# 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_mp013 _database_code_depnum_ccdc_archive 'CCDC 899211' #TrackingRef 'Complex 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H128 B8 Cl4 Fe4 N32 O36 Re4, 8(C H Cl3)' _chemical_formula_sum 'C132 H136 B8 Cl28 Fe4 N32 O36 Re4' _chemical_formula_weight 4794.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.163(3) _cell_length_b 20.152(4) _cell_length_c 20.252(4) _cell_angle_alpha 93.07(3) _cell_angle_beta 90.55(3) _cell_angle_gamma 110.44(3) _cell_volume 6169(2) _cell_formula_units_Z 1 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 150 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 2.542 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 marmux _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24238 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 22.21 _reflns_number_total 14339 _reflns_number_gt 8157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marmux - Micro-beam system, marresearch, 2010' _computing_cell_refinement 'automar, marresearch, 2010' _computing_data_reduction 'automar, marresearch, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14339 _refine_ls_number_parameters 1037 _refine_ls_number_restraints 714 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2787 _refine_ls_wR_factor_gt 0.2546 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Re1 Re 0.51705(4) 0.71980(4) 0.06877(3) 0.0819(3) Uani 1 1 d . . . Re2 Re 0.26627(4) -0.06807(4) 0.61878(3) 0.0785(3) Uani 1 1 d . . . Cl1A Cl 0.4789(11) 0.7842(11) 0.1719(8) 0.114(5) Uani 0.58(2) 1 d PU A 1 C59A C 0.518(3) 0.687(2) -0.007(3) 0.155(13) Uiso 0.58(2) 1 d PDU A 1 O15A O 0.551(3) 0.653(2) -0.0394(18) 0.091(11) Uiso 0.58(2) 1 d PDU A 1 Cl1B Cl 0.5536(14) 0.6451(13) -0.0269(13) 0.119(7) Uani 0.42(2) 1 d PU A 2 C59B C 0.494(3) 0.768(2) 0.120(2) 0.089(11) Uiso 0.42(2) 1 d PDU A 2 O15B O 0.500(4) 0.792(3) 0.173(2) 0.080(13) Uiso 0.42(2) 1 d PDU A 2 Cl2A Cl 0.3249(6) -0.1240(6) 0.5279(5) 0.084(4) Uani 0.57(3) 1 d PU B 1 C62A C 0.222(3) -0.030(2) 0.693(2) 0.119(15) Uiso 0.57(3) 1 d PDU B 1 O18A O 0.2019(19) 0.0030(15) 0.7335(14) 0.097(9) Uiso 0.57(3) 1 d PDU B 1 Cl2B Cl 0.2265(8) 0.0067(8) 0.7075(8) 0.085(6) Uani 0.43(3) 1 d PU B 2 C62B C 0.294(3) -0.124(3) 0.551(2) 0.083(14) Uiso 0.43(3) 1 d PDU B 2 O18B O 0.323(2) -0.1491(18) 0.5099(16) 0.072(10) Uiso 0.43(3) 1 d PDU B 2 Fe1 Fe 1.13472(13) 0.90122(11) 0.20505(11) 0.0745(6) Uani 1 1 d . . . Fe2 Fe 0.44519(16) 0.33730(12) 0.35353(11) 0.0819(7) Uani 1 1 d . . . O1 O 1.2923(8) 0.8762(7) 0.2431(8) 0.128(4) Uani 1 1 d U . . O2 O 1.2757(8) 0.9812(7) 0.2986(7) 0.120(4) Uani 1 1 d U . . O3 O 1.3205(7) 0.9821(7) 0.1878(6) 0.114(4) Uani 1 1 d U . . O4 O 0.9938(8) 0.9005(8) 0.1127(6) 0.127(4) Uani 1 1 d U . . O5 O 0.9486(8) 0.8707(8) 0.2257(7) 0.132(4) Uani 1 1 d U . . O6 O 0.9787(9) 0.7897(7) 0.1537(9) 0.152(5) Uani 1 1 d U . . O7 O 0.4323(9) 0.3920(7) 0.2241(6) 0.119(4) Uani 1 1 d U . . O8 O 0.4339(9) 0.4712(7) 0.3188(7) 0.117(4) Uani 1 1 d U . . O9 O 0.5677(8) 0.4526(6) 0.2858(6) 0.110(4) Uani 1 1 d U . . O10 O 0.3443(8) 0.1940(6) 0.3838(6) 0.107(4) Uani 1 1 d U . . O11 O 0.4011(10) 0.2783(7) 0.4777(7) 0.131(4) Uani 1 1 d U . . O12 O 0.4956(8) 0.2314(8) 0.4170(8) 0.136(4) Uani 1 1 d U . . O13 O 0.5210(8) 0.8343(8) -0.0179(8) 0.130(5) Uani 1 1 d U . . O14 O 0.3184(9) 0.6544(7) 0.0358(7) 0.126(5) Uani 1 1 d U . . O16 O 0.1962(7) -0.2052(7) 0.6917(6) 0.104(4) Uani 1 1 d U . . O17 O 0.0844(8) -0.1081(7) 0.5508(7) 0.120(4) Uani 1 1 d U . . N1 N 1.5999(8) 1.0321(7) 0.3363(6) 0.077(3) Uani 1 1 d U . . N2 N 1.2083(9) 0.8494(7) 0.2206(8) 0.099(4) Uani 1 1 d U . . N3 N 1.1843(9) 0.9540(8) 0.2846(7) 0.096(4) Uani 1 1 d U . . N4 N 1.2346(9) 0.9656(7) 0.1626(6) 0.091(4) Uani 1 1 d U . . N5 N 1.0844(9) 0.9284(9) 0.1293(7) 0.116(5) Uani 1 1 d U . . N6 N 1.0342(9) 0.9039(10) 0.2516(8) 0.120(5) Uani 1 1 d U . . N7 N 1.0634(10) 0.8102(8) 0.1817(11) 0.136(5) Uani 1 1 d U . . N8 N 0.6591(8) 0.7664(7) 0.0985(7) 0.084(3) Uani 1 1 d U A . N9 N 0.5156(9) 0.6332(7) 0.1334(7) 0.093(4) Uani 1 1 d U A . N10 N 0.4044(11) 0.3330(8) 0.2630(7) 0.111(5) Uani 1 1 d U . . N11 N 0.4207(10) 0.4232(7) 0.3685(7) 0.097(4) Uani 1 1 d U . . N12 N 0.5542(10) 0.3936(7) 0.3236(7) 0.098(4) Uani 1 1 d U . . N13 N 0.3626(9) 0.2487(7) 0.3395(7) 0.095(4) Uani 1 1 d U . . N14 N 0.4067(11) 0.3323(8) 0.4402(7) 0.112(4) Uani 1 1 d U . . N15 N 0.5220(10) 0.2888(9) 0.3798(9) 0.121(5) Uani 1 1 d U . . N16 N 0.3194(8) 0.0297(6) 0.5650(6) 0.076(3) Uani 1 1 d U B . B1 B 1.3250(12) 0.9552(11) 0.2507(11) 0.089(4) Uani 1 1 d U . . B2 B 0.9426(12) 0.8438(12) 0.1586(13) 0.102(5) Uani 1 1 d U . . B3 B 0.4835(16) 0.4576(12) 0.2602(12) 0.102(5) Uani 1 1 d U A . B4 B 0.4049(15) 0.2147(12) 0.4433(11) 0.095(4) Uani 1 1 d U . . C1 C 1.5472(10) 1.0717(9) 0.3380(8) 0.082(4) Uani 1 1 d U . . H1 H 1.5721 1.1190 0.3565 0.098 Uiso 1 1 calc R . . C2 C 1.4617(9) 1.0497(8) 0.3156(8) 0.075(4) Uani 1 1 d U . . H2 H 1.4270 1.0786 0.3241 0.090 Uiso 1 1 calc R . . C3 C 1.4259(10) 0.9851(9) 0.2806(8) 0.082(4) Uani 1 1 d U . . C4 C 1.4799(10) 0.9451(9) 0.2743(9) 0.089(4) Uani 1 1 d U . . H4 H 1.4593 0.8999 0.2510 0.107 Uiso 1 1 calc R . . C5 C 1.5647(11) 0.9716(9) 0.3024(8) 0.083(4) Uani 1 1 d U . . H5 H 1.6003 0.9430 0.2964 0.100 Uiso 1 1 calc R . . C6 C 1.1836(11) 0.7823(9) 0.2059(11) 0.107(5) Uani 1 1 d U . . C7 C 1.0937(13) 0.7633(11) 0.1797(13) 0.133(5) Uani 1 1 d U . . C8 C 1.0418(15) 0.6783(10) 0.1651(15) 0.161(7) Uani 1 1 d U . . H8A H 1.0323 0.6674 0.1168 0.194 Uiso 1 1 calc R . . H8B H 0.9832 0.6645 0.1855 0.194 Uiso 1 1 calc R . . C9 C 1.0981(17) 0.6321(13) 0.1950(17) 0.190(8) Uani 1 1 d U . . H9A H 1.0798 0.6234 0.2412 0.228 Uiso 1 1 calc R . . H9B H 1.0770 0.5853 0.1701 0.228 Uiso 1 1 calc R . . C10 C 1.1847(14) 0.6540(11) 0.1962(15) 0.163(7) Uani 1 1 d U . . H10A H 1.2030 0.6412 0.1522 0.196 Uiso 1 1 calc R . . H10B H 1.2033 0.6265 0.2287 0.196 Uiso 1 1 calc R . . C11 C 1.2371(14) 0.7326(11) 0.2127(14) 0.144(6) Uani 1 1 d U . . H11A H 1.2880 0.7478 0.1832 0.172 Uiso 1 1 calc R . . H11B H 1.2609 0.7383 0.2587 0.172 Uiso 1 1 calc R . . C12 C 1.1348(10) 0.9682(9) 0.3278(8) 0.079(4) Uani 1 1 d U . . C13 C 1.1660(11) 1.0129(10) 0.3935(8) 0.096(5) Uani 1 1 d U . . H13A H 1.2207 1.0533 0.3865 0.115 Uiso 1 1 calc R . . H13B H 1.1795 0.9834 0.4266 0.115 Uiso 1 1 calc R . . C14 C 1.0943(12) 1.0410(11) 0.4200(10) 0.113(5) Uani 1 1 d U . . H14A H 1.1082 1.0591 0.4667 0.136 Uiso 1 1 calc R . . H14B H 1.0917 1.0803 0.3937 0.136 Uiso 1 1 calc R . . C15 C 1.0056(11) 0.9793(10) 0.4145(9) 0.105(5) Uani 1 1 d U . . H15A H 1.0121 0.9385 0.4362 0.126 Uiso 1 1 calc R . . H15B H 0.9612 0.9937 0.4388 0.126 Uiso 1 1 calc R . . C16 C 0.9714(11) 0.9556(10) 0.3447(8) 0.095(4) Uani 1 1 d U . . H16A H 0.9546 0.9928 0.3243 0.114 Uiso 1 1 calc R . . H16B H 0.9188 0.9117 0.3442 0.114 Uiso 1 1 calc R . . C17 C 1.0446(11) 0.9422(10) 0.3070(9) 0.096(4) Uani 1 1 d U . . C18 C 1.2264(11) 0.9885(10) 0.1089(8) 0.094(4) Uani 1 1 d U . . C19 C 1.2972(12) 1.0304(11) 0.0659(9) 0.112(5) Uani 1 1 d U . . H19A H 1.3272 0.9993 0.0461 0.135 Uiso 1 1 calc R . . H19B H 1.3415 1.0688 0.0934 0.135 Uiso 1 1 calc R . . C20 C 1.2626(14) 1.0633(13) 0.0104(11) 0.150(7) Uani 1 1 d U . . H20A H 1.2574 1.1082 0.0286 0.179 Uiso 1 1 calc R . . H20B H 1.3075 1.0756 -0.0242 0.179 Uiso 1 1 calc R . . C21 C 1.1788(13) 1.0204(12) -0.0208(11) 0.142(7) Uani 1 1 d U . . H21A H 1.1882 0.9823 -0.0492 0.170 Uiso 1 1 calc R . . H21B H 1.1599 1.0505 -0.0502 0.170 Uiso 1 1 calc R . . C22 C 1.1024(12) 0.9857(12) 0.0254(9) 0.127(6) Uani 1 1 d U . . H22A H 1.0723 1.0198 0.0370 0.152 Uiso 1 1 calc R . . H22B H 1.0588 0.9437 0.0016 0.152 Uiso 1 1 calc R . . C23 C 1.1327(11) 0.9637(10) 0.0869(8) 0.096(4) Uani 1 1 d U . . C24 C 0.8398(10) 0.8179(9) 0.1341(9) 0.093(4) Uani 1 1 d U . . C25 C 0.7840(9) 0.8541(8) 0.1536(7) 0.074(4) Uani 1 1 d U A . H25 H 0.8063 0.8980 0.1790 0.089 Uiso 1 1 calc R . . C26 C 0.6951(9) 0.8249(8) 0.1353(7) 0.074(4) Uani 1 1 d U . . H26 H 0.6576 0.8493 0.1508 0.088 Uiso 1 1 calc R A . C27 C 0.7183(14) 0.7296(12) 0.0798(12) 0.133(6) Uani 1 1 d U . . H27 H 0.6946 0.6855 0.0549 0.160 Uiso 1 1 calc R A . C28 C 0.8044(12) 0.7542(11) 0.0955(11) 0.119(5) Uani 1 1 d U A . H28 H 0.8412 0.7288 0.0808 0.143 Uiso 1 1 calc R . . C29 C 0.4745(13) 0.5680(10) 0.1108(9) 0.113(5) Uani 1 1 d U . . H29 H 0.4491 0.5582 0.0673 0.135 Uiso 1 1 calc R A . C30 C 0.4680(14) 0.5122(11) 0.1520(9) 0.115(5) Uani 1 1 d U A . H30 H 0.4388 0.4649 0.1345 0.138 Uiso 1 1 calc R . . C31 C 0.5006(12) 0.5218(10) 0.2144(8) 0.093(4) Uani 1 1 d U . . C32 C 0.5435(11) 0.5949(9) 0.2366(9) 0.090(4) Uani 1 1 d U A . H32 H 0.5675 0.6063 0.2805 0.108 Uiso 1 1 calc R . . C33 C 0.5505(10) 0.6474(8) 0.1969(8) 0.083(4) Uani 1 1 d U . . H33 H 0.5800 0.6952 0.2128 0.100 Uiso 1 1 calc R A . C34 C 0.3425(12) 0.2834(9) 0.2390(8) 0.095(4) Uani 1 1 d U . . C35 C 0.2957(13) 0.2752(10) 0.1734(9) 0.123(6) Uani 1 1 d U . . H35A H 0.3389 0.2797 0.1380 0.148 Uiso 1 1 calc R . . H35B H 0.2724 0.3143 0.1702 0.148 Uiso 1 1 calc R . . C36 C 0.2211(17) 0.2061(13) 0.1613(12) 0.165(7) Uani 1 1 d U . . H36A H 0.1657 0.2142 0.1726 0.198 Uiso 1 1 calc R . . H36B H 0.2174 0.1929 0.1133 0.198 Uiso 1 1 calc R . . C37 C 0.2231(15) 0.1470(11) 0.1952(11) 0.138(6) Uani 1 1 d U . . H37A H 0.2611 0.1269 0.1691 0.165 Uiso 1 1 calc R . . H37B H 0.1626 0.1116 0.1904 0.165 Uiso 1 1 calc R . . C38 C 0.2515(12) 0.1476(9) 0.2676(9) 0.107(5) Uani 1 1 d U . . H38A H 0.2811 0.1126 0.2731 0.128 Uiso 1 1 calc R . . H38B H 0.1997 0.1360 0.2963 0.128 Uiso 1 1 calc R . . C39 C 0.3194(11) 0.2277(9) 0.2859(9) 0.089(4) Uani 1 1 d U . . C40 C 0.3957(11) 0.4397(9) 0.4276(9) 0.090(4) Uani 1 1 d U . . C41 C 0.3765(13) 0.5038(10) 0.4419(10) 0.109(5) Uani 1 1 d U . . H41A H 0.3336 0.5075 0.4084 0.131 Uiso 1 1 calc R . . H41B H 0.4313 0.5457 0.4399 0.131 Uiso 1 1 calc R . . C42 C 0.3400(17) 0.5024(12) 0.5076(12) 0.150(7) Uani 1 1 d U . . H42A H 0.3800 0.5459 0.5319 0.180 Uiso 1 1 calc R . . H42B H 0.2837 0.5105 0.5006 0.180 Uiso 1 1 calc R . . C43 C 0.3212(16) 0.4504(11) 0.5533(12) 0.141(6) Uani 1 1 d U . . H43A H 0.2565 0.4317 0.5588 0.169 Uiso 1 1 calc R . . H43B H 0.3488 0.4732 0.5964 0.169 Uiso 1 1 calc R . . C44 C 0.3525(13) 0.3851(9) 0.5362(10) 0.111(5) Uani 1 1 d U . . H44A H 0.4019 0.3876 0.5667 0.133 Uiso 1 1 calc R . . H44B H 0.3032 0.3402 0.5424 0.133 Uiso 1 1 calc R . . C45 C 0.3822(11) 0.3855(10) 0.4659(8) 0.087(4) Uani 1 1 d U . . C46 C 0.6288(12) 0.3794(9) 0.3325(9) 0.092(4) Uani 1 1 d U . . C47 C 0.6105(12) 0.3175(9) 0.3689(9) 0.098(4) Uani 1 1 d U . . C48 C 0.6752(11) 0.2896(10) 0.3958(10) 0.107(5) Uani 1 1 d U . . H48A H 0.6698 0.2443 0.3714 0.128 Uiso 1 1 calc R . . H48B H 0.6635 0.2801 0.4429 0.128 Uiso 1 1 calc R . . C49 C 0.7693(12) 0.3433(11) 0.3896(10) 0.117(5) Uani 1 1 d U . . H49A H 0.7812 0.3818 0.4247 0.140 Uiso 1 1 calc R . . H49B H 0.8128 0.3195 0.3953 0.140 Uiso 1 1 calc R . . C50 C 0.7788(15) 0.3735(13) 0.3242(12) 0.143(7) Uani 1 1 d U . . H50A H 0.7651 0.3337 0.2902 0.172 Uiso 1 1 calc R . . H50B H 0.8417 0.4031 0.3199 0.172 Uiso 1 1 calc R . . C51 C 0.7179(11) 0.4227(9) 0.3054(10) 0.105(5) Uani 1 1 d U . . H51A H 0.7419 0.4709 0.3276 0.126 Uiso 1 1 calc R . . H51B H 0.7139 0.4267 0.2570 0.126 Uiso 1 1 calc R . . C52 C 0.3811(11) 0.1479(9) 0.4875(8) 0.087(4) Uani 1 1 d U . . C53 C 0.3015(10) 0.1317(9) 0.5245(8) 0.085(4) Uani 1 1 d U B . H53 H 0.2672 0.1615 0.5229 0.102 Uiso 1 1 calc R . . C54 C 0.2750(10) 0.0743(8) 0.5614(7) 0.076(4) Uani 1 1 d U . . H54 H 0.2227 0.0654 0.5858 0.091 Uiso 1 1 calc R B . C55 C 0.3929(10) 0.0460(9) 0.5302(8) 0.083(4) Uani 1 1 d U . . H55 H 0.4237 0.0135 0.5291 0.100 Uiso 1 1 calc R B . C56 C 0.4273(11) 0.1057(9) 0.4959(8) 0.090(4) Uani 1 1 d U B . H56 H 0.4844 0.1172 0.4781 0.107 Uiso 1 1 calc R . . C57 C 0.5179(13) 0.7913(12) 0.0179(12) 0.135(8) Uani 1 1 d U A . C58 C 0.3947(12) 0.6786(10) 0.0468(10) 0.111(6) Uani 1 1 d U A . C60 C 0.2250(10) -0.1512(8) 0.6623(8) 0.078(4) Uani 1 1 d U B . C61 C 0.1569(10) -0.0958(10) 0.5777(10) 0.104(6) Uani 1 1 d U B . C63 C 0.0591(15) -0.1114(10) 0.7912(9) 0.166(9) Uiso 1 1 d DU . . H63 H 0.1226 -0.0899 0.7797 0.199 Uiso 1 1 calc R . . Cl3 Cl 0.0271(5) -0.0477(4) 0.8283(4) 0.176(3) Uiso 1 1 d DU . . Cl4 Cl -0.0019(7) -0.1496(5) 0.7207(5) 0.226(4) Uiso 1 1 d D . . Cl5 Cl 0.0485(9) -0.1775(6) 0.8437(6) 0.279(5) Uiso 1 1 d D . . C64 C 1.5792(13) 1.2470(14) 0.2083(16) 0.359(19) Uiso 1 1 d DU . . H64 H 1.5769 1.2762 0.2493 0.430 Uiso 1 1 calc R . . Cl6 Cl 1.4852(6) 1.1825(5) 0.1991(5) 0.215(4) Uiso 1 1 d DU . . Cl7 Cl 1.6045(9) 1.3011(7) 0.1458(7) 0.312(6) Uiso 1 1 d DU . . Cl8 Cl 1.6626(9) 1.2164(8) 0.2188(8) 0.332(7) Uiso 1 1 d DU . . C65 C 1.4370(15) 0.7229(12) 0.3793(16) 0.345(18) Uiso 1 1 d DU . . H65 H 1.4364 0.7067 0.4252 0.414 Uiso 1 1 calc R . . Cl9 Cl 1.3994(6) 0.7915(4) 0.3802(4) 0.195(3) Uiso 1 1 d DU . . Cl10 Cl 1.3739(11) 0.6548(8) 0.3288(9) 0.392(9) Uiso 1 1 d DU . . Cl11 Cl 1.5419(10) 0.7535(9) 0.3539(10) 0.408(9) Uiso 1 1 d DU . . C66 C 1.162(2) 0.7446(15) 0.4353(13) 0.40(2) Uiso 1 1 d DU . . H66 H 1.2222 0.7707 0.4556 0.476 Uiso 1 1 calc R . . Cl12 Cl 1.0900(11) 0.7231(8) 0.4963(8) 0.347(8) Uiso 1 1 d DU . . Cl13 Cl 1.1361(11) 0.7992(8) 0.3850(8) 0.339(7) Uiso 1 1 d DU . . Cl14 Cl 1.1646(17) 0.6718(12) 0.3947(12) 0.546(15) Uiso 1 1 d DU . . 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 Re1 0.0669(5) 0.0867(5) 0.0847(5) 0.0135(4) -0.0098(3) 0.0168(3) Re2 0.0630(4) 0.0921(5) 0.0838(5) 0.0159(4) -0.0047(3) 0.0300(3) Cl1A 0.081(9) 0.111(8) 0.137(10) 0.024(6) -0.006(6) 0.016(7) Cl1B 0.073(8) 0.123(12) 0.143(13) 0.073(10) -0.017(8) 0.004(6) Cl2A 0.088(6) 0.092(7) 0.074(8) -0.006(6) -0.006(5) 0.034(5) Cl2B 0.068(7) 0.109(10) 0.083(10) 0.044(7) 0.016(6) 0.033(6) Fe1 0.0613(13) 0.0847(15) 0.0756(15) 0.0104(11) -0.0072(11) 0.0225(11) Fe2 0.0870(16) 0.0828(16) 0.0758(15) 0.0117(12) -0.0062(12) 0.0289(12) O1 0.096(8) 0.103(8) 0.179(10) -0.008(8) -0.039(8) 0.030(7) O2 0.074(7) 0.162(10) 0.118(9) -0.030(8) -0.008(6) 0.036(7) O3 0.078(7) 0.146(9) 0.095(7) 0.043(7) -0.014(6) 0.003(6) O4 0.078(7) 0.173(10) 0.108(8) 0.046(7) -0.017(6) 0.014(7) O5 0.071(7) 0.198(11) 0.108(8) -0.043(8) -0.016(6) 0.031(7) O6 0.088(8) 0.111(8) 0.257(13) 0.009(9) -0.058(8) 0.036(7) O7 0.141(9) 0.104(8) 0.096(8) 0.031(7) -0.018(7) 0.020(7) O8 0.153(9) 0.101(8) 0.112(8) 0.038(7) 0.027(7) 0.060(7) O9 0.109(8) 0.104(8) 0.122(8) 0.043(7) 0.012(7) 0.039(6) O10 0.120(8) 0.084(7) 0.103(8) 0.022(6) -0.034(7) 0.019(6) O11 0.191(11) 0.101(8) 0.106(8) 0.021(7) 0.011(8) 0.053(8) O12 0.093(8) 0.148(10) 0.167(10) 0.072(8) 0.010(8) 0.032(7) O13 0.094(9) 0.152(13) 0.138(12) 0.014(10) -0.019(8) 0.037(8) O14 0.093(9) 0.108(9) 0.156(12) -0.014(9) -0.024(9) 0.012(7) O16 0.077(7) 0.116(9) 0.113(9) 0.028(8) 0.004(6) 0.022(6) O17 0.087(9) 0.137(10) 0.143(11) 0.038(9) 0.002(8) 0.043(8) N1 0.080(8) 0.083(8) 0.070(7) 0.006(6) 0.001(6) 0.032(6) N2 0.069(7) 0.080(8) 0.146(10) -0.009(8) -0.027(7) 0.029(6) N3 0.065(7) 0.131(9) 0.094(9) -0.020(8) -0.014(7) 0.040(7) N4 0.079(8) 0.110(9) 0.072(8) 0.027(7) -0.013(6) 0.016(7) N5 0.073(8) 0.173(11) 0.082(9) 0.044(8) -0.011(7) 0.015(8) N6 0.069(8) 0.190(12) 0.103(10) -0.013(9) -0.010(8) 0.052(8) N7 0.085(9) 0.086(9) 0.228(13) 0.010(10) -0.053(9) 0.023(7) N8 0.072(8) 0.088(8) 0.094(9) -0.003(7) -0.007(7) 0.031(6) N9 0.097(9) 0.075(8) 0.084(8) 0.016(7) -0.005(7) -0.002(7) N10 0.125(10) 0.100(9) 0.080(8) 0.013(7) -0.034(8) 0.005(8) N11 0.133(10) 0.081(8) 0.095(9) 0.032(7) 0.011(8) 0.056(7) N12 0.096(9) 0.093(8) 0.097(9) 0.039(7) 0.012(7) 0.017(7) N13 0.098(9) 0.090(8) 0.084(8) 0.017(7) -0.020(7) 0.017(7) N14 0.166(11) 0.078(9) 0.092(9) 0.032(7) 0.018(8) 0.041(8) N15 0.093(9) 0.124(10) 0.148(11) 0.065(9) 0.004(8) 0.032(8) N16 0.082(8) 0.073(7) 0.080(8) 0.005(6) -0.008(6) 0.035(6) B1 0.063(8) 0.098(9) 0.104(9) 0.013(8) -0.007(8) 0.026(7) B2 0.054(7) 0.119(10) 0.135(10) -0.009(9) -0.030(8) 0.037(7) B3 0.121(10) 0.096(9) 0.094(9) 0.029(8) 0.000(8) 0.041(8) B4 0.101(9) 0.097(9) 0.096(9) 0.033(8) 0.005(8) 0.043(8) C1 0.074(8) 0.082(9) 0.090(9) 0.012(8) 0.001(8) 0.027(7) C2 0.067(8) 0.079(9) 0.087(9) 0.017(8) 0.005(7) 0.032(7) C3 0.068(8) 0.089(8) 0.091(9) 0.011(7) -0.010(7) 0.029(7) C4 0.077(9) 0.089(9) 0.104(10) 0.000(8) 0.001(8) 0.033(8) C5 0.089(9) 0.088(9) 0.075(9) -0.004(8) -0.002(8) 0.036(8) C6 0.083(8) 0.076(8) 0.173(12) -0.003(9) -0.034(9) 0.042(7) C7 0.087(9) 0.087(10) 0.215(13) 0.014(10) -0.041(10) 0.017(8) C8 0.120(12) 0.083(10) 0.261(16) 0.007(12) -0.052(13) 0.013(9) C9 0.133(13) 0.113(12) 0.301(18) 0.007(14) -0.037(15) 0.018(12) C10 0.102(12) 0.120(12) 0.257(17) -0.003(13) -0.036(13) 0.028(11) C11 0.107(11) 0.117(11) 0.205(15) -0.012(12) -0.034(11) 0.041(10) C12 0.061(7) 0.112(9) 0.071(8) -0.006(7) -0.016(7) 0.043(7) C13 0.085(9) 0.130(11) 0.071(9) 0.013(8) -0.003(8) 0.035(8) C14 0.098(10) 0.141(12) 0.094(10) 0.006(10) 0.005(9) 0.033(9) C15 0.092(10) 0.126(11) 0.107(11) 0.006(9) 0.000(9) 0.051(8) C16 0.082(9) 0.128(11) 0.083(10) 0.005(9) -0.011(8) 0.048(8) C17 0.076(8) 0.137(10) 0.082(9) 0.000(8) -0.011(8) 0.048(8) C18 0.079(8) 0.121(10) 0.067(8) 0.020(8) -0.002(7) 0.015(8) C19 0.092(10) 0.146(12) 0.084(10) 0.028(9) -0.001(8) 0.019(9) C20 0.114(12) 0.175(14) 0.114(12) 0.059(11) 0.001(10) -0.014(11) C21 0.105(11) 0.158(13) 0.124(12) 0.068(11) -0.006(10) -0.010(10) C22 0.090(10) 0.168(13) 0.102(11) 0.046(10) -0.024(9) 0.016(10) C23 0.075(8) 0.137(10) 0.066(8) 0.028(8) -0.009(7) 0.021(8) C24 0.070(8) 0.092(9) 0.109(10) 0.001(8) -0.009(8) 0.018(7) C25 0.063(8) 0.084(9) 0.069(8) 0.001(7) -0.014(7) 0.018(7) C26 0.061(8) 0.083(9) 0.080(9) -0.009(8) -0.005(7) 0.031(7) C27 0.109(11) 0.119(12) 0.144(13) -0.021(11) -0.014(11) 0.009(10) C28 0.082(10) 0.124(11) 0.146(12) -0.020(10) -0.012(10) 0.033(9) C29 0.136(12) 0.090(10) 0.089(10) 0.017(9) -0.007(9) 0.009(9) C30 0.139(12) 0.101(11) 0.086(10) -0.005(9) -0.019(10) 0.020(9) C31 0.105(9) 0.101(9) 0.081(9) 0.013(8) -0.017(8) 0.043(8) C32 0.095(9) 0.086(9) 0.085(9) 0.016(8) -0.007(8) 0.026(8) C33 0.087(9) 0.074(9) 0.080(9) 0.009(7) -0.014(8) 0.017(7) C34 0.106(9) 0.088(9) 0.083(9) 0.016(8) -0.027(8) 0.023(8) C35 0.129(12) 0.127(12) 0.091(10) 0.025(9) -0.032(9) 0.013(10) C36 0.180(14) 0.146(14) 0.119(12) 0.019(11) -0.046(12) -0.004(12) C37 0.141(12) 0.116(12) 0.132(12) 0.019(10) -0.054(11) 0.015(10) C38 0.113(11) 0.096(10) 0.102(10) 0.009(9) -0.034(9) 0.027(8) C39 0.094(9) 0.082(9) 0.097(9) 0.002(8) -0.016(8) 0.039(7) C40 0.100(9) 0.098(10) 0.078(9) 0.015(8) -0.006(8) 0.043(8) C41 0.126(11) 0.098(10) 0.103(11) 0.007(10) 0.024(10) 0.039(9) C42 0.172(14) 0.120(12) 0.145(14) 0.000(11) 0.043(12) 0.033(11) C43 0.159(13) 0.108(12) 0.150(14) 0.002(11) 0.039(12) 0.039(11) C44 0.113(11) 0.091(10) 0.119(11) -0.006(10) 0.008(10) 0.024(9) C45 0.097(9) 0.089(9) 0.076(9) 0.002(8) 0.014(8) 0.033(7) C46 0.089(9) 0.088(9) 0.099(9) 0.017(8) 0.011(8) 