#------------------------------------------------------------------------------ #$Date: 2024-07-09 05:02:26 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293324 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312538.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_2312538 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 (C8 H10 Br S) (C18 H15 P) (C O)2]' _chemical_formula_moiety 'C28 H25 Br Mn O2 P S3' _chemical_formula_sum 'C28 H25 Br Mn O2 P S3' _chemical_formula_weight 655.48 _chemical_name_systematic Dicarbonyl[\h^5^-2-bromo-1,3,4-tris(methylsulfanyl)cyclopentadienyl](triphenylphosphane-\kP)manganese _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 92.884(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7717(4) _cell_length_b 13.2135(6) _cell_length_c 23.9428(12) _cell_measurement_reflns_used 9839 _cell_measurement_temperature 108(2) _cell_measurement_theta_max 28.2828 _cell_measurement_theta_min 2.7897 _cell_volume 2771.6(2) _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 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0473 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 51088 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.287 _diffrn_reflns_theta_min 2.985 _diffrn_source 'rotating anode generator' _exptl_absorpt_coefficient_mu 2.227 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS2016; Krause et al., 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1328 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.442 _refine_diff_density_min -0.436 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 359 _refine_ls_number_reflns 6886 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0329 _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^)+(0.0155P)^2^+3.2607P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.0712 _reflns_number_gt 5787 _reflns_number_total 6886 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qf3063.cif _cod_data_source_block compd_4 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2312538 _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 0.860 _shelx_estimated_absorpt_t_max 0.957 _shelx_hkl_file ; 1 0 0 -0.21 0.23 1 0 0 -0.37 0.49 1 0 0 -0.14 0.44 2 0 0 89.88 3.88 -2 0 0 95.50 5.24 2 0 0 81.20 4.82 2 0 0 93.06 5.01 -2 0 0 90.99 4.62 -2 0 0 87.73 3.62 2 0 0 80.33 4.67 -3 0 0 9.50 3.03 3 0 0 5.91 2.44 3 0 0 10.54 1.79 -3 0 0 7.80 1.29 3 0 0 10.36 3.10 -3 0 0 8.92 2.69 3 0 0 11.20 3.11 4 0 0 145.14 9.04 4 0 0 129.67 6.52 -4 0 0 139.01 7.66 4 0 0 137.41 8.33 4 0 0 130.11 7.58 -4 0 0 134.63 5.42 4 0 0 150.71 8.06 5 0 0 2.87 2.01 5 0 0 -0.04 2.75 5 0 0 4.67 3.62 5 0 0 0.00 3.87 -5 0 0 0.63 0.78 5 0 0 2.60 3.71 6 0 0 595.06 24.48 6 0 0 617.02 26.32 6 0 0 584.43 25.72 6 0 0 602.10 22.29 6 0 0 615.04 24.26 7 0 0 1.86 3.41 7 0 0 0.25 5.05 7 0 0 -1.25 4.63 7 0 0 5.97 3.12 8 0 0 1182.92 46.24 8 0 0 1143.76 43.22 8 0 0 1096.25 39.99 9 0 0 1.11 3.14 9 0 0 -8.21 7.74 9 0 0 5.90 6.71 10 0 0 187.07 17.79 10 0 0 162.02 14.75 11 0 0 -2.11 7.83 11 0 0 10.10 4.50 11 0 0 -0.12 11.10 2 -1 0 21.54 2.11 -2 -1 0 21.47 2.79 2 -1 0 22.48 2.19 2 -1 0 22.01 2.22 -2 -1 0 14.79 1.63 2 -1 0 25.34 3.20 2 1 0 20.35 2.95 2 1 0 18.50 2.81 2 1 0 20.64 1.99 -2 1 0 14.68 1.74 -2 1 0 19.08 1.98 -2 1 0 19.73 3.15 -3 -1 0 1145.38 37.79 -3 -1 0 1105.54 35.67 3 -1 0 1085.61 36.55 3 -1 0 1192.67 38.12 3 -1 0 1068.62 37.23 3 -1 0 1100.47 36.32 3 1 0 1085.72 38.29 3 1 0 1076.00 36.08 -3 1 0 1102.16 35.90 3 1 0 1129.70 38.48 -3 1 0 1136.48 37.90 3 1 0 1105.94 37.79 4 -1 0 1692.19 56.28 4 -1 0 1688.27 56.82 -4 -1 0 1788.15 55.04 -4 -1 0 1749.24 54.97 4 -1 0 1784.42 57.07 4 -1 0 1790.26 58.76 -4 -1 0 1786.30 58.14 4 1 0 1766.52 59.18 -4 1 0 1645.23 55.23 4 1 0 1828.11 58.46 4 1 0 1812.91 59.37 -4 1 0 1702.66 58.39 4 1 0 1615.97 55.98 4 1 0 1710.65 58.04 5 -1 0 117.05 9.60 -5 -1 0 161.60 5.64 -5 -1 0 148.65 5.55 5 -1 0 156.22 10.00 5 -1 0 150.56 8.86 5 -1 0 156.41 7.93 5 -1 0 161.75 8.71 5 1 0 156.07 7.69 5 1 0 149.84 10.14 5 1 0 134.55 9.37 5 1 0 157.45 9.39 -5 1 0 185.72 10.45 5 1 0 165.39 10.43 -5 1 0 158.45 6.20 6 -1 0 68.54 5.57 6 -1 0 60.15 7.01 6 -1 0 72.30 8.80 6 -1 0 60.92 7.73 6 -1 0 58.05 6.58 6 1 0 69.77 8.15 6 1 0 68.83 8.08 6 1 0 54.21 8.32 6 1 0 52.26 5.04 7 -1 0 599.29 22.68 7 -1 0 560.24 26.73 7 -1 0 572.14 24.03 7 1 0 582.34 25.51 7 1 0 567.99 25.99 7 1 0 641.89 27.92 7 1 0 567.35 22.19 8 -1 0 31.62 5.37 8 -1 0 27.22 7.02 8 -1 0 46.71 7.07 8 -1 0 31.93 8.46 8 1 0 44.23 5.69 8 1 0 40.13 7.77 8 1 0 44.83 9.81 9 -1 0 26.92 4.89 9 -1 0 46.56 10.38 9 1 0 31.21 8.81 9 1 0 30.43 10.32 9 1 0 27.75 5.05 10 -1 0 150.31 11.02 10 -1 0 143.37 13.31 10 -1 0 161.58 17.94 10 1 0 191.07 18.23 10 1 0 123.21 14.52 11 -1 0 -10.54 6.73 11 -1 0 -14.46 8.64 11 -1 0 2.94 4.14 11 1 0 1.82 3.86 11 1 0 7.06 8.26 11 1 0 -7.24 9.60 0 -2 0 537.40 17.91 0 -2 0 545.42 18.49 0 2 0 533.62 18.02 0 2 0 552.43 18.50 1 -2 0 407.14 14.78 -1 -2 0 433.97 14.71 -1 -2 0 424.14 15.08 1 -2 0 416.99 14.80 1 -2 0 408.79 14.28 -1 -2 0 434.39 15.12 1 2 0 441.05 14.81 -1 2 0 407.53 14.74 1 2 0 427.02 14.74 1 2 0 409.06 14.92 -1 2 0 401.39 14.33 1 2 0 421.07 15.10 2 -2 0 2109.56 65.01 -2 -2 0 2056.79 65.82 2 -2 0 2103.77 63.45 -2 -2 0 1925.05 64.47 -2 -2 0 2082.39 66.16 -2 -2 0 1937.05 64.47 2 -2 0 2089.09 63.42 2 -2 0 1850.15 64.88 2 2 0 2021.08 65.84 2 2 0 2044.88 64.71 -2 2 0 1903.87 64.66 -2 2 0 2174.00 66.19 2 2 0 2106.21 66.06 3 -2 0 1618.59 54.83 3 -2 0 1725.03 54.01 -3 -2 0 1678.36 56.29 -3 -2 0 1741.82 54.28 -3 -2 0 1699.73 56.90 3 -2 0 1674.27 53.91 -3 -2 0 1736.75 54.23 3 -2 0 1672.54 55.84 3 2 0 1711.84 56.53 3 2 0 1732.01 54.67 -3 2 0 1677.16 55.79 3 2 0 1666.65 56.66 3 2 0 1699.97 56.81 -3 2 0 1669.90 54.50 4 -2 0 1532.26 50.23 4 -2 0 1657.94 52.75 4 -2 0 1560.62 50.18 -4 -2 0 1489.48 49.35 -4 -2 0 1605.53 49.56 -4 -2 0 1595.22 52.69 4 -2 0 1535.89 50.73 4 2 0 1651.01 53.79 4 2 0 1478.69 50.30 4 2 0 1503.20 53.01 4 2 0 1501.93 52.65 -4 2 0 1462.77 49.79 -4 2 0 1480.41 52.08 -5 -2 0 971.02 36.77 -5 -2 0 1029.15 32.78 -5 -2 0 1016.88 33.63 5 -2 0 1011.12 34.65 5 -2 0 997.04 34.76 5 -2 0 999.59 37.19 5 2 0 1026.21 38.35 -5 2 0 1004.41 33.38 -5 2 0 963.95 36.70 5 2 0 1062.60 37.59 5 2 0 1041.95 38.15 5 2 0 970.55 34.43 5 2 0 1051.69 37.24 6 -2 0 382.44 18.23 6 -2 0 376.59 18.58 6 -2 0 382.81 16.14 6 -2 0 379.37 15.77 6 -2 0 372.16 15.82 6 2 0 394.01 18.59 6 2 0 362.87 17.73 -6 2 0 369.45 18.02 -6 2 0 389.53 13.27 6 2 0 345.89 19.13 6 2 0 359.21 15.27 7 -2 0 83.49 7.17 