# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'P Power' 'James C. Fettinger' 'Gary J. Long' 'Chengbao Ni.' _publ_contact_author_name 'P Power' _publ_contact_author_email POWER@CHEM.UCDAVIS.EDU _publ_section_title ; Reaction of a sterically encumbered iron(I) aryl/arene with organoazides: formation of an iron(V) imide. ; # Attachment 'C_Fe_NAd2.cif' data_tw45 _database_code_depnum_ccdc_archive 'CCDC 693020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H91 Fe N2' _chemical_formula_sum 'C62 H91 Fe N2' _chemical_formula_weight 920.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9437(14) _cell_length_b 14.9787(15) _cell_length_c 15.5738(16) _cell_angle_alpha 82.3806(15) _cell_angle_beta 66.0829(14) _cell_angle_gamma 65.8148(14) _cell_volume 2710.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9078 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1006 _exptl_absorpt_coefficient_mu 0.317 _exptl_absorpt_correction_type 'Empirical, Twinabs (multi-scan)' _exptl_absorpt_correction_T_min 0.9125 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details 'TWINABS V2008/1 (Sheldrick, 2008)' _exptl_special_details ; An orange block with approximate orthogonal dimensions 0.29 x 0.19 x 0.16mm3 was placed and optically centered on the Bruker SMART1000(1) CCD system at -183\%C. During the initial unit cell determination it was quickly recognized that the crystal was twinned. Several crystals were attempted and a true representative that was well diffracting was chosen. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3\% wide omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoK ] with 0.3\% wide scans, 40 seconds per frame and 606, 455, 606, 455 frames collected per series at varying phi angles (phi=0\%, 90\%, 180\%, 270\%), respectively. The crystal to detector distance was 4.29cm, thus providing a complete sphere of data to 2thetamax=55.10\%. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9803 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.25 _reflns_number_total 9805 _reflns_number_gt 8050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. Data collection was begun and the relative contributions from the multiple twin components were determined using frames from the first two data collection series via a thresholding routine. These reflections were input into Cellnow(2) that determined the twin relationships between the multiple components and generated the orientation matrices for the components and output a useable multiple matrice input file for SAINT(1). At the completion of the run, the optimized merged matrix was re-input and the data were processed a second time. This cyclic procedure was implemented three times. Data collected were corrected for Lorentz and polarization effects and absorption using Blessing's method and merged as incorporated into the program TWINABS(3,4). The major component was now used for structure determination. The SHELXTL(5) program package was now implemented to determine, based upon intensity statistics and lack of systematic absences, the centrosymmetric triclinic space group P-1 (no.2). The structure was determined by direct methods using the program XS(6). All of the non-hydrogen atoms were located after several difference-Fourier least-squares cycles and convergence proceeded quickly. Refinement of the structure was achieved using the program XL(6). Hydrogen atoms were placed in calculated positions throughout the final convergence cycle. A disorder was determined to be 0.79:0.21 for one of the adamantanyl ligands. The final structure was refined to convergence with R(F)=5.56%, wR(F2)=11.50%, GOF=1.102 for all 9803 reflections [R(F)=3.87%, wR(F2)=10.47% for those 8050 data with Fo > 4sigma(Fo)]. The BASF parameter refined to 0.428 indicating a nearly equal percentage of the two domains present. A final difference-Fourier map was featureless indicating that the structure is therefore both correct and complete. References: 1. Bruker (2002) SMART (Version 5.054) and SAINT (Version 7.46a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. Sheldrick, G.M., (private communication) CELLNOW, Twin matrix determination program, Universit\"at G\"ottingen: G\"ottingen, Germany, 2008. 3. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 4. Sheldrick, G.M., (private communication) TWINABS 'An Empirical Correction for Absorption Anisotropy applied to Twinned crystals' v1.05. Universit\"at G\"ottingen: G\"ottingen, Germany, 2003. 5. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 6. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G\"ottingen: G\"ottingen, Germany. ; _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^)+(0.0610P)^2^+0.6269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9805 _refine_ls_number_parameters 642 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.103 _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 0.66092(2) 0.25032(2) 0.25457(2) 0.01874(9) Uani 1 1 d . A . N1 N 0.54305(16) 0.34977(15) 0.28216(14) 0.0321(5) Uani 1 1 d . . . N2 N 0.66713(17) 0.14741(15) 0.22612(14) 0.0315(5) Uani 1 1 d D . . C1 C 0.80294(16) 0.25920(14) 0.25032(13) 0.0148(4) Uani 1 1 d . . . C2 C 0.83880(16) 0.33210(14) 0.19683(14) 0.0166(4) Uani 1 1 d . A . C3 C 0.94428(17) 0.33290(14) 0.18452(15) 0.0190(4) Uani 1 1 d . . . C4 C 1.00125(17) 0.27229(14) 0.23933(15) 0.0193(4) Uani 1 1 d . A . H4 H 1.0688 0.2768 0.2357 0.023 Uiso 1 1 calc R . . C5 C 0.96392(17) 0.20572(14) 0.29890(14) 0.0178(4) Uani 1 1 d . . . C6 C 0.86934(16) 0.19310(14) 0.29796(13) 0.0153(4) Uani 1 1 d . A . C7 C 0.99937(19) 0.39459(16) 0.11131(17) 0.0279(5) Uani 1 1 d . A . H7 H 0.9419 0.4405 0.0862 0.033 Uiso 1 1 calc R . . C8 C 1.0393(2) 0.45520(18) 0.1501(2) 0.0390(6) Uani 1 1 d . . . H8A H 1.0987 0.4113 0.1721 0.059 Uiso 1 1 calc R A . H8B H 0.9746 0.4980 0.2026 0.059 Uiso 1 1 calc R . . H8C H 1.0702 0.4952 0.1004 0.059 Uiso 1 1 calc R . . C9 C 1.1009(2) 0.32665(19) 0.02974(17) 0.0348(6) Uani 1 1 d . . . H9A H 1.1332 0.3660 -0.0198 0.052 Uiso 1 1 calc R A . H9B H 1.0750 0.2884 0.0044 0.052 Uiso 1 1 calc R . . H9C H 1.1593 0.2822 0.0526 0.052 Uiso 1 1 calc R . . C10 C 1.02449(18) 0.14867(15) 0.36363(15) 0.0226(5) Uani 1 1 d . A . H10 H 1.0042 0.0904 0.3841 0.027 Uiso 1 1 calc R . . C11 C 0.9796(2) 0.21256(19) 0.45126(17) 0.0345(6) Uani 1 1 d . . . H11A H 1.0113 0.1738 0.4964 0.052 Uiso 1 1 calc R A . H11B H 0.8962 0.2366 0.4799 0.052 Uiso 1 1 calc R . . H11C H 1.0025 0.2683 0.4337 0.052 Uiso 1 1 calc R . . C12 C 1.15450(19) 0.11164(17) 0.31766(17) 0.0300(5) Uani 1 1 d . . . H12A H 1.1821 0.0760 0.2584 0.045 Uiso 1 1 calc R A . H12B H 1.1875 0.0678 0.3599 0.045 Uiso 1 1 calc R . . H12C H 1.1772 0.1674 0.3052 0.045 Uiso 1 1 calc R . . C13 C 0.76264(16) 0.41505(14) 0.15870(14) 0.0153(4) Uani 1 1 d . . . C14 C 0.74567(17) 0.40402(14) 0.07810(14) 0.0167(4) Uani 1 1 d . A . C15 C 0.67148(17) 0.48543(15) 0.04868(14) 0.0188(4) Uani 1 1 d . . . H15 H 0.6590 0.4777 -0.0050 0.023 Uiso 1 1 calc R A . C16 C 0.61584(17) 0.57649(14) 0.09449(14) 0.0181(4) Uani 1 1 d . A . C17 C 0.63551(17) 0.58586(14) 0.17304(14) 0.0189(4) Uani 1 1 d . . . H17 H 0.5984 0.6479 0.2053 0.023 Uiso 1 1 calc R A . C18 C 0.70769(17) 0.50745(14) 0.20596(14) 0.0171(4) Uani 1 1 d . A . C19 C 0.80613(18) 0.30803(15) 0.02105(14) 0.0202(4) Uani 1 1 d . . . H19 H 0.8442 0.2559 0.0574 0.024 Uiso 1 1 calc R A . C20 C 0.7228(2) 0.27776(16) 0.00370(16) 0.0265(5) Uani 1 1 d . A . H20A H 0.6604 0.2791 0.0636 0.040 Uiso 1 1 calc R . . H20B H 0.7630 0.2114 -0.0250 0.040 Uiso 1 1 calc R . . H20C H 0.6916 0.3235 -0.0386 0.040 Uiso 1 1 calc R . . C21 C 0.89849(19) 0.31398(16) -0.07367(15) 0.0250(5) Uani 1 1 d . A . H21A H 0.8628 0.3637 -0.1112 0.038 Uiso 1 1 calc R . . H21B H 0.9386 0.2502 -0.1076 0.038 Uiso 1 1 calc R . . H21C H 0.9529 0.3318 -0.0626 0.038 Uiso 1 1 calc R . . C22 C 0.54084(18) 0.66297(15) 0.05669(15) 0.0223(5) Uani 1 1 d . . . H22 H 0.5099 0.6369 0.0226 0.027 Uiso 1 1 calc R A . C23 C 0.43943(19) 0.73723(16) 0.13282(17) 0.0309(5) Uani 1 1 d . A . H23A H 0.3953 0.7035 0.1798 0.046 Uiso 1 1 calc R . . H23B H 0.3907 0.7870 0.1041 0.046 Uiso 1 1 calc R . . H23C H 0.4674 0.7687 0.1633 0.046 Uiso 1 1 calc R . . C24 C 0.6121(2) 0.71514(17) -0.01400(17) 0.0304(5) Uani 1 1 d . A . H24A H 0.6428 0.7421 0.0178 0.046 Uiso 1 1 calc R . . H24B H 0.5640 0.7684 -0.0408 0.046 Uiso 1 1 calc R . . H24C H 0.6751 0.6684 -0.0644 0.046 Uiso 1 1 calc R . . C25 C 0.72199(18) 0.52302(15) 0.29421(15) 