 0.9800 . ? C18 C19 1.50(2) . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C19 C20 1.47(2) . ? C19 H19A 0.9900 . ? C20 C21 1.58(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9900 . ? C22 N2 1.468(16) . ? C22 C23 1.509(17) . ? C22 C24 1.528(19) . ? C22 H22A 0.9900 . ? C23 C25 1.513(19) . ? C23 C26 1.548(18) . ? C23 H23A 0.9900 . ? C24 C28 1.512(18) . ? C24 C27 1.519(18) . ? C24 H24A 0.9900 . ? C25 C30 1.52(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C29 1.58(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C29 1.501(18) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C30 1.515(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C31 1.498(19) . ? C29 H29A 0.9900 . ? C30 C31 1.561(18) . ? C30 H30A 0.9900 . ? C31 H31B 0.9800 . ? C31 H31A 0.9800 . ? C32 N4 1.341(14) . ? C32 N3 1.363(11) . ? C32 Fe2 3.435(5) . ? C33 C34 1.4200 . ? C33 C37 1.4200 . ? C33 N3 1.476 . ? C33 Fe2 1.939 . ? C34 C35 1.4200 . ? C34 Fe2 1.958 . ? C34 H34 0.9400 . ? C35 C36 1.4200 . ? C35 Fe2 2.037 . ? C35 H35 0.9400 . ? C36 C37 1.4200 . ? C36 Fe2 2.067 . ? C36 H36 0.9400 . ? C37 Fe2 2.008 . ? C37 H37 0.9400 . ? C38 C42 1.3752 . ? C38 C39 1.4310 . ? C38 N4 1.483 . ? C38 Fe2 1.946 . ? C39 C40 1.4222 . ? C39 Fe2 2.028 . ? C39 H39 0.9400 . ? C40 C41 1.4003 . ? C40 Fe2 2.055 . ? C40 H40 0.9400 . ? C41 C42 1.4037 . ? C41 Fe2 2.057 . ? C41 H41 0.9400 . ? C42 Fe2 1.988 . ? C42 H42 0.9400 . ? C43 N3 1.514(16) . ? C43 C44 1.545(19) . ? C43 C45 1.557(17) . ? C43 H43A 0.9900 . ? C44 C47 1.511(16) . ? C44 C46 1.559(19) . ? C44 H44A 0.9900 . ? C45 C48 1.470(17) . ? C45 C49 1.55(2) . ? C45 H45A 0.9900 . ? C46 C50 1.518(18) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C51 1.576(17) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C51 1.512(19) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.536(18) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C52 1.518(17) . ? C50 H50A 0.9900 . ? C51 C52 1.53(2) . ? C51 H51A 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.49(2) . ? C53 N4 1.59(3) . ? C53 C55 1.63(2) . ? C53 H53A 0.9900 . ? C54 C57 1.45(2) . ? C54 C56 1.51(2) . ? C54 H54A 0.9900 . ? C55 C58 1.45(2) . ? C55 C59 1.461(19) . ? C55 H55A 0.9900 . ? C56 C60 1.68(2) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C61 1.70(3) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C60 1.49(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C61 1.47(2) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 C62 1.48(2) . ? C60 H60A 0.9900 . ? C61 C62 1.47(2) . ? C61 H61A 0.9900 . ? C62 H62B 0.9800 . ? C62 H62A 0.9800 . ? C63 C68 0.45(6) 