#------------------------------------------------------------------------------ #$Date: 2022-01-07 01:33:34 +0200 (Fri, 07 Jan 2022) $ #$Revision: 271922 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243916.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243916 loop_ _publ_author_name 'Ward, Cassandra L.' 'Allen, Matthew J.' 'Lutter, Jacob C.' _publ_section_title ; Hexa-\m-acetato-chlorido(\m-N,2-dioxodobenzene-1-carboximidato)-\m~3~-oxido-tetrairon(III)--water (1/1) and hexa-\m-acetato-(\m-N,2-dioxodobenzene-1-carboximidato)fluorido-\m~3~-oxido-tripyridinetetrairon(III)--pyridine--water (1/1/0.24) ; _journal_coeditor_code ZL5012 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1003 _journal_page_last 1009 _journal_paper_doi 10.1107/S2056989021009208 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac '[Fe4 (C2 H3 O2)6 (C7 H4 O3) F O (C5 H5 N)5], C5 H5 N, 0.24H2 O' _chemical_formula_moiety '2(C34 H37 F Fe4 N4 O16), C5 H5 N, 0.472(H2 O)' _chemical_formula_sum 'C73 H79.94 F2 Fe8 N9 O32.47' _chemical_formula_weight 2087.76 _chemical_melting_point 257 _chemical_name_systematic 'Hexa-\m-acetato-(\m-N,2-dioxodobenzene-1-carboximidato)fluorido-\m~3~-oxido-tripyridinetetrairon(III)--pyridine--water (1/1/0.24)' _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' _space_group_name_H-M_alt 'F d d 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 31.676(2) _cell_length_b 44.806(3) _cell_length_c 12.6056(8) _cell_measurement_reflns_used 9974 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.14 _cell_measurement_theta_min 2.21 _cell_volume 17891(2) _computing_cell_refinement ; SAINT (Bruker, 2001) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT (Bruker, 2001) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/3 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_unetI/netI 0.0493 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 102006 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.440 _diffrn_reflns_theta_min 1.575 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.550 _exptl_crystal_description plate _exptl_crystal_F_000 8534 _exptl_crystal_size_max 0.328 _exptl_crystal_size_mid 0.304 _exptl_crystal_size_min 0.144 _refine_diff_density_max 0.472 _refine_diff_density_min -0.379 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_extinction_coef 0.000039(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/3 (Sheldrick 2018) ; _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 604 _refine_ls_number_reflns 8265 _refine_ls_number_restraints 58 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0385 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+78.0080P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.0902 _reflns_number_gt 7012 _reflns_number_total 8265 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl5012sup1.cif _cod_data_source_block 1-F _cod_depositor_comments 'Adding full bibliography for 2243916--2243917.cif.' _cod_database_code 2243916 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.666 _shelx_estimated_absorpt_t_max 0.830 _shelx_hkl_file ; -2 -2 -2 18.31 1.22 -2 -2 -2 18.60 1.05 -2 -2 -2 20.53 1.21 -2 -2 -2 17.18 1.20 -2 -2 -2 17.10 1.17 -2 -2 -2 18.07 1.11 2 2 2 15.99 1.15 2 2 2 15.31 1.01 2 2 2 16.76 1.20 2 2 2 16.72 1.10 2 2 2 15.79 1.14 2 2 2 16.91 1.17 -3 -3 -3 3.94 0.65 -3 -3 -3 5.38 0.87 -3 -3 -3 2.81 0.70 -3 -3 -3 3.96 0.86 -3 -3 -3 2.69 0.75 -3 -3 -3 3.19 0.77 3 3 3 3.08 0.74 3 3 3 3.36 0.77 3 3 3 3.85 0.76 3 3 3 5.43 0.67 3 3 3 4.49 0.85 -4 -4 -4 36.44 2.48 -4 -4 -4 38.63 2.49 -4 -4 -4 38.64 2.20 -4 -4 -4 43.21 2.50 -4 -4 -4 39.53 2.54 -4 -4 -4 38.89 2.30 4 4 4 42.05 2.56 4 4 4 43.48 2.57 4 4 4 42.44 2.55 4 4 4 39.33 2.43 4 4 4 42.38 2.21 4 4 4 44.04 2.41 -5 -5 -5 68.12 3.85 -5 -5 -5 68.97 3.80 -5 -5 -5 65.31 3.44 -5 -5 -5 69.47 3.83 -5 -5 -5 66.60 3.85 -5 -5 -5 70.17 3.63 5 5 5 67.50 3.89 5 5 5 69.31 3.88 5 5 5 68.74 3.84 5 5 5 65.40 3.43 5 5 5 64.35 3.74 -6 -6 -6 2.51 0.96 -6 -6 -6 2.69 1.04 -6 -6 -6 4.04 1.17 -6 -6 -6 2.99 0.80 6 6 6 3.57 0.83 6 6 6 4.19 1.08 6 6 6 5.45 1.17 -7 -7 -7 12.55 1.76 -7 -7 -7 13.01 1.27 -7 -7 -7 11.75 1.75 7 7 7 9.36 1.20 7 7 7 10.98 1.72 7 7 7 11.57 1.70 -8 -8 -8 14.54 2.05 -8 -8 -8 15.52 1.43 -8 -8 -8 12.52 1.99 8 8 8 16.37 1.74 8 8 8 17.93 2.10 8 8 8 13.53 1.45 8 8 8 15.96 1.96 -9 -9 -9 5.38 1.04 -9 -9 -9 5.91 1.60 -9 -9 -9 2.20 1.32 9 9 9 1.50 1.30 9 9 9 2.75 1.05 9 9 9 2.66 1.18 9 9 9 2.66 1.37 -10 -10 -10 20.42 2.64 -10 -10 -10 17.71 2.69 10 10 10 17.30 2.62 10 10 10 17.37 2.09 10 10 10 17.64 2.52 -11 -11 -11 11.37 2.43 -11 -11 -11 8.56 2.22 11 11 11 9.89 2.23 11 11 11 12.72 1.85 11 11 11 11.36 2.34 -12 -12 -12 4.46 1.94 -12 -12 -12 4.48 2.00 12 12 12 4.87 2.08 12 12 12 8.64 2.28 -13 -13 -13 10.46 2.70 -13 -13 -13 2.13 1.93 13 13 13 10.93 2.63 13 13 13 9.93 2.60 15 13 13 -0.93 1.74 15 13 13 -0.59 1.63 -15 -13 -13 1.30 1.87 -15 -13 -13 1.08 1.81 14 12 12 4.89 2.07 14 12 12 10.24 2.43 -14 -12 -12 10.82 2.47 -14 -12 -12 14.50 2.79 13 11 11 12.11 2.01 13 11 11 14.32 2.58 13 11 11 7.99 2.17 -13 -11 -11 9.08 2.22 -13 -11 -11 14.85 2.71 12 10 10 20.83 2.61 12 10 10 20.39 2.61 12 10 10 16.57 2.18 -12 -10 -10 19.65 2.68 -12 -10 -10 16.98 2.60 11 9 9 31.55 2.85 11 9 9 26.06 2.14 11 9 9 32.56 2.94 -11 -9 -9 27.12 2.89 -11 -9 -9 25.04 2.80 10 8 8 4.47 1.07 10 8 8 6.62 1.53 10 8 8 4.04 1.30 -10 -8 -8 0.58 1.11 -10 -8 -8 3.86 1.33 9 7 7 1.97 1.03 9 7 7 2.90 1.14 9 7 7 2.81 0.90 -9 -7 -7 2.39 1.13 -9 -7 -7 3.04 0.74 -9 -7 -7 2.68 1.15 8 6 6 11.55 1.64 8 6 6 15.58 1.64 8 6 6 11.82 1.31 8 6 6 13.71 1.66 -8 -6 -6 15.45 1.26 -8 -6 -6 17.83 1.87 -8 -6 -6 12.32 1.73 7 5 5 9.24 1.33 7 5 5 9.81 1.15 7 5 5 8.69 1.34 -7 -5 -5 9.29 1.43 -7 -5 -5 7.05 0.95 -7 -5 -5 9.21 1.39 -7 -5 -5 10.99 1.40 -7 -5 -5 9.60 1.45 6 4 4 41.36 2.57 6 4 4 40.25 2.11 6 4 4 39.19 2.31 6 4 4 45.86 2.54 6 4 4 41.85 2.62 6 4 4 44.17 2.62 -6 -4 -4 39.30 2.58 -6 -4 -4 47.33 2.63 -6 -4 -4 41.03 2.58 -6 -4 -4 41.83 2.57 -6 -4 -4 41.57 2.25 -6 -4 -4 42.80 2.47 -6 -4 -4 41.83 2.08 5 3 3 6.46 0.97 5 3 3 7.09 1.00 5 3 3 6.81 1.02 5 3 3 6.15 0.64 5 3 3 6.96 0.99 5 3 3 6.83 0.85 -5 -3 -3 7.55 1.02 -5 -3 -3 6.65 0.97 -5 -3 -3 4.92 0.60 -5 -3 -3 4.50 0.89 -5 -3 -3 5.57 0.74 -5 -3 -3 6.68 1.02 -5 -3 -3 6.74 0.93 4 2 2 4.07 0.73 4 2 2 3.71 0.66 4 2 2 4.27 0.75 4 2 2 3.33 0.42 4 2 2 3.71 0.67 4 2 2 4.37 0.60 4 2 2 4.08 0.48 -4 -2 -2 4.63 0.77 -4 -2 -2 4.64 0.72 -4 -2 -2 4.50 0.70 -4 -2 -2 5.95 0.73 -4 -2 -2 3.26 0.42 -4 -2 -2 6.68 0.83 -4 -2 -2 4.89 0.51 3 1 1 260.18 11.57 3 1 1 252.29 11.51 3 1 1 255.64 11.60 3 1 1 266.22 11.59 3 1 1 256.74 11.61 3 1 1 256.21 11.49 -3 -1 -1 255.26 11.60 -3 -1 -1 257.94 