# ic9802404.cif _publ_contact_author ; Dr. Alan L. Balch Department of Chemistry University of California One Shields Ave Davis, CA 95616-5295 USA ; _publ_contact_author_email balch@chem.ucdavis.edu #AUTHOR LIST loop_ _publ_author_name 'Joe H. Satcher' 'Marilyn M. Olmstead' 'Michael W. Droege' 'Sean R. Parkin' 'Bruce C. Noll' 'Leopold May' 'Alan L. Balch' #JOURNAL _journal_name_full 'submitted to Inorganic Chemistry' data_sp46m #Compound 1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; [Fe~4~(\m-O)~2~(\m-BMDP)~2~(\m-OAc)~2~][NO~3~]~3~[OH]^.^12H~2~O ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C66 H89 N19 O30 Fe4' _chemical_formula_weight 1851.96 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 '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 12.228(3) _cell_length_b 13.915(3) _cell_length_c 14.120(3) _cell_angle_alpha 115.99(2) _cell_angle_beta 108.02(2) _cell_angle_gamma 95.73(2) _cell_volume 1974.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 8.0 _cell_measurement_theta_max 29.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 962 _exptl_absorpt_coefficient_mu 6.605 _exptl_absorpt_correction_type XABS2 _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.718 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens rotating Cu anode' _diffrn_radiation_monochromator 'nickel filter' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method 2\q-\w _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 5118 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 54.30 _reflns_number_total 4829 _reflns_number_observed 3585 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V. 5.03, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXTL V. 5.03, XCIF (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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. One nitrate group is ordered; the other shares its site with a hydroxide molecule. The disordered nitrate was refined by restraining its 1,2- and 1,3- distances to be the same as the ordered nitrate (SAME instruction). Several molecules of solvent water were included at occupancies of 1, 0.5 and 0.25, depending on their peak heights on a difference Fourier map. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+8.2250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4814 _refine_ls_number_parameters 529 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_obs 0.0708 _refine_ls_wR_factor_all 0.2250 _refine_ls_wR_factor_obs 0.1802 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.059 _refine_ls_restrained_S_all 1.122 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.022 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.20064(10) 0.56559(10) 0.58574(10) 0.0320(4) Uani 1 d . . Fe2 Fe 0.01517(10) 0.61535(10) 0.40535(10) 0.0323(4) Uani 1 d . . O1 O 0.0962(5) 0.6347(4) 0.5464(4) 0.0369(13) Uani 1 d . . O2 O 0.1637(4) 0.4263(4) 0.4413(4) 0.0345(13) Uani 1 d . . O3 O 0.0500(5) 0.4657(4) 0.3136(4) 0.0353(13) Uani 1 d . . O4 O 0.1521(4) 0.4814(4) 0.6535(4) 0.0341(13) Uani 1 d . . N1 N 0.3042(5) 0.6793(5) 0.7703(5) 0.036(2) Uani 1 d . . N2 N 0.0654(6) 0.4078(5) 0.7778(5) 0.034(2) Uani 1 d . . N3 N 0.5492(5) 0.7433(5) 0.6876(5) 0.0329(15) Uani 1 d . . N4 N 0.3664(6) 0.6234(5) 0.5905(5) 0.034(2) Uani 1 d . . N5 N 0.1500(6) 0.1479(5) 0.6336(5) 0.0327(15) Uani 1 d . . N6 N 0.0559(5) 0.2491(5) 0.5682(5) 0.034(2) Uani 1 d . . N7 N -0.2464(6) 0.3065(6) 0.7293(6) 0.042(2) Uani 1 d . . N8 N -0.1530(6) 0.3056(5) 0.6170(5) 0.035(2) Uani 1 d . . C1 C 0.1027(7) 0.2976(6) 0.2429(6) 0.037(2) Uani 1 d . . H1A H 0.1510(36) 0.3149(7) 0.2055(27) 0.056 Uiso 1 calc R . H1B H 0.0201(8) 0.2584(21) 0.1870(22) 0.056 Uiso 1 calc R . H1C H 0.1356(41) 0.2504(18) 0.2727(9) 0.056 Uiso 1 calc R . C2 C 0.1049(7) 0.4033(6) 0.3397(7) 0.033(2) Uani 1 d . . C3 C 0.1681(7) 0.5072(7) 0.8395(7) 0.039(2) Uani 1 d . . H3A H 0.2228(7) 0.5115(7) 0.9105(7) 0.046 Uiso 1 calc R . H3B H 0.1399(7) 0.5750(7) 0.8611(7) 0.046 Uiso 1 calc R . C4 C 0.2341(7) 0.4996(7) 0.7614(7) 0.040(2) Uani 1 d . . H4 H 0.2669(7) 0.4338(7) 0.7463(7) 0.048 Uiso 1 calc R . C5 C 0.3387(7) 0.6023(7) 0.8139(7) 0.041(2) Uani 1 d . . H5A H 0.3655(7) 0.6419(7) 0.8984(7) 0.049 Uiso 1 calc R . H5B H 0.4065(7) 0.5784(7) 0.7953(7) 0.049 Uiso 1 calc R . C6 C 0.2309(7) 0.7433(7) 0.8240(7) 0.044(2) Uani 1 d . . H6A H 