Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Junk, Peter C.' 'McCool, Brian J.' 'Moubaraki, Boujemaa' 'Murray, K. S.' 'Spiccia, Leone' 'Steed, Jonathan W.' _publ_contact_author_name 'Dr Peter C Junk' _publ_contact_author_address ; Department of Chemistry Monash University Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'PETER.JUNK@SCI.MONASH.EDU.AU' _publ_section_title ; Utilization of crown ethers to stabilize the dinuclear u-oxo bridged iron (III) aqua ion, [(H2O)5Fe(u-O)Fe(OH2)5]4+ ; data_c:\junkie\papers\feofe\feno\feno _database_code_CSD 174787 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H34 Fe N2 O17.50' _chemical_formula_weight 542.26 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.863(5) _cell_length_b 10.993(2) _cell_length_c 20.758(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.02(3) _cell_angle_gamma 90.00 _cell_volume 4870.0(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8072 _exptl_absorpt_correction_T_max 0.8501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4383 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1647 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4268 _reflns_number_gt 2175 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^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 4268 _refine_ls_number_parameters 324 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1855 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O3A O 0.3549(3) 0.6353(5) 0.8040(3) 0.0827(19) Uani 1 1 d . . . O2A O 0.3158(2) 0.6494(5) 0.6940(2) 0.0652(15) Uani 1 1 d . . . O1A O 0.3970(3) 0.7478(6) 0.7519(3) 0.122(3) Uani 1 1 d . . . O2B O 0.5924(3) 0.3390(6) 0.5754(3) 0.095(2) Uani 1 1 d . . . N1A N 0.3539(3) 0.6774(5) 0.7497(3) 0.0407(14) Uani 1 1 d . . . C11C C 0.2791(3) -0.0999(6) 0.4708(3) 0.0479(19) Uani 1 1 d . . . H11A H 0.2423 -0.1492 0.4480 0.057 Uiso 1 1 calc R . . H11B H 0.3149 -0.1420 0.4668 0.057 Uiso 1 1 calc R . . C2C C 0.3788(4) 0.2804(7) 0.4661(3) 0.057(2) Uani 1 1 d . . . H2C1 H 0.4167 0.2327 0.4759 0.068 Uiso 1 1 calc R . . H2C2 H 0.3808 0.3487 0.4373 0.068 Uiso 1 1 calc R . . C1C C 0.3230(3) 0.2040(6) 0.4290(3) 0.0522(19) Uani 1 1 d . . . H1C1 H 0.2851 0.2473 0.4258 0.063 Uiso 1 1 calc R . . H1C2 H 0.3214 0.1875 0.3825 0.063 Uiso 1 1 calc R . . N1B N 0.5660(3) 0.2718(6) 0.5276(3) 0.0480(15) Uani 1 1 d . . . O3B O 0.5543(3) 0.3042(5) 0.4672(3) 0.089(2) Uani 1 1 d . . . C12C C 0.2716(3) 0.0204(6) 0.4337(3) 0.0514(19) Uani 1 1 d . . . H12A H 0.2652 0.0067 0.3855 0.062 Uiso 1 1 calc R . . H12B H 0.2352 0.0628 0.4361 0.062 Uiso 1 1 calc R . . O1B O 0.5473(3) 0.1689(4) 0.5376(2) 0.0649(16) Uani 1 1 d . . . O1C O 0.3263(2) 0.0921(4) 0.4651(2) 0.0436(12) Uani 1 1 d . . . C8C C 0.2995(4) 0.0425(7) 0.7368(4) 0.057(2) Uani 1 1 d . . . H8C1 H 0.3367 -0.0045 0.7615 0.069 Uiso 1 1 calc R . . H8C2 H 0.2643 0.0069 0.7457 0.069 Uiso 1 1 calc R . . C4C C 0.4174(3) 0.4490(6) 0.6266(4) 0.0497(19) Uani 1 1 d . . . H4C1 H 0.4492 0.5099 0.6479 0.060 Uiso 1 1 calc R . . H4C2 H 0.3766 0.4878 0.6133 0.060 Uiso 1 1 calc R . . C6C C 0.3641(3) 0.3480(6) 0.7513(4) 0.0479(19) Uani 1 1 d . . . H6C1 H 0.3643 0.3781 0.7953 0.057 Uiso 1 1 calc R . . H6C2 H 0.3269 0.3790 0.7153 0.057 Uiso 1 1 calc R . . C5C C 0.4203(3) 0.3898(6) 0.7397(4) 0.0513(19) Uani 1 1 d . . . H5C1 H 0.4226 0.4778 0.7432 0.062 Uiso 1 1 calc R . . H5C2 H 0.4570 0.3570 0.7756 0.062 Uiso 1 1 calc R . . C3C C 0.4265(3) 0.3983(6) 0.5645(3) 0.0488(19) Uani 1 1 d . . . H3C1 H 0.4300 0.4639 0.5348 0.059 Uiso 1 1 calc R . . H3C2 H 0.4648 0.3510 0.5782 0.059 Uiso 1 1 calc R . . C9C C 0.2454(3) -0.0525(6) 0.6296(4) 0.0502(19) Uani 1 1 d . . . H9C1 H 0.2061 -0.0410 0.6367 0.060 Uiso 1 1 calc R . . H9C2 H 0.2622 -0.1313 0.6483 0.060 Uiso 1 1 calc R . . C7C C 0.3084(3) 0.1716(7) 0.7611(3) 0.0513(19) Uani 1 1 d . . . H7C1 H 0.2719 0.2196 0.7351 0.062 Uiso 1 1 calc R . . H7C2 H 0.3137 0.1755 0.8095 0.062 Uiso 1 1 calc R . . C10C C 0.2343(3) -0.0492(6) 0.5552(3) 0.0460(18) Uani 1 1 d . . . H10A H 0.1987 -0.1005 0.5307 0.055 Uiso 1 1 calc R . . H10B H 0.2243 0.0333 0.5383 0.055 Uiso 1 1 calc R . . O3C O 0.4215(2) 0.3544(4) 0.6740(2) 0.0500(13) Uani 1 1 d . . . O5C O 0.2880(2) 0.0398(4) 0.6646(2) 0.0539(13) Uani 1 1 d . . . O1W O 0.5211(2) -0.1558(4) 0.6362(2) 0.0422(12) Uani 1 1 d D . . O2C O 0.3745(2) 0.3234(4) 0.5285(2) 0.0459(12) Uani 1 1 d . . . O1Y O 0.5302(2) 0.1150(4) 0.6554(2) 0.0389(11) Uani 1 1 d D . . O6C O 0.28753(19) -0.0901(4) 0.5420(2) 0.0391(11) Uani 1 1 d . . . O1X O 0.39917(19) -0.1445(4) 0.6414(2) 0.0389(11) Uani 1 1 d D . . O1 O 0.5000 -0.0339(5) 0.7500 0.0346(14) Uani 1 2 d S . . O1V O 0.4009(2) 0.1091(4) 0.6448(2) 0.0372(11) Uani 1 1 d D . . O1Z O 0.43845(18) -0.0013(4) 0.54996(18) 0.0338(10) Uani 1 1 d D . . O4C O 0.36298(19) 0.2188(4) 0.7510(2) 0.0388(11) Uani 1 1 d . . . Fe1 Fe 0.46932(4) -0.02003(7) 0.65844(4) 0.0268(2) Uani 1 1 d . . . H1ZB H 0.3975(16) 0.037(5) 0.523(3) 0.080 Uiso 1 1 d D . . H1ZA H 0.449(3) -0.061(5) 0.520(2) 0.080 Uiso 1 1 d D . . H1XB H 0.3580(13) -0.130(6) 0.604(2) 0.080 Uiso 1 1 d D . . H1YA H 0.537(3) 0.128(6) 0.6108(13) 0.080 Uiso 1 1 d D . . H1YB H 0.5675(18) 0.148(6) 0.6934(18) 0.080 Uiso 1 1 d D . . H1VA H 0.3608(17) 0.095(5) 