# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email adam.fiedler@marquette.edu _publ_contact_author_phone ? _publ_contact_author_name 'Adam T. Fiedler' loop_ _publ_author_name 'Amanda E. Baum' 'Heaweon Park' 'Denan Wang' 'Sergey V. Lindeman' 'Adam T. Fiedler' data_Complex1A _database_code_depnum_ccdc_archive 'CCDC 890618' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C59 H45 B Fe N8 O2, C H2 Cl2' _chemical_formula_sum 'C60 H47 B Cl2 Fe N8 O2' _chemical_formula_weight 1049.62 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C59 H45 N7 O2 B C H2 Cl2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 14.5859(5) _cell_length_b 13.6416(4) _cell_length_c 25.2090(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.779(3) _cell_angle_gamma 90.00 _cell_volume 5005.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12152 _cell_measurement_temperature 99.9(3) _cell_measurement_theta_max 73.7370 _cell_measurement_theta_min 3.4038 _exptl_absorpt_coefficient_mu 3.831 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2176 _exptl_crystal_size_max 0.2728 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.0724 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 35336 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.90 _diffrn_reflns_theta_min 3.51 _diffrn_ambient_temperature 99.9(3) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -115.00 -61.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -148.0000 171.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega -42.00 20.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 30.0000 62 #__ type_ start__ end____ width___ exp.time_ 3 omega -49.00 32.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 150.0000 81 #__ type_ start__ end____ width___ exp.time_ 4 omega 48.00 92.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 40.6487 -125.0000 30.0000 44 #__ type_ start__ end____ width___ exp.time_ 5 omega -135.00 -110.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -61.5000 -125.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 6 omega 26.00 85.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 90.0000 59 #__ type_ start__ end____ width___ exp.time_ 7 omega 95.00 142.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 30.0000 47 #__ type_ start__ end____ width___ exp.time_ 8 omega 24.00 65.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -30.0000 41 #__ type_ start__ end____ width___ exp.time_ 9 omega 48.00 109.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -90.0000 61 #__ type_ start__ end____ width___ exp.time_ 10 omega 78.00 178.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 -150.0000 100 #__ type_ start__ end____ width___ exp.time_ 11 omega 65.00 91.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 12 omega 38.00 105.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 0.0000 67 #__ type_ start__ end____ width___ exp.time_ 13 omega 53.00 82.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 14 omega 42.00 83.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 60.0000 41 #__ type_ start__ end____ width___ exp.time_ 15 omega -119.00 -7.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -77.0000 30.0000 112 #__ type_ start__ end____ width___ exp.time_ 16 omega -117.00 -14.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -37.0000 60.0000 103 #__ type_ start__ end____ width___ exp.time_ 17 omega -115.00 -11.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -90.0000 104 #__ type_ start__ end____ width___ exp.time_ 18 omega -115.00 -11.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -180.0000 104 #__ type_ start__ end____ width___ exp.time_ 19 omega 79.00 157.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 45.0000 120.0000 78 #__ type_ start__ end____ width___ exp.time_ 20 omega 29.00 91.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 120.0000 62 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0295224000 _diffrn_orient_matrix_UB_12 -0.1082047000 _diffrn_orient_matrix_UB_13 -0.0053121000 _diffrn_orient_matrix_UB_21 -0.1014620000 _diffrn_orient_matrix_UB_22 0.0308655000 _diffrn_orient_matrix_UB_23 0.0009925000 _diffrn_orient_matrix_UB_31 -0.0061389000 _diffrn_orient_matrix_UB_32 0.0099702000 _diffrn_orient_matrix_UB_33 -0.0609929000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 8415 _reflns_number_total 9913 _reflns_odcompleteness_completeness 99.96 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.320 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.050 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 672 _refine_ls_number_reflns 9913 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0354 _refine_ls_restrained_S_all 1.041 _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^)+(0.0481P)^2^+1.7199P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.0954 _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 0.155131(19) 0.746132(19) 0.333275(11) 0.01550(7) Uani 1 1 d . . . O1 O 0.07198(8) 0.81580(8) 0.28189(5) 0.0182(3) Uani 1 1 d . . . O2 O 0.08260(9) 1.21945(9) 0.25684(5) 0.0216(3) Uani 1 1 d . . . H2 H 0.031(2) 1.2472(19) 0.2438(12) 0.049(8) Uiso 1 1 d . . . N1 N 0.21363(10) 0.62234(10) 0.29735(6) 0.0166(3) Uani 1 1 d . . . N2 N 0.22603(10) 0.54450(10) 0.33144(6) 0.0165(3) Uani 1 1 d . . . N3 N 0.21485(10) 0.71735(10) 0.41190(6) 0.0172(3) Uani 1 1 d . . . N4 N 0.22452(10) 0.61927(10) 0.42385(6) 0.0175(3) Uani 1 1 d . . . N5 N 0.04894(10) 0.65887(10) 0.36479(6) 0.0168(3) Uani 1 1 d . . . N6 N 0.07555(10) 0.56449(10) 0.37695(6) 0.0172(3) Uani 1 1 d . . . N7 N 0.26520(10) 0.83674(10) 0.30991(6) 0.0172(3) Uani 1 1 d . . . N8 N 0.32560(10) 0.93921(11) 0.25261(6) 0.0198(3) Uani 1 1 d . . . C1 C 0.27063(12) 0.60950(13) 0.47234(7) 0.0198(4) Uani 1 1 d . . . C2 C 0.29061(13) 0.70249(14) 0.49137(8) 0.0235(4) Uani 1 1 d . . . H2A H 0.3237 0.7187 0.5239 0.028 Uiso 1 1 calc R . . C3 C 0.25270(12) 0.76788(13) 0.45354(7) 0.0193(4) Uani 1 1 d . . . C4 C 0.00260(12) 0.51268(13) 0.39246(7) 0.0179(3) Uani 1 1 d . . . C5 C -0.07276(12) 0.57460(13) 0.39005(7) 0.0198(4) Uani 1 1 d . . . H5 H -0.1338 0.5586 0.3980 0.024 Uiso 1 1 calc R . . C6 C -0.04059(12) 0.66565(13) 0.37354(7) 0.0183(3) Uani 1 1 d . . . C7 C 0.28250(12) 0.47724(13) 0.31101(7) 0.0185(3) Uani 1 1 d . . . C8 C 0.30585(12) 0.51128(13) 0.26216(7) 0.0200(4) Uani 1 1 d . . . H8 H 0.3438 0.4794 0.2382 0.024 Uiso 1 1 calc R . . C9 C 0.26239(12) 0.60218(13) 0.25500(7) 0.0176(3) Uani 1 1 d . . . C10 C 0.29351(13) 0.51544(13) 0.49947(7) 0.0201(4) Uani 1 1 d . . . C11 C 0.38120(14) 0.50460(15) 0.52467(8) 0.0260(4) Uani 1 1 d . . . H11 H 0.4251 0.5556 0.5224 0.031 Uiso 1 1 calc R . . C12 C 0.40489(15) 0.41968(16) 0.55311(8) 0.0306(4) Uani 1 1 d . . . H12 H 0.4647 0.4130 0.5700 0.037 Uiso 1 1 calc R . . C13 C 0.34129(15) 0.34496(15) 0.55676(8) 0.0292(4) Uani 1 1 d . . . H13 H 0.3573 0.2870 0.5761 0.035 Uiso 1 1 calc R . . C14 C 0.25405(14) 0.35517(14) 0.53195(8) 0.0251(4) Uani 1 1 d . . . H14 H 0.2104 0.3039 0.5342 0.030 Uiso 1 1 calc R . . C15 C 0.22998(13) 0.43991(13) 0.50374(7) 0.0214(4) Uani 1 1 d . . . H15 H 0.1698 0.4464 0.4873 0.026 Uiso 1 1 calc R . . C16 C 0.24465(13) 0.87555(13) 0.45809(7) 0.0210(4) Uani 1 1 d . . . C17 C 0.27933(14) 0.92307(15) 0.50428(8) 0.0264(4) Uani 1 1 d . . . H17 H 0.3088 0.8860 0.5324 0.032 Uiso 1 1 calc R . . C18 C 0.27106(15) 1.02411(15) 0.50949(9) 0.0301(4) Uani 1 1 d . . . H18 H 0.2950 1.0554 0.5411 0.036 Uiso 1 1 calc R . . C19 C 0.22835(15) 1.07948(15) 0.46908(9) 0.0332(5) Uani 1 1 d . . . H19 H 0.2235 1.1486 0.4727 0.040 Uiso 1 1 calc R . . C20 C 0.19269(15) 1.03311(15) 0.42326(9) 0.0304(4) Uani 1 1 d . . . H20 H 0.1629 1.0706 0.3954 0.036 Uiso 1 1 calc R . . C21 C 0.20035(13) 0.93213(14) 0.41800(8) 0.0244(4) Uani 1 1 d . . . H21 H 0.1750 0.9011 0.3866 0.029 Uiso 1 1 calc R . . C22 C 0.00635(12) 0.40904(13) 0.40910(7) 0.0191(4) Uani 1 1 d . . . C23 C -0.03020(13) 0.38200(14) 0.45689(8) 0.0229(4) Uani 1 1 d . . . H23 H -0.0545 0.4309 0.4789 0.027 Uiso 1 1 calc R . . C24 C -0.03130(14) 0.28445(15) 0.47252(8) 0.0288(4) Uani 1 1 d . . . H24 H -0.0554 0.2667 0.5053 0.035 Uiso 1 1 calc R . . C25 C 0.00310(15) 0.21290(14) 0.43996(9) 0.0320(5) Uani 1 1 d . . . H25 H 0.0027 0.1460 0.4505 0.038 Uiso 1 1 calc R . . C26 C 0.03796(15) 0.23917(14) 0.39205(9) 0.0302(5) Uani 1 1 d . . . H26 H 0.0602 0.1899 0.3696 0.036 Uiso 1 1 calc R . . C27 C 0.04060(13) 0.33671(14) 0.37675(8) 0.0237(4) Uani 1 1 d . . . H27 H 0.0657 0.3542 0.3442 0.028 Uiso 1 1 calc R . . C28 C -0.08985(13) 0.76021(13) 0.37001(7) 0.0195(4) Uani 1 1 d . . . C29 C -0.18220(13) 0.76444(14) 0.35192(8) 0.0244(4) Uani 1 1 d . . . H29 H -0.2134 0.7063 0.3405 0.029 Uiso 1 1 calc R . . C30 C -0.22880(14) 0.85347(15) 0.35053(8) 0.0299(4) Uani 1 1 d . . . H30 H -0.2918 0.8557 0.3384 0.036 Uiso 1 1 calc R . . C31 C -0.18405(15) 0.93873(15) 0.36674(8) 0.0302(4) Uani 1 1 d . . . H31 H -0.2158 0.9995 0.3651 0.036 Uiso 1 1 calc R . . C32 C -0.09272(15) 0.93508(14) 0.38531(8) 0.0289(4) Uani 1 1 d . . . H32 H -0.0618 0.9934 0.3967 0.035 Uiso 1 1 calc R . . C33 C -0.04616(13) 0.84615(14) 0.38729(8) 0.0237(4) Uani 1 1 d . . . H33 H 0.0163 0.8440 0.4006 0.028 Uiso 1 1 calc R . . C34 C 0.31571(12) 0.38942(13) 0.34091(7) 0.0186(3) Uani 1 1 d . . . C35 C 0.29025(14) 0.29558(14) 0.32432(8) 0.0275(4) Uani 1 1 d . . . H35 H 0.2497 0.2867 0.2936 0.033 Uiso 1 1 calc R . . C36 C 0.32443(17) 0.21470(15) 0.35287(9) 0.0360(5) Uani 1 1 d . . . H36 H 0.3077 0.1505 0.3412 0.043 Uiso 1 1 calc R . . C37 C 0.38206(15) 0.22658(15) 0.39780(8) 0.0282(4) Uani 1 1 d . . . H37 H 0.4045 0.1708 0.4172 0.034 Uiso 1 1 calc R . . C38 C 0.40724(13) 0.31939(14) 0.41476(8) 0.0250(4) Uani 1 1 d . . . H38 H 0.4470 0.3278 0.4458 0.030 Uiso 1 1 calc R . . C39 C 0.37434(13) 0.40048(14) 0.38626(8) 0.0244(4) Uani 1 1 d . . . H39 H 0.3921 0.4644 0.3979 0.029 Uiso 1 1 calc R . . C40 C 0.26990(12) 0.67133(13) 0.21053(7) 0.0188(3) Uani 1 1 d . . . C41 C 0.35312(13) 0.67759(15) 0.18621(8) 0.0242(4) Uani 1 1 d . . . H41 H 0.4022 0.6348 0.1971 0.029 Uiso 1 1 calc R . . C42 C 0.36470(15) 0.74572(15) 0.14639(8) 0.0308(5) Uani 1 1 d . . . H42 H 0.4216 0.7497 0.1302 0.037 Uiso 1 1 calc R . . C43 C 0.29303(15) 0.80818(15) 0.13011(8) 0.0299(4) Uani 1 1 d . . . H43 H 0.3014 0.8559 0.1034 0.036 Uiso 1 1 calc R . . C44 C 0.20953(15) 0.80076(14) 0.15278(8) 0.0271(4) Uani 1 1 d . . . H44 H 0.1601 0.8424 0.1410 0.033 Uiso 1 1 calc R . . C45 C 0.19762(13) 0.73271(13) 0.19275(8) 0.0220(4) Uani 1 1 d . . . H45 H 0.1400 0.7279 0.2081 0.026 Uiso 1 1 calc R . . C46 C 0.07669(12) 0.91247(13) 0.27284(7) 0.0166(3) Uani 1 1 d . . . C47 C -0.00491(12) 0.96656(13) 0.26412(7) 0.0185(3) Uani 1 1 d . . . H47 H -0.0620 0.9329 0.2624 0.022 Uiso 1 1 calc R . . C48 C -0.00462(12) 1.06729(13) 0.25795(7) 0.0198(4) Uani 1 1 d . . . H48 H -0.0612 1.1015 0.2526 0.024 Uiso 1 1 calc R . . C49 C 0.07807(12) 1.11928(12) 0.25947(7) 0.0180(3) Uani 1 1 d . . . C50 C 0.15923(12) 1.06744(13) 0.26553(7) 0.0183(3) Uani 1 1 d . . . H50 H 0.2158 1.1019 0.2656 0.022 Uiso 1 1 calc R . . C51 C 0.16048(12) 0.96471(13) 0.27157(7) 0.0176(3) Uani 1 1 d . . . C52 C 0.24883(12) 0.91361(12) 0.27810(7) 0.0171(3) Uani 1 1 d . . . C53 C 0.39496(12) 0.87406(13) 0.26952(7) 0.0204(4) Uani 1 1 d . . . C54 C 0.35617(12) 0.81093(13) 0.30545(7) 0.0184(3) Uani 1 1 d . . . C55 C 0.40832(13) 0.73548(13) 0.32979(8) 0.0224(4) Uani 1 1 d . . . H55 H 0.3833 0.6929 0.3549 0.027 Uiso 1 1 calc R . . C56 C 0.49796(13) 0.72556(15) 0.31569(8) 0.0266(4) Uani 1 1 d . . . H56 H 0.5354 0.6754 0.3318 0.032 Uiso 1 1 calc R . . C57 C 0.53508(13) 0.78741(15) 0.27829(9) 0.0286(4) Uani 1 1 d . . . H57 H 0.5964 0.7770 0.2690 0.034 Uiso 1 1 calc R . . C58 C 0.48465(13) 0.86336(14) 0.25446(8) 0.0263(4) Uani 1 1 d . . . H58 H 0.5098 0.9058 0.2293 0.032 Uiso 1 1 calc R . . C59 C 0.33410(14) 1.00992(14) 0.20988(8) 0.0270(4) Uani 1 1 d . . . H59A H 0.2736 1.0214 0.1917 0.041 Uiso 1 1 calc R . . H59B H 0.3761 0.9842 0.1845 0.041 Uiso 1 1 calc R . . H59C H 0.3584 1.0718 0.2248 0.041 Uiso 1 1 calc R . . B1 B 0.17975(13) 0.54059(14) 0.38482(8) 0.0177(4) Uani 1 1 d . . . H1 H 0.1881 0.4739 0.4009 0.021 Uiso 1 1 calc R . . Cl2 Cl 0.50433(4) 0.85553(4) 0.46747(2) 0.04111(14) Uani 1 1 d . . . Cl3 Cl 0.53505(4) 1.00192(4) 0.38545(2) 0.03987(13) Uani 1 1 d . . . C60 C 0.45300(15) 0.94138(16) 0.42227(9) 0.0321(5) Uani 1 1 d . . . H60A H 0.4189 0.9906 0.4421 0.039 Uiso 1 1 calc R . . H60B H 0.4083 0.9072 0.3975 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01754(14) 0.01185(13) 0.01738(14) 0.00130(10) 0.00328(10) 0.00106(10) O1 0.0201(6) 0.0102(5) 0.0244(6) 0.0025(5) 0.0016(5) -0.0004(4) O2 0.0244(7) 0.0115(6) 0.0285(7) 0.0005(5) -0.0002(5) 0.0010(5) N1 0.0197(7) 0.0122(7) 0.0183(7) 0.0015(6) 0.0032(6) 0.0008(5) N2 0.0183(7) 0.0124(7) 0.0191(7) 0.0006(6) 0.0041(6) 0.0020(5) N3 0.0212(7) 0.0127(7) 0.0181(7) 0.0023(6) 0.0036(6) 0.0009(5) N4 0.0204(7) 0.0122(7) 0.0201(7) 0.0015(6) 0.0039(6) 0.0007(5) N5 0.0183(7) 0.0118(7) 0.0209(7) 0.0019(6) 0.0045(6) 0.0016(5) N6 0.0189(7) 0.0125(7) 0.0207(7) 0.0015(6) 0.0044(6) 0.0015(5) N7 0.0171(7) 0.0133(7) 0.0214(7) 0.0012(6) 0.0018(6) -0.0002(5) N8 0.0191(7) 0.0163(7) 0.0241(8) 0.0028(6) 0.0029(6) -0.0011(6) C1 0.0210(9) 0.0185(9) 0.0201(9) 0.0026(7) 0.0040(7) 0.0007(7) C2 0.0300(10) 0.0204(9) 0.0197(9) 0.0007(7) -0.0010(7) -0.0029(7) C3 0.0207(9) 0.0180(8) 0.0196(9) 0.0005(7) 0.0047(7) -0.0014(7) C4 0.0199(8) 0.0153(8) 0.0188(8) -0.0005(7) 0.0032(7) -0.0009(6) C5 0.0184(8) 0.0185(8) 0.0231(9) 0.0010(7) 0.0051(7) 0.0001(7) C6 0.0191(8) 0.0169(8) 0.0191(9) 0.0005(7) 0.0026(7) 0.0018(7) C7 0.0189(8) 0.0148(8) 0.0218(9) -0.0024(7) 0.0014(7) 0.0012(6) C8 0.0217(9) 0.0176(8) 0.0211(9) -0.0021(7) 0.0047(7) 0.0045(7) C9 0.0171(8) 0.0171(8) 0.0185(8) -0.0023(7) 0.0016(6) -0.0005(6) C10 0.0245(9) 0.0192(9) 0.0168(8) 0.0022(7) 0.0033(7) 0.0027(7) C11 0.0273(10) 0.0254(10) 0.0251(10) 0.0024(8) 0.0017(8) 0.0004(8) C12 0.0303(11) 0.0334(11) 0.0276(10) 0.0055(9) 0.0000(8) 0.0077(9) C13 0.0373(11) 0.0252(10) 0.0257(10) 0.0093(8) 0.0062(8) 0.0097(8) C14 0.0333(10) 0.0186(9) 0.0245(10) 0.0033(7) 0.0094(8) 0.0018(7) C15 0.0241(9) 0.0204(9) 0.0203(9) 0.0019(7) 0.0052(7) 0.0022(7) C16 0.0232(9) 0.0174(9) 0.0232(9) -0.0018(7) 0.0072(7) -0.0018(7) C17 0.0301(10) 0.0238(10) 0.0256(10) -0.0022(8) 0.0032(8) -0.0020(8) C18 0.0357(11) 0.0245(10) 0.0307(11) -0.0082(8) 0.0070(9) -0.0066(8) C19 0.0420(12) 0.0178(9) 0.0409(12) -0.0069(9) 0.0105(10) 0.0001(8) C20 0.0375(12) 0.0211(10) 0.0327(11) -0.0009(8) 0.0028(9) 0.0074(8) C21 0.0294(10) 0.0189(9) 0.0249(10) -0.0035(8) 0.0032(8) 0.0027(7) C22 0.0186(8) 0.0158(8) 0.0231(9) 0.0010(7) 0.0016(7) -0.0012(6) C23 0.0249(9) 0.0190(9) 0.0250(10) 0.0000(7) 0.0046(7) -0.0013(7) C24 0.0338(11) 0.0240(10) 0.0291(10) 0.0075(8) 0.0053(8) -0.0032(8) C25 0.0423(12) 0.0145(9) 0.0389(12) 0.0051(8) 0.0011(10) -0.0018(8) C26 0.0376(12) 0.0169(9) 0.0361(12) -0.0028(8) 0.0019(9) 0.0049(8) C27 0.0273(10) 0.0198(9) 0.0244(10) 0.0014(8) 0.0036(8) 0.0037(7) C28 0.0223(9) 0.0182(9) 0.0188(9) 0.0024(7) 0.0069(7) 0.0032(7) C29 0.0238(9) 0.0228(9) 0.0267(10) 0.0020(8) 0.0027(8) 0.0026(7) C30 0.0267(10) 0.0314(11) 0.0318(11) 0.0058(9) 0.0032(8) 0.0104(8) C31 0.0379(11) 0.0220(10) 0.0316(11) 0.0043(8) 0.0092(9) 0.0133(8) C32 0.0362(11) 0.0177(9) 0.0338(11) -0.0020(8) 0.0094(9) 0.0040(8) C33 0.0250(9) 0.0200(9) 0.0265(10) -0.0015(7) 0.0056(8) 0.0020(7) C34 0.0197(8) 0.0159(8) 0.0208(9) -0.0002(7) 0.0062(7) 0.0030(7) C35 0.0320(10) 0.0197(9) 0.0300(11) 0.0000(8) -0.0048(8) -0.0016(8) C36 0.0501(13) 0.0157(9) 0.0407(13) 0.0031(9) -0.0081(10) -0.0034(9) C37 0.0330(11) 0.0210(9) 0.0304(11) 0.0058(8) -0.0004(8) 0.0047(8) C38 0.0240(9) 0.0241(9) 0.0265(10) 0.0008(8) -0.0006(7) 0.0045(7) C39 0.0262(10) 0.0180(9) 0.0286(10) -0.0022(8) 0.0001(8) 0.0019(7) C40 0.0235(9) 0.0160(8) 0.0170(8) -0.0028(7) 0.0022(7) -0.0012(7) C41 0.0242(9) 0.0268(10) 0.0223(9) -0.0008(8) 0.0066(7) 0.0018(8) C42 0.0323(11) 0.0346(11) 0.0269(11) -0.0006(9) 0.0135(9) -0.0038(9) C43 0.0456(12) 0.0249(10) 0.0201(9) 0.0018(8) 0.0086(9) -0.0031(9) C44 0.0351(11) 0.0230(10) 0.0231(10) 0.0027(8) 0.0020(8) 0.0025(8) C45 0.0231(9) 0.0203(9) 0.0231(9) 0.0012(7) 0.0044(7) 0.0016(7) C46 0.0195(8) 0.0150(8) 0.0154(8) 0.0007(7) 0.0028(6) 0.0001(6) C47 0.0185(8) 0.0162(8) 0.0210(9) 0.0012(7) 0.0018(7) -0.0005(6) C48 0.0198(8) 0.0184(8) 0.0211(9) 0.0003(7) 0.0007(7) 0.0026(7) C49 0.0246(9) 0.0119(8) 0.0178(8) 0.0009(6) 0.0028(7) 0.0010(6) C50 0.0192(8) 0.0148(8) 0.0209(9) 0.0010(7) 0.0021(7) -0.0014(6) C51 0.0193(9) 0.0153(8) 0.0182(8) -0.0002(7) 0.0019(7) 0.0014(6) C52 0.0172(8) 0.0138(8) 0.0204(8) -0.0003(7) 0.0019(6) -0.0020(6) C53 0.0184(8) 0.0183(8) 0.0244(9) -0.0019(7) 0.0008(7) -0.0001(7) C54 0.0167(8) 0.0165(8) 0.0218(9) -0.0037(7) 0.0012(7) -0.0003(6) C55 0.0244(9) 0.0196(9) 0.0230(9) -0.0017(7) 0.0002(7) 0.0026(7) C56 0.0211(9) 0.0259(10) 0.0324(11) -0.0041(8) -0.0028(8) 0.0073(8) C57 0.0170(9) 0.0313(10) 0.0378(11) -0.0054(9) 0.0034(8) 0.0018(8) C58 0.0213(9) 0.0264(10) 0.0315(11) -0.0009(8) 0.0051(8) -0.0023(7) C59 0.0293(10) 0.0212(9) 0.0318(11) 0.0080(8) 0.0103(8) -0.0007(8) B1 0.0186(9) 0.0143(9) 0.0206(10) 0.0015(8) 0.0034(7) 0.0009(7) Cl2 0.0371(3) 0.0341(3) 0.0523(3) 0.0126(2) 0.0043(2) 0.0042(2) Cl3 0.0408(3) 0.0416(3) 0.0384(3) 0.0055(2) 0.0117(2) 0.0010(2) C60 0.0321(11) 0.0278(10) 0.0364(12) 0.0004(9) 0.0021(9) -0.0005(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9609(12) . ? Fe1 N1 2.1218(14) . ? Fe1 N3 2.1481(15) . ? Fe1 N5 2.1470(15) . ? Fe1 N7 2.1393(15) . ? O1 C46 1.341(2) . ? O2 H2 0.89(3) . ? O2 C49 1.370(2) . ? N1 C9 1.349(2) . ? N2 N1 1.371(2) . ? N2 C7 1.357(2) . ? N2 B1 1.546(2) . ? N3 C3 1.344(2) . ? N4 N3 1.377(2) . ? N4 C1 1.362(2) . ? N4 B1 1.569(2) . ? N5 C6 1.342(2) . ? N6 N5 1.3735(19) . ? N6 C4 1.356(2) . ? N6 B1 1.554(2) . ? N7 C52 1.332(2) . ? N7 C54 1.384(2) . ? N8 C52 1.372(2) . ? N8 C53 1.392(2) . ? N8 C59 1.457(2) . ? C1 C2 1.381(3) . ? C1 C10 1.482(2) . ? C2 H2A 0.9500 . ? C2 C3 1.393(3) . ? C3 C16 1.479(2) . ? C4 C5 1.384(2) . ? C4 C22 1.475(2) . ? C5 H5 0.9500 . ? C5 C6 1.401(2) . ? C6 C28 1.476(2) . ? C7 C8 1.380(3) . ? C7 C34 1.480(2) . ? C8 H8 0.9500 . ? C8 C9 1.399(2) . ? C9 C40 1.475(2) . ? C10 C11 1.398(3) . ? C10 C15 1.395(3) . ? C11 H11 0.9500 . ? C11 C12 1.394(3) . ? C12 H12 0.9500 . ? C12 C13 1.385(3) . ? C13 H13 0.9500 . ? C13 C14 1.387(3) . ? C14 H14 0.9500 . ? C14 C15 1.390(3) . ? C15 H15 0.9500 . ? C16 C17 1.398(3) . ? C16 C21 1.396(3) . ? C17 H17 0.9500 . ? C17 C18 1.390(3) . ? C18 H18 0.9500 . ? C18 C19 1.383(3) . ? C19 H19 0.9500 . ? C19 C20 1.388(3) . ? C20 H20 0.9500 . ? C20 C21 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.399(3) . ? C22 C27 1.394(3) . ? C23 H23 0.9500 . ? C23 C24 1.388(3) . ? C24 H24 0.9500 . ? C24 C25 1.390(3) . ? C25 H25 0.9500 . ? C25 C26 1.388(3) . ? C26 H26 0.9500 . ? C26 C27 1.387(3) . ? C27 H27 0.9500 . ? C28 C29 1.395(3) . ? C28 C33 1.391(3) . ? C29 H29 0.9500 . ? C29 C30 1.391(3) . ? C30 H30 0.9500 . ? C30 C31 1.382(3) . ? C31 H31 0.9500 . ? C31 C32 1.383(3) . ? C32 H32 0.9500 . ? C32 C33 1.390(3) . ? C33 H33 0.9500 . ? C34 C35 1.390(3) . ? C34 C39 1.390(3) . ? C35 H35 0.9500 . ? C35 C36 1.391(3) . ? C36 H36 0.9500 . ? C36 C37 1.375(3) . ? C37 H37 0.9500 . ? C37 C38 1.378(3) . ? C38 H38 0.9500 . ? C38 C39 1.387(3) . ? C39 H39 0.9500 . ? C40 C41 1.398(3) . ? C40 C45 1.397(3) . ? C41 H41 0.9500 . ? C41 C42 1.386(3) . ? C42 H42 0.9500 . ? C42 C43 1.390(3) . ? C43 H43 0.9500 . ? C43 C44 1.383(3) . ? C44 H44 0.9500 . ? C44 C45 1.389(3) . ? C45 H45 0.9500 . ? C46 C47 1.405(2) . ? C46 C51 1.417(2) . ? C47 H47 0.9500 . ? C47 C48 1.383(2) . ? C48 H48 0.9500 . ? C48 C49 1.397(2) . ? C49 C50 1.379(2) . ? C50 H50 0.9500 . ? C50 C51 1.410(2) . ? C51 C52 1.465(2) . ? C53 C54 1.396(3) . ? C53 C58 1.394(3) . ? C54 C55 1.397(3) . ? C55 H55 0.9500 . ? C55 C56 1.384(3) . ? C56 H56 0.9500 . ? C56 C57 1.400(3) . ? C57 H57 0.9500 . ? C57 C58 1.385(3) . ? C58 H58 0.9500 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? B1 H1 1.0000 . ? Cl2 C60 1.766(2) . ? Cl3 C60 1.767(2) . ? C60 H60A 0.9900 . ? C60 H60B 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 O1 Fe1 N1 110.64(5) . . ? O1 Fe1 N3 153.34(5) . . ? O1 Fe1 N5 94.78(5) . . ? O1 Fe1 N7 88.90(5) . . ? N1 Fe1 N3 95.65(6) . . ? N1 Fe1 N5 92.11(5) . . ? N1 Fe1 N7 90.69(6) . . ? N5 Fe1 N3 79.38(6) . . ? N7 Fe1 N3 95.37(6) . . ? N7 Fe1 N5 174.27(6) . . ? C46 O1 Fe1 123.55(11) . . ? C49 O2 H2 113.5(18) . . ? N2 N1 Fe1 112.90(10) . . ? C9 N1 Fe1 138.38(12) . . ? C9 N1 N2 106.47(14) . . ? N1 N2 B1 121.70(14) . . ? C7 N2 N1 110.14(14) . . ? C7 N2 B1 128.16(15) . . ? N4 N3 Fe1 114.14(11) . . ? C3 N3 Fe1 138.40(12) . . ? C3 N3 N4 107.26(14) . . ? N3 N4 B1 119.68(14) . . ? C1 N4 N3 109.19(14) . . ? C1 N4 B1 131.01(15) . . ? N6 N5 Fe1 113.71(10) . . ? C6 N5 Fe1 139.13(12) . . ? C6 N5 N6 106.97(14) . . ? N5 N6 B1 118.99(14) . . ? C4 N6 N5 109.70(14) . . ? C4 N6 B1 129.28(15) . . ? C52 N7 Fe1 120.83(12) . . ? C52 N7 C54 106.62(15) . . ? C54 N7 Fe1 128.03(11) . . ? C52 N8 C53 107.04(14) . . ? C52 N8 C59 128.77(15) . . ? C53 N8 C59 123.61(15) . . ? N4 C1 C2 107.61(16) . . ? N4 C1 C10 125.57(16) . . ? C2 C1 C10 126.82(17) . . ? C1 C2 H2A 126.7 . . ? C1 C2 C3 106.56(16) . . ? C3 C2 H2A 126.7 . . ? N3 C3 C2 109.29(16) . . ? N3 C3 C16 122.66(16) . . ? C2 C3 C16 127.79(17) . . ? N6 C4 C5 107.77(15) . . ? N6 C4 C22 124.50(16) . . ? C5 C4 C22 127.73(16) . . ? C4 C5 H5 127.1 . . ? C4 C5 C6 105.87(16) . . ? C6 C5 H5 127.1 . . ? N5 C6 C5 109.66(15) . . ? N5 C6 C28 121.70(16) . . ? C5 C6 C28 128.42(16) . . ? N2 C7 C8 107.62(15) . . ? N2 C7 C34 122.74(16) . . ? C8 C7 C34 129.44(16) . . ? C7 C8 H8 127.0 . . ? C7 C8 C9 106.09(15) . . ? C9 C8 H8 127.0 . . ? N1 C9 C8 109.66(15) . . ? N1 C9 C40 122.71(16) . . ? C8 C9 C40 127.54(16) . . ? C11 C10 C1 118.22(17) . . ? C15 C10 C1 123.02(17) . . ? C15 C10 C11 118.64(17) . . ? C10 C11 H11 119.7 . . ? C12 C11 C10 120.67(19) . . ? C12 C11 H11 119.7 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.08(19) . . ? C13 C12 H12 120.0 . . ? C12 C13 H13 120.2 . . ? C12 C13 C14 119.63(18) . . ? C14 C13 H13 120.2 . . ? C13 C14 H14 119.8 . . ? C13 C14 C15 120.48(19) . . ? C15 C14 H14 119.8 . . ? C10 C15 H15 119.8 . . ? C14 C15 C10 120.48(18) . . ? C14 C15 H15 119.8 . . ? C17 C16 C3 119.94(17) . . ? C21 C16 C3 121.89(17) . . ? C21 C16 C17 118.14(17) . . ? C16 C17 H17 119.7 . . ? C18 C17 C16 120.62(19) . . ? C18 C17 H17 119.7 . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.63(19) . . ? C19 C18 H18 119.7 . . ? C18 C19 H19 120.3 . . ? C18 C19 C20 119.35(19) . . ? C20 C19 H19 120.3 . . ? C19 C20 H20 119.9 . . ? C19 C20 C21 120.2(2) . . ? C21 C20 H20 119.9 . . ? C16 C21 H21 119.5 . . ? C20 C21 C16 121.03(19) . . ? C20 C21 H21 119.5 . . ? C23 C22 C4 119.25(16) . . ? C27 C22 C4 121.36(17) . . ? C27 C22 C23 119.28(17) . . ? C22 C23 H23 119.7 . . ? C24 C23 C22 120.62(18) . . ? C24 C23 H23 119.7 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.62(19) . . ? C25 C24 H24 120.2 . . ? C24 C25 H25 120.0 . . ? C26 C25 C24 119.97(18) . . ? C26 C25 H25 120.0 . . ? C25 C26 H26 119.7 . . ? C27 C26 C25 120.56(19) . . ? C27 C26 H26 119.7 . . ? C22 C27 H27 120.0 . . ? C26 C27 C22 119.94(18) . . ? C26 C27 H27 120.0 . . ? C29 C28 C6 120.77(17) . . ? C33 C28 C6 120.43(17) . . ? C33 C28 C29 118.71(17) . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.28(19) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.45(19) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 120.2 . . ? C30 C31 C32 119.68(18) . . ? C32 C31 H31 120.2 . . ? C31 C32 H32 120.0 . . ? C31 C32 C33 120.07(19) . . ? C33 C32 H32 120.0 . . ? C28 C33 H33 119.6 . . ? C32 C33 C28 120.79(18) . . ? C32 C33 H33 119.6 . . ? C35 C34 C7 121.37(17) . . ? C35 C34 C39 119.02(17) . . ? C39 C34 C7 119.60(16) . . ? C34 C35 H35 120.2 . . ? C34 C35 C36 119.69(19) . . ? C36 C35 H35 120.2 . . ? C35 C36 H36 119.6 . . ? C37 C36 C35 120.8(2) . . ? C37 C36 H36 119.6 . . ? C36 C37 H37 120.0 . . ? C36 C37 C38 119.98(19) . . ? C38 C37 H37 120.0 . . ? C37 C38 H38 120.1 . . ? C37 C38 C39 119.72(18) . . ? C39 C38 H38 120.1 . . ? C34 C39 H39 119.6 . . ? C38 C39 C34 120.82(18) . . ? C38 C39 H39 119.6 . . ? C41 C40 C9 118.86(16) . . ? C45 C40 C9 122.34(16) . . ? C45 C40 C41 118.78(17) . . ? C40 C41 H41 119.7 . . ? C42 C41 C40 120.61(18) . . ? C42 C41 H41 119.7 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 119.98(19) . . ? C43 C42 H42 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 C42 119.94(19) . . ? C44 C43 H43 120.0 . . ? C43 C44 H44 119.9 . . ? C43 C44 C45 120.28(19) . . ? C45 C44 H44 119.9 . . ? C40 C45 H45 119.8 . . ? C44 C45 C40 120.36(18) . . ? C44 C45 H45 119.8 . . ? O1 C46 C47 119.38(15) . . ? O1 C46 C51 123.54(15) . . ? C47 C46 C51 117.08(16) . . ? C46 C47 H47 119.0 . . ? C48 C47 C46 122.04(17) . . ? C48 C47 H47 119.0 . . ? C47 C48 H48 119.7 . . ? C47 C48 C49 120.68(16) . . ? C49 C48 H48 119.7 . . ? O2 C49 C48 123.31(16) . . ? O2 C49 C50 118.24(16) . . ? C50 C49 C48 118.42(16) . . ? C49 C50 H50 119.1 . . ? C49 C50 C51 121.79(16) . . ? C51 C50 H50 119.1 . . ? C46 C51 C52 120.79(15) . . ? C50 C51 C46 119.83(16) . . ? C50 C51 C52 119.35(16) . . ? N7 C52 N8 111.27(15) . . ? N7 C52 C51 124.32(16) . . ? N8 C52 C51 124.41(16) . . ? N8 C53 C54 105.97(15) . . ? N8 C53 C58 131.27(18) . . ? C58 C53 C54 122.68(17) . . ? N7 C54 C53 109.11(15) . . ? N7 C54 C55 130.42(17) . . ? C53 C54 C55 120.46(17) . . ? C54 C55 H55 121.5 . . ? C56 C55 C54 117.08(18) . . ? C56 C55 H55 121.5 . . ? C55 C56 H56 119.1 . . ? C55 C56 C57 121.85(18) . . ? C57 C56 H56 119.1 . . ? C56 C57 H57 119.2 . . ? C58 C57 C56 121.67(18) . . ? C58 C57 H57 119.2 . . ? C53 C58 H58 121.9 . . ? C57 C58 C53 116.19(18) . . ? C57 C58 H58 121.9 . . ? N8 C59 H59A 109.5 . . ? N8 C59 H59B 109.5 . . ? N8 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N2 B1 N4 109.57(14) . . ? N2 B1 N6 111.16(15) . . ? N2 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? N6 B1 N4 107.43(14) . . ? N6 B1 H1 109.5 . . ? Cl2 C60 Cl3 112.07(12) . . ? Cl2 C60 H60A 109.2 . . ? Cl2 C60 H60B 109.2 . . ? Cl3 C60 H60A 109.2 . . ? Cl3 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.89(3) 1.85(3) 2.7339(18) 175(3) 2 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 -141.37(13) . . . . ? Fe1 O1 C46 C51 38.5(2) . . . . ? Fe1 N1 C9 C8 160.73(14) . . . . ? Fe1 N1 C9 C40 -16.2(3) . . . . ? Fe1 N3 C3 C2 -171.70(14) . . . . ? Fe1 N3 C3 C16 13.7(3) . . . . ? Fe1 N5 C6 C5 172.73(14) . . . . ? Fe1 N5 C6 C28 -12.3(3) . . . . ? Fe1 N7 C52 N8 -157.68(11) . . . . ? Fe1 N7 C52 C51 22.8(2) . . . . ? Fe1 N7 C54 C53 155.41(13) . . . . ? Fe1 N7 C54 C55 -23.7(3) . . . . ? O1 Fe1 N1 N2 -144.62(10) . . . . ? O1 Fe1 N1 C9 55.51(19) . . . . ? O1 Fe1 N3 N4 137.12(12) . . . . ? O1 Fe1 N3 C3 -48.7(2) . . . . ? O1 Fe1 N5 N6 142.28(11) . . . . ? O1 Fe1 N5 C6 -31.80(19) . . . . ? O1 Fe1 N7 C52 9.01(14) . . . . ? O1 Fe1 N7 C54 -143.83(15) . . . . ? O1 C46 C47 C48 175.80(16) . . . . ? O1 C46 C51 C50 -175.51(16) . . . . ? O1 C46 C51 C52 2.6(3) . . . . ? O2 C49 C50 C51 176.39(16) . . . . ? N1 Fe1 O1 C46 -128.81(13) . . . . ? N1 Fe1 N3 N4 -33.34(12) . . . . ? N1 Fe1 N3 C3 140.83(18) . . . . ? N1 Fe1 N5 N6 31.36(12) . . . . ? N1 Fe1 N5 C6 -142.71(19) . . . . ? N1 Fe1 N7 C52 119.64(14) . . . . ? N1 Fe1 N7 C54 -33.20(15) . . . . ? N1 N2 C7 C8 -1.2(2) . . . . ? N1 N2 C7 C34 174.17(15) . . . . ? N1 N2 B1 N4 -69.52(19) . . . . ? N1 N2 B1 N6 49.1(2) . . . . ? N1 C9 C40 C41 143.41(18) . . . . ? N1 C9 C40 C45 -34.8(3) . . . . ? N2 N1 C9 C8 0.04(19) . . . . ? N2 N1 C9 C40 -176.94(15) . . . . ? N2 C7 C8 C9 1.1(2) . . . . ? N2 C7 C34 C35 114.6(2) . . . . ? N2 C7 C34 C39 -66.1(2) . . . . ? N3 Fe1 O1 C46 61.34(19) . . . . ? N3 Fe1 N1 N2 30.82(12) . . . . ? N3 Fe1 N1 C9 -129.04(18) . . . . ? N3 Fe1 N5 N6 -63.99(11) . . . . ? N3 Fe1 N5 C6 121.94(19) . . . . ? N3 Fe1 N7 C52 -144.63(13) . . . . ? N3 Fe1 N7 C54 62.54(15) . . . . ? N3 N4 C1 C2 -0.1(2) . . . . ? N3 N4 C1 C10 179.16(16) . . . . ? N3 N4 B1 N2 65.03(19) . . . . ? N3 N4 B1 N6 -55.85(19) . . . . ? N3 C3 C16 C17 174.99(17) . . . . ? N3 C3 C16 C21 -2.9(3) . . . . ? N4 N3 C3 C2 2.7(2) . . . . ? N4 N3 C3 C16 -171.86(16) . . . . ? N4 C1 C2 C3 1.7(2) . . . . ? N4 C1 C10 C11 137.19(19) . . . . ? N4 C1 C10 C15 -46.8(3) . . . . ? N5 Fe1 O1 C46 137.12(13) . . . . ? N5 Fe1 N1 N2 -48.71(11) . . . . ? N5 Fe1 N1 C9 151.42(18) . . . . ? N5 Fe1 N3 N4 57.76(11) . . . . ? N5 Fe1 N3 C3 -128.07(19) . . . . ? N5 Fe1 N7 C52 -121.0(5) . . . . ? N5 Fe1 N7 C54 86.1(6) . . . . ? N5 N6 C4 C5 0.3(2) . . . . ? N5 N6 C4 C22 -179.20(16) . . . . ? N5 N6 B1 N2 -70.79(19) . . . . ? N5 N6 B1 N4 49.1(2) . . . . ? N5 C6 C28 C29 146.54(18) . . . . ? N5 C6 C28 C33 -36.8(3) . . . . ? N6 N5 C6 C5 -1.6(2) . . . . ? N6 N5 C6 C28 173.38(16) . . . . ? N6 C4 C5 C6 -1.2(2) . . . . ? N6 C4 C22 C23 129.75(19) . . . . ? N6 C4 C22 C27 -54.1(3) . . . . ? N7 Fe1 O1 C46 -38.48(13) . . . . ? N7 Fe1 N1 N2 126.29(11) . . . . ? N7 Fe1 N1 C9 -33.58(18) . . . . ? N7 Fe1 N3 N4 -124.58(11) . . . . ? N7 Fe1 N3 C3 49.59(19) . . . . ? N7 Fe1 N5 N6 -87.9(6) . . . . ? N7 Fe1 N5 C6 98.0(6) . . . . ? N7 C54 C55 C56 177.53(18) . . . . ? N8 C53 C54 N7 0.4(2) . . . . ? N8 C53 C54 C55 179.62(16) . . . . ? N8 C53 C58 C57 -177.72(19) . . . . ? C1 N4 N3 Fe1 174.31(11) . . . . ? C1 N4 N3 C3 -1.64(19) . . . . ? C1 N4 B1 N2 -119.19(19) . . . . ? C1 N4 B1 N6 119.93(19) . . . . ? C1 C2 C3 N3 -2.8(2) . . . . ? C1 C2 C3 C16 171.44(18) . . . . ? C1 C10 C11 C12 176.68(18) . . . . ? C1 C10 C15 C14 -176.78(17) . . . . ? C2 C1 C10 C11 -43.7(3) . . . . ? C2 C1 C10 C15 132.3(2) . . . . ? C2 C3 C16 C17 1.5(3) . . . . ? C2 C3 C16 C21 -176.42(19) . . . . ? C3 C16 C17 C18 -179.03(18) . . . . ? C3 C16 C21 C20 179.34(18) . . . . ? C4 N6 N5 Fe1 -175.13(11) . . . . ? C4 N6 N5 C6 0.82(19) . . . . ? C4 N6 B1 N2 127.18(18) . . . . ? C4 N6 B1 N4 -112.95(19) . . . . ? C4 C5 C6 N5 1.8(2) . . . . ? C4 C5 C6 C28 -172.78(18) . . . . ? C4 C22 C23 C24 177.20(18) . . . . ? C4 C22 C27 C26 -176.01(18) . . . . ? C5 C4 C22 C23 -49.6(3) . . . . ? C5 C4 C22 C27 126.5(2) . . . . ? C5 C6 C28 C29 -39.5(3) . . . . ? C5 C6 C28 C33 137.1(2) . . . . ? C6 C28 C29 C30 177.73(18) . . . . ? C6 C28 C33 C32 -178.42(18) . . . . ? C7 N2 N1 Fe1 -165.52(11) . . . . ? C7 N2 N1 C9 0.69(19) . . . . ? C7 N2 B1 N4 110.18(19) . . . . ? C7 N2 B1 N6 -131.23(18) . . . . ? C7 C8 C9 N1 -0.7(2) . . . . ? C7 C8 C9 C40 176.06(17) . . . . ? C7 C34 C35 C36 178.7(2) . . . . ? C7 C34 C39 C38 -179.37(17) . . . . ? C8 C7 C34 C35 -71.2(3) . . . . ? C8 C7 C34 C39 108.1(2) . . . . ? C8 C9 C40 C41 -33.0(3) . . . . ? C8 C9 C40 C45 148.76(19) . . . . ? C9 C40 C41 C42 -176.18(18) . . . . ? C9 C40 C45 C44 176.22(17) . . . . ? C10 C1 C2 C3 -177.52(17) . . . . ? C10 C11 C12 C13 -0.1(3) . . . . ? C11 C10 C15 C14 -0.8(3) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C10 0.7(3) . . . . ? C15 C10 C11 C12 0.5(3) . . . . ? C16 C17 C18 C19 0.0(3) . . . . ? C17 C16 C21 C20 1.4(3) . . . . ? C17 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 C21 -0.4(3) . . . . ? C19 C20 C21 C16 -0.7(3) . . . . ? C21 C16 C17 C18 -1.1(3) . . . . ? C22 C4 C5 C6 178.24(17) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C22 C27 C26 0.2(3) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C27 1.3(3) . . . . ? C25 C26 C27 C22 -1.3(3) . . . . ? C27 C22 C23 C24 0.9(3) . . . . ? C28 C29 C30 C31 0.4(3) . . . . ? C29 C28 C33 C32 -1.7(3) . . . . ? C29 C30 C31 C32 -1.1(3) . . . . ? C30 C31 C32 C33 0.4(3) . . . . ? C31 C32 C33 C28 1.0(3) . . . . ? C33 C28 C29 C30 1.0(3) . . . . ? C34 C7 C8 C9 -173.78(18) . . . . ? C34 C35 C36 C37 1.0(4) . . . . ? C35 C34 C39 C38 0.0(3) . . . . ? C35 C36 C37 C38 -0.6(4) . . . . ? C36 C37 C38 C39 -0.1(3) . . . . ? C37 C38 C39 C34 0.4(3) . . . . ? C39 C34 C35 C36 -0.7(3) . . . . ? C40 C41 C42 C43 -0.4(3) . . . . ? C41 C40 C45 C44 -2.0(3) . . . . ? C41 C42 C43 C44 -1.5(3) . . . . ? C42 C43 C44 C45 1.6(3) . . . . ? C43 C44 C45 C40 0.2(3) . . . . ? C45 C40 C41 C42 2.1(3) . . . . ? C46 C47 C48 C49 0.9(3) . . . . ? C46 C51 C52 N7 -35.5(3) . . . . ? C46 C51 C52 N8 145.04(17) . . . . ? C47 C46 C51 C50 4.4(3) . . . . ? C47 C46 C51 C52 -177.51(16) . . . . ? C47 C48 C49 O2 -175.91(17) . . . . ? C47 C48 C49 C50 2.1(3) . . . . ? C48 C49 C50 C51 -1.7(3) . . . . ? C49 C50 C51 C46 -1.6(3) . . . . ? C49 C50 C51 C52 -179.71(16) . . . . ? C50 C51 C52 N7 142.59(18) . . . . ? C50 C51 C52 N8 -36.9(3) . . . . ? C51 C46 C47 C48 -4.1(3) . . . . ? C52 N7 C54 C53 -0.4(2) . . . . ? C52 N7 C54 C55 -179.52(19) . . . . ? C52 N8 C53 C54 -0.26(19) . . . . ? C52 N8 C53 C58 176.3(2) . . . . ? C53 N8 C52 N7 0.0(2) . . . . ? C53 N8 C52 C51 179.49(16) . . . . ? C53 C54 C55 C56 -1.5(3) . . . . ? C54 N7 C52 N8 0.3(2) . . . . ? C54 N7 C52 C51 -179.23(16) . . . . ? C54 C53 C58 C57 -1.7(3) . . . . ? C54 C55 C56 C57 -0.6(3) . . . . ? C55 C56 C57 C58 1.6(3) . . . . ? C56 C57 C58 C53 -0.5(3) . . . . ? C58 C53 C54 N7 -176.48(17) . . . . ? C58 C53 C54 C55 2.7(3) . . . . ? C59 N8 C52 N7 171.36(17) . . . . ? C59 N8 C52 C51 -9.1(3) . . . . ? C59 N8 C53 C54 -172.18(17) . . . . ? C59 N8 C53 C58 4.4(3) . . . . ? B1 N2 N1 Fe1 14.23(19) . . . . ? B1 N2 N1 C9 -179.56(15) . . . . ? B1 N2 C7 C8 179.12(16) . . . . ? B1 N2 C7 C34 -5.6(3) . . . . ? B1 N4 N3 Fe1 -9.06(18) . . . . ? B1 N4 N3 C3 174.99(15) . . . . ? B1 N4 C1 C2 -176.21(17) . . . . ? B1 N4 C1 C10 3.0(3) . . . . ? B1 N6 N5 Fe1 19.57(18) . . . . ? B1 N6 N5 C6 -164.48(15) . . . . ? B1 N6 C4 C5 163.62(17) . . . . ? B1 N6 C4 C22 -15.9(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3 8 -3 0.1045 2.9993 8.0004 -2.9985 -0.9383 -0.0604 0.2442 0 -8 -6 0.1214 0.0005 -8.0003 -6.0012 0.8975 -0.2529 0.2863 8 0 -11 0.0397 7.9999 0.0001 -10.9998 -0.1778 -0.8226 0.6218 9 0 1 0.0362 9.0002 -0.0001 0.9993 -0.2710 -0.9122 -0.1162 -9 0 -1 0.0362 -9.0002 0.0001 -0.9993 0.2710 0.9122 0.1162 0 0 16 0.0263 0.0004 -0.0002 15.9989 -0.0850 0.0158 -0.9758 0 0 -16 0.0462 -0.0004 0.0002 -15.9989 0.0850 -0.0158 0.9758 #===END data_Complex1B _database_code_depnum_ccdc_archive 'CCDC 890619' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C53 H41 B Fe N6 O3, 1.77(C H2 Cl2)' _chemical_formula_sum 'C54.77 H44.53 B Cl3.53 Fe N6 O3' _chemical_formula_weight 1026.60 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C55 H45 N6 O3 B Cl4' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-x, y+1/2, -z+1/2' _cell_length_a 11.2362(4) _cell_length_b 17.7643(6) _cell_length_c 25.2782(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5045.