# ja9831094.cif data_sir _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe2(m-O2CAr)2(O2CAr)2(THF)2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 Cl2 Fe O5' _chemical_formula_weight 813.56 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' 'Fe' 'Fe' 0.3463 0.8444 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7768(3) _cell_length_b 14.2356(3) _cell_length_c 15.1219(4) _cell_angle_alpha 107.5490(10) _cell_angle_beta 98.4140(10) _cell_angle_gamma 105.7620(10) _cell_volume 2061.87(9) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.733806 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12551 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8751 _reflns_number_gt 5805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1000P)^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_number_reflns 8751 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _refine_ls_shift/su_max 0.384 _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 Fe1 Fe 0.87293(4) -0.46309(3) 1.09179(3) 0.03150(13) Uani 1 1 d . . . O1 O 0.78476(19) -0.45102(16) 1.20308(13) 0.0402(5) Uani 1 1 d . . . O1T O 0.7376(2) -0.40411(16) 1.03202(14) 0.0467(5) Uani 1 1 d . . . O2 O 0.95592(19) -0.50446(15) 1.22212(13) 0.0401(5) Uani 1 1 d . . . O3 O 1.03631(19) -0.36830(15) 1.08513(14) 0.0433(5) Uani 1 1 d . . . O4 O 0.80089(19) -0.60120(14) 0.98287(13) 0.0408(5) Uani 1 1 d . . . C1 C 1.0479(4) 0.0088(3) 1.3230(3) 0.0687(11) Uani 1 1 d . . . H1A H 0.9732 0.0085 1.2773 0.103 Uiso 1 1 calc R . . H1B H 1.1232 0.0082 1.2937 0.103 Uiso 1 1 calc R . . H1C H 1.0745 0.0718 1.3806 0.103 Uiso 1 1 calc R . . C1C C 0.5100(3) -0.5047(3) 0.6419(2) 0.0551(8) Uani 1 1 d . . . H1C1 H 0.4980 -0.4474 0.6914 0.083 Uiso 1 1 calc R . . H1C2 H 0.4264 -0.5434 0.5924 0.083 Uiso 1 1 calc R . . H1C3 H 0.5800 -0.4762 0.6131 0.083 Uiso 1 1 calc R . . C1T C 0.6766(4) -0.4342(3) 0.9334(2) 0.0630(10) Uani 1 1 d . . . H1TA H 0.6361 -0.5113 0.9038 0.076 Uiso 1 1 calc R . . H1TB H 0.7432 -0.4103 0.8993 0.076 Uiso 1 1 calc R . . C2 C 1.0064(3) -0.0865(2) 1.3498(2) 0.0501(8) Uani 1 1 d . . . C2C C 0.5493(3) -0.5773(2) 0.68626(19) 0.0406(7) Uani 1 1 d . . . C2T C 0.5721(4) -0.3844(3) 0.9277(3) 0.0795(13) Uani 1 1 d . . . H2TA H 0.5746 -0.3541 0.8768 0.095 Uiso 1 1 calc R . . H2TB H 0.4826 -0.4362 0.9137 0.095 Uiso 1 1 calc R . . C3 C 0.9035(3) -0.1049(2) 1.3937(2) 0.0522(8) Uani 1 1 d . . . H3B H 0.8580 -0.0557 1.4075 0.063 Uiso 1 1 calc R . . C3C C 0.4553(3) -0.6489(2) 0.7081(2) 0.0427(7) Uani 1 1 d . . . H3CA H 0.3659 -0.6495 0.6976 0.051 Uiso 1 1 calc R . . C3T C 0.6036(5) -0.3011(4) 1.0230(3) 0.0851(14) Uani 1 1 d . . . H3TA H 0.5271 -0.3124 1.0523 0.102 Uiso 1 1 calc R . . H3TB H 0.6240 -0.2316 1.0168 0.102 Uiso 1 1 calc R . . C4 C 0.8643(3) -0.1927(2) 1.4181(2) 0.0479(8) Uani 1 1 d . . . H4A H 0.7939 -0.2020 1.4493 0.057 Uiso 1 1 calc R . . C4C C 0.4874(3) -0.7195(2) 0.74480(19) 0.0387(7) Uani 1 1 d . . . H4CA H 0.4197 -0.7693 0.7567 0.046 Uiso 1 1 calc R . . C4T C 0.7227(4) -0.3076(3) 1.0833(2) 0.0604(10) Uani 1 1 d . . . H4TA H 0.8032 -0.2482 1.0928 0.072 Uiso 1 1 calc R . . H4TB H 0.7081 -0.3061 1.1467 0.072 Uiso 1 1 calc R . . C5 C 0.9267(3) -0.2679(2) 1.39763(19) 0.0390(7) Uani 1 1 d . . . C5C C 0.6196(3) -0.7182(2) 0.76467(18) 0.0331(6) Uani 1 1 d . . . C6 C 1.0329(3) -0.2482(2) 1.3554(2) 0.0497(8) Uani 1 1 d . . . H6A H 1.0803 -0.2961 1.3428 0.060 Uiso 1 1 calc R . . C6C C 0.7149(3) -0.6442(2) 0.74589(19) 0.0363(6) Uani 1 1 d . . . H6CA H 0.8053 -0.6403 0.7601 0.044 Uiso 1 1 calc R . . C7 C 1.0705(3) -0.1599(3) 1.3315(2) 0.0554(9) Uani 1 1 d . . . H7A H 1.1422 -0.1494 1.3017 0.067 Uiso 1 1 calc R . . C7C C 0.6800(3) -0.5755(2) 0.70657(19) 0.0392(7) Uani 1 1 d . . . H7CA H 0.7469 -0.5263 0.6934 0.047 Uiso 1 1 calc R . . C8 C 0.8830(3) -0.3636(2) 1.4213(2) 0.0407(7) Uani 1 1 d . . . C8C C 0.6526(3) -0.7980(2) 0.79949(18) 0.0344(6) Uani 1 1 d . . . C9 C 0.8704(3) -0.3532(3) 1.5141(2) 0.0515(8) Uani 1 1 d . . . H9A H 0.8871 -0.2856 1.5597 0.062 Uiso 1 1 calc R . . C9C C 0.5757(3) -0.9030(2) 0.7527(2) 0.0442(7) Uani 1 1 d . . . H9CA H 0.5006 -0.9221 0.7013 0.053 Uiso 1 1 calc R . . C10 C 0.8346(4) -0.4384(3) 1.5402(2) 0.0638(10) Uani 1 1 d . . . H10A H 0.8300 -0.4293 1.6044 0.077 Uiso 1 1 calc R . . C10C C 0.6068(3) -0.9800(2) 0.7799(2) 0.0520(8) Uani 1 1 d . . . H10B H 0.5529 -1.0512 0.7477 0.062 Uiso 1 1 calc R . . C11 C 0.8050(3) -0.5378(3) 1.4745(2) 0.0555(9) Uani 1 1 d . . . H11A H 0.7795 -0.5963 1.4939 0.067 Uiso 1 1 calc R . . C11C C 0.7157(3) -0.9533(2) 0.8534(2) 0.0466(7) Uani 1 1 d . . . H11B H 0.7369 -1.0069 0.8709 0.056 Uiso 1 1 calc R . . C12 C 0.8120(3) -0.5536(2) 1.3792(2) 0.0429(7) Uani 1 1 d . . . C12C C 0.7965(3) -0.8489(2) 0.90348(19) 0.0366(6) Uani 1 1 d . . . C13 C 0.8536(3) -0.4648(2) 1.35462(19) 0.0358(6) Uani 1 1 d . . . C13C C 0.7631(3) -0.7712(2) 0.87571(18) 0.0320(6) Uani 1 1 d . . . C14 C 0.8664(3) -0.4757(2) 1.25334(19) 0.0340(6) Uani 1 1 d . . . C14C C 0.8488(3) -0.6585(2) 0.92856(18) 0.0320(6) Uani 1 1 d . . . C15 C 0.7706(3) -0.6621(2) 1.3095(2) 0.0425(7) Uani 1 1 d . . . C15C C 0.9115(3) -0.8239(2) 0.9843(2) 0.0370(6) Uani 1 1 d . . . C16 C 0.8103(3) -0.7377(3) 1.3344(3) 0.0616(9) Uani 1 1 d . . . H16A H 0.8643 -0.7195 1.3967 0.074 Uiso 1 1 calc R . . C16C C 1.0009(3) -0.8792(2) 0.9737(2) 0.0441(7) Uani 1 1 d . . . H16B H 0.9905 -0.9305 0.9133 0.053 Uiso 1 1 calc R . . C17 C 0.7721(4) -0.8394(3) 1.2696(3) 0.0696(11) Uani 1 1 d . . . H17A H 0.8000 -0.8896 1.2889 0.084 Uiso 1 1 calc R . . C17C C 1.1039(3) -0.8605(2) 1.0497(2) 0.0479(8) Uani 1 1 d . . . H17B H 1.1642 -0.8983 1.0401 0.058 Uiso 1 1 calc R . . C18 C 0.6953(4) -0.8696(3) 1.1784(3) 0.0610(10) Uani 1 1 d . . . C18C C 1.1216(3) -0.7881(2) 1.1394(2) 0.0436(7) Uani 1 1 d . . . C19 C 0.6617(5) -0.9792(3) 1.1053(3) 0.0910(15) Uani 1 1 d . . . H19A H 0.7074 -1.0184 1.1330 0.136 Uiso 1 1 calc R . . H19B H 0.6906 -0.9744 1.0479 0.136 Uiso 1 1 calc R . . H19C H 0.5653 -1.0152 1.0882 0.136 Uiso 1 1 calc R . . C19C C 1.2313(4) -0.7714(3) 1.2240(2) 0.0625(10) Uani 1 1 d . . . H19D H 1.2067 -0.8301 1.2464 0.094 Uiso 1 1 calc R . . H19E H 1.2431 -0.7062 1.2759 0.094 Uiso 1 1 calc R . . H19F H 1.3146 -0.7670 1.2042 0.094 Uiso 1 1 calc R . . C20 C 0.6507(3) -0.7956(3) 1.1544(3) 0.0550(8) Uani 1 1 d . . . H20A H 0.5935 -0.8149 1.0930 0.066 Uiso 1 1 calc R . . C20C C 1.0348(3) -0.7314(2) 1.1497(2) 0.0456(7) Uani 1 1 d . . . H20B H 1.0465 -0.6797 1.2101 0.055 Uiso 1 1 calc R . . C21 C 0.6883(3) -0.6937(2) 1.2187(2) 0.0457(7) Uani 1 1 d . . . H21A H 0.6571 -0.6445 1.2002 0.055 Uiso 1 1 calc R . . C21C C 0.9317(3) -0.7484(2) 1.0743(2) 0.0403(7) Uani 1 1 d . . . H21B H 0.8739 -0.7084 1.0837 0.048 Uiso 1 1 calc R . . C10S C 1.5019(5) 0.1605(5) 1.4943(3) 0.0999(17) Uani 1 1 d . . . Cl1A Cl 1.4559(5) 0.2406(4) 1.4312(3) 0.0644(11) Uani 0.434(3) 1 d P A 1 Cl2A Cl 1.6322(4) 0.1349(3) 1.4877(3) 0.1248(15) Uani 0.434(3) 1 d P A 1 Cl1 Cl 1.3733(2) 0.06171(15) 1.48742(13) 0.0776(7) Uani 0.566(3) 1 d P A 2 Cl2 Cl 1.4624(8) 0.2383(6) 1.4330(5) 0.169(3) Uani 0.566(3) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0278(2) 0.0364(2) 0.0279(2) 0.00737(16) 0.00673(15) 0.01189(16) O1 0.0381(11) 0.0535(12) 0.0330(10) 0.0168(9) 0.0103(9) 0.0191(10) O1T 0.0517(13) 0.0593(13) 0.0314(10) 0.0078(9) 0.0032(9) 0.0354(11) O2 0.0383(11) 0.0476(11) 0.0392(11) 0.0148(9) 0.0154(9) 0.0198(9) O3 0.0329(11) 0.0466(12) 0.0501(12) 0.0240(10) 0.0070(9) 0.0072(9) O4 0.0426(11) 0.0364(10) 0.0346(10) 0.0029(8) 0.0021(9) 0.0148(9) C1 0.087(3) 0.054(2) 0.060(2) 0.0197(18) 0.020(2) 0.016(2) C1C 0.0451(19) 0.067(2) 0.057(2) 0.0259(17) 0.0066(16) 0.0244(17) C1T 0.075(3) 0.075(2) 0.0399(18) 0.0155(17) 0.0021(17) 0.038(2) C2 0.053(2) 0.0435(17) 0.0410(17) 0.0049(14) 0.0095(15) 0.0082(15) C2C 0.0381(16) 0.0494(17) 0.0305(14) 0.0102(13) 0.0038(12) 0.0161(14) C2T 0.079(3) 0.097(3) 0.068(3) 0.028(2) -0.001(2) 0.050(3) C3 0.0487(19) 0.0411(17) 0.054(2) 0.0035(15) 0.0077(16) 0.0125(15) C3C 0.0274(14) 0.0570(18) 0.0397(16) 0.0095(14) 0.0054(12) 0.0183(14) C3T 0.101(3) 0.118(4) 0.064(3) 0.030(3) 0.020(2) 0.085(3) C4 0.0357(16) 0.0494(18) 0.0434(17) -0.0002(14) 0.0121(14) 0.0085(14) C4C 0.0289(14) 0.0446(16) 0.0347(15) 0.0091(13) 0.0059(12) 0.0070(12) C4T 0.083(3) 0.059(2) 0.050(2) 0.0162(17) 0.0154(18) 0.045(2) C5 0.0319(15) 0.0421(15) 0.0301(14) 0.0016(12) 0.0075(12) 0.0054(12) C5C 0.0297(14) 0.0398(15) 0.0244(13) 0.0054(11) 0.0059(11) 0.0106(12) C6 0.0467(18) 0.0431(17) 0.0555(19) 0.0083(15) 0.0235(16) 0.0140(15) C6C 0.0272(14) 0.0492(16) 0.0332(14) 0.0134(13) 0.0092(11) 0.0144(12) C7 0.053(2) 0.0511(19) 0.052(2) 0.0070(15) 0.0275(17) 0.0062(16) C7C 0.0322(15) 0.0524(17) 0.0365(15) 0.0200(13) 0.0106(12) 0.0139(13) C8 0.0318(15) 0.0508(17) 0.0330(15) 0.0088(13) 0.0096(12) 0.0101(13) C8C 0.0326(14) 0.0403(15) 0.0276(13) 0.0089(12) 0.0112(11) 0.0098(12) C9 0.0481(19) 0.0564(19) 0.0335(16) 0.0052(14) 0.0100(14) 0.0041(15) C9C 0.0412(17) 0.0455(17) 0.0347(15) 0.0068(13) 0.0049(13) 0.0081(14) C10 0.068(2) 0.077(3) 0.0326(17) 0.0187(17) 0.0114(16) 0.005(2) C10C 0.063(2) 0.0349(16) 0.0436(18) 0.0079(14) 0.0065(16) 0.0036(15) C11 0.052(2) 0.066(2) 0.0439(19) 0.0275(17) 0.0093(15) 0.0063(17) C11C 0.060(2) 0.0347(15) 0.0400(17) 0.0132(13) 0.0087(15) 0.0099(14) C12 0.0346(16) 0.0520(18) 0.0393(16) 0.0186(14) 0.0051(13) 0.0097(14) C12C 0.0433(16) 0.0362(14) 0.0301(14) 0.0104(12) 0.0123(12) 0.0128(13) C13 0.0284(14) 0.0464(16) 0.0302(14) 0.0122(12) 0.0074(11) 0.0108(12) C13C 0.0324(14) 0.0364(14) 0.0281(13) 0.0092(11) 0.0129(11) 0.0131(12) C14 0.0295(14) 0.0327(14) 0.0351(15) 0.0087(11) 0.0083(12) 0.0069(11) C14C 0.0320(14) 0.0345(14) 0.0275(13) 0.0128(11) 0.0005(11) 0.0099(12) C15 0.0331(15) 0.0468(17) 0.0500(18) 0.0216(14) 0.0113(13) 0.0118(13) C15C 0.0465(17) 0.0317(14) 0.0367(15) 0.0165(12) 0.0121(13) 0.0137(13) C16 0.047(2) 0.065(2) 0.075(2) 0.035(2) 0.0042(18) 0.0162(18) C16C 0.061(2) 0.0365(15) 0.0358(16) 0.0118(13) 0.0089(14) 0.0201(15) C17 0.065(2) 0.058(2) 0.103(3) 0.041(2) 0.023(2) 0.033(2) C17C 0.059(2) 0.0396(16) 0.0500(18) 0.0184(14) 0.0102(16) 0.0229(15) C18 0.058(2) 0.0464(19) 0.083(3) 0.0220(19) 0.033(2) 0.0168(17) C18C 0.0489(18) 0.0352(15) 0.0444(17) 0.0190(13) 0.0025(14) 0.0098(14) C19 0.113(4) 0.053(2) 0.114(4) 0.024(2) 0.061(3) 0.030(2) C19C 0.073(3) 0.0504(19) 0.051(2) 0.0144(16) -0.0084(18) 0.0170(18) C20 0.050(2) 0.0493(19) 0.055(2) 0.0117(16) 0.0115(16) 0.0082(16) C20C 0.058(2) 0.0403(16) 0.0335(16) 0.0101(13) 0.0071(14) 0.0144(15) C21 0.0416(17) 0.0453(17) 0.0489(18) 0.0172(14) 0.0093(14) 0.0135(14) C21C 0.0481(18) 0.0386(15) 0.0362(15) 0.0135(13) 0.0118(13) 0.0166(13) C10S 0.102(4) 0.145(5) 0.060(3) 0.026(3) 0.016(3) 0.069(4) Cl1A 0.084(3) 0.063(2) 0.040(2) 0.0149(18) -0.0059(18) 0.032(2) Cl2A 0.099(3) 0.136(3) 0.111(3) 0.011(2) 0.004(2) 0.044(2) Cl1 0.0762(13) 0.0842(13) 0.0706(12) 0.0150(9) 0.0155(9) 0.0398(11) Cl2 0.199(7) 0.152(5) 0.107(4) 0.014(4) -0.002(4) 0.040(5) _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 O3 1.9428(19) . ? Fe1 O4 2.0061(18) . ? Fe1 O1 2.0363(19) . ? Fe1 O1T 2.0941(19) . ? Fe1 O2 2.3455(19) . ? O1 C14 1.268(3) . ? O1T C1T 1.419(4) . ? O1T C4T 1.424(4) . ? O2 C14 1.246(3) . ? O3 C14C 1.260(3) 2_747 ? O4 C14C 1.247(3) . ? C1 C2 1.503(5) . ? C1C C2C 1.507(4) . ? C1T C2T 1.490(5) . ? C2 C3 1.379(5) . ? C2 C7 1.385(5) . ? C2C C3C 1.384(4) . ? C2C C7C 1.387(4) . ? C2T C3T 1.485(5) . ? C3 C4 1.385(4) . ? C3C C4C 1.380(4) . ? C3T C4T 1.504(5) . ? C4 C5 1.395(4) . ? C4C C5C 1.406(4) . ? C5 C6 1.394(4) . ? C5 C8 