# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author ; Danielle L. Gray University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_email dgray@illinois.edu _publ_contact_author_fax '1 217 244 8068' _publ_contact_author_phone '1 217 244 1708' _publ_contact_letter ; Please consider this CIF submission for publication as a structural paper in Acta Crystallographica E. ; _publ_requested_category FM _publ_requested_coeditor_name ? _publ_section_title ; ? ; loop_ _publ_author_name M.Olsen D.Gray T.Rauchfuss 'L.De Gioia' G.Zampella data_o _database_code_depnum_ccdc_archive 'CCDC 812366' #TrackingRef 'SMeFe2.cif' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H84 B2 Cl6 F48 Fe4 O8 P4 S6' _chemical_formula_structural ? _chemical_formula_weight 3039.58 _chemical_absolute_configuration ? _chemical_formula_iupac ? _chemical_formula_analytical ? _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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.3263(15) _cell_length_b 18.5078(16) _cell_length_c 20.1683(18) _cell_angle_alpha 105.661(5) _cell_angle_beta 91.642(5) _cell_angle_gamma 99.204(5) _cell_volume 6129.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 24.70 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.639 _exptl_crystal_size_mid 0.256 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3044 _exptl_crystal_id sba26masq _exptl_crystal_preparation ; The data crystal was mounted using ??oil (Parantone-N, Exxon) to a ??0.3 mm cryo-loop (Hampton Research)?? ??0.2 mm Kapton micromount (Thorne, 2003)?? with the (??) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 0.9322 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; ??All crystals examined exhibited non-merohedral twinning (which roughly superimposed the a- and b-axes and inverted the c-axis). ??One??Two? distinct cell??s? was??were? identified using SMART/APEX2 (Bruker, 2001/4) and Cell_Now (Sheldrick, 2004). ??Six?Five?Four? frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2005) then corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SAINT/SADABS??/TWINABS? (Bruker, 2005) to sort, merge, and scale the combined data. Combined unit cell parameters were determined from both??all? components using SAINT (Bruker, 2005). The twin law by rows was (0 1 0), (1 0 0), (.5 .5 -1). Non-overlapping reflections from the primary orientation were used for phasing. Combined data with complete or no overlap were used for refinement. A series of identical frames was collected twice during the experiment to monitor decay. No decay correction was applied.?? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id sba26masq _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 146429 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.43 _reflns_number_total 22515 _reflns_number_gt 16588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.0-1 (Bruker, 2004)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics ; SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) ; _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by direct??dual space??Paterson methods (Sheldrick, 2008). Systematic conditions suggested the un??ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atoms ??; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed ?? dependence on amplitude ??and??or?? resolution. ??esds for MERG 0/HKLF 5 - recommend total minus unique*# of twins?? Since reflections could not be effectively merged, parameter esds were adjusted by increasing the number of extra parameters based on the difference between total observations and unique reflections. ?? ??esds for Hirshfeld test - recommend delta unique from 2T=51.36(d=.82)?? Parameter esds were adjusted by increasing the number of extra parameters based on the change in unique observations beyond 0.82\%A resolution. ?? ??TWINABS tests for racemic twinning (also inverted component)?? Independent parameters refined for each component showed negligible racemic twinning for separate components, so one parameter was refined for the total contribution of the racemate. ?? ??weak data?? For the data crystal, mean I/\s(I) was less than 1 for reflections beyond 1\%A resolution. Reflections between 1 and 0.8\%A resolution were used for least-squares refinement to improve the data-to-variable ratio at the expense of agreement factors. ?? ??Non-ideal crystal volume?? The acicular parent crystals were extremely difficult to cut without damaging the crystal parallel to the a-axis. The data crystal was much longer than ideal; however, the mosaicity of shorter crystals damaged by the cutting process was too broad for data collection. ?? ; _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^)+(0.0652P)^2^+2.8775P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22515 _refine_ls_number_parameters 1960 _refine_ls_number_restraints 5458 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.710 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 _refine_ls_abs_structure_details ? 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_1 Fe 0.61737(4) 0.80243(4) 0.36306(4) 0.03089(18) Uani 1 1 d . A . Fe2_1 Fe 0.70871(4) 0.71323(4) 0.38359(3) 0.02795(17) Uani 1 1 d . A . S1_1 S 0.71997(7) 0.77723(8) 0.30014(6) 0.0337(3) Uani 1 1 d . . . S2_1 S 0.70212(8) 0.83039(7) 0.45678(6) 0.0337(3) Uani 1 1 d . . . S3_1 S 0.84281(7) 0.72189(9) 0.40056(7) 0.0391(3) Uani 1 1 d . . . P1_1 P 0.53945(8) 0.74893(9) 0.26402(7) 0.0384(3) Uani 1 1 d D . . P2_1 P 0.71072(8) 0.66940(9) 0.47847(7) 0.0394(3) Uani 1 1 d D . . O1_1 O 0.6075(3) 0.9542(3) 0.3513(3) 0.0704(14) Uani 1 1 d . A . O2_1 O 0.4834(3) 0.8056(3) 0.4495(2) 0.0607(12) Uani 1 1 d . A . O3_1 O 0.5447(2) 0.6389(2) 0.3699(2) 0.0431(9) Uani 1 1 d . A . O4_1 O 0.7158(3) 0.5658(3) 0.2855(2) 0.0666(13) Uani 1 1 d . A . C1_1 C 0.6126(3) 0.8949(4) 0.3561(3) 0.0467(14) Uani 1 1 d . . . C2_1 C 0.5349(3) 0.8042(3) 0.4164(3) 0.0400(13) Uani 1 1 d . . . C3_1 C 0.5556(4) 0.6570(4) 0.2117(3) 0.0621(19) Uani 1 1 d . A . H3A_1 H 0.5207 0.6411 0.1693 0.093 Uiso 1 1 calc R . . H3B_1 H 0.5446 0.6192 0.2377 0.093 Uiso 1 1 calc R . . H3C_1 H 0.6103 0.6608 0.1997 0.093 Uiso 1 1 calc R . . C4_1 C 0.4358(3) 0.7333(4) 0.2754(3) 0.0465(14) Uani 1 1 d . A . H4A_1 H 0.4065 0.7115 0.2302 0.070 Uiso 1 1 calc R . . H4B_1 H 0.4200 0.7820 0.2983 0.070 Uiso 1 1 calc R . . H4C_1 H 0.4246 0.6981 0.3038 0.070 Uiso 1 1 calc R . . C5_1 C 0.549(2) 0.799(3) 0.198(2) 0.056(7) Uani 0.60(9) 1 d PD A 1 H5A_1 H 0.5078 0.7760 0.1610 0.083 Uiso 0.60(9) 1 calc PR A 1 H5B_1 H 0.6006 0.7967 0.1792 0.083 Uiso 0.60(9) 1 calc PR A 1 H5C_1 H 0.5450 0.8529 0.2186 0.083 Uiso 0.60(9) 1 calc PR A 1 C5B_1 C 0.543(4) 0.818(3) 0.214(3) 0.056(7) Uani 0.40(9) 1 d PD A 2 H5BA_1 H 0.5160 0.7930 0.1684 0.083 Uiso 0.40(9) 1 calc PR A 2 H5BB_1 H 0.5976 0.8381 0.2095 0.083 Uiso 0.40(9) 1 calc PR A 2 H5BC_1 H 0.5166 0.8597 0.2381 0.083 Uiso 0.40(9) 1 calc PR A 2 C6_1 C 0.6032(3) 0.6805(3) 0.3747(3) 0.0349(12) Uani 1 1 d . . . C7_1 C 0.8050(3) 0.8542(4) 0.3245(3) 0.0463(15) Uani 1 1 d . . . H7A_1 H 0.8513 0.8319 0.3331 0.056 Uiso 1 1 calc R . . H7B_1 H 0.8148 0.8750 0.2845 0.056 Uiso 1 1 calc R . . C8_1 C 0.7996(4) 0.9190(3) 0.3862(3) 0.0481(15) Uani 1 1 d . . . H8A_1 H 0.7547 0.9428 0.3770 0.058 Uiso 1 1 calc R . . H8B_1 H 0.8477 0.9577 0.3919 0.058 Uiso 1 1 calc R . . C9_1 C 0.7896(3) 0.8982(3) 0.4537(3) 0.0448(14) Uani 1 1 d . . . H9A_1 H 0.7893 0.9457 0.4909 0.054 Uiso 1 1 calc R . . H9B_1 H 0.8361 0.8771 0.4640 0.054 Uiso 1 1 calc R . . C10_1 C 0.7135(3) 0.6239(3) 0.3234(3) 0.0399(13) Uani 1 1 d . . . C11_1 C 0.8839(4) 0.6810(5) 0.3198(3) 0.0608(18) Uani 1 1 d . . . H11A_1 H 0.9412 0.6933 0.3260 0.091 Uiso 1 1 calc R . . H11B_1 H 0.8652 0.7022 0.2839 0.091 Uiso 1 1 calc R . . H11C_1 H 0.8672 0.6256 0.3059 0.091 Uiso 1 1 calc R . . C12_1 C 0.7809(4) 0.7265(4) 0.5493(3) 0.0496(15) Uani 1 1 d . B . H12A_1 H 0.7753 0.7051 0.5888 0.074 