0.0215(5) Uani 1 1 d . . . H25 H 0.7965 0.4713 0.2922 0.026 Uiso 1 1 calc R A . C26 C 0.6284(2) 0.50821(17) 0.38225(15) 0.0303(5) Uani 1 1 d . A . H26A H 0.5538 0.5572 0.3860 0.045 Uiso 1 1 calc R . . H26B H 0.6408 0.5154 0.4381 0.045 Uiso 1 1 calc R . . H26C H 0.6306 0.4425 0.3790 0.045 Uiso 1 1 calc R . . C27 C 0.7268(2) 0.62242(16) 0.29955(17) 0.0272(5) Uani 1 1 d . A . H27A H 0.7845 0.6316 0.2410 0.041 Uiso 1 1 calc R . . H27B H 0.7468 0.6245 0.3525 0.041 Uiso 1 1 calc R . . H27C H 0.6521 0.6748 0.3086 0.041 Uiso 1 1 calc R . . C28 C 0.84997(16) 0.10201(14) 0.33929(13) 0.0154(4) Uani 1 1 d . . . C29 C 0.76299(16) 0.10175(14) 0.42623(14) 0.0169(4) Uani 1 1 d . A . C30 C 0.75124(17) 0.01347(15) 0.45750(14) 0.0195(4) Uani 1 1 d . . . H30 H 0.6921 0.0139 0.5162 0.023 Uiso 1 1 calc R A . C31 C 0.82231(17) -0.07480(14) 0.40645(14) 0.0190(4) Uani 1 1 d . A . C32 C 0.90970(17) -0.07316(15) 0.32191(15) 0.0190(4) Uani 1 1 d . . . H32 H 0.9600 -0.1326 0.2858 0.023 Uiso 1 1 calc R A . C33 C 0.92611(17) 0.01253(14) 0.28833(13) 0.0165(4) Uani 1 1 d . A . C34 C 0.68168(18) 0.19396(15) 0.48811(15) 0.0232(5) Uani 1 1 d . . . H34 H 0.7023 0.2496 0.4555 0.028 Uiso 1 1 calc R A . C35 C 0.55835(19) 0.21791(18) 0.50249(17) 0.0338(6) Uani 1 1 d . A . H35A H 0.5534 0.2196 0.4412 0.051 Uiso 1 1 calc R . . H35B H 0.5089 0.2819 0.5355 0.051 Uiso 1 1 calc R . . H35C H 0.5337 0.1675 0.5399 0.051 Uiso 1 1 calc R . . C36 C 0.6916(2) 0.18517(18) 0.58414(16) 0.0321(5) Uani 1 1 d . A . H36A H 0.6653 0.1348 0.6197 0.048 Uiso 1 1 calc R . . H36B H 0.6443 0.2482 0.6194 0.048 Uiso 1 1 calc R . . H36C H 0.7713 0.1669 0.5745 0.048 Uiso 1 1 calc R . . C37 C 0.80396(19) -0.16849(15) 0.44416(16) 0.0248(5) Uani 1 1 d . . . H37 H 0.8036 -0.1754 0.5090 0.030 Uiso 1 1 calc R A . C38 C 0.6887(2) -0.16195(18) 0.45250(19) 0.0359(6) Uani 1 1 d . A . H38A H 0.6286 -0.1016 0.4879 0.054 Uiso 1 1 calc R . . H38B H 0.6746 -0.2186 0.4854 0.054 Uiso 1 1 calc R . . H38C H 0.6886 -0.1615 0.3895 0.054 Uiso 1 1 calc R . . C39 C 0.8987(2) -0.26094(16) 0.38663(18) 0.0353(6) Uani 1 1 d . A . H39A H 0.8837 -0.3185 0.4160 0.053 Uiso 1 1 calc R . . H39B H 0.9722 -0.2665 0.3844 0.053 Uiso 1 1 calc R . . H39C H 0.9008 -0.2571 0.3226 0.053 Uiso 1 1 calc R . . C40 C 1.02797(17) 0.00625(15) 0.19707(14) 0.0200(4) Uani 1 1 d . . . H40 H 1.0403 0.0680 0.1944 0.024 Uiso 1 1 calc R A . C41 C 1.0039(2) 0.00166(18) 0.11113(15) 0.0295(5) Uani 1 1 d . A . H41A H 0.9901 -0.0576 0.1119 0.044 Uiso 1 1 calc R . . H41B H 1.0697 0.0001 0.0540 0.044 Uiso 1 1 calc R . . H41C H 0.9364 0.0595 0.1121 0.044 Uiso 1 1 calc R . . C42 C 1.13820(18) -0.07928(16) 0.19459(16) 0.0275(5) Uani 1 1 d . A . H42A H 1.1501 -0.0760 0.2518 0.041 Uiso 1 1 calc R . . H42B H 1.2029 -0.0751 0.1394 0.041 Uiso 1 1 calc R . . H42C H 1.1320 -0.1414 0.1910 0.041 Uiso 1 1 calc R . . C43 C 0.42429(17) 0.40867(16) 0.29942(15) 0.0229(5) Uani 1 1 d . . . C44 C 0.35013(19) 0.36366(18) 0.37807(17) 0.0306(5) Uani 1 1 d . . . H44A H 0.3634 0.3625 0.4361 0.037 Uiso 1 1 calc R . . H44B H 0.3709 0.2954 0.3595 0.037 Uiso 1 1 calc R . . C45 C 0.40334(19) 0.41208(17) 0.20925(16) 0.0272(5) Uani 1 1 d . . . H45A H 0.4263 0.3447 0.1870 0.033 Uiso 1 1 calc R . . H45B H 0.4501 0.4428 0.1594 0.033 Uiso 1 1 calc R . . C46 C 0.3906(2) 0.51427(17) 0.33142(18) 0.0334(6) Uani 1 1 d . . . H46A H 0.4033 0.5132 0.3897 0.040 Uiso 1 1 calc R . . H46B H 0.4389 0.5443 0.2823 0.040 Uiso 1 1 calc R . . C47 C 0.2232(2) 0.4248(2) 0.39673(18) 0.0385(6) Uani 1 1 d . . . H47 H 0.1750 0.3950 0.4476 0.046 Uiso 1 1 calc R . . C48 C 0.2051(2) 0.42424(19) 0.30661(18) 0.0353(6) Uani 1 1 d . . . H48A H 0.2277 0.3560 0.2869 0.042 Uiso 1 1 calc R . . H48B H 0.1233 0.4606 0.3182 0.042 Uiso 1 1 calc R . . C49 C 0.2758(2) 0.47159(17) 0.22884(16) 0.0288(5) Uani 1 1 d . . . H49 H 0.2619 0.4728 0.1705 0.035 Uiso 1 1 calc R . . C50 C 0.2453(2) 0.57525(17) 0.25943(17) 0.0352(6) Uani 1 1 d . . . H50A H 0.1643 0.6155 0.2704 0.042 Uiso 1 1 calc R . . H50B H 0.2929 0.6047 0.2088 0.042 Uiso 1 1 calc R . . C51 C 0.2643(2) 0.57533(18) 0.34936(18) 0.0361(6) Uani 1 1 d . . . H51 H 0.2427 0.6440 0.3692 0.043 Uiso 1 1 calc R . . C52 C 0.1916(2) 0.5285(2) 0.42723(18) 0.0436(7) Uani 1 1 d . . . H52A H 0.2043 0.5276 0.4855 0.052 Uiso 1 1 calc R . . H52B H 0.1098 0.5677 0.4407 0.052 Uiso 1 1 calc R . . C53 C 0.6343(4) 0.0762(3) 0.2028(3) 0.0215(6) Uani 0.79 1 d PD A 1 C54 C 0.6132(3) 0.0096(2) 0.2849(2) 0.0318(7) Uani 0.79 1 d PDU A 1 H54A H 0.5506 0.0487 0.3417 0.038 Uiso 0.79 1 calc PR A 1 H54B H 0.6828 -0.0236 0.2987 0.038 Uiso 0.79 1 calc PR A 1 C55 C 0.7325(3) 0.0159(2) 0.1154(2) 0.0330(7) Uani 0.79 1 d PDU A 1 H55A H 0.8028 -0.0173 0.1282 0.040 Uiso 0.79 1 calc PR A 1 H55B H 0.7473 0.0596 0.0624 0.040 Uiso 0.79 1 calc PR A 1 C56 C 0.5278(2) 0.1284(2) 0.1816(2) 0.0267(6) Uani 0.79 1 d PDU A 1 H56A H 0.5418 0.1727 0.1291 0.032 Uiso 0.79 1 calc PR A 1 H56B H 0.4641 0.1683 0.2375 0.032 Uiso 0.79 1 calc PR A 1 C57 C 0.5809(3) -0.0677(2) 0.2584(2) 0.0326(7) Uani 0.79 1 d PDU A 1 H57 H 0.5658 -0.1118 0.3118 0.039 Uiso 0.79 1 calc PR A 1 C58 C 0.6783(4) -0.1271(3) 0.1721(3) 0.0412(11) Uani 0.79 1 d PDU A 1 H58A H 0.6593 -0.1777 0.1557 0.049 Uiso 0.79 1 calc PR A 1 H58B H 0.7480 -0.1607 0.1857 0.049 Uiso 0.79 1 calc PR A 1 C59 C 0.7010(3) -0.0610(2) 0.0888(3) 0.0357(8) Uani 0.79 1 d PDU A 1 H59 H 0.7648 -0.1010 0.0320 0.043 Uiso 0.79 1 calc PR A 1 C60 C 0.5937(3) -0.0089(3) 0.0694(2) 0.0360(8) Uani 0.79 1 d PDU A 1 H60A H 0.5732 -0.0578 0.0519 0.043 Uiso 0.79 1 calc PR A 1 H60B H 0.6078 0.0342 0.0158 0.043 Uiso 0.79 1 calc PR A 1 C61 C 0.4958(3) 0.0517(3) 0.1548(3) 0.0315(9) Uani 0.79 1 d PDU A 1 H61 H 0.4255 0.0854 0.1409 0.038 Uiso 0.79 1 calc PR A 1 C62 C 0.4745(3) -0.0144(3) 0.2367(3) 0.0339(8) Uani 0.79 1 d PDU A 1 H62A H 0.4518 -0.0629 0.2214 0.041 Uiso 0.79 1 calc PR A 1 H62B H 0.4111 0.0253 0.2928 0.041 Uiso 0.79 1 calc PR A 1 C53B C 0.6466(15) 0.0691(9) 0.2002(12) 0.0215(6) Uani 0.21 1 d PD A 2 C54B C 0.5346(10) 0.0678(9) 0.2770(8) 0.041(3) Uiso 0.21 1 d PDU A 2 H54C H 0.4764 0.1357 0.2901 0.049 Uiso 0.21 1 calc PR A 2 H54D H 0.5477 0.0446 0.3354 0.049 Uiso 0.21 1 calc PR A 2 C55B C 0.7305(11) -0.0413(9) 0.1829(10) 0.050(3) Uiso 0.21 1 d PDU A 2 H55C H 0.8061 -0.0461 0.1357 0.060 Uiso 0.21 1 calc PR A 2 H55D H 0.7399 -0.0669 0.2422 0.060 Uiso 0.21 1 calc PR A 2 C56B C 0.6282(9) 0.0967(7) 0.1082(7) 0.026(2) Uiso 0.21 1 d PDU A 2 H56C H 0.7026 0.0872 0.0562 0.031 Uiso 0.21 1 calc PR A 2 H56D H 0.5781 0.1671 0.1126 0.031 Uiso 0.21 1 calc PR A 2 C57B C 0.4866(14) 0.0025(11) 0.2521(11) 0.041(4) Uiso 0.21 1 d PDU A 2 H57B H 0.4139 0.0050 0.3045 0.050 Uiso 0.21 1 calc PR A 2 C58B C 0.5758(12) -0.1030(10) 0.2304(10) 0.049(3) Uiso 0.21 1 d PDU A 2 H58C H 0.5459 -0.1442 0.2126 0.058 Uiso 0.21 1 calc PR A 2 H58D H 0.5911 -0.1297 0.2872 0.058 Uiso 0.21 1 calc PR A 2 C59B C 0.6896(14) -0.1066(12) 0.1481(12) 0.040(4) Uiso 0.21 1 d PDU A 2 H59B H 0.7480 -0.1754 0.1343 0.048 Uiso 0.21 1 calc PR A 2 C60B C 0.6646(14) -0.0654(11) 0.0629(10) 0.049(3) Uiso 0.21 1 d PDU A 2 H60C H 0.6389 -0.1077 0.0417 0.058 Uiso 0.21 1 calc PR A 2 H60D H 0.7351 -0.0642 0.0114 0.058 Uiso 0.21 1 calc PR A 2 C61B C 0.5742(12) 0.0363(10) 0.0844(10) 0.041(3) Uiso 0.21 1 d PDU A 2 H61B H 0.5577 0.0620 0.0272 0.049 Uiso 0.21 1 calc PR A 2 C62B C 0.4667(13) 0.0404(14) 0.1640(11) 0.042(4) Uiso 0.21 1 d PDU A 2 H62C H 0.4348 0.0009 0.1464 0.051 Uiso 0.21 1 calc PR A 2 H62D H 0.4101 0.1090 0.1760 0.051 Uiso 0.21 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 0.01660(16) 0.02082(17) 0.02291(17) 0.00206(12) -0.01054(13) -0.00870(12) N1 0.0220(10) 0.0413(12) 0.0316(11) 0.0036(9) -0.0109(9) -0.0113(9) N2 0.0341(11) 0.0382(12) 0.0295(11) 0.0019(9) -0.0133(9) -0.0202(10) C1 0.0133(9) 0.0127(9) 0.0152(10) -0.0034(8) -0.0042(8) -0.0022(8) C2 0.0187(10) 0.0135(10) 0.0166(10) -0.0027(8) -0.0072(8) -0.0042(8) C3 0.0195(10) 0.0147(10) 0.0229(11) -0.0004(8) -0.0081(9) -0.0065(8) C4 0.0154(10) 0.0195(10) 0.0277(11) 0.0007(9) -0.0117(9) -0.0078(8) C5 0.0165(10) 0.0141(10) 0.0201(10) -0.0032(8) -0.0078(8) -0.0016(8) C6 0.0165(10) 0.0142(10) 0.0132(10) -0.0006(8) -0.0047(8) -0.0050(8) C7 0.0225(11) 0.0255(12) 0.0388(14) 0.0129(10) -0.0155(10) -0.0123(10) C8 0.0328(13) 0.0288(13) 0.0600(18) 0.0056(12) -0.0164(13) -0.0190(11) C9 0.0282(12) 0.0471(15) 0.0313(13) 0.0109(12) -0.0112(11) -0.0200(12) C10 0.0226(11) 0.0225(11) 0.0286(12) 0.0040(9) -0.0165(10) -0.0087(9) C11 0.0298(13) 0.0481(15) 0.0302(13) -0.0003(11) -0.0199(11) -0.0109(12) C12 