# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Lin, Tzu-Pin' 'Nelson, Ryan' 'Wu, Tianpin' 'Miller, Jeffery T.' 'Gabbai, F.' _publ_contact_author_email 'francois@tamu.edu, gabbai@chem.tamu.edu' _publ_section_title ; Lewis acid enhancement by juxtaposition with an onium ion: The case of a mercury stibonium complex ; # Attachment '- 2-Cl2.cif' data_2-Cl2 _database_code_depnum_ccdc_archive 'CCDC 853646' #TrackingRef '- 2-Cl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-Cl2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H66 Cl2 Hg N O Sb' _chemical_formula_weight 1114.30 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' Sb Sb -0.5866 1.5461 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 11.172(3) _cell_length_b 34.082(9) _cell_length_c 12.621(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.244(3) _cell_angle_gamma 90.00 _cell_volume 4743(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 3.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6933 _exptl_absorpt_correction_T_max 0.8269 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41620 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7453 _reflns_number_gt 6060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+23.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7453 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.82904(2) 0.166167(7) 0.870562(18) 0.02199(8) Uani 1 1 d . . . Sb1 Sb 0.91537(3) 0.085230(11) 0.80532(3) 0.02062(11) Uani 1 1 d . . . Cl1 Cl 0.72059(12) 0.23968(4) 0.90587(11) 0.0175(3) Uani 1 1 d . . . Cl2 Cl 0.71481(14) 0.09830(5) 0.66541(13) 0.0294(4) Uani 1 1 d . . . C9 C 0.9930(5) 0.16490(18) 0.6941(4) 0.0229(13) Uani 1 1 d . . . C7 C 1.0602(6) 0.10230(19) 0.6333(5) 0.0286(15) Uani 1 1 d . . . H7A H 1.0622 0.0745 0.6378 0.034 Uiso 1 1 calc R . . C46 C 0.4461(6) 0.14332(19) 0.4777(5) 0.0351(17) Uani 1 1 d . . . H46A H 0.5296 0.1330 0.4825 0.042 Uiso 1 1 calc R . . H46B H 0.4145 0.1348 0.5430 0.042 Uiso 1 1 calc R . . N1 N 0.5555(4) 0.20554(14) 0.5511(4) 0.0244(12) Uani 1 1 d . . . C12 C 0.6848(6) 0.1565(2) 1.0499(5) 0.0305(15) Uani 1 1 d . . . H12A H 0.6915 0.1843 1.0510 0.037 Uiso 1 1 calc R . . C11 C 0.7398(5) 0.13563(17) 0.9783(5) 0.0221(14) Uani 1 1 d . . . C8 C 0.9957(5) 0.12315(17) 0.6978(5) 0.0224(14) Uani 1 1 d . . . C14 C 0.6071(6) 0.0989(2) 1.1201(5) 0.0337(16) Uani 1 1 d . . . H14A H 0.5617 0.0867 1.1685 0.040 Uiso 1 1 calc R . . C41 C 0.5420(5) 0.24973(18) 0.5404(5) 0.0286(15) Uani 1 1 d . . . H41A H 0.5372 0.2568 0.4637 0.034 Uiso 1 1 calc R . . H41B H 0.4644 0.2575 0.5628 0.034 Uiso 1 1 calc R . . C22 C 1.0454(5) 0.00703(17) 0.7873(5) 0.0264(14) Uani 1 1 d . . . H22A H 1.0924 0.0155 0.8528 0.032 Uiso 1 1 calc R . . C1 C 0.9288(5) 0.18917(17) 0.7591(5) 0.0211(13) Uani 1 1 d . . . C28 C 1.0603(6) 0.07482(18) 1.0360(5) 0.0277(15) Uani 1 1 d . . . H28A H 0.9847 0.0652 1.0506 0.033 Uiso 1 1 calc R . . C21 C 0.9491(5) 0.02971(17) 0.7383(5) 0.0247(14) Uani 1 1 d . . . C10 C 1.0578(5) 0.18360(18) 0.6193(5) 0.0243(14) Uani 1 1 d . . . C19 C 0.7313(5) 0.09421(18) 0.9761(5) 0.0249(14) Uani 1 1 d . . . C5 C 1.1217(6) 0.16079(19) 0.5529(5) 0.0291(15) Uani 1 1 d . . . H5A H 1.1636 0.1734 0.5027 0.035 Uiso 1 1 calc R . . C18 C 0.7866(5) 0.06816(18) 0.9086(5) 0.0256(14) Uani 1 1 d . . . C16 C 0.6994(6) 0.0119(2) 0.9806(5) 0.0354(17) Uani 1 1 d . . . H16A H 0.6879 -0.0158 0.9804 0.042 Uiso 1 1 calc R . . C6 C 1.1237(6) 0.1214(2) 0.5603(5) 0.0321(16) Uani 1 1 d . . . H6A H 1.1679 0.1064 0.5162 0.039 Uiso 1 1 calc R . . C20 C 0.6606(5) 0.07547(18) 1.0485(5) 0.0254(14) Uani 1 1 d . . . C27 C 1.0694(5) 0.08824(16) 0.9329(5) 0.0229(14) Uani 1 1 d . . . C4 C 1.0572(6) 0.22482(18) 0.6088(5) 0.0287(15) Uani 1 1 d . . . H4A H 1.1002 0.2370 0.5585 0.034 Uiso 1 1 calc R . . C33 C 0.5516(5) 0.19276(19) 0.6656(5) 0.0264(14) Uani 1 1 d . . . H33A H 0.5541 0.1637 0.6681 0.032 Uiso 1 1 calc R . . H33B H 0.6259 0.2025 0.7116 0.032 Uiso 1 1 calc R . . C24 C 1.0049(6) -0.04026(19) 0.6462(6) 0.0383(17) Uani 1 1 d . . . H24A H 1.0244 -0.0642 0.6145 0.046 Uiso 1 1 calc R . . C25 C 0.9089(6) -0.01821(19) 0.5974(5) 0.0341(16) Uani 1 1 d . . . H25A H 0.8621 -0.0270 0.5321 0.041 Uiso 1 1 calc R . . C29 C 1.1590(6) 0.0753(2) 1.1165(5) 0.0355(17) Uani 1 1 d . . . H29A H 1.1516 0.0661 1.1862 0.043 Uiso 1 1 calc R . . C17 C 0.7707(6) 0.02869(18) 0.9114(5) 0.0289(15) Uani 1 1 d . . . H17A H 0.8086 0.0123 0.8657 0.035 Uiso 1 1 calc R . . C2 C 0.9316(5) 0.22890(17) 0.7444(5) 0.0239(14) Uani 1 1 d . . . H2A H 0.8881 0.2451 0.7863 0.029 Uiso 1 1 calc R . . C23 C 1.0732(6) -0.02787(19) 0.7411(5) 0.0343(16) Uani 1 1 d . . . H23A H 1.1393 -0.0433 0.7746 0.041 Uiso 1 1 calc R . . C31 C 1.2792(6) 0.10263(18) 0.9951(5) 0.0292(15) Uani 1 1 d . . . H31A H 1.3548 0.1123 0.9808 0.035 Uiso 1 1 calc R . . C13 C 0.6192(6) 0.1382(2) 1.1212(5) 0.0337(16) Uani 1 1 d . . . H13A H 0.5830 0.1535 1.1706 0.040 Uiso 1 1 calc R . . C37 C 0.6757(5) 0.19218(18) 0.5221(5) 0.0277(15) Uani 1 1 d . . . H37A H 0.6867 0.1640 0.5403 0.033 Uiso 1 1 calc R . . H37B H 0.7417 0.2068 0.5670 0.033 Uiso 1 1 calc R . . C32 C 1.1798(6) 0.10216(18) 0.9148(5) 0.0279(15) Uani 1 1 d . . . H32A H 1.1877 0.1117 0.8455 0.033 Uiso 1 1 calc R . . C39 C 0.8111(6) 0.1847(2) 0.3826(6) 0.0395(18) Uani 1 1 d . . . H39A H 0.8748 0.1983 0.4330 0.047 Uiso 1 1 calc R . . H39B H 0.8198 0.1929 0.3089 0.047 Uiso 1 1 calc R . . C15 C 0.6468(6) 0.03445(19) 1.0478(5) 0.0323(16) Uani 1 1 d . . . H15A H 0.5997 0.0225 1.0953 0.039 Uiso 1 1 calc R . . C45 C 0.4505(6) 0.18755(18) 0.4757(5) 0.0285(15) Uani 1 1 d . . . H45A H 0.3738 0.1979 0.4945 0.034 Uiso 1 1 calc R . . H45B H 0.4554 0.1961 0.4016 0.034 Uiso 1 1 calc R . . C26 C 0.8801(6) 0.01674(19) 0.6430(5) 0.0306(15) Uani 1 1 d . . . H26A H 0.8133 0.0319 0.6094 0.037 Uiso 1 1 calc R . . C30 C 1.2689(6) 0.08911(19) 1.0955(5) 0.0324(16) Uani 1 1 d . . . H30A H 1.3375 0.0893 1.1507 0.039 Uiso 1 1 calc R . . C34 C 0.4437(6) 0.20622(19) 0.7137(5) 0.0329(16) Uani 1 1 d . . . H34A H 0.3692 0.2031 0.6601 0.040 Uiso 1 1 calc R . . H34B H 0.4529 0.2344 0.7323 0.040 Uiso 1 1 calc R . . C35 C 0.4310(6) 0.18295(19) 0.8135(5) 0.0355(17) Uani 1 1 d . . . H35A H 0.4086 0.1556 0.7930 0.043 Uiso 1 1 calc R . . H35B H 0.5101 0.1824 0.8619 0.043 Uiso 1 1 calc R . . C42 C 0.6430(6) 0.27309(18) 0.6050(5) 0.0320(16) Uani 1 1 d . . . H42A H 0.7177 0.2702 0.5728 0.038 Uiso 1 1 calc R . . H42B H 0.6597 0.2626 0.6791 0.038 Uiso 1 1 calc R . . C3 C 0.9952(6) 0.24702(19) 0.6706(5) 0.0318(15) Uani 1 1 d . . . H3A H 0.9949 0.2748 0.6641 0.038 Uiso 1 1 calc R . . C47 C 0.3687(6) 0.1259(2) 0.3813(5) 0.0387(17) Uani 1 1 d . . . H47A H 0.3975 0.1351 0.3155 0.046 Uiso 1 1 calc R . . H47B H 0.2839 0.1348 0.3784 0.046 Uiso 1 1 calc R . . C38 C 0.6886(6) 0.1977(2) 0.4050(5) 0.0341(16) Uani 1 1 d . . . H38A H 0.6247 0.1824 0.3594 0.041 Uiso 1 1 calc R . . H38B H 0.6765 0.2257 0.3857 0.041 Uiso 1 1 calc R . . C43 C 0.6104(7) 0.31635(19) 0.6084(6) 0.0382(17) Uani 1 1 d . . . H43A H 0.6851 0.3315 0.6340 0.046 Uiso 1 1 calc R . . H43B H 0.5786 0.3252 0.5346 0.046 Uiso 1 1 calc R . . C40 C 0.8310(7) 0.1408(2) 0.3931(6) 0.0457(19) Uani 1 1 d . . . H40A H 0.9124 0.1343 0.3789 0.069 Uiso 1 1 calc R . . H40B H 0.7704 0.1272 0.3413 0.069 Uiso 1 1 calc R . . H40C H 0.8231 0.1325 0.4660 0.069 Uiso 1 1 calc R . . C36 C 0.3365(7) 0.2002(2) 0.8722(6) 0.048(2) Uani 1 1 d . . . H36A H 0.3313 0.1845 0.9364 0.072 Uiso 1 1 calc R . . H36B H 0.2577 0.2001 0.8251 0.072 Uiso 1 1 calc R . . H36C H 0.3590 0.2272 0.8934 0.072 Uiso 1 1 calc R . . C48 C 0.3727(8) 0.0808(2) 0.3851(6) 0.054(2) Uani 1 1 d . . . H48A H 0.3214 0.0702 0.3213 0.080 Uiso 1 1 calc R . . H48B H 0.3430 0.0716 0.4497 0.080 Uiso 1 1 calc R . . H48C H 0.4564 0.0719 0.3867 0.080 Uiso 1 1 calc R . . C44 C 0.5183(8) 0.3254(2) 0.6793(7) 0.056(2) Uani 1 1 d . . . H44A H 0.5009 0.3536 0.6766 0.084 Uiso 1 1 calc R . . H44B H 0.5503 0.3178 0.7533 0.084 Uiso 1 1 calc R . . H44C H 0.4436 0.3108 0.6542 0.084 Uiso 1 1 calc R . . O1 O 0.3122(6) 0.0386(2) 0.6257(5) 0.083(2) Uani 1 1 d . . . C51 C 0.4612(7) 0.0493(2) 0.7715(7) 0.059(2) Uani 1 1 d . . . H51A H 0.4482 0.0414 0.8443 0.071 Uiso 1 1 calc R . . H51B H 0.5249 0.0698 0.7779 0.071 Uiso 1 1 calc R . . C50 C 0.4964(8) 0.0136(3) 0.7073(8) 0.072(3) Uani 1 1 d . . . H50A H 0.5607 0.0206 0.6652 0.087 Uiso 1 1 calc R . . H50B H 0.5252 -0.0084 0.7559 0.087 Uiso 1 1 calc R . . C49 C 0.3813(10) 0.0030(3) 0.6349(9) 0.085(3) Uani 1 1 d . . . H49A H 0.3979 -0.0057 0.5639 0.101 Uiso 1 1 calc R . . H49B H 0.3378 -0.0182 0.6667 0.101 Uiso 1 1 calc R . . C52 C 0.3564(13) 0.0624(4) 0.7122(10) 0.153(7) Uani 1 1 d . . . H52B H 0.3703 0.0890 0.6852 0.183 Uiso 1 1 calc R . . H52A H 0.2940 0.0646 0.7594 0.183 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02320(13) 0.02107(13) 0.02244(13) -0.00033(10) 0.00596(9) -0.00083(10) Sb1 0.0211(2) 0.0191(2) 0.0221(2) 0.00161(17) 0.00450(17) 0.00063(17) Cl1 0.0215(7) 0.0134(7) 0.0199(7) -0.0067(6) 0.0101(6) -0.0037(6) Cl2 0.0245(8) 0.0287(9) 0.0337(9) 0.0085(7) 0.0007(7) 0.0027(7) C9 0.023(3) 0.027(3) 0.018(3) 0.003(3) 0.001(3) 0.001(3) C7 0.033(4) 0.023(3) 0.031(4) 0.000(3) 0.009(3) -0.001(3) C46 0.036(4) 0.029(4) 0.038(4) -0.002(3) -0.003(3) 0.002(3) N1 0.022(3) 0.028(3) 0.022(3) 0.003(2) 0.000(2) 0.002(2) C12 0.032(4) 0.037(4) 0.023(3) 0.002(3) 0.005(3) 0.001(3) C11 0.019(3) 0.026(3) 0.020(3) 0.004(3) 0.001(3) 0.002(3) C8 0.019(3) 0.026(3) 0.022(3) 0.003(3) 0.001(3) -0.002(3) C14 0.023(4) 0.046(5) 0.033(4) 0.011(3) 0.009(3) 0.003(3) C41 0.029(4) 0.027(4) 0.031(4) 0.005(3) 0.005(3) 0.005(3) C22 0.029(4) 0.023(3) 0.027(3) 0.003(3) 0.002(3) 0.003(3) C1 0.018(3) 0.024(3) 0.021(3) 0.000(3) 0.001(3) -0.003(3) C28 0.023(3) 0.032(4) 0.028(4) 0.002(3) 0.004(3) -0.002(3) C21 0.029(4) 0.023(3) 0.023(3) -0.001(3) 0.004(3) 0.001(3) C10 0.023(3) 0.027(4) 0.023(3) 0.006(3) 0.006(3) -0.003(3) C19 0.016(3) 0.028(4) 0.030(4) 0.011(3) 0.001(3) -0.003(3) C5 0.030(4) 0.034(4) 0.027(3) 0.002(3) 0.012(3) -0.008(3) C18 0.023(3) 0.030(4) 0.024(3) 0.006(3) 0.003(3) -0.002(3) C16 0.033(4) 0.034(4) 0.041(4) 0.010(3) 0.012(3) -0.012(3) C6 0.031(4) 0.039(4) 0.030(4) 0.000(3) 0.015(3) 0.003(3) C20 0.016(3) 0.034(4) 0.025(3) 0.006(3) 0.000(3) 0.003(3) C27 0.027(3) 0.012(3) 0.030(4) 0.000(3) 0.006(3) 0.004(3) C4 0.032(4) 0.027(4) 0.028(4) 0.005(3) 0.007(3) -0.008(3) C33 0.026(3) 0.028(4) 0.025(3) 0.003(3) 0.003(3) 0.002(3) C24 0.048(5) 0.023(4) 0.047(5) -0.007(3) 0.017(4) 0.002(3) C25 0.042(4) 0.030(4) 0.029(4) -0.008(3) 0.002(3) -0.001(3) C29 0.033(4) 0.045(4) 0.027(4) 0.005(3) 0.003(3) -0.002(3) C17 0.031(4) 0.021(4) 0.035(4) 0.003(3) 0.007(3) 0.003(3) C2 0.028(3) 0.020(3) 0.024(3) -0.004(3) 0.005(3) 0.003(3) C23 0.038(4) 0.023(4) 0.040(4) 0.002(3) 0.002(3) 0.009(3) C31 0.022(3) 0.027(4) 0.039(4) -0.002(3) 0.005(3) -0.005(3) C13 0.039(4) 0.043(4) 0.021(4) -0.001(3) 0.011(3) 0.004(3) C37 0.023(3) 0.023(4) 0.035(4) -0.001(3) 0.002(3) 0.004(3) C32 0.030(4) 0.027(4) 0.027(4) -0.003(3) 0.007(3) 0.001(3) C39 0.044(4) 0.040(4) 0.035(4) 0.002(3) 0.009(3) 0.008(3) C15 0.031(4) 0.031(4) 0.038(4) 0.006(3) 0.014(3) -0.004(3) C45 0.029(4) 0.025(4) 0.030(4) 0.004(3) 0.000(3) 0.002(3) C26 0.030(4) 0.029(4) 0.032(4) 0.001(3) 0.002(3) 0.003(3) C30 0.032(4) 0.033(4) 0.031(4) -0.003(3) -0.002(3) 0.001(3) C34 0.035(4) 0.030(4) 0.034(4) 0.003(3) 0.007(3) 0.003(3) C35 0.041(4) 0.028(4) 0.041(4) 0.003(3) 0.014(3) -0.002(3) C42 0.037(4) 0.025(4) 0.037(4) 0.001(3) 0.011(3) 0.000(3) C3 0.039(4) 0.020(3) 0.037(4) 0.002(3) 0.010(3) -0.007(3) C47 0.041(4) 0.047(5) 0.028(4) -0.007(3) 0.006(3) -0.007(3) C38 0.040(4) 0.033(4) 0.030(4) 0.008(3) 0.007(3) 0.006(3) C43 0.046(4) 0.030(4) 0.039(4) 0.004(3) 0.011(3) -0.003(3) C40 0.045(5) 0.051(5) 0.041(4) 0.000(4) 0.006(4) 0.014(4) C36 0.059(5) 0.043(5) 0.048(5) -0.007(4) 0.025(4) -0.005(4) C48 0.070(6) 0.052(5) 0.037(4) -0.012(4) 0.003(4) -0.020(4) C44 0.070(6) 0.032(5) 0.071(6) 0.005(4) 0.027(5) 0.008(4) O1 0.088(5) 0.098(5) 0.058(4) -0.013(4) -0.008(4) 0.010(4) C51 0.045(5) 0.055(6) 0.076(6) 0.008(5) 0.005(5) -0.007(4) C50 0.055(6) 0.086(7) 0.075(7) -0.008(6) 0.008(5) 0.019(5) C49 0.090(8) 0.072(7) 0.089(8) 0.001(6) 0.006(6) 0.012(6) C52 0.169(13) 0.161(13) 0.097(9) -0.075(9) -0.076(9) 0.095(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C1 2.083(6) . ? Hg1 C11 2.088(6) . ? Hg1 Cl1 2.8491(14) . ? Hg1 Sb1 3.0778(8) . ? Sb1 C21 2.131(6) . ? Sb1 C27 2.161(6) . ? Sb1 C8 2.170(6) . ? Sb1 C18 2.171(6) . ? Sb1 Cl2 2.6582(16) . ? C9 C8 1.424(8) . ? C9 