#------------------------------------------------------------------------------ #$Date: 2022-10-14 03:46:53 +0200 (Fri, 14 Oct 2022) $ #$Revision: 278580 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022686.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_2022686 loop_ _publ_author_name 'Blockhaus, Tobias' 'S\"unkel, Karlheinz' _publ_section_title ; Isolation and crystal and molecular structures of [(C5H2Br3)2Fe], [(C5HBr4)2Fe] and [(C5Br5)(C5Br4HgBr)Fe] ; _journal_coeditor_code QW3001 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C Structural Chemistry' _journal_paper_doi 10.1107/S205322962200955X _journal_volume 78 _journal_year 2022 _chemical_formula_iupac '[Fe Hg Br (C5 Br4) (C5 Br5)]' _chemical_formula_moiety 'C10 Br10 Fe Hg' _chemical_formula_sum 'C10 Br10 Fe Hg' _chemical_formula_weight 1175.64 _chemical_name_systematic (1-Bromomercurio-2,3,4,5-tetrabromocyclopentadienyl)(1,2,3,4,5-pentabromocyclopentadienyl)iron(II) _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_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90.6890(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9784(3) _cell_length_b 14.0971(4) _cell_length_c 15.8485(4) _cell_measurement_reflns_used 9571 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 26.0975 _cell_measurement_theta_min 2.5940 _cell_volume 2005.79(10) _computing_cell_refinement ; APEX2 (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2011) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 7.4074 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'D8 Venture' _diffrn_measurement_method 'mix of omega and phi scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_unetI/netI 0.0298 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 33353 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.384 _diffrn_reflns_theta_min 2.890 _diffrn_source 'rotating anode generator' _exptl_absorpt_coefficient_mu 28.279 _exptl_absorpt_correction_T_max 0.3323 _exptl_absorpt_correction_T_min 0.1931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 2064 _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.631 _refine_diff_density_min -1.239 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 4098 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0362 _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^)+(0.0321P)^2^+17.6846P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.0920 _reflns_number_gt 3154 _reflns_number_total 4098 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file qw3001sup1.cif _cod_data_source_block compd_8 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2022686 _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 0.282 _shelx_estimated_absorpt_t_max 0.602 _shelx_hkl_file ; -1 0 0 0.29 0.22 -1 0 0 -0.39 0.14 -1 0 0 -0.11 0.09 2 0 0 201.09 7.20 2 0 0 201.73 7.63 -2 0 0 201.98 7.70 -2 0 0 204.50 7.63 -2 0 0 203.34 7.18 2 0 0 211.07 7.73 3 0 0 3.04 1.17 