Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chen, Jhy-Horung' 'Chen, Ching-Huei' 'Elango, Shanmugham' 'Hsieh, Hsi-Ying' 'Lee, Yu-I.' 'Liao, Fen-Ling' 'Liau, Bing-Chuang' 'Wang, Sue-Lein' _publ_contact_author_name 'Dr Jhy-Horung Chen' _publ_contact_author_address ; Department of Chemistry National Chung-Hsing University Taichung 40227 TAIWAN ; _publ_contact_author_email 'JYHHCHEN@DRAGON.NCHU.EDU.TW' _publ_section_title ; Chloro-N-p-nitrobenzoylimido-meso-tetraphenylporphyrinatoiron(III): A high spin complex ; data_sp12m #[Zn(N-p-NCOC6H4NO2-tpp)(MeOH).MeOH] (compound 4(MeOH).MeOH) _database_code_CSD 182281 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H40 N6 O5 Zn' _chemical_formula_weight 906.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.865(3) _cell_length_b 18.088(3) _cell_length_c 16.773(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.200(4) _cell_angle_gamma 90.00 _cell_volume 4474.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 927 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Tabular _exptl_crystal_colour Blue _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6665 _exptl_absorpt_correction_T_max 0.9368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 26251 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9991 _reflns_number_gt 6639 _reflns_threshold_expression >2sigma(I) _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^)+(0.1466P)^2^+2.5834P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9991 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2432 _refine_ls_wR_factor_gt 0.2223 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _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 Zn1 Zn 1.41246(3) 0.87113(3) 0.77431(3) 0.03978(18) Uani 1 1 d . . . O1 O 1.2404(4) 0.6877(3) 0.7957(9) 0.069(3) Uani 0.67(3) 1 d P . . O1' O 1.2753(16) 0.6859(7) 0.858(2) 0.084(9) Uani 0.33(3) 1 d P . . O2 O 1.6793(4) 0.5254(3) 0.8373(5) 0.144(2) Uani 1 1 d . . . O3 O 1.6125(4) 0.4806(4) 0.7200(4) 0.151(3) Uani 1 1 d . . . O4 O 1.3611(3) 0.97921(17) 0.7801(2) 0.0697(10) Uani 1 1 d . . . O5 O 1.2608(3) 1.0428(2) 0.6568(3) 0.0828(11) Uani 1 1 d . . . N1 N 1.4722(2) 0.87086(17) 0.89200(19) 0.0389(7) Uani 1 1 d . . . N2 N 1.5270(2) 0.87024(18) 0.7290(2) 0.0421(7) Uani 1 1 d . . . N3 N 1.3337(2) 0.86111(17) 0.66405(19) 0.0375(7) Uani 1 1 d . . . N4 N 1.2674(2) 0.83201(18) 0.83117(19) 0.0382(7) Uani 1 1 d . . . N5 N 1.3361(2) 0.78626(18) 0.8087(2) 0.0414(7) Uani 1 1 d . . . N6 N 1.6144(5) 0.5200(5) 0.7799(6) 0.132(3) Uani 1 1 d . . . C1 C 1.2670(3) 0.8567(2) 0.9084(2) 0.0403(8) Uani 1 1 d . . . C2 C 1.3409(3) 0.8547(2) 0.9704(2) 0.0411(8) Uani 1 1 d . . . C3 C 1.4343(3) 0.8542(2) 0.9605(2) 0.0416(8) Uani 1 1 d . . . C4 C 1.5065(3) 0.8368(2) 1.0245(2) 0.0471(9) Uani 1 1 d . . . C5 C 1.5850(3) 0.8419(2) 0.9935(2) 0.0459(9) Uani 1 1 d . . . C6 C 1.5646(2) 0.8641(2) 0.9104(2) 0.0400(8) Uani 1 1 d . . . C7 C 1.6295(3) 0.8728(2) 0.8562(2) 0.0413(8) Uani 1 1 d . . . C8 C 1.6108(2) 0.8784(2) 0.7721(2) 0.0409(8) Uani 1 1 d . . . C9 C 1.6746(3) 0.8938(2) 0.7162(3) 0.0457(9) Uani 1 1 d . . . C10 C 1.6287(3) 0.8919(2) 0.6417(2) 0.0452(9) Uani 1 1 d . . . C11 C 1.5356(3) 0.8751(2) 0.6493(2) 0.0401(8) Uani 1 1 d . . . C12 C 1.4645(3) 0.8653(2) 0.5862(2) 0.0407(8) Uani 1 1 d . . . C13 C 1.3722(3) 0.8539(2) 0.5946(2) 0.0397(8) Uani 1 1 d . . . C14 C 1.3036(3) 0.8316(3) 0.5309(2) 0.0490(10) Uani 1 1 d . . . C15 C 1.2247(3) 0.8268(2) 0.5615(2) 0.0470(9) Uani 1 1 d . . . C16 C 1.2425(2) 0.8446(2) 0.6457(2) 0.0375(8) Uani 1 1 d . . . C17 C 1.1760(2) 0.8481(2) 0.6982(2) 0.0390(8) Uani 1 1 d . . . C18 C 1.1906(2) 0.8535(2) 0.7824(2) 0.0383(8) Uani 1 1 d . . . C19 C 1.1345(3) 0.8871(2) 0.8350(3) 0.0445(9) Uani 1 1 d . . . C20 C 1.1798(3) 0.8891(2) 0.9106(2) 0.0474(9) Uani 1 1 d . . . C21 C 1.3150(3) 0.8575(2) 1.0533(2) 0.0468(10) Uani 1 1 d . . . C22 C 1.2498(3) 0.8085(3) 1.0750(3) 0.0551(11) Uani 1 1 d . . . C23 C 1.2226(4) 0.8095(4) 1.1514(3) 0.0760(16) Uani 1 1 d . . . C24 C 1.2617(5) 0.8607(4) 1.2053(3) 0.0836(19) Uani 1 1 d . . . C25 C 1.3253(5) 0.9098(4) 1.1854(3) 0.0831(19) Uani 1 1 d . . . C26 C 1.3525(4) 0.9086(3) 1.1095(3) 0.0607(12) Uani 1 1 d . . . C27 C 1.7278(3) 0.8698(2) 0.8905(3) 0.0439(9) Uani 1 1 d . . . C28 C 1.7624(3) 0.9188(3) 0.9506(3) 0.0627(12) Uani 1 1 d . . . C29 C 1.8541(4) 0.9149(4) 0.9818(4) 0.0830(17) Uani 1 1 d . . . C30 C 1.9093(3) 0.8629(4) 0.9506(4) 0.0861(19) Uani 1 1 d . . . C31 C 1.8758(3) 0.8154(4) 0.8929(4) 0.0748(16) Uani 1 1 d . . . C32 C 1.7834(3) 0.8177(3) 0.8623(3) 0.0568(11) Uani 1 1 d . . . C33 C 1.4899(3) 0.8649(2) 0.5031(2) 0.0427(9) Uani 1 1 d . . . C34 C 1.5473(3) 0.8108(2) 0.4797(3) 0.0466(9) Uani 1 1 d . . . C35 C 1.5713(3) 0.8106(3) 0.4025(3) 0.0582(12) Uani 1 1 d . . . C36 C 1.5393(4) 0.8645(3) 0.3486(3) 0.0631(13) Uani 1 1 d . . . C37 C 1.4823(4) 0.9185(3) 0.3706(3) 0.0655(13) Uani 1 1 d . . . C38 C 1.4570(3) 0.9182(3) 0.4474(3) 0.0558(11) Uani 1 1 d . . . C39 C 1.0789(2) 0.8523(2) 0.6628(2) 0.0417(9) Uani 1 1 d . . . C40 C 1.0499(3) 0.9012(3) 0.6021(3) 0.0617(12) Uani 1 1 d . . . C41 C 0.9589(3) 0.9043(4) 0.5704(3) 0.0788(17) Uani 1 1 d . . . C42 C 0.8978(3) 0.8583(4) 0.6006(4) 0.0773(17) Uani 1 1 d . . . C43 C 0.9250(3) 0.8103(3) 0.6607(3) 0.0648(13) Uani 1 1 d . . . C44 C 1.0155(3) 0.8062(3) 0.6926(3) 0.0511(10) Uani 1 1 d . . . C45 C 1.3200(3) 0.7167(2) 0.8046(3) 0.0536(11) Uani 1 1 d . . . C46 C 1.3992(3) 0.6700(2) 0.7892(3) 0.0481(10) Uani 1 1 d . . . C47 C 1.4724(5) 0.6713(5) 0.8484(5) 0.110(2) Uani 1 1 d . . . C48 C 1.5436(5) 0.6233(5) 0.8463(5) 0.110(3) Uani 1 1 d . . . C49 C 1.5356(5) 0.5745(3) 0.7849(4) 0.0861(18) Uani 1 1 d . . . C50 C 1.4797(6) 0.5771(4) 0.7232(5) 0.124(3) Uani 1 1 d . . . C51 C 1.3996(6) 0.6247(6) 0.7285(6) 0.152(5) Uani 1 1 d . . . C52 C 1.3668(6) 1.0299(3) 0.8410(4) 0.093(2) Uani 1 1 d . . . C53 C 1.2675(5) 1.0343(4) 0.5768(5) 0.103(2) Uani 1 1 d . . . H4 H 1.3215 0.9936 0.7268 0.080 Uiso 1 1 d . . . H5 H 1.2624 1.0971 0.6735 0.080 Uiso 1 1 d . . . H4A H 1.4949 0.8212 1.0751 0.080 Uiso 1 1 d . . . H5A H 1.6431 0.8305 1.0181 0.080 Uiso 1 1 d . . . H9A H 1.7366 0.9064 0.7320 0.080 Uiso 1 1 d . . . H10A H 1.6562 0.8983 0.5945 0.080 Uiso 1 1 d . . . H14A H 1.3135 0.8226 0.4812 0.080 Uiso 1 1 d . . . H15A H 1.1642 0.8148 0.5304 0.080 Uiso 1 1 d . . . H19A H 1.0794 0.9098 0.8147 0.080 Uiso 1 1 d . . . H20A H 1.1608 0.9095 0.9557 0.080 Uiso 1 1 d . . . H22A H 1.2231 0.7718 1.0349 0.080 Uiso 1 1 d . . . H23A H 1.1772 0.7726 1.1785 0.080 Uiso 1 1 d . . . H24A H 1.2418 0.8627 1.2560 0.080 Uiso 1 1 d . . . H25A H 1.3528 0.9466 1.2176 0.080 Uiso 1 1 d . . . H26A H 1.3981 0.9436 1.0940 0.080 Uiso 1 1 d . . . H28A H 1.7212 0.9541 0.9760 0.080 Uiso 1 1 d . . . H29A H 1.8675 0.9472 1.0337 0.080 Uiso 1 1 d . . . H30A H 1.9680 0.8709 0.9722 0.080 Uiso 1 1 d . . . H31A H 1.9164 0.7738 0.8739 0.080 Uiso 1 1 d . . . H32A H 1.7604 0.7805 0.8200 0.080 Uiso 1 1 d . . . H34A H 1.5675 0.7713 0.5181 0.080 Uiso 1 1 d . . . H35A H 1.6145 0.7746 0.3869 0.080 Uiso 1 1 d . . . H36A H 1.5561 0.8612 0.2983 0.080 Uiso 1 1 d . . . H37A H 1.4602 0.9613 0.3324 0.080 Uiso 1 1 d . . . H38A H 1.4192 0.9518 0.4627 0.080 Uiso 1 1 d . . . H40A H 1.0838 0.9353 0.5780 0.080 Uiso 1 1 d . . . H41A H 0.9434 0.9414 0.5236 0.080 Uiso 1 1 d . . . H42A H 0.8390 0.8604 0.5786 0.080 Uiso 1 1 d . . . H43A H 0.8859 0.7784 0.6841 0.080 Uiso 1 1 d . . . H44A H 1.0380 0.7731 0.7377 0.080 Uiso 1 1 d . . . H47A H 1.4726 0.7069 0.8924 0.080 Uiso 1 1 d . . . H48A H 1.5989 0.6262 0.8868 0.080 Uiso 1 1 d . . . H50A H 1.4904 0.5511 0.6731 0.080 Uiso 1 1 d . . . H51A H 1.3372 0.6239 0.6814 0.080 Uiso 1 1 d . . . H52A H 1.3983 1.0652 0.8285 0.080 Uiso 1 1 d . . . H52B H 1.3949 1.0075 0.8913 0.080 Uiso 1 1 d . . . H52C H 1.3072 1.0466 0.8509 0.080 Uiso 1 1 d . . . H53A H 1.2402 0.9872 0.5616 0.080 Uiso 1 1 d . . . H53B H 1.3307 1.0355 0.5662 0.080 Uiso 1 1 d . . . H53C H 1.2368 1.0742 0.5447 0.080 Uiso 1 1 d . . . 