C10 1.428(8) . ? C9 C1 1.436(8) . ? C7 C8 1.370(8) . ? C7 C6 1.409(8) . ? C7 H7A 0.9500 . ? C46 C47 1.498(9) . ? C46 C45 1.508(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? N1 C45 1.516(7) . ? N1 C37 1.517(7) . ? N1 C33 1.517(7) . ? N1 C41 1.517(8) . ? C12 C11 1.372(8) . ? C12 C13 1.396(9) . ? C12 H12A 0.9500 . ? C11 C19 1.415(8) . ? C14 C13 1.347(9) . ? C14 C20 1.408(9) . ? C14 H14A 0.9500 . ? C41 C42 1.509(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C22 C23 1.382(9) . ? C22 C21 1.387(8) . ? C22 H22A 0.9500 . ? C1 C2 1.368(8) . ? C28 C29 1.375(9) . ? C28 C27 1.399(8) . ? C28 H28A 0.9500 . ? C21 C26 1.392(8) . ? C10 C4 1.411(8) . ? C10 C5 1.417(8) . ? C19 C18 1.436(9) . ? C19 C20 1.449(8) . ? C5 C6 1.346(9) . ? C5 H5A 0.9500 . ? C18 C17 1.358(8) . ? C16 C15 1.348(9) . ? C16 C17 1.396(8) . ? C16 H16A 0.9500 . ? C6 H6A 0.9500 . ? C20 C15 1.406(9) . ? C27 C32 1.375(8) . ? C4 C3 1.355(9) . ? C4 H4A 0.9500 . ? C33 C34 1.506(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C24 C25 1.372(9) . ? C24 C23 1.378(9) . ? C24 H24A 0.9500 . ? C25 C26 1.383(9) . ? C25 H25A 0.9500 . ? C29 C30 1.380(9) . ? C29 H29A 0.9500 . ? C17 H17A 0.9500 . ? C2 C3 1.402(8) . ? C2 H2A 0.9500 . ? C23 H23A 0.9500 . ? C31 C30 1.371(9) . ? C31 C32 1.378(8) . ? C31 H31A 0.9500 . ? C13 H13A 0.9500 . ? C37 C38 1.518(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C32 H32A 0.9500 . ? C39 C38 1.507(9) . ? C39 C40 1.516(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C15 H15A 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C26 H26A 0.9500 . ? C30 H30A 0.9500 . ? C34 C35 1.514(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.503(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C42 C43 1.521(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C3 H3A 0.9500 . ? C47 C48 1.537(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C43 C44 1.499(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O1 C52 1.385(11) . ? O1 C49 1.433(11) . ? C51 C52 1.359(12) . ? C51 C50 1.548(12) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C50 C49 1.497(12) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C52 H52B 0.9900 . ? C52 H52A 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Hg1 C11 172.0(2) . . ? C1 Hg1 Cl1 93.53(16) . . ? C11 Hg1 Cl1 94.42(16) . . ? C1 Hg1 Sb1 86.11(16) . . ? C11 Hg1 Sb1 86.01(16) . . ? Cl1 Hg1 Sb1 171.66(3) . . ? C21 Sb1 C27 99.6(2) . . ? C21 Sb1 C8 99.4(2) . . ? C27 Sb1 C8 94.5(2) . . ? C21 Sb1 C18 100.2(2) . . ? C27 Sb1 C18 95.2(2) . . ? C8 Sb1 C18 156.3(2) . . ? C21 Sb1 Cl2 93.96(17) . . ? C27 Sb1 Cl2 166.40(15) . . ? C8 Sb1 Cl2 82.74(16) . . ? C18 Sb1 Cl2 82.80(16) . . ? C21 Sb1 Hg1 170.10(16) . . ? C27 Sb1 Hg1 90.25(15) . . ? C8 Sb1 Hg1 79.17(16) . . ? C18 Sb1 Hg1 79.22(17) . . ? Cl2 Sb1 Hg1 76.15(4) . . ? C8 C9 C10 117.3(5) . . ? C8 C9 C1 124.5(5) . . ? C10 C9 C1 118.3(5) . . ? C8 C7 C6 121.2(6) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C47 C46 C45 113.5(6) . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C45 N1 C37 110.7(5) . . ? C45 N1 C33 110.1(5) . . ? C37 N1 C33 107.8(4) . . ? C45 N1 C41 106.9(4) . . ? C37 N1 C41 110.8(5) . . ? C33 N1 C41 110.6(5) . . ? C11 C12 C13 122.0(6) . . ? C11 C12 H12A 119.0 . . ? C13 C12 H12A 119.0 . . ? C12 C11 C19 119.7(6) . . ? C12 C11 Hg1 118.8(5) . . ? C19 C11 Hg1 121.5(4) . . ? C7 C8 C9 120.6(5) . . ? C7 C8 Sb1 111.9(4) . . ? C9 C8 Sb1 127.4(4) . . ? C13 C14 C20 121.3(6) . . ? C13 C14 H14A 119.4 . . ? C20 C14 H14A 119.4 . . ? C42 C41 N1 114.9(5) . . ? C42 C41 H41A 108.5 . . ? N1 C41 H41A 108.5 . . ? C42 C41 H41B 108.5 . . ? N1 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? C23 C22 C21 120.1(6) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C2 C1 C9 117.9(5) . . ? C2 C1 Hg1 119.4(4) . . ? C9 C1 Hg1 122.7(4) . . ? C29 C28 C27 121.0(6) . . ? C29 C28 H28A 119.5 . . ? C27 C28 H28A 119.5 . . ? C22 C21 C26 119.4(6) . . ? C22 C21 Sb1 119.5(4) . . ? C26 C21 Sb1 121.1(4) . . ? C4 C10 C5 119.1(5) . . ? C4 C10 C9 120.8(6) . . ? C5 C10 C9 120.2(6) . . ? C11 C19 C18 126.5(5) . . ? C11 C19 C20 118.0(6) . . ? C18 C19 C20 115.6(5) . . ? C6 C5 C10 120.7(6) . . ? C6 C5 H5A 119.6 . . ? C10 C5 H5A 119.6 . . ? C17 C18 C19 121.8(6) . . ? C17 C18 Sb1 112.5(5) . . ? C19 C18 Sb1 125.5(4) . . ? C15 C16 C17 120.6(6) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C5 C6 C7 120.1(6) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C15 C20 C14 120.7(6) . . ? C15 C20 C19 120.3(6) . . ? C14 C20 C19 119.0(6) . . ? C32 C27 C28 117.9(6) . . ? C32 C27 Sb1 121.4(4) . . ? C28 C27 Sb1 120.6(4) . . ? C3 C4 C10 119.8(6) . . ? C3 C4 H4A 120.1 . . ? C10 C4 H4A 120.1 . . ? C34 C33 N1 116.4(5) . . ? C34 C33 H33A 108.2 . . ? N1 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? N1 C33 H33B 108.2 . . ? H33A C33 H33B 107.3 . . ? C25 C24 C23 120.4(6) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.1(6) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C28 C29 C30 119.7(6) . . ? C28 C29 H29A 120.2 . . ? C30 C29 H29A 120.2 . . ? C18 C17 C16 120.8(6) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C1 C2 C3 123.5(6) . . ? C1 C2 H2A 118.3 . . ? C3 C2 H2A 118.3 . . ? C24 C23 C22 120.0(6) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C30 C31 C32 119.9(6) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C14 C13 C12 120.0(6) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? N1 C37 C38 115.1(5) . . ? N1 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? N1 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C27 C32 C31 121.4(6) . . ? C27 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C38 C39 C40 113.4(6) . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C16 C15 C20 120.9(6) . . ? C16 C15 H15A 119.6 . . ? C20 C15 H15A 119.6 . . ? C46 C45 N1 114.7(5) . . ? C46 C45 H45A 108.6 . . ? N1 C45 H45A 108.6 . . ? C46 C45 H45B 108.6 . . ? N1 C45 H45B 108.6 . . ? H45A C45 H45B 107.6 . . ? C25 C26 C21 120.0(6) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? C31 C30 C29 120.1(6) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C33 C34 C35 111.3(5) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 111.8(6) . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35B 109.2 . . ? C34 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C41 C42 C43 111.4(6) . . ? C41 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C46 C47 C48 111.2(6) . . ? C46 C47 H47A 109.4 . . ? C48 C47 H47A 109.4 . . ? C46 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? C39 C38 C37 112.2(5) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C44 C43 C42 114.0(6) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C52 O1 C49 108.2(8) . . ? C52 C51 C50 103.8(8) . . ? C52 C51 H51A 111.0 . . ? C50 C51 H51A 111.0 . . ? C52 C51 H51B 111.0 . . ? C50 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? C49 C50 C51 104.1(7) . . ? C49 C50 H50A 110.9 . . ? C51 C50 H50A 110.9 . . ? C49 C50 H50B 110.9 . . ? C51 C50 H50B 110.9 . . ? H50A C50 H50B 109.0 . . ? O1 C49 C50 104.1(8) . . ? O1 C49 H49A 110.9 . . ? C50 C49 H49A 110.9 . . ? O1 C49 H49B 110.9 . . ? C50 C49 H49B 110.9 . . ? H49A C49 H49B 109.0 . . ? C51 C52 O1 114.1(10) . . ? C51 C52 H52B 108.7 . . ? O1 C52 H52B 108.7 . . ? C51 C52 H52A 108.7 . . ? O1 C52 H52A 108.7 . . ? H52B C52 H52A 107.6 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Hg1 Sb1 C21 -85.0(10) . . . . ? C11 Hg1 Sb1 C21 96.0(10) . . . . ? Cl1 Hg1 Sb1 C21 2.8(10) . . . . ? C1 Hg1 Sb1 C27 92.1(2) . . . . ? C11 Hg1 Sb1 C27 -86.9(2) . . . . ? Cl1 Hg1 Sb1 C27 179.9(2) . . . . ? C1 Hg1 Sb1 C8 -2.4(2) . . . . ? C11 Hg1 Sb1 C8 178.6(2) . . . . ? Cl1 Hg1 Sb1 C8 85.4(2) . . . . ? C1 Hg1 Sb1 C18 -172.6(2) . . . . ? C11 Hg1 Sb1 C18 8.4(2) . . . . ? Cl1 Hg1 Sb1 C18 -84.8(3) . . . . ? C1 Hg1 Sb1 Cl2 -87.46(16) . . . . ? C11 Hg1 Sb1 Cl2 93.53(16) . . . . ? Cl1 Hg1 Sb1 Cl2 0.3(2) . . . . ? C13 C12 C11 C19 -0.4(9) . . . . ? C13 C12 C11 Hg1 177.3(5) . . . . ? C1 Hg1 C11 C12 166.1(14) . . . . ? Cl1 Hg1 C11 C12 -15.1(5) . . . . ? Sb1 Hg1 C11 C12 173.3(5) . . . . ? C1 Hg1 C11 C19 -16.3(19) . . . . ? Cl1 Hg1 C11 C19 162.6(4) . . . . ? Sb1 Hg1 C11 C19 -9.0(4) . . . . ? C6 C7 C8 C9 -1.2(9) . . . . ? C6 C7 C8 Sb1 -177.5(5) . . . . ? C10 C9 C8 C7 1.3(9) . . . . ? C1 C9 C8 C7 -179.5(6) . . . . ? C10 C9 C8 Sb1 177.0(4) . . . . ? C1 C9 C8 Sb1 -3.8(9) . . . . ? C21 Sb1 C8 C7 -10.2(5) . . . . ? C27 Sb1 C8 C7 90.4(5) . . . . ? C18 Sb1 C8 C7 -155.8(5) . . . . ? Cl2 Sb1 C8 C7 -103.0(4) . . . . ? Hg1 Sb1 C8 C7 179.8(4) . . . . ? C21 Sb1 C8 C9 173.8(5) . . . . ? C27 Sb1 C8 C9 -85.6(5) . . . . ? C18 Sb1 C8 C9 28.2(9) . . . . ? Cl2 Sb1 C8 C9 81.0(5) . . . . ? Hg1 Sb1 C8 C9 3.8(5) . . . . ? C45 N1 C41 C42 -176.6(5) . . . . ? C37 N1 C41 C42 -56.0(7) . . . . ? C33 N1 C41 C42 63.6(6) . . . . ? C8 C9 C1 C2 -178.1(6) . . . . ? C10 C9 C1 C2 1.1(8) . . . . ? C8 C9 C1 Hg1 0.3(8) . . . . ? C10 C9 C1 Hg1 179.4(4) . . . . ? C11 Hg1 C1 C2 -172.6(14) . . . . ? Cl1 Hg1 C1 C2 8.6(5) . . . . ? Sb1 Hg1 C1 C2 -179.8(5) . . . . ? C11 Hg1 C1 C9 9.1(19) . . . . ? Cl1 Hg1 C1 C9 -169.8(4) . . . . ? Sb1 Hg1 C1 C9 1.9(4) . . . . ? C23 C22 C21 C26 0.7(9) . . . . ? C23 C22 C21 Sb1 -175.9(5) . . . . ? C27 Sb1 C21 C22 4.6(5) . . . . ? C8 Sb1 C21 C22 100.8(5) . . . . ? C18 Sb1 C21 C22 -92.5(5) . . . . ? Cl2 Sb1 C21 C22 -175.9(5) . . . . ? Hg1 Sb1 C21 C22 -178.3(6) . . . . ? C27 Sb1 C21 C26 -172.0(5) . . . . ? C8 Sb1 C21 C26 -75.7(5) . . . . ? C18 Sb1 C21 C26 90.9(5) . . . . ? Cl2 Sb1 C21 C26 7.5(5) . . . . ? Hg1 Sb1 C21 C26 5.2(13) . . . . ? C8 C9 C10 C4 178.4(5) . . . . ? C1 C9 C10 C4 -0.8(9) . . . . ? C8 C9 C10 C5 -0.3(8) . . . . ? C1 C9 C10 C5 -179.5(5) . . . . ? C12 C11 C19 C18 -178.0(6) . . . . ? Hg1 C11 C19 C18 4.4(8) . . . . ? C12 C11 C19 C20 1.9(8) . . . . ? Hg1 C11 C19 C20 -175.7(4) . . . . ? C4 C10 C5 C6 -179.6(6) . . . . ? C9 C10 C5 C6 -0.9(9) . . . . ? C11 C19 C18 C17 -178.7(6) . . . . ? C20 C19 C18 C17 1.5(9) . . . . ? C11 C19 C18 Sb1 7.7(9) . . . . ? C20 C19 C18 Sb1 -172.2(4) . . . . ? C21 Sb1 C18 C17 5.5(5) . . . . ? C27 Sb1 C18 C17 -95.3(5) . . . . ? C8 Sb1 C18 C17 151.0(5) . . . . ? Cl2 Sb1 C18 C17 98.3(4) . . . . ? Hg1 Sb1 C18 C17 175.4(5) . . . . ? C21 Sb1 C18 C19 179.6(5) . . . . ? C27 Sb1 C18 C19 78.9(5) . . . . ? C8 Sb1 C18 C19 -34.9(9) . . . . ? Cl2 Sb1 C18 C19 -87.6(5) . . . . ? Hg1 Sb1 C18 C19 -10.4(5) . . . . ? C10 C5 C6 C7 1.0(10) . . . . ? C8 C7 C6 C5 0.0(10) . . . . ? C13 C14 C20 C15 -179.7(6) . . . . ? C13 C14 C20 C19 0.9(9) . . . . ? C11 C19 C20 C15 178.4(6) . . . . ? C18 C19 C20 C15 -1.7(8) . . . . ? C11 C19 C20 C14 -2.1(8) . . . . ? C18 C19 C20 C14 177.7(5) . . . . ? C29 C28 C27 C32 -0.5(9) . . . . ? C29 C28 C27 Sb1 177.6(5) . . . . ? C21 Sb1 C27 C32 85.4(5) . . . . ? C8 Sb1 C27 C32 -14.9(5) . . . . ? C18 Sb1 C27 C32 -173.3(5) . . . . ? Cl2 Sb1 C27 C32 -92.5(8) . . . . ? Hg1 Sb1 C27 C32 -94.1(5) . . . . ? C21 Sb1 C27 C28 -92.5(5) . . . . ? C8 Sb1 C27 C28 167.1(5) . . . . ? C18 Sb1 C27 C28 8.7(5) . . . . ? Cl2 Sb1 C27 C28 89.6(8) . . . . ? Hg1 Sb1 C27 C28 87.9(5) . . . . ? C5 C10 C4 C3 179.1(6) . . . . ? C9 C10 C4 C3 0.4(9) . . . . ? C45 N1 C33 C34 -64.3(7) . . . . ? C37 N1 C33 C34 174.9(5) . . . . ? C41 N1 C33 C34 53.6(7) . . . . ? C23 C24 C25 C26 0.1(10) . . . . ? C27 C28 C29 C30 -0.1(10) . . . . ? C19 C18 C17 C16 0.0(10) . . . . ? Sb1 C18 C17 C16 174.4(5) . . . . ? C15 C16 C17 C18 -1.4(10) . . . . ? C9 C1 C2 C3 -1.0(9) . . . . ? Hg1 C1 C2 C3 -179.4(5) . . . . ? C25 C24 C23 C22 -0.3(10) . . . . ? C21 C22 C23 C24 -0.2(10) . . . . ? C20 C14 C13 C12 0.6(10) . . . . ? C11 C12 C13 C14 -0.8(10) . . . . ? C45 N1 C37 C38 51.7(7) . . . . ? C33 N1 C37 C38 172.2(5) . . . . ? C41 N1 C37 C38 -66.6(7) . . . . ? C28 C27 C32 C31 0.6(9) . . . . ? Sb1 C27 C32 C31 -177.4(5) . . . . ? C30 C31 C32 C27 -0.2(10) . . . . ? C17 C16 C15 C20 1.1(10) . . . . ? C14 C20 C15 C16 -178.9(6) . . . . ? C19 C20 C15 C16 0.5(10) . . . . ? C47 C46 C45 N1 -161.7(5) . . . . ? C37 N1 C45 C46 61.1(7) . . . . ? C33 N1 C45 C46 -58.0(7) . . . . ? C41 N1 C45 C46 -178.1(5) . . . . ? C24 C25 C26 C21 0.4(10) . . . . ? C22 C21 C26 C25 -0.9(9) . . . . ? Sb1 C21 C26 C25 175.7(5) . . . . ? C32 C31 C30 C29 -0.4(10) . . . . ? C28 C29 C30 C31 0.6(10) . . . . ? N1 C33 C34 C35 164.0(5) . . . . ? C33 C34 C35 C36 170.8(6) . . . . ? N1 C41 C42 C43 -168.2(5) . . . . ? C10 C4 C3 C2 -0.3(10) . . . . ? C1 C2 C3 C4 0.6(10) . . . . ? C45 C46 C47 C48 177.1(6) . . . . ? C40 C39 C38 C37 67.8(8) . . . . ? N1 C37 C38 C39 178.6(5) . . . . ? C41 C42 C43 C44 73.4(8) . . . . ? C52 C51 C50 C49 -18.2(12) . . . . ? C52 O1 C49 C50 -20.9(13) . . . . ? C51 C50 C49 O1 23.5(10) . . . . ? C50 C51 C52 O1 5.9(16) . . . . ? C49 O1 C52 C51 9.6(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.188 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.120 # Attachment '- 2-DMAP3.cif' data_2-DMAP3 _database_code_depnum_ccdc_archive 'CCDC 853647' #TrackingRef '- 2-DMAP3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-DMAP3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H60 F6 Hg N6 O P Sb' _chemical_formula_weight 1312.