# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Alagar Srinivasan' _publ_contact_author_email SRINI@NISER.AC.IN _publ_section_title ; Calix[n]metallocenyl[m]phyrins (n = 1, 2 and m = 2, 4): Aryl vs Alkyl ; loop_ _publ_author_name 'Alagar Srinivasan' 'K. S. Anju' 'S. Ramakrishnan' 'E. Suresh' 'Ajesh P. Thomas' # Attachment 'Fe-Calix-PF5__4b_.cif' data_rk215 _database_code_depnum_ccdc_archive 'CCDC 732747' #TrackingRef 'Fe-Calix-PF5__4b_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H25 F5 Fe N2' _chemical_formula_weight 576.38 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1820(2) _cell_length_b 10.4371(2) _cell_length_c 21.7536(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.4690(10) _cell_angle_gamma 90.00 _cell_volume 2538.73(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7550 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.0 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7031 _exptl_absorpt_correction_T_max 0.8801 _exptl_absorpt_process_details '(SADABS, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker axs kappa apex2 CCD diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32605 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.25 _reflns_number_total 7550 _reflns_number_gt 5510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altomare etal., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 32 (Farrugia, 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^)+(0.0632P)^2^+0.4317P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7550 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.04737(16) 0.24425(18) 0.99213(10) 0.0405(4) Uani 1 1 d . . . H1 H -0.0125 0.1831 0.9961 0.049 Uiso 1 1 calc R . . C2 C 0.06269(18) 0.3524(2) 1.03010(10) 0.0497(5) Uani 1 1 d . . . H2 H 0.0147 0.3751 1.0631 0.060 Uiso 1 1 calc R . . C3 C 0.1637(2) 0.42030(19) 1.00923(10) 0.0510(5) Uani 1 1 d . . . H3 H 0.1942 0.4954 1.0262 0.061 Uiso 1 1 calc R . . C4 C 0.21032(17) 0.35399(17) 0.95795(9) 0.0399(4) Uani 1 1 d . . . H4 H 0.2769 0.3785 0.9354 0.048 Uiso 1 1 calc R . . C5 C 0.13849(15) 0.24356(16) 0.94651(8) 0.0339(4) Uani 1 1 d . . . C6 C 0.37707(15) 0.21304(16) 1.07861(7) 0.0306(3) Uani 1 1 d . . . C7 C 0.33750(15) 0.09766(16) 1.05018(8) 0.0329(3) Uani 1 1 d . . . H7 H 0.3783 0.0523 1.0201 0.040 Uiso 1 1 calc R . . C8 C 0.22556(16) 0.06343(18) 1.07533(9) 0.0396(4) Uani 1 1 d . . . H8 H 0.1805 -0.0082 1.0646 0.048 Uiso 1 1 calc R . . C9 C 0.19432(17) 0.1557(2) 1.11904(9) 0.0440(5) Uani 1 1 d . . . H9 H 0.1254 0.1557 1.1427 0.053 Uiso 1 1 calc R . . C10 C 0.28623(17) 0.24887(18) 1.12096(8) 0.0390(4) Uani 1 1 d . . . H10 H 0.2872 0.3215 1.1457 0.047 Uiso 1 1 calc R . . C11 C 0.50166(16) 0.27211(16) 1.07852(8) 0.0335(4) Uani 1 1 d . . . C12 C 0.4967(2) 0.4162(2) 1.09244(11) 0.0559(6) Uani 1 1 d . . . H12A H 0.4548 0.4299 1.1302 0.084 Uiso 1 1 calc R . . H12B H 0.4556 0.4597 1.0596 0.084 Uiso 1 1 calc R . . H12C H 0.5765 0.4493 1.0962 0.084 Uiso 1 1 calc R . . C13 C 0.57295(18) 0.2027(3) 1.12956(9) 0.0518(5) Uani 1 1 d . . . H13A H 0.5323 0.2123 1.1680 0.078 Uiso 1 1 calc R . . H13B H 0.6515 0.2394 1.1328 0.078 Uiso 1 1 calc R . . H13C H 0.5794 0.1134 1.1196 0.078 Uiso 1 1 calc R . . C14 C 0.56765(15) 0.25599(15) 1.01907(8) 0.0311(3) Uani 1 1 d . . . C15 C 0.69337(16) 0.27012(18) 1.00914(9) 0.0375(4) Uani 1 1 d . . . H15 H 0.7514 0.2872 1.0389 0.045 Uiso 1 1 calc R . . C16 C 0.71193(15) 0.25368(16) 0.94754(9) 0.0346(4) Uani 1 1 d . . . H16 H 0.7850 0.2576 0.9275 0.042 Uiso 1 1 calc R . . C17 C 0.59900(15) 0.22954(16) 0.92015(8) 0.0315(3) Uani 1 1 d . . . C18 C 0.56579(15) 0.20298(17) 0.85946(8) 0.0334(4) Uani 1 1 d . . . C19 C 0.66013(15) 0.19929(17) 0.81161(8) 0.0337(4) Uani 1 1 d . . . C20 C 0.73256(16) 0.30339(19) 0.79856(9) 0.0393(4) Uani 1 1 d . . . C21 C 0.82137(17) 0.2977(2) 0.75526(9) 0.0460(5) Uani 1 1 d . . . C22 C 0.83944(18) 0.1880(3) 0.72336(9) 0.0528(5) Uani 1 1 d . . . C23 C 0.7696(2) 0.0834(2) 0.73390(10) 0.0528(5) Uani 1 1 d . . . C24 C 0.68118(17) 0.08930(19) 0.77760(8) 0.0414(4) Uani 1 1 d . . . C25 C 0.44701(15) 0.17890(19) 0.84137(8) 0.0376(4) Uani 1 1 d . . . C26 C 0.39291(18) 0.1669(2) 0.78333(9) 0.0508(5) Uani 1 1 d . . . H26 H 0.4320 0.1661 0.7457 0.061 Uiso 1 1 calc R . . C27 C 0.27245(18) 0.1565(2) 0.79194(9) 0.0517(5) Uani 1 1 d . . . H27 H 0.2143 0.1476 0.7614 0.062 Uiso 1 1 calc R . . C28 C 0.25291(15) 0.16205(18) 0.85593(8) 0.0374(4) Uani 1 1 d . . . C29 C 0.13924(15) 0.15186(19) 0.89199(8) 0.0376(4) Uani 1 1 d . . . C30 C 0.12549(18) 0.0122(2) 0.91348(10) 0.0481(5) Uani 1 1 d . . . H30A H 0.0535 0.0038 0.9369 0.072 Uiso 1 1 calc R . . H30B H 0.1930 -0.0111 0.9386 0.072 Uiso 1 1 calc R . . H30C H 0.1214 -0.0433 0.8783 0.072 Uiso 1 1 calc R . . C31 C 0.03298(18) 0.1865(3) 0.84993(10) 0.0586(6) Uani 1 1 d . . . H31A H -0.0400 0.1804 0.8727 0.088 Uiso 1 1 calc R . . H31B H 0.0301 0.1284 0.8158 0.088 Uiso 1 1 calc R . . H31C H 0.0425 0.2725 0.8351 0.088 Uiso 1 1 calc R . . N1 N 0.51360(13) 0.23300(14) 0.96634(7) 0.0334(3) Uani 1 1 d . . . N2 N 0.35692(13) 0.17270(17) 0.88401(7) 0.0386(4) Uani 1 1 d . . . F1 F 0.71735(12) 0.41388(11) 0.82851(6) 0.0587(3) Uani 1 1 d . . . F2 F 0.89166(12) 0.39971(14) 0.74574(7) 0.0707(4) Uani 1 1 d . . . F3 F 0.92644(14) 0.18243(19) 0.68145(7) 0.0878(5) Uani 1 1 d . . . F4 F 0.78669(15) -0.02448(17) 0.70235(8) 0.0902(5) Uani 1 1 d . . . F5 F 0.61548(12) -0.01576(12) 0.78692(6) 0.0585(3) Uani 1 1 d . . . Fe1 Fe 0.21054(2) 0.23872(2) 1.035192(11) 0.03001(8) Uani 1 1 d . . . H2A H 0.372(3) 0.190(3) 0.9193(14) 0.085(9) Uiso 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 0.0241(8) 0.0533(11) 0.0443(10) 0.0107(8) 0.0058(7) 0.0053(7) C2 0.0409(11) 0.0566(12) 0.0520(12) 0.0036(9) 0.0088(9) 0.0220(9) C3 0.0584(13) 0.0340(10) 0.0606(13) 0.0030(9) 0.0005(10) 0.0104(9) C4 0.0375(9) 0.0377(9) 0.0446(10) 0.0133(8) 0.0020(8) 0.0008(7) C5 0.0251(8) 0.0416(9) 0.0352(9) 0.0104(7) 0.0029(7) 0.0035(6) C6 0.0293(8) 0.0365(8) 0.0260(8) 0.0022(6) 0.0035(6) 0.0018(6) C7 0.0305(8) 0.0323(8) 0.0359(9) 0.0041(6) 0.0015(7) 0.0043(6) C8 0.0340(9) 0.0388(9) 0.0461(10) 0.0124(8) 0.0009(8) -0.0032(7) C9 0.0335(9) 0.0634(12) 0.0352(9) 0.0138(9) 0.0101(8) 0.0015(8) C10 0.0341(9) 0.0538(11) 0.0291(8) -0.0022(7) 0.0065(7) 0.0041(8) C11 0.0311(8) 0.0396(9) 0.0299(8) -0.0045(7) 0.0028(7) -0.0037(7) C12 0.0583(13) 0.0467(11) 0.0630(14) -0.0174(10) 0.0213(11) -0.0116(10) C13 0.0376(10) 0.0842(15) 0.0336(10) 0.0029(10) -0.0041(8) -0.0037(10) C14 0.0267(8) 0.0351(8) 0.0314(8) -0.0006(6) 0.0016(6) -0.0006(6) C15 0.0263(8) 0.0469(10) 0.0393(10) -0.0038(7) -0.0016(7) -0.0030(7) C16 0.0234(8) 0.0399(9) 0.0406(9) -0.0006(7) 0.0058(7) -0.0003(6) C17 0.0253(8) 0.0378(9) 0.0315(8) -0.0005(6) 0.0056(6) -0.0006(6) C18 0.0291(8) 0.0400(9) 0.0312(8) 0.0020(7) 0.0085(7) -0.0011(7) C19 0.0271(8) 0.0448(9) 0.0291(8) 0.0040(7) 0.0064(6) 0.0019(7) C20 0.0340(9) 0.0461(10) 0.0378(9) 0.0088(8) 0.0069(7) 0.0042(8) C21 0.0309(9) 0.0656(13) 0.0416(10) 0.0202(9) 0.0070(8) -0.0014(9) C22 0.0365(10) 0.0869(16) 0.0351(10) 0.0091(10) 0.0156(8) 0.0091(10) C23 0.0525(12) 0.0677(14) 0.0382(10) -0.0074(10) 0.0105(9) 0.0148(10) C24 0.0387(10) 0.0513(11) 0.0342(9) 0.0010(8) 0.0063(8) 0.0019(8) C25 0.0283(8) 0.0564(11) 0.0284(8) 0.0005(7) 0.0059(7) -0.0024(8) C26 0.0399(11) 0.0851(16) 0.0274(9) 0.0028(9) 0.0063(8) -0.0077(10) C27 0.0356(10) 0.0894(16) 0.0300(9) 0.0037(10) -0.0028(8) -0.0098(10) C28 0.0290(8) 0.0521(11) 0.0310(8) 0.0039(7) -0.0010(7) -0.0033(7) C29 0.0239(8) 0.0560(11) 0.0330(9) 0.0057(8) -0.0011(7) -0.0028(7) C30 0.0427(11) 0.0521(12) 0.0497(11) -0.0026(9) 0.0067(9) -0.0104(9) C31 0.0303(10) 0.0992(19) 0.0464(12) 0.0067(12) -0.0061(9) 0.0018(11) N1 0.0246(7) 0.0481(8) 0.0276(7) -0.0011(6) 0.0044(5) -0.0016(6) N2 0.0240(7) 0.0655(11) 0.0264(7) 0.0003(7) 0.0028(6) -0.0037(7) F1 0.0625(8) 0.0439(7) 0.0700(8) 0.0008(6) 0.0201(7) -0.0050(6) F2 0.0513(7) 0.0831(10) 0.0780(9) 0.0316(8) 0.0204(7) -0.0144(7) F3 0.0664(9) 0.1312(15) 0.0665(9) 0.0037(9) 0.0460(8) 0.0087(9) F4 0.1031(13) 0.0895(11) 0.0787(10) -0.0344(9) 0.0371(9) 0.0122(9) F5 0.0654(8) 0.0498(7) 0.0606(8) -0.0086(6) 0.0129(6) -0.0098(6) Fe1 0.02630(13) 0.03216(14) 0.03166(14) 0.00316(9) 0.00533(9) 0.00296(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 C1 C2 1.409(3) . ? C1 C5 1.428(3) . ? C1 Fe1 2.0450(19) . ? C1 H1 0.9300 . ? C2 C3 1.411(3) . ? C2 Fe1 2.0374(18) . ? C2 H2 0.9300 . ? C3 C4 1.416(3) . ? C3 Fe1 2.0446(19) . ? C3 H3 0.9300 . ? C4 C5 1.426(3) . ? C4 Fe1 2.0666(18) . ? C4 H4 0.9300 . ? C5 C29 1.524(3) . ? C5 Fe1 2.0852(18) . ? C6 C7 1.423(2) . ? C6 C10 1.427(2) . ? C6 C11 1.524(2) . ? C6 Fe1 2.0982(17) . ? C7 C8 1.416(2) . ? C7 Fe1 2.0692(16) . ? C7 H7 0.9300 . ? C8 C9 1.399(3) . ? C8 Fe1 2.0335(17) . ? C8 H8 0.9300 . ? C9 C10 1.416(3) . ? C9 Fe1 2.0290(18) . ? C9 H9 0.9300 . ? C10 Fe1 2.0452(19) . ? C10 H10 0.9300 . ? C11 C14 1.504(2) . ? C11 C12 1.536(3) . ? C11 C13 1.542(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N1 1.314(2) . ? C14 C15 1.432(2) . ? C15 C16 1.368(3) . ? C15 H15 0.9300 . ? C16 C17 1.415(2) . ? C16 H16 0.9300 . ? C17 N1 1.392(2) . ? C17 C18 1.396(2) . ? C18 C25 1.405(2) . ? C18 C19 1.489(2) . ? C19 C20 1.386(3) . ? C19 C24 1.387(3) . ? C20 F1 1.336(2) . ? C20 C21 1.376(3) . ? C21 F2 1.340(2) . ? C21 C22 1.355(3) . ? C22 F3 1.340(2) . ? C22 C23 1.363(3) . ? C23 F4 1.333(3) . ? C23 C24 1.378(3) . ? C24 F5 1.336(2) . ? C25 N2 1.377(2) . ? C25 C26 1.401(3) . ? C26 C27 1.366(3) . ? C26 H26 0.9300 . ? C27 C28 1.412(3) . ? C27 H27 0.9300 . ? C28 N2 1.314(2) . ? C28 C29 1.503(2) . ? C29 C31 1.537(3) . ? C29 C30 1.539(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N2 H2A 0.80(3) . ? 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 C2 C1 C5 109.12(17) . . ? C2 C1 Fe1 69.53(11) . . ? C5 C1 Fe1 71.29(10) . . ? C2 C1 H1 125.4 . . ? C5 C1 H1 125.4 . . ? Fe1 C1 H1 125.3 . . ? C1 C2 C3 107.91(18) . . ? C1 C2 Fe1 70.11(10) . . ? C3 C2 Fe1 70.05(11) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Fe1 C2 H2 125.4 . . ? C2 C3 C4 108.00(19) . . ? C2 C3 Fe1 69.50(11) . . ? C4 C3 Fe1 70.69(11) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? Fe1 C3 H3 125.4 . . ? C3 C4 C5 108.78(17) . . ? C3 C4 Fe1 69.02(11) . . ? C5 C4 Fe1 70.62(10) . . ? C3 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? Fe1 C4 H4 126.3 . . ? C4 C5 C1 106.19(17) . . ? C4 C5 C29 129.55(16) . . ? C1 C5 C29 123.53(16) . . ? C4 C5 Fe1 69.22(10) . . ? C1 C5 Fe1 68.27(11) . . ? C29 C5 Fe1 134.44(12) . . ? C7 C6 C10 106.39(15) . . ? C7 C6 C11 128.54(15) . . ? C10 C6 C11 123.42(16) . . ? C7 C6 Fe1 68.94(9) . . ? C10 C6 Fe1 67.87(10) . . ? C11 C6 Fe1 139.11(12) . . ? C8 C7 C6 108.56(16) . . ? C8 C7 Fe1 68.46(10) . . ? C6 C7 Fe1 71.14(9) . . ? C8 C7 H7 125.7 . . ? C6 C7 H7 125.7 . . ? Fe1 C7 H7 126.2 . . ? C9 C8 C7 108.38(16) . . ? C9 C8 Fe1 69.68(11) . . ? C7 C8 Fe1 71.17(10) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe1 C8 H8 124.9 . . ? C8 C9 C10 107.91(16) . . ? C8 C9 Fe1 70.03(10) . . ? C10 C9 Fe1 70.29(10) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe1 C9 H9 125.2 . . ? C9 C10 C6 108.75(16) . . ? C9 C10 Fe1 69.06(11) . . ? C6 C10 Fe1 71.87(10) . . ? C9 C10 H10 125.6 . . ? C6 C10 H10 125.6 . . ? Fe1 C10 H10 125.0 . . ? C14 C11 C6 114.28(14) . . ? C14 C11 C12 107.34(15) . . ? C6 C11 C12 111.19(15) . . ? C14 C11 C13 108.20(15) . . ? C6 C11 C13 106.05(15) . . ? C12 C11 C13 109.70(17) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 109.41(15) . . ? N1 C14 C11 123.07(15) . . ? C15 C14 C11 127.41(16) . . ? C16 C15 C14 106.96(16) . . ? C16 C15 H15 126.5 . . ? C14 C15 H15 126.5 . . ? C15 C16 C17 107.03(16) . . ? C15 C16 H16 126.5 . . ? C17 C16 H16 126.5 . . ? N1 C17 C18 120.59(15) . . ? N1 C17 C16 107.85(15) . . ? C18 C17 C16 131.55(16) . . ? C17 C18 C25 122.95(15) . . ? C17 C18 C19 118.80(15) . . ? C25 C18 C19 118.25(15) . . ? C20 C19 C24 115.96(16) . . ? C20 C19 C18 122.79(16) . . ? C24 C19 C18 121.25(16) . . ? F1 C20 C21 117.81(18) . . ? F1 C20 C19 119.99(16) . . ? C21 C20 C19 122.20(19) . . ? F2 C21 C22 120.14(18) . . ? F2 C21 C20 119.9(2) . . ? C22 C21 C20 119.90(19) . . ? F3 C22 C21 119.8(2) . . ? F3 C22 C23 120.0(2) . . ? C21 C22 C23 120.19(18) . . ? F4 C23 C22 120.33(19) . . ? F4 C23 C24 120.0(2) . . ? C22 C23 C24 119.7(2) . . ? F5 C24 C23 117.77(18) . . ? F5 C24 C19 120.16(16) . . ? C23 C24 C19 122.06(19) . . ? N2 C25 C26 106.86(16) . . ? N2 C25 C18 121.00(16) . . ? C26 C25 C18 131.97(16) . . ? C27 C26 C25 107.61(17) . . ? C27 C26 H26 126.2 . . ? C25 C26 H26 126.2 . . ? C26 C27 C28 107.02(17) . . ? C26 C27 H27 126.5 . . ? C28 C27 H27 126.5 . . ? N2 C28 C27 108.56(16) . . ? N2 C28 C29 120.82(15) . . ? C27 C28 C29 130.55(16) . . ? C28 C29 C5 111.83(15) . . ? C28 C29 C31 109.00(15) . . ? C5 C29 C31 107.83(16) . . ? C28 C29 C30 108.22(16) . . ? C5 C29 C30 110.93(15) . . ? C31 C29 C30 108.98(17) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C14 N1 C17 108.74(15) . . ? C28 N2 C25 109.90(15) . . ? C28 N2 H2A 130(2) . . ? C25 N2 H2A 119(2) . . ? C9 Fe1 C8 40.30(8) . . ? C9 Fe1 C2 102.66(8) . . ? C8 Fe1 C2 127.70(8) . . ? C9 Fe1 C3 128.29(9) . . ? C8 Fe1 C3 166.55(8) . . ? C2 Fe1 C3 40.45(9) . . ? C9 Fe1 C1 109.75(8) . . ? C8 Fe1 C1 107.00(8) . . ? C2 Fe1 C1 40.37(8) . . ? C3 Fe1 C1 67.76(8) . . ? C9 Fe1 C10 40.66(8) . . ? C8 Fe1 C10 67.84(8) . . ? C2 Fe1 C10 110.42(8) . . ? C3 Fe1 C10 107.89(8) . . ? C1 Fe1 C10 141.03(8) . . ? C9 Fe1 C4 168.56(8) . . ? C8 Fe1 C4 150.74(8) . . ? C2 Fe1 C4 67.74(8) . . ? C3 Fe1 C4 40.29(8) . . ? C1 Fe1 C4 67.42(8) . . ? C10 Fe1 C4 135.18(8) . . ? C9 Fe1 C7 67.71(7) . . ? C8 Fe1 C7 40.37(7) . . ? C2 Fe1 C7 168.07(8) . . ? C3 Fe1 C7 151.28(8) . . ? C1 Fe1 C7 134.48(7) . . ? C10 Fe1 C7 67.35(7) . . ? C4 Fe1 C7 122.58(7) . . ? C9 Fe1 C5 143.64(8) . . ? C8 Fe1 C5 116.68(7) . . ? C2 Fe1 C5 68.18(8) . . ? C3 Fe1 C5 68.02(8) . . ? C1 Fe1 C5 40.44(7) . . ? C10 Fe1 C5 175.31(7) . . ? C4 Fe1 C5 40.16(7) . . ? C7 Fe1 C5 114.99(7) . . ? C9 Fe1 C6 68.06(7) . . ? C8 Fe1 C6 67.79(7) . . ? C2 Fe1 C6 144.65(8) . . ? C3 Fe1 C6 117.86(8) . . ? C1 Fe1 C6 174.27(7) . . ? C10 Fe1 C6 40.26(7) . . ? C4 Fe1 C6 115.82(7) . . ? C7 Fe1 C6 39.92(7) . . ? C5 Fe1 C6 138.97(7) . . ? 