3 0 0 3.08 1.56 -3 0 0 5.81 1.11 -3 0 0 2.69 1.33 -3 0 0 6.09 1.50 3 0 0 3.44 0.98 -4 0 0 495.78 18.72 4 0 0 506.88 17.69 4 0 0 520.43 18.57 4 0 0 513.08 18.72 -4 0 0 505.42 17.60 -5 0 0 2.03 2.03 5 0 0 1.33 2.05 -5 0 0 -0.09 1.36 5 0 0 3.06 2.33 5 0 0 2.34 1.56 -5 0 0 -1.59 1.80 -6 0 0 52.68 3.69 6 0 0 57.10 5.47 -6 0 0 61.31 5.73 6 0 0 53.23 5.13 -6 0 0 49.33 4.66 7 0 0 1.60 3.11 -7 0 0 3.55 2.05 7 0 0 -0.23 2.25 -7 0 0 -0.15 3.58 7 0 0 0.19 3.28 -8 0 0 65.30 4.80 8 0 0 47.79 4.61 -8 0 0 62.41 7.22 8 0 0 57.13 6.45 9 0 0 0.99 4.32 -9 0 0 1.00 2.74 -9 0 0 3.35 5.05 9 0 0 1.53 2.90 -10 0 0 60.38 5.30 10 0 0 56.95 7.49 -10 0 0 55.39 7.43 10 0 0 47.64 5.20 -11 0 0 0.72 3.34 11 0 0 5.34 5.46 -11 0 0 0.89 2.97 -11 0 0 -4.82 4.38 2 -1 0 0.50 0.82 2 -1 0 1.27 0.80 -2 -1 0 1.23 0.59 2 -1 0 2.60 1.05 -2 -1 0 0.60 0.72 -2 -1 0 0.12 0.78 -2 1 0 1.17 0.81 -2 1 0 0.29 1.06 -2 1 0 2.69 0.74 2 1 0 -0.10 0.73 2 1 0 1.98 0.88 2 1 0 1.26 0.62 3 -1 0 1934.03 64.79 3 -1 0 1906.03 64.58 3 -1 0 1919.99 64.14 3 1 0 1959.56 64.88 3 1 0 1993.66 64.85 -3 1 0 1940.99 64.84 4 -1 0 324.79 12.76 4 -1 0 336.59 12.71 -4 -1 0 319.68 12.88 -4 -1 0 340.57 12.86 -4 -1 0 349.22 11.84 4 -1 0 320.61 11.96 -4 1 0 314.74 12.93 4 1 0 319.76 11.81 -4 1 0 313.74 11.87 4 1 0 327.74 12.91 4 1 0 340.32 12.95 -4 1 0 335.24 12.76 5 -1 0 0.38 2.23 -5 -1 0 -1.05 1.91 5 -1 0 1.13 1.45 -5 -1 0 1.90 2.60 -5 -1 0 0.06 1.38 5 -1 0 2.30 2.13 5 1 0 0.02 2.19 5 1 0 1.80 2.34 -5 1 0 1.72 1.91 5 1 0 4.12 1.61 -5 1 0 0.04 1.89 -5 1 0 1.61 1.55 6 -1 0 4.80 1.83 6 -1 0 0.47 2.44 -6 -1 0 0.04 2.41 -6 -1 0 0.11 2.13 6 -1 0 -0.96 2.42 -6 -1 0 1.47 1.65 -6 1 0 3.86 1.77 6 1 0 -1.49 2.51 -6 1 0 1.61 3.03 -6 1 0 2.62 2.55 6 1 0 0.71 2.69 6 1 0 3.72 2.09 -7 -1 0 109.02 7.43 -7 -1 0 125.87 6.12 -7 -1 0 121.99 8.49 7 -1 0 126.55 7.94 7 -1 0 125.18 6.54 7 -1 0 108.39 7.69 -7 1 0 126.12 8.60 7 1 0 108.74 7.86 -7 1 0 121.37 7.60 7 1 0 110.07 6.16 -7 1 0 127.19 7.00 7 1 0 123.12 8.06 -8 -1 0 21.01 4.43 8 -1 0 18.02 4.48 -8 -1 0 20.20 3.13 8 -1 0 19.41 3.50 -8 1 0 11.87 3.94 8 1 0 17.55 3.47 -8 1 0 21.91 5.38 8 1 0 22.50 4.35 -8 1 0 17.20 3.12 -9 -1 0 18.82 3.26 -9 -1 0 11.33 5.63 9 -1 0 15.71 3.65 9 -1 0 26.00 5.24 -9 1 0 14.66 3.18 9 1 0 18.71 5.04 9 1 0 19.15 3.61 -9 1 0 19.43 5.90 -10 -1 0 11.68 3.29 10 -1 0 18.13 5.97 -10 -1 0 5.00 6.09 -10 1 0 15.02 3.38 -10 1 0 14.77 3.46 -10 1 0 16.83 6.58 10 1 0 3.56 4.80 10 1 0 12.28 3.78 11 -1 0 9.04 6.27 -11 -1 0 5.82 3.30 -11 1 0 2.00 3.70 11 1 0 11.29 6.12 -11 1 0 -0.66 3.17 -11 1 0 19.08 6.87 0 -2 0 8.50 1.13 0 2 0 11.43 1.21 0 2 0 9.20 0.77 1 -2 0 51.68 2.27 -1 -2 0 47.88 2.18 -1 -2 0 51.25 2.55 -1 -2 0 47.64 2.48 1 -2 0 47.59 2.35 1 2 0 51.50 2.46 1 2 0 50.07 2.21 -1 2 0 49.51 2.33 -1 2 0 43.15 2.27 1 2 0 48.25 2.42 -1 2 0 47.34 2.15 -1 2 0 49.38 2.48 -2 -2 0 371.52 14.05 -2 -2 0 394.34 14.08 -2 -2 0 403.07 13.48 2 -2 0 388.53 13.79 2 -2 0 391.09 13.75 -2 2 0 401.83 13.76 2 2 0 