Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'George Newkome' _publ_contact_author_address ; Department of Polymer Science University of Akron Akron 44325 UNITED STATES OF AMERICA ; _publ_contact_author_email NEWKOME@UAKRON.EDU _publ_section_title ; Design, characterization, and X-ray structure of an interlocked dinuclear chair-like metallomacrocycle: [Fe2II(3,5-bis(2,2':6',2'' -terpyridine-4'-phen-3-yl)toluene)2][4PF6_] ; loop_ _publ_author_name G.Newkome S.Durmus I.Eryazici M.Panzer C.D.Shreiner ; Pingshan Wang ; data_mp _database_code_depnum_ccdc_archive 'CCDC 616653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H68 Fe2 N12, 2(C10 H4 O8), 4(C2 H3 N), 6(O)' _chemical_formula_sum 'C126 H88 Fe2 N16 O22' _chemical_formula_weight 2289.82 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' _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 13.6606(17) _cell_length_b 14.6604(18) _cell_length_c 15.2850(19) _cell_angle_alpha 96.396(2) _cell_angle_beta 98.395(2) _cell_angle_gamma 98.598(2) _cell_volume 2966.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5950 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.41 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8561 _exptl_absorpt_correction_T_max 0.9416 _exptl_absorpt_process_details SADABS _exptl_special_details ; Disordered acetonitrile and water solvent atoms were removed using Platon Squeeze. approx. 96 E/cell were removed from the model. This accounts for the large solvent accessible void in the cif alert. ; _diffrn_ambient_temperature 100(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 25244 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12817 _reflns_number_gt 10037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0782P)^2^+0.3435P] 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 12817 _refine_ls_number_parameters 754 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 0.54551(2) 0.29619(2) 0.68696(2) 0.01691(9) Uani 1 1 d . . . O1 O 0.0594(2) 0.24874(16) 0.55224(19) 0.0744(8) Uani 1 1 d . . . O2 O 0.14731(16) 0.20196(15) 0.66600(14) 0.0515(6) Uani 1 1 d . . . O3 O 0.21384(15) 0.06469(14) 0.69569(13) 0.0438(5) Uani 1 1 d . . . H3A H 0.1803 0.1080 0.6910 0.066 Uiso 1 1 calc R . . O4 O 0.21186(15) -0.07530(14) 0.62582(13) 0.0446(5) Uani 1 1 d . . . O5 O 0.19325(15) 0.72085(14) 1.02220(13) 0.0425(5) Uani 1 1 d . . . H5 H 0.1814 0.6944 0.9692 0.064 Uiso 1 1 calc R . . O6 O 0.13808(14) 0.70256(13) 1.14723(13) 0.0403(5) Uani 1 1 d . . . O7 O 0.15071(16) 0.65162(16) 0.86682(13) 0.0517(6) Uani 1 1 d . . . O8 O 0.02016(14) 0.56118(13) 0.78113(11) 0.0368(4) Uani 1 1 d . . . O9 O 0.05262(15) 0.57270(13) 0.61257(12) 0.0403(5) Uani 1 1 d . . . O10 O 0.10682(14) 0.42607(13) 0.52226(13) 