# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Richard Winpenny' _publ_contact_author_address ; Department of Chemistry University of Manchester Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email RICHARD.WINPENNY@MANCHESTER.AC.UK _publ_section_title ; A Family of Heterometallic Wheels Containing Potentially Fourteen Hundred Siblings ; loop_ _publ_author_name 'Richard Winpenny' 'H. Gudel' 'F. K. Larsen' 'Rebecca H. Laye' 'E. McInnes' 'Chris Muryn' ; J.Overgaard ; 'Eva Rentschler' 'Veronica Sanchez' 'S. J. Teat' 'Grigore A. Timco' 'Oliver Waldmann' data_04gt95e_0m _database_code_depnum_ccdc_archive 'CCDC 257789' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H160 F8 Fe7 Mn N O32' _chemical_formula_weight 2318.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.301(11) _cell_length_b 16.334(7) _cell_length_c 30.568(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.180(19) _cell_angle_gamma 90.00 _cell_volume 11857(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9703 _cell_measurement_theta_min 2.417 _cell_measurement_theta_max 21.54 _exptl_crystal_description block _exptl_crystal_colour 'reddish brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4872 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _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 ApexII CCD-based diffractometer' _diffrn_measurement_method '\f and \o scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16739 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 23.26 _reflns_number_total 16739 _reflns_number_gt 10724 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.2000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16739 _refine_ls_number_parameters 587 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.2470 _refine_ls_R_factor_gt 0.1929 _refine_ls_wR_factor_ref 0.5698 _refine_ls_wR_factor_gt 0.5413 _refine_ls_goodness_of_fit_ref 2.328 _refine_ls_restrained_S_all 2.317 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.008 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 Mn1 Mn 0.3375(2) 0.4764(2) 0.75547(12) 0.1503(18) Uani 1 1 d . . . Fe1 Fe 0.26789(9) 0.65180(13) 0.76136(7) 0.0683(7) Uani 1 1 d . . . Fe2 Fe 0.17310(8) 0.70701(12) 0.81237(6) 0.0632(6) Uani 1 1 d . . . Fe3 Fe 0.15084(9) 0.63627(15) 0.90968(7) 0.0781(7) Uani 1 1 d . . . Fe4 Fe 0.16144(10) 0.44885(19) 0.96175(10) 0.1121(11) Uani 1 1 d . . . Fe5 Fe 0.25182(11) 0.28786(18) 0.97491(12) 0.1224(13) Uani 1 1 d . . . Fe6 Fe 0.32550(11) 0.21647(18) 0.90731(14) 0.1340(14) Uani 1 1 d . . . Fe7 Fe 0.37430(16) 0.3097(2) 0.82591(12) 0.1385(14) Uani 1 1 d . . . O11 O 0.1912(4) 0.6377(6) 0.7176(4) 0.078(3) Uiso 1 1 d . . . O12 O 0.1306(4) 0.6464(6) 0.7549(3) 0.072(3) Uiso 1 1 d . . . O13 O 0.2643(4) 0.7699(6) 0.7589(4) 0.083(3) Uiso 1 1 d . . . O14 O 0.1848(4) 0.7973(6) 0.7738(3) 0.074(3) Uiso 1 1 d . . . O21 O 0.2192(4) 0.7679(5) 0.8675(3) 0.068(2) Uiso 1 1 d . . . O22 O 0.2207(4) 0.6996(6) 0.9311(3) 0.077(3) Uiso 1 1 d . . . O23 O 0.1027(4) 0.7569(6) 0.8136(4) 0.082(3) Uiso 1 1 d . . . O24 O 0.1064(4) 0.7342(6) 0.8849(4) 0.083(3) Uiso 1 1 d . . . O31 O 0.0794(4) 0.5733(6) 0.8838(4) 0.081(3) Uiso 1 1 d . . . O32 O 0.0964(5) 0.4453(7) 0.9024(4) 0.098(3) Uiso 1 1 d . . . O33 O 0.1389(5) 0.6551(7) 0.9690(4) 0.100(3) Uiso 1 1 d . . . O34 O 0.1207(5) 0.5354(8) 0.9874(4) 0.101(3) Uiso 1 1 d . . . O41 O 0.2284(6) 0.4658(7) 1.0198(4) 0.102(4) Uiso 1 1 d . . . O42 O 0.2920(5) 0.3797(7) 1.0208(4) 0.094(3) Uiso 1 1 d . . . O43 O 0.1302(7) 0.3546(9) 0.9841(6) 0.131(5) Uiso 1 1 d . . . O44 O 0.1965(6) 0.2730(8) 1.0105(5) 0.111(4) Uiso 1 1 d . . . O51 O 0.2046(6) 0.2061(8) 0.9294(5) 0.108(4) Uiso 1 1 d . . . O52 O 0.2440(7) 0.1810(10) 0.8775(5) 0.130(5) Uiso 1 1 d . . . O53 O 0.3066(6) 0.2080(9) 1.0156(5) 0.127(5) Uiso 1 1 d . . . O54 O 0.3405(6) 0.1477(8) 0.9655(5) 0.120(4) Uiso 1 1 d . . . O61 O 0.4061(6) 0.2545(9) 0.9352(5) 0.116(4) Uiso 1 1 d . . . O62 O 0.4257(6) 0.3410(9) 0.8869(5) 0.120(4) Uiso 1 1 d . . . O63 O 0.3540(10) 0.1277(12) 0.8788(8) 0.183(8) Uiso 1 1 d . . . O64 O 0.4046(10) 0.1968(13) 0.8366(8) 0.190(8) Uiso 1 1 d . . . O71 O 0.3253(9) 0.2801(12) 0.7655(8) 0.181(7) Uiso 1 1 d . . . O72 O 0.2898(8) 0.3911(12) 0.7245(6) 0.155(6) Uiso 1 1 d . . . O73 O 0.4354(8) 0.3332(11) 0.8023(7) 0.160(6) Uiso 1 1 d . . . O74 O 0.4011(10) 0.4219(14) 0.7457(8) 0.198(8) Uiso 1 1 d . . . O81 O 0.3469(5) 0.6609(7) 0.8066(4) 0.093(3) Uiso 1 1 d . . . O82 O 0.3887(6) 0.5551(9) 0.7856(5) 0.125(4) Uiso 1 1 d . . . O83 O 0.3134(8) 0.5261(12) 0.6945(7) 0.164(6) Uiso 1 1 d . . . O84 O 0.2948(5) 0.6540(7) 0.7085(4) 0.089(3) Uiso 1 1 d . . . F1 F 0.2418(3) 0.6506(4) 0.8135(2) 0.0618(18) Uiso 1 1 d . . . F2 F 0.1639(3) 0.6170(4) 0.8507(3) 0.0676(19) Uiso 1 1 d . . . F3 F 0.1929(4) 0.5369(5) 0.9333(3) 0.080(2) Uiso 1 1 d . . . F4 F 0.2022(5) 0.3750(6) 0.9363(4) 0.108(3) Uiso 1 1 d . . . F5 F 0.2994(4) 0.3094(6) 0.9381(3) 0.092(3) Uiso 1 1 d . . . F6 F 0.3139(4) 0.2870(6) 0.8538(4) 0.104(3) Uiso 1 1 d . . . F7 F 0.3497(4) 0.4212(6) 0.8149(3) 0.100(3) Uiso 1 1 d . . . F8 F 0.2749(4) 0.5323(5) 0.7660(3) 0.081(2) Uiso 1 1 d . . . C11 C 0.1415(5) 0.6316(8) 0.7204(4) 0.072(4) Uiso 1 1 d D . . C12 C 0.0952(4) 0.6130(6) 0.6745(4) 0.085(4) Uiso 1 1 d D . . C13 C 0.0395(5) 0.6036(12) 0.6826(6) 0.150(9) Uiso 1 1 d D . . H13A H 0.0097 0.5909 0.6530 0.225 Uiso 1 1 calc R . . H13B H 0.0305 0.6548 0.6952 0.225 Uiso 1 1 calc R . . H13C H 0.0425 0.5591 0.7048 0.225 Uiso 1 1 calc R . . C14 C 0.1089(8) 0.5340(9) 0.6544(6) 0.216(15) Uiso 1 1 d D . . H14A H 0.0785 0.5213 0.6251 0.324 Uiso 1 1 calc R . . H14B H 0.1125 0.4893 0.6767 0.324 Uiso 1 1 calc R . . H14C H 0.1444 0.5405 0.6486 0.324 Uiso 1 1 calc R . . C15 C 0.0908(8) 0.6827(10) 0.6406(5) 0.149(9) Uiso 1 1 d D . . H15A H 0.0606 0.6709 0.6110 0.223 Uiso 1 1 calc R . . H15B H 0.1266 0.6883 0.6351 0.223 Uiso 1 1 calc R . . H15C H 0.0824 0.7337 0.6537 0.223 Uiso 1 1 calc R . . C16 C 0.2238(6) 0.8176(6) 0.7591(4) 0.072(4) Uiso 1 1 d D . . C17 C 0.2273(4) 0.9074(6) 0.7482(3) 0.101(5) Uiso 1 1 d D . . C18 C 0.1688(5) 0.9395(10) 0.7210(6) 0.146(9) Uiso 1 1 d D . . H18A H 0.1712 0.9975 0.7136 0.219 Uiso 1 1 calc R . . H18B H 0.1446 0.9335 0.7399 0.219 Uiso 1 1 calc R . . H18C H 0.1529 0.9083 0.6921 0.219 Uiso 1 1 calc R . . C19 C 0.2517(7) 0.9552(8) 0.7933(5) 0.143(8) Uiso 1 1 d D . . H19A H 0.2546 1.0132 0.7862 0.215 Uiso 1 1 calc R . . H19B H 0.2893 0.9340 0.8111 0.215 Uiso 1 1 calc R . . H19C H 0.2271 0.9493 0.8118 0.215 Uiso 1 1 calc R . . C20 C 0.2651(6) 0.9177(9) 0.7192(5) 0.105(6) Uiso 1 1 d D . . H20A H 0.2675 0.9758 0.7122 0.158 Uiso 1 1 calc R . . H20B H 0.2493 0.8870 0.6900 0.158 Uiso 1 1 calc R . . H20C H 0.3028 0.8969 0.7367 0.158 Uiso 1 1 calc R . . C21 C 0.2371(5) 0.7577(8) 0.9117(4) 0.075(4) Uiso 1 1 d D . . C22 C 0.2808(4) 0.8196(6) 0.9385(4) 0.110(6) Uiso 1 1 d D . . C23 C 0.3027(6) 0.7971(10) 0.9898(4) 0.111(6) Uiso 1 1 d D . . H23A H 0.3312 0.8370 1.0071 0.166 Uiso 1 1 calc R . . H23B H 0.3195 0.7423 0.9937 0.166 Uiso 1 1 calc R . . H23C H 0.2715 0.7974 1.0019 0.166 Uiso 1 1 calc R . . C24 C 0.2545(8) 0.9043(7) 0.9325(7) 0.219(15) Uiso 1 1 d D . . H24A H 0.2829 0.9444 0.9497 0.329 Uiso 1 1 calc R . . H24B H 0.2233 0.9044 0.9446 0.329 Uiso 1 1 calc R . . H24C H 0.2402 0.9188 0.8993 0.329 Uiso 1 1 calc R . . C25 C 0.3294(6) 0.8197(12) 0.9200(6) 0.135(8) Uiso 1 1 d D . . H25A H 0.3577 0.8597 0.9373 0.202 Uiso 1 1 calc R . . H25B H 0.3154 0.8343 0.8868 0.202 Uiso 1 1 calc R . . H25C H 0.3464 0.7651 0.9238 0.202 Uiso 1 1 calc R . . C26 C 0.0841(6) 0.7674(8) 0.8454(5) 0.079(4) Uiso 1 1 d D . . C27 C 0.0357(5) 0.8244(8) 0.8423(5) 0.116(6) Uiso 1 1 d D . . C28 C 0.0288(9) 0.8866(11) 0.8038(6) 0.154(9) Uiso 1 1 d D . . H28A H -0.0024 0.9237 0.8020 0.231 Uiso 1 1 calc R . . H28B H 0.0206 0.8580 0.7740 0.231 Uiso 1 1 calc R . . H28C H 0.0636 0.9181 0.8106 0.231 Uiso 1 1 calc R . . C29 C -0.0182(6) 0.7750(14) 0.8316(11) 0.33(3) Uiso 1 1 d D . . H29A H -0.0494 0.8117 0.8301 0.493 Uiso 1 1 calc R . . H29B H -0.0135 0.7342 0.8562 0.493 Uiso 1 1 calc R . . H29C H -0.0264 0.7471 0.8016 0.493 Uiso 