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.171(5) _cell_length_b 28.753(8) _cell_length_c 13.422(7) _cell_angle_alpha 90.00 _cell_angle_beta 130.397(2) _cell_angle_gamma 90.00 _cell_volume 5341(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 3.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5433 _exptl_absorpt_correction_T_max 0.7685 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22894 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8248 _reflns_number_gt 7880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.038(3) _refine_ls_number_reflns 8248 _refine_ls_number_parameters 658 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg -0.478123(16) 0.827445(6) -0.327491(18) 0.03069(7) Uani 1 1 d . . . Sb1 Sb -0.51226(2) 0.927096(12) -0.42429(3) 0.02877(10) Uani 1 1 d . . . P1 P -0.44365(14) 0.42054(7) -0.27697(17) 0.0490(5) Uani 1 1 d . . . C1 C -0.3626(6) 0.82589(17) -0.3278(7) 0.0295(19) Uani 1 1 d . . . C11 C -0.6059(5) 0.8376(2) -0.3549(7) 0.0285(15) Uani 1 1 d . . . C18 C -0.6191(4) 0.92344(17) -0.4011(6) 0.0272(14) Uani 1 1 d . . . N1 N -0.4865(5) 0.73675(15) -0.3242(7) 0.0390(12) Uani 1 1 d . . . C9 C -0.3366(4) 0.86545(19) -0.3622(5) 0.0282(12) Uani 1 1 d . . . C19 C -0.6502(4) 0.88236(18) -0.3802(5) 0.0265(12) Uani 1 1 d . . . C4 C -0.2088(6) 0.8173(2) -0.3288(7) 0.0400(17) Uani 1 1 d . . . H4A H -0.1577 0.8144 -0.3309 0.048 Uiso 1 1 calc R . . C10 C -0.2570(5) 0.8606(2) -0.3609(6) 0.0341(14) Uani 1 1 d . . . C15 C -0.7768(5) 0.9299(2) -0.4090(6) 0.0375(16) Uani 1 1 d . . . H15A H -0.8302 0.9319 -0.4114 0.045 Uiso 1 1 calc R . . N3 N -0.3607(4) 0.81621(16) -0.0741(5) 0.0366(12) Uani 1 1 d . . . C20 C -0.7313(4) 0.8864(2) -0.3862(6) 0.0326(13) Uani 1 1 d . . . N5 N -0.3822(4) 0.93089(15) -0.1786(5) 0.0320(11) Uani 1 1 d . . . C37 C -0.4309(5) 0.7079(2) -0.2294(6) 0.0384(17) Uani 1 1 d . . . H37A H -0.3932 0.7203 -0.1435 0.046 Uiso 1 1 calc R . . C14 C -0.7662(5) 0.8466(2) -0.3673(6) 0.0373(15) Uani 1 1 d . . . H14A H -0.8197 0.8491 -0.3703 0.045 Uiso 1 1 calc R . . C8 C -0.3828(4) 0.9101(2) -0.3962(5) 0.0321(13) Uani 1 1 d . . . C12 C -0.6440(5) 0.8007(2) -0.3385(7) 0.0379(16) Uani 1 1 d . . . H12A H -0.6152 0.7709 -0.3220 0.045 Uiso 1 1 calc R . . C17 C -0.6652(4) 0.9651(2) -0.4239(6) 0.0368(14) Uani 1 1 d . . . H17A H -0.6429 0.9923 -0.4377 0.044 Uiso 1 1 calc R . . C26 C -0.4490(5) 1.0285(2) -0.3219(7) 0.0377(15) Uani 1 1 d . . . H26A H -0.4021 1.0135 -0.2403 0.045 Uiso 1 1 calc R . . C13 C -0.7235(6) 0.8046(2) -0.3450(7) 0.0447(19) Uani 1 1 d . . . H13A H -0.7480 0.7778 -0.3337 0.054 Uiso 1 1 calc R . . C2 C -0.3108(5) 0.7852(2) -0.2952(6) 0.0372(16) Uani 1 1 d . . . H2A H -0.3278 0.7589 -0.2711 0.045 Uiso 1 1 calc R . . C21 C -0.5104(5) 1.00168(19) -0.4330(6) 0.0331(13) Uani 1 1 d . . . C47 C -0.4054(4) 0.92955(18) -0.1046(5) 0.0308(13) Uani 1 1 d . . . H47A H -0.4714 0.9261 -0.1445 0.037 Uiso 1 1 calc R . . C33 C -0.5428(5) 0.7170(3) -0.4487(7) 0.0427(19) Uani 1 1 d . . . H33A H -0.5868 0.7362 -0.5228 0.051 Uiso 1 1 calc R . . C3 C -0.2339(5) 0.7809(2) -0.2959(7) 0.0407(16) Uani 1 1 d . . . H3A H -0.2003 0.7523 -0.2731 0.049 Uiso 1 1 calc R . . C49 C -0.2352(5) 0.9386(2) 0.0986(6) 0.0383(14) Uani 1 1 d . . . C43 C -0.1930(5) 0.82133(18) 0.1337(6) 0.0389(15) Uani 1 1 d . . . H43A H -0.1265 0.8250 0.1765 0.047 Uiso 1 1 calc R . . C7 C -0.3537(5) 0.9459(2) -0.4277(6) 0.0379(14) Uani 1 1 d . . . H7A H -0.3852 0.9751 -0.4495 0.045 Uiso 1 1 calc R . . C22 C -0.5813(5) 1.0239(2) -0.5554(6) 0.0433(16) Uani 1 1 d . . . H22A H -0.6251 1.0065 -0.6335 0.052 Uiso 1 1 calc R . . C35 C -0.4753(5) 0.6408(2) -0.3629(6) 0.0366(14) Uani 1 1 d . . . C34 C -0.5366(5) 0.6712(2) -0.4670(7) 0.0448(17) Uani 1 1 d . . . H34A H -0.5754 0.6596 -0.5538 0.054 Uiso 1 1 calc R . . C5 C -0.2298(5) 0.8990(2) -0.3943(6) 0.0415(15) Uani 1 1 d . . . H5A H -0.1772 0.8962 -0.3932 0.050 Uiso 1 1 calc R . . C44 C -0.2619(4) 0.82040(19) 0.0008(6) 0.0377(14) Uani 1 1 d . . . H44A H -0.2393 0.8229 -0.0461 0.045 Uiso 1 1 calc R . . C40 C -0.3908(5) 0.8126(2) -0.0100(7) 0.0439(16) Uani 1 1 d . . . H40A H -0.4580 0.8095 -0.0561 0.053 Uiso 1 1 calc R . . C36 C -0.4202(5) 0.6610(2) -0.2384(7) 0.0401(16) Uani 1 1 d . . . H36A H -0.3762 0.6428 -0.1620 0.048 Uiso 1 1 calc R . . C6 C -0.2775(5) 0.9406(2) -0.4286(7) 0.0447(17) Uani 1 1 d . . . H6A H -0.2588 0.9660 -0.4533 0.054 Uiso 1 1 calc R . . C48 C -0.3377(4) 0.93298(19) 0.0281(6) 0.0350(14) Uani 1 1 d . . . H48A H -0.3586 0.9316 0.0771 0.042 Uiso 1 1 calc R . . C16 C -0.7440(5) 0.9689(2) -0.4275(7) 0.0438(16) Uani 1 1 d . . . H16A H -0.7740 0.9981 -0.4427 0.053 Uiso 1 1 calc R . . C25 C -0.4536(5) 1.0764(2) -0.3258(7) 0.0517(18) Uani 1 1 d . . . H25A H -0.4105 1.0941 -0.2482 0.062 Uiso 1 1 calc R . . C50 C -0.2101(4) 0.94010(19) 0.0237(6) 0.0367(13) Uani 1 1 d . . . H50A H -0.1447 0.9436 0.0611 0.044 Uiso 1 1 calc R . . C41 C -0.3272(5) 0.8133(2) 0.1233(6) 0.0429(15) Uani 1 1 d . . . H41A H -0.3524 0.8114 0.1669 0.052 Uiso 1 1 calc R . . C51 C -0.2836(4) 0.93624(19) -0.1098(5) 0.0343(13) Uani 1 1 d . . . H51A H -0.2646 0.9374 -0.1611 0.041 Uiso 1 1 calc R . . C23 C -0.5836(6) 1.0724(2) -0.5554(8) 0.062(2) Uani 1 1 d . . . H23A H -0.6299 1.0881 -0.6360 0.074 Uiso 1 1 calc R . . C42 C -0.2240(5) 0.81673(19) 0.2020(6) 0.0408(15) Uani 1 1 d . . . C27 C -0.6152(4) 0.9054(2) -0.6274(5) 0.0306(12) Uani 1 1 d . . . N4 N -0.1572(5) 0.8160(2) 0.3351(5) 0.0593(16) Uani 1 1 d . . . N6 N -0.1657(4) 0.94254(19) 0.2304(4) 0.0425(12) Uani 1 1 d . . . C32 C -0.6057(5) 0.9206(2) -0.7124(6) 0.0455(17) Uani 1 1 d . . . H32A H -0.5560 0.9420 -0.6857 0.055 Uiso 1 1 calc R . . C30 C -0.7436(6) 0.8721(3) -0.8844(7) 0.0512(16) Uani 1 1 d . . . H30A H -0.7863 0.8622 -0.9730 0.061 Uiso 1 1 calc R . . C31 C -0.6694(5) 0.9049(2) -0.8395(6) 0.0516(17) Uani 1 1 d . . . H31A H -0.6634 0.9166 -0.9002 0.062 Uiso 1 1 calc R . . F4 F -0.4241(7) 0.4488(3) -0.3515(10) 0.170(4) Uani 1 1 d . . . N2 N -0.4672(4) 0.59509(18) -0.3797(6) 0.0519(14) Uani 1 1 d . . . F6 F -0.5304(4) 0.45543(17) -0.3372(6) 0.1060(19) Uani 1 1 d . . . C29 C -0.7520(5) 0.8557(2) -0.7996(7) 0.0502(16) Uani 1 1 d . . . H29A H -0.8000 0.8334 -0.8254 0.060 Uiso 1 1 calc R . . C24 C -0.5223(5) 1.0981(2) -0.4449(7) 0.0501(17) Uani 1 1 d . . . H24A H -0.5266 1.1311 -0.4493 0.060 Uiso 1 1 calc R . . C28 C -0.6879(4) 0.8724(2) -0.6711(5) 0.0400(14) Uani 1 1 d . . . H28A H -0.6937 0.8609 -0.6102 0.048 Uiso 1 1 calc R . . C46 C -0.0513(5) 0.8151(3) 0.4117(6) 0.063(2) Uani 1 1 d . . . H46A H -0.0376 0.8183 0.3524 0.094 Uiso 1 1 calc R . . H46B H -0.0251 0.7855 0.4588 0.094 Uiso 1 1 calc R . . H46C H -0.0211 0.8408 0.4745 0.094 Uiso 1 1 calc R . . C52 C -0.1945(5) 0.9430(3) 0.3058(6) 0.0585(19) Uani 1 1 d . . . H52A H -0.2645 0.9383 0.2486 0.088 Uiso 1 1 calc R . . H52B H -0.1777 0.9730 0.3504 0.088 Uiso 1 1 calc R . . H52C H -0.1613 0.9180 0.3709 0.088 Uiso 1 1 calc R . . F5 F -0.3585(5) 0.3849(2) -0.2182(7) 0.132(2) Uani 1 1 d . . . C53 C -0.0602(5) 0.9485(3) 0.2996(7) 0.069(2) Uani 1 1 d . . . H53A H -0.0507 0.9476 0.2356 0.103 Uiso 1 1 calc R . . H53B H -0.0232 0.9233 0.3632 0.103 Uiso 1 1 calc R . . H53C H -0.0378 0.9785 0.3453 0.103 Uiso 1 1 calc R . . F3 F -0.4712(5) 0.3920(3) -0.2124(8) 0.147(3) Uani 1 1 d . . . C39 C -0.3945(5) 0.5644(2) -0.2661(8) 0.0589(19) Uani 1 1 d . . . H39A H -0.3663 0.5808 -0.1843 0.088 Uiso 1 1 calc R . . H39B H -0.3434 0.5564 -0.2687 0.088 Uiso 1 1 calc R . . H39C H -0.4262 0.5359 -0.2708 0.088 Uiso 1 1 calc R . . C38 C -0.5164(7) 0.5766(2) -0.5099(9) 0.074(2) Uani 1 1 d . . . H38A H -0.5627 0.5997 -0.5754 0.112 Uiso 1 1 calc R . . H38B H -0.5509 0.5481 -0.5220 0.112 Uiso 1 1 calc R . . H38C H -0.4689 0.5697 -0.5202 0.112 Uiso 1 1 calc R . . C45 C -0.1901(7) 0.8106(4) 0.4046(8) 0.089(3) Uani 1 1 d . . . H45A H -0.2609 0.8118 0.3435 0.133 Uiso 1 1 calc R . . H45B H -0.1642 0.8357 0.4688 0.133 Uiso 1 1 calc R . . H45C H -0.1683 0.7806 0.4499 0.133 Uiso 1 1 calc R . . F2 F -0.5124(10) 0.3904(3) -0.3949(7) 0.273(8) Uani 1 1 d . . . F1 F -0.3738(6) 0.4509(2) -0.1600(7) 0.190(4) Uani 1 1 d . . . O1 O 0.0350(13) 0.7224(5) -0.2981(16) 0.237(8) Uani 1 1 d . . . C55 C 0.0117(11) 0.7205(6) -0.1642(13) 0.152(5) Uani 1 1 d . . . H55A H 0.0523 0.6984 -0.0905 0.182 Uiso 1 1 calc R . . H55B H -0.0454 0.7284 -0.1733 0.182 Uiso 1 1 calc R . . C57 C 0.0761(13) 0.7648(6) -0.2284(19) 0.165(6) Uani 1 1 d . . . H57A H 0.1448 0.7671 -0.1882 0.198 Uiso 1 1 calc R . . H57B H 0.0406 0.7918 -0.2872 0.198 Uiso 1 1 calc R . . C56 C 0.0680(14) 0.7635(6) -0.1370(14) 0.174(7) Uani 1 1 d . . . H56A H 0.0335 0.7914 -0.1424 0.209 Uiso 1 1 calc R . . H56B H 0.1325 0.7621 -0.0487 0.209 Uiso 1 1 calc R . . C54 C -0.016(2) 0.7014(6) -0.271(3) 0.40(2) Uani 1 1 d . . . H54B H -0.0860 0.7062 -0.3432 0.475 Uiso 1 1 calc R . . H54C H -0.0025 0.6676 -0.2587 0.475 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03243(12) 0.03079(11) 0.03510(12) 0.00358(12) 0.02468(10) 0.00236(11) Sb1 0.0326(2) 0.0300(2) 0.0320(2) 0.00004(16) 0.0247(2) -0.00070(18) P1 0.0623(13) 0.0536(11) 0.0431(10) -0.0068(8) 0.0396(10) -0.0036(9) C1 0.032(4) 0.031(4) 0.026(4) -0.004(2) 0.019(3) -0.002(2) C11 0.027(4) 0.036(3) 0.027(3) 0.001(3) 0.019(3) 0.000(3) C18 0.023(3) 0.035(3) 0.023(3) 0.000(2) 0.015(3) 0.002(2) N1 0.045(3) 0.044(3) 0.040(3) 0.006(3) 0.032(2) 0.004(3) C9 0.028(3) 0.035(3) 0.025(3) -0.004(2) 0.019(3) -0.002(2) C19 0.023(3) 0.035(3) 0.021(3) -0.006(2) 0.014(2) -0.006(2) C4 0.039(4) 0.050(4) 0.033(4) 0.003(3) 0.024(3) 0.006(3) C10 0.034(4) 0.045(4) 0.029(3) -0.007(3) 0.022(3) -0.004(3) C15 0.033(4) 0.048(4) 0.043(4) 0.000(3) 0.029(3) 0.000(3) N3 0.045(3) 0.037(3) 0.032(3) 0.002(2) 0.026(3) 0.005(2) C20 0.028(3) 0.040(3) 0.027(3) -0.004(3) 0.016(3) -0.001(3) N5 0.043(3) 0.033(3) 0.038(3) 0.001(2) 0.034(3) 0.000(2) C37 0.036(4) 0.058(5) 0.020(3) -0.014(3) 0.017(3) -0.015(3) C14 0.033(4) 0.050(4) 0.042(4) -0.004(3) 0.030(3) -0.008(3) C8 0.034(3) 0.043(3) 0.030(3) -0.007(3) 0.026(3) -0.006(3) C12 0.046(4) 0.026(3) 0.052(4) -0.001(3) 0.036(4) -0.001(3) C17 0.045(4) 0.036(3) 0.036(3) 0.001(3) 0.029(3) 0.002(3) C26 0.044(4) 0.036(3) 0.040(4) 0.007(3) 0.031(4) 0.006(3) C13 0.060(5) 0.031(4) 0.058(5) -0.008(3) 0.045(4) -0.013(3) C2 0.042(4) 0.036(4) 0.046(4) 0.005(3) 0.034(3) 0.003(3) C21 0.036(3) 0.035(3) 0.036(3) 0.010(3) 0.027(3) 0.003(3) C47 0.040(3) 0.034(3) 0.022(3) -0.002(2) 0.021(3) -0.004(3) C33 0.043(4) 0.048(4) 0.025(4) 0.013(3) 0.017(4) 0.015(3) C3 0.041(4) 0.042(4) 0.042(4) 0.004(3) 0.028(3) 0.013(3) C49 0.046(4) 0.034(3) 0.035(3) 0.001(3) 0.026(3) 0.006(3) C43 0.046(4) 0.033(3) 0.042(4) 0.002(3) 0.030(3) 0.007(3) C7 0.054(4) 0.032(3) 0.047(4) -0.001(3) 0.041(3) -0.001(3) C22 0.058(4) 0.039(4) 0.038(4) 0.001(3) 0.033(4) 0.005(3) C35 0.044(4) 0.036(3) 0.040(4) 0.002(3) 0.032(3) -0.003(3) C34 0.043(4) 0.045(4) 0.044(4) -0.006(3) 0.027(4) -0.003(3) C5 0.042(4) 0.051(4) 0.047(4) -0.006(3) 0.036(3) -0.004(3) C44 0.043(4) 0.038(3) 0.039(4) 0.003(3) 0.029(3) 0.007(3) C40 0.044(4) 0.041(3) 0.057(4) 0.005(3) 0.037(4) 0.006(3) C36 0.037(4) 0.042(4) 0.040(4) 0.013(3) 0.025(3) 0.010(3) C6 0.053(4) 0.043(4) 0.063(4) -0.007(3) 0.048(4) -0.009(3) C48 0.041(4) 0.033(3) 0.039(4) 0.003(3) 0.030(3) 0.005(3) C16 0.051(4) 0.039(4) 0.056(4) 0.006(3) 0.041(4) 0.009(3) C25 0.062(5) 0.044(4) 0.060(4) -0.014(4) 0.044(4) -0.011(3) C50 0.032(3) 0.041(3) 0.038(3) 0.004(3) 0.023(3) 0.004(3) C41 0.056(4) 0.045(3) 0.040(4) 0.004(3) 0.036(4) 0.007(3) C51 0.037(3) 0.041(3) 0.035(3) 0.005(3) 0.028(3) 0.006(3) C23 0.094(6) 0.051(5) 0.067(5) 0.028(4) 0.064(5) 0.024(4) C42 0.059(4) 0.031(3) 0.035(3) 0.001(3) 0.032(3) 0.004(3) C27 0.030(3) 0.041(3) 0.023(3) -0.001(2) 0.018(3) -0.001(3) N4 0.076(5) 0.073(4) 0.037(3) -0.005(3) 0.040(4) 0.000(3) N6 0.036(3) 0.063(3) 0.024(3) -0.002(2) 0.017(2) 0.002(3) C32 0.052(4) 0.046(4) 0.040(4) -0.003(3) 0.030(4) -0.005(3) C30 0.055(4) 0.062(4) 0.030(3) -0.013(3) 0.025(3) -0.008(3) C31 0.073(5) 0.056(4) 