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 Zn1 0.0302(3) 0.0447(3) 0.0433(3) -0.00118(18) -0.00007(18) -0.00219(17) O1 0.041(3) 0.047(3) 0.121(9) -0.013(3) 0.023(4) -0.010(2) O1' 0.072(12) 0.056(7) 0.14(2) 0.003(8) 0.061(15) -0.001(6) O2 0.104(4) 0.126(5) 0.209(7) 0.032(5) 0.043(5) 0.051(4) O3 0.126(5) 0.128(5) 0.202(7) -0.080(5) 0.035(4) 0.051(4) O4 0.089(3) 0.0514(19) 0.063(2) -0.0196(15) -0.0124(17) 0.0181(17) O5 0.089(3) 0.056(2) 0.103(3) 0.012(2) 0.009(2) 0.0168(19) N1 0.0289(15) 0.0457(17) 0.0414(17) 0.0012(13) 0.0018(13) 0.0002(13) N2 0.0290(15) 0.056(2) 0.0416(17) 0.0006(14) 0.0031(13) -0.0028(13) N3 0.0255(14) 0.0448(17) 0.0420(17) -0.0055(13) 0.0035(12) -0.0035(12) N4 0.0258(15) 0.0460(18) 0.0424(17) -0.0035(14) 0.0026(12) 0.0042(13) N5 0.0284(15) 0.0434(18) 0.0540(19) -0.0034(14) 0.0113(14) 0.0028(13) N6 0.084(5) 0.119(6) 0.194(8) 0.047(6) 0.018(5) 0.032(4) C1 0.0317(19) 0.048(2) 0.042(2) -0.0013(16) 0.0069(16) 0.0018(15) C2 0.036(2) 0.048(2) 0.0387(19) -0.0002(16) 0.0048(16) 0.0016(16) C3 0.0351(19) 0.047(2) 0.042(2) 0.0016(16) -0.0011(16) 0.0017(16) C4 0.040(2) 0.053(2) 0.046(2) 0.0121(18) -0.0008(17) -0.0011(18) C5 0.035(2) 0.053(2) 0.047(2) 0.0030(18) -0.0045(17) 0.0023(17) C6 0.0292(18) 0.045(2) 0.044(2) -0.0004(16) 0.0003(15) -0.0012(15) C7 0.0302(18) 0.043(2) 0.050(2) 0.0020(16) -0.0016(16) -0.0024(15) C8 0.0277(18) 0.046(2) 0.048(2) 0.0009(17) 0.0039(16) -0.0027(15) C9 0.0300(19) 0.050(2) 0.057(2) 0.0036(19) 0.0031(17) -0.0061(16) C10 0.0328(19) 0.053(2) 0.050(2) 0.0026(18) 0.0059(17) -0.0054(16) C11 0.0306(18) 0.047(2) 0.044(2) 0.0010(16) 0.0084(15) -0.0007(15) C12 0.0324(19) 0.049(2) 0.041(2) -0.0016(16) 0.0059(16) 0.0024(15) C13 0.0317(19) 0.045(2) 0.042(2) -0.0076(16) 0.0038(16) -0.0001(15) C14 0.039(2) 0.066(3) 0.042(2) -0.0149(19) 0.0050(17) -0.0019(19) C15 0.036(2) 0.059(3) 0.045(2) -0.0122(18) -0.0002(17) -0.0067(17) C16 0.0265(17) 0.0408(19) 0.045(2) -0.0048(16) 0.0028(15) -0.0007(14) C17 0.0291(18) 0.0417(19) 0.045(2) -0.0030(16) 0.0013(15) -0.0004(14) C18 0.0270(17) 0.042(2) 0.046(2) -0.0021(16) 0.0051(15) -0.0001(14) C19 0.0316(19) 0.052(2) 0.049(2) -0.0031(18) 0.0026(17) 0.0073(16) C20 0.037(2) 0.059(3) 0.046(2) -0.0088(18) 0.0057(17) 0.0073(18) C21 0.037(2) 0.062(3) 0.041(2) 0.0025(18) 0.0027(17) 0.0117(18) C22 0.041(2) 0.074(3) 0.051(2) 0.002(2) 0.0092(19) 0.008(2) C23 0.074(4) 0.097(4) 0.062(3) 0.021(3) 0.029(3) 0.027(3) C24 0.098(5) 0.106(5) 0.049(3) 0.006(3) 0.019(3) 0.039(4) C25 0.113(5) 0.080(4) 0.051(3) -0.019(3) -0.013(3) 0.032(4) C26 0.067(3) 0.063(3) 0.049(3) -0.004(2) -0.006(2) 0.013(2) C27 0.0285(18) 0.051(2) 0.051(2) 0.0063(17) -0.0032(16) -0.0022(16) C28 0.041(2) 0.066(3) 0.076(3) 0.000(2) -0.015(2) -0.002(2) C29 0.053(3) 0.088(4) 0.098(4) 0.002(3) -0.029(3) -0.013(3) C30 0.031(2) 0.108(5) 0.112(5) 0.024(4) -0.018(3) -0.002(3) C31 0.040(3) 0.100(4) 0.084(4) 0.017(3) 0.006(3) 0.022(3) C32 0.040(2) 0.070(3) 0.059(3) 0.009(2) 0.003(2) 0.009(2) C33 0.0303(18) 0.052(2) 0.045(2) -0.0040(17) 0.0044(16) -0.0051(16) C34 0.036(2) 0.053(2) 0.052(2) -0.0056(18) 0.0106(17) -0.0039(17) C35 0.047(2) 0.072(3) 0.059(3) -0.019(2) 0.020(2) -0.012(2) C36 0.063(3) 0.082(4) 0.046(2) -0.007(2) 0.016(2) -0.018(3) C37 0.076(3) 0.073(3) 0.046(3) 0.002(2) 0.003(2) -0.008(3) C38 0.054(3) 0.061(3) 0.052(2) -0.001(2) 0.003(2) 0.005(2) C39 0.0272(18) 0.053(2) 0.044(2) -0.0051(17) 0.0012(15) -0.0001(15) C40 0.038(2) 0.082(3) 0.064(3) 0.014(3) 0.000(2) 0.004(2) C41 0.040(3) 0.115(5) 0.077(4) 0.019(3) -0.009(2) 0.015(3) C42 0.026(2) 0.122(5) 0.081(4) -0.008(3) -0.003(2) 0.005(3) C43 0.034(2) 0.098(4) 0.063(3) -0.010(3) 0.008(2) -0.017(2) C44 0.036(2) 0.069(3) 0.048(2) -0.006(2) 0.0038(18) -0.0093(19) C45 0.043(2) 0.044(2) 0.079(3) -0.003(2) 0.026(2) -0.0022(18) C46 0.040(2) 0.038(2) 0.068(3) -0.0047(19) 0.013(2) 0.0033(16) C47 0.085(5) 0.131(6) 0.113(5) -0.025(5) 0.007(4) 0.041(4) C48 0.080(5) 0.127(6) 0.122(6) -0.013(5) 0.007(4) 0.035(4) C49 0.111(5) 0.057(3) 0.093(4) -0.002(3) 0.026(4) 0.030(3) C50 0.145(7) 0.100(6) 0.117(6) -0.049(5) -0.022(5) 0.050(5) C51 0.073(5) 0.224(11) 0.152(8) -0.098(8) -0.009(5) 0.049(6) C52 0.153(6) 0.055(3) 0.072(4) -0.016(3) 0.014(4) -0.004(3) C53 0.094(5) 0.082(4) 0.123(6) 0.024(4) -0.031(4) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 1.951(3) . ? Zn1 N5 2.035(3) . ? Zn1 N1 2.061(3) . ? Zn1 N3 2.069(3) . ? Zn1 O4 2.106(3) . ? O1 O1' 1.11(3) . ? O1 C45 1.285(7) . ? O1' C45 1.306(16) . ? O2 N6 1.278(10) . ? O3 N6 1.229(10) . ? O4 C52 1.367(6) . ? O5 C53 1.367(9) . ? N1 C6 1.374(5) . ? N1 C3 1.375(5) . ? N2 C11 1.361(5) . ? N2 