1 1 calc R . . C30 C 0.0479(10) 0.8687(13) 0.8884(6) 0.201(14) Uiso 1 1 d D . . H30A H 0.0164 0.9052 0.8865 0.302 Uiso 1 1 calc R . . H30B H 0.0824 0.9010 0.8952 0.302 Uiso 1 1 calc R . . H30C H 0.0527 0.8286 0.9133 0.302 Uiso 1 1 calc R . . C31 C 0.0665(4) 0.5046(8) 0.8794(4) 0.082(4) Uiso 1 1 d D . . C32 C 0.0075(4) 0.4858(5) 0.8466(3) 0.097(5) Uiso 1 1 d D . . C33 C -0.0013(7) 0.3937(6) 0.8431(5) 0.129(7) Uiso 1 1 d D . . H33A H -0.0395 0.3816 0.8220 0.194 Uiso 1 1 calc R . . H33B H 0.0039 0.3714 0.8741 0.194 Uiso 1 1 calc R . . H33C H 0.0261 0.3687 0.8310 0.194 Uiso 1 1 calc R . . C34 C -0.0002(6) 0.5203(8) 0.7986(3) 0.091(5) Uiso 1 1 d D . . H34A H -0.0385 0.5084 0.7774 0.136 Uiso 1 1 calc R . . H34B H 0.0271 0.4951 0.7866 0.136 Uiso 1 1 calc R . . H34C H 0.0056 0.5797 0.8009 0.136 Uiso 1 1 calc R . . C35 C -0.0352(5) 0.5246(9) 0.8651(5) 0.109(6) Uiso 1 1 d D . . H35A H -0.0733 0.5125 0.8438 0.164 Uiso 1 1 calc R . . H35B H -0.0295 0.5840 0.8673 0.164 Uiso 1 1 calc R . . H35C H -0.0302 0.5024 0.8960 0.164 Uiso 1 1 calc R . . C36 C 0.1227(7) 0.6040(11) 0.9930(6) 0.100(5) Uiso 1 1 d D . . C37 C 0.0988(7) 0.6397(10) 1.0279(6) 0.166(10) Uiso 1 1 d D . . C38 C 0.0931(13) 0.7319(10) 1.0216(10) 0.211(14) Uiso 1 1 d D . . H38A H 0.0788 0.7551 1.0449 0.317 Uiso 1 1 calc R . . H38B H 0.0669 0.7443 0.9903 0.317 Uiso 1 1 calc R . . H38C H 0.1300 0.7557 1.0255 0.317 Uiso 1 1 calc R . . C39 C 0.1380(13) 0.6204(19) 1.0770(5) 0.28(2) Uiso 1 1 d D . . H39A H 0.1234 0.6457 1.0997 0.416 Uiso 1 1 calc R . . H39B H 0.1756 0.6421 1.0815 0.416 Uiso 1 1 calc R . . H39C H 0.1402 0.5609 1.0816 0.416 Uiso 1 1 calc R . . C40 C 0.0413(9) 0.6025(18) 1.0204(12) 0.32(3) Uiso 1 1 d D . . H40A H 0.0255 0.6262 1.0427 0.473 Uiso 1 1 calc R . . H40B H 0.0450 0.5431 1.0250 0.473 Uiso 1 1 calc R . . H40C H 0.0161 0.6142 0.9885 0.473 Uiso 1 1 calc R . . C41 C 0.2781(7) 0.4386(11) 1.0344(5) 0.108(6) Uiso 1 1 d D . . C42 C 0.3166(6) 0.4815(8) 1.0777(5) 0.128(7) Uiso 1 1 d D . . C43 C 0.3146(11) 0.5733(8) 1.0692(9) 0.257(19) Uiso 1 1 d D . . H43A H 0.3392 0.6010 1.0972 0.385 Uiso 1 1 calc R . . H43B H 0.2758 0.5929 1.0618 0.385 Uiso 1 1 calc R . . H43C H 0.3273 0.5851 1.0430 0.385 Uiso 1 1 calc R . . C44 C 0.3765(6) 0.4510(15) 1.0887(8) 0.189(12) Uiso 1 1 d D . . H44A H 0.4017 0.4810 1.1156 0.284 Uiso 1 1 calc R . . H44B H 0.3882 0.4600 1.0617 0.284 Uiso 1 1 calc R . . H44C H 0.3782 0.3924 1.0960 0.284 Uiso 1 1 calc R . . C45 C 0.2972(10) 0.4632(16) 1.1185(6) 0.190(12) Uiso 1 1 d D . . H45A H 0.3205 0.4937 1.1459 0.285 Uiso 1 1 calc R . . H45B H 0.3007 0.4044 1.1252 0.285 Uiso 1 1 calc R . . H45C H 0.2577 0.4797 1.1105 0.285 Uiso 1 1 calc R . . C46 C 0.1511(7) 0.2962(10) 1.0065(6) 0.104(6) Uiso 1 1 d D . . C47 C 0.1111(5) 0.2426(7) 1.0209(4) 0.121(7) Uiso 1 1 d D . . C48 C 0.0601(7) 0.2222(13) 0.9783(6) 0.186(12) Uiso 1 1 d D . . H48A H 0.0342 0.1874 0.9876 0.279 Uiso 1 1 calc R . . H48B H 0.0724 0.1932 0.9554 0.279 Uiso 1 1 calc R . . H48C H 0.0409 0.2730 0.9645 0.279 Uiso 1 1 calc R . . C49 C 0.0921(9) 0.2877(12) 1.0563(6) 0.151(9) Uiso 1 1 d D . . H49A H 0.0659 0.2533 1.0654 0.226 Uiso 1 1 calc R . . H49B H 0.0732 0.3387 1.0425 0.226 Uiso 1 1 calc R . . H49C H 0.1249 0.3004 1.0839 0.226 Uiso 1 1 calc R . . C50 C 0.1408(9) 0.1639(9) 1.0424(8) 0.178(11) Uiso 1 1 d D . . H50A H 0.1148 0.1289 1.0513 0.268 Uiso 1 1 calc R . . H50B H 0.1735 0.1770 1.0700 0.268 Uiso 1 1 calc R . . H50C H 0.1535 0.1352 1.0196 0.268 Uiso 1 1 calc R . . C51 C 0.2086(5) 0.1793(9) 0.8959(5) 0.078(4) Uiso 1 1 d D . . C52 C 0.1521(6) 0.1416(7) 0.8684(6) 0.182(12) Uiso 1 1 d D . . C53 C 0.1087(6) 0.2090(11) 0.8499(7) 0.117(6) Uiso 1 1 d D . . H53A H 0.0731 0.1850 0.8298 0.176 Uiso 1 1 calc R . . H53B H 0.1223 0.2480 0.8318 0.176 Uiso 1 1 calc R . . H53C H 0.1028 0.2374 0.8760 0.176 Uiso 1 1 calc R . . C54 C 0.1335(9) 0.0854(15) 0.9000(11) 0.28(2) Uiso 1 1 d D . . H54A H 0.0980 0.0587 0.8818 0.414 Uiso 1 1 calc R . . H54B H 0.1282 0.1175 0.9252 0.414 Uiso 1 1 calc R . . H54C H 0.1624 0.0436 0.9132 0.414 Uiso 1 1 calc R . . C55 C 0.1574(11) 0.0926(18) 0.8279(9) 0.47(5) Uiso 1 1 d D . . H55A H 0.1206 0.0699 0.8095 0.698 Uiso 1 1 calc R . . H55B H 0.1844 0.0479 0.8399 0.698 Uiso 1 1 calc R . . H55C H 0.1707 0.1285 0.8081 0.698 Uiso 1 1 calc R . . C56 C 0.3338(7) 0.1641(9) 1.0015(5) 0.097(5) Uiso 1 1 d D . . C57 C 0.3635(5) 0.1165(8) 1.0457(4) 0.125(7) Uiso 1 1 d D . . C58 C 0.3368(10) 0.1365(16) 1.0820(6) 0.33(3) Uiso 1 1 d D . . H58A H 0.3566 0.1069 1.1109 0.502 Uiso 1 1 calc R . . H58B H 0.2971 0.1200 1.0704 0.502 Uiso 1 1 calc R . . H58C H 0.3394 0.1955 1.0881 0.502 Uiso 1 1 calc R . . C59 C 0.4253(6) 0.1399(12) 1.0643(7) 0.154(9) Uiso 1 1 d D . . H59A H 0.4446 0.1088 1.0928 0.231 Uiso 1 1 calc R . . H59B H 0.4289 0.1986 1.0714 0.231 Uiso 1 1 calc R . . H59C H 0.4425 0.1276 1.0408 0.231 Uiso 1 1 calc R . . C60 C 0.3580(9) 0.0253(8) 1.0353(8) 0.172(11) Uiso 1 1 d D . . H60A H 0.3783 -0.0054 1.0637 0.258 Uiso 1 1 calc R . . H60B H 0.3739 0.0127 1.0111 0.258 Uiso 1 1 calc R . . H60C H 0.3181 0.0098 1.0244 0.258 Uiso 1 1 calc R . . C61 C 0.4374(7) 0.3043(11) 0.9232(6) 0.111(6) Uiso 1 1 d D . . C62 C 0.4938(6) 0.3230(10) 0.9602(5) 0.135(8) Uiso 1 1 d D . . C63 C 0.5357(8) 0.3474(19) 0.9371(10) 0.250(19) Uiso 1 1 d D . . H63A H 0.5725 0.3577 0.9610 0.375 Uiso 1 1 calc R . . H63B H 0.5226 0.3972 0.9186 0.375 Uiso 1 1 calc R . . H63C H 0.5392 0.3031 0.9166 0.375 Uiso 1 1 calc R . . C64 C 0.4870(12) 0.3928(16) 0.9907(9) 0.253(19) Uiso 1 1 d D . . H64A H 0.5237 0.4058 1.0142 0.380 Uiso 1 1 calc R . . H64B H 0.4607 0.3766 1.0063 0.380 Uiso 1 1 calc R . . H64C H 0.4724 0.4412 0.9713 0.380 Uiso 1 1 calc R . . C65 C 0.5152(12) 0.2475(15) 0.9901(9) 0.32(3) Uiso 1 1 d D . . H65A H 0.5526 0.2586 1.0129 0.486 Uiso 1 1 calc R . . H65B H 0.5174 0.2015 0.9703 0.486 Uiso 1 1 calc R . . H65C H 0.4892 0.2336 1.0066 0.486 Uiso 1 1 calc R . . C66 C 0.3820(8) 0.1313(11) 0.8528(8) 0.130(7) Uiso 1 1 d D . . C67 C 0.4162(7) 0.0592(9) 0.8462(5) 0.197(13) Uiso 1 1 d D . . C68 C 0.4022(11) -0.0161(11) 0.8693(9) 0.215(15) Uiso 1 1 d D . . H68A H 0.4255 -0.0622 0.8662 0.322 Uiso 1 1 calc R . . H68B H 0.3623 -0.0298 0.8542 0.322 Uiso 1 1 calc R . . H68C H 0.4099 -0.0048 0.9024 0.322 Uiso 1 1 calc R . . C69 C 0.4785(6) 0.0784(15) 0.8683(8) 0.177(11) Uiso 1 1 d D . . H69A H 0.5007 0.0318 0.8641 0.266 Uiso 1 1 calc R . . H69B H 0.4876 0.0890 0.9016 0.266 Uiso 1 1 calc R . . H69C H 0.4875 0.1270 0.8533 0.266 Uiso 1 1 calc R . . C70 C 0.4021(11) 0.0429(15) 0.7945(6) 0.209(14) Uiso 1 1 d D . . H70A H 0.4253 -0.0023 0.7903 0.313 Uiso 1 1 calc R . . H70B H 0.4097 0.0922 0.7794 0.313 Uiso 1 1 calc R . . H70C H 0.3622 0.0284 0.7805 0.313 Uiso 1 1 calc R . . C71 C 0.2832(11) 0.315(2) 0.7333(8) 0.203(14) Uiso 1 1 d D . . C72 C 0.2468(9) 0.2683(11) 0.6908(8) 0.184(12) Uiso 1 1 d D . . C73 C 0.1876(8) 0.3035(19) 0.6742(10) 0.212(15) Uiso 1 1 d D . . H73A H 0.1632 0.2702 0.6484 0.318 Uiso 1 1 calc R . . H73B H 0.1885 0.3599 0.6635 0.318 Uiso 1 1 calc R . . H73C H 0.1729 0.3032 0.6999 0.318 Uiso 1 1 calc R . . C74 C 0.2716(12) 0.276(2) 0.6522(9) 0.232(17) Uiso 1 1 d D . . H74A H 0.2489 0.2439 0.6252 0.348 Uiso 1 1 calc R . . H74B H 0.3103 0.2553 0.6634 0.348 Uiso 1 1 calc R . . H74C H 0.2715 0.3336 0.6433 0.348 Uiso 1 1 calc R . . C75 C 0.2447(18) 0.1786(13) 0.7032(16) 0.81(12) Uiso 1 1 d D . . H75A H 0.2197 0.1490 0.6761 1.218 Uiso 1 1 calc R . . H75B H 0.2304 0.1739 0.7291 1.218 Uiso 1 1 calc R . . H75C H 0.2826 0.1552 0.7125 1.218 Uiso 1 1 calc R . . C76 C 0.4487(9) 0.3729(15) 0.7767(8) 0.147(9) Uiso 1 1 d D . . C77 C 0.5021(7) 0.3736(10) 0.7647(6) 0.156(9) Uiso 1 1 d D . . C78 C 0.4868(10) 0.3759(15) 0.7121(6) 0.162(10) Uiso 1 1 d D . . H78A H 0.5212 0.3743 0.7043 0.244 Uiso 1 1 calc R . . H78B H 0.4659 0.4263 0.6998 0.244 Uiso 1 1 calc R . . H78C H 0.4632 0.3284 0.6983 0.244 Uiso 1 1 calc R . . C79 C 0.5367(12) 0.4487(15) 0.7861(10) 0.36(3) Uiso 1 1 d D . . H79A H 0.5711 0.4495 0.7782 0.533 Uiso 1 1 calc R . . H79B H 0.5468 0.4471 0.8200 0.533 Uiso 1 1 calc R . . H79C H 0.5146 0.4982 0.7738 0.533 