data_708764 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H42 Fe N12, C24 H20 B, Br' _chemical_formula_sum 'C48 H62 B Br Fe N12' _chemical_formula_weight 953.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Br' 'Br' -0.2901 2.4595 '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 9.4246(4) _cell_length_b 31.7843(13) _cell_length_c 16.3078(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4885.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9077 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 26.90 _exptl_crystal_description 'needle' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6564 _exptl_absorpt_correction_T_max 0.8053 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61136 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.2586 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 33.48 _reflns_number_total 17521 _reflns_number_gt 5256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17521 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2259 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.62317(5) 0.343518(13) 0.20228(3) 0.03326(12) Uani 1 1 d . . . N1 N 0.6931(3) 0.40393(8) 0.20268(18) 0.0391(6) Uani 1 1 d . . . N2 N 0.6224(3) 0.47407(9) 0.1876(2) 0.0571(9) Uani 1 1 d . . . H2A H 0.5584 0.4910 0.1695 0.069 Uiso 1 1 calc R . . N3 N 0.3665(3) 0.44145(9) 0.1232(2) 0.0590(9) Uani 1 1 d . . . H3A H 0.3867 0.4675 0.1153 0.071 Uiso 1 1 calc R . . N4 N 0.4489(3) 0.37532(9) 0.16361(19) 0.0448(7) Uani 1 1 d . . . N5 N 0.5535(3) 0.34513(8) 0.32205(18) 0.0407(6) Uani 1 1 d . . . N6 N 0.3968(5) 0.31206(11) 0.4118(2) 0.0909(14) Uani 1 1 d . . . H6A H 0.3514 0.2891 0.4218 0.109 Uiso 1 1 calc R . . N7 N 0.4197(4) 0.24083(9) 0.3092(2) 0.0619(9) Uani 1 1 d . . . H7A H 0.3836 0.2384 0.3574 0.074 Uiso 1 1 calc R . . N8 N 0.5311(3) 0.28578(8) 0.21424(18) 0.0428(7) Uani 1 1 d . . . N9 N 0.8146(3) 0.31776(8) 0.22585(18) 0.0438(7) Uani 1 1 d . . . N10 N 1.0165(3) 0.28643(10) 0.1666(2) 0.0605(9) Uani 1 1 d . . . H10A H 1.0593 0.2800 0.1218 0.073 Uiso 1 1 calc R . . N11 N 0.8958(4) 0.30742(15) 0.0134(2) 0.0931(14) Uani 1 1 d . . . H11A H 0.9787 0.2962 0.0156 0.112 Uiso 1 1 calc R . . N12 N 0.6995(3) 0.33220(8) 0.08758(17) 0.0415(7) Uani 1 1 d . . . B1 B 0.7143(4) 0.05349(12) 0.1956(2) 0.0419(9) Uani 1 1 d . . . Br1 Br 0.77921(5) 0.731224(16) 0.00983(3) 0.07890(18) Uani 1 1 d . . . C1 C 0.8333(4) 0.41777(12) 0.2300(3) 0.0621(11) Uani 1 1 d . . . H1A H 0.9035 0.3984 0.2083 0.074 Uiso 1 1 calc R . . H1B H 0.8367 0.4158 0.2893 0.074 Uiso 1 1 calc R . . C2 C 0.8736(5) 0.46067(14) 0.2061(3) 0.0725(13) Uani 1 1 d . . . H2B H 0.8960 0.4613 0.1480 0.087 Uiso 1 1 calc R . . H2C H 0.9578 0.4691 0.2361 0.087 Uiso 1 1 calc R . . C3 C 0.7565(4) 