data_Fe(TPP)(Hdmpz) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(TPP)(Hdmpz) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C49 H36 Fe N6' _chemical_formula_sum 'C49 H36 Fe N6' _chemical_formula_weight 764.69 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 Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3032(2) _cell_length_b 30.8656(6) _cell_length_c 11.7462(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.3580(10) _cell_angle_gamma 90.00 _cell_volume 3951.67(12) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 2.2304 _cell_measurement_theta_min 29.9820 _cell_measurement_theta_max 8746 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8352 _exptl_absorpt_correction_T_max 0.9124 _exptl_absorpt_process_details 'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 84805 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.50 _reflns_number_total 11989 _reflns_number_gt 8806 _reflns_threshold_expression >2sigma(I) #References and fields for routine structure determination _publ_section_references ; Bruker-Nonius AXS. (2007). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2005). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2007). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT/XPREP (Bruker,2007; Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material 'XCIF (Sheldrick, 2008)/enCIFER (CCDC, 2005)' _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^)+(0.0650P)^2^+0.9198P] 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 11989 _refine_ls_number_parameters 582 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.023 _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 0.375535(19) 0.131933(6) 0.805766(18) 0.03768(7) Uani 1 1 d . . . N1 N 0.34128(12) 0.19179(4) 0.87026(11) 0.0401(3) Uani 1 1 d . C . N2 N 0.26137(11) 0.10397(4) 0.89542(11) 0.0408(3) Uani 1 1 d . C . N3 N 0.44794(11) 0.07058(4) 0.78972(11) 0.0398(3) Uani 1 1 d . C . N4 N 0.53049(12) 0.15819(4) 0.76945(11) 0.0410(3) Uani 1 1 d . C . C(A1 C 0.39624(15) 0.23049(5) 0.85671(13) 0.0416(3) Uani 1 1 d . . . C(A2 C 0.25196(14) 0.20092(5) 0.92674(13) 0.0411(3) Uani 1 1 d . . . C(A3 C 0.18342(14) 0.12552(5) 0.94834(13) 0.0426(3) Uani 1 1 d . . . C(A4 C 0.23978(14) 0.06045(5) 0.90426(13) 0.0423(3) Uani 1 1 d . . . C(A5 C 0.39836(14) 0.03178(5) 0.81108(13) 0.0421(3) Uani 1 1 d . . . C(A6 C 0.54445(14) 0.06096(5) 0.74392(14) 0.0417(3) Uani 1 1 d . . . C(A7 C 0.61351(14) 0.13666(5) 0.72284(14) 0.0413(3) Uani 1 1 d . . . C(A8 C 0.55364(14) 0.20167(5) 0.76345(13) 0.0416(3) Uani 1 1 d . . . C(B1 C 0.33859(17) 0.26500(5) 0.90556(15) 0.0510(4) Uani 1 1 d . C . H(B1 H 0.3587 0.2943 0.9074 0.061 Uiso 1 1 calc R . . C(B2 C 0.25036(16) 0.24705(5) 0.94795(15) 0.0502(4) Uani 1 1 d . C . H(B2 H 0.1981 0.2616 0.9841 0.060 Uiso 1 1 calc R . . C(B3 C 0.11171(16) 0.09419(6) 0.99230(16) 0.0520(4) Uani 1 1 d . C . H(B3 H 0.0523 0.1003 1.0318 0.062 Uiso 1 1 calc R . . C(B4 C 0.14653(17) 0.05446(6) 0.96570(16) 0.0532(4) Uani 1 1 d . C . H(B4 H 0.1159 0.0281 0.9837 0.064 Uiso 1 1 calc R . . C(B5 C 0.46630(16) -0.00326(5) 0.77686(16) 0.0524(4) Uani 1 1 d . C . H(B5 H 0.4509 -0.0327 0.7817 0.063 Uiso 1 1 calc R . . C(B6 C 0.55624(17) 0.01468(5) 0.73651(17) 0.0532(4) Uani 1 1 d . C . H(B6 H 0.6149 -0.0001 0.7090 0.064 Uiso 1 1 calc R . . C(B7 C 0.69069(16) 0.16798(5) 0.68641(16) 0.0515(4) Uani 1 1 d . C . H(B7 H 0.7543 0.1620 0.6522 0.062 Uiso 1 1 calc R . . C(B8 C 0.65357(16) 0.20762(5) 0.71122(16) 0.0521(4) Uani 1 1 d . C . H(B8 H 0.6868 0.2340 0.6970 0.062 Uiso 1 1 calc R . . C(M1 C 0.17640(14) 0.17046(5) 0.96081(13) 0.0419(3) Uani 1 1 d . C . C(M2 C 0.29977(14) 0.02675(5) 0.86153(13) 0.0414(3) Uani 1 1 d . C . C(M3 C 0.62114(13) 0.09175(5) 0.71045(13) 0.0411(3) Uani 1 1 d . C . C(M4 C 0.49243(15) 0.23556(5) 0.80410(13) 0.0416(3) Uani 1 1 d . B . C11 C 0.08060(14) 0.18753(5) 1.01613(14) 0.0451(3) Uani 1 1 d . . . C12 C -0.03830(18) 0.19285(8) 0.95014(19) 0.0696(5) Uani 1 1 d . C . H12 H -0.0597 0.1856 0.8704 0.084 Uiso 1 1 calc R . . C13 C -0.1267(2) 0.20888(9) 1.0008(2) 0.0864(7) Uani 1 1 d . . . H13 H -0.2070 0.2122 0.9551 0.104 Uiso 1 1 calc R C . C14 C -0.0969(2) 0.21976(7) 1.1170(2) 0.0745(6) Uani 1 1 d . C . H14 H -0.1566 0.2308 1.1504 0.089 Uiso 1 1 calc R . . C15 C 0.0195(2) 0.21462(7) 1.18401(19) 0.0702(5) Uani 1 1 d . . . H15 H 0.0396 0.2218 1.2637 0.084 Uiso 1 1 calc R C . C16 C 0.10903(18) 0.19863(7) 1.13417(16) 0.0587(4) Uani 1 1 d . C . H16 H 0.1890 0.1953 1.1807 0.070 Uiso 1 1 calc R . . C21 C 0.25262(15) -0.01810(5) 0.86940(14) 0.0446(3) Uani 1 1 d . . . C22 C 0.3145(2) -0.04770(6) 0.95325(17) 0.0617(5) Uani 1 1 d . C . H22 H 0.3886 -0.0400 1.0058 0.074 Uiso 1 1 calc R . . C23 C 0.2661(3) -0.08849(6) 0.9587(2) 0.0784(7) Uani 1 1 d . . . H23 H 0.3076 -0.1080 1.0156 0.094 Uiso 1 1 calc R C . C24 C 0.1581(3) -0.10045(7) 0.8815(3) 0.0835(8) Uani 1 1 d . C . H24 H 0.1264 -0.1280 0.8855 0.100 Uiso 1 1 calc R . . C25 C 0.0970(2) -0.07162(8) 0.7986(3) 0.0854(7) Uani 1 1 d . . . H25 H 0.0235 -0.0797 0.7457 0.102 Uiso 1 1 calc R C . C26 C 0.14318(18) -0.03063(6) 0.79252(19) 0.0631(5) Uani 1 1 d . C . H26 H 0.1002 -0.0112 0.7360 0.076 Uiso 1 1 calc R . . C31 C 0.71980(15) 0.07494(5) 0.65826(14) 0.0457(3) Uani 1 1 d . . . C32 C 0.84223(17) 0.07982(6) 0.71733(18) 0.0593(4) Uani 1 1 d . C . H32 H 0.8638 0.0922 0.7922 0.071 Uiso 1 1 calc R . . C33 C 0.93326(19) 0.06638(7) 0.6656(2) 0.0726(6) Uani 1 1 d . . . H33 H 1.0153 0.0701 0.7058 0.087 Uiso 1 1 calc R C . C34 C 0.9033(2) 0.04777(8) 0.5566(2) 0.0780(6) Uani 1 1 d . C . H34 H 0.9646 0.0393 0.5219 0.094 Uiso 1 1 calc R . . C35 C 0.7820(2) 0.04155(8) 0.4980(2) 0.0775(6) Uani 1 1 d . . . H35 H 0.7615 0.0283 0.4242 0.093 Uiso 1 1 calc R C . C36 C 0.69003(19) 0.05493(7) 0.54834(17) 0.0608(4) Uani 1 1 d . C . H36 H 0.6082 0.0505 0.5084 0.073 Uiso 1 1 calc R . . C41 C 0.53593(15) 0.28079(5) 0.79119(14) 0.0447(3) Uani 1 1 d . . . C44 C 0.6175(3) 0.36439(6) 