Uiso 1 1 calc R . . C80 C 0.5361(11) 0.2969(15) 0.7840(9) 0.243(18) Uiso 1 1 d D . . H80A H 0.5698 0.2962 0.7752 0.364 Uiso 1 1 calc R . . H80B H 0.5131 0.2484 0.7712 0.364 Uiso 1 1 calc R . . H80C H 0.5473 0.2966 0.8181 0.364 Uiso 1 1 calc R . . C81 C 0.3943(6) 0.6104(11) 0.8119(6) 0.110(6) Uiso 1 1 d D . . C82 C 0.4480(6) 0.6416(9) 0.8482(5) 0.171(11) Uiso 1 1 d D . . C83 C 0.4369(11) 0.7242(11) 0.8662(9) 0.231(17) Uiso 1 1 d D . . H83A H 0.4717 0.7444 0.8897 0.347 Uiso 1 1 calc R . . H83B H 0.4077 0.7184 0.8803 0.347 Uiso 1 1 calc R . . H83C H 0.4243 0.7632 0.8403 0.347 Uiso 1 1 calc R . . C84 C 0.4675(9) 0.5812(15) 0.8884(6) 0.208(14) Uiso 1 1 d D . . H84A H 0.5030 0.6004 0.9113 0.312 Uiso 1 1 calc R . . H84B H 0.4733 0.5274 0.8766 0.312 Uiso 1 1 calc R . . H84C H 0.4388 0.5769 0.9032 0.312 Uiso 1 1 calc R . . C85 C 0.4933(7) 0.6507(14) 0.8265(8) 0.164(10) Uiso 1 1 d D . . H85A H 0.5285 0.6689 0.8502 0.246 Uiso 1 1 calc R . . H85B H 0.4813 0.6911 0.8013 0.246 Uiso 1 1 calc R . . H85C H 0.4995 0.5978 0.8138 0.246 Uiso 1 1 calc R . . C86 C 0.3070(8) 0.6070(12) 0.6865(6) 0.127(7) Uiso 1 1 d D . . C87 C 0.3075(6) 0.6340(8) 0.6392(5) 0.136(8) Uiso 1 1 d D . . C88 C 0.2666(9) 0.5816(14) 0.6015(7) 0.241(17) Uiso 1 1 d D . . H88A H 0.2659 0.6004 0.5708 0.362 Uiso 1 1 calc R . . H88B H 0.2289 0.5864 0.6033 0.362 Uiso 1 1 calc R . . H88C H 0.2788 0.5243 0.6060 0.362 Uiso 1 1 calc R . . C89 C 0.3664(7) 0.6242(13) 0.6375(8) 0.151(9) Uiso 1 1 d D . . H89A H 0.3669 0.6427 0.6071 0.227 Uiso 1 1 calc R . . H89B H 0.3775 0.5665 0.6420 0.227 Uiso 1 1 calc R . . H89C H 0.3929 0.6571 0.6623 0.227 Uiso 1 1 calc R . . C90 C 0.2898(10) 0.7232(10) 0.6313(8) 0.185(12) Uiso 1 1 d D . . H90A H 0.2895 0.7405 0.6005 0.278 Uiso 1 1 calc R . . H90B H 0.3165 0.7571 0.6553 0.278 Uiso 1 1 calc R . . H90C H 0.2520 0.7297 0.6329 0.278 Uiso 1 1 calc R . . N1 N 0.2702(15) 0.4644(19) 0.8830(12) 0.208(12) Uiso 1 1 d . B . H1A H 0.2483 0.4715 0.9014 0.249 Uiso 1 1 calc R . . H1B H 0.2870 0.4139 0.8901 0.249 Uiso 1 1 calc R . . C1A C 0.2371(18) 0.464(2) 0.8398(15) 0.219(16) Uiso 1 1 d . . . H1A1 H 0.2599 0.4506 0.8200 0.263 Uiso 1 1 calc R . . H1A2 H 0.2213 0.5191 0.8312 0.263 Uiso 1 1 calc R . . C2A C 0.1886(13) 0.4026(19) 0.8287(11) 0.166(10) Uiso 1 1 d . . . H2A1 H 0.1677 0.4139 0.8501 0.200 Uiso 1 1 calc R . . H2A2 H 0.2050 0.3471 0.8362 0.200 Uiso 1 1 calc R . . C3A C 0.1450(14) 0.400(2) 0.7781(12) 0.194(13) Uiso 1 1 d . . . H3A1 H 0.1147 0.3620 0.7766 0.291 Uiso 1 1 calc R . . H3A2 H 0.1639 0.3827 0.7565 0.291 Uiso 1 1 calc R . . H3A3 H 0.1292 0.4553 0.7693 0.291 Uiso 1 1 calc R . . C1B C 0.3080(19) 0.518(3) 0.8942(15) 0.222(16) Uiso 1 1 d . . . H1B1 H 0.2917 0.5733 0.8887 0.266 Uiso 1 1 calc R A 1 H1B2 H 0.3337 0.5107 0.8763 0.266 Uiso 1 1 calc R A 1 C2B C 0.336(2) 0.504(3) 0.9412(18) 0.124(15) Uiso 0.50 1 d P B 1 H2B1 H 0.3375 0.5595 0.9548 0.149 Uiso 0.50 1 calc PR B 1 H2B2 H 0.3081 0.4736 0.9508 0.149 Uiso 0.50 1 calc PR B 1 C3B C 0.355(2) 0.550(3) 0.9446(19) 0.140(18) Uiso 0.50 1 d P B 2 H3B1 H 0.3834 0.5870 0.9392 0.168 Uiso 0.50 1 calc PR B 2 H3B2 H 0.3370 0.5775 0.9643 0.168 Uiso 0.50 1 calc PR B 2 C4B C 0.381(2) 0.474(3) 0.965(2) 0.32(3) Uiso 1 1 d . . . H4B1 H 0.3846 0.4764 0.9982 0.473 Uiso 1 1 calc R B 1 H4B2 H 0.4122 0.5039 0.9607 0.473 Uiso 1 1 calc R B 1 H4B3 H 0.3825 0.4163 0.9563 0.473 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.231(5) 0.125(3) 0.108(2) 0.052(2) 0.077(3) 0.110(3) Fe1 0.0651(13) 0.0744(14) 0.0621(12) 0.0127(10) 0.0178(10) 0.0135(10) Fe2 0.0585(12) 0.0742(13) 0.0516(11) 0.0083(9) 0.0123(9) 0.0039(10) Fe3 0.0578(13) 0.1061(17) 0.0640(13) 0.0255(12) 0.0130(10) -0.0039(11) Fe4 0.0679(15) 0.139(2) 0.1050(19) 0.0692(18) -0.0010(13) -0.0193(15) Fe5 0.0795(17) 0.108(2) 0.137(2) 0.0570(18) -0.0171(16) -0.0271(15) Fe6 0.0700(17) 0.101(2) 0.182(3) 0.055(2) -0.0201(18) 0.0102(15) Fe7 0.153(3) 0.101(2) 0.125(3) 0.0295(18) 0.002(2) 0.057(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O82 1.833(16) . ? Mn1 O72 1.87(2) . ? Mn1 O83 1.93(2) . ? Mn1 O74 1.95(2) . ? Mn1 F8 1.949(9) . ? Mn1 F7 1.954(10) . ? Fe1 F1 1.924(7) . ? Fe1 O13 1.932(11) . ? Fe1 O11 1.953(11) . ? Fe1 O84 1.956(12) . ? Fe1 F8 1.961(8) . ? Fe1 O81 2.006(12) . ? Fe2 F2 1.943(7) . ? Fe2 F1 1.957(7) . ? Fe2 O21 1.959(9) . ? Fe2 O23 1.971(11) . ? Fe2 O14 1.974(10) . ? Fe2 O12 1.979(10) . ? Fe3 F3 1.938(8) . ? Fe3 O24 1.951(11) . ? Fe3 O22 1.956(10) . ? Fe3 O33 1.963(12) . ? Fe3 F2 1.967(8) . ? Fe3 O31 1.991(11) . ? Fe4 F4 1.918(11) . ? Fe4 O43 1.958(16) . ? Fe4 O32 1.985(13) . ? Fe4 F3 1.984(9) . ? Fe4 O41 2.007(13) . ? Fe4 O34 2.059(13) . ? Fe5 F5 1.943(10) . ? Fe5 F4 1.993(11) . ? Fe5 O51 1.999(14) . ? Fe5 O53 1.996(15) . ? Fe5 O44 2.062(14) . ? Fe5 O42 2.066(12) . ? Fe6 F6 1.938(11) . ? Fe6 O63 1.95(2) . ? Fe6 F5 2.014(10) . ? Fe6 O61 2.018(15) . ? Fe6 O52 2.030(16) . ? Fe6 O54 2.027(15) . ? Fe7 O71 1.90(2) . ? Fe7 F7 1.916(10) . ? Fe7 O62 1.938(15) . ? Fe7 O73 1.96(2) . ? Fe7 O64 1.98(2) . ? Fe7 F6 2.026(11) . ? O11 C11 1.295(15) . ? O12 C11 1.203(15) . ? O13 C16 1.291(15) . ? O14 C16 1.258(15) . ? O21 C21 1.278(14) . ? O22 C21 1.262(15) . ? O23 C26 1.230(16) . ? O24 C26 1.265(16) . ? O31 C31 1.164(15) . ? O32 C31 1.280(16) . ? O33 C36 1.267(19) . ? O34 C36 1.131(18) . ? O41 C41 1.261(19) . ? O42 C41 1.151(18) . ? O43 C46 1.187(19) . ? O44 C46 1.175(18) . ? O51 C51 1.150(17) . ? O52 C51 1.211(18) . ? O53 C56 1.17(2) . ? O54 C56 1.199(19) . ? O61 C61 1.27(2) . ? O62 C61 1.21(2) . ? O63 C66 1.24(3) . ? O64 C66 1.38(3) . ? O71 C71 1.30(3) . ? O72 C71 1.30(3) . ? O73 C76 1.15(2) . ? O74 C76 1.48(3) . ? O81 C81 1.42(2) . ? O82 C81 1.19(2) . ? O83 C86 1.34(2) . ? O84 C86 1.13(2) . ? C11 C12 1.52(2) . ? C12 C13 1.52(2) . ? C12 C15 1.52(2) . ? C12 C14 1.52(2) . ? C16 C17 1.51(2) . ? C17 C20 1.52(2) . ? C17 C18 1.52(2) . ? C17 C19 1.52(2) . ? C21 C22 1.51(2) . ? C22 C24 1.52(2) . ? C22 C23 1.52(2) . ? C22 C25 1.52(2) . ? C26 C27 1.52(2) . ? C27 C29 1.52(2) . ? C27 C28 1.52(2) . ? C27 C30 1.52(2) . ? C31 C32 1.52(2) . ? C32 C33 1.52(2) . ? C32 C34 1.52(2) . ? C32 C35 1.52(2) . ? C36 C37 1.52(2) . ? C37 C38 1.52(2) . ? C37 C39 1.52(2) . ? C37 C40 1.52(2) . ? C41 C42 1.52(2) . ? C42 C43 1.52(2) . ? C42 C44 1.52(2) . ? C42 C45 1.52(2) . ? C46 C47 1.52(2) . ? C47 C49 1.52(2) . ? C47 C50 1.52(2) . ? C47 C48 1.52(2) . ? C51 C52 1.52(2) . ? C52 C55 1.52(2) . ? C52 C53 1.52(2) . ? C52 C54 1.52(2) . ? C56 C57 1.52(2) . ? C57 C60 1.52(2) . ? C57 C59 1.52(2) . ? C57 C58 1.52(2) . ? C61 C62 1.51(2) . ? C62 C65 1.52(2) . ? C62 C63 1.52(2) . ? C62 C64 1.52(2) . ? C66 C67 1.52(2) . ? C67 C69 1.52(2) . ? C67 C70 1.52(2) . ? C67 C68 1.52(2) . ? C71 C72 1.52(2) . ? C72 C75 1.52(2) . ? C72 C74 1.52(2) . ? C72 C73 1.52(2) . ? C76 C77 1.52(2) . ? C77 C79 1.52(2) . ? C77 C78 1.52(2) . ? C77 C80 1.52(2) . ? C81 C82 1.52(2) . ? C82 C83 1.52(2) . ? C82 C85 1.52(2) . ? C82 C84 1.52(2) . ? C86 C87 1.52(2) . ? C87 C90 1.52(2) . ? C87 C89 1.52(2) . ? C87 C88 1.52(2) . ? N1 C1B 1.25(4) . ? N1 C1A 1.30(4) . ? C1A C2A 1.53(4) . ? C2A C3A 1.56(4) . ? C1B C2B 1.38(6) . ? C1B C3B 1.68(7) . ? C2B C4B 1.23(6) . ? C3B C4B 1.44(7) . ? 