# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ales.ruzicka@upce.cz _publ_contact_author_name 'Ales Ruzicka' loop_ _publ_author_name 'Josef Holub' 'Bohumil Stibr' 'Mario Bakardjiev' 'Ales Ruzicka' 'Zdenka Padelkova' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 810292' #TrackingRef 'jhl091216Fe2a_530-2akt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H27 B9 Fe' _chemical_formula_sum 'C13 H27 B9 Fe' _chemical_formula_weight 336.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7301(7) _cell_length_b 12.0972(12) _cell_length_c 26.5778(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3449.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 50955 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.862 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.147 0 0 1 0.245 1 0 0 0.136 -1 0 0 0.194 1 0 1 0.135 -1 0 1 0.195 0 1 0 0.208 0 -1 0 0.160 -1 1 0 0.176 1 1 0 0.164 1 -1 0 0.128 -1 -1 0 0.142 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(1) _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 Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50784 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3917 _reflns_number_gt 2898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _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^)+(0.0386P)^2^+4.5701P] 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 3917 _refine_ls_number_parameters 208 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.078 _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 Fe1 Fe 0.06085(3) 0.18821(3) 0.623509(12) 0.02014(11) Uani 1 1 d . . . B6 B -0.0008(3) 0.0746(2) 0.67705(11) 0.0269(6) Uani 1 1 d . . . H6 H 0.0408 0.0913 0.7141 0.032 Uiso 1 1 d R . . B3 B -0.1052(3) 0.1569(2) 0.58686(11) 0.0239(6) Uani 1 1 d . . . H3 H -0.1299 0.2288 0.5636 0.029 Uiso 1 1 d R . . C4 C 0.0100(2) 0.0656(2) 0.57294(9) 0.0250(5) Uani 1 1 d U . . H4 H 0.0642 0.0758 0.5381 0.030 Uiso 1 1 d R . . B11 B -0.1568(3) 0.0237(3) 0.67266(12) 0.0317(7) Uani 1 1 d . . . H11 H -0.2139 0.0094 0.7064 0.038 Uiso 1 1 d R . . C2 C -0.1156(2) 0.1513(2) 0.65053(9) 0.0231(5) Uani 1 1 d U . . H2 H -0.1518 0.2229 0.6715 0.028 Uiso 1 1 d R . . C14 C 0.0789(2) 0.3425(2) 0.66044(10) 0.0266(6) Uani 1 1 d . . . B5 B 0.0831(3) 0.0166(2) 0.62474(11) 0.0277(6) Uani 1 1 d . . . H5 H 0.1823 -0.0060 0.6264 0.033 Uiso 1 1 d R . . C13 C 0.0591(3) 0.3587(2) 0.60888(10) 0.0315(6) Uani 1 1 d . . . H13 H -0.0044 0.4056 0.5984 0.038 Uiso 1 1 d R . . B9 B -0.0234(3) -0.0670(3) 0.58987(12) 0.0299(7) Uani 1 1 d . . . H9 H 0.0079 -0.1407 0.5692 0.036 Uiso 1 1 d R . . B8 B -0.1406(3) 0.0205(2) 0.56581(11) 0.0272(6) Uani 1 1 d . . . H8 H -0.1859 0.0047 0.5294 0.033 Uiso 1 1 d R . . C15 C 0.1777(3) 0.2738(2) 0.67605(11) 0.0320(6) Uani 1 1 d . . . C16 C 0.2517(3) 0.2194(3) 0.63983(14) 0.0436(8) Uani 1 1 d U . . C18 C 0.1335(3) 0.3055(3) 0.57264(10) 0.0463(9) Uani 1 1 d U . . B7 B -0.2230(3) 0.0771(3) 0.61704(11) 0.0287(6) Uani 1 1 d . . . H7 H -0.3223 0.0988 0.6144 0.034 Uiso 1 1 d R . . C19 C -0.0063(3) 0.3975(3) 0.69766(12) 0.0432(8) Uani 1 1 d U . . H19A H -0.0396 0.3424 0.7199 0.052 Uiso 1 1 d R . . H19B H -0.0733 0.4337 0.6803 0.052 Uiso 1 1 d R . . H19C H 0.0399 0.4509 0.7168 0.052 Uiso 1 1 d R . . B10 B -0.0313(3) -0.0635(3) 0.65631(12) 0.0330(7) Uani 1 1 d . . . H10 H -0.0046 -0.1354 0.6793 0.040 Uiso 1 1 d R . . B12 B -0.1705(3) -0.0614(3) 0.61951(12) 0.0305(7) Uani 1 1 d . . . H12 H -0.2355 -0.1317 0.6185 0.037 Uiso 1 1 d R . . C17 C 0.2291(3) 0.2338(3) 0.58866(14) 0.0496(9) Uani 1 1 d U . . C23 C 0.1026(5) 0.3247(4) 0.51750(12) 0.0827(16) Uani 