11.49 -3 -1 -1 262.37 11.57 -3 -1 -1 259.91 11.51 -3 -1 -1 267.93 11.59 -3 -1 -1 260.07 11.61 -3 -1 -1 260.72 11.59 2 0 0 1.83 0.24 2 0 0 1.65 0.25 -2 0 0 1.51 0.22 -2 0 0 1.68 0.19 -2 0 0 2.04 0.24 -2 0 0 0.51 0.12 1 -1 -1 88.38 3.90 1 -1 -1 86.70 3.88 1 -1 -1 84.91 3.82 1 -1 -1 82.35 3.87 1 -1 -1 83.78 3.83 -1 1 1 89.82 3.83 -1 1 1 85.82 3.87 -1 1 1 74.27 3.86 -1 1 1 87.07 3.84 0 -2 -2 40.32 1.89 0 -2 -2 38.09 1.92 0 -2 -2 40.37 2.05 0 -2 -2 40.37 1.99 0 -2 -2 40.65 2.07 0 -2 -2 39.09 2.06 0 2 2 37.90 2.04 0 2 2 37.77 1.98 0 2 2 35.65 1.92 0 2 2 38.20 2.06 0 2 2 38.18 2.07 0 2 2 37.86 1.90 -1 -3 -3 105.89 5.24 -1 -3 -3 109.85 5.09 -1 -3 -3 102.25 5.24 -1 -3 -3 107.29 5.05 -1 -3 -3 118.33 5.28 -1 -3 -3 108.06 5.25 1 3 3 113.49 5.26 1 3 3 106.82 5.26 1 3 3 104.68 5.16 1 3 3 108.42 5.26 1 3 3 106.28 5.04 1 3 3 107.54 5.02 -2 -4 -4 51.42 2.70 -2 -4 -4 51.71 2.94 -2 -4 -4 48.97 2.64 -2 -4 -4 49.51 2.90 -2 -4 -4 49.79 2.91 -2 -4 -4 53.12 2.91 2 4 4 47.17 2.88 2 4 4 51.05 2.93 2 4 4 50.50 2.80 2 4 4 50.64 2.61 2 4 4 50.72 2.62 2 4 4 50.60 2.90 -3 -5 -5 20.54 1.76 -3 -5 -5 20.76 1.78 -3 -5 -5 21.41 1.79 -3 -5 -5 22.36 1.79 -3 -5 -5 17.39 1.42 -3 -5 -5 19.27 1.51 3 5 5 17.52 1.69 3 5 5 18.38 1.75 3 5 5 17.80 1.43 3 5 5 22.63 1.76 3 5 5 17.41 1.62 3 5 5 19.52 1.40 -4 -6 -6 83.55 4.50 -4 -6 -6 76.86 4.04 -4 -6 -6 80.81 4.52 -4 -6 -6 78.92 4.14 4 6 6 76.43 3.97 4 6 6 77.57 4.32 4 6 6 77.88 4.45 4 6 6 74.25 4.00 -5 -7 -7 14.54 1.88 -5 -7 -7 14.95 1.94 -5 -7 -7 19.78 1.60 5 7 7 16.20 1.88 5 7 7 19.04 1.58 5 7 7 19.20 1.99 5 7 7 19.74 1.64 -6 -8 -8 3.21 1.29 -6 -8 -8 3.92 1.36 -6 -8 -8 6.34 1.13 6 8 8 5.23 1.07 6 8 8 5.86 1.17 6 8 8 4.30 1.32 6 8 8 5.75 1.46 -7 -9 -9 28.46 2.07 -7 -9 -9 26.45 2.70 -7 -9 -9 24.20 2.68 7 9 9 23.26 2.55 7 9 9 29.64 2.72 7 9 9 25.15 2.12 7 9 9 29.54 2.13 -8 -10 -10 8.38 2.02 -8 -10 -10 9.18 2.01 -8 -10 -10 11.20 1.50 8 10 10 9.28 1.98 8 10 10 10.70 1.65 8 10 10 7.70 1.89 -9 -11 -11 29.86 3.33 -9 -11 -11 36.17 2.61 -9 -11 -11 33.82 3.40 9 11 11 29.96 3.23 9 11 11 28.99 3.19 9 11 11 31.65 2.52 -10 -12 -12 1.56 1.64 -10 -12 -12 2.20 1.84 10 12 12 1.66 1.70 10 12 12 2.26 1.74 -11 -13 -13 0.26 1.76 -11 -13 -13 -0.09 1.74 11 13 13 0.25 1.69 11 13 13 1.93 1.80 17 13 13 3.17 2.03 17 13 13 -0.71 1.80 -17 -13 -13 3.26 2.17 -17 -13 -13 5.59 2.31 16 12 12 2.25 1.82 16 12 12 3.36 1.86 -16 -12 -12 3.10 1.88 -16 -12 -12 1.82 1.84 15 11 11 8.37 2.30 15 11 11 10.65 2.04 15 11 11 8.95 2.27 -15 -11 -11 14.68 2.52 -15 -11 -11 10.05 2.46 14 10 10 0.24 1.27 14 10 10 -0.78 1.29 -14 -10 -10 0.49 1.39 -14 -10 -10 -0.66 1.29 13 9 9 9.77 2.28 13 9 9 7.63 1.79 13 9 9 8.94 1.90 -13 -9 -9 9.54 2.00 -13 -9 -9 7.31 1.91 12 8 8 1.89 1.23 12 8 8 6.47 1.67 12 8 8 5.55 1.47 12 8 8 6.92 1.27 -12 -8 -8 3.09 1.38 -12 -8 -8 3.09 1.37 11 7 7 24.93 2.34 11 7 7 25.96 2.27 11 7 7 20.65 1.89 11 7 7 24.72 2.35 -11 -7 -7 29.85 2.53 -11 -7 -7 27.04 2.47 10 6 6 18.27 1.46 10 6 6 24.28 2.04 10 6 6 17.66 1.76 10 6 6 25.28 2.12 -10 -6 -6 23.43 1.39 -10 -6 -6 24.40 2.19 -10 -6 -6 22.18 2.16 9 5 5 26.65 1.64 9 5 5 29.62 2.15 9 5 5 25.87 1.90 9 5 5 25.64 2.11 -9 -5 -5 25.18 2.35 -9 -5 -5 27.22 2.20 -9 -5 -5 26.79 1.57 -9 -5 -5 27.43 2.22 8 4 4 28.49 1.69 8 4 4 28.90 2.15 8 4 4 29.71 2.17 8 4 4 29.49 1.88 8 4 4 31.82 2.07 8 4 4 30.62 2.11 -8 -4 -4 33.79 2.12 -8 -4 -4 30.31 1.70 -8 -4 -4 27.94 2.07 -8 -4 -4 27.08 2.07 -8 -4 -4 30.48 2.04 -8 -4 -4 28.53 2.14 -8 -4 -4 29.73 2.17 -8 -4 -4 30.73 1.57 7 3 3 17.29 1.21 7 3 3 19.27 1.48 7 3 3 18.96 1.59 7 3 3 18.54 1.49 7 3 3 19.69 1.55 7 3 3 17.56 1.14 7 3 3 18.13 1.33 -7 -3 -3 20.82 1.58 -7 -3 -3 18.77 1.14 -7 -3 -3 21.58 1.63 -7 -3 -3 21.29 1.53 -7 -3 -3 19.64 1.47 -7 -3 -3 20.86 1.25 -7 -3 -3 22.08 1.62 6 2 2 29.03 1.71 6 2 2 26.37 1.61 6 2 2 26.82 1.55 6 2 2 26.17 1.58 6 2 2 25.05 1.36 6 2 2 25.97 1.42 -6 -2 -2 22.48 1.58 -6 -2 -2 23.69 1.51 -6 -2 -2 22.30 1.55 -6 -2 -2 21.45 1.38 -6 -2 -2 21.61 1.33 -6 -2 -2 20.53 1.61 -6 -2 -2 21.27 1.52 5 1 1 57.18 2.92 5 1 1 55.19 2.85 5 1 1 59.60 2.91 5 1 1 58.75 2.85 5 1 1 58.13 2.82 5 1 1 58.23 2.81 5 1 1 62.71 2.92 -5 -1 -1 57.11 2.94 -5 -1 -1 58.62 2.81 -5 -1 -1 59.05 2.85 -5 -1 -1 59.47 2.88 -5 -1 -1 59.86 2.90 -5 -1 -1 59.12 2.83 -5 -1 -1 58.76 2.90 4 0 0 954.62 42.15 4 0 0 951.62 42.15 4 0 0 983.66 42.06 4 0 0 976.59 42.11 4 0 0 954.12 42.12 4 0 0 888.83 42.14 -4 0 0 949.73 42.14 -4 0 0 970.31 42.06 -4 0 0 931.62 42.15 -4 0 0 951.92 42.12 -4 0 0 947.82 42.15 -4 0 0 1000.00 42.12 3 -1 -1 256.12 11.33 3 -1 -1 262.39 11.25 3 -1 -1 256.06 11.31 3 -1 -1 239.34 11.22 3 -1 -1 252.13 11.31 3 -1 -1 244.67 11.31 3 -1 -1 250.84 11.26 -3 1 1 238.12 11.22 -3 1 1 263.53 11.33 -3 1 1 262.28 11.26 -3 1 1 256.63 11.33 -3 1 1 252.18 11.26 2 -2 -2 17.02 1.10 2 -2 -2 17.14 1.14 2 -2 -2 18.72 1.06 2 -2 -2 18.30 1.03 2 -2 -2 18.75 1.20 2 -2 -2 17.26 1.07 2 -2 -2 18.81 1.17 2 -2 -2 17.01 1.11 -2 2 2 15.86 1.13 -2 2 2 16.36 1.19 -2 2 2 15.21 1.00 -2 2 2 16.05 1.04 -2 2 2 16.44 1.14 1 -3 -3 108.90 5.25 1 -3 -3 108.79 5.21 1 -3 -3 112.62 5.22 1 -3 -3 112.03 5.01 1 -3 -3 109.48 5.24 1 -3 -3 106.12 5.09 1 -3 -3 105.93 5.08 -1 3 3 107.66 5.22 -1 3 3 101.30 5.19 -1 3 3 103.68 5.07 -1 3 3 113.82 5.23 -1 3 3 104.28 5.09 -1 3 3 106.19 4.98 0 -4 -4 95.77 4.98 0 -4 -4 107.67 5.02 0 -4 -4 100.29 5.04 0 -4 -4 100.83 5.00 0 -4 -4 98.63 4.78 0 -4 -4 105.80 4.88 0 4 4 97.03 4.77 0 4 4 97.39 4.67 0 4 4 99.44 4.99 0 4 4 94.58 4.98 0 4 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4.25 1.41 -17 -25 1 4.07 1.49 16 24 -2 3.56 1.46 16 24 -2 1.20 0.98 16 24 -2 2.22 1.36 -16 -24 2 0.24 1.26 -16 -24 2 0.44 0.77 -16 -24 2 0.90 1.24 15 23 -3 16.57 1.80 15 23 -3 18.13 2.20 15 23 -3 18.23 2.25 -15 -23 3 14.56 2.14 -15 -23 3 19.49 2.24 -15 -23 3 14.27 2.11 -15 -23 3 17.58 1.33 14 22 -4 0.86 0.87 14 22 -4 1.20 1.30 14 22 -4 1.35 1.31 14 22 -4 -0.66 0.84 -14 -22 4 -1.12 1.01 -14 -22 4 0.93 0.60 -14 -22 4 0.70 1.13 -14 -22 4 -0.25 1.08 13 21 -5 14.21 2.04 13 21 -5 15.38 2.14 13 21 -5 15.26 1.56 13 21 -5 14.44 1.77 -13 -21 5 15.12 1.91 -13 -21 5 12.73 2.00 -13 -21 5 15.72 2.13 12 20 -6 3.84 0.82 12 20 -6 7.01 1.10 12 20 -6 6.90 1.67 12 20 -6 4.48 1.62 12 20 -6 4.84 1.26 -12 -20 6 6.13 1.36 -12 -20 6 3.03 1.44 -12 -20 6 6.22 1.71 11 19 -7 11.40 1.33 11 19 -7 7.25 1.08 11 19 -7 9.40 1.32 11 19 -7 8.34 1.59 11 19 -7 12.08 2.06 -11 -19 7 9.62 1.97 -11 -19 7 10.63 1.62 -11 -19 7 9.77 2.00 10 18 -8 10.21 1.81 10 18 -8 10.02 1.33 10 18 -8 15.59 2.44 10 18 -8 9.96 1.54 10 18 -8 10.82 1.46 -10 -18 8 8.22 1.99 -10 -18 8 12.35 1.73 -10 -18 8 9.33 1.91 9 17 -9 10.06 1.42 9 17 -9 12.75 2.10 9 17 -9 12.51 2.26 9 17 -9 10.32 1.66 -9 -17 9 10.84 1.63 -9 -17 9 8.84 2.15 -9 -17 9 8.67 1.93 8 16 -10 10.73 1.58 8 16 -10 7.07 1.81 8 16 -10 10.40 1.88 8 16 -10 12.88 2.51 -8 -16 10 11.77 2.31 -8 -16 10 11.43 2.13 -8 -16 10 13.38 2.55 7 15 -11 26.39 2.78 7 15 -11 25.92 2.35 7 15 -11 25.73 3.00 7 15 -11 25.32 3.12 -7 -15 11 27.50 3.20 -7 -15 11 28.62 3.22 -7 -15 11 31.89 2.83 6 14 -12 9.88 2.04 6 14 -12 14.22 2.56 -6 -14 12 6.77 2.04 -6 -14 12 8.02 2.17 -6 -14 12 8.32 1.92 5 13 -13 2.19 1.50 5 13 -13 3.02 1.74 -5 -13 13 -1.38 1.54 -5 -13 13 2.58 1.82 4 12 -14 3.49 1.74 4 12 -14 3.02 1.82 -4 -12 14 4.39 2.12 -4 -12 14 2.84 2.04 26 32 6 -0.60 2.00 26 32 6 1.59 2.12 26 32 6 0.41 1.72 -26 -32 -6 1.94 2.18 25 31 5 10.66 2.41 25 31 5 5.63 2.29 25 31 5 7.58 2.54 -25 -31 -5 8.39 2.19 -25 -31 -5 8.53 2.45 24 30 4 7.96 2.26 24 30 4 5.99 1.87 24 30 4 6.13 2.20 24 30 4 6.27 1.74 -24 -30 -4 5.03 2.06 -24 -30 -4 8.07 2.05 23 29 3 0.67 1.58 23 29 3 2.31 1.79 -23 -29 -3 3.54 1.70 -23 -29 -3 1.68 1.79 22 28 2 1.66 1.73 22 28 2 1.06 1.61 -22 -28 -2 2.10 1.61 -22 -28 -2 1.28 1.53 21 27 1 0.58 1.46 21 27 1 0.43 1.49 -21 -27 -1 5.61 1.73 -21 -27 -1 3.73 1.65 20 26 0 2.40 1.55 20 26 0 1.63 1.48 -20 -26 0 3.28 1.62 -20 -26 0 4.69 1.67 -20 -26 0 3.97 1.71 19 25 -1 5.21 1.77 19 25 -1 13.33 2.25 19 25 -1 11.15 1.51 -19 -25 1 8.48 1.92 -19 -25 1 7.74 1.98 18 24 -2 4.28 1.71 18 24 -2 5.52 1.19 18 24 -2 1.87 1.40 -18 -24 2 5.23 1.64 -18 -24 2 4.64 1.12 -18 -24 2 5.81 1.78 17 23 -3 12.69 2.17 17 23 -3 13.45 1.64 17 23 -3 10.70 2.03 -17 -23 3 11.73 1.30 -17 -23 3 12.53 2.17 -17 -23 3 9.50 1.86 16 22 -4 4.56 1.60 16 22 -4 3.26 1.11 16 22 -4 3.05 1.46 16 22 -4 4.10 0.77 -16 -22 4 1.86 1.42 -16 -22 4 3.74 1.50 -16 -22 4 3.05 0.88 -16 -22 4 3.51 1.45 15 21 -5 10.83 1.59 15 21 -5 7.75 1.84 15 21 -5 9.30 1.95 15 21 -5 10.55 1.20 -15 -21 5 8.73 1.09 -15 -21 5 9.74 1.92 -15 -21 5 8.35 1.64 -15 -21 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2.23 6 44 -8 1.27 2.02 -6 -44 8 1.42 2.23 -6 -44 8 3.53 2.10 5 43 -9 -2.17 1.88 5 43 -9 0.71 2.44 -5 -43 9 3.06 2.23 -5 -43 9 3.23 2.34 13 49 -3 3.43 1.95 13 49 -3 -3.78 1.81 13 49 -3 2.51 2.35 -13 -49 3 1.41 1.90 -13 -49 3 -2.80 1.62 12 48 -4 1.89 2.18 12 48 -4 -0.92 1.55 12 48 -4 -0.12 2.27 -12 -48 4 1.05 2.03 -12 -48 4 3.33 2.08 11 47 -5 -0.45 2.23 11 47 -5 -0.98 2.04 11 47 -5 -0.29 1.61 -11 -47 5 2.61 2.15 -11 -47 5 2.75 2.42 10 46 -6 6.02 2.43 10 46 -6 6.29 2.76 10 46 -6 2.73 2.23 -10 -46 6 5.04 2.29 -10 -46 6 4.16 2.25 9 45 -7 2.48 2.03 9 45 -7 -1.86 2.11 -9 -45 7 -0.74 1.99 -9 -45 7 0.47 1.91 8 44 -8 1.43 2.13 8 44 -8 -2.99 1.98 -8 -44 8 0.13 1.77 -8 -44 8 0.22 2.30 14 48 -4 -2.51 2.07 14 48 -4 2.07 1.83 14 48 -4 -1.13 2.05 -14 -48 4 0.46 2.02 -14 -48 4 1.19 2.14 -14 -48 4 -0.43 1.85 13 47 -5 0.81 2.24 13 47 -5 0.20 1.87 13 47 -5 -2.85 2.00 -13 -47 5 -2.29 1.75 -13 -47 5 -1.07 1.81 -13 -47 5 2.07 2.55 12 46 -6 1.86 2.41 12 46 -6 7.12 2.37 12 46 -6 3.66 2.66 -12 -46 6 4.24 2.38 -12 -46 6 7.65 2.75 11 45 -7 3.65 2.31 11 45 -7 1.14 2.34 11 45 -7 -0.86 1.75 -11 -45 7 4.42 2.44 -11 -45 7 5.09 2.64 -7 53 -1 1.99 2.21 -7 53 -1 3.50 2.32 -7 53 -1 1.28 2.12 7 -53 1 1.73 1.88 7 -53 1 1.69 2.32 -8 52 -2 5.55 2.31 -8 52 -2 4.57 2.15 8 -52 2 2.32 2.45 8 -52 2 5.01 2.25 -9 51 -3 8.70 2.64 -9 51 -3 13.89 2.89 9 -51 3 11.85 2.84 9 -51 3 16.22 3.07 -10 50 -4 4.53 2.38 -10 50 -4 2.82 2.30 10 -50 4 0.28 1.97 10 -50 4 2.59 2.24 -5 53 -1 2.81 2.04 -5 53 -1 1.84 1.94 -5 53 -1 1.13 2.23 5 -53 1 -1.43 1.67 5 -53 1 -0.04 1.99 -6 52 -2 4.33 2.07 -6 52 -2 4.60 2.28 -6 52 -2 2.23 1.98 6 -52 2 3.53 2.11 6 -52 2 3.83 2.30 -7 51 -3 2.55 2.16 -7 51 -3 3.07 2.18 7 -51 3 1.90 1.96 7 -51 3 3.78 2.34 -8 50 -4 3.63 2.18 -8 50 -4 6.74 2.49 8 -50 4 5.16 2.40 8 -50 4 4.03 2.08 -9 49 -5 -1.17 2.02 -9 49 -5 1.32 2.17 9 -49 5 0.54 1.95 9 -49 5 0.12 1.97 -2 54 0 6.31 2.39 -2 54 0 2.60 2.10 2 -54 0 1.22 2.18 -3 53 -1 6.12 2.31 -3 53 -1 9.46 2.53 -3 53 -1 5.76 2.42 3 -53 1 4.24 2.04 3 -53 1 4.60 2.49 -4 52 -2 5.54 2.21 -4 52 -2 -1.00 1.83 -4 52 -2 3.97 2.14 4 -52 2 1.12 2.17 4 -52 2 3.18 1.94 -5 51 -3 5.24 2.27 -5 51 -3 5.65 2.20 5 -51 3 4.53 2.18 5 -51 3 9.16 2.80 -6 50 -4 1.02 1.80 -6 50 -4 1.03 2.12 6 -50 4 3.86 2.02 6 -50 4 1.87 2.03 -7 49 -5 -0.01 2.12 -7 49 -5 -0.20 1.99 7 -49 5 0.89 1.93 7 -49 5 1.42 2.07 -8 48 -6 2.89 2.25 -8 48 -6 2.17 2.39 8 -48 6 2.04 1.92 8 -48 6 4.79 2.46 0 54 0 -1.84 1.66 0 54 0 0.58 1.79 0 54 0 0.25 2.07 0 -54 0 1.62 2.05 -1 53 -1 2.83 2.24 -1 53 -1 0.87 1.90 -1 53 -1 3.62 2.07 1 -53 1 1.24 2.13 1 -53 1 2.00 1.78 -2 52 -2 3.13 2.11 -2 52 -2 1.09 1.76 -2 52 -2 1.08 2.03 2 -52 2 1.85 1.78 2 -52 2 1.33 2.02 -3 51 -3 0.96 2.03 -3 51 -3 4.93 2.11 3 -51 3 4.59 2.22 3 -51 3 6.70 2.53 -4 50 -4 0.81 1.87 -4 50 -4 -0.86 2.00 4 -50 4 0.12 2.01 4 -50 4 0.01 1.78 -5 49 -5 -0.06 2.10 -5 49 -5 0.11 1.80 5 -49 5 -1.41 1.59 5 -49 5 0.70 1.83 -6 48 -6 1.33 2.28 -6 48 -6 0.31 1.82 6 -48 6 -1.16 1.84 6 -48 6 1.22 1.93 -7 47 -7 -0.87 2.01 2 54 0 1.68 2.01 2 54 0 0.30 1.82 -2 -54 0 0.20 2.06 1 53 -1 1.69 1.90 1 53 -1 -1.57 1.97 1 53 -1 4.39 2.10 -1 -53 1 2.09 1.82 -1 -53 1 2.89 2.31 0 52 -2 -1.40 1.84 0 52 -2 3.31 1.95 0 52 -2 1.23 1.85 0 -52 2 1.74 1.78 0 -52 2 0.32 2.01 -1 51 -3 3.35 2.04 -1 51 -3 -1.66 2.01 1 -51 3 -1.92 1.47 1 -51 3 2.02 1.93 -2 50 -4 2.10 2.42 -2 50 -4 2.61 1.91 2 -50 4 5.23 2.31 2 -50 4 2.67 1.97 -3 49 -5 -2.64 1.55 -3 49 -5 -3.30 2.04 3 -49 5 -0.18 1.55 3 -49 5 2.20 2.10 -4 48 -6 0.42 2.27 -4 48 -6 0.11 1.96 4 -48 6 2.56 1.97 4 -48 6 3.02 2.17 -5 47 -7 -1.90 2.18 -5 47 -7 1.65 1.97 5 -47 7 1.92 2.30 5 -47 7 3.76 2.22 3 53 -1 5.55 2.38 3 53 -1 6.85 2.34 3 53 -1 6.66 2.63 -3 -53 1 8.39 2.20 -3 -53 1 9.62 2.62 2 52 -2 -0.48 1.59 2 52 -2 -0.90 1.74 2 52 -2 3.71 2.21 2 52 -2 1.29 1.89 -2 -52 2 1.77 2.01 -2 -52 2 -0.25 1.67 1 51 -3 0.08 2.06 1 51 -3 -0.62 1.61 -1 -51 3 1.22 1.76 -1 -51 3 1.37 2.04 0 50 -4 -1.58 1.83 0 50 -4 1.43 1.76 0 -50 4 0.87 1.90 0 -50 4 0.86 2.09 -1 49 -5 -1.27 2.15 -1 49 -5 3.07 2.18 1 -49 5 -0.02 1.62 1 -49 5 -3.11 1.95 1 -49 5 -0.98 1.70 -2 48 -6 1.65 2.31 -2 48 -6 3.48 2.16 2 -48 6 -1.27 1.80 2 -48 6 0.60 2.31 -3 47 -7 1.67 2.42 -3 47 -7 2.01 2.03 3 -47 7 0.48 1.97 3 -47 7 2.27 2.37 5 53 -1 -1.78 1.79 5 53 -1 2.51 2.16 5 53 -1 0.99 1.77 -5 -53 1 3.61 2.42 -5 -53 1 -1.23 1.64 -5 -53 1 1.37 2.13 4 52 -2 0.85 2.09 4 52 -2 -0.07 1.75 4 52 -2 6.27 2.23 4 52 -2 2.85 1.93 -4 -52 2 3.42 1.90 -4 -52 2 0.88 2.19 -4 -52 2 2.02 2.14 3 51 -3 3.70 2.14 3 51 -3 5.84 2.37 3 51 -3 6.79 2.31 3 51 -3 1.91 2.18 -3 -51 3 5.30 2.37 -3 -51 3 2.04 1.83 -3 -51 3 6.64 2.51 2 50 -4 -1.12 1.96 2 50 -4 1.11 1.79 -2 -50 4 5.50 2.17 -2 -50 4 2.05 2.29 -2 -50 4 7.13 2.56 1 49 -5 -1.79 2.00 1 49 -5 2.58 2.08 -1 -49 5 0.44 2.17 -1 -49 5 0.08 1.69 0 