7 -2 0 91.53 8.31 7 -2 0 79.59 7.11 7 2 0 104.61 11.79 7 2 0 104.46 10.97 7 2 0 77.51 6.61 8 -2 0 26.69 5.41 8 -2 0 15.13 4.54 8 -2 0 30.41 8.20 8 -2 0 7.40 4.72 8 2 0 35.84 8.17 8 2 0 28.81 8.16 8 2 0 16.57 4.06 9 -2 0 40.47 7.43 9 -2 0 27.63 5.52 9 -2 0 33.24 9.47 9 -2 0 30.59 9.72 9 2 0 34.63 5.44 9 2 0 44.22 10.77 9 2 0 22.90 8.50 10 -2 0 10.48 8.69 10 -2 0 -4.13 5.13 10 -2 0 8.31 4.22 10 2 0 11.57 8.16 11 -2 0 -3.17 6.07 11 -2 0 -5.86 8.84 11 -2 0 -3.92 3.93 11 2 0 2.70 9.83 11 2 0 -4.84 9.86 11 2 0 -4.19 3.35 0 -3 0 -1.97 1.55 0 -3 0 -0.31 1.79 0 -3 0 -0.43 1.67 0 -3 0 1.19 1.63 0 3 0 0.47 1.87 0 3 0 0.80 1.55 0 3 0 1.11 1.59 0 3 0 1.50 1.95 -1 -3 0 0.25 0.77 -2 -3 0 2803.47 93.13 2 -3 0 3060.70 92.18 -2 -3 0 2839.20 92.19 2 -3 0 2862.25 92.59 -2 -3 0 2839.30 92.15 -2 -3 0 2917.58 93.45 2 -3 0 2929.31 92.64 2 3 0 2943.21 93.34 2 3 0 2947.90 92.43 -2 3 0 2884.34 92.22 2 3 0 2866.45 93.33 -3 -3 0 592.87 21.41 3 -3 0 622.08 19.79 3 -3 0 599.51 22.28 3 -3 0 618.26 19.81 -3 -3 0 628.78 23.52 -3 -3 0 597.32 21.50 3 -3 0 605.85 22.20 -3 -3 0 606.08 23.65 -3 3 0 617.21 22.42 3 3 0 638.84 21.99 3 3 0 614.86 23.44 -3 3 0 634.15 21.97 3 3 0 595.63 23.53 4 -3 0 18.23 4.28 -4 -3 0 4.38 4.20 4 -3 0 9.81 3.04 -4 -3 0 7.37 2.00 -4 -3 0 9.91 2.23 4 -3 0 8.92 1.95 4 -3 0 9.47 2.13 -4 -3 0 5.61 3.55 4 3 0 8.40 4.14 4 3 0 4.48 4.03 -4 3 0 11.72 3.69 4 3 0 7.21 3.81 -4 3 0 10.58 2.54 4 3 0 8.97 2.56 -5 -3 0 77.92 7.43 -5 -3 0 74.70 4.74 5 -3 0 86.03 6.40 5 -3 0 85.22 7.58 -5 -3 0 74.98 4.54 5 -3 0 79.10 5.15 -5 3 0 72.13 5.15 -5 3 0 71.62 7.82 5 3 0 80.43 7.38 5 3 0 93.25 8.75 5 3 0 78.01 5.95 5 3 0 81.61 9.14 5 3 0 96.28 7.90 6 -3 0 265.67 11.67 6 -3 0 273.20 14.78 6 -3 0 257.55 11.38 6 -3 0 238.40 12.34 6 3 0 260.73 12.06 6 3 0 279.52 15.45 -6 3 0 242.71 10.44 -6 3 0 252.83 14.07 7 -3 0 18.41 4.58 7 -3 0 19.22 6.45 7 -3 0 18.11 4.66 7 -3 0 25.16 4.67 7 3 0 17.37 7.00 7 3 0 21.55 4.37 7 3 0 28.30 8.04 8 -3 0 137.22 9.77 8 -3 0 137.68 10.05 8 -3 0 132.16 9.11 8 -3 0 150.36 13.20 8 3 0 147.00 15.75 8 3 0 154.12 13.66 8 3 0 132.85 9.34 9 -3 0 511.89 27.23 9 -3 0 552.02 23.01 9 -3 0 490.80 22.20 9 -3 0 547.41 22.18 9 3 0 507.56 27.22 9 3 0 471.25 28.10 9 3 0 526.07 21.99 10 -3 0 29.93 7.06 10 -3 0 24.92 9.54 10 -3 0 31.36 6.32 10 3 0 23.06 9.47 10 3 0 27.96 11.01 11 -3 0 49.52 7.49 11 -3 0 43.56 11.80 11 -3 0 55.27 8.18 11 -3 0 45.64 9.23 11 3 0 42.50 13.07 11 3 0 58.63 14.51 11 3 0 43.21 6.89 0 -4 0 664.75 23.86 0 -4 0 664.59 22.99 0 -4 0 653.32 22.78 0 4 0 625.60 23.69 0 4 0 693.78 22.95 0 4 0 643.85 22.93 0 4 0 679.48 23.97 1 -4 0 418.50 16.17 -1 -4 0 408.98 15.88 -1 -4 0 415.77 16.03 1 -4 0 427.21 15.07 -1 -4 0 406.34 15.82 1 -4 0 410.95 16.23 -1 -4 0 401.00 15.89 1 -4 0 407.25 14.05 1 4 0 391.92 15.71 1 4 0 400.91 15.97 -1 4 0 396.31 14.12 -1 4 0 425.17 16.22 1 4 0 428.19 16.18 -1 4 0 422.74 16.21 1 4 0 416.87 16.16 -1 4 0 395.48 14.07 2 -4 0 468.81 18.39 -2 -4 0 480.50 18.94 2 -4 0 489.79 18.30 -2 -4 0 468.05 17.86 -2 -4 0 496.26 18.90 2 -4 0 447.21 18.19 2 4 0 453.45 18.80 -2 4 0 463.56 17.40 2 4 0 462.44 18.17 2 4 0 502.10 18.73 2 4 0 483.03 18.18 -3 -4 0 166.58 8.54 -3 -4 0 172.12 10.04 -3 -4 0 170.22 10.03 3 -4 0 174.16 8.88 3 -4 0 175.74 9.19 3 -4 0 179.19 9.42 -3 -4 0 168.88 8.45 -3 4 0 172.30 8.84 3 4 0 191.16 9.12 -3 4 0 171.77 8.87 3 4 0 179.95 9.83 3 4 0 185.34 10.69 4 -4 0 9.16 1.21 4 -4 0 14.17 3.70 -4 -4 0 12.72 2.66 -4 -4 0 5.71 4.58 -4 -4 0 6.38 2.52 4 -4 0 9.15 1.23 4 -4 0 9.67 3.40 -4 -4 0 6.54 4.76 4 -4 0 13.10 3.72 -4 4 0 11.10 3.89 -4 4 0 10.45 3.01 4 4 0 12.85 3.03 4 4 0 7.16 4.72 4 4 0 9.29 3.78 -5 -4 0 253.04 14.12 5 -4 0 265.68 13.68 -5 -4 0 278.06 11.11 5 -4 0 243.94 9.75 -5 -4 0 275.71 11.27 5 -4 0 236.83 12.39 5 -4 0 256.10 9.85 5 4 0 269.41 15.04 -5 4 0 241.05 11.43 5 4 0 274.18 12.34 5 4 0 259.59 14.33 -5 4 0 263.07 13.22 5 4 0 257.44 16.07 5 4 0 258.48 14.72 6 -4 0 39.04 3.98 6 -4 0 39.64 6.71 -6 -4 0 39.08 3.77 -6 4 0 39.10 4.35 -6 4 0 51.53 7.46 6 4 0 41.53 7.79 6 4 0 54.50 5.92 7 -4 0 7.17 5.95 7 -4 0 -1.51 2.98 7 -4 0 -2.85 3.12 7 -4 0 -3.15 2.55 7 4 0 2.64 4.87 7 4 0 -1.12 5.96 7 4 0 5.20 3.49 8 -4 0 14.41 4.19 8 -4 0 14.44 4.36 8 -4 0 27.85 8.16 8 -4 0 13.96 4.71 8 4 0 11.82 6.78 8 4 0 26.75 8.90 8 4 0 13.85 4.25 9 -4 0 203.69 11.42 9 -4 0 210.73 11.21 9 -4 0 198.65 16.63 9 -4 0 195.13 12.81 9 -4 0 209.41 13.72 9 4 0 194.29 16.99 9 4 0 186.22 11.82 9 4 0 186.82 18.36 10 -4 0 53.71 7.92 10 -4 0 50.14 8.12 10 -4 0 57.40 7.09 10 -4 0 48.50 11.47 10 4 0 68.21 14.15 10 4 0 56.02 12.41 10 4 0 52.41 8.56 11 -4 0 4.25 5.29 11 -4 0 7.71 6.10 11 -4 0 11.32 10.95 11 -4 0 0.57 5.27 11 4 0 7.61 4.69 11 4 0 14.68 11.54 11 4 0 21.82 11.17 0 -5 0 1.57 1.99 0 -5 0 2.61 2.64 0 -5 0 1.57 2.30 0 -5 0 4.82 2.81 0 5 0 3.09 2.72 0 5 0 4.04 2.37 0 5 0 1.27 2.49 0 5 0 3.73 3.00 -1 -5 0 768.83 27.30 1 -5 0 770.00 27.75 -1 -5 0 729.93 27.07 1 -5 0 764.89 26.38 1 -5 0 765.98 27.82 -1 -5 0 773.29 27.66 -1 -5 0 766.84 27.64 -1 5 0 762.72 25.46 1 5 0 723.59 26.99 -1 5 0 765.30 27.79 1 5 0 754.38 27.69 1 5 0 773.67 27.46 -1 5 0 755.50 25.36 -1 5 0 745.65 27.68 1 5 0 760.28 27.71 -1 5 0 728.69 26.24 2 -5 0 352.36 15.41 2 -5 0 338.21 13.99 -2 -5 0 370.79 15.92 2 -5 0 374.36 15.77 -2 -5 0 362.66 15.12 -2 -5 0 383.01 15.89 2 5 0 368.63 15.64 -2 5 0 326.37 15.07 -2 5 0 296.11 13.85 2 5 0 374.03 15.52 2 5 0 404.87 16.39 -2 5 0 355.40 11.89 2 5 0 361.36 15.43 -2 5 0 370.96 12.00 -3 -5 0 1.33 2.41 3 -5 0 5.22 3.06 -3 -5 0 4.70 3.79 -3 -5 0 5.96 2.68 3 -5 0 1.05 2.83 -3 -5 0 2.48 3.92 3 -5 0 0.73 2.94 3 5 0 1.97 3.14 3 5 0 0.19 3.84 3 5 0 0.35 2.60 -3 5 0 5.00 2.55 4 -5 0 70.40 7.09 4 -5 0 64.61 6.76 -4 -5 0 84.74 8.90 4 -5 0 59.04 6.31 -4 -5 0 63.57 7.51 -4 -5 0 60.19 5.23 4 5 0 57.93 7.54 -4 5 0 61.69 6.54 4 5 0 60.17 7.86 -4 5 0 64.01 5.91 4 5 0 53.78 7.18 4 5 0 73.12 6.27 5 -5 0 6.30 3.62 5 -5 0 7.65 3.95 5 -5 0 10.06 4.01 -5 -5 0 17.71 6.48 -5 -5 0 8.21 2.97 -5 5 0 5.88 3.17 5 5 0 10.26 3.58 -5 5 0 13.76 4.31 5 5 0 10.33 5.74 5 5 0 8.55 5.37 6 -5 0 127.81 5.52 6 -5 0 155.60 11.09 -6 -5 0 153.26 7.95 6 -5 0 137.45 5.57 6 -5 0 140.39 10.10 6 -5 0 153.42 10.16 6 5 0 134.03 9.14 -6 5 0 136.58 8.49 6 5 0 140.66 12.62 -6 5 0 152.66 10.32 6 5 0 144.65 12.60 7 -5 0 9.82 5.39 7 -5 0 -0.18 3.71 7 -5 0 0.76 2.03 7 -5 0 5.61 4.30 7 5 0 3.67 3.71 7 5 0 -1.39 7.01 7 5 0 1.11 6.39 8 -5 0 105.50 9.67 8 -5 0 111.27 12.32 8 -5 0 88.71 5.74 8 -5 0 83.19 9.28 8 5 0 85.23 13.27 8 5 0 85.19 12.85 8 5 0 84.73 8.36 9 -5 0 102.54 6.73 9 -5 0 105.96 13.04 9 -5 0 96.98 6.81 9 -5 0 93.36 10.43 9 -5 0 119.61 10.72 9 5 0 106.31 15.86 9 5 0 96.46 9.04 9 5 0 96.84 14.14 10 -5 0 5.35 9.13 10 -5 0 -6.08 3.97 10 -5 0 2.44 3.08 10 -5 0 0.42 5.67 10 5 0 11.46 5.39 10 5 0 -5.47 10.04 10 5 0 12.73 11.32 11 -5 0 8.37 5.63 11 -5 0 -5.83 8.41 11 -5 0 7.72 6.18 11 5 0 3.45 8.03 11 5 0 14.68 10.77 11 5 0 2.60 4.65 0 -6 0 394.97 17.56 0 -6 0 393.37 16.37 0 -6 0 428.64 16.32 0 6 0 433.72 16.61 0 6 0 424.74 16.74 0 6 0 389.21 17.52 0 6 0 419.19 17.90 1 -6 0 51.26 6.13 1 -6 0 51.62 6.24 -1 -6 0 56.65 6.01 -1 -6 0 39.91 5.46 -1 -6 0 47.39 5.92 -1 -6 0 48.25 5.85 1 -6 0 46.51 4.99 1 6 0 51.71 6.05 -1 6 0 49.38 4.58 -1 6 0 43.58 5.67 -1 6 0 51.13 6.06 -1 6 0 48.93 4.47 -1 6 0 48.09 4.04 1 6 0 47.89 6.00 1 6 0 60.53 6.15 1 6 0 59.26 6.39 2 -6 0 8.28 3.61 2 -6 0 6.43 3.80 -2 -6 0 2.94 1.75 -2 -6 0 5.09 3.60 -2 -6 0 4.81 3.62 -2 -6 0 6.76 3.32 2 -6 0 8.47 3.15 -2 6 0 2.93 2.84 -2 6 0 9.45 3.41 2 6 0 8.09 3.49 -2 6 0 5.25 1.59 -2 6 0 9.54 3.74 2 6 0 3.94 3.86 -2 6 0 6.17 1.75 2 6 0 4.14 3.28 2 6 0 9.98 3.53 -3 -6 0 2226.60 73.35 -3 -6 0 2010.57 71.56 3 -6 0 2193.14 70.80 -3 -6 0 2040.45 71.56 3 -6 0 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2.37 3.85 8 -2 -3 1.34 5.63 8 -2 -3 2.67 2.86 8 2 -3 0.84 7.08 8 2 -3 6.66 6.85 8 2 -3 1.44 2.51 7 -2 -3 5.02 4.97 7 -2 -3 5.28 4.37 7 -2 -3 6.16 2.65 7 -2 -3 1.32 3.24 7 2 -3 3.89 6.13 7 2 -3 5.58 5.96 7 2 -3 0.37 2.23 6 -2 -3 36.51 5.57 6 -2 -3 33.69 6.01 6 -2 -3 34.93 6.28 6 -2 -3 23.87 3.38 6 -2 -3 28.05 4.47 6 2 -3 37.83 7.60 6 2 -3 30.41 6.40 6 2 -3 33.68 3.57 6 2 -3 35.67 6.04 -5 -2 3 2017.65 69.85 5 -2 -3 2006.07 68.16 5 -2 -3 1954.50 68.01 5 -2 -3 2047.82 66.55 5 -2 -3 2088.16 66.71 5 -2 -3 1987.27 65.54 5 2 -3 2044.65 69.49 5 2 -3 2051.70 65.06 5 2 -3 2032.91 69.03 5 2 -3 2102.99 70.07 -4 -2 3 496.39 20.56 4 -2 -3 470.14 17.15 4 -2 -3 465.03 18.78 4 -2 -3 476.08 17.67 4 -2 -3 475.39 17.74 4 -2 -3 507.99 18.94 4 -2 -3 477.40 17.15 4 2 -3 476.70 16.64 4 2 -3 503.04 19.87 4 2 -3 482.16 19.88 4 2 -3 468.66 19.80 -3 -2 3 436.12 17.78 3 -2 -3 464.14 17.17 -3 -2 3 435.16 17.28 3 -2 -3 436.76 15.39 3 -2 -3 430.62 15.50 3 -2 -3 429.01 15.34 3 -2 -3 428.89 16.02 3 2 -3 398.45 17.19 3 2 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4 1937.11 61.69 1 -3 4 1892.82 62.98 -1 -3 -4 1817.19 62.97 -1 -3 -4 1889.91 63.03 1 -3 4 1943.97 63.23 -1 3 -4 1909.55 63.09 1 3 4 1929.73 63.17 1 3 4 2152.65 63.40 1 3 4 1954.61 62.45 -1 3 -4 1985.98 63.35 1 3 4 1898.74 62.33 -1 3 -4 1869.00 61.60 -2 -3 -4 111.76 7.35 2 -3 4 120.57 7.28 2 -3 4 121.98 7.35 2 -3 4 113.22 5.35 -2 -3 -4 100.22 6.63 2 3 4 136.77 8.04 -2 3 -4 104.19 5.32 2 3 4 113.90 7.12 -2 3 -4 109.75 7.07 2 3 4 121.73 7.17 2 3 4 118.67 6.82 -2 3 -4 106.85 7.20 3 -3 4 465.50 16.57 3 -3 4 473.71 18.93 -3 -3 -4 439.83 19.23 3 -3 4 488.64 19.41 -3 3 -4 511.70 16.80 3 3 4 469.47 19.67 3 3 4 493.70 19.92 3 3 4 481.62 18.69 -3 3 -4 402.06 18.87 3 3 4 476.70 19.36 4 -3 4 10.07 4.65 -4 -3 -4 8.50 3.16 4 -3 4 8.77 2.59 4 -3 4 13.82 3.75 -4 -3 -4 4.32 3.78 4 3 4 4.65 3.43 -4 3 -4 11.66 2.57 4 3 4 5.39 4.41 4 3 4 5.64 2.98 -4 3 -4 10.03 3.07 -4 3 -4 9.36 3.78 -5 -3 -4 141.53 8.47 5 -3 4 139.73 7.56 5 -3 4 137.43 9.14 -5 -3 -4 125.01 9.69 5 -3 4 116.87 10.13 5 3 4 150.34 10.79 -5 3 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18.94 4.46 3 -4 4 4.90 3.29 3 4 4 3.64 3.51 -3 4 -4 10.09 2.11 3 4 4 8.26 4.20 3 4 4 6.24 2.96 -3 4 -4 3.20 3.47 3 4 4 2.12 3.29 4 -4 4 177.52 7.43 -4 -4 -4 151.34 10.54 4 -4 4 168.69 10.08 -4 -4 -4 163.36 9.60 4 -4 4 183.38 11.00 -4 4 -4 180.03 7.43 4 4 4 184.38 10.78 4 4 4 160.19 11.25 4 4 4 174.63 10.82 4 4 4 153.06 9.65 -4 4 -4 182.15 10.86 -4 4 -4 159.64 9.67 5 -4 4 141.25 7.17 5 -4 4 184.25 11.53 5 -4 4 143.15 9.88 -5 4 -4 143.34 10.29 5 4 4 137.08 10.45 5 4 4 135.46 11.47 -5 4 -4 149.13 9.40 -5 4 -4 152.79 7.20 5 4 4 150.82 9.67 6 -4 4 37.41 4.44 6 -4 4 38.17 6.40 6 -4 4 24.84 6.96 -6 -4 -4 30.95 4.97 6 4 4 27.34 5.42 -6 4 -4 29.33 5.04 6 4 4 53.43 9.30 6 4 4 43.86 8.49 -7 -4 -4 190.24 10.39 7 -4 4 194.75 15.35 7 -4 4 184.82 9.82 7 -4 4 159.77 11.88 7 -4 4 197.90 9.73 -7 4 -4 191.19 10.89 7 4 4 157.84 14.67 7 4 4 177.10 12.81 7 4 4 171.52 14.40 8 -4 4 74.07 11.62 8 -4 4 55.50 6.13 8 -4 4 46.55 5.86 8 -4 4 58.90 8.14 8 4 4 60.53 8.04 8 4 4 80.21 12.11 8 4 4 72.22 11.71 -8 4 -4 40.24 5.37 9 -4 4 64.91 7.27 9 -4 4 60.71 6.90 9 -4 4 53.43 8.74 9 -4 4 76.41 12.25 9 4 4 77.22 13.83 9 4 4 74.94 13.79 9 4 4 73.78 9.23 10 -4 4 368.70 20.45 10 -4 4 348.62 16.85 10 -4 4 330.80 23.97 10 4 4 356.38 19.31 10 4 4 329.74 25.60 10 4 4 385.54 24.55 11 -4 4 14.13 12.13 11 -4 4 11.97 6.72 11 -4 4 7.46 5.35 11 4 4 -0.61 11.51 11 4 4 3.07 4.90 11 4 4 5.01 10.16 11 -5 -4 5.30 5.45 11 -5 -4 9.85 8.87 11 -5 -4 12.07 4.81 11 5 -4 10.89 4.79 11 5 -4 15.12 11.60 11 5 -4 5.16 10.82 10 -5 -4 33.59 6.41 10 -5 -4 20.93 4.86 10 -5 -4 40.63 7.25 10 -5 -4 40.51 9.45 10 5 -4 41.08 5.81 10 5 -4 39.75 12.41 10 5 -4 40.62 12.09 9 -5 -4 -4.50 4.03 9 -5 -4 -2.37 5.85 9 -5 -4 9.59 3.40 9 -5 -4 -3.49 3.71 9 -5 -4 -3.33 3.64 9 5 -4 8.31 9.56 9 5 -4 1.35 4.27 9 5 -4 8.55 7.45 8 -5 -4 18.80 5.18 8 -5 -4 27.35 5.82 8 -5 -4 9.73 3.79 8 -5 -4 15.81 3.56 8 5 -4 15.19 8.65 8 5 -4 18.88 9.37 8 5 -4 15.74 4.16 7 -5 -4 429.37 15.90 7 -5 -4 409.10 16.04 7 -5 -4 416.12 18.60 7 -5 -4 425.89 19.44 7 -5 -4 407.02 18.56 -7 -5 4 404.91 23.47 7 -5 -4 415.22 19.38 7 5 -4 447.23 23.49 7 5 -4 388.88 22.99 7 5 -4 382.85 17.42 6 -5 -4 31.08 3.68 6 -5 -4 33.66 5.61 6 -5 -4 27.08 5.07 6 -5 -4 35.59 6.00 6 -5 -4 31.01 5.54 -6 -5 4 34.06 7.61 6 -5 -4 29.30 5.16 6 5 -4 28.75 7.07 6 5 -4 30.91 4.80 -5 -5 4 1146.31 42.66 5 -5 -4 1067.97 35.70 5 -5 -4 1042.33 38.66 -5 -5 4 1125.38 36.15 5 -5 -4 1080.30 38.81 5 -5 -4 1040.89 37.98 5 -5 -4 1098.62 38.21 5 -5 -4 1121.02 35.74 5 5 -4 1092.13 41.76 5 5 -4 1084.14 38.13 4 -5 -4 232.89 11.78 4 -5 -4 234.06 8.98 -4 -5 4 231.22 10.20 4 -5 -4 256.20 12.07 4 -5 -4 217.16 10.23 -4 -5 4 216.13 10.12 -4 -5 4 218.35 13.68 -4 5 4 232.54 8.98 -4 5 4 239.48 10.45 4 5 -4 221.14 11.25 4 5 -4 249.01 11.56 4 5 -4 223.08 13.06 4 5 -4 238.41 13.68 4 5 -4 237.62 13.27 3 -5 -4 81.69 6.55 3 -5 -4 72.76 4.37 3 -5 -4 74.35 4.57 -3 -5 4 80.45 8.40 3 -5 -4 77.09 6.59 -3 -5 4 60.04 7.94 -3 -5 4 75.44 5.67 3 5 -4 74.86 8.20 3 5 -4 75.79 8.57 3 5 -4 77.15 6.28 -3 5 4 78.29 4.42 3 5 -4 69.98 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10 -6 -4 121.48 13.61 10 6 -4 128.69 17.44 10 6 -4 117.28 