# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_b2_c _database_code_depnum_ccdc_archive 'CCDC 882865' #TrackingRef '- B2_c.cif' _audit_creation_date 2012-01-17 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H42 Ni, 0.5(C6 H12)' _chemical_formula_sum 'C33 H48 Ni' _chemical_formula_weight 503.42 _chemical_melting_point ? 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _symmetry_Int_Tables_number 2 _cell_length_a 10.0461(3) _cell_length_b 11.0398(4) _cell_length_c 12.8487(3) _cell_angle_alpha 92.056(2) _cell_angle_beta 99.017(2) _cell_angle_gamma 97.933(3) _cell_volume 1391.52(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 15445 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 31.0309 _cell_measurement_theta_min 3.5246 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET) (compiled Feb 15 2011,09:34:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 548 _exptl_crystal_size_max 0.219 _exptl_crystal_size_mid 0.178 _exptl_crystal_size_min 0.056 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 55175 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 3.53 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 10.3347 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -93.00 -16.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 155.0000 -60.0000 77 #__ type_ start__ end____ width___ exp.time_ 2 omega -76.00 -1.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 131.0000 138.0000 75 #__ type_ start__ end____ width___ exp.time_ 3 omega -75.00 -47.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 129.0000 -108.0000 28 #__ type_ start__ end____ width___ exp.time_ 4 omega -93.00 17.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -77.0000 -180.0000 110 #__ type_ start__ end____ width___ exp.time_ 5 omega -81.00 11.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -38.0000 -90.0000 92 #__ type_ start__ end____ width___ exp.time_ 6 omega -33.00 61.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 38.0000 -60.0000 94 #__ type_ start__ end____ width___ exp.time_ 7 omega -93.00 19.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -77.0000 30.0000 112 #__ type_ start__ end____ width___ exp.time_ 8 omega -57.00 48.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 -77.0000 90.0000 105 #__ type_ start__ end____ width___ exp.time_ 9 omega -91.00 11.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -38.0000 30.0000 102 #__ type_ start__ end____ width___ exp.time_ 10 omega -91.00 11.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -38.0000 -60.0000 102 #__ type_ start__ end____ width___ exp.time_ 11 omega -104.00 -32.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 179.0000 -150.0000 72 #__ type_ start__ end____ width___ exp.time_ 12 omega -91.00 11.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 -38.0000 -180.0000 102 #__ type_ start__ end____ width___ exp.time_ 13 omega 22.00 76.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 -131.0000 -174.0000 54 #__ type_ start__ end____ width___ exp.time_ 14 omega -61.00 42.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 -38.0000 90.0000 103 #__ type_ start__ end____ width___ exp.time_ 15 omega -75.00 0.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 129.0000 -108.0000 75 #__ type_ start__ end____ width___ exp.time_ 16 omega -85.00 -10.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 146.0000 161.0000 75 #__ type_ start__ end____ width___ exp.time_ 17 omega -72.00 4.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - -15.0548 124.0000 38.0000 76 #__ type_ start__ end____ width___ exp.time_ 18 omega 56.00 105.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 179.0000 60.0000 49 #__ type_ start__ end____ width___ exp.time_ 19 omega -11.00 91.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 38.0000 60.0000 102 #__ type_ start__ end____ width___ exp.time_ 20 omega -18.00 94.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 77.0000 120.0000 112 #__ type_ start__ end____ width___ exp.time_ 21 omega -74.00 99.00 1.0000 29.9900 omega____ theta____ kappa____ phi______ frames - 15.3673 0.0000 -180.0000 173 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0603938000 _diffrn_orient_matrix_UB_12 0.0246056000 _diffrn_orient_matrix_UB_13 -0.0184447000 _diffrn_orient_matrix_UB_21 -0.0375907000 _diffrn_orient_matrix_UB_22 -0.0598171000 _diffrn_orient_matrix_UB_23 -0.0056674000 _diffrn_orient_matrix_UB_31 -0.0126735000 _diffrn_orient_matrix_UB_32 0.0062548000 _diffrn_orient_matrix_UB_33 0.0525619000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4278 _reflns_number_total 4879 _reflns_threshold_expression I>2u(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET) (compiled Feb 15 2011,09:34:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET) (compiled Feb 15 2011,09:34:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET) (compiled Feb 15 2011,09:34:54) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.884 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.060 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 315 _refine_ls_number_reflns 4879 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0370 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+1.4049P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0860 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ni1 Ni 0.34374(3) 0.28404(3) 0.24203(2) 0.01312(10) Uani 1 1 d . . . C14 C 0.6055(3) 0.6686(2) 0.3126(2) 0.0255(6) Uani 1 1 d . . . H14A H 0.6317 0.6498 0.3863 0.038 Uiso 1 1 calc R . . H14B H 0.5953 0.7555 0.3094 0.038 Uiso 1 1 calc R . . H14C H 0.6761 0.6510 0.2720 0.038 Uiso 1 1 calc R . . C33 C 0.7900(2) 0.2216(2) 0.21473(19) 0.0209(5) Uani 1 1 d . . . H33A H 0.8239 0.2365 0.2905 0.031 Uiso 1 1 calc R . . H33B H 0.8049 0.2984 0.1794 0.031 Uiso 1 1 calc R . . H33C H 0.8389 0.1611 0.1853 0.031 Uiso 1 1 calc R . . C3 C 0.1788(2) 0.1415(2) 0.27429(17) 0.0161(5) Uani 1 1 d . . . C24 C 0.4880(2) 0.3901(2) 0.36626(17) 0.0150(5) Uani 1 1 d . . . H24 H 0.4604 0.4167 0.4279 0.018 Uiso 1 1 d R . . C15 C 0.3603(2) 0.6198(2) 0.33033(18) 0.0213(5) Uani 1 1 d . . . H15A H 0.3910 0.6089 0.4052 0.032 Uiso 1 1 calc R . . H15B H 0.2750 0.5649 0.3057 0.032 Uiso 1 1 calc R . . H15C H 0.3452 0.7049 0.3211 0.032 Uiso 1 1 calc R . . C12 C 0.2278(2) 0.1962(2) -0.05911(18) 0.0208(5) Uani 1 1 d . . . H12A H 0.2074 0.2081 -0.1348 0.031 Uiso 1 1 calc R . . H12B H 0.2144 0.1083 -0.0476 0.031 Uiso 1 1 calc R . . H12C H 0.3226 0.2310 -0.0321 0.031 Uiso 1 1 calc R . . C6 C 0.1326(2) 0.2602(2) -0.00095(17) 0.0184(5) Uani 1 1 d . . . C8 C 0.2786(3) 0.4708(2) 0.02227(18) 0.0216(5) Uani 1 1 d . . . H8 H 0.3574 0.4501 -0.0025 0.026 Uiso 1 1 calc R . . C4 C 0.1467(2) 0.2604(2) 0.29451(18) 0.0162(5) Uani 1 1 d . . . H4 H 0.1363 0.2934 0.3598 0.019 Uiso 1 1 d R . . C5 C 0.1335(2) 0.3207(2) 0.19919(17) 0.0164(5) Uani 1 1 d . . . H5 H 0.1121 0.3996 0.1915 0.020 Uiso 1 1 d R . . C11 C 0.4696(2) 0.5897(2) 0.26583(18) 0.0180(5) Uani 1 1 d . . . C22 C 0.5365(2) 0.3797(2) 0.19926(17) 0.0149(5) Uani 1 1 d . . . H22 H 0.5465 0.3993 0.1308 0.018 Uiso 1 1 d R . . C9 C 0.2967(3) 0.5626(2) 0.09474(18) 0.0214(5) Uani 1 1 d . . . H9 H 0.2176 0.5912 0.1124 0.026 Uiso 1 1 calc R . . C13 C -0.0158(2) 0.2018(2) -0.04351(19) 0.0271(6) Uani 1 1 d . . . H13A H -0.0260 0.1136 -0.0333 0.041 Uiso 1 1 calc R . . H13B H -0.0373 0.2150 -0.1189 0.041 Uiso 1 1 calc R . . H13C H -0.0780 0.2397 -0.0053 0.041 Uiso 1 1 calc R . . C32 C 0.5869(2) 0.1514(2) 0.07818(17) 0.0185(5) Uani 1 1 d . . . H32A H 0.4885 0.1238 0.0652 0.028 Uiso 1 1 calc R . . H32B H 0.6337 0.0889 0.0495 0.028 Uiso 1 1 calc R . . H32C H 0.6067 0.2282 0.0438 0.028 Uiso 1 1 calc R . . C31 C 0.1785(2) 0.0401(2) 0.35142(17) 0.0178(5) Uani 1 1 d . . . C27 C 0.6177(2) 0.0496(2) 0.25150(18) 0.0175(5) Uani 1 1 d . . . H27A H 0.6670 -0.0090 0.2184 0.021 Uiso 1 1 calc R . . H27B H 0.6598 0.0635 0.3267 0.021 Uiso 1 1 calc R . . C29 C 0.4087(2) -0.0217(2) 0.32739(19) 0.0189(5) Uani 1 1 d . . . H29 H 0.4619 -0.0051 0.3956 0.023 Uiso 1 1 calc R . . C23 C 0.4905(2) 0.45600(19) 0.27401(17) 0.0143(5) Uani 1 1 d . . . C21 C 0.5653(2) 0.2689(2) 0.24559(17) 0.0142(5) Uani 1 1 d . . . C30 C 0.2587(2) -0.0622(2) 0.32150(19) 0.0201(5) Uani 1 1 d . . . H30A H 0.2454 -0.1297 0.3692 0.024 Uiso 1 1 calc R . . H30B H 0.2202 -0.0951 0.2487 0.024 Uiso 1 1 calc R . . C10 C 0.4318(2) 0.6248(2) 0.15081(18) 0.0202(5) Uani 1 1 d . . . H10A H 0.4320 0.7145 0.1508 0.024 Uiso 1 1 calc R . . H10B H 0.5032 0.6049 0.1106 0.024 Uiso 1 1 calc R . . C7 C 0.1451(2) 0.3971(2) -0.02361(18) 0.0232(5) Uani 1 1 d . . . H7A H 0.1302 0.4042 -0.1010 0.028 Uiso 1 1 calc R . . H7B H 0.0719 0.4327 0.0045 0.028 Uiso 1 1 calc R . . C25 C 0.5348(2) 0.2766(2) 0.34964(17) 0.0154(5) Uani 1 1 d . . . H25 H 0.5440 0.2172 0.3987 0.018 Uiso 1 1 d R . . C28 C 0.4729(2) -0.0071(2) 0.24539(19) 0.0186(5) Uani 1 1 d . . . H28 H 0.4232 -0.0348 0.1777 0.022 Uiso 1 1 calc R . . C26 C 0.6368(2) 0.1726(2) 0.19742(17) 0.0153(5) Uani 1 1 d . . . C2 C 0.1877(2) 0.1316(2) 0.16467(17) 0.0157(5) Uani 1 1 d . . . H2 H 0.2098 0.0639 0.1294 0.019 Uiso 1 1 d R . . C1 C 0.1582(2) 0.2415(2) 0.11718(17) 0.0160(5) Uani 1 1 d . . . C35 C 0.2343(2) 0.0926(2) 0.46463(18) 0.0220(5) Uani 1 1 d . . . H35A H 0.1757 0.1500 0.4857 0.033 Uiso 1 1 calc R . . H35B H 0.3270 0.1357 0.4677 0.033 Uiso 1 1 calc R . . H35C H 0.2356 0.0257 0.5127 0.033 Uiso 1 1 calc R . . C34 C 0.0289(2) -0.0187(2) 0.3464(2) 0.0250(6) Uani 1 1 d . . . H34A H -0.0083 -0.0516 0.2742 0.038 Uiso 1 1 calc R . . H34B H -0.0246 0.0434 0.3668 0.038 Uiso 1 1 calc R . . H34C H 0.0246 -0.0851 0.3948 0.038 Uiso 1 1 calc R . . C40 C 0.0853(3) 0.6239(3) 0.4905(2) 0.0440(8) Uani 1 1 d . . . H40A H 0.0492 0.6815 0.5359 0.053 Uiso 1 1 calc R . . H40B H 0.1609 0.6699 0.4607 0.053 Uiso 1 1 calc R . . C41 C 0.1369(4) 0.5193(3) 0.5559(3) 0.0509(9) Uani 1 1 d . . . H41A H 0.1822 0.4689 0.5109 0.061 Uiso 1 1 calc R . . H41B H 0.2066 0.5563 0.6158 0.061 Uiso 1 1 calc R . . C42 C 0.0281(3) 0.4352(4) 0.5991(3) 0.0579(10) Uani 1 1 d . . . H42A H -0.0120 0.4829 0.6499 0.069 Uiso 1 1 calc R . . H42B H 0.0702 0.3702 0.6374 0.069 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 Ni1 0.01271(16) 0.01325(16) 0.01424(16) 0.00095(11) 0.00343(11) 0.00343(11) C14 0.0284(14) 0.0165(13) 0.0314(14) 0.0011(10) 0.0063(11) 0.0011(10) C33 0.0154(12) 0.0237(13) 0.0247(13) -0.0002(10) 0.0054(10) 0.0050(10) C3 0.0102(11) 0.0185(12) 0.0193(12) 0.0003(9) 0.0024(9) 0.0012(9) C24 0.0160(11) 0.0162(12) 0.0124(11) -0.0017(9) 0.0036(9) 0.0008(9) C15 0.0300(14) 0.0172(12) 0.0201(12) 0.0013(10) 0.0089(10) 0.0095(10) C12 0.0261(13) 0.0216(13) 0.0157(12) 0.0025(9) 0.0034(10) 0.0073(10) C6 0.0185(12) 0.0206(12) 0.0164(12) 0.0013(9) 0.0003(9) 0.0070(10) C8 0.0285(13) 0.0210(13) 0.0190(12) 0.0082(10) 0.0087(10) 0.0093(10) C4 0.0120(11) 0.0195(12) 0.0184(12) -0.0017(9) 0.0070(9) 0.0019(9) C5 0.0120(11) 0.0152(12) 0.0229(12) 0.0013(9) 0.0028(9) 0.0056(9) C11 0.0232(13) 0.0126(11) 0.0203(12) 0.0026(9) 0.0070(10) 0.0052(9) C22 0.0148(11) 0.0172(12) 0.0131(11) 0.0017(9) 0.0043(9) 0.0008(9) C9 0.0304(14) 0.0197(13) 0.0185(12) 0.0096(10) 0.0076(10) 0.0125(10) C13 0.0229(13) 0.0349(15) 0.0223(13) 0.0008(11) -0.0019(10) 0.0068(11) C32 0.0226(13) 0.0161(12) 0.0189(12) 0.0004(9) 0.0054(10) 0.0076(10) C31 0.0183(12) 0.0179(12) 0.0180(12) 0.0033(9) 0.0048(9) 0.0024(9) C27 0.0182(12) 0.0166(12) 0.0197(12) 0.0018(9) 0.0039(9) 0.0088(9) C29 0.0211(12) 0.0128(12) 0.0241(13) 0.0032(9) 0.0029(10) 0.0074(9) C23 0.0137(11) 0.0114(11) 0.0178(11) -0.0005(9) 0.0032(9) 0.0008(9) C21 0.0099(11) 0.0158(11) 0.0163(11) -0.0001(9) 0.0009(9) 0.0016(9) C30 0.0237(13) 0.0162(12) 0.0223(12) 0.0062(10) 0.0076(10) 0.0041(10) C10 0.0299(14) 0.0118(12) 0.0226(13) 0.0045(9) 0.0107(10) 0.0074(10) C7 0.0292(14) 0.0259(14) 0.0167(12) 0.0054(10) 0.0016(10) 0.0130(11) C25 0.0130(11) 0.0177(12) 0.0145(11) 0.0027(9) -0.0012(9) 0.0020(9) C28 0.0217(12) 0.0117(11) 0.0234(13) 0.0010(9) 0.0034(10) 0.0062(9) C26 0.0151(11) 0.0142(11) 0.0177(12) 0.0005(9) 0.0038(9) 0.0051(9) C2 0.0117(11) 0.0155(12) 0.0198(12) -0.0026(9) 0.0028(9) 0.0023(9) C1 0.0096(11) 0.0196(12) 0.0186(12) 0.0006(9) 0.0009(9) 0.0032(9) C35 0.0257(13) 0.0236(13) 0.0194(12) 0.0063(10) 0.0074(10) 0.0073(10) C34 0.0230(13) 0.0251(14) 0.0292(14) 0.0065(11) 0.0104(11) 0.0028(11) C40 0.0240(15) 0.070(2) 0.0380(17) -0.0185(15) 0.0111(13) 0.0040(14) C41 0.056(2) 0.0422(19) 0.054(2) -0.0107(16) 0.0172(17) -0.0035(16) C42 0.044(2) 0.091(3) 0.0436(19) -0.0069(18) 0.0136(16) 0.0247(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C3 2.222(2) . ? Ni1 C24 2.166(2) . ? Ni1 C4 2.174(2) . ? Ni1 C5 2.195(2) . ? Ni1 C22 2.231(2) . ? Ni1 C23 2.220(2) . ? Ni1 C21 2.248(2) . ? Ni1 C25 2.196(2) . ? Ni1 C2 2.223(2) . ? Ni1 C1 2.244(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 C11 1.537(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33 C26 1.539(3) . ? C3 C4 1.418(3) . ? C3 C31 1.522(3) . ? C3 C2 1.427(3) . ? C24 H24 0.9306 . ? C24 C23 1.415(3) . ? C24 C25 1.418(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 C11 1.540(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 C6 1.532(3) . ? C6 C13 1.546(3) . ? C6 C7 1.541(3) . ? C6 C1 1.526(3) . ? C8 H8 0.9500 . ? C8 C9 1.325(3) . ? C8 C7 1.492(3) . ? C4 H4 0.9293 . ? C4 C5 1.412(3) . ? C5 H5 0.9300 . ? C5 C1 1.419(3) . ? C11 C23 1.524(3) . ? C11 C10 1.544(3) . ? C22 H22 0.9302 . ? C22 C23 1.426(3) . ? C22 C21 1.425(3) . ? C9 H9 0.9500 . ? C9 C10 1.494(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32 C26 1.534(3) . ? C31 C30 1.546(3) . ? C31 C35 1.536(3) . ? C31 C34 1.543(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.491(3) . ? C27 C26 1.549(3) . ? C29 H29 0.9500 . ? C29 C30 1.501(3) . ? C29 C28 1.322(3) . ? C21 C25 1.420(3) . ? C21 C26 1.527(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C25 H25 0.9295 . ? C28 H28 0.9500 . ? C2 H2 0.9309 . ? C2 C1 1.424(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.551(5) . ? C40 C42 1.543(4) 2_566 ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C42 1.521(5) . ? C42 C40 1.543(4) 2_566 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? 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 C3 Ni1 C22 163.46(8) . . ? C3 Ni1 C21 128.20(8) . . ? C3 Ni1 C2 37.44(8) . . ? C3 Ni1 C1 62.89(8) . . ? C24 Ni1 C3 122.80(8) . . ? C24 Ni1 C4 107.26(8) . . ? C24 Ni1 C5 122.48(8) . . ? C24 Ni1 C22 62.32(8) . . ? C24 Ni1 C23 37.61(8) . . ? C24 Ni1 C21 62.91(8) . . ? C24 Ni1 C25 37.94(8) . . ? C24 Ni1 C2 158.61(8) . . ? C24 Ni1 C1 157.55(8) . . ? C4 Ni1 C3 37.61(8) . . ? C4 Ni1 C5 37.70(8) . . ? C4 Ni1 C22 158.92(8) . . ? C4 Ni1 C23 123.09(8) . . ? C4 Ni1 C21 157.37(8) . . ? C4 Ni1 C25 122.38(8) . . ? C4 Ni1 C2 62.33(8) . . ? C4 Ni1 C1 62.80(8) . . ? C5 Ni1 C3 62.83(8) . . ? C5 Ni1 C22 129.99(8) . . ? C5 Ni1 C23 111.76(8) . . ? C5 Ni1 C21 164.91(8) . . ? C5 Ni1 C25 155.30(8) . . ? C5 Ni1 C2 61.98(8) . . ? C5 Ni1 C1 37.26(8) . . ? C22 Ni1 C21 37.09(8) . . ? C22 Ni1 C1 119.29(8) . . ? C23 Ni1 C3 155.83(8) . . ? C23 Ni1 C22 37.38(8) . . ? C23 Ni1 C21 62.83(8) . . ? C23 Ni1 C2 163.78(8) . . ? C23 Ni1 C1 128.60(8) . . ? C25 Ni1 C3 111.23(8) . . ? C25 Ni1 C22 61.95(8) . . ? C25 Ni1 C23 62.93(8) . . ? C25 Ni1 C21 37.24(8) . . ? C25 Ni1 C2 129.38(8) . . ? C25 Ni1 C1 164.50(8) . . ? C2 Ni1 C22 133.56(8) . . ? C2 Ni1 C21 118.93(8) . . ? C2 Ni1 C1 37.17(8) . . ? C1 Ni1 C21 133.58(8) . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? C4 C3 Ni1 69.38(12) . . ? C4 C3 C31 125.27(19) . . ? C4 C3 C2 106.27(19) . . ? C31 C3 Ni1 131.73(15) . . ? C2 C3 Ni1 71.31(12) . . ? C2 C3 C31 127.7(2) . . ? Ni1 C24 H24 120.8 . . ? C23 C24 Ni1 73.26(12) . . ? C23 C24 H24 125.7 . . ? C23 C24 C25 108.89(19) . . ? C25 C24 Ni1 72.18(12) . . ? C25 C24 H24 125.4 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? C12 C6 C13 108.36(19) . . ? C12 C6 C7 110.47(19) . . ? C7 C6 C13 107.47(19) . . ? C1 C6 C12 111.45(18) . . ? C1 C6 C13 107.08(19) . . ? C1 C6 C7 111.82(18) . . ? C9 C8 H8 117.2 . . ? C9 C8 C7 125.5(2) . . ? C7 C8 H8 117.2 . . ? Ni1 C4 H4 121.1 . . ? C3 C4 Ni1 73.00(12) . . ? C3 C4 H4 125.7 . . ? C5 C4 Ni1 71.93(12) . . ? C5 C4 C3 108.87(19) . . ? C5 C4 H4 125.5 . . ? Ni1 C5 H5 122.4 . . ? C4 C5 Ni1 70.37(12) . . ? C4 C5 H5 125.5 . . ? C4 C5 C1 108.9(2) . . ? C1 C5 Ni1 73.26(12) . . ? C1 C5 H5 125.6 . . ? C14 C11 C15 108.44(19) . . ? C14 C11 C10 107.31(19) . . ? C15 C11 C10 109.71(19) . . ? C23 C11 C14 107.34(19) . . ? C23 C11 C15 110.84(18) . . ? C23 C11 C10 113.01(18) . . ? Ni1 C22 H22 123.5 . . ? C23 C22 Ni1 70.88(12) . . ? C23 C22 H22 125.3 . . ? C21 C22 Ni1 72.10(12) . . ? C21 C22 H22 125.1 . . ? C21 C22 C23 109.56(19) . . ? C8 C9 H9 117.5 . . ? C8 C9 C10 125.1(2) . . ? C10 C9 H9 117.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? C3 C31 C30 112.62(18) . . ? C3 C31 C35 110.78(19) . . ? C3 C31 C34 107.03(18) . . ? C35 C31 C30 110.28(19) . . ? C35 C31 C34 108.66(19) . . ? C34 C31 C30 107.28(19) . . ? H27A C27 H27B 107.6 . . ? C28 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? C28 C27 C26 114.38(18) . . ? C26 C27 H27A 108.7 . . ? C26 C27 H27B 108.7 . . ? C30 C29 H29 117.3 . . ? C28 C29 H29 117.3 . . ? C28 C29 C30 125.4(2) . . ? C24 C23 Ni1 69.13(12) . . ? C24 C23 C11 124.99(19) . . ? C24 C23 C22 106.47(19) . . ? C11 C23 Ni1 131.17(15) . . ? C22 C23 Ni1 71.75(12) . . ? C22 C23 C11 127.85(19) . . ? C22 C21 Ni1 70.81(12) . . ? C22 C21 C26 125.40(19) . . ? C25 C21 Ni1 69.38(12) . . ? C25 C21 C22 106.47(19) . . ? C25 C21 C26 127.4(2) . . ? C26 C21 Ni1 132.05(15) . . ? C31 C30 H30A 108.7 . . ? C31 C30 H30B 108.7 . . ? C29 C30 C31 114.33(19) . . ? C29 C30 H30A 108.7 . . ? C29 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C11 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? C9 C10 C11 114.79(19) . . ? C9 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C6 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 C6 114.66(19) . . ? C8 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? Ni1 C25 H25 122.7 . . ? C24 C25 Ni1 69.88(12) . . ? C24 C25 C21 108.59(19) . . ? C24 C25 H25 125.7 . . ? C21 C25 Ni1 73.38(12) . . ? C21 C25 H25 125.7 . . ? C27 C28 H28 117.6 . . ? C29 C28 C27 124.7(2) . . ? C29 C28 H28 117.6 . . ? C33 C26 C27 108.00(18) . . ? C32 C26 C33 108.07(18) . . ? C32 C26 C27 109.97(18) . . ? C21 C26 C33 107.58(18) . . ? C21 C26 C32 111.17(18) . . ? C21 C26 C27 111.89(18) . . ? Ni1 C2 H2 122.8 . . ? C3 C2 Ni1 71.24(12) . . ? C3 C2 H2 125.3 . . ? C1 C2 Ni1 72.23(12) . . ? C1 C2 C3 109.64(19) . . ? C1 C2 H2 125.0 . . ? C6 C1 Ni1 132.94(15) . . ? C5 C1 Ni1 69.48(12) . . ? C5 C1 C6 126.7(2) . . ? C5 C1 C2 106.31(19) . . ? C2 C1 Ni1 70.60(12) . . ? C2 C1 C6 126.1(2) . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? H40A C40 H40B 108.5 . . ? C41 C40 H40A 110.2 . . ? C41 C40 H40B 110.2 . . ? C42 C40 H40A 110.2 2_566 . ? C42 C40 H40B 110.2 2_566 . ? C42 C40 C41 107.6(3) 2_566 . ? C40 C41 H41A 108.4 . . ? C40 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? C42 C41 C40 115.5(3) . . ? C42 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? C40 C42 H42A 109.4 2_566 . ? C40 C42 H42B 109.4 2_566 . ? C41 C42 C40 111.1(3) . 2_566 ? C41 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? data_b_f16 _database_code_depnum_ccdc_archive 'CCDC 882866' #TrackingRef '- B_f16.cif' _audit_creation_date 2012-01-17 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H42 Fe' _chemical_formula_sum 'C30 H42 Fe' _chemical_formula_weight 458.49 _chemical_melting_point ? 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.8147(2) _cell_length_b 10.9245(3) _cell_length_c 13.1469(3) _cell_angle_alpha 67.653(2) _cell_angle_beta 86.4663(18) _cell_angle_gamma 75.074(2) _cell_volume 1258.72(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 33325 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 30.4196 _cell_measurement_theta_min 3.2043 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.278 _exptl_crystal_size_mid 0.233 _exptl_crystal_size_min 0.166 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 75409 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_min 3.21 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 10.3347 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.944 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -86.00 -19.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 148.0000 -144.0000 67 #__ type_ start__ end____ width___ exp.time_ 2 omega -84.00 -50.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 146.0000 60.0000 34 #__ type_ start__ end____ width___ exp.time_ 3 omega -16.00 92.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 77.0000 -120.0000 108 #__ type_ start__ end____ width___ exp.time_ 4 omega -12.00 88.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 38.0000 -180.0000 100 #__ type_ start__ end____ width___ exp.time_ 5 omega -60.00 28.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 -39.0000 119.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega -35.00 48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 -77.0000 -120.0000 83 #__ type_ start__ end____ width___ exp.time_ 7 omega -63.00 48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 -77.0000 60.0000 111 #__ type_ start__ end____ width___ exp.time_ 8 omega -18.00 89.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 77.0000 30.0000 107 #__ type_ start__ end____ width___ exp.time_ 9 omega -88.00 -13.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 151.0000 166.0000 75 #__ type_ start__ end____ width___ exp.time_ 10 omega -103.00 -32.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 179.0000 -60.0000 71 #__ type_ start__ end____ width___ exp.time_ 11 omega -40.00 62.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 38.0000 -180.0000 102 #__ type_ start__ end____ width___ exp.time_ 12 omega -12.00 90.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 38.0000 -150.0000 102 #__ type_ start__ end____ width___ exp.time_ 13 omega -12.00 90.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 38.0000 -30.0000 102 #__ type_ start__ end____ width___ exp.time_ 14 omega -13.00 90.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 39.0000 93.0000 103 #__ type_ start__ end____ width___ exp.time_ 15 omega -88.00 -13.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 151.0000 -69.0000 75 #__ type_ start__ end____ width___ exp.time_ 16 omega -75.00 -1.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 131.0000 -7.0000 74 #__ type_ start__ end____ width___ exp.time_ 17 omega -92.00 20.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 -77.0000 -120.0000 112 #__ type_ start__ end____ width___ exp.time_ 18 omega -40.00 62.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 38.0000 -60.0000 102 #__ type_ start__ end____ width___ exp.time_ 19 omega -83.00 -10.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 145.0000 137.0000 73 #__ type_ start__ end____ width___ exp.time_ 20 omega 56.00 104.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 179.0000 -120.0000 48 #__ type_ start__ end____ width___ exp.time_ 21 omega -103.00 -32.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 179.0000 120.0000 71 #__ type_ start__ end____ width___ exp.time_ 22 omega -84.00 -10.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 146.0000 60.0000 74 #__ type_ start__ end____ width___ exp.time_ 23 omega -92.00 -17.