0.0402(5) Uani 1 1 d . . . O11 O 0.50250(19) 0.21001(14) 0.37717(15) 0.0617(7) Uani 1 1 d . . . N1 N 0.58425(14) 0.17768(13) 0.71593(12) 0.0202(4) Uani 1 1 d . . . N2 N 0.45225(13) 0.21378(12) 0.60071(12) 0.0173(4) Uani 1 1 d . . . N3 N 0.47387(13) 0.38753(12) 0.62911(12) 0.0180(4) Uani 1 1 d . . . N4 N 0.46809(13) 0.29494(12) 0.78591(12) 0.0201(4) Uani 1 1 d . . . N5 N 0.63360(13) 0.38434(12) 0.77213(12) 0.0181(4) Uani 1 1 d . . . N6 N 0.65833(14) 0.31950(12) 0.62052(12) 0.0192(4) Uani 1 1 d . . . N7 N 0.3794(2) 0.5169(2) 0.85651(18) 0.0551(7) Uani 1 1 d . . . N8 N 0.8474(2) 0.69561(17) 0.67024(15) 0.0420(6) Uani 1 1 d . . . C1 C 0.65477(17) 0.16654(16) 0.78273(15) 0.0237(5) Uani 1 1 d . . . H1 H 0.6946 0.2202 0.8185 0.028 Uiso 1 1 calc R . . C2 C 0.6713(2) 0.07976(18) 0.80116(16) 0.0309(6) Uani 1 1 d . . . H2 H 0.7215 0.0742 0.8493 0.037 Uiso 1 1 calc R . . C3 C 0.6154(2) 0.00159(18) 0.75008(17) 0.0316(6) Uani 1 1 d . . . H3 H 0.6260 -0.0586 0.7626 0.038 Uiso 1 1 calc R . . C4 C 0.54296(19) 0.01156(17) 0.67971(16) 0.0266(5) Uani 1 1 d . . . H4 H 0.5039 -0.0416 0.6426 0.032 Uiso 1 1 calc R . . C5 C 0.52863(17) 0.10036(15) 0.66448(14) 0.0196(4) Uani 1 1 d . . . C6 C 0.45209(16) 0.12147(14) 0.59530(14) 0.0185(4) Uani 1 1 d . . . C7 C 0.38394(17) 0.05942(15) 0.53211(14) 0.0211(5) Uani 1 1 d . . . H7 H 0.3862 -0.0053 0.5282 0.025 Uiso 1 1 calc R . . C8 C 0.31206(17) 0.09127(15) 0.47412(14) 0.0209(5) Uani 1 1 d . . . C9 C 0.31118(17) 0.18745(15) 0.48399(14) 0.0228(5) Uani 1 1 d . . . H9 H 0.2614 0.2119 0.4480 0.027 Uiso 1 1 calc R . . C10 C 0.38325(16) 0.24660(15) 0.54650(14) 0.0191(4) Uani 1 1 d . . . C11 C 0.39629(17) 0.34858(15) 0.56252(14) 0.0197(5) Uani 1 1 d . . . C12 C 0.33766(18) 0.40185(16) 0.51570(15) 0.0238(5) Uani 1 1 d . . . H12 H 0.2840 0.3729 0.4697 0.029 Uiso 1 1 calc R . . C13 C 0.35784(18) 0.49777(16) 0.53637(16) 0.0264(5) Uani 1 1 d . . . H13 H 0.3175 0.5355 0.5057 0.032 Uiso 1 1 calc R . . C14 C 0.43769(18) 0.53779(16) 0.60246(16) 0.0264(5) Uani 1 1 d . . . H14 H 0.4543 0.6036 0.6167 0.032 Uiso 1 1 calc R . . C15 C 0.49298(17) 0.48074(15) 0.64747(15) 0.0226(5) Uani 1 1 d . . . H15 H 0.5470 0.5088 0.6935 0.027 Uiso 1 1 calc R . . C16 C 0.23995(17) 0.02695(15) 0.40471(14) 0.0213(5) Uani 1 1 d . . . C17 C 0.22429(18) -0.06940(16) 0.40759(15) 0.0250(5) Uani 1 1 d . . . H17 H 0.2595 -0.0938 0.4555 0.030 Uiso 1 1 calc R . . C18 C 0.15824(19) -0.12893(16) 0.34145(16) 0.0280(5) Uani 1 1 d . . . H18 H 0.1491 -0.1941 0.3437 0.034 Uiso 1 1 calc R . . C19 C 0.10510(18) -0.09471(16) 0.27177(15) 0.0263(5) Uani 1 1 d . . . H19 H 0.0596 -0.1366 0.2268 0.032 Uiso 1 1 calc R . . C20 C 0.11784(17) 0.00053(16) 0.26699(15) 0.0229(5) Uani 1 1 d . . . C21 C 0.18663(17) 0.06019(16) 0.33352(15) 