9.89 10 6 -4 89.21 16.02 9 -6 -4 324.37 19.93 9 -6 -4 340.47 17.75 9 -6 -4 350.16 19.40 9 -6 -4 298.65 11.69 9 6 -4 349.21 23.70 9 6 -4 344.33 16.50 8 -6 -4 -0.48 4.35 8 -6 -4 3.14 2.21 8 -6 -4 4.47 5.60 8 -6 -4 2.70 2.01 8 -6 -4 6.49 4.45 8 6 -4 1.40 8.16 8 6 -4 -11.20 7.27 8 6 -4 1.94 3.84 7 -6 -4 313.12 16.14 7 -6 -4 291.28 10.77 7 -6 -4 293.18 15.56 7 -6 -4 304.66 16.08 7 -6 -4 321.69 10.93 -7 -6 4 314.34 20.72 7 -6 -4 305.15 15.81 7 6 -4 282.71 14.89 7 6 -4 315.92 20.34 6 -6 -4 198.45 12.45 -6 -6 4 195.11 8.88 6 -6 -4 231.64 7.93 6 -6 -4 224.44 12.90 6 -6 -4 222.49 7.84 -6 -6 4 195.99 15.60 6 -6 -4 220.90 11.92 6 -6 -4 227.85 12.03 6 6 -4 236.21 16.32 6 6 -4 202.54 11.91 5 -6 -4 43.39 5.45 5 -6 -4 41.97 2.60 5 -6 -4 45.18 2.55 5 -6 -4 44.73 6.29 5 -6 -4 34.21 5.82 -5 -6 4 34.40 7.79 -5 -6 4 45.33 4.76 5 6 -4 48.73 8.51 -5 6 4 47.58 5.60 4 -6 -4 536.29 22.77 4 -6 -4 534.06 22.93 -4 -6 4 562.22 25.19 4 -6 -4 564.46 18.70 -4 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11 103.55 11.77 8 2 11 95.75 12.86 -8 2 -11 96.18 10.57 9 -2 11 24.90 7.24 9 -2 11 32.12 8.11 9 -2 11 15.37 8.60 9 2 11 9.45 9.35 -9 2 -11 14.07 7.21 9 2 11 32.99 7.81 9 2 11 10.00 10.53 10 -2 11 8.71 10.88 10 -2 11 7.87 7.16 10 -2 11 16.88 7.62 10 2 11 8.68 11.35 10 2 11 30.85 12.92 10 2 11 7.92 7.44 10 -3 -11 5.70 7.10 10 -3 -11 -5.28 6.15 10 3 -11 2.85 8.43 10 3 -11 13.35 11.47 9 -3 -11 63.76 9.94 9 -3 -11 72.75 5.33 9 -3 -11 85.32 10.44 9 -3 -11 69.29 5.14 9 3 -11 61.63 11.98 9 3 -11 88.89 14.02 8 -3 -11 55.83 5.27 8 -3 -11 53.81 5.17 8 -3 -11 50.44 8.39 8 -3 -11 45.59 9.28 -8 -3 11 77.02 12.13 8 3 -11 52.63 10.56 7 -3 -11 0.77 3.60 -7 -3 11 0.03 6.14 7 -3 -11 2.88 2.70 7 -3 -11 4.99 3.99 7 -3 -11 0.78 2.38 7 -3 -11 -1.86 3.72 -7 -3 11 -5.03 6.16 -7 3 11 1.07 4.83 7 3 -11 2.37 2.09 7 3 -11 0.28 6.16 6 -3 -11 1976.26 67.30 6 -3 -11 2015.73 67.78 -6 -3 11 2079.04 72.40 6 -3 -11 1937.48 68.54 6 -3 -11 2010.14 66.30 6 -3 -11 2018.24 66.35 -6 -3 11 2059.74 72.21 6 3 -11 1995.02 65.41 -6 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4 5 14 12.57 7.47 -4 5 -14 15.08 5.17 4 5 14 4.74 6.28 5 -5 14 81.30 10.91 5 -5 14 97.32 9.29 5 -5 14 70.04 11.58 -5 -5 -14 88.18 11.14 5 5 14 88.13 12.29 5 5 14 70.97 11.56 -5 5 -14 90.19 11.24 5 5 14 88.55 10.88 -5 5 -14 84.10 8.95 6 -5 14 108.96 10.21 6 -5 14 80.18 11.67 6 -5 14 118.06 14.47 -6 5 -14 109.18 12.23 6 5 14 106.77 14.48 6 5 14 80.93 12.82 6 5 14 98.40 12.20 -6 5 -14 85.98 9.46 7 -5 14 85.39 14.20 -7 -5 -14 78.74 11.02 7 -5 14 95.36 12.83 7 -5 14 112.27 10.38 7 5 14 124.71 12.21 7 5 14 96.21 15.02 7 5 14 98.42 14.35 8 -5 14 173.74 19.23 8 -5 14 191.98 13.17 -8 -5 -14 161.40 15.57 8 -5 14 175.57 16.74 8 5 14 133.23 15.28 -8 5 -14 158.07 15.61 8 5 14 159.83 19.38 8 5 14 135.88 17.79 9 -5 14 32.83 12.40 9 -5 14 42.18 7.69 9 5 14 33.74 12.63 9 5 14 13.31 11.63 9 -6 -14 118.08 10.16 9 -6 -14 130.25 16.91 9 -6 -14 101.51 9.04 9 -6 -14 105.52 9.85 -9 -6 14 110.23 17.25 9 6 -14 138.90 17.34 8 -6 -14 103.81 9.85 8 -6 -14 119.76 7.62 8 -6 -14 99.63 7.56 -8 -6 14 98.53 14.74 8 -6 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-30 46.30 11.58 4 1 -30 70.79 13.00 -4 1 30 47.36 14.77 -4 1 30 40.85 9.61 -3 -1 30 19.81 12.02 3 -1 -30 -11.03 7.12 -3 -1 30 1.85 8.67 -3 1 30 28.78 12.57 3 1 -30 -6.88 7.69 -3 1 30 -1.66 7.54 2 -1 -30 16.40 9.77 -2 -1 30 11.21 11.07 -2 -1 30 9.41 9.73 -2 1 30 22.72 10.11 -2 1 30 4.80 7.56 2 1 -30 15.54 9.88 1 -1 -30 6.49 9.33 -1 -1 30 18.84 11.92 -1 -1 30 22.84 10.06 1 1 -30 21.12 10.66 -1 1 30 28.79 9.16 -1 1 30 38.84 13.27 0 -1 -30 88.23 15.25 0 -1 30 70.60 13.60 0 -1 30 100.61 17.92 0 1 30 59.46 14.54 0 1 -30 76.24 14.13 0 1 30 92.91 13.20 1 -1 30 17.29 9.27 -1 -1 -30 15.95 10.84 1 -1 30 9.41 10.56 1 1 30 19.04 10.17 -1 1 -30 26.71 11.17 1 1 30 31.00 12.45 2 -1 30 45.64 13.70 -2 -1 -30 54.75 13.17 2 -1 30 58.40 14.21 2 1 30 74.84 15.44 2 1 30 62.25 13.11 -2 1 -30 59.21 13.99 -3 -1 -30 11.87 9.76 3 -1 30 4.39 9.97 3 -1 30 38.54 12.41 -3 1 -30 7.44 9.61 3 1 30 -8.97 8.83 3 1 30 -0.87 11.16 4 -2 -30 11.58 9.14 -4 -2 30 26.28 13.57 -4 2 30 0.20 11.21 4 2 -30 35.13 10.24 -4 2 30 16.04 7.44 3 -2 -30 107.83 15.50 -3 -2 30 116.39 17.92 -3 -2 30 96.37 14.46 3 2 -30 104.35 15.00 -3 2 30 110.34 18.25 -3 2 30 132.65 12.61 2 -2 -30 116.97 16.17 -2 -2 30 117.68 18.08 -2 -2 30 137.25 18.42 -2 2 30 121.18 17.50 -2 2 30 148.72 13.48 2 2 -30 114.33 16.50 1 -2 -30 2.03 8.85 -1 -2 30 6.83 9.66 1 2 -30 5.89 9.33 -1 2 30 5.84 7.76 -1 2 30 -9.74 9.46 0 -2 30 2.83 10.19 0 -2 30 3.29 8.65 0 -2 -30 13.58 10.04 0 2 -30 2.91 9.06 0 2 30 -2.17 7.47 0 2 30 16.23 11.47 -1 -2 -30 2.79 9.92 1 -2 30 -13.11 7.75 1 -2 30 10.13 12.20 1 2 30 15.14 11.21 1 2 30 18.57 9.14 -1 2 -30 7.93 9.69 -2 -2 -30 11.31 10.74 2 -2 30 12.57 10.86 2 -2 30 14.18 10.90 2 2 30 6.46 11.94 -2 2 -30 6.53 9.31 3 -2 30 7.67 11.37 3 -2 30 6.12 10.95 -3 -2 -30 23.30 11.79 -3 2 -30 10.23 10.57 3 2 30 1.73 9.19 3 2 30 7.33 12.09 4 -3 -30 34.91 11.15 -4 -3 30 19.21 10.72 4 3 -30 32.71 10.07 -4 3 30 24.18 7.22 -3 -3 30 185.98 18.26 3 -3 -30 199.59 19.26 -3 -3 30 237.58 22.77 -3 3 30 198.49 21.75 -3 3 30 203.33 14.88 3 3 -30 247.86 19.98 2 -3 -30 14.14 9.56 -2 -3 30 2.28 11.79 -2 -3 30 25.60 10.44 -2 3 30 25.19 7.74 -2 3 30 18.27 11.71 2 3 -30 17.41 10.27 -1 -3 30 105.01 17.57 1 -3 -30 75.74 14.36 -1 -3 30 89.33 14.63 -1 3 30 87.01 11.53 -1 3 30 80.23 15.44 1 3 -30 73.71 13.77 0 -3 30 70.79 15.00 0 -3 30 113.17 16.50 0 -3 -30 80.00 14.42 0 3 -30 94.84 15.89 0 3 30 77.52 11.99 0 3 30 90.27 16.26 1 -3 30 20.43 12.31 1 -3 30 2.27 10.71 -2 -3 -30 92.93 16.93 2 -3 30 96.33 15.77 2 -3 30 67.40 14.84 2 3 30 91.23 16.73 2 3 30 86.53 13.87 -2 3 -30 79.60 15.19 3 -4 -30 14.39 9.60 -3 -4 30 4.07 9.81 -3 -4 30 10.77 11.49 3 4 -30 12.41 9.80 -3 4 30 28.31 12.60 -3 4 30 13.78 7.09 2 -4 -30 15.93 10.22 -2 -4 30 15.90 12.46 -2 -4 30 20.98 10.55 2 4 -30 27.16 11.24 -2 4 30 33.38 7.89 -2 4 30 31.11 12.85 -1 -4 30 32.62 12.03 -1 -4 30 38.01 13.11 1 -4 -30 19.25 10.52 1 4 -30 48.17 12.62 -1 4 30 35.36 12.40 -1 4 30 37.24 8.66 0 -4 30 13.00 11.84 0 -4 -30 10.65 10.43 0 -4 30 -4.40 9.74 0 4 30 -0.73 10.79 0 4 -30 4.05 9.80 0 4 30 10.77 7.27 1 -4 30 7.85 11.59 1 -4 30 0.66 10.12 1 4 30 -0.29 10.67 1 4 30 -4.90 8.07 -1 4 -30 1.30 12.57 2 -4 30 99.42 16.80 -2 -4 -30 120.04 17.55 2 -4 30 135.20 18.10 2 4 30 101.24 14.16 2 4 30 90.96 17.01 -2 4 -30 118.07 18.18 -2 -5 30 88.16 15.91 2 -5 -30 85.11 15.10 -2 -5 30 89.77 15.63 -2 5 30 91.64 9.95 -2 5 30 90.18 