# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_compound1 _database_code_depnum_ccdc_archive 'CCDC 891990' #TrackingRef 'web_deposit_cif_file_0_PierreDechambenoit_1346002016.compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H11 Fe N8, 2(C16 H36 N), 6(H2 O)' _chemical_formula_sum 'C54 H95 Fe N10 O6' _chemical_formula_weight 1036.25 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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 21.267(2) _cell_length_b 11.4830(13) _cell_length_c 26.049(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.875(2) _cell_angle_gamma 90.00 _cell_volume 5903.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7845 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.75 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2252 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9408 _exptl_absorpt_correction_T_max 0.9938 _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 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39068 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.38 _reflns_number_total 20672 _reflns_number_gt 12993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'AUTOSTRUCTURE (Bruker)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material 'WINGX (Farrugia)' _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. All non-hydrogens were refined anisotropically. Hydrogen atoms were assigned to ideal positions and refined isotropically using a riding model. Hydrogen atoms belonging to water molecules were not introduced but are taken into account in the compound formula. Butyl chains on the tetrabutylammonium moities were refined using DFIX, DANG and SIMU constrains/restrains. ; _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^)+(0.1405P)^2^+3.4193P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 20672 _refine_ls_number_parameters 1337 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2525 _refine_ls_wR_factor_gt 0.2127 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe2 Fe 0.25210(5) 0.36393(7) 0.37984(4) 0.0455(2) Uani 1 1 d . . . Fe1 Fe 0.30302(5) 0.18763(8) 0.94559(4) 0.0493(3) Uani 1 1 d . . . N3 N 0.3474(3) 0.1106(4) 1.0161(2) 0.0470(13) Uani 1 1 d . . . N10 N 0.4368(3) 0.3959(5) 0.3714(2) 0.0478(14) Uani 1 1 d . . . N6 N 0.3238(3) 0.2600(4) 0.4248(2) 0.0423(13) Uani 1 1 d . . . N7 N 0.3253(3) 0.4178(4) 0.3571(2) 0.0391(11) Uani 1 1 d . . . N13 N 0.2548(4) 0.3868(6) 1.0027(2) 0.0674(18) Uani 1 1 d . . . N16 N 0.2822(3) 0.5579(5) 0.4696(3) 0.0591(16) Uani 1 1 d . . . C35 C 0.3848(3) 0.3601(5) 0.3837(2) 0.0381(13) Uani 1 1 d . . . N1 N 0.2876(3) 0.2891(5) 0.8828(2) 0.0535(15) Uani 1 1 d . . . C34 C 0.3846(3) 0.2692(5) 0.4230(2) 0.0412(14) Uani 1 1 d . . . C41 C 0.3406(3) 0.4984(5) 0.3246(3) 0.0404(14) Uani 1 1 d . . . N4 N 0.4441(3) 0.0887(5) 1.0926(2) 0.0544(15) Uani 1 1 d . . . C33 C 0.4369(3) 0.1977(5) 0.4553(3) 0.0465(15) Uani 1 1 d . . . H33 H 0.4800 0.2032 0.4543 0.056 Uiso 1 1 calc R . . C40 C 0.2998(3) 0.5822(5) 0.2884(3) 0.0462(16) Uani 1 1 d . . . H40 H 0.2542 0.5905 0.2827 0.055 Uiso 1 1 calc R . . N2 N 0.3915(3) 0.2637(5) 0.9698(2) 0.0476(13) Uani 1 1 d . . . N23 N 0.1576(3) 0.8737(5) 0.3470(3) 0.0657(18) Uani 1 1 d . . . N5 N 0.3318(3) 0.4374(6) 0.8471(3) 0.0592(16) Uani 1 1 d . . . N12 N 0.3458(3) -0.0198(6) 0.8892(3) 0.0681(18) Uani 1 1 d . . . C32 C 0.4226(4) 0.1181(6) 0.4893(3) 0.0546(19) Uani 1 1 d . . . H32 H 0.4569 0.0701 0.5121 0.066 Uiso 1 1 calc R . . C59 C 0.2811(3) 0.8054(6) 0.3830(3) 0.0546(17) Uani 1 1 d . . . H59A H 0.2680 0.7377 0.3990 0.066 Uiso 1 1 calc R . . H59B H 0.2794 0.7844 0.3465 0.066 Uiso 1 1 calc R . . C31 C 0.3581(4) 0.1089(6) 0.4898(3) 0.0572(19) Uani 1 1 d . . . H31 H 0.3479 0.0537 0.5117 0.069 Uiso 1 1 calc R . . C37 C 0.4391(4) 0.5569(6) 0.3065(3) 0.0507(16) Uani 1 1 d . . . H37 H 0.4847 0.5478 0.3123 0.061 Uiso 1 1 calc R . . C61 C 0.4043(3) 0.7449(6) 0.4223(3) 0.0500(16) Uani 1 1 d . . . H61A H 0.3958 0.6786 0.4412 0.075 Uiso 1 1 calc R . . H61B H 0.4494 0.7732 0.4421 0.075 Uiso 1 1 calc R . . H61C H 0.3999 0.7228 0.3856 0.075 Uiso 1 1 calc R . . N17 N 0.2077(3) 0.1768(6) 0.2873(2) 0.0608(16) Uani 1 1 d . . . C38 C 0.4006(4) 0.6416(6) 0.2706(3) 0.0607(19) Uani 1 1 d . . . H38 H 0.4204 0.6910 0.2527 0.073 Uiso 1 1 calc R . . N8 N 0.2022(3) 0.2799(5) 0.4173(3) 0.0590(16) Uani 1 1 d . . . C39 C 0.3309(4) 0.6525(6) 0.2613(3) 0.0550(18) Uani 1 1 d . . . H39 H 0.3052 0.7082 0.2364 0.066 Uiso 1 1 calc R . . C58 C 0.2309(3) 0.9048(5) 0.3780(3) 0.0485(17) Uani 1 1 d . . . H58A H 0.2364 0.9304 0.4149 0.058 Uiso 1 1 calc R . . H58B H 0.2425 0.9699 0.3594 0.058 Uiso 1 1 calc R . . C2 C 0.4008(3) 0.3465(7) 0.9376(3) 0.0505(17) Uani 1 1 d . . . C1 C 0.3416(3) 0.3638(7) 0.8877(3) 0.0510(16) Uani 1 1 d . . . C12 C 0.4020(5) -0.0741(7) 1.1372(3) 0.067(2) Uani 1 1 d . . . H12 H 0.4415 -0.0847 1.1682 0.081 Uiso 1 1 calc R . . C60 C 0.3532(3) 0.8406(6) 0.4191(2) 0.0469(16) Uani 1 1 d . . . H60A H 0.3552 0.8581 0.4561 0.056 Uiso 1 1 calc R . . H60B H 0.3654 0.9107 0.4041 0.056 Uiso 1 1 calc R . . C36 C 0.4085(3) 0.4858(5) 0.3335(3) 0.0450(15) Uani 1 1 d . . . N20 N 0.2893(5) 0.3089(6) 0.6380(4) 0.090(3) Uani 1 1 d . . . N15 N 0.1365(3) 0.5199(6) 0.3070(4) 0.083(2) Uani 1 1 d . . . C3 C 0.4617(4) 0.4074(7) 0.9554(3) 0.064(2) Uani 1 1 d . . . H3 H 0.4692 0.4661 0.9338 0.076 Uiso 1 1 calc R . . C7 C 0.4124(4) 0.1448(6) 1.0450(3) 0.0519(17) Uani 1 1 d . . . C13 C 0.3976(4) 0.0118(6) 1.0962(3) 0.0527(17) Uani 1 1 d . . . N21 N 0.2863(5) 0.2809(7) 0.1617(3) 0.096(3) Uani 1 1 d D . . C8 C 0.3372(4) 0.0233(5) 1.0497(3) 0.0470(16) Uani 1 1 d . . . C43 C 0.2714(4) 0.4861(5) 0.4368(3) 0.0526(17) Uani 1 1 d . . . C6 C 0.4383(3) 0.2348(6) 1.0198(3) 0.0502(16) Uani 1 1 d . . . N9 N 0.2056(5) 0.1317(6) 0.4772(3) 0.082(2) Uani 1 1 d . . . C14 C 0.2648(4) 0.4138(8) 0.8121(3) 0.069(2) Uani 1 1 d . . . C5 C 0.4996(4) 0.2925(7) 1.0402(3) 0.0552(17) Uani 1 1 d . . . H5 H 0.5321 0.2754 1.0748 0.066 Uiso 1 1 calc R . . C19 C 0.1716(4) 0.2830(9) 0.8061(3) 0.071(2) Uani 1 1 d . . . H19 H 0.1541 0.2219 0.8202 0.085 Uiso 1 1 calc R . . C87 C 0.3299(5) 0.3031(8) 0.6010(4) 0.090(3) Uani 1 1 d . . . H87A H 0.2993 0.2857 0.5636 0.108 Uiso 1 1 calc R . . H87B H 0.3619 0.2393 0.6133 0.108 Uiso 1 1 calc R . . C17 C 0.1578(5) 0.4242(11) 0.7356(3) 0.089(3) Uani 1 1 d . . . H17 H 0.1297 0.4574 0.7024 0.107 Uiso 1 1 calc R . . C22 C 0.2136(5) 0.1152(7) 0.9218(3) 0.061(2) Uani 1 1 d . . . C29 C 0.2373(4) 0.1921(6) 0.4511(3) 0.0587(19) Uani 1 1 d . . . C11 C 0.3463(5) -0.1390(8) 1.1289(3) 0.072(2) Uani 1 1 d . . . H11 H 0.3484 -0.1970 1.1544 0.086 Uiso 1 1 calc R . . N22 N 0.1611(5) 0.6967(8) 0.8853(3) 0.108(3) Uani 1 1 d D . . C90 C 0.4522(5) 0.4962(8) 0.5620(4) 0.081(2) Uani 1 1 d . . . H90A H 0.4193 0.5528 0.5414 0.121 Uiso 1 1 calc R . . H90B H 0.4807 0.4763 0.5421 0.121 Uiso 1 1 calc R . . H90C H 0.4795 0.5280 0.5974 0.121 Uiso 1 1 calc R . . C30 C 0.3096(4) 0.1835(6) 0.4570(3) 0.0541(17) Uani 1 1 d . . . C9 C 0.2795(5) -0.0439(6) 1.0429(3) 0.066(2) Uani 1 1 d . . . H9 H 0.2394 -0.0354 1.0124 0.079 Uiso 1 1 calc R . . C62 C 0.1337(4) 0.7887(7) 0.3812(5) 0.096(4) Uani 1 1 d . . . H62A H 0.1643 0.7226 0.3911 0.115 Uiso 1 1 calc R . . H62B H 0.0891 0.7600 0.3583 0.115 Uiso 1 1 calc R . . C54 C 0.1457(5) 0.8162(7) 0.2933(4) 0.090(3) Uani 1 1 d . . . H54A H 0.0975 0.8022 0.2751 0.108 Uiso 1 1 calc R . . H54B H 0.1680 0.7409 0.3006 0.108 Uiso 1 1 calc R . . C4 C 0.5102(4) 0.3793(8) 1.0055(3) 0.064(2) Uani 1 1 d . . . H4 H 0.5516 0.4182 1.0172 0.077 Uiso 1 1 calc R . . C88 C 0.3687(5) 0.4141(8) 0.6000(4) 0.081(3) Uani 1 1 d . . . H88A H 0.3943 0.4398 0.6375 0.098 Uiso 1 1 calc R . . H88B H 0.3373 0.4754 0.5810 0.098 Uiso 1 1 calc R . . C20 C 0.2710(4) 0.3125(6) 0.9812(3) 0.0519(17) Uani 1 1 d . . . C91 C 0.2372(6) 0.4089(7) 0.6196(5) 0.092(3) Uani 1 1 d . . . H91A H 0.2101 0.4062 0.6424 0.111 Uiso 1 1 calc R . . H91B H 0.2619 0.4819 0.6275 0.111 Uiso 1 1 calc R . . C15 C 0.2379(4) 0.3223(7) 0.8336(3) 0.062(2) Uani 1 1 d . . . C89 C 0.4168(5) 0.3895(7) 0.5700(4) 0.074(2) Uani 1 1 d . . . H89A H 0.4503 0.3329 0.5911 0.088 Uiso 1 1 calc R . . H89B H 0.3912 0.3556 0.5342 0.088 Uiso 1 1 calc R . . C27 C 0.1410(5) 0.2760(6) 0.4232(5) 0.081(3) Uani 1 1 d . . . C44 C 0.1812(4) 0.4617(6) 0.3339(4) 0.058(2) Uani 1 1 d . . . C10 C 0.2862(5) -0.1233(7) 1.0841(3) 0.070(2) Uani 1 1 d . . . H10 H 0.2488 -0.1682 1.0819 0.084 Uiso 1 1 calc R . . C16 C 0.2252(5) 0.4653(10) 0.7618(3) 0.084(3) Uani 1 1 d . . . H16 H 0.2424 0.5241 0.7462 0.100 Uiso 1 1 calc R . . C53 C 0.1194(4) 0.9896(6) 0.3377(4) 0.070(2) Uani 1 1 d . . . H53A H 0.1269 1.0248 0.3734 0.084 Uiso 1 1 calc R . . H53B H 0.1380 1.0417 0.3177 0.084 Uiso 1 1 calc R . . C55 C 0.1699(5) 0.8819(7) 0.2530(4) 0.094(3) Uani 1 1 d . . . H55A H 0.1482 0.9576 0.2448 0.113 Uiso 1 1 calc R . . H55B H 0.2185 0.8936 0.2695 0.113 Uiso 1 1 calc R . . C95 C 0.2513(5) 0.1949(7) 0.6292(4) 0.086(3) Uani 1 1 d . . . H95A H 0.2838 0.1331 0.6452 0.103 Uiso 1 1 calc R . . H95B H 0.2307 0.1806 0.5897 0.103 Uiso 1 1 calc R . . C18 C 0.1339(5) 0.3363(10) 0.7586(3) 0.083(3) Uani 1 1 d . . . H18 H 0.0893 0.3122 0.7406 0.100 Uiso 1 1 calc R . . C21 C 0.3312(4) 0.0568(7) 0.9099(3) 0.0579(18) Uani 1 1 d . . . C52 C 0.0432(4) 0.9783(7) 0.3057(5) 0.101(4) Uani 1 1 d . . . H52A H 0.0249 0.9177 0.3221 0.121 Uiso 1 1 calc R . . H52B H 0.0346 0.9570 0.2676 0.121 Uiso 1 1 calc R . . C84 C 0.4254(7) 0.2556(10) 0.7839(5) 0.121(4) Uani 1 1 d . . . H84A H 0.4723 0.2300 0.7978 0.146 Uiso 1 1 calc R . . H84B H 0.4238 0.3331 0.7982 0.146 Uiso 1 1 calc R . . C114 C 0.1506(7) 0.6291(11) 0.0649(5) 0.118(4) Uani 1 1 d . . . H11A H 0.1795 0.6342 0.0442 0.176 Uiso 1 1 calc R . . H11B H 0.1384 0.7060 0.0723 0.176 Uiso 1 1 calc R . . H11C H 0.1104 0.5864 0.0440 0.176 Uiso 1 1 calc R . . C26 C 0.0822(5) 0.3460(8) 0.4003(6) 0.107(4) Uani 1 1 d . . . H26 H 0.0807 0.4085 0.3771 0.129 Uiso 1 1 calc R . . C86 C 0.3333(6) 0.3285(8) 0.6983(5) 0.095(3) Uani 1 1 d . . . H86A H 0.3453 0.4103 0.7036 0.114 Uiso 1 1 calc R . . H86B H 0.3070 0.3102 0.7207 0.114 Uiso 1 1 calc R . . C56 C 0.1525(6) 0.8136(9) 0.2020(4) 0.118(5) Uani 1 1 d DU . . H56A H 0.1860 0.7531 0.2064 0.142 Uiso 1 1 calc R . . H56B H 0.1085 0.7773 0.1926 0.142 Uiso 1 1 calc R . . C28 C 0.1430(5) 0.1828(7) 0.4586(5) 0.087(3) Uani 1 1 d . . . C113 C 0.1873(7) 0.5677(10) 0.1186(5) 0.116(4) Uani 1 1 d . . . H11D H 0.2239 0.6168 0.1420 0.139 Uiso 1 1 calc R . . H11E H 0.1563 0.5546 0.1375 0.139 Uiso 1 1 calc R . . C83 C 0.3844(7) 0.1752(10) 0.8023(5) 0.122(4) Uani 1 1 d . . . H83A H 0.3439 0.2140 0.8012 0.183 Uiso 1 1 calc R . . H83B H 0.4100 0.1504 0.8395 0.183 Uiso 1 1 calc R . . H83C H 0.3725 0.1086 0.7783 0.183 Uiso 1 1 calc R . . C92 C 0.1896(7) 0.4106(9) 0.5599(5) 0.109(4) Uani 1 1 d . . . H92A H 0.1729 0.3324 0.5486 0.131 Uiso 1 1 calc R . . H92B H 0.2142 0.4354 0.5370 0.131 Uiso 1 1 calc R . . C104 C 0.3516(7) 0.1149(9) 0.2279(4) 0.103(4) Uani 1 1 d . . . H10A H 0.3898 0.1221 0.2163 0.124 Uiso 1 1 calc R . . H10B H 0.3205 0.0579 0.2042 0.124 Uiso 1 1 calc R . . C99 C 0.3461(6) 0.3005(10) 0.1438(4) 0.104(4) Uani 1 1 d . . . H99A H 0.3288 0.3246 0.1054 0.125 Uiso 1 1 calc R . . H99B H 0.3695 0.2270 0.1462 0.125 Uiso 1 1 calc R . . C111 C 0.2479(8) 0.3901(9) 0.1649(6) 0.126(5) Uani 1 1 d . . . H11F H 0.2788 0.4423 0.1918 0.152 Uiso 1 1 calc R . . H11G H 0.2126 0.3689 0.1784 0.152 Uiso 1 1 calc R . . C96 C 0.1965(6) 0.1863(9) 0.6529(6) 0.109(4) Uani 1 1 d . . . H96A H 0.2162 0.2028 0.6922 0.131 Uiso 1 1 calc R . . H96B H 0.1624 0.2452 0.6358 0.131 Uiso 1 1 calc R . . C105 C 0.3776(7) 0.0711(9) 0.2900(5) 0.102(4) Uani 1 1 d . . . H10C H 0.4102 0.1264 0.3134 0.123 Uiso 1 1 calc R . . H10D H 0.3397 0.0676 0.3021 0.123 Uiso 1 1 calc R . . C24 C 0.0293(8) 0.2247(11) 0.4474(9) 0.173(8) Uani 1 1 d . . . H24 H -0.0101 0.2075 0.4533 0.207 Uiso 1 1 calc R . . C85 C 0.3964(6) 0.2582(9) 0.7182(5) 0.102(3) Uani 1 1 d . . . H85A H 0.4296 0.2922 0.7053 0.123 Uiso 1 1 calc R . . H85B H 0.3869 0.1796 0.7038 0.123 Uiso 1 1 calc R . . C106 C 0.4101(7) -0.0476(11) 0.2962(5) 0.123(5) Uani 1 1 d . . . H10E H 0.3786 -0.1016 0.2718 0.185 Uiso 1 1 calc R . . H10F H 0.4226 -0.0737 0.3337 0.185 Uiso 1 1 calc R . . H10G H 0.4499 -0.0429 0.2871 0.185 Uiso 1 1 calc R . . C93 C 0.1281(7) 0.4947(9) 0.5505(7) 0.124(4) Uani 1 1 d . . . H93A H 0.1449 0.5671 0.5699 0.148 Uiso 1 1 calc R . . H93B H 0.1072 0.5126 0.5113 0.148 Uiso 1 1 calc R . . C74 C 0.1393(6) 0.7724(11) 0.9220(6) 0.147(6) Uani 1 1 d D . . H74A H 0.1482 0.7303 0.9563 0.176 Uiso 1 1 calc R . . H74B H 0.1685 0.8403 0.9309 0.176 Uiso 1 1 calc R . . C63 C 0.1299(6) 0.8422(10) 0.4353(6) 0.111(4) Uani 1 1 d . . . H63A H 0.1722 0.8816 0.4559 0.133 Uiso 1 1 calc R . . H63B H 0.0937 0.8993 0.4257 0.133 Uiso 1 1 calc R . . C23 C 0.0854(8) 0.1549(9) 0.4731(7) 0.132(5) Uani 1 1 d . . . H23 H 0.0859 0.0955 0.4974 0.158 Uiso 1 1 calc R . . C107 C 0.2411(6) 0.1992(11) 0.1183(5) 0.118(4) Uani 1 1 d D . . H10H H 0.2347 0.2317 0.0823 0.142 Uiso 1 1 calc R . . H10I H 0.2652 0.1262 0.1215 0.142 Uiso 1 1 calc R . . C50 C 0.0306(6) 1.1957(10) 0.2767(7) 0.162(7) Uani 1 1 d . . . H50A H 0.0223 1.1715 0.2395 0.243 Uiso 1 1 calc R . . H50B H 0.0781 1.2111 0.2956 0.243 Uiso 1 1 calc R . . H50C H 0.0052 1.2651 0.2761 0.243 Uiso 1 1 calc R . . C79 C 0.1165(7) 0.5893(8) 0.8639(4) 0.140(5) Uani 1 1 d D . . H79A H 0.0721 0.6136 0.8386 0.168 Uiso 1 1 calc R . . H79B H 0.1363 0.5404 0.8436 0.168 Uiso 1 1 calc R . . C51 C 0.0083(4) 1.0973(8) 0.3076(7) 0.134(6) Uani 1 1 d . . . H51A H -0.0404 1.0878 0.2908 0.161 Uiso 1 1 calc R . . H51B H 0.0196 1.1200 0.3458 0.161 Uiso 1 1 calc R . . C103 C 0.3178(7) 0.2255(9) 0.2219(4) 0.106(4) Uani 1 1 d . . . H10J H 0.3500 