# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm019 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H58 B2 Fe2 N4' _chemical_formula_weight 752.24 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' 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2575(5) _cell_length_b 12.7550(3) _cell_length_c 15.5389(5) _cell_angle_alpha 103.893(2) _cell_angle_beta 109.461(3) _cell_angle_gamma 97.674(3) _cell_volume 1985.85(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10532 _cell_measurement_theta_min 2.8883 _cell_measurement_theta_max 28.7895 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_T_min 0.8559 _exptl_absorpt_correction_T_max 0.9005 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16417 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6985 _reflns_number_gt 6213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0285P)^2^+1.2843P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6985 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.90837(3) 0.36289(2) 0.80976(2) 0.03170(9) Uani 1 1 d . . . Fe2 Fe 0.72608(3) 0.90337(2) 0.38387(2) 0.03093(9) Uani 1 1 d . . . B1 B 0.4787(2) 0.59054(19) 0.58337(16) 0.0317(5) Uani 1 1 d . . . B2 B 0.6391(2) 1.0844(2) 0.02824(17) 0.0352(5) Uani 1 1 d . . . N1 N 0.55187(17) 0.40944(13) 0.52392(11) 0.0304(4) Uani 1 1 d . . . N2 N 0.55973(17) 0.49859(14) 0.59583(11) 0.0310(4) Uani 1 1 d . . . N3 N 0.58529(16) 1.03963(14) 0.09774(12) 0.0333(4) Uani 1 1 d . . . N4 N 0.47342(16) 0.96670(15) 0.07454(12) 0.0329(4) Uani 1 1 d . . . C1 C 0.6165(2) 0.47837(18) 0.67913(14) 0.0340(5) Uani 1 1 d . . . H1 H 0.6329 0.5273 0.7407 0.041 Uiso 1 1 calc R . . C2 C 0.64780(19) 0.37581(17) 0.66235(14) 0.0306(4) Uani 1 1 d . . . C3 C 0.6049(2) 0.33566(17) 0.56341(14) 0.0323(5) Uani 1 1 d . . . H3 H 0.6121 0.2661 0.5286 0.039 Uiso 1 1 calc R . . C4 C 0.5641(2) 0.71054(17) 0.65533(14) 0.0336(5) Uani 1 1 d . . . H4A H 0.5123 0.7660 0.6427 0.040 Uiso 1 1 calc R . . H4B H 0.5790 0.7095 0.7216 0.040 Uiso 1 1 calc R . . C5 C 0.6948(2) 0.75033(19) 0.65091(16) 0.0400(5) Uani 1 1 d . . . H5A H 0.6822 0.7435 0.5835 0.048 Uiso 1 1 calc R . . H5B H 0.7516 0.7009 0.6720 0.048 Uiso 1 1 calc R . . C6 C 0.7636(2) 0.87021(19) 0.71230(17) 0.0448(6) Uani 1 1 d . . . H6A H 0.7089 0.9203 0.6895 0.054 Uiso 1 1 calc R . . H6B H 0.7736 0.8782 0.7795 0.054 Uiso 1 1 calc R . . C7 C 0.8957(3) 0.9057(2) 0.7094(2) 0.0608(7) Uani 1 1 d . . . H7A H 0.9510 0.8576 0.7333 0.091 Uiso 1 1 calc R . . H7B H 0.9352 0.9829 0.7498 0.091 Uiso 1 1 calc R . . H7C H 0.8863 0.8998 0.6433 0.091 Uiso 1 1 calc R . . C8 C 0.3448(2) 0.54873(17) 0.59661(15) 0.0347(5) Uani 1 1 d . . . H8A H 0.2974 0.4771 0.5463 0.042 Uiso 1 1 calc R . . H8B H 0.3676 0.5341 0.6592 0.042 Uiso 1 1 calc R . . C9 C 0.2528(2) 0.62640(19) 0.59245(17) 0.0396(5) Uani 1 1 d . . . H9A H 0.3020 0.7010 0.6371 0.048 Uiso 1 1 calc R . . H9B H 0.2196 0.6332 0.5270 0.048 Uiso 1 1 calc R . . C10 C 0.1384(2) 0.5887(2) 0.61783(18) 0.0452(6) Uani 1 1 d . . . H10A H 0.0904 0.5133 0.5743 0.054 Uiso 1 1 calc R . . H10B H 0.1715 0.5838 0.6839 0.054 Uiso 1 1 calc R . . C11 C 0.0452(2) 0.6648(2) 0.6113(2) 0.0543(7) Uani 1 1 d . . . H11A H 0.0891 0.7373 0.6596 0.081 Uiso 1 1 calc R . . H11B H -0.0299 0.6320 0.6226 0.081 Uiso 1 1 calc R . . H11C H 0.0163 0.6743 0.5473 0.081 Uiso 1 1 calc R . . C12 C 0.7135(2) 0.32373(17) 0.73322(14) 0.0323(5) Uani 1 1 d . . . C13 C 0.7663(2) 0.22914(18) 0.71564(16) 0.0418(5) Uani 1 1 d . . . H13 H 0.7628 0.1871 0.6550 0.050 Uiso 1 1 calc R . . C14 C 0.8253(2) 0.20826(19) 0.80426(18) 0.0457(6) Uani 1 1 d . . . H14 H 0.8679 0.1500 0.8132 0.055 Uiso 1 1 calc R . . C15 C 0.8093(2) 0.2893(2) 0.87656(16) 0.0411(5) Uani 1 1 d . . . H15 H 0.8396 0.2953 0.9428 0.049 Uiso 1 1 calc R . . C16 C 0.7404(2) 0.36026(19) 0.83358(15) 0.0344(5) Uani 1 1 d . . . H16 H 0.7161 0.4218 0.8660 0.041 Uiso 1 1 calc R . . C17 C 0.9868(3) 0.4780(2) 0.7615(2) 0.0561(7) Uani 1 1 d . . . H17 H 0.9404 0.5046 0.7111 0.067 Uiso 1 1 calc R . . C18 C 1.0445(2) 0.3864(2) 0.75160(19) 0.0520(6) Uani 1 1 d . . . H18 H 1.0442 0.3407 0.6934 0.062 Uiso 1 1 calc R . . C19 C 1.1027(2) 0.3748(2) 0.84341(18) 0.0494(6) Uani 1 1 d . . . H19 H 1.1483 0.3197 0.8578 0.059 Uiso 1 1 calc R . . C20 C 1.0815(2) 0.4595(2) 0.91011(19) 0.0506(6) Uani 1 1 d . . . H20 H 1.1103 0.4714 0.9773 0.061 Uiso 1 1 calc R . . C21 C 1.0104(3) 0.5232(2) 0.8598(2) 0.0549(7) Uani 1 1 d . . . H21 H 0.9829 0.5857 0.8870 0.066 Uiso 1 1 calc R . . C22 C 0.6501(2) 1.0653(2) 0.19247(15) 0.0419(5) Uani 1 1 d . . . H22 H 0.7324 1.1155 0.2272 0.050 Uiso 1 1 calc R . . C23 C 0.5812(2) 1.00919(17) 0.23257(14) 0.0329(5) Uani 1 1 d . . . C24 C 0.4697(2) 0.9478(2) 0.15515(15) 0.0400(5) Uani 1 1 d . . . H24 H 0.4006 0.8994 0.1585 0.048 Uiso 1 1 calc R . . C25 C 0.7655(2) 1.0392(2) 0.02577(16) 0.0423(5) Uani 1 1 d . . . H25A H 0.7985 1.0717 -0.0160 0.051 Uiso 1 1 calc R . . H25B H 0.8331 1.0682 0.0913 0.051 Uiso 1 1 calc R . . C26 C 0.7497(2) 0.9145(2) -0.00827(18) 0.0513(6) Uani 1 1 d . . . H26A H 0.6829 0.8847 -0.0741 0.062 Uiso 1 1 calc R . . H26B H 0.7173 0.8812 0.0334 0.062 Uiso 1 1 calc R . . C27 C 0.8723(3) 0.8778(3) -0.0086(2) 0.0850(12) Uani 1 1 d . . . H27A H 0.9089 0.9159 -0.0459 0.102 Uiso 1 1 calc R . . H27B H 0.9367 0.9016 0.0580 0.102 Uiso 1 1 calc R . . C28 C 0.8515(5) 0.7543(4) -0.0505(3) 0.128(2) Uani 1 1 d . . . H28A H 0.8149 0.7158 -0.0143 0.192 Uiso 1 1 calc R . . H28B H 0.9345 0.7360 -0.0469 0.192 Uiso 1 1 calc R . . H28C H 0.7914 0.7305 -0.1177 0.192 Uiso 1 1 calc R . . C29 C 0.6708(2) 1.21789(19) 0.06108(16) 0.0411(5) Uani 1 1 d . . . H29A H 0.7434 1.2451 0.1243 0.049 Uiso 1 1 calc R . . H29B H 0.7025 1.2426 0.0153 0.049 Uiso 1 1 calc R . . C30 C 0.5643(2) 1.2755(2) 0.06914(18) 0.0496(6) Uani 1 1 d . . . H30A H 0.5351 1.2554 0.1177 0.059 Uiso 1 1 calc R . . H30B H 0.4898 1.2478 0.0069 0.059 Uiso 1 1 calc R . . C31 C 0.6045(3) 1.4020(2) 0.0967(2) 0.0591(7) Uani 1 1 d . . . H31A H 0.6768 1.4304 0.1601 0.071 Uiso 1 1 calc R . . H31B H 0.6362 1.4226 0.0494 0.071 Uiso 1 1 calc R . . C32 C 0.4945(4) 1.4566(3) 0.1009(2) 0.0844(11) Uani 1 1 d . . . H32A H 0.4224 1.4286 0.0384 0.127 Uiso 1 1 calc R . . H32B H 0.5244 1.5372 0.1173 0.127 Uiso 1 1 calc R . . H32C H 0.4653 1.4393 0.1498 0.127 Uiso 1 1 calc R . . C33 C 0.6209(2) 1.00863(18) 0.33242(14) 0.0349(5) Uani 1 1 d . . . C34 C 0.5525(2) 0.9424(2) 0.37013(16) 0.0463(6) Uani 1 1 d . . . H34 H 0.4695 0.8933 0.3356 0.056 Uiso 1 1 calc R . . C35 C 0.6298(3) 0.9620(2) 0.46861(17) 0.0521(7) Uani 1 1 d . . . H35 H 0.6072 0.9285 0.5111 0.063 Uiso 1 1 calc R . . C36 C 0.7455(3) 1.0397(2) 0.49188(16) 0.0488(6) Uani 1 1 d . . . H36 H 0.8148 1.0673 0.5528 0.059 Uiso 1 1 calc R . . C37 C 0.7410(2) 1.06971(19) 0.40857(15) 0.0410(5) Uani 1 1 d . . . H37 H 0.8063 1.1213 0.4043 0.049 Uiso 1 1 calc R . . C38 C 0.7446(3) 0.8022(2) 0.26926(18) 0.0549(7) Uani 1 1 d . . . H38 H 0.7050 0.8019 0.2048 0.066 Uiso 1 1 calc R . . C39 C 0.6918(3) 0.7384(2) 0.3162(2) 0.0642(8) Uani 1 1 d . . . H39 H 0.6099 0.6871 0.2892 0.077 Uiso 1 1 calc R . . C40 C 0.7831(3) 0.7649(2) 0.4105(2) 0.0589(7) Uani 1 1 d . . . H40 H 0.7735 0.7337 0.4582 0.071 Uiso 1 1 calc R . . C41 C 0.8888(3) 0.8436(2) 0.42217(19) 0.0539(7) Uani 1 1 d . . . H41 H 0.9636 0.8765 0.4793 0.065 Uiso 1 1 calc R . . C42 C 0.8664(3) 0.8663(2) 0.3356(2) 0.0530(7) Uani 1 1 d . . . H42 H 0.9242 0.9169 0.3235 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03579(17) 0.03355(17) 0.03150(16) 0.00981(13) 0.01808(13) 0.01291(13) Fe2 0.03302(17) 0.03433(17) 0.02757(16) 0.00887(13) 0.01383(13) 0.00969(13) B1 0.0445(14) 0.0300(12) 0.0227(11) 0.0079(10) 0.0133(10) 0.0146(11) B2 0.0306(12) 0.0407(14) 0.0276(12) 0.0077(10) 0.0073(10) 0.0019(11) N1 0.0408(10) 0.0274(9) 0.0237(8) 0.0059(7) 0.0130(7) 0.0114(7) N2 0.0407(10) 0.0296(9) 0.0230(8) 0.0053(7) 0.0129(7) 0.0122(8) N3 0.0293(9) 0.0356(10) 0.0284(9) 0.0070(8) 0.0063(7) 0.0032(8) N4 0.0268(9) 0.0396(10) 0.0298(9) 0.0102(8) 0.0086(7) 0.0061(8) C1 0.0447(12) 0.0362(12) 0.0215(10) 0.0076(9) 0.0119(9) 0.0143(10) C2 0.0345(11) 0.0314(11) 0.0274(10) 0.0089(9) 0.0127(9) 0.0094(9) C3 0.0423(12) 0.0279(11) 0.0290(10) 0.0083(9) 0.0154(9) 0.0115(9) C4 0.0419(12) 0.0327(11) 0.0280(10) 0.0089(9) 0.0145(9) 0.0120(9) C5 0.0436(13) 0.0410(13) 0.0338(11) 0.0059(10) 0.0165(10) 0.0104(10) C6 0.0484(14) 0.0412(13) 0.0399(12) 0.0072(11) 0.0160(11) 0.0055(11) C7 0.0541(16) 0.0535(16) 0.0618(17) 0.0006(13) 0.0246(14) -0.0053(13) C8 0.0444(12) 0.0314(11) 0.0307(11) 0.0108(9) 0.0150(9) 0.0118(10) C9 0.0442(13) 0.0378(12) 0.0429(12) 0.0148(10) 0.0215(10) 0.0118(10) C10 0.0388(12) 0.0491(14) 0.0518(14) 0.0214(12) 0.0180(11) 0.0106(11) C11 0.0429(14) 0.0521(15) 0.0734(18) 0.0216(14) 0.0270(13) 0.0110(12) C12 0.0360(11) 0.0329(11) 0.0301(10) 0.0105(9) 0.0138(9) 0.0095(9) C13 0.0488(13) 0.0328(12) 0.0390(12) 0.0070(10) 0.0119(10) 0.0129(10) C14 0.0458(13) 0.0370(13) 0.0536(14) 0.0223(11) 0.0108(11) 0.0134(11) C15 0.0369(12) 0.0528(14) 0.0384(12) 0.0249(11) 0.0130(10) 0.0088(11) C16 0.0326(11) 0.0448(13) 0.0319(11) 0.0154(10) 0.0167(9) 0.0110(9) C17 0.0554(16) 0.0598(17) 0.0740(18) 0.0380(15) 0.0381(14) 0.0135(13) C18 0.0523(15) 0.0632(17) 0.0533(15) 0.0152(13) 0.0369(13) 0.0156(13) C19 0.0381(13) 0.0605(16) 0.0542(15) 0.0141(13) 0.0239(11) 0.0166(12) C20 0.0391(13) 0.0555(16) 0.0501(14) 0.0038(12) 0.0198(11) 0.0031(12) C21 0.0537(15) 0.0367(13) 0.0797(19) 0.0084(13) 0.0406(14) 0.0049(12) C22 0.0389(12) 0.0467(13) 0.0287(11) 0.0083(10) 0.0045(9) 0.0007(10) C23 0.0333(11) 0.0356(11) 0.0301(10) 0.0085(9) 0.0112(9) 0.0144(9) C24 0.0317(11) 0.0545(14) 0.0335(11) 0.0176(11) 0.0109(9) 0.0056(10) C25 0.0308(11) 0.0557(15) 0.0317(11) 0.0079(10) 0.0067(9) 0.0058(10) C26 0.0516(15) 0.0550(16) 0.0430(13) 0.0142(12) 0.0107(11) 0.0191(12) C27 0.072(2) 0.100(3) 0.0536(17) -0.0068(17) -0.0044(15) 0.054(2) C28 0.163(4) 0.111(3) 0.083(3) 0.003(2) 0.006(3) 0.100(3) C29 0.0414(12) 0.0444(13) 0.0339(11) 0.0087(10) 0.0142(10) 0.0040(10) C30 0.0530(15) 0.0554(16) 0.0482(14) 0.0205(12) 0.0241(12) 0.0168(12) C31 0.078(2) 0.0513(16) 0.0507(15) 0.0161(13) 0.0238(14) 0.0254(15) C32 