# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Christopher Levy' _publ_contact_author_address ; Department of Chemistry Kansas State University KSU Department of Chemistry 111 Willard Hall Manhattan Kansas 66502 UNITED STATES OF AMERICA ; _publ_contact_author_email CLEVY@KSU.EDU _publ_section_title ; Iron(II) and Zinc(II) Monohelical Binaphthyl Salen Complexes ; loop_ _publ_author_name 'Christopher Levy' 'John Desper' 'Alexander V. Wiznycia' data_Compound_(R)-3 _database_code_depnum_ccdc_archive 'CCDC 276257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,3'-(phenanthrenol imine)-2,2'-binaphthyl ; _chemical_name_common "3,3'-(phenanthrenol imine)-2,2'-binaphthyl" _chemical_melting_point ? _chemical_formula_moiety 'C50 H32 N2 O2' _chemical_formula_sum 'C50 H32 N2 O2' _chemical_formula_weight 692.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0977(6) _cell_length_b 16.4934(10) _cell_length_c 18.7071(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3424.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 7648 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 26.15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24779 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4512 _reflns_number_gt 3586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4512 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 0.3058(2) 0.44487(12) 0.47665(11) 0.0273(5) Uani 1 1 d . . . C02 C 0.1888(2) 0.42922(13) 0.45499(11) 0.0299(5) Uani 1 1 d . . . N02 N 0.12954(18) 0.48952(11) 0.41469(10) 0.0326(4) Uani 1 1 d . . . C03 C 0.1316(2) 0.35678(14) 0.47555(13) 0.0361(5) Uani 1 1 d . . . H03 H 0.0531 0.3458 0.4592 0.043 Uiso 1 1 calc R . . C04 C 0.1876(2) 0.30299(14) 0.51831(13) 0.0371(6) Uani 1 1 d . . . H04 H 0.1485 0.2542 0.5300 0.045 Uiso 1 1 calc R . . C05 C 0.3030(2) 0.31824(13) 0.54572(11) 0.0322(5) Uani 1 1 d . . . C06 C 0.3592(3) 0.26642(14) 0.59563(13) 0.0408(6) Uani 1 1 d . . . H06 H 0.3187 0.2196 0.6113 0.049 Uiso 1 1 calc R . . C07 C 0.4705(3) 0.28308(15) 0.62123(13) 0.0449(7) Uani 1 1 d . . . H07 H 0.5056 0.2488 0.6556 0.054 Uiso 1 1 calc R . . C08 C 0.5336(3) 0.35096(15) 0.59683(14) 0.0438(6) Uani 1 1 d . . . H08 H 0.6122 0.3608 0.6134 0.053 Uiso 1 1 calc R . . C09 C 0.4822(2) 0.40302(14) 0.54928(12) 0.0361(5) Uani 1 1 d . . . H09 H 0.5256 0.4485 0.5334 0.043 Uiso 1 1 calc R . . C10 C 0.3642(2) 0.38938(13) 0.52349(11) 0.0290(5) Uani 1 1 d . . . C11 C 0.3706(2) 0.51775(13) 0.44984(11) 0.0277(5) Uani 1 1 d . . . C12 C 0.4563(2) 0.50916(13) 0.39724(12) 0.0312(5) Uani 1 1 d . . . N12 N 0.47810(18) 0.42974(11) 0.37289(10) 0.0325(4) Uani 1 1 d . . . C13 C 0.5193(2) 0.57763(14) 0.37058(14) 0.0402(6) Uani 1 1 d . . . H13 H 0.5799 0.5709 0.3360 0.048 Uiso 1 1 calc R . . C14 C 0.4921(3) 0.65269(14) 0.39507(14) 0.0409(6) Uani 1 1 d . . . H14 H 0.5329 0.6978 0.3762 0.049 Uiso 1 1 calc R . . C15 C 0.4040(2) 0.66462(14) 0.44815(13) 0.0352(5) Uani 1 1 d . . . C16 C 0.3734(3) 0.74287(14) 0.47309(14) 0.0427(6) Uani 1 1 d . . . H16 H 0.4119 0.7885 0.4536 0.051 Uiso 1 1 calc R . . C17 C 0.2895(3) 0.75283(15) 0.52462(15) 0.0461(7) Uani 1 1 d . . . H17 H 0.2684 0.8053 0.5398 0.055 Uiso 1 1 calc R . . C18 C 0.2340(3) 0.68550(15) 0.55525(14) 0.0422(6) Uani 1 1 d . . . H18 H 0.1778 0.6930 0.5922 0.051 Uiso 1 1 calc R . . C19 C 0.2600(2) 0.60873(14) 0.53247(13) 0.0364(6) Uani 1 1 d . . . H19 H 0.2213 0.5640 0.5536 0.044 Uiso 1 1 calc R . . C20 C 0.3449(2) 0.59653(13) 0.47727(12) 0.0296(5) Uani 1 1 d . . . C21 C 0.0009(2) 0.62015(14) 0.35053(12) 0.0323(5) Uani 1 1 d . . . O21 O 0.10049(16) 0.63852(11) 0.38608(10) 0.0429(4) Uani 1 1 d . . . H21 H 0.136(3) 0.5869(16) 0.4032(14) 0.043 Uiso 1 1 d . . . C22 C -0.0347(2) 0.53837(14) 0.34535(12) 0.0331(5) Uani 1 1 d . . . C23 C -0.1367(2) 0.51833(16) 0.30455(13) 0.0396(6) Uani 1 1 d . . . H23 H -0.1613 0.4639 0.3016 0.048 Uiso 1 1 calc R . . C24 C -0.1999(2) 0.57583(15) 0.26953(13) 0.0385(6) Uani 1 1 d . . . H24 H -0.2660 0.5609 0.2410 0.046 Uiso 1 1 calc R . . C25 C -0.1671(2) 0.65849(15) 0.27551(12) 0.0351(5) Uani 1 1 d . . . C26 C -0.2364(2) 0.71735(16) 0.23790(14) 0.0421(6) Uani 1 1 d . . . H26 H -0.3030 0.7006 0.2106 0.050 Uiso 1 1 calc R . . C27 C -0.2080(3) 0.79642(17) 0.24084(14) 0.0453(7) Uani 1 1 d . . . H27 H -0.2530 0.8338 0.2138 0.054 Uiso 1 1 calc R . . C28 C -0.1118(3) 0.82474(15) 0.28392(12) 0.0388(6) Uani 1 1 d . . . C29 C -0.0877(3) 0.90778(16) 0.28886(14) 0.0483(7) Uani 1 1 d . . . H29 H -0.1336 0.9443 0.2615 0.058 Uiso 1 1 calc R . . C30 C -0.0005(3) 0.93661(17) 0.33184(15) 0.0528(8) Uani 1 1 d . . . H30 H 0.0144 0.9926 0.3342 0.063 Uiso 1 1 calc R . . C31 C 0.0672(3) 0.88341(17) 0.37270(15) 0.0528(7) Uani 1 1 d . . . H31 H 0.1268 0.9038 0.4036 0.063 Uiso 1 1 calc R . . C32 C 0.0487(3) 0.80149(15) 0.36869(14) 0.0425(6) Uani 1 1 d . . . H32 H 0.0964 0.7665 0.3964 0.051 Uiso 1 1 calc R . . C33 C -0.0409(2) 0.76872(14) 0.32357(12) 0.0346(5) Uani 1 1 d . . . C34 C -0.0676(2) 0.68260(14) 0.31718(12) 0.0312(5) Uani 1 1 d . . . C35 C 0.0314(2) 0.47553(14) 0.38037(12) 0.0342(5) Uani 1 1 d . . . H35 H 0.0021 0.4221 0.3783 0.041 Uiso 1 1 calc R . . C41 C 0.5158(2) 0.26408(13) 0.34183(12) 0.0309(5) Uani 1 1 d . . . O41 O 0.43446(16) 0.28234(10) 0.39052(9) 0.0379(4) Uani 1 1 d . . . H41 H 0.436(3) 0.3447(17) 0.3960(13) 0.045 Uiso 1 1 d . . . C42 C 0.5757(2) 0.32702(14) 0.30541(12) 0.0332(5) Uani 1 1 d . . . C43 C 0.6627(2) 0.30757(16) 0.25311(13) 0.0400(6) Uani 1 1 d . . . H43 H 0.7008 0.3493 0.2273 0.048 Uiso 1 1 calc R . . C44 C 0.6919(3) 0.22920(16) 0.23981(14) 0.0430(6) Uani 1 1 d . . . H44 H 0.7505 0.2171 0.2052 0.052 Uiso 1 1 calc R . . C45 C 0.6355(2) 0.16595(15) 0.27714(13) 0.0393(6) Uani 1 1 d . . . C46 C 0.6731(3) 0.08404(17) 0.26417(15) 0.0489(7) Uani 1 1 d . . . H46 H 0.7351 0.0740 0.2311 0.059 Uiso 1 1 calc R . . C47 C 0.6216(3) 0.02160(17) 0.29814(16) 0.0516(7) Uani 1 1 d . . . H47 H 0.6487 -0.0313 0.2887 0.062 Uiso 1 1 calc R . . C48 C 0.5271(3) 0.03353(15) 0.34811(15) 0.0454(7) Uani 1 1 d . . . C49 C 0.4744(3) -0.03337(16) 0.38253(18) 0.0557(8) Uani 1 1 d . . . H49 H 0.5014 -0.0859 0.3713 0.067 Uiso 1 1 calc R . . C50 C 0.3852(3) -0.02398(18) 0.4318(2) 0.0611(9) Uani 1 1 d . . . H50 H 0.3515 -0.0693 0.4547 0.073 Uiso 1 1 calc R . . C51 C 0.3446(3) 0.05394(16) 0.44748(17) 0.0526(7) Uani 1 1 d . . . H51 H 0.2829 0.0610 0.4813 0.063 Uiso 1 1 calc R . . C52 C 0.3932(2) 0.12024(15) 0.41440(14) 0.0421(6) Uani 1 1 d . . . H52 H 0.3633 0.1720 0.4256 0.051 Uiso 1 1 calc R . . C53 C 0.4867(2) 0.11304(14) 0.36407(13) 0.0353(5) Uani 1 1 d . . . C54 C 0.5444(2) 0.18085(14) 0.32762(12) 0.0328(5) Uani 1 1 d . . . C55 C 0.5533(2) 0.40995(14) 0.32309(12) 0.0336(5) Uani 1 1 d . . . H55 H 0.5941 0.4510 0.2980 0.040 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 C01 0.0291(12) 0.0244(10) 0.0284(10) -0.0027(8) 0.0032(10) 0.0008(9) C02 0.0308(12) 0.0287(11) 0.0303(10) 0.0000(8) 0.0041(10) 0.0014(9) N02 0.0260(10) 0.0363(10) 0.0355(10) 0.0019(8) 0.0002(8) -0.0006(9) C03 0.0298(13) 0.0412(13) 0.0373(12) -0.0006(10) 0.0012(11) -0.0064(11) C04 0.0408(14) 0.0318(12) 0.0387(12) 0.0015(9) 0.0074(12) -0.0082(11) C05 0.0367(13) 0.0306(11) 0.0295(10) -0.0011(9) 0.0055(10) 0.0025(10) C06 0.0548(18) 0.0300(12) 0.0375(12) 0.0069(10) 0.0064(13) 0.0048(12) C07 0.0567(18) 0.0391(14) 0.0390(13) 0.0065(11) -0.0044(14) 0.0130(13) C08 0.0420(16) 0.0456(14) 0.0439(13) 0.0004(11) -0.0104(13) 0.0064(12) C09 0.0369(13) 0.0332(12) 0.0383(12) -0.0007(10) -0.0047(11) 0.0012(11) C10 0.0332(13) 0.0261(11) 0.0276(10) -0.0030(8) 0.0021(10) 0.0025(9) C11 0.0257(12) 0.0254(11) 0.0320(10) 0.0007(8) -0.0026(9) 0.0004(9) C12 0.0306(13) 0.0255(11) 0.0374(11) -0.0027(9) -0.0018(10) -0.0007(9) N12 0.0323(11) 0.0280(10) 0.0373(10) -0.0033(8) 0.0020(9) -0.0005(8) C13 0.0386(14) 0.0348(13) 0.0473(14) -0.0013(10) 0.0074(12) -0.0077(11) C14 0.0433(15) 0.0274(12) 0.0521(14) 0.0024(10) 0.0018(13) -0.0101(11) C15 0.0382(14) 0.0267(11) 0.0406(12) -0.0011(9) -0.0074(11) 0.0002(10) C16 0.0510(17) 0.0253(12) 0.0519(15) -0.0042(10) -0.0066(14) 0.0003(11) C17 0.0575(18) 0.0283(13) 0.0524(15) -0.0083(11) -0.0059(15) 0.0072(12) C18 0.0434(16) 0.0404(14) 0.0428(13) -0.0096(11) -0.0035(12) 0.0093(12) C19 0.0377(14) 0.0331(13) 0.0384(12) -0.0031(9) -0.0023(11) 0.0021(11) C20 0.0285(12) 0.0275(11) 0.0329(11) -0.0007(9) -0.0063(10) 0.0017(9) C21 0.0265(12) 0.0396(13) 0.0307(11) -0.0015(9) -0.0006(10) -0.0016(10) O21 0.0328(10) 0.0399(10) 0.0562(11) 0.0058(8) -0.0167(9) -0.0052(8) C22 0.0268(12) 0.0366(12) 0.0359(11) -0.0012(9) -0.0006(10) -0.0014(10) C23 0.0320(13) 0.0406(14) 0.0464(13) -0.0035(11) -0.0040(12) -0.0076(11) C24 0.0281(13) 0.0461(14) 0.0414(13) -0.0041(11) -0.0054(11) -0.0026(11) C25 0.0268(12) 0.0449(14) 0.0335(11) -0.0013(10) 0.0024(10) 0.0029(11) C26 0.0305(14) 0.0544(17) 0.0412(13) 0.0000(11) -0.0016(11) 0.0095(12) C27 0.0409(15) 0.0517(16) 0.0433(14) 0.0007(12) -0.0009(12) 0.0179(13) C28 0.0416(15) 0.0412(13) 0.0337(12) 0.0013(10) 0.0078(11) 0.0081(12) C29 0.0605(19) 0.0414(14) 0.0430(14) 0.0030(11) 0.0149(14) 0.0100(14) C30 0.071(2) 0.0365(14) 0.0507(15) -0.0042(12) 0.0178(16) -0.0005(15) C31 0.0595(19) 0.0488(16) 0.0500(15) -0.0101(12) 0.0019(15) -0.0086(15) C32 0.0442(15) 0.0418(14) 0.0414(13) -0.0034(10) 0.0008(12) -0.0026(12) C33 0.0339(14) 0.0366(13) 0.0332(11) -0.0016(9) 0.0064(11) 0.0008(11) C34 0.0262(12) 0.0359(12) 0.0314(11) -0.0022(9) 0.0031(10) 0.0019(10) C35 0.0302(13) 0.0331(12) 0.0393(12) -0.0023(10) 0.0002(11) -0.0001(10) C41 0.0267(12) 0.0329(12) 0.0333(11) -0.0047(9) -0.0028(10) 0.0012(10) O41 0.0380(10) 0.0295(8) 0.0462(9) -0.0053(7) 0.0117(8) -0.0003(7) C42 0.0312(13) 0.0344(12) 0.0341(11) -0.0046(9) 0.0013(11) 0.0017(10) C43 0.0376(14) 0.0451(15) 0.0373(13) -0.0043(10) 0.0064(12) -0.0001(11) C44 0.0401(15) 0.0499(15) 0.0391(13) -0.0080(11) 0.0050(12) 0.0061(13) C45 0.0381(15) 0.0408(14) 0.0390(12) -0.0112(10) -0.0067(12) 0.0064(12) C46 0.0486(17) 0.0445(15) 0.0534(15) -0.0149(13) -0.0031(14) 0.0153(13) C47 0.0532(18) 0.0370(14) 0.0646(17) -0.0122(13) -0.0093(15) 0.0138(13) C48 0.0436(16) 0.0343(13) 0.0584(15) -0.0064(11) -0.0173(14) 0.0051(12) C49 0.0498(18) 0.0287(13) 0.089(2) 0.0038(13) -0.0134(18) 0.0015(12) C50 0.0492(18) 0.0366(15) 0.097(2) 0.0133(15) -0.0067(19) -0.0052(14) C51 0.0445(16) 0.0421(15) 0.0712(19) 0.0103(13) -0.0015(16) -0.0030(13) C52 0.0388(15) 0.0304(12) 0.0571(15) 0.0018(11) -0.0038(13) -0.0006(11) C53 0.0305(13) 0.0292(12) 0.0462(13) -0.0034(9) -0.0104(11) 0.0003(10) C54 0.0315(13) 0.0329(12) 0.0341(11) -0.0055(9) -0.0074(10) 0.0054(10) C55 0.0296(12) 0.0354(12) 0.0358(11) 0.0017(9) 0.0003(10) -0.0019(10) _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 C01 C02 1.384(3) . ? C01 C10 1.423(3) . ? C01 C11 1.488(3) . ? C02 C03 1.407(3) . ? C02 N02 1.411(3) . ? N02 C35 1.285(3) . ? C03 C04 1.346(3) . ? C03 H03 0.9400 . ? C04 C05 1.403(4) . ? C04 H04 0.9400 . ? C05 C06 1.411(3) . ? C05 C10 1.418(3) . ? C06 C07 1.353(4) . ? C06 H06 0.9400 . ? C07 C08 1.397(4) . ? C07 H07 0.9400 . ? C08 C09 1.361(3) . ? C08 H08 0.9400 . ? C09 C10 1.414(3) . ? C09 H09 0.9400 . ? C11 C12 1.375(3) . ? C11 C20 1.426(3) . ? C12 N12 1.408(3) . ? C12 C13 1.419(3) . ? N12 C55 1.293(3) . ? C13 C14 1.354(3) . ? C13 H13 0.9400 . ? C14 C15 1.407(4) . ? C14 H14 0.9400 . ? C15 C20 1.410(3) . ? C15 C16 1.414(3) . ? C16 C17 1.350(4) . ? C16 H16 0.9400 . ? C17 C18 1.393(4) . ? C17 H17 0.9400 . ? C18 C19 1.367(3) . ? C18 H18 0.9400 . ? C19 C20 1.412(3) . ? C19 H19 0.9400 . ? C21 O21 1.325(3) . ? C21 C22 1.409(3) . ? C21 C34 1.424(3) . ? O21 H21 0.99(3) . ? C22 C23 1.404(3) . ? C22 C35 1.429(3) . ? C23 C24 1.349(4) . ? C23 H23 0.9400 . ? C24 C25 1.415(4) . ? C24 H24 0.9400 . ? C25 C34 1.409(3) . ? C25 C26 1.424(3) . ? C26 C27 1.343(4) . ? C26 H26 0.9400 . ? C27 C28 1.417(4) . ? C27 H27 0.9400 . ? C28 C29 1.398(4) . ? C28 C33 1.422(3) . ? C29 C30 1.345(4) . ? C29 H29 0.9400 . ? C30 C31 1.386(4) . ? C30 H30 0.9400 . ? C31 C32 1.369(4) . ? C31 H31 0.9400 . ? C32 C33 1.412(4) . ? C32 H32 0.9400 . ? C33 C34 1.456(3) . ? C35 H35 0.9400 . ? C41 O41 1.318(3) . ? C41 C42 1.408(3) . ? C41 C54 1.434(3) . ? O41 H41 1.03(3) . ? C42 C43 1.412(3) . ? C42 C55 1.429(3) . ? C43 C44 1.355(4) . ? C43 H43 0.9400 . ? C44 C45 1.403(4) . ? C44 H44 0.9400 . ? C45 C54 1.405(3) . ? C45 C46 1.435(4) . ? C46 C47 1.338(4) . ? C46 H46 0.9400 . ? C47 C48 1.419(4) . ? C47 H47 0.9400 . ? C48 C49 1.405(4) . ? C48 C53 1.418(3) . ? C49 C50 1.361(5) . ? C49 H49 0.9400 . ? C50 C51 1.393(4) . ? C50 H50 0.9400 . ? C51 C52 1.367(4) . ? C51 H51 0.9400 . ? C52 C53 1.406(4) . ? C52 H52 0.9400 . ? C53 C54 1.458(3) . ? C55 H55 0.9400 . ? 