1.484(4) . ? C5C C6C 1.387(4) . ? C5C C8C 1.490(4) . ? C6 C7 1.383(5) . ? C6C C7C 1.392(4) . ? C8 C9 1.396(4) . ? C8 C13 1.405(4) . ? C8C C9C 1.392(4) . ? C8C C13C 1.406(4) . ? C9 C10 1.363(5) . ? C9C C10C 1.382(4) . ? C10 C11 1.380(5) . ? C10C C11C 1.370(4) . ? C11 C12 1.407(4) . ? C11C C12C 1.401(4) . ? C12 C13 1.401(4) . ? C12 C15 1.484(4) . ? C12C C13C 1.409(4) . ? C12C C15C 1.486(4) . ? C13 C14 1.523(4) . ? C13C C14C 1.506(4) . ? C14C O3 1.260(3) 2_747 ? C15 C16 1.388(4) . ? C15 C21 1.389(4) . ? C15C C16C 1.399(4) . ? C15C C21C 1.400(4) . ? C16 C17 1.389(5) . ? C16C C17C 1.381(4) . ? C17 C18 1.374(6) . ? C17C C18C 1.383(4) . ? C18 C20 1.389(5) . ? C18 C19 1.523(5) . ? C18C C20C 1.388(4) . ? C18C C19C 1.521(4) . ? C20 C21 1.388(4) . ? C20C C21C 1.382(4) . ? C10S Cl2A 1.552(6) . ? C10S Cl1 1.649(6) . ? C10S Cl2 1.741(8) . ? C10S Cl1A 1.812(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 O3 Fe1 O4 114.33(9) . . ? O3 Fe1 O1 128.66(9) . . ? O4 Fe1 O1 116.11(8) . . ? O3 Fe1 O1T 98.57(9) . . ? O4 Fe1 O1T 92.79(8) . . ? O1 Fe1 O1T 88.02(8) . . ? O3 Fe1 O2 99.84(8) . . ? O4 Fe1 O2 103.69(7) . . ? O1 Fe1 O2 59.52(7) . . ? O1T Fe1 O2 147.40(7) . . ? C14 O1 Fe1 96.21(16) . . ? C1T O1T C4T 108.9(2) . . ? C1T O1T Fe1 126.86(19) . . ? C4T O1T Fe1 122.22(18) . . ? C14 O2 Fe1 82.70(16) . . ? C14C O3 Fe1 156.64(19) 2_747 . ? C14C O4 Fe1 135.98(18) . . ? O1T C1T C2T 106.9(3) . . ? C3 C2 C7 117.0(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 121.2(3) . . ? C3C C2C C7C 117.5(3) . . ? C3C C2C C1C 120.7(3) . . ? C7C C2C C1C 121.8(3) . . ? C3T C2T C1T 105.6(3) . . ? C2 C3 C4 122.1(3) . . ? C4C C3C C2C 122.0(3) . . ? C2T C3T C4T 106.5(3) . . ? C3 C4 C5 120.9(3) . . ? C3C C4C C5C 120.5(3) . . ? O1T C4T C3T 106.0(3) . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C8 121.7(3) . . ? C4 C5 C8 121.2(3) . . ? C6C C5C C4C 117.6(3) . . ? C6C C5C C8C 122.0(2) . . ? C4C C5C C8C 120.3(2) . . ? C7 C6 C5 121.1(3) . . ? C5C C6C C7C 121.0(3) . . ? C6 C7 C2 121.8(3) . . ? C2C C7C C6C 121.3(3) . . ? C9 C8 C13 118.2(3) . . ? C9 C8 C5 118.8(3) . . ? C13 C8 C5 123.1(2) . . ? C9C C8C C13C 118.7(3) . . ? C9C C8C C5C 119.3(2) . . ? C13C C8C C5C 121.9(2) . . ? C10 C9 C8 121.0(3) . . ? C10C C9C C8C 121.1(3) . . ? C9 C10 C11 120.7(3) . . ? C11C C10C C9C 119.9(3) . . ? C10 C11 C12 120.9(3) . . ? C10C C11C C12C 121.7(3) . . ? C13 C12 C11 117.5(3) . . ? C13 C12 C15 123.5(3) . . ? C11 C12 C15 119.0(3) . . ? C11C C12C C13C 117.9(3) . . ? C11C C12C C15C 119.6(3) . . ? C13C C12C C15C 122.5(2) . . ? C12 C13 C8 121.6(3) . . ? C12 C13 C14 120.5(2) . . ? C8 C13 C14 117.9(2) . . ? C8C C13C C12C 120.7(2) . . ? C8C C13C C14C 120.5(2) . . ? C12C C13C C14C 118.8(2) . . ? O2 C14 O1 121.3(3) . . ? O2 C14 C13 121.4(3) . . ? O1 C14 C13 117.2(2) . . ? O4 C14C O3 126.1(2) . 2_747 ? O4 C14C C13C 117.4(2) . . ? O3 C14C C13C 116.5(2) 2_747 . ? C16 C15 C21 117.1(3) . . ? C16 C15 C12 120.5(3) . . ? C21 C15 C12 122.3(3) . . ? C16C C15C C21C 117.4(3) . . ? C16C C15C C12C 120.4(3) . . ? C21C C15C C12C 122.1(3) . . ? C15 C16 C17 120.9(3) . . ? C17C C16C C15C 121.0(3) . . ? C18 C17 C16 122.0(3) . . ? C16C C17C C18C 121.6(3) . . ? C17 C18 C20 117.3(3) . . ? C17 C18 C19 121.8(4) . . ? C20 C18 C19 120.9(4) . . ? C17C C18C C20C 117.6(3) . . ? C17C C18C C19C 121.4(3) . . ? C20C C18C C19C 121.0(3) . . ? C21 C20 C18 121.0(3) . . ? C21C C20C C18C 121.6(3) . . ? C20 C21 C15 121.5(3) . . ? C20C C21C C15C 120.8(3) . . ? Cl2A C10S Cl1 114.9(4) . . ? Cl2A C10S Cl2 117.7(5) . . ? Cl1 C10S Cl2 114.0(4) . . ? Cl2A C10S Cl1A 119.4(4) . . ? Cl1 C10S Cl1A 112.6(3) . . ? Cl2 C10S Cl1A 1.7(4) . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 0.659 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.067 data_new _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe2(m-O2CAr)2(O2CAr)2(py)2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H78 Fe2 N2 O8' _chemical_formula_weight 1475.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6013(7) _cell_length_b 13.5990(9) _cell_length_c 14.9139(10) _cell_angle_alpha 68.8480(10) _cell_angle_beta 71.5410(10) _cell_angle_gamma 78.886(2) _cell_volume 1894.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.855280 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8860 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.25 _reflns_number_total 7145 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0720P)^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_number_reflns 7145 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.002 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 -0.15639(6) -0.09163(5) 0.52852(5) 0.0256(2) Uani 1 1 d . . . N1P N -0.2657(3) -0.0390(3) 0.4193(3) 0.0296(9) Uani 1 1 d . . . O1 O 0.0210(3) -0.1314(2) 0.4438(2) 0.0311(7) Uani 1 1 d . . . O3 O -0.1052(3) -0.2264(2) 0.6680(2) 0.0345(8) Uani 1 1 d . . . O2 O -0.1757(3) 0.0441(2) 0.5514(2) 0.0366(8) Uani 1 1 d . . . O4 O -0.2744(3) -0.2141(2) 0.6089(2) 0.0322(7) Uani 1 1 d . . . C1P C -0.3490(5) 0.0494(4) 0.4057(4) 0.0373(12) Uani 1 1 d . . . C2P C -0.4398(5) 0.0703(5) 0.3516(4) 0.0508(15) Uani 1 1 d . . . C3P C -0.4446(6) -0.0014(5) 0.3081(4) 0.0527(16) Uani 1 1 d . . . C4P C -0.3576(6) -0.0905(5) 0.3180(4) 0.0533(16) Uani 1 1 d . . . C5P C -0.2686(6) -0.1069(4) 0.3735(4) 0.0436(13) Uani 1 1 d . . . C1 C -0.3225(9) 0.4004(8) 0.1756(5) 0.065(2) Uani 1 1 d . . . C2 C -0.3267(5) 0.3549(4) 0.2846(4) 0.0415(13) Uani 1 1 d . . . C3 C -0.4455(5) 0.3368(4) 0.3577(4) 0.0425(13) Uani 1 1 d . . . C4 C -0.4502(5) 0.2988(4) 0.4576(4) 0.0376(12) Uani 1 1 d . . . C5 C -0.3354(4) 0.2765(3) 0.4896(3) 0.0303(11) Uani 1 1 d . . . C6 C -0.2142(5) 0.2931(3) 0.4160(3) 0.0297(11) Uani 1 1 d . . . C7 C -0.2103(5) 0.3312(4) 0.3152(4) 0.0366(12) Uani 1 1 d . . . C8 C -0.3424(4) 0.2409(3) 0.5977(3) 0.0273(10) Uani 1 1 d . . . C9 C -0.4443(5) 0.2859(4) 0.6614(4) 0.0339(11) Uani 1 1 d . . . C10 C -0.4502(5) 0.2576(4) 0.7613(4) 0.0412(13) Uani 1 1 d . . . C11 C -0.3546(5) 0.1868(4) 0.8005(4) 0.0367(12) Uani 1 1 d . . . C12 C -0.2496(5) 0.1411(3) 0.7390(3) 0.0314(11) Uani 1 1 d . . . C13 C -0.2465(4) 0.1663(3) 0.6389(3) 0.0267(10) Uani 1 1 d . . . C14 C -0.1383(5) 0.1099(3) 0.5766(3) 0.0261(10) Uani 1 1 d . . . C15 C -0.1429(5) 0.0674(4) 0.7820(3) 0.0312(11) Uani 1 1 d . . . C16 C -0.0776(5) 0.1010(4) 0.8320(3) 0.0377(12) Uani 1 1 d . . . C17 C 0.0230(6) 0.0353(5) 0.8715(4) 0.0449(13) Uani 1 1 d . . . C18 C 0.0619(5) -0.0641(4) 0.8610(4) 0.0430(13) Uani 1 1 d . . . C19 C -0.0044(5) -0.0969(4) 0.8107(4) 0.0411(13) Uani 1 1 d . . . C20 C -0.1042(5) -0.0322(4) 0.7722(3) 0.0347(11) Uani 1 1 d . . . C21 C 0.1696(8) -0.1367(7) 0.9054(6) 0.0637(19) Uani 1 1 d . . . C22 C -0.1054(9) -0.3742(7) 0.2581(5) 0.0614(18) Uani 1 1 d . . . C23 C -0.1338(5) -0.3946(4) 0.3692(4) 0.0382(12) Uani 1 1 d . . . C24 C -0.2360(5) -0.4542(4) 0.4360(4) 0.0388(13) Uani 1 1 d . . . C25 C -0.2659(5) -0.4731(4) 0.5379(4) 0.0361(12) Uani 1 1 d . . . C26 C -0.1905(4) -0.4330(3) 0.5766(3) 0.0285(10) Uani 1 1 d . . . C27 C -0.0855(5) -0.3756(4) 0.5106(4) 0.0320(11) Uani 1 1 d . . . C28 C -0.0569(5) -0.3560(4) 0.4073(4) 0.0338(11) Uani 1 1 d . . . C29 C -0.2250(4) -0.4552(3) 0.6868(3) 0.0320(11) Uani 1 1 d . . . C30 C -0.2541(5) -0.5575(4) 0.7493(4) 0.0444(13) Uani 1 1 d . . . C31 C -0.2898(6) -0.5834(4) 0.8518(4) 0.0522(15) Uani 1 1 d . . . C32 C -0.2957(6) -0.5074(4) 0.8943(4) 0.0526(15) Uani 1 1 d . . . C33 C -0.2669(5) -0.4039(4) 0.8353(3) 0.0366(12) Uani 1 1 d . . . C34 C -0.2304(4) -0.3778(3) 0.7308(3) 0.0294(10) Uani 1 1 d . . . C35 C -0.2007(4) -0.2661(3) 0.6665(3) 0.0255(10) Uani 1 1 d . . . C36 C -0.2802(5) -0.3249(4) 0.8860(3) 0.0382(12) Uani 1 1 d . . . C37 C -0.2069(6) -0.3402(5) 0.9535(4) 0.0463(13) Uani 1 1 d . . . C38 C -0.2216(6) -0.2678(5) 1.0024(4) 0.0527(16) Uani 1 1 d . . . C39 C -0.3107(5) -0.1785(4) 0.9871(4) 0.0446(13) Uani 1 1 d . . . C40 C -0.3862(6) -0.1642(5) 0.9218(4) 0.0490(14) Uani 1 1 d . . . C41 C -0.3712(5) -0.2359(4) 0.8714(4) 0.0422(13) Uani 1 1 d . . . C42 C -0.3194(9) -0.0966(6) 1.0354(5) 0.0601(19) Uani 1 1 d . . . H32 H -0.318(5) -0.529(4) 0.963(4) 0.057(16) Uiso 1 1 d . . . H31 H -0.311(5) -0.659(5) 0.896(4) 0.074(18) Uiso 1 1 d . . . H17 H 0.070(5) 0.063(4) 0.900(4) 0.057(16) Uiso 1 1 d . . . H41 H -0.429(5) -0.226(4) 0.831(4) 0.064(17) Uiso 1 1 d . . . H22C H -0.085(7) -0.310(6) 0.216(5) 0.10(3) Uiso 1 1 d . . . H1C H -0.367(7) 0.361(5) 0.158(5) 0.10(3) Uiso 1 1 d . . . H40 H -0.442(5) -0.109(4) 0.909(4) 0.055(17) Uiso 1 1 d . . . H1B H -0.350(8) 0.460(6) 0.161(6) 0.11(3) Uiso 1 1 d . . . H21A H 0.234(5) -0.169(4) 0.859(4) 0.056(17) Uiso 1 1 d . . . H30 H -0.245(4) -0.610(3) 0.719(3) 0.024(11) Uiso 1 1 d . . . H1A H -0.229(8) 0.395(5) 0.126(6) 0.12(3) Uiso 1 1 d . . . H22B H -0.014(10) -0.405(8) 0.232(7) 0.18(4) Uiso 1 1 d . . . H25 H -0.335(4) -0.521(3) 0.586(3) 0.015(10) Uiso 1 1 d . . . H9 H -0.505(5) 0.339(4) 0.628(3) 0.043(14) Uiso 1 1 d . . . H22A H -0.174(7) -0.401(5) 0.250(5) 0.09(3) Uiso 1 1 d . . . H38 H -0.167(6) -0.269(4) 1.040(4) 0.073(19) Uiso 1 1 d . . . H16 H -0.098(4) 0.170(4) 0.835(3) 0.041(14) Uiso 1 1 d . . . H10 H -0.514(4) 0.294(3) 0.804(3) 0.028(11) Uiso 1 1 d . . . H11 H -0.359(4) 0.169(3) 0.873(3) 0.032(12) Uiso 1 1 d . . . H19 H 0.010(4) -0.164(3) 0.809(3) 0.029(12) Uiso 1 1 d . . . H37 H -0.136(6) -0.407(4) 0.958(4) 0.077(19) Uiso 1 1 d . . . H20 H -0.148(4) -0.061(3) 0.739(3) 0.033(12) Uiso 1 1 d . . . H42C H -0.271(6) -0.128(5) 1.093(5) 0.09(2) Uiso 1 1 d . . . H3P H -0.503(6) 0.014(5) 0.264(4) 0.079(19) Uiso 1 1 d . . . H21B H 0.227(9) -0.099(7) 0.924(6) 0.16(4) Uiso 1 1 d . . . H42B H -0.254(6) -0.051(4) 0.991(4) 0.07(2) Uiso 1 1 d . . . H42A H -0.395(8) -0.065(6) 1.050(6) 0.11(3) Uiso 1 1 d . . . H21C H 0.150(6) -0.194(5) 0.950(5) 0.07(2) Uiso 1 1 d . . . H4P H -0.355(6) -0.142(5) 0.292(4) 0.07(2) Uiso 1 1 d . . . H3 H -0.523(5) 0.358(4) 0.331(3) 0.045(14) Uiso 1 1 d . . . H1P H -0.335(4) 0.097(3) 0.435(3) 0.029(12) Uiso 1 1 d . . . H24 H -0.292(4) -0.483(3) 0.421(3) 0.032(13) Uiso 1 1 d . . . H5P H -0.211(5) -0.176(5) 0.391(4) 0.075(18) Uiso 1 1 d . . . H4 H -0.533(4) 0.288(3) 0.505(3) 0.027(12) Uiso 1 1 d . . . H6 H -0.133(4) 0.283(3) 0.430(3) 0.020(11) Uiso 1 1 d . . . H27 H -0.038(4) -0.342(4) 0.535(3) 0.047(15) Uiso 1 1 d . . . H7 H -0.126(5) 0.347(3) 0.266(3) 0.036(13) Uiso 1 1 d . . . H28 H 0.023(4) -0.312(3) 0.367(3) 0.035(13) Uiso 1 1 d . . . H2P H -0.489(5) 0.135(4) 0.337(4) 0.060(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0265(4) 0.0237(3) 0.0276(4) -0.0078(3) -0.0087(3) -0.0032(3) N1P 0.032(2) 0.025(2) 0.031(2) -0.0055(17) -0.0122(18) 0.0003(17) O1 0.0291(18) 0.0340(18) 0.0274(17) -0.0095(14) -0.0060(14) 0.0000(15) O3 0.0330(19) 0.0367(19) 0.0380(19) -0.0126(15) -0.0126(15) -0.0067(15) O2 0.048(2) 0.0288(18) 0.046(2) -0.0188(16) -0.0272(17) 0.0044(15) O4 0.0313(18) 0.0257(17) 0.0389(18) -0.0046(14) -0.0172(15) 0.0009(14) C1P 0.040(3) 0.035(3) 0.035(3) -0.010(2) -0.013(2) 0.001(2) C2P 0.038(3) 0.061(4) 0.049(3) -0.013(3) -0.022(3) 0.012(3) C3P 0.045(4) 0.067(4) 0.044(3) 0.000(3) -0.025(3) -0.016(3) C4P 0.081(5) 0.048(4) 0.046(3) -0.008(3) -0.035(3) -0.022(3) C5P 0.065(4) 0.029(3) 0.046(3) -0.013(2) -0.032(3) 0.005(3) C1 0.083(6) 0.069(5) 0.043(4) -0.008(4) -0.035(4) 0.003(4) C2 0.049(3) 0.038(3) 0.035(3) -0.008(2) -0.020(3) 0.006(2) C3 0.040(3) 0.041(3) 0.047(3) -0.006(2) -0.025(3) 0.003(3) C4 0.023(3) 0.039(3) 0.044(3) -0.008(2) -0.007(2) -0.001(2) C5 0.033(3) 0.022(2) 0.038(3) -0.012(2) -0.013(2) 0.002(2) C6 0.026(3) 0.028(3) 0.038(3) -0.010(2) -0.013(2) -0.003(2) C7 