#------------------------------------------------------------------------------ #$Date: 2024-07-09 05:02:26 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293324 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312540.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_2312540 loop_ _publ_author_name 'Klein-Hessling, Christian' 'Blockhaus, Tobias' 'Sünkel, Karlheinz' _publ_section_title ; Synthesis, spectroscopic and crystallographic characterization of various cymantrenyl thioethers [Mn{C5HxBry(SMe)z}(PPh3)(CO)2]. ; _journal_coeditor_code QF3063 _journal_issue 8 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S205322962400603X _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[Mn (C6 H6 S Br) (C18 H15 P) (C O)2], 0.75C6 H12' _chemical_formula_moiety '2(C26 H21 Br Mn O2 P S), 0.75(C6 H12)' _chemical_formula_sum 'C56.5 H51 Br2 Mn2 O4 P2 S2' _chemical_formula_weight 1189.73 _chemical_name_systematic 'Dicarbonyl[\h^5^-1-bromo-2-(methylsulfanyl)cyclopentadienyl](triphenylphosphane-\kP)manganese cyclohexane 0.75-solvate' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 87.692(2) _cell_angle_beta 82.138(2) _cell_angle_gamma 62.507(2) _cell_formula_units_Z 1 _cell_length_a 10.3309(5) _cell_length_b 10.7727(5) _cell_length_c 13.0821(6) _cell_measurement_reflns_used 9912 _cell_measurement_temperature 108 _cell_measurement_theta_max 28.2881 _cell_measurement_theta_min 2.5614 _cell_volume 1278.93(11) _computing_cell_refinement ; APEX2 (Bruker, 2011) ; _computing_data_collection ; APEX2 (Bruker, 2011) ; _computing_data_reduction ; SAINT (Bruker, 2011) ; _computing_publication_material ; Mercury (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 108(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method 'mix of omega and phi scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 21220 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.309 _diffrn_reflns_theta_min 2.900 _diffrn_source 'rotating anode generator' _exptl_absorpt_coefficient_mu 2.247 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS2016; Krause et al., 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 604 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _refine_diff_density_max 5.858 _refine_diff_density_min -1.710 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 328 _refine_ls_number_reflns 6351 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0662 _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^)+(0.0645P)^2^+9.2055P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1635 _refine_ls_wR_factor_ref 0.1701 _reflns_number_gt 5421 _reflns_number_total 6351 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qf3063.cif _cod_data_source_block comp_2 _cod_original_formula_sum 'C56.50 H51 Br2 Mn2 O4 P2 S2' _cod_database_code 2312540 _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 0.896 _shelx_estimated_absorpt_t_max 0.956 _shelx_hkl_file ; -1 0 0 0.27 0.46 -1 0 0 0.04 0.40 1 0 0 -0.27 0.34 -2 0 0 2394.60 64.94 -3 0 0 1036.38 29.66 -3 0 0 1016.70 28.61 -3 0 0 1086.75 29.97 3 0 0 1056.68 29.55 3 0 0 1003.26 28.61 3 0 0 1021.02 29.90 -4 0 0 408.00 14.11 -4 0 0 445.92 14.12 4 0 0 435.59 14.55 4 0 0 400.33 13.68 4 0 0 411.74 12.62 -5 0 0 34.86 4.37 -5 0 0 30.61 2.77 -5 0 0 33.22 4.82 5 0 0 21.71 3.55 5 0 0 33.02 3.36 5 0 0 27.22 3.97 -6 0 0 620.80 21.43 -6 0 0 608.56 21.16 6 0 0 660.98 19.16 6 0 0 680.67 22.34 6 0 0 609.80 20.82 6 0 0 650.13 19.17 -7 0 0 239.16 16.57 7 0 0 289.79 9.92 7 0 0 283.82 13.13 7 0 0 282.19 9.92 -8 0 0 -2.95 4.15 8 0 0 6.12 5.25 8 0 0 4.49 2.33 8 0 0 5.60 2.65 -9 0 0 9.42 5.78 9 0 0 12.64 2.87 9 0 0 9.69 2.82 9 0 0 6.85 6.27 -10 0 0 338.10 17.31 10 0 0 340.84 18.69 10 0 0 342.72 11.79 10 0 0 337.16 11.79 -11 0 0 245.24 15.84 11 0 0 240.27 8.92 11 0 0 246.58 16.46 -12 0 0 0.24 6.41 12 0 0 1.13 8.31 11 -1 0 110.22 6.03 11 -1 0 93.71 12.41 -11 1 0 109.13 11.72 10 -1 0 28.84 4.18 10 -1 0 29.98 3.91 -10 1 0 34.59 7.55 9 -1 0 75.40 5.47 9 -1 0 81.96 10.25 9 -1 0 73.88 5.42 -9 1 0 89.64 9.50 8 -1 0 242.63 9.57 8 -1 0 250.72 14.22 8 -1 0 231.37 9.37 -8 1 0 230.52 12.49 7 -1 0 4.39 2.56 7 -1 0 2.94 4.76 7 -1 0 7.58 2.65 6 -1 0 97.13 6.30 6 -1 0 117.03 7.94 6 -1 0 111.09 5.44 6 -1 0 122.67 5.92 -6 1 0 114.55 7.52 5 -1 0 70.11 5.20 5 -1 0 71.42 5.92 5 -1 0 75.84 4.49 5 -1 0 74.22 4.19 -5 1 0 78.81 5.74 -5 1 0 71.46 5.48 4 -1 0 28.09 3.96 4 -1 0 31.57 2.99 4 -1 0 24.62 3.17 4 -1 0 27.59 2.74 -4 1 0 35.45 3.70 -4 1 0 39.42 4.36 3 -1 0 369.87 11.30 3 -1 0 364.62 12.55 3 -1 0 367.48 11.77 3 -1 0 369.01 11.36 -3 1 0 347.84 11.73 -3 1 0 374.63 12.52 2 -1 0 2240.47 59.72 2 -1 0 2118.90 59.79 2 -1 0 2151.16 58.99 2 -1 0 2130.13 59.04 -2 1 0 2137.59 59.74 -2 1 0 2281.58 59.29 1 -1 0 107.93 3.55 1 -1 0 103.88 3.69 1 -1 0 107.16 4.15 -1 1 0 101.18 3.72 -1 1 0 102.89 4.11 -1 1 0 96.29 3.52 -1 -1 0 0.22 0.29 1 1 0 -0.05 0.34 -2 -1 0 8.49 1.48 -2 -1 0 4.65 1.44 -2 -1 0 5.83 0.99 2 1 0 6.85 1.05 2 1 0 7.14 1.59 2 1 0 7.91 1.51 -3 -1 0 41.40 2.24 -3 -1 0 47.43 3.43 -3 -1 0 43.51 3.17 3 1 0 42.63 3.17 3 1 0 40.56 2.27 3 1 0 44.37 3.03 -4 -1 0 397.24 13.64 -4 -1 0 404.56 13.77 -4 -1 0 427.87 12.29 4 1 0 410.49 12.25 4 1 0 410.24 13.92 4 1 0 412.49 13.49 -5 -1 0 851.35 25.01 -5 -1 0 761.96 24.73 -5 -1 0 814.19 22.96 5 1 0 791.60 24.54 5 1 0 791.77 22.90 5 1 0 804.56 25.12 -6 -1 0 30.36 2.88 -6 -1 0 34.39 4.64 -6 -1 0 23.35 3.86 6 1 0 29.49 2.85 6 1 0 34.02 4.55 6 1 0 30.12 4.73 -7 -1 0 455.40 14.39 -7 -1 0 475.68 17.66 7 1 0 451.83 14.34 7 1 0 449.48 19.18 -8 -1 0 1.44 4.10 8 1 0 -2.16 3.98 8 1 0 0.81 2.22 -9 -1 0 38.48 7.20 9 1 0 33.61 3.61 9 1 0 34.37 7.17 9 1 0 31.32 3.45 -10 -1 0 9.63 5.84 10 1 0 4.22 2.52 10 1 0 0.98 2.58 10 1 0 6.63 6.62 11 1 0 3.61 2.50 11 1 0 5.06 7.51 11 1 0 1.80 2.36 -12 -1 0 34.43 9.09 12 1 0 49.72 11.18 11 -2 0 6.28 8.48 -11 2 0 -3.08 6.59 10 -2 0 82.88 11.29 10 -2 0 75.33 6.14 -10 2 0 82.74 9.70 9 -2 0 226.02 15.59 9 -2 0 202.56 12.32 9 -2 0 201.09 9.60 -9 2 0 217.05 13.08 8 -2 0 552.13 18.15 8 -2 0 554.39 22.56 8 -2 0 531.22 17.89 -8 2 0 529.49 20.64 7 -2 0 85.19 8.66 7 -2 0 74.59 5.25 7 -2 0 70.07 5.81 -7 2 0 81.32 7.74 6 -2 0 271.35 10.39 6 -2 0 276.73 10.15 6 -2 0 246.72 