16.78 2 5 -30 72.42 14.50 1 -5 -30 73.95 13.81 -1 -5 30 70.15 14.09 -1 -5 30 31.66 12.79 -1 5 30 89.57 16.34 1 5 -30 61.51 13.75 -1 5 30 59.23 9.07 0 -5 30 14.41 11.47 0 -5 30 -8.39 8.39 0 -5 -30 -3.54 9.42 0 5 -30 0.20 9.62 0 5 30 -5.46 6.65 0 5 30 -3.77 11.70 1 -5 30 105.70 17.09 -1 -5 -30 121.05 18.18 1 5 30 130.63 18.77 -1 5 -30 128.70 18.00 1 5 30 92.99 12.74 -3 0 31 109.93 17.97 3 0 -31 69.68 13.40 -3 0 31 81.33 12.91 -2 0 31 -17.69 10.45 2 0 -31 7.78 8.98 -2 0 31 -0.03 9.00 1 0 -31 31.61 11.27 -1 0 31 34.43 9.95 -1 0 31 33.06 10.75 0 0 -31 23.40 11.25 0 0 31 10.30 12.29 1 0 31 12.85 9.42 -1 0 -31 9.45 11.02 1 0 31 9.22 11.61 -2 0 -31 -9.22 9.42 2 0 31 -8.02 9.25 2 0 31 8.59 11.60 -3 -1 31 3.38 11.51 3 -1 -31 17.15 10.00 -3 -1 31 16.78 8.59 3 1 -31 18.73 10.03 -3 1 31 8.71 11.70 -3 1 31 4.14 7.96 -2 -1 31 7.00 9.01 2 -1 -31 -12.95 7.79 -2 -1 31 5.97 10.94 -2 1 31 1.23 10.82 -2 1 31 18.37 8.74 2 1 -31 0.80 9.05 -1 -1 31 -4.73 10.40 1 -1 -31 1.92 9.28 1 1 -31 4.34 9.58 -1 1 31 12.91 10.89 -1 1 31 -1.00 8.40 0 -1 31 32.67 13.17 0 -1 31 0.99 8.99 0 -1 -31 27.88 12.24 0 1 31 6.34 9.12 0 1 31 15.83 12.37 0 1 -31 -1.96 8.91 1 -1 31 45.21 14.45 -1 -1 -31 43.20 13.22 1 -1 31 50.31 12.32 1 1 31 64.06 11.96 1 1 31 71.72 15.40 -1 1 -31 63.80 15.03 2 -1 31 47.16 14.19 2 -1 31 59.33 14.02 -2 -1 -31 50.86 13.16 2 1 31 54.31 14.90 -2 1 -31 65.83 14.63 2 1 31 44.71 13.06 -3 -2 31 130.39 16.21 3 -2 -31 125.26 16.43 3 2 -31 143.25 17.56 -3 2 31 98.82 11.97 2 -2 -31 9.99 9.25 -2 -2 31 -5.14 11.22 -2 -2 31 -6.50 9.44 -2 2 31 -0.80 11.70 -2 2 31 3.99 7.61 2 2 -31 1.67 9.45 -1 -2 31 29.35 10.64 1 -2 -31 13.00 10.35 -1 -2 31 20.92 12.38 1 2 -31 22.86 11.21 -1 2 31 17.55 12.26 -1 2 31 33.40 9.63 0 -2 -31 38.51 12.61 0 -2 31 18.90 12.45 0 -2 31 29.44 11.11 0 2 31 17.76 7.86 0 2 31 14.85 9.62 0 2 -31 12.77 10.84 -1 -2 -31 156.37 19.43 1 -2 31 149.36 17.92 1 -2 31 167.62 21.36 -1 2 -31 170.68 20.82 1 2 31 170.53 16.72 1 2 31 143.56 19.72 -2 -3 31 120.35 18.65 2 -3 -31 132.17 17.23 -2 -3 31 127.11 16.65 -2 3 31 137.83 13.52 -2 3 31 115.84 17.86 2 3 -31 88.80 15.25 1 -3 -31 12.32 9.83 -1 -3 31 -8.77 8.79 -1 -3 31 5.20 10.92 1 3 -31 -2.79 9.15 -1 3 31 5.11 8.33 -1 3 31 5.52 11.18 0 -3 31 -10.22 9.90 0 -3 -31 8.39 10.15 0 -3 31 -0.25 9.77 0 3 31 -6.88 6.84 0 3 31 8.36 11.20 0 3 -31 0.76 9.34 1 -3 31 20.81 11.70 -1 -3 -31 35.46 11.95 1 -3 31 31.19 13.32 1 3 31 30.12 12.59 1 3 31 23.60 10.33 -1 3 -31 35.44 12.06 -1 -4 31 14.78 10.21 -1 -4 31 19.74 12.53 1 -4 -31 9.91 9.01 -1 4 31 27.27 13.30 -1 4 31 5.95 6.99 1 4 -31 24.80 11.37 0 -4 31 83.43 16.37 0 -4 31 68.49 13.99 0 -4 -31 93.71 16.18 0 4 31 81.48 12.50 0 4 -31 94.10 16.25 0 4 31 113.36 17.43 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 0.6759 _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 0.71076 8.772 13.214 23.937 89.993 92.886 89.999 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 69620 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 08:43:49 on 20-Jan-2023 CELL 0.71073 8.7717 13.2135 23.9428 90.000 92.884 90.000 ZERR 4.00 0.0004 0.0006 0.0012 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H BR O P S MN UNIT 112 100 4 8 4 12 4 MERG 2 OMIT 1 3 0 OMIT 1 0 1 OMIT -1 0 1 OMIT 0 1 2 OMIT 1 1 1 OMIT 1 0 3 SADI 1.87 C1 BR1A C2 BR1B SADI 1.77 C1 S2B C2 S2A C3 S3 C5 S5 SADI S2A C21A S2B C21B S3 C31 S5 C51 FMAP 2 PLAN 5 TEMP -165 SIZE 0.07 0.03 0.02 BOND $H ACTA CONF LIST 4 L.S. 16 WGHT 0.015500 3.260700 FVAR 0.34842 0.76105 0.18896 0.02386 0.03884 C1 1 0.258593 0.121519 0.413532 11.00000 0.02399 0.01610 = 0.02744 0.00275 -0.00011 -0.00415 C2 1 0.271268 0.144984 0.472059 11.00000 0.02861 0.02133 = 0.02302 0.00799 0.00404 -0.00235 C3 1 0.404694 0.205369 0.481057 11.00000 0.02689 0.02292 = 0.02043 0.00704 -0.00179 -0.00056 C4 1 0.466783 0.224779 0.428267 11.00000 0.02102 0.01834 = 0.02401 0.00494 -0.00031 -0.00154 AFIX 43 H4 2 0.551531 0.267237 0.421846 11.00000 -1.20000 AFIX 0 C5 1 0.379435 0.169293 0.386679 11.00000 0.02469 0.01653 = 0.02326 0.00286 0.00328 0.00080 C6 1 0.032136 0.278999 0.427250 11.00000 0.02809 0.02061 = 0.02278 0.00216 0.00547 -0.00489 C7 1 0.249479 0.387434 0.472586 11.00000 0.02636 0.02421 = 0.01571 0.00566 0.00244 -0.00281 C31 1 0.624605 0.326005 0.529879 11.00000 0.03647 0.05505 = 0.03503 -0.00615 -0.00972 -0.01376 AFIX 137 H31A 2 0.702148 0.290705 0.509154 11.00000 -1.50000 H31B 2 0.672121 0.354909 0.564201 11.00000 -1.50000 H31C 2 0.579318 0.380350 0.506657 11.00000 -1.50000 AFIX 0 C51 1 0.621999 0.167385 0.317770 11.00000 0.03295 0.04971 = 0.04417 0.00461 0.01428 0.00861 AFIX 137 H51A 2 0.649496 0.235749 0.330551 11.00000 -1.50000 H51B 2 0.658374 0.156684 0.280187 11.00000 -1.50000 H51C 2 0.669327 0.117534 0.343513 11.00000 -1.50000 AFIX 0 C101 1 0.420741 0.414264 0.327604 11.00000 0.01577 0.01687 = 0.02003 0.00387 0.00191 0.00041 C102 1 0.524209 0.456695 0.367234 11.00000 0.01980 0.02847 = 0.02200 0.00370 0.00074 -0.00304 AFIX 43 H102 2 0.492976 0.469438 0.403999 11.00000 -1.20000 AFIX 0 C103 1 0.671568 0.480441 0.353718 11.00000 0.01708 0.03535 = 0.03552 0.00728 -0.00478 -0.00561 AFIX 43 H103 2 0.740373 0.509754 0.381040 11.00000 -1.20000 AFIX 0 C104 1 0.718635 0.461522 0.300493 11.00000 0.01564 0.03399 = 0.04210 0.01053 0.00714 0.00130 AFIX 43 H104 2 0.820402 0.476476 0.291429 11.00000 -1.20000 AFIX 0 C105 1 0.617691 0.420920 0.260578 11.00000 0.02644 0.03146 = 0.02973 0.00335 0.01365 0.00426 AFIX 43 H105 2 0.649759 0.408754 0.223865 11.00000 -1.20000 AFIX 0 C106 1 0.468799 0.397627 0.273821 11.00000 0.02242 0.02429 = 0.02443 -0.00163 0.00434 -0.00044 AFIX 43 H106 2 0.399669 0.370227 0.245978 11.00000 -1.20000 AFIX 0 C201 1 0.157884 0.515215 0.359742 11.00000 0.01505 0.01906 = 0.01659 -0.00050 -0.00263 -0.00253 C202 1 0.044230 0.537249 0.396845 11.00000 0.01551 0.02454 = 0.02221 0.00004 0.00137 -0.00434 AFIX 43 H202 2 0.004787 0.484805 0.419103 11.00000 -1.20000 AFIX 0 C203 1 -0.011436 0.635139 0.401418 11.00000 0.02109 0.02889 = 0.03394 -0.00196 0.00625 0.00226 AFIX 43 H203 2 -0.088849 0.649088 0.426688 11.00000 -1.20000 AFIX 0 C204 1 0.044982 0.712443 0.369462 11.00000 0.03612 0.02289 = 0.04340 0.00390 0.00791 0.00820 AFIX 43 H204 2 0.006226 0.779235 0.372560 11.00000 -1.20000 AFIX 0 C205 1 0.158488 0.691778 0.332878 11.00000 0.03624 0.02308 = 0.03137 0.00916 0.00604 0.00060 AFIX 43 H205 2 0.198447 0.744730 0.311108 11.00000 -1.20000 AFIX 0 C206 1 0.213713 0.594456 0.327962 11.00000 0.02198 0.02570 = 0.01964 0.00377 