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 O82 Mn1 O72 175.7(8) . . ? O82 Mn1 O83 97.1(8) . . ? O72 Mn1 O83 83.8(8) . . ? O82 Mn1 O74 85.4(9) . . ? O72 Mn1 O74 90.3(9) . . ? O83 Mn1 O74 92.6(9) . . ? O82 Mn1 F8 93.5(5) . . ? O72 Mn1 F8 90.7(7) . . ? O83 Mn1 F8 87.7(6) . . ? O74 Mn1 F8 178.9(8) . . ? O82 Mn1 F7 89.9(6) . . ? O72 Mn1 F7 89.7(7) . . ? O83 Mn1 F7 171.2(7) . . ? O74 Mn1 F7 93.3(8) . . ? F8 Mn1 F7 86.5(4) . . ? F1 Fe1 O13 91.1(4) . . ? F1 Fe1 O11 91.3(4) . . ? O13 Fe1 O11 94.0(4) . . ? F1 Fe1 O84 179.5(4) . . ? O13 Fe1 O84 88.5(5) . . ? O11 Fe1 O84 89.0(5) . . ? F1 Fe1 F8 88.7(3) . . ? O13 Fe1 F8 177.4(4) . . ? O11 Fe1 F8 88.6(4) . . ? O84 Fe1 F8 91.7(4) . . ? F1 Fe1 O81 88.6(4) . . ? O13 Fe1 O81 88.6(5) . . ? O11 Fe1 O81 177.5(4) . . ? O84 Fe1 O81 91.2(5) . . ? F8 Fe1 O81 88.8(4) . . ? F2 Fe2 F1 85.6(3) . . ? F2 Fe2 O21 91.4(4) . . ? F1 Fe2 O21 87.9(3) . . ? F2 Fe2 O23 90.2(4) . . ? F1 Fe2 O23 175.8(4) . . ? O21 Fe2 O23 92.7(4) . . ? F2 Fe2 O14 178.2(4) . . ? F1 Fe2 O14 92.7(4) . . ? O21 Fe2 O14 88.1(4) . . ? O23 Fe2 O14 91.5(4) . . ? F2 Fe2 O12 90.9(4) . . ? F1 Fe2 O12 89.2(4) . . ? O21 Fe2 O12 176.2(4) . . ? O23 Fe2 O12 90.3(4) . . ? O14 Fe2 O12 89.5(4) . . ? F3 Fe3 O24 178.2(4) . . ? F3 Fe3 O22 90.1(4) . . ? O24 Fe3 O22 91.7(4) . . ? F3 Fe3 O33 91.5(4) . . ? O24 Fe3 O33 88.7(5) . . ? O22 Fe3 O33 91.0(5) . . ? F3 Fe3 F2 87.9(3) . . ? O24 Fe3 F2 91.8(4) . . ? O22 Fe3 F2 88.4(4) . . ? O33 Fe3 F2 179.2(5) . . ? F3 Fe3 O31 91.3(4) . . ? O24 Fe3 O31 86.9(4) . . ? O22 Fe3 O31 176.4(4) . . ? O33 Fe3 O31 92.2(5) . . ? F2 Fe3 O31 88.3(4) . . ? F4 Fe4 O43 89.1(6) . . ? F4 Fe4 O32 90.2(5) . . ? O43 Fe4 O32 89.3(6) . . ? F4 Fe4 F3 85.7(4) . . ? O43 Fe4 F3 173.8(6) . . ? O32 Fe4 F3 87.3(4) . . ? F4 Fe4 O41 92.2(5) . . ? O43 Fe4 O41 96.9(6) . . ? O32 Fe4 O41 173.4(5) . . ? F3 Fe4 O41 86.8(4) . . ? F4 Fe4 O34 175.6(5) . . ? O43 Fe4 O34 95.3(6) . . ? O32 Fe4 O34 90.1(5) . . ? F3 Fe4 O34 89.9(4) . . ? O41 Fe4 O34 87.1(5) . . ? F5 Fe5 F4 85.2(4) . . ? F5 Fe5 O51 93.3(5) . . ? F4 Fe5 O51 87.8(5) . . ? F5 Fe5 O53 92.5(5) . . ? F4 Fe5 O53 175.1(6) . . ? O51 Fe5 O53 96.7(6) . . ? F5 Fe5 O44 174.8(5) . . ? F4 Fe5 O44 89.6(5) . . ? O51 Fe5 O44 86.5(6) . . ? O53 Fe5 O44 92.7(6) . . ? F5 Fe5 O42 90.2(4) . . ? F4 Fe5 O42 86.9(5) . . ? O51 Fe5 O42 173.4(5) . . ? O53 Fe5 O42 88.7(6) . . ? O44 Fe5 O42 89.5(5) . . ? F6 Fe6 O63 92.1(7) . . ? F6 Fe6 F5 88.1(4) . . ? O63 Fe6 F5 177.7(7) . . ? F6 Fe6 O61 90.6(5) . . ? O63 Fe6 O61 86.7(8) . . ? F5 Fe6 O61 91.0(5) . . ? F6 Fe6 O52 87.5(6) . . ? O63 Fe6 O52 93.5(8) . . ? F5 Fe6 O52 88.8(5) . . ? O61 Fe6 O52 178.1(6) . . ? F6 Fe6 O54 176.7(6) . . ? O63 Fe6 O54 89.7(8) . . ? F5 Fe6 O54 90.0(5) . . ? O61 Fe6 O54 86.7(6) . . ? O52 Fe6 O54 95.1(6) . . ? O71 Fe7 F7 90.4(7) . . ? O71 Fe7 O62 178.5(8) . . ? F7 Fe7 O62 89.3(5) . . ? O71 Fe7 O73 91.4(9) . . ? F7 Fe7 O73 89.9(6) . . ? O62 Fe7 O73 87.1(7) . . ? O71 Fe7 O64 90.5(9) . . ? F7 Fe7 O64 176.1(8) . . ? O62 Fe7 O64 89.6(8) . . ? O73 Fe7 O64 86.2(9) . . ? O71 Fe7 F6 91.6(7) . . ? F7 Fe7 F6 90.1(4) . . ? O62 Fe7 F6 89.8(5) . . ? O73 Fe7 F6 176.9(7) . . ? O64 Fe7 F6 93.7(7) . . ? C11 O11 Fe1 136.3(8) . . ? C11 O12 Fe2 131.3(9) . . ? C16 O13 Fe1 128.9(9) . . ? C16 O14 Fe2 134.9(8) . . ? C21 O21 Fe2 137.0(8) . . ? C21 O22 Fe3 130.2(8) . . ? C26 O23 Fe2 131.8(9) . . ? C26 O24 Fe3 136.8(9) . . ? C31 O31 Fe3 136.3(9) . . ? C31 O32 Fe4 128.8(9) . . ? C36 O33 Fe3 127.9(11) . . ? C36 O34 Fe4 137.3(13) . . ? C41 O41 Fe4 134.4(11) . . ? C41 O42 Fe5 135.5(12) . . ? C46 O43 Fe4 132.7(13) . . ? C46 O44 Fe5 136.3(13) . . ? C51 O51 Fe5 131.4(12) . . ? C51 O52 Fe6 126.8(13) . . ? C56 O53 Fe5 122.7(13) . . ? C56 O54 Fe6 129.7(12) . . ? C61 O61 Fe6 135.4(12) . . ? C61 O62 Fe7 128.6(13) . . ? C66 O63 Fe6 129.4(17) . . ? C66 O64 Fe7 126.6(16) . . ? C71 O71 Fe7 135.3(19) . . ? C71 O72 Mn1 135.7(16) . . ? C76 O73 Fe7 144.4(18) . . ? C76 O74 Mn1 132.7(16) . . ? C81 O81 Fe1 129.7(10) . . ? C81 O82 Mn1 140.8(14) . . ? C86 O83 Mn1 124.7(14) . . ? C86 O84 Fe1 136.2(12) . . ? Fe1 F1 Fe2 122.5(4) . . ? Fe2 F2 Fe3 121.7(4) . . ? Fe3 F3 Fe4 121.2(4) . . ? Fe4 F4 Fe5 121.7(6) . . ? Fe5 F5 Fe6 120.2(5) . . ? Fe6 F6 Fe7 123.2(5) . . ? Fe7 F7 Mn1 122.7(5) . . ? Mn1 F8 Fe1 120.9(4) . . ? O12 C11 O11 124(1) . . ? O12 C11 C12 121(1) . . ? O11 C11 C12 114(1) . . ? C11 C12 C13 110(2) . . ? C11 C12 C15 110(2) . . ? C13 C12 C15 110(2) . . ? C11 C12 C14 110(2) . . ? C13 C12 C14 110(2) . . ? C15 C12 C14 110(2) . . ? O14 C16 O13 124(1) . . ? O14 C16 C17 117(1) . . ? O13 C16 C17 118(1) . . ? C16 C17 C20 110(2) . . ? C16 C17 C18 110(2) . . ? C20 C17 C18 110(2) . . ? C16 C17 C19 110(2) . . ? C20 C17 C19 109(2) . . ? C18 C17 C19 109(2) . . ? O22 C21 O21 123(1) . . ? O22 C21 C22 123(1) . . ? O21 C21 C22 114(1) . . ? C21 C22 C24 110(2) . . ? C21 C22 C23 110(2) . . ? C24 C22 C23 109(2) . . ? C21 C22 C25 110(2) . . ? C24 C22 C25 109(2) . . ? C23 C22 C25 109(2) . . ? O23 C26 O24 122(1) . . ? O23 C26 C27 124(1) . . ? O24 C26 C27 114(1) . . ? C26 C27 C29 110(2) . . ? C26 C27 C28 110(2) . . ? C29 C27 C28 110(2) . . ? C26 C27 C30 110(2) . . ? C29 C27 C30 110(2) . . ? C28 C27 C30 109(2) . . ? O31 C31 O32 125(1) . . ? O31 C31 C32 116(1) . . ? O32 C31 C32 118(1) . . ? C31 C32 C33 110(2) . . ? C31 C32 C34 110(2) . . ? C33 C32 C34 110(2) . . ? C31 C32 C35 109(2) . . ? C33 C32 C35 110(2) . . ? C34 C32 C35 109(2) . . ? O34 C36 O33 125(2) . . ? O34 C36 C37 119(2) . . ? O33 C36 C37 116(1) . . ? C36 C37 C38 110(2) . . ? C36 C37 C39 110(2) . . ? C38 C37 C39 110(2) . . ? C36 C37 C40 110(2) . . ? C38 C37 C40 109(2) . . ? C39 C37 C40 109(2) . . ? O42 C41 O41 124(2) . . ? O42 C41 C42 121(1) . . ? O41 C41 C42 114(1) . . ? C41 C42 C43 110(2) . . ? C41 C42 C44 110(2) . . ? C43 C42 C44 110(2) . . ? C41 C42 C45 109(2) . . ? C43 C42 C45 110(2) . . ? C44 C42 C45 110(2) . . ? O44 C46 O43 123(2) . . ? O44 C46 C47 121(1) . . ? O43 C46 C47 115(1) . . ? C46 C47 C49 110(2) . . ? C46 C47 C50 109(2) . . ? C49 C47 C50 110(2) . . ? C46 C47 C48 109(2) . . ? C49 C47 C48 110(2) . . ? C50 C47 C48 110(2) . . ? O51 C51 O52 135(1) . . ? O51 C51 C52 107(1) . . ? O52 C51 C52 117(1) . . ? C51 C52 C55 110(2) . . ? C51 C52 C53 110(2) . . ? C55 C52 C53 110(2) . . ? C51 C52 C54 109(2) . . ? C55 C52 C54 110(2) . . ? C53 C52 C54 110(2) . . ? O53 C56 O54 139(1) . . ? O53 C56 C57 99(1) . . ? O54 C56 C57 121(1) . . ? C56 C57 C60 110(2) . . ? C56 C57 C59 110(2) . . ? C60 C57 C59 110(2) . . ? C56 C57 C58 109(2) . . ? C60 C57 C58 109(2) . . ? C59 C57 C58 109(2) . . ? O62 C61 O61 127(2) . . ? O62 C61 C62 117(2) . . ? O61 C61 C62 116(2) . . ? C61 C62 C65 110(2) . . ? C61 C62 C63 110(2) . . ? C65 C62 C63 109(2) . . ? C61 C62 C64 109(2) . . ? C65 C62 C64 109(2) . . ? C63 C62 C64 109(2) . . ? O63 C66 O64 132(2) . . ? O63 C66 C67 122(2) . . ? O64 C66 C67 103(1) . . ? C66 C67 C69 109(2) . . ? C66 C67 C70 109(2) . . ? C69 C67 C70 109(2) . . ? C66 C67 C68 109(2) . . ? C69 C67 C68 109(2) . . ? C70 C67 C68 109(2) . . ? O72 C71 O71 117(2) . . ? O72 C71 C72 112(2) . . ? O71 C71 C72 122(3) . . ? C71 C72 C75 109(2) . . ? C71 C72 C74 109(2) . . ? C75 C72 C74 109(2) . . ? C71 C72 C73 109(2) . . ? C75 C72 C73 109(2) . . ? C74 C72 C73 109(2) . . ? O73 C76 O74 112(2) . . ? O73 C76 C77 131(2) . . ? O74 C76 C77 116(2) . . ? C76 C77 C79 109(2) . . ? C76 C77 C78 109(2) . . ? C79 C77 C78 110(2) . . ? C76 C77 C80 109(2) . . ? C79 C77 C80 110(2) . . ? C78 C77 C80 110(2) . . ? O82 C81 O81 118(1) . . ? O82 C81 C82 128(2) . . ? O81 C81 C82 113(1) . . ? C81 C82 C83 110(2) . . ? C81 C82 C85 110(2) . . ? C83 C82 C85 110(2) . . ? C81 C82 C84 110(2) . . ? C83 C82 C84 110(2) . . ? C85 C82 C84 110(2) . . ? O84 C86 O83 127(2) . . ? O84 C86 C87 118(1) . . ? O83 C86 C87 115(1) . . ? C86 C87 C90 109(2) . . ? C86 C87 C89 109(2) . . ? C90 C87 C89 110(2) . . ? C86 C87 C88 109(2) . . ? C90 C87 C88 110(2) . . ? C89 C87 C88 110(2) . . ? C1B N1 C1A 117(4) . . ? N1 C1A C2A 115(4) . . ? C1A C2A C3A 118(3) . . ? N1 C1B C2B 104(4) . . ? N1 C1B C3B 135(4) . . ? C2B C1B C3B 31(3) . . ? C4B C2B C1B 136(6) . . ? C4B C3B C1B 102(4) . . ? C2B C4B C3B 37(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.306 _refine_diff_density_min -1.831 _refine_diff_density_rms 0.178 data_04gt214a_0m _database_code_depnum_ccdc_archive 'CCDC 257790' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H160 F8 Fe8 N O32' _chemical_formula_weight 2318.