10.95 6 -2 0 248.67 12.46 -6 2 0 272.23 11.76 5 -2 0 150.14 6.93 5 -2 0 147.13 6.62 5 -2 0 131.86 7.02 5 -2 0 161.06 8.69 -5 2 0 139.62 8.48 -5 2 0 145.32 7.53 4 -2 0 340.94 12.09 4 -2 0 364.50 11.81 4 -2 0 328.28 13.37 4 -2 0 361.46 12.04 -4 2 0 360.73 14.11 -4 2 0 347.14 12.24 3 -2 0 690.50 20.31 3 -2 0 698.29 20.26 3 -2 0 673.87 20.40 3 -2 0 712.58 21.63 -3 2 0 676.95 20.35 -3 2 0 643.90 21.18 2 -2 0 1463.75 40.45 2 -2 0 1396.67 39.51 2 -2 0 1376.55 39.11 -2 2 0 1430.03 39.61 -2 2 0 1373.75 40.21 -2 2 0 1477.67 39.22 1 -2 0 1487.56 40.71 1 -2 0 1508.90 41.16 1 -2 0 1423.74 39.80 -1 2 0 1361.42 40.94 -1 2 0 1532.17 40.83 -1 2 0 1521.21 39.86 0 -2 0 1453.04 39.94 0 2 0 1439.83 39.80 -1 -2 0 3776.98 116.63 1 2 0 3747.55 116.26 -2 -2 0 8935.66 251.99 2 2 0 8361.63 250.15 -3 -2 0 402.71 12.03 -3 -2 0 380.32 12.36 -3 -2 0 391.76 12.25 3 2 0 383.17 12.07 3 2 0 365.72 11.53 3 2 0 375.01 12.28 -4 -2 0 779.77 22.30 -4 -2 0 791.64 23.60 -4 -2 0 756.24 23.53 4 2 0 809.42 23.72 4 2 0 813.23 23.46 4 2 0 754.67 22.34 -5 -2 0 956.47 26.65 -5 -2 0 782.41 24.35 -5 -2 0 896.55 26.52 5 2 0 843.33 26.00 5 2 0 825.31 26.33 -6 -2 0 595.05 19.81 -6 -2 0 584.86 17.38 -6 -2 0 576.03 19.63 6 2 0 595.59 20.04 6 2 0 575.34 17.41 6 2 0 558.22 19.16 -7 -2 0 2089.33 62.43 -7 -2 0 2164.76 59.64 7 2 0 2227.93 59.69 7 2 0 2165.35 62.84 -8 -2 0 501.56 15.65 -8 -2 0 503.40 19.30 8 2 0 487.68 19.25 8 2 0 493.76 15.66 -9 -2 0 6.90 2.53 -9 -2 0 2.06 4.83 9 2 0 7.40 2.64 9 2 0 3.20 4.74 -10 -2 0 250.81 14.64 10 2 0 239.79 14.36 10 2 0 228.19 8.84 10 2 0 221.85 8.68 -11 -2 0 3.43 6.33 11 2 0 4.64 2.44 11 2 0 4.79 8.08 11 2 0 3.68 2.48 -12 -2 0 85.59 11.47 12 2 0 73.83 11.07 10 -3 0 3.81 3.96 10 -3 0 -5.72 7.96 -10 3 0 0.92 6.09 9 -3 0 149.83 8.49 9 -3 0 123.40 13.06 9 -3 0 128.30 8.55 -9 3 0 148.06 11.41 8 -3 0 129.13 8.39 8 -3 0 144.28 12.90 8 -3 0 130.46 7.81 -8 3 0 132.86 9.88 7 -3 0 530.24 18.86 7 -3 0 579.37 19.44 7 -3 0 599.05 23.25 -7 3 0 574.19 20.78 6 -3 0 125.65 7.10 6 -3 0 143.33 7.95 6 -3 0 129.55 9.61 6 -3 0 123.80 7.44 -6 3 0 151.35 8.38 5 -3 0 165.20 7.99 5 -3 0 172.67 8.15 5 -3 0 185.84 8.06 -5 3 0 170.79 8.52 4 -3 0 7.79 3.64 4 -3 0 4.41 2.35 4 -3 0 2.29 2.24 4 -3 0 5.84 2.95 -4 3 0 6.55 2.75 -4 3 0 7.40 3.24 3 -3 0 18.05 3.99 3 -3 0 25.07 2.84 3 -3 0 28.51 3.37 3 -3 0 20.21 3.21 -3 3 0 25.54 4.06 -3 3 0 21.86 2.88 2 -3 0 671.16 20.98 2 -3 0 668.98 19.13 2 -3 0 647.54 20.14 -2 3 0 677.37 20.98 -2 3 0 662.50 19.15 -2 3 0 658.88 20.22 1 -3 0 3063.76 84.97 1 -3 0 3207.81 85.55 1 -3 0 3114.78 83.40 -1 3 0 3116.53 85.44 -1 3 0 3068.24 85.01 -1 3 0 3119.15 83.44 0 -3 0 4531.62 121.18 0 -3 0 4478.23 120.96 0 3 0 4420.49 121.15 -1 -3 0 93.63 3.17 -1 -3 0 100.00 4.58 -1 -3 0 94.39 4.69 1 3 0 97.55 4.56 1 3 0 95.11 4.49 1 3 0 91.08 3.11 -2 -3 0 93.84 4.49 -2 -3 0 94.87 4.66 -2 -3 0 97.06 3.89 -2 -3 0 96.68 4.60 2 3 0 97.38 4.46 2 3 0 90.57 3.85 -3 -3 0 374.49 11.96 -3 -3 0 388.64 11.94 -3 -3 0 372.40 12.34 3 3 0 373.36 11.94 3 3 0 365.73 11.83 3 3 0 369.98 12.36 -4 -3 0 328.43 10.72 -4 -3 0 333.86 11.47 4 3 0 334.38 11.35 4 3 0 315.02 11.57 4 3 0 329.42 10.77 -5 -3 0 2765.54 75.32 -5 -3 0 2759.21 76.87 -5 -3 0 2594.62 76.53 5 3 0 2836.67 75.44 5 3 0 2780.91 76.90 5 3 0 2809.10 76.54 -6 -3 0 1575.27 44.17 -6 -3 0 1580.70 46.35 -6 -3 0 1571.70 46.16 6 3 0 1563.70 45.87 6 3 0 1609.28 44.32 -7 -3 0 335.94 14.01 -7 -3 0 370.93 11.77 7 3 0 347.00 11.75 7 3 0 331.81 14.14 -8 -3 0 9.68 2.64 -8 -3 0 9.34 4.50 8 3 0 9.95 2.71 8 3 0 6.27 4.38 -9 -3 0 293.27 10.83 -9 -3 0 279.55 14.18 9 3 0 304.60 14.83 9 3 0 322.66 11.00 -10 -3 0 7.12 5.79 -10 -3 0 3.19 2.54 10 3 0 3.49 2.71 10 3 0 3.97 5.60 -11 -3 0 51.21 8.76 -11 -3 0 49.28 4.49 11 3 0 47.23 4.28 11 3 0 33.66 7.82 -12 -3 0 152.45 14.31 12 3 0 146.68 14.84 -13 -3 0 46.23 9.76 13 3 0 48.04 10.91 9 -4 0 84.86 12.07 -9 4 0 74.94 9.23 8 -4 0 35.39 9.44 8 -4 0 35.37 5.76 -8 4 0 37.79 6.95 7 -4 0 4.22 5.89 7 -4 0 13.20 4.55 -7 4 0 8.42 4.87 6 -4 0 654.26 24.55 6 -4 0 654.94 21.95 6 -4 0 633.19 21.53 6 -4 0 617.86 21.24 -6 4 0 679.92 22.04 5 -4 0 524.16 19.01 5 -4 0 518.16 18.36 5 -4 0 552.67 21.05 5 -4 0 552.40 18.92 -5 4 0 553.53 18.25 4 -4 0 385.31 14.11 4 -4 0 348.22 12.52 4 -4 0 361.23 16.32 -4 4 0 393.05 13.01 3 -4 0 1773.28 51.96 3 -4 0 1815.68 53.35 3 -4 0 1790.81 50.52 -3 4 0 1863.24 50.73 -3 4 0 1877.27 52.27 -3 4 0 1840.93 53.17 2 -4 0 3024.84 85.34 2 -4 0 3061.39 86.22 2 -4 0 3196.17 85.35 -2 4 0 3095.36 83.55 -2 4 0 3085.73 85.45 1 -4 0 665.17 20.90 1 -4 0 634.07 20.19 -1 4 0 632.51 17.89 -1 4 0 656.23 20.69 -1 4 0 667.52 17.95 -1 4 0 645.55 20.30 0 -4 0 32.91 3.58 0 -4 0 29.22 3.49 0 4 0 33.95 3.62 0 4 0 36.15 3.78 -1 -4 0 643.25 17.05 -1 -4 0 619.48 19.25 -1 -4 0 605.88 17.02 -1 -4 0 648.94 19.52 1 4 0 615.34 19.31 1 4 0 616.93 19.37 -2 -4 0 135.58 6.17 -2 -4 0 150.71 6.54 -2 -4 0 139.19 5.05 -2 -4 0 144.50 6.64 2 4 0 130.39 4.90 2 4 0 135.10 6.25 2 4 0 143.17 6.27 -3 -4 0 78.24 4.23 -3 -4 0 81.43 4.46 -3 -4 0 74.70 4.67 -3 -4 0 73.69 5.10 3 4 0 80.97 4.58 3 4 0 80.36 4.11 3 4 0 70.66 4.70 -4 -4 0 115.95 5.89 -4 -4 0 112.32 5.98 -4 -4 0 118.51 5.66 4 4 0 101.11 5.42 4 4 0 112.50 5.74 4 4 0 113.20 6.13 -5 -4 0 260.43 10.71 -5 -4 0 252.91 10.48 -5 -4 0 261.53 9.65 5 4 0 265.49 9.75 5 4 0 272.14 10.82 5 4 0 272.65 10.31 -6 -4 0 530.60 17.07 -6 -4 0 540.60 18.50 -6 -4 0 541.74 18.71 6 4 0 558.82 17.31 6 4 0 526.60 18.09 6 4 0 551.29 18.86 -7 -4 0 271.97 10.24 -7 -4 0 286.39 12.35 7 4 0 291.47 10.51 7 4 0 279.77 12.69 -8 -4 0 867.41 26.65 -8 -4 0 874.14 29.51 8 4 0 949.06 30.20 8 4 0 895.24 26.83 -9 -4 0 1154.19 38.38 -9 -4 0 1185.50 35.08 9 4 0 1242.12 39.14 9 4 0 1233.77 35.22 -10 -4 0 63.65 5.14 -10 -4 0 79.75 9.51 10 4 0 83.83 9.89 10 4 0 81.82 5.46 -11 -4 0 63.18 5.07 -11 -4 0 56.11 8.94 11 4 0 54.38 8.83 11 4 0 59.30 5.25 -12 -4 0 21.56 3.72 -12 -4 0 26.78 8.01 12 4 0 33.76 9.16 12 4 0 25.55 3.65 -13 -4 0 -0.18 7.34 13 4 0 9.67 8.86 9 -5 0 18.66 5.72 9 -5 0 18.52 9.13 -9 5 0 23.20 6.52 8 -5 0 38.19 6.40 8 -5 0 35.13 9.76 -8 5 0 49.79 7.34 7 -5 0 8.77 5.09 7 -5 0 14.37 7.34 -7 5 0 19.97 5.17 6 -5 0 39.04 7.64 -6 5 0 54.57 5.26 -6 5 0 48.51 5.95 5 -5 0 5.85 5.54 5 -5 0 3.92 4.16 -5 5 0 2.93 2.35 -5 