2_575 ? C63 C65 1.51(6) . ? C63 C67 1.66(5) 2_575 ? C63 C69 1.67(6) 2_575 ? C64 C66 0.36(5) 2_575 ? C64 C67 1.07(5) 2_575 ? C64 C65 1.3900 . ? C64 C69 1.3900 . ? C64 C65 1.62(4) 2_575 ? C65 C68 1.07(3) 2_575 ? C65 C67 1.22(5) 2_575 ? C65 C69 1.31(5) 2_575 ? C65 C66 1.3900 . ? C65 C66 1.55(5) 2_575 ? C65 C64 1.62(4) 2_575 ? C65 C65 1.72(3) 2_575 ? C66 C64 0.36(3) 2_575 ? C66 C69 1.07(6) 2_575 ? C66 C67 1.3900 . ? C66 C65 1.55(4) 2_575 ? C67 C64 1.07(3) 2_575 ? C67 C65 1.22(4) 2_575 ? C67 C68 1.3900 . ? C67 C63 1.66(7) 2_575 ? C68 C63 0.45(5) 2_575 ? C68 C65 1.07(3) 2_575 ? C68 C69 1.3900 . ? C69 C66 1.07(5) 2_575 ? C69 C65 1.31(5) 2_575 ? C69 C63 1.67(6) 2_575 ? 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 C1 N2 119.2(7) . . ? N1 C1 Fe1 59.0(5) . . ? N2 C1 Fe1 61.3(4) . . ? C6 C2 C3 108.0 . . ? C6 C2 N1 123.9 . . ? C3 C2 N1 128.0 . . ? C6 C2 Fe1 70.45 . . ? C3 C2 Fe1 69.64 . . ? N1 C2 Fe1 122.4 . . ? C4 C3 C2 108.0 . . ? C4 C3 Fe1 71.22 . . ? C2 C3 Fe1 68.06 . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Fe1 C3 H3 126.3 . . ? C3 C4 C5 108.0 . . ? C3 C4 Fe1 67.32 . . ? C5 C4 Fe1 70.01 . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 128.2 . . ? C6 C5 C4 108.0 . . ? C6 C5 Fe1 67.75 . . ? C4 C5 Fe1 69.17 . . ? C6 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Fe1 C5 H5 128.7 . . ? C5 C6 C2 108.0 . . ? C5 C6 Fe1 71.10 . . ? C2 C6 Fe1 67.48 . . ? C5 C6 H6 126.0 . . ? C2 C6 H6 126.0 . . ? Fe1 C6 H6 127.0 . . ? C11 C7 C8 108.0 . . ? C11 C7 N2 125.1 . . ? C8 C7 N2 126.9 . . ? C11 C7 Fe1 70.51 . . ? C8 C7 Fe1 69.47 . . ? N2 C7 Fe1 124.9 . . ? C7 C8 C9 108.0 . . ? C7 C8 Fe1 68.66 . . ? C9 C8 Fe1 70.91 . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Fe1 C8 H8 126.0 . . ? C10 C9 C8 108.0 . . ? C10 C9 Fe1 70.19 . . ? C8 C9 Fe1 67.80 . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe1 C9 H9 127.6 . . ? C9 C10 C11 108.0 . . ? C9 C10 Fe1 69.09 . . ? C11 C10 Fe1 68.36 . . ? C9 C10 H10 126.0 . . ? C11 C10 H10 126.0 . . ? Fe1 C10 H10 128.1 . . ? C7 C11 C10 108.0 . . ? C7 C11 Fe1 67.89 . . ? C10 C11 Fe1 70.76 . . ? C7 C11 H11 126.0 . . ? C10 C11 H11 126.0 . . ? Fe1 C11 H11 126.9 . . ? N1 C12 C14 114.4(13) . . ? N1 C12 C13 115.7(12) . . ? C14 C12 C13 107.1(12) . . ? N1 C12 H12A 106.3 . . ? C14 C12 H12A 106.3 . . ? C13 C12 H12A 106.3 . . ? C16 C13 C15 106.4(13) . . ? C16 C13 C12 109.5(14) . . ? C15 C13 C12 108.2(12) . . ? C16 C13 H13A 110.9 . . ? C15 C13 H13A 110.9 . . ? C12 C13 H13A 110.9 . . ? C17 C14 C18 109.1(14) . . ? C17 C14 C12 110.2(15) . . ? C18 C14 C12 112.2(13) . . ? C17 C14 H14A 108.4 . . ? C18 C14 H14A 108.4 . . ? C12 C14 H14A 108.4 . . ? C19 C15 C13 111.3(14) . . ? C19 C15 H15A 109.4 . . ? C13 C15 H15A 109.4 . . ? C19 C15 H15B 109.4 . . ? C13 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C21 C16 C13 116.6(16) . . ? C21 C16 H16A 108.1 . . ? C13 C16 H16A 108.1 . . ? C21 C16 H16B 108.1 . . ? C13 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C14 C17 C21 110.5(14) . . ? C14 C17 H17B 109.6 . . ? C21 C17 H17B 109.6 . . ? C14 C17 H17A 109.6 . . ? C21 C17 H17A 109.6 . . ? H17B C17 H17A 108.1 . . ? C19 C18 C14 108.5(13) . . ? C19 C18 H18B 110.0 . . ? C14 C18 H18B 110.0 . . ? C19 C18 H18A 110.0 . . ? C14 C18 H18A 110.0 . . ? H18B C18 H18A 108.4 . . ? C20 C19 C18 109.7(16) . . ? C20 C19 C15 109.0(15) . . ? C18 C19 C15 110.4(13) . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? C15 C19 H19A 109.2 . . ? C19 C20 C21 110.6(14) . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C16 C21 C20 109.7(16) . . ? C16 C21 C17 108.2(15) . . ? C20 C21 C17 102.6(14) . . ? C16 C21 H21A 112.0 . . ? C20 C21 H21A 112.0 . . ? C17 C21 H21A 112.0 . . ? N2 C22 C23 117.6(11) . . ? N2 C22 C24 113.6(11) . . ? C23 C22 C24 108.4(11) . . ? N2 C22 H22A 105.4 . . ? C23 C22 H22A 105.4 . . ? C24 C22 H22A 105.4 . . ? C22 C23 C25 111.9(12) . . ? C22 C23 C26 108.6(11) . . ? C25 C23 C26 109.0(12) . . ? C22 C23 H23A 109.1 . . ? C25 C23 H23A 109.1 . . ? C26 C23 H23A 109.1 . . ? C28 C24 C27 108.0(11) . . ? C28 C24 C22 110.1(12) . . ? C27 C24 C22 110.1(12) . . ? C28 C24 H24A 109.5 . . ? C27 C24 H24A 109.5 . . ? C22 C24 H24A 109.5 . . ? C23 C25 C30 111.8(12) . . ? C23 C25 H25A 109.3 . . ? C30 C25 H25A 109.3 . . ? C23 C25 H25B 109.3 . . ? C30 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C23 C26 C29 108.4(11) . . ? C23 C26 H26A 110.0 . . ? C29 C26 H26A 110.0 . . ? C23 C26 H26B 110.0 . . ? C29 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C29 C27 C24 110.2(11) . . ? C29 C27 H27A 109.6 . . ? C24 C27 H27A 109.6 . . ? C29 C27 H27B 109.6 . . ? C24 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C24 C28 C30 113.0(12) . . ? C24 C28 H28A 109.0 . . ? C30 C28 H28A 109.0 . . ? C24 C28 H28B 109.0 . . ? C30 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C31 C29 C27 111.6(12) . . ? C31 C29 C26 107.8(13) . . ? C27 C29 C26 107.8(11) . . ? C31 C29 H29A 109.9 . . ? C27 C29 H29A 109.9 . . ? C26 C29 H29A 109.9 . . ? C28 C30 C25 108.2(12) . . ? C28 C30 C31 106.6(11) . . ? C25 C30 C31 107.0(12) . . ? C28 C30 H30A 111.6 . . ? C25 C30 H30A 111.6 . . ? C31 C30 H30A 111.6 . . ? C29 C31 C30 111.6(12) . . ? C29 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? C29 