Uiso 1 1 calc R . . H12B_1 H 0.7711 0.7790 0.5629 0.074 Uiso 1 1 calc R . . H12C_1 H 0.8343 0.7261 0.5345 0.074 Uiso 1 1 calc R . . C13_1 C 0.7378(19) 0.5755(7) 0.4598(9) 0.059(4) Uani 0.83(8) 1 d PD B 1 H13A_1 H 0.7349 0.5576 0.5013 0.088 Uiso 0.83(8) 1 calc PR B 1 H13B_1 H 0.7914 0.5782 0.4453 0.088 Uiso 0.83(8) 1 calc PR B 1 H13C_1 H 0.7017 0.5399 0.4227 0.088 Uiso 0.83(8) 1 calc PR B 1 C13B_1 C 0.709(8) 0.5686(16) 0.466(5) 0.059(4) Uani 0.17(8) 1 d PD B 2 H13D_1 H 0.7261 0.5602 0.5101 0.088 Uiso 0.17(8) 1 calc PR B 2 H13E_1 H 0.7448 0.5504 0.4312 0.088 Uiso 0.17(8) 1 calc PR B 2 H13F_1 H 0.6558 0.5406 0.4514 0.088 Uiso 0.17(8) 1 calc PR B 2 C14_1 C 0.6188(10) 0.653(3) 0.5193(14) 0.066(6) Uani 0.70(10) 1 d PDU B 1 H14D_1 H 0.6284 0.6337 0.5590 0.100 Uiso 0.70(10) 1 calc PR B 1 H14E_1 H 0.5801 0.6153 0.4859 0.100 Uiso 0.70(10) 1 calc PR B 1 H14F_1 H 0.5988 0.7008 0.5349 0.100 Uiso 0.70(10) 1 calc PR B 1 C14B_1 C 0.624(2) 0.686(5) 0.526(2) 0.055(10) Uani 0.30(10) 1 d PDU B 2 H14G_1 H 0.6293 0.6733 0.5703 0.083 Uiso 0.30(10) 1 calc PR B 2 H14H_1 H 0.5769 0.6530 0.4989 0.083 Uiso 0.30(10) 1 calc PR B 2 H14I_1 H 0.6179 0.7392 0.5352 0.083 Uiso 0.30(10) 1 calc PR B 2 Fe1_2 Fe 1.21808(4) 0.72748(4) 0.81540(4) 0.03180(18) Uani 1 1 d . . . Fe2_2 Fe 1.17349(4) 0.81098(4) 0.74360(3) 0.03029(18) Uani 1 1 d . . . S1_2 S 1.26741(7) 0.73508(8) 0.71514(6) 0.0369(3) Uani 1 1 d . . . S2_2 S 1.09862(7) 0.70223(7) 0.75793(7) 0.0339(3) Uani 1 1 d . . . S3_2 S 1.13165(8) 0.79364(10) 0.62974(7) 0.0448(4) Uani 1 1 d . . . P1_2 P 1.34037(8) 0.77720(9) 0.86795(7) 0.0393(3) Uani 1 1 d . . . P2_2 P 1.06414(8) 0.86549(8) 0.76412(8) 0.0375(3) Uani 1 1 d . . . O1_2 O 1.1455(3) 0.7440(3) 0.9475(2) 0.0641(13) Uani 1 1 d . . . O2_2 O 1.2458(3) 0.5768(3) 0.8147(3) 0.0811(16) Uani 1 1 d . . . O3_2 O 1.2175(2) 0.8998(2) 0.88649(19) 0.0464(10) Uani 1 1 d . . . O4_2 O 1.2731(3) 0.9465(3) 0.7247(2) 0.0649(13) Uani 1 1 d . . . C1_2 C 1.2337(4) 0.6351(4) 0.8139(3) 0.0520(15) Uani 1 1 d . . . C2_2 C 1.1735(3) 0.7382(3) 0.8964(3) 0.0421(13) Uani 1 1 d . . . C3_2 C 1.3436(4) 0.8134(4) 0.9610(3) 0.0576(18) Uani 1 1 d . . . H3A_2 H 1.3973 0.8380 0.9791 0.086 Uiso 1 1 calc R . . H3B_2 H 1.3270 0.7712 0.9810 0.086 Uiso 1 1 calc R . . H3C_2 H 1.3084 0.8506 0.9734 0.086 Uiso 1 1 calc R . . C4_2 C 1.4073(4) 0.7097(4) 0.8532(4) 0.067(2) Uani 1 1 d . . . H4A_2 H 1.4605 0.7365 0.8706 0.100 Uiso 1 1 calc R . . H4B_2 H 1.4063 0.6849 0.8036 0.100 Uiso 1 1 calc R . . H4C_2 H 1.3913 0.6711 0.8775 0.100 Uiso 1 1 calc R . . C5_2 C 1.3946(3) 0.8549(4) 0.8408(3) 0.0529(16) Uani 1 1 d . . . H5A_2 H 1.4464 0.8712 0.8663 0.079 Uiso 1 1 calc R . . H5B_2 H 1.3660 0.8977 0.8504 0.079 Uiso 1 1 calc R . . H5C_2 H 1.4010 0.8379 0.7912 0.079 Uiso 1 1 calc R . . C6_2 C 1.2023(3) 0.8528(3) 0.8351(3) 0.0350(12) Uani 1 1 d . . . C7_2 C 1.2285(3) 0.6521(4) 0.6433(3) 0.0507(16) Uani 1 1 d . . . H7A_2 H 1.2099 0.6705 0.6050 0.061 Uiso 1 1 calc R . . H7B_2 H 1.2723 0.6251 0.6272 0.061 Uiso 1 1 calc R . . C8_2 C 1.1627(4) 0.5948(4) 0.6564(3) 0.0552(17) Uani 1 1 d . . . H8A_2 H 1.1814 0.5741 0.6931 0.066 Uiso 1 1 calc R . . H8B_2 H 1.1494 0.5520 0.6138 0.066 Uiso 1 1 calc R . . C9_2 C 1.0893(3) 0.6263(3) 0.6775(3) 0.0461(14) Uani 1 1 d . . . H9A_2 H 1.0487 0.5838 0.6816 0.055 Uiso 1 1 calc R . . H9B_2 H 1.0701 0.6456 0.6400 0.055 Uiso 1 1 calc R . . C10_2 C 1.2350(3) 0.8937(4) 0.7314(3) 0.0433(13) Uani 1 1 d . . . C11_2 C 1.2149(4) 0.8152(5) 0.5807(3) 0.0626(19) Uani 1 1 d . . . H11A_2 H 1.1994 0.7951 0.5311 0.094 Uiso 1 1 calc R . . H11B_2 H 1.2583 0.7917 0.5924 0.094 Uiso 1 1 calc R . . H11C_2 H 1.2318 0.8706 0.5921 0.094 Uiso 1 1 calc R . . C12_2 C 0.9753(3) 0.8128(4) 0.7120(4) 0.0521(16) Uani 1 1 d . . . H12A_2 H 0.9321 0.8411 0.7243 0.078 Uiso 1 1 calc R . . H12B_2 H 0.9621 0.7627 0.7204 0.078 Uiso 1 1 calc R . . H12C_2 H 0.9837 0.8062 0.6630 0.078 Uiso 1 1 calc R . . C13_2 C 1.0743(4) 0.9594(4) 0.7511(4) 0.0640(19) Uani 1 1 d . . . H13A_2 H 1.0254 0.9792 0.7607 0.096 Uiso 1 1 calc R . . H13B_2 H 1.0858 0.9564 0.7033 0.096 Uiso 1 1 calc R . . H13C_2 H 1.1173 0.9936 0.7825 0.096 Uiso 1 1 calc R . . C14_2 C 1.0331(4) 0.8780(4) 0.8513(3) 0.0616(18) Uani 1 1 d . . . H14A_2 H 0.9830 0.8963 0.8544 0.092 Uiso 1 1 calc R . . H14B_2 H 1.0727 0.9152 0.8841 0.092 Uiso 1 1 calc R . . H14C_2 H 1.0270 0.8291 0.8625 0.092 Uiso 1 1 calc R . . B200_3 B 0.8169(3) -0.7184(3) 1.6902(3) 0.0241(11) Uani 1 1 d . . . C200_3 C 0.7614(3) -0.6551(3) 1.6889(2) 0.0248(10) Uani 1 1 d . . . C201_3 C 0.7266(3) -0.6515(3) 1.6264(2) 0.0260(10) Uani 1 1 d . . . H20A_3 H 0.7387 -0.6843 1.5844 0.031 Uiso 1 1 calc R . . C202_3 C 0.6751(3) -0.6018(3) 1.6238(2) 0.0296(11) Uani 1 1 d . . . C203_3 C 0.6560(3) -0.5534(3) 1.6839(3) 0.0331(11) Uani 1 1 d . . . H20B_3 H 0.6213 -0.5189 1.6823 0.040 Uiso 1 1 calc R . . C204_3 C 0.6885(3) -0.5562(3) 1.7464(3) 0.0320(11) Uani 1 1 d . . . C205_3 C 0.7402(3) -0.6059(3) 1.7487(2) 0.0270(10) Uani 1 1 d . . . H20C_3 H 0.7620 -0.6063 1.7923 0.032 Uiso 1 1 calc R . . C206_3 C 0.6427(3) -0.6002(3) 1.5548(3) 0.0402(13) Uani 1 1 d D . . F200_3 F 0.7008(10) -0.5816(15) 1.5172(11) 0.050(4) Uani 0.49(5) 1 d PDU C 1 F201_3 F 0.6040(17) -0.6681(8) 1.5177(13) 0.071(5) Uani 0.49(5) 1 d PDU C 1 F202_3 F 0.5934(15) -0.5516(14) 1.5562(14) 0.066(4) Uani 0.49(5) 1 d PDU C 1 F100_3 F 0.5820(11) -0.6555(12) 1.5289(11) 0.062(4) Uani 0.51(5) 1 d PDU C 2 F101_3 F 0.6169(16) -0.5344(9) 1.5595(13) 0.061(4) Uani 0.51(5) 1 d PDU C 2 F102_3 F 0.6944(10) -0.6053(17) 1.5068(10) 0.053(4) Uani 0.51(5) 1 d PDU C 2 C207_3 C 0.6670(3) -0.5068(3) 1.8124(3) 0.0417(13) Uani 1 1 d D . . F203_3 F 0.6113(11) -0.4674(11) 1.8031(7) 0.077(4) Uani 0.63(4) 1 d PDU D 1 F204_3 F 0.6382(10) -0.5472(7) 1.8544(7) 0.058(3) Uani 0.63(4) 1 d PDU D 1 F205_3 F 0.7273(7) -0.4570(9) 1.8480(7) 0.068(3) Uani 0.63(4) 1 d PDU D 1 F103_3 F 0.7271(11) -0.4811(16) 1.8607(12) 0.065(5) Uani 0.37(4) 1 d PDU D 2 F104_3 F 0.6437(19) -0.4444(11) 1.8051(12) 0.069(5) Uani 0.37(4) 1 d PDU D 2 F105_3 F 0.6114(15) -0.5421(13) 1.8421(13) 0.069(6) Uani 0.37(4) 1 d PDU D 2 C208_3 C 0.7566(3) -0.7951(3) 1.6924(2) 0.0248(10) Uani 1 1 d . . . C209_3 C 0.7154(3) -0.8430(3) 1.6316(2) 0.0279(10) Uani 1 1 d . . . H20D_3 H 0.7264 -0.8322 1.5890 0.033 Uiso 1 1 calc R . . C210_3 C 0.6593(3) -0.9053(3) 1.6311(3) 0.0322(11) Uani 1 1 d . . . C211_3 C 0.6416(3) -0.9234(3) 1.6921(3) 0.0367(12) Uani 1 1 d . . . H21A_3 H 0.6034 -0.9665 1.6919 0.044 Uiso 1 1 calc R . . C212_3 C 0.6812(3) -0.8770(3) 1.7531(3) 0.0358(12) Uani 1 1 d . . . C213_3 C 0.7372(3) -0.8141(3) 1.7530(2) 0.0298(11) Uani 1 1 d . . . H21B_3 H 0.7632 -0.7830 1.7957 0.036 Uiso 1 1 calc R . . C214_3 C 0.6162(3) -0.9543(3) 1.5649(3) 0.0428(13) Uani 1 1 d D . . F206_3 F 0.6344(3) -1.0236(2) 1.5468(2) 0.0691(14) Uani 0.923(6) 1 d PDU E 1 F207_3 F 0.5386(2) -0.9657(3) 1.5699(2) 0.0578(12) Uani 0.923(6) 1 d PDU E 1 F208_3 F 0.6272(3) -0.9246(2) 1.51212(18) 0.0647(14) Uani 0.923(6) 1 d PDU E 1 F106_3 F 0.557(2) -0.928(2) 1.541(2) 0.067(7) Uani 0.077(6) 1 d PDU E 2 F107_3 F 0.6681(19) -0.960(3) 1.5163(17) 0.056(7) Uani 0.077(6) 1 d PDU E 2 F108_3 F 0.588(3) -1.0270(11) 1.561(3) 0.071(7) Uani 0.077(6) 1 d PDU E 2 C215_3 C 0.6616(3) -0.8929(3) 1.8204(3) 0.0487(15) Uani 1 1 d D . . F209_3 F 0.7216(8) -0.8665(9) 1.8683(9) 0.059(3) Uani 0.53(2) 1 d PDU F 1 F210_3 F 0.5998(8) -0.8662(11) 1.8459(9) 0.079(3) Uani 0.53(2) 1 d PDU F 1 F211_3 F 0.6468(10) -0.9689(4) 1.8132(6) 0.064(3) Uani 0.53(2) 1 d PDU F 1 F109_3 F 0.6093(12) -0.9553(9) 1.8149(8) 0.093(4) Uani 0.47(2) 1 d PDU F 2 F110_3 F 0.7225(9) -0.8937(12) 1.8608(10) 0.065(4) Uani 0.47(2) 1 d PDU F 2 F111_3 F 0.6279(10) -0.8354(8) 1.8606(7) 0.061(4) Uani 0.47(2) 1 d PDU F 2 C216_3 C 0.8695(2) -0.7327(3) 1.6229(2) 0.0234(10) Uani 1 1 d . . . C217_3 C 0.8940(3) -0.8021(3) 1.5947(2) 0.0275(10) Uani 1 1 d . . . H21C_3 H 0.8738 -0.8448 1.6105 0.033 Uiso 1 1 calc R . . C218_3 C 0.9475(3) -0.8104(3) 