Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email JASON.LOVE@NOTTINGHAM.AC.UK _publ_contact_author_name 'Dr Jason Love' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_section_title ; Double-stranded, [4+4] helicates of Fe(II) and Mn(II) supported by an extended dipyrrolide ligand ; loop_ _publ_author_name 'Jason Love' 'Alexander J. Blake' 'Walter Kockenberger' 'Stuart D. Reid' 'Claire Wilson' data_MNPYBU _database_code_depnum_ccdc_archive 'CCDC 219487' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H62 Mn N8, 2(C4 H8 O)' _chemical_formula_sum 'C50 H78 Mn N8 O2' _chemical_formula_weight 878.14 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 17.635(2) _cell_length_b 14.208(2) _cell_length_c 21.382(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.152(2) _cell_angle_gamma 90.00 _cell_volume 5030(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5104 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.3 _exptl_crystal_description sphenoid _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(SADABS version 2.03; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17490 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.028 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5926 _reflns_number_gt 4797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _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^)+(0.071P)^2^+4.88P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5695 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.134 _refine_ls_wR_factor_gt 0.126 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 Mn1 Mn 0.5000 0.46757(3) 0.2500 0.02547(12) Uani 1 2 d S . . N1 N 0.41595(9) 0.33802(11) 0.18281(7) 0.0300(3) Uani 1 1 d . . . N2 N 0.39342(9) 0.45764(10) 0.27588(7) 0.0269(3) Uani 1 1 d . . . N3 N 0.54508(9) 0.56032(11) 0.34781(7) 0.0294(3) Uani 1 1 d . . . N4 N 0.76611(10) 0.54949(13) 0.41288(8) 0.0408(4) Uani 1 1 d . . . H4A H 0.7752 0.5682 0.4531 0.049 Uiso 1 1 calc R . . C1 C 0.33948(15) 0.2596(3) 0.07524(13) 0.0706(9) Uani 1 1 d . . . H1A H 0.3154 0.3187 0.0571 0.106 Uiso 1 1 calc R . . H1B H 0.3054 0.2278 0.0951 0.106 Uiso 1 1 calc R . . H1C H 0.3456 0.2213 0.0403 0.106 Uiso 1 1 calc R . . C2 C 0.46304(18) 0.18485(17) 0.15851(14) 0.0594(7) Uani 1 1 d . . . H2A H 0.4299 0.1523 0.1790 0.089 Uiso 1 1 calc R . . H2B H 0.5147 0.1984 0.1915 0.089 Uiso 1 1 calc R . . H2C H 0.4703 0.1460 0.1243 0.089 Uiso 1 1 calc R . . C3 C 0.47500(13) 0.32762(15) 0.09564(10) 0.0399(5) Uani 1 1 d . . . H3A H 0.4496 0.3855 0.0762 0.060 Uiso 1 1 calc R . . H3B H 0.4823 0.2884 0.0616 0.060 Uiso 1 1 calc R . . H3C H 0.5266 0.3409 0.1288 0.060 Uiso 1 1 calc R . . C4 C 0.42187(12) 0.27698(15) 0.12786(10) 0.0374(4) Uani 1 1 d . . . C5 C 0.36242(11) 0.31738(14) 0.20855(9) 0.0330(4) Uani 1 1 d . . . H5A H 0.3307 0.2640 0.1940 0.040 Uiso 1 1 calc R . . C6 C 0.35052(11) 0.37520(14) 0.25944(9) 0.0314(4) Uani 1 1 d . . . C7 C 0.30101(12) 0.36401(16) 0.29733(10) 0.0393(5) Uani 1 1 d . . . H7A H 0.2660 0.3142 0.2953 0.047 Uiso 1 1 calc R . . C8 C 0.31443(12) 0.44273(15) 0.33917(10) 0.0377(4) Uani 1 1 d . . . H8A H 0.2904 0.4553 0.3707 0.045 Uiso 1 1 calc R . . C9 C 0.37106(10) 0.49860(14) 0.32421(8) 0.0293(4) Uani 1 1 d . . . C10 C 0.40695(11) 0.59248(13) 0.35204(9) 0.0308(4) Uani 1 1 d . . . C11 C 0.37079(12) 0.62686(16) 0.40379(10) 0.0414(5) Uani 1 1 d . . . H11A H 0.3820 0.5817 0.4392 0.062 Uiso 1 1 calc R . . H11B H 0.3134 0.6340 0.3830 0.062 Uiso 1 1 calc R . . H11C H 0.3944 0.6863 0.4215 0.062 Uiso 1 1 calc R . . C12 C 0.38809(12) 0.66594(14) 0.29557(10) 0.0377(4) Uani 1 1 d . . . H12A H 0.4103 0.6453 0.2627 0.057 Uiso 1 1 calc R . . H12B H 0.4116 0.7253 0.3136 0.057 Uiso 1 1 calc R . . H12C H 0.3306 0.6729 0.2752 0.057 Uiso 1 1 calc R . . C13 C 0.49835(11) 0.58236(13) 0.38339(8) 0.0289(4) Uani 1 1 d . . . C14 C 0.54442(12) 0.59407(14) 0.45206(9) 0.0351(4) Uani 1 1 d . . . H14A H 0.5246 0.6084 0.4860 0.042 Uiso 1 1 calc R . . C15 C 0.62347(12) 0.58030(14) 0.45863(9) 0.0358(4) Uani 1 1 d . . . H15A H 0.6679 0.5837 0.4977 0.043 Uiso 1 1 calc R . . C16 C 0.62422(11) 0.55968(14) 0.39384(9) 0.0314(4) Uani 1 1 d . . . C17 C 0.68971(11) 0.54418(14) 0.37357(10) 0.0343(4) Uani 1 1 d . . . H17A H 0.6792 0.5289 0.3291 0.041 Uiso 1 1 calc R . . C18 C 0.83745(12) 0.52634(19) 0.39436(11) 0.0477(5) Uani 1 1 d . . . C19 C 0.82333(14) 0.5530(2) 0.32240(12) 0.0578(7) Uani 1 1 d . . . H19A H 0.7792 0.5168 0.2934 0.087 Uiso 1 1 calc R . . H19B H 0.8713 0.5404 0.3122 0.087 Uiso 1 1 calc R . . H19C H 0.8106 0.6188 0.3161 0.087 Uiso 1 1 calc R . . C20 C 0.85362(18) 0.4217(2) 0.40517(19) 0.0774(9) Uani 1 1 d . . . H20A H 0.8088 0.3871 0.3756 0.116 Uiso 1 1 calc R . . H20B H 0.8605 0.4060 0.4505 0.116 Uiso 1 1 calc R . . H20C H 0.9018 0.4058 0.3963 0.116 Uiso 1 1 calc R . . C21 C 0.90750(15) 0.5837(3) 0.44057(14) 0.0758(10) Uani 1 1 d . . . H21A H 0.8960 0.6496 0.4328 0.114 Uiso 1 1 calc R . . H21B H 0.9560 0.5687 0.4319 0.114 Uiso 1 1 calc R . . H21C H 0.9146 0.5690 0.4861 0.114 Uiso 1 1 calc R . . O1S O 0.68479(10) 0.90493(12) 0.44131(8) 0.0504(4) Uani 1 1 d . . . C1S C 0.63147(16) 0.96547(19) 0.39385(13) 0.0562(6) Uani 1 1 d . . . H1SA H 0.6615 1.0115 0.3783 0.067 Uiso 1 1 calc R . . H1SB H 0.5967 0.9985 0.4132 0.067 Uiso 1 1 calc R . . C2S C 0.5838(3) 0.9057(4) 0.3391(2) 0.134(2) Uani 1 1 d . . . H2SA H 0.5268 0.9204 0.3273 0.161 Uiso 1 1 calc R . . H2SB H 0.5993 0.9162 0.3003 0.161 Uiso 1 1 calc R . . C3S C 0.5978(3) 0.8125(3) 0.3596(2) 0.1196(17) Uani 1 1 d . . . H3SA H 0.6053 0.7743 0.3245 0.143 Uiso 1 1 calc R . . H3SB H 0.5523 0.7877 0.3700 0.143 Uiso 1 1 calc R . . C4S C 0.67018(19) 0.8108(2) 0.41827(16) 0.0709(8) Uani 1 1 d . . . H4SA H 0.6623 0.7707 0.4523 0.085 Uiso 1 1 calc R . . H4SB H 0.7155 0.7869 0.4072 0.085 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 Mn1 0.02335(18) 0.0310(2) 0.02432(19) 0.000 0.01104(14) 0.000 N1 0.0295(7) 0.0333(8) 0.0288(7) -0.0060(6) 0.0120(6) -0.0009(6) N2 0.0253(7) 0.0325(8) 0.0243(7) -0.0011(6) 0.0101(5) 