#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239119.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2239119 loop_ _publ_author_name 'Breunig, Jens M.' 'Lerner, Hans-Wolfram' 'Bats, Jan W.' _publ_section_title ; 1-(Bromomercurio)ferrocene ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m13 _journal_paper_doi 10.1107/S1600536813032923 _journal_volume 70 _journal_year 2014 _chemical_formula_iupac '[Fe Hg Br (C5 H5) (C5 H4)]' _chemical_formula_moiety 'C10 H9 Br Fe Hg' _chemical_formula_sum 'C10 H9 Br Fe Hg' _chemical_formula_weight 465.52 _chemical_name_systematic ; 1-(Bromomercurio)ferrocene ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 75.120(12) _cell_angle_beta 87.548(12) _cell_angle_gamma 83.298(12) _cell_formula_units_Z 4 _cell_length_a 7.6484(14) _cell_length_b 9.5715(17) _cell_length_c 14.394(3) _cell_measurement_reflns_used 153 _cell_measurement_temperature 166(2) _cell_measurement_theta_max 23 _cell_measurement_theta_min 3 _cell_volume 1011.4(3) _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 166(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'Siemens SMART 1K CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16880 _diffrn_reflns_theta_full 29.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.21 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 1200 _diffrn_standards_number 299 _exptl_absorpt_coefficient_mu 20.492 _exptl_absorpt_correction_T_max 0.361 _exptl_absorpt_correction_T_min 0.010 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(SHELXTL; Sheldrick, 2008)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 3.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blade _exptl_crystal_F_000 840 _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _refine_diff_density_max 2.778 _refine_diff_density_min -1.928 _refine_ls_extinction_coef 0.0014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 2008)' _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 5759 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.095 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0349 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.037P)^2^+4P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.0907 _reflns_number_gt 4942 _reflns_number_total 5759 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL bm in P-1 CELL 0.71073 7.6484 9.5715 14.3939 75.120 87.548 83.298 ZERR 4.00 0.0014 0.0017 0.0027 0.012 0.012 0.012 LATT 1 SFAC C H FE BR HG UNIT 40 36 4 4 4 OMIT 0 0 1 OMIT -2 60 TEMP -107 L.S. 8 BOND $H FMAP 2 PLAN 20 CONF ACTA REM bm in P-1 REM R1 = 0.1709 for 4115 Fo > 4sig(Fo) and 0.2017 for all 6574 data REM 25 parameters refined using 0 restraints REM bm in P-1 REM R1 = 0.1343 for 4115 