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 C02 C01 C10 119.2(2) . . ? C02 C01 C11 120.4(2) . . ? C10 C01 C11 120.4(2) . . ? C01 C02 C03 120.1(2) . . ? C01 C02 N02 117.5(2) . . ? C03 C02 N02 122.3(2) . . ? C35 N02 C02 122.4(2) . . ? C04 C03 C02 120.9(2) . . ? C04 C03 H03 119.5 . . ? C02 C03 H03 119.5 . . ? C03 C04 C05 121.4(2) . . ? C03 C04 H04 119.3 . . ? C05 C04 H04 119.3 . . ? C04 C05 C06 122.5(2) . . ? C04 C05 C10 118.6(2) . . ? C06 C05 C10 119.0(2) . . ? C07 C06 C05 121.0(2) . . ? C07 C06 H06 119.5 . . ? C05 C06 H06 119.5 . . ? C06 C07 C08 120.3(2) . . ? C06 C07 H07 119.9 . . ? C08 C07 H07 119.9 . . ? C09 C08 C07 120.6(3) . . ? C09 C08 H08 119.7 . . ? C07 C08 H08 119.7 . . ? C08 C09 C10 120.7(2) . . ? C08 C09 H09 119.6 . . ? C10 C09 H09 119.6 . . ? C09 C10 C05 118.4(2) . . ? C09 C10 C01 122.0(2) . . ? C05 C10 C01 119.7(2) . . ? C12 C11 C20 119.3(2) . . ? C12 C11 C01 119.49(19) . . ? C20 C11 C01 121.2(2) . . ? C11 C12 N12 116.5(2) . . ? C11 C12 C13 120.7(2) . . ? N12 C12 C13 122.8(2) . . ? C55 N12 C12 125.4(2) . . ? C14 C13 C12 119.9(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.4(2) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C14 C15 C20 119.0(2) . . ? C14 C15 C16 121.8(2) . . ? C20 C15 C16 119.2(2) . . ? C17 C16 C15 120.8(2) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 118.6(2) . . ? C15 C20 C11 119.6(2) . . ? C19 C20 C11 121.8(2) . . ? O21 C21 C22 119.2(2) . . ? O21 C21 C34 120.0(2) . . ? C22 C21 C34 120.8(2) . . ? C21 O21 H21 107.3(15) . . ? C23 C22 C21 119.3(2) . . ? C23 C22 C35 119.5(2) . . ? C21 C22 C35 121.3(2) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C34 C25 C24 121.1(2) . . ? C34 C25 C26 120.3(2) . . ? C24 C25 C26 118.6(2) . . ? C27 C26 C25 121.0(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 121.3(2) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 120.3(3) . . ? C29 C28 C33 119.8(3) . . ? C27 C28 C33 120.0(2) . . ? C30 C29 C28 121.5(3) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 119.8(3) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 120.9(3) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 121.1(3) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 116.9(2) . . ? C32 C33 C34 124.5(2) . . ? C28 C33 C34 118.6(2) . . ? C25 C34 C21 117.2(2) . . ? C25 C34 C33 118.7(2) . . ? C21 C34 C33 124.1(2) . . ? N02 C35 C22 122.3(2) . . ? N02 C35 H35 118.9 . . ? C22 C35 H35 118.9 . . ? O41 C41 C42 119.29(19) . . ? O41 C41 C54 119.9(2) . . ? C42 C41 C54 120.8(2) . . ? C41 O41 H41 106.7(15) . . ? C41 C42 C43 119.4(2) . . ? C41 C42 C55 120.8(2) . . ? C43 C42 C55 119.8(2) . . ? C44 C43 C42 120.5(2) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 120.8(2) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C54 121.7(2) . . ? C44 C45 C46 119.1(2) . . ? C54 C45 C46 119.2(3) . . ? C47 C46 C45 121.3(3) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C48 121.5(2) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C49 C48 C53 119.9(3) . . ? C49 C48 C47 120.1(3) . . ? C53 C48 C47 120.0(3) . . ? C50 C49 C48 121.6(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C51 118.9(3) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C52 C51 C50 121.0(3) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 121.8(2) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C48 116.9(2) . . ? C52 C53 C54 124.9(2) . . ? C48 C53 C54 118.2(2) . . ? C45 C54 C41 116.8(2) . . ? C45 C54 C53 119.7(2) . . ? C41 C54 C53 123.4(2) . . ? N12 C55 C42 121.4(2) . . ? N12 C55 H55 119.3 . . ? C42 C55 H55 119.3 . . ? 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 C10 C01 C02 C03 -3.9(3) . . . . ? C11 C01 C02 C03 174.54(19) . . . . ? C10 C01 C02 N02 173.57(18) . . . . ? C11 C01 C02 N02 -7.9(3) . . . . ? C01 C02 N02 C35 166.1(2) . . . . ? C03 C02 N02 C35 -16.4(3) . . . . ? C01 C02 C03 C04 2.2(3) . . . . ? N02 C02 C03 C04 -175.2(2) . . . . ? C02 C03 C04 C05 2.1(4) . . . . ? C03 C04 C05 C06 174.2(2) . . . . ? C03 C04 C05 C10 -4.4(3) . . . . ? C04 C05 C06 C07 -179.7(2) . . . . ? C10 C05 C06 C07 -1.2(3) . . . . ? C05 C06 C07 C08 -2.0(4) . . . . ? C06 C07 C08 C09 2.7(4) . . . . ? C07 C08 C09 C10 -0.2(4) . . . . ? C08 C09 C10 C05 -3.0(3) . . . . ? C08 C09 C10 C01 176.7(2) . . . . ? C04 C05 C10 C09 -177.8(2) . . . . ? C06 C05 C10 C09 3.6(3) . . . . ? C04 C05 C10 C01 2.5(3) . . . . ? C06 C05 C10 C01 -176.1(2) . . . . ? C02 C01 C10 C09 -178.1(2) . . . . ? C11 C01 C10 C09 3.4(3) . . . . ? C02 C01 C10 C05 1.6(3) . . . . ? C11 C01 C10 C05 -176.92(19) . . . . ? C02 C01 C11 C12 -103.1(3) . . . . ? C10 C01 C11 C12 75.3(3) . . . . ? C02 C01 C11 C20 76.3(3) . . . . ? C10 C01 C11 C20 -105.2(2) . . . . ? C20 C11 C12 N12 179.5(2) . . . . ? C01 C11 C12 N12 -1.0(3) . . . . ? C20 C11 C12 C13 0.4(3) . . . . ? C01 C11 C12 C13 179.9(2) . . . . ? C11 C12 N12 C55 178.7(2) . . . . ? C13 C12 N12 C55 -2.2(4) . . . . ? C11 C12 C13 C14 -2.5(4) . . . . ? N12 C12 C13 C14 178.5(2) . . . . ? C12 C13 C14 C15 1.6(4) . . . . ? C13 C14 C15 C20 1.3(4) . . . . ? C13 C14 C15 C16 -178.8(3) . . . . ? C14 C15 C16 C17 -179.3(2) . . . . ? C20 C15 C16 C17 0.6(4) . . . . ? C15 C16 C17 C18 1.7(4) . . . . ? C16 C17 C18 C19 -2.2(4) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C14 C15 C20 C19 177.6(2) . . . . ? C16 C15 C20 C19 -2.3(3) . . . . ? C14 C15 C20 C11 -3.4(3) . . . . ? C16 C15 C20 C11 176.7(2) . . . . ? C18 C19 C20 C15 1.8(4) . . . . ? C18 C19 C20 C11 -177.2(2) . . . . ? C12 C11 C20 C15 2.5(3) . . . . ? C01 C11 C20 C15 -176.9(2) . . . . ? C12 C11 C20 C19 -178.4(2) . . . . ? C01 C11 C20 C19 2.1(3) . . . . ? O21 C21 C22 C23 -176.7(2) . . . . ? C34 C21 C22 C23 2.3(3) . . . . ? O21 C21 C22 C35 2.9(3) . . . . ? C34 C21 C22 C35 -178.1(2) . . . . ? C21 C22 C23 C24 0.9(4) . . . . ? C35 C22 C23 C24 -178.6(2) . . . . ? C22 C23 C24 C25 -2.5(4) . . . . ? C23 C24 C25 C34 0.8(4) . . . . ? C23 C24 C25 C26 -179.8(2) . . . . ? C34 C25 C26 C27 0.5(4) . . . . ? C24 C25 C26 C27 -178.9(3) . . . . ? C25 C26 C27 C28 -2.9(4) . . . . ? C26 C27 C28 C29 -176.8(3) . . . . ? C26 C27 C28 C33 1.8(4) . . . . ? C27 C28 C29 C30 176.9(2) . . . . ? C33 C28 C29 C30 -1.7(4) . . . . ? C28 C29 C30 C31 -0.3(4) . . . . ? C29 C30 C31 C32 1.6(4) . . . . ? C30 C31 C32 C33 -0.8(4) . . . . ? C31 C32 C33 C28 -1.2(4) . . . . ? C31 C32 C33 C34 -178.9(3) . . . . ? C29 C28 C33 C32 2.4(3) . . . . ? C27 C28 C33 C32 -176.2(2) . . . . ? C29 C28 C33 C34 -179.7(2) . . . . ? C27 C28 C33 C34 1.7(3) . . . . ? C24 C25 C34 C21 2.4(3) . . . . ? C26 C25 C34 C21 -177.1(2) . . . . ? C24 C25 C34 C33 -177.7(2) . . . . ? C26 C25 C34 C33 2.9(3) . . . . ? O21 C21 C34 C25 175.1(2) . . . . ? C22 C21 C34 C25 -3.9(3) . . . . ? O21 C21 C34 C33 -4.9(3) . . . . ? C22 C21 C34 C33 176.2(2) . . . . ? C32 C33 C34 C25 173.8(2) . . . . ? C28 C33 C34 C25 -3.9(3) . . . . ? C32 C33 C34 C21 -6.2(4) . . . . ? C28 C33 C34 C21 176.1(2) . . . . ? C02 N02 C35 C22 173.8(2) . . . . ? C23 C22 C35 N02 175.5(2) . . . . ? C21 C22 C35 N02 -4.0(4) . . . . ? O41 C41 C42 C43 -179.9(2) . . . . ? C54 C41 C42 C43 1.5(3) . . . . ? O41 C41 C42 C55 3.0(3) . . . . ? C54 C41 C42 C55 -175.6(2) . . . . ? C41 C42 C43 C44 -2.4(4) . . . . ? C55 C42 C43 C44 174.7(2) . . . . ? C42 C43 C44 C45 0.6(4) . . . . ? C43 C44 C45 C54 2.2(4) . . . . ? C43 C44 C45 C46 -176.9(3) . . . . ? C44 C45 C46 C47 -179.6(3) . . . . ? C54 C45 C46 C47 1.3(4) . . . . ? C45 C46 C47 C48 0.4(4) . . . . ? C46 C47 C48 C49 179.6(3) . . . . ? C46 C47 C48 C53 -1.2(4) . . . . ? C53 C48 C49 C50 -0.5(4) . . . . ? C47 C48 C49 C50 178.7(3) . . . . ? C48 C49 C50 C51 0.8(5) . . . . ? C49 C50 C51 C52 -0.1(5) . . . . ? C50 C51 C52 C53 -0.8(4) . . . . ? C51 C52 C53 C48 1.1(4) . . . . ? C51 C52 C53 C54 -178.9(3) . . . . ? C49 C48 C53 C52 -0.5(4) . . . . ? C47 C48 C53 C52 -179.7(2) . . . . ? C49 C48 C53 C54 179.5(2) . . . . ? C47 C48 C53 C54 0.3(4) . . . . ? C44 C45 C54 C41 -3.0(3) . . . . ? C46 C45 C54 C41 176.1(2) . . . . ? C44 C45 C54 C53 178.8(2) . . . . ? C46 C45 C54 C53 -2.1(3) . . . . ? O41 C41 C54 C45 -177.5(2) . . . . ? C42 C41 C54 C45 1.1(3) . . . . ? O41 C41 C54 C53 0.7(3) . . . . ? C42 C41 C54 C53 179.2(2) . . . . ? C52 C53 C54 C45 -178.7(2) . . . . ? C48 C53 C54 C45 1.3(3) . . . . ? C52 C53 C54 C41 3.2(4) . . . . ? C48 C53 C54 C41 -176.7(2) . . . . ? C12 N12 C55 C42 175.5(2) . . . . ? C41 C42 C55 N12 0.2(4) . . . . ? C43 C42 C55 N12 -176.9(2) . . . . ? 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 O21 H21 N02 0.99(3) 1.62(3) 2.536(2) 151(2) . O41 H41 N12 1.03(3) 1.54(3) 2.501(2) 152(2) . _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.357 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.089 data_Compound_(R)-8 _database_code_depnum_ccdc_archive 'CCDC 276258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-bis(2-(1-oxy-2-phenanthrenyl)-1-azaethenyl)(1,1'-binaphthyl)zinc(II) ; _chemical_name_common ;2,2'-bis(2-(1-oxy-2-phenanthrenyl)-1-azaethenyl)(1,1'- binaphthyl)zinc(ii) ; _chemical_melting_point ? _chemical_formula_moiety ; (C50 H30 N2 O2 Zn1) (C1 H4 O1) (C1 H3 O1)0.75 (C1 H2 Cl2)0.25 ; _chemical_formula_sum 'C52 H36.75 Cl0.50 N2 O3.75 Zn' _chemical_formula_weight 832.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.3373(4) _cell_length_b 13.3410(5) _cell_length_c 23.6254(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3888.