396.36 14.10 2 2 0 375.40 13.45 -2 2 0 391.61 13.78 -2 2 0 395.27 13.76 2 2 0 391.67 14.11 -2 2 0 391.66 13.53 -2 2 0 401.68 14.04 -3 -2 0 382.07 14.66 -3 -2 0 389.09 13.42 -3 -2 0 385.85 14.32 3 -2 0 359.78 13.64 3 -2 0 393.43 13.97 3 2 0 367.84 13.40 3 2 0 389.70 14.31 -3 2 0 388.86 14.27 -3 2 0 386.54 13.72 3 2 0 376.31 14.34 -3 2 0 398.48 14.01 -3 2 0 396.27 14.01 -4 -2 0 35.37 3.36 -4 -2 0 33.92 3.34 4 -2 0 31.31 2.84 4 -2 0 37.05 3.34 4 -2 0 28.64 2.54 -4 -2 0 26.82 2.30 -4 2 0 28.22 3.10 -4 2 0 29.94 2.64 -4 2 0 31.28 2.48 4 2 0 32.28 3.29 4 2 0 28.17 2.38 4 2 0 31.51 3.35 -4 2 0 31.79 3.01 -5 -2 0 141.68 6.11 -5 -2 0 131.22 7.03 -5 -2 0 162.12 8.03 5 -2 0 143.21 6.46 5 -2 0 139.69 7.36 5 -2 0 148.75 7.34 -5 2 0 118.50 7.43 5 2 0 146.21 7.37 -5 2 0 138.66 7.06 5 2 0 144.31 6.17 -5 2 0 144.48 6.51 5 2 0 149.86 7.71 -5 2 0 145.22 7.15 6 -2 0 10.84 2.48 -6 -2 0 11.38 3.03 -6 -2 0 10.11 2.10 -6 -2 0 5.63 2.69 6 -2 0 7.74 3.01 6 -2 0 7.42 3.13 -6 2 0 4.93 2.66 6 2 0 5.31 3.13 -6 2 0 9.10 2.83 -6 2 0 6.36 2.28 -6 2 0 9.77 3.07 6 2 0 5.95 2.94 -7 -2 0 172.79 9.99 -7 -2 0 197.46 10.14 -7 -2 0 184.85 8.16 7 -2 0 185.30 8.53 7 -2 0 194.27 9.92 -7 2 0 191.08 8.59 -7 2 0 195.49 9.79 7 2 0 186.95 10.30 -7 2 0 191.25 9.75 7 2 0 196.16 8.40 -7 2 0 193.95 10.22 7 2 0 176.15 10.16 8 -2 0 31.72 5.08 -8 -2 0 35.72 3.71 8 -2 0 37.63 4.31 -8 -2 0 37.12 5.66 -8 2 0 27.90 4.75 -8 2 0 32.33 5.33 -8 2 0 31.70 3.76 8 2 0 33.93 5.46 -8 2 0 24.24 3.77 8 2 0 31.38 3.78 9 -2 0 19.85 5.15 -9 -2 0 12.06 5.74 -9 -2 0 19.82 3.30 -9 2 0 17.75 3.26 -9 2 0 21.34 3.76 9 2 0 19.50 5.33 -9 2 0 20.60 6.01 9 2 0 12.46 3.44 -10 -2 0 13.41 6.28 -10 -2 0 8.96 3.34 10 -2 0 14.32 5.22 -10 2 0 6.19 3.40 -10 2 0 10.21 3.41 10 2 0 9.94 3.49 -10 2 0 19.36 6.62 10 2 0 15.26 5.62 -11 -2 0 58.26 10.74 -11 -2 0 52.47 5.07 11 -2 0 52.53 8.30 11 2 0 46.61 7.65 -11 2 0 39.44 8.15 -11 2 0 37.72 5.05 0 -3 0 3.00 0.78 0 -3 0 1.13 1.21 0 -3 0 0.85 1.13 0 3 0 2.43 1.06 0 3 0 0.22 0.97 0 3 0 -0.16 0.69 1 -3 0 157.40 6.64 1 -3 0 162.36 6.38 -1 -3 0 152.44 6.36 -1 -3 0 166.71 6.01 -1 -3 0 154.29 6.34 1 -3 0 156.71 6.05 1 3 0 167.72 6.36 1 3 0 159.90 6.39 -1 3 0 151.31 6.49 -1 3 0 160.18 6.03 1 3 0 159.72 6.01 -1 3 0 151.76 6.25 2 -3 0 538.79 18.55 2 -3 0 536.90 18.44 2 -3 0 539.32 18.36 -2 -3 0 546.39 18.23 -2 -3 0 529.34 18.86 -2 -3 0 515.71 18.79 -2 3 0 532.31 18.58 2 3 0 519.38 18.24 -2 3 0 533.57 18.29 -2 3 0 527.39 18.46 2 3 0 537.78 18.89 2 3 0 514.68 18.82 -2 3 0 534.48 18.46 -3 -3 0 34.91 2.90 3 -3 0 34.13 2.84 -3 -3 0 32.11 2.36 -3 -3 0 32.13 2.71 -3 3 0 36.71 3.16 3 3 0 36.40 3.27 -3 3 0 34.30 2.69 3 3 0 34.19 2.45 -3 3 0 29.37 2.51 -3 3 0 34.46 2.48 -3 3 0 31.74 2.60 3 3 0 34.69 3.32 4 -3 0 950.67 32.90 -4 -3 0 930.94 32.17 -4 -3 0 926.96 33.35 4 3 0 942.44 32.23 -4 3 0 968.56 32.67 -4 3 0 971.78 32.40 -4 3 0 956.98 33.07 4 3 0 913.59 33.38 -4 3 0 980.75 33.50 -4 3 0 973.50 32.99 -5 -3 0 75.84 4.22 -5 -3 0 79.55 5.86 5 -3 0 79.51 5.24 -5 -3 0 73.96 5.38 -5 3 0 85.13 5.39 -5 3 0 73.92 5.14 5 3 0 74.45 5.23 -5 3 0 74.01 4.70 5 3 0 81.46 5.85 -5 3 0 81.71 4.31 -5 3 0 79.80 5.11 5 3 0 71.58 4.23 -6 -3 0 42.18 4.84 -6 -3 0 42.31 3.47 6 -3 0 34.44 4.26 -6 -3 0 46.35 5.20 -6 3 0 41.02 4.30 -6 3 0 38.90 4.32 6 3 0 41.10 3.49 -6 3 0 38.66 5.07 6 3 0 40.06 4.66 6 3 0 38.36 4.93 -6 3 0 51.04 4.84 -6 3 0 43.46 3.45 -7 -3 0 16.93 3.93 -7 -3 0 22.30 5.05 7 -3 0 15.93 3.83 7 3 0 20.12 4.38 -7 3 0 19.56 2.86 7 3 0 17.95 2.87 -7 3 0 13.11 3.53 7 3 0 17.43 4.40 -7 3 0 16.95 3.88 -7 3 0 14.91 3.09 -7 3 0 11.29 3.63 8 -3 0 331.04 15.35 -8 -3 0 362.39 13.65 -8 3 0 353.64 15.60 8 3 0 349.84 13.78 -8 3 0 332.48 13.89 -8 3 0 360.17 16.70 -8 3 0 345.27 13.83 8 3 0 326.08 15.67 -9 -3 0 14.00 4.73 9 -3 0 7.43 5.23 -9 -3 0 8.55 2.94 -9 3 0 2.29 3.04 -9 3 0 9.56 5.44 9 3 0 11.82 4.94 9 3 0 8.60 3.09 -9 3 0 0.78 2.79 10 -3 0 4.69 4.39 -10 -3 0 2.94 2.95 -10 -3 0 11.75 6.30 -10 3 0 4.63 3.09 10 3 0 -1.91 3.42 -10 3 0 -0.15 5.24 -10 3 0 7.91 3.75 10 3 0 -0.19 3.83 -11 -3 0 12.38 3.48 11 -3 0 10.87 5.68 -11 -3 0 2.03 5.71 -11 3 0 9.27 3.74 -11 3 0 14.39 6.11 11 3 0 7.25 5.96 0 -4 0 434.94 16.66 0 -4 0 450.45 16.85 0 -4 0 463.94 15.91 0 4 0 464.20 16.41 0 4 0 469.03 16.53 0 4 0 453.53 15.88 1 -4 0 2254.92 75.56 2 -4 0 25.31 1.98 -2 -4 0 22.79 2.03 -2 -4 0 21.62 2.51 -2 -4 0 23.17 2.62 2 -4 0 28.12 2.47 2 4 0 27.78 2.77 2 4 0 30.10 2.86 -2 4 0 26.81 2.15 2 4 0 27.01 2.17 -2 4 0 25.51 2.41 -2 4 0 25.82 2.21 -2 4 0 21.30 2.47 3 -4 0 18.67 2.43 3 -4 0 16.00 2.14 -3 -4 0 22.47 2.12 -3 -4 0 20.41 2.70 -3 -4 0 22.96 2.94 3 4 0 17.64 2.79 3 4 0 16.54 2.02 -3 4 0 23.86 2.29 3 4 0 21.54 2.65 -3 4 0 18.19 2.26 -3 4 0 22.62 2.54 -3 4 0 18.49 2.43 -4 -4 0 47.29 3.02 -4 -4 0 44.84 4.40 4 -4 0 45.55 3.61 -4 -4 0 44.34 4.01 4 4 0 41.52 3.78 4 4 0 48.79 3.30 -4 4 0 43.12 3.50 -4 4 0 41.35 3.05 -4 4 0 42.26 4.00 -4 4 0 46.27 4.14 -4 4 0 51.52 3.74 4 4 0 41.15 3.68 -5 -4 0 3.90 2.81 -5 -4 0 2.17 2.45 -5 -4 0 2.45 1.61 5 -4 0 5.16 2.36 -5 4 0 3.52 1.94 -5 4 0 3.23 2.30 -5 4 0 6.34 2.37 -5 4 0 5.75 2.52 5 4 0 4.10 2.25 -5 4 0 3.95 1.72 5 4 0 10.69 3.18 -6 -4 0 143.58 8.93 -6 -4 0 160.06 7.10 6 -4 0 148.40 8.05 -6 -4 0 147.10 8.35 -6 4 0 171.42 7.78 -6 4 0 169.69 8.07 -6 4 0 143.42 8.18 -6 4 0 155.70 7.17 -6 4 0 159.52 8.96 6 4 0 145.76 8.88 6 4 0 154.31 9.93 6 4 0 164.80 7.31 -7 -4 0 8.63 3.30 7 -4 0 12.17 3.58 -7 -4 0 12.30 3.21 -7 -4 0 14.97 2.73 -7 4 0 11.99 3.55 7 4 0 8.89 4.43 7 4 0 7.32 3.05 7 4 0 7.93 2.30 -7 4 0 9.11 3.26 -7 4 0 9.92 3.17 -7 4 0 8.73 2.88 -7 4 0 9.29 3.58 -8 -4 0 0.39 4.41 -8 -4 0 1.47 2.72 8 -4 0 1.98 3.47 -8 4 0 1.21 2.60 8 4 0 0.46 4.93 -8 4 0 3.03 2.81 8 4 0 -0.24 2.60 -8 4 0 4.55 3.42 -8 4 0 5.22 4.70 -9 -4 0 53.35 6.96 9 -4 0 71.34 8.51 -9 -4 0 56.13 4.98 -9 4 0 67.30 5.00 -9 4 0 57.46 5.53 9 4 0 57.87 5.22 -9 4 0 51.99 7.00 9 4 0 47.29 7.16 -10 -4 0 9.29 4.91 10 -4 0 0.43 