0.0240(12) 0.0297(13) 0.0381(14) 0.0024(11) -0.0195(11) -0.0053(10) C13 0.0142(9) 0.0141(10) 0.0181(10) 0.0029(8) -0.0060(8) -0.0070(8) C14 0.0186(10) 0.0164(10) 0.0174(10) 0.0032(8) -0.0075(8) -0.0093(8) C15 0.0208(10) 0.0219(11) 0.0163(10) 0.0017(8) -0.0094(9) -0.0089(9) C16 0.0157(10) 0.0168(10) 0.0206(10) 0.0031(8) -0.0061(8) -0.0069(8) C17 0.0174(10) 0.0138(10) 0.0233(11) -0.0017(8) -0.0067(9) -0.0046(8) C18 0.0167(10) 0.0176(10) 0.0187(10) 0.0009(8) -0.0071(8) -0.0082(8) C19 0.0269(11) 0.0161(10) 0.0177(10) 0.0008(8) -0.0106(9) -0.0067(9) C20 0.0339(13) 0.0240(12) 0.0242(12) -0.0031(9) -0.0100(10) -0.0138(10) C21 0.0258(12) 0.0215(11) 0.0234(11) -0.0028(9) -0.0083(10) -0.0055(9) C22 0.0230(11) 0.0196(11) 0.0274(11) 0.0017(9) -0.0154(10) -0.0061(9) C23 0.0219(11) 0.0244(12) 0.0403(14) 0.0023(10) -0.0143(11) -0.0016(10) C24 0.0292(12) 0.0272(12) 0.0334(13) 0.0103(10) -0.0172(11) -0.0075(10) C25 0.0248(11) 0.0169(11) 0.0250(11) -0.0034(9) -0.0136(9) -0.0049(9) C26 0.0467(15) 0.0313(13) 0.0213(11) 0.0019(9) -0.0176(11) -0.0191(11) C27 0.0300(12) 0.0256(12) 0.0296(12) -0.0047(10) -0.0123(10) -0.0116(10) C28 0.0163(10) 0.0158(10) 0.0164(10) 0.0019(8) -0.0104(8) -0.0048(8) C29 0.0153(10) 0.0193(10) 0.0169(10) 0.0009(8) -0.0093(8) -0.0047(8) C30 0.0175(10) 0.0267(11) 0.0152(10) 0.0053(8) -0.0070(8) -0.0101(9) C31 0.0221(11) 0.0182(10) 0.0231(11) 0.0051(9) -0.0155(9) -0.0085(9) C32 0.0185(10) 0.0155(10) 0.0238(11) -0.0005(8) -0.0125(9) -0.0028(8) C33 0.0152(10) 0.0188(10) 0.0159(10) 0.0016(8) -0.0087(8) -0.0047(8) C34 0.0232(11) 0.0203(11) 0.0187(11) -0.0019(9) -0.0033(9) -0.0054(9) C35 0.0222(12) 0.0328(13) 0.0290(13) -0.0048(10) -0.0050(10) 0.0024(10) C36 0.0393(14) 0.0364(13) 0.0207(11) -0.0057(10) -0.0075(10) -0.0168(11) C37 0.0317(12) 0.0229(11) 0.0261(12) 0.0089(9) -0.0164(10) -0.0139(10) C38 0.0421(14) 0.0356(14) 0.0454(15) 0.0188(12) -0.0259(13) -0.0259(12) C39 0.0478(15) 0.0199(12) 0.0391(14) 0.0062(10) -0.0165(12) -0.0160(11) C40 0.0161(10) 0.0183(11) 0.0205(11) -0.0036(8) -0.0030(9) -0.0048(8) C41 0.0256(12) 0.0384(14) 0.0203(11) 0.0001(10) -0.0066(10) -0.0106(10) C42 0.0175(11) 0.0287(12) 0.0279(12) -0.0064(10) -0.0052(10) -0.0026(9) C43 0.0158(10) 0.0275(12) 0.0220(11) 0.0045(9) -0.0085(9) -0.0052(9) C44 0.0270(12) 0.0348(13) 0.0300(13) 0.0104(10) -0.0141(10) -0.0118(10) C45 0.0237(11) 0.0303(12) 0.0230(12) -0.0007(10) -0.0079(10) -0.0069(10) C46 0.0405(14) 0.0342(14) 0.0308(13) 0.0027(11) -0.0192(12) -0.0147(11) C47 0.0255(12) 0.0594(17) 0.0316(13) 0.0200(12) -0.0124(11) -0.0217(12) C48 0.0219(12) 0.0455(15) 0.0401(14) 0.0077(12) -0.0141(11) -0.0145(11) C49 0.0289(12) 0.0351(13) 0.0242(12) 0.0046(10) -0.0150(10) -0.0106(10) C50 0.0395(14) 0.0305(13) 0.0313(13) 0.0033(11) -0.0184(12) -0.0057(11) C51 0.0388(14) 0.0276(13) 0.0364(14) -0.0073(11) -0.0186(12) -0.0014(11) C52 0.0323(14) 0.0530(17) 0.0253(13) -0.0031(12) -0.0116(11) 0.0040(12) C53 0.0217(15) 0.0265(13) 0.0220(11) 0.0023(10) -0.0107(11) -0.0131(12) C54 0.0448(18) 0.0369(17) 0.0301(16) 0.0106(13) -0.0223(14) -0.0264(15) C55 0.0295(16) 0.0271(16) 0.0380(17) -0.0045(14) -0.0063(14) -0.0120(13) C56 0.0278(15) 0.0243(15) 0.0337(16) 0.0041(12) -0.0177(13) -0.0107(12) C57 0.052(2) 0.0294(17) 0.0327(17) 0.0161(14) -0.0271(16) -0.0257(15) C58 0.044(2) 0.0174(18) 0.068(3) 0.0079(18) -0.032(2) -0.0099(16) C59 0.0322(17) 0.0339(18) 0.0369(19) -0.0090(15) -0.0071(15) -0.0122(14) C60 0.057(2) 0.034(2) 0.0278(17) 0.0031(15) -0.0218(16) -0.0228(19) C61 0.034(2) 0.0287(18) 0.044(2) 0.0104(14) -0.0275(18) -0.0149(16) C62 0.0346(19) 0.040(2) 0.0368(19) 0.0030(15) -0.0149(15) -0.0230(16) C53B 0.0217(15) 0.0265(13) 0.0220(11) 0.0023(10) -0.0107(11) -0.0131(12) _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 N2 1.619(2) . ? Fe1 N1 1.642(2) . ? Fe1 C1 2.0126(19) . ? N1 C43 1.448(3) . ? N2 C53 1.455(3) . ? N2 C53B 1.455(3) . ? C1 C6 1.414(3) . ? C1 C2 1.416(3) . ? C2 C3 1.409(3) . ? C2 C13 1.503(3) . ? C3 C4 1.392(3) . ? C3 C7 1.529(3) . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.413(3) . ? C5 C10 1.527(3) . ? C6 C28 1.509(3) . ? C7 C8 1.526(3) . ? C7 C9 1.535(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.527(3) . ? C10 C12 1.528(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.409(3) . ? C13 C18 1.410(3) . ? C14 C15 1.403(3) . ? C14 C19 1.519(3) . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 C22 1.518(3) . ? C17 C18 1.395(3) . ? C17 H17 0.9500 . ? C18 C25 1.526(3) . ? C19 C20 1.532(3) . ? C19 C21 1.537(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.526(3) . ? C22 C23 1.531(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.529(3) . ? C25 C27 1.532(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.405(3) . ? C28 C33 1.409(3) . ? C29 C30 1.398(3) . ? C29 C34 1.518(3) . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 C32 1.391(3) . ? C31 C37 1.528(3) . ? C32 C33 1.392(3) . ? C32 H32 0.9500 . ? C33 C40 1.528(3) . ? C34 C35 1.530(3) . ? C34 C36 1.540(3) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.522(3) . ? C37 C39 1.528(3) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.522(3) . ? C40 C42 1.535(3) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.533(3) . ? C43 C45 1.537(3) . ? C43 C46 1.543(3) . ? C44 C47 1.543(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C49 1.543(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C51 1.538(3) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C52 1.516(4) . ? C47 C48 1.525(4) . ? C47 H47 1.0000 . ? C48 C49 1.523(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.520(3) . ? C49 H49 1.0000 . ? C50 C51 1.528(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.533(4) . ? C51 H51 1.0000 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C56 1.517(5) . ? C53 C54 1.522(5) . ? C53 C55 1.532(5) . ? C54 C57 1.556(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C59 1.542(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C61 1.546(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.513(6) . ? C57 C62 1.522(5) . ? C57 H57 1.0000 . ? C58 C59 1.531(6) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.512(5) . ? C59 H59 1.0000 . ? C60 C61 1.514(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.514(5) . ? C61 H61 1.0000 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C53B C56B 1.531(15) . ? C53B C54B 1.541(16) . ? C53B C55B 1.566(15) . ? C54B C57B 1.551(14) . ? C54B H54C 0.9900 . ? C54B H54D 0.9900 . ? C55B C59B 1.557(15) . ? C55B H55C 0.9900 . ? C55B H55D 0.9900 . ? C56B C61B 1.549(14) . ? C56B H56C 0.9900 . ? C56B H56D 0.9900 . ? C57B C62B 1.502(17) . ? C57B C58B 1.533(16) . ? C57B H57B 1.0000 . ? C58B C59B 1.569(16) . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? C59B C60B 1.498(16) . ? C59B H59B 1.0000 . ? C60B C61B 1.496(15) . ? C60B H60C 0.9900 . ? C60B H60D 0.9900 . ? C61B C62B 1.491(15) . ? C61B H61B 1.0000 . ? C62B H62C 0.9900 . ? C62B H62D 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 N2 Fe1 N1 121.86(10) . . ? N2 Fe1 C1 119.46(9) . . ? N1 Fe1 C1 118.61(9) . . ? C43 N1 Fe1 156.60(18) . . ? C53 N2 Fe1 160.7(2) . . ? C53B N2 Fe1 166.6(7) . . ? C6 C1 C2 118.99(17) . . ? C6 C1 Fe1 121.64(14) . . ? C2 C1 Fe1 119.36(14) . . ? C3 C2 C1 120.21(17) . . ? C3 C2 C13 117.99(17) . . ? C1 C2 C13 121.60(17) . . ? C4 C3 C2 118.06(18) . . ? C4 C3 C7 119.46(18) . . ? C2 C3 C7 122.44(18) . . ? C5 C4 C3 122.92(18) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C4 C5 C6 118.29(18) . . ? C4 C5 C10 119.85(18) . . ? C6 C5 C10 121.86(18) . . ? C5 C6 C1 120.05(17) . . ? C5 C6 C28 118.18(17) . . ? C1 C6 C28 121.42(17) . . ? C8 C7 C3 113.8(2) . . ? C8 C7 C9 109.5(2) . . ? C3 C7 C9 108.87(18) . . ? C8 C7 H7 108.2 . . ? C3 C7 H7 108.2 . . ? C9 C7 H7 108.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 C11 109.14(17) . . ? C5 C10 C12 114.28(18) . . ? C11 C10 C12 109.94(18) . . ? C5 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? 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 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.57(17) . . ? C14 C13 C2 122.77(17) . . ? C18 C13 C2 117.66(17) . . ? C15 C14 C13 118.63(18) . . ? C15 C14 C19 118.84(17) . . ? C13 C14 C19 122.52(17) . . ? C16 C15 C14 122.76(18) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C15 C16 C17 117.47(18) . . ? C15 C16 C22 120.34(18) . . ? C17 C16 C22 122.13(18) . . ? C16 C17 C18 122.35(18) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C13 119.20(18) . . ? C17 C18 C25 119.12(17) . . ? C13 C18 C25 121.65(17) . . ? C14 C19 C20 112.00(17) . . ? C14 C19 C21 111.18(17) . . ? C20 C19 C21 109.36(17) . . ? C14 C19 H19 108.1 . . ? C20 C19 H19 108.1 . . ? C21 C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 C24 110.03(17) . . ? C16 C22 C23 114.02(18) . . ? C24 C22 C23 109.28(18) . . ? C16 C22 H22 107.8 . . ? C24 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? 