0.041(4) -0.004(3) 0.044(4) -0.005(4) F4 0.248(9) 0.170(7) 0.259(10) 0.071(7) 0.239(9) 0.057(6) N2 0.067(4) 0.039(3) 0.057(4) -0.001(3) 0.043(3) 0.004(3) F6 0.119(5) 0.069(3) 0.143(5) 0.030(3) 0.091(4) 0.032(3) C29 0.040(4) 0.059(4) 0.050(4) -0.014(3) 0.029(4) -0.010(3) C24 0.079(5) 0.033(3) 0.047(4) 0.004(3) 0.044(4) 0.004(3) C28 0.040(4) 0.048(4) 0.030(3) -0.003(3) 0.021(3) -0.002(3) C46 0.053(5) 0.101(6) 0.026(3) -0.005(4) 0.023(4) -0.009(4) C52 0.059(5) 0.087(5) 0.032(4) 0.005(3) 0.031(4) 0.012(4) F5 0.153(6) 0.134(5) 0.181(6) 0.049(5) 0.141(6) 0.063(4) C53 0.042(4) 0.108(6) 0.040(4) -0.001(4) 0.019(4) 0.002(4) F3 0.154(6) 0.156(6) 0.212(8) 0.081(6) 0.156(6) 0.033(5) C39 0.060(5) 0.035(3) 0.077(5) 0.007(3) 0.042(4) 0.006(3) C38 0.110(7) 0.046(4) 0.085(6) -0.015(4) 0.071(6) 0.001(4) C45 0.098(7) 0.130(8) 0.049(5) 0.002(5) 0.052(5) -0.011(6) F2 0.400(15) 0.088(5) 0.083(5) -0.027(4) 0.044(7) 0.041(7) F1 0.173(7) 0.118(5) 0.083(5) -0.043(4) -0.006(4) -0.020(5) O1 0.363(18) 0.260(13) 0.296(17) -0.154(13) 0.306(17) -0.129(14) C55 0.185(14) 0.197(15) 0.128(11) 0.054(11) 0.126(12) 0.045(12) C57 0.184(16) 0.192(17) 0.160(15) 0.058(14) 0.131(14) 0.033(13) C56 0.234(19) 0.154(14) 0.099(10) 0.021(10) 0.091(12) -0.007(13) C54 0.88(7) 0.175(16) 0.70(5) -0.24(3) 0.77(6) -0.25(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C1 2.103(9) . ? Hg1 C11 2.123(7) . ? Hg1 N3 2.611(5) . ? Hg1 N1 2.614(4) . ? Hg1 Sb1 3.0394(9) . ? Sb1 C21 2.149(6) . ? Sb1 C18 2.158(6) . ? Sb1 C27 2.170(5) . ? Sb1 C8 2.184(6) . ? Sb1 N5 2.524(5) . ? P1 F3 1.497(5) . ? P1 F4 1.499(6) . ? P1 F1 1.501(6) . ? P1 F2 1.502(8) . ? P1 F5 1.576(6) . ? P1 F6 1.579(5) . ? C1 C2 1.383(8) . ? C1 C9 1.419(8) . ? C11 C12 1.362(9) . ? C11 C19 1.436(9) . ? C18 C17 1.378(8) . ? C18 C19 1.414(7) . ? N1 C37 1.289(9) . ? N1 C33 1.394(10) . ? C9 C8 1.437(8) . ? C9 C10 1.442(8) . ? C19 C20 1.429(8) . ? C4 C3 1.326(9) . ? C4 C10 1.419(9) . ? C4 H4A 0.9500 . ? C10 C5 1.397(8) . ? C15 C16 1.368(9) . ? C15 C20 1.417(8) . ? C15 H15A 0.9500 . ? N3 C40 1.289(8) . ? N3 C44 1.382(8) . ? C20 C14 1.408(8) . ? N5 C47 1.308(7) . ? N5 C51 1.394(7) . ? C37 C36 1.378(9) . ? C37 H37A 0.9500 . ? C14 C13 1.358(10) . ? C14 H14A 0.9500 . ? C8 C7 1.342(8) . ? C12 C13 1.395(10) . ? C12 H12A 0.9500 . ? C17 C16 1.405(9) . ? C17 H17A 0.9500 . ? C26 C25 1.378(8) . ? C26 C21 1.381(9) . ? C26 H26A 0.9500 . ? C13 H13A 0.9500 . ? C2 C3 1.409(9) . ? C2 H2A 0.9500 . ? C21 C22 1.422(9) . ? C47 C48 1.362(8) . ? C47 H47A 0.9500 . ? C33 C34 1.357(9) . ? C33 H33A 0.9500 . ? C3 H3A 0.9500 . ? C49 C50 1.347(8) . ? C49 N6 1.357(8) . ? C49 C48 1.451(8) . ? C43 C42 1.359(9) . ? C43 C44 1.362(9) . ? C43 H43A 0.9500 . ? C7 C6 1.402(9) . ? C7 H7A 0.9500 . ? C22 C23 1.396(9) . ? C22 H22A 0.9500 . ? C35 N2 1.358(8) . ? C35 C34 1.394(9) . ? C35 C36 1.401(9) . ? C34 H34A 0.9500 . ? C5 C6 1.370(10) . ? C5 H5A 0.9500 . ? C44 H44A 0.9500 . ? C40 C41 1.363(9) . ? C40 H40A 0.9500 . ? C36 H36A 0.9500 . ? C6 H6A 0.9500 . ? C48 H48A 0.9500 . ? C16 H16A 0.9500 . ? C25 C24 1.385(10) . ? C25 H25A 0.9500 . ? C50 C51 1.380(8) . ? C50 H50A 0.9500 . ? C41 C42 1.440(9) . ? C41 H41A 0.9500 . ? C51 H51A 0.9500 . ? C23 C24 1.359(10) . ? C23 H23A 0.9500 . ? C42 N4 1.361(8) . ? C27 C32 1.332(8) . ? C27 C28 1.410(8) . ? N4 C45 1.406(9) . ? N4 C46 1.482(9) . ? N6 C52 1.409(8) . ? N6 C53 1.504(8) . ? C32 C31 1.377(9) . ? C32 H32A 0.9500 . ? C30 C29 1.329(10) . ? C30 C31 1.420(10) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? N2 C38 1.453(10) . ? N2 C39 1.496(9) . ? C29 C28 1.398(8) . ? C29 H29A 0.9500 . ? C24 H24A 0.9500 . ? C28 H28A 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O1 C54 1.334(18) . ? O1 C57 1.419(18) . ? C55 C54 1.30(2) . ? C55 C56 1.490(19) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 C56 1.328(19) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C54 H54B 0.9900 . ? C54 H54C 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Hg1 C11 169.8(3) . . ? C1 Hg1 N3 91.5(2) . . ? C11 Hg1 N3 97.0(2) . . ? C1 Hg1 N1 92.74(18) . . ? C11 Hg1 N1 94.1(2) . . ? N3 Hg1 N1 82.07(18) . . ? C1 Hg1 Sb1 86.94(15) . . ? C11 Hg1 Sb1 84.17(19) . . ? N3 Hg1 Sb1 116.20(10) . . ? N1 Hg1 Sb1 161.73(15) . . ? C21 Sb1 C18 96.0(2) . . ? C21 Sb1 C27 104.4(2) . . ? C18 Sb1 C27 92.5(2) . . ? C21 Sb1 C8 100.3(2) . . ? C18 Sb1 C8 159.0(2) . . ? C27 Sb1 C8 96.2(2) . . ? C21 Sb1 N5 89.6(2) . . ? C18 Sb1 N5 88.95(19) . . ? C27 Sb1 N5 165.61(19) . . ? C8 Sb1 N5 78.01(18) . . ? C21 Sb1 Hg1 163.32(17) . . ? C18 Sb1 Hg1 81.13(14) . . ? C27 Sb1 Hg1 92.13(15) . . ? C8 Sb1 Hg1 79.47(16) . . ? N5 Sb1 Hg1 73.94(10) . . ? F3 P1 F4 175.5(5) . . ? F3 P1 F1 95.0(5) . . ? F4 P1 F1 88.7(6) . . ? F3 P1 F2 86.0(7) . . ? F4 P1 F2 90.3(7) . . ? F1 P1 F2 178.9(8) . . ? F3 P1 F5 86.7(4) . . ? F4 P1 F5 96.1(4) . . ? F1 P1 F5 87.9(4) . . ? F2 P1 F5 91.6(5) . . ? F3 P1 F6 92.7(4) . . ? F4 P1 F6 84.5(4) . . ? F1 P1 F6 93.0(4) . . ? F2 P1 F6 87.4(5) . . ? F5 P1 F6 178.9(4) . . ? C2 C1 C9 118.7(7) . . ? C2 C1 Hg1 119.5(5) . . ? C9 C1 Hg1 121.8(5) . . ? C12 C11 C19 118.2(6) . . ? C12 C11 Hg1 118.5(5) . . ? C19 C11 Hg1 123.1(5) . . ? C17 C18 C19 120.5(6) . . ? C17 C18 Sb1 113.5(4) . . ? C19 C18 Sb1 125.6(4) . . ? C37 N1 C33 114.7(5) . . ? C37 N1 Hg1 129.9(5) . . ? C33 N1 Hg1 113.0(4) . . ? C1 C9 C8 124.9(6) . . ? C1 C9 C10 117.5(6) . . ? C8 C9 C10 117.6(5) . . ? C18 C19 C20 116.8(5) . . ? C18 C19 C11 124.1(6) . . ? C20 C19 C11 119.1(5) . . ? C3 C4 C10 121.0(7) . . ? C3 C4 H4A 119.5 . . ? C10 C4 H4A 119.5 . . ? C5 C10 C4 120.9(6) . . ? C5 C10 C9 118.8(6) . . ? C4 C10 C9 120.4(6) . . ? C16 C15 C20 120.0(6) . . ? C16 C15 H15A 120.0 . . ? C20 C15 H15A 120.0 . . ? C40 N3 C44 115.8(5) . . ? C40 N3 Hg1 122.5(4) . . ? C44 N3 Hg1 121.1(4) . . ? C14 C20 C15 119.2(5) . . ? C14 C20 C19 119.4(5) . . ? C15 C20 C19 121.4(5) . . ? C47 N5 C51 114.1(5) . . ? C47 N5 Sb1 120.1(4) . . ? C51 N5 Sb1 125.7(3) . . ? N1 C37 C36 127.4(6) . . ? N1 C37 H37A 116.3 . . ? C36 C37 H37A 116.3 . . ? C13 C14 C20 120.3(6) . . ? C13 C14 H14A 119.9 . . ? C20 C14 H14A 119.9 . . ? C7 C8 C9 121.1(6) . . ? C7 C8 Sb1 112.0(5) . . ? C9 C8 Sb1 126.6(4) . . ? C11 C12 C13 122.7(6) . . ? C11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C18 C17 C16 122.2(6) . . ? C18 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C25 C26 C21 122.0(6) . . ? C25 C26 H26A 119.0 . . ? C21 C26 H26A 119.0 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C1 C2 C3 123.0(6) . . ? C1 C2 H2A 118.5 . . ? C3 C2 H2A 118.5 . . ? C26 C21 C22 119.3(5) . . ? C26 C21 Sb1 121.9(4) . . ? C22 C21 Sb1 118.4(5) . . ? N5 C47 C48 121.9(6) . . ? N5 C47 H47A 119.1 . . ? C48 C47 H47A 119.1 . . ? C34 C33 N1 122.0(6) . . ? C34 C33 H33A 119.0 . . ? N1 C33 H33A 119.0 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C50 C49 N6 119.5(6) . . ? C50 C49 C48 115.4(5) . . ? N6 C49 C48 125.1(6) . . ? C42 C43 C44 116.8(6) . . ? C42 C43 H43A 121.6 . . ? C44 C43 H43A 121.6 . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C23 C22 C21 117.0(6) . . ? C23 C22 H22A 121.5 . . ? C21 C22 H22A 121.5 . . ? N2 C35 C34 122.9(6) . . ? N2 C35 C36 121.9(6) . . ? C34 C35 C36 115.1(5) . . ? C33 C34 C35 122.2(7) . . ? C33 C34 H34A 118.9 . . ? C35 C34 H34A 118.9 . . ? C6 C5 C10 121.3(6) . . ? C6 C5 H5A 119.4 . . ? C10 C5 H5A 119.4 . . ? C43 C44 N3 127.8(6) . . ? C43 C44 H44A 116.1 . . ? N3 C44 H44A 116.1 . . ? N3 C40 C41 120.6(6) . . ? N3 C40 H40A 119.7 . . ? C41 C40 H40A 119.7 . . ? C37 C36 C35 118.6(6) . . ? C37 C36 H36A 120.7 . . ? C35 C36 H36A 120.7 . . ? C5 C6 C7 120.3(6) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C47 C48 C49 123.5(6) . . ? C47 C48 H48A 118.3 . . ? C49 C48 H48A 118.3 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C26 C25 C24 118.8(6) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C49 C50 C51 117.1(6) . . ? C49 C50 H50A 121.5 . . ? C51 C50 H50A 121.5 . . ? C40 C41 C42 123.9(6) . . ? C40 C41 H41A 118.1 . . ? C42 C41 H41A 118.1 . . ? C50 C51 N5 128.1(5) . . ? C50 C51 H51A 116.0 . . ? N5 C51 H51A 116.0 . . ? C24 C23 C22 122.7(7) . . ? C24 C23 H23A 118.6 . . ? C22 C23 H23A 118.6 . . ? C43 C42 N4 118.7(6) . . ? C43 C42 C41 115.1(6) . . ? N4 C42 C41 126.3(6) . . ? C32 C27 C28 118.1(5) . . ? C32 C27 Sb1 119.8(4) . . ? C28 C27 Sb1 121.9(4) . . ? C42 N4 C45 118.1(7) . . ? C42 N4 C46 124.3(6) . . ? C45 N4 C46 117.2(6) . . ? C49 N6 C52 118.2(6) . . ? C49 N6 C53 123.5(5) . . ? C52 N6 C53 118.2(5) . . ? C27 C32 C31 118.8(6) . . ? C27 C32 H32A 120.6 . . ? C31 C32 H32A 120.6 . . ? C29 C30 C31 118.5(6) . . ? C29 C30 H30A 120.8 . . ? C31 C30 H30A 120.8 . . ? C32 C31 C30 123.2(6) . . ? C32 C31 H31A 118.4 . . ? C30 C31 H31A 118.4 . . ? C35 N2 C38 120.3(6) . . ? C35 N2 C39 121.4(6) . . ? C38 N2 C39 117.3(6) . . ? C30 C29 C28 118.0(6) . . ? C30 C29 H29A 121.0 . . ? C28 C29 H29A 121.0 . . ? C23 C24 C25 120.1(6) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C29 C28 C27 123.4(6) . . ? C29 C28 H28A 118.3 . . ? C27 C28 H28A 118.3 . . ? N4 C46 H46A 109.5 . . ? N4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N6 C52 H52A 109.5 . . ? N6 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N6 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N6 C53 H53A 109.5 . . ? N6 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N6 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N2 C39 H39A 109.5 . . ? N2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C45 H45A 109.5 . . ? N4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C54 O1 C57 111.8(11) . . ? C54 C55 C56 109.5(13) . . ? C54 C55 H55A 109.8 . . ? C56 C55 H55A 109.8 . . ? C54 C55 H55B 109.8 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.2 . . ? C56 C57 O1 105.0(14) . . ? C56 C57 H57A 110.7 . . ? O1 C57 H57A 110.7 . . ? C56 C57 H57B 110.7 . . ? O1 C57 H57B 110.7 . . ? H57A C57 H57B 108.8 . . ? C57 C56 C55 105.4(15) . . ? C57 C56 H56A 110.7 . . ? C55 C56 H56A 110.7 . . ? C57 C56 H56B 110.7 . . ? C55 C56 H56B 110.7 . . ? H56A C56 H56B 108.8 . . ? C55 C54 O1 105.6(17) . . ? C55 C54 H54B 110.6 . . ? O1 C54 H54B 110.6 . . ? C55 C54 H54C 110.6 . . ? O1 C54 H54C 110.6 . . ? H54B C54 H54C 108.7 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Hg1 Sb1 C21 -94.3(6) . . . . ? C11 Hg1 Sb1 C21 90.8(6) . . . . ? N3 Hg1 Sb1 C21 -4.1(6) . . . . ? N1 Hg1 Sb1 C21 176.2(8) . . . . ? C1 Hg1 Sb1 C18 -175.4(3) . . . . ? C11 Hg1 Sb1 C18 9.7(2) . . . . ? N3 Hg1 Sb1 C18 -85.2(2) . . . . ? N1 Hg1 Sb1 C18 95.1(4) . . . . ? C1 Hg1 Sb1 C27 92.4(2) . . . . ? C11 Hg1 Sb1 C27 -82.5(2) . . . . ? N3 Hg1 Sb1 C27 -177.45(19) . . . . ? N1 Hg1 Sb1 C27 2.9(4) . . . . ? C1 Hg1 Sb1 C8 -3.5(2) . . . . ? C11 Hg1 Sb1 C8 -178.4(3) . . . . ? N3 Hg1 Sb1 C8 86.67(19) . . . . ? N1 Hg1 Sb1 C8 -93.0(4) . . . . ? C1 Hg1 Sb1 N5 -83.9(2) . . . . ? C11 Hg1 Sb1 N5 101.2(2) . . . . ? N3 Hg1 Sb1 N5 6.25(16) . . . . ? N1 Hg1 Sb1 N5 -173.4(4) . . . . ? C11 Hg1 C1 C2 -147.4(13) . . . . ? N3 Hg1 C1 C2 66.7(6) . . . . ? N1 Hg1 C1 C2 -15.4(6) . . . . ? Sb1 Hg1 C1 C2 -177.1(6) . . . . ? C11 Hg1 C1 C9 32(2) . . . . ? N3 Hg1 C1 C9 -114.0(5) . . . . ? N1 Hg1 C1 C9 163.8(5) . . . . ? Sb1 Hg1 C1 C9 2.1(5) . . . . ? C1 Hg1 C11 C12 144.0(14) . . . . ? N3 Hg1 C11 C12 -70.3(5) . . . . ? N1 Hg1 C11 C12 12.2(5) . . . . ? Sb1 Hg1 C11 C12 173.9(5) . . . . ? C1 Hg1 C11 C19 -40.9(19) . . . . ? N3 Hg1 C11 C19 104.8(5) . . . . ? N1 Hg1 C11 C19 -172.7(5) . . . . ? Sb1 Hg1 C11 C19 -11.0(5) . . . . ? C21 Sb1 C18 C17 11.8(5) . . . . ? C27 Sb1 C18 C17 -93.0(4) . . . . ? C8 Sb1 C18 C17 152.5(5) . . . . ? N5 Sb1 C18 C17 101.3(4) . . . . ? Hg1 Sb1 C18 C17 175.2(4) . . . . ? C21 Sb1 C18 C19 -175.6(5) . . . . ? C27 Sb1 C18 C19 79.6(5) . . . . ? C8 Sb1 C18 C19 -34.9(9) . . . . ? N5 Sb1 C18 C19 -86.1(5) . . . . ? Hg1 Sb1 C18 C19 -12.2(4) . . . . ? C1 Hg1 N1 C37 75.9(6) . . . . ? C11 Hg1 N1 C37 -111.7(6) . . . . ? N3 Hg1 N1 C37 -15.2(6) . . . . ? Sb1 Hg1 N1 C37 164.5(4) . . . . ? C1 Hg1 N1 C33 -85.5(5) . . . . ? C11 Hg1 N1 C33 86.9(5) . . . . ? N3 Hg1 N1 C33 -176.6(5) . . . . ? Sb1 Hg1 N1 C33 3.0(8) . . . . ? C2 C1 C9 C8 -178.9(6) . . . . ? Hg1 C1 C9 C8 1.8(9) . . . . ? C2 C1 C9 C10 0.0(9) . . . . ? Hg1 C1 C9 C10 -179.3(4) . . . . ? C17 C18 C19 C20 0.9(8) . . . . ? Sb1 C18 C19 C20 -171.2(4) . . . . ? C17 C18 C19 C11 -179.6(6) . . . . ? Sb1 C18 C19 C11 8.3(8) . . . . ? C12 C11 C19 C18 -179.0(6) . . . . ? Hg1 C11 C19 C18 5.8(8) . . . . ? C12 C11 C19 C20 0.5(8) . . . . ? Hg1 C11 C19 C20 -174.6(4) . . . . ? C3 C4 C10 C5 179.4(7) . . . . ? C3 C4 C10 C9 -1.9(10) . . . . ? C1 C9 C10 C5 180.0(6) . . . . ? C8 C9 C10 C5 -1.0(8) . . . . ? C1 C9 C10 C4 1.3(9) . . . . ? C8 C9 C10 C4 -179.7(6) . . . . ? C1 Hg1 N3 C40 -177.7(5) . . . . ? C11 Hg1 N3 C40 8.1(5) . . . . ? N1 Hg1 N3 C40 -85.1(5) . . . . ? Sb1 Hg1 N3 C40 95.0(4) . . . . ? C1 Hg1 N3 C44 11.7(4) . . . . ? C11 Hg1 N3 C44 -162.6(4) . . . . ? N1 Hg1 N3 C44 104.2(4) . . . . ? Sb1 Hg1 N3 C44 -75.7(4) . . . . ? C16 C15 C20 C14 -180.0(6) . . . . ? C16 C15 C20 C19 0.8(9) . . . . ? C18 C19 C20 C14 179.4(5) . . . . ? C11 C19 C20 C14 -0.1(8) . . . . ? C18 C19 C20 C15 -1.4(8) . . . . ? C11 C19 C20 C15 179.1(6) . . . . ? C21 Sb1 N5 C47 96.5(4) . . . . ? C18 Sb1 N5 C47 0.5(4) . . . . ? C27 Sb1 N5 C47 -95.5(8) . . . . ? C8 Sb1 N5 C47 -162.9(4) . . . . ? Hg1 Sb1 N5 C47 -80.5(4) . . . . ? C21 Sb1 N5 C51 -80.9(4) . . . . ? C18 Sb1 N5 C51 -176.8(4) . . . . ? C27 Sb1 N5 C51 87.1(8) . . . . ? C8 Sb1 N5 C51 19.8(4) . . . . ? Hg1 Sb1 N5 C51 102.1(4) . . . . ? C33 N1 C37 C36 1.7(11) . . . . ? Hg1 N1 C37 C36 -159.5(5) . . . . ? C15 C20 C14 C13 -179.8(7) . . . . ? C19 C20 C14 C13 -0.6(8) . . . . ? C1 C9 C8 C7 -180.0(6) . . . . ? C10 C9 C8 C7 1.1(8) . . . . ? C1 C9 C8 Sb1 -7.0(9) . . . . ? C10 C9 C8 Sb1 174.1(4) . . . . ? C21 Sb1 C8 C7 -17.3(5) . . . . ? C18 Sb1 C8 C7 -157.4(5) . . . . ? C27 Sb1 C8 C7 88.7(4) . . . . ? N5 Sb1 C8 C7 -104.7(4) . . . . ? Hg1 Sb1 C8 C7 179.7(4) . . . . ? C21 Sb1 C8 C9 169.2(5) . . . . ? C18 Sb1 C8 C9 29.1(9) . . . . ? C27 Sb1 C8 C9 -84.8(5) . . . . ? N5 Sb1 C8 C9 81.8(5) . . . . ? Hg1 Sb1 C8 C9 6.2(4) . . . . ? C19 C11 C12 C13 -0.2(10) . . . . ? Hg1 C11 C12 C13 175.2(5) . . . . ? C19 C18 C17 C16 0.0(9) . . . . ? Sb1 C18 C17 C16 173.1(5) . . . . ? C20 C14 C13 C12 0.9(10) . . . . ? C11 C12 C13 C14 -0.5(11) . . . . ? C9 C1 C2 C3 -0.8(10) . . . . ? Hg1 C1 C2 C3 178.5(5) . . . . ? C25 C26 C21 C22 -0.5(10) . . . . ? C25 C26 C21 Sb1 -174.0(5) . . . . ? C18 Sb1 C21 C26 89.3(5) . . . . ? C27 Sb1 C21 C26 -176.5(5) . . . . ? C8 Sb1 C21 C26 -77.4(5) . . . . ? N5 Sb1 C21 C26 0.4(5) . . . . ? Hg1 Sb1 C21 C26 10.4(10) . . . . ? C18 Sb1 C21 C22 -84.3(5) . . . . ? C27 Sb1 C21 C22 9.9(5) . . . . ? C8 Sb1 C21 C22 109.1(5) . . . . ? N5 Sb1 C21 C22 -173.2(5) . . . . ? Hg1 Sb1 C21 C22 -163.2(4) . . . . ? C51 N5 C47 C48 -0.2(7) . . . . ? Sb1 N5 C47 C48 -177.9(4) . . . . ? C37 N1 C33 C34 -1.9(11) . . . . ? Hg1 N1 C33 C34 162.6(6) . . . . ? C10 C4 C3 C2 1.1(11) . . . . ? C1 C2 C3 C4 0.2(11) . . . . ? C9 C8 C7 C6 0.2(9) . . . . ? Sb1 C8 C7 C6 -173.7(5) . . . . ? C26 C21 C22 C23 0.7(9) . . . . ? Sb1 C21 C22 C23 174.4(5) . . . . ? N1 C33 C34 C35 1.4(11) . . . . ? N2 C35 C34 C33 -179.0(7) . . . . ? C36 C35 C34 C33 -0.6(10) . . . . ? C4 C10 C5 C6 178.3(7) . . . . ? C9 C10 C5 C6 -0.4(9) . . . . ? C42 C43 C44 N3 1.4(9) . . . . ? C40 N3 C44 C43 -0.2(9) . . . . ? Hg1 N3 C44 C43 171.1(5) . . . . ? C44 N3 C40 C41 0.3(8) . . . . ? Hg1 N3 C40 C41 -170.8(4) . . . . ? N1 C37 C36 C35 -0.9(10) . . . . ? N2 C35 C36 C37 178.7(6) . . . . ? C34 C35 C36 C37 0.3(9) . . . . ? C10 C5 C6 C7 1.7(10) . . . . ? C8 C7 C6 C5 -1.6(10) . . . . ? N5 C47 C48 C49 0.4(9) . . . . ? C50 C49 C48 C47 -0.4(8) . . . . ? N6 C49 C48 C47 179.5(6) . . . . ? C20 C15 C16 C17 0.2(10) . . . . ? C18 C17 C16 C15 -0.6(9) . . . . ? C21 C26 C25 C24 0.2(9) . . . . ? N6 C49 C50 C51 -179.6(5) . . . . ? C48 C49 C50 C51 0.2(8) . . . . ? N3 C40 C41 C42 -1.7(10) . . . . ? C49 C50 C51 N5 -0.1(9) . . . . ? C47 N5 C51 C50 0.1(8) . . . . ? Sb1 N5 C51 C50 177.6(4) . . . . ? C21 C22 C23 C24 -0.6(11) . . . . ? C44 C43 C42 N4 178.0(5) . . . . ? C44 C43 C42 C41 -2.4(8) . . . . ? C40 C41 C42 C43 2.7(9) . . . . ? C40 C41 C42 N4 -177.7(6) . . . . ? C21 Sb1 C27 C32 52.3(5) . . . . ? C18 Sb1 C27 C32 149.1(5) . . . . ? C8 Sb1 C27 C32 -50.0(5) . . . . ? N5 Sb1 C27 C32 -115.2(8) . . . . ? Hg1 Sb1 C27 C32 -129.6(5) . . . . ? C21 Sb1 C27 C28 -133.0(5) . . . . ? C18 Sb1 C27 C28 -36.2(5) . . . . ? C8 Sb1 C27 C28 124.6(5) . . . . ? N5 Sb1 C27 C28 59.4(10) . . . . ? Hg1 Sb1 C27 C28 45.0(5) . . . . ? C43 C42 N4 C45 -179.2(7) . . . . ? C41 C42 N4 C45 1.3(10) . . . . ? C43 C42 N4 C46 -6.6(10) . . . . ? C41 C42 N4 C46 173.8(6) . . . . ? C50 C49 N6 C52 177.2(6) . . . . ? C48 C49 N6 C52 -2.6(9) . . . . ? C50 C49 N6 C53 0.0(10) . . . . ? C48 C49 N6 C53 -179.8(6) . . . . ? C28 C27 C32 C31 2.5(9) . . . . ? Sb1 C27 C32 C31 177.3(5) . . . . ? C27 C32 C31 C30 -1.7(11) . . . . ? C29 C30 C31 C32 -0.1(11) . . . . ? C34 C35 N2 C38 6.1(10) . . . . ? C36 C35 N2 C38 -172.3(6) . . . . ? C34 C35 N2 C39 174.6(6) . . . . ? C36 C35 N2 C39 -3.7(10) . . . . ? C31 C30 C29 C28 1.0(10) . . . . ? C22 C23 C24 C25 0.3(12) . . . . ? C26 C25 C24 C23 -0.1(11) . . . . ? C30 C29 C28 C27 -0.2(10) . . . . ? C32 C27 C28 C29 -1.6(9) . . . . ? Sb1 C27 C28 C29 -176.3(5) . . . . ? C54 O1 C57 C56 14(3) . . . . ? O1 C57 C56 C55 -5(2) . . . . ? C54 C55 C56 C57 -5(3) . . . . ? C56 C55 C54 O1 13(3) . . . . ? C57 O1 C54 C55 -17(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.093 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.079 # Attachment '- 2-F.cif' data_2-F _database_code_depnum_ccdc_archive 'CCDC 853648' #TrackingRef '- 2-F.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-F _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H52 F2 Hg2 O Sb2' _chemical_formula_weight 1567.78 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' Sb Sb -0.5866 1.5461 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.689(8) _cell_length_b 13.651(9) _cell_length_c 16.060(10) _cell_angle_alpha 97.184(7) _cell_angle_beta 95.058(7) _cell_angle_gamma 102.804(7) _cell_volume 2672(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4295 _exptl_absorpt_correction_T_max 0.5805 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23715 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8404 _reflns_number_gt 6849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8404 _refine_ls_number_parameters 676 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg2 Hg 0.56432(2) 0.93972(2) 0.256901(18) 0.02367(10) Uani 1 1 d . . . Hg1 Hg 0.32994(2) 0.80912(2) 0.389341(17) 0.02222(9) Uani 1 1 d . . . Sb2 Sb 0.75874(4) 1.11207(4) 0.34319(3) 0.02111(13) Uani 1 1 d . . . Sb1 Sb 0.23133(4) 0.73983(4) 0.20554(3) 0.02137(13) Uani 1 1 d . . . F1 F 0.3898(3) 0.7929(3) 0.1819(3) 0.0290(10) Uani 1 1 d . . . F2 F 0.6977(3) 1.1693(3) 0.4501(2) 0.0305(10) Uani 1 1 d . . . C11 C 0.3454(6) 0.9567(5) 0.3653(5) 0.0231(17) Uani 1 1 d . . . C1 C 0.3261(6) 0.6573(5) 0.3938(5) 0.0225(17) Uani 1 1 d . . . C19 C 0.2925(6) 0.9769(5) 0.2887(5) 0.0215(17) Uani 1 1 d . . . C20 C 0.2952(7) 1.0795(6) 0.2782(5) 0.0290(19) Uani 1 1 d . . . C18 C 0.2332(6) 0.9002(5) 0.2225(4) 0.0232(17) Uani 1 1 d . . . C33 C 0.6222(6) 0.8498(5) 0.3355(4) 0.0228(17) Uani 1 1 d . . . C40 C 0.7696(6) 0.9933(6) 0.4181(4) 0.0218(17) Uani 1 1 d . . . C52 C 0.5300(6) 1.2204(7) 0.1654(5) 0.034(2) Uani 1 1 d . . . C26 C 0.2460(7) 0.7154(6) 0.0158(5) 0.0293(19) Uani 1 1 d . . . H26A H 0.3213 0.7428 0.0336 0.035 Uiso 1 1 calc R . . C2 C 0.3506(6) 0.6272(6) 0.4715(5) 0.0260(18) Uani 1 1 d . . . H2A H 0.3528 0.6723 0.5221 0.031 Uiso 1 1 calc R . . C8 C 0.2925(6) 0.6107(5) 0.2366(5) 0.0224(17) Uani 1 1 d . . . C21 C 0.1741(6) 0.6989(5) 0.0751(4) 0.0231(17) Uani 1 1 d . . . C9 C 0.3188(6) 0.5894(5) 0.3191(5) 0.0221(17) Uani 1 1 d . . . C59 C 0.8110(6) 1.0402(6) 0.2304(5) 0.0246(17) Uani 1 1 d . . . C41 C 0.7124(6) 0.8905(6) 0.4004(5) 0.0269(18) Uani 1 1 d . . . C51 C 0.5703(6) 1.1495(6) 0.2109(5) 0.0257(18) Uani 1 1 d . . . C38 C 0.8787(6) 0.9603(6) 0.5376(5) 0.0280(18) Uani 1 1 d . . . H38A H 0.9339 0.9852 0.5842 0.034 Uiso 1 1 calc R . . C53 C 0.9035(6) 1.2292(6) 0.3783(5) 0.0286(18) Uani 1 1 d . . . C43 C 0.5252(6) 1.0443(6) 0.1834(5) 0.0285(19) Uani 1 1 d . . . C60 C 0.8001(6) 1.0774(6) 0.1538(5) 0.0304(19) Uani 1 1 d . . . H60A H 0.7658 1.1321 0.1500 0.037 Uiso 1 1 calc R . . C48 C 0.6364(7) 1.3604(6) 0.2651(5) 0.037(2) Uani 1 1 d . . . H48A H 0.6556 1.4310 0.2859 0.044 Uiso 1 1 calc R . . C31 C -0.0623(6) 0.5565(7) 0.2884(6) 0.041(2) Uani 1 1 d . . . H31A H -0.0926 0.4860 0.2871 0.049 Uiso 1 1 calc R . . C27 C 0.0804(6) 0.6910(6) 0.2583(4) 0.0238(17) Uani 1 1 d . . . C50 C 0.6526(6) 1.1912(6) 0.2799(4) 0.0232(17) Uani 1 1 d . . . C37 C 0.8283(6) 0.8602(6) 0.5212(5) 0.0298(19) Uani 1 1 d . . . H37A H 0.8494 0.8147 0.5560 0.036 Uiso 1 1 calc R . . C12 C 0.4035(6) 1.0367(6) 0.4230(5) 0.0277(18) Uani 1 1 d . . . H12A H 0.4367 1.0236 0.4745 0.033 Uiso 1 1 calc R . . C3 C 0.3719(6) 0.5329(6) 0.4761(5) 0.0262(18) Uani 1 1 d . . . H3A H 0.3886 0.5139 0.5297 0.031 Uiso 1 1 calc R . . C34 C 0.5749(6) 0.7472(6) 0.3260(5) 0.0270(18) Uani 1 1 d . . . H34A H 0.5163 0.7197 0.2824 0.032 Uiso 1 1 calc R . . C54 C 0.9791(6) 1.2458(6) 0.3198(5) 0.032(2) Uani 1 1 d . . . H54A H 0.9692 1.2012 0.2679 0.039 Uiso 1 1 calc R . . C35 C 0.6086(6) 0.6823(6) 0.3768(5) 0.034(2) Uani 1 1 d . . . H35A H 0.5731 0.6122 0.3677 0.040 Uiso 1 1 calc R . . C10 C 0.3436(6) 0.4934(6) 0.3250(5) 0.0278(18) Uani 1 1 d . . . C14 C 0.3634(7) 1.1580(6) 0.3400(5) 0.032(2) Uani 1 1 d . . . H14A H 0.3715 1.2268 0.3315 0.038 Uiso 1 1 calc R . . C25 C 0.2081(8) 0.6920(6) -0.0698(5) 0.039(2) Uani 1 1 d . . . H25A H 0.2571 0.7053 -0.1107 0.047 Uiso 1 1 calc R . . C28 C 0.0278(7) 0.7600(6) 0.2951(5) 0.033(2) Uani 1 1 d . . . H28A H 0.0596 0.8306 0.2994 0.040 Uiso 1 1 calc R . . C13 C 0.4157(6) 1.1378(6) 0.4088(5) 0.033(2) Uani 1 1 d . . . H13A H 0.4612 1.1915 0.4482 0.039 Uiso 1 1 calc R . . C61 C 0.8389(7) 1.0349(7) 0.0831(5) 0.041(2) Uani 1 1 d . . . H61A H 0.8341 1.0625 0.0318 0.049 Uiso 1 1 calc R . . C42 C 0.7452(6) 0.8229(6) 0.4533(5) 0.0261(18) Uani 1 1 d . . . C58 C 0.9197(7) 1.2955(6) 0.4543(5) 0.035(2) Uani 1 1 d . . . H58A H 0.8689 1.2859 0.4943 0.042 Uiso 1 1 calc R . . C39 C 0.8484(6) 1.0265(6) 0.4852(5) 0.0272(18) Uani 1 1 d . . . H39A H 0.8839 1.0966 0.4967 0.033 Uiso 1 1 calc R . . C36 C 0.6927(6) 0.7188(6) 0.4399(5) 0.0293(19) Uani 1 1 d . . . H36A H 0.7158 0.6743 0.4747 0.035 Uiso 1 1 calc R . . C4 C 0.3691(6) 0.4664(6) 0.4041(5) 0.0311(19) Uani 1 1 d . . . H4A H 0.3845 0.4020 0.4079 0.037 Uiso 1 1 calc R . . C47 C 0.5635(6) 1.3257(6) 0.1957(5) 0.033(2) Uani 1 1 d . . . H47A H 0.5345 1.3723 0.1668 0.039 Uiso 1 1 calc R . . C15 C 0.2341(8) 1.1020(7) 0.2096(5) 0.042(2) Uani 1 1 d . . . H15A H 0.2352 1.1707 0.2042 0.050 Uiso 1 1 calc R . . C44 C 0.4545(7) 1.0148(7) 0.1116(5) 0.038(2) Uani 1 1 d . . . H44A H 0.4265 0.9442 0.0933 0.045 Uiso 1 1 calc R . . C49 C 0.6849(6) 1.2940(6) 0.3076(5) 0.0307(19) Uani 1 1 d . . . H49A H 0.7390 1.3200 0.3546 0.037 Uiso 1 1 calc R . . C46 C 0.4566(7) 1.1837(7) 0.0910(5) 0.040(2) Uani 1 1 d . . . H46A H 0.4320 1.2306 0.0597 0.049 Uiso 1 1 calc R . . C17 C 0.1728(7) 0.9249(6) 0.1566(5) 0.035(2) Uani 1 1 d . . . H17A H 0.1303 0.8725 0.1146 0.042 Uiso 1 1 calc R . . C64 C 0.8598(6) 0.9600(6) 0.2345(5) 0.035(2) Uani 1 1 d . . . H64A H 0.8679 0.9340 0.2863 0.042 Uiso 1 1 calc R . . C22 C 0.0665(7) 0.6565(7) 0.0497(5) 0.044(2) Uani 1 1 d . . . H22A H 0.0174 0.6428 0.0904 0.053 Uiso 1 1 calc R . . C32 C 0.0353(6) 0.5885(6) 0.2571(5) 0.0307(19) Uani 1 1 d . . . H32A H 0.0721 0.5397 0.2343 0.037 Uiso 1 1 calc R . . C7 C 0.2930(6) 0.5432(6) 0.1665(5) 0.033(2) Uani 1 1 d . . . H7A H 0.2755 0.5598 0.1121 0.039 Uiso 1 1 calc R . . C5 C 0.3440(6) 0.4245(6) 0.2502(5) 0.034(2) Uani 1 1 d . . . H5A H 0.3619 0.3611 0.2546 0.040 Uiso 1 1 calc R . . C57 C 1.0106(7) 1.3753(6) 0.4705(6) 0.043(2) Uani 1 1 d . . . H57A H 1.0234 1.4192 0.5230 0.051 Uiso 1 1 calc R . . C16 C 0.1727(8) 1.0258(7) 0.1505(5) 0.045(2) Uani 1 1 d . . . H16A H 0.1297 1.0415 0.1048 0.054 Uiso 1 1 calc R . . C29 C -0.0688(7) 0.7289(7) 0.3256(6) 0.047(2) Uani 1 1 d . . . H29A H -0.1044 0.7779 0.3497 0.056 Uiso 1 1 calc R . . C24 C 0.1008(8) 0.6501(7) -0.0948(5) 0.046(2) Uani 1 1 d . . . H24A H 0.0755 0.6323 -0.1534 0.056 Uiso 1 1 calc R . . C30 C -0.1155(7) 0.6270(7) 0.3216(6) 0.042(2) Uani 1 1 d . . . H30A H -0.1839 0.6056 0.3416 0.051 Uiso 1 1 calc R . . C55 C 1.0671(6) 1.3266(6) 0.3380(6) 0.040(2) Uani 1 1 d . . . H55A H 1.1184 1.3375 0.2985 0.047 Uiso 1 1 calc R . . C45 C 0.4208(7) 1.0827(7) 0.0633(6) 0.048(3) Uani 1 1 d . . . H45A H 0.3736 1.0588 0.0121 0.057 Uiso 1 1 calc R . . C56 C 1.0829(8) 1.3923(7) 0.4121(7) 0.051(3) Uani 1 1 d . . . H56A H 1.1434 1.4493 0.4232 0.061 Uiso 1 1 calc R . . C6 C 0.3191(7) 0.4497(6) 0.1733(5) 0.039(2) Uani 1 1 d . . . H6A H 0.3192 0.4038 0.1237 0.047 Uiso 1 1 calc R . . C63 C 0.8969(8) 0.9172(8) 0.1635(6) 0.053(3) Uani 1 1 d . . . H63A H 0.9315 0.8626 0.1672 0.064 Uiso 1 1 