0.2810 0.2456 0.128 Uiso 1 1 calc R . . H10K H 0.2816 0.2172 0.2357 0.128 Uiso 1 1 calc R . . C97 C 0.1644(7) 0.0750(10) 0.6450(7) 0.124(4) Uani 1 1 d U . . H97A H 0.1961 0.0186 0.6685 0.149 Uiso 1 1 calc R . . H97B H 0.1530 0.0511 0.6069 0.149 Uiso 1 1 calc R . . C25 C 0.0280(6) 0.3176(10) 0.4138(8) 0.150(6) Uani 1 1 d . . . H25 H -0.0112 0.3625 0.3997 0.180 Uiso 1 1 calc R . . C112 C 0.2152(6) 0.4562(11) 0.1102(5) 0.110(4) Uani 1 1 d . . . H11H H 0.2488 0.4696 0.0940 0.132 Uiso 1 1 calc R . . H11I H 0.1792 0.4091 0.0847 0.132 Uiso 1 1 calc R . . C64 C 0.1173(7) 0.7498(13) 0.4704(8) 0.157(7) Uani 1 1 d D . . H64A H 0.0750 0.7103 0.4500 0.189 Uiso 1 1 calc R . . H64B H 0.1535 0.6928 0.4805 0.189 Uiso 1 1 calc R . . C80 C 0.1089(8) 0.5190(10) 0.9110(6) 0.132(5) Uani 1 1 d DU . . H80A H 0.1527 0.5067 0.9403 0.158 Uiso 1 1 calc R . . H80B H 0.0797 0.5592 0.9262 0.158 Uiso 1 1 calc R . . C102 C 0.4856(12) 0.4987(14) 0.1536(11) 0.234(9) Uani 1 1 d DU . . H10L H 0.4948 0.5433 0.1868 0.351 Uiso 1 1 calc R . . H10M H 0.4582 0.5440 0.1223 0.351 Uiso 1 1 calc R . . H10N H 0.5275 0.4788 0.1498 0.351 Uiso 1 1 calc R . . C72 C 0.0584(8) 0.8750(13) 0.9496(10) 0.249(14) Uani 1 1 d D . . H72A H 0.0595 0.8178 0.9774 0.299 Uiso 1 1 calc R . . H72B H 0.0955 0.9288 0.9666 0.299 Uiso 1 1 calc R . . C77 C 0.3531(6) 0.6646(12) 0.9654(9) 0.169(8) Uani 1 1 d D . . H77A H 0.3565 0.5988 0.9432 0.203 Uiso 1 1 calc R . . H77B H 0.3814 0.7267 0.9606 0.203 Uiso 1 1 calc R . . C67 C 0.1641(12) 0.8201(18) 0.7522(8) 0.222(9) Uani 1 1 d DU . . H67A H 0.1938 0.8860 0.7674 0.266 Uiso 1 1 calc R . . H67B H 0.1176 0.8473 0.7388 0.266 Uiso 1 1 calc R . . C75 C 0.2307(6) 0.6493(17) 0.9114(7) 0.194(9) Uani 1 1 d D . . H75A H 0.2264 0.5781 0.9298 0.232 Uiso 1 1 calc R . . H75B H 0.2439 0.6257 0.8810 0.232 Uiso 1 1 calc R . . C109 C 0.1314(7) 0.0982(17) 0.0741(12) 0.291(15) Uani 1 1 d DU . . H10O H 0.1498 0.1061 0.0454 0.350 Uiso 1 1 calc R . . H10P H 0.1419 0.0193 0.0881 0.350 Uiso 1 1 calc R . . C78 C 0.3765(13) 0.632(2) 1.0218(8) 0.219(11) Uani 1 1 d D . . H78A H 0.3653 0.6912 1.0428 0.328 Uiso 1 1 calc R . . H78B H 0.4247 0.6212 1.0356 0.328 Uiso 1 1 calc R . . H78C H 0.3553 0.5598 1.0253 0.328 Uiso 1 1 calc R . . C101 C 0.4520(11) 0.4000(13) 0.1564(11) 0.217(9) Uani 1 1 d DU . . H10Q H 0.4864 0.3447 0.1775 0.261 Uiso 1 1 calc R . . H10R H 0.4330 0.3699 0.1189 0.261 Uiso 1 1 calc R . . C57 C 0.1517(15) 0.8909(19) 0.1608(7) 0.292(14) Uani 1 1 d DU . . H57A H 0.1404 0.8499 0.1264 0.439 Uiso 1 1 calc R . . H57B H 0.1956 0.9260 0.1706 0.439 Uiso 1 1 calc R . . H57C H 0.1186 0.9505 0.1570 0.439 Uiso 1 1 calc R . . C69 C 0.1556(7) 0.7648(11) 0.8395(6) 0.141(5) Uani 1 1 d D . . H69A H 0.1808 0.8356 0.8539 0.169 Uiso 1 1 calc R . . H69B H 0.1083 0.7873 0.8226 0.169 Uiso 1 1 calc R . . C100 C 0.3978(10) 0.3922(13) 0.1783(8) 0.179(8) Uani 1 1 d D . . H10S H 0.3758 0.4673 0.1756 0.215 Uiso 1 1 calc R . . H10T H 0.4164 0.3693 0.2169 0.215 Uiso 1 1 calc R . . C73 C 0.0700(7) 0.8136(12) 0.9033(9) 0.208(11) Uani 1 1 d D . . H73A H 0.0390 0.7484 0.8909 0.249 Uiso 1 1 calc R . . H73B H 0.0614 0.8666 0.8724 0.249 Uiso 1 1 calc R . . C82 C 0.0673(11) 0.3407(14) 0.9321(7) 0.195(8) Uani 1 1 d U . . H82A H 0.1082 0.3011 0.9542 0.292 Uiso 1 1 calc R . . H82B H 0.0321 0.2847 0.9153 0.292 Uiso 1 1 calc R . . H82C H 0.0537 0.3923 0.9551 0.292 Uiso 1 1 calc R . . C94 C 0.0774(10) 0.4484(15) 0.5687(8) 0.170(7) Uani 1 1 d . . . H94A H 0.0603 0.3767 0.5497 0.255 Uiso 1 1 calc R . . H94B H 0.0410 0.5033 0.5610 0.255 Uiso 1 1 calc R . . H94C H 0.0970 0.4340 0.6078 0.255 Uiso 1 1 calc R . . C108 C 0.1738(8) 0.1723(16) 0.1190(11) 0.249(14) Uani 1 1 d D . . H10U H 0.1797 0.1347 0.1539 0.299 Uiso 1 1 calc R . . H10V H 0.1500 0.2450 0.1177 0.299 Uiso 1 1 calc R . . C81 C 0.0797(13) 0.4108(12) 0.8871(7) 0.189(7) Uani 1 1 d U . . H81A H 0.1103 0.3691 0.8737 0.227 Uiso 1 1 calc R . . H81B H 0.0374 0.4239 0.8562 0.227 Uiso 1 1 calc R . . C76 C 0.2833(7) 0.7039(18) 0.9464(9) 0.195(9) Uani 1 1 d D . . H76A H 0.2734 0.7152 0.9796 0.234 Uiso 1 1 calc R . . H76B H 0.2829 0.7808 0.9309 0.234 Uiso 1 1 calc R . . C65 C 0.1139(12) 0.802(2) 0.5197(11) 0.37(3) Uani 1 1 d D . . H65A H 0.1150 0.7421 0.5457 0.554 Uiso 1 1 calc R . . H65B H 0.0727 0.8457 0.5102 0.554 Uiso 1 1 calc R . . H65C H 0.1520 0.8531 0.5359 0.554 Uiso 1 1 calc R . . C98 C 0.1039(9) 0.0743(16) 0.6574(10) 0.207(8) Uani 1 1 d U . . H98A H 0.0863 -0.0035 0.6540 0.310 Uiso 1 1 calc R . . H98B H 0.0706 0.1245 0.6320 0.310 Uiso 1 1 calc R . . H98C H 0.1143 0.1015 0.6945 0.310 Uiso 1 1 calc R . . C68 C 0.1751(12) 0.7274(14) 0.7959(7) 0.186(7) Uani 1 1 d DU . . H68A H 0.1492 0.6587 0.7789 0.223 Uiso 1 1 calc R . . H68B H 0.2226 0.7060 0.8109 0.223 Uiso 1 1 calc R . . C71 C -0.0052(11) 0.939(2) 0.934(2) 0.38(3) Uani 1 1 d D . . H71A H -0.0254 0.9443 0.8929 0.567 Uiso 1 1 d . . . H71B H 0.0020 1.0157 0.9481 0.567 Uiso 1 1 d . . . H71C H -0.0368 0.8984 0.9455 0.567 Uiso 1 1 d . . . C110 C 0.0602(10) 0.099(3) 0.0458(18) 0.363(17) Uani 1 1 d DU . . H11J H 0.0495 0.1655 0.0208 0.544 Uiso 1 1 d . . . H11K H 0.0402 0.1142 0.0733 0.544 Uiso 1 1 d . . . H11L H 0.0455 0.0304 0.0276 0.544 Uiso 1 1 d . . . C66 C 0.1802(14) 0.7638(15) 0.7046(10) 0.247(13) Uani 1 1 d D . . H66A H 0.1738 0.8202 0.6759 0.370 Uiso 1 1 calc R . . H66B H 0.1505 0.6988 0.6900 0.370 Uiso 1 1 calc R . . H66C H 0.2264 0.7374 0.7184 0.370 Uiso 1 1 calc R . . N14 N 0.1615(4) 0.0742(7) 0.9080(3) 0.081(2) Uani 1 1 d . . . C42 C 0.2245(3) 0.2461(6) 0.3210(3) 0.0459(16) Uani 1 1 d . . . O1 O 0.5787(3) 0.1069(4) 1.17079(19) 0.0634(13) Uani 1 1 d . . . O2 O 0.3234(3) 0.7314(5) 0.5509(2) 0.0779(16) Uani 1 1 d . . . O3 O 0.4299(4) 0.5864(6) 0.7245(2) 0.100(2) Uani 1 1 d . . . O4 O 0.3080(4) 0.6742(6) 0.6520(3) 0.109(2) Uani 1 1 d . . . O5 O 0.3488(5) 0.8143(7) 0.8099(3) 0.135(4) Uani 1 1 d . . . O6 O 0.2652(6) 0.9427(6) 0.5495(3) 0.141(4) Uani 1 1 d . . . O7A O 0.0114(3) 0.6358(8) 0.2790(5) 0.093(3) Uani 0.80 1 d P A 1 O8A O 0.5470(4) 0.2734(7) 0.3531(4) 0.051(2) Uani 0.50 1 d P B 1 O9 O 0.0830(7) 1.1767(14) 0.1855(5) 0.098(4) Uani 0.50 1 d P . . O10 O -0.0890(5) 0.9202(10) 0.8024(4) 0.066(3) Uani 0.50 1 d P . . O11 O 0.3742(4) -0.0072(8) 0.6427(5) 0.173(5) Uani 1 1 d . . . O13 O 0.3778(6) -0.1284(9) 0.7138(4) 0.074(3) Uani 0.50 1 d P C 1 O12 O 0.5735(5) 0.3923(9) 0.4325(4) 0.064(3) Uani 0.50 1 d P . . O8B O 0.5009(6) 0.2713(10) 0.2881(5) 0.078(3) Uani 0.50 1 d P D 2 O13B O 0.3017(6) -0.1073(11) 0.7071(5) 0.082(4) Uani 0.50 1 d P E 2 O15 O 0.0274(7) 1.0690(19) 0.8319(6) 0.158(9) Uani 0.50 1 d P . . O7B O 0.0150(16) 0.670(3) 0.230(2) 0.107(13) Uani 0.20 1 d P F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe2 0.0547(6) 0.0289(4) 0.0612(6) -0.0098(5) 0.0312(4) -0.0011(4) Fe1 0.0579(6) 0.0481(5) 0.0523(5) -0.0114(5) 0.0324(4) 0.0024(4) N3 0.058(4) 0.042(3) 0.051(3) -0.012(3) 0.032(3) 0.005(2) N10 0.049(3) 0.045(3) 0.050(3) 0.000(3) 0.019(3) 0.002(2) N6 0.065(4) 0.022(2) 0.051(3) -0.011(2) 0.034(3) -0.002(2) N7 0.045(3) 0.029(2) 0.043(3) -0.007(2) 0.018(2) 0.002(2) N13 0.093(5) 0.066(4) 0.052(3) -0.005(3) 0.037(3) 0.022(4) N16 0.090(5) 0.034(3) 0.070(4) -0.019(3) 0.050(3) 0.000(3) C35 0.045(3) 0.028(3) 0.040(3) -0.002(3) 0.013(3) 0.007(3) N1 0.052(3) 0.057(3) 0.059(4) -0.012(3) 0.030(3) 0.011(3) C34 0.051(4) 0.032(3) 0.041(3) -0.007(3) 0.018(3) -0.001(3) C41 0.047(4) 0.032(3) 0.048(3) 0.001(3) 0.024(3) 0.002(3) N4 0.067(4) 0.061(4) 0.053(3) -0.001(3) 0.043(3) 0.007(3) C33 0.057(4) 0.035(3) 0.050(4) -0.011(3) 0.023(3) -0.001(3) C40 0.054(4) 0.032(3) 0.047(4) -0.003(3) 0.012(3) 0.002(3) N2 0.061(4) 0.044(3) 0.051(3) -0.003(3) 0.036(3) 0.004(3) N23 0.049(3) 0.038(3) 0.090(4) 0.004(4) 0.002(3) -0.011(3) N5 0.061(4) 0.073(4) 0.057(4) 0.004(3) 0.038(3) 0.017(3) N12 0.083(5) 0.070(4) 0.056(4) -0.016(3) 0.032(3) 0.010(4) C32 0.089(6) 0.037(4) 0.036(3) -0.013(3) 0.021(3) 0.001(3) C59 0.054(4) 0.036(3) 0.067(4) 0.003(3) 0.014(3) -0.003(3) C31 0.102(6) 0.036(4) 0.047(4) -0.005(3) 0.042(4) -0.003(4) C37 0.060(4) 0.044(4) 0.059(4) -0.003(3) 0.034(3) 0.002(3) C61 0.049(4) 0.049(4) 0.046(4) 0.004(3) 0.011(3) -0.005(3) N17 0.065(4) 0.051(4) 0.057(3) -0.013(3) 0.011(3) -0.024(3) C38 0.079(6) 0.048(4) 0.063(5) 0.004(4) 0.035(4) -0.002(4) N8 0.074(4) 0.034(3) 0.085(4) -0.019(3) 0.049(3) -0.002(3) C39 0.071(5) 0.041(4) 0.048(4) 0.007(3) 0.016(3) 0.002(3) C58 0.055(4) 0.028(3) 0.051(4) -0.001(3) 0.006(3) -0.013(3) C2 0.044(4) 0.068(5) 0.055(4) -0.004(4) 0.037(3) 0.003(3) C1 0.063(4) 0.054(4) 0.048(4) 0.008(4) 0.035(3) 0.013(4) C12 0.097(6) 0.060(5) 0.058(4) -0.001(4) 0.043(4) 0.006(4) C60 0.057(4) 0.046(4) 0.037(3) -0.002(3) 0.017(3) -0.011(3) C36 0.064(4) 0.032(3) 0.042(3) 0.000(3) 0.023(3) 0.004(3) N20 0.139(7) 0.057(4) 0.123(7) -0.036(4) 0.106(6) -0.015(4) N15 0.051(4) 0.044(3) 0.146(7) -0.009(4) 0.027(4) -0.005(3) C3 0.070(5) 0.076(5) 0.060(5) 0.019(4) 0.042(4) 0.010(4) C7 0.064(5) 0.053(4) 0.055(4) -0.003(3) 0.040(4) 0.009(3) C13 0.076(5) 0.049(4) 0.054(4) -0.003(3) 0.048(4) 0.005(3) N21 0.170(8) 0.069(4) 0.096(5) -0.033(4) 0.106(6) -0.030(5) C8 0.069(5) 0.035(3) 0.056(4) -0.006(3) 0.046(4) 0.003(3) C43 0.072(5) 0.029(3) 0.075(5) 0.000(4) 0.049(4) -0.001(3) C6 0.053(4) 0.061(4) 0.048(4) 0.002(3) 0.032(3) 0.010(3) N9 0.134(7) 0.040(3) 0.118(6) -0.013(4) 0.099(6) -0.014(4) C14 0.075(6) 0.090(6) 0.051(4) 0.001(4) 0.034(4) 0.043(5) C5 0.052(4) 0.064(4) 0.059(4) 0.006(4) 0.032(3) 0.003(3) C19 0.059(5) 0.093(6) 0.062(5) -0.002(5) 0.025(4) 0.018(4) C87 0.113(7) 0.083(6) 0.111(7) -0.046(6) 0.085(6) -0.033(5) C17 0.066(6) 0.151(10) 0.050(5) 0.014(6) 0.021(4) 0.062(6) C22 0.066(6) 0.060(5) 0.071(5) -0.008(4) 0.044(4) 0.006(4) C29 0.089(5) 0.031(3) 0.084(5) -0.014(4) 0.064(4) -0.005(4) C11 0.108(7) 0.053(4) 0.072(5) -0.004(5) 0.054(5) -0.006(5) N22 0.151(8) 0.069(5) 0.080(5) -0.018(5) 0.017(5) 0.022(6) C90 0.083(6) 0.071(5) 0.102(7) -0.013(5) 0.049(5) -0.011(5) C30 0.095(5) 0.025(3) 0.055(4) -0.013(4) 0.044(4) -0.008(4) C9 0.097(6) 0.048(4) 0.062(5) -0.022(4) 0.039(4) -0.010(4) C62 0.038(4) 0.041(4) 0.180(11) 0.035(6) 0.009(5) -0.015(3) C54 0.085(6) 0.033(4) 0.101(7) -0.001(5) -0.024(5) -0.017(4) C4 0.041(4) 0.077(5) 0.076(5) 0.008(5) 0.024(4) -0.014(4) C88 0.100(7) 0.059(5) 0.104(7) -0.020(5) 0.060(6) -0.009(4) C20 0.067(5) 0.053(4) 0.048(4) -0.005(3) 0.036(3) 0.007(3) C91 0.144(9) 0.048(4) 0.131(9) -0.002(5) 0.105(8) -0.004(5) C15 0.070(5) 0.081(5) 0.052(4) -0.002(4) 0.043(4) 0.021(4) C89 0.086(6) 0.062(5) 0.090(6) -0.029(5) 0.051(5) -0.008(4) C27 0.086(6) 0.040(4) 0.151(9) -0.019(5) 0.084(6) -0.008(4) C44 0.046(4) 0.036(3) 0.095(6) -0.019(4) 0.029(4) -0.010(3) C10 0.099(6) 0.057(5) 0.074(5) -0.007(5) 0.054(5) -0.017(4) C16 0.087(7) 0.124(8) 0.051(5) 0.012(5) 0.039(5) 0.042(6) C53 0.051(4) 0.035(3) 0.100(6) 0.018(4) 0.001(4) -0.005(3) C55 0.122(7) 0.048(5) 0.069(5) -0.015(5) -0.014(5) 0.011(5) C95 0.112(7) 0.053(4) 0.122(7) -0.008(6) 0.079(6) -0.007(5) C18 0.072(6) 0.136(9) 0.048(4) 0.027(5) 0.030(4) 0.035(6) C21 0.067(5) 0.052(4) 0.057(4) -0.009(4) 0.027(4) 0.014(3) C52 0.054(5) 0.043(4) 0.169(10) 0.018(6) -0.002(5) -0.015(4) C84 0.186(12) 0.085(7) 0.145(10) 0.035(7) 0.122(10) 0.021(8) C114 0.150(11) 0.110(8) 0.126(10) -0.056(8) 0.089(9) -0.044(8) C26 0.109(7) 0.052(5) 0.207(12) 0.001(7) 0.113(8) 0.008(5) C86 0.124(8) 0.062(5) 0.142(9) -0.024(6) 0.098(8) 0.004(5) C56 0.121(8) 0.076(6) 0.088(7) -0.024(6) -0.040(6) 0.029(6) C28 0.107(7) 0.047(4) 0.151(9) -0.030(6) 0.100(7) -0.016(5) C113 0.182(12) 0.096(8) 0.106(9) -0.051(7) 0.095(9) -0.040(8) C83 0.206(13) 0.086(7) 0.132(9) 0.000(7) 0.130(10) 0.007(8) C92 0.180(12) 0.062(6) 0.123(10) -0.010(6) 0.098(9) -0.023(7) C104 0.180(11) 0.074(6) 0.099(7) -0.041(6) 0.101(8) -0.041(7) C99 0.164(10) 0.098(7) 0.093(7) -0.017(6) 0.097(7) -0.028(7) C111 0.233(15) 0.082(7) 0.137(10) -0.036(7) 0.151(11) -0.026(8) C96 0.135(9) 0.066(5) 0.170(10) -0.009(7) 0.107(8) 0.001(6) C105 0.160(10) 0.072(6) 0.121(8) -0.004(6) 0.104(8) -0.023(6) C24 0.152(12) 0.077(8) 0.39(3) -0.015(11) 0.215(16) -0.006(8) C85 0.142(9) 0.070(6) 0.129(9) -0.025(6) 0.091(8) -0.023(6) C106 0.187(13) 0.102(8) 0.099(8) -0.040(7) 0.075(8) -0.066(9) C93 0.157(11) 0.058(6) 0.180(13) 0.012(8) 0.090(10) 0.007(7) C74 0.103(9) 0.108(9) 0.214(15) -0.107(10) 0.043(9) -0.019(7) C63 0.084(7) 0.079(7) 0.178(11) 0.020(8) 0.059(7) -0.024(5) C23 0.174(13) 0.065(6) 0.225(15) -0.003(8) 0.154(12) -0.014(7) C107 0.133(10) 0.109(9) 0.135(10) -0.049(8) 0.077(8) -0.005(8) C50 0.086(7) 0.070(7) 0.263(18) 0.071(10) -0.014(9) -0.004(6) C79 0.272(17) 0.056(6) 0.085(7) -0.027(6) 0.059(9) -0.003(8) C51 0.042(5) 0.066(6) 0.247(16) 0.043(8) -0.001(7) -0.003(4) C103 0.184(11) 0.086(7) 0.097(7) -0.008(6) 0.109(8) -0.022(7) C97 0.117(9) 0.095(7) 0.211(13) -0.011(8) 0.118(9) -0.024(7) C25 0.102(8) 0.082(7) 0.33(2) -0.003(10) 0.150(12) 0.009(6) C112 0.128(9) 0.116(9) 0.115(9) -0.065(8) 0.078(7) -0.020(7) C64 0.141(11) 0.120(10) 0.29(2) 0.098(12) 0.169(13) 0.038(8) C80 0.201(13) 0.083(7) 0.137(10) 0.025(8) 0.093(10) 0.062(8) C102 0.31(2) 0.104(11) 0.38(3) 0.043(15) 0.24(2) 0.022(13) C72 0.161(14) 0.090(9) 0.59(5) -0.040(18) 0.25(2) -0.005(10) C77 0.081(9) 0.112(11) 0.33(3) -0.089(15) 0.092(12) -0.032(7) C67 0.33(2) 0.217(19) 0.180(15) 0.019(14) 0.170(16) -0.066(18) C75 0.149(15) 0.26(3) 0.131(12) 0.006(15) 0.009(11) 0.044(16) C109 0.093(10) 0.174(15) 0.60(4) -0.22(2) 0.126(18) -0.043(10) C78 0.31(3) 0.22(2) 0.176(17) -0.062(18) 0.15(2) -0.02(2) C101 0.258(19) 0.106(11) 0.39(2) -0.011(14) 0.241(19) -0.056(11) C57 0.51(4) 0.28(3) 0.095(10) -0.001(14) 0.122(16) 0.17(3) C69 0.152(12) 0.089(8) 0.214(17) -0.024(11) 0.106(12) -0.046(8) C100 0.26(2) 0.108(11) 0.240(18) -0.057(12) 0.181(17) -0.089(12) C73 0.105(11) 0.083(8) 0.43(3) -0.069(14) 