4.22 -10 -4 0 4.65 3.03 10 4 0 14.91 5.80 -10 4 0 3.32 3.18 -10 4 0 13.38 3.91 10 4 0 1.84 3.38 -10 4 0 5.14 5.65 0 -5 0 0.77 1.23 0 -5 0 0.13 1.58 0 -5 0 -1.98 1.63 0 5 0 -0.61 1.41 0 5 0 4.95 1.65 0 5 0 -0.63 1.14 -1 -5 0 198.43 7.37 1 -5 0 187.24 8.90 -1 -5 0 173.55 7.89 1 -5 0 178.15 8.19 -1 -5 0 183.73 8.04 1 -5 0 175.23 7.40 -1 5 0 177.59 8.17 1 5 0 188.07 7.40 -1 5 0 195.56 7.46 -1 5 0 182.19 8.04 1 5 0 189.04 7.96 1 5 0 183.96 7.82 -2 -5 0 202.12 8.98 2 -5 0 196.46 8.29 2 -5 0 199.94 8.70 -2 -5 0 218.06 8.23 -2 -5 0 209.99 8.93 -2 5 0 211.49 9.04 2 5 0 203.69 8.85 -2 5 0 221.53 8.37 2 5 0 211.10 8.27 2 5 0 211.48 8.97 -2 5 0 200.17 8.44 -2 5 0 214.83 8.66 3 -5 0 157.87 6.79 3 -5 0 153.07 7.05 -3 -5 0 157.79 6.51 -3 -5 0 153.78 7.29 -3 -5 0 158.29 7.49 -3 5 0 148.40 7.32 3 5 0 138.34 7.43 -3 5 0 151.80 7.08 3 5 0 147.84 6.55 -3 5 0 149.91 7.46 -3 5 0 150.45 6.58 -3 5 0 150.88 6.90 3 5 0 155.82 7.52 -4 -5 0 35.08 3.08 -4 -5 0 29.10 3.94 4 -5 0 35.12 3.40 -4 -5 0 39.83 4.15 -4 5 0 32.78 3.14 -4 5 0 40.56 4.26 4 5 0 42.01 4.42 -4 5 0 32.57 3.53 -4 5 0 30.69 3.70 4 5 0 29.73 3.61 -4 5 0 35.17 3.44 -4 5 0 34.87 3.69 -5 -5 0 1.89 1.83 5 -5 0 0.50 2.18 -5 -5 0 -0.03 2.51 -5 -5 0 0.40 2.83 -5 5 0 2.61 1.83 -5 5 0 0.17 2.10 5 5 0 -1.64 2.70 -5 5 0 -0.07 1.93 5 5 0 3.05 2.91 -5 5 0 -5.28 2.44 -5 5 0 3.06 2.22 5 5 0 2.75 1.86 -6 -5 0 105.76 7.37 6 -5 0 122.01 6.97 -6 -5 0 130.17 6.15 -6 -5 0 115.64 7.94 6 5 0 115.95 6.22 -6 5 0 110.49 6.92 -6 5 0 106.90 6.80 6 5 0 109.16 7.93 -6 5 0 103.05 6.52 -6 5 0 117.27 6.36 6 5 0 117.19 7.41 -6 5 0 132.10 8.08 7 -5 0 14.34 3.69 -7 -5 0 9.92 2.57 -7 -5 0 14.92 4.55 -7 5 0 14.96 3.42 7 5 0 16.48 3.10 -7 5 0 10.15 4.43 7 5 0 11.69 4.25 -7 5 0 11.04 3.44 -7 5 0 13.43 3.72 -7 5 0 11.93 3.04 -8 -5 0 15.40 3.10 8 -5 0 18.78 4.43 -8 -5 0 26.88 5.77 8 5 0 21.39 5.31 -8 5 0 16.92 3.24 -8 5 0 23.89 4.33 -8 5 0 17.60 4.20 8 5 0 19.73 3.61 -9 -5 0 15.93 4.89 9 -5 0 26.75 5.49 -9 -5 0 23.57 3.69 -9 5 0 20.80 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-1 -4 -19 -1.87 1.62 1 -4 19 -5.17 4.68 1 -4 19 -3.97 3.12 1 4 19 7.12 5.82 -1 4 -19 2.53 5.45 0 -5 19 15.41 5.83 0 5 19 24.84 7.49 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 0.3323 _exptl_absorpt_correction_T_min 0.1931 _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 0.71079 8.982 14.104 15.852 90.001 90.715 89.985 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 78276 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 15:42:38 on 10-Apr-2022 CELL 0.71073 8.9784 14.0971 15.8485 90.000 90.689 90.000 ZERR 4.00 0.0003 0.0004 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C BR FE HG UNIT 40 40 4 4 OMIT -1 0 1 OMIT 0 0 2 OMIT 1 0 1 SIZE 0.06 0.02 0.02 TEMP 22 MERG 2 FMAP 2 PLAN 5 ACTA BOND LIST 4 L.S. 64 WGHT 0.032100 17.684601 FVAR 0.10967 C1 1 0.372846 0.614391 0.469127 11.00000 0.05475 0.05336 = 0.03504 0.01760 0.01339 0.01230 C2 1 0.321941 