0.0231(5) Uani 1 1 d . . . H21 H 0.1973 0.1251 0.3301 0.028 Uiso 1 1 calc R . . C22 C 0.06018(18) 0.03819(15) 0.19299(15) 0.0233(5) Uani 1 1 d . . . C23 C -0.04056(18) 0.00082(16) 0.16318(15) 0.0251(5) Uani 1 1 d . . . H23 H -0.0715 -0.0484 0.1906 0.030 Uiso 1 1 calc R . . C24 C -0.09684(18) 0.03408(17) 0.09399(16) 0.0283(5) Uani 1 1 d . . . C25 C -0.05098(18) 0.10667(16) 0.05512(15) 0.0257(5) Uani 1 1 d . . . H25 H -0.0886 0.1294 0.0074 0.031 Uiso 1 1 calc R . . C26 C 0.04929(18) 0.14681(15) 0.08485(15) 0.0236(5) Uani 1 1 d . . . C27 C 0.10444(17) 0.11191(15) 0.15348(15) 0.0225(5) Uani 1 1 d . . . H27 H 0.1729 0.1384 0.1737 0.027 Uiso 1 1 calc R . . C28 C -0.2059(2) -0.00782(19) 0.0631(2) 0.0382(7) Uani 1 1 d . . . H28A H -0.2381 0.0324 0.0250 0.057 Uiso 1 1 calc R . . H28B H -0.2396 -0.0135 0.1151 0.057 Uiso 1 1 calc R . . H28C H -0.2108 -0.0696 0.0293 0.057 Uiso 1 1 calc R . . C29 C 0.09506(17) 0.22599(15) 0.04335(15) 0.0224(5) Uani 1 1 d . . . C30 C 0.07744(18) 0.22576(16) -0.04842(15) 0.0251(5) Uani 1 1 d . . . H30 H 0.0352 0.1741 -0.0852 0.030 Uiso 1 1 calc R . . C31 C 0.38182(16) 0.23828(16) 0.78777(15) 0.0223(5) Uani 1 1 d . . . H31 H 0.3488 0.1992 0.7347 0.027 Uiso 1 1 calc R . . C32 C 0.33972(18) 0.23492(17) 0.86390(16) 0.0277(5) Uani 1 1 d . . . H32 H 0.2782 0.1945 0.8628 0.033 Uiso 1 1 calc R . . C33 C 0.38708(18) 0.29038(17) 0.94202(16) 0.0268(5) Uani 1 1 d . . . H33 H 0.3597 0.2877 0.9955 0.032 Uiso 1 1 calc R . . C34 C 0.47550(17) 0.35010(16) 0.94067(15) 0.0234(5) Uani 1 1 d . . . H34 H 0.5093 0.3898 0.9932 0.028 Uiso 1 1 calc R . . C35 C 0.51373(16) 0.35112(15) 0.86211(14) 0.0197(5) Uani 1 1 d . . . C36 C 0.60662(16) 0.41025(15) 0.85162(14) 0.0190(4) Uani 1 1 d . . . C37 C 0.66181(16) 0.48536(15) 0.90932(14) 0.0205(5) Uani 1 1 d . . . H37 H 0.6429 0.5022 0.9656 0.025 Uiso 1 1 calc R . . C38 C 0.74575(16) 0.53666(15) 0.88457(14) 0.0199(5) Uani 1 1 d . . . C39 C 0.77386(16) 0.50691(15) 0.80332(14) 0.0199(5) Uani 1 1 d . . . H39 H 0.8312 0.5398 0.7853 0.024 Uiso 1 1 calc R . . C40 C 0.71774(16) 0.42950(15) 0.74948(14) 0.0187(4) Uani 1 1 d . . . C41 C 0.73625(16) 0.38561(15) 0.66396(14) 0.0189(4) Uani 1 1 d . . . C42 C 0.82536(17) 0.40526(16) 0.63070(15) 0.0228(5) Uani 1 1 d . . . H42 H 0.8783 0.4521 0.6621 0.027 Uiso 1 1 calc R . . C43 C 0.83565(18) 0.35566(16) 0.55143(16) 0.0257(5) Uani 1 1 d . . . H43 H 0.8964 0.3668 0.5281 0.031 Uiso 1 1 calc R . . C44 C 0.75638(19) 0.28957(16) 0.50648(15) 0.0251(5) Uani 1 1 d . . . H44 H 0.7616 0.2552 0.4514 0.030 Uiso 1 1 calc R . . C45 C 0.66931(18) 0.27401(15) 0.54249(14) 0.0224(5) Uani 1 1 d . . . H45 H 0.6148 0.2291 0.5105 0.027 Uiso 1 1 calc R . . C46 C 0.80464(16) 0.62020(15) 0.94244(15) 0.0199(5) Uani 1 1 d . . . C47 C 