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? H31B C31 H31A 108.0 . . ? N4 C32 N3 121.4(7) . . ? N4 C32 Fe2 60.4(5) . . ? N3 C32 Fe2 61.0(5) . . ? C34 C33 C37 108.0 . . ? C34 C33 N3 125.4 . . ? C37 C33 N3 126.6 . . ? C34 C33 Fe2 69.33 . . ? C37 C33 Fe2 71.53 . . ? N3 C33 Fe2 123.8(5) . . ? C35 C34 C33 108.0 . . ? C35 C34 Fe2 72.20 . . ? C33 C34 Fe2 67.93 . . ? C35 C34 H34 126.0 . . ? C33 C34 H34 126.0 . . ? Fe2 C34 H34 125.4 . . ? C34 C35 C36 108.0 . . ? C34 C35 Fe2 66.22 . . ? C36 C35 Fe2 70.89 . . ? C34 C35 H35 126.0 . . ? C36 C35 H35 126.0 . . ? Fe2 C35 H35 128.4 . . ? C37 C36 C35 108.0 . . ? C37 C36 Fe2 67.39 . . ? C35 C36 Fe2 68.63 . . ? C37 C36 H36 126.0 . . ? C35 C36 H36 126.0 . . ? Fe2 C36 H36 129.6 . . ? C36 C37 C33 108.0 . . ? C36 C37 Fe2 71.86 . . ? C33 C37 Fe2 66.34 . . ? C36 C37 H37 126.0 . . ? C33 C37 H37 126.0 . . ? Fe2 C37 H37 127.3 . . ? C42 C38 C39 108.3 . . ? C42 C38 N4 127.7 . . ? C39 C38 N4 124.0 . . ? C42 C38 Fe2 71.21 . . ? C39 C38 Fe2 72.00 . . ? N4 C38 Fe2 122.0 . . ? C40 C39 C38 106.1 . . ? C40 C39 Fe2 70.64 . . ? C38 C39 Fe2 65.84 . . ? C40 C39 H39 127.0 . . ? C38 C39 H39 127.0 . . ? Fe2 C39 H39 128.0 . . ? C41 C40 C39 108.7 . . ? C41 C40 Fe2 70.15 . . ? C39 C40 Fe2 68.60 . . ? C41 C40 H40 125.7 . . ? C39 C40 H40 125.7 . . ? Fe2 C40 H40 127.2 . . ? C40 C41 C42 107.4 . . ? C40 C41 Fe2 70.03 . . ? C42 C41 Fe2 67.09 . . ? C40 C41 H41 126.3 . . ? C42 C41 H41 126.3 . . ? Fe2 C41 H41 128.1 . . ? C38 C42 C41 109.5 . . ? C38 C42 Fe2 67.89 . . ? C41 C42 Fe2 72.34 . . ? C38 C42 H42 125.3 . . ? C41 C42 H42 125.3 . . ? Fe2 C42 H42 126.1 . . ? N3 C43 C44 112.1(11) . . ? N3 C43 C45 114.1(11) . . ? C44 C43 C45 108.3(11) . . ? N3 C43 H43A 107.3 . . ? C44 C43 H43A 107.3 . . ? C45 C43 H43A 107.3 . . ? C47 C44 C43 110.7(11) . . ? C47 C44 C46 110.3(11) . . ? C43 C44 C46 107.0(12) . . ? C47 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? C46 C44 H44A 109.6 . . ? C48 C45 C49 111.1(12) . . ? C48 C45 C43 112.0(11) . . ? C49 C45 C43 105.6(11) . . ? C48 C45 H45A 109.3 . . ? C49 C45 H45A 109.3 . . ? C43 C45 H45A 109.3 . . ? C50 C46 C44 111.0(11) . . ? C50 C46 H46A 109.4 . . ? C44 C46 H46A 109.4 . . ? C50 C46 H46B 109.4 . . ? C44 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? C44 C47 C51 108.1(10) . . ? C44 C47 H47A 110.1 . . ? C51 C47 H47A 110.1 . . ? C44 C47 H47B 110.1 . . ? C51 C47 H47B 110.1 . . ? H47A C47 H47B 108.4 . . ? C45 C48 C51 110.5(11) . . ? C45 C48 H48A 109.6 . . ? C51 C48 H48A 109.6 . . ? C45 C48 H48B 109.6 . . ? C51 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? C50 C49 C45 110.1(12) . . ? C50 C49 