1 1 d U . . H23A H 0.0296 0.3702 0.5149 0.099 Uiso 1 1 d R . . H23B H 0.0874 0.2548 0.5015 0.099 Uiso 1 1 d R . . H23C H 0.1714 0.3608 0.5013 0.099 Uiso 1 1 d R . . C20 C 0.2037(4) 0.2608(3) 0.73120(12) 0.0570(10) Uani 1 1 d U . . H20A H 0.2347 0.1878 0.7377 0.068 Uiso 1 1 d R . . H20B H 0.1279 0.2723 0.7497 0.068 Uiso 1 1 d R . . H20C H 0.2646 0.3144 0.7415 0.068 Uiso 1 1 d R . . C22 C 0.3066(4) 0.1683(4) 0.55160(18) 0.0961(19) Uani 1 1 d U . . H22A H 0.3929 0.1873 0.5557 0.115 Uiso 1 1 d R . . H22B H 0.2810 0.1846 0.5178 0.115 Uiso 1 1 d R . . H22C H 0.2954 0.0909 0.5582 0.115 Uiso 1 1 d R . . C21 C 0.3554(4) 0.1444(4) 0.6582(2) 0.0949(19) Uani 1 1 d U . . H21A H 0.3921 0.1072 0.6299 0.114 Uiso 1 1 d R . . H21B H 0.3220 0.0908 0.6811 0.114 Uiso 1 1 d R . . H21C H 0.4178 0.1877 0.6750 0.114 Uiso 1 1 d 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 Fe1 0.02133(17) 0.01718(19) 0.02191(17) -0.00411(14) 0.00185(14) -0.00268(14) B6 0.0324(16) 0.0233(16) 0.0250(14) 0.0014(12) -0.0030(12) -0.0031(13) B3 0.0261(13) 0.0200(15) 0.0255(13) -0.0028(11) -0.0025(11) -0.0011(11) C4 0.0258(12) 0.0223(13) 0.0268(12) -0.0053(10) 0.0016(11) -0.0033(11) B11 0.0389(17) 0.0257(16) 0.0306(16) 0.0008(12) 0.0079(14) -0.0100(14) C2 0.0254(12) 0.0200(13) 0.0239(12) -0.0035(9) 0.0052(10) -0.0002(10) C14 0.0301(13) 0.0190(13) 0.0307(13) -0.0052(10) -0.0035(11) -0.0060(10) B5 0.0285(15) 0.0203(14) 0.0341(15) -0.0026(12) -0.0044(13) 0.0012(11) C13 0.0405(15) 0.0182(13) 0.0357(14) 0.0045(11) -0.0106(12) -0.0087(12) B9 0.0307(15) 0.0179(15) 0.0411(17) -0.0075(13) 0.0017(13) -0.0024(12) B8 0.0280(15) 0.0242(16) 0.0293(15) -0.0065(12) -0.0016(12) -0.0044(12) C15 0.0316(14) 0.0223(14) 0.0420(15) -0.0049(12) -0.0097(12) -0.0072(12) C16 0.0237(14) 0.0287(16) 0.079(2) -0.0203(15) -0.0035(15) -0.0050(12) C18 0.065(2) 0.048(2) 0.0253(13) -0.0040(13) 0.0074(14) -0.0397(18) B7 0.0227(14) 0.0274(16) 0.0360(16) -0.0054(13) 0.0026(12) -0.0033(12) C19 0.0391(17) 0.0397(18) 0.0508(18) -0.0216(14) 0.0032(15) -0.0008(14) B10 0.0412(18) 0.0194(16) 0.0384(17) 0.0033(13) -0.0025(14) -0.0026(13) B12 0.0303(15) 0.0213(15) 0.0397(17) -0.0035(13) 0.0023(14) -0.0063(12) C17 0.0385(17) 0.0435(19) 0.067(2) -0.0285(17) 0.0259(17) -0.0236(16) C23 0.131(4) 0.089(3) 0.0278(16) 0.0057(18) 0.004(2) -0.075(3) C20 0.073(3) 0.044(2) 0.053(2) -0.0026(16) -0.0355(19) -0.0047(18) C22 0.077(3) 0.095(4) 0.117(4) -0.065(3) 0.066(3) -0.049(3) C21 0.038(2) 0.056(3) 0.191(6) -0.043(3) -0.032(3) 0.0116(19) _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 B3 2.066(3) . ? Fe1 C2 2.074(2) . ? Fe1 C4 2.074(2) . ? Fe1 B6 2.086(3) . ? Fe1 B5 2.090(3) . ? Fe1 C13 2.098(3) . ? Fe1 C17 2.103(3) . ? Fe1 C18 2.109(3) . ? Fe1 C14 2.118(3) . ? Fe1 C16 2.127(3) . ? Fe1 C15 2.144(3) . ? B6 C2 1.695(4) . ? B6 B11 1.787(4) . ? B6 B10 1.790(4) . ? B6 B5 1.799(4) . ? B6 H6 1.0999 . ? B3 C2 1.697(4) . ? B3 C4 1.698(4) . ? B3 B7 1.780(4) . ? B3 B8 1.783(4) . ? B3 H3 1.1000 . ? C4 B5 1.692(4) . ? C4 B9 1.704(4) . ? C4 B8 1.716(4) . ? C4 H4 1.0999 . ? B11 C2 1.710(4) . ? B11 B12 1.755(4) . ? B11 B7 1.762(4) . ? B11 B10 1.766(5) . ? B11 H11 1.1000 . ? C2 B7 1.710(4) . ? C2 H2 1.1000 . ? C14 C13 1.400(4) . ? C14 C15 1.410(4) . ? C14 C19 1.502(4) . ? B5 B10 1.775(4) . ? B5 B9 1.785(4) . ? B5 H5 1.1000 . ? C13 C18 1.407(4) . ? C13 H13 0.9299 . ? B9 B8 1.763(4) . ? B9 B12 1.765(4) . ? B9 B10 1.768(5) . ? B9 H9 1.1001 . ? B8 B7 1.762(4) . ? B8 B12 1.767(4) . ? B8 H8 1.0998 . ? C15 C16 1.411(4) . ? C15 C20 1.500(4) . ? C16 C17 1.392(5) . ? C16 C21 1.516(5) . ? C18 C17 1.409(5) . ? C18 C23 1.520(4) . ? B7 