Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Giuliano Longoni' _publ_contact_author_address ; Dipartimento di Chimica Fisca ed Inorganica Universita di Bologna viale Risorgimento 4 Bologna 40136 ITALY ; _publ_contact_author_email LONGONI@MS.FCI.UNIBO.IT _publ_section_title ; Synthesis and Crystal Structure of the [{Fe3(CO)9(?3-O)}2H]3- Trianion: Dimerization of a Metal Carbonyl Cluster via Formation of an Exceptionally Short Hydrogen Bond. ; loop_ _publ_author_name 'Giuliano Longoni' 'Cristina Femoni' 'M. Carmela Iapalucci' 'Stefano Zacchini' 'Enrico Zazzaroni' data_ia-3 _database_code_depnum_ccdc_archive 'CCDC 639851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H61 Fe6 N3 O20' _chemical_formula_weight 1263.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Ia-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z, x, y+1/2' 'z, x+1/2, -y' 'z+1/2, -x, y' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z, x' '-y, z, x+1/2' 'y, z+1/2, -x' _cell_length_a 22.1927(17) _cell_length_b 22.1927(17) _cell_length_c 22.1927(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10930.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 688 _cell_measurement_theta_min 2.2475 _cell_measurement_theta_max 15.482 _exptl_crystal_description cube _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5200 _exptl_absorpt_coefficient_mu 1.623 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7269 _exptl_absorpt_correction_T_max 0.7929 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44478 _diffrn_reflns_av_R_equivalents 0.2068 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1626 _reflns_number_gt 1062 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+41.2330P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1626 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.13734(3) 0.22807(3) 0.19533(3) 0.0383(2) Uani 1 1 d . . . C1 C 0.1000(2) 0.2444(2) 0.2642(2) 0.0526(14) Uani 1 1 d . . . O1 O 0.0755(2) 0.25516(19) 0.30861(18) 0.0816(13) Uani 1 1 d . . . C2 C 0.0788(2) 0.1888(2) 0.1608(2) 0.0471(13) Uani 1 1 d . . . O2 O 0.04021(18) 0.16259(19) 0.13648(18) 0.0731(12) Uani 1 1 d . . . C3 C 0.1289(2) 0.2986(2) 0.1585(2) 0.0464(13) Uani 1 1 d . . . O3 O 0.12024(18) 0.34390(17) 0.13432(19) 0.0737(12) Uani 1 1 d . . . O4 O 0.21895(12) 0.21895(12) 0.21895(12) 0.0374(13) Uani 1 3 d S . . H4 H 0.2500 0.2500 0.2500 0.045 Uiso 1 6 d S . . N1 N 0.9743(2) 0.0000 0.2500 0.0406(14) Uani 1 2 d S . . C4 C 0.9335(2) -0.0109(3) 0.3034(2) 0.0589(15) Uani 1 1 d . . . H4A H 0.9069 0.0234 0.3078 0.071 Uiso 1 1 calc R . . H4B H 0.9087 -0.0459 0.2950 0.071 Uiso 1 1 calc R . . C5 C 0.9658(3) -0.0210(3) 0.3625(3) 0.0756(18) Uani 1 1 d . . . H5A H 0.9932 -0.0542 0.3585 0.113 Uiso 1 1 calc R . . H5B H 0.9369 -0.0299 0.3934 0.113 Uiso 1 1 calc R . . H5C H 0.9878 0.0147 0.3732 0.113 Uiso 1 1 calc R . . C6 C 1.0146(2) 0.0534(2) 0.2609(2) 0.0507(14) Uani 1 1 d . . . H6A H 1.0393 0.0596 0.2254 0.061 Uiso 1 1 calc R . . H6B H 1.0414 0.0439 0.2941 0.061 Uiso 1 1 calc R . . C7 C 0.9824(3) 0.1118(2) 0.2753(3) 0.0725(18) Uani 1 1 d . . . H7A H 0.9601 0.1249 0.2406 0.109 Uiso 1 1 calc R . . H7B H 1.0114 0.1420 0.2860 0.109 Uiso 1 1 calc R . . H7C H 0.9552 0.1056 0.3084 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0367(4) 0.0389(4) 0.0393(4) -0.0018(3) -0.0001(3) 0.0023(3) C1 0.056(3) 0.053(3) 0.049(4) -0.005(3) 0.005(3) 0.008(3) O1 0.103(3) 0.080(3) 0.062(3) -0.006(2) 0.029(3) 0.016(3) C2 0.040(3) 0.054(3) 0.047(3) 0.008(3) 0.000(3) 0.001(3) O2 0.065(3) 0.080(3) 0.074(3) 0.009(2) -0.020(2) -0.028(2) C3 0.044(3) 0.048(3) 0.047(3) 0.001(3) 0.001(2) 0.004(3) O3 0.084(3) 0.050(3) 0.087(3) 0.015(2) -0.004(2) 0.013(2) O4 0.0374(13) 0.0374(13) 0.0374(13) -0.0045(14) -0.0045(14) -0.0045(14) N1 0.027(3) 0.043(3) 0.051(3) 0.000(3) 0.000 0.000 C4 0.045(3) 0.063(4) 0.069(4) -0.004(3) 0.016(3) -0.009(3) C5 0.097(5) 0.074(4) 0.056(4) 0.001(3) 0.010(4) 0.000(4) C6 0.045(3) 0.044(3) 0.063(4) -0.004(3) 0.001(3) -0.010(2) C7 0.084(5) 0.047(3) 0.087(5) -0.015(3) 0.009(4) -0.002(3) _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 C2 1.743(5) . ? Fe1 C1 1.776(5) . ? Fe1 C3 1.776(5) . ? Fe1 O4 1.896(3) . ? Fe1 Fe1 2.4976(11) 9 ? Fe1 Fe1 2.4976(11) 5 ? C1 O1 1.151(5) . ? C2 O2 1.166(6) . ? C3 O3 1.156(6) . ? O4 Fe1 1.896(3) 9 ? O4 Fe1 1.896(3) 5 ? O4 H4 1.193(5) . ? N1 C6 1.505(5) . ? N1 C6 1.505(5) 16_445 ? N1 C4 1.511(5) 16_445 ? N1 C4 1.511(5) . ? C4 C5 1.511(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.514(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 C2 Fe1 C1 97.6(2) . . ? C2 Fe1 C3 99.2(2) . . ? C1 Fe1 C3 99.6(2) . . ? C2 Fe1 O4 141.3(2) . . ? C1 Fe1 O4 103.26(18) . . ? C3 Fe1 O4 108.78(17) . . ? C2 Fe1 Fe1 103.23(16) . 9 ? C1 Fe1 Fe1 151.51(17) . 9 ? C3 Fe1 Fe1 96.01(16) . 9 ? O4 Fe1 Fe1 48.81(8) . 9 ? C2 Fe1 Fe1 96.27(16) . 5 ? C1 Fe1 Fe1 98.87(17) . 5 ? C3 Fe1 Fe1 154.02(16) . 5 ? O4 Fe1 Fe1 48.81(8) . 5 ? Fe1 Fe1 Fe1 60.0 9 5 ? O1 C1 Fe1 179.5(6) . . ? O2 C2 Fe1 178.6(5) . . ? O3 C3 Fe1 176.4(5) . . ? Fe1 O4 Fe1 82.37(16) 9 5 ? Fe1 O4 Fe1 82.37(16) 9 . ? Fe1 O4 Fe1 82.37(16) 5 . ? Fe1 O4 H4 130.50(11) 9 . ? Fe1 O4 H4 130.50(11) 5 . ? Fe1 O4 H4 130.50(11) . . ? C6 N1 C6 107.1(5) . 16_445 ? C6 N1 C4 110.8(3) . 16_445 ? C6 N1 C4 110.9(3) 16_445 16_445 ? C6 N1 C4 110.9(3) . . ? C6 N1 C4 110.8(3) 16_445 . ? C4 N1 C4 106.4(5) 16_445 . ? C5 C4 N1 114.9(4) . . ? C5 C4 H4A 108.5 . . ? N1 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? N1 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 115.3(4) . . ? N1 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? N1 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Fe1 C1 O1 -60(83) . . . . ? C3 Fe1 C1 O1 41(83) . . . . ? O4 Fe1 C1 O1 153(100) . . . . ? Fe1 Fe1 C1 O1 163(100) 9 . . . ? Fe1 Fe1 C1 O1 -158(100) 5 . . . ? C1 Fe1 C2 O2 167(100) . . . . ? C3 Fe1 C2 O2 66(20) . . . . ? O4 Fe1 C2 O2 -71(20) . . . . ? Fe1 Fe1 C2 O2 -33(20) 9 . . . ? Fe1 Fe1 C2 O2 -93(20) 5 . . . ? C2 Fe1 C3 O3 29(8) . . . . ? C1 Fe1 C3 O3 -70(8) . . . . ? O4 Fe1 C3 O3 -178(100) . . . . ? Fe1 Fe1 C3 O3 134(8) 9 . . . ? Fe1 Fe1 C3 O3 155(7) 5 . . . ? C2 Fe1 O4 Fe1 52.7(3) . . . 9 ? C1 Fe1 O4 Fe1 173.52(19) . . . 9 ? C3 Fe1 O4 Fe1 -81.3(2) . . . 9 ? Fe1 Fe1 O4 Fe1 83.27(13) 5 . . 9 ? C2 Fe1 O4 Fe1 -30.6(3) . . . 5 ? C1 Fe1 O4 Fe1 90.2(2) . . . 5 ? C3 Fe1 O4 Fe1 -164.61(17) . . . 5 ? Fe1 Fe1 O4 Fe1 -83.27(13) 9 . . 5 ? C6 N1 C4 C5 -57.5(5) . . . . ? C6 N1 C4 C5 61.2(5) 16_445 . . . ? C4 N1 C4 C5 -178.1(6) 16_445 . . . ? C6 N1 C6 C7 -177.8(6) 16_445 . . . ? C4 N1 C6 C7 61.2(6) 16_445 . . . ? C4 N1 C6 C7 -56.8(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.370 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.073 #===END data_r-3m _database_code_depnum_ccdc_archive 'CCDC 639852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H9 Cs3 Fe6 O21' _chemical_formula_weight 1343.