0.039(3) 0.035(3) 0.030(3) -0.006(2) -0.007(2) -0.002(2) C8 0.024(2) 0.027(2) 0.030(2) -0.010(2) -0.003(2) -0.008(2) C9 0.027(3) 0.033(3) 0.040(3) -0.013(2) -0.001(2) -0.010(2) C10 0.035(3) 0.045(3) 0.043(3) -0.028(3) 0.008(2) -0.010(3) C11 0.040(3) 0.040(3) 0.028(3) -0.013(2) 0.001(2) -0.011(2) C12 0.038(3) 0.028(2) 0.029(2) -0.011(2) 0.000(2) -0.016(2) C13 0.030(3) 0.025(2) 0.026(2) -0.0114(19) -0.003(2) -0.007(2) C14 0.037(3) 0.022(2) 0.020(2) -0.0053(18) -0.011(2) -0.001(2) C15 0.037(3) 0.034(3) 0.022(2) -0.010(2) -0.003(2) -0.012(2) C16 0.044(3) 0.038(3) 0.030(3) -0.008(2) -0.009(2) -0.010(3) C17 0.050(3) 0.052(4) 0.035(3) -0.010(3) -0.014(3) -0.014(3) C18 0.042(3) 0.049(3) 0.031(3) -0.006(2) -0.011(2) -0.003(3) C19 0.054(3) 0.030(3) 0.031(3) -0.004(2) -0.006(3) -0.006(3) C20 0.045(3) 0.037(3) 0.022(2) -0.008(2) -0.006(2) -0.009(2) C21 0.067(5) 0.064(5) 0.050(4) -0.006(4) -0.026(4) 0.010(4) C22 0.080(6) 0.067(5) 0.039(4) -0.015(4) -0.016(4) -0.013(4) C23 0.046(3) 0.029(3) 0.038(3) -0.012(2) -0.014(3) 0.007(2) C24 0.043(3) 0.029(3) 0.058(4) -0.024(3) -0.026(3) 0.007(3) C25 0.040(3) 0.026(3) 0.045(3) -0.013(2) -0.012(3) -0.003(2) C26 0.033(3) 0.017(2) 0.035(3) -0.009(2) -0.011(2) 0.002(2) C27 0.037(3) 0.024(2) 0.037(3) -0.012(2) -0.011(2) -0.001(2) C28 0.035(3) 0.027(3) 0.039(3) -0.012(2) -0.008(2) -0.001(2) C29 0.032(3) 0.027(3) 0.036(3) -0.006(2) -0.012(2) -0.003(2) C30 0.061(4) 0.027(3) 0.044(3) -0.008(2) -0.014(3) -0.009(3) C31 0.077(4) 0.031(3) 0.044(3) -0.001(3) -0.016(3) -0.016(3) C32 0.081(4) 0.042(3) 0.029(3) 0.000(3) -0.015(3) -0.014(3) C33 0.045(3) 0.036(3) 0.031(3) -0.007(2) -0.017(2) -0.005(2) C34 0.035(3) 0.023(2) 0.029(2) -0.0046(19) -0.013(2) 0.001(2) C35 0.025(2) 0.024(2) 0.023(2) -0.0099(19) -0.003(2) 0.003(2) C36 0.049(3) 0.038(3) 0.027(2) -0.005(2) -0.010(2) -0.015(3) C37 0.056(4) 0.051(3) 0.034(3) -0.008(3) -0.018(3) -0.012(3) C38 0.061(4) 0.072(4) 0.035(3) -0.017(3) -0.016(3) -0.025(3) C39 0.052(3) 0.053(3) 0.028(3) -0.014(2) 0.003(3) -0.024(3) C40 0.056(4) 0.053(4) 0.040(3) -0.023(3) -0.010(3) 0.001(3) C41 0.050(3) 0.049(3) 0.037(3) -0.019(3) -0.017(3) -0.007(3) C42 0.070(5) 0.076(5) 0.045(4) -0.034(4) 0.001(4) -0.031(5) _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 O2 1.957(3) . ? Fe1 O1 2.006(3) . ? Fe1 O4 2.047(3) . ? Fe1 N1P 2.132(4) . ? Fe1 O3 2.358(3) . ? Fe1 Fe1 4.2189(13) 2_556 ? N1P C5P 1.340(6) . ? N1P C1P 1.340(6) . ? O1 C14 1.249(5) 2_556 ? O3 C35 1.246(5) . ? O2 C14 1.255(5) . ? O4 C35 1.274(5) . ? C1P C2P 1.370(7) . ? C2P C3P 1.369(8) . ? C3P C4P 1.367(8) . ? C4P C5P 1.381(7) . ? C1 C2 1.505(8) . ? C2 C3 1.375(7) . ? C2 C7 1.390(7) . ? C3 C4 1.377(7) . ? C4 C5 1.386(6) . ? C5 C6 1.395(6) . ? C5 C8 1.488(6) . ? C6 C7 1.392(6) . ? C8 C9 1.400(6) . ? C8 C13 1.410(6) . ? C9 C10 1.381(7) . ? C10 C11 1.375(7) . ? C11 C12 1.402(6) . ? C12 C13 1.396(6) . ? C12 C15 1.501(6) . ? C13 C14 1.506(6) . ? C14 O1 1.249(5) 2_556 ? C15 C20 1.384(6) . ? C15 C16 1.393(6) . ? C16 C17 1.390(7) . ? C17 C18 1.385(7) . ? C18 C19 1.397(7) . ? C18 C21 1.513(8) . ? C19 C20 1.373(7) . ? C22 C23 1.516(7) . ? C23 C24 1.377(7) . ? C23 C28 1.392(7) . ? C24 C25 1.385(7) . ? C25 C26 1.398(6) . ? C26 C27 1.380(6) . ? C26 C29 1.494(6) . ? C27 C28 1.406(6) . ? C29 C30 1.396(6) . ? C29 C34 1.412(6) . ? C30 C31 1.379(7) . ? C31 C32 1.378(7) . ? C32 C33 1.396(7) . ? C33 C34 1.406(6) . ? C33 C36 1.485(6) . ? C34 C35 1.506(6) . ? C36 C41 1.392(7) . ? C36 C37 1.393(7) . ? C37 C38 1.383(7) . ? C38 C39 1.384(8) . ? C39 C40 1.387(7) . ? C39 C42 1.506(8) . ? C40 C41 1.390(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 O2 Fe1 O1 116.42(13) . . ? O2 Fe1 O4 126.98(13) . . ? O1 Fe1 O4 114.46(12) . . ? O2 Fe1 N1P 96.26(13) . . ? O1 Fe1 N1P 98.65(13) . . ? O4 Fe1 N1P 90.01(13) . . ? O2 Fe1 O3 108.11(12) . . ? O1 Fe1 O3 88.63(11) . . ? O4 Fe1 O3 59.18(11) . . ? N1P Fe1 O3 148.25(13) . . ? O2 Fe1 Fe1 53.89(9) . 2_556 ? O1 Fe1 Fe1 63.93(9) . 2_556 ? O4 Fe1 Fe1 154.61(9) . 2_556 ? N1P Fe1 Fe1 115.39(10) . 2_556 ? O3 Fe1 Fe1 95.63(8) . 2_556 ? C5P N1P C1P 117.5(4) . . ? C5P N1P Fe1 117.6(3) . . ? C1P N1P Fe1 123.9(3) . . ? C14 O1 Fe1 135.6(3) 2_556 . ? C35 O3 Fe1 82.8(3) . . ? C14 O2 Fe1 152.8(3) . . ? C35 O4 Fe1 96.2(3) . . ? N1P C1P C2P 123.1(5) . . ? C3P C2P C1P 118.7(5) . . ? C4P C3P C2P 119.3(5) . . ? C3P C4P C5P 119.0(5) . . ? N1P C5P C4P 122.3(5) . . ? C3 C2 C7 117.4(5) . . ? C3 C2 C1 121.5(5) . . ? C7 C2 C1 121.0(5) . . ? C2 C3 C4 121.7(5) . . ? C3 C4 C5 121.7(5) . . ? C4 C5 C6 117.1(4) . . ? C4 C5 C8 121.1(4) . . ? C6 C5 C8 121.7(4) . . ? C7 C6 C5 120.9(4) . . ? C2 C7 C6 121.2(5) . . ? C9 C8 C13 117.8(4) . . ? C9 C8 C5 119.5(4) . . ? C13 C8 C5 122.7(4) . . ? C10 C9 C8 120.7(5) . . ? C11 C10 C9 121.2(4) . . ? C10 C11 C12 119.9(5) . . ? C13 C12 C11 119.0(4) . . ? C13 C12 C15 121.8(4) . . ? C11 C12 C15 119.2(4) . . ? C12 C13 C8 121.3(4) . . ? C12 C13 C14 117.8(4) . . ? C8 C13 C14 120.9(4) . . ? O1 C14 O2 126.3(4) 2_556 . ? O1 C14 C13 117.7(4) 2_556 . ? O2 C14 C13 116.0(4) . . ? C20 C15 C16 118.2(5) . . ? C20 C15 C12 122.8(4) . . ? C16 C15 C12 119.0(4) . . ? C17 C16 C15 120.4(5) . . ? C18 C17 C16 121.1(5) . . ? C17 C18 C19 117.9(5) . . ? C17 C18 C21 121.3(6) . . ? C19 C18 C21 120.7(6) . . ? C20 C19 C18 121.0(5) . . ? C19 C20 C15 121.3(5) . . ? C24 C23 C28 117.9(5) . . ? C24 C23 C22 120.5(5) . . ? C28 C23 C22 121.6(6) . . ? C23 C24 C25 122.0(5) . . ? C24 C25 C26 120.5(5) . . ? C27 C26 C25 118.0(4) . . ? C27 C26 C29 122.8(4) . . ? C25 C26 C29 119.1(4) . . ? C26 C27 C28 121.0(5) . . ? C23 C28 C27 120.5(5) . . ? C30 C29 C34 118.5(4) . . ? C30 C29 C26 118.2(4) . . ? C34 C29 C26 123.3(4) . . ? C31 C30 C29 121.6(5) . . ? C30 C31 C32 119.7(5) . . ? C31 C32 C33 121.2(5) . . ? C32 C33 C34 119.1(4) . . ? C32 C33 C36 118.3(4) . . ? C34 C33 C36 122.6(4) . . ? C33 C34 C29 120.1(4) . . ? C33 C34 C35 119.5(4) . . ? C29 C34 C35 120.4(4) . . ? O3 C35 O4 120.9(4) . . ? O3 C35 C34 121.0(4) . . ? O4 C35 C34 118.0(4) . . ? C41 C36 C37 117.8(5) . . ? C41 C36 C33 121.0(4) . . ? C37 C36 C33 121.1(5) . . ? C38 C37 C36 121.0(6) . . ? C37 C38 C39 121.3(6) . . ? C38 C39 C40 117.9(5) . . ? C38 C39 C42 120.8(6) . . ? C40 C39 C42 121.2(6) . . ? C39 C40 C41 121.3(6) . . ? C40 C41 C36 120.7(5) . . ? _diffrn_measured_fraction_theta_max 0.763 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.763 _refine_diff_density_max 0.511 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.132 data_structure _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe2(m-O2CAr)2(O2CAr)2(1-MeIm)2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H80 Cl4 Fe2 N4 O8' _chemical_formula_weight 1647.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1846(2) _cell_length_b 17.3132(2) _cell_length_c 22.5524(3) _cell_angle_alpha 84.4790(10) _cell_angle_beta 84.1290(10) _cell_angle_gamma 73.6050(10) _cell_volume 4157.14(10) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.813004 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24847 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.27 _reflns_number_total 17450 _reflns_number_gt 10972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0965P)^2^+2.1160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17450 _refine_ls_number_parameters 1023 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 2.978 _refine_ls_shift/su_mean 0.066 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe2 Fe 0.67307(5) -0.50411(3) -0.04726(2) 0.03062(15) Uani 1 1 d . . . Fe1 Fe 0.81750(5) 0.07386(3) -0.48252(2) 0.02796(14) Uani 1 1 d . . . O1A O 0.9522(3) 0.11285(17) -0.52510(11) 0.0397(7) Uani 1 1 d . . . O1 O 0.6825(2) 0.13685(16) -0.42489(12) 0.0373(6) Uani 1 1 d . . . O2 O 0.8655(2) 0.12539(16) -0.39230(11) 0.0373(6) Uani 1 1 d . . . O2A O 0.8449(3) -0.04596(15) -0.46529(12) 0.0394(7) Uani 1 1 d . . . O1B O 0.6326(3) -0.55244(18) -0.13314(12) 0.0437(7) Uani 1 1 d . . . O1C O 0.5362(3) -0.40446(16) -0.06109(12) 0.0418(7) Uani 1 1 d . . . O2B O 0.8188(3) -0.55162(17) -0.11067(12) 0.0424(7) Uani 1 1 d . . . O2C O 0.3505(3) -0.41362(17) -0.01926(12) 0.0432(7) Uani 1 1 d . . . N1N N 0.7820(3) -0.45632(19) 0.00067(14) 0.0338(7) Uani 1 1 d . . . N2N N 0.9102(3) -0.38783(19) 0.02070(15) 0.0372(8) Uani 1 1 d . . . N1M N 0.6918(3) 0.0819(2) -0.54697(14) 0.0348(7) Uani 1 1 d . . . N2M N 0.5427(3) 0.0575(2) -0.59212(15) 0.0407(8) Uani 1 1 d . . . C1N C 0.8286(4) -0.3950(2) -0.01681(18) 0.0378(9) Uani 1 1 d . . . H1NA H 0.8076 -0.3610 -0.0509 0.045 Uiso 1 1 calc R . . C1C C 0.1294(6) -0.4907(4) -0.2447(2) 0.0756(17) Uani 1 1 d . . . H1C1 H 0.0864 -0.4610 -0.2780 0.113 Uiso 1 1 calc R . . H1C2 H 0.0750 -0.5167 -0.2199 0.113 Uiso 1 1 calc R . . H1C3 H 0.2025 -0.5307 -0.2590 0.113 Uiso 1 1 calc R . . C1B C 0.5296(6) -0.1844(4) -0.2133(3) 0.0840(18) Uani 1 1 d . . . H1B1 H 0.4608 -0.1808 -0.1835 0.126 Uiso 1 1 calc R . . H1B2 H 0.4995 -0.1551 -0.2496 0.126 Uiso 1 1 calc R . . H1B3 H 0.5897 -0.1616 -0.1994 0.126 Uiso 1 1 calc R . . C2C C 0.1676(5) -0.4337(3) -0.20881(19) 0.0540(12) Uani 1 1 d . . . C2B C 0.5899(5) -0.2710(4) -0.2247(2) 0.0638(15) Uani 1 1 d . . . C2N C 0.9813(5) -0.3273(3) 0.0150(2) 0.0523(12) Uani 1 1 d . . . H2N1 H 0.9369 -0.2800 -0.0078 0.079 Uiso 1 1 calc R . . H2N2 H 1.0621 -0.3493 -0.0051 0.079 Uiso 1 1 calc R . . H2N3 H 0.9911 -0.3132 0.0540 0.079 Uiso 1 1 calc R . . C3N C 0.9161(4) -0.4478(2) 0.06540(17) 0.0383(9) Uani 1 1 d . . . H3NA H 0.9647 -0.4579 0.0979 0.046 Uiso 1 1 calc R . . C3C C 0.2930(5) -0.4420(3) -0.20057(19) 0.0528(12) Uani 1 1 d . . . H3CA H 0.3543 -0.4836 -0.2181 0.063 Uiso 1 1 calc R . . C3B C 0.5485(6) -0.3099(5) -0.2657(3) 0.0772(18) Uani 1 1 d . . . H3BA H 0.4812 -0.2813 -0.2872 0.093 Uiso 1 1 calc R . . C4C C 0.3288(4) -0.3907(3) -0.16749(18) 0.0443(10) Uani 1 1 d . . . H4CA H 0.4130 -0.3989 -0.1623 0.053 Uiso 1 1 calc R . . C4N C 0.8370(4) -0.4892(2) 0.05294(17) 0.0378(9) Uani 1 1 d . . . H4NA H 0.8218 -0.5334 0.0761 0.045 Uiso 1 1 calc R . . C4B C 0.6037(5) -0.3893(5) -0.2758(2) 0.0721(18) Uani 1 1 d . . . H4BA H 0.5735 -0.4128 -0.3043 0.087 Uiso 1 1 calc R . . C5C C 0.2397(4) -0.3265(3) -0.14166(17) 0.0388(9) Uani 1 1 d . . . C5B C 0.7050(5) -0.4365(3) -0.2442(2) 0.0571(14) Uani 1 1 d . . . C6C C 0.1136(4) -0.3179(3) -0.14969(19) 0.0468(11) Uani 1 1 d . . . H6CA H 0.0521 -0.2759 -0.1328 0.056 Uiso 1 1 calc R . . C6B C 0.7465(5) -0.3974(3) -0.20248(19) 0.0530(12) Uani 1 1 d . . . H6BA H 0.8127 -0.4260 -0.1803 0.064 Uiso 1 1 calc R . . C7B C 0.6918(5) -0.3179(3) -0.1936(2) 0.0575(13) Uani 1 1 d . . . H7BA H 0.7230 -0.2938 -0.1659 0.069 Uiso 1 1 calc R . . C7C C 0.0795(5) -0.3706(3) -0.1822(2) 0.0533(12) Uani 1 1 d . . . H7CA H -0.0049 -0.3636 -0.1865 0.064 Uiso 1 1 calc R . . C8C C 0.2745(4) -0.2664(2) -0.10874(18) 0.0389(9) Uani 1 1 d . . . C8B C 0.7690(5) -0.5207(4) -0.2569(2) 0.0592(14) Uani 1 1 d . . . C9C C 0.2200(4) -0.1845(3) -0.1227(2) 0.0484(11) Uani 1 1 d . . . H9CA H 0.1596 -0.1691 -0.1502 0.058 Uiso 1 1 calc R . . C9B C 0.8077(6) -0.5399(4) -0.3154(2) 0.0779(18) Uani 1 1 d . . . H9BA H 0.7896 -0.4997 -0.3462 0.093 Uiso 1 1 calc R . . C10B C 0.8719(7) -0.6166(5) -0.3287(3) 0.095(2) Uani 1 1 d . . . H10C H 0.8946 -0.6281 -0.3684 0.114 Uiso 1 1 calc R . . C10C C 0.2538(5) -0.1259(3) -0.0965(2) 0.0545(12) Uani 1 1 d . . . H10D H 0.2160 -0.0716 -0.1062 0.065 Uiso 1 1 calc R . . C11C C 0.3442(5) -0.1479(3) -0.0555(2) 0.0501(11) Uani 1 1 d . . . H11C H 0.3677 -0.1083 -0.0382 0.060 Uiso 1 1 calc R . . C11B C 0.9037(6) -0.6771(4) -0.2842(3) 0.082(2) Uani 1 1 d . . . H11D H 0.9487 -0.7289 -0.2938 