48 -6 -2.34 2.05 0 48 -6 2.08 2.07 0 -48 6 -1.80 2.03 0 -48 6 1.07 1.90 -1 47 -7 2.93 2.18 -1 47 -7 2.90 2.50 1 -47 7 2.92 2.31 1 -47 7 7.39 2.44 7 53 -1 -0.81 2.10 7 53 -1 3.76 2.19 7 53 -1 1.68 1.85 -7 -53 1 2.83 2.35 -7 -53 1 1.02 1.94 -7 -53 1 -0.93 2.06 6 52 -2 4.70 1.98 6 52 -2 1.91 2.12 6 52 -2 3.55 2.02 6 52 -2 7.00 2.36 -6 -52 2 -1.18 1.93 -6 -52 2 3.21 1.92 -6 -52 2 6.46 2.48 5 51 -3 8.16 2.30 5 51 -3 7.25 2.42 5 51 -3 5.74 2.17 5 51 -3 3.99 2.41 -5 -51 3 3.66 2.26 -5 -51 3 7.03 2.23 -5 -51 3 4.00 2.47 4 50 -4 1.40 2.32 4 50 -4 1.01 2.15 4 50 -4 1.15 1.93 -4 -50 4 -0.28 1.64 -4 -50 4 1.79 2.27 3 49 -5 0.03 1.88 3 49 -5 -1.90 2.20 -3 -49 5 1.02 2.21 -3 -49 5 -0.08 1.59 2 48 -6 0.55 1.92 2 48 -6 -1.33 1.99 -2 -48 6 -0.32 1.75 -2 -48 6 -0.10 2.13 1 47 -7 2.57 2.10 1 47 -7 2.04 2.39 -1 -47 7 6.43 2.44 -1 -47 7 1.50 2.35 0 46 -8 -0.60 2.34 0 46 -8 4.23 2.48 0 -46 8 -0.40 2.17 8 52 -2 4.13 2.41 8 52 -2 0.98 2.14 8 52 -2 6.14 2.28 -8 -52 2 4.96 2.44 -8 -52 2 4.15 2.20 7 51 -3 4.48 2.31 7 51 -3 1.55 2.31 7 51 -3 8.51 2.26 7 51 -3 4.98 2.05 -7 -51 3 5.68 2.56 -7 -51 3 4.84 2.28 6 50 -4 2.67 2.47 6 50 -4 2.70 1.95 6 50 -4 1.74 2.19 -6 -50 4 1.23 1.97 -6 -50 4 1.68 1.88 5 49 -5 -2.43 2.20 5 49 -5 0.66 1.89 -5 -49 5 2.10 2.32 -5 -49 5 1.80 1.85 4 48 -6 -1.10 1.83 4 48 -6 1.19 2.44 -4 -48 6 2.26 2.35 -4 -48 6 -1.42 1.73 3 47 -7 -1.36 2.24 3 47 -7 1.79 2.10 -3 -47 7 1.47 1.96 -3 -47 7 1.55 2.35 9 51 -3 7.20 2.60 9 51 -3 9.31 2.93 9 51 -3 5.98 2.17 -9 -51 3 11.56 2.97 -9 -51 3 9.26 2.58 8 50 -4 1.41 1.88 8 50 -4 4.83 2.49 8 50 -4 4.41 2.44 -8 -50 4 4.42 2.29 -8 -50 4 6.93 2.51 7 49 -5 2.00 2.15 7 49 -5 -1.14 1.66 7 49 -5 -1.50 2.03 -7 -49 5 -0.80 2.20 -7 -49 5 -0.93 1.66 6 48 -6 -0.15 2.32 6 48 -6 -1.47 1.71 -6 -48 6 -1.48 1.94 -6 -48 6 1.20 1.96 5 47 -7 2.59 2.12 5 47 -7 1.17 2.47 -5 -47 7 2.03 2.19 -5 -47 7 1.61 2.37 10 50 -4 2.25 1.86 10 50 -4 1.92 2.43 10 50 -4 -1.58 1.94 -10 -50 4 0.44 1.97 -10 -50 4 3.94 2.41 9 49 -5 0.53 2.24 9 49 -5 -2.09 2.06 9 49 -5 0.50 1.80 -9 -49 5 1.94 2.05 -9 -49 5 -0.08 2.14 8 48 -6 -2.31 2.18 8 48 -6 5.37 2.54 8 48 -6 0.71 1.96 -8 -48 6 4.11 2.22 -8 -48 6 0.39 1.99 7 47 -7 1.87 2.48 7 47 -7 2.08 2.18 -7 -47 7 2.49 2.23 -1 53 -3 1.29 1.99 -1 53 -3 -2.43 1.95 -2 52 -4 -0.43 2.14 -2 52 -4 1.09 1.89 2 -52 4 4.33 2.28 2 -52 4 2.36 1.96 1 53 -3 0.75 2.03 1 53 -3 2.81 2.09 1 53 -3 1.31 2.28 -1 -53 3 2.26 2.26 0 52 -4 10.59 2.82 0 52 -4 11.29 2.67 0 -52 4 7.64 2.48 0 -52 4 13.78 2.87 0 -52 4 10.77 3.13 -1 51 -5 -4.02 1.90 -1 51 -5 -3.58 1.70 1 -51 5 2.46 2.14 1 -51 5 2.56 1.96 1 -51 5 0.03 2.12 2 52 -4 0.94 2.33 2 52 -4 0.47 1.78 -2 -52 4 0.84 2.26 -2 -52 4 0.38 1.79 -2 -52 4 0.37 1.98 1 51 -5 0.99 1.88 1 51 -5 1.45 2.42 -1 -51 5 4.51 2.21 -1 -51 5 1.55 2.43 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 58113 _shelx_res_file ; TITL jl2109 in Fdd2 jl2109.res created by SHELXL-2018/3 at 16:44:14 on 22-Jun-2021 CELL 0.71073 31.6757 44.8058 12.6056 90.000 90.000 90.000 ZERR 8.00 0.0022 0.0029 0.0008 0.000 0.000 0.000 LATT -4 SYMM -X, -Y, Z SYMM 0.25+X, 0.25-Y, 0.25+Z SYMM 0.25-X, 0.25+Y, 0.25+Z SFAC C H N O F Fe UNIT 584 639.55 72 259.78 16 64 LIST 4 L.S. 10 ACTA EQIV $1 x+1/4, -y+3/4, z+3/4 HTAB C11 N5_$1 EQIV $2 x, y, z-1 HTAB C13 F1_$2 EQIV $3 -x+1, -y+1/2, z-1/2 HTAB C15 F1_$3 EQIV $4 -x+3/4, y+1/4, z+3/4 HTAB C17 O17_$4 HTAB C19 F1_$3 EQIV $5 -x+1, -y+1/2, z+1/2 HTAB C19 O11_$5 HTAB C20 O13 HTAB C20 O15 HTAB C23 O5_$1 HTAB C25 O1 EQIV $6 x-1/4, -y+3/4, z+1/4 HTAB C26 O6_$6 HTAB C29 F1 HTAB C31 O2_$2 EQIV $7 x-1/4, -y+3/4, z-3/4 HTAB C39 O6_$7 EQIV $8 -x+3/4, y-1/4, z-3/4 HTAB O17 O13_$8 BOND $H ISOR 0.01 N5 C35 C36 C37 C38 C39 O17 DFIX 0.84 O17 H17D O17 H17E DANG 1.35 H17D H17E TWIN -1 0 0 0 -1 0 0 0 -1 2 FMAP 2 PLAN 10 SIZE 0.144 0.304 0.328 TEMP -173.000 WGHT 0.039200 78.008003 EXTI 0.000039 BASF 0.04685 FVAR 0.01665 0.23583 FE4 6 0.541616 0.311815 0.778906 11.00000 0.01812 0.02478 = 0.00815 0.00103 -0.00200 -0.00036 FE3 6 0.487069 0.348740 0.601743 11.00000 0.01628 0.02658 = 0.00872 0.00091 -0.00253 -0.00007 FE1 6 0.527402 0.307479 1.073000 11.00000 0.01810 0.02744 = 0.00774 0.00089 0.00039 0.00072 FE2 6 0.536471 0.384304 0.796111 11.00000 0.02190 0.02563 = 0.00929 0.00082 -0.00321 -0.00168 C1 1 0.525004 0.368988 1.034464 11.00000 0.00578 0.03235 = 0.01495 -0.00171 -0.00133 0.00029 C2 1 0.525470 0.400901 1.058397 11.00000 0.00903 0.02780 = 0.01659 -0.00156 -0.00186 0.00479 C3 1 0.517542 0.409240 1.164600 11.00000 0.01538 0.03186 = 0.01273 0.00187 0.00230 0.00077 AFIX 43 H3 2 0.509743 0.394293 1.214328 11.00000 -1.20000 AFIX 0 C4 1 0.520761 0.438214 1.197995 11.00000 0.01976 0.03609 = 0.01967 -0.00857 0.00040 0.00124 AFIX 43 H4 2 0.515227 0.443221 1.269894 11.00000 -1.20000 AFIX 0 C5 1 0.532176 0.460240 1.126000 11.00000 0.03490 0.03024 = 0.02540 -0.00931 0.00085 0.00239 AFIX 43 H5 2 0.534580 0.480378 1.148789 11.00000 -1.20000 AFIX 0 C6 1 0.540053 0.452965 1.021286 11.00000 0.03317 0.02499 = 0.02120 0.00074 0.00116 -0.00099 AFIX 43 H6 2 0.547500 0.468274 0.972619 11.00000 -1.20000 AFIX 0 C7 1 0.537244 0.423370 0.985617 11.00000 0.01595 0.03259 = 0.01233 0.00134 -0.00257 0.00219 C8 1 0.441483 0.391848 0.744365 11.00000 0.03124 0.04250 = 0.01148 0.00356 -0.00112 0.00552 C9 1 0.399624 0.404970 0.775138 11.00000 0.03632 0.09774 = 0.02536 -0.01340 -0.00759 0.02856 AFIX 137 H9A 2 0.404201 0.422996 0.817643 11.00000 -1.50000 H9B 2 0.383642 0.390370 0.816831 11.00000 -1.50000 H9C 2 0.383705 0.410109 0.711027 11.00000 -1.50000 AFIX 0 C10 1 0.540440 0.403505 0.566465 11.00000 0.03058 0.03568 = 0.01725 0.00759 -0.01383 -0.00894 C11 1 0.563788 0.422159 0.487065 11.00000 0.06025 0.07969 = 0.02591 0.02272 -0.00998 -0.03804 AFIX 137 H11A 2 0.554177 0.442903 0.491977 11.00000 -1.50000 H11B 2 0.558316 0.414546 0.415493 11.00000 -1.50000 H11C 2 0.594135 0.421223 0.501821 11.00000 -1.50000 AFIX 0 C12 1 0.547901 0.301501 0.541437 11.00000 0.01935 0.02980 = 0.00987 -0.00369 0.00261 -0.00223 C13 1 0.567328 0.282925 0.454827 11.00000 0.03387 0.03482 = 0.00645 0.00071 0.00596 0.00769 AFIX 137 H13A 2 0.564363 0.293303 0.386799 11.00000 -1.50000 H13B 2 0.552940 0.263589 0.451135 11.00000 -1.50000 H13C 2 0.597333 0.279782 0.470129 11.00000 -1.50000 AFIX 0 C14 1 0.454513 0.293596 0.717278 11.00000 0.01899 0.02670 = 0.01232 -0.00549 0.00214 0.00062 C15 1 0.419540 0.271101 0.725955 11.00000 0.02067 0.03445 = 0.02042 0.00316 -0.00217 -0.00403 AFIX 137 H15A 2 0.405490 0.273258 0.794794 11.00000 -1.50000 H15B 2 0.431269 0.250936 0.719784 11.00000 -1.50000 H15C 2 0.399037 0.274430 0.668949 11.00000 -1.50000 AFIX 0 C16 1 0.619590 0.349986 0.789527 11.00000 0.02286 