0.7663(2) 0.0731(6) Uani 1 1 d . . . H44 H 0.6467 0.3922 0.7597 0.088 Uiso 1 1 calc R A 1 C42A C 0.5985(12) 0.3029(4) 0.8859(10) 0.061(2) Uani 0.53(2) 1 d P B 1 H42A H 0.6160 0.2903 0.9605 0.073 Uiso 0.53(2) 1 calc PR B 1 C43A C 0.6364(13) 0.3439(4) 0.8718(11) 0.074(3) Uani 0.53(2) 1 d P B 1 H43A H 0.6781 0.3589 0.9391 0.088 Uiso 0.53(2) 1 calc PR B 1 C45A C 0.5516(13) 0.3412(4) 0.6692(11) 0.071(2) Uani 0.53(2) 1 d P B 1 H45A H 0.5363 0.3538 0.5948 0.085 Uiso 0.53(2) 1 calc PR B 1 C46A C 0.5069(12) 0.2990(3) 0.6789(9) 0.0570(19) Uani 0.53(2) 1 d P B 1 H46A H 0.4603 0.2841 0.6134 0.068 Uiso 0.53(2) 1 calc PR B 1 C42B C 0.6393(15) 0.2988(4) 0.8738(13) 0.070(3) Uani 0.47(2) 1 d P B 2 H42B H 0.6808 0.2819 0.9374 0.085 Uiso 0.47(2) 1 calc PR B 2 C43B C 0.6819(15) 0.3413(5) 0.8637(14) 0.077(3) Uani 0.47(2) 1 d P B 2 H43B H 0.7490 0.3529 0.9189 0.092 Uiso 0.47(2) 1 calc PR B 2 C45B C 0.5188(15) 0.3488(5) 0.6865(15) 0.079(3) Uani 0.47(2) 1 d P B 2 H45B H 0.4764 0.3658 0.6236 0.095 Uiso 0.47(2) 1 calc PR B 2 C46B C 0.4828(14) 0.3081(5) 0.6994(13) 0.067(3) Uani 0.47(2) 1 d P B 2 H46B H 0.4163 0.2974 0.6415 0.081 Uiso 0.47(2) 1 calc PR B 2 N5A N 0.26399(18) 0.13177(7) 0.62618(16) 0.0529(4) Uani 0.920(2) 1 d P C -1 N6A N 0.31368(19) 0.11241(7) 0.54559(16) 0.0751(6) Uani 0.920(2) 1 d P C -1 H6AA H 0.3839 0.0997 0.5637 0.090 Uiso 0.920(2) 1 calc PR C -1 C1A C 0.2423(2) 0.11517(9) 0.43556(19) 0.0738(7) Uani 0.920(2) 1 d P C -1 C2A C 0.1404(3) 0.13674(9) 0.4444(2) 0.0652(5) Uani 0.920(2) 1 d P C -1 H2AA H 0.0724 0.1436 0.3828 0.078 Uiso 0.920(2) 1 calc PR C -1 C3A C 0.15735(18) 0.14662(6) 0.56350(18) 0.0517(4) Uani 0.920(2) 1 d P C -1 C4A C 0.2815(4) 0.09584(15) 0.3335(3) 0.1307(16) Uani 0.920(2) 1 d P C -1 H4AA H 0.3693 0.0966 0.3502 0.196 Uiso 0.920(2) 1 calc PR C -1 H4AB H 0.2463 0.1122 0.2632 0.196 Uiso 0.920(2) 1 calc PR C -1 H4AC H 0.2538 0.0664 0.3220 0.196 Uiso 0.920(2) 1 calc PR C -1 C5A C 0.0752(2) 0.17118(8) 0.6204(2) 0.0734(6) Uani 0.920(2) 1 d P C -1 H5AA H 0.0584 0.1540 0.6825 0.110 Uiso 0.920(2) 1 calc PR C -1 H5AB H -0.0004 0.1777 0.5627 0.110 Uiso 0.920(2) 1 calc PR C -1 H5AC H 0.1145 0.1977 0.6527 0.110 Uiso 0.920(2) 1 calc PR C -1 N5B N 0.2573(13) 0.1366(7) 0.6287(11) 0.0529(4) Uani 0.080(2) 1 d PGU C -2 N6B N 0.1462(13) 0.1555(6) 0.6216(10) 0.050(2) Uani 0.080(2) 1 d PGU C -2 H6BA H 0.1264 0.1665 0.6813 0.060 Uiso 0.080(2) 1 calc PR C -2 C1B C 0.0718(11) 0.1552(4) 0.5125(10) 0.057(2) Uani 0.080(2) 1 d PGU C -2 C2B C 0.1366(14) 0.1360(7) 0.4437(10) 0.0652(5) Uani 0.080(2) 1 d PGU C -2 H2BA H 0.1103 0.1312 0.3628 0.078 Uiso 0.080(2) 1 calc PR C -2 C3B C 0.2518(12) 0.1247(5) 0.5199(12) 0.059(2) Uani 0.080(2) 1 d PGU C -2 C4B C -0.0568(13) 0.1743(7) 0.4867(16) 0.069(5) Uani 0.080(2) 1 d PGU C -2 H4BA H -0.0620 0.1933 0.5500 0.103 Uiso 0.080(2) 1 calc PR C -2 H4BB H -0.1156 0.1513 0.4797 0.103 Uiso 0.080(2) 1 calc PR C -2 H4BC H -0.0738 0.1904 0.4142 0.103 Uiso 0.080(2) 1 calc PR C -2 C5B C 0.3570(15) 0.1015(7) 0.4913(18) 0.071(5) Uani 0.080(2) 1 d PGU C -2 H5BA H 0.4231 0.0986 0.5617 0.107 Uiso 0.080(2) 1 calc PR C -2 H5BB H 0.3846 0.1177 0.4336 0.107 Uiso 0.080(2) 1 calc PR C -2 H5BC H 0.3307 0.0733 0.4605 0.107 Uiso 0.080(2) 1 calc PR C -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 Fe1 0.04042(12) 0.03411(11) 0.04126(12) -0.00127(8) 0.01564(9) -0.00011(8) N1 0.0434(7) 0.0365(6) 0.0431(6) -0.0022(5) 0.0160(5) 0.0008(5) N2 0.0425(7) 0.0375(6) 0.0459(6) -0.0030(5) 0.0180(5) -0.0005(5) N3 0.0420(6) 0.0356(6) 0.0447(6) 0.0005(5) 0.0169(5) 0.0006(5) N4 0.0444(7) 0.0358(6) 0.0471(6) -0.0009(5) 0.0196(5) 0.0005(5) C(A1 0.0491(8) 0.0349(7) 0.0418(7) 0.0006(5) 0.0141(6) 0.0026(6) C(A2 0.0420(8) 0.0401(7) 0.0422(7) -0.0025(6) 0.0128(6) 0.0064(6) C(A3 0.0413(8) 0.0458(8) 0.0440(7) -0.0041(6) 0.0168(6) -0.0013(6) C(A4 0.0438(8) 0.0406(7) 0.0454(7) -0.0028(6) 0.0171(6) -0.0049(6) C(A5 0.0443(8) 0.0356(7) 0.0475(8) -0.0032(6) 0.0143(6) -0.0020(6) C(A6 0.0435(8) 0.0370(7) 0.0478(8) -0.0025(6) 0.0176(6) 0.0024(6) C(A7 0.0418(8) 0.0414(7) 0.0442(7) -0.0007(6) 0.0177(6) -0.0005(6) C(A8 0.0465(8) 0.0372(7) 0.0441(7) 0.0009(6) 0.0172(6) -0.0030(6) C(B1 0.0647(10) 0.0353(7) 0.0577(9) 0.0018(6) 0.0242(8) 0.0072(7) C(B2 0.0581(10) 0.0408(8) 0.0568(9) 0.0005(7) 0.0245(8) 0.0113(7) C(B3 0.0531(9) 0.0521(9) 0.0602(10) -0.0077(7) 0.0316(8) -0.0073(7) C(B4 0.0588(10) 0.0470(8) 0.0625(10) -0.0043(7) 0.0312(8) -0.0101(7) C(B5 0.0586(10) 0.0344(7) 0.0699(10) -0.0072(7) 0.0270(8) -0.0020(7) C(B6 0.0575(10) 0.0389(8) 0.0711(11) -0.0068(7) 0.0309(8) 0.0024(7) C(B7 0.0537(9) 0.0476(8) 0.0630(10) -0.0017(7) 0.0324(8) -0.0044(7) C(B8 0.0567(10) 0.0434(8) 0.0645(10) -0.0011(7) 0.0307(8) -0.0079(7) C(M1 0.0389(7) 0.0463(8) 0.0423(7) -0.0039(6) 0.0137(6) 0.0034(6) C(M2 0.0433(8) 0.0367(7) 0.0447(7) -0.0021(6) 0.0124(6) -0.0045(6) C(M3 0.0417(8) 0.0422(7) 0.0427(7) -0.0036(6) 0.0169(6) 0.0022(6) C(M4 0.0499(8) 0.0348(7) 0.0409(7) 0.0016(5) 0.0134(6) -0.0012(6) C11 0.0437(8) 0.0449(8) 0.0510(8) -0.0032(6) 0.0199(7) 0.0037(6) C12 0.0513(11) 0.0958(15) 0.0611(11) -0.0077(10) 0.0137(9) 0.0167(10) C13 0.0495(11) 0.113(2) 0.0978(17) -0.0073(15) 0.0212(11) 0.0263(12) C14 0.0686(13) 0.0710(13) 0.0991(16) -0.0098(11) 0.0489(13) 0.0126(10) C15 0.0813(15) 0.0728(13) 0.0689(12) -0.0173(10) 0.0413(11) 0.0004(11) C16 0.0538(10) 0.0723(12) 0.0524(9) -0.0111(8) 0.0184(8) 0.0052(8) C21 0.0530(9) 0.0367(7) 0.0493(8) -0.0049(6) 0.0228(7) -0.0062(6) C22 0.0834(13) 0.0467(9) 0.0544(10) 0.0033(7) 0.0172(9) -0.0043(9) C23 0.129(2) 0.0434(9) 0.0796(14) 0.0084(9) 0.0565(15) -0.0008(11) C24 0.1064(18) 0.0446(10) 0.127(2) -0.0200(12) 0.0790(17) -0.0244(12) C25 0.0660(13) 0.0664(13) 0.130(2) -0.0321(14) 0.0373(14) -0.0286(11) C26 0.0542(10) 0.0540(10) 0.0796(13) -0.0088(9) 0.0149(9) -0.0090(8) C31 0.0480(9) 0.0428(7) 0.0519(8) 0.0000(6) 0.0232(7) 0.0038(6) C32 0.0506(10) 0.0639(11) 0.0655(11) -0.0056(8) 0.0189(8) 0.0072(8) C33 0.0521(11) 0.0748(13) 