Fo > 4sig(Fo) and 0.1660 for all 6574 data REM 97 parameters refined using 0 restraints REM bm in P-1 REM R1 = 0.0421 for 5502 Fo > 4sig(Fo) and 0.0554 for all 6573 data REM 135 parameters refined using 0 restraints REM bm in P-1 REM R1 = 0.0405 for 5502 Fo > 4sig(Fo) and 0.0537 for all 6573 data REM 235 parameters refined using 0 restraints WGHT 0.037000 4.000000 EXTI 0.001425 FVAR 0.21125 HG1 5 0.247512 0.034900 0.406074 11.00000 0.03585 0.02139 = 0.02352 -0.00357 0.00906 -0.00544 HG2 5 0.281077 0.386062 0.552272 11.00000 0.02487 0.02667 = 0.01967 -0.00630 0.00183 0.00328 BR1 4 0.187128 0.047949 0.572429 11.00000 0.06665 0.02925 = 0.02696 -0.00856 0.01307 -0.00797 BR2 4 0.559282 0.296526 0.484715 11.00000 0.02712 0.03116 = 0.03100 -0.01037 0.00383 0.00505 FE1 3 0.451197 0.136449 0.162705 11.00000 0.01585 0.01691 = 0.01822 -0.00230 0.00031 -0.00338 FE2 3 0.013469 0.412283 0.761909 11.00000 0.01650 0.01648 = 0.01837 -0.00476 0.00090 -0.00269 C1 1 0.285844 0.027507 0.265781 11.00000 0.02380 0.02043 = 0.02331 -0.00230 0.00789 -0.00956 C2 1 0.189855 0.112672 0.183978 11.00000 0.01673 0.02530 = 0.03278 -0.00506 0.00115 -0.00682 AFIX 43 H2A 2 0.097869 0.188298 0.184504 11.00000 -1.20000 AFIX 0 C3 1 0.254310 0.065938 0.101137 11.00000 0.02711 0.03141 = 0.02398 -0.00229 -0.00458 -0.01290 AFIX 43 H3A 2 0.212972 0.104577 0.037366 11.00000 -1.20000 AFIX 0 C4 1 0.391894 -0.049164 0.131316 11.00000 0.03390 0.02235 = 0.02780 -0.01088 -0.00017 -0.00819 AFIX 43 H4A 2 0.458457 -0.101024 0.091178 11.00000 -1.20000 AFIX 0 C5 1 0.412123 -0.072902 0.233227 11.00000 0.02727 0.01850 = 0.02380 -0.00226 0.00210 -0.00393 AFIX 43 H5A 2 0.494826 -0.142969 0.272184 11.00000 -1.20000 AFIX 0 C6 1 0.578058 0.273969 0.217555 11.00000 0.03047 0.03701 = 0.03048 -0.01533 0.00304 -0.01602 AFIX 43 H6A 2 0.563539 0.286939 0.280795 11.00000 -1.20000 AFIX 0 C7 1 0.479338 0.353871 0.136250 11.00000 0.02698 0.01569 = 0.04223 -0.00318 0.00190 -0.00584 AFIX 43 H7A 2 0.388074 0.430544 0.135396 11.00000 -1.20000 AFIX 0 C8 1 0.540493 0.299432 0.055799 11.00000 0.03005 0.02518 = 0.02469 0.00297 0.00250 -0.01263 AFIX 43 H8A 2 0.496914 0.332344 -0.007827 11.00000 -1.20000 AFIX 0 C9 1 0.678642 0.186891 0.088672 11.00000 0.02358 0.02955 = 0.02813 -0.00825 0.00964 -0.00716 AFIX 43 H9A 2 0.744330 0.131281 0.050462 11.00000 -1.20000 AFIX 0 C10 1 0.702080 0.171459 0.188209 11.00000 0.01632 0.03307 = 0.03340 -0.00212 -0.00030 -0.00843 AFIX 43 H10A 2 0.786155 0.104208 0.228085 11.00000 -1.20000 AFIX 0 C11 1 0.054147 0.452393 0.616723 11.00000 0.02288 0.02428 = 0.01861 -0.00458 0.00122 -0.00083 C12 1 -0.090439 0.369094 0.645105 11.00000 0.02600 0.03165 = 0.02593 -0.01215 -0.00702 -0.00345 AFIX 43 H12A 2 -0.099207 0.275731 0.635305 11.00000 -1.20000 AFIX 0 C13 1 -0.219997 0.449717 0.690790 11.00000 0.01977 0.03248 = 0.03421 -0.01193 -0.00487 -0.00061 AFIX 43 H13A 2 -0.329568 0.419493 0.717090 11.00000 -1.20000 AFIX 0 C14 1 -0.154796 0.584695 0.689808 11.00000 0.02480 0.02506 = 0.03305 -0.00464 0.00625 0.00492 AFIX 43 H14A 2 -0.213838 0.660063 0.715157 11.00000 -1.20000 AFIX 0 C15 1 0.014089 0.585715 0.644111 11.00000 0.02464 0.02029 = 0.02506 -0.00408 0.00730 0.00162 AFIX 43 H15A 2 0.087410 0.662020 0.633672 11.00000 -1.20000 AFIX 0 C16 1 0.163465 0.231321 0.835199 11.00000 0.04217 0.02665 = 0.02707 -0.00381 -0.00802 0.00702 AFIX 43 H16A 2 0.208145 0.151468 0.810053 11.00000 -1.20000 AFIX 0 C17 1 -0.000782 0.246363 0.883149 11.00000 0.04246 0.03223 = 0.02808 0.00773 -0.00897 -0.01779 AFIX 43 H17A 2 -0.085044 0.178093 0.896208 11.00000 -1.20000 AFIX 0 C18 1 -0.017083 0.381147 0.908151 11.00000 0.02817 0.04939 = 0.02549 -0.01108 0.00314 -0.00763 AFIX 43 H18A 2 -0.114918 0.419621 0.940250 11.00000 -1.20000 AFIX 0 C19 1 0.138696 0.448970 0.876802 11.00000 0.03465 0.03595 = 0.02779 -0.01284 -0.00574 -0.01060 AFIX 43 H19A 2 0.164103 0.539942 0.884842 11.00000 -1.20000 AFIX 0 C20 1 0.249034 0.355625 0.831327 11.00000 0.01993 0.04144 = 0.02975 -0.00309 -0.00420 -0.00181 AFIX 43 H20A 2 0.361388 0.373767 0.803087 11.00000 -1.20000 HKLF 4 REM bm in P-1 REM R1 = 0.0349 for 4942 Fo > 4sig(Fo) and 0.0449 for all 5759 data REM 236 parameters refined using 0 restraints END WGHT 0.0372 4.0390 REM Highest difference peak 2.778, deepest hole -1.928, 1-sigma level 0.277 Q1 1 0.3340 0.3337 0.6017 11.00000 0.05 2.78 Q2 1 0.1964 0.0826 0.3573 11.00000 0.05 2.78 Q3 1 0.2272 0.4433 0.4994 11.00000 0.05 2.60 Q4 1 0.3146 -0.0175 0.4617 11.00000 0.05 2.29 Q5 1 0.1953 0.4203 0.6037 11.00000 0.05 1.71 Q6 1 0.1765 0.0743 0.4586 11.00000 0.05 1.66 Q7 1 0.3221 0.2869 0.5552 11.00000 0.05 1.61 Q8 1 0.2444 0.4626 0.5528 11.00000 0.05 1.54 Q9 1 0.2596 -0.0192 0.3387 11.00000 0.05 1.51 Q10 1 0.2923 -0.0579 0.4102 11.00000 0.05 1.47 Q11 1 0.5184 0.3556 0.4297 11.00000 0.05 1.41 Q12 1 0.2968 0.4267 0.6117 11.00000 0.05 1.40 Q13 1 0.2907 0.3411 0.4853 11.00000 0.05 1.38 Q14 1 0.3306 -0.0021 0.3558 11.00000 0.05 1.37 Q15 1 0.1452 0.1020 0.5182 11.00000 0.05 1.32 Q16 1 0.3694 0.3601 0.4998 11.00000 0.05 1.27 Q17 1 0.3628 0.0747 0.3279 11.00000 0.05 1.23 Q18 1 0.3219 0.1332 0.3559 11.00000 0.05 1.17 Q19 1 0.2077 0.1274 0.4026 11.00000 0.05 1.16 Q20 1 0.2496 0.3447 0.4984 11.00000 0.05 1.14 ; _cod_data_source_file nc2322sup1.cf _cod_data_source_block I _cod_original_cell_volume 1011.3(3) _cod_database_code 2239119 _cod_database_fobs_code 2239119 loop_ _symmetry_equiv_pos_as_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_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity Hg Hg1 0.24751(3) 0.03490(2) 0.406074(17) 0.02741(8) Uani d . 