0.542498 0.411854 11.00000 0.03792 0.03865 = 0.06122 0.02393 0.00007 0.00116 C3 1 0.437841 0.523781 0.354501 11.00000 0.03765 0.02905 = 0.04895 -0.00011 -0.00926 -0.00044 C4 1 0.561789 0.583795 0.375421 11.00000 0.03642 0.03491 = 0.04163 0.00203 0.00254 0.00095 C5 1 0.520533 0.640068 0.445107 11.00000 0.05184 0.03744 = 0.03453 0.00116 -0.00743 0.00309 C6 1 0.198450 0.747122 0.324600 11.00000 0.03661 0.03795 = 0.03698 0.00908 -0.00015 0.00622 C7 1 0.222731 0.689606 0.253819 11.00000 0.04205 0.03927 = 0.03293 0.00594 -0.00406 0.00154 C8 1 0.369208 0.710256 0.225673 11.00000 0.04626 0.03992 = 0.02988 0.00192 0.00264 0.00213 C9 1 0.432400 0.779334 0.278900 11.00000 0.03949 0.03533 = 0.03319 0.01093 0.00114 -0.00185 C10 1 0.327608 0.804095 0.341803 11.00000 0.04213 0.02807 = 0.04196 0.00599 -0.00256 -0.00050 BR1 2 0.270252 0.665419 0.559284 11.00000 0.09752 0.10860 = 0.04304 0.01618 0.03003 0.04433 BR2 2 0.139189 0.481436 0.415846 11.00000 0.04530 0.08256 = 0.13660 0.05309 0.00295 -0.01780 BR3 2 0.438415 0.431416 0.271387 11.00000 0.09653 0.04418 = 0.08187 -0.02331 -0.02751 0.00149 BR4 2 0.743605 0.581603 0.321528 11.00000 0.03804 0.06720 = 0.08489 -0.00396 0.01314 0.00440 BR5 2 0.641988 0.730952 0.498689 11.00000 0.08533 0.05035 = 0.06062 -0.01665 -0.03029 0.00062 BR6 2 0.020296 0.756511 0.385215 11.00000 0.03870 0.06383 = 0.06725 0.00408 0.01104 0.00411 BR7 2 0.084631 0.610346 0.200248 11.00000 0.05104 0.06717 = 0.05664 -0.00581 -0.00806 -0.01222 BR8 2 0.456407 0.658626 0.128895 11.00000 0.07282 0.08403 = 0.04255 -0.00965 0.01393 -0.00538 BR9 2 0.618170 0.836821 0.264685 11.00000 0.05406 0.06140 = 0.05315 0.00078 0.01294 -0.02088 BR10 2 0.308946 1.001349 0.560501 11.00000 0.08755 0.06672 = 0.06699 -0.02100 0.01201 -0.00428 FE1 3 0.376605 0.662516 0.347202 11.00000 0.03129 0.03020 = 0.03159 0.00267 0.00341 0.00008 HG1 4 0.337518 0.897875 0.440727 11.00000 0.05853 0.04069 = 0.04876 -0.00432 0.00521 -0.00033 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.0920, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0362 for 3154 Fo > 4sig(Fo) and 0.0565 for all 4098 data REM 199 parameters refined using 0 restraints END WGHT 0.0318 17.7065 REM Highest difference peak 1.631, deepest hole -1.239, 1-sigma level 0.172 Q1 1 0.5628 0.7264 0.5292 11.00000 0.05 1.63 Q2 1 0.6777 0.7041 0.4922 11.00000 0.05 1.23 Q3 1 0.6420 0.7626 0.4751 11.00000 0.05 1.05 Q4 1 0.6295 0.7445 0.4639 11.00000 0.05 0.98 Q5 1 0.1929 0.6563 0.5428 11.00000 0.05 0.94 ; _shelx_res_checksum 29286 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 0.3728(11) 0.6144(7) 0.4691(5) 0.048(2) Uani d 1 . . C C2 0.3219(10) 0.5425(6) 0.4119(6) 0.046(2) Uani d 1 . . C C3 0.4378(9) 0.5238(6) 0.3545(6) 0.0386(19) Uani d 1 . . C C4 0.5618(9) 0.5838(6) 0.3754(5) 0.0376(19) Uani d 1 . . C C5 0.5205(10) 0.6401(6) 0.4451(5) 0.041(2) Uani d 1 . . C C6 0.1984(9) 0.7471(6) 0.3246(5) 0.0372(19) Uani d 1 . . C