0.652(3) 0.080 Uiso 1 1 d D . . H1WA H 0.543(2) -0.221(4) 0.670(3) 0.080 Uiso 1 1 d D . . H1WB H 0.551(2) -0.122(5) 0.616(3) 0.080 Uiso 1 1 d D . . H1XA H 0.392(2) -0.188(6) 0.680(2) 0.080 Uiso 1 1 d D . . H1VB H 0.406(3) 0.1980(15) 0.639(3) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O3A 0.110(5) 0.094(5) 0.050(3) 0.005(3) 0.036(3) -0.030(4) O2A 0.056(3) 0.072(4) 0.052(3) -0.019(3) 0.001(3) -0.022(3) O1A 0.128(6) 0.158(6) 0.041(3) 0.027(4) -0.016(3) -0.114(5) O2B 0.116(5) 0.100(5) 0.060(4) -0.035(4) 0.020(4) -0.057(4) N1A 0.039(4) 0.032(3) 0.046(4) -0.002(3) 0.009(3) -0.005(3) C11C 0.050(5) 0.044(4) 0.038(4) -0.011(3) 0.002(3) -0.010(4) C2C 0.075(6) 0.044(5) 0.046(4) 0.013(4) 0.016(4) -0.003(4) C1C 0.067(5) 0.042(4) 0.039(4) 0.015(3) 0.007(4) -0.003(4) N1B 0.057(4) 0.048(4) 0.044(4) -0.011(3) 0.023(3) -0.011(3) O3B 0.167(6) 0.050(3) 0.050(4) -0.003(3) 0.040(4) -0.036(4) C12C 0.049(4) 0.053(4) 0.035(4) 0.002(4) -0.005(3) 0.001(4) O1B 0.117(5) 0.041(3) 0.052(3) -0.006(3) 0.050(3) -0.010(3) O1C 0.045(3) 0.038(3) 0.033(2) 0.006(2) -0.004(2) -0.002(2) C8C 0.061(5) 0.060(5) 0.057(5) 0.003(4) 0.028(4) -0.012(4) C4C 0.050(5) 0.027(4) 0.062(5) 0.000(3) 0.008(4) -0.004(3) C6C 0.052(5) 0.049(5) 0.043(4) -0.006(4) 0.017(4) 0.009(4) C5C 0.050(5) 0.038(4) 0.067(5) -0.012(4) 0.022(4) -0.004(4) C3C 0.062(5) 0.038(4) 0.047(4) 0.009(3) 0.019(4) -0.010(4) C9C 0.037(4) 0.044(5) 0.068(5) -0.006(4) 0.016(4) -0.010(3) C7C 0.042(4) 0.074(6) 0.046(4) -0.006(4) 0.026(4) 0.000(4) C10C 0.038(4) 0.048(5) 0.044(4) 0.000(3) 0.005(3) 0.004(3) O3C 0.078(4) 0.032(3) 0.052(3) -0.007(2) 0.038(3) -0.001(2) O5C 0.063(3) 0.057(3) 0.050(3) -0.011(3) 0.031(3) -0.019(3) O1W 0.042(3) 0.046(3) 0.037(3) 0.004(2) 0.013(2) 0.015(2) O2C 0.048(3) 0.040(3) 0.047(3) -0.002(2) 0.015(2) -0.006(2) O1Y 0.041(3) 0.045(3) 0.028(2) -0.002(2) 0.010(2) -0.014(2) O6C 0.031(2) 0.043(3) 0.037(2) 0.003(2) 0.004(2) 0.002(2) O1X 0.037(3) 0.038(3) 0.033(3) 0.005(2) 0.002(2) -0.010(2) O1 0.045(4) 0.033(3) 0.023(3) 0.000 0.009(3) 0.000 O1V 0.036(3) 0.028(2) 0.051(3) 0.003(2) 0.021(2) 0.005(2) O1Z 0.034(2) 0.036(3) 0.025(2) 0.0086(19) 0.0042(17) 0.008(2) O4C 0.032(3) 0.042(3) 0.043(3) -0.001(2) 0.014(2) 0.007(2) Fe1 0.0290(4) 0.0277(4) 0.0218(4) 0.0001(4) 0.0069(3) 0.0005(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 O3A N1A 1.211(7) . ? O2A N1A 1.213(6) . ? O1A N1A 1.240(7) . ? O2B N1B 1.210(7) . ? C11C O6C 1.423(7) . ? C11C C12C 1.508(9) . ? C2C O2C 1.416(7) . ? C2C C1C 1.492(9) . ? C1C O1C 1.428(7) . ? N1B O3B 1.238(7) . ? N1B O1B 1.254(7) . ? C12C O1C 1.424(7) . ? C8C O5C 1.426(8) . ? C8C C7C 1.496(9) . ? C4C O3C 1.412(7) . ? C4C C3C 1.486(9) . ? C6C O4C 1.420(7) . ? C6C C5C 1.466(9) . ? C5C O3C 1.428(7) . ? C3C O2C 1.419(7) . ? C9C O5C 1.413(7) . ? C9C C10C 1.473(9) . ? C7C O4C 1.435(7) . ? C10C O6C 1.414(7) . ? O1W Fe1 2.057(4) . ? O1Y Fe1 2.051(4) . ? O1X Fe1 2.040(4) . ? O1 Fe1 1.7809(11) . ? O1 Fe1 1.7808(11) 2_656 ? O1V Fe1 2.055(4) . ? O1Z Fe1 2.114(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 O3A N1A O2A 123.8(6) . . ? O3A N1A O1A 117.1(6) . . ? O2A N1A O1A 119.0(6) . . ? O6C C11C C12C 114.3(5) . . ? O2C C2C C1C 109.4(6) . . ? O1C C1C C2C 109.9(5) . . ? O2B N1B O3B 121.2(7) . . ? O2B N1B O1B 121.0(6) . . ? O3B N1B O1B 117.8(6) . . ? O1C C12C C11C 109.3(5) . . ? C12C O1C C1C 111.4(5) . . ? O5C C8C C7C 109.0(6) . . ? O3C C4C C3C 109.5(5) . . ? O4C C6C C5C 109.1(6) . . ? O3C C5C C6C 112.9(6) . . ? O2C C3C C4C 108.8(6) . . ? O5C C9C C10C 110.5(6) . . ? O4C C7C C8C 108.3(6) . . ? O6C C10C C9C 111.1(5) . . ? C4C O3C C5C 116.5(5) . . ? C9C O5C C8C 112.8(5) . . ? C2C O2C C3C 110.8(5) . . ? C10C O6C C11C 114.8(5) . . ? Fe1 O1 Fe1 170.2(4) . 2_656 ? C6C O4C C7C 112.0(5) . . ? O1 Fe1 O1X 96.41(17) . . ? O1 Fe1 O1Y 94.77(18) . . ? O1X Fe1 O1Y 168.48(16) . . ? O1 Fe1 O1V 101.26(18) . . ? O1X Fe1 O1V 85.85(17) . . ? O1Y Fe1 O1V 89.22(17) . . ? O1 Fe1 O1W 98.03(18) . . ? O1X Fe1 O1W 87.38(18) . . ? O1Y Fe1 O1W 93.85(18) . . ? O1V Fe1 O1W 160.15(17) . . ? O1 Fe1 O1Z 176.54(13) . . ? O1X Fe1 O1Z 86.54(16) . . ? O1Y Fe1 O1Z 82.39(16) . . ? O1V Fe1 O1Z 80.74(17) . . ? O1W Fe1 O1Z 80.24(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1Z H1ZB O1C 0.996(10) 1.749(15) 2.737(6) 171(5) . O1Z H1ZA O1B 0.998(10) 1.702(17) 2.689(6) 169(6) 5_656 O1X H1XB O6C 0.995(10) 1.720(13) 2.712(6) 174(7) . O1Y H1YA O1B 0.999(10) 1.682(16) 2.676(6) 172(6) . O1Y H1YB O4C 0.998(10) 1.777(16) 2.764(6) 170(5) 2_656 O1V H1VA O5C 0.998(10) 1.871(13) 2.860(6) 170(5) . O1W H1WA O1A 1.000(10) 1.75(4) 2.628(7) 145(6) 2_646 O1X H1XA O1A 0.994(10) 1.618(15) 2.598(7) 167(5) 1_545 O1V H1VB O3C 0.995(10) 1.85(3) 2.767(6) 152(6) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.430 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.096 data_pjfe18 _database_code_CSD 149181 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H72 Cl4 Fe2 O41' _chemical_formula_weight 1270.32 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2655(7) _cell_length_b 12.2247(6) _cell_length_c 12.2953(6) _cell_angle_alpha 71.820(2) _cell_angle_beta 72.129(2) _cell_angle_gamma 66.353(2) _cell_volume 1313.26(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min n/a _cell_measurement_theta_max n/a _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.7238 _exptl_absorpt_correction_T_max 0.9186 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10996 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4784 _reflns_number_gt 4308 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+1.0465P] 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 SHELXL _refine_ls_extinction_coef 0.015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4784 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.52777(3) 0.12025(3) 0.37966(3) 0.02117(12) Uani 1 1 d . . . Cl1 Cl 0.79511(6) 0.05917(5) 0.67344(5) 0.03181(15) Uani 1 1 d . . . Cl2 Cl 0.82336(6) -0.28668(5) 0.24791(5) 0.03068(15) Uani 1 1 d . . . O1 O 0.56430(15) 0.26230(13) 0.24037(12) 0.0229(3) Uani 1 1 d . . . H1B H 0.6243 0.2558 0.1711 0.027 Uiso 1 1 d R . . H1A H 0.5153 0.3426 0.2361 0.027 Uiso 1 1 d R . . O2 O 0.5000 0.0000 0.5000 0.0281(5) Uani 1 2 d S . . O3 O 0.47163(18) 0.25139(15) 0.47548(14) 0.0301(4) Uani 1 1 d . . . H3B H 0.5375 0.2953 0.4512 0.036 Uiso 1 1 d R . . H3A H 0.4588 0.2249 0.5552 0.036 Uiso 1 1 d R . . O4 O 0.59257(19) 0.03200(15) 0.24617(14) 0.0329(4) Uani 1 1 d . . . H4B H 0.5530 0.0617 0.1861 0.040 Uiso 1 1 d R . . H4A H 0.6047 -0.0411 0.2556 0.040 Uiso 1 1 d R . . O5 O 0.74385(17) 0.07692(15) 0.38026(14) 0.0310(4) Uani 1 1 d . . . H5B H 0.7779 0.1303 0.3385 0.037 Uiso 1 1 d R . . H5A H 0.7761 0.0469 0.4473 0.037 Uiso 1 1 d R . . O6 O 0.32333(17) 0.19511(16) 0.34712(14) 0.0327(4) Uani 1 1 d . . . H6B H 0.3009 0.2589 0.2890 0.039 Uiso 1 1 d R . . H6A H 0.2518 0.2017 0.3966 0.039 Uiso 1 1 d R . . O7 O 0.6656(3) 0.1500(3) 0.6444(3) 0.0921(10) Uani 1 1 d . . . O8 O 0.8890(4) 0.1178(4) 0.6737(2) 0.0979(12) Uani 1 1 d . . . O9 O 0.8571(2) -0.0146(2) 0.58680(19) 0.0598(6) Uani 1 1 d . . . O10 O 0.7626(3) -0.0102(2) 0.78671(19) 0.0713(7) Uani 1 1 d . . . O11 O 0.8512(2) -0.3506(2) 0.15898(17) 0.0485(5) Uani 1 1 d . . . O12 O 0.8653(2) -0.37336(18) 0.35165(18) 0.0488(5) Uani 1 1 d . . . O13 O 0.66800(18) -0.21927(16) 0.27525(17) 0.0393(4) Uani 1 1 d . . . O14 O 0.9024(2) -0.2036(2) 0.2090(2) 0.0567(6) Uani 1 1 d . . . O1A O 0.40042(18) 0.50290(15) 0.25427(14) 0.0319(4) Uani 1 1 d . . . O2A O 0.28459(18) 0.38616(15) 0.15170(15) 0.0323(4) Uani 1 1 d . . . O3A O 0.50012(18) 0.18146(15) 0.05371(14) 0.0307(4) Uani 1 1 d . . . O4A O 0.77288(17) 0.20581(15) 0.04412(14) 0.0305(4) Uani 1 1 d . . . O5A O 0.86593(18) 0.24644(16) 0.22592(14) 0.0320(4) Uani 1 1 d . . . O6A O 0.64160(18) 0.39095(15) 0.38345(15) 0.0319(4) Uani 1 1 d . . . C1A C 0.2482(3) 0.5305(3) 0.2621(3) 0.0420(6) Uani 1 1 d . . . H1A2 H 0.1938 0.6161 0.2704 0.050 Uiso 1 1 calc R . . H1A1 H 0.2101 0.4760 0.3319 0.050 Uiso 1 1 calc R . . C2A C 0.2280(3) 0.5130(2) 0.1542(3) 0.0408(6) Uani 1 1 d . . . H2A2 H 0.1232 0.5460 0.1526 0.049 Uiso 1 1 calc R . . H2A1 H 0.2786 0.5585 0.0841 0.049 Uiso 1 1 calc R . . C3A C 0.2852(3) 0.3674(2) 0.0429(2) 0.0362(6) Uani 1 1 d . . . H3A2 H 0.3422 0.4125 -0.0220 0.043 Uiso 1 1 calc R . . H3A1 H 0.1845 0.3990 0.0306 0.043 Uiso 1 1 calc R . . C4A C 0.3510(3) 0.2332(2) 0.0429(2) 0.0366(6) Uani 1 1 d . . . H4A2 H 0.2937 0.1892 0.1086 0.044 Uiso 1 1 calc R . . H4A1 H 0.3444 0.2208 -0.0307 0.044 Uiso 1 1 calc R . . C5A C 0.6004(3) 0.2089(3) -0.0517(2) 0.0380(6) Uani 1 1 d . . . H5A2 H 0.5796 0.2984 -0.0768 0.046 Uiso 1 1 calc R . . H5A1 H 0.5909 0.1802 -0.1148 0.046 Uiso 1 1 calc R . . C6A C 0.7514(3) 0.1461(3) -0.0292(2) 0.0389(6) Uani 1 1 d . . . H6A2 H 0.7656 0.0592 0.0097 0.047 Uiso 1 1 calc R . . H6A1 H 0.8232 0.1492 -0.1043 0.047 Uiso 1 1 calc R . . C7A C 0.9143(3) 0.1448(2) 0.0726(2) 0.0360(6) Uani 1 1 d . . . H7A2 H 0.9874 0.1196 0.0027 0.043 Uiso 1 1 calc R . . H7A1 H 0.9142 0.0704 0.1349 0.043 Uiso 1 1 calc R . . C8A C 0.9534(3) 0.2285(3) 0.1132(2) 0.0366(6) Uani 1 1 d . . . H8A2 H 1.0574 0.1930 0.1175 0.044 Uiso 1 1 calc R . . H8A1 H 0.9379 0.3083 0.0566 0.044 Uiso 1 1 calc R . . C9A C 0.8911(3) 0.3337(3) 0.2641(2) 0.0395(6) Uani 1 1 d . . . H9A2 H 0.8702 0.4130 0.2069 0.047 Uiso 1 1 calc R . . H9A1 H 0.9943 0.3051 0.2695 0.047 Uiso 1 1 calc R . . C10A C 0.7943(3) 0.3499(3) 0.3822(2) 0.0378(6) Uani 1 1 d . . . H10B H 0.8200 0.2710 0.4392 0.045 Uiso 1 1 calc R . . H10A H 0.8136 0.4099 0.4082 0.045 Uiso 1 1 calc R . . C11A C 0.5805(3) 0.5173(2) 0.3307(2) 0.0366(6) Uani 1 1 d . . . H11B H 0.6300 0.5335 0.2475 0.044 Uiso 1 1 calc R . . H11A H 0.5948 0.5689 0.3711 0.044 Uiso 1 1 calc R . . C12A C 0.4219(3) 0.5486(2) 0.3392(2) 0.0368(6) Uani 1 1 d . . . H12B H 0.3773 0.5123 0.4188 0.044 Uiso 1 1 calc R . . H12A H 0.3739 0.6385 0.3256 0.044 Uiso 1 1 calc R . . O1S O 0.0807(2) 0.2436(2) 0.50853(17) 0.0496(5) Uani 1 1 d . . . H1SA H 0.0409 0.1814 0.5498 0.059 Uiso 1 1 d R . . H1SB H 0.0858 0.2838 0.5578 0.059 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02547(18) 0.01956(18) 0.01816(18) 0.00088(13) -0.00555(12) -0.01025(12) Cl1 0.0368(3) 0.0360(3) 0.0258(3) -0.0031(3) -0.0077(2) -0.0173(2) Cl2 0.0301(3) 0.0301(3) 0.0321(3) -0.0069(3) -0.0054(2) -0.0112(2) O1 0.0250(7) 0.0197(7) 0.0205(7) -0.0012(6) -0.0030(6) -0.0077(6) O2 0.0357(12) 0.0256(11) 0.0240(11) 0.0021(10) -0.0083(9) -0.0153(9) O3 