data_publication_text _journal_name_full 'Dalton Trans.' #TrackingRef '- 2-RT& LT.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matthew P. Shores' _publ_title ; Anion-Dependent Spin State Switching Properties of [(H2bip)2Fe(6-Mebpy)]X2 ; _publ_contact_author_address ;Department of Chemistry Colorado State University Fort Collins, CO 80521 ; _publ_contact_author_email shores@lamar.colostate.edu _publ_contact_author_phone 011(970)4916033 _publ_contact_author_fax 011(970)4911801 loop_ _publ_author_name _publ_author_address Z.Ni ;Department of Chemistry Colorado State University Fort Collins, CO 80521 ; M.P.Shores ;Department of Chemistry Colorado State University Fort Collins, CO 80521 ; data_2-LT _database_code_depnum_ccdc_archive 'CCDC 789130' #TrackingRef '- 2-RT& LT.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Fe N10, 2(C24 H20 B)' _chemical_formula_sum 'C75 H78 B2 Fe N10' _chemical_formula_weight 1196.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.3141(6) _cell_length_b 14.5564(3) _cell_length_c 36.7535(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.2620(10) _cell_angle_gamma 90.00 _cell_volume 12343.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9802 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 30.53 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; Responding to errors on checkcif: A: Large non-solvent C Ueq(max)/Ueq(min)...4.72 Ratio. B: Isotropic non-H atoms in Main residue(s)...1. B: Large non-solvent H Ueq(max)/Ueq(min)...4.60 Ratio. our reply: The positional disordered methyl group at the 2-position of 2,2'-Bipyridine has a ratio 0.73:0.27. Due to the partial occupancy, the disordered C27B has a large displacement parameter (Ueq = 0.077). We refine the disorder atoms with isotropic displacement parameters. ; _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 76031 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.57 _reflns_number_total 18930 _reflns_number_gt 14577 _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^)+(0.0386P)^2^+29.2643P] 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 18930 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 Fe1 Fe 0.091613(11) 0.384067(19) 0.121701(7) 0.01525(6) Uani 1 1 d . . . N1 N 0.01968(6) 0.42578(11) 0.08979(4) 0.0160(3) Uani 1 1 d . . . N2 N -0.05406(7) 0.53869(12) 0.08645(5) 0.0212(3) Uani 1 1 d . . . H2A H -0.0637 0.5933 0.0939 0.025 Uiso 1 1 calc R . . N3 N 0.02689(8) 0.64426(12) 0.13353(5) 0.0242(4) Uani 1 1 d . . . H3A H -0.0044 0.6709 0.1220 0.029 Uiso 1 1 calc R . . N4 N 0.07958(7) 0.50507(12) 0.14472(4) 0.0181(3) Uani 1 1 d . . . N5 N 0.14625(7) 0.45462(12) 0.09552(4) 0.0188(3) Uani 1 1 d . . . N6 N 0.24041(7) 0.51868(13) 0.10573(5) 0.0261(4) Uani 1 1 d . . . H6A H 0.2755 0.5147 0.1182 0.031 Uiso 1 1 calc R . . N7 N 0.26694(7) 0.37894(14) 0.15910(5) 0.0266(4) Uani 1 1 d . . . H7A H 0.2953 0.4094 0.1511 0.032 Uiso 1 1 calc R . . N8 N 0.16579(7) 0.35382(12) 0.15258(4) 0.0177(3) Uani 1 1 d . . . N9 N 0.09191(6) 0.26244(11) 0.09638(4) 0.0177(3) Uani 1 1 d . A . N10 N 0.04339(6) 0.31675(12) 0.15161(4) 0.0186(3) Uani 1 1 d . . . B1 B 0.21729(9) 0.34855(17) 0.33317(6) 0.0208(4) Uani 1 1 d . . . B2 B 0.40525(9) 0.34846(16) 0.08214(7) 0.0209(4) Uani 1 1 d . . . C1 C -0.01635(8) 0.37041(14) 0.06197(6) 0.0223(4) Uani 1 1 d . . . H1A H -0.0368 0.3228 0.0744 0.027 Uiso 1 1 calc R . . H1B H 0.0089 0.3388 0.0465 0.027 Uiso 1 1 calc R . . C2 C -0.06080(9) 0.42805(16) 0.03751(6) 0.0252(4) Uani 1 1 d . . . H2B H -0.0408 0.4676 0.0214 0.030 Uiso 1 1 calc R . . H2C H -0.0876 0.3871 0.0217 0.030 Uiso 1 1 calc R . . C3 C -0.09495(8) 0.48729(16) 0.06048(6) 0.0250(4) Uani 1 1 d . . . H3B H -0.1202 0.5301 0.0445 0.030 Uiso 1 1 calc R . . H3C H -0.1198 0.4483 0.0739 0.030 Uiso 1 1 calc R . . C4 C -0.00167(8) 0.50341(13) 0.09923(5) 0.0163(3) Uani 1 1 d . . . C5 C 0.03775(8) 0.55471(13) 0.12760(5) 0.0168(3) Uani 1 1 d . . . C6 C 0.06833(11) 0.69599(17) 0.15947(7) 0.0370(6) Uani 1 1 d . . . H6B H 0.0484 0.7477 0.1698 0.044 Uiso 1 1 calc R . . H6C H 0.0993 0.7215 0.1466 0.044 Uiso 1 1 calc R . . C7 C 0.09377(13) 0.63461(18) 0.18914(7) 0.0428(7) Uani 1 1 d . . . H7B H 0.0635 0.6162 0.2041 0.051 Uiso 1 1 calc R . . H7C H 0.1245 0.6677 0.2054 0.051 Uiso 1 1 calc R . . C8 C 0.11945(10) 0.54894(16) 0.17381(6) 0.0278(5) Uani 1 1 d . . . H8A H 0.1554 0.5660 0.1640 0.033 Uiso 1 1 calc R . . H8B H 0.1300 0.5044 0.1940 0.033 Uiso 1 1 calc R . . C9 C 0.12942(9) 0.51778(16) 0.06484(6) 0.0259(4) Uani 1 1 d . . . H9A H 0.1090 0.5711 0.0737 0.031 Uiso 1 1 calc R . . H9B H 0.1022 0.4862 0.0457 0.031 Uiso 1 1 calc R . . C10 C 0.18147(9) 0.55198(16) 0.04782(6) 0.0256(4) Uani 1 1 d . . . H10A H 0.1977 0.5009 0.0347 0.031 Uiso 1 1 calc R . . H10B H 0.1690 0.6010 0.0297 0.031 Uiso 1 1 calc R . . C11 C 0.22747(9) 0.58891(16) 0.07744(6) 0.0271(4) Uani 1 1 d . . . H11A H 0.2629 0.6043 0.0668 0.033 Uiso 1 1 calc R . . H11B H 0.2134 0.6454 0.0883 0.033 Uiso 1 1 calc R . . C12 C 0.19884(8) 0.45983(14) 0.11289(5) 0.0205(4) Uani 1 1 d . . . C13 C 0.21177(8) 0.39289(14) 0.14336(5) 0.0197(4) Uani 1 1 d . . . C14 C 0.27999(9) 0.31343(19) 0.18936(7) 0.0345(6) Uani 1 1 d . . . H14A H 0.2814 0.3457 0.2132 0.041 Uiso 1 1 calc R . . H14B H 0.3183 0.2848 0.1885 0.041 Uiso 1 1 calc R . . C15 C 0.23368(10) 0.24079(19) 0.18587(8) 0.0370(6) Uani 1 1 d . . . H15A H 0.2391 0.2011 0.2080 0.044 Uiso 1 1 calc R . . H15B H 0.2369 0.2018 0.1642 0.044 Uiso 1 1 calc R . . C16 C 0.17415(8) 0.28445(15) 0.18170(6) 0.0240(4) Uani 1 1 d . . . H16A H 0.1444 0.2359 0.1762 0.029 Uiso 1 1 calc R . . H16B H 0.1685 0.3134 0.2053 0.029 Uiso 1 1 calc R . . C17 C 0.12076(9) 0.23544(15) 0.06852(6) 0.0235(4) Uani 1 1 d . . . H17A H 0.1491 0.2752 0.0609 0.028 Uiso 0.265(7) 1 calc PR A 2 C18 C 0.11000(10) 0.15157(18) 0.05097(7) 0.0329(5) Uani 1 1 d . A . H18A H 0.1316 0.1339 0.0321 0.039 Uiso 1 1 calc R . . C19 C 0.06794(11) 0.09358(17) 0.06095(7) 0.0345(5) Uani 1 1 d . . . H19A H 0.0587 0.0376 0.0482 0.041 Uiso 1 1 calc R A . C20 C 0.03963(9) 0.11915(16) 0.09006(6) 0.0278(4) Uani 1 1 d . A . H20A H 0.0110 0.0803 0.0979 0.033 Uiso 1 1 calc R . . C21 C 0.05354(8) 0.20180(14) 0.10753(5) 0.0187(4) Uani 1 1 d . . . C22 C 0.02863(8) 0.23055(14) 0.14026(5) 0.0183(4) Uani 1 1 d . A . C23 C -0.00508(9) 0.17358(15) 0.15877(6) 0.0237(4) Uani 1 1 d . . . H23A H -0.0139 0.1129 0.1503 0.028 Uiso 1 1 calc R A . C24 C -0.02569(9) 0.20662(18) 0.18988(6) 0.0301(5) Uani 1 1 d . A . H24A H -0.0481 0.1686 0.2035 0.036 Uiso 1 1 calc R . . C25 C -0.01285(10) 0.29598(18) 0.20052(6) 0.0315(5) Uani 1 1 d . . . H25A H -0.0286 0.3215 0.2207 0.038 Uiso 1 1 calc R A . C26 C 0.02286(9) 0.34845(17) 0.18189(6) 0.0284(5) Uani 1 1 d . A . H26A H 0.0333 0.4085 0.1906 0.034 Uiso 0.735(7) 1 calc PR A 1 C27A C 0.16810(14) 0.2898(2) 0.05653(9) 0.0345(9) Uiso 0.735(7) 1 d P A 1 H27A H 0.1971 0.3038 0.0778 0.052 Uiso 0.735(7) 1 calc PR A 1 H27B H 0.1524 0.3472 0.0453 0.052 Uiso 0.735(7) 1 calc PR A 1 H27C H 0.1862 0.2545 0.0385 0.052 Uiso 0.735(7) 1 calc PR A 1 C27B C 0.0474(7) 0.4193(11) 0.2088(4) 0.077(5) Uiso 0.265(7) 1 d P A 2 H27D H 0.0413 0.4804 0.1978 0.115 Uiso 0.265(7) 1 calc PR A 2 H27E H 0.0890 0.4084 0.2158 0.115 Uiso 0.265(7) 1 calc PR A 2 H27F H 0.0281 0.4157 0.2308 0.115 Uiso 0.265(7) 1 calc PR A 2 C28 C 0.28296(9) 0.38824(15) 0.33092(6) 0.0246(4) Uani 1 1 d . . . C29 C 0.30290(10) 0.46834(16) 0.35029(7) 0.0333(5) Uani 1 1 d . . . H29A H 0.2798 0.4946 0.3669 0.040 Uiso 1 1 calc R . . C30 C 0.35503(11) 0.51041(19) 0.34610(9) 0.0450(7) Uani 1 1 d . . . H30A H 0.3667 0.5644 0.3597 0.054 Uiso 1 1 calc R . . C31 C 0.38985(11) 0.4746(2) 0.32247(9) 0.0481(8) Uani 1 1 d . . . H31A H 0.4257 0.5029 0.3199 0.058 Uiso 1 1 calc R . . C32 C 0.37181(10) 0.39664(19) 0.30252(8) 0.0411(7) Uani 1 1 d . . . H32A H 0.3952 0.3715 0.2859 0.049 Uiso 1 1 calc R . . C33 C 0.31928(9) 0.35483(17) 0.30676(7) 0.0305(5) Uani 1 1 d . . . H33A