H49A 109.6 . . ? C45 C49 H49A 109.6 . . ? C50 C49 H49B 109.6 . . ? C45 C49 H49B 109.6 . . ? H49A C49 H49B 108.2 . . ? C46 C50 C52 108.0(11) . . ? C46 C50 C49 107.1(11) . . ? C52 C50 C49 111.4(11) . . ? C46 C50 H50A 110.1 . . ? C52 C50 H50A 110.1 . . ? C49 C50 H50A 110.1 . . ? C48 C51 C52 112.2(12) . . ? C48 C51 C47 108.2(11) . . ? C52 C51 C47 109.0(11) . . ? C48 C51 H51A 109.2 . . ? C52 C51 H51A 109.2 . . ? C47 C51 H51A 109.2 . . ? C50 C52 C51 109.6(12) . . ? C50 C52 H52A 109.8 . . ? C51 C52 H52A 109.8 . . ? C50 C52 H52B 109.8 . . ? C51 C52 H52B 109.8 . . ? H52A C52 H52B 108.2 . . ? C54 C53 N4 107.8(13) . . ? C54 C53 C55 109.6(14) . . ? N4 C53 C55 110.8(18) . . ? C54 C53 H53A 109.5 . . ? N4 C53 H53A 109.5 . . ? C55 C53 H53A 109.5 . . ? C57 C54 C53 114.8(18) . . ? C57 C54 C56 111.6(19) . . ? C53 C54 C56 106.8(17) . . ? C57 C54 H54A 107.8 . . ? C53 C54 H54A 107.8 . . ? C56 C54 H54A 107.8 . . ? C58 C55 C59 114.0(14) . . ? C58 C55 C53 99.1(17) . . ? C59 C55 C53 102.8(14) . . ? C58 C55 H55A 113.2 . . ? C59 C55 H55A 113.2 . . ? C53 C55 H55A 113.2 . . ? C54 C56 C60 110.3(16) . . ? C54 C56 H56A 109.6 . . ? C60 C56 H56A 109.6 . . ? C54 C56 H56B 109.6 . . ? C60 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C54 C57 C61 108.1(13) . . ? C54 C57 H57A 110.1 . . ? C61 C57 H57A 110.1 . . ? C54 C57 H57B 110.1 . . ? C61 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? C55 C58 C60 119.4(14) . . ? C55 C58 H58A 107.5 . . ? C60 C58 H58A 107.5 . . ? C55 C58 H58B 107.5 . . ? C60 C58 H58B 107.5 . . ? H58A C58 H58B 107.0 . . ? C55 C59 C61 118.5(15) . . ? C55 C59 H59A 107.7 . . ? C61 C59 H59A 107.7 . . ? C55 C59 H59B 107.7 . . ? C61 C59 H59B 107.7 . . ? H59A C59 H59B 107.1 . . ? C62 C60 C58 114.5(16) . . ? C62 C60 C56 98.8(17) . . ? C58 C60 C56 98.3(17) . . ? C62 C60 H60A 114.3 . . ? C58 C60 H60A 114.3 . . ? C56 C60 H60A 114.3 . . ? C59 C61 C62 116.0(15) . . ? C59 C61 C57 99.3(15) . . ? C62 C61 C57 100.8(15) . . ? C59 C61 H61A 113.1 . . ? C62 C61 H61A 113.1 . . ? C57 C61 H61A 113.1 . . ? C61 C62 C60 117.4(14) . . ? C61 C62 H62B 108.0 . . ? C60 C62 H62B 108.0 . . ? C61 C62 H62A 108.0 . . ? C60 C62 H62A 108.0 . . ? H62B C62 H62A 107.2 . . ? C68 C63 C65 13(6) 2_575 . ? C68 C63 C67 48(6) 2_575 2_575 ? C65 C63 C67 45(2) . 2_575 ? C68 C63 C69 46(6) 2_575 2_575 ? C65 C63 C69 48(2) . 2_575 ? C67 C63 C69 93(3) 2_575 2_575 ? C66 C64 C67 147(9) 2_575 2_575 ? C67 C64 C65 58(3) 2_575 . ? C66 C64 C69 25(6) 2_575 . ? C67 C64 C69 172(3) 2_575 . ? C65 C64 C69 120.0 . . ? C66 C64 C65 45(5) 2_575 2_575 ? C67 C64 C65 125(4) 2_575 2_575 ? C65 C64 C65 69.3(15) . 