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 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C25 C26 110.46(17) . . ? C18 C25 C27 113.20(18) . . ? C26 C25 C27 111.12(18) . . ? C18 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.98(18) . . ? C29 C28 C6 123.58(17) . . ? C33 C28 C6 117.41(17) . . ? C30 C29 C28 119.03(18) . . ? C30 C29 C34 118.64(18) . . ? C28 C29 C34 122.33(18) . . ? C31 C30 C29 122.85(19) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 117.05(18) . . ? C30 C31 C37 120.21(19) . . ? C32 C31 C37 122.74(18) . . ? C31 C32 C33 122.33(19) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C28 119.64(18) . . ? C32 C33 C40 118.56(17) . . ? C28 C33 C40 121.79(18) . . ? C29 C34 C35 111.02(18) . . ? C29 C34 C36 111.73(17) . . ? C35 C34 C36 109.82(18) . . ? C29 C34 H34 108.0 . . ? C35 C34 H34 108.0 . . ? C36 C34 H34 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C31 111.48(18) . . ? C38 C37 C39 109.9(2) . . ? C31 C37 C39 113.51(19) . . ? C38 C37 H37 107.2 . . ? C31 C37 H37 107.2 . . ? C39 C37 H37 107.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C33 111.63(17) . . ? C41 C40 C42 111.18(17) . . ? C33 C40 C42 112.24(17) . . ? C41 C40 H40 107.2 . . ? C33 C40 H40 107.2 . . ? C42 C40 H40 107.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1 C43 C44 108.78(18) . . ? N1 C43 C45 109.96(18) . . ? C44 C43 C45 110.27(19) . . ? N1 C43 C46 110.78(19) . . ? C44 C43 C46 108.25(19) . . ? C45 C43 C46 108.80(18) . . ? C43 C44 C47 109.54(18) . . ? C43 C44 H44A 109.8 . . ? C47 C44 H44A 109.8 . . ? C43 C44 H44B 109.8 . . ? C47 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? C43 C45 C49 109.84(18) . . ? C43 C45 H45A 109.7 . . ? C49 C45 H45A 109.7 . . ? C43 C45 H45B 109.7 . . ? C49 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C51 C46 C43 109.83(19) . . ? C51 C46 H46A 109.7 . . ? C43 C46 H46A 109.7 . . ? C51 C46 H46B 109.7 . . ? C43 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C52 C47 C48 110.7(2) . . ? C52 C47 C44 109.3(2) . . ? C48 C47 C44 108.6(2) . . ? C52 C47 H47 109.4 . . ? C48 C47 H47 109.4 . . ? C44 C47 H47 109.4 . . ? C49 C48 C47 110.1(2) . . ? C49 C48 H48A 109.6 . . ? C47 C48 H48A 109.6 . . ? C49 C48 H48B 109.6 . . ? C47 C48 H48B 109.6 . . ? H48A C48 H48B 108.1 . . ? C50 C49 C48 110.3(2) . . ? C50 C49 C45 108.0(2) . . ? C48 C49 C45 109.04(19) . . ? C50 C49 H49 109.8 . . ? C48 C49 H49 109.8 . . ? C45 C49 H49 109.8 . . ? C49 C50 C51 110.74(19) . . ? C49 C50 H50A 109.5 . . ? C51 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C50 C51 C52 109.4(2) . . ? C50 C51 C46 109.3(2) . . ? C52 C51 C46 108.5(2) . . ? C50 C51 H51 109.9 . . ? C52 C51 H51 109.9 . . ? C46 C51 H51 109.9 . . ? C47 C52 C51 109.9(2) . . ? C47 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? C47 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? N2 C53 C56 110.1(3) . . ? N2 C53 C54 109.0(3) . . ? C56 C53 C54 110.5(3) . . ? N2 C53 C55 108.0(3) . . ? C56 C53 C55 109.3(3) . . ? C54 C53 C55 109.9(3) . . ? C53 C54 C57 108.6(2) . . ? C53 C54 H54A 110.0 . . ? C57 C54 H54A 110.0 . . ? C53 C54 H54B 110.0 . . ? C57 C54 H54B 110.0 . . ? H54A C54 H54B 108.3 . . ? C53 C55 C59 109.5(2) . . ? C53 C55 H55A 109.8 . . ? C59 C55 H55A 109.8 . . ? C53 C55 H55B 109.8 . . ? C59 C55 H55B 109.8 . . ? H55A C55 H55B 108.2 . . ? C53 C56 C61 109.4(2) . . ? C53 C56 H56A 109.8 . . ? C61 C56 H56A 109.8 . . ? C53 C56 H56B 109.8 . . ? C61 C56 H56B 109.8 . . ? H56A C56 H56B 108.2 . . ? C58 C57 C62 109.5(3) . . ? C58 C57 C54 109.0(3) . . ? C62 C57 C54 108.7(3) . . ? C58 C57 H57 109.9 . . ? C62 C57 H57 109.9 . . ? C54 C57 H57 109.9 . . ? C57 C58 C59 110.6(3) . . ? C57 C58 H58A 109.5 . . ? C59 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 108.1 . . ? C60 C59 C58 109.2(3) . . ? C60 C59 C55 109.0(3) . . ? C58 C59 C55 108.5(3) . . ? C60 C59 H59 110.1 . . ? C58 C59 H59 110.1 . . ? C55 C59 H59 110.1 . . ? C59 C60 C61 110.9(3) . . ? C59 C60 H60A 109.5 . . ? C61 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 108.0 . . ? C60 C61 C62 109.3(3) . . ? C60 C61 C56 109.3(3) . . ? C62 C61 C56 108.3(3) . . ? C60 C61 H61 109.9 . . ? C62 C61 H61 109.9 . . ? C56 C61 H61 109.9 . . ? C61 C62 C57 110.9(3) . . ? C61 C62 H62A 109.5 . . ? C57 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 108.0 . . ? N2 C53B C56B 106.9(9) . . ? N2 C53B C54B 107.4(10) . . ? C56B C53B C54B 108.1(11) . . ? N2 C53B C55B 125.3(12) . . ? C56B C53B C55B 104.0(9) . . ? C54B C53B C55B 104.2(10) . . ? C53B C54B C57B 114.7(9) . . ? C53B C54B H54C 108.6 . . ? C57B C54B H54C 108.6 . . ? C53B C54B H54D 108.6 . . ? C57B C54B H54D 108.6 . . ? H54C C54B H54D 107.6 . . ? C59B C55B C53B 113.5(10) . . ? C59B C55B H55C 108.9 . . ? C53B C55B H55C 108.9 . . ? C59B C55B H55D 108.9 . . ? C53B C55B H55D 108.9 . . ? H55C C55B H55D 107.7 . . ? C53B C56B C61B 113.4(8) . . ? C53B C56B H56C 108.9 . . ? C61B C56B H56C 108.9 . . ? C53B C56B H56D 108.9 . . ? C61B C56B H56D 108.9 . . ? H56C C56B H56D 107.7 . . ? C62B C57B C58B 107.8(13) . . ? C62B C57B C54B 107.1(12) . . ? C58B C57B C54B 109.6(12) . . ? C62B C57B H57B 110.8 . . ? C58B C57B H57B 110.8 . . ? C54B C57B H57B 110.8 . . ? C57B C58B C59B 110.6(11) . . ? C57B C58B H58C 109.5 . . ? C59B C58B H58C 109.5 . . ? C57B C58B H58D 109.5 . . ? C59B C58B H58D 109.5 . . ? H58C C58B H58D 108.1 . . ? C60B C59B C55B 110.6(13) . . ? C60B C59B C58B 108.8(12) . . ? C55B C59B C58B 105.7(12) . . ? C60B C59B H59B 110.6 . . ? C55B C59B H59B 110.6 . . ? C58B C59B H59B 110.6 . . ? C59B C60B C61B 110.6(12) . . ? C59B C60B H60C 109.5 . . ? C61B C60B H60C 109.5 . . ? C59B C60B H60D 109.5 . . ? C61B C60B H60D 109.5 . . ? H60C C60B H60D 108.1 . . ? C62B C61B C60B 112.4(13) . . ? C62B C61B C56B 111.5(12) . . ? C60B C61B C56B 104.6(11) . . ? C62B C61B H61B 109.4 . . ? C60B C61B H61B 109.4 . . ? C56B C61B H61B 109.4 . . ? C61B C62B C57B 111.7(12) . . ? C61B C62B H62C 109.3 . . ? C57B C62B H62C 109.3 . . ? C61B C62B H62D 109.3 . . ? C57B C62B H62D 109.3 . . ? H62C C62B H62D 107.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.507 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.056 # Attachment 'C_Fe_NJ_dimer.cif' data_jf1598fffmi _database_code_depnum_ccdc_archive 'CCDC 693021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C132 H172 Fe2 N2, 5(C6 H14)' _chemical_formula_sum 'C162 H242 Fe2 N2' _chemical_formula_weight 2329.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/a' _symmetry_space_group_name_Hall '-I 2ya' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 25.135(2) _cell_length_b 28.011(3) _cell_length_c 25.235(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.871(1) _cell_angle_gamma 90.00 _cell_volume 15559(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.31 _exptl_crystal_description Rod _exptl_crystal_colour Orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 0.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; An orange rod with approximate orthogonal dimensions 0.081 x 0.146 x 0.466mm3 was placed and optically centered on the Bruker SMART APEXII1 CCD system at 90(2)K. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3\% wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3\% wide scans, 60 seconds per frame and 606 frames collected per series at varying phi angles (phi=0\%, 90\%, 180\%, 270\%). The crystal to detector distance was 5.23cm, thus providing a complete sphere of data to 2Thetamax=55.13\%. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68750 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17858 _reflns_number_gt 12369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.1-4) (Bruker, 2007)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 99177 reflections were collected and corrected for Lorentz and polarization effects and absorption, based upon crystal size and face indexing, using Blessing's method as incorporated into the program SADABS2,3 with 35674 unique. The SHELXTL4 program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric monoclinic space group I2/a (no. 15) or Ia (no. 9) due to the beta angle closer to 90 than the Monoclinic C orientation. The structure was determined by direct methods with the successful location of a majority of the unique molecule within the asymmetric unit using the program XS5. The structure was refined with XL5. The data collected were truncated to two theta max = 55.0\% and merged based upon identical indices yielding 69445 data with XPREP4 that were further merged during least-squares refinement to 17858 unique data [R(int)=0.0339]. A multitude of least-squares difference-Fourier cycles were required to locate the remaining non-hydrogen atoms which were then allowed to refine freely. All full occupancy non-hydrogen atoms were refined anisotropically. The various disorders in the molecule of interest were optimized and one fully occupied disordered hexane molecule was determined while two additional disordered hexane molecules proved elusive regarding their successful optimization due to a couple of short contacts resulting with the main molecule. The system was reduced in symmetry to Ia and six hexane positions were located with two of these at half occupancy due to symmetry related overlaps so the overall number of hexane molecules in this asymmetric unit was believed to be five with a possibility of six should all locations be fully occupied. The troublesome regions were removed and refinement proceeded with a first attempt using Squeeze6. Squeeze indicated that all of the positions were not fully occupied by the electron count found so the system was returned to I2/a and the squeeze procedure implemented there. The two troublesome regions returned an electron count of 29 which was less than 36. This indicates that the two solvent regions containing the hexane molecules are not fully occupied and our resulting five molecules is an approximation. The final structure was refined to convergence with R(F)=8.22%, wR(F2)=21.70%, GOF=1.107 for all 17858 unique reflections [R(F)=6.12%, wR(F2)=20.06% for those 12369 data with Fo > 4 (Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. References: 1. Bruker (2005) SMART APEX (Version 2.14) and SAINT (Version 7.46a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2007/3), 'Siemens Area Detector Absorption Correction' Universit\"at G\"ottingen: G\"ottingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G\"ottingen: G\"ottingen, Germany. 6. Platon, A.L. Spek, (2003), J. Appl. Cryst. 36, 7-13. It should be so noted that a variety of approaches were attempted to resolve the disordered hexane molecules with an additional structure determination in Ia for additional supporting evidence as to number and disorders of hexane molecules. When all orientations were input in I2/a a couple of short interatomic distances resulted which necessitated the use of Squeeze since the advantage gained for true solvent determination has little to no bearing on the structure of interest. 043_ALERT_1_A Check Reported Molecular Weight ................ 2329.28 044_ALERT_1_A Calculated and Reported Dx Differ .............. ? 043-044: True Molecular weight based upon 5 disordered hexane molecules for each main molecule present has been used for Molecular weight and density. 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C81 C81 is a terminal atom in the one located and refined hexane molecule. ; _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^)+(0.1420P)^2^+0.2539P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17858 _refine_ls_number_parameters 707 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.2170 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.122 _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 0.437102(12) 0.697906(10) 0.410319(11) 0.03961(11) Uani 1 1 d . . . N1 N 0.39372(7) 0.64965(6) 0.35178(7) 0.0397(4) Uani 1 1 d . . . H1 H 0.3899(10) 0.6192(8) 0.3643(10) 0.043(6) Uiso 1 1 d . . . C1 C 0.49565(9) 0.70342(7) 0.50109(8) 0.0391(4) Uani 1 1 d . B . C2 C 0.46935(8) 0.68612(7) 0.53571(8) 0.0405(4) Uani 1 1 d . . . C3 C 0.50181(9) 0.68445(8) 0.59892(9) 0.0446(5) Uani 1 1 d . B . C4 C 0.56234(10) 0.69912(8) 0.62708(9) 0.0474(5) Uani 1 1 d . . . H4 H 0.5851 0.6976 0.6700 0.057 Uiso 1 1 calc R B . C5 C 0.59073(9) 0.71574(9) 0.59565(9) 0.0467(5) Uani 1 1 d . B . C6 C 0.55717(9) 0.71811(8) 0.53206(8) 0.0418(4) Uani 1 1 d . . . C7 C 0.47237(10) 0.66981(9) 0.63718(9) 0.0494(5) Uani 1 1 d . . . H7 H 0.4290 0.6616 0.6088 0.059 Uiso 1 1 calc R B . C8 C 0.50187(13) 0.62642(11) 0.67668(11) 0.0687(7) Uani 1 1 d . B . H8A H 0.5002 0.5995 0.6512 0.103 Uiso 1 1 calc R . . H8B H 0.4801 0.6181 0.6988 0.103 Uiso 1 1 calc R . . H8C H 0.5443 0.6337 0.7055 0.103 Uiso 1 1 calc R . . C9 C 0.47272(13) 0.71208(12) 0.67563(13) 0.0708(8) Uani 1 1 d . B . H9A H 0.4480 0.7044 0.6949 0.106 Uiso 1 1 calc R . . H9B H 0.4558 0.7402 0.6498 0.106 Uiso 1 1 calc R . . H9C H 0.5145 0.7188 0.7068 0.106 Uiso 1 1 calc R . . C10 C 0.65713(9) 0.73126(9) 0.63073(9) 0.0522(5) Uani 1 1 d . . . H10 H 0.6683 0.7457 0.6012 0.063 Uiso 1 1 calc R B . C11 C 0.69934(11) 0.68924(10) 0.66082(11) 0.0611(6) Uani 1 1 d . B . H11A H 0.6896 0.6746 0.6904 0.092 Uiso 1 1 calc R . . H11B H 0.7415 0.7004 0.6814 0.092 Uiso 1 1 calc R . . H11C H 0.6941 0.6656 0.6300 0.092 Uiso 1 1 calc R . . C12 C 0.66719(12) 0.76919(11) 0.67838(11) 0.0664(7) Uani 1 1 d . B . H12A H 0.6619 0.7548 0.7109 0.100 Uiso 1 1 calc R . . H12B H 0.6377 0.7951 0.6596 0.100 Uiso 1 1 calc R . . H12C H 0.7084 0.7821 0.6952 0.100 Uiso 1 1 calc R . . C19 C 0.37179(10) 0.75706(8) 0.50228(10) 0.0498(5) Uani 1 1 d . . . H19 H 0.4168 0.7599 0.5286 0.060 Uiso 1 1 calc R A 1 C20 C 0.35315(15) 0.79202(10) 0.45039(13) 0.0775(9) Uani 1 1 d . B . H20A H 0.3722 0.7829 0.4260 0.116 Uiso 1 1 calc R . . H20B H 0.3663 0.8242 0.4666 0.116 Uiso 1 1 calc R . . H20C H 0.3089 0.7915 0.4251 0.116 Uiso 1 1 calc R . . C21 C 0.34202(14) 0.77029(12) 0.54115(17) 0.0852(10) Uani 1 1 d . B . H21A H 0.2981 0.7739 0.5151 0.128 Uiso 1 1 calc R . . H21B H 0.3592 0.8004 0.5623 0.128 Uiso 1 1 calc R . . H21C H 0.3498 0.7450 0.5708 0.128 Uiso 1 1 calc R . . C13 C 0.40362(12) 0.6706(2) 0.5002(2) 0.0386(6) Uani 0.72 1 d PG B 1 C14 C 0.3581(2) 0.70501(14) 0.4782(2) 0.0421(7) Uani 0.72 1 d PG B 1 C15 C 0.29818(17) 0.69180(8) 0.43988(13) 0.0412(8) Uani 0.72 1 d PG B 1 H15 H 0.2671 0.7153 0.4248 0.049 Uiso 0.72 1 calc PR B 1 C16 C 0.28383(9) 0.64421(9) 0.42364(8) 0.0363(6) Uani 0.72 1 d PGD B 1 C17 C 0.32937(14) 0.60984(10) 0.44568(11) 0.0371(7) Uani 0.72 1 d PG B 1 H17 H 0.3196 0.5773 0.4346 0.045 Uiso 0.72 1 calc PR B 1 C18 C 0.38926(11) 0.62304(19) 0.48397(16) 0.0387(7) Uani 0.72 1 d PG B 1 C22 C 0.21799(12) 0.62786(11) 0.38269(12) 0.0402(6) Uani 0.72 1 d PDU B 1 H22 H 0.2193 0.5983 0.3611 0.048 Uiso 0.72 1 calc PR B 1 C23 C 0.1774(4) 0.6641(3) 0.3350(3) 0.0539(9) Uani 0.72 1 d PDU B 1 H23A H 0.1745 0.6932 0.3551 0.081 Uiso 0.72 1 calc PR B 1 H23B H 0.1368 0.6505 0.3106 0.081 Uiso 0.72 1 calc PR B 1 H23C H 0.1949 0.6720 0.3088 0.081 Uiso 0.72 1 calc PR B 1 C24 C 0.18820(15) 0.61503(17) 0.42102(15) 0.0626(9) Uani 0.72 1 d PDU B 1 H24A H 0.1866 0.6434 0.4429 0.094 Uiso 0.72 1 calc PR B 1 H24B H 0.2120 0.5901 0.4501 0.094 Uiso 0.72 1 calc PR B 1 H24C H 0.1469 0.6034 0.3947 0.094 Uiso 0.72 1 calc PR B 1 C13A C 0.4012(3) 0.6707(6) 0.5038(7) 0.0386(6) Uani 0.28 1 d PG B 2 C14A C 0.3574(6) 0.7063(4) 0.4861(6) 0.0421(7) Uani 0.28 1 d PG B 2 C15A C 0.2961(5) 0.6943(2) 0.4555(4) 0.0412(8) Uani 0.28 1 d PG B 2 H15A H 0.2661 0.7186 0.4435 0.049 Uiso 0.28 1 calc PR B 2 C16A C 0.2787(2) 0.6468(3) 0.4426(3) 0.0363(6) Uani 0.28 1 d PGD B 2 C17A C 0.3225(4) 0.6112(3) 0.4602(3) 0.0371(7) Uani 0.28 1 d PG B 2 H17A H 0.3106 0.5787 0.4514 0.045 Uiso 0.28 1 calc PR B 2 C18A C 0.3838(3) 0.6232(5) 0.4908(5) 0.0387(7) Uani 0.28 1 d PG B 2 C22A C 0.2091(3) 0.6354(2) 0.4062(3) 0.0402(6) Uani 0.28 1 d PDU B 2 H22A H 0.1888 0.6513 0.4272 0.048 Uiso 0.28 1 calc PR B 2 C23A C 0.1843(13) 0.6576(8) 0.3439(8) 0.0539(9) Uani 0.28 1 d PDU B 2 H23D H 0.2124 0.6514 0.3281 0.081 Uiso 0.28 1 calc PR B 2 H23E H 0.1799 0.6922 0.3467 0.081 Uiso 0.28 1 calc PR B 2 H23F H 0.1446 0.6436 0.3166 0.081 Uiso 0.28 1 calc PR B 2 C24A C 0.1931(3) 0.5829(3) 0.4001(3) 0.0447(16) Uani 0.28 1 d PDU B 2 H24D H 0.1489 0.5793 0.3806 0.067 Uiso 0.28 1 calc PR B 2 H24E H 0.2116 0.5682 0.4403 0.067 Uiso 0.28 1 calc PR B 2 H24F H 0.2084 0.5672 0.3754 0.067 Uiso 0.28 1 calc PR B 2 C25 C 0.43600(9) 0.58322(8) 0.51221(9) 0.0450(5) Uani 1 1 d . . . H25 H 0.4706 0.5962 0.5501 0.054 Uiso 1 1 calc R B 1 C26 C 0.46082(11) 0.57051(8) 0.46934(10) 0.0521(5) Uani 1 