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7874 _cell_measurement_temperature 100.2 _cell_measurement_theta_max 73.6722 _cell_measurement_theta_min 3.4935 _exptl_absorpt_coefficient_mu 4.518 _exptl_absorpt_correction_T_max 0.716 _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2121 _exptl_crystal_size_max 0.313 _exptl_crystal_size_mid 0.2434 _exptl_crystal_size_min 0.1214 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0496 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 19096 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.88 _diffrn_reflns_theta_min 3.50 _diffrn_ambient_temperature 100.2 _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -31.00 -3.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 125.0000 -180.0000 28 #__ type_ start__ end____ width___ exp.time_ 2 omega -60.00 27.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 0.0000 87 #__ type_ start__ end____ width___ exp.time_ 3 omega 60.00 98.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 40.6487 -125.0000 150.0000 38 #__ type_ start__ end____ width___ exp.time_ 4 omega 95.00 161.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 -60.0000 66 #__ type_ start__ end____ width___ exp.time_ 5 omega 146.00 175.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 90.0000 29 #__ type_ start__ end____ width___ exp.time_ 6 omega 34.00 59.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -56.0000 122.0000 25 #__ type_ start__ end____ width___ exp.time_ 7 omega 94.00 133.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 90.0000 39 #__ type_ start__ end____ width___ exp.time_ 8 omega 50.00 76.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega 33.00 62.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -30.0000 29 #__ type_ start__ end____ width___ exp.time_ 10 omega 81.00 164.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 45.0000 -120.0000 83 #__ type_ start__ end____ width___ exp.time_ 11 omega -119.00 -79.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -77.0000 0.0000 40 #__ type_ start__ end____ width___ exp.time_ 12 omega -115.00 -10.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -64.0000 107.0000 105 #__ type_ start__ end____ width___ exp.time_ 13 omega -39.00 -7.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -77.0000 -120.0000 32 #__ type_ start__ end____ width___ exp.time_ 14 omega 73.00 131.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 77.0000 30.0000 58 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0206305000 _diffrn_orient_matrix_UB_12 -0.0644620000 _diffrn_orient_matrix_UB_13 -0.0398003000 _diffrn_orient_matrix_UB_21 0.1350085000 _diffrn_orient_matrix_UB_22 -0.0049568000 _diffrn_orient_matrix_UB_23 -0.0097692000 _diffrn_orient_matrix_UB_31 0.0112381000 _diffrn_orient_matrix_UB_32 -0.0578297000 _diffrn_orient_matrix_UB_33 0.0450737000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 8545 _reflns_number_total 8984 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.483 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.144 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(7) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 634 _refine_ls_number_reflns 8984 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0814 _refine_ls_restrained_S_all 1.103 _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^)+(0.1480P)^2^+12.3077P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2410 _refine_ls_wR_factor_ref 0.2437 _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 0.19390(8) 0.46937(5) 0.43777(3) 0.0216(2) Uani 1 1 d . . . O1 O 0.2228(3) 0.3847(2) 0.48431(16) 0.0247(8) Uani 1 1 d . . . O2 O -0.0440(4) 0.1376(2) 0.54242(18) 0.0296(9) Uani 1 1 d . . . H3 H -0.1013 0.1289 0.5219 0.044 Uiso 1 1 calc R . . O3 O 0.0606(4) 0.4040(2) 0.40395(15) 0.0247(8) Uani 1 1 d . . . N1 N 0.2576(4) 0.4894(3) 0.35961(18) 0.0233(10) Uani 1 1 d . . . N2 N 0.2692(4) 0.5635(3) 0.34658(19) 0.0229(10) Uani 1 1 d . . . N3 N 0.0973(4) 0.5698(3) 0.43580(19) 0.0235(9) Uani 1 1 d . . . N4 N 0.1507(4) 0.6322(3) 0.41582(19) 0.0235(10) Uani 1 1 d . . . N5 N 0.3297(4) 0.5450(3) 0.46947(19) 0.0225(9) Uani 1 1 d . . . N6 N 0.3646(4) 0.5987(3) 0.43393(19) 0.0231(9) Uani 1 1 d . . . C1 C 0.0752(5) 0.6915(3) 0.4174(2) 0.0257(12) Uani 1 1 d . . . C2 C -0.0329(5) 0.6654(3) 0.4390(3) 0.0289(12) Uani 1 1 d . . . H2 H -0.1035 0.6936 0.4447 0.035 Uiso 1 1 calc R . . C3 C -0.0145(5) 0.5897(3) 0.4501(2) 0.0279(12) Uani 1 1 d . . . C4 C 0.4725(5) 0.6284(3) 0.4491(2) 0.0243(11) Uani 1 1 d . . . C5 C 0.5037(5) 0.5944(3) 0.4967(2) 0.0248(11) Uani 1 1 d . . . H5 H 0.5728 0.6041 0.5172 0.030 Uiso 1 1 calc R . . C6 C 0.4130(5) 0.5431(3) 0.5082(2) 0.0252(11) Uani 1 1 d . . . C7 C 0.2739(5) 0.5714(4) 0.2935(2) 0.0273(12) Uani 1 1 d . . . C8 C 0.2653(6) 0.5011(4) 0.2714(2) 0.0309(13) Uani 1 1 d . . . H8 H 0.2659 0.4891 0.2348 0.037 Uiso 1 1 calc R . . C9 C 0.2552(5) 0.4502(4) 0.3142(2) 0.0262(12) Uani 1 1 d . . . C10 C 0.1052(6) 0.7683(3) 0.4018(2) 0.0280(12) Uani 1 1 d . . . C11 C 0.0232(6) 0.8114(4) 0.3738(3) 0.0334(13) Uani 1 1 d . . . H11 H -0.0523 0.7908 0.3651 0.040 Uiso 1 1 calc R . . C12 C 0.0503(7) 0.8831(4) 0.3587(3) 0.0391(16) Uani 1 1 d . . . H12 H -0.0069 0.9121 0.3400 0.047 Uiso 1 1 calc R . . C13 C 0.1611(7) 0.9144(4) 0.3704(3) 0.0403(16) Uani 1 1 d . . . H13 H 0.1808 0.9636 0.3586 0.048 Uiso 1 1 calc R . . C14 C 0.2417(6) 0.8725(4) 0.3994(3) 0.0370(15) Uani 1 1 d . . . H14 H 0.3159 0.8942 0.4090 0.044 Uiso 1 1 calc R . . C15 C 0.2165(6) 0.8009(4) 0.4143(3) 0.0304(13) Uani 1 1 d . . . H15 H 0.2741 0.7724 0.4333 0.037 Uiso 1 1 calc R . . C16 C -0.0920(5) 0.5313(3) 0.4737(3) 0.0285(12) Uani 1 1 d . . . C17 C -0.2080(6) 0.5201(4) 0.4554(3) 0.0354(14) Uani 1 1 d . . . H17 H -0.2417 0.5542 0.4306 0.042 Uiso 1 1 calc R . . C18 C -0.2740(6) 0.4593(4) 0.4733(3) 0.0396(15) Uani 1 1 d . . . H18 H -0.3521 0.4511 0.4601 0.047 Uiso 1 1 calc R . . C19 C -0.2259(6) 0.4097(4) 0.5109(3) 0.0361(15) Uani 1 1 d . . . H19 H -0.2710 0.3681 0.5233 0.043 Uiso 1 1 calc R . . C20 C -0.1107(6) 0.4224(4) 0.5300(3) 0.0345(14) Uani 1 1 d . . . H20 H -0.0774 0.3895 0.5556 0.041 Uiso 1 1 calc R . . C21 C -0.0463(6) 0.4821(4) 0.5117(2) 0.0299(13) Uani 1 1 d . . . H21 H 0.0316 0.4904 0.5252 0.036 Uiso 1 1 calc R . . C22 C 0.5375(5) 0.6856(3) 0.4198(2) 0.0262(12) Uani 1 1 d . . . C23 C 0.6015(6) 0.7412(4) 0.4466(3) 0.0341(14) Uani 1 1 d . . . H23 H 0.5998 0.7422 0.4842 0.041 Uiso 1 1 calc R . . C24 C 0.6666(7) 0.7946(4) 0.4200(3) 0.0453(17) Uani 1 1 d . . . H24 H 0.7092 0.8317 0.4393 0.054 Uiso 1 1 calc R . . C25 C 0.6707(7) 0.7948(5) 0.3651(3) 0.0481(19) Uani 1 1 d . . . H25 H 0.7146 0.8323 0.3468 0.058 Uiso 1 1 calc R . . C26 C 0.6096(7) 0.7391(5) 0.3370(3) 0.0483(19) Uani 1 1 d . . . H26 H 0.6124 0.7383 0.2995 0.058 Uiso 1 1 calc R . . C27 C 0.5449(6) 0.6851(4) 0.3641(2) 0.0333(14) Uani 1 1 d . . . H27 H 0.5047 0.6469 0.3448 0.040 Uiso 1 1 calc R . . C28 C 0.3970(5) 0.4952(3) 0.5550(2) 0.0242(11) Uani 1 1 d . . . C29 C 0.4926(6) 0.4541(3) 0.5751(2) 0.0279(12) Uani 1 1 d . . . H29 H 0.5676 0.4558 0.5577 0.033 Uiso 1 1 calc R . . C30 C 0.4783(7) 0.4104(4) 0.6206(3) 0.0354(14) Uani 1 1 d . . . H30 H 0.5438 0.3826 0.6343 0.042 Uiso 1 1 calc R . . C31 C 0.3683(7) 0.4073(4) 0.6462(2) 0.0348(14) Uani 1 1 d . . . H31 H 0.3582 0.3772 0.6769 0.042 Uiso 1 1 calc R . . C32 C 0.2746(7) 0.4484(4) 0.6263(2) 0.0348(14) Uani 1 1 d . . . H32 H 0.1995 0.4469 0.6436 0.042 Uiso 1 1 calc R . . C33 C 0.2889(6) 0.4923(3) 0.5811(2) 0.0300(13) Uani 1 1 d . . . H33 H 0.2235 0.5205 0.5679 0.036 Uiso 1 1 calc R . . C34 C 0.2849(6) 0.6458(4) 0.2672(2) 0.0283(13) Uani 1 1 d . . . C35 C 0.3793(7) 0.6590(4) 0.2331(3) 0.0367(14) Uani 1 1 d . . . H35 H 0.4382 0.6214 0.2279 0.044 Uiso 1 1 calc R . . C36 C 0.3878(7) 0.7273(5) 0.2068(3) 0.0424(17) Uani 1 1 d . . . H36 H 0.4525 0.7363 0.1835 0.051 Uiso 1 1 calc R . . C37 C 0.3033(9) 0.7817(4) 0.2143(3) 0.0461(18) Uani 1 1 d . . . H37 H 0.3098 0.8283 0.1961 0.055 Uiso 1 1 calc R . . C38 C 0.2086(9) 0.7696(4) 0.2481(3) 0.0453(18) Uani 1 1 d . . . H38 H 0.1502 0.8076 0.2531 0.054 Uiso 1 1 calc R . . C39 C 0.1994(8) 0.7005(4) 0.2751(3) 0.0392(16) Uani 1 1 d . . . H39 H 0.1348 0.6915 0.2985 0.047 Uiso 1 1 calc R . . C40 C 0.2428(6) 0.3690(4) 0.3119(2) 0.0295(13) Uani 1 1 d . . . C41 C 0.1772(7) 0.3345(4) 0.2712(3) 0.0374(15) Uani 1 1 d . . . H41 H 0.1405 0.3648 0.2448 0.045 Uiso 1 1 calc R . . C42 C 0.1653(7) 0.2575(4) 0.2689(3) 0.0408(16) Uani 1 1 d . . . H42 H 0.1206 0.2353 0.2411 0.049 Uiso 1 1 calc R . . C43 C 0.2180(7) 0.2122(4) 0.3067(3) 0.0426(17) Uani 1 1 d . . . H43 H 0.2097 0.1591 0.3049 0.051 Uiso 1 1 calc R . . C44 C 0.2831(8) 0.2450(4) 0.3474(3) 0.0432(17) Uani 1 1 d . . . H44 H 0.3192 0.2139 0.3734 0.052 Uiso 1 1 calc R . . C45 C 0.2960(7) 0.3224(4) 0.3505(3) 0.0365(14) Uani 1 1 d . . . H45 H 0.3407 0.3441 0.3785 0.044 Uiso 1 1 calc R . . C46 C 0.1541(5) 0.3281(3) 0.4963(2) 0.0219(11) Uani 1 1 d . . . C47 C 0.1714(5) 0.2901(3) 0.5448(2) 0.0253(11) Uani 1 1 d . . . H50 H 0.2314 0.3077 0.5682 0.030 Uiso 1 1 calc R . . C48 C 0.1044(5) 0.2283(3) 0.5595(2) 0.0261(11) Uani 1 1 d . . . H51 H 0.1186 0.2046 0.5926 0.031 Uiso 1 1 calc R . . C49 C 0.0154(5) 0.2006(3) 0.5257(2) 0.0233(11) Uani 1 1 d . . . C50 C -0.0072(5) 0.2375(3) 0.4798(2) 0.0235(11) Uani 1 1 d . . . H53 H -0.0695 0.2197 0.4577 0.028 Uiso 1 1 calc R . . C51 C 0.0580(5) 0.3013(3) 0.4636(2) 0.0206(10) Uani 1 1 d . . . C52 C 0.0212(5) 0.3420(3) 0.4159(2) 0.0239(11) Uani 1 1 d . . . C53 C -0.0732(6) 0.3087(4) 0.3802(3) 0.0335(14) Uani 1 1 d . . . H47A H -0.1506 0.3106 0.3981 0.050 Uiso 1 1 calc R . . H47B H -0.0531 0.2563 0.3722 0.050 Uiso 1 1 calc R . . H47C H -0.0772 0.3377 0.3473 0.050 Uiso 1 1 calc R . . B1 B 0.2761(6) 0.6243(4) 0.3910(2) 0.0204(12) Uani 1 1 d . . . H1 H 0.3020 0.6736 0.3757 0.025 Uiso 1 1 calc R . . Cl1 Cl 0.9232(2) 0.46934(16) 0.26269(10) 0.0677(6) Uani 1 1 d . . . Cl2 Cl 0.8473(3) 0.60257(13) 0.31981(10) 0.0672(7) Uani 1 1 d . . . C1S C 0.9452(10) 0.5274(6) 0.3178(4) 0.060(2) Uani 1 1 d . . . H1SA H 0.9355 0.4970 0.3504 0.072 Uiso 1 1 calc R . . H1SB H 1.0277 0.5468 0.3173 0.072 Uiso 1 1 calc R . . Cl3 Cl 0.5859(4) 0.4820(3) 0.2788(3) 0.108(2) Uani 0.766(10) 1 d P . . Cl4 Cl 0.5358(6) 0.4886(3) 0.1653(2) 0.139(3) Uani 0.766(10) 1 d P . . C2S C 0.5578(17) 0.4326(10) 0.2221(9) 0.095(6) Uani 0.766(10) 1 d P . . H2SA H 0.4860 0.4013 0.2277 0.114 Uiso 0.766(10) 1 calc PR . . H2SB H 0.6253 0.3981 0.2154 0.114 Uiso 0.766(10) 1 calc PR . . 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 0.0236(4) 0.0248(4) 0.0164(4) 0.0025(3) 0.0005(3) -0.0013(3) O1 0.0234(19) 0.029(2) 0.0221(19) 0.0055(16) -0.0020(15) -0.0029(15) O2 0.024(2) 0.034(2) 0.030(2) 0.0087(18) -0.0017(17) -0.0047(17) O3 0.030(2) 0.029(2) 0.0147(18) 0.0016(16) -0.0045(15) -0.0007(16) N1 0.026(2) 0.030(2) 0.014(2) 0.0006(18) 0.0024(18) -0.0023(18) N2 0.023(2) 0.028(2) 0.018(2) 0.0007(19) -0.0018(18) 0.0009(18) N3 0.025(2) 0.027(2) 0.018(2) 0.0013(19) -0.0020(19) -0.0025(18) N4 0.023(2) 0.028(2) 0.020(2) -0.0002(19) -0.0013(18) -0.0038(18) N5 0.022(2) 0.027(2) 0.019(2) 0.0062(18) -0.0016(18) -0.0041(18) N6 0.026(2) 0.027(2) 0.016(2) 0.0027(19) 0.0005(19) -0.0030(18) C1 0.026(3) 0.030(3) 0.020(3) 0.002(2) 0.001(2) 0.000(2) C2 0.023(3) 0.035(3) 0.029(3) 0.000(3) 0.004(2) -0.001(2) C3 0.024(3) 0.033(3) 0.026(3) -0.005(2) 0.006(2) -0.004(2) C4 0.025(3) 0.030(3) 0.018(3) 0.000(2) 0.000(2) 0.001(2) C5 0.023(3) 0.036(3) 0.016(2) 0.000(2) -0.004(2) -0.002(2) C6 0.028(3) 0.029(3) 0.019(3) 0.006(2) -0.002(2) 0.000(2) C7 0.029(3) 0.033(3) 0.019(3) 0.002(2) 0.002(2) 0.004(2) C8 0.046(4) 0.035(3) 0.013(3) -0.001(2) 0.002(2) -0.001(3) C9 0.025(3) 0.038(3) 0.015(3) 0.000(2) 0.001(2) 0.001(2) C10 0.031(3) 0.029(3) 0.023(3) -0.002(2) 0.001(2) 0.002(2) C11 0.032(3) 0.033(3) 0.035(3) -0.002(3) 0.003(3) 0.003(3) C12 0.049(4) 0.036(3) 0.032(3) 0.002(3) 0.003(3) 0.013(3) C13 0.053(4) 0.030(3) 0.038(4) 0.003(3) 0.015(3) -0.001(3) C14 0.035(3) 0.039(3) 0.037(4) -0.003(3) 0.010(3) -0.002(3) C15 0.028(3) 0.032(3) 0.032(3) -0.003(3) 0.006(2) 0.000(2) C16 0.025(3) 0.029(3) 0.032(3) -0.006(3) 0.008(2) 0.001(2) C17 0.027(3) 0.037(3) 0.043(4) 0.000(3) 0.006(3) 0.001(3) C18 0.024(3) 0.047(4) 0.048(4) -0.001(3) 0.006(3) -0.005(3) C19 0.032(3) 0.036(3) 0.041(4) 0.001(3) 0.013(3) -0.004(3) C20 0.036(3) 0.037(3) 0.031(3) 0.000(3) 0.006(3) 0.004(3) C21 0.026(3) 0.039(3) 0.025(3) -0.001(2) 0.004(2) 0.002(2) C22 0.022(3) 0.034(3) 0.023(3) 0.004(2) -0.002(2) 0.000(2) C23 0.035(3) 0.036(3) 0.031(3) 0.001(3) 0.001(3) -0.003(3) C24 0.046(4) 0.040(4) 0.050(4) 0.004(3) -0.005(3) -0.011(3) C25 0.042(4) 0.057(4) 0.045(4) 0.021(4) 0.004(3) -0.014(3) C26 0.033(3) 0.070(5) 0.042(4) 0.018(4) 0.000(3) -0.012(3) C27 0.027(3) 0.054(4) 0.019(3) 0.005(3) 0.000(2) -0.005(3) C28 0.032(3) 0.028(3) 0.012(2) 0.000(2) -0.006(2) -0.005(2) C29 0.033(3) 0.034(3) 0.016(3) 0.002(2) -0.002(2) 0.000(2) C30 0.050(4) 0.035(3) 0.022(3) 0.007(3) -0.005(3) 0.002(3) C31 0.053(4) 0.037(3) 0.014(3) 0.007(2) -0.006(3) -0.005(3) C32 0.046(4) 0.044(4) 0.014(3) -0.002(2) 0.005(2) -0.010(3) C33 0.035(3) 0.031(3) 0.024(3) 0.002(2) -0.001(3) -0.002(2) C34 0.038(3) 0.039(3) 0.007(2) 0.001(2) -0.003(2) -0.002(3) C35 0.036(3) 0.047(4) 0.027(3) 0.000(3) 0.002(3) -0.002(3) C36 0.050(4) 0.058(4) 0.020(3) 0.014(3) -0.001(3) -0.010(3) C37 0.076(5) 0.039(3) 0.023(3) 0.010(3) -0.016(4) -0.007(4) C38 0.073(5) 0.036(3) 0.027(3) 0.004(3) -0.008(4) 0.008(4) C39 0.063(5) 0.034(3) 0.020(3) 0.003(3) -0.002(3) 0.003(3) C40 0.031(3) 0.040(3) 0.017(3) 0.001(3) 0.007(2) 0.001(3) C41 0.044(4) 0.043(4) 0.025(3) -0.006(3) 0.000(3) 0.001(3) C42 0.046(4) 0.043(4) 0.033(4) -0.015(3) 0.006(3) -0.006(3) C43 0.048(4) 0.032(3) 0.048(4) -0.009(3) 0.017(3) -0.007(3) C44 0.053(4) 0.041(4) 0.035(4) 0.004(3) 0.005(3) 0.006(3) C45 0.041(4) 0.036(3) 0.032(3) 0.002(3) -0.002(3) 0.004(3) C46 0.026(3) 0.029(3) 0.011(2) 0.000(2) -0.003(2) 0.002(2) C47 0.030(3) 0.032(3) 0.014(2) 0.002(2) -0.001(2) 0.002(2) C48 0.027(3) 0.032(3) 0.018(3) -0.001(2) -0.004(2) 0.001(2) C49 0.026(3) 0.027(3) 0.017(2) 0.004(2) 0.004(2) 0.002(2) C50 0.022(3) 0.031(3) 0.018(3) 0.000(2) -0.002(2) 0.002(2) C51 0.022(3) 0.028(3) 0.011(2) 0.001(2) -0.0005(19) -0.001(2) C52 0.022(3) 0.032(3) 0.017(3) 0.000(2) 0.000(2) 0.000(2) C53 0.033(3) 0.042(3) 0.025(3) 0.005(3) -0.011(3) -0.008(3) B1 0.027(3) 0.025(3) 0.009(2) 0.002(2) -0.002(2) 0.000(2) Cl1 0.0747(15) 0.0749(14) 0.0534(12) -0.0158(11) -0.0033(11) 0.0115(13) Cl2 0.0999(19) 0.0497(11) 0.0519(12) 0.0000(9) -0.0186(12) 0.0137(11) C1S 0.077(6) 0.058(5) 0.045(4) -0.006(4) -0.008(4) 0.009(5) Cl3 0.075(3) 0.081(3) 0.169(5) -0.026(3) -0.056(3) 0.024(2) Cl4 0.165(5) 0.148(5) 0.105(4) 0.051(3) 0.070(4) 0.123(5) C2S 0.083(11) 0.083(11) 0.120(15) 0.017(10) 0.005(10) 0.047(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.937(4) . ? Fe1 O3 2.079(4) . ? Fe1 N1 2.131(5) . ? Fe1 N3 2.089(5) . ? Fe1 N5 2.185(5) . ? O1 C46 1.303(7) . ? O2 H3 0.8400 . ? O2 C49 1.370(7) . ? O3 C52 1.226(7) . ? N1 C9 1.343(8) . ? N2 N1 1.363(7) . ? N2 C7 1.349(8) . ? N2 B1 1.559(8) . ? N3 C3 1.354(8) . ? N4 N3 1.357(7) . ? N4 C1 1.354(8) . ? N4 B1 1.549(8) . ? N5 C6 1.355(8) . ? N6 N5 1.368(7) . ? N6 C4 1.376(8) . ? N6 B1 1.542(7) . ? C1 C2 1.411(8) . ? C1 C10 1.458(9) . ? C2 H2 0.9500 . ? C2 C3 1.390(9) . ? C3 C16 1.480(8) . ? C4 C5 1.392(8) . ? C4 C22 1.453(8) . ? C5 H5 0.9500 . ? C5 C6 1.398(8) . ? C6 C28 1.469(8) . ? C7 C8 1.371(9) . ? C7 C34 1.486(9) . ? C8 H8 0.9500 . ? C8 C9 1.414(9) . ? C9 C40 1.449(9) . ? C10 C11 1.392(9) . ? C10 C15 1.415(9) . ? C11 H11 0.9500 . ? C11 C12 1.364(10) . ? C12 H12 0.9500 . ? C12 C13 1.395(12) . ? C13 H13 0.9500 . ? C13 C14 1.383(11) . ? C14 H14 0.9500 . ? C14 C15 1.357(10) . ? C15 H15 0.9500 . ? C16 C17 1.397(9) . ? C16 C21 1.398(9) . ? C17 H17 0.9500 . ? C17 C18 1.386(10) . ? C18 H18 0.9500 . ? C18 C19 1.404(11) . ? C19 H19 0.9500 . ? C19 C20 1.399(10) . ? C20 H20 0.9500 . ? C20 C21 1.365(9) . ? C21 H21 0.9500 . ? C22 C23 1.398(9) . ? C22 C27 1.410(9) . ? C23 H23 0.9500 . ? C23 C24 1.373(10) . ? C24 H24 0.9500 . ? C24 C25 1.389(12) . ? C25 H25 0.9500 . ? C25 C26 1.397(13) . ? C26 H26 0.9500 . ? C26 C27 1.384(10) . ? C27 H27 0.9500 . ? C28 C29 1.395(9) . ? C28 C33 1.382(9) . ? C29 H29 0.9500 . ? C29 C30 1.398(9) . ? C30 H30 0.9500 . ? C30 C31 1.396(11) . ? C31 H31 0.9500 . ? C31 C32 1.376(11) . ? C32 H32 0.9500 . ? C32 C33 1.394(9) . ? C33 H33 0.9500 . ? C34 C35 1.386(9) . ? C34 C39 1.381(10) . ? C35 H35 0.9500 . ? C35 C36 1.386(11) . ? C36 H36 0.9500 . ? C36 C37 1.368(13) . ? C37 H37 0.9500 . ? C37 C38 1.381(13) . ? C38 H38 0.9500 . ? C38 C39 1.409(10) . ? C39 H39 0.9500 . ? C40 C41 1.408(10) . ? C40 C45 1.412(9) . ? C41 H41 0.9500 . ? C41 C42 1.375(10) . ? C42 H42 0.9500 . ? C42 C43 1.383(12) . ? C43 H43 0.9500 . ? C43 C44 1.390(12) . ? C44 H44 0.9500 . ? C44 C45 1.385(10) . ? C45 H45 0.9500 . ? C46 C47 1.412(8) . ? C47 H50 0.9500 . ? C47 C48 1.382(9) . ? C48 H51 0.9500 . ? C48 C49 1.405(8) . ? C49 C50 1.357(8) . ? C50 H53 0.9500 . ? C51 C46 1.441(8) . ? C51 C50 1.409(8) . ? C52 C51 1.465(8) . ? C52 C53 1.513(8) . ? C53 H47A 0.9800 . ? C53 H47B 0.9800 . ? C53 H47C 0.9800 . ? B1 H1 1.0000 . ? Cl1 C1S 1.751(9) . ? Cl2 C1S 1.731(10) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? Cl3 C2S 1.71(2) . ? Cl4 C2S 1.764(19) . ? C2S H2SA 0.9900 . ? C2S H2SB 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 O1 Fe1 O3 86.38(16) . . ? O1 Fe1 N1 129.53(19) . . ? O1 Fe1 N3 139.89(19) . . ? O1 Fe1 N5 97.90(17) . . ? O3 Fe1 N1 87.36(17) . . ? O3 Fe1 N3 95.33(17) . . ? O3 Fe1 N5 175.70(17) . . ? N1 Fe1 N5 90.17(19) . . ? N3 Fe1 N1 90.55(19) . . ? N3 Fe1 N5 81.17(18) . . ? C46 O1 Fe1 129.9(4) . . ? C49 O2 H3 109.5 . . ? C52 O3 Fe1 131.4(4) . . ? N2 N1 Fe1 114.7(3) . . ? C9 N1 Fe1 134.3(4) . . ? C9 N1 N2 107.3(5) . . ? N1 N2 B1 120.0(4) . . ? C7 N2 N1 110.1(5) . . ? C7 N2 B1 129.9(5) . . ? N4 N3 Fe1 118.5(4) . . ? C3 N3 Fe1 134.3(4) . . ? C3 N3 N4 107.3(5) . . ? N3 N4 B1 118.7(5) . . ? C1 N4 N3 110.4(5) . . ? C1 N4 B1 130.6(5) . . ? N6 N5 Fe1 112.9(3) . . ? C6 N5 Fe1 137.1(4) . . ? C6 N5 N6 107.0(4) . . ? N5 N6 C4 109.8(5) . . ? N5 N6 B1 118.9(4) . . ? C4 N6 B1 130.6(5) . . ? N4 C1 C2 107.1(5) . . ? N4 C1 C10 125.2(5) . . ? C2 C1 C10 127.6(6) . . ? C1 C2 H2 127.2 . . ? C3 C2 C1 105.6(5) . . ? C3 C2 H2 127.2 . . ? N3 C3 C2 109.7(5) . . ? N3 C3 C16 118.1(5) . . ? C2 C3 C16 132.2(5) . . ? N6 C4 C5 107.2(5) . . ? N6 C4 C22 124.7(5) . . ? C5 C4 C22 128.1(5) . . ? C4 C5 H5 126.9 . . ? C4 C5 C6 106.2(5) . . ? C6 C5 H5 126.9 . . ? N5 C6 C5 109.7(5) . . ? N5 C6 C28 120.8(5) . . ? C5 C6 C28 129.4(5) . . ? N2 C7 C8 107.9(5) . . ? N2 C7 C34 122.8(5) . . ? C8 C7 C34 129.3(5) . . ? C7 C8 H8 127.0 . . ? C7 C8 C9 106.1(5) . . ? C9 C8 H8 127.0 . . ? N1 C9 C8 108.6(5) . . ? N1 C9 C40 123.5(5) . . ? C8 C9 C40 127.9(6) . . ? C11 C10 C1 120.0(6) . . ? C11 C10 C15 118.3(6) . . ? C15 C10 C1 121.8(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 C10 120.6(7) . . ? C12 C11 H11 119.7 . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.8(7) . . ? C13 C12 H12 119.6 . . ? C12 C13 H13 120.6 . . ? C14 C13 C12 118.9(6) . . ? C14 C13 H13 120.6 . . ? C13 C14 H14 119.5 . . ? C15 C14 C13 121.0(7) . . ? C15 C14 H14 119.5 . . ? C10 C15 H15 119.8 . . ? C14 C15 C10 120.4(6) . . ? C14 C15 H15 119.8 . . ? C17 C16 C3 121.0(6) . . ? C17 C16 C21 118.8(6) . . ? C21 C16 C3 119.9(6) . . ? C16 C17 H17 120.0 . . ? C18 C17 C16 120.1(7) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.3(6) . . ? C19 C18 H18 119.9 . . ? C18 C19 H19 120.4 . . ? C20 C19 C18 119.2(6) . . ? C20 C19 H19 120.4 . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.0(6) . . ? C21 C20 H20 120.0 . . ? C16 C21 H21 119.2 . . ? C20 C21 C16 121.5(6) . . ? C20 C21 H21 119.2 . . ? C23 C22 C4 120.3(6) . . ? C23 C22 C27 117.3(6) . . ? C27 C22 C4 122.3(6) . . ? C22 C23 H23 119.2 . . ? C24 C23 C22 121.6(7) . . ? C24 C23 H23 119.2 . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.6(7) . . ? C25 C24 H24 119.7 . . ? C24 C25 H25 120.4 . . ? C24 C25 C26 119.3(7) . . ? C26 C25 H25 120.4 . . ? C25 C26 H26 120.1 . . ? C27 C26 C25 119.9(7) . . ? C27 C26 H26 120.1 . . ? C22 C27 H27 119.3 . . ? C26 C27 C22 121.3(7) . . ? C26 C27 H27 119.3 . . ? C29 C28 C6 120.1(5) . . ? C33 C28 C6 120.9(5) . . ? C33 C28 C29 119.0(5) . . ? C28 C29 H29 119.9 . . ? C28 C29 C30 120.1(6) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 119.9 . . ? C31 C30 C29 120.3(6) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 120.4 . . ? C32 C31 C30 119.2(6) . . ? C32 C31 H31 120.4 . . ? C31 C32 H32 119.7 . . ? C31 C32 C33 120.5(6) . . ? C33 C32 H32 119.7 . . ? C28 C33 C32 120.9(6) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C7 119.6(6) . . ? C39 C34 C7 120.2(6) . . ? C39 C34 C35 120.2(6) . . ? C34 C35 H35 120.0 . . ? C36 C35 C34 119.9(7) . . ? C36 C35 H35 120.0 . . ? C35 C36 H36 119.9 . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36 119.9 . . ? C36 C37 H37 119.6 . . ? C36 C37 C38 120.7(7) . . ? C38 C37 H37 119.6 . . ? C37 C38 H38 120.3 . . ? C37 C38 C39 119.4(8) . . ? C39 C38 H38 120.3 . . ? C34 C39 C38 119.5(8) . . ? C34 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C41 C40 C9 120.8(6) . . ? C41 C40 C45 118.1(6) . . ? C45 C40 C9 121.0(6) . . ? C40 C41 H41 119.5 . . ? C42 C41 C40 121.0(7) . . ? C42 C41 H41 119.5 . . ? C41 C42 H42 119.7 . . ? C41 C42 C43 120.6(7) . . ? C43 C42 H42 119.7 . . ? C42 C43 H43 120.2 . . ? C42 C43 C44 119.6(7) . . ? C44 C43 H43 120.2 . . ? C43 C44 H44 119.6 . . ? C45 C44 C43 120.8(7) . . ? C45 C44 H44 119.6 . . ? C40 C45 H45 120.0 . . ? C44 C45 C40 120.0(7) . . ? C44 C45 H45 120.0 . . ? O1 C46 C47 119.3(5) . . ? O1 C46 C51 124.5(5) . . ? C47 C46 C51 116.3(5) . . ? C46 C47 H50 118.7 . . ? C48 C47 C46 122.6(6) . . ? C48 C47 H50 118.7 . . ? C47 C48 H51 119.9 . . ? C47 C48 C49 120.2(5) . . ? C49 C48 H51 119.9 . . ? O2 C49 C48 116.5(5) . . ? C50 C49 O2 124.6(5) . . ? C50 C49 C48 118.9(5) . . ? C49 C50 H53 118.6 . . ? C49 C50 C51 122.7(5) . . ? C51 C50 H53 118.6 . . ? C46 C51 C52 121.3(5) . . ? C50 C51 C46 119.2(5) . . ? C50 C51 C52 119.3(5) . . ? O3 C52 C51 123.0(5) . . ? O3 C52 C53 117.2(5) . . ? C51 C52 C53 119.7(5) . . ? C52 C53 H47A 109.5 . . ? C52 C53 H47B 109.5 . . ? C52 C53 H47C 109.5 . . ? H47A C53 H47B 109.5 . . ? H47A C53 H47C 109.5 . . ? H47B C53 H47C 109.5 . . ? N2 B1 H1 110.1 . . ? N4 B1 N2 108.0(4) . . ? N4 B1 H1 110.1 . . ? N6 B1 N2 109.5(5) . . ? N6 B1 N4 109.1(4) . . ? N6 B1 H1 110.1 . . ? Cl1 C1S H1SA 109.0 . . ? Cl1 C1S H1SB 109.0 . . ? Cl2 C1S Cl1 112.8(6) . . ? Cl2 C1S H1SA 109.0 . . ? Cl2 C1S H1SB 109.0 . . ? H1SA C1S H1SB 107.8 . . ? Cl3 C2S Cl4 114.8(10) . . ? Cl3 C2S H2SA 108.6 . . ? Cl3 C2S H2SB 108.6 . . ? Cl4 C2S H2SA 108.6 . . ? Cl4 C2S H2SB 108.6 . . ? H2SA C2S H2SB 107.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H3 O1 0.84 2.00 2.735(6) 146.0 3_456 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 -155.2(4) . . . . ? Fe1 O1 C46 C51 23.7(8) . . . . ? Fe1 O3 C52 C51 5.7(9) . . . . ? Fe1 O3 C52 C53 -176.8(4) . . . . ? Fe1 N1 C9 C8 156.0(5) . . . . ? Fe1 N1 C9 C40 -23.5(9) . . . . ? Fe1 N3 C3 C2 -178.9(4) . . . . ? Fe1 N3 C3 C16 1.3(9) . . . . ? Fe1 N5 C6 C5 156.2(5) . . . . ? Fe1 N5 C6 C28 -27.1(9) . . . . ? O1 Fe1 O3 C52 5.2(5) . . . . ? O1 Fe1 N1 N2 -151.3(3) . . . . ? O1 Fe1 N1 C9 53.9(6) . . . . ? O1 Fe1 N3 N4 138.1(4) . . . . ? O1 Fe1 N3 C3 -42.8(7) . . . . ? O1 Fe1 N5 N6 156.8(4) . . . . ? O1 Fe1 N5 C6 -0.2(6) . . . . ? O1 C46 C47 C48 -178.1(5) . . . . ? O2 C49 C50 C51 -178.5(5) . . . . ? O3 Fe1 O1 C46 -19.6(5) . . . . ? O3 Fe1 N1 N2 125.6(4) . . . . ? O3 Fe1 N1 C9 -29.2(6) . . . . ? O3 Fe1 N3 N4 -131.2(4) . . . . ? O3 Fe1 N3 C3 47.9(6) . . . . ? O3 Fe1 N5 N6 -28(3) . . . . ? O3 Fe1 N5 C6 175(2) . . . . ? O3 C52 C51 C46 -7.5(9) . . . . ? O3 C52 C51 C50 168.0(5) . . . . ? N1 Fe1 O1 C46 -103.2(5) . . . . ? N1 Fe1 O3 C52 135.1(5) . . . . ? N1 Fe1 N3 N4 -43.8(4) . . . . ? N1 Fe1 N3 C3 135.3(6) . . . . ? N1 Fe1 N5 N6 26.8(4) . . . . ? N1 Fe1 N5 C6 -130.2(6) . . . . ? N1 N2 C7 C8 -0.1(7) . . . . ? N1 N2 C7 C34 179.2(5) . . . . ? N1 N2 B1 N4 -72.1(6) . . . . ? N1 N2 B1 N6 46.7(6) . . . . ? N1 C9 C40 C41 144.0(6) . . . . ? N1 C9 C40 C45 -35.9(9) . . . . ? N2 N1 C9 C8 -0.2(7) . . . . ? N2 N1 C9 C40 -179.6(6) . . . . ? N2 C7 C8 C9 0.0(7) . . . . ? N2 C7 C34 C35 122.9(7) . . . . ? N2 C7 C34 C39 -59.4(9) . . . . ? N3 Fe1 O1 C46 74.3(6) . . . . ? N3 Fe1 O3 C52 -134.6(5) . . . . ? N3 Fe1 N1 N2 30.3(4) . . . . ? N3 Fe1 N1 C9 -124.5(6) . . . . ? N3 Fe1 N5 N6 -63.8(4) . . . . ? N3 Fe1 N5 C6 139.3(6) . . . . ? N3 N4 C1 C2 -0.7(7) . . . . ? N3 N4 C1 C10 176.5(5) . . . . ? N3 N4 B1 N2 55.9(6) . . . . ? N3 N4 B1 N6 -63.1(6) . . . . ? N3 C3 C16 C17 -131.1(6) . . . . ? N3 C3 C16 C21 43.4(8) . . . . ? N4 N3 C3 C2 0.3(7) . . . . ? N4 N3 C3 C16 -179.5(5) . . . . ? N4 C1 C2 C3 0.9(7) . . . . ? N4 C1 C10 C11 139.8(6) . . . . ? N4 C1 C10 C15 -40.1(9) . . . . ? N5 Fe1 O1 C46 160.0(5) . . . . ? N5 Fe1 O3 C52 -170(2) . . . . ? N5 Fe1 N1 N2 -50.9(4) . . . . ? N5 Fe1 N1 C9 154.3(6) . . . . ? N5 Fe1 N3 N4 46.3(4) . . . . ? N5 Fe1 N3 C3 -134.6(6) . . . . ? N5 N6 C4 C5 -2.4(6) . . . . ? N5 N6 C4 C22 178.4(5) . . . . ? N5 N6 B1 N2 -77.0(6) . . . . ? N5 N6 B1 N4 41.1(6) . . . . ? N5 C6 C28 C29 137.8(6) . . . . ? N5 C6 C28 C33 -44.5(8) . . . . ? N6 N5 C6 C5 -1.7(6) . . . . ? N6 N5 C6 C28 175.0(5) . . . . ? N6 C4 C5 C6 1.3(6) . . . . ? N6 C4 C22 C23 143.6(6) . . . . ? N6 C4 C22 C27 -40.0(9) . . . . ? C1 N4 N3 Fe1 179.7(4) . . . . ? C1 N4 N3 C3 0.3(6) . . . . ? C1 N4 B1 N2 -117.1(6) . . . . ? C1 N4 B1 N6 124.0(6) . . . . ? C1 C2 C3 N3 -0.7(7) . . . . ? C1 C2 C3 C16 179.1(6) . . . . ? C1 C10 C11 C12 -179.6(6) . . . . ? C1 C10 C15 C14 -179.8(6) . . . . ? C2 C1 C10 C11 -43.5(9) . . . . ? C2 C1 C10 C15 136.6(7) . . . . ? C2 C3 C16 C17 49.1(10) . . . . ? C2 C3 C16 C21 -136.3(7) . . . . ? C3 C16 C17 C18 171.9(6) . . . . ? C3 C16 C21 C20 -172.5(6) . . . . ? C4 N6 N5 Fe1 -161.3(4) . . . . ? C4 N6 N5 C6 2.5(6) . . . . ? C4 N6 B1 N2 114.1(6) . . . . ? C4 N6 B1 N4 -127.8(6) . . . . ? C4 C5 C6 N5 0.2(7) . . . . ? C4 C5 C6 C28 -176.1(6) . . . . ? C4 C22 C23 C24 178.1(6) . . . . ? C4 C22 C27 C26 -178.6(7) . . . . ? C5 C4 C22 C23 -35.4(9) . . . . ? C5 C4 C22 C27 140.9(7) . . . . ? C5 C6 C28 C29 -46.2(9) . . . . ? C5 C6 C28 C33 131.4(7) . . . . ? C6 C28 C29 C30 178.0(6) . . . . ? C6 C28 C33 C32 -178.3(6) . . . . ? C7 N2 N1 Fe1 -161.3(4) . . . . ? C7 N2 N1 C9 0.1(6) . . . . ? C7 N2 B1 N4 108.4(6) . . . . ? C7 N2 B1 N6 -132.8(6) . . . . ? C7 C8 C9 N1 0.1(8) . . . . ? C7 C8 C9 C40 179.5(6) . . . . ? C7 C34 C35 C36 177.5(6) . . . . ? C7 C34 C39 C38 -177.4(6) . . . . ? C8 C7 C34 C35 -58.0(10) . . . . ? C8 C7 C34 C39 119.7(8) . . . . ? C8 C9 C40 C41 -35.3(10) . . . . ? C8 C9 C40 C45 144.8(7) . . . . ? C9 C40 C41 C42 180.0(6) . . . . ? C9 C40 C45 C44 -179.9(7) . . . . ? C10 C1 C2 C3 -176.2(6) . . . . ? C10 C11 C12 C13 0.8(11) . . . . ? C11 C10 C15 C14 0.3(9) . . . . ? C11 C12 C13 C14 -2.4(11) . . . . ? C12 C13 C14 C15 3.0(10) . . . . ? C13 C14 C15 C10 -1.9(10) . . . . ? C15 C10 C11 C12 0.3(10) . . . . ? C16 C17 C18 C19 1.6(11) . . . . ? C17 C16 C21 C20 2.1(9) . . . . ? C17 C18 C19 C20 -0.1(11) . . . . ? C18 C19 C20 C21 -0.4(10) . . . . ? C19 C20 C21 C16 -0.6(10) . . . . ? C21 C16 C17 C18 -2.6(10) . . . . ? C22 C4 C5 C6 -179.5(6) . . . . ? C22 C23 C24 C25 0.1(12) . . . . ? C23 C22 C27 C26 -2.1(10) . . . . ? C23 C24 C25 C26 -1.2(13) . . . . ? C24 C25 C26 C27 0.6(13) . . . . ? C25 C26 C27 C22 1.1(12) . . . . ? C27 C22 C23 C24 1.6(10) . . . . ? C28 C29 C30 C31 0.3(10) . . . . ? C29 C28 C33 C32 -0.6(9) . . . . ? C29 C30 C31 C32 -0.7(10) . . . . ? C30 C31 C32 C33 0.4(10) . . . . ? C31 C32 C33 C28 0.3(10) . . . . ? C33 C28 C29 C30 0.3(9) . . . . ? C34 C7 C8 C9 -179.2(6) . . . . ? C34 C35 C36 C37 0.1(11) . . . . ? C35 C34 C39 C38 0.3(10) . . . . ? C35 C36 C37 C38 0.0(11) . . . . ? C36 C37 C38 C39 0.0(12) . . . . ? C37 C38 C39 C34 -0.2(11) . . . . ? C39 C34 C35 C36 -0.2(10) . . . . ? C40 C41 C42 C43 -0.1(11) . . . . ? C41 C40 C45 C44 0.2(10) . . . . ? C41 C42 C43 C44 0.2(11) . . . . ? C42 C43 C44 C45 -0.1(12) . . . . ? C43 C44 C45 C40 -0.1(12) . . . . ? C45 C40 C41 C42 -0.1(10) . . . . ? C46 C47 C48 C49 0.3(9) . . . . ? C46 C51 C50 C49 1.0(9) . . . . ? C47 C48 C49 O2 177.8(5) . . . . ? C47 C48 C49 C50 -3.1(9) . . . . ? C48 C49 C50 C51 2.4(9) . . . . ? C50 C51 C46 O1 177.5(5) . . . . ? C50 C51 C46 C47 -3.6(8) . . . . ? C51 C46 C47 C48 3.0(8) . . . . ? C52 C51 C46 O1 -7.0(9) . . . . ? C52 C51 C46 C47 171.8(5) . . . . ? C52 C51 C50 C49 -174.5(5) . . . . ? C53 C52 C51 C46 175.1(5) . . . . ? C53 C52 C51 C50 -9.5(8) . . . . ? B1 N2 N1 Fe1 19.1(6) . . . . ? B1 N2 N1 C9 -179.4(5) . . . . ? B1 N2 C7 C8 179.5(6) . . . . ? B1 N2 C7 C34 -1.3(9) . . . . ? B1 N4 N3 Fe1 5.4(6) . . . . ? B1 N4 N3 C3 -174.0(5) . . . . ? B1 N4 C1 C2 172.6(5) . . . . ? B1 N4 C1 C10 -10.2(10) . . . . ? B1 N6 N5 Fe1 27.6(6) . . . . ? B1 N6 N5 C6 -168.6(5) . . . . ? B1 N6 C4 C5 167.3(5) . . . . ? B1 N6 C4 C22 -11.9(9) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 7 3 -4 0.1197 7.0000 3.0000 -4.0000 -0.1750 0.9704 -0.2753 0 0 -16 0.0510 0.0000 -0.0000 -16.0000 0.6383 0.1555 -0.7222 0 -10 -8 0.1154 0.0000 -10.0000 -8.0000 0.9641 0.1244 0.2167 -2 9 10 0.0444 -2.0000 9.0000 10.0000 -0.9391 -0.4093 -0.0911 -6 -6 -6 0.1180 -6.0000 -6.0000 -6.0000 0.7473 -0.7242 0.0084 -2 -3 16 0.0273 -2.0000 -3.0000 16.0000 -0.4044 -0.4116 0.8731 0 -10 7 0.0925 0.0000 -10.0000 7.0000 0.3658 -0.0214 0.8938 6 1 10 0.1313 6.0000 1.0000 10.0000 -0.5844 0.7086 0.4610 #==END data_Complex1C _database_code_depnum_ccdc_archive 'CCDC 890620' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C53 H41 B Fe N6 O2' _chemical_formula_sum 'C53 H41 B Fe N6 O2' _chemical_formula_weight 860.58 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C53 H41 N6 O2 B' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.41289(18) _cell_length_b 30.8300(5) _cell_length_c 13.1758(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.6340(15) _cell_angle_gamma 90.00 _cell_volume 4229.55(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 21135 _cell_measurement_temperature 100.5 _cell_measurement_theta_max 29.5838 _cell_measurement_theta_min 3.2819 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_unetI/netI 0.0280 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 58359 _diffrn_reflns_theta_full 28.00 _diffrn_reflns_theta_max 29.65 _diffrn_reflns_theta_min 3.29 _diffrn_ambient_temperature 100.5 _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -32.00 38.