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_space_group_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' _cell_length_a 26.041(3) _cell_length_b 20.515(2) _cell_length_c 26.199(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.125(3) _cell_angle_gamma 90.00 _cell_volume 13142(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6435 _cell_measurement_theta_min 2.035 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4876 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ApexII CCD-based diffractometer' _diffrn_measurement_method '\f and \o scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50353 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 24.11 _reflns_number_total 20654 _reflns_number_gt 16407 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(6) _refine_ls_number_reflns 20654 _refine_ls_number_parameters 538 _refine_ls_number_restraints 161 _refine_ls_R_factor_all 0.2139 _refine_ls_R_factor_gt 0.1875 _refine_ls_wR_factor_ref 0.5457 _refine_ls_wR_factor_gt 0.5261 _refine_ls_goodness_of_fit_ref 2.424 _refine_ls_restrained_S_all 2.415 _refine_ls_shift/su_max 0.244 _refine_ls_shift/su_mean 0.020 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 Fe1A Fe 0.5000 0.4526(4) 0.5000 0.100(2) Uani 1 2 d S . . Fe2A Fe 0.37603(10) 0.3841(3) 0.42576(10) 0.0456(7) Uani 1 1 d . . . Fe3A Fe 0.32794(15) 0.2309(3) 0.39889(17) 0.1023(17) Uani 1 1 d . . . Fe4A Fe 0.37648(8) 0.0726(3) 0.42505(8) 0.0343(6) Uani 1 1 d . . . Fe5A Fe 0.5000 0.0101(4) 0.5000 0.145(4) Uani 1 2 d S . . F1A F 0.4472(3) 0.3822(5) 0.4895(3) 0.0334(18) Uiso 1 1 d . . . F2A F 0.3870(4) 0.2908(6) 0.4142(4) 0.054(3) Uiso 1 1 d . . . F3A F 0.3742(4) 0.1660(5) 0.4462(4) 0.044(2) Uiso 1 1 d . . . F4A F 0.4583(3) 0.0774(5) 0.4543(3) 0.0375(2) Uiso 1 1 d . . . O11A O 0.4972(14) 0.4497(18) 0.4281(14) 0.173(12) Uiso 1 1 d . . . O12A O 0.4134(7) 0.4072(9) 0.3756(7) 0.075(4) Uiso 1 1 d . . . O13A O 0.4312(9) 0.5156(11) 0.4977(9) 0.106(6) Uiso 1 1 d . . . O14A O 0.3670(7) 0.4770(9) 0.4492(6) 0.074(4) Uiso 1 1 d . . . O21A O 0.3370(6) 0.3546(8) 0.4782(6) 0.071(4) Uiso 1 1 d . . . O22A O 0.3168(9) 0.2637(13) 0.4704(9) 0.115(6) Uiso 1 1 d . . . O23A O 0.3078(7) 0.3847(9) 0.3639(7) 0.080(4) Uiso 1 1 d . . . O24A O 0.2681(5) 0.2913(7) 0.3592(5) 0.057(3) Uiso 1 1 d . . . O31A O 0.3336(7) 0.2008(10) 0.3370(7) 0.088(5) Uiso 1 1 d . . . O32A O 0.3785(7) 0.0979(9) 0.3526(7) 0.080(4) Uiso 1 1 d . . . O33A O 0.2638(8) 0.1676(11) 0.3905(8) 0.097(5) Uiso 1 1 d . . . O34A O 0.2981(7) 0.0687(9) 0.3952(6) 0.079(4) Uiso 1 1 d . . . O41A O 0.3706(6) 0.0428(8) 0.4896(6) 0.067(4) Uiso 1 1 d . . . O42A O 0.4359(8) 0.0234(9) 0.5511(7) 0.087(5) Uiso 1 1 d . . . O43A O 0.3807(6) -0.0225(8) 0.4095(6) 0.066(4) Uiso 1 1 d . . . O44A O 0.4428(8) -0.0709(10) 0.4718(8) 0.093(5) Uiso 1 1 d . . . C11A C 0.4639(8) 0.4342(9) 0.3820(6) 0.057(5) Uiso 1 1 d D . . C12A C 0.4705(6) 0.4532(8) 0.3297(6) 0.078(6) Uiso 1 1 d D . . C13A C 0.5283(8) 0.4729(16) 0.3399(11) 0.168(3) Uiso 1 1 d D . . H13A H 0.5328 0.4846 0.3054 0.253 Uiso 1 1 calc R . . H13B H 0.5527 0.4365 0.3566 0.253 Uiso 1 1 calc R . . H13C H 0.5375 0.5105 0.3645 0.253 Uiso 1 1 calc R . . C14A C 0.4562(14) 0.3969(13) 0.2915(9) 0.168(3) Uiso 1 1 d D . . H14A H 0.4613 0.4091 0.2574 0.253 Uiso 1 1 calc R . . H14B H 0.4180 0.3846 0.2841 0.253 Uiso 1 1 calc R . . H14C H 0.4800 0.3599 0.3078 0.253 Uiso 1 1 calc R . . C15A C 0.4335(12) 0.5091(13) 0.3053(11) 0.168(3) Uiso 1 1 d D . . H15A H 0.4379 0.5216 0.2709 0.253 Uiso 1 1 calc R . . H15B H 0.4429 0.5461 0.3304 0.253 Uiso 1 1 calc R . . H15C H 0.3955 0.4961 0.2985 0.253 Uiso 1 1 calc R . . C16A C 0.3955(7) 0.5275(8) 0.4588(7) 0.051(4) Uiso 1 1 d D . . C17A C 0.3741(6) 0.5955(8) 0.4523(7) 0.095(8) Uiso 1 1 d D . . C18A C 0.4097(12) 0.6366(11) 0.4977(11) 0.168(3) Uiso 1 1 d D . . H18A H 0.3951 0.6810 0.4939 0.253 Uiso 1 1 calc R . . H18B H 0.4468 0.6374 0.4964 0.253 Uiso 1 1 calc R . . H18C H 0.4104 0.6183 0.5325 0.253 Uiso 1 1 calc R . . C19A C 0.3739(13) 0.6224(13) 0.3994(10) 0.168(3) Uiso 1 1 d D . . H19A H 0.3588 0.6667 0.3948 0.253 Uiso 1 1 calc R . . H19B H 0.3513 0.5947 0.3697 0.253 Uiso 1 1 calc R . . H19C H 0.4114 0.6236 0.3991 0.253 Uiso 1 1 calc R . . C20A C 0.3172(8) 0.5954(14) 0.4535(14) 0.168(3) Uiso 1 1 d D . . H20A H 0.3031 0.6401 0.4490 0.253 Uiso 1 1 calc R . . H20B H 0.3174 0.5780 0.4884 0.253 Uiso 1 1 calc R . . H20C H 0.2939 0.5682 0.4238 0.253 Uiso 1 1 calc R . . C21A C 0.3113(8) 0.3145(10) 0.4858(7) 0.063(5) Uiso 1 1 d D . . C22A C 0.2923(7) 0.3347(9) 0.5310(7) 0.109(9) Uiso 1 1 d D . . C23A C 0.2436(10) 0.3779(14) 0.5093(13) 0.168(3) Uiso 1 1 d D . . H23A H 0.2530 0.4157 0.4913 0.253 Uiso 1 1 calc R . . H23B H 0.2320 0.3927 0.5392 0.253 Uiso 1 1 calc R . . H23C H 0.2137 0.3536 0.4829 0.253 Uiso 1 1 calc R . . C24A C 0.3370(12) 0.3707(16) 0.5729(10) 0.168(3) Uiso 1 1 d D . . H24A H 0.3482 0.4081 0.5560 0.253 Uiso 1 1 calc R . . H24B H 0.3682 0.3416 0.5887 0.253 Uiso 1 1 calc R . . H24C H 0.3238 0.3861 0.6016 0.253 Uiso 1 1 calc R . . C25A C 0.2774(14) 0.2758(13) 0.5561(12) 0.168(3) Uiso 1 1 d D . . H25A H 0.2479 0.2522 0.5286 0.253 Uiso 1 1 calc R . . H25B H 0.2650 0.2890 0.5859 0.253 Uiso 1 1 calc R . . H25C H 0.3094 0.2473 0.5702 0.253 Uiso 1 1 calc R . . C26A C 0.2755(6) 0.3439(9) 0.3313(6) 0.051(4) Uiso 1 1 d D . . C27A C 0.2246(5) 0.3675(7) 0.2888(5) 0.051(4) Uiso 1 1 d D . . C28A C 0.2372(10) 0.3884(16) 0.2399(7) 0.168(3) Uiso 1 1 d D . . H28A H 0.2035 0.4025 0.2114 0.253 Uiso 1 1 calc R . . H28B H 0.2532 0.3517 0.2265 0.253 Uiso 1 1 calc R . . H28C H 0.2633 0.4246 0.2496 0.253 Uiso 1 1 calc R . . C29A C 0.1833(8) 0.3140(11) 0.2736(12) 0.168(3) Uiso 1 1 d D . . H29A H 0.1501 0.3293 0.2450 0.253 Uiso 1 1 calc R . . H29B H 0.1744 0.3010 0.3055 0.253 Uiso 1 1 calc R . . H29C H 0.1983 0.2766 0.2602 0.253 Uiso 1 1 calc R . . C30A C 0.2021(11) 0.4239(12) 0.3103(11) 0.168(3) Uiso 1 1 d D . . H30A H 0.1684 0.4391 0.2824 0.253 Uiso 1 1 calc R . . H30B H 0.2290 0.4594 0.3198 0.253 Uiso 1 1 calc R . . H30C H 0.1943 0.4104 0.3427 0.253 Uiso 1 1 calc R . . C31A C 0.3647(6) 0.1502(8) 0.3228(5) 0.040(3) Uiso 1 1 d D . . C32A C 0.3634(6) 0.1542(8) 0.2655(5) 0.079(6) Uiso 1 1 d D . . C33A C 0.3076(8) 0.1366(16) 0.2279(7) 0.168(3) Uiso 1 1 d D . . H33A H 0.3066 0.1398 0.1902 0.253 Uiso 1 1 calc R . . H33B H 0.2807 0.1666 0.2334 0.253 Uiso 1 1 calc R . . H33C H 0.2990 0.0919 0.2353 0.253 Uiso 1 1 calc R . . C34A C 0.3768(13) 0.2219(10) 0.2538(10) 0.168(3) Uiso 1 1 d D . . H34A H 0.3755 0.2247 0.2160 0.253 Uiso 1 1 calc R . . H34B H 0.4136 0.2333 0.2782 0.253 Uiso 1 1 calc R . . H34C H 0.3502 0.2523 0.2594 0.253 Uiso 1 1 calc R . . C35A C 0.4042(11) 0.1081(14) 0.2576(10) 0.168(3) Uiso 1 1 d D . . H35A H 0.4033 0.1108 0.2199 0.253 Uiso 1 1 calc R . . H35B H 0.3954 0.0636 0.2653 0.253 Uiso 1 1 calc R . . H35C H 0.4408 0.1196 0.2823 0.253 Uiso 1 1 calc R . . C36A C 0.2584(5) 0.1124(7) 0.3800(6) 0.035(3) Uiso 1 1 d D . . C37A C 0.2031(6) 0.0872(9) 0.3475(7) 0.19(2) Uiso 1 1 d D . . C38A C 0.1935(12) 0.0239(11) 0.3707(14) 0.168(3) Uiso 1 1 d D . . H38A H 0.1575 0.0068 0.3487 0.253 Uiso 1 1 calc R . . H38B H 0.1947 0.0306 0.4081 0.253 Uiso 1 1 calc R . . H38C H 0.2219 -0.0073 0.3704 0.253 Uiso 1 1 calc R . . C39A C 0.1997(11) 0.0774(2) 0.2901(7) 0.168(3) Uiso 1 1 d D . . H39A H 0.2059 0.1191 0.2748 0.253 Uiso 1 1 calc R . . H39B H 0.1634 0.0607 0.2688 0.253 Uiso 1 1 calc R . . H39C H 0.2277 0.0461 0.2890 0.253 Uiso 1 1 calc R . . C40A C 0.1608(7) 0.1352(15) 0.3493(14) 0.168(3) Uiso 1 1 d D . . H40A H 0.1660 0.1762 0.3324 0.253 Uiso 1 1 calc R . . H40B H 0.1642 0.1434 0.3872 0.253 Uiso 1 1 calc R . . H40C H 0.1243 0.1178 0.3295 0.253 Uiso 1 1 calc R . . C41A C 0.3964(9) 0.0292(11) 0.5410(8) 0.068(6) Uiso 1 1 d D . . C42A C 0.3671(7) 0.0244(9) 0.5807(7) 0.109(9) Uiso 1 1 d D . . C43A C 0.3211(11) -0.0230(14) 0.5603(13) 0.168(3) Uiso 1 1 d D . . H43A H 0.2953 -0.0076 0.5255 0.253 Uiso 1 1 calc R . . H43B H 0.3022 -0.0267 0.5867 0.253 Uiso 1 1 calc R . . H43C H 0.3355 -0.0657 0.5553 0.253 Uiso 1 1 calc R . . C44A C 0.3450(13) 0.0896(11) 0.5875(13) 0.168(3) Uiso 1 1 d D . . H44A H 0.3202 0.1050 0.5522 0.253 Uiso 1 1 calc R . . H44B H 0.3753 0.1205 0.6017 0.253 Uiso 1 1 calc R . . H44C H 0.3251 0.0862 0.6130 0.253 Uiso 1 1 calc R . . C45A C 0.4058(12) 0.0016(17) 0.6342(8) 0.168(3) Uiso 1 1 d D . . H45A H 0.4193 -0.0419 0.6300 0.253 Uiso 1 1 calc R . . H45B H 0.3868 -0.0002 0.6606 0.253 Uiso 1 1 calc R . . H45C H 0.4366 0.0320 0.6470 0.253 Uiso 1 1 calc R . . C46A C 0.4072(7) -0.0652(7) 0.4177(7) 0.047(4) Uiso 1 1 d D . . C47A C 0.3929(6) -0.1290(7) 0.3891(6) 0.075(6) Uiso 1 1 d D . . C48A C 0.4016(13) -0.1254(14) 0.3358(8) 0.168(3) Uiso 1 1 d D . . H48A H 0.3924 -0.1675 0.3172 0.253 Uiso 1 1 calc