1 1 Hg Hg2 0.28108(3) 0.38606(2) 0.552272(16) 0.02422(8) Uani d . 1 1 Br Br1 0.18713(12) 0.04795(8) 0.57243(5) 0.04088(18) Uani d . 1 1 Br Br2 0.55928(8) 0.29653(7) 0.48471(5) 0.03010(14) Uani d . 1 1 Fe Fe1 0.45120(10) 0.13645(8) 0.16271(6) 0.01728(15) Uani d . 1 1 Fe Fe2 0.01347(10) 0.41228(8) 0.76191(6) 0.01701(15) Uani d . 1 1 C C1 0.2858(7) 0.0275(6) 0.2658(4) 0.0228(11) Uani d . 1 1 C C2 0.1899(7) 0.1127(7) 0.1840(5) 0.0250(12) Uani d . 1 1 H H2A 0.0979 0.1883 0.1845 0.030 Uiso calc R 1 1 C C3 0.2543(8) 0.0659(7) 0.1011(5) 0.0275(12) Uani d . 1 1 H H3A 0.2130 0.1046 0.0374 0.033 Uiso calc R 1 1 C C4 0.3919(8) -0.0492(7) 0.1313(5) 0.0268(12) Uani d . 1 1 H H4A 0.4585 -0.1010 0.0912 0.032 Uiso calc R 1 1 C C5 0.4121(8) -0.0729(6) 0.2332(5) 0.0237(11) Uani d . 1 1 H H5A 0.4948 -0.1430 0.2722 0.028 Uiso calc R 1 1 C C6 0.5781(8) 0.2740(8) 0.2176(5) 0.0305(13) Uani d . 1 1 H H6A 0.5635 0.2869 0.2808 0.037 Uiso calc R 1 1 C C7 0.4793(8) 0.3539(6) 0.1362(5) 0.0289(13) Uani d . 1 1 H H7A 0.3881 0.4305 0.1354 0.035 Uiso calc R 1 1 C C8 0.5405(8) 0.2994(7) 0.0558(5) 0.0277(12) Uani d . 1 1 H H8A 0.4969 0.3323 -0.0078 0.033 Uiso calc R 1 1 C C9 0.6786(8) 0.1869(7) 0.0887(5) 0.0269(12) Uani d . 1 1 H H9A 0.7443 0.1313 0.0505 0.032 Uiso calc R 1 1 C C10 0.7021(7) 0.1715(7) 0.1882(5) 0.0283(13) Uani d . 1 1 H H10A 0.7862 0.1042 0.2281 0.034 Uiso calc R 1 1 C C11 0.0541(7) 0.4524(7) 0.6167(4) 0.0223(11) Uani d . 1 1 C C12 -0.0904(8) 0.3691(7) 0.6451(5) 0.0267(12) Uani d . 1 1 H H12A -0.0992 0.2757 0.6353 0.032 Uiso calc R 1 1 C C13 -0.2200(8) 0.4497(7) 0.6908(5) 0.0282(13) Uani d . 1 1 H H13A -0.3296 0.4195 0.7171 0.034 Uiso calc R 1 1 C C14 -0.1548(8) 0.5847(7) 0.6898(5) 0.0290(13) Uani d . 1 1 H H14A -0.2138 0.6601 0.7152 0.035 Uiso calc R 1 1 C C15 0.0141(8) 0.5857(6) 0.6441(4) 0.0242(11) Uani d . 1 1 H H15A 0.0874 0.6620 0.6337 0.029 Uiso calc R 1 1 C C16 0.1635(10) 0.2313(8) 0.8352(5) 0.0332(14) Uani d . 1 1 H H16A 0.2081 0.1515 0.8101 0.040 Uiso calc R 1 1 C C17 -0.0008(10) 0.2464(8) 0.8831(5) 0.0357(16) Uani d . 1 1 H H17A -0.0850 0.1781 0.8962 0.043 Uiso calc R 1 1 C C18 -0.0171(9) 0.3811(9) 0.9082(5) 0.0339(14) Uani d . 1 1 H H18A -0.1149 0.4196 0.9403 0.041 Uiso calc R 1 1 C C19 0.1387(9) 0.4490(8) 0.8768(5) 0.0312(13) Uani d . 1 1 H H19A 0.1641 0.5399 0.8848 0.037 Uiso calc R 1 1 C C20 0.2490(8) 0.3556(8) 0.8313(5) 0.0315(14) Uani d . 