0.0952(16) 0.0018(12) 0.0270(11) 0.0145(10) C34 0.0754(15) 0.0821(14) 0.0918(16) 0.0006(12) 0.0488(13) 0.0241(11) C35 0.0853(16) 0.0905(16) 0.0667(12) -0.0144(11) 0.0377(12) 0.0179(12) C36 0.0603(11) 0.0692(11) 0.0566(10) -0.0104(8) 0.0218(8) 0.0070(9) C41 0.0550(9) 0.0356(7) 0.0462(8) 0.0017(6) 0.0184(7) -0.0013(6) C44 0.1027(18) 0.0411(9) 0.0822(14) 0.0058(9) 0.0363(14) -0.0115(10) C42A 0.096(6) 0.042(3) 0.042(2) -0.0070(18) 0.015(4) -0.013(4) C43A 0.100(7) 0.052(3) 0.066(3) -0.016(2) 0.017(5) -0.031(5) C45A 0.085(7) 0.063(4) 0.063(3) 0.020(3) 0.018(4) -0.014(4) C46A 0.077(5) 0.044(4) 0.046(2) 0.005(2) 0.009(2) -0.012(3) C42B 0.095(8) 0.040(3) 0.063(5) 0.007(3) -0.003(4) -0.004(4) C43B 0.087(7) 0.051(3) 0.083(5) 0.000(3) 0.005(5) -0.028(5) C45B 0.080(6) 0.063(5) 0.091(7) 0.045(5) 0.016(4) 0.006(4) C46B 0.069(5) 0.056(5) 0.065(6) 0.013(4) -0.004(4) -0.007(4) N5A 0.0537(8) 0.0576(9) 0.0456(7) -0.0046(6) 0.0100(6) 0.0089(7) N6A 0.0743(13) 0.0957(15) 0.0506(10) -0.0149(9) 0.0080(9) 0.0306(11) C1A 0.0843(17) 0.0803(15) 0.0492(11) -0.0143(10) 0.0046(11) 0.0132(13) C2A 0.0665(12) 0.0627(11) 0.0547(10) -0.0046(8) -0.0045(9) 0.0050(9) C3A 0.0529(11) 0.0430(9) 0.0563(11) -0.0006(8) 0.0093(9) -0.0020(8) C4A 0.146(3) 0.177(4) 0.0609(16) -0.0392(19) 0.0121(18) 0.057(3) C5A 0.0629(14) 0.0789(15) 0.0777(15) -0.0012(12) 0.0175(11) 0.0150(12) N5B 0.0537(8) 0.0576(9) 0.0456(7) -0.0046(6) 0.0100(6) 0.0089(7) N6B 0.049(4) 0.055(4) 0.047(4) -0.005(4) 0.014(4) 0.009(4) C1B 0.056(4) 0.059(4) 0.053(4) -0.002(4) 0.006(4) 0.006(4) C2B 0.0665(12) 0.0627(11) 0.0547(10) -0.0046(8) -0.0045(9) 0.0050(9) C3B 0.060(3) 0.061(3) 0.050(3) -0.004(3) 0.004(3) 0.007(3) C4B 0.063(8) 0.075(8) 0.057(8) 0.000(7) -0.003(7) 0.008(8) C5B 0.076(9) 0.078(8) 0.054(8) -0.002(8) 0.007(7) 0.010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.0589(12) . ? Fe1 N1 2.0718(12) . ? Fe1 N4 2.0741(12) . ? Fe1 N3 2.0912(12) . ? Fe1 N5A 2.1519(18) . ? Fe1 N5B 2.159(11) . ? N1 C(A1 1.3750(19) . ? N1 C(A2 1.3761(19) . ? N2 C(A4 1.3739(19) . ? N2 C(A3 1.3767(19) . ? N3 C(A6 1.3706(19) . ? N3 C(A5 1.3733(19) . ? N4 C(A8 1.3728(19) . ? N4 C(A7 1.3762(19) . ? C(A1 C(M4 1.394(2) . ? C(A1 C(B1 1.444(2) . ? C(A2 C(M1 1.398(2) . ? C(A2 C(B2 1.446(2) . ? C(A3 C(M1 1.399(2) . ? C(A3 C(B3 1.442(2) . ? C(A4 C(M2 1.405(2) . ? C(A4 C(B4 1.438(2) . ? C(A5 C(M2 1.402(2) . ? C(A5 C(B5 1.444(2) . ? C(A6 C(M3 1.411(2) . ? C(A6 C(B6 1.440(2) . ? C(A7 C(M3 1.399(2) . ? C(A7 C(B7 1.441(2) . ? C(A8 C(M4 1.406(2) . ? C(A8 C(B8 1.433(2) . ? C(B1 C(B2 1.346(2) . ? C(B1 H(B1 0.9300 . ? C(B2 H(B2 0.9300 . ? C(B3 C(B4 1.349(2) . ? C(B3 H(B3 0.9300 . ? C(B4 H(B4 0.9300 . ? C(B5 C(B6 1.349(2) . ? C(B5 H(B5 0.9300 . ? C(B6 H(B6 0.9300 . ? C(B7 C(B8 1.350(2) . ? C(B7 H(B7 0.9300 . ? C(B8 H(B8 0.9300 . ? C(M1 C11 1.498(2) . ? C(M2 C21 1.495(2) . ? C(M3 C31 1.500(2) . ? C(M4 C41 1.501(2) . ? C11 C12 1.372(3) . ? C11 C16 1.381(2) . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.358(3) . ? C13 H13 0.9300 . ? C14 C15 1.352(3) . ? C14 H14 0.9300 . ? C15 C16 1.387(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.380(2) . ? C21 C22 1.389(2) . ? C22 C23 1.381(3) . ? C22 H22 0.9300 . ? C23 C24 1.365(4) . ? C23 H23 0.9300 . ? C24 C25 1.364(4) . ? C24 H24 0.9300 . ? C25 C26 1.378(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.382(3) . ? C31 C36 1.390(2) . ? C32 C33 1.389(3) . ? C32 H32 0.9300 . ? C33 C34 1.363(3) . ? C33 H33 0.9300 . ? C34 C35 1.375(3) . ? C34 H34 0.9300 . ? C35 C36 1.388(3) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42A 1.336(11) . ? C41 C46B 1.374(14) . ? C41 C46A 1.390(11) . ? C41 C42B 1.419(15) . ? C44 C45B 1.342(17) . ? C44 C43A 1.356(13) . ? C44 C43B 1.381(16) . ? C44 C45A 1.385(14) . ? C44 H44 0.9300 . ? C42A C43A 1.361(16) . ? C42A H42A 0.9300 . ? C43A H43A 0.9300 . ? C45A C46A 1.413(16) . ? C45A H45A 0.9300 . ? C46A H46A 0.9300 . ? C42B C43B 1.413(18) . ? C42B H42B 0.9300 . ? C43B H43B 0.9300 . ? C45B C46B 1.34(2) . ? C45B H45B 0.9300 . ? C46B H46B 0.9300 . ? N5A C3A 1.317(3) . ? N5A N6A 1.360(3) . ? N6A C1A 1.333(3) . ? N6A H6AA 0.8600 . ? C1A C2A 1.357(4) . ? C1A C4A 1.507(4) . ? C2A C3A 1.395(3) . ? C2A H2AA 0.9300 . ? C3A C5A 1.488(3) . ? C4A H4AA 0.9600 . ? C4A H4AB 0.9600 . ? C4A H4AC 0.9600 . ? C5A H5AA 0.9600 . ? C5A H5AB 0.9600 . ? C5A H5AC 0.9600 . ? N5B C3B 1.3145 . ? N5B N6B 1.3676 . ? N6B C1B 1.3338 . ? N6B H6BA 0.8600 . ? C1B C2B 1.3622 . ? C1B C4B 1.5225 . ? C2B C3B 1.4143 . ? C2B H2BA 0.9300 . ? C3B C5B 1.5008 . ? C4B H4BA 0.9600 . ? C4B H4BB 0.9600 . ? C4B H4BC 0.9600 . ? C5B H5BA 0.9600 . ? C5B H5BB 0.9600 . ? C5B H5BC 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 89.07(5) . . ? N2 Fe1 N4 161.22(5) . . ? N1 Fe1 N4 88.66(5) . . ? N2 Fe1 N3 88.84(5) . . ? N1 Fe1 N3 162.93(5) . . ? N4 Fe1 N3 87.90(5) . . ? N2 Fe1 N5A 102.50(7) . . ? N1 Fe1 N5A 104.05(6) . . ? N4 Fe1 N5A 96.13(7) . . ? N3 Fe1 N5A 92.94(6) . . ? N2 Fe1 N5B 102.0(5) . . ? N1 Fe1 N5B 99.5(5) . . ? N4 Fe1 N5B 96.7(5) . . ? N3 Fe1 N5B 97.5(5) . . ? N5A Fe1 N5B 4.6(5) . . ? C(A1 N1 C(A2 106.83(12) . . ? C(A1 N1 Fe1 126.76(10) . . ? C(A2 N1 Fe1 126.23(10) . . ? C(A4 N2 C(A3 106.89(12) . . ? C(A4 N2 Fe1 126.61(10) . . ? C(A3 N2 Fe1 126.24(10) . . ? C(A6 N3 C(A5 106.77(12) . . ? C(A6 N3 Fe1 127.06(10) . . ? C(A5 N3 Fe1 125.80(10) . . ? C(A8 N4 C(A7 107.00(12) . . ? C(A8 N4 Fe1 125.12(10) . . ? C(A7 N4 Fe1 126.52(10) . . ? N1 C(A1 C(M4 125.31(13) . . ? N1 C(A1 C(B1 109.24(13) . . ? C(M4 C(A1 C(B1 125.45(14) . . ? N1 C(A2 C(M1 125.59(13) . . ? N1 C(A2 C(B2 109.21(13) . . ? C(M1 C(A2 C(B2 125.19(14) . . ? N2 C(A3 C(M1 125.95(14) . . ? N2 C(A3 C(B3 108.97(13) . . ? C(M1 C(A3 C(B3 125.06(14) . . ? N2 C(A4 C(M2 125.78(13) . . ? N2 C(A4 C(B4 109.39(13) . . ? C(M2 C(A4 C(B4 124.83(14) . . ? N3 C(A5 C(M2 125.59(13) . . ? N3 C(A5 C(B5 109.24(13) . . ? C(M2 C(A5 C(B5 125.14(14) . . ? N3 C(A6 C(M3 125.11(13) . . ? N3 C(A6 C(B6 109.56(13) . . ? C(M3 C(A6 C(B6 125.33(14) . . ? N4 