0.1553(21) 0.6925(8) 0.8032(37) 0.066 Uiso 1 calc R . H6B H 0.2144(40) 0.7964(31) 0.7971(35) 0.066 Uiso 1 calc R . H6C H 0.2741(21) 0.7837(35) 0.9075(7) 0.066 Uiso 1 calc R . C7 C 0.4142(7) 0.7547(7) 0.7926(7) 0.041(2) Uani 1 d . . H7A H 0.4803(7) 0.7656(7) 0.8613(7) 0.049 Uiso 1 calc R . H7B H 0.4010(7) 0.8281(7) 0.8071(7) 0.049 Uiso 1 calc R . C8 C 0.4462(7) 0.7058(6) 0.6916(6) 0.035(2) Uani 1 d . . C9 C 0.6504(7) 0.8362(7) 0.7822(7) 0.042(2) Uani 1 d . . H9A H 0.6881(29) 0.8754(26) 0.7524(9) 0.063 Uiso 1 calc R . H9B H 0.7088(23) 0.8080(8) 0.8206(28) 0.063 Uiso 1 calc R . H9C H 0.6221(10) 0.8875(23) 0.8371(23) 0.063 Uiso 1 calc R . C10 C 0.5369(7) 0.6821(6) 0.5743(7) 0.034(2) Uani 1 d . . C11 C 0.6154(7) 0.6904(7) 0.5230(7) 0.040(2) Uani 1 d . . H11 H 0.6929(7) 0.7414(7) 0.5656(7) 0.049 Uiso 1 calc R . C12 C 0.5733(8) 0.6196(7) 0.4059(7) 0.041(2) Uani 1 d . . H12 H 0.6233(8) 0.6221(7) 0.3667(7) 0.050 Uiso 1 calc R . C13 C 0.4596(8) 0.5446(7) 0.3437(7) 0.040(2) Uani 1 d . . H13 H 0.4343(8) 0.4980(7) 0.2633(7) 0.048 Uiso 1 calc R . C14 C 0.3824(7) 0.5360(6) 0.3954(7) 0.035(2) Uani 1 d . . H14 H 0.3054(7) 0.4842(6) 0.3527(7) 0.043 Uiso 1 calc R . C15 C 0.4242(7) 0.6080(6) 0.5145(6) 0.032(2) Uani 1 d . . C16 C 0.0984(8) 0.3063(6) 0.7709(6) 0.037(2) Uani 1 d . . H16A H 0.0392(8) 0.2639(6) 0.7828(6) 0.045 Uiso 1 calc R . H16B H 0.1776(8) 0.3277(6) 0.8328(6) 0.045 Uiso 1 calc R . C17 C 0.1032(7) 0.2340(6) 0.6578(6) 0.034(2) Uani 1 d . . C18 C 0.2042(8) 0.1062(7) 0.7099(7) 0.045(2) Uani 1 d . . H18A H 0.2867(17) 0.1077(42) 0.7167(37) 0.068 Uiso 1 calc R . H18B H 0.1582(29) 0.0297(17) 0.6786(24) 0.068 Uiso 1 calc R . H18C H 0.2043(44) 0.1532(27) 0.7858(15) 0.068 Uiso 1 calc R . C19 C 0.1329(7) 0.1009(6) 0.5196(7) 0.036(2) Uani 1 d . . C20 C 0.1644(8) 0.0116(7) 0.4498(7) 0.045(2) Uani 1 d . . H20 H 0.2067(8) -0.0300(7) 0.4784(7) 0.053 Uiso 1 calc R . C21 C 0.1317(8) -0.0143(7) 0.3363(7) 0.044(2) Uani 1 d . . H21 H 0.1513(8) -0.0753(7) 0.2858(7) 0.053 Uiso 1 calc R . C22 C 0.0700(8) 0.0483(6) 0.2952(7) 0.043(2) Uani 1 d . . H22 H 0.0480(8) 0.0282(6) 0.2170(7) 0.052 Uiso 1 calc R . C23 C 0.0408(7) 0.1375(6) 0.3648(7) 0.036(2) Uani 1 d . . H23 H 0.0003(7) 0.1802(6) 0.3364(7) 0.044 Uiso 1 calc R . C24 C 0.0720(7) 0.1636(6) 0.4778(6) 0.035(2) Uani 1 d . . C25 C -0.0309(7) 0.4248(7) 0.8217(7) 0.040(2) Uani 1 d . . H25A H -0.0342(7) 0.5029(7) 0.8508(7) 0.048 Uiso 1 calc R . H25B H -0.0155(7) 0.4080(7) 0.8852(7) 0.048 Uiso 1 calc R . C26 C -0.1457(7) 0.3481(6) 0.7244(7) 0.037(2) Uani 1 d . . C27 C -0.2749(9) 0.3421(8) 0.8310(8) 0.056(2) Uani 1 d . . H27A H -0.3042(53) 0.2767(9) 0.8356(30) 0.083 Uiso 1 calc R . H27B H -0.3367(41) 0.3814(46) 0.8256(27) 0.083 Uiso 1 calc R . H27C H -0.2027(16) 0.3918(42) 0.8999(9) 0.083 Uiso 1 calc R . C28 C -0.2656(7) 0.2303(7) 0.5474(7) 0.040(2) Uani 1 d . . C29 C -0.3174(8) 0.1580(7) 0.4294(7) 0.044(2) Uani 1 d . . H29 H -0.2760(8) 0.1556(7) 0.3819(7) 0.053 Uiso 1 calc R . C30 C -0.4301(9) 0.0909(8) 0.3849(9) 0.057(3) Uani 1 d . . H30 H -0.4680(9) 0.0406(8) 0.3047(9) 0.069 Uiso 1 calc R . C31 C -0.4911(9) 0.0945(8) 0.4551(10) 0.063(3) Uani 1 d . . H31 H -0.5701(9) 0.0473(8) 0.4206(10) 0.075 Uiso 1 calc R . C32 C -0.4416(8) 0.1631(8) 0.5711(9) 0.054(2) Uani 1 d . . H32 H -0.4835(8) 0.1641(8) 0.6179(9) 0.065 Uiso 1 calc R . C33 C -0.3277(7) 0.2308(7) 0.6165(8) 0.042(2) Uani 1 d . . N9 N -0.0561(10) 0.7099(7) 1.0061(7) 0.065(2) Uani 1 d D . O5 O 0.0468(7) 0.7006(6) 1.0216(6) 0.076(2) Uani 1 d D . O6 O -0.1462(7) 0.6247(6) 0.9545(6) 0.069(2) Uani 1 d D . O7 O -0.0755(9) 0.8032(6) 1.0419(7) 0.102(3) Uani 1 d D . N10 N 0.4538(18) 0.4048(17) 0.9051(16) 0.081(6) Uiso 0.50 d PD 1 O8 O 0.4125(19) 0.3229(16) 0.8102(17) 0.106(8) Uiso 0.50 d PD 1 O9 O 0.4110(25) 0.4418(22) 0.9750(22) 0.175(10) Uiso 0.50 d PD 1 O10 O 0.5321(25) 0.4840(22) 0.9132(27) 0.203(12) Uiso 0.50 d PD 1 O11 O 0.4169(21) 0.3293(20) 0.8578(22) 0.108(7) Uiso 0.50 d P 2 O1W O -0.3489(8) 0.7052(7) 0.9548(8) 0.100(3) Uiso 1 d . 2 O2W O 0.4540(9) 0.8278(8) 1.1098(8) 0.117(3) Uiso 1 d . 2 O3W O 0.5113(30) 1.0383(26) 0.9026(27) 0.083(9) Uiso 0.25 d P 2 O4W O 0.2716(18) 1.0587(15) 0.9220(15) 0.097(5) Uiso 0.50 d P 2 O5W O 0.2282(9) 0.8923(8) 1.1145(9) 0.121(3) Uiso 1 d . 