1 1 H H20A 0.3614 0.3738 0.8031 0.038 Uiso calc R 1 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 Hg1 0.03585(13) 0.02139(12) 0.02352(12) -0.00544(9) 0.00906(9) -0.00357(9) Hg2 0.02487(12) 0.02667(12) 0.01967(12) 0.00328(8) 0.00183(8) -0.00630(9) Br1 0.0666(5) 0.0293(3) 0.0270(3) -0.0080(3) 0.0131(3) -0.0086(3) Br2 0.0271(3) 0.0312(3) 0.0310(3) 0.0051(2) 0.0038(2) -0.0104(3) Fe1 0.0159(3) 0.0169(3) 0.0182(4) -0.0034(3) 0.0003(3) -0.0023(3) Fe2 0.0165(3) 0.0165(3) 0.0184(4) -0.0027(3) 0.0009(3) -0.0048(3) C1 0.024(2) 0.020(2) 0.023(3) -0.010(2) 0.008(2) -0.002(2) C2 0.017(2) 0.025(3) 0.033(3) -0.007(2) 0.001(2) -0.005(3) C3 0.027(3) 0.031(3) 0.024(3) -0.013(2) -0.005(2) -0.002(3) C4 0.034(3) 0.022(3) 0.028(3) -0.008(2) 0.000(2) -0.011(2) C5 0.027(3) 0.019(2) 0.024(3) -0.004(2) 0.002(2) -0.002(2) C6 0.030(3) 0.037(3) 0.030(3) -0.016(3) 0.003(3) -0.015(3) C7 0.027(3) 0.016(2) 0.042(4) -0.006(2) 0.002(3) -0.003(3) C8 0.030(3) 0.025(3) 0.025(3) -0.013(2) 0.003(2) 0.003(2) C9 0.024(3) 0.030(3) 0.028(3) -0.007(2) 0.010(2) -0.008(3) C10 0.016(2) 0.033(3) 0.033(3) -0.008(2) 0.000(2) -0.002(3) C11 0.023(2) 0.024(3) 0.019(3) -0.001(2) 0.001(2) -0.005(2) C12 0.026(3) 0.032(3) 0.026(3) -0.003(2) -0.007(2) -0.012(3) C13 0.020(2) 0.032(3) 0.034(3) -0.001(2) -0.005(2) -0.012(3) C14 0.025(3) 0.025(3) 0.033(3) 0.005(2) 0.006(2) -0.005(3) C15 0.025(3) 0.020(3) 0.025(3) 0.002(2) 0.007(2) -0.004(2) C16 0.042(4) 0.027(3) 0.027(3) 0.007(3) -0.008(3) -0.004(3) C17 0.042(4) 0.032(3) 0.028(3) -0.018(3) -0.009(3) 0.008(3) C18 0.028(3) 0.049(4) 0.025(3) -0.008(3) 0.003(3) -0.011(3) C19 0.035(3) 0.036(3) 0.028(3) -0.011(3) -0.006(3) -0.013(3) C20 0.020(3) 0.041(4) 0.030(3) -0.002(2) -0.004(2) -0.003(3) 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' Fe Fe 0.3463 0.8444 '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' 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 C1 Hg1 Br1 . . 177.32(17) yes C1 Hg1 Br2 . 2_656 99.46(17) ? Br1 Hg1 Br2 . 2_656 82.33(3) ? C1 Hg1 Br1 . 2_556 96.81(16) ? Br1 Hg1 Br1 . 2_556 80.94(3) ? Br2 Hg1 Br1 2_656 2_556 97.82(2) ? C11 Hg2 Br2 . . 176.42(17) yes C11 Hg2 Br2 . 2_666 94.10(17) ? Br2 Hg2 Br2 . 2_666 87.16(2) ? C11 Hg2 Br1 . . 95.97(17) ? Br2 Hg2 Br1 . . 82.77(3) ? Br2 Hg2 Br1 2_666 . 169.922(19) ? Hg1 Br1 Hg2 . . 98.97(3) ? Hg1 Br1 Hg1 . 2_556 99.06(3) ? Hg2 Br1 Hg1 . 2_556 121.04(3) ? Hg2 Br2 Hg2 . 2_666 92.84(2) ? Hg2 Br2 Hg1 . 2_656 118.45(3) ? Hg2 Br2 Hg1 2_666 2_656 128.28(2) ? C2 Fe1 C3 . . 40.9(3) ? C2 Fe1 C9 . . 157.9(3) ? C3 Fe1 C9 . . 121.0(3) ? C2 Fe1 C4 . . 68.7(3) ? C3 Fe1 C4 . . 40.8(3) ? C9 Fe1 C4 . . 105.8(3) ? C2 Fe1 C8 . . 122.1(3) ? C3 Fe1 C8 . . 104.7(3) ? C9 Fe1 C8 . . 40.6(3) ? C4 Fe1 C8 . . 119.7(3) ? C2 Fe1 C6 . . 123.9(3) ? C3 Fe1 C6 . . 158.2(3) ? C9 Fe1 C6 . . 68.1(3) ? C4 Fe1 C6 . . 160.7(3) ? C8 Fe1 C6 . . 68.5(3) ? C2 Fe1 C10 . . 160.1(3) ? C3 Fe1 C10 . . 