H 0.3077 0.3015 0.2927 0.037 Uiso 1 1 calc R . . C34 C 0.20645(8) 0.31754(14) 0.37480(6) 0.0208(4) Uani 1 1 d . . . C35 C 0.24070(9) 0.34217(15) 0.40800(6) 0.0241(4) Uani 1 1 d . . . H35A H 0.2744 0.3782 0.4071 0.029 Uiso 1 1 calc R . . C36 C 0.22710(10) 0.31584(15) 0.44220(6) 0.0266(4) Uani 1 1 d . . . H36A H 0.2516 0.3342 0.4639 0.032 Uiso 1 1 calc R . . C37 C 0.17838(10) 0.26333(15) 0.44504(6) 0.0260(4) Uani 1 1 d . . . H37A H 0.1689 0.2464 0.4684 0.031 Uiso 1 1 calc R . . C38 C 0.14364(9) 0.23596(15) 0.41283(6) 0.0244(4) Uani 1 1 d . . . H38A H 0.1103 0.1991 0.4140 0.029 Uiso 1 1 calc R . . C39 C 0.15787(9) 0.26276(15) 0.37895(6) 0.0235(4) Uani 1 1 d . . . H39A H 0.1335 0.2431 0.3574 0.028 Uiso 1 1 calc R . . C40 C 0.20378(8) 0.25863(14) 0.30654(5) 0.0208(4) Uani 1 1 d . . . C41 C 0.23821(9) 0.17883(15) 0.31310(6) 0.0247(4) Uani 1 1 d . . . H41A H 0.2685 0.1784 0.3334 0.030 Uiso 1 1 calc R . . C42 C 0.22957(10) 0.10074(15) 0.29103(6) 0.0269(4) Uani 1 1 d . . . H42A H 0.2546 0.0493 0.2959 0.032 Uiso 1 1 calc R . . C43 C 0.18431(10) 0.09795(15) 0.26191(6) 0.0262(4) Uani 1 1 d . . . H43A H 0.1783 0.0450 0.2467 0.031 Uiso 1 1 calc R . . C44 C 0.14826(9) 0.17350(16) 0.25544(6) 0.0256(4) Uani 1 1 d . . . H44A H 0.1164 0.1718 0.2362 0.031 Uiso 1 1 calc R . . C45 C 0.15860(9) 0.25247(15) 0.27710(5) 0.0223(4) Uani 1 1 d . . . H45A H 0.1339 0.3041 0.2716 0.027 Uiso 1 1 calc R . . C46 C 0.17342(8) 0.43444(14) 0.31845(6) 0.0215(4) Uani 1 1 d . . . C47 C 0.12241(10) 0.45680(16) 0.33238(6) 0.0279(4) Uani 1 1 d . . . H47A H 0.1109 0.4197 0.3513 0.033 Uiso 1 1 calc R . . C48 C 0.08772(11) 0.53155(18) 0.31950(7) 0.0341(5) Uani 1 1 d . . . H48A H 0.0533 0.5441 0.3296 0.041 Uiso 1 1 calc R . . C49 C 0.10332(10) 0.58738(17) 0.29207(7) 0.0317(5) Uani 1 1 d . . . H49A H 0.0802 0.6388 0.2834 0.038 Uiso 1 1 calc R . . C50 C 0.15340(10) 0.56691(18) 0.27743(7) 0.0343(5) Uani 1 1 d . . . H50A H 0.1648 0.6045 0.2586 0.041 Uiso 1 1 calc R . . C51 C 0.18675(10) 0.49189(18) 0.29023(6) 0.0310(5) Uani 1 1 d . . . H51A H 0.2204 0.4786 0.2793 0.037 Uiso 1 1 calc R . . C52 C 0.40848(8) 0.39428(14) 0.12312(6) 0.0210(4) Uani 1 1 d . . . C53 C 0.38583(8) 0.48122(14) 0.12953(6) 0.0207(4) Uani 1 1 d . . . H53A H 0.3692 0.5168 0.1090 0.025 Uiso 1 1 calc R . . C54 C 0.38674(8) 0.51755(15) 0.16475(6) 0.0240(4) Uani 1 1 d . . . H54A H 0.3700 0.5760 0.1678 0.029 Uiso 1 1 calc R . . C55 C 0.41204(9) 0.46851(16) 0.19525(6) 0.0274(4) Uani 1 1 d . . . H55A H 0.4125 0.4927 0.2193 0.033 Uiso 1 1 calc R . . C56 C 0.43661(9) 0.38352(17) 0.19006(6) 0.0288(4) Uani 1 1 d . . . H56A H 0.4552 0.3499 0.2106 0.035 Uiso 1 1 calc R . . C57 C 0.43411(9) 0.34760(16) 0.15490(6) 0.0264(4) Uani 1 1 d . . . H57A H 0.4505 0.2887 0.1521 0.032 Uiso 1 1 calc R . . C58 C 0.47020(8) 0.31147(14) 0.07600(6) 0.0204(4) Uani 1 1 d . . . C59 C 0.52132(9) 0.35201(15) 0.09371(6) 0.0255(4) Uani 1 1 d . . . H59A H 0.5184 0.3976 0.1119 0.031 Uiso 1 1 calc R . . C60 C 0.57623(9) 0.32838(15) 0.08584(7) 0.0298(5) Uani 1 1 d . . . H60A H 0.6097 0.3581 0.0983 0.036 Uiso 1 1 calc R . . C61 C 0.58179(9) 0.26137(16) 0.05980(7) 0.0301(5) Uani 1 1 d . . . H61A H 0.6190 0.2443 0.0544 0.036 Uiso 1 1 calc R . . C62 C 0.53237(10) 0.21967(16) 0.04185(6) 0.0286(5) Uani 1 1 d . . . H62A H 0.5357 0.1737 0.0239 0.034 Uiso 1 1 calc R . . C63 C 0.47763(9) 0.24448(15) 0.04976(6) 0.0235(4) Uani 1 1 d . . . H63A H 0.4444 0.2150 0.0369 0.028 Uiso 1 1 calc R . . C64 C 0.35861(8) 0.26209(14) 0.07759(6) 0.0221(4) Uani 1 1 d . . . C65 C 0.34528(9) 0.20891(15) 0.10715(7) 0.0273(4) Uani 1 1 d . . . H65A H 0.3634 0.2238 0.1312 0.033 Uiso 1 1 calc R . . C66 C 0.30666(10) 0.13531(16) 0.10278(7) 0.0320(5) Uani 1 1 d . . . H66A H 0.2996 0.1008 0.1236 0.038 Uiso 1 1 calc R . . C67 C 0.27872(10) 0.11226(16) 0.06844(7) 0.0333(5) Uani 1 1 d . . . H67A H 0.2517 0.0630 0.0655 0.040 Uiso 1 1 calc R . . C68 C 0.29066(10) 0.16224(16) 0.03818(7) 0.0323(5) Uani 1 1 d . . . H68A H 0.2719 0.1471 0.0142 0.039 Uiso 1 1 calc R . . C69 C 0.33019(9) 0.23450(15) 0.04304(7) 0.0273(4) Uani 1 1 d . . . H69A H 0.3383 0.2668 0.0219 0.033 Uiso 1 1 calc R . . C70 C 0.38692(8) 0.42764(14) 0.05066(5) 0.0198(4) Uani 1 1 d . . . C71 C 0.32934(9) 0.44913(14) 0.03668(6) 0.0234(4) Uani 1 1 d . . . H71A H 0.2991 0.4165 0.0458 0.028 Uiso 1 1 calc R . . C72 C 0.31467(9) 0.51645(15) 0.00998(6) 0.0262(4) Uani 1 1 d . . . H72A H 0.2751 0.5272 0.0006 0.031 Uiso 1 1 calc R . . C73 C 0.35771(9) 0.56791(15) -0.00293(6) 0.0260(4) Uani 1 1 d . . . H73A H 0.3479 0.6138 -0.0212 0.031 Uiso 1 1 calc R . . C74 C 0.41505(9) 0.55141(14) 0.01114(6) 0.0245(4) Uani 1 1 d . . . H74A H 0.4449 0.5875 0.0033 0.029 Uiso 1 1 calc R . . C75 C 0.42888(9) 0.48176(14) 0.03690(6) 0.0223(4) Uani 1 1 d . . . H75A H 0.4686 0.4703 0.0456 0.027 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 0.01295(11) 0.01380(13) 0.01932(12) 0.00155(10) 0.00336(9) 0.00011(10) N1 0.0132(6) 0.0148(8) 0.0200(7) -0.0008(6) 0.0019(5) -0.0001(6) N2 0.0163(7) 0.0164(8) 0.0303(9) -0.0033(7) 0.0014(6) 0.0030(6) N3 0.0242(8) 0.0163(8) 0.0295(9) -0.0051(7) -0.0051(7) 0.0026(7) N4 0.0179(7) 0.0182(8) 0.0179(7) -0.0001(6) 0.0019(6) 0.0004(6) N5 0.0151(7) 0.0217(9) 0.0199(7) 0.0068(6) 0.0039(6) 0.0007(6) N6 0.0169(7) 0.0285(10) 0.0326(9) 0.0131(8) 0.0021(7) -0.0036(7) N7 0.0141(7) 0.0331(10) 0.0316(9) 0.0151(8) 0.0002(6) -0.0026(7) N8 0.0149(7) 0.0173(8) 0.0211(8) 0.0053(6) 0.0033(6) 0.0008(6) N9 0.0140(7) 0.0157(8) 0.0234(8) 0.0027(6) 0.0030(6) 0.0011(6) N10 0.0131(6) 0.0194(8) 0.0232(8) 0.0001(6) 0.0026(6) 0.0008(6) B1 0.0177(9) 0.0201(11) 0.0237(10) -0.0016(9) 0.0004(8) -0.0029(8) B2 0.0193(9) 0.0163(10) 0.0282(11) 0.0031(9) 0.0066(8) 0.0018(8) C1 0.0195(8) 0.0183(10) 0.0275(10) -0.0060(8) -0.0019(7) 0.0009(7) C2 0.0190(9) 0.0292(12) 0.0259(10) -0.0046(9) -0.0020(7) 0.0030(8) C3 0.0157(8) 0.0272(11) 0.0308(11) -0.0033(9) -0.0017(7) 0.0031(8) C4 0.0153(8) 0.0162(9) 0.0181(8) 0.0009(7) 0.0049(6) -0.0019(7) C5 0.0163(8) 0.0161(9) 0.0187(8) -0.0004(7) 0.0051(6) 0.0002(7) C6 0.0388(13) 0.0269(13) 0.0399(13) -0.0129(10) -0.0127(10) 0.0048(10) C7 0.0568(16) 0.0303(14) 0.0354(13) -0.0088(11) -0.0134(12) 0.0065(12) C8 0.0301(10) 0.0247(11) 0.0247(10) -0.0033(8) -0.0090(8) 0.0053(9) C9 0.0185(9) 0.0327(12) 0.0270(10) 0.0141(9) 0.0050(7) 0.0029(8) C10 0.0206(9) 0.0295(12) 0.0279(10) 0.0138(9) 0.0075(8) 0.0021(8) C11 0.0259(10) 0.0253(11) 0.0311(11) 0.0123(9) 0.0073(8) -0.0012(8) C12 0.0173(8) 0.0214(10) 0.0231(9) 0.0075(8) 0.0042(7) -0.0008(7) C13 0.0174(8) 0.0210(10) 0.0203(9) 0.0053(7) 0.0012(6) 0.0002(7) C14 0.0177(9) 0.0486(15) 0.0357(12) 0.0227(11) -0.0015(8) 0.0015(9) C15 0.0252(10) 0.0406(15) 0.0464(14) 0.0231(12) 0.0090(10) 0.0076(10) C16 0.0179(8) 0.0251(11) 0.0295(10) 0.0135(8) 0.0051(7) 0.0014(8) C17 0.0195(9) 0.0231(11) 0.0292(10) 0.0025(8) 0.0084(7) 0.0005(8) C18 0.0325(11) 0.0329(13) 0.0362(12) -0.0067(10) 0.0149(9) 0.0024(10) C19 0.0401(13) 0.0285(13) 0.0367(12) -0.0106(10) 0.0121(10) -0.0081(10) C20 0.0281(10) 0.0221(11) 0.0344(11) -0.0021(9) 0.0093(8) -0.0087(9) C21 0.0163(8) 0.0171(9) 0.0227(9) 0.0020(7) 0.0031(7) -0.0012(7) C22 0.0133(7) 0.0187(9) 0.0226(9) 0.0037(7) 0.0020(6) 0.0003(7) C23 0.0211(9) 0.0223(10) 0.0285(10) 0.0055(8) 0.0060(8) -0.0025(8) C24 0.0241(10) 0.0390(14) 0.0291(11) 0.0091(10) 0.0103(8) -0.0022(9) C25 0.0301(11) 0.0440(14) 0.0218(10) -0.0017(10) 0.0079(8) 0.0011(10) C26 0.0203(9) 0.0332(12) 0.0324(11) -0.0085(9) 0.0064(8) -0.0021(9) C28 0.0200(9) 0.0181(10) 0.0340(11) 0.0066(9) -0.0020(8) -0.0008(8) C29 0.0296(11) 0.0215(11) 0.0453(14) 0.0055(10) -0.0061(10) -0.0050(9) C30 0.0341(13) 0.0293(14) 0.0651(18) 0.0181(13) -0.0154(12) -0.0165(11) C31 0.0226(11) 0.0422(16) 0.075(2) 0.0372(15) -0.0083(12) -0.0113(11) C32 0.0235(10) 0.0385(15) 0.0618(17) 0.0320(13) 0.0075(10) 0.0026(10) C33 0.0249(10) 0.0242(11) 0.0430(13) 0.0133(10) 0.0073(9) -0.0004(8) C34 0.0229(9) 0.0144(9) 0.0244(9) -0.0031(7) 