0.0402(9) 0.0300(9) 0.0218(8) -0.0042(7) -0.0008(6) -0.0188(7) O4 0.0508(10) 0.0229(8) 0.0255(9) -0.0019(7) -0.0140(7) -0.0108(7) O5 0.0302(8) 0.0321(9) 0.0288(9) 0.0034(8) -0.0096(6) -0.0137(7) O6 0.0285(8) 0.0381(9) 0.0273(8) 0.0055(8) -0.0078(6) -0.0150(7) O7 0.093(2) 0.0786(19) 0.097(2) -0.0316(17) -0.0668(18) 0.0225(16) O8 0.123(3) 0.170(3) 0.0637(16) -0.0339(19) 0.0030(16) -0.122(3) O9 0.0590(14) 0.0705(15) 0.0481(13) -0.0274(12) -0.0049(10) -0.0137(11) O10 0.125(2) 0.0552(14) 0.0319(12) 0.0092(12) -0.0137(12) -0.0452(15) O11 0.0444(11) 0.0582(13) 0.0462(11) -0.0272(10) -0.0144(9) -0.0051(9) O12 0.0564(13) 0.0433(11) 0.0420(11) -0.0008(10) -0.0215(9) -0.0104(9) O13 0.0304(9) 0.0284(9) 0.0515(11) -0.0092(9) -0.0024(8) -0.0063(7) O14 0.0502(12) 0.0573(13) 0.0704(15) -0.0085(12) -0.0036(10) -0.0365(10) O1A 0.0348(9) 0.0280(8) 0.0309(9) -0.0084(8) -0.0100(7) -0.0048(7) O2A 0.0344(9) 0.0302(9) 0.0301(9) 0.0010(8) -0.0145(7) -0.0085(7) O3A 0.0342(9) 0.0342(9) 0.0240(8) -0.0002(7) -0.0107(6) -0.0130(7) O4A 0.0281(8) 0.0330(9) 0.0276(8) -0.0088(7) -0.0050(6) -0.0064(6) O5A 0.0313(9) 0.0386(9) 0.0289(9) -0.0042(8) -0.0031(7) -0.0192(7) O6A 0.0374(9) 0.0278(8) 0.0345(9) -0.0027(8) -0.0094(7) -0.0168(7) C1A 0.0314(13) 0.0379(14) 0.0494(16) -0.0143(13) -0.0100(11) 0.0004(10) C2A 0.0347(13) 0.0335(13) 0.0485(16) -0.0056(13) -0.0196(11) -0.0003(10) C3A 0.0354(13) 0.0417(14) 0.0305(13) -0.0008(12) -0.0166(10) -0.0102(11) C4A 0.0365(13) 0.0423(14) 0.0374(14) -0.0043(12) -0.0170(10) -0.0161(11) C5A 0.0455(15) 0.0494(16) 0.0211(11) -0.0050(12) -0.0062(10) -0.0205(12) C6A 0.0403(14) 0.0467(15) 0.0298(13) -0.0162(12) -0.0017(10) -0.0130(11) C7A 0.0266(12) 0.0402(14) 0.0324(13) -0.0096(12) -0.0037(9) -0.0029(10) C8A 0.0255(12) 0.0486(15) 0.0308(13) -0.0026(12) -0.0022(9) -0.0148(10) C9A 0.0390(14) 0.0458(15) 0.0424(15) -0.0062(13) -0.0077(11) -0.0261(12) C10A 0.0411(14) 0.0437(15) 0.0396(14) -0.0076(12) -0.0126(11) -0.0233(11) C11A 0.0568(16) 0.0279(12) 0.0307(13) -0.0008(11) -0.0127(11) -0.0214(11) C12A 0.0527(16) 0.0266(12) 0.0293(13) -0.0084(11) -0.0103(11) -0.0086(11) O1S 0.0431(11) 0.0709(14) 0.0425(11) -0.0173(11) -0.0027(8) -0.0279(10) _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 1.7752(3) . ? Fe1 O6 2.0368(16) . ? Fe1 O4 2.0394(16) . ? Fe1 O5 2.0654(16) . ? Fe1 O3 2.0763(16) . ? Fe1 O1 2.0884(15) . ? Cl1 O10 1.405(2) . ? Cl1 O7 1.410(2) . ? Cl1 O8 1.415(2) . ? Cl1 O9 1.441(2) . ? Cl2 O14 1.427(2) . ? Cl2 O11 1.4322(19) . ? Cl2 O12 1.436(2) . ? Cl2 O13 1.4577(17) . ? O2 Fe1 1.7752(3) 2_656 ? O1A C12A 1.434(3) . ? O1A C1A 1.438(3) . ? O2A C3A 1.425(3) . ? O2A C2A 1.428(3) . ? O3A C5A 1.428(3) . ? O3A C4A 1.434(3) . ? O4A C6A 1.434(3) . ? O4A C7A 1.438(3) . ? O5A C9A 1.426(3) . ? O5A C8A 1.429(3) . ? O6A C11A 1.431(3) . ? O6A C10A 1.438(3) . ? C1A C2A 1.494(4) . ? C3A C4A 1.502(4) . ? C5A C6A 1.498(4) . ? C7A C8A 1.494(4) . ? C9A C10A 1.507(4) . ? C11A C12A 1.493(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 O2 Fe1 O6 98.24(5) . . ? O2 Fe1 O4 99.55(5) . . ? O6 Fe1 O4 89.07(7) . . ? O2 Fe1 O5 95.19(5) . . ? O6 Fe1 O5 166.57(7) . . ? O4 Fe1 O5 88.82(7) . . ? O2 Fe1 O3 97.13(5) . . ? O6 Fe1 O3 88.75(7) . . ? O4 Fe1 O3 163.31(7) . . ? O5 Fe1 O3 89.47(7) . . ? O2 Fe1 O1 178.39(4) . . ? O6 Fe1 O1 83.05(6) . . ? O4 Fe1 O1 81.40(6) . . ? O5 Fe1 O1 83.52(6) . . ? O3 Fe1 O1 81.92(6) . . ? O10 Cl1 O7 109.0(2) . . ? O10 Cl1 O8 108.42(17) . . ? O7 Cl1 O8 108.2(2) . . ? O10 Cl1 O9 111.91(15) . . ? O7 Cl1 O9 107.37(15) . . ? O8 Cl1 O9 111.77(16) . . ? O14 Cl2 O11 110.66(14) . . ? O14 Cl2 O12 109.65(14) . . ? O11 Cl2 O12 109.35(13) . . ? O14 Cl2 O13 109.60(12) . . ? O11 Cl2 O13 108.76(12) . . ? O12 Cl2 O13 108.78(12) . . ? Fe1 O2 Fe1 180.000(16) . 2_656 ? C12A O1A C1A 111.11(19) . . ? C3A O2A C2A 111.8(2) . . ? C5A O3A C4A 114.19(19) . . ? C6A O4A C7A 111.21(18) . . ? C9A O5A C8A 112.02(19) . . ? C11A O6A C10A 114.88(19) . . ? O1A C1A C2A 109.4(2) . . ? O2A C2A C1A 110.3(2) . . ? O2A C3A C4A 109.7(2) . . ? O3A C4A C3A 113.4(2) . . ? O3A C5A C6A 108.6(2) . . ? O4A C6A C5A 109.4(2) . . ? O4A C7A C8A 109.9(2) . . ? O5A C8A C7A 110.1(2) . . ? O5A C9A C10A 109.4(2) . . ? O6A C10A C9A 114.0(2) . . ? O6A C11A C12A 109.6(2) . . ? O1A C12A C11A 110.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Fe1 O2 Fe1 0(100) . . . 2_656 ? O4 Fe1 O2 Fe1 -91(100) . . . 2_656 ? O5 Fe1 O2 Fe1 179(100) . . . 2_656 ? O3 Fe1 O2 Fe1 89(100) . . . 2_656 ? O1 Fe1 O2 Fe1 143(100) . . . 2_656 ? C12A O1A C1A C2A 164.7(2) . . . . ? C3A O2A C2A C1A -172.0(2) . . . . ? O1A C1A C2A O2A 69.4(3) . . . . ? C2A O2A C3A C4A 177.8(2) . . . . ? C5A O3A C4A C3A -77.3(3) . . . . ? O2A C3A C4A O3A -62.6(3) . . . . ? C4A O3A C5A C6A -178.1(2) . . . . ? C7A O4A C6A C5A 177.3(2) . . . . ? O3A C5A C6A O4A -71.4(3) . . . . ? C6A O4A C7A C8A 161.2(2) . . . . ? C9A O5A C8A C7A -175.2(2) . . . . ? O4A C7A C8A O5A 70.6(3) . . . . ? C8A O5A C9A C10A 179.1(2) . . . . ? C11A O6A C10A C9A -74.8(3) . . . . ? O5A C9A C10A O6A -59.2(3) . . . . ? C10A O6A C11A C12A -179.17(19) . . . . ? C1A O1A C12A C11A 179.2(2) . . . . ? O6A C11A C12A O1A -76.