data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H41 Co N4 O2' _chemical_formula_weight 536.59 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' 'Co' 'Co' 0.3494 0.9721 '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 12.590(2) _cell_length_b 16.240(3) _cell_length_c 16.649(3) _cell_angle_alpha 111.071(3) _cell_angle_beta 99.370(3) _cell_angle_gamma 109.899(3) _cell_volume 2824.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8876 _cell_measurement_theta_min 2.305 _cell_measurement_theta_max 24.538 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method ? _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details SADABS _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 '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 42216 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.71 _reflns_number_total 9575 _reflns_number_gt 6074 _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^)+(0.0609P)^2^+2.1916P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 9575 _refine_ls_number_parameters 653 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1465 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.003 _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 Co1 Co 0.64025(5) 0.66889(4) 0.19592(4) 0.01873(17) Uani 1 1 d . . . O1 O 0.5742(3) 0.7495(3) 0.0850(3) 0.0684(14) Uani 1 1 d . . . N1 N 0.6685(3) 0.7391(2) 0.3261(2) 0.0182(8) Uani 1 1 d . . . C1 C 0.7626(5) 0.7916(4) 0.4878(3) 0.0303(12) Uani 1 1 d . . . H1A H 0.6856 0.7532 0.4911 0.045 Uiso 1 1 calc R . . H1B H 0.7771 0.8605 0.5113 0.045 Uiso 1 1 calc R . . H1C H 0.8265 0.7859 0.5245 0.045 Uiso 1 1 calc R . . C2 C 0.7603(4) 0.7536(3) 0.3907(3) 0.0205(10) Uani 1 1 d . . . N2 N 0.8076(3) 0.6931(2) 0.2142(2) 0.0180(8) Uani 1 1 d . . . O2 O 0.4678(3) 0.4771(3) 0.0991(3) 0.0433(10) Uani 1 1 d . . . Co2 Co 0.59729(5) 0.16031(4) 0.19525(4) 0.01780(17) Uani 1 1 d . . . N3 N 0.5947(3) 0.7132(3) 0.1308(3) 0.0306(10) Uani 1 1 d . . . C3 C 0.8576(4) 0.7365(3) 0.3732(3) 0.0208(10) Uani 1 1 d . . . H3A H 0.9119 0.7394 0.4221 0.025 Uiso 1 1 calc R . . O3 O 0.5133(4) 0.2331(3) 0.0826(3) 0.0455(10) Uani 1 1 d . . . N4 N 0.5504(4) 0.5479(3) 0.1540(3) 0.0264(9) Uani 1 1 d . . . C4 C 0.8838(4) 0.7155(3) 0.2916(3) 0.0190(10) Uani 1 1 d . . . O4 O 0.6355(3) 0.0152(3) 0.0712(3) 0.0454(10) Uani 1 1 d . . . C5 C 1.0070(4) 0.7203(3) 0.2956(3) 0.0234(11) Uani 1 1 d . . . H5A H 1.0390 0.7520 0.2590 0.035 Uiso 1 1 calc R . . H5B H 1.0017 0.6538 0.2714 0.035 Uiso 1 1 calc R . . H5C H 1.0601 0.7582 0.3589 0.035 Uiso 1 1 calc R . . N5 N 0.4761(3) 0.1208(2) 0.2507(2) 0.0173(8) Uani 1 1 d . . . C6 C 0.5880(4) 0.7811(3) 0.3524(3) 0.0187(10) Uani 1 1 d . . . N6 N 0.7215(3) 0.2513(3) 0.3130(2) 0.0189(8) Uani 1 1 d . . . C7 C 0.6231(4) 0.8813(3) 0.3766(3) 0.0205(10) Uani 1 1 d . . . N7 N 0.5555(3) 0.2029(3) 0.1257(3) 0.0237(9) Uani 1 1 d . . . C8 C 0.5432(4) 0.9206(3) 0.3973(3) 0.0238(11) Uani 1 1 d . . . H8A H 0.5666 0.9883 0.4151 0.029 Uiso 1 1 calc R . . N8 N 0.6283(3) 0.0650(3) 0.1388(3) 0.0277(10) Uani 1 1 d . . . C9 C 0.4304(4) 0.8628(3) 0.3925(3) 0.0229(11) Uani 1 1 d . . . H9A H 0.3764 0.8906 0.4061 0.027 Uiso 1 1 calc R . . C10 C 0.3966(4) 0.7650(3) 0.3679(3) 0.0209(10) Uani 1 1 d . . . H10A H 0.3188 0.7258 0.3648 0.025 Uiso 1 1 calc R . . C11 C 0.4732(4) 0.7218(3) 0.3475(3) 0.0191(10) Uani 1 1 d . . . C12 C 0.4063(5) 0.5892(4) 0.3981(4) 0.0360(13) Uani 1 1 d . . . H12A H 0.4783 0.6285 0.4518 0.054 Uiso 1 1 calc R . . H12B H 0.3843 0.5195 0.3794 0.054 Uiso 1 1 calc R . . H12C H 0.3407 0.6041 0.4129 0.054 Uiso 1 1 calc R . . C13 C 0.4307(4) 0.6136(3) 0.3201(3) 0.0232(11) Uani 1 1 d . . . H13A H 0.4954 0.5952 0.3046 0.028 Uiso 1 1 calc R . . C14 C 0.3194(4) 0.5533(3) 0.2356(3) 0.0322(13) Uani 1 1 d . . . H14A H 0.3363 0.5698 0.1865 0.048 Uiso 1 1 calc R . . H14B H 0.2535 0.5680 0.2499 0.048 Uiso 1 1 calc R . . H14C H 0.2971 0.4834 0.2162 0.048 Uiso 1 1 calc R . . C15 C 0.8150(5) 1.0339(4) 0.4752(4) 0.0568(18) Uani 1 1 d . . . H15A H 0.8928 1.0751 0.4752 0.085 Uiso 1 1 calc R . . H15B H 0.8270 1.0088 0.5197 0.085 Uiso 1 1 calc R . . H15C H 0.7702 1.0728 0.4914 0.085 Uiso 1 1 calc R . . C16 C 0.7449(4) 0.9480(3) 0.3804(3) 0.0310(13) Uani 1 1 d . . . H16A H 0.7915 0.9089 0.3649 0.037 Uiso 1 1 calc R . . C17 C 0.7303(5) 0.9876(4) 0.3109(4) 0.0419(15) Uani 1 1 d . . . H17A H 0.6862 0.9328 0.2500 0.063 Uiso 1 1 calc R . . H17B H 0.8093 1.0281 0.3121 0.063 Uiso 1 1 calc R . . H17C H 0.6862 1.0273 0.3260 0.063 Uiso 1 1 calc R . . C18 C 0.8445(4) 0.6828(3) 0.1352(3) 0.0182(10) Uani 1 1 d . . . C19 C 0.8750(4) 0.7611(3) 0.1127(3) 0.0207(10) Uani 1 1 d . . . C20 C 0.9034(4) 0.7485(3) 0.0338(3) 0.0257(11) Uani 1 1 d . . . H20A H 0.9221 0.8005 0.0170 0.031 Uiso 1 1 calc R . . C21 C 0.9053(4) 0.6617(3) -0.0218(3) 0.0254(11) Uani 1 1 d . . . H21A H 0.9271 0.6550 -0.0750 0.031 Uiso 1 1 calc R . . C22 C 0.8753(4) 0.5859(3) 0.0016(3) 0.0234(11) Uani 1 1 d . . . H22A H 0.8766 0.5267 -0.0363 0.028 Uiso 1 1 calc R . . C23 C 0.8433(4) 0.5931(3) 0.0786(3) 0.0201(10) Uani 1 1 d . . . C24 C 0.8963(5) 0.4634(4) 0.0997(4) 0.0351(13) Uani 1 1 d . . . H24A H 0.9725 0.5144 0.1460 0.053 Uiso 1 1 calc R . . H24B H 0.9073 0.4409 0.0399 0.053 Uiso 1 1 calc R . . H24C H 0.8678 0.4083 0.1144 0.053 Uiso 1 1 calc R . . C25 C 0.8044(4) 0.5051(3) 0.0975(3) 0.0252(11) Uani 1 1 d . . . H25A H 0.7927 0.5258 0.1584 0.030 Uiso 1 1 calc R . . C26 C 0.6843(4) 0.4250(3) 0.0258(3) 0.0296(12) Uani 1 1 d . . . H26A H 0.6252 0.4517 0.0250 0.044 Uiso 1 1 calc R . . H26B H 0.6566 0.3701 0.0410 0.044 Uiso 1 1 calc R . . H26C H 0.6943 0.4022 -0.0343 0.044 Uiso 1 1 calc R . . C27 C 1.0003(4) 0.9256(3) 0.2471(3) 0.0333(13) Uani 1 1 d . . . H27A H 1.0205 0.8918 0.2812 0.050 Uiso 1 1 calc R . . H27B H 0.9977 0.9850 0.2887 0.050 Uiso 1 1 calc R . . H27C H 1.0609 0.9433 0.2184 0.050 Uiso 1 1 calc R . . C28 C 0.8785(4) 0.8582(3) 0.1739(3) 0.0233(11) Uani 1 1 d . . . H28A H 0.8184 0.8439 0.2055 0.028 Uiso 1 1 calc R . . C29 C 0.8449(4) 0.9110(3) 0.1213(3) 0.0293(12) Uani 1 1 d . . . H29A H 0.7659 0.8677 0.0751 0.044 Uiso 1 1 calc R . . H29B H 0.9042 0.9287 0.0916 0.044 Uiso 1 1 calc R . . H29C H 0.8430 0.9705 0.1636 0.044 Uiso 1 1 calc R . . C30 C 0.3996(4) 0.0847(3) 0.3668(3) 0.0224(11) Uani 1 1 d . . . H30A H 0.3285 0.0905 0.3407 0.034 Uiso 1 1 calc R . . H30B H 0.4243 0.1184 0.4334 0.034 Uiso 1 1 calc R . . H30C H 0.3812 0.0153 0.3470 0.034 Uiso 1 1 calc R . . C31 C 0.5000(4) 0.1307(3) 0.3349(3) 0.0155(10) Uani 1 1 d . . . C32 C 0.6150(4) 0.1825(3) 0.3975(3) 0.0191(10) Uani 1 1 d . . . H32A H 0.6252 0.1749 0.4518 0.023 Uiso 1 1 calc R . . C33 C 0.7164(4) 0.2438(3) 0.3894(3) 0.0181(10) Uani 1 1 d . . . C34 C 0.8249(4) 0.3069(3) 0.4734(3) 0.0253(11) Uani 1 1 d . . . H34A H 0.8947 0.3003 0.4587 0.038 Uiso 1 1 calc R . . H34B H 0.8122 0.2860 0.5208 0.038 Uiso 1 1 calc R . . H34C H 0.8384 0.3754 0.4953 0.038 Uiso 1 1 calc R . . C35 C 0.3548(4) 0.0755(3) 0.1920(3) 0.0166(10) Uani 1 1 d . . . C36 C 0.2942(4) -0.0271(3) 0.1417(3) 0.0187(10) Uani 1 1 d . . . C37 C 0.1824(4) -0.0666(3) 0.0785(3) 0.0223(11) Uani 1 1 d . . . H37A H 0.1396 -0.1356 0.0442 0.027 Uiso 1 1 calc R . . C38 C 0.1320(4) -0.0080(3) 0.0644(3) 0.0232(11) Uani 1 1 d . . . H38A H 0.0565 -0.0366 0.0190 0.028 Uiso 1 1 calc R . . C39 C 0.1906(4) 0.0920(3) 0.1158(3) 0.0216(11) Uani 1 1 d . . . H39A H 0.1533 0.1316 0.1074 0.026 Uiso 1 1 calc R . . C40 C 0.3033(4) 0.1360(3) 0.1796(3) 0.0185(10) Uani 1 1 d . . . C41 C 0.3619(4) 0.2812(3) 0.3324(3) 0.0302(12) Uani 1 1 d . . . H41A H 0.3909 0.2465 0.3614 0.045 Uiso 1 1 calc R . . H41B H 0.2790 0.2668 0.3303 0.045 Uiso 1 1 calc R . . H41C H 0.4118 0.3518 0.3676 0.045 Uiso 1 1 calc R . . C42 C 0.3682(4) 0.2472(3) 0.2349(3) 0.0191(10) Uani 1 1 d . . . H42A H 0.4543 0.2666 0.2402 0.023 Uiso 1 1 calc R . . C43 C 0.3254(4) 0.3019(3) 0.1896(4) 0.0318(12) Uani 1 1 d . . . H43A H 0.3309 0.2807 0.1280 0.048 Uiso 1 1 calc R . . H43B H 0.3756 0.3725 0.2254 0.048 Uiso 1 1 calc R . . H43C H 0.2423 0.2878 0.1863 0.048 Uiso 1 1 calc R . . C44 C 0.2642(4) -0.1710(3) 0.1760(4) 0.0320(12) Uani 1 1 d . . . H44A H 0.2512 -0.1370 0.2327 0.048 Uiso 1 1 calc R . . H44B H 0.3017 -0.2127 0.1837 0.048 Uiso 1 1 calc R . . H44C H 0.1874 -0.2114 0.1268 0.048 Uiso 1 1 calc R . . C45 C 0.3460(4) -0.0955(3) 0.1521(3) 0.0217(11) Uani 1 1 d . . . H45A H 0.4242 -0.0556 0.2025 0.026 Uiso 1 1 calc R . . C46 C 0.3687(5) -0.1482(3) 0.0644(3) 0.0325(13) Uani 1 1 d . . . H46A H 0.4221 -0.0997 0.0498 0.049 Uiso 1 1 calc R . . H46B H 0.2927 -0.1887 0.0143 0.049 Uiso 1 1 calc R . . H46C H 0.4059 -0.1898 0.0729 0.049 Uiso 1 1 calc R . . C47 C 0.8210(4) 0.3313(3) 0.3167(3) 0.0179(10) Uani 1 1 d . . . C48 C 0.9159(4) 0.3169(3) 0.2912(3) 0.0173(10) Uani 1 1 d . . . C49 C 1.0090(4) 0.3953(3) 0.2930(3) 0.0240(11) Uani 1 1 d . . . H49A H 1.0742 0.3864 0.2758 0.029 Uiso 1 1 calc R . . C50 C 1.0076(4) 0.4853(3) 0.3197(3) 0.0241(11) Uani 1 1 d . . . H50A H 1.0720 0.5383 0.3212 0.029 Uiso 1 1 calc R . . C51 C 0.9137(4) 0.4992(3) 0.3441(3) 0.0215(11) Uani 1 1 d . . . H51A H 0.9136 0.5617 0.3616 0.026 Uiso 1 1 calc R . . C52 C 0.8190(4) 0.4235(3) 0.3436(3) 0.0185(10) Uani 1 1 d . . . C53 C 0.6511(4) 0.4668(4) 0.3030(4) 0.0329(13) Uani 1 1 d . . . H53A H 0.6225 0.4132 0.2415 0.049 Uiso 1 1 calc R . . H53B H 0.7061 0.5274 0.3047 0.049 Uiso 1 1 calc R . . H53C H 0.5831 0.4753 0.3196 0.049 Uiso 1 1 calc R . . C54 C 0.7164(4) 0.4423(3) 0.3706(3) 0.0261(11) Uani 1 1 d . . . H54A H 0.6585 0.3812 0.3691 0.031 Uiso 1 1 calc R . . C55 C 0.7600(5) 0.5251(4) 0.4667(3) 0.0341(13) Uani 1 1 d . . . H55A H 0.8010 0.5089 0.5099 0.051 Uiso 1 1 calc R . . H55B H 0.6916 0.5335 0.4828 0.051 Uiso 1 1 calc R . . H55C H 0.8155 0.5860 0.4691 0.051 Uiso 1 1 calc R . . C56 C 1.0236(4) 0.2228(4) 0.3275(4) 0.0367(13) Uani 1 1 d . . . H56A H 1.0163 0.2452 0.3885 0.055 Uiso 1 1 calc R . . H56B H 1.0994 0.2686 0.3289 0.055 Uiso 1 1 calc R . . H56C H 1.0217 0.1576 0.3076 0.055 Uiso 1 1 calc R . . C57 C 0.9196(4) 0.2182(3) 0.2609(3) 0.0214(11) Uani 1 1 d . . . H57A H 0.8434 0.1702 0.2596 0.026 Uiso 1 1 calc R . . C58 C 0.9278(5) 0.1823(3) 0.1648(3) 0.0350(13) Uani 1 1 d . . . H58A H 0.8602 0.1790 0.1231 0.052 Uiso 1 1 calc R . . H58B H 0.9259 0.1170 0.1448 0.052 Uiso 1 1 calc R . . H58C H 1.0027 0.2277 0.1648 0.052 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 Co1 0.0211(4) 0.0172(3) 0.0226(4) 0.0094(3) 0.0093(3) 0.0118(3) O1 0.040(3) 0.068(3) 0.104(4) 0.070(3) -0.005(2) 0.010(2) N1 0.017(2) 0.0157(19) 0.026(2) 0.0111(17) 0.0084(17) 0.0082(16) C1 0.038(3) 0.037(3) 0.022(3) 0.013(2) 0.012(2) 0.022(3) C2 0.026(3) 0.015(2) 0.024(3) 0.010(2) 0.011(2) 0.011(2) N2 0.022(2) 0.0144(19) 0.020(2) 0.0072(17) 0.0081(18) 0.0099(17) O2 0.038(2) 0.031(2) 0.047(2) 0.007(2) 0.015(2) 0.0119(19) Co2 0.0192(4) 0.0172(3) 0.0200(4) 0.0085(3) 0.0083(3) 0.0101(3) N3 0.022(2) 0.028(2) 0.045(3) 0.021(2) 0.011(2) 0.0101(19) C3 0.027(3) 0.019(2) 0.024(3) 0.012(2) 0.008(2) 0.015(2) O3 0.072(3) 0.062(3) 0.045(2) 0.040(2) 0.031(2) 0.052(2) N4 0.024(2) 0.022(2) 0.027(2) 0.006(2) 0.008(2) 0.0081(19) C4 0.018(3) 0.011(2) 0.030(3) 0.009(2) 0.009(2) 0.0082(19) O4 0.052(3) 0.039(2) 0.042(2) 0.009(2) 0.020(2) 0.025(2) C5 0.024(3) 0.023(3) 0.027(3) 0.010(2) 0.009(2) 0.014(2) N5 0.019(2) 0.0157(19) 0.020(2) 0.0083(17) 0.0059(17) 0.0100(16) C6 0.026(3) 0.019(2) 0.018(2) 0.009(2) 0.010(2) 0.016(2) N6 0.018(2) 0.019(2) 0.025(2) 0.0139(18) 0.0093(17) 0.0097(17) C7 0.025(3) 0.018(2) 0.022(3) 0.008(2) 0.012(2) 0.013(2) N7 0.031(2) 0.024(2) 0.023(2) 0.0103(19) 0.0154(19) 0.0160(19) C8 0.032(3) 0.017(2) 0.025(3) 0.009(2) 0.011(2) 0.013(2) N8 0.026(2) 0.022(2) 0.026(2) 0.0009(19) 0.0110(19) 0.0100(19) C9 0.026(3) 0.026(3) 0.023(3) 0.009(2) 0.010(2) 0.019(2) C10 0.025(3) 0.023(2) 0.017(2) 0.008(2) 0.009(2) 0.013(2) C11 0.022(3) 0.021(2) 0.019(2) 0.009(2) 0.011(2) 0.013(2) C12 0.055(4) 0.032(3) 0.043(3) 0.024(3) 0.030(3) 0.028(3) C13 0.024(3) 0.020(2) 0.031(3) 0.012(2) 0.012(2) 0.012(2) C14 0.027(3) 0.021(3) 0.044(3) 0.010(2) 0.012(3) 0.011(2) C15 0.040(4) 0.034(3) 0.062(4) 0.004(3) 0.011(3) 0.000(3) C16 0.028(3) 0.017(2) 0.047(3) 0.008(2) 0.019(3) 0.012(2) C17 0.049(4) 0.031(3) 0.073(4) 0.031(3) 0.043(3) 0.028(3) C18 0.017(3) 0.020(2) 0.021(3) 0.010(2) 0.010(2) 0.009(2) C19 0.016(3) 0.020(2) 0.027(3) 0.010(2) 0.007(2) 0.008(2) C20 0.027(3) 0.029(3) 0.029(3) 0.019(2) 0.013(2) 0.012(2) C21 0.026(3) 0.029(3) 0.021(3) 0.011(2) 0.010(2) 0.010(2) C22 0.020(3) 0.020(2) 0.027(3) 0.007(2) 0.008(2) 0.009(2) C23 0.018(3) 0.026(3) 0.020(3) 0.009(2) 0.010(2) 0.012(2) C24 0.047(3) 0.035(3) 0.036(3) 0.016(3) 0.016(3) 0.030(3) C25 0.035(3) 0.020(2) 0.029(3) 0.011(2) 0.016(2) 0.017(2) C26 0.032(3) 0.019(3) 0.040(3) 0.011(2) 0.019(3) 0.013(2) C27 0.042(3) 0.019(3) 0.040(3) 0.011(2) 0.015(3) 0.016(2) C28 0.028(3) 0.020(2) 0.030(3) 0.015(2) 0.015(2) 0.013(2) C29 0.037(3) 0.030(3) 0.040(3) 0.024(3) 0.021(3) 0.023(2) C30 0.023(3) 0.024(3) 0.024(3) 0.012(2) 0.010(2) 0.012(2) C31 0.020(3) 0.012(2) 0.024(3) 0.011(2) 0.012(2) 0.0119(19) C32 0.022(3) 0.017(2) 0.022(3) 0.010(2) 0.008(2) 0.012(2) C33 0.019(3) 0.015(2) 0.025(3) 