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 13.0952(3) _cell_length_b 13.0952(3) _cell_length_c 18.5660(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2757.23(17) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5555 _cell_measurement_theta_min 2.8355 _cell_measurement_theta_max 28.263 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1890 _exptl_absorpt_coefficient_mu 5.312 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4318 _exptl_absorpt_correction_T_max 0.5926 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10703 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0082 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.98 _reflns_number_total 837 _reflns_number_gt 772 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following restraints were applied in order to obtain a satisfatctory model: simu .001 $o; simu .001 $c; delu .001 fe1 > c14; dfix 1.43 .01 o10 c11 o10 c14; dfix 1.53 .01 c11 c12 c12 c13 c13 c14; dfix 2.38 .01 o10 c12 o10 c13; dfix 2.30 .01 c11 c14; dfix 2.35 .01 c12 c14 c11 c13; dfix -4 cs1 c11 cs1 c12 cs1 c13 cs1 c14; dfix -4 cs1 c11 cs1 c12 cs1 c13 cs1 c14 cs1 C13_$13 cs1 C13_$12 cs1 C13_$15; dfix -4 cs1 c13_$14 cs1 c14_$13 cs1 c14_$14 cs1 c14_$15 cs1 c14_$12; dfix -4 cs1 c12_$12 cs1 c12_$13 cs1 c12_$14 cs1 c12_$15; dfix -4 cs1 c12_$16 cs1 c12_$17 cs1 c12_$18 cs1 c12_$19; dfix -4 cs1 c11_$16 cs1 c11_$17 cs1 c11_$18 cs1 c11_$19;dfix -4 c11 cs1_$10 c12 cs1_$10 c13 cs1_$10 c13 cs1_$11 c14 cs1_$11 ; _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^)+(0.0296P)^2^+5.7606P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 837 _refine_ls_number_parameters 64 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.550 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.93663(2) 0.06337(2) 0.13027(3) 0.03253(19) Uani 1 2 d SU . . C1 C 0.92229(19) 0.07771(19) 0.2232(2) 0.0422(7) Uani 1 2 d SU . . O1 O 0.91401(18) 0.08599(18) 0.28442(17) 0.0572(8) Uani 1 2 d SU . . C2 C 0.7868(3) 0.0065(3) 0.10317(16) 0.0440(7) Uani 1 1 d U . . O2 O 0.6910(3) -0.0278(3) 0.08720(17) 0.0704(8) Uani 1 1 d U . . O4 O 1.0000 0.0000 0.0642(2) 0.0331(7) Uani 1 6 d SU . . H4 H 1.0000 0.0000 0.0000 0.050 Uiso 1 12 d S . . Cs1 Cs 0.6667 -0.1667 0.3333 0.0842(3) Uani 1 4 d SDU . . O10 O 0.275(3) 0.606(3) 0.1074(17) 0.079(7) Uiso 0.08 1 d PDU . -1 C11 C 0.382(5) 0.615(6) 0.134(2) 0.079(7) Uiso 0.17 2 d SPDU . -1 H11A H 0.4280 0.6095 0.0945 0.095 Uiso 0.08 1 calc PR . -1 H11B H 0.3654 0.5529 0.1682 0.095 Uiso 0.08 1 calc PR . -1 C12 C 0.450(2) 0.736(6) 0.170(2) 0.079(7) Uiso 0.08 1 d PDU . -1 H12A H 0.5034 0.7372 0.2069 0.095 Uiso 0.08 1 calc PR . -1 H12B H 0.4942 0.7981 0.1354 0.095 Uiso 0.08 1 calc PR . -1 C13 C 0.350(3) 0.747(4) 0.203(2) 0.079(7) Uiso 0.08 1 d PDU . -1 H13A H 0.3271 0.7087 0.2494 0.095 Uiso 0.08 1 calc PR . -1 H13B H 0.3708 0.8289 0.2079 0.095 Uiso 0.08 1 calc PR . -1 C14 C 0.253(3) 0.684(5) 0.148(3) 0.079(7) Uiso 0.08 1 d PDU . -1 H14A H 0.1772 0.6405 0.1721 0.095 Uiso 0.08 1 calc PR . -1 H14B H 0.2496 0.7412 0.1160 0.095 Uiso 0.08 1 calc PR . -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0339(3) 0.0339(3) 0.0340(3) 0.00015(10) -0.00015(10) 0.0200(2) C1 0.0530(11) 0.0530(11) 0.0371(10) -0.0010(6) 0.0010(6) 0.0388(11) O1 0.0684(9) 0.0684(9) 0.0384(10) -0.0041(8) 0.0041(8) 0.0369(10) C2 0.0406(11) 0.0486(17) 0.0499(15) -0.0051(13) -0.0053(11) 0.0277(14) O2 0.0464(12) 0.080(2) 0.0894(19) -0.0168(16) -0.0216(14) 0.0354(15) O4 0.0347(12) 0.0347(12) 0.0300(17) 0.000 0.000 0.0174(6) Cs1 0.1053(5) 0.0492(2) 0.1167(5) 0.0242(2) 0.0484(4) 0.0527(3) _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 C1 1.756(4) . ? Fe1 C2 1.788(3) . ? Fe1 C2 1.788(3) 22_665 ? Fe1 O4 1.890(3) . ? Fe1 Fe1 2.4896(10) 2_645 ? Fe1 Fe1 2.4896(10) 3_765 ? C1 O1 1.152(5) . ? C1 Cs1 3.862(2) 3_765 ? C1 Cs1 3.862(2) . ? O1 Cs1 3.3980(8) 3_765 ? O1 Cs1 3.3980(8) . ? C2 O2 1.140(4) . ? O2 Cs1 3.150(3) 15_654 ? O4 Fe1 1.890(3) 3_765 ? O4 Fe1 1.890(3) 2_645 ? O4 H4 1.191(5) . ? Cs1 O2 3.149(3) 26 ? Cs1 O2 3.150(3) 28 ? Cs1 O2 3.150(3) 10_545 ? Cs1 O2 3.150(3) 8_545 ? Cs1 O1 3.3979(8) 32 ? Cs1 O1 3.3980(8) 31_645 ? Cs1 O1 3.3980(8) 2_645 ? Cs1 C11 3.63(4) 27_545 ? Cs1 C11 3.63(4) 9 ? Cs1 O10 3.73(3) 12_545 ? Cs1 O10 3.73(3) 7_545 ? O10 C14 1.418(12) . ? O10 C11 1.431(13) . ? O10 Cs1 3.73(3) 13_454 ? C11 C12 1.530(14) . ? C11 Cs1 3.63(4) 14_544 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.517(14) . ? C12 Cs1 3.90(4) 1_565 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.513(13) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 Fe1 C2 99.64(13) . . ? C1 Fe1 C2 99.64(13) . 22_665 ? C2 Fe1 C2 98.4(2) . 22_665 ? C1 Fe1 O4 141.17(18) . . ? C2 Fe1 O4 105.41(12) . . ? C2 Fe1 O4 105.41(12) 22_665 . ? C1 Fe1 Fe1 99.23(12) . 2_645 ? C2 Fe1 Fe1 97.59(11) . 2_645 ? C2 Fe1 Fe1 152.77(11) 22_665 2_645 ? O4 Fe1 Fe1 48.81(8) . 2_645 ? C1 Fe1 Fe1 99.23(12) . 3_765 ? C2 Fe1 Fe1 152.77(11) . 3_765 ? C2 Fe1 Fe1 97.59(11) 22_665 3_765 ? O4 Fe1 Fe1 48.81(8) . 3_765 ? Fe1 Fe1 Fe1 60.0 2_645 3_765 ? O1 C1 Fe1 178.7(4) . . ? O1 C1 Cs1 58.15(5) . 3_765 ? Fe1 C1 Cs1 121.76(5) . 3_765 ? O1 C1 Cs1 58.15(5) . . ? Fe1 C1 Cs1 121.76(5) . . ? Cs1 C1 Cs1 115.92(10) 3_765 . ? C1 O1 Cs1 105.12(5) . 3_765 ? C1 O1 Cs1 105.12(5) . . ? Cs1 O1 Cs1 148.93(10) 3_765 . ? O2 C2 Fe1 178.1(3) . . ? C2 O2 Cs1 150.4(3) . 15_654 ? Fe1 O4 Fe1 82.39(16) 3_765 2_645 ? Fe1 O4 Fe1 82.39(16) 3_765 . ? Fe1 O4 Fe1 82.39(16) 2_645 . ? Fe1 O4 H4 130.49(11) 3_765 . ? Fe1 O4 H4 130.49(11) 2_645 . ? Fe1 O4 H4 130.49(11) . . ? O2 Cs1 O2 63.16(12) 26 28 ? O2 Cs1 O2 116.85(12) 26 10_545 ? O2 Cs1 O2 180.0 28 10_545 ? O2 Cs1 O2 180.0 26 8_545 ? O2 Cs1 O2 116.84(12) 28 8_545 ? O2 Cs1 O2 63.15(12) 10_545 8_545 ? O2 Cs1 O1 118.58(9) 26 32 ? O2 Cs1 O1 111.63(8) 28 32 ? O2 Cs1 O1 68.37(8) 10_545 32 ? O2 Cs1 O1 61.42(9) 8_545 32 ? O2 Cs1 O1 68.37(8) 26 31_645 ? O2 Cs1 O1 61.42(9) 28 31_645 ? O2 Cs1 O1 118.58(9) 10_545 31_645 ? O2 Cs1 O1 111.63(8) 8_545 31_645 ? O1 Cs1 O1 59.62(13) 32 31_645 ? O2 Cs1 O1 61.42(9) 26 2_645 ? O2 Cs1 O1 68.37(8) 28 2_645 ? O2 Cs1 O1 111.63(8) 10_545 2_645 ? O2 Cs1 O1 118.58(9) 8_545 2_645 ? O1 Cs1 O1 180.0 32 2_645 ? O1 Cs1 O1 120.38(13) 31_645 2_645 ? O2 Cs1 O1 111.63(8) 26 . ? O2 Cs1 O1 118.58(9) 28 . ? O2 Cs1 O1 61.42(9) 10_545 . ? O2 Cs1 O1 68.37(8) 8_545 . ? O1 Cs1 O1 120.38(13) 32 . ? O1 Cs1 O1 180.0 31_645 . ? O1 Cs1 O1 59.62(13) 2_645 . ? O2 Cs1 C11 64.6(11) 26 27_545 ? O2 Cs1 C11 114.9(9) 28 27_545 ? O2 Cs1 C11 65.1(9) 10_545 27_545 ? O2 Cs1 C11 115.4(11) 8_545 27_545 ? O1 Cs1 C11 65.4(8) 32 27_545 ? O1 Cs1 C11 65.1(6) 31_645 27_545 ? O1 Cs1 C11 114.6(8) 2_645 27_545 ? O1 Cs1 C11 114.9(6) . 27_545 ? O2 Cs1 C11 115.4(11) 26 9 ? O2 Cs1 C11 65.1(9) 28 9 ? O2 Cs1 C11 114.9(9) 10_545 9 ? O2 Cs1 C11 64.6(11) 8_545 9 ? O1 Cs1 C11 114.6(8) 32 9 ? O1 Cs1 C11 114.9(6) 31_645 9 ? O1 Cs1 C11 65.4(8) 2_645 9 ? O1 Cs1 C11 65.1(6) . 9 ? C11 Cs1 C11 179.998(3) 27_545 9 ? O2 Cs1 O10 63.0(5) 26 12_545 ? O2 Cs1 O10 105.2(5) 28 12_545 ? O2 Cs1 O10 74.8(5) 10_545 12_545 ? O2 Cs1 O10 117.0(5) 8_545 12_545 ? O1 Cs1 O10 60.5(5) 32 12_545 ? O1 Cs1 O10 52.8(5) 31_645 12_545 ? O1 Cs1 O10 119.5(5) 2_645 12_545 ? O1 Cs1 O10 127.2(5) . 