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O4A 0.89 1.88 2.751(2) 166.7 . O1 H1A O1A 0.90 1.88 2.771(2) 170.4 . O3 H3B O6A 0.95 1.75 2.685(2) 168.7 . O3 H3A O13 0.92 2.09 2.934(2) 152.8 2_656 O3 H3A O7 0.92 2.41 2.961(3) 119.0 . O4 H4B O3A 0.86 1.87 2.670(2) 153.5 . O4 H4A O13 0.83 1.96 2.782(2) 170.4 . O4 H4A Cl2 0.83 2.95 3.6559(17) 144.8 . O5 H5B O5A 0.82 1.94 2.763(2) 173.6 . O5 H5A O9 0.90 1.94 2.837(3) 176.2 . O5 H5A Cl1 0.90 2.90 3.7286(18) 154.3 . O6 H6B O2A 0.88 1.90 2.779(2) 170.7 . O6 H6A O1S 0.79 1.86 2.647(2) 170.8 . O1S H1SA O8 0.94 2.03 2.896(3) 151.9 1_455 O1S H1SB O12 0.91 2.06 2.961(3) 169.1 2_656 O1S H1SB Cl2 0.91 2.83 3.664(2) 151.8 2_656 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.726 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.057 data_feno315 _database_code_CSD 149182 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H68 Fe2 N5 O39.50' _chemical_formula_weight 1122.49 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.7399(7) _cell_length_b 14.7129(4) _cell_length_c 22.0035(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.860(2) _cell_angle_gamma 90.00 _cell_volume 4761.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2364 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5946 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16428 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8780 _reflns_number_gt 7432 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+6.4788P] 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 SHELXL _refine_ls_extinction_coef 0.0023(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8780 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.10631(2) 0.99137(2) 0.065326(17) 0.01935(11) Uani 1 1 d . . . Fe2 Fe 0.26648(2) 1.00642(2) -0.321837(16) 0.01715(11) Uani 1 1 d . . . O1 O 0.0000 1.0000 0.0000 0.0225(5) Uani 1 2 d S . . O2 O 0.23011(12) 0.98067(13) 0.14709(9) 0.0275(4) Uani 1 1 d . . . H22 H 0.2340 0.9732 0.1893 0.033 Uiso 1 1 d R . . H21 H 0.2853 1.0051 0.1468 0.033 Uiso 1 1 d R . . O3 O 0.14699(13) 0.87380(14) 0.03469(12) 0.0418(6) Uani 1 1 d . . . H32 H 0.1123 0.8263 0.0157 0.050 Uiso 1 1 d R . . H31 H 0.2003 0.8570 0.0420 0.050 Uiso 1 1 d R . . O4 O 0.18686(13) 1.05281(14) 0.02340(9) 0.0339(5) Uani 1 1 d . . . H42 H 0.1589 1.0619 -0.0188 0.041 Uiso 1 1 d R . . H41 H 0.2245 1.0957 0.0421 0.041 Uiso 1 1 d R . . O5 O 0.08910(15) 1.11098(14) 0.10767(10) 0.0406(5) Uani 1 1 d . . . H52 H 0.0579 1.1604 0.0859 0.049 Uiso 1 1 d R . . H51 H 0.1291 1.1260 0.1480 0.049 Uiso 1 1 d R . . O6 O 0.05650(13) 0.92299(17) 0.12438(11) 0.0434(6) Uani 1 1 d . . . H62 H -0.0009 0.9290 0.1220 0.052 Uiso 1 1 d R . . H61 H 0.0888 0.8824 0.1548 0.052 Uiso 1 1 d R . . O7 O 0.22932(12) 0.98072(12) -0.24528(8) 0.0239(4) Uani 1 1 d . . . H72 H 0.1725 0.9624 -0.2486 0.029 Uiso 1 1 d R . . H71 H 0.2581 0.9867 -0.2101 0.029 Uiso 1 1 d R . . O8 O 0.29350(12) 1.01837(12) -0.40284(8) 0.0218(4) Uani 1 1 d . . . H82 H 0.3170 1.0626 -0.4143 0.026 Uiso 1 1 d R . . H81 H 0.3057 0.9656 -0.4240 0.026 Uiso 1 1 d R . . O9 O 0.20065(12) 0.89215(12) -0.36232(9) 0.0249(4) Uani 1 1 d . . . H92 H 0.2239 0.8352 -0.3435 0.030 Uiso 1 1 d R . . H91 H 0.1432 0.8859 -0.4008 0.030 Uiso 1 1 d R . . O10 O 0.15537(11) 1.08153(12) -0.35821(8) 0.0227(4) Uani 1 1 d . . . H101 H 0.1262 1.0996 -0.3986 0.027 Uiso 1 1 d R . . H102 H 0.1175 1.0959 -0.3379 0.027 Uiso 1 1 d R . . O11 O 0.37826(12) 0.93209(12) -0.27808(8) 0.0243(4) Uani 1 1 d . . . H112 H 0.4257 0.9301 -0.2921 0.029 Uiso 1 1 d R . . H111 H 0.3709 0.8870 -0.2608 0.029 Uiso 1 1 d R . . O12 O 0.33732(12) 1.11554(12) -0.28378(8) 0.0226(4) Uani 1 1 d . . . H122 H 0.3904 1.1174 -0.2520 0.027 Uiso 1 1 d R . . H121 H 0.3162 1.1742 -0.2931 0.027 Uiso 1 1 d R . . O13 O 0.22888(13) 0.78861(13) 0.31814(8) 0.0276(4) Uani 1 1 d . . . O14 O 0.21994(13) 0.91769(13) 0.26812(9) 0.0321(4) Uani 1 1 d . . . O15 O 0.13543(12) 0.80366(12) 0.21889(9) 0.0261(4) Uani 1 1 d . . . O16 O 0.32946(13) 0.85007(15) 0.08258(10) 0.0366(5) Uani 1 1 d . . . O17 O 0.3172(2) 0.73853(17) 0.01789(12) 0.0603(7) Uani 1 1 d . . . O18 O 0.45082(16) 0.7901(2) 0.07609(12) 0.0551(7) Uani 1 1 d . . . O19 O 0.34593(16) 1.14819(15) 0.07591(11) 0.0439(5) Uani 1 1 d . . . O20 O 0.48634(18) 1.1081(2) 0.10884(16) 0.0663(8) Uani 1 1 d . . . O21 O 0.39876(13) 1.04746(14) 0.15392(10) 0.0347(5) Uani 1 1 d . . . O22 O 0.29250(19) 0.63760(17) -0.23199(12) 0.0618(8) Uani 1 1 d . . . O23 O 0.24486(19) 0.72712(15) -0.31429(10) 0.0545(7) Uani 1 1 d . . . O24 O 0.35719(14) 0.76733(14) -0.22674(10) 0.0379(5) Uani 1 1 d . . . O25 O 0.03134(14) 0.86125(15) -0.43554(9) 0.0368(5) Uani 1 1 d . . . O26 O 0.04074(13) 0.92006(13) -0.52384(9) 0.0296(4) Uani 1 1 d . . . O27 O -0.08600(13) 0.86084(14) -0.52401(9) 0.0323(5) Uani 1 1 d . . . N1 N 0.19518(14) 0.83725(15) 0.26842(10) 0.0220(5) Uani 1 1 d . . . N2 N 0.36526(17) 0.79228(17) 0.05849(11) 0.0326(5) Uani 1 1 d . . . N3 N 0.41109(17) 1.10105(17) 0.11211(14) 0.0371(6) Uani 1 1 d . . . N4 N 0.29814(17) 0.71015(16) -0.25761(12) 0.0329(5) Uani 1 1 d . . . N5 N -0.00353(14) 0.88171(15) -0.49497(10) 0.0240(5) Uani 1 1 d . . . O1A O 0.16640(15) 0.88184(15) -0.14868(11) 0.0411(5) Uani 1 1 d . . . O2A O 0.30653(14) 1.00343(14) -0.11744(10) 0.0346(5) Uani 1 1 d . . . O3A O 0.20797(13) 1.16037(14) -0.15703(9) 