0.007(2) 0.010(2) 0.012(2) C34 0.018(3) 0.029(3) 0.025(3) 0.012(2) 0.004(2) 0.006(2) C35 0.015(2) 0.020(2) 0.022(2) 0.014(2) 0.010(2) 0.010(2) C36 0.024(3) 0.018(2) 0.022(3) 0.011(2) 0.013(2) 0.013(2) C37 0.021(3) 0.019(2) 0.022(3) 0.009(2) 0.005(2) 0.005(2) C38 0.020(3) 0.022(3) 0.026(3) 0.010(2) 0.004(2) 0.010(2) C39 0.020(3) 0.023(2) 0.032(3) 0.015(2) 0.011(2) 0.016(2) C40 0.022(3) 0.019(2) 0.023(3) 0.012(2) 0.012(2) 0.014(2) C41 0.032(3) 0.027(3) 0.036(3) 0.011(2) 0.017(2) 0.019(2) C42 0.020(3) 0.017(2) 0.026(3) 0.011(2) 0.010(2) 0.011(2) C43 0.031(3) 0.025(3) 0.046(3) 0.018(3) 0.010(3) 0.017(2) C44 0.039(3) 0.021(3) 0.040(3) 0.019(2) 0.013(3) 0.012(2) C45 0.021(3) 0.013(2) 0.028(3) 0.007(2) 0.005(2) 0.008(2) C46 0.036(3) 0.025(3) 0.036(3) 0.006(2) 0.012(3) 0.020(2) C47 0.015(2) 0.019(2) 0.019(2) 0.009(2) 0.005(2) 0.006(2) C48 0.015(2) 0.018(2) 0.020(2) 0.008(2) 0.006(2) 0.008(2) C49 0.017(3) 0.022(3) 0.029(3) 0.009(2) 0.009(2) 0.007(2) C50 0.021(3) 0.020(2) 0.028(3) 0.014(2) 0.006(2) 0.003(2) C51 0.024(3) 0.015(2) 0.025(3) 0.009(2) 0.007(2) 0.008(2) C52 0.019(3) 0.014(2) 0.016(2) 0.0011(19) 0.005(2) 0.006(2) C53 0.027(3) 0.027(3) 0.045(3) 0.014(3) 0.010(3) 0.015(2) C54 0.023(3) 0.018(2) 0.039(3) 0.011(2) 0.016(2) 0.010(2) C55 0.043(3) 0.029(3) 0.036(3) 0.013(3) 0.018(3) 0.021(3) C56 0.030(3) 0.030(3) 0.054(4) 0.020(3) 0.005(3) 0.019(2) C57 0.020(3) 0.018(2) 0.030(3) 0.010(2) 0.009(2) 0.012(2) C58 0.043(3) 0.024(3) 0.046(3) 0.015(3) 0.026(3) 0.019(3) _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 Co1 N3 1.633(4) . ? Co1 N4 1.695(4) . ? Co1 N1 1.955(4) . ? Co1 N2 1.957(4) . ? O1 N3 1.165(5) . ? N1 C2 1.333(5) . ? N1 C6 1.442(5) . ? C1 C2 1.501(6) . ? C2 C3 1.397(6) . ? N2 C4 1.317(5) . ? N2 C18 1.437(5) . ? O2 N4 1.166(5) . ? Co2 N7 1.650(4) . ? Co2 N8 1.707(4) . ? Co2 N5 1.952(4) . ? Co2 N6 1.954(4) . ? C3 C4 1.400(6) . ? O3 N7 1.159(5) . ? C4 C5 1.516(6) . ? O4 N8 1.166(5) . ? N5 C31 1.323(5) . ? N5 C35 1.436(5) . ? C6 C11 1.407(6) . ? C6 C7 1.409(6) . ? N6 C33 1.331(5) . ? N6 C47 1.438(5) . ? C7 C8 1.389(6) . ? C7 C16 1.522(6) . ? C8 C9 1.381(6) . ? C9 C10 1.374(6) . ? C10 C11 1.392(6) . ? C11 C13 1.512(6) . ? C12 C13 1.534(6) . ? C13 C14 1.529(6) . ? C15 C16 1.530(7) . ? C16 C17 1.527(7) . ? C18 C19 1.401(6) . ? C18 C23 1.416(6) . ? C19 C20 1.379(6) . ? C19 C28 1.520(6) . ? C20 C21 1.392(6) . ? C21 C22 1.373(6) . ? C22 C23 1.382(6) . ? C23 C25 1.509(6) . ? C24 C25 1.528(6) . ? C25 C26 1.536(6) . ? C27 C28 1.524(7) . ? C28 C29 1.532(6) . ? C30 C31 1.517(6) . ? C31 C32 1.392(6) . ? C32 C33 1.388(6) . ? C33 C34 1.505(6) . ? C35 C40 1.402(6) . ? C35 C36 1.408(6) . ? C36 C37 1.386(6) . ? C36 C45 1.510(6) . ? C37 C38 1.374(6) . ? C38 C39 1.376(6) . ? C39 C40 1.387(6) . ? C40 C42 1.528(6) . ? C41 C42 1.541(6) . ? C42 C43 1.523(6) . ? C44 C45 1.532(6) . ? C45 C46 1.533(6) . ? C47 C48 1.396(6) . ? C47 C52 1.412(6) . ? C48 C49 1.392(6) . ? C48 C57 1.518(6) . ? C49 C50 1.375(6) . ? C50 C51 1.374(6) . ? C51 C52 1.388(6) . ? C52 C54 1.523(6) . ? C53 C54 1.530(7) . ? C54 C55 1.529(6) . ? C56 C57 1.533(6) . ? C57 C58 1.528(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 N3 Co1 N4 110.5(2) . . ? N3 Co1 N1 117.00(18) . . ? N4 Co1 N1 111.65(17) . . ? N3 Co1 N2 112.47(17) . . ? N4 Co1 N2 111.17(16) . . ? N1 Co1 N2 93.03(15) . . ? C2 N1 C6 119.1(4) . . ? C2 N1 Co1 123.5(3) . . ? C6 N1 Co1 117.4(3) . . ? N1 C2 C3 123.3(4) . . ? N1 C2 C1 119.6(4) . . ? C3 C2 C1 117.1(4) . . ? C4 N2 C18 120.3(4) . . ? C4 N2 Co1 124.3(3) . . ? C18 N2 Co1 115.3(3) . . ? N7 Co2 N8 110.23(19) . . ? N7 Co2 N5 111.35(17) . . ? N8 Co2 N5 110.80(17) . . ? N7 Co2 N6 119.42(17) . . ? N8 Co2 N6 110.84(17) . . ? N5 Co2 N6 93.02(15) . . ? O1 N3 Co1 173.0(4) . . ? C2 C3 C4 127.2(4) . . ? O2 N4 Co1 150.1(4) . . ? N2 C4 C3 123.2(4) . . ? N2 C4 C5 120.2(4) . . ? C3 C4 C5 116.7(4) . . ? C31 N5 C35 120.6(4) . . ? C31 N5 Co2 124.3(3) . . ? C35 N5 Co2 115.1(3) . . ? C11 C6 C7 120.4(4) . . ? C11 C6 N1 120.7(4) . . ? C7 C6 N1 118.7(4) . . ? C33 N6 C47 119.1(4) . . ? C33 N6 Co2 123.0(3) . . ? C47 N6 Co2 117.9(3) . . ? C8 C7 C6 118.7(4) . . ? C8 C7 C16 118.7(4) . . ? C6 C7 C16 122.6(4) . . ? O3 N7 Co2 170.0(4) . . ? C9 C8 C7 121.2(4) . . ? O4 N8 Co2 148.0(4) . . ? C10 C9 C8 119.7(4) . . ? C9 C10 C11 121.7(4) . . ? C10 C11 C6 118.2(4) . . ? C10 C11 C13 119.4(4) . . ? C6 C11 C13 122.4(4) . . ? C11 C13 C14 110.8(4) . . ? C11 C13 C12 111.8(4) . . ? C14 C13 C12 110.4(4) . . ? C7 C16 C17 110.2(4) . . ? C7 C16 C15 111.7(4) . . ? C17 C16 C15 109.2(4) . . ? C19 C18 C23 120.8(4) . . ? C19 C18 N2 118.8(4) . . ? C23 C18 N2 120.3(4) . . ? C20 C19 C18 118.4(4) . . ? C20 C19 C28 120.5(4) . . ? C18 C19 C28 121.1(4) . . ? C19 C20 C21 121.8(4) . . ? C22 C21 C20 118.9(4) . . ? C21 C22 C23 122.1(4) . . ? C22 C23 C18 118.0(4) . . ? C22 C23 C25 119.5(4) . . ? C18 C23 C25 122.5(4) . . ? C23 C25 C24 113.0(4) . . ? C23 C25 C26 109.8(4) . . ? C24 C25 C26 109.6(4) . . ? C19 C28 C27 111.3(4) . . ? C19 C28 C29 113.1(4) . . ? C27 C28 C29 109.9(4) . . ? N5 C31 C32 122.9(4) . . ? N5 C31 C30 119.9(4) . . ? C32 C31 C30 117.2(4) . . ? C33 C32 C31 127.3(4) . . ? N6 C33 C32 123.8(4) . . ? N6 C33 C34 118.9(4) . . ? C32 C33 C34 117.3(4) . . ? C40 C35 C36 121.3(4) . . ? C40 C35 N5 118.3(4) . . ? C36 C35 N5 120.2(4) . . ? C37 C36 C35 117.9(4) . . ? C37 C36 C45 118.8(4) . . ? C35 C36 C45 123.4(4) . . ? C38 C37 C36 121.4(4) . . ? C37 C38 C39 120.1(4) . . ? C38 C39 C40 121.1(4) . . ? C39 C40 C35 118.1(4) . . ? C39 C40 C42 120.5(4) . . ? C35 C40 C42 121.4(4) . . ? C43 C42 C40 113.6(4) . . ? C43 C42 C41 110.0(4) . . ? C40 C42 C41 111.9(4) . . ? C36 C45 C44 111.9(4) . . ? C36 C45 C46 110.2(4) . . ? C44 C45 C46 109.7(4) . . ? C48 C47 C52 120.7(4) . . ? C48 C47 N6 120.4(4) . . ? C52 C47 N6 118.9(4) . . ? C49 C48 C47 118.9(4) . . ? C49 C48 C57 119.4(4) . . ? C47 C48 C57 121.7(4) . . ? C50 C49 C48 120.6(4) . . ? C51 C50 C49 120.5(4) . . ? C50 C51 C52 121.1(4) . . ? C51 C52 C47 118.3(4) . . ? C51 C52 C54 119.2(4) . . ? C47 C52 C54 122.5(4) . . ? C52 C54 C55 111.6(4) . . ? C52 C54 C53 110.6(4) . . ? C55 C54 C53 109.6(4) . . ? C48 C57 C58 110.3(4) . . ? C48 C57 C56 111.3(4) . . ? C58 C57 C56 110.7(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.852 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.084 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H41 Br Fe N3 O' _chemical_formula_weight 583.41 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.442(3) _cell_length_b 20.007(5) _cell_length_c 13.102(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.805(4) _cell_angle_gamma 90.00 _cell_volume 2936.