0.125(3) 0.092(3) 0.069(2) 0.0326(19) 0.056(2) 0.067(2) C33 0.0364(11) 0.0401(12) 0.0290(10) 0.0083(9) 0.0118(9) 0.0170(10) C34 0.0356(12) 0.0732(17) 0.0375(12) 0.0185(12) 0.0185(10) 0.0220(12) C35 0.0552(15) 0.087(2) 0.0346(12) 0.0258(13) 0.0284(12) 0.0387(15) C36 0.0555(15) 0.0585(16) 0.0276(11) 0.0033(11) 0.0108(11) 0.0288(13) C37 0.0480(13) 0.0355(12) 0.0315(11) 0.0031(9) 0.0082(10) 0.0150(10) C38 0.0761(19) 0.0621(17) 0.0358(13) 0.0113(12) 0.0253(13) 0.0427(15) C39 0.0622(17) 0.0362(14) 0.083(2) -0.0051(14) 0.0334(16) 0.0037(13) C40 0.097(2) 0.0463(15) 0.0577(17) 0.0280(13) 0.0439(16) 0.0345(16) C41 0.0512(15) 0.0560(16) 0.0548(15) 0.0148(13) 0.0157(12) 0.0287(13) C42 0.0604(16) 0.0517(15) 0.0738(18) 0.0270(14) 0.0475(15) 0.0284(13) _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 C21 2.030(3) . ? Fe1 C13 2.030(2) . ? Fe1 C17 2.031(2) . ? Fe1 C14 2.036(2) . ? Fe1 C20 2.040(2) . ? Fe1 C12 2.040(2) . ? Fe1 C15 2.040(2) . ? Fe1 C16 2.042(2) . ? Fe1 C18 2.046(2) . ? Fe1 C19 2.048(2) . ? Fe2 C38 2.024(2) . ? Fe2 C42 2.025(2) . ? Fe2 C39 2.033(3) . ? Fe2 C36 2.035(2) . ? Fe2 C34 2.035(2) . ? Fe2 C37 2.037(2) . ? Fe2 C33 2.038(2) . ? Fe2 C41 2.038(2) . ? Fe2 C35 2.040(2) . ? Fe2 C40 2.045(2) . ? B1 N1 1.586(3) 2_666 ? B1 N2 1.588(3) . ? B1 C4 1.608(3) . ? B1 C8 1.625(3) . ? B2 N3 1.581(3) . ? B2 N4 1.585(3) 2_675 ? B2 C29 1.608(3) . ? B2 C25 1.614(3) . ? N1 C3 1.342(3) . ? N1 N2 1.359(2) . ? N1 B1 1.586(3) 2_666 ? N2 C1 1.343(3) . ? N3 C22 1.340(3) . ? N3 N4 1.343(2) . ? N4 C24 1.344(3) . ? N4 B2 1.585(3) 2_675 ? C1 C2 1.387(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(3) . ? C2 C12 1.463(3) . ? C3 H3 0.9500 . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.529(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.514(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.523(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.520(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.517(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.423(3) . ? C12 C16 1.428(3) . ? C13 C14 1.422(3) . ? C13 H13 0.9500 . ? C14 C15 1.411(3) . ? C14 H14 0.9500 . ? C15 C16 1.414(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.412(4) . ? C17 C21 1.415(4) . ? C17 H17 0.9500 . ? C18 C19 1.411(4) . ? C18 H18 0.9500 . ? C19 C20 1.413(3) . ? C19 H19 0.9500 . ? C20 C21 1.405(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.374(3) . ? C22 H22 0.9500 . ? C23 C24 1.384(3) . ? C23 C33 1.467(3) . ? C24 H24 0.9500 . ? C25 C26 1.516(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.517(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.507(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.511(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.528(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.511(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.419(3) . ? C33 C37 1.430(3) . ? C34 C35 1.426(3) . ? C34 H34 0.9500 . ? C35 C36 1.406(4) . ? C35 H35 0.9500 . ? C36 C37 1.423(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C42 1.402(4) . ? C38 C39 1.412(4) . ? C38 H38 0.9500 . ? C39 C40 1.409(4) . ? C39 H39 0.9500 . ? C40 C41 1.380(4) . ? C40 H40 0.9500 . ? C41 C42 1.393(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? 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 C21 Fe1 C13 155.64(11) . . ? C21 Fe1 C17 40.79(11) . . ? C13 Fe1 C17 120.08(11) . . ? C21 Fe1 C14 162.03(11) . . ? C13 Fe1 C14 40.94(9) . . ? C17 Fe1 C14 155.98(11) . . ? C21 Fe1 C20 40.39(11) . . ? C13 Fe1 C20 162.13(10) . . ? C17 Fe1 C20 68.26(12) . . ? C14 Fe1 C20 125.56(10) . . ? C21 Fe1 C12 120.31(10) . . ? C13 Fe1 C12 40.94(8) . . ? C17 Fe1 C12 106.24(10) . . ? C14 Fe1 C12 68.94(9) . . ? C20 Fe1 C12 156.12(9) . . ? C21 Fe1 C15 125.20(11) . . ? C13 Fe1 C15 68.52(10) . . ? C17 Fe1 C15 161.63(11) . . ? C14 Fe1 C15 40.50(10) . . ? C20 Fe1 C15 108.70(10) . . ? C12 Fe1 C15 68.80(8) . . ? C21 Fe1 C16 107.68(10) . . ? C13 Fe1 C16 68.53(9) . . ? C17 Fe1 C16 124.36(10) . . ? C14 Fe1 C16 68.30(10) . . ? C20 Fe1 C16 121.64(9) . . ? C12 Fe1 C16 40.96(8) . . ? C15 Fe1 C16 40.53(9) . . ? C21 Fe1 C18 68.17(11) . . ? C13 Fe1 C18 107.19(11) . . ? C17 Fe1 C18 40.52(11) . . ? C14 Fe1 C18 121.36(11) . . ? C20 Fe1 C18 68.00(11) . . ? C12 Fe1 C18 123.83(10) . . ? C15 Fe1 C18 156.82(10) . . ? C16 Fe1 C18 161.09(10) . . ? C21 Fe1 C19 67.99(11) . . ? C13 Fe1 C19 124.92(10) . . ? C17 Fe1 C19 68.09(11) . . ? C14 Fe1 C19 108.46(10) . . ? C20 Fe1 C19 40.43(10) . . ? C12 Fe1 C19 161.10(9) . . ? C15 Fe1 C19 122.20(10) . . ? C16 Fe1 C19 157.04(9) . . ? C18 Fe1 C19 40.32(10) . . ? C38 Fe2 C42 40.51(11) . . ? C38 Fe2 C39 40.74(12) . . ? C42 Fe2 C39 67.85(11) . . ? C38 Fe2 C36 162.19(12) . . ? C42 Fe2 C36 125.85(12) . . ? C39 Fe2 C36 155.95(12) . . ? C38 Fe2 C34 119.32(10) . . ? C42 Fe2 C34 153.86(10) . . ? C39 Fe2 C34 108.10(12) . . ? C36 Fe2 C34 68.55(10) . . ? C38 Fe2 C37 124.19(11) . . ? C42 Fe2 C37 106.87(11) . . ? C39 Fe2 C37 162.04(11) . . ? C36 Fe2 C37 40.92(10) . . ? C34 Fe2 C37 68.59(11) . . ? C38 Fe2 C33 105.71(9) . . ? C42 Fe2 C33 118.78(10) . . ? C39 Fe2 C33 124.95(11) . . ? C36 Fe2 C33 69.06(9) . . ? C34 Fe2 C33 40.79(9) . . ? C37 Fe2 C33 41.09(9) . . ? C38 Fe2 C41 67.99(11) . . ? C42 Fe2 C41 40.08(11) . . ? C39 Fe2 C41 67.68(12) . . ? C36 Fe2 C41 108.82(10) . . ? C34 Fe2 C41 164.50(11) . . ? C37 Fe2 C41 120.14(11) . . ? C33 Fe2 C41 153.98(11) . . ? C38 Fe2 C35 155.29(12) . . ? C42 Fe2 C35 163.41(11) . . ? C39 Fe2 C35 121.43(12) . . ? C36 Fe2 C35 40.38(11) . . ? C34 Fe2 C35 40.95(9) . . ? C37 Fe2 C35 68.46(11) . . ? C33 Fe2 C35 68.90(9) . . ? C41 Fe2 C35 127.28(10) . . ? C38 Fe2 C40 67.85(11) . . ? C42 Fe2 C40 66.93(11) . . ? C39 Fe2 C40 40.42(12) . . ? C36 Fe2 C40 121.65(10) . . ? C34 Fe2 C40 127.78(12) . . ? C37 Fe2 C40 155.09(11) . . ? C33 Fe2 C40 163.50(11) . . ? C41 Fe2 C40 39.52(11) . . ? C35 Fe2 C40 110.18(11) . . ? N1 B1 N2 104.51(15) 2_666 . ? N1 B1 C4 109.45(17) 2_666 . ? N2 B1 C4 110.51(17) . . ? N1 B1 C8 109.87(17) 2_666 . ? N2 B1 C8 107.20(17) . . ? C4 B1 C8 114.79(17) . . ? N3 B2 N4 105.05(17) . 2_675 ? N3 B2 C29 110.01(18) . . ? N4 B2 C29 111.18(18) 2_675 . ? N3 B2 C25 110.34(18) . . ? N4 B2 C25 108.81(18) 2_675 . ? C29 B2 C25 111.27(19) . . ? C3 N1 N2 108.09(15) . . ? C3 N1 B1 125.84(16) . 2_666 ? N2 N1 B1 124.11(16) . 2_666 ? C1 N2 N1 107.71(16) . . ? C1 N2 B1 124.55(16) . . ? N1 N2 B1 125.22(15) . . ? C22 N3 N4 107.63(18) . . ? C22 N3 B2 124.34(18) . . ? N4 N3 B2 127.94(16) . . ? N3 N4 C24 108.06(16) . . ? N3 N4 B2 126.79(17) . 2_675 ? C24 N4 B2 125.08(18) . 2_675 ? N2 C1 C2 110.19(18) . . ? N2 C1 H1 124.9 . . ? C2 C1 H1 124.9 . . ? C3 C2 C1 103.97(17) . . ? C3 C2 C12 128.28(19) . . ? C1 C2 C12 127.74(18) . . ? N1 C3 C2 110.02(18) . . ? N1 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? C5 C4 B1 117.04(18) . . ? C5 C4 H4A 108.0 . . ? B1 C4 H4A 108.0 . . ? C5 C4 H4B 108.0 . . ? B1 C4 H4B 108.0 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C6 114.27(18) . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C5 112.9(2) . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? 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 . . ? C9 C8 B1 117.06(18) . . ? C9 C8 H8A 108.0 . . ? B1 C8 H8A 108.0 . . ? C9 C8 H8B 108.0 . . ? B1 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 114.06(19) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 113.9(2) . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C16 107.02(18) . . ? C13 C12 C2 126.44(19) . . ? C16 C12 C2 126.51(19) . . ? C13 C12 Fe1 69.17(13) . . ? C16 C12 Fe1 69.59(12) . . ? C2 C12 Fe1 124.85(15) . . ? C14 C13 C12 108.3(2) . . ? C14 C13 Fe1 69.75(13) . . ? C12 C13 Fe1 69.90(12) . . ? C14 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? Fe1 C13 H13 126.1 . . ? C15 C14 C13 108.0(2) . . ? C15 C14 Fe1 69.89(13) . . ? C13 C14 Fe1 69.31(13) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Fe1 C14 H14 126.3 . . ? C14 C15 C16 108.28(19) . . ? C14 C15 Fe1 69.60(13) . . ? C16 C15 Fe1 69.81(12) . . ? C14 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Fe1 C15 H15 126.3 . . ? C15 C16 C12 108.40(19) . . ? C15 C16 Fe1 69.66(12) . . ? C12 C16 Fe1 69.45(12) . . ? C15 C16 H16 125.8 . . ? C12 C16 H16 125.8 . . ? Fe1 C16 H16 126.7 . . ? C18 C17 C21 107.8(2) . . ? C18 C17 Fe1 70.32(15) . . ? C21 C17 Fe1 69.55(14) . . ? C18 C17 H17 126.1 . . ? C21 C17 H17 126.1 . . ? Fe1 C17 H17 125.6 . . ? C19 C18 C17 108.0(2) . . ? C19 C18 Fe1 69.92(14) . . ? C17 C18 Fe1 69.16(14) . . ? C19 C18 H18 126.0 . . ? C17 C18 H18 126.0 . . ? Fe1 C18 H18 126.5 . . ? C18 C19 C20 108.0(2) . . ? C18 C19 Fe1 69.75(14) . . ? C20 C19 Fe1 69.45(14) . . ? C18 C19 H19 126.0 . . ? C20 C19 H19 126.0 . . ? Fe1 C19 H19 126.4 . . ? C21 C20 C19 108.1(2) . . ? C21 C20 Fe1 69.43(15) . . ? C19 C20 Fe1 70.12(14) . . ? C21 C20 H20 126.0 . . ? C19 C20 H20 126.0 . . ? Fe1 C20 H20 126.1 . . ? C20 C21 C17 108.2(2) . . ? C20 C21 Fe1 70.18(15) . . ? C17 C21 Fe1 69.65(15) . . ? C20 C21 H21 125.9 . . ? C17 C21 H21 125.9 . . ? Fe1 C21 H21 125.8 . . ? N3 C22 C23 110.8(2) . . ? N3 C22 H22 124.6 . . ? C23 C22 H22 124.6 . . ? C22 C23 C24 103.48(18) . . ? C22 C23 C33 128.1(2) . . ? C24 C23 C33 128.3(2) . . ? N4 C24 C23 110.0(2) . . ? N4 C24 H24 125.0 . . ? C23 C24 H24 125.0 . . ? C26 C25 B2 117.6(2) . . ? C26 C25 H25A 107.9 . . ? B2 C25 H25A 107.9 . . ? C26 C25 H25B 107.9 . . ? B2 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? C25 C26 C27 114.8(2) . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.5 . . ? C28 C27 C26 113.7(3) . . ? C28 C27 H27A 108.8 . . ? C26 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? C26 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 B2 118.9(2) . . ? C30 C29 H29A 107.6 . . ? B2 C29 H29A 107.6 . . ? C30 C29 H29B 107.6 . . ? B2 C29 H29B 107.6 . . ? H29A C29 H29B 107.0 . . ? C29 C30 C31 114.0(2) . . ? C29 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? C29 C30 H30B 108.7 . . ? C31 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C32 C31 C30 112.6(3) . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? C30 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C37 107.28(19) . . ? C34 C33 C23 126.8(2) . . ? C37 C33 C23 125.8(2) . . ? C34 C33 Fe2 69.51(12) . . ? C37 C33 Fe2 69.41(12) . . ? C23 C33 Fe2 123.06(14) . . ? C33 C34 C35 108.4(2) . . ? C33 C34 Fe2 69.71(12) . . ? C35 C34 Fe2 69.70(13) . . ? C33 C34 H34 125.8 . . ? C35 C34 H34 125.8 . . ? Fe2 C34 H34 126.4 . . ? C36 C35 C34 108.1(2) . . ? C36 C35 Fe2 69.61(13) . . ? C34 C35 Fe2 69.35(13) . . ? C36 C35 H35 126.0 . . ? C34 C35 H35 126.0 . . ? Fe2 C35 H35 126.6 . . ? C35 C36 C37 108.3(2) . . ? C35 C36 Fe2 70.01(14) . . ? C37 C36 Fe2 69.62(12) . . ? C35 C36 H36 125.9 . . ? C37 C36 H36 125.9 . . ? Fe2 C36 H36 126.1 . . ? C36 C37 C33 108.0(2) . . ? C36 C37 Fe2 69.46(13) . . ? C33 C37 Fe2 69.50(12) . . ? C36 C37 H37 126.0 . . ? C33 C37 H37 126.0 . . ? Fe2 C37 H37 126.6 . . ? C42 C38 C39 107.2(2) . . ? C42 C38 Fe2 69.81(14) . . ? C39 C38 Fe2 69.99(14) . . ? C42 C38 H38 126.4 . . ? C39 C38 H38 126.4 . . ? Fe2 C38 H38 125.4 . . ? C40 C39 C38 107.2(3) . . ? C40 C39 Fe2 70.23(15) . . ? C38 C39 Fe2 69.28(15) . . ? C40 C39 H39 126.4 . . ? C38 C39 H39 126.4 . . ? Fe2 C39 H39 125.7 . . ? C41 C40 C39 108.8(2) . . ? C41 C40 Fe2 70.00(14) . . ? C39 C40 Fe2 69.35(15) . . ? C41 C40 H40 125.6 . . ? C39 C40 H40 125.6 . . ? Fe2 C40 H40 126.6 . . ? C40 C41 C42 108.1(2) . . ? C40 C41 Fe2 70.48(15) . . ? C42 C41 Fe2 69.46(14) . . ? C40 C41 H41 126.0 . . ? C42 C41 H41 126.0 . . ? Fe2 C41 H41 125.7 . . ? C41 C42 C38 108.7(2) . . ? C41 C42 Fe2 70.46(14) . . ? C38 C42 Fe2 69.68(14) . . ? C41 C42 H42 125.6 . . ? C38 C42 H42 125.6 . . ? Fe2 C42 H42 125.8 . . ? 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 C3 N1 N2 C1 -0.6(2) . . . . ? B1 N1 N2 C1 -165.43(19) 2_666 . . . ? C3 N1 N2 B1 -163.22(19) . . . . ? B1 N1 N2 B1 32.0(3) 2_666 . . . ? N1 B1 N2 C1 173.30(19) 2_666 . . . ? C4 B1 N2 C1 55.7(3) . . . . ? C8 B1 N2 C1 -70.1(2) . . . . ? N1 B1 N2 N1 -26.9(3) 2_666 . . . ? C4 B1 N2 N1 -144.56(19) . . . . ? C8 B1 N2 N1 89.7(2) . . . . ? N4 B2 N3 C22 -178.68(19) 2_675 . . . ? C29 B2 N3 C22 -58.9(3) . . . . ? C25 B2 N3 C22 64.2(3) . . . . ? N4 B2 N3 N4 5.1(3) 2_675 . . . ? C29 B2 N3 N4 124.8(2) . . . . ? C25 B2 N3 N4 -112.0(2) . . . . ? C22 N3 N4 C24 0.1(2) . . . . ? B2 N3 N4 C24 176.8(2) . . . . ? C22 N3 N4 B2 177.1(2) . . . 2_675 ? B2 N3 N4 B2 -6.1(4) . . . 2_675 ? N1 N2 C1 C2 0.7(2) . . . . ? B1 N2 C1 C2 163.44(19) . . . . ? N2 C1 C2 C3 -0.5(2) . . . . ? N2 C1 C2 C12 178.3(2) . . . . ? N2 N1 C3 C2 0.3(2) . . . . ? B1 N1 C3 C2 164.81(19) 2_666 . . . ? C1 C2 C3 N1 0.1(2) . . . . ? C12 C2 C3 N1 -178.7(2) . . . . ? N1 B1 C4 C5 -60.1(2) 2_666 . . . ? N2 B1 C4 C5 54.5(2) . . . . ? C8 B1 C4 C5 175.83(18) . . . . ? B1 C4 C5 C6 173.04(18) . . . . ? C4 C5 C6 C7 177.7(2) . . . . ? N1 B1 C8 C9 -69.8(2) 2_666 . . . ? N2 B1 C8 C9 177.15(17) . . . . ? C4 B1 C8 C9 54.0(2) . . . . ? B1 C8 C9 C10 -172.65(19) . . . . ? C8 C9 C10 C11 -178.6(2) . . . . ? C3 C2 C12 C13 11.4(4) . . . . ? C1 C2 C12 C13 -167.1(2) . . . . ? C3 C2 C12 C16 -170.8(2) . . . . ? C1 C2 C12 C16 10.7(4) . . . . ? C3 C2 C12 Fe1 99.9(2) . . . . ? C1 C2 C12 Fe1 -78.5(3) . . . . ? C21 Fe1 C12 C13 159.45(14) . . . . ? C17 Fe1 C12 C13 117.45(15) . . . . ? C14 Fe1 C12 C13 -37.68(14) . . . . ? C20 Fe1 C12 C13 -169.7(2) . . . . ? C15 Fe1 C12 C13 -81.24(15) . . . . ? C16 Fe1 C12 C13 -118.41(18) . . . . ? C18 Fe1 C12 C13 76.73(17) . . . . ? C19 Fe1 C12 C13 47.9(3) . . . . ? C21 Fe1 C12 C16 -82.13(16) . . . . ? C13 Fe1 C12 C16 118.41(18) . . . . ? C17 Fe1 C12 C16 -124.14(14) . . . . ? C14 Fe1 C12 C16 80.74(14) . . . . ? C20 Fe1 C12 C16 -51.3(3) . . . . ? C15 Fe1 C12 C16 37.17(13) . . . . ? C18 Fe1 C12 C16 -164.85(14) . . . . ? C19 Fe1 C12 C16 166.3(3) . . . . ? C21 Fe1 C12 C2 38.8(2) . . . . ? C13 Fe1 C12 C2 -120.6(2) . . . . ? C17 Fe1 C12 C2 -3.2(2) . . . . ? C14 Fe1 C12 C2 -158.3(2) . . . . ? C20 Fe1 C12 C2 69.7(3) . . . . ? C15 Fe1 C12 C2 158.1(2) . . . . ? C16 Fe1 C12 C2 121.0(2) . . . . ? C18 Fe1 C12 C2 -43.9(2) . . . . ? C19 Fe1 C12 C2 -72.7(4) . . . . ? C16 C12 C13 C14 -0.2(3) . . . . ? C2 C12 C13 C14 178.0(2) . . . . ? Fe1 C12 C13 C14 59.36(17) . . . . ? C16 C12 C13 Fe1 -59.56(15) . . . . ? C2 C12 C13 Fe1 118.6(2) . . . . ? C21 Fe1 C13 C14 -166.7(2) . . . . ? C17 Fe1 C13 C14 160.57(15) . . . . ? C20 Fe1 C13 C14 46.9(4) . . . . ? C12 Fe1 C13 C14 -119.5(2) . . . . ? C15 Fe1 C13 C14 -37.50(14) . . . . ? C16 Fe1 C13 C14 -81.20(15) . . . . ? C18 Fe1 C13 C14 118.33(15) . . . . ? C19 Fe1 C13 C14 77.56(18) . . . . ? C21 Fe1 C13 C12 -47.3(3) . . . . ? C17 Fe1 C13 C12 -79.94(16) . . . . ? C14 Fe1 C13 C12 119.5(2) . . . . ? C20 Fe1 C13 C12 166.4(3) . . . . ? C15 Fe1 C13 C12 81.99(14) . . . . ? C16 Fe1 C13 C12 38.29(12) . . . . ? C18 Fe1 C13 C12 -122.18(14) . . . . ? C19 Fe1 C13 C12 -162.95(13) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? Fe1 C13 C14 C15 59.43(17) . . . . ? C12 C13 C14 Fe1 -59.45(16) . . . . ? C21 Fe1 C14 C15 42.9(4) . . . . ? C13 Fe1 C14 C15 -119.28(19) . . . . ? C17 Fe1 C14 C15 -164.3(2) . . . . ? C20 Fe1 C14 C15 76.70(16) . . . . ? C12 Fe1 C14 C15 -81.61(14) . . . . ? C16 Fe1 C14 C15 -37.47(12) . . . . ? C18 Fe1 C14 C15 160.75(14) . . . . ? C19 Fe1 C14 C15 118.30(14) . . . . ? C21 Fe1 C14 C13 162.1(3) . . . . ? C17 Fe1 C14 C13 -45.0(3) . . . . ? C20 Fe1 C14 C13 -164.02(14) . . . . ? C12 Fe1 C14 C13 37.67(14) . . . . ? C15 Fe1 C14 C13 119.28(19) . . . . ? C16 Fe1 C14 C13 81.81(14) . . . . ? C18 Fe1 C14 C13 -79.96(17) . . . . ? C19 Fe1 C14 C13 -122.42(15) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? Fe1 C14 C15 C16 59.30(16) . . . . ? C13 C14 C15 Fe1 -59.06(17) . . . . ? C21 Fe1 C15 C14 -165.12(14) . . . . ? C13 Fe1 C15 C14 37.89(13) . . . . ? C17 Fe1 C15 C14 159.5(3) . . . . ? C20 Fe1 C15 C14 -123.30(14) . . . . ? C12 Fe1 C15 C14 82.00(14) . . . . ? C16 Fe1 C15 C14 119.55(19) . . . . ? C18 Fe1 C15 C14 -45.7(3) . . . . ? C19 Fe1 C15 C14 -80.73(16) . . . . ? C21 Fe1 C15 C16 75.33(17) . . . . ? C13 Fe1 C15 C16 -81.66(14) . . . . ? C17 Fe1 C15 C16 39.9(4) . . . . ? C14 Fe1 C15 C16 -119.55(19) . . . . ? C20 Fe1 C15 C16 117.15(14) . . . . ? C12 Fe1 C15 C16 -37.56(13) . . . . ? C18 Fe1 C15 C16 -165.2(2) . . . . ? C19 Fe1 C15 C16 159.71(13) . . . . ? C14 C15 C16 C12 -0.4(3) . . . . ? Fe1 C15 C16 C12 58.81(15) . . . . ? C14 C15 C16 Fe1 -59.17(16) . . . . ? C13 C12 C16 C15 0.3(2) . . . . ? C2 C12 C16 C15 -177.8(2) . . . . ? Fe1 C12 C16 C15 -58.94(15) . . . . ? C13 C12 C16 Fe1 59.28(16) . . . . ? C2 C12 C16 Fe1 -118.9(2) . . . . ? C21 Fe1 C16 C15 -123.94(15) . . . . ? C13 Fe1 C16 C15 81.64(15) . . . . ? C17 Fe1 C16 C15 -165.81(15) . . . . ? C14 Fe1 C16 C15 37.45(14) . . . . ? C20 Fe1 C16 C15 -81.89(17) . . . . ? C12 Fe1 C16 C15 119.90(19) . . . . ? C18 Fe1 C16 C15 162.0(3) . . . . ? C19 Fe1 C16 C15 -48.8(3) . . . . ? C21 Fe1 C16 C12 116.16(14) . . . . ? C13 Fe1 C16 C12 -38.27(12) . . . . ? C17 Fe1 C16 C12 74.29(17) . . . . ? C14 Fe1 C16 C12 -82.45(14) . . . . ? C20 Fe1 C16 C12 158.21(14) . . . . ? C15 Fe1 C16 C12 -119.90(19) . . . . ? C18 Fe1 C16 C12 42.1(4) . . . . ? C19 Fe1 C16 C12 -168.7(2) . . . . ? C21 Fe1 C17 C18 118.7(2) . . . . ? C13 Fe1 C17 C18 -81.26(18) . . . . ? C14 Fe1 C17 C18 -48.9(3) . . . . ? C20 Fe1 C17 C18 81.13(17) . . . . ? C12 Fe1 C17 C18 -123.48(16) . . . . ? C15 Fe1 C17 C18 165.1(3) . . . . ? C16 Fe1 C17 C18 -164.57(15) . . . . ? C19 Fe1 C17 C18 37.43(16) . . . . ? C13 Fe1 C17 C21 160.07(15) . . . . ? C14 Fe1 C17 C21 -167.6(2) . . . . ? C20 Fe1 C17 C21 -37.54(16) . . . . ? C12 Fe1 C17 C21 117.85(16) . . . . ? C15 Fe1 C17 C21 46.4(4) . . . . ? C16 Fe1 C17 C21 76.75(19) . . . . ? C18 Fe1 C17 C21 -118.7(2) . . . . ? C19 Fe1 C17 C21 -81.25(17) . . . . ? C21 C17 C18 C19 0.3(3) . . . . ? Fe1 C17 C18 C19 -59.36(18) . . . . ? C21 C17 C18 Fe1 59.70(17) . . . . ? C21 Fe1 C18 C19 81.26(17) . . . . ? C13 Fe1 C18 C19 -124.15(16) . . . . ? C17 Fe1 C18 C19 119.4(2) . . . . ? C14 Fe1 C18 C19 -81.66(18) . . . . ? C20 Fe1 C18 C19 37.57(16) . . . . ? C12 Fe1 C18 C19 -166.03(14) . . . . ? C15 Fe1 C18 C19 -48.7(3) . . . . ? C16 Fe1 C18 C19 162.1(3) . . . . ? C21 Fe1 C18 C17 -38.13(17) . . . . ? C13 Fe1 C18 C17 116.46(17) . . . . ? C14 Fe1 C18 C17 158.95(16) . . . . ? C20 Fe1 C18 C17 -81.82(18) . . . . ? C12 Fe1 C18 C17 74.58(19) . . . . ? C15 Fe1 C18 C17 -168.1(2) . . . . ? C16 Fe1 C18 C17 42.7(4) . . . . ? C19 Fe1 C18 C17 -119.4(2) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? Fe1 C18 C19 C20 -59.12(17) . . . . ? C17 C18 C19 Fe1 58.88(18) . . . . ? C21 Fe1 C19 C18 -81.75(18) . . . . ? C13 Fe1 C19 C18 74.61(19) . . . . ? C17 Fe1 C19 C18 -37.60(16) . . . . ? C14 Fe1 C19 C18 117.04(16) . . . . ? C20 Fe1 C19 C18 -119.3(2) . . . . ? C12 Fe1 C19 C18 38.3(4) . . . . ? C15 Fe1 C19 C18 159.55(15) . . . . ? C16 Fe1 C19 C18 -165.2(2) . . . . ? C21 Fe1 C19 C20 37.60(16) . . . . ? C13 Fe1 C19 C20 -166.04(15) . . . . ? C17 Fe1 C19 C20 81.75(18) . . . . ? C14 Fe1 C19 C20 -123.61(17) . . . . ? C12 Fe1 C19 C20 157.6(3) . . . . ? C15 Fe1 C19 C20 -81.10(19) . . . . ? C16 Fe1 C19 C20 -45.8(3) . . . . ? C18 Fe1 C19 C20 119.3(2) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? Fe1 C19 C20 C21 -59.27(17) . . . . ? C18 C19 C20 Fe1 59.31(18) . . . . ? C13 Fe1 C20 C21 159.4(3) . . . . ? C17 Fe1 C20 C21 37.91(15) . . . . ? C14 Fe1 C20 C21 -164.63(15) . . . . ? C12 Fe1 C20 C21 -43.1(3) . . . . ? C15 Fe1 C20 C21 -122.77(16) . . . . ? C16 Fe1 C20 C21 -79.99(17) . . . . ? C18 Fe1 C20 C21 81.72(17) . . . . ? C19 Fe1 C20 C21 119.2(2) . . . . ? C21 Fe1 C20 C19 -119.2(2) . . . . ? C13 Fe1 C20 C19 40.2(4) . . . . ? C17 Fe1 C20 C19 -81.29(17) . . . . ? C14 Fe1 C20 C19 76.18(19) . . . . ? C12 Fe1 C20 C19 -162.2(2) . . . . ? C15 Fe1 C20 C19 118.04(16) . . . . ? C16 Fe1 C20 C19 160.81(15) . . . . ? C18 Fe1 C20 C19 -37.47(16) . . . . ? C19 C20 C21 C17 0.2(3) . . . . ? Fe1 C20 C21 C17 -59.53(18) . . . . ? C19 C20 C21 Fe1 59.71(17) . . . . ? C18 C17 C21 C20 -0.3(3) . . . . ? Fe1 C17 C21 C20 59.86(18) . . . . ? C18 C17 C21 Fe1 -60.18(18) . . . . ? C13 Fe1 C21 C20 -164.8(2) . . . . ? C17 Fe1 C21 C20 -119.1(2) . . . . ? C14 Fe1 C21 C20 44.3(4) . . . . ? C12 Fe1 C21 C20 161.33(14) . . . . ? C15 Fe1 C21 C20 77.08(17) . . . . ? C16 Fe1 C21 C20 118.36(15) . . . . ? C18 Fe1 C21 C20 -81.26(16) . . . . ? C19 Fe1 C21 C20 -37.64(15) . . . . ? C13 Fe1 C21 C17 -45.7(3) . . . . ? C14 Fe1 C21 C17 163.5(3) . . . . ? C20 Fe1 C21 C17 119.1(2) . . . . ? C12 Fe1 C21 C17 -79.53(17) . . . . ? C15 Fe1 C21 C17 -163.78(15) . . . . ? C16 Fe1 C21 C17 -122.50(16) . . . . ? C18 Fe1 C21 C17 37.88(16) . . . . ? C19 Fe1 C21 C17 81.50(17) . . . . ? N4 N3 C22 C23 0.1(3) . . . . ? B2 N3 C22 C23 -176.82(19) . . . . ? N3 C22 C23 C24 -0.2(3) . . . . ? N3 C22 C23 C33 176.0(2) . . . . ? N3 N4 C24 C23 -0.2(2) . . . . ? B2 N4 C24 C23 -177.31(19) 2_675 . . . ? C22 C23 C24 N4 0.2(3) . . . . ? C33 C23 C24 N4 -175.92(19) . . . . ? N3 B2 C25 C26 60.3(2) . . . . ? N4 B2 C25 C26 -54.5(3) 2_675 . . . ? C29 B2 C25 C26 -177.28(19) . . . . ? B2 C25 C26 C27 -179.9(2) . . . . ? C25 C26 C27 C28 -175.1(3) . . . . ? N3 B2 C29 C30 -56.4(3) . . . . ? N4 B2 C29 C30 59.5(3) 2_675 . . . ? C25 B2 C29 C30 -179.04(19) . . . . ? B2 C29 C30 C31 -177.5(2) . . . . ? C29 C30 C31 C32 178.1(2) . . . . ? C22 C23 C33 C34 -174.1(2) . . . . ? C24 C23 C33 C34 1.2(4) . . . . ? C22 C23 C33 C37 1.2(4) . . . . ? C24 C23 C33 C37 176.4(2) . . . . ? C22 C23 C33 Fe2 -86.0(3) . . . . ? C24 C23 C33 Fe2 89.2(3) . . . . ? C38 Fe2 C33 C34 116.92(16) . . . . ? C42 Fe2 C33 C34 158.62(15) . . . . ? C39 Fe2 C33 C34 76.71(17) . . . . ? C36 Fe2 C33 C34 -81.03(15) . . . . ? C37 Fe2 C33 C34 -118.63(19) . . . . ? C41 Fe2 C33 C34 -171.2(2) . . . . ? C35 Fe2 C33 C34 -37.63(15) . . . . ? C40 Fe2 C33 C34 52.4(4) . . . . ? C38 Fe2 C33 C37 -124.45(15) . . . . ? C42 Fe2 C33 C37 -82.75(16) . . . . ? C39 Fe2 C33 C37 -164.66(15) . . . . ? C36 Fe2 C33 C37 37.60(15) . . . . ? C34 Fe2 C33 C37 118.63(19) . . . . ? C41 Fe2 C33 C37 -52.6(3) . . . . ? C35 Fe2 C33 C37 81.00(15) . . . . ? C40 Fe2 C33 C37 171.0(3) . . . . ? C38 Fe2 C33 C23 -4.4(2) . . . . ? C42 Fe2 C33 C23 37.3(2) . . . . ? C39 Fe2 C33 C23 -44.6(2) . . . . ? C36 Fe2 C33 C23 157.6(2) . . . . ? C34 Fe2 C33 C23 -121.3(2) . . . . ? C37 Fe2 C33 C23 120.0(2) . . . . ? C41 Fe2 C33 C23 67.4(3) . . . . ? C35 Fe2 C33 C23 -159.0(2) . . . . ? C40 Fe2 C33 C23 -69.0(4) . . . . ? C37 C33 C34 C35 -0.2(3) . . . . ? C23 C33 C34 C35 175.8(2) . . . . ? Fe2 C33 C34 C35 59.17(16) . . . . ? C37 C33 C34 Fe2 -59.37(15) . . . . ? C23 C33 C34 Fe2 116.6(2) . . . . ? C38 Fe2 C34 C33 -79.88(17) . . . . ? C42 Fe2 C34 C33 -46.5(3) . . . . ? C39 Fe2 C34 C33 -122.94(15) . . . . ? C36 Fe2 C34 C33 82.40(15) . . . . ? C37 Fe2 C34 C33 38.29(13) . . . . ? C41 Fe2 C34 C33 165.5(4) . . . . ? C35 Fe2 C34 C33 119.7(2) . . . . ? C40 Fe2 C34 C33 -163.47(14) . . . . ? C38 Fe2 C34 C35 160.46(17) . . . . ? C42 Fe2 C34 C35 -166.1(2) . . . . ? C39 Fe2 C34 C35 117.40(18) . . . . ? C36 Fe2 C34 C35 -37.26(17) . . . . ? C37 Fe2 C34 C35 -81.37(17) . . . . ? C33 Fe2 C34 C35 -119.7(2) . . . . ? C41 Fe2 C34 C35 45.8(5) . . . . ? C40 Fe2 C34 C35 76.9(2) . . . . ? C33 C34 C35 C36 -0.1(3) . . . . ? Fe2 C34 C35 C36 59.03(17) . . . . ? C33 C34 C35 Fe2 -59.18(16) . . . . ? C38 Fe2 C35 C36 -163.8(2) . . . . ? C42 Fe2 C35 C36 38.7(4) . . . . ? C39 Fe2 C35 C36 158.97(16) . . . . ? C34 Fe2 C35 C36 -119.6(2) . . . . ? C37 Fe2 C35 C36 -37.84(14) . . . . ? C33 Fe2 C35 C36 -82.10(15) . . . . ? C41 Fe2 C35 C36 74.37(19) . . . . ? C40 Fe2 C35 C36 115.52(16) . . . . ? C38 Fe2 C35 C34 -44.2(3) . . . . ? C42 Fe2 C35 C34 158.3(3) . . . . ? C39 Fe2 C35 C34 -81.5(2) . . . . ? C36 Fe2 C35 C34 119.6(2) . . . . ? C37 Fe2 C35 C34 81.74(17) . . . . ? C33 Fe2 C35 C34 37.48(15) . . . . ? C41 Fe2 C35 C34 -166.05(16) . . . . ? C40 Fe2 C35 C34 -124.91(17) . . . . ? C34 C35 C36 C37 0.4(3) . . . . ? Fe2 C35 C36 C37 59.31(16) . . . . ? C34 C35 C36 Fe2 -58.87(17) . . . . ? C38 Fe2 C36 C35 157.6(3) . . . . ? C42 Fe2 C36 C35 -167.27(14) . . . . ? C39 Fe2 C36 C35 -48.7(3) . . . . ? C34 Fe2 C36 C35 37.77(14) . . . . ? C37 Fe2 C36 C35 119.4(2) . . . . ? C33 Fe2 C36 C35 81.66(15) . . . . ? C41 Fe2 C36 C35 -125.95(15) . . . . ? C40 Fe2 C36 C35 -84.31(18) . . . . ? C38 Fe2 C36 C37 38.2(4) . . . . ? C42 Fe2 C36 C37 73.32(17) . . . . ? C39 Fe2 C36 C37 -168.1(2) . . . . ? C34 Fe2 C36 C37 -81.64(15) . . . . ? C33 Fe2 C36 C37 -37.75(14) . . . . ? C41 Fe2 C36 C37 114.64(15) . . . . ? C35 Fe2 C36 C37 -119.4(2) . . . . ? C40 Fe2 C36 C37 156.28(16) . . . . ? C35 C36 C37 C33 -0.6(3) . . . . ? Fe2 C36 C37 C33 58.99(15) . . . . ? C35 C36 C37 Fe2 -59.56(17) . . . . ? C34 C33 C37 C36 0.5(2) . . . . ? C23 C33 C37 C36 -175.55(19) . . . . ? Fe2 C33 C37 C36 -58.96(15) . . . . ? C34 C33 C37 Fe2 59.44(15) . . . . ? C23 C33 C37 Fe2 -116.6(2) . . . . ? C38 Fe2 C37 C36 -166.79(15) . . . . ? C42 Fe2 C37 C36 -125.77(16) . . . . ? C39 Fe2 C37 C36 164.2(3) . . . . ? C34 Fe2 C37 C36 81.52(15) . . . . ? C33 Fe2 C37 C36 119.5(2) . . . . ? C41 Fe2 C37 C36 -84.23(17) . . . . ? C35 Fe2 C37 C36 37.36(14) . . . . ? C40 Fe2 C37 C36 -54.4(3) . . . . ? C38 Fe2 C37 C33 73.68(17) . . . . ? C42 Fe2 C37 C33 114.69(15) . . . . ? C39 Fe2 C37 C33 44.7(4) . . . . ? C36 Fe2 C37 C33 -119.5(2) . . . . ? C34 Fe2 C37 C33 -38.01(13) . . . . ? C41 Fe2 C37 C33 156.24(14) . . . . ? C35 Fe2 C37 C33 -82.18(14) . . . . ? C40 Fe2 C37 C33 -173.9(2) . . . . ? C39 Fe2 C38 C42 -118.0(2) . . . . ? C36 Fe2 C38 C42 45.9(4) . . . . ? C34 Fe2 C38 C42 158.07(15) . . . . ? C37 Fe2 C38 C42 75.22(18) . . . . ? C33 Fe2 C38 C42 116.15(16) . . . . ? C41 Fe2 C38 C42 -37.13(16) . . . . ? C35 Fe2 C38 C42 -170.3(2) . . . . ? C40 Fe2 C38 C42 -79.92(17) . . . . ? C42 Fe2 C38 C39 118.0(2) . . . . ? C36 Fe2 C38 C39 163.9(3) . . . . ? C34 Fe2 C38 C39 -83.91(19) . . . . ? C37 Fe2 C38 C39 -166.76(16) . . . . ? C33 Fe2 C38 C39 -125.83(17) . . . . ? C41 Fe2 C38 C39 80.89(18) . . . . ? C35 Fe2 C38 C39 -52.3(3) . . . . ? C40 Fe2 C38 C39 38.10(18) . . . . ? C42 C38 C39 C40 -0.1(3) . . . . ? Fe2 C38 C39 C40 -60.27(18) . . . . ? C42 C38 C39 Fe2 60.17(17) . . . . ? C38 Fe2 C39 C40 118.2(2) . . . . ? C42 Fe2 C39 C40 79.94(19) . . . . ? C36 Fe2 C39 C40 -49.8(3) . . . . ? C34 Fe2 C39 C40 -127.61(17) . . . . ? C37 Fe2 C39 C40 156.1(3) . . . . ? C33 Fe2 C39 C40 -169.59(16) . . . . ? C41 Fe2 C39 C40 36.48(17) . . . . ? C35 Fe2 C39 C40 -84.61(19) . . . . ? C42 Fe2 C39 C38 -38.25(16) . . . . ? C36 Fe2 C39 C38 -168.0(2) . . . . ? C34 Fe2 C39 C38 114.20(16) . . . . ? C37 Fe2 C39 C38 37.9(4) . . . . ? C33 Fe2 C39 C38 72.22(19) . . . . ? C41 Fe2 C39 C38 -81.71(18) . . . . ? C35 Fe2 C39 C38 157.20(15) . . . . ? C40 Fe2 C39 C38 -118.2(2) . . . . ? C38 C39 C40 C41 0.6(3) . . . . ? Fe2 C39 C40 C41 -59.07(18) . . . . ? C38 C39 C40 Fe2 59.66(18) . . . . ? C38 Fe2 C40 C41 81.80(18) . . . . ? C42 Fe2 C40 C41 37.77(16) . . . . ? C39 Fe2 C40 C41 120.2(2) . . . . ? C36 Fe2 C40 C41 -81.26(19) . . . . ? C34 Fe2 C40 C41 -167.50(15) . . . . ? C37 Fe2 C40 C41 -42.5(3) . . . . ? C33 Fe2 C40 C41 151.6(3) . . . . ? C35 Fe2 C40 C41 -124.65(17) . . . . ? C38 Fe2 C40 C39 -38.39(17) . . . . ? C42 Fe2 C40 C39 -82.43(19) . . . . ? C36 Fe2 C40 C39 158.54(17) . . . . ? C34 Fe2 C40 C39 72.3(2) . . . . ? C37 Fe2 C40 C39 -162.7(2) . . . . ? C33 Fe2 C40 C39 31.4(4) . . . . ? C41 Fe2 C40 C39 -120.2(2) . . . . ? C35 Fe2 C40 C39 115.16(18) . . . . ? C39 C40 C41 C42 -0.9(3) . . . . ? Fe2 C40 C41 C42 -59.53(17) . . . . ? C39 C40 C41 Fe2 58.67(19) . . . . ? C38 Fe2 C41 C40 -81.44(18) . . . . ? C42 Fe2 C41 C40 -118.9(2) . . . . ? C39 Fe2 C41 C40 -37.28(17) . . . . ? C36 Fe2 C41 C40 117.27(17) . . . . ? C34 Fe2 C41 C40 39.8(5) . . . . ? C37 Fe2 C41 C40 160.78(15) . . . . ? C33 Fe2 C41 C40 -162.1(2) . . . . ? C35 Fe2 C41 C40 76.0(2) . . . . ? C38 Fe2 C41 C42 37.51(17) . . . . ? C39 Fe2 C41 C42 81.66(18) . . . . ? C36 Fe2 C41 C42 -123.78(17) . . . . ? C34 Fe2 C41 C42 158.8(4) . . . . ? C37 Fe2 C41 C42 -80.28(18) . . . . ? C33 Fe2 C41 C42 -43.1(3) . . . . ? C35 Fe2 C41 C42 -165.02(17) . . . . ? C40 Fe2 C41 C42 118.9(2) . . . . ? C40 C41 C42 C38 0.8(3) . . . . ? Fe2 C41 C42 C38 -59.38(17) . . . . ? C40 C41 C42 Fe2 60.17(18) . . . . ? C39 C38 C42 C41 -0.4(3) . . . . ? Fe2 C38 C42 C41 59.86(17) . . . . ? C39 C38 C42 Fe2 -60.28(17) . . . . ? C38 Fe2 C42 C41 -119.6(2) . . . . ? C39 Fe2 C42 C41 -81.19(19) . . . . ? C36 Fe2 C42 C41 76.08(19) . . . . ? C34 Fe2 C42 C41 -167.3(2) . . . . ? C37 Fe2 C42 C41 117.04(16) . . . . ? C33 Fe2 C42 C41 159.99(15) . . . . ? C35 Fe2 C42 C41 46.1(4) . . . . ? C40 Fe2 C42 C41 -37.25(17) . . . . ? C39 Fe2 C42 C38 38.46(16) . . . . ? C36 Fe2 C42 C38 -164.28(15) . . . . ? C34 Fe2 C42 C38 -47.7(3) . . . . ? C37 Fe2 C42 C38 -123.31(16) . . . . ? C33 Fe2 C42 C38 -80.36(17) . . . . ? C41 Fe2 C42 C38 119.6(2) . . . . ? C35 Fe2 C42 C38 165.7(4) . . . . ? C40 Fe2 C42 C38 82.40(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.347 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 950018' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm001 #TrackingRef 'rm001.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29 B Fe N2' _chemical_formula_weight 400.14 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.8211(18) _cell_length_b 14.6473(9) _cell_length_c 11.4189(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.981(13) _cell_angle_gamma 90.00 _cell_volume 2143.