B12 1.770(4) . ? B7 H7 1.0999 . ? C19 H19A 0.9601 . ? C19 H19B 0.9599 . ? C19 H19C 0.9599 . ? B10 B12 1.786(4) . ? B10 H10 1.1000 . ? B12 H12 1.1001 . ? C17 C22 1.513(4) . ? C23 H23A 0.9601 . ? C23 H23B 0.9602 . ? C23 H23C 0.9601 . ? C20 H20A 0.9601 . ? C20 H20B 0.9598 . ? C20 H20C 0.9600 . ? C22 H22A 0.9599 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 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 B3 Fe1 C2 48.41(10) . . ? B3 Fe1 C4 48.44(11) . . ? C2 Fe1 C4 80.24(10) . . ? B3 Fe1 B6 85.82(12) . . ? C2 Fe1 B6 48.10(11) . . ? C4 Fe1 B6 83.54(11) . . ? B3 Fe1 B5 85.62(12) . . ? C2 Fe1 B5 83.40(11) . . ? C4 Fe1 B5 47.93(11) . . ? B6 Fe1 B5 51.04(12) . . ? B3 Fe1 C13 94.89(11) . . ? C2 Fe1 C13 105.52(11) . . ? C4 Fe1 C13 125.46(10) . . ? B6 Fe1 C13 140.44(12) . . ? B5 Fe1 C13 168.52(12) . . ? B3 Fe1 C17 125.53(13) . . ? C2 Fe1 C17 173.21(14) . . ? C4 Fe1 C17 97.35(11) . . ? B6 Fe1 C17 138.22(15) . . ? B5 Fe1 C17 99.75(13) . . ? C13 Fe1 C17 70.63(13) . . ? B3 Fe1 C18 98.05(12) . . ? C2 Fe1 C18 134.78(13) . . ? C4 Fe1 C18 99.37(11) . . ? B6 Fe1 C18 176.10(12) . . ? B5 Fe1 C18 129.49(13) . . ? C13 Fe1 C18 39.07(12) . . ? C17 Fe1 C18 39.08(14) . . ? B3 Fe1 C14 117.32(11) . . ? C2 Fe1 C14 96.47(10) . . ? C4 Fe1 C14 162.63(10) . . ? B6 Fe1 C14 107.08(11) . . ? B5 Fe1 C14 149.08(11) . . ? C13 Fe1 C14 38.79(10) . . ? C17 Fe1 C14 83.93(11) . . ? C18 Fe1 C14 70.75(11) . . ? B3 Fe1 C16 163.57(13) . . ? C2 Fe1 C16 147.84(12) . . ? C4 Fe1 C16 120.79(11) . . ? B6 Fe1 C16 106.44(13) . . ? B5 Fe1 C16 93.60(12) . . ? C13 Fe1 C16 82.67(12) . . ? C17 Fe1 C16 38.44(14) . . ? C18 Fe1 C16 69.86(14) . . ? C14 Fe1 C16 70.21(11) . . ? B3 Fe1 C15 154.22(11) . . ? C2 Fe1 C15 114.37(10) . . ? C4 Fe1 C15 157.10(11) . . ? B6 Fe1 C15 93.41(11) . . ? B5 Fe1 C15 113.75(11) . . ? C13 Fe1 C15 69.59(11) . . ? C17 Fe1 C15 69.99(12) . . ? C18 Fe1 C15 82.89(11) . . ? C14 Fe1 C15 38.64(10) . . ? C16 Fe1 C15 38.57(11) . . ? C2 B6 B11 58.72(17) . . ? C2 B6 B10 104.5(2) . . ? B11 B6 B10 59.18(17) . . ? C2 B6 B5 104.84(19) . . ? B11 B6 B5 106.5(2) . . ? B10 B6 B5 59.27(17) . . ? C2 B6 Fe1 65.57(13) . . ? B11 B6 Fe1 118.65(18) . . ? B10 B6 Fe1 117.58(18) . . ? B5 B6 Fe1 64.61(14) . . ? C2 B6 H6 124.5 . . ? B11 B6 H6 120.1 . . ? B10 B6 H6 121.4 . . ? B5 B6 H6 124.1 . . ? Fe1 B6 H6 111.2 . . ? C2 B3 C4 103.8(2) . . ? C2 B3 B7 58.84(15) . . ? C4 B3 B7 105.2(2) . . ? C2 B3 B8 105.2(2) . . ? C4 B3 B8 59.01(16) . . ? B7 B3 B8 59.28(16) . . ? C2 B3 Fe1 66.04(13) . . ? C4 B3 Fe1 66.05(13) . . ? B7 B3 Fe1 119.94(18) . . ? B8 B3 Fe1 120.09(18) . . ? C2 B3 H3 125.1 . . ? C4 B3 H3 124.6 . . ? B7 B3 H3 120.7 . . ? B8 B3 H3 120.3 . . ? Fe1 B3 H3 109.1 . . ? B5 C4 B3 112.8(2) . . ? B5 C4 B9 63.43(17) . . ? B3 C4 B9 113.6(2) . . ? B5 C4 B8 114.5(2) . . ? B3 C4 B8 62.95(16) . . ? B9 C4 B8 62.06(17) . . ? B5 C4 Fe1 66.53(13) . . ? B3 C4 Fe1 65.52(12) . . ? B9 C4 Fe1 123.87(17) . . ? B8 C4 Fe1 123.12(17) . . ? B5 C4 H4 118.6 . . ? B3 C4 H4 119.7 . . ? B9 C4 H4 116.0 . . ? B8 C4 H4 116.1 . . ? Fe1 C4 H4 109.1 . . ? C2 B11 B12 105.9(2) . . ? C2 B11 B7 58.99(16) . . ? B12 B11 B7 60.41(17) . . ? C2 B11 B10 104.9(2) . . ? B12 B11 B10 60.95(18) . . ? B7 B11 B10 108.6(2) . . ? C2 B11 B6 57.95(16) . . ? B12 B11 B6 109.4(2) . . ? B7 B11 B6 107.8(2) . . ? B10 B11 B6 60.48(18) . . ? C2 B11 H11 124.5 . . ? B12 B11 H11 121.2 . . ? B7 B11 H11 121.2 . . ? B10 B11 H11 122.1 . . ? B6 B11 H11 121.5 . . ? B6 C2 B3 112.85(19) . . ? B6 C2 B11 63.32(18) . . ? B3 C2 B11 113.3(2) . . ? B6 C2 B7 114.7(2) . . ? B3 C2 B7 63.00(16) . . ? B11 C2 B7 62.05(17) . . ? B6 C2 Fe1 