0.82116(17) 0.62376(16) 1.03504(15) 0.0221(5) Uani 1 1 d . . . H47 H 0.7921 0.5733 1.0620 0.026 Uiso 1 1 calc R . . C48 C 0.88011(17) 0.70107(16) 1.08725(15) 0.0237(5) Uani 1 1 d . . . H48 H 0.8914 0.7038 1.1504 0.028 Uiso 1 1 calc R . . C49 C 0.84622(16) 0.69567(15) 0.90445(15) 0.0212(5) Uani 1 1 d . . . H49 H 0.8342 0.6936 0.8414 0.025 Uiso 1 1 calc R . . C50 C 0.04849(19) 0.08682(19) 0.54813(17) 0.0333(6) Uani 1 1 d . . . C51 C 0.08540(19) 0.00574(18) 0.56669(16) 0.0311(6) Uani 1 1 d . . . C52 C 0.03583(19) -0.07824(19) 0.51766(17) 0.0338(6) Uani 1 1 d . . . H52 H 0.0610 -0.1333 0.5298 0.041 Uiso 1 1 calc R . . C53 C 0.0879(2) 0.1865(2) 0.5907(2) 0.0458(7) Uani 1 1 d . . . C54 C 0.1766(2) -0.0031(2) 0.63364(17) 0.0345(6) Uani 1 1 d . . . C55 C 0.02552(17) 0.53481(16) 1.08679(15) 0.0229(5) Uani 1 1 d . . . H55 H 0.0434 0.5595 1.1482 0.028 Uiso 1 1 calc R . . C56 C 0.06598(17) 0.58598(16) 1.02593(15) 0.0226(5) Uani 1 1 d . . . C57 C 0.03884(17) 0.54928(16) 0.93492(15) 0.0232(5) Uani 1 1 d . . . C58 C 0.13544(18) 0.67549(17) 1.06941(17) 0.0282(5) Uani 1 1 d . . . C59 C 0.07187(19) 0.59114(18) 0.85490(17) 0.0306(6) Uani 1 1 d . . . C60 C 0.3146(2) 0.4828(2) 0.80185(19) 0.0400(7) Uani 1 1 d . . . C61 C 0.2311(2) 0.4377(2) 0.73244(19) 0.0445(7) Uani 1 1 d . . . H61A H 0.2330 0.3709 0.7217 0.067 Uiso 1 1 calc R . . H61B H 0.2368 0.4649 0.6772 0.067 Uiso 1 1 calc R . . H61C H 0.1676 0.4471 0.7517 0.067 Uiso 1 1 calc R . . C62 C 0.9292(2) 0.72928(19) 0.68250(17) 0.0352(6) Uani 1 1 d . . . C63 C 1.0349(2) 0.7743(2) 0.6991(2) 0.0454(7) Uani 1 1 d . . . H63A H 1.0389 0.8420 0.7105 0.068 Uiso 1 1 calc R . . H63B H 1.0658 0.7584 0.6467 0.068 Uiso 1 1 calc R . . H63C H 1.0705 0.7526 0.7512 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01721(17) 0.01230(16) 0.01840(16) 0.00116(12) -0.00178(12) -0.00127(12) O1 0.0807(18) 0.0310(13) 0.0914(19) 0.0027(12) -0.0311(15) -0.0062(12) O2 0.0419(12) 0.0442(13) 0.0528(13) -0.0142(10) -0.0120(10) -0.0081(10) O3 0.0379(11) 0.0469(13) 0.0376(11) 0.0003(9) -0.0053(9) -0.0068(9) O4 0.0407(12) 0.0419(12) 0.0459(12) 0.0114(10) -0.0066(9) -0.0005(10) O5 0.0410(11) 0.0355(11) 0.0408(11) 0.0092(9) -0.0068(9) -0.0156(9) O6 0.0380(11) 0.0322(11) 0.0416(11) -0.0088(8) -0.0005(9) -0.0066(8) O7 0.0436(12) 0.0625(15) 0.0395(11) 0.0166(10) -0.0001(9) -0.0219(10) O8 0.0377(11) 0.0435(11) 0.0263(9) 0.0085(8) 0.0023(8) -0.0024(9) O9 0.0515(12) 0.0379(11) 0.0328(10) 0.0077(8) 0.0066(9) 0.0104(9) O10 0.0360(11) 0.0396(11) 0.0415(11) -0.0026(9) 0.0028(9) 0.0043(9) O11 0.0842(17) 0.0298(11) 0.0559(14) 0.0042(10) -0.0247(12) -0.0022(11) N1 0.0202(10) 0.0178(9) 0.0206(9) 0.0011(7) 0.0008(7) 0.0004(7) N2 0.0179(9) 0.0129(9) 0.0197(9) 0.0020(7) 0.0002(7) 0.0010(7) N3 0.0179(9) 