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 C5 C1 C2 C3 -0.4(2) . . . . ? Fe1 C1 C2 C3 60.11(14) . . . . ? C5 C1 C2 Fe1 -60.54(13) . . . . ? C1 C2 C3 C4 0.3(2) . . . . ? Fe1 C2 C3 C4 60.49(14) . . . . ? C1 C2 C3 Fe1 -60.15(14) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? Fe1 C3 C4 C5 59.62(13) . . . . ? C2 C3 C4 Fe1 -59.74(14) . . . . ? C3 C4 C5 C1 -0.1(2) . . . . ? Fe1 C4 C5 C1 58.49(12) . . . . ? C3 C4 C5 C29 170.23(17) . . . . ? Fe1 C4 C5 C29 -131.14(18) . . . . ? C3 C4 C5 Fe1 -58.63(13) . . . . ? C2 C1 C5 C4 0.3(2) . . . . ? Fe1 C1 C5 C4 -59.11(12) . . . . ? C2 C1 C5 C29 -170.75(16) . . . . ? Fe1 C1 C5 C29 129.80(16) . . . . ? C2 C1 C5 Fe1 59.45(13) . . . . ? C10 C6 C7 C8 -0.67(19) . . . . ? C11 C6 C7 C8 164.80(16) . . . . ? Fe1 C6 C7 C8 -58.40(12) . . . . ? C10 C6 C7 Fe1 57.73(12) . . . . ? C11 C6 C7 Fe1 -136.79(17) . . . . ? C6 C7 C8 C9 0.1(2) . . . . ? Fe1 C7 C8 C9 -60.00(13) . . . . ? C6 C7 C8 Fe1 60.06(12) . . . . ? C7 C8 C9 C10 0.6(2) . . . . ? Fe1 C8 C9 C10 -60.35(13) . . . . ? C7 C8 C9 Fe1 60.93(12) . . . . ? C8 C9 C10 C6 -1.0(2) . . . . ? Fe1 C9 C10 C6 -61.20(13) . . . . ? C8 C9 C10 Fe1 60.19(13) . . . . ? C7 C6 C10 C9 1.0(2) . . . . ? C11 C6 C10 C9 -165.37(16) . . . . ? Fe1 C6 C10 C9 59.45(13) . . . . ? C7 C6 C10 Fe1 -58.41(11) . . . . ? C11 C6 C10 Fe1 135.18(16) . . . . ? C7 C6 C11 C14 36.7(2) . . . . ? C10 C6 C11 C14 -160.06(16) . . . . ? Fe1 C6 C11 C14 -65.9(2) . . . . ? C7 C6 C11 C12 158.40(18) . . . . ? C10 C6 C11 C12 -38.4(2) . . . . ? Fe1 C6 C11 C12 55.8(2) . . . . ? C7 C6 C11 C13 -82.4(2) . . . . ? C10 C6 C11 C13 80.8(2) . . . . ? Fe1 C6 C11 C13 175.00(16) . . . . ? C6 C11 C14 N1 21.4(2) . . . . ? C12 C11 C14 N1 -102.4(2) . . . . ? C13 C11 C14 N1 139.31(18) . . . . ? C6 C11 C14 C15 -162.68(16) . . . . ? C12 C11 C14 C15 73.5(2) . . . . ? C13 C11 C14 C15 -44.8(2) . . . . ? N1 C14 C15 C16 -0.3(2) . . . . ? C11 C14 C15 C16 -176.64(16) . . . . ? C14 C15 C16 C17 -0.12(19) . . . . ? C15 C16 C17 N1 0.47(19) . . . . ? C15 C16 C17 C18 -178.20(19) . . . . ? N1 C17 C18 C25 0.2(3) . . . . ? C16 C17 C18 C25 178.69(18) . . . . ? N1 C17 C18 C19 -179.56(15) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C17 C18 C19 C20 -59.5(2) . . . . ? C25 C18 C19 C20 120.8(2) . . . . ? C17 C18 C19 C24 119.9(2) . . . . ? C25 C18 C19 C24 -59.8(2) . . . . ? C24 C19 C20 F1 179.04(16) . . . . ? C18 C19 C20 F1 -1.5(3) . . . . ? C24 C19 C20 C21 -1.0(3) . . . . ? C18 C19 C20 C21 178.38(17) . . . . ? F1 C20 C21 F2 2.1(3) . . . . ? C19 C20 C21 F2 -177.79(17) . . . . ? F1 C20 C21 C22 -179.45(18) . . . . ? C19 C20 C21 C22 0.6(3) . . . . ? F2 C21 C22 F3 -1.2(3) . . . . ? C20 C21 C22 F3 -179.61(19) . . . . ? F2 C21 C22 C23 178.65(19) . . . . ? C20 C21 C22 C23 0.2(3) . . . . ? F3 C22 C23 F4 -0.5(3) . . . . ? C21 C22 C23 F4 179.6(2) . . . . ? F3 C22 C23 C24 179.2(2) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? F4 C23 C24 F5 0.4(3) . . . . ? C22 C23 C24 F5 -179.38(19) . . . . ? F4 C23 C24 C19 179.93(19) . . . . ? C22 C23 C24 C19 0.2(3) . . . . ? C20 C19 C24 F5 -179.82(17) . . . . ? C18 C19 C24 F5 0.7(3) . . . . ? C20 C19 C24 C23 0.6(3) . . . . ? C18 C19 C24 C23 -178.79(18) . . . . ? C17 C18 C25 N2 -4.0(3) . . . . ? C19 C18 C25 N2 175.74(17) . . . . ? C17 C18 C25 C26 170.6(2) . . . . ? C19 C18 C25 C26 -9.7(3) . . . . ? N2 C25 C26 C27 1.3(3) . . . . ? C18 C25 C26 C27 -173.9(2) . . . . ? C25 C26 C27 C28 -0.1(3) . . . . ? C26 C27 C28 N2 -1.1(3) . . . . ? C26 C27 C28 C29 -178.1(2) . . . . ? N2 C28 C29 C5 41.7(2) . . . . ? C27 C28 C29 C5 -141.6(2) . . . . ? N2 C28 C29 C31 160.9(2) . . . . ? C27 C28 C29 C31 -22.5(3) . . . . ? N2 C28 C29 C30 -80.8(2) . . . . ? C27 C28 C29 C30 95.9(2) . . . . ? C4 C5 C29 C28 18.0(2) . . . . ? C1 C5 C29 C28 -173.11(16) . . . . ? Fe1 C5 C29 C28 -81.5(2) . . . . ? C4 C5 C29 C31 -101.8(2) . . . . ? C1 C5 C29 C31 67.1(2) . . . . ? Fe1 C5 C29 C31 158.66(15) . . . . ? C4 C5 C29 C30 138.92(18) . . . . ? C1 C5 C29 C30 -52.2(2) . . . . ? Fe1 C5 C29 C30 39.4(2) . . . . ? C15 C14 N1 C17 0.60(19) . . . . ? C11 C14 N1 C17 177.13(15) . . . . ? C18 C17 N1 C14 178.17(16) . . . . ? C16 C17 N1 C14 -0.67(19) . . . . ? C27 C28 N2 C25 2.0(2) . . . . ? C29 C28 N2 C25 179.28(17) . . . . ? C26 C25 N2 C28 -2.0(2) . . . . ? C18 C25 N2 C28 173.78(18) . . . . ? C10 C9 Fe1 C8 118.55(16) . . . . ? C8 C9 Fe1 C2 134.75(12) . . . . ? C10 C9 Fe1 C2 -106.70(12) . . . . ? C8 C9 Fe1 C3 170.03(12) . . . . ? C10 C9 Fe1 C3 -71.42(14) . . . . ? C8 C9 Fe1 C1 93.26(12) . . . . ? C10 C9 Fe1 C1 -148.19(11) . . . . ? C8 C9 Fe1 C10 -118.55(16) . . . . ? C8 C9 Fe1 C4 166.8(4) . . . . ? C10 C9 Fe1 C4 -74.6(4) . . . . ? C8 C9 Fe1 C7 -37.84(11) . . . . ? C10 C9 Fe1 C7 80.70(11) . . . . ? C8 C9 Fe1 C5 64.47(16) . . . . ? C10 C9 Fe1 C5 -176.99(11) . . . . ? C8 C9 Fe1 C6 -81.08(11) . . . . ? C10 C9 Fe1 C6 37.47(10) . . . . ? C7 C8 Fe1 C9 -118.79(16) . . . . ? C9 C8 Fe1 C2 -61.12(15) . . . . ? C7 C8 Fe1 C2 -179.91(11) . . . . ? C9 C8 Fe1 C3 -35.7(4) . . . . ? C7 C8 Fe1 C3 -154.5(3) . . . . ? C9 C8 Fe1 C1 -100.71(12) . . . . ? C7 C8 Fe1 C1 140.50(11) . . . . ? C9 C8 Fe1 C10 38.17(11) . . . . ? C7 C8 Fe1 C10 -80.62(11) . . . . ? C9 C8 Fe1 C4 -174.69(14) . . . . ? C7 C8 Fe1 C4 66.52(19) . . . . ? C9 C8 Fe1 C7 118.79(16) . . . . ? C9 C8 Fe1 C5 -143.23(11) . . . . ? C7 C8 Fe1 C5 97.98(11) . . . . ? C9 C8 Fe1 C6 81.80(12) . . . . ? C7 C8 Fe1 C6 -36.99(10) . . . . ? C1 C2 Fe1 C9 -105.69(13) . . . . ? C3 C2 Fe1 C9 135.68(13) . . . . ? C1 C2 Fe1 C8 -70.20(15) . . . . ? C3 C2 Fe1 C8 171.16(12) . . . . ? C1 C2 Fe1 C3 118.63(18) . . . . ? C3 C2 Fe1 C1 -118.63(18) . . . . ? C1 C2 Fe1 C10 -147.44(11) . . . . ? C3 C2 Fe1 C10 93.93(14) . . . . ? C1 C2 Fe1 C4 80.84(12) . . . . ? C3 C2 Fe1 C4 -37.79(13) . . . . ? C1 C2 Fe1 C7 -70.5(4) . . . . ? C3 C2 Fe1 C7 170.9(3) . . . . ? C1 C2 Fe1 C5 37.36(11) . . . . ? C3 C2 Fe1 C5 -81.27(13) . . . . ? C1 C2 Fe1 C6 -175.49(11) . . . . ? C3 C2 Fe1 C6 65.88(18) . . . . ? C2 C3 Fe1 C9 -60.29(17) . . . . ? C4 C3 Fe1 C9 -179.01(11) . . . . ? C2 C3 Fe1 C8 -31.5(4) . . . . ? C4 C3 Fe1 C8 -150.2(3) . . . . ? C4 C3 Fe1 C2 -118.72(19) . . . . ? C2 C3 Fe1 C1 37.89(13) . . . . ? C4 C3 Fe1 C1 -80.83(13) . . . . ? C2 C3 Fe1 C10 -100.76(14) . . . . ? C4 C3 Fe1 C10 140.52(12) . . . . ? C2 C3 Fe1 C4 118.72(19) . . . . ? C2 C3 Fe1 C7 -176.10(14) . . . . ? C4 C3 Fe1 C7 65.2(2) . . . . ? C2 C3 Fe1 C5 81.70(14) . . . . ? C4 C3 Fe1 C5 -37.02(11) . . . . ? C2 C3 Fe1 C6 -143.33(12) . . . . ? C4 C3 Fe1 C6 97.95(13) . . . . ? C2 C1 Fe1 C9 86.41(13) . . . . ? C5 C1 Fe1 C9 -153.88(11) . . . . ? C2 C1 Fe1 C8 128.88(12) . . . . ? C5 C1 Fe1 C8 -111.41(11) . . . . ? C5 C1 Fe1 C2 119.71(16) . . . . ? C2 C1 Fe1 C3 -37.97(12) . . . . ? C5 C1 Fe1 C3 81.74(11) . . . . ? C2 C1 Fe1 C10 53.31(17) . . . . ? C5 C1 Fe1 C10 173.02(12) . . . . ? C2 C1 Fe1 C4 -81.71(13) . . . . ? C5 C1 Fe1 C4 38.00(10) . . . . ? C2 C1 Fe1 C7 164.15(12) . . . . ? C5 C1 Fe1 C7 -76.14(13) . . . . ? C2 C1 Fe1 C5 -119.71(16) . . . . ? C2 C1 Fe1 C6 152.9(6) . . . . ? C5 C1 Fe1 C6 -87.4(7) . . . . ? C6 C10 Fe1 C9 119.17(15) . . . . ? C9 C10 Fe1 C8 -37.84(11) . . . . ? C6 C10 Fe1 C8 81.33(11) . . . . ? C9 C10 Fe1 C2 85.72(13) . . . . ? C6 C10 Fe1 C2 -155.10(11) . . . . ? C9 C10 Fe1 C3 128.58(12) . . . . ? C6 C10 Fe1 C3 -112.25(12) . . . . ? C9 C10 Fe1 C1 52.07(17) . . . . ? C6 C10 Fe1 C1 171.24(12) . . . . ? C9 C10 Fe1 C4 164.26(12) . . . . ? C6 C10 Fe1 C4 -76.56(14) . . . . ? C9 C10 Fe1 C7 -81.67(12) . . . . ? C6 C10 Fe1 C7 37.51(10) . . . . ? C9 C10 Fe1 C5 157.6(8) . . . . ? C6 C10 Fe1 C5 -83.2(8) . . . . ? C9 C10 Fe1 C6 -119.17(15) . . . . ? C3 C4 Fe1 C9 3.9(4) . . . . ? C5 C4 Fe1 C9 -116.1(4) . . . . ? C3 C4 Fe1 C8 166.34(15) . . . . ? C5 C4 Fe1 C8 46.31(19) . . . . ? C3 C4 Fe1 C2 37.94(13) . . . . ? C5 C4 Fe1 C2 -82.09(12) . . . . ? C5 C4 Fe1 C3 -120.03(17) . . . . ? C3 C4 Fe1 C1 81.77(13) . . . . ? C5 C4 Fe1 C1 -38.26(11) . . . . ? C3 C4 Fe1 C10 -59.13(16) . . . . ? C5 C4 Fe1 C10 -179.16(10) . . . . ? C3 C4 Fe1 C7 -148.83(12) . . . . ? C5 C4 Fe1 C7 91.14(12) . . . . ? C3 C4 Fe1 C5 120.03(17) . . . . ? C3 C4 Fe1 C6 -103.42(13) . . . . ? C5 C4 Fe1 C6 136.56(10) . . . . ? C8 C7 Fe1 C9 37.78(12) . . . . ? C6 C7 Fe1 C9 -81.99(11) . . . . ? C6 C7 Fe1 C8 -119.76(15) . . . . ? C8 C7 Fe1 C2 0.3(4) . . . . ? C6 C7 Fe1 C2 -119.4(4) . . . . ? C8 C7 Fe1 C3 167.99(16) . . . . ? C6 C7 Fe1 C3 48.2(2) . . . . ? C8 C7 Fe1 C1 -58.49(15) . . . . ? C6 C7 Fe1 C1 -178.26(10) . . . . ? C8 C7 Fe1 C10 81.94(12) . . . . ? C6 C7 Fe1 C10 -37.82(10) . . . . ? C8 C7 Fe1 C4 -147.86(12) . . . . ? C6 C7 Fe1 C4 92.38(11) . . . . ? C8 C7 Fe1 C5 -102.51(12) . . . . ? C6 C7 Fe1 C5 137.73(10) . . . . ? C8 C7 Fe1 C6 119.76(15) . . . . ? C4 C5 Fe1 C9 162.52(13) . . . . ? C1 C5 Fe1 C9 44.34(17) . . . . ? C29 C5 Fe1 C9 -71.9(2) . . . . ? C4 C5 Fe1 C8 -156.70(11) . . . . ? C1 C5 Fe1 C8 85.11(12) . . . . ? C29 C5 Fe1 C8 -31.12(19) . . . . ? C4 C5 Fe1 C2 80.89(12) . . . . ? C1 C5 Fe1 C2 -37.30(11) . . . . ? C29 C5 Fe1 C2 -153.53(19) . . . . ? C4 C5 Fe1 C3 37.14(11) . . . . ? C1 C5 Fe1 C3 -81.05(12) . . . . ? C29 C5 Fe1 C3 162.72(19) . . . . ? C4 C5 Fe1 C1 118.19(15) . . . . ? C29 C5 Fe1 C1 -116.2(2) . . . . ? C4 C5 Fe1 C10 7.3(9) . . . . ? C1 C5 Fe1 C10 -110.9(8) . . . . ? C29 C5 Fe1 C10 132.8(8) . . . . ? C1 C5 Fe1 C4 -118.19(15) . . . . ? C29 C5 Fe1 C4 125.6(2) . . . . ? C4 C5 Fe1 C7 -111.65(11) . . . . ? C1 C5 Fe1 C7 130.16(11) . . . . ? C29 C5 Fe1 C7 13.93(19) . . . . ? C4 C5 Fe1 C6 -70.55(14) . . . . ? C1 C5 Fe1 C6 171.27(11) . . . . ? C29 C5 Fe1 C6 55.0(2) . . . . ? C7 C6 Fe1 C9 81.04(11) . . . . ? C10 C6 Fe1 C9 -37.83(11) . . . . ? C11 C6 Fe1 C9 -153.8(2) . . . . ? C7 C6 Fe1 C8 37.40(10) . . . . ? C10 C6 Fe1 C8 -81.47(12) . . . . ? C11 C6 Fe1 C8 162.5(2) . . . . ? C7 C6 Fe1 C2 161.87(13) . . . . ? C10 C6 Fe1 C2 42.99(18) . . . . ? C11 C6 Fe1 C2 -73.0(2) . . . . ? C7 C6 Fe1 C3 -156.09(11) . . . . ? C10 C6 Fe1 C3 85.04(13) . . . . ? C11 C6 Fe1 C3 -31.0(2) . . . . ? C7 C6 Fe1 C1 12.6(7) . . . . ? C10 C6 Fe1 C1 -106.3(7) . . . . ? C11 C6 Fe1 C1 137.7(6) . . . . ? C7 C6 Fe1 C10 118.87(15) . . . . ? C11 C6 Fe1 C10 -116.0(2) . . . . ? C7 C6 Fe1 C4 -110.73(11) . . . . ? C10 C6 Fe1 C4 130.40(11) . . . . ? C11 C6 Fe1 C4 14.4(2) . . . . ? C10 C6 Fe1 C7 -118.87(15) . . . . ? C11 C6 Fe1 C7 125.1(2) . . . . ? C7 C6 Fe1 C5 -68.24(14) . . . . ? C10 C6 Fe1 C5 172.89(11) . . . . ? C11 C6 Fe1 C5 56.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A N1 0.80(3) 1.93(3) 2.573(2) 136(3) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.341 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.062 # Attachment 'Fe-Calix-p-NO2_3a_.cif' data_rk283 _database_code_depnum_ccdc_archive 'CCDC 732748' #TrackingRef 'Fe-Calix-p-NO2_3a_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C51 H37 Fe N3 O2, C H1 Cl3, C7 H16' _chemical_formula_sum 'C59 H54 Cl3 Fe N3 O2' _chemical_formula_weight 999.25 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8374(12) _cell_length_b 25.707(3) _cell_length_c 18.728(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.443(3) _cell_angle_gamma 90.00 _cell_volume 5029.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2460 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 22.5 _exptl_crystal_description Prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.8630 _exptl_absorpt_correction_T_max 0.9056 _exptl_special_details ; Lattice solvent molecules N-heptane and CHCL3 located from The difference Fiurier map showed higher temperature factor indicating the presence of dynamic disorder. However, the peaks obtained from the Difference Fourier map for both the lattice solvent molecules were so weak and diffused modeling of these molecules were difficult.DFIX and DANG constraints were applied to fix the C-C distance(1.52A) for the N-heptane and C-Cl distance (1.74A) for CHCL3 molecule for better geometry and bond lengths. Both these lattice solvents were refined only isotropicaly.It was also observed that the the nitro group attached to the phenyl ring showed higher temperature factor.Attempts made to model the whole C6H4-NO2 fragmnet yeilded no much promising results.Hence the Nitro group attached to the phenyl ring is kept isotropic during the refinemet. C-C bond lengths of the phenyl ring, C-N and N-O distances are also restrained to appropriate lengths. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46883 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8837 _reflns_number_gt 7027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.1411P)^2^+14.3730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8837 _refine_ls_number_parameters 548 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.2615 _refine_ls_wR_factor_gt 0.2433 _refine_ls_goodness_of_fit_ref 1.032 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1471(4) 0.19104(19) 0.4410(2) 0.0362(10) Uani 1 d . . . H1 H 0.1302 0.1585 0.4190 0.043 Uiso 1 calc R . . C2 C 0.1356(4) 0.23958(17) 0.4025(2) 0.0326(9) Uani 1 d . . . C3 C 0.1703(4) 0.27892(19) 0.4580(3) 0.0405(11) Uani 1 d . . . H3 H 0.1720 0.3145 0.4492 0.049 Uiso 1 calc R . . C4 C 0.2018(5) 0.2551(2) 0.5285(3) 0.0456(12) Uani 1 d . . . H4 H 0.2268 0.2723 0.5737 0.055 Uiso 1 calc R . . C5 C 0.1890(4) 0.2009(2) 0.5191(3) 0.0412(11) Uani 1 d . . . H5 H 0.2048 0.1760 0.5566 0.049 Uiso 1 calc R . . C6 C 0.4880(5) 0.26854(18) 0.5110(3) 0.0424(11) Uani 1 d . . . H6 H 0.4973 0.2985 0.5398 0.051 Uiso 1 calc R . . C7 C 0.4985(4) 0.21681(19) 0.5378(3) 0.0386(10) Uani 1 d . . . H7 H 0.5155 0.2072 0.5873 0.046 Uiso 1 calc R . . C8 C 0.4787(4) 0.18190(17) 0.4767(2) 0.0327(9) Uani 1 d . . . C9 C 0.4561(4) 0.21367(19) 0.4114(3) 0.0381(10) Uani 1 d . . . H9 H 0.4408 0.2014 0.3631 0.046 Uiso 1 calc R . . C10 C 0.4608(5) 0.26667(19) 0.4325(3) 0.0427(11) Uani 1 d . . . H10 H 0.4484 0.2951 0.4007 0.051 Uiso 1 calc R . . C11 C 0.0719(4) 0.25003(17) 0.3199(2) 0.0324(9) Uani 1 d . . . C12 C -0.0686(4) 0.26712(17) 0.3117(3) 0.0357(10) Uani 1 d . . . C13 C -0.1305(5) 0.2554(2) 0.3652(3) 0.0546(14) Uani 1 d . . . H13 H -0.0867 0.2379 0.4078 0.065 Uiso 1 calc R . . C14 C -0.2570(6) 0.2696(3) 0.3561(4) 0.0715(19) Uani 1 d . . . H14 H -0.2973 0.2616 0.3928 0.086 Uiso 1 calc R . . C15 C -0.3234(5) 0.2952(3) 0.2935(4) 0.0690(17) Uani 1 d . . . H15 H -0.4083 0.3047 0.2878 0.083 Uiso 1 calc R . . C16 C -0.2639(5) 0.3069(2) 0.2392(3) 0.0594(15) Uani 1 d . . . H16 H -0.3088 0.3237 0.1961 0.071 Uiso 1 calc R . . C17 C -0.1360(5) 0.2934(2) 0.2488(3) 0.0460(12) Uani 1 d . . . H17 H -0.0953 0.3021 0.2126 0.055 Uiso 1 calc R . . C18 C 0.1476(4) 0.29335(18) 0.2921(2) 0.0350(10) Uani 1 d . . . C19 C 0.1357(5) 0.34484(19) 0.3106(3) 0.0455(11) Uani 1 d . . . H19 H 0.0789 0.3536 0.3382 0.055 Uiso 1 calc R . . C20 C 0.2065(6) 0.3835(2) 0.2888(3) 0.0561(14) Uani 1 d . . . H20 H 0.1979 0.4178 0.3022 0.067 Uiso 1 calc R . . C21 C 0.2901(6) 0.3712(3) 0.2472(3) 0.0618(16) Uani 1 d . . . H21 H 0.3387 0.3971 0.2329 0.074 Uiso 1 calc R . . C22 C 0.3008(5) 0.3206(3) 0.2273(3) 0.0585(15) Uani 1 d . . . H22 H 0.3557 0.3122 0.1984 0.070 Uiso 1 calc R . . C23 C 0.2310(5) 0.2820(2) 0.2494(3) 0.0465(12) Uani 1 d . . . H23 H 0.2400 0.2478 0.2356 0.056 Uiso 1 calc R . . C24 C 0.0687(4) 0.20159(17) 0.2728(2) 0.0352(10) Uani 1 d . . . C25 C -0.0165(5) 0.1880(2) 0.2039(3) 0.0488(12) Uani 1 d . . . H25 H -0.0886 0.2067 0.1788 0.059 Uiso 1 calc R . . C26 C 0.0259(5) 0.1428(2) 0.1808(3) 0.0474(12) Uani 1 d . . . H26 H -0.0113 0.1250 0.1372 0.057 Uiso 1 calc R . . C27 C 0.1365(5) 0.12814(18) 0.2356(2) 0.0395(10) Uani 1 d . . . C28 C 0.2190(5) 0.08495(18) 0.2409(3) 0.0405(11) Uani 1 d . . . C29 C 0.3257(5) 0.07693(18) 0.3009(3) 0.0401(10) Uani 1 d . . . C30 C 0.4175(5) 0.03600(19) 0.3188(3) 0.0472(12) Uani 1 d . . . H30 H 0.4215 0.0069 0.2901 0.057 Uiso 1 calc R . . C31 C 0.4980(5) 0.04756(19) 0.3860(3) 0.0440(11) Uani 1 d . . . H31 H 0.5673 0.0276 0.4116 0.053 Uiso 1 calc R . . C32 C 0.4579(4) 0.09506(18) 0.4099(2) 0.0359(10) Uani 1 d . . . C33 C 0.5015(4) 0.12267(17) 0.4841(2) 0.0331(9) Uani 1 d . . . C34 C 0.4247(4) 0.10026(17) 0.5360(3) 0.0345(10) Uani 1 d . . . C35 C 0.3093(4) 0.07428(19) 0.5083(3) 0.0421(11) Uani 1 d . . . H35 H 0.2785 0.0691 0.4575 0.051 Uiso 1 calc R . . C36 C 0.2399(5) 0.0561(2) 0.5547(3) 0.0474(12) Uani 1 d . . . H36 H 0.1627 0.0390 0.5350 0.057 Uiso 1 calc R . . C37 C 0.2835(5) 0.0629(2) 0.6302(3) 0.0521(13) Uani 1 d . . . H37 H 0.2358 0.0507 0.6613 0.063 Uiso 1 calc R . . C38 C 0.3981(5) 0.0878(2) 0.6590(3) 0.0473(12) Uani 1 d . . . H38 H 0.4283 0.0925 0.7100 0.057 Uiso 1 calc R . . C39 C 0.4690(5) 0.10600(19) 0.6126(3) 0.0415(11) Uani 1 d . . . H39 H 0.5471 0.1223 0.6329 0.050 Uiso 1 calc R . . C40 C 0.6471(4) 0.11282(18) 0.5164(3) 0.0381(10) Uani 1 d . . . C41 C 0.6896(5) 0.0657(2) 0.5506(3) 0.0498(13) Uani 1 d . . . H41 H 0.6304 0.0404 0.5546 0.060 Uiso 1 calc R . . C42 C 0.8198(6) 0.0559(3) 0.5791(4) 0.0660(17) Uani 1 d . . . H42 H 0.8475 0.0244 0.6024 0.079 Uiso 1 calc R . . C43 C 0.9075(6) 0.0932(3) 0.5725(4) 0.076(2) Uani 1 d . . . H43 H 0.9947 0.0869 0.5911 0.091 Uiso 1 calc R . . C44 C 0.8660(5) 0.1394(3) 0.5385(4) 0.0711(18) Uani 1 d . . . H44 H 0.9254 0.1645 0.5344 0.085 Uiso 1 calc R . . C45 C 0.7374(5) 0.1491(2) 0.5103(3) 0.0539(13) Uani 1 d . . . H45 H 0.7110 0.1806 0.4868 0.065 Uiso 1 calc R . . C46 C 0.1888(5) 0.04531(17) 0.1805(2) 0.0460(11) Uani 1 d DU . . C47 C 0.2744(6) 0.0360(2) 0.1381(3) 0.0656(16) Uani 1 d DU . . H47 H 0.3497 0.0552 0.1467 0.079 Uiso 1 calc R . . C48 C 0.2481(7) -0.0014(2) 0.0835(3) 0.0794(19) Uani 1 d DU . . H48 H 0.3055 -0.0074 0.0552 0.095 Uiso 1 calc R . . C49 C 0.1379(6) -0.0298(2) 0.0708(3) 0.0717(18) Uani 1 d DU . . C50 C 0.0519(7) -0.0215(2) 0.1114(3) 0.0780(19) Uani 1 d DU . . H50 H -0.0229 -0.0411 0.1026 0.094 Uiso 1 calc R . . C51 C 0.0781(6) 0.0166(2) 0.1663(3) 0.0641(15) Uani 1 d DU . . H51 H 0.0195 0.0227 0.1938 0.077 Uiso 1 calc R . . C52 C 0.8462(13) 0.3994(7) 0.3997(8) 0.218(8) Uiso 1 d D . . H52 H 0.8516 0.3685 0.3702 0.262 Uiso 1 calc R . . C53 C 0.3755(17) 0.2035(8) 0.0899(9) 0.221(8) Uiso 1 d D . . H53A H 0.3102 0.2280 0.0929 0.331 Uiso 1 calc R . . H53B H 0.3363 0.1727 0.0649 0.331 Uiso 1 calc R . . H53C H 0.4304 0.2187 0.0630 0.331 Uiso 1 calc R . . C54 C 0.4544(15) 0.1894(7) 0.1682(9) 0.181(6) Uiso 1 d D . . H54A H 0.4904 0.2213 0.1926 0.217 Uiso 1 calc R . . H54B H 0.3959 0.1759 0.1949 0.217 Uiso 1 calc R . . C55 C 0.5633(14) 0.1503(6) 0.1770(8) 0.180(6) Uiso 1 d D . . H55A H 0.6201 0.1624 0.1482 0.216 Uiso 1 calc R . . H55B H 0.5275 0.1174 0.1560 0.216 Uiso 1 calc R . . C56 C 0.6429(15) 0.1409(7) 0.2567(8) 0.189(6) Uiso 1 d D . . H56A H 0.5865 0.1308 0.2868 0.227 Uiso 1 calc R . . H56B H 0.6855 0.1729 0.2768 0.227 Uiso 1 calc R . . C57 C 0.7441(14) 0.0979(6) 0.2608(8) 0.169(5) Uiso 1 d D . . H57A H 0.7034 0.0646 0.2461 0.202 Uiso 1 calc R . . H57B H 0.7985 0.1061 0.2287 0.202 Uiso 1 calc R . . C58 C 0.8221(15) 0.0969(7) 0.3420(9) 0.205(7) Uiso 1 d D . . H58A H 0.8530 0.1316 0.3574 0.245 Uiso 1 calc R . . H58B H 0.7677 0.0858 0.3728 0.245 Uiso 1 calc R . . C59 C 0.9353(11) 0.0599(5) 0.3529(7) 0.131(4) Uiso 1 d D . . H59A H 0.9829 0.0598 0.4041 0.196 Uiso 1 calc R . . H59B H 0.9898 0.0711 0.3230 0.196 Uiso 1 calc R . . H59C H 0.9047 0.0254 0.3384 0.196 Uiso 1 calc R . . N1 N 0.1585(4) 0.16582(16) 0.2902(2) 0.0381(9) Uani 1 d . . . N2 N 0.3562(4) 0.11230(15) 0.3588(2) 0.0391(9) Uani 1 d . . . H1A H 0.216(6) 0.165(3) 0.315(4) 0.06(2) Uiso 1 d . . . N3 N 0.1127(7) -0.0719(3) 0.0138(4) 0.0932(19) Uiso 1 d D . . O1 O 0.0154(7) -0.0948(3) 0.0076(4) 0.120(2) Uiso 1 d D . . O2 O 0.1910(8) -0.0777(3) -0.0192(5) 0.138(3) Uiso 1 d D . . Fe1 Fe 0.32110(6) 0.22915(2) 0.46830(3) 0.0315(2) Uani 1 d . . . Cl1 Cl 0.8281(11) 0.4570(5) 0.3497(7) 0.412(6) Uiso 1 d D . . Cl2 Cl 0.9863(8) 0.4122(3) 0.4692(5) 0.305(4) Uiso 1 d D . . Cl3 Cl 0.7303(7) 0.3951(3) 0.4481(4) 0.282(3) Uiso 1 d 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 0.032(2) 0.041(2) 0.035(2) 0.0020(19) 0.0073(18) -0.0009(18) C2 0.030(2) 0.034(2) 0.033(2) -0.0033(18) 0.0049(18) 0.0042(17) C3 0.038(2) 0.041(3) 0.040(3) -0.004(2) 0.005(2) 0.012(2) C4 0.041(3) 0.064(3) 0.030(2) -0.010(2) 0.006(2) 0.012(2) C5 0.038(2) 0.055(3) 0.032(2) 0.005(2) 0.011(2) 0.007(2) C6 0.041(3) 0.035(2) 0.047(3) -0.006(2) 0.004(2) -0.003(2) C7 0.032(2) 0.043(3) 0.036(2) -0.005(2) 0.0011(19) -0.0001(19) C8 0.026(2) 0.035(2) 0.035(2) -0.0053(18) 0.0042(17) 0.0009(17) C9 0.035(2) 0.043(3) 0.036(2) -0.002(2) 0.0090(19) 0.0001(19) C10 0.040(3) 0.037(3) 0.051(3) 0.004(2) 0.012(2) -0.002(2) C11 0.031(2) 0.031(2) 0.033(2) -0.0010(18) 0.0048(18) 0.0026(17) C12 0.031(2) 0.035(2) 0.039(2) -0.0022(19) 0.0047(19) 0.0009(18) C13 0.040(3) 0.067(4) 0.057(3) 0.015(3) 0.012(2) 0.005(3) C14 0.040(3) 0.101(5) 0.079(4) 0.016(4) 0.024(3) 0.004(3) C15 0.035(3) 0.087(5) 0.083(5) 0.010(4) 0.013(3) 0.009(3) C16 0.041(3) 0.068(4) 0.061(4) 0.007(3) -0.002(3) 0.013(3) C17 0.039(3) 0.049(3) 0.047(3) 0.004(2) 0.006(2) 0.009(2) C18 0.033(2) 0.037(2) 0.030(2) 0.0021(18) 0.0004(18) -0.0003(18) C19 0.049(3) 0.039(3) 0.044(3) -0.002(2) 0.004(2) 0.000(2) C20 0.059(3) 0.041(3) 0.058(3) 0.002(2) -0.003(3) -0.010(2) C21 0.054(3) 0.067(4) 0.056(3) 0.018(3) 0.002(3) -0.022(3) C22 0.045(3) 0.079(4) 0.053(3) 0.016(3) 0.017(3) -0.004(3) C23 0.043(3) 0.053(3) 0.044(3) 0.003(2) 0.012(2) 0.003(2) C24 0.039(2) 0.033(2) 0.031(2) 0.0006(18) 0.0032(18) 0.0013(19) C25 0.053(3) 0.042(3) 0.040(3) -0.003(2) -0.009(2) 0.010(2) C26 0.059(3) 0.042(3) 0.032(2) -0.008(2) -0.003(2) 0.002(2) C27 0.053(3) 0.031(2) 0.029(2) -0.0047(18) 0.002(2) -0.001(2) C28 0.052(3) 0.032(2) 0.034(2) -0.0033(19) 0.006(2) -0.001(2) C29 0.047(3) 0.033(2) 0.037(2) -0.0078(19) 0.005(2) 0.002(2) C30 0.058(3) 0.036(3) 0.045(3) -0.007(2) 0.009(2) 0.009(2) C31 0.045(3) 0.039(3) 0.044(3) -0.002(2) 0.004(2) 0.013(2) C32 0.033(2) 0.037(2) 0.034(2) -0.0032(19) 0.0041(19) 0.0042(18) C33 0.027(2) 0.034(2) 0.035(2) -0.0033(18) 0.0037(18) 0.0041(17) C34 0.032(2) 0.029(2) 0.040(2) -0.0001(18) 0.0042(19) 0.0055(17) C35 0.034(2) 0.041(3) 0.047(3) -0.008(2) 0.004(2) 0.001(2) C36 0.037(2) 0.042(3) 0.062(3) -0.005(2) 0.010(2) -0.003(2) C37 0.048(3) 0.051(3) 0.061(3) -0.001(3) 0.022(3) -0.002(2) C38 0.052(3) 0.046(3) 0.044(3) 0.002(2) 0.012(2) 0.001(2) C39 0.038(2) 0.041(3) 0.042(3) -0.002(2) 0.005(2) 0.000(2) C40 0.027(2) 0.043(3) 0.040(2) -0.008(2) 0.0018(18) 0.0054(19) C41 0.040(3) 0.051(3) 0.053(3) -0.006(2) 0.002(2) 0.015(2) C42 0.048(3) 0.076(4) 0.064(4) -0.011(3) -0.003(3) 0.032(3) C43 0.033(3) 0.109(6) 0.078(4) -0.025(4) 0.002(3) 0.023(3) C44 0.034(3) 0.099(5) 0.080(4) -0.007(4) 0.016(3) -0.005(3) C45 0.035(3) 0.066(4) 0.061(3) -0.001(3) 0.013(2) 0.000(2) C46 0.066(3) 0.030(2) 0.033(2) -0.0033(19) -0.002(2) 0.007(2) C47 0.096(4) 0.055(3) 0.048(3) -0.013(3) 0.024(3) -0.003(3) C48 0.126(6) 0.063(4) 0.048(3) -0.015(3) 0.022(4) 0.017(4) C49 0.108(5) 0.046(3) 0.043(3) -0.015(3) -0.013(3) 0.027(3) C50 0.085(4) 0.054(4) 0.074(4) -0.021(3) -0.015(3) -0.003(3) C51 0.069(4) 0.053(3) 0.062(4) -0.023(3) 0.003(3) -0.002(3) N1 0.040(2) 0.036(2) 0.032(2) -0.0074(17) -0.0020(19) 0.0056(18) N2 0.043(2) 0.037(2) 0.033(2) -0.0091(16) 0.0013(17) 0.0059(17) Fe1 0.0313(4) 0.0319(4) 0.0295(4) -0.0023(2) 0.0050(3) 0.0028(2) _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 C2 1.430(6) . ? C1 C5 1.434(6) . ? C1 Fe1 2.065(4) . ? C1 H1 0.9300 . ? C2 C3 1.427(6) . ? C2 C11 1.540(6) . ? C2 Fe1 2.077(4) . ? C3 C4 1.413(7) . ? C3 Fe1 2.043(4) . ? C3 H3 0.9300 . ? C4 C5 1.406(8) . ? C4 Fe1 2.040(5) . ? C4 H4 0.9300 . ? C5 Fe1 2.051(5) . ? C5 H5 0.9300 . ? C6 C7 1.415(7) . ? C6 C10 1.422(7) . ? C6 Fe1 2.041(5) . ? C6 H6 0.9300 . ? C7 C8 1.424(6) . ? C7 Fe1 2.039(4) . ? C7 H7 0.9300 . ? C8 C9 1.437(6) . ? C8 C33 1.543(6) . ? C8 Fe1 2.068(4) . ? C9 C10 1.416(7) . ? C9 Fe1 2.065(5) . ? C9 H9 0.9300 . ? C10 Fe1 2.053(5) . ? C10 H10 0.9300 . ? C11 C24 1.522(6) . ? C11 C12 1.553(6) . ? C11 C18 1.553(6) . ? C12 C13 1.378(7) . ? C12 C17 1.385(7) . ? C13 C14 1.385(8) . ? C13 H13 0.9300 . ? C14 C15 1.370(9) . ? C14 H14 0.9300 . ? C15 C16 1.375(9) . ? C15 H15 0.9300 . ? C16 C17 1.394(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.383(7) . ? C18 C23 1.388(7) . ? C19 C20 1.382(8) . ? C19 H19 0.9300 . ? C20 C21 1.380(9) . ? C20 H20 0.9300 . ? C21 C22 1.366(9) . ? C21 H21 0.9300 . ? C22 C23 1.377(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N1 1.316(6) . ? C24 C25 1.416(6) . ? C25 C26 1.362(7) . ? C25 H25 0.9300 . ? C26 C27 1.406(7) . ? C26 H26 0.9300 . ? C27 N1 1.382(6) . ? C27 C28 1.412(7) . ? C28 C29 1.396(7) . ? C28 C46 1.492(6) . ? C29 N2 1.386(6) . ? C29 C30 1.425(7) . ? C30 C31 1.358(7) . ? C30 H30 0.9300 . ? C31 C32 1.409(6) . ? C31 H31 0.9300 . ? C32 N2 1.329(6) . ? C32 C33 1.518(6) . ? C33 C34 1.549(6) . ? C33 C40 1.552(6) . ? C34 C35 1.391(6) . ? C34 C39 1.395(7) . ? C35 C36 1.374(7) . ? C35 H35 0.9300 . ? C36 C37 1.376(8) . ? C36 H36 0.9300 . ? C37 C38 1.375(8) . ? C37 H37 0.9300 . ? C38 C39 1.385(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.379(7) . ? C40 C41 1.391(7) . ? C41 C42 1.392(7) . ? C41 H41 0.9300 . ? C42 C43 1.378(10) . ? C42 H42 0.9300 . ? C43 C44 1.366(10) . ? C43 H43 0.9300 . ? C44 C45 1.375(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.374(6) . ? C46 C47 1.393(6) . ? C47 C48 1.379(6) . ? C47 H47 0.9300 . ? C48 C49 1.365(7) . ? C48 H48 0.9300 . ? C49 C50 1.368(7) . ? C49 N3 1.493(8) . ? C50 C51 1.393(6) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 Cl1 1.735(12) . ? C52 Cl3 1.738(12) . ? C52 Cl2 1.748(12) . ? C52 H52 0.9800 . ? C53 C54 1.531(12) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.525(12) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.532(12) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.544(12) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.532(12) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.523(12) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? N1 H1A 0.67(6) . ? N3 O1 1.185(8) . ? N3 O2 1.186(8) . ? 