158.3(3) ? C9 Fe1 C10 . . 40.6(3) ? C4 Fe1 C10 . . 123.2(3) ? C8 Fe1 C10 . . 68.4(3) ? C6 Fe1 C10 . . 40.4(3) ? C2 Fe1 C5 . . 68.5(2) ? C3 Fe1 C5 . . 68.9(3) ? C9 Fe1 C5 . . 122.2(3) ? C4 Fe1 C5 . . 41.1(3) ? C8 Fe1 C5 . . 156.8(3) ? C6 Fe1 C5 . . 125.4(3) ? C10 Fe1 C5 . . 108.8(3) ? C2 Fe1 C7 . . 108.0(2) ? C3 Fe1 C7 . . 121.1(3) ? C9 Fe1 C7 . . 68.1(3) ? C4 Fe1 C7 . . 156.2(3) ? C8 Fe1 C7 . . 40.7(3) ? C6 Fe1 C7 . . 40.4(3) ? C10 Fe1 C7 . . 67.9(3) ? C5 Fe1 C7 . . 161.5(3) ? C2 Fe1 C1 . . 40.7(2) ? C3 Fe1 C1 . . 69.0(3) ? C9 Fe1 C1 . . 159.2(3) ? C4 Fe1 C1 . . 68.9(3) ? C8 Fe1 C1 . . 159.6(3) ? C6 Fe1 C1 . . 109.8(3) ? C10 Fe1 C1 . . 124.4(3) ? C5 Fe1 C1 . . 40.8(2) ? C7 Fe1 C1 . . 124.8(3) ? C16 Fe2 C11 . . 112.4(3) ? C16 Fe2 C12 . . 108.9(3) ? C11 Fe2 C12 . . 40.8(2) ? C16 Fe2 C17 . . 40.7(3) ? C11 Fe2 C17 . . 142.1(3) ? C12 Fe2 C17 . . 112.4(3) ? C16 Fe2 C13 . . 134.6(3) ? C11 Fe2 C13 . . 68.9(3) ? C12 Fe2 C13 . . 40.8(3) ? C17 Fe2 C13 . . 109.3(3) ? C16 Fe2 C15 . . 142.9(3) ? C11 Fe2 C15 . . 40.8(2) ? C12 Fe2 C15 . . 68.6(3) ? C17 Fe2 C15 . . 176.2(3) ? C13 Fe2 C15 . . 68.8(3) ? C16 Fe2 C20 . . 40.5(3) ? C11 Fe2 C20 . . 110.1(3) ? C12 Fe2 C20 . . 135.1(3) ? C17 Fe2 C20 . . 68.1(3) ? C13 Fe2 C20 . . 174.7(3) ? C15 Fe2 C20 . . 114.0(3) ? C16 Fe2 C14 . . 175.3(3) ? C11 Fe2 C14 . . 68.7(2) ? C12 Fe2 C14 . . 68.7(3) ? C17 Fe2 C14 . . 135.8(3) ? C13 Fe2 C14 . . 41.0(3) ? C15 Fe2 C14 . . 40.7(2) ? C20 Fe2 C14 . . 144.0(3) ? C16 Fe2 C18 . . 68.2(3) ? C11 Fe2 C18 . . 176.5(3) ? C12 Fe2 C18 . . 142.7(3) ? C17 Fe2 C18 . . 40.4(3) ? C13 Fe2 C18 . . 113.4(3) ? C15 Fe2 C18 . . 136.8(3) ? C20 Fe2 C18 . . 68.0(3) ? C14 Fe2 C18 . . 111.0(3) ? C16 Fe2 C19 . . 68.1(3) ? C11 Fe2 C19 . . 136.3(3) ? C12 Fe2 C19 . . 175.3(3) ? C17 Fe2 C19 . . 68.0(3) ? C13 Fe2 C19 . . 143.8(3) ? C15 Fe2 C19 . . 111.4(3) ? C20 Fe2 C19 . . 40.3(3) ? C14 Fe2 C19 . . 114.6(3) ? C18 Fe2 C19 . . 40.4(3) ? C2 C1 C5 . . 107.3(5) ? C2 C1 Hg1 . . 127.8(4) ? C5 C1 Hg1 . . 124.8(5) ? C2 C1 Fe1 . . 68.9(3) ? C5 C1 Fe1 . . 69.3(3) ? Hg1 C1 Fe1 . . 129.4(3) ? C1 C2 C3 . . 109.0(5) ? C1 C2 Fe1 . . 70.4(3) ? C3 C2 Fe1 . . 69.6(3) ? C1 C2 H2A . . 125.5 ? C3 C2 H2A . . 125.5 ? Fe1 C2 H2A . . 126.1 ? C4 C3 C2 . . 107.7(5) ? C4 C3 Fe1 . . 69.7(3) ? C2 C3 Fe1 . . 69.5(3) ? C4 C3 H3A . . 126.2 ? C2 C3 H3A . . 126.2 ? Fe1 C3 H3A . . 126.2 ? C3 C4 C5 . . 107.9(6) ? C3 C4 Fe1 . . 69.4(3) ? C5 C4 Fe1 . . 69.6(3) ? C3 C4 H4A . . 126.0 ? C5 C4 H4A . . 126.0 ? Fe1 C4 H4A . . 126.5 ? C1 C5 C4 . . 108.1(5) ? C1 C5 Fe1 . . 69.9(3) ? C4 C5 Fe1 . . 69.3(3) ? C1 C5 H5A . . 126.0 ? C4 C5 H5A . . 126.0 ? Fe1 C5 H5A . . 126.4 ? C10 C6 C7 . . 108.1(6) ? C10 C6 Fe1 . . 69.9(4) ? C7 C6 Fe1 . . 70.0(3) ? C10 C6 H6A . . 