Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #=========================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone 'int+050 918218' _publ_contact_author_fax 'int+050 20237' _publ_contact_author_email 'facal@dcci.unipi.it' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The first crystallographically established bis-qtpy (qtpy = 2,2': 6',2'': 6'',2'''-quaterpyridine) metal complex. ; loop_ _publ_author_name _publ_author_address ; Dell' Amico, Daniela Belli ; ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Calderazzo, Fausto' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Englert, Ulli' ; Institut f\"ur Anorganische Chemie RWTH Professor-Pirlet-Strasse 1 52074 Aachen Germany ; 'Labella, Luca' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Ingegneria Chimica, dei Materiali e delle Materie Prime e Metallurgia Universita'' "La Sapienza" di Roma Via del Castro Laurenziano, 7 I-00185 Roma Italy ; #=========================================================================== data_ll2 _database_code_CSD 156001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Iron-bis(2,2':6',2'':6'',2'''-quaterpyridine) diperchlorate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Fe(N4C20H14)2](ClO4)2' _chemical_formula_sum 'C40 H28 Cl2 Fe N8 O8' _chemical_formula_weight 875.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/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 10.392(3) _cell_length_b 8.867(4) _cell_length_c 40.177(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.39(2) _cell_angle_gamma 90.00 _cell_volume 3701(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18 _cell_measurement_theta_max 24 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Ruby-red' _exptl_crystal_size_max '0.33 mm' _exptl_crystal_size_mid '0.21 mm' _exptl_crystal_size_min '0.10 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 5.178 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ; 37 azimuthal scans in steps of 10 degrees ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 11938 _diffrn_reflns_av_R_equivalents 0.074 _diffrn_reflns_av_sigmaI/netI 0.3962 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 61.94 _reflns_number_total 5730 _reflns_number_gt 1859 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0139P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5730 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2339 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.753 _refine_ls_restrained_S_all 0.753 _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 Fe Fe 0.74123(12) 0.65360(16) 0.12956(3) 0.0382(4) Uani 1 1 d . . . Cl1 Cl 0.1077(3) 0.2951(4) 