1.5439(3) 0.0328(11) Uani 1 1 d . . . C219_3 C 0.9792(3) -0.7494(3) 1.5199(2) 0.0353(12) Uani 1 1 d . . . H21D_3 H 1.0157 -0.7551 1.4855 0.042 Uiso 1 1 calc R . . C220_3 C 0.9560(3) -0.6799(3) 1.5475(2) 0.0309(11) Uani 1 1 d . . . C221_3 C 0.9027(3) -0.6721(3) 1.5978(2) 0.0273(10) Uani 1 1 d . . . H22A_3 H 0.8881 -0.6237 1.6160 0.033 Uiso 1 1 calc R . . C222_3 C 0.9701(3) -0.8867(3) 1.5164(3) 0.0530(17) Uani 1 1 d D . . F212_3 F 0.9092(8) -0.9339(11) 1.4772(13) 0.070(5) Uani 0.47(4) 1 d PDU G 1 F213_3 F 1.0271(11) -0.8819(15) 1.4728(10) 0.061(4) Uani 0.47(4) 1 d PDU G 1 F214_3 F 0.9970(14) -0.9164(15) 1.5632(10) 0.063(4) Uani 0.47(4) 1 d PDU G 1 F112_3 F 1.0165(11) -0.9004(12) 1.5649(9) 0.057(4) Uani 0.53(4) 1 d PDU G 2 F113_3 F 0.9094(7) -0.9463(7) 1.5065(13) 0.067(4) Uani 0.53(4) 1 d PDU G 2 F114_3 F 1.0094(13) -0.8966(15) 1.4598(8) 0.069(4) Uani 0.53(4) 1 d PDU G 2 C223_3 C 0.9900(3) -0.6112(3) 1.5265(2) 0.0449(14) Uani 1 1 d D . . F215_3 F 1.0396(13) -0.5632(12) 1.5768(9) 0.060(4) Uani 0.55(6) 1 d PDU H 1 F216_3 F 1.0316(13) -0.6292(13) 1.4709(9) 0.064(4) Uani 0.55(6) 1 d PDU H 1 F217_3 F 0.9363(10) -0.5734(14) 1.5100(14) 0.058(4) Uani 0.55(6) 1 d PDU H 1 F115_3 F 0.9351(13) -0.5888(17) 1.4919(14) 0.055(4) Uani 0.45(6) 1 d PDU H 2 F116_3 F 1.016(2) -0.5488(13) 1.5799(9) 0.062(5) Uani 0.45(6) 1 d PDU H 2 F117_3 F 1.0494(14) -0.6189(19) 1.4856(15) 0.068(5) Uani 0.45(6) 1 d PDU H 2 C224_3 C 0.8872(3) -0.6891(3) 1.7527(2) 0.0274(10) Uani 1 1 d . . . C225_3 C 0.9250(3) -0.6133(3) 1.7745(3) 0.0356(12) Uani 1 1 d . . . H22B_3 H 0.9023 -0.5759 1.7605 0.043 Uiso 1 1 calc R . . C226_3 C 0.9952(3) -0.5909(3) 1.8161(3) 0.0479(15) Uani 1 1 d . . . C227_3 C 1.0287(3) -0.6436(4) 1.8390(3) 0.0481(15) Uani 1 1 d . . . H22C_3 H 1.0755 -0.6281 1.8687 0.058 Uiso 1 1 calc R . . C228_3 C 0.9929(3) -0.7192(3) 1.8180(3) 0.0376(12) Uani 1 1 d . . . C229_3 C 0.9236(3) -0.7413(3) 1.7756(2) 0.0313(11) Uani 1 1 d . . . H22D_3 H 0.9000 -0.7936 1.7618 0.038 Uiso 1 1 calc R . . C230_3 C 1.0376(4) -0.5117(4) 1.8304(4) 0.085(3) Uani 1 1 d D . . F218_3 F 1.1082(7) -0.4957(12) 1.8604(10) 0.098(5) Uani 0.401(9) 1 d PDU I 1 F219_3 F 1.0196(10) -0.4701(9) 1.7923(8) 0.092(4) Uani 0.401(9) 1 d PDU I 1 F220_3 F 0.9976(9) -0.4777(9) 1.8882(8) 0.139(5) Uani 0.401(9) 1 d PDU I 1 F118_3 F 1.0838(7) -0.4883(8) 1.8876(5) 0.095(4) Uani 0.599(9) 1 d PDU I 2 F119_3 F 1.0861(6) -0.5040(5) 1.7761(5) 0.117(4) Uani 0.599(9) 1 d PDU I 2 F120_3 F 0.9974(6) -0.4606(5) 1.8296(7) 0.094(3) Uani 0.599(9) 1 d PDU I 2 C231_3 C 1.0303(4) -0.7768(4) 1.8388(3) 0.0615(19) Uani 1 1 d D . . F221_3 F 1.0316(6) -0.7741(5) 1.9038(3) 0.086(2) Uani 0.701(12) 1 d PDU J 1 F222_3 F 1.0006(6) -0.8482(4) 1.8046(6) 0.068(2) Uani 0.701(12) 1 d PDU J 1 F223_3 F 1.1093(3) -0.7712(4) 1.8221(5) 0.071(2) Uani 0.701(12) 1 d PDU J 1 F121_3 F 1.0252(15) -0.8441(11) 1.7956(14) 0.081(7) Uani 0.299(12) 1 d PDU J 2 F122_3 F 1.0987(8) -0.7464(9) 1.8737(11) 0.081(4) Uani 0.299(12) 1 d PDU J 2 F123_3 F 0.9884(12) -0.7872(15) 1.8932(9) 0.117(6) Uani 0.299(12) 1 d PDU J 2 B300_4 B 0.6906(3) -0.2047(3) 1.8111(3) 0.0276(12) Uani 1 1 d . . . C300_4 C 0.6166(3) -0.2325(3) 1.7516(2) 0.0275(10) Uani 1 1 d . . . C301_4 C 0.5825(3) -0.1806(3) 1.7266(2) 0.0301(11) Uani 1 1 d . . . H30A_4 H 0.6055 -0.1282 1.7414 0.036 Uiso 1 1 calc R . . C302_4 C 0.5159(3) -0.2033(3) 1.6809(3) 0.0336(12) Uani 1 1 d . . . C303_4 C 0.4794(3) -0.2790(3) 1.6586(3) 0.0341(12) Uani 1 1 d . . . H30B_4 H 0.4342 -0.2945 1.6270 0.041 Uiso 1 1 calc R . . C304_4 C 0.5112(3) -0.3312(3) 1.6840(2) 0.0315(11) Uani 1 1 d . . . C305_4 C 0.5784(3) -0.3084(3) 1.7290(2) 0.0295(11) Uani 1 1 d . . . H30C_4 H 0.5991 -0.3457 1.7450 0.035 Uiso 1 1 calc R . . C306_4 C 0.4843(3) -0.1450(3) 1.6539(3) 0.0504(16) Uani 1 1 d D . . F300_4 F 0.5370(7) -0.1122(9) 1.6187(8) 0.067(3) Uani 0.58(3) 1 d PDU K 1 F301_4 F 0.4216(7) -0.1756(7) 1.6084(8) 0.062(3) Uani 0.58(3) 1 d PDU K 1 F302_4 F 0.4680(12) -0.0874(8) 1.7032(7) 0.077(4) Uani 0.58(3) 1 d PDU K 1 F400_4 F 0.4064(5) -0.1585(10) 1.6418(14) 0.064(4) Uani 0.42(3) 1 d PDU K 2 F401_4 F 0.4966(12) -0.0769(10) 1.7012(11) 0.071(5) Uani 0.42(3) 1 d PDU K 2 F402_4 F 0.5199(14) -0.1341(15) 1.5998(9) 0.080(5) Uani 0.42(3) 1 d PDU K 2 C307_4 C 0.4712(3) -0.4119(3) 1.6623(3) 0.0437(14) Uani 1 1 d D . . F303_4 F 0.4733(5) -0.4460(4) 1.5953(3) 0.096(2) Uani 0.795(8) 1 d PDU L 1 F304_4 F 0.4991(3) -0.4570(3) 1.6949(4) 0.0760(19) Uani 0.795(8) 1 d PDU L 1 F305_4 F 0.3951(2) -0.4208(3) 1.6737(4) 0.0694(18) Uani 0.795(8) 1 d PDU L 1 F403_4 F 0.4551(15) -0.4384(12) 1.7158(8) 0.081(5) Uani 0.205(8) 1 d PDU L 2 F404_4 F 0.4084(11) -0.4235(11) 1.6203(12) 0.072(5) Uani 0.205(8) 1 d PDU L 2 F405_4 F 0.5195(10) -0.4542(10) 1.6278(12) 0.070(5) Uani 0.205(8) 1 d PDU L 2 C308_4 C 0.6494(3) -0.1990(3) 1.8845(2) 0.0286(11) Uani 1 1 d . . . C309_4 C 0.6311(3) -0.1319(3) 1.9274(3) 0.0326(11) Uani 1 1 d . . . H30D_4 H 0.6428 -0.0861 1.9141 0.039 Uiso 1 1 calc R . . C310_4 C 0.5963(3) -0.1302(3) 1.9892(3) 0.0377(12) Uani 1 1 d . . . C311_4 C 0.5743(3) -0.1961(4) 2.0085(3) 0.0420(14) Uani 1 1 d . . . H31A_4 H 0.5495 -0.1950 2.0500 0.050 Uiso 1 1 calc R . . C312_4 C 0.5893(3) -0.2641(3) 1.9658(3) 0.0385(13) Uani 1 1 d . . . C313_4 C 0.6271(3) -0.2646(3) 1.9055(2) 0.0328(11) Uani 1 1 d . . . H31B_4 H 0.6380 -0.3116 1.8776 0.039 Uiso 1 1 calc R . . C314_4 C 0.5859(3) -0.0573(4) 2.0377(3) 0.0531(16) Uani 1 1 d D . . F306_4 F 0.6156(10) 0.0051(6) 2.0204(7) 0.073(3) Uani 0.53(2) 1 d PDU M 1 F307_4 F 0.5107(5) -0.0541(10) 2.0479(10) 0.079(4) Uani 0.53(2) 1 d PDU M 1 F308_4 F 0.6178(11) -0.0480(8) 2.1017(4) 0.081(4) Uani 0.53(2) 1 d PDU M 1 F406_4 F 0.5234(8) -0.0607(11) 2.0732(9) 0.078(4) Uani 0.47(2) 1 d PDU M 2 F407_4 F 0.6490(8) -0.0270(9) 2.0819(10) 0.086(4) Uani 0.47(2) 1 d PDU M 2 F408_4 F 0.5817(13) -0.0043(9) 2.0046(8) 0.077(4) Uani 0.47(2) 1 d PDU M 2 C315_4 C 0.5671(4) -0.3354(4) 1.9851(3) 0.066(2) Uani 1 1 d D . . F309_4 F 0.6128(7) -0.3322(6) 2.0410(5) 0.105(3) Uani 0.540(9) 1 d PDU N 1 F310_4 F 0.4962(6) -0.3340(6) 2.0157(6) 0.087(3) Uani 0.540(9) 1 d PDU N 1 F311_4 F 0.5598(8) -0.3977(5) 1.9388(5) 0.086(3) Uani 0.540(9) 1 d PDU N 1 F409_4 F 0.5172(8) -0.3873(7) 1.9353(7) 0.093(4) Uani 0.460(9) 1 d PDU N 2 F410_4 F 0.6273(6) -0.3781(6) 1.9790(7) 0.093(3) Uani 0.460(9) 1 d PDU N 2 F411_4 F 0.5397(10) -0.3366(7) 2.0428(5) 0.093(4) Uani 0.460(9) 1 d PDU N 2 C316_4 C 0.7526(3) -0.2645(3) 1.8033(2) 0.0277(10) Uani 1 1 d . . . C317_4 C 0.8024(3) -0.2600(3) 1.8605(2) 0.0320(11) Uani 1 1 d . . . H31C_4 H 0.7962 -0.2249 1.9033 0.038 Uiso 1 1 calc R . . C318_4 C 0.8599(3) -0.3038(3) 1.8579(3) 0.0345(12) Uani 1 1 d . . . C319_4 C 0.8717(3) -0.3554(3) 1.7965(3) 0.0345(12) Uani 1 1 d . . . H31D_4 H 0.9113 -0.3859 1.7943 0.041 Uiso 1 1 calc R . . C320_4 C 0.8235(3) -0.3609(3) 1.7385(2) 0.0291(11) Uani 1 1 d . . . C321_4 C 0.7659(3) -0.3163(3) 1.7418(2) 0.0283(10) Uani 1 1 d . . . H32A_4 H 0.7343 -0.3212 1.7010 0.034 Uiso 1 1 calc R . . C322_4 C 0.9094(3) -0.2962(3) 1.9224(3) 0.0492(15) Uani 1 1 d D . . F312_4 F 0.8777(8) -0.3381(9) 1.9606(7) 0.082(3) Uani 0.62(3) 1 d PDU O 1 F313_4 F 0.9812(5) -0.3125(9) 1.9084(5) 0.065(3) Uani 0.62(3) 1 d PDU O 1 F314_4 F 0.9240(9) -0.2242(5) 1.9621(8) 0.066(3) Uani 0.62(3) 1 d PDU O 1 F412_4 F 0.9493(13) -0.2275(8) 1.9519(13) 0.062(5) Uani 0.38(3) 1 d PDU O 2 F413_4 F 0.8619(9) -0.3091(13) 1.9717(9) 0.070(5) Uani 0.38(3) 1 d PDU O 2 F414_4 F 0.9561(14) -0.3473(12) 1.9181(8) 0.077(4) Uani 0.38(3) 1 d PDU O 2 C323_4 C 0.8385(3) -0.4132(3) 1.6712(2) 0.0362(12) Uani 1 1 d D . . F315_4 F 0.8518(19) -0.4803(9) 1.6774(12) 0.044(4) Uani 0.59(9) 1 d PDU P 1 F316_4 F 0.7768(12) -0.4292(17) 1.6246(13) 0.043(4) Uani 0.59(9) 1 d PDU P 1 F317_4 F 0.9004(14) -0.3844(16) 1.6424(15) 0.057(4) Uani 0.59(9) 1 d PDU P 1 F415_4 F 0.887(2) -0.375(2) 1.636(2) 0.051(5) Uani 0.41(9) 1 d PDU P 2 F416_4 F 0.874(3) -0.4697(18) 1.6783(17) 