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 9216 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 30.44 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6184 _exptl_absorpt_correction_T_max 0.7904 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64961 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 29.57 _reflns_number_total 8235 _reflns_number_gt 6896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0041P)^2^+5.6891P] 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 8235 _refine_ls_number_parameters 354 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.294 _refine_ls_restrained_S_all 1.294 _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 0.12811(3) 0.91979(2) 0.29676(3) 0.01777(10) Uani 1 1 d DU . . Br1 Br 0.16087(6) 1.03760(3) 0.28219(6) 0.02152(16) Uani 0.6676(18) 1 d PDU A 1 N1 N 0.2077(4) 0.8865(2) 0.4220(4) 0.0227(8) Uani 0.6676(18) 1 d PDU A 1 O1 O 0.2736(7) 0.8631(4) 0.5139(6) 0.076(3) Uani 0.6676(18) 1 d PDU A 1 Br1A Br 0.24063(14) 0.86014(8) 0.47572(14) 0.0290(4) Uani 0.3324(18) 1 d PDU A 2 N1A N 0.1545(6) 0.9989(4) 0.2990(7) 0.0212(15) Uani 0.3324(18) 1 d PDU A 2 O1A O 0.1609(17) 1.0568(6) 0.2689(16) 0.085(6) Uani 0.3324(18) 1 d PDU A 2 N2 N -0.0459(2) 0.90521(11) 0.22814(19) 0.0151(4) Uani 1 1 d . A . N3 N 0.1561(2) 0.87652(11) 0.17820(19) 0.0163(4) Uani 1 1 d . A . C1 C 0.1061(3) 0.87536(17) -0.0252(3) 0.0282(7) Uani 1 1 d . A . H1A H 0.1791 0.9002 -0.0111 0.042 Uiso 1 1 calc R . . H1B H 0.0409 0.8909 -0.0960 0.042 Uiso 1 1 calc R . . H1C H 0.1196 0.8276 -0.0313 0.042 Uiso 1 1 calc R . . C2 C 0.0734(3) 0.88664(14) 0.0715(2) 0.0184(5) Uani 1 1 d . . . C3 C -0.0440(3) 0.90528(14) 0.0451(2) 0.0206(6) Uani 1 1 d . A . H3 H -0.0907 0.9186 -0.0312 0.025 Uiso 1 1 calc R . . C4 C -0.1027(2) 0.90714(14) 0.1158(2) 0.0192(5) Uani 1 1 d . . . C5 C -0.2375(3) 0.91022(17) 0.0565(3) 0.0257(6) Uani 1 1 d . A . H5A H -0.2706 0.8841 0.0994 0.039 Uiso 1 1 calc R . . H5B H -0.2657 0.8918 -0.0201 0.039 Uiso 1 1 calc R . . H5C H -0.2635 0.9568 0.0519 0.039 Uiso 1 1 calc R . . C11 C 0.2621(2) 0.83854(14) 0.1964(2) 0.0186(5) Uani 1 1 d . . . C12 C 0.2538(3) 0.76835(15) 0.1953(2) 0.0215(6) Uani 1 1 d . A . C13 C 0.3552(3) 0.73136(16) 0.2119(3) 0.0287(7) Uani 1 1 d . . . H13 H 0.3513 0.6839 0.2107 0.034 Uiso 1 1 calc R A . C14 C 0.4611(3) 0.76251(17) 0.2299(3) 0.0301(7) Uani 1 1 d . A . H14 H 0.5288 0.7365 0.2396 0.036 Uiso 1 1 calc R . . C15 C 0.4685(3) 0.83150(16) 0.2340(3) 0.0267(7) Uani 1 1 d . . . H15 H 0.5424 0.8524 0.2487 0.032 Uiso 1 1 calc R A . C16 C 0.3695(3) 0.87097(15) 0.2168(2) 0.0218(6) Uani 1 1 d . A . C21 C -0.1119(2) 0.90527(14) 0.2960(2) 0.0164(5) Uani 1 1 d . . . C22 C -0.1206(2) 0.84525(14) 0.3476(2) 0.0195(5) Uani 1 1 d . A . C23 C -0.1838(3) 0.84580(15) 0.4127(2) 0.0223(6) Uani 1 1 d . . . H23 H -0.1922 0.8055 0.4469 0.027 Uiso 1 1 calc R A . C24 C -0.2346(3) 0.90399(16) 0.4286(2) 0.0234(6) Uani 1 1 d . A . H24 H -0.2778 0.9034 0.4731 0.028 Uiso 1 1 calc R . . C25 C -0.2226(2) 0.96270(16) 0.3798(2) 0.0214(6) Uani 1 1 d . . . H25 H -0.2568 1.0025 0.3923 0.026 Uiso 1 1 calc R A . C26 C -0.1614(2) 0.96510(14) 0.3125(2) 0.0177(5) Uani 1 1 d . A . C121 C 0.1401(3) 0.73241(15) 0.1796(3) 0.0252(6) Uani 1 1 d . . . H121 H 0.0796 0.7669 0.1743 0.030 Uiso 1 1 calc R A . C122 C 0.0878(3) 0.6903(2) 0.0716(3) 0.0399(9) Uani 1 1 d . A . H12A H 0.0727 0.7189 0.0060 0.060 Uiso 1 1 calc R . . H12B H 0.0127 0.6700 0.0632 0.060 Uiso 1 1 calc R . . H12C H 0.1445 0.6551 0.0764 0.060 Uiso 1 1 calc R . . C123 C 0.1642(4) 0.68831(18) 0.2830(3) 0.0380(8) Uani 1 1 d . A . H12D H 0.2211 0.6531 0.2882 0.057 Uiso 1 1 calc R . . H12E H 0.0893 0.6680 0.2750 0.057 Uiso 1 1 calc R . . H12F H 0.1977 0.7157 0.3519 0.057 Uiso 1 1 calc R . . C161 C 0.3814(3) 0.94638(15) 0.2222(3) 0.0243(6) Uani 1 1 d . . . H161 H 0.2992 0.9659 0.1875 0.029 Uiso 1 1 calc R A . C162 C 0.4440(3) 0.97008(17) 0.3456(3) 0.0326(7) Uani 1 1 d . A . H16A H 0.3998 0.9540 0.3871 0.049 Uiso 1 1 calc R . . H16B H 0.4467 1.0190 0.3477 0.049 Uiso 1 1 calc R . . H16C H 0.5255 0.9523 0.3810 0.049 Uiso 1 1 calc R . . C163 C 0.4481(3) 0.97237(18) 0.1561(3) 0.0349(8) Uani 1 1 d . A . H16D H 0.5314 0.9574 0.1932 0.052 Uiso 1 1 calc R . . H16E H 0.4455 1.0213 0.1543 0.052 Uiso 1 1 calc R . . H16F H 0.4102 0.9550 0.0785 0.052 Uiso 1 1 calc R . . C221 C -0.0672(3) 0.78034(15) 0.3303(3) 0.0237(6) Uani 1 1 d . . . H221 H 0.0027 0.7923 0.3153 0.028 Uiso 1 1 calc R A . C222 C -0.1576(4) 0.74393(18) 0.2253(3) 0.0423(9) Uani 1 1 d . A . H22A H -0.2312 0.7361 0.2335 0.063 Uiso 1 1 calc R . . H22B H -0.1241 0.7010 0.2173 0.063 Uiso 1 1 calc R . . H22C H -0.1753 0.7714 0.1579 0.063 Uiso 1 1 calc R . . C223 C -0.0216(4) 0.73490(18) 0.4336(3) 0.0380(8) Uani 1 1 d . A . H22D H 0.0367 0.7591 0.4994 0.057 Uiso 1 1 calc R . . H22E H 0.0165 0.6955 0.4191 0.057 Uiso 1 1 calc R . . H22F H -0.0886 0.7207 0.4488 0.057 Uiso 1 1 calc R . . C261 C -0.1483(3) 1.03195(14) 0.2647(2) 0.0201(6) Uani 1 1 d . . . H261 H -0.1098 1.0241 0.2127 0.024 Uiso 1 1 calc R A . C262 C -0.2686(3) 1.06663(16) 0.1969(3) 0.0280(7) Uani 1 1 d . A . H26A H -0.3207 1.0372 0.1356 0.042 Uiso 1 1 calc R . . H26B H -0.2557 1.1084 0.1647 0.042 Uiso 1 1 calc R . . H26C H -0.3062 1.0765 0.2472 0.042 Uiso 1 1 calc R . . C263 C -0.0666(3) 1.07817(17) 0.3610(3) 0.0339(7) Uani 1 1 d . A . H26D H -0.1039 1.0876 0.4118 0.051 Uiso 1 1 calc R . . H26E H -0.0545 1.1202 0.3290 0.051 Uiso 1 1 calc R . . H26F H 0.0106 1.0562 0.4038 0.051 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 0.01553(19) 0.0203(2) 0.01615(19) -0.00378(16) 0.00561(15) 0.00148(15) Br1 0.0224(2) 0.0151(3) 0.0287(3) -0.0020(2) 0.0128(2) -0.0016(2) N1 0.0239(19) 0.029(2) 0.0133(18) 0.0070(16) 0.0063(15) 0.0059(16) O1 0.070(5) 0.108(6) 0.031(3) 0.029(4) 0.006(3) 0.030(4) Br1A 0.0300(7) 0.0342(7) 0.0205(8) 0.0022(6) 0.0089(6) 0.0073(5) N1A 0.016(3) 0.016(3) 0.033(4) 0.000(3) 0.012(3) 0.007(3) O1A 0.099(11) 0.038(5) 0.116(12) 0.030(7) 0.047(8) 0.000(7) N2 0.0160(10) 0.0154(11) 0.0152(11) 0.0005(8) 0.0079(9) 0.0017(8) N3 0.0192(11) 0.0143(11) 0.0166(11) 0.0014(8) 0.0089(9) 0.0023(8) C1 0.0299(16) 0.0376(18) 0.0195(15) 0.0034(13) 0.0130(13) 0.0077(14) C2 0.0239(14) 0.0152(13) 0.0174(13) 0.0026(10) 0.0102(11) 0.0017(10) C3 0.0207(13) 0.0242(15) 0.0146(13) 0.0026(11) 0.0054(11) 0.0041(11) C4 0.0195(13) 0.0161(13) 0.0200(14) -0.0001(10) 0.0068(11) 0.0017(10) C5 0.0197(14) 0.0348(17) 0.0192(14) -0.0037(12) 0.0053(11) 0.0033(12) C11 0.0210(13) 0.0209(14) 0.0157(13) 0.0008(10) 0.0096(11) 