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 157.0000 -26.0000 75 #__ type_ start__ end____ width___ exp.time_ 24 omega -103.00 74.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - -13.6182 0.0000 -180.0000 177 #__ type_ start__ end____ width___ exp.time_ 25 omega 56.00 104.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 13.9307 179.0000 30.0000 48 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0657441000 _diffrn_orient_matrix_UB_12 0.0164169000 _diffrn_orient_matrix_UB_13 -0.0279571000 _diffrn_orient_matrix_UB_21 0.0202144000 _diffrn_orient_matrix_UB_22 -0.0626403000 _diffrn_orient_matrix_UB_23 -0.0082337000 _diffrn_orient_matrix_UB_31 -0.0295354000 _diffrn_orient_matrix_UB_32 -0.0327643000 _diffrn_orient_matrix_UB_33 0.0505858000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_current 40 _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6294 _reflns_number_total 7236 _reflns_threshold_expression I>2u(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.766 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 7236 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.7080P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.0877 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.287869(19) 0.376554(19) 0.728733(15) 0.01593(6) Uani 1 1 d . A . C1 C 0.49744(14) 0.38725(14) 0.73751(11) 0.0195(3) Uani 1 1 d . A . C2 C 0.48846(13) 0.24804(14) 0.77984(11) 0.0188(2) Uani 1 1 d . . . H2 H 0.5165 0.1842 0.8525 0.023 Uiso 1 1 calc R . . C3 C 0.43102(14) 0.21943(14) 0.69649(11) 0.0193(3) Uani 1 1 d . A . C4 C 0.40099(15) 0.34445(14) 0.60188(11) 0.0206(3) Uani 1 1 d . . . H4 H 0.3605 0.3575 0.5336 0.025 Uiso 1 1 calc R . . C5 C 0.44172(14) 0.44607(14) 0.62699(11) 0.0205(3) Uani 1 1 d . . . H5 H 0.4332 0.5381 0.5781 0.025 Uiso 1 1 calc R . . C6 C 0.58435(15) 0.44573(13) 0.79028(12) 0.0241(3) Uani 1 1 d D . . C7 C 0.5499(2) 0.60433(15) 0.7419(3) 0.0294(5) Uani 0.848(4) 1 d PD A 1 H7A H 0.6091 0.6347 0.7811 0.035 Uiso 0.848(4) 1 calc PR A 1 H7B H 0.5732 0.6365 0.6633 0.035 Uiso 0.848(4) 1 calc PR A 1 C8 C 0.39876(18) 0.66656(19) 0.7520(2) 0.0287(4) Uani 0.848(4) 1 d PD A 1 H8 H 0.3639 0.6562 0.8230 0.034 Uiso 0.848(4) 1 calc PR A 1 C9 C 0.31020(17) 0.73696(18) 0.66370(16) 0.0301(5) Uani 0.848(4) 1 d PD A 1 H9 H 0.3495 0.7622 0.5931 0.036 Uiso 0.848(4) 1 calc PR A 1 C10 C 0.15445(17) 0.77790(17) 0.66961(15) 0.0281(4) Uani 0.848(4) 1 d PD A 1 H10A H 0.1200 0.8768 0.6248 0.034 Uiso 0.848(4) 1 calc PR A 1 H10B H 0.1304 0.7637 0.7468 0.034 Uiso 0.848(4) 1 calc PR A 1 C14 C -0.0820(2) 0.7510(2) 0.6395(2) 0.0347(5) Uani 0.848(4) 1 d PD A 1 H14A H -0.1346 0.7018 0.6146 0.052 Uiso 0.848(4) 1 calc PR A 1 H14B H -0.1116 0.8490 0.5944 0.052 Uiso 0.848(4) 1 calc PR A 1 H14C H -0.1011 0.7365 0.7168 0.052 Uiso 0.848(4) 1 calc PR A 1 C11 C 0.0772(2) 0.6971(3) 0.6284(2) 0.0234(4) Uani 0.848(4) 1 d PDU A 1 C15 C 0.1066(3) 0.7244(3) 0.50641(19) 0.0294(5) Uani 0.848(4) 1 d PD A 1 H15A H 0.2058 0.6818 0.4996 0.044 Uiso 0.848(4) 1 calc PR A 1 H15B H 0.0866 0.8232 0.4645 0.044 Uiso 0.848(4) 1 calc PR A 1 H15C H 0.0460 0.6854 0.4775 0.044 Uiso 0.848(4) 1 calc PR A 1 C12 C 0.57728(17) 0.39033(16) 0.91549(12) 0.0279(3) Uani 1 1 d . A . H12A H 0.4795 0.4167 0.9359 0.042 Uiso 1 1 calc R . . H12B H 0.6369 0.4284 0.9462 0.042 Uiso 1 1 calc R . . H12C H 0.6109 0.2903 0.9447 0.042 Uiso 1 1 calc R . . C13 C 0.73900(17) 0.3988(2) 0.76044(16) 0.0392(4) Uani 1 1 d . A . H13A H 0.7709 0.2988 0.7937 0.059 Uiso 1 1 calc R . . H13B H 0.7993 0.4388 0.7885 0.059 Uiso 1 1 calc R . . H13C H 0.7446 0.4292 0.6803 0.059 Uiso 1 1 calc R . . C21 C 0.14267(14) 0.34125(14) 0.85276(11) 0.0198(3) Uani 1 1 d . . . C22 C 0.15170(14) 0.48044(14) 0.81312(11) 0.0190(2) Uani 1 1 d . A . H22 H 0.1784 0.5234 0.8566 0.023 Uiso 1 1 calc R . . C23 C 0.11432(14) 0.54484(14) 0.69791(11) 0.0199(3) Uani 1 1 d . . . C24 C 0.08488(14) 0.44280(14) 0.66620(11) 0.0213(3) Uani 1 1 d . A . H24 H 0.0585 0.4555 0.5938 0.026 Uiso 1 1 calc R . . C25 C 0.10127(14) 0.31909(14) 0.76002(11) 0.0213(3) Uani 1 1 d . A . H25 H 0.0871 0.2358 0.7610 0.026 Uiso 1 1 calc R . . C26 C 0.1372(7) 0.2515(5) 0.9729(11) 0.0222(8) Uani 0.490(4) 1 d PDU B 1 C32 C 0.2483(12) 0.2682(15) 1.0408(13) 0.0275(17) Uani 0.490(4) 1 d PD B 1 H32A H 0.3421 0.2436 1.0128 0.041 Uiso 0.490(4) 1 calc PR B 1 H32B H 0.2468 0.2081 1.1181 0.041 Uiso 0.490(4) 1 calc PR B 1 H32C H 0.2269 0.3635 1.0347 0.041 Uiso 0.490(4) 1 calc PR B 1 C33 C -0.0099(5) 0.2963(5) 1.0146(4) 0.0322(9) Uani 0.490(4) 1 d PD B 1 H33A H -0.0292 0.3929 1.0047 0.048 Uiso 0.490(4) 1 calc PR B 1 H33B H -0.0128 0.2404 1.0929 0.048 Uiso 0.490(4) 1 calc PR B 1 H33C H -0.0813 0.2842 0.9730 0.048 Uiso 0.490(4) 1 calc PR B 1 C27 C 0.1619(4) 0.0974(3) 0.9943(3) 0.0298(8) Uani 0.490(4) 1 d PD B 1 H27A H 0.1636 0.0451 1.0746 0.036 Uiso 0.490(4) 1 calc PR B 1 H27B H 0.0819 0.0847 0.9604 0.036 Uiso 0.490(4) 1 calc PR B 1 C28 C 0.2954(3) 0.0411(3) 0.9496(2) 0.0271(8) Uani 0.490(4) 1 d PD B 1 H28 H 0.3816 0.0361 0.9819 0.032 Uiso 0.490(4) 1 calc PR B 1 C29 C 0.3026(5) -0.0031(4) 0.8670(3) 0.0271(9) Uani 0.490(4) 1 d PD B 1 H29 H 0.2192 -0.0147 0.8429 0.033 Uiso 0.490(4) 1 calc PR B 1 C30 C 0.4359(6) -0.0348(9) 0.8117(5) 0.0229(8) Uani 0.490(4) 1 d PDU B 1 H30A H 0.4481 -0.1236 0.8040 0.028 Uiso 0.490(4) 1 calc PR B 1 H30B H 0.5170 -0.0420 0.8568 0.028 Uiso 0.490(4) 1 calc PR B 1 C31 C 0.43196(16) 0.08007(13) 0.69628(11) 0.0237(3) Uani 1 1 d D . . C34 C 0.57688(19) 0.02792(18) 0.65430(16) 0.0385(4) Uani 1 1 d . B . H34A H 0.5882 0.0930 0.5806 0.058 Uiso 1 1 calc R . . H34B H 0.5828 -0.0615 0.6511 0.058 Uiso 1 1 calc R . . H34C H 0.6518 0.0190 0.7045 0.058 Uiso 1 1 calc R . . C35 C 0.31691(18) 0.09152(16) 0.61734(13) 0.0306(3) Uani 1 1 d . B . H35A H 0.2244 0.1319 0.6394 0.046 Uiso 1 1 calc R . . H35B H 0.3191 0.0002 0.6198 0.046 Uiso 1 1 calc R . . H35C H 0.3335 0.1498 0.5423 0.046 Uiso 1 1 calc R . . C46 C 0.1599(6) 0.2423(4) 0.9734(11) 0.0220(8) Uani 0.510(4) 1 d PDU B 2 C52 C 0.2298(11) 0.2935(13) 1.0456(12) 0.0249(16) Uani 0.510(4) 1 d PD B 2 H52A H 0.2427 0.2260 1.1213 0.037 Uiso 0.510(4) 1 calc PR B 2 H52B H 0.1693 0.3808 1.0446 0.037 Uiso 0.510(4) 1 calc PR B 2 H52C H 0.3217 0.3064 1.0169 0.037 Uiso 0.510(4) 1 calc PR B 2 C53 C 0.0090(4) 0.2392(5) 1.0119(4) 0.0343(10) Uani 0.510(4) 1 d PD B 2 H53A H -0.0441 0.3311 1.0056 0.051 Uiso 0.510(4) 1 calc PR B 2 H53B H 0.0130 0.1759 1.0887 0.051 Uiso 0.510(4) 1 calc PR B 2 H53C H -0.0379 0.2085 0.9657 0.051 Uiso 0.510(4) 1 calc PR B 2 C47 C 0.2471(3) 0.0962(3) 0.9872(2) 0.0229(7) Uani 0.510(4) 1 d PD B 2 H47A H 0.3441 0.1013 0.9643 0.027 Uiso 0.510(4) 1 calc PR B 2 H47B H 0.2535 0.0377 1.0665 0.027 Uiso 0.510(4) 1 calc PR B 2 C48 C 0.1944(3) 0.0266(3) 0.9262(2) 0.0270(7) Uani 0.510(4) 1 d PD B 2 H48 H 0.1017 0.0149 0.9414 0.032 Uiso 0.510(4) 1 calc PR B 2 C49 C 0.2621(4) -0.0215(4) 0.8523(3) 0.0248(8) Uani 0.510(4) 1 d PD B 2 H49 H 0.2109 -0.0624 0.8211 0.030 Uiso 0.510(4) 1 calc PR B 2 C50 C 0.4069(5) -0.0194(9) 0.8128(5) 0.0229(8) Uani 0.510(4) 1 d PDU B 2 H50A H 0.4546 -0.1132 0.8177 0.028 Uiso 0.510(4) 1 calc PR B 2 H50B H 0.4572 -0.0011 0.8663 0.028 Uiso 0.510(4) 1 calc PR B 2 C60 C 0.2182(9) 0.7571(9) 0.6262(6) 0.019(2) Uiso 0.152(4) 1 d PD A 2 H60A H 0.3003 0.7168 0.5912 0.023 Uiso 0.152(4) 1 calc PR A 2 H60B H 0.1904 0.8568 0.5828 0.023 Uiso 0.152(4) 1 calc PR A 2 C59 C 0.2629(8) 0.7345(9) 0.7391(6) 0.020(2) Uiso 0.152(4) 1 d PD A 2 H59 H 0.1921 0.7698 0.7805 0.024 Uiso 0.152(4) 1 calc PR A 2 C58 C 0.3899(8) 0.6708(13) 0.7901(10) 0.028(3) Uiso 0.152(4) 1 d PD A 2 H58 H 0.4001 0.6693 0.8620 0.034 Uiso 0.152(4) 1 calc PR A 2 C64 C -0.0435(13) 0.7722(14) 0.6549(11) 0.031(3) Uiso 0.152(4) 1 d PD A 2 H64A H -0.1199 0.7311 0.6513 0.047 Uiso 0.152(4) 1 calc PR A 2 H64B H -0.0673 0.8687 0.6052 0.047 Uiso 0.152(4) 1 calc PR A 2 H64C H -0.0309 0.7655 0.7304 0.047 