0.0005(6) N3 0.0274(7) 0.0338(8) 0.0270(7) -0.0008(6) 0.0095(6) -0.0015(6) N4 0.0297(8) 0.0588(11) 0.0321(8) -0.0025(8) 0.0083(7) -0.0053(8) C1 0.0474(13) 0.116(3) 0.0504(14) -0.0445(16) 0.0192(11) -0.0241(15) C2 0.0915(19) 0.0378(12) 0.0677(16) -0.0078(11) 0.0515(15) 0.0002(12) C3 0.0474(11) 0.0435(11) 0.0347(10) -0.0095(8) 0.0218(9) -0.0056(9) C4 0.0394(10) 0.0414(11) 0.0365(10) -0.0156(8) 0.0195(8) -0.0090(9) C5 0.0310(9) 0.0337(10) 0.0352(9) -0.0055(7) 0.0125(7) -0.0064(8) C6 0.0273(8) 0.0360(10) 0.0320(9) -0.0014(7) 0.0118(7) -0.0036(7) C7 0.0342(9) 0.0476(12) 0.0422(11) -0.0054(9) 0.0207(8) -0.0107(9) C8 0.0344(9) 0.0499(12) 0.0349(10) -0.0022(8) 0.0198(8) -0.0018(9) C9 0.0260(8) 0.0378(10) 0.0255(8) 0.0000(7) 0.0107(6) 0.0035(7) C10 0.0317(9) 0.0356(10) 0.0268(8) -0.0026(7) 0.0120(7) 0.0037(7) C11 0.0389(10) 0.0517(13) 0.0373(10) -0.0099(9) 0.0178(8) 0.0053(9) C12 0.0403(10) 0.0351(10) 0.0359(10) 0.0011(8) 0.0108(8) 0.0058(8) C13 0.0329(9) 0.0290(9) 0.0258(8) -0.0020(7) 0.0114(7) -0.0017(7) C14 0.0390(10) 0.0412(11) 0.0257(9) -0.0036(7) 0.0120(7) -0.0017(8) C15 0.0359(9) 0.0428(11) 0.0261(9) -0.0017(8) 0.0071(7) -0.0055(8) C16 0.0303(9) 0.0343(10) 0.0277(9) -0.0001(7) 0.0077(7) -0.0035(7) C17 0.0310(9) 0.0386(11) 0.0314(9) 0.0007(8) 0.0084(7) -0.0044(8) C18 0.0279(9) 0.0715(16) 0.0441(12) 0.0055(11) 0.0128(8) -0.0022(10) C19 0.0381(11) 0.093(2) 0.0442(12) 0.0016(12) 0.0166(10) -0.0040(12) C20 0.0591(16) 0.082(2) 0.102(2) 0.0233(18) 0.0415(17) 0.0231(16) C21 0.0371(12) 0.136(3) 0.0520(15) -0.0051(17) 0.0121(11) -0.0250(15) O1S 0.0495(9) 0.0484(9) 0.0423(8) -0.0041(7) 0.0017(7) 0.0010(7) C1S 0.0554(14) 0.0555(15) 0.0569(15) 0.0101(11) 0.0183(12) 0.0141(11) C2S 0.120(3) 0.125(4) 0.088(3) 0.006(3) -0.052(3) 0.006(3) C3S 0.116(3) 0.082(3) 0.110(3) -0.032(2) -0.025(2) -0.031(2) C4S 0.0793(19) 0.0429(15) 0.080(2) -0.0006(13) 0.0134(15) 0.0010(13) _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 Mn1 N2 2.1390(14) . ? Mn1 N3 2.3659(15) . ? Mn1 N1 2.4863(15) . ? N1 C5 1.280(2) . ? N1 C4 1.493(2) . ? N2 C9 1.357(2) . ? N2 C6 1.373(2) . ? N3 C13 1.337(2) . ? N3 C16 1.404(2) . ? N4 C17 1.322(2) . ? N4 C18 1.480(3) . ? C1 C4 1.520(3) . ? C2 C4 1.530(3) . ? C3 C4 1.521(3) . ? C5 C6 1.435(3) . ? C6 C7 1.390(3) . ? C7 C8 1.401(3) . ? C8 C9 1.396(3) . ? C9 C10 1.508(3) . ? C10 C13 1.524(2) . ? C10 C11 1.535(2) . ? C10 C12 1.543(3) . ? C13 C14 1.422(2) . ? C14 C15 1.366(3) . ? C15 C16 1.420(3) . ? C16 C17 1.384(3) . ? C18 C20 1.516(4) . ? C18 C19 1.520(3) . ? C18 C21 1.525(4) . ? O1S C1S 1.413(3) . ? O1S C4S 1.418(3) . ? C1S C2S 1.457(5) . ? C2S C3S 1.390(6) . ? C3S C4S 1.449(5) . ? 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 Mn1 N2 172.44(8) 2_655 . ? N2 Mn1 N3 102.00(5) 2_655 . ? N2 Mn1 N3 82.28(5) . . ? N3 Mn1 N3 112.30(8) . 2_655 ? N2 Mn1 N1 101.75(5) 2_655 . ? N2 Mn1 N1 72.46(5) . . ? N3 Mn1 N1 151.05(5) . . ? N3 Mn1 N1 87.12(5) 2_655 . ? N1 Mn1 N1 84.48(7) . 2_655 ? C5 N1 C4 117.86(16) . . ? C5 N1 Mn1 107.60(12) . . ? C4 N1 Mn1 134.07(11) . . ? C9 N2 C6 106.36(15) . . ? C9 N2 Mn1 132.87(12) . . ? C6 N2 Mn1 116.48(11) . . ? C13 N3 C16 105.16(14) . . ? C13 N3 Mn1 123.24(12) . . ? C16 N3 Mn1 124.50(12) . . ? C17 N4 C18 126.24(18) . . ? N1 C4 C1 111.64(17) . . ? N1 C4 C3 107.62(15) . . ? C1 C4 C3 108.80(19) . . ? N1 C4 C2 108.14(17) . . ? C1 C4 C2 111.7(2) . . ? C3 C4 C2 108.86(18) . . ? N1 C5 C6 121.13(17) . . ? N2 C6 C7 110.47(17) . . ? N2 C6 C5 118.09(15) . . ? C7 C6 C5 131.44(18) . . ? C6 C7 C8 106.22(17) . . ? C9 C8 C7 106.52(17) . . ? N2 C9 C8 110.43(17) . . ? N2 C9 C10 119.15(15) . . ? C8 C9 C10 130.42(16) . . ? C9 C10 C13 109.06(14) . . ? C9 C10 C11 110.11(16) . . ? C13 C10 C11 110.61(15) . . ? C9 C10 C12 109.97(15) . . ? C13 C10 C12 108.55(15) . . ? C11 C10 C12 108.52(16) . . ? N3 C13 C14 111.72(16) . . ? N3 C13 C10 122.51(15) . . ? C14 C13 C10 125.77(16) . . ? C15 C14 C13 106.81(16) . . ? C14 C15 C16 106.34(16) . . ? C17 C16 N3 121.12(16) . . ? C17 C16 C15 128.87(17) . . ? N3 C16 C15 109.96(16) . . ? N4 C17 C16 124.71(18) . . ? N4 C18 C20 108.03(19) . . ? N4 C18 C19 110.95(18) . . ? C20 C18 C19 110.8(2) . . ? N4 C18 C21 106.3(2) . . ? C20 C18 C21 111.0(2) . . ? C19 C18 C21 109.6(2) . . ? C1S O1S C4S 109.2(2) . . ? O1S C1S C2S 106.2(3) . . ? C3S C2S C1S 108.1(3) . . ? C2S C3S C4S 107.3(3) . . ? O1S C4S C3S 106.6(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.49 _refine_diff_density_min -0.30 _refine_diff_density_rms 0.06 #===END of CIF data_MNBUPY _database_code_depnum_ccdc_archive 'CCDC 219488' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H32 N4' _chemical_formula_sum 'C21 H32 N4' _chemical_formula_weight 340.51 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 19.508(2) _cell_length_b 10.4058(10) _cell_length_c 10.7926(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.609(2) _cell_angle_gamma 90.00 _cell_volume 2022.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2422 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.25 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS version 2.03; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% none _diffrn_reflns_number 5998 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.52 _reflns_number_total 2284 _reflns_number_gt 1856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; ? ; _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^)+(0.048P)^2^+1.003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2284 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 N1 N 0.16372(5) 1.01337(9) 0.22864(9) 0.0274(2) Uani 1 1 d . . . N2 N 0.06807(5) 0.80507(9) 0.19604(9) 0.0249(2) Uani 1 1 d . . . H2 H 0.0924 0.8256 0.2808 0.030 Uiso 1 1 calc R . . C1 C 0.29009(6) 1.07650(12) 0.35220(13) 0.0362(3) Uani 1 1 d . . . H1C H 0.2844 1.0406 0.4317 0.054 Uiso 1 1 calc R . . H1B H 0.3251 1.1486 0.3790 0.054 Uiso 1 1 calc R . . H1A H 0.3091 1.0100 0.3094 0.054 Uiso 1 1 calc R . . C2 C 0.18465(7) 1.22674(12) 0.31990(13) 0.0345(3) Uani 1 1 d . . . H2C H 0.1796 1.1906 0.3999 