0.029(7) C47 0.085(9) 0.097(9) 0.112(10) 0.026(8) 0.006(8) 0.031(7) C48 0.083(9) 0.120(11) 0.125(11) 0.044(9) -0.008(9) 0.040(8) C49 0.102(10) 0.128(12) 0.122(12) 0.035(10) 0.010(10) 0.038(9) C50 0.118(12) 0.152(13) 0.139(13) 0.006(12) 0.017(11) 0.021(11) C51 0.097(10) 0.106(11) 0.116(11) 0.004(9) 0.016(9) 0.042(8) C52 0.078(8) 0.097(9) 0.091(9) 0.023(7) -0.009(7) 0.035(7) C53 0.081(9) 0.086(9) 0.094(10) 0.006(8) -0.005(8) 0.037(7) C54 0.080(9) 0.062(8) 0.078(9) 0.015(7) 0.006(7) 0.014(7) C55 0.078(9) 0.090(9) 0.092(10) 0.015(8) 0.007(8) 0.041(7) C56 0.084(9) 0.089(10) 0.104(10) 0.026(8) 0.006(8) 0.037(8) C57 0.110(14) 0.118(16) 0.170(19) 0.097(14) -0.025(13) 0.018(11) C58 0.076(11) 0.106(13) 0.126(15) -0.002(11) -0.059(11) 0.005(10) C60 0.069(9) 0.070(10) 0.096(11) 0.035(9) 0.016(8) 0.022(7) C61 0.043(9) 0.132(14) 0.140(15) 0.013(12) -0.010(9) 0.034(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C59B 1.50(5) . ? Re1 C59A 1.64(5) . ? Re1 C57 1.811(18) . ? Re1 C58 1.897(17) . ? Re1 N8 2.218(12) . ? Re1 N9 2.231(13) . ? Re1 Cl1B 2.59(3) . ? Re1 Cl1A 2.592(16) . ? Re2 C61 1.833(16) . ? Re2 C60 1.849(15) . ? Re2 C62B 1.89(3) . ? Re2 C62A 1.90(3) . ? Re2 N1 2.198(12) 2_766 ? Re2 N16 2.207(12) . ? Re2 Cl2A 2.474(12) . ? Re2 Cl2B 2.514(18) . ? C59A O15A 1.18(2) . ? C59B O15B 1.15(2) . ? C62A O18A 1.16(2) . ? C62B O18B 1.14(2) . ? Fe1 N7 1.827(15) . ? Fe1 N2 1.871(13) . ? Fe1 N3 1.889(14) . ? Fe1 N6 1.901(15) . ? Fe1 N5 1.921(13) . ? Fe1 N4 1.927(13) . ? Fe2 N13 1.823(13) . ? Fe2 N12 1.860(14) . ? Fe2 N14 1.864(16) . ? Fe2 N11 1.915(13) . ? Fe2 N15 1.916(15) . ? Fe2 N10 1.930(13) . ? O1 N2 1.339(16) . ? O1 B1 1.49(2) . ? O2 N3 1.403(16) . ? O2 B1 1.45(2) . ? O3 N4 1.394(15) . ? O3 B1 1.42(2) . ? O4 N5 1.403(16) . ? O4 B2 1.52(3) . ? O5 N6 1.393(17) . ? O5 B2 1.43(3) . ? O6 N7 1.390(17) . ? O6 B2 1.40(2) . ? O7 N10 1.403(17) . ? O7 B3 1.44(3) . ? O8 N11 1.399(16) . ? O8 B3 1.50(3) . ? O9 N12 1.401(16) . ? O9 B3 1.49(2) . ? O10 N13 1.411(16) . ? O10 B4 1.49(2) . ? O11 N14 1.337(17) . ? O11 B4 1.45(3) . ? O12 N15 1.357(17) . ? O12 B4 1.50(2) . ? O13 C57 1.149(18) . ? O14 C58 1.170(18) . ? O16 C60 1.215(16) . ? O17 C61 1.226(17) . ? N1 C5 1.303(19) . ? N1 C1 1.355(19) . ? N1 Re2 2.198(12) 2_766 ? N2 C6 1.286(19) . ? N3 C12 1.278(19) . ? N4 C18 1.228(18) . ? N5 C23 1.243(19) . ? N6 C17 1.30(2) . ? N7 C7 1.21(2) . ? N8 C26 1.304(18) . ? N8 C27 1.44(3) . ? N9 C29 1.30(2) . ? N9 C33 1.374(18) . ? N10 C34 1.215(19) . ? N11 C40 1.33(2) . ? N12 C46 1.35(2) . ? N13 C39 1.255(19) . ? N14 C45 1.35(2) . ? N15 C47 1.37(2) . ? N16 C55 1.336(19) . ? N16 C54 1.336(18) . ? B1 C3 1.63(2) . ? B2 C24 1.62(2) . ? B3 C31 1.58(3) . ? B4 C52 1.59(2) . ? C1 C2 1.360(19) . ? C1 H1 0.9500 . ? C2 C3 1.38(2) . ? C2 H2 0.9500 . ? C3 C4 1.38(2) . ? C4 C5 1.39(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.45(2) . ? C6 C11 1.54(2) . ? C7 C8 1.63(3) . ? C8 C9 1.64(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.31(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.53(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.42(2) . ? C12 C13 1.54(2) . ? C13 C14 1.55(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.53(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.50(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.51(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C23 1.47(2) . ? C18 C19 1.48(2) . ? C19 C20 1.53(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.45(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.54(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.48(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 C25 1.39(2) . ? C24 C28 1.40(2) . ? C25 C26 1.387(19) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.33(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.41(2) . ? C29 H29 0.9500 . ? C30 C31 1.34(2) . ? C30 H30 0.9500 . ? C31 C32 1.44(2) . ? C32 C33 1.34(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.46(2) . ? C34 C35 1.50(2) . ? C35 C36 1.50(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.42(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.53(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.62(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C40 C45 1.33(2) . ? C40 C41 1.45(2) . ? C41 C42 1.46(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.39(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.59(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.51(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C46 C47 1.43(2) . ? C46 C51 1.53(2) . ? C47 C48 1.46(2) . ? C48 C49 1.54(2) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.47(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.68(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C56 1.33(2) . ? C52 C53 1.44(2) . ? C53 C54 1.35(2) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.37(2) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C63 Cl3 1.687(16) . ? C63 Cl5 1.710(16) . ? C63 Cl4 1.712(16) . ? C63 H63 1.0000 . ? C64 Cl6 1.619(19) . ? C64 Cl7 1.67(2) . ? C64 Cl8 1.68(2) . ? C64 H64 1.0000 . ? C65 Cl10 1.680(19) . ? C65 Cl11 1.69(2) . ? C65 Cl9 1.693(19) . ? C65 H65 1.0000 . ? C66 Cl14 1.66(2) . ? C66 Cl12 1.67(2) . ? C66 Cl13 1.69(2) . ? C66 H66 1.0000 . ? 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 C59B Re1 C59A 153(2) . . ? C59B Re1 C57 80.0(18) . . ? C59A Re1 C57 76.4(18) . . ? C59B Re1 C58 87.8(17) . . ? C59A Re1 C58 78.3(17) . . ? C57 Re1 C58 86.6(8) . . ? C59B Re1 N8 91.2(17) . . ? C59A Re1 N8 103.5(16) . . ? C57 Re1 N8 95.2(7) . . ? C58 Re1 N8 177.7(7) . . ? C59B Re1 N9 98.7(16) . . ? C59A Re1 N9 104.9(17) . . ? C57 Re1 N9 178.7(10) . . ? C58 Re1 N9 93.5(7) . . ? N8 Re1 N9 84.7(5) . . ? C59B Re1 Cl1B 174.6(16) . . ? C59A Re1 Cl1B 21.8(16) . . ? C57 Re1 Cl1B 94.7(10) . . ? C58 Re1 Cl1B 91.0(8) . . ? N8 Re1 Cl1B 90.3(6) . . ? N9 Re1 Cl1B 86.6(6) . . ? C59B Re1 Cl1A 11.0(17) . . ? C59A Re1 Cl1A 162.4(16) . . ? C57 Re1 Cl1A 91.0(10) . . ? C58 Re1 Cl1A 88.9(8) . . ? N8 Re1 Cl1A 89.7(5) . . ? N9 Re1 Cl1A 87.7(6) . . ? Cl1B Re1 Cl1A 174.3(7) . . ? C61 Re2 C60 87.0(8) . . ? C61 Re2 C62B 86.0(17) . . ? C60 Re2 C62B 85.0(17) . . ? C61 Re2 C62A 89.4(16) . . ? C60 Re2 C62A 83.5(16) . . ? C62B Re2 C62A 168(2) . . ? C61 Re2 N1 177.2(7) . 2_766 ? C60 Re2 N1 95.4(6) . 2_766 ? C62B Re2 N1 92.9(16) . 2_766 ? C62A Re2 N1 92.2(15) . 2_766 ? C61 Re2 N16 94.0(7) . . ? C60 Re2 N16 177.8(6) . . ? C62B Re2 N16 93.1(17) . . ? C62A Re2 N16 98.5(16) . . ? N1 Re2 N16 83.5(4) 2_766 . ? C61 Re2 Cl2A 92.0(7) . . ? C60 Re2 Cl2A 92.6(6) . . ? C62B Re2 Cl2A 9.5(17) . . ? C62A Re2 Cl2A 175.8(15) . . ? N1 Re2 Cl2A 86.6(4) 2_766 . ? N16 Re2 Cl2A 85.4(4) . . ? C61 Re2 Cl2B 93.1(7) . . ? C60 Re2 Cl2B 95.3(6) . . ? C62B Re2 Cl2B 179.0(16) . . ? C62A Re2 Cl2B 12.2(16) . . ? N1 Re2 Cl2B 88.1(4) 2_766 . ? N16 Re2 Cl2B 86.7(4) . . ? Cl2A Re2 Cl2B 170.9(3) . . ? O15A C59A Re1 142(4) . . ? O15B C59B Re1 150(5) . . ? O18A C62A Re2 169(4) . . ? O18B C62B Re2 169(4) . . ? N7 Fe1 N2 77.3(6) . . ? N7 Fe1 N3 136.2(8) . . ? N2 Fe1 N3 85.9(6) . . ? N7 Fe1 N6 83.3(9) . . ? N2 Fe1 N6 129.4(7) . . ? N3 Fe1 N6 76.8(7) . . ? N7 Fe1 N5 86.7(8) . . ? N2 Fe1 N5 136.9(8) . . ? N3 Fe1 N5 129.9(7) . . ? N6 Fe1 N5 87.0(7) . . ? N7 Fe1 N4 131.5(9) . . ? N2 Fe1 N4 85.6(6) . . ? N3 Fe1 N4 86.1(6) . . ? N6 Fe1 N4 138.6(7) . . ? N5 Fe1 N4 75.5(6) . . ? N13 Fe2 N12 140.6(7) . . ? N13 Fe2 N14 85.6(7) . . ? N12 Fe2 N14 127.5(7) . . ? N13 Fe2 N11 125.5(6) . . ? N12 Fe2 N11 86.7(7) . . ? N14 Fe2 N11 76.8(7) . . ? N13 Fe2 N15 85.1(7) . . ? N12 Fe2 N15 77.0(7) . . ? N14 Fe2 N15 87.3(7) . . ? N11 Fe2 N15 143.3(7) . . ? N13 Fe2 N10 75.1(6) . . ? N12 Fe2 N10 85.2(7) . . ? N14 Fe2 N10 142.2(7) . . ? N11 Fe2 N10 88.3(7) . . ? N15 Fe2 N10 122.1(8) . . ? N2 O1 B1 111.9(12) . . ? N3 O2 B1 112.6(13) . . ? N4 O3 B1 113.9(12) . . ? N5 O4 B2 112.3(11) . . ? N6 O5 B2 115.1(14) . . ? N7 O6 B2 113.0(14) . . ? N10 O7 B3 114.2(13) . . ? N11 O8 B3 115.5(13) . . ? N12 O9 B3 112.7(13) . . ? N13 O10 B4 112.3(12) . . ? N14 O11 B4 116.1(15) . . ? N15 O12 B4 114.2(14) . . ? C5 N1 C1 113.0(14) . . ? C5 N1 Re2 123.2(11) . 2_766 ? C1 N1 Re2 123.7(11) . 2_766 ? C6 N2 O1 112.0(13) . . ? C6 N2 Fe1 121.8(11) . . ? O1 N2 Fe1 126.0(10) . . ? C12 N3 O2 116.9(13) . . ? C12 N3 Fe1 120.4(11) . . ? O2 N3 Fe1 122.7(11) . . ? C18 N4 O3 116.9(13) . . ? C18 N4 Fe1 121.4(11) . . ? O3 N4 Fe1 121.4(9) . . ? C23 N5 O4 115.8(13) . . ? C23 N5 Fe1 120.5(12) . . ? O4 N5 Fe1 122.8(10) . . ? C17 N6 O5 117.9(15) . . ? C17 N6 Fe1 119.9(12) . . ? O5 N6 Fe1 122.0(12) . . ? C7 N7 O6 113.4(16) . . ? C7 N7 Fe1 119.8(14) . . ? O6 N7 Fe1 125.7(12) . . ? C26 N8 C27 114.9(14) . . ? C26 N8 Re1 125.1(11) . . ? C27 N8 Re1 120.0(11) . . ? C29 N9 C33 120.4(15) . . ? C29 N9 Re1 117.8(12) . . ? C33 N9 Re1 121.6(10) . . ? C34 N10 O7 114.4(14) . . ? C34 N10 Fe2 122.3(13) . . ? O7 N10 Fe2 122.3(10) . . ? C40 N11 O8 119.2(13) . . ? C40 N11 Fe2 120.2(11) . . ? O8 N11 Fe2 120.5(11) . . ? C46 N12 O9 112.1(13) . . ? C46 N12 Fe2 123.3(12) . . ? O9 N12 Fe2 124.6(11) . . ? C39 N13 O10 111.7(13) . . ? C39 N13 Fe2 122.8(12) . . ? O10 N13 Fe2 125.3(10) . . ? O11 N14 C45 118.5(16) . . ? O11 N14 Fe2 123.5(12) . . ? C45 N14 Fe2 118.0(12) . . ? O12 N15 C47 116.5(14) . . ? O12 N15 Fe2 123.2(12) . . ? C47 N15 Fe2 119.7(12) . . ? C55 N16 C54 115.4(13) . . ? C55 N16 Re2 123.6(10) . . ? C54 N16 Re2 120.8(11) . . ? O3 B1 O2 110.7(15) . . ? O3 B1 O1 108.7(17) . . ? O2 B1 O1 112.2(16) . . ? O3 B1 C3 110.6(15) . . ? O2 B1 C3 104.5(15) . . ? O1 B1 C3 110.1(14) . . ? O6 B2 O5 109.4(18) . . ? O6 B2 O4 107.2(18) . . ? O5 B2 O4 112.3(17) . . ? O6 B2 C24 113.5(17) . . ? O5 B2 C24 107.9(17) . . ? O4 B2 C24 106.6(15) . . ? O7 B3 O9 109.7(17) . . ? O7 B3 O8 110.4(18) . . ? O9 B3 O8 107.5(16) . . ? O7 B3 C31 110.0(16) . . ? O9 B3 C31 111.7(17) . . ? O8 B3 C31 107.4(16) . . ? O11 B4 O10 111.2(15) . . ? O11 B4 O12 107.9(17) . . ? O10 B4 O12 105.2(16) . . ? O11 B4 C52 114.2(17) . . ? O10 B4 C52 107.7(16) . . ? O12 B4 C52 110.4(15) . . ? N1 C1 C2 125.8(15) . . ? N1 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? C1 C2 C3 119.3(15) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 116.0(14) . . ? C2 C3 B1 122.8(15) . . ? C4 C3 B1 121.2(16) . . ? C3 C4 C5 119.4(16) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 125.9(16) . . ? N1 C5 H5 117.0 . . ? C4 C5 H5 117.0 . . ? N2 C6 C7 104.4(14) . . ? N2 C6 C11 128.3(16) . . ? C7 C6 C11 127.2(17) . . ? N7 C7 C6 116.0(18) . . ? N7 C7 C8 128.2(18) . . ? C6 C7 C8 114.6(16) . . ? C7 C8 C9 111.3(17) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 123(2) . . ? C10 C9 H9A 106.6 . . ? C8 C9 H9A 106.6 . . ? C10 C9 H9B 106.6 . . ? C8 C9 H9B 106.6 . . ? H9A C9 H9B 106.6 . . ? C9 C10 C11 119(2) . . ? C9 C10 H10A 107.6 . . ? C11 C10 H10A 107.6 . . ? C9 C10 H10B 107.6 . . ? C11 C10 H10B 107.6 . . ? H10A C10 H10B 107.0 . . ? C10 C11 C6 114.7(17) . . ? C10 C11 H11A 108.6 . . ? C6 C11 H11A 108.6 . . ? C10 C11 H11B 108.6 . . ? C6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N3 C12 C17 112.3(15) . . ? N3 C12 C13 126.2(14) . . ? C17 C12 C13 121.4(15) . . ? C12 C13 C14 110.9(13) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 107.7(16) . . ? C15 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? C15 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? C16 C15 C14 114.3(16) . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C15 C16 C17 107.3(14) . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.5 . . ? N6 C17 C12 110.1(16) . . ? N6 C17 C16 125.3(15) . . ? C12 C17 C16 124.7(16) . . ? N4 C18 C23 110.7(14) . . ? N4 C18 C19 127.9(16) . . ? C23 C18 C19 121.2(14) . . ? C18 C19 C20 113.0(16) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 116.7(17) . . ? C21 C20 H20A 108.1 . . ? C19 C20 H20A 108.1 . . ? C21 C20 H20B 108.1 . . ? C19 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C20 C21 C22 116.8(18) . . ? C20 C21 H21A 108.1 . . ? C22 C21 H21A 108.1 . . ? C20 C21 H21B 108.1 . . ? C22 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C23 C22 C21 112.6(15) . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? N5 C23 C18 111.1(14) . . ? N5 C23 C22 125.9(16) . . ? C18 C23 C22 122.7(15) . . ? C25 C24 C28 118.7(15) . . ? C25 C24 B2 122.6(16) . . ? C28 C24 B2 118.6(17) . . ? C26 C25 C24 118.8(14) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N8 C26 C25 125.0(14) . . ? N8 C26 H26 117.5 . . ? C25 C26 H26 117.5 . . ? C28 C27 N8 123.6(19) . . ? C28 C27 H27 118.2 . . ? N8 C27 H27 118.2 . . ? C27 C28 C24 119(2) . . ? C27 C28 H28 120.5 . . ? C24 C28 H28 120.5 . . ? N9 C29 C30 119.1(17) . . ? N9 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 124.0(18) . . ? C31 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? C30 C31 C32 114.0(16) . . ? C30 C31 B3 121.5(18) . . ? C32 C31 B3 124.2(16) . . ? C33 C32 C31 121.5(16) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 N9 120.9(15) . . ? C32 C33 H33 119.5 . . ? N9 C33 H33 119.5 . . ? N10 C34 C39 107.8(15) . . ? N10 C34 C35 129.4(17) . . ? C39 C34 C35 122.8(16) . . ? C34 C35 C36 114.0(17) . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 118(2) . . ? C37 C36 H36A 107.7 . . ? C35 C36 H36A 107.7 . . ? C37 C36 H36B 107.7 . . ? C35 C36 H36B 107.7 . . ? H36A C36 H36B 107.1 . . ? C36 C37 C38 126.5(19) . . ? C36 C37 H37A 105.7 . . ? C38 C37 H37A 105.7 . . ? C36 C37 H37B 105.7 . . ? C38 C37 H37B 105.7 . . ? H37A C37 H37B 106.1 . . ? C37 C38 C39 105.4(15) . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38B 110.7 . . ? C39 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? N13 C39 C34 111.3(15) . . ? N13 C39 C38 125.4(15) . . ? C34 C39 C38 123.2(15) . . ? N11 C40 C45 109.4(16) . . ? N11 C40 C41 122.7(15) . . ? C45 C40 C41 127.5(18) . . ? C40 C41 C42 109.7(18) . . ? C40 C41 H41A 109.7 . . ? C42 C41 H41A 109.7 . . ? C40 C41 H41B 109.7 . . ? C42 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C43 C42 C41 130(2) . . ? C43 C42 H42A 104.8 . . ? C41 C42 H42A 104.8 . . ? C43 C42 H42B 104.8 . . ? C41 C42 H42B 104.8 . . ? H42A C42 H42B 105.8 . . ? C42 C43 C44 117(2) . . ? C42 C43 H43A 108.1 . . ? C44 C43 H43A 108.1 . . ? C42 C43 H43B 108.1 . . ? C44 C43 H43B 108.1 . . ? H43A C43 H43B 107.3 . . ? C45 C44 C43 110.9(17) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C40 C45 N14 115.0(17) . . ? C40 C45 C44 124.2(18) . . ? N14 C45 C44 120.4(17) . . ? N12 C46 C47 109.6(15) . . ? N12 C46 C51 124.1(16) . . ? C47 C46 C51 126.3(16) . . ? N15 C47 C46 110.2(15) . . ? N15 C47 C48 123.1(16) . . ? C46 C47 C48 126.6(16) . . ? C47 C48 C49 110.1(15) . . ? C47 C48 H48A 109.6 . . ? C49 C48 H48A 109.6 . . ? C47 C48 H48B 109.6 . . ? C49 C48 H48B 109.6 . . ? H48A C48 H48B 108.2 . . ? C50 C49 C48 110.1(17) . . ? C50 C49 H49A 109.6 . . ? C48 C49 H49A 109.6 . . ? C50 C49 H49B 109.6 . . ? C48 C49 H49B 109.6 . . ? H49A C49 H49B 108.2 . . ? C49 C50 C51 118.6(19) . . ? C49 C50 H50A 107.7 . . ? C51 C50 H50A 107.7 . . ? C49 C50 H50B 107.7 . . ? C51 C50 H50B 107.7 . . ? H50A C50 H50B 107.1 . . ? C46 C51 C50 101.1(15) . . ? C46 C51 H51A 111.6 . . ? C50 C51 H51A 111.6 . . ? C46 C51 H51B 111.6 . . ? C50 C51 H51B 111.6 . . ? H51A C51 H51B 109.4 . . ? C56 C52 C53 115.3(15) . . ? C56 C52 B4 127.7(17) . . ? C53 C52 B4 117.0(15) . . ? C54 C53 C52 120.6(15) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? N16 C54 C53 122.7(15) . . ? N16 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? N16 C55 C56 125.1(15) . . ? N16 C55 H55 117.5 . . ? C56 C55 H55 117.5 . . ? C52 C56 C55 120.3(17) . . ? C52 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? O13 C57 Re1 175(2) . . ? O14 C58 Re1 177(2) . . ? O16 C60 Re2 178.2(14) . . ? O17 C61 Re2 174.3(16) . . ? Cl3 C63 Cl5 110.2(12) . . ? Cl3 C63 Cl4 112.8(12) . . ? Cl5 C63 Cl4 107.5(11) . . ? Cl3 C63 H63 108.8 . . ? Cl5 C63 H63 108.8 . . ? Cl4 C63 H63 108.8 . . ? Cl6 C64 Cl7 114.7(17) . . ? Cl6 C64 Cl8 111.2(16) . . ? Cl7 C64 Cl8 107.7(15) . . ? Cl6 C64 H64 107.7 . . ? Cl7 C64 H64 107.7 . . ? Cl8 C64 H64 107.7 . . ? Cl10 C65 Cl11 110.9(16) . . ? Cl10 C65 Cl9 111.1(16) . . ? Cl11 C65 Cl9 107.1(15) . . ? Cl10 C65 H65 109.2 . . ? Cl11 C65 H65 109.2 . . ? Cl9 C65 H65 109.2 . . ? Cl14 C66 Cl12 110.0(17) . . ? Cl14 C66 Cl13 112.2(17) . . ? Cl12 C66 Cl13 109.9(16) . . ? Cl14 C66 H66 108.2 . . ? Cl12 C66 H66 108.2 . . ? Cl13 C66 H66 108.2 . . ? 