2 O6W O 0.1044(13) 0.9672(12) 0.9762(12) 0.074(4) Uiso 0.50 d P 2 O7W O 0.4411(20) 1.0169(15) 0.9225(16) 0.096(5) Uiso 0.50 d P 2 O8W O 0.1901(23) 1.0146(20) 0.9190(20) 0.138(8) Uiso 0.50 d P 2 O9W O 0.1519(24) 0.9304(22) 1.0442(23) 0.066(7) Uiso 0.25 d P 2 O10W O 0.3679(30) 1.0268(24) 0.8977(25) 0.070(8) Uiso 0.25 d P 2 O11W O 0.3800(29) 0.8807(26) 1.1402(26) 0.083(9) Uiso 0.25 d P 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 0.0300(7) 0.0338(7) 0.0291(7) 0.0139(6) 0.0111(5) 0.0074(6) Fe2 0.0335(8) 0.0332(7) 0.0305(7) 0.0153(6) 0.0130(6) 0.0109(6) O1 0.037(3) 0.040(3) 0.033(3) 0.016(3) 0.015(2) 0.011(3) O2 0.035(3) 0.036(3) 0.030(3) 0.017(2) 0.010(3) 0.007(2) O3 0.046(3) 0.033(3) 0.031(3) 0.017(2) 0.017(3) 0.012(3) O4 0.032(3) 0.041(3) 0.030(3) 0.020(2) 0.009(2) 0.013(3) N1 0.030(4) 0.036(4) 0.036(4) 0.013(3) 0.015(3) 0.003(3) N2 0.035(4) 0.039(4) 0.032(3) 0.020(3) 0.015(3) 0.012(3) N3 0.027(4) 0.031(4) 0.041(4) 0.019(3) 0.013(3) 0.005(3) N4 0.039(4) 0.031(4) 0.034(4) 0.018(3) 0.015(3) 0.010(3) N5 0.035(4) 0.031(4) 0.032(4) 0.017(3) 0.011(3) 0.013(3) N6 0.032(4) 0.037(4) 0.034(4) 0.018(3) 0.014(3) 0.013(3) N7 0.048(5) 0.044(4) 0.058(5) 0.035(4) 0.032(4) 0.018(4) N8 0.031(4) 0.034(4) 0.043(4) 0.022(3) 0.012(3) 0.018(3) C1 0.038(5) 0.038(5) 0.035(4) 0.017(4) 0.015(4) 0.011(4) C2 0.027(4) 0.033(4) 0.040(5) 0.019(4) 0.016(4) 0.005(4) C3 0.043(5) 0.039(5) 0.035(4) 0.019(4) 0.016(4) 0.008(4) C4 0.036(5) 0.047(5) 0.040(5) 0.023(4) 0.013(4) 0.018(4) C5 0.038(5) 0.044(5) 0.036(4) 0.020(4) 0.010(4) 0.004(4) C6 0.035(5) 0.047(5) 0.038(5) 0.011(4) 0.014(4) 0.013(4) C7 0.028(5) 0.042(5) 0.044(5) 0.015(4) 0.012(4) 0.011(4) C8 0.040(5) 0.034(5) 0.034(5) 0.021(4) 0.012(4) 0.013(4) C9 0.030(5) 0.036(5) 0.047(5) 0.015(4) 0.011(4) -0.002(4) C10 0.034(5) 0.030(4) 0.043(5) 0.022(4) 0.015(4) 0.014(4) C11 0.033(5) 0.039(5) 0.054(6) 0.027(4) 0.018(4) 0.007(4) C12 0.047(6) 0.043(5) 0.053(6) 0.031(5) 0.031(5) 0.017(4) C13 0.048(6) 0.040(5) 0.044(5) 0.024(4) 0.028(4) 0.016(4) C14 0.038(5) 0.031(4) 0.042(5) 0.021(4) 0.016(4) 0.012(4) C15 0.028(5) 0.032(4) 0.042(5) 0.021(4) 0.016(4) 0.011(4) C16 0.048(5) 0.040(5) 0.035(4) 0.025(4) 0.016(4) 0.022(4) C17 0.028(4) 0.033(5) 0.035(5) 0.016(4) 0.008(4) 0.005(4) C18 0.051(6) 0.041(5) 0.052(5) 0.027(4) 0.022(5) 0.017(4) C19 0.033(5) 0.033(5) 0.041(5) 0.017(4) 0.016(4) 0.006(4) C20 0.048(6) 0.042(5) 0.050(5) 0.024(4) 0.024(4) 0.013(4) C21 0.049(6) 0.036(5) 0.044(5) 0.014(4) 0.024(4) 0.014(4) C22 0.052(6) 0.033(5) 0.039(5) 0.012(4) 0.020(4) 0.005(4) C23 0.031(5) 0.034(5) 0.040(5) 0.017(4) 0.012(4) 0.010(4) C24 0.034(5) 0.027(4) 0.033(5) 0.007(4) 0.014(4) 0.005(4) C25 0.045(5) 0.043(5) 0.043(5) 0.026(4) 0.023(4) 0.022(4) C26 0.041(5) 0.036(5) 0.045(5) 0.023(4) 0.023(4) 0.020(4) C27 0.055(6) 0.072(7) 0.065(6) 0.048(6) 0.032(5) 0.024(5) C28 0.038(5) 0.034(5) 0.052(5) 0.025(4) 0.015(4) 0.012(4) C29 0.036(5) 0.041(5) 0.056(6) 0.027(5) 0.014(4) 0.016(4) C30 0.058(7) 0.038(5) 0.067(6) 0.026(5) 0.010(6) 0.017(5) C31 0.045(6) 0.052(6) 0.086(8) 0.046(6) 0.005(6) 0.009(5) C32 0.051(6) 0.052(6) 0.079(7) 0.050(6) 0.027(5) 0.010(5) C33 0.038(5) 0.036(5) 0.065(6) 0.035(5) 0.021(5) 0.014(4) N9 0.095(8) 0.048(6) 0.054(5) 0.028(4) 0.030(5) 0.014(6) O5 0.054(5) 0.089(6) 0.088(5) 0.052(5) 0.020(4) 0.018(4) O6 0.078(5) 0.052(4) 0.074(5) 0.028(4) 0.036(4) 0.006(4) O7 0.148(8) 0.051(5) 0.099(6) 0.019(4) 0.063(6) 0.039(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 O1 1.772(5) . ? Fe1 O4 1.958(5) . ? Fe1 O2 1.978(5) . ? Fe1 N4 2.074(6) . ? Fe1 N1 2.201(6) . ? Fe2 O1 1.810(5) . ? Fe2 O4 2.026(5) 2_566 ? Fe2 O3 2.085(5) . ? Fe2 N6 2.089(6) 2_566 ? Fe2 N8 2.101(7) 2_566 ? Fe2 N2 2.322(6) 2_566 ? O2 C2 1.262(9) . ? O3 C2 1.259(9) . ? O4 C4 1.434(9) . ? O4 Fe2 2.026(5) 2_566 ? N1 C6 1.470(10) . ? N1 C7 1.475(10) . ? N1 C5 1.487(10) . ? N2 C3 1.473(10) . ? N2 C16 1.478(9) . ? N2 C25 1.485(10) . ? N2 Fe2 2.322(6) 2_566 ? N3 C8 1.343(10) . ? N3 C10 1.393(10) . ? N3 C9 1.459(10) . ? N4 C8 1.336(10) . ? N4 C15 1.413(9) . ? N5 C17 1.334(9) . ? N5 C19 1.380(10) . ? N5 C18 1.456(10) . ? N6 C17 1.335(10) . ? N6 C24 1.398(9) . ? N6 Fe2 2.089(6) 2_566 ? N7 C26 1.342(10) . ? N7 C33 1.405(11) . ? N7 C27 1.466(11) . ? N8 C26 1.333(10) . ? N8 C28 1.390(10) . ? N8 Fe2 2.101(7) 2_566 ? C1 C2 1.497(10) . ? C3 C4 1.531(11) . ? C4 C5 1.532(11) . ? C7 C8 1.482(11) . ? C10 C15 1.382(11) . ? C10 C11 1.393(11) . ? C11 C12 1.383(11) . ? C12 C13 