0.099(15) -0.016(7) C82 0.34(2) 0.130(13) 0.200(15) 0.041(12) 0.196(17) 0.095(14) C94 0.217(19) 0.121(11) 0.206(17) 0.012(12) 0.119(15) 0.032(12) C108 0.167(15) 0.152(15) 0.52(4) -0.17(2) 0.23(2) -0.069(13) C81 0.38(2) 0.085(9) 0.167(13) -0.011(9) 0.171(14) 0.025(12) C76 0.109(12) 0.23(2) 0.27(2) -0.100(19) 0.091(13) -0.047(13) C65 0.23(3) 0.30(4) 0.71(8) 0.23(5) 0.34(4) 0.07(3) C98 0.159(14) 0.138(12) 0.33(2) -0.044(15) 0.094(15) -0.024(11) C68 0.30(2) 0.118(12) 0.192(15) 0.009(11) 0.151(16) -0.029(13) C71 0.19(2) 0.167(19) 0.85(9) -0.01(4) 0.27(4) 0.010(17) C110 0.187(18) 0.26(2) 0.64(4) -0.15(3) 0.15(2) 0.024(18) C66 0.41(4) 0.099(12) 0.32(3) 0.013(16) 0.25(3) -0.006(17) N14 0.071(5) 0.088(5) 0.097(5) -0.019(4) 0.044(4) -0.011(4) C42 0.034(3) 0.040(3) 0.063(4) 0.002(4) 0.017(3) -0.006(3) O1 0.088(4) 0.063(3) 0.052(3) -0.002(2) 0.042(3) -0.012(3) O2 0.101(4) 0.057(3) 0.086(4) -0.030(3) 0.047(3) -0.010(3) O3 0.141(6) 0.107(5) 0.072(4) -0.045(4) 0.063(4) -0.047(4) O4 0.192(7) 0.066(4) 0.076(4) -0.017(4) 0.058(4) -0.028(4) O5 0.193(8) 0.104(5) 0.074(4) -0.026(4) 0.010(4) 0.083(5) O6 0.278(12) 0.052(4) 0.102(5) 0.004(4) 0.080(7) 0.022(5) O7A 0.038(4) 0.094(6) 0.140(8) -0.040(6) 0.025(5) 0.005(4) O8A 0.058(6) 0.041(5) 0.064(6) 0.005(4) 0.036(5) 0.006(4) O9 0.106(9) 0.111(10) 0.079(7) -0.010(8) 0.039(7) -0.016(8) O10 0.074(7) 0.074(7) 0.053(6) 0.006(5) 0.026(5) -0.009(5) O11 0.100(5) 0.144(7) 0.286(12) -0.157(9) 0.084(7) -0.037(5) O13 0.119(9) 0.044(5) 0.077(7) -0.006(6) 0.056(6) 0.000(6) O12 0.054(6) 0.068(7) 0.068(6) 0.002(5) 0.022(5) -0.002(5) O8B 0.087(8) 0.063(7) 0.076(7) -0.022(6) 0.021(6) -0.009(6) O13B 0.098(9) 0.092(9) 0.070(7) -0.003(6) 0.047(6) 0.027(7) O15 0.088(10) 0.23(2) 0.102(10) 0.094(13) -0.024(8) -0.070(11) O7B 0.08(2) 0.049(17) 0.16(4) -0.04(2) 0.01(2) 0.010(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 Fe2 C44 1.903(8) . ? Fe2 N8 1.945(6) . ? Fe2 N6 1.947(5) . ? Fe2 N7 1.960(5) . ? Fe2 C42 1.964(7) . ? Fe2 C43 1.971(7) . ? Fe1 N1 1.934(6) . ? Fe1 N3 1.938(6) . ? Fe1 C22 1.952(9) . ? Fe1 N2 1.953(6) . ? Fe1 C20 1.961(7) . ? Fe1 C21 1.974(7) . ? N3 C7 1.362(9) . ? N3 C8 1.400(8) . ? N10 C35 1.329(8) . ? N10 C36 1.399(8) . ? N6 C34 1.316(8) . ? N6 C30 1.325(8) . ? N7 C35 1.367(7) . ? N7 C41 1.373(8) . ? N13 C20 1.143(8) . ? N16 C43 1.147(8) . ? C35 C34 1.462(9) . ? N1 C15 1.377(9) . ? N1 C1 1.401(9) . ? C34 C33 1.386(9) . ? C41 C36 1.382(9) . ? C41 C40 1.401(9) . ? N4 C7 1.335(9) . ? N4 C13 1.356(9) . ? C33 C32 1.382(10) . ? C40 C39 1.390(10) . ? N2 C2 1.331(9) . ? N2 C6 1.354(9) . ? N23 C54 1.482(12) . ? N23 C58 1.508(8) . ? N23 C62 1.529(11) . ? N23 C53 1.531(9) . ? N5 C1 1.308(9) . ? N5 C14 1.403(11) . ? N12 C21 1.134(9) . ? C32 C31 1.382(11) . ? C59 C60 1.525(9) . ? C59 C58 1.534(9) . ? C31 C30 1.368(10) . ? C37 C38 1.386(10) . ? C37 C36 1.388(9) . ? C61 C60 1.525(9) . ? N17 C42 1.139(8) . ? C38 C39 1.415(11) . ? N8 C29 1.363(10) . ? N8 C27 1.366(10) . ? C2 C3 1.390(11) . ? C2 C1 1.447(10) . ? C12 C11 1.346(12) . ? C12 C13 1.431(10) . ? N20 C95 1.511(11) . ? N20 C86 1.514(14) . ? N20 C87 1.516(10) . ? N20 C91 1.543(13) . ? N15 C44 1.160(9) . ? C3 C4 1.367(11) . ? C7 C6 1.439(10) . ? C13 C8 1.405(10) . ? N21 C107 1.507(11) . ? N21 C111 1.517(15) . ? N21 C99 1.524(12) . ? N21 C103 1.590(14) . ? C8 C9 1.402(10) . ? C6 C5 1.379(10) . ? N9 C29 1.317(9) . ? N9 C28 1.369(12) . ? C14 C16 1.396(11) . ? C14 C15 1.409(12) . ? C5 C4 1.419(10) . ? C19 C18 1.345(11) . ? C19 C15 1.398(12) . ? C87 C88 1.525(12) . ? C17 C18 1.366(15) . ? C17 C16 1.420(14) . ? C22 N14 1.133(10) . ? C29 C30 1.490(11) . ? C11 C10 1.384(12) . ? N22 C69 1.396(12) . ? N22 C75 1.484(13) . ? N22 C74 1.487(12) . ? N22 C79 1.529(14) . ? C90 C89 1.493(12) . ? C9 C10 1.376(11) . ? C62 C63 1.568(16) . ? C54 C55 1.528(14) . ? C88 C89 1.525(11) . ? C91 C92 1.508(15) . ? C27 C28 1.404(13) . ? C27 C26 1.418(14) . ? C53 C52 1.526(11) . ? C55 C56 1.468(13) . ? C95 C96 1.512(12) . ? C52 C51 1.564(14) . ? C84 C83 1.468(15) . ? C84 C85 1.589(16) . ? C114 C113 1.499(17) . ? C26 C25 1.365(14) . ? C86 C85 1.484(15) . ? C56 C57 1.386(16) . ? C28 C23 1.445(14) . ? C113 C112 1.460(16) . ? C92 C93 1.571(16) . ? C104 C103 1.439(15) . ? C104 C105 1.583(15) . ? C99 C100 1.546(17) . ? C111 C112 1.532(18) . ? C96 C97 1.427(14) . ? C105 C106 1.510(17) . ? C24 C25 1.37(2) . ? C24 C23 1.38(2) . ? C93 C94 1.433(19) . ? C74 C73 1.449(14) . ? C63 C64 1.490(15) . ? C107 C108 1.472(13) . ? C50 C51 1.559(17) . ? C79 C80 1.525(9) . ? C97 C98 1.44(2) . ? C64 C65 1.441(19) . ? C80 C81 1.42(2) . ? C102 C101 1.355(15) . ? C72 C71 1.459(17) . ? C72 C73 1.495(17) . ? C77 C78 1.418(16) . ? C77 C76 1.451(15) . ? C67 C68 1.512(16) . ? C67 C66 1.546(16) . ? C75 C76 1.310(15) . ? C109 C110 1.415(18) . ? C109 C108 1.456(16) . ? C101 C100 1.468(14) . ? C69 C68 1.411(14) . ? C82 C81 1.52(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 C44 Fe2 N8 99.0(3) . . ? C44 Fe2 N6 178.0(3) . . ? N8 Fe2 N6 81.1(2) . . ? C44 Fe2 N7 99.0(3) . . ? N8 Fe2 N7 162.1(2) . . ? N6 Fe2 N7 81.0(2) . . ? C44 Fe2 C42 88.8(3) . . ? N8 Fe2 C42 89.4(3) . . ? N6 Fe2 C42 89.2(2) . . ? N7 Fe2 C42 91.3(2) . . ? C44 Fe2 C43 87.0(3) . . ? N8 Fe2 C43 88.6(2) . . ? N6 Fe2 C43 95.0(3) . . ? N7 Fe2 C43 92.1(2) . . ? C42 Fe2 C43 175.0(3) . . ? N1 Fe1 N3 161.0(3) . . ? N1 Fe1 C22 98.6(3) . . ? N3 Fe1 C22 100.3(3) . . ? N1 Fe1 N2 81.0(2) . . ? N3 Fe1 N2 80.1(2) . . ? C22 Fe1 N2 178.5(3) . . ? N1 Fe1 C20 88.8(3) . . ? N3 Fe1 C20 91.0(2) . . ? C22 Fe1 C20 89.6(3) . . ? N2 Fe1 C20 89.0(3) . . ? N1 Fe1 C21 92.6(3) . . ? N3 Fe1 C21 88.5(3) . . ? C22 Fe1 C21 87.5(3) . . ? N2 Fe1 C21 93.9(3) . . ? C20 Fe1 C21 177.0(3) . . ? C7 N3 C8 102.9(5) . . ? C7 N3 Fe1 115.3(5) . . ? C8 N3 Fe1 141.7(5) . . ? C35 N10 C36 102.7(5) . . ? C34 N6 C30 122.4(6) . . ? C34 N6 Fe2 119.3(4) . . ? C30 N6 Fe2 118.3(5) . . ? C35 N7 C41 104.6(5) . . ? C35 N7 Fe2 112.5(4) . . ? C41 N7 Fe2 142.8(4) . . ? N10 C35 N7 115.1(5) . . ? N10 C35 C34 127.6(5) . . ? N7 C35 C34 117.2(5) . . ? C15 N1 C1 103.6(6) . . ? C15 N1 Fe1 141.5(6) . . ? C1 N1 Fe1 114.7(4) . . ? N6 C34 C33 120.4(6) . . ? N6 C34 C35 109.9(5) . . ? C33 C34 C35 129.6(6) . . ? N7 C41 C36 107.4(5) . . ? N7 C41 C40 130.4(6) . . ? C36 C41 C40 122.1(6) . . ? C7 N4 C13 104.5(6) . . ? C32 C33 C34 117.6(7) . . ? C39 C40 C41 116.6(6) . . ? C2 N2 C6 123.5(6) . . ? C2 N2 Fe1 117.9(5) . . ? C6 N2 Fe1 118.4(4) . . ? C54 N23 C58 112.8(7) . . ? C54 N23 C62 106.8(7) . . ? C58 N23 C62 110.0(6) . . ? C54 N23 C53 110.2(6) . . ? C58 N23 C53 105.1(5) . . ? C62 N23 C53 112.1(7) . . ? C1 N5 C14 102.6(7) . . ? C33 C32 C31 120.8(7) . . ? C60 C59 C58 111.3(5) . . ? C30 C31 C32 117.8(6) . . ? C38 C37 C36 118.9(7) . . ? C37 C38 C39 119.7(7) . . ? C29 N8 C27 102.6(7) . . ? C29 N8 Fe2 114.9(5) . . ? C27 N8 Fe2 142.5(6) . . ? C40 C39 C38 121.9(6) . . ? N23 C58 C59 114.7(5) . . ? N2 C2 C3 119.2(6) . . ? N2 C2 C1 112.4(6) . . ? C3 C2 C1 128.4(7) . . ? N5 C1 N1 116.3(6) . . ? N5 C1 C2 129.7(7) . . ? N1 C1 C2 114.0(6) . . ? C11 C12 C13 116.9(8) . . ? C59 C60 C61 112.0(5) . . ? C41 C36 C37 120.8(6) . . ? C41 C36 N10 110.1(6) . . ? C37 C36 N10 129.1(6) . . ? C95 N20 C86 112.0(8) . . ? C95 N20 C87 105.3(6) . . ? C86 N20 C87 112.8(8) . . ? C95 N20 C91 108.4(7) . . ? C86 N20 C91 107.9(7) . . ? C87 N20 C91 110.4(8) . . ? C4 C3 C2 118.6(7) . . ? N4 C7 N3 115.5(6) . . ? N4 C7 C6 128.5(7) . . ? N3 C7 C6 116.0(6) . . ? N4 C13 C8 109.6(6) . . ? N4 C13 C12 130.9(7) . . ? C8 C13 C12 119.5(7) . . ? C107 N21 C111 110.5(10) . . ? C107 N21 C99 103.6(7) . . ? C111 N21 C99 115.0(8) . . ? C107 N21 C103 114.0(8) . . ? C111 N21 C103 108.3(7) . . ? C99 N21 C103 105.5(9) . . ? N3 C8 C9 130.3(7) . . ? N3 C8 C13 107.5(6) . . ? C9 C8 C13 122.2(7) . . ? N16 C43 Fe2 179.4(8) . . ? N2 C6 C5 120.2(6) . . ? N2 C6 C7 110.1(6) . . ? C5 C6 C7 129.6(7) . . ? C29 N9 C28 102.1(8) . . ? C16 C14 N5 129.7(9) . . ? C16 C14 C15 119.8(9) . . ? N5 C14 C15 110.5(7) . . ? C6 C5 C4 116.4(6) . . ? C18 C19 C15 117.8(9) . . ? N20 C87 C88 114.5(7) . . ? C18 C17 C16 120.5(8) . . ? N14 C22 Fe1 179.4(8) . . ? N9 C29 N8 117.4(7) . . ? N9 C29 C30 128.1(8) . . ? N8 C29 C30 114.3(6) . . ? C12 C11 C10 123.0(8) . . ? C69 N22 C75 110.3(11) . . ? C69 N22 C74 106.0(11) . . ? C75 N22 C74 114.7(10) . . ? C69 N22 C79 107.2(8) . . ? C75 N22 C79 104.4(9) . . ? C74 N22 C79 114.0(10) . . ? N6 C30 C31 120.9(7) . . ? N6 C30 C29 111.2(6) . . ? C31 C30 C29 127.9(7) . . ? C10 C9 C8 115.8(8) . . ? N23 C62 C63 114.4(7) . . ? N23 C54 C55 116.5(6) . . ? C3 C4 C5 122.0(7) . . ? C87 C88 C89 109.0(7) . . ? N13 C20 Fe1 177.4(7) . . ? C92 C91 N20 117.3(8) . . ? N1 C15 C19 131.8(8) . . ? N1 C15 C14 107.0(7) . . ? C19 C15 C14 121.2(7) . . ? C90 C89 C88 112.9(7) . . ? N8 C27 C28 107.6(8) . . ? N8 C27 C26 131.5(8) . . ? C28 C27 C26 120.9(8) . . ? N15 C44 Fe2 177.4(8) . . ? C9 C10 C11 122.5(8) . . ? C14 C16 C17 117.3(10) . . ? C52 C53 N23 113.9(6) . . ? C56 C55 C54 108.9(9) . . ? N20 C95 C96 116.4(7) . . ? C19 C18 C17 123.3(9) . . ? N12 C21 Fe1 178.1(8) . . ? C53 C52 C51 109.1(7) . . ? C83 C84 C85 108.9(11) . . ? C25 C26 C27 117.0(11) . . ? C85 C86 N20 114.2(7) . . ? C57 C56 C55 106.5(11) . . ? N9 C28 C27 110.2(7) . . ? N9 C28 C23 128.4(10) . . ? C27 C28 C23 121.3(10) . . ? C112 C113 C114 112.0(10) . . ? C91 C92 C93 111.6(10) . . ? C103 C104 C105 111.2(8) . . ? N21 C99 C100 114.7(8) . . ? N21 C111 C112 115.2(8) . . ? C97 C96 C95 113.6(9) . . ? C106 C105 C104 111.6(9) . . ? C25 C24 C23 124.6(10) . . ? C86 C85 C84 109.0(9) . . ? C94 C93 C92 113.9(11) . . ? C73 C74 N22 119.8(12) . . ? C64 C63 C62 110.8(11) . . ? C24 C23 C28 114.0(11) . . ? C108 C107 N21 118.2(10) . . ? C80 C79 N22 111.7(9) . . ? C50 C51 C52 112.3(11) . . ? C104 C103 N21 118.1(8) . . ? C96 C97 C98 113.1(12) . . ? C26 C25 C24 122.0(12) . . ? C113 C112 C111 111.4(9) . . ? C65 C64 C63 109.3(16) . . ? C81 C80 C79 105.6(11) . . ? C71 C72 C73 115(2) . . ? C78 C77 C76 110.8(19) . . ? C68 C67 C66 106.9(17) . . ? C76 C75 N22 126.1(16) . . ? C110 C109 C108 129.4(18) . . ? C102 C101 C100 125.2(16) . . ? N22 C69 C68 124.2(12) . . ? C101 C100 C99 107.9(13) . . ? C74 C73 C72 109.6(13) . . ? C109 C108 C107 115.2(14) . . ? C80 C81 C82 107.3(13) . . ? C75 C76 C77 125.9(16) . . ? C69 C68 C67 112.5(15) . . ? N17 C42 Fe2 178.7(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.853 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.075 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 898146' #TrackingRef 'web_deposit_cif_file_0_DechambenoitPierre_1347283466.compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H27 Co N5 O, 2(B F4)' _chemical_formula_sum 'C29 H27 B2 Co F8 N5 O' _chemical_formula_weight 694.11 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.346(5) _cell_length_b 12.362(5) _cell_length_c 12.855(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.033(13) _cell_angle_gamma 90.00 _cell_volume 2936.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9050 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 30.06 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8777 _exptl_absorpt_correction_T_max 0.9546 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19792 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.09 _reflns_number_total 4285 _reflns_number_gt 3797 _reflns_threshold_expression >2\s(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 ? _computing_publication_material ? _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^ > 2\s(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. Hydrogen atoms belonging to oxygen atom are placed according to difference Fourier map without further constraints. ; _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^)+(0.0389P)^2^+2.0883P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4285 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _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 0.0000 0.714569(18) 0.2500 0.01512(7) Uani 1 2 d S . . N3 N 0.0000 0.54528(12) 0.2500 0.0161(3) Uani 1 2 d S . . F1 F 0.16882(6) 1.02547(8) 0.22622(11) 0.0416(2) Uani 1 1 d . . . F2 F 0.12099(5) 0.99854(8) 0.34669(9) 0.0390(2) Uani 1 1 d . . . F3 F 0.06556(6) 1.11088(10) 0.18615(11) 0.0547(3) Uani 1 1 d . . . F4 F 0.17206(7) 1.16022(9) 0.34773(11) 0.0486(3) Uani 1 1 d . . . N1 N -0.10467(6) 0.70105(9) 0.09289(10) 0.0182(2) Uani 1 1 d . . . N2 N 0.06469(6) 0.71357(9) 0.16633(10) 0.0189(2) Uani 1 1 d . . . C1 C -0.15109(6) 0.62404(10) 0.08810(11) 0.0162(2) Uani 1 1 d . . . C2 C -0.12800(6) 0.55636(10) 0.20315(11) 0.0171(2) Uani 1 1 d . . . C3 C 0.05964(8) 0.37771(11) 0.26400(13) 0.0250(3) Uani 1 1 d . . . H3 H 0.0995 0.3408 0.2708 0.030 Uiso 1 1 calc R . . C4 C 0.0000 0.32155(16) 0.2500 0.0276(4) Uani 1 2 d S . . H4 H 0.0000 0.2463 0.2500 0.033 Uiso 1 2 calc SR . . C5 C 0.05952(7) 0.49066(10) 0.26782(11) 0.0176(2) Uani 1 1 d . . . C6 C 0.11538(7) 0.63613(10) 0.19515(11) 0.0181(2) Uani 1 1 d . . . C7 C 0.05839(8) 0.79181(11) 0.08833(13) 0.0246(3) Uani 1 1 d . . . H7 H 0.0238 0.8454 0.0696 0.030 Uiso 1 1 calc R . . C8 C 0.10061(8) 0.79627(13) 0.03510(13) 0.0287(3) Uani 1 1 d . . . H8 H 0.0955 0.8523 -0.0169 0.034 Uiso 1 1 calc R . . C9 C 0.15081(8) 0.71503(13) 0.06123(13) 0.0280(3) Uani 1 1 d . . . H9 H 0.1794 0.7147 0.0255 0.034 Uiso 1 1 calc R . . C10 C 0.15812(7) 0.63376(12) 0.14145(12) 0.0235(3) Uani 1 1 d . . . H10 H 0.1913 0.5782 0.1591 0.028 Uiso 1 1 calc R . . C11 C -0.12472(7) 0.76341(11) -0.00459(12) 0.0231(3) Uani 1 1 d . . . H11 H -0.0932 0.8173 -0.0005 0.028 Uiso 1 1 calc R . . C12 C -0.18968(7) 0.75159(12) -0.11034(12) 0.0242(3) Uani 1 1 d . . . H12 H -0.2015 0.7961 -0.1759 0.029 Uiso 1 1 calc R . . C13 C -0.23679(7) 0.67193(11) -0.11631(12) 0.0229(3) Uani 1 1 d . . . H13 H -0.2808 0.6614 -0.1865 0.028 Uiso 1 1 calc R . . C14 C -0.21752(7) 0.60775(11) -0.01607(11) 0.0204(2) Uani 1 1 d . . . H14 H -0.2488 0.5542 -0.0184 0.025 Uiso 1 1 calc R . . C15 C -0.18953(7) 0.47748(11) 0.18061(13) 0.0240(3) Uani 1 1 d . . . H15A H -0.1980 0.4290 0.1165 0.036 Uiso 1 1 calc R . . H15B H -0.2328 0.5177 0.1590 0.036 Uiso 1 1 calc R . . H15C H -0.1760 0.4367 0.2523 0.036 Uiso 1 1 calc R . . O1 O 0.0000 0.88096(11) 0.2500 0.0283(3) Uani 1 2 d S . . B2 B 0.13155(9) 1.07467(13) 0.27513(16) 0.0260(3) Uani 1 1 d . . . H1A H 0.0366(11) 0.9164(18) 0.272(2) 0.047(6) Uiso 1 1 d . . . 