0.00302 0.00095 AFIX 43 H206 2 0.290989 0.581164 0.302534 11.00000 -1.20000 AFIX 0 C301 1 0.118664 0.342622 0.288814 11.00000 0.01636 0.02089 = 0.01603 -0.00186 0.00094 -0.00010 C302 1 0.096579 0.403262 0.241467 11.00000 0.02411 0.02455 = 0.01796 -0.00156 -0.00088 0.00165 AFIX 43 H302 2 0.142408 0.468354 0.240665 11.00000 -1.20000 AFIX 0 C303 1 0.007739 0.369248 0.195208 11.00000 0.03009 0.03772 = 0.01648 -0.00228 -0.00245 0.00541 AFIX 43 H303 2 -0.007245 0.411379 0.163251 11.00000 -1.20000 AFIX 0 C304 1 -0.058463 0.274317 0.195848 11.00000 0.02221 0.04307 = 0.01959 -0.01235 -0.00074 -0.00019 AFIX 43 H304 2 -0.118561 0.250991 0.164325 11.00000 -1.20000 AFIX 0 C305 1 -0.036849 0.213530 0.242521 11.00000 0.02407 0.03047 = 0.02687 -0.00968 0.00423 -0.00840 AFIX 43 H305 2 -0.081821 0.148147 0.242939 11.00000 -1.20000 AFIX 0 C306 1 0.050339 0.247485 0.288887 11.00000 0.02043 0.02523 = 0.02000 -0.00164 0.00248 -0.00329 AFIX 43 H306 2 0.063433 0.205378 0.320930 11.00000 -1.20000 AFIX 0 O1 4 -0.098727 0.273240 0.428573 11.00000 0.02335 0.03793 = 0.05098 0.00559 0.00987 -0.00587 O2 4 0.261163 0.452721 0.504919 11.00000 0.04933 0.02711 = 0.02116 -0.00336 0.00126 -0.00615 P1 5 0.230447 0.385304 0.351584 11.00000 0.01476 0.01723 = 0.01330 0.00045 0.00064 -0.00280 S3 6 0.478234 0.238021 0.547542 11.00000 0.04469 0.04188 = 0.01973 0.00819 -0.00765 -0.00539 S5 6 0.417196 0.152996 0.316034 11.00000 0.03455 0.02551 = 0.02699 -0.00730 0.00885 -0.00410 MN1 7 0.235787 0.282057 0.426715 11.00000 0.01927 0.01714 = 0.01465 0.00208 0.00220 -0.00385 PART 1 21 BR1A 3 0.125815 0.023779 0.378394 21.00000 0.03437 0.02017 = 0.03108 -0.00320 0.00108 -0.01186 S2A 6 0.156653 0.093540 0.523858 21.00000 0.02722 0.02312 = 0.03168 0.00964 0.00750 -0.00411 C21A 1 0.253081 -0.026683 0.534313 21.00000 0.04875 0.02855 = 0.04473 0.01926 0.00806 -0.00001 AFIX 137 H21A 2 0.252379 -0.063535 0.498781 21.00000 -1.50000 H21B 2 0.200261 -0.066734 0.561858 21.00000 -1.50000 H21C 2 0.358780 -0.014831 0.547959 21.00000 -1.50000 PART 2 -21 AFIX 0 BR1B 3 0.159075 0.100114 0.532703 -21.00000 0.06861 0.03151 = 0.05011 0.01085 0.02470 -0.00718 S2B 6 0.130809 0.036516 0.391267 -21.00000 0.04536 0.02184 = 0.04057 -0.00855 0.00161 -0.01503 C21B 1 0.223716 -0.077258 0.415592 -21.00000 0.03946 0.02623 = 0.07095 0.00142 0.00772 0.00323 AFIX 33 H21D 2 0.159721 -0.135744 0.405178 -21.00000 -1.50000 H21E 2 0.322487 -0.083621 0.398520 -21.00000 -1.50000 H21F 2 0.239714 -0.074587 0.456370 -21.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.0712, GooF = S = 1.104, Restrained GooF = 1.103 for all data REM R1 = 0.0329 for 5787 Fo > 4sig(Fo) and 0.0448 for all 6886 data REM 359 parameters refined using 13 restraints END WGHT 0.0155 3.2633 REM Highest difference peak 0.442, deepest hole -0.436, 1-sigma level 0.065 Q1 1 0.3371 0.4016 0.3373 11.00000 0.05 0.44 Q2 1 0.4580 0.4575 0.3456 11.00000 0.05 0.36 Q3 1 0.1770 0.4567 0.3564 11.00000 0.05 0.35 Q4 1 0.4244 0.2001 0.4094 11.00000 0.05 0.34 Q5 1 0.1799 0.3644 0.3155 11.00000 0.05 0.33 ; _shelx_res_checksum 38930 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 C C1 0.2586(2) 0.12152(16) 0.41353(10) 0.0226(4) Uani d 1 . . C C2 0.2713(3) 0.14498(17) 0.47206(9) 0.0242(5) Uani d 1 . . C C3 0.4047(3) 0.20537(17) 0.48106(9) 0.0235(5) Uani d 1 . . C C4 0.4668(2) 0.22478(16) 0.42827(9) 0.0212(4) Uani d 1 . . H H4 0.551531 0.267237 0.421846 0.025 Uiso calc 1 . . C C5 0.3794(2) 0.16929(16) 0.38668(9) 0.0214(4) Uani d 1 . . C C6 0.0321(3) 0.27900(17) 0.42725(9) 0.0237(5) Uani d 1 . . C C7 0.2495(2) 0.38743(17) 0.47259(9) 0.0220(4) Uani d 1 . . C C31 0.6246(3) 0.3260(2) 0.52988(12) 0.0426(7) Uani d 1 . . H H31A 0.702148 0.290705 0.509154 0.064 Uiso calc 1 . . H H31B 0.672121 0.354909 0.564201 0.064 Uiso calc 1 . . H H31C 0.579318 0.380350 0.506657 0.064 Uiso calc 1 . . C C51 0.6220(3) 0.1674(2) 0.31777(12) 0.0419(7) Uani d 1 . . H H51A 0.649496 0.235749 0.330551 0.063 Uiso calc 1 . . H H51B 0.658374 0.156684 0.280187 0.063 Uiso calc 1 . . H H51C 0.669327 0.117534 0.343513 0.063 Uiso calc 1 . . C C101 0.4207(2) 0.41426(15) 0.32760(9) 0.0175(4) Uani d 1 . . C C102 0.5242(2) 0.45669(17) 0.36723(10) 0.0234(5) Uani d 1 . . H H102 0.492976 0.469438 0.403999 0.028 Uiso calc 1 . . C C103 0.6716(3) 0.48044(19) 0.35372(11) 0.0295(5) Uani d 1 . . H H103 0.740373 0.509754 0.381040 0.035 Uiso calc 1 . . C C104 0.7186(3) 0.46152(19) 0.30049(11) 0.0304(5) Uani d 1 . . H H104 0.820402 0.476476 0.291429 0.036 Uiso calc 1 . . C C105 0.6177(3) 0.42092(18) 0.26058(10) 0.0288(5) Uani d 1 . . H H105 0.649759 0.408754 0.223865 0.035 Uiso calc 1 . . C C106 0.4688(2) 0.39763(17) 0.27382(10) 0.0236(5) Uani d 1 . . H H106 0.399669 0.370227 0.245978 0.028 Uiso calc 1 . . C C201 0.1579(2) 0.51522(15) 0.35974(8) 0.0170(4) Uani d 1 . . C C202 0.0442(2) 0.53725(16) 0.39684(9) 0.0207(4) Uani d 1 . . H H202 0.004787 0.484805 0.419103 0.025 Uiso calc 1 . . C C203 -0.0114(3) 0.63514(18) 0.40142(10) 0.0278(5) Uani d 1 . . H H203 -0.088849 0.649088 0.426688 0.033 Uiso calc 1 . . C C204 0.0450(3) 0.71244(19) 0.36946(11) 0.0339(6) Uani d 1 . . H H204 0.006226 0.779235 0.372560 0.041 Uiso calc 1 . . C C205 0.1585(3) 0.69178(18) 0.33288(10) 0.0301(5) Uani d 1 . . H H205 0.198447 0.744730 0.311108 0.036 Uiso calc 1 . . C C206 0.2137(2) 0.59446(17) 0.32796(9) 0.0224(4) Uani d 1 . . H H206 0.290989 0.581164 0.302534 0.027 Uiso calc 1 . . C C301 0.1187(2) 0.34262(16) 0.28881(8) 0.0178(4) Uani d 1 . . C C302 0.0966(2) 0.40326(17) 0.24147(9) 0.0223(4) Uani d 1 . . H H302 0.142408 0.468354 0.240665 0.027 Uiso calc 1 . . C C303 0.0077(3) 0.36925(19) 0.19521(10) 0.0282(5) Uani d 1 . . H H303 -0.007245 0.411379 0.163251 0.034 Uiso calc 1 . . C C304 -0.0585(3) 0.27432(19) 0.19585(10) 0.0284(5) Uani d 1 . . H H304 -0.118561 0.250991 0.164325 0.034 Uiso calc 1 . . C C305 -0.0368(3) 0.21353(19) 0.24252(10) 0.0270(5) Uani d 1 . . H H305 -0.081821 0.148147 0.242939 0.032 Uiso calc 1 . . C C306 0.0503(2) 0.24749(17) 0.28889(9) 0.0218(4) Uani d 1 . . H H306 0.063433 0.205378 0.320930 0.026 Uiso calc 1 . . O O1 -0.09873(19) 0.27324(14) 0.42857(8) 0.0372(4) Uani d 1 . . O O2 0.2612(2) 0.45272(13) 0.50492(7) 0.0326(4) Uani d 1 . . P P1 0.23045(6) 0.38530(4) 0.35158(2) 0.01510(11) Uani d 1 . . S S3 0.47823(8) 0.23802(5) 0.54754(3) 0.03575(15) Uani d 1 . . S S5 0.41720(7) 0.15300(5) 0.31603(3) 0.02877(13) Uani d 1 . . Mn Mn1 0.23579(4) 0.28206(2) 0.42672(2) 0.01697(8) Uani d 1 . . Br