12_545 ? C11 Cs1 O10 12.3(8) 27_545 12_545 ? C11 Cs1 O10 167.7(8) 9 12_545 ? O2 Cs1 O10 105.2(5) 26 7_545 ? O2 Cs1 O10 63.0(5) 28 7_545 ? O2 Cs1 O10 117.0(5) 10_545 7_545 ? O2 Cs1 O10 74.8(5) 8_545 7_545 ? O1 Cs1 O10 127.2(5) 32 7_545 ? O1 Cs1 O10 119.5(5) 31_645 7_545 ? O1 Cs1 O10 52.8(5) 2_645 7_545 ? O1 Cs1 O10 60.5(5) . 7_545 ? C11 Cs1 O10 167.4(9) 27_545 7_545 ? C11 Cs1 O10 12.6(9) 9 7_545 ? O10 Cs1 O10 167.1(10) 12_545 7_545 ? C14 O10 C11 107.7(8) . . ? C14 O10 Cs1 92.2(18) . 13_454 ? C11 O10 Cs1 160.0(18) . 13_454 ? O10 C11 C12 106.2(11) . . ? O10 C11 Cs1 109.3(19) . 14_544 ? C12 C11 Cs1 126(3) . 14_544 ? O10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? Cs1 C11 H11A 17.4 14_544 . ? O10 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? Cs1 C11 H11B 93.8 14_544 . ? H11A C11 H11B 108.7 . . ? C13 C12 C11 101.1(12) . . ? C13 C12 Cs1 100(2) . 1_565 ? C11 C12 Cs1 129(3) . 1_565 ? C13 C12 H12A 111.6 . . ? C11 C12 H12A 111.6 . . ? Cs1 C12 H12A 18.1 1_565 . ? C13 C12 H12B 111.6 . . ? C11 C12 H12B 111.6 . . ? Cs1 C12 H12B 102.2 1_565 . ? H12A C12 H12B 109.4 . . ? C14 C13 C12 102.2(11) . . ? C14 C13 H13A 111.3 . . ? C12 C13 H13A 111.3 . . ? C14 C13 H13B 111.3 . . ? C12 C13 H13B 111.3 . . ? H13A C13 H13B 109.2 . . ? O10 C14 C13 109.2(9) . . ? O10 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? O10 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O4 1.191(5) 1.191(5) 2.383(9) 180.0 19_755 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.457 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.080 #===END data_p-1 _database_code_depnum_ccdc_archive 'CCDC 639853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H16 Cs2 Fe4 O15' _chemical_formula_weight 997.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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 9.3755(11) _cell_length_b 9.4461(11) _cell_length_c 17.669(2) _cell_angle_alpha 90.984(2) _cell_angle_beta 96.280(2) _cell_angle_gamma 101.695(2) _cell_volume 1521.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7504 _cell_measurement_theta_min 2.2035 _cell_measurement_theta_max 28.1895 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 4.292 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4960 _exptl_absorpt_correction_T_max 0.6269 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16581 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6562 _reflns_number_gt 5376 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The following restraints were applied in order to obtain a satisfatctory model: simu .005 $c; simu .01 $o; simu .005 o20 > c34;isor .005 c21 > c24;isor .005 c31 > c34 ; _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^)+(0.0332P)^2^+1.0137P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6562 _refine_ls_number_parameters 379 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.94511(6) 0.73707(6) 0.20379(3) 0.01609(12) Uani 1 1 d . . . Fe2 Fe 1.10570(6) 0.89611(6) 0.31572(3) 0.01539(12) Uani 1 1 d . . . Fe3 Fe 1.10939(6) 0.62641(6) 0.30432(3) 0.01576(12) Uani 1 1 d . . . Fe4 Fe 1.23035(6) 0.80009(6) 0.21085(3) 0.01550(12) Uani 1 1 d . . . C1 C 0.8821(4) 0.8837(4) 0.1587(2) 0.0205(9) Uani 1 1 d . . . C2 C 0.9282(4) 0.6205(4) 0.1232(2) 0.0190(8) Uani 1 1 d . . . C3 C 0.7770(4) 0.6534(4) 0.2382(2) 0.0208(9) Uani 1 1 d . . . C4 C 1.1542(4) 1.0503(4) 0.2617(2) 0.0199(9) Uani 1 1 d . . . C5 C 0.9197(5) 0.8983(4) 0.3273(2) 0.0216(9) Uani 1 1 d . . . C6 C 1.1734(5) 0.9807(4) 0.4060(3) 0.0241(9) Uani 1 1 d . . . C7 C 1.0043(4) 0.6466(4) 0.3787(2) 0.0196(9) Uani 1 1 d . . . C8 C 1.2271(4) 0.5291(4) 0.3559(2) 0.0185(8) Uani 1 1 d . . . C9 C 1.0032(4) 0.4706(5) 0.2521(2) 0.0197(9) Uani 1 1 d . . . C10 C 1.2389(4) 0.6237(5) 0.1805(3) 0.0244(9) Uani 1 1 d . . . C11 C 1.4185(5) 0.8738(4) 0.2054(2) 0.0222(9) Uani 1 1 d . . . C12 C 1.1710(4) 0.8801(4) 0.1268(2) 0.0178(8) Uani 1 1 d . . . C13 C 1.2844(4) 0.8086(4) 0.3239(2) 0.0206(9) Uani 1 1 d . . . O1 O 0.8419(3) 0.9778(3) 0.12840(19) 0.0299(7) Uani 1 1 d . . . O2 O 0.9157(3) 0.5436(3) 0.06958(17) 0.0268(7) Uani 1 1 d . . . O3 O 0.6677(3) 0.5989(3) 0.25841(19) 0.0312(7) Uani 1 1 d . . . O4 O 1.1813(3) 1.1589(3) 0.23118(18) 0.0274(7) Uani 1 1 d . . . O5 O 0.8058(3) 0.9095(3) 0.34338(18) 0.0265(7) Uani 1 1 d . . . O6 O 1.2159(4) 1.0390(4) 0.46382(19) 0.0404(9) Uani 1 1 d . . . O7 O 0.9348(3) 0.6410(3) 0.43000(18) 0.0253(7) Uani 1 1 d . . . O8 O 1.3003(3) 0.4642(3) 0.39096(18) 0.0269(7) Uani 1 1 d . . . O9 O 0.9429(3) 0.3621(3) 0.22223(17) 0.0254(7) Uani 1 1 d . . . O10 O 1.2566(3) 0.5179(3) 0.15139(19) 0.0302(7) Uani 1 1 d . . . O11 O 1.5407(3) 0.9151(4) 0.1996(2) 0.0348(8) Uani 1 1 d . . . O12 O 1.1452(3) 0.9349(3) 0.06973(17) 0.0236(6) Uani 1 1 d . . . O13 O 1.3961(3) 0.8267(3) 0.36604(17) 0.0225(6) Uani 1 1 d . . . Cs1 Cs 0.61906(2) 0.67962(3) 0.442810(15) 0.01865(7) Uani 1 1 d . . . Cs2 Cs 0.94430(3) 0.75180(3) -0.070565(15) 0.02051(7) Uani 1 1 d . . . O20 O 0.4104(3) 0.6537(3) 0.56945(17) 0.0267(6) Uani 1 1 d U . . C21 C 0.2744(5) 0.6936(5) 0.5403(3) 0.0293(9) Uani 1 1 d U . . H21A H 0.2046 0.6086 0.5152 0.035 Uiso 1 1 calc R . . H21B H 0.2923 0.7698 0.5027 0.035 Uiso 1 1 calc R . . C22 C 0.2142(5) 0.7484(6) 0.6074(3) 0.0372(10) Uani 1 1 d U . . H22A H 0.1464 0.6698 0.6295 0.045 Uiso 1 1 calc R . . H22B H 0.1619 0.8270 0.5932 0.045 Uiso 1 1 calc R . . C23 C 0.3507(6) 0.8043(7) 0.6627(4) 0.0535(13) Uani 1 1 d U . . H23A H 0.3817 0.9106 0.6599 0.064 Uiso 1 1 calc R . . H23B H 0.3312 0.7815 0.7155 0.064 Uiso 1 1 calc R . . C24 C 0.4644(6) 0.7326(6) 0.6403(3) 0.0396(11) Uani 1 1 d U . . H24A H 0.5543 0.8053 0.6344 0.048 Uiso 1 1 calc R . . H24B H 0.4887 0.6658 0.6800 0.048 Uiso 1 1 calc R . . O30 O 0.6296(4) 0.7214(5) -0.0434(2) 0.0481(9) Uani 1 1 d U . . C31 C 0.5328(6) 0.7203(8) -0.1117(4) 0.0592(13) Uani 1 1 d U . . H31A H 0.5185 0.6261 -0.1399 0.071 Uiso 1 1 calc R . . H31B H 0.5753 0.7974 -0.1449 0.071 Uiso 1 1 calc R . . C32 C 0.3932(6) 0.7442(8) -0.0918(4) 0.0571(13) Uani 1 1 d U . . H32A H 0.3110 0.6727 -0.1191 0.068 Uiso 1 1 calc R . . H32B H 0.3802 0.8427 -0.1047 0.068 Uiso 1 1 calc R . . C33 C 0.3996(7) 0.7264(9) -0.0089(4) 0.0677(15) Uani 1 1 d U . . H33A H 0.3564 0.8003 0.0154 0.081 Uiso 1 1 calc R . . H33B H 0.3450 0.6293 0.0023 0.081 Uiso 1 1 calc R . . C34 C 0.5526(7) 0.7436(9) 0.0187(4) 0.0660(14) Uani 1 1 d U . . H34A H 0.5906 0.8420 0.0420 0.079 Uiso 1 1 calc R . . H34B H 0.5658 0.6725 0.0581 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0134(3) 0.0138(3) 0.0203(3) -0.0018(2) 0.0000(2) 0.0024(2) Fe2 0.0162(3) 0.0115(3) 0.0186(3) -0.0032(2) 0.0017(2) 0.0039(2) Fe3 0.0135(3) 0.0115(3) 0.0225(3) 0.0002(2) 0.0019(2) 0.0033(2) Fe4 0.0132(3) 0.0132(3) 0.0200(3) -0.0018(2) 0.0033(2) 0.0019(2) C1 0.0125(18) 0.022(2) 0.026(2) -0.0020(18) 0.0041(17) 0.0007(16) C2 0.0183(19) 0.016(2) 0.023(2) 0.0034(17) 0.0028(17) 