0.0330(5) Uani 1 1 d . . . O4A O 0.06207(13) 1.11503(14) -0.27807(10) 0.0318(4) Uani 1 1 d . . . O5A O 0.05532(13) 0.92076(14) -0.27834(10) 0.0343(5) Uani 1 1 d . . . C1A C 0.2560(2) 0.8506(2) -0.11815(16) 0.0455(8) Uani 1 1 d . . . H1A2 H 0.2817 0.8322 -0.1513 0.055 Uiso 1 1 calc R . . H1A1 H 0.2565 0.7971 -0.0908 0.055 Uiso 1 1 calc R . . C2A C 0.3120(2) 0.9252(2) -0.07701(15) 0.0401(7) Uani 1 1 d . . . H2A2 H 0.2889 0.9407 -0.0419 0.048 Uiso 1 1 calc R . . H2A1 H 0.3760 0.9053 -0.0568 0.048 Uiso 1 1 calc R . . C3A C 0.3386(2) 1.0857(2) -0.08334(14) 0.0377(7) Uani 1 1 d . . . H3A2 H 0.4059 1.0857 -0.0648 0.045 Uiso 1 1 calc R . . H3A1 H 0.3153 1.0924 -0.0473 0.045 Uiso 1 1 calc R . . C4A C 0.30553(19) 1.1623(2) -0.13060(14) 0.0328(6) Uani 1 1 d . . . H4A2 H 0.3267 1.2210 -0.1083 0.039 Uiso 1 1 calc R . . H4A1 H 0.3301 1.1561 -0.1660 0.039 Uiso 1 1 calc R . . C5A C 0.1678(2) 1.2218(2) -0.20925(14) 0.0323(6) Uani 1 1 d . . . H5A2 H 0.1989 1.2174 -0.2411 0.039 Uiso 1 1 calc R . . H5A1 H 0.1740 1.2849 -0.1926 0.039 Uiso 1 1 calc R . . C6A C 0.07011(19) 1.19848(19) -0.24115(13) 0.0299(6) Uani 1 1 d . . . H6A2 H 0.0419 1.1904 -0.2078 0.036 Uiso 1 1 calc R . . H6A1 H 0.0380 1.2484 -0.2705 0.036 Uiso 1 1 calc R . . C7A C -0.02128(19) 1.0678(2) -0.29045(15) 0.0328(6) Uani 1 1 d . . . H7A2 H -0.0725 1.1040 -0.3198 0.039 Uiso 1 1 calc R . . H7A1 H -0.0319 1.0577 -0.2492 0.039 Uiso 1 1 calc R . . C8A C -0.01546(19) 0.9788(2) -0.32132(14) 0.0315(6) Uani 1 1 d . . . H8A2 H -0.0747 0.9472 -0.3333 0.038 Uiso 1 1 calc R . . H8A1 H -0.0029 0.9898 -0.3617 0.038 Uiso 1 1 calc R . . C9A C 0.0253(2) 0.8665(2) -0.23673(17) 0.0445(8) Uani 1 1 d . . . H9A2 H -0.0211 0.8225 -0.2626 0.053 Uiso 1 1 calc R . . H9A1 H -0.0022 0.9053 -0.2119 0.053 Uiso 1 1 calc R . . C10A C 0.1052(2) 0.8173(2) -0.19144(17) 0.0468(8) Uani 1 1 d . . . H10B H 0.0851 0.7727 -0.1657 0.056 Uiso 1 1 calc R . . H10A H 0.1366 0.7840 -0.2164 0.056 Uiso 1 1 calc R . . O1B O 0.33292(12) 0.86152(12) -0.44884(9) 0.0259(4) Uani 1 1 d . . . O2B O 0.49463(12) 0.91195(14) -0.33738(9) 0.0309(4) Uani 1 1 d . . . O3B O 0.49654(13) 1.10481(14) -0.36523(10) 0.0324(4) Uani 1 1 d . . . O4B O 0.32819(13) 1.17349(12) -0.45474(9) 0.0265(4) Uani 1 1 d . . . O5B O 0.31236(12) 1.01589(12) -0.53061(9) 0.0250(4) Uani 1 1 d . . . C1B C 0.39979(19) 0.80024(19) -0.40825(14) 0.0310(6) Uani 1 1 d . . . H1B2 H 0.4013 0.7450 -0.4335 0.037 Uiso 1 1 calc R . . H1B1 H 0.3820 0.7817 -0.3712 0.037 Uiso 1 1 calc R . . C2B C 0.4938(2) 0.8416(2) -0.38236(15) 0.0359(7) Uani 1 1 d . . . H2B2 H 0.5392 0.7945 -0.3603 0.043 Uiso 1 1 calc R . . H2B1 H 0.5096 0.8671 -0.4186 0.043 Uiso 1 1 calc R . . C3B C 0.57431(19) 0.9689(2) -0.31857(15) 0.0365(7) Uani 1 1 d . . . H3B2 H 0.6280 0.9312 -0.3148 0.044 Uiso 1 1 calc R . . H3B1 H 0.5841 0.9955 -0.2753 0.044 Uiso 1 1 calc R . . C4B C 0.56654(18) 1.0443(2) -0.36625(15) 0.0349(7) Uani 1 1 d . . . H4B2 H 0.6250 1.0773 -0.3544 0.042 Uiso 1 1 calc R . . H4B1 H 0.5519 1.0188 -0.4105 0.042 Uiso 1 1 calc R . . C5B C 0.4924(2) 1.1831(2) -0.40380(15) 0.0347(7) Uani 1 1 d . . . H5B2 H 0.4981 1.1655 -0.4456 0.042 Uiso 1 1 calc R . . H5B1 H 0.5428 1.2250 -0.3808 0.042 Uiso 1 1 calc R . . C6B C 0.4024(2) 1.22928(19) -0.41601(14) 0.0315(6) Uani 1 1 d . . . H6B2 H 0.3956 1.2426 -0.3739 0.038 Uiso 1 1 calc R . . H6B1 H 0.4011 1.2877 -0.4386 0.038 Uiso 1 1 calc R . . C7B C 0.3138(2) 1.17544(19) -0.52311(13) 0.0296(6) Uani 1 1 d . . . H7B2 H 0.3730 1.1740 -0.5295 0.035 Uiso 1 1 calc R . . H7B1 H 0.2816 1.2319 -0.5430 0.035 Uiso 1 1 calc R . . C8B C 0.25831(19) 1.09431(19) -0.55432(13) 0.0295(6) Uani 1 1 d . . . H8B2 H 0.2026 1.0916 -0.5433 0.035 Uiso 1 1 calc R . . H8B1 H 0.2402 1.0980 -0.6022 0.035 Uiso 1 1 calc R . . C9B C 0.26300(19) 0.93353(19) -0.55136(13) 0.0280(6) Uani 1 1 d . . . H9B2 H 0.2460 0.9261 -0.5989 0.034 Uiso 1 1 calc R . . H9B1 H 0.2067 0.9346 -0.5411 0.034 Uiso 1 1 calc R . . C10B C 0.3225(2) 0.85672(19) -0.51650(13) 0.0294(6) Uani 1 1 d . . . H10D H 0.2946 0.7980 -0.5352 0.035 Uiso 1 1 calc R . . H10C H 0.3827 0.8613 -0.5212 0.035 Uiso 1 1 calc R . . O1S O 0.11616(12) 1.04585(14) -0.10800(9) 0.0298(4) Uani 1 1 d . . . H1S2 H 0.1440 1.0827 -0.1281 0.036 Uiso 1 1 d R . . H1S1 H 0.1266 0.9920 -0.1180 0.036 Uiso 1 1 d R . . O2S O -0.01031(12) 1.24113(13) 0.02741(9) 0.0292(4) Uani 1 1 d . . . H2S2 H 0.0150 1.2611 -0.0038 0.035 Uiso 1 1 d R . . H2S1 H -0.0147 1.2915 0.0467 0.035 Uiso 1 1 d R . . O3S O 0.48836(14) 1.10631(16) -0.19145(11) 0.0471(6) Uani 1 1 d . . . H3S2 H 0.5184 1.0541 -0.1890 0.056 Uiso 1 1 d R . . H3S1 H 0.5077 1.1455 -0.1574 0.056 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01598(19) 0.0220(2) 0.01921(19) 0.00070(13) 0.00525(14) 0.00028(14) Fe2 0.01591(19) 0.01805(19) 0.01799(19) -0.00008(13) 0.00666(14) -0.00015(13) O1 0.0198(13) 0.0247(13) 0.0225(13) 0.0002(10) 0.0069(10) -0.0013(10) O2 0.0186(9) 0.0400(11) 0.0225(9) 0.0012(8) 0.0057(7) 0.0005(8) O3 0.0194(10) 0.0299(11) 0.0691(15) -0.0173(10) 0.0073(10) 0.0015(9) O4 0.0297(10) 0.0404(12) 0.0298(10) 0.0006(9) 0.0084(8) -0.0160(9) O5 0.0435(12) 0.0355(12) 0.0282(10) -0.0109(9) -0.0052(9) 0.0141(10) O6 0.0189(10) 0.0656(16) 0.0470(13) 0.0338(11) 