0.21388(7) 0.0688(9) Uani 1 1 d . . . Cl2 Cl 1.2116(3) 1.0367(4) 0.05163(7) 0.0700(9) Uani 1 1 d . . . O10 O 0.1160(7) 0.1342(9) 0.2124(2) 0.141(4) Uani 1 1 d . . . O11 O -0.0042(6) 0.3316(8) 0.23169(17) 0.097(3) Uani 1 1 d . . . O12 O 0.0974(6) 0.3512(9) 0.18151(17) 0.103(3) Uani 1 1 d . . . O13 O 0.2161(7) 0.3648(11) 0.22956(18) 0.143(4) Uani 1 1 d . . . O20 O 1.1055(7) 1.0986(8) 0.03474(17) 0.100(3) Uani 1 1 d . . . O21 O 1.2831(9) 1.1575(13) 0.0635(3) 0.197(6) Uani 1 1 d . . . O22 O 1.1783(6) 0.9541(9) 0.08021(17) 0.104(3) Uani 1 1 d . . . O23 O 1.2773(11) 0.9545(14) 0.0298(2) 0.232(7) Uani 1 1 d . . . N1 N 0.9121(7) 0.7048(8) 0.16068(17) 0.042(2) Uani 1 1 d . . . N2 N 0.6934(7) 0.5991(8) 0.17849(16) 0.0371(19) Uani 1 1 d . . . N3 N 0.5430(6) 0.5675(7) 0.12658(17) 0.0330(18) Uani 1 1 d . . . N4 N 0.6157(7) 0.4898(8) 0.05581(19) 0.050(2) Uani 1 1 d . . . N5 N 0.8124(7) 0.4044(8) 0.13011(17) 0.044(2) Uani 1 1 d . . . N6 N 0.8601(6) 0.6228(8) 0.08755(16) 0.0335(18) Uani 1 1 d . . . N7 N 0.7183(6) 0.8605(8) 0.09820(15) 0.0364(18) Uani 1 1 d . . . N8 N 0.6089(6) 0.8963(8) 0.15843(19) 0.049(2) Uani 1 1 d . . . C1 C 1.0250(9) 0.7521(9) 0.1494(2) 0.049(3) Uani 1 1 d . . . H1 H 1.0314 0.7660 0.1266 0.058 Uiso 1 1 calc R . . C2 C 1.1331(9) 0.7821(11) 0.1690(3) 0.062(3) Uani 1 1 d . . . H2 H 1.2084 0.8187 0.1600 0.075 Uiso 1 1 calc R . . C3 C 1.1237(10) 0.7551(12) 0.2028(3) 0.072(4) Uani 1 1 d . . . H3 H 1.1939 0.7725 0.2171 0.087 Uiso 1 1 calc R . . C4 C 1.0104(9) 0.7024(11) 0.2151(2) 0.060(3) Uani 1 1 d . . . H4 H 1.0028 0.6829 0.2378 0.072 Uiso 1 1 calc R . . C5 C 0.9077(8) 0.6789(10) 0.1932(2) 0.037(2) Uani 1 1 d . . . C6 C 0.7783(9) 0.6194(10) 0.2037(2) 0.042(3) Uani 1 1 d . . . C7 C 0.7504(10) 0.5881(12) 0.2357(2) 0.066(3) Uani 1 1 d . . . H7 H 0.8115 0.6042 0.2526 0.079 Uiso 1 1 calc R . . C8 C 0.6296(11) 0.5318(12) 0.2430(2) 0.073(4) Uani 1 1 d . . . H8 H 0.6088 0.5067 0.2647 0.087 Uiso 1 1 calc R . . C9 C 0.5430(10) 0.5144(12) 0.2175(3) 0.066(3) Uani 1 1 d . . . H9 H 0.4607 0.4796 0.2219 0.079 Uiso 1 1 calc R . . C10 C 0.5736(9) 0.5463(10) 0.1863(2) 0.042(3) Uani 1 1 d . . . C11 C 0.4895(9) 0.5329(10) 0.1557(2) 0.045(3) Uani 1 1 d . . . C12 C 0.3614(9) 0.4860(12) 0.1576(3) 0.071(3) Uani 1 1 d . . . H12 H 0.3258 0.4646 0.1781 0.085 Uiso 1 1 calc R . . C13 C 0.2891(9) 0.4722(14) 0.1288(3) 0.086(4) Uani 1 1 d . . . H13 H 0.2049 0.4370 0.1293 0.103 Uiso 1 1 calc R . . C14 C 0.3432(9) 0.5114(12) 0.0987(3) 0.074(4) Uani 1 1 d . . . H14 H 0.2939 0.5092 0.0790 0.089 Uiso 1 1 calc R . . C15 C 0.4705(9) 0.5536(10) 0.0982(2) 0.043(3) Uani 1 1 d . . . C16 C 0.5269(8) 0.5860(11) 0.0659(2) 0.041(2) Uani 1 1 d . . . C17 C 0.4889(10) 0.7137(11) 0.0478(2) 0.065(3) Uani 1 1 d . . . H17 H 0.4294 0.7812 0.0562 0.078 Uiso 1 1 calc R . . C18 C 0.5417(10) 0.7369(13) 0.0173(3) 0.075(4) Uani 1 1 d . . . H18 H 0.5155 0.8189 0.0044 0.090 Uiso 1 1 calc R . . C19 C 0.6329(9) 0.6399(14) 0.0057(2) 0.068(4) Uani 1 1 d . . . H19 H 0.6724 0.6550 -0.0145 0.081 Uiso 1 1 calc R . . C20 C 0.6624(8) 0.5190(12) 0.0259(3) 0.058(3) Uani 1 1 d . . . H20 H 0.7213 0.4501 0.0178 0.070 Uiso 1 1 calc R . . C21 C 0.7878(9) 0.3021(11) 0.1523(2) 0.060(3) Uani 1 1 d . . . H21 H 0.7281 0.3253 0.1684 0.072 Uiso 1 1 calc R . . C22 C 0.8466(9) 0.1567(12) 0.1536(2) 0.058(3) Uani 1 1 d . . . H22 H 0.8224 0.0828 0.1686 0.070 Uiso 1 1 calc R . . C23 C 0.9401(10) 0.1344(12) 0.1313(3) 0.072(3) Uani 1 1 d . . . H23 H 0.9865 0.0448 0.1320 0.086 Uiso 1 1 calc R . . C24 C 0.9680(9) 0.2383(12) 0.1079(3) 0.066(3) Uani 1 1 d . . . H24 H 1.0290 0.2176 0.0920 0.079 Uiso 1 1 calc R . . C25 C 0.9040(8) 0.3783(11) 0.1079(2) 0.042(3) Uani 1 1 d . . . C26 C 0.9275(8) 0.4942(11) 0.0839(2) 0.041(3) Uani 1 1 d . . . C27 C 1.0174(8) 0.4817(12) 0.0584(2) 0.055(3) Uani 1 1 d . . . H27 H 1.0655 0.3939 0.0562 0.066 Uiso 1 1 calc R . . C28 C 1.0337(9) 0.5990(12) 0.0370(3) 0.063(3) Uani 1 1 d . . . H28 H 1.0937 0.5913 0.0203 0.076 Uiso 1 1 calc R . . C29 C 0.9626(8) 0.7274(11) 0.0398(2) 0.055(3) Uani 1 1 d . . . H29 H 0.9720 0.8068 0.0250 0.066 Uiso 1 1 calc R . . C30 C 0.8746(7) 0.7369(11) 0.0659(2) 0.037(2) Uani 1 1 d . . . C31 C 0.7922(8) 0.8696(10) 0.0709(2) 0.038(2) Uani 1 1 d . . . C32 C 0.7870(8) 0.9849(12) 0.0486(2) 0.056(3) Uani 1 1 d . . . H32 H 0.8408 0.9861 0.0304 0.067 Uiso 1 1 calc R . . C33 C 0.7018(10) 1.0983(12) 0.0534(2) 0.071(4) Uani 1 1 d . . . H33 H 0.6933 1.1767 0.0381 0.085 Uiso 1 1 calc R . . C34 C 0.6301(8) 1.0942(10) 0.0807(2) 0.048(3) Uani 1 1 d . . . H34 H 0.5743 1.1737 0.0848 0.057 Uiso 1 1 calc R . . C35 C 0.6368(8) 0.9757(11) 0.1029(2) 0.045(3) Uani 1 1 d . . . C36 C 0.5620(8) 0.9743(10) 0.1336(2) 0.038(2) Uani 1 1 d . . . C37 C 0.4492(8) 1.0599(11) 0.1357(2) 0.059(3) Uani 1 1 d . . . H37 H 0.4163 1.1119 0.1173 0.071 Uiso 1 1 calc R . . C38 C 0.3887(9) 1.0651(12) 0.1654(3) 0.064(3) Uani 1 1 d . . . H38 H 0.3131 1.1203 0.1671 0.077 Uiso 1 1 calc R . . C39 C 0.4379(9) 0.9893(12) 0.1932(3) 0.066(3) Uani 1 1 d . . . H39 H 0.3997 0.9946 0.2139 0.079 Uiso 1 1 calc R . . C40 C 0.5485(9) 0.9048(11) 0.1879(2) 0.058(3) Uani 1 1 d . . . H40 H 0.5832 0.8505 0.2058 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0344(8) 0.0446(10) 0.0356(8) 0.0053(9) 0.0019(6) -0.0058(9) Cl1 0.070(2) 0.082(2) 0.0551(18) -0.0009(18) 0.0176(16) -0.0121(18) Cl2 0.072(2) 