0.49081(14) 0.2234(4) 0.0867(17) Uani 1 1 d . . . H3B H 0.7783 0.5180 0.1995 0.104 Uiso 1 1 calc R . . H3C H 0.7458 0.4944 0.2821 0.104 Uiso 1 1 calc R . . C4 C 0.6027(3) 0.43191(10) 0.1838(2) 0.0397(8) Uani 1 1 d . . . C5 C 0.4638(3) 0.41544(10) 0.1555(2) 0.0399(8) Uani 1 1 d . . . C6 C 0.2274(5) 0.42557(16) 0.1016(4) 0.0981(19) Uani 1 1 d . . . H6B H 0.1588 0.4357 0.1413 0.118 Uiso 1 1 calc R . . H6C H 0.2009 0.4366 0.0483 0.118 Uiso 1 1 calc R . . C7 C 0.2220(7) 0.38168(18) 0.0993(8) 0.253(7) Uani 1 1 d . . . H7B H 0.1272 0.3740 0.1171 0.304 Uiso 1 1 calc R . . H7C H 0.2283 0.3739 0.0419 0.304 Uiso 1 1 calc R . . C8 C 0.3135(4) 0.35544(13) 0.1404(3) 0.0644(12) Uani 1 1 d . . . H8A H 0.3334 0.3312 0.1061 0.077 Uiso 1 1 calc R . . H8B H 0.2669 0.3453 0.1897 0.077 Uiso 1 1 calc R . . C9 C 0.5642(4) 0.38080(12) 0.3802(2) 0.0588(11) Uani 1 1 d . . . H9A H 0.6622 0.3900 0.3826 0.071 Uiso 1 1 calc R . . H9B H 0.5082 0.4041 0.3593 0.071 Uiso 1 1 calc R . . C10 C 0.5166(6) 0.37104(17) 0.4628(3) 0.0919(17) Uani 1 1 d . . . H10B H 0.5057 0.3973 0.4926 0.110 Uiso 1 1 calc R . . H10C H 0.5906 0.3550 0.4899 0.110 Uiso 1 1 calc R . . C11 C 0.3818(7) 0.34710(15) 0.4695(3) 0.098(2) Uani 1 1 d . . . H11B H 0.3684 0.3368 0.5250 0.117 Uiso 1 1 calc R . . H11C H 0.3016 0.3647 0.4549 0.117 Uiso 1 1 calc R . . C12 C 0.4762(4) 0.31387(11) 0.3454(2) 0.0463(9) Uani 1 1 d . . . C13 C 0.4740(4) 0.27789(9) 0.2854(2) 0.0418(8) Uani 1 1 d . . . C14 C 0.4212(5) 0.20425(12) 0.2537(3) 0.0777(14) Uani 1 1 d . . . H14A H 0.4372 0.1788 0.2853 0.093 Uiso 1 1 calc R . . H14B H 0.3298 0.2018 0.2268 0.093 Uiso 1 1 calc R . . C15 C 0.5329(7) 0.20862(14) 0.1918(4) 0.105(2) Uani 1 1 d . . . H15A H 0.6234 0.2019 0.2169 0.126 Uiso 1 1 calc R . . H15B H 0.5160 0.1882 0.1486 0.126 Uiso 1 1 calc R . . C16 C 0.5424(5) 0.25051(11) 0.1550(2) 0.0587(10) Uani 1 1 d . . . H16A H 0.4675 0.2534 0.1146 0.070 Uiso 1 1 calc R . . H16B H 0.6323 0.2528 0.1264 0.070 Uiso 1 1 calc R . . C17 C 0.8692(4) 0.30923(14) 0.3080(2) 0.0616(11) Uani 1 1 d . . . H17A H 0.8268 0.2834 0.3281 0.074 Uiso 1 1 calc R . . H17B H 0.8401 0.3318 0.3443 0.074 Uiso 1 1 calc R . . C18 C 1.0286(6) 0.3051(2) 0.3114(4) 0.1065(19) Uani 1 1 d . . . H18A H 1.0565 0.2943 0.3647 0.128 Uiso 1 1 calc R . . H18B H 1.0718 0.3325 0.3044 0.128 Uiso 1 1 calc R . . C19 C 1.0805(5) 0.27573(13) 0.2450(3) 0.0690(12) Uani 1 1 d . . . H19A H 1.1829 0.2777 0.2407 0.083 Uiso 1 1 calc R . . H19B H 1.0564 0.2470 0.2592 0.083 Uiso 1 1 calc R . . C20 C 0.8898(3) 0.30647(10) 0.1637(2) 0.0395(8) Uani 1 1 d . . . C21 C 0.8252(4) 0.31624(10) 0.0837(2) 0.0443(8) Uani 1 1 d . . . C22 C 0.8320(7) 0.3169(3) -0.0665(3) 0.148(3) Uani 1 1 d . . . H22A H 0.8913 0.3374 -0.0941 