0.050(5) Uani 0.41(9) 1 d PDU P 2 F417_4 F 0.7740(14) -0.444(2) 1.6291(18) 0.042(5) Uani 0.41(9) 1 d PDU P 2 C324_4 C 0.7467(3) -0.1253(3) 1.8077(2) 0.0292(11) Uani 1 1 d . . . C325_4 C 0.7881(3) -0.0730(3) 1.8661(2) 0.0329(11) Uani 1 1 d . . . H32B_4 H 0.7803 -0.0817 1.9099 0.039 Uiso 1 1 calc R . . C326_4 C 0.8404(3) -0.0089(3) 1.8628(3) 0.0407(13) Uani 1 1 d . . . C327_4 C 0.8536(3) 0.0058(3) 1.8000(3) 0.0383(12) Uani 1 1 d . . . H32C_4 H 0.8884 0.0501 1.7976 0.046 Uiso 1 1 calc R . . C328_4 C 0.8150(3) -0.0455(3) 1.7407(3) 0.0322(11) Uani 1 1 d . . . C329_4 C 0.7631(3) -0.1093(3) 1.7451(2) 0.0288(10) Uani 1 1 d . . . H32D_4 H 0.7375 -0.1437 1.7036 0.035 Uiso 1 1 calc R . . C330_4 C 0.8823(4) 0.0455(3) 1.9280(3) 0.066(2) Uani 1 1 d D . . F318_4 F 0.8307(4) 0.0603(4) 1.9775(3) 0.072(2) Uani 0.650(8) 1 d PDU Q 1 F319_4 F 0.9358(5) 0.0191(5) 1.9545(5) 0.108(3) Uani 0.650(8) 1 d PDU Q 1 F320_4 F 0.9004(6) 0.1165(4) 1.9196(4) 0.096(3) Uani 0.650(8) 1 d PDU Q 1 F418_4 F 0.9609(5) 0.0617(7) 1.9206(5) 0.062(3) Uani 0.350(8) 1 d PDU Q 2 F419_4 F 0.8620(9) 0.1109(7) 1.9466(9) 0.104(4) Uani 0.350(8) 1 d PDU Q 2 F420_4 F 0.8840(11) 0.0144(9) 1.9805(7) 0.104(4) Uani 0.350(8) 1 d PDU Q 2 C331_4 C 0.8305(3) -0.0328(3) 1.6720(3) 0.0410(13) Uani 1 1 d D . . F321_4 F 0.8979(8) -0.0504(12) 1.6510(9) 0.074(3) Uani 0.46(2) 1 d PDU R 1 F322_4 F 0.7748(9) -0.0698(10) 1.6226(8) 0.072(4) Uani 0.46(2) 1 d PDU R 1 F323_4 F 0.8356(9) 0.0401(5) 1.6739(8) 0.058(3) Uani 0.46(2) 1 d PDU R 1 F421_4 F 0.7646(6) -0.0411(10) 1.6329(7) 0.068(3) Uani 0.54(2) 1 d PDU R 2 F422_4 F 0.8709(11) 0.0345(7) 1.6741(8) 0.089(4) Uani 0.54(2) 1 d PDU R 2 F423_4 F 0.8680(9) -0.0849(8) 1.6337(6) 0.065(3) Uani 0.54(2) 1 d PDU R 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_1 0.0285(4) 0.0359(4) 0.0306(4) 0.0125(3) 0.0046(3) 0.0064(3) Fe2_1 0.0260(4) 0.0321(4) 0.0249(3) 0.0067(3) 0.0026(3) 0.0047(3) S1_1 0.0262(6) 0.0476(8) 0.0278(6) 0.0135(6) 0.0025(5) 0.0024(5) S2_1 0.0394(7) 0.0331(7) 0.0272(6) 0.0068(5) 0.0016(5) 0.0054(6) S3_1 0.0277(6) 0.0541(9) 0.0354(7) 0.0125(6) 0.0012(5) 0.0069(6) P1_1 0.0242(7) 0.0598(10) 0.0338(7) 0.0180(7) 0.0024(5) 0.0061(6) P2_1 0.0395(8) 0.0456(9) 0.0355(7) 0.0186(6) 0.0006(6) 0.0021(6) O1_1 0.075(3) 0.056(3) 0.098(4) 0.044(3) 0.017(3) 0.021(3) O2_1 0.056(3) 0.069(3) 0.067(3) 0.026(2) 0.035(2) 0.024(2) O3_1 0.031(2) 0.039(2) 0.057(2) 0.0139(19) 0.0001(17) -0.0026(17) O4_1 0.073(3) 0.048(3) 0.066(3) -0.010(2) 0.010(2) 0.018(2) C1_1 0.039(3) 0.049(4) 0.056(4) 0.021(3) 0.005(3) 0.007(3) C2_1 0.044(3) 0.040(3) 0.040(3) 0.015(3) 0.006(3) 0.013(3) C3_1 0.041(3) 0.090(5) 0.043(3) -0.008(3) -0.008(3) 0.023(3) C4_1 0.027(3) 0.059(4) 0.055(4) 0.019(3) 0.003(2) 0.007(3) C5_1 0.044(8) 0.094(16) 0.031(13) 0.029(14) 0.000(9) 0.000(9) C5B_1 0.044(8) 0.094(16) 0.031(13) 0.029(14) 0.000(9) 0.000(9) C6_1 0.034(3) 0.039(3) 0.031(3) 0.007(2) 0.002(2) 0.009(2) C7_1 0.034(3) 0.062(4) 0.044(3) 0.026(3) -0.002(2) -0.010(3) C8_1 0.045(3) 0.046(4) 0.050(3) 0.018(3) -0.005(3) -0.010(3) C9_1 0.047(3) 0.038(3) 0.043(3) 0.008(3) -0.006(3) -0.004(3) C10_1 0.035(3) 0.047(4) 0.035(3) 0.007(3) 0.004(2) 0.009(2) C11_1 0.035(3) 0.095(6) 0.051(4) 0.013(4) 0.013(3) 0.020(3) C12_1 0.066(4) 0.048(4) 0.034(3) 0.013(3) -0.005(3) 0.005(3) C13_1 0.080(11) 0.037(4) 0.058(5) 0.021(4) -0.016(8) -0.004(5) C13B_1 0.080(11) 0.037(4) 0.058(5) 0.021(4) -0.016(8) -0.004(5) C14_1 0.057(8) 0.09(2) 0.067(8) 0.047(11) 0.020(6) 0.006(8) C14B_1 0.035(13) 0.10(3) 0.045(14) 0.062(19) 0.002(11) -0.009(16) Fe1_2 0.0268(4) 0.0341(4) 0.0309(4) 0.0024(3) -0.0026(3) 0.0075(3) Fe2_2 0.0253(4) 0.0345(4) 0.0278(4) 0.0035(3) -0.0002(3) 0.0051(3) S1_2 0.0286(6) 0.0483(8) 0.0273(6) -0.0029(6) -0.0013(5) 0.0109(6) S2_2 0.0269(6) 0.0321(7) 0.0387(7) 0.0037(6) -0.0037(5) 0.0051(5) S3_2 0.0345(7) 0.0662(10) 0.0320(7) 0.0111(7) -0.0036(6) 0.0097(7) P1_2 0.0279(7) 0.0539(9) 0.0301(7) 0.0020(6) -0.0034(5) 0.0072(6) P2_2 0.0317(7) 0.0349(8) 0.0465(8) 0.0102(6) 0.0028(6) 0.0095(6) O1_2 0.051(3) 0.099(4) 0.047(3) 0.027(3) 0.014(2) 0.014(2) O2_2 0.089(4) 0.047(3) 0.104(4) 0.011(3) -0.023(3) 0.026(3) O3_2 0.052(2) 0.042(2) 0.037(2) -0.0048(19) -0.0018(18) 0.0103(19) O4_2 0.062(3) 0.059(3) 0.072(3) 0.027(2) 0.009(2) -0.011(2) C1_2 0.045(3) 0.046(4) 0.059(4) 0.005(3) -0.009(3) 0.012(3) C2_2 0.032(3) 0.051(4) 0.045(3) 0.015(3) -0.001(2) 0.007(3) C3_2 0.049(4) 0.083(5) 0.028(3) 0.003(3) -0.009(3) 0.000(3) C4_2 0.039(3) 0.085(5) 0.074(5) 0.009(4) -0.010(3) 0.027(3) C5_2 0.035(3) 0.072(5) 0.039(3) 0.002(3) 0.002(2) -0.004(3) C6_2 0.028(3) 0.040(3) 0.034(3) 0.005(3) 0.002(2) 0.006(2) C7_2 0.046(3) 0.061(4) 0.034(3) -0.011(3) -0.004(3) 0.020(3) C8_2 0.054(4) 0.045(4) 0.050(4) -0.015(3) -0.013(3) 0.012(3) C9_2 0.042(3) 0.038(3) 0.045(3) -0.007(3) -0.009(3) 0.001(3) C10_2 0.038(3) 0.051(4) 0.038(3) 0.009(3) -0.001(2) 0.004(3) C11_2 0.050(4) 0.100(6) 0.036(3) 0.020(3) 0.001(3) 0.007(4) C12_2 0.028(3) 0.053(4) 0.075(4) 0.016(3) -0.003(3) 0.011(3) C13_2 0.054(4) 0.043(4) 0.100(6) 0.026(4) 0.006(4) 0.015(3) C14_2 0.045(4) 0.079(5) 0.060(4) 0.008(4) 0.015(3) 0.027(3) B200_3 0.023(3) 0.026(3) 0.024(3) 0.007(2) 0.001(2) 0.004(2) C200_3 0.022(2) 0.028(3) 0.025(2) 0.009(2) 0.0036(18) 0.0029(19) C201_3 0.023(2) 0.029(3) 0.028(2) 0.009(2) 0.0039(19) 0.0058(19) C202_3 0.026(2) 0.035(3) 0.033(3) 0.017(2) 0.002(2) 0.007(2) C203_3 0.030(3) 0.032(3) 0.044(3) 0.016(2) 0.008(2) 0.014(2) C204_3 0.031(3) 0.031(3) 0.035(3) 0.009(2) 0.009(2) 0.007(2) C205_3 0.026(2) 0.028(3) 0.028(2) 0.011(2) 0.0009(19) 0.004(2) C206_3 0.038(3) 0.050(4) 0.041(3) 0.024(3) 0.003(2) 0.013(3) F200_3 0.062(6) 0.054(9) 0.034(6) 0.015(5) 0.006(4) 0.003(5) F201_3 0.083(9) 0.064(6) 0.060(8) 0.027(5) -0.038(7) -0.010(6) F202_3 0.063(8) 0.095(8) 0.058(6) 0.032(7) -0.002(7) 0.049(7) F100_3 0.049(7) 0.087(7) 0.049(6) 0.030(5) -0.014(5) -0.014(5) F101_3 0.070(9) 0.068(6) 0.061(6) 0.033(5) -0.008(7) 0.035(6) F102_3 0.052(6) 0.087(10) 0.032(6) 0.028(7) 0.011(5) 0.029(6) C207_3 0.045(3) 0.037(3) 0.044(3) 0.008(3) 0.010(3) 0.013(3) F203_3 0.087(8) 0.084(7) 0.066(4) 0.004(5) 0.014(5) 0.064(6) F204_3 0.073(6) 0.054(4) 0.052(5) 0.013(3) 0.035(5) 0.022(4) F205_3 0.071(5) 0.055(7) 0.055(5) -0.012(4) 0.019(3) -0.011(4) F103_3 0.069(7) 0.064(10) 0.052(8) -0.007(7) 0.003(6) 0.020(6) F104_3 0.104(11) 0.047(7) 0.065(7) 0.013(6) 0.022(8) 0.043(8) F105_3 0.064(9) 0.060(8) 0.069(9) -0.002(6) 0.039(8) -0.001(7) C208_3 0.020(2) 0.027(3) 0.032(2) 0.011(2) 0.0030(19) 0.0111(19) C209_3 0.028(2) 0.030(3) 0.030(2) 0.012(2) 0.005(2) 0.009(2) C210_3 0.030(3) 0.027(3) 0.038(3) 0.005(2) 0.004(2) 0.008(2) C211_3 0.034(3) 0.030(3) 0.049(3) 0.018(2) 0.008(2) 0.000(2) C212_3 0.033(3) 0.038(3) 0.042(3) 0.020(2) 0.007(2) 0.009(2) C213_3 0.027(2) 0.036(3) 0.029(3) 0.011(2) 0.003(2) 0.009(2) C214_3 0.041(3) 0.033(3) 0.049(3) 0.007(3) 0.003(3) 0.000(2) F206_3 0.070(3) 0.042(2) 0.078(3) -0.015(2) -0.011(2) 0.019(2) F207_3 0.038(2) 0.069(3) 0.055(2) 0.005(2) -0.0067(17) -0.0015(18) F208_3 0.083(3) 0.062(3) 0.035(2) 0.0090(18) -0.0079(19) -0.018(2) F106_3 0.065(10) 0.067(10) 0.057(10) 0.007(9) -0.004(9) -0.003(9) F107_3 0.061(10) 0.050(10) 0.047(10) 0.002(9) -0.009(9) -0.001(9) F108_3 0.062(10) 0.062(10) 0.073(10) -0.004(9) 0.000(10) 0.005(9) C215_3 0.050(4) 0.056(4) 0.051(4) 0.031(3) 0.015(3) 0.010(3) F209_3 0.080(6) 0.061(8) 0.048(5) 0.035(6) 0.008(4) 0.014(5) F210_3 0.063(6) 0.118(8) 0.082(7) 0.058(6) 0.039(5) 0.037(6) F211_3 0.078(7) 0.059(5) 0.069(5) 0.045(4) 0.018(5) 0.003(4) F109_3 0.097(8) 0.100(7) 0.074(6) 0.038(5) 0.028(7) -0.033(6) F110_3 0.075(6) 0.083(10) 0.065(7) 0.052(7) 0.014(5) 0.041(6) F111_3 0.060(7) 0.090(8) 0.049(5) 0.036(5) 0.026(5) 0.023(6) C216_3 0.018(2) 0.028(3) 0.023(2) 0.0052(19) -0.0007(17) 0.0045(18) C217_3 0.021(2) 0.028(3) 0.032(3) 0.007(2) -0.0011(19) 0.0035(19) C218_3 0.021(2) 0.039(3) 0.032(3) -0.002(2) -0.001(2) 0.006(2) C219_3 0.020(2) 0.054(4) 0.025(2) 0.000(2) 0.0019(19) 