Uiso 0.152(4) 1 calc PR A 2 C57 C 0.5168(16) 0.6023(3) 0.7463(15) 0.0294(5) Uani 0.152(4) 1 d PD A 2 H57A H 0.5925 0.6449 0.7510 0.035 Uiso 0.152(4) 1 calc PR A 2 H57B H 0.4951 0.6301 0.6669 0.035 Uiso 0.152(4) 1 calc PR A 2 C61 C 0.0942(11) 0.6958(18) 0.6200(13) 0.0233(13) Uani 0.152(4) 1 d PDU A 2 C65 C 0.0720(14) 0.7153(16) 0.4994(12) 0.018(3) Uiso 0.152(4) 1 d PD A 2 H65A H 0.1557 0.6620 0.4765 0.027 Uiso 0.152(4) 1 calc PR A 2 H65B H 0.0569 0.8124 0.4524 0.027 Uiso 0.152(4) 1 calc PR A 2 H65C H -0.0107 0.6839 0.4924 0.027 Uiso 0.152(4) 1 calc PR A 2 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 0.01516(9) 0.01772(10) 0.01464(9) -0.00561(7) 0.00222(6) -0.00484(7) C1 0.0164(6) 0.0229(6) 0.0220(6) -0.0110(5) 0.0061(5) -0.0072(5) C2 0.0157(6) 0.0214(6) 0.0192(6) -0.0083(5) 0.0026(5) -0.0039(5) C3 0.0189(6) 0.0212(6) 0.0194(6) -0.0098(5) 0.0035(5) -0.0051(5) C4 0.0230(6) 0.0239(6) 0.0167(6) -0.0095(5) 0.0048(5) -0.0071(5) C5 0.0217(6) 0.0222(6) 0.0184(6) -0.0074(5) 0.0073(5) -0.0087(5) C6 0.0223(7) 0.0277(7) 0.0273(7) -0.0131(6) 0.0029(5) -0.0108(6) C7 0.0307(13) 0.0324(8) 0.0340(9) -0.0149(7) 0.0049(10) -0.0199(7) C8 0.0358(11) 0.0252(9) 0.0300(11) -0.0123(8) 0.0033(8) -0.0134(8) C9 0.0360(10) 0.0234(8) 0.0350(10) -0.0134(7) -0.0001(8) -0.0102(7) C10 0.0373(10) 0.0193(8) 0.0256(9) -0.0064(7) -0.0008(7) -0.0063(7) C14 0.0281(11) 0.0261(10) 0.0391(12) -0.0054(9) -0.0039(9) 0.0018(8) C11 0.0249(9) 0.0199(7) 0.0213(8) -0.0041(6) -0.0019(7) -0.0036(7) C15 0.0378(14) 0.0245(10) 0.0220(10) -0.0020(7) -0.0056(10) -0.0104(10) C12 0.0283(7) 0.0327(8) 0.0279(7) -0.0156(6) -0.0008(6) -0.0094(6) C13 0.0251(8) 0.0597(11) 0.0470(10) -0.0300(9) 0.0091(7) -0.0211(8) C21 0.0163(6) 0.0210(6) 0.0194(6) -0.0054(5) 0.0043(5) -0.0042(5) C22 0.0173(6) 0.0206(6) 0.0180(6) -0.0075(5) 0.0031(5) -0.0033(5) C23 0.0161(6) 0.0208(6) 0.0202(6) -0.0057(5) 0.0006(5) -0.0032(5) C24 0.0172(6) 0.0236(6) 0.0212(6) -0.0062(5) -0.0017(5) -0.0047(5) C25 0.0163(6) 0.0224(6) 0.0251(7) -0.0078(5) 0.0023(5) -0.0067(5) C26 0.0213(18) 0.0212(12) 0.0200(11) -0.0053(12) 0.0036(19) -0.0028(12) C32 0.038(4) 0.023(4) 0.018(2) -0.008(2) 0.007(2) -0.003(3) C33 0.0266(19) 0.034(2) 0.0282(18) -0.007(2) 0.0135(14) -0.006(2) C27 0.035(2) 0.0236(15) 0.0256(16) -0.0037(12) 0.0074(14) -0.0097(14) C28 0.0370(18) 0.0178(14) 0.0207(14) -0.0024(12) 0.0005(13) -0.0048(12) C29 0.036(2) 0.0149(16) 0.0288(18) -0.0052(12) -0.0031(17) -0.0077(16) C30 0.0214(17) 0.0140(19) 0.0281(12) -0.0060(11) -0.0073(13) 0.0033(16) C31 0.0283(7) 0.0202(6) 0.0236(7) -0.0103(5) -0.0012(5) -0.0045(5) C34 0.0392(9) 0.0294(8) 0.0479(10) -0.0208(8) 0.0058(8) -0.0019(7) C35 0.0433(9) 0.0237(7) 0.0276(7) -0.0109(6) -0.0076(7) -0.0094(7) C46 0.0169(18) 0.0233(12) 0.0186(11) -0.0022(12) 0.0064(18) -0.0031(12) C52 0.029(3) 0.027(5) 0.015(2) -0.008(2) 0.002(2) -0.002(2) C53 0.0264(19) 0.035(2) 0.0286(18) -0.0031(19) 0.0117(14) -0.0033(19) C47 0.0207(16) 0.0219(14) 0.0190(13) -0.0016(11) 0.0050(11) -0.0037(12) C48 0.0223(14) 0.0221(14) 0.0299(15) -0.0006(11) 0.0022(11) -0.0091(11) C49 0.0274(19) 0.0182(16) 0.0291(17) -0.0056(12) 0.0009(15) -0.0113(13) C50 0.0214(19) 0.0141(18) 0.0290(12) -0.0062(11) -0.0079(14) 0.0017(15) C57 0.0307(13) 0.0324(8) 0.0340(9) -0.0149(7) 0.0049(10) -0.0199(7) C61 0.0232(19) 0.0193(18) 0.0226(19) -0.0038(18) -0.0015(18) -0.0033(18) _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 C1 2.1026(13) . ? Fe1 C2 2.0785(13) . ? Fe1 C3 2.0827(13) . ? Fe1 C4 2.0378(13) . ? Fe1 C5 2.0531(13) . ? Fe1 C21 2.0873(13) . ? Fe1 C22 2.0732(13) . ? Fe1 C23 2.0858(13) . ? Fe1 C24 2.0434(13) . ? Fe1 C25 2.0543(13) . ? C1 C2 1.4317(18) . ? C1 C5 1.4248(19) . ? C1 C6 1.5191(19) . ? C2 C3 1.4295(18) . ? C3 C4 1.4302(19) . ? C3 C31 1.5212(18) . ? C4 C5 1.4229(19) . ? C6 C7 1.5516(16) . ? C6 C12 1.527(2) . ? C6 C13 1.549(2) . ? C6 C57 1.5523(19) . ? C7 C8 1.4846(18) . ? C8 C9 1.340(2) . ? C9 C10 1.4840(18) . ? C10 C11 1.5515(17) . ? C14 C11 1.5402(17) . ? C11 C15 1.5389(16) . ? C11 C23 1.519(4) . ? C21 C22 1.4328(19) . ? C21 C25 1.4305(19) . ? C21 C26 1.515(12) . ? C21 C46 1.533(12) . ? C22 C23 1.4314(18) . ? C23 C24 1.4261(19) . ? C23 C61 1.543(19) . ? C24 C25 1.4207(19) . ? C26 C32 1.5381(19) . ? C26 C33 1.5389(19) . ? C26 C27 1.5524(18) . ? C27 C28 1.484(2) . ? C28 C29 1.337(3) . ? C29 C30 1.484(2) . ? C30 C31 1.5533(18) . ? C31 C34 1.542(2) . ? C31 C35 1.530(2) . ? C31 C50 1.5539(18) . ? C46 C52 1.5380(19) . ? C46 C53 1.5391(19) . ? C46 C47 1.5520(18) . ? C47 C48 1.485(2) . ? C48 C49 1.338(3) . ? C49 C50 1.485(2) . ? C60 C59 1.484(2) . ? C60 C61 1.5522(19) . ? C59 C58 1.338(3) . ? C58 C57 1.484(2) . ? C64 C61 1.539(2) . ? C61 C65 1.539(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # C7 C6 C57 12.3(6) . . ? # C26 C21 C46 8.2(3) . . ? # C11 C23 C61 7.3(4) . . ? # C30 C31 C50 10.9(3) . . ? C2 Fe1 C1 40.04(5) . . ? C2 Fe1 C3 40.18(5) . . ? C2 Fe1 C21 112.76(5) . . ? C2 Fe1 C23 160.72(5) . . ? C3 Fe1 C1 68.07(5) . . ? C3 Fe1 C21 122.95(5) . . ? C3 Fe1 C23 156.41(5) . . ? C4 Fe1 C1 68.01(5) . . ? C4 Fe1 C2 67.48(5) . . ? C4 Fe1 C3 40.60(5) . . ? C4 Fe1 C5 40.71(5) . . ? C4 Fe1 C21 155.24(6) . . ? C4 Fe1 C22 158.88(5) . . ? C4 Fe1 C23 120.30(5) . . ? C4 Fe1 C24 102.60(6) . . ? C4 Fe1 C25 117.82(6) . . ? C5 Fe1 C1 40.08(5) . . ? C5 Fe1 C2 67.18(5) . . ? C5 Fe1 C3 68.21(5) . . ? C5 Fe1 C21 163.95(5) . . ? C5 Fe1 C22 126.03(5) . . ? C5 Fe1 C23 106.29(5) . . ? C5 Fe1 C25 153.28(6) . . ? C21 Fe1 C1 129.36(5) . . ? C22 Fe1 C1 112.91(5) . . ? C22 Fe1 C2 127.83(5) . . ? C22 Fe1 C3 160.51(5) . . ? C22 Fe1 C21 40.29(5) . . ? C22 Fe1 C23 40.26(5) . . ? C23 Fe1 C1 123.39(5) . . ? C23 Fe1 C21 68.22(5) . . ? C24 Fe1 C1 155.44(6) . . ? C24 Fe1 C2 158.87(6) . . ? C24 Fe1 C3 120.34(5) . . ? C24 Fe1 C5 118.24(6) . . ? C24 Fe1 C21 68.07(5) . . ? C24 Fe1 C22 67.48(5) . . ? C24 Fe1 C23 40.39(5) . . ? C24 Fe1 C25 40.57(5) . . ? C25 Fe1 C1 163.93(5) . . ? C25 Fe1 C2 126.00(5) . . ? C25 Fe1 C3 105.89(5) . . ? C25 Fe1 C21 40.40(5) . . ? C25 Fe1 C22 67.56(5) . . ? C25 Fe1 C23 68.16(5) . . ? C2 C1 Fe1 69.07(7) . . ? C2 C1 C6 125.08(12) . . ? C5 C1 Fe1 68.09(7) . . ? C5 C1 C2 106.30(11) . . ? C5 C1 C6 126.78(12) . . ? C6 C1 Fe1 139.43(9) . . ? C1 C2 Fe1 70.88(8) . . ? C3 C2 Fe1 70.06(8) . . ? C3 C2 C1 109.92(12) . . ? C2 C3 Fe1 69.75(7) . . ? C2 C3 C4 106.18(11) . . ? C2 C3 C31 127.64(12) . . ? C4 C3 Fe1 68.01(7) . . ? C4 C3 C31 124.81(12) . . ? C31 C3 Fe1 137.06(10) . . ? C3 C4 Fe1 71.39(7) . . ? C5 C4 Fe1 70.23(7) . . ? C5 C4 C3 108.74(12) . . ? C1 C5 Fe1 71.83(7) . . ? C4 C5 Fe1 69.07(7) . . ? C4 C5 C1 108.84(12) . . ? C1 C6 C7 113.94(15) . . ? C1 C6 C12 112.18(11) . . ? C1 C6 C13 105.94(12) . . ? C1 C6 C57 105.8(9) . . ? C12 C6 C7 111.06(16) . . ? C12 C6 C13 108.32(13) . . ? C12 C6 C57 107.9(7) . . ? C13 C6 C7 104.85(13) . . ? C13 C6 C57 116.7(5) . . ? C8 C7 C6 111.73(14) . . ? C9 C8 C7 121.9(2) . . ? C8 C9 C10 123.94(18) . . ? C9 C10 C11 113.33(15) . . ? C14 C11 C10 107.05(18) . . ? C15 C11 C10 109.73(19) . . ? C15 C11 C14 109.0(2) . . ? C23 C11 C10 112.97(19) . . ? C23 C11 C14 106.47(16) . . ? C23 C11 C15 111.40(17) . . ? C22 C21 Fe1 69.33(7) . . ? C22 C21 C26 125.0(3) . . ? C22 C21 C46 125.6(3) . . ? C25 C21 Fe1 68.56(7) . . ? C25 C21 C22 106.55(12) . . ? C25 C21 C26 126.4(3) . . ? C25 C21 C46 127.5(3) . . ? C26 C21 Fe1 139.7(2) . . ? C46 C21 Fe1 131.46(16) . . ? C21 C22 Fe1 70.38(7) . . ? C23 C22 Fe1 70.34(7) . . ? C23 C22 C21 109.58(12) . . ? C11 C23 Fe1 138.06(11) . . ? C22 C23 Fe1 69.40(7) . . ? C22 C23 C11 127.28(14) . . ? C22 C23 C61 129.7(4) . . ? C24 C23 Fe1 68.20(8) . . ? C24 C23 C11 124.84(13) . . ? C24 C23 C22 106.30(12) . . ? C24 C23 C61 123.8(4) . . ? C61 C23 Fe1 130.9(4) . . ? C23 C24 Fe1 71.40(8) . . ? C25 C24 Fe1 70.13(8) . . ? C25 C24 C23 109.18(12) . . ? C21 C25 Fe1 71.04(8) . . ? C24 C25 Fe1 