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 -77.0000 -60.0000 140 #__ type_ start__ end____ width___ exp.time_ 2 omega -15.00 87.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 37.0000 120.0000 204 #__ type_ start__ end____ width___ exp.time_ 3 omega 4.00 32.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - -11.8259 -109.0000 168.0000 56 #__ type_ start__ end____ width___ exp.time_ 4 omega -22.00 90.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 77.0000 -120.0000 224 #__ type_ start__ end____ width___ exp.time_ 5 omega -11.00 59.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 -109.0000 94.0000 140 #__ type_ start__ end____ width___ exp.time_ 6 omega -15.00 22.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 37.0000 -150.0000 74 #__ type_ start__ end____ width___ exp.time_ 7 omega -28.00 64.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - -11.8259 37.0000 -180.0000 184 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0376745000 _diffrn_orient_matrix_UB_12 -0.0179010000 _diffrn_orient_matrix_UB_13 0.0163974000 _diffrn_orient_matrix_UB_21 -0.0324260000 _diffrn_orient_matrix_UB_22 -0.0135492000 _diffrn_orient_matrix_UB_23 -0.0354378000 _diffrn_orient_matrix_UB_31 0.0465632000 _diffrn_orient_matrix_UB_32 0.0050444000 _diffrn_orient_matrix_UB_33 -0.0370655000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 9383 _reflns_number_total 10931 _reflns_odcompleteness_completeness 99.74 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET) (compiled Nov 25 2010,17:55:46) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.354 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 569 _refine_ls_number_reflns 10931 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0375 _refine_ls_restrained_S_all 1.027 _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^)+(0.0348P)^2^+3.2735P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0891 _refine_ls_wR_factor_ref 0.0953 _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 0.213541(19) 0.117799(6) 0.194507(15) 0.01487(6) Uani 1 1 d . . . O1 O 0.17622(11) 0.06299(3) 0.13039(8) 0.0238(2) Uani 1 1 d . . . O2 O 0.09056(10) 0.09625(3) 0.30958(8) 0.0199(2) Uani 1 1 d . . . N1 N 0.11128(11) 0.17657(4) 0.18061(9) 0.0155(2) Uani 1 1 d . . . N2 N 0.18207(11) 0.21396(4) 0.17863(9) 0.0151(2) Uani 1 1 d . . . N3 N 0.33343(11) 0.14404(4) 0.30732(9) 0.0152(2) Uani 1 1 d . . . N4 N 0.35744(11) 0.18739(4) 0.29953(9) 0.0148(2) Uani 1 1 d . . . N5 N 0.35793(11) 0.14467(4) 0.08799(9) 0.0156(2) Uani 1 1 d . . . N6 N 0.39310(11) 0.18644(4) 0.11121(9) 0.0155(2) Uani 1 1 d . . . C1 C 0.42150(13) 0.20132(5) 0.38366(10) 0.0170(3) Uani 1 1 d . . . C2 C 0.43984(14) 0.16613(5) 0.44729(11) 0.0186(3) Uani 1 1 d . . . H2 H 0.4822 0.1659 0.5115 0.022 Uiso 1 1 calc R . . C3 C 0.38269(13) 0.13094(5) 0.39686(10) 0.0164(3) Uani 1 1 d . . . C4 C 0.48910(13) 0.19982(5) 0.04942(10) 0.0175(3) Uani 1 1 d . . . C5 C 0.51761(14) 0.16593(5) -0.01453(11) 0.0209(3) Uani 1 1 d . . . H5 H 0.5810 0.1655 -0.0658 0.025 Uiso 1 1 calc R . . C6 C 0.43409(14) 0.13236(5) 0.01158(10) 0.0176(3) Uani 1 1 d . . . C7 C 0.10244(13) 0.24886(4) 0.17306(10) 0.0162(3) Uani 1 1 d . . . C8 C -0.02255(14) 0.23351(5) 0.17262(11) 0.0182(3) Uani 1 1 d . . . H8 H -0.0991 0.2502 0.1696 0.022 Uiso 1 1 calc R . . C9 C -0.01284(13) 0.18844(5) 0.17756(10) 0.0167(3) Uani 1 1 d . . . C10 C 0.46156(14) 0.24697(5) 0.39642(10) 0.0182(3) Uani 1 1 d . . . C11 C 0.37281(15) 0.28059(5) 0.38789(12) 0.0231(3) Uani 1 1 d . . . H11 H 0.2847 0.2743 0.3757 0.028 Uiso 1 1 calc R . . C12 C 0.41291(17) 0.32328(5) 0.39713(13) 0.0290(3) Uani 1 1 d . . . H12 H 0.3523 0.3462 0.3906 0.035 Uiso 1 1 calc R . . C13 C 0.54090(18) 0.33275(5) 0.41586(13) 0.0301(4) Uani 1 1 d . . . H13 H 0.5679 0.3621 0.4218 0.036 Uiso 1 1 calc R . . C14 C 0.62964(16) 0.29959(5) 0.42601(12) 0.0255(3) Uani 1 1 d . . . H14 H 0.7174 0.3061 0.4395 0.031 Uiso 1 1 calc R . . C15 C 0.59006(15) 0.25667(5) 0.41647(11) 0.0209(3) Uani 1 1 d . . . H15 H 0.6509 0.2339 0.4236 0.025 Uiso 1 1 calc R . . C16 C 0.37083(13) 0.08541(5) 0.42861(11) 0.0177(3) Uani 1 1 d . . . C17 C 0.35835(14) 0.07479(5) 0.53134(11) 0.0220(3) Uani 1 1 d . . . H17 H 0.3615 0.0970 0.5813 0.026 Uiso 1 1 calc R . . C18 C 0.34129(16) 0.03188(5) 0.56053(13) 0.0267(3) Uani 1 1 d . . . H18 H 0.3320 0.0250 0.6303 0.032 Uiso 1 1 calc R . . C19 C 0.33780(15) -0.00086(5) 0.48869(13) 0.0270(3) Uani 1 1 d . . . H19 H 0.3258 -0.0301 0.5091 0.032 Uiso 1 1 calc R . . C20 C 0.35194(15) 0.00923(5) 0.38652(13) 0.0248(3) Uani 1 1 d . . . H20 H 0.3501 -0.0132 0.3370 0.030 Uiso 1 1 calc R . . C21 C 0.36875(14) 0.05200(5) 0.35711(11) 0.0197(3) Uani 1 1 d . . . H21 H 0.3790 0.0587 0.2873 0.024 Uiso 1 1 calc R . . C22 C 0.54117(14) 0.24447(5) 0.04833(11) 0.0189(3) Uani 1 1 d . . . C23 C 0.59453(14) 0.26418(5) 0.13418(12) 0.0226(3) Uani 1 1 d . . . H23 H 0.6014 0.2485 0.1960 0.027 Uiso 1 1 calc R . . C24 C 0.63766(16) 0.30679(5) 0.12938(13) 0.0274(3) Uani 1 1 d . . . H24 H 0.6735 0.3202 0.1881 0.033 Uiso 1 1 calc R . . C25 C 0.62864(16) 0.32983(5) 0.03922(14) 0.0293(4) Uani 1 1 d . . . H25 H 0.6573 0.3591 0.0365 0.035 Uiso 1 1 calc R . . C26 C 0.57809(17) 0.31032(5) -0.04675(13) 0.0289(4) Uani 1 1 d . . . H26 H 0.5731 0.3260 -0.1088 0.035 Uiso 1 1 calc R . . C27 C 0.53456(16) 0.26783(5) -0.04241(12) 0.0240(3) Uani 1 1 d . . . H27 H 0.5000 0.2545 -0.1017 0.029 Uiso 1 1 calc R . . C28 C 0.42663(14) 0.08983(5) -0.03990(10) 0.0184(3) Uani 1 1 d . . . C29 C 0.53956(15) 0.06784(5) -0.06291(12) 0.0233(3) Uani 1 1 d . . . H29 H 0.6198 0.0789 -0.0397 0.028 Uiso 1 1 calc R . . C30 C 0.53596(17) 0.02980(5) -0.11955(12) 0.0273(3) Uani 1 1 d . . . H30 H 0.6134 0.0149 -0.1342 0.033 Uiso 1 1 calc R . . C31 C 0.42019(17) 0.01378(5) -0.15447(12) 0.0281(3) Uani 1 1 d . . . H31 H 0.4180 -0.0118 -0.1947 0.034 Uiso 1 1 calc R . . C32 C 0.30717(17) 0.03492(5) -0.13102(13) 0.0281(3) Uani 1 1 d . . . H32 H 0.2273 0.0236 -0.1543 0.034 Uiso 1 1 calc R . . C33 C 0.31023(15) 0.07266(5) -0.07358(12) 0.0236(3) Uani 1 1 d . . . H33 H 0.2322 0.0869 -0.0571 0.028 Uiso 1 1 calc R . . C34 C 0.14349(14) 0.29456(4) 0.16650(11) 0.0179(3) Uani 1 1 d . . . C35 C 0.24804(15) 0.30793(5) 0.10930(12) 0.0222(3) Uani 1 1 d . . . H35 H 0.2980 0.2871 0.0742 0.027 Uiso 1 1 calc R . . C36 C 0.27930(17) 0.35159(5) 0.10356(14) 0.0311(4) Uani 1 1 d . . . H36 H 0.3512 0.3604 0.0649 0.037 Uiso 1 1 calc R . . C37 C 0.20698(19) 0.38234(5) 0.15350(15) 0.0346(4) Uani 1 1 d . . . H37 H 0.2297 0.4121 0.1497 0.042 Uiso 1 1 calc R . . C38 C 0.10143(18) 0.36963(5) 0.20901(13) 0.0305(4) Uani 1 1 d . . . H38 H 0.0506 0.3907 0.2425 0.037 Uiso 1 1 calc R . . C39 C 0.06986(16) 0.32600(5) 0.21577(11) 0.0234(3) Uani 1 1 d . . . H39 H -0.0024 0.3174 0.2542 0.028 Uiso 1 1 calc R . . C40 C -0.11913(13) 0.15719(5) 0.18222(11) 0.0183(3) Uani 1 1 d . . . C41 C -0.22855(15) 0.16903(5) 0.23561(13) 0.0248(3) Uani 1 1 d . . . H41 H -0.2314 0.1963 0.2689 0.030 Uiso 1 1 calc R . . C42 C -0.33309(16) 0.14134(6) 0.24048(15) 0.0321(4) Uani 1 1 d . . . H42 H -0.4076 0.1498 0.2764 0.039 Uiso 1 1 calc R . . C43 C -0.32870(16) 0.10138(6) 0.19299(15) 0.0325(4) Uani 1 1 d . . . H43 H -0.4007 0.0825 0.1956 0.039 Uiso 1 1 calc R . . C44 C -0.21968(15) 0.08884(5) 0.14173(13) 0.0272(3) Uani 1 1 d . . . H44 H -0.2161 0.0610 0.1108 0.033 Uiso 1 1 calc R . . C45 C -0.11546(14) 0.11678(5) 0.13540(11) 0.0209(3) Uani 1 1 d . . . H45 H -0.0414 0.1083 0.0990 0.025 Uiso 1 1 calc R . . C46 C 0.12119(14) 0.02773(5) 0.16310(12) 0.0208(3) Uani 1 1 d . . . C47 C 0.12684(16) -0.00948(5) 0.10004(14) 0.0284(3) Uani 1 1 d . . . H49 H 0.1656 -0.0071 0.0353 0.034 Uiso 1 1 calc R . . C48 C 0.07808(17) -0.04878(5) 0.12957(15) 0.0328(4) Uani 1 1 d . . . H50 H 0.0846 -0.0731 0.0858 0.039 Uiso 1 1 calc R . . C49 C 0.01885(17) -0.05322(5) 0.22366(14) 0.0322(4) Uani 1 1 d . . . H51 H -0.0123 -0.0806 0.2452 0.039 Uiso 1 1 calc R . . C50 C 0.00630(16) -0.01740(5) 0.28443(13) 0.0278(3) Uani 1 1 d . . . H52 H -0.0370 -0.0202 0.3472 0.033 Uiso 1 1 calc R . . C51 C 0.05569(14) 0.02363(5) 0.25686(12) 0.0210(3) Uani 1 1 d . . . C52 C 0.03997(15) 0.06068(5) 0.32466(12) 0.0235(3) Uani 1 1 d . . . C53 C -0.0414(3) 0.05706(7) 0.41767(18) 0.0633(8) Uani 1 1 d . . . H53A H -0.0475 0.0855 0.4504 0.095 Uiso 1 1 calc R . . H53B H -0.0022 0.0363 0.4650 0.095 Uiso 1 1 calc R . . H53C H -0.1275 0.0470 0.3983 0.095 Uiso 1 1 calc R . . B1 B 0.32854(15) 0.21160(5) 0.19823(11) 0.0155(3) Uani 1 1 d . . . H1 H 0.3646 0.2416 0.2019 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01671(10) 0.01161(9) 0.01628(10) -0.00181(7) 0.00041(7) -0.00135(7) O1 0.0284(6) 0.0166(5) 0.0266(6) -0.0045(4) 0.0072(4) -0.0071(4) O2 0.0226(5) 0.0171(5) 0.0201(5) -0.0011(4) 0.0033(4) -0.0023(4) N1 0.0161(5) 0.0137(5) 0.0165(5) -0.0008(4) 0.0000(4) -0.0021(4) N2 0.0181(6) 0.0120(5) 0.0153(5) -0.0008(4) 0.0004(4) -0.0010(4) N3 0.0177(5) 0.0124(5) 0.0154(5) 0.0001(4) 0.0009(4) -0.0007(4) N4 0.0163(5) 0.0127(5) 0.0154(5) -0.0005(4) 0.0008(4) -0.0008(4) N5 0.0178(6) 0.0133(5) 0.0159(5) -0.0013(4) 0.0000(4) 0.0001(4) N6 0.0174(6) 0.0130(5) 0.0162(5) 0.0006(4) 0.0006(4) -0.0016(4) C1 0.0175(6) 0.0174(6) 0.0160(6) -0.0029(5) -0.0002(5) -0.0008(5) C2 0.0210(7) 0.0190(7) 0.0157(6) -0.0005(5) -0.0019(5) -0.0005(5) C3 0.0159(6) 0.0166(6) 0.0168(6) -0.0004(5) 0.0009(5) 0.0017(5) C4 0.0182(7) 0.0192(7) 0.0149(6) 0.0014(5) 0.0010(5) -0.0017(5) C5 0.0231(7) 0.0217(7) 0.0181(7) -0.0005(6) 0.0043(5) -0.0009(6) C6 0.0194(7) 0.0181(6) 0.0152(6) -0.0004(5) 0.0009(5) 0.0012(5) C7 0.0195(7) 0.0149(6) 0.0140(6) -0.0004(5) -0.0004(5) 0.0018(5) C8 0.0177(7) 0.0174(6) 0.0195(7) -0.0001(5) 0.0000(5) 0.0020(5) C9 0.0175(6) 0.0175(6) 0.0150(6) -0.0012(5) 0.0011(5) 0.0009(5) C10 0.0246(7) 0.0173(6) 0.0128(6) -0.0014(5) -0.0006(5) -0.0021(5) C11 0.0250(8) 0.0188(7) 0.0254(8) -0.0050(6) -0.0020(6) -0.0004(6) C12 0.0356(9) 0.0180(7) 0.0334(9) -0.0051(6) -0.0024(7) 0.0017(6) C13 0.0422(10) 0.0183(7) 0.0296(8) -0.0043(6) -0.0019(7) -0.0090(7) C14 0.0292(8) 0.0271(8) 0.0201(7) -0.0020(6) -0.0020(6) -0.0102(6) C15 0.0244(7) 0.0222(7) 0.0161(7) -0.0004(6) -0.0028(5) -0.0022(6) C16 0.0162(6) 0.0173(6) 0.0195(7) 0.0031(5) -0.0004(5) 0.0001(5) C17 0.0231(7) 0.0230(7) 0.0199(7) 0.0020(6) -0.0007(5) 0.0019(6) C18 0.0265(8) 0.0282(8) 0.0256(8) 0.0118(6) 0.0032(6) 0.0032(6) C19 0.0238(8) 0.0192(7) 0.0382(9) 0.0101(7) 0.0038(6) -0.0001(6) C20 0.0234(8) 0.0175(7) 0.0334(8) -0.0003(6) 0.0004(6) 0.0004(6) C21 0.0198(7) 0.0181(7) 0.0210(7) 0.0022(5) 0.0000(5) 0.0014(5) C22 0.0189(7) 0.0179(7) 0.0199(7) 0.0013(5) 0.0049(5) -0.0015(5) C23 0.0218(7) 0.0233(7) 0.0227(7) 0.0021(6) 0.0017(6) -0.0031(6) C24 0.0248(8) 0.0256(8) 0.0320(8) -0.0050(7) 0.0023(6) -0.0074(6) C25 0.0295(8) 0.0198(7) 0.0390(9) 0.0019(7) 0.0107(7) -0.0064(6) C26 0.0356(9) 0.0240(8) 0.0274(8) 0.0074(6) 0.0117(7) -0.0022(7) C27 0.0293(8) 0.0228(7) 0.0202(7) 0.0014(6) 0.0056(6) -0.0018(6) C28 0.0240(7) 0.0170(6) 0.0143(6) -0.0002(5) 0.0022(5) 0.0011(5) C29 0.0242(7) 0.0237(7) 0.0222(7) -0.0010(6) 0.0024(6) 0.0023(6) C30 0.0319(9) 0.0236(8) 0.0266(8) -0.0020(6) 0.0052(6) 0.0091(6) C31 0.0412(9) 0.0194(7) 0.0238(8) -0.0050(6) 0.0027(7) 0.0028(7) C32 0.0314(9) 0.0257(8) 0.0272(8) -0.0061(6) -0.0026(6) -0.0019(6) C33 0.0240(7) 0.0225(7) 0.0242(7) -0.0039(6) 0.0001(6) 0.0033(6) C34 0.0224(7) 0.0142(6) 0.0170(6) 0.0009(5) -0.0049(5) 0.0011(5) C35 0.0235(7) 0.0183(7) 0.0247(7) 0.0042(6) -0.0019(6) 0.0009(6) C36 0.0290(8) 0.0216(8) 0.0426(10) 0.0106(7) -0.0024(7) -0.0043(6) C37 0.0428(10) 0.0143(7) 0.0463(11) 0.0042(7) -0.0103(8) -0.0033(7) C38 0.0443(10) 0.0173(7) 0.0297(8) -0.0041(6) -0.0085(7) 0.0080(7) C39 0.0325(8) 0.0192(7) 0.0184(7) -0.0008(6) -0.0031(6) 0.0051(6) C40 0.0169(7) 0.0189(7) 0.0190(7) 0.0013(5) -0.0006(5) -0.0004(5) C41 0.0213(7) 0.0212(7) 0.0321(8) 0.0004(6) 0.0063(6) 0.0014(6) C42 0.0201(8) 0.0288(8) 0.0477(10) 0.0033(8) 0.0119(7) 0.0010(6) C43 0.0214(8) 0.0256(8) 0.0505(11) 0.0038(8) 0.0023(7) -0.0068(6) C44 0.0253(8) 0.0200(7) 0.0362(9) -0.0019(7) -0.0016(6) -0.0031(6) C45 0.0184(7) 0.0217(7) 0.0226(7) -0.0018(6) 0.0000(5) -0.0003(5) C46 0.0190(7) 0.0160(6) 0.0274(7) -0.0031(6) -0.0014(6) -0.0018(5) C47 0.0298(8) 0.0205(7) 0.0347(9) -0.0076(7) 0.0028(7) -0.0026(6) C48 0.0360(9) 0.0169(7) 0.0456(10) -0.0073(7) 0.0003(8) -0.0027(7) C49 0.0362(9) 0.0170(7) 0.0432(10) 0.0031(7) -0.0055(7) -0.0067(7) C50 0.0303(8) 0.0227(7) 0.0303(8) 0.0038(6) -0.0022(6) -0.0059(6) C51 0.0201(7) 0.0168(7) 0.0260(7) 0.0007(6) -0.0024(6) -0.0023(5) C52 0.0250(8) 0.0209(7) 0.0247(7) 0.0016(6) 0.0025(6) -0.0034(6) C53 0.102(2) 0.0367(11) 0.0522(13) -0.0130(10) 0.0510(14) -0.0297(12) B1 0.0169(7) 0.0142(7) 0.0154(7) -0.0003(6) -0.0003(5) -0.0010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9267(10) . ? Fe1 O2 2.1030(10) . ? Fe1 N1 2.1084(12) . ? Fe1 N3 2.0933(12) . ? Fe1 N5 2.2278(12) . ? O1 C46 1.3043(17) . ? O2 C52 1.2339(18) . ? N1 C9 1.3435(18) . ? N2 N1 1.3688(15) . ? N2 C7 1.3596(17) . ? N2 B1 1.5459(19) . ? N3 C3 1.3434(18) . ? N4 N3 1.3637(15) . ? N4 C1 1.3572(18) . ? N4 B1 1.5556(19) . ? N5 C6 1.3432(18) . ? N6 N5 1.3725(16) . ? N6 C4 1.3602(17) . ? N6 B1 1.5444(19) . ? C1 C2 1.383(2) . ? C1 C10 1.4767(19) . ? C2 H2 0.9500 . ? C2 C3 1.402(2) . ? C3 C16 1.4703(19) . ? C4 C5 1.377(2) . ? C4 C22 1.4797(19) . ? C5 H5 0.9500 . ? C5 C6 1.397(2) . ? C6 C28 1.4779(19) . ? C7 C8 1.385(2) . ? C7 C34 1.4751(19) . ? C8 H8 0.9500 . ? C8 C9 1.3945(19) . ? C9 C40 1.4692(19) . ? C10 C11 1.392(2) . ? C10 C15 1.393(2) . ? C11 H11 0.9500 . ? C11 C12 1.386(2) . ? C12 H12 0.9500 . ? C12 C13 1.384(3) . ? C13 H13 0.9500 . ? C13 C14 1.384(2) . ? C14 H14 0.9500 . ? C14 C15 1.391(2) . ? C15 H15 0.9500 . ? C16 C17 1.400(2) . ? C16 C21 1.396(2) . ? C17 H17 0.9500 . ? C17 C18 1.390(2) . ? C18 H18 0.9500 . ? C18 C19 1.384(2) . ? C19 H19 0.9500 . ? C19 C20 1.391(2) . ? C20 H20 0.9500 . ? C20 C21 1.386(2) . ? C21 H21 0.9500 . ? C22 C23 1.394(2) . ? C22 C27 1.397(2) . ? C23 H23 0.9500 . ? C23 C24 1.390(2) . ? C24 H24 0.9500 . ? C24 C25 1.386(2) . ? C25 H25 0.9500 . ? C25 C26 1.381(3) . ? C26 H26 0.9500 . ? C26 C27 1.387(2) . ? C27 H27 0.9500 . ? C28 C29 1.394(2) . ? C28 C33 1.391(2) . ? C29 H29 0.9500 . ? C29 C30 1.390(2) . ? C30 H30 0.9500 . ? C30 C31 1.377(2) . ? C31 H31 0.9500 . ? C31 C32 1.383(2) . ? C32 H32 0.9500 . ? C32 C33 1.388(2) . ? C33 H33 0.9500 . ? C34 C35 1.393(2) . ? C34 C39 1.400(2) . ? C35 H35 0.9500 . ? C35 C36 1.387(2) . ? C36 H36 0.9500 . ? C36 C37 1.382(3) . ? C37 H37 0.9500 . ? C37 C38 1.384(3) . ? C38 H38 0.9500 . ? C38 C39 1.388(2) . ? C39 H39 0.9500 . ? C40 C41 1.394(2) . ? C40 C45 1.391(2) . ? C41 H41 0.9500 . ? C41 C42 1.386(2) . ? C42 H42 0.9500 . ? C42 C43 1.383(3) . ? C43 H43 0.9500 . ? C43 C44 1.383(2) . ? C44 H44 0.9500 . ? C44 C45 1.389(2) . ? C45 H45 0.9500 . ? C46 C47 1.418(2) . ? C47 H49 0.9500 . ? C47 C48 1.372(2) . ? C48 H50 0.9500 . ? C48 C49 1.397(3) . ? C49 H51 0.9500 . ? C49 C50 1.371(2) . ? C50 H52 0.9500 . ? C51 C46 1.423(2) . ? C51 C50 1.415(2) . ? C52 C51 1.460(2) . ? C52 C53 1.501(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? B1 H1 1.0000 . ? 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 O1 Fe1 O2 85.28(4) . . ? O1 Fe1 N1 128.04(5) . . ? O1 Fe1 N3 140.01(5) . . ? O1 Fe1 N5 100.61(4) . . ? O2 Fe1 N1 91.32(4) . . ? O2 Fe1 N5 172.83(4) . . ? N1 Fe1 N5 88.25(4) . . ? N3 Fe1 O2 88.47(4) . . ? N3 Fe1 N1 91.50(4) . . ? N3 Fe1 N5 84.39(4) . . ? C46 O1 Fe1 132.32(10) . . ? C52 O2 Fe1 131.40(10) . . ? N2 N1 Fe1 117.00(8) . . ? C9 N1 Fe1 136.18(9) . . ? C9 N1 N2 106.74(11) . . ? N1 N2 B1 119.18(11) . . ? C7 N2 N1 109.83(11) . . ? C7 N2 B1 130.26(11) . . ? N4 N3 Fe1 115.70(9) . . ? C3 N3 Fe1 136.57(9) . . ? C3 N3 N4 107.00(11) . . ? N3 N4 B1 120.05(11) . . ? C1 N4 N3 109.73(11) . . ? C1 N4 B1 129.62(12) . . ? N6 N5 Fe1 112.88(8) . . ? C6 N5 Fe1 140.83(10) . . ? C6 N5 N6 105.89(11) . . ? N5 N6 B1 121.29(11) . . ? C4 N6 N5 110.32(11) . . ? C4 N6 B1 128.38(12) . . ? N4 C1 C2 108.07(12) . . ? N4 C1 C10 122.01(12) . . ? C2 C1 C10 129.91(13) . . ? C1 C2 H2 127.3 . . ? C1 C2 C3 105.36(12) . . ? C3 C2 H2 127.3 . . ? N3 C3 C2 109.84(12) . . ? N3 C3 C16 120.31(12) . . ? C2 C3 C16 129.85(13) . . ? N6 C4 C5 107.52(12) . . ? N6 C4 C22 124.04(12) . . ? C5 C4 C22 128.22(13) . . ? C4 C5 H5 127.1 . . ? C4 C5 C6 105.81(12) . . ? C6 C5 H5 127.1 . . ? N5 C6 C5 110.45(12) . . ? N5 C6 C28 124.48(13) . . ? C5 C6 C28 125.02(13) . . ? N2 C7 C8 107.60(12) . . ? N2 C7 C34 125.59(13) . . ? C8 C7 C34 126.80(13) . . ? C7 C8 H8 127.1 . . ? C7 C8 C9 105.82(12) . . ? C9 C8 H8 127.1 . . ? N1 C9 C8 110.00(12) . . ? N1 C9 C40 123.02(12) . . ? C8 C9 C40 126.94(13) . . ? C11 C10 C1 120.92(13) . . ? C11 C10 C15 119.38(13) . . ? C15 C10 C1 119.70(13) . . ? C10 C11 H11 120.0 . . ? C12 C11 C10 120.06(15) . . ? C12 C11 H11 120.0 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.31(15) . . ? C13 C12 H12 119.8 . . ? C12 C13 H13 119.9 . . ? C14 C13 C12 120.15(15) . . ? C14 C13 H13 119.9 . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.82(15) . . ? C15 C14 H14 120.1 . . ? C10 C15 H15 119.9 . . ? C14 C15 C10 120.27(14) . . ? C14 C15 H15 119.9 . . ? C17 C16 C3 120.49(13) . . ? C21 C16 C3 120.87(13) . . ? C21 C16 C17 118.62(13) . . ? C16 C17 H17 119.9 . . ? C18 C17 C16 120.24(14) . . ? C18 C17 H17 119.9 . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.50(15) . . ? C19 C18 H18 119.7 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.77(14) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 120.1 . . ? C21 C20 C19 119.89(15) . . ? C21 C20 H20 120.1 . . ? C16 C21 H21 119.5 . . ? C20 C21 C16 120.96(14) . . ? C20 C21 H21 119.5 . . ? C23 C22 C4 122.71(13) . . ? C23 C22 C27 119.03(14) . . ? C27 C22 C4 118.26(13) . . ? C22 C23 H23 120.0 . . ? C24 C23 C22 120.06(15) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.29(16) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 120.0 . . ? C26 C25 C24 120.07(15) . . ? C26 C25 H25 120.0 . . ? C25 C26 H26 120.0 . . ? C25 C26 C27 119.93(15) . . ? C27 C26 H26 120.0 . . ? C22 C27 H27 119.7 . . ? C26 C27 C22 120.60(15) . . ? C26 C27 H27 119.7 . . ? C29 C28 C6 119.42(13) . . ? C33 C28 C6 121.68(13) . . ? C33 C28 C29 118.69(14) . . ? C28 C29 H29 119.7 . . ? C30 C29 C28 120.61(15) . . ? C30 C29 H29 119.7 . . ? C29 C30 H30 120.0 . . ? C31 C30 C29 120.01(15) . . ? C31 C30 H30 120.0 . . ? C30 C31 H31 120.0 . . ? C30 C31 C32 120.02(15) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.15(16) . . ? C33 C32 H32 119.9 . . ? C28 C33 H33 119.8 . . ? C32 C33 C28 120.50(15) . . ? C32 C33 H33 119.8 . . ? C35 C34 C7 122.89(13) . . ? C35 C34 C39 118.76(14) . . ? C39 C34 C7 118.27(13) . . ? C34 C35 H35 119.9 . . ? C36 C35 C34 120.13(15) . . ? C36 C35 H35 119.9 . . ? C35 C36 H36 119.7 . . ? C37 C36 C35 120.69(16) . . ? C37 C36 H36 119.7 . . ? C36 C37 H37 120.1 . . ? C36 C37 C38 119.83(15) . . ? C38 C37 H37 120.1 . . ? C37 C38 H38 120.0 . . ? C37 C38 C39 119.91(16) . . ? C39 C38 H38 120.0 . . ? C34 C39 H39 119.7 . . ? C38 C39 C34 120.66(16) . . ? C38 C39 H39 119.7 . . ? C41 C40 C9 118.00(13) . . ? C45 C40 C9 122.98(13) . . ? C45 C40 C41 119.01(14) . . ? C40 C41 H41 119.7 . . ? C42 C41 C40 120.58(15) . . ? C42 C41 H41 119.7 . . ? C41 C42 H42 120.1 . . ? C43 C42 C41 119.88(15) . . ? C43 C42 H42 120.1 . . ? C42 C43 H43 119.9 . . ? C42 C43 C44 120.12(15) . . ? C44 C43 H43 119.9 . . ? C43 C44 H44 119.9 . . ? C43 C44 C45 120.15(15) . . ? C45 C44 H44 119.9 . . ? C40 C45 H45 119.9 . . ? C44 C45 C40 120.24(14) . . ? C44 C45 H45 119.9 . . ? O1 C46 C47 117.36(14) . . ? O1 C46 C51 125.26(13) . . ? C47 C46 C51 117.39(14) . . ? C46 C47 H49 119.0 . . ? C48 C47 C46 122.04(16) . . ? C48 C47 H49 119.0 . . ? C47 C48 H50 119.8 . . ? C47 C48 C49 120.44(16) . . ? C49 C48 H50 119.8 . . ? C48 C49 H51 120.5 . . ? C50 C49 C48 119.01(15) . . ? C50 C49 H51 120.5 . . ? C49 C50 H52 118.9 . . ? C49 C50 C51 122.21(16) . . ? C51 C50 H52 118.9 . . ? C46 C51 C52 121.30(13) . . ? C50 C51 C46 118.77(14) . . ? C50 C51 C52 119.92(14) . . ? O2 C52 C51 123.08(14) . . ? O2 C52 C53 116.31(15) . . ? C51 C52 C53 120.61(14) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 B1 N4 110.31(11) . . ? N2 B1 H1 109.5 . . ? N4 B1 H1 109.5 . . ? N6 B1 N2 109.66(11) . . ? N6 B1 N4 108.33(11) . . ? N6 B1 H1 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 -170.38(11) . . . . ? Fe1 O1 C46 C51 9.8(2) . . . . ? Fe1 O2 C52 C51 -1.7(2) . . . . ? Fe1 O2 C52 C53 178.77(16) . . . . ? Fe1 N1 C9 C8 176.81(10) . . . . ? Fe1 N1 C9 C40 -1.4(2) . . . . ? Fe1 N3 C3 C2 -169.69(10) . . . . ? Fe1 N3 C3 C16 9.9(2) . . . . ? Fe1 N5 C6 C5 -171.83(11) . . . . ? Fe1 N5 C6 C28 10.3(2) . . . . ? O1 Fe1 O2 C52 8.72(14) . . . . ? O1 Fe1 N1 N2 -142.49(9) . . . . ? O1 Fe1 N1 C9 41.55(15) . . . . ? O1 Fe1 N3 N4 156.33(8) . . . . ? O1 Fe1 N3 C3 -34.98(17) . . . . ? O1 Fe1 N5 N6 174.25(9) . . . . ? O1 Fe1 N5 C6 -14.42(16) . . . . ? O1 C46 C47 C48 176.48(16) . . . . ? O2 Fe1 O1 C46 -12.58(14) . . . . ? O2 Fe1 N1 N2 132.48(9) . . . . ? O2 Fe1 N1 C9 -43.48(14) . . . . ? O2 Fe1 N3 N4 -122.88(9) . . . . ? O2 Fe1 N3 C3 45.80(14) . . . . ? O2 Fe1 N5 N6 -40.9(4) . . . . ? O2 Fe1 N5 C6 130.5(3) . . . . ? O2 C52 C51 C46 -6.2(2) . . . . ? O2 C52 C51 C50 173.26(15) . . . . ? N1 Fe1 O1 C46 -100.56(14) . . . . ? N1 Fe1 O2 C52 136.79(14) . . . . ? N1 Fe1 N3 N4 -31.60(9) . . . . ? N1 Fe1 N3 C3 137.09(14) . . . . ? N1 Fe1 N5 N6 45.82(9) . . . . ? N1 Fe1 N5 C6 -142.84(15) . . . . ? N1 N2 C7 C8 0.69(15) . . . . ? N1 N2 C7 C34 -178.13(12) . . . . ? N1 N2 B1 N4 -53.20(15) . . . . ? N1 N2 B1 N6 66.03(15) . . . . ? N1 C9 C40 C41 143.05(15) . . . . ? N1 C9 C40 C45 -37.4(2) . . . . ? N2 N1 C9 C8 0.57(15) . . . . ? N2 N1 C9 C40 -177.68(12) . . . . ? N2 C7 C8 C9 -0.32(15) . . . . ? N2 C7 C34 C35 38.8(2) . . . . ? N2 C7 C34 C39 -144.61(14) . . . . ? N3 Fe1 O1 C46 69.36(16) . . . . ? N3 Fe1 O2 C52 -131.75(14) . . . . ? N3 Fe1 N1 N2 43.98(9) . . . . ? N3 Fe1 N1 C9 -131.98(14) . . . . ? N3 Fe1 N5 N6 -45.86(9) . . . . ? N3 Fe1 N5 C6 125.48(15) . . . . ? N3 N4 C1 C2 0.22(15) . . . . ? N3 N4 C1 C10 179.52(12) . . . . ? N3 N4 B1 N2 68.59(15) . . . . ? N3 N4 B1 N6 -51.44(15) . . . . ? N3 C3 C16 C17 -147.10(14) . . . . ? N3 C3 C16 C21 31.4(2) . . . . ? N4 N3 C3 C2 -0.34(15) . . . . ? N4 N3 C3 C16 179.20(12) . . . . ? N4 C1 C2 C3 -0.41(16) . . . . ? N4 C1 C10 C11 54.5(2) . . . . ? N4 C1 C10 C15 -124.99(15) . . . . ? N5 Fe1 O1 C46 163.29(13) . . . . ? N5 Fe1 O2 C52 -136.7(3) . . . . ? N5 Fe1 N1 N2 -40.36(9) . . . . ? N5 Fe1 N1 C9 143.68(14) . . . . ? N5 Fe1 N3 N4 56.50(9) . . . . ? N5 Fe1 N3 C3 -134.82(14) . . . . ? N5 N6 C4 C5 -0.55(16) . . . . ? N5 N6 C4 C22 174.36(13) . . . . ? N5 N6 B1 N2 -57.86(16) . . . . ? N5 N6 B1 N4 62.58(15) . . . . ? N5 C6 C28 C29 -137.46(15) . . . . ? N5 C6 C28 C33 47.9(2) . . . . ? N6 N5 C6 C5 -0.13(16) . . . . ? N6 N5 C6 C28 -177.96(13) . . . . ? N6 C4 C5 C6 0.45(16) . . . . ? N6 C4 C22 C23 58.2(2) . . . . ? N6 C4 C22 C27 -120.83(16) . . . . ? C1 N4 N3 Fe1 171.97(9) . . . . ? C1 N4 N3 C3 0.08(15) . . . . ? C1 N4 B1 N2 -121.30(14) . . . . ? C1 N4 B1 N6 118.66(14) . . . . ? C1 C2 C3 N3 0.47(16) . . . . ? C1 C2 C3 C16 -179.02(14) . . . . ? C1 C10 C11 C12 -178.09(14) . . . . ? C1 C10 C15 C14 178.32(13) . . . . ? C2 C1 C10 C11 -126.38(17) . . . . ? C2 C1 C10 C15 54.1(2) . . . . ? C2 C3 C16 C17 32.3(2) . . . . ? C2 C3 C16 C21 -149.17(15) . . . . ? C3 C16 C17 C18 177.06(14) . . . . ? C3 C16 C21 C20 -177.15(13) . . . . ? C4 N6 N5 Fe1 174.75(9) . . . . ? C4 N6 N5 C6 0.42(15) . . . . ? C4 N6 B1 N2 123.47(14) . . . . ? C4 N6 B1 N4 -116.09(15) . . . . ? C4 C5 C6 N5 -0.20(17) . . . . ? C4 C5 C6 C28 177.61(13) . . . . ? C4 C22 C23 C24 -177.66(14) . . . . ? C4 C22 C27 C26 177.86(14) . . . . ? C5 C4 C22 C23 -127.94(17) . . . . ? C5 C4 C22 C27 53.0(2) . . . . ? C5 C6 C28 C29 45.0(2) . . . . ? C5 C6 C28 C33 -129.63(16) . . . . ? C6 C28 C29 C30 -173.99(14) . . . . ? C6 C28 C33 C32 173.18(14) . . . . ? C7 N2 N1 Fe1 -177.86(9) . . . . ? C7 N2 N1 C9 -0.78(14) . . . . ? C7 N2 B1 N4 115.98(15) . . . . ? C7 N2 B1 N6 -124.79(14) . . . . ? C7 C8 C9 N1 -0.16(16) . . . . ? C7 C8 C9 C40 178.01(13) . . . . ? C7 C34 C35 C36 177.91(14) . . . . ? C7 C34 C39 C38 -177.66(14) . . . . ? C8 C7 C34 C35 -139.80(16) . . . . ? C8 C7 C34 C39 36.8(2) . . . . ? C8 C9 C40 C41 -34.9(2) . . . . ? C8 C9 C40 C45 144.65(15) . . . . ? C9 C40 C41 C42 178.39(15) . . . . ? C9 C40 C45 C44 -179.34(14) . . . . ? C10 C1 C2 C3 -179.64(14) . . . . ? C10 C11 C12 C13 -0.6(3) . . . . ? C11 C10 C15 C14 -1.2(2) . . . . ? C11 C12 C13 C14 -0.3(3) . . . . ? C12 C13 C14 C15 0.6(2) . . . . ? C13 C14 C15 C10 0.2(2) . . . . ? C15 C10 C11 C12 1.4(2) . . . . ? C16 C17 C18 C19 0.7(2) . . . . ? C17 C16 C21 C20 1.4(2) . . . . ? C17 C18 C19 C20 0.2(2) . . . . ? C18 C19 C20 C21 -0.3(2) . . . . ? C19 C20 C21 C16 -0.5(2) . . . . ? C21 C16 C17 C18 -1.5(2) . . . . ? C22 C4 C5 C6 -174.18(14) . . . . ? C22 C23 C24 C25 -0.4(2) . . . . ? C23 C22 C27 C26 -1.2(2) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C24 C25 C26 C27 1.0(3) . . . . ? C25 C26 C27 C22 0.1(2) . . . . ? C27 C22 C23 C24 1.4(2) . . . . ? C28 C29 C30 C31 0.8(2) . . . . ? C29 C28 C33 C32 -1.5(2) . . . . ? C29 C30 C31 C32 -1.7(3) . . . . ? C30 C31 C32 C33 1.0(3) . . . . ? C31 C32 C33 C28 0.6(2) . . . . ? C33 C28 C29 C30 0.8(2) . . . . ? C34 C7 C8 C9 178.47(13) . . . . ? C34 C35 C36 C37 -0.5(3) . . . . ? C35 C34 C39 C38 -0.9(2) . . . . ? C35 C36 C37 C38 -0.7(3) . . . . ? C36 C37 C38 C39 1.1(3) . . . . ? C37 C38 C39 C34 -0.3(2) . . . . ? C39 C34 C35 C36 1.3(2) . . . . ? C40 C41 C42 C43 0.7(3) . . . . ? C41 C40 C45 C44 0.2(2) . . . . ? C41 C42 C43 C44 0.8(3) . . . . ? C42 C43 C44 C45 -1.7(3) . . . . ? C43 C44 C45 C40 1.3(2) . . . . ? C45 C40 C41 C42 -1.2(2) . . . . ? C46 C47 C48 C49 0.9(3) . . . . ? C46 C51 C50 C49 -0.3(2) . . . . ? C47 C48 C49 C50 2.2(3) . . . . ? C48 C49 C50 C51 -2.5(3) . . . . ? C50 C51 C46 O1 -176.83(15) . . . . ? C50 C51 C46 C47 3.3(2) . . . . ? C51 C46 C47 C48 -3.7(2) . . . . ? C52 C51 C46 O1 2.6(2) . . . . ? C52 C51 C46 C47 -177.24(15) . . . . ? C52 C51 C50 C49 -179.79(16) . . . . ? C53 C52 C51 C46 173.36(19) . . . . ? C53 C52 C51 C50 -7.2(3) . . . . ? B1 N2 N1 Fe1 -6.62(15) . . . . ? B1 N2 N1 C9 170.46(11) . . . . ? B1 N2 C7 C8 -169.28(13) . . . . ? B1 N2 C7 C34 11.9(2) . . . . ? B1 N4 N3 Fe1 -16.12(15) . . . . ? B1 N4 N3 C3 171.99(11) . . . . ? B1 N4 C1 C2 -170.69(13) . . . . ? B1 N4 C1 C10 8.6(2) . . . . ? B1 N6 N5 Fe1 -4.14(15) . . . . ? B1 N6 N5 C6 -178.46(12) . . . . ? B1 N6 C4 C5 178.23(13) . . . . ? B1 N6 C4 C22 -6.9(2) . . . . ? #==END data_Complex1D _database_code_depnum_ccdc_archive 'CCDC 890621' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-06 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H41 B Fe N6 O3, C F3 O3 S, C6 H16 N' _chemical_formula_sum 'C59 H57 B F3 Fe N7 O6 S' _chemical_formula_weight 1115.84 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C52 H43 N6 O3 B S O3 C F3 N H Et3' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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' _cell_length_a 9.6832(4) _cell_length_b 9.8868(5) _cell_length_c 28.3671(15) _cell_angle_alpha 85.740(4) _cell_angle_beta 86.952(4) _cell_angle_gamma 81.003(4) _cell_volume 2672.5(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5257 _cell_measurement_temperature 100.05(10) _cell_measurement_theta_max 73.6278 _cell_measurement_theta_min 4.5337 _exptl_absorpt_coefficient_mu 3.209 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1164 _exptl_crystal_size_max 0.5543 _exptl_crystal_size_mid 0.2374 _exptl_crystal_size_min 0.0231 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 15029 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.94 _diffrn_reflns_theta_min 4.54 _diffrn_ambient_temperature 100.05(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -13.00 15.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 37.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 2 omega -70.00 -7.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 125.0000 -90.0000 63 #__ type_ start__ end____ width___ exp.time_ 3 omega -46.00 30.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 37.0000 90.0000 76 #__ type_ start__ end____ width___ exp.time_ 4 omega -49.00 35.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 37.0000 -60.0000 84 #__ type_ start__ end____ width___ exp.time_ 5 omega -114.00 -21.