0.099 Uiso 1 1 calc R . . C12B C 0.8670(5) -0.6600(3) -0.2233(2) 0.0598(14) Uani 1 1 d . . . C12C C 0.4000(4) -0.2293(2) -0.04029(18) 0.0391(9) Uani 1 1 d . . . C13C C 0.3640(4) -0.2882(2) -0.06657(17) 0.0352(9) Uani 1 1 d . . . C13B C 0.7977(4) -0.5827(3) -0.2108(2) 0.0507(12) Uani 1 1 d . . . C14C C 0.4217(4) -0.3765(2) -0.04787(16) 0.0355(9) Uani 1 1 d . . . C14B C 0.7461(4) -0.5617(3) -0.14793(18) 0.0407(10) Uani 1 1 d . . . C15C C 0.4904(4) -0.2501(2) 0.00742(17) 0.0372(9) Uani 1 1 d . . . C15B C 0.9057(4) -0.7253(3) -0.1764(3) 0.0614(16) Uani 1 1 d . . . C16B C 1.0258(5) -0.7782(4) -0.1793(3) 0.0757(18) Uani 1 1 d . . . H16C H 1.0814 -0.7722 -0.2119 0.091 Uiso 1 1 calc R . . C16C C 0.5810(4) -0.2088(3) 0.0088(2) 0.0449(10) Uani 1 1 d . . . H16D H 0.5902 -0.1706 -0.0219 0.054 Uiso 1 1 calc R . . C17C C 0.6574(4) -0.2249(3) 0.0561(2) 0.0485(11) Uani 1 1 d . . . H17C H 0.7175 -0.1972 0.0562 0.058 Uiso 1 1 calc R . . C17B C 1.0642(6) -0.8380(4) -0.1364(4) 0.087(2) Uani 1 1 d . . . H17D H 1.1447 -0.8724 -0.1409 0.104 Uiso 1 1 calc R . . C18C C 0.6465(4) -0.2808(3) 0.10274(19) 0.0434(10) Uani 1 1 d . . . C18B C 0.9872(7) -0.8498(3) -0.0855(4) 0.093(2) Uani 1 1 d . . . C19B C 0.8657(6) -0.7978(3) -0.0820(3) 0.083(2) Uani 1 1 d . . . H19C H 0.8108 -0.8039 -0.0492 0.100 Uiso 1 1 calc R . . C19C C 0.5590(4) -0.3230(3) 0.10024(17) 0.0388(9) Uani 1 1 d . . . H19D H 0.5520 -0.3625 0.1303 0.047 Uiso 1 1 calc R . . C20C C 0.4821(4) -0.3075(2) 0.05397(17) 0.0370(9) Uani 1 1 d . . . H20C H 0.4232 -0.3361 0.0539 0.044 Uiso 1 1 calc R . . C20B C 0.8260(5) -0.7377(3) -0.1262(3) 0.0680(16) Uani 1 1 d . . . H20D H 0.7445 -0.7046 -0.1227 0.082 Uiso 1 1 calc R . . C21C C 0.7248(5) -0.2952(3) 0.1558(2) 0.0626(14) Uani 1 1 d . . . H21A H 0.6963 -0.2500 0.1802 0.094 Uiso 1 1 calc R . . H21B H 0.8108 -0.3016 0.1420 0.094 Uiso 1 1 calc R . . H21C H 0.7169 -0.3433 0.1790 0.094 Uiso 1 1 calc R . . C21B C 1.0307(8) -0.9113(4) -0.0354(5) 0.155(4) Uani 1 1 d . . . H21D H 1.1011 -0.9532 -0.0498 0.233 Uiso 1 1 calc R . . H21E H 0.9641 -0.9343 -0.0198 0.233 Uiso 1 1 calc R . . H21F H 1.0547 -0.8860 -0.0042 0.233 Uiso 1 1 calc R . . C1M C 0.6381(4) 0.0261(3) -0.55720(18) 0.0383(9) Uani 1 1 d . . . H1MA H 0.6628 -0.0275 -0.5423 0.046 Uiso 1 1 calc R . . C1 C 0.6733(6) 0.3996(3) -0.6244(2) 0.0722(16) Uani 1 1 d . . . H1A H 0.6366 0.3685 -0.6464 0.108 Uiso 1 1 calc R . . H1B H 0.7598 0.3912 -0.6383 0.108 Uiso 1 1 calc R . . H1C H 0.6300 0.4558 -0.6304 0.108 Uiso 1 1 calc R . . C1A C 0.7632(5) 0.0156(3) -0.7394(2) 0.0647(14) Uani 1 1 d . . . H1A1 H 0.8198 -0.0257 -0.7620 0.097 Uiso 1 1 calc R . . H1A2 H 0.7046 0.0508 -0.7651 0.097 Uiso 1 1 calc R . . H1A3 H 0.7188 -0.0089 -0.7078 0.097 Uiso 1 1 calc R . . C2A C 0.8353(4) 0.0632(3) -0.71321(19) 0.0456(10) Uani 1 1 d . . . C2 C 0.6633(5) 0.3731(3) -0.5586(2) 0.0488(11) Uani 1 1 d . . . C2M C 0.4607(5) 0.0140(3) -0.6118(2) 0.0665(15) Uani 1 1 d . . . H2M1 H 0.4814 -0.0402 -0.5938 0.100 Uiso 1 1 calc R . . H2M2 H 0.4717 0.0126 -0.6545 0.100 Uiso 1 1 calc R . . H2M3 H 0.3753 0.0410 -0.6001 0.100 Uiso 1 1 calc R . . C3M C 0.5364(4) 0.1369(3) -0.6055(2) 0.0500(11) Uani 1 1 d . . . H3MA H 0.4800 0.1740 -0.6290 0.060 Uiso 1 1 calc R . . C3A C 0.8034(4) 0.1473(3) -0.71932(19) 0.0481(11) Uani 1 1 d . . . H3AA H 0.7354 0.1751 -0.7407 0.058 Uiso 1 1 calc R . . C3 C 0.5500(5) 0.3932(3) -0.5243(2) 0.0548(12) Uani 1 1 d . . . H3A H 0.4788 0.4236 -0.5424 0.066 Uiso 1 1 calc R . . C4 C 0.5395(4) 0.3691(3) -0.4639(2) 0.0500(11) Uani 1 1 d . . . H4A H 0.4618 0.3832 -0.4425 0.060 Uiso 1 1 calc R . . C4A C 0.8697(4) 0.1905(3) -0.69452(18) 0.0445(10) Uani 1 1 d . . . H4AA H 0.8454 0.2466 -0.6991 0.053 Uiso 1 1 calc R . . C4M C 0.6287(4) 0.1507(3) -0.5776(2) 0.0477(11) Uani 1 1 d . . . H4MA H 0.6467 0.2001 -0.5790 0.057 Uiso 1 1 calc R . . C5 C 0.6445(4) 0.3240(2) -0.43509(18) 0.0365(9) Uani 1 1 d . . . C5A C 0.9736(4) 0.1509(2) -0.66241(16) 0.0351(9) Uani 1 1 d . . . C6A C 1.0063(4) 0.0670(2) -0.65676(16) 0.0367(9) Uani 1 1 d . . . H6AA H 1.0753 0.0391 -0.6362 0.044 Uiso 1 1 calc R . . C6 C 0.7574(4) 0.3050(2) -0.46949(19) 0.0412(10) Uani 1 1 d . . . H6A H 0.8291 0.2752 -0.4516 0.049 Uiso 1 1 calc R . . C7A C 0.9376(4) 0.0238(3) -0.68136(17) 0.0416(10) Uani 1 1 d . . . H7AA H 0.9608 -0.0323 -0.6763 0.050 Uiso 1 1 calc R . . C7 C 0.7669(4) 0.3290(3) -0.5296(2) 0.0462(10) Uani 1 1 d . . . H7A H 0.8446 0.3151 -0.5510 0.055 Uiso 1 1 calc R . . C8A C 1.0455(4) 0.1984(2) -0.63699(17) 0.0378(9) Uani 1 1 d . . . C8 C 0.6340(4) 0.2989(2) -0.37004(18) 0.0368(9) Uani 1 1 d . . . C9 C 0.5748(4) 0.3572(3) -0.3299(2) 0.0478(11) Uani 1 1 d . . . H9A H 0.5391 0.4100 -0.3443 0.057 Uiso 1 1 calc R . . C9A C 1.0726(5) 0.2638(3) -0.6707(2) 0.0535(12) Uani 1 1 d . . . H9AA H 1.0453 0.2770 -0.7090 0.064 Uiso 1 1 calc R . . C10A C 1.1389(5) 0.3095(3) -0.6488(2) 0.0658(15) Uani 1 1 d . . . H10A H 1.1550 0.3535 -0.6720 0.079 Uiso 1 1 calc R . . C10 C 0.5690(5) 0.3370(3) -0.2693(2) 0.0537(12) Uani 1 1 d . . . H10B H 0.5292 0.3764 -0.2431 0.064 Uiso 1 1 calc R . . C11A C 1.1814(5) 0.2901(3) -0.5926(2) 0.0566(13) Uani 1 1 d . . . H11A H 1.2264 0.3211 -0.5782 0.068 Uiso 1 1 calc R . . C11 C 0.6216(4) 0.2588(3) -0.24700(19) 0.0451(10) Uani 1 1 d . . . H11B H 0.6174 0.2461 -0.2060 0.054 Uiso 1 1 calc R . . C12A C 1.1581(4) 0.2244(2) -0.55659(17) 0.0378(9) Uani 1 1 d . . . C12 C 0.6808(4) 0.1989(2) -0.28560(17) 0.0338(9) Uani 1 1 d . . . C13A C 1.0905(3) 0.1787(2) -0.57947(16) 0.0310(8) Uani 1 1 d . . . C13 C 0.6877(3) 0.2195(2) -0.34723(16) 0.0301(8) Uani 1 1 d . . . C14A C 1.0640(4) 0.1066(2) -0.54334(16) 0.0298(8) Uani 1 1 d . . . C14 C 0.7516(4) 0.1558(2) -0.38982(16) 0.0294(8) Uani 1 1 d . . . C15A C 1.2026(4) 0.2091(2) -0.49477(18) 0.0355(9) Uani 1 1 d . . . C15 C 0.7321(3) 0.1146(2) -0.25997(16) 0.0310(8) Uani 1 1 d . . . C16A C 1.3206(4) 0.2166(3) -0.4851(2) 0.0461(11) Uani 1 1 d . . . H16A H 1.3732 0.2269 -0.5177 0.055 Uiso 1 1 calc R . . C16 C 0.8160(4) 0.0964(3) -0.21600(18) 0.0401(10) Uani 1 1 d . . . H16B H 0.8440 0.1372 -0.2032 0.048 Uiso 1 1 calc R . . C17 C 0.8583(4) 0.0188(3) -0.19099(19) 0.0429(10) Uani 1 1 d . . . H17A H 0.9147 0.0082 -0.1617 0.051 Uiso 1 1 calc R . . C17A C 1.3603(4) 0.2090(3) -0.4285(2) 0.0510(12) Uani 1 1 d . . . H17B H 1.4391 0.2144 -0.4236 0.061 Uiso 1 1 calc R . . C18 C 0.8188(4) -0.0437(2) -0.20854(18) 0.0391(9) Uani 1 1 d . . . C18A C 1.2849(4) 0.1936(3) -0.3788(2) 0.0465(11) Uani 1 1 d . . . C19A C 1.1699(4) 0.1830(2) -0.38809(19) 0.0403(10) Uani 1 1 d . . . H19A H 1.1192 0.1705 -0.3554 0.048 Uiso 1 1 calc R . . C19 C 0.7362(4) -0.0257(2) -0.25286(18) 0.0401(10) Uani 1 1 d . . . H19B H 0.7084 -0.0667 -0.2656 0.048 Uiso 1 1 calc R . . C20A C 1.1289(4) 0.1908(2) -0.44502(17) 0.0354(9) Uani 1 1 d . . . H20A H 1.0512 0.1836 -0.4499 0.042 Uiso 1 1 calc R . . C20 C 0.6941(4) 0.0515(2) -0.27860(17) 0.0370(9) Uani 1 1 d . . . H20B H 0.6396 0.0616 -0.3087 0.044 Uiso 1 1 calc R . . C21A C 1.3272(5) 0.1892(4) -0.3166(2) 0.0689(15) Uani 1 1 d . . . H21G H 1.4164 0.1789 -0.3188 0.103 Uiso 1 1 calc R . . H21H H 1.3032 0.1464 -0.2924 0.103 Uiso 1 1 calc R . . H21I H 1.2886 0.2395 -0.2990 0.103 Uiso 1 1 calc R . . C21 C 0.8654(5) -0.1286(3) -0.1811(2) 0.0595(13) Uani 1 1 d . . . H21J H 0.8016 -0.1560 -0.1807 0.089 Uiso 1 1 calc R . . H21K H 0.8853 -0.1269 -0.1409 0.089 Uiso 1 1 calc R . . H21L H 0.9389 -0.1570 -0.2042 0.089 Uiso 1 1 calc R . . C1S C 0.5646(11) 0.0638(7) -0.1174(5) 0.079(4) Uiso 0.676(11) 1 d P . . Cl1 Cl 0.6730(8) -0.0035(4) -0.0572(3) 0.091(2) Uiso 0.338(6) 1 d P A 1 Cl2 Cl 0.4508(8) 0.0201(4) -0.1217(4) 0.106(2) Uiso 0.338(6) 1 d P A 1 Cl1A Cl 0.6243(11) -0.0040(3) -0.0640(3) 0.0568(13) Uiso 0.338(6) 1 d P A 2 Cl2A Cl 0.4214(6) 0.0331(5) -0.1429(6) 0.0691(15) Uiso 0.338(6) 1 d P A 2 Cl1B Cl 0.5806(11) 0.0007(4) -0.0687(3) 0.089(2) Uiso 0.324(11) 1 d P A 3 Cl2B Cl 0.4175(6) 0.0501(5) -0.1656(5) 0.089(2) Uiso 0.324(11) 1 d P A 3 C2S C 0.5416(14) 0.0635(9) -0.1323(7) 0.033(4) Uiso 0.324(11) 1 d P A 3 C10S C 1.8615(17) 0.5759(12) 0.4522(8) 0.060(5) Uiso 0.315(5) 1 d P B 4 Cl11 Cl 1.8253(9) 0.5756(6) 0.3869(4) 0.145(4) Uiso 0.315(5) 1 d P B 4 Cl10 Cl 1.8072(6) 0.5242(4) 0.5062(3) 0.110(3) Uiso 0.315(5) 1 d P B 4 C22S C 1.876(3) 0.5356(18) 0.4209(15) 0.080(7) Uiso 0.185(5) 1 d P B 5 C20S C 1.844(3) 0.539(2) 0.4598(16) 0.063(8) Uiso 0.185(5) 1 d P B 5 C21S C 1.985(3) 0.5157(18) 0.4785(12) 0.064(8) Uiso 0.185(5) 1 d P . 5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe2 0.0292(3) 0.0339(3) 0.0285(3) -0.0067(2) -0.0040(2) -0.0061(2) Fe1 0.0242(3) 0.0318(3) 0.0303(3) -0.0051(2) -0.0026(2) -0.0104(2) O1A 0.0386(16) 0.0540(18) 0.0341(15) -0.0071(13) 0.0034(12) -0.0260(14) O1 0.0365(15) 0.0415(16) 0.0381(15) -0.0129(12) -0.0033(12) -0.0139(12) O2 0.0298(15) 0.0414(16) 0.0351(15) -0.0047(12) -0.0002(12) -0.0007(12) O2A 0.0454(17) 0.0291(15) 0.0471(17) -0.0012(12) -0.0157(13) -0.0121(13) O1B 0.0400(17) 0.0603(19) 0.0380(16) -0.0148(14) 0.0063(13) -0.0254(14) O1C 0.0395(17) 0.0410(17) 0.0382(16) -0.0055(12) -0.0104(13) 0.0032(13) O2B 0.0420(16) 0.0513(18) 0.0397(16) -0.0198(13) -0.0010(13) -0.0176(14) O2C 0.0555(19) 0.0394(17) 0.0388(16) 0.0079(13) -0.0145(14) -0.0191(14) N1N 0.0362(18) 0.0330(18) 0.0313(17) -0.0090(14) -0.0082(14) -0.0038(14) N2N 0.0395(19) 0.0357(19) 0.0400(19) -0.0122(15) -0.0056(15) -0.0122(15) N1M 0.0323(18) 0.0407(19) 0.0342(17) -0.0096(15) -0.0042(14) -0.0117(15) N2M 0.0313(18) 0.058(2) 0.0390(19) -0.0124(16) -0.0061(15) -0.0180(16) C1N 0.042(2) 0.039(2) 0.032(2) -0.0072(17) -0.0044(18) -0.0080(18) C1C 0.103(5) 0.083(4) 0.053(3) 0.000(3) -0.028(3) -0.039(4) C1B 0.067(4) 0.083(5) 0.100(5) 0.018(4) -0.013(3) -0.023(3) C2C 0.068(3) 0.067(3) 0.033(2) 0.011(2) -0.019(2) -0.027(3) C2B 0.052(3) 0.097(4) 0.051(3) 0.015(3) -0.003(2) -0.042(3) C2N 0.056(3) 0.046(3) 0.062(3) -0.007(2) -0.006(2) -0.025(2) C3N 0.043(2) 0.041(2) 0.031(2) -0.0038(18) -0.0120(18) -0.0100(19) C3C 0.062(3) 0.057(3) 0.037(2) -0.003(2) -0.003(2) -0.011(2) C3B 0.058(4) 0.114(6) 0.068(4) 0.012(4) -0.008(3) -0.042(4) C4C 0.041(2) 0.060(3) 0.031(2) 0.000(2) -0.0061(18) -0.013(2) C4N 0.043(2) 0.039(2) 0.034(2) -0.0045(17) -0.0081(18) -0.0118(18) C4B 0.070(4) 0.133(6) 0.035(3) 0.006(3) -0.013(3) -0.064(4) C5C 0.038(2) 0.047(2) 0.029(2) 0.0113(18) -0.0094(17) -0.0090(19) C5B 0.067(3) 0.088(4) 0.034(2) -0.008(2) 0.008(2) -0.052(3) C6C 0.041(2) 0.053(3) 0.042(2) 0.012(2) -0.013(2) -0.007(2) C6B 0.062(3) 0.072(4) 0.037(2) 0.005(2) -0.010(2) -0.040(3) C7B 0.067(3) 0.068(4) 0.049(3) 0.003(2) -0.007(2) -0.039(3) C7C 0.047(3) 0.068(3) 0.046(3) 0.018(2) -0.022(2) -0.020(2) C8C 0.038(2) 0.039(2) 0.035(2) 0.0058(17) -0.0067(18) -0.0039(18) C8B 0.067(3) 0.100(4) 0.032(2) -0.015(3) 0.009(2) -0.060(3) C9C 0.046(3) 0.044(3) 0.047(3) 0.010(2) -0.009(2) -0.001(2) C9B 0.100(5) 0.110(5) 0.046(3) -0.030(3) 0.016(3) -0.065(4) C10B 0.116(6) 0.147(7) 0.050(3) -0.037(4) 0.031(4) -0.085(5) C10C 0.058(3) 0.038(3) 0.058(3) 0.008(2) -0.007(2) -0.001(2) C11C 0.063(3) 0.037(2) 0.049(3) 0.002(2) -0.003(2) -0.012(2) C11B 0.073(4) 0.104(5) 0.088(4) -0.066(4) 0.036(3) -0.050(4) C12B 0.057(3) 0.078(4) 0.060(3) -0.033(3) 0.022(3) -0.044(3) C12C 0.040(2) 0.038(2) 0.038(2) 0.0004(18) -0.0026(18) -0.0092(18) C13C 0.034(2) 0.034(2) 0.032(2) 0.0027(16) -0.0008(17) -0.0038(17) C13B 0.045(3) 0.070(3) 0.054(3) -0.034(3) 0.012(2) -0.038(2) C14C 0.043(2) 0.038(2) 0.0254(19) -0.0001(16) -0.0128(18) -0.0076(19) C14B 0.046(3) 0.048(3) 0.037(2) -0.0141(19) 0.0058(19) -0.028(2) C15C 0.040(2) 0.036(2) 