2_575 ? C69 C64 C65 50.9(15) . 2_575 ? C68 C65 C67 74(3) 2_575 2_575 ? C68 C65 C69 70(3) 2_575 2_575 ? C67 C65 C69 144(3) 2_575 2_575 ? C68 C65 C64 122(5) 2_575 . ? C67 C65 C64 48(3) 2_575 . ? C69 C65 C64 165(3) 2_575 . ? C68 C65 C66 117(5) 2_575 . ? C67 C65 C66 166(3) 2_575 . ? C69 C65 C66 47(3) 2_575 . ? C64 C65 C66 120.0 . . ? C68 C65 C63 5(3) 2_575 . ? C67 C65 C63 73.6(19) 2_575 . ? C69 C65 C63 72.0(19) 2_575 . ? C64 C65 C63 121(3) . . ? C66 C65 C63 118(3) . . ? C68 C65 C66 132(4) 2_575 2_575 ? C67 C65 C66 59(2) 2_575 2_575 ? C69 C65 C66 152(3) 2_575 2_575 ? C64 C65 C66 12.6(17) . 2_575 ? C66 C65 C66 108.5(17) . 2_575 ? C63 C65 C66 132(2) . 2_575 ? C68 C65 C64 125(5) 2_575 2_575 ? C67 C65 C64 155(4) 2_575 2_575 ? C69 C65 C64 55(3) 2_575 2_575 ? C64 C65 C64 110.7(13) . 2_575 ? C66 C65 C64 10.5(13) . 2_575 ? C63 C65 C64 127(3) . 2_575 ? C66 C65 C64 99(2) 2_575 2_575 ? C68 C65 C65 167(4) 2_575 2_575 ? C67 C65 C65 108(3) 2_575 2_575 ? C69 C65 C65 104(3) 2_575 2_575 ? C64 C65 C65 61.7(16) . 2_575 ? C66 C65 C65 58.6(16) . 2_575 ? C63 C65 C65 172(2) . 2_575 ? C66 C65 C65 49.9(10) 2_575 2_575 ? C64 C65 C65 49.0(13) 2_575 2_575 ? C64 C66 C69 147(9) 2_575 2_575 ? C64 C66 C67 25(6) 2_575 . ? C69 C66 C67 172(4) 2_575 . ? C69 C66 C65 63(4) 2_575 . ? C67 C66 C65 120.0 . . ? C64 C66 C65 57(6) 2_575 2_575 ? C69 C66 C65 132(4) 2_575 2_575 ? C67 C66 C65 48.8(13) . 2_575 ? C65 C66 C65 71.5(13) . 2_575 ? C64 C67 C65 74(2) 2_575 2_575 ? C64 C67 C66 8(2) 2_575 . ? C65 C67 C66 72.5(17) 2_575 . ? C64 C67 C68 122(2) 2_575 . ? C65 C67 C68 48.0(17) 2_575 . ? C66 C67 C68 120.0 . . ? C64 C67 C63 135(3) 2_575 2_575 ? C65 C67 C63 61(3) 2_575 2_575 ? C66 C67 C63 134(2) . 2_575 ? C68 C67 C63 14(2) . 2_575 ? C63 C68 C65 162(9) 2_575 2_575 ? C63 C68 C67 118(9) 2_575 . ? C65 C68 C67 58(3) 2_575 . ? C63 C68 C69 120(9) 2_575 . ? C65 C68 C69 63(3) 2_575 . ? C67 C68 C69 120.0 . . ? C66 C69 C65 70(2) 2_575 2_575 ? C66 C69 C68 117(2) 2_575 . ? C65 C69 C68 46.7(13) 2_575 . ? C66 C69 C64 8(2) 2_575 . ? C65 C69 C64 73.7(13) 2_575 . ? C68 C69 C64 120.0 . . ? C66 C69 C63 130(4) 2_575 2_575 ? C65 C69 C63 60(3) 2_575 2_575 ? C68 C69 C63 14(2) . 2_575 ? C64 C69 C63 133(2) . 2_575 ? C1 N1 C2 131.0 . . ? C1 N1 C12 112.6(10) . . ? C2 N1 C12 112.3 . . ? C1 N2 C7 127.2 . . ? C1 N2 C22 115.0(9) . . ? C7 N2 C22 115.9 . . ? C32 N3 C33 127.9 . . ? C32 N3 C43 118.6(8) . . ? C33 N3 C43 112.2 . . ? C32 N4 C38 130.0 . . ? C32 N4 C53 119.3(12) . . ? C38 N4 C53 108.1 . . ? C2 Fe1 C3 42.29 . . ? C2 Fe1 C7 93.6 . . ? C3 Fe1 C7 113.7 . . ? C2 Fe1 C8 110.0 . . ? C3 Fe1 C8 99.7 . . ? C7 Fe1 C8 41.87 . . ? C2 Fe1 C6 