1.394(11) . ? C13 C14 1.385(11) . ? C14 C15 1.408(11) . ? C16 C17 1.492(10) . ? C19 C20 1.386(11) . ? C19 C24 1.406(11) . ? C20 C21 1.387(12) . ? C21 C22 1.403(12) . ? C22 C23 1.368(11) . ? C23 C24 1.382(11) . ? C25 C26 1.490(11) . ? C28 C29 1.392(12) . ? C28 C33 1.409(12) . ? C29 C30 1.364(13) . ? C30 C31 1.401(14) . ? C31 C32 1.364(14) . ? C32 C33 1.376(12) . ? N9 O5 1.239(11) . ? N9 O7 1.248(10) . ? N9 O6 1.279(10) . ? N10 O9 1.20(2) . ? N10 O8 1.22(2) . ? N10 O10 1.32(2) . ? O9 O10 1.34(3) 2_667 ? O10 O9 1.34(3) 2_667 ? O2W O11W 1.28(3) . ? O3W O7W 1.04(3) . ? O3W O10W 1.72(5) . ? O4W O8W 1.10(2) . ? O4W O10W 1.39(3) . ? O5W O9W 1.46(3) . ? O5W O11W 1.82(3) . ? O6W O9W 1.29(3) . ? O6W O8W 1.74(3) . ? O7W O10W 0.90(3) . ? 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 O4 113.9(2) . . ? O1 Fe1 O2 104.1(2) . . ? O4 Fe1 O2 90.9(2) . . ? O1 Fe1 N4 112.4(2) . . ? O4 Fe1 N4 131.4(2) . . ? O2 Fe1 N4 91.6(2) . . ? O1 Fe1 N1 103.8(2) . . ? O4 Fe1 N1 77.8(2) . . ? O2 Fe1 N1 152.1(2) . . ? N4 Fe1 N1 77.8(2) . . ? O1 Fe2 O4 106.9(2) . 2_566 ? O1 Fe2 O3 96.4(2) . . ? O4 Fe2 O3 84.4(2) 2_566 . ? O1 Fe2 N6 106.0(2) . 2_566 ? O4 Fe2 N6 88.4(2) 2_566 2_566 ? O3 Fe2 N6 157.6(2) . 2_566 ? O1 Fe2 N8 100.3(2) . 2_566 ? O4 Fe2 N8 152.3(2) 2_566 2_566 ? O3 Fe2 N8 87.5(2) . 2_566 ? N6 Fe2 N8 89.0(2) 2_566 2_566 ? O1 Fe2 N2 172.7(2) . 2_566 ? O4 Fe2 N2 79.4(2) 2_566 2_566 ? O3 Fe2 N2 80.3(2) . 2_566 ? N6 Fe2 N2 77.5(2) 2_566 2_566 ? N8 Fe2 N2 73.1(2) 2_566 2_566 ? Fe1 O1 Fe2 128.4(3) . . ? C2 O2 Fe1 128.7(5) . . ? C2 O3 Fe2 135.0(5) . . ? C4 O4 Fe1 118.9(5) . . ? C4 O4 Fe2 115.7(4) . 2_566 ? Fe1 O4 Fe2 124.9(2) . 2_566 ? C6 N1 C7 110.4(6) . . ? C6 N1 C5 111.8(6) . . ? C7 N1 C5 108.6(6) . . ? C6 N1 Fe1 111.0(5) . . ? C7 N1 Fe1 111.9(5) . . ? C5 N1 Fe1 102.9(4) . . ? C3 N2 C16 113.9(6) . . ? C3 N2 C25 113.3(6) . . ? C16 N2 C25 110.4(6) . . ? C3 N2 Fe2 103.5(4) . 2_566 ? C16 N2 Fe2 109.4(4) . 2_566 ? C25 N2 Fe2 105.7(4) . 2_566 ? C8 N3 C10 106.7(6) . . ? C8 N3 C9 126.2(6) . . ? C10 N3 C9 126.9(6) . . ? C8 N4 C15 104.2(6) . . ? C8 N4 Fe1 116.4(5) . . ? C15 N4 Fe1 139.2(5) . . ? C17 N5 C19 107.3(6) . . ? C17 N5 C18 127.3(6) . . ? C19 N5 C18 125.4(6) . . ? C17 N6 C24 105.1(6) . . ? C17 N6 Fe2 117.6(5) . 2_566 ? C24 N6 Fe2 137.3(5) . 2_566 ? C26 N7 C33 107.9(7) . . ? C26 N7 C27 127.1(8) . . ? C33 N7 C27 124.6(7) . . ? C26 N8 C28 106.3(7) . . ? C26 N8 Fe2 115.8(5) . 2_566 ? C28 N8 Fe2 136.8(5) . 2_566 ? O3 C2 O2 124.1(7) . . ? O3 C2 C1 117.0(7) . . ? O2 C2 C1 118.9(7) . . ? N2 C3 C4 108.8(6) . . ? O4 C4 C3 110.1(6) . . ? O4 C4 C5 109.4(6) . . ? C3 C4 C5 113.5(7) . . ? N1 C5 C4 111.5(6) . . ? N1 C7 C8 109.2(6) . . ? N4 C8 N3 113.5(7) . . ? N4 C8 C7 120.8(7) . . ? N3 C8 C7 125.5(7) . . ? C15 C10 N3 106.4(6) . . ? C15 C10 C11 123.4(7) . . ? N3 C10 C11 130.2(7) . . ? C12 C11 C10 115.7(8) . . ? C11 C12 C13 121.9(7) . . ? C14 C13 C12 122.1(8) . . ? C13 C14 C15 116.5(7) . . ? C10 C15 C14 120.4(7) . . ? C10 C15 N4 109.2(7) . . ? C14 C15 N4 130.3(7) . . ? N2 C16 C17 111.8(6) . . ? N5 C17 N6 113.2(7) . . ? N5 C17 C16 125.2(7) . . ? N6 C17 C16 121.5(7) . . ? N5 C19 C20 132.3(7) . . ? N5 C19 C24 106.2(6) . . ? C20 C19 C24 121.5(7) . . ? C19 C20 C21 117.2(8) . . ? C20 C21 C22 120.9(8) . . ? C23 C22 C21 121.8(8) . . ? C22 C23 C24 117.9(8) . . ? C23 C24 N6 131.0(7) . . ? C23 C24 C19 120.8(7) . . ? N6 C24 C19 108.2(7) . . ? N2 C25 C26 107.3(6) . . ? N8 C26 N7 112.1(7) . . ? N8 C26 C25 119.7(7) . . ? N7 C26 C25 128.0(7) . . ? C29 C28 N8 130.6(8) . . ? C29 C28 C33 120.4(8) . . ? N8 C28 C33 109.0(7) . . ? C30 C29 C28 117.3(9) . . ? C29 C30 C31 121.3(9) . . ? C32 C31 C30 122.6(9) . . ? C31 C32 C33 116.4(9) . . ? C32 C33 N7 133.2(8) . . ? C32 C33 C28 122.1(9) . . ? N7 C33 C28 104.7(7) . . ? O5 N9 O7 121.1(10) . . ? O5 N9 O6 121.5(9) . . ? O7 N9 O6 117.4(10) . . ? O9 N10 O8 130.4(23) . . ? O9 N10 O10 111.7(21) . . ? O8 N10 O10 112.2(21) . . ? N10 O9 O10 127.8(30) . 2_667 ? N10 O10 O9 106.5(28) . 2_667 ? O7W O3W O10W 25.4(18) . . ? O8W O4W O10W 133.6(25) . . ? O9W O5W O11W 132.0(16) . . ? O9W O6W O8W 119.6(18) . . ? O10W O7W O3W 125.0(37) . . ? O4W O8W O6W 154.6(23) . . ? O6W O9W O5W 167.3(24) . . ? O7W O10W O4W 148.3(35) . . ? O7W O10W O3W 29.6(22) . . ? O4W O10W O3W 158.9(25) . . ? O2W O11W O5W 150.5(24) . . ? _refine_diff_density_max 0.893 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.100 data_sa08 #Compound 2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ; [Fe~8~(\m-O)~4~(\m-BMDP)~4~(OH)~4~(OAc)~4~]{BF~4~]~3~[OH]^.