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5384 _cell_measurement_theta_min 2.9131 _cell_measurement_theta_max 32.3712 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_T_min 0.7989 _exptl_absorpt_correction_T_max 0.8648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16576 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3770 _reflns_number_gt 3098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.1576P)^2^+6.2648P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3770 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.2992 _refine_ls_wR_factor_gt 0.2878 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.95109(7) 0.17837(6) 0.23538(8) 0.0481(4) Uani 1 1 d . . . B1 B 0.4179(5) -0.0325(5) -0.4370(6) 0.0448(15) Uani 1 1 d . . . N1 N 0.6059(3) 0.0152(3) -0.4191(4) 0.0391(10) Uani 1 1 d . . . N2 N 0.5355(4) -0.0008(3) -0.3654(4) 0.0421(11) Uani 1 1 d . . . C1 C 0.6990(4) 0.0295(4) -0.3248(5) 0.0458(14) Uani 1 1 d . . . H1 H 0.7609 0.0424 -0.3360 0.055 Uiso 1 1 calc R . . C2 C 0.6890(5) 0.0224(4) -0.2096(5) 0.0455(14) Uani 1 1 d . . . C3 C 0.5847(5) 0.0030(4) -0.2405(5) 0.0484(14) Uani 1 1 d . . . H3 H 0.5531 -0.0060 -0.1824 0.058 Uiso 1 1 calc R . . C4 C 0.7666(5) 0.0335(4) -0.0859(6) 0.0499(14) Uani 1 1 d . . . C5 C 0.8308(5) 0.0443(5) 0.0176(6) 0.0506(14) Uani 1 1 d . . . C6 C 0.9058(5) 0.0564(4) 0.1435(6) 0.0512(15) Uani 1 1 d . . . C7 C 1.0154(6) 0.0706(5) 0.1779(7) 0.069(2) Uani 1 1 d . . . H7 H 1.0512 0.0731 0.1233 0.082 Uiso 1 1 calc R . . C8 C 1.0586(8) 0.0801(6) 0.3101(9) 0.091(3) Uani 1 1 d . . . H8 H 1.1287 0.0906 0.3578 0.109 Uiso 1 1 calc R . . C9 C 0.9823(10) 0.0714(6) 0.3573(7) 0.089(3) Uani 1 1 d . . . H9 H 0.9918 0.0739 0.4423 0.107 Uiso 1 1 calc R . . C10 C 0.8856(8) 0.0580(5) 0.2554(7) 0.073(2) Uani 1 1 d . . . H10 H 0.8207 0.0514 0.2615 0.087 Uiso 1 1 calc R . . C11 C 0.8756(8) 0.2796(6) 0.1153(8) 0.081(2) Uani 1 1 d . . . H11 H 0.8300 0.2711 0.0322 0.097 Uiso 1 1 calc R . . C12 C 0.9813(9) 0.2940(6) 0.1544(9) 0.085(3) Uani 1 1 d . . . H12 H 1.0197 0.2965 0.1028 0.102 Uiso 1 1 calc R . . C13 C 1.0201(12) 0.3041(7) 0.2842(11) 0.107(4) Uani 1 1 d . . . H13 H 1.0895 0.3152 0.3346 0.128 Uiso 1 1 calc R . . C14 C 0.9402(15) 0.2952(7) 0.3266(10) 0.112(5) Uani 1 1 d . . . H14 H 0.9455 0.2985 0.4102 0.134 Uiso 1 1 calc R . . C15 C 0.8483(9) 0.2800(7) 0.2200(13) 0.105(4) Uani 1 1 d . . . H15 H 0.7816 0.2717 0.2201 0.125 Uiso 1 1 calc R . . C16 C 0.4093(5) -0.1407(5) -0.4143(6) 0.0580(17) Uani 1 1 d . . . H16A H 0.4365 -0.1514 -0.3239 0.070 Uiso 1 1 calc R . . H16B H 0.3359 -0.1567 -0.4460 0.070 Uiso 1 1 calc R . . C17 C 0.4629(8) -0.2053(5) -0.4714(8) 0.075(2) Uani 1 1 d . . . H17A H 0.5371 -0.1920 -0.4370 0.090 Uiso 1 1 calc R . . H17B H 0.4377 -0.1941 -0.5617 0.090 Uiso 1 1 calc R . . C18 C 0.4478(13) -0.3053(6) -0.4501(10) 0.120(5) Uani 1 1 d . . . H18A H 0.4817 -0.3178 -0.3605 0.143 Uiso 1 1 calc R . . H18B H 0.3737 -0.3161 -0.4728 0.143 Uiso 1 1 calc R . . C19 C 0.485(2) -0.3684(9) -0.5160(15) 0.219(12) Uani 1 1 d . . . H19A H 0.4329 -0.3782 -0.5986 0.328 Uiso 1 1 calc R . . H19B H 0.5006 -0.4251 -0.4707 0.328 Uiso 1 1 calc R . . H19C H 0.5473 -0.3448 -0.5236 0.328 Uiso 1 1 calc R . . C20 C 0.3406(5) 0.0249(5) -0.3905(6) 0.0571(17) Uani 1 1 d . . . H20A H 0.2706 0.0022 -0.4360 0.069 Uiso 1 1 calc R . . H20B H 0.3578 0.0106 -0.3020 0.069 Uiso 1 1 calc R . . C21 C 0.3367(6) 0.1279(6) -0.4028(8) 0.071(2) Uani 1 1 d . . . H21A H 0.3168 0.1434 -0.4914 0.086 Uiso 1 1 calc R . . H21B H 0.4063 0.1518 -0.3583 0.086 Uiso 1 1 calc R . . C22 C 0.2621(8) 0.1756(8) -0.3527(12) 0.105(4) Uani 1 1 d . . . H22A H 0.1919 0.1540 -0.4000 0.126 Uiso 1 1 calc R . . H22B H 0.2799 0.1579 -0.2653 0.126 Uiso 1 1 calc R . . C23 C 0.2622(10) 0.2778(9) -0.3597(15) 0.151(6) Uani 1 1 d . . . H23A H 0.3277 0.3008 -0.3019 0.227 Uiso 1 1 calc R . . H23B H 0.2066 0.3017 -0.3375 0.227 Uiso 1 1 calc R . . H23C H 0.2523 0.2964 -0.4440 0.227 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0512(6) 0.0509(6) 0.0343(6) -0.0004(3) 0.0069(4) 0.0074(4) B1 0.037(3) 0.054(4) 0.038(3) -0.007(3) 0.007(3) -0.012(3) N1 0.031(2) 0.045(3) 0.038(2) -0.0036(19) 0.0095(18) -0.0078(18) N2 0.041(3) 0.048(3) 0.034(2) -0.0055(19) 0.011(2) -0.007(2) C1 0.033(3) 0.052(3) 0.044(3) -0.004(2) 0.004(2) -0.004(2) C2 0.044(3) 0.041(3) 0.039(3) -0.006(2) 0.001(2) 0.000(2) C3 0.049(3) 0.062(4) 0.030(3) -0.005(2) 0.011(2) -0.003(3) C4 0.045(3) 0.052(4) 0.045(3) -0.004(3) 0.007(3) 0.000(3) C5 0.048(3) 0.055(4) 0.040(3) -0.003(3) 0.007(3) -0.001(3) C6 0.058(4) 0.047(3) 0.037(3) -0.002(2) 0.005(3) 0.005(3) C7 0.056(4) 0.075(5) 0.058(4) -0.022(4) 0.001(3) 0.017(4) C8 0.086(6) 0.073(6) 0.066(5) -0.017(4) -0.027(5) 0.032(5) C9 0.144(9) 0.063(5) 0.032(4) 0.005(3) -0.001(5) 0.005(5) C10 0.107(6) 0.056(4) 0.048(4) 0.002(3) 0.022(4) -0.011(4) C11 0.095(6) 0.073(5) 0.064(5) 0.020(4) 0.018(5) 0.031(5) C12 0.113(8) 0.072(5) 0.074(6) 0.017(4) 0.038(5) 0.000(5) C13 0.147(10) 0.060(5) 0.080(7) -0.005(5) 0.003(7) -0.023(6) C14 0.226(16) 0.062(5) 0.062(6) -0.001(4) 0.070(8) 0.017(7) C15 0.112(8) 0.074(6) 0.150(11) 0.019(6) 0.074(8) 0.040(6) C16 0.059(4) 0.063(4) 0.044(3) 0.003(3) 0.011(3) -0.021(3) C17 0.106(6) 0.052(4) 0.062(5) -0.001(3) 0.027(4) -0.005(4) C18 0.213(15) 0.049(5) 0.086(7) 0.008(4) 0.044(8) -0.005(6) C19 0.49(4) 0.062(7) 0.149(13) 0.001(7) 0.173(19) 0.039(13) C20 0.045(3) 0.086(5) 0.038(3) -0.008(3) 0.013(3) -0.008(3) C21 0.052(4) 0.083(5) 0.072(5) -0.021(4) 0.014(3) 0.000(4) C22 0.069(6) 0.114(9) 0.125(9) -0.050(6) 0.029(6) 0.004(5) C23 0.106(9) 0.105(10) 0.216(16) -0.066(10) 0.029(9) 0.020(7) _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 C8 2.015(8) . ? Fe1 C15 2.019(9) . ? Fe1 C11 2.024(7) . ? Fe1 C9 2.032(8) . ? Fe1 C10 2.034(8) . ? Fe1 C7 2.037(7) . ? Fe1 C14 2.038(9) . ? Fe1 C12 2.047(9) . ? Fe1 C6 2.047(6) . ? Fe1 C13 2.053(10) . ? B1 N1 1.571(8) 3_654 ? B1 N2 1.591(7) . ? B1 C20 1.598(10) . ? B1 C16 1.619(10) . ? N1 C1 1.350(7) . ? N1 N2 1.350(6) . ? N1 B1 1.571(8) 3_654 ? N2 C3 1.332(7) . ? C1 C2 1.377(8) . ? C1 H1 0.9300 . ? C2 C3 1.380(9) . ? C2 C4 1.428(8) . ? C3 H3 0.9300 . ? C4 C5 1.193(8) . ? C5 C6 1.434(8) . ? C6 C10 1.407(10) . ? C6 C7 1.430(10) . ? C7 C8 1.407(12) . ? C7 H7 0.9300 . ? C8 C9 1.358(15) . ? C8 H8 0.9300 . ? C9 C10 1.419(13) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.374(14) . ? C11 C15 1.382(13) . ? C11 H11 0.9300 . ? C12 C13 1.383(14) . ? C12 H12 0.9300 . ? C13 C14 1.369(19) . ? C13 H13 0.9300 . ? C14 C15 1.410(17) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.494(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.513(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.406(18) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.514(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.524(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.499(17) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 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 C8 Fe1 C15 161.2(5) . . ? C8 Fe1 C11 157.2(5) . . ? C15 Fe1 C11 40.0(4) . . ? C8 Fe1 C9 39.2(4) . . ? C15 Fe1 C9 126.1(5) . . ? C11 Fe1 C9 162.2(5) . . ? C8 Fe1 C10 67.8(4) . . ? C15 Fe1 C10 108.7(5) . . ? C11 Fe1 C10 125.0(4) . . ? C9 Fe1 C10 40.9(4) . . ? C8 Fe1 C7 40.6(3) . . ? C15 Fe1 C7 157.0(5) . . ? C11 Fe1 C7 121.7(4) . . ? C9 Fe1 C7 67.5(4) . . ? C10 Fe1 C7 68.3(4) . . ? C8 Fe1 C14 124.6(5) . . ? C15 Fe1 C14 40.7(5) . . ? C11 Fe1 C14 67.2(4) . . ? C9 Fe1 C14 109.5(4) . . ? C10 Fe1 C14 123.3(5) . . ? C7 Fe1 C14 160.1(6) . . ? C8 Fe1 C12 122.7(5) . . ? C15 Fe1 C12 66.8(4) . . ? C11 Fe1 C12 39.5(4) . . ? C9 Fe1 C12 157.1(5) . . ? C10 Fe1 C12 160.6(4) . . ? C7 Fe1 C12 108.0(4) . . ? C14 Fe1 C12 66.6(5) . . ? C8 Fe1 C6 68.2(3) . . ? C15 Fe1 C6 121.9(4) . . ? C11 Fe1 C6 108.1(3) . . ? C9 Fe1 C6 67.9(3) . . ? C10 Fe1 C6 40.3(3) . . ? C7 Fe1 C6 41.0(3) . . ? C14 Fe1 C6 158.1(6) . . ? C12 Fe1 C6 124.4(3) . . ? C8 Fe1 C13 109.4(5) . . ? C15 Fe1 C13 66.6(6) . . ? C11 Fe1 C13 66.2(4) . . ? C9 Fe1 C13 123.2(4) . . ? C10 Fe1 C13 158.2(4) . . ? C7 Fe1 C13 124.6(5) . . ? C14 Fe1 C13 39.1(5) . . ? C12 Fe1 C13 39.4(4) . . ? C6 Fe1 C13 160.7(5) . . ? N1 B1 N2 105.3(4) 3_654 . ? N1 B1 C20 111.0(5) 3_654 . ? N2 B1 C20 111.0(5) . . ? N1 B1 C16 109.1(5) 3_654 . ? N2 B1 C16 109.0(5) . . ? C20 B1 C16 111.3(5) . . ? C1 N1 N2 107.4(4) . . ? C1 N1 B1 124.9(5) . 3_654 ? N2 N1 B1 126.8(4) . 3_654 ? C3 N2 N1 108.2(5) . . ? C3 N2 B1 125.2(5) . . ? N1 N2 B1 126.1(4) . . ? N1 C1 C2 110.1(5) . . ? N1 C1 H1 125.0 . . ? C2 C1 H1 125.0 . . ? C1 C2 C3 103.9(5) . . ? C1 C2 C4 129.1(6) . . ? C3 C2 C4 127.0(6) . . ? N2 C3 C2 110.4(5) . . ? N2 C3 H3 124.8 . . ? C2 C3 H3 124.8 . . ? C5 C4 C2 178.9(7) . . ? C4 C5 C6 178.3(7) . . ? C10 C6 C7 107.4(6) . . ? C10 C6 C5 126.7(7) . . ? C7 C6 C5 125.9(6) . . ? C10 C6 Fe1 69.3(4) . . ? C7 C6 Fe1 69.1(4) . . ? C5 C6 Fe1 126.1(5) . . ? C8 C7 C6 106.8(8) . . ? C8 C7 Fe1 68.8(4) . . ? C6 C7 Fe1 69.9(4) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? Fe1 C7 H7 126.2 . . ? C9 C8 C7 109.6(8) . . ? C9 C8 Fe1 71.1(5) . . ? C7 C8 Fe1 70.5(4) . . ? C9 C8 H8 125.2 . . ? C7 C8 H8 125.2 . . ? Fe1 C8 H8 124.8 . . ? C8 C9 C10 108.7(7) . . ? C8 C9 Fe1 69.7(5) . . ? C10 C9 Fe1 69.7(4) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe1 C9 H9 126.6 . . ? C6 C10 C9 107.5(9) . . ? C6 C10 Fe1 70.3(4) . . ? C9 C10 Fe1 69.5(5) . . ? C6 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Fe1 C10 H10 125.5 . . ? C12 C11 C15 108.6(9) . . ? C12 C11 Fe1 71.1(5) . . ? C15 C11 Fe1 69.8(5) . . ? C12 C11 H11 125.7 . . ? C15 C11 H11 125.7 . . ? Fe1 C11 H11 124.9 . . ? C11 C12 C13 107.7(10) . . ? C11 C12 Fe1 69.4(5) . . ? C13 C12 Fe1 70.6(6) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? Fe1 C12 H12 125.5 . . ? C14 C13 C12 109.2(11) . . ? C14 C13 Fe1 69.9(6) . . ? C12 C13 Fe1 70.0(5) . . ? C14 C13 H13 125.4 . . ? C12 C13 H13 125.4 . . ? Fe1 C13 H13 126.3 . . ? C13 C14 C15 107.2(9) . . ? C13 C14 Fe1 71.1(6) . . ? C15 C14 Fe1 69.0(5) . . ? C13 C14 H14 126.4 . . ? C15 C14 H14 126.4 . . ? Fe1 C14 H14 125.2 . . ? C11 C15 C14 107.4(10) . . ? C11 C15 Fe1 70.2(5) . . ? C14 C15 Fe1 70.4(6) . . ? C11 C15 H15 126.3 . . ? C14 C15 H15 126.3 . . ? Fe1 C15 H15 124.7 . . ? C17 C16 B1 118.2(6) . . ? C17 C16 H16A 107.8 . . ? B1 C16 H16A 107.8 . . ? C17 C16 H16B 107.8 . . ? B1 C16 H16B 107.8 . . ? H16A C16 H16B 107.1 . . ? C16 C17 C18 114.9(8) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 116.7(12) . . ? C19 C18 H18A 108.1 . . ? C17 C18 H18A 108.1 . . ? C19 C18 H18B 108.1 . . ? C17 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? 