C7 0.2227(9) 0.6896(6) 0.2538(5) 0.0381(19) Uani d 1 . . C C8 0.3692(10) 0.7103(6) 0.2257(5) 0.0387(19) Uani d 1 . . C C9 0.4324(9) 0.7793(6) 0.2789(5) 0.0360(18) Uani d 1 . . C C10 0.3276(9) 0.8041(6) 0.3418(5) 0.0374(19) Uani d 1 . . Br Br1 0.27025(16) 0.66542(10) 0.55928(7) 0.0828(4) Uani d 1 . . Br Br2 0.13919(12) 0.48144(10) 0.41585(10) 0.0881(5) Uani d 1 . . Br Br3 0.43841(15) 0.43142(8) 0.27139(8) 0.0744(4) Uani d 1 . . Br Br4 0.74361(11) 0.58160(8) 0.32153(8) 0.0633(3) Uani d 1 . . Br Br5 0.64199(14) 0.73095(8) 0.49869(7) 0.0657(3) Uani d 1 . . Br Br6 0.02030(11) 0.75651(8) 0.38521(7) 0.0565(3) Uani d 1 . . Br Br7 0.08463(12) 0.61035(8) 0.20025(7) 0.0584(3) Uani d 1 . . Br Br8 0.45641(13) 0.65863(9) 0.12890(6) 0.0664(3) Uani d 1 . . Br Br9 0.61817(11) 0.83682(8) 0.26468(6) 0.0561(3) Uani d 1 . . Br Br10 0.30895(15) 1.00135(9) 0.56050(8) 0.0737(3) Uani d 1 . . Fe Fe1 0.37661(12) 0.66252(8) 0.34720(7) 0.0310(2) Uani d 1 . . Hg Hg1 0.33752(4) 0.89788(3) 0.44073(2) 0.04929(13) Uani d 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 C1 0.055(6) 0.053(6) 0.035(5) 0.012(5) 0.013(4) 0.018(4) C2 0.038(5) 0.039(5) 0.061(6) 0.001(4) 0.000(4) 0.024(4) C3 0.038(5) 0.029(4) 0.049(5) 0.000(4) -0.009(4) 0.000(4) C4 0.036(4) 0.035(5) 0.042(5) 0.001(4) 0.003(4) 0.002(4) C5 0.052(5) 0.037(5) 0.035(4) 0.003(4) -0.007(4) 0.001(4) C6 0.037(4) 0.038(5) 0.037(4) 0.006(4) 0.000(4) 0.009(4) C7 0.042(5) 0.039(5) 0.033(4) 0.002(4) -0.004(4) 0.006(4) C8 0.046(5) 0.040(5) 0.030(4) 0.002(4) 0.003(4) 0.002(4) C9 0.039(5) 0.035(5) 0.033(4) -0.002(4) 0.001(3) 0.011(4) C10 0.042(5) 0.028(4) 0.042(5) -0.001(4) -0.003(4) 0.006(4) Br1 0.0975(9) 0.1086(10) 0.0430(6) 0.0443(8) 0.0300(6) 0.0162(6) Br2 0.0453(6) 0.0826(9) 0.1366(12) -0.0178(6) 0.0029(7) 0.0531(9) Br3 0.0965(9) 0.0442(6) 0.0819(8) 0.0015(6) -0.0275(7) -0.0233(6) Br4 0.0380(5) 0.0672(7) 0.0849(8) 0.0044(5) 0.0131(5) -0.0040(6) Br5 0.0853(8) 0.0504(6) 0.0606(6) 0.0006(5) -0.0303(6) -0.0166(5) Br6 0.0387(5) 0.0638(6) 0.0673(6) 0.0041(4) 0.0110(5) 0.0041(5) Br7 0.0510(6) 0.0672(7) 0.0566(6) -0.0122(5) -0.0081(5) -0.0058(5) Br8 0.0728(7) 0.0840(8) 0.0426(5) -0.0054(6) 0.0139(5) -0.0096(5) Br9 0.0541(6) 0.0614(6) 0.0532(6) -0.0209(5) 0.0129(5) 0.0008(5) Br10 0.0875(9) 0.0667(7) 0.0670(7) -0.0043(6) 0.0120(6) -0.0210(6) Fe1 0.0313(6) 0.0302(6) 0.0316(6) 0.0001(5) 0.0034(4) 0.0027(5) Hg1 0.0585(2) 0.0407(2) 0.0488(2) -0.00033(17) 0.00521(17) -0.00432(17) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 . . 107.5(8) ? C5 C1 Br1 . . 125.3(8) ? C2 C1 Br1 . . 127.3(7) ? C5 C1 Fe1 . . 68.9(5) ? C2 C1 Fe1 . . 69.2(5) ? Br1 C1 Fe1 . . 127.8(5) ? C3 C2 C1 . . 107.9(8) ? C3 C2 Br2 . . 126.4(7) ? C1 C2 Br2 . . 125.6(7) ? C3 C2 Fe1 . . 69.4(5) ? C1 C2 Fe1 . . 69.8(5) ? Br2 C2 Fe1 . . 128.3(5) ? C2 C3 C4 . . 108.4(8) ? C2 C3 Br3 . . 126.6(7) ? C4 C3 Br3 . . 124.8(6) ? C2 C3 Fe1 . . 69.9(5) ? C4 C3 Fe1 . . 69.8(5) ? Br3 C3 Fe1 . . 