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 C2 C1 C5 108.8(4) . . ? C2 C1 Fe1 70.3(2) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 H1 125.6 . . ? C5 C1 H1 125.6 . . ? Fe1 C1 H1 126.6 . . ? C3 C2 C1 106.3(4) . . ? C3 C2 C11 124.6(4) . . ? C1 C2 C11 127.9(4) . . ? C3 C2 Fe1 68.5(2) . . ? C1 C2 Fe1 69.3(2) . . ? C11 C2 Fe1 136.3(3) . . ? C4 C3 C2 108.9(4) . . ? C4 C3 Fe1 69.6(3) . . ? C2 C3 Fe1 71.0(2) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 125.4 . . ? C5 C4 C3 108.8(4) . . ? C5 C4 Fe1 70.3(3) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 H4 125.6 . . ? C3 C4 H4 125.6 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 107.2(4) . . ? C4 C5 Fe1 69.5(3) . . ? C1 C5 Fe1 70.1(3) . . ? C4 C5 H5 126.4 . . ? C1 C5 H5 126.4 . . ? Fe1 C5 H5 125.6 . . ? C7 C6 C10 108.0(4) . . ? C7 C6 Fe1 69.6(3) . . ? C10 C6 Fe1 70.1(3) . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? Fe1 C6 H6 125.9 . . ? C6 C7 C8 109.1(4) . . ? C6 C7 Fe1 69.8(3) . . ? C8 C7 Fe1 70.8(2) . . ? C6 C7 H7 125.4 . . ? C8 C7 H7 125.4 . . ? Fe1 C7 H7 125.5 . . ? C7 C8 C9 106.3(4) . . ? C7 C8 C33 124.4(4) . . ? C9 C8 C33 128.6(4) . . ? C7 C8 Fe1 68.6(2) . . ? C9 C8 Fe1 69.6(2) . . ? C33 C8 Fe1 134.1(3) . . ? C10 C9 C8 108.9(4) . . ? C10 C9 Fe1 69.4(3) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? Fe1 C9 H9 126.9 . . ? C9 C10 C6 107.6(4) . . ? C9 C10 Fe1 70.3(3) . . ? C6 C10 Fe1 69.2(3) . . ? C9 C10 H10 126.2 . . ? C6 C10 H10 126.2 . . ? Fe1 C10 H10 125.8 . . ? C24 C11 C2 112.0(3) . . ? C24 C11 C12 107.7(3) . . ? C2 C11 C12 108.3(4) . . ? C24 C11 C18 108.9(4) . . ? C2 C11 C18 109.0(3) . . ? C12 C11 C18 110.8(3) . . ? C13 C12 C17 118.4(4) . . ? C13 C12 C11 121.4(4) . . ? C17 C12 C11 120.2(4) . . ? C12 C13 C14 120.7(5) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 120.5(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 120.8(5) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C23 117.6(5) . . ? C19 C18 C11 120.6(4) . . ? C23 C18 C11 121.7(4) . . ? C20 C19 C18 121.2(5) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C19 120.2(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.7(5) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C22 C23 C18 121.1(5) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? N1 C24 C25 108.3(4) . . ? N1 C24 C11 121.8(4) . . ? C25 C24 C11 129.7(4) . . ? C26 C25 C24 107.8(4) . . ? C26 C25 H25 126.1 . . ? C24 C25 H25 126.1 . . ? C25 C26 C27 107.0(4) . . ? C25 C26 H26 126.5 . . ? C27 C26 H26 126.5 . . ? N1 C27 C26 107.3(4) . . ? N1 C27 C28 121.2(4) . . ? C26 C27 C28 131.5(4) . . ? C29 C28 C27 123.1(4) . . ? C29 C28 C46 118.4(4) . . ? C27 C28 C46 118.5(4) . . ? N2 C29 C28 120.4(4) . . ? N2 C29 C30 107.1(4) . . ? C28 C29 C30 132.5(4) . . ? C31 C30 C29 107.0(4) . . ? C31 C30 H30 126.5 . . ? C29 C30 H30 126.5 . . ? C30 C31 C32 107.9(4) . . ? C30 C31 H31 126.0 . . ? C32 C31 H31 126.0 . . ? N2 C32 C31 109.0(4) . . ? N2 C32 C33 120.0(4) . . ? C31 C32 C33 130.5(4) . . ? C32 C33 C8 112.1(4) . . ? C32 C33 C34 108.1(4) . . ? C8 C33 C34 108.8(3) . . ? C32 C33 C40 108.5(3) . . ? C8 C33 C40 108.5(3) . . ? C34 C33 C40 110.8(4) . . ? C35 C34 C39 117.6(4) . . ? C35 C34 C33 121.7(4) . . ? C39 C34 C33 120.8(4) . . ? C36 C35 C34 121.1(5) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 120.7(5) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 119.3(5) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 120.3(5) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.9(5) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C45 C40 C41 118.2(5) . . ? C45 C40 C33 121.8(4) . . ? C41 C40 C33 120.0(4) . . ? C40 C41 C42 120.8(6) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C43 C42 C41 119.5(6) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C44 C43 C42 119.8(5) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.8(6) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C40 121.0(6) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? C51 C46 C47 118.5(5) . . ? C51 C46 C28 121.2(5) . . ? C47 C46 C28 120.3(5) . . ? C48 C47 C46 120.4(6) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 C47 120.0(6) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 121.0(5) . . ? C48 C49 N3 119.8(6) . . ? C50 C49 N3 119.2(6) . . ? C49 C50 C51 119.0(6) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C46 C51 C50 121.1(6) . . ? C46 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? Cl1 C52 Cl3 110.1(10) . . ? Cl1 C52 Cl2 101.1(10) . . ? Cl3 C52 Cl2 103.2(9) . . ? Cl1 C52 H52 113.7 . . ? Cl3 C52 H52 113.7 . . ? Cl2 C52 H52 113.7 . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C53 118.6(15) . . ? C55 C54 H54A 107.7 . . ? C53 C54 H54A 107.7 . . ? C55 C54 H54B 107.7 . . ? C53 C54 H54B 107.7 . . ? H54A C54 H54B 107.1 . . ? C54 C55 C56 115.4(13) . . ? C54 C55 H55A 108.4 . . ? C56 C55 H55A 108.4 . . ? C54 C55 H55B 108.4 . . ? C56 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C55 C56 C57 111.7(13) . . ? C55 C56 H56A 109.3 . . ? C57 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C57 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? C58 C57 C56 104.9(12) . . ? C58 C57 H57A 110.8 . . ? C56 C57 H57A 110.8 . . ? C58 C57 H57B 110.8 . . ? C56 C57 H57B 110.8 . . ? H57A C57 H57B 108.8 . . ? C59 C58 C57 110.8(13) . . ? C59 C58 H58A 109.5 . . ? C57 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 108.1 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C24 N1 C27 109.6(4) . . ? C24 N1 H1A 133(6) . . ? C27 N1 H1A 115(6) . . ? C32 N2 C29 108.9(4) . . ? O1 N3 O2 128.9(8) . . ? O1 N3 C49 114.7(7) . . ? O2 N3 C49 116.4(7) . . ? C7 Fe1 C4 109.08(19) . . ? C7 Fe1 C6 40.58(19) . . ? C4 Fe1 C6 104.3(2) . . ? C7 Fe1 C3 138.77(19) . . ? C4 Fe1 C3 40.5(2) . . ? C6 Fe1 C3 109.2(2) . . ? C7 Fe1 C5 107.75(19) . . ? C4 Fe1 C5 40.2(2) . . ? C6 Fe1 C5 130.5(2) . . ? C3 Fe1 C5 68.1(2) . . ? C7 Fe1 C10 68.3(2) . . ? C4 Fe1 C10 131.2(2) . . ? C6 Fe1 C10 40.7(2) . . ? C3 Fe1 C10 108.4(2) . . ? C5 Fe1 C10 169.9(2) . . ? C7 Fe1 C1 136.73(19) . . ? C4 Fe1 C1 67.7(2) . . ? C6 Fe1 C1 171.12(19) . . ? C3 Fe1 C1 67.6(2) . . ? C5 Fe1 C1 40.78(18) . . ? C10 Fe1 C1 147.80(19) . . ? C7 Fe1 C9 67.80(19) . . ? C4 Fe1 C9 171.2(2) . . ? C6 Fe1 C9 67.80(19) . . ? C3 Fe1 C9 136.9(2) . . ? C5 Fe1 C9 148.1(2) . . ? C10 Fe1 C9 40.21(19) . . ? C1 Fe1 C9 120.42(18) . . ? C7 Fe1 C8 40.56(17) . . ? C4 Fe1 C8 141.44(19) . . ? C6 Fe1 C8 68.50(18) . . ? C3 Fe1 C8 176.96(19) . . ? C5 Fe1 C8 114.89(19) . . ? C10 Fe1 C8 68.57(18) . . ? C1 Fe1 C8 114.94(18) . . ? C9 Fe1 C8 40.69(18) . . ? C7 Fe1 C2 176.41(18) . . ? C4 Fe1 C2 68.27(18) . . ? C6 Fe1 C2 141.75(18) . . ? C3 Fe1 C2 40.51(18) . . ? C5 Fe1 C2 68.66(18) . . ? C10 Fe1 C2 115.28(19) . . ? C1 Fe1 C2 40.38(17) . . ? C9 Fe1 C2 115.19(18) . . ? C8 Fe1 C2 140.43(17) . . ? 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 C5 C1 C2 C3 -0.2(5) . . . . ? Fe1 C1 C2 C3 -58.7(3) . . . . ? C5 C1 C2 C11 -168.2(4) . . . . ? Fe1 C1 C2 C11 133.2(4) . . . . ? C5 C1 C2 Fe1 58.5(3) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C11 C2 C3 C4 168.3(4) . . . . ? Fe1 C2 C3 C4 -59.5(3) . . . . ? C1 C2 C3 Fe1 59.3(3) . . . . ? C11 C2 C3 Fe1 -132.2(4) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? Fe1 C3 C4 C5 -59.8(3) . . . . ? C2 C3 C4 Fe1 60.4(3) . . . . ? C3 C4 C5 C1 -0.7(5) . . . . ? Fe1 C4 C5 C1 -60.2(3) . . . . ? C3 C4 C5 Fe1 59.5(3) . . . . ? C2 C1 C5 C4 0.6(5) . . . . ? Fe1 C1 C5 C4 59.8(3) . . . . ? C2 C1 C5 Fe1 -59.2(3) . . . . ? C10 C6 C7 C8 0.3(5) . . . . ? Fe1 C6 C7 C8 60.1(3) . . . . ? C10 C6 C7 Fe1 -59.8(3) . . . . ? C6 C7 C8 C9 0.2(5) . . . . ? Fe1 C7 C8 C9 59.7(3) . . . . ? C6 C7 C8 C33 170.9(4) . . . . ? Fe1 C7 C8 C33 -129.6(4) . . . . ? C6 C7 C8 Fe1 -59.5(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? C33 C8 C9 C10 -170.7(4) . . . . ? Fe1 C8 C9 C10 58.5(3) . . . . ? C7 C8 C9 Fe1 -59.1(3) . . . . ? C33 C8 C9 Fe1 130.8(4) . . . . ? C8 C9 C10 C6 0.7(5) . . . . ? Fe1 C9 C10 C6 59.4(3) . . . . ? C8 C9 C10 Fe1 -58.7(3) . . . . ? C7 C6 C10 C9 -0.6(5) . . . . ? Fe1 C6 C10 C9 -60.1(3) . . . . ? C7 C6 C10 Fe1 59.5(3) . . . . ? C3 C2 C11 C24 169.7(4) . . . . ? C1 C2 C11 C24 -24.4(6) . . . . ? Fe1 C2 C11 C24 75.2(5) . . . . ? C3 C2 C11 C12 -71.7(5) . . . . ? C1 C2 C11 C12 94.3(5) . . . . ? Fe1 C2 C11 C12 -166.1(3) . . . . ? C3 C2 C11 C18 49.0(5) . . . . ? C1 C2 C11 C18 -145.0(4) . . . . ? Fe1 C2 C11 C18 -45.4(5) . . . . ? C24 C11 C12 C13 100.3(5) . . . . ? C2 C11 C12 C13 -21.1(6) . . . . ? C18 C11 C12 C13 -140.7(5) . . . . ? C24 C11 C12 C17 -77.9(5) . . . . ? C2 C11 C12 C17 160.8(4) . . . . ? C18 C11 C12 C17 41.2(6) . . . . ? C17 C12 C13 C14 0.1(9) . . . . ? C11 C12 C13 C14 -178.1(5) . . . . ? C12 C13 C14 C15 0.4(11) . . . . ? C13 C14 C15 C16 0.1(11) . . . . ? C14 C15 C16 C17 -1.1(10) . . . . ? C13 C12 C17 C16 -1.1(8) . . . . ? C11 C12 C17 C16 177.1(5) . . . . ? C15 C16 C17 C12 1.6(9) . . . . ? C24 C11 C18 C19 162.0(4) . . . . ? C2 C11 C18 C19 -75.5(5) . . . . ? C12 C11 C18 C19 43.7(5) . . . . ? C24 C11 C18 C23 -19.4(6) . . . . ? C2 C11 C18 C23 103.2(5) . . . . ? C12 C11 C18 C23 -137.7(4) . . . . ? C23 C18 C19 C20 -1.5(7) . . . . ? C11 C18 C19 C20 177.2(4) . . . . ? C18 C19 C20 C21 0.7(8) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C20 C21 C22 C23 -1.3(9) . . . . ? C21 C22 C23 C18 0.5(8) . . . . ? C19 C18 C23 C22 0.9(7) . . . . ? C11 C18 C23 C22 -177.8(5) . . . . ? C2 C11 C24 N1 -31.4(6) . . . . ? C12 C11 C24 N1 -150.3(4) . . . . ? C18 C11 C24 N1 89.4(5) . . . . ? C2 C11 C24 C25 154.2(5) . . . . ? C12 C11 C24 C25 35.2(7) . . . . ? C18 C11 C24 C25 -85.1(6) . . . . ? N1 C24 C25 C26 0.0(6) . . . . ? C11 C24 C25 C26 175.1(5) . . . . ? C24 C25 C26 C27 0.4(6) . . . . ? C25 C26 C27 N1 -0.7(6) . . . . ? C25 C26 C27 C28 179.8(5) . . . . ? N1 C27 C28 C29 0.8(8) . . . . ? C26 C27 C28 C29 -179.7(5) . . . . ? N1 C27 C28 C46 179.2(4) . . . . ? C26 C27 C28 C46 -1.4(8) . . . . ? C27 C28 C29 N2 -0.6(8) . . . . ? C46 C28 C29 N2 -179.0(4) . . . . ? C27 C28 C29 C30 177.3(5) . . . . ? C46 C28 C29 C30 -1.1(9) . . . . ? N2 C29 C30 C31 0.5(6) . . . . ? C28 C29 C30 C31 -177.6(5) . . . . ? C29 C30 C31 C32 -0.1(6) . . . . ? C30 C31 C32 N2 -0.4(6) . . . . ? C30 C31 C32 C33 171.3(5) . . . . ? N2 C32 C33 C8 -34.1(6) . . . . ? C31 C32 C33 C8 154.9(5) . . . . ? N2 C32 C33 C34 85.8(5) . . . . ? C31 C32 C33 C34 -85.1(6) . . . . ? N2 C32 C33 C40 -154.0(4) . . . . ? C31 C32 C33 C40 35.0(7) . . . . ? C7 C8 C33 C32 173.4(4) . . . . ? C9 C8 C33 C32 -18.0(6) . . . . ? Fe1 C8 C33 C32 80.7(5) . . . . ? C7 C8 C33 C34 53.9(5) . . . . ? C9 C8 C33 C34 -137.5(4) . . . . ? Fe1 C8 C33 C34 -38.9(5) . . . . ? C7 C8 C33 C40 -66.7(5) . . . . ? C9 C8 C33 C40 101.8(5) . . . . ? Fe1 C8 C33 C40 -159.5(3) . . . . ? C32 C33 C34 C35 -20.2(5) . . . . ? C8 C33 C34 C35 101.8(5) . . . . ? C40 C33 C34 C35 -139.0(4) . . . . ? C32 C33 C34 C39 160.4(4) . . . . ? C8 C33 C34 C39 -77.6(5) . . . . ? C40 C33 C34 C39 41.6(5) . . . . ? C39 C34 C35 C36 1.5(7) . . . . ? C33 C34 C35 C36 -177.8(4) . . . . ? C34 C35 C36 C37 -0.4(8) . . . . ? C35 C36 C37 C38 -0.4(8) . . . . ? C36 C37 C38 C39 0.1(8) . . . . ? C37 C38 C39 C34 1.1(8) . . . . ? C35 C34 C39 C38 -1.9(7) . . . . ? C33 C34 C39 C38 177.5(4) . . . . ? C32 C33 C40 C45 99.2(5) . . . . ? C8 C33 C40 C45 -22.9(6) . . . . ? C34 C33 C40 C45 -142.3(5) . . . . ? C32 C33 C40 C41 -78.8(5) . . . . ? C8 C33 C40 C41 159.1(4) . . . . ? C34 C33 C40 C41 39.7(6) . . . . ? C45 C40 C41 C42 1.1(8) . . . . ? C33 C40 C41 C42 179.2(5) . . . . ? C40 C41 C42 C43 -0.7(9) . . . . ? C41 C42 C43 C44 0.3(10) . . . . ? C42 C43 C44 C45 -0.4(10) . . . . ? C43 C44 C45 C40 0.8(10) . . . . ? C41 C40 C45 C44 -1.1(8) . . . . ? C33 C40 C45 C44 -179.2(5) . . . . ? C29 C28 C46 C51 115.5(5) . . . . ? C27 C28 C46 C51 -63.0(6) . . . . ? C29 C28 C46 C47 -63.3(5) . . . . ? C27 C28 C46 C47 118.2(5) . . . . ? C51 C46 C47 C48 -0.3(2) . . . . ? C28 C46 C47 C48 178.5(4) . . . . ? C46 C47 C48 C49 -0.2(3) . . . . ? C47 C48 C49 C50 0.3(5) . . . . ? C47 C48 C49 N3 -177.2(5) . . . . ? C48 C49 C50 C51 0.2(7) . . . . ? N3 C49 C50 C51 177.7(5) . . . . ? C47 C46 C51 C50 0.8(5) . . . . ? C28 C46 C51 C50 -178.0(5) . . . . ? C49 C50 C51 C46 -0.8(7) . . . . ? C53 C54 C55 C56 176.3(16) . . . . ? C54 C55 C56 C57 175.7(13) . . . . ? C55 C56 C57 C58 175.0(15) . . . . ? C56 C57 C58 C59 -174.1(13) . . . . ? C25 C24 N1 C27 -0.5(6) . . . . ? C11 C24 N1 C27 -176.0(4) . . . . ? C26 C27 N1 C24 0.7(6) . . . . ? C28 C27 N1 C24 -179.7(4) . . . . ? C31 C32 N2 C29 0.7(6) . . . . ? C33 C32 N2 C29 -172.0(4) . . . . ? C28 C29 N2 C32 177.6(5) . . . . ? C30 C29 N2 C32 -0.8(6) . . . . ? C48 C49 N3 O1 179.0(6) . . . . ? C50 C49 N3 O1 1.5(9) . . . . ? C48 C49 N3 O2 -1.7(10) . . . . ? C50 C49 N3 O2 -179.2(7) . . . . ? C6 C7 Fe1 C4 -89.9(3) . . . . ? C8 C7 Fe1 C4 150.3(3) . . . . ? C8 C7 Fe1 C6 -119.8(4) . . . . ? C6 C7 Fe1 C3 -55.6(4) . . . . ? C8 C7 Fe1 C3 -175.5(3) . . . . ? C6 C7 Fe1 C5 -132.4(3) . . . . ? C8 C7 Fe1 C5 107.8(3) . . . . ? C6 C7 Fe1 C10 37.8(3) . . . . ? C8 C7 Fe1 C10 -82.0(3) . . . . ? C6 C7 Fe1 C1 -167.3(3) . . . . ? C8 C7 Fe1 C1 72.9(4) . . . . ? C6 C7 Fe1 C9 81.3(3) . . . . ? C8 C7 Fe1 C9 -38.5(3) . . . . ? C6 C7 Fe1 C8 119.8(4) . . . . ? C6 C7 Fe1 C2 -132(3) . . . . ? C8 C7 Fe1 C2 108(3) . . . . ? C5 C4 Fe1 C7 -95.2(3) . . . . ? C3 C4 Fe1 C7 145.1(3) . . . . ? C5 C4 Fe1 C6 -137.4(3) . . . . ? C3 C4 Fe1 C6 103.0(3) . . . . ? C5 C4 Fe1 C3 119.7(4) . . . . ? C3 C4 Fe1 C5 -119.7(4) . . . . ? C5 C4 Fe1 C10 -172.6(3) . . . . ? C3 C4 Fe1 C10 67.7(4) . . . . ? C5 C4 Fe1 C1 38.5(3) . . . . ? C3 C4 Fe1 C1 -81.2(3) . . . . ? C5 C4 Fe1 C9 -162.8(11) . . . . ? C3 C4 Fe1 C9 77.5(13) . . . . ? C5 C4 Fe1 C8 -64.0(4) . . . . ? C3 C4 Fe1 C8 176.3(3) . . . . ? C5 C4 Fe1 C2 82.2(3) . . . . ? C3 C4 Fe1 C2 -37.5(3) . . . . ? C10 C6 Fe1 C7 119.0(4) . . . . ? C7 C6 Fe1 C4 102.7(3) . . . . ? C10 C6 Fe1 C4 -138.2(3) . . . . ? C7 C6 Fe1 C3 144.8(3) . . . . ? C10 C6 Fe1 C3 -96.1(3) . . . . ? C7 C6 Fe1 C5 67.7(4) . . . . ? C10 C6 Fe1 C5 -173.3(3) . . . . ? C7 C6 Fe1 C10 -119.0(4) . . . . ? C7 C6 Fe1 C1 77.2(12) . . . . ? C10 C6 Fe1 C1 -163.8(11) . . . . ? C7 C6 Fe1 C9 -81.3(3) . . . . ? C10 C6 Fe1 C9 37.7(3) . . . . ? C7 C6 Fe1 C8 -37.3(3) . . . . ? C10 C6 Fe1 C8 81.7(3) . . . . ? C7 C6 Fe1 C2 175.7(3) . . . . ? C10 C6 Fe1 C2 -65.3(4) . . . . ? C4 C3 Fe1 C7 -55.1(4) . . . . ? C2 C3 Fe1 C7 -174.6(3) . . . . ? C2 C3 Fe1 C4 -119.6(4) . . . . ? C4 C3 Fe1 C6 -89.7(3) . . . . ? C2 C3 Fe1 C6 150.7(3) . . . . ? C4 C3 Fe1 C5 37.2(3) . . . . ? C2 C3 Fe1 C5 -82.4(3) . . . . ? C4 C3 Fe1 C10 -132.8(3) . . . . ? C2 C3 Fe1 C10 107.7(3) . . . . ? C4 C3 Fe1 C1 81.4(3) . . . . ? C2 C3 Fe1 C1 -38.2(3) . . . . ? C4 C3 Fe1 C9 -167.4(3) . . . . ? C2 C3 Fe1 C9 73.0(4) . . . . ? C4 C3 Fe1 C8 -131(3) . . . . ? C2 C3 Fe1 C8 110(3) . . . . ? C4 C3 Fe1 C2 119.6(4) . . . . ? C4 C5 Fe1 C7 98.8(3) . . . . ? C1 C5 Fe1 C7 -143.1(3) . . . . ? C1 C5 Fe1 C4 118.1(4) . . . . ? C4 C5 Fe1 C6 59.6(4) . . . . ? C1 C5 Fe1 C6 177.8(3) . . . . ? C4 C5 Fe1 C3 -37.5(3) . . . . ? C1 C5 Fe1 C3 80.7(3) . . . . ? C4 C5 Fe1 C10 33.8(12) . . . . ? C1 C5 Fe1 C10 151.9(10) . . . . ? C4 C5 Fe1 C1 -118.1(4) . . . . ? C4 C5 Fe1 C9 175.1(3) . . . . ? C1 C5 Fe1 C9 -66.7(4) . . . . ? C4 C5 Fe1 C8 141.9(3) . . . . ? C1 C5 Fe1 C8 -100.0(3) . . . . ? C4 C5 Fe1 C2 -81.2(3) . . . . ? C1 C5 Fe1 C2 37.0(3) . . . . ? C9 C10 Fe1 C7 80.9(3) . . . . ? C6 C10 Fe1 C7 -37.8(3) . . . . ? C9 C10 Fe1 C4 177.7(3) . . . . ? C6 C10 Fe1 C4 59.1(4) . . . . ? C9 C10 Fe1 C6 118.6(4) . . . . ? C9 C10 Fe1 C3 -143.0(3) . . . . ? C6 C10 Fe1 C3 98.4(3) . . . . ? C9 C10 Fe1 C5 149.2(10) . . . . ? C6 C10 Fe1 C5 30.6(12) . . . . ? C9 C10 Fe1 C1 -66.0(5) . . . . ? C6 C10 Fe1 C1 175.4(3) . . . . ? C6 C10 Fe1 C9 -118.6(4) . . . . ? C9 C10 Fe1 C8 37.1(3) . . . . ? C6 C10 Fe1 C8 -81.5(3) . . . . ? C9 C10 Fe1 C2 -99.8(3) . . . . ? C6 C10 Fe1 C2 141.6(3) . . . . ? C2 C1 Fe1 C7 176.8(3) . . . . ? C5 C1 Fe1 C7 56.6(4) . . . . ? C2 C1 Fe1 C4 82.2(3) . . . . ? C5 C1 Fe1 C4 -38.0(3) . . . . ? C2 C1 Fe1 C6 109.1(12) . . . . ? C5 C1 Fe1 C6 -11.1(13) . . . . ? C2 C1 Fe1 C3 38.3(3) . . . . ? C5 C1 Fe1 C3 -81.9(3) . . . . ? C2 C1 Fe1 C5 120.2(4) . . . . ? C2 C1 Fe1 C10 -50.9(4) . . . . ? C5 C1 Fe1 C10 -171.1(3) . . . . ? C2 C1 Fe1 C9 -94.1(3) . . . . ? C5 C1 Fe1 C9 145.7(3) . . . . ? C2 C1 Fe1 C8 -139.9(3) . . . . ? C5 C1 Fe1 C8 99.9(3) . . . . ? C5 C1 Fe1 C2 -120.2(4) . . . . ? C10 C9 Fe1 C7 -82.1(3) . . . . ? C8 C9 Fe1 C7 38.4(3) . . . . ? C10 C9 Fe1 C4 -11.4(13) . . . . ? C8 C9 Fe1 C4 109.1(12) . . . . ? C10 C9 Fe1 C6 -38.1(3) . . . . ? C8 C9 Fe1 C6 82.4(3) . . . . ? C10 C9 Fe1 C3 56.7(4) . . . . ? C8 C9 Fe1 C3 177.2(3) . . . . ? C10 C9 Fe1 C5 -170.3(3) . . . . ? C8 C9 Fe1 C5 -49.8(4) . . . . ? C8 C9 Fe1 C10 120.5(4) . . . . ? C10 C9 Fe1 C1 145.6(3) . . . . ? C8 C9 Fe1 C1 -93.9(3) . . . . ? C10 C9 Fe1 C8 -120.5(4) . . . . ? C10 C9 Fe1 C2 100.1(3) . . . . ? C8 C9 Fe1 C2 -139.4(3) . . . . ? C9 C8 Fe1 C7 -117.9(4) . . . . ? C33 C8 Fe1 C7 117.7(5) . . . . ? C7 C8 Fe1 C4 -48.8(4) . . . . ? C9 C8 Fe1 C4 -166.6(3) . . . . ? C33 C8 Fe1 C4 68.9(5) . . . . ? C7 C8 Fe1 C6 37.3(3) . . . . ? C9 C8 Fe1 C6 -80.5(3) . . . . ? C33 C8 Fe1 C6 155.0(5) . . . . ? C7 C8 Fe1 C3 79(3) . . . . ? C9 C8 Fe1 C3 -39(3) . . . . ? C33 C8 Fe1 C3 -163(3) . . . . ? C7 C8 Fe1 C5 -88.6(3) . . . . ? C9 C8 Fe1 C5 153.6(3) . . . . ? C33 C8 Fe1 C5 29.1(5) . . . . ? C7 C8 Fe1 C10 81.2(3) . . . . ? C9 C8 Fe1 C10 -36.7(3) . . . . ? C33 C8 Fe1 C10 -161.1(5) . . . . ? C7 C8 Fe1 C1 -133.7(3) . . . . ? C9 C8 Fe1 C1 108.4(3) . . . . ? C33 C8 Fe1 C1 -16.0(5) . . . . ? C7 C8 Fe1 C9 117.9(4) . . . . ? C33 C8 Fe1 C9 -124.4(5) . . . . ? C7 C8 Fe1 C2 -174.6(3) . . . . ? C9 C8 Fe1 C2 67.5(4) . . . . ? C33 C8 Fe1 C2 -56.9(5) . . . . ? C3 C2 Fe1 C7 81(3) . . . . ? C1 C2 Fe1 C7 -38(3) . . . . ? C11 C2 Fe1 C7 -161(3) . . . . ? C3 C2 Fe1 C4 37.4(3) . . . . ? C1 C2 Fe1 C4 -80.7(3) . . . . ? C11 C2 Fe1 C4 155.6(5) . . . . ? C3 C2 Fe1 C6 -48.2(4) . . . . ? C1 C2 Fe1 C6 -166.4(3) . . . . ? C11 C2 Fe1 C6 69.9(5) . . . . ? C1 C2 Fe1 C3 -118.1(4) . . . . ? C11 C2 Fe1 C3 118.1(5) . . . . ? C3 C2 Fe1 C5 80.8(3) . . . . ? C1 C2 Fe1 C5 -37.3(3) . . . . ? C11 C2 Fe1 C5 -161.0(5) . . . . ? C3 C2 Fe1 C10 -89.1(3) . . . . ? C1 C2 Fe1 C10 152.8(3) . . . . ? C11 C2 Fe1 C10 29.0(5) . . . . ? C3 C2 Fe1 C1 118.1(4) . . . . ? C11 C2 Fe1 C1 -123.7(5) . . . . ? C3 C2 Fe1 C9 -133.8(3) . . . . ? C1 C2 Fe1 C9 108.1(3) . . . . ? C11 C2 Fe1 C9 -15.6(5) . . . . ? C3 C2 Fe1 C8 -175.5(3) . . . . ? C1 C2 Fe1 C8 66.4(4) . . . . ? C11 C2 Fe1 C8 -57.4(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A N2 0.67(6) 2.04(7) 2.582(6) 139(7) . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.873 _refine_diff_density_min -1.407 _refine_diff_density_rms 0.103 # Attachment 'Fe-Dimer__6b_.cif' data_215rkm _database_code_depnum_ccdc_archive 'CCDC 732749' #TrackingRef 'Fe-Dimer__6b_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H50 F10 Fe2 N4' _chemical_formula_weight 1152.76 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.0784(17) _cell_length_b 11.4123(17) _cell_length_c 12.3519(19) _cell_angle_alpha 117.468(2) _cell_angle_beta 99.411(2) _cell_angle_gamma 106.469(2) _cell_volume 1246.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2112 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.42 _exptl_crystal_description BLOCKS _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8249 _exptl_absorpt_correction_T_max 0.9242 _exptl_absorpt_process_details BRUKER-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CDD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10763 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5645 _reflns_number_gt 4862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0542P)^2^+1.0799P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5645 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.82692(3) 0.59613(4) 0.71909(3) 0.01352(11) Uani 1 d . . . F1 F 0.56269(16) -0.30579(16) 0.19828(15) 0.0234(3) Uani 1 d . . . F2 F 0.34325(16) -0.48885(16) -0.01609(16) 0.0274(4) Uani 1 d . . . F3 F 0.28916(16) -0.42723(19) -0.20142(16) 0.0316(4) Uani 1 d . . . F4 F 0.45993(17) -0.18225(19) -0.17284(16) 0.0293(4) Uani 1 d . . . F5 F 0.67940(15) 0.00151(16) 0.04013(15) 0.0228(3) Uani 1 d . . . N1 N 0.8300(2) 0.1413(2) 0.4817(2) 0.0156(4) Uani 1 d . . . N2 N 0.9931(2) 0.0891(2) 0.3437(2) 0.0151(4) Uani 1 d . . . C1 C 0.9192(2) 0.4662(3) 0.7289(2) 0.0146(5) Uani 1 d . . . C2 C 0.9383(2) 0.4932(3) 0.6298(2) 0.0158(5) Uani 1 d . . . H2 H 0.9095 0.4194 0.5371 0.019 Uiso 1 calc R . . C3 C 1.0054(3) 0.6452(3) 0.6880(3) 0.0179(5) Uani 1 d . . . H3 H 1.0314 0.6943 0.6427 0.021 Uiso 1 calc R . . C4 C 1.0272(3) 0.7131(3) 0.8228(3) 0.0203(6) Uani 1 d . . . H4 H 1.0711 0.8175 0.8871 0.024 Uiso 1 calc R . . C5 C 0.9749(2) 0.6044(3) 0.8488(3) 0.0177(5) Uani 1 d . . . H5 H 0.9761 0.6208 0.9342 0.021 Uiso 1 calc R . . C6 C 0.7232(2) 0.6914(3) 0.6577(3) 0.0164(5) Uani 1 d . . . C7 C 0.7307(2) 0.7294(3) 0.7865(3) 0.0172(5) Uani 1 d . . . H7 H 0.7721 0.8280 0.8637 0.021 Uiso 1 calc R . . C8 C 0.6701(3) 0.6012(3) 0.7856(3) 0.0199(5) Uani 1 d . . . H8 H 0.6611 0.5959 0.8610 0.024 Uiso 1 calc R . . C9 C 0.6251(3) 0.4826(3) 0.6561(3) 0.0210(6) Uani 1 d . . . H9 H 0.5794 0.3804 0.6261 0.025 Uiso 1 calc R . . C10 C 0.6569(2) 0.5364(3) 0.5769(3) 0.0200(5) Uani 1 d . . . H10 H 0.6375 0.4778 0.4830 0.024 Uiso 1 calc R . . C11 C 0.8693(3) 0.3191(3) 0.7144(2) 0.0151(5) Uani 1 d . . . C12 C 0.7795(2) 0.2011(3) 0.5761(2) 0.0143(5) Uani 1 d . . . C13 C 0.6409(3) 0.1354(3) 0.5193(3) 0.0174(5) Uani 1 d . . . H13 H 0.5802 0.1546 0.5615 0.021 Uiso 1 calc R . . C14 C 0.6084(3) 0.0351(3) 0.3872(3) 0.0172(5) Uani 1 d . . . H14 H 0.5224 -0.0238 0.3258 0.021 Uiso 1 calc R . . C15 C 0.7273(2) 0.0390(3) 0.3640(2) 0.0160(5) Uani 1 d . . . C16 C 0.7511(2) -0.0402(3) 0.2468(2) 0.0150(5) Uani 1 d . . . C17 C 0.8761(3) -0.0204(3) 0.2371(2) 0.0158(5) Uani 1 d . . . C18 C 0.9125(3) -0.0917(3) 0.1246(2) 0.0170(5) Uani 1 d . . . H18 H 0.8549 -0.1695 0.0421 0.020 Uiso 1 calc R . . C19 C 1.0472(3) -0.0229(3) 0.1630(2) 0.0171(5) Uani 1 d . . . H19 H 1.1003 -0.0441 0.1119 0.021 Uiso 1 calc R . . C20 C 1.0929(3) 0.0904(3) 0.2995(2) 0.0160(5) Uani 1 d . . . C21 C 1.2349(2) 0.2022(3) 0.3847(2) 0.0160(5) Uani 1 d . . . C22 C 0.6296(2) -0.1453(3) 0.1270(2) 0.0160(5) Uani 1 d . . . C23 C 0.5401(3) -0.2715(3) 0.1088(2) 0.0180(5) Uani 1 d . . . C24 C 0.4264(3) -0.3665(3) -0.0009(3) 0.0201(6) Uani 1 d . . . C25 C 0.3981(3) -0.3365(3) -0.0958(3) 0.0223(6) Uani 1 d . . . C26 C 0.4853(3) -0.2115(3) -0.0806(3) 0.0207(6) Uani 1 d . . . C27 C 0.5981(3) -0.1191(3) 0.0293(3) 0.0179(5) Uani 1 d . . . C28 C 0.9951(3) 0.2926(3) 0.7497(3) 0.0199(5) Uani 1 d . . . H28A H 0.9682 0.1977 0.7360 0.030 Uiso 1 calc R . . H28B H 1.0489 0.3639 0.8394 0.030 Uiso 1 calc R . . H28C H 1.0464 0.2998 0.6958 0.030 Uiso 1 calc R . . C29 C 0.7934(3) 0.3177(3) 0.8070(3) 0.0208(6) Uani 1 d . . . H29A H 0.7154 0.3348 0.7859 0.031 Uiso 1 calc R . . H29B H 0.8507 0.3922 0.8949 0.031 Uiso 1 calc R . . H29C H 0.7664 0.2252 0.7983 0.031 Uiso 1 calc R . . C30 C 1.2451(3) 0.2815(3) 0.5273(3) 0.0217(6) Uani 1 d . . . H30A H 1.3367 0.3467 0.5812 0.033 Uiso 1 calc R . . H30B H 1.2144 0.2124 0.5512 0.033 Uiso 1 calc R . . H30C H 1.1904 0.3353 0.5390 0.033 Uiso 1 calc R . . C31 C 1.3304(3) 0.1249(3) 0.3685(3) 0.0208(6) Uani 1 d . . . H31A H 1.3190 0.0687 0.2781 0.031 Uiso 1 calc R . . H31B H 1.3103 0.0623 0.4007 0.031 Uiso 1 calc R . . H31C H 1.4214 0.1957 0.4165 0.031 Uiso 1 calc R . . H1C H 0.909(3) 0.157(3) 0.485(3) 0.025(9) Uiso 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 Fe1 0.01213(18) 0.00992(18) 0.01531(19) 0.00467(15) 0.00493(14) 0.00400(14) F1 0.0266(8) 0.0173(8) 0.0212(8) 0.0100(7) 0.0057(7) 0.0044(7) F2 0.0227(8) 0.0144(8) 0.0265(9) 0.0038(7) 0.0061(7) -0.0026(7) F3 0.0187(8) 0.0307(9) 0.0199(8) 0.0023(7) -0.0027(7) 0.0026(7) F4 0.0292(9) 0.0376(10) 0.0223(9) 0.0170(8) 0.0058(7) 0.0154(8) F5 0.0224(8) 0.0201(8) 0.0263(8) 0.0146(7) 0.0073(7) 0.0061(7) N1 0.0136(11) 0.0132(10) 0.0149(10) 0.0047(9) 0.0038(9) 0.0047(9) N2 0.0134(10) 0.0131(10) 0.0169(11) 0.0069(9) 0.0039(9) 0.0057(8) C1 0.0132(12) 0.0114(11) 0.0143(12) 0.0041(10) 0.0039(10) 0.0043(9) C2 0.0154(12) 0.0148(12) 0.0180(12) 0.0078(10) 0.0081(10) 0.0078(10) C3 0.0166(12) 0.0129(12) 0.0249(14) 0.0095(11) 0.0094(11) 0.0068(10) C4 0.0133(12) 0.0153(12) 0.0249(14) 0.0068(11) 0.0049(11) 0.0045(10) C5 0.0149(12) 0.0150(12) 0.0162(12) 0.0054(11) 0.0026(10) 0.0040(10) C6 0.0112(12) 0.0152(12) 0.0198(13) 0.0074(11) 0.0052(10) 0.0054(10) C7 0.0155(12) 0.0150(12) 0.0223(13) 0.0091(11) 0.0097(11) 0.0076(10) C8 0.0162(13) 0.0199(13) 0.0277(14) 0.0133(12) 0.0128(11) 0.0086(11) C9 0.0134(12) 0.0161(12) 0.0306(15) 0.0121(12) 0.0053(11) 0.0043(10) C10 0.0128(12) 0.0154(12) 0.0219(13) 0.0060(11) 0.0005(10) 0.0032(10) C11 0.0172(12) 0.0129(11) 0.0133(12) 0.0062(10) 0.0046(10) 0.0053(10) C12 0.0175(12) 0.0106(11) 0.0147(12) 0.0070(10) 0.0054(10) 0.0054(10) C13 0.0161(12) 0.0129(12) 0.0209(13) 0.0081(11) 0.0062(10) 0.0051(10) C14 0.0151(12) 0.0123(11) 0.0182(13) 0.0058(10) 0.0033(10) 0.0034(10) C15 0.0152(12) 0.0104(11) 0.0174(12) 0.0054(10) 0.0031(10) 0.0038(10) C16 0.0152(12) 0.0101(11) 0.0166(12) 0.0063(10) 0.0032(10) 0.0040(10) C17 0.0169(12) 0.0112(11) 0.0166(12) 0.0071(10) 0.0036(10) 0.0042(10) C18 0.0207(13) 0.0117(11) 0.0136(12) 0.0044(10) 0.0038(10) 0.0058(10) C19 0.0185(13) 0.0144(12) 0.0174(13) 0.0078(11) 0.0068(10) 0.0065(10) C20 0.0179(12) 0.0131(11) 0.0167(12) 0.0080(10) 0.0045(10) 0.0065(10) C21 0.0147(12) 0.0160(12) 0.0177(12) 0.0088(11) 0.0052(10) 0.0074(10) C22 0.0143(12) 0.0135(12) 0.0157(12) 0.0041(10) 0.0044(10) 0.0068(10) C23 0.0197(13) 0.0142(12) 0.0163(12) 0.0061(11) 0.0070(11) 0.0053(10) C24 0.0158(13) 0.0128(12) 0.0237(14) 0.0053(11) 0.0086(11) 0.0024(10) C25 0.0165(13) 0.0199(13) 0.0156(13) 0.0005(11) 0.0022(10) 0.0060(11) C26 0.0213(13) 0.0240(14) 0.0190(13) 0.0108(12) 0.0082(11) 0.0125(11) C27 0.0157(12) 0.0139(12) 0.0215(13) 0.0072(11) 0.0083(11) 0.0056(10) C28 0.0214(13) 0.0163(12) 0.0183(13) 0.0085(11) 0.0022(11) 0.0068(11) C29 0.0229(14) 0.0203(13) 0.0184(13) 0.0102(11) 0.0102(11) 0.0066(11) C30 0.0171(13) 0.0218(13) 0.0176(13) 0.0077(11) 0.0033(11) 0.0038(11) C31 0.0176(13) 0.0189(13) 0.0251(14) 0.0111(12) 0.0059(11) 0.0084(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 Fe1 C9 2.035(3) . ? Fe1 C4 2.040(3) . ? Fe1 C8 2.044(3) . ? Fe1 C5 2.044(3) . ? Fe1 C7 2.045(2) . ? Fe1 C10 2.046(3) . ? Fe1 C2 2.047(2) . ? Fe1 C3 2.047(3) . ? Fe1 C1 2.061(2) . ? Fe1 C6 2.064(3) . ? F1 C23 1.342(3) . ? F2 C24 1.344(3) . ? F3 C25 1.327(3) . ? F4 C26 1.337(3) . ? F5 C27 1.346(3) . ? N1 C12 1.355(3) . ? N1 C15 1.382(3) . ? N1 H1C 0.84(3) . ? N2 C20 1.310(3) . ? N2 C17 1.408(3) . ? C1 C2 1.427(3) . ? C1 C5 1.434(3) . ? C1 C11 1.523(3) . ? C2 C3 1.422(3) . ? C2 H2 0.9800 . ? C3 C4 1.416(4) . ? C3 H3 0.9800 . ? C4 C5 1.413(4) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C6 C7 1.424(4) . ? C6 C10 1.435(3) . ? C6 C21 1.520(4) 2_766 ? C7 C8 1.420(4) . ? C7 H7 0.9800 . ? C8 C9 1.414(4) . ? C8 H8 0.9800 . ? C9 C10 1.415(4) . ? C9 H9 0.9800 . ? C10 H10 0.9800 . ? C11 C12 1.511(3) . ? C11 C29 1.530(3) . ? C11 C28 1.544(3) . ? C12 C13 1.386(4) . ? C13 C14 1.397(4) . ? C13 H13 0.9300 . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 C16 1.427(3) . ? C16 C17 1.372(4) . ? C16 C22 1.496(3) . ? C17 C18 1.443(3) . ? C18 C19 1.352(4) . ? C18 H18 0.9300 . ? C19 C20 1.452(4) . ? C19 H19 0.9300 . ? C20 C21 1.513(3) . ? C21 C6 1.520(4) 2_766 ? C21 C30 1.530(4) . ? C21 C31 1.540(3) . ? C22 C27 1.386(4) . ? C22 C23 1.388(3) . ? C23 C24 1.382(4) . ? C24 C25 1.379(4) . ? C25 C26 1.383(4) . ? C26 C27 1.376(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Fe1 C4 166.20(11) . . ? C9 Fe1 C8 40.56(11) . . ? C4 Fe1 C8 128.22(11) . . ? C9 Fe1 C5 128.48(11) . . ? C4 Fe1 C5 40.49(10) . . ? C8 Fe1 C5 108.87(11) . . ? C9 Fe1 C7 68.13(11) . . ? C4 Fe1 C7 108.34(11) . . ? C8 Fe1 C7 40.63(10) . . ? C5 Fe1 C7 119.38(11) . . ? C9 Fe1 C10 40.57(11) . . ? C4 Fe1 C10 151.96(11) . . ? C8 Fe1 C10 68.31(11) . . ? C5 Fe1 C10 165.94(10) . . ? C7 Fe1 C10 68.12(11) . . ? C9 Fe1 C2 118.63(11) . . ? C4 Fe1 C2 68.31(10) . . ? C8 Fe1 C2 152.79(11) . . ? C5 Fe1 C2 68.32(10) . . ? C7 Fe1 C2 164.92(10) . . ? C10 Fe1 C2 107.49(11) . . ? C9 Fe1 C3 152.15(11) . . ? C4 Fe1 C3 40.54(11) . . ? C8 Fe1 C3 165.61(11) . . ? C5 Fe1 C3 68.20(11) . . ? C7 Fe1 C3 127.38(10) . . ? C10 Fe1 C3 118.03(11) . . ? C2 Fe1 C3 40.65(10) . . ? C9 Fe1 C1 108.21(10) . . ? C4 Fe1 C1 68.57(10) . . ? C8 Fe1 C1 119.19(10) . . ? C5 Fe1 C1 40.89(10) . . ? C7 Fe1 C1 153.34(10) . . ? C10 Fe1 C1 127.34(10) . . ? C2 Fe1 C1 40.65(10) . . ? C3 Fe1 C1 68.51(10) . . ? C9 Fe1 C6 68.61(10) . . ? C4 Fe1 C6 118.04(10) . . ? C8 Fe1 C6 68.63(10) . . ? C5 Fe1 C6 152.33(10) . . ? C7 Fe1 C6 40.55(10) . . ? C10 Fe1 C6 40.86(10) . . ? C2 Fe1 C6 126.82(10) . . ? C3 Fe1 C6 107.02(10) . . ? C1 Fe1 C6 164.97(10) . . ? C12 N1 C15 110.3(2) . . ? C12 N1 H1C 130(2) . . ? C15 N1 H1C 119(2) . . ? C20 N2 C17 106.4(2) . . ? C2 C1 C5 106.8(2) . . ? C2 C1 C11 126.5(2) . . ? C5 C1 C11 126.1(2) . . ? C2 C1 Fe1 69.16(14) . . ? C5 C1 Fe1 68.92(14) . . ? C11 C1 Fe1 133.72(17) . . ? C3 C2 C1 108.5(2) . . ? C3 C2 Fe1 69.68(14) . . ? C1 C2 Fe1 70.19(14) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe1 C2 H2 125.7 . . ? C4 C3 C2 107.9(2) . . ? C4 C3 Fe1 69.44(15) . . ? C2 C3 Fe1 69.67(14) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Fe1 C3 H3 126.1 . . ? C5 C4 C3 108.3(2) . . ? C5 C4 Fe1 69.92(15) . . ? C3 C4 Fe1 70.02(15) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe1 C4 H4 125.8 . . ? C4 C5 C1 108.4(2) . . ? C4 C5 Fe1 69.59(15) . . ? C1 C5 Fe1 70.19(14) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe1 C5 H5 125.8 . . ? C7 C6 C10 106.5(2) . . ? C7 C6 C21 125.4(2) . 2_766 ? C10 C6 C21 127.8(2) . 2_766 ? C7 C6 Fe1 69.00(14) . . ? C10 C6 Fe1 68.87(14) . . ? C21 C6 Fe1 131.59(17) 2_766 . ? C8 C7 C6 109.0(2) . . ? C8 C7 Fe1 69.62(14) . . ? C6 C7 Fe1 70.45(14) . . ? C8 C7 H7 125.5 . . ? C6 C7 H7 125.5 . . ? Fe1 C7 H7 125.5 . . ? C9 C8 C7 107.6(2) . . ? C9 C8 Fe1 69.41(15) . . ? C7 C8 Fe1 69.74(14) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? Fe1 C8 H8 126.2 . . ? C8 C9 C10 108.5(2) . . ? C8 C9 Fe1 70.04(15) . . ? C10 C9 Fe1 70.11(15) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 125.7 . . ? C9 C10 C6 108.4(2) . . ? C9 C10 Fe1 69.32(15) . . ? C6 C10 Fe1 70.27(14) . . ? C9 C10 H10 125.8 . . ? C6 C10 H10 125.8 . . ? Fe1 C10 H10 125.8 . . ? C12 C11 C1 110.7(2) . . ? C12 C11 C29 109.5(2) . . ? C1 C11 C29 111.3(2) . . ? C12 C11 C28 109.7(2) . . ? C1 C11 C28 106.5(2) . . ? C29 C11 C28 109.1(2) . . ? N1 C12 C13 107.3(2) . . ? N1 C12 C11 121.8(2) . . ? C13 C12 C11 130.9(2) . . ? C12 C13 C14 107.9(2) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? C15 C14 C13 107.8(2) . . ? C15 C14 H14 126.1 . . ? C13 C14 H14 126.1 . . ? N1 C15 C14 106.6(2) . . ? N1 C15 C16 122.6(2) . . ? C14 C15 C16 130.8(2) . . ? C17 C16 C15 124.4(2) . . ? C17 C16 C22 119.2(2) . . ? C15 C16 C22 116.2(2) . . ? C16 C17 N2 121.3(2) . . ? C16 C17 C18 129.4(2) . . ? N2 C17 C18 109.1(2) . . ? C19 C18 C17 106.3(2) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? C18 C19 C20 106.8(2) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.6 . . ? N2 C20 C19 111.4(2) . . ? N2 C20 C21 121.7(2) . . ? C19 C20 C21 126.9(2) . . ? C20 C21 C6 110.1(2) . 2_766 ? C20 C21 C30 110.0(2) . . ? C6 C21 C30 110.6(2) 2_766 . ? C20 C21 C31 108.9(2) . . ? C6 C21 C31 107.8(2) 2_766 . ? C30 C21 C31 109.2(2) . . ? C27 C22 C23 116.2(2) . . ? C27 C22 C16 121.4(2) . . ? C23 C22 C16 122.3(2) . . ? F1 C23 C24 117.6(2) . . ? F1 C23 C22 120.3(2) . . ? C24 C23 C22 122.0(2) . . ? F2 C24 C25 119.6(2) . . ? F2 C24 C23 120.3(2) . . ? C25 C24 C23 120.1(2) . . ? F3 C25 C24 120.4(2) . . ? F3 C25 C26 120.3(3) . . ? C24 C25 C26 119.3(2) . . ? F4 C26 C27 120.7(2) . . ? F4 C26 C25 119.9(2) . . ? C27 C26 C25 119.4(2) . . ? F5 C27 C26 117.2(2) . . ? F5 C27 C22 119.8(2) . . ? C26 C27 C22 122.9(2) . . ? C11 C28 H28A 109.5 . . ? C11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C11 C29 H29A 109.5 . . ? C11 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C11 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C21 C30 H30A 109.5 . . ? C21 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C21 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 0.809 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.087 # Attachment 'Methyl-DPM__1b_.cif' data_fadpm _database_code_depnum_ccdc_archive 'CCDC 732750' #TrackingRef 'Methyl-DPM__1b_.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Fe N2' _chemical_formula_weight 400.33 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3633(3) _cell_length_b 12.0119(5) _cell_length_c 12.4506(6) _cell_angle_alpha 105.413(2) _cell_angle_beta 95.925(2) _cell_angle_gamma 106.768(2) _cell_volume 996.98(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6249 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24.2 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8134 _exptl_absorpt_correction_T_max 0.8567 _exptl_absorpt_process_details 'SADABS(Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27755 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 33.64 _reflns_number_total 7805 _reflns_number_gt 5876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altornare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _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^)+(0.0572P)^2^+0.2258P] 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 7805 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 1.1402(3) -0.33194(14) 0.65891(14) 0.0431(3) Uani 1 1 d . . . H1 H 1.0251 -0.3975 0.6345 0.052 Uiso 1 1 calc R . . C2 C 1.2618(3) -0.29041(18) 0.76689(15) 0.0554(5) Uani 1 1 d . . . H2 H 1.2409 -0.3240 0.8256 0.066 Uiso 1 1 calc R . . C3 C 1.4196(3) -0.1897(2) 0.77016(15) 0.0553(5) Uani 1 1 d . . . H3 H 1.5211 -0.1450 0.8316 0.066 Uiso 1 1 calc R . . C4 C 1.3984(2) -0.16772(15) 0.66395(13) 0.0395(3) Uani 1 1 d . . . H4 H 1.4833 -0.1063 0.6436 0.047 Uiso 1 1 calc R . . C5 C 1.2235(2) -0.25647(12) 0.59373(12) 0.0323(2) Uani 1 1 d . . . C6 C 1.1499(2) -0.27667(13) 0.46998(12) 0.0337(3) Uani 1 1 d . . . C7 C 0.9275(2) -0.33171(18) 0.44132(16) 0.0489(4) Uani 1 1 d . . . H7A H 0.8880 -0.4082 0.4571 0.073 Uiso 1 1 calc R . . H7B H 0.8825 -0.3449 0.3623 0.073 Uiso 1 1 calc R . . H7C H 0.8733 -0.2763 0.4867 0.073 Uiso 1 1 calc R . . C8 C 1.2096(3) -0.15685(15) 0.44080(15) 0.0470(4) Uani 1 1 d . . . H8A H 1.1516 -0.1017 0.4831 0.070 Uiso 1 1 calc R . . H8B H 1.1668 -0.1732 0.3610 0.070 Uiso 1 1 calc R . . H8C H 1.3478 -0.1204 0.4601 0.070 Uiso 1 1 calc R . . C9 C 1.2358(2) -0.36513(13) 0.40006(11) 0.0337(3) Uani 1 1 d . . . C10 C 1.3771(2) -0.41003(14) 0.42894(13) 0.0395(3) Uani 1 1 d . . . H10 H 1.4466 -0.3914 0.5018 0.047 Uiso 1 1 calc R . . C11 C 1.4000(3) -0.49002(15) 0.32894(15) 0.0462(3) Uani 1 1 d . . . H11 H 1.4864 -0.5335 0.3240 0.055 Uiso 1 1 calc R . . C12 C 1.2722(3) -0.49133(15) 0.24178(14) 0.0469(4) Uani 1 1 d . . . H12 H 1.2550 -0.5363 0.1659 0.056 Uiso 1 1 calc R . . C13 C 1.0066(2) -0.05166(14) 0.70511(15) 0.0414(3) Uani 1 1 d . . . H13 H 0.9800 -0.0379 0.6360 0.050 Uiso 1 1 calc R . . C14 C 0.8947(3) -0.15002(17) 0.73847(19) 0.0542(5) Uani 1 1 d . . . H14 H 0.7834 -0.2123 0.6947 0.065 Uiso 1 1 calc R . . C15 C 0.9810(3) -0.13689(17) 0.84836(19) 0.0584(5) Uani 1 1 d . . . H15 H 0.9361 -0.1886 0.8907 0.070 Uiso 1 1 calc R . . C16 C 1.1479(3) -0.03186(16) 0.88435(15) 0.0501(4) Uani 1 1 d . . . H16 H 1.2318 -0.0029 0.9543 0.060 Uiso 1 1 calc R . . C17 C 1.1662(2) 0.02230(13) 0.79533(13) 0.0368(3) Uani 1 1 d . . . C18 C 1.3126(2) 0.14242(14) 0.79961(15) 0.0422(3) Uani 1 1 d . . . C19 C 1.3432(3) 0.14374(17) 0.67991(19) 0.0609(5) Uani 1 1 d . . . H19A H 1.2226 0.1326 0.6338 0.091 Uiso 1 1 calc R . . H19B H 1.3910 0.0787 0.6466 0.091 Uiso 1 1 calc R . . H19C H 1.4354 0.2207 0.6844 0.091 Uiso 1 1 calc R . . C20 C 1.5063(3) 0.1640(2) 0.8736(3) 0.0739(7) Uani 1 1 d . . . H20A H 1.5986 0.2386 0.8726 0.111 Uiso 1 1 calc R . . H20B H 1.5522 0.0970 0.8446 0.111 Uiso 1 1 calc R . . H20C H 1.4896 0.1701 0.9502 0.111 Uiso 1 1 calc R . . C21 C 1.2320(2) 0.24286(13) 0.85027(13) 0.0381(3) Uani 1 1 d . . . C22 C 1.0674(2) 0.24003(15) 0.89131(14) 0.0431(3) Uani 1 1 d . . . H22 H 0.9726 0.1706 0.8936 0.052 Uiso 1 1 calc R . . C23 C 1.0660(3) 0.36171(16) 0.92995(14) 0.0495(4) Uani 1 1 d . . . H23 H 0.9707 0.3869 0.9625 0.059 Uiso 1 1 calc R . . C24 C 1.2284(3) 0.43423(16) 0.91072(16) 0.0538(4) Uani 1 1 d . . . H24 H 1.2653 0.5188 0.9278 0.065 Uiso 1 1 calc R . . N1 N 1.1732(2) -0.41515(13) 0.28487(11) 0.0430(3) Uani 1 1 d . . . H1A H 1.0847 -0.4007 0.2456 0.052 Uiso 1 1 calc R . . N2 N 1.3292(2) 0.36202(13) 0.86184(14) 0.0498(3) Uani 1 1 d . . . H2A H 1.4377 0.3877 0.8414 0.060 Uiso 1 1 calc R . . Fe Fe 1.16871(3) -0.154505(18) 0.740439(17) 0.03432(7) 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 0.0626(10) 0.0331(7) 0.0445(8) 0.0194(6) 0.0214(7) 0.0212(7) C2 0.0889(14) 0.0580(10) 0.0408(8) 0.0253(8) 0.0176(9) 0.0452(10) C3 0.0577(10) 0.0742(13) 0.0400(8) 0.0109(8) 0.0007(7) 0.0397(10) C4 0.0325(6) 0.0451(8) 0.0408(7) 0.0088(6) 0.0080(5) 0.0165(6) C5 0.0360(6) 0.0328(6) 0.0335(6) 0.0127(5) 0.0100(5) 0.0162(5) C6 0.0348(6) 0.0349(6) 0.0339(6) 0.0137(5) 0.0070(5) 0.0120(5) C7 0.0363(7) 0.0561(10) 0.0515(9) 0.0130(8) 0.0033(6) 0.0161(7) C8 0.0653(10) 0.0408(8) 0.0440(8) 0.0207(7) 0.0161(7) 0.0225(7) C9 0.0367(6) 0.0330(6) 0.0307(6) 0.0114(5) 0.0068(5) 0.0086(5) C10 0.0439(8) 0.0418(7) 0.0354(7) 0.0116(6) 0.0082(6) 0.0182(6) C11 0.0529(9) 0.0417(8) 0.0476(8) 0.0123(7) 0.0193(7) 0.0190(7) C12 0.0560(9) 0.0415(8) 0.0357(7) 0.0054(6) 0.0150(7) 0.0087(7) C13 0.0375(7) 0.0402(7) 0.0517(9) 0.0146(6) 0.0130(6) 0.0189(6) C14 0.0399(8) 0.0427(8) 0.0793(13) 0.0136(8) 0.0266(8) 0.0120(7) C15 0.0776(13) 0.0437(9) 0.0693(12) 0.0262(8) 0.0491(11) 0.0230(9) C16 0.0754(12) 0.0455(8) 0.0380(8) 0.0147(6) 0.0232(8) 0.0270(8) C17 0.0404(7) 0.0328(6) 0.0425(7) 0.0129(5) 0.0177(6) 0.0156(5) C18 0.0384(7) 0.0337(7) 0.0549(9) 0.0131(6) 0.0143(6) 0.0113(6) C19 0.0769(13) 0.0388(8) 0.0738(13) 0.0199(8) 0.0470(11) 0.0158(8) C20 0.0426(10) 0.0546(12) 0.114(2) 0.0178(12) -0.0016(11) 0.0138(9) C21 0.0434(7) 0.0313(6) 0.0377(7) 0.0095(5) 0.0068(6) 0.0111(5) C22 0.0485(8) 0.0379(7) 0.0425(8) 0.0096(6) 0.0124(6) 0.0150(6) C23 0.0636(11) 0.0471(9) 0.0396(8) 0.0060(7) 0.0090(7) 0.0282(8) C24 0.0728(12) 0.0336(7) 0.0509(10) 0.0068(7) 0.0034(8) 0.0200(8) N1 0.0461(7) 0.0467(7) 0.0327(6) 0.0113(5) 0.0040(5) 0.0123(6) N2 0.0525(8) 0.0333(6) 0.0598(9) 0.0126(6) 0.0127(7) 0.0096(6) Fe 0.04049(12) 0.03293(11) 0.03560(11) 0.01421(8) 0.01390(8) 0.01558(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.413(3) . ? C1 C5 1.425(2) . ? C1 Fe 2.0408(15) . ? C1 H1 0.9300 . ? C2 C3 1.403(3) . ? C2 Fe 2.0318(17) . ? C2 H2 0.9300 . ? C3 C4 1.418(2) . ? C3 Fe 2.0305(17) . ? C3 H3 0.9300 . ? C4 C5 1.428(2) . ? C4 Fe 2.0492(15) . ? C4 H4 0.9300 . ? C5 C6 1.5098(19) . ? C5 Fe 2.0609(13) . ? C6 C9 1.516(2) . ? C6 C8 1.531(2) . ? C6 C7 1.541(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.361(2) . ? C9 N1 1.3697(18) . ? C10 C11 1.415(2) . ? C10 H10 0.9300 . ? C11 C12 1.354(3) . ? C11 H11 0.9300 . ? C12 N1 1.364(2) . ? C12 H12 0.9300 . ? C13 C14 1.420(2) . ? C13 C17 1.424(2) . ? C13 Fe 2.0437(15) . ? C13 H13 0.9300 . ? C14 C15 1.396(3) . ? C14 Fe 2.0318(18) . ? C14 H14 0.9300 . ? C15 C16 1.412(3) . ? C15 Fe 2.0402(17) . ? C15 H15 0.9300 . ? C16 C17 1.426(2) . ? C16 Fe 2.0464(16) . ? C16 H16 0.9300 . ? C17 C18 1.516(2) . ? C17 Fe 2.0571(14) . ? C18 C21 1.514(2) . ? C18 C20 1.529(3) . ? C18 C19 1.534(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.358(2) . ? C21 N2 1.364(2) . ? C22 C23 1.416(2) . ? C22 H22 0.9300 . ? C23 C24 1.347(3) . ? C23 H23 0.9300 . ? C24 N2 1.363(2) . ? C24 H24 0.9300 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? 