C8 1.367(5) . ? N3 C13 1.367(5) . ? N3 C16 1.384(4) . ? N4 C1 1.371(5) . ? N4 C18 1.376(5) . ? N4 N5 1.402(4) . ? N5 C45 1.281(5) . ? N6 C49 1.541(9) . ? C1 C2 1.416(5) . ? C1 C20 1.427(5) . ? C2 C3 1.419(5) . ? C2 C21 1.489(5) . ? C3 C4 1.453(5) . ? C4 C5 1.340(6) . ? C5 C6 1.446(6) . ? C6 C7 1.415(6) . ? C7 C8 1.408(6) . ? C7 C27 1.502(5) . ? C8 C9 1.442(6) . ? C9 C10 1.347(6) . ? C10 C11 1.438(5) . ? C11 C12 1.409(6) . ? C12 C13 1.412(5) . ? C12 C33 1.489(6) . ? C13 C14 1.439(5) . ? C14 C15 1.342(6) . ? C15 C16 1.440(5) . ? C16 C17 1.406(5) . ? C17 C18 1.404(5) . ? C17 C39 1.493(5) . ? C18 C19 1.424(5) . ? C19 C20 1.360(6) . ? C21 C26 1.388(6) . ? C21 C22 1.394(6) . ? C22 C23 1.390(6) . ? C23 C24 1.372(10) . ? C24 C25 1.369(10) . ? C25 C26 1.383(8) . ? C27 C32 1.376(6) . ? C27 C28 1.391(6) . ? C28 C29 1.398(7) . ? C29 C30 1.394(9) . ? C30 C31 1.342(9) . ? C31 C32 1.406(7) . ? C33 C34 1.387(6) . ? C33 C38 1.389(6) . ? C34 C35 1.385(6) . ? C35 C36 1.374(7) . ? C36 C37 1.373(8) . ? C37 C38 1.386(7) . ? C39 C40 1.375(6) . ? C39 C44 1.398(6) . ? C40 C41 1.391(6) . ? C41 C42 1.374(8) . ? C42 C43 1.354(8) . ? C43 C44 1.386(6) . ? C45 C46 1.498(5) . ? C46 C51 1.307(9) . ? C46 C47 1.378(9) . ? C47 C48 1.373(9) . ? C48 C49 1.351(10) . ? C49 C50 1.244(10) . ? C50 C51 1.481(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N5 130.50(13) . . ? N2 Zn1 N1 94.62(13) . . ? N5 Zn1 N1 85.17(13) . . ? N2 Zn1 N3 94.30(13) . . ? N5 Zn1 N3 85.06(13) . . ? N1 Zn1 N3 169.66(12) . . ? N2 Zn1 O4 111.42(15) . . ? N5 Zn1 O4 117.97(14) . . ? N1 Zn1 O4 94.22(12) . . ? N3 Zn1 O4 87.38(12) . . ? O1' O1 C45 65.7(7) . . ? O1 O1' C45 63.7(13) . . ? C52 O4 Zn1 131.9(4) . . ? C6 N1 C3 107.2(3) . . ? C6 N1 Zn1 120.9(3) . . ? C3 N1 Zn1 128.9(2) . . ? C11 N2 C8 108.8(3) . . ? C11 N2 Zn1 125.1(3) . . ? C8 N2 Zn1 125.1(3) . . ? C13 N3 C16 107.0(3) . . ? C13 N3 Zn1 121.3(2) . . ? C16 N3 Zn1 130.3(3) . . ? C1 N4 C18 111.6(3) . . ? C1 N4 N5 122.4(3) . . ? C18 N4 N5 125.8(3) . . ? C45 N5 N4 117.1(3) . . ? C45 N5 Zn1 146.4(3) . . ? N4 N5 Zn1 94.7(2) . . ? O3 N6 O2 126.7(7) . . ? O3 N6 C49 118.3(8) . . ? O2 N6 C49 114.7(9) . . ? N4 C1 C2 126.2(3) . . ? N4 C1 C20 105.7(3) . . ? C2 C1 C20 127.9(4) . . ? C1 C2 C3 126.5(4) . . ? C1 C2 C21 114.7(3) . . ? C3 C2 C21 118.7(4) . . ? N1 C3 C2 127.3(3) . . ? N1 C3 C4 108.9(3) . . ? C2 C3 C4 123.8(4) . . ? C5 C4 C3 107.2(3) . . ? C4 C5 C6 107.8(3) . . ? N1 C6 C7 126.1(4) . . ? N1 C6 C5 108.9(3) . . ? C7 C6 C5 124.9(3) . . ? C8 C7 C6 125.9(4) . . ? C8 C7 C27 116.5(4) . . ? C6 C7 C27 117.4(4) . . ? N2 C8 C7 125.1(3) . . ? N2 C8 C9 107.9(3) . . ? C7 C8 C9 127.0(4) . . ? C10 C9 C8 107.4(3) . . ? C9 C10 C11 107.8(4) . . ? N2 C11 C12 125.1(3) . . ? N2 C11 C10 108.1(3) . . ? C12 C11 C10 126.8(4) . . ? C11 C12 C13 126.2(4) . . ? C11 C12 C33 116.7(3) . . ? C13 C12 C33 117.1(3) . . ? N3 C13 C12 125.9(3) . . ? N3 C13 C14 109.1(3) . . ? C12 C13 C14 125.0(4) . . ? C15 C14 C13 107.8(3) . . ? C14 C15 C16 107.4(3) . . ? N3 C16 C17 126.7(3) . . ? N3 C16 C15 108.7(3) . . ? C17 C16 C15 124.6(3) . . ? C18 C17 C16 126.9(3) . . ? C18 C17 C39 114.6(3) . . ? C16 C17 C39 118.3(3) . . ? N4 C18 C17 126.2(3) . . ? N4 C18 C19 105.0(3) . . ? C17 C18 C19 128.6(4) . . ? C20 C19 C18 109.2(3) . . ? C19 C20 C1 108.1(4) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 C2 121.9(4) . . ? C22 C21 C2 119.5(4) . . ? C23 C22 C21 121.7(5) . . ? C24 C23 C22 117.9(6) . . ? C25 C24 C23 121.7(5) . . ? C24 C25 C26 120.3(5) . . ? C25 C26 C21 119.8(5) . . ? C32 C27 C28 120.1(4) . . ? C32 C27 C7 119.4(4) . . ? C28 C27 C7 120.5(4) . . ? C27 C28 C29 119.6(5) . . ? C30 C29 C28 119.0(5) . . ? C31 C30 C29 121.3(5) . . ? C30 C31 C32 120.1(5) . . ? C27 C32 C31 119.8(5) . . ? C34 C33 C38 118.4(4) . . ? C34 C33 C12 120.4(4) . . ? C38 C33 C12 121.1(4) . . ? C35 C34 C33 120.5(4) . . ? C36 C35 C34 120.2(4) . . ? C37 C36 C35 120.2(4) . . ? C36 C37 C38 119.7(5) . . ? C37 C38 C33 120.9(4) . . ? C40 C39 C44 119.1(4) . . ? C40 C39 C17 121.7(4) . . ? C44 C39 C17 119.2(4) . . ? C39 C40 C41 120.6(5) . . ? C42 C41 C40 119.3(5) . . ? C43 C42 C41 120.9(4) . . ? C42 C43 C44 120.4(5) . . ? C43 C44 C39 119.6(4) . . ? N5 C45 O1 124.8(5) . . ? N5 C45 O1' 