0.0131(9) 0.0097(10) O7 0.0188(9) 0.0337(10) 0.0192(9) 0.0023(7) 0.0069(7) -0.0010(8) O8 0.0247(9) 0.0192(9) 0.0254(9) -0.0010(7) 0.0136(8) -0.0018(7) O9 0.0256(9) 0.0202(9) 0.0263(9) -0.0007(7) 0.0059(8) -0.0039(8) O10 0.0189(9) 0.0289(10) 0.0206(9) 0.0042(7) 0.0074(7) 0.0060(7) O11 0.0225(9) 0.0256(9) 0.0268(9) 0.0048(7) 0.0112(8) 0.0045(8) O12 0.0193(9) 0.0221(9) 0.0241(9) -0.0028(7) 0.0049(7) -0.0005(7) O13 0.0330(10) 0.0257(10) 0.0215(9) 0.0045(7) 0.0065(8) 0.0035(8) O14 0.0339(11) 0.0258(10) 0.0305(10) 0.0023(8) 0.0041(8) -0.0068(9) O15 0.0233(9) 0.0254(10) 0.0245(9) -0.0007(7) 0.0025(7) 0.0014(8) O16 0.0227(10) 0.0463(13) 0.0379(11) -0.0116(10) 0.0074(9) 0.0054(9) O17 0.089(2) 0.0393(14) 0.0412(14) -0.0102(11) 0.0089(13) -0.0062(14) O18 0.0353(13) 0.0801(19) 0.0504(14) -0.0080(13) 0.0160(11) 0.0235(13) O19 0.0434(13) 0.0378(12) 0.0419(13) 0.0058(10) 0.0049(10) -0.0013(10) O20 0.0433(15) 0.0610(17) 0.106(2) 0.0253(16) 0.0403(15) 0.0043(13) O21 0.0294(10) 0.0340(11) 0.0440(12) 0.0110(9) 0.0172(9) 0.0011(9) O22 0.0662(17) 0.0418(14) 0.0488(14) 0.0226(11) -0.0145(12) -0.0212(13) O23 0.0833(18) 0.0288(12) 0.0268(11) 0.0053(9) -0.0106(11) 0.0008(12) O24 0.0347(11) 0.0317(11) 0.0423(12) 0.0039(9) 0.0074(9) -0.0015(9) O25 0.0316(11) 0.0413(12) 0.0265(10) 0.0105(9) -0.0030(8) -0.0101(9) O26 0.0283(10) 0.0283(10) 0.0376(11) 0.0017(8) 0.0183(9) 0.0009(8) O27 0.0240(10) 0.0388(11) 0.0275(10) 0.0066(8) 0.0012(8) -0.0085(9) N1 0.0184(10) 0.0235(11) 0.0233(11) 0.0002(9) 0.0066(9) 0.0028(9) N2 0.0391(14) 0.0296(13) 0.0274(12) 0.0013(10) 0.0098(10) 0.0043(11) N3 0.0344(14) 0.0271(13) 0.0564(17) -0.0108(12) 0.0241(13) -0.0093(11) N4 0.0376(14) 0.0272(13) 0.0309(13) 0.0068(10) 0.0085(11) 0.0062(11) N5 0.0234(11) 0.0197(11) 0.0268(12) 0.0004(9) 0.0064(9) -0.0010(9) O1A 0.0440(13) 0.0392(12) 0.0431(12) 0.0099(10) 0.0192(10) 0.0036(10) O2A 0.0325(11) 0.0457(13) 0.0250(10) 0.0027(8) 0.0095(9) 0.0031(9) O3A 0.0313(11) 0.0368(11) 0.0323(11) 0.0036(9) 0.0129(9) -0.0012(9) O4A 0.0243(10) 0.0394(12) 0.0343(11) -0.0018(9) 0.0135(8) -0.0001(9) O5A 0.0286(10) 0.0347(11) 0.0424(12) 0.0000(9) 0.0160(9) -0.0053(9) C1A 0.049(2) 0.048(2) 0.0410(18) 0.0173(15) 0.0177(15) 0.0076(16) C2A 0.0353(16) 0.0486(19) 0.0351(16) 0.0193(14) 0.0108(13) 0.0125(15) C3A 0.0283(15) 0.055(2) 0.0279(14) -0.0035(13) 0.0072(12) -0.0032(14) C4A 0.0241(14) 0.0390(17) 0.0345(15) -0.0088(13) 0.0093(12) -0.0076(12) C5A 0.0382(16) 0.0317(15) 0.0286(14) 0.0000(11) 0.0140(12) -0.0013(13) C6A 0.0349(15) 0.0284(15) 0.0282(14) 0.0006(11) 0.0136(12) 0.0076(12) C7A 0.0211(13) 0.0407(17) 0.0357(15) 0.0037(13) 0.0090(12) 0.0034(12) C8A 0.0201(13) 0.0435(17) 0.0278(14) 0.0001(12) 0.0048(11) -0.0051(12) C9A 0.049(2) 0.0416(18) 0.0464(19) 0.0018(15) 0.0214(16) -0.0128(16) C10A 0.056(2) 0.0305(17) 0.051(2) 0.0082(14) 0.0155(16) -0.0119(15) O1B 0.0289(10) 0.0245(9) 0.0281(10) -0.0029(7) 0.0148(8) 0.0030(8) O2B 0.0222(9) 0.0394(11) 0.0334(10) -0.0040(9) 0.0128(8) -0.0002(8) O3B 0.0253(10) 0.0402(12) 0.0350(11) 0.0000(9) 0.0148(8) -0.0042(9) O4B 0.0293(10) 0.0249(10) 0.0292(10) 0.0015(8) 0.0152(8) -0.0022(8) O5B 0.0242(10) 0.0251(9) 0.0260(9) -0.0018(7) 0.0095(8) -0.0008(8) C1B 0.0337(15) 0.0243(14) 0.0376(15) 0.0002(11) 0.0158(13) 0.0078(12) C2B 0.0268(15) 0.0412(17) 0.0424(17) -0.0064(13) 0.0155(13) 0.0095(13) C3B 0.0189(13) 0.0521(19) 0.0357(16) 0.0020(14) 0.0061(12) -0.0016(13) C4B 0.0179(13) 0.0522(19) 0.0347(16) -0.0022(14) 0.0095(12) -0.0027(13) C5B 0.0329(15) 0.0388(17) 0.0370(16) -0.0047(13) 0.0182(13) -0.0141(13) C6B 0.0384(16) 0.0232(14) 0.0396(16) -0.0069(12) 0.0220(13) -0.0102(12) C7B 0.0363(15) 0.0291(14) 0.0278(14) 0.0065(11) 0.0169(12) 0.0046(12) C8B 0.0285(14) 0.0322(15) 0.0281(14) 0.0046(11) 0.0103(11) 0.0052(12) C9B 0.0303(14) 0.0292(14) 0.0255(13) -0.0079(11) 0.0112(11) -0.0072(12) C10B 0.0358(15) 0.0283(14) 0.0301(14) -0.0077(11) 0.0189(12) -0.0046(12) O1S 0.0224(9) 0.0389(11) 0.0313(10) 0.0091(8) 0.0134(8) 0.0034(8) O2S 0.0292(10) 0.0230(10) 0.0359(11) -0.0047(8) 0.0122(8) -0.0016(8) O3S 0.0341(12) 0.0377(12) 0.0493(13) -0.0097(10) -0.0098(10) 0.0080(10) _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 1.7803(4) . ? Fe1 O6 2.010(2) . ? Fe1 O4 2.0270(19) . ? Fe1 O3 2.041(2) . ? Fe1 O5 2.054(2) . ? Fe1 O2 2.1358(18) . ? Fe2 O12 1.9640(17) . ? Fe2 O10 1.9808(17) . ? Fe2 O8 1.9820(17) . ? Fe2 O11 2.0030(17) . ? Fe2 O7 2.0061(17) . ? Fe2 O9 2.0089(18) . ? O1 Fe1 1.7803(4) 3_575 ? O13 N1 1.256(3) . ? O14 N1 1.247(3) . ? O15 N1 1.260(3) . ? O16 N2 1.239(3) . ? O17 N2 1.231(3) . ? O18 N2 1.262(3) . ? O19 N3 1.259(3) . ? O20 N3 1.216(3) . ? O21 N3 1.278(3) . ? O22 N4 1.225(3) . ? O23 N4 1.256(3) . ? O24 N4 1.258(3) . ? O25 N5 1.261(3) . ? O26 N5 1.234(3) . ? O27 N5 1.264(3) . ? O1A C1A 1.406(4) . ? O1A C10A 1.438(4) . ? O2A C3A 1.419(4) . ? O2A C2A 1.438(4) . ? O3A C5A 1.421(3) . ? O3A C4A 1.436(3) . ? O4A C7A 1.423(3) . ? O4A C6A 1.453(3) . ? O5A C9A 1.417(4) . ? O5A C8A 1.454(4) . ? C1A C2A 1.494(5) . ? C3A C4A 1.496(4) . ? C5A C6A 1.485(4) . ? C7A C8A 1.493(4) . ? C9A C10A 1.485(5) . ? O1B C1B 1.431(3) . ? O1B C10B 1.441(3) . ? O2B C2B 1.428(3) . ? O2B C3B 1.441(3) . ? O3B C5B 1.419(4) . ? O3B C4B 1.423(4) . ? O4B C6B 1.434(3) . ? O4B