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 -57.0000 150.0000 93 #__ type_ start__ end____ width___ exp.time_ 6 omega 36.00 97.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 40.4246 -125.0000 -180.0000 61 #__ type_ start__ end____ width___ exp.time_ 7 omega 98.00 178.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 77.0000 60.0000 80 #__ type_ start__ end____ width___ exp.time_ 8 omega 117.00 170.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 150.0000 53 #__ type_ start__ end____ width___ exp.time_ 9 omega 44.00 105.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 -180.0000 61 #__ type_ start__ end____ width___ exp.time_ 10 omega 30.00 82.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -30.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 11 omega 94.00 149.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 125.0000 150.0000 55 #__ type_ start__ end____ width___ exp.time_ 12 omega 23.00 107.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 -90.0000 84 #__ type_ start__ end____ width___ exp.time_ 13 omega 53.00 105.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -94.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 14 omega 81.00 121.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -125.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 15 omega 76.00 147.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 77.0000 -150.0000 71 #__ type_ start__ end____ width___ exp.time_ 16 omega 34.00 137.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -61.0000 30.0000 103 #__ type_ start__ end____ width___ exp.time_ 17 omega 90.00 165.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 45.0000 120.0000 75 #__ type_ start__ end____ width___ exp.time_ 18 omega 45.00 90.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 -45.0000 -90.0000 45 #__ type_ start__ end____ width___ exp.time_ 19 omega -119.00 -7.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 -77.0000 60.0000 112 #__ type_ start__ end____ width___ exp.time_ 20 omega -114.00 -11.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 -57.0000 -60.0000 103 #__ type_ start__ end____ width___ exp.time_ 21 omega -49.00 36.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 37.0000 -180.0000 85 #__ type_ start__ end____ width___ exp.time_ 22 omega -119.00 -7.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 -77.0000 120.0000 112 #__ type_ start__ end____ width___ exp.time_ 23 omega -114.00 -11.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - -40.4246 -57.0000 -150.0000 103 #__ type_ start__ end____ width___ exp.time_ 24 omega 73.00 153.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 77.0000 30.0000 80 #__ type_ start__ end____ width___ exp.time_ 25 omega 23.00 178.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 107.0119 8.0000 18.0000 155 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1218974000 _diffrn_orient_matrix_UB_12 0.0823802000 _diffrn_orient_matrix_UB_13 0.0018858000 _diffrn_orient_matrix_UB_21 -0.1033533000 _diffrn_orient_matrix_UB_22 0.1349585000 _diffrn_orient_matrix_UB_23 -0.0053370000 _diffrn_orient_matrix_UB_31 -0.0212539000 _diffrn_orient_matrix_UB_32 -0.0002134000 _diffrn_orient_matrix_UB_33 0.0542123000 loop_ _diffrn_oxdiff_twin_id _diffrn_oxdiff_twin_ratio _diffrn_oxdiff_twin_reflns_isolated _diffrn_oxdiff_twin_reflns_overlapped 1 0.5109 7205 22371 2 0.4891 7209 22371 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 12570 _reflns_number_total 15029 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.729 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.106 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 709 _refine_ls_number_reflns 15029 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0864 _refine_ls_restrained_S_all 1.074 _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^)+(0.1262P)^2^+6.9507P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2278 _refine_ls_wR_factor_ref 0.2402 _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 0.47338(8) 0.62499(8) 0.21277(3) 0.02326(18) Uani 1 1 d . . . O1 O 0.3433(4) 0.5125(3) 0.24278(12) 0.0275(7) Uani 1 1 d . . . O2 O 0.2924(5) 0.4619(5) 0.43774(14) 0.0446(10) Uani 1 1 d . . . H3 H 0.2472 0.3988 0.4477 0.067 Uiso 1 1 calc R . . O3 O 0.4979(4) 0.6382(4) 0.29303(12) 0.0289(7) Uani 1 1 d . . . N1 N 0.4582(4) 0.8427(4) 0.20873(14) 0.0230(8) Uani 1 1 d . . . N2 N 0.5419(4) 0.8928(4) 0.17328(14) 0.0209(7) Uani 1 1 d . . . N3 N 0.6962(4) 0.5907(4) 0.20925(14) 0.0244(8) Uani 1 1 d . . . N4 N 0.7456(4) 0.7014(4) 0.18730(13) 0.0211(8) Uani 1 1 d . . . N5 N 0.4899(4) 0.6299(4) 0.13553(14) 0.0209(7) Uani 1 1 d . . . N6 N 0.5942(4) 0.7016(4) 0.11830(13) 0.0219(8) Uani 1 1 d . . . C1 C 0.5231(5) 1.0339(5) 0.17327(17) 0.0235(9) Uani 1 1 d . . . C2 C 0.4273(5) 1.0708(5) 0.21019(18) 0.0258(9) Uani 1 1 d . . . H2 H 0.3943 1.1610 0.2194 0.031 Uiso 1 1 calc R . . C3 C 0.3891(5) 0.9479(5) 0.23112(17) 0.0241(9) Uani 1 1 d . . . C4 C 0.6071(5) 0.6990(5) 0.07022(17) 0.0238(9) Uani 1 1 d . . . C5 C 0.5082(5) 0.6250(5) 0.05654(17) 0.0264(10) Uani 1 1 d . . . H5 H 0.4906 0.6066 0.0252 0.032 Uiso 1 1 calc R . . C6 C 0.4393(5) 0.5827(4) 0.09828(17) 0.0247(10) Uani 1 1 d . . . C7 C 0.8842(5) 0.6941(5) 0.19451(16) 0.0224(9) Uani 1 1 d . . . C8 C 0.9251(5) 0.5712(5) 0.22129(18) 0.0260(10) Uani 1 1 d . . . H8 H 1.0164 0.5362 0.2315 0.031 Uiso 1 1 calc R . . C9 C 0.8052(5) 0.5107(4) 0.22989(16) 0.0222(9) Uani 1 1 d . . . C10 C 0.5933(5) 1.1213(5) 0.13868(17) 0.0224(9) Uani 1 1 d . . . C11 C 0.6137(5) 1.0957(5) 0.09132(18) 0.0270(10) Uani 1 1 d . . . H11 H 0.5812 1.0185 0.0803 0.032 Uiso 1 1 calc R . . C12 C 0.6799(5) 1.1795(5) 0.06001(18) 0.0293(10) Uani 1 1 d . . . H12 H 0.6934 1.1599 0.0277 0.035 Uiso 1 1 calc R . . C13 C 0.7274(5) 1.2943(5) 0.07603(19) 0.0308(11) Uani 1 1 d . . . H13 H 0.7745 1.3524 0.0548 0.037 Uiso 1 1 calc R . . C14 C 0.7050(5) 1.3216(5) 0.12281(19) 0.0292(10) Uani 1 1 d . . . H14 H 0.7361 1.3998 0.1337 0.035 Uiso 1 1 calc R . . C15 C 0.6385(5) 1.2381(5) 0.15423(19) 0.0279(10) Uani 1 1 d . . . H15 H 0.6231 1.2592 0.1864 0.033 Uiso 1 1 calc R . . C16 C 0.2906(5) 0.9323(5) 0.27157(17) 0.0260(10) Uani 1 1 d . . . C17 C 0.2848(5) 1.0179(5) 0.30897(18) 0.0307(11) Uani 1 1 d . . . H17 H 0.3421 1.0880 0.3072 0.037 Uiso 1 1 calc R . . C18 C 0.1975(6) 1.0025(6) 0.3483(2) 0.0359(12) Uani 1 1 d . . . H18 H 0.1941 1.0623 0.3732 0.043 Uiso 1 1 calc R . . C19 C 0.1136(6) 0.8985(6) 0.35146(19) 0.0364(12) Uani 1 1 d . . . H19 H 0.0547 0.8857 0.3788 0.044 Uiso 1 1 calc R . . C20 C 0.1178(6) 0.8145(5) 0.3140(2) 0.0339(11) Uani 1 1 d . . . H20 H 0.0603 0.7445 0.3156 0.041 Uiso 1 1 calc R . . C21 C 0.2049(5) 0.8320(5) 0.27457(19) 0.0305(11) Uani 1 1 d . . . H21 H 0.2060 0.7744 0.2492 0.037 Uiso 1 1 calc R . . C22 C 0.7098(5) 0.7631(5) 0.04016(17) 0.0260(10) Uani 1 1 d . . . C23 C 0.6631(5) 0.8441(5) -0.00016(17) 0.0283(10) Uani 1 1 d . . . H23 H 0.5668 0.8574 -0.0071 0.034 Uiso 1 1 calc R . . C24 C 0.7579(6) 0.9053(6) -0.03028(19) 0.0353(12) Uani 1 1 d . . . H24 H 0.7258 0.9601 -0.0576 0.042 Uiso 1 1 calc R . . C25 C 0.8981(6) 0.8866(6) -0.0204(2) 0.0354(12) Uani 1 1 d . . . H25 H 0.9625 0.9276 -0.0411 0.042 Uiso 1 1 calc R . . C26 C 0.9445(6) 0.8073(6) 0.01986(19) 0.0343(12) Uani 1 1 d . . . H26 H 1.0407 0.7953 0.0268 0.041 Uiso 1 1 calc R . . C27 C 0.8513(5) 0.7456(5) 0.04998(18) 0.0299(11) Uani 1 1 d . . . H27 H 0.8840 0.6913 0.0774 0.036 Uiso 1 1 calc R . . C28 C 0.3230(5) 0.5014(5) 0.10130(17) 0.0242(9) Uani 1 1 d . . . C29 C 0.2952(5) 0.4202(5) 0.14206(18) 0.0275(10) Uani 1 1 d . . . H29 H 0.3547 0.4120 0.1680 0.033 Uiso 1 1 calc R . . C30 C 0.1810(5) 0.3521(5) 0.14443(19) 0.0308(11) Uani 1 1 d . . . H30 H 0.1612 0.2984 0.1724 0.037 Uiso 1 1 calc R . . C31 C 0.0943(6) 0.3609(5) 0.1064(2) 0.0340(12) Uani 1 1 d . . . H31 H 0.0165 0.3127 0.1082 0.041 Uiso 1 1 calc R . . C32 C 0.1224(5) 0.4399(5) 0.0660(2) 0.0317(11) Uani 1 1 d . . . H32 H 0.0635 0.4470 0.0400 0.038 Uiso 1 1 calc R . . C33 C 0.2368(6) 0.5094(5) 0.06353(19) 0.0310(11) Uani 1 1 d . . . H33 H 0.2562 0.5632 0.0355 0.037 Uiso 1 1 calc R . . C34 C 0.9671(5) 0.7993(5) 0.17681(17) 0.0225(9) Uani 1 1 d . . . C35 C 0.9183(5) 0.9386(5) 0.18215(17) 0.0246(10) Uani 1 1 d . . . H35 H 0.8289 0.9654 0.1969 0.030 Uiso 1 1 calc R . . C36 C 0.9994(5) 1.0376(5) 0.16606(19) 0.0276(10) Uani 1 1 d . . . H36 H 0.9650 1.1320 0.1693 0.033 Uiso 1 1 calc R . . C37 C 1.1307(5) 0.9983(5) 0.14530(18) 0.0287(10) Uani 1 1 d . . . H37 H 1.1876 1.0658 0.1350 0.034 Uiso 1 1 calc R . . C38 C 1.1793(6) 0.8621(5) 0.13951(19) 0.0296(11) Uani 1 1 d . . . H38 H 1.2688 0.8363 0.1246 0.036 Uiso 1 1 calc R . . C39 C 1.0986(5) 0.7613(5) 0.15536(17) 0.0256(10) Uani 1 1 d . . . H39 H 1.1332 0.6673 0.1515 0.031 Uiso 1 1 calc R . . C40 C 0.7949(5) 0.3744(5) 0.25380(17) 0.0250(10) Uani 1 1 d . . . C41 C 0.9166(5) 0.2785(5) 0.25768(19) 0.0293(10) Uani 1 1 d . . . H41 H 1.0042 0.3041 0.2470 0.035 Uiso 1 1 calc R . . C42 C 0.9110(6) 0.1462(5) 0.2770(2) 0.0372(12) Uani 1 1 d . . . H42 H 0.9945 0.0819 0.2796 0.045 Uiso 1 1 calc R . . C43 C 0.7829(6) 0.1079(5) 0.2924(2) 0.0345(12) Uani 1 1 d . . . H43 H 0.7785 0.0172 0.3054 0.041 Uiso 1 1 calc R . . C44 C 0.6637(6) 0.2016(5) 0.2887(2) 0.0347(12) Uani 1 1 d . . . H44 H 0.5762 0.1756 0.2992 0.042 Uiso 1 1 calc R . . C45 C 0.6688(5) 0.3359(5) 0.26945(19) 0.0294(11) Uani 1 1 d . . . H45 H 0.5852 0.4002 0.2672 0.035 Uiso 1 1 calc R . . C46 C 0.3281(5) 0.4954(5) 0.28987(18) 0.0275(10) Uani 1 1 d . . . C47 C 0.2357(6) 0.4177(6) 0.3129(2) 0.0344(12) Uani 1 1 d . . . H51 H 0.1807 0.3709 0.2948 0.041 Uiso 1 1 calc R . . C48 C 0.2212(6) 0.4062(6) 0.3620(2) 0.0385(13) Uani 1 1 d . . . H50 H 0.1549 0.3536 0.3769 0.046 Uiso 1 1 calc R . . C49 C 0.3010(6) 0.4693(6) 0.38925(18) 0.0334(11) Uani 1 1 d . . . C50 C 0.3988(6) 0.5484(5) 0.36725(19) 0.0321(11) Uani 1 1 d . . . H48 H 0.4565 0.5916 0.3856 0.039 Uiso 1 1 calc R . . C51 C 0.4084(5) 0.5615(5) 0.31870(17) 0.0284(10) Uani 1 1 d . . . C52 C 0.5875(6) 0.7063(6) 0.3179(2) 0.0389(13) Uani 1 1 d . . . H52A H 0.6489 0.7509 0.2953 0.058 Uiso 1 1 calc R . . H52B H 0.6445 0.6393 0.3390 0.058 Uiso 1 1 calc R . . H52C H 0.5309 0.7756 0.3367 0.058 Uiso 1 1 calc R . . B1 B 0.6585(5) 0.7949(5) 0.14937(18) 0.0211(10) Uani 1 1 d . . . H1 H 0.7212 0.8491 0.1293 0.025 Uiso 1 1 calc R . . S1 S 0.15815(16) 0.18311(15) 0.51645(5) 0.0403(3) Uani 1 1 d . . . F1 F 0.0630(6) 0.3727(5) 0.5737(2) 0.0927(18) Uani 1 1 d . . . F2 F 0.2814(5) 0.3655(5) 0.55227(19) 0.0792(14) Uani 1 1 d . . . F3 F 0.2159(6) 0.2123(6) 0.60308(15) 0.0800(15) Uani 1 1 d . . . O4 O 0.1203(5) 0.2784(5) 0.47671(17) 0.0580(13) Uani 1 1 d . . . O5 O 0.0503(5) 0.1083(5) 0.53537(16) 0.0540(12) Uani 1 1 d . . . O6 O 0.2942(5) 0.1013(5) 0.51090(18) 0.0584(13) Uani 1 1 d . . . C53 C 0.1808(8) 0.2876(8) 0.5626(3) 0.0561(18) Uani 1 1 d . . . N7 N 0.7088(5) 0.1822(5) 0.45589(17) 0.0387(11) Uani 1 1 d . . . H7 H 0.7199 0.0914 0.4681 0.046 Uiso 1 1 calc R . . C54 C 0.7428(7) 0.2611(7) 0.4953(2) 0.0467(15) Uani 1 1 d . . . H54A H 0.6983 0.3580 0.4902 0.056 Uiso 1 1 calc R . . H54B H 0.8454 0.2594 0.4951 0.056 Uiso 1 1 calc R . . C55 C 0.6931(9) 0.2031(8) 0.5428(2) 0.0584(19) Uani 1 1 d . . . H55A H 0.5906 0.2154 0.5446 0.088 Uiso 1 1 calc R . . H55B H 0.7261 0.2512 0.5680 0.088 Uiso 1 1 calc R . . H55C H 0.7303 0.1051 0.5467 0.088 Uiso 1 1 calc R . . C56 C 0.8132(8) 0.1835(7) 0.4149(2) 0.0509(16) Uani 1 1 d . . . H56A H 0.9075 0.1462 0.4261 0.061 Uiso 1 1 calc R . . H56B H 0.7904 0.1226 0.3912 0.061 Uiso 1 1 calc R . . C57 C 0.8161(10) 0.3236(7) 0.3916(3) 0.065(2) Uani 1 1 d . . . H57A H 0.8777 0.3171 0.3630 0.098 Uiso 1 1 calc R . . H57B H 0.8511 0.3811 0.4135 0.098 Uiso 1 1 calc R . . H57C H 0.7212 0.3646 0.3830 0.098 Uiso 1 1 calc R . . C58 C 0.5571(7) 0.2164(8) 0.4449(3) 0.0576(18) Uani 1 1 d . . . H58A H 0.5001 0.2134 0.4748 0.069 Uiso 1 1 calc R . . H58B H 0.5393 0.3114 0.4304 0.069 Uiso 1 1 calc R . . C59 C 0.5107(8) 0.1227(9) 0.4124(3) 0.062(2) Uani 1 1 d . . . H59A H 0.5728 0.1175 0.3840 0.093 Uiso 1 1 calc R . . H59B H 0.4147 0.1579 0.4035 0.093 Uiso 1 1 calc R . . H59C H 0.5139 0.0310 0.4284 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0239(4) 0.0199(3) 0.0277(4) 0.0013(3) 0.0009(3) -0.0104(3) O1 0.0357(19) 0.0253(17) 0.0246(16) -0.0020(13) -0.0048(14) -0.0125(14) O2 0.058(3) 0.047(3) 0.030(2) 0.0036(17) 0.0049(18) -0.018(2) O3 0.0334(18) 0.0293(18) 0.0281(17) 0.0002(14) -0.0017(14) -0.0183(15) N1 0.0195(17) 0.0262(19) 0.0246(19) 0.0016(16) 0.0029(15) -0.0108(15) N2 0.0223(18) 0.0147(17) 0.0282(19) 0.0008(15) 0.0011(15) -0.0125(14) N3 0.0253(19) 0.0221(18) 0.028(2) 0.0026(16) -0.0035(16) -0.0118(15) N4 0.0245(19) 0.0160(17) 0.0249(19) 0.0017(14) -0.0014(15) -0.0108(15) N5 0.0217(18) 0.0156(17) 0.0267(19) -0.0005(14) -0.0035(15) -0.0063(14) N6 0.0240(19) 0.0216(19) 0.0234(19) 0.0007(15) 0.0017(15) -0.0154(15) C1 0.025(2) 0.015(2) 0.031(2) 0.0031(18) -0.0028(19) -0.0100(17) C2 0.025(2) 0.019(2) 0.035(2) -0.0016(19) 0.002(2) -0.0112(17) C3 0.026(2) 0.022(2) 0.026(2) 0.0017(18) 0.0008(18) -0.0114(18) C4 0.029(2) 0.015(2) 0.028(2) 0.0013(17) 0.0011(19) -0.0095(18) C5 0.029(2) 0.023(2) 0.029(2) -0.0021(18) -0.004(2) -0.0078(19) C6 0.033(3) 0.014(2) 0.028(2) -0.0004(17) -0.0052(19) -0.0078(18) C7 0.021(2) 0.019(2) 0.029(2) -0.0009(18) 0.0011(18) -0.0093(17) C8 0.023(2) 0.021(2) 0.035(3) 0.0020(19) -0.0034(19) -0.0057(17) C9 0.023(2) 0.017(2) 0.028(2) 0.0000(17) -0.0039(18) -0.0081(17) C10 0.026(2) 0.016(2) 0.028(2) 0.0027(17) 0.0000(18) -0.0123(17) C11 0.032(3) 0.019(2) 0.032(3) -0.0005(19) -0.004(2) -0.0115(19) C12 0.033(3) 0.025(2) 0.029(2) 0.0013(19) 0.002(2) -0.007(2) C13 0.030(3) 0.029(3) 0.036(3) 0.005(2) 0.001(2) -0.014(2) C14 0.024(2) 0.024(2) 0.042(3) -0.003(2) 0.001(2) -0.0124(19) C15 0.031(3) 0.019(2) 0.037(3) -0.0033(19) -0.001(2) -0.0133(19) C16 0.027(2) 0.027(2) 0.026(2) 0.0006(19) -0.0014(19) -0.0096(19) C17 0.031(3) 0.030(3) 0.033(3) -0.006(2) -0.002(2) -0.009(2) C18 0.035(3) 0.040(3) 0.033(3) -0.005(2) 0.002(2) -0.006(2) C19 0.038(3) 0.042(3) 0.028(3) 0.001(2) 0.004(2) -0.007(2) C20 0.033(3) 0.030(3) 0.038(3) 0.005(2) -0.001(2) -0.008(2) C21 0.035(3) 0.024(2) 0.033(3) 0.001(2) -0.004(2) -0.007(2) C22 0.032(2) 0.021(2) 0.028(2) -0.0038(18) 0.001(2) -0.0143(19) C23 0.031(3) 0.031(3) 0.024(2) -0.0005(19) 0.0023(19) -0.013(2) C24 0.047(3) 0.031(3) 0.029(3) 0.003(2) 0.001(2) -0.015(2) C25 0.039(3) 0.035(3) 0.037(3) -0.005(2) 0.012(2) -0.023(2) C26 0.031(3) 0.039(3) 0.037(3) -0.009(2) 0.006(2) -0.019(2) C27 0.032(3) 0.031(3) 0.030(2) -0.008(2) 0.001(2) -0.012(2) C28 0.027(2) 0.019(2) 0.030(2) -0.0044(18) -0.0005(19) -0.0110(18) C29 0.029(2) 0.024(2) 0.031(3) 0.0021(19) 0.002(2) -0.010(2) C30 0.034(3) 0.028(3) 0.033(3) 0.002(2) 0.001(2) -0.015(2) C31 0.031(3) 0.026(2) 0.048(3) -0.003(2) -0.004(2) -0.013(2) C32 0.028(3) 0.030(3) 0.040(3) -0.002(2) -0.010(2) -0.012(2) C33 0.037(3) 0.025(2) 0.032(3) -0.001(2) -0.006(2) -0.008(2) C34 0.019(2) 0.019(2) 0.030(2) -0.0018(18) 0.0004(19) -0.0058(17) C35 0.027(2) 0.018(2) 0.031(2) -0.0038(18) 0.0009(19) -0.0127(18) C36 0.028(2) 0.017(2) 0.040(3) 0.0005(19) 0.000(2) -0.0113(19) C37 0.026(2) 0.027(2) 0.034(3) 0.004(2) 0.000(2) -0.012(2) C38 0.033(3) 0.019(2) 0.037(3) 0.0011(19) 0.003(2) -0.008(2) C39 0.020(2) 0.023(2) 0.034(2) 0.0031(19) 0.0001(19) -0.0063(18) C40 0.030(2) 0.017(2) 0.029(2) 0.0012(18) -0.0039(19) -0.0083(18) C41 0.030(2) 0.023(2) 0.036(3) 0.003(2) -0.005(2) -0.0088(19) C42 0.046(3) 0.020(2) 0.044(3) 0.005(2) -0.002(3) -0.004(2) C43 0.045(3) 0.021(2) 0.037(3) 0.005(2) -0.003(2) -0.007(2) C44 0.040(3) 0.027(3) 0.039(3) 0.006(2) -0.002(2) -0.014(2) C45 0.031(3) 0.020(2) 0.038(3) 0.007(2) -0.001(2) -0.0127(19) C46 0.030(3) 0.025(2) 0.030(2) 0.0005(19) 0.003(2) -0.013(2) C47 0.034(3) 0.037(3) 0.036(3) 0.004(2) -0.002(2) -0.021(2) C48 0.040(3) 0.035(3) 0.041(3) 0.005(2) 0.009(2) -0.014(2) C49 0.040(3) 0.033(3) 0.027(3) 0.004(2) 0.008(2) -0.011(2) C50 0.037(3) 0.030(3) 0.031(3) -0.001(2) 0.000(2) -0.012(2) C51 0.035(3) 0.025(2) 0.027(2) 0.0024(19) 0.000(2) -0.011(2) C52 0.038(3) 0.043(3) 0.041(3) -0.004(3) -0.005(2) -0.022(3) B1 0.017(2) 0.024(3) 0.024(2) -0.003(2) -0.0011(19) -0.011(2) S1 0.0486(8) 0.0364(7) 0.0373(7) 0.0017(6) 0.0034(6) -0.0141(6) F1 0.086(4) 0.062(3) 0.132(5) -0.044(3) 0.035(3) -0.014(3) F2 0.087(3) 0.066(3) 0.097(4) -0.016(3) 0.008(3) -0.049(3) F3 0.101(4) 0.106(4) 0.045(2) -0.003(2) -0.009(2) -0.050(3) O4 0.062(3) 0.065(3) 0.045(3) 0.022(2) -0.006(2) -0.017(2) O5 0.070(3) 0.054(3) 0.046(2) 0.000(2) 0.000(2) -0.037(2) O6 0.050(3) 0.050(3) 0.067(3) 0.001(2) 0.010(2) 0.008(2) C53 0.061(4) 0.053(4) 0.061(4) -0.007(3) 0.009(3) -0.031(3) N7 0.037(3) 0.043(3) 0.037(2) 0.000(2) -0.001(2) -0.010(2) C54 0.052(4) 0.054(4) 0.037(3) -0.007(3) -0.004(3) -0.016(3) C55 0.078(5) 0.062(5) 0.037(3) -0.006(3) 0.002(3) -0.015(4) C56 0.065(4) 0.047(4) 0.043(3) -0.005(3) 0.009(3) -0.018(3) C57 0.101(6) 0.047(4) 0.053(4) -0.007(3) 0.015(4) -0.034(4) C58 0.042(4) 0.060(4) 0.070(5) -0.003(4) -0.013(3) -0.003(3) C59 0.064(5) 0.083(6) 0.045(4) 0.007(4) -0.012(3) -0.033(4) _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 O1 1.931(3) . ? Fe1 O3 2.317(3) . ? Fe1 N1 2.130(4) . ? Fe1 N3 2.129(4) . ? Fe1 N5 2.186(4) . ? O1 C46 1.337(6) . ? O2 H3 0.8400 . ? O2 C49 1.371(6) . ? O3 C51 1.383(6) . ? O3 C52 1.423(6) . ? N1 C3 1.329(6) . ? N2 N1 1.370(5) . ? N2 C1 1.378(6) . ? N2 B1 1.532(6) . ? N3 C9 1.348(6) . ? N4 N3 1.359(5) . ? N4 C7 1.359(6) . ? N4 B1 1.558(6) . ? N5 C6 1.332(6) . ? N6 N5 1.371(5) . ? N6 C4 1.365(6) . ? N6 B1 1.541(6) . ? C1 C2 1.393(7) . ? C1 C10 1.469(6) . ? C2 H2 0.9500 . ? C2 C3 1.406(6) . ? C3 C16 1.467(6) . ? C4 C5 1.380(6) . ? C4 C22 1.464(6) . ? C5 H5 0.9500 . ? C5 C6 1.397(7) . ? C6 C28 1.478(6) . ? C7 C8 1.398(6) . ? C7 C34 1.455(6) . ? C8 H8 0.9500 . ? C8 C9 1.390(6) . ? C9 C40 1.478(6) . ? C10 C11 1.384(7) . ? C10 C15 1.405(6) . ? C11 H11 0.9500 . ? C11 C12 1.371(7) . ? C12 H12 0.9500 . ? C12 C13 1.403(7) . ? C13 H13 0.9500 . ? C13 C14 1.373(7) . ? C14 H14 0.9500 . ? C14 C15 1.373(7) . ? C15 H15 0.9500 . ? C16 C17 1.399(7) . ? C16 C21 1.384(7) . ? C17 H17 0.9500 . ? C17 C18 1.377(7) . ? C18 H18 0.9500 . ? C18 C19 1.402(8) . ? C19 H19 0.9500 . ? C19 C20 1.391(8) . ? C20 H20 0.9500 . ? C20 C21 1.383(7) . ? C21 H21 0.9500 . ? C22 C23 1.400(7) . ? C22 C27 1.395(7) . ? C23 H23 0.9500 . ? C23 C24 1.398(7) . ? C24 H24 0.9500 . ? C24 C25 1.382(8) . ? C25 H25 0.9500 . ? C25 C26 1.390(8) . ? C26 H26 0.9500 . ? C26 C27 1.389(7) . ? C27 H27 0.9500 . ? C28 C29 1.397(7) . ? C28 C33 1.383(7) . ? C29 H29 0.9500 . ? C29 C30 1.378(7) . ? C30 H30 0.9500 . ? C30 C31 1.392(8) . ? C31 H31 0.9500 . ? C31 C32 1.376(8) . ? C32 H32 0.9500 . ? C32 C33 1.388(7) . ? C33 H33 0.9500 . ? C34 C35 1.401(6) . ? C34 C39 1.391(6) . ? C35 H35 0.9500 . ? C35 C36 1.385(6) . ? C36 H36 0.9500 . ? C36 C37 1.384(7) . ? C37 H37 0.9500 . ? C37 C38 1.375(7) . ? C38 H38 0.9500 . ? C38 C39 1.395(6) . ? C39 H39 0.9500 . ? C40 C41 1.396(7) . ? C40 C45 1.377(7) . ? C41 H41 0.9500 . ? C41 C42 1.388(7) . ? C42 H42 0.9500 . ? C42 C43 1.392(8) . ? C43 H43 0.9500 . ? C43 C44 1.366(8) . ? C44 H44 0.9500 . ? C44 C45 1.405(7) . ? C45 H45 0.9500 . ? C46 C47 1.376(7) . ? C46 C51 1.417(7) . ? C47 H51 0.9500 . ? C48 C47 1.391(8) . ? C48 H50 0.9500 . ? C49 C48 1.367(8) . ? C50 C49 1.412(7) . ? C50 H48 0.9500 . ? C51 C50 1.373(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? B1 H1 1.0000 . ? S1 O4 1.439(5) . ? S1 O5 1.432(4) . ? S1 O6 1.441(5) . ? S1 C53 1.770(8) . ? F1 C53 1.345(9) . ? F2 C53 1.341(8) . ? F3 C53 1.350(9) . ? N7 H7 0.9300 . ? N7 C54 1.488(8) . ? N7 C56 1.501(8) . ? N7 C58 1.499(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.511(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C56 C57 1.493(9) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C58 C59 1.485(10) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 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 O1 Fe1 O3 75.70(13) . . ? O1 Fe1 N1 128.45(15) . . ? O1 Fe1 N3 129.98(15) . . ? O1 Fe1 N5 115.55(14) . . ? N1 Fe1 O3 85.29(14) . . ? N1 Fe1 N5 89.37(15) . . ? N3 Fe1 O3 84.49(14) . . ? N3 Fe1 N1 94.15(14) . . ? N3 Fe1 N5 85.58(15) . . ? N5 Fe1 O3 168.35(14) . . ? C46 O1 Fe1 121.6(3) . . ? C49 O2 H3 109.5 . . ? C51 O3 Fe1 109.9(3) . . ? C51 O3 C52 118.7(4) . . ? C52 O3 Fe1 131.4(3) . . ? N2 N1 Fe1 113.4(3) . . ? C3 N1 Fe1 138.1(3) . . ? C3 N1 N2 108.5(4) . . ? N1 N2 C1 108.9(4) . . ? N1 N2 B1 119.7(4) . . ? C1 N2 B1 129.6(4) . . ? N4 N3 Fe1 110.2(3) . . ? C9 N3 Fe1 140.6(3) . . ? C9 N3 N4 107.2(4) . . ? N3 N4 C7 110.3(4) . . ? N3 N4 B1 120.5(4) . . ? C7 N4 B1 127.2(4) . . ? N6 N5 Fe1 110.6(3) . . ? C6 N5 Fe1 142.8(3) . . ? C6 N5 N6 106.5(4) . . ? N5 N6 B1 121.7(4) . . ? C4 N6 N5 109.9(4) . . ? C4 N6 B1 127.0(4) . . ? N2 C1 C2 107.1(4) . . ? N2 C1 C10 123.4(4) . . ? C2 C1 C10 129.5(4) . . ? C1 C2 H2 126.9 . . ? C1 C2 C3 106.2(4) . . ? C3 C2 H2 126.9 . . ? N1 C3 C2 109.3(4) . . ? N1 C3 C16 123.5(4) . . ? C2 C3 C16 127.2(5) . . ? N6 C4 C5 107.3(4) . . ? N6 C4 C22 124.8(4) . . ? C5 C4 C22 127.9(4) . . ? C4 C5 H5 127.1 . . ? C4 C5 C6 105.8(4) . . ? C6 C5 H5 127.1 . . ? N5 C6 C5 110.4(4) . . ? N5 C6 C28 124.0(4) . . ? C5 C6 C28 125.5(4) . . ? N4 C7 C8 106.9(4) . . ? N4 C7 C34 123.8(4) . . ? C8 C7 C34 129.3(4) . . ? C7 C8 H8 127.0 . . ? C9 C8 C7 106.1(4) . . ? C9 C8 H8 127.0 . . ? N3 C9 C8 109.6(4) . . ? N3 C9 C40 122.9(4) . . ? C8 C9 C40 127.3(4) . . ? C11 C10 C1 123.0(4) . . ? C11 C10 C15 118.6(4) . . ? C15 C10 C1 118.4(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C11 C12 H12 120.2 . . ? C11 C12 C13 119.6(5) . . ? C13 C12 H12 120.2 . . ? C12 C13 H13 120.4 . . ? C14 C13 C12 119.1(5) . . ? C14 C13 H13 120.4 . . ? C13 C14 H14 119.3 . . ? C13 C14 C15 121.4(5) . . ? C15 C14 H14 119.3 . . ? C10 C15 H15 120.1 . . ? C14 C15 C10 119.8(5) . . ? C14 C15 H15 120.1 . . ? C17 C16 C3 119.8(4) . . ? C21 C16 C3 121.8(5) . . ? C21 C16 C17 118.5(5) . . ? C16 C17 H17 119.4 . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.8(5) . . ? C19 C18 H18 120.1 . . ? C18 C19 H19 120.5 . . ? C20 C19 C18 119.0(5) . . ? C20 C19 H19 120.5 . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.8 . . ? C16 C21 H21 119.5 . . ? C20 C21 C16 120.9(5) . . ? C20 C21 H21 119.5 . . ? C23 C22 C4 118.2(4) . . ? C27 C22 C4 122.6(5) . . ? C27 C22 C23 119.2(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.1(5) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.2(5) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 120.1 . . ? C24 C25 C26 119.8(5) . . ? C26 C25 H25 120.1 . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26 119.8 . . ? C22 C27 H27 119.9 . . ? C26 C27 C22 120.2(5) . . ? C26 C27 H27 119.9 . . ? C29 C28 C6 121.5(4) . . ? C33 C28 C6 119.3(4) . . ? C33 C28 C29 119.2(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 C28 119.7(5) . . ? C30 C29 H29 120.2 . . ? C29 C30 H30 119.5 . . ? C29 C30 C31 120.9(5) . . ? C31 C30 H30 119.5 . . ? C30 C31 H31 120.3 . . ? C32 C31 C30 119.4(5) . . ? C32 C31 H31 120.3 . . ? C31 C32 H32 120.0 . . ? C31 C32 C33 119.9(5) . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 120.9(5) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C7 121.1(4) . . ? C39 C34 C7 119.7(4) . . ? C39 C34 C35 119.2(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 C34 120.6(5) . . ? C36 C35 H35 119.7 . . ? C35 C36 H36 120.2 . . ? C37 C36 C35 119.7(5) . . ? C37 C36 H36 120.2 . . ? C36 C37 H37 119.9 . . ? C38 C37 C36 120.3(5) . . ? C38 C37 H37 119.9 . . ? C37 C38 H38 119.7 . . ? C37 C38 C39 120.6(5) . . ? C39 C38 H38 119.7 . . ? C34 C39 C38 119.6(4) . . ? C34 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C41 C40 C9 118.5(4) . . ? C45 C40 C9 122.4(4) . . ? C45 C40 C41 119.0(4) . . ? C40 C41 H41 119.7 . . ? C42 C41 C40 120.7(5) . . ? C42 C41 H41 119.7 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 119.9(5) . . ? C43 C42 H42 120.0 . . ? C42 C43 H43 120.3 . . ? C44 C43 C42 119.5(5) . . ? C44 C43 H43 120.3 . . ? C43 C44 H44 119.6 . . ? C43 C44 C45 120.8(5) . . ? C45 C44 H44 119.6 . . ? C40 C45 C44 120.1(5) . . ? C40 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? O1 C46 C47 123.8(5) . . ? O1 C46 C51 119.6(4) . . ? C47 C46 C51 116.6(5) . . ? C46 C47 H51 119.2 . . ? C46 C47 C48 121.5(5) . . ? C48 C47 H51 119.2 . . ? C47 C48 H50 119.5 . . ? C49 C48 C47 120.9(5) . . ? C49 C48 H50 119.5 . . ? O2 C49 C50 116.4(5) . . ? C48 C49 O2 124.0(5) . . ? C48 C49 C50 119.6(5) . . ? C49 C50 H48 120.8 . . ? C51 C50 C49 118.3(5) . . ? C51 C50 H48 120.8 . . ? O3 C51 C46 113.2(4) . . ? C50 C51 O3 123.9(5) . . ? C50 C51 C46 122.9(5) . . ? O3 C52 H52A 109.5 . . ? O3 C52 H52B 109.5 . . ? O3 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N2 B1 N4 110.3(4) . . ? N2 B1 N6 109.8(4) . . ? N2 B1 H1 109.6 . . ? N4 B1 H1 109.6 . . ? N6 B1 N4 108.0(4) . . ? N6 B1 H1 109.6 . . ? O4 S1 O6 114.1(3) . . ? O4 S1 C53 104.6(3) . . ? O5 S1 O4 115.2(3) . . ? O5 S1 O6 114.6(3) . . ? O5 S1 C53 103.3(3) . . ? O6 S1 C53 102.9(4) . . ? F1 C53 S1 112.3(6) . . ? F1 C53 F3 105.5(6) . . ? F2 C53 S1 113.0(5) . . ? F2 C53 F1 107.1(6) . . ? F2 C53 F3 106.5(6) . . ? F3 C53 S1 111.9(5) . . ? C54 N7 H7 104.8 . . ? C54 N7 C56 112.6(5) . . ? C54 N7 C58 111.4(5) . . ? C56 N7 H7 104.8 . . ? C58 N7 H7 104.8 . . ? C58 N7 C56 117.0(5) . . ? N7 C54 H54A 109.2 . . ? N7 C54 H54B 109.2 . . ? N7 C54 C55 111.9(5) . . ? H54A C54 H54B 107.9 . . ? C55 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N7 C56 H56A 109.0 . . ? N7 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? C57 C56 N7 113.0(6) . . ? C57 C56 H56A 109.0 . . ? C57 C56 H56B 109.0 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N7 C58 H58A 108.8 . . ? N7 C58 H58B 108.8 . . ? H58A C58 H58B 107.7 . . ? C59 C58 N7 113.9(6) . . ? C59 C58 H58A 108.8 . . ? C59 C58 H58B 108.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H3 O4 0.84 1.95 2.782(6) 169.5 . N7 H7 O6 0.93 1.98 2.894(7) 168.5 2_656 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 179.2(4) . . . . ? Fe1 O1 C46 C51 0.3(6) . . . . ? Fe1 O3 C51 C46 0.6(5) . . . . ? Fe1 O3 C51 C50 179.8(4) . . . . ? Fe1 N1 C3 C2 -179.8(4) . . . . ? Fe1 N1 C3 C16 0.8(8) . . . . ? Fe1 N3 C9 C8 -160.4(4) . . . . ? Fe1 N3 C9 C40 24.6(8) . . . . ? Fe1 N5 C6 C5 -176.7(4) . . . . ? Fe1 N5 C6 C28 5.4(8) . . . . ? O1 Fe1 O3 C51 -0.3(3) . . . . ? O1 Fe1 O3 C52 178.1(5) . . . . ? O1 Fe1 N1 N2 -160.5(3) . . . . ? O1 Fe1 N1 C3 19.4(6) . . . . ? O1 Fe1 N3 N4 -175.7(3) . . . . ? O1 Fe1 N3 C9 -15.3(6) . . . . ? O1 Fe1 N5 N6 -174.2(3) . . . . ? O1 Fe1 N5 C6 1.3(6) . . . . ? O1 C46 C47 C48 -178.3(5) . . . . ? O1 C46 C51 O3 -0.6(7) . . . . ? O1 C46 C51 C50 -179.8(5) . . . . ? O2 C49 C48 C47 -179.8(6) . . . . ? O3 Fe1 O1 C46 0.1(4) . . . . ? O3 Fe1 N1 N2 132.0(3) . . . . ? O3 Fe1 N1 C3 -48.2(5) . . . . ? O3 Fe1 N3 N4 -109.6(3) . . . . ? O3 Fe1 N3 C9 50.8(5) . . . . ? O3 Fe1 N5 N6 -10.0(9) . . . . ? O3 Fe1 N5 C6 165.5(6) . . . . ? O3 C51 C50 C49 178.7(5) . . . . ? N1 Fe1 O1 C46 -71.8(4) . . . . ? N1 Fe1 O3 C51 131.3(3) . . . . ? N1 Fe1 O3 C52 -50.2(5) . . . . ? N1 Fe1 N3 N4 -24.7(3) . . . . ? N1 Fe1 N3 C9 135.7(5) . . . . ? N1 Fe1 N5 N6 52.6(3) . . . . ? N1 Fe1 N5 C6 -131.8(5) . . . . ? N1 N2 C1 C2 1.1(5) . . . . ? N1 N2 C1 C10 -177.8(4) . . . . ? N1 N2 B1 N4 -47.9(5) . . . . ? N1 N2 B1 N6 71.0(5) . . . . ? N1 C3 C16 C17 142.4(5) . . . . ? N1 C3 C16 C21 -35.8(7) . . . . ? N2 N1 C3 C2 0.0(5) . . . . ? N2 N1 C3 C16 -179.3(4) . . . . ? N2 C1 C2 C3 -1.0(5) . . . . ? N2 C1 C10 C11 39.2(7) . . . . ? N2 C1 C10 C15 -142.5(5) . . . . ? N3 Fe1 O1 C46 70.0(4) . . . . ? N3 Fe1 O3 C51 -134.0(3) . . . . ? N3 Fe1 O3 C52 44.4(5) . . . . ? N3 Fe1 N1 N2 47.9(3) . . . . ? N3 Fe1 N1 C3 -132.3(5) . . . . ? N3 Fe1 N5 N6 -41.6(3) . . . . ? N3 Fe1 N5 C6 134.0(5) . . . . ? N3 N4 C7 C8 1.5(5) . . . . ? N3 N4 C7 C34 -178.1(4) . . . . ? N3 N4 B1 N2 78.9(5) . . . . ? N3 N4 B1 N6 -41.1(5) . . . . ? N3 C9 C40 C41 155.4(5) . . . . ? N3 C9 C40 C45 -20.1(8) . . . . ? N4 N3 C9 C8 0.3(5) . . . . ? N4 N3 C9 C40 -174.6(4) . . . . ? N4 C7 C8 C9 -1.3(5) . . . . ? N4 C7 C34 C35 46.7(7) . . . . ? N4 C7 C34 C39 -135.1(5) . . . . ? N5 Fe1 O1 C46 176.8(3) . . . . ? N5 Fe1 O3 C51 -165.7(6) . . . . ? N5 Fe1 O3 C52 12.8(9) . . . . ? N5 Fe1 N1 N2 -37.7(3) . . . . ? N5 Fe1 N1 C3 142.2(5) . . . . ? N5 Fe1 N3 N4 64.3(3) . . . . ? N5 Fe1 N3 C9 -135.3(5) . . . . ? N5 N6 C4 C5 0.5(5) . . . . ? N5 N6 C4 C22 -178.9(4) . . . . ? N5 N6 B1 N2 -50.8(5) . . . . ? N5 N6 B1 N4 69.6(5) . . . . ? N5 C6 C28 C29 -27.2(7) . . . . ? N5 C6 C28 C33 150.6(5) . . . . ? N6 N5 C6 C5 -1.0(5) . . . . ? N6 N5 C6 C28 -178.9(4) . . . . ? N6 C4 C5 C6 -1.1(5) . . . . ? N6 C4 C22 C23 -132.3(5) . . . . ? N6 C4 C22 C27 48.2(7) . . . . ? C1 N2 N1 Fe1 179.2(3) . . . . ? C1 N2 N1 C3 -0.7(5) . . . . ? C1 N2 B1 N4 115.0(5) . . . . ? C1 N2 B1 N6 -126.1(5) . . . . ? C1 C2 C3 N1 0.6(6) . . . . ? C1 C2 C3 C16 179.9(5) . . . . ? C1 C10 C11 C12 -179.9(5) . . . . ? C1 C10 C15 C14 179.7(5) . . . . ? C2 C1 C10 C11 -139.4(6) . . . . ? C2 C1 C10 C15 38.9(8) . . . . ? C2 C3 C16 C17 -36.8(8) . . . . ? C2 C3 C16 C21 145.0(5) . . . . ? C3 C16 C17 C18 -177.5(5) . . . . ? C3 C16 C21 C20 176.8(5) . . . . ? C4 N6 N5 Fe1 177.5(3) . . . . ? C4 N6 N5 C6 0.3(5) . . . . ? C4 N6 B1 N2 114.7(5) . . . . ? C4 N6 B1 N4 -125.0(5) . . . . ? C4 C5 C6 N5 1.3(5) . . . . ? C4 C5 C6 C28 179.2(4) . . . . ? C4 C22 C23 C24 -178.9(5) . . . . ? C4 C22 C27 C26 179.1(5) . . . . ? C5 C4 C22 C23 48.4(7) . . . . ? C5 C4 C22 C27 -131.1(6) . . . . ? C5 C6 C28 C29 155.2(5) . . . . ? C5 C6 C28 C33 -27.0(7) . . . . ? C6 C28 C29 C30 176.4(5) . . . . ? C6 C28 C33 C32 -176.8(5) . . . . ? C7 N4 N3 Fe1 165.9(3) . . . . ? C7 N4 N3 C9 -1.2(5) . . . . ? C7 N4 B1 N2 -118.7(5) . . . . ? C7 N4 B1 N6 121.3(5) . . . . ? C7 C8 C9 N3 0.6(6) . . . . ? C7 C8 C9 C40 175.2(5) . . . . ? C7 C34 C35 C36 178.6(5) . . . . ? C7 C34 C39 C38 -178.4(5) . . . . ? C8 C7 C34 C35 -132.8(5) . . . . ? C8 C7 C34 C39 45.5(8) . . . . ? C8 C9 C40 C41 -18.6(8) . . . . ? C8 C9 C40 C45 165.9(5) . . . . ? C9 C40 C41 C42 -175.7(5) . . . . ? C9 C40 C45 C44 175.1(5) . . . . ? C10 C1 C2 C3 177.7(5) . . . . ? C10 C11 C12 C13 -0.4(8) . . . . ? C11 C10 C15 C14 -1.9(8) . . . . ? C11 C12 C13 C14 -0.9(8) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 C10 0.6(8) . . . . ? C15 C10 C11 C12 1.8(8) . . . . ? C16 C17 C18 C19 0.7(8) . . . . ? C17 C16 C21 C20 -1.4(8) . . . . ? C17 C18 C19 C20 -1.5(8) . . . . ? C18 C19 C20 C21 0.9(8) . . . . ? C19 C20 C21 C16 0.6(8) . . . . ? C21 C16 C17 C18 0.8(8) . . . . ? C22 C4 C5 C6 178.3(5) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C23 C22 C27 C26 -0.4(7) . . . . ? C23 C24 C25 C26 -0.5(8) . . . . ? C24 C25 C26 C27 0.7(8) . . . . ? C25 C26 C27 C22 -0.3(8) . . . . ? C27 C22 C23 C24 0.6(7) . . . . ? C28 C29 C30 C31 1.3(8) . . . . ? C29 C28 C33 C32 1.1(8) . . . . ? C29 C30 C31 C32 -0.7(8) . . . . ? C30 C31 C32 C33 0.4(8) . . . . ? C31 C32 C33 C28 -0.6(8) . . . . ? C33 C28 C29 C30 -1.5(7) . . . . ? C34 C7 C8 C9 178.3(5) . . . . ? C34 C35 C36 C37 -1.2(8) . . . . ? C35 C34 C39 C38 -0.1(7) . . . . ? C35 C36 C37 C38 1.7(8) . . . . ? C36 C37 C38 C39 -1.4(8) . . . . ? C37 C38 C39 C34 0.6(8) . . . . ? C39 C34 C35 C36 0.4(7) . . . . ? C40 C41 C42 C43 0.4(8) . . . . ? C41 C40 C45 C44 -0.4(8) . . . . ? C41 C42 C43 C44 -0.5(9) . . . . ? C42 C43 C44 C45 0.1(9) . . . . ? C43 C44 C45 C40 0.4(8) . . . . ? C45 C40 C41 C42 0.0(8) . . . . ? C46 C51 C50 C49 -2.2(8) . . . . ? C47 C46 C51 O3 -179.6(5) . . . . ? C47 C46 C51 C50 1.2(8) . . . . ? C49 C48 C47 C46 -1.6(9) . . . . ? C50 C49 C48 C47 0.5(9) . . . . ? C51 C46 C47 C48 0.7(8) . . . . ? C51 C50 C49 O2 -178.4(5) . . . . ? C51 C50 C49 C48 1.3(8) . . . . ? C52 O3 C51 C46 -178.1(5) . . . . ? C52 O3 C51 C50 1.1(8) . . . . ? B1 N2 N1 Fe1 -14.6(5) . . . . ? B1 N2 N1 C3 165.5(4) . . . . ? B1 N2 C1 C2 -163.3(4) . . . . ? B1 N2 C1 C10 17.9(7) . . . . ? B1 N4 N3 Fe1 -28.9(5) . . . . ? B1 N4 N3 C9 164.0(4) . . . . ? B1 N4 C7 C8 -162.4(4) . . . . ? B1 N4 C7 C34 18.0(7) . . . . ? B1 N6 N5 Fe1 -14.8(5) . . . . ? B1 N6 N5 C6 168.0(4) . . . . ? B1 N6 C4 C5 -166.3(4) . . . . ? B1 N6 C4 C22 14.3(8) . . . . ? O4 S1 C53 F1 61.0(6) . . . . ? O4 S1 C53 F2 -60.3(7) . . . . ? O4 S1 C53 F3 179.4(5) . . . . ? O5 S1 C53 F1 -60.0(6) . . . . ? O5 S1 C53 F2 178.7(6) . . . . ? O5 S1 C53 F3 58.5(6) . . . . ? O6 S1 C53 F1 -179.5(5) . . . . ? O6 S1 C53 F2 59.1(6) . . . . ? O6 S1 C53 F3 -61.1(6) . . . . ? C54 N7 C56 C57 -64.0(8) . . . . ? C54 N7 C58 C59 -169.0(6) . . . . ? C56 N7 C54 C55 -149.7(6) . . . . ? C56 N7 C58 C59 59.5(8) . . . . ? C58 N7 C54 C55 76.6(7) . . . . ? C58 N7 C56 C57 67.0(8) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 6 -3 0.0858 -0.0029 5.9971 -2.6719 0.4886 0.8239 -0.1461 1 -6 3 0.1178 1.0032 -5.9975 2.9223 -0.3663 -0.9287 0.1384 1 1 19 0.0174 1.0045 1.0043 18.6270 0.2403 -0.0677 0.9883 -1 -1 -19 0.0057 -1.0045 -1.0043 -18.6270 -0.2403 0.0677 -0.9883 6 2 -1 0.2819 6.0001 1.9962 -0.7207 0.8945 -0.3469 -0.1670 -6 -2 2 0.2286 -5.9999 -1.9959 1.7201 -0.8925 0.3416 0.2212 #==END data_Complex1F _database_code_depnum_ccdc_archive 'CCDC 890622' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-21 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C68 H55 B Fe N8 O2' _chemical_formula_sum 'C68 H55 B Fe N8 O2' _chemical_formula_weight 1082.86 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C68 H55 N8 O2 B' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 17.8034(7) _cell_length_b 22.3235(10) _cell_length_c 13.6123(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.746(4) _cell_angle_gamma 90.00 _cell_volume 5331.9(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20222 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 29.5917 _cell_measurement_theta_min 3.4205 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2264 _exptl_crystal_size_max 0.5848 _exptl_crystal_size_mid 0.2597 _exptl_crystal_size_min 0.0546 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 62124 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 29.66 _diffrn_reflns_theta_min 3.43 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.903 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 36.00 99.