125.9 ? C7 C6 H6A . . 125.9 ? Fe1 C6 H6A . . 125.8 ? C6 C7 C8 . . 108.3(6) ? C6 C7 Fe1 . . 69.6(4) ? C8 C7 Fe1 . . 69.5(3) ? C6 C7 H7A . . 125.9 ? C8 C7 H7A . . 125.9 ? Fe1 C7 H7A . . 126.6 ? C9 C8 C7 . . 107.2(6) ? C9 C8 Fe1 . . 69.4(3) ? C7 C8 Fe1 . . 69.8(3) ? C9 C8 H8A . . 126.4 ? C7 C8 H8A . . 126.4 ? Fe1 C8 H8A . . 125.9 ? C10 C9 C8 . . 108.5(6) ? C10 C9 Fe1 . . 70.0(3) ? C8 C9 Fe1 . . 69.9(3) ? C10 C9 H9A . . 125.7 ? C8 C9 H9A . . 125.7 ? Fe1 C9 H9A . . 125.9 ? C6 C10 C9 . . 107.9(6) ? C6 C10 Fe1 . . 69.7(3) ? C9 C10 Fe1 . . 69.4(3) ? C6 C10 H10A . . 126.0 ? C9 C10 H10A . . 126.0 ? Fe1 C10 H10A . . 126.4 ? C12 C11 C15 . . 107.9(5) ? C12 C11 Fe2 . . 69.7(3) ? C15 C11 Fe2 . . 69.7(3) ? C12 C11 Hg2 . . 125.1(5) ? C15 C11 Hg2 . . 126.9(4) ? Fe2 C11 Hg2 . . 124.6(3) ? C11 C12 C13 . . 108.4(6) ? C11 C12 Fe2 . . 69.6(3) ? C13 C12 Fe2 . . 69.6(4) ? C11 C12 H12A . . 125.8 ? C13 C12 H12A . . 125.8 ? Fe2 C12 H12A . . 126.6 ? C12 C13 C14 . . 107.6(6) ? C12 C13 Fe2 . . 69.5(3) ? C14 C13 Fe2 . . 69.6(4) ? C12 C13 H13A . . 126.2 ? C14 C13 H13A . . 126.2 ? Fe2 C13 H13A . . 126.3 ? C15 C14 C13 . . 107.9(5) ? C15 C14 Fe2 . . 69.6(3) ? C13 C14 Fe2 . . 69.4(4) ? C15 C14 H14A . . 126.0 ? C13 C14 H14A . . 126.0 ? Fe2 C14 H14A . . 126.6 ? C14 C15 C11 . . 108.2(5) ? C14 C15 Fe2 . . 69.7(4) ? C11 C15 Fe2 . . 69.4(3) ? C14 C15 H15A . . 125.9 ? C11 C15 H15A . . 125.9 ? Fe2 C15 H15A . . 126.5 ? C20 C16 C17 . . 108.1(6) ? C20 C16 Fe2 . . 70.3(4) ? C17 C16 Fe2 . . 70.1(4) ? C20 C16 H16A . . 125.9 ? C17 C16 H16A . . 125.9 ? Fe2 C16 H16A . . 125.2 ? C18 C17 C16 . . 107.9(6) ? C18 C17 Fe2 . . 70.2(4) ? C16 C17 Fe2 . . 69.2(4) ? C18 C17 H17A . . 126.0 ? C16 C17 H17A . . 126.0 ? Fe2 C17 H17A . . 126.1 ? C17 C18 C19 . . 108.1(6) ? C17 C18 Fe2 . . 69.4(4) ? C19 C18 Fe2 . . 70.4(4) ? C17 C18 H18A . . 125.9 ? C19 C18 H18A . . 125.9 ? Fe2 C18 H18A . . 125.9 ? C20 C19 C18 . . 107.4(6) ? C20 C19 Fe2 . . 68.9(4) ? C18 C19 Fe2 . . 69.2(4) ? C20 C19 H19A . . 126.3 ? C18 C19 H19A . . 126.3 ? Fe2 C19 H19A . . 127.1 ? C16 C20 C19 . . 108.4(6) ? C16 C20 Fe2 . . 69.2(4) ? C19 C20 Fe2 . . 70.8(4) ? C16 C20 H20A . . 125.8 ? C19 C20 H20A . . 125.8 ? Fe2 C20 H20A . . 125.8 ? 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 Hg1 C1 . 2.046(6) yes Hg1 Br1 . 2.4511(9) yes Hg1 Br2 2_656 3.3558(9) yes Hg1 Br1 2_556 3.4895(11) yes Hg2 C11 . 2.045(6) yes Hg2 Br2 . 2.4562(7) yes Hg2 Br2 2_666 3.3142(9) yes Hg2 Br1 . 3.3341(10) yes Br1 Hg1 2_556 3.4895(11) ? Br2 Hg2 2_666 3.3142(9) ? Br2 Hg1 2_656 3.3558(9) ? Fe1 C2 . 2.039(5) ? Fe1 C3 . 2.041(6) ? Fe1 C9 . 2.042(6) ? Fe1 C4 . 2.045(6) ? Fe1 C8 . 2.048(6) ? Fe1 C6 . 2.048(6) ? Fe1 C10 . 2.050(6) ? Fe1 C5 . 2.050(6) ? Fe1 C7 . 2.052(6) ? Fe1 C1 . 2.059(5) ? Fe2 C16 . 