119.3(9) . . ? O1 C45 O1' 50.6(11) . . ? N5 C45 C46 114.6(4) . . ? O1 C45 C46 118.8(4) . . ? O1' C45 C46 111.0(8) . . ? C51 C46 C47 119.4(5) . . ? C51 C46 C45 124.6(5) . . ? C47 C46 C45 115.6(5) . . ? C48 C47 C46 120.9(7) . . ? C49 C48 C47 116.0(7) . . ? C50 C49 C48 126.5(6) . . ? C50 C49 N6 114.4(7) . . ? C48 C49 N6 117.6(7) . . ? C49 C50 C51 115.5(7) . . ? C46 C51 C50 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 1.449 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.091 #===END data_au02m #[Fe(N-p-NCOC6H4NO2-tpp)Cl](compound 5) _database_code_CSD 182282 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H33 Cl4 Fe N6 O3' _chemical_formula_weight 987.49 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 10.0270(11) _cell_length_b 17.2766(18) _cell_length_c 26.645(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4615.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Equant _exptl_crystal_colour Green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9211 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 29828 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11062 _reflns_number_gt 5357 _reflns_threshold_expression >2sigma(I) _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^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment noref _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 -0.040(19) _refine_ls_number_reflns 11062 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.75620(6) 0.42889(3) 0.174507(19) 0.03561(15) Uani 1 1 d . . . Cl1 Cl 0.94790(11) 0.43894(6) 0.13200(4) 0.0544(3) Uani 1 1 d . . . Cl2 Cl 0.4802(2) -0.06475(12) -0.00485(7) 0.1243(7) Uani 1 1 d . . . Cl3 Cl 0.4332(3) -0.15305(13) 0.08395(8) 0.1403(8) Uani 1 1 d . . . Cl4 Cl 0.4820(3) 0.00964(13) 0.09137(8) 0.1622(11) Uani 1 1 d . . . O1 O 0.3762(3) 0.4566(2) 0.10948(11) 0.0610(9) Uani 1 1 d . . . O2 O 0.2352(7) 0.3685(4) 0.3673(2) 0.167(3) Uani 1 1 d . . . O3 O 0.1421(6) 0.4786(4) 0.35348(19) 0.144(2) Uani 1 1 d . . . N1 N 0.7063(3) 0.54605(16) 0.17238(12) 0.0357(8) Uani 1 1 d . . . N2 N 0.7828(3) 0.43386(18) 0.24802(11) 0.0381(8) Uani 1 1 d . . . N3 N 0.7506(3) 0.30873(16) 0.17697(11) 0.0374(7) Uani 1 1 d . . . N4 N 0.6338(3) 0.41922(18) 0.09588(11) 0.0359(8) Uani 1 1 d . . . N5 N 0.5748(3) 0.41516(18) 0.14383(11) 0.0381(8) Uani 1 1 d . . . N6 N 0.2100(6) 0.4253(4) 0.3408(2) 0.0994(18) Uani 1 1 d . . . C1 C 0.7177(4) 0.5955(2) 0.21232(15) 0.0381(10) Uani 1 1 d . . . C2 C 0.7605(4) 0.5749(2) 0.26048(13) 0.0397(9) Uani 1 1 d . . . C3 C 0.7913(4) 0.5002(2) 0.27629(15) 0.0402(11) Uani 1 1 d . . . C4 C 0.8284(5) 0.4781(3) 0.32693(17) 0.0520(12) Uani 1 1 d . . . C5 C 0.8409(5) 0.4009(2) 0.32811(18) 0.0531(12) Uani 1 1 d . . . C6 C 0.8093(4) 0.3709(2) 0.27952(15) 0.0401(11) Uani 1 1 d . . . C7 C 0.8037(4) 0.2935(2) 0.26633(15) 0.0396(10) Uani 1 1 d . . . C8 C 0.7703(4) 0.2650(2) 0.21852(15) 0.0385(10) Uani 1 1 d . . . C9 C 0.7523(5) 0.1842(2) 0.20581(16) 0.0447(10) Uani 1 1 d . . . C10 C 0.7177(4) 0.1811(2) 0.15666(16) 0.0441(11) Uani 1 1 d . . . C11 C 0.7161(4) 0.2590(2) 0.13799(15) 0.0362(10) Uani 1 1 d . . . C12 C 0.6861(4) 0.2789(2) 0.08764(14) 0.0374(10) Uani 1 1 d . . . C13 C 0.6657(4) 0.3533(2) 0.06842(15) 0.0376(10) Uani 1 1 d . . . C14 C 0.6861(5) 0.3789(2) 0.01894(16) 0.0452(11) Uani 1 1 d . . . C15 C 0.6723(5) 0.4584(2) 0.01747(15) 0.0430(11) Uani 1 1 d . . . C16 C 0.6408(4) 0.4847(2) 0.06667(15) 0.0388(10) Uani 1 1 d . . . C17 C 0.6329(4) 0.5627(2) 0.08308(14) 0.0387(10) Uani 1 1 d . . . C18 C 0.6575(4) 0.5886(2) 0.13269(16) 0.0395(10) Uani 1 1 d . . . C19 C 0.6401(5) 0.6680(2) 0.14825(16) 0.0453(11) Uani 1 1 d . . . C20 C 0.6793(4) 0.6717(2) 0.19723(17) 0.0437(11) Uani 1 1 d . . . C21 C 0.7673(5) 0.6382(2) 0.29880(14) 0.0404(10) Uani 1 1 d . . . C22 C 0.6542(5) 0.6675(3) 0.3208(2) 0.0661(15) Uani 1 1 d . . . C23 C 0.6595(6) 0.7269(4) 0.3550(2) 0.0785(18) Uani 1 1 d . . . C24 C 0.7767(7) 0.7583(3) 0.3673(2) 0.0853(19) Uani 1 1 d . . . C25 C 0.8949(6) 0.7309(3) 0.3466(2) 0.086(2) Uani 1 1 d . . . C26 C 0.8875(5) 0.6714(3) 0.3127(2) 0.0673(16) Uani 1 1 d . . . C27 C 0.8230(5) 0.2339(2) 0.30679(15) 0.0408(10) Uani 1 1 d . . . C28 C 0.7151(5) 0.2069(3) 0.33347(19) 