0.0034(16) C3 0.023(2) 0.018(2) 0.022(2) -0.0016(17) 0.0011(18) 0.0063(17) C4 0.0182(19) 0.022(2) 0.019(2) -0.0045(17) -0.0006(17) 0.0051(17) C5 0.030(2) 0.0114(19) 0.024(2) -0.0022(17) 0.0040(18) 0.0041(17) C6 0.031(2) 0.014(2) 0.027(2) -0.0011(18) -0.0008(19) 0.0035(17) C7 0.0151(18) 0.016(2) 0.027(2) -0.0027(17) -0.0037(17) 0.0059(16) C8 0.0161(19) 0.0154(19) 0.023(2) -0.0042(17) 0.0039(17) 0.0013(16) C9 0.0158(19) 0.025(2) 0.021(2) 0.0045(18) 0.0061(16) 0.0070(17) C10 0.018(2) 0.019(2) 0.035(3) -0.0002(19) 0.0002(18) 0.0007(17) C11 0.023(2) 0.021(2) 0.021(2) -0.0029(17) 0.0031(17) 0.0020(17) C12 0.0162(18) 0.0111(18) 0.027(2) -0.0052(16) 0.0073(17) 0.0017(15) C13 0.0175(19) 0.018(2) 0.027(2) 0.0018(17) 0.0031(17) 0.0038(16) O1 0.0222(15) 0.0225(16) 0.046(2) 0.0089(15) 0.0023(14) 0.0067(13) O2 0.0334(17) 0.0222(16) 0.0243(17) -0.0019(13) 0.0048(14) 0.0042(13) O3 0.0244(16) 0.0282(17) 0.040(2) 0.0003(15) 0.0114(15) 0.0000(13) O4 0.0338(17) 0.0190(16) 0.0294(17) 0.0037(13) 0.0052(14) 0.0044(13) O5 0.0233(15) 0.0207(16) 0.0387(19) -0.0024(14) 0.0115(14) 0.0085(13) O6 0.060(2) 0.0293(19) 0.0260(19) -0.0132(15) -0.0078(17) 0.0048(17) O7 0.0213(15) 0.0254(16) 0.0309(17) -0.0003(13) 0.0080(13) 0.0064(13) O8 0.0263(16) 0.0222(16) 0.0331(18) 0.0004(13) -0.0031(14) 0.0103(13) O9 0.0300(16) 0.0175(15) 0.0260(17) -0.0058(13) -0.0017(13) 0.0016(13) O10 0.0315(17) 0.0183(16) 0.041(2) -0.0071(14) 0.0087(15) 0.0038(13) O11 0.0192(16) 0.041(2) 0.042(2) -0.0059(16) 0.0085(14) -0.0026(14) O12 0.0265(16) 0.0224(15) 0.0225(16) 0.0030(13) 0.0034(13) 0.0058(13) O13 0.0181(14) 0.0217(15) 0.0259(16) -0.0015(12) -0.0025(12) 0.0027(12) Cs1 0.01430(12) 0.01760(13) 0.02467(14) -0.00128(10) 0.00325(10) 0.00435(9) Cs2 0.02531(14) 0.01410(13) 0.02168(14) -0.00087(10) 0.00147(10) 0.00380(10) O20 0.0284(15) 0.0261(15) 0.0277(15) -0.0056(13) 0.0052(13) 0.0101(12) C21 0.0313(19) 0.0292(19) 0.032(2) 0.0054(17) 0.0075(17) 0.0142(16) C22 0.037(2) 0.035(2) 0.043(2) -0.0090(19) 0.0124(19) 0.0116(18) C23 0.050(2) 0.056(2) 0.056(2) -0.024(2) 0.003(2) 0.020(2) C24 0.040(2) 0.039(2) 0.038(2) -0.0135(19) 0.0049(19) 0.0058(18) O30 0.0294(17) 0.073(2) 0.046(2) -0.0071(18) 0.0069(15) 0.0197(17) C31 0.045(2) 0.081(3) 0.056(3) 0.000(2) 0.008(2) 0.023(2) C32 0.042(2) 0.074(3) 0.059(3) 0.006(2) 0.011(2) 0.017(2) C33 0.050(2) 0.091(3) 0.063(3) -0.009(3) 0.011(2) 0.015(2) C34 0.049(2) 0.092(3) 0.058(3) -0.015(2) 0.005(2) 0.020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.758(4) . ? Fe1 C1 1.781(4) . ? Fe1 C3 1.788(4) . ? Fe1 Fe3 2.5958(8) . ? Fe1 Fe2 2.6008(8) . ? Fe1 Fe4 2.6079(8) . ? Fe2 C4 1.764(4) . ? Fe2 C6 1.766(5) . ? Fe2 C5 1.782(4) . ? Fe2 C13 2.006(4) . ? Fe2 Fe4 2.5431(8) . ? Fe2 Fe3 2.5596(8) . ? Fe3 C7 1.756(4) . ? Fe3 C8 1.764(4) . ? Fe3 C9 1.780(4) . ? Fe3 C13 2.117(4) . ? Fe3 Fe4 2.5404(8) . ? Fe4 C10 1.762(4) . ? Fe4 C12 1.764(4) . ? Fe4 C11 1.774(4) . ? Fe4 C13 2.002(4) . ? C1 O1 1.152(5) . ? C2 O2 1.166(5) . ? C2 Cs2 3.670(4) . ? C3 O3 1.147(5) . ? C4 O4 1.162(5) . ? C5 O5 1.160(5) . ? C6 O6 1.143(5) . ? C7 O7 1.169(5) . ? C8 O8 1.150(5) . ? C8 Cs1 3.802(4) 1_655 ? C9 O9 1.153(5) . ? C10 O10 1.165(5) . ? C11 O11 1.150(5) . ? C12 O12 1.167(5) . ? C12 Cs2 3.917(4) . ? C13 O13 1.197(5) . ? O1 Cs2 3.170(3) 2_775 ? O2 Cs2 3.189(3) . ? O2 Cs2 3.315(3) 2_765 ? O3 Cs1 3.433(3) . ? O4 Cs2 3.148(3) 2_775 ? O5 Cs1 3.183(3) . ? O6 Cs1 3.131(3) 2_776 ? O7 Cs1 3.087(3) . ? O8 Cs1 3.284(3) 1_655 ? O8 Cs1 3.333(3) 2_766 ? O9 Cs2 3.231(3) 2_765 ? O10 Cs2 3.069(3) 2_765 ? O12 Cs2 3.193(3) . ? O12 Cs2 3.236(3) 2_775 ? O13 Cs1 2.960(3) 1_655 ? Cs1 O13 2.960(3) 1_455 ? Cs1 O20 3.106(3) 2_666 ? Cs1 O20 3.111(3) . ? Cs1 O6 3.131(3) 2_776 ? Cs1 O8 3.284(3) 1_455 ? Cs1 O8 3.333(3) 2_766 ? Cs1 C8 3.802(4) 1_455 ? Cs1 C21 3.849(4) . ? Cs1 C21 3.862(4) 2_666 ? Cs2 O30 2.998(3) . ? Cs2 O10 3.069(3) 2_765 ? Cs2 O4 3.148(3) 2_775 ? Cs2 O1 3.170(3) 2_775 ? Cs2 O9 3.231(3) 2_765 ? Cs2 O12 3.236(3) 2_775 ? Cs2 O2 3.315(3) 2_765 ? Cs2 C31 3.797(6) . ? O20 C24 1.434(6) . ? O20 C21 1.446(5) . ? O20 Cs1 3.106(3) 2_666 ? C21 C22 1.496(6) . ? C21 Cs1 3.862(4) 2_666 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.518(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.458(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O30 C34 1.413(7) . ? O30 C31 1.428(7) . ? C31 C32 1.451(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.473(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.439(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? 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 C2 Fe1 C1 98.67(19) . . ? C2 Fe1 C3 96.66(18) . . ? C1 Fe1 C3 97.65(18) . . ? C2 Fe1 Fe3 103.07(13) . . ? C1 Fe1 Fe3 153.59(14) . . ? C3 Fe1 Fe3 94.57(13) . . ? C2 Fe1 Fe2 150.53(13) . . ? C1 Fe1 Fe2 94.90(14) . . ? C3 Fe1 Fe2 107.33(14) . . ? Fe3 Fe1 Fe2 59.02(2) . . ? C2 Fe1 Fe4 92.56(13) . . ? C1 Fe1 Fe4 106.10(12) . . ? C3 Fe1 Fe4 152.89(13) . . ? Fe3 Fe1 Fe4 58.44(2) . . ? Fe2 Fe1 Fe4 58.45(2) . . ? C4 Fe2 C6 96.82(19) . . ? C4 Fe2 C5 101.79(18) . . ? C6 Fe2 C5 93.6(2) . . ? C4 Fe2 C13 103.85(17) . . ? C6 Fe2 C13 86.99(19) . . ? C5 Fe2 C13 154.09(17) . . ? C4 Fe2 Fe4 77.62(13) . . ? C6 Fe2 Fe4 132.57(15) . . ? C5 Fe2 Fe4 133.79(14) . . ? C13 Fe2 Fe4 50.54(12) . . ? C4 Fe2 Fe3 136.98(14) . . ? C6 Fe2 Fe3 115.32(13) . . ? C5 Fe2 Fe3 103.75(13) . . ? C13 Fe2 Fe3 53.61(12) . . ? Fe4 Fe2 Fe3 59.72(2) . . ? C4 Fe2 Fe1 95.48(13) . . ? C6 Fe2 Fe1 163.67(15) . . ? C5 Fe2 Fe1 73.34(14) . . ? C13 Fe2 Fe1 100.44(13) . . ? Fe4 Fe2 Fe1 60.91(2) . . ? Fe3 Fe2 Fe1 60.39(2) . . ? C7 Fe3 C8 96.22(18) . . ? C7 Fe3 C9 102.69(18) . . ? C8 Fe3 C9 94.09(18) . . ? C7 Fe3 C13 102.33(18) . . ? C8 Fe3 C13 86.36(17) . . ? C9 Fe3 C13 154.77(17) . . ? C7 Fe3 Fe4 133.36(13) . . ? C8 Fe3 Fe4 114.82(13) . . ? C9 Fe3 Fe4 108.46(13) . . ? C13 Fe3 Fe4 49.89(12) . . ? C7 Fe3 Fe2 73.68(13) . . ? C8 Fe3 Fe2 128.82(13) . . ? C9 Fe3 Fe2 137.02(13) . . ? C13 Fe3 Fe2 49.70(11) . . ? Fe4 Fe3 Fe2 59.82(2) . . ? C7 Fe3 Fe1 94.22(13) . . ? C8 Fe3 Fe1 167.78(13) . . ? C9 Fe3 Fe1 77.38(13) . . ? C13 Fe3 Fe1 97.62(11) . . ? Fe4 Fe3 Fe1 61.02(2) . . ? Fe2 Fe3 Fe1 60.59(2) . . ? C10 Fe4 C12 104.18(19) . . ? C10 Fe4 C11 95.05(19) . . ? C12 Fe4 C11 93.75(18) . . ? C10 Fe4 C13 105.21(19) . . ? C12 Fe4 C13 150.52(17) . . ? C11 Fe4 C13 85.89(18) . . ? C10 Fe4 Fe3 72.44(15) . . ? C12 Fe4 Fe3 135.91(13) . . ? C11 Fe4 Fe3 130.18(14) . . ? C13 Fe4 Fe3 54.01(12) . . ? C10 Fe4 Fe2 132.61(14) . . ? C12 Fe4 Fe2 105.68(13) . . ? C11 Fe4 Fe2 118.55(14) . . ? C13 Fe4 Fe2 50.68(12) . . ? Fe3 Fe4 Fe2 60.46(2) . . ? C10 Fe4 Fe1 92.68(13) . . ? C12 Fe4 Fe1 76.04(12) . . ? C11 Fe4 Fe1 168.48(14) . . ? C13 Fe4 Fe1 100.32(12) . . ? Fe3 Fe4 Fe1 60.54(2) . . ? Fe2 Fe4 Fe1 60.64(2) . . ? O1 C1 Fe1 178.9(4) . . ? O2 C2 Fe1 179.3(4) . . ? O2 C2 Cs2 57.0(2) . . ? Fe1 C2 Cs2 122.72(17) . . ? O3 C3 Fe1 178.3(4) . . ? O4 C4 Fe2 173.8(4) . . ? O5 C5 Fe2 171.3(4) . . ? O6 C6 Fe2 178.0(4) . . ? O7 C7 Fe3 171.0(4) . . ? O8 C8 Fe3 177.8(4) . . ? O8 C8 Cs1 55.1(2) . 