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 178.0000 120.0000 126 #__ type_ start__ end____ width___ exp.time_ 2 omega -2.00 36.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 37.0000 30.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega -18.00 84.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 57.0000 -120.0000 204 #__ type_ start__ end____ width___ exp.time_ 4 omega -62.00 41.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 -57.0000 -90.0000 206 #__ type_ start__ end____ width___ exp.time_ 5 omega -18.00 37.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 57.0000 60.0000 110 #__ type_ start__ end____ width___ exp.time_ 6 omega -20.00 54.00 0.5000 30.0000 omega____ theta____ kappa____ phi______ frames - 11.6697 -99.0000 -150.0000 148 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0349414000 _diffrn_orient_matrix_UB_12 -0.0149597000 _diffrn_orient_matrix_UB_13 -0.0168936000 _diffrn_orient_matrix_UB_21 0.0202852000 _diffrn_orient_matrix_UB_22 -0.0261687000 _diffrn_orient_matrix_UB_23 -0.0092267000 _diffrn_orient_matrix_UB_31 -0.0008314000 _diffrn_orient_matrix_UB_32 -0.0100412000 _diffrn_orient_matrix_UB_33 0.0492653000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_number_gt 11161 _reflns_number_total 13600 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.339 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 731 _refine_ls_number_reflns 13600 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0414 _refine_ls_restrained_S_all 1.058 _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^)+(0.0331P)^2^+5.1360P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.1083 _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 0.247303(13) 0.449679(11) 0.271694(17) 0.01579(6) Uani 1 1 d . . . O1 O 0.33946(7) 0.49277(6) 0.30765(10) 0.0241(3) Uani 1 1 d . . . O2 O 0.54158(8) 0.66106(7) 0.21023(11) 0.0296(3) Uani 1 1 d . . . H2 H 0.5180(16) 0.6876(14) 0.172(2) 0.058(9) Uiso 1 1 d . . . N1 N 0.16731(7) 0.44231(6) 0.14138(10) 0.0157(3) Uani 1 1 d . . . N2 N 0.09386(7) 0.42807(6) 0.15088(10) 0.0157(3) Uani 1 1 d . . . N3 N 0.19402(8) 0.38536(6) 0.34724(10) 0.0171(3) Uani 1 1 d . . . N4 N 0.11582(8) 0.38358(6) 0.32748(10) 0.0165(3) Uani 1 1 d . . . N5 N 0.16168(7) 0.51322(6) 0.32436(10) 0.0169(3) Uani 1 1 d . . . N6 N 0.08759(7) 0.49360(6) 0.29957(10) 0.0163(3) Uani 1 1 d . . . N7 N 0.31645(8) 0.37143(7) 0.21511(11) 0.0193(3) Uani 1 1 d . . . N8 N 0.38885(8) 0.38972(7) 0.21407(11) 0.0199(3) Uani 1 1 d . . . H7 H 0.3998(13) 0.4279(11) 0.2307(17) 0.034(6) Uiso 1 1 d . . . C1 C 0.09121(10) 0.33362(8) 0.37027(12) 0.0191(3) Uani 1 1 d . . . C2 C 0.15453(10) 0.30328(8) 0.41831(13) 0.0223(4) Uani 1 1 d . . . H2A H 0.1551 0.2670 0.4548 0.027 Uiso 1 1 calc R . . C3 C 0.21768(10) 0.33679(8) 0.40243(12) 0.0192(3) Uani 1 1 d . . . C4 C 0.03901(9) 0.53425(8) 0.32974(12) 0.0174(3) Uani 1 1 d . . . C5 C 0.08232(9) 0.58132(8) 0.37368(13) 0.0193(3) Uani 1 1 d . . . H5 H 0.0644 0.6167 0.4008 0.023 Uiso 1 1 calc R . . C6 C 0.15829(9) 0.56615(8) 0.37003(12) 0.0183(3) Uani 1 1 d . . . C7 C 0.05437(9) 0.41157(7) 0.06025(12) 0.0171(3) Uani 1 1 d . . . C8 C 0.10339(10) 0.41514(8) -0.00845(12) 0.0189(3) Uani 1 1 d . . . H8 H 0.0920 0.4064 -0.0777 0.023 Uiso 1 1 calc R . . C9 C 0.17314(9) 0.43431(7) 0.04522(12) 0.0172(3) Uani 1 1 d . . . C10 C 0.01055(10) 0.31558(8) 0.36342(13) 0.0209(3) Uani 1 1 d . . . C11 C -0.00791(11) 0.25537(9) 0.34361(15) 0.0281(4) Uani 1 1 d . . . H11 H 0.0309 0.2278 0.3344 0.034 Uiso 1 1 calc R . . C12 C -0.08258(12) 0.23565(10) 0.33730(17) 0.0356(5) Uani 1 1 d . . . H12 H -0.0946 0.1947 0.3237 0.043 Uiso 1 1 calc R . . C13 C -0.13950(12) 0.27553(10) 0.35080(17) 0.0356(5) Uani 1 1 d . . . H13 H -0.1906 0.2620 0.3459 0.043 Uiso 1 1 calc R . . C14 C -0.12198(11) 0.33520(9) 0.37150(15) 0.0289(4) Uani 1 1 d . . . H14 H -0.1610 0.3625 0.3813 0.035 Uiso 1 1 calc R . . C15 C -0.04726(10) 0.35509(9) 0.37787(13) 0.0231(4) Uani 1 1 d . . . H15 H -0.0355 0.3960 0.3922 0.028 Uiso 1 1 calc R . . C16 C 0.29935(10) 0.32350(9) 0.43431(13) 0.0224(4) Uani 1 1 d . . . C17 C 0.32331(11) 0.26400(9) 0.44769(14) 0.0268(4) Uani 1 1 d . . . H17 H 0.2866 0.2327 0.4406 0.032 Uiso 1 1 calc R . . C18 C 0.40028(12) 0.25011(10) 0.47123(14) 0.0326(5) Uani 1 1 d . . . H18 H 0.4159 0.2095 0.4794 0.039 Uiso 1 1 calc R . . C19 C 0.45435(11) 0.29521(11) 0.48278(15) 0.0350(5) Uani 1 1 d . . . H19 H 0.5070 0.2856 0.4987 0.042 Uiso 1 1 calc R . . C20 C 0.43155(11) 0.35415(11) 0.47110(15) 0.0334(5) Uani 1 1 d . . . H20 H 0.4686 0.3852 0.4792 0.040 Uiso 1 1 calc R . . C21 C 0.35456(11) 0.36839(9) 0.44749(14) 0.0269(4) Uani 1 1 d . . . H21 H 0.3394 0.4092 0.4403 0.032 Uiso 1 1 calc R . . C22 C -0.04392(9) 0.52426(7) 0.32420(13) 0.0177(3) Uani 1 1 d . . . C23 C -0.07515(10) 0.53545(8) 0.40995(13) 0.0206(3) Uani 1 1 d . . . H23 H -0.0436 0.5508 0.4678 0.025 Uiso 1 1 calc R . . C24 C -0.15191(10) 0.52441(9) 0.41152(14) 0.0249(4) Uani 1 1 d . . . H24 H -0.1726 0.5321 0.4702 0.030 Uiso 1 1 calc R . . C25 C -0.19799(10) 0.50214(9) 0.32690(15) 0.0270(4) Uani 1 1 d . . . H25 H -0.2500 0.4934 0.3284 0.032 Uiso 1 1 calc R . . C26 C -0.16852(10) 0.49261(8) 0.24000(14) 0.0242(4) Uani 1 1 d . . . H26 H -0.2007 0.4785 0.1817 0.029 Uiso 1 1 calc R . . C27 C -0.09180(9) 0.50372(8) 0.23852(13) 0.0204(3) Uani 1 1 d . . . H27 H -0.0718 0.4973 0.1790 0.024 Uiso 1 1 calc R . . C28 C 0.22605(9) 0.59923(8) 0.41970(13) 0.0200(3) Uani 1 1 d . . . C29 C 0.22444(11) 0.66167(9) 0.42352(15) 0.0264(4) Uani 1 1 d . . . H29 H 0.1826 0.6829 0.3867 0.032 Uiso 1 1 calc R . . C30 C 0.28364(12) 0.69310(9) 0.48094(16) 0.0333(5) Uani 1 1 d . . . H30 H 0.2820 0.7356 0.4836 0.040 Uiso 1 1 calc R . . C31 C 0.34511(11) 0.66245(10) 0.53429(16) 0.0335(5) Uani 1 1 d . . . H31 H 0.3851 0.6839 0.5744 0.040 Uiso 1 1 calc R . . C32 C 0.34812(11) 0.60074(10) 0.52911(15) 0.0297(4) Uani 1 1 d . . . H32 H 0.3909 0.5799 0.5642 0.036 Uiso 1 1 calc R . . C33 C 0.28869(10) 0.56907(9) 0.47263(13) 0.0230(4) Uani 1 1 d . . . H33 H 0.2908 0.5266 0.4701 0.028 Uiso 1 1 calc R . . C34 C -0.02740(9) 0.39586(8) 0.03944(13) 0.0182(3) Uani 1 1 d . . . C35 C -0.07193(10) 0.42085(8) -0.04526(13) 0.0222(4) Uani 1 1 d . . . H35 H -0.0493 0.4473 -0.0865 0.027 Uiso 1 1 calc R . . C36 C -0.14902(10) 0.40725(9) -0.06939(15) 0.0270(4) Uani 1 1 d . . . H36 H -0.1788 0.4242 -0.1272 0.032 Uiso 1 1 calc R . . C37 C -0.18240(10) 0.36913(9) -0.00942(15) 0.0295(4) Uani 1 1 d . . . H37 H -0.2354 0.3606 -0.0251 0.035 Uiso 1 1 calc R . . C38 C -0.13859(10) 0.34325(9) 0.07368(14) 0.0257(4) Uani 1 1 d . . . H38 H -0.1615 0.3165 0.1142 0.031 Uiso 1 1 calc R . . C39 C -0.06123(10) 0.35619(8) 0.09808(13) 0.0205(3) Uani 1 1 d . . . H39 H -0.0314 0.3380 0.1547 0.025 Uiso 1 1 calc R . . C40 C 0.24702(9) 0.44189(8) 0.01193(12) 0.0186(3) Uani 1 1 d . . . C41 C 0.26795(11) 0.40194(9) -0.05731(14) 0.0276(4) Uani 1 1 d . . . H41 H 0.2331 0.3721 -0.0862 0.033 Uiso 1 1 calc R . . C42 C 0.33949(12) 0.40570(10) -0.08407(16) 0.0354(5) Uani 1 1 d . . . H42 H 0.3536 0.3781 -0.1309 0.042 Uiso 1 1 calc R . . C43 C 0.39056(11) 0.44933(10) -0.04304(16) 0.0321(4) Uani 1 1 d . . . H43 H 0.4399 0.4512 -0.0608 0.039 Uiso 1 1 calc R . . C44 C 0.36975(10) 0.49026(9) 0.02393(14) 0.0265(4) Uani 1 1 d . . . H44 H 0.4043 0.5207 0.0513 0.032 Uiso 1 1 calc R . . C45 C 0.29808(10) 0.48647(8) 0.05084(13) 0.0210(3) Uani 1 1 d . . . H45 H 0.2837 0.5147 0.0965 0.025 Uiso 1 1 calc R . . C46 C 0.38568(9) 0.53659(8) 0.28712(13) 0.0199(3) Uani 1 1 d . . . C47 C 0.35966(10) 0.58810(8) 0.23460(13) 0.0222(4) Uani 1 1 d . . . H62 H 0.3063 0.5948 0.2176 0.027 Uiso 1 1 calc R . . C48 C 0.40970(10) 0.63013(8) 0.20630(14) 0.0225(4) Uani 1 1 d . . . C49 C 0.48789(10) 0.62124(8) 0.23533(13) 0.0212(3) Uani 1 1 d . . . C50 C 0.51625(9) 0.57180(8) 0.29202(13) 0.0204(3) Uani 1 1 d . . . C51 C 0.46457(9) 0.53017(8) 0.31763(13) 0.0198(3) Uani 1 1 d . . . H66 H 0.4833 0.4965 0.3569 0.024 Uiso 1 1 calc R . . C52 C 0.38020(12) 0.68278(9) 0.14128(17) 0.0344(5) Uani 1 1 d . . . H67A H 0.3856 0.6744 0.0722 0.052 Uiso 1 1 calc R . . H67B H 0.4095 0.7187 0.1646 0.052 Uiso 1 1 calc R . . H67C H 0.3263 0.6894 0.1449 0.052 Uiso 1 1 calc R . . C53 C 0.60102(10) 0.56283(9) 0.32279(15) 0.0280(4) Uani 1 1 d . . . H68A H 0.6233 0.5510 0.2646 0.042 Uiso 1 1 calc R . . H68B H 0.6104 0.5314 0.3736 0.042 Uiso 1 1 calc R . . H68C H 0.6245 0.6003 0.3501 0.042 Uiso 1 1 calc R . . C54 C 0.31784(10) 0.31188(8) 0.19939(12) 0.0193(3) Uani 1 1 d . . . C55 C 0.39186(10) 0.29344(8) 0.19048(13) 0.0213(3) Uani 1 1 d . . . H47 H 0.4081 0.2537 0.1802 0.026 Uiso 1 1 calc R . . C56 C 0.43603(10) 0.34426(8) 0.19954(13) 0.0209(3) Uani 1 1 d . . . C57 C 0.51690(10) 0.35215(9) 0.19200(13) 0.0221(4) Uani 1 1 d . . . C58 C 0.56132(11) 0.30138(10) 0.18420(15) 0.0290(4) Uani 1 1 d . . . H54 H 0.5387 0.2628 0.1822 0.035 Uiso 1 1 calc R . . C59 C 0.63836(11) 0.30694(10) 0.17927(16) 0.0344(5) Uani 1 1 d . . . H53 H 0.6682 0.2721 0.1748 0.041 Uiso 1 1 calc R . . C60 C 0.67185(11) 0.36271(11) 0.18081(16) 0.0337(5) Uani 1 1 d . . . H52 H 0.7247 0.3663 0.1783 0.040 Uiso 1 1 calc R . . C61 C 0.62796(11) 0.41335(10) 0.18608(15) 0.0299(4) Uani 1 1 d . . . H51 H 0.6506 0.4519 0.1859 0.036 Uiso 1 1 calc R . . C62 C 0.55101(10) 0.40831(9) 0.19166(14) 0.0259(4) Uani 1 1 d . . . H50 H 0.5214 0.4434 0.1953 0.031 Uiso 1 1 calc R . . C63 C 0.25093(10) 0.27197(8) 0.19043(12) 0.0204(3) Uani 1 1 d . . . C64 C 0.17693(10) 0.29222(8) 0.15836(13) 0.0212(3) Uani 1 1 d . . . H56 H 0.1682 0.3334 0.1428 0.025 Uiso 1 1 calc R . . C65 C 0.11563(11) 0.25288(9) 0.14890(14) 0.0258(4) Uani 1 1 d . . . H57 H 0.0654 0.2673 0.1270 0.031 Uiso 1 1 calc R . . C66 C 0.12753(12) 0.19261(9) 0.17128(15) 0.0290(4) Uani 1 1 d . . . H58 H 0.0856 0.1658 0.1657 0.035 Uiso 1 1 calc R . . C67 C 0.20103(12) 0.17180(9) 0.20184(15) 0.0314(4) Uani 1 1 d . . . H59 H 0.2095 0.1305 0.2164 0.038 Uiso 1 1 calc R . . C68 C 0.26229(11) 0.21089(9) 0.21135(15) 0.0282(4) Uani 1 1 d . . . H60 H 0.3125 0.1961 0.2323 0.034 Uiso 1 1 calc R . . B1 B 0.07051(10) 0.43047(8) 0.25589(14) 0.0162(3) Uani 1 1 d . . . H1 H 0.0147 0.4222 0.2496 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01243(11) 0.01653(12) 0.01864(12) -0.00018(9) 0.00333(9) -0.00216(9) O1 0.0170(6) 0.0229(7) 0.0327(7) -0.0032(5) 0.0056(5) -0.0062(5) O2 0.0271(7) 0.0270(7) 0.0362(8) 0.0012(6) 0.0101(6) -0.0076(6) N1 0.0140(6) 0.0156(7) 0.0182(6) 0.0009(5) 0.0050(5) -0.0009(5) N2 0.0137(6) 0.0152(7) 0.0185(7) 0.0002(5) 0.0034(5) -0.0018(5) N3 0.0145(6) 0.0192(7) 0.0177(7) 0.0001(5) 0.0031(5) -0.0003(5) N4 0.0149(6) 0.0179(7) 0.0173(6) -0.0003(5) 0.0047(5) -0.0023(5) N5 0.0136(6) 0.0175(7) 0.0198(7) -0.0004(5) 0.0038(5) -0.0035(5) N6 0.0127(6) 0.0180(7) 0.0187(7) -0.0003(5) 0.0043(5) -0.0017(5) N7 0.0162(6) 0.0207(7) 0.0213(7) 0.0012(6) 0.0045(5) -0.0009(6) N8 0.0169(6) 0.0202(8) 0.0232(7) 0.0001(6) 0.0047(6) 0.0005(6) C1 0.0205(8) 0.0202(8) 0.0177(8) 0.0001(6) 0.0068(6) -0.0020(7) C2 0.0249(8) 0.0226(9) 0.0203(8) 0.0053(7) 0.0065(7) -0.0012(7) C3 0.0214(8) 0.0197(8) 0.0166(8) 0.0010(6) 0.0032(6) 0.0000(7) C4 0.0169(7) 0.0174(8) 0.0185(8) 0.0015(6) 0.0046(6) 0.0011(6) C5 0.0179(7) 0.0177(8) 0.0233(8) -0.0016(6) 0.0057(7) -0.0006(6) C6 0.0185(7) 0.0176(8) 0.0194(8) -0.0007(6) 0.0052(6) -0.0019(6) C7 0.0181(7) 0.0146(8) 0.0183(8) 0.0005(6) 0.0017(6) -0.0004(6) C8 0.0219(8) 0.0187(8) 0.0164(7) 0.0002(6) 0.0036(6) -0.0018(7) C9 0.0194(8) 0.0149(8) 0.0182(8) 0.0010(6) 0.0051(6) -0.0008(6) C10 0.0226(8) 0.0221(9) 0.0192(8) 0.0035(7) 0.0070(7) -0.0045(7) C11 0.0284(9) 0.0227(9) 0.0350(10) 0.0033(8) 0.0105(8) -0.0035(8) C12 0.0343(11) 0.0258(10) 0.0485(13) 0.0016(9) 0.0125(10) -0.0128(9) C13 0.0260(9) 0.0385(12) 0.0440(12) 0.0047(10) 0.0109(9) -0.0118(9) C14 0.0245(9) 0.0321(11) 0.0326(10) 0.0028(8) 0.0124(8) -0.0022(8) C15 0.0246(8) 0.0250(9) 0.0216(8) 0.0008(7) 0.0093(7) -0.0051(7) C16 0.0211(8) 0.0293(10) 0.0169(8) 0.0037(7) 0.0033(7) 0.0022(7) C17 0.0288(9) 0.0300(10) 0.0219(9) 0.0062(7) 0.0053(7) 0.0037(8) C18 0.0321(10) 0.0414(12) 0.0248(9) 0.0092(8) 0.0066(8) 0.0142(9) C19 0.0232(9) 0.0560(14) 0.0258(10) 0.0106(9) 0.0041(8) 0.0099(9) C20 0.0232(9) 0.0480(13) 0.0279(10) 0.0052(9) 0.0007(8) -0.0048(9) C21 0.0256(9) 0.0316(10) 0.0222(9) 0.0034(7) 0.0001(7) -0.0009(8) C22 0.0155(7) 0.0143(8) 0.0235(8) 0.0034(6) 0.0041(6) 0.0017(6) C23 0.0187(8) 0.0209(9) 0.0224(8) 0.0015(7) 0.0042(7) 0.0010(7) C24 0.0214(8) 0.0256(9) 0.0299(9) 0.0043(7) 0.0103(7) 0.0031(7) C25 0.0144(7) 0.0299(10) 0.0370(10) 0.0062(8) 0.0057(7) 0.0007(7) C26 0.0175(8) 0.0254(9) 0.0278(9) 0.0025(7) -0.0020(7) -0.0002(7) C27 0.0186(8) 0.0199(8) 0.0229(8) 0.0033(7) 0.0041(7) 0.0027(7) C28 0.0178(7) 0.0224(9) 0.0216(8) -0.0037(7) 0.0083(7) -0.0058(7) C29 0.0268(9) 0.0208(9) 0.0330(10) -0.0037(7) 0.0093(8) -0.0050(7) C30 0.0374(11) 0.0248(10) 0.0402(11) -0.0091(9) 0.0135(9) -0.0130(9) C31 0.0274(9) 0.0383(12) 0.0354(11) -0.0131(9) 0.0073(8) -0.0155(9) C32 0.0210(8) 0.0385(12) 0.0296(10) -0.0063(8) 0.0042(8) -0.0049(8) C33 0.0210(8) 0.0243(9) 0.0248(9) -0.0049(7) 0.0066(7) -0.0031(7) C34 0.0158(7) 0.0171(8) 0.0212(8) -0.0037(6) 0.0022(6) -0.0005(6) C35 0.0226(8) 0.0192(9) 0.0242(9) -0.0016(7) 0.0019(7) 0.0010(7) C36 0.0203(8) 0.0280(10) 0.0296(9) -0.0026(8) -0.0044(7) 0.0052(7) C37 0.0164(8) 0.0332(11) 0.0374(11) -0.0080(9) 0.0004(8) -0.0018(7) C38 0.0220(8) 0.0247(9) 0.0315(10) -0.0041(8) 0.0080(7) -0.0060(7) C39 0.0193(8) 0.0195(8) 0.0221(8) -0.0014(7) 0.0018(7) -0.0018(7) C40 0.0191(7) 0.0190(8) 0.0184(8) 0.0028(6) 0.0055(6) 0.0006(6) C41 0.0300(9) 0.0251(10) 0.0304(10) -0.0038(8) 0.0126(8) -0.0040(8) C42 0.0384(11) 0.0336(11) 0.0399(11) -0.0072(9) 0.0232(10) 0.0008(9) C43 0.0246(9) 0.0370(11) 0.0393(11) 0.0044(9) 0.0184(8) 0.0027(8) C44 0.0215(8) 0.0296(10) 0.0294(9) 0.0038(8) 0.0072(7) -0.0038(7) C45 0.0207(8) 0.0227(9) 0.0206(8) 0.0006(7) 0.0065(7) -0.0008(7) C46 0.0162(7) 0.0210(9) 0.0229(8) -0.0068(7) 0.0046(6) -0.0031(6) C47 0.0155(7) 0.0218(9) 0.0278(9) -0.0056(7) -0.0009(7) 0.0009(7) C48 0.0237(8) 0.0185(8) 0.0243(9) -0.0042(7) 0.0006(7) -0.0008(7) C49 0.0203(8) 0.0205(9) 0.0238(8) -0.0035(7) 0.0066(7) -0.0045(7) C50 0.0152(7) 0.0242(9) 0.0217(8) -0.0043(7) 0.0028(6) -0.0006(7) C51 0.0172(7) 0.0198(8) 0.0225(8) -0.0006(7) 0.0032(6) -0.0003(6) C52 0.0346(10) 0.0243(10) 0.0399(11) 0.0034(9) -0.0066(9) -0.0012(8) C53 0.0153(8) 0.0332(11) 0.0351(10) -0.0008(8) 0.0028(7) -0.0020(7) C54 0.0217(8) 0.0185(8) 0.0177(8) 0.0018(6) 0.0035(6) 0.0024(7) C55 0.0225(8) 0.0206(9) 0.0212(8) 0.0005(7) 0.0046(7) 0.0051(7) C56 0.0196(8) 0.0240(9) 0.0197(8) 0.0004(7) 0.0047(6) 0.0042(7) C57 0.0188(8) 0.0287(10) 0.0191(8) 0.0000(7) 0.0041(7) 0.0041(7) C58 0.0256(9) 0.0315(11) 0.0300(10) -0.0027(8) 0.0055(8) 0.0054(8) C59 0.0263(9) 0.0396(12) 0.0388(11) -0.0035(9) 0.0099(9) 0.0114(9) C60 0.0195(8) 0.0481(13) 0.0350(11) 0.0001(9) 0.0091(8) 0.0045(9) C61 0.0220(9) 0.0362(11) 0.0326(10) 0.0008(8) 0.0077(8) -0.0005(8) C62 0.0209(8) 0.0296(10) 0.0281(9) 0.0017(8) 0.0069(7) 0.0044(7) C63 0.0244(8) 0.0198(8) 0.0183(8) 0.0000(6) 0.0070(7) -0.0004(7) C64 0.0237(8) 0.0165(8) 0.0243(8) -0.0023(7) 0.0072(7) 0.0001(7) C65 0.0244(9) 0.0248(9) 0.0298(9) -0.0043(7) 0.0089(7) -0.0022(7) C66 0.0347(10) 0.0231(10) 0.0312(10) -0.0036(8) 0.0114(8) -0.0091(8) C67 0.0415(11) 0.0178(9) 0.0344(10) 0.0030(8) 0.0049(9) -0.0029(8) C68 0.0311(10) 0.0214(9) 0.0315(10) 0.0023(8) 0.0033(8) 0.0025(8) B1 0.0137(8) 0.0165(9) 0.0192(8) -0.0008(7) 0.0045(7) -0.0015(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.8934(12) . ? Fe1 N1 2.0849(14) . ? Fe1 N3 2.0854(14) . ? Fe1 N5 2.2847(14) . ? Fe1 N7 2.3411(15) . ? O1 C46 1.338(2) . ? O2 H2 0.85(3) . ? O2 C49 1.390(2) . ? N1 C9 1.342(2) . ? N2 N1 1.3729(18) . ? N2 C7 1.363(2) . ? N2 B1 1.556(2) . ? N3 C3 1.346(2) . ? N4 N3 1.3732(18) . ? N4 C1 1.364(2) . ? N4 B1 1.559(2) . ? N5 C6 1.341(2) . ? N6 N5 1.3766(18) . ? N6 C4 1.364(2) . ? N6 B1 1.540(2) . ? N7 C54 1.347(2) . ? N8 N7 1.3545(19) . ? N8 H7 0.89(2) . ? N8 C56 1.353(2) . ? C1 C2 1.381(2) . ? C1 C10 1.479(2) . ? C2 H2A 0.9500 . ? C2 C3 1.397(2) . ? C3 C16 1.475(2) . ? C4 C5 1.379(2) . ? C4 C22 1.483(2) . ? C5 H5 0.9500 . ? C5 C6 1.403(2) . ? C6 C28 1.477(2) . ? C7 C8 1.385(2) . ? C7 C34 1.477(2) . ? C8 H8 0.9500 . ? C8 C9 1.397(2) . ? C9 C40 1.472(2) . ? C10 C11 1.399(3) . ? C10 C15 1.394(3) . ? C11 H11 0.9500 . ? C11 C12 1.389(3) . ? C12 H12 0.9500 . ? C12 C13 1.384(3) . ? C13 H13 0.9500 . ? C13 C14 1.386(3) . ? C14 H14 0.9500 . ? C14 C15 1.391(2) . ? C15 H15 0.9500 . ? C16 C17 1.398(3) . ? C16 C21 1.394(3) . ? C17 H17 0.9500 . ? C17 C18 1.389(3) . ? C18 H18 0.9500 . ? C18 C19 1.383(3) . ? C19 H19 0.9500 . ? C19 C20 1.378(3) . ? C20 H20 0.9500 . ? C20 C21 1.391(3) . ? C21 H21 0.9500 . ? C22 C23 1.398(2) . ? C22 C27 1.400(2) . ? C23 H23 0.9500 . ? C23 C24 1.392(2) . ? C24 H24 0.9500 . ? C24 C25 1.388(3) . ? C25 H25 0.9500 . ? C25 C26 1.389(3) . ? C26 H26 0.9500 . ? C26 C27 1.392(2) . ? C27 H27 0.9500 . ? C28 C29 1.395(3) . ? C28 C33 1.394(3) . ? C29 H29 0.9500 . ? C29 C30 1.391(3) . ? C30 H30 0.9500 . ? C30 C31 1.387(3) . ? C31 H31 0.9500 . ? C31 C32 1.381(3) . ? C32 H32 0.9500 . ? C32 C33 1.391(3) . ? C33 H33 0.9500 . ? C34 C35 1.400(2) . ? C34 C39 1.395(2) . ? C35 H35 0.9500 . ? C35 C36 1.390(2) . ? C36 H36 0.9500 . ? C36 C37 1.381(3) . ? C37 H37 0.9500 . ? C37 C38 1.387(3) . ? C38 H38 0.9500 . ? C38 C39 1.391(2) . ? C39 H39 0.9500 . ? C40 C41 1.393(2) . ? C40 C45 1.391(2) . ? C41 H41 0.9500 . ? C41 C42 1.385(3) . ? C42 H42 0.9500 . ? C42 C43 1.384(3) . ? C43 H43 0.9500 . ? C43 C44 1.385(3) . ? C44 H44 0.9500 . ? C44 C45 1.388(2) . ? C45 H45 0.9500 . ? C46 C47 1.391(3) . ? C46 C51 1.403(2) . ? C47 H62 0.9500 . ? C47 C48 1.392(3) . ? C48 C49 1.395(2) . ? C48 C52 1.511(3) . ? C49 C50 1.392(3) . ? C50 C51 1.393(2) . ? C50 C53 1.510(2) . ? C51 H66 0.9500 . ? C52 H67A 0.9800 . ? C52 H67B 0.9800 . ? C52 H67C 0.9800 . ? C53 H68A 0.9800 . ? C53 H68B 0.9800 . ? C53 H68C 0.9800 . ? C54 C63 1.476(2) . ? C55 C54 1.405(2) . ? C55 H47 0.9500 . ? C56 C55 1.374(3) . ? C56 C57 1.471(2) . ? C57 C58 1.396(3) . ? C57 C62 1.393(3) . ? C58 H54 0.9500 . ? C59 C58 1.390(3) . ? C59 H53 0.9500 . ? C60 C59 1.379(3) . ? C60 H52 0.9500 . ? C61 C60 1.383(3) . ? C61 H51 0.9500 . ? C62 C61 1.390(2) . ? C62 H50 0.9500 . ? C63 C64 1.391(2) . ? C63 C68 1.401(3) . ? C64 H56 0.9500 . ? C64 C65 1.390(2) . ? C65 H57 0.9500 . ? C65 C66 1.388(3) . ? C66 H58 0.9500 . ? C66 C67 1.384(3) . ? C67 H59 0.9500 . ? C67 C68 1.386(3) . ? C68 H60 0.9500 . ? B1 H1 1.0000 . ? 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 O1 Fe1 N1 134.21(6) . . ? O1 Fe1 N3 131.98(6) . . ? O1 Fe1 N5 101.45(5) . . ? O1 Fe1 N7 89.04(5) . . ? N1 Fe1 N3 93.61(5) . . ? N1 Fe1 N5 85.41(5) . . ? N1 Fe1 N7 89.01(5) . . ? N3 Fe1 N5 83.65(5) . . ? N3 Fe1 N7 87.53(5) . . ? N5 Fe1 N7 169.24(5) . . ? C46 O1 Fe1 148.67(12) . . ? C49 O2 H2 108(2) . . ? N2 N1 Fe1 117.55(10) . . ? C9 N1 Fe1 133.29(11) . . ? C9 N1 N2 107.05(13) . . ? N1 N2 B1 119.04(13) . . ? C7 N2 N1 109.32(13) . . ? C7 N2 B1 131.59(13) . . ? N4 N3 Fe1 117.01(10) . . ? C3 N3 Fe1 134.80(11) . . ? C3 N3 N4 107.29(13) . . ? N3 N4 B1 120.21(13) . . ? C1 N4 N3 109.17(13) . . ? C1 N4 B1 130.26(14) . . ? N6 N5 Fe1 112.83(10) . . ? C6 N5 Fe1 141.00(11) . . ? C6 N5 N6 106.11(13) . . ? N5 N6 B1 120.28(13) . . ? C4 N6 N5 110.15(13) . . ? C4 N6 B1 129.16(13) . . ? N8 N7 Fe1 109.45(11) . . ? C54 N7 Fe1 144.41(11) . . ? C54 N7 N8 104.63(14) . . ? N7 N8 H7 116.8(15) . . ? C56 N8 N7 113.01(15) . . ? C56 N8 H7 129.6(15) . . ? N4 C1 C2 107.91(15) . . ? N4 C1 C10 125.05(15) . . ? C2 C1 C10 127.03(16) . . ? C1 C2 H2A 126.9 . . ? C1 C2 C3 106.13(15) . . ? C3 C2 H2A 126.9 . . ? N3 C3 C2 109.50(15) . . ? N3 C3 C16 121.74(15) . . ? C2 C3 C16 128.72(16) . . ? N6 C4 C5 107.54(14) . . ? N6 C4 C22 124.14(15) . . ? C5 C4 C22 128.01(15) . . ? C4 C5 H5 127.1 . . ? C4 C5 C6 105.80(15) . . ? C6 C5 H5 127.1 . . ? N5 C6 C5 110.38(14) . . ? N5 C6 C28 123.72(15) . . ? C5 C6 C28 125.50(15) . . ? N2 C7 C8 107.94(14) . . ? N2 C7 C34 125.32(15) . . ? C8 C7 C34 126.67(15) . . ? C7 C8 H8 127.2 . . ? C7 C8 C9 105.69(15) . . ? C9 C8 H8 127.2 . . ? N1 C9 C8 110.00(14) . . ? N1 C9 C40 120.37(15) . . ? C8 C9 C40 129.48(15) . . ? C11 C10 C1 117.89(16) . . ? C15 C10 C1 123.42(16) . . ? C15 C10 C11 118.68(16) . . ? C10 C11 H11 119.8 . . ? C12 C11 C10 120.49(19) . . ? C12 C11 H11 119.8 . . ? C11 C12 H12 119.9 . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C12 C13 H13 120.0 . . ? C12 C13 C14 120.03(18) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 120.0 . . ? C13 C14 C15 119.95(19) . . ? C15 C14 H14 120.0 . . ? C10 C15 H15 119.7 . . ? C14 C15 C10 120.67(18) . . ? C14 C15 H15 119.7 . . ? C17 C16 C3 119.55(17) . . ? C21 C16 C3 122.13(17) . . ? C21 C16 C17 118.26(17) . . ? C16 C17 H17 119.7 . . ? C18 C17 C16 120.65(19) . . ? C18 C17 H17 119.7 . . ? C17 C18 H18 119.9 . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.9 . . ? C18 C19 H19 120.1 . . ? C20 C19 C18 119.74(18) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 119.9 . . ? C19 C20 C21 120.3(2) . . ? C21 C20 H20 119.9 . . ? C16 C21 H21 119.6 . . ? C20 C21 C16 120.77(19) . . ? C20 C21 H21 119.6 . . ? C23 C22 C4 117.66(15) . . ? C23 C22 C27 118.81(15) . . ? C27 C22 C4 123.52(15) . . ? C22 C23 H23 119.6 . . ? C24 C23 C22 120.76(17) . . ? C24 C23 H23 119.6 . . ? C23 C24 H24 120.2 . . ? C25 C24 C23 119.62(17) . . ? C25 C24 H24 120.2 . . ? C24 C25 H25 119.8 . . ? C24 C25 C26 120.41(16) . . ? C26 C25 H25 119.8 . . ? C25 C26 H26 120.1 . . ? C25 C26 C27 119.87(17) . . ? C27 C26 H26 120.1 . . ? C22 C27 H27 119.8 . . ? C26 C27 C22 120.46(16) . . ? C26 C27 H27 119.8 . . ? C29 C28 C6 119.74(16) . . ? C33 C28 C6 121.00(16) . . ? C33 C28 C29 118.87(16) . . ? C28 C29 H29 119.8 . . ? C30 C29 C28 120.41(19) . . ? C30 C29 H29 119.8 . . ? C29 C30 H30 120.0 . . ? C31 C30 C29 120.07(19) . . ? C31 C30 H30 120.0 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 119.95(18) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.19(19) . . ? C33 C32 H32 119.9 . . ? C28 C33 H33 119.8 . . ? C32 C33 C28 120.48(18) . . ? C32 C33 H33 119.8 . . ? C35 C34 C7 117.75(15) . . ? C39 C34 C7 123.22(15) . . ? C39 C34 C35 119.00(15) . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.44(17) . . ? C36 C35 H35 119.8 . . ? C35 C36 H36 120.0 . . ? C37 C36 C35 120.10(18) . . ? C37 C36 H36 120.0 . . ? C36 C37 H37 120.0 . . ? C36 C37 C38 119.99(17) . . ? C38 C37 H37 120.0 . . ? C37 C38 H38 119.8 . . ? C37 C38 C39 120.37(18) . . ? C39 C38 H38 119.8 . . ? C34 C39 H39 120.0 . . ? C38 C39 C34 120.07(17) . . ? C38 C39 H39 120.0 . . ? C41 C40 C9 119.33(16) . . ? C45 C40 C9 121.71(15) . . ? C45 C40 C41 118.90(16) . . ? C40 C41 H41 119.9 . . ? C42 C41 C40 120.13(18) . . ? C42 C41 H41 119.9 . . ? C41 C42 H42 119.8 . . ? C43 C42 C41 120.46(19) . . ? C43 C42 H42 119.8 . . ? C42 C43 H43 120.0 . . ? C42 C43 C44 119.96(17) . . ? C44 C43 H43 120.0 . . ? C43 C44 H44 120.2 . . ? C43 C44 C45 119.59(18) . . ? C45 C44 H44 120.2 . . ? C40 C45 H45 119.5 . . ? C44 C45 C40 120.91(17) . . ? C44 C45 H45 119.5 . . ? O1 C46 C47 123.27(15) . . ? O1 C46 C51 118.94(16) . . ? C47 C46 C51 117.77(16) . . ? C46 C47 H62 119.1 . . ? C46 C47 C48 121.75(16) . . ? C48 C47 H62 119.1 . . ? C47 C48 C49 118.70(17) . . ? C47 C48 C52 120.73(17) . . ? C49 C48 C52 120.51(17) . . ? O2 C49 C48 122.28(17) . . ? O2 C49 C50 116.33(15) . . ? C50 C49 C48 121.38(16) . . ? C49 C50 C51 118.35(15) . . ? C49 C50 C53 120.72(16) . . ? C51 C50 C53 120.91(17) . . ? C46 C51 H66 119.1 . . ? C50 C51 C46 121.90(17) . . ? C50 C51 H66 119.1 . . ? C48 C52 H67A 109.5 . . ? C48 C52 H67B 109.5 . . ? C48 C52 H67C 109.5 . . ? H67A C52 H67B 109.5 . . ? H67A C52 H67C 109.5 . . ? H67B C52 H67C 109.5 . . ? C50 C53 H68A 109.5 . . ? C50 C53 H68B 109.5 . . ? C50 C53 H68C 109.5 . . ? H68A C53 H68B 109.5 . . ? H68A C53 H68C 109.5 . . ? H68B C53 H68C 109.5 . . ? N7 C54 C55 110.21(15) . . ? N7 C54 C63 124.92(15) . . ? C55 C54 C63 124.86(16) . . ? C54 C55 H47 126.8 . . ? C56 C55 C54 106.33(16) . . ? C56 C55 H47 126.8 . . ? N8 C56 C55 105.80(15) . . ? N8 C56 C57 124.02(17) . . ? C55 C56 C57 130.14(16) . . ? C58 C57 C56 118.79(17) . . ? C62 C57 C56 122.69(16) . . ? C62 C57 C58 118.52(17) . . ? C57 C58 H54 119.8 . . ? C59 C58 C57 120.5(2) . . ? C59 C58 H54 119.8 . . ? C58 C59 H53 119.8 . . ? C60 C59 C58 120.49(19) . . ? C60 C59 H53 119.8 . . ? C59 C60 H52 120.3 . . ? C59 C60 C61 119.48(18) . . ? C61 C60 H52 120.3 . . ? C60 C61 H51 119.7 . . ? C60 C61 C62 120.5(2) . . ? C62 C61 H51 119.7 . . ? C57 C62 H50 119.8 . . ? C61 C62 C57 120.48(18) . . ? C61 C62 H50 119.8 . . ? C64 C63 C54 122.54(16) . . ? C64 C63 C68 118.46(17) . . ? C68 C63 C54 118.95(16) . . ? C63 C64 H56 119.6 . . ? C65 C64 C63 120.72(17) . . ? C65 C64 H56 119.6 . . ? C64 C65 H57 119.9 . . ? C66 C65 C64 120.27(18) . . ? C66 C65 H57 119.9 . . ? C65 C66 H58 120.2 . . ? C67 C66 C65 119.51(18) . . ? C67 C66 H58 120.2 . . ? C66 C67 H59 119.8 . . ? C66 C67 C68 120.39(18) . . ? C68 C67 H59 119.8 . . ? C63 C68 H60 119.7 . . ? C67 C68 C63 120.64(18) . . ? C67 C68 H60 119.7 . . ? N2 B1 N4 111.15(13) . . ? N2 B1 H1 109.3 . . ? N4 B1 H1 109.3 . . ? N6 B1 N2 108.68(13) . . ? N6 B1 N4 109.01(13) . . ? N6 B1 H1 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 29.1(3) . . . . ? Fe1 O1 C46 C51 -149.39(17) . . . . ? Fe1 N1 C9 C8 162.76(12) . . . . ? Fe1 N1 C9 C40 -13.3(2) . . . . ? Fe1 N3 C3 C2 -168.18(13) . . . . ? Fe1 N3 C3 C16 9.6(3) . . . . ? Fe1 N5 C6 C5 176.12(13) . . . . ? Fe1 N5 C6 C28 -10.8(3) . . . . ? Fe1 N7 C54 C55 -161.88(15) . . . . ? Fe1 N7 C54 C63 19.5(3) . . . . ? O1 Fe1 N1 N2 -153.40(10) . . . . ? O1 Fe1 N1 C9 45.59(18) . . . . ? O1 Fe1 N3 N4 148.90(10) . . . . ? O1 Fe1 N3 C3 -43.61(19) . . . . ? O1 Fe1 N5 N6 175.46(10) . . . . ? O1 Fe1 N5 C6 -1.37(19) . . . . ? O1 Fe1 N7 N8 -9.69(11) . . . . ? O1 Fe1 N7 C54 152.8(2) . . . . ? O1 C46 C47 C48 -173.79(16) . . . . ? O1 C46 C51 C50 174.91(16) . . . . ? O2 C49 C50 C51 -179.01(15) . . . . ? O2 C49 C50 C53 -0.5(2) . . . . ? N1 Fe1 O1 C46 15.1(3) . . . . ? N1 Fe1 N3 N4 -35.77(11) . . . . ? N1 Fe1 N3 C3 131.72(16) . . . . ? N1 Fe1 N5 N6 41.24(10) . . . . ? N1 Fe1 N5 C6 -135.60(18) . . . . ? N1 Fe1 N7 N8 124.56(11) . . . . ? N1 Fe1 N7 C54 -72.9(2) . . . . ? N1 N2 C7 C8 0.15(18) . . . . ? N1 N2 C7 C34 -176.93(15) . . . . ? N1 N2 B1 N4 -63.71(18) . . . . ? N1 N2 B1 N6 56.26(18) . . . . ? N1 C9 C40 C41 139.36(18) . . . . ? N1 C9 C40 C45 -38.0(2) . . . . ? N2 N1 C9 C8 0.32(18) . . . . ? N2 N1 C9 C40 -175.71(14) . . . . ? N2 C7 C8 C9 0.04(19) . . . . ? N2 C7 C34 C35 134.03(18) . . . . ? N2 C7 C34 C39 -48.0(3) . . . . ? N3 Fe1 O1 C46 -171.4(2) . . . . ? N3 Fe1 N1 N2 31.44(11) . . . . ? N3 Fe1 N1 C9 -129.57(15) . . . . ? N3 Fe1 N5 N6 -52.92(10) . . . . ? N3 Fe1 N5 C6 130.24(18) . . . . ? N3 Fe1 N7 N8 -141.78(11) . . . . ? N3 Fe1 N7 C54 20.7(2) . . . . ? N3 N4 C1 C2 0.25(18) . . . . ? N3 N4 C1 C10 -178.59(15) . . . . ? N3 N4 B1 N2 58.56(19) . . . . ? N3 N4 B1 N6 -61.21(18) . . . . ? N3 C3 C16 C17 -149.75(17) . . . . ? N3 C3 C16 C21 27.3(3) . . . . ? N4 N3 C3 C2 0.15(19) . . . . ? N4 N3 C3 C16 177.92(15) . . . . ? N4 C1 C2 C3 -0.15(19) . . . . ? N4 C1 C10 C11 135.53(18) . . . . ? N4 C1 C10 C15 -46.0(3) . . . . ? N5 Fe1 O1 C46 -79.7(2) . . . . ? N5 Fe1 N1 N2 -51.88(11) . . . . ? N5 Fe1 N1 C9 147.11(16) . . . . ? N5 Fe1 N3 N4 49.20(11) . . . . ? N5 Fe1 N3 C3 -143.31(16) . . . . ? N5 Fe1 N7 N8 -176.7(2) . . . . ? N5 Fe1 N7 C54 -14.2(4) . . . . ? N5 N6 C4 C5 0.74(18) . . . . ? N5 N6 C4 C22 -173.36(15) . . . . ? N5 N6 B1 N2 -67.02(18) . . . . ? N5 N6 B1 N4 54.27(18) . . . . ? N5 C6 C28 C29 149.89(17) . . . . ? N5 C6 C28 C33 -37.4(2) . . . . ? N6 N5 C6 C5 -0.84(18) . . . . ? N6 N5 C6 C28 172.24(15) . . . . ? N6 C4 C5 C6 -1.21(19) . . . . ? N6 C4 C22 C23 130.07(18) . . . . ? N6 C4 C22 C27 -49.2(2) . . . . ? N7 Fe1 O1 C46 102.8(2) . . . . ? N7 Fe1 N1 N2 118.90(11) . . . . ? N7 Fe1 N1 C9 -42.11(15) . . . . ? N7 Fe1 N3 N4 -124.62(11) . . . . ? N7 Fe1 N3 C3 42.86(16) . . . . ? N7 Fe1 N5 N6 -17.8(3) . . . . ? N7 Fe1 N5 C6 165.4(2) . . . . ? N7 N8 C56 C55 0.1(2) . . . . ? N7 N8 C56 C57 177.93(15) . . . . ? N7 C54 C63 