0.178 Uiso 1 1 calc R . . H22B H 0.8332 0.2914 -0.0993 0.178 Uiso 1 1 calc R . . C23 C 0.7027(7) 0.3312(3) -0.0650(4) 0.159(4) Uani 1 1 d . . . H23A H 0.6448 0.3108 -0.0941 0.190 Uiso 1 1 calc R . . H23B H 0.7024 0.3566 -0.0979 0.190 Uiso 1 1 calc R . . C24 C 0.6265(5) 0.34132(14) 0.0111(3) 0.0644(11) Uani 1 1 d . . . H24A H 0.6037 0.3711 0.0104 0.077 Uiso 1 1 calc R . . H24B H 0.5375 0.3260 0.0110 0.077 Uiso 1 1 calc R . . C25 C 0.8022(4) 0.09513(10) 0.1661(2) 0.0483(9) Uani 1 1 d . . . C26 C 0.8656(6) 0.12331(13) 0.2166(3) 0.0779(14) Uani 1 1 d . . . H26A H 0.8617 0.1198 0.2731 0.093 Uiso 1 1 calc R . . C27 C 0.9401(8) 0.15915(17) 0.1814(5) 0.126(3) Uani 1 1 d . . . H27A H 0.9839 0.1782 0.2164 0.152 Uiso 1 1 calc R . . C28 C 0.9476(7) 0.16555(17) 0.1018(5) 0.106(2) Uani 1 1 d . . . H28A H 0.9960 0.1887 0.0808 0.127 Uiso 1 1 calc R . . C29 C 0.8853(6) 0.13860(15) 0.0528(4) 0.0797(15) Uani 1 1 d . . . H29A H 0.8880 0.1432 -0.0035 0.096 Uiso 1 1 calc R . . C30 C 0.8173(4) 0.10429(12) 0.0821(3) 0.0576(10) Uani 1 1 d . . . H30A H 0.7782 0.0856 0.0445 0.069 Uiso 1 1 calc R . . C31 C 0.5526(4) 0.05775(10) 0.1604(2) 0.0407(8) Uani 1 1 d . . . C32 C 0.4873(4) 0.03092(12) 0.1053(2) 0.0513(9) Uani 1 1 d . . . H32A H 0.5368 0.0076 0.0863 0.062 Uiso 1 1 calc R . . C33 C 0.3517(5) 0.03779(14) 0.0778(3) 0.0650(11) Uani 1 1 d . . . H33A H 0.3120 0.0187 0.0412 0.078 Uiso 1 1 calc R . . C34 C 0.2739(4) 0.07107(15) 0.1019(3) 0.0662(12) Uani 1 1 d . . . H34A H 0.1823 0.0750 0.0821 0.079 Uiso 1 1 calc R . . C35 C 0.3303(5) 0.09813(13) 0.1542(3) 0.0664(12) Uani 1 1 d . . . H35A H 0.2780 0.1212 0.1720 0.080 Uiso 1 1 calc R . . C36 C 0.4675(4) 0.09202(11) 0.1826(3) 0.0522(9) Uani 1 1 d . . . H36A H 0.5052 0.1119 0.2185 0.063 Uiso 1 1 calc R . . C37 C 0.7154(4) 0.04989(10) 0.2960(2) 0.0438(8) Uani 1 1 d . . . C38 C 0.8433(5) 0.04188(13) 0.3362(3) 0.0663(12) Uani 1 1 d . . . H38A H 0.9263 0.0401 0.3056 0.080 Uiso 1 1 calc R . . C39 C 0.8503(7) 0.03647(15) 0.4222(3) 0.0866(16) Uani 1 1 d . . . H39A H 0.9369 0.0309 0.4473 0.104 Uiso 1 1 calc R . . C40 C 0.7269(8) 0.03947(16) 0.4692(3) 0.099(2) Uani 1 1 d . . . H40A H 0.7310 0.0357 0.5257 0.119 Uiso 1 1 calc R . . C41 C 0.6028(7) 0.04776(14) 0.4328(3) 0.0820(15) Uani 1 1 d . . . H41A H 0.5205 0.0501 0.4640 0.098 Uiso 1 1 calc R . . C42 C 0.5973(5) 0.05283(11) 0.3473(2) 0.0542(10) Uani 1 1 d . . . H42A H 0.5097 0.0585 0.3235 0.065 Uiso 1 1 calc R . . C43 C 0.7932(4) 0.00961(10) 0.1621(2) 0.0387(7) Uani 1 1 d . . . C44 C 0.7334(4) -0.02906(11) 0.1800(2) 0.0546(10) Uani 1 1 d . . . H44A H 0.6484 -0.0298 0.2088 0.065 Uiso 1 1 calc R . . C45 C 0.7953(5) -0.06658(12) 0.1567(3) 0.0613(11) Uani 1 1 d . . . H45A H 0.7533 -0.0919 0.1715 0.074 Uiso 1 