1_655 ? Fe3 C8 Cs1 126.23(17) . 1_655 ? O9 C9 Fe3 173.4(4) . . ? O10 C10 Fe4 169.2(4) . . ? O11 C11 Fe4 176.3(4) . . ? O12 C12 Fe4 173.6(3) . . ? O12 C12 Cs2 44.6(2) . . ? Fe4 C12 Cs2 137.45(17) . . ? O13 C13 Fe4 135.9(3) . . ? O13 C13 Fe2 134.9(3) . . ? Fe4 C13 Fe2 78.78(15) . . ? O13 C13 Fe3 130.7(3) . . ? Fe4 C13 Fe3 76.10(15) . . ? Fe2 C13 Fe3 76.69(14) . . ? C1 O1 Cs2 123.4(3) . 2_775 ? C2 O2 Cs2 105.1(3) . . ? C2 O2 Cs2 122.5(3) . 2_765 ? Cs2 O2 Cs2 120.19(9) . 2_765 ? C3 O3 Cs1 116.5(3) . . ? C4 O4 Cs2 130.3(3) . 2_775 ? C5 O5 Cs1 122.4(3) . . ? C6 O6 Cs1 149.1(3) . 2_776 ? C7 O7 Cs1 132.4(3) . . ? C8 O8 Cs1 108.2(3) . 1_655 ? C8 O8 Cs1 147.4(3) . 2_766 ? Cs1 O8 Cs1 81.70(7) 1_655 2_766 ? C9 O9 Cs2 119.8(3) . 2_765 ? C10 O10 Cs2 135.4(3) . 2_765 ? C12 O12 Cs2 120.5(3) . . ? C12 O12 Cs2 120.5(3) . 2_775 ? Cs2 O12 Cs2 105.93(8) . 2_775 ? C13 O13 Cs1 144.1(3) . 1_655 ? O13 Cs1 O7 139.92(8) 1_455 . ? O13 Cs1 O20 122.35(8) 1_455 2_666 ? O7 Cs1 O20 76.12(8) . 2_666 ? O13 Cs1 O20 81.73(8) 1_455 . ? O7 Cs1 O20 136.51(8) . . ? O20 Cs1 O20 91.76(8) 2_666 . ? O13 Cs1 O6 92.85(9) 1_455 2_776 ? O7 Cs1 O6 82.37(9) . 2_776 ? O20 Cs1 O6 143.62(9) 2_666 2_776 ? O20 Cs1 O6 83.97(9) . 2_776 ? O13 Cs1 O5 77.01(8) 1_455 . ? O7 Cs1 O5 64.52(8) . . ? O20 Cs1 O5 125.91(8) 2_666 . ? O20 Cs1 O5 142.32(8) . . ? O6 Cs1 O5 66.60(9) 2_776 . ? O13 Cs1 O8 65.94(7) 1_455 1_455 ? O7 Cs1 O8 131.28(8) . 1_455 ? O20 Cs1 O8 59.00(7) 2_666 1_455 ? O20 Cs1 O8 67.25(8) . 1_455 ? O6 Cs1 O8 145.79(9) 2_776 1_455 ? O5 Cs1 O8 127.97(8) . 1_455 ? O13 Cs1 O8 140.00(8) 1_455 2_766 ? O7 Cs1 O8 78.68(8) . 2_766 ? O20 Cs1 O8 66.68(8) 2_666 2_766 ? O20 Cs1 O8 58.41(7) . 2_766 ? O6 Cs1 O8 80.65(8) 2_776 2_766 ? O5 Cs1 O8 132.77(8) . 2_766 ? O8 Cs1 O8 98.30(7) 1_455 2_766 ? O13 Cs1 O3 82.44(8) 1_455 . ? O7 Cs1 O3 68.40(8) . . ? O20 Cs1 O3 73.86(8) 2_666 . ? O20 Cs1 O3 148.13(8) . . ? O6 Cs1 O3 124.34(9) 2_776 . ? O5 Cs1 O3 58.26(8) . . ? O8 Cs1 O3 81.05(7) 1_455 . ? O8 Cs1 O3 133.38(8) 2_766 . ? O13 Cs1 C8 49.37(8) 1_455 1_455 ? O7 Cs1 C8 140.37(8) . 1_455 ? O20 Cs1 C8 74.40(8) 2_666 1_455 ? O20 Cs1 C8 70.37(8) . 1_455 ? O6 Cs1 C8 135.85(9) 2_776 1_455 ? O5 Cs1 C8 114.91(8) . 1_455 ? O8 Cs1 C8 16.70(7) 1_455 1_455 ? O8 Cs1 C8 112.30(8) 2_766 1_455 ? O3 Cs1 C8 78.32(8) . 1_455 ? O13 Cs1 C21 61.45(9) 1_455 . ? O7 Cs1 C21 157.17(9) . . ? O20 Cs1 C21 99.06(9) 2_666 . ? O20 Cs1 C21 20.70(8) . . ? O6 Cs1 C21 89.53(10) 2_776 . ? O5 Cs1 C21 130.99(8) . . ? O8 Cs1 C21 57.13(9) 1_455 . ? O8 Cs1 C21 78.96(8) 2_766 . ? O3 Cs1 C21 132.39(9) . . ? C8 Cs1 C21 54.95(10) 1_455 . ? O13 Cs1 C21 142.26(9) 1_455 2_666 ? O7 Cs1 C21 58.20(9) . 2_666 ? O20 Cs1 C21 20.50(9) 2_666 2_666 ? O20 Cs1 C21 98.71(9) . 2_666 ? O6 Cs1 C21 124.83(10) 2_776 2_666 ? O5 Cs1 C21 117.10(8) . 2_666 ? O8 Cs1 C21 79.35(9) 1_455 2_666 ? O8 Cs1 C21 56.66(9) 2_766 2_666 ? O3 Cs1 C21 77.80(9) . 2_666 ? C8 Cs1 C21 94.90(9) 1_455 2_666 ? C21 Cs1 C21 111.70(7) . 2_666 ? O30 Cs2 O10 66.83(10) . 2_765 ? O30 Cs2 O4 81.28(9) . 2_775 ? O10 Cs2 O4 72.14(8) 2_765 2_775 ? O30 Cs2 O1 128.80(10) . 2_775 ? O10 Cs2 O1 133.46(9) 2_765 2_775 ? O4 Cs2 O1 68.90(8) 2_775 2_775 ? O30 Cs2 O2 76.74(10) . . ? O10 Cs2 O2 80.48(8) 2_765 . ? O4 Cs2 O2 149.98(8) 2_775 . ? O1 Cs2 O2 141.12(8) 2_775 . ? O30 Cs2 O12 108.39(9) . . ? O10 Cs2 O12 155.34(8) 2_765 . ? O4 Cs2 O12 132.20(7) 2_775 . ? O1 Cs2 O12 69.34(8) 2_775 . ? O2 Cs2 O12 74.92(7) . . ? O30 Cs2 O9 125.36(9) . 2_765 ? O10 Cs2 O9 65.06(8) 2_765 2_765 ? O4 Cs2 O9 60.67(8) 2_775 2_765 ? O1 Cs2 O9 74.11(8) 2_775 2_765 ? O2 Cs2 O9 118.07(8) . 2_765 ? O12 Cs2 O9 126.11(7) . 2_765 ? O30 Cs2 O12 69.61(10) . 2_775 ? O10 Cs2 O12 122.52(8) 2_765 2_775 ? O4 Cs2 O12 65.77(8) 2_775 2_775 ? O1 Cs2 O12 60.52(7) 2_775 2_775 ? O2 Cs2 O12 123.07(8) . 2_775 ? O12 Cs2 O12 74.07(8) . 2_775 ? O9 Cs2 O12 118.82(7) 2_765 2_775 ? O30 Cs2 O2 118.19(10) . 2_765 ? O10 Cs2 O2 64.59(8) 2_765 2_765 ? O4 Cs2 O2 115.96(8) 2_775 2_765 ? O1 Cs2 O2 112.18(8) 2_775 2_765 ? O2 Cs2 O2 59.81(9) . 2_765 ? O12 Cs2 O2 100.60(7) . 2_765 ? O9 Cs2 O2 59.21(7) 2_765 2_765 ? O12 Cs2 O2 171.96(7) 2_775 2_765 ? O30 Cs2 C2 75.07(10) . . ? O10 Cs2 C2 96.10(9) 2_765 . ? O4 Cs2 C2 156.24(8) 2_775 . ? O1 Cs2 C2 129.04(9) 2_775 . ? O2 Cs2 C2 17.85(8) . . ? O12 Cs2 C2 59.93(8) . . ? O9 Cs2 C2 133.76(8) 2_765 . ? O12 Cs2 C2 107.00(8) 2_775 . ? O2 Cs2 C2 74.55(9) 2_765 . ? O30 Cs2 C31 20.20(12) . . ? O10 Cs2 C31 58.06(12) 2_765 . ? O4 Cs2 C31 61.78(11) 2_775 . ? O1 Cs2 C31 119.23(12) 2_775 . ? O2 Cs2 C31 93.43(12) . . ? O12 Cs2 C31 124.62(12) . . ? O9 Cs2 C31 107.38(11) 2_765 . ? O12 Cs2 C31 68.07(12) 2_775 . ? O2 Cs2 C31 119.89(12) 2_765 . ? C2 Cs2 C31 94.46(12) . . ? O30 Cs2 C12 105.17(9) . . ? O10 Cs2 C12 140.52(8) 2_765 . ? O4 Cs2 C12 146.97(8) 2_775 . ? O1 Cs2 C12 82.88(8) 2_775 . ? O2 Cs2 C12 60.29(8) . . ? O12 Cs2 C12 14.86(7) . . ? O9 Cs2 C12 128.38(8) 2_765 . ? O12 Cs2 C12 85.82(8) 2_775 . ? O2 Cs2 C12 89.95(8) 2_765 . ? C2 Cs2 C12 46.16(8) . . ? C31 Cs2 C12 124.15(11) . . ? C24 O20 C21 108.4(3) . . ? C24 O20 Cs1 120.7(3) . 2_666 ? C21 O20 Cs1 110.7(2) . 2_666 ? C24 O20 Cs1 117.7(3) . . ? C21 O20 Cs1 109.8(2) . . ? Cs1 O20 Cs1 88.24(7) 2_666 . ? O20 C21 C22 106.4(4) . . ? O20 C21 Cs1 49.52(19) . . ? C22 C21 Cs1 146.4(3) . . ? O20 C21 Cs1 48.81(19) . 2_666 ? C22 C21 Cs1 116.6(3) . 2_666 ? Cs1 C21 Cs1 68.30(7) . 2_666 ? O20 C21 H21A 110.4 . . ? C22 C21 H21A 110.4 . . ? Cs1 C21 H21A 101.0 . . ? Cs1 C21 H21A 62.2 2_666 . ? O20 C21 H21B 110.4 . . ? C22 C21 H21B 110.4 . . ? Cs1 C21 H21B 68.2 . . ? Cs1 C21 H21B 132.2 2_666 . ? H21A C21 H21B 108.6 . . ? C21 C22 C23 103.0(4) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C24 C23 C22 106.8(4) . . ? C24 C23 H23A 110.4 . . ? C22 C23 H23A 110.4 . . ? C24 C23 H23B 110.4 . . ? C22 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? O20 C24 C23 108.3(4) . . ? O20 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? O20 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C34 O30 C31 107.8(4) . . ? C34 O30 Cs2 136.6(3) . . ? C31 O30 Cs2 113.3(3) . . ? O30 C31 C32 108.7(5) . . ? O30 C31 Cs2 46.5(2) . . ? C32 C31 Cs2 152.2(5) . . ? O30 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? Cs2 C31 H31A 93.1 . . ? O30 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? Cs2 C31 H31B 75.5 . . ? H31A C31 H31B 108.3 . . ? C31 C32 C33 105.0(5) . . ? C31 C32 H32A 110.7 . . ? C33 C32 H32A 110.7 . . ? C31 C32 H32B 110.7 . . ? C33 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C34 C33 C32 106.0(6) . . ? C34 C33 H33A 110.5 . . ? C32 C33 H33A 110.5 . . ? C34 C33 H33B 110.5 . . ? C32 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? O30 C34 C33 108.4(5) . . ? O30 C34 H34A 110.0 . . ? C33 C34 H34A 110.0 . . ? O30 C34 H34B 110.0 . . ? C33 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Fe1 Fe2 C4 84.0(3) . . . . ? C1 Fe1 Fe2 C4 -33.35(18) . . . . ? C3 Fe1 Fe2 C4 -132.94(19) . . . . ? Fe3 Fe1 Fe2 C4 142.21(13) . . . . ? Fe4 Fe1 Fe2 C4 