0.03560 = 0.00548 -0.00066 -0.00211 -0.00259 C17 1 0.666964 0.350915 0.798315 11.00000 0.01878 0.04584 = 0.02129 -0.00223 -0.00127 -0.00215 AFIX 137 H17A 2 0.678782 0.331942 0.773528 11.00000 -1.50000 H17B 2 0.675002 0.354151 0.872503 11.00000 -1.50000 H17C 2 0.677951 0.367257 0.754637 11.00000 -1.50000 AFIX 0 C18 1 0.549767 0.257121 0.918921 11.00000 0.01771 0.03689 = 0.00773 0.00047 0.00193 -0.00387 C19 1 0.550388 0.224527 0.906295 11.00000 0.05224 0.02646 = 0.01307 0.00073 0.00997 -0.00642 AFIX 137 H19A 2 0.574786 0.218749 0.863130 11.00000 -1.50000 H19B 2 0.524375 0.218023 0.871126 11.00000 -1.50000 H19C 2 0.552416 0.215068 0.976207 11.00000 -1.50000 AFIX 0 SAME N5 C35 C36 C37 C38 C39 N2 3 0.594761 0.313228 1.097157 11.00000 0.01891 0.02957 = 0.00921 0.00090 -0.00148 -0.00328 C20 1 0.624844 0.304871 1.028195 11.00000 0.02490 0.05010 = 0.00724 -0.00379 -0.00302 -0.00163 AFIX 43 H20 2 0.616422 0.295587 0.963831 11.00000 -1.20000 AFIX 0 C21 1 0.666684 0.309043 1.045971 11.00000 0.02298 0.07734 = 0.01773 -0.00749 0.00521 -0.00237 AFIX 43 H21 2 0.686801 0.302801 0.994668 11.00000 -1.20000 AFIX 0 C22 1 0.679879 0.322385 1.138847 11.00000 0.01680 0.06197 = 0.02897 0.00305 -0.00709 -0.00946 AFIX 43 H22 2 0.709048 0.325374 1.152790 11.00000 -1.20000 AFIX 0 C23 1 0.649528 0.331306 1.211214 11.00000 0.02929 0.03852 = 0.02144 0.00269 -0.00788 -0.00649 AFIX 43 H23 2 0.657353 0.340841 1.275592 11.00000 -1.20000 AFIX 0 C24 1 0.607896 0.326061 1.187815 11.00000 0.02768 0.03388 = 0.01451 -0.00094 -0.00301 -0.00091 AFIX 43 H24 2 0.587203 0.331804 1.238401 11.00000 -1.20000 AFIX 0 C25 1 0.436566 0.315870 0.991739 11.00000 0.02376 0.03163 = 0.01848 -0.00539 -0.00134 0.00219 AFIX 43 H25 2 0.449451 0.329993 0.945790 11.00000 -1.20000 AFIX 0 C26 1 0.393461 0.312567 0.989001 11.00000 0.02494 0.04034 = 0.01884 -0.00784 -0.00442 0.01257 AFIX 43 H26 2 0.376923 0.324675 0.943172 11.00000 -1.20000 AFIX 0 C27 1 0.374198 0.291514 1.053316 11.00000 0.02434 0.04279 = 0.02758 -0.01571 -0.00072 -0.00258 AFIX 43 H27 2 0.344487 0.288675 1.051419 11.00000 -1.20000 AFIX 0 C28 1 0.399125 0.274871 1.119812 11.00000 0.02466 0.04027 = 0.02744 -0.00692 0.00568 -0.00483 AFIX 43 H28 2 0.386806 0.260344 1.165143 11.00000 -1.20000 AFIX 0 C29 1 0.442491 0.279412 1.120387 11.00000 0.03146 0.03270 = 0.01407 -0.00401 0.00360 -0.00109 AFIX 43 H29 2 0.459466 0.267775 1.166747 11.00000 -1.20000 AFIX 0 C30 1 0.463683 0.349848 0.362550 11.00000 0.01421 0.02450 = 0.01740 0.00592 -0.00180 0.00004 AFIX 43 H30 2 0.493365 0.351881 0.354525 11.00000 -1.20000 AFIX 0 C31 1 0.438578 0.348770 0.272577 11.00000 0.02310 0.02785 = 0.01170 -0.00218 -0.00125 0.00124 AFIX 43 H31 2 0.450918 0.350379 0.204127 11.00000 -1.20000 AFIX 0 C32 1 0.395888 0.345369 0.283225 11.00000 0.02429 0.03381 = 0.01515 -0.00221 -0.00517 0.00344 AFIX 43 H32 2 0.378207 0.344755 0.222390 11.00000 -1.20000 AFIX 0 C33 1 0.378745 0.342827 0.384175 11.00000 0.01705 0.04199 = 0.01239 0.00101 -0.00007 -0.00035 AFIX 43 H33 2 0.349239 0.340097 0.393566 11.00000 -1.20000 AFIX 0 C34 1 0.405251 0.344333 0.470175 11.00000 0.01897 0.03635 = 0.01029 -0.00084 0.00424 -0.00051 AFIX 43 H34 2 0.393338 0.342633 0.539074 11.00000 -1.20000 AFIX 0 F1 5 0.524576 0.294974 1.212108 11.00000 0.02439 0.03809 = 0.00715 0.00267 0.00077 0.00100 N1 3 0.530521 0.359652 0.935370 11.00000 0.01564 0.02092 = 0.01249 0.00042 -0.00228 -0.00048 N3 3 0.461264 0.299683 1.057677 11.00000 0.02295 0.02508 = 0.01390 -0.00394 0.00131 -0.00097 N4 3 0.447215 0.348092 0.461758 11.00000 0.01527 0.02823 = 0.00970 0.00431 -0.00070 0.00338 O1 4 0.531197 0.328207 0.928994 11.00000 0.02050 0.02141 = 0.01151 -0.00365 -0.00306 -0.00100 O2 4 0.519460 0.350018 1.109859 11.00000 0.01903 0.03059 = 0.00934 0.00077 0.00018 -0.00092 O3 4 0.546691 0.417810 0.885172 11.00000 0.03317 0.02636 = 0.01170 0.00149 -0.00119 -0.00425 O4 4 0.473366 0.397446 0.799588 11.00000 0.02888 0.03852 = 0.02534 -0.00786 -0.00961 0.00608 O5 4 0.441283 0.374960 0.663046 11.00000 0.02366 0.04306 = 0.00810 -0.00449 -0.00592 0.00950 O6 4 0.547970 0.408230 0.663332 11.00000 0.03512 0.03164 = 0.01825 0.00476 -0.00411 -0.00917 O7 4 0.515013 0.384709 0.532169 11.00000 0.03109 0.03521 = 0.01508 0.00433 -0.00896 -0.00773 O8 4 0.554397 0.293094 0.635497 11.00000 0.02766 0.02867 = 0.01040 0.00106 -0.00087 0.00222 O9 4 0.525475 0.323265 0.514591 11.00000 0.02223 0.03677 = 0.01238 0.00355 -0.00264 0.00888 O10 4 0.484827 0.291147 0.781245 11.00000 0.02256 0.03005 = 0.01353 0.00360 -0.00345 -0.00430 O11 4 0.451837 0.313060 0.644720 11.00000 0.02678 0.03116 = 0.01181 0.00544 -0.00646 -0.00212 O12 4 0.599835 0.374348 0.790944 11.00000 0.02635 0.02639 = 0.01561 0.00032 -0.00009 -0.00110 O13 4 0.602804 0.324486 0.784634 11.00000 0.02152 0.02781 = 0.01354 0.00037 0.00188 -0.00257 O14 4 0.536572 0.267761 1.006770 11.00000 0.02387 0.02813 = 0.00987 -0.00018 0.00043 0.00449 O15 4 0.562414 0.273376 0.843518 11.00000 0.01939 0.02941 = 0.01228 0.00095 -0.00077 -0.00079 O16 4 0.521580 0.348200 0.722240 11.00000 0.01514 0.03036 = 0.00892 -0.00057 0.00104 -0.00153 PART -1 N5 3 0.285753 0.267051 -0.144400 10.50000 0.18362 0.13998 = 0.14057 -0.00863 0.03538 -0.00512 C35 1 0.294008 0.237851 -0.162513 10.50000 0.15763 0.10057 = 0.12132 -0.01062 0.01092 -0.00527 AFIX 43 H35 2 0.311010 0.232929 -0.222080 10.50000 -1.20000 AFIX 0 C36 1 0.279661 0.215260 -0.101462 10.50000 0.08877 0.06675 = 0.06415 -0.00797 0.02330 -0.01901 AFIX 43 H36 2 0.283212 0.195132 -0.123399 10.50000 -1.20000 AFIX 0 C37 1 0.259601 0.221814 -0.005983 10.50000 0.06649 0.04201 = 0.08045 -0.00535 0.00233 -0.01359 AFIX 43 H37 2 0.254457 0.206792 0.045608 10.50000 -1.20000 AFIX 0 C38 1 0.247303 0.251503 0.010888 10.50000 0.07722 0.06697 = 0.07748 0.00503 0.00251 -0.01184 AFIX 43 H38 2 0.227845 0.256511 0.065403 10.50000 -1.20000 AFIX 0 C39 1 0.264329 0.273334 -0.054186 10.50000 0.11200 0.07340 = 0.09895 0.00020 0.01679 -0.02643 AFIX 43 H39 2 0.260803 0.293654 -0.034580 10.50000 -1.20000 AFIX 0 PART 0 O17 4 0.085104 0.024771 0.026504 21.00000 0.06332 0.04747 = 0.09479 -0.00925 0.00757 -0.01567 AFIX 3 H17D 2 0.071299 0.026512 -0.031577 21.00000 -1.50000 H17E 2 0.105232 0.036950 0.018911 21.00000 -1.50000 AFIX 0 HKLF 4 REM jl2109 in Fdd2 REM wR2 = 0.0902, GooF = S = 1.045, Restrained GooF = 1.047 for all data REM R1 = 0.0385 for 7012 Fo > 4sig(Fo) and 0.0547 for all 8265 data REM 604 parameters refined using 58 restraints END WGHT 0.0391 78.0729 REM Highest difference peak 0.472, deepest hole -0.379, 1-sigma level 0.082 Q1 1 0.0672 0.0296 -0.0783 11.00000 0.05 0.47 Q2 1 0.4825 0.3233 0.6026 11.00000 0.05 0.39 Q3 