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 C2 C1 C5 108.49(16) . . ? C2 C1 Fe 69.36(10) . . ? C5 C1 Fe 70.44(8) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe C1 H1 126.0 . . ? C3 C2 C1 108.13(15) . . ? C3 C2 Fe 69.75(10) . . ? C1 C2 Fe 70.05(9) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 125.8 . . ? C2 C3 C4 108.52(16) . . ? C2 C3 Fe 69.85(11) . . ? C4 C3 Fe 70.38(9) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe C3 H3 125.6 . . ? C3 C4 C5 107.91(15) . . ? C3 C4 Fe 68.96(10) . . ? C5 C4 Fe 70.11(8) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe C4 H4 126.5 . . ? C1 C5 C4 106.95(13) . . ? C1 C5 C6 125.65(14) . . ? C4 C5 C6 127.09(13) . . ? C1 C5 Fe 68.92(8) . . ? C4 C5 Fe 69.23(8) . . ? C6 C5 Fe 131.76(9) . . ? C5 C6 C9 107.68(11) . . ? C5 C6 C8 111.41(12) . . ? C9 C6 C8 109.37(12) . . ? C5 C6 C7 110.25(12) . . ? C9 C6 C7 109.56(13) . . ? C8 C6 C7 108.55(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 106.83(13) . . ? C10 C9 C6 132.09(13) . . ? N1 C9 C6 121.08(13) . . ? C9 C10 C11 108.19(14) . . ? C9 C10 H10 125.9 . . ? C11 C10 H10 125.9 . . ? C12 C11 C10 107.09(15) . . ? C12 C11 H11 126.5 . . ? C10 C11 H11 126.5 . . ? C11 C12 N1 108.00(14) . . ? C11 C12 H12 126.0 . . ? N1 C12 H12 126.0 . . ? C14 C13 C17 108.44(16) . . ? C14 C13 Fe 69.15(10) . . ? C17 C13 Fe 70.19(8) . . ? C14 C13 H13 125.8 . . ? C17 C13 H13 125.8 . . ? Fe C13 H13 126.4 . . ? C15 C14 C13 108.04(16) . . ? C15 C14 Fe 70.28(11) . . ? C13 C14 Fe 70.06(9) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Fe C14 H14 125.3 . . ? C14 C15 C16 108.50(16) . . ? C14 C15 Fe 69.62(10) . . ? C16 C15 Fe 70.01(10) . . ? C14 C15 H15 125.8 . . ? C16 C15 H15 125.8 . . ? Fe C15 H15 126.2 . . ? C15 C16 C17 108.47(17) . . ? C15 C16 Fe 69.55(10) . . ? C17 C16 Fe 70.07(9) . . ? C15 C16 H16 125.8 . . ? C17 C16 H16 125.8 . . ? Fe C16 H16 126.2 . . ? C13 C17 C16 106.54(15) . . ? C13 C17 C18 126.01(14) . . ? C16 C17 C18 127.13(16) . . ? C13 C17 Fe 69.18(8) . . ? C16 C17 Fe 69.26(9) . . ? C18 C17 Fe 131.35(10) . . ? C21 C18 C17 107.25(12) . . ? C21 C18 C20 109.67(15) . . ? C17 C18 C20 110.71(15) . . ? C21 C18 C19 109.14(15) . . ? C17 C18 C19 110.76(14) . . ? C20 C18 C19 109.27(18) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N2 107.21(14) . . ? C22 C21 C18 131.73(14) . . ? N2 C21 C18 121.06(14) . . ? C21 C22 C23 107.76(15) . . ? C21 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? C24 C23 C22 107.25(16) . . ? C24 C23 H23 126.4 . . ? C22 C23 H23 126.4 . . ? C23 C24 N2 108.07(15) . . ? C23 C24 H24 126.0 . . ? N2 C24 H24 126.0 . . ? C12 N1 C9 109.90(14) . . ? C12 N1 H1A 125.1 . . ? C9 N1 H1A 125.1 . . ? C24 N2 C21 109.70(15) . . ? C24 N2 H2A 125.1 . . ? C21 N2 H2A 125.1 . . ? C3 Fe C14 163.78(9) . . ? C3 Fe C2 40.40(9) . . ? C14 Fe C2 125.30(9) . . ? C3 Fe C15 127.14(9) . . ? C14 Fe C15 40.09(9) . . ? C2 Fe C15 104.35(8) . . ? C3 Fe C1 68.10(8) . . ? C14 Fe C1 105.59(7) . . ? C2 Fe C1 40.59(7) . . ? C15 Fe C1 113.48(7) . . ? C3 Fe C13 154.24(9) . . ? C14 Fe C13 40.79(7) . . ? C2 Fe C13 165.17(8) . . ? C15 Fe C13 67.84(8) . . ? C1 Fe C13 129.37(7) . . ? C3 Fe C16 108.61(8) . . ? C14 Fe C16 67.95(9) . . ? C2 Fe C16 114.99(7) . . ? C15 Fe C16 40.44(8) . . ? C1 Fe C16 146.84(7) . . ? C13 Fe C16 67.89(7) . . ? C3 Fe C4 40.67(7) . . ? C14 Fe C4 152.64(8) . . ? C2 Fe C4 68.24(8) . . ? C15 Fe C4 167.26(8) . . ? C1 Fe C4 68.18(7) . . ? C13 Fe C4 121.69(7) . . ? C16 Fe C4 131.96(7) . . ? C3 Fe C17 119.81(8) . . ? C14 Fe C17 68.70(7) . . ? C2 Fe C17 150.03(8) . . ? C15 Fe C17 68.40(6) . . ? C1 Fe C17 169.37(7) . . ? C13 Fe C17 40.62(6) . . ? C16 Fe C17 40.67(6) . . ? C4 Fe C17 112.47(6) . . ? C3 Fe C5 68.44(6) . . ? C14 Fe C5 117.22(7) . . ? C2 Fe C5 68.47(6) . . ? C15 Fe C5 147.87(8) . . ? C1 Fe C5 40.65(6) . . ? C13 Fe C5 110.97(6) . . ? C16 Fe C5 171.35(7) . . ? C4 Fe C5 40.66(6) . . ? C17 Fe C5 132.96(5) . . ? 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 C5 C1 C2 C3 0.21(19) . . . . ? Fe C1 C2 C3 -59.58(12) . . . . ? C5 C1 C2 Fe 59.79(11) . . . . ? C1 C2 C3 C4 -0.2(2) . . . . ? Fe C2 C3 C4 -59.99(12) . . . . ? C1 C2 C3 Fe 59.76(12) . . . . ? C2 C3 C4 C5 0.16(19) . . . . ? Fe C3 C4 C5 -59.51(10) . . . . ? C2 C3 C4 Fe 59.66(13) . . . . ? C2 C1 C5 C4 -0.11(17) . . . . ? Fe C1 C5 C4 59.01(10) . . . . ? C2 C1 C5 C6 173.87(13) . . . . ? Fe C1 C5 C6 -127.01(13) . . . . ? C2 C1 C5 Fe -59.12(11) . . . . ? C3 C4 C5 C1 -0.03(17) . . . . ? Fe C4 C5 C1 -58.81(10) . . . . ? C3 C4 C5 C6 -173.90(14) . . . . ? Fe C4 C5 C6 127.31(13) . . . . ? C3 C4 C5 Fe 58.79(11) . . . . ? C1 C5 C6 C9 -85.21(16) . . . . ? C4 C5 C6 C9 87.57(16) . . . . ? Fe C5 C6 C9 -177.90(10) . . . . ? C1 C5 C6 C8 154.87(14) . . . . ? C4 C5 C6 C8 -32.35(19) . . . . ? Fe C5 C6 C8 62.17(17) . . . . ? C1 C5 C6 C7 34.27(19) . . . . ? C4 C5 C6 C7 -152.95(14) . . . . ? Fe C5 C6 C7 -58.42(17) . . . . ? C5 C6 C9 C10 -10.4(2) . . . . ? C8 C6 C9 C10 110.77(18) . . . . ? C7 C6 C9 C10 -130.36(17) . . . . ? C5 C6 C9 N1 170.21(13) . . . . ? C8 C6 C9 N1 -68.58(18) . . . . ? C7 C6 C9 N1 50.28(18) . . . . ? N1 C9 C10 C11 -0.43(17) . . . . ? C6 C9 C10 C11 -179.85(15) . . . . ? C9 C10 C11 C12 0.18(19) . . . . ? C10 C11 C12 N1 0.15(19) . . . . ? C17 C13 C14 C15 0.90(19) . . . . ? Fe C13 C14 C15 60.29(13) . . . . ? C17 C13 C14 Fe -59.39(10) . . . . ? C13 C14 C15 C16 -0.7(2) . . . . ? Fe C14 C15 C16 59.42(13) . . . . ? C13 C14 C15 Fe -60.15(11) . . . . ? C14 C15 C16 C17 0.3(2) . . . . ? Fe C15 C16 C17 59.47(12) . . . . ? C14 C15 C16 Fe -59.18(13) . . . . ? C14 C13 C17 C16 -0.71(17) . . . . ? Fe C13 C17 C16 -59.46(11) . . . . ? C14 C13 C17 C18 -174.57(14) . . . . ? Fe C13 C17 C18 126.68(14) . . . . ? C14 C13 C17 Fe 58.75(11) . . . . ? C15 C16 C17 C13 0.27(18) . . . . ? Fe C16 C17 C13 59.41(10) . . . . ? C15 C16 C17 C18 174.04(15) . . . . ? Fe C16 C17 C18 -126.82(15) . . . . ? C15 C16 C17 Fe -59.14(12) . . . . ? C13 C17 C18 C21 87.70(18) . . . . ? C16 C17 C18 C21 -84.91(19) . . . . ? Fe C17 C18 C21 -179.19(12) . . . . ? C13 C17 C18 C20 -152.68(17) . . . . ? C16 C17 C18 C20 34.7(2) . . . . ? Fe C17 C18 C20 -59.6(2) . . . . ? C13 C17 C18 C19 -31.3(2) . . . . ? C16 C17 C18 C19 156.08(17) . . . . ? Fe C17 C18 C19 61.8(2) . . . . ? C17 C18 C21 C22 2.4(3) . . . . ? C20 C18 C21 C22 -117.9(2) . . . . ? C19 C18 C21 C22 122.4(2) . . . . ? C17 C18 C21 N2 -177.92(15) . . . . ? C20 C18 C21 N2 61.8(2) . . . . ? C19 C18 C21 N2 -57.9(2) . . . . ? N2 C21 C22 C23 -0.54(19) . . . . ? C18 C21 C22 C23 179.18(17) . . . . ? C21 C22 C23 C24 0.3(2) . . . . ? C22 C23 C24 N2 0.0(2) . . . . ? C11 C12 N1 C9 -0.43(19) . . . . ? C10 C9 N1 C12 0.53(18) . . . . ? C6 C9 N1 C12 -179.97(13) . . . . ? C23 C24 N2 C21 -0.4(2) . . . . ? C22 C21 N2 C24 0.6(2) . . . . ? C18 C21 N2 C24 -179.18(15) . . . . ? C2 C3 Fe C14 32.1(3) . . . . ? C4 C3 Fe C14 151.4(3) . . . . ? C4 C3 Fe C2 119.34(15) . . . . ? C2 C3 Fe C15 65.77(14) . . . . ? C4 C3 Fe C15 -174.89(10) . . . . ? C2 C3 Fe C1 -37.77(10) . . . . ? C4 C3 Fe C1 81.56(11) . . . . ? C2 C3 Fe C13 -175.50(14) . . . . ? C4 C3 Fe C13 -56.2(2) . . . . ? C2 C3 Fe C16 106.98(11) . . . . ? C4 C3 Fe C16 -133.69(11) . . . . ? C2 C3 Fe C4 -119.34(15) . . . . ? C2 C3 Fe C17 150.14(10) . . . . ? C4 C3 Fe C17 -90.53(11) . . . . ? C2 C3 Fe C5 -81.68(11) . . . . ? C4 C3 Fe C5 37.66(10) . . . . ? C15 C14 Fe C3 43.4(3) . . . . ? C13 C14 Fe C3 162.1(2) . . . . ? C15 C14 Fe C2 68.32(14) . . . . ? C13 C14 Fe C2 -173.00(10) . . . . ? C13 C14 Fe C15 118.69(15) . . . . ? C15 C14 Fe C1 108.11(11) . . . . ? C13 C14 Fe C1 -133.20(10) . . . . ? C15 C14 Fe C13 -118.69(16) . . . . ? C15 C14 Fe C16 -37.44(11) . . . . ? C13 C14 Fe C16 81.24(11) . . . . ? C15 C14 Fe C4 -179.36(13) . . . . ? C13 C14 Fe C4 -60.67(19) . . . . ? C15 C14 Fe C17 -81.35(11) . . . . ? C13 C14 Fe C17 37.33(10) . . . . ? C15 C14 Fe C5 150.18(10) . . . . ? C13 C14 Fe C5 -91.13(11) . . . . ? C1 C2 Fe C3 -119.13(15) . . . . ? C3 C2 Fe C14 -169.53(11) . . . . ? C1 C2 Fe C14 71.33(14) . . . . ? C3 C2 Fe C15 -131.38(12) . . . . ? C1 C2 Fe C15 109.49(12) . . . . ? C3 C2 Fe C1 119.13(15) . . . . ? C3 C2 Fe C13 172.3(2) . . . . ? C1 C2 Fe C13 53.2(3) . . . . ? C3 C2 Fe C16 -89.75(12) . . . . ? C1 C2 Fe C16 151.11(11) . . . . ? C3 C2 Fe C4 37.71(10) . . . . ? C1 C2 Fe C4 -81.42(11) . . . . ? C3 C2 Fe C17 -59.86(18) . . . . ? C1 C2 Fe C17 -178.99(11) . . . . ? C3 C2 Fe C5 81.61(11) . . . . ? C1 C2 Fe C5 -37.52(10) . . . . ? C14 C15 Fe C3 -166.07(12) . . . . ? C16 C15 Fe C3 74.25(15) . . . . ? C16 C15 Fe C14 -119.68(16) . . . . ? C14 C15 Fe C2 -128.48(12) . . . . ? C16 C15 Fe C2 111.84(12) . . . . ? C14 C15 Fe C1 -86.51(12) . . . . ? C16 C15 Fe C1 153.81(11) . . . . ? C14 C15 Fe C13 38.23(11) . . . . ? C16 C15 Fe C13 -81.45(12) . . . . ? C14 C15 Fe C16 119.68(16) . . . . ? C14 C15 Fe C4 178.7(3) . . . . ? C16 C15 Fe C4 59.0(3) . . . . ? C14 C15 Fe C17 82.16(11) . . . . ? C16 C15 Fe C17 -37.52(11) . . . . ? C14 C15 Fe C5 -56.24(17) . . . . ? C16 C15 Fe C5 -175.92(10) . . . . ? C2 C1 Fe C3 37.60(12) . . . . ? C5 C1 Fe C3 -81.97(11) . . . . ? C2 C1 Fe C14 -126.61(13) . . . . ? C5 C1 Fe C14 113.83(11) . . . . ? C5 C1 Fe C2 -119.57(15) . . . . ? C2 C1 Fe C15 -84.74(14) . . . . ? C5 C1 Fe C15 155.70(11) . . . . ? C2 C1 Fe C13 -164.62(11) . . . . ? C5 C1 Fe C13 75.81(12) . . . . ? C2 C1 Fe C16 -53.18(19) . . . . ? C5 C1 Fe C16 -172.75(12) . . . . ? C2 C1 Fe C4 81.57(12) . . . . ? C5 C1 Fe C4 -37.99(9) . . . . ? C2 C1 Fe C17 177.3(3) . . . . ? C5 C1 Fe C17 57.7(4) . . . . ? C2 C1 Fe C5 119.57(15) . . . . ? C14 C13 Fe C3 -168.59(16) . . . . ? C17 C13 Fe C3 -48.8(2) . . . . ? C17 C13 Fe C14 119.80(15) . . . . ? C14 C13 Fe C2 22.9(3) . . . . ? C17 C13 Fe C2 142.7(2) . . . . ? C14 C13 Fe C15 -37.60(12) . . . . ? C17 C13 Fe C15 82.20(11) . . . . ? C14 C13 Fe C1 65.25(14) . . . . ? C17 C13 Fe C1 -174.95(8) . . . . ? C14 C13 Fe C16 -81.41(12) . . . . ? C17 C13 Fe C16 38.39(9) . . . . ? C14 C13 Fe C4 151.91(11) . . . . ? C17 C13 Fe C4 -88.29(10) . . . . ? C14 C13 Fe C17 -119.80(15) . . . . ? C14 C13 Fe C5 107.81(12) . . . . ? C17 C13 Fe C5 -132.39(9) . . . . ? C15 C16 Fe C3 -125.95(14) . . . . ? C17 C16 Fe C3 114.39(12) . . . . ? C15 C16 Fe C14 37.13(13) . . . . ? C17 C16 Fe C14 -82.52(12) . . . . ? C15 C16 Fe C2 -82.81(15) . . . . ? C17 C16 Fe C2 157.54(11) . . . . ? C17 C16 Fe C15 -119.66(17) . . . . ? C15 C16 Fe C1 -47.7(2) . . . . ? C17 C16 Fe C1 -167.39(12) . . . . ? C15 C16 Fe C13 81.31(13) . . . . ? C17 C16 Fe C13 -38.35(10) . . . . ? C15 C16 Fe C4 -165.28(12) . . . . ? C17 C16 Fe C4 75.06(13) . . . . ? C15 C16 Fe C17 119.66(17) . . . . ? C15 C16 Fe C5 165.4(4) . . . . ? C17 C16 Fe C5 45.8(5) . . . . ? C5 C4 Fe C3 119.31(15) . . . . ? C3 C4 Fe C14 -163.09(15) . . . . ? C5 C4 Fe C14 -43.77(18) . . . . ? C3 C4 Fe C2 -37.47(12) . . . . ? C5 C4 Fe C2 81.85(10) . . . . ? C3 C4 Fe C15 18.8(3) . . . . ? C5 C4 Fe C15 138.1(3) . . . . ? C3 C4 Fe C1 -81.34(12) . . . . ? C5 C4 Fe C1 37.98(9) . . . . ? C3 C4 Fe C13 154.90(12) . . . . ? C5 C4 Fe C13 -85.79(10) . . . . ? C3 C4 Fe C16 67.17(14) . . . . ? C5 C4 Fe C16 -173.52(8) . . . . ? C3 C4 Fe C17 110.12(12) . . . . ? C5 C4 Fe C17 -130.56(9) . . . . ? C3 C4 Fe C5 -119.31(15) . . . . ? C13 C17 Fe C3 157.86(10) . . . . ? C16 C17 Fe C3 -84.12(13) . . . . ? C18 C17 Fe C3 37.65(18) . . . . ? C13 C17 Fe C14 -37.48(11) . . . . ? C16 C17 Fe C14 80.54(13) . . . . ? C18 C17 Fe C14 -157.69(18) . . . . ? C13 C17 Fe C2 -161.90(15) . . . . ? C16 C17 Fe C2 -43.88(19) . . . . ? C18 C17 Fe C2 77.9(2) . . . . ? C13 C17 Fe C15 -80.70(11) . . . . ? C16 C17 Fe C15 37.32(13) . . . . ? C18 C17 Fe C15 159.09(18) . . . . ? C13 C17 Fe C1 21.6(4) . . . . ? C16 C17 Fe C1 139.7(3) . . . . ? C18 C17 Fe C1 -98.6(3) . . . . ? C16 C17 Fe C13 118.02(14) . . . . ? C18 C17 Fe C13 -120.21(19) . . . . ? C13 C17 Fe C16 -118.02(14) . . . . ? C18 C17 Fe C16 121.8(2) . . . . ? C13 C17 Fe C4 113.02(10) . . . . ? C16 C17 Fe C4 -128.97(11) . . . . ? C18 C17 Fe C4 -7.19(17) . . . . ? C13 C17 Fe C5 70.45(11) . . . . ? C16 C17 Fe C5 -171.53(10) . . . . ? C18 C17 Fe C5 -49.76(19) . . . . ? C1 C5 Fe C3 81.06(12) . . . . ? C4 C5 Fe C3 -37.66(11) . . . . ? C6 C5 Fe C3 -159.39(16) . . . . ? C1 C5 Fe C14 -82.24(11) . . . . ? C4 C5 Fe C14 159.05(10) . . . . ? C6 C5 Fe C14 37.32(16) . . . . ? C1 C5 Fe C2 37.47(11) . . . . ? C4 C5 Fe C2 -81.24(11) . . . . ? C6 C5 Fe C2 157.03(16) . . . . ? C1 C5 Fe C15 -45.21(17) . . . . ? C4 C5 Fe C15 -163.93(14) . . . . ? C6 C5 Fe C15 74.34(19) . . . . ? C4 C5 Fe C1 -118.71(13) . . . . ? C6 C5 Fe C1 119.55(17) . . . . ? C1 C5 Fe C13 -126.62(10) . . . . ? C4 C5 Fe C13 114.67(9) . . . . ? C6 C5 Fe C13 -7.06(15) . . . . ? C1 C5 Fe C16 152.7(4) . . . . ? C4 C5 Fe C16 33.9(4) . . . . ? C6 C5 Fe C16 -87.8(4) . . . . ? C1 C5 Fe C4 118.71(13) . . . . ? C6 C5 Fe C4 -121.73(17) . . . . ? C1 C5 Fe C17 -167.69(10) . . . . ? C4 C5 Fe C17 73.59(11) . . . . ? C6 C5 Fe C17 -48.14(16) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.776 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.068 # Attachment 'Ru-Dimer_7_.CIF' data_394rk22m _database_code_depnum_ccdc_archive 'CCDC 732751' #TrackingRef 'Ru-Dimer_7_.