5 0 8.62 3.48 4 -5 0 16.18 5.48 4 -5 0 20.57 3.89 4 -5 0 11.70 4.40 -4 5 0 14.98 3.20 -4 5 0 10.11 2.49 3 -5 0 51.80 4.80 3 -5 0 65.87 8.14 -3 5 0 52.47 3.47 -3 5 0 54.47 5.74 -3 5 0 53.37 3.86 2 -5 0 375.87 14.39 2 -5 0 356.57 13.44 -2 5 0 336.04 13.81 -2 5 0 351.94 11.24 -2 5 0 371.22 13.69 -2 5 0 371.38 10.96 1 -5 0 70.42 5.68 1 -5 0 69.28 6.04 -1 5 0 73.83 5.79 -1 5 0 62.87 5.07 0 -5 0 674.70 21.19 0 -5 0 716.98 21.59 0 5 0 584.81 20.99 0 5 0 672.97 21.18 -1 -5 0 33.19 3.91 -1 -5 0 34.93 4.46 1 5 0 30.97 3.87 1 5 0 27.08 3.81 -2 -5 0 548.79 18.13 -2 -5 0 543.67 17.90 -2 -5 0 555.94 15.87 -2 -5 0 570.01 15.87 2 5 0 545.82 18.09 2 5 0 551.68 18.03 -3 -5 0 327.75 11.91 -3 -5 0 312.89 11.58 -3 -5 0 327.50 10.27 -3 -5 0 296.13 11.20 3 5 0 296.63 11.33 3 5 0 291.93 9.98 -4 -5 0 127.90 6.80 -4 -5 0 120.34 6.84 -4 -5 0 119.86 5.84 -4 -5 0 105.63 5.80 4 5 0 113.43 6.55 4 5 0 114.46 5.54 4 5 0 109.76 6.06 -5 -5 0 19.96 3.60 -5 -5 0 19.45 3.29 -5 -5 0 19.14 3.13 5 5 0 20.19 3.03 5 5 0 35.83 4.63 5 5 0 30.94 3.80 -6 -5 0 5.52 3.04 -6 -5 0 6.11 2.79 -6 -5 0 8.81 2.56 6 5 0 7.92 2.90 6 5 0 4.43 3.08 6 5 0 9.27 2.69 -7 -5 0 396.75 13.80 -7 -5 0 372.21 15.38 7 5 0 421.30 14.11 7 5 0 381.77 15.58 -8 -5 0 15.91 3.22 -8 -5 0 10.57 4.61 8 5 0 12.42 3.31 8 5 0 11.10 4.63 -9 -5 0 21.05 3.81 -9 -5 0 25.59 5.95 9 5 0 20.72 5.73 9 5 0 28.84 4.22 -10 -5 0 61.17 5.48 -10 -5 0 62.85 8.31 10 5 0 75.84 9.39 10 5 0 77.30 5.81 -11 -5 0 15.17 7.08 -11 -5 0 19.54 3.94 11 5 0 22.32 4.07 11 5 0 21.25 7.11 -12 -5 0 120.59 7.15 -12 -5 0 138.62 13.70 12 5 0 135.09 12.95 12 5 0 149.46 7.50 -13 -5 0 247.06 16.95 13 5 0 263.80 10.02 13 5 0 274.81 18.83 8 -6 0 10.92 9.06 8 -6 0 9.34 6.01 -8 6 0 7.06 5.25 7 -6 0 8.27 5.96 7 -6 0 16.73 7.92 -7 6 0 13.08 4.96 6 -6 0 73.66 10.19 6 -6 0 71.61 8.07 -6 6 0 96.23 7.22 -6 6 0 75.86 6.12 5 -6 0 4.39 5.17 5 -6 0 6.28 6.24 -5 6 0 3.34 2.57 -5 6 0 0.01 3.00 4 -6 0 207.50 12.92 4 -6 0 221.43 11.67 -4 6 0 214.28 8.52 -4 6 0 199.21 8.11 3 -6 0 850.87 28.86 -3 6 0 856.45 27.54 -3 6 0 841.62 24.13 -3 6 0 800.85 23.85 2 -6 0 1825.71 54.30 -2 6 0 1835.41 49.27 -2 6 0 1826.20 53.25 -2 6 0 1797.28 49.20 1 -6 0 2947.00 84.96 1 -6 0 2955.69 84.32 -1 6 0 3112.85 84.63 0 -6 0 1272.66 38.80 0 -6 0 1242.42 38.33 0 6 0 1339.34 39.01 0 6 0 1284.90 38.50 -1 -6 0 1426.86 41.72 -1 -6 0 1420.57 41.86 1 6 0 1427.42 41.76 1 6 0 1368.71 41.79 -2 -6 0 699.20 23.00 -2 -6 0 688.28 22.50 -2 -6 0 741.12 19.61 -2 -6 0 739.66 19.64 2 6 0 631.68 22.45 2 6 0 688.86 22.61 -3 -6 0 2180.91 63.28 -3 -6 0 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5 5 14 62.61 10.01 6 5 14 28.18 8.17 -7 -5 -14 381.31 12.66 -7 -5 -14 377.90 19.95 7 5 14 360.04 19.91 -8 -5 -14 309.90 11.03 -9 -5 -14 7.12 8.21 9 5 14 0.88 8.05 1 -6 -14 28.23 8.12 1 -6 -14 25.76 7.39 -1 6 14 31.53 7.00 0 -6 -14 81.62 9.24 0 6 14 79.91 9.47 -1 -6 -14 26.43 6.22 -1 -6 -14 15.94 6.71 1 6 14 19.88 7.08 -2 -6 -14 25.20 7.27 -2 -6 -14 27.97 5.94 2 6 14 25.91 7.71 -3 -6 -14 1.13 4.60 -3 -6 -14 0.64 6.16 -4 -6 -14 76.51 8.02 -4 -6 -14 74.73 11.88 4 6 14 82.46 11.29 -5 -6 -14 6.10 4.16 -5 -6 -14 0.58 6.57 5 6 14 7.41 7.15 -6 -6 -14 142.78 13.26 -6 -6 -14 157.15 8.76 6 6 14 149.90 13.82 -7 -6 -14 315.65 12.33 -7 -6 -14 263.23 16.54 7 6 14 297.40 18.10 -8 -6 -14 9.37 7.15 -8 -6 -14 3.97 3.75 8 6 14 10.13 7.84 -9 -6 -14 154.69 14.13 -9 -6 -14 173.11 9.46 9 6 14 164.73 15.60 0 -7 -14 13.32 10.69 0 -7 -14 27.79 7.99 0 7 14 38.46 8.44 -1 -7 -14 3.64 5.67 -2 -7 -14 -0.19 6.59 -2 -7 -14 2.22 5.43 2 7 14 -0.91 6.40 -3 -7 -14 -4.12 6.67 -3 -7 -14 -0.37 4.88 3 7 14 2.29 6.13 -4 -7 -14 75.18 7.85 4 7 14 62.51 10.54 -5 -7 -14 1.92 4.50 -5 -7 -14 8.52 6.91 5 7 14 12.68 7.44 -6 -7 -14 91.20 8.39 -6 -7 -14 95.07 11.23 6 7 14 96.13 12.19 -7 -7 -14 0.60 7.17 7 7 14 4.30 7.70 -8 -7 -14 23.67 8.96 8 7 14 26.54 9.05 -9 -7 -14 76.14 11.58 9 7 14 89.70 13.12 -2 -8 -14 74.69 9.67 2 8 14 81.58 10.32 -3 -8 -14 115.19 11.13 3 8 14 109.59 11.99 -4 -8 -14 70.87 10.90 -4 -8 -14 68.04 8.67 4 8 14 51.10 9.64 -5 -8 -14 11.15 7.17 -5 -8 -14 12.27 5.71 5 8 14 19.67 8.47 -6 -8 -14 3.03 6.59 -6 -8 -14 2.53 4.69 6 8 14 3.97 7.46 -7 -8 -14 55.43 7.29 -7 -8 -14 73.42 10.31 7 8 14 63.26 10.64 -8 -8 -14 0.54 7.71 -8 -8 -14 5.47 4.87 8 8 14 5.13 8.12 -5 -9 -14 329.85 16.61 -5 -9 -14 303.86 17.09 5 9 14 321.36 18.85 4 6 -15 3.86 7.36 -4 -6 15 -0.61 6.94 -4 -6 15 1.96 6.73 3 6 -15 -9.49 7.60 -3 -6 15 -9.44 6.99 -3 -6 15 3.49 3.42 2 6 -15 57.58 10.13 -2 -6 15 68.86 11.29 1 6 -15 86.24 10.85 -1 -6 15 90.45 12.35 0 6 -15 47.05 8.95 0 -6 15 49.71 10.46 -1 6 -15 13.55 6.92 1 -6 15 11.15 8.93 4 5 -15 85.54 11.65 -4 -5 15 77.42 9.68 -4 -5 15 88.42 9.32 3 5 -15 123.26 13.37 -3 -5 15 117.54 7.50 -3 -5 15 133.78 12.95 2 5 -15 125.23 13.22 1 5 -15 14.39 7.69 -1 -5 15 8.29 7.45 0 5 -15 28.70 7.76 0 -5 15 30.34 8.87 -1 5 -15 35.94 8.24 1 -5 15 48.08 10.40 -2 5 -15 28.94 7.94 2 -5 15 44.56 10.90 -3 5 -15 3.82 7.20 3 -5 15 22.39 10.72 5 4 -15 62.67 10.70 5 4 -15 72.37 7.90 -5 -4 15 87.77 8.74 4 4 -15 61.33 6.80 4 4 -15 49.94 10.38 -4 -4 15 68.63 8.79 3 4 -15 -1.31 6.93 -3 -4 15 0.09 3.61 -3 -4 15 3.49 6.41 2 4 -15 10.55 6.78 -2 -4 15 16.33 7.54 -2 -4 15 10.02 4.19 1 4 -15 6.20 6.65 -1 -4 15 17.36 7.94 0 4 -15 27.09 8.64 0 -4 15 23.86 8.22 -1 4 -15 6.18 7.34 1 -4 15 0.21 8.12 -2 4 -15 21.12 7.55 2 -4 15 25.03 8.72 -3 4 -15 -4.57 7.33 3 -4 15 -0.76 8.93 -4 4 -15 15.97 7.67 4 -4 15 28.06 9.72 5 3 -15 185.78 11.78 5 3 -15 195.30 15.31 -5 -3 15 187.95 10.84 4 3 -15 482.26 23.08 4 3 -15 473.16 18.42 -4 -3 15 504.25 19.78 3 3 -15 300.60 17.64 3 3 -15 315.56 12.82 -3 -3 15 322.40 16.00 2 3 -15 362.39 19.24 -2 -3 15 376.78 18.14 -2 -3 15 386.88 13.08 1 3 -15 256.08 16.22 -1 -3 15 229.93 15.17 0 3 -15 58.16 10.15 0 -3 15 63.51 10.14 -1 3 -15 31.95 7.63 1 -3 15 40.24 9.75 -2 3 -15 7.88 7.77 2 -3 15 9.06 8.09 -3 3 -15 10.19 7.84 3 -3 15 13.83 8.60 -4 3 -15 74.23 10.58 4 -3 15 77.18 12.20 -5 3 -15 33.31 9.47 5 -3 15 17.70 9.46 5 2 -15 4.44 5.09 5 2 -15 5.69 8.16 4 2 -15 82.42 8.14 4 2 -15 80.64 11.57 -4 -2 15 77.40 7.92 3 2 -15 76.06 7.06 3 2 -15 63.04 9.62 -3 -2 15 72.24 8.23 2 2 -15 15.73 3.55 2 2 -15 7.52 6.47 -2 -2 15 13.14 6.40 1 2 -15 27.64 7.87 -1 -2 15 