1 0.2903 0.2154 0.0736 11.00000 0.05 0.38 Q4 1 0.5397 0.4139 0.7852 11.00000 0.05 0.36 Q5 1 0.5273 0.3332 1.0696 11.00000 0.05 0.35 Q6 1 0.5422 0.3433 0.7773 11.00000 0.05 0.34 Q7 1 0.4838 0.3733 0.5971 11.00000 0.05 0.32 Q8 1 0.5474 0.3557 0.7617 11.00000 0.05 0.32 Q9 1 0.6000 0.3964 0.7888 11.00000 0.05 0.32 Q10 1 0.5411 0.3618 0.7880 11.00000 0.05 0.32 ; _shelx_res_checksum 68328 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe4 0.54162(3) 0.31181(2) 0.77891(6) 0.0170(2) Uani d 1 . . Fe Fe3 0.48707(3) 0.34874(2) 0.60174(7) 0.0172(2) Uani d 1 . . Fe Fe1 0.52740(3) 0.30748(2) 1.07300(7) 0.0178(2) Uani d 1 . . Fe Fe2 0.53647(3) 0.38430(2) 0.79611(7) 0.0189(2) Uani d 1 . . C C1 0.52500(18) 0.36899(15) 1.0345(5) 0.0177(14) Uani d 1 . . C C2 0.52547(19) 0.40090(15) 1.0584(5) 0.0178(14) Uani d 1 . . C C3 0.5175(2) 0.40924(16) 1.1646(5) 0.0200(15) Uani d 1 . . H H3 0.509743 0.394293 1.214328 0.024 Uiso calc 1 . . C C4 0.5208(2) 0.43821(16) 1.1980(5) 0.0252(17) Uani d 1 . . H H4 0.515227 0.443221 1.269894 0.030 Uiso calc 1 . . C C5 0.5322(2) 0.46024(18) 1.1260(6) 0.0302(18) Uani d 1 . . H H5 0.534580 0.480378 1.148789 0.036 Uiso calc 1 . . C C6 0.5401(2) 0.45296(16) 1.0213(6) 0.0265(16) Uani d 1 . . H H6 0.547500 0.468274 0.972619 0.032 Uiso calc 1 . . C C7 0.5372(2) 0.42337(16) 0.9856(5) 0.0203(15) Uani d 1 . . C C8 0.4415(2) 0.39185(17) 0.7444(5) 0.0284(17) Uani d 1 . . C C9 0.3996(3) 0.4050(2) 0.7751(7) 0.053(3) Uani d 1 . . H H9A 0.404201 0.422996 0.817643 0.080 Uiso calc 1 . . H H9B 0.383642 0.390370 0.816831 0.080 Uiso calc 1 . . H H9C 0.383705 0.410109 0.711027 0.080 Uiso calc 1 . . C C10 0.5404(2) 0.40351(17) 0.5665(5) 0.0278(17) Uani d 1 . . C C11 0.5638(3) 0.4222(2) 0.4871(7) 0.055(3) Uani d 1 . . H H11A 0.554177 0.442903 0.491977 0.083 Uiso calc 1 . . H H11B 0.558316 0.414546 0.415493 0.083 Uiso calc 1 . . H H11C 0.594135 0.421223 0.501821 0.083 Uiso calc 1 . . C C12 0.5479(2) 0.30150(15) 0.5414(5) 0.0197(14) Uani d 1 . . C C13 0.5673(2) 0.28292(16) 0.4548(5) 0.0250(16) Uani d 1 . . H H13A 0.564363 0.293303 0.386799 0.038 Uiso calc 1 . . H H13B 0.552940 0.263589 0.451135 0.038 Uiso calc 1 . . H H13C 0.597333 0.279782 0.470129 0.038 Uiso calc 1 . . C C14 0.4545(2) 0.29360(15) 0.7173(5) 0.0193(14) Uani d 1 . . C C15 0.4195(2) 0.27110(16) 0.7260(6) 0.0252(16) Uani d 1 . . H H15A 0.405490 0.273258 0.794794 0.038 Uiso calc 1 . . H H15B 0.431269 0.250936 0.719784 0.038 Uiso calc 1 . . H H15C 0.399037 0.274430 0.668949 0.038 Uiso calc 1 . . C C16 0.6196(2) 0.34999(17) 0.7895(5) 0.0213(14) Uani d 1 . . C C17 0.6670(2) 0.35092(17) 0.7983(6) 0.0286(16) Uani d 1 . . H H17A 0.678782 0.331942 0.773528 0.043 Uiso calc 1 . . H H17B 0.675002 0.354151 0.872503 0.043 Uiso calc 1 . . H H17C 0.677951 0.367257 0.754637 0.043 Uiso calc 1 . . C C18 0.5498(2) 0.25712(16) 0.9189(5) 0.0208(15) Uani d 1 . . C C19 0.5504(3) 0.22453(16) 0.9063(5) 0.0306(18) Uani d 1 . . H H19A 0.574786 0.218749 0.863130 0.046 Uiso calc 1 . . H H19B 0.524375 0.218023 0.871126 0.046 Uiso calc 1 . . H H19C 0.552416 0.215068 0.976207 0.046 Uiso calc 1 . . N N2 0.59476(16) 0.31323(12) 1.0972(4) 0.0192(12) Uani d 1 . . C C20 0.6248(2) 0.30487(17) 1.0282(5) 0.0274(17) Uani d 1 . . H H20 0.616422 0.295587 0.963831 0.033 Uiso calc 1 . . C C21 0.6667(2) 0.3090(2) 1.0460(6) 0.039(2) Uani d 1 . . H H21 0.686801 0.302801 0.994668 0.047 Uiso calc 1 . . C C22 0.6799(2) 0.32238(19) 1.1388(6) 0.036(2) Uani d 1 . . H H22 0.709048 0.325374 1.152790 0.043 Uiso calc 1 . . C C23 0.6495(2) 0.33131(17) 1.2112(6) 0.0297(17) Uani d 1 . . H H23 0.657353 0.340841 1.275592 0.036 Uiso calc 1 . . C C24 0.6079(2) 0.32606(16) 1.1878(5) 0.0254(16) Uani d 1 . . H H24 0.587203 0.331804 1.238401 0.030 Uiso calc 1 . . C C25 0.4366(2) 0.31587(16) 0.9917(5) 0.0246(16) Uani d 1 . . H H25 0.449451 0.329993 0.945790 0.030 Uiso calc 1 . . C C26 0.3935(2) 0.31257(17) 0.9890(5) 0.0280(17) Uani d 1 . . H H26 0.376923 0.324675 0.943172 0.034 Uiso calc 1 . . C C27 0.3742(2) 0.29151(17) 1.0533(6) 0.0316(18) Uani d 1 . . H H27 0.344487 0.288675 1.051419 0.038 Uiso calc 1 . . C C28 0.3991(2) 0.27487(17) 1.1198(6) 0.0308(18) Uani d 1 . . H H28 0.386806 0.260344 1.165143 0.037 Uiso calc 1 . . C C29 0.4425(2) 0.27941(16) 1.1204(5) 0.0261(16) Uani d 1 . . H H29 0.459466 0.267775 1.166747 0.031 Uiso calc 1 . . C C30 0.4637(2) 0.34985(15) 0.3626(5) 0.0187(14) Uani d 1 . . H H30 0.493365 0.351881 0.354525 0.022 Uiso calc 1 . . C C31 0.4386(2) 0.34877(15) 0.2726(5) 0.0209(14) Uani d 1 . . H H31 0.450918 0.350379 0.204127 0.025 Uiso calc 1 . . C C32 0.3959(2) 0.34537(16) 0.2832(6) 0.0244(15) Uani d 1 . . H H32 0.378207 0.344755 0.222390 0.029 Uiso calc 1 . . C C33 0.3787(2) 0.34283(16) 0.3842(5) 0.0238(16) Uani d 1 . . H H33 0.349239 0.340097 0.393566 0.029 Uiso calc 1 . . C C34 0.4053(2) 0.34433(15) 0.4702(5) 0.0219(15) Uani d 1 . . H H34 0.393338 0.342633 0.539074 0.026 Uiso calc 1 . . F F1 0.52458(12) 0.29497(9) 1.2121(3) 0.0232(9) Uani d 1 . . N N1 0.53052(17) 0.35965(12) 0.9354(4) 0.0163(12) Uani d 1 . . N N3 0.46126(16) 0.29968(12) 1.0577(4) 0.0206(12) Uani d 1 . . N N4 0.44722(16) 0.34809(12) 0.4618(4) 0.0177(12) Uani d 1 . . O O1 0.53120(14) 0.32821(10) 0.9290(3) 0.0178(10) Uani d 1 . . O O2 0.51946(13) 0.35002(10) 1.1099(3) 0.0197(10) Uani d 1 . . O O3 0.54669(15) 0.41781(11) 0.8852(3) 0.0237(11) Uani d 1 . . O O4 0.47337(15) 0.39745(11) 0.7996(4) 0.0309(12) Uani d 1 . . O O5 0.44128(14) 0.37496(11) 0.6630(3) 0.0249(11) Uani d 1 . . O O6 0.54797(16) 0.40823(11) 0.6633(4) 0.0283(12) Uani d 1 . . O O7 0.51501(15) 0.38471(11) 0.5322(4) 0.0271(11) Uani d 1 . . O O8 0.55440(14) 0.29309(10) 0.6355(3) 0.0222(11) Uani d 1 . . O O9 0.52547(14) 0.32326(11) 0.5146(3) 0.0238(11) Uani d 1 . . O O10 0.48483(13) 0.29115(10) 0.7812(3) 0.0220(10) Uani d 1 . . O O11 0.45184(14) 0.31306(11) 0.6447(3) 0.0232(11) Uani d 1 . . O O12 0.59983(14) 0.37435(10) 0.7909(4) 0.0228(11) Uani d 1 . . O O13 0.60280(13) 0.32449(10) 0.7846(3) 0.0210(10) Uani d 1 . . O O14 0.53657(14) 0.26776(10) 1.0068(3) 0.0206(10) Uani d 1 . . O O15 0.56241(13) 0.27338(10) 0.8435(3) 0.0204(10) Uani d 1 . . O O16 0.52158(13) 0.34820(10) 0.7222(3) 0.0181(10) Uani d 1 . . N N5 0.2858(10) 0.2671(6) -0.144(2) 0.155(12) Uani d 0.5 A -1 C C35 0.2940(10) 0.2379(6) -0.163(2) 0.127(11) Uani d 0.5 A -1 H H35 0.311010 0.232929 -0.222080 0.152 Uiso calc 0.5 A -1 C C36 0.2797(7) 0.2153(5) -0.1015(17) 0.073(6) Uani d 0.5 A -1 H H36 0.283212 0.195132 -0.123399 0.088 Uiso calc 0.5 A -1 C C37 0.2596(7) 0.2218(4) -0.0060(17) 0.063(6) Uani d 0.5 A -1 H H37 0.254457 0.206792 0.045608 0.076 Uiso calc 0.5 A -1 C C38 0.2473(17) 0.2515(7) 0.0109(14) 0.074(6) Uani d 0.5 A -1 H H38 0.227845 0.256511 0.065403 0.089 Uiso calc 0.5 A -1 C C39 0.2643(10) 0.2733(5) -0.054(2) 0.095(9) Uani d 0.5 A -1 H H39 0.260803 0.293654 -0.034580 0.114 Uiso calc 0.5 A -1 O O17 0.0851(9) 0.0248(6) 0.027(3) 0.069(12) Uani d 0.236(17) . . H H17D 0.071299 0.026512 -0.031577 0.103 Uiso d 0.236(17) . . H H17E 0.105232 0.036950 0.018911 0.103 Uiso d 0.236(17) . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe4 0.0181(5) 0.0248(5) 0.0081(4) -0.0004(4) -0.0020(4) 0.0010(4) Fe3 0.0163(5) 0.0266(5) 0.0087(4) -0.0001(4) -0.0025(4) 0.0009(4) Fe1 0.0181(5) 0.0274(5) 0.0077(4) 0.0007(4) 0.0004(4) 0.0009(4) Fe2 0.0219(5) 0.0256(5) 0.0093(5) -0.0017(4) -0.0032(4) 0.0008(4) C1 0.006(3) 0.032(4) 0.015(3) 0.000(3) -0.001(3) -0.002(3) C2 0.009(3) 0.028(4) 0.017(4) 0.005(3) -0.002(2) -0.002(3) C3 0.015(4) 0.032(4) 0.013(3) 0.001(3) 0.002(3) 0.002(3) C4 0.020(4) 0.036(4) 0.020(4) 0.001(3) 0.000(3) -0.009(3) C5 0.035(4) 0.030(4) 0.025(4) 0.002(3) 0.001(3) -0.009(3) C6 0.033(4) 0.025(4) 0.021(4) -0.001(3) 0.001(3) 0.001(3) C7 0.016(3) 0.033(4) 0.012(3) 0.002(3) -0.003(3) 0.001(3) C8 0.031(4) 0.043(5) 0.011(3) 0.006(3) -0.001(3) 0.004(3) C9 0.036(5) 0.098(8) 0.025(5) 0.029(5) -0.008(4) -0.013(5) C10 0.031(4) 0.036(4) 0.017(4) -0.009(3) -0.014(3) 0.008(3) C11 0.060(6) 0.080(7) 0.026(4) -0.038(5) -0.010(4) 0.023(5) C12 0.019(3) 0.030(4) 0.010(3) -0.002(3) 0.003(3) -0.004(3) C13 0.034(4) 0.035(4) 0.006(3) 0.008(3) 0.006(3) 0.001(3) C14 0.019(3) 0.027(4) 0.012(3) 0.001(3) 0.002(3) -0.005(3) C15 0.021(4) 0.034(4) 0.020(4) -0.004(3) -0.002(3) 0.003(3) C16 0.023(3) 0.036(4) 0.005(3) -0.003(3) -0.002(3) -0.001(3) C17 0.019(3) 0.046(5) 0.021(4) -0.002(3) -0.001(3) -0.002(3) C18 0.018(4) 0.037(4) 0.008(3) -0.004(3) 0.002(3) 0.000(3) C19 0.052(5) 0.026(4) 0.013(4) -0.006(4) 0.010(3) 0.001(3) N2 0.019(3) 0.030(3) 0.009(3) -0.003(2) -0.001(2) 0.001(2) C20 0.025(4) 0.050(5) 0.007(3) -0.002(3) -0.003(3) -0.004(3) C21 0.023(4) 0.077(6) 0.018(4) -0.002(4) 0.005(3) -0.007(4) C22 0.017(4) 0.062(6) 0.029(4) -0.009(4) -0.007(3) 0.003(4) C23 0.029(4) 0.039(5) 0.021(4) -0.006(3) -0.008(3) 0.003(3) C24 0.028(4) 0.034(4) 0.015(4) -0.001(3) -0.003(3) -0.001(3) C25 0.024(4) 0.032(4) 0.018(4) 0.002(3) -0.001(3) -0.005(3) C26 0.025(4) 0.040(5) 0.019(4) 0.013(3) -0.004(3) -0.008(3) C27 0.024(4) 0.043(5) 0.028(4) -0.003(3) -0.001(3) -0.016(4) C28 0.025(4) 0.040(5) 0.027(4) -0.005(3) 0.006(3) -0.007(4) C29 0.031(4) 0.033(4) 0.014(3) -0.001(3) 0.004(3) -0.004(3) C30 0.014(3) 0.025(4) 0.017(3) 0.000(3) -0.002(3) 0.006(3) C31 0.023(3) 0.028(4) 0.012(3) 0.001(3) -0.001(3) -0.002(3) C32 0.024(4) 0.034(4) 0.015(3) 0.003(3) -0.005(3) -0.002(3) C33 0.017(4) 0.042(5) 0.012(3) 0.000(3) 0.000(3) 0.001(3) C34 0.019(3) 0.036(4) 0.010(3) -0.001(3) 0.004(3) -0.001(3) F1 0.024(2) 0.038(2) 0.0072(18) 0.0010(17) 0.0008(15) 0.0027(17) N1 0.016(3) 0.021(3) 0.012(3) 0.000(2) -0.002(2) 0.000(2) N3 0.023(3) 0.025(3) 0.014(3) -0.001(2) 0.001(2) -0.004(2) N4 0.015(3) 0.028(3) 0.010(3) 0.003(2) -0.001(2) 0.004(2) O1 0.020(2) 0.021(3) 0.012(2) -0.001(2) -0.0031(17) -0.004(2) O2 0.019(2) 0.031(3) 0.009(2) -0.001(2) 0.0002(18) 0.001(2) O3 0.033(3) 0.026(3) 0.012(2) -0.004(2) -0.001(2) 0.001(2) O4 0.029(3) 0.039(3) 0.025(3) 0.006(2) -0.010(2) -0.008(2) O5 0.024(3) 0.043(3) 0.008(2) 0.010(2) -0.0059(19) -0.004(2) O6 0.035(3) 0.032(3) 0.018(3) -0.009(2) -0.004(2) 0.005(2) O7 0.031(3) 0.035(3) 0.015(2) -0.008(2) -0.009(2) 0.004(2) O8 0.028(3) 0.029(3) 0.010(2) 0.002(2) -0.001(2) 0.001(2) O9 0.022(2) 0.037(3) 0.012(2) 0.009(2) -0.0026(19) 0.004(2) O10 0.023(2) 0.030(3) 0.014(2) -0.004(2) -0.003(2) 0.004(2) O11 0.027(3) 0.031(3) 0.012(2) -0.002(2) -0.006(2) 0.005(2) O12 0.026(3) 0.026(3) 0.016(2) -0.001(2) 0.000(2) 0.000(2) O13 0.022(2) 0.028(3) 0.014(2) -0.003(2) 0.0019(19) 0.000(2) O14 0.024(2) 0.028(3) 0.010(2) 0.004(2) 0.0004(18) -0.0002(19) O15 0.019(2) 0.029(3) 0.012(2) -0.001(2) -0.0008(19) 0.001(2) O16 0.015(2) 0.030(3) 0.009(2) -0.002(2) 0.0010(18) -0.001(2) N5 0.184(16) 0.140(16) 0.141(16) -0.005(12) 0.035(13) -0.009(12) C35 0.158(16) 0.101(15) 0.121(16) -0.005(12) 0.011(13) -0.011(12) C36 0.089(12) 0.067(11) 0.064(11) -0.019(10) 0.023(10) -0.008(9) C37 0.066(11) 0.042(10) 0.080(12) -0.014(9) 0.002(10) -0.005(9) C38 0.077(12) 0.067(10) 0.077(10) -0.012(9) 0.003(14) 0.005(14) C39 0.112(15) 0.073(13) 0.099(14) -0.026(11) 0.017(12) 0.000(11) O17 0.063(18) 0.047(17) 0.09(2) -0.016(13) 0.008(15) -0.009(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O16 Fe4 O15 . . 178.35(19) y O16 Fe4 O13 . . 95.35(18) y O15 Fe4 O13 . . 84.96(18) y O16 Fe4 O10 . . 95.84(18) y O15 Fe4 O10 . . 83.89(18) y O13 Fe4 O10 . . 168.72(19) y O16 Fe4 O8 . . 94.97(18) y O15 Fe4 O8 . . 86.66(18) y O13 Fe4 O8 . . 87.52(18) y O10 Fe4 O8 . . 90.07(18) y O16 Fe4 O1 . . 89.18(18) y O15 Fe4 O1 . . 89.19(18) y O13 Fe4 O1 . . 91.19(18) y O10 Fe4 O1 . . 90.42(18) y O8 Fe4 O1 . . 175.74(18) y O16 Fe3 O9 . . 94.78(18) y O16 Fe3 O5 . . 96.68(18) y O9 Fe3 O5 . . 168.52(18) y O16 Fe3 O11 . . 95.43(18) y O9 Fe3 O11 . . 91.8(2) y O5 Fe3 O11 . . 87.8(2) y O16 Fe3 O7 . . 96.08(19) y O9 Fe3 O7 . . 87.2(2) y O5 Fe3 O7 . . 90.9(2) y O11 Fe3 O7 . . 168.49(18) y O16 Fe3 N4 . . 178.5(2) y O9 Fe3 N4 . . 84.23(19) y O5 Fe3 N4 . . 84.33(18) y O11 Fe3 N4 . . 83.47(19) y O7 Fe3 N4 . . 85.02(19) y F1 Fe1 O2 . . 93.63(18) y F1 Fe1 O14 . . 97.73(18) y O2 Fe1 O14 . . 168.62(18) y F1 Fe1 O1 . . 170.62(18) y O2 Fe1 O1 . . 77.18(18) y O14 Fe1 O1 . . 91.44(17) y F1 Fe1 N3 . . 89.35(19) y O2 Fe1 N3 . . 93.10(19) y O14 Fe1 N3 . . 87.6(2) y O1 Fe1 N3 . . 93.0(2) y F1 Fe1 N2 . . 87.15(18) y O2 Fe1 N2 . . 88.72(19) y O14 Fe1 N2 . . 91.2(2) y O1 Fe1 N2 . . 90.74(19) y N3 Fe1 N2 . . 176.2(2) y O3 Fe2 O16 . . 171.98(19) y O3 Fe2 O6 . . 92.3(2) y O16 Fe2 O6 . . 95.12(19) y O3 Fe2 O12 . . 91.36(19) y O16 Fe2 O12 . . 92.38(18) y O6 Fe2 O12 . . 85.01(19) y O3 Fe2 N1 . . 86.4(2) y O16 Fe2 N1 . . 86.6(2) y O6 Fe2 N1 . . 174.8(2) y O12 Fe2 N1 . . 90.0(2) y O3 Fe2 O4 . . 85.9(2) y O16 Fe2 O4 . . 90.72(19) y O6 Fe2 O4 . . 92.3(2) y O12 Fe2 O4 . . 176.1(2) y N1 Fe2 O4 . . 92.6(2) y O2 C1 N1 . . 120.3(6) ? O2 C1 C2 . . 119.7(6) ? N1 C1 C2 . . 120.0(6) ? C7 C2 C3 . . 118.3(6) ? C7 C2 C1 . . 124.5(6) ? C3 C2 C1 . . 116.9(6) ? C4 C3 C2 . . 122.0(6) ? C4 C3 H3 . . 119.0 ? C2 C3 H3 . . 119.0 ? C3 C4 C5 . . 119.5(6) ? C3 C4 H4 . . 120.2 ? C5 C4 H4 . . 120.2 ? C6 C5 C4 . . 120.2(7) ? C6 C5 H5 . . 119.9 ? C4 C5 H5 . . 119.9 ? C5 C6 C7 . . 121.2(7) ? C5 C6 H6 . . 119.4 ? C7 C6 H6 . . 119.4 ? O3 C7 C6 . . 118.0(6) ? O3 C7 C2 . . 123.1(6) ? C6 C7 C2 . . 118.8(6) ? O4 C8 O5 . . 