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 C59B Re1 C59A O15A 167(6) . . . . ? C57 Re1 C59A O15A 137(7) . . . . ? C58 Re1 C59A O15A -133(7) . . . . ? N8 Re1 C59A O15A 45(7) . . . . ? N9 Re1 C59A O15A -43(7) . . . . ? Cl1B Re1 C59A O15A -9(5) . . . . ? Cl1A Re1 C59A O15A -177(4) . . . . ? C59A Re1 C59B O15B -172(8) . . . . ? C57 Re1 C59B O15B -143(9) . . . . ? C58 Re1 C59B O15B 130(9) . . . . ? N8 Re1 C59B O15B -48(9) . . . . ? N9 Re1 C59B O15B 37(9) . . . . ? Cl1B Re1 C59B O15B -153(14) . . . . ? Cl1A Re1 C59B O15B 34(8) . . . . ? C61 Re2 C62A O18A -105(21) . . . . ? C60 Re2 C62A O18A 168(21) . . . . ? C62B Re2 C62A O18A -172(17) . . . . ? N1 Re2 C62A O18A 73(21) 2_766 . . . ? N16 Re2 C62A O18A -11(21) . . . . ? Cl2A Re2 C62A O18A 146(14) . . . . ? Cl2B Re2 C62A O18A 3(15) . . . . ? C61 Re2 C62B O18B 134(26) . . . . ? C60 Re2 C62B O18B -139(26) . . . . ? C62A Re2 C62B O18B -158(21) . . . . ? N1 Re2 C62B O18B -44(26) 2_766 . . . ? N16 Re2 C62B O18B 40(26) . . . . ? Cl2A Re2 C62B O18B 4(17) . . . . ? Cl2B Re2 C62B O18B 116(92) . . . . ? B1 O1 N2 C6 171.6(18) . . . . ? B1 O1 N2 Fe1 -4(2) . . . . ? N7 Fe1 N2 C6 4.6(18) . . . . ? N3 Fe1 N2 C6 143.8(18) . . . . ? N6 Fe1 N2 C6 75(2) . . . . ? N5 Fe1 N2 C6 -66(2) . . . . ? N4 Fe1 N2 C6 -129.7(18) . . . . ? N7 Fe1 N2 O1 179.7(18) . . . . ? N3 Fe1 N2 O1 -41.1(16) . . . . ? N6 Fe1 N2 O1 -110.2(16) . . . . ? N5 Fe1 N2 O1 108.7(16) . . . . ? N4 Fe1 N2 O1 45.4(16) . . . . ? B1 O2 N3 C12 173.0(16) . . . . ? B1 O2 N3 Fe1 -8.8(19) . . . . ? N7 Fe1 N3 C12 -67.3(17) . . . . ? N2 Fe1 N3 C12 -134.2(15) . . . . ? N6 Fe1 N3 C12 -2.0(14) . . . . ? N5 Fe1 N3 C12 72.5(16) . . . . ? N4 Fe1 N3 C12 140.0(15) . . . . ? N7 Fe1 N3 O2 114.6(14) . . . . ? N2 Fe1 N3 O2 47.7(13) . . . . ? N6 Fe1 N3 O2 179.9(14) . . . . ? N5 Fe1 N3 O2 -105.6(13) . . . . ? N4 Fe1 N3 O2 -38.1(13) . . . . ? B1 O3 N4 C18 178.7(18) . . . . ? B1 O3 N4 Fe1 -8(2) . . . . ? N7 Fe1 N4 C18 65.8(19) . . . . ? N2 Fe1 N4 C18 134.5(17) . . . . ? N3 Fe1 N4 C18 -139.3(17) . . . . ? N6 Fe1 N4 C18 -74.4(19) . . . . ? N5 Fe1 N4 C18 -6.3(16) . . . . ? N7 Fe1 N4 O3 -107.1(13) . . . . ? N2 Fe1 N4 O3 -38.3(13) . . . . ? N3 Fe1 N4 O3 47.9(13) . . . . ? N6 Fe1 N4 O3 112.8(13) . . . . ? N5 Fe1 N4 O3 -179.2(14) . . . . ? B2 O4 N5 C23 165.8(19) . . . . ? B2 O4 N5 Fe1 -4(2) . . . . ? N7 Fe1 N5 C23 -126.1(19) . . . . ? N2 Fe1 N5 C23 -59(2) . . . . ? N3 Fe1 N5 C23 80(2) . . . . ? N6 Fe1 N5 C23 150.4(19) . . . . ? N4 Fe1 N5 C23 8.3(18) . . . . ? N7 Fe1 N5 O4 42.9(16) . . . . ? N2 Fe1 N5 O4 110.4(15) . . . . ? N3 Fe1 N5 O4 -110.5(15) . . . . ? N6 Fe1 N5 O4 -40.5(16) . . . . ? N4 Fe1 N5 O4 177.4(17) . . . . ? B2 O5 N6 C17 165.8(19) . . . . ? B2 O5 N6 Fe1 -9(2) . . . . ? N7 Fe1 N6 C17 147.1(17) . . . . ? N2 Fe1 N6 C17 79.6(18) . . . . ? N3 Fe1 N6 C17 6.4(15) . . . . ? N5 Fe1 N6 C17 -125.9(17) . . . . ? N4 Fe1 N6 C17 -61.8(19) . . . . ? N7 Fe1 N6 O5 -38.5(15) . . . . ? N2 Fe1 N6 O5 -106.0(15) . . . . ? N3 Fe1 N6 O5 -179.2(16) . . . . ? N5 Fe1 N6 O5 48.5(15) . . . . ? N4 Fe1 N6 O5 112.6(15) . . . . ? B2 O6 N7 C7 178(3) . . . . ? B2 O6 N7 Fe1 -14(3) . . . . ? N2 Fe1 N7 C7 -7(2) . . . . ? N3 Fe1 N7 C7 -77(3) . . . . ? N6 Fe1 N7 C7 -140(2) . . . . ? N5 Fe1 N7 C7 132(2) . . . . ? N4 Fe1 N7 C7 65(3) . . . . ? N2 Fe1 N7 O6 -175(2) . . . . ? N3 Fe1 N7 O6 115.1(18) . . . . ? N6 Fe1 N7 O6 52.3(19) . . . . ? N5 Fe1 N7 O6 -35(2) . . . . ? N4 Fe1 N7 O6 -102(2) . . . . ? C59B Re1 N8 C26 -14(2) . . . . ? C59A Re1 N8 C26 144(2) . . . . ? C57 Re1 N8 C26 66.3(16) . . . . ? C58 Re1 N8 C26 -77(18) . . . . ? N9 Re1 N8 C26 -112.4(14) . . . . ? Cl1B Re1 N8 C26 161.1(14) . . . . ? Cl1A Re1 N8 C26 -24.7(14) . . . . ? C59B Re1 N8 C27 163(2) . . . . ? C59A Re1 N8 C27 -40(2) . . . . ? C57 Re1 N8 C27 -117.1(17) . . . . ? C58 Re1 N8 C27 100(18) . . . . ? N9 Re1 N8 C27 64.2(15) . . . . ? Cl1B Re1 N8 C27 -22.3(15) . . . . ? Cl1A Re1 N8 C27 151.9(15) . . . . ? C59B Re1 N9 C29 134(2) . . . . ? C59A Re1 N9 C29 -33(2) . . . . ? C57 Re1 N9 C29 140(31) . . . . ? C58 Re1 N9 C29 46.0(16) . . . . ? N8 Re1 N9 C29 -135.3(15) . . . . ? Cl1B Re1 N9 C29 -44.8(15) . . . . ? Cl1A Re1 N9 C29 134.8(15) . . . . ? C59B Re1 N9 C33 -41(2) . . . . ? C59A Re1 N9 C33 152(2) . . . . ? C57 Re1 N9 C33 -35(32) . . . . ? C58 Re1 N9 C33 -128.9(14) . . . . ? N8 Re1 N9 C33 49.8(13) . . . . ? Cl1B Re1 N9 C33 140.3(14) . . . . ? Cl1A Re1 N9 C33 -40.1(13) . . . . ? B3 O7 N10 C34 160(2) . . . . ? B3 O7 N10 Fe2 -8(2) . . . . ? N13 Fe2 N10 C34 7.3(18) . . . . ? N12 Fe2 N10 C34 152.9(19) . . . . ? N14 Fe2 N10 C34 -54(2) . . . . ? N11 Fe2 N10 C34 -120.3(19) . . . . ? N15 Fe2 N10 C34 81(2) . . . . ? N13 Fe2 N10 O7 174.9(16) . . . . ? N12 Fe2 N10 O7 -39.5(15) . . . . ? N14 Fe2 N10 O7 113.2(15) . . . . ? N11 Fe2 N10 O7 47.4(15) . . . . ? N15 Fe2 N10 O7 -110.9(15) . . . . ? B3 O8 N11 C40 165.1(17) . . . . ? B3 O8 N11 Fe2 -11(2) . . . . ? N13 Fe2 N11 C40 78.2(16) . . . . ? N12 Fe2 N11 C40 -126.2(15) . . . . ? N14 Fe2 N11 C40 3.6(14) . . . . ? N15 Fe2 N11 C40 -63.1(19) . . . . ? N10 Fe2 N11 C40 148.5(15) . . . . ? N13 Fe2 N11 O8 -105.6(13) . . . . ? N12 Fe2 N11 O8 50.0(13) . . . . ? N14 Fe2 N11 O8 179.7(14) . . . . ? N15 Fe2 N11 O8 113.1(14) . . . . ? N10 Fe2 N11 O8 -35.3(13) . . . . ? B3 O9 N12 C46 164.6(17) . . . . ? B3 O9 N12 Fe2 -12(2) . . . . ? N13 Fe2 N12 C46 -66.2(18) . . . . ? N14 Fe2 N12 C46 75.2(18) . . . . ? N11 Fe2 N12 C46 145.8(16) . . . . ? N15 Fe2 N12 C46 -1.0(15) . . . . ? N10 Fe2 N12 C46 -125.6(16) . . . . ? N13 Fe2 N12 O9 109.7(14) . . . . ? N14 Fe2 N12 O9 -108.9(14) . . . . ? N11 Fe2 N12 O9 -38.3(13) . . . . ? N15 Fe2 N12 O9 174.9(15) . . . . ? N10 Fe2 N12 O9 50.3(14) . . . . ? B4 O10 N13 C39 171.2(16) . . . . ? B4 O10 N13 Fe2 -4(2) . . . . ? N12 Fe2 N13 C39 -64.9(19) . . . . ? N14 Fe2 N13 C39 144.9(16) . . . . ? N11 Fe2 N13 C39 74.5(17) . . . . ? N15 Fe2 N13 C39 -127.5(16) . . . . ? N10 Fe2 N13 C39 -2.4(15) . . . . ? N12 Fe2 N13 O10 109.6(15) . . . . ? N14 Fe2 N13 O10 -40.7(14) . . . . ? N11 Fe2 N13 O10 -111.0(13) . . . . ? N15 Fe2 N13 O10 47.0(14) . . . . ? N10 Fe2 N13 O10 172.1(15) . . . . ? B4 O11 N14 C45 163.9(17) . . . . ? B4 O11 N14 Fe2 -15(2) . . . . ? N13 Fe2 N14 O11 52.2(15) . . . . ? N12 Fe2 N14 O11 -104.4(15) . . . . ? N11 Fe2 N14 O11 -179.7(16) . . . . ? N15 Fe2 N14 O11 -33.0(15) . . . . ? N10 Fe2 N14 O11 110.8(16) . . . . ? N13 Fe2 N14 C45 -126.9(15) . . . . ? N12 Fe2 N14 C45 76.5(17) . . . . ? N11 Fe2 N14 C45 1.2(14) . . . . ? N15 Fe2 N14 C45 147.9(15) . . . . ? N10 Fe2 N14 C45 -68.2(18) . . . . ? B4 O12 N15 C47 163.6(18) . . . . ? B4 O12 N15 Fe2 -8(2) . . . . ? N13 Fe2 N15 O12 -40.8(16) . . . . ? N12 Fe2 N15 O12 174.5(17) . . . . ? N14 Fe2 N15 O12 45.0(16) . . . . ? N11 Fe2 N15 O12 108.5(16) . . . . ? N10 Fe2 N15 O12 -109.8(16) . . . . ? N13 Fe2 N15 C47 148.3(17) . . . . ? N12 Fe2 N15 C47 3.6(16) . . . . ? N14 Fe2 N15 C47 -126.0(17) . . . . ? N11 Fe2 N15 C47 -62(2) . . . . ? N10 Fe2 N15 C47 79.3(17) . . . . ? C61 Re2 N16 C55 -125.3(13) . . . . ? C60 Re2 N16 C55 -8(15) . . . . ? C62B Re2 N16 C55 -39(2) . . . . ? C62A Re2 N16 C55 144.6(18) . . . . ? N1 Re2 N16 C55 53.4(12) 2_766 . . . ? Cl2A Re2 N16 C55 -33.7(12) . . . . ? Cl2B Re2 N16 C55 141.8(12) . . . . ? C61 Re2 N16 C54 49.6(13) . . . . ? C60 Re2 N16 C54 166(15) . . . . ? C62B Re2 N16 C54 135.8(19) . . . . ? C62A Re2 N16 C54 -40.4(18) . . . . ? N1 Re2 N16 C54 -131.7(12) 2_766 . . . ? Cl2A Re2 N16 C54 141.2(11) . . . . ? Cl2B Re2 N16 C54 -43.3(11) . . . . ? N4 O3 B1 O2 -57(2) . . . . ? N4 O3 B1 O1 66.2(19) . . . . ? N4 O3 B1 C3 -172.8(14) . . . . ? N3 O2 B1 O3 67.4(19) . . . . ? N3 O2 B1 O1 -54.3(19) . . . . ? N3 O2 B1 C3 -173.5(13) . . . . ? N2 O1 B1 O3 -61(2) . . . . ? N2 O1 B1 O2 62(2) . . . . ? N2 O1 B1 C3 178.0(15) . . . . ? N7 O6 B2 O5 -53(2) . . . . ? N7 O6 B2 O4 70(2) . . . . ? N7 O6 B2 C24 -173.1(18) . . . . ? N6 O5 B2 O6 64(2) . . . . ? N6 O5 B2 O4 -55(2) . . . . ? N6 O5 B2 C24 -171.8(15) . . . . ? N5 O4 B2 O6 -59(2) . . . . ? N5 O4 B2 O5 61(2) . . . . ? N5 O4 B2 C24 179.1(16) . . . . ? N10 O7 B3 O9 64(2) . . . . ? N10 O7 B3 O8 -54(2) . . . . ? N10 O7 B3 C31 -172.5(16) . . . . ? N12 O9 B3 O7 -54(2) . . . . ? N12 O9 B3 O8 65.8(19) . . . . ? N12 O9 B3 C31 -176.7(15) . . . . ? N11 O8 B3 O7 66(2) . . . . ? N11 O8 B3 O9 -53(2) . . . . ? N11 O8 B3 C31 -173.7(14) . . . . ? N14 O11 B4 O10 -48(2) . . . . ? N14 O11 B4 O12 67(2) . . . . ? N14 O11 B4 C52 -169.8(15) . . . . ? N13 O10 B4 O11 57(2) . . . . ? N13 O10 B4 O12 -59.5(19) . . . . ? N13 O10 B4 C52 -177.2(14) . . . . ? N15 O12 B4 O11 -53(2) . . . . ? N15 O12 B4 O10 65(2) . . . . ? N15 O12 B4 C52 -178.6(16) . . . . ? C5 N1 C1 C2 9(2) . . . . ? Re2 N1 C1 C2 -174.4(12) 2_766 . . . ? N1 C1 C2 C3 -8(2) . . . . ? C1 C2 C3 C4 4(2) . . . . ? C1 C2 C3 B1 -178.8(15) . . . . ? O3 B1 C3 C2 85(2) . . . . ? O2 B1 C3 C2 -34(2) . . . . ? O1 B1 C3 C2 -154.8(17) . . . . ? O3 B1 C3 C4 -98(2) . . . . ? O2 B1 C3 C4 143.3(17) . . . . ? O1 B1 C3 C4 23(2) . . . . ? C2 C3 C4 C5 0(2) . . . . ? B1 C3 C4 C5 -177.9(16) . . . . ? C1 N1 C5 C4 -5(2) . . . . ? Re2 N1 C5 C4 178.2(13) 2_766 . . . ? C3 C4 C5 N1 1(3) . . . . ? O1 N2 C6 C7 -177.2(18) . . . . ? Fe1 N2 C6 C7 -2(3) . . . . ? O1 N2 C6 C11 1(3) . . . . ? Fe1 N2 C6 C11 177.2(19) . . . . ? O6 N7 C7 C6 178(2) . . . . ? Fe1 N7 C7 C6 9(4) . . . . ? O6 N7 C7 C8 -16(4) . . . . ? Fe1 N7 C7 C8 176(2) . . . . ? N2 C6 C7 N7 -4(3) . . . . ? C11 C6 C7 N7 177(3) . . . . ? N2 C6 C7 C8 -173(2) . . . . ? C11 C6 C7 C8 8(4) . . . . ? N7 C7 C8 C9 -158(3) . . . . ? C6 C7 C8 C9 9(3) . . . . ? C7 C8 C9 C10 -35(4) . . . . ? C8 C9 C10 C11 39(5) . . . . ? C9 C10 C11 C6 -18(4) . . . . ? N2 C6 C11 C10 175(2) . . . . ? C7 C6 C11 C10 -7(4) . . . . ? O2 N3 C12 C17 176.2(14) . . . . ? Fe1 N3 C12 C17 -2(2) . . . . ? O2 N3 C12 C13 1(2) . . . . ? Fe1 N3 C12 C13 -177.5(12) . . . . ? N3 C12 C13 C14 159.4(17) . . . . ? C17 C12 C13 C14 -16(2) . . . . ? C12 C13 C14 C15 45.8(19) . . . . ? C13 C14 C15 C16 -69.1(19) . . . . ? C14 C15 C16 C17 52(2) . . . . ? O5 N6 C17 C12 176.4(15) . . . . ? Fe1 N6 C17 C12 -9(2) . . . . ? O5 N6 C17 C16 -2(3) . . . . ? Fe1 N6 C17 C16 172.7(13) . . . . ? N3 C12 C17 N6 7(2) . . . . ? C13 C12 C17 N6 -177.5(16) . . . . ? N3 C12 C17 C16 -174.9(16) . . . . ? C13 C12 C17 C16 1(3) . . . . ? C15 C16 C17 N6 160.5(19) . . . . ? C15 C16 C17 C12 -18(2) . . . . ? O3 N4 C18 C23 176.9(15) . . . . ? Fe1 N4 C18 C23 4(2) . . . . ? O3 N4 C18 C19 2(3) . . . . ? Fe1 N4 C18 C19 -171.4(16) . . . . ? N4 C18 C19 C20 -167(2) . . . . ? C23 C18 C19 C20 18(3) . . . . ? C18 C19 C20 C21 -39(3) . . . . ? C19 C20 C21 C22 49(3) . . . . ? C20 C21 C22 C23 -35(3) . . . . ? O4 N5 C23 C18 -178.4(16) . . . . ? Fe1 N5 C23 C18 -9(3) . . . . ? O4 N5 C23 C22 8(3) . . . . ? Fe1 N5 C23 C22 177.6(17) . . . . ? N4 C18 C23 N5 3(3) . . . . ? C19 C18 C23 N5 179(2) . . . . ? N4 C18 C23 C22 177(2) . . . . ? C19 C18 C23 C22 -8(3) . . . . ? C21 C22 C23 N5 -172(2) . . . . ? C21 C22 C23 C18 15(3) . . . . ? O6 B2 C24 C25 158.8(19) . . . . ? O5 B2 C24 C25 37(2) . . . . ? O4 B2 C24 C25 -83(2) . . . . ? O6 B2 C24 C28 -17(3) . . . . ? O5 B2 C24 C28 -138.2(19) . . . . ? O4 B2 C24 C28 101(2) . . . . ? C28 C24 C25 C26 1(3) . . . . ? B2 C24 C25 C26 -174.3(16) . . . . ? C27 N8 C26 C25 3(2) . . . . ? Re1 N8 C26 C25 -179.7(11) . . . . ? C24 C25 C26 N8 -3(2) . . . . ? C26 N8 C27 C28 -3(3) . . . . ? Re1 N8 C27 C28 179.8(17) . . . . ? N8 C27 C28 C24 2(3) . . . . ? C25 C24 C28 C27 -1(3) . . . . ? B2 C24 C28 C27 175(2) . . . . ? C33 N9 C29 C30 -1(3) . . . . ? Re1 N9 C29 C30 -176.4(15) . . . . ? N9 C29 C30 C31 1(3) . . . . ? C29 C30 C31 C32 0(3) . . . . ? C29 C30 C31 B3 174(2) . . . . ? O7 B3 C31 C30 1(3) . . . . ? O9 B3 C31 C30 124(2) . . . . ? O8 B3 C31 C30 -119(2) . . . . ? O7 B3 C31 C32 175.0(17) . . . . ? O9 B3 C31 C32 -63(3) . . . . ? O8 B3 C31 C32 55(2) . . . . ? C30 C31 C32 C33 -1(3) . . . . ? B3 C31 C32 C33 -175.1(18) . . . . ? C31 C32 C33 N9 1(3) . . . . ? C29 N9 C33 C32 0(3) . . . . ? Re1 N9 C33 C32 175.2(13) . . . . ? O7 N10 C34 C39 -178.0(15) . . . . ? Fe2 N10 C34 C39 -9(2) . . . . ? O7 N10 C34 C35 3(3) . . . . ? Fe2 N10 C34 C35 172.0(18) . . . . ? N10 C34 C35 C36 -179(2) . . . . ? C39 C34 C35 C36 2(3) . . . . ? C34 C35 C36 C37 -25(4) . . . . ? C35 C36 C37 C38 41(4) . . . . ? C36 C37 C38 C39 -26(3) . . . . ? O10 N13 C39 C34 -176.7(14) . . . . ? Fe2 N13 C39 C34 -2(2) . . . . ? O10 N13 C39 C38 -1(3) . . . . ? Fe2 N13 C39 C38 174.2(13) . . . . ? N10 C34 C39 N13 7(2) . . . . ? C35 C34 C39 N13 -174.6(19) . . . . ? N10 C34 C39 C38 -169.1(18) . . . . ? C35 C34 C39 C38 10(3) . . . . ? C37 C38 C39 N13 -175(2) . . . . ? C37 C38 C39 C34 1(2) . . . . ? O8 N11 C40 C45 176.5(14) . . . . ? Fe2 N11 C40 C45 -7(2) . . . . ? O8 N11 C40 C41 4(3) . . . . ? Fe2 N11 C40 C41 179.9(13) . . . . ? N11 C40 C41 C42 172.6(19) . . . . ? C45 C40 C41 C42 1(3) . . . . ? C40 C41 C42 C43 -2(4) . . . . ? C41 C42 C43 C44 7(4) . . . . ? C42 C43 C44 C45 -11(3) . . . . ? N11 C40 C45 N14 8(2) . . . . ? C41 C40 C45 N14 -179.7(18) . . . . ? N11 C40 C45 C44 -179.5(16) . . . . ? C41 C40 C45 C44 -7(3) . . . . ? O11 N14 C45 C40 175.2(16) . . . . ? Fe2 N14 C45 C40 -6(2) . . . . ? O11 N14 C45 C44 2(3) . . . . ? Fe2 N14 C45 C44 -178.6(13) . . . . ? C43 C44 C45 C40 12(3) . . . . ? C43 C44 C45 N14 -176.3(17) . . . . ? O9 N12 C46 C47 -177.8(14) . . . . ? Fe2 N12 C46 C47 -1(2) . . . . ? O9 N12 C46 C51 1(3) . . . . ? Fe2 N12 C46 C51 176.8(13) . . . . ? O12 N15 C47 C46 -176.7(16) . . . . ? Fe2 N15 C47 C46 -5(2) . . . . ? O12 N15 C47 C48 -1(3) . . . . ? Fe2 N15 C47 C48 170.9(15) . . . . ? N12 C46 C47 N15 4(2) . . . . ? C51 C46 C47 N15 -174.3(18) . . . . ? N12 C46 C47 C48 -172.0(19) . . . . ? C51 C46 C47 C48 10(3) . . . . ? N15 C47 C48 C49 -166.0(19) . . . . ? C46 C47 C48 C49 9(3) . . . . ? C47 C48 C49 C50 -43(3) . . . . ? C48 C49 C50 C51 64(2) . . . . ? N12 C46 C51 C50 -173.1(18) . . . . ? C47 C46 C51 C50 5(2) . . . . ? C49 C50 C51 C46 -42(2) . . . . ? O11 B4 C52 C56 -129(2) . . . . ? O10 B4 C52 C56 107(2) . . . . ? O12 B4 C52 C56 -7(3) . . . . ? O11 B4 C52 C53 49(2) . . . . ? O10 B4 C52 C53 -75(2) . . . . ? O12 B4 C52 C53 171.0(16) . . . . ? C56 C52 C53 C54 -4(2) . . . . ? B4 C52 C53 C54 177.7(16) . . . . ? C55 N16 C54 C53 1(2) . . . . ? Re2 N16 C54 C53 -174.4(11) . . . . ? C52 C53 C54 N16 -1(2) . . . . ? C54 N16 C55 C56 4(2) . . . . ? Re2 N16 C55 C56 179.5(12) . . . . ? C53 C52 C56 C55 9(3) . . . . ? B4 C52 C56 C55 -173.0(17) . . . . ? N16 C55 C56 C52 -10(3) . . . . ? C59B Re1 C57 O13 170(21) . . . . ? C59A Re1 C57 O13 -23(21) . . . . ? C58 Re1 C57 O13 -101(21) . . . . ? N8 Re1 C57 O13 80(21) . . . . ? N9 Re1 C57 O13 164(21) . . . . ? Cl1B Re1 C57 O13 -11(21) . . . . ? Cl1A Re1 C57 O13 170(21) . . . . ? C59B Re1 C58 O14 -19(34) . . . . ? C59A Re1 C58 O14 -176(100) . . . . ? C57 Re1 C58 O14 -99(34) . . . . ? N8 Re1 C58 O14 44(46) . . . . ? N9 Re1 C58 O14 80(34) . . . . ? Cl1B Re1 C58 O14 166(34) . . . . ? Cl1A Re1 C58 O14 -8(34) . . . . ? C61 Re2 C60 O16 -62(50) . . . . ? C62B Re2 C60 O16 -148(50) . . . . ? C62A Re2 C60 O16 28(50) . . . . ? N1 Re2 C60 O16 119(50) 2_766 . . . ? N16 Re2 C60 O16 -179(100) . . . . ? Cl2A Re2 C60 O16 -154(50) . . . . ? Cl2B Re2 C60 O16 31(50) . . . . ? C60 Re2 C61 O17 142(17) . . . . ? C62B Re2 C61 O17 -133(17) . . . . ? C62A Re2 C61 O17 58(17) . . . . ? N1 Re2 C61 O17 -68(26) 2_766 . . . ? N16 Re2 C61 O17 -40(17) . . . . ? Cl2A Re2 C61 O17 -126(17) . . . . ? Cl2B Re2 C61 O17 46(17) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 22.21 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.805 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.149 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.079 0.421 0.035 2292 519 ' ' 2 0.308 0.633 0.470 6 1 ' ' 3 0.420 0.671 0.480 9 3 ' ' 4 0.593 0.334 0.521 11 3 ' ' 5 0.709 0.371 0.532 3 1 ' ' _platon_squeeze_details ; ; data_mdw2-7a _database_code_depnum_ccdc_archive 'CCDC 899212' #TrackingRef 'Ligand 1.cif' _audit_update_record ; 2012-06-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 B2 Fe N8 O6, 2(C7 H8)' _chemical_formula_sum 'C42 H48 B2 Fe N8 O6' _chemical_formula_weight 838.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.705(5) _cell_length_b 9.3657(12) _cell_length_c 20.454(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.680(9) _cell_angle_gamma 90.00 _cell_volume 3983.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 189 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5087 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23221 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4570 _reflns_number_gt 3742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+5.9823P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4570 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 Fe1 Fe 0.0000 0.40625(4) 0.2500 0.00988(9) Uani 1 2 d S . . O1 O 0.10637(6) 0.26219(13) 0.24403(7) 0.0138(3) Uani 1 1 d . . . O2 O 0.12140(6) 0.52163(13) 0.27008(7) 0.0129(3) Uani 1 1 d . . . O3 O 0.04784(6) 0.43559(13) 0.14322(6) 0.0133(3) Uani 1 1 d . . . N1 N 0.05208(7) 0.24876(15) 0.25225(8) 0.0111(3) Uani 1 1 d . . . N2 N 0.07798(7) 0.51383(15) 0.29705(8) 0.0114(3) Uani 1 1 d . . . N3 N -0.00245(7) 0.45838(15) 0.15827(8) 0.0113(3) Uani 1 1 d . . . N4 N 0.27444(7) 0.41596(18) 0.16665(8) 0.0196(3) Uani 1 1 d . . . B1 B 0.10934(9) 0.4055(2) 0.21333(11) 0.0127(4) Uani 1 1 d . . . C1 C 0.02995(8) 0.11869(18) 0.24825(9) 0.0120(4) Uani 1 1 d . . . C2 C 0.05987(8) -0.01509(19) 0.23899(10) 0.0159(4) Uani 1 1 d . . . H2A H 0.1009 -0.0332 0.2849 0.019 Uiso 1 1 calc R . . H2B H 0.0693 -0.0033 0.1971 0.019 Uiso 1 1 calc R . . C3 C 0.01455(9) -0.1429(2) 0.22347(10) 0.0182(4) Uani 1 1 d . . . H3A H 0.0387 -0.2327 0.2299 0.022 Uiso 1 1 calc R . . H3B H -0.0205 -0.1386 0.1713 0.022 Uiso 1 1 calc R . . C4 C 0.09601(8) 0.56808(18) 0.36326(9) 0.0118(3) Uani 1 1 d . . . C5 C 0.15621(8) 0.6530(2) 0.40793(10) 0.0160(4) Uani 1 1 d . . . H5A H 0.1527 0.7460 0.3833 0.019 Uiso 1 1 calc R . . H5B H 0.1934 0.6010 0.4101 0.019 Uiso 1 1 calc R . . C6 C 0.16719(9) 0.6784(2) 0.48751(10) 0.0212(4) Uani 1 1 d . . . H6A H 0.1843 0.5899 0.5170 0.025 Uiso 1 1 calc R . . H6B H 0.1999 0.7543 0.5114 0.025 Uiso 1 1 calc R . . C7 C -0.04942(8) 0.54045(19) 0.11164(9) 0.0122(3) Uani 1 1 d . . . C8 C -0.05545(8) 0.6007(2) 0.04064(9) 0.0156(4) Uani 1 1 d . . . H8A H -0.0686 0.5242 0.0027 0.019 Uiso 1 1 calc R . . H8B H -0.0132 0.6377 0.0497 0.019 Uiso 1 1 calc R . . C9 C -0.10539(9) 0.7222(2) 0.01112(10) 0.0193(4) Uani 1 1 d . . . H9A H -0.0871 0.8084 0.0422 0.023 Uiso 1 1 calc R . . H9B H -0.1156 0.7461 -0.0406 0.023 Uiso 1 1 calc R . . C10 C 0.16755(8) 0.40704(19) 0.19474(9) 0.0126(3) Uani 1 1 d . . . C11 C 0.18253(9) 0.5293(2) 0.16661(10) 0.0171(4) Uani 1 1 d . . . H11 H 0.1566 0.6124 0.1560 0.021 Uiso 1 1 calc R . . C12 C 0.23552(9) 0.5289(2) 0.15412(10) 0.0192(4) Uani 1 1 d . . . H12 H 0.2447 0.6138 0.1356 0.023 Uiso 1 1 calc R . . C13 C 0.25927(9) 0.2976(2) 0.19215(10) 0.0208(4) Uani 1 1 d . . . H13 H 0.2853 0.2152 0.2009 0.025 Uiso 1 1 calc R . . C14 C 0.20747(9) 0.2888(2) 0.20656(10) 0.0175(4) Uani 1 1 d . . . H14 H 0.1992 0.2020 0.2245 0.021 Uiso 1 1 calc R . . C15 C -0.15032(10) 0.1178(2) 0.00637(11) 0.0241(4) Uani 1 1 d . . . C16 C -0.17506(10) 0.0814(2) -0.06850(11) 0.0266(5) Uani 1 1 d . . . H16 H -0.2189 0.0537 -0.0967 0.032 Uiso 1 1 calc R . . C17 C -0.13644(11) 0.0850(2) -0.10241(11) 0.0276(5) Uani 1 1 d . . . H17 H -0.1539 0.0597 -0.1534 0.033 Uiso 1 1 calc R . . C18 C -0.07228(11) 0.1257(2) -0.06192(12) 0.0284(5) Uani 1 1 d . . . H18 H -0.0457 0.1265 -0.0849 0.034 Uiso 1 1 calc R . . C19 C -0.04737(10) 0.1651(2) 0.01221(12) 0.0278(5) Uani 1 1 d . . . H19 H -0.0038 0.1947 0.0399 0.033 Uiso 1 1 calc R . . C20 C -0.08618(10) 0.1611(2) 0.04578(11) 0.0256(5) Uani 1 1 d . . . H20 H -0.0688 0.1883 0.0966 0.031 Uiso 1 1 calc R . . C21 C -0.19097(12) 0.1076(3) 0.04509(14) 0.0389(6) Uani 1 1 d . . . H21A H -0.2365 0.1171 0.0082 0.058 Uiso 1 1 calc R . . H21B H -0.1789 0.1843 0.0820 0.058 Uiso 1 1 calc R . . H21C H -0.1838 0.0149 0.0701 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00753(17) 0.01026(17) 0.01127(17) 0.000 0.00405(14) 0.000 O1 0.0092(6) 0.0148(6) 0.0198(6) 0.0017(5) 0.0089(5) 0.0004(5) O2 0.0100(6) 0.0156(6) 0.0155(6) -0.0015(5) 0.0080(5) -0.0022(5) O3 0.0084(6) 0.0192(7) 0.0139(6) 0.0005(5) 0.0067(5) 0.0014(5) N1 0.0081(7) 0.0133(7) 0.0118(7) 0.0007(6) 0.0047(6) 0.0011(6) N2 0.0086(7) 0.0123(7) 0.0135(7) 0.0009(6) 0.0056(6) 0.0007(6) N3 0.0083(7) 0.0127(7) 0.0126(7) -0.0020(6) 0.0047(6) -0.0002(6) N4 0.0131(7) 0.0308(9) 0.0152(8) -0.0038(7) 0.0071(6) -0.0031(7) B1 0.0104(9) 0.0122(9) 0.0136(9) -0.0012(8) 0.0043(8) 0.0012(8) C1 0.0104(8) 0.0130(9) 0.0101(8) 0.0006(6) 0.0030(7) 0.0012(6) C2 0.0144(9) 0.0133(9) 0.0199(9) -0.0010(7) 0.0081(8) 0.0020(7) C3 0.0200(9) 0.0117(8) 0.0212(9) -0.0014(7) 0.0086(8) 0.0006(7) C4 0.0099(8) 0.0113(8) 0.0114(8) 0.0008(6) 0.0028(7) 0.0005(6) C5 0.0105(8) 0.0204(9) 0.0150(9) -0.0022(7) 0.0043(7) -0.0040(7) C6 0.0129(9) 0.0325(11) 0.0140(9) -0.0040(8) 0.0030(8) -0.0066(8) C7 0.0099(8) 0.0126(8) 0.0121(8) -0.0012(7) 0.0038(7) -0.0013(7) C8 0.0136(8) 0.0212(9) 0.0122(8) 0.0026(7) 0.0064(7) 0.0012(7) C9 0.0189(9) 0.0248(10) 0.0125(9) 0.0056(7) 0.0062(8) 0.0058(8) C10 0.0097(8) 0.0176(9) 0.0078(8) -0.0021(7) 0.0021(7) -0.0015(7) C11 0.0173(9) 0.0170(9) 0.0188(9) -0.0028(7) 0.0101(8) -0.0003(7) C12 0.0204(10) 0.0208(10) 0.0194(9) -0.0038(8) 0.0120(8) -0.0065(8) C13 0.0157(9) 0.0292(11) 0.0172(9) 0.0037(8) 0.0076(8) 0.0074(8) C14 0.0159(9) 0.0205(10) 0.0168(9) 0.0035(7) 0.0085(8) 0.0035(8) C15 0.0289(11) 0.0196(10) 0.0271(11) 0.0065(8) 0.0162(9) 0.0022(8) C16 0.0233(10) 0.0260(11) 0.0261(11) 0.0026(9) 0.0084(9) -0.0046(9) C17 0.0363(12) 0.0261(11) 0.0198(10) -0.0027(9) 0.0130(9) -0.0039(10) C18 0.0318(12) 0.0302(12) 0.0311(12) -0.0037(9) 0.0214(10) -0.0049(9) C19 0.0250(11) 0.0301(12) 0.0260(11) -0.0030(9) 0.0104(9) -0.0058(9) C20 0.0342(12) 0.0239(11) 0.0178(10) 0.0000(8) 0.0118(9) -0.0024(9) C21 0.0447(14) 0.0411(14) 0.0422(14) 0.0082(11) 0.0301(12) 0.0014(12) _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 N1 1.9098(15) . ? Fe1 N1 1.9098(15) 2 ? Fe1 N2 1.9106(15) . ? Fe1 N2 1.9107(15) 2 ? Fe1 N3 1.9124(14) . ? Fe1 N3 1.9124(14) 2 ? O1 N1 1.3813(18) . ? O1 B1 1.497(2) . ? O2 N2 1.3836(18) . ? O2 B1 1.515(2) . ? O3 N3 1.3834(18) . ? O3 B1 1.502(2) . ? N1 C1 1.313(2) . ? N2 C4 1.311(2) . ? N3 C7 1.312(2) . ? N4 C12 1.345(3) . ? N4 C13 1.346(3) . ? B1 C10 1.598(3) . ? C1 C1 1.455(3) 2 ? C1 C2 1.496(2) . ? C2 C3 1.536(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C3 1.540(4) 2 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.447(2) 2 ? C4 C5 1.501(2) . ? C5 C6 1.539(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C9 1.535(3) 2 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C4 1.447(2) 2 ? C7 C8 1.500(2) . ? C8 C9 1.541(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C6 1.535(3) 2 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C14 1.400(2) . ? C10 C11 1.402(3) . ? C11 C12 1.397(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.396(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.394(3) . ? C15 C20 1.396(3) . ? C15 C21 1.516(3) . ? C16 C17 1.389(3) . ? C16 H16 0.9500 . ? C17 C18 1.391(3) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 78.88(9) . 