1 calc R . . C46 C 0.9181(4) -0.06671(13) 0.1119(2) 0.0599(11) Uani 1 1 d . . . H46A H 0.9592 -0.0919 0.0952 0.072 Uiso 1 1 calc R . . C47 C 0.9783(4) -0.02956(13) 0.0925(2) 0.0581(10) Uani 1 1 d . . . H47A H 1.0615 -0.0291 0.0619 0.070 Uiso 1 1 calc R . . C48 C 0.9171(4) 0.00818(11) 0.1181(2) 0.0502(9) Uani 1 1 d . . . H48A H 0.9621 0.0333 0.1048 0.060 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 0.0320(2) 0.0301(2) 0.0377(3) -0.00250(19) 0.00408(19) -0.00143(18) N1 0.0304(14) 0.0398(15) 0.0472(17) -0.0056(13) -0.0024(12) -0.0048(12) N2 0.0464(17) 0.0371(16) 0.088(3) -0.0087(16) 0.0032(18) -0.0031(13) N3 0.0397(17) 0.0464(18) 0.091(3) -0.0094(17) -0.0051(17) -0.0005(14) N4 0.0325(14) 0.0464(17) 0.0555(19) -0.0135(14) 0.0032(13) -0.0078(12) N5 0.0426(15) 0.0345(14) 0.0451(17) -0.0098(13) 0.0041(13) -0.0059(12) N6 0.147(4) 0.067(2) 0.058(2) -0.011(2) 0.043(3) -0.033(2) N7 0.076(2) 0.0455(18) 0.064(2) -0.0020(16) 0.0167(19) -0.0134(16) N8 0.0557(18) 0.0323(14) 0.0405(17) -0.0074(12) -0.0004(14) 0.0031(13) N9 0.0444(16) 0.0414(15) 0.0455(18) 0.0007(13) -0.0042(14) 0.0028(12) N10 0.0396(17) 0.072(2) 0.070(2) -0.0074(18) -0.0054(16) 0.0176(15) N11 0.059(2) 0.167(4) 0.053(2) -0.008(3) 0.0058(19) 0.045(3) N12 0.0364(15) 0.0437(15) 0.0445(17) 0.0115(13) 0.0033(13) 0.0022(12) B1 0.047(2) 0.040(2) 0.038(2) 0.0011(17) 0.0050(18) -0.0024(17) Br1 0.0618(3) 0.0908(3) 0.0841(4) -0.0379(3) 0.0104(2) 0.0147(2) C1 0.042(2) 0.058(2) 0.086(3) 0.002(2) -0.004(2) -0.0168(18) C2 0.061(3) 0.075(3) 0.082(3) 0.003(2) -0.009(2) -0.017(2) C3 0.052(3) 0.070(3) 0.138(5) -0.045(3) 0.019(3) -0.030(2) C4 0.0351(17) 0.0398(18) 0.044(2) -0.0096(15) 0.0079(15) -0.0097(14) C5 0.0320(17) 0.0379(18) 0.050(2) -0.0078(15) 0.0065(15) -0.0001(13) C6 0.042(2) 0.084(3) 0.169(6) -0.027(4) -0.031(3) 0.005(2) C7 0.110(5) 0.054(3) 0.60(2) 0.031(6) -0.217(9) -0.021(3) C8 0.037(2) 0.061(2) 0.096(3) -0.024(2) 0.003(2) -0.0144(17) C9 0.059(2) 0.057(2) 0.060(3) -0.026(2) 0.008(2) -0.0090(18) C10 0.101(4) 0.114(4) 0.060(3) -0.046(3) 0.009(3) -0.025(3) C11 0.147(5) 0.090(4) 0.056(3) -0.023(3) 0.035(3) -0.030(3) C12 0.049(2) 0.047(2) 0.043(2) 0.0024(16) 0.0040(17) -0.0027(16) C13 0.0446(19) 0.0323(17) 0.049(2) -0.0028(15) -0.0019(17) -0.0017(13) C14 0.085(3) 0.038(2) 0.110(4) -0.009(2) 0.010(3) -0.005(2) C15 0.156(6) 0.045(3) 0.113(5) -0.016(3) 0.026(5) -0.012(3) C16 0.081(3) 0.044(2) 0.052(2) -0.0091(18) 0.002(2) 0.002(2) C17 0.060(2) 0.072(3) 0.053(3) 0.012(2) -0.009(2) 0.014(2) C18 0.097(4) 0.138(5) 0.085(4) 0.007(4) -0.031(3) 0.027(4) C19 0.052(2) 0.064(3) 0.091(4) 0.007(2) -0.014(2) 0.0117(19) C20 0.0368(17) 0.0343(17) 0.047(2) -0.0002(15) 0.0004(16) 0.0014(13) C21 0.0414(19) 0.0457(19) 0.046(2) -0.0050(16) 