0.052 Uiso 1 1 calc R . . H2B H 0.1360 1.2559 0.2567 0.052 Uiso 1 1 calc R . . H2A H 0.2191 1.2997 0.3460 0.052 Uiso 1 1 calc R . . C3 C 0.22261(7) 1.17979(12) 0.12842(13) 0.0356(3) Uani 1 1 d . . . H3C H 0.1740 1.2093 0.0653 0.053 Uiso 1 1 calc R . . H3B H 0.2417 1.1136 0.0855 0.053 Uiso 1 1 calc R . . H3A H 0.2572 1.2524 0.1545 0.053 Uiso 1 1 calc R . . C4 C 0.21471(6) 1.12380(11) 0.25300(11) 0.0279(3) Uani 1 1 d . . . C5 C 0.12573(6) 0.97426(11) 0.11063(11) 0.0272(3) Uani 1 1 d . . . H5A H 0.1303 1.0159 0.0358 0.033 Uiso 1 1 calc R . . C6 C 0.07546(6) 0.86648(11) 0.08946(11) 0.0265(2) Uani 1 1 d . . . C7 C 0.02862(7) 0.80655(12) -0.02496(12) 0.0325(3) Uani 1 1 d . . . H7A H 0.0219 0.8282 -0.1144 0.039 Uiso 1 1 calc R . . C8 C -0.00787(6) 0.70668(11) 0.01455(12) 0.0307(3) Uani 1 1 d . . . H8A H -0.0436 0.6493 -0.0438 0.037 Uiso 1 1 calc R . . C9 C 0.01748(6) 0.70734(10) 0.15204(11) 0.0245(2) Uani 1 1 d . . . C10 C 0.0000 0.62316(14) 0.2500 0.0260(3) Uani 1 2 d S . . C11 C -0.06730(6) 0.53750(11) 0.17332(13) 0.0332(3) Uani 1 1 d . . . H11C H -0.1103 0.5917 0.1242 0.050 Uiso 1 1 calc R . . H11B H -0.0787 0.4833 0.2371 0.050 Uiso 1 1 calc R . . H11A H -0.0558 0.4830 0.1098 0.050 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 N1 0.0261(5) 0.0261(5) 0.0317(5) 0.0024(4) 0.0130(4) -0.0010(4) N2 0.0237(4) 0.0252(5) 0.0248(5) -0.0010(4) 0.0083(4) -0.0014(4) C1 0.0271(6) 0.0329(6) 0.0453(7) 0.0031(5) 0.0102(5) -0.0017(5) C2 0.0366(6) 0.0316(6) 0.0356(7) -0.0018(5) 0.0141(5) 0.0008(5) C3 0.0407(7) 0.0323(6) 0.0389(7) 0.0020(5) 0.0210(6) -0.0074(5) C4 0.0278(6) 0.0255(6) 0.0313(6) 0.0024(4) 0.0124(5) -0.0019(4) C5 0.0281(6) 0.0263(6) 0.0303(6) 0.0041(4) 0.0145(5) 0.0023(4) C6 0.0262(5) 0.0264(5) 0.0284(6) 0.0016(4) 0.0120(4) 0.0033(4) C7 0.0343(6) 0.0359(6) 0.0261(6) 0.0000(5) 0.0104(5) 0.0004(5) C8 0.0267(6) 0.0320(6) 0.0301(6) -0.0046(5) 0.0072(5) -0.0016(5) C9 0.0189(5) 0.0231(5) 0.0312(6) -0.0019(4) 0.0093(4) 0.0017(4) C10 0.0230(7) 0.0219(7) 0.0335(8) 0.000 0.0112(6) 0.000 C11 0.0289(6) 0.0278(6) 0.0441(7) -0.0061(5) 0.0154(5) -0.0056(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.4757(14) . ? N1 C5 1.2694(15) . ? N2 C6 1.3711(14) . ? N2 C9 1.3686(13) . ? C1 C4 1.5299(16) . ? C2 C4 1.5291(16) . ? C3 C4 1.5266(16) . ? C5 C6 1.4489(16) . ? C6 C7 1.3715(16) . ? C7 C8 1.4150(17) . ? C8 C9 1.3719(16) . ? C9 C10 1.5096(14) . ? C10 C11 1.5387(14) . ? 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 C5 N1 C4 121.46(10) . . ? C9 N2 C6 110.46(9) . . ? N1 C4 C3 115.45(10) . . ? N1 C4 C2 105.96(9) . . ? C3 C4 C2 109.60(10) . . ? N1 C4 C1 105.96(9) . . ? C3 C4 C1 110.10(10) . . ? C2 C4 C1 109.56(10) . . ? N1 C5 C6 120.34(10) . . ? N2 C6 C7 107.15(10) . . ? N2 C6 C5 120.76(10) . . ? C7 C6 C5 132.08(11) . . ? C6 C7 C8 107.51(10) . . ? C9 C8 C7 107.96(10) . . ? N2 C9 C8 106.92(10) . . ? N2 C9 C10 121.00(9) . . ? C8 C9 C10 132.06(10) . . ? C9 C10 C9 109.05(12) 2 . ? C9 C10 C11 109.70(6) 2 . ? C9 C10 C11 109.59(6) . . ? C11 C10 C11 109.20(13) . 2 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.24 _refine_diff_density_min -0.15 _refine_diff_density_rms 0.03 data_MNTBPY _database_code_depnum_ccdc_archive 'CCDC 219489' _refine_special_details ; One tert-butyl group disordered, refined methyl groups as half-occupancy over two sites with appropriate geometric restraints. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H60 Mn2 N8' _chemical_formula_sum 'C42 H60 Mn2 N8' _chemical_formula_weight 786.86 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' Mn Mn 0.3368 0.7283 '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 11.099(2) _cell_length_b 13.738(2) _cell_length_c 14.997(2) _cell_angle_alpha 74.705(2) _cell_angle_beta 79.934(2) _cell_angle_gamma 71.465(2) _cell_volume 2081.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4186 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details '(SHELXTL version 6.12; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17924 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.083 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.9 _reflns_number_total 9604 _reflns_number_gt 6458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.070P)^2^] 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 9604 _refine_ls_number_parameters 467 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.136 _refine_ls_wR_factor_gt 0.126 _refine_ls_goodness_of_fit_ref 0.95 _refine_ls_restrained_S_all 0.97 _refine_ls_shift/su_max 0.011 _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 Mn1 Mn 0.28408(4) 0.04632(3) 0.30893(3) 0.01877(12) Uani 1 1 d . . . Mn2 Mn 0.33627(4) 0.38852(3) 0.24930(3) 0.01958(12) Uani 1 1 d . . . N1 N 0.3335(2) -0.11467(18) 0.38805(16) 0.0186(5) Uani 1 1 d . . . N2 N 0.4755(2) -0.00128(18) 0.25709(17) 0.0195(5) Uani 1 1 d . . . N3 N 0.3581(2) 0.29892(18) 0.15172(16) 0.0188(5) Uani 1 1 d . . . N4 N 0.1749(2) 0.48605(19) 0.17224(17) 0.0216(5) Uani 1 1 d . . . N5 N 0.1312(2) 0.07392(19) 0.22477(16) 0.0205(5) Uani 1 1 d . . . N6 N 0.1593(2) 0.17985(18) 0.35031(16) 0.0179(5) Uani 1 1 d . . . N7 N 0.3307(2) 0.36422(18) 0.39302(16) 0.0185(5) Uani 1 1 d . . . N8 N 0.4578(2) 0.48452(19) 0.25400(17) 0.0226(6) Uani 1 1 d . A . C1 C 0.2415(4) -0.2657(3) 0.4361(3) 0.0459(10) Uani 1 1 d . . . H1A H 0.1953 -0.2393 0.3806 0.069 Uiso 1 1 calc R . . H1B H 0.1921 -0.3024 0.4868 0.069 Uiso 1 1 calc R . . H1C H 0.3249 -0.3146 0.4225 0.069 Uiso 1 1 calc R . . C2 C 0.1322(3) -0.0967(2) 0.4836(2) 0.0307(8) Uani 1 1 d . . . H2A H 0.1443 -0.0377 0.5026 0.046 Uiso 1 1 calc R . . H2B H 0.0807 -0.1324 0.5333 0.046 Uiso 1 1 calc R . . H2C H 0.0882 -0.0701 0.4270 0.046 Uiso 1 1 calc R . . C3 C 0.3315(3) -0.2116(3) 0.5515(2) 0.0476(11) Uani 1 1 d . . . H3A H 0.3430 -0.1512 0.5686 0.071 Uiso 1 1 calc R . . H3B H 0.4153 -0.2606 0.5389 0.071 Uiso 1 1 calc R . . H3C H 0.2820 -0.2475 0.6027 0.071 Uiso 1 1 calc R . . C4 C 0.2607(3) -0.1734(2) 0.4650(2) 0.0227(7) Uani 1 1 d . . . C5 C 0.4449(3) -0.1647(2) 0.3537(2) 0.0223(7) Uani 