^2CH~3~CN^.^8H~2~O ; _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C136 H179 B3 F12 Fe8 N34 O29' _chemical_formula_weight 3461.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4(1)/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 38.555(3) _cell_length_b 38.555(3) _cell_length_c 11.865(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17637.2(24) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 21.0 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7184 _exptl_absorpt_coefficient_mu 5.83 _exptl_absorpt_correction_type XABS2 _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.91 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens rotating anode' _diffrn_radiation_monochromator 'nickel filter' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method 2\q-\w _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0 _diffrn_reflns_number 5803 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 54.29 _reflns_number_total 5354 _reflns_number_observed 3129 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL 5.03, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXTL 5.03, XCIF (Sheldrick, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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. No disorder was present in the cation portion of the molecule. For charge balance there should be four anions per formula unit. Of these, there were three BF~4~ groups and one hydroxide. These are: {B1, F1, F2, F3, F4} at 0.5 occupancy; {B2, F5, F6, F7, F8} at 0.25 occupancy with the site shared by O10 at 0.25 occupancy; O6 and O9 at 0.5 occupancy; O7, O8, O11, O12 at 0.25 occupancy. There is also a molecule of acetonitrile at 0.5 occupancy. Hydrogen atoms for these disordered atoms were not assigned. All ordered non- hydrogen atoms were assigned anisotropic thermal ellipsoids, as well as atoms of the acetonitrile molecule. The two BF~4~ groups were refined with distance constraints. The high R values apparently stem from the degree of disorder present and the lack of high angle scattering. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2390P)^2^+243.4101P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5354 _refine_ls_number_parameters 530 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1759 _refine_ls_R_factor_obs 0.1175 _refine_ls_wR_factor_all 0.3837 _refine_ls_wR_factor_obs 0.3240 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.135 _refine_ls_shift/esd_max 0.154 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.45121(5) 0.33434(5) 0.3356(2) 0.0438(7) Uani 1 d . . Fe2 Fe 0.37014(5) 0.27366(5) 0.3083(2) 0.0454(7) Uani 1 d . . O1 O 0.4952(2) 0.3609(2) 0.3169(7) 0.042(2) Uani 1 d . . O2 O 0.4402(2) 0.3506(2) 0.4797(7) 0.050(2) Uani 1 d . . O3 O 0.3845(2) 0.2480(3) 0.1867(8) 0.054(3) Uani 1 d . . O4 O 0.4115(2) 0.3035(2) 0.3214(6) 0.030(2) Uani 1 d . . O5 O 0.4775(2) 0.2923(2) 0.3827(8) 0.044(2) Uani 1 d . . N1 N 0.3472(3) 0.3005(3) 0.4629(10) 0.048(3) Uani 1 d . . N2 N 0.2739(3) 0.2365(3) 0.4115(12) 0.060(3) Uani 1 d . . N3 N 0.3211(3) 0.2516(3) 0.3156(11) 0.053(3) Uani 1 d . . N4 N 0.3218(3) 0.3696(3) 0.2652(12) 0.055(3) Uani 1 d . . N5 N 0.3471(3) 0.3180(3) 0.2423(11) 0.051(3) Uani 1 d . . N6 N 0.4638(3) 0.3194(3) 0.1553(10) 0.050(3) Uani 1 d . . N7 N 0.4082(3) 0.3946(3) 0.0795(11) 0.060(3) Uani 1 d . . N8 N 0.4245(3) 0.3719(3) 0.2444(10) 0.045(3) Uani 1 d . . C1 C 0.3134(4) 0.2843(4) 0.4925(13) 0.058(4) Uani 1 d . . H1A H 0.2959(4) 0.3021(4) 0.4920(13) 0.050 Uiso 1 d R . H1B H 0.3146(4) 0.2747(4) 0.5670(13) 0.050 Uiso 1 d R . C2 C 0.3035(4) 0.2566(4) 0.4097(13) 0.055(4) Uani 1 d . . C3 C 0.2497(4) 0.2350(5) 0.5119(15) 0.080(6) Uani 1 d . . H3A H 0.2308(4) 0.2194(5) 0.4967(15) 0.050 Uiso 1 d R . H3B H 0.2623(4) 0.2270(5) 0.5765(15) 0.050 Uiso 1 d R . H3C H 0.2407(4) 0.2578(5) 0.5267(15) 0.050 Uiso 1 d R . C4 C 0.2732(4) 0.2176(4) 0.3151(14) 0.057(4) Uani 1 d . . C5 C 0.2490(4) 0.1928(4) 0.2747(19) 0.072(5) Uani 1 d . . H5A H 0.2285(4) 0.1863(4) 0.3154(19) 0.050 Uiso 1 d R . C6 C 0.2564(4) 0.1781(4) 0.1740(17) 0.072(5) Uani 1 d . . H6A H 0.2400(4) 0.1615(4) 0.1458(17) 0.050 Uiso 1 d R . C7 C 0.2846(4) 0.1879(4) 0.1128(15) 