1 d . B . H26A H 0.4936 0.5471 0.4888 0.078 Uiso 1 1 calc R . . H26B H 0.4766 0.5994 0.4598 0.078 Uiso 1 1 calc R . . H26C H 0.4282 0.5569 0.4319 0.078 Uiso 1 1 calc R . . C27 C 0.41364(12) 0.53806(9) 0.52931(11) 0.0569(6) Uani 1 1 d . B . H27A H 0.3982 0.5463 0.5572 0.085 Uiso 1 1 calc R . . H27B H 0.4473 0.5154 0.5490 0.085 Uiso 1 1 calc R . . H27C H 0.3810 0.5235 0.4927 0.085 Uiso 1 1 calc R . . C28 C 0.58635(9) 0.73759(8) 0.49612(8) 0.0436(5) Uani 1 1 d . B . C29 C 0.61060(9) 0.70602(8) 0.46996(9) 0.0456(5) Uani 1 1 d . . . C30 C 0.63550(10) 0.72526(9) 0.43548(9) 0.0526(5) Uani 1 1 d . B . H30 H 0.6517 0.7041 0.4174 0.063 Uiso 1 1 calc R . . C31 C 0.63746(11) 0.77359(10) 0.42673(10) 0.0556(6) Uani 1 1 d . . . C32 C 0.61508(11) 0.80369(9) 0.45478(10) 0.0559(6) Uani 1 1 d . B . H32 H 0.6167 0.8372 0.4498 0.067 Uiso 1 1 calc R . . C33 C 0.59040(9) 0.78698(9) 0.48977(9) 0.0495(5) Uani 1 1 d . . . C34 C 0.61250(10) 0.65248(9) 0.47962(10) 0.0510(5) Uani 1 1 d . B . H34 H 0.5977 0.6462 0.5093 0.061 Uiso 1 1 calc R . . C35 C 0.57119(11) 0.62516(9) 0.42185(11) 0.0562(6) Uani 1 1 d . . . H35A H 0.5292 0.6362 0.4061 0.084 Uiso 1 1 calc R B . H35B H 0.5735 0.5909 0.4308 0.084 Uiso 1 1 calc R . . H35C H 0.5843 0.6308 0.3916 0.084 Uiso 1 1 calc R . . C36 C 0.67720(12) 0.63311(12) 0.50683(12) 0.0717(8) Uani 1 1 d . . . H36A H 0.6908 0.6343 0.4764 0.108 Uiso 1 1 calc R B . H36B H 0.6780 0.6000 0.5197 0.108 Uiso 1 1 calc R . . H36C H 0.7043 0.6526 0.5418 0.108 Uiso 1 1 calc R . . C37 C 0.66481(13) 0.79452(11) 0.38918(12) 0.0672(7) Uani 0.57 1 d P B 1 H37 H 0.6736 0.8289 0.4011 0.081 Uiso 0.57 1 calc PR B 1 C38 C 0.6240(2) 0.7940(2) 0.32343(19) 0.0661(13) Uani 0.57 1 d P B 1 H38A H 0.6181 0.7610 0.3087 0.099 Uiso 0.57 1 calc PR B 1 H38B H 0.6421 0.8128 0.3034 0.099 Uiso 0.57 1 calc PR B 1 H38C H 0.5848 0.8079 0.3144 0.099 Uiso 0.57 1 calc PR B 1 C39 C 0.7273(2) 0.7711(3) 0.4032(3) 0.0782(16) Uani 0.57 1 d P B 1 H39A H 0.7203 0.7385 0.3872 0.117 Uiso 0.57 1 calc PR B 1 H39B H 0.7543 0.7704 0.4470 0.117 Uiso 0.57 1 calc PR B 1 H39C H 0.7461 0.7900 0.3839 0.117 Uiso 0.57 1 calc PR B 1 C37A C 0.66481(13) 0.79452(11) 0.38918(12) 0.0672(7) Uani 0.43 1 d P B 2 H37A H 0.6380 0.8222 0.3673 0.081 Uiso 0.43 1 calc PR B 2 C38A C 0.7208(4) 0.8145(5) 0.4254(4) 0.128(5) Uani 0.43 1 d P B 2 H38D H 0.7479 0.7903 0.4537 0.191 Uiso 0.43 1 calc PR B 2 H38E H 0.7165 0.8411 0.4482 0.191 Uiso 0.43 1 calc PR B 2 H38F H 0.7379 0.8261 0.4003 0.191 Uiso 0.43 1 calc PR B 2 C39A C 0.6584(4) 0.7609(4) 0.3398(4) 0.091(2) Uani 0.43 1 d P B 2 H39D H 0.6695 0.7775 0.3124 0.136 Uiso 0.43 1 calc PR B 2 H39E H 0.6162 0.7499 0.3170 0.136 Uiso 0.43 1 calc PR B 2 H39F H 0.6852 0.7333 0.3578 0.136 Uiso 0.43 1 calc PR B 2 C40 C 0.57025(11) 0.82218(9) 0.52296(11) 0.0580(6) Uani 1 1 d . B . H40 H 0.5654 0.8039 0.5544 0.070 Uiso 1 1 calc R . . C41 C 0.51005(16) 0.84427(14) 0.48101(14) 0.1000(12) Uani 1 1 d . . . H41A H 0.5125 0.8601 0.4476 0.150 Uiso 1 1 calc R B . H41B H 0.4995 0.8678 0.5032 0.150 Uiso 1 1 calc R . . H41C H 0.4788 0.8194 0.4648 0.150 Uiso 1 1 calc R . . C42 C 0.61786(17) 0.86095(13) 0.55524(16) 0.0936(10) Uani 1 1 d . . . H42A H 0.6231 0.8797 0.5253 0.140 Uiso 1 1 calc R B . H42B H 0.6566 0.8461 0.5835 0.140 Uiso 1 1 calc R . . H42C H 0.6044 0.8819 0.5775 0.140 Uiso 1 1 calc R . . C43 C 0.37000(9) 0.64810(7) 0.28976(8) 0.0394(4) Uani 1 1 d . . . C44 C 0.36284(9) 0.69123(7) 0.25823(9) 0.0424(5) Uani 1 1 d . . . C45 C 0.33981(12) 0.69062(8) 0.19584(10) 0.0528(6) Uani 1 1 d . . . H45 H 0.3354 0.7198 0.1750 0.063 Uiso 1 1 calc R . . C46 C 0.32317(13) 0.64819(9) 0.16345(10) 0.0612(6) Uani 1 1 d . . . H46 H 0.3074 0.6483 0.1208 0.073 Uiso 1 1 calc R . . C47 C 0.32981(11) 0.60566(9) 0.19417(9) 0.0552(6) Uani 1 1 d . . . H47 H 0.3185 0.5765 0.1722 0.066 Uiso 1 1 calc R . . C48 C 0.35274(9) 0.60489(7) 0.25663(8) 0.0428(4) Uani 1 1 d . . . C49 C 0.37950(9) 0.73775(8) 0.29087(8) 0.0444(5) Uani 1 1 d . . . C50 C 0.33567(10) 0.76474(8) 0.29716(9) 0.0508(5) Uani 1 1 d . . . C51 C 0.34746(12) 0.81219(9) 0.31403(11) 0.0622(7) Uani 1 1 d . . . H51 H 0.3174 0.8306 0.3172 0.075 Uiso 1 1 calc R . . C52 C 0.40226(12) 0.83377(9) 0.32650(11) 0.0683(8) Uani 1 1 d . . . C53 C 0.44709(12) 0.80535(9) 0.32633(11) 0.0647(7) Uani 1 1 d . . . H53 H 0.4860 0.8188 0.3385 0.078 Uiso 1 1 calc R . . C54 C 0.43714(10) 0.75766(8) 0.30887(9) 0.0522(6) Uani 1 1 d . . . C55 C 0.27473(10) 0.74361(8) 0.28218(10) 0.0505(5) Uani 1 1 d . . . H55A H 0.2624 0.7554 0.3116 0.061 Uiso 1 1 calc R . . H55B H 0.2785 0.7084 0.2862 0.061 Uiso 1 1 calc R . . C56 C 0.41028(16) 0.88704(10) 0.33978(17) 0.1047(14) Uani 1 1 d . . . H56A H 0.4529 0.8958 0.3546 0.157 Uiso 1 1 calc R . . H56B H 0.3986 0.8948 0.3706 0.157 Uiso 1 1 calc R . . H56C H 0.3845 0.9049 0.3027 0.157 Uiso 1 1 calc R . . C57 C 0.48555(11) 0.72858(11) 0.30573(12) 0.0660(7) Uani 1 1 d . . . H57A H 0.4760 0.7251 0.2634 0.099 Uiso 1 1 calc R . . H57B H 0.4875 0.6969 0.3232 0.099 Uiso 1 1 calc R . . H57C H 0.5249 0.7446 0.3286 0.099 Uiso 1 1 calc R . . C58 C 0.35887(9) 0.55896(7) 0.28903(8) 0.0416(4) Uani 1 1 d . . . C59 C 0.41200(10) 0.53143(8) 0.31013(10) 0.0495(5) Uani 1 1 d . . . C60 C 0.41682(11) 0.48972(8) 0.34189(11) 0.0580(6) Uani 1 1 d . . . H60 H 0.4525 0.4709 0.3557 0.070 Uiso 1 1 calc R . . C61 C 0.37134(11) 0.47452(8) 0.35408(10) 0.0558(6) Uani 1 1 d . . . C62 C 0.31893(11) 0.50163(8) 0.33162(10) 0.0522(5) Uani 1 1 d . . . H62 H 0.2868 0.4914 0.3386 0.063 Uiso 1 1 calc R . . C63 C 0.31191(9) 0.54368(8) 0.29898(9) 0.0447(5) Uani 1 1 d . . . C64 C 0.46273(12) 0.54693(10) 0.29840(13) 0.0658(7) Uani 1 1 d . . . H64A H 0.4982 0.5265 0.3212 0.099 Uiso 1 1 calc R . . H64B H 0.4735 0.5802 0.3113 0.099 Uiso 1 1 calc R . . H64C H 0.4495 0.5442 0.2551 0.099 Uiso 1 1 calc R . . C65 C 0.37829(15) 0.43026(10) 0.39085(15) 0.0817(9) Uani 1 1 d . . . H65A H 0.4015 0.4063 0.3823 0.122 Uiso 1 1 calc R . . H65B H 0.3380 0.4175 0.3801 0.122 Uiso 1 1 calc R . . H65C H 0.3998 0.4383 0.4340 0.122 Uiso 1 1 calc R . . C66 C 0.25429(11) 0.57209(10) 0.27451(12) 0.0591(6) Uani 1 1 d . . . H66A H 0.2634 0.6042 0.2921 0.089 Uiso 1 1 calc R . . H66B H 0.2259 0.5562 0.2850 0.089 Uiso 1 1 calc R . . H66C H 0.2360 0.5744 0.2304 0.089 Uiso 1 1 calc R . . C81 C 0.7922(7) 0.9372(7) 0.3095(9) 0.217(6) Uiso 0.50 1 d PDU C 1 H81A H 0.7891 0.9493 0.2716 0.325 Uiso 0.50 1 calc PR C 1 H81B H 0.8259 0.9145 0.3280 0.325 Uiso 0.50 1 calc PR C 1 H81C H 0.7994 0.9639 0.3373 0.325 Uiso 0.50 1 calc PR C 1 C82 C 0.7263(5) 0.9093(4) 0.2946(5) 0.126(3) Uiso 0.50 1 d PDU C 1 H82A H 0.6971 0.9074 0.2508 0.151 Uiso 0.50 1 calc PR C 1 H82B H 0.7330 0.8773 0.3134 0.151 Uiso 0.50 1 calc PR C 1 C83 C 0.7081(5) 0.9490(5) 0.3294(6) 0.145(2) Uiso 0.50 1 d PDU C 1 H83A H 0.7385 0.9504 0.3728 0.174 Uiso 0.50 1 calc PR C 1 H83B H 0.7044 0.9810 0.3112 0.174 Uiso 0.50 1 calc PR C 1 C84 C 0.6463(4) 0.9316(4) 0.3205(5) 0.120(3) Uiso 0.50 1 d PDU C 1 H84A H 0.6161 0.9326 0.2770 0.144 Uiso 0.50 1 calc PR C 1 H84B H 0.6500 0.8981 0.3344 0.144 Uiso 0.50 1 calc PR C 1 C85 C 0.6246(6) 0.9616(5) 0.3548(6) 0.159(4) Uiso 0.50 1 d PDU C 1 H85A H 0.6260 0.9958 0.3456 0.191 Uiso 0.50 1 calc PR C 1 H85B H 0.6505 0.9566 0.3988 0.191 Uiso 0.50 1 calc PR C 1 C86 C 0.5565(6) 0.9457(7) 0.3341(8) 0.196(4) Uiso 0.50 1 d PDU C 1 H86A H 0.5383 0.9324 0.2931 0.293 Uiso 0.50 1 calc PR C 1 H86B H 0.5330 0.9734 0.3345 0.293 Uiso 0.50 1 calc PR C 1 H86C H 0.5565 0.9213 0.3620 0.293 Uiso 0.50 1 calc PR C 1 C81A C 0.7689(6) 0.9133(4) 0.2884(5) 0.137(3) Uiso 0.50 1 d PDU D 2 H81D H 0.7730 0.8792 0.2986 0.206 Uiso 0.50 1 calc PR D 2 H81E H 0.8073 0.9252 0.2922 0.206 Uiso 0.50 1 calc PR D 2 H81F H 0.7364 0.9177 0.2467 0.206 Uiso 0.50 1 calc PR D 2 C82A C 0.7538(6) 0.9404(5) 0.3310(6) 0.172(4) Uiso 0.50 1 d PDU D 2 H82C H 0.7798 0.9289 0.3728 0.206 Uiso 0.50 1 calc PR D 2 H82D H 0.7623 0.9747 0.3296 0.206 Uiso 0.50 1 calc PR D 2 C83A C 0.6925(5) 0.9344(5) 0.3153(6) 0.145(2) Uiso 0.50 1 d PDU D 2 H83C H 0.6688 0.9512 0.2763 0.174 Uiso 0.50 1 calc PR D 2 H83D H 0.6837 0.9000 0.3066 0.174 Uiso 0.50 1 calc PR D 2 C84A C 0.6673(5) 0.9475(5) 0.3512(6) 0.163(3) Uiso 0.50 1 d PDU D 2 H84C H 0.6776 0.9813 0.3632 0.196 Uiso 0.50 1 calc PR D 2 H84D H 0.6862 0.9281 0.3887 0.196 Uiso 0.50 1 calc PR D 2 C85A C 0.6012(6) 0.9419(6) 0.3228(7) 0.185(4) Uiso 0.50 1 d PDU D 2 H85C H 0.5908 0.9090 0.3070 0.223 Uiso 0.50 1 calc PR D 2 H85D H 0.5823 0.9639 0.2877 0.223 Uiso 0.50 1 calc PR D 2 C86A C 0.5739(7) 0.9511(7) 0.3619(8) 