66.33(13) . . ? B3 C2 Fe1 65.55(12) . . ? B11 C2 Fe1 123.36(18) . . ? B7 C2 Fe1 123.21(16) . . ? B6 C2 H2 118.5 . . ? B3 C2 H2 119.7 . . ? B11 C2 H2 116.5 . . ? B7 C2 H2 116.0 . . ? Fe1 C2 H2 109.1 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 C19 119.4(3) . . ? C15 C14 C19 121.6(3) . . ? C13 C14 Fe1 69.84(15) . . ? C15 C14 Fe1 71.67(15) . . ? C19 C14 Fe1 129.78(19) . . ? C4 B5 B10 104.8(2) . . ? C4 B5 B9 58.62(16) . . ? B10 B5 B9 59.57(17) . . ? C4 B5 B6 105.1(2) . . ? B10 B5 B6 60.10(17) . . ? B9 B5 B6 107.5(2) . . ? C4 B5 Fe1 65.54(13) . . ? B10 B5 Fe1 118.08(19) . . ? B9 B5 Fe1 118.74(18) . . ? B6 B5 Fe1 64.36(13) . . ? C4 B5 H5 124.7 . . ? B10 B5 H5 121.0 . . ? B9 B5 H5 120.0 . . ? B6 B5 H5 123.4 . . ? Fe1 B5 H5 111.0 . . ? C14 C13 C18 121.4(3) . . ? C14 C13 Fe1 71.37(15) . . ? C18 C13 Fe1 70.89(17) . . ? C14 C13 H13 119.3 . . ? C18 C13 H13 119.3 . . ? Fe1 C13 H13 131.5 . . ? C4 B9 B8 59.31(17) . . ? C4 B9 B12 105.7(2) . . ? B8 B9 B12 60.11(17) . . ? C4 B9 B10 104.6(2) . . ? B8 B9 B10 108.3(2) . . ? B12 B9 B10 60.71(18) . . ? C4 B9 B5 57.96(16) . . ? B8 B9 B5 107.8(2) . . ? B12 B9 B5 108.6(2) . . ? B10 B9 B5 59.92(17) . . ? C4 B9 H9 124.6 . . ? B8 B9 H9 121.6 . . ? B12 B9 H9 121.8 . . ? B10 B9 H9 122.1 . . ? B5 B9 H9 121.5 . . ? C4 B8 B7 105.3(2) . . ? C4 B8 B9 58.63(16) . . ? B7 B8 B9 108.1(2) . . ? C4 B8 B12 105.1(2) . . ? B7 B8 B12 60.19(17) . . ? B9 B8 B12 60.01(18) . . ? C4 B8 B3 58.04(15) . . ? B7 B8 B3 60.30(16) . . ? B9 B8 B3 106.8(2) . . ? B12 B8 B3 107.7(2) . . ? C4 B8 H8 124.7 . . ? B7 B8 H8 121.7 . . ? B9 B8 H8 122.0 . . ? B12 B8 H8 122.2 . . ? B3 B8 H8 122.1 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 C20 119.3(3) . . ? C16 C15 C20 120.9(3) . . ? C14 C15 Fe1 69.69(14) . . ? C16 C15 Fe1 70.05(16) . . ? C20 C15 Fe1 134.0(2) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 C21 121.1(3) . . ? C15 C16 C21 118.2(4) . . ? C17 C16 Fe1 69.87(17) . . ? C15 C16 Fe1 71.38(16) . . ? C21 C16 Fe1 131.8(2) . . ? C13 C18 C17 119.2(3) . . ? C13 C18 C23 117.8(4) . . ? C17 C18 C23 123.0(4) . . ? C13 C18 Fe1 70.04(15) . . ? C17 C18 Fe1 70.22(18) . . ? C23 C18 Fe1 129.8(2) . . ? C2 B7 B8 105.6(2) . . ? C2 B7 B11 58.97(16) . . ? B8 B7 B11 107.7(2) . . ? C2 B7 B12 105.3(2) . . ? B8 B7 B12 60.05(17) . . ? B11 B7 B12 59.58(18) . . ? C2 B7 B3 58.15(15) . . ? B8 B7 B3 60.43(16) . . ? B11 B7 B3 106.9(2) . . ? B12 B7 B3 107.7(2) . . ? C2 B7 H7 124.2 . . ? B8 B7 H7 121.9 . . ? B11 B7 H7 122.1 . . ? B12 B7 H7 122.4 . . ? B3 B7 H7 122.0 . . ? C14 C19 H19A 109.0 . . ? C14 C19 H19B 110.0 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.4 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? B11 B10 B9 107.2(2) . . ? B11 B10 B5 108.5(2) . . ? B9 B10 B5 60.50(17) . . ? B11 B10 B12 59.20(18) . . ? B9 B10 B12 59.56(17) . . ? B5 B10 B12 108.2(2) . . ? B11 B10 B6 60.35(18) . . ? B9 B10 B6 108.7(2) . . ? B5 B10 B6 60.63(17) . . ? B12 B10 B6 107.9(2) . . ? B11 B10 H10 122.3 . . ? B9 B10 H10 121.6 . . ? B5 B10 H10 120.9 . . ? B12 B10 H10 122.2 . . ? B6 B10 H10 121.3 . . ? B11 B12 B9 107.9(2) . . ? B11 B12 B8 107.8(2) . . ? B9 B12 B8 59.88(17) . . ? B11 B12 B7 60.01(17) . . ? B9 B12 B7 107.7(2) . . ? B8 B12 B7 59.77(17) . . ? B11 B12 B10 59.84(18) . . ? B9 B12 B10 59.73(18) . . ? B8 B12 B10 107.3(2) . . ? B7 B12 B10 107.5(2) . . ? B11 B12 H12 121.8 . . ? B9 B12 H12 121.8 . . ? B8 B12 H12 121.9 . . ? B7 B12 H12 122.0 . . ? B10 B12 H12 122.2 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 C22 118.3(4) . . ? C18 C17 C22 121.7(4) . . ? C16 C17 Fe1 71.69(17) . . ? C18 C17 Fe1 70.70(17) . . ? C22 C17 Fe1 128.4(2) . . ? C18 