69.30(8) . . ? C24 C25 C21 108.37(12) . . ? C21 C26 C32 109.4(7) . . ? C21 C26 C33 109.3(6) . . ? C21 C26 C27 113.8(7) . . ? C32 C26 C33 108.8(8) . . ? C32 C26 C27 108.9(8) . . ? C33 C26 C27 106.5(3) . . ? C28 C27 C26 113.2(3) . . ? C29 C28 C27 124.5(3) . . ? C28 C29 C30 122.5(7) . . ? C29 C30 C31 109.7(3) . . ? C3 C31 C30 115.4(5) . . ? C3 C31 C34 105.90(12) . . ? C3 C31 C35 111.30(11) . . ? C3 C31 C50 111.3(5) . . ? C34 C31 C30 101.24(19) . . ? C34 C31 C50 112.1(2) . . ? C35 C31 C30 113.6(5) . . ? C35 C31 C34 108.46(13) . . ? C35 C31 C50 107.9(4) . . ? C21 C46 C52 111.7(6) . . ? C21 C46 C53 105.5(6) . . ? C21 C46 C47 112.2(6) . . ? C52 C46 C53 108.3(8) . . ? C52 C46 C47 108.9(7) . . ? C53 C46 C47 110.1(3) . . ? C48 C47 C46 117.3(5) . . ? C49 C48 C47 127.6(3) . . ? C48 C49 C50 128.6(5) . . ? C49 C50 C31 121.3(3) . . ? C59 C60 C61 115.0(8) . . ? C58 C59 C60 128.3(9) . . ? C59 C58 C57 126.9(12) . . ? C58 C57 C6 125.2(8) . . ? C23 C61 C60 114.0(10) . . ? C64 C61 C23 104.6(9) . . ? C64 C61 C60 110.8(10) . . ? C65 C61 C23 111.5(9) . . ? C65 C61 C60 108.1(9) . . ? C65 C61 C64 107.6(12) . . ? data_b_f7 _database_code_depnum_ccdc_archive 'CCDC 882867' #TrackingRef '- B_f7.cif' _audit_creation_date 2012-01-17 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H42 Fe' _chemical_formula_sum 'C30 H42 Fe' _chemical_formula_weight 458.49 _chemical_melting_point ? 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.8085(2) _cell_length_b 10.9220(2) _cell_length_c 13.2038(3) _cell_angle_alpha 67.2990(19) _cell_angle_beta 85.9538(17) _cell_angle_gamma 75.7027(18) _cell_volume 1264.02(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 41307 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 31.7022 _cell_measurement_theta_min 3.1904 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.545 _exptl_crystal_size_mid 0.289 _exptl_crystal_size_min 0.082 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 112046 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_theta_max 31.77 _diffrn_reflns_theta_min 3.20 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 10.3347 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -93.00 -67.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 154.0000 58.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -76.00 -46.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 129.0000 3.0000 30 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 58.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 77.0000 -30.0000 78 #__ type_ start__ end____ width___ exp.time_ 4 omega -72.00 -38.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 -179.0000 -30.0000 34 #__ type_ start__ end____ width___ exp.time_ 5 omega -93.00 -49.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 154.0000 -72.0000 44 #__ type_ start__ end____ width___ exp.time_ 6 omega -54.00 22.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -57.0000 -90.0000 76 #__ type_ start__ end____ width___ exp.time_ 7 omega -57.00 50.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -77.0000 -180.0000 107 #__ type_ start__ end____ width___ exp.time_ 8 omega 39.00 75.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 38.0000 -30.0000 36 #__ type_ start__ end____ width___ exp.time_ 9 omega 56.00 98.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 179.0000 60.0000 42 #__ type_ start__ end____ width___ exp.time_ 10 omega -11.00 95.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 77.0000 30.0000 106 #__ type_ start__ end____ width___ exp.time_ 11 omega 4.00 95.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 77.0000 -120.0000 91 #__ type_ start__ end____ width___ exp.time_ 12 omega 30.00 58.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -99.0000 60.0000 28 #__ type_ start__ end____ width___ exp.time_ 13 omega 17.00 45.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -69.0000 70.0000 28 #__ type_ start__ end____ width___ exp.time_ 14 omega -12.00 90.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 57.0000 -180.0000 102 #__ type_ start__ end____ width___ exp.time_ 15 omega 42.00 75.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -124.0000 -56.0000 33 #__ type_ start__ end____ width___ exp.time_ 16 omega -92.00 11.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 -38.0000 -60.0000 103 #__ type_ start__ end____ width___ exp.time_ 17 omega -106.00 -34.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 -179.0000 0.0000 72 #__ type_ start__ end____ width___ exp.time_ 18 omega -90.00 14.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 -57.0000 -150.0000 104 #__ type_ start__ end____ width___ exp.time_ 19 omega -106.00 -34.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.7963 -179.0000 -180.0000 72 #__ type_ start__ end____ width___ exp.time_ 20 omega 56.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 179.0000 -180.0000 50 #__ type_ start__ end____ width___ exp.time_ 21 omega -10.00 92.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 38.0000 -120.0000 102 #__ type_ start__ end____ width___ exp.time_ 22 omega 53.00 105.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -179.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 23 omega -4.00 58.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -99.0000 30.0000 62 #__ type_ start__ end____ width___ exp.time_ 24 omega -60.00 43.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 -38.0000 -180.0000 103 #__ type_ start__ end____ width___ exp.time_ 25 omega -16.00 92.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 69.0000 109.0000 108 #__ type_ start__ end____ width___ exp.time_ 26 omega -13.00 90.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 57.0000 -60.0000 103 #__ type_ start__ end____ width___ exp.time_ 27 omega 17.00 75.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -124.0000 -56.0000 58 #__ type_ start__ end____ width___ exp.time_ 28 omega -10.00 92.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 38.0000 -180.0000 102 #__ type_ start__ end____ width___ exp.time_ 29 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -180.0000 179 #__ type_ start__ end____ width___ exp.time_ 30 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -150.0000 179 #__ type_ start__ end____ width___ exp.time_ 31 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -120.0000 179 #__ type_ start__ end____ width___ exp.time_ 32 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -90.0000 179 #__ type_ start__ end____ width___ exp.time_ 33 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -60.0000 179 #__ type_ start__ end____ width___ exp.time_ 34 omega -73.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 -30.0000 179 #__ type_ start__ end____ width___ exp.time_ 35 omega -73.00 -8.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 0.0000 0.0000 65 #__ type_ start__ end____ width___ exp.time_ 36 omega 56.00 106.