0.0133(9) 0.0207(9) 0.0022(7) -0.0001(7) -0.0013(7) N4 0.0179(9) 0.0152(9) 0.0249(9) 0.0024(7) -0.0018(8) 0.0006(7) N5 0.0173(9) 0.0155(9) 0.0202(9) 0.0040(7) 0.0003(7) 0.0005(7) N6 0.0237(10) 0.0136(9) 0.0194(9) 0.0033(7) -0.0006(7) 0.0034(7) N7 0.0525(17) 0.0606(19) 0.0515(16) 0.0150(14) -0.0049(14) 0.0151(14) N8 0.0535(16) 0.0374(14) 0.0307(12) -0.0001(10) -0.0053(11) 0.0086(12) C1 0.0228(12) 0.0225(12) 0.0229(11) 0.0024(9) -0.0030(9) 0.0018(9) C2 0.0326(14) 0.0291(14) 0.0287(12) 0.0090(10) -0.0071(11) 0.0061(11) C3 0.0405(15) 0.0215(13) 0.0323(13) 0.0073(10) -0.0018(11) 0.0086(11) C4 0.0317(13) 0.0186(12) 0.0269(12) 0.0049(10) -0.0020(10) 0.0012(10) C5 0.0207(11) 0.0187(11) 0.0183(10) 0.0028(9) 0.0012(8) 0.0017(9) C6 0.0213(11) 0.0127(10) 0.0201(10) 0.0027(8) 0.0012(9) -0.0001(8) C7 0.0264(12) 0.0141(11) 0.0211(11) 0.0019(9) 0.0024(9) 0.0001(9) C8 0.0232(12) 0.0177(11) 0.0196(11) 0.0011(9) 0.0007(9) 0.0000(9) C9 0.0249(12) 0.0182(11) 0.0213(11) 0.0003(9) -0.0041(9) 0.0008(9) C10 0.0192(11) 0.0151(11) 0.0219(11) 0.0038(9) 0.0009(9) 0.0008(9) C11 0.0215(11) 0.0151(11) 0.0196(10) -0.0011(8) -0.0004(9) 0.0008(9) C12 0.0252(12) 0.0179(11) 0.0257(12) 0.0019(9) -0.0027(9) 0.0028(9) C13 0.0302(13) 0.0170(11) 0.0304(12) 0.0040(10) -0.0022(10) 0.0048(10) C14 0.0318(13) 0.0139(11) 0.0316(13) 0.0032(9) 0.0008(10) 0.0016(10) C15 0.0224(12) 0.0163(11) 0.0263(12) -0.0002(9) 0.0007(9) -0.0007(9) C16 0.0247(12) 0.0141(11) 0.0215(11) -0.0006(9) -0.0022(9) -0.0005(9) C17 0.0302(13) 0.0179(12) 0.0234(11) 0.0040(9) -0.0033(10) -0.0001(10) C18 0.0365(14) 0.0134(11) 0.0294(12) 0.0029(9) -0.0034(10) -0.0018(10) C19 0.0293(13) 0.0168(12) 0.0264(12) -0.0003(9) -0.0076(10) -0.0025(10) C20 0.0244(12) 0.0177(11) 0.0235(11) 0.0011(9) -0.0009(9) -0.0004(9) C21 0.0279(12) 0.0139(11) 0.0238(11) 0.0002(9) -0.0020(9) 0.0001(9) C22 0.0275(12) 0.0150(11) 0.0235(11) -0.0033(9) -0.0027(9) 0.0015(9) C23 0.0281(13) 0.0153(11) 0.0280(12) 0.0014(9) -0.0008(10) -0.0019(9) C24 0.0256(13) 0.0214(12) 0.0331(13) 0.0031(10) -0.0055(10) -0.0011(10) C25 0.0262(12) 0.0187(12) 0.0274(12) 0.0034(9) -0.0085(10) 0.0010(9) C26 0.0265(12) 0.0156(11) 0.0253(11) -0.0004(9) -0.0019(9) 0.0012(9) C27 0.0235(12) 0.0145(11) 0.0237(11) -0.0026(9) -0.0058(9) -0.0024(9) C28 0.0283(14) 0.0303(15) 0.0501(16) 0.0145(12) -0.0098(12) -0.0043(11) C29 0.0203(11) 0.0168(11) 0.0268(11) 0.0030(9) -0.0048(9) 0.0013(9) C30 0.0267(12) 0.0173(12) 0.0262(12) -0.0030(9) -0.0046(10) 0.0008(9) C31 0.0184(11) 0.0191(11) 0.0270(12) 0.0022(9) 0.0003(9) -0.0002(9) C32 0.0208(12) 0.0231(13) 0.0371(13) 0.0050(10) 0.0033(10) -0.0019(10) C33 0.0253(12) 0.0262(13) 0.0304(12) 0.0077(10) 0.0081(10) 0.0030(10) C34 0.0250(12) 0.0203(12) 0.0239(11) 0.0024(9) 0.0020(9) 0.0032(9) C35 