C23 H23A 109.6 . . ? C18 C23 H23B 109.3 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.4 . . ? C15 C20 H20A 109.7 . . ? C15 C20 H20B 109.2 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C22 H22A 109.3 . . ? C17 C22 H22B 110.2 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 108.9 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C21 H21A 109.3 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.6 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.362 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.068 # Attachment 'jhl100217Fe1akt.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 810293' #TrackingRef 'jhl100217Fe1akt.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H23 B9 Fe' _chemical_formula_sum 'C11 H23 B9 Fe' _chemical_formula_weight 308.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 12.6261(6) _cell_length_b 9.6201(5) _cell_length_c 12.6258(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1533.58(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 13537 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.963 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.096 0 0 -1 0.075 0 1 0 0.084 0 -1 0 0.221 -1 0 0 0.154 1 0 0 0.063 -1 1 0 0.097 1 -1 0 0.127 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 150(1) _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 Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13504 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3289 _reflns_number_gt 3053 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _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^)+(0.0227P)^2^+0.7830P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(16) _refine_ls_number_reflns 3289 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 Fe1 Fe 0.689324(19) 0.05700(2) 0.34677(3) 0.01407(7) Uani 1 1 d . . . C2 C 0.56607(17) -0.0549(2) 0.27935(17) 0.0199(4) Uani 1 1 d . . . H2 H 0.5649 -0.0357 0.1934 0.024 Uiso 1 1 d R . . 5 B 0.5948(2) 0.0463(3) 0.4835(2) 0.0199(5) Uani 1 1 d . . . H5 H 0.6145 0.1301 0.5394 0.024 Uiso 1 1 d R . . C4 C 0.67090(18) -0.0964(2) 0.46119(19) 0.0205(4) Uani 1 1 d . . . H4 H 0.7454 -0.1063 0.5057 0.025 Uiso 1 1 d R . . B6 B 0.52431(18) 0.0729(2) 0.3608(3) 0.0194(6) Uani 1 1 d . . . H6 H 0.4964 0.1753 0.3341 0.023 Uiso 1 1 d R . . B11 B 0.44495(18) -0.0775(2) 0.3378(3) 0.0252(5) Uani 1 1 d . . . H11 H 0.3686 -0.0717 0.2960 0.030 Uiso 1 1 d R . . B7 B 0.5326(2) -0.2189(3) 0.3193(2) 0.0250(6) Uani 1 1 d . . . H7 H 0.5140 -0.3044 0.2645 0.030 Uiso 1 1 d R . . B8 B 0.6013(2) -0.2463(3) 0.4389(2) 0.0268(6) Uani 1 1 d . . . H8 H 0.6279 -0.3505 0.4628 0.032 Uiso 1 1 d R . . B10 B 0.4617(2) -0.0152(3) 0.4687(2) 0.0228(5) Uani 1 1 d . . . H10 H 0.3964 0.0336 0.5127 0.027 Uiso 1 1 d R . . B3 B 0.66359(19) -0.1544(2) 0.3340(2) 0.0211(5) Uani 1 1 d . . . H3 H 0.7300 -0.2020 0.2908 0.025 Uiso 1 1 d R . . B9 B 0.5570(2) -0.1223(3) 0.5319(2) 0.0236(5) Uani 1 1 d . . . H9 H 0.5537 -0.1461 0.6170 0.028 Uiso 1 1 d R . . B12 B 0.4659(2) -0.1969(3) 0.4423(2) 0.0258(6) Uani 1 1 d . . . H12 H 0.4032 -0.2679 0.4693 0.031 Uiso 1 1 d R . . C13 C 0.85456(16) 0.0514(2) 0.3293(2) 0.0204(6) Uani 1 1 d . . . H13 H 0.9041 -0.0179 0.3428 0.025 Uiso 1 1 d R . . C18 C 0.80893(17) 0.0596(2) 0.22785(18) 0.0210(5) Uani 1 1 d . . . C19 C 0.8759(2) 0.1312(3) 0.5187(2) 0.0306(5) Uani 1 1 d . . . H19A H 0.8919 0.0353 0.5324 0.037 Uiso 1 1 d R . . H19B H 0.8257 0.1640 0.5701 0.037 Uiso 1 1 d R . . H19C H 0.9395 0.1854 0.5232 0.037 Uiso 1 1 d R . . C16 C 0.70697(19) 0.2639(2) 0.28731(19) 0.0223(5) Uani 1 1 d . . . C17 C 0.73370(17) 