Br1A 0.1258(2) 0.02378(11) 0.37839(6) 0.0286(2) Uani d 0.7611(16) A 1 S S2A 0.1567(3) 0.0935(3) 0.5239(2) 0.0271(4) Uani d 0.7611(16) A 1 C C21A 0.2531(4) -0.0267(3) 0.53431(16) 0.0405(9) Uani d 0.7611(16) A 1 H H21A 0.252379 -0.063535 0.498781 0.061 Uiso calc 0.7611(16) A 1 H H21B 0.200261 -0.066734 0.561858 0.061 Uiso calc 0.7611(16) A 1 H H21C 0.358780 -0.014831 0.547959 0.061 Uiso calc 0.7611(16) A 1 Br Br1B 0.1591(6) 0.1001(5) 0.5327(3) 0.0493(18) Uani d 0.2389(16) A 2 S S2B 0.131(2) 0.0365(10) 0.3913(5) 0.036(2) Uani d 0.2389(16) A 2 C C21B 0.2237(14) -0.0773(8) 0.4156(6) 0.045(3) Uani d 0.2389(16) A 2 H H21D 0.159721 -0.135744 0.405178 0.068 Uiso calc 0.2389(16) A 2 H H21E 0.322487 -0.083621 0.398520 0.068 Uiso calc 0.2389(16) A 2 H H21F 0.239714 -0.074587 0.456370 0.068 Uiso calc 0.2389(16) A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0240(11) 0.0161(10) 0.0274(12) -0.0042(8) -0.0001(9) 0.0027(9) C2 0.0286(11) 0.0213(11) 0.0230(11) -0.0023(9) 0.0040(9) 0.0080(9) C3 0.0269(11) 0.0229(11) 0.0204(11) -0.0006(9) -0.0018(9) 0.0070(9) C4 0.0210(10) 0.0183(10) 0.0240(11) -0.0015(8) -0.0003(8) 0.0049(9) C5 0.0247(11) 0.0165(10) 0.0233(11) 0.0008(8) 0.0033(9) 0.0029(8) C6 0.0281(11) 0.0206(11) 0.0228(11) -0.0049(9) 0.0055(9) 0.0022(9) C7 0.0264(11) 0.0242(11) 0.0157(10) -0.0028(9) 0.0024(8) 0.0057(9) C31 0.0365(15) 0.0550(18) 0.0350(15) -0.0138(13) -0.0097(12) -0.0061(13) C51 0.0330(14) 0.0497(17) 0.0442(16) 0.0086(12) 0.0143(12) 0.0046(13) C101 0.0158(9) 0.0169(9) 0.0200(10) 0.0004(7) 0.0019(8) 0.0039(8) C102 0.0198(10) 0.0285(12) 0.0220(11) -0.0030(9) 0.0007(8) 0.0037(9) C103 0.0171(10) 0.0354(13) 0.0355(14) -0.0056(9) -0.0048(9) 0.0073(11) C104 0.0156(10) 0.0340(13) 0.0421(15) 0.0013(9) 0.0071(10) 0.0105(11) C105 0.0264(11) 0.0315(12) 0.0297(13) 0.0043(10) 0.0136(10) 0.0034(10) C106 0.0224(10) 0.0243(11) 0.0244(11) -0.0004(9) 0.0043(9) -0.0016(9) C201 0.0151(9) 0.0191(10) 0.0166(10) -0.0025(8) -0.0026(7) -0.0005(8) C202 0.0155(9) 0.0245(11) 0.0222(11) -0.0043(8) 0.0014(8) 0.0000(9) C203 0.0211(11) 0.0289(12) 0.0339(13) 0.0023(9) 0.0062(9) -0.0020(10) C204 0.0361(13) 0.0229(12) 0.0434(15) 0.0082(10) 0.0079(11) 0.0039(11) C205 0.0362(13) 0.0231(11) 0.0314(13) 0.0006(10) 0.0060(10) 0.0092(10) C206 0.0220(10) 0.0257(11) 0.0196(11) 0.0009(9) 0.0030(8) 0.0038(9) C301 0.0164(9) 0.0209(10) 0.0160(10) -0.0001(8) 0.0009(8) -0.0019(8) C302 0.0241(11) 0.0245(11) 0.0180(10) 0.0017(9) -0.0009(8) -0.0016(9) C303 0.0301(12) 0.0377(13) 0.0165(11) 0.0054(10) -0.0024(9) -0.0023(10) C304 0.0222(11) 0.0431(14) 0.0196(11) -0.0002(10) -0.0007(9) -0.0124(10) C305 0.0241(11) 0.0305(12) 0.0269(12) -0.0084(9) 0.0042(9) -0.0097(10) C306 0.0204(10) 0.0252(11) 0.0200(11) -0.0033(8) 0.0025(8) -0.0016(9) O1 0.0234(9) 0.0379(10) 0.0510(12) -0.0059(7) 0.0099(8) 0.0056(9) O2 0.0493(11) 0.0271(9) 0.0212(8) -0.0062(8) 0.0013(8) -0.0034(7) P1 0.0148(2) 0.0172(2) 0.0133(2) -0.00280(19) 0.00064(18) 0.00045(19) S3 0.0447(4) 0.0419(4) 0.0197(3) -0.0054(3) -0.0077(3) 0.0082(3) S5 0.0346(3) 0.0255(3) 0.0270(3) -0.0041(2) 0.0088(2) -0.0073(2) Mn1 0.01927(15) 0.01714(15) 0.01465(15) -0.00385(12) 0.00220(12) 0.00208(12) Br1A 0.0344(3) 0.0202(4) 0.0311(5) -0.0119(3) 0.0011(3) -0.0032(3) S2A 0.0272(9) 0.0231(8) 0.0317(11) -0.0041(6) 0.0075(6) 0.0096(7) C21A 0.049(2) 0.0285(17) 0.045(2) 0.0000(15) 0.0081(17) 0.0193(16) Br1B 0.069(2) 0.0315(15) 0.050(3) -0.0072(11) 0.0247(15) 0.0108(14) S2B 0.045(3) 0.022(3) 0.041(5) -0.015(2) 0.002(4) -0.009(3) C21B 0.039(6) 0.026(6) 0.071(9) 0.003(5) 0.008(6) 0.001(6) 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 C5 C1 C2 . . 108.93(19) ? C5 C1 S2B . . 131.8(5) ? C2 C1 S2B . . 118.6(5) ? C5 C1 Br1A . . 123.81(18) ? C2 C1 Br1A . . 126.40(17) ? C5 C1 Mn1 . . 72.83(12) ? C2 C1 Mn1 . . 69.35(12) ? S2B C1 Mn1 . . 130.4(5) ? Br1A C1 Mn1 . . 132.24(12) ? C3 C2 C1 . . 106.96(19) ? C3 C2 S2A . . 126.9(2) ? C1 C2 S2A . . 125.6(2) ? C3 C2 Br1B . . 121.0(3) ? C1 C2 Br1B . . 131.7(3) ? C3 C2 Mn1 . . 72.42(12) ? C1 C2 Mn1 . . 71.53(12) ? S2A C2 Mn1 . . 127.65(17) ? Br1B C2 Mn1 . . 126.2(2) ? C2 C3 C4 . . 108.3(2) ? C2 C3 S3 . . 122.75(17) ? C4 C3 S3 . . 128.74(17) ? C2 C3 Mn1 . . 68.91(12) ? C4 C3 Mn1 . . 70.39(12) ? S3 C3 Mn1 . . 129.93(13) ? C3 C4 C5 . . 108.09(19) ? C3 C4 Mn1 . . 71.24(12) ? C5 C4 Mn1 . . 72.43(12) ? C3 C4 H4 . . 126.0 ? C5 C4 H4 . . 126.0 ? Mn1 C4 H4 . . 122.1 ? C1 C5 C4 . . 107.46(19) ? C1 C5 S5 . . 124.44(17) ? C4 C5 S5 . . 127.95(16) ? C1 C5 Mn1 . . 69.27(12) ? C4 C5 Mn1 . . 69.37(12) ? S5 C5 Mn1 . . 130.03(12) ? O1 C6 Mn1 . . 177.3(2) ? O2 C7 Mn1 . . 176.22(19) ? S3 C31 H31A . . 109.5 ? S3 C31 H31B . . 109.5 ? H31A C31 H31B . . 109.5 ? S3 C31 H31C . . 109.5 ? H31A C31 H31C . . 109.5 ? H31B C31 H31C . . 109.5 ? S5 C51 H51A . . 109.5 ? S5 C51 H51B . . 109.5 ? H51A C51 H51B . . 109.5 ? S5 C51 H51C . . 109.5 ? H51A C51 H51C . . 109.5 ? H51B C51 H51C . . 109.5 ? C106 C101 C102 . . 118.35(19) ? C106 C101 P1 . . 125.43(16) ? C102 C101 P1 . . 116.22(16) ? C103 C102 C101 . . 121.0(2) ? C103 C102 H102 . . 119.5 ? C101 C102 H102 . . 119.5 ? C104 C103 C102 . . 120.0(2) ? C104 C103 H103 . . 120.0 ? C102 C103 H103 . . 120.0 ? C105 C104 C103 . . 119.9(2) ? C105 C104 H104 . . 120.1 ? C103 C104 H104 . . 120.1 ? C104 C105 C106 . . 120.3(2) ? C104 C105 H105 . . 119.8 ? C106 C105 H105 . . 119.8 ? C101 C106 C105 . . 120.4(2) ? C101 C106 H106 . . 119.8 ? C105 C106 H106 . . 119.8 ? C206 C201 C202 . . 118.06(19) ? C206 C201 P1 . . 120.49(16) ? C202 C201 P1 . . 121.44(16) ? C203 C202 C201 . . 120.6(2) ? C203 C202 H202 . . 119.7 ? C201 C202 H202 . . 119.7 ? C204 C203 C202 . . 120.5(2) ? C204 C203 H203 . . 119.8 ? C202 C203 H203 . . 119.8 ? C203 C204 C205 . . 119.5(2) ? C203 C204 H204 . . 120.2 ? C205 C204 H204 . . 120.2 ? C206 C205 C204 . . 120.2(2) ? C206 C205 H205 . . 119.9 ? C204 C205 H205 . . 119.9 ? C205 C206 C201 . . 121.1(2) ? C205 C206 H206 . . 119.4 ? C201 C206 H206 . . 119.4 ? C306 C301 C302 . . 118.5(2) ? C306 C301 P1 . . 119.14(16) ? C302 C301 P1 . . 122.30(16) ? C301 C302 C303 . . 120.6(2) ? C301 C302 H302 . . 119.7 ? C303 C302 H302 . . 119.7 ? C304 C303 C302 . . 120.1(2) ? C304 C303 H303 . . 120.0 ? C302 C303 H303 . . 120.0 ? C305 C304 C303 . . 119.7(2) ? C305 C304 H304 . . 120.1 ? C303 C304 H304 . . 120.1 ? C304 C305 C306 . . 120.4(2) ? C304 C305 H305 . . 119.8 ? C306 C305 H305 . . 119.8 ? C305 C306 C301 . . 120.6(2) ? C305 C306 H306 . . 119.7 ? C301 C306 H306 . . 119.7 ? C101 P1 C301 . . 