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.1088 179.0000 -90.0000 50 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0281362000 _diffrn_orient_matrix_UB_12 0.0696909000 _diffrn_orient_matrix_UB_13 -0.0331151000 _diffrn_orient_matrix_UB_21 0.0619450000 _diffrn_orient_matrix_UB_22 0.0009019000 _diffrn_orient_matrix_UB_23 -0.0311617000 _diffrn_orient_matrix_UB_31 -0.0307315000 _diffrn_orient_matrix_UB_32 -0.0199400000 _diffrn_orient_matrix_UB_33 -0.0364105000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_current 40 _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6952 _reflns_number_total 7975 _reflns_threshold_expression I>2u(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.635 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 394 _refine_ls_number_reflns 7975 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0379 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.5416P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.0957 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.286214(18) 0.374498(17) 0.729092(14) 0.01756(6) Uani 1 1 d . A . C1 C 0.49565(13) 0.38651(13) 0.73764(10) 0.0208(2) Uani 1 1 d . A . C2 C 0.48571(13) 0.24707(13) 0.78016(10) 0.0209(2) Uani 1 1 d . . . H2 H 0.5124 0.1831 0.8527 0.025 Uiso 1 1 calc R . . C3 C 0.42936(13) 0.21862(13) 0.69665(10) 0.0214(2) Uani 1 1 d . A . C4 C 0.40097(14) 0.34376(13) 0.60230(10) 0.0220(2) Uani 1 1 d . . . H4 H 0.3616 0.3568 0.5342 0.026 Uiso 1 1 calc R . . C5 C 0.44159(13) 0.44590(13) 0.62737(10) 0.0219(2) Uani 1 1 d . . . H5 H 0.4339 0.5381 0.5787 0.026 Uiso 1 1 calc R . . C6 C 0.58196(14) 0.44524(13) 0.79045(11) 0.0254(3) Uani 1 1 d D . . C7 C 0.54784(19) 0.60342(14) 0.7418(2) 0.0299(4) Uani 0.901(3) 1 d PDU A 1 H7A H 0.6060 0.6346 0.7809 0.036 Uiso 0.901(3) 1 calc PR A 1 H7B H 0.5731 0.6356 0.6635 0.036 Uiso 0.901(3) 1 calc PR A 1 C8 C 0.39702(16) 0.66526(16) 0.75071(17) 0.0286(4) Uani 0.901(3) 1 d PD A 1 H8 H 0.3607 0.6550 0.8214 0.034 Uiso 0.901(3) 1 calc PR A 1 C9 C 0.31017(15) 0.73508(15) 0.66244(14) 0.0299(4) Uani 0.901(3) 1 d PD A 1 H9 H 0.3510 0.7602 0.5921 0.036 Uiso 0.901(3) 1 calc PR A 1 C10 C 0.15464(15) 0.77573(15) 0.66711(14) 0.0295(4) Uani 0.901(3) 1 d PD A 1 H10A H 0.1218 0.8742 0.6214 0.035 Uiso 0.901(3) 1 calc PR A 1 H10B H 0.1284 0.7624 0.7438 0.035 Uiso 0.901(3) 1 calc PR A 1 C14 C -0.08057(19) 0.74654(19) 0.63728(17) 0.0377(4) Uani 0.901(3) 1 d PD A 1 H14A H -0.1327 0.6986 0.6106 0.057 Uiso 0.901(3) 1 calc PR A 1 H14B H -0.1085 0.8449 0.5934 0.057 Uiso 0.901(3) 1 calc PR A 1 H14C H -0.1017 0.7298 0.7145 0.057 Uiso 0.901(3) 1 calc PR A 1 C11 C 0.07852(17) 0.6937(2) 0.62676(18) 0.0254(3) Uani 0.901(3) 1 d PDU A 1 C15 C 0.1100(3) 0.7198(2) 0.50543(15) 0.0331(4) Uani 0.901(3) 1 d PD A 1 H15A H 0.2090 0.6777 0.4990 0.050 Uiso 0.901(3) 1 calc PR A 1 H15B H 0.0911 0.8185 0.4628 0.050 Uiso 0.901(3) 1 calc PR A 1 H15C H 0.0498 0.6798 0.4773 0.050 Uiso 0.901(3) 1 calc PR A 1 C12 C 0.57106(15) 0.39056(15) 0.91552(12) 0.0283(3) Uani 1 1 d . A . H12A H 0.4730 0.4174 0.9350 0.043 Uiso 1 1 calc R . . H12B H 0.6304 0.4286 0.9463 0.043 Uiso 1 1 calc R . . H12C H 0.6027 0.2907 0.9454 0.043 Uiso 1 1 calc R . . C13 C 0.73664(16) 0.3984(2) 0.76194(15) 0.0395(4) Uani 1 1 d . A . H13A H 0.7667 0.2985 0.7952 0.059 Uiso 1 1 calc R . . H13B H 0.7967 0.4381 0.7905 0.059 Uiso 1 1 calc R . . H13C H 0.7446 0.4290 0.6820 0.059 Uiso 1 1 calc R . . C21 C 0.13837(13) 0.33910(13) 0.85289(10) 0.0213(2) Uani 1 1 d . . . C22 C 0.14910(13) 0.47859(13) 0.81217(10) 0.0207(2) Uani 1 1 d . A . H22 H 0.1756 0.5222 0.8550 0.025 Uiso 1 1 calc R . . C23 C 0.11380(13) 0.54199(13) 0.69710(10) 0.0212(2) Uani 1 1 d . . . C24 C 0.08464(13) 0.43874(13) 0.66650(11) 0.0235(2) Uani 1 1 d . A . H24 H 0.0598 0.4504 0.5945 0.028 Uiso 1 1 calc R . . C25 C 0.09888(13) 0.31570(13) 0.76111(11) 0.0228(2) Uani 1 1 d . A . H25 H 0.0845 0.2320 0.7629 0.027 Uiso 1 1 calc R . . C26 C 0.1323(3) 0.2507(3) 0.9732(6) 0.0239(5) Uani 0.717(4) 1 d PDU B 1 C32 C 0.2413(7) 0.2680(7) 1.0418(7) 0.0275(9) Uani 0.717(4) 1 d PDU B 1 H32A H 0.3357 0.2434 1.0149 0.041 Uiso 0.717(4) 1 calc PR B 1 H32B H 0.2370 0.2083 1.1190 0.041 Uiso 0.717(4) 1 calc PR B 1 H32C H 0.2205 0.3633 1.0352 0.041 Uiso 0.717(4) 1 calc PR B 1 C33 C -0.0149(3) 0.2962(3) 1.0143(2) 0.0345(5) Uani 0.717(4) 1 d PD B 1 H33A H -0.0338 0.3935 1.0016 0.052 Uiso 0.717(4) 1 calc PR B 1 H33B H -0.0189 0.2428 1.0931 0.052 Uiso 0.717(4) 1 calc PR B 1 H33C H -0.0858 0.2814 0.9744 0.052 Uiso 0.717(4) 1 calc PR B 1 C27 C 0.1545(2) 0.09722(17) 0.99466(17) 0.0317(5) Uani 0.717(4) 1 d PD B 1 H27A H 0.1523 0.0451 1.0747 0.038 Uiso 0.717(4) 1 calc PR B 1 H27B H 0.0756 0.0852 0.9595 0.038 Uiso 0.717(4) 1 calc PR B 1 C28 C 0.2890(2) 0.03996(19) 0.95249(16) 0.0293(5) Uani 0.717(4) 1 d PD B 1 H28 H 0.3745 0.0336 0.9859 0.035 Uiso 0.717(4) 1 calc PR B 1 C29 C 0.2963(3) -0.0033(3) 0.8696(2) 0.0331(6) Uani 0.717(4) 1 d PD B 1 H29 H 0.2126 -0.0155 0.8466 0.040 Uiso 0.717(4) 1 calc PR B 1 C30 C 0.4280(3) -0.0331(5) 0.8119(3) 0.0280(6) Uani 0.717(4) 1 d PDU B 1 H30A H 0.4380 -0.1218 0.8047 0.034 Uiso 0.717(4) 1 calc PR B 1 H30B H 0.5093 -0.0415 0.8566 0.034 Uiso 0.717(4) 1 calc PR B 1 C31 C 0.43036(15) 0.07938(12) 0.69638(10) 0.0258(3) Uani 1 1 d D . . C34 C 0.57491(19) 0.02926(17) 0.65225(15) 0.0403(4) Uani 1 1 d . B . H34A H 0.5855 0.0947 0.5782 0.060 Uiso 1 1 calc R . . H34B H 0.5806 -0.0603 0.6496 0.060 Uiso 1 1 calc R . . H34C H 0.6502 0.0216 0.7009 0.060 Uiso 1 1 calc R . . C35 C 0.31512(18) 0.09040(15) 0.61876(13) 0.0343(3) Uani 1 1 d . B . H35A H 0.2231 0.1291 0.6420 0.051 Uiso 1 1 calc R . . H35B H 0.3171 -0.0007 0.6208 0.051 Uiso 1 1 calc R . . H35C H 0.3315 0.1498 0.5438 0.051 Uiso 1 1 calc R . . C46 C 0.1588(8) 0.2368(6) 0.9745(15) 0.0248(11) Uani 0.283(4) 1 d PDU B 2 C52 C 0.228(2) 0.2930(18) 1.0429(19) 0.027(2) Uani 0.283(4) 1 d PDU B 2 H52A H 0.2392 0.2281 1.1195 0.041 Uiso 0.283(4) 1 calc PR B 2 H52B H 0.1675 0.3809 1.0393 0.041 Uiso 0.283(4) 1 calc PR B 2 H52C H 0.3199 0.3057 1.0136 0.041 Uiso 0.283(4) 1 calc PR B 2 C53 C 0.0073(6) 0.2318(8) 1.0114(5) 0.0359(14) Uani 0.283(4) 1 d PD B 2 H53A H -0.0481 0.3244 0.9995 0.054 Uiso 0.283(4) 1 calc PR B 2 H53B H 0.0086 0.1738 1.0896 0.054 Uiso 0.283(4) 1 calc PR B 2 H53C H -0.0352 0.1941 0.9687 0.054 Uiso 0.283(4) 1 calc PR B 2 C47 C 0.2457(5) 0.0926(4) 0.9863(3) 0.0237(11) Uani 0.283(4) 1 d PD B 2 H47A H 0.3423 0.1000 0.9623 0.028 Uiso 0.283(4) 1 calc PR B 2 H47B H 0.2527 0.0333 1.0654 0.028 Uiso 0.283(4) 1 calc PR B 2 C48 C 0.1945(5) 0.0218(5) 0.9262(4) 0.0280(12) Uani 0.283(4) 1 d PD B 2 H48 H 0.1023 0.0081 0.9424 0.034 Uiso 0.283(4) 1 calc PR B 2 C49 C 0.2624(7) -0.0251(7) 0.8518(6) 0.0299(15) Uani 0.283(4) 1 d PD B 2 H49 H 0.2120 -0.0661 0.8202 0.036 Uiso 0.283(4) 1 calc PR B 2 C50 C 0.4075(7) -0.0201(16) 0.8137(7) 0.0280(11) Uani 0.283(4) 1 d PDU B 2 H50A H 0.4575 -0.1134 0.8199 0.034 Uiso 0.283(4) 1 calc PR B 2 H50B H 0.4550 0.0020 0.8659 0.034 Uiso 0.283(4) 1 calc PR B 2 C60 C 0.2186(11) 0.7556(11) 0.6247(7) 0.012(2) Uiso 0.099(3) 1 d PD A 2 H60A H 0.3011 0.7158 0.5901 0.015 Uiso 0.099(3) 1 calc PR A 2 H60B H 0.1918 0.8551 0.5808 0.015 Uiso 0.099(3) 1 calc PR A 2 C59 C 0.2619(10) 0.7348(11) 0.7368(7) 0.015(2) Uiso 0.099(3) 1 d PD A 2 H59 H 0.1915 0.7723 0.7770 0.018 Uiso 0.099(3) 1 calc PR A 2 C58 C 0.3872(10) 0.6700(15) 0.7887(12) 0.021(3) Uiso 0.099(3) 1 d PD A 2 H58 H 0.3938 0.6680 0.8608 0.026 Uiso 0.099(3) 1 calc PR A 2 C64 C -0.0398(16) 0.7692(15) 0.6559(13) 0.023(3) Uiso 0.099(3) 1 d PD A 2 H64A H -0.1131 0.7188 0.6667 0.035 Uiso 0.099(3) 1 calc PR A 2 H64B H -0.0721 0.8612 0.5998 0.035 Uiso 0.099(3) 1 calc PR A 2 H64C H -0.0202 0.7758 0.7251 0.035 Uiso 0.099(3) 1 calc PR A 2 C57 C 0.517(2) 0.6011(4) 0.749(2) 0.0301(14) Uani 0.099(3) 1 d PDU A 2 H57A H 0.5921 0.6422 0.7581 0.036 Uiso 0.099(3) 1 calc PR A 2 H57B H 0.5013 0.6315 0.6687 0.036 Uiso 0.099(3) 1 calc PR A 2 C61 C 0.0952(13) 0.693(2) 0.6182(17) 0.0249(14) Uani 0.099(3) 1 d PDU A 2 C65 C 0.0698(17) 0.7164(19) 0.4979(15) 0.018(4) Uiso 0.099(3) 1 d PD A 2 H65A H 0.1526 0.6664 0.4721 0.027 Uiso 0.099(3) 1 calc PR A 2 H65B H 0.0530 0.8142 0.4524 0.027 Uiso 0.099(3) 1 calc PR A 2 H65C H -0.0125 0.6832 0.4925 0.027 Uiso 0.099(3) 1 calc PR A 2 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 0.01918(9) 0.01727(9) 0.01731(9) -0.00674(6) 0.00224(6) -0.00649(6) C1 0.0200(5) 0.0227(6) 0.0234(6) -0.0118(5) 0.0055(4) -0.0077(4) C2 0.0207(5) 0.0212(5) 0.0217(6) -0.0096(5) 0.0029(4) -0.0051(4) C3 0.0247(6) 0.0201(5) 0.0215(6) -0.0098(5) 0.0040(4) -0.0068(4) C4 0.0283(6) 0.0227(6) 0.0185(5) -0.0101(5) 0.0049(5) -0.0095(5) C5 0.0247(6) 0.0221(6) 0.0210(6) -0.0092(5) 0.0075(4) -0.0098(5) C6 0.0231(6) 0.0282(6) 0.0305(7) -0.0150(5) 