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 0.01360(12) 0.01302(11) 0.01920(12) 0.000 0.00857(9) 0.000 N3 0.0169(7) 0.0145(6) 0.0176(7) 0.000 0.0091(6) 0.000 F1 0.0476(6) 0.0296(5) 0.0649(7) -0.0014(4) 0.0412(6) 0.0046(4) F2 0.0298(5) 0.0414(5) 0.0427(5) 0.0127(4) 0.0159(4) -0.0083(4) F3 0.0404(6) 0.0665(8) 0.0507(7) 0.0226(6) 0.0180(5) 0.0262(5) F4 0.0648(7) 0.0351(6) 0.0594(7) -0.0136(5) 0.0412(6) -0.0179(5) N1 0.0159(5) 0.0191(5) 0.0197(5) 0.0018(4) 0.0088(4) -0.0008(4) N2 0.0173(5) 0.0198(5) 0.0204(5) 0.0016(4) 0.0099(4) 0.0001(4) C1 0.0157(5) 0.0161(5) 0.0185(5) -0.0011(4) 0.0098(5) 0.0001(4) C2 0.0163(5) 0.0161(5) 0.0199(6) 0.0005(4) 0.0099(5) -0.0022(4) C3 0.0237(7) 0.0168(6) 0.0309(7) -0.0010(5) 0.0110(6) 0.0033(5) C4 0.0287(10) 0.0131(8) 0.0339(10) 0.000 0.0103(8) 0.000 C5 0.0183(6) 0.0154(5) 0.0184(5) -0.0006(4) 0.0086(5) 0.0011(4) C6 0.0168(5) 0.0197(6) 0.0178(5) -0.0030(4) 0.0087(5) -0.0012(4) C7 0.0216(6) 0.0268(7) 0.0260(6) 0.0064(5) 0.0124(5) 0.0014(5) C8 0.0293(7) 0.0352(8) 0.0242(7) 0.0063(6) 0.0152(6) -0.0020(6) C9 0.0276(7) 0.0402(8) 0.0226(6) -0.0007(6) 0.0172(6) -0.0019(6) C10 0.0228(6) 0.0289(7) 0.0220(6) -0.0028(5) 0.0135(5) 0.0015(5) C11 0.0200(6) 0.0237(6) 0.0259(6) 0.0061(5) 0.0116(5) -0.0005(5) C12 0.0231(6) 0.0276(7) 0.0208(6) 0.0057(5) 0.0103(5) 0.0040(5) C13 0.0195(6) 0.0260(7) 0.0181(6) -0.0022(5) 0.0055(5) 0.0019(5) C14 0.0183(6) 0.0206(6) 0.0210(6) -0.0030(5) 0.0088(5) -0.0023(4) C15 0.0209(6) 0.0226(6) 0.0309(7) 0.0000(5) 0.0148(6) -0.0060(5) O1 0.0195(7) 0.0161(6) 0.0496(9) 0.000 0.0175(7) 0.000 B2 0.0240(7) 0.0220(7) 0.0355(8) 0.0041(6) 0.0175(7) 0.0025(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.0568(17) . ? Co1 N3 2.0927(17) . ? Co1 N2 2.1332(12) 2 ? Co1 N2 2.1332(12) . ? Co1 N1 2.1405(12) . ? Co1 N1 2.1405(12) 2 ? N3 C5 1.3532(14) 2 ? N3 C5 1.3532(14) . ? F1 B2 1.3779(19) . ? F2 B2 1.4108(19) . ? F3 B2 1.371(2) . ? F4 B2 1.389(2) . ? N1 C11 1.3457(17) . ? N1 C1 1.3531(16) . ? N2 C6 1.3502(16) . ? N2 C7 1.3503(17) . ? C1 C14 1.3942(18) . ? C1 C2 1.5493(18) . ? C2 C15 1.5424(17) . ? C2 C5 1.5458(17) 2 ? C2 C6 1.5496(18) 2 ? C3 C4 1.3805(17) . ? C3 C5 1.3971(19) . ? C3 H3 0.9300 . ? C4 C3 1.3805(17) 2 ? C4 H4 0.9300 . ? C5 C2 1.5458(17) 2 ? C6 C10 1.3929(18) . ? C6 C2 1.5496(18) 2 ? C7 C8 1.379(2) . ? C7 H7 0.9300 . ? C8 C9 1.382(2) . ? C8 H8 0.9300 . ? C9 C10 1.391(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.3803(19) . ? C11 H11 0.9300 . ? C12 C13 1.382(2) . ? C12 H12 0.9300 . ? C13 C14 1.3886(19) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O1 H1A 0.81(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 O1 Co1 N3 180.0 . . ? O1 Co1 N2 90.33(3) . 2 ? N3 Co1 N2 89.67(3) . 2 ? O1 Co1 N2 90.33(3) . . ? N3 Co1 N2 89.67(3) . . ? N2 Co1 N2 179.34(6) 2 . ? O1 Co1 N1 94.48(3) . . ? N3 Co1 N1 85.52(3) . . ? N2 Co1 N1 80.90(5) 2 . ? N2 Co1 N1 99.04(5) . . ? O1 Co1 N1 94.48(3) . 2 ? N3 Co1 N1 85.52(3) . 2 ? N2 Co1 N1 99.04(5) 2 2 ? N2 Co1 N1 80.90(5) . 2 ? N1 Co1 N1 171.04(6) . 2 ? C5 N3 C5 120.14(15) 2 . ? C5 N3 Co1 119.93(8) 2 . ? C5 N3 Co1 119.93(8) . . ? C11 N1 C1 118.44(11) . . ? C11 N1 Co1 121.95(9) . . ? C1 N1 Co1 119.52(8) . . ? C6 N2 C7 118.68(11) . . ? C6 N2 Co1 119.85(9) . . ? C7 N2 Co1 121.41(9) . . ? N1 C1 C14 120.99(11) . . ? N1 C1 C2 117.42(10) . . ? C14 C1 C2 121.58(11) . . ? C15 C2 C5 109.06(10) . 2 ? C15 C2 C1 109.14(10) . . ? C5 C2 C1 108.95(10) 2 . ? C15 C2 C6 109.44(10) . 2 ? C5 C2 C6 112.74(10) 2 2 ? C1 C2 C6 107.43(10) . 2 ? C4 C3 C5 119.30(13) . . ? C4 C3 H3 120.3 . . ? C5 C3 H3 120.3 . . ? C3 C4 C3 119.61(18) 2 . ? C3 C4 H4 120.2 2 . ? C3 C4 H4 120.2 . . ? N3 C5 C3 120.71(12) . . ? N3 C5 C2 118.23(11) . 2 ? C3 C5 C2 121.03(11) . 2 ? N2 C6 C10 120.84(12) . . ? N2 C6 C2 117.37(11) . 2 ? C10 C6 C2 121.62(11) . 2 ? N2 C7 C8 123.38(13) . . ? N2 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C9 118.05(13) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C8 C9 C10 119.38(13) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C6 119.59(13) . . ? C9 C10 H10 120.2 . . ? C6 C10 H10 120.2 . . ? N1 C11 C12 123.44(13) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 118.33(12) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C12 C13 C14 119.10(12) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C1 119.69(12) . . ? C13 C14 H14 120.2 . . ? C1 C14 H14 120.2 . . ? C2 C15 H15A 109.5 . . ? C2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Co1 O1 H1A 122.6(15) . . ? F3 B2 F1 110.50(14) . . ? F3 B2 F4 110.26(14) . . ? F1 B2 F4 109.58(13) . . ? F3 B2 F2 109.21(13) . . ? F1 B2 F2 108.67(13) . . ? F4 B2 F2 108.59(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 N3 C5 -170(100) . . . 2 ? N2 Co1 N3 C5 35.62(7) 2 . . 2 ? N2 Co1 N3 C5 -144.38(7) . . . 2 ? N1 Co1 N3 C5 -45.28(7) . . . 2 ? N1 Co1 N3 C5 134.72(7) 2 . . 2 ? O1 Co1 N3 C5 10(100) . . . . ? N2 Co1 N3 C5 -144.38(7) 2 . . . ? N2 Co1 N3 C5 35.62(7) . . . . ? N1 Co1 N3 C5 134.72(7) . . . . ? N1 Co1 N3 C5 -45.28(7) 2 . . . ? O1 Co1 N1 C11 43.44(10) . . . . ? N3 Co1 N1 C11 -136.56(10) . . . . ? N2 Co1 N1 C11 133.06(11) 2 . . . ? N2 Co1 N1 C11 -47.61(11) . . . . ? N1 Co1 N1 C11 -136.56(10) 2 . . . ? O1 Co1 N1 C1 -140.04(9) . . . . ? N3 Co1 N1 C1 39.96(9) . . . . ? N2 Co1 N1 C1 -50.43(9) 2 . . . ? N2 Co1 N1 C1 128.90(9) . . . . ? N1 Co1 N1 C1 39.96(9) 2 . . . ? O1 Co1 N2 C6 144.50(9) . . . . ? N3 Co1 N2 C6 -35.50(9) . . . . ? N2 Co1 N2 C6 -35.50(10) 2 . . . ? N1 Co1 N2 C6 -120.91(10) . . . . ? N1 Co1 N2 C6 50.02(9) 2 . . . ? O1 Co1 N2 C7 -32.58(10) . . . . ? N3 Co1 N2 C7 147.42(10) . . . . ? N2 Co1 N2 C7 147.42(10) 2 . . . ? N1 Co1 N2 C7 62.01(11) . . . . ? N1 Co1 N2 C7 -127.06(11) 2 . . . ? C11 N1 C1 C14 1.42(18) . . . . ? Co1 N1 C1 C14 -175.22(9) . . . . ? C11 N1 C1 C2 -177.65(11) . . . . ? Co1 N1 C1 C2 5.71(14) . . . . ? N1 C1 C2 C15 177.42(11) . . . . ? C14 C1 C2 C15 -1.65(16) . . . . ? N1 C1 C2 C5 -63.59(14) . . . 2 ? C14 C1 C2 C5 117.35(13) . . . 2 ? N1 C1 C2 C6 58.85(14) . . . 2 ? C14 C1 C2 C6 -120.22(12) . . . 2 ? C5 C3 C4 C3 2.15(9) . . . 2 ? C5 N3 C5 C3 2.22(9) 2 . . . ? Co1 N3 C5 C3 -177.78(9) . . . . ? C5 N3 C5 C2 -175.67(12) 2 . . 2 ? Co1 N3 C5 C2 4.33(12) . . . 2 ? C4 C3 C5 N3 -4.42(18) . . . . ? C4 C3 C5 C2 173.41(10) . . . 2 ? C7 N2 C6 C10 -2.99(18) . . . . ? Co1 N2 C6 C10 179.85(9) . . . . ? C7 N2 C6 C2 172.29(11) . . . 2 ? Co1 N2 C6 C2 -4.87(14) . . . 2 ? C6 N2 C7 C8 0.8(2) . . . . ? Co1 N2 C7 C8 177.89(11) . . . . ? N2 C7 C8 C9 1.4(2) . . . . ? C7 C8 C9 C10 -1.4(2) . . . . ? C8 C9 C10 C6 -0.7(2) . . . . ? N2 C6 C10 C9 3.0(2) . . . . ? C2 C6 C10 C9 -172.10(12) 2 . . . ? C1 N1 C11 C12 -1.4(2) . . . . ? Co1 N1 C11 C12 175.20(11) . . . . ? N1 C11 C12 C13 0.3(2) . . . . ? C11 C12 C13 C14 0.6(2) . . . . ? C12 C13 C14 C1 -0.5(2) . . . . ? N1 C1 C14 C13 -0.52(19) . . . . ? C2 C1 C14 C13 178.51(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.397 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.054 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 898147' #TrackingRef 'web_deposit_cif_file_1_DechambenoitPierre_1347283466.compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H13 Fe N8, H2 O' _chemical_formula_sum 'C22 H15 F0 Fe N8 O' _chemical_formula_weight 463.27 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 10.9398(12) _cell_length_b 22.107(3) _cell_length_c 16.8809(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.003(6) _cell_angle_gamma 90.00 _cell_volume 4080.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4617 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.90 _exptl_crystal_description square _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9267 _exptl_absorpt_correction_T_max 0.9624 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 84823 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.38 _reflns_number_total 7485 _reflns_number_gt 4976 _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 ? _computing_publication_material 'WINGX (Farrugia)' _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. All non-hydrogens were refined anisotropically. Hydrogen atoms were assigned to ideal positions and refined isotropically using a riding model, except for those connected to the nitrogen atoms of the ligand: the latter were placed using the difference Fourier map and refined using DFIX contraints. The hydrogen atoms belonging to the lattice water molecule were not introduced but are taken into account in the molecular formula. ; _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^)+(0.0735P)^2^+6.5246P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7485 _refine_ls_number_parameters 589 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.019 _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 0.98809(5) 0.86663(2) 0.25677(3) 0.01901(17) Uani 1 1 d . . . Fe2 Fe 0.47384(5) 0.61805(2) 0.25710(3) 0.02105(18) Uani 1 1 d . . . N14 N 0.8252(3) 0.89599(15) 0.3979(2) 0.0262(8) Uani 1 1 d . . . N7 N 1.1512(3) 0.84285(16) 0.1137(2) 0.0318(9) Uani 1 1 d . . . N16 N 0.3026(3) 0.59255(16) 0.3961(2) 0.0313(9) Uani 1 1 d . . . O1W O 1.3038(3) 0.69988(12) 0.49311(17) 0.0278(7) Uani 1 1 d . . . N2 N 1.2442(3) 0.79757(14) 0.4061(2) 0.0205(7) Uani 1 1 d D . . C20 C 0.8848(4) 0.88399(17) 0.3465(3) 0.0222(9) Uani 1 1 d . . . N11 N 0.2357(3) 0.51997(14) 0.1266(2) 0.0235(8) Uani 1 1 d D . . N9 N 0.3405(3) 0.59456(14) 0.18409(19) 0.0194(7) Uani 1 1 d . . . N12 N 0.7564(3) 0.55541(16) 0.3913(2) 0.0255(8) Uani 1 1 d D . . C44 C 0.3658(4) 0.60344(17) 0.3457(3) 0.0230(9) Uani 1 1 d . . . N1 N 0.8411(3) 0.84640(14) 0.19255(19) 0.0188(7) Uani 1 1 d . . . C3 C 0.6256(4) 0.94651(18) 0.0792(2) 0.0242(9) Uani 1 1 d . . . H3 H 0.6093 0.9863 0.0645 0.029 Uiso 1 1 calc R . . N3 N 0.7160(3) 0.77400(14) 0.1463(2) 0.0220(8) Uani 1 1 d D . . C7 C 0.8176(3) 0.78649(17) 0.1898(2) 0.0198(9) Uani 1 1 d . . . N5 N 0.9861(3) 0.77992(13) 0.27230(19) 0.0176(7) Uani 1 1 d . . . N6 N 1.1272(3) 0.85915(14) 0.33113(19) 0.0182(7) Uani 1 1 d . . . C21 C 1.0920(4) 0.85262(17) 0.1657(3) 0.0227(9) Uani 1 1 d . . . N8 N 0.5048(3) 0.53184(15) 0.25283(19) 0.0209(8) Uani 1 1 d . . . C29 C 0.3335(4) 0.53449(17) 0.1718(2) 0.0201(9) Uani 1 1 d . . . N10 N 0.6179(3) 0.61378(15) 0.3282(2) 0.0238(8) Uani 1 1 d . . . C1 C 0.7477(3) 0.87379(17) 0.1476(2) 0.0202(9) Uani 1 1 d . . . C2 C 0.7267(4) 0.93435(17) 0.1282(2) 0.0210(9) Uani 1 1 d . . . H2 H 0.7781 0.9650 0.1472 0.025 Uiso 1 1 calc R . . C4 C 0.5466(4) 0.90036(19) 0.0508(2) 0.0271(10) Uani 1 1 d . . . H4 H 0.4794 0.9106 0.0184 0.033 Uiso 1 1 calc R . . C5 C 0.5665(4) 0.84044(18) 0.0699(2) 0.0253(9) Uani 1 1 d . . . H5 H 0.5143 0.8100 0.0513 0.030 Uiso 1 1 calc R . . C6 C 0.6686(4) 0.82817(17) 0.1182(2) 0.0218(9) Uani 1 1 d . . . C8 C 0.9009(3) 0.74632(16) 0.2337(2) 0.0182(8) Uani 1 1 d . . . C12 C 1.0743(3) 0.75441(17) 0.3183(2) 0.0185(8) Uani 1 1 d . . . C13 C 1.1516(3) 0.80180(17) 0.3528(2) 0.0187(8) Uani 1 1 d . . . C14 C 1.2863(3) 0.85606(18) 0.4210(2) 0.0213(9) Uani 1 1 d . . . C15 C 1.3797(4) 0.87704(18) 0.4704(2) 0.0249(9) Uani 1 1 d . . . H15 H 1.4295 0.8509 0.5002 0.030 Uiso 1 1 calc R . . C16 C 1.3954(4) 0.93911(19) 0.4735(2) 0.0283(10) Uani 1 1 d . . . H16 H 1.4575 0.9553 0.5060 0.034 Uiso 1 1 calc R . . C17 C 1.3195(4) 0.97825(19) 0.4283(3) 0.0267(10) Uani 1 1 d . . . H17 H 1.3327 1.0197 0.4322 0.032 Uiso 1 1 calc R . . C18 C 1.2267(4) 0.95765(18) 0.3786(2) 0.0244(9) Uani 1 1 d . . . H18 H 1.1768 0.9841 0.3493 0.029 Uiso 1 1 calc R . . C19 C 1.2109(3) 0.89488(17) 0.3742(2) 0.0193(8) Uani 1 1 d . . . C11 C 1.0811(4) 0.69204(17) 0.3259(3) 0.0233(9) Uani 1 1 d . . . H11 H 1.1423 0.6742 0.3576 0.028 Uiso 1 1 calc R . . C10 C 0.9940(4) 0.65658(17) 0.2850(2) 0.0231(9) Uani 1 1 d . . . H10 H 0.9972 0.6146 0.2890 0.028 Uiso 1 1 calc R . . C9 C 0.9027(3) 0.68391(17) 0.2384(2) 0.0209(9) Uani 1 1 d . . . H9 H 0.8441 0.6608 0.2110 0.025 Uiso 1 1 calc R . . C22 C 0.9964(4) 0.9526(2) 0.2370(3) 0.0271(10) Uani 1 1 d . . . N4 N 1.0027(4) 1.00240(17) 0.2250(2) 0.0366(10) Uani 1 1 d . . . C35 C 0.5981(4) 0.50859(18) 0.2961(2) 0.0226(9) Uani 1 1 d . . . C34 C 0.6219(4) 0.44674(18) 0.2954(2) 0.0264(10) Uani 1 1 d . . . H34 H 0.6870 0.4304 0.3252 0.032 Uiso 1 1 calc R . . C32 C 0.5450(4) 0.41020(19) 0.2488(3) 0.0287(10) Uani 1 1 d . . . H32 H 0.5593 0.3688 0.2469 0.034 Uiso 1 1 calc R . . C31 C 0.4478(4) 0.43444(18) 0.2053(2) 0.0241(9) Uani 1 1 d . . . H31 H 0.3962 0.4098 0.1745 0.029 Uiso 1 1 calc R . . C30 C 0.4286(3) 0.49672(17) 0.2085(2) 0.0193(9) Uani 1 1 d . . . C28 C 0.1732(4) 0.57276(17) 0.1074(2) 0.0223(9) Uani 1 1 d . . . C27 C 0.0668(4) 0.58329(19) 0.0618(3) 0.0286(10) Uani 1 1 d . . . H27 H 0.0219 0.5519 0.0385 0.034 Uiso 1 1 calc R . . C26 C 0.0317(4) 0.6431(2) 0.0531(3) 0.0301(10) Uani 1 1 d . . . H26 H -0.0394 0.6522 0.0237 0.036 Uiso 1 1 calc R . . C25 C 0.1006(4) 0.69027(19) 0.0874(2) 0.0280(10) Uani 1 1 d . . . H25 H 0.0750 0.7299 0.0786 0.034 Uiso 1 1 calc R . . C24 C 0.2044(4) 0.68018(18) 0.1333(2) 0.0229(9) Uani 1 1 d . . . H24 H 0.2485 0.7119 0.1565 0.027 Uiso 1 1 calc R . . C23 C 0.2409(3) 0.61992(17) 0.1438(2) 0.0195(9) Uani 1 1 d . . . C36 C 0.6607(4) 0.55707(18) 0.3405(2) 0.0227(9) Uani 1 1 d . . . C38 C 0.7798(4) 0.6141(2) 0.4153(2) 0.0287(10) Uani 1 1 d . . . C39 C 0.8688(4) 0.6379(2) 0.4674(3) 0.0371(12) Uani 1 1 d . . . H39 H 0.9254 0.6134 0.4944 0.045 Uiso 1 1 calc R . . C40 C 0.8681(5) 0.6993(2) 0.4766(3) 0.0418(13) Uani 1 1 d . . . H40 H 0.9275 0.7170 0.5099 0.050 Uiso 1 1 calc R . . C41 C 0.7816(5) 0.7366(2) 0.4377(3) 0.0426(13) Uani 1 1 d . . . H41 H 0.7844 0.7781 0.4468 0.051 Uiso 1 1 calc R . . C42 C 0.6923(4) 0.7136(2) 0.3864(3) 0.0347(11) Uani 1 1 d . . . H42 H 0.6351 0.7384 0.3604 0.042 Uiso 1 1 calc R . . C37 C 0.6927(4) 0.65103(19) 0.3758(2) 0.0264(10) Uani 1 1 d . . . C43 C 0.5781(4) 0.63638(17) 0.1668(3) 0.0236(9) Uani 1 1 d . . . N15 N 0.6376(3) 0.64915(16) 0.1176(2) 0.0270(8) Uani 1 1 d . . . C45 C 0.4404(4) 0.7039(2) 0.2630(3) 0.0285(10) Uani 1 1 d . . . N13 N 0.4235(4) 0.75399(16) 0.2675(2) 0.0342(9) Uani 1 1 d . . . O2W O 0.8482(4) 0.45764(18) 0.4757(2) 0.0687(12) Uani 1 1 d . . . H3N H 0.690(5) 0.7341(13) 0.134(3) 0.082 Uiso 1 1 d D . . H2N H 1.273(5) 0.7639(18) 0.436(3) 0.082 Uiso 1 1 d D . . H11N H 0.214(5) 0.4809(14) 0.109(3) 0.082 Uiso 1 1 d D . . H12N H 0.804(5) 0.524(2) 0.414(3) 0.082 Uiso 1 1 d D . . 