1 1 d . . . H5A H 0.4776 -0.2385 0.3763 0.027 Uiso 1 1 calc R . . C6 C 0.5184(3) -0.1104(2) 0.2827(2) 0.0209(6) Uani 1 1 d . . . C7 C 0.6339(3) -0.1467(2) 0.2314(2) 0.0271(7) Uani 1 1 d . . . H7A H 0.6830 -0.2181 0.2353 0.033 Uiso 1 1 calc R . . C8 C 0.6636(3) -0.0588(2) 0.1734(2) 0.0284(7) Uani 1 1 d . . . H8A H 0.7368 -0.0584 0.1298 0.034 Uiso 1 1 calc R . . C9 C 0.5652(3) 0.0294(2) 0.1913(2) 0.0223(7) Uani 1 1 d . . . C10 C 0.5580(3) 0.1454(2) 0.1569(2) 0.0208(6) Uani 1 1 d . . . C11 C 0.5862(3) 0.1827(3) 0.2375(2) 0.0280(7) Uani 1 1 d . . . H11A H 0.5217 0.1739 0.2903 0.042 Uiso 1 1 calc R . . H11B H 0.5839 0.2571 0.2171 0.042 Uiso 1 1 calc R . . H11C H 0.6710 0.1406 0.2564 0.042 Uiso 1 1 calc R . . C12 C 0.6600(3) 0.1595(3) 0.0746(2) 0.0331(8) Uani 1 1 d . . . H12A H 0.6431 0.1357 0.0231 0.050 Uiso 1 1 calc R . . H12B H 0.7446 0.1177 0.0940 0.050 Uiso 1 1 calc R . . H12C H 0.6572 0.2340 0.0544 0.050 Uiso 1 1 calc R . . C13 C 0.4285(3) 0.2090(2) 0.1239(2) 0.0196(6) Uani 1 1 d . . . C14 C 0.3705(3) 0.1924(2) 0.0558(2) 0.0267(7) Uani 1 1 d . . . H14A H 0.4008 0.1353 0.0254 0.032 Uiso 1 1 calc R . . C15 C 0.2597(3) 0.2759(2) 0.0410(2) 0.0265(7) Uani 1 1 d . . . H15A H 0.1996 0.2866 -0.0012 0.032 Uiso 1 1 calc R . . C16 C 0.2542(3) 0.3404(2) 0.0997(2) 0.0217(6) Uani 1 1 d . . . C17 C 0.1641(3) 0.4376(2) 0.1121(2) 0.0258(7) Uani 1 1 d . . . H17A H 0.0942 0.4676 0.0753 0.031 Uiso 1 1 calc R . . C18 C 0.0841(3) 0.5909(2) 0.1788(2) 0.0277(7) Uani 1 1 d . . . C19 C -0.0547(3) 0.5861(3) 0.1954(3) 0.0423(9) Uani 1 1 d . . . H19A H -0.0746 0.5657 0.1430 0.063 Uiso 1 1 calc R . . H19B H -0.1124 0.6554 0.2011 0.063 Uiso 1 1 calc R . . H19C H -0.0656 0.5340 0.2528 0.063 Uiso 1 1 calc R . . C20 C 0.1146(4) 0.6224(3) 0.2597(3) 0.0416(9) Uani 1 1 d . . . H20A H 0.2031 0.6256 0.2492 0.062 Uiso 1 1 calc R . . H20B H 0.1038 0.5702 0.3171 0.062 Uiso 1 1 calc R . . H20C H 0.0568 0.6917 0.2654 0.062 Uiso 1 1 calc R . . C21 C 0.0995(4) 0.6710(3) 0.0885(3) 0.0423(9) Uani 1 1 d . . . H21A H 0.1879 0.6744 0.0768 0.064 Uiso 1 1 calc R . . H21B H 0.0417 0.7405 0.0936 0.064 Uiso 1 1 calc R . . H21C H 0.0788 0.6495 0.0370 0.064 Uiso 1 1 calc R . . C22 C 0.0840(4) 0.0767(3) 0.0675(2) 0.0381(9) Uani 1 1 d . . . H22A H 0.1554 0.1056 0.0390 0.057 Uiso 1 1 calc R . . H22B H 0.0056 0.1345 0.0717 0.057 Uiso 1 1 calc R . . H22C H 0.0733 0.0326 0.0294 0.057 Uiso 1 1 calc R . . C23 C 0.0013(3) -0.0354(3) 0.2093(2) 0.0364(8) Uani 1 1 d . . . H23A H 0.0202 -0.0784 0.2715 0.055 Uiso 1 1 calc R . . H23B H -0.0096 -0.0794 0.1711 0.055 Uiso 1 1 calc R . . H23C H -0.0774 0.0219 0.2142 0.055 Uiso 1 1 calc R . . C24 C 0.2341(3) -0.0782(3) 0.1586(3) 0.0389(9) Uani 1 1 d . . . H24A H 0.3048 -0.0488 0.1293 0.058 Uiso 1 1 calc R . . H24B H 0.2242 -0.1238 0.1216 0.058 Uiso 1 1 calc R . . H24C H 0.2524 -0.1196 0.2214 0.058 Uiso 1 1 calc R . . C25 C 0.1116(3) 0.0107(2) 0.1642(2) 0.0246(7) Uani 1 1 d . . . C26 C 0.0468(3) 0.1610(2) 0.2338(2) 0.0224(7) Uani 1 1 d . . . H26A H -0.0245 0.1866 0.1984 0.027 Uiso 1 1 calc R . . C27 C 0.0578(3) 0.2201(2) 0.2958(2) 0.0217(6) Uani 1 1 d . . . C28 C -0.0207(3) 0.3143(2) 0.3164(2) 0.0258(7) Uani 1 1 d . . . H28A H -0.0962 0.3577 0.2887 0.031 Uiso 1 1 calc R . . C29 C 0.0328(3) 0.3328(2) 0.3853(2) 0.0250(7) Uani 1 1 d . . . H29A H 0.0010 0.3914 0.4137 0.030 Uiso 1 1 calc R . . C30 C 0.1430(3) 0.2484(2) 0.4049(2) 0.0190(6) Uani 1 1 d . . . C31 C 0.2252(3) 0.2271(2) 0.4829(2) 0.0201(6) Uani 1 1 d . . . C32 C 0.3404(3) 0.1292(2) 0.4813(2) 0.0253(7) Uani 1 1 d . . . H32A H 0.3940 0.1400 0.4224 0.038 Uiso 1 1 calc R . . H32B H 0.3103 0.0677 0.4875 0.038 Uiso 1 1 calc R . . H32C H 0.3903 0.1175 0.5329 0.038 Uiso 1 1 calc R . . C33 C 0.1426(3) 0.2074(3) 0.5761(2) 0.0310(8) Uani 1 1 d . . . H33A H 0.0684 0.2690 0.5786 0.047 Uiso 1 1 calc R . . H33B H 0.1933 0.1950 0.6274 0.047 Uiso 1 1 calc R . . H33C H 0.1136 0.1455 0.5815 0.047 Uiso 1 1 calc R . . C34 C 0.2736(3) 0.3209(2) 0.4748(2) 0.0204(6) Uani 1 1 d . . . C35 C 0.2796(3) 0.3692(2) 0.5447(2) 0.0258(7) Uani 1 1 d . . . H35A H 0.2459 0.3535 0.6078 0.031 Uiso 1 1 calc R . . C36 C 0.3441(3) 0.4445(2) 0.5044(2) 0.0266(7) Uani 1 1 d . . . H36A H 0.3627 0.4901 0.5345 0.032 Uiso 1 1 calc R . . C37 C 0.3758(3) 0.4397(2) 0.4116(2) 0.0203(6) Uani 1 1 d . . . C38 C 0.4447(3) 0.4960(2) 0.3387(2) 0.0232(7) Uani 1 1 d . . . H38A H 0.4821 0.5432 0.3522 0.028 Uiso 1 1 calc R . . C39 C 0.5353(3) 0.5403(2) 0.1800(2) 0.0298(7) Uani 1 1 d D . . C40 C 0.6483(7) 0.4517(5) 0.1449(5) 0.0454(19) Uiso 0.50 1 d PD A 1 H40A H 0.6330 0.3830 0.1721 0.068 Uiso 0.50 1 calc PR A 1 H40B H 0.7286 0.4519 0.1636 0.068 Uiso 0.50 1 calc PR A 1 H40C H 0.6540 0.4650 0.0770 0.068 Uiso 0.50 1 calc PR A 1 C41 C 0.6022(8) 0.6053(6) 0.2118(6) 0.052(2) Uiso 0.50 1 d PD A 1 H41A H 0.5380 0.6631 0.2351 0.078 Uiso 0.50 1 calc PR A 1 H41B H 0.6563 0.6342 0.1592 0.078 Uiso 0.50 1 calc PR A 1 H41C H 0.6552 0.5602 0.2614 0.078 Uiso 0.50 1 calc PR A 1 C42 C 0.4599(7) 0.6037(6) 0.1008(5) 0.047(2) Uiso 0.50 1 d PD A 1 H42A H 0.3888 0.6593 0.1216 0.070 Uiso 0.50 1 calc PR A 1 H42B H 0.4264 0.5581 0.0776 0.070 Uiso 0.50 1 calc PR A 1 H42C H 0.5149 0.6356 0.0510 0.070 Uiso 0.50 1 calc PR A 1 C40' C 0.6713(6) 0.5013(7) 0.1987(6) 0.061(2) Uiso 0.50 1 d PD A 2 H40D H 0.6857 0.5399 0.2404 0.092 Uiso 0.50 1 calc PR A 2 H40E H 0.7256 0.5123 0.1402 0.092 Uiso 0.50 1 calc PR A 2 H40F H 0.6925 0.4260 0.2281 0.092 Uiso 0.50 1 calc PR A 2 C41' C 0.4794(8) 0.6603(5) 0.1763(6) 0.053(2) Uiso 0.50 1 d PD A 2 H41D H 0.3980 0.6731 0.2155 0.079 Uiso 0.50 1 calc PR A 2 H41E H 0.4654 0.6984 0.1121 0.079 Uiso 0.50 1 calc PR A 2 H41F H 0.5395 0.6850 0.1990 0.079 Uiso 0.50 1 calc PR A 2 C42' C 0.5123(7) 0.5230(6) 0.0892(4) 0.0414(18) Uiso 0.50 1 d PD A 2 H42D H 0.4302 0.5712 0.0698 0.062 Uiso 0.50 1 calc PR A 2 H42E H 0.5108 0.4501 0.0979 0.062 Uiso 0.50 1 calc PR A 2 H42F H 0.5810 0.5365 0.0413 0.062 Uiso 0.50 1 calc PR A 2 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 Mn1 0.0137(2) 0.0184(2) 