0.080(2) 0.0589(19) 0.0115(19) 0.0006(17) 0.0115(19) O10 0.139(7) 0.044(6) 0.246(11) 0.022(7) 0.100(7) 0.034(6) O11 0.114(6) 0.064(6) 0.117(6) -0.003(5) 0.078(5) 0.003(5) O12 0.101(6) 0.157(8) 0.052(5) 0.000(6) 0.009(4) -0.071(6) O13 0.100(6) 0.239(12) 0.088(6) 0.025(7) -0.054(5) -0.048(7) O20 0.102(6) 0.113(7) 0.085(6) 0.016(5) -0.021(5) 0.043(5) O21 0.203(10) 0.222(13) 0.161(10) 0.081(10) -0.086(8) -0.149(10) O22 0.124(6) 0.117(7) 0.073(6) 0.048(5) 0.008(5) -0.014(6) O23 0.314(13) 0.286(15) 0.099(8) 0.037(9) 0.076(8) 0.254(12) N1 0.050(5) 0.032(5) 0.045(5) 0.012(4) -0.011(4) -0.013(4) N2 0.050(5) 0.035(5) 0.026(4) 0.003(4) -0.008(4) 0.001(4) N3 0.032(4) 0.025(5) 0.042(5) 0.002(4) -0.004(4) 0.001(4) N4 0.047(5) 0.050(6) 0.054(5) 0.006(5) 0.004(4) 0.004(5) N5 0.054(5) 0.039(5) 0.039(5) 0.014(4) -0.004(4) -0.005(4) N6 0.042(5) 0.025(5) 0.033(4) 0.001(4) -0.006(4) -0.005(4) N7 0.041(4) 0.037(5) 0.031(4) 0.005(4) 0.002(4) -0.002(4) N8 0.053(5) 0.049(6) 0.044(5) 0.010(5) 0.015(4) 0.000(4) C1 0.069(7) 0.022(6) 0.053(7) -0.012(5) -0.021(6) -0.010(6) C2 0.039(6) 0.044(7) 0.104(10) 0.008(7) -0.009(7) -0.001(5) C3 0.060(8) 0.082(9) 0.074(9) 0.003(8) -0.015(7) -0.015(7) C4 0.068(7) 0.066(8) 0.045(6) -0.003(6) -0.029(6) 0.014(7) C5 0.048(6) 0.033(6) 0.031(5) 0.003(5) -0.006(5) 0.011(5) C6 0.073(7) 0.032(6) 0.020(5) -0.007(5) -0.008(5) 0.006(5) C7 0.073(8) 0.082(9) 0.041(6) 0.007(6) -0.018(6) 0.013(7) C8 0.107(10) 0.080(9) 0.031(6) 0.016(7) 0.015(7) 0.008(8) C9 0.078(8) 0.063(8) 0.057(7) 0.021(7) 0.016(7) 0.006(7) C10 0.053(7) 0.035(6) 0.038(6) 0.001(5) -0.007(5) 0.008(5) C11 0.043(6) 0.036(6) 0.058(7) 0.006(6) 0.015(5) 0.004(5) C12 0.035(6) 0.095(10) 0.083(9) -0.004(8) 0.023(6) -0.008(7) C13 0.049(7) 0.132(12) 0.075(9) 0.002(9) -0.014(7) -0.038(7) C14 0.053(7) 0.103(10) 0.065(8) 0.010(8) -0.014(6) -0.017(7) C15 0.051(6) 0.027(6) 0.051(6) 0.003(5) -0.005(6) 0.003(5) C16 0.040(6) 0.037(7) 0.044(6) -0.011(6) -0.012(5) -0.007(5) C17 0.103(9) 0.038(7) 0.053(7) 0.009(6) -0.020(7) -0.002(7) C18 0.090(9) 0.063(9) 0.070(9) 0.026(8) -0.035(7) -0.005(7) C19 0.065(8) 0.101(11) 0.037(6) 0.007(8) 0.001(6) -0.032(8) C20 0.046(6) 0.069(9) 0.060(7) -0.016(7) 0.016(6) -0.008(6) C21 0.077(8) 0.030(7) 0.070(8) 0.000(6) -0.038(6) -0.002(6) C22 0.068(7) 0.040(7) 0.065(8) 0.012(6) -0.011(6) -0.027(7) C23 0.068(8) 0.031(7) 0.116(11) -0.008(8) -0.013(7) 0.008(7) C24 0.057(7) 0.057(9) 0.083(9) -0.006(7) 0.012(6) -0.010(7) C25 0.046(6) 0.030(7) 0.049(6) 0.000(5) 0.004(5) 0.008(5) C26 0.030(5) 0.050(7) 0.043(6) 0.000(6) -0.006(5) -0.010(5) C27 0.047(6) 0.069(9) 0.049(7) -0.001(6) 0.006(5) 0.024(6) C28 0.061(7) 0.062(8) 0.067(8) -0.010(7) 