52.71 8.68 0 2 -15 -2.39 6.32 0 -2 15 4.42 6.87 -1 2 -15 3.32 6.20 1 -2 15 2.74 6.83 -2 2 -15 168.20 14.02 2 -2 15 160.83 13.69 -3 2 -15 503.89 23.06 3 -2 15 478.05 23.71 -4 2 -15 7.36 8.07 4 -2 15 0.77 9.19 -5 2 -15 24.93 7.85 5 -2 15 15.69 8.89 -6 2 -15 -8.01 7.13 6 -2 15 -6.95 8.36 5 1 -15 29.22 6.84 5 1 -15 43.08 9.33 -5 -1 15 22.42 4.31 4 1 -15 3.16 4.67 4 1 -15 6.43 7.20 -4 -1 15 4.35 4.48 3 1 -15 115.24 12.86 3 1 -15 98.16 8.43 -3 -1 15 113.05 9.65 2 1 -15 59.43 5.91 2 1 -15 51.49 9.71 -2 -1 15 68.60 8.39 1 1 -15 182.47 13.47 1 1 -15 175.25 7.77 -1 -1 15 173.99 7.29 -1 -1 15 184.36 12.69 0 1 -15 137.47 11.89 0 -1 15 143.91 12.44 -1 1 -15 54.62 9.18 1 -1 15 43.83 8.89 -2 1 -15 80.84 10.40 2 -1 15 61.68 9.78 -3 1 -15 125.32 12.99 3 -1 15 99.15 11.87 -4 1 -15 76.38 11.09 4 -1 15 60.74 11.06 -5 1 -15 58.37 9.34 5 -1 15 64.76 11.56 -6 1 -15 49.46 9.71 6 -1 15 66.34 11.22 -7 1 -15 22.90 8.37 7 -1 15 22.98 9.68 4 0 -15 19.97 7.77 4 0 -15 34.25 6.64 -4 0 15 30.57 7.00 3 0 -15 9.56 4.48 3 0 -15 9.48 7.98 -3 0 15 11.18 5.12 2 0 -15 57.12 9.37 2 0 -15 58.00 6.05 -2 0 15 57.67 8.05 1 0 -15 1.49 6.89 1 0 -15 5.67 2.98 -1 0 15 0.48 2.82 -1 0 15 -4.25 5.94 0 0 -15 18.61 7.00 0 0 15 9.86 6.04 -1 0 -15 51.56 8.81 1 0 15 67.07 9.02 -2 0 -15 47.77 8.73 2 0 15 52.20 9.15 -3 0 -15 291.31 16.78 -4 0 -15 722.91 28.62 4 0 15 733.10 29.37 -5 0 -15 197.97 14.52 5 0 15 209.20 15.81 -6 0 -15 24.14 7.79 6 0 15 22.61 8.97 -7 0 -15 16.29 7.65 7 0 15 16.50 10.19 4 -1 -15 293.05 17.90 4 -1 -15 266.01 14.95 3 -1 -15 21.49 5.42 3 -1 -15 17.75 8.26 -3 1 15 22.40 5.44 2 -1 -15 5.66 6.61 2 -1 -15 6.63 4.24 -2 1 15 -0.32 4.77 1 -1 -15 22.59 7.92 1 -1 -15 29.89 4.73 -1 1 15 28.49 6.71 0 -1 -15 12.81 2.95 0 -1 -15 16.26 7.03 0 1 15 14.63 3.05 0 1 15 13.36 6.64 -1 -1 -15 -1.04 6.59 1 1 15 4.78 6.67 -2 -1 -15 49.69 8.90 2 1 15 39.43 8.12 -3 -1 -15 11.06 7.42 3 1 15 -4.98 6.82 -4 -1 -15 141.23 12.44 4 1 15 159.01 14.03 -5 -1 -15 31.88 8.06 5 1 15 27.33 8.87 -6 -1 -15 114.86 12.11 6 1 15 87.45 12.08 -7 -1 -15 85.16 11.09 7 1 15 71.25 11.56 -8 -1 -15 17.30 9.29 8 1 15 14.65 9.56 3 -2 -15 39.91 7.31 3 -2 -15 37.80 9.27 -3 2 15 38.53 5.97 2 -2 -15 90.31 8.32 1 -2 -15 5.82 7.12 -1 2 15 2.67 5.14 0 -2 -15 91.89 10.93 0 -2 -15 112.19 7.13 0 2 15 86.74 9.12 0 2 15 109.05 10.57 -1 -2 -15 88.42 5.31 -1 -2 -15 89.34 10.72 1 2 15 92.18 9.92 1 2 15 89.64 5.47 -2 -2 -15 14.71 6.90 2 2 15 27.94 7.52 -3 -2 -15 17.98 7.32 3 2 15 34.25 9.11 -4 -2 -15 18.88 7.13 4 2 15 16.53 7.96 -5 -2 -15 105.42 11.94 5 2 15 144.88 13.66 -6 -2 -15 76.20 10.55 6 2 15 139.96 14.40 -7 -2 -15 33.04 8.76 7 2 15 38.03 10.84 -8 -2 -15 69.39 10.75 8 2 15 48.87 11.08 3 -3 -15 346.58 19.36 3 -3 -15 341.83 17.43 -3 3 15 340.81 14.98 2 -3 -15 265.40 14.46 2 -3 -15 240.92 16.32 -2 3 15 271.11 13.75 1 -3 -15 24.17 8.38 1 -3 -15 39.44 6.29 -1 3 15 39.86 7.18 0 -3 -15 8.08 7.07 0 -3 -15 13.10 4.63 0 3 15 3.14 6.06 -1 -3 -15 126.21 7.70 -1 -3 -15 148.46 13.08 1 3 15 121.87 11.69 -2 -3 -15 65.77 9.55 -2 -3 -15 99.07 5.71 -2 -3 -15 87.74 5.35 2 3 15 92.91 10.67 -3 -3 -15 370.10 19.40 3 3 15 404.39 21.82 -4 -3 -15 36.52 8.30 4 3 15 21.28 8.74 -5 -3 -15 1.35 6.91 5 3 15 -4.66 6.91 -6 -3 -15 11.91 8.08 6 3 15 17.81 8.37 -7 -3 -15 28.86 8.16 7 3 15 26.84 9.21 -8 -3 -15 24.44 8.85 8 3 15 15.30 9.29 2 -4 -15 18.85 7.46 2 -4 -15 10.90 5.82 -2 4 15 11.20 5.40 1 -4 -15 8.41 7.12 1 -4 -15 1.26 4.78 -1 4 15 11.73 6.18 0 -4 -15 74.03 7.72 0 -4 -15 81.41 10.88 0 4 15 87.31 9.71 -1 -4 -15 354.01 18.88 -1 -4 -15 381.19 16.81 1 4 15 354.96 18.02 -2 -4 -15 344.11 13.28 -2 -4 -15 333.31 18.23 2 4 15 343.20 18.06 -3 -4 -15 47.75 8.55 -3 -4 -15 62.21 5.19 -4 -4 -15 5.89 6.52 4 4 15 6.83 7.24 -5 -4 -15 5.18 6.66 5 4 15 -3.22 7.77 -6 -4 -15 -0.30 6.51 6 4 15 10.89 7.82 -7 -4 -15 -2.05 7.20 7 4 15 7.00 8.80 -8 -4 -15 23.31 8.21 8 4 15 10.59 8.69 1 -5 -15 8.79 6.01 1 -5 -15 10.25 7.33 -1 5 15 4.28 5.56 0 -5 -15 11.52 5.58 0 -5 -15 3.41 6.72 0 5 15 -2.53 5.91 -1 -5 -15 123.94 9.22 -1 -5 -15 97.54 11.54 1 5 15 101.48 11.08 -2 -5 -15 165.92 13.00 -2 -5 -15 170.49 13.46 -3 -5 -15 73.06 10.13 -3 -5 -15 92.96 7.11 3 5 15 93.61 11.58 -4 -5 -15 231.65 15.77 -4 -5 -15 231.03 9.93 4 5 15 228.10 15.48 -5 -5 -15 167.10 14.26 -5 -5 -15 161.40 7.37 5 5 15 185.47 14.65 -6 -5 -15 14.14 7.48 6 5 15 18.09 9.21 -7 -5 -15 7.44 7.45 7 5 15 10.69 8.96 -8 -5 -15 1.14 7.75 8 5 15 -3.96 7.60 0 -6 -15 81.60 9.46 0 -6 -15 67.54 9.63 0 6 15 96.62 16.45 -1 -6 -15 53.15 7.38 -1 -6 -15 66.41 9.95 1 6 15 63.41 9.35 -2 -6 -15 186.64 13.95 -2 -6 -15 160.14 10.68 2 6 15 169.14 13.66 -3 -6 -15 276.11 16.63 -3 -6 -15 279.12 13.20 3 6 15 290.07 16.64 -4 -6 -15 81.36 10.58 -4 -6 -15 58.90 7.42 4 6 15 57.31 10.15 -5 -6 -15 38.04 8.77 -5 -6 -15 56.96 5.91 5 6 15 52.69 10.29 -6 -6 -15 50.22 10.08 -6 -6 -15 59.07 5.73 6 6 15 58.69 11.54 -7 -6 -15 39.08 9.79 -7 -6 -15 34.55 5.67 7 6 15 37.75 9.86 -8 -6 -15 330.24 19.89 8 6 15 354.55 21.77 -2 -7 -15 32.59 8.29 -2 -7 -15 34.32 6.92 2 7 15 32.83 8.07 -3 -7 -15 93.75 9.09 -3 -7 -15 74.85 9.94 3 7 15 101.81 11.60 -4 -7 -15 78.93 10.33 -4 -7 -15 115.10 9.40 4 7 15 113.57 12.95 -5 -7 -15 70.18 7.45 -5 -7 -15 69.78 10.66 5 7 15 78.57 11.44 -6 -7 -15 38.86 9.21 6 7 15 24.92 9.31 -7 -7 -15 4.78 5.17 -7 -7 -15 14.27 7.23 7 7 15 15.87 9.54 1 5 -16 16.76 9.13 -1 -5 16 1.58 8.69 0 5 -16 23.04 8.81 0 -5 16 11.38 9.35 3 4 -16 17.27 9.63 -3 -4 16 14.03 7.39 2 4 -16 51.29 9.78 -2 -4 16 51.74 10.92 1 4 -16 10.43 8.17 -1 -4 16 2.81 8.09 0 4 -16 68.02 9.93 0 -4 16 73.64 11.41 -1 4 -16 242.93 15.76 1 -4 16 210.26 17.38 -2 4 -16 208.44 16.03 2 -4 16 205.93 16.42 3 3 -16 20.72 4.51 3 3 -16 19.83 8.39 -3 -3 16 16.09 7.11 2 3 -16 151.16 14.66 -2 -3 16 145.90 12.55 1 3 -16 106.70 12.17 0 3 -16 32.67 8.61 0 -3 16 33.76 9.69 -1 3 -16 50.01 9.18 1 -3 16 49.58 10.42 -2 3 -16 59.75 9.98 2 -3 16 52.13 10.88 -3 3 -16 8.82 7.79 3 -3 16 10.90 8.79 4 -3 16 -0.06 9.92 3 2 -16 316.18 18.69 3 2 -16 322.52 13.26 -3 -2 16 322.54 16.28 2 2 -16 63.69 10.27 -2 -2 16 77.07 9.49 1 2 -16 120.33 13.33 -1 -2 16 141.06 12.58 0 2 -16 226.65 15.96 0 -2 16 244.98 22.50 -1 2 -16 8.76 7.08 1 -2 16 14.35 8.59 -2 2 -16 -0.52 6.64 2 -2 16 -1.14 8.21 -3 2 -16 9.61 7.38 3 -2 16 