0.0188(11) 0.0170(11) 0.0220(11) 0.0036(9) -0.0002(9) 0.0020(9) C36 0.0175(11) 0.0183(11) 0.0197(10) 0.0045(9) -0.0019(8) 0.0015(9) C37 0.0220(11) 0.0188(11) 0.0202(11) 0.0026(9) 0.0018(9) 0.0034(9) C38 0.0204(11) 0.0159(11) 0.0214(11) 0.0037(9) -0.0026(9) 0.0013(9) C39 0.0191(11) 0.0163(11) 0.0234(11) 0.0051(9) 0.0008(9) 0.0009(9) C40 0.0176(11) 0.0163(11) 0.0207(10) 0.0056(9) -0.0015(8) -0.0001(8) C41 0.0189(11) 0.0151(11) 0.0220(11) 0.0052(9) -0.0008(9) 0.0021(8) C42 0.0247(12) 0.0163(11) 0.0260(11) 0.0050(9) 0.0029(9) -0.0011(9) C43 0.0254(12) 0.0245(12) 0.0297(12) 0.0094(10) 0.0084(10) 0.0046(10) C44 0.0354(14) 0.0203(12) 0.0210(11) 0.0030(9) 0.0077(10) 0.0056(10) C45 0.0282(12) 0.0159(11) 0.0207(11) 0.0018(9) -0.0014(9) 0.0017(9) C46 0.0167(11) 0.0157(11) 0.0255(11) 0.0008(9) -0.0002(9) 0.0021(8) C47 0.0207(11) 0.0215(12) 0.0227(11) 0.0035(9) 0.0005(9) 0.0020(9) C48 0.0263(12) 0.0216(12) 0.0202(11) -0.0005(9) -0.0011(9) 0.0019(9) C49 0.0205(11) 0.0192(11) 0.0211(11) 0.0014(9) -0.0035(9) 0.0021(9) C50 0.0300(14) 0.0331(15) 0.0299(13) -0.0029(11) 0.0036(11) -0.0101(11) C51 0.0286(13) 0.0320(14) 0.0288(13) 0.0030(11) 0.0039(10) -0.0054(11) C52 0.0304(14) 0.0343(15) 0.0331(14) 0.0043(11) 0.0024(11) -0.0030(11) C53 0.0419(17) 0.0332(16) 0.0525(18) -0.0031(14) -0.0047(14) -0.0058(13) C54 0.0311(14) 0.0358(16) 0.0321(14) 0.0066(12) 0.0018(11) -0.0073(12) C55 0.0206(11) 0.0242(12) 0.0226(11) 0.0021(9) -0.0019(9) 0.0056(9) C56 0.0197(11) 0.0173(11) 0.0275(12) 0.0034(9) -0.0059(9) 0.0018(9) C57 0.0181(11) 0.0225(12) 0.0284(12) 0.0064(10) -0.0013(9) 0.0043(9) C58 0.0225(12) 0.0217(12) 0.0354(14) 0.0048(11) -0.0082(10) -0.0006(10) C59 0.0270(13) 0.0326(14) 0.0308(13) 0.0089(11) 0.0008(10) 0.0005(11) C60 0.0479(18) 0.0411(17) 0.0372(15) 0.0141(13) 0.0105(14) 0.0175(14) C61 0.0535(19) 0.0431(18) 0.0353(15) 0.0072(13) 0.0063(13) 0.0032(14) C62 0.0537(19) 0.0273(14) 0.0248(13) 0.0025(11) 0.0037(12) 0.0106(13) C63 0.0538(19) 0.0323(16) 0.0492(17) 0.0004(13) 0.0163(15) 0.0009(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.8749(17) . ? Fe1 N5 1.8751(18) . ? Fe1 N4 1.9682(19) . ? Fe1 N1 1.9678(19) . ? Fe1 N6 1.9749(19) . ? Fe1 N3 1.9840(18) . ? O1 C53 1.220(4) . ? O2 C53 1.285(3) . ? O3 C54 1.282(3) . ? O4 C54 1.228(3) . ? O5 C58 1.305(3) . ? O6 C58 1.205(3) . ? O7 C59 1.265(3) . ? O8 C59 1.236(3) . ? N1 C1 1.340(3) . ? N1 C5 1.360(3) . ? N2 C10 1.343(3) . ? N2 C6 1.346(3) . ? N3 C15 1.342(3) . ? N3 C11 1.364(3) . ? N4 C31 1.342(3) . ? N4 C35 1.358(3) . ? N5 C40 1.349(3) . ? N5 C36 1.351(3) . ? N6 C45 1.340(3) . ? N6 C41 1.362(3) . ? N7 C60 1.136(4) . ? N8 C62 1.132(4) . ? C1 C2 1.377(3) . ? C2 C3 1.368(4) . ? C3 C4 1.387(3) . ? C4 C5 1.385(3) . ? C5 C6 1.468(3) . ? C6 C7 1.384(3) . ? C7 