0.0637(14) Uani 1 1 d . . . C29 C 0.7317(6) 0.1500(3) 0.36877(19) 0.0712(15) Uani 1 1 d . . . C30 C 0.8555(7) 0.1199(3) 0.37791(18) 0.0616(14) Uani 1 1 d . . . C31 C 0.9625(6) 0.1459(3) 0.35318(19) 0.0611(14) Uani 1 1 d . . . C32 C 0.9487(5) 0.2047(3) 0.31731(17) 0.0556(13) Uani 1 1 d . . . C33 C 0.6831(5) 0.2158(2) 0.04975(16) 0.0421(11) Uani 1 1 d . . . C34 C 0.7926(5) 0.1694(3) 0.04254(17) 0.0547(13) Uani 1 1 d . . . C35 C 0.7918(6) 0.1128(3) 0.0045(2) 0.0694(16) Uani 1 1 d . . . C36 C 0.6797(6) 0.1041(3) -0.02426(19) 0.0643(15) Uani 1 1 d . . . C37 C 0.5711(6) 0.1496(3) -0.01699(18) 0.0603(14) Uani 1 1 d . . . C38 C 0.5741(5) 0.2056(3) 0.01902(16) 0.0497(12) Uani 1 1 d . . . C39 C 0.6031(5) 0.6185(2) 0.04267(15) 0.0411(11) Uani 1 1 d . . . C40 C 0.4903(5) 0.6062(3) 0.01352(18) 0.0552(13) Uani 1 1 d . . . C41 C 0.4640(6) 0.6535(4) -0.02723(19) 0.0764(17) Uani 1 1 d . . . C42 C 0.5503(8) 0.7162(3) -0.0374(2) 0.0776(18) Uani 1 1 d . . . C43 C 0.6566(7) 0.7285(3) -0.0078(2) 0.0769(17) Uani 1 1 d . . . C44 C 0.6839(6) 0.6804(3) 0.03151(18) 0.0580(14) Uani 1 1 d . . . C45 C 0.4419(4) 0.4363(2) 0.14555(15) 0.0383(9) Uani 1 1 d . . . C46 C 0.3839(4) 0.4316(2) 0.19652(15) 0.0398(9) Uani 1 1 d . . . C47 C 0.2628(6) 0.4664(3) 0.20500(18) 0.0692(14) Uani 1 1 d . . . C48 C 0.2032(5) 0.4652(3) 0.2531(2) 0.0782(17) Uani 1 1 d . . . C49 C 0.2698(5) 0.4257(3) 0.28999(17) 0.0682(14) Uani 1 1 d . . . C50 C 0.3871(6) 0.3864(4) 0.28257(19) 0.0765(17) Uani 1 1 d . . . C51 C 0.4460(5) 0.3902(3) 0.23559(17) 0.0577(13) Uani 1 1 d . . . C52 C 0.5186(7) -0.0735(4) 0.0584(2) 0.108(2) Uani 1 1 d . . . H4A H 0.8617 0.5226 0.3479 0.080 Uiso 1 1 d . . . H5A H 0.8551 0.3610 0.3555 0.080 Uiso 1 1 d . . . H9A H 0.7512 0.1460 0.2302 0.080 Uiso 1 1 d . . . H10A H 0.6818 0.1381 0.1371 0.080 Uiso 1 1 d . . . H14A H 0.7189 0.3473 -0.0085 0.080 Uiso 1 1 d . . . H15A H 0.7073 0.4979 -0.0092 0.080 Uiso 1 1 d . . . H19A H 0.6298 0.7147 0.1259 0.080 Uiso 1 1 d . . . H20A H 0.7110 0.7225 0.2156 0.080 Uiso 1 1 d . . . H22A H 0.5731 0.6401 0.3087 0.080 Uiso 1 1 d . . . H23A H 0.5624 0.7372 0.3781 0.080 Uiso 1 1 d . . . H24A H 0.8057 0.7891 0.3925 0.080 Uiso 1 1 d . . . H25A H 0.9940 0.7616 0.3528 0.080 Uiso 1 1 d . . . H26A H 0.9812 0.6530 0.2916 0.080 Uiso 1 1 d . . . H28A H 0.6228 0.2385 0.3268 0.080 Uiso 1 1 d . . . H29A H 0.6654 0.1071 0.3822 0.080 Uiso 1 1 d . . . H30A H 0.8283 0.0707 0.4021 0.080 Uiso 1 1 d . . . H31A H 1.0609 0.1232 0.3570 0.080 Uiso 1 1 d . . . H32A H 1.0168 0.2024 0.2939 0.080 Uiso 1 1 d . . . H34A H 0.8869 0.1819 0.0601 0.080 Uiso 1 1 d . . . H35A H 0.8766 0.0810 -0.0058 0.080 Uiso 1 1 d . . . H36A H 0.6701 0.0743 -0.0522 0.080 Uiso 1 1 d . . . H37A H 0.4953 0.1429 -0.0448 0.080 Uiso 1 1 d . . . H38A H 0.5128 0.2365 0.0282 0.080 Uiso 1 1 d . . . H40A H 0.4291 0.5637 0.0195 0.080 Uiso 1 1 d . . . H41A H 0.3931 0.6538 -0.0507 0.080 Uiso 1 1 d . . . H42A H 0.4975 0.7500 -0.0656 0.080 Uiso 1 1 d . . . H43A H 0.7380 0.7752 -0.0150 0.080 Uiso 1 1 d . . . H44A H 0.7698 0.6998 0.0538 0.080 Uiso 1 1 d . . . H47A H 0.2112 0.4802 0.1717 0.080 Uiso 1 1 d . . . H48A H 0.1210 0.4998 0.2658 0.080 Uiso 1 1 d . . . H50A H 0.4431 0.3721 0.3119 0.080 Uiso 1 1 d . . . H51A H 0.5438 0.3665 0.2280 0.080 Uiso 1 1 d . . . H52A H 0.6364 -0.0801 0.0598 0.080 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0418(3) 0.0328(3) 0.0322(3) -0.0029(3) -0.0017(3) 0.0014(3) Cl1 0.0504(7) 0.0516(7) 0.0610(7) -0.0058(6) 0.0142(6) -0.0024(6) Cl2 0.1573(19) 0.1262(15) 0.0894(12) -0.0046(12) 0.0120(12) -0.0191(16) Cl3 0.166(2) 0.1353(17) 0.1195(16) 0.0133(14) 0.0169(15) -0.0224(16) Cl4 0.238(3) 0.1330(17) 0.1160(16) -0.0354(14) 0.0304(18) -0.0511(19) O1 0.048(2) 0.091(3) 0.0445(19) 0.0089(17) -0.0118(16) 0.0024(17) O2 0.206(7) 0.187(6) 0.108(4) 0.057(4) 0.095(5) 0.011(5) O3 0.148(5) 0.183(5) 0.100(4) -0.029(4) 0.062(4) 0.019(4) N1 0.042(2) 0.0319(17) 0.0330(18) -0.0046(16) -0.0058(16) 0.0013(13) N2 0.044(2) 0.0353(17) 0.0352(18) -0.0058(16) -0.0050(15) 0.0023(17) N3 0.0463(19) 0.0342(16) 0.0319(17) -0.0027(15) -0.0044(19) 0.0007(17) N4 0.047(2) 0.0316(18) 0.0286(18) -0.0050(16) 0.0009(15) 0.0007(16) N5 0.050(2) 0.0353(19) 0.0290(18) -0.0021(15) 