0.036(2) -0.0078(17) 0.0022(18) -0.0108(18) C15B 0.041(3) 0.067(3) 0.092(4) -0.060(3) 0.028(3) -0.033(2) C16B 0.069(4) 0.065(4) 0.107(5) -0.049(4) 0.025(3) -0.040(3) C16C 0.048(3) 0.036(2) 0.050(3) -0.0079(19) 0.005(2) -0.013(2) C17C 0.047(3) 0.046(3) 0.060(3) -0.022(2) 0.000(2) -0.021(2) C17B 0.058(4) 0.057(4) 0.152(7) -0.058(4) 0.036(4) -0.025(3) C18C 0.038(2) 0.049(3) 0.043(2) -0.016(2) -0.0007(19) -0.010(2) C18B 0.095(5) 0.032(3) 0.151(6) -0.026(3) 0.034(5) -0.022(3) C19B 0.077(4) 0.050(3) 0.124(5) -0.035(4) 0.049(4) -0.029(3) C19C 0.040(2) 0.046(2) 0.029(2) -0.0081(17) 0.0035(17) -0.0097(19) C20C 0.035(2) 0.045(2) 0.033(2) -0.0051(18) 0.0006(17) -0.0148(18) C20B 0.069(4) 0.043(3) 0.099(4) -0.040(3) 0.035(3) -0.030(3) C21C 0.055(3) 0.084(4) 0.058(3) -0.022(3) -0.010(2) -0.025(3) C21B 0.139(8) 0.059(5) 0.221(11) 0.023(6) 0.056(7) 0.013(5) C1M 0.036(2) 0.043(2) 0.041(2) -0.0065(18) -0.0095(18) -0.0154(18) C1 0.091(4) 0.069(4) 0.053(3) 0.017(3) -0.020(3) -0.018(3) C1A 0.068(4) 0.072(4) 0.062(3) -0.008(3) -0.023(3) -0.024(3) C2A 0.043(2) 0.059(3) 0.036(2) -0.008(2) -0.0051(19) -0.014(2) C2 0.063(3) 0.037(2) 0.049(3) 0.005(2) -0.018(2) -0.015(2) C2M 0.054(3) 0.091(4) 0.072(3) -0.027(3) -0.017(3) -0.037(3) C3M 0.052(3) 0.052(3) 0.046(3) 0.001(2) -0.018(2) -0.011(2) C3A 0.044(3) 0.056(3) 0.041(2) -0.003(2) -0.013(2) -0.004(2) C3 0.058(3) 0.043(3) 0.061(3) 0.007(2) -0.026(3) -0.007(2) C4 0.040(2) 0.043(3) 0.063(3) -0.001(2) -0.009(2) -0.004(2) C4A 0.053(3) 0.042(3) 0.038(2) -0.0027(19) -0.007(2) -0.010(2) C4M 0.056(3) 0.045(3) 0.048(3) -0.001(2) -0.018(2) -0.021(2) C5 0.037(2) 0.026(2) 0.047(2) -0.0001(17) -0.0099(19) -0.0067(17) C5A 0.039(2) 0.041(2) 0.0239(19) 0.0000(16) -0.0006(16) -0.0110(18) C6A 0.038(2) 0.046(2) 0.0240(19) -0.0042(17) -0.0021(16) -0.0073(18) C6 0.040(2) 0.034(2) 0.047(2) 0.0042(18) -0.009(2) -0.0057(18) C7A 0.049(3) 0.045(3) 0.032(2) -0.0070(18) -0.0043(19) -0.014(2) C7 0.048(3) 0.040(2) 0.049(3) 0.002(2) -0.002(2) -0.012(2) C8A 0.044(2) 0.039(2) 0.032(2) -0.0003(17) 0.0006(18) -0.0150(19) C8 0.030(2) 0.035(2) 0.044(2) -0.0063(18) -0.0030(18) -0.0054(17) C9 0.051(3) 0.028(2) 0.056(3) -0.0062(19) 0.004(2) -0.0004(19) C9A 0.073(3) 0.055(3) 0.038(2) 0.009(2) -0.003(2) -0.030(3) C10A 0.095(4) 0.059(3) 0.057(3) 0.020(3) -0.010(3) -0.050(3) C10 0.060(3) 0.046(3) 0.054(3) -0.021(2) 0.010(2) -0.011(2) C11A 0.073(3) 0.058(3) 0.053(3) 0.007(2) -0.005(3) -0.045(3) C11 0.055(3) 0.043(3) 0.037(2) -0.0126(19) 0.002(2) -0.012(2) C12A 0.039(2) 0.042(2) 0.037(2) -0.0052(18) 0.0036(18) -0.0198(19) C12 0.036(2) 0.035(2) 0.034(2) -0.0105(17) 0.0015(17) -0.0157(17) C13A 0.0292(19) 0.035(2) 0.0291(19) -0.0035(16) 0.0051(15) -0.0121(16) C13 0.0267(19) 0.031(2) 0.034(2) -0.0064(16) -0.0035(16) -0.0086(15) C14A 0.036(2) 0.033(2) 0.0254(18) -0.0037(15) -0.0050(16) -0.0167(17) C14 0.036(2) 0.0256(19) 0.0280(19) -0.0014(15) -0.0001(16) -0.0112(16) C15A 0.033(2) 0.034(2) 0.042(2) -0.0077(17) 0.0003(17) -0.0134(17) C15 0.033(2) 0.036(2) 0.0256(18) -0.0081(16) -0.0001(16) -0.0120(16) C16A 0.037(2) 0.058(3) 0.052(3) -0.013(2) 0.005(2) -0.027(2) C16 0.044(2) 0.043(2) 0.039(2) -0.0059(18) -0.0096(19) -0.0179(19) C17 0.037(2) 0.052(3) 0.041(2) -0.003(2) -0.0098(19) -0.011(2) C17A 0.038(2) 0.067(3) 0.059(3) -0.015(2) -0.008(2) -0.026(2) C18 0.036(2) 0.040(2) 0.038(2) -0.0039(18) 0.0023(18) -0.0059(18) C18A 0.043(2) 0.051(3) 0.050(3) -0.018(2) -0.008(2) -0.014(2) C19A 0.038(2) 0.046(3) 0.039(2) -0.0116(19) -0.0008(18) -0.0124(19) C19 0.047(2) 0.039(2) 0.039(2) -0.0077(18) -0.0032(19) -0.0176(19) C20A 0.030(2) 0.037(2) 0.042(2) -0.0110(17) -0.0002(17) -0.0124(17) C20 0.040(2) 0.038(2) 0.035(2) -0.0064(17) -0.0077(18) -0.0122(18) C21A 0.063(3) 0.087(4) 0.067(3) -0.025(3) -0.017(3) -0.024(3) C21 0.061(3) 0.050(3) 0.061(3) 0.005(2) -0.011(3) -0.004(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 Fe2 O1C 1.980(3) . ? Fe2 O2C 2.017(3) 2_645 ? Fe2 N1N 2.085(3) . ? Fe2 O2B 2.090(3) . ? Fe2 O1B 2.315(3) . ? Fe1 O1A 1.950(3) . ? Fe1 O2A 2.015(3) . ? Fe1 O1 2.025(3) . ? Fe1 N1M 2.092(3) . ? O1A C14A 1.254(4) . ? O1 C14 1.284(4) . ? O2 C14 1.230(4) . ? O2A C14A 1.255(4) 2_754 ? O1B C14B 1.247(5) . ? O1C C14C 1.250(5) . ? O2B C14B 1.283(5) . ? O2C C14C 1.251(5) . ? O2C Fe2 2.017(3) 2_645 ? N1N C1N 1.321(5) . ? N1N C4N 1.383(5) . ? N2N C1N 1.344(5) . ? N2N C3N 1.368(5) . ? N2N C2N 1.473(5) . ? N1M C1M 1.321(5) . ? N1M C4M 1.364(5) . ? N2M C1M 1.348(5) . ? N2M C3M 1.363(6) . ? N2M C2M 1.463(5) . ? C1C C2C 1.507(7) . ? C1B C2B 1.496(8) . ? C2C C7C 1.387(7) . ? C2C C3C 1.399(7) . ? C2B C3B 1.381(8) . ? C2B C7B 1.408(7) . ? C3N C4N 1.350(5) . ? C3C C4C 1.376(6) . ? C3B C4B 1.369(9) . ? C4C C5C 1.396(6) . ? C4B C5B 1.411(8) . ? C5C C6C 1.405(6) . ? C5C C8C 1.491(6) . ? C5B C6B 1.397(6) . ? C5B C8B 1.471(8) . ? C6C C7C 1.378(6) . ? C6B C7B 1.364(7) . ? C8C C13C 1.400(5) . ? C8C C9C 1.396(6) . ? C8B C9B 1.389(7) . ? C8B C13B 1.411(7) . ? C9C C10C 1.378(6) . ? C9B C10B 1.364(9) . ? C10B C11B 1.375(9) . ? C10C C11C 1.388(6) . ? C11C C12C 1.396(6) . ? C11B C12B 1.428(7) . ? C12B C13B 1.383(7) . ? C12B C15B 1.474(8) . ? C12C C13C 1.396(5) . ? C12C C15C 1.501(6) . ? C13C C14C 1.519(5) . ? C13B C14B 1.514(6) . ? C15C C20C 1.389(5) . ? C15C C16C 1.399(5) . ? C15B C20B 1.406(7) . ? C15B C16B 1.396(8) . ? C16B C17B 1.355(9) . ? C16C C17C 1.392(6) . ? C17C C18C 1.380(6) . ? C17B C18B 1.397(9) . ? C18C C19C 1.384(6) . ? C18C C21C 1.516(6) . ? C18B C19B 1.402(8) . ? C18B C21B 1.497(10) . ? C19B C20B 1.379(8) . ? C19C C20C 1.379(5) . ? C1 C2 1.514(6) . ? C1A C2A 1.498(6) . ? C2A C7A 1.387(6) . ? C2A C3A 1.396(6) . ? C2 C3 1.388(7) . ? C2 C7 1.383(6) . ? C3M C4M 1.350(6) . ? C3A C4A 1.379(6) . ? C3 C4 1.389(6) . ? C4 C5 1.397(6) . ? C4A C5A 1.404(6) . ? C5 C6 1.386(6) . ? C5 C8 1.492(6) . ? C5A C6A 1.390(5) . ? C5A C8A 1.487(5) . ? C6A C7A 1.396(5) . ? C6 C7 1.381(6) . ? C8A C9A 1.391(6) . ? C8A C13A 1.416(5) . ? C8 C13 1.406(5) . ? C8 C9 1.397(6) . ? C9 C10 1.378(6) . ? C9A C10A 1.380(6) . ? C10A C11A 1.378(7) . ? C10 C11 1.382(6) . ? C11A C12A 1.403(6) . ? C11 C12 1.393(5) . ? C12A C13A 1.401(5) . ? C12A C15A 1.503(5) . ? C12 C13 1.401(5) . ? C12 C15 1.492(5) . ? C13A C14A 1.507(5) . ? C13 C14 1.506(5) . ? C14A O2A 1.255(4) 2_754 ? C15A C20A 1.389(5) . ? C15A C16A 1.402(5) . ? C15 C16 1.388(5) . ? C15 C20 1.392(5) . ? C16A C17A 1.376(6) . ? C16 C17 1.377(6) . ? C17 C18 1.383(6) . ? C17A C18A 1.384(6) . ? C18 C19 1.385(6) . ? C18 C21 1.507(6) . ? C18A C19A 1.388(6) . ? C18A C21A 1.515(6) . ? C19A C20A 1.389(5) . ? C19 C20 1.377(5) . ? C1S Cl1B 1.460(12) . ? C1S Cl1A 1.651(13) . ? C1S Cl2 1.670(13) . ? C1S Cl2A 1.977(13) . ? C1S Cl1 1.976(13) . ? C1S Cl2B 2.141(13) . ? Cl1B C2S 1.728(17) . ? Cl2B C2S 1.725(17) . ? C10S Cl10 1.61(2) . ? C10S Cl11 1.57(2) . ? C22S C20S 0.91(4) . ? C20S C21S 1.60(4) . ? C21S C21S 1.10(5) 2_966 ? 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 O1C Fe2 O2C 119.54(13) . 2_645 ? O1C Fe2 N1N 98.26(12) . . ? O2C Fe2 N1N 94.09(12) 2_645 . ? O1C Fe2 O2B 124.76(12) . . ? O2C Fe2 O2B 112.76(12) 2_645 . ? N1N Fe2 O2B 94.48(11) . . ? O1C Fe2 O1B 89.81(11) . . ? O2C Fe2 O1B 105.18(11) 2_645 . ? N1N Fe2 O1B 152.00(11) . . ? O2B Fe2 O1B 59.55(10) . . ? O1A Fe1 O2A 118.74(12) . . ? O1A Fe1 O1 125.25(11) . . ? O2A Fe1 O1 111.27(11) . . ? O1A Fe1 N1M 104.64(12) . . ? O2A Fe1 N1M 93.47(12) . . ? O1 Fe1 N1M 92.77(12) . . ? C14A O1A Fe1 153.9(3) . . ? C14 O1 Fe1 99.3(2) . . ? C14A O2A Fe1 136.9(2) 2_754 . ? C14B O1B Fe2 85.0(2) . . ? C14C O1C Fe2 140.1(3) . . ? C14B O2B Fe2 94.2(2) . . ? C14C O2C Fe2 147.9(3) . 2_645 ? C1N N1N C4N 104.8(3) . . ? C1N N1N Fe2 127.1(3) . . ? C4N N1N Fe2 127.4(3) . . ? C1N N2N C3N 107.3(3) . . ? C1N N2N C2N 126.7(4) . . ? C3N N2N C2N 126.0(3) . . ? C1M N1M C4M 105.5(3) . . ? C1M N1M Fe1 126.9(3) . . ? C4M N1M Fe1 126.2(3) . . ? C1M N2M C3M 107.5(3) . . ? C1M N2M C2M 126.1(4) . . ? C3M N2M C2M 126.4(4) . . ? N1N C1N N2N 111.7(4) . . ? C7C C2C C3C 116.8(4) . . ? C7C C2C C1C 121.3(5) . . ? C3C C2C C1C 121.8(5) . . ? C3B C2B C7B 116.0(6) . . ? C3B C2B C1B 122.3(6) . . ? C7B C2B C1B 121.7(5) . . ? C4N C3N N2N 106.2(3) . . ? C4C C3C C2C 122.3(5) . . ? C4B C3B C2B 122.1(6) . . ? C3C C4C C5C 120.5(4) . . ? C3N C4N N1N 110.0(4) . . ? C3B C4B C5B 121.9(5) . . ? C4C C5C C6C 117.5(4) . . ? C4C C5C C8C 122.5(4) . . ? C6C C5C C8C 120.0(4) . . ? C6B C5B C4B 116.1(5) . . ? C6B C5B C8B 121.5(5) . . ? C4B C5B C8B 122.3(5) . . ? C7C C6C C5C 121.1(5) . . ? C7B C6B C5B 121.3(5) . . ? C6B C7B C2B 122.6(5) . . ? C6C C7C C2C 121.7(4) . . ? C13C C8C C9C 118.4(4) . . ? C13C C8C C5C 123.0(4) . . ? C9C C8C C5C 118.5(4) . . ? C9B C8B C13B 118.3(6) . . ? C9B C8B C5B 119.7(5) . . ? C13B C8B C5B 122.0(4) . . ? C10C C9C C8C 121.3(4) . . ? C10B C9B C8B 121.3(6) . . ? C9B C10B C11B 121.0(6) . . ? C9C C10C C11C 120.0(4) . . ? C10C C11C C12C 120.1(4) . . ? C10B C11B C12B 119.6(6) . . ? C13B C12B C11B 118.6(6) . . ? C13B C12B C15B 122.9(4) . . ? C11B C12B C15B 118.5(5) . . ? C11C C12C C13C 119.4(4) . . ? C11C C12C C15C 118.1(4) . . ? C13C C12C C15C 122.3(4) . . ? C12C C13C C8C 120.7(4) . . ? C12C C13C C14C 119.0(3) . . ? C8C C13C C14C 120.4(4) . . ? C12B C13B C8B 121.1(5) . . ? C12B C13B C14B 121.6(5) . . ? C8B C13B C14B 117.3(4) . . ? O1C C14C O2C 126.4(4) . . ? O1C C14C C13C 116.9(3) . . ? O2C C14C C13C 116.7(4) . . ? O1B C14B O2B 120.5(4) . . ? O1B C14B C13B 119.7(4) . . ? O2B C14B C13B 119.7(4) . . ? C20C C15C C16C 117.5(4) . . ? C20C C15C C12C 121.1(4) . . ? C16C C15C C12C 121.3(4) . . ? C20B C15B C16B 116.1(6) . . ? C20B C15B C12B 122.8(5) . . ? C16B C15B C12B 121.1(5) . . ? C17B C16B C15B 122.2(6) . . ? C15C C16C C17C 120.2(4) . . ? C18C C17C C16C 121.9(4) . . ? C16B C17B C18B 122.3(6) . . ? C17C C18C C19C 117.6(4) . . ? C17C C18C C21C 122.0(4) . . ? C19C C18C C21C 120.4(4) . . ? C17B C18B C19B 116.4(7) . . ? C17B C18B C21B 123.2(7) . . ? C19B C18B C21B 120.4(7) . . ? C20B C19B C18B 121.3(6) . . ? C20C C19C C18C 121.2(4) . . ? C19C C20C C15C 121.6(4) . . ? C19B C20B C15B 121.6(5) . . ? N1M C1M N2M 110.8(4) . . ? C7A C2A C3A 117.5(4) . . ? C7A C2A C1A 120.1(4) . . ? C3A C2A C1A 122.4(4) . . ? C3 C2 C7 117.0(4) . . ? C3 C2 C1 121.5(4) . . ? C7 C2 C1 121.6(5) . . ? C4M C3M N2M 105.8(4) . . ? C4A C3A C2A 121.8(4) . . ? C2 C3 C4 122.0(4) . . ? C5 C4 C3 120.6(4) . . ? C3A C4A C5A 120.8(4) . . ? C3M C4M N1M 110.4(4) . . ? C4 C5 C6 116.9(4) . . ? C4 C5 C8 120.8(4) . . ? C6 C5 C8 122.2(4) . . ? C6A C5A C4A 117.4(4) . . ? C6A C5A C8A 122.5(4) . . ? C4A C5A C8A 120.0(4) . . ? C5A C6A C7A 121.4(4) . . ? C5 C6 C7 122.1(4) . . ? C2A C7A C6A 121.0(4) . . ? C6 C7 C2 121.4(4) . . ? C9A C8A C13A 117.9(4) . . ? C9A C8A C5A 119.7(4) . . ? C13A C8A C5A 122.4(3) . . ? C13 C8 C9 118.6(4) . . ? C13 C8 C5 122.3(3) . . ? C9 C8 C5 118.9(4) . . ? C10 C9 C8 120.6(4) . . ? C10A C9A C8A 121.5(4) . . ? C9A C10A C11A 120.0(4) . . ? C11 C10 C9 120.7(4) . . ? C10A C11A C12A 121.2(4) . . ? C10 C11 C12 120.4(4) . . ? C11A C12A C13A 118.1(4) . . ? C11A C12A C15A 118.1(4) . . ? C13A C12A C15A 123.7(3) . . ? C11 C12 C13 118.9(4) . . ? C11 C12 C15 118.8(3) . . ? C13 C12 C15 122.2(3) . . ? C12A C13A C8A 121.2(3) . . ? C12A C13A C14A 120.7(3) . . ? C8A C13A C14A 118.1(3) . . ? C12 C13 C8 120.8(3) . . ? C12 C13 C14 119.9(3) . . ? C8 C13 C14 119.4(3) . . ? O2A C14A O1A 126.1(3) 2_754 . ? O2A C14A C13A 117.4(3) 2_754 . ? O1A C14A C13A 116.5(3) . . ? O2 C14 O1 121.6(3) . . ? O2 C14 C13 121.5(3) . . ? O1 C14 C13 116.9(3) . . ? C20A C15A C16A 117.2(4) . . ? C20A C15A C12A 122.6(3) . . ? C16A C15A C12A 120.1(4) . . ? C16 C15 C20 117.7(4) . . ? C16 C15 C12 121.8(3) . . ? C20 C15 C12 120.5(3) . . ? C17A C16A C15A 121.6(4) . . ? C15 C16 C17 121.1(4) . . ? C18 C17 C16 121.4(4) . . ? C16A C17A C18A 121.0(4) . . ? C19 C18 C17 117.5(4) . . ? C19 C18 C21 121.2(4) . . ? C17 C18 C21 121.3(4) . . ? C17A C18A C19A 117.8(4) . . ? C17A C18A C21A 120.6(4) . . ? C19A C18A C21A 121.6(4) . . ? C18A C19A C20A 121.5(4) . . ? C18 C19 C20 121.6(4) . . ? C15A C20A C19A 120.7(4) . . ? C19 C20 C15 120.7(4) . . ? Cl1B C1S Cl1A 16.9(4) . . ? Cl1B C1S Cl2 75.0(7) . . ? Cl1A C1S Cl2 90.9(7) . . ? Cl1B C1S Cl2A 91.1(7) . . ? Cl1A C1S Cl2A 106.8(7) . . ? Cl2 C1S Cl2A 16.2(4) . . ? Cl1B C1S Cl1 32.1(4) . . ? Cl1A C1S Cl1 15.4(3) . . ? Cl2 C1S Cl1 106.0(7) . . ? Cl2A C1S Cl1 121.8(7) . . ? Cl1B C1S Cl2B 105.7(7) . . ? Cl1A C1S Cl2B 120.8(7) . . ? Cl2 C1S Cl2B 31.1(4) . . ? Cl2A C1S Cl2B 15.1(2) . . ? Cl1 C1S Cl2B 135.2(7) . . ? C1S Cl1B C2S 12.8(7) . . ? C2S Cl2B C1S 4.7(7) . . ? Cl2B C2S Cl1B 114.2(9) . . ? Cl10 C10S Cl11 120.2(13) . . ? C22S C20S C21S 88(3) . . ? C21S C21S C20S 124(4) 2_966 . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.964 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.099 data_structure _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe2(m-OH)2(m-O2CAr)2(O2CAr)2(py)2] _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H80 Cl6 Fe2 N2 O10' _chemical_formula_weight 1758.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7957(2) _cell_length_b 15.4489(2) _cell_length_c 22.27310(10) _cell_angle_alpha 91.8950(10) _cell_angle_beta 102.2890(10) _cell_angle_gamma 103.7510(10) _cell_volume 4487.78(9) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'greenish ye' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.735962 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26809 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 28.20 _reflns_number_total 18901 _reflns_number_gt 13454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1020P)^2^+3.0620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18901 _refine_ls_number_parameters 1102 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 1.542 _refine_ls_shift/su_mean 0.029 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 0.06994(3) 1.03918(3) 1.557440(19) 0.02271(11) Uani 1 1 d . . . Fe2 Fe -0.06689(3) 1.46496(3) 1.03885(2) 0.02376(12) Uani 1 1 d . . . O1C O -0.14626(16) 1.55384(14) 0.99931(10) 0.0278(5) Uani 1 1 d . . . O1 O 0.18400(16) 1.14345(14) 1.59303(10) 0.0287(5) Uani 1 1 d . . . O1B O 0.14734(16) 0.95104(14) 1.53361(9) 0.0252(4) Uani 1 1 d . . . O1D O -0.18144(17) 1.36081(14) 1.03776(10) 0.0303(5) Uani 1 1 d . . . O2B O 0.04216(16) 0.89244(14) 1.44065(10) 0.0262(5) Uani 1 1 d . . . O2C O 0.04367(16) 1.39264(14) 1.06532(10) 0.0282(5) Uani 1 1 d . . . O2 O 0.1947(2) 1.23433(16) 1.51683(11) 0.0408(6) Uani 1 1 d . . . O2D O -0.1901(2) 1.27165(17) 0.95402(13) 0.0514(7) Uani 1 1 d . . . O20 O -0.05758(18) 1.43739(18) 0.95331(11) 0.0288(5) Uani 1 1 d . . . O10 O -0.05560(17) 0.93691(16) 1.53068(10) 0.0274(5) Uani 1 1 d . . . N1 N 0.0965(2) 1.00097(18) 1.65024(12) 0.0291(6) Uani 1 1 d . . . N2 N -0.0854(2) 1.50087(18) 1.12880(12) 0.0296(6) Uani 1 1 d . . . C1A C -0.0950(3) 1.4715(3) 1.5812(2) 0.0514(10) Uani 1 1 d . . . H1A1 H -0.0883 1.5200 1.6111 0.077 Uiso 1 1 calc R . . H1A2 H -0.1497 1.4222 1.5854 0.077 Uiso 1 1 calc R . . H1A3 H -0.1099 1.4908 1.5405 0.077 Uiso 1 1 calc R . . C1P C 0.1898(3) 0.9941(3) 1.67810(18) 0.0478(10) Uani 1 1 d . . . H1PA H 0.2405 1.0023 1.6557 0.057 Uiso 1 1 calc R . . C1D C 0.0869(4) 1.0386(3) 1.1104(2) 0.0571(11) Uani 1 1 d . . . H1D1 H 0.1420 1.0883 1.1303 0.086 Uiso 1 1 calc R . . H1D2 H 0.1024 1.0157 1.0740 0.086 Uiso 1 1 calc R . . H1D3 H 0.0783 0.9925 1.1381 0.086 Uiso 1 1 calc R . . C1Q C -0.0313(3) 1.4750(3) 1.17923(17) 0.0503(10) Uani 1 1 d . . . H1QA H 0.0195 1.4465 1.1752 0.060 Uiso 1 1 calc R . . C1B C -0.0217(4) 0.7197(3) 1.7065(2) 0.0666(13) Uani 1 1 d . . . H1B1 H 0.0237 0.7160 1.7449 0.100 Uiso 1 1 calc R . . H1B2 H -0.0762 0.6660 1.6967 0.100 Uiso 1 1 calc R . . H1B3 H -0.0500 0.7703 1.7099 0.100 Uiso 1 1 calc R . . C1C C 0.0034(5) 1.2015(4) 0.7710(2) 0.0871(18) Uani 1 1 d . . . H1C1 H -0.0591 1.1552 0.7644 0.131 Uiso 1 1 calc R . . H1C2 H 0.0486 1.1842 0.7483 0.131 Uiso 1 1 calc R . . H1C3 H -0.0116 1.2561 0.7572 0.131 Uiso 1 1 calc R . . C2D C -0.0103(3) 1.0689(3) 1.09294(18) 0.0445(9) Uani 1 1 d . . . C2B C 0.0372(3) 0.7305(3) 1.65560(19) 0.0452(9) Uani 1 1 d . . . C2A C 0.0041(3) 1.4424(2) 1.59152(16) 0.0401(8) Uani 1 1 d . . . C2Q C -0.0489(4) 1.4896(4) 1.2370(2) 0.0669(14) Uani 1 1 d . . . H2QA H -0.0094 1.4718 1.2713 0.080 Uiso 1 1 calc R . . C2C C 0.0546(4) 1.2157(3) 0.8395(2) 0.0560(11) Uani 1 1 d . . . C2P C 0.2141(4) 0.9753(3) 1.7390(2) 0.0630(13) Uani 1 1 d . . . H2PA H 0.2797 0.9703 1.7569 0.076 Uiso 1 1 calc R . . C3D C -0.1016(3) 1.0095(3) 1.06200(19) 0.0482(10) Uani 1 1 d . . . H3DA H -0.1017 0.9507 1.0517 0.058 Uiso 1 1 calc R . . C3Q C -0.1241(3) 1.5300(3) 1.24394(18) 0.0517(10) Uani 1 1 d . . . H3QA H -0.1387 1.5378 1.2824 0.062 Uiso 1 1 calc R . . C3B C 0.1430(3) 0.7445(3) 1.6688(2) 0.0540(11) Uani 1 1 d . . . H3BA H 0.1781 0.7448 1.7094 0.065 Uiso 1 1 calc R . . C3A C 0.0941(3) 1.5011(2) 1.58536(18) 0.0437(9) Uani 1 1 d . . . H3AA H 0.0928 1.5581 1.5737 0.052 Uiso 1 1 calc R . . C3P C 0.1403(4) 0.9641(3) 1.77267(19) 0.0600(12) Uani 1 1 d . . . H3PA H 0.1551 0.9522 1.8138 0.072 Uiso 1 1 calc R . . C3C C 0.1599(4) 1.2243(3) 0.8603(2) 0.0547(11) Uani 1 1 d . . . H3CA H 0.1985 1.2171 0.8318 0.066 Uiso 1 1 calc R . . C4B C 0.1977(3) 0.7581(3) 1.62288(18) 0.0466(9) Uani 1 1 d . . . H4BA H 0.2686 0.7673 1.6332 0.056 Uiso 1 1 calc R . . C4Q C -0.1777(3) 1.5588(3) 1.19261(19) 0.0514(10) Uani 1 1 d . . . H4QA H -0.2277 1.5885 1.1960 0.062 Uiso 1 1 calc R . . C4A C 0.1856(3) 1.4760(2) 1.59622(18) 0.0435(9) Uani 1 1 d . . . H4AA H 0.2448 1.5166 1.5917 0.052 Uiso 1 1 calc R . . C4D C -0.1919(3) 1.0360(3) 1.04621(18) 0.0471(9) Uani 1 1 d . . . H4DA H -0.2514 0.9946 1.0254 0.057 Uiso 1 1 calc R . . C4C C 0.2077(3) 1.2431(3) 0.92170(18) 0.0439(9) Uani 1 1 d . . . H4CA H 0.2781 1.2502 0.9338 0.053 Uiso 1 1 calc R . . C4P C 0.0436(4) 0.9707(3) 1.7442(2) 0.0594(12) Uani 1 1 d . . . H4PA H -0.0082 0.9626 1.7657 0.071 Uiso 1 1 calc R . . C5B C 0.1477(3) 0.7582(2) 1.56141(16) 0.0318(7) Uani 1 1 d . . . C5D C -0.1957(3) 1.1244(2) 1.06098(16) 0.0386(8) Uani 1 1 d . . . C5A C 0.1914(3) 1.3904(2) 1.61398(16) 0.0359(8) Uani 1 1 d . . . C5C C 0.1518(3) 1.2517(2) 0.96660(17) 0.0362(8) Uani 1 1 d . . . C5Q C -0.1569(3) 1.5432(3) 1.13578(18) 0.0455(9) Uani 1 1 d . . . H5QA H -0.1938 1.5628 1.1012 0.055 Uiso 1 1 calc R . . C5P C 0.0245(3) 0.9894(3) 1.68310(17) 0.0431(9) Uani 1 1 d . . . H5PA H -0.0407 0.9942 1.6642 0.052 Uiso 1 1 calc R . . C6B C 0.0414(3) 0.7418(2) 1.54779(17) 0.0340(7) Uani 1 1 d . . . H6BA H 0.0061 0.7397 1.5070 0.041 Uiso 1 1 calc R . . C6A C 0.1003(3) 1.3316(2) 1.61919(16) 0.0357(8) Uani 1 1 d . . . H6AA H 0.1012 1.2743 1.6303 0.043 Uiso 1 1 calc R . . C6C C 0.0458(3) 1.2398(2) 0.94661(19) 0.0423(9) Uani 1 1 d . . . H6CA H 0.0064 1.2436 0.9752 0.051 Uiso 1 1 calc R . . C6D C -0.1044(3) 1.1839(2) 1.09162(18) 0.0433(9) Uani 1 1 d . . . H6DA H -0.1042 1.2428 1.1018 0.052 Uiso 1 1 calc R . . C7B C -0.0133(3) 0.7282(2) 1.59448(18) 0.0397(8) Uani 1 1 d . . . H7BA H -0.0844 0.7174 1.5843 0.048 Uiso 1 1 calc R . . C7D C -0.0138(3) 1.1573(2) 1.10729(18) 0.0454(9) Uani 1 1 d . . . H7DA H 0.0459 1.1987 1.1277 0.054 Uiso 1 1 calc R . . C7A C 0.0087(3) 1.3565(2) 1.60827(16) 0.0383(8) Uani 1 1 d . . . H7AA H -0.0508 1.3156 1.6121 0.046 Uiso 1 1 calc R . . C7C C -0.0009(3) 1.2224(3) 0.8840(2) 0.0528(11) Uani 1 1 d . . . H7CA H -0.0713 1.2151 0.8716 0.063 Uiso 1 1 calc R . . C8B C 0.2078(2) 0.7781(2) 1.51255(15) 0.0296(7) Uani 1 1 d . . . C8C C 0.2055(3) 1.2717(2) 1.03297(16) 0.0317(7) Uani 1 1 d . . . C8D C -0.2971(3) 1.1482(2) 1.04506(17) 0.0399(8) Uani 1 1 d . . . C8A C 0.2924(3) 1.3673(2) 1.63178(17) 0.0389(8) Uani 1 1 d . . . C9B C 0.2779(3) 0.7280(2) 1.50485(17) 0.0355(8) Uani 1 1 d . . . H9BA H 0.2860 0.6818 1.5297 0.043 Uiso 1 1 calc R . . C9C C 0.2700(3) 1.2187(2) 1.05989(19) 0.0408(9) Uani 1 1 d . . . H9CA H 0.2783 1.1717 1.0359 0.049 Uiso 1 1 calc R . . C9A C 0.3738(3) 1.4310(3) 1.6697(2) 0.0589(12) Uani 1 1 d . . . H9AA H 0.3645 1.4865 1.6807 0.071 Uiso 1 1 calc R . . C9D C -0.3826(4) 1.0889(3) 1.0584(2) 0.0581(12) Uani 1 1 d . . . H9DA H -0.3744 1.0383 1.0784 0.070 Uiso 1 1 calc R . . C10B C 0.3347(3) 0.7471(2) 1.46053(18) 0.0377(8) Uani 1 1 d . . . H10A H 0.3806 0.7135 1.4556 0.045 Uiso 1 1 calc R . . C10C C 0.3212(3) 1.2347(3) 1.12098(19) 0.0458(9) Uani 1 1 d . . . H10C H 0.3624 1.1980 1.1381 0.055 Uiso 1 1 calc R . . C10D C -0.4793(4) 1.1052(3) 1.0419(3) 0.0698(14) Uani 1 1 d . . . H10D H -0.5353 1.0654 1.0510 0.084 Uiso 1 1 calc R . . C10A C 0.4682(4) 1.4126(3) 1.6911(3) 0.0715(15) Uani 1 1 d . . . H10B H 0.5225 1.4563 1.7149 0.086 Uiso 1 1 calc R . . C11B C 0.3236(2) 0.8162(2) 1.42336(16) 0.0320(7) Uani 1 1 d . . . H11A H 0.3628 0.8287 1.3941 0.038 Uiso 1 1 calc R . . C11C C 0.3113(3) 1.3054(2) 1.15671(17) 0.0380(8) Uani 1 1 d . . . H11C H 0.3474 1.3165 1.1977 0.046 Uiso 1 1 calc R . . C11A C 0.4811(3) 1.3286(3) 1.6767(2) 0.0624(13) Uani 1 1 d . . . H11B H 0.5436 1.3157 1.6925 0.075 Uiso 1 1 calc R . . C12B C 0.2544(2) 0.8675(2) 1.42925(14) 0.0267(6) Uani 1 1 d . . . C12A C 0.4017(3) 1.2630(2) 1.63896(18) 0.0412(8) Uani 1 1 d . . . C12C C 0.2481(3) 1.3607(2) 1.13272(16) 0.0310(7) Uani 1 1 d . . . C12D C -0.4093(3) 1.2411(3) 0.9987(2) 0.0456(9) Uani 1 1 d . . . C13B C 0.1964(2) 0.8466(2) 1.47436(14) 0.0245(6) Uani 1 1 d . . . C13A C 0.3076(3) 1.2836(2) 1.61516(16) 0.0342(7) Uani 1 1 d . . . C13C C 0.1942(2) 1.3423(2) 1.07043(15) 0.0285(7) Uani 1 1 d . . . C13D C -0.3109(3) 1.2253(2) 1.01607(17) 0.0363(8) Uani 1 1 d . . . C14B C 0.1220(2) 0.90114(19) 1.48338(14) 0.0238(6) Uani 1 1 d . . . C14D C -0.2202(3) 1.2903(2) 0.99995(16) 0.0327(7) Uani 1 1 d . . . C15B C 0.2489(2) 0.9444(2) 1.39084(15) 0.0286(7) Uani 1 1 d . . . C15C C 0.2437(2) 1.4388(2) 1.17230(15) 0.0319(7) Uani 1 1 d . . . C15A C 0.4199(3) 1.1724(2) 1.62754(18) 0.0390(8) Uani 1 1 d . . . C15D C -0.4311(3) 1.3184(3) 0.9650(2) 0.0481(10) Uani 1 1 d . . . C16B C 0.2521(3) 0.9370(3) 1.32827(16) 0.0380(8) Uani 1 1 d . . . H16A H 0.2536 0.8824 1.3101 0.046 Uiso 1 1 calc R . . C16A C 0.4578(3) 1.1287(3) 1.67749(18) 0.0453(9) Uani 1 1 d . . . H16B H 0.4710 1.1561 1.7172 0.054 Uiso 1 1 calc R . . C16C C 0.2355(3) 1.4301(3) 1.23342(17) 0.0416(8) Uani 1 1 d . . . H16C H 0.2331 1.3749 1.2493 0.050 Uiso 1 1 calc R . . C16D C -0.5023(4) 1.3022(4) 0.9079(3) 0.0679(13) Uani 1 1 d . . . H16D H -0.5314 1.2435 0.8909 0.081 Uiso 1 1 calc R . . C17D C -0.5302(4) 1.3722(4) 0.8761(3) 0.0787(16) Uani 1 1 d . . . H17C H -0.5762 1.3597 0.8379 0.094 Uiso 1 1 calc R . . C17B C 0.2529(3) 1.0086(3) 1.29339(17) 0.0442(9) Uani 1 1 d . . . H17A H 0.2547 1.0012 1.2521 0.053 Uiso 1 1 calc R . . C17A C 0.4763(3) 1.0450(3) 1.66918(19) 0.0471(9) Uani 1 1 d . . . H17B H 0.5012 1.0170 1.7034 0.057 Uiso 1 1 calc R . . C17C C 0.2309(3) 1.5020(3) 1.27086(19) 0.0517(10) Uani 1 1 d . . . H17D H 0.2256 1.4946 1.3114 0.062 Uiso 1 1 calc R . . C18A C 0.4580(3) 1.0024(3) 1.61028(19) 0.0416(9) Uani 1 1 d . . . C18B C 0.2511(3) 1.0923(3) 1.31815(19) 0.0439(9) Uani 1 1 d . . . C18C C 0.2342(3) 1.5855(3) 1.2480(2) 0.0523(10) Uani 1 1 d . . . C18D C -0.4897(4) 1.4604(4) 0.9011(3) 0.0718(15) Uani 1 1 d . . . C19B C 0.2469(3) 