0.1665(2) 0.20883(19) 0.0217(4) Uani 1 1 d . . . H17 H 0.7016 0.1729 0.1427 0.026 Uiso 1 1 d R . . C21 C 0.8352(2) -0.0441(3) 0.1430(2) 0.0288(5) Uani 1 1 d . . . H21A H 0.8895 -0.0069 0.0979 0.035 Uiso 1 1 d R . . H21B H 0.7731 -0.0637 0.1017 0.035 Uiso 1 1 d R . . H21C H 0.8601 -0.1282 0.1755 0.035 Uiso 1 1 d R . . C15 C 0.75356(18) 0.2510(2) 0.3875(2) 0.0217(4) Uani 1 1 d . . . H15 H 0.7349 0.3130 0.4408 0.026 Uiso 1 1 d R . . C20 C 0.6294(2) 0.3789(3) 0.2650(2) 0.0329(6) Uani 1 1 d . . . H20A H 0.5910 0.4019 0.3282 0.040 Uiso 1 1 d R . . H20B H 0.5807 0.3495 0.2111 0.040 Uiso 1 1 d R . . H20C H 0.6677 0.4591 0.2408 0.040 Uiso 1 1 d R . . C14 C 0.82864(16) 0.1453(2) 0.41003(18) 0.0211(5) 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 Fe1 0.01262(11) 0.01368(12) 0.01592(12) 0.00162(16) 0.00052(16) -0.00013(9) C2 0.0185(10) 0.0224(11) 0.0189(10) 0.0009(9) 0.0015(8) -0.0059(9) 5 0.0223(12) 0.0205(12) 0.0169(11) 0.0000(9) 0.0027(10) -0.0016(10) C4 0.0208(11) 0.0175(10) 0.0231(11) 0.0055(9) 0.0015(9) 0.0012(8) B6 0.0138(9) 0.0209(10) 0.0235(17) -0.0010(11) 0.0002(10) 0.0011(8) B11 0.0187(9) 0.0306(12) 0.0263(14) -0.0005(14) 0.0008(14) -0.0084(8) B7 0.0283(13) 0.0225(12) 0.0243(15) -0.0026(9) 0.0068(10) -0.0101(10) B8 0.0324(14) 0.0160(11) 0.0320(15) 0.0060(11) 0.0093(12) -0.0017(10) B10 0.0200(12) 0.0242(13) 0.0241(13) -0.0002(10) 0.0064(10) -0.0004(10) B3 0.0258(11) 0.0132(9) 0.0242(15) -0.0020(11) 0.0051(12) -0.0005(8) B9 0.0254(13) 0.0230(13) 0.0224(12) 0.0054(10) 0.0054(10) -0.0011(11) B12 0.0261(13) 0.0241(13) 0.0273(14) -0.0011(11) 0.0058(11) -0.0070(11) C13 0.0127(8) 0.0207(9) 0.0280(17) 0.0034(9) 0.0025(9) -0.0006(7) C18 0.0158(10) 0.0247(11) 0.0225(11) 0.0045(9) 0.0045(9) -0.0010(9) C19 0.0321(13) 0.0295(13) 0.0302(12) 0.0013(11) -0.0108(11) -0.0067(11) C16 0.0182(11) 0.0160(11) 0.0327(13) 0.0071(9) -0.0003(10) -0.0041(9) C17 0.0183(10) 0.0250(11) 0.0218(10) 0.0072(9) 0.0020(9) -0.0035(9) C21 0.0254(12) 0.0381(14) 0.0230(12) 0.0003(10) 0.0073(9) 0.0028(10) C15 0.0200(11) 0.0156(10) 0.0294(10) -0.0030(9) 0.0021(9) -0.0052(9) C20 0.0308(14) 0.0224(12) 0.0456(15) 0.0103(11) -0.0013(12) 0.0028(10) C14 0.0174(10) 0.0210(11) 0.0248(12) 0.0014(9) -0.0031(9) -0.0059(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 Fe1 B3 2.066(2) . ? Fe1 C2 2.075(2) . ? Fe1 C4 2.078(2) . ? Fe1 B6 2.097(2) . ? Fe1 C13 2.099(2) . ? Fe1 C15 2.099(2) . ? Fe1 5 2.102(2) . ? Fe1 C14 2.110(2) . ? Fe1 C17 2.111(2) . ? Fe1 C18 2.130(2) . ? Fe1 C16 2.139(2) . ? C2 B6 1.688(3) . ? C2 B7 1.709(3) . ? C2 B3 1.705(3) . ? C2 B11 1.712(3) . ? C2 H2 1.1003 . ? 5 C4 1.700(3) . ? 5 B10 1.792(4) . ? 5 B9 1.797(4) . ? 5 B6 1.804(4) . ? 5 H5 1.1000 . ? C4 B3 1.703(4) . ? C4 B9 1.711(3) . ? C4 B8 1.712(4) . ? C4 H4 1.0998 . ? B6 B11 1.784(3) . ? B6 B10 1.788(4) . ? B6 H6 1.0992 . ? B11 B10 1.770(5) . ? B11 B7 1.769(4) . ? B11 B12 1.769(4) . ? B11 H11 1.0999 . ? B7 B8 1.761(4) . ? B7 B3 1.776(3) . ? B7 B12 1.779(4) . ? B7 H7 1.1002 . ? B8 B3 1.776(4) . ? B8 B9 1.765(4) . ? B8 B12 1.774(4) . ? B8 H8 1.0994 . ? B10 B9 1.774(4) . ? B10 B12 1.780(4) . ? B10 H10 1.1000 . ? B3 H3 1.1000 . ? B9 B12 1.765(4) . ? B9 H9 1.1001 . ? B12 H12 1.1000 . ? C13 C18 1.406(3) . ? C13 C14 1.401(3) . ? C13 H13 0.9295 . ? C18 C17 1.420(3) . ? C18 C21 1.501(3) . ? C19 C14 1.503(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9605 . ? C19 H19C 0.9591 . ? C16 C15 1.401(3) . ? C16 C17 1.405(3) . ? C16 C20 1.505(3) . ? C17 H17 0.9298 . ? C21 H21A 0.9604 . ? C21 H21B 0.9603 . ? C21 H21C 0.9602 . ? C15 C14 1.419(3) . ? C15 H15 0.9297 . ? C20 H20A 0.9596 . ? C20 H20B 0.9598 . ? C20 H20C 0.9604 . ? 