0.0222(3) -0.00324(18) -0.00156(18) -0.00298(17) Mn2 0.0204(2) 0.0204(2) 0.0180(2) -0.00173(18) -0.00321(19) -0.00716(19) N1 0.0163(12) 0.0198(13) 0.0189(13) -0.0021(10) -0.0025(10) -0.0055(10) N2 0.0166(12) 0.0182(12) 0.0216(13) -0.0028(10) -0.0008(10) -0.0039(10) N3 0.0172(12) 0.0224(13) 0.0157(13) -0.0008(10) 0.0013(10) -0.0084(10) N4 0.0158(12) 0.0216(13) 0.0234(14) -0.0002(11) -0.0004(10) -0.0047(10) N5 0.0183(13) 0.0252(14) 0.0177(13) -0.0038(10) 0.0000(10) -0.0074(11) N6 0.0152(12) 0.0193(12) 0.0176(13) -0.0013(10) 0.0002(10) -0.0060(10) N7 0.0172(12) 0.0179(12) 0.0200(13) -0.0011(10) -0.0031(10) -0.0064(10) N8 0.0215(13) 0.0218(13) 0.0237(14) 0.0011(11) -0.0008(11) -0.0109(11) C1 0.053(2) 0.031(2) 0.055(3) -0.0131(18) 0.019(2) -0.0247(18) C2 0.0253(17) 0.0281(18) 0.0322(19) -0.0009(15) 0.0051(14) -0.0079(14) C3 0.031(2) 0.071(3) 0.027(2) 0.0139(19) -0.0056(16) -0.0152(19) C4 0.0200(15) 0.0204(15) 0.0229(16) 0.0017(13) 0.0006(13) -0.0060(12) C5 0.0183(15) 0.0206(15) 0.0259(17) -0.0045(13) -0.0050(13) -0.0019(12) C6 0.0180(15) 0.0195(15) 0.0240(16) -0.0029(12) -0.0041(12) -0.0039(12) C7 0.0224(16) 0.0214(16) 0.0334(19) -0.0074(14) 0.0022(14) -0.0021(13) C8 0.0203(16) 0.0307(18) 0.0308(18) -0.0112(15) 0.0067(14) -0.0039(13) C9 0.0203(15) 0.0251(16) 0.0205(16) -0.0039(13) 0.0000(12) -0.0074(13) C10 0.0171(15) 0.0255(16) 0.0199(16) -0.0042(13) -0.0003(12) -0.0075(12) C11 0.0221(16) 0.0285(17) 0.0322(19) -0.0045(14) -0.0051(14) -0.0062(13) C12 0.0266(18) 0.0345(19) 0.034(2) -0.0004(15) 0.0050(15) -0.0129(15) C13 0.0203(15) 0.0205(15) 0.0160(15) 0.0007(12) 0.0035(12) -0.0096(12) C14 0.0325(18) 0.0270(17) 0.0231(17) -0.0090(14) -0.0034(14) -0.0088(14) C15 0.0265(17) 0.0304(18) 0.0250(17) -0.0012(14) -0.0088(14) -0.0120(14) C16 0.0188(15) 0.0240(16) 0.0225(16) 0.0003(13) -0.0036(12) -0.0104(12) C17 0.0175(15) 0.0311(18) 0.0254(17) 0.0034(14) -0.0047(13) -0.0086(13) C18 0.0193(16) 0.0217(16) 0.0335(19) 0.0006(14) -0.0010(14) -0.0004(13) C19 0.0217(18) 0.036(2) 0.061(3) -0.0057(19) -0.0004(17) -0.0031(15) C20 0.038(2) 0.034(2) 0.048(2) -0.0159(18) -0.0081(18) 0.0045(16) C21 0.042(2) 0.0248(18) 0.047(2) 0.0039(16) -0.0006(18) -0.0021(16) C22 0.057(2) 0.042(2) 0.0245(18) -0.0019(16) -0.0108(17) -0.0273(19) C23 0.040(2) 0.036(2) 0.039(2) -0.0075(17) -0.0022(17) -0.0213(17) C24 0.038(2) 0.042(2) 0.040(2) -0.0228(18) -0.0052(17) -0.0050(17) C25 0.0241(16) 0.0289(17) 0.0230(17) -0.0051(13) -0.0035(13) -0.0106(13) C26 0.0190(15) 0.0269(16) 0.0194(16) 0.0008(13) -0.0047(12) -0.0073(13) C27 0.0165(15) 0.0216(15) 0.0227(16) 0.0003(13) -0.0014(12) -0.0040(12) C28 0.0195(16) 0.0218(16) 0.0310(18) -0.0023(14) -0.0048(13) -0.0005(13) C29 0.0241(16) 0.0177(15) 0.0318(18) -0.0101(13) -0.0010(14) -0.0011(13) C30 0.0152(14) 0.0177(14) 0.0219(16) -0.0017(12) 0.0035(12) -0.0067(12) C31 0.0224(16) 0.0206(15) 0.0173(15) -0.0013(12) 0.0011(12) -0.0102(12) C32 0.0276(17) 0.0207(16) 0.0303(18) -0.0034(13) -0.0082(14) -0.0096(13) C33 0.0354(19) 0.039(2) 0.0221(17) -0.0012(15) 0.0017(14) -0.0215(16) C34 0.0197(15) 0.0178(15) 0.0216(16) -0.0016(12) -0.0011(12) -0.0052(12) C35 0.0300(18) 0.0259(17) 0.0197(16) -0.0034(13) -0.0017(13) -0.0073(14) C36 0.0353(18) 0.0235(16) 0.0238(17) -0.0045(13) -0.0095(14) -0.0093(14) C37 0.0216(15) 0.0170(14) 0.0226(16) -0.0022(12) -0.0054(12) -0.0061(12) C38 0.0234(16) 0.0193(15) 0.0292(18) -0.0018(13) -0.0093(13) -0.0087(12) C39 0.0336(19) 0.0333(18) 0.0272(18) -0.0021(15) -0.0019(14) -0.0205(15) _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 Mn1 N1 2.162(2) . ? Mn1 N2 2.086(2) . ? Mn2 N3 2.086(2) . ? Mn2 N4 2.172(2) . ? Mn1 N5 2.169(2) . ? Mn1 N6 2.086(2) . ? Mn2 N7 2.085(2) . ? Mn2 N8 2.186(2) . ? N1 C5 1.300(4) . ? N1 C4 1.495(4) . ? N2 C9 1.359(4) . ? N2 C6 1.389(4) . ? N3 C13 1.362(4) . ? N3 C16 1.387(4) . ? N4 C17 1.294(4) . ? N4 C18 1.490(4) . ? N5 C26 1.287(4) . ? N5 C25 1.494(4) . ? N6 C30 1.354(4) . ? N6 C27 1.389(4) . ? N7 C34 1.358(4) . ? N7 C37 1.391(4) . ? N8 C38 1.299(4) . ? N8 C39 1.481(4) . ? C1 C4 1.528(4) . ? C2 C4 1.511(4) . ? C3 C4 1.520(4) . ? C5 C6 1.420(4) . ? C6 C7 1.391(4) . ? C7 C8 1.388(4) . ? C8 C9 1.401(4) . ? C9 C10 1.520(4) . ? C10 C13 1.515(4) . ? C10 C12 1.538(4) . ? C10 C11 1.544(4) . ? C13 C14 1.398(4) . ? C14 C15 1.394(4) . ? C15 C16 1.386(4) . ? C16 C17 1.427(4) . ? C18 C20 1.513(5) . ? C18 C21 1.525(4) . ? C18 C19 1.537(4) . ? C22 C25 1.518(4) . ? C23 C25 1.528(4) . ? C24 C25 1.518(4) . ? C26 C27 1.429(4) . ? C27 C28 1.389(4) . ? C28 C29 1.391(4) . ? C29 C30 1.404(4) . ? C30 C31 1.520(4) . ? C31 C34 1.516(4) . ? C31 C32 1.535(4) . ? C31 C33 1.542(4) . ? C34 C35 1.400(4) . ? C35 C36 1.392(4) . ? C36 C37 1.388(4) . ? C37 C38 1.420(4) . ? C39 C40' 1.483(6) . ? C39 C42 1.485(6) . ? C39 C42' 1.518(6) . ? C39 C41 1.533(6) . ? C39 C41' 1.556(6) . ? C39 C40 1.571(6) . ? 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 N6 Mn1 N2 136.59(9) . . ? N6 Mn1 N1 128.42(9) . . ? N2 Mn1 N1 81.11(9) . . ? N6 Mn1 N5 81.37(9) . . ? N2 Mn1 N5 121.46(9) . . ? N1 Mn1 N5 110.30(9) . . ? N7 Mn2 N3 137.82(9) . . ? N7 Mn2 N4 122.94(9) . . ? N3 Mn2 N4 81.37(9) . . ? N7 Mn2 N8 81.03(9) . . ? N3 Mn2 N8 126.32(9) . . ? N4 Mn2 N8 109.42(9) . . ? C5 N1 C4 119.5(2) . . ? C5 N1 Mn1 108.46(19) . . ? C4 N1 Mn1 131.84(18) . . ? C9 N2 C6 106.3(2) . . ? C9 N2 Mn1 143.0(2) . . ? C6 N2 Mn1 108.10(18) . . ? C13 N3 C16 105.8(2) . . ? C13 N3 Mn2 144.5(2) . . ? C16 N3 Mn2 109.23(19) . . ? C17 N4 C18 120.2(3) . . ? C17 N4 Mn2 108.3(2) . . ? C18 N4 Mn2 131.4(2) . . ? C26 N5 C25 119.8(2) . . ? C26 N5 Mn1 108.8(2) . . ? C25 N5 Mn1 131.43(18) . . ? C30 N6 C27 106.4(2) . . ? C30 N6 Mn1 144.40(19) . . ? C27 N6 Mn1 108.87(18) . . ? C34 N7 C37 106.2(2) . . ? C34 N7 Mn2 143.1(2) . . ? C37 N7 Mn2 108.08(18) . . ? C38 N8 C39 120.5(2) . . ? C38 N8 Mn2 107.45(19) . . ? C39 N8 Mn2 131.76(19) . . ? N1 C4 C2 106.8(2) . . ? N1 C4 C3 109.4(2) . . ? C2 C4 C3 109.7(3) . . ? N1 C4 C1 110.5(3) . . ? C2 C4 C1 109.4(3) . . ? C3 C4 C1 110.9(3) . . ? N1 C5 C6 120.9(3) . . ? N2 C6 C7 