0.005(2) C220_3 0.023(2) 0.045(3) 0.024(2) 0.012(2) -0.0030(19) -0.001(2) C221_3 0.024(2) 0.032(3) 0.026(2) 0.009(2) -0.0003(19) 0.005(2) C222_3 0.035(3) 0.046(4) 0.065(4) -0.008(3) 0.011(3) 0.009(3) F212_3 0.059(5) 0.045(6) 0.084(9) -0.018(6) 0.001(6) 0.004(4) F213_3 0.044(6) 0.061(8) 0.055(6) -0.024(6) 0.007(5) 0.014(5) F214_3 0.070(9) 0.036(9) 0.091(7) 0.024(6) 0.027(6) 0.020(7) F112_3 0.047(7) 0.029(7) 0.094(6) 0.015(4) 0.006(5) 0.007(5) F113_3 0.047(4) 0.039(5) 0.091(10) -0.018(5) 0.011(5) 0.000(3) F114_3 0.074(8) 0.070(9) 0.053(6) -0.012(6) 0.020(6) 0.032(7) C223_3 0.040(3) 0.059(4) 0.036(3) 0.019(3) 0.007(3) -0.002(3) F215_3 0.060(7) 0.054(6) 0.061(5) 0.023(4) -0.004(5) -0.018(5) F216_3 0.052(6) 0.091(7) 0.048(6) 0.029(5) 0.021(5) -0.012(6) F217_3 0.068(5) 0.048(8) 0.066(9) 0.034(7) 0.011(5) 0.003(5) F115_3 0.074(6) 0.047(8) 0.044(8) 0.018(7) -0.006(5) 0.005(5) F116_3 0.074(10) 0.052(8) 0.043(5) 0.009(5) -0.004(6) -0.028(7) F117_3 0.054(8) 0.088(9) 0.070(9) 0.038(7) 0.027(7) 0.006(7) C224_3 0.026(2) 0.034(3) 0.023(2) 0.008(2) 0.0029(19) 0.007(2) C225_3 0.037(3) 0.034(3) 0.035(3) 0.006(2) -0.008(2) 0.009(2) C226_3 0.045(3) 0.038(3) 0.053(4) 0.003(3) -0.017(3) 0.007(3) C227_3 0.036(3) 0.057(4) 0.046(3) 0.009(3) -0.018(3) 0.004(3) C228_3 0.033(3) 0.044(3) 0.041(3) 0.022(3) -0.004(2) 0.005(2) C229_3 0.030(3) 0.036(3) 0.032(3) 0.015(2) 0.000(2) 0.004(2) C230_3 0.063(5) 0.061(5) 0.112(7) 0.001(5) -0.037(5) 0.003(4) F218_3 0.082(8) 0.075(7) 0.127(9) 0.031(8) -0.037(7) -0.012(6) F219_3 0.097(8) 0.055(7) 0.111(9) 0.024(7) -0.009(7) -0.021(6) F220_3 0.157(9) 0.085(8) 0.152(9) 0.008(7) -0.025(8) 0.001(7) F118_3 0.098(6) 0.071(5) 0.089(6) 0.010(5) -0.054(5) -0.032(5) F119_3 0.133(7) 0.068(5) 0.127(6) 0.013(5) 0.040(6) -0.033(5) F120_3 0.091(6) 0.043(4) 0.144(8) 0.025(5) -0.035(6) 0.005(4) C231_3 0.044(4) 0.069(5) 0.078(5) 0.042(4) -0.025(3) -0.003(3) F221_3 0.112(6) 0.105(5) 0.055(3) 0.044(3) -0.031(4) 0.027(5) F222_3 0.048(5) 0.056(4) 0.110(5) 0.038(3) -0.022(4) 0.014(3) F223_3 0.044(3) 0.079(4) 0.109(6) 0.051(4) 0.006(3) 0.025(3) F121_3 0.061(12) 0.080(9) 0.108(10) 0.026(8) -0.017(9) 0.034(8) F122_3 0.063(7) 0.082(8) 0.105(9) 0.045(7) -0.039(7) 0.012(6) F123_3 0.137(12) 0.129(10) 0.109(10) 0.079(8) -0.041(9) 0.022(10) B300_4 0.028(3) 0.029(3) 0.026(3) 0.008(2) -0.005(2) 0.003(2) C300_4 0.025(2) 0.031(3) 0.026(2) 0.008(2) 0.0027(19) 0.005(2) C301_4 0.028(2) 0.032(3) 0.031(3) 0.013(2) 0.003(2) 0.001(2) C302_4 0.024(2) 0.046(3) 0.035(3) 0.019(2) 0.004(2) 0.007(2) C303_4 0.023(2) 0.045(3) 0.031(3) 0.008(2) -0.003(2) 0.004(2) C304_4 0.026(2) 0.034(3) 0.031(3) 0.004(2) 0.001(2) 0.004(2) C305_4 0.027(2) 0.033(3) 0.030(3) 0.009(2) 0.002(2) 0.009(2) C306_4 0.035(3) 0.063(4) 0.065(4) 0.042(4) -0.007(3) 0.002(3) F300_4 0.062(5) 0.070(7) 0.080(6) 0.054(6) -0.010(5) -0.011(4) F301_4 0.047(5) 0.071(6) 0.078(7) 0.042(5) -0.023(5) 0.005(4) F302_4 0.090(9) 0.075(6) 0.089(5) 0.039(5) 0.006(6) 0.051(6) F400_4 0.036(5) 0.063(7) 0.102(10) 0.044(7) -0.017(5) 0.006(4) F401_4 0.059(9) 0.060(7) 0.103(8) 0.033(6) -0.017(6) 0.019(6) F402_4 0.097(10) 0.091(11) 0.067(8) 0.054(7) -0.006(7) 0.005(7) C307_4 0.031(3) 0.041(3) 0.053(4) 0.003(3) -0.009(3) 0.008(2) F303_4 0.124(5) 0.067(4) 0.063(4) -0.022(3) 0.006(4) -0.018(4) F304_4 0.058(3) 0.035(3) 0.129(5) 0.022(3) -0.038(3) 0.000(2) F305_4 0.030(2) 0.041(3) 0.129(5) 0.014(3) 0.007(3) -0.0010(19) F403_4 0.077(9) 0.051(8) 0.105(9) 0.019(7) 0.010(8) -0.011(8) F404_4 0.057(8) 0.048(8) 0.096(9) -0.002(8) -0.034(8) 0.005(7) F405_4 0.068(8) 0.035(7) 0.092(9) -0.010(7) -0.001(8) 0.013(7) C308_4 0.024(2) 0.036(3) 0.026(2) 0.010(2) -0.0055(19) 0.005(2) C309_4 0.028(3) 0.038(3) 0.032(3) 0.010(2) -0.002(2) 0.007(2) C310_4 0.029(3) 0.047(3) 0.034(3) 0.005(2) -0.001(2) 0.010(2) C311_4 0.031(3) 0.065(4) 0.029(3) 0.013(3) 0.004(2) 0.004(3) C312_4 0.038(3) 0.046(3) 0.033(3) 0.017(3) -0.001(2) 0.001(2) C313_4 0.033(3) 0.035(3) 0.029(3) 0.008(2) -0.002(2) 0.004(2) C314_4 0.047(4) 0.065(5) 0.043(3) 0.002(3) 0.001(3) 0.021(3) F306_4 0.080(7) 0.050(5) 0.070(6) -0.011(4) 0.023(5) 0.001(5) F307_4 0.061(5) 0.080(6) 0.087(9) -0.003(7) 0.025(5) 0.028(4) F308_4 0.119(8) 0.081(6) 0.037(4) -0.005(4) -0.011(5) 0.035(6) F406_4 0.087(7) 0.084(6) 0.056(7) 0.001(6) 0.041(5) 0.024(6) F407_4 0.069(6) 0.070(7) 0.090(7) -0.028(6) -0.011(6) 0.019(5) F408_4 0.095(10) 0.053(6) 0.080(8) 0.005(6) 0.029(7) 0.027(6) C315_4 0.076(5) 0.074(5) 0.056(4) 0.038(4) 0.007(4) 0.002(4) F309_4 0.142(7) 0.092(6) 0.098(6) 0.071(5) -0.021(6) 0.001(6) F310_4 0.095(7) 0.078(5) 0.086(7) 0.034(5) 0.038(5) -0.012(5) F311_4 0.148(9) 0.039(4) 0.076(5) 0.020(4) 0.058(6) 0.016(6) F409_4 0.137(10) 0.053(6) 0.097(7) 0.036(5) 0.013(7) 0.012(7) F410_4 0.121(7) 0.073(6) 0.115(7) 0.064(5) 0.025(6) 0.035(5) F411_4 0.150(9) 0.081(6) 0.060(6) 0.042(5) 0.039(6) 0.011(7) C316_4 0.027(2) 0.028(3) 0.027(2) 0.008(2) -0.0001(19) 0.000(2) C317_4 0.033(3) 0.034(3) 0.026(2) 0.003(2) -0.001(2) 0.007(2) C318_4 0.030(3) 0.040(3) 0.032(3) 0.008(2) -0.005(2) 0.006(2) C319_4 0.030(3) 0.038(3) 0.036(3) 0.010(2) 0.002(2) 0.008(2) C320_4 0.028(2) 0.029(3) 0.029(3) 0.009(2) 0.005(2) 0.002(2) C321_4 0.027(2) 0.034(3) 0.026(2) 0.012(2) -0.0007(19) 0.003(2) C322_4 0.049(4) 0.057(4) 0.041(3) 0.006(3) -0.007(3) 0.022(3) F312_4 0.088(6) 0.095(7) 0.074(5) 0.055(5) -0.027(4) -0.004(5) F313_4 0.044(4) 0.090(7) 0.057(4) 0.005(4) -0.017(3) 0.028(4) F314_4 0.065(7) 0.073(5) 0.046(5) -0.007(4) -0.022(5) 0.022(4) F412_4 0.054(9) 0.076(7) 0.049(8) 0.017(6) -0.021(7) -0.008(6) F413_4 0.079(7) 0.088(10) 0.056(7) 0.043(7) -0.020(5) 0.019(7) F414_4 0.086(8) 0.086(8) 0.066(6) 0.015(6) -0.021(6) 0.051(7) C323_4 0.039(3) 0.035(3) 0.034(3) 0.010(2) 0.003(2) 0.004(2) F315_4 0.052(8) 0.033(4) 0.045(4) 0.005(3) 0.003(6) 0.013(5) F316_4 0.061(5) 0.037(8) 0.028(4) 0.003(5) -0.007(4) 0.010(4) F317_4 0.055(7) 0.059(7) 0.053(6) 0.009(4) 0.027(6) 0.003(5) F415_4 0.050(8) 0.061(8) 0.043(7) 0.013(5) 0.026(7) 0.012(7) F416_4 0.056(10) 0.045(7) 0.050(6) 0.002(6) 0.005(8) 0.026(7) F417_4 0.052(6) 0.030(9) 0.037(7) 0.002(6) 0.002(5) 0.002(5) C324_4 0.027(2) 0.031(3) 0.030(3) 0.010(2) 0.002(2) 0.007(2) C325_4 0.035(3) 0.035(3) 0.026(2) 0.008(2) 0.002(2) 0.001(2) C326_4 0.043(3) 0.037(3) 0.033(3) 0.001(2) 0.007(2) -0.002(2) C327_4 0.038(3) 0.028(3) 0.044(3) 0.005(2) 0.011(2) -0.001(2) C328_4 0.032(3) 0.035(3) 0.033(3) 0.012(2) 0.007(2) 0.011(2) C329_4 0.028(2) 0.031(3) 0.027(2) 0.006(2) -0.0010(19) 0.008(2) C330_4 0.089(6) 0.050(4) 0.044(4) 0.009(3) 0.012(4) -0.024(4) F318_4 0.088(4) 0.070(4) 0.035(3) -0.013(3) 0.013(3) -0.006(3) F319_4 0.074(4) 0.129(5) 0.085(5) -0.032(4) -0.036(4) 0.027(4) F320_4 0.126(5) 0.068(4) 0.064(4) -0.002(3) 0.021(4) -0.038(4) F418_4 0.052(5) 0.068(6) 0.049(5) 0.001(4) -0.023(4) -0.008(4) F419_4 0.095(7) 0.087(6) 0.099(7) -0.025(5) 0.010(6) 0.012(6) F420_4 0.107(7) 0.108(7) 0.074(6) 0.009(5) -0.009(6) -0.015(6) C331_4 0.044(3) 0.041(3) 0.042(3) 0.016(3) 0.008(3) 0.009(3) F321_4 0.077(6) 0.108(8) 0.068(7) 0.052(6) 0.043(5) 0.055(6) F322_4 0.104(8) 0.067(8) 0.041(5) 0.024(6) -0.001(6) -0.016(6) F323_4 0.079(7) 0.046(5) 0.070(5) 0.041(4) 0.031(6) 0.027(4) F421_4 0.066(5) 0.110(9) 0.049(6) 0.040(6) 0.007(4) 0.041(5) F422_4 0.116(8) 0.076(6) 0.069(5) 0.033(5) 0.022(7) -0.022(5) F423_4 0.094(7) 0.074(7) 0.047(5) 0.030(5) 0.042(5) 0.042(6) _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_1 C1_1 1.770(7) . ? Fe1_1 C2_1 1.813(6) . ? Fe1_1 S1_1 2.2501(14) . ? Fe1_1 S2_1 2.2509(15) . ? Fe1_1 P1_1 2.2680(16) . ? Fe1_1 C6_1 2.306(6) . ? Fe1_1 Fe2_1 2.5629(10) . ? Fe2_1 C10_1 1.784(6) . ? Fe2_1 C6_1 1.819(5) . ? Fe2_1 P2_1 2.2725(15) . ? Fe2_1 S2_1 2.2923(15) . ? Fe2_1 S1_1 2.3012(14) . ? Fe2_1 S3_1 2.3124(14) . ? S1_1 C7_1 1.831(5) . ? S2_1 C9_1 1.822(6) . ? S3_1 C11_1 1.818(6) . ? P1_1 C4_1 1.804(5) . ? P1_1 C3_1 1.814(7) . ? P1_1 C5_1 1.818(10) . ? P1_1 C5B_1 1.820(13) . ? P2_1 C13B_1 1.811(16) . ? P2_1 C13_1 