C64 26.1(3) . . . . ? N7 C54 C63 C68 -156.31(17) . . . . ? N8 N7 C54 C55 1.08(18) . . . . ? N8 N7 C54 C63 -177.58(15) . . . . ? N8 C56 C55 C54 0.58(19) . . . . ? N8 C56 C57 C58 175.41(17) . . . . ? N8 C56 C57 C62 -5.0(3) . . . . ? C1 N4 N3 Fe1 170.48(11) . . . . ? C1 N4 N3 C3 -0.25(18) . . . . ? C1 N4 B1 N2 -113.70(18) . . . . ? C1 N4 B1 N6 126.53(17) . . . . ? C1 C2 C3 N3 0.0(2) . . . . ? C1 C2 C3 C16 -177.56(17) . . . . ? C1 C10 C11 C12 179.36(18) . . . . ? C1 C10 C15 C14 -179.28(17) . . . . ? C2 C1 C10 C11 -43.1(3) . . . . ? C2 C1 C10 C15 135.4(2) . . . . ? C2 C3 C16 C17 27.6(3) . . . . ? C2 C3 C16 C21 -155.37(19) . . . . ? C3 C16 C17 C18 175.71(16) . . . . ? C3 C16 C21 C20 -175.67(17) . . . . ? C4 N6 N5 Fe1 -177.86(10) . . . . ? C4 N6 N5 C6 0.06(17) . . . . ? C4 N6 B1 N2 121.05(17) . . . . ? C4 N6 B1 N4 -117.66(17) . . . . ? C4 C5 C6 N5 1.3(2) . . . . ? C4 C5 C6 C28 -171.64(16) . . . . ? C4 C22 C23 C24 -177.04(16) . . . . ? C4 C22 C27 C26 176.94(16) . . . . ? C5 C4 C22 C23 -42.8(3) . . . . ? C5 C4 C22 C27 137.97(19) . . . . ? C5 C6 C28 C29 -38.1(3) . . . . ? C5 C6 C28 C33 134.66(19) . . . . ? C6 C28 C29 C30 171.54(17) . . . . ? C6 C28 C33 C32 -172.11(16) . . . . ? C7 N2 N1 Fe1 -165.95(11) . . . . ? C7 N2 N1 C9 -0.30(17) . . . . ? C7 N2 B1 N4 113.47(18) . . . . ? C7 N2 B1 N6 -126.56(17) . . . . ? C7 C8 C9 N1 -0.23(19) . . . . ? C7 C8 C9 C40 175.34(17) . . . . ? C7 C34 C35 C36 179.28(16) . . . . ? C7 C34 C39 C38 -179.68(16) . . . . ? C8 C7 C34 C35 -42.5(2) . . . . ? C8 C7 C34 C39 135.42(19) . . . . ? C8 C9 C40 C41 -35.8(3) . . . . ? C8 C9 C40 C45 146.87(19) . . . . ? C9 C40 C41 C42 -175.32(18) . . . . ? C9 C40 C45 C44 175.29(16) . . . . ? C10 C1 C2 C3 178.66(16) . . . . ? C10 C11 C12 C13 -0.1(3) . . . . ? C11 C10 C15 C14 -0.8(3) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C13 C14 C15 C10 0.1(3) . . . . ? C15 C10 C11 C12 0.8(3) . . . . ? C16 C17 C18 C19 0.7(3) . . . . ? C17 C16 C21 C20 1.4(3) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C18 C19 C20 C21 -0.2(3) . . . . ? C19 C20 C21 C16 -0.6(3) . . . . ? C21 C16 C17 C18 -1.5(3) . . . . ? C22 C4 C5 C6 172.59(16) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C23 C22 C27 C26 -2.3(3) . . . . ? C23 C24 C25 C26 -2.0(3) . . . . ? C24 C25 C26 C27 2.0(3) . . . . ? C25 C26 C27 C22 0.2(3) . . . . ? C27 C22 C23 C24 2.3(3) . . . . ? C28 C29 C30 C31 0.5(3) . . . . ? C29 C28 C33 C32 0.7(3) . . . . ? C29 C30 C31 C32 1.0(3) . . . . ? C30 C31 C32 C33 -1.7(3) . . . . ? C31 C32 C33 C28 0.8(3) . . . . ? C33 C28 C29 C30 -1.4(3) . . . . ? C34 C7 C8 C9 177.08(16) . . . . ? C34 C35 C36 C37 0.4(3) . . . . ? C35 C34 C39 C38 -1.8(3) . . . . ? C35 C36 C37 C38 -1.5(3) . . . . ? C36 C37 C38 C39 1.0(3) . . . . ? C37 C38 C39 C34 0.6(3) . . . . ? C39 C34 C35 C36 1.3(3) . . . . ? C40 C41 C42 C43 -0.5(3) . . . . ? C41 C40 C45 C44 -2.0(3) . . . . ? C41 C42 C43 C44 -1.1(3) . . . . ? C42 C43 C44 C45 1.2(3) . . . . ? C43 C44 C45 C40 0.4(3) . . . . ? C45 C40 C41 C42 2.1(3) . . . . ? C46 C47 C48 C49 -2.7(3) . . . . ? C46 C47 C48 C52 174.36(17) . . . . ? C47 C46 C51 C50 -3.6(3) . . . . ? C47 C48 C49 O2 -179.96(16) . . . . ? C47 C48 C49 C50 -0.4(3) . . . . ? C48 C49 C50 C51 1.4(3) . . . . ? C48 C49 C50 C53 179.98(17) . . . . ? C49 C50 C51 C46 0.6(3) . . . . ? C51 C46 C47 C48 4.7(3) . . . . ? C52 C48 C49 O2 2.9(3) . . . . ? C52 C48 C49 C50 -177.52(17) . . . . ? C53 C50 C51 C46 -177.91(16) . . . . ? C54 C63 C64 C65 178.60(16) . . . . ? C54 C63 C68 C67 -178.69(17) . . . . ? C55 C54 C63 C64 -152.32(17) . . . . ? C55 C54 C63 C68 25.2(3) . . . . ? C55 C56 C57 C58 -7.3(3) . . . . ? C55 C56 C57 C62 172.28(19) . . . . ? C56 N8 N7 Fe1 168.86(11) . . . . ? C56 N8 N7 C54 -0.72(19) . . . . ? C56 C55 C54 N7 -1.1(2) . . . . ? C56 C55 C54 C63 177.60(16) . . . . ? C56 C57 C58 C59 -178.49(18) . . . . ? C56 C57 C62 C61 178.91(17) . . . . ? C57 C56 C55 C54 -177.10(17) . . . . ? C57 C62 C61 C60 0.0(3) . . . . ? C58 C57 C62 C61 -1.5(3) . . . . ? C60 C59 C58 C57 -0.8(3) . . . . ? C61 C60 C59 C58 -0.8(3) . . . . ? C62 C57 C58 C59 1.9(3) . . . . ? C62 C61 C60 C59 1.2(3) . . . . ? C63 C64 C65 C66 -0.1(3) . . . . ? C64 C63 C68 C67 -1.0(3) . . . . ? C64 C65 C66 C67 -0.8(3) . . . . ? C65 C66 C67 C68 0.8(3) . . . . ? C66 C67 C68 C63 0.1(3) . . . . ? C68 C63 C64 C65 1.0(3) . . . . ? B1 N2 N1 Fe1 11.81(18) . . . . ? B1 N2 N1 C9 177.47(14) . . . . ? B1 N2 C7 C8 -177.23(16) . . . . ? B1 N2 C7 C34 5.7(3) . . . . ? B1 N4 N3 Fe1 -3.27(18) . . . . ? B1 N4 N3 C3 -174.00(14) . . . . ? B1 N4 C1 C2 173.18(16) . . . . ? B1 N4 C1 C10 -5.7(3) . . . . ? B1 N6 N5 Fe1 8.80(17) . . . . ? B1 N6 N5 C6 -173.28(14) . . . . ? B1 N6 C4 C5 173.32(16) . . . . ? B1 N6 C4 C22 -0.8(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2 -31 0 0.1259 1.9999 -31.0001 -0.0000 0.3939 0.8518 0.3096 -2 31 0 0.1259 -1.9999 31.0001 0.0000 -0.3939 -0.8518 -0.3096 5 8 -19 0.2463 5.0001 8.0003 -18.9999 0.0266 0.0674 -1.0205 25 -1 0 0.0328 25.0000 -0.9997 0.0001 -0.8586 0.5333 -0.0107 -25 1 0 0.0218 -25.0000 0.9997 -0.0001 0.8586 -0.5333 0.0107 9 19 13 0.2324 9.0000 19.0000 13.0000 -0.8183 -0.4346 0.4422 6 -16 15 0.1840 5.9999 -16.0001 14.9999 -0.2237 0.4020 0.8946 #==END data_Complex2E _database_code_depnum_ccdc_archive 'CCDC 890623' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-06 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C98 H76 B2 Fe2 N12 O4, 2(C4 H10 O)' _chemical_formula_sum 'C106 H96 B2 Fe2 N12 O6' _chemical_formula_weight 1767.27 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe2 C8 O4 H8 (B C9 H4 N6 Ph6)2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' _cell_length_a 9.6359(10) _cell_length_b 13.4413(14) _cell_length_c 18.205(2) _cell_angle_alpha 95.633(9) _cell_angle_beta 105.298(10) _cell_angle_gamma 99.002(9) _cell_volume 2222.1(4) _cell_formula_units_Z 1 _cell_measurement_reflns_used 2323 _cell_measurement_temperature 101(1) _cell_measurement_theta_max 73.9052 _cell_measurement_theta_min 3.3625 _exptl_absorpt_coefficient_mu 3.131 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 926 _exptl_crystal_size_max 0.3275 _exptl_crystal_size_mid 0.0381 _exptl_crystal_size_min 0.025 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.1096 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 15573 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 74.07 _diffrn_reflns_theta_min 3.37 _diffrn_ambient_temperature 101(1) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -67.00 38.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 77.0000 -150.0000 105 #__ type_ start__ end____ width___ exp.time_ 2 omega -34.00 -7.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega -69.00 31.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 57.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 4 omega -73.00 38.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 77.0000 90.0000 111 #__ type_ start__ end____ width___ exp.time_ 5 omega 40.00 65.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 40.6487 -125.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 6 omega 33.00 99.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 90.0000 66 #__ type_ start__ end____ width___ exp.time_ 7 omega 44.00 106.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -90.0000 62 #__ type_ start__ end____ width___ exp.time_ 8 omega 29.00 68.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 150.0000 39 #__ type_ start__ end____ width___ exp.time_ 9 omega 23.00 62.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -30.0000 39 #__ type_ start__ end____ width___ exp.time_ 10 omega 62.00 106.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -180.0000 44 #__ type_ start__ end____ width___ exp.time_ 11 omega 67.00 102.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -30.0000 35 #__ type_ start__ end____ width___ exp.time_ 12 omega 43.00 97.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -60.0000 54 #__ type_ start__ end____ width___ exp.time_ 13 omega 76.00 177.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 77.0000 30.0000 101 #__ type_ start__ end____ width___ exp.time_ 14 omega 69.00 117.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -125.0000 90.0000 48 #__ type_ start__ end____ width___ exp.time_ 15 omega 44.00 69.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 16 omega 119.00 177.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 61.0000 -120.0000 58 #__ type_ start__ end____ width___ exp.time_ 17 omega 89.00 172.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 0.0000 83 #__ type_ start__ end____ width___ exp.time_ 18 omega 86.00 163.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 45.0000 -60.0000 77 #__ type_ start__ end____ width___ exp.time_ 19 omega 24.00 108.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 90.0000 84 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0612219000 _diffrn_orient_matrix_UB_12 -0.1140934000 _diffrn_orient_matrix_UB_13 -0.0291451000 _diffrn_orient_matrix_UB_21 -0.0332173000 _diffrn_orient_matrix_UB_22 0.0219187000 _diffrn_orient_matrix_UB_23 -0.0837385000 _diffrn_orient_matrix_UB_31 0.1537860000 _diffrn_orient_matrix_UB_32 -0.0162200000 _diffrn_orient_matrix_UB_33 -0.0020343000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 5402 _reflns_number_total 8687 _reflns_odcompleteness_completeness 99.89 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.588 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 569 _refine_ls_number_reflns 8687 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0718 _refine_ls_restrained_S_all 1.025 _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^)+(0.0978P)^2^+0.0244P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1807 _refine_ls_wR_factor_ref 0.2227 _refine_special_details ; For the two disordered Ph groups, ShelXL SAME instructions have been used to keep their molecular geometry (1.2- and 1,3-distances) equal for both alternative orientations. 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 0.64997(7) 0.62250(6) 0.72675(4) 0.0399(2) Uani 1 1 d . . . O1 O 0.5150(3) 0.6272(3) 0.63019(18) 0.0495(8) Uani 1 1 d . . . O2 O 0.6829(4) 0.4919(3) 0.64285(19) 0.0610(10) Uani 1 1 d . . . N1 N 0.6420(4) 0.5266(3) 0.8110(2) 0.0392(8) Uani 1 1 d . A . N2 N 0.7138(3) 0.5708(3) 0.88518(19) 0.0360(7) Uani 1 1 d . . . N3 N 0.8725(3) 0.6788(3) 0.7861(2) 0.0377(7) Uani 1 1 d . A . N4 N 0.8982(3) 0.7128(3) 0.8618(2) 0.0369(7) Uani 1 1 d . . . N5 N 0.5995(3) 0.7488(3) 0.7967(2) 0.0379(7) Uani 1 1 d . . . N6 N 0.6537(3) 0.7462(3) 0.8733(2) 0.0361(7) Uani 1 1 d . . . C1 C 0.7137(4) 0.4995(3) 0.9337(2) 0.0375(9) Uani 1 1 d . . . C2 C 0.6382(4) 0.4083(4) 0.8889(3) 0.0436(10) Uani 1 1 d . A . H2 H 0.6194 0.3446 0.9064 0.052 Uiso 1 1 calc R . . C3 C 0.5954(4) 0.4273(3) 0.8145(3) 0.0423(10) Uani 1 1 d . . . C4 C 1.0435(4) 0.7547(3) 0.8935(3) 0.0368(8) Uani 1 1 d . . . C5 C 1.1104(4) 0.7437(3) 0.8354(3) 0.0407(9) Uani 1 1 d . A . H5 H 1.2115 0.7643 0.8398 0.049 Uiso 1 1 calc R . . C6 C 1.0002(4) 0.6963(3) 0.7691(3) 0.0400(9) Uani 1 1 d . . . C7 C 0.6024(4) 0.8147(3) 0.9148(3) 0.0366(9) Uani 1 1 d . . . C8 C 0.5139(4) 0.8628(3) 0.8621(3) 0.0399(9) Uani 1 1 d . . . H8 H 0.4628 0.9145 0.8736 0.048 Uiso 1 1 calc R . . C9 C 0.5146(4) 0.8205(3) 0.7889(3) 0.0383(9) Uani 1 1 d . . . C10 C 0.7762(4) 0.5192(3) 1.0172(3) 0.0390(9) Uani 1 1 d . . . C11 C 0.6876(5) 0.4810(4) 1.0624(3) 0.0423(9) Uani 1 1 d . . . H11 H 0.5906 0.4453 1.0376 0.051 Uiso 1 1 calc R . . C12 C 0.7377(5) 0.4939(4) 1.1412(3) 0.0486(10) Uani 1 1 d . . . H12 H 0.6758 0.4677 1.1705 0.058 Uiso 1 1 calc R . . C13 C 0.8793(5) 0.5456(5) 1.1778(3) 0.0545(12) Uani 1 1 d . . . H13 H 0.9147 0.5554 1.2324 0.065 Uiso 1 1 calc R . . C14 C 0.9699(5) 0.5833(4) 1.1345(3) 0.0473(11) Uani 1 1 d . . . H14 H 1.0675 0.6176 1.1595 0.057 Uiso 1 1 calc R . . C15 C 0.9180(4) 0.5709(3) 1.0553(3) 0.0409(9) Uani 1 1 d . . . H15 H 0.9799 0.5981 1.0264 0.049 Uiso 1 1 calc R . . C16 C 0.5264(10) 0.3523(6) 0.7429(4) 0.0360(19) Uiso 0.610(9) 1 d PD A 1 C16A C 0.4925(19) 0.3589(12) 0.7493(9) 0.061(5) Uiso 0.390(9) 1 d PD A 2 C17 C 0.5549(13) 0.2514(7) 0.7431(6) 0.048(3) Uiso 0.610(9) 1 d PD A 1 H17 H 0.6169 0.2333 0.7876 0.058 Uiso 0.610(9) 1 calc PR A 1 C17A C 0.520(2) 0.2589(11) 0.7381(9) 0.054(5) Uiso 0.390(9) 1 d PD A 2 H17A H 0.5998 0.2402 0.7732 0.065 Uiso 0.390(9) 1 calc PR A 2 C18 C 0.4910(12) 0.1798(7) 0.6774(5) 0.057(2) Uiso 0.610(9) 1 d PD A 1 H18 H 0.5059 0.1116 0.6775 0.069 Uiso 0.610(9) 1 calc PR A 1 C18A C 0.431(2) 0.1874(12) 0.6765(9) 0.068(4) Uiso 0.390(9) 1 d PD A 2 H18A H 0.4514 0.1209 0.6691 0.082 Uiso 0.390(9) 1 calc PR A 2 C19 C 0.4052(11) 0.2082(8) 0.6117(6) 0.068(3) Uiso 0.610(9) 1 d PD A 1 H19 H 0.3614 0.1590 0.5670 0.082 Uiso 0.610(9) 1 calc PR A 1 C19A C 0.313(2) 0.2135(13) 0.6270(11) 0.086(6) Uiso 0.390(9) 1 d PD A 2 H19A H 0.2504 0.1651 0.5854 0.104 Uiso 0.390(9) 1 calc PR A 2 C20 C 0.3825(11) 0.3083(8) 0.6104(6) 0.067(3) Uiso 0.610(9) 1 d PD A 1 H20 H 0.3291 0.3279 0.5640 0.080 Uiso 0.610(9) 1 calc PR A 1 C20A C 0.288(2) 0.3114(13) 0.6383(10) 0.085(5) Uiso 0.390(9) 1 d PD A 2 H20A H 0.2069 0.3295 0.6030 0.102 Uiso 0.390(9) 1 calc PR A 2 C21 C 0.4375(10) 0.3785(7) 0.6762(5) 0.054(2) Uiso 0.610(9) 1 d PD A 1 H21 H 0.4151 0.4449 0.6765 0.064 Uiso 0.610(9) 1 calc PR A 1 C21A C 0.3740(15) 0.3841(11) 0.6986(8) 0.059(4) Uiso 0.390(9) 1 d PD A 2 H21A H 0.3521 0.4503 0.7050 0.071 Uiso 0.390(9) 1 calc PR A 2 C22 C 1.1105(4) 0.8066(3) 0.9721(3) 0.0386(9) Uani 1 1 d . . . C23 C 1.2562(4) 0.8015(3) 1.0084(3) 0.0399(9) Uani 1 1 d . . . H23 H 1.3069 0.7610 0.9830 0.048 Uiso 1 1 calc R . . C24 C 1.3269(4) 0.8552(4) 1.0813(3) 0.0436(10) Uani 1 1 d . . . H24 H 1.4261 0.8518 1.1052 0.052 Uiso 1 1 calc R . . C25 C 1.2536(5) 0.9135(4) 1.1192(3) 0.0472(10) Uani 1 1 d . . . H25 H 1.3015 0.9486 1.1696 0.057 Uiso 1 1 calc R . . C26 C 1.1099(5) 0.9205(4) 1.0833(3) 0.0432(10) Uani 1 1 d . . . H26 H 1.0598 0.9613 1.1090 0.052 Uiso 1 1 calc R . . C27 C 1.0394(4) 0.8683(3) 1.0100(3) 0.0405(9) Uani 1 1 d . . . H27 H 0.9418 0.8745 0.9854 0.049 Uiso 1 1 calc R . . C28 C 1.0135(9) 0.6638(10) 0.6915(5) 0.039(3) Uiso 0.610(9) 1 d PD A 1 C28A C 1.0176(16) 0.6844(16) 0.6931(8) 0.047(6) Uiso 0.390(9) 1 d PD A 2 C29 C 1.1460(11) 0.6388(11) 0.6849(6) 0.041(4) Uiso 0.610(9) 1 d PD A 1 H29 H 1.2241 0.6412 0.7300 0.050 Uiso 0.610(9) 1 calc PR A 1 C29A C 1.1426(18) 0.6527(18) 0.6808(9) 0.047(8) Uiso 0.390(9) 1 d PD A 2 H29A H 1.2151 0.6406 0.7240 0.056 Uiso 0.390(9) 1 calc PR A 2 C30 C 1.1639(10) 0.6108(9) 0.6140(5) 0.053(3) Uiso 0.610(9) 1 d PD A 1 H30 H 1.2549 0.5960 0.6097 0.063 Uiso 0.610(9) 1 calc PR A 1 C30A C 1.1655(15) 0.6383(15) 0.6095(8) 0.055(5) Uiso 0.390(9) 1 d PD A 2 H30A H 1.2521 0.6169 0.6039 0.066 Uiso 0.390(9) 1 calc PR A 2 C31 C 1.0470(10) 0.6044(10) 0.5479(6) 0.066(3) Uiso 0.610(9) 1 d PD A 1 H31 H 1.0595 0.5858 0.4987 0.079 Uiso 0.610(9) 1 calc PR A 1 C31A C 1.0618(14) 0.6552(14) 0.5461(8) 0.061(4) Uiso 0.390(9) 1 d PD A 2 H31A H 1.0784 0.6500 0.4968 0.074 Uiso 0.390(9) 1 calc PR A 2 C32 C 0.9151(11) 0.6245(11) 0.5533(6) 0.074(3) Uiso 0.610(9) 1 d PD A 1 H32 H 0.8349 0.6150 0.5082 0.089 Uiso 0.610(9) 1 calc PR A 1 C32A C 0.9347(16) 0.6795(15) 0.5557(8) 0.069(4) Uiso 0.390(9) 1 d PD A 2 H32A H 0.8571 0.6816 0.5114 0.083 Uiso 0.390(9) 1 calc PR A 2 C33 C 0.8973(9) 0.6590(8) 0.6251(5) 0.049(2) Uiso 0.610(9) 1 d PD A 1 H33 H 0.8085 0.6786 0.6286 0.058 Uiso 0.610(9) 1 calc PR A 1 C33A C 0.9154(16) 0.7014(15) 0.6283(8) 0.059(4) Uiso 0.390(9) 1 d PD A 2 H33A H 0.8321 0.7279 0.6335 0.071 Uiso 0.390(9) 1 calc PR A 2 C34 C 0.6472(4) 0.8353(3) 0.9992(2) 0.0374(9) Uani 1 1 d . . . C35 C 0.6926(4) 0.9352(3) 1.0361(2) 0.0373(9) Uani 1 1 d . . . H35 H 0.6889 0.9895 1.0064 0.045 Uiso 1 1 calc R . . C36 C 0.7435(4) 0.9565(3) 1.1156(3) 0.0410(9) Uani 1 1 d . . . H36 H 0.7765 1.0252 1.1398 0.049 Uiso 1 1 calc R . . C37 C 0.7466(4) 0.8785(4) 1.1604(3) 0.0430(10) Uani 1 1 d . . . H37 H 0.7808 0.8933 1.2150 0.052 Uiso 1 1 calc R . . C38 C 0.6985(4) 0.7776(4) 1.1238(3) 0.0415(9) Uani 1 1 d . . . H38 H 0.6994 0.7235 1.1538 0.050 Uiso 1 1 calc R . . C39 C 0.6498(4) 0.7560(3) 1.0447(2) 0.0377(9) Uani 1 1 d . . . H39 H 0.6178 0.6872 1.0206 0.045 Uiso 1 1 calc R . . C40 C 0.4441(5) 0.8513(3) 0.7148(3) 0.0420(9) Uani 1 1 d . . . C41 C 0.3149(5) 0.8896(4) 0.7051(3) 0.0467(10) Uani 1 1 d . . . H41 H 0.2726 0.8947 0.7466 0.056 Uiso 1 1 calc R . . C42 C 0.2473(6) 0.9201(4) 0.6366(3) 0.0548(12) Uani 1 1 d . . . H42 H 0.1584 0.9446 0.6311 0.066 Uiso 1 1 calc R . . C43 C 0.3082(7) 0.9152(5) 0.5757(3) 0.0628(14) Uani 1 1 d . . . H43 H 0.2624 0.9368 0.5286 0.075 Uiso 1 1 calc R . . C44 C 0.4365(7) 0.8785(5) 0.5847(3) 0.0652(14) Uani 1 1 d . . . H44 H 0.4788 0.8749 0.5432 0.078 Uiso 1 1 calc R . . C45 C 0.5055(6) 0.8467(4) 0.6532(3) 0.0555(12) Uani 1 1 d . . . H45 H 0.5941 0.8219 0.6581 0.067 Uiso 1 1 calc R . . C46 C 0.5066(4) 0.5665(4) 0.5663(3) 0.0439(10) Uani 1 1 d . . . C47 C 0.5939(5) 0.4925(4) 0.5693(3) 0.0492(11) Uani 1 1 d . . . C48 C 0.5882(5) 0.4266(4) 0.5044(3) 0.0475(11) Uani 1 1 d . . . H48 H 0.6489 0.3770 0.5083 0.057 Uiso 1 1 calc R . . C49 C 0.7780(6) 0.4201(5) 0.6530(3) 0.0615(15) Uani 1 1 d . . . H49A H 0.8506 0.4352 0.6248 0.092 Uiso 1 1 calc R . . H49B H 0.7205 0.3513 0.6334 0.092 Uiso 1 1 calc R . . H49C H 0.8282 0.4245 0.7079 0.092 Uiso 1 1 calc R . . B1 B 0.7779(4) 0.6865(4) 0.9028(3) 0.0345(9) Uani 1 1 d . . . H1 H 0.8211 0.7068 0.9597 0.041 Uiso 1 1 calc R . . O3 O 0.9435(7) 0.0766(6) 0.6569(5) 0.125(2) Uani 1 1 d . . . C50 C 0.8723(9) 0.0255(9) 0.7051(5) 0.114(4) Uani 1 1 d . . . H50A H 0.8908 0.0721 0.7537 0.136 Uiso 1 1 calc R . . H50B H 0.7655 0.0120 0.6798 0.136 Uiso 1 1 calc R . . C51 C 0.9092(5) -0.0587(6) 0.7221(4) 0.0678(18) Uani 1 1 d . . . H51A H 0.9028 -0.1031 0.6748 0.102 Uiso 1 1 calc R . . H51B H 0.8431 -0.0922 0.7487 0.102 Uiso 1 1 calc R . . H51C H 1.0101 -0.0453 0.7557 0.102 Uiso 1 1 calc R . . C52 C 0.9273(10) 0.1712(8) 0.6535(6) 0.092(2) Uani 1 1 d . . . H52A H 0.8343 0.1709 0.6139 0.110 Uiso 1 1 calc R . . H52B H 0.9168 0.1998 0.7035 0.110 Uiso 1 1 calc R . . C53 C 1.020(2) 0.2259(15) 0.6397(17) 0.314(16) Uani 1 1 d . . . H53A H 1.1011 0.2497 0.6867 0.471 Uiso 1 1 calc R . . H53B H 0.9819 0.2845 0.6198 0.471 Uiso 1 1 calc R . . H53C H 1.0552 0.1898 0.6009 0.471 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0335(3) 0.0470(4) 0.0339(3) -0.0025(3) 0.0043(2) 0.0067(3) O1 0.0454(16) 0.062(2) 0.0352(15) -0.0090(14) 0.0030(12) 0.0182(15) O2 0.065(2) 0.081(3) 0.0331(16) -0.0077(16) -0.0012(14) 0.0405(19) N1 0.0366(17) 0.044(2) 0.0307(17) -0.0017(14) 0.0057(13) 0.0007(14) N2 0.0295(15) 0.0407(18) 0.0332(17) -0.0014(14) 0.0044(12) 0.0050(13) N3 0.0276(15) 0.045(2) 0.0365(17) -0.0004(14) 0.0058(12) 0.0058(13) N4 0.0289(15) 0.0425(19) 0.0351(17) 0.0020(14) 0.0053(13) 0.0037(13) N5 0.0320(16) 0.0419(19) 0.0346(17) -0.0022(14) 0.0053(13) 0.0041(14) N6 0.0285(15) 0.0385(18) 0.0371(17) -0.0026(14) 0.0061(13) 0.0049(13) C1 0.0275(17) 0.042(2) 0.041(2) 0.0023(17) 0.0091(15) 0.0071(15) C2 0.038(2) 0.038(2) 0.049(2) -0.0029(18) 0.0095(17) 0.0000(17) C3 0.035(2) 0.039(2) 0.047(2) -0.0018(18) 0.0074(17) 0.0013(16) C4 0.0301(18) 0.034(2) 0.045(2) 0.0027(17) 0.0104(15) 0.0058(15) C5 0.0282(18) 0.046(2) 0.047(2) 0.0022(19) 0.0119(16) 0.0065(16) C6 0.0340(19) 0.043(2) 0.044(2) 0.0043(18) 0.0121(16) 0.0076(16) C7 0.0252(17) 0.036(2) 0.045(2) -0.0014(17) 0.0083(15) 0.0016(15) C8 0.0307(19) 0.039(2) 0.044(2) -0.0009(17) 0.0053(16) 0.0040(16) C9 0.0263(17) 0.036(2) 0.046(2) -0.0006(17) 0.0045(15) 0.0003(15) C10 0.0328(19) 0.040(2) 0.043(2) 0.0022(17) 0.0079(16) 0.0076(16) C11 0.036(2) 0.047(2) 0.043(2) 0.0091(19) 0.0084(16) 0.0069(17) C12 0.051(3) 0.053(3) 0.046(2) 0.014(2) 0.017(2) 0.014(2) C13 0.049(3) 0.071(3) 0.041(2) 0.010(2) 0.005(2) 0.016(2) C14 0.032(2) 0.065(3) 0.039(2) 0.005(2) 0.0022(16) 0.0061(19) C15 0.0311(19) 0.044(2) 0.047(2) 0.0073(18) 0.0104(16) 0.0070(16) C22 0.0310(19) 0.040(2) 0.043(2) 0.0041(17) 0.0092(16) 0.0036(16) C23 0.0305(18) 0.040(2) 0.045(2) 0.0008(18) 0.0082(16) 0.0037(16) C24 0.034(2) 0.045(2) 0.048(2) 0.0044(19) 0.0057(17) 0.0052(17) C25 0.041(2) 0.049(3) 0.045(2) -0.003(2) 0.0106(18) 0.0000(19) C26 0.037(2) 0.042(2) 0.046(2) -0.0034(19) 0.0103(17) 0.0056(17) C27 0.0316(19) 0.039(2) 0.049(2) -0.0028(18) 0.0095(16) 0.0068(16) C34 0.0240(17) 0.044(2) 0.041(2) 0.0003(17) 0.0076(14) 0.0058(15) C35 0.0311(18) 0.039(2) 0.039(2) 0.0010(17) 0.0082(15) 0.0040(15) C36 0.0332(19) 0.042(2) 0.044(2) -0.0035(18) 0.0074(16) 0.0067(16) C37 0.036(2) 0.053(3) 0.037(2) 0.0008(19) 0.0070(16) 0.0101(18) C38 0.035(2) 0.048(2) 0.044(2) 0.0071(19) 0.0131(16) 0.0103(17) C39 0.0281(18) 0.040(2) 0.044(2) 0.0006(17) 0.0107(15) 0.0072(15) C40 0.041(2) 0.038(2) 0.043(2) 0.0019(18) 0.0096(17) 0.0030(17) C41 0.041(2) 0.047(3) 0.047(3) 0.002(2) 0.0059(18) 0.0058(19) C42 0.056(3) 0.057(3) 0.049(3) 0.013(2) 0.008(2) 0.015(2) C43 0.075(3) 0.059(3) 0.045(3) 0.009(2) -0.001(2) 0.017(3) C44 0.084(4) 0.071(4) 0.044(3) 0.011(3) 0.022(3) 0.017(3) C45 0.058(3) 0.059(3) 0.050(3) 0.007(2) 0.015(2) 0.015(2) C46 0.035(2) 0.055(3) 0.037(2) -0.0054(19) 0.0062(16) 0.0087(18) C47 0.042(2) 0.066(3) 0.036(2) 0.000(2) 0.0043(17) 0.018(2) C48 0.040(2) 0.057(3) 0.040(2) -0.002(2) 0.0023(17) 0.0144(19) C49 0.054(3) 0.087(4) 0.042(3) 0.001(3) -0.001(2) 0.038(3) B1 0.0258(19) 0.039(2) 0.034(2) 0.0007(18) 0.0051(15) 0.0021(16) O3 0.088(4) 0.133(6) 0.145(6) -0.004(5) 0.040(4) -0.003(4) C50 0.081(5) 0.160(9) 0.066(4) 0.012(5) 0.011(4) -0.060(6) C51 0.031(2) 0.090(5) 0.072(4) -0.014(3) 0.001(2) 0.021(3) C52 0.090(5) 0.099(6) 0.106(6) 0.053(5) 0.044(5) 0.025(5) C53 0.171(17) 0.155(18) 0.60(5) 0.08(2) 0.03(2) 0.084(14) _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 O1 1.904(3) . ? Fe1 O2 2.328(3) . ? Fe1 N1 2.107(4) . ? Fe1 N3 2.108(3) . ? Fe1 N5 2.213(4) . ? O1 C46 1.329(5) . ? O2 C47 1.388(6) . ? O2 C49 1.423(6) . ? N1 C3 1.354(6) . ? N2 N1 1.369(5) . ? N2 C1 1.364(6) . ? N2 B1 1.549(6) . ? N3 C6 1.338(5) . ? N4 N3 1.354(5) . ? N4 C4 1.369(5) . ? N4 B1 1.551(6) . ? N5 C9 1.354(6) . ? N6 N5 1.360(5) . ? N6 C7 1.366(5) . ? N6 B1 1.553(6) . ? C1 C2 1.381(6) . ? C1 C10 1.460(6) . ? C2 H2 0.9500 . ? C2 C3 1.370(7) . ? C3 C16 1.494(8) . ? C3 C16A 1.454(15) . ? C4 C5 1.385(6) . ? C4 C22 1.458(6) . ? C5 H5 0.9500 . ? C5 C6 1.397(6) . ? C6 C28 1.482(10) . ? C6 C28A 1.433(15) . ? C7 C8 1.388(6) . ? C7 C34 1.468(6) . ? C8 H8 0.9500 . ? C8 C9 1.398(6) . ? C9 C40 1.473(6) . ? C10 C11 1.409(6) . ? C10 C15 1.393(6) . ? C11 H11 0.9500 . ? C11 C12 1.372(7) . ? C12 H12 0.9500 . ? C12 C13 1.387(7) . ? C13 H13 0.9500 . ? C13 C14 1.394(7) . ? C14 H14 0.9500 . ? C14 C15 1.378(6) . ? C15 H15 0.9500 . ? C16 C17 1.424(12) . ? C16 C21 1.400(10) . ? C16A C17A 1.414(16) . ? C16A C21A 1.378(15) . ? C17 H17 0.9500 . ? C17 C18 1.392(11) . ? C17A H17A 0.9500 . ? C17A C18A 1.393(15) . ? C18 H18 0.9500 . ? C18 C19 1.388(13) . ? C18A H18A 0.9500 . ? C18A C19A 1.364(18) . ? C19 H19 0.9500 . ? C19 C20 1.398(13) . ? C19A H19A 0.9500 . ? C19A C20A 1.384(18) . ? C20 H20 0.9500 . ? C20 C21 1.377(12) . ? C20A H20A 0.9500 . ? C20A C21A 1.379(17) . ? C21 H21 0.9500 . ? C21A H21A 0.9500 . ? C22 C23 1.400(6) . ? C22 C27 1.396(6) . ? C23 H23 0.9500 . ? C23 C24 1.388(6) . ? C24 H24 0.9500 . ? C24 C25 1.384(7) . ? C25 H25 0.9500 . ? C25 C26 1.389(7) . ? C26 H26 0.9500 . ? C26 C27 1.386(6) . ? C27 H27 0.9500 . ? C28 C29 1.401(10) . ? C28 C33 1.402(10) . ? C28A C29A 1.402(14) . ? C28A C33A 1.387(14) . ? C29 H29 0.9500 . ? C29 C30 1.371(10) . ? C29A H29A 0.9500 . ? C29A C30A 1.375(14) . ? C30 H30 0.9500 . ? C30 C31 1.398(12) . ? C30A H30A 0.9500 . ? C30A C31A 1.377(15) . ? C31 H31 0.9500 . ? C31 C32 1.365(13) . ? C31A H31A 0.9500 . ? C31A C32A 1.365(15) . ? C32 H32 0.9500 . ? C32 C33 1.408(12) . ? C32A H32A 0.9500 . ? C32A C33A 1.394(15) . ? C33 H33 0.9500 . ? C33A H33A 0.9500 . ? C34 C35 1.389(6) . ? C34 C39 1.413(6) . ? C35 H35 0.9500 . ? C35 C36 1.386(6) . ? C36 H36 0.9500 . ? C36 C37 1.389(7) . ? C37 H37 0.9500 . ? C37 C38 1.400(7) . ? C38 H38 0.9500 . ? C38 C39 1.377(6) . ? C39 H39 0.9500 . ? C40 C41 1.396(7) . ? C40 C45 1.400(7) . ? C41 H41 0.9500 . ? C41 C42 1.380(7) . ? C42 H42 0.9500 . ? C42 C43 1.385(8) . ? C43 H43 0.9500 . ? C43 C44 1.377(9) . ? C44 H44 0.9500 . ? C44 C45 1.391(8) . ? C45 H45 0.9500 . ? C46 C47 1.395(7) . ? C46 C48 1.388(6) 2_666 ? C47 C48 1.389(7) . ? C48 C46 1.388(6) 2_666 ? C48 H48 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? B1 H1 1.0000 . ? O3 C50 1.415(10) . ? O3 C52 1.311(11) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C50 C51 1.281(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 C53 1.16(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 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 O1 Fe1 O2 75.22(13) . . ? O1 Fe1 N1 131.92(15) . . ? O1 Fe1 N3 138.70(16) . . ? O1 Fe1 N5 98.90(13) . . ? N1 Fe1 O2 91.76(15) . . ? N1 Fe1 N3 88.26(14) . . ? N1 Fe1 N5 91.81(14) . . ? N3 Fe1 O2 97.87(13) . . ? N3 Fe1 N5 86.94(13) . . ? N5 Fe1 O2 174.09(12) . . ? C46 O1 Fe1 122.6(3) . . ? C47 O2 Fe1 109.1(3) . . ? C47 O2 C49 118.2(4) . . ? C49 O2 Fe1 132.6(3) . . ? N2 N1 Fe1 115.2(3) . . ? C3 N1 Fe1 138.5(3) . . ? C3 N1 N2 106.0(4) . . ? N1 N2 B1 119.8(4) . . ? C1 N2 N1 110.1(3) . . ? C1 N2 B1 130.1(3) . . ? N4 N3 Fe1 114.5(2) . . ? C6 N3 Fe1 137.5(3) . . ? C6 N3 N4 107.9(3) . . ? N3 N4 C4 109.9(3) . . ? N3 N4 B1 120.5(3) . . ? C4 N4 B1 128.8(3) . . ? N6 N5 Fe1 111.3(3) . . ? C9 N5 Fe1 140.3(3) . . ? C9 N5 N6 107.5(3) . . ? N5 N6 C7 110.1(3) . . ? N5 N6 B1 120.5(3) . . ? C7 N6 B1 128.4(4) . . ? N2 C1 C2 106.8(4) . . ? N2 C1 C10 125.6(4) . . ? C2 C1 C10 127.5(4) . . ? C1 C2 H2 126.6 . . ? C3 C2 C1 106.9(4) . . ? C3 C2 H2 126.6 . . ? N1 C3 C2 110.2(4) . . ? N1 C3 C16 121.1(5) . . ? N1 C3 C16A 122.3(7) . . ? C2 C3 C16 128.1(5) . . ? C2 C3 C16A 126.5(8) . . ? C16A C3 C16 15.3(7) . . ? N4 C4 C5 106.7(4) . . ? N4 C4 C22 125.8(4) . . ? C5 C4 C22 127.4(4) . . ? C4 C5 H5 126.7 . . ? C4 C5 C6 106.6(3) . . ? C6 C5 H5 126.7 . . ? N3 C6 C5 109.0(4) . . ? N3 C6 C28 122.3(5) . . ? N3 C6 C28A 125.4(7) . . ? C5 C6 C28 128.6(5) . . ? C5 C6 C28A 124.8(8) . . ? C28A C6 C28 10.5(10) . . ? N6 C7 C8 106.9(4) . . ? N6 C7 C34 123.9(4) . . ? C8 C7 C34 129.1(4) . . ? C7 C8 H8 126.6 . . ? C7 C8 C9 106.8(4) . . ? C9 C8 H8 126.6 . . ? N5 C9 C8 108.7(4) . . ? N5 C9 C40 124.1(4) . . ? C8 C9 C40 127.1(4) . . ? C11 C10 C1 117.6(4) . . ? C15 C10 C1 124.8(4) . . ? C15 C10 C11 117.7(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 C10 121.8(4) . . ? C12 C11 H11 119.1 . . ? C11 C12 H12 120.3 . . ? C11 C12 C13 119.5(5) . . ? C13 C12 H12 120.3 . . ? C12 C13 H13 120.0 . . ? C12 C13 C14 120.0(5) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C10 C15 H15 119.5 . . ? C14 C15 C10 121.0(4) . . ? C14 C15 H15 119.5 . . ? C17 C16 C3 118.2(6) . . ? C21 C16 C3 122.2(7) . . ? C21 C16 C17 119.6(7) . . ? C17A C16A C3 116.0(11) . . ? C21A C16A C3 125.5(12) . . ? C21A C16A C17A 118.5(13) . . ? C16 C17 H17 120.3 . . ? C18 C17 C16 119.4(10) . . ? C18 C17 H17 120.3 . . ? C16A C17A H17A 119.4 . . ? C18A C17A C16A 121.3(15) . . ? C18A C17A H17A 119.4 . . ? C17 C18 H18 120.1 . . ? C19 C18 C17 119.8(10) . . ? C19 C18 H18 120.1 . . ? C17A C18A H18A 120.3 . . ? C19A C18A C17A 119.4(15) . . ? C19A C18A H18A 120.3 . . ? C18 C19 H19 119.6 . . ? C18 C19 C20 120.9(9) . . ? C20 C19 H19 119.6 . . ? C18A C19A H19A 120.5 . . ? C18A C19A C20A 119.0(16) . . ? C20A C19A H19A 120.5 . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.0(9) . . ? C21 C20 H20 120.0 . . ? C19A C20A H20A 118.6 . . ? C21A C20A C19A 122.9(15) . . ? C21A C20A H20A 118.6 . . ? C16 C21 H21 119.9 . . ? C20 C21 C16 120.1(9) . . ? C20 C21 H21 119.9 . . ? C16A C21A C20A 118.9(14) . . ? C16A C21A H21A 120.6 . . ? C20A C21A H21A 120.6 . . ? C23 C22 C4 118.7(4) . . ? C27 C22 C4 122.4(4) . . ? C27 C22 C23 118.6(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.8 . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 120.1 . . ? C24 C25 C26 119.8(4) . . ? C26 C25 H25 120.1 . . ? C25 C26 H26 119.9 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26 119.9 . . ? C22 C27 H27 119.7 . . ? C26 C27 C22 120.6(4) . . ? C26 C27 H27 119.7 . . ? C29 C28 C6 118.9(7) . . ? C29 C28 C33 119.9(8) . . ? C33 C28 C6 121.2(7) . . ? C29A C28A C6 120.1(11) . . ? C33A C28A C6 123.7(11) . . ? C33A C28A C29A 116.1(13) . . ? C28 C29 H29 119.7 . . ? C30 C29 C28 120.6(9) . . ? C30 C29 H29 119.7 . . ? C28A C29A H29A 118.4 . . ? C30A C29A C28A 123.3(14) . . ? C30A C29A H29A 118.4 . . ? C29 C30 H30 120.3 . . ? C29 C30 C31 119.4(9) . . ? C31 C30 H30 120.3 . . ? C29A C30A H30A 120.3 . . ? C29A C30A C31A 119.4(13) . . ? C31A C30A H30A 120.3 . . ? C30 C31 H31 119.6 . . ? C32 C31 C30 120.9(9) . . ? C32 C31 H31 119.6 . . ? C30A C31A H31A 120.7 . . ? C32A C31A C30A 118.6(13) . . ? C32A C31A H31A 120.7 . . ? C31 C32 H32 119.8 . . ? C31 C32 C33 120.5(9) . . ? C33 C32 H32 119.8 . . ? C31A C32A H32A 119.0 . . ? C31A C32A C33A 122.0(13) . . ? C33A C32A H32A 119.0 . . ? C28 C33 C32 118.5(8) . . ? C28 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C28A C33A C32A 120.0(13) . . ? C28A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C35 C34 C7 119.7(4) . . ? C35 C34 C39 118.5(4) . . ? C39 C34 C7 121.9(4) . . ? C34 C35 H35 119.6 . . ? C36 C35 C34 120.8(4) . . ? C36 C35 H35 119.6 . . ? C35 C36 H36 119.6 . . ? C35 C36 C37 120.7(4) . . ? C37 C36 H36 119.6 . . ? C36 C37 H37 120.5 . . ? C36 C37 C38 118.9(4) . . ? C38 C37 H37 120.5 . . ? C37 C38 H38 119.7 . . ? C39 C38 C37 120.6(4) . . ? C39 C38 H38 119.7 . . ? C34 C39 H39 119.7 . . ? C38 C39 C34 120.5(4) . . ? C38 C39 H39 119.7 . . ? C41 C40 C9 120.1(4) . . ? C41 C40 C45 118.0(5) . . ? C45 C40 C9 121.9(4) . . ? C40 C41 H41 119.3 . . ? C42 C41 C40 121.4(5) . . ? C42 C41 H41 119.3 . . ? C41 C42 H42 119.8 . . ? C41 C42 C43 120.4(5) . . ? C43 C42 H42 119.8 . . ? C42 C43 H43 120.6 . . ? C44 C43 C42 118.8(5) . . ? C44 C43 H43 120.6 . . ? C43 C44 H44 119.2 . . ? C43 C44 C45 121.6(6) . . ? C45 C44 H44 119.2 . . ? C40 C45 H45 120.1 . . ? C44 C45 C40 119.9(5) . . ? C44 C45 H45 120.1 . . ? O1 C46 C47 119.9(4) . . ? O1 C46 C48 122.1(4) . 2_666 ? C48 C46 C47 118.1(4) 2_666 . ? O2 C47 C46 113.1(4) . . ? O2 C47 C48 124.8(4) . . ? C48 C47 C46 122.1(4) . . ? C46 C48 C47 119.8(5) 2_666 . ? C46 C48 H48 120.1 2_666 . ? C47 C48 H48 120.1 . . ? O2 C49 H49A 109.5 . . ? O2 C49 H49B 109.5 . . ? O2 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N2 B1 N4 110.4(3) . . ? N2 B1 N6 109.3(3) . . ? N2 B1 H1 109.5 . . ? N4 B1 N6 108.7(4) . . ? N4 B1 H1 109.5 . . ? N6 B1 H1 109.5 . . ? C52 O3 C50 115.2(8) . . ? O3 C50 H50A 108.1 . . ? O3 C50 H50B 108.1 . . ? H50A C50 H50B 107.3 . . ? C51 C50 O3 116.7(10) . . ? C51 C50 H50A 108.1 . . ? C51 C50 H50B 108.1 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O3 C52 H52A 108.0 . . ? O3 C52 H52B 108.0 . . ? H52A C52 H52B 107.3 . . ? C53 C52 O3 117.0(12) . . ? C53 C52 H52A 108.0 . . ? C53 C52 H52B 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C46 C47 3.2(7) . . . . ? Fe1 O1 C46 C48 -177.4(4) . . . 