C(A7 C(M3 125.96(13) . . ? N4 C(A7 C(B7 108.93(13) . . ? C(M3 C(A7 C(B7 125.10(14) . . ? N4 C(A8 C(M4 126.33(13) . . ? N4 C(A8 C(B8 109.26(13) . . ? C(M4 C(A8 C(B8 124.39(14) . . ? C(B2 C(B1 C(A1 107.43(14) . . ? C(B2 C(B1 H(B1 126.3 . . ? C(A1 C(B1 H(B1 126.3 . . ? C(B1 C(B2 C(A2 107.29(14) . . ? C(B1 C(B2 H(B2 126.4 . . ? C(A2 C(B2 H(B2 126.4 . . ? C(B4 C(B3 C(A3 107.48(14) . . ? C(B4 C(B3 H(B3 126.3 . . ? C(A3 C(B3 H(B3 126.3 . . ? C(B3 C(B4 C(A4 107.27(14) . . ? C(B3 C(B4 H(B4 126.4 . . ? C(A4 C(B4 H(B4 126.4 . . ? C(B6 C(B5 C(A5 107.23(14) . . ? C(B6 C(B5 H(B5 126.4 . . ? C(A5 C(B5 H(B5 126.4 . . ? C(B5 C(B6 C(A6 107.19(14) . . ? C(B5 C(B6 H(B6 126.4 . . ? C(A6 C(B6 H(B6 126.4 . . ? C(B8 C(B7 C(A7 107.26(14) . . ? C(B8 C(B7 H(B7 126.4 . . ? C(A7 C(B7 H(B7 126.4 . . ? C(B7 C(B8 C(A8 107.55(14) . . ? C(B7 C(B8 H(B8 126.2 . . ? C(A8 C(B8 H(B8 126.2 . . ? C(A2 C(M1 C(A3 125.51(13) . . ? C(A2 C(M1 C11 117.00(13) . . ? C(A3 C(M1 C11 117.48(13) . . ? C(A5 C(M2 C(A4 125.57(14) . . ? C(A5 C(M2 C21 117.69(13) . . ? C(A4 C(M2 C21 116.73(13) . . ? C(A7 C(M3 C(A6 125.40(13) . . ? C(A7 C(M3 C31 117.27(13) . . ? C(A6 C(M3 C31 117.32(13) . . ? C(A1 C(M4 C(A8 125.36(13) . . ? C(A1 C(M4 C41 117.64(13) . . ? C(A8 C(M4 C41 116.99(13) . . ? C12 C11 C16 118.05(16) . . ? C12 C11 C(M1 120.62(15) . . ? C16 C11 C(M1 121.32(15) . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.00(18) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.15(19) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.67(18) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C26 C21 C22 118.39(16) . . ? C26 C21 C(M2 119.44(15) . . ? C22 C21 C(M2 122.16(15) . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.8(2) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 119.51(19) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.6(2) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.7(2) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C31 C36 118.59(16) . . ? C32 C31 C(M3 120.73(15) . . ? C36 C31 C(M3 120.66(15) . . ? C31 C32 C33 120.47(19) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.77(19) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 120.3(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.25(19) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C42A C41 C46B 111.5(7) . . ? C42A C41 C46A 121.6(7) . . ? C46B C41 C42B 114.0(8) . . ? C46A C41 C42B 115.8(8) . . ? C42A C41 C(M4 120.4(5) . . ? C46B C41 C(M4 124.2(6) . . ? C46A C41 C(M4 118.0(5) . . ? C42B C41 C(M4 121.8(5) . . ? C45B C44 C43A 111.8(7) . . ? C45B C44 C43B 123.4(8) . . ? C43A C44 C45A 115.6(7) . . ? C43B C44 C45A 117.7(8) . . ? C45B C44 H44 121.4 . . ? C43A C44 H44 122.2 . . ? C43B C44 H44 115.1 . . ? C45A C44 H44 122.2 . . ? C41 C42A C43A 119.2(10) . . ? C41 C42A H42A 120.4 . . ? C43A C42A H42A 120.4 . . ? C44 C43A C42A 124.5(9) . . ? C44 C43A H43A 117.7 . . ? C42A C43A H43A 117.7 . . ? C44 C45A C46A 122.4(10) . . ? C44 C45A H45A 118.8 . . ? C46A C45A H45A 118.8 . . ? C41 C46A C45A 116.7(9) . . ? C41 C46A H46A 121.6 . . ? C45A C46A H46A 121.6 . . ? C43B C42B C41 122.9(11) . . ? C43B C42B H42B 118.6 . . ? C41 C42B H42B 118.6 . . ? C44 C43B C42B 115.6(11) . . ? C44 C43B H43B 122.2 . . ? C42B C43B H43B 122.2 . . ? C46B C45B C44 118.6(12) . . ? C46B C45B H45B 120.7 . . ? C44 C45B H45B 120.7 . . ? C45B C46B C41 125.4(13) . . ? C45B C46B H46B 117.3 . . ? C41 C46B H46B 117.3 . . ? C3A N5A N6A 104.43(18) . . ? C3A N5A Fe1 139.38(16) . . ? N6A N5A Fe1 116.14(14) . . ? C1A N6A N5A 113.0(2) . . ? C1A N6A H6AA 123.5 . . ? N5A N6A H6AA 123.5 . . ? N6A C1A C2A 105.4(2) . . ? N6A C1A C4A 121.1(2) . . ? C2A C1A C4A 133.5(2) . . ? C1A C2A C3A 106.9(2) . . ? C1A C2A H2AA 126.6 . . ? C3A C2A H2AA 126.6 . . ? N5A C3A C2A 110.3(2) . . ? N5A C3A C5A 120.9(2) . . ? C2A C3A C5A 128.7(2) . . ? C3B N5B N6B 104.7 . . ? C3B N5B Fe1 140.9(6) . . ? N6B N5B Fe1 114.3(6) . . ? C1B N6B N5B 113.0 . . ? C1B N6B H6BA 123.5 . . ? N5B N6B H6BA 123.5 . . ? N6B C1B C2B 105.8 . . ? N6B C1B C4B 120.9 . . ? C2B C1B C4B 133.3 . . ? C1B C2B C3B 106.3 . . ? C1B C2B H2BA 126.8 . . ? C3B C2B H2BA 126.8 . . ? N5B C3B C2B 110.2 . . ? N5B C3B C5B 120.9 . . ? C2B C3B C5B 128.8 . . ? C1B C4B H4BA 109.5 . . ? C1B C4B H4BB 109.5 . . ? H4BA C4B H4BB 109.5 . . ? C1B C4B H4BC 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? C3B C5B H5BA 109.5 . . ? C3B C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? C3B C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.306 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.044 #===end data_Fe(TOCH3PP)(Hdmpz) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(TOCH3PP)(Hdmpz) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C53 H44 Fe N6 O4, C7 H8' _chemical_formula_sum 'C60 H52 Fe N6 O4' _chemical_formula_weight 976.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9585(3) _cell_length_b 35.4853(9) _cell_length_c 11.9857(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.9490(10) _cell_angle_gamma 90.00 _cell_volume 4865.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9013 _cell_measurement_theta_min 2.4082 _cell_measurement_theta_max 28.2861 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8322 _exptl_absorpt_correction_T_max 0.9303 _exptl_absorpt_process_details 'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.' _exptl_special_details ; ? ; _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 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86053 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.46 _reflns_number_total 12075 _reflns_number_gt 10028 _reflns_threshold_expression >2sigma(I) #References and fields for routine structure determination _publ_section_references ; Bruker-Nonius AXS. (2007). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2005). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2007). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT/XPREP (Bruker,2007; Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material 'XCIF (Sheldrick, 2008)/enCIFER (CCDC, 2005)' _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^)+(0.0548P)^2^+3.1845P] 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 12075 _refine_ls_number_parameters 692 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.025 _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 0.63725(2) 0.144834(6) 0.213710(19) 0.01619(7) Uani 1 1 d . . . N1 N 0.56250(12) 0.09290(4) 0.22528(11) 0.0177(3) Uani 1 1 d . A . N2 N 0.49539(13) 0.17051(4) 0.24516(12) 0.0194(3) Uani 1 1 d . A . N3 N 0.67946(12) 0.19597(4) 0.15224(11) 0.0174(3) Uani 1 1 d . A . N4 N 0.74507(12) 0.11836(4) 0.13033(12) 0.0179(3) Uani 1 1 d . A . C(A1 C 0.60159(14) 0.05820(4) 0.20197(13) 0.0176(3) Uani 1 1 d . . . C(A2 C 0.46702(14) 0.08643(4) 0.26378(13) 0.0177(3) Uani 1 1 d . . . C(A3 C 0.41316(15) 0.15318(4) 0.28707(14) 0.0197(3) Uani 1 1 d . . . C(A4 C 0.47883(15) 0.20867(4) 0.25315(15) 0.0214(3) Uani 1 1 d . . . C(A5 C 0.63708(14) 0.23053(4) 0.17130(13) 0.0171(3) Uani 1 1 d . . . C(A6 C 0.77103(14) 0.20272(4) 0.10753(13) 0.0175(3) Uani 1 1 d . . . C(A7 C 0.82477(14) 0.13568(4) 0.08411(13) 0.0177(3) Uani 1 1 d . . . C(A8 C 0.75983(14) 0.08020(4) 0.12091(13) 0.0175(3) Uani 1 1 d . . . C(B1 C 0.52850(15) 0.02901(4) 0.22837(14) 0.0201(3) Uani 1 1 d . A . H(B1 H 0.5370 0.0026 0.2203 0.024 Uiso 1 1 calc R . . C(B2 C 0.44595(14) 0.04633(4) 0.26670(14) 0.0187(3) Uani 1 1 d . A . H(B2 H 0.3857 0.0345 0.2909 0.022 Uiso 1 1 calc R . . C(B3 C 0.34360(16) 0.18121(5) 0.32291(16) 0.0246(4) Uani 1 1 d . A . H(B3 H 0.2812 0.1767 0.3553 0.030 Uiso 1 1 calc R . . C(B4 C 0.38405(17) 0.21529(5) 0.30159(16) 0.0260(4) Uani 1 1 d . A . H(B4 H 0.3551 0.2392 0.3160 0.031 Uiso 1 1 calc R . . C(B5 C 0.70399(15) 0.25993(4) 0.13709(14) 0.0203(3) Uani 1 1 d . A . H(B5 H 0.6920 0.2863 0.1410 0.024 Uiso 1 1 calc R . . C(B6 C 0.78681(15) 0.24286(5) 0.09850(14) 0.0205(3) Uani 1 1 d . A . H(B6 H 0.8444 0.2550 0.0707 0.025 Uiso 1 1 calc R . . C(B7 C 0.89118(14) 0.10741(5) 0.04469(14) 0.0197(3) Uani 1 1 d . A . H(B7 H 0.9510 0.1118 0.0086 0.024 Uiso 1 1 calc R . . C(B8 C 0.85205(14) 0.07333(5) 0.06896(14) 0.0192(3) Uani 1 1 d . A . H(B8 H 0.8804 0.0494 0.0543 0.023 Uiso 1 1 calc R . . C(M1 C 0.39836(14) 0.11412(4) 0.29476(13) 0.0180(3) Uani 1 1 d . A . C(M2 C 0.54476(14) 0.23671(4) 0.21928(14) 0.0181(3) Uani 1 1 d . A . C(M3 C 0.83945(14) 0.17495(4) 0.07544(13) 0.0176(3) Uani 1 1 d . A . C(M4 C 0.69433(14) 0.05179(4) 0.15579(13) 0.0175(3) Uani 1 1 d . A . C11 C 0.30321(14) 0.10178(4) 0.34448(14) 0.0176(3) Uani 1 1 d . . . C12 C 0.32906(15) 0.09513(5) 0.46370(14) 0.0210(3) Uani 1 1 d . A . H12 H 0.4079 0.0967 0.5111 0.025 Uiso 1 1 calc R . . C13 C 0.24267(15) 0.08639(5) 0.51449(14) 0.0221(3) Uani 1 1 d . . . H13 H 0.2621 0.0820 0.5961 0.027 Uiso 1 1 calc R A . C14 C 0.12704(14) 0.08408(5) 0.44600(14) 0.0203(3) Uani 1 1 d . A . C15 C 0.09919(15) 0.09013(5) 0.32693(15) 0.0219(3) Uani 1 1 d . . . H15 H 0.0204 0.0884 0.2796 0.026 Uiso 1 1 calc R A . C16 C 0.18778(15) 0.09879(5) 0.27701(14) 0.0217(3) Uani 1 1 d . A . H16 H 0.1686 0.1027 0.1952 0.026 Uiso 1 1 calc R . . O1 O 0.04737(11) 0.07545(4) 0.50391(11) 0.0284(3) Uani 1 1 d . . . C17 C -0.07048(16) 0.06947(6) 0.43572(17) 0.0297(4) Uani 1 1 d . A . H17A H -0.1025 0.0929 0.3959 0.044 Uiso 1 1 calc R . . H17B H -0.1172 0.0616 0.4866 0.044 Uiso 1 1 calc R . . H17C H -0.0729 0.0498 0.3777 0.044 Uiso 1 1 calc R . . C21 C 0.51495(14) 0.27691(4) 0.23661(14) 0.0184(3) Uani 1 1 d . . . C22 C 0.4270(2) 0.29596(5) 0.15451(16) 0.0362(5) Uani 1 1 d . A . H22 H 0.3840 0.2834 0.0854 0.043 Uiso 1 1 calc R . . C23 C 0.4011(2) 0.33303(5) 0.17213(17) 0.0379(5) Uani 1 1 d . . . H23 H 0.3404 0.3456 0.1153 0.045 Uiso 1 1 calc R A . C24 C 0.46318(15) 0.35206(4) 0.27226(15) 0.0209(3) Uani 1 1 d . A . C25 C 0.55114(15) 0.33375(5) 0.35435(15) 0.0225(3) Uani 1 1 d . . . H25 H 0.5950 0.3465 0.4229 0.027 Uiso 1 1 calc R A . C26 C 0.57496(14) 0.29619(5) 0.33530(15) 0.0222(3) Uani 1 1 d . A . H26 H 0.6349 0.2835 0.3927 0.027 Uiso 1 1 calc R . . O2 O 0.42924(11) 0.38855(3) 0.28160(11) 0.0274(3) Uani 1 1 d . . . C27 C 0.48252(17) 0.40759(5) 0.38848(16) 0.0289(4) Uani 1 1 d . A . H27A H 0.4676 0.3935 0.4531 0.043 Uiso 1 1 calc R . . H27B H 0.4496 0.4330 0.3854 0.043 Uiso 1 1 calc R . . H27C H 0.5670 0.4093 0.4004 0.043 Uiso 1 1 calc R . . C31 C 0.93539(14) 0.18751(4) 0.02760(14) 0.0190(3) Uani 1 1 d . . . C32 C 0.91281(15) 0.20575(5) -0.07982(15) 0.0222(3) Uani 1 1 d . A . H32 H 0.8345 0.2117 -0.1223 0.027 Uiso 1 1 calc R . . C33 C 1.00294(16) 0.21528(5) -0.12547(16) 0.0254(4) Uani 1 1 d . . . H33 H 0.9866 0.2279 -0.1984 0.030 Uiso 1 1 calc R A . C34 C 1.11795(16) 0.20623(5) -0.06375(17) 0.0260(4) Uani 1 1 d . A . C35 C 1.14221(16) 0.18927(5) 0.04409(17) 0.0272(4) Uani 1 1 d . . . H35 H 1.2206 0.1838 0.0873 0.033 Uiso 1 1 calc R A . C36 C 1.05098(15) 0.18027(5) 0.08897(15) 0.0237(3) Uani 1 1 d . A . H36 H 1.0681 0.1688 0.1637 0.028 Uiso 1 1 calc R . . O3 O 0.84811(13) -0.09546(3) 0.09432(11) 0.0319(3) Uani 1 1 d . . . C37 C 1.3141(2) 0.19776(6) -0.0665(3) 0.0477(6) Uani 1 1 d . A . H37A H 1.3516 0.2100 0.0085 0.071 Uiso 1 1 calc R . . H37B H 1.3629 0.2012 -0.1188 0.071 Uiso 1 1 calc R . . H37C H 1.3050 0.1708 -0.0540 0.071 Uiso 1 1 calc R . . C41 C 0.72765(14) 0.01185(4) 0.14095(14) 0.0183(3) Uani 1 1 d . . . C42 C 0.70925(15) -0.00432(5) 0.03082(14) 0.0226(3) Uani 1 1 d . A . H42 H 0.6694 0.0097 -0.0366 0.027 Uiso 1 1 calc R . . C43 C 0.74786(16) -0.04031(5) 0.01796(15) 0.0250(4) Uani 1 1 d . . . H43 H 0.7339 -0.0509 -0.0577 0.030 Uiso 1 1 calc R A . C44 C 0.80714(15) -0.06100(4) 0.11570(15) 0.0219(3) Uani 1 1 d . A . C45 C 0.82289(15) -0.04612(4) 0.22578(14) 0.0204(3) Uani 1 1 d . . . H45 H 0.8614 -0.0604 0.2931 0.025 Uiso 1 1 calc R A . C46 C 0.78186(14) -0.01004(4) 0.23727(14) 0.0192(3) Uani 1 1 d . A . H46 H 0.7913 -0.0002 0.3131 0.023 Uiso 1 1 calc R . . O4 O 1.20110(13) 0.21439(4) -0.11802(13) 0.0354(3) Uani 1 1 d . . . C47 C 0.9154(2) -0.11575(6) 0.19374(19) 0.0446(6) Uani 1 1 d . . . H47A H 0.9814 -0.1002 0.2375 0.067 Uiso 1 1 calc R . . H47B H 0.9450 -0.1390 0.1684 0.067 Uiso 1 1 calc R . . H47C H 0.8663 -0.1220 0.2438 0.067 Uiso 1 1 calc R . . N5A N 0.76467(17) 0.15478(6) 0.37829(16) 0.0224(4) Uani 0.918(2) 1 d P A 1 N6A N 0.87215(15) 0.16826(5) 0.37981(15) 0.0272(4) Uani 0.918(2) 1 d P A 1 H6A H 0.8928 0.1731 0.3166 0.033 Uiso 0.918(2) 1 calc PR A 1 C1A C 0.94267(18) 0.17329(5) 0.48864(18) 0.0286(5) Uani 0.918(2) 1 d P A 1 C2A C 0.8782(2) 0.16295(7) 0.56165(19) 0.0279(4) Uani 0.918(2) 1 d P A 1 H2A H 0.9030 0.1634 0.6445 0.034 Uiso 0.918(2) 1 calc PR A 1 C3A C 0.76900(19) 0.15167(5) 0.49006(16) 0.0233(4) Uani 0.918(2) 1 d P A 1 C4A C 1.0654(2) 0.18733(7) 0.5119(2) 0.0424(6) Uani 0.918(2) 1 d P A 1 H4A1 H 1.1138 0.1676 0.4922 0.064 Uiso 0.918(2) 1 calc PR A 1 H4A2 H 1.0968 0.1938 0.5946 0.064 Uiso 0.918(2) 1 calc PR A 1 H4A3 H 1.0659 0.2097 0.4642 0.064 Uiso 0.918(2) 1 calc PR A 1 C5A C 0.6662(2) 0.13796(6) 0.52416(19) 0.0337(5) Uani 0.918(2) 1 d P A 1 H5A1 H 0.6046 0.1572 0.5049 0.051 Uiso 0.918(2) 1 calc PR A 1 H5A2 H 0.6893 0.1330 0.6083 0.051 Uiso 0.918(2) 1 calc PR A 1 H5A3 H 0.6368 0.1147 0.4818 0.051 Uiso 0.918(2) 1 calc PR A 1 N5B N 0.7574(12) 0.1497(5) 0.3898(8) 0.023(3) Uani 0.082(2) 1 d PGU A 2 N6B N 0.7106(10) 0.1377(4) 0.4764(9) 0.020(3) Uani 0.082(2) 1 d PGU A 2 H6B H 0.6421 0.1266 0.4630 0.023 Uiso 0.082(2) 1 calc PR A 2 C1B C 0.7825(10) 0.1448(3) 0.5838(8) 0.022(2) Uani 0.082(2) 1 d PGU A 2 C2B C 0.8810(11) 0.1616(5) 0.5688(9) 0.0279(4) Uani 0.082(2) 1 d PGU A 2 H2B H 0.9481 0.1698 0.6281 0.034 Uiso 0.082(2) 1 calc PR A 2 C3B C 0.8614(11) 0.1642(3) 0.4465(10) 0.026(2) Uani 0.082(2) 1 d PGU A 2 C4B C 0.7490(15) 0.1346(5) 0.6919(10) 0.030(4) Uani 0.082(2) 1 d PGU A 2 H4B1 H 0.6682 0.1424 0.6826 0.045 Uiso 0.082(2) 1 calc PR A 2 H4B2 H 0.8013 0.1474 0.7596 0.045 Uiso 0.082(2) 1 calc PR A 2 H4B3 H 0.7558 0.1072 0.7039 0.045 Uiso 0.082(2) 1 calc PR A 2 C5B C 0.9400(15) 0.1797(5) 0.3829(14) 0.032(4) Uani 0.082(2) 1 d PGU A 2 H5B1 H 0.9378 0.1635 0.3160 0.049 Uiso 0.082(2) 1 calc PR A 2 H5B2 H 1.0201 0.1807 0.4352 0.049 Uiso 0.082(2) 1 calc PR A 2 H5B3 H 0.9143 0.2051 0.3552 0.049 Uiso 0.082(2) 1 calc PR A 2 C1S C 0.18843(16) -0.02218(5) 0.26071(16) 0.0276(4) Uani 1 1 d . . . C2S C 0.20865(18) -0.00695(5) 0.37103(17) 0.0295(4) Uani 1 1 d . . . H2SA H 0.1510 0.0087 0.3874 0.035 Uiso 1 1 calc R . . C3S C 0.31099(19) -0.01413(5) 0.45757(17) 0.0315(4) Uani 1 1 d . . . H3S H 0.3229 -0.0035 0.5329 0.038 Uiso 1 1 calc R . . C4S C 0.39618(18) -0.03659(5) 0.43576(16) 0.0308(4) Uani 1 1 d . . . H4S H 0.4673 -0.0411 0.4952 0.037 Uiso 1 1 calc R . . C5S C 0.37736(18) -0.05249(5) 0.32677(17) 0.0302(4) Uani 1 1 d . . . H5S H 0.4354 -0.0682 0.3111 0.036 Uiso 1 1 calc R . . C6S C 0.27389(17) -0.04561(5) 0.24029(16) 0.0291(4) Uani 1 1 d . . . H6S H 0.2610 -0.0570 0.1659 0.035 Uiso 1 1 calc R . . C7S C 0.07959(18) -0.01277(7) 0.16492(19) 0.0385(5) Uani 1 1 d . . . H7S1 H 0.0225 -0.0010 0.1984 0.058 Uiso 1 1 calc R . . H7S2 H 0.0463 -0.0359 0.1238 0.058 Uiso 1 1 calc R . . H7S3 H 0.0989 0.0047 0.1100 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 0.01845(13) 0.01198(11) 0.01817(11) 0.00051(8) 0.00539(8) 0.00008(8) N1 0.0200(7) 0.0138(6) 0.0197(6) 0.0005(5) 0.0064(5) -0.0002(5) N2 0.0238(7) 0.0131(6) 0.0232(7) 0.0011(5) 0.0097(5) 0.0000(5) N3 0.0176(7) 0.0160(6) 0.0182(6) 0.0006(5) 0.0048(5) 0.0001(5) N4 0.0183(7) 0.0151(6) 0.0197(6) 0.0012(5) 0.0046(5) -0.0002(5) C(A1 0.0199(8) 0.0134(7) 0.0181(7) 0.0001(5) 0.0035(6) -0.0008(6) C(A2 0.0193(8) 0.0161(7) 0.0166(7) 0.0016(5) 0.0034(6) -0.0012(6) C(A3 0.0220(8) 0.0165(7) 0.0225(8) 0.0008(6) 0.0095(6) -0.0001(6) C(A4 0.0261(9) 0.0163(7) 0.0242(8) -0.0008(6) 0.0109(7) 0.0004(6) C(A5 0.0189(8) 0.0138(7) 0.0173(7) 0.0002(5) 0.0036(6) -0.0011(6) C(A6 0.0174(8) 0.0158(7) 0.0179(7) 0.0015(6) 0.0029(6) -0.0018(6) C(A7 0.0173(8) 0.0186(7) 0.0163(7) 0.0009(6) 0.0034(6) 0.0001(6) C(A8 0.0182(8) 0.0156(7) 0.0170(7) 0.0005(5) 0.0026(6) 0.0020(6) C(B1 0.0219(8) 0.0142(7) 0.0224(8) 0.0008(6) 0.0036(6) -0.0017(6) C(B2 0.0201(8) 0.0160(7) 0.0186(7) 0.0011(6) 0.0033(6) -0.0025(6) C(B3 0.0291(10) 0.0189(8) 0.0313(9) 0.0005(7) 0.0173(7) 0.0010(7) C(B4 0.0328(10) 0.0171(8) 0.0336(9) 0.0001(7) 0.0184(8) 0.0015(7) C(B5 0.0222(8) 0.0146(7) 0.0240(8) 0.0002(6) 0.0066(6) -0.0030(6) C(B6 0.0205(8) 0.0175(7) 0.0225(8) 0.0001(6) 0.0049(6) -0.0033(6) C(B7 0.0192(8) 0.0201(7) 0.0191(7) -0.0001(6) 0.0047(6) 0.0020(6) C(B8 0.0189(8) 0.0189(7) 0.0192(7) -0.0008(6) 0.0046(6) 0.0027(6) C(M1 0.0199(8) 0.0159(7) 0.0181(7) 0.0017(6) 0.0057(6) -0.0009(6) C(M2 0.0218(8) 0.0136(7) 0.0189(7) -0.0009(5) 0.0059(6) 0.0004(6) C(M3 0.0160(8) 0.0188(7) 0.0170(7) 0.0019(6) 0.0030(6) -0.0010(6) C(M4 0.0201(8) 0.0141(7) 0.0164(7) 0.0002(5) 0.0023(6) 0.0015(6) C11 0.0195(8) 0.0121(7) 0.0224(8) 0.0004(6) 0.0078(6) -0.0002(6) C12 0.0166(8) 0.0226(8) 0.0219(8) 0.0013(6) 0.0028(6) -0.0023(6) C13 0.0214(9) 0.0255(8) 0.0178(7) 0.0014(6) 0.0033(6) -0.0041(6) C14 0.0182(8) 0.0179(7) 0.0252(8) 0.0015(6) 0.0071(6) -0.0027(6) C15 0.0168(8) 0.0227(8) 0.0237(8) 0.0018(6) 0.0019(6) -0.0025(6) C16 0.0240(9) 0.0205(8) 0.0189(7) 0.0023(6) 0.0037(6) -0.0002(6) O1 0.0182(6) 0.0418(8) 0.0252(6) 0.0045(5) 0.0065(5) -0.0078(5) C17 0.0166(9) 0.0333(10) 0.0371(10) 0.0032(8) 0.0046(7) -0.0058(7) C21 0.0216(8) 0.0134(7) 0.0220(8) 0.0000(6) 0.0093(6) -0.0002(6) C22 0.0577(14) 0.0170(8) 0.0218(9) -0.0017(7) -0.0074(8) 0.0048(8) C23 0.0528(13) 0.0179(8) 0.0280(10) 0.0003(7) -0.0117(9) 0.0089(8) C24 0.0240(9) 0.0132(7) 0.0248(8) -0.0001(6) 0.0061(6) 0.0004(6) C25 0.0185(8) 0.0200(8) 0.0263(8) -0.0074(6) 0.0021(6) -0.0001(6) C26 0.0160(8) 0.0192(8) 0.0281(9) -0.0031(6) 0.0009(6) 0.0033(6) O2 0.0314(7) 0.0142(5) 0.0304(7) -0.0030(5) -0.0010(5) 0.0043(5) C27 0.0337(10) 0.0190(8) 