0.0011(7) 0.0000(7) C35 0.0245(9) 0.0175(10) 0.0290(10) -0.0048(8) -0.0011(8) -0.0004(8) C36 0.0333(11) 0.0217(11) 0.0229(10) -0.0060(8) -0.0028(8) 0.0060(9) C37 0.0360(11) 0.0193(10) 0.0235(10) -0.0006(8) 0.0073(8) 0.0084(9) C38 0.0274(10) 0.0180(10) 0.0285(10) -0.0010(8) 0.0062(8) 0.0015(8) C39 0.0257(9) 0.0208(10) 0.0233(9) -0.0021(8) 0.0012(7) -0.0024(8) C40 0.0199(8) 0.0221(10) 0.0214(9) -0.0004(8) 0.0063(7) -0.0053(7) C41 0.0245(9) 0.0230(11) 0.0261(10) -0.0004(8) 0.0020(8) -0.0048(8) C42 0.0306(10) 0.0201(11) 0.0312(11) -0.0016(8) 0.0080(8) -0.0038(8) C43 0.0340(11) 0.0235(11) 0.0232(10) -0.0037(8) 0.0107(8) -0.0123(9) C44 0.0275(10) 0.0312(12) 0.0185(9) -0.0007(8) 0.0051(7) -0.0104(9) C45 0.0209(9) 0.0257(11) 0.0211(9) -0.0002(8) 0.0059(7) -0.0040(8) C46 0.0206(9) 0.0195(10) 0.0235(9) -0.0015(8) -0.0002(7) -0.0031(7) C47 0.0318(11) 0.0263(12) 0.0264(10) 0.0012(9) 0.0071(8) 0.0028(9) C48 0.0346(12) 0.0365(14) 0.0326(12) 0.0000(10) 0.0094(9) 0.0129(10) C49 0.0345(11) 0.0257(12) 0.0328(12) 0.0019(9) -0.0015(9) 0.0069(9) C50 0.0291(11) 0.0358(14) 0.0362(12) 0.0142(10) -0.0014(9) -0.0030(10) C51 0.0235(10) 0.0375(13) 0.0320(11) 0.0081(10) 0.0041(8) -0.0016(9) C52 0.0163(8) 0.0191(10) 0.0288(10) 0.0031(8) 0.0074(7) 0.0026(7) C53 0.0140(8) 0.0188(10) 0.0298(10) 0.0025(8) 0.0051(7) 0.0002(7) C54 0.0189(9) 0.0199(10) 0.0342(11) -0.0019(8) 0.0068(8) 0.0010(7) C55 0.0246(10) 0.0295(12) 0.0293(11) -0.0014(9) 0.0078(8) 0.0001(9) C56 0.0281(10) 0.0305(12) 0.0281(10) 0.0063(9) 0.0058(8) 0.0052(9) C57 0.0245(10) 0.0242(11) 0.0312(11) 0.0032(9) 0.0066(8) 0.0076(8) C58 0.0199(8) 0.0133(9) 0.0294(10) 0.0044(8) 0.0087(7) 0.0016(7) C59 0.0223(9) 0.0149(9) 0.0405(12) -0.0005(9) 0.0086(8) 0.0006(8) C60 0.0196(9) 0.0194(11) 0.0516(14) 0.0042(10) 0.0093(9) -0.0013(8) C61 0.0248(10) 0.0235(11) 0.0455(13) 0.0112(10) 0.0176(9) 0.0072(8) C62 0.0350(11) 0.0248(11) 0.0285(11) 0.0029(9) 0.0137(9) 0.0100(9) C63 0.0250(9) 0.0201(10) 0.0261(10) 0.0039(8) 0.0059(8) 0.0044(8) C64 0.0194(8) 0.0148(9) 0.0335(11) 0.0043(8) 0.0084(8) 0.0040(7) C65 0.0286(10) 0.0205(11) 0.0349(11) 0.0046(9) 0.0124(9) 0.0035(8) C66 0.0333(11) 0.0210(11) 0.0455(13) 0.0093(10) 0.0186(10) 0.0015(9) C67 0.0239(10) 0.0205(11) 0.0570(15) 0.0072(11) 0.0108(10) -0.0009(9) C68 0.0252(10) 0.0238(12) 0.0464(14) 0.0046(10) -0.0003(9) -0.0029(9) C69 0.0246(10) 0.0200(11) 0.0368(12) 0.0091(9) 0.0030(8) -0.0013(8) C70 0.0212(9) 0.0143(9) 0.0253(9) 0.0007(7) 0.0075(7) 0.0013(7) C71 0.0217(9) 0.0191(10) 0.0316(10) 0.0059(8) 0.0112(8) 0.0041(8) C72 0.0247(9) 0.0232(11) 0.0327(11) 0.0076(9) 0.0107(8) 0.0080(8) C73 0.0326(11) 0.0179(10) 0.0294(10) 0.0064(8) 0.0117(8) 0.0053(8) C74 0.0289(10) 0.0168(10) 0.0301(10) 0.0013(8) 0.0117(8) -0.0025(8) C75 0.0220(9) 0.0177(10) 0.0279(10) 0.0011(8) 0.0059(7) -0.0007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N10 1.9461(16) . ? Fe1 N8 1.9769(15) . ? Fe1 N5 1.9889(16) . ? Fe1 N4 1.9912(17) . ? Fe1 N1 1.9979(15) . ? Fe1 N9 2.0007(17) . ? N1 C4 1.302(2) . ? N1 C1 1.467(2) . ? N2 C4 1.346(2) . ? N2 C3 1.455(3) . ? N2 H2A 0.8800 . ? N3 C5 1.351(3) . ? N3 C6 1.465(3) . ? N3 H3A 0.8800 . ? N4 C5 1.301(2) . ? N4 C8 1.459(3) . ? N5 C12 1.301(2) . ? N5 C9 1.464(3) . ? N6 C12 1.348(2) . ? N6 C11 1.458(3) . ? N6 H6A 0.8800 . ? N7 C13 1.348(2) . ? N7 C14 1.464(3) . ? N7 H7A 0.8800 . ? N8 C13 1.301(2) . ? N8 C16 1.464(2) . ? N9 C21 1.361(2) . ? N9 C17 1.361(3) . ? N10 C22 1.351(3) . ? N10 C26 1.354(3) . ? B1 C40 1.638(3) . ? B1 C34 1.649(3) . ? B1 C28 1.650(3) . ? B1 C46 1.656(3) . ? B2 C52 1.639(3) . ? B2 C70 1.645(3) . ? B2 C58 1.653(3) . ? B2 C64 1.655(3) . ? C1 C2 1.523(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.511(3) . ? C2 H2B 0.9900 . ? C2 H2C 0.9900 . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C4 C5 1.488(3) . ? C6 C7 1.467(4) . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C7 C8 1.526(3) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.527(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.513(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.482(3) . ? C14 C15 1.504(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.514(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.387(3) . ? C17 C27A 1.476(4) . ? C17 H17A 0.9500 . ? C18 C19 1.383(3) . ? C18 H18A 0.9500 . ? C19 C20 1.387(3) . ? C19 H19A 0.9500 . ? C20 C21 1.380(3) . ? C20 H20A 0.9500 . ? C21 C22 1.470(3) . ? C22 C23 1.386(3) . ? C23 C24 1.389(3) . ? C23 H23A 0.9500 . ? C24 C25 1.379(4) . ? C24 H24A 0.9500 . ? C25 C26 1.382(3) . ? C25 H25A 0.9500 . ? C26 C27B 1.486(16) . ? C26 H26A 0.9500 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28 C33 1.399(3) . ? C28 C29 1.410(3) . ? C29 C30 1.389(3) . ? C29 H29A 0.9500 . ? C30 C31 1.374(5) . ? C30 H30A 0.9500 . ? C31 C32 1.383(4) . ? C31 H31A 0.9500 . ? C32 C33 1.396(3) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.405(3) . ? C34 C39 1.411(3) . ? C35 C36 1.393(3) . ? C35 H35A 0.9500 . ? C36 C37 1.385(3) . ? C36 H36A 0.9500 . ? C37 C38 1.393(3) . ? C37 H37A 0.9500 . ? C38 C39 1.390(3) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C45 1.400(3) . ? C40 C41 1.413(3) . ? C41 C42 1.394(3) . ? C41 H41A 0.9500 . ? C42 C43 1.391(3) . ? C42 H42A 0.9500 . ? C43 C44 1.384(3) . ? C43 H43A 0.9500 . ? C44 C45 1.399(3) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.399(3) . ? C46 C51 1.402(3) . ? C47 C48 1.397(3) . ? C47 H47A 0.9500 . ? C48 C49 1.384(3) . ? C48 H48A 0.9500 . ? C49 C50 1.386(3) . ? C49 H49A 0.9500 . ? C50 C51 1.383(3) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.404(3) . ? C52 C57 1.408(3) . ? C53 C54 1.395(3) . ? C53 H53A 0.9500 . ? C54 C55 1.387(3) . ? C54 H54A 0.9500 . ? C55 C56 1.388(3) . ? C55 H55A 0.9500 . ? C56 C57 1.387(3) . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C58 C63 1.400(3) . ? C58 C59 1.403(3) . ? C59 C60 1.395(3) . ? C59 H59A 0.9500 . ? C60 C61 1.386(3) . ? C60 H60A 0.9500 . ? C61 C62 1.383(3) . ? C61 H61A 0.9500 . ? C62 C63 1.397(3) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C69 1.404(3) . ? C64 C65 1.405(3) . ? C65 C66 1.394(3) . ? C65 H65A 0.9500 . ? C66 C67 1.376(4) . ? C66 H66A 0.9500 . ? C67 C68 1.390(3) . ? C67 H67A 0.9500 . ? C68 C69 1.393(3) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? C70 C71 1.402(3) . ? C70 C75 1.405(3) . ? C71 C72 1.394(3) . ? C71 H71A 0.9500 . ? C72 C73 1.389(3) . ? C72 H72A 0.9500 . ? C73 C74 1.383(3) . ? C73 H73A 0.9500 . ? C74 C75 1.393(3) . ? C74 H74A 0.9500 . ? C75 H75A 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 N10 Fe1 N8 95.30(7) . . ? N10 Fe1 N5 174.50(7) . . ? N8 Fe1 N5 79.89(6) . . ? N10 Fe1 N4 94.43(7) . . ? N8 Fe1 N4 96.78(7) . . ? N5 Fe1 N4 83.57(7) . . ? N10 Fe1 N1 88.87(6) . . ? N8 Fe1 N1 174.83(7) . . ? N5 Fe1 N1 95.79(6) . . ? N4 Fe1 N1 79.80(6) . . ? N10 Fe1 N9 81.84(7) . . ? N8 Fe1 N9 90.50(7) . . ? N5 Fe1 N9 100.75(7) . . ? N4 Fe1 N9 172.11(6) . . ? N1 Fe1 N9 93.13(6) . . ? C4 N1 C1 117.38(15) . . ? C4 N1 Fe1 115.35(13) . . ? C1 N1 Fe1 126.17(13) . . ? C4 N2 C3 120.59(17) . . ? C4 N2 H2A 119.7 . . ? C3 N2 H2A 119.7 . . ? C5 N3 C6 118.66(17) . . ? C5 N3 H3A 120.7 . . ? C6 N3 H3A 120.7 . . ? C5 N4 C8 117.74(17) . . ? C5 N4 Fe1 115.30(13) . . ? C8 N4 Fe1 125.78(13) . . ? C12 N5 C9 118.09(16) . . ? C12 N5 Fe1 114.63(13) . . ? C9 N5 Fe1 125.27(12) . . ? C12 N6 C11 120.27(17) . . ? C12 N6 H6A 119.9 . . ? C11 N6 H6A 119.9 . . ? C13 N7 C14 120.38(17) . . ? C13 N7 H7A 119.8 . . ? C14 N7 H7A 119.8 . . ? C13 N8 C16 117.63(16) . . ? C13 N8 Fe1 116.03(13) . . ? C16 N8 Fe1 125.94(12) . . ? C21 N9 C17 117.16(17) . . ? C21 N9 Fe1 112.79(13) . . ? C17 N9 Fe1 129.83(14) . . ? C22 N10 C26 117.75(18) . . ? C22 N10 Fe1 115.82(13) . . ? C26 N10 Fe1 126.42(15) . . ? C40 B1 C34 107.08(17) . . ? C40 B1 C28 110.50(17) . . ? C34 B1 C28 114.17(16) . . ? C40 B1 C46 110.58(16) . . ? C34 B1 C46 109.87(16) . . ? C28 B1 C46 104.67(16) . . ? C52 B2 C70 109.51(17) . . ? C52 B2 C58 109.63(16) . . ? C70 B2 C58 106.42(16) . . ? C52 B2 C64 110.18(16) . . ? C70 B2 C64 111.14(17) . . ? C58 B2 C64 109.89(16) . . ? N1 C1 C2 112.43(17) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C1 110.68(17) . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 . . ? H2B C2 H2C 108.1 . . ? N2 C3 C2 108.16(16) . . ? N2 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? N2 C3 H3C 110.1 . . ? C2 C3 H3C 110.1 . . ? H3B C3 H3C 108.4 . . ? N1 C4 N2 126.92(18) . . ? N1 C4 C5 113.65(16) . . ? N2 C4 C5 119.42(17) . . ? N4 C5 N3 127.05(18) . . ? N4 C5 C4 113.87(17) . . ? N3 C5 C4 119.07(17) . . ? N3 C6 C7 109.2(2) . . ? N3 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? N3 C6 H6C 109.8 . . ? C7 C6 H6C 109.8 . . ? H6B C6 H6C 108.3 . . ? C6 C7 C8 111.2(2) . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7C 109.4 . . ? C8 C7 H7C 109.4 . . ? H7B C7 H7C 108.0 . . ? N4 C8 C7 112.70(18) . . ? N4 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N5 C9 C10 112.30(16) . . ? N5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 110.13(18) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N6 C11 C10 108.45(18) . . ? N6 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N6 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N5 C12 N6 126.50(18) . . ? N5 C12 C13 114.06(17) . . ? N6 C12 C13 119.44(17) . . ? N8 C13 N7 126.43(18) . . ? N8 C13 C12 113.47(16) . . ? N7 C13 C12 120.08(17) . . ? N7 C14 C15 108.96(18) . . ? N7 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? N7 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 110.5(2) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N8 C16 C15 112.80(17) . . ? N8 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? N8 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N9 C17 C18 121.88(19) . . ? N9 C17 C27A 122.8(2) . . ? C18 C17 C27A 115.2(2) . . ? N9 C17 H17A 119.1 . . ? C18 C17 H17A 119.1 . . ? C19 C18 C17 120.1(2) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 118.4(2) . . ? C18 C19 H19A 120.8 . . ? C20 C19 H19A 120.8 . . ? C21 C20 C19 119.1(2) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? N9 C21 C20 123.08(18) . . ? N9 C21 C22 114.58(17) . . ? C20 C21 C22 122.32(18) . . ? N10 C22 C23 122.78(19) . . ? N10 C22 C21 113.81(16) . . ? C23 C22 C21 123.36(19) . . ? C22 C23 C24 119.0(2) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C25 C24 C23 118.3(2) . . ? C25 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? C24 C25 C26 120.2(2) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? N10 C26 C25 121.9(2) . . ? N10 C26 C27B 129.5(7) . . ? C25 C26 C27B 104.8(7) . . ? N10 C26 H26A 119.1 . . ? C25 C26 H26A 119.1 . . ? C17 C27A H27A 109.5 . . ? C17 C27A H27B 109.5 . . ? C17 C27A H27C 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C33 C28 C29 115.0(2) . . ? C33 C28 B1 124.1(2) . . ? C29 C28 B1 120.4(2) . . ? C30 C29 C28 122.6(3) . . ? C30 C29 H29A 118.7 . . ? C28 C29 H29A 118.7 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C30 C31 C32 118.9(2) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C32 C33 C28 122.7(3) . . ? C32 C33 H33A 118.7 . . ? C28 C33 H33A 118.7 . . ? C35 C34 C39 114.53(19) . . ? C35 C34 B1 126.30(18) . . ? C39 C34 B1 119.15(17) . . ? C36 C35 C34 122.6(2) . . ? C36 C35 H35A 118.7 . . ? C34 C35 H35A 118.7 . . ? C37 C36 C35 121.0(2) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 118.5(2) . . ? C36 C37 H37A 120.8 . . ? C38 C37 H37A 120.8 . . ? C39 C38 C37 119.8(2) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C38 C39 C34 123.64(19) . . ? C38 C39 H39A 118.2 . . ? C34 C39 H39A 118.2 . . ? C45 C40 C41 115.15(19) . . ? C45 C40 B1 124.87(19) . . ? C41 C40 B1 119.97(17) . . ? C42 C41 C40 122.7(2) . . ? C42 C41 H41A 118.7 . . ? C40 C41 H41A 118.7 . . ? C43 C42 C41 120.1(2) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 118.9(2) . . ? C44 C43 H43A 120.5 . . ? C42 C43 H43A 120.5 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H44A 119.9 . . ? C45 C44 H44A 119.9 . . ? C44 C45 C40 122.8(2) . . ? C44 C45 H45A 118.6 . . ? C40 C45 H45A 118.6 . . ? C47 C46 C51 115.0(2) . . ? C47 C46 B1 125.01(19) . . ? C51 C46 B1 119.99(18) . . ? C48 C47 C46 122.6(2) . . ? C48 C47 H47A 118.7 . . ? C46 C47 H47A 118.7 . . ? C49 C48 C47 120.3(2) . . ? C49 C48 H48A 119.9 . . ? C47 C48 H48A 119.9 . . ? C48 C49 C50 118.7(2) . . ? C48 C49 H49A 120.6 . . ? C50 C49 H49A 120.6 . . ? C51 C50 C49 120.1(2) . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C50 C51 C46 123.3(2) . . ? C50 C51 H51A 118.3 . . ? C46 C51 H51A 118.3 . . ? C53 C52 C57 114.88(19) . . ? C53 C52 B2 123.53(18) . . ? C57 C52 B2 121.59(18) . . ? C54 C53 C52 122.77(19) . . ? C54 C53 H53A 118.6 . . ? C52 C53 H53A 118.6 . . ? C55 C54 C53 120.2(2) . . ? C55 C54 H54A 119.9 . . ? C53 C54 H54A 119.9 . . ? C54 C55 C56 118.9(2) . . ? C54 C55 H55A 120.5 . . ? C56 C55 H55A 120.5 . . ? C57 C56 C55 120.1(2) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C52 123.1(2) . . ? C56 C57 H57A 118.4 . . ? C52 C57 H57A 118.4 . . ? C63 C58 C59 115.56(18) . . ? C63 C58 B2 121.84(18) . . ? C59 C58 B2 122.24(18) . . ? C60 C59 C58 122.9(2) . . ? C60 C59 H59A 118.5 . . ? C58 C59 H59A 118.5 . . ? C61 C60 C59 119.8(2) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C62 C61 C60 118.97(19) . . ? C62 C61 H61A 120.5 . . ? C60 C61 H61A 120.5 . . ? C61 C62 C63 120.7(2) . . ? C61 C62 H62A 119.6 . . ? C63 C62 H62A 119.6 . . ? C62 C63 C58 122.1(2) . . ? C62 C63 H63A 119.0 . . ? C58 C63 H63A 119.0 . . ? C69 C64 C65 114.5(2) . . ? C69 C64 B2 121.78(18) . . ? C65 C64 B2 123.7(2) . . ? C66 C65 C64 123.0(2) . . ? C66 C65 H65A 118.5 . . ? C64 C65 H65A 118.5 . . ? C67 C66 C65 120.4(2) . . ? C67 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C66 C67 C68 118.9(2) . . ? C66 C67 H67A 120.6 . . ? C68 C67 H67A 120.6 . . ? C67 C68 C69 119.8(2) . . ? C67 C68 H68A 120.1 . . ? C69 C68 H68A 120.1 . . ? C68 C69 C64 123.3(2) . . ? C68 C69 H69A 118.3 . . ? C64 C69 H69A 118.3 . . ? C71 C70 C75 114.97(18) . . ? C71 C70 B2 123.52(17) . . ? C75 C70 B2 121.46(17) . . ? C72 C71 C70 122.68(19) . . ? C72 C71 H71A 118.7 . . ? C70 C71 H71A 118.7 . . ? C73 C72 C71 120.2(2) . . ? C73 C72 H72A 119.9 . . ? C71 C72 H72A 119.9 . . ? C74 C73 C72 119.0(2) . . ? C74 C73 H73A 120.5 . . ? C72 C73 H73A 120.5 . . ? C73 C74 C75 119.82(19) . . ? C73 C74 H74A 120.1 . . ? C75 C74 H74A 120.1 . . ? C74 C75 C70 123.20(19) . . ? C74 C75 H75A 118.4 . . ? C70 C75 H75A 118.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.094 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.066 #===END data_2-RT _database_code_depnum_ccdc_archive 'CCDC 789131' #TrackingRef '- 2-RT& LT.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H38 Fe N10, 2(C24 H20 B)' _chemical_formula_sum 'C75 H78 B2 Fe N10' _chemical_formula_weight 1196.