0.012(6) 0.009(7) C29 0.052(6) 0.048(7) 0.066(7) 0.010(6) 0.014(5) 0.014(6) C30 0.029(5) 0.041(7) 0.041(6) -0.013(5) 0.007(5) -0.010(5) C31 0.052(6) 0.029(6) 0.033(5) 0.004(5) 0.002(5) -0.012(5) C32 0.051(7) 0.076(9) 0.042(6) 0.011(6) 0.015(5) 0.005(6) C33 0.094(9) 0.066(9) 0.055(7) 0.018(7) 0.024(7) 0.015(7) C34 0.052(6) 0.032(6) 0.059(7) 0.001(6) 0.001(5) 0.022(5) C35 0.038(6) 0.045(7) 0.050(6) -0.003(6) -0.005(5) 0.003(5) C36 0.039(6) 0.038(6) 0.037(6) -0.003(5) 0.004(5) -0.001(5) C37 0.041(6) 0.078(9) 0.059(7) 0.002(7) 0.000(6) 0.018(6) C38 0.042(7) 0.076(9) 0.074(8) -0.007(7) 0.000(6) 0.008(6) C39 0.063(8) 0.065(9) 0.070(8) -0.015(7) 0.015(7) -0.018(7) C40 0.065(7) 0.059(8) 0.049(7) 0.003(6) -0.008(6) -0.010(6) _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 Fe N2 2.096(6) . ? Fe N6 2.133(7) . ? Fe N1 2.195(7) . ? Fe N3 2.197(6) . ? Fe N7 2.235(7) . ? Fe N5 2.330(8) . ? Cl1 O12 1.394(7) . ? Cl1 O11 1.417(6) . ? Cl1 O13 1.420(7) . ? Cl1 O10 1.431(7) . ? Cl2 O23 1.338(8) . ? Cl2 O21 1.382(9) . ? Cl2 O20 1.394(6) . ? Cl2 O22 1.412(6) . ? N1 C5 1.327(9) . ? N1 C1 1.334(9) . ? N2 C6 1.340(9) . ? N2 C10 1.373(9) . ? N3 C11 1.344(9) . ? N3 C15 1.356(9) . ? N4 C16 1.328(10) . ? N4 C20 1.332(10) . ? N5 C21 1.303(10) . ? N5 C25 1.341(9) . ? N6 C30 1.344(9) . ? N6 C26 1.348(10) . ? N7 C35 1.344(10) . ? N7 C31 1.356(9) . ? N8 C36 1.299(10) . ? N8 C40 1.357(10) . ? C1 C2 1.382(10) . ? C2 C3 1.383(12) . ? C3 C4 1.370(11) . ? C4 C5 1.384(10) . ? C5 C6 1.515(10) . ? C6 C7 1.352(10) . ? C7 C8 1.389(11) . ? C8 C9 1.357(12) . ? C9 C10 1.332(11) . ? C10 C11 1.493(11) . ? C11 C12 1.399(10) . ? C12 C13 1.372(11) . ? C13 C14 1.391(12) . ? C14 C15 1.375(10) . ? C15 C16 1.465(11) . ? C16 C17 1.398(11) . ? C17 C18 1.370(12) . ? C18 C19 1.369(12) . ? C19 C20 1.375(12) . ? C21 C22 1.427(12) . ? C22 C23 1.353(11) . ? C23 C24 1.352(12) . ? C24 C25 1.408(11) . ? C25 C26 1.434(11) . ? C26 C27 1.407(10) . ? C27 C28 1.363(11) . ? C28 C29 1.364(11) . ? C29 C30 1.410(10) . ? C30 C31 1.472(11) . ? C31 C32 1.360(10) . ? C32 C33 1.356(11) . ? C33 C34 1.343(10) . ? C34 C35 1.379(11) . ? C35 C36 1.473(11) . ? C36 C37 1.401(10) . ? C37 C38 1.363(11) . ? C38 C39 1.389(12) . ? C39 C40 1.392(11) . ? 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 Fe N6 150.2(3) . . ? N2 Fe N1 73.8(3) . . ? N6 Fe N1 90.1(3) . . ? N2 Fe N3 74.2(3) . . ? N6 Fe N3 118.2(3) . . ? N1 Fe N3 148.0(3) . . ? N2 Fe N7 133.9(3) . . ? N6 Fe N7 73.4(3) . . ? N1 Fe N7 103.0(2) . . ? N3 Fe N7 99.6(2) . . ? N2 Fe N5 81.7(3) . . ? N6 Fe N5 72.3(3) . . ? N1 Fe N5 86.5(2) . . ? N3 Fe N5 88.2(2) . . ? N7 Fe N5 144.4(3) . . ? O12 Cl1 O11 110.2(5) . . ? O12 Cl1 