0.0041(11) C12 0.0257(15) 0.0221(14) 0.0193(14) -0.0004(11) 0.0124(12) 0.0017(11) C13 0.0345(18) 0.0204(15) 0.0355(18) 0.0015(13) 0.0192(15) 0.0054(13) C14 0.0261(16) 0.0319(17) 0.0334(18) 0.0009(14) 0.0140(14) 0.0107(13) C15 0.0195(14) 0.0324(17) 0.0269(16) -0.0005(13) 0.0090(12) 0.0026(12) C16 0.0229(14) 0.0231(14) 0.0192(14) 0.0024(11) 0.0089(11) 0.0035(11) C21 0.0147(12) 0.0207(13) 0.0133(12) -0.0019(10) 0.0056(10) -0.0019(10) C22 0.0188(13) 0.0194(13) 0.0179(13) -0.0012(10) 0.0058(11) -0.0027(10) C23 0.0217(14) 0.0244(15) 0.0208(14) 0.0021(11) 0.0091(11) -0.0067(11) C24 0.0176(13) 0.0365(17) 0.0182(14) 0.0001(12) 0.0096(11) -0.0044(12) C25 0.0180(13) 0.0278(15) 0.0189(14) -0.0019(11) 0.0085(11) 0.0006(11) C26 0.0148(12) 0.0216(14) 0.0146(12) -0.0002(10) 0.0046(10) -0.0015(10) C121 0.0315(16) 0.0177(14) 0.0340(17) -0.0004(12) 0.0214(14) 0.0029(12) C122 0.038(2) 0.040(2) 0.042(2) -0.0114(17) 0.0180(17) -0.0105(16) C123 0.048(2) 0.0283(18) 0.047(2) 0.0113(16) 0.0294(18) 0.0072(16) C161 0.0174(13) 0.0249(15) 0.0281(16) -0.0003(12) 0.0076(12) 0.0000(11) C162 0.0293(17) 0.0305(18) 0.0345(18) -0.0064(14) 0.0106(14) -0.0033(13) C163 0.0255(16) 0.0352(19) 0.041(2) 0.0097(15) 0.0115(15) -0.0005(14) C221 0.0299(16) 0.0197(14) 0.0227(15) -0.0009(11) 0.0126(13) -0.0027(12) C222 0.057(2) 0.0242(17) 0.036(2) -0.0090(15) 0.0107(18) -0.0016(16) C223 0.051(2) 0.0320(19) 0.0357(19) 0.0103(15) 0.0234(17) 0.0135(16) C261 0.0214(14) 0.0190(14) 0.0217(14) -0.0004(11) 0.0111(11) 0.0017(11) C262 0.0293(16) 0.0268(16) 0.0317(17) 0.0067(13) 0.0167(14) 0.0083(13) C263 0.0358(18) 0.0256(16) 0.0405(19) -0.0080(15) 0.0168(15) -0.0104(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1A 1.613(8) . ? Fe1 N1 1.644(5) . ? Fe1 N3 1.938(2) . ? Fe1 N2 1.971(2) . ? Fe1 Br1 2.4136(9) . ? Fe1 Br1A 2.4544(17) . ? N1 O1 1.217(6) . ? N1A O1A 1.238(9) . ? N2 C4 1.327(4) . ? N2 C21 1.449(3) . ? N3 C2 1.342(4) . ? N3 C11 1.450(3) . ? C1 C2 1.507(4) . ? C2 C3 1.397(4) . ? C3 C4 1.407(4) . ? C4 C5 1.512(4) . ? C11 C16 1.402(4) . ? C11 C12 1.408(4) . ? C12 C13 1.395(4) . ? C12 C121 1.520(4) . ? C13 C14 1.382(5) . ? C14 C15 1.383(5) . ? C15 C16 1.397(4) . ? C16 C161 1.515(4) . ? C21 C22 1.405(4) . ? C21 C26 1.406(4) . ? C22 C23 1.389(4) . ? C22 C221 1.520(4) . ? C23 C24 1.383(4) . ? C24 C25 1.376(4) . ? C25 C26 1.394(4) . ? C26 C261 1.516(4) . ? C121 C122 1.527(5) . ? C121 C123 1.532(5) . ? C161 C163 1.528(5) . ? C161 C162 1.533(4) . ? C221 C223 1.520(4) . ? C221 C222 1.530(5) . ? C261 C262 1.534(4) . ? C261 C263 1.538(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Fe1 N1 110.5(3) . . ? N1A Fe1 N3 110.3(3) . . ? N1 Fe1 N3 112.24(16) . . ? N1A Fe1 N2 109.1(3) . . ? N1 Fe1 N2 117.38(15) . . ? N3 Fe1 N2 96.49(10) . . ? N1A Fe1 Br1 5.0(3) . . ? N1 Fe1 Br1 115.22(15) . . ? N3 Fe1 Br1 106.11(7) . . ? N2 Fe1 Br1 107.35(7) . . ? N1A Fe1 Br1A 115.6(3) . . ? N1 Fe1 Br1A 5.17(15) . . ? N3 Fe1 Br1A 108.77(8) . . ? N2 Fe1 Br1A 114.85(8) . . ? Br1 Fe1 Br1A 120.31(4) . . ? O1 N1 Fe1 175.5(6) . . ? O1A N1A Fe1 162.4(12) . . ? C4 N2 C21 120.6(2) . . ? C4 N2 Fe1 116.76(19) . . ? C21 N2 Fe1 121.57(17) . . ? C2 N3 C11 118.7(2) . . ? C2 N3 Fe1 116.36(18) . . ? C11 N3 Fe1 124.80(18) . . ? N3 C2 C3 122.9(3) . . ? N3 C2 C1 119.2(3) . . ? C3 C2 C1 117.9(3) . . ? C2 C3 C4 129.1(3) . . ? N2 C4 C3 123.4(3) . . ? N2 C4 C5 120.4(3) . . ? C3 C4 C5 116.1(2) . . ? C16 C11 C12 121.5(3) . . ? C16 C11 N3 120.8(2) . . ? C12 C11 N3 117.6(2) . . ? C13 C12 C11 118.1(3) . . ? C13 C12 C121 119.7(3) . . ? C11 C12 C121 122.2(3) . . ? C14 C13 C12 121.1(3) . . ? C13 C14 C15 120.0(3) . . ? C14 C15 C16 121.2(3) . . ? C15 C16 C11 118.0(3) . . ? C15 C16 C161 119.6(3) . . ? C11 C16 C161 122.4(3) . . ? C22 C21 C26 121.5(2) . . ? C22 C21 N2 118.5(2) . . ? C26 C21 N2 119.9(2) . . ? C23 C22 C21 118.1(3) . . ? C23 C22 C221 119.9(3) . . ? C21 C22 C221 121.9(3) . . ? C24 C23 C22 121.1(3) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 C26 121.5(3) . . ? C25 C26 C21 117.7(3) . . ? C25 C26 C261 118.6(3) . . ? C21 C26 C261 123.6(2) . . ? C12 C121 C122 112.4(3) . . ? C12 C121 C123 109.9(3) . . ? C122 C121 C123 110.0(3) . . ? C16 C161 C163 112.2(3) . . ? C16 C161 C162 110.6(3) . . ? C163 C161 C162 109.9(3) . . ? C223 C221 C22 113.3(3) . . ? C223 C221 C222 111.0(3) . . ? C22 C221 C222 110.1(3) . . ? C26 C261 C262 112.6(2) . . ? C26 C261 C263 110.0(2) . . ? C262 C261 C263 109.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.466 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.081 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 Br Fe N2 O' _chemical_formula_weight 625.50 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1792(6) _cell_length_b 14.7884(8) _cell_length_c 21.7305(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.3570(10) _cell_angle_gamma 90.00 _cell_volume 3265.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9789 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.45 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5476 _exptl_absorpt_correction_T_max 0.7259 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 52989 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5786 _reflns_number_gt 5567 _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^)+(0.0000P)^2^+10.5354P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 5786 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.265 _refine_ls_restrained_S_all 1.265 _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 Br1 Br 0.60812(4) 0.33565(3) 0.249002(19) 0.02790(11) Uani 1 1 d . . . Fe1 Fe 0.84057(5) 0.36812(3) 0.25216(2) 0.01671(12) Uani 1 1 d . . . N2 N 0.9245(3) 0.43480(19) 0.32417(13) 0.0179(6) Uani 1 1 d . . . O1 O 0.9089(3) 0.23810(16) 0.24173(12) 0.0254(6) Uani 1 1 d . . . C19 C 0.8222(4) 0.4330(3) 0.08255(17) 0.0242(8) Uani 1 1 d . . . C4 C 0.9516(3) 0.5231(2) 0.31995(16) 0.0196(7) Uani 1 1 d . . . N1 N 0.9163(3) 0.44992(19) 0.18943(13) 0.0173(6) Uani 1 1 d . . . C18 C 0.9260(3) 0.4180(2) 0.12706(16) 0.0197(7) Uani 1 1 d . . . C2 C 0.9472(3) 0.5352(2) 0.20365(16) 0.0197(7) Uani 1 1 d . . . C11 C 0.8689(4) 0.3753(3) 0.42610(17) 0.0246(8) Uani 1 1 d . . . C3 C 0.9524(3) 0.5696(2) 0.26414(16) 0.0205(7) Uani 1 1 d . . . H3A H 0.9570 0.6336 0.2674 0.025 Uiso 1 1 calc R . . C23 C 1.0375(4) 0.3677(3) 0.11277(17) 0.0246(8) Uani 1 1 d . . . C5 C 0.9830(4) 0.5776(3) 0.37790(18) 0.0283(9) Uani 1 1 d . . . H5A H 1.0440 0.5435 0.4057 0.042 Uiso 1 1 calc R . . H5B H 0.9016 0.5895 0.3985 0.042 Uiso 1 1 calc R . . H5C H 1.0236 0.6351 0.3670 0.042 Uiso 1 1 calc R . . C33 C 0.9176(4) 