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 3931 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.85 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1725 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41396 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9192 _reflns_number_gt 7464 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.782 _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(8) _refine_ls_number_reflns 9192 _refine_ls_number_parameters 555 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1S O 0.6813(3) 0.3111(2) 0.23128(14) 0.0581(8) Uani 0.75 1 d P A 1 C1S C 0.7590(4) 0.3602(4) 0.2643(2) 0.0699(13) Uani 0.75 1 d P A 1 H1SA H 0.8174 0.3141 0.2733 0.105 Uiso 0.75 1 calc PR A 1 H1SB H 0.7258 0.3836 0.2991 0.105 Uiso 0.75 1 calc PR A 1 H1SC H 0.7878 0.4169 0.2435 0.105 Uiso 0.75 1 calc PR A 1 C2S C 0.8198(15) 0.3574(10) 0.2827(6) 0.101(6) Uiso 0.25 1 d PD B 2 H2SA H 0.7816 0.3803 0.3167 0.122 Uiso 0.25 1 calc PR B 2 H2SB H 0.8849 0.3212 0.2949 0.122 Uiso 0.25 1 calc PR B 2 Cl1 Cl 0.8584(3) 0.4620(2) 0.24218(17) 0.0700(9) Uani 0.25 1 d PD B 2 Cl2 Cl 0.7347(3) 0.2747(3) 0.2443(2) 0.0723(11) Uani 0.25 1 d PD B 2 Zn1 Zn 0.382165(18) 0.500474(19) 0.205060(10) 0.02742(7) Uani 1 1 d . . . C01 C 0.43547(18) 0.64168(15) 0.07839(9) 0.0243(4) Uani 1 1 d . . . C02 C 0.33417(18) 0.62842(15) 0.10213(9) 0.0263(5) Uani 1 1 d . . . N02 N 0.30324(14) 0.53868(13) 0.13077(8) 0.0259(4) Uani 1 1 d . . . C03 C 0.2580(2) 0.70749(18) 0.10212(11) 0.0346(5) Uani 1 1 d . . . H03 H 0.1886 0.6966 0.1173 0.042 Uiso 1 1 calc R . . C04 C 0.2832(2) 0.79884(17) 0.08062(11) 0.0368(6) Uani 1 1 d . . . H04 H 0.2302 0.8495 0.0796 0.044 Uiso 1 1 calc R . . C05 C 0.3878(2) 0.81835(15) 0.05988(9) 0.0303(5) Uani 1 1 d . . . C06 C 0.4189(2) 0.91538(17) 0.04195(11) 0.0399(6) Uani 1 1 d . . . H06 H 0.3679 0.9678 0.0428 0.048 Uiso 1 1 calc R . . C07 C 0.5212(2) 0.93389(17) 0.02350(11) 0.0393(6) Uani 1 1 d . . . H07 H 0.5407 0.9987 0.0116 0.047 Uiso 1 1 calc R . . C08 C 0.5976(2) 0.85664(17) 0.02218(10) 0.0377(6) Uani 1 1 d . . . H08 H 0.6684 0.8697 0.0095 0.045 Uiso 1 1 calc R . . C09 C 0.5699(2) 0.76233(17) 0.03916(10) 0.0314(5) Uani 1 1 d . . . H09 H 0.6222 0.7112 0.0377 0.038 Uiso 1 1 calc R . . C10 C 0.46505(19) 0.73969(15) 0.05877(9) 0.0262(5) Uani 1 1 d . . . C11 C 0.51591(17) 0.55911(14) 0.07200(9) 0.0236(4) Uani 1 1 d . . . C12 C 0.56638(17) 0.51791(15) 0.11849(9) 0.0269(5) Uani 1 1 d . . . N12 N 0.53161(15) 0.54806(14) 0.17368(7) 0.0268(4) Uani 1 1 d . . . C13 C 0.65080(19) 0.44868(16) 0.11307(10) 0.0328(5) Uani 1 1 d . . . H13 H 0.6836 0.4217 0.1456 0.039 Uiso 1 1 calc R . . C14 C 0.6856(2) 0.42022(16) 0.06066(10) 0.0340(5) Uani 1 1 d . . . H14 H 0.7436 0.3749 0.0574 0.041 Uiso 1 1 calc R . . C15 C 0.63608(18) 0.45771(16) 0.01168(10) 0.0299(5) Uani 1 1 d . . . C16 C 0.6691(2) 0.42777(17) -0.04305(11) 0.0356(5) Uani 1 1 d . . . H16 H 0.7248 0.3801 -0.0467 0.043 Uiso 1 1 calc R . . C17 C 0.6230(2) 0.46560(18) -0.09040(10) 0.0379(6) Uani 1 1 d . . . H17 H 0.6461 0.4441 -0.1263 0.046 Uiso 1 1 calc R . . C18 C 0.54074(19) 0.53697(18) -0.08535(10) 0.0341(5) Uani 1 1 d . . . H18 H 0.5097 0.5648 -0.1181 0.041 Uiso 1 1 calc R . . C19 C 0.50492(18) 0.56674(17) -0.03326(9) 0.0294(5) Uani 1 1 d . . . H19 H 0.4486 0.6140 -0.0309 0.035 Uiso 1 1 calc R . . C20 C 0.55027(17) 0.52838(15) 0.01680(9) 0.0264(5) Uani 1 1 d . . . C21 C 0.17109(17) 0.39146(15) 0.20015(10) 0.0267(4) Uani 1 1 d . . . O21 O 0.24943(13) 0.42827(12) 0.22907(7) 0.0337(4) Uani 1 1 d . . . C22 C 0.15110(18) 0.42184(16) 0.14362(9) 0.0270(5) Uani 1 1 d . . . C23 C 0.06408(19) 0.38004(18) 0.11241(10) 0.0348(5) Uani 1 1 d . . . H23 H 0.0480 0.4054 0.0762 0.042 Uiso 1 1 calc R . . C24 C 0.0039(2) 0.3046(2) 0.13364(11) 0.0433(6) Uani 1 1 d . . . H24 H -0.0511 0.2756 0.1115 0.052 Uiso 1 1 calc R . . C25 C 0.0230(2) 0.2691(2) 0.18889(11) 0.0400(6) Uani 1 1 d . . . C26 C -0.0365(3) 0.1852(2) 0.20890(13) 0.0580(8) Uani 1 1 d . . . H26 H -0.0873 0.1549 0.1847 0.070 Uiso 1 1 calc R . . C27 C -0.0230(3) 0.1477(2) 0.26073(13) 0.0581(8) Uani 1 1 d . . . H27 H -0.0618 0.0904 0.2719 0.070 Uiso 1 1 calc R . . C28 C 0.0503(2) 0.19436(18) 0.29943(11) 0.0415(6) Uani 1 1 d . . . C29 C 0.0626(3) 0.1558(2) 0.35473(12) 0.0519(7) Uani 1 1 d . . . H29 H 0.0251 0.0973 0.3651 0.062 Uiso 1 1 calc R . . C30 C 0.1273(3) 0.2016(2) 0.39304(12) 0.0492(7) Uani 1 1 d . . . H30 H 0.1355 0.1747 0.4296 0.059 Uiso 1 1 calc R . . C31 C 0.1822(2) 0.2893(2) 0.37763(11) 0.0429(6) Uani 1 1 d . . . H31 H 0.2254 0.3225 0.4045 0.052 Uiso 1 1 calc R . . C32 C 0.1736(2) 0.32742(18) 0.32390(10) 0.0347(5) Uani 1 1 d . . . H32 H 0.2112 0.3864 0.3145 0.042 Uiso 1 1 calc R . . C33 C 0.10958(19) 0.27989(16) 0.28256(9) 0.0310(5) Uani 1 1 d . . . C34 C 0.09991(18) 0.31533(16) 0.22454(9) 0.0282(5) Uani 1 1 d . . . C35 C 0.21155(16) 0.49881(19) 0.11552(8) 0.0272(4) Uani 1 1 d . . . H35 H 0.1812 0.5236 0.0818 0.033 Uiso 1 1 calc R . . C41 C 0.48598(17) 0.62173(15) 0.29194(10) 0.0269(5) Uani 1 1 d . . . O41 O 0.39644(13) 0.59740(13) 0.26669(7) 0.0371(4) Uani 1 1 d . . . C42 C 0.58697(18) 0.62158(16) 0.26354(9) 0.0290(5) Uani 1 1 d . . . C43 C 0.68035(18) 0.66008(17) 0.29055(10) 0.0328(5) Uani 1 1 d . . . H43 H 0.7471 0.6588 0.2714 0.039 Uiso 1 1 calc R . . C44 C 0.67560(19) 0.69873(17) 0.34349(10) 0.0323(5) Uani 1 1 d . . . H44 H 0.7377 0.7276 0.3598 0.039 Uiso 1 1 calc R . . C45 C 0.57779(18) 0.69570(16) 0.37402(10) 0.0276(5) Uani 1 1 d . . . C46 C 0.5748(2) 0.73580(17) 0.43016(10) 0.0324(5) Uani 1 1 d . . . H46 H 0.6367 0.7678 0.4446 0.039 Uiso 1 1 calc R . . C47 C 0.48656(19) 0.72901(17) 0.46257(10) 0.0321(5) Uani 1 1 d . . . H47 H 0.4867 0.7576 0.4989 0.039 Uiso 1 1 calc R . . C48 C 0.39236(19) 0.67889(15) 0.44266(9) 0.0275(5) Uani 1 1 d . . . C49 C 0.30386(19) 0.66339(17) 0.47937(10) 0.0336(5) Uani 1 1 d . . . H49 H 0.3062 0.6903 0.5161 0.040 Uiso 1 1 calc R . . C50 C 0.2151(2) 0.61037(18) 0.46290(11) 0.0365(6) Uani 1 1 d . . . H50 H 0.1571 0.6000 0.4880 0.044 Uiso 1 1 calc R . . C51 C 0.2118(2) 0.5718(2) 0.40812(11) 0.0386(6) Uani 1 1 d . . . H51 H 0.1512 0.5345 0.3965 0.046 Uiso 1 1 calc R . . C52 C 0.29543(19) 0.58711(18) 0.37084(10) 0.0336(5) Uani 1 1 d . . . H52 H 0.2903 0.5610 0.3340 0.040 Uiso 1 1 calc R . . C53 C 0.38878(18) 0.64116(14) 0.38662(9) 0.0250(4) Uani 1 1 d . . . C54 C 0.48326(18) 0.65274(15) 0.35073(9) 0.0254(4) Uani 1 1 d . . . C55 C 0.60222(17) 0.58864(15) 0.20638(10) 0.0279(4) Uani 1 1 d . . . H55 H 0.6718 0.5978 0.1911 0.033 Uiso 1 1 calc R . . C61 C 0.4656(3) 0.3557(2) 0.30133(15) 0.0613(9) Uani 1 1 d . . . H61A H 0.5073 0.2955 0.3089 0.092 Uiso 1 1 calc R . . H61B H 0.3906 0.3446 0.3119 0.092 Uiso 1 1 calc R . . H61C H 0.4948 0.4109 0.3232 0.092 Uiso 1 1 calc R . . O61 O 0.47166(16) 0.37895(14) 0.24275(8) 0.0502(5) Uani 1 1 d . . . H61 H 0.5501 0.3720 0.2352 0.060 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1S 0.0489(19) 0.0587(18) 0.067(2) 0.0064(16) 0.0001(16) 0.0054(15) C1S 0.067(3) 0.080(3) 0.062(3) 0.018(3) -0.003(3) 0.009(3) Cl1 0.064(2) 0.0536(16) 0.092(3) 0.0055(17) 0.0051(18) 0.0029(15) Cl2 0.055(2) 0.061(2) 0.101(3) -0.012(2) -0.024(2) 0.0026(17) Zn1 0.02680(12) 0.03555(12) 0.01992(11) -0.00043(13) -0.00162(10) -0.00753(12) C01 0.0277(11) 0.0278(10) 0.0175(10) -0.0019(8) -0.0007(9) 0.0008(9) C02 0.0292(11) 0.0276(10) 0.0220(11) 0.0006(9) -0.0006(9) -0.0011(9) N02 0.0259(9) 0.0300(8) 0.0217(9) 0.0010(7) 0.0029(8) -0.0022(7) C03 0.0276(12) 0.0402(13) 0.0362(14) -0.0008(11) 0.0020(10) 0.0019(10) C04 0.0354(13) 0.0317(11) 0.0432(15) -0.0012(11) -0.0026(11) 0.0081(10) C05 0.0379(12) 0.0269(10) 0.0261(11) -0.0009(9) -0.0004(11) 0.0023(10) C06 0.0550(17) 0.0274(11) 0.0373(14) 0.0018(10) -0.0019(13) -0.0005(11) C07 0.0575(17) 0.0271(11) 0.0331(14) 0.0036(10) -0.0014(12) -0.0097(11) C08 0.0418(15) 0.0416(12) 0.0297(13) 0.0046(10) 0.0023(11) -0.0139(11) C09 0.0341(13) 0.0345(11) 0.0257(12) 0.0016(10) -0.0017(11) -0.0028(10) C10 0.0326(12) 0.0276(10) 0.0182(11) 0.0010(8) -0.0008(9) -0.0029(9) C11 0.0249(11) 0.0241(10) 0.0219(11) -0.0017(8) 0.0009(9) -0.0030(8) C12 0.0296(11) 0.0297(12) 0.0214(10) -0.0007(9) 0.0006(9) -0.0018(9) N12 0.0282(10) 0.0327(9) 0.0193(9) 0.0028(8) 0.0001(8) -0.0014(8) C13 0.0359(13) 0.0322(11) 0.0304(12) 0.0030(10) -0.0067(10) 0.0052(10) C14 0.0352(13) 0.0278(10) 0.0390(14) -0.0033(10) 0.0018(11) 0.0061(10) C15 0.0322(13) 0.0279(9) 0.0296(12) -0.0036(9) 0.0016(10) -0.0023(9) C16 0.0348(13) 0.0331(11) 0.0389(14) -0.0072(10) 0.0081(12) -0.0009(10) C17 0.0406(14) 0.0452(12) 0.0280(12) -0.0133(10) 0.0088(11) -0.0104(11) C18 0.0312(13) 0.0466(12) 0.0247(12) -0.0016(10) -0.0007(10) -0.0100(10) C19 0.0258(11) 0.0369(11) 0.0256(12) -0.0010(9) -0.0016(10) -0.0049(9) C20 0.0257(11) 0.0294(11) 0.0240(11) -0.0017(8) 0.0015(9) -0.0049(8) C21 0.0233(10) 0.0318(10) 0.0249(11) -0.0040(9) 0.0029(10) -0.0028(8) O21 0.0314(9) 0.0465(9) 0.0232(8) 0.0018(7) -0.0024(7) -0.0152(7) C22 0.0257(11) 0.0302(10) 0.0252(12) -0.0036(9) 0.0010(9) -0.0022(9) C23 0.0334(13) 0.0456(13) 0.0253(12) -0.0019(11) -0.0039(10) -0.0097(11) C24 0.0434(15) 0.0562(15) 0.0304(13) -0.0055(12) -0.0058(12) -0.0221(13) C25 0.0420(14) 0.0448(13) 0.0333(14) -0.0037(11) 0.0039(11) -0.0153(12) C26 0.0625(19) 0.0679(18) 0.0436(17) -0.0029(16) 0.0004(16) -0.0404(16) C27 0.072(2) 0.0559(17) 0.0465(18) 0.0058(15) 0.0053(16) -0.0349(16) C28 0.0486(15) 0.0420(13) 0.0338(14) 0.0040(12) 0.0100(13) -0.0122(11) C29 0.0627(19) 0.0498(15) 0.0433(16) 0.0089(13) 0.0127(15) -0.0148(14) C30 0.0571(18) 0.0576(16) 0.0331(14) 0.0151(13) 0.0060(14) 0.0005(14) C31 0.0456(15) 0.0565(15) 0.0268(13) 0.0048(12) -0.0018(12) -0.0036(12) C32 0.0335(13) 0.0421(13) 0.0286(13) 0.0035(10) 0.0037(11) -0.0029(11) C33 0.0291(11) 0.0343(10) 0.0297(12) 0.0001(9) 0.0065(10) 0.0009(10) C34 0.0272(12) 0.0321(10) 0.0254(11) -0.0017(9) 0.0039(9) -0.0047(9) C35 0.0283(10) 0.0333(9) 0.0201(9) 0.0010(11) 0.0012(8) 0.0013(11) C41 0.0274(11) 0.0283(10) 0.0249(11) 0.0000(10) -0.0051(10) -0.0038(8) O41 0.0258(8) 0.0589(10) 0.0265(8) -0.0135(8) -0.0005(7) -0.0089(8) C42 0.0312(12) 0.0326(10) 0.0233(11) 0.0028(9) -0.0022(9) -0.0059(9) C43 0.0253(11) 0.0416(11) 0.0316(13) 0.0018(11) 0.0012(11) -0.0080(9) C44 0.0271(12) 0.0396(12) 0.0301(13) -0.0029(10) -0.0062(10) -0.0093(10) C45 0.0279(11) 0.0294(10) 0.0256(11) 0.0009(9) -0.0050(9) -0.0013(9) C46 0.0300(12) 0.0346(11) 0.0325(13) -0.0083(10) -0.0083(11) -0.0032(10) C47 0.0343(13) 0.0356(12) 0.0264(12) -0.0085(10) -0.0051(11) 0.0020(10) C48 0.0300(12) 0.0259(9) 0.0266(11) -0.0041(8) 0.0003(10) 0.0042(9) C49 0.0364(13) 0.0364(11) 0.0279(12) -0.0054(10) 0.0041(10) 0.0053(10) C50 0.0324(12) 0.0441(13) 0.0330(14) -0.0013(11) 0.0113(11) 0.0001(10) C51 0.0310(13) 0.0483(14) 0.0364(14) -0.0041(12) 0.0047(11) -0.0095(11) C52 0.0311(12) 0.0430(12) 0.0266(12) -0.0032(10) 0.0012(10) -0.0068(10) C53 0.0275(11) 0.0259(9) 0.0218(10) 0.0005(8) -0.0035(9) 0.0014(9) C54 0.0265(11) 0.0272(10) 0.0226(11) 0.0000(9) -0.0031(9) -0.0022(8) C55 0.0267(11) 0.0324(10) 0.0246(11) 0.0024(9) 0.0023(10) -0.0035(9) C61 0.065(2) 0.0613(18) 0.058(2) 0.0174(17) -0.0077(18) 0.0088(16) O61 0.0441(11) 0.0549(11) 0.0515(12) 0.0214(10) 0.0060(10) 0.0034(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 O1S C1S 1.400(6) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? C1S H1SC 0.9700 . ? C2S Cl1 1.758(10) . ? C2S Cl2 1.772(10) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? Zn1 O41 1.9553(16) . ? Zn1 O21 1.9828(15) . ? Zn1 N02 2.0708(18) . ? Zn1 N12 2.0861(18) . ? Zn1 O61 2.1542(18) . ? C01 C02 1.381(3) . ? C01 C10 1.435(3) . ? C01 C11 1.490(3) . ? C02 C03 1.413(3) . ? C02 N02 1.427(3) . ? N02 C35 1.301(3) . ? C03 C04 1.356(3) . ? C03 H03 0.9400 . ? C04 C05 1.404(4) . ? C04 H04 0.9400 . ? C05 C06 1.415(3) . ? C05 C10 1.418(3) . ? C06 C07 1.359(4) . ? C06 H06 0.9400 . ? C07 C08 1.397(4) . ? C07 H07 0.9400 . ? C08 C09 1.364(3) . ? C08 H08 0.9400 . ? C09 C10 1.407(3) . ? C09 H09 0.9400 . ? C11 C12 1.377(3) . ? C11 C20 1.431(3) . ? C12 C13 1.398(3) . ? C12 N12 1.430(3) . ? N12 C55 1.284(3) . ? C13 C14 1.364(3) . ? C13 H13 0.9400 . ? C14 C15 1.401(3) . ? C14 H14 0.9400 . ? C15 C16 1.413(3) . ? C15 C20 1.423(3) . ? C16 C17 1.353(4) . ? C16 H16 0.9400 . ? C17 C18 1.397(3) . ? C17 H17 0.9400 . ? C18 C19 1.367(3) . ? C18 H18 0.9400 . ? C19 C20 1.405(3) . ? C19 H19 0.9400 . ? C21 O21 1.281(3) . ? C21 C22 1.417(3) . ? C21 C34 1.461(3) . ? C22 C23 1.417(3) . ? C22 C35 1.432(3) . ? C23 C24 1.347(3) . ? C23 H23 0.9400 . ? C24 C25 1.408(4) . ? C24 H24 0.9400 . ? C25 C34 1.410(3) . ? C25 C26 1.420(3) . ? C26 C27 1.333(4) . ? C26 H26 0.9400 . ? C27 C28 1.428(4) . ? C27 H27 0.9400 . ? C28 C29 1.412(4) . ? C28 C33 1.413(3) . ? C29 C30 1.353(4) . ? C29 H29 0.9400 . ? C30 C31 1.400(4) . ? C30 H30 0.9400 . ? C31 C32 1.372(3) . ? C31 H31 0.9400 . ? C32 C33 1.407(3) . ? C32 H32 0.9400 . ? C33 C34 1.455(3) . ? C35 H35 0.9400 . ? C41 O41 1.297(3) . ? C41 C42 1.415(3) . ? C41 C54 1.450(3) . ? C42 C43 1.414(3) . ? C42 C55 1.433(3) . ? C43 C44 1.354(3) . ? C43 H43 0.9400 . ? C44 C45 1.406(3) . ? C44 H44 0.9400 . ? C45 C54 1.411(3) . ? C45 C46 1.431(3) . ? C46 C47 1.334(3) . ? C46 H46 0.9400 . ? C47 C48 1.421(3) . ? C47 H47 0.9400 . ? C48 C49 1.410(3) . ? C48 C53 1.417(3) . ? C49 C50 1.360(3) . ? C49 H49 0.9400 . ? C50 C51 1.393(4) . ? C50 H50 0.9400 . ? C51 C52 1.372(3) . ? C51 H51 0.9400 . ? C52 C53 1.409(3) . ? C52 H52 0.9400 . ? C53 C54 1.450(3) . ? C55 H55 0.9400 . ? C61 O61 1.420(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? O61 H61 0.9881 . ? 