25.37 9.31 -4 2 -16 22.27 8.85 4 -2 16 19.48 9.41 3 1 -16 -2.91 7.92 3 1 -16 2.84 4.16 -3 -1 16 3.66 5.60 2 1 -16 1.07 3.36 2 1 -16 2.87 8.08 -2 -1 16 -3.46 5.99 1 1 -16 66.10 10.67 -1 -1 16 90.18 10.44 0 1 -16 240.22 16.35 0 -1 16 245.81 15.60 -1 1 -16 46.58 9.12 1 -1 16 61.14 10.17 -2 1 -16 98.03 12.16 2 -1 16 96.20 11.47 -3 1 -16 15.60 7.65 3 -1 16 17.40 8.67 -4 1 -16 48.69 10.18 4 -1 16 57.97 10.73 -5 1 -16 8.24 7.66 5 -1 16 0.43 9.22 3 0 -16 112.56 9.02 3 0 -16 77.34 11.86 -3 0 16 93.45 8.98 2 0 -16 274.73 16.95 2 0 -16 260.09 11.51 -2 0 16 257.34 14.56 1 0 -16 333.27 11.95 1 0 -16 317.32 18.26 -1 0 16 376.90 17.49 0 0 -16 327.03 18.49 0 0 16 393.09 18.94 -1 0 -16 289.95 17.04 -3 0 -16 211.46 15.09 3 0 16 209.35 15.49 -4 0 -16 212.41 15.38 4 0 16 206.50 16.03 -5 0 -16 50.81 9.75 5 0 16 81.61 12.70 -6 0 -16 37.06 9.21 6 0 16 34.81 11.19 2 -1 -16 3.30 6.94 2 -1 -16 2.43 4.35 -2 1 16 -1.37 5.71 1 -1 -16 26.58 8.10 1 -1 -16 22.86 4.16 -1 1 16 20.68 7.04 0 -1 -16 -1.36 7.12 0 1 16 -3.33 6.50 -1 -1 -16 83.55 11.10 1 1 16 73.08 10.31 -2 -1 -16 19.90 8.50 2 1 16 16.94 8.51 -3 -1 -16 20.45 7.70 3 1 16 37.54 8.82 -4 -1 -16 8.45 8.11 4 1 16 7.86 8.64 -5 -1 -16 61.10 10.45 5 1 16 60.27 10.89 -6 -1 -16 43.23 9.89 6 1 16 31.26 10.53 2 -2 -16 10.00 7.69 2 -2 -16 3.69 4.84 -2 2 16 5.00 5.81 1 -2 -16 59.41 9.76 0 -2 -16 176.92 8.62 0 -2 -16 151.92 14.16 0 2 16 165.01 12.74 -1 -2 -16 244.60 16.21 1 2 16 206.74 14.75 2 2 16 197.93 15.05 -3 -2 -16 2.86 7.03 3 2 16 10.21 7.51 -4 -2 -16 61.57 9.97 4 2 16 60.82 11.14 -5 -2 -16 274.06 17.19 5 2 16 299.43 19.50 -6 -2 -16 179.25 15.35 6 2 16 131.11 14.63 -7 -2 -16 226.53 16.55 7 2 16 247.26 18.26 1 -3 -16 98.75 9.01 1 -3 -16 92.96 12.00 -1 3 16 105.42 10.72 0 -3 -16 55.74 9.27 0 3 16 55.56 9.15 -1 -3 -16 -0.46 7.33 -1 -3 -16 -0.94 3.04 -2 -3 -16 23.38 8.32 2 3 16 10.07 7.67 -3 -3 -16 38.18 8.95 3 3 16 58.06 9.63 -4 -3 -16 65.78 10.85 4 3 16 48.73 10.02 -5 -3 -16 -2.80 7.33 5 3 16 -2.03 8.36 -6 -3 -16 117.76 13.29 6 3 16 121.66 14.34 -7 -3 -16 65.42 10.62 7 3 16 68.82 11.91 0 -4 -16 9.44 7.05 0 -4 -16 19.56 5.37 0 4 16 23.55 7.35 -1 -4 -16 11.24 7.95 1 4 16 7.05 7.10 -2 -4 -16 35.74 4.69 -2 -4 -16 30.73 8.21 2 4 16 20.79 8.43 -3 -4 -16 1.63 7.44 3 4 16 3.72 7.65 -4 -4 -16 45.71 10.02 4 4 16 30.15 8.91 -5 -4 -16 9.66 7.65 5 4 16 9.46 8.79 -6 -4 -16 78.44 10.94 6 4 16 87.01 11.98 -7 -4 -16 171.50 15.72 7 4 16 173.96 16.77 -1 -5 -16 19.42 8.05 -1 -5 -16 31.13 5.93 1 5 16 27.67 7.90 -2 -5 -16 6.35 6.98 2 5 16 -9.33 5.88 -3 -5 -16 25.26 4.51 -3 -5 -16 17.60 8.09 3 5 16 26.74 9.05 -4 -5 -16 10.81 7.61 -4 -5 -16 -0.46 4.17 4 5 16 4.97 7.26 -5 -5 -16 73.21 11.19 5 5 16 57.28 11.21 -6 -5 -16 10.69 7.26 6 5 16 15.62 9.04 -3 -6 -16 269.58 17.04 -3 -6 -16 268.07 12.65 3 6 16 253.40 16.94 -4 -6 -16 228.57 11.17 4 6 16 236.52 17.24 5 6 16 290.75 18.22 0 2 -17 -0.29 8.03 0 -2 17 8.58 8.35 -1 2 -17 55.15 10.08 1 -2 17 53.83 11.01 -2 2 -17 14.36 8.24 2 -2 17 22.01 8.88 1 1 -17 7.42 7.86 -1 -1 17 13.15 8.14 0 1 -17 8.90 8.20 0 -1 17 -11.70 7.16 -1 1 -17 43.63 9.61 1 -1 17 37.42 10.10 -2 1 -17 13.45 8.26 2 -1 17 -6.71 8.34 -3 1 -17 27.55 10.04 3 -1 17 34.78 10.98 1 0 -17 21.69 8.80 0 0 -17 165.21 15.28 0 0 17 208.39 14.62 -1 0 -17 275.16 17.53 1 0 17 281.59 17.71 -2 0 -17 70.18 10.94 2 0 17 54.76 10.78 -3 0 -17 19.99 9.33 3 0 17 15.03 8.94 -4 0 -17 7.91 8.49 4 0 17 -14.26 7.07 0 -1 -17 72.90 11.33 0 1 17 93.93 10.76 -1 -1 -17 16.88 8.80 1 1 17 13.63 8.30 -2 -1 -17 29.91 8.80 2 1 17 34.48 9.72 -3 -1 -17 2.76 7.70 3 1 17 -17.91 7.60 -4 -1 -17 20.74 9.10 4 1 17 -6.86 8.39 0 2 17 87.29 10.34 -1 -2 -17 83.76 11.57 1 2 17 93.98 11.29 -2 -2 -17 350.05 19.94 -3 -2 -17 186.00 15.03 3 2 17 211.98 15.63 -4 -2 -17 39.90 10.25 4 2 17 56.50 10.81 -2 -3 -17 18.94 8.94 2 3 17 22.32 8.10 -3 -3 -17 4.84 8.44 3 3 17 18.89 8.63 -4 -3 -17 10.90 8.73 4 3 17 10.96 8.15 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6912 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71075 10.334 10.779 13.090 87.710 82.166 62.503 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 73765 _shelx_res_file ; TITL shelxt_a.res in P-1 shelx.res created by SHELXL-2019/3 at 12:58:15 on 24-Apr-2024 CELL 0.71073 10.3309 10.7727 13.0821 87.692 82.138 62.507 ZERR 1.00 0.0005 0.0005 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H BR O P S MN UNIT 56.5 51 2 4 2 2 2 MERG 2 OMIT 1 0 0 OMIT 1 1 1 OMIT 0 -1 1 OMIT 1 0 1 OMIT 0 1 1 OMIT 1 1 0 SADI 1.86 C1 BR1 C3 BR1a SADI 3.56 BR1 S1 BR1A S1 SIZE 0.05 0.03 0.02 TEMP -165 ACTA FMAP 2 PLAN -5 BOND $H CONF L.S. 64 WGHT 0.064500 9.205500 FVAR 0.59745 0.73796 0.09057 MOLE 1 MN1 7 0.547147 0.164697 0.713076 11.00000 0.01593 0.01693 = 0.01218 -0.00325 0.00185 -0.00827 P1 5 0.358160 0.285828 0.835194 11.00000 0.01504 0.01679 = 0.01209 -0.00273 0.00094 -0.00906 S1 6 0.824562 0.064498 0.511708 11.00000 0.02351 0.03924 = 0.03441 0.00137 0.01343 -0.01004 C1 1 0.510086 0.188258 0.553862 11.00000 0.02997 0.02841 = 0.01283 -0.00046 -0.00085 -0.01644 PART 2 AFIX 43 H1 2 0.491185 0.269896 0.515011 10.04500 -1.20000 PART 1 AFIX 0 BR1 3 0.475951 0.339466 0.467063 10.95500 0.03882 0.03443 = 0.02047 0.00277 -0.00119 -0.01399 PART 0 C2 1 0.651927 0.075869 0.563376 11.00000 0.03013 0.02609 = 0.01648 -0.00844 0.00679 -0.01073 C3 1 0.629300 -0.024556 0.625643 11.00000 0.03558 0.01960 = 0.02169 -0.01005 0.00377 -0.01002 PART 1 AFIX 43 H3 2 0.704560 -0.111543 0.644236 10.95500 -1.20000 PART 2 AFIX 0 BR1A 3 0.810390 -0.174848 0.613505 10.04500 0.03889 0.02399 = 0.02193 -0.00972 0.00126 -0.00471 PART 0 C4 1 0.476983 0.025317 0.655654 11.00000 0.03736 0.02825 = 0.01987 -0.00782 0.00013 -0.02204 AFIX 43 H4 2 0.432080 -0.021757 0.697919 11.00000 -1.20000 AFIX 0 C5 1 0.402315 0.158734 0.611422 11.00000 0.02816 0.03501 = 0.01639 -0.00650 -0.00117 -0.01955 AFIX 43 H5 2 0.298887 0.217106 0.619266 11.00000 -1.20000 AFIX 0 C6 1 0.609466 0.293733 0.708778 11.00000 0.01899 0.02738 = 0.01563 -0.00253 0.00166 -0.01073 C7 1 0.660189 0.069099 0.808305 11.00000 0.01747 0.01993 = 0.02309 -0.00422 0.00332 -0.00878 C8 1 0.852764 -0.006909 0.387355 11.00000 0.04399 0.05175 = 0.02729 -0.02047 0.01521 -0.02673 AFIX 137 H8A 2 0.843033 -0.093309 