0.0026(5) -0.0101(5) C7 0.0325(11) 0.0312(7) 0.0343(9) -0.0152(6) 0.0049(8) -0.0190(6) C8 0.0352(9) 0.0240(8) 0.0315(9) -0.0124(7) 0.0027(7) -0.0131(6) C9 0.0382(9) 0.0213(7) 0.0335(8) -0.0108(6) 0.0004(6) -0.0122(6) C10 0.0385(9) 0.0185(6) 0.0293(8) -0.0062(6) -0.0026(7) -0.0069(6) C14 0.0317(9) 0.0271(8) 0.0443(11) -0.0062(8) -0.0074(8) 0.0004(7) C11 0.0287(7) 0.0191(6) 0.0246(7) -0.0038(5) -0.0040(6) -0.0052(6) C15 0.0437(13) 0.0268(9) 0.0247(9) -0.0015(6) -0.0083(9) -0.0125(9) C12 0.0300(7) 0.0316(7) 0.0292(7) -0.0163(6) -0.0013(5) -0.0091(5) C13 0.0259(7) 0.0557(10) 0.0504(10) -0.0310(8) 0.0083(6) -0.0180(7) C21 0.0195(5) 0.0197(5) 0.0224(6) -0.0060(4) 0.0039(4) -0.0052(4) C22 0.0202(5) 0.0198(5) 0.0213(5) -0.0078(4) 0.0033(4) -0.0044(4) C23 0.0194(5) 0.0197(5) 0.0225(6) -0.0057(5) -0.0002(4) -0.0046(4) C24 0.0219(6) 0.0249(6) 0.0236(6) -0.0070(5) -0.0024(5) -0.0081(5) C25 0.0202(5) 0.0219(6) 0.0275(6) -0.0087(5) 0.0020(5) -0.0089(4) C26 0.0246(13) 0.0199(9) 0.0230(8) -0.0043(10) 0.0037(14) -0.0051(9) C32 0.0355(18) 0.019(2) 0.0219(10) -0.0038(15) 0.0013(12) -0.0028(15) C33 0.0315(11) 0.0349(14) 0.0321(11) -0.0083(11) 0.0133(9) -0.0098(11) C27 0.0388(14) 0.0213(9) 0.0309(10) -0.0039(7) 0.0082(8) -0.0118(8) C28 0.0363(11) 0.0180(8) 0.0305(10) -0.0058(8) -0.0003(8) -0.0063(8) C29 0.0456(16) 0.0157(11) 0.0353(13) -0.0055(8) 0.0018(11) -0.0094(10) C30 0.0353(11) 0.0171(13) 0.0297(9) -0.0081(8) -0.0033(8) -0.0029(10) C31 0.0362(7) 0.0194(6) 0.0238(6) -0.0103(5) -0.0003(5) -0.0064(5) C34 0.0456(9) 0.0289(7) 0.0468(9) -0.0206(7) 0.0045(7) -0.0007(6) C35 0.0487(9) 0.0234(6) 0.0346(8) -0.0130(6) -0.0097(7) -0.0091(6) C46 0.020(2) 0.0232(16) 0.0213(15) -0.0011(16) 0.007(2) -0.0022(15) C52 0.035(3) 0.022(5) 0.018(2) -0.005(3) 0.000(2) 0.000(3) C53 0.035(3) 0.033(3) 0.027(3) -0.002(3) 0.012(2) -0.003(3) C47 0.021(2) 0.024(2) 0.018(2) -0.0017(17) 0.0058(16) -0.0042(18) C48 0.025(2) 0.022(2) 0.031(2) -0.0024(18) 0.0027(18) -0.0093(17) C49 0.032(3) 0.014(3) 0.043(4) -0.008(2) 0.007(3) -0.011(2) C50 0.0362(19) 0.0165(19) 0.0307(16) -0.0088(15) -0.0047(16) -0.0040(18) C57 0.034(2) 0.0307(19) 0.036(2) -0.0156(19) 0.002(2) -0.021(2) C61 0.027(2) 0.0180(19) 0.026(2) -0.0035(19) -0.0033(19) -0.0050(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.1041(12) . ? Fe1 C2 2.0826(12) . ? Fe1 C3 2.0859(12) . ? Fe1 C4 2.0405(12) . ? Fe1 C5 2.0554(12) . ? Fe1 C21 2.0926(12) . ? Fe1 C22 2.0745(12) . ? Fe1 C23 2.0884(12) . ? Fe1 C24 2.0450(13) . ? Fe1 C25 2.0570(12) . ? C1 C2 1.4317(17) . ? C1 C5 1.4254(18) . ? C1 C6 1.5203(17) . ? C2 C3 1.4329(18) . ? C3 C4 1.4298(17) . ? C3 C31 1.5198(17) . ? C4 C5 1.4269(17) . ? C6 C7 1.5484(15) . ? C6 C12 1.530(2) . ? C6 C13 1.546(2) . ? C6 C57 1.5490(19) . ? C7 C8 1.4839(17) . ? C8 C9 1.341(2) . ? C9 C10 1.4837(17) . ? C10 C11 1.5485(15) . ? C14 C11 1.5406(16) . ? C11 C15 1.5375(15) . ? C11 C23 1.518(3) . ? C21 C22 1.4354(17) . ? C21 C25 1.4276(18) . ? C21 C26 1.514(6) . ? C21 C46 1.555(17) . ? C22 C23 1.4323(17) . ? C23 C24 1.4297(18) . ? C23 C61 1.55(2) . ? C24 C25 1.4220(18) . ? C26 C32 1.5377(18) . ? C26 C33 1.5395(17) . ? C26 C27 1.5494(17) . ? C27 C28 1.4835(18) . ? C28 C29 1.341(2) . ? C29 C30 1.483(2) . ? C30 C31 1.5494(16) . ? C31 C34 1.548(2) . ? C31 C35 1.531(2) . ? C31 C50 1.5493(18) . ? C46 C52 1.5383(19) . ? C46 C53 1.5387(19) . ? C46 C47 1.5488(19) . ? C47 C48 1.483(2) . ? C48 C49 1.341(3) . ? C49 C50 1.483(2) . ? C60 C59 1.483(2) . ? C60 C61 1.5489(19) . ? C59 C58 1.340(3) . ? C58 C57 1.483(2) . ? C64 C61 1.539(2) . ? C61 C65 1.5385(19) . ? 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 # C7 C6 C57 11.7(7) . . ? # C26 C21 C46 9.8(2) . . ? # C11 C23 C61 7.1(5) . . ? # C50 C31 C30 8.2(5) . . ? C2 Fe1 C1 39.99(5) . . ? C2 Fe1 C3 40.21(5) . . ? C2 Fe1 C21 113.07(5) . . ? C2 Fe1 C23 160.93(5) . . ? C3 Fe1 C1 67.95(5) . . ? C3 Fe1 C21 123.46(5) . . ? C3 Fe1 C23 155.96(5) . . ? C4 Fe1 C1 67.94(5) . . ? C4 Fe1 C2 67.50(5) . . ? C4 Fe1 C3 40.53(5) . . ? C4 Fe1 C5 40.78(5) . . ? C4 Fe1 C21 155.55(5) . . ? C4 Fe1 C22 158.37(5) . . ? C4 Fe1 C23 119.88(5) . . ? C4 Fe1 C24 102.41(5) . . ? C4 Fe1 C25 118.08(5) . . ? C5 Fe1 C1 40.06(5) . . ? C5 Fe1 C2 67.25(5) . . ? C5 Fe1 C3 68.21(5) . . ? C5 Fe1 C21 163.61(5) . . ? C5 Fe1 C22 125.58(5) . . ? C5 Fe1 C23 105.97(5) . . ? C5 Fe1 C25 153.54(5) . . ? C21 Fe1 C1 129.44(5) . . ? C22 Fe1 C1 112.97(5) . . ? C22 Fe1 C2 128.14(5) . . ? C22 Fe1 C3 161.08(5) . . ? C22 Fe1 C21 40.29(5) . . ? C22 Fe1 C23 40.25(5) . . ? C23 Fe1 C1 123.49(5) . . ? C23 Fe1 C21 68.15(5) . . ? C24 Fe1 C1 155.57(5) . . ? C24 Fe1 C2 158.61(5) . . ? C24 Fe1 C3 120.07(5) . . ? C24 Fe1 C5 118.21(5) . . ? C24 Fe1 C21 67.98(5) . . ? C24 Fe1 C22 67.53(5) . . ? C24 Fe1 C23 40.46(5) . . ? C24 Fe1 C25 40.57(5) . . ? C25 Fe1 C1 163.81(5) . . ? C25 Fe1 C2 126.01(5) . . ? C25 Fe1 C3 106.13(5) . . ? C25 Fe1 C21 40.23(5) . . ? C25 Fe1 C22 67.49(5) . . ? C25 Fe1 C23 68.14(5) . . ? C2 C1 Fe1 69.20(7) . . ? C2 C1 C6 124.86(11) . . ? C5 C1 Fe1 68.13(7) . . ? C5 C1 C2 106.65(11) . . ? C5 C1 C6 126.71(11) . . ? C6 C1 Fe1 139.32(9) . . ? C1 C2 Fe1 70.81(7) . . ? C1 C2 C3 109.65(11) . . ? C3 C2 Fe1 70.02(7) . . ? C2 C3 Fe1 69.77(7) . . ? C2 C3 C31 127.47(11) . . ? C4 C3 Fe1 68.03(7) . . ? C4 C3 C2 106.32(11) . . ? C4 C3 C31 124.81(11) . . ? C31 C3 Fe1 137.20(9) . . ? C3 C4 Fe1 71.44(7) . . ? C5 C4 Fe1 70.17(7) . . ? C5 C4 C3 108.75(11) . . ? C1 C5 Fe1 71.81(7) . . ? C1 C5 C4 108.61(11) . . ? C4 C5 Fe1 69.05(7) . . ? C1 C6 C7 113.43(15) . . ? C1 C6 C12 112.17(11) . . ? C1 C6 C13 106.03(11) . . ? C1 C6 C57 106.8(13) . . ? C12 C6 C7 110.73(15) . . ? C12 C6 C13 108.44(12) . . ? C12 C6 C57 106.3(10) . . ? C13 C6 C7 105.59(12) . . ? C13 C6 C57 117.2(6) . . ? C8 C7 C6 112.37(13) . . ? C9 C8 C7 122.3(2) . . ? C8 C9 C10 124.45(16) . . ? C9 C10 C11 113.21(13) . . ? C14 C11 C10 107.01(15) . . ? C15 C11 C10 110.03(16) . . ? C15 C11 C14 108.9(2) . . ? C23 C11 C10 112.99(16) . . ? C23 C11 C14 106.39(14) . . ? C23 C11 C15 111.29(14) . . ? C22 C21 Fe1 69.18(7) . . ? C22 C21 C26 124.48(17) . . ? C22 C21 C46 126.2(4) . . ? C25 C21 Fe1 68.54(7) . . ? C25 C21 C22 106.58(11) . . ? C25 C21 C26 127.10(19) . . ? C25 C21 C46 127.2(4) . . ? C26 C21 Fe1 139.05(13) . . ? C46 C21 Fe1 129.3(2) . . ? C21 C22 Fe1 70.53(7) . . ? C23 C22 Fe1 70.40(7) . . ? C23 C22 C21 109.55(11) . . ? C11 C23 Fe1 138.02(9) . . ? C22 C23 Fe1 69.36(7) . . ? C22 C23 C11 127.31(12) . . ? C22 C23 C61 129.6(5) . . ? C24 C23 Fe1 68.14(7) . . ? C24 C23 C11 124.89(12) . . ? C24 C23 C22 106.26(11) . . ? C24 C23 C61 123.9(5) . . ? C61 C23 Fe1 131.1(4) . . ? C23 C24 Fe1 71.40(7) . . ? C25 C24 Fe1 70.17(7) . . ? C25 C24 C23 109.04(11) . . ? C21 C25 Fe1 71.22(7) . . ? C24 C25 Fe1 69.27(7) . . ? C24 C25 C21 108.54(11) . . ? C21 C26 C32 110.9(4) . . ? C21 C26 C33 108.6(3) . . ? C21 C26 C27 113.0(4) . . ? C32 C26 C33 108.0(5) . . ? C32 C26 C27 109.4(4) . . ? C33 C26 C27 106.7(2) . . ? C28 C27 C26 113.25(17) . . ? C29 C28 C27 123.4(2) . . ? C28 C29 C30 123.4(4) . . ? C29 C30 C31 112.3(2) . . ? C3 C31 C30 114.5(3) . . ? C3 C31 C34 106.20(11) . . ? C3 C31 C35 111.04(11) . . ? C3 C31 C50 110.4(8) . . ? C34 C31 C30 103.73(15) . . ? C34 C31 C50 111.9(4) . . ? C35 C31 C30 112.5(3) . . ? C35 C31 C34 108.27(12) . . ? C35 C31 C50 109.0(6) . . ? C52 C46 C21 110.2(9) . . ? C52 C46 C53 109.9(13) . . ? C52 C46 C47 110.5(10) . . ? C53 C46 C21 103.2(8) . . ? C53 C46 C47 110.3(5) . . ? C47 C46 C21 112.5(9) . . ? C48 C47 C46 118.1(7) . . ? C49 C48 C47 128.0(5) . . ? C48 C49 C50 127.1(9) . . ? C49 C50 C31 119.6(4) . . ? C59 C60 C61 115.8(10) . . ? C58 C59 C60 128.6(11) . . ? C59 C58 C57 128.7(17) . . ? C58 C57 C6 126.4(11) . . ? C60 C61 C23 113.8(12) . . ? C64 C61 C23 104.3(11) . . ? C64 C61 C60 109.2(11) . . ? C65 C61 C23 112.8(11) . . ? C65 C61 C60 109.1(12) . . ? C65 C61 C64 107.3(14) . . ?