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 B3 Fe1 C2 48.64(9) . . ? B3 Fe1 C4 48.52(11) . . ? C2 Fe1 C4 80.38(9) . . ? B3 Fe1 B6 85.54(9) . . ? C2 Fe1 B6 47.73(9) . . ? C4 Fe1 B6 83.21(10) . . ? B3 Fe1 C13 97.06(9) . . ? C2 Fe1 C13 133.56(9) . . ? C4 Fe1 C13 99.57(9) . . ? B6 Fe1 C13 177.03(10) . . ? B3 Fe1 C15 162.79(10) . . ? C2 Fe1 C15 148.40(9) . . ? C4 Fe1 C15 120.27(10) . . ? B6 Fe1 C15 107.35(9) . . ? C13 Fe1 C15 70.39(9) . . ? B3 Fe1 5 85.80(11) . . ? C2 Fe1 5 83.43(9) . . ? C4 Fe1 5 47.98(9) . . ? B6 Fe1 5 50.91(11) . . ? C13 Fe1 5 130.54(10) . . ? C15 Fe1 5 93.53(10) . . ? B3 Fe1 C14 123.84(9) . . ? C2 Fe1 C14 171.59(9) . . ? C4 Fe1 C14 96.66(9) . . ? B6 Fe1 C14 140.07(10) . . ? C13 Fe1 C14 38.88(9) . . ? C15 Fe1 C14 39.40(9) . . ? 5 Fe1 C14 100.50(9) . . ? B3 Fe1 C17 117.93(11) . . ? C2 Fe1 C17 96.85(9) . . ? C4 Fe1 C17 163.23(9) . . ? B6 Fe1 C17 107.29(11) . . ? C13 Fe1 C17 70.25(9) . . ? C15 Fe1 C17 69.89(9) . . ? 5 Fe1 C17 148.54(9) . . ? C14 Fe1 C17 83.70(9) . . ? B3 Fe1 C18 93.89(10) . . ? C2 Fe1 C18 104.40(9) . . ? C4 Fe1 C18 125.29(9) . . ? B6 Fe1 C18 139.78(11) . . ? C13 Fe1 C18 38.84(9) . . ? C15 Fe1 C18 83.60(9) . . ? 5 Fe1 C18 169.29(9) . . ? C14 Fe1 C18 70.80(9) . . ? C17 Fe1 C18 39.13(8) . . ? B3 Fe1 C16 154.83(10) . . ? C2 Fe1 C16 114.64(9) . . ? C4 Fe1 C16 156.42(9) . . ? B6 Fe1 C16 93.74(9) . . ? C13 Fe1 C16 83.29(9) . . ? C15 Fe1 C16 38.60(9) . . ? 5 Fe1 C16 113.15(10) . . ? C14 Fe1 C16 70.82(9) . . ? C17 Fe1 C16 38.60(9) . . ? C18 Fe1 C16 70.60(9) . . ? B6 C2 B7 114.52(18) . . ? B6 C2 B3 112.83(18) . . ? B7 C2 B3 62.68(15) . . ? B6 C2 B11 63.29(14) . . ? B7 C2 B11 62.27(14) . . ? B3 C2 B11 113.53(19) . . ? B6 C2 Fe1 66.81(11) . . ? B7 C2 Fe1 122.90(15) . . ? B3 C2 Fe1 65.41(11) . . ? B11 C2 Fe1 123.98(17) . . ? B6 C2 H2 118.3 . . ? B7 C2 H2 116.3 . . ? B3 C2 H2 120.2 . . ? B11 C2 H2 115.7 . . ? Fe1 C2 H2 109.1 . . ? C4 5 B10 104.25(17) . . ? C4 5 B9 58.50(14) . . ? B10 5 B9 59.23(14) . . ? C4 5 B6 104.54(17) . . ? B10 5 B6 59.64(14) . . ? B9 5 B6 106.79(17) . . ? C4 5 Fe1 65.29(11) . . ? B10 5 Fe1 117.58(15) . . ? B9 5 Fe1 118.29(15) . . ? B6 5 Fe1 64.40(11) . . ? C4 5 H5 124.8 . . ? B10 5 H5 121.4 . . ? B9 5 H5 120.2 . . ? B6 5 H5 123.9 . . ? Fe1 5 H5 111.3 . . ? B3 C4 5 112.98(17) . . ? B3 C4 B9 113.49(18) . . ? 5 C4 B9 63.61(14) . . ? B3 C4 B8 62.68(15) . . ? 5 C4 B8 114.66(18) . . ? B9 C4 B8 62.07(15) . . ? B3 C4 Fe1 65.36(11) . . ? 5 C4 Fe1 66.73(11) . . ? B9 C4 Fe1 124.05(15) . . ? B8 C4 Fe1 122.76(16) . . ? B3 C4 H4 120.0 . . ? 5 C4 H4 118.0 . . ? B9 C4 H4 116.1 . . ? B8 C4 H4 116.8 . . ? Fe1 C4 H4 108.7 . . ? C2 B6 B11 59.02(14) . . ? C2 B6 B10 104.87(17) . . ? B11 B6 B10 59.40(17) . . ? C2 B6 5 105.42(17) . . ? B11 B6 5 107.6(2) . . ? B10 B6 5 59.82(15) . . ? C2 B6 Fe1 65.46(11) . . ? B11 B6 Fe1 119.02(14) . . ? B10 B6 Fe1 118.00(17) . . ? 5 B6 Fe1 64.69(11) . . ? C2 B6 H6 124.5 . . ? B11 B6 H6 119.8 . . ? B10 B6 H6 121.1 . . ? 5 B6 H6 123.3 . . ? Fe1 B6 H6 111.0 . . ? C2 B11 B10 104.66(18) . . ? C2 B11 B7 58.80(14) . . ? B10 B11 B7 108.0(2) . . ? C2 B11 B12 105.67(18) . . ? B10 B11 B12 60.38(17) . . ? B7 B11 B12 60.35(15) . . ? C2 B11 B6 57.70(13) . . ? B10 B11 B6 60.43(16) . . ? B7 B11 B6 107.09(16) . . ? B12 B11 B6 108.7(2) . . ? C2 B11 H11 124.7 . . ? B10 B11 H11 122.4 . . ? B7 B11 H11 121.6 . . ? B12 B11 H11 121.5 . . ? B6 B11 H11 121.9 . . ? C2 B7 B8 105.64(18) . . ? C2 B7 B11 58.94(14) . . ? B8 B7 B11 108.1(2) . . ? C2 B7 B3 58.55(13) . . ? B8 B7 B3 60.28(16) . . ? B11 B7 B3 107.47(17) . . ? C2 B7 B12 105.37(18) . . ? B8 