2_666 ? Fe1 O2 C47 C46 -2.5(6) . . . . ? Fe1 O2 C47 C48 178.3(5) . . . . ? Fe1 N1 C3 C2 172.4(3) . . . . ? Fe1 N1 C3 C16 0.0(8) . . . . ? Fe1 N1 C3 C16A -17.9(12) . . . . ? Fe1 N3 C6 C5 174.9(3) . . . . ? Fe1 N3 C6 C28 -7.5(9) . . . . ? Fe1 N3 C6 C28A 4.6(12) . . . . ? Fe1 N5 C9 C8 167.0(3) . . . . ? Fe1 N5 C9 C40 -16.6(7) . . . . ? O1 Fe1 O2 C47 3.1(4) . . . . ? O1 Fe1 O2 C49 179.5(6) . . . . ? O1 Fe1 N1 N2 -148.8(2) . . . . ? O1 Fe1 N1 C3 38.4(5) . . . . ? O1 Fe1 N3 N4 138.9(3) . . . . ? O1 Fe1 N3 C6 -36.5(6) . . . . ? O1 Fe1 N5 N6 164.2(3) . . . . ? O1 Fe1 N5 C9 -3.2(5) . . . . ? O1 C46 C47 O2 0.1(7) . . . . ? O1 C46 C47 C48 179.4(5) . . . . ? O2 Fe1 O1 C46 -3.3(4) . . . . ? O2 Fe1 N1 N2 139.6(3) . . . . ? O2 Fe1 N1 C3 -33.2(4) . . . . ? O2 Fe1 N3 N4 -144.6(3) . . . . ? O2 Fe1 N3 C6 40.1(5) . . . . ? O2 Fe1 N5 N6 158.4(14) . . . . ? O2 Fe1 N5 C9 -9.1(18) . . . . ? O2 C47 C48 C46 179.2(5) . . . 2_666 ? N1 Fe1 O1 C46 -82.1(4) . . . . ? N1 Fe1 O2 C47 136.2(4) . . . . ? N1 Fe1 O2 C49 -47.4(5) . . . . ? N1 Fe1 N3 N4 -53.0(3) . . . . ? N1 Fe1 N3 C6 131.6(5) . . . . ? N1 Fe1 N5 N6 31.2(3) . . . . ? N1 Fe1 N5 C9 -136.2(5) . . . . ? N1 N2 C1 C2 -0.8(4) . . . . ? N1 N2 C1 C10 -178.1(4) . . . . ? N1 N2 B1 N4 -62.8(4) . . . . ? N1 N2 B1 N6 56.8(5) . . . . ? N1 C3 C16 C17 144.4(7) . . . . ? N1 C3 C16 C21 -34.6(11) . . . . ? N1 C3 C16A C17A 141.0(13) . . . . ? N1 C3 C16A C21A -39(2) . . . . ? N2 N1 C3 C2 -0.7(5) . . . . ? N2 N1 C3 C16 -173.2(5) . . . . ? N2 N1 C3 C16A 168.9(10) . . . . ? N2 C1 C2 C3 0.3(5) . . . . ? N2 C1 C10 C11 130.1(4) . . . . ? N2 C1 C10 C15 -51.3(6) . . . . ? N3 Fe1 O1 C46 81.7(4) . . . . ? N3 Fe1 O2 C47 -135.3(4) . . . . ? N3 Fe1 O2 C49 41.1(6) . . . . ? N3 Fe1 N1 N2 41.7(3) . . . . ? N3 Fe1 N1 C3 -131.0(4) . . . . ? N3 Fe1 N5 N6 -56.9(3) . . . . ? N3 Fe1 N5 C9 135.6(5) . . . . ? N3 N4 C4 C5 -1.6(5) . . . . ? N3 N4 C4 C22 174.8(4) . . . . ? N3 N4 B1 N2 49.4(5) . . . . ? N3 N4 B1 N6 -70.5(5) . . . . ? N3 C6 C28 C29 -149.7(10) . . . . ? N3 C6 C28 C33 31.1(14) . . . . ? N3 C6 C28A C29A -146.8(16) . . . . ? N3 C6 C28A C33A 32(2) . . . . ? N4 N3 C6 C5 -0.6(5) . . . . ? N4 N3 C6 C28 177.0(6) . . . . ? N4 N3 C6 C28A -171.0(11) . . . . ? N4 C4 C5 C6 1.1(5) . . . . ? N4 C4 C22 C23 149.1(4) . . . . ? N4 C4 C22 C27 -36.6(7) . . . . ? N5 Fe1 O1 C46 177.3(4) . . . . ? N5 Fe1 O2 C47 9.0(17) . . . . ? N5 Fe1 O2 C49 -174.5(13) . . . . ? N5 Fe1 N1 N2 -45.1(3) . . . . ? N5 Fe1 N1 C3 142.1(4) . . . . ? N5 Fe1 N3 N4 38.9(3) . . . . ? N5 Fe1 N3 C6 -136.5(5) . . . . ? N5 N6 C7 C8 -0.6(5) . . . . ? N5 N6 C7 C34 -176.1(4) . . . . ? N5 N6 B1 N2 -74.3(5) . . . . ? N5 N6 B1 N4 46.2(5) . . . . ? N5 C9 C40 C41 152.6(4) . . . . ? N5 C9 C40 C45 -29.6(7) . . . . ? N6 N5 C9 C8 -0.8(4) . . . . ? N6 N5 C9 C40 175.6(4) . . . . ? N6 C7 C8 C9 0.2(5) . . . . ? N6 C7 C34 C35 130.2(4) . . . . ? N6 C7 C34 C39 -47.8(6) . . . . ? C1 N2 N1 Fe1 -174.1(2) . . . . ? C1 N2 N1 C3 0.9(4) . . . . ? C1 N2 B1 N4 118.4(4) . . . . ? C1 N2 B1 N6 -122.1(4) . . . . ? C1 C2 C3 N1 0.3(5) . . . . ? C1 C2 C3 C16 172.0(6) . . . . ? C1 C2 C3 C16A -168.8(10) . . . . ? C1 C10 C11 C12 178.8(4) . . . . ? C1 C10 C15 C14 -177.9(4) . . . . ? C2 C1 C10 C11 -46.6(6) . . . . ? C2 C1 C10 C15 131.9(5) . . . . ? C2 C3 C16 C17 -26.5(11) . . . . ? C2 C3 C16 C21 154.4(7) . . . . ? C2 C3 C16A C17A -51(2) . . . . ? C2 C3 C16A C21A 129.3(15) . . . . ? C3 C16 C17 C18 179.4(9) . . . . ? C3 C16 C21 C20 176.6(8) . . . . ? C3 C16A C17A C18A -178.4(16) . . . . ? C3 C16A C21A C20A 178.6(16) . . . . ? C4 N4 N3 Fe1 -175.3(3) . . . . ? C4 N4 N3 C6 1.4(5) . . . . ? C4 N4 B1 N2 -119.0(4) . . . . ? C4 N4 B1 N6 121.1(4) . . . . ? C4 C5 C6 N3 -0.3(5) . . . . ? C4 C5 C6 C28 -177.7(7) . . . . ? C4 C5 C6 C28A 170.1(10) . . . . ? C4 C22 C23 C24 175.9(4) . . . . ? C4 C22 C27 C26 -176.6(4) . . . . ? C5 C4 C22 C23 -35.3(7) . . . . ? C5 C4 C22 C27 139.0(5) . . . . ? C5 C6 C28 C29 27.4(15) . . . . ? C5 C6 C28 C33 -151.9(8) . . . . ? C5 C6 C28A C29A 44(2) . . . . ? C5 C6 C28A C33A -136.5(16) . . . . ? C6 C28 C29 C30 -178.4(11) . . . . ? C6 C28 C33 C32 -178.0(10) . . . . ? C6 C28A C29A C30A 179.0(19) . . . . ? C6 C28A C33A C32A -174.4(16) . . . . ? C7 N6 N5 Fe1 -170.7(3) . . . . ? C7 N6 N5 C9 0.9(4) . . . . ? C7 N6 B1 N2 118.2(4) . . . . ? C7 N6 B1 N4 -121.2(4) . . . . ? C7 C8 C9 N5 0.4(5) . . . . ? C7 C8 C9 C40 -175.9(4) . . . . ? C7 C34 C35 C36 -176.2(4) . . . . ? C7 C34 C39 C38 177.1(4) . . . . ? C8 C7 C34 C35 -44.1(6) . . . . ? C8 C7 C34 C39 137.9(4) . . . . ? C8 C9 C40 C41 -31.7(7) . . . . ? C8 C9 C40 C45 146.2(5) . . . . ? C9 C40 C41 C42 179.3(4) . . . . ? C9 C40 C45 C44 -178.7(5) . . . . ? C10 C1 C2 C3 177.5(4) . . . . ? C10 C11 C12 C13 -0.2(8) . . . . ? C11 C10 C15 C14 0.6(7) . . . . ? C11 C12 C13 C14 -0.4(8) . . . . ? C12 C13 C14 C15 1.2(8) . . . . ? C13 C14 C15 C10 -1.3(8) . . . . ? C15 C10 C11 C12 0.1(7) . . . . ? C16 C3 C16A C17A 51(2) . . . . ? C16 C3 C16A C21A -129(4) . . . . ? C16 C17 C18 C19 2.6(16) . . . . ? C16A C3 C16 C17 -116(3) . . . . ? C16A C3 C16 C21 65(3) . . . . ? C16A C17A C18A C19A -1(3) . . . . ? C17 C16 C21 C20 -2.4(14) . . . . ? C17 C18 C19 C20 0.3(16) . . . . ? C17A C16A C21A C20A -1(3) . . . . ? C17A C18A C19A C20A 1(3) . . . . ? C18 C19 C20 C21 -4.2(16) . . . . ? C18A C19A C20A C21A -1(3) . . . . ? C19 C20 C21 C16 5.3(15) . . . . ? C19A C20A C21A C16A 1(3) . . . . ? C21 C16 C17 C18 -1.5(15) . . . . ? C21A C16A C17A C18A 1(3) . . . . ? C22 C4 C5 C6 -175.1(4) . . . . ? C22 C23 C24 C25 0.7(7) . . . . ? C23 C22 C27 C26 -2.3(7) . . . . ? C23 C24 C25 C26 -1.8(8) . . . . ? C24 C25 C26 C27 0.8(8) . . . . ? C25 C26 C27 C22 1.2(8) . . . . ? C27 C22 C23 C24 1.3(7) . . . . ? C28 C6 C28A C29A -70(4) . . . . ? C28 C6 C28A C33A 109(5) . . . . ? C28 C29 C30 C31 -2(2) . . . . ? C28A C6 C28 C29 100(5) . . . . ? C28A C6 C28 C33 -79(4) . . . . ? C28A C29A C30A C31A 0(3) . . . . ? C29 C28 C33 C32 2.8(18) . . . . ? C29 C30 C31 C32 -1(2) . . . . ? C29A C28A C33A C32A 5(3) . . . . ? C29A C30A C31A C32A -4(3) . . . . ? C30 C31 C32 C33 4(2) . . . . ? C30A C31A C32A C33A 9(3) . . . . ? C31 C32 C33 C28 -5.5(19) . . . . ? C31A C32A C33A C28A -9(3) . . . . ? C33 C28 C29 C30 1(2) . . . . ? C33A C28A C29A C30A 0(3) . . . . ? C34 C7 C8 C9 175.3(4) . . . . ? C34 C35 C36 C37 -1.6(6) . . . . ? C35 C34 C39 C38 -0.9(5) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C36 C37 C38 C39 0.4(6) . . . . ? C37 C38 C39 C34 -0.2(6) . . . . ? C39 C34 C35 C36 1.8(6) . . . . ? C40 C41 C42 C43 -1.2(8) . . . . ? C41 C40 C45 C44 -0.8(8) . . . . ? C41 C42 C43 C44 0.6(9) . . . . ? C42 C43 C44 C45 -0.1(10) . . . . ? C43 C44 C45 C40 0.2(9) . . . . ? C45 C40 C41 C42 1.3(7) . . . . ? C46 C47 C48 C46 0.1(9) . . . 2_666 ? C48 C46 C47 O2 -179.3(5) 2_666 . . . ? C48 C46 C47 C48 -0.1(9) 2_666 . . . ? C49 O2 C47 C46 -179.5(5) . . . . ? C49 O2 C47 C48 1.3(9) . . . . ? B1 N2 N1 Fe1 6.9(4) . . . . ? B1 N2 N1 C3 -178.1(3) . . . . ? B1 N2 C1 C2 178.1(4) . . . . ? B1 N2 C1 C10 0.9(6) . . . . ? B1 N4 N3 Fe1 14.3(5) . . . . ? B1 N4 N3 C6 -169.0(4) . . . . ? B1 N4 C4 C5 167.8(4) . . . . ? B1 N4 C4 C22 -15.9(7) . . . . ? B1 N6 N5 Fe1 19.7(4) . . . . ? B1 N6 N5 C9 -168.6(3) . . . . ? B1 N6 C7 C8 167.8(4) . . . . ? B1 N6 C7 C34 -7.6(7) . . . . ? C50 O3 C52 C53 152.7(19) . . . . ? C52 O3 C50 C51 -166.3(8) . . . . ? # end Validation Reply Form loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1 -1 -11 0.0090 -1.0004 -1.0000 -10.9992 0.4959 0.9324 -0.1152 1 1 11 0.0160 1.0004 1.0000 10.9992 -0.4959 -0.9324 0.1152 0 -8 5 0.0230 0.0001 -8.0001 4.9999 0.7670 -0.5940 0.1196 0 8 -5 0.0100 -0.0001 8.0001 -4.9999 -0.7670 0.5940 -0.1196 6 -4 -2 0.1493 6.0002 -4.0002 -2.0003 0.1473 -0.1195 0.9917 -6 4 2 0.1493 -6.0002 4.0002 2.0003 -0.1473 0.1195 -0.9917 #==END data_Complex2F _database_code_depnum_ccdc_archive 'CCDC 890624' #TrackingRef '- Fiedler Dalton 2012 - Revised.cif' _audit_creation_date 2012-06-06 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C100 H79 B2 Fe2 N13 O2, 1.67(C2 H4 Cl2)' _chemical_formula_sum 'C103.35 H85.69 B2 Cl3.35 Fe2 N13 O2' _chemical_formula_weight 1793.68 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C53 H43 N6 O2 B' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_H-M_alt 'P 1 n 1' _space_group_name_Hall 'P -2yac' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x+1/2, -y, z+1/2' _cell_length_a 13.4895(3) _cell_length_b 10.0544(3) _cell_length_c 32.9607(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.806(3) _cell_angle_gamma 90.00 _cell_volume 4438.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7187 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.6156 _cell_measurement_theta_min 3.4111 _exptl_absorpt_coefficient_mu 4.018 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1863 _exptl_crystal_size_max 0.3535 _exptl_crystal_size_mid 0.0751 _exptl_crystal_size_min 0.0419 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_unetI/netI 0.0654 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 23318 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.78 _diffrn_reflns_theta_min 3.41 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -39.00 -13.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -93.00 -2.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 125.0000 30.0000 91 #__ type_ start__ end____ width___ exp.time_ 3 omega -115.00 -90.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -137.0000 -8.0000 25 #__ type_ start__ end____ width___ exp.time_ 4 omega -117.00 -10.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -77.0000 -60.0000 107 #__ type_ start__ end____ width___ exp.time_ 5 omega -114.00 -88.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega 29.00 65.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 7 omega 112.00 170.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 -180.0000 58 #__ type_ start__ end____ width___ exp.time_ 8 omega 101.00 171.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 125.0000 30.0000 70 #__ type_ start__ end____ width___ exp.time_ 9 omega 78.00 169.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 -150.0000 91 #__ type_ start__ end____ width___ exp.time_ 10 omega 48.00 120.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -125.0000 -120.0000 72 #__ type_ start__ end____ width___ exp.time_ 11 omega 42.00 109.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 0.0000 67 #__ type_ start__ end____ width___ exp.time_ 12 omega 54.00 90.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 30.0000 36 #__ type_ start__ end____ width___ exp.time_ 13 omega -117.00 -14.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -37.0000 30.0000 103 #__ type_ start__ end____ width___ exp.time_ 14 omega -115.00 -11.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 150.0000 104 #__ type_ start__ end____ width___ exp.time_ 15 omega 1.00 76.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 40.6487 -99.0000 -90.0000 75 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0368637000 _diffrn_orient_matrix_UB_12 0.1406208000 _diffrn_orient_matrix_UB_13 0.0126400000 _diffrn_orient_matrix_UB_21 0.0891732000 _diffrn_orient_matrix_UB_22 -0.0605459000 _diffrn_orient_matrix_UB_23 0.0273469000 _diffrn_orient_matrix_UB_31 0.0625504000 _diffrn_orient_matrix_UB_32 0.0031906000 _diffrn_orient_matrix_UB_33 -0.0362094000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 9630 _reflns_number_total 12059 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _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 ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.648 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.080 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1132 _refine_ls_number_reflns 12059 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0638 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1143P)^2^+1.4461P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1662 _refine_ls_wR_factor_ref 0.1826 _refine_special_details ; Hirshfeld-type rigid-body restrains were applied for anisotropic displacement parameters of the entire hydroquinone ligand (ShelXL DELU instruction); also, the geometry of both solvent molecule was restrained to be equal (SAME instruction). Thermal displacement parameters for for both alternative positions of the ipso-atom of the disordered Ph group were constrained to be the same (EADP instruction). 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 0.97565(7) 0.08835(10) 0.22187(3) 0.0303(2) Uani 1 1 d . . . Fe2 Fe 1.05691(7) 0.41948(10) -0.01634(3) 0.0272(2) Uani 1 1 d . . . O1 O 0.9705(7) 0.2220(7) 0.18300(19) 0.093(3) Uani 1 1 d U . . O2 O 1.0876(5) 0.3727(11) 0.0359(2) 0.105(3) Uani 1 1 d U . . N1 N 0.8704(4) -0.0262(5) 0.24920(15) 0.0247(11) Uani 1 1 d . . . N2 N 0.8983(4) -0.0599(5) 0.28872(15) 0.0231(11) Uani 1 1 d . . . N3 N 1.0952(4) -0.0295(5) 0.25107(15) 0.0248(11) Uani 1 1 d . . . N4 N 1.0860(4) -0.0706(5) 0.29004(15) 0.0247(11) Uani 1 1 d . . . N5 N 0.9810(4) 0.2060(6) 0.27790(16) 0.0287(12) Uani 1 1 d . . . N6 N 1.0045(4) 0.1368(5) 0.31392(16) 0.0278(12) Uani 1 1 d . . . N7 N 0.9298(4) 0.5241(6) -0.04232(15) 0.0271(11) Uani 1 1 d . A . N8 N 0.9281(4) 0.5440(5) -0.08386(15) 0.0241(11) Uani 1 1 d . . . N9 N 1.0577(4) 0.3001(5) -0.06928(15) 0.0241(11) Uani 1 1 d . . . N10 N 1.0469(4) 0.3675(5) -0.10549(15) 0.0217(10) Uani 1 1 d . . . N11 N 1.1506(4) 0.5559(5) -0.04374(15) 0.0234(11) Uani 1 1 d . . . N12 N 1.1119(4) 0.5949(5) -0.08295(15) 0.0231(11) Uani 1 1 d . . . N13 N 0.9666(5) -0.0639(8) 0.1699(2) 0.0589(19) Uani 1 1 d . . . C1 C 1.1619(4) -0.1532(6) 0.30314(19) 0.0254(13) Uani 1 1 d . . . C2 C 1.2198(5) -0.1663(8) 0.2723(2) 0.0340(15) Uani 1 1 d . . . H2 H 1.2780 -0.2196 0.2726 0.041 Uiso 1 1 calc R . . C3 C 1.1777(5) -0.0870(7) 0.2402(2) 0.0302(15) Uani 1 1 d . . . C4 C 1.0222(5) 0.2225(7) 0.3459(2) 0.0306(14) Uani 1 1 d . . . C5 C 1.0085(5) 0.3501(7) 0.3296(2) 0.0338(15) Uani 1 1 d . . . H5 H 1.0159 0.4314 0.3444 0.041 Uiso 1 1 calc R . . C6 C 0.9824(5) 0.3360(7) 0.2885(2) 0.0340(15) Uani 1 1 d . . . C7 C 0.8296(5) -0.1446(7) 0.30106(19) 0.0283(13) Uani 1 1 d . . . C8 C 0.7564(5) -0.1633(6) 0.26840(19) 0.0281(13) Uani 1 1 d . . . H8 H 0.6990 -0.2183 0.2679 0.034 Uiso 1 1 calc R . . C9 C 0.7831(5) -0.0861(6) 0.2366(2) 0.0271(13) Uani 1 1 d . . . C10 C 1.1775(5) -0.2109(7) 0.3443(2) 0.0324(14) Uani 1 1 d . . . C11 C 1.2716(5) -0.1939(8) 0.3672(2) 0.0368(16) Uani 1 1 d . . . H11 H 1.3232 -0.1478 0.3558 0.044 Uiso 1 1 calc R . . C12 C 1.2886(5) -0.2459(8) 0.4072(2) 0.0401(17) Uani 1 1 d . . . H12 H 1.3517 -0.2339 0.4229 0.048 Uiso 1 1 calc R . . C13 C 1.2148(5) -0.3131(9) 0.4231(2) 0.0473(19) Uani 1 1 d . . . H13 H 1.2266 -0.3474 0.4501 0.057 Uiso 1 1 calc R . . C14 C 1.1230(5) -0.3321(8) 0.4007(2) 0.0417(17) Uani 1 1 d . . . H14 H 1.0724 -0.3797 0.4122 0.050 Uiso 1 1 calc R . . C15 C 1.1045(5) -0.2829(7) 0.3619(2) 0.0351(15) Uani 1 1 d . . . H15 H 1.0413 -0.2977 0.3466 0.042 Uiso 1 1 calc R . . C16 C 1.2132(6) -0.0640(9) 0.1996(2) 0.047(2) Uani 1 1 d . . . C17 C 1.2608(6) -0.1736(12) 0.1826(2) 0.064(3) Uani 1 1 d . . . H17 H 1.2670 -0.2577 0.1958 0.077 Uiso 1 1 calc R . . C18 C 1.2985(7) -0.1498(15) 0.1447(3) 0.079(4) Uani 1 1 d . . . H18 H 1.3317 -0.2199 0.1325 0.095 Uiso 1 1 calc R . . C19 C 1.2886(7) -0.0295(15) 0.1252(3) 0.082(4) Uani 1 1 d . . . H19 H 1.3187 -0.0141 0.1010 0.098 Uiso 1 1 calc R . . C20 C 1.2353(7) 0.0667(13) 0.1410(3) 0.074(3) Uani 1 1 d . . . H20 H 1.2231 0.1472 0.1262 0.089 Uiso 1 1 calc R . . C21 C 1.1976(6) 0.0530(10) 0.1781(2) 0.051(2) Uani 1 1 d . . . H21 H 1.1613 0.1236 0.1885 0.061 Uiso 1 1 calc R . . C22 C 1.0477(5) 0.1849(7) 0.3892(2) 0.0333(15) Uani 1 1 d . . . C23 C 1.0104(6) 0.2649(9) 0.4185(2) 0.048(2) Uani 1 1 d . . . H23 H 0.9685 0.3383 0.4103 0.058 Uiso 1 1 calc R . . C24 C 1.0343(6) 0.2374(11) 0.4592(3) 0.056(3) Uani 1 1 d . . . H24 H 1.0112 0.2946 0.4790 0.067 Uiso 1 1 calc R . . C25 C 1.0916(7) 0.1276(10) 0.4719(3) 0.057(2) Uani 1 1 d . . . H25 H 1.1048 0.1061 0.5000 0.068 Uiso 1 1 calc R . . C26 C 1.1294(7) 0.0497(8) 0.4427(2) 0.0491(19) Uani 1 1 d . . . H26 H 1.1705 -0.0245 0.4509 0.059 Uiso 1 1 calc R . . C27 C 1.1079(5) 0.0787(7) 0.4018(2) 0.0371(15) Uani 1 1 d . . . H27 H 1.1348 0.0248 0.3821 0.045 Uiso 1 1 calc R . . C28 C 0.9517(5) 0.4392(7) 0.2577(2) 0.0355(16) Uani 1 1 d . . . C29 C 1.0086(6) 0.5554(7) 0.2570(2) 0.0399(18) Uani 1 1 d . . . H29 H 1.0665 0.5673 0.2761 0.048 Uiso 1 1 calc R . . C30 C 0.9793(7) 0.6542(7) 0.2280(3) 0.053(2) Uani 1 1 d . . . H30 H 1.0185 0.7324 0.2270 0.064 Uiso 1 1 calc R . . C31 C 0.8932(7) 0.6385(8) 0.2007(3) 0.053(2) Uani 1 1 d . . . H31 H 0.8730 0.7057 0.1812 0.063 Uiso 1 1 calc R . . C32 C 0.8373(6) 0.5236(8) 0.2024(3) 0.050(2) Uani 1 1 d . . . H32 H 0.7778 0.5123 0.1842 0.060 Uiso 1 1 calc R . . C33 C 0.8675(6) 0.4261(7) 0.2302(3) 0.0438(19) Uani 1 1 d . . . H33 H 0.8290 0.3471 0.2305 0.053 Uiso 1 1 calc R . . C34 C 0.8325(4) -0.1984(6) 0.3432(2) 0.0288(14) Uani 1 1 d . . . C35 C 0.8229(5) -0.3377(7) 0.3476(2) 0.0365(16) Uani 1 1 d . . . H35 H 0.8196 -0.3951 0.3246 0.044 Uiso 1 1 calc R . . C36 C 0.8185(5) -0.3886(8) 0.3872(2) 0.0452(19) Uani 1 1 d . . . H36 H 0.8098 -0.4814 0.3906 0.054 Uiso 1 1 calc R . . C37 C 0.8265(6) -0.3087(9) 0.4203(3) 0.053(2) Uani 1 1 d . . . H37 H 0.8247 -0.3462 0.4467 0.064 Uiso 1 1 calc R . . C38 C 0.8375(5) -0.1688(9) 0.4161(2) 0.0466(19) Uani 1 1 d . . . H38 H 0.8427 -0.1126 0.4394 0.056 Uiso 1 1 calc R . . C39 C 0.8404(5) -0.1156(7) 0.3773(2) 0.0357(15) Uani 1 1 d . . . H39 H 0.8478 -0.0224 0.3740 0.043 Uiso 1 1 calc R . . C40 C 0.7298(5) -0.0685(7) 0.1957(2) 0.0327(15) Uani 1 1 d . . . C41 C 0.6653(6) -0.1660(9) 0.1789(2) 0.051(2) Uani 1 1 d . . . H41 H 0.6576 -0.2450 0.1941 0.061 Uiso 1 1 calc R . . C42 C 0.6124(7) -0.1521(11) 0.1413(3) 0.067(3) Uani 1 1 d . . . H42 H 0.5669 -0.2191 0.1307 0.081 Uiso 1 1 calc R . . C43 C 0.6259(7) -0.0384(11) 0.1185(3) 0.065(3) Uani 1 1 d . . . H43 H 0.5910 -0.0287 0.0919 0.077 Uiso 1 1 calc R . . C44 C 0.6896(7) 0.0598(9) 0.1344(3) 0.059(2) Uani 1 1 d . . . H44 H 0.6982 0.1374 0.1188 0.070 Uiso 1 1 calc R . . C45 C 0.7416(6) 0.0469(8) 0.1731(2) 0.0423(18) Uani 1 1 d . . . H45 H 0.7848 0.1159 0.1842 0.051 Uiso 1 1 calc R . . C46 C 0.8448(5) 0.6110(6) -0.09763(19) 0.0264(13) Uani 1 1 d . . . C47 C 0.7922(5) 0.6385(8) -0.0655(2) 0.0362(17) Uani 1 1 d . A . H47 H 0.7314 0.6866 -0.0661 0.043 Uiso 1 1 calc R . . C48 C 0.8476(5) 0.5800(8) -0.0316(2) 0.0388(18) Uani 1 1 d . . . C49 C 1.0505(5) 0.2836(6) -0.13669(18) 0.0262(13) Uani 1 1 d . . . C50 C 1.0620(5) 0.1570(6) -0.12058(19) 0.0270(13) Uani 1 1 d . . . H50 H 1.0652 0.0763 -0.1354 0.032 Uiso 1 1 calc R . . C51 C 1.0679(5) 0.1711(6) -0.07866(18) 0.0264(13) Uani 1 1 d . . . C52 C 1.1708(5) 0.6919(6) -0.09604(18) 0.0246(12) Uani 1 1 d . . . C53 C 1.2469(4) 0.7163(6) -0.06578(18) 0.0265(13) Uani 1 1 d . . . H53 H 1.2992 0.7792 -0.0664 0.032 Uiso 1 1 calc R . . C54 C 1.2323(4) 0.6301(6) -0.03363(18) 0.0256(13) Uani 1 1 d . . . C55 C 0.8168(5) 0.6418(7) -0.1421(2) 0.0337(15) Uani 1 1 d . . . C56 C 0.7877(5) 0.7696(8) -0.1536(2) 0.0384(17) Uani 1 1 d . . . H56 H 0.7897 0.8376 -0.1335 0.046 Uiso 1 1 calc R . . C57 C 0.7561(6) 0.7995(9) -0.1937(2) 0.050(2) Uani 1 1 d . . . H57 H 0.7359 0.8874 -0.2014 0.059 Uiso 1 1 calc R . . C58 C 0.7540(6) 0.6983(10) -0.2234(2) 0.053(2) Uani 1 1 d . . . H58 H 0.7316 0.7178 -0.2512 0.064 Uiso 1 1 calc R . . C59 C 0.7840(6) 0.5722(9) -0.2124(2) 0.0468(19) Uani 1 1 d . . . H59 H 0.7829 0.5045 -0.2325 0.056 Uiso 1 1 calc R . . C60 C 0.8161(5) 0.5431(8) -0.1719(2) 0.0356(15) Uani 1 1 d . . . H60 H 0.8377 0.4556 -0.1644 0.043 Uiso 1 1 calc R . . C61 C 0.8131(11) 0.5554(14) 0.0089(4) 0.026(2) Uiso 0.50 1 d P A 1 C61A C 0.8273(11) 0.6000(13) 0.0109(4) 0.026(2) Uiso 0.50 1 d P A 2 C62 C 0.7105(12) 0.5592(16) 0.0129(5) 0.046(4) Uiso 0.50 1 d P A 1 H62 H 0.6624 0.5630 -0.0106 0.056 Uiso 0.50 1 calc PR A 1 C62A C 0.7854(14) 0.704(2) 0.0251(6) 0.058(5) Uiso 0.50 1 d P A 2 H62A H 0.7718 0.7782 0.0077 0.069 Uiso 0.50 1 calc PR A 2 C63 C 0.6808(16) 0.557(2) 0.0521(6) 0.066(5) Uiso 0.50 1 d P A 1 H63 H 0.6118 0.5660 0.0549 0.079 Uiso 0.50 1 calc PR A 1 C63A C 0.7597(18) 0.711(3) 0.0644(7) 0.085(7) Uiso 0.50 1 d P A 2 H63A H 0.7272 0.7888 0.0723 0.103 Uiso 0.50 1 calc PR A 2 C64 C 0.7488(14) 0.5436(19) 0.0874(6) 0.053(4) Uiso 0.50 1 d P A 1 H64 H 0.7290 0.5302 0.1138 0.064 Uiso 0.50 1 calc PR A 1 C64A C 0.7770(15) 0.620(2) 0.0900(6) 0.063(5) Uiso 0.50 1 d P A 2 H64A H 0.7606 0.6346 0.1169 0.075 Uiso 0.50 1 calc PR A 2 C65 C 0.8431(13) 0.5510(19) 0.0805(5) 0.046(4) Uiso 0.50 1 d P A 1 H65 H 0.8925 0.5530 0.1036 0.055 Uiso 0.50 1 calc PR A 1 C65A C 0.8257(18) 0.480(3) 0.0797(7) 0.078(6) Uiso 0.50 1 d P A 2 H65A H 0.8395 0.4085 0.0984 0.094 Uiso 0.50 1 calc PR A 2 C66 C 0.8745(13) 0.5561(17) 0.0431(5) 0.045(4) Uiso 0.50 1 d P A 1 H66 H 0.9442 0.5605 0.0414 0.054 Uiso 0.50 1 calc PR A 1 C66A C 0.8454(15) 0.481(2) 0.0367(6) 0.064(5) Uiso 0.50 1 d P A 2 H66A H 0.8703 0.4024 0.0253 0.077 Uiso 0.50 1 calc PR A 2 C67 C 1.0428(5) 0.3210(7) -0.18046(18) 0.0273(13) Uani 1 1 d . . . C68 C 0.9918(5) 0.2385(7) -0.2092(2) 0.0311(14) Uani 1 1 d . . . H68 H 0.9626 0.1586 -0.2009 0.037 Uiso 1 1 calc R . . C69 C 0.9832(6) 0.2732(9) -0.2512(2) 0.0442(19) Uani 1 1 d . . . H69 H 0.9464 0.2172 -0.2708 0.053 Uiso 1 1 calc R . . C70 C 1.0256(5) 0.3827(8) -0.2635(2) 0.0391(16) Uani 1 1 d . . . H70 H 1.0179 0.4051 -0.2917 0.047 Uiso 1 1 calc R . . C71 C 1.0819(5) 0.4660(8) -0.2353(2) 0.0385(16) Uani 1 1 d . . . H71 H 1.1142 0.5424 -0.2444 0.046 Uiso 1 1 calc R . . C72 C 1.0899(5) 0.4357(6) -0.19385(19) 0.0302(14) Uani 1 1 d . . . H72 H 1.1271 0.4922 -0.1746 0.036 Uiso 1 1 calc R . . C73 C 1.0815(5) 0.0656(7) -0.0472(2) 0.0289(14) Uani 1 1 d . . . C74 C 1.0224(7) -0.0468(7) -0.0508(2) 0.0447(19) Uani 1 1 d . . . H74 H 0.9720 -0.0548 -0.0734 0.054 Uiso 1 1 calc R . . C75 C 1.0345(8) -0.1462(8) -0.0227(3) 0.055(2) Uani 1 1 d . . . H75 H 0.9935 -0.2232 -0.0261 0.066 Uiso 1 1 calc R . . C76 C 1.1044(9) -0.1361(10) 0.0098(3) 0.069(3) Uani 1 1 d . . . H76 H 1.1134 -0.2067 0.0290 0.082 Uiso 1 1 calc R . . C77 C 1.1629(8) -0.0239(11) 0.0153(3) 0.067(3) Uani 1 1 d . . . H77 H 1.2099 -0.0154 0.0390 0.080 Uiso 1 1 calc R . . C78 C 1.1532(6) 0.0782(9) -0.0141(2) 0.046(2) Uani 1 1 d . . . H78 H 1.1952 0.1543 -0.0111 0.055 Uiso 1 1 calc R . . C79 C 1.1528(5) 0.7520(6) -0.13714(17) 0.0248(12) Uani 1 1 d . . . C80 C 1.2310(5) 0.7678(7) -0.1599(2) 0.0327(14) Uani 1 1 d . . . H80 H 1.2960 0.7405 -0.1487 0.039 Uiso 1 1 calc R . . C81 C 1.2177(6) 0.8220(7) -0.1985(2) 0.0385(16) Uani 1 1 d . . . H81 H 1.2728 0.8304 -0.2138 0.046 Uiso 1 1 calc R . . C82 C 1.1252(6) 0.8638(7) -0.2147(2) 0.0375(16) Uani 1 1 d . . . H82 H 1.1161 0.9025 -0.2412 0.045 Uiso 1 1 calc R . . C83 C 1.0445(5) 0.8498(6) -0.19253(19) 0.0329(14) Uani 1 1 d . . . H83 H 0.9799 0.8770 -0.2041 0.039 Uiso 1 1 calc R . . C84 C 1.0582(4) 0.7965(6) -0.15385(19) 0.0255(12) Uani 1 1 d . . . H84 H 1.0033 0.7898 -0.1384 0.031 Uiso 1 1 calc R . . C85 C 1.2966(4) 0.6146(7) 0.0060(2) 0.0296(14) Uani 1 1 d . . . C86 C 1.3523(5) 0.7241(8) 0.0224(2) 0.0367(16) Uani 1 1 d . . . H86 H 1.3465 0.8074 0.0086 0.044 Uiso 1 1 calc R . . C87 C 1.4149(6) 0.7114(9) 0.0581(2) 0.0459(19) Uani 1 1 d . . . H87 H 1.4516 0.7865 0.0689 0.055 Uiso 1 1 calc R . . C88 C 1.4258(7) 0.5912(9) 0.0785(3) 0.056(2) Uani 1 1 d . . . H88 H 1.4694 0.5839 0.1033 0.067 Uiso 1 1 calc R . . C89 C 1.3716(7) 0.4802(11) 0.0623(3) 0.063(3) Uani 1 1 d . . . H89 H 1.3793 0.3969 0.0759 0.076 Uiso 1 1 calc R . . C90 C 1.3066(6) 0.4916(8) 0.0263(2) 0.0421(18) Uani 1 1 d . . . H90 H 1.2692 0.4168 0.0156 0.050 Uiso 1 1 calc R . . C91 C 0.9817(9) -0.092(2) 0.1368(4) 0.157(9) Uani 1 1 d . . . C92 C 1.0038(13) -0.152(2) 0.0993(5) 0.175(9) Uani 1 1 d . . . H92A H 0.9495 -0.1337 0.0776 0.262 Uiso 1 1 calc R . . H92B H 1.0105 -0.2488 0.1031 0.262 Uiso 1 1 calc R . . H92C H 1.0664 -0.1160 0.0917 0.262 Uiso 1 1 calc R . . C93 C 0.9990(10) 0.2587(11) 0.1468(3) 0.077(3) Uani 1 1 d U . . C94 C 1.0569(7) 0.3631(10) 0.1441(3) 0.060(2) Uani 1 1 d U . . H94 H 1.0779 0.4130 0.1681 0.072 Uiso 1 1 calc R . . C95 C 1.0885(7) 0.4029(10) 0.1069(3) 0.063(2) Uani 1 1 d U . . C96 C 1.0551(8) 0.3362(15) 0.0715(3) 0.085(3) Uani 1 1 d U . . C97 C 0.9860(10) 0.2408(15) 0.0730(3) 0.093(4) Uani 1 1 d U . . C98 C 0.9544(10) 0.1955(15) 0.1107(3) 0.105(5) Uani 1 1 d U . . H98 H 0.9061 0.1270 0.1114 0.126 Uiso 1 1 calc R . . C99 C 1.1538(12) 0.5331(13) 0.1084(4) 0.112(5) Uani 1 1 d U . . H99A H 1.1516 0.5776 0.1348 0.168 Uiso 1 1 calc R . . H99B H 1.1274 0.5929 0.0863 0.168 Uiso 1 1 calc R . . H99C H 1.2230 0.5098 0.1052 0.168 Uiso 1 1 calc R . . C100 C 0.9343(10) 0.174(2) 0.0335(4) 0.138(7) Uani 1 1 d U . . H10A H 0.9260 0.2403 0.0114 0.207 Uiso 1 1 calc R . . H10B H 0.8687 0.1406 0.0385 0.207 Uiso 1 1 calc R . . H10C H 0.9756 0.1008 0.0257 0.207 Uiso 1 1 calc R . . B1 B 0.9996(5) -0.0158(7) 0.3125(2) 0.0251(15) Uani 1 1 d . . . H1 H 1.0055 -0.0520 0.3410 0.030 Uiso 1 1 calc R . . B2 B 1.0230(5) 0.5199(7) -0.1052(2) 0.0217(14) Uani 1 1 d . . . H2A H 1.0107 0.5525 -0.1341 0.026 Uiso 1 1 calc R . . Cl1 Cl 1.34175(19) 0.4005(3) 0.17628(8) 0.0761(7) Uani 1 1 d D . . Cl2 Cl 1.5778(2) 0.3632(3) 0.15666(9) 0.0780(8) Uani 1 1 d D . . C1S C 1.4290(7) 0.2768(11) 0.1983(3) 0.071(3) Uani 1 1 d D . . H1SA H 1.4684 0.3140 0.2229 0.085 Uiso 1 1 calc R . . H1SB H 1.3917 0.1988 0.2068 0.085 Uiso 1 1 calc R . . C2S C 1.4944(7) 0.2356(11) 0.1703(3) 0.080(3) Uani 1 1 d D . . H2SA H 1.4542 0.2036 0.1451 0.096 Uiso 1 1 calc R . . H2SB H 1.5346 0.1597 0.1822 0.096 Uiso 1 1 calc R . . Cl3 Cl 0.6911(4) 0.1794(8) 0.03293(15) 0.124(2) Uani 0.674(7) 1 d PD . . Cl4 Cl 0.4422(4) 0.1285(6) 0.03172(15) 0.109(2) Uani 0.674(7) 1 d PD . . C3S C 0.5931(13) 0.3023(19) 0.0274(7) 0.128(8) Uiso 0.674(7) 1 d PD . . H3SA H 0.5745 0.3278 0.0545 0.153 Uiso 0.674(7) 1 calc PR . . H3SB H 0.6154 0.3829 0.0138 0.153 Uiso 0.674(7) 1 calc PR . . C4S C 0.5172(10) 0.2482(14) 0.0052(4) 0.069(4) Uiso 0.674(7) 1 d PD . . H4SA H 0.5423 0.2016 -0.0180 0.082 Uiso 0.674(7) 1 calc PR . . H4SB H 0.4724 0.3202 -0.0064 0.082 Uiso 0.674(7) 1 calc PR . . 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 0.0337(6) 0.0264(5) 0.0337(6) 0.0053(5) 0.0162(4) 0.0022(5) Fe2 0.0264(5) 0.0314(6) 0.0244(5) 0.0045(4) 0.0061(4) 0.0036(5) O1 0.178(8) 0.064(4) 0.043(3) 0.016(3) 0.042(4) 0.000(5) O2 0.053(4) 0.218(10) 0.046(3) 0.058(5) 0.010(3) -0.012(5) N1 0.022(2) 0.027(3) 0.026(3) -0.001(2) 0.008(2) -0.004(2) N2 0.026(3) 0.023(3) 0.020(2) 0.0018(19) 0.004(2) -0.004(2) N3 0.027(3) 0.025(3) 0.025(3) -0.001(2) 0.010(2) -0.007(2) N4 0.025(3) 0.027(3) 0.023(2) 0.000(2) 0.005(2) -0.002(2) N5 0.029(3) 0.028(3) 0.030(3) -0.002(2) 0.010(2) -0.006(2) N6 0.031(3) 0.024(3) 0.029(3) -0.002(2) 0.008(2) -0.002(2) N7 0.024(3) 0.035(3) 0.022(3) 0.003(2) 0.005(2) 0.006(2) N8 0.022(2) 0.023(3) 0.029(3) 0.002(2) 0.008(2) 0.006(2) N9 0.026(3) 0.022(3) 0.025(3) 0.001(2) 0.002(2) 0.000(2) N10 0.024(2) 0.024(3) 0.018(2) -0.001(2) 0.0034(19) 0.001(2) N11 0.026(3) 0.025(3) 0.020(2) 0.0031(19) 0.003(2) 0.001(2) N12 0.028(3) 0.020(2) 0.021(2) 0.0017(19) 0.001(2) 0.001(2) N13 0.054(4) 0.060(5) 0.063(5) -0.008(4) 0.010(4) -0.006(4) C1 0.017(3) 0.023(3) 0.037(3) 0.002(3) 0.003(2) 0.002(2) C2 0.023(3) 0.044(4) 0.036(4) -0.005(3) 0.009(3) 0.000(3) C3 0.025(3) 0.040(4) 0.026(3) -0.011(3) 0.004(3) 0.000(3) C4 0.026(3) 0.029(3) 0.038(4) -0.006(3) 0.010(3) -0.004(3) C5 0.032(3) 0.024(3) 0.043(4) -0.010(3) -0.003(3) -0.003(3) C6 0.029(3) 0.028(3) 0.046(4) -0.007(3) 0.008(3) -0.005(3) C7 0.024(3) 0.029(3) 0.033(3) 0.001(3) 0.011(2) -0.005(3) C8 0.022(3) 0.029(3) 0.033(3) -0.002(3) 0.004(2) -0.009(3) C9 0.023(3) 0.026(3) 0.031(3) -0.002(3) -0.002(2) 0.001(3) C10 0.023(3) 0.037(4) 0.036(3) -0.008(3) 0.000(3) 0.003(3) C11 0.026(3) 0.045(4) 0.040(4) -0.011(3) 0.006(3) 0.001(3) C12 0.030(3) 0.057(5) 0.032(4) 0.001(3) -0.004(3) 0.005(3) C13 0.036(4) 0.068(5) 0.037(4) 0.012(4) 0.001(3) 0.012(4) C14 0.038(4) 0.043(4) 0.045(4) 0.012(3) 0.011(3) 0.003(3) C15 0.033(3) 0.032(4) 0.039(4) -0.001(3) 0.000(3) 0.002(3) C16 0.030(4) 0.073(6) 0.038(4) -0.010(4) 0.011(3) -0.001(4) C17 0.029(4) 0.125(9) 0.038(4) -0.018(5) 0.002(3) 0.023(5) C18 0.044(5) 0.158(12) 0.037(5) -0.028(6) 0.013(4) 0.019(6) C19 0.044(5) 0.177(13) 0.027(4) 0.003(6) 0.017(4) 0.017(7) C20 0.057(6) 0.127(10) 0.040(5) 0.003(5) 0.013(4) -0.032(6) C21 0.041(4) 0.084(7) 0.033(4) 0.002(4) 0.019(3) -0.015(4) C22 0.029(3) 0.038(4) 0.035(3) -0.015(3) 0.010(3) -0.021(3) C23 0.033(4) 0.067(6) 0.046(4) -0.022(4) 0.013(3) -0.013(4) C24 0.035(4) 0.090(7) 0.045(5) -0.029(5) 0.019(4) -0.026(5) C25 0.063(6) 0.072(6) 0.037(4) -0.008(4) 0.015(4) -0.028(5) C26 0.063(5) 0.050(5) 0.033(4) 0.000(3) -0.001(3) -0.015(4) C27 0.044(4) 0.029(3) 0.039(4) -0.007(3) 0.009(3) -0.011(3) C28 0.032(4) 0.026(4) 0.048(4) -0.006(3) 0.000(3) 0.001(3) C29 0.035(4) 0.027(4) 0.055(5) 0.001(3) -0.010(3) -0.009(3) C30 0.064(5) 0.018(3) 0.070(6) -0.002(4) -0.022(4) 0.001(4) C31 0.062(5) 0.032(4) 0.056(5) -0.004(4) -0.025(4) 0.013(4) C32 0.044(4) 0.040(4) 0.059(5) -0.008(4) -0.022(4) 0.010(4) C33 0.036(4) 0.032(4) 0.061(5) -0.008(3) -0.004(4) 0.000(3) C34 0.019(3) 0.026(3) 0.042(4) 0.009(3) 0.006(3) -0.009(3) C35 0.028(3) 0.034(4) 0.046(4) 0.013(3) -0.001(3) -0.004(3) C36 0.035(4) 0.047(5) 0.053(5) 0.026(4) 0.004(3) -0.006(3) C37 0.036(4) 0.072(6) 0.054(5) 0.037(5) 0.012(4) -0.011(4) C38 0.035(4) 0.072(6) 0.035(4) 0.007(4) 0.014(3) 0.006(4) C39 0.032(3) 0.040(4) 0.037(4) 0.000(3) 0.009(3) -0.009(3) C40 0.035(4) 0.034(4) 0.029(3) -0.003(3) 0.003(3) 0.004(3) C41 0.051(5) 0.056(5) 0.041(4) 0.007(4) -0.009(4) -0.013(4) C42 0.064(6) 0.076(7) 0.054(5) 0.009(5) -0.027(4) -0.022(5) C43 0.064(6) 0.081(7) 0.041(5) 0.001(5) -0.025(4) -0.007(5) C44 0.072(6) 0.057(6) 0.044(5) 0.010(4) -0.006(4) 0.025(5) C45 0.039(4) 0.046(4) 0.040(4) 0.003(3) -0.002(3) 0.005(4) C46 0.024(3) 0.030(3) 0.026(3) 0.004(2) 0.004(2) 0.008(3) C47 0.031(3) 0.051(4) 0.030(3) 0.010(3) 0.015(3) 0.018(3) C48 0.029(4) 0.052(5) 0.039(4) 0.008(3) 0.014(3) 0.013(3) C49 0.026(3) 0.027(3) 0.026(3) 0.002(2) 0.004(2) 0.004(3) C50 0.028(3) 0.024(3) 0.029(3) -0.001(2) 0.005(3) 0.001(3) C51 0.028(3) 0.026(3) 0.026(3) -0.003(2) 0.005(3) 0.002(3) C52 0.029(3) 0.019(3) 0.027(3) 0.001(2) 0.007(2) -0.001(2) C53 0.022(3) 0.031(3) 0.028(3) -0.005(2) 0.007(2) -0.005(3) C54 0.023(3) 0.029(3) 0.025(3) -0.004(2) 0.003(2) 0.002(3) C55 0.022(3) 0.045(4) 0.035(3) 0.009(3) 0.005(3) 0.008(3) C56 0.031(3) 0.051(5) 0.033(4) 0.012(3) 0.007(3) 0.016(3) C57 0.042(4) 0.059(5) 0.050(5) 0.021(4) 0.013(4) 0.021(4) C58 0.036(4) 0.087(7) 0.037(4) 0.022(4) 0.003(3) 0.014(4) C59 0.041(4) 0.063(5) 0.034(4) 0.005(4) -0.004(3) 0.000(4) C60 0.030(3) 0.043(4) 0.033(3) 0.010(3) 0.000(3) 0.003(3) C67 0.022(3) 0.032(3) 0.029(3) 0.001(3) 0.005(2) -0.001(3) C68 0.021(3) 0.037(4) 0.035(3) -0.003(3) 0.003(3) -0.006(3) C69 0.035(4) 0.062(5) 0.036(4) -0.007(4) 0.002(3) 0.002(4) C70 0.037(4) 0.051(4) 0.029(3) 0.005(3) 0.000(3) 0.005(3) C71 0.039(4) 0.043(4) 0.035(4) 0.013(3) 0.013(3) 0.011(3) C72 0.029(3) 0.031(3) 0.032(3) 0.001(3) 0.010(3) -0.002(3) C73 0.032(3) 0.030(3) 0.027(3) -0.001(3) 0.010(3) 0.006(3) C74 0.068(5) 0.024(4) 0.045(4) -0.002(3) 0.018(4) 0.012(4) C75 