1.817(8) . ? P2_1 C12_1 1.820(6) . ? P2_1 C14_1 1.834(10) . ? P2_1 C14B_1 1.837(14) . ? O1_1 C1_1 1.144(7) . ? O2_1 C2_1 1.129(6) . ? O3_1 C6_1 1.155(6) . ? O4_1 C10_1 1.145(7) . ? C3_1 H3A_1 0.9800 . ? C3_1 H3B_1 0.9800 . ? C3_1 H3C_1 0.9800 . ? C4_1 H4A_1 0.9800 . ? C4_1 H4B_1 0.9800 . ? C4_1 H4C_1 0.9800 . ? C5_1 H5A_1 0.9800 . ? C5_1 H5B_1 0.9800 . ? C5_1 H5C_1 0.9800 . ? C5B_1 H5BA_1 0.9800 . ? C5B_1 H5BB_1 0.9800 . ? C5B_1 H5BC_1 0.9800 . ? C7_1 C8_1 1.495(9) . ? C7_1 H7A_1 0.9900 . ? C7_1 H7B_1 0.9900 . ? C8_1 C9_1 1.517(8) . ? C8_1 H8A_1 0.9900 . ? C8_1 H8B_1 0.9900 . ? C9_1 H9A_1 0.9900 . ? C9_1 H9B_1 0.9900 . ? C11_1 H11A_1 0.9800 . ? C11_1 H11B_1 0.9800 . ? C11_1 H11C_1 0.9800 . ? C12_1 H12A_1 0.9800 . ? C12_1 H12B_1 0.9800 . ? C12_1 H12C_1 0.9800 . ? C13_1 H13A_1 0.9800 . ? C13_1 H13B_1 0.9800 . ? C13_1 H13C_1 0.9800 . ? C13B_1 H13D_1 0.9800 . ? C13B_1 H13E_1 0.9800 . ? C13B_1 H13F_1 0.9800 . ? C14_1 H14D_1 0.9800 . ? C14_1 H14E_1 0.9800 . ? C14_1 H14F_1 0.9800 . ? C14B_1 H14G_1 0.9800 . ? C14B_1 H14H_1 0.9800 . ? C14B_1 H14I_1 0.9800 . ? Fe1_2 C1_2 1.767(7) . ? Fe1_2 C2_2 1.803(6) . ? Fe1_2 S1_2 2.2478(15) . ? Fe1_2 S2_2 2.2597(14) . ? Fe1_2 P1_2 2.2761(15) . ? Fe1_2 C6_2 2.307(6) . ? Fe1_2 Fe2_2 2.5705(10) . ? Fe2_2 C10_2 1.799(6) . ? Fe2_2 C6_2 1.818(5) . ? Fe2_2 P2_2 2.2826(15) . ? Fe2_2 S1_2 2.3021(15) . ? Fe2_2 S2_2 2.3061(15) . ? Fe2_2 S3_2 2.3096(15) . ? S1_2 C7_2 1.823(6) . ? S2_2 C9_2 1.820(5) . ? S3_2 C11_2 1.826(6) . ? P1_2 C5_2 1.809(7) . ? P1_2 C4_2 1.810(6) . ? P1_2 C3_2 1.811(6) . ? P2_2 C13_2 1.809(7) . ? P2_2 C12_2 1.817(6) . ? P2_2 C14_2 1.820(6) . ? O1_2 C2_2 1.137(7) . ? O2_2 C1_2 1.134(7) . ? O3_2 C6_2 1.151(6) . ? O4_2 C10_2 1.131(7) . ? C3_2 H3A_2 0.9800 . ? C3_2 H3B_2 0.9800 . ? C3_2 H3C_2 0.9800 . ? C4_2 H4A_2 0.9800 . ? C4_2 H4B_2 0.9800 . ? C4_2 H4C_2 0.9800 . ? C5_2 H5A_2 0.9800 . ? C5_2 H5B_2 0.9800 . ? C5_2 H5C_2 0.9800 . ? C7_2 C8_2 1.507(9) . ? C7_2 H7A_2 0.9900 . ? C7_2 H7B_2 0.9900 . ? C8_2 C9_2 1.508(8) . ? C8_2 H8A_2 0.9900 . ? C8_2 H8B_2 0.9900 . ? C9_2 H9A_2 0.9900 . ? C9_2 H9B_2 0.9900 . ? C11_2 H11A_2 0.9800 . ? C11_2 H11B_2 0.9800 . ? C11_2 H11C_2 0.9800 . ? C12_2 H12A_2 0.9800 . ? C12_2 H12B_2 0.9800 . ? C12_2 H12C_2 0.9800 . ? C13_2 H13A_2 0.9800 . ? C13_2 H13B_2 0.9800 . ? C13_2 H13C_2 0.9800 . ? C14_2 H14A_2 0.9800 . ? C14_2 H14B_2 0.9800 . ? C14_2 H14C_2 0.9800 . ? B200_3 C208_3 1.635(7) . ? B200_3 C200_3 1.636(7) . ? B200_3 C216_3 1.642(6) . ? B200_3 C224_3 1.643(7) . ? C200_3 C205_3 1.398(7) . ? C200_3 C201_3 1.403(6) . ? C201_3 C202_3 1.389(7) . ? C201_3 H20A_3 0.9500 . ? C202_3 C203_3 1.385(7) . ? C202_3 C206_3 1.495(7) . ? C203_3 C204_3 1.383(7) . ? C203_3 H20B_3 0.9500 . ? C204_3 C205_3 1.391(7) . ? C204_3 C207_3 1.493(7) . ? C205_3 H20C_3 0.9500 . ? C208_3 C213_3 1.395(7) . ? C208_3 C209_3 1.400(7) . ? C209_3 C210_3 1.383(7) . ? C209_3 H20D_3 0.9500 . ? C210_3 C211_3 1.389(7) . ? C210_3 C214_3 1.495(7) . ? C211_3 C212_3 1.385(8) . ? C211_3 H21A_3 0.9500 . ? C212_3 C213_3 1.392(7) . ? C212_3 C215_3 1.501(7) . ? C213_3 H21B_3 0.9500 . ? C216_3 C217_3 1.396(7) . ? C216_3 C221_3 1.399(7) . ? C217_3 C218_3 1.395(7) . ? C217_3 H21C_3 0.9500 . ? C218_3 C219_3 1.386(8) . ? C218_3 C222_3 1.491(8) . ? C219_3 C220_3 1.384(8) . ? C219_3 H21D_3 0.9500 . ? C220_3 C221_3 1.386(6) . ? C220_3 C223_3 1.488(7) . ? C221_3 H22A_3 0.9500 . ? C224_3 C225_3 1.395(7) . ? C224_3 C229_3 1.401(7) . ? C225_3 C226_3 1.396(7) . ? C225_3 H22B_3 0.9500 . ? C226_3 C227_3 1.382(8) . ? C226_3 C230_3 1.479(10) . ? C227_3 C228_3 1.382(8) . ? C227_3 H22C_3 0.9500 . ? C228_3 C229_3 1.391(7) . ? C228_3 C231_3 1.475(8) . ? C229_3 H22D_3 0.9500 . ? B300_4 C316_4 1.643(7) . ? B300_4 C308_4 1.646(7) . ? B300_4 C324_4 1.646(7) . ? B300_4 C300_4 1.648(7) . ? C300_4 C301_4 1.397(7) . ? C300_4 C305_4 1.399(7) . ? C301_4 C302_4 1.390(7) . ? C301_4 H30A_4 0.9500 . ? C302_4 C303_4 1.388(8) . ? C302_4 C306_4 1.499(8) . ? C303_4 C304_4 1.386(7) . ? C303_4 H30B_4 0.9500 . ? C304_4 C305_4 1.390(7) . ? C304_4 C307_4 1.484(7) . ? C305_4 H30C_4 0.9500 . ? C308_4 C313_4 1.393(7) . ? C308_4 C309_4 1.397(7) . ? C309_4 C310_4 1.395(7) . ? C309_4 H30D_4 0.9500 . ? C310_4 C311_4 1.379(8) . ? C310_4 C314_4 1.477(8) . ? C311_4 C312_4 1.387(8) . ? C311_4 H31A_4 0.9500 . ? C312_4 C313_4 1.396(7) . ? C312_4 C315_4 1.471(8) . ? C313_4 H31B_4 0.9500 . ? C316_4 C317_4 1.396(7) . ? C316_4 C321_4 1.398(7) . ? C317_4 C318_4 1.376(7) . ? C317_4 H31C_4 0.9500 . ? C318_4 C319_4 1.388(7) . ? C318_4 C322_4 1.499(7) . ? C319_4 C320_4 1.389(7) . ? C319_4 H31D_4 0.9500 . ? C320_4 C321_4 1.386(7) . ? C320_4 C323_4 1.495(7) . ? C321_4 H32A_4 0.9500 . ? C324_4 C325_4 1.397(7) . ? C324_4 C329_4 1.399(7) . ? C325_4 C326_4 1.391(7) . ? C325_4 H32B_4 0.9500 . ? C326_4 C327_4 1.384(8) . ? C326_4 C330_4 1.505(8) . ? C327_4 C328_4 1.384(7) . ? C327_4 H32C_4 0.9500 . ? C328_4 C329_4 1.391(7) . ? C328_4 C331_4 1.492(7) . ? C329_4 H32D_4 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_1 Fe1_1 C2_1 91.5(3) . . ? C1_1 Fe1_1 S1_1 99.94(19) . . ? C2_1 Fe1_1 S1_1 168.54(18) . . ? C1_1 Fe1_1 S2_1 100.7(2) . . ? C2_1 Fe1_1 S2_1 90.99(18) . . ? S1_1 Fe1_1 S2_1 86.55(5) . . ? C1_1 Fe1_1 P1_1 91.0(2) . . ? C2_1 Fe1_1 P1_1 92.90(18) . . ? S1_1 Fe1_1 P1_1 87.31(5) . . ? S2_1 Fe1_1 P1_1 167.56(6) . . ? C1_1 Fe1_1 C6_1 171.1(2) . . ? C2_1 Fe1_1 C6_1 80.5(2) . . ? S1_1 Fe1_1 C6_1 88.05(13) . . ? S2_1 Fe1_1 C6_1 83.48(13) . . ? P1_1 Fe1_1 C6_1 85.50(14) . . ? C1_1 Fe1_1 Fe2_1 145.04(19) . . ? C2_1 Fe1_1 Fe2_1 112.93(17) . . ? S1_1 Fe1_1 Fe2_1 56.68(4) . . ? S2_1 Fe1_1 Fe2_1 56.43(4) . . ? P1_1 Fe1_1 Fe2_1 111.26(5) . . ? C6_1 Fe1_1 Fe2_1 43.47(13) . . ? C10_1 Fe2_1 C6_1 85.6(2) . . ? C10_1 Fe2_1 P2_1 95.31(19) . . ? C6_1 Fe2_1 P2_1 86.88(17) . . ? C10_1 Fe2_1 S2_1 177.36(19) . . ? C6_1 Fe2_1 S2_1 94.42(17) . . ? P2_1 Fe2_1 S2_1 87.33(6) . . ? C10_1 Fe2_1 S1_1 92.99(19) . . ? C6_1 Fe2_1 S1_1 99.80(17) . . ? P2_1 Fe2_1 S1_1 169.73(6) . . ? S2_1 Fe2_1 S1_1 84.40(5) . . ? C10_1 Fe2_1 S3_1 84.29(18) . . ? C6_1 Fe2_1 S3_1 163.85(18) . . ? P2_1 Fe2_1 S3_1 81.56(5) . . ? S2_1 Fe2_1 S3_1 96.25(6) . . ? S1_1 Fe2_1 S3_1 93.28(5) . . ? C10_1 Fe2_1 Fe1_1 123.10(18) . . ? C6_1 Fe2_1 Fe1_1 60.72(17) . . ? P2_1 Fe2_1 Fe1_1 124.01(5) . . ? S2_1 Fe2_1 Fe1_1 54.90(4) . . ? S1_1 Fe2_1 Fe1_1 54.79(4) . . ? S3_1 Fe2_1 Fe1_1 135.39(5) . . ? C7_1 S1_1 Fe1_1 113.1(2) . . ? C7_1 S1_1 Fe2_1 109.16(19) . . ? Fe1_1 S1_1 Fe2_1 68.53(4) . . ? C9_1 S2_1 Fe1_1 113.35(19) . . ? C9_1 S2_1 Fe2_1 110.0(2) . . ? Fe1_1 S2_1 Fe2_1 68.68(4) . . ? C11_1 S3_1 Fe2_1 110.6(2) . . ? C4_1 P1_1 C3_1 103.5(3) . . ? C4_1 P1_1 C5_1 104.8(14) . . ? C3_1 P1_1 C5_1 98.1(19) . . ? C4_1 P1_1 C5B_1 100(2) . . ? C3_1 P1_1 C5B_1 111.8(19) . . ? C5_1 P1_1 C5B_1 14(2) . . ? C4_1 P1_1 Fe1_1 114.8(2) . . ? C3_1 P1_1 Fe1_1 117.0(2) . . ? C5_1 P1_1 Fe1_1 116.4(16) . . ? C5B_1 P1_1 Fe1_1 109(2) . . ? C13B_1 P2_1 C13_1 17(3) . . ? C13B_1 P2_1 C12_1 111(3) . . ? C13_1 P2_1 C12_1 103.5(7) . . ? C13B_1 P2_1 C14_1 84(5) . . ? C13_1 P2_1 C14_1 100.7(19) . . ? C12_1 P2_1 C14_1 104.5(11) . . ? C13B_1 P2_1 C14B_1 102(5) . . ? C13_1 P2_1 C14B_1 118(3) . . ? C12_1 P2_1 C14B_1 95(2) . . ? C14_1 P2_1 C14B_1 18.0(17) . . ? C13B_1 P2_1 Fe2_1 119(3) . . ? C13_1 P2_1 Fe2_1 112.3(6) . . ? C12_1 P2_1 Fe2_1 115.4(2) . . ? C14_1 P2_1 Fe2_1 118.5(10) . . ? C14B_1 P2_1 Fe2_1 110.9(16) . . ? O1_1 C1_1 Fe1_1 178.2(6) . . ? O2_1 C2_1 Fe1_1 179.6(5) . . ? P1_1 C3_1 H3A_1 109.5 . . ? P1_1 C3_1 H3B_1 109.5 . . ? H3A_1 C3_1 H3B_1 109.5 . . ? P1_1 C3_1 H3C_1 109.5 . . ? H3A_1 C3_1 H3C_1 109.5 . . ? H3B_1 C3_1 H3C_1 109.5 . . ? P1_1 C4_1 H4A_1 109.5 . . ? P1_1 C4_1 H4B_1 109.5 . . ? H4A_1 C4_1 H4B_1 109.5 . . ? P1_1 C4_1 H4C_1 109.5 . . ? H4A_1 C4_1 H4C_1 109.5 . . ? H4B_1 C4_1 H4C_1 109.5 . . ? P1_1 C5_1 H5A_1 109.5 . . ? P1_1 C5_1 H5B_1 109.5 . . ? P1_1 C5_1 H5C_1 109.5 . . ? P1_1 C5B_1 H5BA_1 109.5 . . ? P1_1 C5B_1 H5BB_1 109.5 . . ? H5BA_1 C5B_1 H5BB_1 