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.726(5) _cell_length_b 14.829(3) _cell_length_c 37.103(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.91(3) _cell_angle_gamma 90.00 _cell_volume 12897(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.79 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5072 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8886 _exptl_absorpt_correction_T_max 0.9217 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; Responding to errors on checkcif: B: Isotropic non-H atoms in Main residues...3. our reply: C7 and C15 are the middle atoms of H2bip ligands, "chair configuration" disorder common for those atoms. C27 is the Methyl group at 2-position of 2,2'-Bipyridine. We refine the disorder atoms with isotropic displacement parameters. The ratios of main part for C7, C15 and C27 are 0.59, 0.54 and 0.71, respectively. B: Large Non-solvent C Ueq(max)/Ueq(min)...4.31 Ratio. Due to the partial occupancy, the disordered C27B has a large displacement parameter (Ueq = 0.199) at room temperature. Because C26 is connected with C27B,it results in error B: Check Low Ueq as compared to Neighbors for C26. B: Check High Ueq as compared to Neighbors for C6. C:Check High Ueq as compared to Neighbors for C8. C:Check Low Ueq as compared to Neighbors for C7B. C:Check Low Ueq as compared to Neighbors for C7A. The C6 and C8 atoms are connected with the disorder atom C7. Suitable/obvious disordered 2nd component were not found in the difference map, So we left C6 and C8 with (large) anisotropic parameters. ; _diffrn_ambient_temperature 296(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 95303 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.71 _reflns_number_total 11001 _reflns_number_gt 8351 _reflns_threshold_expression >2sigma(I) _comp_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^)+(0.0438P)^2^+20.3163P] 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 11001 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Fe1 Fe 0.093829(17) 0.61223(3) 0.121517(11) 0.04582(13) Uani 1 1 d . . . N1 N 0.01954(10) 0.56416(17) 0.08744(6) 0.0483(6) Uani 1 1 d . . . N2 N -0.05358(11) 0.45760(18) 0.08749(8) 0.0629(7) Uani 1 1 d . . . H2A H -0.0637 0.4082 0.0968 0.075 Uiso 1 1 calc R . . N3 N 0.02637(12) 0.35369(18) 0.13338(8) 0.0692(8) Uani 1 1 d . A . H3A H -0.0020 0.3274 0.1203 0.083 Uiso 1 1 calc R . . N4 N 0.07619(11) 0.48924(18) 0.14654(7) 0.0590(7) Uani 1 1 d . A . N5 N 0.15320(11) 0.53907(19) 0.09700(7) 0.0635(7) Uani 1 1 d . . . N6 N 0.24579(13) 0.4799(2) 0.11032(9) 0.0828(10) Uani 1 1 d . . . H6E H 0.2786 0.4844 0.1238 0.099 Uiso 1 1 calc R . . N7 N 0.27105(11) 0.6269(2) 0.15766(9) 0.0776(9) Uani 1 1 d . B . H7E H 0.2980 0.6001 0.1489 0.093 Uiso 1 1 calc R . . N8 N 0.17218(11) 0.64411(17) 0.15400(7) 0.0560(7) Uani 1 1 d . B . N9 N 0.08937(10) 0.74181(17) 0.09517(7) 0.0533(6) Uani 1 1 d . C . N10 N 0.04319(10) 0.68978(19) 0.15213(7) 0.0569(7) Uani 1 1 d . . . B1 B 0.40606(16) 0.6499(3) 0.08163(11) 0.0562(9) Uani 1 1 d . . . B2 B 0.28679(16) 0.1461(3) 0.16795(10) 0.0565(9) Uani 1 1 d . . . C1 C -0.01689(14) 0.6158(2) 0.05969(10) 0.0692(10) Uani 1 1 d . . . H1A H 0.0066 0.6442 0.0438 0.083 Uiso 1 1 calc R . . H1B H -0.0356 0.6632 0.0715 0.083 Uiso 1 1 calc R . . C2 C -0.06124(16) 0.5595(3) 0.03724(10) 0.0817(11) Uani 1 1 d . . . H2B H -0.0876 0.5985 0.0219 0.098 Uiso 1 1 calc R . . H2C H -0.0430 0.5206 0.0215 0.098 Uiso 1 1 calc R . . C3 C -0.09350(15) 0.5033(3) 0.05990(11) 0.0786(11) Uani 1 1 d . . . H3B H -0.1189 0.5410 0.0715 0.094 Uiso 1 1 calc R . . H3C H -0.1163 0.4594 0.0447 0.094 Uiso 1 1 calc R . . C4 C -0.00150(12) 0.4906(2) 0.09876(8) 0.0462(7) Uani 1 1 d . . . C5 C 0.03685(13) 0.4414(2) 0.12819(8) 0.0499(7) Uani 1 1 d . . . C6 C 0.0635(2) 0.3034(3) 0.16128(13) 0.1075(17) Uani 1 1 d . . . H6A H 0.0428 0.2899 0.1812 0.129 Uiso 0.412(15) 1 calc PR A 1 H6B H 0.0738 0.2467 0.1510 0.129 Uiso 0.412(15) 1 calc PR A 1 H6C H 0.0409 0.2586 0.1716 0.129 Uiso 0.588(15) 1 d PR A 2 H6D H 0.0920 0.2718 0.1500 0.129 Uiso 0.588(15) 1 d PR A 2 C7A C 0.1139(5) 0.3515(6) 0.1751(3) 0.072(4) Uiso 0.412(15) 1 d P A 1 H7A H 0.1256 0.3316 0.2000 0.087 Uiso 0.412(15) 1 calc PR A 1 H7B H 0.1433 0.3317 0.1613 0.087 Uiso 0.412(15) 1 calc PR A 1 C7B C 0.0892(4) 0.3567(4) 0.1889(2) 0.067(3) Uiso 0.588(15) 1 d P A 2 H7C H 0.1192 0.3225 0.2036 0.081 Uiso 0.588(15) 1 calc PR A 2 H7D H 0.0614 0.3729 0.2044 0.081 Uiso 0.588(15) 1 calc PR A 2 C8 C 0.11521(18) 0.4444(3) 0.17541(11) 0.0860(12) Uani 1 1 d . . . H8A H 0.1538 0.4638 0.1737 0.103 Uiso 0.412(15) 1 calc PR A 1 H8B H 0.1065 0.4649 0.1988 0.103 Uiso 0.412(15) 1 calc PR A 1 H8C H 0.1239 0.4851 0.1960 0.103 Uiso 0.588(15) 1 d PR A 2 H8D H 0.1506 0.4309 0.1665 0.103 Uiso 0.588(15) 1 d PR A 2 C9 C 0.13826(18) 0.4701(3) 0.06863(12) 0.0987(15) Uani 1 1 d . . . H9A H 0.1106 0.4950 0.0492 0.118 Uiso 1 1 calc R . . H9B H 0.1207 0.4192 0.0790 0.118 Uiso 1 1 calc R . . C10 C 0.18898(18) 0.4384(3) 0.05323(13) 0.1016(16) Uani 1 1 d . . . H10A H 0.2026 0.4866 0.0392 0.122 Uiso 1 1 calc R . . H10B H 0.1781 0.3882 0.0368 0.122 Uiso 1 1 calc R . . C11 C 0.2364(2) 0.4090(3) 0.08278(13) 0.0940(14) Uani 1 1 d . . . H11A H 0.2259 0.3532 0.0938 0.113 Uiso 1 1 calc R . . H11B H 0.2710 0.3986 0.0725 0.113 Uiso 1 1 calc R . . C12 C 0.20452(14) 0.5380(2) 0.11494(9) 0.0596(8) Uani 1 1 d . . . C13 C 0.21674(13) 0.6082(2) 0.14417(9) 0.0539(7) Uani 1 1 d . . . C14 C 0.28514(17) 0.6921(3) 0.18708(12) 0.0993(15) Uani 1 1 d . . . H14A H 0.3204 0.7229 0.1845 0.119 Uiso 0.544(10) 1 calc PR B 1 H14B H 0.2905 0.6613 0.2104 0.119 Uiso 0.544(10) 1 calc PR B 1 H14C H 0.3185 0.6717 0.2035 0.119 Uiso 0.456(10) 1 d PR B 2 H14D H 0.2941 0.7498 0.1771 0.119 Uiso 0.456(10) 1 d PR B 2 C15A C 0.2370(3) 0.7595(5) 0.1854(2) 0.076(3) Uiso 0.544(10) 1 d P B 1 H15A H 0.2426 0.7963 0.2073 0.091 Uiso 0.544(10) 1 calc PR B 1 H15B H 0.2374 0.7991 0.1646 0.091 Uiso 0.544(10) 1 calc PR B 1 C15B C 0.2386(4) 0.7070(7) 0.2057(3) 0.079(3) Uiso 0.456(10) 1 d P B 2 H15C H 0.2455 0.7623 0.2196 0.094 Uiso 0.456(10) 1 calc PR B 2 H15D H 0.2373 0.6582 0.2229 0.094 Uiso 0.456(10) 1 calc PR B 2 C16 C 0.18133(16) 0.7138(3) 0.18215(11) 0.0811(12) Uani 1 1 d . . . H16A H 0.1778 0.6866 0.2055 0.097 Uiso 0.544(10) 1 calc PR B 1 H16B H 0.1514 0.7587 0.1769 0.097 Uiso 0.544(10) 1 calc PR B 1 H16C H 0.1509 0.7113 0.1968 0.097 Uiso 0.456(10) 1 d PR B 2 H16D H 0.1800 0.7727 0.1706 0.097 Uiso 0.456(10) 1 d PR B 2 C17 C 0.11439(15) 0.7669(2) 0.06661(10) 0.0686(10) Uani 1 1 d . . . H17B H 0.1395 0.7272 0.0579 0.082 Uiso 0.286(10) 1 calc PR C 2 C18 C 0.10413(19) 0.8493(3) 0.04985(11) 0.0873(12) Uani 1 1 d . C . H18A H 0.1228 0.8653 0.0305 0.105 Uiso 1 1 calc R . . C19 C 0.0667(2) 0.9068(3) 0.06158(12) 0.0961(14) Uani 1 1 d . . . H19A H 0.0585 0.9619 0.0500 0.115 Uiso 1 1 calc R C . C20 C 0.04107(17) 0.8826(3) 0.09092(11) 0.0791(11) Uani 1 1 d . C . H20A H 0.0152 0.9214 0.0993 0.095 Uiso 1 1 calc R . . C21 C 0.05373(12) 0.8015(2) 0.10776(8) 0.0510(7) Uani 1 1 d . . . C22 C 0.03011(12) 0.7737(2) 0.14049(8) 0.0518(8) Uani 1 1 d . C . C23 C -0.00242(14) 0.8300(3) 0.15869(10) 0.0696(10) Uani 1 1 d . . . H23A H -0.0105 0.8886 0.1505 0.084 Uiso 1 1 calc R C . C24 C -0.02258(17) 0.7985(3) 0.18884(11) 0.0842(12) Uani 1 1 d . C . H24A H -0.0442 0.8358 0.2015 0.101 Uiso 1 1 calc R . . C25 C -0.01106(17) 0.7132(4) 0.20024(11) 0.0854(12) Uani 1 1 d . . . H25A H -0.0255 0.6904 0.2203 0.103 Uiso 1 1 calc R C . C26 C 0.02247(15) 0.6606(3) 0.18167(10) 0.0769(11) Uani 1 1 d . C . H26A H 0.0312 0.6022 0.1899 0.092 Uiso 0.714(10) 1 calc PR C 1 C27A C 0.1549(3) 0.7090(5) 0.0532(2) 0.123(3) Uiso 0.714(10) 1 d P C 1 H27A H 0.1796 0.6826 0.0734 0.184 Uiso 0.714(10) 1 calc PR C 1 H27B H 0.1772 0.7434 0.0386 0.184 Uiso 0.714(10) 1 calc PR C 1 H27C H 0.1350 0.6620 0.0386 0.184 Uiso 0.714(10) 1 calc PR C 1 C27B C 0.0454(12) 0.5907(19) 0.2060(8) 0.199(13) Uiso 0.286(10) 1 d P C 2 H27D H 0.0513 0.5376 0.1922 0.298 Uiso 0.286(10) 1 calc PR C 2 H27E H 0.0193 0.5774 0.2226 0.298 Uiso 0.286(10) 1 calc PR C 2 H27F H 0.0812 0.6100 0.2195 0.298 Uiso 0.286(10) 1 calc PR C 2 C28 C 0.40984(13) 0.6041(2) 0.12234(9) 0.0566(8) Uani 1 1 d . . . C29 C 0.38806(13) 0.5196(2) 0.12846(10) 0.0581(8) Uani 1 1 d . . . H29A H 0.3723 0.4854 0.1084 0.070 Uiso 1 1 calc R . . C30 C 0.38876(15) 0.4839(3) 0.16301(11) 0.0709(10) Uani 1 1 d . . . H30A H 0.3727 0.4275 0.1657 0.085 Uiso 1 1 calc R . . C31 C 0.41311(17) 0.5314(3) 0.19340(11) 0.0810(11) Uani 1 1 d . . . H31A H 0.4134 0.5081 0.2167 0.097 Uiso 1 1 calc R . . C32 C 0.43687(18) 0.6140(3) 0.18844(11) 0.0862(12) Uani 1 1 d . . . H32A H 0.4544 0.6466 0.2085 0.103 Uiso 1 1 calc R . . C33 C 0.43486(15) 0.6489(3) 0.15379(10) 0.0722(10) Uani 1 1 d . . . H33A H 0.4510 0.7053 0.1513 0.087 Uiso 1 1 calc R . . C34 C 0.46987(14) 0.6867(2) 0.07570(9) 0.0554(8) Uani 1 1 d . . . C35 C 0.52024(14) 0.6482(2) 0.09288(10) 0.0659(9) Uani 1 1 d . . . H35A H 0.5181 0.6044 0.1106 0.079 Uiso 1 1 calc R . . C36 C 0.57372(15) 0.6715(2) 0.08504(12) 0.0768(11) Uani 1 1 d . . . H36A H 0.6062 0.6435 0.0972 0.092 Uiso 1 1 calc R . . C37 C 0.57832(18) 0.7361(3) 0.05923(13) 0.0824(12) Uani 1 1 d . . . H37A H 0.6139 0.7524 0.0537 0.099 Uiso 1 1 calc R . . C38 C 0.52995(19) 0.7762(3) 0.04173(11) 0.0806(11) Uani 1 1 d . . . H38A H 0.5327 0.8202 0.0243 0.097 Uiso 1 1 calc R . . C39 C 0.47672(16) 0.7520(2) 0.04966(9) 0.0656(9) Uani 1 1 d . . . H39A H 0.4445 0.7803 0.0372 0.079 Uiso 1 1 calc R . . C40 C 0.35993(14) 0.7341(2) 0.07739(10) 0.0608(9) Uani 1 1 d . . . C41 C 0.34838(17) 0.7878(2) 0.10621(11) 0.0757(10) Uani 1 1 d . . . H41A H 0.3674 0.7749 0.1295 0.091 Uiso 1 1 calc R . . C42 C 0.3105(2) 0.8589(3) 0.10224(15) 0.0934(13) Uani 1 1 d . . . H42A H 0.3053 0.8932 0.1224 0.112 Uiso 1 1 calc R . . C43 C 0.28062(18) 0.8790(3) 0.06875(15) 0.0907(13) Uani 1 1 d . . . H43A H 0.2538 0.9252 0.0662 0.109 Uiso 1 1 calc R . . C44 C 0.29042(17) 0.8306(3) 0.03914(13) 0.0898(13) Uani 1 1 d . . . H44A H 0.2712 0.8446 0.0161 0.108 Uiso 1 1 calc R . . C45 C 0.32954(16) 0.7599(3) 0.04375(12) 0.0794(11) Uani 1 1 d . . . H45A H 0.3358 0.7279 0.0232 0.095 Uiso 1 1 calc R . . C46 C 0.38770(14) 0.5720(2) 0.05043(9) 0.0552(8) Uani 1 1 d . . . C47 C 0.33146(15) 0.5494(2) 0.03682(10) 0.0689(10) Uani 1 1 d . . . H47A H 0.3024 0.5806 0.0456 0.083 Uiso 1 1 calc R . . C48 C 0.31665(17) 0.4826(3) 0.01084(11) 0.0818(12) Uani 1 1 d . . . H48A H 0.2784 0.4716 0.0019 0.098 Uiso 1 1 calc R . . C49 C 0.35847(18) 0.4327(3) -0.00171(11) 0.0800(11) Uani 1 1 d . . . H49A H 0.3489 0.3875 -0.0190 0.096 Uiso 1 1 calc R . . C50 C 0.41393(17) 0.4506(2) 0.01161(10) 0.0714(10) Uani 1 1 d . . . H50A H 0.4426 0.4163 0.0039 0.086 Uiso 1 1 calc R . . C51 C 0.42810(15) 0.5194(2) 0.03660(9) 0.0632(9) Uani 1 1 d . . . H51A H 0.4665 0.5312 0.0446 0.076 Uiso 1 1 calc R . . C52 C 0.30009(13) 0.2351(2) 0.19393(8) 0.0529(8) Uani 1 1 d . . . C53 C 0.34435(14) 0.2421(2) 0.22330(9) 0.0608(9) Uani 1 1 d . . . H53A H 0.3683 0.1928 0.2291 0.073 Uiso 1 1 calc R . . C54 C 0.35416(16) 0.3205(3) 0.24438(9) 0.0706(10) Uani 1 1 d . . . H54A H 0.3847 0.3229 0.2634 0.085 Uiso 1 1 calc R . . C55 C 0.31903(18) 0.3936(3) 0.23721(10) 0.0743(11) Uani 1 1 d . . . H55A H 0.3249 0.4451 0.2516 0.089 Uiso 1 1 calc R . . C56 C 0.27484(17) 0.3898(2) 0.20843(11) 0.0744(10) Uani 1 1 d . . . H56A H 0.2506 0.4390 0.2032 0.089 Uiso 1 1 calc R . . C57 C 0.26655(15) 0.3128(2) 0.18728(9) 0.0636(9) Uani 1 1 d . . . H57A H 0.2371 0.3126 0.1676 0.076 Uiso 1 1 calc R . . C58 C 0.29689(14) 0.1768(2) 0.12655(9) 0.0569(8) Uani 1 1 d . . . C59 C 0.34486(16) 0.2284(2) 0.12216(10) 0.0678(9) Uani 1 1 d . . . H59A H 0.3696 0.2450 0.1430 0.081 Uiso 1 1 calc R . . C60 C 0.35768(18) 0.2561(3) 0.08882(11) 0.0761(10) Uani 1 1 d . . . H60A H 0.3901 0.2907 0.0877 0.091 Uiso 1 1 calc R . . C61 C 0.3224(2) 0.2323(3) 0.05737(11) 0.0826(12) Uani 1 1 d . . . H61A H 0.3307 0.2499 0.0347 0.099 Uiso 1 1 calc R . . C62 C 0.2751(2) 0.1826(3) 0.05990(10) 0.0824(12) Uani 1 1 d . . . H62A H 0.2507 0.1664 0.0388 0.099 Uiso 1 1 calc R . . C63 C 0.26239(16) 0.1554(2) 0.09379(10) 0.0714(10) Uani 1 1 d . . . H63A H 0.2296 0.1216 0.0945 0.086 Uiso 1 1 calc R . . C64 C 0.22203(14) 0.1076(2) 0.16948(10) 0.0632(9) Uani 1 1 d . . . C65 C 0.18607(15) 0.1407(2) 0.19248(11) 0.0737(10) Uani 1 1 d . . . H65A H 0.1974 0.1918 0.2062 0.088 Uiso 1 1 calc R . . C66 C 0.13388(18) 0.1014(3) 0.19612(14) 0.0995(16) Uani 1 1 d . . . H66A H 0.1113 0.1264 0.2119 0.119 Uiso 1 1 calc R . . C67 C 0.1160(2) 0.0257(4) 0.17623(19) 0.123(2) Uani 1 1 d . . . H67A H 0.0809 -0.0004 0.1779 0.148 Uiso 1 1 calc R . . C68 C 0.1509(2) -0.0103(3) 0.15407(18) 0.118(2) Uani 1 1 d . . . H68A H 0.1398 -0.0628 0.1412 0.142 Uiso 1 1 calc R . . C69 C 0.20227(17) 0.0293(3) 0.15027(13) 0.0874(13) Uani 1 1 d . . . H69A H 0.2245 0.0033 0.1345 0.105 Uiso 1 1 calc R . . C70 C 0.32996(13) 0.0621(2) 0.18264(8) 0.0565(8) Uani 1 1 d . . . C71 C 0.31703(16) 0.0049(3) 0.21000(10) 0.0775(11) Uani 1 1 d . . . H71A H 0.2841 0.0163 0.2200 0.093 Uiso 1 1 calc R . . C72 C 0.35059(19) -0.0681(3) 0.22315(11) 0.0885(12) Uani 1 1 d . . . H72A H 0.3397 -0.1049 0.2412 0.106 Uiso 1 1 calc R . . C73 C 0.3997(2) -0.0856(3) 0.20953(12) 0.0901(13) Uani 1 1 d . . . H73A H 0.4228 -0.1340 0.2183 0.108 Uiso 1 1 calc R . . C74 C 0.41423(19) -0.0313(3) 0.18300(12) 0.0931(13) Uani 1 1 d . . . H74A H 0.4477 -0.0426 0.1736 0.112 Uiso 1 1 calc R . . C75 C 0.37996(16) 0.0410(3) 0.16970(10) 0.0751(10) Uani 1 1 d . . . H75A H 0.3911 0.0766 0.1514 0.090 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 0.0417(2) 0.0438(2) 0.0529(3) -0.0032(2) 0.01023(18) 0.00069(19) N1 0.0424(13) 0.0515(15) 0.0500(14) 0.0087(12) 0.0040(11) 0.0013(11) N2 0.0506(15) 0.0575(16) 0.0760(19) 0.0106(14) -0.0046(13) -0.0095(13) N3 0.0717(18) 0.0514(16) 0.0761(19) 0.0166(15) -0.0146(15) -0.0091(14) N4 0.0628(16) 0.0518(16) 0.0568(16) 0.0020(13) -0.0087(13) -0.0003(13) N5 0.0562(17) 0.0722(19) 0.0645(17) -0.0290(15) 0.0172(14) -0.0085(14) N6 0.0607(18) 0.078(2) 0.112(3) -0.0414(19) 0.0210(17) 0.0077(16) N7 0.0488(16) 0.092(2) 0.092(2) -0.0400(19) 0.0115(15) 0.0006(15) N8 0.0532(15) 0.0523(15) 0.0652(17) -0.0197(13) 0.0179(13) 0.0001(12) N9 0.0499(14) 0.0545(16) 0.0575(16) -0.0007(13) 0.0150(12) -0.0030(12) N10 0.0436(14) 0.0689(18) 0.0597(16) 0.0059(14) 0.0125(12) 0.0012(13) B1 0.056(2) 0.050(2) 0.064(2) -0.0063(18) 0.0146(18) -0.0075(17) B2 0.053(2) 0.054(2) 0.059(2) -0.0049(18) 0.0002(17) -0.0004(17) C1 0.062(2) 0.068(2) 0.072(2) 0.0225(19) -0.0074(17) -0.0072(18) C2 0.068(2) 0.099(3) 0.071(2) 0.023(2) -0.0095(19) -0.004(2) C3 0.056(2) 0.084(3) 0.089(3) 0.013(2) -0.0129(19) -0.0103(19) C4 0.0430(16) 0.0479(17) 0.0481(17) -0.0036(14) 0.0080(13) -0.0014(13) C5 0.0521(17) 0.0474(18) 0.0506(18) 0.0017(15) 0.0095(14) 0.0017(14) C6 0.121(4) 0.073(3) 0.109(3) 0.037(3) -0.042(3) -0.015(3) C8 0.094(3) 0.072(3) 0.078(3) 0.010(2) -0.030(2) -0.005(2) C9 0.086(3) 0.119(4) 0.098(3) -0.068(3) 0.033(2) -0.026(3) C10 0.086(3) 0.110(4) 0.116(4) -0.067(3) 0.039(3) -0.020(3) C11 0.106(3) 0.071(3) 0.114(4) -0.037(3) 0.046(3) -0.003(2) C12 0.0527(19) 0.058(2) 0.072(2) -0.0198(17) 0.0250(17) -0.0026(16) C13 0.0479(17) 0.0540(18) 0.0612(19) -0.0101(16) 0.0128(14) -0.0031(15) C14 0.064(2) 0.127(4) 0.105(3) -0.061(3) 0.006(2) -0.014(2) C16 0.071(2) 0.085(3) 0.087(3) -0.045(2) 0.013(2) 0.003(2) C17 0.069(2) 0.066(2) 0.078(2) 0.0012(19) 0.0334(19) 0.0023(18) C18 0.103(3) 0.082(3) 0.086(3) 0.025(2) 0.043(2) 0.003(2) C19 0.118(4) 0.077(3) 0.100(3) 0.033(2) 0.039(3) 0.028(3) C20 0.091(3) 0.064(2) 0.087(3) 0.009(2) 0.027(2) 0.019(2) C21 0.0455(16) 0.0469(18) 0.0593(19) -0.0039(15) 0.0038(14) 0.0019(14) C22 0.0374(15) 0.060(2) 0.0570(19) -0.0075(16) 0.0037(13) -0.0013(14) C23 0.062(2) 0.075(2) 0.076(2) -0.010(2) 0.0220(18) 0.0089(18) C24 0.072(2) 0.113(4) 0.071(3) -0.016(3) 0.024(2) 0.014(2) C25 0.070(2) 0.130(4) 0.061(2) 0.009(3) 0.0231(19) 0.007(3) C26 0.061(2) 0.096(3) 0.076(2) 0.023(2) 0.0184(19) 0.006(2) C28 0.0484(17) 0.058(2) 0.067(2) -0.0083(17) 0.0182(15) -0.0055(15) C29 0.0483(17) 0.054(2) 0.074(2) -0.0005(17) 0.0164(16) 0.0023(15) C30 0.062(2) 0.063(2) 0.090(3) 0.014(2) 0.020(2) 0.0021(18) C31 0.082(3) 0.092(3) 0.072(3) 0.014(2) 0.022(2) 0.000(2) C32 0.087(3) 0.106(3) 0.067(3) -0.011(2) 0.017(2) -0.014(3) C33 0.076(2) 0.073(2) 0.070(2) -0.005(2) 0.0174(19) -0.0185(19) C34 0.063(2) 0.0407(17) 0.067(2) -0.0084(15) 0.0221(16) -0.0062(15) C35 0.065(2) 0.0446(18) 0.091(3) -0.0002(18) 0.0235(19) -0.0006(16) C36 0.059(2) 0.057(2) 0.117(3) -0.010(2) 0.025(2) -0.0002(17) C37 0.075(3) 0.071(3) 0.111(3) -0.018(2) 0.046(2) -0.015(2) C38 0.104(3) 0.071(3) 0.075(3) 0.001(2) 0.039(2) -0.025(2) C39 0.074(2) 0.060(2) 0.065(2) -0.0046(18) 0.0163(18) -0.0094(18) C40 0.0571(19) 0.0523(19) 0.076(2) -0.0140(18) 0.0179(17) -0.0080(15) C41 0.087(3) 0.060(2) 0.085(3) -0.010(2) 0.032(2) -0.001(2) C42 0.104(3) 0.069(3) 0.117(4) -0.026(3) 0.046(3) 0.006(2) C43 0.075(3) 0.067(3) 