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 . . ? C21 C20 B1 119.9(6) . . ? C21 C20 H20A 107.4 . . ? B1 C20 H20A 107.4 . . ? C21 C20 H20B 107.4 . . ? B1 C20 H20B 107.4 . . ? H20A C20 H20B 106.9 . . ? C20 C21 C22 115.3(8) . . ? C20 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? C20 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C21 115.1(11) . . ? C23 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 C1 N1 N2 C3 -0.4(6) . . . . ? B1 N1 N2 C3 -169.9(5) 3_654 . . . ? C1 N1 N2 B1 -172.6(5) . . . . ? B1 N1 N2 B1 17.9(10) 3_654 . . . ? N1 B1 N2 C3 174.3(5) 3_654 . . . ? C20 B1 N2 C3 54.1(8) . . . . ? C16 B1 N2 C3 -68.9(7) . . . . ? N1 B1 N2 N1 -14.8(8) 3_654 . . . ? C20 B1 N2 N1 -135.0(6) . . . . ? C16 B1 N2 N1 102.1(6) . . . . ? N2 N1 C1 C2 0.3(6) . . . . ? B1 N1 C1 C2 170.0(5) 3_654 . . . ? N1 C1 C2 C3 -0.1(7) . . . . ? N1 C1 C2 C4 -179.1(6) . . . . ? N1 N2 C3 C2 0.4(7) . . . . ? B1 N2 C3 C2 172.7(5) . . . . ? C1 C2 C3 N2 -0.2(7) . . . . ? C4 C2 C3 N2 178.9(6) . . . . ? C1 C2 C4 C5 98(38) . . . . ? C3 C2 C4 C5 -81(38) . . . . ? C2 C4 C5 C6 89(47) . . . . ? C4 C5 C6 C10 -14(25) . . . . ? C4 C5 C6 C7 167(24) . . . . ? C4 C5 C6 Fe1 -104(24) . . . . ? C8 Fe1 C6 C10 80.9(6) . . . . ? C15 Fe1 C6 C10 -81.4(6) . . . . ? C11 Fe1 C6 C10 -123.1(5) . . . . ? C9 Fe1 C6 C10 38.4(6) . . . . ? C7 Fe1 C6 C10 119.0(7) . . . . ? C14 Fe1 C6 C10 -49.2(10) . . . . ? C12 Fe1 C6 C10 -163.6(6) . . . . ? C13 Fe1 C6 C10 167.5(12) . . . . ? C8 Fe1 C6 C7 -38.2(6) . . . . ? C15 Fe1 C6 C7 159.6(6) . . . . ? C11 Fe1 C6 C7 117.8(5) . . . . ? C9 Fe1 C6 C7 -80.6(6) . . . . ? C10 Fe1 C6 C7 -119.0(7) . . . . ? C14 Fe1 C6 C7 -168.2(9) . . . . ? C12 Fe1 C6 C7 77.4(6) . . . . ? C13 Fe1 C6 C7 48.5(13) . . . . ? C8 Fe1 C6 C5 -158.1(8) . . . . ? C15 Fe1 C6 C5 39.7(8) . . . . ? C11 Fe1 C6 C5 -2.1(7) . . . . ? C9 Fe1 C6 C5 159.5(8) . . . . ? C10 Fe1 C6 C5 121.1(8) . . . . ? C7 Fe1 C6 C5 -119.9(8) . . . . ? C14 Fe1 C6 C5 71.9(11) . . . . ? C12 Fe1 C6 C5 -42.5(8) . . . . ? C13 Fe1 C6 C5 -71.4(14) . . . . ? C10 C6 C7 C8 0.2(8) . . . . ? C5 C6 C7 C8 179.3(7) . . . . ? Fe1 C6 C7 C8 59.2(5) . . . . ? C10 C6 C7 Fe1 -59.0(5) . . . . ? C5 C6 C7 Fe1 120.2(7) . . . . ? C15 Fe1 C7 C8 -167.6(11) . . . . ? C11 Fe1 C7 C8 160.7(7) . . . . ? C9 Fe1 C7 C8 -36.4(6) . . . . ? C10 Fe1 C7 C8 -80.7(7) . . . . ? C14 Fe1 C7 C8 48.9(14) . . . . ? C12 Fe1 C7 C8 119.6(7) . . . . ? C6 Fe1 C7 C8 -118.2(8) . . . . ? C13 Fe1 C7 C8 79.3(8) . . . . ? C8 Fe1 C7 C6 118.2(8) . . . . ? C15 Fe1 C7 C6 -49.4(13) . . . . ? C11 Fe1 C7 C6 -81.1(6) . . . . ? C9 Fe1 C7 C6 81.8(5) . . . . ? C10 Fe1 C7 C6 37.5(4) . . . . ? C14 Fe1 C7 C6 167.1(10) . . . . ? C12 Fe1 C7 C6 -122.2(5) . . . . ? C13 Fe1 C7 C6 -162.5(5) . . . . ? C6 C7 C8 C9 0.7(9) . . . . ? Fe1 C7 C8 C9 60.6(6) . . . . ? C6 C7 C8 Fe1 -59.8(5) . . . . ? C15 Fe1 C8 C9 45.0(17) . . . . ? C11 Fe1 C8 C9 -166.4(9) . . . . ? C10 Fe1 C8 C9 -37.7(5) . . . . ? C7 Fe1 C8 C9 -119.9(8) . . . . ? C14 Fe1 C8 C9 78.3(8) . . . . ? C12 Fe1 C8 C9 160.8(5) . . . . ? C6 Fe1 C8 C9 -81.3(5) . . . . ? C13 Fe1 C8 C9 119.1(7) . . . . ? C15 Fe1 C8 C7 164.9(13) . . . . ? C11 Fe1 C8 C7 -46.5(13) . . . . ? C9 Fe1 C8 C7 119.9(8) . . . . ? C10 Fe1 C8 C7 82.2(6) . . . . ? C14 Fe1 C8 C7 -161.8(7) . . . . ? C12 Fe1 C8 C7 -79.3(7) . . . . ? C6 Fe1 C8 C7 38.5(5) . . . . ? C13 Fe1 C8 C7 -121.0(7) . . . . ? C7 C8 C9 C10 -1.3(10) . . . . ? Fe1 C8 C9 C10 58.9(6) . . . . ? C7 C8 C9 Fe1 -60.2(6) . . . . ? C15 Fe1 C9 C8 -163.6(6) . . . . ? C11 Fe1 C9 C8 162.6(11) . . . . ? C10 Fe1 C9 C8 120.1(8) . . . . ? C7 Fe1 C9 C8 37.7(5) . . . . ? C14 Fe1 C9 C8 -121.2(7) . . . . ? C12 Fe1 C9 C8 -45.3(12) . . . . ? C6 Fe1 C9 C8 82.2(5) . . . . ? C13 Fe1 C9 C8 -80.0(8) . . . . ? C8 Fe1 C9 C10 -120.1(8) . . . . ? C15 Fe1 C9 C10 76.3(8) . . . . ? C11 Fe1 C9 C10 42.5(14) . . . . ? C7 Fe1 C9 C10 -82.4(6) . . . . ? C14 Fe1 C9 C10 118.7(7) . . . . ? C12 Fe1 C9 C10 -165.4(9) . . . . ? C6 Fe1 C9 C10 -37.9(5) . . . . ? C13 Fe1 C9 C10 159.9(7) . . . . ? C7 C6 C10 C9 -0.9(9) . . . . ? C5 C6 C10 C9 179.9(7) . . . . ? Fe1 C6 C10 C9 -59.8(5) . . . . ? C7 C6 C10 Fe1 58.9(5) . . . . ? C5 C6 C10 Fe1 -120.3(7) . . . . ? C8 C9 C10 C6 1.4(10) . . . . ? Fe1 C9 C10 C6 60.3(5) . . . . ? C8 C9 C10 Fe1 -58.9(6) . . . . ? C8 Fe1 C10 C6 -82.1(5) . . . . ? C15 Fe1 C10 C6 117.6(6) . . . . ? C11 Fe1 C10 C6 76.3(6) . . . . ? C9 Fe1 C10 C6 -118.3(8) . . . . ? C7 Fe1 C10 C6 -38.1(4) . . . . ? C14 Fe1 C10 C6 160.2(6) . . . . ? C12 Fe1 C10 C6 44.5(14) . . . . ? C13 Fe1 C10 C6 -168.9(12) . . . . ? C8 Fe1 C10 C9 36.2(6) . . . . ? C15 Fe1 C10 C9 -124.1(7) . . . . ? C11 Fe1 C10 C9 -165.4(6) . . . . ? C7 Fe1 C10 C9 80.2(7) . . . . ? C14 Fe1 C10 C9 -81.5(8) . . . . ? C12 Fe1 C10 C9 162.8(12) . . . . ? C6 Fe1 C10 C9 118.3(8) . . . . ? C13 Fe1 C10 C9 -50.6(15) . . . . ? C8 Fe1 C11 C12 -45.8(12) . . . . ? C15 Fe1 C11 C12 119.0(10) . . . . ? C9 Fe1 C11 C12 163.4(10) . . . . ? C10 Fe1 C11 C12 -164.0(6) . . . . ? C7 Fe1 C11 C12 -79.6(7) . . . . ? C14 Fe1 C11 C12 80.3(8) . . . . ? C6 Fe1 C11 C12 -122.6(6) . . . . ? C13 Fe1 C11 C12 37.6(7) . . . . ? C8 Fe1 C11 C15 -164.9(10) . . . . ? C9 Fe1 C11 C15 44.3(15) . . . . ? C10 Fe1 C11 C15 77.0(8) . . . . ? C7 Fe1 C11 C15 161.4(7) . . . . ? C14 Fe1 C11 C15 -38.7(8) . . . . ? C12 Fe1 C11 C15 -119.0(10) . . . . ? C6 Fe1 C11 C15 118.4(7) . . . . ? C13 Fe1 C11 C15 -81.4(8) . . . . ? C15 C11 C12 C13 -0.5(11) . . . . ? Fe1 C11 C12 C13 -60.5(7) . . . . ? C15 C11 C12 Fe1 60.0(6) . . . . ? C8 Fe1 C12 C11 160.7(6) . . . . ? C15 Fe1 C12 C11 -37.7(6) . . . . ? C9 Fe1 C12 C11 -167.0(10) . . . . ? C10 Fe1 C12 C11 42.8(15) . . . . ? C7 Fe1 C12 C11 118.4(6) . . . . ? C14 Fe1 C12 C11 -82.1(8) . . . . ? C6 Fe1 C12 C11 76.1(7) . . . . ? C13 Fe1 C12 C11 -118.5(10) . . . . ? C8 Fe1 C12 C13 -80.8(9) . . . . ? C15 Fe1 C12 C13 80.8(9) . . . . ? C11 Fe1 C12 C13 118.5(10) . . . . ? C9 Fe1 C12 C13 -48.6(14) . . . . ? C10 Fe1 C12 C13 161.2(12) . . . . ? C7 Fe1 C12 C13 -123.1(8) . . . . ? C14 Fe1 C12 C13 36.4(8) . . . . ? C6 Fe1 C12 C13 -165.4(8) . . . . ? C11 C12 C13 C14 0.7(12) . . . . ? Fe1 C12 C13 C14 -59.0(8) . . . . ? C11 C12 C13 Fe1 59.7(7) . . . . ? C8 Fe1 C13 C14 -121.4(8) . . . . ? C15 Fe1 C13 C14 38.9(7) . . . . ? C11 Fe1 C13 C14 82.7(8) . . . . ? C9 Fe1 C13 C14 -80.1(9) . . . . ? C10 Fe1 C13 C14 -42.9(16) . . . . ? C7 Fe1 C13 C14 -164.1(7) . . . . ? C12 Fe1 C13 C14 120.4(11) . . . . ? C6 Fe1 C13 C14 159.3(10) . . . . ? C8 Fe1 C13 C12 118.3(7) . . . . ? C15 Fe1 C13 C12 -81.5(8) . . . . ? C11 Fe1 C13 C12 -37.7(6) . . . . ? C9 Fe1 C13 C12 159.6(7) . . . . ? C10 Fe1 C13 C12 -163.3(10) . . . . ? C7 Fe1 C13 C12 75.5(8) . . . . ? C14 Fe1 C13 C12 -120.4(11) . . . . ? C6 Fe1 C13 C12 38.9(16) . . . . ? C12 C13 C14 C15 -0.6(12) . . . . ? Fe1 C13 C14 C15 -59.8(7) . . . . ? C12 C13 C14 Fe1 59.2(7) . . . . ? C8 Fe1 C14 C13 78.0(8) . . . . ? C15 Fe1 C14 C13 -117.8(9) . . . . ? C11 Fe1 C14 C13 -79.7(7) . . . . ? C9 Fe1 C14 C13 119.0(7) . . . . ? C10 Fe1 C14 C13 162.4(6) . . . . ? C7 Fe1 C14 C13 41.4(14) . . . . ? C12 Fe1 C14 C13 -36.7(6) . . . . ? C6 Fe1 C14 C13 -161.7(8) . . . . ? C8 Fe1 C14 C15 -164.3(7) . . . . ? C11 Fe1 C14 C15 38.1(6) . . . . ? C9 Fe1 C14 C15 -123.2(7) . . . . ? C10 Fe1 C14 C15 -79.8(7) . . . . ? C7 Fe1 C14 C15 159.2(10) . . . . ? C12 Fe1 C14 C15 81.1(7) . . . . ? C6 Fe1 C14 C15 -43.9(12) . . . . ? C13 Fe1 C14 C15 117.8(9) . . . . ? C12 C11 C15 C14 0.1(11) . . . . ? Fe1 C11 C15 C14 60.9(7) . . . . ? C12 C11 C15 Fe1 -60.8(7) . . . . ? C13 C14 C15 C11 0.3(11) . . . . ? Fe1 C14 C15 C11 -60.8(6) . . . . ? C13 C14 C15 Fe1 61.1(7) . . . . ? C8 Fe1 C15 C11 161.7(13) . . . . ? C9 Fe1 C15 C11 -164.7(6) . . . . ? C10 Fe1 C15 C11 -122.6(6) . . . . ? C7 Fe1 C15 C11 -44.2(14) . . . . ? C14 Fe1 C15 C11 117.7(10) . . . . ? C12 Fe1 C15 C11 37.2(6) . . . . ? C6 Fe1 C15 C11 -80.1(7) . . . . ? C13 Fe1 C15 C11 80.3(7) . . . . ? C8 Fe1 C15 C14 44.0(18) . . . . ? C11 Fe1 C15 C14 -117.7(10) . . . . ? C9 Fe1 C15 C14 77.6(8) . . . . ? C10 Fe1 C15 C14 119.7(7) . . . . ? C7 Fe1 C15 C14 -161.9(10) . . . . ? C12 Fe1 C15 C14 -80.5(8) . . . . ? C6 Fe1 C15 C14 162.2(6) . . . . ? C13 Fe1 C15 C14 -37.4(6) . . . . ? N1 B1 C16 C17 47.3(8) 3_654 . . . ? N2 B1 C16 C17 -67.2(7) . . . . ? C20 B1 C16 C17 170.1(6) . . . . ? B1 C16 C17 C18 -177.8(8) . . . . ? C16 C17 C18 C19 171.8(14) . . . . ? N1 B1 C20 C21 -58.5(7) 3_654 . . . ? N2 B1 C20 C21 58.2(8) . . . . ? C16 B1 C20 C21 179.8(6) . . . . ? B1 C20 C21 C22 -178.7(7) . . . . ? C20 C21 C22 C23 177.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.171 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 891091' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rm006 #TrackingRef 'rm006.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H33 B Fe N2' _chemical_formula_weight 476.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.2196(6) _cell_length_b 13.2314(4) _cell_length_c 21.5639(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.074(4) _cell_angle_gamma 90.00 _cell_volume 4893.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4949 _cell_measurement_theta_min 2.8996 _cell_measurement_theta_max 32.4396 _exptl_crystal_description tiny-block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_T_min 0.9106 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Micro-Focus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION SUPER NOVA' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20852 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4300 _reflns_number_gt 3362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0496P)^2^+12.4718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4300 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.92406(3) 0.27344(3) 0.57770(2) 0.02475(15) Uani 1 1 d . . . B1 B 0.56998(19) -0.1691(3) 0.20662(15) 0.0206(7) Uani 1 1 d . . . N1 N 0.57779(13) -0.14651(17) 0.27965(11) 0.0183(5) Uani 1 1 d . . . N2 N 0.51750(13) -0.13741(17) 0.31553(11) 0.0187(5) Uani 1 1 d . . . C1 C 0.54615(18) -0.1161(2) 0.37372(13) 0.0223(6) Uani 1 1 d . . . H1 H 0.5166 -0.1065 0.4073 0.027 Uiso 1 1 calc R . . C2 C 0.62726(17) -0.1106(2) 0.37624(13) 0.0206(6) Uani 1 1 d . . . C3 C 0.64379(17) -0.1302(2) 0.31550(14) 0.0215(6) Uani 1 1 d . . . H3 H 0.6935 -0.1317 0.3018 0.026 Uiso 1 1 calc R . . C4 C 0.68182(18) -0.0912(2) 0.42880(14) 0.0242(7) Uani 1 1 d . . . C5 C 0.72961(18) -0.0754(2) 0.47138(14) 0.0245(7) Uani 1 1 d . . . C6 C 0.78797(17) -0.0580(2) 0.52242(14) 0.0244(7) Uani 1 1 d . . . C7 C 0.83111(18) -0.1391(2) 0.54934(15) 0.0276(7) Uani 1 1 d . . . H7 H 0.8222 -0.2044 0.5344 0.033 Uiso 1 1 calc R . . C8 C 0.88655(19) -0.1215(2) 0.59794(16) 0.0324(8) Uani 1 1 d . . . H8 H 0.9158 -0.1753 0.6152 0.039 Uiso 1 1 calc R . . C9 C 0.89969(18) -0.0256(2) 0.62167(15) 