1.1002(2) 1.37981(17) 0.0357(8) Uani 1 1 d . . . H19A H 0.2451 1.1550 1.3976 0.043 Uiso 1 1 calc R . . C19A C 0.4213(3) 1.0466(3) 1.56045(19) 0.0429(9) Uani 1 1 d . . . H19B H 0.4089 1.0194 1.5208 0.051 Uiso 1 1 calc R . . C19C C 0.2441(3) 1.5947(3) 1.18774(19) 0.0480(10) Uani 1 1 d . . . H19C H 0.2470 1.6500 1.1720 0.058 Uiso 1 1 calc R . . C19D C -0.4187(4) 1.4770(3) 0.9570(3) 0.0695(15) Uani 1 1 d . . . H19D H -0.3901 1.5358 0.9737 0.083 Uiso 1 1 calc R . . C20B C 0.2455(2) 1.0277(2) 1.41569(16) 0.0304(7) Uani 1 1 d . . . H20A H 0.2421 1.0349 1.4568 0.036 Uiso 1 1 calc R . . C20C C 0.2497(3) 1.5226(2) 1.15031(17) 0.0379(8) Uani 1 1 d . . . H20C H 0.2575 1.5308 1.1103 0.046 Uiso 1 1 calc R . . C20A C 0.4025(3) 1.1305(3) 1.56819(18) 0.0406(8) Uani 1 1 d . . . H20B H 0.3784 1.1587 1.5339 0.049 Uiso 1 1 calc R . . C20D C -0.3889(3) 1.4078(3) 0.9889(2) 0.0577(12) Uani 1 1 d . . . H20D H -0.3406 1.4211 1.0262 0.069 Uiso 1 1 calc R . . C21A C 0.4781(3) 0.9114(3) 1.6013(2) 0.0541(11) Uani 1 1 d . . . H21A H 0.5436 0.9109 1.6266 0.081 Uiso 1 1 calc R . . H21B H 0.4778 0.8988 1.5588 0.081 Uiso 1 1 calc R . . H21C H 0.4256 0.8667 1.6129 0.081 Uiso 1 1 calc R . . C21B C 0.2569(4) 1.1722(3) 1.2801(2) 0.0687(14) Uani 1 1 d . . . H21D H 0.1931 1.1651 1.2507 0.103 Uiso 1 1 calc R . . H21E H 0.3112 1.1765 1.2588 0.103 Uiso 1 1 calc R . . H21F H 0.2701 1.2258 1.3069 0.103 Uiso 1 1 calc R . . C21C C 0.2241(5) 1.6630(4) 1.2877(3) 0.0821(17) Uani 1 1 d . . . H21G H 0.1531 1.6628 1.2820 0.123 Uiso 1 1 calc R . . H21H H 0.2611 1.7183 1.2760 0.123 Uiso 1 1 calc R . . H21I H 0.2517 1.6570 1.3303 0.123 Uiso 1 1 calc R . . C21D C -0.5227(4) 1.5355(4) 0.8676(4) 0.101(2) Uani 1 1 d . . . H21J H -0.5099 1.5335 0.8269 0.152 Uiso 1 1 calc R . . H21K H -0.4846 1.5918 0.8899 0.152 Uiso 1 1 calc R . . H21L H -0.5945 1.5290 0.8647 0.152 Uiso 1 1 calc R . . C14A C 0.2221(2) 1.2162(2) 1.57021(15) 0.0294(7) Uani 1 1 d . . . C14C C 0.1222(2) 1.39848(19) 1.04355(14) 0.0252(6) Uani 1 1 d . . . C11D C -0.4927(3) 1.1795(3) 1.0122(2) 0.0627(13) Uani 1 1 d . . . H11D H -0.5580 1.1890 1.0009 0.075 Uiso 1 1 calc R . . C1S C 0.3744(5) 1.3948(5) 1.4868(3) 0.0950(19) Uiso 1 1 d . . . Cl1 Cl 0.4302(7) 1.3289(6) 1.4596(6) 0.120(4) Uiso 0.285(11) 1 d P A 1 Cl2 Cl 0.3386(7) 1.4581(8) 1.4263(6) 0.125(4) Uiso 0.285(11) 1 d P A 1 Cl1A Cl 0.3438(3) 1.4878(3) 1.4545(3) 0.0920(16) Uiso 0.531(11) 1 d P A 1 Cl2A Cl 0.4425(5) 1.3394(4) 1.4319(4) 0.137(2) Uiso 0.531(11) 1 d P A 1 Cl2B Cl 0.3428(15) 1.3618(12) 1.4107(9) 0.174(8) Uiso 0.180(6) 1 d P A 1 Cl1B Cl 0.3612(7) 1.5183(7) 1.4861(6) 0.085(3) Uiso 0.180(6) 1 d P A 1 C10S C 0.6303(11) 1.1267(9) 0.8496(7) 0.103(4) Uiso 0.564(4) 1 d P B 3 Cl10 Cl 0.7033(3) 1.0421(3) 0.87323(16) 0.1065(12) Uiso 0.564(4) 1 d P B 3 Cl11 Cl 0.49991(18) 1.07489(16) 0.84320(11) 0.0701(8) Uiso 0.564(4) 1 d P B 3 C10T C 0.631(2) 1.1067(16) 0.8859(12) 0.071(6) Uiso 0.243(7) 1 d P C 4 Cl20 Cl 0.6647(6) 0.9884(4) 0.8657(3) 0.061(2) Uiso 0.243(7) 1 d P C 4 Cl21 Cl 0.6990(6) 1.1544(4) 0.8114(3) 0.065(2) Uiso 0.243(7) 1 d P C 4 C10U C 0.6824(16) 1.1039(13) 0.8768(9) 0.032(4) Uiso 0.180(7) 1 d P D 5 Cl30 Cl 0.6146(9) 0.9858(6) 0.8478(5) 0.076(3) Uiso 0.180(7) 1 d P D 5 Cl31 Cl 0.6563(9) 1.1618(6) 0.8145(4) 0.069(3) Uiso 0.180(7) 1 d P D 5 H1S H -0.065(2) 0.888(2) 1.5352(15) 0.015(8) Uiso 1 1 d . . . H2S H -0.071(3) 1.396(3) 0.9444(19) 0.033(13) Uiso 1 1 d . . . Cl40 Cl 0.4335(4) 0.8297(4) 0.7764(3) 0.182(2) Uiso 0.607(6) 1 d P . . C50S C 0.3778(17) 0.7599(15) 0.8089(10) 0.085(6) Uiso 0.421(5) 1 d P E 6 Cl50 Cl 0.2925(4) 0.6900(3) 0.8261(2) 0.1003(17) Uiso 0.421(5) 1 d P E 6 C60S C 0.4400(9) 0.7610(10) 0.7531(6) 0.081(3) Uiso 0.579(5) 1 d P E 7 Cl60 Cl 0.4444(10) 0.6851(9) 0.7072(6) 0.024(6) Uiso 0.065(6) 1 d P E 7 Cl71 Cl 0.3623(10) 0.6626(8) 0.7559(6) 0.225(5) Uiso 0.393(6) 1 d P F 8 Cl70 Cl 0.4674(16) 0.6910(13) 0.6884(10) 0.371(12) Uiso 0.393(6) 1 d P F 8 C80S C 0.409(2) 0.6717(18) 0.7357(12) 0.047(5) Uiso 0.20 1 d P E 9 Cl81 Cl 0.373(2) 0.7339(15) 0.8161(11) 0.169(9) Uiso 0.20 1 d P E 9 Cl80 Cl 0.4369(12) 0.7096(14) 0.7327(9) 0.125(4) Uiso 0.20 1 d P E 9 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 0.0210(2) 0.0229(2) 0.0241(2) 0.00362(17) 0.00391(17) 0.00619(17) Fe2 0.0235(2) 0.0222(2) 0.0271(2) 0.00485(17) 0.00889(18) 0.00565(17) O1C 0.0278(12) 0.0274(11) 0.0315(12) 0.0082(9) 0.0096(9) 0.0096(9) O1 0.0258(11) 0.0252(11) 0.0332(12) 0.0054(9) 0.0045(9) 0.0042(9) O1B 0.0243(11) 0.0257(11) 0.0266(11) 0.0037(9) 0.0051(9) 0.0088(9) O1D 0.0281(12) 0.0263(11) 0.0365(12) 0.0039(9) 0.0114(10) 0.0031(9) O2B 0.0229(11) 0.0264(11) 0.0298(11) 0.0017(9) 0.0050(9) 0.0083(9) O2C 0.0279(12) 0.0266(11) 0.0345(12) 0.0097(9) 0.0112(9) 0.0103(9) O2 0.0458(15) 0.0321(13) 0.0360(14) 0.0083(10) -0.0001(11) 0.0008(11) O2D 0.0609(18) 0.0382(14) 0.0512(16) -0.0073(12) 0.0306(14) -0.0096(13) O20 0.0282(13) 0.0242(13) 0.0334(13) 0.0023(10) 0.0105(10) 0.0022(10) O10 0.0263(12) 0.0257(12) 0.0298(12) 0.0044(10) 0.0060(9) 0.0058(10) N1 0.0274(14) 0.0317(14) 0.0264(13) 0.0067(11) 0.0048(11) 0.0043(11) N2 0.0267(14) 0.0291(14) 0.0323(14) 0.0008(11) 0.0084(11) 0.0046(11) C1A 0.055(3) 0.050(2) 0.051(2) -0.0008(19) 0.005(2) 0.023(2) C1P 0.034(2) 0.070(3) 0.042(2) 0.0192(19) 0.0074(16) 0.0169(19) C1D 0.061(3) 0.058(3) 0.055(3) 0.017(2) 0.015(2) 0.016(2) C1Q 0.053(3) 0.072(3) 0.033(2) 0.0004(19) 0.0072(17) 0.032(2) C1B 0.077(3) 0.071(3) 0.063(3) 0.028(2) 0.037(3) 0.018(3) C1C 0.096(4) 0.088(4) 0.060(3) -0.018(3) -0.008(3) 0.017(3) C2D 0.055(2) 0.043(2) 0.038(2) 0.0151(17) 0.0153(18) 0.0104(18) C2B 0.053(2) 0.042(2) 0.048(2) 0.0199(17) 0.0222(19) 0.0129(18) C2A 0.055(2) 0.0377(19) 0.0302(18) -0.0024(15) 0.0089(16) 0.0180(18) C2Q 0.080(3) 0.102(4) 0.030(2) 0.005(2) 0.007(2) 0.052(3) C2C 0.063(3) 0.044(2) 0.053(3) -0.0120(19) -0.003(2) 0.014(2) C2P 0.055(3) 0.089(4) 0.044(2) 0.024(2) -0.003(2) 0.024(3) C3D 0.064(3) 0.0320(19) 0.045(2) 0.0000(17) 0.010(2) 0.0074(19) C3Q 0.058(3) 0.067(3) 0.031(2) -0.0072(19) 0.0140(18) 0.017(2) C3B 0.052(3) 0.069(3) 0.041(2) 0.026(2) 0.0086(19) 0.012(2) C3A 0.062(3) 0.0299(18) 0.044(2) 0.0057(16) 0.0163(19) 0.0165(18) C3P 0.069(3) 0.076(3) 0.031(2) 0.024(2) 0.005(2) 0.014(2) C3C 0.068(3) 0.053(2) 0.047(2) -0.005(2) 0.018(2) 0.020(2) C4B 0.035(2) 0.057(2) 0.048(2) 0.0223(19) 0.0060(17) 0.0125(18) C4Q 0.054(3) 0.062(3) 0.049(2) -0.002(2) 0.023(2) 0.026(2) C4A 0.054(2) 0.0292(18) 0.046(2) 0.0042(16) 0.0167(18) 0.0040(17) C4D 0.053(2) 0.035(2) 0.044(2) 0.0022(16) 0.0024(18) 0.0007(18) C4C 0.043(2) 0.045(2) 0.049(2) 0.0025(17) 0.0125(18) 0.0201(18) C4P 0.056(3) 0.087(3) 0.040(2) 0.021(2) 0.021(2) 0.017(2) C5B 0.0325(18) 0.0235(15) 0.0420(19) 0.0107(14) 0.0104(15) 0.0093(13) C5D 0.047(2) 0.0302(17) 0.0346(19) 0.0095(14) 0.0113(16) -0.0004(16) C5A 0.047(2) 0.0242(16) 0.0363(18) -0.0014(14) 0.0120(16) 0.0076(15) C5C 0.042(2) 0.0234(16) 0.045(2) 0.0012(14) 0.0114(16) 0.0120(15) C5Q 0.051(2) 0.057(2) 0.037(2) 0.0079(18) 0.0136(17) 0.027(2) C5P 0.038(2) 0.058(2) 0.0341(19) 0.0097(17) 0.0095(16) 0.0103(18) C6B 0.0328(18) 0.0293(17) 0.0410(19) 0.0077(14) 0.0082(15) 0.0095(14) C6A 0.048(2) 0.0265(16) 0.0329(18) 0.0000(14) 0.0101(15) 0.0089(15) C6C 0.037(2) 0.0324(18) 0.056(2) -0.0015(17) 0.0064(17) 0.0094(16) C6D 0.052(2) 0.0286(18) 0.044(2) 0.0080(16) 0.0093(18) 0.0022(17) C7B 0.0334(19) 0.0335(18) 0.057(2) 0.0163(17) 0.0173(17) 0.0090(15) C7D 0.051(2) 0.0339(19) 0.042(2) 0.0105(16) 0.0052(18) -0.0028(17) C7A 0.043(2) 0.0346(18) 0.0368(19) -0.0047(15) 0.0120(16) 0.0065(16) C7C 0.043(2) 0.040(2) 0.065(3) -0.006(2) -0.006(2) 0.0089(18) C8B 0.0266(16) 0.0245(15) 0.0364(18) 0.0038(13) 0.0045(13) 0.0063(13) C8C 0.0285(17) 0.0299(16) 0.0422(19) 0.0097(14) 0.0140(14) 0.0116(14) C8D 0.040(2) 0.0327(18) 0.042(2) 0.0038(15) 0.0112(16) -0.0038(15) C8A 0.040(2) 0.0294(17) 0.042(2) -0.0034(15) 0.0064(16) 0.0022(15) C9B 0.0311(18) 0.0284(17) 0.048(2) 0.0081(15) 0.0043(15) 0.0124(14) C9C 0.040(2) 0.0353(19) 0.055(2) 0.0083(17) 0.0165(18) 0.0198(16) C9A 0.049(3) 0.039(2) 0.075(3) -0.016(2) -0.003(2) 0.0032(19) C9D 0.060(3) 0.039(2) 0.071(3) 0.018(2) 0.022(2) -0.005(2) C10B 0.0307(18) 0.0343(18) 0.052(2) -0.0016(16) 0.0099(16) 0.0155(15) C10C 0.046(2) 0.046(2) 0.054(2) 0.0184(19) 0.0103(18) 0.0268(19) C10D 0.045(3) 0.064(3) 0.098(4) 0.020(3) 0.030(3) -0.006(2) C10A 0.049(3) 0.049(3) 0.094(4) -0.027(3) -0.010(3) -0.002(2) C11B 0.0270(17) 0.0317(17) 0.0384(18) -0.0023(14) 0.0089(14) 0.0088(14) C11C 0.0354(19) 0.045(2) 0.0375(19) 0.0176(16) 0.0075(15) 0.0162(16) C11A 0.036(2) 0.056(3) 0.081(3) -0.016(2) -0.011(2) 0.008(2) C12B 0.0225(15) 0.0238(15) 0.0310(16) -0.0008(12) 0.0037(12) 0.0031(12) C12A 0.0306(19) 0.039(2) 0.048(2) -0.0022(16) 0.0017(16) 0.0034(15) C12C 0.0281(17) 0.0324(17) 0.0351(17) 0.0119(14) 0.0112(14) 0.0079(14) C12D 0.035(2) 0.043(2) 0.058(2) 0.0046(18) 0.0185(18) 0.0014(17) C13B 0.0195(14) 0.0238(15) 0.0296(16) -0.0001(12) 0.0029(12) 0.0073(12) C13A 0.0301(18) 0.0320(17) 0.0358(18) 0.0012(14) 0.0058(14) 0.0002(14) C13C 0.0257(16) 0.0272(16) 0.0365(17) 0.0090(13) 0.0120(13) 0.0090(13) C13D 0.0365(19) 0.0300(17) 0.0397(19) 0.0024(14) 0.0142(15) -0.0015(15) C14B 0.0255(15) 0.0196(14) 0.0284(16) 0.0082(12) 0.0083(12) 0.0067(12) C14D 0.0309(18) 0.0286(17) 0.0373(18) 0.0058(14) 0.0100(14) 0.0026(14) C15B 0.0222(15) 0.0318(16) 0.0316(17) 0.0039(13) 0.0068(13) 0.0057(13) C15C 0.0251(16) 0.0378(18) 0.0328(17) 0.0073(14) 0.0059(13) 0.0077(14) C15A 0.0240(17) 0.042(2) 0.046(2) -0.0014(16) 0.0027(15) 0.0054(15) C15D 0.0296(19) 0.048(2) 0.069(3) 0.009(2) 0.0157(19) 0.0093(17) C16B 0.040(2) 0.044(2) 0.0322(18) 0.0027(15) 0.0110(15) 0.0121(16) C16A 0.036(2) 0.055(2) 0.042(2) -0.0017(18) 0.0015(16) 0.0139(18) C16C 0.038(2) 0.051(2) 0.0359(19) 0.0112(17) 0.0084(16) 0.0107(17) C16D 0.051(3) 0.066(3) 0.080(4) 0.010(3) 0.006(2) 0.010(2) C17D 0.054(3) 0.092(4) 0.092(4) 0.038(3) 0.011(3) 0.022(3) C17B 0.045(2) 0.059(2) 0.0294(18) 0.0085(17) 0.0114(16) 0.0111(19) C17A 0.037(2) 0.058(2) 0.048(2) 0.0132(19) 0.0052(17) 0.0180(19) C17C 0.049(2) 0.068(3) 0.035(2) -0.0015(19) 0.0101(18) 0.009(2) C18A 0.0253(18) 0.042(2) 0.056(2) 0.0001(17) 0.0054(16) 0.0092(15) C18B 0.038(2) 0.049(2) 0.048(2) 0.0214(18) 0.0139(17) 0.0099(17) C18C 0.047(2) 0.054(3) 0.050(2) -0.015(2) 0.0054(19) 0.010(2) C18D 0.042(3) 0.082(4) 0.106(4) 0.041(3) 0.032(3) 0.026(3) C19B 0.0327(18) 0.0323(18) 0.043(2) 0.0112(15) 0.0101(15) 0.0083(15) C19A 0.0310(19) 0.048(2) 0.046(2) -0.0034(17) 0.0029(16) 0.0103(17) C19C 0.053(2) 0.039(2) 0.047(2) -0.0027(17) 0.0025(19) 0.0116(18) C19D 0.042(3) 0.052(3) 0.123(5) 0.022(3) 0.031(3) 0.016(2) C20B 0.0254(16) 0.0328(17) 0.0340(17) 0.0046(14) 0.0084(13) 0.0076(13) C20C 0.040(2) 0.0374(19) 0.0338(18) 0.0035(15) 0.0027(15) 0.0098(16) C20A 0.0295(18) 0.047(2) 0.043(2) 0.0027(17) 0.0007(15) 0.0115(16) C20D 0.038(2) 0.055(3) 0.084(3) 0.009(2) 0.019(2) 0.014(2) C21A 0.041(2) 0.048(2) 0.072(3) 0.003(2) 0.005(2) 0.0137(19) C21B 0.085(4) 0.068(3) 0.065(3) 0.041(3) 0.029(3) 0.028(3) C21C 0.095(4) 0.079(4) 0.067(3) -0.032(3) 0.012(3) 0.023(3) C21D 0.059(3) 0.104(5) 0.161(7) 0.075(5) 0.043(4) 0.036(3) C14A 0.0271(16) 0.0272(16) 0.0339(18) 0.0023(13) 0.0055(13) 0.0080(13) C14C 0.0247(15) 0.0227(15) 0.0285(16) 0.0026(12) 0.0068(12) 0.0056(12) C11D 0.040(2) 0.058(3) 0.089(4) 0.016(3) 0.026(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.969(2) . ? Fe1 O10 1.986(2) 2_578 ? Fe1 O10 2.012(2) . ? Fe1 O1B 2.040(2) . ? Fe1 O2B 2.076(2) 2_578 ? Fe1 N1 2.149(3) . ? Fe1 Fe1 2.8843(9) 2_578 ? Fe2 O1D 1.964(2) . ? Fe2 O20 