109.5 . . ? P1_1 C5B_1 H5BC_1 109.5 . . ? H5BA_1 C5B_1 H5BC_1 109.5 . . ? H5BB_1 C5B_1 H5BC_1 109.5 . . ? O3_1 C6_1 Fe2_1 158.1(5) . . ? O3_1 C6_1 Fe1_1 125.9(4) . . ? Fe2_1 C6_1 Fe1_1 75.8(2) . . ? C8_1 C7_1 S1_1 116.7(4) . . ? C8_1 C7_1 H7A_1 108.1 . . ? S1_1 C7_1 H7A_1 108.1 . . ? C8_1 C7_1 H7B_1 108.1 . . ? S1_1 C7_1 H7B_1 108.1 . . ? H7A_1 C7_1 H7B_1 107.3 . . ? C7_1 C8_1 C9_1 115.5(5) . . ? C7_1 C8_1 H8A_1 108.4 . . ? C9_1 C8_1 H8A_1 108.4 . . ? C7_1 C8_1 H8B_1 108.4 . . ? C9_1 C8_1 H8B_1 108.4 . . ? H8A_1 C8_1 H8B_1 107.5 . . ? C8_1 C9_1 S2_1 116.4(4) . . ? C8_1 C9_1 H9A_1 108.2 . . ? S2_1 C9_1 H9A_1 108.2 . . ? C8_1 C9_1 H9B_1 108.2 . . ? S2_1 C9_1 H9B_1 108.2 . . ? H9A_1 C9_1 H9B_1 107.3 . . ? O4_1 C10_1 Fe2_1 178.7(6) . . ? S3_1 C11_1 H11A_1 109.5 . . ? S3_1 C11_1 H11B_1 109.5 . . ? H11A_1 C11_1 H11B_1 109.5 . . ? S3_1 C11_1 H11C_1 109.5 . . ? H11A_1 C11_1 H11C_1 109.5 . . ? H11B_1 C11_1 H11C_1 109.5 . . ? P2_1 C12_1 H12A_1 109.5 . . ? P2_1 C12_1 H12B_1 109.5 . . ? H12A_1 C12_1 H12B_1 109.5 . . ? P2_1 C12_1 H12C_1 109.5 . . ? H12A_1 C12_1 H12C_1 109.5 . . ? H12B_1 C12_1 H12C_1 109.5 . . ? P2_1 C13_1 H13A_1 109.5 . . ? P2_1 C13_1 H13B_1 109.5 . . ? P2_1 C13_1 H13C_1 109.5 . . ? P2_1 C13B_1 H13D_1 109.5 . . ? P2_1 C13B_1 H13E_1 109.5 . . ? H13D_1 C13B_1 H13E_1 109.5 . . ? P2_1 C13B_1 H13F_1 109.5 . . ? H13D_1 C13B_1 H13F_1 109.5 . . ? H13E_1 C13B_1 H13F_1 109.5 . . ? P2_1 C14_1 H14D_1 109.5 . . ? P2_1 C14_1 H14E_1 109.5 . . ? P2_1 C14_1 H14F_1 109.5 . . ? P2_1 C14B_1 H14G_1 109.5 . . ? P2_1 C14B_1 H14H_1 109.5 . . ? H14G_1 C14B_1 H14H_1 109.5 . . ? P2_1 C14B_1 H14I_1 109.5 . . ? H14G_1 C14B_1 H14I_1 109.5 . . ? H14H_1 C14B_1 H14I_1 109.5 . . ? C1_2 Fe1_2 C2_2 91.3(3) . . ? C1_2 Fe1_2 S1_2 99.2(2) . . ? C2_2 Fe1_2 S1_2 169.40(19) . . ? C1_2 Fe1_2 S2_2 101.6(2) . . ? C2_2 Fe1_2 S2_2 90.57(17) . . ? S1_2 Fe1_2 S2_2 86.43(5) . . ? C1_2 Fe1_2 P1_2 90.0(2) . . ? C2_2 Fe1_2 P1_2 92.99(18) . . ? S1_2 Fe1_2 P1_2 87.95(5) . . ? S2_2 Fe1_2 P1_2 167.74(7) . . ? C1_2 Fe1_2 C6_2 171.3(2) . . ? C2_2 Fe1_2 C6_2 81.8(2) . . ? S1_2 Fe1_2 C6_2 87.74(14) . . ? S2_2 Fe1_2 C6_2 83.85(13) . . ? P1_2 Fe1_2 C6_2 85.05(13) . . ? C1_2 Fe1_2 Fe2_2 145.3(2) . . ? C2_2 Fe1_2 Fe2_2 113.49(18) . . ? S1_2 Fe1_2 Fe2_2 56.61(4) . . ? S2_2 Fe1_2 Fe2_2 56.60(4) . . ? P1_2 Fe1_2 Fe2_2 111.35(5) . . ? C6_2 Fe1_2 Fe2_2 43.35(13) . . ? C10_2 Fe2_2 C6_2 85.7(2) . . ? C10_2 Fe2_2 P2_2 95.79(19) . . ? C6_2 Fe2_2 P2_2 86.45(17) . . ? C10_2 Fe2_2 S1_2 93.62(19) . . ? C6_2 Fe2_2 S1_2 99.36(17) . . ? P2_2 Fe2_2 S1_2 169.30(6) . . ? C10_2 Fe2_2 S2_2 177.72(19) . . ? C6_2 Fe2_2 S2_2 94.70(18) . . ? P2_2 Fe2_2 S2_2 86.48(5) . . ? S1_2 Fe2_2 S2_2 84.10(5) . . ? C10_2 Fe2_2 S3_2 82.75(18) . . ? C6_2 Fe2_2 S3_2 163.29(18) . . ? P2_2 Fe2_2 S3_2 82.76(6) . . ? S1_2 Fe2_2 S3_2 93.40(5) . . ? S2_2 Fe2_2 S3_2 97.33(6) . . ? C10_2 Fe2_2 Fe1_2 123.67(18) . . ? C6_2 Fe2_2 Fe1_2 60.58(18) . . ? P2_2 Fe2_2 Fe1_2 122.69(5) . . ? S1_2 Fe2_2 Fe1_2 54.61(4) . . ? S2_2 Fe2_2 Fe1_2 54.89(4) . . ? S3_2 Fe2_2 Fe1_2 136.13(5) . . ? C7_2 S1_2 Fe1_2 112.6(2) . . ? C7_2 S1_2 Fe2_2 109.6(2) . . ? Fe1_2 S1_2 Fe2_2 68.79(4) . . ? C9_2 S2_2 Fe1_2 113.64(19) . . ? C9_2 S2_2 Fe2_2 109.4(2) . . ? Fe1_2 S2_2 Fe2_2 68.52(4) . . ? C11_2 S3_2 Fe2_2 110.2(2) . . ? C5_2 P1_2 C4_2 101.7(3) . . ? C5_2 P1_2 C3_2 104.2(3) . . ? C4_2 P1_2 C3_2 104.4(3) . . ? C5_2 P1_2 Fe1_2 116.5(2) . . ? C4_2 P1_2 Fe1_2 113.8(2) . . ? C3_2 P1_2 Fe1_2 114.6(2) . . ? C13_2 P2_2 C12_2 104.4(3) . . ? C13_2 P2_2 C14_2 104.7(4) . . ? C12_2 P2_2 C14_2 102.0(3) . . ? C13_2 P2_2 Fe2_2 113.9(2) . . ? C12_2 P2_2 Fe2_2 115.8(2) . . ? C14_2 P2_2 Fe2_2 114.7(2) . . ? O2_2 C1_2 Fe1_2 177.6(6) . . ? O1_2 C2_2 Fe1_2 179.1(6) . . ? P1_2 C3_2 H3A_2 109.5 . . ? P1_2 C3_2 H3B_2 109.5 . . ? H3A_2 C3_2 H3B_2 109.5 . . ? P1_2 C3_2 H3C_2 109.5 . . ? H3A_2 C3_2 H3C_2 109.5 . . ? H3B_2 C3_2 H3C_2 109.5 . . ? P1_2 C4_2 H4A_2 109.5 . . ? P1_2 C4_2 H4B_2 109.5 . . ? H4A_2 C4_2 H4B_2 109.5 . . ? P1_2 C4_2 H4C_2 109.5 . . ? H4A_2 C4_2 H4C_2 109.5 . . ? H4B_2 C4_2 H4C_2 109.5 . . ? P1_2 C5_2 H5A_2 109.5 . . ? P1_2 C5_2 H5B_2 109.5 . . ? H5A_2 C5_2 H5B_2 109.5 . . ? P1_2 C5_2 H5C_2 109.5 . . ? H5A_2 C5_2 H5C_2 109.5 . . ? H5B_2 C5_2 H5C_2 109.5 . . ? O3_2 C6_2 Fe2_2 157.7(5) . . ? O3_2 C6_2 Fe1_2 126.0(4) . . ? Fe2_2 C6_2 Fe1_2 76.07(19) . . ? C8_2 C7_2 S1_2 117.6(4) . . ? C8_2 C7_2 H7A_2 107.9 . . ? S1_2 C7_2 H7A_2 107.9 . . ? C8_2 C7_2 H7B_2 107.9 . . ? S1_2 C7_2 H7B_2 107.9 . . ? H7A_2 C7_2 H7B_2 107.2 . . ? C7_2 C8_2 C9_2 114.4(5) . . ? C7_2 C8_2 H8A_2 108.7 . . ? C9_2 C8_2 H8A_2 108.7 . . ? C7_2 C8_2 H8B_2 108.7 . . ? C9_2 C8_2 H8B_2 108.7 . . ? H8A_2 C8_2 H8B_2 107.6 . . ? C8_2 C9_2 S2_2 116.3(4) . . ? C8_2 C9_2 H9A_2 108.2 . . ? S2_2 C9_2 H9A_2 108.2 . . ? C8_2 C9_2 H9B_2 108.2 . . ? S2_2 C9_2 H9B_2 108.2 . . ? H9A_2 C9_2 H9B_2 107.4 . . ? O4_2 C10_2 Fe2_2 178.8(6) . . ? S3_2 C11_2 H11A_2 109.5 . . ? S3_2 C11_2 H11B_2 109.5 . . ? H11A_2 C11_2 H11B_2 109.5 . . ? S3_2 C11_2 H11C_2 109.5 . . ? H11A_2 C11_2 H11C_2 109.5 . . ? H11B_2 C11_2 H11C_2 109.5 . . ? P2_2 C12_2 H12A_2 109.5 . . ? P2_2 C12_2 H12B_2 109.5 . . ? H12A_2 C12_2 H12B_2 109.5 . . ? P2_2 C12_2 H12C_2 109.5 . . ? H12A_2 C12_2 H12C_2 109.5 . . ? H12B_2 C12_2 H12C_2 109.5 . . ? P2_2 C13_2 H13A_2 109.5 . . ? P2_2 C13_2 H13B_2 109.5 . . ? H13A_2 C13_2 H13B_2 109.5 . . ? P2_2 C13_2 H13C_2 109.5 . . ? H13A_2 C13_2 H13C_2 109.5 . . ? H13B_2 C13_2 H13C_2 109.5 . . ? P2_2 C14_2 H14A_2 109.5 . . ? P2_2 C14_2 H14B_2 109.5 . . ? H14A_2 C14_2 H14B_2 109.5 . . ? P2_2 C14_2 H14C_2 109.5 . . ? H14A_2 C14_2 H14C_2 109.5 . . ? H14B_2 C14_2 H14C_2 109.5 . . ? C208_3 B200_3 C200_3 105.3(4) . . ? C208_3 B200_3 C216_3 112.6(4) . . ? C200_3 B200_3 C216_3 111.2(4) . . ? C208_3 B200_3 C224_3 114.3(4) . . ? C200_3 B200_3 C224_3 113.6(4) . . ? C216_3 B200_3 C224_3 100.1(3) . . ? C205_3 C200_3 C201_3 115.7(4) . . ? C205_3 C200_3 B200_3 123.3(4) . . ? C201_3 C200_3 B200_3 120.8(4) . . ? C202_3 C201_3 C200_3 122.4(4) . . ? C202_3 C201_3 H20A_3 118.8 . . ? C200_3 C201_3 H20A_3 118.8 . . ? C203_3 C202_3 C201_3 120.4(4) . . ? C203_3 C202_3 C206_3 120.7(4) . . ? C201_3 C202_3 C206_3 118.8(4) . . ? C204_3 C203_3 C202_3 118.5(4) . . ? C204_3 C203_3 H20B_3 120.7 . . ? C202_3 C203_3 H20B_3 120.7 . . ? C203_3 C204_3 C205_3 120.7(5) . . ? C203_3 C204_3 C207_3 120.1(4) . . ? C205_3 C204_3 C207_3 119.2(4) . . ? C204_3 C205_3 C200_3 122.2(4) . . ? C204_3 C205_3 H20C_3 118.9 . . ? C200_3 C205_3 H20C_3 118.9 . . ? C213_3 C208_3 C209_3 115.7(4) . . ? C213_3 C208_3 B200_3 124.1(4) . . ? C209_3 C208_3 B200_3 119.9(4) . . ? C210_3 C209_3 C208_3 122.4(4) . . ? C210_3 C209_3 H20D_3 118.8 . . ? C208_3 C209_3 H20D_3 118.8 . . ? C209_3 C210_3 C211_3 120.7(5) . . ? C209_3 C210_3 C214_3 120.5(5) . . ? C211_3 C210_3 C214_3 118.8(5) . . ? C212_3 C211_3 C210_3 118.1(5) . . ? C212_3 C211_3 H21A_3 120.9 . . ? C210_3 C211_3 H21A_3 120.9 . . ? C211_3 C212_3 C213_3 120.6(5) . . ? C211_3 C212_3 C215_3 119.8(5) . . ? C213_3 C212_3 C215_3 119.5(5) . . ? C212_3 C213_3 C208_3 122.3(5) . . ? C212_3 C213_3 H21B_3 118.8 . . ? C208_3 C213_3 H21B_3 118.8 . . ? C217_3 C216_3 C221_3 115.8(4) . . ? C217_3 C216_3 B200_3 122.3(4) . . ? C221_3 C216_3 B200_3 121.1(4) . . ? C218_3 C217_3 C216_3 121.8(5) . . ? C218_3 C217_3 H21C_3 119.1 . . ? C216_3 C217_3 H21C_3 119.1 . . ? C219_3 C218_3 C217_3 121.0(5) . . ? C219_3 C218_3 C222_3 120.9(4) . . ? C217_3 C218_3 C222_3 118.1(5) . . ? C220_3 C219_3 C218_3 118.2(4) . . ? C220_3 C219_3 H21D_3 120.9 . . ? C218_3 C219_3 H21D_3 120.9 . . ? C219_3 C220_3 C221_3 120.5(5) . . ? C219_3 C220_3 C223_3 121.2(4) . . ? C221_3 C220_3 C223_3 118.3(5) . . ? C220_3 C221_3 C216_3 122.7(5) . . ? C220_3 C221_3 H22A_3 118.6 . . ? C216_3 C221_3 H22A_3 118.6 . . ? C225_3 C224_3 C229_3 116.0(4) . . ? C225_3 C224_3 B200_3 121.6(4) . . ? C229_3 C224_3 B200_3 120.9(4) . . ? C224_3 C225_3 C226_3 122.0(5) . . ? C224_3 C225_3 H22B_3 119.0 . . ? C226_3 