129.7(5) ? C5 C4 C3 . . 107.6(7) ? C5 C4 Br4 . . 127.6(7) ? C3 C4 Br4 . . 124.7(6) ? C5 C4 Fe1 . . 69.3(5) ? C3 C4 Fe1 . . 69.1(5) ? Br4 C4 Fe1 . . 128.9(4) ? C4 C5 C1 . . 108.6(8) ? C4 C5 Br5 . . 125.5(7) ? C1 C5 Br5 . . 126.0(7) ? C4 C5 Fe1 . . 70.2(5) ? C1 C5 Fe1 . . 70.1(5) ? Br5 C5 Fe1 . . 126.8(5) ? C7 C6 C10 . . 110.0(7) ? C7 C6 Br6 . . 126.2(7) ? C10 C6 Br6 . . 123.7(6) ? C7 C6 Fe1 . . 70.8(5) ? C10 C6 Fe1 . . 70.2(5) ? Br6 C6 Fe1 . . 128.8(4) ? C6 C7 C8 . . 106.6(7) ? C6 C7 Br7 . . 126.9(6) ? C8 C7 Br7 . . 126.2(6) ? C6 C7 Fe1 . . 68.9(5) ? C8 C7 Fe1 . . 69.3(5) ? Br7 C7 Fe1 . . 131.0(5) ? C9 C8 C7 . . 108.8(7) ? C9 C8 Br8 . . 126.2(6) ? C7 C8 Br8 . . 124.9(6) ? C9 C8 Fe1 . . 69.7(5) ? C7 C8 Fe1 . . 69.9(5) ? Br8 C8 Fe1 . . 129.4(5) ? C8 C9 C10 . . 109.0(7) ? C8 C9 Br9 . . 125.6(6) ? C10 C9 Br9 . . 125.2(6) ? C8 C9 Fe1 . . 70.0(5) ? C10 C9 Fe1 . . 69.9(5) ? Br9 C9 Fe1 . . 129.8(4) ? C9 C10 C6 . . 105.6(7) ? C9 C10 Fe1 . . 69.3(5) ? C6 C10 Fe1 . . 68.6(5) ? C9 C10 Hg1 . . 132.1(6) ? C6 C10 Hg1 . . 122.3(6) ? Fe1 C10 Hg1 . . 126.1(4) ? C6 Fe1 C5 . . 136.1(3) ? C6 Fe1 C3 . . 142.1(3) ? C5 Fe1 C3 . . 68.8(3) ? C6 Fe1 C9 . . 68.2(3) ? C5 Fe1 C9 . . 111.9(4) ? C3 Fe1 C9 . . 137.7(4) ? C6 Fe1 C8 . . 67.8(3) ? C5 Fe1 C8 . . 141.7(4) ? C3 Fe1 C8 . . 112.1(3) ? C9 Fe1 C8 . . 40.3(3) ? C6 Fe1 C2 . . 112.5(3) ? C5 Fe1 C2 . . 69.0(4) ? C3 Fe1 C2 . . 40.6(4) ? C9 Fe1 C2 . . 177.9(4) ? C8 Fe1 C2 . . 137.9(4) ? C6 Fe1 C4 . . 176.2(4) ? C5 Fe1 C4 . . 40.6(3) ? C3 Fe1 C4 . . 41.2(3) ? C9 Fe1 C4 . . 110.5(3) ? C8 Fe1 C4 . . 113.7(3) ? C2 Fe1 C4 . . 68.9(3) ? C6 Fe1 C10 . . 41.3(3) ? C5 Fe1 C10 . . 108.6(3) ? C3 Fe1 C10 . . 176.6(3) ? C9 Fe1 C10 . . 40.8(3) ? C8 Fe1 C10 . . 68.5(3) ? C2 Fe1 C10 . . 141.0(4) ? C4 Fe1 C10 . . 135.5(3) ? C6 Fe1 C7 . . 40.3(3) ? C5 Fe1 C7 . . 176.3(4) ? C3 Fe1 C7 . . 113.6(3) ? C9 Fe1 C7 . . 68.5(3) ? C8 Fe1 C7 . . 40.8(3) ? C2 Fe1 C7 . . 110.7(4) ? C4 Fe1 C7 . . 143.0(3) ? C10 Fe1 C7 . . 69.2(3) ? C6 Fe1 C1 . . 109.9(3) ? C5 Fe1 C1 . . 41.0(4) ? C3 Fe1 C1 . . 68.6(4) ? C9 Fe1 C1 . . 140.9(4) ? C8 Fe1 C1 . . 177.2(4) ? C2 Fe1 C1 . . 41.0(4) ? C4 Fe1 C1 . . 68.7(3) ? C10 Fe1 C1 . . 110.9(4) ? C7 Fe1 C1 . . 136.4(4) ? C10 Hg1 Br10 . . 171.0(2) ? 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 . 1.431(13) ? C1 C2 . 1.432(14) ? C1 Br1 . 1.855(9) ? C1 Fe1 . 2.049(8) ? C2 C3 . 1.415(13) ? C2 Br2 . 1.855(9) ? C2 Fe1 . 2.041(8) ? C3 C4 . 1.434(11) ? C3 Br3 . 1.852(9) ? C3 Fe1 . 2.034(8) ? C4 C5 . 1.413(12) ? C4 Br4 . 1.852(8) ? C4 Fe1 . 2.044(8) ? C5 Br5 . 1.879(9) ? C5 Fe1 . 2.032(8) ? C6 C7 . 1.403(12) ? C6 C10 . 1.434(12) ? C6 Br6 . 1.880(8) ? C6 Fe1 . 2.024(8) ? C7 C8 . 1.424(12) ? C7 Br7 . 1.866(9) ? C7 Fe1 . 2.048(8) ? C8 C9 . 1.404(12) ? C8 Br8 . 1.877(8) ? C8 Fe1 . 2.041(8) ? C9 C10 . 1.422(11) ? C9 Br9 . 1.870(8) ? C9 Fe1 . 2.037(8) ? C10 Fe1 . 2.045(8) ? C10 Hg1 . 2.052(9) ? Br10 Hg1 . 2.4101(12) ? _cod_database_fobs_code 2022686