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 0.0223(3) 0.0110(3) 0.0231(3) 0.0005(2) -0.0076(2) -0.0016(2) Fe2 0.0266(3) 0.0130(3) 0.0227(3) -0.0001(2) -0.0095(3) -0.0015(2) N14 0.032(2) 0.0178(18) 0.028(2) 0.0034(16) -0.0070(17) 0.0073(15) N7 0.039(2) 0.024(2) 0.033(2) -0.0024(17) -0.0023(19) -0.0057(17) N16 0.038(2) 0.025(2) 0.030(2) -0.0027(17) -0.0086(19) 0.0079(17) O1W 0.0307(16) 0.0202(15) 0.0318(17) 0.0025(13) -0.0088(13) 0.0051(12) N2 0.0220(18) 0.0170(18) 0.0223(19) 0.0012(14) -0.0048(15) -0.0006(14) C20 0.026(2) 0.0089(19) 0.031(3) 0.0022(18) -0.014(2) 0.0022(16) N11 0.0295(19) 0.0138(17) 0.027(2) -0.0007(15) -0.0079(16) -0.0060(15) N9 0.0247(18) 0.0109(16) 0.0221(18) 0.0004(14) -0.0045(14) -0.0025(13) N12 0.0251(19) 0.029(2) 0.0219(19) -0.0007(16) -0.0073(16) 0.0009(15) C44 0.028(2) 0.014(2) 0.026(2) -0.0010(18) -0.012(2) 0.0074(17) N1 0.0229(17) 0.0111(16) 0.0221(18) 0.0002(14) -0.0012(14) -0.0006(13) C3 0.031(2) 0.016(2) 0.024(2) -0.0003(17) -0.0019(19) 0.0033(17) N3 0.0241(18) 0.0120(17) 0.029(2) -0.0026(15) -0.0068(15) -0.0030(14) C7 0.020(2) 0.014(2) 0.026(2) -0.0008(17) -0.0035(17) -0.0036(15) N5 0.0211(17) 0.0081(16) 0.0233(18) 0.0004(14) -0.0012(14) -0.0016(13) N6 0.0213(17) 0.0111(16) 0.0218(18) 0.0013(14) -0.0032(14) -0.0006(13) C21 0.023(2) 0.013(2) 0.031(3) -0.0011(18) -0.0083(19) -0.0055(16) N8 0.0265(19) 0.0165(18) 0.0196(18) 0.0043(14) -0.0030(15) 0.0006(13) C29 0.027(2) 0.013(2) 0.020(2) -0.0012(16) -0.0027(18) -0.0042(16) N10 0.0271(19) 0.0202(18) 0.0237(19) 0.0004(15) -0.0037(15) -0.0041(14) C1 0.020(2) 0.021(2) 0.019(2) -0.0005(17) -0.0033(17) 0.0018(16) C2 0.027(2) 0.012(2) 0.024(2) -0.0008(16) -0.0038(18) -0.0024(16) C4 0.028(2) 0.029(2) 0.024(2) 0.0024(19) -0.0078(18) 0.0048(18) C5 0.026(2) 0.022(2) 0.028(2) -0.0023(19) -0.0081(18) -0.0034(17) C6 0.023(2) 0.018(2) 0.024(2) -0.0025(17) -0.0028(18) -0.0006(16) C8 0.021(2) 0.0120(19) 0.021(2) 0.0002(16) -0.0014(17) -0.0031(15) C12 0.018(2) 0.016(2) 0.021(2) 0.0016(16) -0.0008(16) 0.0004(15) C13 0.020(2) 0.014(2) 0.022(2) 0.0030(16) -0.0016(17) 0.0014(15) C14 0.024(2) 0.017(2) 0.023(2) 0.0000(17) -0.0017(17) -0.0016(16) C15 0.025(2) 0.027(2) 0.023(2) 0.0011(18) -0.0070(18) 0.0000(18) C16 0.032(2) 0.028(2) 0.024(2) -0.0010(19) -0.0087(19) -0.0121(19) C17 0.033(2) 0.018(2) 0.029(2) 0.0003(18) -0.0068(19) -0.0102(18) C18 0.030(2) 0.018(2) 0.025(2) 0.0039(18) -0.0021(19) -0.0022(17) C19 0.020(2) 0.016(2) 0.021(2) 0.0002(17) -0.0071(17) -0.0041(16) C11 0.023(2) 0.017(2) 0.030(2) 0.0038(18) -0.0006(18) 0.0038(17) C10 0.027(2) 0.0093(19) 0.033(2) 0.0007(17) 0.0013(18) 0.0001(16) C9 0.022(2) 0.014(2) 0.027(2) -0.0018(17) -0.0039(18) -0.0041(16) C22 0.028(2) 0.025(3) 0.027(2) -0.0010(19) -0.0112(19) 0.0010(18) N4 0.051(3) 0.015(2) 0.042(2) 0.0013(18) -0.019(2) -0.0007(17) C35 0.027(2) 0.021(2) 0.020(2) 0.0015(17) -0.0042(18) 0.0027(17) C34 0.030(2) 0.022(2) 0.027(2) 0.0088(19) -0.0019(19) 0.0083(18) C32 0.037(2) 0.015(2) 0.034(3) -0.0017(19) 0.004(2) 0.0035(18) C31 0.031(2) 0.016(2) 0.026(2) -0.0015(18) 0.0023(19) -0.0013(17) C30 0.025(2) 0.014(2) 0.018(2) -0.0025(16) -0.0022(17) -0.0032(16) C28 0.026(2) 0.017(2) 0.023(2) 0.0039(17) -0.0046(18) -0.0021(16) C27 0.028(2) 0.026(2) 0.031(3) -0.0038(19) -0.0076(19) -0.0055(18) C26 0.029(2) 0.035(3) 0.026(2) 0.001(2) -0.0111(19) 0.006(2) C25 0.033(2) 0.023(2) 0.027(2) 0.0045(19) -0.0053(19) 0.0060(19) C24 0.030(2) 0.018(2) 0.020(2) 0.0021(17) -0.0027(18) 0.0032(17) C23 0.022(2) 0.019(2) 0.017(2) 0.0022(16) -0.0041(17) -0.0026(16) C36 0.024(2) 0.021(2) 0.023(2) 0.0023(18) -0.0014(18) 0.0045(17) C38 0.023(2) 0.042(3) 0.021(2) 0.003(2) -0.0039(18) -0.0062(19) C39 0.032(3) 0.052(3) 0.027(3) 0.005(2) -0.005(2) -0.011(2) C40 0.043(3) 0.057(4) 0.025(3) -0.002(2) -0.005(2) -0.022(3) C41 0.056(3) 0.035(3) 0.037(3) -0.002(2) 0.000(3) -0.028(2) C42 0.050(3) 0.023(2) 0.030(3) 0.001(2) -0.008(2) -0.016(2) C37 0.032(2) 0.027(2) 0.020(2) 0.0005(18) -0.0046(18) -0.0144(19) C43 0.032(2) 0.009(2) 0.029(3) 0.0014(18) -0.020(2) -0.0066(17) N15 0.033(2) 0.0186(19) 0.029(2) -0.0014(16) -0.0114(18) -0.0028(16) C45 0.031(2) 0.028(3) 0.025(2) 0.0008(19) -0.0107(19) -0.0053(19) N13 0.050(2) 0.016(2) 0.037(2) -0.0030(17) -0.0083(19) -0.0056(17) O2W 0.094(3) 0.055(3) 0.058(3) 0.015(2) 0.004(2) 0.034(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C22 1.933(5) . ? Fe1 N5 1.935(3) . ? Fe1 N6 1.946(3) . ? Fe1 N1 1.959(3) . ? Fe1 C20 1.960(5) . ? Fe1 C21 1.968(5) . ? Fe2 C45 1.937(5) . ? Fe2 N8 1.938(3) . ? Fe2 N9 1.947(3) . ? Fe2 N10 1.950(3) . ? Fe2 C44 1.965(5) . ? Fe2 C43 1.977(5) . ? N14 C20 1.134(5) . ? N7 C21 1.130(5) . ? N16 C44 1.141(5) . ? N2 C13 1.334(5) . ? N2 C14 1.393(5) . ? N2 H2N 0.95(2) . ? N11 C29 1.332(5) . ? N11 C28 1.385(5) . ? N11 H11N 0.94(2) . ? N9 C29 1.346(5) . ? N9 C23 1.384(5) . ? N12 C36 1.331(5) . ? N12 C38 1.380(6) . ? N12 H12N 0.95(2) . ? N1 C7 1.350(5) . ? N1 C1 1.391(5) . ? C3 C2 1.384(5) . ? C3 C4 1.410(6) . ? C3 H3 0.9300 . ? N3 C7 1.339(5) . ? N3 C6 1.382(5) . ? N3 H3N 0.95(2) . ? C7 C8 1.457(5) . ? N5 C12 1.341(5) . ? N5 C8 1.343(5) . ? N6 C13 1.344(5) . ? N6 C19 1.394(5) . ? N8 C35 1.337(5) . ? N8 C30 1.347(5) . ? C29 C30 1.456(5) . ? N10 C36 1.351(5) . ? N10 C37 1.395(5) . ? C1 C2 1.395(5) . ? C1 C6 1.408(5) . ? C2 H2 0.9300 . ? C4 C5 1.379(6) . ? C4 H4 0.9300 . ? C5 C6 1.387(6) . ? C5 H5 0.9300 . ? C8 C9 1.382(5) . ? C12 C11 1.387(5) . ? C12 C13 1.455(5) . ? C14 C15 1.376(5) . ? C14 C19 1.414(5) . ? C15 C16 1.384(6) . ? C15 H15 0.9300 . ? C16 C17 1.406(6) . ? C16 H16 0.9300 . ? C17 C18 1.372(6) . ? C17 H17 0.9300 . ? C18 C19 1.400(5) . ? C18 H18 0.9300 . ? C11 C10 1.398(6) . ? C11 H11 0.9300 . ? C10 C9 1.387(5) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? C22 N4 1.121(5) . ? C35 C34 1.392(6) . ? C35 C36 1.463(6) . ? C34 C32 1.391(6) . ? C34 H34 0.9300 . ? C32 C31 1.379(6) . ? C32 H32 0.9300 . ? C31 C30 1.394(5) . ? C31 H31 0.9300 . ? C28 C27 1.392(6) . ? C28 C23 1.407(5) . ? C27 C26 1.383(6) . ? C27 H27 0.9300 . ? C26 C25 1.401(6) . ? C26 H26 0.9300 . ? C25 C24 1.370(6) . ? C25 H25 0.9300 . ? C24 C23 1.400(5) . ? C24 H24 0.9300 . ? C38 C39 1.392(6) . ? C38 C37 1.406(6) . ? C39 C40 1.366(7) . ? C39 H39 0.9300 . ? C40 C41 1.402(7) . ? C40 H40 0.9300 . ? C41 C42 1.380(6) . ? C41 H41 0.9300 . ? C42 C37 1.396(6) . ? C42 H42 0.9300 . ? C43 N15 1.110(5) . ? C45 N13 1.125(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Fe1 N5 176.95(17) . . ? C22 Fe1 N6 98.88(15) . . ? N5 Fe1 N6 80.83(13) . . ? C22 Fe1 N1 99.89(15) . . ? N5 Fe1 N1 80.57(13) . . ? N6 Fe1 N1 161.07(13) . . ? C22 Fe1 C20 88.44(17) . . ? N5 Fe1 C20 94.59(15) . . ? N6 Fe1 C20 88.70(15) . . ? N1 Fe1 C20 89.32(15) . . ? C22 Fe1 C21 89.31(17) . . ? N5 Fe1 C21 87.67(15) . . ? N6 Fe1 C21 91.74(15) . . ? N1 Fe1 C21 90.97(15) . . ? C20 Fe1 C21 177.74(16) . . ? C45 Fe2 N8 178.83(17) . . ? C45 Fe2 N9 98.95(15) . . ? N8 Fe2 N9 80.92(13) . . ? C45 Fe2 N10 99.54(16) . . ? N8 Fe2 N10 80.59(13) . . ? N9 Fe2 N10 161.51(14) . . ? C45 Fe2 C44 90.14(17) . . ? N8 Fe2 C44 88.70(15) . . ? N9 Fe2 C44 88.88(15) . . ? N10 Fe2 C44 91.07(15) . . ? C45 Fe2 C43 87.35(17) . . ? N8 Fe2 C43 93.81(15) . . ? N9 Fe2 C43 90.37(15) . . ? N10 Fe2 C43 90.49(15) . . ? C44 Fe2 C43 177.24(16) . . ? C13 N2 C14 107.2(3) . . ? C13 N2 H2N 130(4) . . ? C14 N2 H2N 122(4) . . ? N14 C20 Fe1 177.8(4) . . ? C29 N11 C28 108.1(3) . . ? C29 N11 H11N 126(4) . . ? C28 N11 H11N 125(4) . . ? C29 N9 C23 106.5(3) . . ? C29 N9 Fe2 113.5(3) . . ? C23 N9 Fe2 139.8(3) . . ? C36 N12 C38 107.3(3) . . ? C36 N12 H12N 134(4) . . ? C38 N12 H12N 119(4) . . ? N16 C44 Fe2 177.2(4) . . ? C7 N1 C1 105.8(3) . . ? C7 N1 Fe1 113.3(3) . . ? C1 N1 Fe1 140.9(3) . . ? C2 C3 C4 122.0(4) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C7 N3 C6 107.7(3) . . ? C7 N3 H3N 123(4) . . ? C6 N3 H3N 129(4) . . ? N3 C7 N1 112.0(3) . . ? N3 C7 C8 130.2(3) . . ? N1 C7 C8 117.7(3) . . ? C12 N5 C8 121.4(3) . . ? C12 N5 Fe1 118.9(2) . . ? C8 N5 Fe1 119.5(3) . . ? C13 N6 C19 105.8(3) . . ? C13 N6 Fe1 113.5(2) . . ? C19 N6 Fe1 140.6(3) . . ? N7 C21 Fe1 178.0(4) . . ? C35 N8 C30 121.9(3) . . ? C35 N8 Fe2 119.3(3) . . ? C30 N8 Fe2 118.8(3) . . ? N11 C29 N9 111.5(3) . . ? N11 C29 C30 130.8(3) . . ? N9 C29 C30 117.7(3) . . ? C36 N10 C37 105.5(3) . . ? C36 N10 Fe2 114.0(3) . . ? C37 N10 Fe2 140.4(3) . . ? N1 C1 C2 131.1(4) . . ? N1 C1 C6 108.1(3) . . ? C2 C1 C6 120.7(4) . . ? C3 C2 C1 116.6(4) . . ? C3 C2 H2 121.7 . . ? C1 C2 H2 121.7 . . ? C5 C4 C3 121.8(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 116.3(4) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? N3 C6 C5 131.0(4) . . ? N3 C6 C1 106.4(3) . . ? C5 C6 C1 122.6(4) . . ? N5 C8 C9 121.1(4) . . ? N5 C8 C7 108.7(3) . . ? C9 C8 C7 130.2(4) . . ? N5 C12 C11 120.5(4) . . ? N5 C12 C13 109.0(3) . . ? C11 C12 C13 130.5(4) . . ? N2 C13 N6 112.9(3) . . ? N2 C13 C12 129.5(3) . . ? N6 C13 C12 117.6(3) . . ? C15 C14 N2 131.1(4) . . ? C15 C14 C19 122.7(4) . . ? N2 C14 C19 106.2(3) . . ? C14 C15 C16 116.5(4) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C15 C16 C17 121.3(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 122.6(4) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 116.7(4) . . ? C17 C18 H18 121.7 . . ? C19 C18 H18 121.7 . . ? N6 C19 C18 131.8(4) . . ? N6 C19 C14 107.9(3) . . ? C18 C19 C14 120.2(4) . . ? C12 C11 C10 118.6(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C8 C9 C10 118.4(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N4 C22 Fe1 179.0(5) . . ? N8 C35 C34 120.8(4) . . ? N8 C35 C36 109.4(3) . . ? C34 C35 C36 129.8(4) . . ? C32 C34 C35 117.8(4) . . ? C32 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C31 C32 C34 121.1(4) . . ? C31 C32 H32 119.5 . . ? C34 C32 H32 119.5 . . ? C32 C31 C30 118.5(4) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? N8 C30 C31 120.0(4) . . ? N8 C30 C29 109.0(3) . . ? C31 C30 C29 131.0(4) . . ? N11 C28 C27 131.8(4) . . ? N11 C28 C23 105.9(3) . . ? C27 C28 C23 122.3(4) . . ? C26 C27 C28 116.2(4) . . ? C26 C27 H27 121.9 . . ? C28 C27 H27 121.9 . . ? C27 C26 C25 121.7(4) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C24 C25 C26 122.4(4) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C24 C23 117.0(4) . . ? C25 C24 H24 121.5 . . ? C23 C24 H24 121.5 . . ? N9 C23 C24 131.6(4) . . ? N9 C23 C28 107.9(3) . . ? C24 C23 C28 120.4(4) . . ? N12 C36 N10 112.6(4) . . ? N12 C36 C35 130.8(4) . . ? N10 C36 C35 116.6(3) . . ? N12 C38 C39 131.3(4) . . ? N12 C38 C37 106.9(3) . . ? C39 C38 C37 121.8(4) . . ? C40 C39 C38 116.2(5) . . ? C40 C39 H39 121.9 . . ? C38 C39 H39 121.9 . . ? C39 C40 C41 122.5(4) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C42 C41 C40 121.9(5) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C37 116.2(5) . . ? C41 C42 H42 121.9 . . ? C37 C42 H42 121.9 . . ? N10 C37 C42 130.9(4) . . ? N10 C37 C38 107.7(4) . . ? C42 C37 C38 121.4(4) . . ? N15 C43 Fe2 176.9(4) . . ? N13 C45 Fe2 178.4(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.061 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.115 data_compound_[FeCo]90K _database_code_depnum_ccdc_archive 'CCDC 898148' #TrackingRef 'web_deposit_cif_file_2_DechambenoitPierre_1347283466.[FeCo]90K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C51 H36 Co Fe N13), 5(C H4 O)' _chemical_formula_sum 'C107 H92 Co2 Fe2 N26 O5' _chemical_formula_weight 2051.63 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' 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 13.5995(10) _cell_length_b 14.2091(10) _cell_length_c 24.9650(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.148(3) _cell_angle_gamma 90.00 _cell_volume 4697.