C225_3 H22B_3 119.0 . . ? C227_3 C226_3 C225_3 120.5(5) . . ? C227_3 C226_3 C230_3 119.6(5) . . ? C225_3 C226_3 C230_3 119.6(5) . . ? C228_3 C227_3 C226_3 118.8(5) . . ? C228_3 C227_3 H22C_3 120.6 . . ? C226_3 C227_3 H22C_3 120.6 . . ? C227_3 C228_3 C229_3 120.3(5) . . ? C227_3 C228_3 C231_3 119.5(5) . . ? C229_3 C228_3 C231_3 120.2(5) . . ? C228_3 C229_3 C224_3 122.3(5) . . ? C228_3 C229_3 H22D_3 118.8 . . ? C224_3 C229_3 H22D_3 118.8 . . ? C316_4 B300_4 C308_4 108.6(4) . . ? C316_4 B300_4 C324_4 102.9(4) . . ? C308_4 B300_4 C324_4 114.3(4) . . ? C316_4 B300_4 C300_4 114.1(4) . . ? C308_4 B300_4 C300_4 104.6(4) . . ? C324_4 B300_4 C300_4 112.6(4) . . ? C301_4 C300_4 C305_4 115.7(4) . . ? C301_4 C300_4 B300_4 122.0(4) . . ? C305_4 C300_4 B300_4 121.9(4) . . ? C302_4 C301_4 C300_4 122.1(5) . . ? C302_4 C301_4 H30A_4 119.0 . . ? C300_4 C301_4 H30A_4 119.0 . . ? C303_4 C302_4 C301_4 121.2(5) . . ? C303_4 C302_4 C306_4 119.6(5) . . ? C301_4 C302_4 C306_4 119.2(5) . . ? C304_4 C303_4 C302_4 117.7(5) . . ? C304_4 C303_4 H30B_4 121.2 . . ? C302_4 C303_4 H30B_4 121.2 . . ? C303_4 C304_4 C305_4 120.9(5) . . ? C303_4 C304_4 C307_4 118.2(4) . . ? C305_4 C304_4 C307_4 121.0(5) . . ? C304_4 C305_4 C300_4 122.4(5) . . ? C304_4 C305_4 H30C_4 118.8 . . ? C300_4 C305_4 H30C_4 118.8 . . ? C313_4 C308_4 C309_4 115.8(4) . . ? C313_4 C308_4 B300_4 119.8(4) . . ? C309_4 C308_4 B300_4 124.3(4) . . ? C310_4 C309_4 C308_4 122.0(5) . . ? C310_4 C309_4 H30D_4 119.0 . . ? C308_4 C309_4 H30D_4 119.0 . . ? C311_4 C310_4 C309_4 120.8(5) . . ? C311_4 C310_4 C314_4 118.0(5) . . ? C309_4 C310_4 C314_4 121.1(5) . . ? C310_4 C311_4 C312_4 118.5(5) . . ? C310_4 C311_4 H31A_4 120.8 . . ? C312_4 C311_4 H31A_4 120.8 . . ? C311_4 C312_4 C313_4 120.1(5) . . ? C311_4 C312_4 C315_4 119.8(5) . . ? C313_4 C312_4 C315_4 120.1(5) . . ? C308_4 C313_4 C312_4 122.7(5) . . ? C308_4 C313_4 H31B_4 118.6 . . ? C312_4 C313_4 H31B_4 118.6 . . ? C317_4 C316_4 C321_4 115.2(4) . . ? C317_4 C316_4 B300_4 118.9(4) . . ? C321_4 C316_4 B300_4 125.6(4) . . ? C318_4 C317_4 C316_4 123.2(5) . . ? C318_4 C317_4 H31C_4 118.4 . . ? C316_4 C317_4 H31C_4 118.4 . . ? C317_4 C318_4 C319_4 120.7(5) . . ? C317_4 C318_4 C322_4 119.4(5) . . ? C319_4 C318_4 C322_4 119.9(5) . . ? C318_4 C319_4 C320_4 117.6(5) . . ? C318_4 C319_4 H31D_4 121.2 . . ? C320_4 C319_4 H31D_4 121.2 . . ? C321_4 C320_4 C319_4 121.1(5) . . ? C321_4 C320_4 C323_4 120.8(4) . . ? C319_4 C320_4 C323_4 118.0(4) . . ? C320_4 C321_4 C316_4 122.2(4) . . ? C320_4 C321_4 H32A_4 118.9 . . ? C316_4 C321_4 H32A_4 118.9 . . ? C325_4 C324_4 C329_4 114.8(5) . . ? C325_4 C324_4 B300_4 122.7(4) . . ? C329_4 C324_4 B300_4 122.1(4) . . ? C326_4 C325_4 C324_4 122.9(5) . . ? C326_4 C325_4 H32B_4 118.5 . . ? C324_4 C325_4 H32B_4 118.5 . . ? C327_4 C326_4 C325_4 120.4(5) . . ? C327_4 C326_4 C330_4 119.6(5) . . ? C325_4 C326_4 C330_4 120.1(5) . . ? C328_4 C327_4 C326_4 118.5(5) . . ? C328_4 C327_4 H32C_4 120.7 . . ? C326_4 C327_4 H32C_4 120.7 . . ? C327_4 C328_4 C329_4 120.1(5) . . ? C327_4 C328_4 C331_4 119.7(5) . . ? C329_4 C328_4 C331_4 120.2(5) . . ? C328_4 C329_4 C324_4 123.2(5) . . ? C328_4 C329_4 H32D_4 118.4 . . ? C324_4 C329_4 H32D_4 118.4 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.994 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_time ? _refine_diff_density_max 0.788 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.066 _publ_section_references ; ??CSDB??Allen, F.H. and Kennard, O. (1993). Chemical Design Automation News. 8(1), 1 & 31-37. ??CSDB??Allen, F.H., Kennard, O., and Taylor, R. (1983). Accounts Chem. Res. 16, 146-153. ??Organic/Bonds??Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G., and Taylor, R. (1987). J. Chem. Soc. Perkin Trans. II. S1-S19. Bruker (2001). SMART. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2004). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). SAINT, SHELXTL, XCIF, XPREP. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). TOPAS Version 3. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2007). SADABS, TWINABS. Bruker AXS, Inc., Madison, Wisconsin, USA. CrystalMaker (1994). CrystalMaker, a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd., Oxford, England (www.crystalmaker.com). ??WinGX??Farrugia, L.J. (1999). J. Appl. Cryst. 32, 837-838. ??Absolute Structure??Flack, H. D. (1983), Acta Cryst. A39, 876-881. Flack, H. D. (2000), J. Appl. Cryst., 33, 1143-1148. ??Hydrogen bonding??Hamilton, W.C. and Ibers, J.A. (1968). Hydrogen Bonding in Solids. W.A.Benjamin, Inc., New York, New York, USA. ??Organometallic/Bonds??Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G., and Taylor, R. (1989). J. Chem. Soc. Dalton Trans. II. S1-S83. ??PLATON/SQUEEZE??Spek, A. L. and van der Sluis, P. (1990). Acta Cryst. A46, 194-201. ??SHELXD??Schneider, T.R. and Sheldrick, G.M. (2002). Acta Cryst. D58, 1772-1779. ??SHELX - all versions"A short history of SHELX".?? Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ??Cell_Now??Sheldrick, G.M. (2004). Cell_Now. Program to isolate multiple orientations for crystals suffering from non-merohedral twinning. Institute fur anorg chemie, G\"ottingen, Germany. ??MiTeGen micromounts??Thorne, R. E., Stum, Z., Kmetko, J., O'Neill, and Gillilan, R. (2003) J. Appl. Cryst. 36, 1455-1460. ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ??The unlabeled atoms are related by the symmetry operator (2-x, -y, -z).?? ; _publ_section_exptl_prep ; Synthesis was carried out by reaction of ??. Crystals were grown from ??. ; _publ_section_exptl_refinement ; Disorder?? Symmetry?? Idealized from CSD (Allen et al, 1983, 1993)?? Restraints(Allen et al, 1987)?? ??Rigid-bond restraints (esd 0.01) were imposed on displacement parameters for all disordered sites and similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of van der Waals radii. ??[A structural model consisting of the host plus XX disordered XXXX solvate molecules was developed; however, positions for the idealized solvate molecules were poorly determined. This model converged with wR2 = 0.XXX and R1 = 0.XXX for XXX parameters with XXX restraints against XXXXX data. Since positions for the solvate molecules were poorly determined a second structural model was refined with contributions from the solvate molecules removed from the diffraction data using the bypass procedure in PLATON (Spek, 1990). No positions for the host network differed by more than two su's between these two refined models. The electron count from the "squeeze" model converged in good agreement with the number of solvate molecules predicted by the complete refinement. The "squeeze" data are reported here.]?? ??[H atom treatment - Methyl H atom positions, R-CH~3~, were optimized by rotation about R-C bonds with idealized C-H, R--H and H--H distances. Hydroxyl H atom positions, R-OH, were optimized by rotation about R-O bonds with idealized O-H and R--H distances. Remaining H atoms were included as riding idealized contributors. Methyl, hydroxyl and amine H atom U's were assigned as 1.5 times U~eq~ of the carrier atom; remaining H atom U's were assigned as 1.2 times carrier U~eq~. ]?? On the basis of ???? unmerged Friedel opposites, the fractional contribution of the racemic twin was negligible (Flack, 1983 & 2000). ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; _platon_squeeze_details ; The solvent accessible voids contained 3 highly disordered dichloromethane molecuels each. Their positions were poorly determined so they were squeezed ou The void electron count removed is consistent with 2.5 DCM/void. ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.2930 -4.00 1.00 0.00 0.2870 0.00 1.00 0.00 0.0850 0.00 -1.00 0.00 0.1170 0.00 0.00 -1.00 0.0650 0.00 0.00 1.00 0.0210 -2.00 3.00 -2.00 0.2210 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.242 0.434 -0.038 305 100 ' ' 2 0.758 0.566 0.039 305 101 ' '