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 O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? Cl1 C2S Cl2 112.0(7) . . ? Cl1 C2S H2SA 109.2 . . ? Cl2 C2S H2SA 109.2 . . ? Cl1 C2S H2SB 109.2 . . ? Cl2 C2S H2SB 109.2 . . ? H2SA C2S H2SB 107.9 . . ? O41 Zn1 O21 100.52(7) . . ? O41 Zn1 N02 120.71(7) . . ? O21 Zn1 N02 88.49(7) . . ? O41 Zn1 N12 89.07(7) . . ? O21 Zn1 N12 168.37(7) . . ? N02 Zn1 N12 92.26(7) . . ? O41 Zn1 O61 98.26(8) . . ? O21 Zn1 O61 86.53(7) . . ? N02 Zn1 O61 140.95(8) . . ? N12 Zn1 O61 85.58(7) . . ? C02 C01 C10 118.6(2) . . ? C02 C01 C11 123.30(18) . . ? C10 C01 C11 118.14(19) . . ? C01 C02 C03 120.40(19) . . ? C01 C02 N02 122.81(19) . . ? C03 C02 N02 116.66(19) . . ? C35 N02 C02 116.37(19) . . ? C35 N02 Zn1 122.89(15) . . ? C02 N02 Zn1 118.85(14) . . ? C04 C03 C02 121.3(2) . . ? C04 C03 H03 119.4 . . ? C02 C03 H03 119.4 . . ? C03 C04 C05 120.5(2) . . ? C03 C04 H04 119.8 . . ? C05 C04 H04 119.8 . . ? C04 C05 C06 121.5(2) . . ? C04 C05 C10 119.1(2) . . ? C06 C05 C10 119.3(2) . . ? C07 C06 C05 121.0(2) . . ? C07 C06 H06 119.5 . . ? C05 C06 H06 119.5 . . ? C06 C07 C08 120.0(2) . . ? C06 C07 H07 120.0 . . ? C08 C07 H07 120.0 . . ? C09 C08 C07 120.3(2) . . ? C09 C08 H08 119.8 . . ? C07 C08 H08 119.8 . . ? C08 C09 C10 121.7(2) . . ? C08 C09 H09 119.2 . . ? C10 C09 H09 119.2 . . ? C09 C10 C05 117.7(2) . . ? C09 C10 C01 122.4(2) . . ? C05 C10 C01 119.8(2) . . ? C12 C11 C20 118.58(19) . . ? C12 C11 C01 121.02(19) . . ? C20 C11 C01 120.09(18) . . ? C11 C12 C13 121.8(2) . . ? C11 C12 N12 118.64(18) . . ? C13 C12 N12 119.52(19) . . ? C55 N12 C12 117.62(19) . . ? C55 N12 Zn1 120.94(15) . . ? C12 N12 Zn1 120.23(14) . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 121.9(2) . . ? C14 C15 C20 119.4(2) . . ? C16 C15 C20 118.7(2) . . ? C17 C16 C15 122.0(2) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 119.3(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.7(2) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 121.6(2) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C15 117.8(2) . . ? C19 C20 C11 123.00(19) . . ? C15 C20 C11 119.20(19) . . ? O21 C21 C22 121.61(19) . . ? O21 C21 C34 120.6(2) . . ? C22 C21 C34 117.76(19) . . ? C21 O21 Zn1 131.04(15) . . ? C23 C22 C21 120.7(2) . . ? C23 C22 C35 115.8(2) . . ? C21 C22 C35 123.45(19) . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C34 121.3(2) . . ? C24 C25 C26 119.1(2) . . ? C34 C25 C26 119.6(2) . . ? C27 C26 C25 122.4(3) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C33 120.0(2) . . ? C29 C28 C27 120.1(2) . . ? C33 C28 C27 119.9(2) . . ? C30 C29 C28 121.2(2) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119.2(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 120.9(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 121.2(2) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 117.3(2) . . ? C32 C33 C34 123.6(2) . . ? C28 C33 C34 119.1(2) . . ? C25 C34 C33 118.4(2) . . ? C25 C34 C21 118.2(2) . . ? C33 C34 C21 123.2(2) . . ? N02 C35 C22 128.1(2) . . ? N02 C35 H35 115.9 . . ? C22 C35 H35 115.9 . . ? O41 C41 C42 122.1(2) . . ? O41 C41 C54 119.5(2) . . ? C42 C41 C54 118.36(19) . . ? C41 O41 Zn1 125.79(15) . . ? C43 C42 C41 120.2(2) . . ? C43 C42 C55 115.5(2) . . ? C41 C42 C55 124.3(2) . . ? C44 C43 C42 121.3(2) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C45 120.0(2) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C54 121.4(2) . . ? C44 C45 C46 119.1(2) . . ? C54 C45 C46 119.5(2) . . ? C47 C46 C45 121.9(2) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 C47 C48 120.6(2) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C53 119.9(2) . . ? C49 C48 C47 119.9(2) . . ? C53 C48 C47 120.1(2) . . ? C50 C49 C48 121.6(2) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C51 118.8(2) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C52 C51 C50 121.3(2) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 121.4(2) . . ? C51 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C52 C53 C48 117.0(2) . . ? C52 C53 C54 123.85(19) . . ? C48 C53 C54 118.92(19) . . ? C45 C54 C53 118.67(19) . . ? C45 C54 C41 118.1(2) . . ? C53 C54 C41 123.27(19) . . ? N12 C55 C42 127.4(2) . . ? N12 C55 H55 116.3 . . ? C42 C55 H55 116.3 . . ? O61 C61 H61A 109.5 . . ? O61 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O61 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C61 O61 Zn1 122.72(18) . . ? C61 O61 H61 101.9 . . ? Zn1 O61 H61 119.9 . . ? 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 C10 C01 C02 C03 5.9(3) . . . . ? C11 C01 C02 C03 -174.0(2) . . . . ? C10 C01 C02 N02 -169.9(2) . . . . ? C11 C01 C02 N02 10.2(3) . . . . ? C01 C02 N02 C35 -130.2(2) . . . . ? C03 C02 N02 C35 53.8(3) . . . . ? C01 C02 N02 Zn1 65.0(2) . . . . ? C03 C02 N02 Zn1 -111.0(2) . . . . ? O41 Zn1 N02 C35 -112.62(17) . . . . ? O21 Zn1 N02 C35 -11.27(18) . . . . ? N12 Zn1 N02 C35 157.12(18) . . . . ? O61 Zn1 N02 C35 71.3(2) . . . . ? O41 Zn1 N02 C02 51.16(17) . . . . ? O21 Zn1 N02 C02 152.51(15) . . . . ? N12 Zn1 N02 C02 -39.11(15) . . . . ? O61 Zn1 N02 C02 -124.88(15) . . . . ? C01 C02 C03 C04 -2.1(4) . . . . ? N02 C02 C03 C04 173.9(2) . . . . ? C02 C03 C04 C05 -2.7(4) . . . . ? C03 C04 C05 C06 -174.3(2) . . . . ? C03 C04 C05 C10 3.5(4) . . . . ? C04 C05 C06 C07 178.1(2) . . . . ? C10 C05 C06 C07 0.3(4) . . . . ? C05 C06 C07 C08 -0.2(4) . . . . ? C06 C07 C08 C09 0.2(4) . . . . ? C07 C08 C09 C10 -0.5(4) . . . . ? C08 C09 C10 C05 0.6(3) . . . . ? C08 C09 C10 C01 -178.1(2) . . . . ? C04 C05 C10 C09 -178.4(2) . . . . ? C06 C05 C10 C09 -0.5(3) . . . . ? C04 C05 C10 C01 0.4(3) . . . . ? C06 C05 C10 C01 178.2(2) . . . . ? C02 C01 C10 C09 173.6(2) . . . . ? C11 C01 C10 C09 -6.4(3) . . . . ? C02 C01 C10 C05 -5.0(3) . . . . ? C11 C01 C10 C05 174.92(19) . . . . ? C02 C01 C11 C12 -69.7(3) . . . . ? C10 C01 C11 C12 110.4(2) . . . . ? C02 C01 C11 C20 116.8(2) . . . . ? C10 C01 C11 C20 -63.1(3) . . . . ? C20 C11 C12 C13 1.1(3) . . . . ? C01 C11 C12 C13 -172.54(19) . . . . ? C20 C11 C12 N12 -179.59(18) . . . . ? C01 C11 C12 N12 6.8(3) . . . . ? C11 C12 N12 C55 -120.6(2) . . . . ? C13 C12 N12 C55 58.7(3) . . . . ? C11 C12 N12 Zn1 71.9(2) . . . . ? C13 C12 N12 Zn1 -108.8(2) . . . . ? O41 Zn1 N12 C55 24.63(17) . . . . ? O21 Zn1 N12 C55 -121.2(3) . . . . ? N02 Zn1 N12 C55 145.33(17) . . . . ? O61 Zn1 N12 C55 -73.73(17) . . . . ? O41 Zn1 N12 C12 -168.29(16) . . . . ? O21 Zn1 N12 C12 45.9(4) . . . . ? N02 Zn1 N12 C12 -47.59(16) . . . . ? O61 Zn1 N12 C12 93.35(16) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? N12 C12 C13 C14 -179.2(2) . . . . ? C12 C13 C14 C15 -1.5(4) . . . . ? C13 C14 C15 C16 -178.6(2) . . . . ? C13 C14 C15 C20 1.7(3) . . . . ? C14 C15 C16 C17 -178.5(2) . . . . ? C20 C15 C16 C17 1.2(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C19 -1.6(3) . . . . ? C17 C18 C19 C20 1.1(3) . . . . ? C18 C19 C20 C15 0.6(3) . . . . ? C18 C19 C20 C11 179.0(2) . . . . ? C14 C15 C20 C19 178.0(2) . . . . ? C16 C15 C20 C19 -1.7(3) . . . . ? C14 C15 C20 C11 -0.4(3) . . . . ? C16 C15 C20 C11 179.86(19) . . . . ? C12 C11 C20 C19 -179.2(2) . . . . ? C01 C11 C20 C19 -5.6(3) . . . . ? C12 C11 C20 C15 -0.9(3) . . . . ? C01 C11 C20 C15 172.78(18) . . . . ? C22 C21 O21 Zn1 -18.6(3) . . . . ? C34 C21 O21 Zn1 160.66(16) . . . . ? O41 Zn1 O21 C21 143.81(19) . . . . ? N02 Zn1 O21 C21 22.8(2) . . . . ? N12 Zn1 O21 C21 -71.1(4) . . . . ? O61 Zn1 O21 C21 -118.4(2) . . . . ? O21 C21 C22 C23 179.9(2) . . . . ? C34 C21 C22 C23 0.7(3) . . . . ? O21 C21 C22 C35 -3.6(3) . . . . ? C34 C21 C22 C35 177.1(2) . . . . ? C21 C22 C23 C24 -5.7(4) . . . . ? C35 C22 C23 C24 177.6(2) . . . . ? C22 C23 C24 C25 3.3(4) . . . . ? C23 C24 C25 C34 4.2(4) . . . . ? C23 C24 C25 C26 -175.8(3) . . . . ? C24 C25 C26 C27 -179.8(3) . . . . ? C34 C25 C26 C27 0.2(5) . . . . ? C25 C26 C27 C28 2.6(5) . . . . ? C26 C27 C28 C29 178.6(3) . . . . ? C26 C27 C28 C33 -0.7(5) . . . . ? C33 C28 C29 C30 2.6(4) . . . . ? C27 C28 C29 C30 -176.7(3) . . . . ? C28 C29 C30 C31 0.7(5) . . . . ? C29 C30 C31 C32 -2.0(4) . . . . ? C30 C31 C32 C33 0.1(4) . . . . ? C31 C32 C33 C28 3.1(4) . . . . ? C31 C32 C33 C34 -178.2(2) . . . . ? C29 C28 C33 C32 -4.4(4) . . . . ? C27 C28 C33 C32 174.9(3) . . . . ? C29 C28 C33 C34 176.9(2) . . . . ? C27 C28 C33 C34 -3.8(4) . . . . ? C24 C25 C34 C33 175.2(2) . . . . ? C26 C25 C34 C33 -4.7(4) . . . . ? C24 C25 C34 C21 -9.0(4) . . . . ? C26 C25 C34 C21 171.0(2) . . . . ? C32 C33 C34 C25 -172.2(2) . . . . ? C28 C33 C34 C25 6.5(3) . . . . ? C32 C33 C34 C21 12.4(4) . . . . ? C28 C33 C34 C21 -169.0(2) . . . . ? O21 C21 C34 C25 -172.8(2) . . . . ? C22 C21 C34 C25 6.5(3) . . . . ? O21 C21 C34 C33 2.7(3) . . . . ? C22 C21 C34 C33 -178.1(2) . . . . ? C02 N02 C35 C22 -166.8(2) . . . . ? Zn1 N02 C35 C22 -2.7(3) . . . . ? C23 C22 C35 N02 -169.0(2) . . . . ? C21 C22 C35 N02 14.4(4) . . . . ? C42 C41 O41 Zn1 31.5(3) . . . . ? C54 C41 O41 Zn1 -150.12(16) . . . . ? O21 Zn1 O41 C41 137.37(18) . . . . ? N02 Zn1 O41 C41 -128.08(18) . . . . ? N12 Zn1 O41 C41 -36.00(19) . . . . ? O61 Zn1 O41 C41 49.39(19) . . . . ? O41 C41 C42 C43 172.3(2) . . . . ? C54 C41 C42 C43 -6.0(3) . . . . ? O41 C41 C42 C55 -4.5(3) . . . . ? C54 C41 C42 C55 177.2(2) . . . . ? C41 C42 C43 C44 -0.7(3) . . . . ? C55 C42 C43 C44 176.4(2) . . . . ? C42 C43 C44 C45 3.8(4) . . . . ? C43 C44 C45 C54 0.1(3) . . . . ? C43 C44 C45 C46 179.2(2) . . . . ? C44 C45 C46 C47 -175.4(2) . . . . ? C54 C45 C46 C47 3.7(3) . . . . ? C45 C46 C47 C48 1.6(4) . . . . ? C46 C47 C48 C49 173.5(2) . . . . ? C46 C47 C48 C53 -4.1(3) . . . . ? C53 C48 C49 C50 1.8(3) . . . . ? C47 C48 C49 C50 -175.9(2) . . . . ? C48 C49 C50 C51 -0.8(4) . . . . ? C49 C50 C51 C52 -0.6(4) . . . . ? C50 C51 C52 C53 1.0(4) . . . . ? C51 C52 C53 C48 0.0(3) . . . . ? C51 C52 C53 C54 174.7(2) . . . . ? C49 C48 C53 C52 -1.3(3) . . . . ? C47 C48 C53 C52 176.3(2) . . . . ? C49 C48 C53 C54 -176.3(2) . . . . ? C47 C48 C53 C54 1.3(3) . . . . ? C44 C45 C54 C53 172.8(2) . . . . ? C46 C45 C54 C53 -6.3(3) . . . . ? C44 C45 C54 C41 -6.8(3) . . . . ? C46 C45 C54 C41 174.08(19) . . . . ? C52 C53 C54 C45 -170.8(2) . . . . ? C48 C53 C54 C45 3.9(3) . . . . ? C52 C53 C54 C41 8.8(3) . . . . ? C48 C53 C54 C41 -176.57(19) . . . . ? O41 C41 C54 C45 -168.8(2) . . . . ? C42 C41 C54 C45 9.6(3) . . . . ? O41 C41 C54 C53 11.6(3) . . . . ? C42 C41 C54 C53 -169.98(19) . . . . ? C12 N12 C55 C42 -177.9(2) . . . . ? Zn1 N12 C55 C42 -10.5(3) . . . . ? C43 C42 C55 N12 177.5(2) . . . . ? C41 C42 C55 N12 -5.6(4) . . . . ? O41 Zn1 O61 C61 38.3(2) . . . . ? O21 Zn1 O61 C61 -61.9(2) . . . . ? N02 Zn1 O61 C61 -145.2(2) . . . . ? N12 Zn1 O61 C61 126.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.315 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.068 data_Compound_(R)-9 _database_code_depnum_ccdc_archive 'CCDC 276259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(II)/binaphthyl bis(phenanthrenolate)imine ; _chemical_name_common 'Fe(ii)/binaphthyl bis(phenanthrenolate)imine' _chemical_melting_point ? _chemical_formula_moiety ; (C50 H30 N2 O2 Fe) (C H2 Cl2) ; _chemical_formula_sum 'C51 H32 Cl2 Fe N2 O2' _chemical_formula_weight 831.