124.8(7) ? O4 C8 C9 . . 119.4(7) ? O5 C8 C9 . . 115.9(7) ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? O7 C10 O6 . . 124.9(7) ? O7 C10 C11 . . 117.7(6) ? O6 C10 C11 . . 117.3(6) ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? O9 C12 O8 . . 125.4(6) ? O9 C12 C13 . . 117.8(6) ? O8 C12 C13 . . 116.8(6) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? O10 C14 O11 . . 125.0(6) ? O10 C14 C15 . . 117.2(6) ? O11 C14 C15 . . 117.7(6) ? C14 C15 H15A . . 109.5 ? C14 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C14 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? O12 C16 O13 . . 125.2(6) ? O12 C16 C17 . . 118.1(6) ? O13 C16 C17 . . 116.7(6) ? C16 C17 H17A . . 109.5 ? C16 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C16 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? O15 C18 O14 . . 122.8(6) ? O15 C18 C19 . . 119.2(6) ? O14 C18 C19 . . 118.0(6) ? C18 C19 H19A . . 109.5 ? C18 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C18 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? C20 N2 C24 . . 116.7(6) ? C20 N2 Fe1 . . 125.0(4) ? C24 N2 Fe1 . . 118.3(5) ? N2 C20 C21 . . 123.2(6) ? N2 C20 H20 . . 118.4 ? C21 C20 H20 . . 118.4 ? C20 C21 C22 . . 119.7(7) ? C20 C21 H21 . . 120.1 ? C22 C21 H21 . . 120.1 ? C21 C22 C23 . . 118.3(7) ? C21 C22 H22 . . 120.9 ? C23 C22 H22 . . 120.9 ? C24 C23 C22 . . 118.5(7) ? C24 C23 H23 . . 120.8 ? C22 C23 H23 . . 120.8 ? N2 C24 C23 . . 123.6(7) ? N2 C24 H24 . . 118.2 ? C23 C24 H24 . . 118.2 ? N3 C25 C26 . . 122.2(7) ? N3 C25 H25 . . 118.9 ? C26 C25 H25 . . 118.9 ? C25 C26 C27 . . 119.8(7) ? C25 C26 H26 . . 120.1 ? C27 C26 H26 . . 120.1 ? C28 C27 C26 . . 118.3(7) ? C28 C27 H27 . . 120.8 ? C26 C27 H27 . . 120.8 ? C27 C28 C29 . . 119.5(7) ? C27 C28 H28 . . 120.2 ? C29 C28 H28 . . 120.2 ? N3 C29 C28 . . 122.3(7) ? N3 C29 H29 . . 118.9 ? C28 C29 H29 . . 118.9 ? N4 C30 C31 . . 122.1(6) ? N4 C30 H30 . . 118.9 ? C31 C30 H30 . . 118.9 ? C32 C31 C30 . . 119.4(6) ? C32 C31 H31 . . 120.3 ? C30 C31 H31 . . 120.3 ? C31 C32 C33 . . 119.1(6) ? C31 C32 H32 . . 120.5 ? C33 C32 H32 . . 120.5 ? C34 C33 C32 . . 118.7(6) ? C34 C33 H33 . . 120.6 ? C32 C33 H33 . . 120.6 ? N4 C34 C33 . . 123.3(6) ? N4 C34 H34 . . 118.4 ? C33 C34 H34 . . 118.4 ? C1 N1 O1 . . 111.7(5) ? C1 N1 Fe2 . . 129.6(4) ? O1 N1 Fe2 . . 118.7(3) ? C29 N3 C25 . . 117.9(6) ? C29 N3 Fe1 . . 119.5(5) ? C25 N3 Fe1 . . 122.4(5) ? C34 N4 C30 . . 117.4(5) ? C34 N4 Fe3 . . 120.9(4) ? C30 N4 Fe3 . . 121.7(4) ? N1 O1 Fe1 . . 113.7(3) ? N1 O1 Fe4 . . 114.3(3) ? Fe1 O1 Fe4 . . 131.7(2) ? C1 O2 Fe1 . . 116.5(4) ? C7 O3 Fe2 . . 132.4(4) ? C8 O4 Fe2 . . 134.9(5) ? C8 O5 Fe3 . . 130.5(4) ? C10 O6 Fe2 . . 132.7(5) ? C10 O7 Fe3 . . 131.9(4) ? C12 O8 Fe4 . . 132.9(4) ? C12 O9 Fe3 . . 129.9(4) ? C14 O10 Fe4 . . 129.0(4) ? C14 O11 Fe3 . . 134.5(4) ? C16 O12 Fe2 . . 132.4(4) ? C16 O13 Fe4 . . 131.3(4) ? C18 O14 Fe1 . . 138.3(5) ? C18 O15 Fe4 . . 133.9(4) ? Fe3 O16 Fe4 . . 120.9(2) ? Fe3 O16 Fe2 . . 121.7(2) ? Fe4 O16 Fe2 . . 117.4(2) ? C35 N5 C39 . . 116(2) ? C36 C35 N5 . . 124(2) ? C36 C35 H35 . . 117.9 ? N5 C35 H35 . . 117.9 ? C35 C36 C37 . . 119(2) ? C35 C36 H36 . . 120.4 ? C37 C36 H36 . . 120.4 ? C36 C37 C38 . . 117.3(19) ? C36 C37 H37 . . 121.4 ? C38 C37 H37 . . 121.4 ? C39 C38 C37 . . 118(3) ? C39 C38 H38 . . 120.9 ? C37 C38 H38 . . 120.9 ? N5 C39 C38 . . 123(2) ? N5 C39 H39 . . 118.5 ? C38 C39 H39 . . 118.5 ? H17D O17 H17E . . 103.3 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe4 O16 . 1.890(5) y Fe4 O15 . 2.016(5) y Fe4 O13 . 2.021(4) y Fe4 O10 . 2.023(4) y Fe4 O8 . 2.034(4) y Fe4 O1 . 2.056(4) y Fe3 O16 . 1.872(4) y Fe3 O9 . 1.997(5) y Fe3 O5 . 2.020(5) y Fe3 O11 . 2.024(5) y Fe3 O7 . 2.037(5) y Fe3 N4 . 2.170(5) y Fe1 F1 . 1.843(4) y Fe1 O2 . 1.978(5) y Fe1 O14 . 1.987(4) y Fe1 O1 . 2.043(5) y Fe1 N3 . 2.133(5) y Fe1 N2 . 2.171(5) y Fe2 O3 . 1.902(5) y Fe2 O16 . 1.925(4) y Fe2 O6 . 2.021(5) y Fe2 O12 . 2.057(5) y Fe2 N1 . 2.083(5) y Fe2 O4 . 2.084(5) y C1 O2 . 1.287(8) ? C1 N1 . 1.329(8) ? C1 C2 . 1.461(9) ? C2 C7 . 1.412(9) ? C2 C3 . 1.412(9) ? C3 C4 . 1.369(10) ? C3 H3 . 0.9500 ? C4 C5 . 1.389(10) ? C4 H4 . 0.9500 ? C5 C6 . 1.382(10) ? C5 H5 . 0.9500 ? C6 C7 . 1.403(10) ? C6 H6 . 0.9500 ? C7 O3 . 1.325(8) ? C8 O4 . 1.252(8) ? C8 O5 . 1.274(9) ? C8 C9 . 1.501(11) ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? C10 O7 . 1.243(8) ? C10 O6 . 1.262(8) ? C10 C11 . 1.499(10) ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 O9 . 1.253(8) ? C12 O8 . 1.261(8) ? C12 C13 . 1.504(9) ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C13 H13C . 0.9800 ? C14 O10 . 1.259(8) ? C14 O11 . 1.267(8) ? C14 C15 . 1.502(9) ? C15 H15A . 0.9800 ? C15 H15B . 0.9800 ? C15 H15C . 0.9800 ? C16 O12 . 1.258(8) ? C16 O13 . 1.262(8) ? C16 C17 . 1.505(9) ? C17 H17A . 0.9800 ? C17 H17B . 0.9800 ? C17 H17C . 0.9800 ? C18 O15 . 1.263(8) ? C18 O14 . 1.276(8) ? C18 C19 . 1.469(10) ? C19 H19A . 0.9800 ? C19 H19B . 0.9800 ? C19 H19C . 0.9800 ? N2 C20 . 1.343(8) ? N2 C24 . 1.345(8) ? C20 C21 . 1.357(9) ? C20 H20 . 0.9500 ? C21 C22 . 1.379(10) ? C21 H21 . 0.9500 ? C22 C23 . 1.384(10) ? C22 H22 . 0.9500 ? C23 C24 . 1.372(10) ? C23 H23 . 0.9500 ? C24 H24 . 0.9500 ? C25 N3 . 1.352(9) ? C25 C26 . 1.374(9) ? C25 H25 . 0.9500 ? C26 C27 . 1.385(11) ? C26 H26 . 0.9500 ? C27 C28 . 1.372(11) ? C27 H27 . 0.9500 ? C28 C29 . 1.389(10) ? C28 H28 . 0.9500 ? C29 N3 . 1.343(9) ? C29 H29 . 0.9500 ? C30 N4 . 1.357(8) ? C30 C31 . 1.386(9) ? C30 H30 . 0.9500 ? C31 C32 . 1.367(9) ? C31 H31 . 0.9500 ? C32 C33 . 1.388(9) ? C32 H32 . 0.9500 ? C33 C34 . 1.373(9) ? C33 H33 . 0.9500 ? C34 N4 . 1.344(8) ? C34 H34 . 0.9500 ? N1 O1 . 1.411(6) ? N5 C35 . 1.35(2) ? N5 C39 . 1.35(2) ? C35 C36 . 1.35(2) ? C35 H35 . 0.9500 ? C36 C37 . 1.39(2) ? C36 H36 . 0.9500 ? C37 C38 . 1.40(3) ? C37 H37 . 0.9500 ? C38 C39 . 1.39(3) ? C38 H38 . 0.9500 ? C39 H39 . 0.9500 ? O17 H17D . 0.8564 ? O17 H17E . 0.8446 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C11 H11A N5 7 0.98 2.37 3.23(3) 146.4 yes C13 H13A F1 1_554 0.98 2.54 3.389(7) 145.2 yes C15 H15B F1 6_654 0.98 2.49 3.454(8) 167.9 yes C17 H17A O17 12 0.98 2.60 3.42(3) 141.8 yes C19 H19B F1 6_654 0.98 2.60 3.520(9) 156.4 yes C19 H19C O11 6_655 0.98 2.47 3.446(8) 171.5 yes C20 H20 O13 . 0.95 2.64 3.269(8) 124.2 yes C20 H20 O15 . 0.95 2.49 3.365(8) 152.5 yes C23 H23 O5 7 0.95 2.55 3.473(9) 163.8 yes C25 H25 O1 . 0.95 2.60 3.149(8) 117.2 yes C26 H26 O6 15_455 0.95 2.64 3.431(8) 140.7 yes C29 H29 F1 . 0.95 2.46 2.930(8) 110.2 yes C31 H31 O2 1_554 0.95 2.48 3.282(8) 142.8 yes C39 H39 O6 15_454 0.95 2.54 3.27(2) 133.7 yes O17 H17E O13 16_544 0.84 2.15 2.97(3) 163.8 yes