0.0054(16) -0.0051(17) N6 0.085(4) 0.141(5) 0.073(4) 0.000(4) 0.035(3) -0.006(4) C1 0.036(3) 0.037(2) 0.041(2) -0.0051(19) -0.0028(19) 0.0054(18) C2 0.048(2) 0.034(2) 0.037(2) -0.0065(19) -0.002(2) -0.004(2) C3 0.041(3) 0.047(3) 0.033(2) -0.007(2) -0.0025(19) 0.001(2) C4 0.065(3) 0.053(3) 0.038(3) -0.008(2) -0.010(2) 0.002(2) C5 0.076(4) 0.044(3) 0.040(3) 0.002(2) -0.008(3) 0.004(2) C6 0.050(3) 0.038(2) 0.032(2) -0.001(2) -0.005(2) 0.008(2) C7 0.045(3) 0.039(2) 0.035(2) 0.005(2) -0.003(2) 0.0033(19) C8 0.041(3) 0.035(2) 0.039(2) 0.0010(18) 0.001(2) 0.000(2) C9 0.045(3) 0.039(2) 0.050(3) 0.0087(19) -0.002(3) 0.002(2) C10 0.046(3) 0.035(2) 0.051(3) -0.006(2) 0.001(2) -0.003(2) C11 0.039(3) 0.034(2) 0.036(2) -0.0043(18) 0.0020(19) 0.0027(18) C12 0.043(3) 0.036(2) 0.033(2) -0.0082(19) 0.0023(19) 0.001(2) C13 0.043(3) 0.034(2) 0.036(2) -0.006(2) -0.002(2) -0.003(2) C14 0.052(3) 0.050(3) 0.034(3) -0.008(2) 0.002(2) -0.002(2) C15 0.052(3) 0.041(2) 0.036(3) -0.004(2) 0.001(2) 0.000(2) C16 0.045(3) 0.037(2) 0.035(2) 0.003(2) 0.000(2) -0.002(2) C17 0.040(3) 0.040(2) 0.036(2) 0.003(2) -0.0001(19) 0.005(2) C18 0.039(3) 0.033(2) 0.046(3) 0.000(2) 0.001(2) -0.0016(19) C19 0.061(3) 0.029(2) 0.045(3) -0.003(2) 0.001(2) 0.008(2) C20 0.049(3) 0.036(2) 0.046(3) -0.002(2) -0.003(2) 0.003(2) C21 0.046(3) 0.043(2) 0.032(2) -0.0040(18) -0.007(2) 0.001(2) C22 0.060(4) 0.073(3) 0.065(4) -0.031(3) -0.003(3) -0.001(3) C23 0.062(4) 0.097(4) 0.077(4) -0.046(4) 0.009(3) 0.017(3) C24 0.104(5) 0.068(4) 0.084(4) -0.047(3) -0.018(4) 0.014(4) C25 0.079(4) 0.082(4) 0.098(5) -0.058(4) -0.015(4) -0.014(3) C26 0.054(3) 0.073(4) 0.075(4) -0.026(3) 0.001(3) 0.003(3) C27 0.044(3) 0.044(2) 0.034(2) -0.0020(19) -0.002(2) 0.005(2) C28 0.056(4) 0.070(3) 0.065(3) 0.016(3) -0.002(3) 0.004(3) C29 0.075(4) 0.073(3) 0.065(3) 0.033(3) 0.003(3) -0.008(3) C30 0.095(5) 0.042(3) 0.048(3) 0.009(2) -0.006(3) -0.008(3) C31 0.068(4) 0.051(3) 0.064(3) 0.009(3) -0.017(3) 0.017(3) C32 0.061(3) 0.063(3) 0.042(3) 0.004(2) 0.004(3) 0.016(3) C33 0.048(3) 0.033(2) 0.044(3) -0.001(2) 0.003(2) -0.003(2) C34 0.062(3) 0.046(3) 0.056(3) -0.011(2) -0.002(2) 0.006(2) C35 0.082(4) 0.056(3) 0.071(4) -0.023(3) 0.025(3) -0.002(3) C36 0.085(4) 0.059(3) 0.049(3) -0.018(3) 0.014(3) -0.023(3) C37 0.070(4) 0.068(3) 0.043(3) -0.016(3) 0.007(3) -0.013(3) C38 0.055(3) 0.056(3) 0.037(3) -0.009(2) -0.002(2) -0.001(2) C39 0.056(3) 0.035(2) 0.032(2) -0.0005(19) -0.001(2) 0.005(2) C40 0.063(4) 0.054(3) 0.048(3) -0.006(2) -0.011(3) -0.003(3) C41 0.092(5) 0.097(4) 0.040(3) -0.001(3) -0.023(3) 0.028(4) C42 0.113(5) 0.069(4) 0.050(4) 0.018(3) 0.001(4) 0.022(4) C43 0.107(5) 0.057(4) 0.067(4) 0.014(3) 0.016(4) -0.003(3) C44 0.077(4) 0.046(3) 0.051(3) 0.003(2) 0.012(3) -0.005(3) C45 0.036(2) 0.042(2) 0.037(2) -0.006(2) -0.002(2) -0.003(2) C46 0.035(2) 0.042(2) 0.042(2) 0.000(2) -0.0023(19) -0.007(2) C47 0.063(4) 0.094(4) 0.051(3) 0.010(3) 0.012(3) 0.007(3) C48 0.060(4) 0.098(4) 0.077(4) 0.000(3) 0.023(3) 0.013(3) C49 0.056(4) 0.102(4) 0.046(3) 0.007(3) 0.014(3) -0.005(4) C50 0.056(4) 0.132(5) 0.042(3) 0.011(3) 0.001(3) -0.006(3) C51 0.050(3) 0.076(3) 0.048(3) 0.011(3) 0.000(3) 0.002(3) C52 0.120(6) 0.124(5) 0.078(4) -0.016(5) 0.002(4) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.979(3) . ? Fe1 N5 2.008(3) . ? Fe1 N3 2.078(3) . ? Fe1 N1 2.086(3) . ? Fe1 Cl1 2.2377(12) . ? Fe1 N4 2.434(3) . ? Cl2 C52 1.736(7) . ? Cl3 C52 1.756(7) . ? Cl4 C52 1.723(7) . ? O1 C45 1.217(4) . ? O2 N6 1.235(7) . ? O3 N6 1.193(7) . ? N1 C1 1.369(5) . ? N1 C18 1.378(5) . ? N2 C3 1.375(5) . ? N2 C6 1.400(5) . ? N3 C8 1.355(5) . ? N3 C11 1.392(5) . ? N4 C16 1.376(5) . ? N4 C13 1.391(5) . ? N4 N5 1.409(4) . ? N5 C45 1.383(5) . ? N6 C49 1.481(7) . ? C1 C2 1.399(5) . ? C1 C20 1.429(5) . ? C2 C3 1.391(5) . ? C2 C21 1.498(5) . ? C3 C4 1.451(6) . ? C4 C5 1.341(6) . ? C5 C6 1.430(6) . ? C6 C7 1.382(5) . ? C7 C8 1.406(5) . ? C7 C27 1.504(5) . ? C8 C9 1.449(5) . ? C9 C10 1.356(6) . ? C10 C11 1.434(5) . ? C11 C12 1.417(5) . ? C12 C13 1.398(5) . ? C12 C33 1.486(5) . ? C13 C14 1.406(6) . ? C14 C15 1.380(5) . ? C15 C16 1.423(5) . ? C16 C17 1.418(5) . ? C17 C18 1.417(5) . ? C17 C39 1.476(5) . ? C18 C19 