72.56(13) . . . . ? C2 Fe1 Fe2 C6 -137.3(5) . . . . ? C1 Fe1 Fe2 C6 105.4(5) . . . . ? C3 Fe1 Fe2 C6 5.8(5) . . . . ? Fe3 Fe1 Fe2 C6 -79.0(5) . . . . ? Fe4 Fe1 Fe2 C6 -148.7(5) . . . . ? C2 Fe1 Fe2 C5 -175.3(3) . . . . ? C1 Fe1 Fe2 C5 67.34(18) . . . . ? C3 Fe1 Fe2 C5 -32.25(19) . . . . ? Fe3 Fe1 Fe2 C5 -117.09(14) . . . . ? Fe4 Fe1 Fe2 C5 173.25(14) . . . . ? C2 Fe1 Fe2 C13 -21.2(3) . . . . ? C1 Fe1 Fe2 C13 -138.55(17) . . . . ? C3 Fe1 Fe2 C13 121.85(18) . . . . ? Fe3 Fe1 Fe2 C13 37.01(12) . . . . ? Fe4 Fe1 Fe2 C13 -32.65(12) . . . . ? C2 Fe1 Fe2 Fe4 11.4(3) . . . . ? C1 Fe1 Fe2 Fe4 -105.90(13) . . . . ? C3 Fe1 Fe2 Fe4 154.50(14) . . . . ? Fe3 Fe1 Fe2 Fe4 69.66(2) . . . . ? C2 Fe1 Fe2 Fe3 -58.2(3) . . . . ? C1 Fe1 Fe2 Fe3 -175.56(13) . . . . ? C3 Fe1 Fe2 Fe3 84.84(13) . . . . ? Fe4 Fe1 Fe2 Fe3 -69.66(2) . . . . ? C4 Fe2 Fe3 C7 -168.0(2) . . . . ? C6 Fe2 Fe3 C7 57.6(2) . . . . ? C5 Fe2 Fe3 C7 -43.25(19) . . . . ? C13 Fe2 Fe3 C7 122.7(2) . . . . ? Fe4 Fe2 Fe3 C7 -176.26(13) . . . . ? Fe1 Fe2 Fe3 C7 -104.66(13) . . . . ? C4 Fe2 Fe3 C8 107.2(3) . . . . ? C6 Fe2 Fe3 C8 -27.2(2) . . . . ? C5 Fe2 Fe3 C8 -128.0(2) . . . . ? C13 Fe2 Fe3 C8 37.9(2) . . . . ? Fe4 Fe2 Fe3 C8 98.94(17) . . . . ? Fe1 Fe2 Fe3 C8 170.54(17) . . . . ? C4 Fe2 Fe3 C9 -76.8(3) . . . . ? C6 Fe2 Fe3 C9 148.8(2) . . . . ? C5 Fe2 Fe3 C9 48.0(2) . . . . ? C13 Fe2 Fe3 C9 -146.1(2) . . . . ? Fe4 Fe2 Fe3 C9 -85.02(19) . . . . ? Fe1 Fe2 Fe3 C9 -13.42(19) . . . . ? C4 Fe2 Fe3 C13 69.3(2) . . . . ? C6 Fe2 Fe3 C13 -65.1(2) . . . . ? C5 Fe2 Fe3 C13 -165.9(2) . . . . ? Fe4 Fe2 Fe3 C13 61.06(15) . . . . ? Fe1 Fe2 Fe3 C13 132.66(15) . . . . ? C4 Fe2 Fe3 Fe4 8.22(19) . . . . ? C6 Fe2 Fe3 Fe4 -126.18(16) . . . . ? C5 Fe2 Fe3 Fe4 133.01(14) . . . . ? C13 Fe2 Fe3 Fe4 -61.06(15) . . . . ? Fe1 Fe2 Fe3 Fe4 71.60(3) . . . . ? C4 Fe2 Fe3 Fe1 -63.39(19) . . . . ? C6 Fe2 Fe3 Fe1 162.22(16) . . . . ? C5 Fe2 Fe3 Fe1 61.41(14) . . . . ? C13 Fe2 Fe3 Fe1 -132.66(15) . . . . ? Fe4 Fe2 Fe3 Fe1 -71.60(3) . . . . ? C2 Fe1 Fe3 C7 -136.83(18) . . . . ? C1 Fe1 Fe3 C7 78.6(3) . . . . ? C3 Fe1 Fe3 C7 -38.89(19) . . . . ? Fe2 Fe1 Fe3 C7 68.59(13) . . . . ? Fe4 Fe1 Fe3 C7 138.26(13) . . . . ? C2 Fe1 Fe3 C8 11.8(6) . . . . ? C1 Fe1 Fe3 C8 -132.8(7) . . . . ? C3 Fe1 Fe3 C8 109.7(6) . . . . ? Fe2 Fe1 Fe3 C8 -142.8(6) . . . . ? Fe4 Fe1 Fe3 C8 -73.1(6) . . . . ? C2 Fe1 Fe3 C9 -34.75(18) . . . . ? C1 Fe1 Fe3 C9 -179.4(3) . . . . ? C3 Fe1 Fe3 C9 63.18(18) . . . . ? Fe2 Fe1 Fe3 C9 170.67(13) . . . . ? Fe4 Fe1 Fe3 C9 -119.66(13) . . . . ? C2 Fe1 Fe3 C13 120.12(17) . . . . ? C1 Fe1 Fe3 C13 -24.5(3) . . . . ? C3 Fe1 Fe3 C13 -141.95(18) . . . . ? Fe2 Fe1 Fe3 C13 -34.46(12) . . . . ? Fe4 Fe1 Fe3 C13 35.21(12) . . . . ? C2 Fe1 Fe3 Fe4 84.91(13) . . . . ? C1 Fe1 Fe3 Fe4 -59.7(3) . . . . ? C3 Fe1 Fe3 Fe4 -177.15(13) . . . . ? Fe2 Fe1 Fe3 Fe4 -69.67(2) . . . . ? C2 Fe1 Fe3 Fe2 154.58(13) . . . . ? C1 Fe1 Fe3 Fe2 10.0(3) . . . . ? C3 Fe1 Fe3 Fe2 -107.49(13) . . . . ? Fe4 Fe1 Fe3 Fe2 69.67(2) . . . . ? C7 Fe3 Fe4 C10 -169.6(2) . . . . ? C8 Fe3 Fe4 C10 63.5(2) . . . . ? C9 Fe3 Fe4 C10 -40.21(19) . . . . ? C13 Fe3 Fe4 C10 124.8(2) . . . . ? Fe2 Fe3 Fe4 C10 -174.49(14) . . . . ? Fe1 Fe3 Fe4 C10 -103.59(14) . . . . ? C7 Fe3 Fe4 C12 -77.1(3) . . . . ? C8 Fe3 Fe4 C12 156.0(2) . . . . ? C9 Fe3 Fe4 C12 52.2(2) . . . . ? C13 Fe3 Fe4 C12 -142.8(2) . . . . ? Fe2 Fe3 Fe4 C12 -82.04(18) . . . . ? Fe1 Fe3 Fe4 C12 -11.14(18) . . . . ? C7 Fe3 Fe4 C11 108.9(3) . . . . ? C8 Fe3 Fe4 C11 -18.1(2) . . . . ? C9 Fe3 Fe4 C11 -121.8(2) . . . . ? C13 Fe3 Fe4 C11 43.2(2) . . . . ? Fe2 Fe3 Fe4 C11 103.92(18) . . . . ? Fe1 Fe3 Fe4 C11 174.82(18) . . . . ? C7 Fe3 Fe4 C13 65.7(2) . . . . ? C8 Fe3 Fe4 C13 -61.2(2) . . . . ? C9 Fe3 Fe4 C13 -164.97(19) . . . . ? Fe2 Fe3 Fe4 C13 60.76(14) . . . . ? Fe1 Fe3 Fe4 C13 131.66(14) . . . . ? C7 Fe3 Fe4 Fe2 4.94(18) . . . . ? C8 Fe3 Fe4 Fe2 -122.00(15) . . . . ? C9 Fe3 Fe4 Fe2 134.28(13) . . . . ? C13 Fe3 Fe4 Fe2 -60.76(14) . . . . ? Fe1 Fe3 Fe4 Fe2 70.90(2) . . . . ? C7 Fe3 Fe4 Fe1 -65.96(18) . . . . ? C8 Fe3 Fe4 Fe1 167.10(15) . . . . ? C9 Fe3 Fe4 Fe1 63.38(13) . . . . ? C13 Fe3 Fe4 Fe1 -131.66(14) . . . . ? Fe2 Fe3 Fe4 Fe1 -70.90(2) . . . . ? C4 Fe2 Fe4 C10 -167.1(2) . . . . ? C6 Fe2 Fe4 C10 105.0(3) . . . . ? C5 Fe2 Fe4 C10 -72.6(3) . . . . ? C13 Fe2 Fe4 C10 73.0(2) . . . . ? Fe3 Fe2 Fe4 C10 7.14(19) . . . . ? Fe1 Fe2 Fe4 C10 -63.60(19) . . . . ? C4 Fe2 Fe4 C12 -39.98(18) . . . . ? C6 Fe2 Fe4 C12 -127.9(2) . . . . ? C5 Fe2 Fe4 C12 54.6(2) . . . . ? C13 Fe2 Fe4 C12 -159.8(2) . . . . ? Fe3 Fe2 Fe4 C12 134.30(13) . . . . ? Fe1 Fe2 Fe4 C12 63.56(13) . . . . ? C4 Fe2 Fe4 C11 63.3(2) . . . . ? C6 Fe2 Fe4 C11 -24.6(2) . . . . ? C5 Fe2 Fe4 C11 157.9(2) . . . . ? C13 Fe2 Fe4 C11 -56.5(2) . . . . ? Fe3 Fe2 Fe4 C11 -122.40(16) . . . . ? Fe1 Fe2 Fe4 C11 166.86(16) . . . . ? C4 Fe2 Fe4 C13 119.9(2) . . . . ? C6 Fe2 Fe4 C13 32.0(2) . . . . ? C5 Fe2 Fe4 C13 -145.6(2) . . . . ? Fe3 Fe2 Fe4 C13 -65.85(15) . . . . ? Fe1 Fe2 Fe4 C13 -136.60(15) . . . . ? C4 Fe2 Fe4 Fe3 -174.27(13) . . . . ? C6 Fe2 Fe4 Fe3 97.82(18) . . . . ? C5 Fe2 Fe4 Fe3 -79.72(18) . . . . ? C13 Fe2 Fe4 Fe3 65.85(15) . . . . ? Fe1 Fe2 Fe4 Fe3 -70.74(2) . . . . ? C4 Fe2 Fe4 Fe1 -103.53(13) . . . . ? C6 Fe2 Fe4 Fe1 168.56(18) . . . . ? C5 Fe2 Fe4 Fe1 -8.98(18) . . . . ? C13 Fe2 Fe4 Fe1 136.60(15) . . . . ? Fe3 Fe2 Fe4 Fe1 70.74(2) . . . . ? C2 Fe1 Fe4 C10 -35.69(19) . . . . ? C1 Fe1 Fe4 C10 -135.5(2) . . . . ? C3 Fe1 Fe4 C10 74.3(3) . . . . ? Fe3 Fe1 Fe4 C10 68.08(15) . . . . ? Fe2 Fe1 Fe4 C10 138.71(15) . . . . ? C2 Fe1 Fe4 C12 68.26(18) . . . . ? C1 Fe1 Fe4 C12 -31.52(19) . . . . ? C3 Fe1 Fe4 C12 178.3(3) . . . . ? Fe3 Fe1 Fe4 C12 172.04(13) . . . . ? Fe2 Fe1 Fe4 C12 -117.34(13) . . . . ? C2 Fe1 Fe4 C11 96.4(7) . . . . ? C1 Fe1 Fe4 C11 -3.4(7) . . . . ? C3 Fe1 Fe4 C11 -153.6(8) . . . . ? Fe3 Fe1 Fe4 C11 -159.8(7) . . . . ? Fe2 Fe1 Fe4 C11 -89.2(7) . . . . ? C2 Fe1 Fe4 C13 -141.69(17) . . . . ? C1 Fe1 Fe4 C13 118.53(19) . . . . ? C3 Fe1 Fe4 C13 -31.7(3) . . . . ? Fe3 Fe1 Fe4 C13 -37.91(12) . . . . ? Fe2 Fe1 Fe4 C13 32.71(12) . . . . ? C2 Fe1 Fe4 Fe3 -103.78(13) . . . . ? C1 Fe1 Fe4 Fe3 156.44(15) . . . . ? C3 Fe1 Fe4 Fe3 6.2(3) . . . . ? Fe2 Fe1 Fe4 Fe3 70.62(3) . . . . ? C2 Fe1 Fe4 Fe2 -174.40(13) . . . . ? C1 Fe1 Fe4 Fe2 85.82(15) . . . . ? C3 Fe1 Fe4 Fe2 -64.4(3) . . . . ? Fe3 Fe1 Fe4 Fe2 -70.62(3) . . . . ? C2 Fe1 C1 O1 -24(20) . . . . ? C3 Fe1 C1 O1 -122(20) . . . . ? Fe3 Fe1 C1 O1 122(20) . . . . ? Fe2 Fe1 C1 O1 130(20) . . . . ? Fe4 Fe1 C1 O1 72(20) . . . . ? C1 Fe1 C2 O2 -40(34) . . . . ? C3 Fe1 C2 O2 59(34) . . . . ? Fe3 Fe1 C2 O2 155(34) . . . . ? Fe2 Fe1 C2 O2 -157(34) . . . . ? Fe4 Fe1 C2 O2 -147(34) . . . . ? C1 Fe1 C2 Cs2 25.9(2) . . . . ? C3 Fe1 C2 Cs2 124.74(19) . . . . ? Fe3 Fe1 C2 Cs2 -138.97(13) . . . . ? Fe2 Fe1 C2 Cs2 -90.5(3) . . . . ? Fe4 Fe1 C2 Cs2 -80.80(16) . . . . ? C2 Fe1 C3 O3 -32(13) . . . . ? C1 Fe1 C3 O3 68(13) . . . . ? Fe3 Fe1 C3 O3 -136(13) . . . . ? Fe2 Fe1 C3 O3 165(13) . . . . ? Fe4 Fe1 C3 O3 -141(12) . . . . ? C6 Fe2 C4 O4 -44(3) . . . . ? C5 Fe2 C4 O4 52(3) . . . . ? C13 Fe2 C4 O4 -132(3) . . . . ? Fe4 Fe2 C4 O4 -176(3) . . . . ? Fe3 Fe2 C4 O4 177(3) . . . . ? Fe1 Fe2 C4 O4 126(3) . . . . ? C4 Fe2 C5 O5 -93(2) . . . . ? C6 Fe2 C5 O5 5(2) . . . . ? C13 Fe2 C5 O5 95(2) . . . . ? Fe4 Fe2 C5 O5 -177(2) . . . . ? Fe3 Fe2 C5 O5 122(2) . . . . ? Fe1 Fe2 C5 O5 175(2) . . . . ? C4 Fe2 C6 O6 38(13) . . . . ? C5 Fe2 C6 O6 -64(13) . . . . ? C13 Fe2 C6 O6 142(13) . . . . ? Fe4 Fe2 C6 O6 118(12) . . . . ? Fe3 Fe2 C6 O6 -171(12) . . . . ? Fe1 Fe2 C6 O6 -100(12) . . . . ? C8 Fe3 C7 O7 -42(2) . . . . ? C9 Fe3 C7 O7 53(2) . . . . ? C13 Fe3 C7 O7 -130(2) . . . . ? Fe4 Fe3 C7 O7 -176(2) . . . . ? Fe2 Fe3 C7 O7 -171(2) . . . . ? Fe1 Fe3 C7 O7 131(2) . . . . ? C7 Fe3 C8 O8 25(10) . . . . ? C9 Fe3 C8 O8 -78(10) . . . . ? C13 Fe3 C8 O8 127(10) . . . . ? Fe4 Fe3 C8 O8 169(10) . . . . ? Fe2 Fe3 C8 O8 99(10) . . . . ? Fe1 Fe3 C8 O8 -124(9) . . . . ? C7 Fe3 C8 Cs1 -102.5(2) . . . 