0.0063(17) 0.0003(15) C22 0.116(5) 0.288(10) 0.041(3) 0.003(5) 0.007(3) 0.084(6) C23 0.107(5) 0.314(11) 0.056(4) 0.001(5) -0.009(3) 0.101(6) C24 0.050(2) 0.081(3) 0.062(3) 0.015(2) -0.002(2) 0.008(2) C25 0.051(2) 0.0328(18) 0.061(3) -0.0007(17) 0.0022(19) -0.0004(15) C26 0.106(4) 0.058(3) 0.070(3) -0.010(2) 0.019(3) -0.026(2) C27 0.137(6) 0.065(3) 0.177(7) -0.039(4) 0.018(6) -0.051(4) C28 0.122(5) 0.068(4) 0.126(5) 0.034(4) 0.047(5) -0.013(3) C29 0.091(4) 0.066(3) 0.082(4) 0.019(3) 0.024(3) -0.006(3) C30 0.066(3) 0.049(2) 0.057(3) 0.0120(19) -0.001(2) -0.0054(18) C31 0.051(2) 0.0352(17) 0.0355(19) 0.0040(14) 0.0076(16) -0.0036(14) C32 0.056(2) 0.060(2) 0.039(2) -0.0082(18) -0.0012(18) -0.0100(18) C33 0.060(3) 0.075(3) 0.060(3) -0.001(2) -0.013(2) -0.017(2) C34 0.049(2) 0.082(3) 0.068(3) 0.013(3) -0.005(2) -0.015(2) C35 0.059(3) 0.056(2) 0.084(3) 0.019(2) 0.007(2) 0.014(2) C36 0.052(2) 0.045(2) 0.059(2) 0.0042(18) -0.0024(19) -0.0036(17) C37 0.060(2) 0.0332(17) 0.038(2) -0.0076(15) -0.0052(17) 0.0014(15) C38 0.081(3) 0.060(3) 0.058(3) -0.010(2) -0.013(2) 0.012(2) C39 0.115(4) 0.074(3) 0.071(4) -0.010(3) -0.037(3) 0.018(3) C40 0.178(7) 0.075(3) 0.046(3) -0.009(3) -0.013(4) 0.010(4) C41 0.132(5) 0.064(3) 0.050(3) -0.001(2) 0.015(3) 0.002(3) C42 0.073(3) 0.046(2) 0.043(2) -0.0075(17) 0.005(2) -0.0049(18) C43 0.0457(19) 0.0417(18) 0.0286(17) -0.0008(14) -0.0010(15) 0.0020(14) C44 0.063(2) 0.043(2) 0.057(3) -0.0017(18) 0.015(2) 0.0004(17) C45 0.081(3) 0.043(2) 0.060(3) -0.0030(19) -0.003(2) -0.0003(19) C46 0.070(3) 0.065(3) 0.045(2) -0.0084(19) -0.005(2) 0.026(2) C47 0.055(2) 0.066(3) 0.053(3) 0.006(2) 0.011(2) 0.018(2) C48 0.051(2) 0.053(2) 0.047(2) 0.0090(17) 0.0074(18) 0.0046(17) _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 N9 2.018(3) . ? Fe1 N4 2.029(3) . ? Fe1 N1 2.030(3) . ? Fe1 N12 2.036(3) . ? Fe1 N8 2.039(3) . ? Fe1 N5 2.061(3) . ? N1 C4 1.270(4) . ? N1 C1 1.462(5) . ? N2 C4 1.354(4) . ? N2 C3 1.490(6) . ? N2 H2A 0.8600 . ? N3 C5 1.343(5) . ? N3 C6 1.448(5) . ? N3 H3A 0.8600 . ? N4 C5 1.290(4) . ? N4 C8 1.474(5) . ? N5 C12 1.289(4) . ? N5 C9 1.481(4) . ? N6 C12 1.318(5) . ? N6 C11 1.465(5) . ? N6 H6A 0.8600 . ? N7 C13 1.342(4) . ? N7 C14 1.473(5) . ? N7 H7A 0.8600 . ? N8 C13 1.303(4) . ? N8 C16 1.484(4) . ? N9 C20 1.287(4) . ? N9 C17 1.460(5) . ? N10 C20 1.354(4) . ? N10 C19 1.453(6) . ? N10 H10A 0.8600 . ? N11 C21 1.355(5) . ? N11 C22 1.466(7) . ? N11 H11A 0.8600 . ? N12 C21 1.290(4) . ? N12 C24 1.453(5) . ? B1 C31 1.633(6) . ? B1 C25 1.634(5) . ? B1 C37 1.641(6) . ? B1 C43 1.672(5) . ? C1 C2 1.468(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.488(6) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.483(5) . ? C6 C7 1.397(7) . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.375(8) . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.453(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.485(8) . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 C13 1.505(5) . ? C14 C15 1.466(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.463(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.509(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.511(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.473(5) . ? C22 C23 1.301(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.470(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.356(6) . ? C25 C30 1.408(5) . ? C26 C27 1.456(7) . ? C26 H26A 0.9300 . ? C27 C28 1.315(9) . ? C27 H27A 0.9300 . ? C28 C29 1.310(8) . ? C28 H28A 0.9300 . ? C29 C30 1.352(6) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.384(5) . ? C31 C36 1.400(5) . ? C32 C33 1.372(6) . ? C32 H32A 0.9300 . ? C33 C34 1.346(6) . ? C33 H33A 0.9300 . ? C34 C35 1.324(6) . ? C34 H34A 0.9300 . ? C35 C36 1.388(6) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C38 1.396(6) . ? C37 C42 1.396(5) . ? C38 C39 1.413(7) . ? C38 H38A 0.9300 . ? C39 C40 1.396(8) . ? C39 H39A 0.9300 . ? C40 C41 1.338(9) . ? C40 H40A 0.9300 . ? C41 C42 1.404(6) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C48 1.371(5) . ? C43 C44 1.383(5) . ? C44 C45 1.381(5) . ? C44 H44A 0.9300 . ? C45 C46 1.369(6) . ? C45 H45A 0.9300 . ? C46 C47 1.347(6) . ? C46 H46A 0.9300 . ? C47 C48 1.394(5) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Fe1 N4 170.03(11) . . ? N9 Fe1 N1 95.32(11) . . ? N4 Fe1 N1 78.03(11) . . ? N9 Fe1 N12 77.72(12) . . ? N4 Fe1 N12 95.08(11) . . ? N1 Fe1 N12 93.17(11) . . ? N9 Fe1 N8 89.83(11) . . ? N4 Fe1 N8 97.69(11) . . ? N1 Fe1 N8 171.50(11) . . ? N12 Fe1 N8 94.54(11) . . ? N9 Fe1 N5 96.58(12) . . ? N4 Fe1 N5 91.39(12) . . ? N1 Fe1 N5 94.41(10) . . ? N12 Fe1 N5 170.91(11) . . ? N8 Fe1 N5 78.24(11) . . ? C4 N1 C1 118.0(3) . . ? C4 N1 Fe1 116.3(2) . . ? C1 N1 Fe1 125.4(2) . . ? C4 N2 C3 119.2(3) . . ? C4 N2 H2A 120.4 . . ? C3 N2 H2A 120.4 . . ? C5 N3 C6 120.0(3) . . ? C5 N3 H3A 120.0 . . ? C6 N3 H3A 120.0 . . ? C5 N4 C8 119.5(3) . . ? C5 N4 Fe1 115.9(2) . . ? C8 N4 Fe1 124.6(2) . . ? C12 N5 C9 116.1(3) . . ? C12 N5 Fe1 116.1(2) . . ? C9 N5 Fe1 127.2(2) . . ? C12 N6 C11 123.3(4) . . ? C12 N6 H6A 118.3 . . ? C11 N6 H6A 118.3 . . ? C13 N7 C14 120.8(3) . . ? C13 N7 H7A 119.6 . . ? C14 N7 H7A 119.6 . . ? C13 N8 C16 117.6(3) . . ? C13 N8 Fe1 115.7(2) . . ? C16 N8 Fe1 126.0(2) . . ? C20 N9 C17 118.5(3) . . ? C20 N9 Fe1 117.1(2) . . ? C17 N9 Fe1 124.4(2) . . ? C20 N10 C19 120.5(3) . . ? C20 N10 H10A 119.8 . . ? C19 N10 H10A 119.8 . . ? C21 N11 C22 120.5(4) . . ? C21 N11 H11A 