109.7(3) . . ? N2 C6 C5 118.8(3) . . ? C7 C6 C5 131.4(3) . . ? C8 C7 C6 106.9(3) . . ? C7 C8 C9 106.9(3) . . ? N2 C9 C8 110.1(3) . . ? N2 C9 C10 120.5(3) . . ? C8 C9 C10 128.9(3) . . ? C13 C10 C9 110.9(2) . . ? C13 C10 C12 108.0(2) . . ? C9 C10 C12 109.9(2) . . ? C13 C10 C11 111.7(2) . . ? C9 C10 C11 107.5(2) . . ? C12 C10 C11 108.8(3) . . ? N3 C13 C14 110.5(3) . . ? N3 C13 C10 122.6(3) . . ? C14 C13 C10 126.6(3) . . ? C15 C14 C13 106.7(3) . . ? C16 C15 C14 106.7(3) . . ? C15 C16 N3 110.3(3) . . ? C15 C16 C17 131.0(3) . . ? N3 C16 C17 118.6(3) . . ? N4 C17 C16 121.8(3) . . ? N4 C18 C20 107.6(3) . . ? N4 C18 C21 109.5(3) . . ? C20 C18 C21 110.7(3) . . ? N4 C18 C19 111.0(3) . . ? C20 C18 C19 109.4(3) . . ? C21 C18 C19 108.6(3) . . ? N5 C25 C22 111.6(3) . . ? N5 C25 C24 106.7(2) . . ? C22 C25 C24 109.9(3) . . ? N5 C25 C23 109.2(3) . . ? C22 C25 C23 110.0(3) . . ? C24 C25 C23 109.4(3) . . ? N5 C26 C27 121.5(3) . . ? N6 C27 C28 110.0(3) . . ? N6 C27 C26 118.9(3) . . ? C28 C27 C26 131.1(3) . . ? C27 C28 C29 106.6(3) . . ? C28 C29 C30 107.0(3) . . ? N6 C30 C29 110.1(3) . . ? N6 C30 C31 123.2(2) . . ? C29 C30 C31 126.3(3) . . ? C34 C31 C30 110.2(2) . . ? C34 C31 C32 108.6(2) . . ? C30 C31 C32 111.8(2) . . ? C34 C31 C33 110.0(2) . . ? C30 C31 C33 108.1(2) . . ? C32 C31 C33 108.1(2) . . ? N7 C34 C35 110.0(3) . . ? N7 C34 C31 120.7(3) . . ? C35 C34 C31 129.0(3) . . ? C36 C35 C34 107.3(3) . . ? C37 C36 C35 106.4(3) . . ? C36 C37 N7 110.1(3) . . ? C36 C37 C38 131.0(3) . . ? N7 C37 C38 118.9(3) . . ? N8 C38 C37 121.5(3) . . ? N8 C39 C40' 110.2(4) . . ? N8 C39 C42 111.1(4) . . ? N8 C39 C42' 106.1(4) . . ? C40' C39 C42' 113.8(5) . . ? N8 C39 C41 115.6(4) . . ? C42 C39 C41 111.5(5) . . ? N8 C39 C41' 107.9(4) . . ? C40' C39 C41' 111.7(5) . . ? C42' C39 C41' 106.8(5) . . ? N8 C39 C40 105.8(4) . . ? C42 C39 C40 108.4(5) . . ? C41 C39 C40 103.9(5) . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.24 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.09 data_fepytb _database_code_depnum_ccdc_archive 'CCDC 219490' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H60 Fe2 N8' _chemical_formula_weight 788.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.0298(13) _cell_length_b 13.728(2) _cell_length_c 15.100(2) _cell_angle_alpha 72.860(2) _cell_angle_beta 80.369(2) _cell_angle_gamma 72.095(2) _cell_volume 2071.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4976 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.5 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03 (2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17851 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.59 _reflns_number_total 9114 _reflns_number_gt 6750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2003)' _refine_special_details ; Data showed evidence of twinning, several large residual peaks of electron density in structurally nonsenical positions and many Fobs greater than Fcalc. ROTAX used and a new hklf 5 format file produced using WINGX corresponding to a 180 degree rotation about the 101 reciprocal lattice direction. The twin component fraction refined to 0.117(2) and a marked improvement in the refinement. ; _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^)+(0.0681P)^2^+0.9670P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9114 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.28678(4) 0.05114(3) 0.30416(3) 0.01933(11) Uani 1 1 d . . . N1 N 0.3320(2) -0.10790(17) 0.38287(15) 0.0195(5) Uani 1 1 d . . . C1 C 0.2401(3) -0.2615(3) 0.4320(3) 0.0392(8) Uani 1 1 d . . . H1D H 0.3235 -0.3108 0.4216 0.059 Uiso 1 1 calc R . . H1E H 0.1963 -0.2344 0.3747 0.059 Uiso 1 1 calc R . . H1F H 0.1883 -0.2985 0.4818 0.059 Uiso 1 1 calc R . . Fe2 Fe 0.33610(4) 0.39071(3) 0.25644(3) 0.01917(11) Uani 1 1 d . . . N2 N 0.4718(2) 0.00991(17) 0.25402(15) 0.0204(5) Uani 1 1 d . . . C2 C 0.1295(3) -0.0926(2) 0.4758(2) 0.0284(6) Uani 1 1 d . . . H2D H 0.1413 -0.0333 0.4937 0.043 Uiso 1 1 calc R . . H2E H 0.0778 -0.1298 0.5256 0.043 Uiso 1 1 calc R . . H2F H 0.0858 -0.0657 0.4185 0.043 Uiso 1 1 calc R . . N3 N 0.3540(2) 0.31314(17) 0.15823(15) 0.0200(5) Uani 1 1 d . . . C3 C 0.3301(3) -0.2078(3) 0.5471(2) 0.0385(8) Uani 1 1 d . . . H3D H 0.3410 -0.1472 0.5634 0.058 Uiso 1 1 calc R . . H3E H 0.4143 -0.2557 0.5357 0.058 Uiso 1 1 calc R . . H3F H 0.2810 -0.2457 0.5984 0.058 Uiso 1 1 calc R . . N4 N 0.1712(2) 0.49083(17) 0.18994(16) 0.0214(5) Uani 1 1 d . . . C4 C 0.2591(3) -0.1688(2) 0.45989(19) 0.0219(6) Uani 1 1 d . . . N5 N 0.1407(2) 0.07911(17) 0.21845(15) 0.0209(5) Uani 1 1 d . . . C5 C 0.4420(2) -0.1569(2) 0.34893(19) 0.0211(5) Uani 1 1 d . . . H5B H 0.4738 -0.2316 0.3714 0.025 Uiso 1 1 calc R . . N6 N 0.1655(2) 0.17346(17) 0.34942(15) 0.0192(5) Uani 1 1 d . . . C6 C 0.5151(3) -0.0995(2) 0.27838(19) 0.0221(6) Uani 1 1 d . . . N7 N 0.3331(2) 0.35923(17) 0.39611(15) 0.0194(5) Uani 1 1 d . . . C7 C 0.6296(3) -0.1324(2) 0.2267(2) 0.0275(6) Uani 1 1 d . . . H7B H 0.6782 -0.2034 0.2293 0.033 Uiso 1 1 calc R . . N8 N 0.4537(2) 0.48570(18) 0.25912(16) 0.0222(5) Uani 1 1 d . . . C8 C 0.6592(3) -0.0406(2) 0.1703(2) 0.0275(6) Uani 1 1 d . . . H8B H 0.7321 -0.0372 0.1272 0.033 Uiso 1 1 calc R . . C9 C 0.5615(3) 0.0455(2) 0.18919(19) 0.0221(6) Uani 1 1 d . . . C10 C 0.5546(3) 0.1620(2) 0.15691(19) 0.0218(6) Uani 1 1 d . . . C11 C 0.5898(3) 0.1936(2) 0.2372(2) 0.0270(6) Uani 1 1 d . . . H11D H 0.5284 0.1813 0.2913 0.041 Uiso 1 1 calc R . . H11E H 0.5874 0.2688 0.2175 0.041 Uiso 1 1 calc R . . H11F H 0.6760 0.1508 0.2537 0.041 Uiso 1 1 calc R . . C12 C 0.6534(3) 0.1826(2) 0.0735(2) 0.0316(7) Uani 1 1 d . . . H12D H 0.6333 0.1632 0.0213 0.047 Uiso 1 1 calc R . . H12E H 0.7391 0.1399 0.0912 0.047 Uiso 1 1 calc R . . H12F H 0.6505 0.2579 0.0550 0.047 Uiso 1 1 calc R . . C13 C 0.4234(3) 0.2272(2) 0.12719(18) 0.0206(5) Uani 1 1 d . . . C14 C 0.3609(3) 0.2158(2) 0.0591(2) 0.0258(6) Uani 1 1 d . . . H14B H 0.3895 0.1618 0.0269 0.031 Uiso 1 1 calc R . . C15 C 0.2489(3) 0.2986(2) 0.0472(2) 0.0263(6) Uani 