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1443(12) _cell_length_b 16.4557(15) _cell_length_c 18.9601(17) _cell_angle_alpha 99.736(6) _cell_angle_beta 104.006(6) _cell_angle_gamma 94.156(4) _cell_volume 3894.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1833 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49344 _diffrn_reflns_av_R_equivalents 0.1024 _diffrn_reflns_av_sigmaI/netI 0.1408 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 28.39 _reflns_number_total 17792 _reflns_number_gt 7587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17792 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1632 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6428(4) 0.6001(3) 0.2743(3) 0.0672(14) Uani 1 1 d . . . H1A H 0.6366 0.5389 0.2598 0.081 Uiso 1 1 calc R . . H1B H 0.5899 0.6140 0.3024 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.76945(11) 0.63690(9) 0.33119(8) 0.0798(4) Uani 1 1 d . . . Cl2 Cl 0.61647(11) 0.64330(10) 0.19500(7) 0.0821(4) Uani 1 1 d . . . C2 C 0.8771(4) 0.9139(3) 0.2326(3) 0.0638(14) Uani 1 1 d . . . H2A H 0.8884 0.9752 0.2467 0.077 Uiso 1 1 calc R . . H2B H 0.9225 0.8967 0.1994 0.077 Uiso 1 1 calc R . . Cl3 Cl 0.74523(11) 0.88263(9) 0.18494(8) 0.0791(4) Uani 1 1 d . . . Cl4 Cl 0.91462(11) 0.87176(9) 0.31216(7) 0.0779(4) Uani 1 1 d . . . Fe1 Fe 0.46475(4) 0.18555(3) 0.29862(3) 0.03463(16) Uani 1 1 d . . . Fe2 Fe 0.06238(4) 0.32639(3) 0.20226(3) 0.03479(16) Uani 1 1 d . . . C101 C 0.4166(3) 0.2809(2) 0.46336(19) 0.0284(8) Uani 1 1 d . . . C102 C 0.3445(3) 0.2634(2) 0.3950(2) 0.0313(9) Uani 1 1 d . . . N102 N 0.3423(2) 0.18792(18) 0.34475(16) 0.0326(7) Uani 1 1 d . . . C103 C 0.2795(3) 0.3225(2) 0.3699(2) 0.0393(10) Uani 1 1 d . . . H103 H 0.2322 0.3100 0.3219 0.047 Uiso 1 1 calc R . . C104 C 0.2843(3) 0.3973(2) 0.4142(2) 0.0394(10) Uani 1 1 d . . . H104 H 0.2374 0.4356 0.3979 0.047 Uiso 1 1 calc R . . C105 C 0.3575(3) 0.4190(2) 0.4838(2) 0.0338(9) Uani 1 1 d . . . C106 C 0.3671(3) 0.4980(2) 0.5285(2) 0.0420(10) Uani 1 1 d . . . H106 H 0.3193 0.5361 0.5133 0.050 Uiso 1 1 calc R . . C107 C 0.4429(3) 0.5206(2) 0.5926(2) 0.0424(10) Uani 1 1 d . . . H107 H 0.4485 0.5744 0.6219 0.051 Uiso 1 1 calc R . . C108 C 0.5137(3) 0.4648(2) 0.6163(2) 0.0374(10) Uani 1 1 d . . . H108 H 0.5683 0.4815 0.6608 0.045 Uiso 1 1 calc R . . C109 C 0.5041(3) 0.3867(2) 0.57559(19) 0.0320(9) Uani 1 1 d . . . H109 H 0.5510 0.3489 0.5931 0.038 Uiso 1 1 calc R . . C110 C 0.4264(3) 0.3607(2) 0.50811(19) 0.0305(9) Uani 1 1 d . . . C111 C 0.4803(3) 0.2148(2) 0.48999(19) 0.0272(8) Uani 1 1 d . . . C112 C 0.5566(3) 0.1873(2) 0.45740(19) 0.0299(9) Uani 1 1 d . . . N112 N 0.5759(2) 0.21989(18) 0.39597(15) 0.0309(7) Uani 1 1 d . . . C113 C 0.6133(3) 0.1216(2) 0.4796(2) 0.0380(10) Uani 1 1 d . . . H113 H 0.6647 0.1024 0.4552 0.046 Uiso 1 1 calc R . . C114 C 0.5943(3) 0.0866(2) 0.5348(2) 0.0378(10) Uani 1 1 d . . . H114 H 0.6319 0.0421 0.5487 0.045 Uiso 1 1 calc R . . C115 C 0.5196(3) 0.1148(2) 0.5727(2) 0.0352(9) Uani 1 1 d . . . C116 C 0.5033(3) 0.0818(2) 0.6337(2) 0.0444(11) Uani 1 1 d . . . H116 H 0.5420 0.0385 0.6489 0.053 Uiso 1 1 calc R . . C117 C 0.4336(4) 0.1109(3) 0.6710(2) 0.0503(12) Uani 1 1 d . . . H117 H 0.4255 0.0894 0.7131 0.060 Uiso 1 1 calc R . . C118 C 0.3736(3) 0.1725(3) 0.6475(2) 0.0462(11) Uani 1 1 d . . . H118 H 0.3233 0.1917 0.6729 0.055 Uiso 1 1 calc R . . C119 C 0.3863(3) 0.2054(2) 0.5885(2) 0.0358(9) Uani 1 1 d . . . H119 H 0.3440 0.2468 0.5730 0.043 Uiso 1 1 calc R . . C120 C 0.4611(3) 0.1792(2) 0.54995(19) 0.0288(8) Uani 1 1 d . . . C121 C 0.3324(3) 0.0245(2) 0.2458(2) 0.0367(10) Uani 1 1 d . . . O121 O 0.4107(2) 0.07696(15) 0.24498(14) 0.0383(6) Uani 1 1 d . . . C122 C 0.2658(3) 0.0451(2) 0.2922(2) 0.0352(9) Uani 1 1 d . . . C123 C 0.1873(3) -0.0156(3) 0.2976(2) 0.0488(11) Uani 1 1 d . . . H123 H 0.1432 -0.0017 0.3297 0.059 Uiso 1 1 calc R . . C124 C 0.1751(3) -0.0932(3) 0.2571(3) 0.0555(13) Uani 1 1 d . . . H124 H 0.1233 -0.1337 0.2620 0.067 Uiso 1 1 calc R . . C125 C 0.2384(3) -0.1155(3) 0.2072(3) 0.0507(12) Uani 1 1 d . . . C126 C 0.2216(4) -0.1985(3) 0.1651(3) 0.0655(15) Uani 1 1 d . . . H126 H 0.1679 -0.2375 0.1699 0.079 Uiso 1 1 calc R . . C127 C 0.2817(4) -0.2210(3) 0.1189(3) 0.0694(16) Uani 1 1 d . . . H127 H 0.2714 -0.2769 0.0931 0.083 Uiso 1 1 calc R . . C128 C 0.3589(4) -0.1656(3) 0.1071(3) 0.0590(14) Uani 1 1 d . . . C129 C 0.4171(4) -0.1916(3) 0.0567(3) 0.0723(17) Uani 1 1 d . . . H129 H 0.4053 -0.2480 0.0319 0.087 Uiso 1 1 calc R . . C130 C 0.4898(4) -0.1389(4) 0.0420(3) 0.0810(18) Uani 1 1 d . . . H130 H 0.5277 -0.1575 0.0067 0.097 Uiso 1 1 calc R . . C131 C 0.5075(4) -0.0575(3) 0.0796(2) 0.0648(14) Uani 1 1 d . . . H131 H 0.5589 -0.0201 0.0701 0.078 Uiso 1 1 calc R . . C132 C 0.4535(3) -0.0295(3) 0.1298(2) 0.0539(13) Uani 1 1 d . . . H132 H 0.4679 0.0270 0.1543 0.065 Uiso 1 1 calc R . . C133 C 0.3766(3) -0.0820(2) 0.1463(2) 0.0452(12) Uani 1 1 d . . . C134 C 0.3158(3) -0.0571(2) 0.1996(2) 0.0401(10) Uani 1 1 d . . . C135 C 0.2744(3) 0.1247(2) 0.3393(2) 0.0351(9) Uani 1 1 d . . . H135 H 0.2260 0.1315 0.3692 0.042 Uiso 1 1 calc R . . C141 C 0.6294(3) 0.3043(2) 0.2796(2) 0.0370(10) Uani 1 1 d . . . O141 O 0.5330(2) 0.26362(16) 0.25721(14) 0.0410(7) Uani 1 1 d . . . C142 C 0.6940(3) 0.3042(2) 0.3500(2) 0.0356(9) Uani 1 1 d . . . C143 C 0.7972(3) 0.3479(2) 0.3722(2) 0.0469(11) Uani 1 1 d . . . H143 H 0.8415 0.3467 0.4196 0.056 Uiso 1 1 calc R . . C144 C 0.8334(4) 0.3912(3) 0.3273(3) 0.0527(12) Uani 1 1 d . . . H144 H 0.9031 0.4194 0.3428 0.063 Uiso 1 1 calc R . . C145 C 0.7687(4) 0.3946(2) 0.2581(3) 0.0466(11) Uani 1 1 d . . . C146 C 0.8074(4) 0.4452(3) 0.2145(3) 0.0609(13) Uani 1 1 d . . . H146 H 0.8778 0.4719 0.2317 0.073 Uiso 1 1 calc R . . C147 C 0.7475(5) 0.4561(3) 0.1500(3) 0.0658(15) Uani 1 1 d . . . H147 H 0.7740 0.4939 0.1242 0.079 Uiso 1 1 calc R . . C148 C 0.6460(4) 0.4130(3) 0.1195(3) 0.0569(13) Uani 1 1 d . . . C149 C 0.5848(5) 0.4227(3) 0.0506(3) 0.0760(17) Uani 1 1 d . . . H149 H 0.6125 0.4609 0.0257 0.091 Uiso 1 1 calc R . . C150 C 0.4879(5) 0.3803(3) 0.0179(3) 0.0684(16) Uani 1 1 d . . . H150 H 0.4483 0.3889 -0.0288 0.082 Uiso 1 1 calc R . . C151 C 0.4477(4) 0.3233(3) 0.0546(3) 0.0611(14) Uani 1 1 d . . . H151 H 0.3810 0.2914 0.0319 0.073 Uiso 1 1 calc R . . C152 C 0.5037(4) 0.3133(3) 0.1226(2) 0.0515(12) Uani 1 1 d . . . H152 H 0.4743 0.2749 0.1466 0.062 Uiso 1 1 calc R . . C153 C 0.6033(4) 0.3578(2) 0.1584(2) 0.0460(11) Uani 1 1 d . . . C154 C 0.6652(3) 0.3518(2) 0.2310(2) 0.0409(10) Uani 1 1 d . . . C155 C 0.6640(3) 0.2647(2) 0.4036(2) 0.0353(9) Uani 1 1 d . . . H155 H 0.7141 0.2719 0.4504 0.042 Uiso 1 1 calc R . . C201 C 0.0983(3) 0.2198(2) 0.03758(19) 0.0299(8) Uani 1 1 d . . . C202 C 0.1759(3) 0.2419(2) 0.10351(19) 0.0300(9) Uani 1 1 d . . . N202 N 0.1803(2) 0.31898(19) 0.15182(15) 0.0323(7) Uani 1 1 d . . . C203 C 0.2480(3) 0.1861(2) 0.1261(2) 0.0427(10) Uani 1 1 d . . . H203 H 0.3014 0.2022 0.1713 0.051 Uiso 1 1 calc R . . C204 C 0.2418(3) 0.1102(2) 0.0843(2) 0.0464(11) Uani 1 1 d . . . H204 H 0.2923 0.0740 0.0997 0.056 Uiso 1 1 calc R . . C205 C 0.1618(3) 0.0838(2) 0.0183(2) 0.0362(9) Uani 1 1 d . . . C206 C 0.1504(4) 0.0028(2) -0.0248(2) 0.0485(11) Uani 1 1 d . . . H206 H 0.2017 -0.0335 -0.0113 0.058 Uiso 1 1 calc R . . C207 C 0.0684(4) -0.0233(3) -0.0844(2) 0.0520(12) Uani 1 1 d . . . H207 H 0.0617 -0.0781 -0.1122 0.062 Uiso 1 1 calc R . . C208 C -0.0075(3) 0.0295(2) -0.1058(2) 0.0447(11) Uani 1 1 d . . . H208 H -0.0660 0.0100 -0.1475 0.054 Uiso 1 1 calc R . . C209 C 0.0021(3) 0.1081(2) -0.0676(2) 0.0361(9) Uani 1 1 d . . . H209 H -0.0493 0.1435 -0.0833 0.043 Uiso 1 1 calc R . . C210 C 0.0871(3) 0.1386(2) -0.00472(19) 0.0311(9) Uani 1 1 d . . . C211 C 0.0312(3) 0.2832(2) 0.00981(19) 0.0285(8) Uani 1 1 d . . . C212 C -0.0416(3) 0.3146(2) 0.0438(2) 0.0329(9) Uani 1 1 d . . . N212 N -0.0554(2) 0.28754(18) 0.10883(17) 0.0338(8) Uani 1 1 d . . . C213 C -0.1020(3) 0.3772(2) 0.0185(2) 0.0427(11) Uani 1 1 d . . . H213 H -0.1516 0.3984 0.0436 0.051 Uiso 1 1 calc R . . C214 C -0.0883(3) 0.4063(2) -0.0416(2) 0.0444(11) Uani 1 1 d . . . H214 H -0.1279 0.4488 -0.0578 0.053 Uiso 1 1 calc R . . C215 C -0.0165(3) 0.3749(2) -0.0803(2) 0.0389(10) Uani 1 1 d . . . C216 C -0.0056(3) 0.4008(3) -0.1452(2) 0.0486(12) Uani 1 1 d . . . H216 H -0.0459 0.4423 -0.1629 0.058 Uiso 1 1 calc R . . C217 C 0.0617(4) 0.3673(3) -0.1830(3) 0.0591(13) Uani 1 1 d . . . H217 H 0.0660 0.3838 -0.2279 0.071 Uiso 1 1 calc R . . C218 C 0.1242(4) 0.3090(3) -0.1563(2) 0.0528(12) Uani 1 1 d . . . H218 H 0.1721 0.2869 -0.1827 0.063 Uiso 1 1 calc R . . C219 C 0.1179(3) 0.2831(2) -0.0934(2) 0.0403(10) Uani 1 1 d . . . H219 H 0.1627 0.2443 -0.0754 0.048 Uiso 1 1 calc R . . C220 C 0.0452(3) 0.3132(2) -0.0538(2) 0.0339(9) Uani 1 1 d . . . C221 C 0.1976(3) 0.4878(2) 0.2439(2) 0.0357(10) Uani 1 1 d . . . O221 O 0.12124(19) 0.43669(15) 0.25129(13) 0.0385(7) Uani 1 1 d . . . C222 C 0.2595(3) 0.4620(2) 0.1954(2) 0.0381(10) Uani 1 1 d . . . C223 C 0.3362(3) 0.5206(3) 0.1843(2) 0.0483(11) Uani 1 1 d . . . H223 H 0.3784 0.5027 0.1518 0.058 Uiso 1 1 calc R . . C224 C 0.3504(4) 0.6001(3) 0.2181(3) 0.0542(12) Uani 1 1 d . . . H224 H 0.4003 0.6385 0.2083 0.065 Uiso 1 1 calc R . . C225 C 0.2914(3) 0.6268(3) 0.2683(3) 0.0517(13) Uani 1 1 d . . . C226 C 0.3076(4) 0.7124(3) 0.3027(3) 0.0650(14) Uani 1 1 d . . . H226 H 0.3600 0.7487 0.2933 0.078 Uiso 1 1 calc R . . C227 C 0.2495(4) 0.7420(3) 0.3482(3) 0.0646(15) Uani 1 1 d . . . H227 H 0.2595 0.7998 0.3684 0.078 Uiso 1 1 calc R . . C228 C 0.1744(4) 0.6906(3) 0.3671(2) 0.0575(13) Uani 1 1 d . . . C229 C 0.1162(4) 0.7228(3) 0.4146(3) 0.0745(17) Uani 1 1 d . . . H229 H 0.1253 0.7811 0.4321 0.089 Uiso 1 1 calc R . . C230 C 0.0468(4) 0.6751(3) 0.4376(3) 0.0723(17) Uani 1 1 d . . . H230 H 0.0090 0.6995 0.4710 0.087 Uiso 1 1 calc R . . C231 C 0.0318(4) 0.5882(3) 0.4108(3) 0.0658(15) Uani 1 1 d . . . H231 H -0.0160 0.5536 0.4263 0.079 Uiso 1 1 calc R . . C232 C 0.0867(3) 0.5542(3) 0.3621(2) 0.0512(12) Uani 1 1 d . . . H232 H 0.0758 0.4959 0.3446 0.061 Uiso 1 1 calc R . . C233 C 0.1585(3) 0.6026(2) 0.3370(2) 0.0458(11) Uani 1 1 d . . . C234 C 0.2161(3) 0.5719(2) 0.2846(2) 0.0418(10) Uani 1 1 d . . . C235 C 0.2472(3) 0.3803(2) 0.1526(2) 0.0353(9) Uani 1 1 d . . . H235 H 0.2932 0.3700 0.1212 0.042 Uiso 1 1 calc R . . C241 C -0.0945(3) 0.2128(2) 0.2339(2) 0.0402(10) Uani 1 1 d . . . O241 O -0.0005(2) 0.25416(16) 0.25069(14) 0.0406(7) Uani 1 1 d . . . C242 C -0.1664(3) 0.2097(2) 0.1648(2) 0.0404(10) Uani 1 1 d . . . C243 C -0.2685(3) 0.1647(3) 0.1480(3) 0.0572(13) Uani 1 1 d . . . H243 H -0.3178 0.1638 0.1019 0.069 Uiso 1 1 calc R . . C244 C -0.2954(4) 0.1227(3) 0.1982(3) 0.0681(16) Uani 1 1 d . . . H244 H -0.3641 0.0932 0.1868 0.082 Uiso 1 1 calc R . . C245 C -0.2253(4) 0.1221(3) 0.2654(3) 0.0603(14) Uani 1 1 d . . . C246 C -0.2542(5) 0.0715(3) 0.3134(4) 0.087(2) Uani 1 1 d . . . H246 H -0.3230 0.0419 0.3000 0.104 Uiso 1 1 calc R . . C247 C -0.1871(6) 0.0651(3) 0.3764(4) 0.090(2) Uani 1 1 d . . . H247 H -0.2080 0.0284 0.4055 0.108 Uiso 1 1 calc R . . C248 C -0.0851(5) 0.1112(3) 0.4020(4) 0.0733(17) Uani 1 1 d . . . C249 C -0.0149(6) 0.1052(4) 0.4708(4) 0.088(2) Uani 1 1 d . . . H249 H -0.0360 0.0680 0.4992 0.106 Uiso 1 1 calc R . . C250 C 0.0785(6) 0.1499(4) 0.4962(4) 0.094(2) Uani 1 1 d . . . H250 H 0.1249 0.1430 0.5411 0.112 Uiso 1 1 calc R . . C251 C 0.1083(4) 0.2073(3) 0.4566(3) 0.0702(15) Uani 1 1 d . . . H251 H 0.1734 0.2421 0.4763 0.084 Uiso 1 1 calc R . . C252 C 0.0443(4) 0.2142(3) 0.3893(3) 0.0563(13) Uani 1 1 d . . . H252 H 0.0670 0.2530 0.3627 0.068 Uiso 1 1 calc R . . C253 C -0.0531(4) 0.1656(3) 0.3590(3) 0.0530(13) Uani 1 1 d . . . C254 C -0.1231(3) 0.1678(2) 0.2868(3) 0.0477(12) Uani 1 1 d . . . C255 C -0.1428(3) 0.2450(2) 0.1069(2) 0.0386(10) Uani 1 1 d . . . H255 H -0.1968 0.2367 0.0619 0.046 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 C1 0.068(3) 0.075(4) 0.066(3) 0.010(3) 0.034(3) 0.013(3) Cl1 0.0728(9) 0.0890(11) 0.0780(9) 0.0086(8) 0.0198(7) 0.0289(8) Cl2 0.0781(9) 0.1155(12) 0.0612(8) 0.0200(8) 0.0313(7) 0.0145(9) C2 0.070(3) 0.076(4) 0.062(3) 0.023(3) 0.038(3) 0.023(3) Cl3 0.0736(9) 0.0879(10) 0.0825(10) 0.0204(8) 0.0235(7) 0.0333(8) Cl4 0.0879(10) 0.1011(11) 0.0599(8) 0.0298(8) 0.0337(7) 0.0264(8) Fe1 0.0375(3) 0.0325(3) 0.0319(3) 0.0023(2) 0.0086(3) 0.0018(3) Fe2 0.0357(3) 0.0326(3) 0.0341(3) 0.0031(3) 0.0083(3) 0.0023(3) C101 0.030(2) 0.028(2) 0.030(2) 0.0090(16) 0.0117(16) 0.0069(16) C102 0.033(2) 0.028(2) 0.037(2) 0.0099(17) 0.0126(17) 0.0073(17) N102 0.0340(18) 0.0267(17) 0.0334(17) 0.0034(14) 0.0034(14) 0.0033(15) C103 0.034(2) 0.044(3) 0.037(2) 0.0098(19) 0.0021(18) 0.0108(19) C104 0.041(2) 0.037(2) 0.044(2) 0.014(2) 0.0089(19) 0.0186(19) C105 0.040(2) 0.028(2) 0.039(2) 0.0103(18) 0.0164(18) 0.0105(18) C106 0.048(3) 0.033(2) 0.050(3) 0.010(2) 0.017(2) 0.021(2) C107 0.058(3) 0.027(2) 0.047(3) 0.0039(19) 0.021(2) 0.014(2) C108 0.045(2) 0.031(2) 0.035(2) 0.0048(18) 0.0092(18) 0.0050(19) C109 0.044(2) 0.027(2) 0.0282(19) 0.0090(16) 0.0113(17) 0.0112(18) C110 0.037(2) 0.027(2) 0.032(2) 0.0096(17) 0.0124(17) 0.0094(17) C111 0.033(2) 0.0207(19) 0.0271(19) 0.0034(15) 0.0051(16) 0.0070(16) C112 0.037(2) 0.025(2) 0.0255(19) 0.0018(16) 0.0047(16) 0.0059(17) N112 0.0368(18) 0.0268(17) 0.0299(17) 0.0016(14) 0.0117(14) 0.0074(15) C113 0.037(2) 0.029(2) 0.044(2) 0.0017(19) 0.0050(19) 0.0087(18) C114 0.043(2) 0.022(2) 0.046(2) 0.0085(18) 0.0036(19) 0.0124(18) C115 0.038(2) 0.024(2) 0.038(2) 0.0074(17) -0.0006(18) -0.0014(17) C116 0.052(3) 0.030(2) 0.046(3) 0.017(2) -0.002(2) 0.002(2) C117 0.060(3) 0.045(3) 0.049(3) 0.024(2) 0.011(2) -0.006(2) C118 0.053(3) 0.049(3) 0.042(2) 0.013(2) 0.017(2) 0.006(2) C119 0.043(2) 0.032(2) 0.035(2) 0.0080(18) 0.0121(18) 0.0062(18) C120 0.034(2) 0.0222(19) 0.0273(19) 0.0054(16) 0.0021(16) 0.0016(16) C121 0.036(2) 0.032(2) 0.036(2) 0.0070(18) -0.0035(18) 0.0085(19) O121 0.0390(15) 0.0302(15) 0.0426(16) 0.0008(12) 0.0088(12) 0.0034(13) C122 0.031(2) 0.030(2) 0.041(2) 0.0101(18) -0.0002(18) 0.0031(18) C123 0.038(2) 0.043(3) 0.062(3) 0.015(2) 0.001(2) 0.005(2) C124 0.035(2) 0.035(3) 0.085(4) 0.020(2) -0.010(2) -0.006(2) C125 0.041(3) 0.035(3) 0.062(3) 0.007(2) -0.012(2) 0.007(2) C126 0.055(3) 0.039(3) 0.079(4) 0.011(3) -0.025(3) -0.006(2) C127 0.068(4) 0.041(3) 0.074(4) -0.014(3) -0.014(3) 0.014(3) C128 0.053(3) 0.040(3) 0.063(3) -0.011(2) -0.013(2) 0.014(2) C129 0.074(4) 0.050(3) 0.070(4) -0.024(3) -0.004(3) 0.025(3) C130 0.076(4) 0.078(4) 0.069(4) -0.025(3) 0.003(3) 0.030(3) C131 0.061(3) 0.068(3) 0.056(3) -0.013(3) 0.009(2) 0.028(3) C132 0.048(3) 0.046(3) 0.052(3) -0.008(2) -0.006(2) 0.014(2) C133 0.043(2) 0.032(2) 0.044(2) -0.0079(19) -0.014(2) 0.019(2) C134 0.035(2) 0.026(2) 0.046(2) 0.0031(18) -0.0115(19) 0.0074(18) C135 0.027(2) 0.043(2) 0.037(2) 0.0143(19) 0.0057(17) 0.0099(19) C141 0.041(2) 0.026(2) 0.050(3) 0.0048(19) 0.024(2) 0.0105(19) O141 0.0462(17) 0.0412(17) 0.0391(16) 0.0097(13) 0.0158(13) 0.0070(14) C142 0.039(2) 0.028(2) 0.043(2) 0.0054(18) 0.0159(19) 0.0103(18) C143 0.037(2) 0.042(3) 0.061(3) 0.004(2) 0.016(2) 0.007(2) C144 0.045(3) 0.043(3) 0.074(3) 0.005(2) 0.028(3) 0.003(2) C145 0.056(3) 0.031(2) 0.065(3) 0.009(2) 0.038(3) 0.010(2) C146 0.075(4) 0.043(3) 0.078(4) 0.008(3) 0.047(3) 0.006(3) C147 0.092(4) 0.045(3) 0.079(4) 0.010(3) 0.058(3) 0.012(3) C148 0.092(4) 0.044(3) 0.055(3) 0.014(2) 0.049(3) 0.030(3) C149 0.138(6) 0.045(3) 0.064(4) 0.013(3) 0.055(4) 0.027(4) C150 0.125(5) 0.057(3) 0.039(3) 0.018(3) 0.033(3) 0.048(3) C151 0.082(4) 0.064(3) 0.049(3) 0.011(3) 0.029(3) 0.041(3) C152 0.075(3) 0.053(3) 0.041(2) 0.017(2) 0.030(2) 0.032(3) C153 0.063(3) 0.035(2) 0.053(3) 0.012(2) 0.033(2) 0.022(2) C154 0.059(3) 0.030(2) 0.049(3) 0.0085(19) 0.036(2) 0.020(2) C155 0.034(2) 0.029(2) 0.041(2) 0.0000(18) 0.0085(18) 0.0084(18) C201 0.032(2) 0.028(2) 0.032(2) 0.0105(17) 0.0095(16) 0.0083(17) C202 0.031(2) 0.027(2) 0.035(2) 0.0105(17) 0.0101(17) 0.0067(17) N202 0.0305(17) 0.0328(18) 0.0318(17) 0.0062(14) 0.0036(14) 0.0086(15) C203 0.041(2) 0.043(3) 0.043(2) 0.014(2) 0.0018(19) 0.015(2) C204 0.051(3) 0.036(3) 0.059(3) 0.021(2) 0.014(2) 0.022(2) C205 0.049(2) 0.028(2) 0.040(2) 0.0127(18) 0.021(2) 0.0150(19) C206 0.071(3) 0.032(2) 0.055(3) 0.018(2) 0.029(3) 0.025(2) C207 0.083(4) 0.027(2) 0.053(3) 0.004(2) 0.032(3) 0.013(2) C208 0.058(3) 0.035(2) 0.040(2) 0.0017(19) 0.016(2) 0.005(2) C209 0.041(2) 0.032(2) 0.037(2) 0.0055(18) 0.0123(18) 0.0071(18) C210 0.043(2) 0.026(2) 0.030(2) 0.0116(16) 0.0147(17) 0.0079(17) C211 0.031(2) 0.0228(19) 0.0284(19) 0.0028(16) 0.0019(16) 0.0072(16) C212 0.034(2) 0.026(2) 0.034(2) 0.0028(17) 0.0030(17) 0.0024(17) N212 0.0314(18) 0.0291(18) 0.0402(19) 0.0024(14) 0.0094(15) 0.0092(15) C213 0.037(2) 0.030(2) 0.052(3) -0.002(2) 0.001(2) 0.0108(19) C214 0.041(2) 0.029(2) 0.055(3) 0.011(2) -0.006(2) 0.0087(19) C215 0.037(2) 0.026(2) 0.047(2) 0.0119(19) -0.0046(19) 0.0015(18) C216 0.051(3) 0.037(3) 0.054(3) 0.025(2) -0.004(2) 0.004(2) C217 0.069(3) 0.056(3) 0.054(3) 0.030(2) 0.009(3) -0.003(3) C218 0.062(3) 0.051(3) 0.055(3) 0.025(2) 0.021(2) 0.012(2) C219 0.045(2) 0.040(2) 0.040(2) 0.0174(19) 0.012(2) 0.009(2) C220 0.039(2) 0.023(2) 0.034(2) 0.0077(17) -0.0012(18) 0.0005(17) C221 0.032(2) 0.025(2) 0.042(2) 0.0094(18) -0.0084(18) 0.0045(18) O221 0.0384(15) 0.0353(16) 0.0390(15) 0.0017(12) 0.0071(12) 0.0086(13) C222 0.033(2) 0.035(2) 0.042(2) 0.0107(19) -0.0009(18) 0.0067(19) C223 0.039(2) 0.046(3) 0.055(3) 0.015(2) 0.001(2) 0.000(2) C224 0.050(3) 0.041(3) 0.064(3) 0.014(2) -0.001(2) -0.001(2) C225 0.045(3) 0.030(2) 0.063(3) 0.013(2) -0.020(2) 0.000(2) C226 0.059(3) 0.043(3) 0.074(4) 0.014(3) -0.015(3) -0.004(2) C227 0.068(3) 0.038(3) 0.068(3) 0.005(3) -0.015(3) 0.004(3) C228 0.054(3) 0.051(3) 0.051(3) -0.007(2) -0.010(2) 0.021(3) C229 0.076(4) 0.056(4) 0.070(4) -0.013(3) -0.009(3) 0.029(3) C230 0.067(4) 0.074(4) 0.055(3) -0.025(3) -0.005(3) 0.036(3) C231 0.056(3) 0.071(4) 0.061(3) -0.008(3) 0.007(2) 0.030(3) C232 0.048(3) 0.052(3) 0.043(3) -0.009(2) -0.002(2) 0.026(2) C233 0.039(2) 0.033(2) 0.050(3) -0.003(2) -0.012(2) 0.011(2) C234 0.041(2) 0.036(2) 0.039(2) 0.0029(19) -0.0076(19) 0.014(2) C235 0.032(2) 0.035(2) 0.039(2) 0.0122(18) 0.0065(17) 0.0071(19) C241 0.050(3) 0.027(2) 0.055(3) 0.0050(19) 0.034(2) 0.014(2) O241 0.0378(16) 0.0453(17) 0.0427(16) 0.0135(13) 0.0152(13) 0.0028(13) C242 0.033(2) 0.028(2) 0.060(3) -0.001(2) 0.019(2) 0.0061(18) C243 0.044(3) 0.048(3) 0.078(3) -0.008(3) 0.027(3) 0.001(2) C244 0.051(3) 0.043(3) 0.112(5) -0.013(3) 0.046(3) -0.007(2) C245 0.075(4) 0.037(3) 0.089(4) 0.005(3) 0.063(3) 0.010(3) C246 0.112(5) 0.045(3) 0.133(6) 0.003(4) 0.100(5) 0.004(3) C247 0.149(7) 0.039(3) 0.130(6) 0.027(4) 0.119(5) 0.025(4) C248 0.120(5) 0.043(3) 0.102(5) 0.033(3) 0.093(4) 0.041(3) C249 0.160(7) 0.072(4) 0.094(5) 0.054(4) 0.105(5) 0.074(5) C250 0.143(6) 0.105(5) 0.086(5) 0.058(4) 0.082(5) 0.085(5) C251 0.083(4) 0.094(4) 0.061(3) 0.037(3) 0.045(3) 0.053(3) C252 0.068(3) 0.066(3) 0.060(3) 0.031(3) 0.043(3) 0.035(3) C253 0.081(4) 0.040(3) 0.067(3) 0.023(2) 0.058(3) 0.034(3) C254 0.057(3) 0.032(2) 0.070(3) 0.009(2) 0.045(3) 0.014(2) C255 0.034(2) 0.033(2) 0.046(2) -0.0001(19) 0.0085(19) 0.0125(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Cl2 1.741(5) . ? C1 Cl1 1.750(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 Cl3 1.743(5) . ? C2 Cl4 1.744(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? Fe1 O121 1.893(2) . ? Fe1 O141 1.894(3) . ? Fe1 N102 2.008(3) . ? Fe1 N112 2.021(3) . ? Fe2 O241 1.879(3) . ? Fe2 O221 1.907(2) . ? Fe2 N202 2.010(3) . ? Fe2 N212 2.022(3) . ? C101 C102 1.379(5) . ? C101 C110 1.417(5) . ? C101 C111 1.501(5) . ? C102 C103 1.408(5) . ? C102 N102 1.426(4) . ? N102 C135 1.294(4) . ? C103 C104 1.355(5) . ? C103 H103 0.9500 . ? C104 C105 1.404(5) . ? C104 H104 0.9500 . ? C105 C106 1.406(5) . ? C105 C110 1.424(5) . ? C106 C107 1.348(5) . ? C106 H106 0.9500 . ? C107 C108 1.405(5) . ? C107 H107 0.9500 . ? C108 C109 1.363(5) . ? C108 H108 0.9500 . ? C109 C110 1.408(5) . ? C109 H109 0.9500 . ? C111 C112 1.365(5) . ? C111 C120 1.429(5) . ? C112 C113 1.421(5) . ? C112 N112 1.430(4) . ? N112 C155 1.290(4) . ? C113 C114 1.342(5) . ? C113 H113 0.9500 . ? C114 C115 1.411(5) . ? C114 H114 0.9500 . ? C115 C116 1.411(5) . ? C115 C120 1.419(5) . ? C116 C117 1.353(6) . ? C116 H116 0.9500 . ? C117 C118 1.395(6) . ? C117 H117 0.9500 . ? C118 C119 1.363(5) . ? C118 H118 0.9500 . ? C119 C120 1.410(5) . ? C119 H119 0.9500 . ? C121 O121 1.299(4) . ? C121 C122 1.405(5) . ? C121 C134 1.443(5) . ? C122 C123 1.417(5) . ? C122 C135 1.434(5) . ? C123 C124 1.351(6) . ? C123 H123 0.9500 . ? C124 C125 1.424(6) . ? C124 H124 0.9500 . ? C125 C134 1.398(6) . ? C125 C126 1.433(6) . ? C126 C127 1.341(7) . ? C126 H126 0.9500 . ? C127 C128 1.398(7) . ? C127 H127 0.9500 . ? C128 C129 1.395(7) . ? C128 C133 1.422(5) . ? C129 C130 1.354(7) . ? C129 H129 0.9500 . ? C130 C131 1.382(6) . ? C130 H130 0.9500 . ? C131 C132 1.360(6) . ? C131 H131 0.9500 . ? C132 C133 1.409(6) . ? C132 H132 0.9500 . ? C133 C134 1.460(6) . ? C135 H135 0.9500 . ? C141 O141 1.326(4) . ? C141 C142 1.398(5) . ? C141 C154 1.443(5) . ? C142 C155 1.411(5) . ? C142 C143 1.419(5) . ? C143 C144 1.345(6) . ? C143 H143 0.9500 . ? C144 C145 1.393(6) . ? C144 H144 0.9500 . ? C145 C146 1.417(6) . ? C145 C154 1.418(6) . ? C146 C147 1.333(6) . ? C146 H146 0.9500 . ? C147 C148 1.403(7) . ? C147 H147 0.9500 . ? C148 C149 1.399(7) . ? C148 C153 1.427(6) . ? C149 C150 1.356(7) . ? C149 H149 0.9500 . ? C150 C151 1.404(7) . ? C150 H150 0.9500 . ? C151 C152 1.365(6) . ? C151 H151 0.9500 . ? C152 C153 1.405(6) . ? C152 H152 0.9500 . ? C153 C154 1.443(6) . ? C155 H155 0.9500 . ? C201 C202 1.382(5) . ? C201 C210 1.414(5) . ? C201 C211 1.497(5) . ? C202 C203 1.409(5) . ? C202 N202 1.422(4) . ? N202 C235 1.285(4) . ? C203 C204 1.347(5) . ? C203 H203 0.9500 . ? C204 C205 1.405(5) . ? C204 H204 0.9500 . ? C205 C206 1.417(5) . ? C205 C210 1.423(5) . ? C206 C207 1.343(6) . ? C206 H206 0.9500 . ? C207 C208 1.402(6) . ? C207 H207 0.9500 . ? C208 C209 1.353(5) . ? C208 H208 0.9500 . ? C209 C210 1.411(5) . ? C209 H209 0.9500 . ? C211 C212 1.362(5) . ? C211 C220 1.423(5) . ? C212 C213 1.421(5) . ? C212 N212 1.426(5) . ? N212 C255 1.290(5) . ? C213 C214 1.353(6) . ? C213 H213 0.9500 . ? C214 C215 1.405(6) . ? C214 H214 0.9500 . ? C215 C216 1.402(6) . ? C215 C220 1.427(5) . ? C216 C217 1.359(6) . ? C216 H216 0.9500 . ? C217 C218 1.390(6) . ? C217 H217 0.9500 . ? C218 C219 1.351(5) . ? C218 H218 0.9500 . ? C219 C220 1.419(5) . ? C219 H219 0.9500 . ? C221 O221 1.311(4) . ? C221 C222 1.403(5) . ? C221 C234 1.438(5) . ? C222 C223 1.422(5) . ? C222 C235 1.424(5) . ? C223 C224 1.334(6) . ? C223 H223 0.9500 . ? C224 C225 1.401(6) . ? C224 H224 0.9500 . ? C225 C234 1.416(6) . ? C225 C226 1.425(6) . ? C226 C227 1.340(7) . ? C226 H226 0.9500 . ? C227 C228 1.405(7) . ? C227 H227 0.9500 . ? C228 C229 1.381(7) . ? C228 C233 1.444(6) . ? C229 C230 1.357(7) . ? C229 H229 0.9500 . ? C230 C231 1.416(6) . ? C230 H230 0.9500 . ? C231 C232 1.376(6) . ? C231 H231 0.9500 . ? C232 C233 1.409(6) . ? C232 H232 0.9500 . ? C233 C234 1.437(6) . ? C235 H235 0.9500 . ? C241 O241 1.306(4) . ? C241 C242 1.409(6) . ? C241 C254 1.445(6) . ? C242 C255 1.412(6) . ? C242 C243 1.422(5) . ? C243 C244 1.364(7) . ? C243 H243 0.9500 . ? C244 C245 1.381(7) . ? C244 H244 0.9500 . ? C245 C254 1.421(6) . ? C245 C246 1.430(7) . ? C246 C247 1.328(8) . ? C246 H246 0.9500 . ? C247 C248 1.422(8) . ? C247 H247 0.9500 . ? C248 C253 1.415(6) . ? C248 C249 1.426(8) . ? C249 C250 1.320(8) . ? C249 H249 0.9500 . ? C250 C251 1.391(7) . ? C250 H250 0.9500 . ? C251 C252 1.376(6) . ? C251 H251 0.9500 . ? C252 C253 1.397(6) . ? C252 H252 0.9500 . ? C253 C254 1.461(6) . ? C255 H255 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 C1 Cl1 111.5(3) . . ? Cl2 C1 H1A 109.3 . . ? Cl1 C1 H1A 109.3 . . ? Cl2 C1 H1B 109.3 . . ? Cl1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? Cl3 C2 Cl4 112.5(3) . . ? Cl3 C2 H2A 109.1 . . ? Cl4 C2 H2A 109.1 . . ? Cl3 C2 H2B 109.1 . . ? Cl4 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? O121 Fe1 O141 121.68(11) . . ? O121 Fe1 N102 89.95(11) . . ? O141 Fe1 N102 133.38(12) . . ? O121 Fe1 N112 128.37(12) . . ? O141 Fe1 N112 90.52(12) . . ? N102 Fe1 N112 94.80(12) . . ? O241 Fe2 O221 121.06(11) . . ? O241 Fe2 N202 133.44(12) . . ? O221 Fe2 N202 89.48(11) . . ? O241 Fe2 N212 90.39(12) . . ? O221 Fe2 N212 129.28(12) . . ? N202 Fe2 N212 95.70(12) . . ? C102 C101 C110 118.8(3) . . ? C102 C101 C111 119.8(3) . . ? C110 C101 C111 121.4(3) . . ? C101 C102 C103 121.3(3) . . ? C101 C102 N102 120.1(3) . . ? C103 C102 N102 118.3(3) . . ? C135 N102 C102 120.6(3) . . ? C135 N102 Fe1 125.0(3) . . ? C102 N102 Fe1 113.8(2) . . ? C104 C103 C102 120.1(3) . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C105 121.1(4) . . ? C103 C104 H104 119.5 . . ? C105 C104 H104 119.5 . . ? C104 C105 C106 121.5(4) . . ? C104 C105 C110 119.0(3) . . ? C106 C105 C110 119.4(3) . . ? C107 C106 C105 121.2(4) . . ? C107 C106 H106 119.4 . . ? C105 C106 H106 119.4 . . ? C106 C107 C108 120.2(4) . . ? C106 C107 H107 119.9 . . ? C108 C107 H107 119.9 . . ? C109 C108 C107 120.1(4) . . ? C109 C108 H108 119.9 . . ? C107 C108 H108 119.9 . . ? C108 C109 C110 121.5(3) . . ? C108 C109 H109 119.3 . . ? C110 C109 H109 119.3 . . ? C109 C110 C101 122.8(3) . . ? C109 C110 C105 117.5(3) . . ? C101 C110 C105 119.6(3) . . ? C112 C111 C120 119.0(3) . . ? C112 C111 C101 121.0(3) . . ? C120 C111 C101 120.1(3) . . ? C111 C112 C113 121.3(4) . . ? C111 C112 N112 120.4(3) . . ? C113 C112 N112 118.1(3) . . ? C155 N112 C112 119.6(3) . . ? C155 N112 Fe1 123.5(3) . . ? C112 N112 Fe1 116.8(2) . . ? C114 C113 C112 120.2(4) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C115 121.1(4) . . ? C113 C114 H114 119.4 . . ? C115 C114 H114 119.4 . . ? C116 C115 C114 121.7(4) . . ? C116 C115 C120 119.2(4) . . ? C114 C115 C120 119.1(4) . . ? C117 C116 C115 121.3(4) . . ? C117 C116 H116 119.4 . . ? C115 C116 H116 119.4 . . ? C116 C117 C118 119.7(4) . . ? C116 C117 H117 120.1 . . ? C118 C117 H117 120.1 . . ? C119 C118 C117 120.8(4) . . ? C119 C118 H118 119.6 . . ? C117 C118 H118 119.6 . . ? C118 C119 C120 121.2(4) . . ? C118 C119 H119 119.4 . . ? C120 C119 H119 119.4 . . ? C119 C120 C115 117.7(3) . . ? C119 C120 C111 122.9(3) . . ? C115 C120 C111 119.3(3) . . ? O121 C121 C122 121.1(3) . . ? O121 C121 C134 119.2(4) . . ? C122 C121 C134 119.7(4) . . ? C121 O121 Fe1 133.3(2) . . ? C121 C122 C123 120.1(4) . . ? C121 C122 C135 124.1(3) . . ? C123 C122 C135 115.7(4) . . ? C124 C123 C122 120.1(4) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 121.3(4) . . ? C123 C124 H124 119.4 . . ? C125 C124 H124 119.4 . . ? C134 C125 C124 120.3(4) . . ? C134 C125 C126 120.7(5) . . ? C124 C125 C126 119.0(4) . . ? C127 C126 C125 119.8(5) . . ? C127 C126 H126 120.1 . . ? C125 C126 H126 120.1 . . ? C126 C127 C128 122.7(5) . . ? C126 C127 H127 118.6 . . ? C128 C127 H127 118.6 . . ? C129 C128 C127 120.4(5) . . ? C129 C128 C133 120.2(5) . . ? C127 C128 C133 119.4(5) . . ? C130 C129 C128 122.0(5) . . ? C130 C129 H129 119.0 . . ? C128 C129 H129 119.0 . . ? C129 C130 C131 118.4(5) . . ? C129 C130 H130 120.8 . . ? C131 C130 H130 120.8 . . ? C132 C131 C130 121.8(5) . . ? C132 C131 H131 119.1 . . ? C130 C131 H131 119.1 . . ? C131 C132 C133 121.7(4) . . ? C131 C132 H132 119.2 . . ? C133 C132 H132 119.2 . . ? C132 C133 C128 116.0(4) . . ? C132 C133 C134 125.1(4) . . ? C128 C133 C134 118.9(4) . . ? C125 C134 C121 118.3(4) . . ? C125 C134 C133 118.4(4) . . ? C121 C134 C133 123.4(4) . . ? N102 C135 C122 125.8(4) . . ? N102 C135 H135 117.1 . . ? C122 C135 H135 117.1 . . ? O141 C141 C142 120.9(4) . . ? O141 C141 C154 118.6(4) . . ? C142 C141 C154 120.4(4) . . ? C141 O141 Fe1 131.0(3) . . ? C141 C142 C155 125.0(4) . . ? C141 C142 C143 119.5(4) . . ? C155 C142 C143 115.5(4) . . ? C144 C143 C142 121.3(4) . . ? C144 C143 H143 119.4 . . ? C142 C143 H143 119.4 . . ? C143 C144 C145 119.9(4) . . ? C143 C144 H144 120.0 . . ? C145 C144 H144 120.0 . . ? C144 C145 C146 118.1(4) . . ? C144 C145 C154 122.6(4) . . ? C146 C145 C154 119.2(5) . . ? C147 C146 C145 121.6(5) . . ? C147 C146 H146 119.2 . . ? C145 C146 H146 119.2 . . ? C146 C147 C148 121.4(5) . . ? C146 C147 H147 119.3 . . ? C148 C147 H147 119.3 . . ? C149 C148 C147 121.1(5) . . ? C149 C148 C153 118.6(5) . . ? C147 C148 C153 120.2(5) . . ? C150 C149 C148 123.2(5) . . ? C150 C149 H149 118.4 . . ? C148 C149 H149 118.4 . . ? C149 C150 C151 118.3(5) . . ? C149 C150 H150 120.9 . . ? C151 C150 H150 120.9 . . ? C152 C151 C150 120.4(5) . . ? C152 C151 H151 119.8 . . ? C150 C151 H151 119.8 . . ? C151 C152 C153 122.3(5) . . ? C151 C152 H152 118.8 . . ? C153 C152 H152 118.8 . . ? C152 C153 C148 117.0(4) . . ? C152 C153 C154 125.1(4) . . ? C148 C153 C154 117.9(4) . . ? C145 C154 C141 116.2(4) . . ? C145 C154 C153 119.4(4) . . ? C141 C154 C153 124.5(4) . . ? N112 C155 C142 126.9(4) . . ? N112 C155 H155 116.5 . . ? C142 C155 H155 116.5 . . ? C202 C201 C210 119.4(3) . . ? C202 C201 C211 119.7(3) . . ? C210 C201 C211 120.8(3) . . ? C201 C202 C203 120.4(3) . . ? C201 C202 N202 120.6(3) . . ? C203 C202 N202 118.8(3) . . ? C235 N202 C202 119.7(3) . . ? C235 N202 Fe2 125.0(3) . . ? C202 N202 Fe2 114.6(2) . . ? C204 C203 C202 120.7(4) . . ? C204 C203 H203 119.7 . . ? C202 C203 H203 119.7 . . ? C203 C204 C205 120.9(4) . . ? C203 C204 H204 119.5 . . ? C205 C204 H204 119.5 . . ? C204 C205 C206 122.0(4) . . ? C204 C205 C210 119.2(3) . . ? C206 C205 C210 118.7(4) . . ? C207 C206 C205 121.0(4) . . ? C207 C206 H206 119.5 . . ? C205 C206 H206 119.5 . . ? C206 C207 C208 120.5(4) . . ? C206 C207 H207 119.8 . . ? C208 C207 H207 119.8 . . ? C209 C208 C207 120.4(4) . . ? C209 C208 H208 119.8 . . ? C207 C208 H208 119.8 . . ? C208 C209 C210 121.3(4) . . ? C208 C209 H209 119.4 . . ? C210 C209 H209 119.4 . . ? C209 C210 C201 122.8(3) . . ? C209 C210 C205 118.0(3) . . ? C201 C210 C205 119.1(3) . . ? C212 C211 C220 118.6(3) . . ? C212 C211 C201 122.5(3) . . ? C220 C211 C201 118.8(3) . . ? C211 C212 C213 121.9(4) . . ? C211 C212 N212 119.9(3) . . ? C213 C212 N212 118.1(3) . . ? C255 N212 C212 119.8(3) . . ? C255 N212 Fe2 123.5(3) . . ? C212 N212 Fe2 116.6(2) . . ? C214 C213 C212 119.6(4) . . ? C214 C213 H213 120.2 . . ? C212 C213 H213 120.2 . . ? C213 C214 C215 121.2(4) . . ? C213 C214 H214 119.4 . . ? C215 C214 H214 119.4 . . ? C216 C215 C214 122.1(4) . . ? C216 C215 C220 119.1(4) . . ? C214 C215 C220 118.8(4) . . ? C217 C216 C215 120.9(4) . . ? C217 C216 H216 119.6 . . ? C215 C216 H216 119.6 . . ? C216 C217 C218 120.3(4) . . ? C216 C217 H217 119.9 . . ? C218 C217 H217 119.9 . . ? C219 C218 C217 121.0(4) . . ? C219 C218 H218 119.5 . . ? C217 C218 H218 119.5 . . ? C218 C219 C220 120.9(4) . . ? C218 C219 H219 119.6 . . ? C220 C219 H219 119.6 . . ? C219 C220 C211 122.5(3) . . ? C219 C220 C215 117.8(4) . . ? C211 C220 C215 119.8(4) . . ? O221 C221 C222 120.7(3) . . ? O221 C221 C234 119.5(4) . . ? C222 C221 C234 119.8(4) . . ? C221 O221 Fe2 133.0(2) . . ? C221 C222 C223 119.3(4) . . ? C221 C222 C235 124.0(4) . . ? C223 C222 C235 116.5(4) . . ? C224 C223 C222 121.9(4) . . ? C224 C223 H223 119.1 . . ? C222 C223 H223 119.1 . . ? C223 C224 C225 119.7(4) . . ? C223 C224 H224 120.2 . . ? C225 C224 H224 120.2 . . ? C224 C225 C234 122.1(4) . . ? C224 C225 C226 118.2(5) . . ? C234 C225 C226 119.7(5) . . ? C227 C226 C225 120.7(5) . . ? C227 C226 H226 119.6 . . ? C225 C226 H226 119.6 . . ? C226 C227 C228 122.2(5) . . ? C226 C227 H227 118.9 . . ? C228 C227 H227 118.9 . . ? C229 C228 C227 121.0(5) . . ? C229 C228 C233 119.6(5) . . ? C227 C228 C233 119.5(5) . . ? C230 C229 C228 123.2(5) . . ? C230 C229 H229 118.4 . . ? C228 C229 H229 118.4 . . ? C229 C230 C231 118.6(5) . . ? C229 C230 H230 120.7 . . ? C231 C230 H230 120.7 . . ? C232 C231 C230 119.8(5) . . ? C232 C231 H231 120.1 . . ? C230 C231 H231 120.1 . . ? C231 C232 C233 122.6(4) . . ? C231 C232 H232 118.7 . . ? C233 C232 H232 118.7 . . ? C232 C233 C234 125.8(4) . . ? C232 C233 C228 116.2(4) . . ? C234 C233 C228 118.0(4) . . ? C225 C234 C233 119.7(4) . . ? C225 C234 C221 117.0(4) . . ? C233 C234 C221 123.2(4) . . ? N202 C235 C222 126.8(4) . . ? N202 C235 H235 116.6 . . ? C222 C235 H235 116.6 . . ? O241 C241 C242 121.0(4) . . ? O241 C241 C254 118.9(4) . . ? C242 C241 C254 120.0(4) . . ? C241 O241 Fe2 132.1(3) . . ? C241 C242 C255 124.4(4) . . ? C241 C242 C243 120.0(4) . . ? C255 C242 C243 115.4(4) . . ? C244 C243 C242 119.7(5) . . ? C244 C243 H243 120.2 . . ? C242 C243 H243 120.2 . . ? C243 C244 C245 121.6(5) . . ? C243 C244 H244 119.2 . . ? C245 C244 H244 119.2 . . ? C244 C245 C254 121.8(5) . . ? C244 C245 C246 119.4(5) . . ? C254 C245 C246 118.8(6) . . ? C247 C246 C245 121.5(6) . . ? C247 C246 H246 119.2 . . ? C245 C246 H246 119.2 . . ? C246 C247 C248 122.2(6) . . ? C246 C247 H247 118.9 . . ? C248 C247 H247 118.9 . . ? C253 C248 C247 119.3(6) . . ? C253 C248 C249 119.1(6) . . ? C247 C248 C249 121.6(6) . . ? C250 C249 C248 122.0(6) . . ? C250 C249 H249 119.0 . . ? C248 C249 H249 119.0 . . ? C249 C250 C251 119.4(7) . . ? C249 C250 H250 120.3 . . ? C251 C250 H250 120.3 . . ? C252 C251 C250 120.7(6) . . ? C252 C251 H251 119.7 . . ? C250 C251 H251 119.7 . . ? C251 C252 C253 121.6(5) . . ? C251 C252 H252 119.2 . . ? C253 C252 H252 119.2 . . ? C252 C253 C248 117.0(5) . . ? C252 C253 C254 124.4(4) . . ? C248 C253 C254 118.6(5) . . ? C245 C254 C241 116.8(5) . . ? C245 C254 C253 119.2(4) . . ? C241 C254 C253 124.0(4) . . ? N212 C255 C242 126.6(4) . . ? N212 C255 H255 116.7 . . ? C242 C255 H255 116.7 . . ? 