105.32(9) ? C101 P1 C201 . . 99.41(9) ? C301 P1 C201 . . 101.48(9) ? C101 P1 Mn1 . . 113.16(7) ? C301 P1 Mn1 . . 117.03(7) ? C201 P1 Mn1 . . 118.15(7) ? C3 S3 C31 . . 100.44(12) ? C5 S5 C51 . . 101.60(12) ? C7 Mn1 C6 . . 92.86(10) ? C7 Mn1 C2 . . 110.42(9) ? C6 Mn1 C2 . . 95.61(9) ? C7 Mn1 C1 . . 149.24(9) ? C6 Mn1 C1 . . 94.53(9) ? C2 Mn1 C1 . . 39.13(9) ? C7 Mn1 C4 . . 103.30(9) ? C6 Mn1 C4 . . 158.16(9) ? C2 Mn1 C4 . . 65.17(8) ? C1 Mn1 C4 . . 64.16(8) ? C7 Mn1 C3 . . 88.42(9) ? C6 Mn1 C3 . . 129.55(9) ? C2 Mn1 C3 . . 38.66(8) ? C1 Mn1 C3 . . 64.10(9) ? C4 Mn1 C3 . . 38.37(8) ? C7 Mn1 C5 . . 141.11(9) ? C6 Mn1 C5 . . 125.58(9) ? C2 Mn1 C5 . . 64.76(8) ? C1 Mn1 C5 . . 37.90(8) ? C4 Mn1 C5 . . 38.19(8) ? C3 Mn1 C5 . . 63.72(8) ? C7 Mn1 P1 . . 90.98(7) ? C6 Mn1 P1 . . 92.22(7) ? C2 Mn1 P1 . . 156.73(7) ? C1 Mn1 P1 . . 118.47(6) ? C4 Mn1 P1 . . 101.96(6) ? C3 Mn1 P1 . . 138.21(6) ? C5 Mn1 P1 . . 92.95(6) ? C2 S2A C21A . . 99.0(2) ? S2A C21A H21A . . 109.5 ? S2A C21A H21B . . 109.5 ? H21A C21A H21B . . 109.5 ? S2A C21A H21C . . 109.5 ? H21A C21A H21C . . 109.5 ? H21B C21A H21C . . 109.5 ? C1 S2B C21B . . 100.1(9) ? S2B C21B H21D . . 109.5 ? S2B C21B H21E . . 109.5 ? H21D C21B H21E . . 109.5 ? S2B C21B H21F . . 109.5 ? H21D C21B H21F . . 109.5 ? H21E C21B H21F . . 109.5 ? 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 C1 C5 . 1.416(3) ? C1 C2 . 1.434(3) ? C1 S2B . 1.656(14) ? C1 Br1A . 1.906(3) ? C1 Mn1 . 2.155(2) ? C2 C3 . 1.424(3) ? C2 S2A . 1.771(5) ? C2 Br1B . 1.890(7) ? C2 Mn1 . 2.127(2) ? C3 C4 . 1.425(3) ? C3 S3 . 1.742(2) ? C3 Mn1 . 2.173(2) ? C4 C5 . 1.428(3) ? C4 Mn1 . 2.162(2) ? C4 H4 . 0.9500 ? C5 S5 . 1.753(2) ? C5 Mn1 . 2.202(2) ? C6 O1 . 1.152(3) ? C6 Mn1 . 1.788(2) ? C7 O2 . 1.160(3) ? C7 Mn1 . 1.774(2) ? C31 S3 . 1.798(3) ? C31 H31A . 0.9800 ? C31 H31B . 0.9800 ? C31 H31C . 0.9800 ? C51 S5 . 1.805(3) ? C51 H51A . 0.9800 ? C51 H51B . 0.9800 ? C51 H51C . 0.9800 ? C101 C106 . 1.392(3) ? C101 C102 . 1.397(3) ? C101 P1 . 1.833(2) ? C102 C103 . 1.384(3) ? C102 H102 . 0.9500 ? C103 C104 . 1.382(4) ? C103 H103 . 0.9500 ? C104 C105 . 1.378(4) ? C104 H104 . 0.9500 ? C105 C106 . 1.394(3) ? C105 H105 . 0.9500 ? C106 H106 . 0.9500 ? C201 C206 . 1.397(3) ? C201 C202 . 1.399(3) ? C201 P1 . 1.845(2) ? C202 C203 . 1.389(3) ? C202 H202 . 0.9500 ? C203 C204 . 1.383(3) ? C203 H203 . 0.9500 ? C204 C205 . 1.386(3) ? C204 H204 . 0.9500 ? C205 C206 . 1.381(3) ? C205 H205 . 0.9500 ? C206 H206 . 0.9500 ? C301 C306 . 1.393(3) ? C301 C302 . 1.394(3) ? C301 P1 . 1.841(2) ? C302 C303 . 1.396(3) ? C302 H302 . 0.9500 ? C303 C304 . 1.383(3) ? C303 H303 . 0.9500 ? C304 C305 . 1.382(3) ? C304 H304 . 0.9500 ? C305 C306 . 1.390(3) ? C305 H305 . 0.9500 ? C306 H306 . 0.9500 ? P1 Mn1 . 2.2563(6) ? S2A C21A . 1.811(5) ? C21A H21A . 0.9800 ? C21A H21B . 0.9800 ? C21A H21C . 0.9800 ? S2B C21B . 1.793(13) ? C21B H21D . 0.9800 ? C21B H21E . 0.9800 ? C21B H21F . 0.9800 ? 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 . . . . -1.8(2) ? S2B C1 C2 C3 . . . . 170.1(6) ? Br1A C1 C2 C3 . . . . 167.84(17) ? Mn1 C1 C2 C3 . . . . -64.23(15) ? C5 C1 C2 S2A . . . . -174.0(2) ? Br1A C1 C2 S2A . . . . -4.4(3) ? Mn1 C1 C2 S2A . . . . 123.6(2) ? C5 C1 C2 Br1B . . . . -175.1(3) ? S2B C1 C2 Br1B . . . . -3.2(7) ? Mn1 C1 C2 Br1B . . . . 122.5(3) ? C5 C1 C2 Mn1 . . . . 62.43(15) ? S2B C1 C2 Mn1 . . . . -125.7(6) ? Br1A C1 C2 Mn1 . . . . -127.93(18) ? C1 C2 C3 C4 . . . . 4.1(2) ? S2A C2 C3 C4 . . . . 176.2(2) ? Br1B C2 C3 C4 . . . . 178.3(3) ? Mn1 C2 C3 C4 . . . . -59.54(15) ? C1 C2 C3 S3 . . . . -171.62(17) ? S2A C2 C3 S3 . . . . 0.5(3) ? Br1B C2 C3 S3 . . . . 2.5(4) ? Mn1 C2 C3 S3 . . . . 124.75(17) ? C1 C2 C3 Mn1 . . . . 63.63(15) ? S2A C2 C3 Mn1 . . . . -124.3(2) ? Br1B C2 C3 Mn1 . . . . -122.2(3) ? C2 C3 C4 C5 . . . . -4.9(2) ? S3 C3 C4 C5 . . . . 170.51(17) ? Mn1 C3 C4 C5 . . . . -63.49(15) ? C2 C3 C4 Mn1 . . . . 58.63(16) ? S3 C3 C4 Mn1 . . . . -126.0(2) ? C2 C1 C5 C4 . . . . -1.2(2) ? S2B C1 C5 C4 . . . . -171.6(7) ? Br1A C1 C5 C4 . . . . -171.13(16) ? Mn1 C1 C5 C4 . . . . 59.08(15) ? C2 C1 C5 S5 . . . . 174.69(16) ? S2B C1 C5 S5 . . . . 4.3(7) ? Br1A C1 C5 S5 . . . . 4.7(3) ? Mn1 C1 C5 S5 . . . . -125.05(17) ? C2 C1 C5 Mn1 . . . . -60.25(15) ? S2B C1 C5 Mn1 . . . . 129.3(7) ? Br1A C1 C5 Mn1 . . . . 129.79(18) ? C3 C4 C5 C1 . . . . 3.7(2) ? Mn1 C4 C5 C1 . . . . -59.02(15) ? C3 C4 C5 S5 . . . . -171.97(17) ? Mn1 C4 C5 S5 . . . . 125.31(18) ? C3 C4 C5 Mn1 . . . . 62.72(15) ? C106 C101 C102 C103 . . . . -0.9(3) ? P1 C101 C102 C103 . . . . 179.28(18) ? C101 C102 C103 C104 . . . . -0.5(4) ? C102 C103 C104 C105 . . . . 1.3(4) ? C103 C104 C105 C106 . . . . -0.8(4) ? C102 C101 C106 C105 . . . . 1.4(3) ? P1 C101 C106 C105 . . . . -178.77(17) ? C104 C105 C106 C101 . . . . -0.6(4) ? C206 C201 C202 C203 . . . . 0.4(3) ? P1 C201 C202 C203 . . . . -178.47(17) ? C201 C202 C203 C204 . . . . -0.2(4) ? C202 C203 C204 C205 . . . . -0.3(4) ? C203 C204 C205 C206 . . . . 0.7(4) ? C204 C205 C206 C201 . . . . -0.5(4) ? C202 C201 C206 C205 . . . . -0.1(3) ? P1 C201 C206 C205 . . . . 178.81(18) ? C306 C301 C302 C303 . . . . 0.1(3) ? P1 C301 C302 C303 . . . . -178.32(17) ? C301 C302 C303 C304 . . . . -0.5(3) ? C302 C303 C304 C305 . . . . 0.3(3) ? C303 C304 C305 C306 . . . . 0.3(3) ? C304 C305 C306 C301 . . . . -0.8(3) ? C302 C301 C306 C305 . . . . 0.6(3) ? P1 C301 C306 C305 . . . . 178.98(16) ? C106 C101 P1 C301 . . . . -5.0(2) ? C102 C101 P1 C301 . . . . 174.82(16) ? C106 C101 P1 C201 . . . . -109.79(19) ? C102 C101 P1 C201 . . . . 70.06(18) ? C106 C101 P1 Mn1 . . . . 123.98(18) ? C102 C101 P1 Mn1 . . . . -56.16(18) ? C306 C301 P1 C101 . . . . 123.01(17) ? C302 C301 P1 C101 . . . . -58.62(19) ? C306 C301 P1 C201 . . . . -133.77(17) ? C302 C301 P1 C201 . . . . 44.60(19) ? C306 C301 P1 Mn1 . . . . -3.68(19) ? C302 C301 P1 Mn1 . . . . 174.69(15) ? C206 C201 P1 C101 . . . . 26.67(19) ? C202 C201 P1 C101 . . . . -154.49(17) ? C206 C201 P1 C301 . . . . -81.20(18) ? C202 C201 P1 C301 . . . . 97.63(18) ? C206 C201 P1 Mn1 . . . . 149.41(15) ? C202 C201 P1 Mn1 . . . . -31.76(19) ? C2 C3 S3 C31 . . . . -172.4(2) ? C4 C3 S3 C31 . . . . 12.8(2) ? Mn1 C3 S3 C31 . . . . -83.51(18) ? C1 C5 S5 C51 . . . . -148.7(2) ? C4 C5 S5 C51 . . . . 26.3(2) ? Mn1 C5 S5 C51 . . . . 120.45(16) ? C3 C2 S2A C21A . . . . -90.2(3) ? C1 C2 S2A C21A . . . . 80.5(3) ? Mn1 C2 S2A C21A . . . . 174.0(2) ? C5 C1 S2B C21B . . . . 95.2(8) ? C2 C1 S2B C21B . . . . -74.5(9) ? Mn1 C1 S2B C21B . . . . -160.9(5) ?