1_655 ? C9 Fe3 C8 Cs1 154.2(2) . . . 1_655 ? C13 Fe3 C8 Cs1 -0.5(2) . . . 1_655 ? Fe4 Fe3 C8 Cs1 41.7(2) . . . 1_655 ? Fe2 Fe3 C8 Cs1 -28.5(3) . . . 1_655 ? Fe1 Fe3 C8 Cs1 109.0(6) . . . 1_655 ? C7 Fe3 C9 O9 -96(3) . . . . ? C8 Fe3 C9 O9 1(3) . . . . ? C13 Fe3 C9 O9 92(3) . . . . ? Fe4 Fe3 C9 O9 119(3) . . . . ? Fe2 Fe3 C9 O9 -175(3) . . . . ? Fe1 Fe3 C9 O9 173(3) . . . . ? C12 Fe4 C10 O10 48(2) . . . . ? C11 Fe4 C10 O10 -47(2) . . . . ? C13 Fe4 C10 O10 -134(2) . . . . ? Fe3 Fe4 C10 O10 -178(2) . . . . ? Fe2 Fe4 C10 O10 175.8(19) . . . . ? Fe1 Fe4 C10 O10 124(2) . . . . ? C10 Fe4 C11 O11 15(6) . . . . ? C12 Fe4 C11 O11 -89(6) . . . . ? C13 Fe4 C11 O11 120(6) . . . . ? Fe3 Fe4 C11 O11 87(6) . . . . ? Fe2 Fe4 C11 O11 161(6) . . . . ? Fe1 Fe4 C11 O11 -117(6) . . . . ? C10 Fe4 C12 O12 -80(3) . . . . ? C11 Fe4 C12 O12 17(3) . . . . ? C13 Fe4 C12 O12 105(3) . . . . ? Fe3 Fe4 C12 O12 -159(3) . . . . ? Fe2 Fe4 C12 O12 138(3) . . . . ? Fe1 Fe4 C12 O12 -169(3) . . . . ? C10 Fe4 C12 Cs2 26.1(3) . . . . ? C11 Fe4 C12 Cs2 122.3(3) . . . . ? C13 Fe4 C12 Cs2 -149.5(3) . . . . ? Fe3 Fe4 C12 Cs2 -53.2(3) . . . . ? Fe2 Fe4 C12 Cs2 -116.7(2) . . . . ? Fe1 Fe4 C12 Cs2 -63.2(2) . . . . ? C10 Fe4 C13 O13 80.9(5) . . . . ? C12 Fe4 C13 O13 -103.6(5) . . . . ? C11 Fe4 C13 O13 -13.2(5) . . . . ? Fe3 Fe4 C13 O13 135.1(5) . . . . ? Fe2 Fe4 C13 O13 -146.0(5) . . . . ? Fe1 Fe4 C13 O13 176.5(4) . . . . ? C10 Fe4 C13 Fe2 -133.17(16) . . . . ? C12 Fe4 C13 Fe2 42.4(4) . . . . ? C11 Fe4 C13 Fe2 132.71(17) . . . . ? Fe3 Fe4 C13 Fe2 -78.89(11) . . . . ? Fe1 Fe4 C13 Fe2 -37.50(11) . . . . ? C10 Fe4 C13 Fe3 -54.27(17) . . . . ? C12 Fe4 C13 Fe3 121.3(3) . . . . ? C11 Fe4 C13 Fe3 -148.40(16) . . . . ? Fe2 Fe4 C13 Fe3 78.89(11) . . . . ? Fe1 Fe4 C13 Fe3 41.39(10) . . . . ? C4 Fe2 C13 O13 85.9(5) . . . . ? C6 Fe2 C13 O13 -10.4(4) . . . . ? C5 Fe2 C13 O13 -102.5(5) . . . . ? Fe4 Fe2 C13 O13 146.7(5) . . . . ? Fe3 Fe2 C13 O13 -135.2(5) . . . . ? Fe1 Fe2 C13 O13 -175.7(4) . . . . ? C4 Fe2 C13 Fe4 -60.73(18) . . . . ? C6 Fe2 C13 Fe4 -157.02(17) . . . . ? C5 Fe2 C13 Fe4 110.9(4) . . . . ? Fe3 Fe2 C13 Fe4 78.19(12) . . . . ? Fe1 Fe2 C13 Fe4 37.63(11) . . . . ? C4 Fe2 C13 Fe3 -138.92(15) . . . . ? C6 Fe2 C13 Fe3 124.80(17) . . . . ? C5 Fe2 C13 Fe3 32.7(5) . . . . ? Fe4 Fe2 C13 Fe3 -78.19(12) . . . . ? Fe1 Fe2 C13 Fe3 -40.55(11) . . . . ? C7 Fe3 C13 O13 83.0(4) . . . . ? C8 Fe3 C13 O13 -12.6(4) . . . . ? C9 Fe3 C13 O13 -104.4(5) . . . . ? Fe4 Fe3 C13 O13 -139.7(5) . . . . ? Fe2 Fe3 C13 O13 138.8(5) . . . . ? Fe1 Fe3 C13 O13 179.1(4) . . . . ? C7 Fe3 C13 Fe4 -137.30(15) . . . . ? C8 Fe3 C13 Fe4 127.13(16) . . . . ? C9 Fe3 C13 Fe4 35.3(4) . . . . ? Fe2 Fe3 C13 Fe4 -81.52(12) . . . . ? Fe1 Fe3 C13 Fe4 -41.25(10) . . . . ? C7 Fe3 C13 Fe2 -55.78(17) . . . . ? C8 Fe3 C13 Fe2 -151.35(17) . . . . ? C9 Fe3 C13 Fe2 116.8(4) . . . . ? Fe4 Fe3 C13 Fe2 81.52(12) . . . . ? Fe1 Fe3 C13 Fe2 40.27(11) . . . . ? Fe1 C1 O1 Cs2 -71(20) . . . 2_775 ? Fe1 C2 O2 Cs2 66(34) . . . . ? Fe1 C2 O2 Cs2 -151(34) . . . 2_765 ? Cs2 C2 O2 Cs2 142.2(3) . . . 2_765 ? Fe1 C3 O3 Cs1 -164(12) . . . . ? Fe2 C4 O4 Cs2 -116(3) . . . 2_775 ? Fe2 C5 O5 Cs1 -89(2) . . . . ? Fe2 C6 O6 Cs1 -44(13) . . . 2_776 ? Fe3 C7 O7 Cs1 -119(2) . . . . ? Fe3 C8 O8 Cs1 -129(10) . . . 1_655 ? Fe3 C8 O8 Cs1 -25(10) . . . 2_766 ? Cs1 C8 O8 Cs1 103.4(5) 1_655 . . 2_766 ? Fe3 C9 O9 Cs2 -89(3) . . . 2_765 ? Fe4 C10 O10 Cs2 -117.1(19) . . . 2_765 ? Fe4 C12 O12 Cs2 112(3) . . . . ? Fe4 C12 O12 Cs2 -112(3) . . . 2_775 ? Cs2 C12 O12 Cs2 135.8(3) . . . 2_775 ? Fe4 C13 O13 Cs1 -86.0(6) . . . 1_655 ? Fe2 C13 O13 Cs1 144.8(3) . . . 1_655 ? Fe3 C13 O13 Cs1 29.6(7) . . . 1_655 ? C7 O7 Cs1 O13 -25.9(4) . . . 1_455 ? C7 O7 Cs1 O20 98.4(4) . . . 2_666 ? C7 O7 Cs1 O20 176.0(3) . . . . ? C7 O7 Cs1 O6 -111.2(4) . . . 2_776 ? C7 O7 Cs1 O5 -43.5(4) . . . . ? C7 O7 Cs1 O8 75.7(4) . . . 1_455 ? C7 O7 Cs1 O8 166.9(4) . . . 2_766 ? C7 O7 Cs1 O3 20.5(4) . . . . ? C7 O7 Cs1 C8 55.5(4) . . . 1_455 ? C7 O7 Cs1 C21 178.7(3) . . . . ? C7 O7 Cs1 C21 109.2(4) . . . 2_666 ? C5 O5 Cs1 O13 -160.0(4) . . . 1_455 ? C5 O5 Cs1 O7 8.4(3) . . . . ? C5 O5 Cs1 O20 -39.3(4) . . . 2_666 ? C5 O5 Cs1 O20 142.7(3) . . . . ? C5 O5 Cs1 O6 101.1(4) . . . 2_776 ? C5 O5 Cs1 O8 -115.3(3) . . . 1_455 ? C5 O5 Cs1 O8 51.0(4) . . . 2_766 ? C5 O5 Cs1 O3 -70.9(3) . . . . ? C5 O5 Cs1 C8 -127.6(3) . . . 1_455 ? C5 O5 Cs1 C21 168.2(3) . . . . ? C5 O5 Cs1 C21 -17.5(4) . . . 2_666 ? C3 O3 Cs1 O13 111.8(3) . . . 1_455 ? C3 O3 Cs1 O7 -40.1(3) . . . . ? C3 O3 Cs1 O20 -121.3(3) . . . 2_666 ? C3 O3 Cs1 O20 172.6(3) . . . . ? C3 O3 Cs1 O6 23.5(3) . . . 2_776 ? C3 O3 Cs1 O5 32.5(3) . . . . ? C3 O3 Cs1 O8 178.5(3) . . . 1_455 ? C3 O3 Cs1 O8 -88.5(3) . . . 2_766 ? C3 O3 Cs1 C8 161.8(3) . . . 1_455 ? C3 O3 Cs1 C21 151.1(3) . . . . ? C3 O3 Cs1 C21 -100.5(3) . . . 2_666 ? C2 O2 Cs2 O30 -82.4(3) . . . . ? Cs2 O2 Cs2 O30 134.32(13) 2_765 . . . ? C2 O2 Cs2 O10 -150.7(3) . . . 2_765 ? Cs2 O2 Cs2 O10 66.06(11) 2_765 . . 2_765 ? C2 O2 Cs2 O4 -126.4(3) . . . 2_775 ? Cs2 O2 Cs2 O4 90.31(17) 2_765 . . 2_775 ? C2 O2 Cs2 O1 54.7(3) . . . 2_775 ? Cs2 O2 Cs2 O1 -88.52(15) 2_765 . . 2_775 ? C2 O2 Cs2 O12 31.1(3) . . . . ? Cs2 O2 Cs2 O12 -112.16(11) 2_765 . . . ? C2 O2 Cs2 O9 154.3(3) . . . 2_765 ? Cs2 O2 Cs2 O9 11.08(13) 2_765 . . 2_765 ? C2 O2 Cs2 O12 -27.9(3) . . . 2_775 ? Cs2 O2 Cs2 O12 -171.17(8) 2_765 . . 2_775 ? C2 O2 Cs2 O2 143.2(3) . . . 2_765 ? Cs2 O2 Cs2 O2 0.0 2_765 . . 2_765 ? Cs2 O2 Cs2 C2 -143.2(3) 2_765 . . . ? C2 O2 Cs2 C31 -93.9(3) . . . . ? Cs2 O2 Cs2 C31 122.86(14) 2_765 . . . ? C2 O2 Cs2 C12 33.9(3) . . . . ? Cs2 O2 Cs2 C12 -109.31(12) 2_765 . . . ? C12 O12 Cs2 O30 79.8(3) . . . . ? Cs2 O12 Cs2 O30 -61.53(11) 2_775 . . . ? C12 O12 Cs2 O10 5.4(4) . . . 2_765 ? Cs2 O12 Cs2 O10 -135.89(16) 2_775 . . 2_765 ? C12 O12 Cs2 O4 174.7(3) . . . 2_775 ? Cs2 O12 Cs2 O4 33.39(13) 2_775 . . 2_775 ? C12 O12 Cs2 O1 -154.7(3) . . . 2_775 ? Cs2 O12 Cs2 O1 63.94(8) 2_775 . . 2_775 ? C12 O12 Cs2 O2 9.7(3) . . . . ? Cs2 O12 Cs2 O2 -131.66(10) 2_775 . . . ? C12 O12 Cs2 O9 -104.3(3) . . . 