C7B 1.440(3) . ? O5B C8B 1.418(3) . ? O5B C9B 1.424(3) . ? C1B C2B 1.512(4) . ? C3B C4B 1.501(4) . ? C5B C6B 1.505(4) . ? C7B C8B 1.494(4) . ? C9B C10B 1.494(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 O6 94.98(6) . . ? O1 Fe1 O4 99.27(6) . . ? O6 Fe1 O4 165.59(8) . . ? O1 Fe1 O3 96.26(6) . . ? O6 Fe1 O3 91.70(10) . . ? O4 Fe1 O3 84.66(9) . . ? O1 Fe1 O5 93.85(6) . . ? O6 Fe1 O5 89.47(10) . . ? O4 Fe1 O5 91.68(9) . . ? O3 Fe1 O5 169.68(8) . . ? O1 Fe1 O2 177.04(5) . . ? O6 Fe1 O2 82.38(8) . . ? O4 Fe1 O2 83.42(8) . . ? O3 Fe1 O2 85.20(8) . . ? O5 Fe1 O2 84.79(8) . . ? O12 Fe2 O10 90.10(7) . . ? O12 Fe2 O8 92.28(7) . . ? O10 Fe2 O8 91.63(7) . . ? O12 Fe2 O11 88.46(7) . . ? O10 Fe2 O11 175.46(7) . . ? O8 Fe2 O11 92.73(7) . . ? O12 Fe2 O7 94.99(7) . . ? O10 Fe2 O7 87.99(7) . . ? O8 Fe2 O7 172.71(7) . . ? O11 Fe2 O7 87.84(7) . . ? O12 Fe2 O9 176.38(7) . . ? O10 Fe2 O9 92.64(7) . . ? O8 Fe2 O9 85.27(7) . . ? O11 Fe2 O9 88.99(7) . . ? O7 Fe2 O9 87.48(7) . . ? Fe1 O1 Fe1 180.0 . 3_575 ? O14 N1 O13 120.6(2) . . ? O14 N1 O15 120.4(2) . . ? O13 N1 O15 118.9(2) . . ? O17 N2 O16 119.7(3) . . ? O17 N2 O18 121.3(3) . . ? O16 N2 O18 119.0(2) . . ? O20 N3 O19 120.4(3) . . ? O20 N3 O21 119.7(3) . . ? O19 N3 O21 119.8(2) . . ? O22 N4 O23 119.9(3) . . ? O22 N4 O24 119.7(2) . . ? O23 N4 O24 120.5(2) . . ? O26 N5 O25 121.7(2) . . ? O26 N5 O27 121.2(2) . . ? O25 N5 O27 117.1(2) . . ? C1A O1A C10A 114.9(3) . . ? C3A O2A C2A 115.1(2) . . ? C5A O3A C4A 114.8(2) . . ? C7A O4A C6A 114.3(2) . . ? C9A O5A C8A 113.4(2) . . ? O1A C1A C2A 108.9(3) . . ? O2A C2A C1A 108.7(2) . . ? O2A C3A C4A 107.8(2) . . ? O3A C4A C3A 108.9(2) . . ? O3A C5A C6A 108.9(2) . . ? O4A C6A C5A 109.2(2) . . ? O4A C7A C8A 108.3(2) . . ? O5A C8A C7A 112.1(2) . . ? O5A C9A C10A 108.1(3) . . ? O1A C10A C9A 109.1(3) . . ? C1B O1B C10B 113.7(2) . . ? C2B O2B C3B 114.4(2) . . ? C5B O3B C4B 111.7(2) . . ? C6B O4B C7B 113.6(2) . . ? C8B O5B C9B 112.8(2) . . ? O1B C1B C2B 112.6(2) . . ? O2B C2B C1B 108.6(2) . . ? O2B C3B C4B 112.5(2) . . ? O3B C4B C3B 108.8(2) . . ? O3B C5B C6B 108.3(2) . . ? O4B C6B C5B 111.3(2) . . ? O4B C7B C8B 108.2(2) . . ? O5B C8B C7B 107.7(2) . . ? O5B C9B C10B 108.0(2) . . ? O1B C10B C9B 108.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Fe1 O1 Fe1 7.89(7) . . . 3_575 ? O4 Fe1 O1 Fe1 -174.25(7) . . . 3_575 ? O3 Fe1 O1 Fe1 100.16(7) . . . 3_575 ? O5 Fe1 O1 Fe1 -81.92(7) . . . 3_575 ? O2 Fe1 O1 Fe1 -19.2(11) . . . 3_575 ? C10A O1A C1A C2A 178.4(3) . . . . ? C3A O2A C2A C1A 166.2(3) . . . . ? O1A C1A C2A O2A -56.9(3) . . . . ? C2A O2A C3A C4A -164.9(2) . . . . ? C5A O3A C4A C3A -171.7(2) . . . . ? O2A C3A C4A O3A 59.4(3) . . . . ? C4A O3A C5A C6A 167.4(2) . . . . ? C7A O4A C6A C5A 157.8(2) . . . . ? O3A C5A C6A O4A -72.6(3) . . . . ? C6A O4A C7A C8A -173.2(2) . . . . ? C9A O5A C8A C7A 87.5(3) . . . . ? O4A C7A C8A O5A 63.2(3) . . . . ? C8A O5A C9A C10A -174.8(3) . . . . ? C1A O1A C10A C9A -160.4(3) . . . . ? O5A C9A C10A O1A 67.0(4) . . . . ? C10B O1B C1B C2B 89.3(3) . . . . ? C3B O2B C2B C1B -168.5(2) . . . . ? O1B C1B C2B O2B 68.3(3) . . . . ? C2B O2B C3B C4B 84.1(3) . . . . ? C5B O3B C4B C3B 173.4(2) . . . . ? O2B C3B C4B O3B 66.1(3) . . . . ? C4B O3B C5B C6B 163.9(2) . . . . ? C7B O4B C6B C5B -79.0(3) . . . . ? O3B C5B C6B O4B -65.3(3) . . . . ? C6B O4B C7B C8B 161.4(2) . . . . ? C9B O5B C8B C7B 173.3(2) . . . . ? O4B C7B C8B O5B -67.5(3) . . . . ? C8B O5B C9B C10B -172.4(2) . . . . ? C1B O1B C10B C9B -170.8(2) . . . . ? O5B C9B C10B O1B 69.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H22 O14 0.92 2.00 2.878(3) 160.3 . O2 H21 O21 0.94 1.84 2.784(3) 174.5 . O3 H32 O2S 0.89 1.84 2.695(3) 160.0 3_575 O3 H31 O16 0.83 1.91 2.707(3) 159.4 . O4 H42 O1S 0.88 1.85 2.705(3) 162.1 . O4 H41 O19 0.86 1.95 2.741(3) 152.4 . O4 H41 O17 0.86 2.44 2.873(3) 111.3 2 O5 H52 O2S 0.91 1.80 2.695(3) 167.2 . O5 H51 O22 0.91 1.83 2.735(3) 171.1 2 O6 H62 O1S 0.89 1.77 2.651(3) 171.0 3_575 O6 H61 O15 0.91 1.77 2.667(3) 169.8 . O7 H72 O5A 0.91 1.83 2.718(3) 164.4 . O7 H72 O1A 0.91 2.53 3.019(3) 114.1 . O7 H71 O2A 0.75 1.92 2.658(3) 167.3 . O8 H82 O4B 0.83 1.90 2.694(2) 160.4 . O8 H81 O1B 0.96 1.73 2.680(2) 169.9 . O9 H92 O23 0.95 1.70 2.641(3) 169.3 . O9 H91 O25 1.00 1.69 2.617(3) 152.3 . O10 H101 O27 0.88 1.69 2.571(2) 171.3 3_574 O10 H101 N5 0.88 2.46 3.308(3) 160.1 3_574 O10 H101 O26 0.88 2.59 3.249(3) 132.2 3_574 O10 H102 O4A 0.89 1.84 2.712(3) 165.8 . O11 H112 O2B 0.90 1.74 2.617(3) 164.1 . O11 H111 O24 0.79 1.96 2.744(3) 172.5 . O12 H122 O3S 0.88 1.65 2.522(3) 172.5 . O12 H121 O13 0.92 1.83 2.753(3) 175.6 2 O12 H121 O15 0.92 2.45 3.074(3) 125.4 2 O12 H121 N1 0.92 2.48 3.338(3) 155.0 2 O1S H1S2 O3A 0.91 1.78 2.684(3) 172.3 . O1S H1S1 O1A 0.85 1.94 2.784(3) 168.3 . O2S H2S2 O18 0.95 1.90 2.846(3) 170.4 2 O2S H2S1 O20 0.87 2.01 2.864(3) 167.7 4_585 O2S H2S1 O19 0.87 2.65 3.260(3) 128.3 4_585 O2S H2S1 N3 0.87 2.67 3.469(3) 153.4 4_585 O3S H3S2 O21 0.89 1.95 2.813(3) 161.1 3_675 O3S H3S1 O18 0.91 1.92 2.820(3) 169.9 3_675 O3S H3S1 O16 0.91 2.51 3.079(3) 121.5 3_675 O3S H3S1 N2 0.91 2.54 3.360(3) 149.9 3_675 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.099 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.068