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 C110 C101 C102 C103 -1.4(5) . . . . ? C111 C101 C102 C103 176.6(3) . . . . ? C110 C101 C102 N102 171.8(3) . . . . ? C111 C101 C102 N102 -10.2(5) . . . . ? C101 C102 N102 C135 98.5(4) . . . . ? C103 C102 N102 C135 -88.1(4) . . . . ? C101 C102 N102 Fe1 -72.6(4) . . . . ? C103 C102 N102 Fe1 100.8(3) . . . . ? O121 Fe1 N102 C135 9.4(3) . . . . ? O141 Fe1 N102 C135 145.6(3) . . . . ? N112 Fe1 N102 C135 -119.1(3) . . . . ? O121 Fe1 N102 C102 180.0(2) . . . . ? O141 Fe1 N102 C102 -43.8(3) . . . . ? N112 Fe1 N102 C102 51.5(2) . . . . ? C101 C102 C103 C104 -2.3(6) . . . . ? N102 C102 C103 C104 -175.6(3) . . . . ? C102 C103 C104 C105 3.4(6) . . . . ? C103 C104 C105 C106 176.5(4) . . . . ? C103 C104 C105 C110 -0.9(6) . . . . ? C104 C105 C106 C107 -174.9(4) . . . . ? C110 C105 C106 C107 2.6(6) . . . . ? C105 C106 C107 C108 -0.5(6) . . . . ? C106 C107 C108 C109 -1.8(6) . . . . ? C107 C108 C109 C110 2.1(6) . . . . ? C108 C109 C110 C101 177.9(4) . . . . ? C108 C109 C110 C105 -0.1(5) . . . . ? C102 C101 C110 C109 -174.1(3) . . . . ? C111 C101 C110 C109 7.9(5) . . . . ? C102 C101 C110 C105 3.9(5) . . . . ? C111 C101 C110 C105 -174.1(3) . . . . ? C104 C105 C110 C109 175.3(3) . . . . ? C106 C105 C110 C109 -2.2(5) . . . . ? C104 C105 C110 C101 -2.8(5) . . . . ? C106 C105 C110 C101 179.7(3) . . . . ? C102 C101 C111 C112 69.3(5) . . . . ? C110 C101 C111 C112 -112.8(4) . . . . ? C102 C101 C111 C120 -110.3(4) . . . . ? C110 C101 C111 C120 67.7(5) . . . . ? C120 C111 C112 C113 3.0(5) . . . . ? C101 C111 C112 C113 -176.5(3) . . . . ? C120 C111 C112 N112 178.3(3) . . . . ? C101 C111 C112 N112 -1.3(5) . . . . ? C111 C112 N112 C155 112.6(4) . . . . ? C113 C112 N112 C155 -72.0(4) . . . . ? C111 C112 N112 Fe1 -71.5(4) . . . . ? C113 C112 N112 Fe1 103.9(3) . . . . ? O121 Fe1 N112 C155 119.4(3) . . . . ? O141 Fe1 N112 C155 -13.3(3) . . . . ? N102 Fe1 N112 C155 -146.9(3) . . . . ? O121 Fe1 N112 C112 -56.4(3) . . . . ? O141 Fe1 N112 C112 171.0(2) . . . . ? N102 Fe1 N112 C112 37.3(3) . . . . ? C111 C112 C113 C114 -1.8(5) . . . . ? N112 C112 C113 C114 -177.1(3) . . . . ? C112 C113 C114 C115 -1.0(5) . . . . ? C113 C114 C115 C116 -176.3(4) . . . . ? C113 C114 C115 C120 2.2(5) . . . . ? C114 C115 C116 C117 178.1(4) . . . . ? C120 C115 C116 C117 -0.4(5) . . . . ? C115 C116 C117 C118 2.3(6) . . . . ? C116 C117 C118 C119 -1.7(6) . . . . ? C117 C118 C119 C120 -0.8(6) . . . . ? C118 C119 C120 C115 2.7(5) . . . . ? C118 C119 C120 C111 -177.0(3) . . . . ? C116 C115 C120 C119 -2.0(5) . . . . ? C114 C115 C120 C119 179.4(3) . . . . ? C116 C115 C120 C111 177.6(3) . . . . ? C114 C115 C120 C111 -0.9(5) . . . . ? C112 C111 C120 C119 178.0(3) . . . . ? C101 C111 C120 C119 -2.5(5) . . . . ? C112 C111 C120 C115 -1.7(5) . . . . ? C101 C111 C120 C115 177.8(3) . . . . ? C122 C121 O121 Fe1 1.9(5) . . . . ? C134 C121 O121 Fe1 -176.4(2) . . . . ? O141 Fe1 O121 C121 -150.3(3) . . . . ? N102 Fe1 O121 C121 -6.5(3) . . . . ? N112 Fe1 O121 C121 89.6(3) . . . . ? O121 C121 C122 C123 -173.9(3) . . . . ? C134 C121 C122 C123 4.4(6) . . . . ? O121 C121 C122 C135 2.7(6) . . . . ? C134 C121 C122 C135 -179.0(3) . . . . ? C121 C122 C123 C124 -1.1(6) . . . . ? C135 C122 C123 C124 -178.0(4) . . . . ? C122 C123 C124 C125 -1.4(6) . . . . ? C123 C124 C125 C134 0.6(6) . . . . ? C123 C124 C125 C126 -179.4(4) . . . . ? C134 C125 C126 C127 1.2(7) . . . . ? C124 C125 C126 C127 -178.8(4) . . . . ? C125 C126 C127 C128 -2.7(7) . . . . ? C126 C127 C128 C129 -178.0(5) . . . . ? C126 C127 C128 C133 1.1(7) . . . . ? C127 C128 C129 C130 177.7(5) . . . . ? C133 C128 C129 C130 -1.5(7) . . . . ? C128 C129 C130 C131 1.3(8) . . . . ? C129 C130 C131 C132 -0.6(8) . . . . ? C130 C131 C132 C133 0.2(7) . . . . ? C131 C132 C133 C128 -0.3(6) . . . . ? C131 C132 C133 C134 179.5(4) . . . . ? C129 C128 C133 C132 1.0(6) . . . . ? C127 C128 C133 C132 -178.2(4) . . . . ? C129 C128 C133 C134 -178.9(4) . . . . ? C127 C128 C133 C134 1.9(6) . . . . ? C124 C125 C134 C121 2.7(6) . . . . ? C126 C125 C134 C121 -177.3(4) . . . . ? C124 C125 C134 C133 -178.2(4) . . . . ? C126 C125 C134 C133 1.8(6) . . . . ? O121 C121 C134 C125 173.2(3) . . . . ? C122 C121 C134 C125 -5.1(5) . . . . ? O121 C121 C134 C133 -5.8(5) . . . . ? C122 C121 C134 C133 175.8(3) . . . . ? C132 C133 C134 C125 176.9(4) . . . . ? C128 C133 C134 C125 -3.3(5) . . . . ? C132 C133 C134 C121 -4.1(6) . . . . ? C128 C133 C134 C121 175.8(4) . . . . ? C102 N102 C135 C122 -178.6(3) . . . . ? Fe1 N102 C135 C122 -8.6(5) . . . . ? C121 C122 C135 N102 1.2(6) . . . . ? C123 C122 C135 N102 178.0(3) . . . . ? C142 C141 O141 Fe1 -11.1(5) . . . . ? C154 C141 O141 Fe1 171.4(2) . . . . ? O121 Fe1 O141 C141 -121.3(3) . . . . ? N102 Fe1 O141 C141 113.1(3) . . . . ? N112 Fe1 O141 C141 16.0(3) . . . . ? O141 C141 C142 C155 -2.1(6) . . . . ? C154 C141 C142 C155 175.4(3) . . . . ? O141 C141 C142 C143 179.6(3) . . . . ? C154 C141 C142 C143 -2.9(5) . . . . ? C141 C142 C143 C144 1.4(6) . . . . ? C155 C142 C143 C144 -177.0(4) . . . . ? C142 C143 C144 C145 1.0(6) . . . . ? C143 C144 C145 C146 176.0(4) . . . . ? C143 C144 C145 C154 -2.0(6) . . . . ? C144 C145 C146 C147 -175.3(4) . . . . ? C154 C145 C146 C147 2.8(6) . . . . ? C145 C146 C147 C148 -5.0(7) . . . . ? C146 C147 C148 C149 -177.9(4) . . . . ? C146 C147 C148 C153 1.9(7) . . . . ? C147 C148 C149 C150 177.7(4) . . . . ? C153 C148 C149 C150 -2.1(7) . . . . ? C148 C149 C150 C151 -0.6(7) . . . . ? C149 C150 C151 C152 2.1(7) . . . . ? C150 C151 C152 C153 -0.9(6) . . . . ? C151 C152 C153 C148 -1.9(6) . . . . ? C151 C152 C153 C154 178.3(4) . . . . ? C149 C148 C153 C152 3.3(6) . . . . ? C147 C148 C153 C152 -176.5(4) . . . . ? C149 C148 C153 C154 -176.9(4) . . . . ? C147 C148 C153 C154 3.3(6) . . . . ? C144 C145 C154 C141 0.5(6) . . . . ? C146 C145 C154 C141 -177.4(3) . . . . ? C144 C145 C154 C153 -179.5(4) . . . . ? C146 C145 C154 C153 2.5(6) . . . . ? O141 C141 C154 C145 179.5(3) . . . . ? C142 C141 C154 C145 1.9(5) . . . . ? O141 C141 C154 C153 -0.5(5) . . . . ? C142 C141 C154 C153 -178.1(3) . . . . ? C152 C153 C154 C145 174.4(4) . . . . ? C148 C153 C154 C145 -5.4(5) . . . . ? C152 C153 C154 C141 -5.6(6) . . . . ? C148 C153 C154 C141 174.6(4) . . . . ? C112 N112 C155 C142 -177.3(3) . . . . ? Fe1 N112 C155 C142 7.0(5) . . . . ? C141 C142 C155 N112 3.4(6) . . . . ? C143 C142 C155 N112 -178.2(3) . . . . ? C210 C201 C202 C203 4.3(5) . . . . ? C211 C201 C202 C203 -172.4(3) . . . . ? C210 C201 C202 N202 -171.8(3) . . . . ? C211 C201 C202 N202 11.6(5) . . . . ? C201 C202 N202 C235 -100.9(4) . . . . ? C203 C202 N202 C235 83.0(4) . . . . ? C201 C202 N202 Fe2 69.8(4) . . . . ? C203 C202 N202 Fe2 -106.3(3) . . . . ? O241 Fe2 N202 C235 -144.5(3) . . . . ? O221 Fe2 N202 C235 -9.9(3) . . . . ? N212 Fe2 N202 C235 119.5(3) . . . . ? O241 Fe2 N202 C202 45.3(3) . . . . ? O221 Fe2 N202 C202 179.9(2) . . . . ? N212 Fe2 N202 C202 -50.7(2) . . . . ? C201 C202 C203 C204 -0.7(6) . . . . ? N202 C202 C203 C204 175.4(4) . . . . ? C202 C203 C204 C205 -1.8(6) . . . . ? C203 C204 C205 C206 -176.9(4) . . . . ? C203 C204 C205 C210 0.6(6) . . . . ? C204 C205 C206 C207 174.5(4) . . . . ? C210 C205 C206 C207 -3.0(6) . . . . ? C205 C206 C207 C208 0.8(7) . . . . ? C206 C207 C208 C209 1.3(7) . . . . ? C207 C208 C209 C210 -1.1(6) . . . . ? C208 C209 C210 C201 -178.5(4) . . . . ? C208 C209 C210 C205 -1.1(6) . . . . ? C202 C201 C210 C209 172.0(3) . . . . ? C211 C201 C210 C209 -11.4(5) . . . . ? C202 C201 C210 C205 -5.4(5) . . . . ? C211 C201 C210 C205 171.2(3) . . . . ? C204 C205 C210 C209 -174.5(4) . . . . ? C206 C205 C210 C209 3.1(5) . . . . ? C204 C205 C210 C201 3.0(5) . . . . ? C206 C205 C210 C201 -179.5(4) . . . . ? C202 C201 C211 C212 -69.3(5) . . . . ? C210 C201 C211 C212 114.1(4) . . . . ? C202 C201 C211 C220 109.5(4) . . . . ? C210 C201 C211 C220 -67.1(5) . . . . ? C220 C211 C212 C213 -1.2(5) . . . . ? C201 C211 C212 C213 177.6(3) . . . . ? C220 C211 C212 N212 -178.3(3) . . . . ? C201 C211 C212 N212 0.5(5) . . . . ? C211 C212 N212 C255 -113.3(4) . . . . ? C213 C212 N212 C255 69.5(4) . . . . ? C211 C212 N212 Fe2 71.1(4) . . . . ? C213 C212 N212 Fe2 -106.1(3) . . . . ? O241 Fe2 N212 C255 13.8(3) . . . . ? O221 Fe2 N212 C255 -118.4(3) . . . . ? N202 Fe2 N212 C255 147.6(3) . . . . ? O241 Fe2 N212 C212 -170.8(3) . . . . ? O221 Fe2 N212 C212 57.0(3) . . . . ? N202 Fe2 N212 C212 -37.0(3) . . . . ? C211 C212 C213 C214 0.7(5) . . . . ? N212 C212 C213 C214 177.8(3) . . . . ? C212 C213 C214 C215 1.1(6) . . . . ? C213 C214 C215 C216 176.2(4) . . . . ? C213 C214 C215 C220 -2.2(5) . . . . ? C214 C215 C216 C217 -177.7(4) . . . . ? C220 C215 C216 C217 0.7(6) . . . . ? C215 C216 C217 C218 -2.6(7) . . . . ? C216 C217 C218 C219 1.4(7) . . . . ? C217 C218 C219 C220 1.7(6) . . . . ? C218 C219 C220 C211 175.6(4) . . . . ? C218 C219 C220 C215 -3.4(5) . . . . ? C212 C211 C220 C219 -179.0(3) . . . . ? C201 C211 C220 C219 2.2(5) . . . . ? C212 C211 C220 C215 0.0(5) . . . . ? C201 C211 C220 C215 -178.8(3) . . . . ? C216 C215 C220 C219 2.2(5) . . . . ? C214 C215 C220 C219 -179.3(3) . . . . ? C216 C215 C220 C211 -176.8(3) . . . . ? C214 C215 C220 C211 1.7(5) . . . . ? C222 C221 O221 Fe2 -5.1(5) . . . . ? C234 C221 O221 Fe2 173.1(2) . . . . ? O241 Fe2 O221 C221 151.9(3) . . . . ? N202 Fe2 O221 C221 9.1(3) . . . . ? N212 Fe2 O221 C221 -87.9(3) . . . . ? O221 C221 C222 C223 175.1(3) . . . . ? C234 C221 C222 C223 -3.2(5) . . . . ? O221 C221 C222 C235 -1.5(6) . . . . ? C234 C221 C222 C235 -179.7(3) . . . . ? C221 C222 C223 C224 -0.7(6) . . . . ? C235 C222 C223 C224 176.1(4) . . . . ? C222 C223 C224 C225 2.4(6) . . . . ? C223 C224 C225 C234 -0.1(6) . . . . ? C223 C224 C225 C226 -179.2(4) . . . . ? C224 C225 C226 C227 176.6(4) . . . . ? C234 C225 C226 C227 -2.5(7) . . . . ? C225 C226 C227 C228 3.2(7) . . . . ? C226 C227 C228 C229 179.5(5) . . . . ? C226 C227 C228 C233 0.2(7) . . . . ? C227 C228 C229 C230 -176.4(5) . . . . ? C233 C228 C229 C230 2.9(7) . . . . ? C228 C229 C230 C231 -1.0(8) . . . . ? C229 C230 C231 C232 -0.5(7) . . . . ? C230 C231 C232 C233 -0.1(7) . . . . ? C231 C232 C233 C234 -177.9(4) . . . . ? C231 C232 C233 C228 1.8(6) . . . . ? C229 C228 C233 C232 -3.2(6) . . . . ? C227 C228 C233 C232 176.2(4) . . . . ? C229 C228 C233 C234 176.6(4) . . . . ? C227 C228 C233 C234 -4.1(6) . . . . ? C224 C225 C234 C233 179.4(4) . . . . ? C226 C225 C234 C233 -1.5(6) . . . . ? C224 C225 C234 C221 -3.6(6) . . . . ? C226 C225 C234 C221 175.4(4) . . . . ? C232 C233 C234 C225 -175.6(4) . . . . ? C228 C233 C234 C225 4.7(5) . . . . ? C232 C233 C234 C221 7.7(6) . . . . ? C228 C233 C234 C221 -172.1(3) . . . . ? O221 C221 C234 C225 -173.1(3) . . . . ? C222 C221 C234 C225 5.2(5) . . . . ? O221 C221 C234 C233 3.8(5) . . . . ? C222 C221 C234 C233 -178.0(4) . . . . ? C202 N202 C235 C222 177.7(3) . . . . ? Fe2 N202 C235 C222 8.0(5) . . . . ? C221 C222 C235 N202 -0.6(6) . . . . ? C223 C222 C235 N202 -177.2(4) . . . . ? C242 C241 O241 Fe2 7.7(5) . . . . ? C254 C241 O241 Fe2 -174.1(2) . . . . ? O221 Fe2 O241 C241 123.9(3) . . . . ? N202 Fe2 O241 C241 -112.3(3) . . . . ? N212 Fe2 O241 C241 -14.1(3) . . . . ? O241 C241 C242 C255 4.2(6) . . . . ? C254 C241 C242 C255 -174.0(4) . . . . ? O241 C241 C242 C243 -179.6(3) . . . . ? C254 C241 C242 C243 2.1(5) . . . . ? C241 C242 C243 C244 -1.7(6) . . . . ? C255 C242 C243 C244 174.8(4) . . . . ? C242 C243 C244 C245 -0.7(7) . . . . ? C243 C244 C245 C254 2.6(7) . . . . ? C243 C244 C245 C246 -174.7(4) . . . . ? C244 C245 C246 C247 176.0(5) . . . . ? C254 C245 C246 C247 -1.5(7) . . . . ? C245 C246 C247 C248 3.5(8) . . . . ? C246 C247 C248 C253 -0.3(8) . . . . ? C246 C247 C248 C249 178.3(5) . . . . ? C253 C248 C249 C250 1.1(8) . . . . ? C247 C248 C249 C250 -177.6(5) . . . . ? C248 C249 C250 C251 2.8(9) . . . . ? C249 C250 C251 C252 -4.0(8) . . . . ? C250 C251 C252 C253 1.4(7) . . . . ? C251 C252 C253 C248 2.4(6) . . . . ? C251 C252 C253 C254 -177.9(4) . . . . ? C247 C248 C253 C252 175.1(4) . . . . ? C249 C248 C253 C252 -3.6(6) . . . . ? C247 C248 C253 C254 -4.6(6) . . . . ? C249 C248 C253 C254 176.7(4) . . . . ? C244 C245 C254 C241 -2.1(6) . . . . ? C246 C245 C254 C241 175.3(4) . . . . ? C244 C245 C254 C253 179.1(4) . . . . ? C246 C245 C254 C253 -3.5(6) . . . . ? O241 C241 C254 C245 -178.5(3) . . . . ? C242 C241 C254 C245 -0.3(5) . . . . ? O241 C241 C254 C253 0.2(6) . . . . ? C242 C241 C254 C253 178.5(4) . . . . ? C252 C253 C254 C245 -173.2(4) . . . . ? C248 C253 C254 C245 6.5(6) . . . . ? C252 C253 C254 C241 8.1(6) . . . . ? C248 C253 C254 C241 -172.2(4) . . . . ? C212 N212 C255 C242 176.0(3) . . . . ? Fe2 N212 C255 C242 -8.7(5) . . . . ? C241 C242 C255 N212 -2.9(6) . . . . ? C243 C242 C255 N212 -179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.515 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.071