2 ? N1 Fe1 N2 86.40(6) . . ? N1 Fe1 N2 151.33(6) 2 . ? N1 Fe1 N2 151.33(6) . 2 ? N1 Fe1 N2 86.40(6) 2 2 ? N2 Fe1 N2 116.35(9) . 2 ? N1 Fe1 N3 86.32(6) . . ? N1 Fe1 N3 117.30(6) 2 . ? N2 Fe1 N3 85.76(6) . . ? N2 Fe1 N3 78.74(6) 2 . ? N1 Fe1 N3 117.30(6) . 2 ? N1 Fe1 N3 86.31(6) 2 2 ? N2 Fe1 N3 78.74(6) . 2 ? N2 Fe1 N3 85.76(6) 2 2 ? N3 Fe1 N3 150.42(9) . 2 ? N1 O1 B1 111.51(12) . . ? N2 O2 B1 111.39(12) . . ? N3 O3 B1 111.21(12) . . ? C1 N1 O1 116.40(14) . . ? C1 N1 Fe1 118.72(12) . . ? O1 N1 Fe1 123.78(10) . . ? C4 N2 O2 117.08(14) . . ? C4 N2 Fe1 118.79(12) . . ? O2 N2 Fe1 123.51(10) . . ? C7 N3 O3 116.74(14) . . ? C7 N3 Fe1 118.58(12) . . ? O3 N3 Fe1 123.73(10) . . ? C12 N4 C13 115.79(16) . . ? O1 B1 O3 110.45(14) . . ? O1 B1 O2 110.61(14) . . ? O3 B1 O2 109.67(14) . . ? O1 B1 C10 109.14(14) . . ? O3 B1 C10 108.93(14) . . ? O2 B1 C10 107.99(14) . . ? N1 C1 C1 111.53(10) . 2 ? N1 C1 C2 125.82(16) . . ? C1 C1 C2 122.63(10) 2 . ? C1 C2 C3 110.59(15) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C3 111.08(13) . 2 ? C2 C3 H3A 109.4 . . ? C3 C3 H3A 109.4 2 . ? C2 C3 H3B 109.4 . . ? C3 C3 H3B 109.4 2 . ? H3A C3 H3B 108.0 . . ? N2 C4 C7 111.79(15) . 2 ? N2 C4 C5 125.28(16) . . ? C7 C4 C5 122.91(15) 2 . ? C4 C5 C6 110.78(15) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C9 C6 C5 112.48(15) 2 . ? C9 C6 H6A 109.1 2 . ? C5 C6 H6A 109.1 . . ? C9 C6 H6B 109.1 2 . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N3 C7 C4 111.89(15) . 2 ? N3 C7 C8 125.30(16) . . ? C4 C7 C8 122.81(15) 2 . ? C7 C8 C9 110.84(15) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C6 C9 C8 110.86(16) 2 . ? C6 C9 H9A 109.5 2 . ? C8 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 2 . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C14 C10 C11 115.68(16) . . ? C14 C10 B1 122.75(16) . . ? C11 C10 B1 121.55(16) . . ? C12 C11 C10 120.00(18) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? N4 C12 C11 124.23(18) . . ? N4 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? N4 C13 C14 123.78(18) . . ? N4 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C10 120.48(18) . . ? C13 C14 H14 119.8 . . ? C10 C14 H14 119.8 . . ? C16 C15 C20 118.21(19) . . ? C16 C15 C21 121.4(2) . . ? C20 C15 C21 120.4(2) . . ? C17 C16 C15 120.77(19) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.25(19) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 119.9(2) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C15 121.27(19) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? 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 B1 O1 N1 C1 152.59(15) . . . . ? B1 O1 N1 Fe1 -15.23(17) . . . . ? N1 Fe1 N1 C1 2.77(9) 2 . . . ? N2 Fe1 N1 C1 158.04(13) . . . . ? N2 Fe1 N1 C1 -57.7(2) 2 . . . ? N3 Fe1 N1 C1 -115.99(13) . . . . ? N3 Fe1 N1 C1 82.68(14) 2 . . . ? N1 Fe1 N1 O1 170.32(16) 2 . . . ? N2 Fe1 N1 O1 -34.40(12) . . . . ? N2 Fe1 N1 O1 109.86(15) 2 . . . ? N3 Fe1 N1 O1 51.57(12) . . . . ? N3 Fe1 N1 O1 -109.77(12) 2 . . . ? B1 O2 N2 C4 155.08(15) . . . . ? B1 O2 N2 Fe1 -15.74(17) . . . . ? N1 Fe1 N2 C4 -118.56(13) . . . . ? N1 Fe1 N2 C4 -59.8(2) 2 . . . ? N2 Fe1 N2 C4 79.67(13) 2 . . . ? N3 Fe1 N2 C4 154.88(14) . . . . ? N3 Fe1 N2 C4 0.20(13) 2 . . . ? N1 Fe1 N2 O2 52.12(12) . . . . ? N1 Fe1 N2 O2 110.93(15) 2 . . . ? N2 Fe1 N2 O2 -109.65(12) 2 . . . ? N3 Fe1 N2 O2 -34.44(12) . . . . ? N3 Fe1 N2 O2 170.88(13) 2 . . . ? B1 O3 N3 C7 152.42(15) . . . . ? B1 O3 N3 Fe1 -16.28(17) . . . . ? N1 Fe1 N3 C7 158.28(14) . . . . ? N1 Fe1 N3 C7 82.81(14) 2 . . . ? N2 Fe1 N3 C7 -115.06(14) . . . . ? N2 Fe1 N3 C7 2.88(13) 2 . . . ? N3 Fe1 N3 C7 -56.89(12) 2 . . . ? N1 Fe1 N3 O3 -33.22(12) . . . . ? N1 Fe1 N3 O3 -108.70(12) 2 . . . ? N2 Fe1 N3 O3 53.43(12) . . . . ? N2 Fe1 N3 O3 171.37(13) 2 . . . ? N3 Fe1 N3 O3 111.61(12) 2 . . . ? N1 O1 B1 O3 -52.64(17) . . . . ? N1 O1 B1 O2 68.96(16) . . . . ? N1 O1 B1 C10 -172.38(12) . . . . ? N3 O3 B1 O1 69.89(17) . . . . ? N3 O3 B1 O2 -52.27(18) . . . . ? N3 O3 B1 C10 -170.25(13) . . . . ? N2 O2 B1 O1 -52.00(17) . . . . ? N2 O2 B1 O3 70.06(17) . . . . ? N2 O2 B1 C10 -171.36(13) . . . . ? O1 N1 C1 C1 -175.47(15) . . . 2 ? Fe1 N1 C1 C1 -7.0(2) . . . 2 ? O1 N1 C1 C2 2.8(2) . . . . ? Fe1 N1 C1 C2 171.29(13) . . . . ? N1 C1 C2 C3 -170.47(16) . . . . ? C1 C1 C2 C3 7.6(3) 2 . . . ? C1 C2 C3 C3 -45.2(2) . . . 2 ? O2 N2 C4 C7 -174.08(13) . . . 2 ? Fe1 N2 C4 C7 -2.80(19) . . . 2 ? O2 N2 C4 C5 7.8(2) . . . . ? Fe1 N2 C4 C5 179.06(13) . . . . ? N2 C4 C5 C6 -170.84(17) . . . . ? C7 C4 C5 C6 11.2(2) 2 . . . ? C4 C5 C6 C9 -44.1(2) . . . 2 ? O3 N3 C7 C4 -174.33(13) . . . 2 ? Fe1 N3 C7 C4 -5.03(19) . . . 2 ? O3 N3 C7 C8 5.4(2) . . . . ? Fe1 N3 C7 C8 174.70(13) . . . . ? N3 C7 C8 C9 -164.88(17) . . . . ? C4 C7 C8 C9 14.8(2) 2 . . . ? C7 C8 C9 C6 -46.9(2) . . . 2 ? O1 B1 C10 C14 0.2(2) . . . . ? O3 B1 C10 C14 -120.51(17) . . . . ? O2 B1 C10 C14 120.45(17) . . . . ? O1 B1 C10 C11 -178.61(15) . . . . ? O3 B1 C10 C11 60.7(2) . . . . ? O2 B1 C10 C11 -58.3(2) . . . . ? C14 C10 C11 C12 -1.7(3) . . . . ? B1 C10 C11 C12 177.14(16) . . . . ? C13 N4 C12 C11 0.7(3) . . . . ? C10 C11 C12 N4 0.7(3) . . . . ? C12 N4 C13 C14 -1.0(3) . . . . ? N4 C13 C14 C10 0.0(3) . . . . ? C11 C10 C14 C13 1.4(3) . . . . ? B1 C10 C14 C13 -177.44(16) . . . . ? C20 C15 C16 C17 1.4(3) . . . . ? C21 C15 C16 C17 -177.1(2) . . . . ? C15 C16 C17 C18 -0.2(3) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C17 C18 C19 C20 1.2(3) . . . . ? C18 C19 C20 C15 0.1(3) . . . . ? C16 C15 C20 C19 -1.3(3) . . . . ? C21 C15 C20 C19 177.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.379 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.059 _iucr_refine_instructions_details ; TITL MDW2-7a in C2/c CELL 0.71073 23.7046 9.3657 20.4539 90.0000 118.6802 90.0000 ZERR 4.00 0.0053 0.0012 0.0025 0.0000 0.0090 0.0000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H B N O FE UNIT 168 192 8 32 24 4 REM ---------------------------------------------------------- REM Data collection: Bruker Nonius APEX II CCD REM Absorption correction: SADABS REM Crystal habit: prismatic; Crystal colour: red REM Mole 1 is the Fe(II) complex REM Mole 2 is a solvent molecule (toluene) REM ---------------------------------------------------------- L.S. 10 ACTA CONF WPDB -2 SIZE 0.445 0.116 0.115 BOND $H FMAP 2 PLAN 10 TEMP -173 WGHT 0.020200 5.982300 FVAR 0.30505 MOLE 1 FE1 6 0.000000 0.406248 0.250000 10.50000 0.00753 0.01026 = 0.01127 0.00000 0.00405 0.00000 O1 5 0.106374 0.262191 0.244032 11.00000 0.00922 0.01480 = 0.01979 0.00166 0.00891 0.00043 O2 5 0.121397 0.521634 0.270076 11.00000 0.00996 0.01557 = 0.01551 -0.00150 0.00796 -0.00223 O3 5 0.047839 0.435586 0.143218 11.00000 0.00844 0.01915 = 0.01388 0.00052 0.00668 0.00141 N1 4 0.052084 0.248763 0.252253 11.00000 0.00811 0.01326 = 0.01184 0.00067 0.00475 0.00114 N2 4 0.077975 0.513828 0.297049 11.00000 0.00864 0.01233 = 0.01355 0.00088 0.00563 0.00066 N3 4 -0.002448 0.458382 0.158273 11.00000 0.00833 0.01270 = 0.01256 -0.00199 0.00474 -0.00023 N4 4 0.274443 0.415958 0.166652 11.00000 0.01309 0.03084 = 0.01522 -0.00384 0.00711 -0.00313 B1 3 0.109338 0.405458 0.213331 11.00000 0.01042 0.01225 = 0.01365 -0.00120 0.00432 0.00120 C1 1 0.029945 0.118693 0.248252 11.00000 0.01039 0.01301 = 0.01015 0.00059 0.00304 0.00123 C2 1 0.059870 -0.015088 0.238993 11.00000 0.01437 0.01328 = 0.01988 -0.00101 0.00814 0.00197 AFIX 23 H2A 2 0.100945 -0.033229 0.284851 11.00000 -1.20000 H2B 2 0.069335 -0.003318 0.197130 11.00000 -1.20000 AFIX 0 C3 1 0.014552 -0.142887 0.223474 11.00000 0.01999 0.01171 = 0.02119 -0.00140 0.00856 0.00056 AFIX 23 H3A 2 0.038678 -0.232714 0.229876 11.00000 -1.20000 H3B 2 -0.020472 -0.138588 0.171273 11.00000 -1.20000 AFIX 0 C4 1 0.096005 0.568083 0.363259 11.00000 0.00991 0.01130 = 0.01136 0.00082 0.00284 0.00048 C5 1 0.156207 0.653004 0.407934 11.00000 0.01047 0.02045 = 0.01497 -0.00221 0.00434 -0.00399 AFIX 23 H5A 2 0.152727 0.745998 0.383261 11.00000 -1.20000 H5B 2 0.193444 0.601026 0.410129 11.00000 -1.20000 AFIX 0 C6 1 0.167193 0.678421 0.487514 11.00000 0.01289 0.03250 = 0.01399 -0.00404 0.00300 -0.00660 AFIX 23 H6A 2 0.184258 0.589933 0.517004 11.00000 -1.20000 H6B 2 0.199869 0.754290 0.511351 11.00000 -1.20000 AFIX 0 C7 1 -0.049418 0.540453 0.111642 11.00000 0.00990 0.01265 = 0.01208 -0.00119 0.00380 -0.00128 C8 1 -0.055447 0.600743 0.040639 11.00000 0.01358 0.02120 = 0.01223 0.00262 0.00636 0.00124 AFIX 23 H8A 2 -0.068627 0.524207 0.002732 11.00000 -1.20000 H8B 2 -0.013180 0.637694 0.049669 11.00000 -1.20000 AFIX 0 C9 1 -0.105390 0.722234 0.011119 11.00000 0.01891 0.02481 = 0.01249 0.00560 0.00618 0.00584 AFIX 23 H9A 2 -0.087113 0.808431 0.042250 11.00000 -1.20000 H9B 2 -0.115606 0.746097 -0.040557 11.00000 -1.20000 AFIX 0 C10 1 0.167550 0.407040 0.194740 11.00000 0.00975 0.01765 = 0.00782 -0.00211 0.00209 -0.00151 C11 1 0.182535 0.529286 0.166606 11.00000 0.01726 0.01704 = 0.01883 -0.00279 0.01013 -0.00030 AFIX 43 H11 2 0.156648 0.612444 0.156027 11.00000 -1.20000 AFIX 0 C12 1 0.235520 0.528857 0.154123 11.00000 0.02045 0.02081 = 0.01936 -0.00375 0.01205 -0.00648 AFIX 43 H12 2 0.244651 0.613812 0.135584 11.00000 -1.20000 AFIX 0 C13 1 0.259267 0.297576 0.192153 11.00000 0.01568 0.02921 = 0.01717 0.00365 0.00756 0.00737 AFIX 43 H13 2 0.285310 0.215204 0.200854 11.00000 -1.20000 AFIX 0 C14 1 0.207474 0.288824 0.206556 11.00000 0.01586 0.02047 = 0.01684 0.00349 0.00850 0.00348 AFIX 43 H14 2 0.199250 0.202020 0.224509 11.00000 -1.20000 AFIX 0 MOLE 2 C15 1 -0.150320 0.117833 0.006369 11.00000 0.02895 0.01962 = 0.02709 0.00646 0.01616 0.00215 C16 1 -0.175064 0.081367 -0.068503 11.00000 0.02335 0.02598 = 0.02612 0.00258 0.00841 -0.00465 AFIX 43 H16 2 -0.218850 0.053681 -0.096666 11.00000 -1.20000 AFIX 0 C17 1 -0.136437 0.085042 -0.102407 11.00000 0.03625 0.02612 = 0.01983 -0.00267 0.01298 -0.00392 AFIX 43 H17 2 -0.153904 0.059673 -0.153437 11.00000 -1.20000 AFIX 0 C18 1 -0.072282 0.125727 -0.061922 11.00000 0.03183 0.03021 = 0.03113 -0.00370 0.02141 -0.00490 AFIX 43 H18 2 -0.045691 0.126548 -0.084896 11.00000 -1.20000 AFIX 0 C19 1 -0.047371 0.165095 0.012213 11.00000 0.02498 0.03009 = 0.02604 -0.00302 0.01042 -0.00581 AFIX 43 H19 2 -0.003823 0.194750 0.039948 11.00000 -1.20000 AFIX 0 C20 1 -0.086181 0.161077 0.045779 11.00000 0.03416 0.02394 = 0.01777 0.00001 0.01182 -0.00238 AFIX 43 H20 2 -0.068771 0.188277 0.096557 11.00000 -1.20000 AFIX 0 C21 1 -0.190969 0.107633 0.045093 11.00000 0.04468 0.04112 = 0.04224 0.00820 0.03006 0.00140 AFIX 33 H21A 2 -0.236499 0.117129 0.008203 11.00000 -1.50000 H21B 2 -0.178900 0.184250 0.082042 11.00000 -1.50000 H21C 2 -0.183789 0.014925 0.070070 11.00000 -1.50000 MOLE 0 HKLF 4 REM MDW2-7a in C2/c REM R1 = 0.0406 for 3742 Fo > 4sig(Fo) and 0.0572 for all 4570 data REM 267 parameters refined using 0 restraints END WGHT 0.0200 5.9951 REM Highest difference peak 0.379, deepest hole -0.522, 1-sigma level 0.059 Q1 1 -0.0770 0.5361 0.1171 11.00000 0.05 0.38 Q2 1 0.0047 0.5003 0.2721 11.00000 0.05 0.37 Q3 1 0.0210 0.2999 0.2705 11.00000 0.05 0.36 Q4 1 0.1377 0.4017 0.2021 11.00000 0.05 0.35 Q5 1 0.0342 0.4106 0.2355 11.00000 0.05 0.34 Q6 1 0.0000 0.1082 0.2500 10.50000 0.05 0.34 Q7 1 0.0469 0.0538 0.2521 11.00000 0.05 0.32 Q8 1 0.1259 0.5910 0.3879 11.00000 0.05 0.31 Q9 1 -0.0598 0.5623 0.0701 11.00000 0.05 0.30 Q10 1 -0.0298 0.4874 0.1282 11.00000 0.05 0.30 ; data_mdw1-86f3 _database_code_depnum_ccdc_archive 'CCDC 899213' #TrackingRef 'Ligand 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H62 B4 Fe2 N14 O12, 4(C H2 Cl2), 2(Cl)' _chemical_formula_sum 'C56 H70 B4 Cl10 Fe2 N14 O12' _chemical_formula_weight 1640.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.235(5) _cell_length_b 10.862(4) _cell_length_c 16.008(6) _cell_angle_alpha 97.163(18) _cell_angle_beta 98.93(2) _cell_angle_gamma 93.02(2) _cell_volume 1739.6(12) _cell_formula_units_Z 1 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 523 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 marmux _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12176 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.66 _reflns_number_total 7357 _reflns_number_gt 5047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marmux - Micro-beam system, marresearch, 2010' _computing_cell_refinement 'automar, marresearch, 2010' _computing_data_reduction 'automar, marresearch, 2010' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+1.4142P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7357 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2018 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Fe1 Fe 0.32099(6) 0.27829(6) 0.28707(4) 0.02832(18) Uani 1 1 d . . . O1 O 0.5752(3) 0.3837(3) 0.2584(2) 0.0360(7) Uani 1 1 d . . . O2 O 0.4247(3) 0.2918(3) 0.12820(19) 0.0345(7) Uani 1 1 d . . . O3 O 0.3819(3) 0.4936(3) 0.2037(2) 0.0352(7) Uani 1 1 d . . . O4 O 0.0705(3) 0.2250(3) 0.34486(19) 0.0326(7) Uani 1 1 d . . . O5 O 0.2123(3) 0.0501(3) 0.33477(19) 0.0339(7) Uani 1 1 d . . . O6 O 0.2668(3) 0.2213(3) 0.45234(19) 0.0350(7) Uani 1 1 d . . . N1 N 0.5039(4) 0.3367(3) 0.3145(2) 0.0332(8) Uani 1 1 d . . . N2 N 0.3604(4) 0.2194(3) 0.1763(2) 0.0313(8) Uani 1 1 d . . . N3 N 0.2925(4) 0.4338(3) 0.2453(2) 0.0334(8) Uani 1 1 d . . . N4 N 0.1415(3) 0.3000(3) 0.3017(2) 0.0299(8) Uani 1 1 d . . . N5 N 0.2752(3) 0.1048(3) 0.2781(2) 0.0312(8) Uani 1 1 d . . . N6 N 0.3549(4) 0.2743(3) 0.4077(2) 0.0322(8) Uani 1 1 d . . . N7 N 0.7412(4) 0.5889(4) 0.0294(2) 0.0381(9) Uani 1 1 d . . . H7 H 0.7932 0.6246 -0.0009 0.046 Uiso 1 1 calc R . . B1 B 0.4853(5) 0.4101(5) 0.1809(3) 0.0322(10) Uani 1 1 d . . . B2 B 0.1567(5) 0.1428(5) 0.3938(3) 0.0293(10) Uani 1 1 d . . . C1 C 0.5623(4) 0.3472(4) 0.3940(3) 0.0319(9) Uani 1 1 d . . . C2 C 0.7032(4) 0.3960(5) 0.4268(3) 0.0401(11) Uani 1 1 d . . . H2A H 0.7195 0.4775 0.4073 0.048 Uiso 1 1 calc R . . H2B H 0.7638 0.3379 0.4031 0.048 Uiso 1 1 calc R . . C3 C 0.7325(5) 0.4106(5) 0.5232(3) 0.0472(12) Uani 1 1 d . . . H3A H 0.6953 0.4873 0.5467 0.057 Uiso 1 1 calc R . . H3B H 0.8297 0.4195 0.5421 0.057 Uiso 1 1 calc R . . C4 C 0.6740(5) 0.3002(5) 0.5576(3) 0.0478(12) Uani 1 1 d . . . H4A H 0.7040 0.3087 0.6200 0.057 Uiso 1 1 calc R . . H4B H 0.7079 0.2233 0.5316 0.057 Uiso 1 1 calc R . . C5 C 0.5226(5) 0.2879(5) 0.5395(3) 0.0417(11) Uani 1 1 d . . . H5A H 0.4898 0.2054 0.5511 0.050 Uiso 1 1 calc R . . H5B H 0.4873 0.3526 0.5773 0.050 Uiso 1 1 calc R . . C6 C 0.4757(4) 0.3025(4) 0.4480(3) 0.0325(9) Uani 1 1 d . . . C7 C 0.3487(4) 0.0998(4) 0.1510(3) 0.0324(9) Uani 1 1 d . . . C8 C 0.3957(5) 0.0355(4) 0.0748(3) 0.0380(10) Uani 1 1 d . . . H8A H 0.4851 0.0716 0.0711 0.046 Uiso 1 1 calc R . . H8B H 0.3350 0.0479 0.0225 0.046 Uiso 1 1 calc R . . C9 C 0.4008(6) -0.1040(5) 0.0807(4) 0.0507(13) Uani 1 1 d . . . H9A H 0.4146 -0.1477 0.0251 0.061 Uiso 1 1 calc R . . H9B H 0.4773 -0.1169 0.1240 0.061 Uiso 1 1 calc R . . C10 C 0.2779(6) -0.1585(5) 0.1039(4) 0.0496(13) Uani 1 1 d . . . H10A H 0.2824 -0.2497 0.1012 0.059 Uiso 1 1 calc R . . H10B H 0.2011 -0.1427 0.0618 0.059 Uiso 1 1 calc R . . C11 C 0.2566(5) -0.1047(4) 0.1935(3) 0.0362(10) Uani 1 1 d . . . H11A H 0.1631 -0.1230 0.1996 0.043 Uiso 1 1 calc R . . H11B H 0.3136 -0.1445 0.2366 0.043 Uiso 1 1 calc R . . C12 C 0.2891(4) 0.0328(4) 0.2089(3) 0.0311(9) Uani 1 1 d . . . C13 C 0.1775(4) 0.4779(4) 0.2439(3) 0.0286(8) Uani 1 1 d . A . C14 C 0.1330(5) 0.5910(4) 0.2066(3) 0.0363(10) Uani 1 1 d . . . H14A H 0.0987 0.5689 0.1449 0.044 Uiso 0.49(3) 1 calc PR A 1 H14B H 0.2088 0.6539 0.2132 0.044 Uiso 0.49(3) 1 calc PR A 1 H14C H 0.1462 0.5831 0.1462 0.044 Uiso 0.51(3) 1 calc PR A 2 H14D H 0.1885 0.6650 0.2377 0.044 Uiso 0.51(3) 1 calc PR A 2 C15A C 0.0208(14) 0.6462(13) 0.2539(12) 0.037(3) Uani 0.49(3) 1 d P A 1 H15A H 0.0579 0.6776 0.3141 0.045 Uiso 0.49(3) 1 calc PR A 1 H15B H -0.0154 0.7165 0.2261 0.045 Uiso 0.49(3) 1 calc PR A 1 C16A C -0.0899(14) 0.5438(15) 0.2501(13) 0.042(3) Uani 0.49(3) 1 d P A 1 H16A H -0.1656 0.5803 0.2733 0.051 Uiso 0.49(3) 1 calc PR A 1 H16B H -0.1213 0.5079 0.1899 0.051 Uiso 0.49(3) 1 calc PR A 1 C15B C -0.0101(13) 0.6101(15) 0.2110(14) 0.047(4) Uani 0.51(3) 1 d P A 2 H15C H -0.0255 0.6983 0.2059 0.056 Uiso 0.51(3) 1 calc PR A 2 H15D H -0.0657 0.5585 0.1616 0.056 Uiso 0.51(3) 1 calc PR A 2 C16B C -0.0532(18) 0.5788(15) 0.2898(15) 0.048(4) Uani 0.51(3) 1 d P A 2 H16C H -0.1468 0.5983 0.2890 0.058 Uiso 0.51(3) 1 calc PR A 2 H16D H 0.0010 0.6314 0.3394 0.058 Uiso 0.51(3) 1 calc PR A 2 C17 C -0.0410(4) 0.4417(4) 0.3011(3) 0.0360(10) Uani 1 1 d . . . H17A H -0.0336 0.4719 0.3627 0.043 Uiso 0.49(3) 1 calc PR A 1 H17B H -0.1068 0.3690 0.2873 0.043 Uiso 0.49(3) 1 calc PR A 1 H17C H -0.0506 0.4297 0.3602 0.043 Uiso 0.51(3) 1 calc PR A 2 H17D H -0.1128 0.3898 0.2617 0.043 Uiso 0.51(3) 1 calc PR A 2 C18 C 0.0899(4) 0.4018(4) 0.2832(3) 0.0293(9) Uani 1 1 d . A . C19 C 0.5750(4) 0.4776(4) 0.1237(3) 0.0330(9) Uani 1 1 d . . . C20 C 0.5715(5) 0.6023(4) 0.1133(3) 0.0381(10) Uani 1 1 d . . . H20 H 0.5098 0.6513 0.1383 0.046 Uiso 1 1 calc R . . C21 C 0.6567(5) 0.6558(5) 0.0669(3) 0.0438(12) Uani 1 1 d . . . H21 H 0.6547 0.7419 0.0618 0.053 Uiso 1 1 calc R . . C22 C 0.7491(5) 0.4693(5) 0.0368(3) 0.0412(11) Uani 1 1 d . . . H22 H 0.8112 0.4235 0.0098 0.049 Uiso 1 