calc R . . C62 C 0.8845(8) 0.9526(8) 0.0875(6) 0.053(3) Uani 1 1 d . . . H62A H 0.9072 0.9206 0.0385 0.064 Uiso 1 1 calc R . . C23 C 0.0287(8) 0.6332(7) -0.0369(6) 0.054(3) Uani 1 1 d . . . H23A H -0.0465 0.6058 -0.0552 0.064 Uiso 1 1 calc R . . C68 C 0.672(2) 1.6717(16) 0.0329(11) 0.205(7) Uani 1 1 d U . . H68A H 0.7024 1.7349 0.0103 0.246 Uiso 1 1 calc R . . H68B H 0.6182 1.6247 -0.0106 0.246 Uiso 1 1 calc R . . C65 C 0.673(3) 1.5423(13) 0.0909(17) 0.27(2) Uani 1 1 d . . . H65A H 0.6217 1.5010 0.0430 0.329 Uiso 1 1 calc R . . H65B H 0.7081 1.4975 0.1224 0.329 Uiso 1 1 calc R . . C66 C 0.626(2) 1.6005(18) 0.1408(14) 0.231(15) Uani 1 1 d . . . H66A H 0.6660 1.6171 0.1986 0.277 Uiso 1 1 calc R . . H66B H 0.5499 1.5657 0.1440 0.277 Uiso 1 1 calc R . . O1 O 0.7566(19) 1.6251(18) 0.0625(12) 0.270(8) Uani 1 1 d U . . C67 C 0.631(2) 1.6900(18) 0.1028(12) 0.218(8) Uani 1 1 d U . . H67A H 0.5579 1.7024 0.0913 0.261 Uiso 1 1 calc R . . H67B H 0.6785 1.7500 0.1398 0.261 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg2 0.02193(17) 0.02187(17) 0.02568(17) 0.00629(13) 0.00023(12) 0.00145(13) Hg1 0.02632(18) 0.01866(17) 0.02177(17) 0.00414(12) 0.00019(12) 0.00588(13) Sb2 0.0222(3) 0.0197(3) 0.0207(3) 0.0057(2) 0.0016(2) 0.0022(2) Sb1 0.0238(3) 0.0185(3) 0.0208(3) 0.0023(2) 0.0014(2) 0.0038(2) F1 0.025(2) 0.027(2) 0.035(3) 0.008(2) 0.0009(19) 0.0045(19) F2 0.043(3) 0.030(2) 0.021(2) 0.0046(19) 0.009(2) 0.013(2) C11 0.026(4) 0.022(4) 0.028(4) 0.007(3) 0.015(3) 0.012(3) C1 0.018(4) 0.021(4) 0.028(4) 0.011(3) 0.001(3) 0.000(3) C19 0.023(4) 0.017(4) 0.026(4) 0.006(3) 0.008(3) 0.006(3) C20 0.044(5) 0.019(4) 0.027(4) 0.005(4) 0.013(4) 0.010(4) C18 0.032(4) 0.018(4) 0.019(4) 0.003(3) 0.003(3) 0.005(3) C33 0.020(4) 0.023(4) 0.024(4) 0.004(3) 0.000(3) 0.001(3) C40 0.019(4) 0.026(4) 0.020(4) 0.004(3) 0.001(3) 0.005(3) C52 0.031(5) 0.041(5) 0.032(5) 0.011(4) 0.009(4) 0.004(4) C26 0.034(5) 0.023(4) 0.030(5) 0.000(4) 0.005(4) 0.009(4) C2 0.023(4) 0.025(4) 0.030(4) 0.008(4) 0.003(3) 0.005(3) C8 0.018(4) 0.016(4) 0.036(5) 0.011(3) 0.009(3) 0.006(3) C21 0.030(4) 0.023(4) 0.015(4) 0.003(3) -0.002(3) 0.006(3) C9 0.016(4) 0.016(4) 0.032(4) 0.005(3) 0.002(3) -0.002(3) C59 0.016(4) 0.027(4) 0.027(4) 0.007(4) 0.004(3) -0.004(3) C41 0.017(4) 0.029(5) 0.036(5) 0.003(4) 0.013(3) 0.006(3) C51 0.024(4) 0.028(5) 0.027(4) 0.010(4) 0.007(3) 0.006(4) C38 0.029(4) 0.034(5) 0.020(4) 0.004(4) -0.002(3) 0.008(4) C53 0.029(4) 0.023(4) 0.031(5) 0.001(4) -0.007(4) 0.007(4) C43 0.027(4) 0.031(5) 0.023(4) 0.011(4) -0.004(3) -0.002(4) C60 0.021(4) 0.038(5) 0.033(5) 0.011(4) -0.002(4) 0.007(4) C48 0.047(5) 0.022(5) 0.042(5) 0.009(4) 0.005(4) 0.010(4) C31 0.032(5) 0.036(5) 0.052(6) 0.006(4) 0.014(4) 0.002(4) C27 0.022(4) 0.027(4) 0.023(4) 0.003(3) 0.006(3) 0.005(3) C50 0.021(4) 0.032(5) 0.022(4) 0.012(3) 0.007(3) 0.010(3) C37 0.030(4) 0.042(5) 0.023(4) 0.011(4) 0.008(4) 0.014(4) C12 0.021(4) 0.025(4) 0.037(5) 0.003(4) -0.003(4) 0.008(3) C3 0.028(4) 0.022(4) 0.031(5) 0.017(4) 0.000(3) 0.005(3) C34 0.029(4) 0.020(4) 0.032(5) 0.007(4) 0.003(4) 0.004(4) C54 0.034(5) 0.028(5) 0.030(5) 0.005(4) -0.004(4) -0.001(4) C35 0.037(5) 0.013(4) 0.050(6) 0.004(4) 0.017(4) -0.001(4) C10 0.019(4) 0.022(4) 0.045(5) 0.015(4) 0.010(4) 0.002(3) C14 0.043(5) 0.022(4) 0.033(5) 0.008(4) 0.015(4) 0.008(4) C25 0.059(6) 0.033(5) 0.029(5) 0.007(4) 0.014(4) 0.015(5) C28 0.043(5) 0.027(5) 0.036(5) 0.009(4) 0.015(4) 0.014(4) C13 0.023(4) 0.029(5) 0.043(5) 0.003(4) 0.004(4) 0.004(4) C61 0.043(5) 0.066(6) 0.017(4) 0.007(4) 0.003(4) 0.017(5) C42 0.024(4) 0.037(5) 0.021(4) 0.006(4) 0.007(3) 0.013(4) C58 0.040(5) 0.035(5) 0.031(5) 0.010(4) -0.005(4) 0.011(4) C39 0.026(4) 0.025(4) 0.027(4) 0.005(4) -0.003(3) 0.000(3) C36 0.026(4) 0.026(5) 0.038(5) 0.012(4) 0.003(4) 0.009(4) C4 0.031(5) 0.021(4) 0.042(5) 0.012(4) -0.006(4) 0.007(4) C47 0.035(5) 0.034(5) 0.040(5) 0.018(4) 0.007(4) 0.021(4) C15 0.070(7) 0.031(5) 0.032(5) 0.023(4) 0.002(5) 0.017(5) C44 0.038(5) 0.040(5) 0.033(5) 0.015(4) -0.003(4) 0.003(4) C49 0.034(5) 0.028(5) 0.032(5) 0.007(4) 0.004(4) 0.010(4) C46 0.028(5) 0.050(6) 0.047(6) 0.030(5) 0.000(4) 0.006(4) C17 0.043(5) 0.033(5) 0.029(5) 0.007(4) -0.006(4) 0.013(4) C64 0.043(5) 0.046(5) 0.022(4) 0.009(4) 0.007(4) 0.021(4) C22 0.045(6) 0.046(6) 0.033(5) 0.004(4) 0.008(4) -0.006(5) C32 0.033(5) 0.029(5) 0.034(5) 0.011(4) 0.012(4) 0.008(4) C7 0.042(5) 0.031(5) 0.030(5) 0.005(4) 0.010(4) 0.014(4) C5 0.040(5) 0.017(4) 0.046(5) 0.000(4) 0.008(4) 0.014(4) C57 0.048(6) 0.021(5) 0.047(6) -0.002(4) -0.025(5) -0.001(4) C16 0.073(7) 0.041(6) 0.024(5) 0.008(4) -0.016(5) 0.025(5) C29 0.051(6) 0.050(6) 0.057(6) 0.025(5) 0.022(5) 0.033(5) C24 0.066(7) 0.037(5) 0.026(5) 0.002(4) -0.008(5) -0.001(5) C30 0.034(5) 0.051(6) 0.049(6) 0.022(5) 0.019(4) 0.013(5) C55 0.023(5) 0.035(5) 0.056(6) 0.011(5) 0.005(4) -0.005(4) C45 0.040(6) 0.054(6) 0.041(6) 0.019(5) -0.010(4) -0.008(5) C56 0.042(6) 0.032(5) 0.067(7) 0.022(5) -0.016(5) -0.011(4) C6 0.053(6) 0.034(5) 0.034(5) 0.003(4) 0.011(4) 0.019(4) C63 0.061(7) 0.065(7) 0.053(6) 0.025(5) 0.024(5) 0.043(6) C62 0.074(7) 0.067(7) 0.036(5) 0.020(5) 0.021(5) 0.040(6) C23 0.048(6) 0.058(7) 0.037(6) 0.007(5) -0.012(5) -0.018(5) C68 0.40(2) 0.238(15) 0.102(10) 0.120(10) 0.132(12) 0.251(14) C65 0.53(5) 0.062(12) 0.26(3) 0.059(15) 0.27(3) 0.02(2) C66 0.46(4) 0.20(2) 0.139(18) 0.079(17) 0.16(2) 0.22(3) O1 0.35(2) 0.335(18) 0.214(14) 0.113(14) 0.086(15) 0.202(16) C67 0.41(2) 0.249(15) 0.112(11) 0.095(11) 0.152(13) 0.239(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg2 C33 2.064(7) . ? Hg2 C43 2.076(8) . ? Hg2 F1 2.708(4) . ? Hg2 Sb2 3.0905(14) . ? Hg1 C11 2.069(7) . ? Hg1 C1 2.073(7) . ? Hg1 F2 2.622(4) 2_676 ? Hg1 Sb1 3.0495(18) . ? Sb2 F2 2.080(4) . ? Sb2 C53 2.130(8) . ? Sb2 C40 2.157(7) . ? Sb2 C50 2.167(7) . ? Sb2 C59 2.177(7) . ? Sb1 F1 2.066(4) . ? Sb1 C21 2.118(7) . ? Sb1 C18 2.166(7) . ? Sb1 C27 2.166(7) . ? Sb1 C8 2.172(7) . ? F2 Hg1 2.622(4) 2_676 ? C11 C12 1.366(10) . ? C11 C19 1.435(10) . ? C1 C2 1.391(10) . ? C1 C9 1.404(10) . ? C19 C18 1.423(10) . ? C19 C20 1.425(10) . ? C20 C15 1.396(11) . ? C20 C14 1.433(11) . ? C18 C17 1.372(11) . ? C33 C34 1.380(10) . ? C33 C41 1.439(10) . ? C40 C39 1.361(10) . ? C40 C41 1.410(10) . ? C52 C46 1.412(12) . ? C52 C47 1.415(11) . ? C52 C51 1.436(11) . ? C26 C21 1.380(10) . ? C26 C25 1.389(11) . ? C26 H26A 0.9500 . ? C2 C3 1.382(10) . ? C2 H2A 0.9500 . ? C8 C7 1.365(10) . ? C8 C9 1.419(10) . ? C21 C22 1.363(11) . ? C9 C10 1.427(10) . ? C59 C64 1.378(11) . ? C59 C60 1.395(10) . ? C41 C42 1.432(11) . ? C51 C50 1.421(10) . ? C51 C43 1.421(11) . ? C38 C37 1.356(11) . ? C38 C39 1.401(10) . ? C38 H38A 0.9500 . ? C53 C58 1.397(11) . ? C53 C54 1.403(11) . ? C43 C44 1.355(11) . ? C60 C61 1.390(11) . ? C60 H60A 0.9500 . ? C48 C47 1.346(11) . ? C48 C49 1.412(11) . ? C48 H48A 0.9500 . ? C31 C30 1.375(11) . ? C31 C32 1.380(10) . ? C31 H31A 0.9500 . ? C27 C28 1.375(10) . ? C27 C32 1.386(10) . ? C50 C49 1.375(10) . ? C37 C42 1.407(11) . ? C37 H37A 0.9500 . ? C12 C13 1.403(11) . ? C12 H12A 0.9500 . ? C3 C4 1.371(11) . ? C3 H3A 0.9500 . ? C34 C35 1.386(11) . ? C34 H34A 0.9500 . ? C54 C55 1.365(10) . ? C54 H54A 0.9500 . ? C35 C36 1.364(11) . ? C35 H35A 0.9500 . ? C10 C4 1.396(11) . ? C10 C5 1.431(11) . ? C14 C13 1.329(11) . ? C14 H14A 0.9500 . ? C25 C24 1.359(12) . ? C25 H25A 0.9500 . ? C28 C29 1.360(11) . ? C28 H28A 0.9500 . ? C13 H13A 0.9500 . ? C61 C62 1.379(12) . ? C61 H61A 0.9500 . ? C42 C36 1.409(11) . ? C58 C57 1.380(11) . ? C58 H58A 0.9500 . ? C39 H39A 0.9500 . ? C36 H36A 0.9500 . ? C4 H4A 0.9500 . ? C47 H47A 0.9500 . ? C15 C16 1.361(11) . ? C15 H15A 0.9500 . ? C44 C45 1.393(12) . ? C44 H44A 0.9500 . ? C49 H49A 0.9500 . ? C46 C45 1.355(12) . ? C46 H46A 0.9500 . ? C17 C16 1.393(11) . ? C17 H17A 0.9500 . ? C64 C63 1.384(11) . ? C64 H64A 0.9500 . ? C22 C23 1.404(12) . ? C22 H22A 0.9500 . ? C32 H32A 0.9500 . ? C7 C6 1.402(11) . ? C7 H7A 0.9500 . ? C5 C6 1.353(11) . ? C5 H5A 0.9500 . ? C57 C56 1.373(13) . ? C57 H57A 0.9500 . ? C16 H16A 0.9500 . ? C29 C30 1.377(12) . ? C29 H29A 0.9500 . ? C24 C23 1.365(12) . ? C24 H24A 0.9500 . ? C30 H30A 0.9500 . ? C55 C56 1.368(12) . ? C55 H55A 0.9500 . ? C45 H45A 0.9500 . ? C56 H56A 0.9500 . ? C6 H6A 0.9500 . ? C63 C62 1.377(12) . ? C63 H63A 0.9500 . ? C62 H62A 0.9500 . ? C23 H23A 0.9500 . ? C68 C67 1.297(19) . ? C68 O1 1.44(2) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C65 C66 1.33(2) . ? C65 O1 1.51(3) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.42(2) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C33 Hg2 C43 172.5(3) . . ? C33 Hg2 F1 95.2(2) . . ? C43 Hg2 F1 92.3(2) . . ? C33 Hg2 Sb2 86.1(2) . . ? C43 Hg2 Sb2 86.5(2) . . ? F1 Hg2 Sb2 178.15(9) . . ? C11 Hg1 C1 170.0(3) . . ? C11 Hg1 F2 100.8(2) . 2_676 ? C1 Hg1 F2 88.8(2) . 2_676 ? C11 Hg1 Sb1 87.3(2) . . ? C1 Hg1 Sb1 85.8(2) . . ? F2 Hg1 Sb1 148.76(10) 2_676 . ? F2 Sb2 C53 88.6(2) . . ? F2 Sb2 C40 81.2(2) . . ? C53 Sb2 C40 107.4(3) . . ? F2 Sb2 C50 82.8(2) . . ? C53 Sb2 C50 101.5(3) . . ? C40 Sb2 C50 146.4(3) . . ? F2 Sb2 C59 174.9(2) . . ? C53 Sb2 C59 96.4(3) . . ? C40 Sb2 C59 96.1(3) . . ? C50 Sb2 C59 97.3(3) . . ? F2 Sb2 Hg2 102.25(12) . . ? C53 Sb2 Hg2 168.5(2) . . ? C40 Sb2 Hg2 78.37(19) . . ? C50 Sb2 Hg2 76.3(2) . . ? C59 Sb2 Hg2 72.92(18) . . ? F1 Sb1 C21 92.5(2) . . ? F1 Sb1 C18 82.5(2) . . ? C21 Sb1 C18 100.6(3) . . ? F1 Sb1 C27 167.7(2) . . ? C21 Sb1 C27 99.7(3) . . ? C18 Sb1 C27 96.2(3) . . ? F1 Sb1 C8 82.8(2) . . ? C21 Sb1 C8 103.4(3) . . ? C18 Sb1 C8 152.4(3) . . ? C27 Sb1 C8 93.2(3) . . ? F1 Sb1 Hg1 83.12(12) . . ? C21 Sb1 Hg1 175.5(2) . . ? C18 Sb1 Hg1 77.64(19) . . ? C27 Sb1 Hg1 84.67(19) . . ? C8 Sb1 Hg1 77.5(2) . . ? Sb1 F1 Hg2 136.34(19) . . ? Sb2 F2 Hg1 155.3(2) . 2_676 ? C12 C11 C19 118.8(7) . . ? C12 C11 Hg1 120.6(6) . . ? C19 C11 Hg1 120.5(5) . . ? C2 C1 C9 119.6(7) . . ? C2 C1 Hg1 118.9(5) . . ? C9 C1 Hg1 120.5(5) . . ? C18 C19 C20 116.8(7) . . ? C18 C19 C11 124.1(6) . . ? C20 C19 C11 119.0(7) . . ? C15 C20 C19 120.8(7) . . ? C15 C20 C14 121.6(7) . . ? C19 C20 C14 117.6(7) . . ? C17 C18 C19 120.5(7) . . ? C17 C18 Sb1 111.8(5) . . ? C19 C18 Sb1 127.6(5) . . ? C34 C33 C41 117.9(7) . . ? C34 C33 Hg2 120.1(5) . . ? C41 C33 Hg2 122.0(5) . . ? C39 C40 C41 120.9(7) . . ? C39 C40 Sb2 111.5(5) . . ? C41 C40 Sb2 127.5(5) . . ? C46 C52 C47 120.9(8) . . ? C46 C52 C51 119.2(8) . . ? C47 C52 C51 119.9(7) . . ? C21 C26 C25 120.0(8) . . ? C21 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C3 C2 C1 121.0(7) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C7 C8 C9 121.4(7) . . ? C7 C8 Sb1 112.1(5) . . ? C9 C8 Sb1 126.1(5) . . ? C22 C21 C26 120.0(7) . . ? C22 C21 Sb1 120.1(6) . . ? C26 C21 Sb1 119.9(6) . . ? C1 C9 C8 124.7(7) . . ? C1 C9 C10 118.5(7) . . ? C8 C9 C10 116.7(7) . . ? C64 C59 C60 118.9(7) . . ? C64 C59 Sb2 120.3(6) . . ? C60 C59 Sb2 120.7(6) . . ? C40 C41 C42 116.9(7) . . ? C40 C41 C33 124.9(7) . . ? C42 C41 C33 118.1(7) . . ? C50 C51 C43 125.5(7) . . ? C50 C51 C52 116.7(7) . . ? C43 C51 C52 117.8(7) . . ? C37 C38 C39 119.2(7) . . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 120.4 . . ? C58 C53 C54 119.3(7) . . ? C58 C53 Sb2 121.5(6) . . ? C54 C53 Sb2 118.8(6) . . ? C44 C43 C51 119.2(7) . . ? C44 C43 Hg2 121.6(6) . . ? C51 C43 Hg2 119.1(5) . . ? C61 C60 C59 120.6(8) . . ? C61 C60 H60A 119.7 . . ? C59 C60 H60A 119.7 . . ? C47 C48 C49 121.5(8) . . ? C47 C48 H48A 119.3 . . ? C49 C48 H48A 119.3 . . ? C30 C31 C32 119.7(8) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C28 C27 C32 118.2(7) . . ? C28 C27 Sb1 121.4(6) . . ? C32 C27 Sb1 120.4(5) . . ? C49 C50 C51 122.0(7) . . ? C49 C50 Sb2 110.4(5) . . ? C51 C50 Sb2 127.0(6) . . ? C38 C37 C42 120.8(8) . . ? C38 C37 H37A 119.6 . . ? C42 C37 H37A 119.6 . . ? C11 C12 C13 122.1(7) . . ? C11 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? C4 C3 C2 120.7(7) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C33 C34 C35 123.4(7) . . ? C33 C34 H34A 118.3 . . ? C35 C34 H34A 118.3 . . ? C55 C54 C53 119.6(8) . . ? C55 C54 H54A 120.2 . . ? C53 C54 H54A 120.2 . . ? C36 C35 C34 120.1(7) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C4 C10 C9 120.1(7) . . ? C4 C10 C5 119.4(7) . . ? C9 C10 C5 120.5(7) . . ? C13 C14 C20 122.1(7) . . ? C13 C14 H14A 118.9 . . ? C20 C14 H14A 118.9 . . ? C24 C25 C26 119.7(8) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C29 C28 C27 121.2(8) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C14 C13 C12 119.7(8) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C62 C61 C60 119.8(8) . . ? C62 C61 H61A 120.1 . . ? C60 C61 H61A 120.1 . . ? C37 C42 C36 119.1(7) . . ? C37 C42 C41 120.3(7) . . ? C36 C42 C41 120.6(7) . . ? C57 C58 C53 119.0(8) . . ? C57 C58 H58A 120.5 . . ? C53 C58 H58A 120.5 . . ? C40 C39 C38 121.9(7) . . ? C40 C39 H39A 119.1 . . ? C38 C39 H39A 119.1 . . ? C35 C36 C42 119.8(8) . . ? C35 C36 H36A 120.1 . . ? C42 C36 H36A 120.1 . . ? C3 C4 C10 120.0(7) . . ? C3 C4 H4A 120.0 . . ? C10 C4 H4A 120.0 . . ? C48 C47 C52 120.4(8) . . ? C48 C47 H47A 119.8 . . ? C52 C47 H47A 119.8 . . ? C16 C15 C20 120.3(8) . . ? C16 C15 H15A 119.9 . . ? C20 C15 H15A 119.9 . . ? C43 C44 C45 123.5(8) . . ? C43 C44 H44A 118.3 . . ? C45 C44 H44A 118.3 . . ? C50 C49 C48 119.0(7) . . ? C50 C49 H49A 120.5 . . ? C48 C49 H49A 120.5 . . ? C45 C46 C52 121.2(8) . . ? C45 C46 H46A 119.4 . . ? C52 C46 H46A 119.4 . . ? C18 C17 C16 121.0(8) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C59 C64 C63 120.2(8) . . ? C59 C64 H64A 119.9 . . ? C63 C64 H64A 119.9 . . ? C21 C22 C23 119.6(8) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C31 C32 C27 120.9(8) . . ? C31 C32 H32A 119.6 . . ? C27 C32 H32A 119.6 . . ? C8 C7 C6 121.2(8) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C6 C5 C10 119.9(7) . . ? C6 C5 H5A 120.0 . . ? C10 C5 H5A 120.0 . . ? C56 C57 C58 121.2(8) . . ? C56 C57 H57A 119.4 . . ? C58 C57 H57A 119.4 . . ? C15 C16 C17 120.3(8) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C28 C29 C30 120.6(8) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C25 C24 C23 120.9(8) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C31 C30 C29 119.4(8) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C54 C55 C56 121.3(8) . . ? C54 C55 H55A 119.4 . . ? C56 C55 H55A 119.4 . . ? C46 C45 C44 118.7(8) . . ? C46 C45 H45A 120.7 . . ? C44 C45 H45A 120.7 . . ? C55 C56 C57 119.5(8) . . ? C55 C56 H56A 120.2 . . ? C57 C56 H56A 120.2 . . ? C5 C6 C7 120.3(8) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C62 C63 C64 121.0(9) . . ? C62 C63 H63A 119.5 . . ? C64 C63 H63A 119.5 . . ? C63 C62 C61 119.5(9) . . ? C63 C62 H62A 120.3 . . ? C61 C62 H62A 120.3 . . ? C24 C23 C22 119.6(9) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C67 C68 O1 100.0(17) . . ? C67 C68 H68A 111.8 . . ? O1 C68 H68A 111.8 . . ? C67 C68 H68B 111.8 . . ? O1 C68 H68B 111.8 . . ? H68A C68 H68B 109.5 . . ? C66 C65 O1 98.6(18) . . ? C66 C65 H65A 112.0 . . ? O1 C65 H65A 112.0 . . ? C66 C65 H65B 112.0 . . ? O1 C65 H65B 112.0 . . ? H65A C65 H65B 109.7 . . ? C65 C66 C67 105.1(17) . . ? C65 C66 H66A 110.7 . . ? C67 C66 H66A 110.7 . . ? C65 C66 H66B 110.7 . . ? C67 C66 H66B 110.7 . . ? H66A C66 H66B 108.8 . . ? C68 O1 C65 91(2) . . ? C68 C67 C66 104.5(17) . . ? C68 C67 H67A 110.9 . . ? C66 C67 H67A 110.9 . . ? C68 C67 H67B 110.9 . . ? C66 C67 H67B 110.9 . . ? H67A C67 H67B 108.9 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 Hg2 Sb2 F2 -85.1(2) . . . . ? C43 Hg2 Sb2 F2 96.1(2) . . . . ? F1 Hg2 Sb2 F2 49(3) . . . . ? C33 Hg2 Sb2 C53 114.8(10) . . . . ? C43 Hg2 Sb2 C53 -64.0(11) . . . . ? F1 Hg2 Sb2 C53 -112(3) . . . . ? C33 Hg2 Sb2 C40 -6.9(3) . . . . ? C43 Hg2 Sb2 C40 174.4(3) . . . . ? F1 Hg2 Sb2 C40 127(3) . . . . ? C33 Hg2 Sb2 C50 -164.5(3) . . . . ? C43 Hg2 Sb2 C50 16.7(3) . . . . ? F1 Hg2 Sb2 C50 -31(3) . . . . ? C33 Hg2 Sb2 C59 93.3(3) . . . . ? C43 Hg2 Sb2 C59 -85.5(3) . . . . ? F1 Hg2 Sb2 C59 -133(3) . . . . ? C11 Hg1 Sb1 F1 72.1(2) . . . . ? C1 Hg1 Sb1 F1 -100.6(2) . . . . ? F2 Hg1 Sb1 F1 178.7(2) 2_676 . . . ? C11 Hg1 Sb1 C21 55(3) . . . . ? C1 Hg1 Sb1 C21 -117(3) . . . . ? F2 Hg1 Sb1 C21 162(3) 2_676 . . . ? C11 Hg1 Sb1 C18 -11.7(3) . . . . ? C1 Hg1 Sb1 C18 175.6(3) . . . . ? F2 Hg1 Sb1 C18 94.9(3) 2_676 . . . ? C11 Hg1 Sb1 C27 -109.3(3) . . . . ? C1 Hg1 Sb1 C27 78.1(3) . . . . ? F2 Hg1 Sb1 C27 -2.7(3) 2_676 . . . ? C11 Hg1 Sb1 C8 156.2(3) . . . . ? C1 Hg1 Sb1 C8 -16.4(3) . . . . ? F2 Hg1 Sb1 C8 -97.2(3) 2_676 . . . ? C21 Sb1 F1 Hg2 148.6(3) . . . . ? C18 Sb1 F1 Hg2 48.2(3) . . . . ? C27 Sb1 F1 Hg2 -36.5(12) . . . . ? C8 Sb1 F1 Hg2 -108.3(3) . . . . ? Hg1 Sb1 F1 Hg2 -30.1(2) . . . . ? C33 Hg2 F1 Sb1 87.7(3) . . . . ? C43 Hg2 F1 Sb1 -93.4(3) . . . . ? Sb2 Hg2 F1 Sb1 -46(3) . . . . ? C53 Sb2 F2 Hg1 -84.6(5) . . . 2_676 ? C40 Sb2 F2 Hg1 23.3(5) . . . 2_676 ? C50 Sb2 F2 Hg1 173.6(5) . . . 2_676 ? C59 Sb2 F2 Hg1 82(3) . . . 2_676 ? Hg2 Sb2 F2 Hg1 99.3(5) . . . 2_676 ? C1 Hg1 C11 C12 -123.3(15) . . . . ? F2 Hg1 C11 C12 40.3(6) 2_676 . . . ? Sb1 Hg1 C11 C12 -170.1(6) . . . . ? C1 Hg1 C11 C19 58.6(18) . . . . ? F2 Hg1 C11 C19 -137.8(5) 2_676 . . . ? Sb1 Hg1 C11 C19 11.8(5) . . . . ? C11 Hg1 C1 C2 141.4(15) . . . . ? F2 Hg1 C1 C2 -22.5(6) 2_676 . . . ? Sb1 Hg1 C1 C2 -171.7(6) . . . . ? C11 Hg1 C1 C9 -27.0(19) . . . . ? F2 Hg1 C1 C9 169.1(6) 2_676 . . . ? Sb1 Hg1 C1 C9 19.9(5) . . . . ? C12 C11 C19 C18 177.6(7) . . . . ? Hg1 C11 C19 C18 -4.4(9) . . . . ? C12 C11 C19 C20 -4.7(10) . . . . ? Hg1 C11 C19 C20 173.4(5) . . . . ? C18 C19 C20 C15 5.7(11) . . . . ? C11 C19 C20 C15 -172.2(7) . . . . ? C18 C19 C20 C14 -173.8(7) . . . . ? C11 C19 C20 C14 8.3(10) . . . . ? C20 C19 C18 C17 -6.7(11) . . . . ? C11 C19 C18 C17 171.1(7) . . . . ? C20 C19 C18 Sb1 169.4(5) . . . . ? C11 C19 C18 Sb1 -12.8(10) . . . . ? F1 Sb1 C18 C17 107.6(6) . . . . ? C21 Sb1 C18 C17 16.4(6) . . . . ? C27 Sb1 C18 C17 -84.7(6) . . . . ? C8 Sb1 C18 C17 166.0(6) . . . . ? Hg1 Sb1 C18 C17 -167.9(6) . . . . ? F1 Sb1 C18 C19 -68.8(6) . . . . ? C21 Sb1 C18 C19 -160.0(6) . . . . ? C27 Sb1 C18 C19 98.9(7) . . . . ? C8 Sb1 C18 C19 -10.4(10) . . . . ? Hg1 Sb1 C18 C19 15.8(6) . . . . ? C43 Hg2 C33 C34 -164(2) . . . . ? F1 Hg2 C33 C34 7.6(6) . . . . ? Sb2 Hg2 C33 C34 -173.7(6) . . . . ? C43 Hg2 C33 C41 15(3) . . . . ? F1 Hg2 C33 C41 -173.2(5) . . . . ? Sb2 Hg2 C33 C41 5.5(5) . . . . ? F2 Sb2 C40 C39 -69.9(5) . . . . ? C53 Sb2 C40 C39 15.9(6) . . . . ? C50 Sb2 C40 C39 -132.5(6) . . . . ? C59 Sb2 C40 C39 114.5(5) . . . . ? Hg2 Sb2 C40 C39 -174.4(5) . . . . ? F2 Sb2 C40 C41 115.4(6) . . . . ? C53 Sb2 C40 C41 -158.9(6) . . . . ? C50 Sb2 C40 C41 52.7(9) . . . . ? C59 Sb2 C40 C41 -60.3(6) . . . . ? Hg2 Sb2 C40 C41 10.9(6) . . . . ? C9 C1 C2 C3 2.4(11) . . . . ? Hg1 C1 C2 C3 -166.1(5) . . . . ? F1 Sb1 C8 C7 -83.2(5) . . . . ? C21 Sb1 C8 C7 7.7(6) . . . . ? C18 Sb1 C8 C7 -141.5(6) . . . . ? C27 Sb1 C8 C7 108.5(6) . . . . ? Hg1 Sb1 C8 C7 -167.7(6) . . . . ? F1 Sb1 C8 C9 103.3(6) . . . . ? C21 Sb1 C8 C9 -165.8(6) . . . . ? C18 Sb1 C8 C9 45.0(9) . . . . ? C27 Sb1 C8 C9 -65.0(6) . . . . ? Hg1 Sb1 C8 C9 18.8(5) . . . . ? C25 C26 C21 C22 2.2(12) . . . . ? C25 C26 C21 Sb1 -177.7(6) . . . . ? F1 Sb1 C21 C22 -179.9(7) . . . . ? C18 Sb1 C21 C22 -97.1(7) . . . . ? C27 Sb1 C21 C22 1.2(7) . . . . ? C8 Sb1 C21 C22 96.9(7) . . . . ? Hg1 Sb1 C21 C22 -163(2) . . . . ? F1 Sb1 C21 C26 0.0(6) . . . . ? C18 Sb1 C21 C26 82.8(6) . . . . ? C27 Sb1 C21 C26 -178.9(6) . . . . ? C8 Sb1 C21 C26 -83.2(6) . . . . ? Hg1 Sb1 C21 C26 17(3) . . . . ? C2 C1 C9 C8 178.8(7) . . . . ? Hg1 C1 C9 C8 -12.9(10) . . . . ? C2 C1 C9 C10 -3.8(10) . . . . ? Hg1 C1 C9 C10 164.5(5) . . . . ? C7 C8 C9 C1 176.1(7) . . . . ? Sb1 C8 C9 C1 -10.9(10) . . . . ? C7 C8 C9 C10 -1.3(10) . . . . ? Sb1 C8 C9 C10 171.7(5) . . . . ? F2 Sb2 C59 C64 -73(3) . . . . ? C53 Sb2 C59 C64 93.7(6) . . . . ? C40 Sb2 C59 C64 -14.7(6) . . . . ? C50 Sb2 C59 C64 -163.7(6) . . . . ? Hg2 Sb2 C59 C64 -90.5(6) . . . . ? F2 Sb2 C59 C60 110(3) . . . . ? C53 Sb2 C59 C60 -83.4(6) . . . . ? C40 Sb2 C59 C60 168.2(6) . . . . ? C50 Sb2 C59 C60 19.1(6) . . . . ? Hg2 Sb2 C59 C60 92.4(6) . . . . ? C39 C40 C41 C42 -3.2(10) . . . . ? Sb2 C40 C41 C42 171.1(5) . . . . ? C39 C40 C41 C33 174.7(7) . . . . ? Sb2 C40 C41 C33 -11.0(10) . . . . ? C34 C33 C41 C40 179.8(7) . . . . ? Hg2 C33 C41 C40 0.6(10) . . . . ? C34 C33 C41 C42 -2.3(10) . . . . ? Hg2 C33 C41 C42 178.5(5) . . . . ? C46 C52 C51 C50 173.4(7) . . . . ? C47 C52 C51 C50 -6.9(11) . . . . ? C46 C52 C51 C43 -6.5(11) . . . . ? C47 C52 C51 C43 173.2(7) . . . . ? F2 Sb2 C53 C58 5.1(6) . . . . ? C40 Sb2 C53 C58 -75.3(7) . . . . ? C50 Sb2 C53 C58 87.5(6) . . . . ? C59 Sb2 C53 C58 -173.7(6) . . . . ? Hg2 Sb2 C53 C58 165.7(7) . . . . ? F2 Sb2 C53 C54 -168.7(6) . . . . ? C40 Sb2 C53 C54 110.9(6) . . . . ? C50 Sb2 C53 C54 -86.3(6) . . . . ? C59 Sb2 C53 C54 12.5(7) . . . . ? Hg2 Sb2 C53 C54 -8.1(15) . . . . ? C50 C51 C43 C44 -173.8(7) . . . . ? C52 C51 C43 C44 6.2(11) . . . . ? C50 C51 C43 Hg2 8.8(10) . . . . ? C52 C51 C43 Hg2 -171.3(5) . . . . ? C33 Hg2 C43 C44 155.1(19) . . . . ? F1 Hg2 C43 C44 -16.7(7) . . . . ? Sb2 Hg2 C43 C44 164.7(7) . . . . ? C33 Hg2 C43 C51 -28(3) . . . . ? F1 Hg2 C43 C51 160.7(6) . . . . ? Sb2 Hg2 C43 C51 -17.9(6) . . . . ? C64 C59 C60 C61 -0.7(11) . . . . ? Sb2 C59 C60 C61 176.4(6) . . . . ? F1 Sb1 C27 C28 77.3(13) . . . . ? C21 Sb1 C27 C28 -107.9(7) . . . . ? C18 Sb1 C27 C28 -6.0(7) . . . . ? C8 Sb1 C27 C28 148.0(7) . . . . ? Hg1 Sb1 C27 C28 70.9(6) . . . . ? F1 Sb1 C27 C32 -101.6(11) . . . . ? C21 Sb1 C27 C32 73.3(7) . . . . ? C18 Sb1 C27 C32 175.1(6) . . . . ? C8 Sb1 C27 C32 -30.9(7) . . . . ? Hg1 Sb1 C27 C32 -108.0(6) . . . . ? C43 C51 C50 C49 -173.8(7) . . . . ? C52 C51 C50 C49 6.3(10) . . . . ? C43 C51 C50 Sb2 15.7(11) . . . . ? C52 C51 C50 Sb2 -164.2(5) . . . . ? F2 Sb2 C50 C49 62.9(5) . . . . ? C53 Sb2 C50 C49 -24.1(6) . . . . ? C40 Sb2 C50 C49 125.2(6) . . . . ? C59 Sb2 C50 C49 -122.2(5) . . . . ? Hg2 Sb2 C50 C49 167.4(5) . . . . ? F2 Sb2 C50 C51 -125.6(6) . . . . ? C53 Sb2 C50 C51 147.3(6) . . . . ? C40 Sb2 C50 C51 -63.4(8) . . . . ? C59 Sb2 C50 C51 49.2(6) . . . . ? Hg2 Sb2 C50 C51 -21.1(6) . . . . ? C39 C38 C37 C42 -1.1(11) . . . . ? C19 C11 C12 C13 -1.9(11) . . . . ? Hg1 C11 C12 C13 180.0(6) . . . . ? C1 C2 C3 C4 -0.1(11) . . . . ? C41 C33 C34 C35 1.3(11) . . . . ? Hg2 C33 C34 C35 -179.4(6) . . . . ? C58 C53 C54 C55 -0.2(12) . . . . ? Sb2 C53 C54 C55 173.7(6) . . . . ? C33 C34 C35 C36 -0.2(12) . . . . ? C1 C9 C10 C4 3.1(10) . . . . ? C8 C9 C10 C4 -179.3(7) . . . . ? C1 C9 C10 C5 -176.0(7) . . . . ? C8 C9 C10 C5 1.6(10) . . . . ? C15 C20 C14 C13 175.0(8) . . . . ? C19 C20 C14 C13 -5.6(11) . . . . ? C21 C26 C25 C24 -2.0(12) . . . . ? C32 C27 C28 C29 -3.5(12) . . . . ? Sb1 C27 C28 C29 177.7(6) . . . . ? C20 C14 C13 C12 -1.0(12) . . . . ? C11 C12 C13 C14 4.9(12) . . . . ? C59 C60 C61 C62 2.8(12) . . . . ? C38 C37 C42 C36 -178.2(7) . . . . ? C38 C37 C42 C41 -0.1(11) . . . . ? C40 C41 C42 C37 2.2(10) . . . . ? C33 C41 C42 C37 -175.9(6) . . . . ? C40 C41 C42 C36 -179.8(6) . . . . ? C33 C41 C42 C36 2.2(10) . . . . ? C54 C53 C58 C57 -0.7(12) . . . . ? Sb2 C53 C58 C57 -174.5(6) . . . . ? C41 C40 C39 C38 2.2(11) . . . . ? Sb2 C40 C39 C38 -173.0(6) . . . . ? C37 C38 C39 C40 0.1(11) . . . . ? C34 C35 C36 C42 0.0(11) . . . . ? C37 C42 C36 C35 177.0(7) . . . . ? C41 C42 C36 C35 -1.1(11) . . . . ? C2 C3 C4 C10 -0.6(11) . . . . ? C9 C10 C4 C3 -0.9(11) . . . . ? C5 C10 C4 C3 178.2(7) . . . . ? C49 C48 C47 C52 2.7(12) . . . . ? C46 C52 C47 C48 -177.7(8) . . . . ? C51 C52 C47 C48 2.6(12) . . . . ? C19 C20 C15 C16 -1.6(13) . . . . ? C14 C20 C15 C16 177.9(8) . . . . ? C51 C43 C44 C45 -1.6(13) . . . . ? Hg2 C43 C44 C45 175.8(7) . . . . ? C51 C50 C49 C48 -1.3(11) . . . . ? Sb2 C50 C49 C48 170.6(6) . . . . ? C47 C48 C49 C50 -3.4(12) . . . . ? C47 C52 C46 C45 -177.4(8) . . . . ? C51 C52 C46 C45 2.3(12) . . . . ? C19 C18 C17 C16 3.6(12) . . . . ? Sb1 C18 C17 C16 -173.0(7) . . . . ? C60 C59 C64 C63 -0.2(12) . . . . ? Sb2 C59 C64 C63 -177.3(7) . . . . ? C26 C21 C22 C23 -2.3(13) . . . . ? Sb1 C21 C22 C23 177.6(7) . . . . ? C30 C31 C32 C27 -0.2(13) . . . . ? C28 C27 C32 C31 2.9(12) . . . . ? Sb1 C27 C32 C31 -178.2(6) . . . . ? C9 C8 C7 C6 0.4(12) . . . . ? Sb1 C8 C7 C6 -173.5(6) . . . . ? C4 C10 C5 C6 179.8(8) . . . . ? C9 C10 C5 C6 -1.2(11) . . . . ? C53 C58 C57 C56 2.2(12) . . . . ? C20 C15 C16 C17 -1.8(14) . . . . ? C18 C17 C16 C15 0.7(14) . . . . ? C27 C28 C29 C30 1.2(14) . . . . ? C26 C25 C24 C23 1.9(14) . . . . ? C32 C31 C30 C29 -2.1(14) . . . . ? C28 C29 C30 C31 1.6(14) . . . . ? C53 C54 C55 C56 -0.3(13) . . . . ? C52 C46 C45 C44 2.3(13) . . . . ? C43 C44 C45 C46 -2.8(14) . . . . ? C54 C55 C56 C57 1.8(14) . . . . ? C58 C57 C56 C55 -2.7(14) . . . . ? C10 C5 C6 C7 0.2(12) . . . . ? C8 C7 C6 C5 0.2(13) . . . . ? C59 C64 C63 C62 -1.0(14) . . . . ? C64 C63 C62 C61 3.0(15) . . . . ? C60 C61 C62 C63 -3.9(14) . . . . ? C25 C24 C23 C22 -2.0(15) . . . . ? C21 C22 C23 C24 2.2(15) . . . . ? O1 C65 C66 C67 33(3) . . . . ? C67 C68 O1 C65 59(2) . . . . ? C66 C65 O1 C68 -55(3) . . . . ? O1 C68 C67 C66 -43(3) . . . . ? C65 C66 C67 C68 5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.903 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.189 # Attachment '- 2-THF.cif' data_2-THF _database_code_depnum_ccdc_archive 'CCDC 853649' #TrackingRef '- 2-THF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2-THF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 F6 Hg O1.50 P Sb' _chemical_formula_weight 981.96 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' Sb Sb -0.5866 1.5461 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2206(15) _cell_length_b 21.054(2) _cell_length_c 13.5998(15) _cell_angle_alpha 90.00 _cell_angle_beta 118.1540(10) _cell_angle_gamma 90.00 _cell_volume 3337.