0.1736(3) 0.2923(2) 0.0322(9) Uani 1 1 d . . . H33A H 0.8293 0.1581 0.3060 0.039 Uiso 1 1 calc R . . H33B H 0.9724 0.1974 0.3278 0.039 Uiso 1 1 calc R . . C28 C 1.1501(4) 0.3501(3) 0.16081(18) 0.0303(9) Uani 1 1 d . . . H28A H 1.1102 0.3386 0.2011 0.036 Uiso 1 1 calc R . . C25 C 0.7001(4) 0.4866(3) 0.09587(18) 0.0295(9) Uani 1 1 d . . . H25A H 0.7087 0.5068 0.1399 0.035 Uiso 1 1 calc R . . C6 C 0.9609(4) 0.3882(2) 0.38098(16) 0.0218(8) Uani 1 1 d . . . C1 C 0.9829(4) 0.6008(3) 0.15412(18) 0.0294(9) Uani 1 1 d . . . H1A H 0.9155 0.5989 0.1200 0.044 Uiso 1 1 calc R . . H1B H 1.0683 0.5840 0.1389 0.044 Uiso 1 1 calc R . . H1C H 0.9881 0.6621 0.1713 0.044 Uiso 1 1 calc R . . C7 C 1.0896(4) 0.3524(3) 0.38857(17) 0.0289(9) Uani 1 1 d . . . C22 C 1.0431(4) 0.3341(3) 0.05312(18) 0.0338(9) Uani 1 1 d . . . H22A H 1.1183 0.3007 0.0425 0.041 Uiso 1 1 calc R . . C26 C 0.5760(4) 0.4284(4) 0.0872(2) 0.0413(11) Uani 1 1 d . . . H26A H 0.5855 0.3745 0.1133 0.062 Uiso 1 1 calc R . . H26B H 0.5636 0.4101 0.0439 0.062 Uiso 1 1 calc R . . H26C H 0.4996 0.4634 0.0988 0.062 Uiso 1 1 calc R . . C13 C 0.7309(4) 0.4114(3) 0.41939(18) 0.0319(9) Uani 1 1 d . . . H13A H 0.7193 0.4425 0.3786 0.038 Uiso 1 1 calc R . . C16 C 1.1899(4) 0.3655(3) 0.33968(19) 0.0382(11) Uani 1 1 d . . . H16A H 1.1397 0.3796 0.2999 0.046 Uiso 1 1 calc R . . C32 C 0.9822(5) 0.0923(3) 0.2635(2) 0.0433(12) Uani 1 1 d . . . H32A H 0.9636 0.0360 0.2861 0.052 Uiso 1 1 calc R . . H32B H 1.0786 0.1005 0.2629 0.052 Uiso 1 1 calc R . . C8 C 1.1248(5) 0.3059(3) 0.44269(19) 0.0380(11) Uani 1 1 d . . . H8A H 1.2115 0.2827 0.4489 0.046 Uiso 1 1 calc R . . C21 C 0.9413(4) 0.3483(3) 0.00893(18) 0.0371(10) Uani 1 1 d . . . H21A H 0.9465 0.3242 -0.0314 0.044 Uiso 1 1 calc R . . C10 C 0.9104(5) 0.3266(3) 0.47923(18) 0.0342(10) Uani 1 1 d . . . H10A H 0.8501 0.3167 0.5103 0.041 Uiso 1 1 calc R . . C30 C 0.8730(5) 0.1869(3) 0.1858(2) 0.0373(10) Uani 1 1 d . . . H30A H 0.9172 0.2122 0.1503 0.045 Uiso 1 1 calc R . . H30B H 0.7767 0.1889 0.1766 0.045 Uiso 1 1 calc R . . C20 C 0.8333(4) 0.3970(3) 0.02357(18) 0.0304(9) Uani 1 1 d . . . H20A H 0.7642 0.4067 -0.0070 0.037 Uiso 1 1 calc R . . C12 C 0.6300(5) 0.3347(4) 0.4204(2) 0.0532(14) Uani 1 1 d . . . H12A H 0.6468 0.2909 0.3879 0.080 Uiso 1 1 calc R . . H12B H 0.5411 0.3595 0.4133 0.080 Uiso 1 1 calc R . . H12C H 0.6374 0.3045 0.4606 0.080 Uiso 1 1 calc R . . C29 C 1.2403(4) 0.4323(3) 0.1694(2) 0.0439(12) Uani 1 1 d . . . H29A H 1.1878 0.4856 0.1787 0.066 Uiso 1 1 calc R . . H29B H 1.2855 0.4429 0.1315 0.066 Uiso 1 1 calc R . . H29C H 1.3055 0.4211 0.2035 0.066 Uiso 1 1 calc R . . C9 C 1.0363(5) 0.2931(3) 0.4874(2) 0.0399(11) Uani 1 1 d . . . H9A H 1.0621 0.2609 0.5240 0.048 Uiso 1 1 calc R . . C31 C 0.9180(6) 0.0907(3) 0.1985(3) 0.0533(14) Uani 1 1 d . . . H31A H 0.9819 0.0715 0.1684 0.064 Uiso 1 1 calc R . . H31B H 0.8422 0.0486 0.1959 0.064 Uiso 1 1 calc R . . C15 C 1.2818(5) 0.4445(3) 0.3545(3) 0.0526(13) Uani 1 1 d . . . H15A H 1.2298 0.4992 0.3607 0.079 Uiso 1 1 calc R . . H15B H 1.3387 0.4540 0.3202 0.079 Uiso 1 1 calc R . . H15C H 1.3361 0.4312 0.3921 0.079 Uiso 1 1 calc R . . C24 C 0.6846(5) 0.5711(3) 0.0550(2) 0.0493(13) Uani 1 1 d . . . H24A H 0.7637 0.6087 0.0607 0.074 Uiso 1 1 calc R . . H24B H 0.6077 0.6057 0.0666 0.074 Uiso 1 1 calc R . . H24C H 0.6725 0.5528 0.0117 0.074 Uiso 1 1 calc R . . C27 C 1.2339(5) 0.2672(4) 0.1465(2) 0.0534(14) Uani 1 1 d . . . H27A H 1.1770 0.2140 0.1412 0.080 Uiso 1 1 calc R . . H27B H 1.2993 0.2567 0.1807 0.080 Uiso 1 1 calc R . . H27C H 1.2790 0.2780 0.1086 0.080 Uiso 1 1 calc R . . C17 C 1.2695(4) 0.2795(3) 0.3297(2) 0.0475(13) Uani 1 1 d . . . H17A H 1.2094 0.2291 0.3199 0.071 Uiso 1 1 calc R . . H17B H 1.3234 0.2654 0.3674 0.071 Uiso 1 1 calc R . . H17C H 1.3267 0.2888 0.2956 0.071 Uiso 1 1 calc R . . C14 C 0.7041(5) 0.4811(4) 0.4701(2) 0.0560(14) Uani 1 1 d . . . H14A H 0.7684 0.5303 0.4691 0.084 Uiso 1 1 calc R . . H14B H 0.7118 0.4515 0.5105 0.084 Uiso 1 1 calc R . . H14C H 0.6151 0.5057 0.4629 0.084 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 Br1 0.02083(19) 0.02256(19) 0.0402(2) 0.00103(16) 0.00057(16) -0.00428(15) Fe1 0.0191(3) 0.0134(2) 0.0176(2) -0.00014(19) 0.00057(19) -0.00209(19) N2 0.0204(15) 0.0175(15) 0.0155(14) -0.0006(12) 0.0003(12) 0.0015(12) O1 0.0286(14) 0.0163(13) 0.0320(15) -0.0018(11) 0.0061(11) -0.0010(11) C19 0.027(2) 0.026(2) 0.0198(18) 0.0029(15) 0.0011(15) -0.0030(16) C4 0.0173(17) 0.0180(18) 0.0234(18) -0.0042(14) 0.0007(14) 0.0003(14) N1 0.0166(14) 0.0185(15) 0.0168(14) 0.0003(12) 0.0002(11) 0.0001(12) C18 0.0203(18) 0.0202(18) 0.0191(17) 0.0013(14) 0.0052(14) -0.0036(14) C2 0.0166(17) 0.0171(17) 0.0252(19) 0.0031(15) -0.0010(14) -0.0004(14) C11 0.032(2) 0.0213(19) 0.0202(18) -0.0027(15) 0.0006(15) -0.0075(16) C3 0.0228(18) 0.0129(16) 0.0260(19) -0.0006(14) 0.0024(15) -0.0001(14) C23 0.0228(19) 0.030(2) 0.0214(18) 0.0015(16) 0.0053(15) -0.0019(16) C5 0.037(2) 0.0209(19) 0.027(2) -0.0056(16) 0.0021(17) -0.0026(17) C33 0.038(2) 0.0185(19) 0.041(2) 0.0088(17) 0.0026(18) 0.0011(17) C28 0.023(2) 0.041(2) 0.026(2) -0.0039(18) 0.0020(16) 0.0059(18) C25 0.025(2) 0.037(2) 0.025(2) -0.0037(17) -0.0069(16) 0.0043(17) C6 0.032(2) 0.0152(17) 0.0176(17) -0.0014(14) -0.0047(15) -0.0023(15) C1 0.034(2) 0.025(2) 0.029(2) 0.0057(17) 0.0004(17) -0.0089(17) C7 0.036(2) 0.025(2) 0.024(2) -0.0064(16) -0.0079(16) 0.0076(17) C22 0.032(2) 0.044(2) 0.027(2) -0.0034(19) 0.0080(17) 0.006(2) C26 0.024(2) 0.065(3) 0.034(2) -0.008(2) -0.0019(18) -0.002(2) C13 0.030(2) 0.042(2) 0.025(2) 0.0023(18) 0.0075(17) -0.0098(19) C16 0.032(2) 0.054(3) 0.028(2) -0.004(2) -0.0058(18) 0.021(2) C32 0.038(3) 0.017(2) 0.075(3) -0.004(2) 0.002(2) 0.0054(18) C8 0.050(3) 0.032(2) 0.031(2) -0.0057(18) -0.011(2) 0.015(2) C21 0.044(3) 0.051(3) 0.0173(19) -0.0042(18) 0.0055(17) 0.002(2) C10 0.055(3) 0.027(2) 0.0203(19) -0.0003(16) 0.0012(18) -0.015(2) C30 0.053(3) 0.023(2) 0.037(2) -0.0112(18) 0.011(2) -0.0039(19) C20 0.028(2) 0.041(2) 0.0220(19) 0.0018(17) -0.0024(16) -0.0013(18) C12 0.043(3) 0.074(4) 0.042(3) 0.015(3) -0.002(2) -0.029(3) C29 0.019(2) 0.057(3) 0.055(3) 0.003(2) 0.000(2) 0.000(2) C9 0.064(3) 0.026(2) 0.028(2) 0.0039(18) -0.013(2) 0.001(2) C31 0.070(4) 0.026(2) 0.065(3) -0.012(2) 0.009(3) 0.007(2) C15 0.056(3) 0.039(3) 0.065(3) -0.001(2) 0.018(3) 0.005(2) C24 0.053(3) 0.041(3) 0.051(3) 0.004(2) -0.018(2) 0.014(2) C27 0.048(3) 0.062(3) 0.049(3) -0.015(3) -0.009(2) 0.024(3) C17 0.028(2) 0.049(3) 0.064(3) -0.021(3) -0.004(2) 0.011(2) C14 0.044(3) 0.072(4) 0.053(3) -0.015(3) 