119.7 . . ? C22 N11 H11A 119.7 . . ? C21 N12 C24 118.1(3) . . ? C21 N12 Fe1 116.1(2) . . ? C24 N12 Fe1 125.8(2) . . ? C31 B1 C25 107.6(3) . . ? C31 B1 C37 111.2(3) . . ? C25 B1 C37 110.3(3) . . ? C31 B1 C43 111.7(3) . . ? C25 B1 C43 110.7(3) . . ? C37 B1 C43 105.4(3) . . ? N1 C1 C2 115.6(4) . . ? N1 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? N1 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? C1 C2 C3 110.8(4) . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? C3 C2 H2C 109.5 . . ? H2B C2 H2C 108.1 . . ? C2 C3 N2 109.0(3) . . ? C2 C3 H3B 109.9 . . ? N2 C3 H3B 109.9 . . ? C2 C3 H3C 109.9 . . ? N2 C3 H3C 109.9 . . ? H3B C3 H3C 108.3 . . ? N1 C4 N2 126.1(3) . . ? N1 C4 C5 114.9(3) . . ? N2 C4 C5 119.0(3) . . ? N4 C5 N3 125.1(3) . . ? N4 C5 C4 114.4(3) . . ? N3 C5 C4 120.5(3) . . ? C7 C6 N3 112.8(4) . . ? C7 C6 H6B 109.0 . . ? N3 C6 H6B 109.0 . . ? C7 C6 H6C 109.0 . . ? N3 C6 H6C 109.0 . . ? H6B C6 H6C 107.8 . . ? C8 C7 C6 124.7(6) . . ? C8 C7 H7B 106.1 . . ? C6 C7 H7B 106.1 . . ? C8 C7 H7C 106.1 . . ? C6 C7 H7C 106.1 . . ? H7B C7 H7C 106.3 . . ? C7 C8 N4 114.1(4) . . ? C7 C8 H8A 108.7 . . ? N4 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? N4 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 N5 114.1(3) . . ? C10 C9 H9A 108.7 . . ? N5 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? N5 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 116.2(4) . . ? C9 C10 H10B 108.2 . . ? C11 C10 H10B 108.2 . . ? C9 C10 H10C 108.2 . . ? C11 C10 H10C 108.2 . . ? H10B C10 H10C 107.4 . . ? N6 C11 C10 105.1(4) . . ? N6 C11 H11B 110.7 . . ? C10 C11 H11B 110.7 . . ? N6 C11 H11C 110.7 . . ? C10 C11 H11C 110.7 . . ? H11B C11 H11C 108.8 . . ? N5 C12 N6 126.6(3) . . ? N5 C12 C13 113.7(3) . . ? N6 C12 C13 119.6(3) . . ? N8 C13 N7 125.8(3) . . ? N8 C13 C12 115.3(3) . . ? N7 C13 C12 119.0(3) . . ? C15 C14 N7 110.8(4) . . ? C15 C14 H14A 109.5 . . ? N7 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? N7 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 114.4(4) . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C15 C16 N8 114.6(4) . . ? C15 C16 H16A 108.6 . . ? N8 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? N8 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N9 C17 C18 113.6(4) . . ? N9 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? N9 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 110.4(5) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N10 C19 C18 110.6(3) . . ? N10 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? N10 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? N9 C20 N10 126.1(3) . . ? N9 C20 C21 114.3(3) . . ? N10 C20 C21 119.6(3) . . ? N12 C21 N11 125.0(4) . . ? N12 C21 C20 114.7(3) . . ? N11 