1.969(3) 2_587 ? Fe2 O20 1.976(2) . ? Fe2 O1C 2.060(2) . ? Fe2 O2C 2.096(2) . ? Fe2 N2 2.144(3) . ? Fe2 Fe2 2.8472(8) 2_587 ? O1C C14C 1.277(4) 2_587 ? O1 C14A 1.291(4) . ? O1B C14B 1.271(4) . ? O1D C14D 1.286(4) . ? O2B C14B 1.270(4) . ? O2B Fe1 2.076(2) 2_578 ? O2C C14C 1.263(4) . ? O2 C14A 1.231(4) . ? O2 O10 2.888(3) 2_578 ? O2D C14D 1.233(4) . ? O2D O20 5.022(4) 2_587 ? O20 Fe2 1.969(3) 2_587 ? O10 Fe1 1.986(2) 2_578 ? N1 C1P 1.336(5) . ? N1 C5P 1.337(4) . ? N2 C5Q 1.339(5) . ? N2 C1Q 1.339(5) . ? C1A C2A 1.513(5) . ? C1P C2P 1.385(5) . ? C1D C2D 1.502(6) . ? C1Q C2Q 1.381(5) . ? C1B C2B 1.521(6) . ? C1C C2C 1.523(7) . ? C2D C3D 1.393(6) . ? C2D C7D 1.406(5) . ? C2B C3B 1.388(6) . ? C2B C7B 1.386(6) . ? C2A C3A 1.388(6) . ? C2A C7A 1.403(5) . ? C2Q C3Q 1.364(6) . ? C2C C3C 1.400(6) . ? C2C C7C 1.390(7) . ? C2P C3P 1.370(7) . ? C3D C4D 1.381(6) . ? C3Q C4Q 1.371(6) . ? C3B C4B 1.387(6) . ? C3A C4A 1.383(6) . ? C3P C4P 1.380(6) . ? C3C C4C 1.375(6) . ? C4B C5B 1.396(5) . ? C4Q C5Q 1.382(5) . ? C4A C5A 1.408(5) . ? C4D C5D 1.411(5) . ? C4C C5C 1.407(5) . ? C4P C5P 1.383(5) . ? C5B C6B 1.390(5) . ? C5B C8B 1.501(5) . ? C5D C6D 1.392(5) . ? C5D C8D 1.503(6) . ? C5A C6A 1.394(5) . ? C5A C8A 1.495(5) . ? C5C C6C 1.399(5) . ? C5C C8C 1.492(5) . ? C6B C7B 1.403(5) . ? C6A C7A 1.382(5) . ? C6C C7C 1.394(6) . ? C6D C7D 1.386(6) . ? C8B C13B 1.397(4) . ? C8B C9B 1.407(5) . ? C8C C9C 1.405(5) . ? C8C C13C 1.409(5) . ? C8D C9D 1.404(5) . ? C8D C13D 1.406(5) . ? C8A C9A 1.399(5) . ? C8A C13A 1.408(5) . ? C9B C10B 1.384(5) . ? C9C C10C 1.377(6) . ? C9A C10A 1.388(7) . ? C9D C10D 1.392(7) . ? C10B C11B 1.390(5) . ? C10C C11C 1.380(5) . ? C10D C11D 1.374(7) . ? C10A C11A 1.386(6) . ? C11B C12B 1.400(4) . ? C11C C12C 1.402(5) . ? C11A C12A 1.399(5) . ? C12B C13B 1.412(4) . ? C12B C15B 1.494(4) . ? C12A C13A 1.408(5) . ? C12A C15A 1.503(5) . ? C12C C13C 1.412(5) . ? C12C C15C 1.491(5) . ? C12D C11D 1.402(5) . ? C12D C13D 1.412(5) . ? C12D C15D 1.488(6) . ? C13B C14B 1.514(4) . ? C13A C14A 1.525(5) . ? C13C C14C 1.513(4) . ? C13D C14D 1.523(5) . ? C15B C20B 1.400(5) . ? C15B C16B 1.405(5) . ? C15C C20C 1.390(5) . ? C15C C16C 1.398(5) . ? C15A C16A 1.391(5) . ? C15A C20A 1.399(5) . ? C15D C20D 1.401(6) . ? C15D C16D 1.405(7) . ? C16B C17B 1.372(5) . ? C16A C17A 1.391(6) . ? C16C C17C 1.389(6) . ? C16D C17D 1.398(7) . ? C17D C18D 1.391(8) . ? C17B C18B 1.397(6) . ? C17A C18A 1.393(6) . ? C17C C18C 1.396(6) . ? C18A C19A 1.389(5) . ? C18A C21A 1.511(5) . ? C18B C19B 1.389(5) . ? C18B C21B 1.517(5) . ? C18C C19C 1.385(6) . ? C18C C21C 1.517(6) . ? C18D C19D 1.383(8) . ? C18D C21D 1.508(7) . ? C19B C20B 1.397(5) . ? C19A C20A 1.394(5) . ? C19C C20C 1.396(5) . ? C19D C20D 1.398(6) . ? C14C O1C 1.276(4) 2_587 ? C1S Cl1 1.590(11) . ? C1S Cl2B 1.687(19) . ? C1S Cl1A 1.729(8) . ? C1S Cl2 1.747(11) . ? C1S Cl1B 1.959(12) . ? C1S Cl2A 1.978(10) . ? Cl1 Cl2A 0.689(10) . ? Cl1 Cl2B 1.63(2) . ? Cl2 Cl1A 0.746(12) . ? Cl2 Cl1B 1.529(19) . ? Cl2 Cl2B 1.53(2) . ? Cl1A Cl1B 0.792(11) . ? Cl1A Cl2B 2.14(2) . ? Cl2A Cl2B 1.481(19) . ? C10S Cl11 1.759(15) . ? C10S Cl10 1.857(15) . ? C10T Cl20 2.05(3) . ? C10T Cl21 2.14(3) . ? C10U Cl31 1.70(2) . ? C10U Cl30 1.86(2) . ? Cl40 C60S 1.197(14) . ? Cl40 C50S 1.47(2) . ? Cl40 Cl80 2.08(2) . ? Cl40 Cl81 1.86(2) . ? Cl40 C80S 2.49(3) . ? C50S Cl50 1.52(2) . ? C60S Cl60 1.552(19) . ? Cl71 Cl70 2.29(3) . ? C80S Cl80 0.64(3) . ? C80S Cl81 2.20(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O10 98.07(10) . 2_578 ? O1 Fe1 O10 171.95(9) . . ? O10 Fe1 O10 87.66(10) 2_578 . ? O1 Fe1 O1B 101.08(9) . . ? O10 Fe1 O1B 82.74(9) 2_578 . ? O10 Fe1 O1B 85.19(9) . . ? O1 Fe1 O2B 93.98(9) . 2_578 ? O10 Fe1 O2B 86.92(9) 2_578 2_578 ? O10 Fe1 O2B 80.63(9) . 2_578 ? O1B Fe1 O2B 162.76(9) . 2_578 ? O1 Fe1 N1 83.28(10) . . ? O10 Fe1 N1 172.48(10) 2_578 . ? O10 Fe1 N1 91.78(10) . . ? O1B Fe1 N1 89.74(9) . . ? O2B Fe1 N1 100.39(9) 2_578 . ? O1 Fe1 Fe1 141.94(7) . 2_578 ? O10 Fe1 Fe1 44.19(7) 2_578 2_578 ? O10 Fe1 Fe1 43.48(6) . 2_578 ? O1B Fe1 Fe1 81.64(6) . 2_578 ? O2B Fe1 Fe1 81.34(6) 2_578 2_578 ? N1 Fe1 Fe1 134.78(8) . 2_578 ? O1D Fe2 O20 173.47(10) . 2_587 ? O1D Fe2 O20 94.79(10) . . ? O20 Fe2 O20 87.61(11) 2_587 . ? O1D Fe2 O1C 100.08(9) . . ? O20 Fe2 O1C 86.21(10) 2_587 . ? O20 Fe2 O1C 83.60(10) . . ? O1D Fe2 O2C 93.16(9) . . ? O20 Fe2 O2C 80.93(10) 2_587 . ? O20 Fe2 O2C 86.16(10) . . ? O1C Fe2 O2C 163.87(9) . . ? O1D Fe2 N2 85.21(10) . . ? O20 Fe2 N2 92.87(10) 2_587 . ? O20 Fe2 N2 175.50(11) . . ? O1C Fe2 N2 91.97(9) . . ? O2C Fe2 N2 98.33(10) . . ? O1D Fe2 Fe2 138.17(7) . 2_587 ? O20 Fe2 Fe2 43.90(7) 2_587 2_587 ? O20 Fe2 Fe2 43.72(7) . 2_587 ? O1C Fe2 Fe2 82.93(6) . 2_587 ? O2C Fe2 Fe2 81.06(6) . 2_587 ? N2 Fe2 Fe2 136.59(8) . 2_587 ? C14C O1C Fe2 124.14(19) 2_587 . ? C14A O1 Fe1 131.7(2) . . ? C14B O1B Fe1 125.45(19) . . ? C14D O1D Fe2 131.5(2) . . ? C14B O2B Fe1 124.11(19) . 2_578 ? C14C O2C Fe2 125.08(19) . . ? C14A O2 O10 97.5(2) . 2_578 ? C14D O2D O20 76.4(2) . 2_587 ? Fe2 O20 Fe2 92.38(11) 2_587 . ? Fe1 O10 Fe1 92.33(10) 2_578 . ? C1P N1 C5P 118.1(3) . . ? C1P N1 Fe1 119.4(2) . . ? C5P N1 Fe1 122.4(2) . . ? C5Q N2 C1Q 118.1(3) . . ? C5Q N2 Fe2 121.0(2) . . ? C1Q N2 Fe2 120.7(2) . . ? N1 C1P C2P 122.6(4) . . ? N2 C1Q C2Q 121.8(4) . . ? C3D C2D C7D 117.2(4) . . ? C3D C2D C1D 120.9(4) . . ? C7D C2D C1D 122.0(4) . . ? C3B C2B C7B 117.9(4) . . ? C3B C2B C1B 121.4(4) . . ? C7B C2B C1B 120.7(4) . . ? C3A C2A C7A 117.9(3) . . ? C3A C2A C1A 120.5(3) . . ? C7A C2A C1A 121.6(4) . . ? C3Q C2Q C1Q 120.2(4) . . ? C3C C2C C7C 117.2(4) . . ? C3C C2C C1C 121.4(5) . . ? C7C C2C C1C 121.4(5) . . ? C3P C2P C1P 119.2(4) . . ? C4D C3D C2D 121.6(4) . . ? C2Q C3Q C4Q 118.1(4) . . ? C2B C3B C4B 121.7(4) . . ? C4A C3A C2A 121.1(3) . . ? C2P C3P C4P 118.6(4) . . ? C4C C3C C2C 121.6(4) . . ? C3B C4B C5B 120.8(4) . . ? C3Q C4Q C5Q 119.6(4) . . ? C3A C4A C5A 121.5(4) . . ? C3D C4D C5D 121.3(4) . . ? C3C C4C C5C 121.1(4) . . ? C5P C4P C3P 119.2(4) . . ? C6B C5B C4B 117.7(3) . . ? C6B C5B C8B 121.8(3) . . ? C4B C5B C8B 120.5(3) . . ? C6D C5D C4D 117.1(4) . . ? C6D C5D C8D 124.0(3) . . ? C4D C5D C8D 118.9(3) . . ? C6A C5A C4A 117.0(3) . . ? C6A C5A C8A 121.9(3) . . ? C4A C5A C8A 120.9(3) . . ? C6C C5C C4C 117.7(4) . . ? C6C C5C C8C 122.3(3) . . ? C4C C5C C8C 120.0(3) . . ? N2 C5Q C4Q 122.2(4) . . ? N1 C5P C4P 122.4(4) . . ? C5B C6B C7B 121.1(3) . . ? C7A C6A C5A 121.7(3) . . ? C7C C6C C5C 120.3(4) . . ? C7D C6D C5D 121.5(4) . . ? C2B C7B C6B 120.8(4) . . ? C6D C7D C2D 121.3(4) . . ? C6A C7A C2A 120.9(4) . . ? C6C C7C C2C 122.0(4) . . ? C13B C8B C9B 118.7(3) . . ? C13B C8B C5B 121.1(3) . . ? C9B C8B C5B 120.2(3) . . ? C9C C8C C13C 118.0(3) . . ? C9C C8C C5C 119.4(3) . . ? C13C C8C C5C 122.5(3) . . ? C9D C8D C13D 118.7(4) . . ? C9D C8D C5D 118.0(3) . . ? C13D C8D C5D 123.3(3) . . ? C9A C8A C13A 118.9(4) . . ? C9A C8A C5A 117.7(3) . . ? C13A C8A C5A 123.3(3) . . ? C10B C9B C8B 120.3(3) . . ? C10C C9C C8C 121.5(3) . . ? C10A C9A C8A 121.1(4) . . ? C10D C9D C8D 120.6(4) . . ? C9B C10B C11B 120.4(3) . . ? C9C C10C C11C 119.8(3) . . ? C11D C10D C9D 120.5(4) . . ? C11A C10A C9A 119.5(4) . . ? C10B C11B C12B 121.2(3) . . ? C10C C11C C12C 121.5(4) . . ? C10A C11A C12A 121.2(4) . . ? C11B C12B C13B 117.7(3) . . ? C11B C12B C15B 119.5(3) . . ? C13B C12B C15B 122.7(3) . . ? C11A C12A C13A 118.8(4) . . ? C11A C12A C15A 118.1(3) . . ? C13A C12A C15A 123.0(3) . . ? C11C C12C C13C 118.1(3) . . ? C11C C12C C15C 119.5(3) . . ? C13C C12C C15C 122.4(3) . . ? C11D C12D C13D 118.7(4) . . ? C11D C12D C15D 117.4(4) . . ? C13D C12D C15D 123.9(3) . . ? C8B C13B C12B 121.7(3) . . ? C8B C13B C14B 118.5(3) . . ? C12B C13B C14B 119.7(3) . . ? C8A C13A C12A 120.3(3) . . ? C8A C13A C14A 119.5(3) . . ? C12A C13A C14A 120.2(3) . . ? C8C C13C C12C 121.1(3) . . ? C8C C13C C14C 119.4(3) . . ? C12C C13C C14C 119.6(3) . . ? C8D C13D C12D 120.7(3) . . ? C8D C13D C14D 120.1(3) . . ? C12D C13D C14D 119.2(3) . . ? O2B C14B O1B 127.3(3) . . ? O2B C14B C13B 117.3(3) . . ? O1B C14B C13B 115.5(3) . . ? O2D C14D O1D 126.2(3) . . ? O2D C14D C13D 119.3(3) . . ? O1D C14D C13D 114.5(3) . . ? C20B C15B C16B 117.0(3) . . ? C20B C15B C12B 122.1(3) . . ? C16B C15B C12B 120.9(3) . . ? C20C C15C C16C 117.9(3) . . ? C20C C15C C12C 121.4(3) . . ? C16C C15C C12C 120.7(3) . . ? C16A C15A C20A 118.2(4) . . ? C16A C15A C12A 119.2(3) . . ? C20A C15A C12A 122.5(3) . . ? C20D C15D C16D 117.4(4) . . ? C20D C15D C12D 123.4(4) . . ? C16D C15D C12D 119.1(4) . . ? C17B C16B C15B 121.4(3) . . ? C15A C16A C17A 121.3(4) . . ? C17C C16C C15C 121.4(4) . . ? C17D C16D C15D 121.5(5) . . ? C18D C17D C16D 120.5(5) . . ? C16B C17B C18B 121.9(3) . . ? C16A C17A C18A 120.8(4) . . ? C16C C17C C18C 120.3(4) . . ? C19A C18A C17A 117.7(4) . . ? C19A C18A C21A 121.5(4) . . ? C17A C18A C21A 120.7(4) . . ? C19B C18B C17B 117.3(3) . . ? C19B C18B C21B 121.1(4) . . ? C17B C18B C21B 121.6(4) . . ? C19C C18C C17C 118.4(4) . . ? C19C C18C C21C 121.1(4) . . ? C17C C18C C21C 120.5(4) . . ? C19D C18D C17D 118.4(5) . . ? C19D C18D C21D 121.3(6) . . ? C17D C18D C21D 120.3(6) . . ? C18B C19B C20B 121.3(3) . . ? C18A C19A C20A 122.0(4) . . ? C18C C19C C20C 121.3(4) . . ? C18D C19D C20D 121.8(5) . . ? C19B C20B C15B 121.1(3) . . ? C15C C20C C19C 120.6(4) . . ? C19A C20A C15A 119.9(4) . . ? C19D C20D C15D 120.5(5) . . ? O2 C14A O1 125.7(3) . . ? O2 C14A C13A 119.2(3) . . ? O1 C14A C13A 115.0(3) . . ? O2C C14C O1C 126.6(3) . 2_587 ? O2C C14C C13C 116.7(3) . . ? O1C C14C C13C 116.7(3) 2_587 . ? C10D C11D C12D 120.9(4) . . ? Cl1 C1S Cl2B 59.7(8) . . ? Cl1 C1S Cl1A 126.9(6) . . ? Cl2B C1S Cl1A 77.7(7) . . ? Cl1 C1S Cl2 105.1(6) . . ? Cl2B C1S Cl2 53.0(8) . . ? Cl1A C1S Cl2 24.8(4) . . ? Cl1 C1S Cl1B 141.8(7) . . ? Cl2B C1S Cl1B 101.3(8) . . ? Cl1A C1S Cl1B 23.7(3) . . ? Cl2 C1S Cl1B 48.3(6) . . ? Cl1 C1S Cl2A 18.5(4) . . ? Cl2B C1S Cl2A 46.8(7) . . ? Cl1A C1S Cl2A 108.4(4) . . ? Cl2 C1S Cl2A 87.1(5) . . ? Cl1B C1S Cl2A 124.8(5) . . ? Cl2A Cl1 C1S 114.6(13) . . ? Cl2A Cl1 Cl2B 65.1(11) . . ? C1S Cl1 Cl2B 63.1(8) . . ? Cl1A Cl2 Cl1B 6.2(7) . . ? Cl1A Cl2 Cl2B 137.5(14) . . ? Cl1B Cl2 Cl2B 134.6(10) . . ? Cl1A Cl2 C1S 76.2(9) . . ? Cl1B Cl2 C1S 73.1(7) . . ? Cl2B Cl2 C1S 61.5(8) . . ? Cl2 Cl1A Cl1B 167.9(13) . . ? Cl2 Cl1A C1S 79.0(9) . . ? Cl1B Cl1A C1S 94.7(9) . . ? Cl2 Cl1A Cl2B 28.9(9) . . ? Cl1B Cl1A Cl2B 144.5(10) . . ? C1S Cl1A Cl2B 50.3(5) . . ? Cl1 Cl2A Cl2B 89.9(13) . . ? Cl1 Cl2A C1S 46.9(10) . . ? Cl2B Cl2A C1S 56.2(8) . . ? Cl2A Cl2B Cl2 117.1(13) . . ? Cl2A Cl2B Cl1 25.0(5) . . ? Cl2 Cl2B Cl1 113.7(13) . . ? Cl2A Cl2B C1S 77.0(10) . . ? Cl2 Cl2B C1S 65.5(9) . . ? Cl1 Cl2B C1S 57.2(8) . . ? Cl2A Cl2B Cl1A 110.9(11) . . ? Cl2 Cl2B Cl1A 13.6(5) . . ? Cl1 Cl2B Cl1A 102.8(10) . . ? C1S Cl2B Cl1A 52.0(6) . . ? Cl1A Cl1B Cl2 5.8(6) . . ? Cl1A Cl1B C1S 61.6(8) . . ? Cl2 Cl1B C1S 58.6(5) . . ? Cl11 C10S Cl10 107.2(8) . . ? Cl20 C10T Cl21 85.8(10) . . ? Cl31 C10U Cl30 103.7(11) . . ? C60S Cl40 C50S 75.6(11) . . ? C60S Cl40 Cl80 3.2(8) . . ? C50S Cl40 Cl80 75.4(10) . . ? C60S Cl40 Cl81 70.2(10) . . ? C50S Cl40 Cl81 6.5(15) . . ? Cl80 Cl40 Cl81 70.1(9) . . ? C60S Cl40 C80S 13.6(9) . . ? C50S Cl40 C80S 63.6(11) . . ? Cl80 Cl40 C80S 12.2(8) . . ? Cl81 Cl40 C80S 58.6(10) . . ? Cl40 C50S Cl50 162.0(18) . . ? Cl40 C60S Cl60 164.7(11) . . ? Cl80 C80S Cl81 88(4) . . ? Cl80 C80S Cl40 44(3) . . ? Cl81 C80S Cl40 46.3(8) . . ? Cl40 Cl81 C80S 75.1(11) . . ? C80S Cl80 Cl40 124(4) . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 0.914 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.083