0.016(2) 0.002(3) _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 Br1 Fe1 2.4114(6) . ? Fe1 N2 1.999(3) . ? Fe1 N1 2.010(3) . ? Fe1 O1 2.062(3) . ? N2 C4 1.339(5) . ? N2 C6 1.443(4) . ? O1 C33 1.453(5) . ? O1 C30 1.460(5) . ? C19 C20 1.398(5) . ? C19 C18 1.408(5) . ? C19 C25 1.517(5) . ? C4 C3 1.394(5) . ? C4 C5 1.513(5) . ? N1 C2 1.332(5) . ? N1 C18 1.444(4) . ? C18 C23 1.407(5) . ? C2 C3 1.408(5) . ? C2 C1 1.509(5) . ? C11 C10 1.404(5) . ? C11 C6 1.408(5) . ? C11 C13 1.503(6) . ? C23 C22 1.393(5) . ? C23 C28 1.527(5) . ? C33 C32 1.522(6) . ? C28 C29 1.529(6) . ? C28 C27 1.536(6) . ? C25 C26 1.531(6) . ? C25 C24 1.535(6) . ? C6 C7 1.414(5) . ? C7 C8 1.391(6) . ? C7 C16 1.528(6) . ? C22 C21 1.387(6) . ? C13 C12 1.532(6) . ? C13 C14 1.544(6) . ? C16 C15 1.519(7) . ? C16 C17 1.531(6) . ? C32 C31 1.522(7) . ? C8 C9 1.376(7) . ? C21 C20 1.368(6) . ? C10 C9 1.376(6) . ? C30 C31 1.515(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 N2 Fe1 N1 94.06(12) . . ? N2 Fe1 O1 114.51(11) . . ? N1 Fe1 O1 109.98(11) . . ? N2 Fe1 Br1 119.62(9) . . ? N1 Fe1 Br1 121.01(8) . . ? O1 Fe1 Br1 98.50(7) . . ? C4 N2 C6 118.7(3) . . ? C4 N2 Fe1 120.5(2) . . ? C6 N2 Fe1 120.7(2) . . ? C33 O1 C30 106.8(3) . . ? C33 O1 Fe1 122.3(2) . . ? C30 O1 Fe1 120.4(2) . . ? C20 C19 C18 118.2(4) . . ? C20 C19 C25 119.0(3) . . ? C18 C19 C25 122.8(3) . . ? N2 C4 C3 123.5(3) . . ? N2 C4 C5 119.8(3) . . ? C3 C4 C5 116.7(3) . . ? C2 N1 C18 119.9(3) . . ? C2 N1 Fe1 120.5(2) . . ? C18 N1 Fe1 119.4(2) . . ? C23 C18 C19 121.0(3) . . ? C23 C18 N1 118.7(3) . . ? C19 C18 N1 120.2(3) . . ? N1 C2 C3 123.6(3) . . ? N1 C2 C1 120.5(3) . . ? C3 C2 C1 115.9(3) . . ? C10 C11 C6 117.5(4) . . ? C10 C11 C13 119.8(4) . . ? C6 C11 C13 122.7(3) . . ? C4 C3 C2 129.2(3) . . ? C22 C23 C18 118.2(3) . . ? C22 C23 C28 120.3(3) . . ? C18 C23 C28 121.5(3) . . ? O1 C33 C32 102.5(3) . . ? C23 C28 C29 111.6(4) . . ? C23 C28 C27 113.7(3) . . ? C29 C28 C27 108.8(4) . . ? C19 C25 C26 111.2(3) . . ? C19 C25 C24 111.9(4) . . ? C26 C25 C24 109.3(4) . . ? C11 C6 C7 121.2(3) . . ? C11 C6 N2 120.8(3) . . ? C7 C6 N2 117.9(3) . . ? C8 C7 C6 118.3(4) . . ? C8 C7 C16 120.1(4) . . ? C6 C7 C16 121.6(3) . . ? C21 C22 C23 121.4(4) . . ? C11 C13 C12 111.1(4) . . ? C11 C13 C14 111.8(4) . . ? C12 C13 C14 109.7(4) . . ? C15 C16 C7 112.2(4) . . ? C15 C16 C17 110.1(4) . . ? C7 C16 C17 112.0(4) . . ? C33 C32 C31 102.8(4) . . ? C9 C8 C7 121.2(4) . . ? C20 C21 C22 119.8(4) . . ? C9 C10 C11 121.6(4) . . ? O1 C30 C31 106.2(4) . . ? C21 C20 C19 121.5(4) . . ? C10 C9 C8 120.1(4) . . ? C30 C31 C32 105.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.936 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.084 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H41 Br2 Fe N2' _chemical_formula_weight 633.31 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5714(10) _cell_length_b 19.9181(16) _cell_length_c 13.2247(11) _cell_angle_alpha 90.00 _cell_angle_beta 116.9340(10) _cell_angle_gamma 90.00 _cell_volume 2952.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9799 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.30 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method ? _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 3.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5105 _exptl_absorpt_correction_T_max 0.6600 _exptl_absorpt_process_details SADABS _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 '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 52094 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.33 _reflns_number_total 5987 _reflns_number_gt 5497 _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^)+(0.0267P)^2^+1.6140P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 5987 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Br1 Br 0.335753(14) -0.034367(7) 0.714565(14) 0.02019(5) Uani 1 1 d . . . Fe1 Fe 0.364064(19) 0.081219(10) 0.703310(18) 0.01301(6) Uani 1 1 d . . . N1 N 0.33756(12) 0.12414(6) 0.82216(11) 0.0141(3) Uani 1 1 d . . . C1 C 0.38995(16) 0.12268(9) 1.02552(15) 0.0247(4) Uani 1 1 d . . . H1A H 0.3758 0.1705 1.0324 0.037 Uiso 1 1 calc R . . H1B H 0.4562 0.1069 1.0962 0.037 Uiso 1 1 calc R . . H1C H 0.3178 0.0971 1.0107 0.037 Uiso 1 1 calc R . . Br2 Br 0.253523(15) 0.130412(8) 0.527345(14) 0.02194(5) Uani 1 1 d . . . N2 N 0.53797(11) 0.09632(6) 0.77366(11) 0.0142(3) Uani 1 1 d . . . C2 C 0.42084(15) 0.11280(8) 0.92895(13) 0.0174(3) Uani 1 1 d . . . C3 C 0.53805(15) 0.09385(8) 0.95611(14) 0.0191(3) Uani 1 1 d . . . H3 H 0.5850 0.0794 1.0321 0.023 Uiso 1 1 calc R . . C4 C 0.59622(14) 0.09318(8) 0.88645(13) 0.0168(3) Uani 1 1 d . . . C5 C 0.73061(15) 0.09018(9) 0.94689(14) 0.0238(4) Uani 1 1 d . . . H5A H 0.7567 0.0435 0.9503 0.036 Uiso 1 1 calc R . . H5B H 0.7593 0.1078 1.0240 0.036 Uiso 1 1 calc R . . H5C H 0.7632 0.1173 0.9056 0.036 Uiso 1 1 calc R . . C6 C 0.23241(14) 0.16214(8) 0.80423(13) 0.0161(3) Uani 1 1 d . . . C7 C 0.12547(15) 0.12946(8) 0.78388(14) 0.0186(3) Uani 1 1 d . . . C8 C 0.02765(15) 0.16910(9) 0.76829(15) 0.0239(4) Uani 1 1 d . . . H8 H -0.0459 0.1481 0.7534 0.029 Uiso 1 1 calc R . . C9 C 0.03584(16) 0.23827(9) 0.77421(16) 0.0263(4) Uani 1 1 d . . . H9 H -0.0312 0.2643 0.7652 0.032 Uiso 1 1 calc R . . C10 C 0.14142(16) 0.26976(9) 0.79321(15) 0.0246(4) Uani 1 1 d . . . H10 H 0.1459 0.3174 0.7964 0.030 Uiso 1 1 calc R . . C11 C 0.24146(15) 0.23256(8) 0.80773(14) 0.0190(3) Uani 1 1 d . . . C12 C 0.32907(18) 0.31316(9) 0.72065(17) 0.0309(4) Uani 1 1 d . . . H12A H 0.2975 0.2852 0.6522 0.046 Uiso 1 1 calc R . . H12B H 0.4032 0.3347 0.7304 0.046 Uiso 1 1 calc R . . H12C H 0.2704 0.3477 0.7132 0.046 Uiso 1 1 calc R . . C13 C 0.35429(16) 0.26915(8) 0.82411(15) 0.0229(4) Uani 1 1 d . . . H13 H 0.4148 0.2347 0.8304 0.028 Uiso 1 1 calc R . . C14 C 0.40719(18) 0.31149(10) 0.93223(17) 0.0323(4) Uani 1 1 d . . . H14A H 0.3512 0.3473 0.9262 0.048 Uiso 1 1 calc R . . H14B H 0.4826 0.3314 0.9422 0.048 Uiso 1 1 calc R . . H14C H 0.4217 0.2830 0.9976 0.048 Uiso 1 1 calc R . . C15 C 0.04994(17) 0.02697(9) 0.84432(17) 0.0298(4) Uani 1 1 d . . . H15A H 0.0924 0.0427 0.9229 0.045 Uiso 1 1 calc R . . H15B H 0.0497 -0.0222 0.8432 0.045 Uiso 1 1 calc R . . H15C H -0.0324 0.0435 0.8104 0.045 Uiso 1 1 calc R . . C16 C 0.11255(15) 0.05338(8) 0.77646(15) 0.0218(4) Uani 1 1 d . . . H16 H 0.1943 0.0334 0.8092 0.026 Uiso 1 1 calc R . . C17 C 0.04454(16) 0.03070(9) 0.65206(16) 0.0274(4) Uani 1 1 d . . . H17A H -0.0365 0.0492 0.6186 0.041 Uiso 1 1 calc R . . H17B H 0.0406 -0.0184 0.6487 0.041 Uiso 1 1 calc R . . H17C H 0.0862 0.0469 