0.0295(7) Uani 1 1 d . . . H9 H 0.9371 -0.0158 0.6549 0.035 Uiso 1 1 calc R . . C10 C 0.85759(17) 0.0567(2) 0.59646(14) 0.0238(7) Uani 1 1 d . . . C11 C 0.80165(17) 0.0394(2) 0.54633(14) 0.0245(7) Uani 1 1 d . . . H11 H 0.7732 0.0934 0.5287 0.029 Uiso 1 1 calc R . . C12 C 0.87180(18) 0.1591(2) 0.62219(14) 0.0268(7) Uani 1 1 d . . . C13 C 0.9395(2) 0.1936(3) 0.65889(14) 0.0316(8) Uani 1 1 d . . . H13 H 0.9827 0.1545 0.6722 0.038 Uiso 1 1 calc R . . C14 C 0.9298(2) 0.2979(3) 0.67159(15) 0.0347(8) Uani 1 1 d . . . H14 H 0.9656 0.3386 0.6947 0.042 Uiso 1 1 calc R . . C15 C 0.8571(2) 0.3297(3) 0.64352(16) 0.0357(8) Uani 1 1 d . . . H15 H 0.8365 0.3946 0.6447 0.043 Uiso 1 1 calc R . . C16 C 0.8205(2) 0.2442(2) 0.61279(16) 0.0310(8) Uani 1 1 d . . . H16 H 0.7717 0.2437 0.5905 0.037 Uiso 1 1 calc R . . C17 C 1.0242(2) 0.2629(3) 0.53294(16) 0.0414(9) Uani 1 1 d . . . H17 H 1.0713 0.2342 0.5486 0.050 Uiso 1 1 calc R . . C18 C 1.0019(2) 0.3648(3) 0.53926(15) 0.0362(8) Uani 1 1 d . . . H18 H 1.0317 0.4148 0.5602 0.043 Uiso 1 1 calc R . . C19 C 0.9276(2) 0.3780(3) 0.50895(15) 0.0389(9) Uani 1 1 d . . . H19 H 0.8994 0.4380 0.5058 0.047 Uiso 1 1 calc R . . C20 C 0.9029(2) 0.2828(3) 0.48383(15) 0.0396(9) Uani 1 1 d . . . H20 H 0.8554 0.2693 0.4614 0.048 Uiso 1 1 calc R . . C21 C 0.9627(2) 0.2129(3) 0.49886(16) 0.0420(9) Uani 1 1 d . . . H21 H 0.9618 0.1448 0.4880 0.050 Uiso 1 1 calc R . . C22 C 0.57782(18) -0.2881(2) 0.19203(14) 0.0252(7) Uani 1 1 d . . . H22A H 0.5347 -0.3229 0.2089 0.030 Uiso 1 1 calc R . . H22B H 0.5718 -0.2971 0.1472 0.030 Uiso 1 1 calc R . . C23 C 0.6531(2) -0.3401(3) 0.21697(16) 0.0370(8) Uani 1 1 d . . . H23A H 0.6610 -0.3294 0.2616 0.044 Uiso 1 1 calc R . . H23B H 0.6965 -0.3090 0.1983 0.044 Uiso 1 1 calc R . . C24 C 0.6534(3) -0.4562(4) 0.2036(2) 0.0771(17) Uani 1 1 d . . . H24A H 0.7034 -0.4835 0.2199 0.093 Uiso 1 1 calc R . . H24B H 0.6137 -0.4877 0.2262 0.093 Uiso 1 1 calc R . . C25 C 0.6398(3) -0.4850(4) 0.1378(2) 0.0776(15) Uani 1 1 d . . . H25A H 0.5889 -0.4628 0.1217 0.116 Uiso 1 1 calc R . . H25B H 0.6431 -0.5572 0.1341 0.116 Uiso 1 1 calc R . . H25C H 0.6784 -0.4539 0.1146 0.116 Uiso 1 1 calc R . . C26 C 0.62940(17) -0.0950(2) 0.17494(13) 0.0227(7) Uani 1 1 d . . . H26A H 0.6822 -0.1158 0.1886 0.027 Uiso 1 1 calc R . . H26B H 0.6223 -0.1048 0.1302 0.027 Uiso 1 1 calc R . . C27 C 0.62217(18) 0.0180(2) 0.18809(14) 0.0257(7) Uani 1 1 d . . . H27A H 0.5689 0.0387 0.1762 0.031 Uiso 1 1 calc R . . H27B H 0.6322 0.0288 0.2326 0.031 Uiso 1 1 calc R . . C28 C 0.67677(18) 0.0853(2) 0.15468(15) 0.0307(7) Uani 1 1 d . . . H28A H 0.6661 0.0760 0.1101 0.037 Uiso 1 1 calc R . . H28B H 0.7301 0.0644 0.1660 0.037 Uiso 1 1 calc R . . C29 C 0.6687(2) 0.1972(3) 0.17003(18) 0.0382(8) Uani 1 1 d . . . H29A H 0.6158 0.2182 0.1597 0.057 Uiso 1 1 calc R . . H29B H 0.7027 0.2361 0.1464 0.057 Uiso 1 1 calc R . . H29C H 0.6825 0.2077 0.2137 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0263(3) 0.0247(3) 0.0230(3) -0.00242(18) 0.00061(19) -0.00431(19) B1 0.0175(16) 0.0244(18) 0.0188(17) -0.0023(13) -0.0043(14) 0.0043(14) N1 0.0168(12) 0.0173(12) 0.0204(13) -0.0008(9) -0.0006(10) 0.0013(10) N2 0.0178(12) 0.0192(13) 0.0189(12) -0.0005(9) -0.0002(11) -0.0005(10) C1 0.0255(16) 0.0225(16) 0.0182(15) -0.0026(12) -0.0013(13) -0.0004(13) C2 0.0219(15) 0.0169(14) 0.0219(15) 0.0000(12) -0.0037(13) -0.0006(12) C3 0.0177(14) 0.0194(15) 0.0266(16) 0.0010(12) -0.0020(13) 0.0004(12) C4 0.0272(16) 0.0188(15) 0.0261(17) -0.0010(12) -0.0001(15) -0.0003(13) C5 0.0261(16) 0.0213(16) 0.0260(17) -0.0033(12) 0.0009(15) -0.0005(13) C6 0.0221(15) 0.0283(17) 0.0220(16) -0.0033(12) -0.0017(13) -0.0037(13) C7 0.0263(17) 0.0221(17) 0.0338(18) -0.0029(13) -0.0008(15) 0.0009(13) C8 0.0302(18) 0.0274(18) 0.0376(19) -0.0002(14) -0.0086(16) 0.0057(14) C9 0.0262(17) 0.0351(19) 0.0253(17) 0.0016(14) -0.0081(14) -0.0048(14) C10 0.0229(15) 0.0246(16) 0.0241(16) -0.0015(12) 0.0030(14) -0.0049(13) C11 0.0256(16) 0.0218(16) 0.0257(16) 0.0018(12) 0.0004(14) -0.0016(13) C12 0.0282(17) 0.0316(18) 0.0205(16) -0.0003(13) 0.0006(14) -0.0093(14) C13 0.0357(19) 0.0386(19) 0.0198(16) 0.0016(14) -0.0014(15) -0.0103(15) C14 0.044(2) 0.039(2) 0.0225(17) -0.0093(14) 0.0076(16) -0.0210(16) C15 0.044(2) 0.0284(18) 0.036(2) -0.0092(15) 0.0141(17) -0.0089(16) C16 0.0274(17) 0.0287(18) 0.0380(19) -0.0067(14) 0.0083(15) -0.0051(14) C17 0.0336(19) 0.059(3) 0.0319(19) 0.0025(17) 0.0073(17) 0.0068(18) C18 0.041(2) 0.042(2) 0.0272(18) -0.0044(15) 0.0074(16) -0.0167(17) C19 0.050(2) 0.037(2) 0.0314(19) 0.0089(15) 0.0115(18) 0.0037(17) C20 0.037(2) 0.057(2) 0.0236(18) 0.0018(16) -0.0037(16) -0.0103(18) C21 0.063(3) 0.036(2) 0.0287(19) -0.0084(15) 0.0164(19) -0.0024(19) C22 0.0261(16) 0.0264(17) 0.0221(16) -0.0038(12) -0.0033(14) 0.0024(13) C23 0.040(2) 0.0339(19) 0.036(2) -0.0065(15) -0.0043(17) 0.0132(16) C24 0.095(4) 0.070(3) 0.058(3) -0.024(2) -0.033(3) 0.057(3) C25 0.076(3) 0.064(3) 0.093(4) -0.026(3) 0.008(3) 0.017(3) C26 0.0174(15) 0.0307(17) 0.0196(15) -0.0012(12) 0.0002(13) 0.0024(12) C27 0.0257(16) 0.0291(17) 0.0229(16) -0.0003(13) 0.0051(14) -0.0002(13) C28 0.0245(16) 0.0355(19) 0.0322(18) 0.0032(14) 0.0029(15) -0.0032(14) C29 0.0339(19) 0.033(2) 0.047(2) 0.0039(16) -0.0016(17) -0.0059(15) _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 C20 2.029(3) . ? Fe1 C19 2.032(3) . ? Fe1 C18 2.035(3) . ? Fe1 C16 2.035(3) . ? Fe1 C13 2.042(3) . ? Fe1 C12 2.043(3) . ? Fe1 C21 2.044(3) . ? Fe1 C14 2.044(3) . ? Fe1 C15 2.047(3) . ? Fe1 C17 2.055(4) . ? B1 N2 1.596(4) 2_655 ? B1 N1 1.597(4) . ? B1 C26 1.613(4) . ? B1 C22 1.614(4) . ? N1 C3 1.334(4) . ? N1 N2 1.354(3) . ? N2 C1 1.337(4) . ? N2 B1 1.596(4) 2_655 ? C1 C2 1.395(4) . ? C1 H1 0.9300 . ? C2 C3 1.389(4) . ? C2 C4 1.430(4) . ? C3 H3 0.9300 . ? C4 C5 1.196(4) . ? C5 C6 1.442(4) . ? C6 C11 1.400(4) . ? C6 C7 1.401(4) . ? C7 C8 1.374(4) . ? C7 H7 0.9300 . ? C8 C9 1.380(4) . ? C8 H8 0.9300 . ? C9 C10 1.392(4) . ? C9 H9 0.9300 . ? C10 C11 1.402(4) . ? C10 C12 1.476(4) . ? C11 H11 0.9300 . ? C12 C13 1.426(4) . ? C12 C16 1.434(5) . ? C13 C14 1.420(5) . ? C13 H13 0.9300 . ? C14 C15 1.406(5) . ? C14 H14 0.9300 . ? C15 C16 1.429(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C21 1.401(5) . ? C17 C18 1.412(5) . ? C17 H17 0.9300 . ? C18 C19 1.396(5) . ? C18 H18 0.9300 . ? C19 C20 1.421(5) . ? C19 H19 0.9300 . ? C20 C21 1.401(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.523(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.563(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.467(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.528(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.522(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.526(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 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 C20 Fe1 C19 40.97(14) . . ? C20 Fe1 C18 67.92(14) . . ? C19 Fe1 C18 40.14(14) . . ? C20 Fe1 C16 107.25(15) . . ? C19 Fe1 C16 118.97(15) . . ? C18 Fe1 C16 153.50(14) . . ? C20 Fe1 C13 152.29(14) . . ? C19 Fe1 C13 165.35(14) . . ? C18 Fe1 C13 128.01(14) . . ? C16 Fe1 C13 68.59(14) . . ? C20 Fe1 C12 117.78(13) . . ? C19 Fe1 C12 152.81(14) . . ? C18 Fe1 C12 164.73(14) . . ? C16 Fe1 C12 41.19(13) . . ? C13 Fe1 C12 40.85(12) . . ? C20 Fe1 C21 40.26(15) . . ? C19 Fe1 C21 68.11(15) . . ? C18 Fe1 C21 67.62(14) . . ? C16 Fe1 C21 126.55(15) . . ? C13 Fe1 C21 118.87(15) . . ? C12 Fe1 C21 106.84(14) . . ? C20 Fe1 C14 165.32(16) . . ? C19 Fe1 C14 127.79(14) . . ? C18 Fe1 C14 109.49(13) . . ? C16 Fe1 C14 68.21(14) . . ? C13 Fe1 C14 40.68(13) . . ? C12 Fe1 C14 68.70(12) . . ? C21 Fe1 C14 153.56(16) . . ? C20 Fe1 C15 127.39(16) . . ? C19 Fe1 C15 108.26(14) . . ? C18 Fe1 C15 119.90(14) . . ? C16 Fe1 C15 40.99(13) . . ? C13 Fe1 C15 68.43(14) . . ? C12 Fe1 C15 69.20(13) . . ? C21 Fe1 C15 164.73(16) . . ? C14 Fe1 C15 40.20(14) . . ? C20 Fe1 C17 67.65(15) . . ? C19 Fe1 C17 67.87(15) . . ? C18 Fe1 C17 40.40(14) . . ? C16 Fe1 C17 164.04(14) . . ? C13 Fe1 C17 108.43(15) . . ? C12 Fe1 C17 126.39(14) . . ? C21 Fe1 C17 39.97(15) . . ? C14 Fe1 C17 120.48(15) . . ? C15 Fe1 C17 153.99(15) . . ? N2 B1 N1 103.9(2) 2_655 . ? N2 B1 C26 109.3(2) 2_655 . ? N1 B1 C26 107.6(2) . . ? N2 B1 C22 106.9(2) 2_655 . ? N1 B1 C22 112.0(2) . . ? C26 B1 C22 116.4(2) . . ? C3 N1 N2 108.1(2) . . ? C3 N1 B1 126.5(2) . . ? N2 N1 B1 125.3(2) . . ? C1 N2 N1 108.5(2) . . ? C1 N2 B1 126.6(2) . 2_655 ? N1 N2 B1 123.8(2) . 2_655 ? N2 C1 C2 109.4(3) . . ? N2 C1 H1 125.3 . . ? C2 C1 H1 125.3 . . ? C3 C2 C1 104.0(3) . . ? C3 C2 C4 127.3(3) . . ? C1 C2 C4 128.7(3) . . ? N1 C3 C2 110.0(3) . . ? N1 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? C5 C4 C2 177.6(3) . . ? C4 C5 C6 179.0(3) . . ? C11 C6 C7 119.1(3) . . ? C11 C6 C5 120.8(3) . . ? C7 C6 C5 120.1(3) . . ? C8 C7 C6 119.6(3) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 118.2(3) . . ? C9 C10 C12 120.5(3) . . ? C11 C10 C12 121.3(3) . . ? C6 C11 C10 121.1(3) . . ? C6 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C13 C12 C16 106.9(3) . . ? C13 C12 C10 127.1(3) . . ? C16 C12 C10 126.0(3) . . ? C13 C12 Fe1 69.56(18) . . ? C16 C12 Fe1 69.13(18) . . ? C10 C12 Fe1 124.7(2) . . ? C14 C13 C12 108.3(3) . . ? C14 C13 Fe1 69.73(19) . . ? C12 C13 Fe1 69.59(18) . . ? C14 C13 H13 125.9 . . ? C12 C13 H13 125.9 . . ? Fe1 C13 H13 126.4 . . ? C15 C14 C13 108.9(3) . . ? C15 C14 Fe1 69.99(19) . . ? C13 C14 Fe1 69.59(17) . . ? C15 C14 H14 125.6 . . ? C13 C14 H14 125.6 . . ? Fe1 C14 H14 126.4 . . ? C14 C15 C16 107.6(3) . . ? C14 C15 Fe1 69.80(19) . . ? C16 C15 Fe1 69.08(18) . . ? C14 C15 H15 126.2 . . ? C16 C15 H15 126.2 . . ? Fe1 C15 H15 126.5 . . ? C15 C16 C12 108.4(3) . . ? C15 C16 Fe1 69.93(18) . . ? C12 C16 Fe1 69.68(18) . . ? C15 C16 H16 125.8 . . ? C12 C16 H16 125.8 . . ? Fe1 C16 H16 126.1 . . ? C21 C17 C18 107.6(3) . . ? C21 C17 Fe1 69.6(2) . . ? C18 C17 Fe1 69.04(19) . . ? C21 C17 H17 126.2 . . ? C18 C17 H17 126.2 . . ? Fe1 C17 H17 126.7 . . ? C19 C18 C17 108.7(3) . . ? C19 C18 Fe1 69.83(19) . . ? C17 C18 Fe1 70.6(2) . . ? C19 C18 H18 125.6 . . ? C17 C18 H18 125.6 . . ? Fe1 C18 H18 125.5 . . ? C18 C19 C20 107.4(3) . . ? C18 C19 Fe1 70.03(19) . . ? C20 C19 Fe1 69.38(19) . . ? C18 C19 H19 126.3 . . ? C20 C19 H19 126.3 . . ? Fe1 C19 H19 125.9 . . ? C21 C20 C19 107.9(3) . . ? C21 C20 Fe1 70.5(2) . . ? C19 C20 Fe1 69.65(19) . . ? C21 C20 H20 126.0 . . ? C19 C20 H20 126.0 . . ? Fe1 C20 H20 125.4 . . ? C17 C21 C20 108.4(3) . . ? C17 C21 Fe1 70.4(2) . . ? C20 C21 Fe1 69.29(19) . . ? C17 C21 H21 125.8 . . ? C20 C21 H21 125.8 . . ? Fe1 C21 H21 126.1 . . ? C23 C22 B1 117.1(3) . . ? C23 C22 H22A 108.0 . . ? B1 C22 H22A 108.0 . . ? C23 C22 H22B 108.0 . . ? B1 C22 H22B 108.0 . . ? H22A C22 H22B 107.3 . . ? C22 C23 C24 113.2(3) . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 115.6(4) . . ? C25 C24 H24A 108.4 . . ? C23 C24 H24A 108.4 . . ? C25 C24 H24B 108.4 . . ? C23 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 B1 116.8(2) . . ? C27 C26 H26A 108.1 . . ? B1 C26 H26A 108.1 . . ? C27 C26 H26B 108.1 . . ? B1 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C28 C27 C26 114.9(2) . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C26 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 C29 113.2(3) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 N2 B1 N1 C3 -157.5(2) 2_655 . . . ? C26 B1 N1 C3 -41.6(4) . . . . ? C22 B1 N1 C3 87.5(3) . . . . ? N2 B1 N1 N2 20.3(3) 2_655 . . . ? C26 B1 N1 N2 136.1(3) . . . . ? C22 B1 N1 N2 -94.8(3) . . . . ? C3 N1 N2 C1 -0.4(3) . . . . ? B1 N1 N2 C1 -178.5(2) . . . . ? C3 N1 N2 B1 -169.4(2) . . . 2_655 ? B1 N1 N2 B1 12.6(3) . . . 2_655 ? N1 N2 C1 C2 0.3(3) . . . . ? B1 N2 C1 C2 168.8(3) 2_655 . . . ? N2 C1 C2 C3 0.0(3) . . . . ? N2 C1 C2 C4 -179.0(3) . . . . ? N2 N1 C3 C2 0.4(3) . . . . ? B1 N1 C3 C2 178.5(2) . . . . ? C1 C2 C3 N1 -0.2(3) . . . . ? C4 C2 C3 N1 178.8(3) . . . . ? C3 C2 C4 C5 -1(8) . . . . ? C1 C2 C4 C5 177(100) . . . . ? C2 C4 C5 C6 -49(25) . . . . ? C4 C5 C6 C11 155(21) . . . . ? C4 C5 C6 C7 -26(21) . . . . ? C11 C6 C7 C8 -0.9(5) . . . . ? C5 C6 C7 C8 180.0(3) . . . . ? C6 C7 C8 C9 1.2(5) . . . . ? C7 C8 C9 C10 -0.8(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C8 C9 C10 C12 179.8(3) . . . . ? C7 C6 C11 C10 0.1(4) . . . . ? C5 C6 C11 C10 179.2(3) . . . . ? C9 C10 C11 C6 0.4(4) . . . . ? C12 C10 C11 C6 -179.5(3) . . . . ? C9 C10 C12 C13 20.2(5) . . . . ? C11 C10 C12 C13 -159.9(3) . . . . ? C9 C10 C12 C16 -162.3(3) . . . . ? C11 C10 C12 C16 17.7(5) . . . . ? C9 C10 C12 Fe1 109.6(3) . . . . ? C11 C10 C12 Fe1 -70.4(4) . . . . ? C20 Fe1 C12 C13 157.0(2) . . . . ? C19 Fe1 C12 C13 -170.4(3) . . . . ? C18 Fe1 C12 C13 48.6(6) . . . . ? C16 Fe1 C12 C13 -118.3(3) . . . . ? C21 Fe1 C12 C13 114.9(2) . . . . ? C14 Fe1 C12 C13 -37.5(2) . . . . ? C15 Fe1 C12 C13 -80.7(2) . . . . ? C17 Fe1 C12 C13 75.4(2) . . . . ? C20 Fe1 C12 C16 -84.7(2) . . . . ? C19 Fe1 C12 C16 -52.0(4) . . . . ? C18 Fe1 C12 C16 166.9(5) . . . . ? C13 Fe1 C12 C16 118.3(3) . . . . ? C21 Fe1 C12 C16 -126.8(2) . . . . ? C14 Fe1 C12 C16 80.8(2) . . . . ? C15 Fe1 C12 C16 37.6(2) . . . . ? C17 Fe1 C12 C16 -166.3(2) . . . . ? C20 Fe1 C12 C10 35.4(3) . . . . ? C19 Fe1 C12 C10 68.0(4) . . . . ? C18 Fe1 C12 C10 -73.0(6) . . . . ? C16 Fe1 C12 C10 120.1(3) . . . . ? C13 Fe1 C12 C10 -121.6(4) . . . . ? C21 Fe1 C12 C10 -6.7(3) . . . . ? C14 Fe1 C12 C10 -159.1(3) . . . . ? C15 Fe1 C12 C10 157.7(3) . . . . ? C17 Fe1 C12 C10 -46.2(3) . . . . ? C16 C12 C13 C14 -0.1(3) . . . . ? C10 C12 C13 C14 177.8(3) . . . . ? Fe1 C12 C13 C14 59.2(2) . . . . ? C16 C12 C13 Fe1 -59.3(2) . . . . ? C10 C12 C13 Fe1 118.6(3) . . . . ? C20 Fe1 C13 C14 -167.5(3) . . . . ? C19 Fe1 C13 C14 42.8(6) . . . . ? C18 Fe1 C13 C14 74.9(2) . . . . ? C16 Fe1 C13 C14 -81.1(2) . . . . ? C12 Fe1 C13 C14 -119.6(3) . . . . ? C21 Fe1 C13 C14 158.0(2) . . . . ? C15 Fe1 C13 C14 -36.86(19) . . . . ? C17 Fe1 C13 C14 115.6(2) . . . . ? C20 Fe1 C13 C12 -48.0(4) . . . . ? C19 Fe1 C13 C12 162.4(5) . . . . ? C18 Fe1 C13 C12 -165.48(19) . . . . ? C16 Fe1 C13 C12 38.52(19) . . . . ? C21 Fe1 C13 C12 -82.4(2) . . . . ? C14 Fe1 C13 C12 119.6(3) . . . . ? C15 Fe1 C13 C12 82.7(2) . . . . ? C17 Fe1 C13 C12 -124.8(2) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? Fe1 C13 C14 C15 59.1(2) . . . . ? C12 C13 C14 Fe1 -59.1(2) . . . . ? C20 Fe1 C14 C15 36.5(6) . . . . ? C19 Fe1 C14 C15 72.3(2) . . . . ? C18 Fe1 C14 C15 113.6(2) . . . . ? C16 Fe1 C14 C15 -38.14(19) . . . . ? C13 Fe1 C14 C15 -120.2(3) . . . . ? C12 Fe1 C14 C15 -82.6(2) . . . . ? C21 Fe1 C14 C15 -167.7(3) . . . . ? C17 Fe1 C14 C15 156.8(2) . . . . ? C20 Fe1 C14 C13 156.7(5) . . . . ? C19 Fe1 C14 C13 -167.4(2) . . . . ? C18 Fe1 C14 C13 -126.2(2) . . . . ? C16 Fe1 C14 C13 82.1(2) . . . . ? C12 Fe1 C14 C13 37.63(19) . . . . ? C21 Fe1 C14 C13 -47.5(4) . . . . ? C15 Fe1 C14 C13 120.2(3) . . . . ? C17 Fe1 C14 C13 -83.0(2) . . . . ? C13 C14 C15 C16 0.1(4) . . . . ? Fe1 C14 C15 C16 59.0(2) . . . . ? C13 C14 C15 Fe1 -58.9(2) . . . . ? C20 Fe1 C15 C14 -169.1(2) . . . . ? C19 Fe1 C15 C14 -127.5(2) . . . . ? C18 Fe1 C15 C14 -85.2(2) . . . . ? C16 Fe1 C15 C14 119.0(3) . . . . ? C13 Fe1 C15 C14 37.28(19) . . . . ? C12 Fe1 C15 C14 81.2(2) . . . . ? C21 Fe1 C15 C14 158.8(5) . . . . ? C17 Fe1 C15 C14 -50.7(4) . . . . ? C20 Fe1 C15 C16 71.9(3) . . . . ? C19 Fe1 C15 C16 113.4(2) . . . . ? C18 Fe1 C15 C16 155.8(2) . . . . ? C13 Fe1 C15 C16 -81.7(2) . . . . ? C12 Fe1 C15 C16 -37.8(2) . . . . ? C21 Fe1 C15 C16 39.8(6) . . . . ? C14 Fe1 C15 C16 -119.0(3) . . . . ? C17 Fe1 C15 C16 -169.8(3) . . . . ? C14 C15 C16 C12 -0.1(4) . . . . ? Fe1 C15 C16 C12 59.3(2) . . . . ? C14 C15 C16 Fe1 -59.4(2) . . . . ? C13 C12 C16 C15 0.1(4) . . . . ? C10 C12 C16 C15 -177.8(3) . . . . ? Fe1 C12 C16 C15 -59.4(2) . . . . ? C13 C12 C16 Fe1 59.6(2) . . . . ? C10 C12 C16 Fe1 -118.4(3) . . . . ? C20 Fe1 C16 C15 -127.7(2) . . . . ? C19 Fe1 C16 C15 -84.8(2) . . . . ? C18 Fe1 C16 C15 -52.8(4) . . . . ? C13 Fe1 C16 C15 81.3(2) . . . . ? C12 Fe1 C16 C15 119.5(3) . . . . ? C21 Fe1 C16 C15 -167.9(2) . . . . ? C14 Fe1 C16 C15 37.4(2) . . . . ? C17 Fe1 C16 C15 163.5(5) . . . . ? C20 Fe1 C16 C12 112.7(2) . . . . ? C19 Fe1 C16 C12 155.68(19) . . . . ? C18 Fe1 C16 C12 -172.3(3) . . . . ? C13 Fe1 C16 C12 -38.21(18) . . . . ? C21 Fe1 C16 C12 72.6(2) . . . . ? C14 Fe1 C16 C12 -82.1(2) . . . . ? C15 Fe1 C16 C12 -119.5(3) . . . . ? C17 Fe1 C16 C12 44.0(6) . . . . ? C20 Fe1 C17 C21 -37.4(2) . . . . ? C19 Fe1 C17 C21 -81.9(2) . . . . ? C18 Fe1 C17 C21 -119.2(3) . . . . ? C16 Fe1 C17 C21 36.8(6) . . . . ? C13 Fe1 C17 C21 113.2(2) . . . . ? C12 Fe1 C17 C21 71.4(3) . . . . ? C14 Fe1 C17 C21 156.2(2) . . . . ? C15 Fe1 C17 C21 -168.3(3) . . . . ? C20 Fe1 C17 C18 81.7(2) . . . . ? C19 Fe1 C17 C18 37.3(2) . . . . ? C16 Fe1 C17 C18 155.9(5) . . . . ? C13 Fe1 C17 C18 -127.6(2) . . . . ? C12 Fe1 C17 C18 -169.44(19) . . . . ? C21 Fe1 C17 C18 119.2(3) . . . . ? C14 Fe1 C17 C18 -84.6(2) . . . . ? C15 Fe1 C17 C18 -49.2(4) . . . . ? C21 C17 C18 C19 -0.5(4) . . . . ? Fe1 C17 C18 C19 -59.6(2) . . . . ? C21 C17 C18 Fe1 59.1(2) . . . . ? C20 Fe1 C18 C19 38.5(2) . . . . ? C16 Fe1 C18 C19 -46.0(4) . . . . ? C13 Fe1 C18 C19 -168.0(2) . . . . ? C12 Fe1 C18 C19 153.5(4) . . . . ? C21 Fe1 C18 C19 82.1(2) . . . . ? C14 Fe1 C18 C19 -126.1(2) . . . . ? C15 Fe1 C18 C19 -83.0(2) . . . . ? C17 Fe1 C18 C19 119.5(3) . . . . ? C20 Fe1 C18 C17 -81.0(2) . . . . ? C19 Fe1 C18 C17 -119.5(3) . . . . ? C16 Fe1 C18 C17 -165.5(3) . . . . ? C13 Fe1 C18 C17 72.6(3) . . . . ? C12 Fe1 C18 C17 34.1(6) . . . . ? C21 Fe1 C18 C17 -37.3(2) . . . . ? C14 Fe1 C18 C17 114.5(2) . . . . ? C15 Fe1 C18 C17 157.5(2) . . . . ? C17 C18 C19 C20 0.5(4) . . . . ? Fe1 C18 C19 C20 -59.6(2) . . . . ? C17 C18 C19 Fe1 60.1(2) . . . . ? C20 Fe1 C19 C18 -118.4(3) . . . . ? C16 Fe1 C19 C18 158.5(2) . . . . ? C13 Fe1 C19 C18 40.6(6) . . . . ? C12 Fe1 C19 C18 -165.1(3) . . . . ? C21 Fe1 C19 C18 -80.8(2) . . . . ? C14 Fe1 C19 C18 74.6(3) . . . . ? C15 Fe1 C19 C18 115.0(2) . . . . ? C17 Fe1 C19 C18 -37.5(2) . . . . ? C18 Fe1 C19 C20 118.4(3) . . . . ? C16 Fe1 C19 C20 -83.1(2) . . . . ? C13 Fe1 C19 C20 159.0(5) . . . . ? C12 Fe1 C19 C20 -46.7(4) . . . . ? C21 Fe1 C19 C20 37.7(2) . . . . ? C14 Fe1 C19 C20 -166.9(2) . . . . ? C15 Fe1 C19 C20 -126.5(2) . . . . ? C17 Fe1 C19 C20 80.9(2) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? Fe1 C19 C20 C21 -60.3(2) . . . . ? C18 C19 C20 Fe1 60.0(2) . . . . ? C19 Fe1 C20 C21 118.7(3) . . . . ? C18 Fe1 C20 C21 81.0(2) . . . . ? C16 Fe1 C20 C21 -126.7(2) . . . . ? C13 Fe1 C20 C21 -50.1(4) . . . . ? C12 Fe1 C20 C21 -83.4(2) . . . . ? C14 Fe1 C20 C21 163.6(5) . . . . ? C15 Fe1 C20 C21 -167.5(2) . . . . ? C17 Fe1 C20 C21 37.2(2) . . . . ? C18 Fe1 C20 C19 -37.7(2) . . . . ? C16 Fe1 C20 C19 114.6(2) . . . . ? C13 Fe1 C20 C19 -168.8(3) . . . . ? C12 Fe1 C20 C19 157.9(2) . . . . ? C21 Fe1 C20 C19 -118.7(3) . . . . ? C14 Fe1 C20 C19 45.0(6) . . . . ? C15 Fe1 C20 C19 73.8(3) . . . . ? C17 Fe1 C20 C19 -81.5(2) . . . . ? C18 C17 C21 C20 0.3(4) . . . . ? Fe1 C17 C21 C20 59.1(2) . . . . ? C18 C17 C21 Fe1 -58.8(2) . . . . ? C19 C20 C21 C17 0.0(4) . . . . ? Fe1 C20 C21 C17 -59.8(2) . . . . ? C19 C20 C21 Fe1 59.8(2) . . . . ? C20 Fe1 C21 C17 119.5(3) . . . . ? C19 Fe1 C21 C17 81.2(2) . . . . ? C18 Fe1 C21 C17 37.7(2) . . . . ? C16 Fe1 C21 C17 -168.2(2) . . . . ? C13 Fe1 C21 C17 -84.5(2) . . . . ? C12 Fe1 C21 C17 -127.1(2) . . . . ? C14 Fe1 C21 C17 -51.2(4) . . . . ? C15 Fe1 C21 C17 160.3(5) . . . . ? C19 Fe1 C21 C20 -38.3(2) . . . . ? C18 Fe1 C21 C20 -81.8(2) . . . . ? C16 Fe1 C21 C20 72.3(3) . . . . ? C13 Fe1 C21 C20 156.0(2) . . . . ? C12 Fe1 C21 C20 113.3(2) . . . . ? C14 Fe1 C21 C20 -170.8(3) . . . . ? C15 Fe1 C21 C20 40.8(6) . . . . ? C17 Fe1 C21 C20 -119.5(3) . . . . ? N2 B1 C22 C23 -172.0(3) 2_655 . . . ? N1 B1 C22 C23 -58.8(4) . . . . ? C26 B1 C22 C23 65.6(4) . . . . ? B1 C22 C23 C24 176.9(3) . . . . ? C22 C23 C24 C25 56.9(6) . . . . ? N2 B1 C26 C27 58.4(3) 2_655 . . . ? N1 B1 C26 C27 -53.9(3) . . . . ? C22 B1 C26 C27 179.6(3) . . . . ? B1 C26 C27 C28 -177.2(3) . . . . ? C26 C27 C28 C29 -178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.772 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.066 _database_code_depnum_ccdc_archive 'CCDC 891092'