1 1 d . . . H15B H 0.1865 0.3122 0.0055 0.032 Uiso 1 1 calc R . . C16 C 0.2464(3) 0.3574(2) 0.10863(19) 0.0213(6) Uani 1 1 d . . . C17 C 0.1562(3) 0.4504(2) 0.12675(19) 0.0231(6) Uani 1 1 d . . . H17B H 0.0836 0.4832 0.0917 0.028 Uiso 1 1 calc R . . C18 C 0.0820(3) 0.5945(2) 0.2003(2) 0.0259(6) Uani 1 1 d . . . C19 C -0.0574(3) 0.5917(3) 0.2107(3) 0.0395(8) Uani 1 1 d . . . H19D H -0.0717 0.5362 0.2662 0.059 Uiso 1 1 calc R . . H19E H -0.0760 0.5766 0.1557 0.059 Uiso 1 1 calc R . . H19F H -0.1139 0.6605 0.2169 0.059 Uiso 1 1 calc R . . C20 C 0.1121(3) 0.6144(3) 0.2860(3) 0.0425(9) Uani 1 1 d . . . H20D H 0.2014 0.6161 0.2791 0.064 Uiso 1 1 calc R . . H20E H 0.0986 0.5575 0.3405 0.064 Uiso 1 1 calc R . . H20F H 0.0558 0.6825 0.2942 0.064 Uiso 1 1 calc R . . C21 C 0.1038(4) 0.6811(3) 0.1137(3) 0.0449(9) Uani 1 1 d . . . H21D H 0.1930 0.6830 0.1069 0.067 Uiso 1 1 calc R . . H21E H 0.0472 0.7498 0.1200 0.067 Uiso 1 1 calc R . . H21F H 0.0852 0.6659 0.0587 0.067 Uiso 1 1 calc R . . C22 C 0.0856(3) 0.0915(3) 0.0609(2) 0.0379(8) Uani 1 1 d . . . H22D H 0.1537 0.1255 0.0317 0.057 Uiso 1 1 calc R . . H22E H 0.0053 0.1460 0.0676 0.057 Uiso 1 1 calc R . . H22F H 0.0750 0.0494 0.0219 0.057 Uiso 1 1 calc R . . C23 C 0.0152(3) -0.0341(3) 0.2029(2) 0.0365(7) Uani 1 1 d . . . H23D H 0.0385 -0.0803 0.2643 0.055 Uiso 1 1 calc R . . H23E H 0.0045 -0.0765 0.1642 0.055 Uiso 1 1 calc R . . H23F H -0.0652 0.0201 0.2099 0.055 Uiso 1 1 calc R . . C24 C 0.2460(3) -0.0642(3) 0.1467(3) 0.0420(8) Uani 1 1 d . . . H24D H 0.3135 -0.0295 0.1170 0.063 Uiso 1 1 calc R . . H24E H 0.2362 -0.1072 0.1082 0.063 Uiso 1 1 calc R . . H24F H 0.2692 -0.1098 0.2082 0.063 Uiso 1 1 calc R . . C25 C 0.1209(3) 0.0193(2) 0.15676(19) 0.0259(6) Uani 1 1 d . . . C26 C 0.0517(3) 0.1631(2) 0.2304(2) 0.0239(6) Uani 1 1 d . . . H26B H -0.0206 0.1893 0.1951 0.029 Uiso 1 1 calc R . . C27 C 0.0616(3) 0.2160(2) 0.29535(19) 0.0208(5) Uani 1 1 d . . . C28 C -0.0173(3) 0.3070(2) 0.3184(2) 0.0243(6) Uani 1 1 d . . . H28B H -0.0940 0.3511 0.2915 0.029 Uiso 1 1 calc R . . C29 C 0.0376(3) 0.3209(2) 0.3885(2) 0.0238(6) Uani 1 1 d . . . H29B H 0.0055 0.3766 0.4187 0.029 Uiso 1 1 calc R . . C30 C 0.1492(2) 0.2375(2) 0.40625(18) 0.0195(5) Uani 1 1 d . . . C31 C 0.2343(2) 0.2131(2) 0.48371(18) 0.0196(5) Uani 1 1 d . . . C32 C 0.3527(3) 0.1192(2) 0.4788(2) 0.0252(6) Uani 1 1 d . . . H32D H 0.4039 0.1364 0.4197 0.038 Uiso 1 1 calc R . . H32E H 0.3256 0.0562 0.4831 0.038 Uiso 1 1 calc R . . H32F H 0.4042 0.1051 0.5305 0.038 Uiso 1 1 calc R . . C33 C 0.1564(3) 0.1833(2) 0.5772(2) 0.0290(6) Uani 1 1 d . . . H33D H 0.0802 0.2422 0.5819 0.044 Uiso 1 1 calc R . . H33E H 0.2089 0.1688 0.6283 0.044 Uiso 1 1 calc R . . H33F H 0.1304 0.1200 0.5809 0.044 Uiso 1 1 calc R . . C34 C 0.2784(3) 0.3090(2) 0.47745(18) 0.0203(5) Uani 1 1 d . . . C35 C 0.2824(3) 0.3541(2) 0.54824(19) 0.0246(6) Uani 1 1 d . . . H35B H 0.2497 0.3340 0.6112 0.030 Uiso 1 1 calc R . . C36 C 0.3437(3) 0.4344(2) 0.50907(19) 0.0254(6) Uani 1 1 d . . . H36B H 0.3601 0.4796 0.5399 0.030 Uiso 1 1 calc R . . C37 C 0.3754(3) 0.4347(2) 0.41617(19) 0.0207(5) Uani 1 1 d . . . C38 C 0.4424(3) 0.4957(2) 0.34323(19) 0.0220(6) Uani 1 1 d . . . H38B H 0.4789 0.5438 0.3561 0.026 Uiso 1 1 calc R . . C39 C 0.5300(3) 0.5459(2) 0.1847(2) 0.0262(6) Uani 1 1 d . . . C40 C 0.6697(4) 0.4996(4) 0.2023(3) 0.0612(12) Uani 1 1 d . . . H40D H 0.6959 0.4243 0.2034 0.092 Uiso 1 1 calc R . . H40E H 0.6826 0.5072 0.2624 0.092 Uiso 1 1 calc R . . H40F H 0.7212 0.5372 0.1527 0.092 Uiso 1 1 calc R . . C41 C 0.4860(5) 0.6637(3) 0.1827(3) 0.0582(12) Uani 1 1 d . . . H41D H 0.3954 0.6922 0.1711 0.087 Uiso 1 1 calc R . . H41E H 0.5366 0.7022 0.1329 0.087 Uiso 1 1 calc R . . H41F H 0.4980 0.6722 0.2426 0.087 Uiso 1 1 calc R . . C42 C 0.5082(3) 0.5329(3) 0.0935(2) 0.0384(8) Uani 1 1 d . . . H42D H 0.5363 0.4576 0.0947 0.058 Uiso 1 1 calc R . . H42E H 0.5571 0.5717 0.0428 0.058 Uiso 1 1 calc R . . H42F H 0.4169 0.5610 0.0838 0.058 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 0.0174(2) 0.0186(2) 0.0208(2) -0.00651(15) -0.00004(15) -0.00276(15) N1 0.0178(11) 0.0195(11) 0.0210(11) -0.0052(9) -0.0006(9) -0.0054(9) C1 0.0440(19) 0.0281(16) 0.051(2) -0.0180(15) 0.0164(16) -0.0202(15) Fe2 0.0205(2) 0.0203(2) 0.0182(2) -0.00637(15) -0.00167(15) -0.00640(15) N2 0.0202(11) 0.0202(11) 0.0198(11) -0.0064(9) 0.0008(9) -0.0043(9) C2 0.0233(15) 0.0250(15) 0.0339(16) -0.0069(12) 0.0054(12) -0.0073(12) N3 0.0216(12) 0.0186(11) 0.0195(11) -0.0048(9) 0.0003(9) -0.0065(9) C3 0.0308(17) 0.048(2) 0.0254(16) 0.0081(14) -0.0033(13) -0.0111(15) N4 0.0205(12) 0.0191(11) 0.0233(12) -0.0047(9) -0.0017(9) -0.0045(9) C4 0.0207(13) 0.0188(13) 0.0233(14) -0.0043(11) 0.0011(11) -0.0040(11) N5 0.0240(12) 0.0207(11) 0.0194(11) -0.0065(9) -0.0011(9) -0.0072(9) C5 0.0205(13) 0.0165(13) 0.0252(14) -0.0061(10) -0.0031(11) -0.0023(10) N6 0.0180(11) 0.0204(11) 0.0191(11) -0.0060(9) -0.0006(9) -0.0051(9) C6 0.0199(13) 0.0209(13) 0.0253(14) -0.0084(11) -0.0012(11) -0.0032(11) N7 0.0199(11) 0.0200(11) 0.0187(11) -0.0046(9) -0.0014(9) -0.0067(9) C7 0.0217(14) 0.0237(14) 0.0338(16) -0.0100(12) 0.0019(12) -0.0013(11) N8 0.0243(12) 0.0210(12) 0.0217(12) -0.0036(9) -0.0018(9) -0.0089(9) C8 0.0236(15) 0.0287(15) 0.0281(15) -0.0098(12) 0.0047(12) -0.0054(12) C9 0.0215(13) 0.0255(14) 0.0193(13) -0.0073(11) 0.0016(11) -0.0067(11) C10 0.0209(14) 0.0223(14) 0.0206(14) -0.0060(11) 0.0035(11) -0.0061(11) C11 0.0275(15) 0.0279(15) 0.0282(15) -0.0091(12) -0.0031(12) -0.0091(12) C12 0.0269(15) 0.0326(16) 0.0310(16) -0.0056(13) 0.0087(13) -0.0105(13) C13 0.0245(14) 0.0196(13) 0.0174(13) -0.0034(10) 0.0019(11) -0.0088(11) C14 0.0302(15) 0.0250(14) 0.0248(15) -0.0081(11) -0.0009(12) -0.0101(12) C15 0.0301(15) 0.0271(15) 0.0237(15) -0.0056(12) -0.0065(12) -0.0095(12) C16 0.0234(14) 0.0209(13) 0.0218(14) -0.0058(11) -0.0024(11) -0.0084(11) C17 0.0237(14) 0.0228(14) 0.0227(14) -0.0029(11) -0.0052(11) -0.0077(11) C18 0.0229(14) 0.0213(14) 0.0317(16) -0.0082(12) -0.0029(12) -0.0019(11) C19 