0.392390 11.00000 -1.50000 H8B 2 0.951684 -0.027761 0.353846 11.00000 -1.50000 H8C 2 0.779304 0.060516 0.346471 11.00000 -1.50000 AFIX 0 C11 1 0.402266 0.289625 0.965881 11.00000 0.02359 0.01713 = 0.01466 -0.00298 -0.00324 -0.01056 C12 1 0.517659 0.319848 0.978014 11.00000 0.02547 0.02558 = 0.02111 -0.00355 -0.00265 -0.01381 AFIX 43 H12 2 0.574311 0.332310 0.918705 11.00000 -1.20000 AFIX 0 C13 1 0.550191 0.331786 1.075365 11.00000 0.03682 0.02957 = 0.02909 -0.00443 -0.01575 -0.01763 AFIX 43 H13 2 0.628362 0.352716 1.082559 11.00000 -1.20000 AFIX 0 C14 1 0.468139 0.313053 1.162404 11.00000 0.05983 0.03128 = 0.01792 -0.00127 -0.01472 -0.02153 AFIX 43 H14 2 0.490055 0.321166 1.229262 11.00000 -1.20000 AFIX 0 C15 1 0.355582 0.282861 1.151545 11.00000 0.06360 0.04431 = 0.01666 0.00043 0.00007 -0.03215 AFIX 43 H15 2 0.299858 0.270087 1.211285 11.00000 -1.20000 AFIX 0 C16 1 0.321431 0.270544 1.053732 11.00000 0.04215 0.03950 = 0.01478 -0.00409 0.00215 -0.02782 AFIX 43 H16 2 0.243299 0.249221 1.047335 11.00000 -1.20000 AFIX 0 C21 1 0.248399 0.473533 0.815523 11.00000 0.01632 0.01745 = 0.01916 -0.00241 0.00004 -0.00898 C22 1 0.264150 0.528859 0.720023 11.00000 0.02468 0.01906 = 0.02209 -0.00244 0.00532 -0.00813 AFIX 43 H22 2 0.334099 0.469859 0.665733 11.00000 -1.20000 AFIX 0 C23 1 0.178106 0.670535 0.702944 11.00000 0.02988 0.02265 = 0.02935 0.00545 0.00280 -0.00770 AFIX 43 H23 2 0.189550 0.707571 0.637129 11.00000 -1.20000 AFIX 0 C24 1 0.076368 0.757116 0.781365 11.00000 0.02506 0.01764 = 0.03960 -0.00426 0.00228 -0.00630 AFIX 43 H24 2 0.017167 0.853396 0.769258 11.00000 -1.20000 AFIX 0 C25 1 0.060557 0.703952 0.877361 11.00000 0.02147 0.02342 = 0.02866 -0.00996 0.00406 -0.00946 AFIX 43 H25 2 -0.008946 0.763828 0.931452 11.00000 -1.20000 AFIX 0 C26 1 0.146155 0.562993 0.894971 11.00000 0.01927 0.02366 = 0.02067 -0.00589 0.00261 -0.01008 AFIX 43 H26 2 0.135349 0.526954 0.961299 11.00000 -1.20000 AFIX 0 C31 1 0.217783 0.224487 0.853835 11.00000 0.01982 0.02227 = 0.01242 -0.00346 0.00282 -0.01381 C32 1 0.075835 0.306285 0.830995 11.00000 0.02328 0.02626 = 0.01879 0.00043 -0.00297 -0.01424 AFIX 43 H32 2 0.047084 0.399577 0.809408 11.00000 -1.20000 AFIX 0 C33 1 -0.025652 0.252952 0.839385 11.00000 0.02158 0.04105 = 0.02495 -0.00097 -0.00263 -0.02008 AFIX 43 H33 2 -0.122260 0.309435 0.822666 11.00000 -1.20000 AFIX 0 C34 1 0.015348 0.117254 0.872219 11.00000 0.02952 0.03752 = 0.02328 -0.00631 0.00454 -0.02586 AFIX 43 H34 2 -0.053502 0.081039 0.878505 11.00000 -1.20000 AFIX 0 C35 1 0.156457 0.034777 0.895781 11.00000 0.03467 0.02590 = 0.02015 -0.00369 0.00388 -0.02060 AFIX 43 H35 2 0.183997 -0.057732 0.918830 11.00000 -1.20000 AFIX 0 C36 1 0.258445 0.086957 0.885818 11.00000 0.02115 0.02184 = 0.01853 -0.00385 0.00150 -0.01189 AFIX 43 H36 2 0.355770 0.029192 0.900736 11.00000 -1.20000 AFIX 0 O1 4 0.653820 0.375156 0.702088 11.00000 0.03613 0.03609 = 0.03735 0.00091 -0.00001 -0.02668 O2 4 0.738253 0.003994 0.867176 11.00000 0.02362 0.02749 = 0.02969 0.00381 -0.00900 -0.00752 MOLE 2 PART 1 10.75 C1S 1 1.033068 -0.406035 0.466429 10.75000 0.06902 0.08365 = 0.20561 0.07553 -0.06489 -0.03910 AFIX 23 H1S1 2 1.005659 -0.318186 0.428126 10.75000 -1.20000 H1S2 2 1.129538 -0.433667 0.490033 10.75000 -1.20000 AFIX 0 C2S 1 0.932260 -0.385724 0.547044 10.75000 0.05315 0.07845 = 0.11436 -0.05189 -0.02388 -0.00097 AFIX 23 H2S1 2 0.931956 -0.318171 0.596311 10.75000 -1.20000 H2S2 2 0.833780 -0.345250 0.523974 10.75000 -1.20000 AFIX 0 C3S 1 0.957653 -0.499301 0.591723 10.75000 0.10584 0.23799 = 0.05816 0.05499 -0.04011 -0.11538 AFIX 23 H3S1 2 1.050981 -0.533266 0.621448 10.75000 -1.20000 H3S2 2 0.877962 -0.481000 0.649513 10.75000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.1701, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0662 for 5421 Fo > 4sig(Fo) and 0.0765 for all 6351 data REM 328 parameters refined using 2 restraints END WGHT 0.0644 9.2077 REM Highest difference peak 5.858, deepest hole -1.710, 1-sigma level 0.143 Q1 1 0.7953 0.0397 0.4651 11.00000 0.05 5.86 Q2 1 0.8045 0.1277 0.5011 11.00000 0.05 1.41 Q3 1 0.2578 0.4186 0.4637 11.00000 0.05 0.82 Q4 1 0.3601 0.4059 0.4482 11.00000 0.05 0.51 Q5 1 0.0980 0.6324 0.8754 11.00000 0.05 0.50 ; _shelx_res_checksum 89082 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Mn Mn1 0.54715(7) 0.16470(6) 0.71308(5) 0.01502(15) Uani d 1 . . P P1 0.35816(11) 0.28583(11) 0.83519(8) 0.0142(2) Uani d 1 . . S S1 0.82456(14) 0.06450(15) 0.51171(11) 0.0360(3) Uani d 1 . . C C1 0.5101(5) 0.1883(5) 0.5539(3) 0.0227(9) Uani d 1 . . H H1 0.491185 0.269896 0.515011 0.027 Uiso calc 0.045 A 2 Br Br1 0.47595(6) 0.33947(6) 0.46706(4) 0.03273(16) Uani d 0.955 B 1 C C2 0.6519(5) 0.0759(5) 0.5634(3) 0.0259(9) Uani d 1 . . C C3 0.6293(6) -0.0246(5) 0.6256(4) 0.0272(10) Uani d 1 . . H H3 0.704560 -0.111543 0.644236 0.033 Uiso calc 0.955 C 1 Br Br1A 0.8104(13) -0.1748(11) 0.6135(8) 0.032(2) Uani d 0.045 D 2 C C4 0.4770(6) 0.0253(5) 0.6557(4) 0.0259(10) Uani d 1 . . H H4 0.432080 -0.021757 0.697919 0.031 Uiso calc 1 . . C C5 0.4023(5) 0.1587(5) 0.6114(3) 0.0245(9) Uani d 1 . . H H5 0.298887 0.217106 0.619266 0.029 Uiso calc 1 . . C C6 0.6095(5) 0.2937(5) 0.7088(3) 0.0210(8) Uani d 1 . . C C7 0.6602(5) 0.0691(5) 0.8083(3) 0.0206(8) Uani d 1 . . C C8 0.8528(7) -0.0069(7) 0.3874(4) 0.0406(14) Uani d 1 . . H H8A 0.843033 -0.093309 0.392390 0.061 Uiso calc 1 . . H H8B 0.951684 -0.027761 0.353846 0.061 Uiso calc 1 . . H H8C 0.779304 0.060516 0.346471 0.061 Uiso calc 1 . . C C11 0.4023(5) 0.2896(4) 0.9659(3) 0.0178(8) Uani d 1 . . C C12 0.5177(5) 0.3198(5) 0.9780(4) 0.0232(9) Uani d 1 . . H H12 0.574311 0.332310 0.918705 0.028 Uiso calc 1 . . C C13 0.5502(6) 0.3318(5) 1.0754(4) 0.0296(10) Uani d 1 . . H H13 0.628362 0.352716 1.082559 0.035 Uiso calc 1 . . C C14 0.4681(7) 0.3131(6) 1.1624(4) 0.0351(12) Uani d 1 . . H H14 0.490055 0.321166 1.229262 0.042 Uiso calc 1 . . C C15 0.3556(7) 0.2829(6) 1.1515(4) 0.0392(13) Uani d 1 . . H H15 0.299858 0.270087 1.211285 0.047 Uiso calc 1 . . C C16 0.3214(6) 0.2705(6) 1.0537(3) 0.0291(10) Uani d 1 . . H H16 0.243299 0.249221 1.047335 0.035 Uiso calc 1 . . C C21 0.2484(4) 