0.068(4) Uani 1 d . . H7A H 0.2876(4) 0.1764(4) 0.0418(15) 0.050 Uiso 1 d R . C8 C 0.3091(4) 0.2117(4) 0.1499(13) 0.059(4) Uani 1 d . . H8A H 0.3286(4) 0.2188(4) 0.1052(13) 0.050 Uiso 1 d R . C9 C 0.3027(3) 0.2260(4) 0.2526(14) 0.054(4) Uani 1 d . . C10 C 0.3439(4) 0.3381(3) 0.4349(13) 0.053(4) Uani 1 d . . H10A H 0.3650(4) 0.3497(3) 0.4545(13) 0.050 Uiso 1 d R . H10B H 0.3252(4) 0.3479(3) 0.4780(13) 0.050 Uiso 1 d R . C11 C 0.3366(3) 0.3420(4) 0.3151(13) 0.050(4) Uani 1 d . . C12 C 0.3058(4) 0.3997(4) 0.3190(14) 0.065(4) Uani 1 d . . H12A H 0.2963(4) 0.4159(4) 0.2658(14) 0.050 Uiso 1 d R . H12B H 0.2878(4) 0.3919(4) 0.3688(14) 0.050 Uiso 1 d R . H12C H 0.3238(4) 0.4108(4) 0.3620(14) 0.050 Uiso 1 d R . C13 C 0.3222(4) 0.3632(4) 0.1468(15) 0.064(4) Uani 1 d . . C14 C 0.3097(4) 0.3818(4) 0.0562(16) 0.067(4) Uani 1 d . . H14A H 0.2980(4) 0.4036(4) 0.0656(16) 0.050 Uiso 1 d R . C15 C 0.3279(4) 0.3363(5) -0.0600(15) 0.072(5) Uani 1 d . . H15A H 0.3306(4) 0.3272(5) -0.1348(15) 0.050 Uiso 1 d R . C16 C 0.3129(5) 0.3672(5) -0.0487(19) 0.085(6) Uani 1 d . . H16A H 0.3054(5) 0.3809(5) -0.1118(19) 0.050 Uiso 1 d R . C17 C 0.3411(4) 0.3166(4) 0.0298(13) 0.060(4) Uani 1 d . . H17A H 0.3509(4) 0.2939(4) 0.0216(13) 0.050 Uiso 1 d R . C18 C 0.3377(3) 0.3307(4) 0.1331(15) 0.055(4) Uani 1 d . . C19 C 0.3733(3) 0.2933(3) 0.5507(12) 0.051(4) Uani 1 d . . H19A H 0.3631(3) 0.2975(3) 0.6232(12) 0.050 Uiso 1 d R . H19B H 0.3931(3) 0.3082(3) 0.5428(12) 0.050 Uiso 1 d R . C20 C 0.3846(3) 0.2553(3) 0.5477(11) 0.046(3) Uani 1 d . . H20A H 0.3667(3) 0.2414(3) 0.5811(11) 0.050 Uiso 1 d R . C21 C 0.4998(3) 0.3325(4) 0.1387(12) 0.054(4) Uani 1 d . . H21A H 0.5043(3) 0.3365(4) 0.0602(12) 0.050 Uiso 1 d R . H21B H 0.5157(3) 0.3152(4) 0.1656(12) 0.050 Uiso 1 d R . C22 C 0.4629(4) 0.2822(4) 0.1280(14) 0.067(4) Uani 1 d . . H22A H 0.4687(4) 0.2781(4) 0.0505(14) 0.050 Uiso 1 d R . H22B H 0.4785(4) 0.2695(4) 0.1756(14) 0.050 Uiso 1 d R . H22C H 0.4395(4) 0.2747(4) 0.1419(14) 0.050 Uiso 1 d R . C23 C 0.4392(4) 0.3379(4) 0.0759(12) 0.064(4) Uani 1 d . . H23A H 0.4509(4) 0.3451(4) 0.0082(12) 0.050 Uiso 1 d R . H23B H 0.4211(4) 0.3220(4) 0.0563(12) 0.050 Uiso 1 d R . C24 C 0.4246(3) 0.3687(4) 0.1313(14) 0.058(4) Uani 1 d . . C25 C 0.4036(5) 0.3985(5) -0.0444(13) 0.083(5) Uani 1 d . . H25A H 0.3905(5) 0.4193(5) -0.0580(13) 0.050 Uiso 1 d R . H25B H 0.4257(5) 0.4002(5) -0.0816(13) 0.050 Uiso 1 d R . H25C H 0.3911(5) 0.3789(5) -0.0731(13) 0.050 Uiso 1 d R . C26 C 0.3972(4) 0.4168(4) 0.1629(16) 0.062(4) Uani 1 d . . C27 C 0.3797(5) 0.4480(5) 0.1537(21) 0.085(6) Uani 1 d . . H27A H 0.3725(5) 0.4585(5) 0.0841(21) 0.050 Uiso 1 d R . C28 C 0.3725(4) 0.4634(5) 0.2498(24) 0.089(7) Uani 1 d . . H28A H 0.3610(4) 0.4855(5) 0.2469(24) 0.050 Uiso 1 d R . C29 C 0.3821(4) 0.4504(4) 0.3558(20) 0.083(6) Uani 1 d . . H29A H 0.3748(4) 0.4638(4) 0.4198(20) 0.050 Uiso 1 d R . C30 C 0.4004(4) 0.4186(4) 0.3651(15) 0.063(4) Uani 1 d . . H30A H 0.4072(4) 0.4098(4) 0.4374(15) 0.050 Uiso 1 d R . C31 C 0.4075(4) 0.4021(4) 0.2652(14) 0.056(4) Uani 1 d . . C32 C 0.4611(6) 0.3559(5) 0.5716(23) 0.111(8) Uani 1 d . . C33 C 0.4496(3) 0.3542(4) 0.6804(10) 0.045(3) Uani 1 d . . H33A H 0.4674(3) 0.3582(4) 0.7353(10) 0.050 Uiso 1 d R . H33B H 0.4319(3) 0.3716(4) 0.6875(10) 0.050 Uiso 1 d R . H33C H 0.4396(3) 0.3317(4) 0.6925(10) 0.050 Uiso 1 d R . N9 N 0.3742(9) 0.3773(10) 0.6858(25) 0.090(10) Uani 0.50 d P . C34 C 0.3398(8) 0.4345(8) 0.6641(32) 0.073(10) Uani 0.50 d P . C35 C 0.3590(9) 0.4028(11) 0.6759(26) 0.064(10) Uani 0.50 d P . O6 O 0.2534(7) 0.2986(7) -0.2804(24) 0.100(8) Uiso 0.50 d P . O7 O 0.4407(13) 0.1555(13) -0.0811(47) 0.100(16) Uiso 0.25 d P . O8 O 0.4049(10) 0.2524(10) -0.0838(36) 0.066(11) Uiso 0.25 d P . O9 O 0.3705(6) 0.2422(6) -0.1203(23) 0.092(7) Uiso 0.50 d P . O11 O 0.2567(20) 0.4685(20) 0.1377(69) 0.147(26) Uiso 0.25 d P 1 O12 O 0.2435(11) 0.4514(11) 0.1704(36) 0.063(11) Uiso 0.25 d P 2 B1 B 0.3632(5) 0.5067(5) 0.8748(17) 0.056(9) Uiso 0.50 d PD . F1 F 0.3492(4) 0.5115(4) 0.9761(14) 0.078(5) Uiso 0.50 d PD . F2 F 0.3384(5) 0.5123(5) 0.7978(17) 0.110(7) Uiso 0.50 d PD . F3 F 0.3760(4) 0.4753(4) 0.8688(16) 0.086(6) Uiso 0.50 d PD . F4 F 0.3884(5) 0.5291(6) 0.8573(20) 0.138(9) Uiso 0.50 d PD . B2 B 0.3220(7) 0.2439(7) -0.2078(23) 0.007(9) Uiso 0.25 d PD 1 F5 F 0.3119(9) 0.2238(9) -0.2931(26) 