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H38 F10 N4 Ru2' _chemical_formula_weight 1231.10 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' 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' Ru Ru -1.2594 0.8363 '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 11.2539(10) _cell_length_b 11.5076(10) _cell_length_c 12.2368(11) _cell_angle_alpha 117.3260(10) _cell_angle_beta 99.1430(10) _cell_angle_gamma 107.6930(10) _cell_volume 1255.16(19) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1348 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 18.5 _exptl_crystal_description BLOCKS _exptl_crystal_colour RED _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.6837 _exptl_absorpt_correction_T_max 0.7477 _exptl_special_details ; In the case of Cp ring the three atoms with reasonably good temperature factor could be located from the difference Fourier map and the rest two attached to the regular pentagon ( with C-C-default value 1.42) is fitted to the C5 ring as a rigid group by AFIX 59 command. Finally the Cp ring is refined anisotropiacally and hydrogen atoms are fixed to the Cp. This has improved the thermal ellipsoids and the bond angles and distances of the Cp ring considerably. The methyl groups(C28, C29)also showed high thermal ellipsoids and the disordered position is modelled by using FVAR command and C-C bond length is restrained to 1.52 A. Disordered atoms are refined only isotropically and no hydrogen atoms are fixed to the disordered methyl groups.Phenyl ring C17-C23 is also restrained for C-C bond legth 1.39A and the C17 carbon atom is resfined only isotropically. The high residual electron density peaks are located near to the Ru atom (0.87A and 0.95) which is probably ripples around the heavy metal. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8079 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3893 _reflns_number_gt 3647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0000P)^2^+27.8171P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3893 _refine_ls_number_parameters 319 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.1092 _refine_ls_wR_factor_ref 0.2328 _refine_ls_wR_factor_gt 0.2284 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.178 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.33513(9) 0.59455(12) 1.20289(13) 0.0600(5) Uani 1 d . . . F1 F 0.1610(6) -0.0042(6) 0.5336(6) 0.0358(14) Uani 1 d . . . F2 F -0.0588(6) -0.1999(7) 0.3202(6) 0.0450(16) Uani 1 d . . . F3 F -0.2200(6) -0.4459(7) 0.2981(6) 0.0484(17) Uani 1 d . . . F4 F -0.1556(6) -0.4957(6) 0.4910(6) 0.0382(15) Uani 1 d . . . F5 F 0.0626(6) -0.3008(6) 0.7052(6) 0.0341(14) Uani 1 d . . . N1 N 0.3317(8) 0.1496(8) 0.9840(8) 0.0241(17) Uani 1 d . . . H1C H 0.405(13) 0.153(14) 0.967(13) 0.06(4) Uiso 1 d . . . N2 N 0.4844(8) 0.0850(8) 0.8386(9) 0.031(2) Uani 1 d . . . C1 C 0.1626(5) 0.5407(5) 1.0559(6) 0.078(4) Uani 1 d GU . . H1 H 0.1525 0.4884 0.9676 0.094 Uiso 1 calc R . . C2 C 0.1197(4) 0.4808(5) 1.1304(6) 0.056(3) Uani 1 d GU . . H2 H 0.0770 0.3828 1.0990 0.068 Uiso 1 calc R . . C3 C 0.1543(5) 0.5985(6) 1.2619(7) 0.072(4) Uani 1 d GU . . H3 H 0.1379 0.5903 1.3307 0.086 Uiso 1 calc R . . C4 C 0.2185(5) 0.7311(6) 1.2687(7) 0.064(3) Uani 1 d GU . . H4 H 0.2512 0.8241 1.3427 0.077 Uiso 1 calc R . . C5 C 0.2237(5) 0.6955(6) 1.1413(7) 0.047(3) Uani 1 d GU . . C6 C 0.5428(4) 0.7203(4) 1.3305(5) 0.024(2) Uani 1 d G . . H6 H 0.5808 0.8196 1.3915 0.029 Uiso 1 calc R . . C7 C 0.5382(4) 0.6537(5) 1.2023(5) 0.039(3) Uani 1 d G . . H7 H 0.5731 0.7002 1.1618 0.046 Uiso 1 calc R . . C8 C 0.4710(4) 0.5021(4) 1.1430(4) 0.048(3) Uani 1 d G . . H8 H 0.4528 0.4325 1.0560 0.058 Uiso 1 calc R . . C9 C 0.4362(3) 0.4732(4) 1.2365(3) 0.028(2) Uani 1 d G . . C10 C 0.4796(4) 0.6109(4) 1.3530(4) 0.025(2) Uani 1 d G . . H10 H 0.4683 0.6267 1.4315 0.030 Uiso 1 calc R . . C11 C 0.3771(4) 0.3254(4) 1.2200(4) 0.029(2) Uani 1 d G . . C12 C 0.2861(5) 0.2092(5) 1.0792(5) 0.027(2) Uani 1 d G . . C13 C 0.1448(5) 0.1440(5) 1.0251(6) 0.029(2) Uani 1 d G . . H13 H 0.0877 0.1653 1.0704 0.034 Uiso 1 calc R . . C14 C 0.1079(9) 0.0437(10) 0.8935(9) 0.024(2) Uani 1 d . . . H14 H 0.0211 -0.0147 0.8334 0.029 Uiso 1 calc R . . C15 C 0.2256(9) 0.0454(9) 0.8657(8) 0.0205(19) Uani 1 d . . . C16 C 0.2427(9) -0.0343(10) 0.7486(10) 0.028(2) Uani 1 d . . . C17 C 0.1189(8) -0.1443(9) 0.6288(8) 0.023(2) Uiso 1 d DU . . C18 C 0.0346(8) -0.2722(8) 0.6125(9) 0.030(2) Uani 1 d DU . . C19 C -0.0788(8) -0.3736(9) 0.5019(8) 0.028(2) Uani 1 d DU . . C20 C -0.1115(9) -0.3487(10) 0.4034(9) 0.035(2) Uani 1 d DU . . C21 C -0.0292(8) -0.2230(9) 0.4154(9) 0.034(2) Uani 1 d DU . . C22 C 0.0837(9) -0.1240(9) 0.5272(8) 0.029(2) Uani 1 d DU . . C23 C 0.3654(9) -0.0199(9) 0.7310(9) 0.022(2) Uani 1 d . . . C24 C 0.3976(10) -0.0894(10) 0.6202(11) 0.033(2) Uani 1 d . . . H24 H 0.3376 -0.1655 0.5368 0.039 Uiso 1 calc R . . C25 C 0.5327(10) -0.0258(10) 0.6559(11) 0.036(3) Uani 1 d . . . H25 H 0.5820 -0.0488 0.6015 0.043 Uiso 1 calc R . . C26 C 0.5837(9) 0.0819(10) 0.7918(11) 0.032(2) Uani 1 d . . . C27 C 0.7283(9) 0.1847(10) 0.8826(10) 0.032(2) Uani 1 d D . . C28 C 0.8160(14) 0.1045(15) 0.8677(16) 0.031(3) Uiso 0.68 d PD A 1 C29 C 0.7374(16) 0.2623(19) 1.0288(13) 0.034(4) Uiso 0.66 d PD A 1 C28A C 0.810(3) 0.114(3) 0.807(3) 0.033(8) Uiso 0.31 d PD A 2 C29A C 0.741(3) 0.194(4) 1.012(2) 0.035(7) Uiso 0.34 d PD A 2 C30 C 0.4954(10) 0.2915(11) 1.2548(11) 0.037(3) Uani 1 d . . . H30A H 0.4620 0.1969 1.2414 0.056 Uiso 1 calc R . . H30B H 0.5511 0.3624 1.3452 0.056 Uiso 1 calc R . . H30C H 0.5464 0.2943 1.1995 0.056 Uiso 1 calc R . . C31 C 0.2992(11) 0.3282(11) 1.3126(10) 0.034(2) Uani 1 d . . . H31A H 0.2282 0.3534 1.2933 0.051 Uiso 1 calc R . . H31B H 0.3580 0.3986 1.4020 0.051 Uiso 1 calc R . . H31C H 0.2626 0.2343 1.3004 0.051 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0253(5) 0.0474(7) 0.0952(9) 0.0560(7) -0.0159(5) -0.0083(4) F1 0.039(3) 0.035(3) 0.037(3) 0.023(3) 0.013(3) 0.012(3) F2 0.045(4) 0.060(4) 0.028(3) 0.024(3) 0.006(3) 0.023(3) F3 0.025(3) 0.049(4) 0.033(4) 0.007(3) -0.004(3) 0.003(3) F4 0.029(3) 0.022(3) 0.042(4) 0.008(3) 0.012(3) 0.001(2) F5 0.033(3) 0.028(3) 0.036(3) 0.019(3) 0.007(3) 0.007(3) N1 0.023(4) 0.025(4) 0.025(4) 0.013(4) 0.011(4) 0.012(4) N2 0.018(4) 0.021(4) 0.045(5) 0.018(4) 0.004(4) 0.003(3) C1 0.062(9) 0.062(7) 0.076(8) 0.039(6) -0.024(7) 0.006(7) C2 0.022(6) 0.041(6) 0.090(8) 0.043(6) -0.008(6) -0.002(5) C3 0.040(7) 0.081(9) 0.101(9) 0.057(7) 0.027(8) 0.020(7) C4 0.054(8) 0.075(7) 0.092(8) 0.055(7) 0.035(8) 0.040(7) C5 0.018(5) 0.047(6) 0.067(7) 0.040(6) -0.009(5) -0.001(5) C6 0.024(5) 0.012(4) 0.023(5) -0.001(4) 0.007(4) 0.008(4) C7 0.047(7) 0.023(5) 0.031(6) 0.013(5) 0.011(5) 0.002(5) C8 0.072(8) 0.023(6) 0.024(6) 0.009(5) 0.013(6) -0.001(6) C9 0.025(5) 0.025(5) 0.030(6) 0.016(5) 0.004(4) 0.007(4) C10 0.028(5) 0.026(5) 0.022(5) 0.011(4) 0.013(4) 0.016(4) C11 0.033(5) 0.020(5) 0.023(5) 0.012(4) 0.000(4) 0.001(4) C12 0.026(5) 0.019(5) 0.031(6) 0.015(4) 0.006(4) 0.006(4) C13 0.024(5) 0.029(5) 0.030(6) 0.015(5) 0.014(4) 0.008(4) C14 0.017(4) 0.022(5) 0.028(5) 0.009(4) 0.008(4) 0.006(4) C15 0.027(5) 0.012(4) 0.014(5) 0.002(4) 0.005(4) 0.008(4) C16 0.021(5) 0.020(5) 0.036(6) 0.017(5) -0.002(4) 0.003(4) C18 0.026(5) 0.027(5) 0.032(5) 0.014(4) 0.008(4) 0.010(4) C19 0.018(4) 0.021(5) 0.031(5) 0.005(4) 0.010(4) 0.005(4) C20 0.020(5) 0.030(5) 0.032(5) 0.006(4) 0.000(4) 0.007(4) C21 0.027(5) 0.042(6) 0.030(5) 0.018(5) 0.006(4) 0.016(4) C22 0.030(5) 0.022(5) 0.026(5) 0.008(4) 0.008(4) 0.010(4) C23 0.025(5) 0.014(4) 0.016(5) -0.002(4) 0.011(4) 0.010(4) C24 0.033(6) 0.015(5) 0.037(6) 0.007(5) 0.009(5) 0.008(4) C25 0.032(6) 0.021(5) 0.045(7) 0.011(5) 0.012(5) 0.010(4) C26 0.020(5) 0.020(5) 0.052(7) 0.019(5) 0.008(5) 0.008(4) C27 0.021(5) 0.030(5) 0.042(6) 0.020(5) 0.007(5) 0.009(4) C30 0.029(6) 0.032(6) 0.036(6) 0.019(5) -0.004(5) 0.002(5) C31 0.038(6) 0.030(6) 0.030(6) 0.019(5) 0.010(5) 0.006(5) _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 Ru1 C1 2.127(4) . ? Ru1 C10 2.145(4) . ? Ru1 C8 2.154(4) . ? Ru1 C2 2.168(4) . ? Ru1 C6 2.169(4) . ? Ru1 C7 2.179(4) . ? Ru1 C9 2.180(3) . ? Ru1 C5 2.209(5) . ? Ru1 C3 2.271(5) . ? Ru1 C4 2.295(5) . ? F1 C22 1.347(10) . ? F2 C21 1.325(11) . ? F3 C20 1.322(10) . ? F4 C19 1.339(10) . ? F5 C18 1.337(11) . ? N1 C12 1.327(10) . ? N1 C15 1.395(12) . ? N1 H1C 0.88(13) . ? N2 C26 1.336(13) . ? N2 C23 1.408(12) . ? C1 C5 1.4335 . ? C1 C2 1.4336 . ? C1 H1 0.9300 . ? C2 C3 1.4334 . ? C2 H2 0.9300 . ? C3 C4 1.4326 . ? C3 H3 0.9300 . ? C4 C5 1.4343 . ? C4 H4 0.9300 . ? C5 C27 1.499(11) 2_667 ? C6 C7 1.3770 . ? C6 C10 1.4151 . ? C6 H6 0.9300 . ? C7 C8 1.4153 . ? C7 H7 0.9300 . ? C8 C9 1.4086 . ? C8 H8 0.9300 . ? C9 C10 1.4196 . ? C9 C11 1.5268 . ? C10 H10 0.9300 . ? C11 C12 1.5157 . ? C11 C31 1.535(11) . ? C11 C30 1.546(11) . ? C12 C13 1.4190 . ? C13 C14 1.374(11) . ? C13 H13 0.9300 . ? C14 C15 1.415(13) . ? C14 H14 0.9300 . ? C15 C16 1.386(14) . ? C16 C23 1.404(13) . ? C16 C17 1.505(12) . ? C17 C22 1.387(8) . ? C17 C18 1.388(8) . ? C18 C19 1.384(8) . ? C19 C20 1.382(8) . ? C20 C21 1.386(8) . ? C21 C22 1.386(8) . ? C23 C24 1.395(14) . ? C24 C25 1.363(14) . ? C24 H24 0.9300 . ? C25 C26 1.415(15) . ? C25 H25 0.9300 . ? C26 C27 1.527(13) . ? C27 C5 1.499(15) 2_667 ? C27 C28 1.521(14) . ? C27 C29A 1.525(10) . ? C27 C28A 1.545(18) . ? C27 C29 1.559(14) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 N1 C15 110.0(7) . . ? C12 N1 H1C 143(9) . . ? C15 N1 H1C 107(9) . . ? C26 N2 C23 106.4(8) . . ? C5 C1 C2 108.0 . . ? C5 C1 H1 126.0 . . ? C2 C1 H1 126.0 . . ? C3 C2 C1 108.0 . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? C4 C3 C2 108.0 . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C3 C4 C5 108.0 . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? C1 C5 C4 108.0 . . ? C1 C5 C27 132.8(5) . 2_667 ? C4 C5 C27 118.7(5) . 2_667 ? C7 C6 C10 107.9 . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? C6 C7 C8 108.1 . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Ru1 C7 H7 124.6 . . ? C9 C8 C7 109.3 . . ? C9 C8 H8 125.4 . . ? C7 C8 H8 125.4 . . ? C8 C9 C10 105.6 . . ? C8 C9 C11 127.0 . . ? C10 C9 C11 127.1 . . ? C10 C9 Ru1 69.48(11) . . ? C6 C10 C9 109.1 . . ? C6 C10 H10 125.5 . . ? C9 C10 H10 125.5 . . ? Ru1 C10 H10 122.2 . . ? C12 C11 C9 110.7 . . ? C12 C11 C31 109.5(5) . . ? C9 C11 C31 110.8(4) . . ? C12 C11 C30 109.2(5) . . ? C9 C11 C30 106.9(4) . . ? C31 C11 C30 109.6(6) . . ? N1 C12 C13 108.4(4) . . ? N1 C12 C11 122.7(4) . . ? C13 C12 C11 128.9 . . ? C14 C13 C12 107.4(5) . . ? C14 C13 H13 126.3 . . ? C12 C13 H13 126.3 . . ? C13 C14 C15 107.7(7) . . ? C13 C14 H14 126.1 . . ? C15 C14 H14 126.1 . . ? C16 C15 N1 123.1(8) . . ? C16 C15 C14 130.5(8) . . ? N1 C15 C14 106.4(8) . . ? C15 C16 C23 125.8(8) . . ? C15 C16 C17 117.3(8) . . ? C23 C16 C17 116.9(9) . . ? C22 C17 C18 116.1(8) . . ? C22 C17 C16 121.5(7) . . ? C18 C17 C16 122.4(7) . . ? F5 C18 C19 118.0(7) . . ? F5 C18 C17 119.8(7) . . ? C19 C18 C17 122.3(8) . . ? F4 C19 C20 120.5(7) . . ? F4 C19 C18 119.6(8) . . ? C20 C19 C18 120.0(8) . . ? F3 C20 C19 119.7(8) . . ? F3 C20 C21 120.8(8) . . ? C19 C20 C21 119.5(8) . . ? F2 C21 C20 119.8(7) . . ? F2 C21 C22 121.2(8) . . ? C20 C21 C22 119.0(8) . . ? F1 C22 C21 116.7(7) . . ? F1 C22 C17 120.2(7) . . ? C21 C22 C17 123.1(8) . . ? C24 C23 C16 132.0(9) . . ? C24 C23 N2 108.6(8) . . ? C16 C23 N2 119.3(8) . . ? C25 C24 C23 107.8(9) . . ? C25 C24 H24 126.1 . . ? C23 C24 H24 126.1 . . ? C24 C25 C26 106.8(10) . . ? C24 C25 H25 126.6 . . ? C26 C25 H25 126.6 . . ? N2 C26 C25 110.5(9) . . ? N2 C26 C27 120.5(9) . . ? C25 C26 C27 129.0(9) . . ? C5 C27 C28 113.1(9) 2_667 . ? C5 C27 C29A 129.2(16) 2_667 . ? C28 C27 C29A 84.9(16) . . ? C5 C27 C26 109.0(9) 2_667 . ? C28 C27 C26 111.7(9) . . ? C29A C27 C26 106.7(14) . . ? C5 C27 C28A 90.2(15) 2_667 . ? C29A C27 C28A 115(2) . . ? C26 C27 C28A 104.0(15) . . ? C5 C27 C29 104.6(10) 2_667 . ? C28 C27 C29 108.0(11) . . ? C26 C27 C29 110.2(9) . . ? C28A C27 C29 135.2(16) . . ? C11 C30 H30A 109.5 . . ? C11 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C11 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 C31 H31A 109.5 . . ? C11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.978 _refine_diff_density_min -4.531 _refine_diff_density_rms 0.174