1 calc R . . C23 C 0.6683(5) 0.4108(5) 0.0833(3) 0.0408(11) Uani 1 1 d . . . H23 H 0.6751 0.3250 0.0882 0.049 Uiso 1 1 calc R . . C24 C 0.0713(4) 0.0678(4) 0.4483(3) 0.0299(9) Uani 1 1 d . . . C25 C 0.0084(4) 0.1278(4) 0.5113(3) 0.0339(9) Uani 1 1 d . . . H25 H 0.0130 0.2162 0.5201 0.041 Uiso 1 1 calc R . . C26 C 0.0609(4) -0.0620(4) 0.4382(3) 0.0334(9) Uani 1 1 d . . . H26 H 0.1022 -0.1066 0.3958 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.95880(13) 0.68766(13) -0.05256(9) 0.0507(3) Uani 1 1 d . . . C27 C 0.9195(6) 0.0770(6) 0.1633(4) 0.0588(15) Uani 1 1 d . . . H27A H 0.9625 0.1454 0.1394 0.071 Uiso 1 1 calc R . . H27B H 0.9740 0.0680 0.2187 0.071 Uiso 1 1 calc R . . Cl2 Cl 0.91523(16) -0.06276(15) 0.09298(11) 0.0652(4) Uani 1 1 d . . . Cl3 Cl 0.75951(18) 0.11700(17) 0.18076(13) 0.0740(5) Uani 1 1 d . . . C28 C 0.7098(6) -0.0521(6) 0.3638(4) 0.0644(16) Uani 1 1 d . . . H28A H 0.7366 -0.0768 0.4211 0.077 Uiso 1 1 calc R . . H28B H 0.7809 0.0064 0.3531 0.077 Uiso 1 1 calc R . . Cl4 Cl 0.56457(17) 0.02203(16) 0.36197(13) 0.0747(5) Uani 1 1 d . . . Cl5 Cl 0.6924(3) -0.1834(2) 0.28769(13) 0.0988(8) Uani 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 Fe1 0.0295(3) 0.0317(3) 0.0263(3) 0.0079(2) 0.0100(2) 0.0004(2) O1 0.0318(16) 0.0447(19) 0.0346(17) 0.0095(14) 0.0139(13) -0.0042(13) O2 0.0386(17) 0.0392(17) 0.0300(16) 0.0101(13) 0.0170(13) -0.0032(13) O3 0.0418(18) 0.0327(16) 0.0374(17) 0.0142(13) 0.0198(14) -0.0011(13) O4 0.0284(15) 0.0386(17) 0.0355(16) 0.0167(14) 0.0123(12) -0.0031(12) O5 0.0385(17) 0.0352(17) 0.0331(16) 0.0095(13) 0.0189(13) -0.0003(13) O6 0.0327(16) 0.0457(18) 0.0293(16) 0.0112(14) 0.0100(12) -0.0026(13) N1 0.039(2) 0.037(2) 0.0275(19) 0.0084(15) 0.0158(15) -0.0018(16) N2 0.0337(19) 0.035(2) 0.0293(18) 0.0109(15) 0.0114(14) 0.0015(15) N3 0.035(2) 0.037(2) 0.0321(19) 0.0087(16) 0.0157(15) -0.0018(16) N4 0.0325(19) 0.0318(19) 0.0278(18) 0.0121(15) 0.0073(14) -0.0010(14) N5 0.0302(18) 0.039(2) 0.0276(18) 0.0113(15) 0.0117(14) -0.0009(15) N6 0.032(2) 0.035(2) 0.0334(19) 0.0111(16) 0.0115(15) 0.0015(15) N7 0.037(2) 0.048(2) 0.033(2) 0.0166(18) 0.0125(16) -0.0066(17) B1 0.029(2) 0.035(3) 0.036(3) 0.009(2) 0.0130(19) -0.0006(19) B2 0.034(3) 0.031(2) 0.024(2) 0.0061(19) 0.0083(18) 0.0028(19) C1 0.029(2) 0.035(2) 0.033(2) 0.0056(18) 0.0081(17) 0.0006(17) C2 0.031(2) 0.050(3) 0.040(3) 0.005(2) 0.0097(19) 0.000(2) C3 0.036(3) 0.061(3) 0.040(3) 0.004(2) -0.002(2) 0.000(2) C4 0.043(3) 0.059(3) 0.040(3) 0.009(2) -0.001(2) 0.002(2) C5 0.042(3) 0.052(3) 0.033(2) 0.013(2) 0.0054(19) 0.002(2) C6 0.034(2) 0.035(2) 0.029(2) 0.0062(18) 0.0077(17) 0.0033(18) C7 0.036(2) 0.037(2) 0.026(2) 0.0063(18) 0.0103(17) 0.0013(18) C8 0.048(3) 0.039(3) 0.031(2) 0.0050(19) 0.018(2) -0.005(2) C9 0.072(4) 0.037(3) 0.049(3) 0.001(2) 0.031(3) -0.001(2) C10 0.067(4) 0.036(3) 0.049(3) -0.002(2) 0.027(3) -0.004(2) C11 0.043(3) 0.032(2) 0.037(2) 0.0079(19) 0.0145(19) -0.0013(19) C12 0.035(2) 0.033(2) 0.028(2) 0.0057(17) 0.0111(17) 0.0038(17) C13 0.030(2) 0.029(2) 0.028(2) 0.0036(17) 0.0084(16) 0.0030(16) C14 0.044(3) 0.034(2) 0.034(2) 0.0120(19) 0.0105(19) 0.0020(19) C15A 0.033(6) 0.033(6) 0.047(8) 0.012(6) 0.002(5) 0.006(5) C16A 0.040(7) 0.034(7) 0.052(9) 0.004(6) 0.009(6) 0.001(5) C15B 0.040(7) 0.043(7) 0.059(10) 0.023(7) -0.001(6) 0.002(5) C16B 0.047(8) 0.038(7) 0.068(11) 0.008(7) 0.031(7) 0.013(6) C17 0.034(2) 0.036(2) 0.041(3) 0.010(2) 0.0144(19) 0.0029(18) C18 0.031(2) 0.030(2) 0.027(2) 0.0018(17) 0.0082(16) -0.0035(17) C19 0.031(2) 0.039(2) 0.029(2) 0.0051(18) 0.0043(17) -0.0054(18) C20 0.034(2) 0.038(2) 0.047(3) 0.010(2) 0.019(2) 0.0038(19) C21 0.052(3) 0.040(3) 0.046(3) 0.016(2) 0.023(2) -0.001(2) C22 0.042(3) 0.044(3) 0.040(3) 0.005(2) 0.017(2) 0.000(2) C23 0.044(3) 0.042(3) 0.041(3) 0.010(2) 0.017(2) 0.002(2) C24 0.027(2) 0.036(2) 0.028(2) 0.0091(18) 0.0070(16) 0.0009(17) C25 0.039(2) 0.031(2) 0.035(2) 0.0066(18) 0.0150(19) 0.0014(18) C26 0.039(2) 0.034(2) 0.032(2) 0.0072(18) 0.0190(18) 0.0042(18) Cl1 0.0492(7) 0.0543(8) 0.0522(8) 0.0076(6) 0.0225(6) -0.0064(6) C27 0.053(3) 0.059(4) 0.061(4) 0.007(3) 0.002(3) -0.007(3) Cl2 0.0650(10) 0.0604(9) 0.0650(10) 0.0030(7) 0.0000(7) 0.0017(7) Cl3 0.0639(10) 0.0726(11) 0.0875(12) 0.0167(9) 0.0116(8) 0.0108(8) C28 0.056(4) 0.075(4) 0.059(4) 0.005(3) 0.002(3) 0.011(3) Cl4 0.0628(10) 0.0625(10) 0.0935(13) -0.0005(9) -0.0010(9) 0.0244(8) Cl5 0.146(2) 0.0826(13) 0.0668(11) -0.0067(10) 0.0101(12) 0.0550(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 1.900(4) . ? Fe1 N4 1.910(4) . ? Fe1 N1 1.911(4) . ? Fe1 N3 1.913(4) . ? Fe1 N6 1.915(4) . ? Fe1 N2 1.919(4) . ? O1 N1 1.372(4) . ? O1 B1 1.493(6) . ? O2 N2 1.377(4) . ? O2 B1 1.493(6) . ? O3 N3 1.392(4) . ? O3 B1 1.489(6) . ? O4 N4 1.380(4) . ? O4 B2 1.494(6) . ? O5 N5 1.366(4) . ? O5 B2 1.490(6) . ? O6 N6 1.379(4) . ? O6 B2 1.499(6) . ? N1 C1 1.307(6) . ? N2 C7 1.305(6) . ? N3 C13 1.292(6) . ? N4 C18 1.297(5) . ? N5 C12 1.305(6) . ? N6 C6 1.304(6) . ? N7 C22 1.324(6) . ? N7 C21 1.325(6) . ? N7 H7 0.8800 . ? B1 C19 1.605(6) . ? B2 C24 1.591(6) . ? C1 C6 1.437(6) . ? C1 C2 1.500(6) . ? C2 C3 1.511(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.527(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.500(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C12 1.434(6) . ? C7 C8 1.487(6) . ? C8 C9 1.533(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.480(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.531(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.494(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C18 1.453(6) . ? C13 C14 1.494(6) . ? C14 C15B 1.501(13) . ? C14 C15A 1.575(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15A C16A 1.53(2) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17 1.518(14) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C15B C16B 1.47(3) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17 1.532(14) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17 C18 1.487(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 H17C 0.9900 . ? C17 H17D 0.9900 . ? C19 C20 1.387(6) . ? C19 C23 1.416(6) . ? C20 C21 1.380(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.377(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.392(6) . ? C24 C26 1.395(6) . ? C25 C26 1.392(6) 2_556 ? C25 H25 0.9500 . ? C26 C25 1.391(6) 2_556 ? C26 H26 0.9500 . ? C27 Cl2 1.768(6) . ? C27 Cl3 1.771(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 Cl4 1.725(6) . ? C28 Cl5 1.738(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 N5 Fe1 N4 86.21(15) . . ? N5 Fe1 N1 118.74(16) . . ? N4 Fe1 N1 148.79(16) . . ? N5 Fe1 N3 149.14(16) . . ? N4 Fe1 N3 78.39(15) . . ? N1 Fe1 N3 86.09(16) . . ? N5 Fe1 N6 85.63(15) . . ? N4 Fe1 N6 85.64(15) . . ? N1 Fe1 N6 78.51(15) . . ? N3 Fe1 N6 119.18(16) . . ? N5 Fe1 N2 78.18(15) . . ? N4 Fe1 N2 119.82(16) . . ? N1 Fe1 N2 85.59(15) . . ? N3 Fe1 N2 86.49(15) . . ? N6 Fe1 N2 148.27(16) . . ? N1 O1 B1 110.8(3) . . ? N2 O2 B1 110.7(3) . . ? N3 O3 B1 111.1(3) . . ? N4 O4 B2 112.3(3) . . ? N5 O5 B2 112.3(3) . . ? N6 O6 B2 111.7(3) . . ? C1 N1 O1 116.4(4) . . ? C1 N1 Fe1 118.8(3) . . ? O1 N1 Fe1 124.2(3) . . ? C7 N2 O2 116.3(3) . . ? C7 N2 Fe1 118.5(3) . . ? O2 N2 Fe1 123.9(3) . . ? C13 N3 O3 116.8(4) . . ? C13 N3 Fe1 119.1(3) . . ? O3 N3 Fe1 123.4(3) . . ? C18 N4 O4 116.6(3) . . ? C18 N4 Fe1 118.7(3) . . ? O4 N4 Fe1 123.7(2) . . ? C12 N5 O5 115.9(4) . . ? C12 N5 Fe1 119.2(3) . . ? O5 N5 Fe1 124.4(3) . . ? C6 N6 O6 116.7(4) . . ? C6 N6 Fe1 118.2(3) . . ? O6 N6 Fe1 123.9(3) . . ? C22 N7 C21 121.3(4) . . ? C22 N7 H7 119.4 . . ? C21 N7 H7 119.4 . . ? O3 B1 O1 111.5(4) . . ? O3 B1 O2 111.4(4) . . ? O1 B1 O2 110.7(4) . . ? O3 B1 C19 108.9(4) . . ? O1 B1 C19 107.3(3) . . ? O2 B1 C19 106.8(4) . . ? O5 B2 O4 110.7(3) . . ? O5 B2 O6 110.1(4) . . ? O4 B2 O6 109.2(4) . . ? O5 B2 C24 107.6(3) . . ? O4 B2 C24 109.7(3) . . ? O6 B2 C24 109.6(3) . . ? N1 C1 C6 111.6(4) . . ? N1 C1 C2 125.6(4) . . ? C6 C1 C2 122.8(4) . . ? C1 C2 C3 111.3(4) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 111.5(4) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 112.8(4) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 109.5(4) . . ? C6 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? N6 C6 C1 112.4(4) . . ? N6 C6 C5 124.9(4) . . ? C1 C6 C5 122.7(4) . . ? N2 C7 C12 111.6(4) . . ? N2 C7 C8 126.2(4) . . ? C12 C7 C8 122.1(4) . . ? C7 C8 C9 110.2(4) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 112.3(5) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 112.4(4) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 110.8(4) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N5 C12 C7 112.0(4) . . ? N5 C12 C11 124.7(4) . . ? C7 C12 C11 123.2(4) . . ? N3 C13 C18 111.5(4) . . ? N3 C13 C14 126.7(4) . . ? C18 C13 C14 121.7(4) . . ? C13 C14 C15B 112.4(5) . . ? C13 C14 C15A 109.1(5) . . ? C13 C14 H14A 109.9 . . ? C15B C14 H14A 82.7 . . ? C15A C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? C15B C14 H14B 129.1 . . ? C15A C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C13 C14 H14C 109.1 . . ? C15B C14 H14C 109.1 . . ? C15A C14 H14C 132.6 . . ? H14B C14 H14C 81.8 . . ? C13 C14 H14D 109.1 . . ? C15B C14 H14D 109.1 . . ? C15A C14 H14D 84.6 . . ? H14A C14 H14D 130.3 . . ? H14C C14 H14D 107.9 . . ? C16A C15A C14 109.1(14) . . ? C16A C15A H15A 109.9 . . ? C14 C15A H15A 109.9 . . ? C16A C15A H15B 109.9 . . ? C14 C15A H15B 109.9 . . ? H15A C15A H15B 108.3 . . ? C17 C16A C15A 111.0(13) . . ? C17 C16A H16A 109.4 . . ? C15A C16A H16A 109.4 . . ? C17 C16A H16B 109.4 . . ? C15A C16A H16B 109.4 . . ? H16A C16A H16B 108.0 . . ? C16B C15B C14 114.2(15) . . ? C16B C15B H15C 108.7 . . ? C14 C15B H15C 108.7 . . ? C16B C15B H15D 108.7 . . ? C14 C15B H15D 108.7 . . ? H15C C15B H15D 107.6 . . ? C15B C16B C17 112.9(15) . . ? C15B C16B H16C 109.0 . . ? C17 C16B H16C 109.0 . . ? C15B C16B H16D 109.0 . . ? C17 C16B H16D 109.0 . . ? H16C C16B H16D 107.8 . . ? C18 C17 C16A 112.5(6) . . ? C18 C17 C16B 110.4(6) . . ? C18 C17 H17A 109.1 . . ? C16A C17 H17A 109.1 . . ? C16B C17 H17A 84.6 . . ? C18 C17 H17B 109.1 . . ? C16A C17 H17B 109.1 . . ? C16B C17 H17B 131.4 . . ? H17A C17 H17B 107.8 . . ? C18 C17 H17C 109.6 . . ? C16A C17 H17C 129.1 . . ? C16B C17 H17C 109.6 . . ? H17B C17 H17C 82.0 . . ? C18 C17 H17D 109.6 . . ? C16A C17 H17D 83.4 . . ? C16B C17 H17D 109.6 . . ? H17A C17 H17D 130.2 . . ? H17C C17 H17D 108.1 . . ? N4 C18 C13 111.9(4) . . ? N4 C18 C17 125.9(4) . . ? C13 C18 C17 122.2(4) . . ? C20 C19 C23 116.1(4) . . ? C20 C19 B1 123.8(4) . . ? C23 C19 B1 120.1(4) . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N7 C21 C20 121.0(5) . . ? N7 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? N7 C22 C23 120.6(5) . . ? N7 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C19 120.4(5) . . ? C22 C23 H23 119.8 . . ? C19 C23 H23 119.8 . . ? C25 C24 C26 116.6(4) . . ? C25 C24 B2 121.9(4) . . ? C26 C24 B2 121.5(4) . . ? C26 C25 C24 121.8(4) 2_556 . ? C26 C25 H25 119.1 2_556 . ? C24 C25 H25 119.1 . . ? C25 C26 C24 121.6(4) 2_556 . ? C25 C26 H26 119.2 2_556 . ? C24 C26 H26 119.2 . . ? Cl2 C27 Cl3 112.6(3) . . ? Cl2 C27 H27A 109.1 . . ? Cl3 C27 H27A 109.1 . . ? Cl2 C27 H27B 109.1 . . ? Cl3 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? Cl4 C28 Cl5 111.9(4) . . ? Cl4 C28 H28A 109.2 . . ? Cl5 C28 H28A 109.2 . . ? Cl4 C28 H28B 109.2 . . ? Cl5 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? 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 B1 O1 N1 C1 -158.6(4) . . . . ? B1 O1 N1 Fe1 12.9(5) . . . . ? N5 Fe1 N1 C1 -78.9(4) . . . . ? N4 Fe1 N1 C1 60.5(5) . . . . ? N3 Fe1 N1 C1 120.3(4) . . . . ? N6 Fe1 N1 C1 -0.5(3) . . . . ? N2 Fe1 N1 C1 -152.9(4) . . . . ? N5 Fe1 N1 O1 109.7(3) . . . . ? N4 Fe1 N1 O1 -110.9(4) . . . . ? N3 Fe1 N1 O1 -51.0(3) . . . . ? N6 Fe1 N1 O1 -171.8(4) . . . . ? N2 Fe1 N1 O1 35.8(3) . . . . ? B1 O2 N2 C7 -154.3(4) . . . . ? B1 O2 N2 Fe1 12.7(4) . . . . ? N5 Fe1 N2 C7 -4.6(3) . . . . ? N4 Fe1 N2 C7 -83.2(4) . . . . ? N1 Fe1 N2 C7 116.0(4) . . . . ? N3 Fe1 N2 C7 -157.7(4) . . . . ? N6 Fe1 N2 C7 56.3(5) . . . . ? N5 Fe1 N2 O2 -171.4(3) . . . . ? N4 Fe1 N2 O2 110.0(3) . . . . ? N1 Fe1 N2 O2 -50.8(3) . . . . ? N3 Fe1 N2 O2 35.6(3) . . . . ? N6 Fe1 N2 O2 -110.5(4) . . . . ? B1 O3 N3 C13 -158.2(4) . . . . ? B1 O3 N3 Fe1 11.6(5) . . . . ? N5 Fe1 N3 C13 60.3(5) . . . . ? N4 Fe1 N3 C13 -1.3(3) . . . . ? N1 Fe1 N3 C13 -154.1(4) . . . . ? N6 Fe1 N3 C13 -79.6(4) . . . . ? N2 Fe1 N3 C13 120.1(4) . . . . ? N5 Fe1 N3 O3 -109.4(4) . . . . ? N4 Fe1 N3 O3 -171.0(3) . . . . ? N1 Fe1 N3 O3 36.3(3) . . . . ? N6 Fe1 N3 O3 110.8(3) . . . . ? N2 Fe1 N3 O3 -49.5(3) . . . . ? B2 O4 N4 C18 -156.3(4) . . . . ? B2 O4 N4 Fe1 11.9(4) . . . . ? N5 Fe1 N4 C18 -156.5(3) . . . . ? N1 Fe1 N4 C18 58.4(5) . . . . ? N3 Fe1 N4 C18 -3.4(3) . . . . ? N6 Fe1 N4 C18 117.6(3) . . . . ? N2 Fe1 N4 C18 -82.4(4) . . . . ? N5 Fe1 N4 O4 35.6(3) . . . . ? N1 Fe1 N4 O4 -109.6(4) . . . . ? N3 Fe1 N4 O4 -171.3(3) . . . . ? N6 Fe1 N4 O4 -50.3(3) . . . . ? N2 Fe1 N4 O4 109.7(3) . . . . ? B2 O5 N5 C12 -159.0(4) . . . . ? B2 O5 N5 Fe1 12.6(5) . . . . ? N4 Fe1 N5 C12 121.3(3) . . . . ? N1 Fe1 N5 C12 -78.4(4) . . . . ? N3 Fe1 N5 C12 61.6(5) . . . . ? N6 Fe1 N5 C12 -152.8(3) . . . . ? N2 Fe1 N5 C12 -0.2(3) . . . . ? N4 Fe1 N5 O5 -50.0(3) . . . . ? N1 Fe1 N5 O5 110.2(3) . . . . ? N3 Fe1 N5 O5 -109.7(4) . . . . ? N6 Fe1 N5 O5 35.9(3) . . . . ? N2 Fe1 N5 O5 -171.5(3) . . . . ? B2 O6 N6 C6 -154.3(4) . . . . ? B2 O6 N6 Fe1 13.0(5) . . . . ? N5 Fe1 N6 C6 116.7(3) . . . . ? N4 Fe1 N6 C6 -156.8(3) . . . . ? N1 Fe1 N6 C6 -3.8(3) . . . . ? N3 Fe1 N6 C6 -82.7(4) . . . . ? N2 Fe1 N6 C6 57.6(5) . . . . ? N5 Fe1 N6 O6 -50.5(3) . . . . ? N4 Fe1 N6 O6 36.0(3) . . . . ? N1 Fe1 N6 O6 -171.0(3) . . . . ? N3 Fe1 N6 O6 110.1(3) . . . . ? N2 Fe1 N6 O6 -109.6(4) . . . . ? N3 O3 B1 O1 -68.3(4) . . . . ? N3 O3 B1 O2 55.9(5) . . . . ? N3 O3 B1 C19 173.4(3) . . . . ? N1 O1 B1 O3 54.9(4) . . . . ? N1 O1 B1 O2 -69.7(4) . . . . ? N1 O1 B1 C19 174.2(3) . . . . ? N2 O2 B1 O3 -69.4(4) . . . . ? N2 O2 B1 O1 55.3(4) . . . . ? N2 O2 B1 C19 171.8(3) . . . . ? N5 O5 B2 O4 53.2(4) . . . . ? N5 O5 B2 O6 -67.6(4) . . . . ? N5 O5 B2 C24 173.1(3) . . . . ? N4 O4 B2 O5 -66.4(4) . . . . ? N4 O4 B2 O6 55.0(4) . . . . ? N4 O4 B2 C24 175.1(3) . . . . ? N6 O6 B2 O5 53.2(4) . . . . ? N6 O6 B2 O4 -68.6(4) . . . . ? N6 O6 B2 C24 171.3(3) . . . . ? O1 N1 C1 C6 176.2(4) . . . . ? Fe1 N1 C1 C6 4.1(5) . . . . ? O1 N1 C1 C2 -5.5(7) . . . . ? Fe1 N1 C1 C2 -177.5(4) . . . . ? N1 C1 C2 C3 172.7(5) . . . . ? C6 C1 C2 C3 -9.1(7) . . . . ? C1 C2 C3 C4 43.1(6) . . . . ? C2 C3 C4 C5 -65.2(6) . . . . ? C3 C4 C5 C6 46.7(6) . . . . ? O6 N6 C6 C1 175.1(4) . . . . ? Fe1 N6 C6 C1 7.0(5) . . . . ? O6 N6 C6 C5 -3.5(6) . . . . ? Fe1 N6 C6 C5 -171.6(4) . . . . ? N1 C1 C6 N6 -6.9(6) . . . . ? C2 C1 C6 N6 174.7(4) . . . . ? N1 C1 C6 C5 171.6(4) . . . . ? C2 C1 C6 C5 -6.8(7) . . . . ? C4 C5 C6 N6 166.4(4) . . . . ? C4 C5 C6 C1 -12.0(7) . . . . ? O2 N2 C7 C12 175.7(3) . . . . ? Fe1 N2 C7 C12 8.0(5) . . . . ? O2 N2 C7 C8 -1.3(7) . . . . ? Fe1 N2 C7 C8 -169.1(4) . . . . ? N2 C7 C8 C9 163.6(5) . . . . ? C12 C7 C8 C9 -13.2(6) . . . . ? C7 C8 C9 C10 47.6(6) . . . . ? C8 C9 C10 C11 -64.5(6) . . . . ? C9 C10 C11 C12 41.9(6) . . . . ? O5 N5 C12 C7 176.4(3) . . . . ? Fe1 N5 C12 C7 4.4(5) . . . . ? O5 N5 C12 C11 -7.8(6) . . . . ? Fe1 N5 C12 C11 -179.8(3) . . . . ? N2 C7 C12 N5 -7.7(6) . . . . ? C8 C7 C12 N5 169.5(4) . . . . ? N2 C7 C12 C11 176.4(4) . . . . ? C8 C7 C12 C11 -6.4(7) . . . . ? C10 C11 C12 N5 177.0(4) . . . . ? C10 C11 C12 C7 -7.6(6) . . . . ? O3 N3 C13 C18 175.4(3) . . . . ? Fe1 N3 C13 C18 5.1(5) . . . . ? O3 N3 C13 C14 -3.8(6) . . . . ? Fe1 N3 C13 C14 -174.1(3) . . . . ? N3 C13 C14 C15B 176.1(11) . . . . ? C18 C13 C14 C15B -3.0(12) . . . . ? N3 C13 C14 C15A -153.6(9) . . . . ? C18 C13 C14 C15A 27.3(10) . . . . ? C13 C14 C15A C16A -54.2(16) . . . . ? C15B C14 C15A C16A 47.6(17) . . . . ? C14 C15A C16A C17 66(2) . . . . ? C13 C14 C15B C16B 38(2) . . . . ? C15A C14 C15B C16B -51(2) . . . . ? C14 C15B C16B C17 -62(3) . . . . ? C15A C16A C17 C18 -46.3(18) . . . . ? C15A C16A C17 C16B 45.0(17) . . . . ? C15B C16B C17 C18 46(2) . . . . ? C15B C16B C17 C16A -54(2) . . . . ? O4 N4 C18 C13 175.6(3) . . . . ? Fe1 N4 C18 C13 6.8(5) . . . . ? O4 N4 C18 C17 -2.8(6) . . . . ? Fe1 N4 C18 C17 -171.6(3) . . . . ? N3 C13 C18 N4 -7.4(5) . . . . ? C14 C13 C18 N4 171.8(4) . . . . ? N3 C13 C18 C17 171.0(4) . . . . ? C14 C13 C18 C17 -9.7(6) . . . . ? C16A C17 C18 N4 -163.5(9) . . . . ? C16B C17 C18 N4 166.6(11) . . . . ? C16A C17 C18 C13 18.3(10) . . . . ? C16B C17 C18 C13 -11.6(12) . . . . ? O3 B1 C19 C20 11.9(6) . . . . ? O1 B1 C19 C20 -109.0(5) . . . . ? O2 B1 C19 C20 132.3(5) . . . . ? O3 B1 C19 C23 -170.8(4) . . . . ? O1 B1 C19 C23 68.3(5) . . . . ? O2 B1 C19 C23 -50.4(5) . . . . ? C23 C19 C20 C21 -1.0(7) . . . . ? B1 C19 C20 C21 176.4(5) . . . . ? C22 N7 C21 C20 -1.6(8) . . . . ? C19 C20 C21 N7 1.8(8) . . . . ? C21 N7 C22 C23 0.6(8) . . . . ? N7 C22 C23 C19 0.2(8) . . . . ? C20 C19 C23 C22 0.0(7) . . . . ? B1 C19 C23 C22 -177.5(4) . . . . ? O5 B2 C24 C25 178.3(4) . . . . ? O4 B2 C24 C25 -61.2(5) . . . . ? O6 B2 C24 C25 58.6(5) . . . . ? O5 B2 C24 C26 1.5(6) . . . . ? O4 B2 C24 C26 122.0(4) . . . . ? O6 B2 C24 C26 -118.2(4) . . . . ? C26 C24 C25 C26 0.2(7) . . . 2_556 ? B2 C24 C25 C26 -176.8(4) . . . 2_556 ? C25 C24 C26 C25 -0.2(7) . . . 