0.4735(4) 0.8155(3) 0.0173(8) Uani d 1 . . C C22 0.2642(5) 0.5289(5) 0.7200(4) 0.0235(9) Uani d 1 . . H H22 0.334099 0.469859 0.665733 0.028 Uiso calc 1 . . C C23 0.1781(6) 0.6705(5) 0.7029(4) 0.0299(10) Uani d 1 . . H H23 0.189550 0.707571 0.637129 0.036 Uiso calc 1 . . C C24 0.0764(5) 0.7571(5) 0.7814(4) 0.0294(10) Uani d 1 . . H H24 0.017167 0.853396 0.769258 0.035 Uiso calc 1 . . C C25 0.0606(5) 0.7040(5) 0.8774(4) 0.0253(9) Uani d 1 . . H H25 -0.008946 0.763828 0.931452 0.030 Uiso calc 1 . . C C26 0.1462(5) 0.5630(5) 0.8950(3) 0.0215(8) Uani d 1 . . H H26 0.135349 0.526954 0.961299 0.026 Uiso calc 1 . . C C31 0.2178(5) 0.2245(4) 0.8538(3) 0.0169(8) Uani d 1 . . C C32 0.0758(5) 0.3063(5) 0.8310(3) 0.0216(8) Uani d 1 . . H H32 0.047084 0.399577 0.809408 0.026 Uiso calc 1 . . C C33 -0.0257(5) 0.2530(6) 0.8394(4) 0.0270(10) Uani d 1 . . H H33 -0.122260 0.309435 0.822666 0.032 Uiso calc 1 . . C C34 0.0153(5) 0.1173(5) 0.8722(4) 0.0266(10) Uani d 1 . . H H34 -0.053502 0.081039 0.878505 0.032 Uiso calc 1 . . C C35 0.1565(6) 0.0348(5) 0.8958(3) 0.0249(9) Uani d 1 . . H H35 0.183997 -0.057732 0.918830 0.030 Uiso calc 1 . . C C36 0.2584(5) 0.0870(5) 0.8858(3) 0.0200(8) Uani d 1 . . H H36 0.355770 0.029192 0.900736 0.024 Uiso calc 1 . . O O1 0.6538(4) 0.3752(4) 0.7021(3) 0.0331(8) Uani d 1 . . O O2 0.7383(4) 0.0040(4) 0.8672(3) 0.0281(7) Uani d 1 . . C C1S 1.0331(18) -0.4060(19) 0.466(2) 0.115(7) Uani d 0.75 E 1 H H1S1 1.005659 -0.318186 0.428126 0.138 Uiso calc 0.75 E 1 H H1S2 1.129538 -0.433667 0.490033 0.138 Uiso calc 0.75 E 1 C C2S 0.9323(15) -0.3857(16) 0.5470(15) 0.091(5) Uani d 0.75 E 1 H H2S1 0.931956 -0.318171 0.596311 0.109 Uiso calc 0.75 E 1 H H2S2 0.833780 -0.345250 0.523974 0.109 Uiso calc 0.75 E 1 C C3S 0.958(2) -0.499(3) 0.5917(11) 0.118(8) Uani d 0.75 E 1 H H3S1 1.050981 -0.533266 0.621448 0.142 Uiso calc 0.75 E 1 H H3S2 0.877962 -0.481000 0.649513 0.142 Uiso calc 0.75 E 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn1 0.0159(3) 0.0169(3) 0.0122(3) -0.0083(2) 0.0018(2) -0.0032(2) P1 0.0150(5) 0.0168(5) 0.0121(4) -0.0091(4) 0.0009(3) -0.0027(3) S1 0.0235(6) 0.0392(7) 0.0344(7) -0.0100(5) 0.0134(5) 0.0014(5) C1 0.030(2) 0.028(2) 0.0128(18) -0.0164(19) -0.0009(16) -0.0005(16) Br1 0.0388(3) 0.0344(3) 0.0205(2) -0.0140(2) -0.0012(2) 0.00277(19) C2 0.030(2) 0.026(2) 0.016(2) -0.0107(19) 0.0068(17) -0.0084(17) C3 0.036(3) 0.020(2) 0.022(2) -0.0100(19) 0.0038(19) -0.0100(17) Br1A 0.039(6) 0.024(5) 0.022(5) -0.005(4) 0.001(4) -0.010(4) C4 0.037(3) 0.028(2) 0.020(2) -0.022(2) 0.0001(18) -0.0078(17) C5 0.028(2) 0.035(2) 0.016(2) -0.020(2) -0.0012(17) -0.0065(17) C6 0.019(2) 0.027(2) 0.0156(19) -0.0107(17) 0.0017(15) -0.0025(16) C7 0.0175(19) 0.020(2) 0.023(2) -0.0088(16) 0.0033(16) -0.0042(16) C8 0.044(3) 0.052(3) 0.027(3) -0.027(3) 0.015(2) -0.020(2) C11 0.024(2) 0.0171(19) 0.0147(18) -0.0106(16) -0.0032(15) -0.0030(14) C12 0.025(2) 0.026(2) 0.021(2) -0.0138(18) -0.0026(17) -0.0035(17) C13 0.037(3) 0.030(2) 0.029(2) -0.018(2) -0.016(2) -0.0044(19) C14 0.060(4) 0.031(3) 0.018(2) -0.022(3) -0.015(2) -0.0013(19) C15 0.064(4) 0.044(3) 0.017(2) -0.032(3) 0.000(2) 0.000(2) C16 0.042(3) 0.039(3) 0.015(2) -0.028(2) 0.0022(19) -0.0041(18) C21 0.0163(18) 0.0175(19) 0.0192(19) -0.0090(15) 0.0000(15) -0.0024(15) C22 0.025(2) 0.019(2) 0.022(2) -0.0081(17) 0.0053(17) -0.0024(16) C23 0.030(2) 0.023(2) 0.029(2) -0.0077(19) 0.0028(19) 0.0054(18) C24 0.025(2) 0.018(2) 0.040(3) -0.0063(18) 0.002(2) -0.0043(19) C25 0.021(2) 0.023(2) 0.029(2) -0.0095(18) 0.0041(18) -0.0100(18) C26 0.019(2) 0.024(2) 0.021(2) -0.0101(17) 0.0026(16) -0.0059(16) C31 0.0198(19) 0.022(2) 0.0124(17) -0.0138(16) 0.0028(14) -0.0035(14) C32 0.023(2) 0.026(2) 0.019(2) -0.0142(18) -0.0030(16) 0.0004(16) C33 0.022(2) 0.041(3) 0.025(2) -0.020(2) -0.0026(17) -0.0010(19) C34 0.030(2) 0.038(3) 0.023(2) -0.026(2) 0.0045(18) -0.0063(19) C35 0.035(2) 0.026(2) 0.020(2) -0.021(2) 0.0039(18) -0.0037(17) C36 0.021(2) 0.022(2) 0.0185(19) -0.0119(17) 0.0015(16) -0.0038(15) O1 0.036(2) 0.036(2) 0.037(2) -0.0267(17) 0.0000(16) 0.0009(16) O2 0.0236(16) 0.0275(17) 0.0297(18) -0.0075(14) -0.0090(14) 0.0038(14) C1S 0.069(10) 0.084(10) 0.21(2) -0.039(9) -0.065(13) 0.076(13) C2S 0.053(7) 0.078(9) 0.114(12) -0.001(6) -0.024(8) -0.052(9) C3S 0.106(13) 0.24(3) 0.058(8) -0.115(16) -0.040(8) 0.055(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' Br Br -0.2901 2.4595 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 C6 Mn1 C7 . . 92.4(2) ? C6 Mn1 C3 . . 130.5(2) ? C7 Mn1 C3 . . 88.9(2) ? C6 Mn1 C2 . . 96.08(19) ? C7 Mn1 C2 . . 110.3(2) ? C3 Mn1 C2 . . 38.83(18) ? C6 Mn1 C4 . . 157.66(19) ? C7 Mn1 C4 . . 105.0(2) ? C3 Mn1 C4 . . 38.58(19) ? C2 Mn1 C4 . . 65.07(19) ? C6 Mn1 C1 . . 93.66(19) ? C7 Mn1 C1 . . 149.07(19) ? C3 Mn1 C1 . . 64.38(19) ? C2 Mn1 C1 . . 38.84(18) ? C4 Mn1 C1 . . 64.22(18) ? C6 Mn1 C5 . . 123.9(2) ? C7 Mn1 C5 . . 143.4(2) ? C3 Mn1 C5 . . 64.7(2) ? C2 Mn1 C5 . . 65.09(19) ? C4 Mn1 C5 . . 38.68(19) ? C1 Mn1 C5 . . 38.17(17) ? C6 Mn1 P1 . . 92.24(14) ? C7 Mn1 P1 . . 91.15(14) ? C3 Mn1 P1 . . 137.23(14) ? C2 Mn1 P1 . . 156.51(15) ? C4 Mn1 P1 . . 101.06(13) ? C1 Mn1 P1 . . 118.84(13) ? C5 Mn1 P1 . . 92.09(13) ? C21 P1 C11 . . 100.49(19) ? C21 P1 C31 . . 102.39(19) ? C11 P1 C31 . . 103.84(19) ? C21 P1 Mn1 . . 117.10(14) ? C11 P1 Mn1 . . 116.99(14) ? C31 P1 Mn1 . . 113.90(13) ? C8 S1 C2 . . 102.4(3) ? C5 C1 C2 . . 109.0(4) ? C5 C1 Br1 . . 126.4(4) ? C2 C1 Br1 . . 124.3(3) ? C5 C1 Mn1 . . 71.1(2) ? C2 C1 Mn1 . . 69.7(3) ? Br1 C1 Mn1 . . 130.1(2) ? C5 C1 H1 . . 125.5 ? C2 C1 H1 . . 125.5 ? Mn1 C1 H1 . . 125.3 ? C3 C2 C1 . . 106.8(4) ? C3 C2 S1 . . 125.9(4) ? C1 C2 S1 . . 127.3(4) ? C3 C2 Mn1 . . 70.3(2) ? C1 C2 Mn1 . . 71.4(2) ? S1 C2 Mn1 . . 121.7(3) ? C4 C3 C2 . . 108.9(4) ? C4 C3 Br1A . . 146.5(6) ? C2 C3 Br1A . . 103.4(5) ? C4 C3 Mn1 . . 71.4(3) ? C2 C3 Mn1 . . 70.8(3) ? Br1A C3 Mn1 . . 129.5(5) ? C4 C3 H3 . . 125.5 ? C2 C3 H3 . . 125.5 ? Mn1 C3 H3 . . 123.8 ? C3 C4 C5 . . 107.9(4) ? C3 C4 Mn1 . . 70.0(3) ? C5 C4 Mn1 . . 71.2(3) ? C3 C4 H4 . . 126.0 ? C5 C4 H4 . . 126.0 ? Mn1 C4 H4 . . 124.4 ? C1 C5 C4 . . 107.4(4) ? C1 C5 Mn1 . . 70.8(3) ? C4 C5 Mn1 . . 