0.096(12) Uiso 0.25 d PD 1 F6 F 0.3194(9) 0.2265(9) -0.1108(24) 0.092(12) Uiso 0.25 d PD 1 F7 F 0.3007(10) 0.2714(8) -0.2065(37) 0.126(16) Uiso 0.25 d PD 1 F8 F 0.3543(7) 0.2553(10) -0.2174(36) 0.124(16) Uiso 0.25 d PD 1 O10 O 0.3086(9) 0.2437(8) -0.2441(31) 0.040(8) Uiso 0.25 d P 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 0.0436(12) 0.0433(12) 0.0443(14) 0.0012(10) -0.0005(10) -0.0006(9) Fe2 0.0375(12) 0.0520(13) 0.0467(14) 0.0014(11) 0.0018(10) -0.0002(9) O1 0.048(5) 0.039(5) 0.040(6) 0.002(4) -0.001(4) -0.008(4) O2 0.052(5) 0.066(6) 0.030(5) -0.006(5) -0.008(4) -0.006(5) O3 0.043(5) 0.069(6) 0.052(6) -0.025(5) -0.001(5) -0.012(5) O4 0.017(4) 0.039(4) 0.033(5) -0.001(4) -0.004(3) -0.009(3) O5 0.033(4) 0.033(4) 0.066(6) 0.006(4) 0.000(4) 0.004(3) N1 0.039(6) 0.051(7) 0.054(8) -0.002(6) -0.004(6) 0.004(5) N2 0.041(7) 0.060(7) 0.079(10) 0.017(7) 0.012(6) 0.003(6) N3 0.034(6) 0.055(7) 0.069(9) 0.014(6) -0.001(6) -0.006(5) N4 0.037(6) 0.051(7) 0.078(10) 0.006(7) -0.004(6) 0.005(5) N5 0.034(6) 0.054(7) 0.064(8) 0.005(7) 0.000(6) 0.007(5) N6 0.050(6) 0.056(7) 0.044(7) -0.009(6) 0.002(6) -0.009(5) N7 0.051(7) 0.070(8) 0.060(9) 0.024(7) -0.013(7) -0.004(6) N8 0.045(6) 0.048(7) 0.040(7) 0.000(5) -0.001(5) 0.001(5) C1 0.058(9) 0.072(10) 0.044(9) 0.003(8) 0.021(7) 0.012(8) C2 0.057(9) 0.047(8) 0.060(11) 0.014(8) 0.010(8) 0.017(7) C3 0.046(8) 0.097(13) 0.098(14) 0.038(11) 0.025(9) 0.008(9) C4 0.052(9) 0.055(9) 0.064(11) -0.002(8) -0.006(8) 0.021(8) C5 0.035(8) 0.062(10) 0.119(17) 0.025(11) -0.014(10) -0.007(7) C6 0.062(11) 0.063(10) 0.091(15) 0.009(11) -0.033(11) -0.008(8) C7 0.062(10) 0.074(10) 0.067(12) -0.022(9) -0.009(9) -0.009(9) C8 0.060(9) 0.071(10) 0.046(10) 0.004(8) -0.004(8) -0.012(8) C9 0.024(7) 0.067(9) 0.072(11) 0.014(9) 0.004(7) -0.013(7) C10 0.044(8) 0.045(8) 0.070(11) 0.001(8) 0.011(7) 0.010(6) C11 0.037(7) 0.049(8) 0.063(11) 0.004(8) -0.004(7) 0.006(6) C12 0.063(9) 0.054(9) 0.077(12) -0.003(8) -0.007(9) 0.000(8) C13 0.044(8) 0.074(11) 0.073(12) 0.018(10) 0.006(8) -0.007(8) C14 0.055(9) 0.065(10) 0.080(13) 0.017(10) -0.014(9) 0.004(8) C15 0.075(11) 0.081(12) 0.062(12) 0.021(10) -0.021(9) 0.001(10) C16 0.073(12) 0.099(15) 0.084(15) 0.018(12) -0.024(11) -0.004(11) C17 0.047(8) 0.074(10) 0.059(11) 0.001(9) -0.004(8) -0.012(7) C18 0.039(8) 0.053(9) 0.074(12) 0.000(9) -0.003(8) -0.007(7) C19 0.051(8) 0.053(8) 0.050(9) -0.004(7) 0.006(7) 0.009(7) C20 0.041(7) 0.057(8) 0.040(8) -0.006(7) -0.010(6) -0.001(6) C21 0.052(8) 0.067(9) 0.044(9) -0.006(8) 0.010(7) 0.006(7) C22 0.065(10) 0.071(10) 0.065(11) -0.014(9) 0.009(9) -0.018(8) C23 0.070(10) 0.089(12) 0.033(9) -0.009(8) -0.008(8) -0.013(9) C24 0.038(8) 0.066(10) 0.070(12) 0.001(9) -0.006(8) -0.007(7) C25 0.077(11) 0.122(15) 0.049(11) 0.028(11) -0.014(9) -0.003(11) C26 0.039(8) 0.053(9) 0.093(14) 0.013(10) -0.010(9) -0.005(7) C27 0.091(14) 0.062(12) 0.101(17) 0.021(12) -0.012(12) 0.004(10) C28 0.057(10) 0.052(10) 0.159(23) 0.017(14) -0.034(13) 0.002(8) C29 0.068(11) 0.058(10) 0.122(18) -0.035(12) -0.001(12) -0.004(9) C30 0.058(9) 0.050(9) 0.082(13) -0.012(9) -0.011(9) 0.012(7) C31 0.048(8) 0.048(8) 0.072(12) -0.003(9) -0.006(8) -0.004(7) C32 0.118(18) 0.059(11) 0.156(25) 0.042(14) 0.029(17) 0.024(11) C33 0.042(7) 0.073(9) 0.021(7) 0.002(7) 0.004(6) -0.008(7) N9 0.095(24) 0.135(30) 0.041(18) -0.041(20) -0.007(17) -0.012(22) C34 0.055(18) 0.066(21) 0.099(29) -0.027(20) 0.015(19) -0.025(16) C35 0.060(21) 0.104(29) 0.027(17) -0.026(20) 0.010(16) -0.031(20) _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 1.870(9) . ? Fe1 O4 1.947(7) . ? Fe1 O5 1.991(7) . ? Fe1 O1 1.992(8) . ? Fe1 N8 2.082(11) . ? Fe1 N6 2.268(11) . ? Fe2 O3 1.836(9) . ? Fe2 O4 1.971(7) . ? Fe2 O1 1.984(8) 16_656 ? Fe2 N3 2.075(10) . ? Fe2 N5 2.080(11) . ? Fe2 N1 2.286(11) . ? O1 C20 1.426(15) 11_666 ? O1 Fe2 1.984(8) 11_666 ? O2 C32 1.37(3) . ? O3 C32 1.47(2) 16_656 ? N1 C19 1.48(2) . ? N1 C1 1.49(2) . ? N1 C10 1.49(2) . ? N2 C4 1.36(2) . ? N2 C2 1.38(2) . ? N2 C3 1.51(2) . ? N3 C2 1.32(2) . ? N3 C9 1.43(2) . ? N4 C11 1.34(2) . ? N4 C13 1.43(2) . ? N4 C12 1.46(2) . ? N5 C11 1.33(2) . ? N5 C18 1.43(2) . ? N6 C22 1.47(2) . ? N6 C21 1.49(2) . ? N6 C23 1.51(2) . ? N7 C24 1.33(2) . ? N7 C26 1.37(2) . ? N7 C25 1.49(2) . ? N8 C24 1.35(2) . ? N8 C31 1.36(2) . ? C1 C2 1.50(2) . ? C4 C9 1.39(2) . ? C4 C5 1.42(2) . ? C5 