0.0306(9) -0.0065(7) 0.0039(7) 0.0022(7) C31 0.0188(8) 0.0163(7) 0.0224(8) -0.0005(6) 0.0066(6) -0.0005(6) C32 0.0218(9) 0.0201(8) 0.0245(8) 0.0028(6) 0.0065(6) 0.0018(6) C33 0.0326(10) 0.0198(8) 0.0276(9) 0.0050(6) 0.0148(7) 0.0024(7) C34 0.0287(10) 0.0174(8) 0.0381(10) -0.0032(7) 0.0194(8) -0.0025(7) C35 0.0188(9) 0.0290(9) 0.0342(10) 0.0001(7) 0.0082(7) 0.0002(7) C36 0.0200(9) 0.0264(8) 0.0238(8) 0.0027(7) 0.0051(6) -0.0008(7) O3 0.0440(8) 0.0172(6) 0.0296(7) -0.0020(5) 0.0030(6) 0.0108(5) C37 0.0395(13) 0.0344(11) 0.0855(18) 0.0172(11) 0.0440(13) 0.0099(9) C41 0.0183(8) 0.0149(7) 0.0220(8) 0.0000(6) 0.0064(6) -0.0003(6) C42 0.0273(9) 0.0172(7) 0.0198(8) 0.0018(6) 0.0016(6) 0.0024(6) C43 0.0316(10) 0.0197(8) 0.0210(8) -0.0034(6) 0.0034(7) 0.0027(7) C44 0.0234(9) 0.0133(7) 0.0274(8) -0.0007(6) 0.0050(7) 0.0016(6) C45 0.0218(8) 0.0167(7) 0.0217(8) 0.0040(6) 0.0046(6) 0.0011(6) C46 0.0207(8) 0.0180(7) 0.0194(7) 0.0001(6) 0.0065(6) 0.0001(6) O4 0.0356(8) 0.0289(7) 0.0530(9) 0.0085(6) 0.0306(7) 0.0033(6) C47 0.0648(16) 0.0220(9) 0.0386(11) 0.0004(8) 0.0020(10) 0.0203(10) N5A 0.0219(9) 0.0200(9) 0.0239(8) 0.0019(7) 0.0045(7) -0.0009(7) N6A 0.0217(9) 0.0296(9) 0.0279(9) 0.0031(7) 0.0033(7) -0.0041(7) C1A 0.0244(11) 0.0205(9) 0.0335(11) -0.0002(8) -0.0031(8) 0.0025(7) C2A 0.0322(10) 0.0200(8) 0.0249(9) -0.0014(7) -0.0022(7) 0.0042(7) C3A 0.0297(11) 0.0168(8) 0.0212(9) -0.0001(7) 0.0039(7) 0.0036(7) C4A 0.0260(12) 0.0392(13) 0.0517(15) 0.0022(10) -0.0050(10) -0.0052(9) C5A 0.0401(13) 0.0365(11) 0.0254(10) -0.0002(8) 0.0107(9) -0.0077(9) N5B 0.022(5) 0.020(5) 0.026(5) 0.001(4) 0.004(4) 0.005(4) N6B 0.020(5) 0.018(4) 0.022(4) 0.003(4) 0.009(4) 0.005(4) C1B 0.026(4) 0.019(4) 0.021(4) -0.001(3) 0.004(3) 0.007(3) C2B 0.0322(10) 0.0200(8) 0.0249(9) -0.0014(7) -0.0022(7) 0.0042(7) C3B 0.029(4) 0.020(4) 0.025(4) 0.000(4) 0.000(4) 0.005(4) C4B 0.035(8) 0.028(7) 0.022(7) -0.003(6) 0.002(6) 0.004(7) C5B 0.034(8) 0.027(7) 0.028(7) -0.004(7) -0.004(7) -0.010(7) C1S 0.0265(10) 0.0285(9) 0.0292(9) 0.0035(7) 0.0104(7) -0.0039(7) C2S 0.0358(11) 0.0229(8) 0.0348(10) 0.0005(7) 0.0180(8) -0.0014(7) C3S 0.0452(12) 0.0253(9) 0.0251(9) -0.0007(7) 0.0121(8) -0.0025(8) C4S 0.0364(11) 0.0256(9) 0.0265(9) 0.0038(7) 0.0031(8) -0.0013(8) C5S 0.0337(11) 0.0272(9) 0.0289(9) 0.0034(7) 0.0078(8) 0.0055(8) C6S 0.0319(10) 0.0310(9) 0.0242(9) -0.0009(7) 0.0077(7) 0.0006(8) C7S 0.0261(10) 0.0511(13) 0.0389(11) 0.0023(9) 0.0102(8) 0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.0548(14) . ? Fe1 N1 2.0704(13) . ? Fe1 N4 2.0724(14) . ? Fe1 N3 2.0755(13) . ? Fe1 N5A 2.1412(18) . ? Fe1 N5B 2.186(10) . ? N1 C(A2 1.370(2) . ? N1 C(A1 1.374(2) . ? N2 C(A3 1.373(2) . ? N2 C(A4 1.376(2) . ? N3 C(A5 1.371(2) . ? N3 C(A6 1.373(2) . ? N4 C(A8 1.3745(19) . ? N4 C(A7 1.379(2) . ? C(A1 C(M4 1.395(2) . ? C(A1 C(B1 1.449(2) . ? C(A2 C(M1 1.398(2) . ? C(A2 C(B2 1.447(2) . ? C(A3 C(M1 1.404(2) . ? C(A3 C(B3 1.440(2) . ? C(A4 C(M2 1.401(2) . ? C(A4 C(B4 1.435(2) . ? C(A5 C(M2 1.403(2) . ? C(A5 C(B5 1.445(2) . ? C(A6 C(M3 1.404(2) . ? C(A6 C(B6 1.445(2) . ? C(A7 C(M3 1.412(2) . ? C(A7 C(B7 1.442(2) . ? C(A8 C(M4 1.413(2) . ? C(A8 C(B8 1.437(2) . ? C(B1 C(B2 1.352(2) . ? C(B1 H(B1 0.9500 . ? C(B2 H(B2 0.9500 . ? C(B3 C(B4 1.354(2) . ? C(B3 H(B3 0.9500 . ? C(B4 H(B4 0.9500 . ? C(B5 C(B6 1.352(2) . ? C(B5 H(B5 0.9500 . ? C(B6 H(B6 0.9500 . ? C(B7 C(B8 1.358(2) . ? C(B7 H(B7 0.9500 . ? C(B8 H(B8 0.9500 . ? C(M1 C11 1.496(2) . ? C(M2 C21 1.499(2) . ? C(M3 C31 1.492(2) . ? C(M4 C41 1.497(2) . ? C11 C16 1.386(2) . ? C11 C12 1.391(2) . ? C12 C13 1.379(2) . ? C12 H12 0.9500 . ? C13 C14 1.390(2) . ? C13 H13 0.9500 . ? C14 O1 1.367(2) . ? C14 C15 1.384(2) . ? C15 C16 1.394(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? O1 C17 1.424(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C26 1.374(2) . ? C21 C22 1.389(2) . ? C22 C23 1.381(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(2) . ? C23 H23 0.9500 . ? C24 O2 1.3714(19) . ? C24 C25 1.376(2) . ? C25 C26 1.396(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O2 C27 1.424(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C36 1.387(2) . ? C31 C32 1.395(2) . ? C32 C33 1.385(2) . ? C32 H32 0.9500 . ? C33 C34 1.396(3) . ? C33 H33 0.9500 . ? C34 O4 1.368(2) . ? C34 C35 1.378(3) . ? C35 C36 1.387(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O3 C44 1.3693(19) . ? O3 C47 1.424(2) . ? C37 O4 1.439(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C46 1.386(2) . ? C41 C42 1.397(2) . ? C42 C43 1.382(2) . ? C42 H42 0.9500 . ? C43 C44 1.389(2) . ? C43 H43 0.9500 . ? C44 C45 1.382(2) . ? C45 C46 1.392(2) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? N5A C3A 1.330(3) . ? N5A N6A 1.367(3) . ? N6A C1A 1.343(3) . ? N6A H6A 0.8800 . ? C1A C2A 1.374(3) . ? C1A C4A 1.497(3) . ? C2A C3A 1.396(3) . ? C2A H2A 0.9500 . ? C3A C5A 1.486(3) . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? N5B C3B 1.3337 . ? N5B N6B 1.3831 . ? N6B C1B 1.3473 . ? N6B H6B 0.8800 . ? C1B C2B 1.3765 . ? C1B C4B 1.5090 . ? C2B C3B 1.4181 . ? C2B H2B 0.9500 . ? C3B C5B 1.4788 . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C4B H4B3 0.9800 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C1S C2S 1.383(3) . ? C1S C6S 1.393(3) . ? C1S C7S 1.501(3) . ? C2S C3S 1.378(3) . ? C2S H2SA 0.9500 . ? C3S C4S 1.377(3) . ? C3S H3S 0.9500 . ? C4S C5S 1.380(3) . ? C4S H4S 0.9500 . ? C5S C6S 1.385(3) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 89.24(5) . . ? N2 Fe1 N4 162.24(5) . . ? N1 Fe1 N4 88.30(5) . . ? N2 Fe1 N3 88.67(5) . . ? N1 Fe1 N3 163.03(5) . . ? N4 Fe1 N3 88.58(5) . . ? N2 Fe1 N5A 99.31(7) . . ? N1 Fe1 N5A 106.87(6) . . ? N4 Fe1 N5A 98.23(7) . . ? N3 Fe1 N5A 90.09(6) . . ? N2 Fe1 N5B 97.7(4) . . ? N1 Fe1 N5B 100.4(4) . . ? N4 Fe1 N5B 100.1(4) . . ? N3 Fe1 N5B 96.5(4) . . ? N5A Fe1 N5B 6.7(4) . . ? C(A2 N1 C(A1 106.53(13) . . ? C(A2 N1 Fe1 126.18(10) . . ? C(A1 N1 Fe1 127.22(11) . . ? C(A3 N2 C(A4 106.39(13) . . ? C(A3 N2 Fe1 125.89(11) . . ? C(A4 N2 Fe1 126.32(11) . . ? C(A5 N3 C(A6 106.54(13) . . ? C(A5 N3 Fe1 125.65(11) . . ? C(A6 N3 Fe1 126.52(10) . . ? C(A8 N4 C(A7 106.61(13) . . ? C(A8 N4 Fe1 126.80(11) . . ? C(A7 N4 Fe1 126.29(10) . . ? N1 C(A1 C(M4 125.70(14) . . ? N1 C(A1 C(B1 109.49(14) . . ? C(M4 C(A1 C(B1 124.76(14) . . ? N1 C(A2 C(M1 125.67(14) . . ? N1 C(A2 C(B2 109.95(14) . . ? C(M1 C(A2 C(B2 124.38(15) . . ? N2 C(A3 C(M1 125.70(15) . . ? N2 C(A3 C(B3 109.72(14) . . ? C(M1 C(A3 C(B3 124.58(15) . . ? N2 C(A4 C(M2 125.04(15) . . ? N2 C(A4 C(B4 109.63(14) . . ? C(M2 C(A4 C(B4 125.33(15) . . ? N3 C(A5 C(M2 125.55(14) . . ? N3 C(A5 C(B5 109.65(14) . . ? C(M2 C(A5 C(B5 124.79(14) . . ? N3 C(A6 C(M3 125.40(14) . . ? N3 C(A6 C(B6 109.72(14) . . ? C(M3 C(A6 C(B6 124.88(15) . . ? N4 C(A7 C(M3 125.79(14) . . ? N4 C(A7 C(B7 109.43(14) . . ? C(M3 C(A7 C(B7 124.78(15) . . ? N4 C(A8 C(M4 125.68(15) . . ? N4 C(A8 C(B8 109.63(14) . . ? C(M4 C(A8 C(B8 124.68(14) . . ? C(B2 C(B1 C(A1 107.22(14) . . ? C(B2 C(B1 H(B1 126.4 . . ? C(A1 C(B1 H(B1 126.4 . . ? C(B1 C(B2 C(A2 106.81(14) . . ? C(B1 C(B2 H(B2 126.6 . . ? C(A2 C(B2 H(B2 126.6 . . ? C(B4 C(B3 C(A3 106.94(15) . . ? C(B4 C(B3 H(B3 126.5 . . ? C(A3 C(B3 H(B3 126.5 . . ? C(B3 C(B4 C(A4 107.32(15) . . ? C(B3 C(B4 H(B4 126.3 . . ? C(A4 C(B4 H(B4 126.3 . . ? C(B6 C(B5 C(A5 107.16(14) . . ? C(B6 C(B5 H(B5 126.4 . . ? C(A5 C(B5 H(B5 126.4 . . ? C(B5 C(B6 C(A6 106.93(14) . . ? C(B5 C(B6 H(B6 126.5 . . ? C(A6 C(B6 H(B6 126.5 . . ? C(B8 C(B7 C(A7 106.99(14) . . ? C(B8 C(B7 H(B7 126.5 . . ? C(A7 C(B7 H(B7 126.5 . . ? C(B7 C(B8 C(A8 107.32(14) . . ? C(B7 C(B8 H(B8 126.3 . . ? C(A8 C(B8 H(B8 126.3 . . ? C(A2 C(M1 C(A3 125.55(15) . . ? C(A2 C(M1 C11 118.29(14) . . ? C(A3 C(M1 C11 116.13(14) . . ? C(A4 C(M2 C(A5 125.76(14) . . ? C(A4 C(M2 C21 117.32(14) . . ? C(A5 C(M2 C21 116.92(14) . . ? C(A6 C(M3 C(A7 125.27(15) . . ? C(A6 C(M3 C31 118.06(14) . . ? C(A7 C(M3 C31 116.67(14) . . ? C(A1 C(M4 C(A8 125.06(14) . . ? C(A1 C(M4 C41 118.13(14) . . ? C(A8 C(M4 C41 116.80(14) . . ? C16 C11 C12 118.15(15) . . ? C16 C11 C(M1 122.28(14) . . ? C12 C11 C(M1 119.46(15) . . ? C13 C12 C11 121.39(15) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 119.81(15) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? O1 C14 C15 124.36(15) . . ? O1 C14 C13 115.73(15) . . ? C15 C14 C13 119.92(15) . . ? C14 C15 C16 119.47(15) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 121.25(15) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C14 O1 C17 117.49(14) . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C21 C22 117.73(15) . . ? C26 C21 C(M2 120.49(15) . . ? C22 C21 C(M2 121.78(15) . . ? C23 C22 C21 120.82(17) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.55(17) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? O2 C24 C25 124.77(15) . . ? O2 C24 C23 115.69(15) . . ? C25 C24 C23 119.54(15) . . ? C24 C25 C26 118.94(15) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 122.42(15) . . ? C21 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C24 O2 C27 117.12(13) . . ? O2 C27 H27A 109.5 . . ? O2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C36 C31 C32 118.04(15) . . ? C36 C31 C(M3 119.98(14) . . ? C32 C31 C(M3 121.96(15) . . ? C33 C32 C31 120.94(16) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.62(16) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? O4 C34 C35 123.70(17) . . ? O4 C34 C33 116.08(17) . . ? C35 C34 C33 120.21(16) . . ? C34 C35 C36 119.35(17) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C35 C36 C31 121.77(16) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? C44 O3 C47 116.16(14) . . ? O4 C37 H37A 109.5 . . ? O4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C46 C41 C42 117.62(14) . . ? C46 C41 C(M4 120.52(14) . . ? C42 C41 C(M4 121.82(14) . . ? C43 C42 C41 121.29(15) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 119.96(16) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? O3 C44 C45 124.28(15) . . ? O3 C44 C43 115.89(15) . . ? C45 C44 C43 119.82(15) . . ? C44 C45 C46 119.46(15) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 121.73(15) . . ? C41 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C34 O4 C37 115.54(15) . . ? O3 C47 H47A 109.5 . . ? O3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C3A N5A N6A 104.79(18) . . ? C3A N5A Fe1 136.26(16) . . ? N6A N5A Fe1 118.95(14) . . ? C1A N6A N5A 112.43(18) . . ? C1A N6A H6A 123.8 . . ? N5A N6A H6A 123.8 . . ? N6A C1A C2A 105.84(18) . . ? N6A C1A C4A 122.0(2) . . ? C2A C1A C4A 132.2(2) . . ? C1A C2A C3A 106.45(19) . . ? C1A C2A H2A 126.8 . . ? C3A C2A H2A 126.8 . . ? N5A C3A C2A 110.5(2) . . ? N5A C3A C5A 120.78(19) . . ? C2A C3A C5A 128.73(19) . . ? C3B N5B N6B 104.9 . . ? C3B N5B Fe1 140.8(6) . . ? N6B N5B Fe1 113.8(6) . . ? C1B N6B N5B 111.9 . . ? C1B N6B H6B 124.0 . . ? N5B N6B H6B 124.0 . . ? N6B C1B C2B 106.8 . . ? N6B C1B C4B 121.3 . . ? C2B C1B C4B 131.9 . . ? C1B C2B C3B 105.8 . . ? C1B C2B H2B 127.1 . . ? C3B C2B H2B 127.1 . . ? N5B C3B C2B 110.5 . . ? N5B C3B C5B 121.3 . . ? C2B C3B C5B 128.2 . . ? C1B C4B H4B1 109.5 . . ? C1B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C1B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C3B C5B H5B1 109.5 . . ? C3B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C3B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? C2S C1S C6S 117.93(18) . . ? C2S C1S C7S 121.02(18) . . ? C6S C1S C7S 121.02(17) . . ? C3S C2S C1S 121.12(18) . . ? C3S C2S H2SA 119.4 . . ? C1S C2S H2SA 119.4 . . ? C4S C3S C2S 120.53(18) . . ? C4S C3S H3S 119.7 . . ? C2S C3S H3S 119.7 . . ? C3S C4S C5S 119.40(18) . . ? C3S C4S H4S 120.3 . . ? C5S C4S H4S 120.3 . . ? C4S C5S C6S 120.00(18) . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.99(18) . . ? C5S C6S H6S 119.5 . . ? C1S C6S H6S 119.5 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.625 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.056