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 25.30 _exptl_crystal_description square _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8573 _exptl_absorpt_correction_T_max 0.9313 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33940 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8376 _reflns_number_gt 7378 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'AUTOSTRUCTURE (Bruker)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material 'WINGX (Farrugia)' _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^ > 2\s(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.All non-hydrogens were refined anisotropically. Hydrogen atoms were assigned to ideal positions and refined isotropically using a riding model. Two crystallographically independent methanol molecule were found to have positional disorder. The methanol molecule bearing C3S was refined using DFIX and SIMU constraint/restrain. Hydrogen atoms for the disordered mathanol molecules were not introduced, but are taken into account in the compound formula. ; _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^)+(0.0417P)^2^+13.5224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8376 _refine_ls_number_parameters 669 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.126 _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 Co1 Co 0.29954(3) 0.99725(3) 0.352985(17) 0.01582(13) Uani 1 1 d . . . Fe1 Fe 0.21365(4) 0.98793(3) 0.149385(19) 0.01836(13) Uani 1 1 d . . . N11 N 0.1265(2) 1.2259(2) 0.06295(13) 0.0303(7) Uani 1 1 d . . . N4 N 0.2185(2) 0.8785(2) 0.34662(11) 0.0192(6) Uani 1 1 d . . . N1 N 0.4287(2) 0.89917(19) 0.35306(11) 0.0190(6) Uani 1 1 d . . . N5 N 0.33049(19) 0.98372(19) 0.43313(11) 0.0168(6) Uani 1 1 d . . . N2 N 0.1727(2) 1.0950(2) 0.35585(12) 0.0221(6) Uani 1 1 d . . . N3 N 0.3748(2) 1.1192(2) 0.36073(11) 0.0194(6) Uani 1 1 d . . . N9 N 0.1711(2) 0.9764(2) 0.07054(12) 0.0208(6) Uani 1 1 d . . . C46 C 0.2634(2) 0.7739(2) 0.17401(14) 0.0180(7) Uani 1 1 d . . . C47 C 0.2965(3) 0.7614(2) 0.23104(14) 0.0216(7) Uani 1 1 d . . . H47 H 0.3007 0.8117 0.2553 0.026 Uiso 1 1 calc R . . N8 N 0.2211(2) 0.7283(2) 0.08361(12) 0.0217(6) Uani 1 1 d . . . N10 N 0.1796(2) 1.1178(2) 0.13153(12) 0.0205(6) Uani 1 1 d . . . C38 C 0.1758(2) 1.2037(2) 0.15651(15) 0.0226(7) Uani 1 1 d . . . C32 C 0.0761(3) 0.9649(2) 0.16020(14) 0.0239(8) Uani 1 1 d . . . C11 C 0.2505(3) 0.8040(2) 0.37908(14) 0.0204(7) Uani 1 1 d . . . C12 C 0.1939(3) 0.7216(3) 0.37346(15) 0.0264(8) Uani 1 1 d . . . H12 H 0.2166 0.6708 0.3964 0.032 Uiso 1 1 calc R . . C13 C 0.1046(3) 0.7140(3) 0.33442(16) 0.0317(9) Uani 1 1 d . . . H13 H 0.0664 0.6592 0.3312 0.038 Uiso 1 1 calc R . . C14 C 0.0734(3) 0.7899(3) 0.30010(16) 0.0305(9) Uani 1 1 d . . . H14 H 0.0144 0.7868 0.2727 0.037 Uiso 1 1 calc R . . C15 C 0.1317(3) 0.8701(3) 0.30757(15) 0.0267(8) Uani 1 1 d . . . H15 H 0.1104 0.9211 0.2846 0.032 Uiso 1 1 calc R . . C26 C 0.3545(3) 0.8120(2) 0.41924(14) 0.0198(7) Uani 1 1 d . . . C10 C 0.4341(2) 0.8208(2) 0.38414(14) 0.0196(7) Uani 1 1 d . . . C6 C 0.4937(3) 0.9080(3) 0.32026(15) 0.0269(8) Uani 1 1 d . . . H6 H 0.4891 0.9613 0.2982 0.032 Uiso 1 1 calc R . . C7 C 0.5673(3) 0.8423(3) 0.31740(17) 0.0315(9) Uani 1 1 d . . . H7 H 0.6123 0.8520 0.2949 0.038 Uiso 1 1 calc R . . C8 C 0.5722(3) 0.7619(3) 0.34878(17) 0.0313(9) Uani 1 1 d . . . H8 H 0.6204 0.7159 0.3476 0.038 Uiso 1 1 calc R . . C9 C 0.5046(3) 0.7504(3) 0.38208(16) 0.0276(8) Uani 1 1 d . . . H9 H 0.5060 0.6960 0.4030 0.033 Uiso 1 1 calc R . . C27 C 0.3755(3) 0.7226(3) 0.45506(16) 0.0289(8) Uani 1 1 d . . . H27A H 0.3273 0.7182 0.4777 0.043 Uiso 1 1 calc R . . H27B H 0.4424 0.7258 0.4781 0.043 Uiso 1 1 calc R . . H27C H 0.3700 0.6682 0.4318 0.043 Uiso 1 1 calc R . . C25 C 0.3605(2) 0.8994(2) 0.45678(14) 0.0197(7) Uani 1 1 d . . . C21 C 0.3302(2) 1.0605(2) 0.46578(14) 0.0202(7) Uani 1 1 d . . . C22 C 0.3636(3) 1.0541(3) 0.52249(14) 0.0265(8) Uani 1 1 d . . . H22 H 0.3622 1.1067 0.5445 0.032 Uiso 1 1 calc R . . C23 C 0.3986(3) 0.9698(3) 0.54595(15) 0.0277(8) Uani 1 1 d . . . H23 H 0.4235 0.9654 0.5838 0.033 Uiso 1 1 calc R . . C24 C 0.3967(3) 0.8918(3) 0.51316(14) 0.0262(8) Uani 1 1 d . . . H24 H 0.4197 0.8342 0.5288 0.031 Uiso 1 1 calc R . . C28 C 0.2929(3) 1.1545(2) 0.43753(14) 0.0218(7) Uani 1 1 d . . . C5 C 0.1837(3) 1.1447(2) 0.40281(15) 0.0218(7) Uani 1 1 d . . . C1 C 0.0815(3) 1.0960(3) 0.32041(16) 0.0292(8) Uani 1 1 d . . . H1 H 0.0744 1.0649 0.2870 0.035 Uiso 1 1 calc R . . C2 C -0.0019(3) 1.1410(3) 0.33136(18) 0.0361(10) Uani 1 1 d . . . H2 H -0.0631 1.1420 0.3056 0.043 Uiso 1 1 calc R . . C3 C 0.0087(3) 1.1844(3) 0.3816(2) 0.0436(11) Uani 1 1 d . . . H3 H -0.0470 1.2115 0.3914 0.052 Uiso 1 1 calc R . . C4 C 0.1023(3) 1.1874(3) 0.41755(18) 0.0334(9) Uani 1 1 d . . . H4 H 0.1105 1.2178 0.4513 0.040 Uiso 1 1 calc R . . C29 C 0.2952(3) 1.2320(3) 0.48119(16) 0.0310(9) Uani 1 1 d . . . H29A H 0.2693 1.2896 0.4633 0.047 Uiso 1 1 calc R . . H29B H 0.3635 1.2415 0.5014 0.047 Uiso 1 1 calc R . . H29C H 0.2544 1.2130 0.5060 0.047 Uiso 1 1 calc R . . C20 C 0.3628(2) 1.1827(2) 0.39909(14) 0.0212(7) Uani 1 1 d . . . C16 C 0.4314(3) 1.1441(3) 0.32503(15) 0.0263(8) Uani 1 1 d . . . H16 H 0.4375 1.1015 0.2977 0.032 Uiso 1 1 calc R . . C17 C 0.4805(3) 1.2290(3) 0.32692(17) 0.0327(9) Uani 1 1 d . . . H17 H 0.5196 1.2430 0.3019 0.039 Uiso 1 1 calc R . . C18 C 0.4703(3) 1.2930(3) 0.36673(18) 0.0360(10) Uani 1 1 d . . . H18 H 0.5033 1.3508 0.3694 0.043 Uiso 1 1 calc R . . C19 C 0.4103(3) 1.2699(3) 0.40271(17) 0.0304(9) Uani 1 1 d . . . H19 H 0.4018 1.3128 0.4294 0.037 Uiso 1 1 calc R . . N6 N 0.2749(2) 1.0046(2) 0.27414(13) 0.0248(7) Uani 1 1 d . . . C30 C 0.2541(3) 0.9994(2) 0.22672(15) 0.0220(7) Uani 1 1 d . . . C31 C 0.3556(3) 1.0081(3) 0.14514(19) 0.0368(10) Uani 1 1 d . . . N12 N 0.4381(3) 1.0203(3) 0.1435(3) 0.0757(17) Uani 1 1 d . . . C44 C 0.1698(3) 0.8909(2) 0.04760(14) 0.0225(7) Uani 1 1 d . . . C45 C 0.2076(3) 0.8202(2) 0.08959(14) 0.0200(7) Uani 1 1 d . . . N7 N 0.2321(2) 0.85307(19) 0.14256(11) 0.0191(6) Uani 1 1 d . . . C48 C 0.3226(3) 0.6712(2) 0.24958(15) 0.0245(8) Uani 1 1 d . . . H48 H 0.3454 0.6608 0.2871 0.029 Uiso 1 1 calc R . . C49 C 0.3156(3) 0.5947(2) 0.21330(16) 0.0274(8) Uani 1 1 d . . . H49 H 0.3341 0.5351 0.2274 0.033 Uiso 1 1 calc R . . C50 C 0.2819(3) 0.6060(2) 0.15725(15) 0.0237(8) Uani 1 1 d . . . H50 H 0.2761 0.5548 0.1336 0.028 Uiso 1 1 calc R . . C51 C 0.2567(2) 0.6968(2) 0.13708(14) 0.0203(7) Uani 1 1 d . . . C43 C 0.1349(3) 0.8794(3) -0.00867(14) 0.0266(8) Uani 1 1 d . . . H43 H 0.1307 0.8200 -0.0246 0.032 Uiso 1 1 calc R . . C42 C 0.1060(3) 0.9597(3) -0.04068(15) 0.0312(9) Uani 1 1 d . . . H42 H 0.0842 0.9540 -0.0786 0.037 Uiso 1 1 calc R . . C41 C 0.1096(3) 1.0477(3) -0.01642(15) 0.0300(8) Uani 1 1 d . . . H41 H 0.0903 1.1011 -0.0377 0.036 Uiso 1 1 calc R . . C40 C 0.1425(3) 1.0547(3) 0.04032(15) 0.0245(8) Uani 1 1 d . . . C39 C 0.1488(3) 1.1366(2) 0.07617(15) 0.0238(8) Uani 1 1 d . . . C33 C 0.1972(3) 1.2300(3) 0.21208(16) 0.0258(8) Uani 1 1 d . . . H33 H 0.2181 1.1860 0.2399 0.031 Uiso 1 1 calc R . . C34 C 0.1862(3) 1.3241(3) 0.22394(18) 0.0320(9) Uani 1 1 d . . . H34 H 0.1996 1.3437 0.2604 0.038 Uiso 1 1 calc R . . C35 C 0.1549(3) 1.3903(3) 0.18170(19) 0.0353(10) Uani 1 1 d . . . H35 H 0.1480 1.4529 0.1910 0.042 Uiso 1 1 calc R . . C36 C 0.1341(3) 1.3656(3) 0.12683(18) 0.0352(10) Uani 1 1 d . . . H36 H 0.1144 1.4104 0.0993 0.042 Uiso 1 1 calc R . . C37 C 0.1437(3) 1.2698(2) 0.11397(16) 0.0257(8) Uani 1 1 d . . . N13 N -0.0016(3) 0.9515(3) 0.16937(15) 0.0408(9) Uani 1 1 d . . . O1 O 0.1641(3) 0.6425(3) 0.98012(13) 0.0560(9) Uani 1 1 d . . . H1A H 0.1863 0.6601 1.0119 0.084 Uiso 1 1 calc R . . O2A O -0.2060(3) 0.8871(3) 0.13687(19) 0.0562(16) Uani 0.759(8) 1 d P A 1 C1S C 0.0918(4) 0.5757(4) 0.9793(3) 0.0704(17) Uani 1 1 d . . . H1S1 H 0.1163 0.5297 1.0073 0.106 Uiso 1 1 calc R . . H1S2 H 0.0762 0.5456 0.9439 0.106 Uiso 1 1 calc R . . H1S3 H 0.0320 0.6048 0.9860 0.106 Uiso 1 1 calc R . . C2S C -0.2645(5) 0.9713(4) 0.1472(3) 0.0739(18) Uani 1 1 d . . . O2B O -0.3647(11) 1.0283(12) 0.1228(8) 0.075(6) Uani 0.241(8) 1 d P A 2 C3S C 0.5000 0.5000 0.5000 0.273(16) Uani 1 2 d SDU . . O3B O 0.4884(18) 0.5140(14) 0.4396(8) 0.105(7) Uani 0.25 1 d PU B 2 O3A O 0.4168(19) 0.451(2) 0.5170(11) 0.144(12) Uani 0.25 1 d PDU B 1 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 0.0164(2) 0.0154(2) 0.0146(2) -0.00215(17) 0.00137(17) 0.00053(17) Fe1 0.0212(3) 0.0153(2) 0.0176(3) -0.00003(19) 0.00221(19) 0.00152(19) N11 0.0338(17) 0.0258(16) 0.0330(18) 0.0118(14) 0.0109(14) 0.0032(14) N4 0.0149(13) 0.0223(15) 0.0208(15) -0.0030(12) 0.0047(11) 0.0007(11) N1 0.0167(14) 0.0196(14) 0.0204(15) -0.0040(11) 0.0035(11) 0.0003(11) N5 0.0123(13) 0.0206(14) 0.0184(14) -0.0029(11) 0.0053(11) -0.0026(11) N2 0.0185(14) 0.0219(15) 0.0242(16) -0.0005(12) 0.0016(12) 0.0017(12) N3 0.0158(13) 0.0214(14) 0.0213(15) 0.0030(12) 0.0051(11) 0.0038(11) N9 0.0205(14) 0.0226(15) 0.0198(15) 0.0019(12) 0.0053(12) 0.0015(12) C46 0.0162(15) 0.0172(16) 0.0216(18) 0.0007(13) 0.0065(13) -0.0002(13) C47 0.0241(17) 0.0190(17) 0.0218(18) -0.0031(14) 0.0054(14) -0.0010(14) N8 0.0241(15) 0.0222(15) 0.0196(15) -0.0040(12) 0.0064(12) -0.0038(12) N10 0.0210(14) 0.0200(14) 0.0212(15) 0.0025(12) 0.0066(12) 0.0011(12) C38 0.0176(16) 0.0174(17) 0.035(2) 0.0011(15) 0.0108(15) -0.0018(13) C32 0.031(2) 0.0242(18) 0.0161(18) 0.0026(14) 0.0033(15) -0.0005(15) C11 0.0209(17) 0.0221(17) 0.0201(18) -0.0037(14) 0.0088(14) -0.0003(14) C12 0.031(2) 0.0253(19) 0.025(2) -0.0019(15) 0.0096(16) -0.0060(15) C13 0.031(2) 0.031(2) 0.035(2) -0.0091(17) 0.0134(17) -0.0149(17) C14 0.0168(17) 0.038(2) 0.035(2) -0.0116(18) 0.0018(15) -0.0039(16) C15 0.0185(17) 0.0291(19) 0.030(2) -0.0029(16) 0.0010(15) 0.0035(15) C26 0.0227(17) 0.0175(16) 0.0192(17) 0.0011(13) 0.0045(14) -0.0017(14) C10 0.0157(16) 0.0198(17) 0.0218(18) -0.0038(14) 0.0011(13) -0.0013(13) C6 0.0286(19) 0.0252(19) 0.030(2) -0.0022(16) 0.0139(16) -0.0031(15) C7 0.0258(19) 0.030(2) 0.044(2) -0.0101(18) 0.0174(17) -0.0028(16) C8 0.0234(18) 0.0248(19) 0.047(2) -0.0095(17) 0.0102(17) 0.0053(15) C9 0.0226(18) 0.0205(18) 0.037(2) -0.0020(16) 0.0015(16) 0.0008(15) C27 0.031(2) 0.0256(19) 0.029(2) 0.0061(16) 0.0044(16) -0.0002(16) C25 0.0121(15) 0.0267(18) 0.0200(18) -0.0016(14) 0.0030(13) -0.0015(13) C21 0.0156(16) 0.0271(18) 0.0201(18) -0.0058(14) 0.0085(13) -0.0046(14) C22 0.0232(18) 0.037(2) 0.0196(19) -0.0111(16) 0.0054(15) -0.0057(16) C23 0.0226(18) 0.044(2) 0.0151(18) -0.0009(16) 0.0015(14) -0.0057(16) C24 0.0242(18) 0.034(2) 0.0191(19) 0.0040(15) 0.0023(15) 0.0000(16) C28 0.0194(17) 0.0224(17) 0.0251(19) -0.0077(14) 0.0081(14) -0.0021(14) C5 0.0201(17) 0.0179(17) 0.0280(19) -0.0023(14) 0.0071(14) -0.0008(14) C1 0.0271(19) 0.0273(19) 0.029(2) 0.0006(16) -0.0023(16) -0.0010(16) C2 0.0178(18) 0.032(2) 0.052(3) -0.0018(19) -0.0042(17) 0.0021(16) C3 0.0187(19) 0.045(3) 0.068(3) -0.015(2) 0.012(2) 0.0049(18) C4 0.026(2) 0.032(2) 0.044(2) -0.0106(18) 0.0123(17) -0.0005(16) C29 0.029(2) 0.032(2) 0.032(2) -0.0162(17) 0.0078(16) -0.0002(16) C20 0.0168(16) 0.0193(17) 0.0267(19) -0.0025(14) 0.0032(14) 0.0029(13) C16 0.0229(18) 0.031(2) 0.0264(19) 0.0051(16) 0.0084(15) 0.0045(15) C17 0.0272(19) 0.035(2) 0.038(2) 0.0138(18) 0.0123(17) 0.0040(17) C18 0.0235(19) 0.027(2) 0.056(3) 0.0075(19) 0.0053(18) -0.0062(16) C19 0.0274(19) 0.0221(18) 0.041(2) -0.0027(16) 0.0051(17) -0.0012(15) N6 0.0288(16) 0.0171(15) 0.0244(18) -0.0040(12) -0.0024(13) 0.0059(12) C30 0.0247(18) 0.0148(16) 0.025(2) -0.0014(14) 0.0017(14) 0.0041(14) C31 0.031(2) 0.0180(19) 0.061(3) -0.0061(18) 0.0095(19) -0.0036(16) N12 0.034(2) 0.030(2) 0.167(6) -0.014(3) 0.031(3) -0.0001(18) C44 0.0221(17) 0.0259(18) 0.0210(18) 0.0011(14) 0.0083(14) -0.0004(14) C45 0.0224(17) 0.0216(17) 0.0161(17) -0.0018(14) 0.0046(13) -0.0023(14) N7 0.0230(14) 0.0177(14) 0.0160(14) -0.0011(11) 0.0031(11) 0.0005(11) C48 0.0288(19) 0.0239(18) 0.0206(18) 0.0031(14) 0.0052(15) 0.0015(15) C49 0.032(2) 0.0176(17) 0.034(2) 0.0020(15) 0.0104(16) 0.0010(15) C50 0.0258(18) 0.0181(17) 0.029(2) -0.0034(14) 0.0106(15) -0.0022(14) C51 0.0176(16) 0.0208(17) 0.0233(18) -0.0024(14) 0.0064(14) -0.0016(13) C43 0.0270(19) 0.034(2) 0.0190(19) -0.0016(15) 0.0063(15) 0.0014(16) C42 0.032(2) 0.044(2) 0.0171(19) 0.0039(17) 0.0036(15) 0.0045(18) C41 0.031(2) 0.038(2) 0.022(2) 0.0090(16) 0.0067(16) 0.0030(17) C40 0.0245(18) 0.0276(19) 0.0230(19) 0.0077(15) 0.0085(15) 0.0027(15) C39 0.0228(18) 0.0253(18) 0.0245(19) 0.0079(15) 0.0076(15) 0.0016(15) C33 0.0226(18) 0.0218(18) 0.033(2) -0.0021(15) 0.0056(15) -0.0013(14) C34 0.0268(19) 0.026(2) 0.043(2) -0.0087(17) 0.0061(17) -0.0029(16) C35 0.032(2) 0.0171(18) 0.058(3) -0.0027(18) 0.0124(19) -0.0013(16) C36 0.032(2) 0.0197(19) 0.052(3) 0.0107(18) 0.0067(19) 0.0020(16) C37 0.0218(18) 0.0219(18) 0.034(2) 0.0055(16) 0.0083(15) -0.0013(14) N13 0.033(2) 0.054(2) 0.036(2) 0.0124(17) 0.0075(16) -0.0002(17) O1 0.057(2) 0.073(2) 0.0393(19) -0.0164(18) 0.0136(16) -0.0123(18) O2A 0.049(3) 0.064(3) 0.055(3) -0.012(2) 0.012(2) -0.015(2) C1S 0.055(3) 0.073(4) 0.082(4) -0.035(3) 0.015(3) -0.028(3) C2S 0.075(4) 0.046(3) 0.084(4) 0.020(3) -0.016(3) -0.008(3) O2B 0.044(9) 0.076(12) 0.102(14) 0.041(10) 0.007(8) -0.006(8) C3S 0.49(4) 0.102(14) 0.157(19) 0.032(13) -0.08(3) 0.08(2) O3B 0.141(18) 0.076(12) 0.076(13) -0.028(10) -0.022(12) 0.027(12) O3A 0.17(2) 0.14(2) 0.103(18) 0.031(16) -0.013(16) -0.081(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N6 1.923(3) . ? Co1 N5 1.958(3) . ? Co1 N3 1.999(3) . ? Co1 N4 2.001(3) . ? Co1 N2 2.228(3) . ? Co1 N1 2.242(3) . ? Fe1 C30 1.890(4) . ? Fe1 N9 1.928(3) . ? Fe1 N10 1.929(3) . ? Fe1 N7 1.945(3) . ? Fe1 C32 1.977(4) . ? Fe1 C31 1.978(4) . ? N11 C39 1.328(5) . ? N11 C37 1.390(5) . ? N4 C11 1.344(4) . ? N4 C15 1.354(4) . ? N1 C6 1.341(4) . ? N1 C10 1.349(4) . ? N5 C25 1.356(4) . ? N5 C21 1.362(4) . ? N2 C5 1.348(4) . ? N2 C1 1.349(5) . ? N3 C16 1.350(4) . ? N3 C20 1.353(4) . ? N9 C44 1.342(4) . ? N9 C40 1.351(4) . ? C46 N7 1.383(4) . ? C46 C47 1.403(5) . ? C46 C51 1.421(5) . ? C47 C48 1.382(5) . ? C47 H47 0.9300 . ? N8 C45 1.332(4) . ? N8 C51 1.386(4) . ? N10 C39 1.376(4) . ? N10 C38 1.377(4) . ? C38 C33 1.402(5) . ? C38 C37 1.411(5) . ? C32 N13 1.147(5) . ? C11 C12 1.392(5) . ? C11 C26 1.540(5) . ? C12 C13 1.377(5) . ? C12 H12 0.9300 . ? C13 C14 1.383(6) . ? C13 H13 0.9300 . ? C14 C15 1.377(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C26 C27 1.542(5) . ? C26 C10 1.545(5) . ? C26 C25 1.547(5) . ? C10 C9 1.395(5) . ? C6 C7 1.383(5) . ? C6 H6 0.9300 . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C25 C24 1.386(5) . ? C21 C22 1.388(5) . ? C21 C28 1.541(5) . ? C22 C23 1.370(6) . ? C22 H22 0.9300 . ? C23 C24 1.374(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C28 C29 1.545(5) . ? C28 C5 1.546(5) . ? C28 C20 1.549(5) . ? C5 C4 1.384(5) . ? C1 C2 1.382(5) . ? C1 H1 0.9300 . ? C2 C3 1.376(6) . ? C2 H2 0.9300 . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C20 C19 1.392(5) . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.377(6) . ? C17 H17 0.9300 . ? C18 C19 1.383(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? N6 C30 1.155(5) . ? C31 N12 1.145(6) . ? C44 C43 1.386(5) . ? C44 C45 1.458(5) . ? C45 N7 1.370(4) . ? C48 C49 1.403(5) . ? C48 H48 0.9300 . ? C49 C50 1.379(5) . ? C49 H49 0.9300 . ? C50 C51 1.400(5) . ? C50 H50 0.9300 . ? C43 C42 1.397(5) . ? C43 H43 0.9300 . ? C42 C41 1.385(6) . ? C42 H42 0.9300 . ? C41 C40 1.389(5) . ? C41 H41 0.9300 . ? C40 C39 1.459(5) . ? C33 C34 1.384(5) . ? C33 H33 0.9300 . ? C34 C35 1.405(6) . ? C34 H34 0.9300 . ? C35 C36 1.380(6) . ? C35 H35 0.9300 . ? C36 C37 1.411(5) . ? C36 H36 0.9300 . ? O1 C1S 1.363(6) . ? O1 H1A 0.8200 . ? O2A C2S 1.491(8) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2S O2B 1.583(16) . ? C3S O3A 1.474(16) 3_666 ? C3S O3A 1.474(16) . ? C3S O3B 1.49(2) 3_666 ? C3S O3B 1.49(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 N6 Co1 N5 176.56(12) . . ? N6 Co1 N3 91.02(12) . . ? N5 Co1 N3 89.99(11) . . ? N6 Co1 N4 90.02(12) . . ? N5 Co1 N4 89.13(11) . . ? N3 Co1 N4 177.05(11) . . ? N6 Co1 N2 92.47(11) . . ? N5 Co1 N2 90.94(11) . . ? N3 Co1 N2 80.80(11) . . ? N4 Co1 N2 96.40(11) . . ? N6 Co1 N1 89.35(11) . . ? N5 Co1 N1 87.24(11) . . ? N3 Co1 N1 98.91(10) . . ? N4 Co1 N1 83.86(10) . . ? N2 Co1 N1 178.16(10) . . ? C30 Fe1 N9 179.46(14) . . ? C30 Fe1 N10 98.76(13) . . ? N9 Fe1 N10 81.10(12) . . ? C30 Fe1 N7 99.26(13) . . ? N9 Fe1 N7 80.86(12) . . ? N10 Fe1 N7 161.94(12) . . ? C30 Fe1 C32 86.51(15) . . ? N9 Fe1 C32 92.97(13) . . ? N10 Fe1 C32 90.30(13) . . ? N7 Fe1 C32 89.65(13) . . ? C30 Fe1 C31 88.95(17) . . ? N9 Fe1 C31 91.58(16) . . ? N10 Fe1 C31 91.98(14) . . ? N7 Fe1 C31 89.50(14) . . ? C32 Fe1 C31 175.19(17) . . ? C39 N11 C37 102.7(3) . . ? C11 N4 C15 118.3(3) . . ? C11 N4 Co1 121.3(2) . . ? C15 N4 Co1 120.4(2) . . ? C6 N1 C10 118.1(3) . . ? C6 N1 Co1 124.5(2) . . ? C10 N1 Co1 117.0(2) . . ? C25 N5 C21 119.2(3) . . ? C25 N5 Co1 120.3(2) . . ? C21 N5 Co1 120.2(2) . . ? C5 N2 C1 117.9(3) . . ? C5 N2 Co1 114.9(2) . . ? C1 N2 Co1 126.0(2) . . ? C16 N3 C20 118.1(3) . . ? C16 N3 Co1 121.3(2) . . ? C20 N3 Co1 120.3(2) . . ? C44 N9 C40 122.3(3) . . ? C44 N9 Fe1 119.0(2) . . ? C40 N9 Fe1 118.7(2) . . ? N7 C46 C47 131.7(3) . . ? N7 C46 C51 107.0(3) . . ? C47 C46 C51 121.3(3) . . ? C48 C47 C46 117.1(3) . . ? C48 C47 H47 121.5 . . ? C46 C47 H47 121.5 . . ? C45 N8 C51 103.6(3) . . ? C39 N10 C38 104.3(3) . . ? C39 N10 Fe1 114.9(2) . . ? C38 N10 Fe1 140.8(2) . . ? N10 C38 C33 131.6(3) . . ? N10 C38 C37 106.7(3) . . ? C33 C38 C37 121.8(3) . . ? N13 C32 Fe1 176.4(3) . . ? N4 C11 C12 120.4(3) . . ? N4 C11 C26 117.3(3) . . ? C12 C11 C26 122.2(3) . . ? C13 C12 C11 121.1(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 118.3(3) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 118.3(3) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N4 C15 C14 123.5(4) . . ? N4 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C11 C26 C27 109.8(3) . . ? C11 C26 C10 107.2(3) . . ? C27 C26 C10 109.5(3) . . ? C11 C26 C25 111.6(3) . . ? C27 C26 C25 109.4(3) . . ? C10 C26 C25 109.3(3) . . ? N1 C10 C9 121.3(3) . . ? N1 C10 C26 116.1(3) . . ? C9 C10 C26 122.6(3) . . ? N1 C6 C7 123.7(4) . . ? N1 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C8 C7 C6 118.2(3) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C25 C24 120.9(3) . . ? N5 C25 C26 118.4(3) . . ? C24 C25 C26 120.7(3) . . ? N5 C21 C22 120.9(3) . . ? N5 C21 C28 117.7(3) . . ? C22 C21 C28 121.4(3) . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 119.5(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C21 C28 C29 110.1(3) . . ? C21 C28 C5 110.7(3) . . ? C29 C28 C5 108.8(3) . . ? C21 C28 C20 108.9(3) . . ? C29 C28 C20 109.6(3) . . ? C5 C28 C20 108.8(3) . . ? N2 C5 C4 121.6(3) . . ? N2 C5 C28 115.9(3) . . ? C4 C5 C28 122.4(3) . . ? N2 C1 C2 123.2(4) . . ? N2 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C20 C19 120.7(3) . . ? N3 C20 C28 117.1(3) . . ? C19 C20 C28 122.1(3) . . ? N3 C16 C17 123.5(4) . . ? N3 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C16 C17 C18 118.5(4) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C30 N6 Co1 172.0(3) . . ? N6 C30 Fe1 177.1(3) . . ? N12 C31 Fe1 179.0(5) . . ? N9 C44 C43 120.5(3) . . ? N9 C44 C45 110.4(3) . . ? C43 C44 C45 129.1(3) . . ? N8 C45 N7 115.7(3) . . ? N8 C45 C44 129.0(3) . . ? N7 C45 C44 115.3(3) . . ? C45 N7 C46 104.3(3) . . ? C45 N7 Fe1 114.4(2) . . ? C46 N7 Fe1 141.4(2) . . ? C47 C48 C49 121.8(3) . . ? C47 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C50 C49 C48 121.5(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C51 118.0(3) . . ? C49 C50 H50 121.0 . . ? C51 C50 H50 121.0 . . ? N8 C51 C50 130.3(3) . . ? N8 C51 C46 109.5(3) . . ? C50 C51 C46 120.2(3) . . ? C44 C43 C42 118.1(4) . . ? C44 C43 H43 121.0 . . ? C42 C43 H43 121.0 . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C41 C40 118.8(3) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? N9 C40 C41 119.7(3) . . ? N9 C40 C39 110.2(3) . . ? C41 C40 C39 130.1(3) . . ? N11 C39 N10 115.8(3) . . ? N11 C39 C40 129.1(3) . . ? N10 C39 C40 115.0(3) . . ? C34 C33 C38 117.5(4) . . ? C34 C33 H33 121.3 . . ? C38 C33 H33 121.3 . . ? C33 C34 C35 121.0(4) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C36 C35 C34 122.2(4) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C35 C36 C37 117.6(4) . . ? C35 C36 H36 121.2 . . ? C37 C36 H36 121.2 . . ? N11 C37 C38 110.5(3) . . ? N11 C37 C36 129.5(3) . . ? C38 C37 C36 120.0(4) . . ? C1S O1 H1A 109.5 . . ? O1 C1S H1S1 109.5 . . ? O1 C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1 C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2A C2S O2B 142.2(9) . . ? O3A C3S O3A 180.0(17) 3_666 . ? O3A C3S O3B 116.3(14) 3_666 3_666 ? O3A C3S O3B 63.7(14) . 3_666 ? O3A C3S O3B 63.7(14) 3_666 . ? O3A C3S O3B 116.3(14) . . ? O3B C3S O3B 180.0(3) 3_666 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.792 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.085 data_compound_[FeCo]370K _database_code_depnum_ccdc_archive 'CCDC 898149' #TrackingRef 'web_deposit_cif_file_3_DechambenoitPierre_1347283466.[FeCo]370K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C51 H36 Co Fe N13), 5(C H4 O)' _chemical_formula_sum 'C107 H92 Co2 Fe2 N26 O5' _chemical_formula_weight 2051.63 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' 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 13.6545(15) _cell_length_b 14.3480(17) _cell_length_c 25.328(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.313(5) _cell_angle_gamma 90.00 _cell_volume 4847.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 370(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 25.29 _exptl_crystal_description square _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8613 _exptl_absorpt_correction_T_max 0.9333 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 370(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43392 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.38 _reflns_number_total 8774 _reflns_number_gt 7005 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'AUTOSTRUCTURE (Bruker)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material 'WINGX (Farrugia)' _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^ > 2\s(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.All non-hydrogens were refined anisotropically. Hydrogen atoms were assigned to ideal positions and refined isotropically using a riding model. Two crystallographically independent methanol molecule were found to have positional disorder. The methanol molecule bearing C2S was refined using DFIX constraint/restrain. Hydrogen atoms for methanol molecules were not introduced, but are taken into account in the compound formula. ; _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^)+(0.0533P)^2^+6.5157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8774 _refine_ls_number_parameters 657 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.007 _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 0.69993(3) -0.00056(3) 0.149728(15) 0.03194(12) Uani 1 1 d . . . Fe1 Fe 0.78676(3) 0.00785(3) 0.352551(17) 0.03599(13) Uani 1 1 d . . . N5 N 0.67085(18) 0.01660(18) 0.06704(10) 0.0354(6) Uani 1 1 d . . . N1 N 0.57522(18) 0.09613(17) 0.14826(10) 0.0383(6) Uani 1 1 d . . . N7 N 0.7695(2) 0.14171(17) 0.35909(10) 0.0377(6) Uani 1 1 d . . . N2 N 0.82186(19) -0.09457(19) 0.14234(11) 0.0438(6) Uani 1 1 d . . . N3 N 0.62049(19) -0.12728(18) 0.13734(11) 0.0397(6) Uani 1 1 d . . . N4 N 0.78343(18) 0.12335(18) 0.15590(10) 0.0395(6) Uani 1 1 d . . . C10 C 0.5699(2) 0.1742(2) 0.11860(13) 0.0390(7) Uani 1 1 d . . . N6 N 0.7217(2) -0.01147(19) 0.23048(12) 0.0484(7) Uani 1 1 d . . . C30 C 0.7446(2) -0.0046(2) 0.27671(14) 0.0397(7) Uani 1 1 d . . . N9 N 0.8300(2) 0.02000(19) 0.43014(10) 0.0407(6) Uani 1 1 d . . . C45 C 0.7950(2) 0.1746(2) 0.41091(13) 0.0418(7) Uani 1 1 d . . . N8 N 0.7832(2) 0.26538(19) 0.41690(11) 0.0453(7) Uani 1 1 d . . . C46 C 0.7475(2) 0.2959(2) 0.36428(13) 0.0408(7) Uani 1 1 d . . . C47 C 0.7391(2) 0.2199(2) 0.32836(12) 0.0366(7) Uani 1 1 d . . . N10 N 0.8205(2) -0.12072(18) 0.37043(11) 0.0417(6) Uani 1 1 d . . . C25 C 0.6436(2) 0.1009(2) 0.04528(12) 0.0406(7) Uani 1 1 d . . . C24 C 0.6096(3) 0.1105(3) -0.01008(14) 0.0548(9) Uani 1 1 d . . . H24 H 0.5906 0.1688 -0.0248 0.066 Uiso 1 1 calc R . . C23 C 0.6040(3) 0.0340(3) -0.04322(14) 0.0620(11) Uani 1 1 d . . . H23 H 0.5794 0.0399 -0.0802 0.074 Uiso 1 1 calc R . . C22 C 0.6345(3) -0.0495(3) -0.02150(15) 0.0597(10) Uani 1 1 d . . . H22 H 0.6328 -0.1014 -0.0437 0.072 Uiso 1 1 calc R . . C21 C 0.6689(2) -0.0585(2) 0.03476(13) 0.0437(8) Uani 1 1 d . . . C28 C 0.7046(2) -0.1528(2) 0.06130(14) 0.0455(8) Uani 1 1 d . . . C5 C 0.8114(3) -0.1440(2) 0.09659(15) 0.0473(8) Uani 1 1 d . . . C4 C 0.8931(3) -0.1868(3) 0.0830(2) 0.0754(13) Uani 1 1 d . . . H4 H 0.8865 -0.2170 0.0499 0.090 Uiso 1 1 calc R . . C3 C 0.9843(3) -0.1845(4) 0.1186(3) 0.0947(17) Uani 1 1 d . . . H3 H 1.0397 -0.2131 0.1096 0.114 Uiso 1 1 calc R . . C2 C 0.9939(3) -0.1403(3) 0.1672(2) 0.0755(13) Uani 1 1 d . . . H2 H 1.0543 -0.1407 0.1925 0.091 Uiso 1 1 calc R . . C1 C 0.9107(3) -0.0951(3) 0.17754(17) 0.0591(10) Uani 1 1 d . . . H1 H 0.9164 -0.0637 0.2102 0.071 Uiso 1 1 calc R . . C20 C 0.6332(2) -0.1852(2) 0.09771(14) 0.0434(8) Uani 1 1 d . . . C19 C 0.5855(3) -0.2712(3) 0.09082(18) 0.0627(11) Uani 1 1 d . . . H19 H 0.5936 -0.3101 0.0627 0.075 Uiso 1 1 calc R . . C18 C 0.5265(3) -0.2986(3) 0.1257(2) 0.0743(13) Uani 1 1 d . . . H18 H 0.4941 -0.3560 0.1213 0.089 Uiso 1 1 calc R . . C17 C 0.5159(3) -0.2403(3) 0.16693(19) 0.0681(12) Uani 1 1 d . . . H17 H 0.4769 -0.2576 0.1913 0.082 Uiso 1 1 calc R . . C16 C 0.5637(3) -0.1564(3) 0.17158(15) 0.0525(9) Uani 1 1 d . . . H16 H 0.5568 -0.1173 0.1998 0.063 Uiso 1 1 calc R . . C29 C 0.7049(3) -0.2269(3) 0.01694(18) 0.0726(12) Uani 1 1 d . . . H29A H 0.7479 -0.2066 -0.0063 0.109 Uiso 1 1 calc R . . H29B H 0.6380 -0.2351 -0.0039 0.109 Uiso 1 1 calc R . . H29C H 0.7291 -0.2850 0.0335 0.109 Uiso 1 1 calc R . . C26 C 0.6491(2) 0.1856(2) 0.08353(13) 0.0420(7) Uani 1 1 d . . . C11 C 0.7526(2) 0.1950(2) 0.12242(12) 0.0392(7) Uani 1 1 d . . . C12 C 0.8093(3) 0.2753(3) 0.12584(15) 0.0559(9) Uani 1 1 d . . . H12 H 0.7877 0.3244 0.1022 0.067 Uiso 1 1 calc R . . C13 C 0.8979(3) 0.2836(3) 0.16407(17) 0.0647(11) Uani 1 1 d . . . H13 H 0.9365 0.3374 0.1659 0.078 Uiso 1 1 calc R . . C14 C 0.9277(3) 0.2114(3) 0.19908(17) 0.0617(11) Uani 1 1 d . . . H14 H 0.9863 0.2151 0.2256 0.074 Uiso 1 1 calc R . . C15 C 0.8687(3) 0.1337(3) 0.19389(15) 0.0540(9) Uani 1 1 d . . . H15 H 0.8884 0.0849 0.2180 0.065 Uiso 1 1 calc R . . C27 C 0.6267(3) 0.2752(3) 0.04958(16) 0.0636(11) Uani 1 1 d . . . H27A H 0.6335 0.3283 0.0732 0.095 Uiso 1 1 calc R . . H27B H 0.5596 0.2727 0.0283 0.095 Uiso 1 1 calc R . . H27C H 0.6732 0.2805 0.0261 0.095 Uiso 1 1 calc R . . C6 C 0.5104(3) 0.0848(3) 0.18062(15) 0.0525(9) Uani 1 1 d . . . H6 H 0.5154 0.0316 0.2020 0.063 Uiso 1 1 calc R . . C7 C 0.4358(3) 0.1493(3) 0.18349(19) 0.0665(11) Uani 1 1 d . . . H7 H 0.3899 0.1382 0.2051 0.080 Uiso 1 1 calc R . . C8 C 0.4313(3) 0.2292(3) 0.15401(19) 0.0680(12) Uani 1 1 d . . . H8 H 0.3832 0.2742 0.1559 0.082 Uiso 1 1 calc R . . C9 C 0.4988(3) 0.2424(3) 0.12145(16) 0.0558(9) Uani 1 1 d . . . H9 H 0.4969 0.2969 0.1013 0.067 Uiso 1 1 calc R . . C32 C 0.6478(3) -0.0134(2) 0.35948(17) 0.0556(9) Uani 1 1 d . . . N13 N 0.5669(3) -0.0247(3) 0.3634(2) 0.1019(16) Uani 1 1 d . . . C44 C 0.8319(3) 0.1049(2) 0.45250(13) 0.0444(8) Uani 1 1 d . . . C48 C 0.7056(2) 0.2318(2) 0.27279(13) 0.0436(8) Uani 1 1 d . . . H48 H 0.7004 0.1815 0.2492 0.052 Uiso 1 1 calc R . . C49 C 0.6804(3) 0.3211(2) 0.25409(15) 0.0539(9) Uani 1 1 d . . . H49 H 0.6572 0.3310 0.2173 0.065 Uiso 1 1 calc R . . C50 C 0.6892(3) 0.3970(2) 0.28967(16) 0.0566(9) Uani 1 1 d . . . H50 H 0.6720 0.4563 0.2759 0.068 Uiso 1 1 calc R . . C51 C 0.7228(3) 0.3858(2) 0.34456(15) 0.0520(9) Uani 1 1 d . . . H51 H 0.7290 0.4366 0.3678 0.062 Uiso 1 1 calc R . . C43 C 0.8662(3) 0.1165(3) 0.50779(14) 0.0564(10) Uani 1 1 d . . . H43 H 0.8702 0.1754 0.5235 0.068 Uiso 1 1 calc R . . C42 C 0.8945(3) 0.0371(3) 0.53887(14) 0.0616(10) Uani 1 1 d . . . H42 H 0.9163 0.0428 0.5761 0.074 Uiso 1 1 calc R . . C41 C 0.8908(3) -0.0491(3) 0.51571(14) 0.0580(10) Uani 1 1 d . . . H41 H 0.9096 -0.1016 0.5369 0.070 Uiso 1 1 calc R . . C40 C 0.8584(3) -0.0574(3) 0.45993(13) 0.0470(8) Uani 1 1 d . . . C39 C 0.8519(3) -0.1379(2) 0.42502(14) 0.0475(8) Uani 1 1 d . . . N11 N 0.8733(2) -0.2260(2) 0.43813(13) 0.0585(8) Uani 1 1 d . . . C38 C 0.8558(3) -0.2706(2) 0.38845(17) 0.0534(9) Uani 1 1 d . . . C33 C 0.8238(2) -0.2063(2) 0.34614(14) 0.0439(8) Uani 1 1 d . . . C34 C 0.8020(3) -0.2329(2) 0.29185(16) 0.0515(9) Uani 1 1 d . . . H34 H 0.7807 -0.1899 0.2643 0.062 Uiso 1 1 calc R . . C35 C 0.8135(3) -0.3260(3) 0.28088(19) 0.0629(11) Uani 1 1 d . . . H35 H 0.8003 -0.3460 0.2451 0.075 Uiso 1 1 calc R . . C36 C 0.8442(3) -0.3905(3) 0.3218(2) 0.0730(13) Uani 1 1 d . . . H36 H 0.8512 -0.4526 0.3126 0.088 Uiso 1 1 calc R . . C37 C 0.8644(3) -0.3658(3) 0.3754(2) 0.0691(12) Uani 1 1 d . . . H37 H 0.8832 -0.4102 0.4024 0.083 Uiso 1 1 calc R . . C31 C 0.9225(3) 0.0297(3) 0.33994(13) 0.0475(8) Uani 1 1 d . . . N12 N 0.9998(3) 0.0413(3) 0.33087(16) 0.0791(11) Uani 1 1 d . . . O1 O 0.8391(5) 0.3626(5) 0.5153(2) 0.190(3) Uani 1 1 d . . . C1S C 0.9127(6) 0.4199(6) 0.5194(4) 0.161(4) Uani 1 1 d . . . C2S C 1.2647(7) 0.0222(6) 0.3479(4) 0.148(3) Uani 1 1 d D . . O2 O 1.2081(6) 0.1029(7) 0.3602(3) 0.155(3) Uani 0.65 1 d PD A 1 C3S C 0.5000 0.5000 0.0000 0.40(3) Uani 1 2 d S . . O2B O 1.3557(14) -0.0349(14) 0.3692(8) 0.181(7) Uani 0.35 1 d P A 2 O3 O 0.4406(18) 0.4412(14) 0.0197(8) 0.272(9) Uani 0.50 1 d P . . 