0.6096 0.041 Uiso 1 1 calc R . . C18 C 0.60343(13) 0.09788(8) 0.70729(13) 0.0150(3) Uani 1 1 d . . . C19 C 0.61023(14) 0.15924(8) 0.65727(13) 0.0169(3) Uani 1 1 d . . . C20 C 0.67336(15) 0.16014(8) 0.59357(14) 0.0199(3) Uani 1 1 d . . . H20 H 0.6806 0.2011 0.5604 0.024 Uiso 1 1 calc R . . C21 C 0.72555(15) 0.10275(9) 0.57780(14) 0.0214(3) Uani 1 1 d . . . H21 H 0.7682 0.1045 0.5342 0.026 Uiso 1 1 calc R . . C22 C 0.71582(14) 0.04290(8) 0.62523(14) 0.0193(3) Uani 1 1 d . . . H22 H 0.7512 0.0036 0.6129 0.023 Uiso 1 1 calc R . . C23 C 0.65507(14) 0.03879(8) 0.69097(13) 0.0164(3) Uani 1 1 d . . . C24 C 0.56513(17) -0.07595(9) 0.63996(16) 0.0270(4) Uani 1 1 d . . . H24A H 0.4875 -0.0545 0.5958 0.040 Uiso 1 1 calc R . . H24B H 0.5539 -0.1185 0.6712 0.040 Uiso 1 1 calc R . . H24C H 0.6030 -0.0846 0.5908 0.040 Uiso 1 1 calc R . . C25 C 0.64470(15) -0.02955(8) 0.73688(15) 0.0193(3) Uani 1 1 d . . . H25 H 0.6067 -0.0232 0.7882 0.023 Uiso 1 1 calc R . . C26 C 0.76694(16) -0.06301(9) 0.80531(16) 0.0273(4) Uani 1 1 d . . . H26A H 0.8028 -0.0731 0.7549 0.041 Uiso 1 1 calc R . . H26B H 0.7567 -0.1047 0.8392 0.041 Uiso 1 1 calc R . . H26C H 0.8193 -0.0325 0.8654 0.041 Uiso 1 1 calc R . . C27 C 0.50886(18) 0.26968(9) 0.57151(17) 0.0309(4) Uani 1 1 d . . . H27A H 0.5753 0.2849 0.5576 0.046 Uiso 1 1 calc R . . H27B H 0.4696 0.3087 0.5852 0.046 Uiso 1 1 calc R . . H27C H 0.4513 0.2450 0.5051 0.046 Uiso 1 1 calc R . . C28 C 0.55639(16) 0.22369(8) 0.67532(14) 0.0208(3) Uani 1 1 d . . . H28 H 0.4876 0.2111 0.6899 0.025 Uiso 1 1 calc R . . C29 C 0.64742(19) 0.26069(10) 0.78009(17) 0.0362(5) Uani 1 1 d . . . H29A H 0.6705 0.2321 0.8471 0.054 Uiso 1 1 calc R . . H29B H 0.6120 0.3024 0.7903 0.054 Uiso 1 1 calc R . . H29C H 0.7181 0.2713 0.7700 0.054 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 Br1 0.02023(9) 0.01320(8) 0.02884(10) -0.00081(6) 0.01260(7) -0.00062(6) Fe1 0.01287(11) 0.01276(11) 0.01373(11) 0.00016(8) 0.00630(9) 0.00098(8) N1 0.0149(7) 0.0134(6) 0.0153(6) 0.0003(5) 0.0081(5) 0.0007(5) C1 0.0248(9) 0.0346(10) 0.0182(8) 0.0039(7) 0.0128(7) 0.0056(7) Br2 0.02148(9) 0.02690(9) 0.01598(9) 0.00484(6) 0.00722(7) 0.00592(6) N2 0.0144(7) 0.0138(6) 0.0148(6) -0.0001(5) 0.0071(5) 0.0003(5) C2 0.0210(8) 0.0165(7) 0.0165(8) 0.0006(6) 0.0101(7) 0.0002(6) C3 0.0194(8) 0.0222(8) 0.0147(8) 0.0023(6) 0.0070(7) 0.0030(6) C4 0.0178(8) 0.0150(7) 0.0173(8) 0.0005(6) 0.0076(7) 0.0009(6) C5 0.0174(8) 0.0345(10) 0.0176(8) -0.0026(7) 0.0063(7) 0.0022(7) C6 0.0165(8) 0.0189(7) 0.0141(7) 0.0015(6) 0.0080(6) 0.0041(6) C7 0.0177(8) 0.0212(8) 0.0171(8) 0.0004(6) 0.0079(7) 0.0017(6) C8 0.0174(8) 0.0268(9) 0.0282(9) -0.0004(7) 0.0108(7) 0.0020(7) C9 0.0220(9) 0.0261(9) 0.0323(10) 0.0007(7) 0.0136(8) 0.0093(7) C10 0.0288(10) 0.0174(8) 0.0306(10) 0.0001(7) 0.0161(8) 0.0057(7) C11 0.0212(8) 0.0196(8) 0.0185(8) -0.0004(6) 0.0111(7) 0.0021(6) C12 0.0416(11) 0.0223(9) 0.0413(11) 0.0037(8) 0.0295(10) 0.0031(8) C13 0.0266(9) 0.0162(8) 0.0328(10) 0.0005(7) 0.0195(8) 0.0025(7) C14 0.0294(10) 0.0321(10) 0.0371(11) -0.0070(8) 0.0165(9) -0.0065(8) C15 0.0236(10) 0.0312(10) 0.0356(11) 0.0085(8) 0.0142(9) 0.0012(7) C16 0.0169(8) 0.0194(8) 0.0297(9) 0.0022(7) 0.0110(7) 0.0014(6) C17 0.0220(9) 0.0253(9) 0.0329(10) -0.0045(7) 0.0107(8) 0.0001(7) C18 0.0114(7) 0.0188(7) 0.0140(7) -0.0017(6) 0.0051(6) -0.0030(6) C19 0.0146(8) 0.0190(8) 0.0154(8) -0.0016(6) 0.0052(6) -0.0031(6) C20 0.0187(8) 0.0218(8) 0.0201(8) 0.0012(7) 0.0094(7) -0.0043(6) C21 0.0168(8) 0.0309(9) 0.0196(8) -0.0013(7) 0.0109(7) -0.0024(7) C22 0.0153(8) 0.0239(8) 0.0192(8) -0.0021(6) 0.0084(7) 0.0009(6) C23 0.0125(7) 0.0199(8) 0.0153(8) -0.0006(6) 0.0051(6) -0.0006(6) C24 0.0292(10) 0.0244(9) 0.0337(10) -0.0068(7) 0.0198(8) -0.0054(7) C25 0.0198(8) 0.0181(8) 0.0237(9) 0.0017(6) 0.0131(7) 0.0026(6) C26 0.0271(10) 0.0265(9) 0.0330(10) 0.0083(8) 0.0178(8) 0.0088(7) C27 0.0387(11) 0.0264(9) 0.0329(10) 0.0081(8) 0.0209(9) 0.0080(8) C28 0.0261(9) 0.0156(7) 0.0240(9) -0.0001(6) 0.0144(7) -0.0016(6) C29 0.0441(12) 0.0228(9) 0.0341(11) -0.0095(8) 0.0111(10) -0.0029(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 Br1 Fe1 2.3446(3) . ? Fe1 N1 1.9459(13) . ? Fe1 N2 1.9730(13) . ? Fe1 Br2 2.3188(3) . ? N1 C2 1.342(2) . ? N1 C6 1.4466(19) . ? C1 C2 1.507(2) . ? N2 C4 1.333(2) . ? N2 C18 1.450(2) . ? C2 C3 1.401(2) . ? C3 C4 1.412(2) . ? C4 C5 1.508(2) . ? C6 C7 1.406(2) . ? C6 C11 1.406(2) . ? C7 C8 1.396(2) . ? C7 C16 1.523(2) . ? C8 C9 1.381(3) . ? C9 C10 1.384(3) . ? C10 C11 1.396(2) . ? C11 C13 1.520(2) . ? C12 C13 1.532(2) . ? C13 C14 1.529(3) . ? C15 C16 1.530(2) . ? C16 C17 1.539(3) . ? C18 C23 1.407(2) . ? C18 C19 1.411(2) . ? C19 C20 1.395(2) . ? C19 C28 1.520(2) . ? C20 C21 1.380(2) . ? C21 C22 1.378(2) . ? C22 C23 1.396(2) . ? C23 C25 1.520(2) . ? C24 C25 1.528(2) . ? C25 C26 1.538(2) . ? C27 C28 1.529(2) . ? C28 C29 1.528(2) . ? 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 N1 Fe1 N2 96.36(5) . . ? N1 Fe1 Br2 112.39(4) . . ? N2 Fe1 Br2 116.18(4) . . ? N1 Fe1 Br1 107.08(4) . . ? N2 Fe1 Br1 106.70(4) . . ? Br2 Fe1 Br1 116.068(11) . . ? C2 N1 C6 118.67(13) . . ? C2 N1 Fe1 116.01(10) . . ? C6 N1 Fe1 125.14(10) . . ? C4 N2 C18 120.25(13) . . ? C4 N2 Fe1 116.77(10) . . ? C18 N2 Fe1 121.96(10) . . ? N1 C2 C3 122.92(14) . . ? N1 C2 C1 119.48(14) . . ? C3 C2 C1 117.57(15) . . ? C2 C3 C4 129.09(15) . . ? N2 C4 C3 123.06(15) . . ? N2 C4 C5 120.73(14) . . ? C3 C4 C5 116.20(14) . . ? C7 C6 C11 121.62(15) . . ? C7 C6 N1 120.86(14) . . ? C11 C6 N1 117.52(14) . . ? C8 C7 C6 117.95(15) . . ? C8 C7 C16 119.49(15) . . ? C6 C7 C16 122.55(14) . . ? C9 C8 C7 121.18(16) . . ? C8 C9 C10 120.20(16) . . ? C9 C10 C11 120.97(16) . . ? C10 C11 C6 118.06(15) . . ? C10 C11 C13 119.30(15) . . ? C6 C11 C13 122.63(14) . . ? C11 C13 C14 112.35(14) . . ? C11 C13 C12 110.16(15) . . ? C14 C13 C12 110.24(15) . . ? C7 C16 C15 111.87(14) . . ? C7 C16 C17 110.64(14) . . ? C15 C16 C17 109.99(15) . . ? C23 C18 C19 121.51(14) . . ? C23 C18 N2 120.16(14) . . ? C19 C18 N2 118.30(14) . . ? C20 C19 C18 117.80(15) . . ? C20 C19 C28 119.98(14) . . ? C18 C19 C28 122.16(14) . . ? C21 C20 C19 121.34(15) . . ? C22 C21 C20 120.09(15) . . ? C21 C22 C23 121.39(15) . . ? C22 C23 C18 117.84(14) . . ? C22 C23 C25 118.14(14) . . ? C18 C23 C25 123.98(14) . . ? C23 C25 C24 110.39(14) . . ? C23 C25 C26 112.31(14) . . ? C24 C25 C26 109.36(14) . . ? C19 C28 C29 110.23(15) . . ? C19 C28 C27 112.69(14) . . ? C29 C28 C27 110.66(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.609 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.058