B7 B12 60.16(15) . . ? B11 B7 B12 59.83(18) . . ? B3 B7 B12 107.94(19) . . ? C2 B7 H7 123.9 . . ? B8 B7 H7 122.2 . . ? B11 B7 H7 121.6 . . ? B3 B7 H7 121.7 . . ? B12 B7 H7 122.5 . . ? C4 B8 B7 105.53(17) . . ? C4 B8 B3 58.41(14) . . ? B7 B8 B3 60.28(14) . . ? C4 B8 B9 58.93(14) . . ? B7 B8 B9 108.2(2) . . ? B3 B8 B9 107.46(18) . . ? C4 B8 B12 105.36(18) . . ? B7 B8 B12 60.41(16) . . ? B3 B8 B12 108.14(18) . . ? B9 B8 B12 59.83(15) . . ? C4 B8 H8 124.5 . . ? B7 B8 H8 121.5 . . ? B3 B8 H8 121.5 . . ? B9 B8 H8 122.0 . . ? B12 B8 H8 122.1 . . ? B11 B10 B9 107.73(18) . . ? B11 B10 B12 59.80(15) . . ? B9 B10 B12 59.57(15) . . ? B11 B10 B6 60.17(14) . . ? B9 B10 B6 108.53(18) . . ? B12 B10 B6 108.05(17) . . ? B11 B10 5 108.75(17) . . ? B9 B10 5 60.55(15) . . ? B12 B10 5 108.40(18) . . ? B6 B10 5 60.53(14) . . ? B11 B10 H10 121.8 . . ? B9 B10 H10 121.9 . . ? B12 B10 H10 122.5 . . ? B6 B10 H10 120.9 . . ? 5 B10 H10 120.6 . . ? C4 B3 C2 103.69(17) . . ? C4 B3 B8 58.91(15) . . ? C2 B3 B8 105.15(18) . . ? C4 B3 B7 105.26(18) . . ? C2 B3 B7 58.77(14) . . ? B8 B3 B7 59.44(15) . . ? C4 B3 Fe1 66.12(11) . . ? C2 B3 Fe1 65.95(11) . . ? B8 B3 Fe1 120.08(17) . . ? B7 B3 Fe1 119.88(15) . . ? C4 B3 H3 124.2 . . ? C2 B3 H3 125.7 . . ? B8 B3 H3 120.0 . . ? B7 B3 H3 120.8 . . ? Fe1 B3 H3 109.2 . . ? C4 B9 B12 105.81(18) . . ? C4 B9 B8 59.00(15) . . ? B12 B9 B8 60.35(16) . . ? C4 B9 B10 104.56(17) . . ? B12 B9 B10 60.39(15) . . ? B8 B9 B10 107.95(19) . . ? C4 B9 5 57.90(13) . . ? B12 B9 5 108.79(18) . . ? B8 B9 5 107.46(18) . . ? B10 B9 5 60.22(14) . . ? C4 B9 H9 124.8 . . ? B12 B9 H9 121.2 . . ? B8 B9 H9 121.4 . . ? B10 B9 H9 122.4 . . ? 5 B9 H9 122.0 . . ? B9 B12 B11 108.14(18) . . ? B9 B12 B7 107.44(19) . . ? B11 B12 B7 59.82(15) . . ? B9 B12 B8 59.82(15) . . ? B11 B12 B8 107.47(18) . . ? B7 B12 B8 59.43(16) . . ? B9 B12 B10 60.05(15) . . ? B11 B12 B10 59.82(15) . . ? B7 B12 B10 107.12(18) . . ? B8 B12 B10 107.27(18) . . ? B9 B12 H12 121.5 . . ? B11 B12 H12 121.8 . . ? B7 B12 H12 122.5 . . ? B8 B12 H12 122.3 . . ? B10 B12 H12 122.0 . . ? C18 C13 C14 122.1(2) . . ? C18 C13 Fe1 71.77(12) . . ? C14 C13 Fe1 71.01(12) . . ? C18 C13 H13 118.8 . . ? C14 C13 H13 119.1 . . ? Fe1 C13 H13 131.9 . . ? C13 C18 C17 117.9(2) . . ? C13 C18 C21 121.5(2) . . ? C17 C18 C21 120.5(2) . . ? C13 C18 Fe1 69.38(12) . . ? C17 C18 Fe1 69.72(13) . . ? C21 C18 Fe1 130.71(16) . . ? C14 C19 H19A 109.6 . . ? C14 C19 H19B 109.0 . . ? H19A C19 H19B 109.4 . . ? C14 C19 H19C 109.7 . . ? H19A C19 H19C 109.6 . . ? H19B C19 H19C 109.5 . . ? C15 C16 C17 118.5(2) . . ? C15 C16 C20 120.5(2) . . ? C17 C16 C20 121.0(2) . . ? C15 C16 Fe1 69.15(14) . . ? C17 C16 Fe1 69.62(13) . . ? C20 C16 Fe1 133.02(17) . . ? C16 C17 C18 121.6(2) . . ? C16 C17 Fe1 71.77(13) . . ? C18 C17 Fe1 71.14(13) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.4 . . ? Fe1 C17 H17 131.1 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.7 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.1 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C15 C14 121.7(2) . . ? C16 C15 Fe1 72.25(14) . . ? C14 C15 Fe1 70.73(13) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.0 . . ? Fe1 C15 H15 130.5 . . ? C16 C20 H20A 110.0 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 108.8 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C14 C15 118.2(2) . . ? C13 C14 C19 120.9(2) . . ? C15 C14 C19 120.9(2) . . ? C13 C14 Fe1 70.11(12) . . ? C15 C14 Fe1 69.87(13) . . ? C19 C14 Fe1 129.82(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.214 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.048