0.082(7) 0.030(4) 0.061(6) 0.010(4) 0.037(5) 0.005(4) C76 0.105(8) 0.043(5) 0.067(6) 0.031(5) 0.047(6) 0.037(6) C77 0.083(7) 0.081(7) 0.038(4) 0.012(4) 0.017(4) 0.048(6) C78 0.046(4) 0.053(5) 0.039(4) 0.003(3) 0.002(3) 0.010(4) C79 0.035(3) 0.016(3) 0.024(3) -0.004(2) 0.006(2) -0.005(3) C80 0.028(3) 0.033(4) 0.039(4) 0.003(3) 0.011(3) -0.002(3) C81 0.040(4) 0.035(4) 0.042(4) 0.002(3) 0.013(3) -0.010(3) C82 0.051(4) 0.030(3) 0.033(3) 0.005(3) 0.006(3) -0.014(3) C83 0.038(3) 0.029(3) 0.031(3) 0.003(3) 0.002(3) 0.000(3) C84 0.025(3) 0.016(3) 0.037(3) -0.005(2) 0.011(3) 0.000(2) C85 0.015(3) 0.038(4) 0.036(4) -0.006(3) 0.004(3) -0.002(3) C86 0.035(4) 0.045(4) 0.031(3) -0.008(3) 0.004(3) 0.003(3) C87 0.041(4) 0.053(5) 0.040(4) -0.015(4) -0.012(3) -0.006(4) C88 0.051(5) 0.063(6) 0.049(5) -0.006(4) -0.016(4) 0.006(4) C89 0.064(6) 0.069(6) 0.050(5) 0.005(5) -0.017(4) 0.012(5) C90 0.041(4) 0.050(5) 0.032(4) -0.006(3) -0.009(3) 0.001(4) C91 0.063(7) 0.31(2) 0.103(10) -0.130(13) 0.043(7) -0.022(11) C92 0.130(14) 0.29(3) 0.110(12) -0.083(16) 0.049(11) -0.013(16) C93 0.125(9) 0.070(7) 0.035(4) 0.019(4) 0.007(5) -0.023(6) C94 0.068(6) 0.065(6) 0.044(4) 0.017(4) 0.000(4) -0.009(4) C95 0.062(6) 0.077(6) 0.052(4) 0.029(4) 0.012(4) 0.009(4) C96 0.061(6) 0.156(10) 0.038(4) 0.047(5) 0.003(4) -0.015(6) C97 0.094(8) 0.137(11) 0.049(5) 0.013(6) 0.010(5) -0.032(7) C98 0.125(11) 0.131(11) 0.067(5) -0.027(7) 0.045(7) -0.073(9) C99 0.151(13) 0.097(9) 0.095(9) 0.029(7) 0.044(8) -0.021(8) C100 0.088(9) 0.25(2) 0.079(7) -0.044(10) 0.019(7) -0.009(10) B1 0.029(4) 0.019(3) 0.028(4) 0.001(3) 0.007(3) -0.012(3) B2 0.018(3) 0.026(4) 0.022(3) 0.002(3) 0.007(3) 0.002(3) Cl1 0.0541(13) 0.106(2) 0.0669(14) -0.0009(14) 0.0022(11) 0.0054(14) Cl2 0.0638(15) 0.0735(17) 0.102(2) -0.0034(15) 0.0335(14) -0.0054(13) C1S 0.070(6) 0.084(7) 0.059(6) 0.014(5) 0.004(5) -0.002(6) C2S 0.050(5) 0.104(9) 0.085(7) -0.010(7) 0.006(5) -0.005(6) Cl3 0.109(4) 0.193(7) 0.072(3) 0.015(3) 0.013(3) -0.013(4) Cl4 0.084(3) 0.145(5) 0.091(3) -0.031(3) -0.016(2) 0.047(3) _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 O1 1.852(6) . ? Fe1 N1 2.111(5) . ? Fe1 N3 2.136(6) . ? Fe1 N5 2.187(5) . ? Fe1 N13 2.289(8) . ? Fe2 O2 1.784(6) . ? Fe2 N7 2.105(5) . ? Fe2 N9 2.119(5) . ? Fe2 N11 2.136(5) . ? O1 C93 1.348(10) . ? O2 C96 1.352(10) . ? N1 C9 1.345(8) . ? N2 N1 1.355(7) . ? N2 C7 1.355(8) . ? N2 B1 1.557(9) . ? N3 C3 1.340(8) . ? N4 N3 1.369(7) . ? N4 C1 1.349(8) . ? N4 B1 1.555(9) . ? N5 C6 1.352(9) . ? N6 N5 1.380(8) . ? N6 C4 1.361(8) . ? N6 B1 1.536(9) . ? N7 C48 1.328(8) . ? N8 N7 1.381(7) . ? N8 C46 1.342(8) . ? N8 B2 1.552(8) . ? N9 C51 1.345(8) . ? N10 N9 1.365(7) . ? N10 C49 1.335(8) . ? N10 B2 1.566(9) . ? N11 C54 1.340(8) . ? N12 N11 1.392(7) . ? N12 C52 1.360(8) . ? N12 B2 1.529(9) . ? N13 C91 1.168(13) . ? C1 C2 1.361(9) . ? C1 C10 1.468(9) . ? C2 H2 0.9500 . ? C2 C3 1.391(10) . ? C3 C16 1.491(10) . ? C4 C5 1.394(9) . ? C4 C22 1.478(10) . ? C5 H5 0.9500 . ? C5 C6 1.368(10) . ? C6 C28 1.477(10) . ? C7 C8 1.385(9) . ? C7 C34 1.487(9) . ? C8 H8 0.9500 . ? C8 C9 1.385(9) . ? C9 C40 1.460(9) . ? C10 C11 1.408(8) . ? C10 C15 1.401(10) . ? C11 H11 0.9500 . ? C11 C12 1.410(10) . ? C12 H12 0.9500 . ? C12 C13 1.361(11) . ? C13 H13 0.9500 . ? C13 C14 1.378(10) . ? C14 H14 0.9500 . ? C14 C15 1.365(9) . ? C15 H15 0.9500 . ? C16 C17 1.423(12) . ? C16 C21 1.376(12) . ? C17 H17 0.9500 . ? C17 C18 1.424(12) . ? C18 H18 0.9500 . ? C18 C19 1.369(18) . ? C19 H19 0.9500 . ? C19 C20 1.346(16) . ? C20 H20 0.9500 . ? C20 C21 1.385(10) . ? C21 H21 0.9500 . ? C22 C23 1.396(10) . ? C22 C27 1.376(10) . ? C23 H23 0.9500 . ? C23 C24 1.368(12) . ? C24 H24 0.9500 . ? C24 C25 1.384(14) . ? C25 H25 0.9500 . ? C25 C26 1.384(12) . ? C26 H26 0.9500 . ? C26 C27 1.373(10) . ? C27 H27 0.9500 . ? C28 C29 1.399(10) . ? C28 C33 1.372(10) . ? C29 H29 0.9500 . ? C29 C30 1.403(10) . ? C30 H30 0.9500 . ? C30 C31 1.391(11) . ? C31 H31 0.9500 . ? C31 C32 1.384(12) . ? C32 H32 0.9500 . ? C32 C33 1.371(11) . ? C33 H33 0.9500 . ? C34 C35 1.415(9) . ? C34 C39 1.393(9) . ? C35 H35 0.9500 . ? C35 C36 1.408(10) . ? C36 H36 0.9500 . ? C36 C37 1.350(12) . ? C37 H37 0.9500 . ? C37 C38 1.423(12) . ? C38 H38 0.9500 . ? C38 C39 1.391(10) . ? C39 H39 0.9500 . ? C40 C41 1.383(10) . ? C40 C45 1.398(10) . ? C41 H41 0.9500 . ? C41 C42 1.364(11) . ? C42 H42 0.9500 . ? C42 C43 1.392(13) . ? C43 H43 0.9500 . ? C43 C44 1.371(13) . ? C44 H44 0.9500 . ? C44 C45 1.388(11) . ? C45 H45 0.9500 . ? C46 C47 1.372(9) . ? C46 C55 1.502(9) . ? C47 H47 0.9500 . ? C47 C48 1.398(10) . ? C48 C61 1.485(16) . ? C48 C61A 1.471(16) . ? C49 C50 1.381(9) . ? C49 C67 1.482(8) . ? C50 H50 0.9500 . ? C50 C51 1.382(9) . ? C51 C73 1.479(9) . ? C52 C53 1.366(8) . ? C52 C79 1.477(8) . ? C53 H53 0.9500 . ? C53 C54 1.401(9) . ? C54 C85 1.489(9) . ? C55 C56 1.384(10) . ? C55 C60 1.396(10) . ? C56 H56 0.9500 . ? C56 C57 1.374(10) . ? C57 H57 0.9500 . ? C57 C58 1.408(13) . ? C58 H58 0.9500 . ? C58 C59 1.367(12) . ? C59 H59 0.9500 . ? C59 C60 1.384(9) . ? C60 H60 0.9500 . ? C61 C62 1.41(2) . ? C61 C66 1.32(2) . ? C61A C62A 1.30(2) . ? C61A C66A 1.47(3) . ? C62 H62 0.9500 . ? C62 C63 1.40(2) . ? C62A H62A 0.9500 . ? C62A C63A 1.38(3) . ? C63 H63 0.9500 . ? C63 C64 1.40(3) . ? C63A H63A 0.9500 . ? C63A C64A 1.24(3) . ? C64 H64 0.9500 . ? C64 C65 1.32(2) . ? C64A H64A 0.9500 . ? C64A C65A 1.61(3) . ? C65 H65 0.9500 . ? C65 C66 1.35(2) . ? C65A H65A 0.9500 . ? C65A C66A 1.47(3) . ? C66 H66 0.9500 . ? C66A H66A 0.9500 . ? C67 C68 1.381(9) . ? C67 C72 1.412(9) . ? C68 H68 0.9500 . ? C68 C69 1.418(10) . ? C69 H69 0.9500 . ? C69 C70 1.327(11) . ? C70 H70 0.9500 . ? C70 C71 1.406(11) . ? C71 H71 0.9500 . ? C71 C72 1.390(9) . ? C72 H72 0.9500 . ? C73 C74 1.380(11) . ? C73 C78 1.377(10) . ? C74 H74 0.9500 . ? C74 C75 1.360(11) . ? C75 H75 0.9500 . ? C75 C76 1.344(14) . ? C76 H76 0.9500 . ? C76 C77 1.377(16) . ? C77 H77 0.9500 . ? C77 C78 1.406(12) . ? C78 H78 0.9500 . ? C79 C80 1.376(8) . ? C79 C84 1.401(8) . ? C80 H80 0.9500 . ? C80 C81 1.374(9) . ? C81 H81 0.9500 . ? C81 C82 1.364(10) . ? C82 H82 0.9500 . ? C82 C83 1.389(10) . ? C83 H83 0.9500 . ? C83 C84 1.375(9) . ? C84 H84 0.9500 . ? C85 C86 1.404(10) . ? C85 C90 1.405(10) . ? C86 H86 0.9500 . ? C86 C87 1.371(9) . ? C87 H87 0.9500 . ? C87 C88 1.383(12) . ? C88 H88 0.9500 . ? C88 C89 1.406(13) . ? C89 H89 0.9500 . ? C89 C90 1.392(11) . ? C90 H90 0.9500 . ? C91 C92 1.441(16) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 C94 1.318(13) . ? C93 C98 1.419(14) . ? C94 H94 0.9500 . ? C94 C95 1.403(12) . ? C95 C96 1.375(15) . ? C95 C99 1.575(16) . ? C96 C97 1.343(16) . ? C97 C98 1.433(14) . ? C97 C100 1.554(17) . ? C98 H98 0.9500 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? B1 H1 1.0000 . ? B2 H2A 1.0000 . ? Cl1 C1S 1.805(10) . ? Cl2 C2S 1.797(10) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C1S C2S 1.413(12) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Cl3 C3S 1.803(17) . ? Cl4 C4S 1.856(13) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C3S C4S 1.305(17) . ? C4S H4SA 0.9900 . ? C4S H4SB 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 O1 Fe1 N1 136.0(3) . . ? O1 Fe1 N3 132.7(3) . . ? O1 Fe1 N5 100.7(3) . . ? O1 Fe1 N13 88.5(3) . . ? N1 Fe1 N3 90.9(2) . . ? N1 Fe1 N5 83.8(2) . . ? N1 Fe1 N13 88.6(2) . . ? N3 Fe1 N5 88.4(2) . . ? N3 Fe1 N13 86.4(2) . . ? N5 Fe1 N13 170.6(2) . . ? O2 Fe2 N7 127.5(3) . . ? O2 Fe2 N9 128.4(4) . . ? O2 Fe2 N11 119.7(3) . . ? N7 Fe2 N9 91.8(2) . . ? N7 Fe2 N11 90.1(2) . . ? N9 Fe2 N11 87.4(2) . . ? C93 O1 Fe1 145.0(7) . . ? C96 O2 Fe2 147.9(6) . . ? N2 N1 Fe1 115.0(4) . . ? C9 N1 Fe1 136.2(4) . . ? C9 N1 N2 108.5(5) . . ? N1 N2 C7 108.9(5) . . ? N1 N2 B1 122.7(5) . . ? C7 N2 B1 128.1(5) . . ? N4 N3 Fe1 116.3(4) . . ? C3 N3 Fe1 136.5(4) . . ? C3 N3 N4 107.0(5) . . ? N3 N4 B1 119.8(5) . . ? C1 N4 N3 109.7(5) . . ? C1 N4 B1 130.5(5) . . ? N6 N5 Fe1 115.8(4) . . ? C6 N5 Fe1 137.6(5) . . ? C6 N5 N6 105.7(5) . . ? N5 N6 B1 118.3(5) . . ? C4 N6 N5 110.3(5) . . ? C4 N6 B1 131.2(6) . . ? N8 N7 Fe2 113.2(4) . . ? C48 N7 Fe2 140.2(5) . . ? C48 N7 N8 106.6(5) . . ? N7 N8 B2 120.6(5) . . ? C46 N8 N7 108.9(5) . . ? C46 N8 B2 128.9(5) . . ? N10 N9 Fe2 115.4(4) . . ? C51 N9 Fe2 138.3(4) . . ? C51 N9 N10 106.3(5) . . ? N9 N10 B2 118.8(5) . . ? C49 N10 N9 110.5(5) . . ? C49 N10 B2 130.4(5) . . ? N12 N11 Fe2 113.5(4) . . ? C54 N11 Fe2 139.7(4) . . ? C54 N11 N12 106.3(5) . . ? N11 N12 B2 119.5(5) . . ? C52 N12 N11 109.2(5) . . ? C52 N12 B2 131.0(5) . . ? C91 N13 Fe1 149.3(12) . . ? N4 C1 C2 107.5(6) . . ? N4 C1 C10 124.0(5) . . ? C2 C1 C10 128.4(6) . . ? C1 C2 H2 126.4 . . ? C1 C2 C3 107.2(6) . . ? C3 C2 H2 126.4 . . ? N3 C3 C2 108.7(6) . . ? N3 C3 C16 122.5(6) . . ? C2 C3 C16 128.8(6) . . ? N6 C4 C5 106.4(6) . . ? N6 C4 C22 125.8(6) . . ? C5 C4 C22 127.7(6) . . ? C4 C5 H5 126.5 . . ? C6 C5 C4 107.0(6) . . ? C6 C5 H5 126.5 . . ? N5 C6 C5 110.5(6) . . ? N5 C6 C28 120.5(6) . . ? C5 C6 C28 128.9(6) . . ? N2 C7 C8 107.6(5) . . ? N2 C7 C34 124.5(6) . . ? C8 C7 C34 127.8(5) . . ? C7 C8 H8 126.7 . . ? C9 C8 C7 106.6(5) . . ? C9 C8 H8 126.7 . . ? N1 C9 C8 108.3(5) . . ? N1 C9 C40 123.2(6) . . ? C8 C9 C40 128.5(6) . . ? C11 C10 C1 117.9(6) . . ? C15 C10 C1 123.7(6) . . ? C15 C10 C11 118.3(6) . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.5(7) . . ? C12 C11 H11 120.3 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(6) . . ? C13 C12 H12 120.0 . . ? C12 C13 H13 119.6 . . ? C12 C13 C14 120.9(7) . . ? C14 C13 H13 119.6 . . ? C13 C14 H14 119.8 . . ? C15 C14 C13 120.4(7) . . ? C15 C14 H14 119.8 . . ? C10 C15 H15 119.5 . . ? C14 C15 C10 121.0(6) . . ? C14 C15 H15 119.5 . . ? C17 C16 C3 116.1(8) . . ? C21 C16 C3 123.3(7) . . ? C21 C16 C17 120.5(8) . . ? C16 C17 H17 122.0 . . ? C16 C17 C18 116.1(11) . . ? C18 C17 H17 122.0 . . ? C17 C18 H18 118.8 . . ? C19 C18 C17 122.4(10) . . ? C19 C18 H18 118.8 . . ? C18 C19 H19 120.7 . . ? C20 C19 C18 118.7(9) . . ? C20 C19 H19 120.7 . . ? C19 C20 H20 118.7 . . ? C19 C20 C21 122.6(11) . . ? C21 C20 H20 118.7 . . ? C16 C21 C20 119.3(9) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C4 117.4(7) . . ? C27 C22 C4 123.6(6) . . ? C27 C22 C23 119.0(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 C22 120.0(9) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 119.5 . . ? C23 C24 C25 121.0(8) . . ? C25 C24 H24 119.5 . . ? C24 C25 H25 120.6 . . ? C24 C25 C26 118.7(8) . . ? C26 C25 H25 120.6 . . ? C25 C26 H26 119.7 . . ? C27 C26 C25 120.6(8) . . ? C27 C26 H26 119.7 . . ? C22 C27 H27 119.7 . . ? C26 C27 C22 120.7(7) . . ? C26 C27 H27 119.7 . . ? C29 C28 C6 119.2(6) . . ? C33 C28 C6 122.0(7) . . ? C33 C28 C29 118.8(7) . . ? C28 C29 H29 120.3 . . ? C28 C29 C30 119.4(7) . . ? C30 C29 H29 120.3 . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.4(8) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 120.4 . . ? C32 C31 C30 119.1(8) . . ? C32 C31 H31 120.4 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.2(7) . . ? C33 C32 H32 119.9 . . ? C28 C33 H33 119.0 . . ? C32 C33 C28 122.0(7) . . ? C32 C33 H33 119.0 . . ? C35 C34 C7 117.6(6) . . ? C39 C34 C7 121.8(6) . . ? C39 C34 C35 120.5(6) . . ? C34 C35 H35 121.0 . . ? C36 C35 C34 118.0(7) . . ? C36 C35 H35 121.0 . . ? C35 C36 H36 119.2 . . ? C37 C36 C35 121.7(7) . . ? C37 C36 H36 119.2 . . ? C36 C37 H37 119.7 . . ? C36 C37 C38 120.6(7) . . ? C38 C37 H37 119.7 . . ? C37 C38 H38 120.5 . . ? C39 C38 C37 119.0(8) . . ? C39 C38 H38 120.5 . . ? C34 C39 H39 119.9 . . ? C38 C39 C34 120.3(7) . . ? C38 C39 H39 119.9 . . ? C41 C40 C9 120.0(7) . . ? C41 C40 C45 118.7(7) . . ? C45 C40 C9 121.2(6) . . ? C40 C41 H41 119.1 . . ? C42 C41 C40 121.9(8) . . ? C42 C41 H41 119.1 . . ? C41 C42 H42 120.4 . . ? C41 C42 C43 119.2(9) . . ? C43 C42 H42 120.4 . . ? C42 C43 H43 120.0 . . ? C44 C43 C42 120.1(8) . . ? C44 C43 H43 120.0 . . ? C43 C44 H44 119.7 . . ? C43 C44 C45 120.7(9) . . ? C45 C44 H44 119.7 . . ? C40 C45 H45 120.3 . . ? C44 C45 C40 119.4(8) . . ? C44 C45 H45 120.3 . . ? N8 C46 C47 109.2(5) . . ? N8 C46 C55 122.5(5) . . ? C47 C46 C55 128.3(6) . . ? C46 C47 H47 127.6 . . ? C46 C47 C48 104.8(6) . . ? C48 C47 H47 127.6 . . ? N7 C48 C47 110.5(6) . . ? N7 C48 C61 122.0(8) . . ? N7 C48 C61A 124.6(8) . . ? C47 C48 C61 126.3(8) . . ? C47 C48 C61A 124.0(8) . . ? C61A C48 C61 19.0(7) . . ? N10 C49 C50 107.4(5) . . ? N10 C49 C67 125.8(6) . . ? C50 C49 C67 126.8(6) . . ? C49 C50 H50 126.9 . . ? C49 C50 C51 106.3(6) . . ? C51 C50 H50 126.9 . . ? N9 C51 C50 109.5(6) . . ? N9 C51 C73 122.6(5) . . ? C50 C51 C73 127.9(6) . . ? N12 C52 C53 108.3(5) . . ? N12 C52 C79 123.1(5) . . ? C53 C52 C79 128.6(6) . . ? C52 C53 H53 126.9 . . ? C52 C53 C54 106.3(5) . . ? C54 C53 H53 126.9 . . ? N11 C54 C53 110.0(5) . . ? N11 C54 C85 122.5(6) . . ? C53 C54 C85 127.5(6) . . ? C56 C55 C46 119.3(6) . . ? C56 C55 C60 119.3(6) . . ? C60 C55 C46 121.4(6) . . ? C55 C56 H56 119.6 . . ? C57 C56 C55 120.9(8) . . ? C57 C56 H56 119.6 . . ? C56 C57 H57 120.4 . . ? C56 C57 C58 119.2(8) . . ? C58 C57 H57 120.4 . . ? C57 C58 H58 119.8 . . ? C59 C58 C57 120.3(7) . . ? C59 C58 H58 119.8 . . ? C58 C59 H59 120.0 . . ? C58 C59 C60 120.1(8) . . ? C60 C59 H59 120.0 . . ? C55 C60 H60 119.9 . . ? C59 C60 C55 120.2(7) . . ? C59 C60 H60 119.9 . . ? C62 C61 C48 119.7(12) . . ? C66 C61 C48 122.4(13) . . ? C66 C61 C62 116.5(14) . . ? C48 C61A C66A 113.6(13) . . ? C62A C61A C48 126.3(14) . . ? C62A C61A C66A 119.6(16) . . ? C61 C62 H62 120.7 . . ? C63 C62 C61 118.6(15) . . ? C63 C62 H62 120.7 . . ? C61A C62A H62A 118.4 . . ? C61A C62A C63A 123(2) . . ? C63A C62A H62A 118.4 . . ? C62 C63 H63 118.7 . . ? C62 C63 C64 122.6(18) . . ? C64 C63 H63 118.7 . . ? C62A C63A H63A 118.3 . . ? C64A C63A C62A 123(2) . . ? C64A C63A H63A 118.3 . . ? C63 C64 H64 123.2 . . ? C65 C64 C63 113.6(17) . . ? C65 C64 H64 123.2 . . ? C63A C64A H64A 118.4 . . ? C63A C64A C65A 123(2) . . ? C65A C64A H64A 118.4 . . ? C64 C65 H65 117.5 . . ? C64 C65 C66 124.9(17) . . ? C66 C65 H65 117.5 . . ? C64A C65A H65A 125.6 . . ? C66A C65A C64A 109(2) . . ? C66A C65A H65A 125.6 . . ? C61 C66 C65 123.2(16) . . ? C61 C66 H66 118.4 . . ? C65 C66 H66 118.4 . . ? C61A C66A C65A 121(2) . . ? C61A C66A H66A 119.3 . . ? C65A C66A H66A 119.2 . . ? C68 C67 C49 119.2(6) . . ? C68 C67 C72 118.8(6) . . ? C72 C67 C49 122.0(6) . . ? C67 C68 H68 120.0 . . ? C67 C68 C69 120.0(7) . . ? C69 C68 H68 120.0 . . ? C68 C69 H69 119.5 . . ? C70 C69 C68 121.0(7) . . ? C70 C69 H69 119.5 . . ? C69 C70 H70 119.7 . . ? C69 C70 C71 120.6(7) . . ? C71 C70 H70 119.7 . . ? C70 C71 H71 120.2 . . ? C72 C71 C70 119.6(7) . . ? C72 C71 H71 120.2 . . ? C67 C72 H72 120.0 . . ? C71 C72 C67 120.0(6) . . ? C71 C72 H72 120.0 . . ? C74 C73 C51 120.3(6) . . ? C78 C73 C51 120.5(7) . . ? C78 C73 C74 119.2(7) . . ? C73 C74 H74 119.3 . . ? C75 C74 C73 121.4(9) . . ? C75 C74 H74 119.3 . . ? C74 C75 H75 119.9 . . ? C76 C75 C74 120.3(9) . . ? C76 C75 H75 119.9 . . ? C75 C76 H76 119.9 . . ? C75 C76 C77 120.2(8) . . ? C77 C76 H76 119.9 . . ? C76 C77 H77 119.9 . . ? C76 C77 C78 120.2(9) . . ? C78 C77 H77 119.9 . . ? C73 C78 C77 118.6(9) . . ? C73 C78 H78 120.7 . . ? C77 C78 H78 120.7 . . ? C80 C79 C52 119.6(6) . . ? C80 C79 C84 118.1(6) . . ? C84 C79 C52 122.3(5) . . ? C79 C80 H80 119.1 . . ? C81 C80 C79 121.7(7) . . ? C81 C80 H80 119.1 . . ? C80 C81 H81 120.1 . . ? C82 C81 C80 119.9(7) . . ? C82 C81 H81 120.1 . . ? C81 C82 H82 120.0 . . ? C81 C82 C83 120.0(6) . . ? C83 C82 H82 120.0 . . ? C82 C83 H83 120.0 . . ? C84 C83 C82 120.0(6) . . ? C84 C83 H83 120.0 . . ? C79 C84 H84 119.9 . . ? C83 C84 C79 120.3(6) . . ? C83 C84 H84 119.9 . . ? C86 C85 C54 119.0(6) . . ? C86 C85 C90 119.4(6) . . ? C90 C85 C54 121.5(6) . . ? C85 C86 H86 119.9 . . ? C87 C86 C85 120.2(7) . . ? C87 C86 H86 119.9 . . ? C86 C87 H87 119.3 . . ? C86 C87 C88 121.3(7) . . ? C88 C87 H87 119.3 . . ? C87 C88 H88 120.4 . . ? C87 C88 C89 119.2(8) . . ? C89 C88 H88 120.4 . . ? C88 C89 H89 119.8 . . ? C90 C89 C88 120.4(9) . . ? C90 C89 H89 119.8 . . ? C85 C90 H90 120.2 . . ? C89 C90 C85 119.5(8) . . ? C89 C90 H90 120.2 . . ? N13 C91 C92 169(2) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92B 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O1 C93 C98 118.9(10) . . ? C94 C93 O1 120.8(9) . . ? C94 C93 C98 119.7(9) . . ? C93 C94 H94 119.0 . . ? C93 C94 C95 122.0(9) . . ? C95 C94 H94 119.0 . . ? C94 C95 C99 115.8(10) . . ? C96 C95 C94 120.0(9) . . ? C96 C95 C99 124.0(9) . . ? O2 C96 C95 119.8(11) . . ? C97 C96 O2 121.7(11) . . ? C97 C96 C95 118.4(9) . . ? C96 C97 C98 122.6(11) . . ? C96 C97 C100 121.3(10) . . ? C98 C97 C100 116.1(12) . . ? C93 C98 C97 116.3(10) . . ? C93 C98 H98 121.8 . . ? C97 C98 H98 121.8 . . ? C95 C99 H99A 109.5 . . ? C95 C99 H99B 109.5 . . ? C95 C99 H99C 109.5 . . ? H99A C99 H99B 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C97 C100 H10A 109.5 . . ? C97 C100 H10B 109.5 . . ? C97 C100 H10C 109.5 . . ? H10A C100 H10B 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N2 B1 H1 109.7 . . ? N4 B1 N2 108.7(5) . . ? N4 B1 H1 109.7 . . ? N6 B1 N2 109.4(5) . . ? N6 B1 N4 109.6(5) . . ? N6 B1 H1 109.7 . . ? N8 B2 N10 109.7(5) . . ? N8 B2 H2A 109.1 . . ? N10 B2 H2A 109.1 . . ? N12 B2 N8 110.3(5) . . ? N12 B2 N10 109.6(5) . . ? N12 B2 H2A 109.1 . . ? Cl1 C1S H1SA 109.3 . . ? Cl1 C1S H1SB 109.3 . . ? H1SA C1S H1SB 108.0 . . ? C2S C1S Cl1 111.5(7) . . ? C2S C1S H1SA 109.3 . . ? C2S C1S H1SB 109.3 . . ? Cl2 C2S H2SA 108.7 . . ? Cl2 C2S H2SB 108.7 . . ? C1S C2S Cl2 114.3(8) . . ? C1S C2S H2SA 108.7 . . ? C1S C2S H2SB 108.7 . . ? H2SA C2S H2SB 107.6 . . ? Cl3 C3S H3SA 110.4 . . ? Cl3 C3S H3SB 110.4 . . ? H3SA C3S H3SB 108.6 . . ? C4S C3S Cl3 106.8(14) . . ? C4S C3S H3SA 110.4 . . ? C4S C3S H3SB 110.4 . . ? Cl4 C4S H4SA 108.3 . . ? Cl4 C4S H4SB 108.3 . . ? C3S C4S Cl4 116.1(13) . . ? C3S C4S H4SA 108.2 . . ? C3S C4S H4SB 108.3 . . ? H4SA C4S H4SB 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 O1 C93 C94 -118.1(13) . . . . ? Fe1 O1 C93 C98 71.0(19) . . . . ? Fe1 N1 C9 C8 171.5(5) . . . . ? Fe1 N1 C9 C40 -8.3(10) . . . . ? Fe1 N3 C3 C2 -172.3(5) . . . . ? Fe1 N3 C3 C16 7.7(11) . . . . ? Fe1 N5 C6 C5 -166.4(5) . . . . ? Fe1 N5 C6 C28 17.4(10) . . . . ? Fe1 N13 C91 C92 146(6) . . . . ? Fe2 O2 C96 C95 -127.9(15) . . . . ? Fe2 O2 C96 C97 48(3) . . . . ? Fe2 N7 C48 C47 178.8(6) . . . . ? Fe2 N7 C48 C61 -13.0(14) . . . . ? Fe2 N7 C48 C61A 9.6(14) . . . . ? Fe2 N9 C51 C50 -179.5(5) . . . . ? Fe2 N9 C51 C73 1.5(10) . . . . ? Fe2 N11 C54 C53 -170.6(5) . . . . ? Fe2 N11 C54 C85 11.3(10) . . . . ? O1 Fe1 N1 N2 -146.6(4) . . . . ? O1 Fe1 N1 C9 40.3(8) . . . . ? O1 Fe1 N3 N4 149.5(4) . . . . ? O1 Fe1 N3 C3 -37.8(8) . . . . ? O1 Fe1 N5 N6 -168.1(5) . . . . ? O1 Fe1 N5 C6 -0.9(7) . . . . ? O1 Fe1 N13 C91 27.5(19) . . . . ? O1 C93 C94 C95 179.4(10) . . . . ? O1 C93 C98 C97 178.6(12) . . . . ? O2 Fe2 N7 N8 -179.7(5) . . . . ? O2 Fe2 N7 C48 0.6(10) . . . . ? O2 Fe2 N9 N10 -169.5(4) . . . . ? O2 Fe2 N9 C51 8.9(8) . . . . ? O2 Fe2 N11 N12 -173.2(5) . . . . ? O2 Fe2 N11 C54 -3.1(8) . . . . ? O2 C96 C97 C98 176.5(13) . . . . ? O2 C96 C97 C100 -4(2) . . . . ? N1 Fe1 O1 C93 -122.6(13) . . . . ? N1 Fe1 N3 N4 -37.4(4) . . . . ? N1 Fe1 N3 C3 135.3(6) . . . . ? N1 Fe1 N5 N6 56.2(4) . . . . ? N1 Fe1 N5 C6 -136.6(7) . . . . ? N1 Fe1 N13 C91 163.6(19) . . . . ? N1 N2 C7 C8 -0.6(7) . . . . ? N1 N2 C7 C34 -177.1(6) . . . . ? N1 N2 B1 N4 -59.4(7) . . . . ? N1 N2 B1 N6 60.2(7) . . . . ? N1 C9 C40 C41 154.6(7) . . . . ? N1 C9 C40 C45 -26.3(10) . . . . ? N2 N1 C9 C8 -2.0(7) . . . . ? N2 N1 C9 C40 178.2(6) . . . . ? N2 C7 C8 C9 -0.7(7) . . . . ? N2 C7 C34 C35 -129.4(7) . . . . ? N2 C7 C34 C39 53.0(9) . . . . ? N3 Fe1 O1 C93 47.4(15) . . . . ? N3 Fe1 N1 N2 40.7(4) . . . . ? N3 Fe1 N1 C9 -132.4(6) . . . . ? N3 Fe1 N5 N6 -34.8(4) . . . . ? N3 Fe1 N5 C6 132.3(7) . . . . ? N3 Fe1 N13 C91 -105.4(19) . . . . ? N3 N4 C1 C2 -0.6(7) . . . . ? N3 N4 C1 C10 177.1(6) . . . . ? N3 N4 B1 N2 62.9(7) . . . . ? N3 N4 B1 N6 -56.7(7) . . . . ? N3 C3 C16 C17 -146.4(7) . . . . ? N3 C3 C16 C21 30.5(11) . . . . ? N4 N3 C3 C2 0.9(7) . . . . ? N4 N3 C3 C16 -179.1(6) . . . . ? N4 C1 C2 C3 1.1(8) . . . . ? N4 C1 C10 C11 -126.6(7) . . . . ? N4 C1 C10 C15 54.0(9) . . . . ? N5 Fe1 O1 C93 145.2(13) . . . . ? N5 Fe1 N1 N2 -47.5(4) . . . . ? N5 Fe1 N1 C9 139.3(6) . . . . ? N5 Fe1 N3 N4 46.3(4) . . . . ? N5 Fe1 N3 C3 -140.9(6) . . . . ? N5 Fe1 N13 C91 -161.4(19) . . . . ? N5 N6 C4 C5 0.6(7) . . . . ? N5 N6 C4 C22 178.9(6) . . . . ? N5 N6 B1 N2 -49.0(7) . . . . ? N5 N6 B1 N4 70.1(7) . . . . ? N5 C6 C28 C29 -136.6(7) . . . . ? N5 C6 C28 C33 45.1(10) . . . . ? N6 N5 C6 C5 1.6(7) . . . . ? N6 N5 C6 C28 -174.6(6) . . . . ? N6 C4 C5 C6 0.4(7) . . . . ? N6 C4 C22 C23 -144.7(7) . . . . ? N6 C4 C22 C27 37.3(10) . . . . ? N7 Fe2 O2 C96 32(2) . . . . ? N7 Fe2 N9 N10 47.1(4) . . . . ? N7 Fe2 N9 C51 -134.5(7) . . . . ? N7 Fe2 N11 N12 -38.6(4) . . . . ? N7 Fe2 N11 C54 131.5(7) . . . . ? N7 N8 C46 C47 1.3(8) . . . . ? N7 N8 C46 C55 -176.2(6) . . . . ? N7 N8 B2 N10 69.2(7) . . . . ? N7 N8 B2 N12 -51.5(7) . . . . ? N7 C48 C61 C62 -149.7(12) . . . . ? N7 C48 C61 C66 44.2(19) . . . . ? N7 C48 C61A C62A 140.5(15) . . . . ? N7 C48 C61A C66A -48.1(17) . . . . ? N8 N7 C48 C47 -0.9(9) . . . . ? N8 N7 C48 C61 167.3(9) . . . . ? N8 N7 C48 C61A -170.1(9) . . . . ? N8 C46 C47 C48 -1.8(8) . . . . ? N8 C46 C55 C56 -132.3(7) . . . . ? N8 C46 C55 C60 50.0(9) . . . . ? N9 Fe2 O2 C96 -99.6(19) . . . . ? N9 Fe2 N7 N8 -35.8(4) . . . . ? N9 Fe2 N7 C48 144.5(8) . . . . ? N9 Fe2 N11 N12 53.2(4) . . . . ? N9 Fe2 N11 C54 -136.7(7) . . . . ? N9 N10 C49 C50 1.2(7) . . . . ? N9 N10 C49 C67 -179.1(5) . . . . ? N9 N10 B2 N8 -55.0(7) . . . . ? N9 N10 B2 N12 66.2(6) . . . . ? N9 C51 C73 C74 129.6(7) . . . . ? N9 C51 C73 C78 -50.3(9) . . . . ? N10 N9 C51 C50 -0.9(7) . . . . ? N10 N9 C51 C73 180.0(6) . . . . ? N10 C49 C50 C51 -1.7(7) . . . . ? N10 C49 C67 C68 -142.6(7) . . . . ? N10 C49 C67 C72 40.2(10) . . . . ? N11 Fe2 O2 C96 147.7(18) . . . . ? N11 Fe2 N7 N8 51.6(4) . . . . ? N11 Fe2 N7 C48 -128.1(8) . . . . ? N11 Fe2 N9 N10 -42.9(4) . . . . ? N11 Fe2 N9 C51 135.6(7) . . . . ? N11 N12 C52 C53 -0.1(7) . . . . ? N11 N12 C52 C79 177.7(5) . . . . ? N11 N12 B2 N8 67.6(7) . . . . ? N11 N12 B2 N10 -53.2(7) . . . . ? N11 C54 C85 C86 -153.2(6) . . . . ? N11 C54 C85 C90 29.9(9) . . . . ? N12 N11 C54 C53 0.0(7) . . . . ? N12 N11 C54 C85 -178.2(5) . . . . ? N12 C52 C53 C54 0.1(7) . . . . ? N12 C52 C79 C80 -133.5(6) . . . . ? N12 C52 C79 C84 47.7(8) . . . . ? N13 Fe1 O1 C93 -36.2(14) . . . . ? N13 Fe1 N1 N2 127.1(4) . . . . ? N13 Fe1 N1 C9 -46.1(6) . . . . ? N13 Fe1 N3 N4 -125.9(4) . . . . ? N13 Fe1 N3 C3 46.8(7) . . . . ? N13 Fe1 N5 N6 21.0(17) . . . . ? N13 Fe1 N5 C6 -171.8(13) . . . . ? C1 N4 N3 Fe1 174.6(4) . . . . ? C1 N4 N3 C3 -0.2(7) . . . . ? C1 N4 B1 N2 -120.4(7) . . . . ? C1 N4 B1 N6 120.0(7) . . . . ? C1 C2 C3 N3 -1.2(8) . . . . ? C1 C2 C3 C16 178.8(7) . . . . ? C1 C10 C11 C12 178.8(6) . . . . ? C1 C10 C15 C14 -178.8(6) . . . . ? C2 C1 C10 C11 50.6(10) . . . . ? C2 C1 C10 C15 -128.7(8) . . . . ? C2 C3 C16 C17 33.6(11) . . . . ? C2 C3 C16 C21 -149.5(8) . . . . ? C3 C16 C17 C18 -177.3(7) . . . . ? C3 C16 C21 C20 178.4(7) . . . . ? C4 N6 N5 Fe1 169.7(4) . . . . ? C4 N6 N5 C6 -1.4(7) . . . . ? C4 N6 B1 N2 125.8(7) . . . . ? C4 N6 B1 N4 -115.1(7) . . . . ? C4 C5 C6 N5 -1.3(8) . . . . ? C4 C5 C6 C28 174.5(7) . . . . ? C4 C22 C23 C24 -177.8(7) . . . . ? C4 C22 C27 C26 179.4(6) . . . . ? C5 C4 C22 C23 33.2(10) . . . . ? C5 C4 C22 C27 -144.9(7) . . . . ? C5 C6 C28 C29 48.0(11) . . . . ? C5 C6 C28 C33 -130.3(9) . . . . ? C6 C28 C29 C30 -179.5(8) . . . . ? C6 C28 C33 C32 178.0(7) . . . . ? C7 N2 N1 Fe1 -173.4(4) . . . . ? C7 N2 N1 C9 1.6(7) . . . . ? C7 N2 B1 N4 113.7(7) . . . . ? C7 N2 B1 N6 -126.6(6) . . . . ? C7 C8 C9 N1 1.7(7) . . . . ? C7 C8 C9 C40 -178.6(6) . . . . ? C7 C34 C35 C36 -175.6(6) . . . . ? C7 C34 C39 C38 176.6(6) . . . . ? C8 C7 C34 C35 54.7(9) . . . . ? C8 C7 C34 C39 -122.9(8) . . . . ? C8 C9 C40 C41 -25.1(11) . . . . ? C8 C9 C40 C45 154.0(7) . . . . ? C9 C40 C41 C42 178.5(9) . . . . ? C9 C40 C45 C44 -180.0(7) . . . . ? C10 C1 C2 C3 -176.5(6) . . . . ? C10 C11 C12 C13 0.7(11) . . . . ? C11 C10 C15 C14 1.9(10) . . . . ? C11 C12 C13 C14 0.4(12) . . . . ? C12 C13 C14 C15 -0.3(12) . . . . ? C13 C14 C15 C10 -0.8(11) . . . . ? C15 C10 C11 C12 -1.8(10) . . . . ? C16 C17 C18 C19 -0.9(14) . . . . ? C17 C16 C21 C20 -4.8(12) . . . . ? C17 C18 C19 C20 -4.7(16) . . . . ? C18 C19 C20 C21 5.8(15) . . . . ? C19 C20 C21 C16 -1.1(14) . . . . ? C21 C16 C17 C18 5.7(12) . . . . ? C22 C4 C5 C6 -177.8(6) . . . . ? C22 C23 C24 C25 -2.8(12) . . . . ? C23 C22 C27 C26 1.4(10) . . . . ? C23 C24 C25 C26 3.6(12) . . . . ? C24 C25 C26 C27 -1.9(12) . . . . ? C25 C26 C27 C22 -0.6(11) . . . . ? C27 C22 C23 C24 0.3(11) . . . . ? C28 C29 C30 C31 1.6(13) . . . . ? C29 C28 C33 C32 -0.3(12) . . . . ? C29 C30 C31 C32 -0.5(14) . . . . ? C30 C31 C32 C33 -0.9(14) . . . . ? C31 C32 C33 C28 1.4(13) . . . . ? C33 C28 C29 C30 -1.2(12) . . . . ? C34 C7 C8 C9 175.8(6) . . . . ? C34 C35 C36 C37 -2.2(11) . . . . ? C35 C34 C39 C38 -1.0(10) . . . . ? C35 C36 C37 C38 1.4(12) . . . . ? C36 C37 C38 C39 -0.3(11) . . . . ? C37 C38 C39 C34 0.1(10) . . . . ? C39 C34 C35 C36 2.0(10) . . . . ? C40 C41 C42 C43 2.0(16) . . . . ? C41 C40 C45 C44 -0.9(12) . . . . ? C41 C42 C43 C44 -1.9(17) . . . . ? C42 C43 C44 C45 0.3(16) . . . . ? C43 C44 C45 C40 1.0(13) . . . . ? C45 C40 C41 C42 -0.7(13) . . . . ? C46 N8 N7 Fe2 179.9(4) . . . . ? C46 N8 N7 C48 -0.2(7) . . . . ? C46 N8 B2 N10 -127.1(7) . . . . ? C46 N8 B2 N12 112.1(7) . . . . ? C46 C47 C48 N7 1.7(9) . . . . ? C46 C47 C48 C61 -165.9(10) . . . . ? C46 C47 C48 C61A 170.9(9) . . . . ? C46 C55 C56 C57 -176.2(6) . . . . ? C46 C55 C60 C59 175.9(6) . . . . ? C47 C46 C55 C56 50.7(11) . . . . ? C47 C46 C55 C60 -127.0(8) . . . . ? C47 C48 C61 C62 16.5(19) . . . . ? C47 C48 C61 C66 -149.5(13) . . . . ? C47 C48 C61A C62A -27(2) . . . . ? C47 C48 C61A C66A 144.1(12) . . . . ? C48 C61 C62 C63 -169.7(14) . . . . ? C48 C61 C66 C65 171.2(15) . . . . ? C48 C61A C62A C63A 173.5(16) . . . . ? C48 C61A C66A C65A -177.8(17) . . . . ? C49 N10 N9 Fe2 178.7(4) . . . . ? C49 N10 N9 C51 -0.2(7) . . . . ? C49 N10 B2 N8 118.0(7) . . . . ? C49 N10 B2 N12 -120.7(7) . . . . ? C49 C50 C51 N9 1.7(7) . . . . ? C49 C50 C51 C73 -179.3(6) . . . . ? C49 C67 C68 C69 179.5(6) . . . . ? C49 C67 C72 C71 179.1(6) . . . . ? C50 C49 C67 C68 37.0(9) . . . . ? C50 C49 C67 C72 -140.2(7) . . . . ? C50 C51 C73 C74 -49.3(10) . . . . ? C50 C51 C73 C78 130.8(7) . . . . ? C51 C73 C74 C75 178.9(7) . . . . ? C51 C73 C78 C77 179.4(7) . . . . ? C52 N12 N11 Fe2 173.4(4) . . . . ? C52 N12 N11 C54 0.1(6) . . . . ? C52 N12 B2 N8 -119.5(7) . . . . ? C52 N12 B2 N10 119.7(6) . . . . ? C52 C53 C54 N11 0.0(7) . . . . ? C52 C53 C54 C85 178.0(6) . . . . ? C52 C79 C80 C81 179.4(6) . . . . ? C52 C79 C84 C83 -178.9(6) . . . . ? C53 C52 C79 C80 43.9(9) . . . . ? C53 C52 C79 C84 -134.9(7) . . . . ? C53 C54 C85 C86 29.0(9) . . . . ? C53 C54 C85 C90 -147.9(7) . . . . ? C54 C85 C86 C87 -177.6(6) . . . . ? C54 C85 C90 C89 176.7(7) . . . . ? C55 C46 C47 C48 175.6(7) . . . . ? C55 C56 C57 C58 -0.4(11) . . . . ? C56 C55 C60 C59 -1.8(10) . . . . ? C56 C57 C58 C59 -0.7(12) . . . . ? C57 C58 C59 C60 0.4(12) . . . . ? C58 C59 C60 C55 0.8(11) . . . . ? C60 C55 C56 C57 1.6(10) . . . . ? C61 C48 C61A C62A -131(4) . . . . ? C61 C48 C61A C66A 41(2) . . . . ? C61 C62 C63 C64 -4(3) . . . . ? C61A C48 C61 C62 106(3) . . . . ? C61A C48 C61 C66 -60(3) . . . . ? C61A C62A C63A C64A 2(4) . . . . ? C62 C61 C66 C65 5(3) . . . . ? C62 C63 C64 C65 9(3) . . . . ? C62A C61A C66A C65A -6(3) . . . . ? C62A C63A C64A C65A -4(4) . . . . ? C63 C64 C65 C66 -7(3) . . . . ? C63A C64A C65A C66A 0(3) . . . . ? C64 C65 C66 C61 1(3) . . . . ? C64A C65A C66A C61A 4(3) . . . . ? C66 C61 C62 C63 -3(2) . . . . ? C66A C61A C62A C63A 3(3) . . . . ? C67 C49 C50 C51 178.6(6) . . . . ? C67 C68 C69 C70 1.7(11) . . . . ? C68 C67 C72 C71 1.9(9) . . . . ? C68 C69 C70 C71 1.2(11) . . . . ? C69 C70 C71 C72 -2.4(11) . . . . ? C70 C71 C72 C67 0.9(10) . . . . ? C72 C67 C68 C69 -3.2(10) . . . . ? C73 C74 C75 C76 0.9(13) . . . . ? C74 C73 C78 C77 -0.6(11) . . . . ? C74 C75 C76 C77 1.2(13) . . . . ? C75 C76 C77 C78 -3.0(13) . . . . ? C76 C77 C78 C73 2.7(12) . . . . ? C78 C73 C74 C75 -1.2(11) . . . . ? C79 C52 C53 C54 -177.6(6) . . . . ? C79 C80 C81 C82 1.1(11) . . . . ? C80 C79 C84 C83 2.3(9) . . . . ? C80 C81 C82 C83 -0.9(11) . . . . ? C81 C82 C83 C84 1.4(10) . . . . ? C82 C83 C84 C79 -2.1(9) . . . . ? C84 C79 C80 C81 -1.8(9) . . . . ? C85 C86 C87 C88 0.7(12) . . . . ? C86 C85 C90 C89 -0.2(11) . . . . ? C86 C87 C88 C89 0.2(14) . . . . ? C87 C88 C89 C90 -1.0(14) . . . . ? C88 C89 C90 C85 1.0(13) . . . . ? C90 C85 C86 C87 -0.7(10) . . . . ? C93 C94 C95 C96 3.2(16) . . . . ? C93 C94 C95 C99 177.6(11) . . . . ? C94 C93 C98 C97 8(2) . . . . ? C94 C95 C96 O2 -178.4(10) . . . . ? C94 C95 C96 C97 5.4(17) . . . . ? C95 C96 C97 C98 -7(2) . . . . ? C95 C96 C97 C100 171.7(13) . . . . ? C96 C97 C98 C93 1(2) . . . . ? C98 C93 C94 C95 -9.8(18) . . . . ? C99 C95 C96 O2 7.8(18) . . . . ? C99 C95 C96 C97 -168.4(12) . . . . ? C100 C97 C98 C93 -178.1(14) . . . . ? B1 N2 N1 Fe1 0.9(7) . . . . ? B1 N2 N1 C9 175.9(5) . . . . ? B1 N2 C7 C8 -174.5(6) . . . . ? B1 N2 C7 C34 8.9(10) . . . . ? B1 N4 N3 Fe1 -8.1(6) . . . . ? B1 N4 N3 C3 177.2(5) . . . . ? B1 N4 C1 C2 -177.5(6) . . . . ? B1 N4 C1 C10 0.2(10) . . . . ? B1 N6 N5 Fe1 -14.5(7) . . . . ? B1 N6 N5 C6 174.5(5) . . . . ? B1 N6 C4 C5 -174.5(6) . . . . ? B1 N6 C4 C22 3.7(11) . . . . ? B2 N8 N7 Fe2 -13.5(7) . . . . ? B2 N8 N7 C48 166.4(6) . . . . ? B2 N8 C46 C47 -163.8(6) . . . . ? B2 N8 C46 C55 18.6(10) . . . . ? B2 N10 N9 Fe2 -6.9(6) . . . . ? B2 N10 N9 C51 174.2(5) . . . . ? B2 N10 C49 C50 -172.3(6) . . . . ? B2 N10 C49 C67 7.4(10) . . . . ? B2 N12 N11 Fe2 -12.2(6) . . . . ? B2 N12 N11 C54 174.4(5) . . . . ? B2 N12 C52 C53 -173.6(6) . . . . ? B2 N12 C52 C79 4.2(10) . . . . ? Cl1 C1S C2S Cl2 65.9(10) . . . . ? Cl3 C3S C4S Cl4 77.6(16) . . . . ? # end Validation Reply Form loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 8 0 5 0.0295 8.0031 0.0024 4.9979 0.3585 0.8502 0.3196 -7 0 14 0.0119 -7.0013 -0.0013 14.0105 -0.0812 -0.2411 -0.9453 2 6 -2 0.1399 1.9992 6.0057 -2.0060 0.8929 -0.2402 0.2169 0 -6 -2 0.2001 0.0011 -6.0054 -1.9970 -0.8697 0.3091 0.0532 7 -1 -16 0.0251 7.0014 -0.9997 -16.0108 -0.0849 0.2470 1.0145 -5 0 -16 0.0068 -5.0029 -0.0021 -16.0048 -0.3870 -0.8837 0.2666 # start Validation Reply Form _vrf_PLAT201_Complex2E ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 12 RESPONSE: In two disordered Ph rings anisotropic refinement of atoms was not feasible because of ensuing large correlations ; _vrf_PLAT360_Complex2E ; PROBLEM: Short C(sp3)-C(sp3) Bond C52 - C53 ... 1.16 Ang. RESPONSE: This is a result of unresolved disorder in the solvent molecule ; _vrf_PLAT222_Complex2F ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: Some parts of the molecule are very much disordered, particularly the central bridging ligand and MeCN molecule. This results in the observed discrepancy. ; # end Validation Reply Form #==END