0.196(4) Uiso 0.50 1 d PDU D 2 H86D H 0.6060 0.9591 0.4028 0.293 Uiso 0.50 1 calc PR D 2 H86E H 0.5523 0.9225 0.3636 0.293 Uiso 0.50 1 calc PR D 2 H86F H 0.5454 0.9778 0.3455 0.293 Uiso 0.50 1 calc PR D 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 0.03162(16) 0.05120(19) 0.02412(16) -0.00287(11) 0.00402(12) 0.00045(11) N1 0.0408(9) 0.0453(9) 0.0246(7) 0.0027(6) 0.0090(6) -0.0002(7) C1 0.0326(9) 0.0523(11) 0.0258(8) -0.0049(8) 0.0089(7) 0.0043(8) C2 0.0301(9) 0.0548(11) 0.0292(9) -0.0081(8) 0.0084(7) 0.0058(8) C3 0.0378(10) 0.0634(13) 0.0282(9) -0.0071(9) 0.0124(8) 0.0028(9) C4 0.0369(10) 0.0742(15) 0.0232(9) -0.0041(9) 0.0081(8) 0.0024(9) C5 0.0349(10) 0.0658(13) 0.0287(9) -0.0075(9) 0.0068(8) 0.0015(9) C6 0.0329(9) 0.0573(12) 0.0288(9) -0.0045(8) 0.0099(8) 0.0052(8) C7 0.0424(11) 0.0731(15) 0.0314(10) -0.0089(10) 0.0167(9) -0.0036(10) C8 0.0721(17) 0.094(2) 0.0420(12) 0.0084(13) 0.0293(12) 0.0106(14) C9 0.0680(16) 0.102(2) 0.0584(15) -0.0305(15) 0.0432(14) -0.0198(15) C10 0.0343(10) 0.0816(16) 0.0283(9) -0.0025(10) 0.0053(8) -0.0040(10) C11 0.0354(11) 0.0873(18) 0.0418(12) 0.0034(11) 0.0037(9) -0.0005(11) C12 0.0498(13) 0.0926(19) 0.0373(11) -0.0161(12) 0.0055(10) -0.0100(13) C19 0.0344(10) 0.0541(12) 0.0539(12) -0.0091(10) 0.0157(9) -0.0005(9) C20 0.082(2) 0.0515(14) 0.0637(17) -0.0029(12) 0.0072(15) 0.0011(13) C21 0.0679(18) 0.091(2) 0.115(3) -0.0462(19) 0.0586(19) -0.0199(16) C13 0.0321(9) 0.0518(11) 0.0267(11) -0.0030(9) 0.0101(8) 0.0030(8) C14 0.0334(10) 0.0521(12) 0.0351(17) -0.0040(10) 0.0120(10) 0.0012(8) C15 0.0331(11) 0.0531(13) 0.033(2) -0.0009(12) 0.0124(14) 0.0042(9) C16 0.0372(11) 0.0524(13) 0.0203(14) -0.0027(12) 0.0147(10) 0.0002(10) C17 0.0404(13) 0.0460(12) 0.0227(16) -0.0010(11) 0.0134(11) 0.0000(10) C18 0.0362(11) 0.0530(12) 0.0246(13) -0.0011(10) 0.0129(9) 0.0047(10) C22 0.0340(12) 0.0555(15) 0.0293(14) -0.0025(11) 0.0138(10) -0.0010(10) C23 0.033(2) 0.066(3) 0.040(2) 0.0082(13) -0.0001(19) 0.001(2) C24 0.0389(16) 0.102(3) 0.0437(17) 0.0007(18) 0.0172(13) -0.0119(18) C13A 0.0321(9) 0.0518(11) 0.0267(11) -0.0030(9) 0.0101(8) 0.0030(8) C14A 0.0334(10) 0.0521(12) 0.0351(17) -0.0040(10) 0.0120(10) 0.0012(8) C15A 0.0331(11) 0.0531(13) 0.033(2) -0.0009(12) 0.0124(14) 0.0042(9) C16A 0.0372(11) 0.0524(13) 0.0203(14) -0.0027(12) 0.0147(10) 0.0002(10) C17A 0.0404(13) 0.0460(12) 0.0227(16) -0.0010(11) 0.0134(11) 0.0000(10) C18A 0.0362(11) 0.0530(12) 0.0246(13) -0.0011(10) 0.0129(9) 0.0047(10) C22A 0.0340(12) 0.0555(15) 0.0293(14) -0.0025(11) 0.0138(10) -0.0010(10) C23A 0.033(2) 0.066(3) 0.040(2) 0.0082(13) -0.0001(19) 0.001(2) C24A 0.044(4) 0.052(4) 0.035(3) -0.004(3) 0.017(3) -0.008(3) C25 0.0434(11) 0.0543(12) 0.0296(9) 0.0018(8) 0.0114(8) 0.0088(9) C26 0.0578(13) 0.0557(13) 0.0416(11) 0.0088(9) 0.0231(10) 0.0157(10) C27 0.0619(14) 0.0615(14) 0.0476(12) 0.0142(10) 0.0269(11) 0.0167(11) C28 0.0297(9) 0.0653(13) 0.0247(8) -0.0014(8) 0.0043(7) 0.0005(8) C29 0.0353(10) 0.0678(14) 0.0276(9) 0.0024(9) 0.0102(8) 0.0033(9) C30 0.0445(11) 0.0774(16) 0.0320(10) 0.0003(10) 0.0153(9) 0.0042(11) C31 0.0468(12) 0.0784(17) 0.0327(10) 0.0066(10) 0.0121(9) -0.0029(11) C32 0.0484(13) 0.0676(15) 0.0358(11) -0.0005(10) 0.0078(10) -0.0060(10) C33 0.0361(10) 0.0671(14) 0.0291(9) -0.0041(9) 0.0030(8) -0.0020(9) C34 0.0471(12) 0.0700(14) 0.0394(11) 0.0075(10) 0.0236(9) 0.0136(10) C35 0.0603(14) 0.0627(14) 0.0508(13) 0.0019(11) 0.0310(11) 0.0077(11) C36 0.0535(14) 0.103(2) 0.0579(15) 0.0194(14) 0.0262(12) 0.0262(14) C37 0.0601(15) 0.0917(19) 0.0465(13) 0.0133(13) 0.0231(12) -0.0056(13) C38 0.049(2) 0.102(4) 0.040(2) 0.015(2) 0.0159(19) -0.010(2) C39 0.046(2) 0.127(5) 0.061(3) 0.032(3) 0.026(2) 0.014(3) C37A 0.0601(15) 0.0917(19) 0.0465(13) 0.0133(13) 0.0231(12) -0.0056(13) C38A 0.078(6) 0.218(12) 0.060(5) 0.025(6) 0.012(4) -0.077(7) C39A 0.073(5) 0.143(7) 0.086(5) 0.012(5) 0.061(4) -0.001(5) C40 0.0498(13) 0.0656(14) 0.0427(12) -0.0117(11) 0.0098(10) -0.0012(11) C41 0.084(2) 0.120(3) 0.0625(18) -0.0237(18) 0.0087(16) 0.042(2) C42 0.096(2) 0.095(2) 0.087(2) -0.0425(19) 0.0422(19) -0.0293(19) C43 0.0350(9) 0.0518(11) 0.0256(8) 0.0014(8) 0.0101(7) 0.0002(8) C44 0.0384(10) 0.0546(12) 0.0267(9) 0.0011(8) 0.0097(8) -0.0051(8) C45 0.0635(14) 0.0582(13) 0.0302(10) 0.0067(9) 0.0176(10) -0.0068(10) C46 0.0792(17) 0.0719(15) 0.0258(10) -0.0006(10) 0.0201(10) -0.0063(13) C47 0.0684(15) 0.0598(13) 0.0306(10) -0.0039(9) 0.0186(10) -0.0021(11) C48 0.0443(10) 0.0506(11) 0.0287(9) -0.0020(8) 0.0138(8) 0.0006(9) C49 0.0435(11) 0.0492(11) 0.0286(9) 0.0052(8) 0.0079(8) -0.0059(9) C50 0.0483(12) 0.0537(12) 0.0336(10) -0.0004(9) 0.0064(9) -0.0046(10) C51 0.0594(15) 0.0499(13) 0.0478(13) -0.0014(10) 0.0026(11) 0.0001(11) C52 0.0626(15) 0.0527(13) 0.0469(13) 0.0038(10) -0.0074(11) -0.0119(12) C53 0.0487(13) 0.0660(15) 0.0427(12) 0.0132(10) -0.0070(10) -0.0169(11) C54 0.0427(11) 0.0637(14) 0.0307(10) 0.0141(9) 0.0023(8) -0.0088(10) C55 0.0469(12) 0.0510(12) 0.0426(11) -0.0012(9) 0.0129(10) -0.0012(9) C56 0.078(2) 0.0525(15) 0.105(2) 0.0045(16) -0.0184(18) -0.0142(14) C57 0.0443(13) 0.0892(19) 0.0533(14) 0.0221(13) 0.0146(11) -0.0045(12) C58 0.0461(11) 0.0445(11) 0.0279(9) -0.0036(8) 0.0129(8) 0.0020(8) C59 0.0439(11) 0.0566(13) 0.0415(11) -0.0099(9) 0.0155(9) 0.0006(9) C60 0.0488(13) 0.0508(13) 0.0556(13) -0.0041(10) 0.0103(10) 0.0085(10) C61 0.0549(13) 0.0458(12) 0.0466(12) -0.0026(9) 0.0086(10) 0.0008(10) C62 0.0535(13) 0.0503(12) 0.0470(12) 0.0002(10) 0.0197(10) -0.0019(10) C63 0.0426(11) 0.0515(11) 0.0337(10) -0.0046(8) 0.0134(8) 0.0026(9) C64 0.0484(13) 0.0786(17) 0.0692(16) -0.0055(13) 0.0273(12) 0.0006(12) C65 0.083(2) 0.0549(15) 0.085(2) 0.0154(14) 0.0228(17) -0.0006(14) C66 0.0545(13) 0.0702(15) 0.0542(13) 0.0108(11) 0.0274(11) 0.0151(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9086(17) . ? Fe1 C1 2.0447(18) . ? N1 C43 1.380(2) . ? N1 H1 0.93(2) . ? C1 C2 1.411(3) . ? C1 C6 1.416(3) . ? C2 C3 1.398(3) . ? C2 C13 1.514(3) . ? C2 C13A 1.561(6) . ? C3 C4 1.394(3) . ? C3 C7 1.529(3) . ? C4 C5 1.379(3) . ? C4 H4 0.9500 . ? C5 C6 1.408(3) . ? C5 C10 1.527(3) . ? C6 C28 1.517(3) . ? C7 C8 1.519(4) . ? C7 C9 1.528(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.520(3) . ? C10 C12 1.532(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C19 C14A 1.477(9) . ? C19 C20 1.517(4) . ? C19 C21 1.539(4) . ? C19 C14 1.553(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 C22 1.538(3) . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C25 1.524(4) . ? C22 C24 1.525(4) . ? C22 C23 1.529(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C13A C14A 1.3900 . ? C13A C18A 1.3900 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A C17A 1.3900 . ? C16A C22A 1.567(7) . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C25 1.606(9) . ? C22A C24A 1.514(7) . ? C22A C23A 1.517(8) . ? C22A H22A 1.0000 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25 C26 1.529(3) . ? C25 C27 1.529(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.402(3) . ? C28 C29 1.407(3) . ? C29 C30 1.402(3) . ? C29 C34 1.516(3) . ? C30 C31 1.376(4) . ? C30 H30 0.9500 . ? C31 C32 1.383(4) . ? C31 C37 1.531(3) . ? C32 C33 1.383(3) . ? C32 H32 0.9500 . ? C33 C40 1.530(3) . ? C34 C35 1.525(3) . ? C34 C36 1.527(3) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.470(5) . ? C37 C39 1.576(6) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40 C41 1.499(4) . ? C40 C42 1.528(4) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.410(3) . ? C43 C48 1.415(3) . ? C44 C45 1.391(3) . ? C44 C49 1.490(3) . ? C45 C46 1.387(3) . ? C45 H45 0.9500 . ? C46 C47 1.387(3) . ? C46 H46 0.9500 . ? C47 C48 1.393(3) . ? C47 H47 0.9500 . ? C48 C58 1.492(3) . ? C49 C50 1.407(3) . ? C49 C54 1.407(3) . ? C50 C51 1.384(3) . ? C50 C55 1.510(3) . ? C51 C52 1.394(4) . ? C51 H51 0.9500 . ? C52 C53 1.381(4) . ? C52 C56 1.521(4) . ? C53 C54 1.391(3) . ? C53 H53 0.9500 . ? C54 C57 1.498(4) . ? C55 C55 1.537(4) 7_565 ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C63 1.388(3) . ? C58 C59 1.405(3) . ? C59 C60 1.389(3) . ? C59 C64 1.506(3) . ? C60 C61 1.386(4) . ? C60 H60 0.9500 . ? C61 C62 1.383(3) . ? C61 C65 1.508(4) . ? C62 C63 1.399(3) . ? C62 H62 0.9500 . ? C63 C66 1.499(3) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C81 C82 1.700(14) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.614(12) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.538(12) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.484(12) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.592(14) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C81A C82A 1.506(13) . ? C81A H81D 0.9800 . ? C81A H81E 0.9800 . ? C81A H81F 0.9800 . ? C82A C83A 1.402(13) . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? C83A C84A 1.385(12) . ? C83A H83C 0.9900 . ? C83A H83D 0.9900 . ? C84A C85A 1.465(14) . ? C84A H84C 0.9900 . ? C84A H84D 0.9900 . ? C85A C86A 1.472(14) . ? C85A H85C 0.9900 . ? C85A H85D 0.9900 . ? C86A H86D 0.9800 . ? C86A H86E 0.9800 . ? C86A H86F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 C1 138.91(8) . . ? C43 N1 Fe1 132.26(14) . . ? C43 N1 H1 107.4(14) . . ? Fe1 N1 H1 120.0(13) . . ? C2 C1 C6 118.11(17) . . ? C2 C1 Fe1 111.63(13) . . ? C6 C1 Fe1 130.08(14) . . ? C3 C2 C1 121.86(18) . . ? C3 C2 C13 122.3(3) . . ? C1 C2 C13 115.8(3) . . ? C3 C2 C13A 118.0(7) . . ? C1 C2 C13A 120.0(6) . . ? C4 C3 C2 117.62(19) . . ? C4 C3 C7 119.93(18) . . ? C2 C3 C7 122.38(18) . . ? C5 C4 C3 123.14(18) . . ? C5 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C4 C5 C6 118.65(18) . . ? C4 C5 C10 119.15(17) . . ? C6 C5 C10 122.20(19) . . ? C5 C6 C1 120.60(19) . . ? C5 C6 C28 120.10(18) . . ? C1 C6 C28 119.28(16) . . ? C8 C7 C9 110.6(2) . . ? C8 C7 C3 113.41(19) . . ? C9 C7 C3 109.7(2) . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C3 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C5 111.9(2) . . ? C11 C10 C12 109.53(19) . . ? C5 C10 C12 111.87(19) . . ? C11 C10 H10 107.8 . . ? C5 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? 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 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14A C19 C20 116.8(6) . . ? C14A C19 C21 106.1(6) . . ? C20 C19 C21 110.6(2) . . ? C20 C19 C14 110.5(3) . . ? C21 C19 C14 113.0(3) . . ? C14A C19 H19 107.9 . . ? C20 C19 H19 107.5 . . ? C21 C19 H19 107.5 . . ? C14 C19 H19 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C13 C18 120.0 . . ? C14 C13 C2 119.4(4) . . ? C18 C13 C2 120.2(4) . . ? C13 C14 C15 120.0 . . ? C13 C14 C19 120.6(3) . . ? C15 C14 C19 118.9(3) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 C22 121.7(2) . . ? C17 C16 C22 118.3(2) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 C25 117.5(3) . . ? C13 C18 C25 122.1(3) . . ? C24 C22 C23 108.1(5) . . ? C24 C22 C16 110.0(2) . . ? C23 C22 C16 115.0(4) . . ? C24 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? C16 C22 H22 107.8 . . ? 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 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14A C13A C18A 120.0 . . ? C14A C13A C2 118.0(10) . . ? C18A C13A C2 121.9(10) . . ? C15A C14A C13A 120.0 . . ? C15A C14A C19 116.4(9) . . ? C13A C14A C19 123.4(9) . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C17A C16A C15A 120.0 . . ? C17A C16A C22A 122.1(6) . . ? C15A C16A C22A 117.9(6) . . ? C16A C17A C18A 120.0 . . ? C16A C17A H17A 120.0 . . ? C18A C17A H17A 120.0 . . ? C17A C18A C13A 120.0 . . ? C17A C18A C25 121.7(9) . . ? C13A C18A C25 118.3(9) . . ? C24A C22A C23A 109.7(9) . . ? C24A C22A C16A 115.0(6) . . ? C23A C22A C16A 107.9(12) . . ? C24A C22A H22A 108.0 . . ? C23A C22A H22A 108.0 . . ? C16A C22A H22A 108.0 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C18 C25 C26 109.0(2) . . ? C18 C25 C27 115.6(2) . . ? C26 C25 C27 109.77(18) . . ? C26 C25 C18A 118.1(5) . . ? C27 C25 C18A 108.6(5) . . ? C18 C25 H25 107.4 . . ? C26 C25 H25 107.4 . . ? C27 C25 H25 107.4 . . ? C18A C25 H25 105.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 119.7(2) . . ? C33 C28 C6 120.40(19) . . ? C29 C28 C6 119.9(2) . . ? C30 C29 C28 118.3(2) . . ? C30 C29 C34 119.4(2) . . ? C28 C29 C34 122.23(19) . . ? C31 C30 C29 122.6(2) . . ? C31 C30 H30 118.7 . . ? C29 C30 H30 118.7 . . ? C30 C31 C32 117.5(2) . . ? C30 C31 C37 122.5(2) . . ? C32 C31 C37 119.9(2) . . ? C31 C32 C33 122.6(2) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C32 C33 C28 119.1(2) . . ? C32 C33 C40 120.0(2) . . ? C28 C33 C40 120.8(2) . . ? C29 C34 C35 112.85(18) . . ? C29 C34 C36 111.6(2) . . ? C35 C34 C36 109.7(2) . . ? C29 C34 H34 107.5 . . ? C35 C34 H34 107.5 . . ? C36 C34 H34 107.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C31 114.7(3) . . ? C38 C37 C39 109.0(4) . . ? C31 C37 C39 113.5(3) . . ? C38 C37 H37 106.3 . . ? C31 C37 H37 106.3 . . ? C39 C37 H37 106.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? H38D C38A H38E 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? H39D C39A H39E 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C41 C40 C42 110.3(3) . . ? C41 C40 C33 111.6(2) . . ? C42 C40 C33 111.7(2) . . ? C41 C40 H40 107.7 . . ? C42 C40 H40 107.7 . . ? C33 C40 H40 107.7 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1 C43 C44 118.71(18) . . ? N1 C43 C48 122.57(18) . . ? C44 C43 C48 118.72(17) . . ? C45 C44 C43 119.90(19) . . ? C45 C44 C49 119.28(18) . . ? C43 C44 C49 120.83(17) . . ? C46 C45 C44 121.3(2) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 119.07(19) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C46 C47 C48 121.2(2) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 119.79(19) . . ? C47 C48 C58 120.69(18) . . ? C43 C48 C58 119.53(16) . . ? C50 C49 C54 119.4(2) . . ? C50 C49 C44 120.41(19) . . ? C54 C49 C44 119.7(2) . . ? C51 C50 C49 119.2(2) . . ? C51 C50 C55 119.6(2) . . ? C49 C50 C55 121.1(2) . . ? C50 C51 C52 121.8(3) . . ? C50 C51 H51 119.1 . . ? C52 C51 H51 119.1 . . ? C53 C52 C51 117.9(2) . . ? C53 C52 C56 123.0(3) . . ? C51 C52 C56 119.1(3) . . ? C52 C53 C54 122.1(2) . . ? C52 C53 H53 118.9 . . ? C54 C53 H53 118.9 . . ? C53 C54 C49 118.9(2) . . ? C53 C54 C57 120.8(2) . . ? C49 C54 C57 120.2(2) . . ? C50 C55 C55 112.2(2) . 7_565 ? C50 C55 H55A 109.2 . . ? C55 C55 H55A 109.2 7_565 . ? C50 C55 H55B 109.2 . . ? C55 C55 H55B 109.2 7_565 . ? H55A C55 H55B 107.9 . . ? C52 C56 H56A 109.5 . . ? C52 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C52 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C63 C58 C59 119.9(2) . . ? C63 C58 C48 119.56(18) . . ? C59 C58 C48 120.57(19) . . ? C60 C59 C58 118.8(2) . . ? C60 C59 C64 120.7(2) . . ? C58 C59 C64 120.5(2) . . ? C61 C60 C59 122.3(2) . . ? C61 C60 H60 118.8 . . ? C59 C60 H60 118.8 . . ? C62 C61 C60 117.7(2) . . ? C62 C61 C65 120.5(3) . . ? C60 C61 C65 121.8(2) . . ? C61 C62 C63 121.9(2) . . ? C61 C62 H62 119.1 . . ? C63 C62 H62 119.1 . . ? C58 C63 C62 119.3(2) . . ? C58 C63 C66 119.9(2) . . ? C62 C63 C66 120.8(2) . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C61 C65 H65A 109.5 . . ? C61 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C61 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C81 93.8(8) . . ? C83 C82 H82A 113.0 . . ? C81 C82 H82A 113.0 . . ? C83 C82 H82B 113.0 . . ? C81 C82 H82B 113.0 . . ? H82A C82 H82B 110.4 . . ? C84 C83 C82 103.6(8) . . ? C84 C83 H83A 111.0 . . ? C82 C83 H83A 111.0 . . ? C84 C83 H83B 111.0 . . ? C82 C83 H83B 111.0 . . ? H83A C83 H83B 109.0 . . ? C85 C84 C83 111.4(9) . . ? C85 C84 H84A 109.3 . . ? C83 C84 H84A 109.3 . . ? C85 C84 H84B 109.3 . . ? C83 C84 H84B 109.3 . . ? H84A C84 H84B 108.0 . . ? C84 C85 C86 106.8(11) . . ? C84 C85 H85A 110.4 . . ? C86 C85 H85A 110.4 . . ? C84 C85 H85B 110.4 . . ? C86 C85 H85B 110.4 . . ? H85A C85 H85B 108.6 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C82A C81A H81D 109.5 . . ? C82A C81A H81E 109.5 . . ? H81D C81A H81E 109.5 . . ? C82A C81A H81F 109.5 . . ? H81D C81A H81F 109.5 . . ? H81E C81A H81F 109.5 . . ? C83A C82A C81A 111.1(11) . . ? C83A C82A H82C 109.4 . . ? C81A C82A H82C 109.4 . . ? C83A C82A H82D 109.4 . . ? C81A C82A H82D 109.4 . . ? H82C C82A H82D 108.0 . . ? C84A C83A C82A 124.9(11) . . ? C84A C83A H83C 106.1 . . ? C82A C83A H83C 106.1 . . ? C84A C83A H83D 106.1 . . ? C82A C83A H83D 106.1 . . ? H83C C83A H83D 106.3 . . ? C83A C84A C85A 114.9(12) . . ? C83A C84A H84C 108.6 . . ? C85A C84A H84C 108.6 . . ? C83A C84A H84D 108.6 . . ? C85A C84A H84D 108.6 . . ? H84C C84A H84D 107.5 . . ? C84A C85A C86A 115.9(13) . . ? C84A C85A H85C 108.3 . . ? C86A C85A H85C 108.3 . . ? C84A C85A H85D 108.3 . . ? C86A C85A H85D 108.3 . . ? H85C C85A H85D 107.4 . . ? C85A C86A H86D 109.5 . . ? C85A C86A H86E 109.5 . . ? H86D C86A H86E 109.5 . . ? C85A C86A H86F 109.5 . . ? H86D C86A H86F 109.5 . . ? H86E C86A H86F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.526 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.062 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.004 0.000 0.461 2010.1 29.4 2 -0.092 0.500 0.051 2010.1 29.4 _platon_squeeze_details ; ;