C6 1.35(2) . ? C6 C7 1.36(2) . ? C7 C8 1.39(2) . ? C8 C9 1.36(2) . ? C10 C11 1.46(2) . ? C13 C14 1.38(2) . ? C13 C18 1.40(2) . ? C14 C16 1.37(2) . ? C15 C16 1.33(2) . ? C15 C17 1.40(2) . ? C17 C18 1.35(2) . ? C19 C20 1.53(2) . ? C20 O1 1.425(15) 16_656 ? C20 C21 1.49(2) 16_656 ? C21 C20 1.49(2) 11_666 ? C23 C24 1.47(2) . ? C26 C27 1.38(2) . ? C26 C31 1.40(2) . ? C27 C28 1.31(3) . ? C28 C29 1.40(3) . ? C29 C30 1.42(2) . ? C30 C31 1.37(2) . ? C32 C33 1.37(3) . ? C32 O3 1.47(2) 11_666 ? N9 C35 1.15(5) . ? C34 C35 1.44(5) . ? O8 O9 1.45(4) . ? O9 F8 1.40(4) . ? B1 F3 1.31(2) . ? B1 F4 1.32(2) . ? B1 F1 1.33(2) . ? B1 F2 1.34(2) . ? B2 F8 1.32(2) . ? B2 F5 1.33(2) . ? B2 F6 1.34(2) . ? B2 F7 1.34(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O4 96.1(4) . . ? O2 Fe1 O5 97.6(4) . . ? O4 Fe1 O5 85.9(3) . . ? O2 Fe1 O1 97.0(4) . . ? O4 Fe1 O1 166.8(3) . . ? O5 Fe1 O1 90.9(3) . . ? O2 Fe1 N8 97.4(4) . . ? O4 Fe1 N8 89.4(4) . . ? O5 Fe1 N8 164.7(4) . . ? O1 Fe1 N8 90.3(4) . . ? O2 Fe1 N6 174.9(4) . . ? O4 Fe1 N6 86.1(3) . . ? O5 Fe1 N6 87.1(4) . . ? O1 Fe1 N6 81.0(4) . . ? N8 Fe1 N6 78.0(4) . . ? O3 Fe2 O4 97.6(3) . . ? O3 Fe2 O1 100.1(4) . 16_656 ? O4 Fe2 O1 88.0(3) . 16_656 ? O3 Fe2 N3 95.0(4) . . ? O4 Fe2 N3 166.4(4) . . ? O1 Fe2 N3 94.5(4) 16_656 . ? O3 Fe2 N5 106.1(5) . . ? O4 Fe2 N5 84.0(4) . . ? O1 Fe2 N5 153.3(4) 16_656 . ? N3 Fe2 N5 87.9(4) . . ? O3 Fe2 N1 173.0(4) . . ? O4 Fe2 N1 89.2(3) . . ? O1 Fe2 N1 78.2(4) 16_656 . ? N3 Fe2 N1 78.4(4) . . ? N5 Fe2 N1 76.3(4) . . ? C20 O1 Fe2 121.0(7) 11_666 11_666 ? C20 O1 Fe1 113.8(7) 11_666 . ? Fe2 O1 Fe1 125.3(4) 11_666 . ? C32 O2 Fe1 130.1(11) . . ? C32 O3 Fe2 130.5(12) 16_656 . ? Fe1 O4 Fe2 178.0(4) . . ? C19 N1 C1 110.7(11) . . ? C19 N1 C10 113.5(10) . . ? C1 N1 C10 112.7(10) . . ? C19 N1 Fe2 102.4(7) . . ? C1 N1 Fe2 109.8(8) . . ? C10 N1 Fe2 107.1(8) . . ? C4 N2 C2 107.6(12) . . ? C4 N2 C3 129.3(13) . . ? C2 N2 C3 122.9(14) . . ? C2 N3 C9 106.8(11) . . ? C2 N3 Fe2 116.3(10) . . ? C9 N3 Fe2 135.5(10) . . ? C11 N4 C13 107.0(12) . . ? C11 N4 C12 128.0(14) . . ? C13 N4 C12 124.9(13) . . ? C11 N5 C18 105.9(11) . . ? C11 N5 Fe2 117.3(10) . . ? C18 N5 Fe2 136.8(10) . . ? C22 N6 C21 108.8(11) . . ? C22 N6 C23 107.9(11) . . ? C21 N6 C23 110.0(11) . . ? C22 N6 Fe1 116.7(9) . . ? C21 N6 Fe1 103.8(8) . . ? C23 N6 Fe1 109.5(8) . . ? C24 N7 C26 106.4(13) . . ? C24 N7 C25 125.9(15) . . ? C26 N7 C25 127.8(14) . . ? C24 N8 C31 105.1(12) . . ? C24 N8 Fe1 116.9(9) . . ? C31 N8 Fe1 137.8(10) . . ? N1 C1 C2 111.5(11) . . ? N3 C2 N2 110.9(13) . . ? N3 C2 C1 121.8(13) . . ? N2 C2 C1 126.8(13) . . ? N2 C4 C9 108.0(13) . . ? N2 C4 C5 131.2(16) . . ? C9 C4 C5 120.8(16) . . ? C6 C5 C4 116.1(16) . . ? C5 C6 C7 121.7(16) . . ? C6 C7 C8 123.9(17) . . ? C9 C8 C7 115.3(15) . . ? C8 C9 C4 122.1(14) . . ? C8 C9 N3 131.3(12) . . ? C4 C9 N3 106.6(14) . . ? C11 C10 N1 109.7(12) . . ? N5 C11 N4 113.2(13) . . ? N5 C11 C10 120.2(12) . . ? N4 C11 C10 126.5(13) . . ? C14 C13 C18 121.7(17) . . ? C14 C13 N4 132.3(16) . . ? C18 C13 N4 105.9(14) . . ? C13 C14 C16 117.5(17) . . ? C16 C15 C17 124.3(19) . . ? C15 C16 C14 119.9(18) . . ? C18 C17 C15 116.1(16) . . ? C17 C18 C13 120.5(16) . . ? C17 C18 N5 131.4(14) . . ? C13 C18 N5 108.0(14) . . ? N1 C19 C20 111.0(11) . . ? O1 C20 C21 109.8(11) 16_656 16_656 ? O1 C20 C19 108.6(11) 16_656 . ? C21 C20 C19 111.4(11) 16_656 . ? N6 C21 C20 110.6(11) . 11_666 ? C24 C23 N6 110.0(12) . . ? N7 C24 N8 112.8(14) . . ? N7 C24 C23 125.6(15) . . ? N8 C24 C23 121.4(14) . . ? N7 C26 C27 129.4(18) . . ? N7 C26 C31 106.6(12) . . ? C27 C26 C31 124.0(18) . . ? C28 C27 C26 115.3(19) . . ? C27 C28 C29 124.1(17) . . ? C28 C29 C30 120.7(18) . . ? C31 C30 C29 115.7(17) . . ? N8 C31 C30 130.6(15) . . ? N8 C31 C26 109.1(14) . . ? C30 C31 C26 120.3(14) . . ? C33 C32 O2 123.7(18) . . ? C33 C32 O3 112.9(21) . 11_666 ? O2 C32 O3 123.4(18) . 11_666 ? N9 C35 C34 179.4(35) . . ? F8 O9 O8 123.7(27) . . ? F3 B1 F4 108.6(16) . . ? F3 B1 F1 109.3(16) . . ? F4 B1 F1 110.5(16) . . ? F3 B1 F2 112.4(16) . . ? F4 B1 F2 108.3(16) . . ? F1 B1 F2 107.8(15) . . ? F8 B2 F5 113.7(22) . . ? F8 B2 F6 108.1(21) . . ? F5 B2 F6 109.9(21) . . ? F8 B2 F7 108.4(21) . . ? F5 B2 F7 106.7(21) . . ? F6 B2 F7 110.0(21) . . ? B2 F8 O9 103.2(26) . . ? _refine_diff_density_max 1.413 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.147