C21 C20 120.2(3) . . ? C23 C22 N11 116.1(5) . . ? C23 C22 H22A 108.3 . . ? N11 C22 H22A 108.3 . . ? C23 C22 H22B 108.3 . . ? N11 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 C24 123.3(5) . . ? C22 C23 H23A 106.5 . . ? C24 C23 H23A 106.5 . . ? C22 C23 H23B 106.5 . . ? C24 C23 H23B 106.5 . . ? H23A C23 H23B 106.5 . . ? N12 C24 C23 116.7(4) . . ? N12 C24 H24A 108.1 . . ? C23 C24 H24A 108.1 . . ? N12 C24 H24B 108.1 . . ? C23 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C30 114.2(3) . . ? C26 C25 B1 125.5(4) . . ? C30 C25 B1 120.4(3) . . ? C25 C26 C27 119.4(5) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C28 C27 C26 122.4(6) . . ? C28 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C29 C28 C27 118.5(5) . . ? C29 C28 H28A 120.8 . . ? C27 C28 H28A 120.8 . . ? C28 C29 C30 121.6(5) . . ? C28 C29 H29A 119.2 . . ? C30 C29 H29A 119.2 . . ? C29 C30 C25 124.0(4) . . ? C29 C30 H30A 118.0 . . ? C25 C30 H30A 118.0 . . ? C32 C31 C36 113.1(4) . . ? C32 C31 B1 126.3(3) . . ? C36 C31 B1 120.5(3) . . ? C33 C32 C31 121.9(4) . . ? C33 C32 H32A 119.1 . . ? C31 C32 H32A 119.1 . . ? C34 C33 C32 122.6(4) . . ? C34 C33 H33A 118.7 . . ? C32 C33 H33A 118.7 . . ? C35 C34 C33 118.7(4) . . ? C35 C34 H34A 120.7 . . ? C33 C34 H34A 120.7 . . ? C34 C35 C36 119.9(4) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 123.8(4) . . ? C35 C36 H36A 118.1 . . ? C31 C36 H36A 118.1 . . ? C38 C37 C42 114.7(4) . . ? C38 C37 B1 119.2(3) . . ? C42 C37 B1 126.0(4) . . ? C37 C38 C39 121.9(5) . . ? C37 C38 H38A 119.0 . . ? C39 C38 H38A 119.0 . . ? C40 C39 C38 119.8(5) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C41 C40 C39 119.8(5) . . ? C41 C40 H40A 120.1 . . ? C39 C40 H40A 120.1 . . ? C40 C41 C42 119.7(5) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C37 C42 C41 123.9(5) . . ? C37 C42 H42A 118.0 . . ? C41 C42 H42A 118.0 . . ? C48 C43 C44 115.3(3) . . ? C48 C43 B1 125.3(3) . . ? C44 C43 B1 119.4(3) . . ? C45 C44 C43 122.5(4) . . ? C45 C44 H44A 118.8 . . ? C43 C44 H44A 118.8 . . ? C46 C45 C44 120.4(4) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? C47 C46 C45 118.6(4) . . ? C47 C46 H46A 120.7 . . ? C45 C46 H46A 120.7 . . ? C46 C47 C48 120.6(4) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C43 C48 C47 122.5(3) . . ? C43 C48 H48A 118.8 . . ? C47 C48 H48A 118.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6A Br1 0.86 2.48 3.314(3) 163.9 2_645 N7 H7A Br1 0.86 2.66 3.510(3) 168.1 2_645 N10 H10A Br1 0.86 2.66 3.508(3) 171.3 3_765 N11 H11A Br1 0.86 2.48 3.322(4) 167.4 3_765 _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 33.48 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 0.748 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.119