42.07 . . ? C3 Fe1 C6 70.61 . . ? C7 Fe1 C6 111.9 . . ? C8 Fe1 C6 147.3 . . ? C2 Fe1 C11 115.2 . . ? C3 Fe1 C11 152.0 . . ? C7 Fe1 C11 41.60 . . ? C8 Fe1 C11 69.93 . . ? C6 Fe1 C11 103.5 . . ? C2 Fe1 C4 70.34 . . ? C3 Fe1 C4 41.47 . . ? C7 Fe1 C4 154.5 . . ? C8 Fe1 C4 124.1 . . ? C6 Fe1 C4 69.57 . . ? C11 Fe1 C4 163.6 . . ? C2 Fe1 C9 149.9 . . ? C3 Fe1 C9 120.7 . . ? C7 Fe1 C9 69.80 . . ? C8 Fe1 C9 41.29 . . ? C6 Fe1 C9 167.5 . . ? C11 Fe1 C9 69.12 . . ? C4 Fe1 C9 114.6 . . ? C2 Fe1 C5 70.10 . . ? C3 Fe1 C5 69.70 . . ? C7 Fe1 C5 152.1 . . ? C8 Fe1 C5 164.7 . . ? C6 Fe1 C5 41.16 . . ? C11 Fe1 C5 124.5 . . ? C4 Fe1 C5 40.82 . . ? C9 Fe1 C5 134.3 . . ? C2 Fe1 C10 155.8 . . ? C3 Fe1 C10 160.5 . . ? C7 Fe1 C10 69.50 . . ? C8 Fe1 C10 69.29 . . ? C6 Fe1 C10 127.3 . . ? C11 Fe1 C10 40.89 . . ? C4 Fe1 C10 131.3 . . ? C9 Fe1 C10 40.71 . . ? C5 Fe1 C10 117.2 . . ? C2 Fe1 C1 47.09 . . ? C3 Fe1 C1 78.13 . . ? C7 Fe1 C1 46.73 . . ? C8 Fe1 C1 75.20 . . ? C6 Fe1 C1 72.22 . . ? C11 Fe1 C1 74.08 . . ? C4 Fe1 C1 115.9 . . ? C9 Fe1 C1 113.80 . . ? C5 Fe1 C1 111.9 . . ? C10 Fe1 C1 112.8 . . ? C33 Fe2 C38 94.7 . . ? C33 Fe2 C34 42.74 . . ? C38 Fe2 C34 111.1 . . ? C33 Fe2 C42 115.5 . . ? C38 Fe2 C42 40.91 . . ? C34 Fe2 C42 101.9 . . ? C33 Fe2 C37 42.13 . . ? C38 Fe2 C37 116.5 . . ? C34 Fe2 C37 70.80 . . ? C42 Fe2 C37 153.5 . . ? C33 Fe2 C39 112.1 . . ? C38 Fe2 C39 42.15 . . ? C34 Fe2 C39 148.3 . . ? C42 Fe2 C39 69.00 . . ? C37 Fe2 C39 103.4 . . ? C33 Fe2 C35 70.55 . . ? C38 Fe2 C35 151.1 . . ? C34 Fe2 C35 41.59 . . ? C42 Fe2 C35 122.7 . . ? C37 Fe2 C35 69.22 . . ? C39 Fe2 C35 166.5 . . ? C33 Fe2 C40 151.7 . . ? C38 Fe2 C40 69.43 . . ? C34 Fe2 C40 164.5 . . ? C42 Fe2 C40 67.92 . . ? C37 Fe2 C40 123.5 . . ? C39 Fe2 C40 40.76 . . ? C35 Fe2 C40 133.4 . . ? C33 Fe2 C41 155.6 . . ? C38 Fe2 C41 69.00 . . ? C34 Fe2 C41 125.0 . . ? C42 Fe2 C41 40.57 . . ? C37 Fe2 C41 161.7 . . ? C39 Fe2 C41 68.31 . . ? C35 Fe2 C41 115.2 . . ? C40 Fe2 C41 39.82 . . ? C33 Fe2 C36 69.91 . . ? C38 Fe2 C36 156.9 . . ? C34 Fe2 C36 69.56 . . ? C42 Fe2 C36 161.6 . . ? C37 Fe2 C36 40.76 . . ? C39 Fe2 C36 126.8 . . ? C35 Fe2 C36 40.48 . . ? C40 Fe2 C36 116.4 . . ? C41 Fe2 C36 130.8 . . ? C33 Fe2 C32 47.17 . . ? C38 Fe2 C32 47.48 . . ? C34 Fe2 C32 74.08 . . ? C42 Fe2 C32 76.45 . . ? C37 Fe2 C32 77.09 . . ? C39 Fe2 C32 74.27 . . ? C35 Fe2 C32 113.6 . . ? C40 Fe2 C32 112.96 . . ? C41 Fe2 C32 114.3 . . ? C36 Fe2 C32 114.9 . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.575 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.087 #===eof========================================================