2.032(7) ? Fe2 C11 . 2.042(6) ? Fe2 C12 . 2.044(6) ? Fe2 C17 . 2.045(7) ? Fe2 C13 . 2.045(6) ? Fe2 C15 . 2.046(6) ? Fe2 C20 . 2.046(6) ? Fe2 C14 . 2.048(6) ? Fe2 C18 . 2.056(7) ? Fe2 C19 . 2.071(6) ? C1 C2 . 1.425(9) ? C1 C5 . 1.432(8) ? C2 C3 . 1.427(9) ? C2 H2A . 0.9500 ? C3 C4 . 1.426(9) ? C3 H3A . 0.9500 ? C4 C5 . 1.438(9) ? C4 H4A . 0.9500 ? C5 H5A . 0.9500 ? C6 C10 . 1.415(10) ? C6 C7 . 1.416(10) ? C6 H6A . 0.9500 ? C7 C8 . 1.428(10) ? C7 H7A . 0.9500 ? C8 C9 . 1.420(9) ? C8 H8A . 0.9500 ? C9 C10 . 1.419(9) ? C9 H9A . 0.9500 ? C10 H10A . 0.9500 ? C11 C12 . 1.423(8) ? C11 C15 . 1.426(8) ? C12 C13 . 1.427(9) ? C12 H12A . 0.9500 ? C13 C14 . 1.435(9) ? C13 H13A . 0.9500 ? C14 C15 . 1.424(8) ? C14 H14A . 0.9500 ? C15 H15A . 0.9500 ? C16 C20 . 1.411(10) ? C16 C17 . 1.418(11) ? C16 H16A . 0.9500 ? C17 C18 . 1.416(11) ? C17 H17A . 0.9500 ? C18 C19 . 1.424(9) ? C18 H18A . 0.9500 ? C19 C20 . 1.420(10) ? C19 H19A . 0.9500 ? C20 H20A . 0.9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C3 H3A Cg2 1_554 0.95 2.91 3.794(8) 156 C19 H19A Cg1 2_666 0.95 2.78 3.618(8) 148 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 C5 C1 C2 C3 0.3(6) Hg1 C1 C2 C3 -176.7(4) Fe1 C1 C2 C3 59.1(4) C5 C1 C2 Fe1 -58.8(4) Hg1 C1 C2 Fe1 124.2(4) C1 C2 C3 C4 -0.1(6) Fe1 C2 C3 C4 59.5(4) C1 C2 C3 Fe1 -59.6(4) C2 C3 C4 C5 -0.1(6) Fe1 C3 C4 C5 59.2(4) C2 C3 C4 Fe1 -59.3(4) C2 C1 C5 C4 -0.4(6) Hg1 C1 C5 C4 176.7(4) Fe1 C1 C5 C4 -58.9(4) C2 C1 C5 Fe1 58.6(4) Hg1 C1 C5 Fe1 -124.3(4) C3 C4 C5 C1 0.3(7) Fe1 C4 C5 C1 59.4(4) C3 C4 C5 Fe1 -59.1(4) C10 C6 C7 C8 0.8(7) Fe1 C6 C7 C8 -58.9(4) C10 C6 C7 Fe1 59.7(4) C6 C7 C8 C9 -0.7(6) Fe1 C7 C8 C9 -59.6(4) C6 C7 C8 Fe1 59.0(4) C7 C8 C9 C10 0.3(7) Fe1 C8 C9 C10 -59.6(4) C7 C8 C9 Fe1 59.9(4) C7 C6 C10 C9 -0.7(7) Fe1 C6 C10 C9 59.1(4) C7 C6 C10 Fe1 -59.7(4) C8 C9 C10 C6 0.2(7) Fe1 C9 C10 C6 -59.3(4) C8 C9 C10 Fe1 59.5(4) C15 C11 C12 C13 -0.4(7) Fe2 C11 C12 C13 59.0(4) Hg2 C11 C12 C13 177.7(4) C15 C11 C12 Fe2 -59.4(4) Hg2 C11 C12 Fe2 118.7(4) C11 C12 C13 C14 0.4(7) Fe2 C12 C13 C14 59.4(5) C11 C12 C13 Fe2 -59.0(4) C12 C13 C14 C15 -0.3(8) Fe2 C13 C14 C15 59.1(5) C12 C13 C14 Fe2 -59.4(4) C13 C14 C15 C11 0.0(7) Fe2 C14 C15 C11 59.0(4) C13 C14 C15 Fe2 -59.0(5) C12 C11 C15 C14 0.3(7) Fe2 C11 C15 C14 -59.2(4) Hg2 C11 C15 C14 -177.8(5) C12 C11 C15 Fe2 59.4(4) Hg2 C11 C15 Fe2 -118.6(5) C20 C16 C17 C18 0.5(8) Fe2 C16 C17 C18 -59.8(5) C20 C16 C17 Fe2 60.3(5) C16 C17 C18 C19 -0.8(8) Fe2 C17 C18 C19 -59.9(5) C16 C17 C18 Fe2 59.1(5) C17 C18 C19 C20 0.8(8) Fe2 C18 C19 C20 -58.5(5) C17 C18 C19 Fe2 59.3(5) C17 C16 C20 C19 0.0(8) Fe2 C16 C20 C19 60.2(5) C17 C16 C20 Fe2 -60.2(5) C18 C19 C20 C16 -0.5(8) Fe2 C19 C20 C16 -59.2(5) C18 C19 C20 Fe2 58.7(5)