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 0.0334(2) 0.0323(2) 0.0293(2) -0.00305(16) 0.00489(16) 0.00182(16) Fe1 0.0415(3) 0.0336(2) 0.0324(2) 0.00175(18) 0.00684(19) 0.00336(18) N5 0.0327(13) 0.0431(15) 0.0308(13) -0.0030(11) 0.0075(10) -0.0027(11) N1 0.0340(13) 0.0372(14) 0.0445(15) -0.0050(12) 0.0101(12) 0.0009(11) N7 0.0448(15) 0.0341(14) 0.0334(14) -0.0005(11) 0.0067(11) 0.0021(11) N2 0.0353(15) 0.0435(15) 0.0514(17) -0.0029(13) 0.0067(13) 0.0035(12) N3 0.0346(14) 0.0399(15) 0.0465(15) 0.0024(12) 0.0129(12) 0.0020(11) N4 0.0317(14) 0.0430(15) 0.0421(15) -0.0033(12) 0.0039(11) -0.0003(11) C10 0.0331(16) 0.0344(16) 0.0456(18) -0.0023(14) -0.0002(14) 0.0006(13) N6 0.0632(19) 0.0402(16) 0.0372(16) -0.0045(12) 0.0008(13) 0.0079(13) C30 0.0455(18) 0.0320(16) 0.0401(19) -0.0026(14) 0.0059(14) 0.0053(13) N9 0.0440(15) 0.0456(16) 0.0331(14) 0.0042(12) 0.0097(12) 0.0013(12) C45 0.0442(18) 0.0456(19) 0.0363(17) -0.0047(14) 0.0099(14) -0.0038(14) N8 0.0500(16) 0.0432(16) 0.0438(16) -0.0099(13) 0.0125(13) -0.0049(13) C46 0.0388(17) 0.0390(18) 0.0471(19) -0.0053(14) 0.0146(15) -0.0042(13) C47 0.0371(16) 0.0321(16) 0.0423(17) -0.0006(13) 0.0121(14) -0.0006(12) N10 0.0447(15) 0.0367(14) 0.0446(15) 0.0069(12) 0.0115(12) 0.0023(12) C25 0.0341(16) 0.052(2) 0.0349(17) 0.0016(15) 0.0053(13) -0.0063(14) C24 0.054(2) 0.069(3) 0.0379(19) 0.0086(18) 0.0025(16) -0.0037(18) C23 0.058(2) 0.094(3) 0.0292(18) 0.001(2) -0.0015(16) -0.015(2) C22 0.058(2) 0.080(3) 0.041(2) -0.021(2) 0.0111(18) -0.020(2) C21 0.0380(17) 0.059(2) 0.0374(17) -0.0125(16) 0.0145(14) -0.0133(15) C28 0.0403(18) 0.0470(19) 0.052(2) -0.0186(16) 0.0161(15) -0.0043(14) C5 0.0441(19) 0.0399(18) 0.063(2) -0.0101(16) 0.0231(17) -0.0013(14) C4 0.048(2) 0.077(3) 0.106(4) -0.032(3) 0.027(2) 0.005(2) C3 0.046(3) 0.089(4) 0.154(5) -0.030(4) 0.032(3) 0.011(2) C2 0.038(2) 0.066(3) 0.116(4) -0.002(3) 0.002(2) 0.0068(19) C1 0.045(2) 0.055(2) 0.071(3) 0.0009(19) -0.0016(19) 0.0034(17) C20 0.0365(17) 0.0367(17) 0.057(2) -0.0048(15) 0.0104(15) 0.0009(13) C19 0.061(2) 0.039(2) 0.086(3) -0.0101(19) 0.013(2) -0.0095(17) C18 0.060(3) 0.048(2) 0.115(4) 0.012(2) 0.018(3) -0.0169(19) C17 0.053(2) 0.066(3) 0.092(3) 0.025(2) 0.029(2) -0.002(2) C16 0.047(2) 0.054(2) 0.061(2) 0.0099(18) 0.0228(18) 0.0027(16) C29 0.072(3) 0.072(3) 0.077(3) -0.044(2) 0.025(2) -0.005(2) C26 0.0458(19) 0.0379(17) 0.0402(18) 0.0083(14) 0.0045(14) 0.0002(14) C11 0.0420(17) 0.0397(17) 0.0375(17) -0.0011(14) 0.0121(14) -0.0046(14) C12 0.063(2) 0.052(2) 0.054(2) 0.0016(18) 0.0147(18) -0.0162(18) C13 0.061(3) 0.062(3) 0.073(3) -0.013(2) 0.020(2) -0.026(2) C14 0.0362(19) 0.073(3) 0.072(3) -0.021(2) 0.0044(18) -0.0111(18) C15 0.0419(19) 0.057(2) 0.059(2) -0.0051(18) 0.0013(17) 0.0024(16) C27 0.072(3) 0.050(2) 0.064(2) 0.0199(19) 0.004(2) 0.0015(19) C6 0.049(2) 0.047(2) 0.067(2) -0.0042(18) 0.0261(18) -0.0005(16) C7 0.050(2) 0.059(3) 0.099(3) -0.017(2) 0.037(2) -0.0016(18) C8 0.045(2) 0.057(3) 0.104(3) -0.015(2) 0.021(2) 0.0114(18) C9 0.046(2) 0.042(2) 0.075(3) -0.0002(18) 0.0044(19) 0.0079(16) C32 0.053(2) 0.0353(18) 0.080(3) -0.0030(17) 0.018(2) 0.0020(16) N13 0.057(2) 0.065(2) 0.192(5) -0.019(3) 0.045(3) -0.0035(19) C44 0.0472(19) 0.053(2) 0.0347(17) -0.0009(15) 0.0125(15) 0.0001(15) C48 0.0502(19) 0.0382(18) 0.0420(18) -0.0018(14) 0.0092(15) 0.0037(14) C49 0.067(2) 0.044(2) 0.051(2) 0.0075(17) 0.0121(18) 0.0036(17) C50 0.072(3) 0.0363(19) 0.064(2) 0.0080(17) 0.019(2) 0.0050(17) C51 0.059(2) 0.0358(18) 0.065(2) -0.0093(17) 0.0226(19) -0.0040(16) C43 0.062(2) 0.071(3) 0.0374(19) -0.0053(18) 0.0122(17) 0.0012(19) C42 0.065(2) 0.089(3) 0.0296(18) 0.003(2) 0.0070(17) 0.006(2) C41 0.062(2) 0.073(3) 0.039(2) 0.0198(19) 0.0113(17) 0.008(2) C40 0.0472(19) 0.055(2) 0.0410(19) 0.0140(16) 0.0137(15) 0.0029(16) C39 0.0455(19) 0.050(2) 0.049(2) 0.0170(17) 0.0142(16) 0.0047(15) N11 0.064(2) 0.0483(18) 0.065(2) 0.0245(16) 0.0162(16) 0.0042(15) C38 0.045(2) 0.0419(19) 0.074(3) 0.0182(19) 0.0157(18) -0.0003(15) C33 0.0372(17) 0.0349(17) 0.062(2) 0.0064(15) 0.0156(16) -0.0012(13) C34 0.047(2) 0.0416(19) 0.067(2) -0.0025(17) 0.0156(18) -0.0001(15) C35 0.056(2) 0.044(2) 0.089(3) -0.015(2) 0.017(2) -0.0042(17) C36 0.062(3) 0.035(2) 0.124(4) -0.005(2) 0.023(3) -0.0013(18) C37 0.065(3) 0.039(2) 0.100(4) 0.017(2) 0.009(2) -0.0016(18) C31 0.052(2) 0.053(2) 0.0370(18) 0.0080(15) 0.0082(16) 0.0037(16) N12 0.053(2) 0.106(3) 0.080(3) 0.025(2) 0.0184(19) 0.002(2) O1 0.146(5) 0.278(8) 0.151(5) -0.101(5) 0.043(4) 0.002(5) C1S 0.097(5) 0.136(6) 0.260(10) -0.077(6) 0.062(6) -0.065(5) C2S 0.152(7) 0.100(5) 0.179(8) 0.036(5) 0.006(6) 0.028(5) O2 0.114(6) 0.186(9) 0.164(7) -0.022(6) 0.024(5) -0.053(6) C3S 0.86(8) 0.092(11) 0.22(2) 0.085(13) 0.02(3) -0.04(2) O2B 0.152(14) 0.195(17) 0.200(17) 0.039(14) 0.045(12) -0.056(13) O3 0.38(3) 0.200(17) 0.24(2) -0.053(15) 0.076(18) 0.054(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N6 2.009(3) . ? Co1 N5 2.062(2) . ? Co1 N4 2.100(3) . ? Co1 N3 2.106(3) . ? Co1 N2 2.182(3) . ? Co1 N1 2.191(2) . ? Fe1 C30 1.892(3) . ? Fe1 N10 1.932(3) . ? Fe1 N9 1.936(3) . ? Fe1 N7 1.946(3) . ? Fe1 C32 1.966(4) . ? Fe1 C31 1.972(4) . ? N5 C25 1.348(4) . ? N5 C21 1.349(4) . ? N1 C6 1.339(4) . ? N1 C10 1.342(4) . ? N7 C45 1.368(4) . ? N7 C47 1.378(4) . ? N2 C5 1.340(4) . ? N2 C1 1.344(4) . ? N3 C20 1.343(4) . ? N3 C16 1.347(4) . ? N4 C11 1.341(4) . ? N4 C15 1.351(4) . ? C10 C9 1.392(5) . ? C10 C26 1.547(5) . ? N6 C30 1.150(4) . ? N9 C44 1.341(4) . ? N9 C40 1.353(4) . ? C45 N8 1.324(4) . ? C45 C44 1.462(5) . ? N8 C46 1.389(4) . ? C46 C51 1.398(5) . ? C46 C47 1.409(4) . ? C47 C48 1.394(4) . ? N10 C33 1.378(4) . ? N10 C39 1.380(4) . ? C25 C24 1.387(5) . ? C25 C26 1.545(5) . ? C24 C23 1.374(6) . ? C24 H24 0.9300 . ? C23 C22 1.347(6) . ? C23 H23 0.9300 . ? C22 C21 1.408(5) . ? C22 H22 0.9300 . ? C21 C28 1.543(5) . ? C28 C5 1.545(5) . ? C28 C29 1.548(5) . ? C28 C20 1.548(5) . ? C5 C4 1.381(5) . ? C4 C3 1.374(7) . ? C4 H4 0.9300 . ? C3 C2 1.366(7) . ? C3 H3 0.9300 . ? C2 C1 1.381(6) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C20 C19 1.389(5) . ? C19 C18 1.374(6) . ? C19 H19 0.9300 . ? C18 C17 1.371(6) . ? C18 H18 0.9300 . ? C17 C16 1.363(5) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C26 C27 1.541(5) . ? C26 C11 1.547(4) . ? C11 C12 1.381(5) . ? C12 C13 1.384(6) . ? C12 H12 0.9300 . ? C13 C14 1.368(6) . ? C13 H13 0.9300 . ? C14 C15 1.366(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C6 C7 1.390(5) . ? C6 H6 0.9300 . ? C7 C8 1.362(6) . ? C7 H7 0.9300 . ? C8 C9 1.374(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C32 N13 1.141(5) . ? C44 C43 1.389(5) . ? C48 C49 1.384(5) . ? C48 H48 0.9300 . ? C49 C50 1.402(5) . ? C49 H49 0.9300 . ? C50 C51 1.377(5) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C43 C42 1.393(6) . ? C43 H43 0.9300 . ? C42 C41 1.364(6) . ? C42 H42 0.9300 . ? C41 C40 1.393(5) . ? C41 H41 0.9300 . ? C40 C39 1.445(5) . ? C39 N11 1.324(4) . ? N11 C38 1.386(5) . ? C38 C33 1.411(5) . ? C38 C37 1.416(5) . ? C33 C34 1.397(5) . ? C34 C35 1.380(5) . ? C34 H34 0.9300 . ? C35 C36 1.386(6) . ? C35 H35 0.9300 . ? C36 C37 1.374(6) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C31 N12 1.139(5) . ? O1 C1S 1.285(8) . ? C2S O2 1.462(10) . ? C2S O2B 1.49(2) . ? C3S O3 1.34(2) . ? C3S O3 1.34(2) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Co1 N5 176.50(11) . . ? N6 Co1 N4 91.72(11) . . ? N5 Co1 N4 87.61(10) . . ? N6 Co1 N3 92.53(11) . . ? N5 Co1 N3 88.30(10) . . ? N4 Co1 N3 175.03(10) . . ? N6 Co1 N2 95.11(11) . . ? N5 Co1 N2 88.39(10) . . ? N4 Co1 N2 96.75(10) . . ? N3 Co1 N2 80.31(10) . . ? N6 Co1 N1 90.72(11) . . ? N5 Co1 N1 85.79(10) . . ? N4 Co1 N1 82.69(9) . . ? N3 Co1 N1 99.82(9) . . ? N2 Co1 N1 174.16(10) . . ? C30 Fe1 N10 98.83(12) . . ? C30 Fe1 N9 179.75(13) . . ? N10 Fe1 N9 80.92(11) . . ? C30 Fe1 N7 99.40(12) . . ? N10 Fe1 N7 161.73(11) . . ? N9 Fe1 N7 80.85(11) . . ? C30 Fe1 C32 89.18(16) . . ? N10 Fe1 C32 91.02(13) . . ? N9 Fe1 C32 90.83(15) . . ? N7 Fe1 C32 90.47(13) . . ? C30 Fe1 C31 86.76(14) . . ? N10 Fe1 C31 90.24(13) . . ? N9 Fe1 C31 93.23(13) . . ? N7 Fe1 C31 89.57(13) . . ? C32 Fe1 C31 175.89(16) . . ? C25 N5 C21 120.0(3) . . ? C25 N5 Co1 119.9(2) . . ? C21 N5 Co1 119.7(2) . . ? C6 N1 C10 118.8(3) . . ? C6 N1 Co1 121.7(2) . . ? C10 N1 Co1 119.1(2) . . ? C45 N7 C47 104.2(3) . . ? C45 N7 Fe1 114.3(2) . . ? C47 N7 Fe1 141.5(2) . . ? C5 N2 C1 119.1(3) . . ? C5 N2 Co1 117.3(2) . . ? C1 N2 Co1 123.0(2) . . ? C20 N3 C16 118.3(3) . . ? C20 N3 Co1 120.1(2) . . ? C16 N3 Co1 121.4(2) . . ? C11 N4 C15 118.2(3) . . ? C11 N4 Co1 120.6(2) . . ? C15 N4 Co1 121.2(2) . . ? N1 C10 C9 120.8(3) . . ? N1 C10 C26 116.7(3) . . ? C9 C10 C26 122.4(3) . . ? C30 N6 Co1 168.2(3) . . ? N6 C30 Fe1 178.0(3) . . ? C44 N9 C40 122.2(3) . . ? C44 N9 Fe1 119.0(2) . . ? C40 N9 Fe1 118.8(2) . . ? N8 C45 N7 115.9(3) . . ? N8 C45 C44 128.4(3) . . ? N7 C45 C44 115.6(3) . . ? C45 N8 C46 103.1(3) . . ? N8 C46 C51 130.0(3) . . ? N8 C46 C47 109.8(3) . . ? C51 C46 C47 120.2(3) . . ? N7 C47 C48 131.6(3) . . ? N7 C47 C46 107.0(3) . . ? C48 C47 C46 121.4(3) . . ? C33 N10 C39 104.8(3) . . ? C33 N10 Fe1 140.8(2) . . ? C39 N10 Fe1 114.4(2) . . ? N5 C25 C24 120.4(3) . . ? N5 C25 C26 118.5(3) . . ? C24 C25 C26 121.1(3) . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N5 C21 C22 120.0(3) . . ? N5 C21 C28 118.2(3) . . ? C22 C21 C28 121.8(3) . . ? C21 C28 C5 110.6(3) . . ? C21 C28 C29 109.6(3) . . ? C5 C28 C29 109.1(3) . . ? C21 C28 C20 110.0(3) . . ? C5 C28 C20 108.4(3) . . ? C29 C28 C20 109.0(3) . . ? N2 C5 C4 120.6(3) . . ? N2 C5 C28 117.2(3) . . ? C4 C5 C28 122.2(3) . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C2 C1 117.7(4) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? N2 C1 C2 122.7(4) . . ? N2 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? N3 C20 C19 120.8(3) . . ? N3 C20 C28 117.2(3) . . ? C19 C20 C28 122.0(3) . . ? C18 C19 C20 119.9(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C16 C17 C18 118.6(4) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N3 C16 C17 123.3(4) . . ? N3 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C26 C25 109.2(3) . . ? C27 C26 C10 109.2(3) . . ? C25 C26 C10 109.3(3) . . ? C27 C26 C11 109.1(3) . . ? C25 C26 C11 112.5(3) . . ? C10 C26 C11 107.4(2) . . ? N4 C11 C12 120.2(3) . . ? N4 C11 C26 117.2(3) . . ? C12 C11 C26 122.4(3) . . ? C11 C12 C13 120.7(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 117.9(4) . . ? C15 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N4 C15 C14 124.0(4) . . ? N4 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C6 C7 122.6(4) . . ? N1 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C8 C7 C6 118.7(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 119.2(4) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 119.9(4) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N13 C32 Fe1 179.3(4) . . ? N9 C44 C43 120.5(3) . . ? N9 C44 C45 110.2(3) . . ? C43 C44 C45 129.4(3) . . ? C49 C48 C47 117.5(3) . . ? C49 C48 H48 121.2 . . ? C47 C48 H48 121.2 . . ? C48 C49 C50 121.2(3) . . ? C48 C49 H49 119.4 . . ? C50 C49 H49 119.4 . . ? C51 C50 C49 121.5(3) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C50 C51 C46 118.1(3) . . ? C50 C51 H51 120.9 . . ? C46 C51 H51 120.9 . . ? C44 C43 C42 117.7(4) . . ? C44 C43 H43 121.2 . . ? C42 C43 H43 121.2 . . ? C41 C42 C43 121.2(3) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C42 C41 C40 119.3(3) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? N9 C40 C41 119.1(3) . . ? N9 C40 C39 110.0(3) . . ? C41 C40 C39 130.8(3) . . ? N11 C39 N10 115.3(3) . . ? N11 C39 C40 128.9(3) . . ? N10 C39 C40 115.8(3) . . ? C39 N11 C38 103.1(3) . . ? N11 C38 C33 110.7(3) . . ? N11 C38 C37 130.5(4) . . ? C33 C38 C37 118.8(4) . . ? N10 C33 C34 131.5(3) . . ? N10 C33 C38 106.1(3) . . ? C34 C33 C38 122.4(3) . . ? C35 C34 C33 117.0(4) . . ? C35 C34 H34 121.5 . . ? C33 C34 H34 121.5 . . ? C34 C35 C36 121.7(4) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 122.1(4) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C36 C37 C38 118.1(4) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? N12 C31 Fe1 177.7(4) . . ? O2 C2S O2B 142.7(12) . . ? O3 C3S O3 180(2) . 3_665 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.103 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.061