R . . H48B H 0.4400 -0.1150 0.3420 0.253 Uiso 1 1 calc R . . H48C H 0.3781 -0.0914 0.3133 0.253 Uiso 1 1 calc R . . C49A C 0.3344(8) -0.1443(14) 0.3798(13) 0.168(3) Uiso 1 1 d D . . H49A H 0.3251 -0.1868 0.3618 0.253 Uiso 1 1 calc R . . H49B H 0.3110 -0.1106 0.3567 0.253 Uiso 1 1 calc R . . H49C H 0.3284 -0.1457 0.4147 0.253 Uiso 1 1 calc R . . C50A C 0.4282(12) -0.1812(9) 0.4231(12) 0.168(3) Uiso 1 1 d D . . H50A H 0.4184 -0.2232 0.4046 0.253 Uiso 1 1 calc R . . H50B H 0.4228 -0.1832 0.4583 0.253 Uiso 1 1 calc R . . H50C H 0.4666 -0.1715 0.4288 0.253 Uiso 1 1 calc R . . Fe1B Fe 0.0000 0.9872(3) 0.0000 0.0469(9) Uani 1 2 d S . . Fe2B Fe 0.1223(2) 0.9190(4) 0.0746(3) 0.163(4) Uani 1 1 d . . . Fe3B Fe 0.17174(9) 0.7664(3) 0.10205(9) 0.0366(6) Uani 1 1 d . . . Fe4B Fe 0.12457(14) 0.6071(3) 0.0750(3) 0.138(3) Uani 1 1 d . . . Fe5B Fe 0.0000 0.5447(3) 0.0000 0.0387(8) Uani 1 2 d S . . F1B F 0.0441(4) 0.9167(6) 0.0475(4) 0.055(3) Uiso 1 1 d . . . F2B F 0.1209(4) 0.8301(5) 0.0542(4) 0.039(2) Uiso 1 1 d . . . F3B F 0.1119(4) 0.7046(5) 0.0837(4) 0.044(2) Uiso 1 1 d . . . F4B F 0.0579(5) 0.6145(6) 0.0138(4) 0.057(3) Uiso 1 1 d . . . O11B O -0.0461(6) 0.9970(8) 0.0429(6) 0.071(4) Uiso 1 1 d . . . O12B O 0.1172(8) 0.9407(10) -0.0147(8) 0.089(5) Uiso 1 1 d . . . O13B O 0.0444(6) 1.0500(7) 0.0464(6) 0.062(3) Uiso 1 1 d . . . O14B O 0.1260(15) 1.0018(18) 0.0961(15) 0.176(12) Uiso 1 1 d . . . O21B O 0.1308(11) 0.9080(14) 0.1422(11) 0.124(8) Uiso 1 1 d . . . O22B O 0.1368(9) 0.7962(12) 0.1546(9) 0.114(7) Uiso 1 1 d . . . O23B O 0.2069(8) 0.9199(10) 0.0874(8) 0.090(5) Uiso 1 1 d . . . O24B O 0.2272(6) 0.8305(7) 0.1348(6) 0.061(3) Uiso 1 1 d . . . O31B O 0.1966(6) 0.7372(8) 0.0454(6) 0.065(3) Uiso 1 1 d . . . O32B O 0.1656(8) 0.6218(10) 0.0371(8) 0.095(5) Uiso 1 1 d . . . O33B O 0.2132(6) 0.7057(8) 0.1584(6) 0.064(4) Uiso 1 1 d . . . O34B O 0.1921(9) 0.6099(11) 0.1489(9) 0.104(6) Uiso 1 1 d . . . O41B O 0.0796(10) 0.5874(13) 0.1214(10) 0.126(7) Uiso 1 1 d . . . O42B O 0.0084(6) 0.5408(8) 0.0784(6) 0.068(4) Uiso 1 1 d . . . O43B O 0.1300(5) 0.5192(7) 0.0770(5) 0.047(3) Uiso 1 1 d . . . O44B O 0.0525(6) 0.4728(8) 0.0154(6) 0.068(4) Uiso 1 1 d . . . C11B C 0.0901(11) 0.9754(14) -0.0414(8) 0.091(8) Uiso 1 1 d D . . C12B C 0.0957(8) 0.9844(10) -0.0957(8) 0.168(17) Uiso 1 1 d D . . C13B C 0.0444(10) 0.9632(17) -0.1391(10) 0.168(3) Uiso 1 1 d D . . H13D H 0.0133 0.9870 -0.1352 0.253 Uiso 1 1 calc R . . H13E H 0.0392 0.9163 -0.1358 0.253 Uiso 1 1 calc R . . H13F H 0.0470 0.9726 -0.1748 0.253 Uiso 1 1 calc R . . C14B C 0.1062(14) 1.0544(11) -0.1035(13) 0.168(3) Uiso 1 1 d D . . H14D H 0.0769 1.0811 -0.0988 0.253 Uiso 1 1 calc R . . H14E H 0.1072 1.0609 -0.1402 0.253 Uiso 1 1 calc R . . H14F H 0.1413 1.0674 -0.0767 0.253 Uiso 1 1 calc R . . C15B C 0.1424(11) 0.9443(16) -0.0987(14) 0.168(3) Uiso 1 1 d D . . H15D H 0.1763 0.9591 -0.0709 0.253 Uiso 1 1 calc R . . H15E H 0.1454 0.9491 -0.1347 0.253 Uiso 1 1 calc R . . H15F H 0.1361 0.8984 -0.0923 0.253 Uiso 1 1 calc R . . C16B C 0.0876(8) 1.0575(8) 0.0871(8) 0.059(5) Uiso 1 1 d D . . C17B C 0.1048(6) 1.1235(8) 0.1108(6) 0.073(6) Uiso 1 1 d D . . C18B C 0.1649(7) 1.1238(14) 0.1410(12) 0.168(3) Uiso 1 1 d D . . H18D H 0.1760 1.1668 0.1574 0.253 Uiso 1 1 calc R . . H18E H 0.1843 1.1142 0.1158 0.253 Uiso 1 1 calc R . . H18F H 0.1738 1.0906 0.1696 0.253 Uiso 1 1 calc R . . C19B C 0.0913(14) 1.1727(10) 0.0663(11) 0.168(3) Uiso 1 1 d D . . H19D H 0.1010 1.2163 0.0819 0.253 Uiso 1 1 calc R . . H19E H 0.0521 1.1710 0.0453 0.253 Uiso 1 1 calc R . . H19F H 0.1121 1.1631 0.0422 0.253 Uiso 1 1 calc R . . C20B C 0.0753(12) 1.1399(14) 0.1488(11) 0.168(3) Uiso 1 1 d D . . H20D H 0.0860 1.1836 0.1638 0.253 Uiso 1 1 calc R . . H20E H 0.0847 1.1080 0.1784 0.253 Uiso 1 1 calc R . . H20F H 0.0357 1.1388 0.1291 0.253 Uiso 1 1 calc R . . C21B C 0.1137(8) 0.8711(10) 0.1601(7) 0.061(5) Uiso 1 1 d D . . C22B C 0.1213(8) 0.8807(10) 0.2187(7) 1.9(9) Uiso 1 1 d D . . C23B C 0.0838(12) 0.9332(14) 0.2240(12) 0.168(3) Uiso 1 1 d D . . H23D H 0.0458 0.9193 0.2064 0.253 Uiso 1 1 calc R . . H23E H 0.0904 0.9730 0.2065 0.253 Uiso 1 1 calc R . . H23F H 0.0906 0.9418 0.2625 0.253 Uiso 1 1 calc R . . C24B C 0.1791(9) 0.9000(18) 0.2489(10) 0.168(3) Uiso 1 1 d D . . H24D H 0.1875 0.9404 0.2335 0.253 Uiso 1 1 calc R . . H24E H 0.2037 0.8653 0.2456 0.253 Uiso 1 1 calc R . . H24F H 0.1840 0.9067 0.2873 0.253 Uiso 1 1 calc R . . C25B C 0.1087(15) 0.8189(14) 0.2419(12) 0.168(3) Uiso 1 1 d D . . H25D H 0.0704 0.8070 0.2228 0.253 Uiso 1 1 calc R . . H25E H 0.1147 0.8250 0.2806 0.253 Uiso 1 1 calc R . . H25F H 0.1326 0.7841 0.2374 0.253 Uiso 1 1 calc R . . C26B C 0.2398(6) 0.8901(12) 0.1193(9) 0.081(7) Uiso 1 1 d D . . C27B C 0.2986(6) 0.9091(7) 0.1402(6) 0.053(4) Uiso 1 1 d D . . C28B C 0.3311(10) 0.8612(13) 0.1212(14) 0.168(3) Uiso 1 1 d D . . H28D H 0.3697 0.8740 0.1346 0.253 Uiso 1 1 calc R . . H28E H 0.3177 0.8603 0.0813 0.253 Uiso 1 1 calc R . . H28F H 0.3273 0.8178 0.1351 0.253 Uiso 1 1 calc R . . C29B C 0.3049(11) 0.9753(9) 0.1196(13) 0.168(3) Uiso 1 1 d D . . H29D H 0.3435 0.9880 0.1336 0.253 Uiso 1 1 calc R . . H29E H 0.2832 1.0067 0.1318 0.253 Uiso 1 1 calc R . . H29F H 0.2920 0.9746 0.0798 0.253 Uiso 1 1 calc R . . C30B C 0.3187(11) 0.9100(18) 0.2008(6) 0.168(3) Uiso 1 1 d D . . H30D H 0.3572 0.9234 0.2145 0.253 Uiso 1 1 calc R . . H30E H 0.3153 0.8663 0.2144 0.253 Uiso 1 1 calc R . . H30F H 0.2969 0.9409 0.2134 0.253 Uiso 1 1 calc R . . C31B C 0.1897(8) 0.6916(11) 0.0138(7) 0.065(5) Uiso 1 1 d D . . C32B C 0.2134(7) 0.7013(9) -0.0300(7) 0.123(11) Uiso 1 1 d D . . C33B C 0.1948(14) 0.7651(12) -0.0572(12) 0.168(3) Uiso 1 1 d D . . H33D H 0.1549 0.7650 -0.0742 0.253 Uiso 1 1 calc R . . H33E H 0.2114 0.7721 -0.0852 0.253 Uiso 1 1 calc R . . H33F H 0.2059 0.8002 -0.0303 0.253 Uiso 1 1 calc R . . C34B C 0.2743(7) 0.7007(2) -0.0058(12) 0.168(3) Uiso 1 1 d D . . H34D H 0.2898 0.7085 -0.0344 0.253 Uiso 1 1 calc R . . H34E H 0.2865 0.6582 0.0111 0.253 Uiso 1 1 calc R . . H34F H 0.2864 0.7349 0.0218 0.253 Uiso 1 1 calc R . . C35B C 0.1948(14) 0.6477(15) -0.0706(10) 0.168(3) Uiso 1 1 d D . . H35D H 0.1548 0.6469 -0.0853 0.253 Uiso 1 1 calc R . . H35E H 0.2084 0.6059 -0.0531 0.253 Uiso 1 1 calc R . . H35F H 0.2091 0.6551 -0.1002 0.253 Uiso 1 1 calc R . . C36B C 0.2244(8) 0.6463(11) 0.1609(8) 0.071(6) Uiso 1 1 d D . . C37B C 0.2770(8) 0.6226(10) 0.2010(8) 1.8(7) Uiso 1 1 d D . . C38B C 0.2785(14) 0.5500(10) 0.1995(15) 0.168(3) Uiso 1 1 d D . . H38D H 0.3128 0.5343 0.2261 0.253 Uiso 1 1 calc R . . H38E H 0.2760 0.5356 0.1630 0.253 Uiso 1 1 calc R . . H38F H 0.2476 0.5322 0.2083 0.253 Uiso 1 1 calc R . . C39B C 0.3236(9) 0.6495(18) 0.1870(15) 0.168(3) Uiso 1 1 d D . . H39D H 0.3241 0.6971 0.1903 0.253 Uiso 1 1 calc R . . H39E H 0.3193 0.6376 0.1495 0.253 Uiso 1 1 calc R . . H39F H 0.3580 0.6316 0.2118 0.253 Uiso 1 1 calc R . . C40B C 0.2815(14) 0.6445(18) 0.2566(8) 0.168(3) Uiso 1 1 d D . . H40D H 0.2801 0.6922 0.2576 0.253 Uiso 1 1 calc R . . H40E H 0.3162 0.6292 0.2829 0.253 Uiso 1 1 calc R . . H40F H 0.2510 0.6264 0.2660 0.253 Uiso 1 1 calc R . . C41B C 0.0416(8) 0.5588(10) 0.1227(7) 0.063(5) Uiso 1 1 d D . . C42B C 0.0417(8) 0.5292(10) 0.1747(7) 0.21(3) Uiso 1 1 d D . . C43B C 0.0479(15) 0.4571(10) 0.1723(13) 0.168(3) Uiso 1 1 d D . . H43D H 0.0469 0.4375 0.2061 0.253 Uiso 1 1 calc R . . H43E H 0.0829 0.4470 0.1680 0.253 Uiso 1 1 calc R . . H43F H 0.0179 0.4395 0.1414 0.253 Uiso 1 1 calc R . . C44B C -0.0109(11) 0.5445(18) 0.1830(13) 0.168(3) Uiso 1 1 d D . . H44D H -0.0107 0.5254 0.2173 0.253 Uiso 1 1 calc R . . H44E H -0.0413 0.5264 0.1528 0.253 Uiso 1 1 calc R . . H44F H -0.0151 0.5919 0.1841 0.253 Uiso 1 1 calc R . . C45B C 0.0881(12) 0.5562(17) 0.2208(8) 0.168(3) Uiso 1 1 d D . . H45D H 0.0873 0.5379 0.2551 0.253 Uiso 1 1 calc R . . H45E H 0.0848 0.6037 0.2216 0.253 Uiso 1 1 calc R . . H45F H 0.1228 0.5446 0.2162 0.253 Uiso 1 1 calc R . . C46B C 0.1136(13) 0.4714(10) 0.0406(12) 0.121(11) Uiso 1 1 d D . . C47B C 0.1304(7) 0.4018(10) 0.0511(7) 0.087(7) Uiso 1 1 d D . . C48B C 0.1036(13) 0.3723(16) 0.0875(12) 