O13 107.5(5) . . ? O11 Cl1 O13 109.2(5) . . ? O12 Cl1 O10 108.7(6) . . ? O11 Cl1 O10 107.4(5) . . ? O13 Cl1 O10 113.9(6) . . ? O23 Cl2 O21 111.7(8) . . ? O23 Cl2 O20 107.8(6) . . ? O21 Cl2 O20 106.0(6) . . ? O23 Cl2 O22 112.8(6) . . ? O21 Cl2 O22 105.1(6) . . ? O20 Cl2 O22 113.2(5) . . ? C5 N1 C1 116.1(8) . . ? C5 N1 Fe 118.5(6) . . ? C1 N1 Fe 125.3(6) . . ? C6 N2 C10 117.3(8) . . ? C6 N2 Fe 120.8(6) . . ? C10 N2 Fe 121.9(6) . . ? C11 N3 C15 118.6(8) . . ? C11 N3 Fe 116.0(6) . . ? C15 N3 Fe 125.3(6) . . ? C16 N4 C20 114.9(9) . . ? C21 N5 C25 119.4(9) . . ? C21 N5 Fe 126.8(7) . . ? C25 N5 Fe 112.8(6) . . ? C30 N6 C26 119.9(8) . . ? C30 N6 Fe 119.4(6) . . ? C26 N6 Fe 120.5(6) . . ? C35 N7 C31 116.1(8) . . ? C35 N7 Fe 127.1(6) . . ? C31 N7 Fe 116.8(6) . . ? C36 N8 C40 117.9(8) . . ? N1 C1 C2 125.2(9) . . ? C1 C2 C3 116.7(10) . . ? C4 C3 C2 119.7(10) . . ? C3 C4 C5 118.4(9) . . ? N1 C5 C4 123.8(9) . . ? N1 C5 C6 112.8(7) . . ? C4 C5 C6 123.4(8) . . ? N2 C6 C7 122.6(9) . . ? N2 C6 C5 114.1(7) . . ? C7 C6 C5 123.3(8) . . ? C6 C7 C8 119.4(9) . . ? C9 C8 C7 117.8(9) . . ? C10 C9 C8 121.2(10) . . ? C9 C10 N2 121.7(9) . . ? C9 C10 C11 127.5(10) . . ? N2 C10 C11 110.9(8) . . ? N3 C11 C12 122.0(9) . . ? N3 C11 C10 116.8(8) . . ? C12 C11 C10 121.2(9) . . ? C13 C12 C11 118.9(10) . . ? C12 C13 C14 119.2(10) . . ? C15 C14 C13 119.2(10) . . ? N3 C15 C14 121.9(9) . . ? N3 C15 C16 120.0(8) . . ? C14 C15 C16 118.0(9) . . ? N4 C16 C17 123.4(10) . . ? N4 C16 C15 116.1(9) . . ? C17 C16 C15 120.4(10) . . ? C18 C17 C16 118.2(11) . . ? C19 C18 C17 120.4(11) . . ? C18 C19 C20 115.8(10) . . ? N4 C20 C19 127.1(10) . . ? N5 C21 C22 124.3(10) . . ? C23 C22 C21 115.0(10) . . ? C24 C23 C22 122.1(11) . . ? C23 C24 C25 119.4(10) . . ? N5 C25 C24 119.7(9) . . ? N5 C25 C26 117.3(9) . . ? C24 C25 C26 123.0(9) . . ? N6 C26 C27 120.1(9) . . ? N6 C26 C25 115.8(8) . . ? C27 C26 C25 124.0(10) . . ? C28 C27 C26 119.6(10) . . ? C27 C28 C29 120.5(10) . . ? C28 C29 C30 118.3(10) . . ? N6 C30 C29 121.4(9) . . ? N6 C30 C31 116.0(8) . . ? C29 C30 C31 122.6(9) . . ? N7 C31 C32 124.3(9) . . ? N7 C31 C30 113.9(8) . . ? C32 C31 C30 121.7(9) . . ? C33 C32 C31 118.6(9) . . ? C34 C33 C32 118.3(10) . . ? C33 C34 C35 122.0(9) . . ? N7 C35 C34 120.7(8) . . ? N7 C35 C36 117.3(9) . . ? C34 C35 C36 121.9(9) . . ? N8 C36 C37 122.7(9) . . ? N8 C36 C35 116.8(9) . . ? C37 C36 C35 120.4(9) . . ? C38 C37 C36 118.4(10) . . ? C37 C38 C39 121.2(10) . . ? C38 C39 C40 115.3(10) . . ? N8 C40 C39 124.3(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 61.94 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.343 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.072