2_556 ? B2 C24 C26 C25 176.8(4) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.539 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.095 _iucr_refine_instructions_details ; TITL MDW1-86F3 in P-1 CELL 0.71073 10.2350 10.8620 16.0080 97.163 98.930 93.017 ZERR 1.00 0.0050 0.0040 0.0060 0.018 0.022 0.023 LATT 1 SFAC C H B N O CL FE UNIT 56 70 4 14 12 10 2 REM ------------------------------------------------------------------------- REM Data measured on the marmux REM Crystal colour: red; Crystal habit: prismatic REM ------------------------------------------------------------------------- L.S. 10 OMIT -2 1 0 OMIT 4 0 1 OMIT 0 2 5 OMIT -5 3 2 ACTA 50 CONF BOND $H WPDB -2 SIZE 0.32 0.25 0.20 FMAP 2 PLAN 10 TEMP -133 WGHT 0.090300 1.414200 FVAR 0.56561 0.49059 MOLE 1 FE1 7 0.320986 0.278290 0.287067 11.00000 0.02950 0.03175 = 0.02627 0.00791 0.00997 0.00037 O1 5 0.575217 0.383742 0.258369 11.00000 0.03183 0.04472 = 0.03464 0.00953 0.01393 -0.00418 O2 5 0.424739 0.291776 0.128204 11.00000 0.03858 0.03924 = 0.03004 0.01009 0.01703 -0.00322 O3 5 0.381871 0.493633 0.203692 11.00000 0.04176 0.03269 = 0.03743 0.01420 0.01983 -0.00110 O4 5 0.070495 0.224977 0.344857 11.00000 0.02842 0.03858 = 0.03549 0.01673 0.01231 -0.00315 O5 5 0.212289 0.050078 0.334774 11.00000 0.03848 0.03520 = 0.03314 0.00946 0.01885 -0.00034 O6 5 0.266830 0.221340 0.452336 11.00000 0.03271 0.04571 = 0.02927 0.01125 0.01003 -0.00261 N1 4 0.503911 0.336707 0.314548 11.00000 0.03950 0.03657 = 0.02755 0.00843 0.01577 -0.00178 N2 4 0.360398 0.219417 0.176281 11.00000 0.03365 0.03455 = 0.02934 0.01090 0.01144 0.00149 N3 4 0.292469 0.433809 0.245256 11.00000 0.03475 0.03715 = 0.03213 0.00871 0.01566 -0.00177 N4 4 0.141531 0.300039 0.301677 11.00000 0.03247 0.03182 = 0.02775 0.01212 0.00726 -0.00100 N5 4 0.275235 0.104765 0.278105 11.00000 0.03017 0.03934 = 0.02763 0.01129 0.01175 -0.00095 N6 4 0.354894 0.274282 0.407739 11.00000 0.03208 0.03468 = 0.03342 0.01115 0.01150 0.00153 N7 4 0.741242 0.588911 0.029439 11.00000 0.03693 0.04836 = 0.03300 0.01655 0.01246 -0.00662 AFIX 43 H7 2 0.793154 0.624616 -0.000921 11.00000 -1.20000 AFIX 0 B1 3 0.485304 0.410059 0.180883 11.00000 0.02858 0.03523 = 0.03600 0.00917 0.01303 -0.00063 B2 3 0.156705 0.142799 0.393806 11.00000 0.03419 0.03114 = 0.02429 0.00609 0.00829 0.00279 C1 1 0.562329 0.347228 0.393997 11.00000 0.02911 0.03464 = 0.03304 0.00556 0.00806 0.00061 C2 1 0.703178 0.395967 0.426810 11.00000 0.03103 0.04969 = 0.04011 0.00482 0.00975 0.00019 AFIX 23 H2A 2 0.719475 0.477526 0.407279 11.00000 -1.20000 H2B 2 0.763770 0.337930 0.403141 11.00000 -1.20000 AFIX 0 C3 1 0.732474 0.410621 0.523155 11.00000 0.03638 0.06125 = 0.04013 0.00401 -0.00205 -0.00048 AFIX 23 H3A 2 0.695292 0.487317 0.546664 11.00000 -1.20000 H3B 2 0.829682 0.419472 0.542107 11.00000 -1.20000 AFIX 0 C4 1 0.674032 0.300196 0.557550 11.00000 0.04288 0.05876 = 0.03998 0.00950 -0.00102 0.00243 AFIX 23 H4A 2 0.703978 0.308676 0.619978 11.00000 -1.20000 H4B 2 0.707914 0.223264 0.531572 11.00000 -1.20000 AFIX 0 C5 1 0.522634 0.287920 0.539465 11.00000 0.04151 0.05184 = 0.03337 0.01288 0.00541 0.00214 AFIX 23 H5A 2 0.489792 0.205395 0.551060 11.00000 -1.20000 H5B 2 0.487269 0.352584 0.577310 11.00000 -1.20000 AFIX 0 C6 1 0.475692 0.302507 0.447951 11.00000 0.03426 0.03525 = 0.02942 0.00620 0.00767 0.00332 C7 1 0.348700 0.099798 0.151012 11.00000 0.03629 0.03702 = 0.02585 0.00631 0.01029 0.00132 C8 1 0.395693 0.035517 0.074805 11.00000 0.04757 0.03867 = 0.03085 0.00500 0.01804 -0.00487 AFIX 23 H8A 2 0.485127 0.071648 0.071121 11.00000 -1.20000 H8B 2 0.334979 0.047915 0.022527 11.00000 -1.20000 AFIX 0 C9 1 0.400783 -0.103998 0.080722 11.00000 0.07151 0.03686 = 0.04853 0.00093 0.03060 -0.00146 AFIX 23 H9A 2 0.414625 -0.147726 0.025069 11.00000 -1.20000 H9B 2 0.477253 -0.116941 0.124013 11.00000 -1.20000 AFIX 0 C10 1 0.277939 -0.158517 0.103920 11.00000 0.06655 0.03590 = 0.04896 -0.00229 0.02678 -0.00364 AFIX 23 H10A 2 0.282413 -0.249727 0.101173 11.00000 -1.20000 H10B 2 0.201106 -0.142734 0.061839 11.00000 -1.20000 AFIX 0 C11 1 0.256608 -0.104668 0.193453 11.00000 0.04270 0.03191 = 0.03706 0.00787 0.01446 -0.00128 AFIX 23 H11A 2 0.163066 -0.122995 0.199613 11.00000 -1.20000 H11B 2 0.313606 -0.144545 0.236551 11.00000 -1.20000 AFIX 0 C12 1 0.289136 0.032823 0.208899 11.00000 0.03484 0.03347 = 0.02752 0.00570 0.01112 0.00384 C13 1 0.177495 0.477891 0.243868 11.00000 0.03024 0.02891 = 0.02783 0.00360 0.00843 0.00296 C14 1 0.132989 0.591048 0.206573 11.00000 0.04352 0.03434 = 0.03421 0.01197 0.01054 0.00198 PART 1 AFIX 23 H14A 2 0.098656 0.568933 0.144901 21.00000 -1.20000 H14B 2 0.208807 0.653904 0.213223 21.00000 -1.20000 AFIX 23 PART 2 H14C 2 0.146160 0.583121 0.146214 -21.00000 -1.20000 H14D 2 0.188458 0.664987 0.237713 -21.00000 -1.20000 AFIX 0 PART 1 C15A 1 0.020780 0.646201 0.253863 21.00000 0.03294 0.03299 = 0.04716 0.01213 0.00230 0.00606 AFIX 23 H15A 2 0.057863 0.677641 0.314064 21.00000 -1.20000 H15B 2 -0.015407 0.716474 0.226132 21.00000 -1.20000 AFIX 0 C16A 1 -0.089888 0.543813 0.250092 21.00000 0.04049 0.03444 = 0.05233 0.00431 0.00928 0.00063 AFIX 23 H16A 2 -0.165618 0.580287 0.273253 21.00000 -1.20000 H16B 2 -0.121297 0.507872 0.189933 21.00000 -1.20000 AFIX 0 PART 2 C15B 1 -0.010113 0.610128 0.210982 -21.00000 0.03966 0.04278 = 0.05859 0.02312 -0.00075 0.00170 AFIX 23 H15C 2 -0.025543 0.698305 0.205930 -21.00000 -1.20000 H15D 2 -0.065740 0.558517 0.161569 -21.00000 -1.20000 AFIX 0 C16B 1 -0.053233 0.578817 0.289809 -21.00000 0.04709 0.03840 = 0.06794 0.00781 0.03119 0.01325 AFIX 23 H16C 2 -0.146803 0.598274 0.288984 -21.00000 -1.20000 H16D 2 0.000978 0.631365 0.339367 -21.00000 -1.20000 AFIX 0 PART 0 C17 1 -0.040958 0.441684 0.301083 11.00000 0.03437 0.03593 = 0.04137 0.00955 0.01443 0.00293 PART 1 AFIX 23 H17A 2 -0.033624 0.471879 0.362708 21.00000 -1.20000 H17B 2 -0.106821 0.369042 0.287313 21.00000 -1.20000 AFIX 23 PART 2 H17C 2 -0.050550 0.429735 0.360197 -21.00000 -1.20000 H17D 2 -0.112815 0.389789 0.261685 -21.00000 -1.20000 AFIX 0 PART 0 C18 1 0.089877 0.401773 0.283242 11.00000 0.03090 0.03010 = 0.02685 0.00185 0.00820 -0.00351 C19 1 0.575007 0.477602 0.123700 11.00000 0.03059 0.03876 = 0.02872 0.00511 0.00435 -0.00536 C20 1 0.571466 0.602303 0.113268 11.00000 0.03433 0.03807 = 0.04717 0.01032 0.01895 0.00381 AFIX 43 H20 2 0.509809 0.651326 0.138262 11.00000 -1.20000 AFIX 0 C21 1 0.656712 0.655843 0.066898 11.00000 0.05217 0.03997 = 0.04620 0.01577 0.02315 -0.00057 AFIX 43 H21 2 0.654732 0.741949 0.061774 11.00000 -1.20000 AFIX 0 C22 1 0.749146 0.469346 0.036786 11.00000 0.04207 0.04433 = 0.03994 0.00456 0.01732 0.00041 AFIX 43 H22 2 0.811156 0.423529 0.009756 11.00000 -1.20000 AFIX 0 C23 1 0.668258 0.410807 0.083272 11.00000 0.04391 0.04243 = 0.04053 0.01041 0.01710 0.00171 AFIX 43 H23 2 0.675098 0.325048 0.088233 11.00000 -1.20000 AFIX 0 C24 1 0.071256 0.067774 0.448333 11.00000 0.02691 0.03631 = 0.02849 0.00915 0.00701 0.00088 C25 1 0.008430 0.127811 0.511308 11.00000 0.03856 0.03104 = 0.03531 0.00656 0.01502 0.00137 AFIX 43 H25 2 0.013005 0.216162 0.520071 11.00000 -1.20000 AFIX 0 C26 1 0.060908 -0.062030 0.438198 11.00000 0.03855 0.03448 = 0.03231 0.00717 0.01902 0.00415 AFIX 43 H26 2 0.102213 -0.106578 0.395787 11.00000 -1.20000 AFIX 0 MOLE 2 CL1 6 0.958799 0.687657 -0.052560 11.00000 0.04919 0.05431 = 0.05224 0.00759 0.02247 -0.00641 MOLE 3 C27 1 0.919523 0.077021 0.163342 11.00000 0.05312 0.05862 = 0.06093 0.00663 0.00235 -0.00652 AFIX 23 H27A 2 0.962548 0.145358 0.139436 11.00000 -1.20000 H27B 2 0.973993 0.068004 0.218715 11.00000 -1.20000 AFIX 0 CL2 6 0.915226 -0.062762 0.092983 11.00000 0.06500 0.06038 = 0.06495 0.00304 -0.00004 0.00168 CL3 6 0.759512 0.117003 0.180757 11.00000 0.06390 0.07261 = 0.08750 0.01673 0.01162 0.01081 MOLE 4 C28 1 0.709776 -0.052134 0.363787 11.00000 0.05597 0.07505 = 0.05948 0.00540 0.00194 0.01065 AFIX 23 H28A 2 0.736568 -0.076797 0.421117 11.00000 -1.20000 H28B 2 0.780893 0.006368 0.353088 11.00000 -1.20000 AFIX 0 CL4 6 0.564567 0.022026 0.361970 11.00000 0.06282 0.06248 = 0.09354 -0.00048 -0.00102 0.02442 CL5 6 0.692433 -0.183396 0.287689 11.00000 0.14552 0.08262 = 0.06679 -0.00668 0.01014 0.05501 MOLE 0 HKLF 4 REM MDW1-86F3 in P-1 REM R1 = 0.0728 for 5047 Fo > 4sig(Fo) and 0.1076 for all 7357 data REM 461 parameters refined using 0 restraints END WGHT 0.0903 1.4139 REM Highest difference peak 0.539, deepest hole -0.578, 1-sigma level 0.095 Q1 1 0.3020 -0.0866 0.0439 11.00000 0.05 0.54 Q2 1 0.8587 -0.0941 0.1367 11.00000 0.05 0.50 Q3 1 0.9867 0.7491 0.0115 11.00000 0.05 0.46 Q4 1 0.4005 0.3543 0.3494 11.00000 0.05 0.45 Q5 1 0.2109 0.3069 0.2342 11.00000 0.05 0.44 Q6 1 0.3525 0.3365 0.3619 11.00000 0.05 0.41 Q7 1 0.1309 0.2810 0.4044 11.00000 0.05 0.40 Q8 1 -0.1465 0.8117 0.1759 11.00000 0.05 0.39 Q9 1 0.2857 0.1679 0.2534 11.00000 0.05 0.39 Q10 1 0.2239 0.2032 0.2399 11.00000 0.05 0.37 ; data_mdw3-81b _database_code_depnum_ccdc_archive 'CCDC 919266' #TrackingRef 'mdw3-81b.cif' _audit_update_record ; 2013-01-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 B2 Fe N8 O14 Zn2' _chemical_formula_sum 'C56 H48 B2 Fe N8 O14 Zn2' _chemical_formula_weight 1265.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.166(4) _cell_length_b 18.520(4) _cell_length_c 21.805(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.600(18) _cell_angle_gamma 90.00 _cell_volume 9399(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 256 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5097 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52494 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.07 _reflns_number_total 10528 _reflns_number_gt 8426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+87.0888P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10528 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2541 _refine_ls_wR_factor_gt 0.2456 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Zn1 Zn 0.67280(3) 0.5000 0.63931(3) 0.01923(19) Uani 1 2 d S . . Zn2 Zn 0.70688(3) 0.5000 0.78142(3) 0.02028(19) Uani 1 2 d S . . Fe1 Fe 0.69260(4) 0.5000 0.21121(4) 0.0288(2) Uani 1 2 d S . . O1 O 0.61331(16) 0.4255(2) 0.64706(18) 0.0444(10) Uani 1 1 d . . . O2 O 0.64275(14) 0.4240(2) 0.75321(16) 0.0338(8) Uani 1 1 d . . . O3 O 0.76535(15) 0.4242(2) 0.77341(18) 0.0417(9) Uani 1 1 d . . . O4 O 0.73667(16) 0.4245(2) 0.66684(19) 0.0444(10) Uani 1 1 d . . . O5A O 0.6975(4) 0.4294(5) 0.3320(3) 0.0332(17) Uani 0.50 1 d P . 1 O6A O 0.7131(4) 0.4252(5) 0.1002(4) 0.0362(17) Uani 0.50 1 d P . 1 O5B O 0.7281(4) 0.4433(4) 0.3410(4) 0.0300(16) Uani 0.50 1 d P . 2 O6B O 0.7445(4) 0.4454(4) 0.1139(4) 0.0357(17) Uani 0.50 1 d P . 2 O7 O 0.6426(3) 0.4761(3) 0.0758(3) 0.0281(15) Uani 0.50 1 d P . . O8 O 0.6257(3) 0.5270(4) 0.3028(3) 0.0319(15) Uani 0.50 1 d P . . N1 N 0.6711(2) 0.5000 0.5446(3) 0.0251(11) Uani 1 2 d S . . N2A N 0.7102(5) 0.4280(12) 0.2724(10) 0.032(3) Uani 0.50 1 d P . 1 N3A N 0.7166(6) 0.4208(7) 0.1672(7) 0.036(3) Uani 0.50 1 d P . 1 N2B N 0.7315(6) 0.4349(10) 0.2800(8) 0.028(3) Uani 0.50 1 d P . 2 N3B N 0.7387(5) 0.4379(6) 0.1755(6) 0.030(3) Uani 0.50 1 d P . 2 N4 N 0.6328(3) 0.4829(4) 0.1352(3) 0.026(2) Uani 0.50 1 d P . . N5 N 0.6250(3) 0.5176(4) 0.2395(3) 0.029(2) Uani 0.50 1 d P . . B1 B 0.6826(3) 0.5000 0.3457(4) 0.0370(19) Uani 1 2 d S . . B2 B 0.7032(4) 0.5000 0.0767(4) 0.0376(19) Uani 1 2 d S . . C1 C 0.60887(19) 0.4064(2) 0.7011(2) 0.0274(9) Uani 1 1 d . . . C2 C 0.5577(2) 0.3615(3) 0.7034(2) 0.0319(10) Uani 1 1 d . . . C3 C 0.5084(3) 0.3619(4) 0.6525(3) 0.0502(15) Uani 1 1 d . . . H3 H 0.5080 0.3887 0.6152 0.060 Uiso 1 1 calc R . . C4 C 0.4600(3) 0.3239(4) 0.6555(3) 0.0501(15) Uani 1 1 d . . . H4 H 0.4260 0.3264 0.6213 0.060 Uiso 1 1 calc R . . C5 C 0.4610(2) 0.2816(3) 0.7095(3) 0.0452(14) Uani 1 1 d . . . C6 C 0.5080(2) 0.2856(4) 0.7610(3) 0.0456(14) Uani 1 1 d . . . H6 H 0.5079 0.2605 0.7989 0.055 Uiso 1 1 calc R . . C7 C 0.5555(2) 0.3254(4) 0.7585(3) 0.0472(15) Uani 1 1 d . . . H7 H 0.5873 0.3282 0.7952 0.057 Uiso 1 1 calc R . . C8 C 0.7693(2) 0.4056(3) 0.7190(3) 0.0317(10) Uani 1 1 d . . . C9 C 0.8185(2) 0.3561(3) 0.7169(3) 0.0342(11) Uani 1 1 d . . . C10 C 0.8542(3) 0.3263(4) 0.7736(3) 0.0590(19) Uani 1 1 d . . . H10 H 0.8477 0.3370 0.8137 0.071 Uiso 1 1 calc R . . C11 C 0.8987(3) 0.2811(5) 0.7695(3) 0.071(2) Uani 1 1 d . . . H11 H 0.9216 0.2598 0.8076 0.086 Uiso 1 1 calc R . . C12 C 0.9117(2) 0.2650(3) 0.7118(3) 0.0423(13) Uani 1 1 d . . . C13 C 0.8740(2) 0.2938(4) 0.6560(3) 0.0467(15) Uani 1 1 d . . . H13 H 0.8805 0.2830 0.6159 0.056 Uiso 1 1 calc R . . C14 C 0.8280(2) 0.3373(3) 0.6581(3) 0.0413(13) Uani 1 1 d . . . H14 H 0.8026 0.3544 0.6197 0.050 Uiso 1 1 calc R . . C15 C 0.7220(3) 0.5000 0.5315(4) 0.064(3) Uani 1 2 d S . . H15 H 0.7562 0.5000 0.5655 0.076 Uiso 1 2 calc SR . . C16 C 0.7259(4) 0.5000 0.4689(4) 0.067(3) Uani 1 2 d S . . H16 H 0.7627 0.5000 0.4610 0.080 Uiso 1 2 calc SR . . C17 C 0.6775(3) 0.5000 0.4183(3) 0.0391(17) Uani 1 2 d S . . C18 C 0.6255(4) 0.5000 0.4335(4) 0.061(3) Uani 1 2 d S . . H18 H 0.5906 0.5000 0.4006 0.073 Uiso 1 2 calc SR . . C19 C 0.6241(4) 0.5000 0.4971(4) 0.050(2) Uani 1 2 d S . . H19 H 0.5879 0.5000 0.5064 0.061 Uiso 1 2 calc SR . . C20 C 0.7485(2) 0.3741(3) 0.2658(3) 0.0366(11) Uani 1 1 d . . . C21 C 0.7740(3) 0.3152(3) 0.3119(3) 0.0539(16) Uani 1 1 d . . . H21A H 0.7426 0.2860 0.3204 0.065 Uiso 1 1 calc R . . H21B H 0.7957 0.3373 0.3527 0.065 Uiso 1 1 calc R . . C22 C 0.8136(3) 0.2662(4) 0.2884(4) 0.069(2) Uani 1 1 d . . . H22A H 0.8195 0.2210 0.3136 0.083 Uiso 1 1 calc R . . H22B H 0.8515 0.2900 0.2949 0.083 Uiso 1 1 calc R . . C23 C 0.7888(3) 0.2477(3) 0.2165(4) 0.0581(18) Uani 1 1 d . . . H23A H 0.8141 0.2122 0.2035 0.070 Uiso 1 1 calc R . . H23B H 0.7503 0.2257 0.2097 0.070 Uiso 1 1 calc R . . C24 C 0.7842(3) 0.3169(3) 0.1751(3) 0.0568(18) Uani 1 1 d . . . H24A H 0.8231 0.3341 0.1757 0.068 Uiso 1 1 calc R . . H24B H 0.7632 0.3058 0.1305 0.068 Uiso 1 1 calc R . . C25 C 0.7527(3) 0.3746(3) 0.2009(3) 0.0437(13) Uani 1 1 d . . . C26 C 0.5787(3) 0.5000 0.1357(4) 0.048(2) Uani 1 2 d S . . C27 C 0.5269(4) 0.5000 0.0796(4) 0.072(4) Uani 1 2 d S . . H27A H 0.5343 0.4707 0.0447 0.087 Uiso 0.50 1 calc PR . . H27B H 0.5176 0.5499 0.0639 0.087 Uiso 0.50 1 calc PR . . C28 C 0.4729(4) 0.4653(10) 0.1029(5) 0.076(7) Uani 0.50 1 d P . . H28A H 0.4369 0.4703 0.0683 0.091 Uiso 0.50 1 calc PR . . H28B H 0.4798 0.4132 0.1120 0.091 Uiso 0.50 1 calc PR . . C29 C 0.4671(4) 0.5000 0.1566(5) 0.135(9) Uani 1 2 d S . . H29A H 0.4336 0.4785 0.1679 0.162 Uiso 0.50 1 calc PR . . H29B H 0.4572 0.5510 0.1450 0.162 Uiso 0.50 1 calc PR . . C30 C 0.5175(3) 0.5000 0.2169(4) 0.050(2) Uani 1 2 d S . . H30A H 0.5151 0.5433 0.2427 0.061 Uiso 0.50 1 calc PR . . H30B H 0.5151 0.4567 0.2427 0.061 Uiso 0.50 1 calc PR . . C31 C 0.5741(3) 0.5000 0.1996(3) 0.0371(17) Uani 1 2 d S . . C32 C 0.7072(3) 0.5000 0.0040(3) 0.0353(16) Uani 1 2 d S . . C33 C 0.6905(9) 0.4417(12) -0.0332(7) 0.078(6) Uani 0.50 1 d P . . H33 H 0.6765 0.4007 -0.0159 0.093 Uiso 0.50 1 calc PR . . C34 C 0.6930(8) 0.4397(8) -0.0961(6) 0.052(4) Uani 0.50 1 d P . . H34 H 0.6821 0.3969 -0.1203 0.062 Uiso 0.50 1 calc PR . . N6 N 0.7114(2) 0.5000 -0.1244(3) 0.0285(12) Uani 1 2 d S . . C35 C 0.7291(8) 0.5558(10) -0.0888(7) 0.065(5) Uani 0.50 1 d P . . H35 H 0.7423 0.5965 -0.1072 0.078 Uiso 0.50 1 calc PR . . C36 C 0.7297(9) 0.5594(10) -0.0240(7) 0.069(6) Uani 0.50 1 d P . . H36 H 0.7448 0.6006 0.0008 0.083 Uiso 0.50 1 calc PR . . 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 Zn1 0.0174(3) 0.0210(4) 0.0229(4) 0.000 0.0116(3) 0.000 Zn2 0.0198(3) 0.0231(4) 0.0229(4) 0.000 0.0144(3) 0.000 Fe1 0.0343(5) 0.0354(5) 0.0212(4) 0.000 0.0153(4) 0.000 O1 0.039(2) 0.054(2) 0.040(2) 0.0134(18) 0.0119(16) -0.0214(18) O2 0.0334(17) 0.0388(19) 0.0360(18) -0.0091(15) 0.0208(15) -0.0166(15) O3 0.0324(18) 0.049(2) 0.044(2) -0.0054(18) 0.0116(15) 0.0192(17) O4 0.040(2) 0.053(2) 0.048(2) 0.0118(19) 0.0249(17) 0.0231(18) O5A 0.039(4) 0.044(5) 0.021(3) 0.003(3) 0.016(3) -0.003(4) O6A 0.047(5) 0.042(5) 0.027(4) -0.004(3) 0.022(4) -0.001(4) O5B 0.046(4) 0.020(3) 0.031(4) 0.005(3) 0.021(4) 0.000(3) O6B 0.046(5) 0.033(4) 0.039(4) -0.006(3) 0.031(4) 0.000(4) O7 0.041(3) 0.039(4) 0.008(2) -0.011(2) 0.014(2) -0.008(3) O8 0.039(3) 0.045(4) 0.017(3) 0.002(2) 0.017(2) 0.004(3) N1 0.025(3) 0.030(3) 0.024(3) 0.000 0.013(2) 0.000 N2A 0.031(7) 0.041(6) 0.028(7) 0.007(5) 0.014(7) 0.004(7) N3A 0.048(8) 0.035(7) 0.031(5) 0.004(4) 0.021(6) -0.010(5) N2B 0.045(8) 0.030(7) 0.012(5) 0.002(4) 0.013(7) 0.021(7) N3B 0.045(7) 0.020(6) 0.037(6) 0.011(4) 0.033(6) 0.006(5) N4 0.043(4) 0.029(6) 0.011(3) -0.004(2) 0.015(3) -0.006(3) N5 0.039(4) 0.036(7) 0.018(3) 0.002(3) 0.018(3) 0.004(3) B1 0.027(4) 0.061(6) 0.023(4) 0.000 0.007(3) 0.000 B2 0.060(5) 0.038(4) 0.023(4) 0.000 0.024(4) 0.000 C1 0.027(2) 0.021(2) 0.039(3) 0.0034(19) 0.0171(19) -0.0003(17) C2 0.031(2) 0.033(3) 0.037(3) -0.002(2) 0.019(2) -0.012(2) C3 0.056(3) 0.059(4) 0.038(3) 0.006(3) 0.017(3) -0.022(3) C4 0.051(3) 0.058(4) 0.040(3) 0.001(3) 0.011(3) -0.029(3) C5 0.042(3) 0.056(4) 0.041(3) 0.007(3) 0.016(2) -0.029(3) C6 0.041(3) 0.060(4) 0.040(3) 0.003(3) 0.017(2) -0.019(3) C7 0.038(3) 0.070(4) 0.035(3) 0.007(3) 0.012(2) -0.023(3) C8 0.025(2) 0.029(2) 0.045(3) 0.005(2) 0.017(2) 0.0045(19) C9 0.025(2) 0.037(3) 0.044(3) -0.001(2) 0.014(2) 0.011(2) C10 0.051(3) 0.083(5) 0.044(3) -0.006(3) 0.015(3) 0.042(4) C11 0.070(4) 0.096(6) 0.045(4) 0.002(4) 0.010(3) 0.064(4) C12 0.036(3) 0.054(3) 0.039(3) -0.001(2) 0.013(2) 0.024(3) C13 0.044(3) 0.065(4) 0.036(3) 0.002(3) 0.021(2) 0.028(3) C14 0.039(3) 0.049(3) 0.042(3) 0.018(2) 0.020(2) 0.025(2) C15 0.024(4) 0.146(11) 0.024(4) 0.000 0.012(3) 0.000 C16 0.034(4) 0.146(11) 0.028(4) 0.000 0.022(3) 0.000 C17 0.040(4) 0.052(5) 0.029(4) 0.000 0.016(3) 0.000 C18 0.041(4) 0.123(10) 0.022(4) 0.000 0.013(3) 0.000 C19 0.040(4) 0.083(7) 0.034(4) 0.000 0.020(3) 0.000 C20 0.052(3) 0.021(2) 0.039(3) 0.001(2) 0.016(2) 0.001(2) C21 0.077(4) 0.032(3) 0.047(3) 0.010(3) 0.005(3) 0.012(3) C22 0.075(5) 0.045(4) 0.087(5) 0.020(4) 0.021(4) 0.032(4) C23 0.080(5) 0.031(3) 0.078(5) 0.011(3) 0.048(4) 0.022(3) C24 0.087(5) 0.036(3) 0.066(4) 0.015(3) 0.052(4) 0.025(3) C25 0.058(3) 0.031(3) 0.053(3) 0.008(2) 0.034(3) 0.013(2) C26 0.032(4) 0.092(7) 0.024(4) 0.000 0.015(3) 0.000 C27 0.038(4) 0.160(13) 0.024(4) 0.000 0.017(3) 0.000 C28 0.023(5) 0.18(2) 0.023(5) -0.012(7) 0.004(4) -0.008(7) C29 0.025(4) 0.35(3) 0.035(5) 0.000 0.010(4) 0.000 C30 0.028(4) 0.091(7) 0.037(4) 0.000 0.015(3) 0.000 C31 0.030(3) 0.064(5) 0.021(3) 0.000 0.013(3) 0.000 C32 0.035(3) 0.056(5) 0.019(3) 0.000 0.016(3) 0.000 C33 0.122(15) 0.099(14) 0.021(7) -0.008(7) 0.034(9) -0.053(13) C34 0.098(11) 0.045(7) 0.025(6) -0.010(5) 0.039(8) -0.017(8) N6 0.025(3) 0.044(3) 0.023(3) 0.000 0.018(2) 0.000 C35 0.084(11) 0.089(12) 0.038(7) -0.015(7) 0.041(8) -0.052(10) C36 0.127(15) 0.065(10) 0.026(7) -0.023(7) 0.038(9) -0.045(12) _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 Zn1 O1 2.032(3) 6_565 ? Zn1 O1 2.032(3) . ? Zn1 O4 2.049(4) . ? Zn1 O4 2.049(4) 6_565 ? Zn1 N1 2.054(5) . ? Zn1 Zn2 2.9846(11) . ? Zn2 N6 2.026(5) 1_556 ? Zn2 O3 2.032(3) . ? Zn2 O3 2.032(3) 6_565 ? Zn2 O2 2.061(3) . ? Zn2 O2 2.061(3) 6_565 ? Fe1 N2A 1.85(2) 6_565 ? Fe1 N2A 1.85(2) . ? Fe1 N3B 1.907(12) . ? Fe1 N3B 1.907(12) 6_565 ? Fe1 N4 1.910(7) 6_565 ? Fe1 N4 1.910(7) . ? Fe1 N5 1.922(7) 6_565 ? Fe1 N5 1.922(7) . ? Fe1 N3A 1.925(15) 6_565 ? Fe1 N3A 1.925(15) . ? Fe1 N2B 1.956(17) 6_565 ? Fe1 N2B 1.956(17) . ? O1 C1 1.263(6) . ? O2 C1 1.251(6) . ? O3 C8 1.262(6) . ? O4 C8 1.248(6) . ? O5A B1 1.410(9) . ? O5A N2A 1.41(2) . ? O6A N3A 1.442(16) . ? O6A B2 1.475(9) . ? O5B N2B 1.363(18) . ? O5B B1 1.544(10) . ? O6B N3B 1.395(15) . ? O6B B2 1.496(11) . ? O7 O7 0.884(13) 6_565 ? O7 N4 1.383(8) . ? O7 B2 1.526(11) . ? O7 N4 1.572(8) 6_565 ? O8 O8 1.000(14) 6_565 ? O8 N5 1.387(9) . ? O8 B1 1.525(10) . ? O8 N5 1.605(9) 6_565 ? N1 C19 1.316(10) . ? N1 C15 1.335(9) . ? N2A C20 1.40(2) . ? N3A C25 1.299(16) . ? N2B C20 1.266(18) . ? N3B C25 1.302(13) . ? N4 N4 0.632(13) 6_565 ? N4 C26 1.347(10) . ? N4 O7 1.572(8) 6_565 ? N5 N5 0.651(14) 6_565 ? N5 C31 1.341(10) . ? N5 O8 1.605(9) 6_565 ? B1 O5A 1.410(9) 6_565 ? B1 O8 1.525(10) 6_565 ? B1 O5B 1.544(10) 6_565 ? B1 C17 1.619(10) . ? B2 O6A 1.475(9) 6_565 ? B2 O6B 1.496(11) 6_565 ? B2 O7 1.526(11) 6_565 ? B2 C32 1.615(10) . ? C1 C2 1.502(6) . ? C2 C7 1.390(7) . ? C2 C3 1.393(8) . ? C3 C4 1.382(8) . ? C3 H3 0.9500 . ? C4 C5 1.407(8) . ? C4 H4 0.9500 . ? C5 C6 1.368(8) . ? C5 C12 1.485(6) 8_455 ? C6 C7 1.376(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.512(6) . ? C9 C14 1.405(7) . ? C9 C10 1.415(8) . ? C10 C11 1.383(7) . ? C10 H10 0.9500 . ? C11 C12 1.408(8) . ? C11 H11 0.9500 . ? C12 C13 1.414(8) . ? C12 C5 1.485(6) 8 ? C13 C14 1.384(7) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.394(11) . ? C15 H15 0.9500 . ? C16 C17 1.375(11) . ? C16 H16 0.9500 . ? C17 C18 1.385(11) . ? C18 C19 1.396(11) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.445(8) . ? C20 C21 1.499(7) . ? C21 C22 1.504(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.559(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.553(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.506(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 N4 1.347(10) 6_565 ? C26 C31 1.429(9) . ? C26 C27 1.496(11) . ? C27 C28 1.653(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.376(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.533(12) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N5 1.341(10) 6_565 ? C32 C33 1.345(19) . ? C32 C33 1.345(19) 6_565 ? C32 C36 1.433(16) 6_565 ? C32 C36 1.433(16) . ? C33 C34 1.388(18) . ? C33 H33 0.9500 . ? C34 N6 1.405(13) . ? C34 H34 0.9500 . ? N6 N6 0.000(12) 6_565 ? N6 C35 1.295(16) . ? N6 C35 1.295(16) 6_565 ? N6 C34 1.405(13) 6_565 ? N6 Zn2 2.026(5) 1_554 ? C35 C36 1.410(19) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 Zn1 O1 85.5(3) 6_565 . ? O1 Zn1 O4 158.89(16) 6_565 . ? O1 Zn1 O4 90.38(17) . . ? O1 Zn1 O4 90.38(17) 6_565 6_565 ? O1 Zn1 O4 158.89(16) . 