0.168(3) Uiso 1 1 d D . . H48D H 0.1156 0.3270 0.0954 0.253 Uiso 1 1 calc R . . H48E H 0.0638 0.3736 0.0696 0.253 Uiso 1 1 calc R . . H48F H 0.1138 0.3970 0.1216 0.253 Uiso 1 1 calc R . . C49B C 0.1910(8) 0.3979(17) 0.0777(13) 0.168(3) Uiso 1 1 d D . . H49D H 0.2020 0.3522 0.0844 0.253 Uiso 1 1 calc R . . H49E H 0.2021 0.4216 0.1123 0.253 Uiso 1 1 calc R . . H49F H 0.2086 0.4175 0.0539 0.253 Uiso 1 1 calc R . . C50B C 0.1135(14) 0.3655(15) -0.0014(10) 0.168(3) Uiso 1 1 d D . . H50D H 0.1258 0.3202 0.0054 0.253 Uiso 1 1 calc R . . H50E H 0.1301 0.3859 -0.0258 0.253 Uiso 1 1 calc R . . H50F H 0.0736 0.3667 -0.0182 0.253 Uiso 1 1 calc R . . N1A N 0.5000 0.254(3) 0.5000 0.139(16) Uiso 1 2 d S . . H1A1 H 0.4714 0.2816 0.4822 0.167 Uiso 0.50 1 calc PR . . H1A2 H 0.5286 0.2816 0.5178 0.167 Uiso 0.50 1 calc PR . . C1A C 0.5147(10) 0.2307(14) 0.4598(10) 0.077(6) Uiso 1 1 d . . . H1A3 H 0.5485 0.2054 0.4777 0.092 Uiso 1 1 calc R . . H1A4 H 0.4862 0.1983 0.4411 0.092 Uiso 1 1 calc R . . C2A C 0.5234(15) 0.2612(2) 0.4232(14) 0.115(10) Uiso 1 1 d . . . H2A1 H 0.5573 0.2876 0.4363 0.137 Uiso 1 1 calc R . . H2A2 H 0.4921 0.2886 0.4019 0.137 Uiso 1 1 calc R . . C3A C 0.532(2) 0.181(3) 0.383(2) 0.21(2) Uiso 1 1 d . . . H3A1 H 0.5403 0.1930 0.3509 0.308 Uiso 1 1 calc R . . H3A2 H 0.4975 0.1557 0.3720 0.308 Uiso 1 1 calc R . . H3A3 H 0.5614 0.1536 0.4070 0.308 Uiso 1 1 calc R . . N1B N 0.0000 0.734(2) 0.0000 0.104(10) Uiso 1 2 d S . . H1B1 H 0.0299 0.7082 0.0172 0.125 Uiso 0.50 1 calc PR . . H1B2 H -0.0299 0.7082 -0.0172 0.125 Uiso 0.50 1 calc PR . . C1B C 0.0109(10) 0.7806(12) -0.0367(9) 0.070(6) Uiso 1 1 d . . . H1B3 H 0.0449 0.8049 -0.0175 0.084 Uiso 1 1 calc R . . H1B4 H -0.0195 0.8122 -0.0495 0.084 Uiso 1 1 calc R . . C2B C 0.017(2) 0.743(3) -0.0869(2) 0.163(17) Uiso 1 1 d . . . H2B1 H 0.0399 0.7041 -0.0708 0.196 Uiso 1 1 calc R . . H2B2 H -0.0199 0.7252 -0.1068 0.196 Uiso 1 1 calc R . . C3B C 0.0348(14) 0.7621(18) -0.1238(14) 0.111(9) Uiso 1 1 d . . . H3B1 H 0.0340 0.7259 -0.1485 0.166 Uiso 1 1 calc R . . H3B2 H 0.0725 0.7777 -0.1071 0.166 Uiso 1 1 calc R . . H3B3 H 0.0117 0.7976 -0.1441 0.166 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 Fe1A 0.102(4) 0.053(3) 0.100(4) 0.000 -0.021(4) 0.000 Fe2A 0.0440(15) 0.0380(13) 0.0459(14) 0.0065(11) 0.0039(12) 0.0038(11) Fe3A 0.082(3) 0.0541(2) 0.106(3) -0.035(2) -0.050(2) 0.0121(2) Fe4A 0.0207(10) 0.0364(12) 0.0336(11) -0.0036(10) -0.0061(9) 0.0022(9) Fe5A 0.069(4) 0.039(3) 0.229(9) 0.000 -0.077(5) 0.000 Fe1B 0.049(2) 0.040(2) 0.0362(17) 0.000 -0.0044(16) 0.000 Fe2B 0.079(3) 0.045(2) 0.285(9) 0.014(3) -0.038(4) -0.006(2) Fe3B 0.0320(11) 0.0382(12) 0.0371(11) 0.0106(10) 0.0088(9) 0.0032(10) Fe4B 0.0386(2) 0.059(2) 0.266(8) 0.041(3) -0.014(3) -0.0118(16) Fe5B 0.0278(16) 0.0336(17) 0.054(2) 0.000 0.0129(15) 0.000 _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 Fe1A O11A 1.86(4) . ? Fe1A O11A 1.86(4) 2_656 ? Fe1A F1A 1.949(9) . ? Fe1A F1A 1.949(9) 2_656 ? Fe1A O13A 2.19(2) . ? Fe1A O13A 2.19(2) 2_656 ? Fe2A O12A 1.945(16) . ? Fe2A O23A 1.951(17) . ? Fe2A F2A 1.976(11) . ? Fe2A F1A 2.024(8) . ? Fe2A O14A 2.039(17) . ? Fe2A O21A 2.060(16) . ? Fe3A O31A 1.788(18) . ? Fe3A F2A 1.899(12) . ? Fe3A F3A 1.932(10) . ? Fe3A O24A 1.981(14) . ? Fe3A O33A 2.07(2) . ? Fe3A O22A 2.10(2) . ? Fe4A O41A 1.852(14) . ? Fe4A O34A 1.919(16) . ? Fe4A O32A 1.988(17) . ? Fe4A F3A 2.000(10) . ? Fe4A O43A 2.003(16) . ? Fe4A F4A 2.004(8) . ? Fe5A F4A 1.903(9) 2_656 ? Fe5A F4A 1.903(9) . ? Fe5A O44A 2.18(2) . ? Fe5A O44A 2.18(2) 2_656 ? O11A C11A 1.26(4) . ? O12A C11A 1.38(2) . ? O13A C16A 1.14(2) . ? O14A C16A 1.25(2) . ? O21A C21A 1.12(2) . ? O22A C21A 1.15(3) . ? O23A C26A 1.28(2) . ? O24A C26A 1.35(2) . ? O31A C31A 1.44(2) . ? O32A C31A 1.30(2) . ? O33A C36A 1.16(2) . ? O34A C36A 1.32(2) . ? O41A C41A 1.31(2) . ? O42A C41A 0.98(2) . ? O43A C46A 1.09(2) . ? O44A C46A 1.41(3) . ? C11A C12A 1.49(5) . ? C12A C13A 1.49(4) . ? C12A C14A 1.49(4) . ? C12A C15A 1.49(4) . ? C16A C17A 1.49(5) . ? C17A C20A 1.49(4) . ? C17A C19A 1.49(4) . ? C17A C18A 1.49(4) . ? C21A C22A 1.49(5) . ? C22A C25A 1.49(4) . ? C22A C24A 1.49(4) . ? C22A C23A 1.49(4) . ? C26A C27A 1.49(5) . ? C27A C28A 1.49(4) . ? C27A C29A 1.49(4) . ? C27A C30A 1.49(4) . ? C31A C32A 1.49(5) . ? C32A C35A 1.49(4) . ? C32A C33A 1.49(4) . ? C32A C34A 1.49(4) . ? C36A C37A 1.49(5) . ? C37A C38A 1.49(4) . ? C37A C40A 1.49(4) . ? C37A C39A 1.49(4) . ? C41A C42A 1.49(5) . ? C42A C45A 1.49(4) . ? C42A C44A 1.49(4) . ? C42A C43A 1.49(4) . ? C46A C47A 1.49(5) . ? C47A C49A 1.49(4) . ? C47A C48A 1.49(4) . ? C47A C50A 1.49(4) . ? Fe1B O13B 1.873(14) . ? Fe1B O13B 1.873(14) 2 ? Fe1B O11B 1.917(16) . ? Fe1B O11B 1.917(16) 2 ? Fe1B F1B 1.993(11) 2 ? Fe1B F1B 1.993(11) . ? Fe2B O21B 1.72(3) . ? Fe2B O14B 1.78(4) . ? Fe2B F2B 1.897(10) . ? Fe2B F1B 1.911(12) . ? Fe2B O23B 2.11(2) . ? Fe2B O12B 2.34(2) . ? Fe3B O31B 1.908(14) . ? Fe3B O24B 1.924(14) . ? Fe3B F3B 1.936(10) . ? Fe3B O33B 1.948(15) . ? Fe3B F2B 1.973(9) . ? Fe3B O22B 1.99(2) . ? Fe4B O32B 1.72(2) . ? Fe4B O43B 1.809(13) . ? Fe4B F4B 1.921(12) . ? Fe4B O41B 2.00(3) . ? Fe4B F3B 2.053(10) . ? Fe4B O34B 2.12(2) . ? Fe5B O44B 1.958(16) 2 ? Fe5B O44B 1.958(16) . ? Fe5B O42B 1.990(15) 2 ? Fe5B O42B 1.990(15) . ? Fe5B F4B 2.020(11) . ? Fe5B F4B 2.020(11) 2 ? O11B C11B 1.21(3) 2 ? O12B C11B 1.07(3) . ? O13B C16B 1.27(2) . ? O14B C16B 1.48(4) . ? O21B C21B 1.07(3) . ? O22B C21B 1.67(3) . ? O23B C26B 1.15(3) . ? O24B C26B 1.36(3) . ? O31B C31B 1.22(2) . ? O32B C31B 1.76(3) . ? O33B C36B 1.25(3) . ? O34B C36B 1.09(3) . ? O41B C41B 1.16(3) . ? O42B C41B 1.24(2) . ? O43B C46B 1.33(3) . ? O44B C46B 1.50(3) . ? C11B O11B 1.21(3) 2 ? C11B C12B 1.49(5) . ? C12B C14B 1.49(4) . ? C12B C13B 1.49(4) . ? C12B C15B 1.49(4) . ? C16B C17B 1.49(5) . ? C17B C19B 1.49(4) . ? C17B C20B 1.49(4) . ? C17B C18B 1.49(4) . ? C21B C22B 1.49(5) . ? C22B C24B 1.49(4) . ? C22B C23B 1.49(4) . ? C22B C25B 1.49(4) . ? C26B C27B 1.49(5) . ? C27B C28B 1.49(4) . ? C27B C30B 1.49(4) . ? C27B C29B 1.49(4) . ? C31B C32B 1.49(5) . ? C32B C34B 1.49(4) . ? C32B C35B 1.49(4) . ? C32B C33B 1.49(4) . ? C36B C37B 1.49(5) . ? C37B C39B 1.49(4) . ? C37B C38B 1.49(4) . ? C37B C40B 1.49(4) . ? C41B C42B 1.49(5) . ? C42B C44B 1.49(4) . ? C42B C45B 1.49(4) . ? C42B C43B 1.49(4) . ? C46B C47B 1.49(5) . ? C47B C50B 1.49(4) . ? C47B C49B 1.49(4) . ? C47B C48B 1.49(4) . ? N1A C1A 1.33(3) . ? N1A C1A 1.33(3) 2_656 ? C1A C2A 1.23(4) . ? C2A C3A 2.01(7) . ? N1B C1B 1.45(3) . ? N1B C1B 1.45(3) 2 ? C1B C2B 1.59(5) . ? C2B C3B 1.27(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11A Fe1A O11A 176(2) . 2_656 ? O11A Fe1A F1A 93.1(12) . . ? O11A Fe1A F1A 84.2(11) 2_656 . ? O11A Fe1A F1A 84.2(11) . 2_656 ? O11A Fe1A F1A 93.1(11) 2_656 2_656 ? F1A Fe1A F1A 84.3(5) . 2_656 ? O11A Fe1A O13A 104.1(12) . . ? O11A Fe1A O13A 78.1(12) 2_656 . ? F1A Fe1A O13A 84.4(6) . . ? F1A Fe1A O13A 166.3(6) 2_656 . ? O11A Fe1A O13A 78.1(12) . 2_656 ? O11A Fe1A O13A 104.1(12) 2_656 2_656 ? F1A Fe1A O13A 166.3(6) . 2_656 ? F1A Fe1A O13A 84.4(6) 2_656 2_656 ? O13A Fe1A O13A 107.8(12) . 2_656 ? O12A Fe2A O23A 87.8(7) . . ? O12A Fe2A F2A 90.0(6) . . ? O23A Fe2A F2A 91.0(6) . . ? O12A Fe2A F1A 92.0(6) . . ? O23A Fe2A F1A 179.1(6) . . ? F2A Fe2A F1A 88.2(4) . . ? O12A Fe2A O14A 96.5(7) . . ? O23A Fe2A O14A 94.5(7) . . ? F2A Fe2A O14A 171.7(6) . . ? F1A Fe2A O14A 86.4(5) . . ? O12A Fe2A O21A 177.0(7) . . ? O23A Fe2A O21A 92.2(7) . . ? F2A Fe2A O21A 87.0(5) . . ? F1A Fe2A O21A 88.0(5) . . ? O14A Fe2A O21A 86.5(6) . . ? O31A Fe3A F2A 95.9(7) . . ? O31A Fe3A F3A 96.6(7) . . ? F2A Fe3A F3A 91.7(4) . . ? O31A Fe3A O24A 92.0(7) . . ? F2A Fe3A O24A 98.1(5) . . ? F3A Fe3A O24A 166.3(6) . . ? O31A Fe3A O33A 90.0(8) . . ? F2A Fe3A O33A 174.0(7) . . ? F3A Fe3A O33A 86.4(7) . . ? O24A Fe3A O33A 82.9(7) . . ? O31A Fe3A O22A 176.6(9) . . ? F2A Fe3A O22A 87.4(7) . . ? F3A Fe3A O22A 84.1(7) . . ? O24A Fe3A O22A 86.8(8) . . ? O33A Fe3A O22A 86.7(9) . . ? O41A Fe4A O34A 87.0(7) . . ? O41A Fe4A O32A 174.9(7) . . ? O34A Fe4A O32A 89.8(7) . . ? O41A Fe4A F3A 92.5(5) . . ? O34A Fe4A F3A 91.4(6) . . ? O32A Fe4A F3A 91.5(6) . . ? O41A Fe4A O43A 83.7(6) . . ? O34A Fe4A O43A 90.1(7) . . ? O32A Fe4A O43A 92.3(7) . . ? F3A Fe4A O43A 175.9(5) . . ? O41A Fe4A F4A 94.5(5) . . ? O34A Fe4A F4A 178.5(6) . . ? O32A Fe4A F4A 88.7(5) . . ? F3A Fe4A F4A 88.6(4) . . ? O43A Fe4A F4A 90.0(5) . . ? F4A Fe5A F4A 87.0(6) 2_656 . ? F4A Fe5A O44A 160.0(6) 2_656 . ? F4A Fe5A O44A 99.4(6) . . ? F4A Fe5A O44A 99.4(6) 2_656 2_656 ? F4A Fe5A O44A 160.0(6) . 