70.1(3) ? C1 C5 H5 . . 126.3 ? C4 C5 H5 . . 126.3 ? Mn1 C5 H5 . . 124.4 ? O1 C6 Mn1 . . 177.1(4) ? O2 C7 Mn1 . . 177.3(4) ? S1 C8 H8A . . 109.5 ? S1 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? S1 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C16 C11 C12 . . 118.6(4) ? C16 C11 P1 . . 122.7(3) ? C12 C11 P1 . . 118.6(3) ? C13 C12 C11 . . 120.9(4) ? C13 C12 H12 . . 119.5 ? C11 C12 H12 . . 119.5 ? C12 C13 C14 . . 119.8(5) ? C12 C13 H13 . . 120.1 ? C14 C13 H13 . . 120.1 ? C15 C14 C13 . . 119.8(4) ? C15 C14 H14 . . 120.1 ? C13 C14 H14 . . 120.1 ? C14 C15 C16 . . 121.0(5) ? C14 C15 H15 . . 119.5 ? C16 C15 H15 . . 119.5 ? C11 C16 C15 . . 119.8(5) ? C11 C16 H16 . . 120.1 ? C15 C16 H16 . . 120.1 ? C22 C21 C26 . . 118.8(4) ? C22 C21 P1 . . 119.8(3) ? C26 C21 P1 . . 121.4(3) ? C21 C22 C23 . . 120.5(4) ? C21 C22 H22 . . 119.8 ? C23 C22 H22 . . 119.8 ? C24 C23 C22 . . 120.2(5) ? C24 C23 H23 . . 119.9 ? C22 C23 H23 . . 119.9 ? C23 C24 C25 . . 120.0(4) ? C23 C24 H24 . . 120.0 ? C25 C24 H24 . . 120.0 ? C24 C25 C26 . . 120.1(4) ? C24 C25 H25 . . 120.0 ? C26 C25 H25 . . 120.0 ? C25 C26 C21 . . 120.4(4) ? C25 C26 H26 . . 119.8 ? C21 C26 H26 . . 119.8 ? C32 C31 C36 . . 118.9(4) ? C32 C31 P1 . . 122.2(3) ? C36 C31 P1 . . 118.8(3) ? C31 C32 C33 . . 120.7(4) ? C31 C32 H32 . . 119.6 ? C33 C32 H32 . . 119.6 ? C34 C33 C32 . . 119.8(4) ? C34 C33 H33 . . 120.1 ? C32 C33 H33 . . 120.1 ? C35 C34 C33 . . 120.0(4) ? C35 C34 H34 . . 120.0 ? C33 C34 H34 . . 120.0 ? C34 C35 C36 . . 120.3(4) ? C34 C35 H35 . . 119.9 ? C36 C35 H35 . . 119.9 ? C35 C36 C31 . . 120.2(4) ? C35 C36 H36 . . 119.9 ? C31 C36 H36 . . 119.9 ? C3S C1S C2S 2_746 . 109.4(15) ? C3S C1S H1S1 2_746 . 109.8 ? C2S C1S H1S1 . . 109.8 ? C3S C1S H1S2 2_746 . 109.8 ? C2S C1S H1S2 . . 109.8 ? H1S1 C1S H1S2 . . 108.2 ? C3S C2S C1S . . 111.0(14) ? C3S C2S H2S1 . . 109.4 ? C1S C2S H2S1 . . 109.4 ? C3S C2S H2S2 . . 109.4 ? C1S C2S H2S2 . . 109.4 ? H2S1 C2S H2S2 . . 108.0 ? C1S C3S C2S 2_746 . 113.9(14) ? C1S C3S H3S1 2_746 . 108.8 ? C2S C3S H3S1 . . 108.8 ? C1S C3S H3S2 2_746 . 108.8 ? C2S C3S H3S2 . . 108.8 ? H3S1 C3S H3S2 . . 107.7 ? 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 Mn1 C6 . 1.778(5) ? Mn1 C7 . 1.778(5) ? Mn1 C3 . 2.124(4) ? Mn1 C2 . 2.130(4) ? Mn1 C4 . 2.142(4) ? Mn1 C1 . 2.153(4) ? Mn1 C5 . 2.157(4) ? Mn1 P1 . 2.2426(11) ? P1 C21 . 1.834(4) ? P1 C11 . 1.835(4) ? P1 C31 . 1.837(4) ? S1 C8 . 1.757(5) ? S1 C2 . 1.769(5) ? C1 C5 . 1.409(6) ? C1 C2 . 1.424(7) ? C1 Br1 . 1.870(5) ? C1 H1 . 0.9500 ? C2 C3 . 1.414(7) ? C3 C4 . 1.409(7) ? C3 Br1A . 1.814(12) ? C3 H3 . 0.9500 ? C4 C5 . 1.424(7) ? C4 H4 . 0.9500 ? C5 H5 . 0.9500 ? C6 O1 . 1.158(6) ? C7 O2 . 1.157(6) ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C11 C16 . 1.392(6) ? C11 C12 . 1.402(6) ? C12 C13 . 1.386(6) ? C12 H12 . 0.9500 ? C13 C14 . 1.390(8) ? C13 H13 . 0.9500 ? C14 C15 . 1.370(9) ? C14 H14 . 0.9500 ? C15 C16 . 1.400(7) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? C21 C22 . 1.384(6) ? C21 C26 . 1.402(6) ? C22 C23 . 1.394(6) ? C22 H22 . 0.9500 ? C23 C24 . 1.380(7) ? C23 H23 . 0.9500 ? C24 C25 . 1.380(7) ? C24 H24 . 0.9500 ? C25 C26 . 1.389(7) ? C25 H25 . 0.9500 ? C26 H26 . 0.9500 ? C31 C32 . 1.386(6) ? C31 C36 . 1.404(6) ? C32 C33 . 1.400(6) ? C32 H32 . 0.9500 ? C33 C34 . 1.389(7) ? C33 H33 . 0.9500 ? C34 C35 . 1.384(7) ? C34 H34 . 0.9500 ? C35 C36 . 1.395(6) ? C35 H35 . 0.9500 ? C36 H36 . 0.9500 ? C1S C3S 2_746 1.26(3) ? C1S C2S . 1.32(2) ? C1S H1S1 . 0.9900 ? C1S H1S2 . 0.9900 ? C2S C3S . 1.26(2) ? C2S H2S1 . 0.9900 ? C2S H2S2 . 0.9900 ? C3S H3S1 . 0.9900 ? C3S H3S2 . 0.9900 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C5 C1 C2 C3 . . . . 1.4(5) ? Br1 C1 C2 C3 . . . . -172.7(3) ? Mn1 C1 C2 C3 . . . . 61.8(3) ? C5 C1 C2 S1 . . . . -176.7(3) ? Br1 C1 C2 S1 . . . . 9.3(6) ? Mn1 C1 C2 S1 . . . . -116.2(4) ? C5 C1 C2 Mn1 . . . . -60.5(3) ? Br1 C1 C2 Mn1 . . . . 125.4(3) ? C8 S1 C2 C3 . . . . 95.3(5) ? C8 S1 C2 C1 . . . . -87.1(5) ? C8 S1 C2 Mn1 . . . . -177.1(3) ? C1 C2 C3 C4 . . . . -1.0(5) ? S1 C2 C3 C4 . . . . 177.1(3) ? Mn1 C2 C3 C4 . . . . 61.6(3) ? C1 C2 C3 Br1A . . . . 169.8(5) ? S1 C2 C3 Br1A . . . . -12.1(6) ? Mn1 C2 C3 Br1A . . . . -127.6(4) ? C1 C2 C3 Mn1 . . . . -62.6(3) ? S1 C2 C3 Mn1 . . . . 115.5(4) ? C2 C3 C4 C5 . . . . 0.2(5) ? Br1A C3 C4 C5 . . . . -163.5(8) ? Mn1 C3 C4 C5 . . . . 61.5(3) ? C2 C3 C4 Mn1 . . . . -61.2(3) ? Br1A C3 C4 Mn1 . . . . 135.1(9) ? C2 C1 C5 C4 . . . . -1.2(5) ? Br1 C1 C5 C4 . . . . 172.7(3) ? Mn1 C1 C5 C4 . . . . -60.9(3) ? C2 C1 C5 Mn1 . . . . 59.6(3) ? Br1 C1 C5 Mn1 . . . . -126.4(4) ? C3 C4 C5 C1 . . . . 0.6(5) ? Mn1 C4 C5 C1 . . . . 61.3(3) ? C3 C4 C5 Mn1 . . . . -60.7(3) ? C21 P1 C11 C16 . . . . 96.5(4) ? C31 P1 C11 C16 . . . . -9.2(4) ? Mn1 P1 C11 C16 . . . . -135.6(4) ? C21 P1 C11 C12 . . . . -80.3(4) ? C31 P1 C11 C12 . . . . 174.0(3) ? Mn1 P1 C11 C12 . . . . 47.6(4) ? C16 C11 C12 C13 . . . . -0.6(7) ? P1 C11 C12 C13 . . . . 176.4(4) ? C11 C12 C13 C14 . . . . 0.3(7) ? C12 C13 C14 C15 . . . . 0.0(8) ? C13 C14 C15 C16 . . . . 0.0(9) ? C12 C11 C16 C15 . . . . 0.5(7) ? P1 C11 C16 C15 . . . . -176.2(4) ? C14 C15 C16 C11 . . . . -0.2(9) ? C11 P1 C21 C22 . . . . 140.8(4) ? C31 P1 C21 C22 . . . . -112.4(4) ? Mn1 P1 C21 C22 . . . . 13.0(4) ? C11 P1 C21 C26 . . . . -40.3(4) ? C31 P1 C21 C26 . . . . 66.6(4) ? Mn1 P1 C21 C26 . . . . -168.1(3) ? C26 C21 C22 C23 . . . . -1.0(7) ? P1 C21 C22 C23 . . . . 177.9(4) ? C21 C22 C23 C24 . . . . 0.1(8) ? C22 C23 C24 C25 . . . . 0.7(8) ? C23 C24 C25 C26 . . . . -0.5(8) ? C24 C25 C26 C21 . . . . -0.4(7) ? C22 C21 C26 C25 . . . . 1.2(6) ? P1 C21 C26 C25 . . . . -177.8(3) ? C21 P1 C31 C32 . . . . 13.2(4) ? C11 P1 C31 C32 . . . . 117.4(4) ? Mn1 P1 C31 C32 . . . . -114.2(3) ? C21 P1 C31 C36 . . . . -171.1(3) ? C11 P1 C31 C36 . . . . -66.8(4) ? Mn1 P1 C31 C36 . . . . 61.5(3) ? C36 C31 C32 C33 . . . . -0.1(6) ? P1 C31 C32 C33 . . . . 175.6(3) ? C31 C32 C33 C34 . . . . 0.8(7) ? C32 C33 C34 C35 . . . . -0.5(7) ? C33 C34 C35 C36 . . . . -0.6(7) ? C34 C35 C36 C31 . . . . 1.3(6) ? C32 C31 C36 C35 . . . . -0.9(6) ? P1 C31 C36 C35 . . . . -176.8(3) ? C3S C1S C2S C3S 2_746 . . . 53(2) ? C1S C2S C3S C1S . . . 2_746 -56(2) ?