6_565 ? O4 Zn1 O4 86.0(3) . 6_565 ? O1 Zn1 N1 105.08(15) 6_565 . ? O1 Zn1 N1 105.08(15) . . ? O4 Zn1 N1 95.99(15) . . ? O4 Zn1 N1 95.99(15) 6_565 . ? O1 Zn1 Zn2 85.27(11) 6_565 . ? O1 Zn1 Zn2 85.27(11) . . ? O4 Zn1 Zn2 73.74(11) . . ? O4 Zn1 Zn2 73.74(11) 6_565 . ? N1 Zn1 Zn2 165.69(15) . . ? N6 Zn2 O3 103.77(15) 1_556 . ? N6 Zn2 O3 103.77(16) 1_556 6_565 ? O3 Zn2 O3 87.4(2) . 6_565 ? N6 Zn2 O2 97.68(14) 1_556 . ? O3 Zn2 O2 89.26(16) . . ? O3 Zn2 O2 158.48(15) 6_565 . ? N6 Zn2 O2 97.69(14) 1_556 6_565 ? O3 Zn2 O2 158.48(15) . 6_565 ? O3 Zn2 O2 89.26(16) 6_565 6_565 ? O2 Zn2 O2 86.1(2) . 6_565 ? N6 Zn2 Zn1 167.55(15) 1_556 . ? O3 Zn2 Zn1 85.11(11) . . ? O3 Zn2 Zn1 85.11(11) 6_565 . ? O2 Zn2 Zn1 73.42(10) . . ? O2 Zn2 Zn1 73.42(10) 6_565 . ? N2A Fe1 N2A 92.0(13) 6_565 . ? N2A Fe1 N3B 133.0(5) 6_565 . ? N2A Fe1 N3B 79.3(7) . . ? N2A Fe1 N3B 79.3(7) 6_565 6_565 ? N2A Fe1 N3B 133.0(5) . 6_565 ? N3B Fe1 N3B 74.1(6) . 6_565 ? N2A Fe1 N4 118.6(6) 6_565 6_565 ? N2A Fe1 N4 135.8(5) . 6_565 ? N3B Fe1 N4 97.7(5) . 6_565 ? N3B Fe1 N4 86.3(5) 6_565 6_565 ? N2A Fe1 N4 135.8(5) 6_565 . ? N2A Fe1 N4 118.6(6) . . ? N3B Fe1 N4 86.3(5) . . ? N3B Fe1 N4 97.7(5) 6_565 . ? N4 Fe1 N4 19.1(4) 6_565 . ? N2A Fe1 N5 86.7(5) 6_565 6_565 ? N2A Fe1 N5 72.4(5) . 6_565 ? N3B Fe1 N5 132.0(4) . 6_565 ? N3B Fe1 N5 150.9(4) 6_565 6_565 ? N4 Fe1 N5 78.2(3) 6_565 6_565 ? N4 Fe1 N5 74.9(3) . 6_565 ? N2A Fe1 N5 72.4(5) 6_565 . ? N2A Fe1 N5 86.7(5) . . ? N3B Fe1 N5 150.9(4) . . ? N3B Fe1 N5 132.0(4) 6_565 . ? N4 Fe1 N5 74.9(3) 6_565 . ? N4 Fe1 N5 78.2(3) . . ? N5 Fe1 N5 19.5(4) 6_565 . ? N2A Fe1 N3A 76.7(8) 6_565 6_565 ? N2A Fe1 N3A 149.9(5) . 6_565 ? N3B Fe1 N3A 88.1(5) . 6_565 ? N3B Fe1 N3A 18.2(4) 6_565 6_565 ? N4 Fe1 N3A 72.6(5) 6_565 6_565 ? N4 Fe1 N3A 87.3(5) . 6_565 ? N5 Fe1 N3A 133.2(4) 6_565 6_565 ? N5 Fe1 N3A 115.3(4) . 6_565 ? N2A Fe1 N3A 149.9(5) 6_565 . ? N2A Fe1 N3A 76.7(8) . . ? N3B Fe1 N3A 18.2(4) . . ? N3B Fe1 N3A 88.1(5) 6_565 . ? N4 Fe1 N3A 87.3(5) 6_565 . ? N4 Fe1 N3A 72.6(5) . . ? N5 Fe1 N3A 115.3(4) 6_565 . ? N5 Fe1 N3A 133.2(4) . . ? N3A Fe1 N3A 99.2(7) 6_565 . ? N2A Fe1 N2B 15.2(6) 6_565 6_565 ? N2A Fe1 N2B 85.5(4) . 6_565 ? N3B Fe1 N2B 118.1(6) . 6_565 ? N3B Fe1 N2B 74.2(6) 6_565 6_565 ? N4 Fe1 N2B 131.2(5) 6_565 6_565 ? N4 Fe1 N2B 149.6(5) . 6_565 ? N5 Fe1 N2B 97.7(5) 6_565 6_565 ? N5 Fe1 N2B 85.7(5) . 6_565 ? N3A Fe1 N2B 76.4(6) 6_565 6_565 ? N3A Fe1 N2B 134.7(6) . 6_565 ? N2A Fe1 N2B 85.5(4) 6_565 . ? N2A Fe1 N2B 15.2(6) . . ? N3B Fe1 N2B 74.2(6) . . ? N3B Fe1 N2B 118.1(6) 6_565 . ? N4 Fe1 N2B 149.6(5) 6_565 . ? N4 Fe1 N2B 131.2(5) . . ? N5 Fe1 N2B 85.7(5) 6_565 . ? N5 Fe1 N2B 97.7(5) . . ? N3A Fe1 N2B 134.7(6) 6_565 . ? N3A Fe1 N2B 76.4(6) . . ? N2B Fe1 N2B 76.1(10) 6_565 . ? C1 O1 Zn1 120.5(3) . . ? C1 O2 Zn2 134.8(3) . . ? C8 O3 Zn2 119.9(3) . . ? C8 O4 Zn1 134.4(4) . . ? B1 O5A N2A 110.1(11) . . ? N3A O6A B2 111.3(8) . . ? N2B O5B B1 112.0(9) . . ? N3B O6B B2 111.3(7) . . ? O7 O7 N4 84.8(4) 6_565 . ? O7 O7 B2 73.2(3) 6_565 . ? N4 O7 B2 111.5(6) . . ? O7 O7 N4 61.2(3) 6_565 6_565 ? B2 O7 N4 101.9(5) . 6_565 ? O8 O8 N5 82.8(4) 6_565 . ? O8 O8 B1 70.9(3) 6_565 . ? N5 O8 B1 109.7(6) . . ? O8 O8 N5 59.0(3) 6_565 6_565 ? B1 O8 N5 99.1(5) . 6_565 ? C19 N1 C15 118.8(6) . . ? C19 N1 Zn1 124.8(5) . . ? C15 N1 Zn1 116.4(5) . . ? C20 N2A O5A 114.9(15) . . ? C20 N2A Fe1 118.1(12) . . ? O5A N2A Fe1 125.8(14) . . ? C25 N3A O6A 117.2(11) . . ? C25 N3A Fe1 117.8(9) . . ? O6A N3A Fe1 121.3(10) . . ? C20 N2B O5B 116.7(14) . . ? C20 N2B Fe1 118.8(11) . . ? O5B N2B Fe1 122.3(11) . . ? C25 N3B O6B 114.7(9) . . ? C25 N3B Fe1 118.8(8) . . ? O6B N3B Fe1 123.7(8) . . ? N4 N4 C26 76.4(3) 6_565 . ? N4 N4 O7 95.2(4) 6_565 . ? C26 N4 O7 116.0(7) . . ? N4 N4 O7 61.2(3) 6_565 6_565 ? C26 N4 O7 104.7(6) . 6_565 ? N4 N4 Fe1 80.5(2) 6_565 . ? C26 N4 Fe1 117.7(5) . . ? O7 N4 Fe1 123.2(5) . . ? O7 N4 Fe1 112.9(5) 6_565 . ? N5 N5 C31 76.0(3) 6_565 . ? N5 N5 O8 97.2(4) 6_565 . ? C31 N5 O8 116.0(6) . . ? N5 N5 O8 59.0(3) 6_565 6_565 ? C31 N5 O8 103.1(6) . 6_565 ? N5 N5 Fe1 80.2(2) 6_565 . ? C31 N5 Fe1 117.5(5) . . ? O8 N5 Fe1 123.8(6) . . ? O8 N5 Fe1 112.1(5) 6_565 . ? O5A B1 O5A 136.0(9) . 6_565 ? O5A B1 O8 78.8(5) . 6_565 ? O5A B1 O8 114.4(6) 6_565 6_565 ? O5A B1 O8 114.4(6) . . ? O5A B1 O8 78.8(5) 6_565 . ? O5A B1 O5B 112.9(7) 6_565 . ? O8 B1 O5B 106.1(5) 6_565 . ? O8 B1 O5B 136.3(6) . . ? O5A B1 O5B 112.9(7) . 6_565 ? O8 B1 O5B 136.3(6) 6_565 6_565 ? O8 B1 O5B 106.1(5) . 6_565 ? O5B B1 O5B 85.7(7) . 6_565 ? O5A B1 C17 107.4(4) . . ? O5A B1 C17 107.4(4) 6_565 . ? O8 B1 C17 107.9(6) 6_565 . ? O8 B1 C17 107.9(6) . . ? O5B B1 C17 107.9(5) . . ? O5B B1 C17 107.9(5) 6_565 . ? O6A B2 O6A 140.1(9) . 6_565 ? O6A B2 O6B 115.1(8) . 6_565 ? O6A B2 O6B 115.1(8) 6_565 . ? O6B B2 O6B 85.0(9) 6_565 . ? O6A B2 O7 110.0(6) . 6_565 ? O6A B2 O7 78.3(5) 6_565 6_565 ? O6B B2 O7 108.0(5) 6_565 6_565 ? O6B B2 O7 134.5(6) . 6_565 ? O6A B2 O7 78.3(5) . . ? O6A B2 O7 110.0(6) 6_565 . ? O6B B2 O7 134.5(6) 6_565 . ? O6B B2 O7 108.0(5) . . ? O6A B2 C32 107.1(4) . . ? O6A B2 C32 107.1(4) 6_565 . ? O6B B2 C32 109.0(5) 6_565 . ? O6B B2 C32 109.0(5) . . ? O7 B2 C32 107.4(6) 6_565 . ? O7 B2 C32 107.4(6) . . ? O2 C1 O1 125.1(4) . . ? O2 C1 C2 117.3(4) . . ? O1 C1 C2 117.6(4) . . ? C7 C2 C3 118.0(4) . . ? C7 C2 C1 121.2(5) . . ? C3 C2 C1 120.4(5) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 118.7(5) . . ? C6 C5 C12 120.0(5) . 8_455 ? C4 C5 C12 121.2(5) . 8_455 ? C5 C6 C7 120.9(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 121.1(5) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? O4 C8 O3 126.2(4) . . ? O4 C8 C9 116.8(5) . . ? O3 C8 C9 116.9(4) . . ? C14 C9 C10 119.3(4) . . ? C14 C9 C8 120.1(5) . . ? C10 C9 C8 120.6(5) . . ? C11 C10 C9 118.8(6) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 123.3(6) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C13 116.4(5) . . ? C11 C12 C5 121.9(5) . 8 ? C13 C12 C5 121.7(5) . 8 ? C14 C13 C12 121.7(5) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C9 120.4(5) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? N1 C15 C16 121.2(7) . . ? N1 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C17 C16 C15 121.3(7) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 115.9(7) . . ? C16 C17 B1 120.9(6) . . ? C18 C17 B1 123.2(7) . . ? C17 C18 C19 120.3(8) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? N1 C19 C18 122.4(7) . . ? N1 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? N2B C20 C25 110.2(9) . . ? N2A C20 C25 108.6(9) . . ? N2B C20 C21 125.8(9) . . ? N2A C20 C21 128.1(10) . . ? C25 C20 C21 122.5(5) . . ? C20 C21 C22 113.2(6) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 111.5(6) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 110.6(6) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 109.4(5) . . ? C25 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? C25 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N3A C25 C20 110.2(7) . . ? N3B C25 C20 110.2(7) . . ? N3A C25 C24 125.9(8) . . ? N3B C25 C24 125.5(7) . . ? C20 C25 C24 122.4(5) . . ? N4 C26 C31 109.7(6) . . ? N4 C26 C31 109.7(6) 6_565 . ? N4 C26 C27 126.5(6) . . ? N4 C26 C27 126.5(6) 6_565 . ? C31 C26 C27 122.0(7) . . ? C26 C27 C28 107.8(6) . . ? C26 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? C26 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.5 . . ? C29 C28 C27 110.5(10) . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C28 C29 C30 119.4(8) . . ? C28 C29 H29A 107.5 . . ? C30 C29 H29A 107.5 . . ? C28 C29 H29B 107.5 . . ? C30 C29 H29B 107.5 . . ? H29A C29 H29B 107.0 . . ? C31 C30 C29 110.5(7) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? N5 C31 C26 109.5(6) . . ? N5 C31 C26 109.5(6) 6_565 . ? N5 C31 C30 124.9(6) . . ? N5 C31 C30 124.9(6) 6_565 . ? C26 C31 C30 123.7(7) . . ? C33 C32 C33 106.7(18) . 6_565 ? C33 C32 C36 116.5(8) 6_565 6_565 ? C33 C32 C36 116.5(8) . . ? C36 C32 C36 100.2(15) 6_565 . ? C33 C32 B2 120.3(7) . . ? C33 C32 B2 120.3(7) 6_565 . ? C36 C32 B2 123.2(6) 6_565 . ? C36 C32 B2 123.2(6) . . ? C32 C33 C34 122.1(14) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C33 C34 N6 121.0(12) . . ? C33 C34 H34 119.5 . . ? N6 C34 H34 119.5 . . ? C35 N6 C35 105.9(18) . 6_565 ? C35 N6 C34 117.5(8) 6_565 6_565 ? C35 N6 C34 117.5(8) . . ? C34 N6 C34 105.2(12) 6_565 . ? C35 N6 Zn2 121.9(7) . 1_554 ? C35 N6 Zn2 121.9(7) 6_565 1_554 ? C34 N6 Zn2 120.6(6) 6_565 1_554 ? C34 N6 Zn2 120.6(6) . 1_554 ? N6 C35 C36 123.5(13) . . ? N6 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C35 C36 C32 119.1(12) . . ? C35 C36 H36 120.4 . . ? C32 C36 H36 120.4 . . ? 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 Zn1 Zn2 N6 42.95(13) 6_565 . . 1_556 ? O1 Zn1 Zn2 N6 -42.93(13) . . . 1_556 ? O4 Zn1 Zn2 N6 -134.72(13) . . . 1_556 ? O4 Zn1 Zn2 N6 134.73(13) 6_565 . . 1_556 ? N1 Zn1 Zn2 N6 -179.994(3) . . . 1_556 ? O1 Zn1 Zn2 O3 179.06(18) 6_565 . . . ? O1 Zn1 Zn2 O3 93.19(18) . . . . ? O4 Zn1 Zn2 O3 1.40(17) . . . . ? O4 Zn1 Zn2 O3 -89.16(18) 6_565 . . . ? N1 Zn1 Zn2 O3 -43.88(12) . . . . ? O1 Zn1 Zn2 O3 -93.18(18) 6_565 . . 6_565 ? O1 Zn1 Zn2 O3 -179.06(18) . . . 6_565 ? O4 Zn1 Zn2 O3 89.16(18) . . . 6_565 ? O4 Zn1 Zn2 O3 -1.40(17) 6_565 . . 6_565 ? N1 Zn1 Zn2 O3 43.88(12) . . . 6_565 ? O1 Zn1 Zn2 O2 88.38(17) 6_565 . . . ? O1 Zn1 Zn2 O2 2.50(17) . . . . ? O4 Zn1 Zn2 O2 -89.28(17) . . . . ? O4 Zn1 Zn2 O2 -179.84(17) 6_565 . . . ? N1 Zn1 Zn2 O2 -134.56(11) . . . . ? O1 Zn1 Zn2 O2 -2.50(17) 6_565 . . 6_565 ? O1 Zn1 Zn2 O2 -88.38(17) . . . 6_565 ? O4 Zn1 Zn2 O2 179.84(17) . . . 6_565 ? O4 Zn1 Zn2 O2 89.28(17) 6_565 . . 6_565 ? N1 Zn1 Zn2 O2 134.56(11) . . . 6_565 ? O1 Zn1 O1 C1 -84.2(4) 6_565 . . . ? O4 Zn1 O1 C1 75.1(4) . . . . ? O4 Zn1 O1 C1 -4.8(8) 6_565 . . . ? N1 Zn1 O1 C1 171.4(4) . . . . ? Zn2 Zn1 O1 C1 1.4(4) . . . . ? N6 Zn2 O2 C1 162.0(4) 1_556 . . . ? O3 Zn2 O2 C1 -94.2(5) . . . . ? O3 Zn2 O2 C1 -13.3(7) 6_565 . . . ? O2 Zn2 O2 C1 64.8(5) 6_565 . . . ? Zn1 Zn2 O2 C1 -9.0(4) . . . . ? N6 Zn2 O3 C8 173.1(4) 1_556 . . . ? O3 Zn2 O3 C8 -83.4(4) 6_565 . . . ? O2 Zn2 O3 C8 75.3(4) . . . . ? O2 Zn2 O3 C8 -2.2(7) 6_565 . . . ? Zn1 Zn2 O3 C8 1.9(4) . . . . ? O1 Zn1 O4 C8 -12.9(9) 6_565 . . . ? O1 Zn1 O4 C8 -91.3(5) . . . . ? O4 Zn1 O4 C8 67.8(5) 6_565 . . . ? N1 Zn1 O4 C8 163.5(5) . . . . ? Zn2 Zn1 O4 C8 -6.4(5) . . . . ? O1 Zn1 N1 C19 -44.68(13) 6_565 . . . ? O1 Zn1 N1 C19 44.68(13) . . . . ? O4 Zn1 N1 C19 136.70(13) . . . . ? O4 Zn1 N1 C19 -136.69(13) 6_565 . . . ? Zn2 Zn1 N1 C19 180.000(2) . . . . ? O1 Zn1 N1 C15 135.32(13) 6_565 . . . ? O1 Zn1 N1 C15 -135.32(13) . . . . ? O4 Zn1 N1 C15 -43.30(13) . . . . ? O4 Zn1 N1 C15 43.31(13) 6_565 . . . ? Zn2 Zn1 N1 C15 0.000(3) . . . . ? B1 O5A N2A C20 152.6(10) . . . . ? B1 O5A N2A Fe1 -14.6(14) . . . . ? N2A Fe1 N2A C20 -128.0(10) 6_565 . . . ? N3B Fe1 N2A C20 5.4(10) . . . . ? N3B Fe1 N2A C20 -50.8(16) 6_565 . . . ? N4 Fe1 N2A C20 95.5(9) 6_565 . . . ? N4 Fe1 N2A C20 85.1(10) . . . . ? N5 Fe1 N2A C20 146.2(12) 6_565 . . . ? N5 Fe1 N2A C20 159.8(11) . . . . ? N3A Fe1 N2A C20 -61(2) 6_565 . . . ? N3A Fe1 N2A C20 23.8(10) . . . . ? N2B Fe1 N2A C20 -114.3(10) 6_565 . . . ? N2B Fe1 N2A C20 -64(3) . . . . ? N2A Fe1 N2A O5A 38.9(13) 6_565 . . . ? N3B Fe1 N2A O5A 172.3(12) . . . . ? N3B Fe1 N2A O5A 116.1(10) 6_565 . . . ? N4 Fe1 N2A O5A -97.6(14) 6_565 . . . ? N4 Fe1 N2A O5A -108.0(12) . . . . ? N5 Fe1 N2A O5A -47.0(10) 6_565 . . . ? N5 Fe1 N2A O5A -33.4(11) . . . . ? N3A Fe1 N2A O5A 105.4(14) 6_565 . . . ? N3A Fe1 N2A O5A -169.3(12) . . . . ? N2B Fe1 N2A O5A 52.6(13) 6_565 . . . ? N2B Fe1 N2A O5A 103(5) . . . . ? B2 O6A N3A C25 -144.1(9) . . . . ? B2 O6A N3A Fe1 13.6(12) . . . . ? N2A Fe1 N3A C25 42.8(19) 6_565 . . . ? N2A Fe1 N3A C25 -27.6(8) . . . . ? N3B Fe1 N3A C25 69(2) . . . . ? N3B Fe1 N3A C25 107.5(7) 6_565 . . . ? N4 Fe1 N3A C25 -166.1(8) 6_565 . . . ? N4 Fe1 N3A C25 -153.8(9) . . . . ? N5 Fe1 N3A C25 -90.5(9) 6_565 . . . ? N5 Fe1 N3A C25 -99.8(9) . . . . ? N3A Fe1 N3A C25 122.0(8) 6_565 . . . ? N2B Fe1 N3A C25 42.0(13) 6_565 . . . ? N2B Fe1 N3A C25 -12.0(9) . . . . ? N2A Fe1 N3A O6A -114.8(17) 6_565 . . . ? N2A Fe1 N3A O6A 174.8(10) . . . . ? N3B Fe1 N3A O6A -89(2) . . . . ? N3B Fe1 N3A O6A -50.1(10) 6_565 . . . ? N4 Fe1 N3A O6A 36.3(9) 6_565 . . . ? N4 Fe1 N3A O6A 48.6(9) . . . . ? N5 Fe1 N3A O6A 111.9(9) 6_565 . . . ? N5 Fe1 N3A O6A 102.6(9) . . . . ? N3A Fe1 N3A O6A -35.6(12) 6_565 . . . ? N2B Fe1 N3A O6A -115.6(11) 6_565 . . . ? N2B Fe1 N3A O6A -169.6(10) . . . . ? B1 O5B N2B C20 -152.9(9) . . . . ? B1 O5B N2B Fe1 9.9(14) . . . . ? N2A Fe1 N2B C20 -161.3(11) 6_565 . . . ? N2A Fe1 N2B C20 83(4) . . . . ? N3B Fe1 N2B C20 -24.3(10) . . . . ? N3B Fe1 N2B C20 -86.0(12) 6_565 . . . ? N4 Fe1 N2B C20 53.9(16) 6_565 . . . ? N4 Fe1 N2B C20 46.1(13) . . . . ? N5 Fe1 N2B C20 111.7(11) 6_565 . . . ? N5 Fe1 N2B C20 127.1(10) . . . . ? N3A Fe1 N2B C20 -95.2(13) 6_565 . . . ? N3A Fe1 N2B C20 -5.6(10) . . . . ? N2B Fe1 N2B C20 -149.3(8) 6_565 . . . ? N2A Fe1 N2B O5B 36.2(13) 6_565 . . . ? N2A Fe1 N2B O5B -79(4) . . . . ? N3B Fe1 N2B O5B 173.3(13) . . . . ? N3B Fe1 N2B O5B 111.5(11) 6_565 . . . ? N4 Fe1 N2B O5B -108.5(13) 6_565 . . . ? N4 Fe1 N2B O5B -116.4(11) . . . . ? N5 Fe1 N2B O5B -50.8(11) 6_565 . . . ? N5 Fe1 N2B O5B -35.3(12) . . . . ? N3A Fe1 N2B O5B 102.4(12) 6_565 . . . ? N3A Fe1 N2B O5B -168.1(13) . . . . ? N2B Fe1 N2B O5B 48.3(13) 6_565 . . . ? B2 O6B N3B C25 151.8(9) . . . . ? B2 O6B N3B Fe1 -9.0(13) . . . . ? N2A Fe1 N3B C25 92.7(13) 6_565 . . . ? N2A Fe1 N3B C25 9.9(10) . . . . ? N3B Fe1 N3B C25 150.7(7) 6_565 . . . ? N4 Fe1 N3B C25 -125.4(9) 6_565 . . . ? N4 Fe1 N3B C25 -110.1(10) . . . . ? N5 Fe1 N3B C25 -44.3(13) 6_565 . . . ? N5 Fe1 N3B C25 -52.6(16) . . . . ? N3A Fe1 N3B C25 162.4(11) 6_565 . . . ? N3A Fe1 N3B C25 -70(2) . . . . ? N2B Fe1 N3B C25 88.9(11) 6_565 . . . ? N2B Fe1 N3B C25 24.6(10) . . . . ? N2A Fe1 N3B O6B -107.3(14) 6_565 . . . ? N2A Fe1 N3B O6B 170.0(11) . . . . ? N3B Fe1 N3B O6B -49.3(12) 6_565 . . . ? N4 Fe1 N3B O6B 34.6(10) 6_565 . . . ? N4 Fe1 N3B O6B 49.9(10) . . . . ? N5 Fe1 N3B O6B 115.7(9) 6_565 . . . ? N5 Fe1 N3B O6B 107.4(10) . . . . ? N3A Fe1 N3B O6B -37.5(11) 6_565 . . . ? N3A Fe1 N3B O6B 90(3) . . . . ? N2B Fe1 N3B O6B -111.1(11) 6_565 . . . ? N2B Fe1 N3B O6B -175.3(12) . . . . ? O7 O7 N4 N4 -0.002(3) 6_565 . . 6_565 ? B2 O7 N4 N4 69.6(4) . . . 6_565 ? O7 O7 N4 C26 77.4(5) 6_565 . . . ? B2 O7 N4 C26 147.0(5) . . . . ? N4 O7 N4 C26 77.4(5) 6_565 . . . ? B2 O7 N4 O7 69.6(4) . . . 6_565 ? N4 O7 N4 O7 0.002(5) 6_565 . . 6_565 ? O7 O7 N4 Fe1 -82.0(5) 6_565 . . . ? B2 O7 N4 Fe1 -12.4(8) . . . . ? N4 O7 N4 Fe1 -82.0(5) 6_565 . . . ? N2A Fe1 N4 N4 29.0(9) 6_565 . . 6_565 ? N2A Fe1 N4 N4 157.4(7) . . . 6_565 ? N3B Fe1 N4 N4 -127.0(3) . . . 6_565 ? N3B Fe1 N4 N4 -53.6(3) 6_565 . . 6_565 ? N5 Fe1 N4 N4 97.6(2) 6_565 . . 6_565 ? N5 Fe1 N4 N4 77.8(2) . . . 6_565 ? N3A Fe1 N4 N4 -38.7(3) 6_565 . . 6_565 ? N3A Fe1 N4 N4 -139.1(4) . . . 6_565 ? N2B Fe1 N4 N4 18.4(9) 6_565 . . 6_565 ? N2B Fe1 N4 N4 167.8(6) . . . 6_565 ? N2A Fe1 N4 C26 -40.1(11) 6_565 . . . ? N2A Fe1 N4 C26 88.3(8) . . . . ? N3B Fe1 N4 C26 163.9(6) . . . . ? N3B Fe1 N4 C26 -122.7(5) 6_565 . . . ? N4 Fe1 N4 C26 -69.1(5) 6_565 . . . ? N5 Fe1 N4 C26 28.5(5) 6_565 . . . ? N5 Fe1 N4 C26 8.7(5) . . . . ? N3A Fe1 N4 C26 -107.8(6) 6_565 . . . ? N3A Fe1 N4 C26 151.8(6) . . . . ? N2B Fe1 N4 C26 -50.7(11) 6_565 . . . ? N2B Fe1 N4 C26 98.7(7) . . . . ? N2A Fe1 N4 O7 119.0(10) 6_565 . . . ? N2A Fe1 N4 O7 -112.6(8) . . . . ? N3B Fe1 N4 O7 -36.9(6) . . . . ? N3B Fe1 N4 O7 36.5(7) 6_565 . . . ? N4 Fe1 N4 O7 90.0(6) 6_565 . . . ? N5 Fe1 N4 O7 -172.3(6) 6_565 . . . ? N5 Fe1 N4 O7 167.9(6) . . . . ? N3A Fe1 N4 O7 51.4(7) 6_565 . . . ? N3A Fe1 N4 O7 -49.1(7) . . . . ? N2B Fe1 N4 O7 108.4(11) 6_565 . . . ? N2B Fe1 N4 O7 -102.2(8) . . . . ? N2A Fe1 N4 O7 82.0(10) 6_565 . . 6_565 ? N2A Fe1 N4 O7 -149.6(7) . . . 6_565 ? N3B Fe1 N4 O7 -73.9(5) . . . 6_565 ? N3B Fe1 N4 O7 -0.5(6) 6_565 . . 6_565 ? N4 Fe1 N4 O7 53.0(4) 6_565 . . 6_565 ? N5 Fe1 N4 O7 150.7(5) 6_565 . . 6_565 ? N5 Fe1 N4 O7 130.9(5) . . . 6_565 ? N3A Fe1 N4 O7 14.4(5) 6_565 . . 6_565 ? N3A Fe1 N4 O7 -86.1(6) . . . 6_565 ? N2B Fe1 N4 O7 71.4(11) 6_565 . . 6_565 ? N2B Fe1 N4 O7 -139.2(7) . . . 6_565 ? O8 O8 N5 N5 -0.006(3) 6_565 . . 6_565 ? B1 O8 N5 N5 66.6(4) . . . 6_565 ? O8 O8 N5 C31 77.8(5) 6_565 . . . ? B1 O8 N5 C31 144.5(5) . . . . ? N5 O8 N5 C31 77.8(5) 6_565 . . . ? B1 O8 N5 O8 66.7(4) . . . 6_565 ? N5 O8 N5 O8 0.006(4) 6_565 . . 6_565 ? O8 O8 N5 Fe1 -83.1(5) 6_565 . . . ? B1 O8 N5 Fe1 -16.4(8) . . . . ? N5 O8 N5 Fe1 -83.1(5) 6_565 . . . ? N2A Fe1 N5 N5 -135.4(7) 6_565 . . 6_565 ? N2A Fe1 N5 N5 -42.1(6) . . . 6_565 ? N3B Fe1 N5 N5 18.7(9) . . . 6_565 ? N3B Fe1 N5 N5 167.9(6) 6_565 . . 6_565 ? N4 Fe1 N5 N5 97.3(2) 6_565 . . 6_565 ? N4 Fe1 N5 N5 78.0(2) . . . 6_565 ? N3A Fe1 N5 N5 159.3(5) 6_565 . . 6_565 ? N3A Fe1 N5 N5 26.0(6) . . . 6_565 ? N2B Fe1 N5 N5 -127.9(5) 6_565 . . 6_565 ? N2B Fe1 N5 N5 -52.6(5) . . . 