0.133(4) -0.016(3) 0.023(3) 0.012(2) C44 0.071(2) 0.077(3) 0.114(3) -0.014(3) -0.011(2) 0.008(2) C45 0.074(2) 0.070(2) 0.090(3) -0.025(2) 0.000(2) 0.011(2) C46 0.064(2) 0.0448(17) 0.0604(19) -0.0001(15) 0.0212(16) -0.0056(15) C47 0.066(2) 0.067(2) 0.078(2) -0.0216(19) 0.0262(18) -0.0141(18) C48 0.079(3) 0.083(3) 0.087(3) -0.029(2) 0.027(2) -0.030(2) C49 0.102(3) 0.064(2) 0.082(3) -0.026(2) 0.037(2) -0.024(2) C50 0.090(3) 0.051(2) 0.079(2) -0.0121(19) 0.031(2) 0.0005(19) C51 0.073(2) 0.0478(19) 0.070(2) -0.0050(17) 0.0166(18) 0.0005(16) C52 0.0475(17) 0.058(2) 0.0546(19) -0.0035(15) 0.0134(14) -0.0088(15) C53 0.0573(19) 0.072(2) 0.0542(19) -0.0045(17) 0.0138(16) -0.0141(17) C54 0.075(2) 0.089(3) 0.0492(19) -0.009(2) 0.0145(17) -0.036(2) C55 0.100(3) 0.061(2) 0.068(2) -0.013(2) 0.032(2) -0.028(2) C56 0.089(3) 0.056(2) 0.081(3) -0.008(2) 0.022(2) -0.009(2) C57 0.066(2) 0.058(2) 0.065(2) -0.0062(17) 0.0048(17) -0.0091(17) C58 0.0621(19) 0.0472(18) 0.059(2) -0.0099(15) 0.0006(16) 0.0024(15) C59 0.075(2) 0.066(2) 0.062(2) -0.0046(18) 0.0070(18) -0.0060(19) C60 0.092(3) 0.065(2) 0.076(3) -0.002(2) 0.026(2) 0.002(2) C61 0.119(4) 0.068(3) 0.064(3) -0.006(2) 0.025(2) 0.018(3) C62 0.113(3) 0.072(3) 0.056(2) -0.016(2) -0.007(2) 0.011(2) C63 0.079(2) 0.057(2) 0.073(2) -0.0135(19) -0.0041(19) -0.0030(18) C64 0.0522(18) 0.0512(19) 0.081(2) 0.0106(18) -0.0050(17) 0.0003(16) C65 0.057(2) 0.060(2) 0.102(3) 0.026(2) 0.007(2) 0.0008(17) C66 0.065(2) 0.094(3) 0.140(4) 0.062(3) 0.018(3) 0.005(2) C67 0.059(3) 0.108(4) 0.190(6) 0.079(4) -0.019(3) -0.026(3) C68 0.091(4) 0.073(3) 0.170(6) 0.035(3) -0.043(4) -0.034(3) C69 0.076(3) 0.059(2) 0.117(3) 0.003(2) -0.018(2) -0.011(2) C70 0.0554(19) 0.060(2) 0.0510(18) -0.0071(16) -0.0014(15) -0.0022(15) C71 0.066(2) 0.093(3) 0.072(2) 0.013(2) 0.0068(19) 0.010(2) C72 0.089(3) 0.096(3) 0.076(3) 0.023(2) 0.000(2) 0.005(3) C73 0.098(3) 0.085(3) 0.082(3) 0.005(2) -0.001(2) 0.031(3) C74 0.088(3) 0.103(3) 0.091(3) 0.005(3) 0.024(2) 0.037(3) C75 0.075(2) 0.079(3) 0.074(2) 0.008(2) 0.0172(19) 0.014(2) _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 N5 2.094(3) . ? Fe1 N8 2.107(3) . ? Fe1 N10 2.116(3) . ? Fe1 N4 2.117(3) . ? Fe1 N1 2.127(2) . ? Fe1 N9 2.151(3) . ? N1 C4 1.297(4) . ? N1 C1 1.455(4) . ? N2 C4 1.334(4) . ? N2 C3 1.451(4) . ? N2 H2A 0.8600 . ? N3 C5 1.344(4) . ? N3 C6 1.456(4) . ? N3 H3A 0.8600 . ? N4 C5 1.281(4) . ? N4 C8 1.462(4) . ? N5 C12 1.294(4) . ? N5 C9 1.471(4) . ? N6 C12 1.335(4) . ? N6 C11 1.460(5) . ? N6 H6E 0.8600 . ? N7 C13 1.337(4) . ? N7 C14 1.457(4) . ? N7 H7E 0.8600 . ? N8 C13 1.286(4) . ? N8 C16 1.462(4) . ? N9 C17 1.345(4) . ? N9 C21 1.356(4) . ? N10 C22 1.338(4) . ? N10 C26 1.341(4) . ? B1 C46 1.646(5) . ? B1 C28 1.646(5) . ? B1 C40 1.651(5) . ? B1 C34 1.655(5) . ? B2 C52 1.635(5) . ? B2 C64 1.649(5) . ? B2 C70 1.651(5) . ? B2 C58 1.655(5) . ? C1 C2 1.492(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.478(5) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.498(4) . ? C6 C7B 1.361(7) . ? C6 C7A 1.419(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7A C8 1.378(10) . ? C7A H7A 0.9700 . ? C7A H7B 0.9700 . ? C7B C8 1.555(8) . ? C7B H7C 0.9700 . ? C7B H7D 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C9 C10 1.486(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.508(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.499(4) . ? C14 C15B 1.407(9) . ? C14 C15A 1.513(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C14 H14D 0.9700 . ? C15A C16 1.472(8) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C15B C16 1.501(9) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C16 H16D 0.9700 . ? C17 C27A 1.435(8) . ? C17 H17B 0.9300 . ? C18 C19 1.350(5) . ? C18 H18A 0.9300 . ? C19 C20 1.375(5) . ? C19 H19A 0.9300 . ? C20 C21 1.368(5) . ? C20 H20A 0.9300 . ? C21 C22 1.473(4) . ? C22 C23 1.382(4) . ? C23 C24 1.366(5) . ? C23 H23A 0.9300 . ? C24 C25 1.348(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27B 1.42(3) . ? C26 H26A 0.9300 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28 C29 1.387(4) . ? C28 C33 1.394(5) . ? C29 C30 1.385(5) . ? C29 H29A 0.9300 . ? C30 C31 1.379(5) . ? C30 H30A 0.9300 . ? C31 C32 1.373(5) . ? C31 H31A 0.9300 . ? C32 C33 1.380(5) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.388(5) . ? C34 C39 1.395(4) . ? C35 C36 1.389(5) . ? C35 H35A 0.9300 . ? C36 C37 1.371(5) . ? C36 H36A 0.9300 . ? C37 C38 1.364(6) . ? C37 H37A 0.9300 . ? C38 C39 1.387(5) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.394(5) . ? C40 C45 1.395(5) . ? C41 C42 1.378(5) . ? C41 H41A 0.9300 . ? C42 C43 1.365(6) . ? C42 H42A 0.9300 . ? C43 C44 1.362(6) . ? C43 H43A 0.9300 . ? C44 C45 1.393(5) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C47 1.392(5) . ? C46 C51 1.394(4) . ? C47 C48 1.389(5) . ? C47 H47A 0.9300 . ? C48 C49 1.376(5) . ? C48 H48A 0.9300 . ? C49 C50 1.358(5) . ? C49 H49A 0.9300 . ? C50 C51 1.385(5) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 C53 1.395(4) . ? C52 C57 1.401(5) . ? C53 C54 1.401(5) . ? C53 H53A 0.9300 . ? C54 C55 1.368(5) . ? C54 H54A 0.9300 . ? C55 C56 1.377(5) . ? C55 H55A 0.9300 . ? C56 C57 1.382(5) . ? C56 H56A 0.9300 . ? C57 H57A 0.9300 . ? C58 C63 1.392(4) . ? C58 C59 1.401(5) . ? C59 C60 1.381(5) . ? C59 H59A 0.9300 . ? C60 C61 1.373(5) . ? C60 H60A 0.9300 . ? C61 C62 1.359(6) . ? C61 H61A 0.9300 . ? C62 C63 1.397(5) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C64 C65 1.387(5) . ? C64 C69 1.404(5) . ? C65 C66 1.393(5) . ? C65 H65A 0.9300 . ? C66 C67 1.374(7) . ? C66 H66A 0.9300 . ? C67 C68 1.362(8) . ? C67 H67A 0.9300 . ? C68 C69 1.381(6) . ? C68 H68A 0.9300 . ? C69 H69A 0.9300 . ? C70 C75 1.383(5) . ? C70 C71 1.392(5) . ? C71 C72 1.387(5) . ? C71 H71A 0.9300 . ? C72 C73 1.364(6) . ? C72 H72A 0.9300 . ? C73 C74 1.357(6) . ? C73 H73A 0.9300 . ? C74 C75 1.389(5) . ? C74 H74A 0.9300 . ? C75 H75A 0.9300 . ? 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 N5 Fe1 N8 76.79(10) . . ? N5 Fe1 N10 172.14(10) . . ? N8 Fe1 N10 95.45(10) . . ? N5 Fe1 N4 86.34(11) . . ? N8 Fe1 N4 99.16(10) . . ? N10 Fe1 N4 93.75(11) . . ? N5 Fe1 N1 96.86(10) . . ? N8 Fe1 N1 172.74(9) . . ? N10 Fe1 N1 90.81(10) . . ? N4 Fe1 N1 76.70(9) . . ? N5 Fe1 N9 104.74(11) . . ? N8 Fe1 N9 92.09(10) . . ? N10 Fe1 N9 76.50(10) . . ? N4 Fe1 N9 165.81(10) . . ? N1 Fe1 N9 92.95(9) . . ? C4 N1 C1 117.1(2) . . ? C4 N1 Fe1 114.51(19) . . ? C1 N1 Fe1 126.2(2) . . ? C4 N2 C3 121.4(3) . . ? C4 N2 H2A 119.3 . . ? C3 N2 H2A 119.3 . . ? C5 N3 C6 119.5(3) . . ? C5 N3 H3A 120.3 . . ? C6 N3 H3A 120.3 . . ? C5 N4 C8 117.7(3) . . ? C5 N4 Fe1 114.9(2) . . ? C8 N4 Fe1 124.5(2) . . ? C12 N5 C9 117.6(3) . . ? C12 N5 Fe1 115.2(2) . . ? C9 N5 Fe1 124.6(2) . . ? C12 N6 C11 121.3(3) . . ? C12 N6 H6E 119.4 . . ? C11 N6 H6E 119.4 . . ? C13 N7 C14 120.9(3) . . ? C13 N7 H7E 119.5 . . ? C14 N7 H7E 119.5 . . ? C13 N8 C16 117.2(3) . . ? C13 N8 Fe1 115.9(2) . . ? C16 N8 Fe1 126.0(2) . . ? C17 N9 C21 117.8(3) . . ? C17 N9 Fe1 127.5(2) . . ? C21 N9 Fe1 114.57(19) . . ? C22 N10 C26 117.9(3) . . ? C22 N10 Fe1 117.0(2) . . ? C26 N10 Fe1 125.0(3) . . ? C46 B1 C28 109.0(3) . . ? C46 B1 C40 111.4(3) . . ? C28 B1 C40 109.9(3) . . ? C46 B1 C34 106.6(3) . . ? C28 B1 C34 109.7(3) . . ? C40 B1 C34 110.2(3) . . ? C52 B2 C64 110.8(3) . . ? C52 B2 C70 111.2(3) . . ? C64 B2 C70 105.1(3) . . ? C52 B2 C58 106.4(3) . . ? C64 B2 C58 113.4(3) . . ? C70 B2 C58 110.0(3) . . ? N1 C1 C2 113.0(3) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 112.3(3) . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2C 109.1 . . ? C1 C2 H2C 109.1 . . ? H2B C2 H2C 107.9 . . ? N2 C3 C2 109.0(3) . . ? N2 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? N2 C3 H3C 109.9 . . ? C2 C3 H3C 109.9 . . ? H3B C3 H3C 108.3 . . ? N1 C4 N2 126.2(3) . . ? N1 C4 C5 115.1(3) . . ? N2 C4 C5 118.6(3) . . ? N4 C5 N3 126.6(3) . . ? N4 C5 C4 115.3(3) . . ? N3 C5 C4 118.1(3) . . ? C7B C6 N3 112.9(4) . . ? C7A C6 N3 112.5(5) . . ? C7B C6 H6A 76.5 . . ? C7A C6 H6A 109.1 . . ? N3 C6 H6A 109.1 . . ? C7B C6 H6B 133.4 . . ? C7A C6 H6B 109.1 . . ? N3 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C7B C6 H6C 108.1 . . ? C7A C6 H6C 133.5 . . ? N3 C6 H6C 108.8 . . ? H6B C6 H6C 75.4 . . ? C7B C6 H6D 110.2 . . ? C7A C6 H6D 78.1 . . ? N3 C6 H6D 108.9 . . ? H6A C6 H6D 134.3 . . ? H6C C6 H6D 107.7 . . ? C8 C7A C6 121.4(8) . . ? C8 C7A H6D 140.8 . . ? C8 C7A H7A 107.0 . . ? C6 C7A H7A 107.0 . . ? H6D C7A H7A 111.3 . . ? C8 C7A H7B 107.0 . . ? C6 C7A H7B 107.0 . . ? H6D C7A H7B 69.7 . . ? H7A C7A H7B 106.7 . . ? C6 C7A H8D 142.1 . . ? H6D C7A H8D 128.0 . . ? H7A C7A H8D 110.1 . . ? H7B C7A H8D 69.3 . . ? C6 C7B C8 113.4(6) . . ? C6 C7B H7C 108.9 . . ? C8 C7B H7C 108.9 . . ? C6 C7B H7D 108.9 . . ? C8 C7B H7D 108.9 . . ? H7C C7B H7D 107.7 . . ? C7A C8 N4 115.9(5) . . ? N4 C8 C7B 112.2(4) . . ? C7A C8 H8A 108.3 . . ? N4 C8 H8A 108.3 . . ? C7B C8 H8A 133.9 . . ? C7A C8 H8B 108.3 . . ? N4 C8 H8B 108.3 . . ? C7B C8 H8B 79.9 . . ? H8A C8 H8B 107.4 . . ? C7A C8 H8C 129.1 . . ? N4 C8 H8C 109.1 . . ? C7B C8 H8C 108.3 . . ? H8A C8 H8C 77.3 . . ? C7A C8 H8D 79.0 . . ? N4 C8 H8D 109.2 . . ? C7B C8 H8D 110.2 . . ? H8B C8 H8D 133.1 . . ? H8C C8 H8D 107.8 . . ? N5 C9 C10 112.1(3) . . ? N5 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N5 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 111.6(4) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? N6 C11 C10 108.5(3) . . ? N6 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N6 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N5 C12 N6 126.3(3) . . ? N5 C12 C13 115.1(3) . . ? N6 C12 C13 118.5(3) . . ? N8 C13 N7 126.5(3) . . ? N8 C13 C12 114.7(3) . . ? N7 C13 C12 118.8(3) . . ? C15B C14 N7 111.4(5) . . ? N7 C14 C15A 108.9(4) . . ? C15B C14 H14A 136.6 . . ? N7 C14 H14A 109.9 . . ? C15A C14 H14A 109.9 . . ? C15B C14 H14B 68.8 . . ? N7 C14 H14B 109.9 . . ? C15A C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C15B C14 H14C 111.5 . . ? N7 C14 H14C 109.5 . . ? C15A C14 H14C 140.4 . . ? H14A C14 H14C 65.0 . . ? H14B C14 H14C 46.5 . . ? C15B C14 H14D 106.5 . . ? N7 C14 H14D 109.7 . . ? C15A C14 H14D 67.0 . . ? H14A C14 H14D 45.8 . . ? H14B C14 H14D 138.7 . . ? H14C C14 H14D 108.1 . . ? C16 C15A C14 111.2(6) . . ? C16 C15A H14D 142.8 . . ? C16 C15A H15A 109.4 . . ? C14 C15A H15A 109.4 . . ? H14D C15A H15A 103.0 . . ? C16 C15A H15B 109.4 . . ? C14 C15A H15B 109.4 . . ? H14D C15A H15B 76.4 . . ? H15A C15A H15B 108.0 . . ? C14 C15A H16D 142.2 . . ? H14D C15A H16D 144.7 . . ? H15A C15A H16D 104.5 . . ? H15B C15A H16D 74.3 . . ? C14 C15B C16 115.7(7) . . ? C14 C15B H15C 108.4 . . ? C16 C15B H15C 108.4 . . ? C14 C15B H15D 108.4 . . ? C16 C15B H15D 108.4 . . ? H15C C15B H15D 107.4 . . ? N8 C16 C15A 114.6(4) . . ? N8 C16 C15B 112.9(4) . . ? N8 C16 H16A 108.6 . . ? C15A C16 H16A 108.6 . . ? C15B C16 H16A 69.4 . . ? N8 C16 H16B 108.6 . . ? C15A C16 H16B 108.6 . . ? C15B C16 H16B 137.0 . . ? H16A C16 H16B 107.6 . . ? N8 C16 H16C 109.4 . . ? C15A C16 H16C 135.1 . . ? C15B C16 H16C 110.9 . . ? H16A C16 H16C 46.2 . . ? H16B C16 H16C 63.6 . . ? N8 C16 H16D 109.3 . . ? C15A C16 H16D 65.7 . . ? C15B C16 H16D 106.3 . . ? H16A C16 H16D 140.0 . . ? H16B C16 H16D 47.4 . . ? H16C C16 H16D 107.9 . . ? N9 C17 C18 122.2(3) . . ? N9 C17 C27A 120.6(4) . . ? C18 C17 C27A 117.1(4) . . ? N9 C17 H17B 118.9 . . ? C18 C17 H17B 118.9 . . ? C19 C18 C17 119.6(4) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 119.0(4) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? N9 C21 C20 121.4(3) . . ? N9 C21 C22 116.0(3) . . ? C20 C21 C22 122.5(3) . . ? N10 C22 C23 121.6(3) . . ? N10 C22 C21 115.3(3) . . ? C23 C22 C21 123.1(3) . . ? C24 C23 C22 119.1(4) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 118.7(4) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? N10 C26 C25 122.7(4) . . ? N10 C26 C27B 126.8(12) . . ? C25 C26 C27B 106.9(12) . . ? N10 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C17 C27A H27A 109.5 . . ? C17 C27A H27B 109.5 . . ? C17 C27A H27C 109.5 . . ? C26 C27B H27D 109.5 . . ? C26 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C29 C28 C33 114.5(3) . . ? C29 C28 B1 123.7(3) . . ? C33 C28 B1 121.8(3) . . ? C30 C29 C28 123.1(3) . . ? C30 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? C31 C30 C29 120.3(4) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 118.4(4) . . ? C32 C31 H31A 120.8 . . ? C30 C31 H31A 120.8 . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C32 C33 C28 123.4(4) . . ? C32 C33 H33A 118.3 . . ? C28 C33 H33A 118.3 . . ? C35 C34 C39 114.8(3) . . ? C35 C34 B1 122.9(3) . . ? C39 C34 B1 121.8(3) . . ? C34 C35 C36 123.4(3) . . ? C34 C35 H35A 118.3 . . ? C36 C35 H35A 118.3 . . ? C37 C36 C35 119.6(4) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C38 C37 C36 119.0(4) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C37 C38 C39 120.9(4) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C39 C34 122.3(4) . . ? C38 C39 H39A 118.9 . . ? C34 C39 H39A 118.9 . . ? C41 C40 C45 113.2(3) . . ? C41 C40 B1 124.4(3) . . ? C45 C40 B1 122.4(3) . . ? C42 C41 C40 123.9(4) . . ? C42 C41 H41A 118.1 . . ? C40 C41 H41A 118.1 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? C44 C43 C42 119.3(4) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C43 C44 C45 119.4(4) . . ? C43 C44 H44A 120.3 . . ? C45 C44 H44A 120.3 . . ? C44 C45 C40 123.9(4) . . ? C44 C45 H45A 118.0 . . ? C40 C45 H45A 118.0 . . ? C47 C46 C51 114.0(3) . . ? C47 C46 B1 123.9(3) . . ? C51 C46 B1 122.0(3) . . ? C48 C47 C46 123.3(3) . . ? C48 C47 H47A 118.4 . . ? C46 C47 H47A 118.4 . . ? C49 C48 C47 120.0(4) . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C50 C49 C48 118.7(3) . . ? C50 C49 H49A 120.6 . . ? C48 C49 H49A 120.6 . . ? C49 C50 C51 120.6(3) . . ? C49 C50 H50A 119.7 . . ? C51 C50 H50A 119.7 . . ? C50 C51 C46 123.3(3) . . ? C50 C51 H51A 118.3 . . ? C46 C51 H51A 118.3 . . ? C53 C52 C57 114.5(3) . . ? C53 C52 B2 125.0(3) . . ? C57 C52 B2 120.5(3) . . ? C52 C53 C54 122.5(4) . . ? C52 C53 H53A 118.7 . . ? C54 C53 H53A 118.7 . . ? C55 C54 C53 120.4(3) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 119.1(3) . . ? C54 C55 H55A 120.4 . . ? C56 C55 H55A 120.4 . . ? C55 C56 C57 119.9(4) . . ? C55 C56 H56A 120.1 . . ? C57 C56 H56A 120.1 . . ? C56 C57 C52 123.6(3) . . ? C56 C57 H57A 118.2 . . ? C52 C57 H57A 118.2 . . ? C63 C58 C59 113.6(3) . . ? C63 C58 B2 126.7(3) . . ? C59 C58 B2 119.7(3) . . ? C60 C59 C58 124.2(3) . . ? C60 C59 H59A 117.9 . . ? C58 C59 H59A 117.9 . . ? C61 C60 C59 119.7(4) . . ? C61 C60 H60A 120.2 . . ? C59 C60 H60A 120.2 . . ? C62 C61 C60 118.9(4) . . ? C62 C61 H61A 120.6 . . ? C60 C61 H61A 120.6 . . ? C61 C62 C63 120.9(4) . . ? C61 C62 H62A 119.5 . . ? C63 C62 H62A 119.5 . . ? C58 C63 C62 122.7(4) . . ? C58 C63 H63A 118.6 . . ? C62 C63 H63A 118.6 . . ? C65 C64 C69 114.6(3) . . ? C65 C64 B2 124.3(3) . . ? C69 C64 B2 120.6(3) . . ? C64 C65 C66 123.6(4) . . ? C64 C65 H65A 118.2 . . ? C66 C65 H65A 118.2 . . ? C67 C66 C65 119.6(5) . . ? C67 C66 H66A 120.2 . . ? C65 C66 H66A 120.2 . . ? C68 C67 C66 118.6(5) . . ? C68 C67 H67A 120.7 . . ? C66 C67 H67A 120.7 . . ? C67 C68 C69 121.6(5) . . ? C67 C68 H68A 119.2 . . ? C69 C68 H68A 119.2 . . ? C68 C69 C64 122.0(5) . . ? C68 C69 H69A 119.0 . . ? C64 C69 H69A 119.0 . . ? C75 C70 C71 114.4(3) . . ? C75 C70 B2 125.3(3) . . ? C71 C70 B2 120.3(3) . . ? C72 C71 C70 123.5(4) . . ? C72 C71 H71A 118.2 . . ? C70 C71 H71A 118.2 . . ? C73 C72 C71 119.6(4) . . ? C73 C72 H72A 120.2 . . ? C71 C72 H72A 120.2 . . ? C74 C73 C72 118.9(4) . . ? C74 C73 H73A 120.5 . . ? C72 C73 H73A 120.5 . . ? C73 C74 C75 121.0(4) . . ? C73 C74 H74A 119.5 . . ? C75 C74 H74A 119.5 . . ? C70 C75 C74 122.5(4) . . ? C70 C75 H75A 118.7 . . ? C74 C75 H75A 118.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.364 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.041