2_656 ? O44A Fe5A O44A 80.9(11) . 2_656 ? Fe1A F1A Fe2A 120.2(4) . . ? Fe3A F2A Fe2A 120.6(6) . . ? Fe3A F3A Fe4A 123.7(5) . . ? Fe5A F4A Fe4A 120.4(5) . . ? C11A O11A Fe1A 139(3) . . ? C11A O12A Fe2A 134(1) . . ? C16A O13A Fe1A 124(2) . . ? C16A O14A Fe2A 136(1) . . ? C21A O21A Fe2A 143(1) . . ? C21A O22A Fe3A 133(2) . . ? C26A O23A Fe2A 139(1) . . ? C26A O24A Fe3A 123(1) . . ? C31A O31A Fe3A 135(1) . . ? C31A O32A Fe4A 134(1) . . ? C36A O33A Fe3A 132(2) . . ? C36A O34A Fe4A 135(1) . . ? C41A O41A Fe4A 146(1) . . ? C46A O43A Fe4A 145(1) . . ? C46A O44A Fe5A 114(1) . . ? O11A C11A O12A 122(2) . . ? O11A C11A C12A 124(2) . . ? O12A C11A C12A 114(1) . . ? C11A C12A C13A 110(3) . . ? C11A C12A C14A 109(3) . . ? C13A C12A C14A 110(2) . . ? C11A C12A C15A 110(3) . . ? C13A C12A C15A 109(2) . . ? C14A C12A C15A 109(2) . . ? O13A C16A O14A 104(2) . . ? O13A C16A C17A 117(2) . . ? O14A C16A C17A 125(2) . . ? C16A C17A C20A 110(3) . . ? C16A C17A C19A 110(3) . . ? C20A C17A C19A 110(2) . . ? C16A C17A C18A 109(3) . . ? C20A C17A C18A 109(2) . . ? C19A C17A C18A 110(2) . . ? O21A C21A O22A 117(2) . . ? O21A C21A C22A 109(2) . . ? O22A C21A C22A 131(2) . . ? C25A C22A C24A 110(2) . . ? C25A C22A C23A 109(2) . . ? C24A C22A C23A 110(2) . . ? C25A C22A C21A 109(3) . . ? C24A C22A C21A 110(3) . . ? C23A C22A C21A 110(3) . . ? O23A C26A O24A 110(1) . . ? O23A C26A C27A 120(1) . . ? O24A C26A C27A 114(1) . . ? C26A C27A C28A 109(3) . . ? C26A C27A C29A 110(3) . . ? C28A C27A C29A 109(2) . . ? C26A C27A C30A 110(3) . . ? C28A C27A C30A 109(2) . . ? C29A C27A C30A 109(2) . . ? O32A C31A O31A 120(1) . . ? O32A C31A C32A 124(1) . . ? O31A C31A C32A 114(1) . . ? C31A C32A C35A 110(3) . . ? C31A C32A C33A 110(3) . . ? C35A C32A C33A 109(2) . . ? C31A C32A C34A 110(3) . . ? C35A C32A C34A 109(2) . . ? C33A C32A C34A 109(2) . . ? O33A C36A O34A 125(2) . . ? O33A C36A C37A 119(2) . . ? O34A C36A C37A 116(1) . . ? C38A C37A C40A 109(2) . . ? C38A C37A C39A 109(2) . . ? C40A C37A C39A 109(2) . . ? C38A C37A C36A 110(3) . . ? C40A C37A C36A 110(3) . . ? C39A C37A C36A 109(3) . . ? O42A C41A O41A 115(2) . . ? O42A C41A C42A 123(2) . . ? O41A C41A C42A 122(2) . . ? C45A C42A C44A 109(2) . . ? C45A C42A C43A 109(2) . . ? C44A C42A C43A 109(2) . . ? C45A C42A C41A 109(3) . . ? C44A C42A C41A 110(3) . . ? C43A C42A C41A 110(3) . . ? O43A C46A O44A 115(2) . . ? O43A C46A C47A 125(2) . . ? O44A C46A C47A 113(1) . . ? C46A C47A C49A 110(3) . . ? C46A C47A C48A 110(3) . . ? C49A C47A C48A 109(2) . . ? C46A C47A C50A 110(3) . . ? C49A C47A C50A 109(2) . . ? C48A C47A C50A 109(2) . . ? O13B Fe1B O13B 93.0(9) . 2 ? O13B Fe1B O11B 85.3(6) . . ? O13B Fe1B O11B 86.4(6) 2 . ? O13B Fe1B O11B 86.4(6) . 2 ? O13B Fe1B O11B 85.3(6) 2 2 ? O11B Fe1B O11B 168.0(9) . 2 ? O13B Fe1B F1B 176.9(6) . 2 ? O13B Fe1B F1B 90.0(5) 2 2 ? O11B Fe1B F1B 95.7(6) . 2 ? O11B Fe1B F1B 93.0(6) 2 2 ? O13B Fe1B F1B 90.0(5) . . ? O13B Fe1B F1B 176.9(6) 2 . ? O11B Fe1B F1B 93.0(6) . . ? O11B Fe1B F1B 95.7(6) 2 . ? F1B Fe1B F1B 87.0(6) 2 . ? O21B Fe2B O14B 80.0(15) . . ? O21B Fe2B F2B 98.5(10) . . ? O14B Fe2B F2B 177.7(13) . . ? O21B Fe2B F1B 97.1(10) . . ? O14B Fe2B F1B 94.4(12) . . ? F2B Fe2B F1B 87.6(5) . . ? O21B Fe2B O23B 94.6(10) . . ? O14B Fe2B O23B 90.0(13) . . ? F2B Fe2B O23B 88.3(6) . . ? F1B Fe2B O23B 168.0(8) . . ? O21B Fe2B O12B 174.8(11) . . ? O14B Fe2B O12B 96.4(13) . . ? F2B Fe2B O12B 84.9(6) . . ? F1B Fe2B O12B 86.9(6) . . ? O23B Fe2B O12B 81.5(8) . . ? O31B Fe3B O24B 99.0(6) . . ? O31B Fe3B F3B 93.5(5) . . ? O24B Fe3B F3B 167.1(5) . . ? O31B Fe3B O33B 98.1(6) . . ? O24B Fe3B O33B 87.9(6) . . ? F3B Fe3B O33B 87.7(5) . . ? O31B Fe3B F2B 92.7(5) . . ? O24B Fe3B F2B 93.9(5) . . ? F3B Fe3B F2B 88.2(4) . . ? O33B Fe3B F2B 168.7(5) . . ? O31B Fe3B O22B 173.1(8) . . ? O24B Fe3B O22B 86.2(8) . . ? F3B Fe3B O22B 81.5(7) . . ? O33B Fe3B O22B 86.5(8) . . ? F2B Fe3B O22B 82.5(7) . . ? O32B Fe4B O43B 97.7(8) . . ? O32B Fe4B F4B 93.8(8) . . ? O43B Fe4B F4B 98.2(6) . . ? O32B Fe4B O41B 177.3(10) . . ? O43B Fe4B O41B 80.6(9) . . ? F4B Fe4B O41B 88.5(8) . . ? O32B Fe4B F3B 92.9(8) . . ? O43B Fe4B F3B 169.2(6) . . ? F4B Fe4B F3B 83.3(4) . . ? O41B Fe4B F3B 88.8(8) . . ? O32B Fe4B O34B 92.1(9) . . ? O43B Fe4B O34B 88.2(7) . . ? F4B Fe4B O34B 170.6(7) . . ? O41B Fe4B O34B 85.7(10) . . ? F3B Fe4B O34B 89.2(7) . . ? O44B Fe5B O44B 82.2(9) 2 . ? O44B Fe5B O42B 86.3(6) 2 2 ? O44B Fe5B O42B 90.2(6) . 2 ? O44B Fe5B O42B 90.2(6) 2 . ? O44B Fe5B O42B 86.3(6) . . ? O42B Fe5B O42B 175.4(9) 2 . ? O44B Fe5B F4B 175.5(6) 2 . ? O44B Fe5B F4B 94.1(5) . . ? O42B Fe5B F4B 91.3(5) 2 . ? O42B Fe5B F4B 91.9(5) . . ? O44B Fe5B F4B 94.1(5) 2 2 ? O44B Fe5B F4B 175.5(6) . 2 ? O42B Fe5B F4B 91.9(5) 2 2 ? O42B Fe5B F4B 91.3(5) . 2 ? F4B Fe5B F4B 89.8(6) . 2 ? Fe2B F1B Fe1B 121.7(6) . . ? Fe2B F2B Fe3B 120.9(5) . . ? Fe3B F3B Fe4B 121.2(5) . . ? Fe4B F4B Fe5B 119.9(6) . . ? C11B O11B Fe1B 136(2) 2 . ? C11B O12B Fe2B 125(2) . . ? C16B O13B Fe1B 143(1) . . ? C16B O14B Fe2B 136(2) . . ? C21B O21B Fe2B 128(2) . . ? C21B O22B Fe3B 127(2) . . ? C26B O23B Fe2B 126(2) . . ? C26B O24B Fe3B 135(1) . . ? C31B O31B Fe3B 139(1) . . ? Fe4B O32B C31B 135(1) . . ? C36B O33B Fe3B 136(1) . . ? C36B O34B Fe4B 127(2) . . ? C41B O41B Fe4B 144(2) . . ? C41B O42B Fe5B 138(1) . . ? C46B O43B Fe4B 135(1) . . ? C46B O44B Fe5B 132(1) . . ? O12B C11B O11B 132(2) . 2 ? O12B C11B C12B 116(2) . . ? O11B C11B C12B 109(2) 2 . ? C14B C12B C13B 109(2) . . ? C14B C12B C15B 109(2) . . ? C13B C12B C15B 109(2) . . ? C14B C12B C11B 109(3) . . ? C13B C12B C11B 110(3) . . ? C15B C12B C11B 109(3) . . ? O13B C16B O14B 113(2) . . ? O13B C16B C17B 121(2) . . ? O14B C16B C17B 123(2) . . ? C19B C17B C20B 109(2) . . ? C19B C17B C18B 109(2) . . ? C20B C17B C18B 109(2) . . ? C19B C17B C16B 109(3) . . ? C20B C17B C16B 110(3) . . ? C18B C17B C16B 110(3) . . ? O21B C21B C22B 115(2) . . ? O21B C21B O22B 113(2) . . ? C22B C21B O22B 107(1) . . ? C24B C22B C23B 109(2) . . ? C24B C22B C25B 109(2) . . ? C23B C22B C25B 109(2) . . ? C24B C22B C21B 110(3) . . ? C23B C22B C21B 109(3) . . ? C25B C22B C21B 110(3) . . ? O23B C26B O24B 120(2) . . ? O23B C26B C27B 123(2) . . ? O24B C26B C27B 117(2) . . ? C26B C27B C28B 110(3) . . ? C26B C27B C30B 110(3) . . ? C28B C27B C30B 109(2) . . ? C26B C27B C29B 109(3) . . ? C28B C27B C29B 109(2) . . ? C30B C27B C29B 109(2) . . ? O31B C31B C32B 115(2) . . ? O31B C31B O32B 112(1) . . ? C32B C31B O32B 132(2) . . ? C34B C32B C35B 109(2) . . ? C34B C32B C33B 109(2) . . ? C35B C32B C33B 109(2) . . ? C34B C32B C31B 110(3) . . ? C35B C32B C31B 109(3) . . ? C33B C32B C31B 110(3) . . ? O34B C36B O33B 121(2) . . ? O34B C36B C37B 114(2) . . ? O33B C36B C37B 120(2) . . ? C39B C37B C38B 109(2) . . ? C39B C37B C40B 109(2) . . ? C38B C37B C40B 109(2) . . ? C39B C37B C36B 110(3) . . ? C38B C37B C36B 109(3) . . ? C40B C37B C36B 110(3) . . ? O41B C41B O42B 117(2) . . ? O41B C41B C42B 120(2) . . ? O42B C41B C42B 121(2) . . ? C41B C42B C44B 109(3) . . ? C41B C42B C45B 110(3) . . ? C44B C42B C45B 109(2) . . ? C41B C42B C43B 109(3) . . ? C44B C42B C43B 109(2) . . ? C45B C42B C43B 109(2) . . ? O43B C46B C47B 125(2) . . ? O43B C46B O44B 109(2) . . ? C47B C46B O44B 107(2) . . ? C50B C47B C49B 109(2) . . ? C50B C47B C48B 109(2) . . ? C49B C47B C48B 109(2) . . ? C50B C47B C46B 110(3) . . ? C49B C47B C46B 110(3) . . ? C48B C47B C46B 110(3) . . ? C1A N1A C1A 137(5) . 2_656 ? C2A C1A N1A 128(3) . . ? C1A C2A C3A 94(3) . . ? C1B N1B C1B 98(3) . 2 ? N1B C1B C2B 109(3) . . ? C3B C2B C1B 130(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.592 _refine_diff_density_min -1.883 _refine_diff_density_rms 0.211