6_565 ? N2A Fe1 N5 C31 156.2(9) 6_565 . . . ? N2A Fe1 N5 C31 -110.6(8) . . . . ? N3B Fe1 N5 C31 -49.8(11) . . . . ? N3B Fe1 N5 C31 99.4(7) 6_565 . . . ? N4 Fe1 N5 C31 28.9(5) 6_565 . . . ? N4 Fe1 N5 C31 9.6(5) . . . . ? N5 Fe1 N5 C31 -68.5(5) 6_565 . . . ? N3A Fe1 N5 C31 90.9(7) 6_565 . . . ? N3A Fe1 N5 C31 -42.4(9) . . . . ? N2B Fe1 N5 C31 163.7(7) 6_565 . . . ? N2B Fe1 N5 C31 -121.0(7) . . . . ? N2A Fe1 N5 O8 -43.2(9) 6_565 . . . ? N2A Fe1 N5 O8 50.0(8) . . . . ? N3B Fe1 N5 O8 110.9(10) . . . . ? N3B Fe1 N5 O8 -99.9(8) 6_565 . . . ? N4 Fe1 N5 O8 -170.5(7) 6_565 . . . ? N4 Fe1 N5 O8 170.2(7) . . . . ? N5 Fe1 N5 O8 92.2(6) 6_565 . . . ? N3A Fe1 N5 O8 -108.5(8) 6_565 . . . ? N3A Fe1 N5 O8 118.2(8) . . . . ? N2B Fe1 N5 O8 -35.7(8) 6_565 . . . ? N2B Fe1 N5 O8 39.6(8) . . . . ? N2A Fe1 N5 O8 -84.6(8) 6_565 . . 6_565 ? N2A Fe1 N5 O8 8.6(7) . . . 6_565 ? N3B Fe1 N5 O8 69.4(11) . . . 6_565 ? N3B Fe1 N5 O8 -141.4(7) 6_565 . . 6_565 ? N4 Fe1 N5 O8 148.1(5) 6_565 . . 6_565 ? N4 Fe1 N5 O8 128.8(5) . . . 6_565 ? N5 Fe1 N5 O8 50.7(5) 6_565 . . 6_565 ? N3A Fe1 N5 O8 -150.0(6) 6_565 . . 6_565 ? N3A Fe1 N5 O8 76.7(8) . . . 6_565 ? N2B Fe1 N5 O8 -77.2(7) 6_565 . . 6_565 ? N2B Fe1 N5 O8 -1.9(7) . . . 6_565 ? N2A O5A B1 O5A -31.3(17) . . . 6_565 ? N2A O5A B1 O8 82.4(8) . . . 6_565 ? N2A O5A B1 O8 68.1(10) . . . . ? N2A O5A B1 O5B -76.3(11) . . . . ? N2A O5A B1 O5B -53.3(11) . . . 6_565 ? N2A O5A B1 C17 -172.1(8) . . . . ? O8 O8 B1 O5A 23.0(5) 6_565 . . . ? N5 O8 B1 O5A -51.6(8) . . . . ? N5 O8 B1 O5A -29.6(7) 6_565 . . . ? O8 O8 B1 O5A 158.7(5) 6_565 . . 6_565 ? N5 O8 B1 O5A 84.1(6) . . . 6_565 ? N5 O8 B1 O5A 106.1(5) 6_565 . . 6_565 ? N5 O8 B1 O8 -74.6(5) . . . 6_565 ? N5 O8 B1 O8 -52.6(4) 6_565 . . 6_565 ? O8 O8 B1 O5B 47.2(6) 6_565 . . . ? N5 O8 B1 O5B -27.4(10) . . . . ? N5 O8 B1 O5B -5.4(9) 6_565 . . . ? O8 O8 B1 O5B 148.1(5) 6_565 . . 6_565 ? N5 O8 B1 O5B 73.5(7) . . . 6_565 ? N5 O8 B1 O5B 95.5(6) 6_565 . . 6_565 ? O8 O8 B1 C17 -96.4(3) 6_565 . . . ? N5 O8 B1 C17 -171.0(5) . . . . ? N5 O8 B1 C17 -149.1(4) 6_565 . . . ? N2B O5B B1 O5A 80.8(13) . . . . ? N2B O5B B1 O5A -67.0(12) . . . 6_565 ? N2B O5B B1 O8 59.0(10) . . . 6_565 ? N2B O5B B1 O8 30.8(13) . . . . ? N2B O5B B1 O5B -78.1(10) . . . 6_565 ? N2B O5B B1 C17 174.5(9) . . . . ? N3A O6A B2 O6A 25.8(19) . . . 6_565 ? N3A O6A B2 O6B 52.4(11) . . . 6_565 ? N3A O6A B2 O6B 75.2(10) . . . . ? N3A O6A B2 O7 -69.9(10) . . . 6_565 ? N3A O6A B2 O7 -81.5(8) . . . . ? N3A O6A B2 C32 173.7(8) . . . . ? N3B O6B B2 O6A -81.7(10) . . . . ? N3B O6B B2 O6A 65.7(11) . . . 6_565 ? N3B O6B B2 O6B 77.7(9) . . . 6_565 ? N3B O6B B2 O7 -32.8(12) . . . 6_565 ? N3B O6B B2 O7 -57.7(9) . . . . ? N3B O6B B2 C32 -174.0(8) . . . . ? O7 O7 B2 O6A 160.1(4) 6_565 . . . ? N4 O7 B2 O6A 82.9(6) . . . . ? N4 O7 B2 O6A 105.4(5) 6_565 . . . ? O7 O7 B2 O6A 20.8(5) 6_565 . . 6_565 ? N4 O7 B2 O6A -56.4(8) . . . 6_565 ? N4 O7 B2 O6A -33.8(7) 6_565 . . 6_565 ? O7 O7 B2 O6B 46.2(7) 6_565 . . 6_565 ? N4 O7 B2 O6B -31.0(10) . . . 6_565 ? N4 O7 B2 O6B -8.5(10) 6_565 . . 6_565 ? O7 O7 B2 O6B 147.2(5) 6_565 . . . ? N4 O7 B2 O6B 70.0(7) . . . . ? N4 O7 B2 O6B 92.6(6) 6_565 . . . ? N4 O7 B2 O7 -77.2(5) . . . 6_565 ? N4 O7 B2 O7 -54.6(4) 6_565 . . 6_565 ? O7 O7 B2 C32 -95.4(2) 6_565 . . . ? N4 O7 B2 C32 -172.6(5) . . . . ? N4 O7 B2 C32 -150.1(4) 6_565 . . . ? Zn2 O2 C1 O1 13.8(8) . . . . ? Zn2 O2 C1 C2 -163.6(3) . . . . ? Zn1 O1 C1 O2 -8.0(7) . . . . ? Zn1 O1 C1 C2 169.4(3) . . . . ? O2 C1 C2 C7 -16.3(8) . . . . ? O1 C1 C2 C7 166.0(5) . . . . ? O2 C1 C2 C3 156.0(5) . . . . ? O1 C1 C2 C3 -21.6(8) . . . . ? C7 C2 C3 C4 -3.8(10) . . . . ? C1 C2 C3 C4 -176.4(6) . . . . ? C2 C3 C4 C5 -2.8(11) . . . . ? C3 C4 C5 C6 7.4(11) . . . . ? C3 C4 C5 C12 -174.4(6) . . . 8_455 ? C4 C5 C6 C7 -5.3(11) . . . . ? C12 C5 C6 C7 176.4(6) 8_455 . . . ? C5 C6 C7 C2 -1.4(11) . . . . ? C3 C2 C7 C6 6.0(10) . . . . ? C1 C2 C7 C6 178.5(6) . . . . ? Zn1 O4 C8 O3 10.6(9) . . . . ? Zn1 O4 C8 C9 -168.9(4) . . . . ? Zn2 O3 C8 O4 -7.0(8) . . . . ? Zn2 O3 C8 C9 172.5(3) . . . . ? O4 C8 C9 C14 4.0(8) . . . . ? O3 C8 C9 C14 -175.6(5) . . . . ? O4 C8 C9 C10 -173.7(6) . . . . ? O3 C8 C9 C10 6.8(8) . . . . ? C14 C9 C10 C11 2.1(11) . . . . ? C8 C9 C10 C11 179.8(7) . . . . ? C9 C10 C11 C12 2.2(13) . . . . ? C10 C11 C12 C13 -4.3(13) . . . . ? C10 C11 C12 C5 177.8(8) . . . 8 ? C11 C12 C13 C14 2.0(11) . . . . ? C5 C12 C13 C14 180.0(6) 8 . . . ? C12 C13 C14 C9 2.2(10) . . . . ? C10 C9 C14 C13 -4.3(10) . . . . ? C8 C9 C14 C13 178.0(6) . . . . ? C19 N1 C15 C16 0.000(2) . . . . ? Zn1 N1 C15 C16 180.000(2) . . . . ? N1 C15 C16 C17 0.000(2) . . . . ? C15 C16 C17 C18 0.000(2) . . . . ? C15 C16 C17 B1 180.000(2) . . . . ? O5A B1 C17 C16 76.3(6) . . . . ? O5A B1 C17 C16 -76.3(6) 6_565 . . . ? O8 B1 C17 C16 159.9(3) 6_565 . . . ? O8 B1 C17 C16 -159.9(3) . . . . ? O5B B1 C17 C16 45.6(4) . . . . ? O5B B1 C17 C16 -45.6(4) 6_565 . . . ? O5A B1 C17 C18 -103.7(6) . . . . ? O5A B1 C17 C18 103.7(6) 6_565 . . . ? O8 B1 C17 C18 -20.1(3) 6_565 . . . ? O8 B1 C17 C18 20.1(3) . . . . ? O5B B1 C17 C18 -134.4(4) . . . . ? O5B B1 C17 C18 134.4(4) 6_565 . . . ? C16 C17 C18 C19 0.000(2) . . . . ? B1 C17 C18 C19 180.000(2) . . . . ? C15 N1 C19 C18 0.000(2) . . . . ? Zn1 N1 C19 C18 180.000(1) . . . . ? C17 C18 C19 N1 0.000(2) . . . . ? O5B N2B C20 N2A 93(4) . . . . ? Fe1 N2B C20 N2A -70(4) . . . . ? O5B N2B C20 C25 -177.1(9) . . . . ? Fe1 N2B C20 C25 19.5(12) . . . . ? O5B N2B C20 C21 -10.6(16) . . . . ? Fe1 N2B C20 C21 -174.1(6) . . . . ? O5A N2A C20 N2B -88(4) . . . . ? Fe1 N2A C20 N2B 81(4) . . . . ? O5A N2A C20 C25 174.2(9) . . . . ? Fe1 N2A C20 C25 -17.5(12) . . . . ? O5A N2A C20 C21 4.7(17) . . . . ? Fe1 N2A C20 C21 173.0(6) . . . . ? N2B C20 C21 C22 -153.4(10) . . . . ? N2A C20 C21 C22 179.7(10) . . . . ? C25 C20 C21 C22 11.4(9) . . . . ? C20 C21 C22 C23 -41.7(9) . . . . ? C21 C22 C23 C24 64.0(8) . . . . ? C22 C23 C24 C25 -51.2(8) . . . . ? O6A N3A C25 N3B 88(2) . . . . ? Fe1 N3A C25 N3B -70(2) . . . . ? O6A N3A C25 C20 -176.6(8) . . . . ? Fe1 N3A C25 C20 24.9(10) . . . . ? O6A N3A C25 C24 -10.6(14) . . . . ? Fe1 N3A C25 C24 -169.1(6) . . . . ? O6B N3B C25 N3A -88(3) . . . . ? Fe1 N3B C25 N3A 73(2) . . . . ? O6B N3B C25 C20 176.6(8) . . . . ? Fe1 N3B C25 C20 -21.7(11) . . . . ? O6B N3B C25 C24 12.4(15) . . . . ? Fe1 N3B C25 C24 174.2(6) . . . . ? N2B C20 C25 N3A -27.7(11) . . . . ? N2A C20 C25 N3A -5.0(11) . . . . ? C21 C20 C25 N3A 165.3(7) . . . . ? N2B C20 C25 N3B 1.0(11) . . . . ? N2A C20 C25 N3B 23.7(11) . . . . ? C21 C20 C25 N3B -166.0(8) . . . . ? N2B C20 C25 C24 165.7(9) . . . . ? N2A C20 C25 C24 -171.5(9) . . . . ? C21 C20 C25 C24 -1.3(10) . . . . ? C23 C24 C25 N3A -142.9(9) . . . . ? C23 C24 C25 N3B -176.1(9) . . . . ? C23 C24 C25 C20 21.5(9) . . . . ? O7 N4 C26 N4 -89.2(5) . . . 6_565 ? O7 N4 C26 N4 -54.8(4) 6_565 . . 6_565 ? Fe1 N4 C26 N4 71.4(4) . . . 6_565 ? N4 N4 C26 C31 -94.9(2) 6_565 . . . ? O7 N4 C26 C31 175.8(5) . . . . ? O7 N4 C26 C31 -149.8(4) 6_565 . . . ? Fe1 N4 C26 C31 -23.6(5) . . . . ? N4 N4 C26 C27 100.3(3) 6_565 . . . ? O7 N4 C26 C27 11.0(7) . . . . ? O7 N4 C26 C27 45.4(6) 6_565 . . . ? Fe1 N4 C26 C27 171.7(2) . . . . ? N4 C26 C27 C28 138.9(8) . . . . ? N4 C26 C27 C28 172.9(8) 6_565 . . . ? C31 C26 C27 C28 -24.1(7) . . . . ? C26 C27 C28 C29 52.1(12) . . . . ? C27 C28 C29 C30 -59.1(13) . . . . ? C28 C29 C30 C31 32.4(9) . . . . ? O8 N5 C31 N5 -91.3(6) . . . 6_565 ? O8 N5 C31 N5 -52.9(5) 6_565 . . 6_565 ? Fe1 N5 C31 N5 70.9(4) . . . 6_565 ? N5 N5 C31 C26 -95.1(2) 6_565 . . . ? O8 N5 C31 C26 173.7(5) . . . . ? O8 N5 C31 C26 -148.0(4) 6_565 . . . ? Fe1 N5 C31 C26 -24.2(5) . . . . ? N5 N5 C31 C30 100.1(3) 6_565 . . . ? O8 N5 C31 C30 8.8(8) . . . . ? O8 N5 C31 C30 47.2(6) 6_565 . . . ? Fe1 N5 C31 C30 171.0(2) . . . . ? N4 C26 C31 N5 29.4(5) . . . . ? N4 C26 C31 N5 0.5(5) 6_565 . . . ? C27 C26 C31 N5 -165.1(3) . . . . ? N4 C26 C31 N5 -0.5(5) . . . 6_565 ? N4 C26 C31 N5 -29.4(5) 6_565 . . 6_565 ? C27 C26 C31 N5 165.1(3) . . . 6_565 ? N4 C26 C31 C30 -165.6(3) . . . . ? N4 C26 C31 C30 165.6(3) 6_565 . . . ? C27 C26 C31 C30 0.0 . . . . ? C29 C30 C31 N5 162.8(4) . . . . ? C29 C30 C31 N5 -162.8(4) . . . 6_565 ? C29 C30 C31 C26 0.0 . . . . ? O6A B2 C32 C33 32.1(16) . . . . ? O6A B2 C32 C33 -168.8(14) 6_565 . . . ? O6B B2 C32 C33 157.2(14) 6_565 . . . ? O6B B2 C32 C33 66.0(15) . . . . ? O7 B2 C32 C33 -86.0(13) 6_565 . . . ? O7 B2 C32 C33 -50.7(14) . . . . ? O6A B2 C32 C33 168.8(14) . . . 6_565 ? O6A B2 C32 C33 -32.1(16) 6_565 . . 6_565 ? O6B B2 C32 C33 -66.0(15) 6_565 . . 6_565 ? O6B B2 C32 C33 -157.2(14) . . . 6_565 ? O7 B2 C32 C33 50.7(14) 6_565 . . 6_565 ? O7 B2 C32 C33 86.0(13) . . . 6_565 ? O6A B2 C32 C36 -13.1(15) . . . 6_565 ? O6A B2 C32 C36 146.0(13) 6_565 . . 6_565 ? O6B B2 C32 C36 112.0(13) 6_565 . . 6_565 ? O6B B2 C32 C36 20.8(14) . . . 6_565 ? O7 B2 C32 C36 -131.2(13) 6_565 . . 6_565 ? O7 B2 C32 C36 -95.9(13) . . . 6_565 ? O6A B2 C32 C36 -146.0(13) . . . . ? O6A B2 C32 C36 13.1(15) 6_565 . . . ? O6B B2 C32 C36 -20.8(14) 6_565 . . . ? O6B B2 C32 C36 -112.0(13) . . . . ? O7 B2 C32 C36 95.9(13) 6_565 . . . ? O7 B2 C32 C36 131.2(13) . . . . ? C33 C32 C33 C34 38(3) 6_565 . . . ? C36 C32 C33 C34 -74(2) 6_565 . . . ? C36 C32 C33 C34 -2(3) . . . . ? B2 C32 C33 C34 179.7(16) . . . . ? C32 C33 C34 N6 -2(3) . . . . ? C33 C34 N6 N6 0.00(11) . . . 6_565 ? C33 C34 N6 C35 4(3) . . . . ? C33 C34 N6 C35 83(2) . . . 6_565 ? C33 C34 N6 C34 -33(3) . . . 6_565 ? C33 C34 N6 Zn2 -173.5(15) . . . 1_554 ? N6 N6 C35 C36 0.00(14) 6_565 . . . ? C35 N6 C35 C36 -38(3) 6_565 . . . ? C34 N6 C35 C36 76.7(19) 6_565 . . . ? C34 N6 C35 C36 -1(3) . . . . ? Zn2 N6 C35 C36 176.2(16) 1_554 . . . ? N6 C35 C36 C32 -3(3) . . . . ? C33 C32 C36 C35 5(3) . . . . ? C33 C32 C36 C35 -79(2) 6_565 . . . ? C36 C32 C36 C35 41(3) 6_565 . . . ? B2 C32 C36 C35 -177.2(15) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.706 _refine_diff_density_min -2.815 _refine_diff_density_rms 0.119 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.350 -0.024 0.073 4548 817 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL MDW3-81b in C2/m CELL 0.71073 24.1663 18.5195 21.8052 90.000 105.600 90.000 ZERR 4.00 0.0035 0.0035 0.0034 0.000 0.018 0.000 LATT 7 SYMM -X, Y, -Z SFAC C H B N O FE ZN UNIT 224 192 8 32 56 4 8 REM ---------------------------------------------------------- REM Data collection: Bruker Nonius APEX II CCD REM Absorption correction: SADABS REM Crystal habit: prismatic; Crystal colour: red REM Solvent has been completely SQUEEZED REM ---------------------------------------------------------- L.S. 10 FMAP 2 ACTA CONF SIZE 0.407 0.329 0.232 WPDB -2 BOND $H PLAN 10 EQIV $2 X, 1-Y, Z FREE C33 C36_$2 FREE C33 C35_$2 FREE C34 C35_$2 FREE C34 C36_$2 FREE C35 C34_$2 FREE C35 C33_$2 FREE C36 C33_$2 FREE C36 C34_$2 FREE C27 C28_$2 FREE C28 C28_$2 FREE C29 C28_$2 FREE C34 N6_$2 FREE C35 N6_$2 TEMP -173 WGHT 0.109400 87.088806 FVAR 2.78321 ZN1 7 0.672795 0.500000 0.639312 10.50000 0.01738 0.02100 = 0.02288 0.00000 0.01157 0.00000 ZN2 7 0.706880 0.500000 0.781424 10.50000 0.01982 0.02308 = 0.02294 0.00000 0.01438 0.00000 FE1 6 0.692605 0.500000 0.211213 10.50000 0.03430 0.03545 = 0.02118 0.00000 0.01528 0.00000 O1 5 0.613305 0.425511 0.647064 11.00000 0.03946 0.05448 = 0.03987 0.01340 0.01195 -0.02141 O2 5 0.642748 0.423993 0.753205 11.00000 0.03341 0.03876 = 0.03600 -0.00910 0.02085 -0.01656 O3 5 0.765354 0.424222 0.773406 11.00000 0.03245 0.04945 = 0.04389 -0.00536 0.01156 0.01918 O4 5 0.736675 0.424527 0.666840 11.00000 0.03987 0.05329 = 0.04773 0.01181 0.02492 0.02313 PART 1 O5A 5 0.697549 0.429380 0.331969 10.50000 0.03936 0.04402 = 0.02080 0.00258 0.01601 -0.00315 O6A 5 0.713112 0.425160 0.100207 10.50000 0.04694 0.04175 = 0.02698 -0.00390 0.02200 -0.00066 PART 2 O5B 5 0.728095 0.443284 0.340950 10.50000 0.04555 0.01983 = 0.03122 0.00541 0.02146 0.00004 O6B 5 0.744491 0.445404 0.113862 10.50000 0.04635 0.03276 = 0.03913 -0.00577 0.03054 0.00036 PART 0 O7 5 0.642551 0.476129 0.075843 10.50000 0.04098 0.03932 = 0.00808 -0.01065 0.01375 -0.00785 O8 5 0.625688 0.526989 0.302752 10.50000 0.03939 0.04511 = 0.01696 0.00184 0.01729 0.00367 N1 4 0.671091 0.500000 0.544620 10.50000 0.02452 0.03031 = 0.02414 0.00000 0.01272 0.00000 PART 1 N2A 4 0.710211 0.428031 0.272362 10.50000 0.03127 0.04118 = 0.02767 0.00716 0.01373 0.00429 N3A 4 0.716635 0.420848 0.167195 10.50000 0.04824 0.03469 = 0.03095 0.00364 0.02093 -0.01003 PART 2 N2B 4 0.731531 0.434909 0.279981 10.50000 0.04522 0.02986 = 0.01239 0.00232 0.01326 0.02119 N3B 4 0.738715 0.437946 0.175501 10.50000 0.04483 0.02034 = 0.03707 0.01113 0.03316 0.00577 PART 0 N4 4 0.632778 0.482936 0.135235 10.50000 0.04324 0.02862 = 0.01075 -0.00424 0.01515 -0.00579 N5 4 0.625030 0.517587 0.239459 10.50000 0.03883 0.03587 = 0.01804 0.00179 0.01844 0.00407 B1 3 0.682592 0.500000 0.345700 10.50000 0.02691 0.06117 = 0.02289 0.00000 0.00677 0.00000 B2 3 0.703213 0.500000 0.076713 10.50000 0.06011 0.03751 = 0.02256 0.00000 0.02408 0.00000 C1 1 0.608874 0.406389 0.701142 11.00000 0.02674 0.02075 = 0.03943 0.00342 0.01706 -0.00034 C2 1 0.557692 0.361472 0.703369 11.00000 0.03137 0.03307 = 0.03672 -0.00175 0.01861 -0.01230 C3 1 0.508366 0.361929 0.652471 11.00000 0.05586 0.05925 = 0.03802 0.00629 0.01702 -0.02236 AFIX 43 H3 2 0.508004 0.388685 0.615193 11.00000 -1.20000 AFIX 0 C4 1 0.459956 0.323943 0.655540 11.00000 0.05128 0.05787 = 0.04021 0.00126 0.01083 -0.02870 AFIX 43 H4 2 0.426020 0.326381 0.621310 11.00000 -1.20000 AFIX 0 C5 1 0.461025 0.281639 0.709468 11.00000 0.04152 0.05642 = 0.04061 0.00679 0.01604 -0.02935 C6 1 0.508044 0.285580 0.760970 11.00000 0.04090 0.05985 = 0.03982 0.00266 0.01747 -0.01948 AFIX 43 H6 2 0.507936 0.260495 0.798941 11.00000 -1.20000 AFIX 0 C7 1 0.555505 0.325383 0.758542 11.00000 0.03848 0.06978 = 0.03467 0.00683 0.01189 -0.02277 AFIX 43 H7 2 0.587314 0.328234 0.795213 11.00000 -1.20000 AFIX 0 C8 1 0.769304 0.405623 0.719045 11.00000 0.02535 0.02907 = 0.04527 0.00509 0.01716 0.00450 C9 1 0.818535 0.356137 0.716926 11.00000 0.02540 0.03662 = 0.04368 -0.00107 0.01445 0.01114 C10 1 0.854192 0.326266 0.773584 11.00000 0.05061 0.08333 = 0.04425 -0.00596 0.01508 0.04244 AFIX 43 H10 2 0.847707 0.337039 0.813681 11.00000 -1.20000 AFIX 0 C11 1 0.898665 0.281089 0.769534 11.00000 0.06976 0.09636 = 0.04536 0.00233 0.01042 0.06408 AFIX 43 H11 2 0.921575 0.259835 0.807575 11.00000 -1.20000 AFIX 0 C12 1 0.911661 0.265046 0.711822 11.00000 0.03648 0.05350 = 0.03854 -0.00112 0.01271 0.02385 C13 1 0.874018 0.293781 0.655961 11.00000 0.04430 0.06506 = 0.03634 0.00175 0.02052 0.02793 AFIX 43 H13 2 0.880482 0.282973 0.615860 11.00000 -1.20000 AFIX 0 C14 1 0.827983 0.337255 0.658148 11.00000 0.03861 0.04914 = 0.04169 0.01801 0.02030 0.02506 AFIX 43 H14 2 0.802646 0.354412 0.619705 11.00000 -1.20000 AFIX 0 C15 1 0.721973 0.500000 0.531544 10.50000 0.02435 0.14565 = 0.02390 0.00000 0.01204 0.00000 AFIX 43 H15 2 0.756152 0.500000 0.565542 10.50000 -1.20000 AFIX 0 C16 1 0.725870 0.500000 0.468897 10.50000 0.03358 0.14645 = 0.02823 0.00000 0.02155 0.00000 AFIX 43 H16 2 0.762679 0.500000 0.461044 10.50000 -1.20000 AFIX 0 C17 1 0.677536 0.500000 0.418264 10.50000 0.03989 0.05224 = 0.02899 0.00000 0.01593 0.00000 C18 1 0.625495 0.500000 0.433528 10.50000 0.04069 0.12282 = 0.02229 0.00000 0.01327 0.00000 AFIX 43 H18 2 0.590577 0.500000 0.400565 10.50000 -1.20000 AFIX 0 C19 1 0.624088 0.500000 0.497104 10.50000 0.04000 0.08340 = 0.03389 0.00000 0.01993 0.00000 AFIX 43 H19 2 0.587872 0.500000 0.506401 10.50000 -1.20000 AFIX 0 C20 1 0.748497 0.374062 0.265783 11.00000 0.05163 0.02086 = 0.03935 0.00086 0.01588 0.00117 C21 1 0.774047 0.315183 0.311923 11.00000 0.07668 0.03186 = 0.04679 0.00977 0.00544 0.01224 AFIX 23 H21A 2 0.742596 0.285956 0.320383 11.00000 -1.20000 H21B 2 0.795655 0.337275 0.352675 11.00000 -1.20000 AFIX 0 C22 1 0.813641 0.266227 0.288437 11.00000 0.07533 0.04498 = 0.08689 0.01972 0.02060 0.03230 AFIX 23 H22A 2 0.819530 0.221020 0.313594 11.00000 -1.20000 H22B 2 0.851453 0.290029 0.294860 11.00000 -1.20000 AFIX 0 C23 1 0.788824 0.247748 0.216522 11.00000 0.08045 0.03145 = 0.07774 0.01146 0.04754 0.02211 AFIX 23 H23A 2 0.814123 0.212248 0.203495 11.00000 -1.20000 H23B 2 0.750325 0.225687 0.209666 11.00000 -1.20000 AFIX 0 C24 1 0.784172 0.316876 0.175098 11.00000 0.08735 0.03553 = 0.06568 0.01471 0.05168 0.02483 AFIX 23 H24A 2 0.823086 0.334147 0.175711 11.00000 -1.20000 H24B 2 0.763229 0.305789 0.130478 11.00000 -1.20000 AFIX 0 C25 1 0.752715 0.374644 0.200907 11.00000 0.05841 0.03111 = 0.05270 0.00833 0.03417 0.01332 C26 1 0.578703 0.500000 0.135656 10.50000 0.03233 0.09152 = 0.02396 0.00000 0.01523 0.00000 C27 1 0.526921 0.500000 0.079606 10.50000 0.03765 0.16027 = 0.02425 0.00000 0.01678 0.00000 AFIX 23 H27A 2 0.534315 0.470710 0.044658 10.50000 -1.20000 H27B 2 0.517633 0.549900 0.063920 10.50000 -1.20000 AFIX 0 C28 1 0.472868 0.465300 0.102891 10.50000 0.02273 0.18084 = 0.02335 -0.01211 0.00417 -0.00752 AFIX 23 H28A 2 0.436886 0.470283 0.068331 10.50000 -1.20000 H28B 2 0.479829 0.413220 0.112013 10.50000 -1.20000 AFIX 0 C29 1 0.467067 0.500000 0.156603 10.50000 0.02521 0.34515 = 0.03525 0.00000 0.00971 0.00000 AFIX 23 H29A 2 0.433622 0.478450 0.167891 10.50000 -1.20000 H29B 2 0.457221 0.550990 0.144987 10.50000 -1.20000 AFIX 0 C30 1 0.517450 0.500000 0.216873 10.50000 0.02768 0.09061 = 0.03692 0.00000 0.01509 0.00000 AFIX 23 H30A 2 0.515133 0.543276 0.242721 10.50000 -1.20000 H30B 2 0.515133 0.456724 0.242721 10.50000 -1.20000 AFIX 0 C31 1 0.574131 0.500000 0.199635 10.50000 0.03038 0.06361 = 0.02105 0.00000 0.01347 0.00000 C32 1 0.707173 0.500000 0.003953 10.50000 0.03492 0.05631 = 0.01947 0.00000 0.01553 0.00000 C33 1 0.690488 0.441748 -0.033228 10.50000 0.12157 0.09899 = 0.02126 -0.00762 0.03449 -0.05326 AFIX 43 H33 2 0.676545 0.400675 -0.015942 10.50000 -1.20000 AFIX 0 C34 1 0.692986 0.439707 -0.096081 10.50000 0.09791 0.04544 = 0.02485 -0.00996 0.03872 -0.01661 AFIX 43 H34 2 0.682082 0.396882 -0.120300 10.50000 -1.20000 AFIX 0 N6 4 0.711393 0.500000 -0.124424 10.50000 0.02538 0.04418 = 0.02272 0.00000 0.01796 0.00000 C35 1 0.729053 0.555797 -0.088753 10.50000 0.08364 0.08892 = 0.03798 -0.01495 0.04138 -0.05152 AFIX 43 H35 2 0.742308 0.596512 -0.107211 10.50000 -1.20000 AFIX 0 C36 1 0.729666 0.559374 -0.023966 10.50000 0.12694 0.06466 = 0.02632 -0.02290 0.03840 -0.04529 AFIX 43 H36 2 0.744790 0.600597 0.000832 10.50000 -1.20000 HKLF 4 1 -1 -1 0 1 -1 0 0 0 1 REM MDW3-81b in C2/m REM R1 = 0.0954 for 8426 Fo > 4sig(Fo) and 0.1093 for all 10528 data REM 478 parameters refined using 0 restraints END WGHT 0.1094 87.1146 REM Highest difference peak 1.706, deepest hole -2.815, 1-sigma level 0.119 Q1 1 0.6902 0.5528 0.2114 11.00000 0.05 1.71 Q2 1 0.7119 0.5563 0.7890 11.00000 0.05 1.68 Q3 1 0.6771 0.5602 0.6475 11.00000 0.05 1.61 Q4 1 0.5665 0.5000 0.5195 10.50000 0.05 1.51 Q5 1 0.5360 0.5000 0.3789 10.50000 0.05 1.00 Q6 1 0.6760 0.5207 0.7580 11.00000 0.05 0.99 Q7 1 0.7072 0.5000 -0.1700 10.50000 0.05 0.78 Q8 1 0.5284 0.3095 0.6510 11.00000 0.05 0.76 Q9 1 0.6769 0.5000 0.1647 10.50000 0.05 0.67 Q10 1 0.4876 0.2685 0.6508 11.00000 0.05 0.67 ;