C8 1.394(3) . ? C8 C9 1.403(3) . ? C8 C16 1.476(3) . ? C9 C10 1.385(3) . ? C10 C11 1.467(3) . ? C11 C12 1.381(3) . ? C12 C13 1.383(3) . ? C13 C14 1.382(3) . ? C14 C15 1.382(3) . ? C16 C21 1.395(3) . ? C16 C17 1.403(3) . ? C17 C18 1.378(3) . ? C18 C19 1.384(3) . ? C19 C20 1.393(3) . ? C20 C21 1.400(3) . ? C20 C22 1.488(3) . ? C22 C23 1.392(3) . ? C22 C27 1.398(3) . ? C23 C24 1.392(3) . ? C24 C25 1.389(3) . ? C24 C28 1.508(3) . ? C25 C26 1.395(3) . ? C26 C27 1.391(3) . ? C26 C29 1.484(3) . ? C29 C30 1.388(3) . ? C29 C49 1.390(3) 2_666 ? C30 C48 1.377(3) 2_666 ? C31 C32 1.374(3) . ? C32 C33 1.381(3) . ? C33 C34 1.386(3) . ? C34 C35 1.378(3) . ? C35 C36 1.466(3) . ? C36 C37 1.378(3) . ? C37 C38 1.398(3) . ? C38 C39 1.396(3) . ? C38 C46 1.478(3) . ? C39 C40 1.379(3) . ? C40 C41 1.464(3) . ? C41 C42 1.390(3) . ? C42 C43 1.379(3) . ? C43 C44 1.380(3) . ? C44 C45 1.381(3) . ? C46 C49 1.391(3) . ? C46 C47 1.394(3) . ? C47 C48 1.381(3) . ? C48 C30 1.377(3) 2_666 ? C49 C29 1.390(3) 2_666 ? C50 C52 1.394(4) 2_556 ? C50 C51 1.400(4) . ? C50 C53 1.516(4) . ? C51 C52 1.390(4) . ? C51 C54 1.523(4) . ? C52 C50 1.394(4) 2_556 ? C55 C57 1.379(3) 2_567 ? C55 C56 1.384(3) . ? C56 C57 1.409(3) . ? C56 C58 1.521(3) . ? C57 C55 1.379(3) 2_567 ? C57 C59 1.524(3) . ? C60 C61 1.458(4) . ? C62 C63 1.467(4) . ? 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 176.37(8) . . ? N2 Fe1 N4 98.42(8) . . ? N5 Fe1 N4 80.63(8) . . ? N2 Fe1 N1 80.73(8) . . ? N5 Fe1 N1 102.71(8) . . ? N4 Fe1 N1 88.32(8) . . ? N2 Fe1 N6 100.47(8) . . ? N5 Fe1 N6 80.72(8) . . ? N4 Fe1 N6 160.80(7) . . ? N1 Fe1 N6 91.32(8) . . ? N2 Fe1 N3 80.75(7) . . ? N5 Fe1 N3 95.79(7) . . ? N4 Fe1 N3 93.90(8) . . ? N1 Fe1 N3 161.48(7) . . ? N6 Fe1 N3 92.52(7) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Fe1 126.65(16) . . ? C5 N1 Fe1 114.86(14) . . ? C10 N2 C6 119.98(18) . . ? C10 N2 Fe1 119.95(15) . . ? C6 N2 Fe1 120.02(14) . . ? C15 N3 C11 117.64(19) . . ? C15 N3 Fe1 128.04(15) . . ? C11 N3 Fe1 114.32(14) . . ? C31 N4 C35 118.15(19) . . ? C31 N4 Fe1 126.59(15) . . ? C35 N4 Fe1 114.89(14) . . ? C40 N5 C36 120.28(18) . . ? C40 N5 Fe1 119.44(14) . . ? C36 N5 Fe1 119.79(15) . . ? C45 N6 C41 117.61(19) . . ? C45 N6 Fe1 127.78(15) . . ? C41 N6 Fe1 114.43(14) . . ? N1 C1 C2 122.0(2) . . ? C3 C2 C1 120.0(2) . . ? C2 C3 C4 118.9(2) . . ? C5 C4 C3 118.8(2) . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 113.29(19) . . ? C4 C5 C6 124.9(2) . . ? N2 C6 C7 120.96(19) . . ? N2 C6 C5 111.07(18) . . ? C7 C6 C5 127.9(2) . . ? C6 C7 C8 120.5(2) . . ? C7 C8 C9 117.3(2) . . ? C7 C8 C16 121.7(2) . . ? C9 C8 C16 121.1(2) . . ? C10 C9 C8 119.7(2) . . ? N2 C10 C9 121.5(2) . . ? N2 C10 C11 111.64(18) . . ? C9 C10 C11 126.9(2) . . ? N3 C11 C12 122.1(2) . . ? N3 C11 C10 113.27(18) . . ? C12 C11 C10 124.7(2) . . ? C11 C12 C13 119.4(2) . . ? C14 C13 C12 118.8(2) . . ? C15 C14 C13 119.0(2) . . ? N3 C15 C14 123.0(2) . . ? C21 C16 C17 118.1(2) . . ? C21 C16 C8 120.8(2) . . ? C17 C16 C8 121.0(2) . . ? C18 C17 C16 120.5(2) . . ? C17 C18 C19 120.6(2) . . ? C18 C19 C20 120.6(2) . . ? C19 C20 C21 118.3(2) . . ? C19 C20 C22 121.0(2) . . ? C21 C20 C22 120.7(2) . . ? C16 C21 C20 121.8(2) . . ? C23 C22 C27 118.9(2) . . ? C23 C22 C20 119.7(2) . . ? C27 C22 C20 121.4(2) . . ? C24 C23 C22 121.3(2) . . ? C25 C24 C23 118.8(2) . . ? C25 C24 C28 121.1(2) . . ? C23 C24 C28 120.1(2) . . ? C24 C25 C26 121.2(2) . . ? C27 C26 C25 119.1(2) . . ? C27 C26 C29 121.2(2) . . ? C25 C26 C29 119.7(2) . . ? C26 C27 C22 120.7(2) . . ? C30 C29 C49 117.9(2) . 2_666 ? C30 C29 C26 121.1(2) . . ? C49 C29 C26 121.0(2) 2_666 . ? C48 C30 C29 121.3(2) 2_666 . ? N4 C31 C32 122.2(2) . . ? C31 C32 C33 119.8(2) . . ? C32 C33 C34 118.5(2) . . ? C35 C34 C33 119.1(2) . . ? N4 C35 C34 122.2(2) . . ? N4 C35 C36 113.15(19) . . ? C34 C35 C36 124.6(2) . . ? N5 C36 C37 120.9(2) . . ? N5 C36 C35 110.74(18) . . ? C37 C36 C35 128.3(2) . . ? C36 C37 C38 119.6(2) . . ? C39 C38 C37 118.4(2) . . ? C39 C38 C46 120.0(2) . . ? C37 C38 C46 121.6(2) . . ? C40 C39 C38 119.5(2) . . ? N5 C40 C39 121.1(2) . . ? N5 C40 C41 110.96(18) . . ? C39 C40 C41 127.9(2) . . ? N6 C41 C42 122.2(2) . . ? N6 C41 C40 113.32(19) . . ? C42 C41 C40 124.4(2) . . ? C43 C42 C41 118.9(2) . . ? C42 C43 C44 119.1(2) . . ? C43 C44 C45 119.2(2) . . ? N6 C45 C44 122.9(2) . . ? C49 C46 C47 119.2(2) . . ? C49 C46 C38 119.9(2) . . ? C47 C46 C38 120.8(2) . . ? C48 C47 C46 119.6(2) . . ? C30 C48 C47 120.4(2) 2_666 . ? C29 C49 C46 121.5(2) 2_666 . ? C52 C50 C51 118.1(2) 2_556 . ? C52 C50 C53 113.2(3) 2_556 . ? C51 C50 C53 128.7(2) . . ? C52 C51 C50 117.7(2) . . ? C52 C51 C54 114.2(2) . . ? C50 C51 C54 128.1(2) . . ? C51 C52 C50 124.2(3) . 2_556 ? O1 C53 O2 122.8(3) . . ? O1 C53 C50 117.9(3) . . ? O2 C53 C50 119.2(3) . . ? O4 C54 O3 122.4(3) . . ? O4 C54 C51 118.4(2) . . ? O3 C54 C51 119.2(3) . . ? C57 C55 C56 125.0(2) 2_567 . ? C55 C56 C57 117.3(2) . . ? C55 C56 C58 113.3(2) . . ? C57 C56 C58 129.4(2) . . ? C55 C57 C56 117.7(2) 2_567 . ? C55 C57 C59 114.3(2) 2_567 . ? C56 C57 C59 128.0(2) . . ? O6 C58 O5 120.8(2) . . ? O6 C58 C56 119.8(2) . . ? O5 C58 C56 119.3(2) . . ? O8 C59 O7 124.0(2) . . ? O8 C59 C57 116.9(2) . . ? O7 C59 C57 119.1(2) . . ? N7 C60 C61 179.1(3) . . ? N8 C62 C63 179.1(3) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.005 0.324 0.717 9.0 0.0 2 0.005 0.676 0.283 9.0 0.3 3 0.500 1.000 1.000 441.4 95.8 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.620 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.069