1.444(5) . ? C19 C20 1.365(5) . ? C21 C22 1.373(6) . ? C21 C26 1.385(6) . ? C22 C23 1.375(7) . ? C23 C24 1.335(8) . ? C24 C25 1.391(8) . ? C25 C26 1.370(7) . ? C27 C28 1.376(6) . ? C27 C32 1.386(6) . ? C28 C29 1.371(6) . ? C29 C30 1.368(7) . ? C30 C31 1.337(7) . ? C31 C32 1.402(6) . ? C33 C34 1.373(6) . ? C33 C38 1.376(6) . ? C34 C35 1.410(6) . ? C35 C36 1.368(8) . ? C36 C37 1.355(7) . ? C37 C38 1.364(6) . ? C39 C44 1.374(6) . ? C39 C40 1.388(6) . ? C40 C41 1.384(7) . ? C41 C42 1.414(8) . ? C42 C43 1.344(8) . ? C43 C44 1.364(7) . ? C45 C46 1.479(5) . ? C46 C47 1.374(6) . ? C46 C51 1.409(6) . ? C47 C48 1.413(7) . ? C48 C49 1.371(7) . ? C49 C50 1.373(7) . ? C50 C51 1.385(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N5 122.02(13) . . ? N2 Fe1 N3 90.90(12) . . ? N5 Fe1 N3 82.55(13) . . ? N2 Fe1 N1 90.98(13) . . ? N5 Fe1 N1 83.48(12) . . ? N3 Fe1 N1 164.59(13) . . ? N2 Fe1 Cl1 112.45(10) . . ? N5 Fe1 Cl1 125.53(9) . . ? N3 Fe1 Cl1 96.69(10) . . ? N1 Fe1 Cl1 96.71(9) . . ? N2 Fe1 N4 157.38(12) . . ? N5 Fe1 N4 35.37(11) . . ? N3 Fe1 N4 86.85(11) . . ? N1 Fe1 N4 85.55(12) . . ? Cl1 Fe1 N4 90.17(8) . . ? C1 N1 C18 107.1(3) . . ? C1 N1 Fe1 124.4(3) . . ? C18 N1 Fe1 128.6(3) . . ? C3 N2 C6 108.0(3) . . ? C3 N2 Fe1 125.9(3) . . ? C6 N2 Fe1 125.8(2) . . ? C8 N3 C11 107.5(3) . . ? C8 N3 Fe1 125.4(2) . . ? C11 N3 Fe1 126.9(2) . . ? C16 N4 C13 111.4(3) . . ? C16 N4 N5 125.1(3) . . ? C13 N4 N5 122.2(3) . . ? C16 N4 Fe1 113.9(2) . . ? C13 N4 Fe1 113.1(2) . . ? N5 N4 Fe1 55.58(17) . . ? C45 N5 N4 114.9(3) . . ? C45 N5 Fe1 145.9(3) . . ? N4 N5 Fe1 89.0(2) . . ? O3 N6 O2 124.7(6) . . ? O3 N6 C49 119.1(7) . . ? O2 N6 C49 116.3(6) . . ? N1 C1 C2 125.4(3) . . ? N1 C1 C20 109.5(3) . . ? C2 C1 C20 125.1(4) . . ? C3 C2 C1 125.6(3) . . ? C3 C2 C21 117.4(3) . . ? C1 C2 C21 117.0(3) . . ? N2 C3 C2 126.4(3) . . ? N2 C3 C4 107.8(3) . . ? C2 C3 C4 125.6(4) . . ? C5 C4 C3 107.9(4) . . ? C4 C5 C6 108.6(4) . . ? C7 C6 N2 126.3(4) . . ? C7 C6 C5 126.1(4) . . ? N2 C6 C5 107.6(3) . . ? C6 C7 C8 125.4(4) . . ? C6 C7 C27 118.4(4) . . ? C8 C7 C27 116.1(3) . . ? N3 C8 C7 125.4(3) . . ? N3 C8 C9 109.2(3) . . ? C7 C8 C9 125.4(4) . . ? C10 C9 C8 107.2(3) . . ? C9 C10 C11 107.6(3) . . ? N3 C11 C12 127.5(3) . . ? N3 C11 C10 108.5(3) . . ? C12 C11 C10 124.0(4) . . ? C13 C12 C11 126.9(3) . . ? C13 C12 C33 115.0(4) . . ? C11 C12 C33 118.0(3) . . ? N4 C13 C12 126.4(4) . . ? N4 C13 C14 105.6(3) . . ? C12 C13 C14 127.7(4) . . ? C15 C14 C13 109.0(4) . . ? C14 C15 C16 108.3(4) . . ? N4 C16 C17 127.2(4) . . ? N4 C16 C15 105.6(3) . . ? C17 C16 C15 126.9(4) . . ? C18 C17 C16 125.3(4) . . ? C18 C17 C39 120.6(4) . . ? C16 C17 C39 114.0(3) . . ? N1 C18 C17 127.6(3) . . ? N1 C18 C19 109.2(3) . . ? C17 C18 C19 123.1(4) . . ? C20 C19 C18 106.5(4) . . ? C19 C20 C1 107.7(4) . . ? C22 C21 C26 116.9(4) . . ? C22 C21 C2 121.4(4) . . ? C26 C21 C2 121.7(4) . . ? C21 C22 C23 121.7(5) . . ? C24 C23 C22 120.0(5) . . ? C23 C24 C25 121.0(4) . . ? C26 C25 C24 118.1(5) . . ? C25 C26 C21 122.3(5) . . ? C28 C27 C32 119.2(4) . . ? C28 C27 C7 120.1(4) . . ? C32 C27 C7 120.7(4) . . ? C29 C28 C27 120.1(5) . . ? C30 C29 C28 120.4(5) . . ? C31 C30 C29 120.8(4) . . ? C30 C31 C32 120.1(5) . . ? C27 C32 C31 119.4(5) . . ? C34 C33 C38 118.5(4) . . ? C34 C33 C12 120.4(4) . . ? C38 C33 C12 121.0(4) . . ? C33 C34 C35 120.1(5) . . ? C36 C35 C34 118.9(5) . . ? C37 C36 C35 121.1(4) . . ? C36 C37 C38 119.6(5) . . ? C37 C38 C33 121.8(5) . . ? C44 C39 C40 118.6(4) . . ? C44 C39 C17 123.1(4) . . ? C40 C39 C17 118.2(4) . . ? C41 C40 C39 120.3(5) . . ? C40 C41 C42 119.1(5) . . ? C43 C42 C41 119.6(5) . . ? C42 C43 C44 120.9(5) . . ? C43 C44 C39 121.4(5) . . ? O1 C45 N5 124.9(4) . . ? O1 C45 C46 121.9(4) . . ? N5 C45 C46 113.3(3) . . ? C47 C46 C51 119.4(4) . . ? C47 C46 C45 118.4(4) . . ? C51 C46 C45 122.2(4) . . ? C46 C47 C48 121.1(5) . . ? C49 C48 C47 116.8(5) . . ? C48 C49 C50 124.1(5) . . ? C48 C49 N6 117.5(5) . . ? C50 C49 N6 118.4(5) . . ? C49 C50 C51 118.2(5) . . ? C50 C51 C46 120.2(5) . . ? Cl4 C52 Cl2 112.0(4) . . ? Cl4 C52 Cl3 110.6(4) . . ? Cl2 C52 Cl3 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.388 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.058