0.0232(16) 0.0360(18) 0.059(2) -0.0178(16) -0.0036(15) -0.0026(13) C20 0.0363(19) 0.0387(19) 0.056(2) -0.0291(17) -0.0122(16) 0.0058(15) C21 0.051(2) 0.0242(16) 0.051(2) -0.0073(15) 0.0040(17) -0.0052(15) C22 0.052(2) 0.0393(18) 0.0285(17) -0.0087(14) -0.0111(15) -0.0171(16) C23 0.0451(19) 0.0343(17) 0.0383(18) -0.0132(14) -0.0003(15) -0.0208(15) C24 0.0410(19) 0.044(2) 0.045(2) -0.0293(17) -0.0068(16) 0.0008(16) C25 0.0325(16) 0.0275(15) 0.0212(14) -0.0098(11) -0.0036(12) -0.0091(12) C26 0.0214(14) 0.0227(14) 0.0259(15) -0.0040(11) -0.0030(11) -0.0053(11) C27 0.0208(13) 0.0171(13) 0.0232(14) -0.0040(10) -0.0024(11) -0.0042(10) C28 0.0208(14) 0.0196(13) 0.0300(15) -0.0055(11) -0.0030(11) -0.0024(11) C29 0.0219(14) 0.0212(14) 0.0298(15) -0.0106(11) 0.0007(11) -0.0056(11) C30 0.0207(13) 0.0180(13) 0.0207(13) -0.0067(10) 0.0036(10) -0.0076(10) C31 0.0212(13) 0.0201(13) 0.0176(13) -0.0039(10) 0.0012(10) -0.0080(11) C32 0.0267(15) 0.0214(14) 0.0287(15) -0.0071(11) -0.0034(12) -0.0073(12) C33 0.0312(16) 0.0368(17) 0.0216(15) -0.0063(12) 0.0041(12) -0.0172(13) C34 0.0207(13) 0.0181(13) 0.0216(14) -0.0068(10) -0.0018(11) -0.0031(10) C35 0.0330(16) 0.0226(14) 0.0177(13) -0.0052(11) -0.0019(11) -0.0069(12) C36 0.0348(16) 0.0207(14) 0.0241(14) -0.0080(11) -0.0086(12) -0.0072(12) C37 0.0221(13) 0.0172(13) 0.0234(14) -0.0047(10) -0.0051(11) -0.0049(10) C38 0.0239(14) 0.0179(13) 0.0269(15) -0.0050(11) -0.0084(11) -0.0067(11) C39 0.0262(15) 0.0292(15) 0.0251(15) -0.0034(12) -0.0001(12) -0.0146(12) C40 0.035(2) 0.098(4) 0.051(2) -0.002(2) -0.0047(18) -0.033(2) C41 0.102(3) 0.036(2) 0.041(2) -0.0083(17) 0.016(2) -0.038(2) C42 0.043(2) 0.044(2) 0.0306(17) -0.0058(14) 0.0023(15) -0.0221(16) _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 N6 2.016(2) . ? Fe1 N2 2.021(2) . ? Fe1 N1 2.104(2) . ? Fe1 N5 2.107(2) . ? N1 C5 1.296(3) . ? N1 C4 1.492(3) . ? C1 C4 1.533(4) . ? Fe2 N3 2.019(2) . ? Fe2 N7 2.021(2) . ? Fe2 N4 2.113(2) . ? Fe2 N8 2.115(2) . ? N2 C9 1.366(3) . ? N2 C6 1.382(3) . ? C2 C4 1.519(4) . ? N3 C13 1.360(3) . ? N3 C16 1.387(3) . ? C3 C4 1.519(4) . ? N4 C17 1.292(4) . ? N4 C18 1.495(3) . ? N5 C26 1.301(3) . ? N5 C25 1.489(3) . ? C5 C6 1.419(4) . ? N6 C30 1.356(3) . ? N6 C27 1.394(3) . ? C6 C7 1.391(4) . ? N7 C34 1.362(3) . ? N7 C37 1.383(3) . ? C7 C8 1.395(4) . ? N8 C38 1.299(4) . ? N8 C39 1.489(3) . ? C8 C9 1.397(4) . ? C9 C10 1.509(4) . ? C10 C13 1.510(4) . ? C10 C12 1.541(4) . ? C10 C11 1.543(4) . ? C13 C14 1.398(4) . ? C14 C15 1.394(4) . ? C15 C16 1.389(4) . ? C16 C17 1.425(4) . ? C18 C20 1.506(4) . ? C18 C21 1.529(4) . ? C18 C19 1.530(4) . ? C22 C25 1.528(4) . ? C23 C25 1.529(4) . ? C24 C25 1.517(4) . ? C26 C27 1.416(4) . ? C27 C28 1.387(4) . ? C28 C29 1.389(4) . ? C29 C30 1.401(4) . ? C30 C31 1.518(4) . ? C31 C34 1.512(4) . ? C31 C32 1.537(4) . ? C31 C33 1.539(4) . ? C34 C35 1.396(4) . ? C35 C36 1.401(4) . ? C36 C37 1.387(4) . ? C37 C38 1.423(4) . ? C39 C42 1.505(4) . ? C39 C40 1.512(5) . ? C39 C41 1.532(5) . ? 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 N6 Fe1 N2 137.35(9) . . ? N6 Fe1 N1 124.89(9) . . ? N2 Fe1 N1 82.85(9) . . ? N6 Fe1 N5 83.69(9) . . ? N2 Fe1 N5 119.72(9) . . ? N1 Fe1 N5 109.79(9) . . ? C5 N1 C4 119.6(2) . . ? C5 N1 Fe1 107.94(17) . . ? C4 N1 Fe1 132.31(16) . . ? N3 Fe2 N7 139.11(9) . . ? N3 Fe2 N4 83.57(9) . . ? N7 Fe2 N4 119.11(9) . . ? N3 Fe2 N8 124.86(9) . . ? N7 Fe2 N8 82.53(9) . . ? N4 Fe2 N8 108.09(9) . . ? C9 N2 C6 106.5(2) . . ? C9 N2 Fe1 143.26(19) . . ? C6 N2 Fe1 107.90(17) . . ? C13 N3 C16 106.2(2) . . ? C13 N3 Fe2 144.64(18) . . ? C16 N3 Fe2 108.63(17) . . ? C17 N4 C18 119.6(2) . . ? C17 N4 Fe2 107.78(18) . . ? C18 N4 Fe2 132.56(18) . . ? N1 C4 C3 109.2(2) . . ? N1 C4 C2 106.8(2) . . ? C3 C4 C2 110.1(2) . . ? N1 C4 C1 110.3(2) . . ? C3 C4 C1 111.1(3) . . ? C2 C4 C1 109.3(2) . . ? C26 N5 C25 119.1(2) . . ? C26 N5 Fe1 108.03(18) . . ? C25 N5 Fe1 132.72(18) . . ? N1 C5 C6 120.3(2) . . ? C30 N6 C27 106.2(2) . . ? C30 N6 Fe1 144.99(18) . . ? C27 N6 Fe1 108.46(17) . . ? N2 C6 C7 109.9(2) . . ? N2 C6 C5 118.2(2) . . ? C7 C6 C5 131.9(3) . . ? C34 N7 C37 106.5(2) . . ? C34 N7 Fe2 142.76(18) . . ? C37 N7 Fe2 108.17(17) . . ? C6 C7 C8 106.5(2) . . ? C38 N8 C39 119.4(2) . . ? C38 N8 Fe2 107.75(18) . . ? C39 N8 Fe2 132.55(18) . . ? C7 C8 C9 107.1(2) . . ? N2 C9 C8 109.8(2) . . ? N2 C9 C10 120.9(2) . . ? C8 C9 C10 128.9(2) . . ? C9 C10 C13 110.9(2) . . ? C9 C10 C12 110.3(2) . . ? C13 C10 C12 108.3(2) . . ? C9 C10 C11 107.9(2) . . ? C13 C10 C11 111.8(2) . . ? C12 C10 C11 107.7(2) . . ? N3 C13 C14 110.1(2) . . ? N3 C13 C10 123.3(2) . . ? C14 C13 C10 126.3(3) . . ? C15 C14 C13 107.1(3) . . ? C16 C15 C14 106.4(2) . . ? N3 C16 C15 110.2(2) . . ? N3 C16 C17 118.3(2) . . ? C15 C16 C17 131.5(3) . . ? N4 C17 C16 121.2(2) . . ? N4 C18 C20 107.5(2) . . ? N4 C18 C21 108.4(2) . . ? C20 C18 C21 110.8(3) . . ? N4 C18 C19 111.0(2) . . ? C20 C18 C19 109.7(3) . . ? C21 C18 C19 109.3(3) . . ? N5 C25 C24 106.8(2) . . ? N5 C25 C22 111.8(2) . . ? C24 C25 C22 109.5(3) . . ? N5 C25 C23 109.0(2) . . ? C24 C25 C23 109.8(3) . . ? C22 C25 C23 109.9(3) . . ? N5 C26 C27 120.7(3) . . ? C28 C27 N6 109.9(2) . . ? C28 C27 C26 131.4(3) . . ? N6 C27 C26 118.7(2) . . ? C27 C28 C29 106.7(2) . . ? C28 C29 C30 107.1(2) . . ? N6 C30 C29 110.2(2) . . ? N6 C30 C31 123.3(2) . . ? C29 C30 C31 126.2(2) . . ? C34 C31 C30 109.8(2) . . ? C34 C31 C32 108.5(2) . . ? C30 C31 C32 112.0(2) . . ? C34 C31 C33 110.4(2) . . ? C30 C31 C33 108.1(2) . . ? C32 C31 C33 108.0(2) . . ? N7 C34 C35 109.8(2) . . ? N7 C34 C31 120.9(2) . . ? C35 C34 C31 129.0(2) . . ? C34 C35 C36 107.2(2) . . ? C37 C36 C35 106.1(2) . . ? N7 C37 C36 110.3(2) . . ? N7 C37 C38 118.0(2) . . ? C36 C37 C38 131.7(3) . . ? N8 C38 C37 120.2(2) . . ? N8 C39 C42 107.3(2) . . ? N8 C39 C40 108.7(3) . . ? C42 C39 C40 110.1(3) . . ? N8 C39 C41 110.6(3) . . ? C42 C39 C41 109.3(3) . . ? C40 C39 C41 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.261 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.077