2_765 ? Cs2 O12 Cs2 O9 114.35(9) 2_775 . . 2_765 ? C12 O12 Cs2 O12 141.3(3) . . . 2_775 ? Cs2 O12 Cs2 O12 0.0 2_775 . . 2_775 ? C12 O12 Cs2 O2 -44.9(3) . . . 2_765 ? Cs2 O12 Cs2 O2 173.81(8) 2_775 . . 2_765 ? C12 O12 Cs2 C2 20.2(3) . . . . ? Cs2 O12 Cs2 C2 -121.12(11) 2_775 . . . ? C12 O12 Cs2 C31 93.3(3) . . . . ? Cs2 O12 Cs2 C31 -48.01(16) 2_775 . . . ? Cs2 O12 Cs2 C12 -141.3(3) 2_775 . . . ? O2 C2 Cs2 O30 93.1(3) . . . . ? Fe1 C2 Cs2 O30 -86.2(2) . . . . ? O2 C2 Cs2 O10 29.0(3) . . . 2_765 ? Fe1 C2 Cs2 O10 -150.22(19) . . . 2_765 ? O2 C2 Cs2 O4 87.5(3) . . . 2_775 ? Fe1 C2 Cs2 O4 -91.7(3) . . . 2_775 ? O2 C2 Cs2 O1 -138.7(3) . . . 2_775 ? Fe1 C2 Cs2 O1 42.0(2) . . . 2_775 ? Fe1 C2 Cs2 O2 -179.3(4) . . . . ? O2 C2 Cs2 O12 -144.8(3) . . . . ? Fe1 C2 Cs2 O12 35.92(17) . . . . ? O2 C2 Cs2 O9 -32.0(3) . . . 2_765 ? Fe1 C2 Cs2 O9 148.78(16) . . . 2_765 ? O2 C2 Cs2 O12 155.8(3) . . . 2_775 ? Fe1 C2 Cs2 O12 -23.5(2) . . . 2_775 ? O2 C2 Cs2 O2 -32.5(3) . . . 2_765 ? Fe1 C2 Cs2 O2 148.3(2) . . . 2_765 ? O2 C2 Cs2 C31 87.3(3) . . . . ? Fe1 C2 Cs2 C31 -91.9(2) . . . . ? O2 C2 Cs2 C12 -137.8(3) . . . . ? Fe1 C2 Cs2 C12 42.97(17) . . . . ? O12 C12 Cs2 O30 -104.6(3) . . . . ? Fe4 C12 Cs2 O30 84.1(3) . . . . ? O12 C12 Cs2 O10 -176.4(3) . . . 2_765 ? Fe4 C12 Cs2 O10 12.3(3) . . . 2_765 ? O12 C12 Cs2 O4 -7.2(4) . . . 2_775 ? Fe4 C12 Cs2 O4 -178.47(19) . . . 2_775 ? O12 C12 Cs2 O1 23.7(3) . . . 2_775 ? Fe4 C12 Cs2 O1 -147.5(3) . . . 2_775 ? O12 C12 Cs2 O2 -169.2(3) . . . . ? Fe4 C12 Cs2 O2 19.5(2) . . . . ? Fe4 C12 Cs2 O12 -171.3(5) . . . . ? O12 C12 Cs2 O9 86.9(3) . . . 2_765 ? Fe4 C12 Cs2 O9 -84.3(3) . . . 2_765 ? O12 C12 Cs2 O12 -37.0(3) . . . 2_775 ? Fe4 C12 Cs2 O12 151.7(2) . . . 2_775 ? O12 C12 Cs2 O2 136.1(3) . . . 2_765 ? Fe4 C12 Cs2 O2 -35.2(2) . . . 2_765 ? O12 C12 Cs2 C2 -155.5(3) . . . . ? Fe4 C12 Cs2 C2 33.2(2) . . . . ? O12 C12 Cs2 C31 -96.9(3) . . . . ? Fe4 C12 Cs2 C31 91.8(3) . . . . ? O13 Cs1 O20 C24 -113.5(3) 1_455 . . . ? O7 Cs1 O20 C24 52.5(3) . . . . ? O20 Cs1 O20 C24 124.1(3) 2_666 . . . ? O6 Cs1 O20 C24 -19.7(3) 2_776 . . . ? O5 Cs1 O20 C24 -57.5(3) . . . . ? O8 Cs1 O20 C24 179.2(3) 1_455 . . . ? O8 Cs1 O20 C24 63.0(3) 2_766 . . . ? O3 Cs1 O20 C24 -174.4(3) . . . . ? C8 Cs1 O20 C24 -163.2(3) 1_455 . . . ? C21 Cs1 O20 C24 -124.5(4) . . . . ? C21 Cs1 O20 C24 104.7(3) 2_666 . . . ? O13 Cs1 O20 C21 11.1(3) 1_455 . . . ? O7 Cs1 O20 C21 177.0(2) . . . . ? O20 Cs1 O20 C21 -111.4(3) 2_666 . . . ? O6 Cs1 O20 C21 104.8(3) 2_776 . . . ? O5 Cs1 O20 C21 67.0(3) . . . . ? O8 Cs1 O20 C21 -56.3(3) 1_455 . . . ? O8 Cs1 O20 C21 -172.4(3) 2_766 . . . ? O3 Cs1 O20 C21 -49.9(3) . . . . ? C8 Cs1 O20 C21 -38.6(3) 1_455 . . . ? C21 Cs1 O20 C21 -130.8(2) 2_666 . . . ? O13 Cs1 O20 Cs1 122.45(8) 1_455 . . 2_666 ? O7 Cs1 O20 Cs1 -71.56(12) . . . 2_666 ? O20 Cs1 O20 Cs1 0.0 2_666 . . 2_666 ? O6 Cs1 O20 Cs1 -143.78(9) 2_776 . . 2_666 ? O5 Cs1 O20 Cs1 178.41(9) . . . 2_666 ? O8 Cs1 O20 Cs1 55.14(7) 1_455 . . 2_666 ? O8 Cs1 O20 Cs1 -61.06(8) 2_766 . . 2_666 ? O3 Cs1 O20 Cs1 61.50(16) . . . 2_666 ? C8 Cs1 O20 Cs1 72.75(8) 1_455 . . 2_666 ? C21 Cs1 O20 Cs1 111.4(3) . . . 2_666 ? C21 Cs1 O20 Cs1 -19.38(9) 2_666 . . 2_666 ? C24 O20 C21 C22 -23.2(5) . . . . ? Cs1 O20 C21 C22 111.3(3) 2_666 . . . ? Cs1 O20 C21 C22 -152.9(3) . . . . ? C24 O20 C21 Cs1 129.8(4) . . . . ? Cs1 O20 C21 Cs1 -95.80(18) 2_666 . . . ? C24 O20 C21 Cs1 -134.4(4) . . . 2_666 ? Cs1 O20 C21 Cs1 95.80(18) . . . 2_666 ? O13 Cs1 C21 O20 -167.5(3) 1_455 . . . ? O7 Cs1 C21 O20 -5.2(4) . . . . ? O20 Cs1 C21 O20 70.5(3) 2_666 . . . ? O6 Cs1 C21 O20 -74.0(3) 2_776 . . . ? O5 Cs1 C21 O20 -131.8(2) . . . . ? O8 Cs1 C21 O20 114.1(3) 1_455 . . . ? O8 Cs1 C21 O20 6.5(2) 2_766 . . . ? O3 Cs1 C21 O20 146.9(2) . . . . ? C8 Cs1 C21 O20 134.1(3) 1_455 . . . ? C21 Cs1 C21 O20 53.7(2) 2_666 . . . ? O13 Cs1 C21 C22 -115.4(6) 1_455 . . . ? O7 Cs1 C21 C22 46.9(7) . . . . ? O20 Cs1 C21 C22 122.6(6) 2_666 . . . ? O20 Cs1 C21 C22 52.1(5) . . . . ? O6 Cs1 C21 C22 -21.9(6) 2_776 . . . ? O5 Cs1 C21 C22 -79.7(6) . . . . ? O8 Cs1 C21 C22 166.2(6) 1_455 . . . ? O8 Cs1 C21 C22 58.7(5) 2_766 . . . ? O3 Cs1 C21 C22 -161.0(5) . . . . ? C8 Cs1 C21 C22 -173.8(6) 1_455 . . . ? C21 Cs1 C21 C22 105.8(6) 2_666 . . . ? O13 Cs1 C21 Cs1 138.80(11) 1_455 . . 2_666 ? O7 Cs1 C21 Cs1 -58.9(2) . . . 2_666 ? O20 Cs1 C21 Cs1 16.79(8) 2_666 . . 2_666 ? O20 Cs1 C21 Cs1 -53.7(2) . . . 2_666 ? O6 Cs1 C21 Cs1 -127.70(8) 2_776 . . 2_666 ? O5 Cs1 C21 Cs1 174.53(8) . . . 2_666 ? O8 Cs1 C21 Cs1 60.39(8) 1_455 . . 2_666 ? O8 Cs1 C21 Cs1 -47.13(7) 2_766 . . 2_666 ? O3 Cs1 C21 Cs1 93.17(10) . . . 2_666 ? C8 Cs1 C21 Cs1 80.39(10) 1_455 . . 2_666 ? C21 Cs1 C21 Cs1 0.0 2_666 . . 2_666 ? O20 C21 C22 C23 26.9(5) . . . . ? Cs1 C21 C22 C23 -11.8(7) . . . . ? Cs1 C21 C22 C23 78.6(4) 2_666 . . . ? C21 C22 C23 C24 -21.2(6) . . . . ? C21 O20 C24 C23 9.4(6) . . . . ? Cs1 O20 C24 C23 -119.7(4) 2_666 . . . ? Cs1 O20 C24 C23 134.6(4) . . . . ? C22 C23 C24 O20 7.9(7) . . . . ? O10 Cs2 O30 C34 140.2(6) 2_765 . . . ? O4 Cs2 O30 C34 -145.6(6) 2_775 . . . ? O1 Cs2 O30 C34 -91.8(6) 2_775 . . . ? O2 Cs2 O30 C34 55.0(6) . . . . ? O12 Cs2 O30 C34 -13.9(6) . . . . ? O9 Cs2 O30 C34 170.2(6) 2_765 . . . ? O12 Cs2 O30 C34 -78.3(6) 2_775 . . . ? O2 Cs2 O30 C34 99.6(6) 2_765 . . . ? C2 Cs2 O30 C34 36.7(6) . . . . ? C31 Cs2 O30 C34 -160.0(8) . . . . ? C12 Cs2 O30 C34 1.3(6) . . . . ? O10 Cs2 O30 C31 -59.8(4) 2_765 . . . ? O4 Cs2 O30 C31 14.5(4) 2_775 . . . ? O1 Cs2 O30 C31 68.3(4) 2_775 . . . ? O2 Cs2 O30 C31 -145.0(4) . . . . ? O12 Cs2 O30 C31 146.1(4) . . . . ? O9 Cs2 O30 C31 -29.8(4) 2_765 . . . ? O12 Cs2 O30 C31 81.7(4) 2_775 . . . ? O2 Cs2 O30 C31 -100.4(4) 2_765 . . . ? C2 Cs2 O30 C31 -163.3(4) . . . . ? C12 Cs2 O30 C31 161.3(4) . . . . ? C34 O30 C31 C32 0.8(7) . . . . ? Cs2 O30 C31 C32 -164.9(4) . . . . ? C34 O30 C31 Cs2 165.7(6) . . . . ? O10 Cs2 C31 O30 110.6(4) 2_765 . . . ? O4 Cs2 C31 O30 -163.7(4) 2_775 . . . ? O1 Cs2 C31 O30 -124.0(4) 2_775 . . . ? O2 Cs2 C31 O30 34.0(4) . . . . ? O12 Cs2 C31 O30 -40.0(4) . . . . ? O9 Cs2 C31 O30 154.9(4) 2_765 . . . ? O12 Cs2 C31 O30 -90.4(4) 2_775 . . . ? O2 Cs2 C31 O30 90.9(4) 2_765 . . . ? C2 Cs2 C31 O30 16.2(4) . . . . ? C12 Cs2 C31 O30 -22.0(4) . . . . ? O30 Cs2 C31 C32 31.8(9) . . . . ? O10 Cs2 C31 C32 142.4(11) 2_765 . . . ? O4 Cs2 C31 C32 -131.9(10) 2_775 . . . ? O1 Cs2 C31 C32 -92.1(10) 2_775 . . . ? O2 Cs2 C31 C32 65.9(10) . . . . ? O12 Cs2 C31 C32 -8.2(11) . . . . ? O9 Cs2 C31 C32 -173.3(10) 2_765 . . . ? O12 Cs2 C31 C32 -58.5(10) 2_775 . . . ? O2 Cs2 C31 C32 122.7(10) 2_765 . . . ? C2 Cs2 C31 C32 48.0(10) . . . . ? C12 Cs2 C31 C32 9.9(11) . . . . ? O30 C31 C32 C33 -12.6(8) . . . . ? Cs2 C31 C32 C33 -36.4(12) . . . . ? C31 C32 C33 C34 19.4(8) . . . . ? C31 O30 C34 C33 11.8(8) . . . . ? Cs2 O30 C34 C33 172.6(4) . . . . ? C32 C33 C34 O30 -19.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.353 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.130