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 5.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4539 _exptl_absorpt_correction_T_max 0.6665 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25560 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5249 _reflns_number_gt 4967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5249 _refine_ls_number_parameters 442 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0512 _refine_ls_wR_factor_gt 0.0503 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.103128(14) 0.378660(8) 0.260189(14) 0.01816(7) Uani 1 1 d . . . Sb1 Sb 0.25643(2) 0.486777(13) 0.25513(2) 0.01535(8) Uani 1 1 d . . . P1 P -0.24056(11) 0.30535(6) 0.15860(11) 0.0277(3) Uani 1 1 d . . . F6 F -0.2425(3) 0.30115(15) 0.2752(2) 0.0392(7) Uani 1 1 d . . . F4 F -0.2431(3) 0.22987(14) 0.1533(3) 0.0426(8) Uani 1 1 d . . . F1 F -0.1024(2) 0.30294(17) 0.2244(2) 0.0412(8) Uani 1 1 d . . . C32 C 0.4101(4) 0.3828(2) 0.2469(4) 0.0214(10) Uani 1 1 d . . . H32A H 0.3836 0.3986 0.1733 0.026 Uiso 1 1 calc R . . O1 O 0.1856(3) 0.26215(17) 0.3412(3) 0.0358(9) Uani 1 1 d . . . C28 C 0.4086(4) 0.3864(2) 0.4238(4) 0.0207(10) Uani 1 1 d . . . H28A H 0.3816 0.4045 0.4711 0.025 Uiso 1 1 calc R . . C9 C 0.1706(4) 0.4789(2) 0.4407(3) 0.0167(9) Uani 1 1 d . . . C8 C 0.2109(4) 0.5186(2) 0.3803(3) 0.0171(9) Uani 1 1 d . . . C19 C 0.0879(4) 0.4102(2) 0.0348(4) 0.0182(10) Uani 1 1 d . . . C27 C 0.3699(4) 0.4091(2) 0.3163(4) 0.0172(9) Uani 1 1 d . . . C22 C 0.3243(4) 0.6214(2) 0.2163(4) 0.0208(10) Uani 1 1 d . . . H22A H 0.2444 0.6298 0.1853 0.025 Uiso 1 1 calc R . . F2 F -0.3774(3) 0.30634(16) 0.0938(3) 0.0469(8) Uani 1 1 d . . . C21 C 0.3663(4) 0.5609(2) 0.2562(4) 0.0180(9) Uani 1 1 d . . . C30 C 0.5262(4) 0.3104(2) 0.3928(4) 0.0232(10) Uani 1 1 d . . . H30A H 0.5790 0.2761 0.4188 0.028 Uiso 1 1 calc R . . C11 C 0.0664(4) 0.3623(2) 0.0972(4) 0.0194(10) Uani 1 1 d . . . C29 C 0.4873(4) 0.3370(2) 0.4616(4) 0.0237(10) Uani 1 1 d . . . H29A H 0.5145 0.3213 0.5352 0.028 Uiso 1 1 calc R . . C10 C 0.1690(4) 0.5074(2) 0.5359(4) 0.0201(10) Uani 1 1 d . . . C18 C 0.1493(4) 0.4686(2) 0.0796(3) 0.0184(10) Uani 1 1 d . . . F3 F -0.2372(4) 0.38063(16) 0.1706(4) 0.0778(14) Uani 1 1 d . . . C4 C 0.1347(4) 0.4706(2) 0.6018(4) 0.0238(11) Uani 1 1 d . . . H4A H 0.1362 0.4889 0.6663 0.029 Uiso 1 1 calc R . . C20 C 0.0439(4) 0.4011(2) -0.0834(4) 0.0226(10) Uani 1 1 d . . . C25 C 0.5565(4) 0.5958(2) 0.3036(4) 0.0236(10) Uani 1 1 d . . . H25A H 0.6360 0.5872 0.3321 0.028 Uiso 1 1 calc R . . C15 C 0.0583(4) 0.4494(3) -0.1489(4) 0.0257(11) Uani 1 1 d . . . H15A H 0.0288 0.4428 -0.2268 0.031 Uiso 1 1 calc R . . C7 C 0.2359(4) 0.5813(2) 0.4069(4) 0.0213(10) Uani 1 1 d . . . H7A H 0.2612 0.6066 0.3649 0.026 Uiso 1 1 calc R . . C2 C 0.0964(4) 0.3822(2) 0.4787(4) 0.0241(11) Uani 1 1 d . . . H2A H 0.0695 0.3399 0.4592 0.029 Uiso 1 1 calc R . . C26 C 0.4828(4) 0.5479(2) 0.2998(4) 0.0183(9) Uani 1 1 d . . . H26A H 0.5116 0.5067 0.3267 0.022 Uiso 1 1 calc R . . C6 C 0.2249(4) 0.6090(2) 0.4957(4) 0.0257(11) Uani 1 1 d . . . H6A H 0.2377 0.6532 0.5100 0.031 Uiso 1 1 calc R . . C23 C 0.3979(4) 0.6690(2) 0.2217(4) 0.0240(10) Uani 1 1 d . . . H23A H 0.3692 0.7104 0.1954 0.029 Uiso 1 1 calc R . . C1 C 0.1310(4) 0.4151(2) 0.4121(4) 0.0182(9) Uani 1 1 d . . . C3 C 0.0997(4) 0.4094(2) 0.5747(4) 0.0250(11) Uani 1 1 d . . . H3A H 0.0776 0.3852 0.6203 0.030 Uiso 1 1 calc R . . C17 C 0.1594(4) 0.5139(2) 0.0122(4) 0.0214(10) Uani 1 1 d . . . H17A H 0.1987 0.5524 0.0441 0.026 Uiso 1 1 calc R . . C12 C 0.0061(4) 0.3092(2) 0.0430(4) 0.0232(10) Uani 1 1 d . . . H12A H -0.0093 0.2779 0.0844 0.028 Uiso 1 1 calc R . . C5 C 0.1960(4) 0.5724(2) 0.5606(4) 0.0235(10) Uani 1 1 d . . . H5A H 0.1938 0.5907 0.6235 0.028 Uiso 1 1 calc R . . C16 C 0.1127(4) 0.5042(3) -0.1032(4) 0.0269(11) Uani 1 1 d . . . H16A H 0.1194 0.5363 -0.1490 0.032 Uiso 1 1 calc R . . C31 C 0.4884(4) 0.3338(2) 0.2859(4) 0.0242(11) Uani 1 1 d . . . H31A H 0.5166 0.3160 0.2393 0.029 Uiso 1 1 calc R . . C14 C -0.0155(4) 0.3444(2) -0.1330(4) 0.0263(11) Uani 1 1 d . . . H14A H -0.0430 0.3377 -0.2106 0.032 Uiso 1 1 calc R . . C24 C 0.5142(4) 0.6566(2) 0.2655(4) 0.0243(11) Uani 1 1 d . . . H24A H 0.5651 0.6895 0.2697 0.029 Uiso 1 1 calc R . . F5 F -0.2391(3) 0.3095(3) 0.0440(3) 0.0801(15) Uani 1 1 d . . . C13 C -0.0338(4) 0.2992(2) -0.0714(4) 0.0284(11) Uani 1 1 d . . . H13A H -0.0734 0.2612 -0.1057 0.034 Uiso 1 1 calc R . . C33 C 0.2483(5) 0.2471(3) 0.4576(4) 0.0324(12) Uani 1 1 d . . . H33A H 0.1950 0.2377 0.4879 0.039 Uiso 1 1 calc R . . H33B H 0.2979 0.2832 0.4997 0.039 Uiso 1 1 calc R . . C36 C 0.2295(6) 0.2258(3) 0.2825(5) 0.0439(15) Uani 1 1 d . . . H36A H 0.2887 0.2502 0.2735 0.053 Uiso 1 1 calc R . . H36B H 0.1673 0.2145 0.2076 0.053 Uiso 1 1 calc R . . C34 C 0.3206(5) 0.1892(3) 0.4669(5) 0.0474(15) Uani 1 1 d . . . H34A H 0.4030 0.2004 0.5027 0.057 Uiso 1 1 calc R . . H34B H 0.3091 0.1556 0.5116 0.057 Uiso 1 1 calc R . . C35 C 0.2805(6) 0.1673(3) 0.3501(5) 0.0420(14) Uani 1 1 d . . . H35A H 0.2224 0.1332 0.3298 0.050 Uiso 1 1 calc R . . H35B H 0.3454 0.1514 0.3398 0.050 Uiso 1 1 calc R . . C38 C -0.4223(7) 0.4686(4) -0.0009(6) 0.068(2) Uani 1 1 d D . . H38A H -0.3389 0.4598 0.0344 0.081 Uiso 1 1 calc R . . H38B H -0.4595 0.4328 -0.0529 0.081 Uiso 1 1 calc R . . O2 O -0.4383(7) 0.5229(4) -0.0737(7) 0.046(2) Uani 0.50 1 d PD . . C37 C -0.5467(7) 0.5415(5) -0.0914(8) 0.104(4) Uani 1 1 d D . . H37A H -0.6042 0.5188 -0.1582 0.125 Uiso 1 1 calc R . . H37B H -0.5552 0.5873 -0.1097 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.02035(11) 0.01731(10) 0.01873(10) -0.00337(7) 0.01078(8) -0.00341(7) Sb1 0.01650(16) 0.01582(16) 0.01515(15) -0.00088(11) 0.00864(12) -0.00063(11) P1 0.0230(7) 0.0252(7) 0.0258(7) 0.0058(5) 0.0040(5) -0.0051(5) F6 0.0381(18) 0.0445(19) 0.0344(17) -0.0089(14) 0.0167(14) 0.0049(14) F4 0.0433(19) 0.0267(17) 0.053(2) -0.0157(15) 0.0190(16) -0.0013(14) F1 0.0219(16) 0.064(2) 0.0295(16) 0.0132(15) 0.0052(13) -0.0123(14) C32 0.028(3) 0.019(2) 0.020(2) 0.0006(19) 0.014(2) -0.0005(19) O1 0.040(2) 0.034(2) 0.034(2) 0.0065(16) 0.0189(18) 0.0136(17) C28 0.019(2) 0.027(3) 0.019(2) -0.0027(19) 0.011(2) -0.0017(19) C9 0.012(2) 0.023(2) 0.016(2) -0.0012(18) 0.0067(18) 0.0024(18) C8 0.014(2) 0.024(2) 0.015(2) -0.0035(18) 0.0073(18) 0.0017(18) C19 0.012(2) 0.027(3) 0.015(2) -0.0024(19) 0.0062(18) 0.0061(19) C27 0.018(2) 0.013(2) 0.022(2) -0.0004(18) 0.0097(19) -0.0001(18) C22 0.020(2) 0.023(3) 0.023(2) 0.0017(19) 0.013(2) 0.0019(19) F2 0.0222(16) 0.050(2) 0.050(2) 0.0033(16) 0.0013(15) 0.0018(14) C21 0.020(2) 0.020(2) 0.018(2) -0.0003(18) 0.0124(19) -0.0023(19) C30 0.021(2) 0.019(2) 0.026(3) 0.002(2) 0.008(2) 0.0023(19) C11 0.013(2) 0.025(2) 0.017(2) -0.0044(19) 0.0053(19) 0.0032(19) C29 0.018(2) 0.031(3) 0.017(2) 0.005(2) 0.004(2) 0.001(2) C10 0.016(2) 0.027(3) 0.017(2) -0.0028(19) 0.0071(19) 0.0010(19) C18 0.016(2) 0.026(3) 0.014(2) -0.0024(18) 0.0071(18) 0.0040(19) F3 0.071(3) 0.025(2) 0.093(3) 0.0207(19) 0.001(2) -0.0079(18) C4 0.022(3) 0.033(3) 0.018(2) 0.000(2) 0.011(2) 0.004(2) C20 0.015(2) 0.032(3) 0.021(2) -0.003(2) 0.009(2) 0.009(2) C25 0.021(2) 0.028(3) 0.025(2) -0.002(2) 0.014(2) 0.000(2) C15 0.017(2) 0.046(3) 0.016(2) 0.000(2) 0.009(2) 0.010(2) C7 0.021(2) 0.020(2) 0.026(2) -0.0024(19) 0.014(2) -0.0028(19) C2 0.026(3) 0.021(3) 0.029(3) 0.001(2) 0.016(2) 0.000(2) C26 0.019(2) 0.019(2) 0.019(2) -0.0007(18) 0.0108(19) 0.0012(19) C6 0.025(3) 0.024(3) 0.033(3) -0.010(2) 0.017(2) -0.006(2) C23 0.031(3) 0.018(2) 0.028(3) 0.005(2) 0.018(2) 0.004(2) C1 0.019(2) 0.018(2) 0.018(2) -0.0018(18) 0.0085(19) -0.0002(18) C3 0.025(3) 0.029(3) 0.026(3) 0.006(2) 0.017(2) 0.003(2) C17 0.017(2) 0.028(3) 0.020(2) 0.002(2) 0.010(2) 0.0018(19) C12 0.018(2) 0.024(3) 0.026(3) -0.003(2) 0.010(2) 0.001(2) C5 0.020(2) 0.027(3) 0.025(2) -0.011(2) 0.012(2) -0.004(2) C16 0.023(3) 0.037(3) 0.023(3) 0.006(2) 0.013(2) 0.006(2) C31 0.030(3) 0.020(2) 0.026(3) -0.004(2) 0.016(2) 0.001(2) C14 0.017(2) 0.039(3) 0.018(2) -0.009(2) 0.005(2) 0.006(2) C24 0.031(3) 0.021(3) 0.028(3) -0.001(2) 0.019(2) -0.007(2) F5 0.043(2) 0.164(5) 0.0256(18) 0.028(2) 0.0100(16) -0.017(3) C13 0.020(3) 0.028(3) 0.028(3) -0.011(2) 0.004(2) 0.002(2) C33 0.036(3) 0.035(3) 0.028(3) -0.002(2) 0.016(2) -0.005(2) C36 0.061(4) 0.034(3) 0.033(3) -0.001(3) 0.020(3) 0.014(3) C34 0.044(4) 0.046(4) 0.039(3) 0.007(3) 0.009(3) 0.011(3) C35 0.059(4) 0.033(3) 0.047(3) 0.013(3) 0.035(3) 0.015(3) C38 0.071(5) 0.078(5) 0.061(5) 0.035(4) 0.038(4) 0.029(4) O2 0.050(5) 0.050(5) 0.054(5) 0.031(4) 0.037(4) 0.019(4) C37 0.093(7) 0.131(9) 0.136(9) -0.060(7) 0.091(7) -0.023(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C11 2.062(4) . ? Hg1 C1 2.067(4) . ? Hg1 O1 2.700(3) . ? Hg1 F1 2.986(3) . ? Hg1 Sb1 3.0701(4) . ? Sb1 C27 2.107(4) . ? Sb1 C21 2.127(4) . ? Sb1 C18 2.159(4) . ? Sb1 C8 2.162(4) . ? P1 F5 1.571(4) . ? P1 F4 1.590(3) . ? P1 F3 1.592(4) . ? P1 F2 1.595(3) . ? P1 F6 1.600(3) . ? P1 F1 1.612(3) . ? C32 C31 1.379(7) . ? C32 C27 1.397(6) . ? C32 H32A 0.9500 . ? O1 C36 1.413(6) . ? O1 C33 1.434(6) . ? C28 C27 1.387(6) . ? C28 C29 1.388(7) . ? C28 H28A 0.9500 . ? C9 C1 1.427(6) . ? C9 C10 1.436(6) . ? C9 C8 1.438(6) . ? C8 C7 1.368(6) . ? C19 C11 1.432(7) . ? C19 C18 1.439(6) . ? C19 C20 1.440(6) . ? C22 C23 1.375(7) . ? C22 C21 1.393(6) . ? C22 H22A 0.9500 . ? C21 C26 1.392(6) . ? C30 C29 1.381(7) . ? C30 C31 1.386(7) . ? C30 H30A 0.9500 . ? C11 C12 1.369(7) . ? C29 H29A 0.9500 . ? C10 C4 1.412(7) . ? C10 C5 1.415(7) . ? C18 C17 1.373(6) . ? C4 C3 1.358(7) . ? C4 H4A 0.9500 . ? C20 C14 1.412(7) . ? C20 C15 1.423(7) . ? C25 C26 1.386(6) . ? C25 C24 1.394(7) . ? C25 H25A 0.9500 . ? C15 C16 1.347(7) . ? C15 H15A 0.9500 . ? C7 C6 1.409(7) . ? C7 H7A 0.9500 . ? C2 C1 1.379(6) . ? C2 C3 1.407(7) . ? C2 H2A 0.9500 . ? C26 H26A 0.9500 . ? C6 C5 1.356(7) . ? C6 H6A 0.9500 . ? C23 C24 1.386(7) . ? C23 H23A 0.9500 . ? C3 H3A 0.9500 . ? C17 C16 1.404(7) . ? C17 H17A 0.9500 . ? C12 C13 1.402(7) . ? C12 H12A 0.9500 . ? C5 H5A 0.9500 . ? C16 H16A 0.9500 . ? C31 H31A 0.9500 . ? C14 C13 1.363(7) . ? C14 H14A 0.9500 . ? C24 H24A 0.9500 . ? C13 H13A 0.9500 . ? C33 C34 1.517(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C36 C35 1.495(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C34 C35 1.491(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C38 O2 1.460(9) . ? C38 C37 1.508(10) 3_465 ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? O2 C37 1.393(10) . ? C37 C38 1.508(10) 3_465 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Hg1 C1 167.59(18) . . ? C11 Hg1 O1 97.59(15) . . ? C1 Hg1 O1 94.72(14) . . ? C11 Hg1 F1 90.05(14) . . ? C1 Hg1 F1 94.64(14) . . ? O1 Hg1 F1 75.08(10) . . ? C11 Hg1 Sb1 85.58(13) . . ? C1 Hg1 Sb1 86.48(12) . . ? O1 Hg1 Sb1 122.63(8) . . ? F1 Hg1 Sb1 162.16(6) . . ? C27 Sb1 C21 102.13(17) . . ? C27 Sb1 C18 105.79(17) . . ? C21 Sb1 C18 103.14(17) . . ? C27 Sb1 C8 109.91(16) . . ? C21 Sb1 C8 102.15(17) . . ? C18 Sb1 C8 130.11(16) . . ? C27 Sb1 Hg1 76.72(12) . . ? C21 Sb1 Hg1 178.39(12) . . ? C18 Sb1 Hg1 78.31(12) . . ? C8 Sb1 Hg1 77.28(12) . . ? F5 P1 F4 91.2(2) . . ? F5 P1 F3 91.9(3) . . ? F4 P1 F3 176.9(2) . . ? F5 P1 F2 89.5(2) . . ? F4 P1 F2 89.65(18) . . ? F3 P1 F2 90.8(2) . . ? F5 P1 F6 179.8(2) . . ? F4 P1 F6 88.83(18) . . ? F3 P1 F6 88.1(2) . . ? F2 P1 F6 90.24(18) . . ? F5 P1 F1 90.64(19) . . ? F4 P1 F1 89.31(18) . . ? F3 P1 F1 90.3(2) . . ? F2 P1 F1 178.9(2) . . ? F6 P1 F1 89.57(16) . . ? P1 F1 Hg1 141.23(17) . . ? C31 C32 C27 119.5(4) . . ? C31 C32 H32A 120.2 . . ? C27 C32 H32A 120.2 . . ? C36 O1 C33 109.1(4) . . ? C36 O1 Hg1 117.1(3) . . ? C33 O1 Hg1 124.3(3) . . ? C27 C28 C29 119.2(4) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C1 C9 C10 118.6(4) . . ? C1 C9 C8 125.3(4) . . ? C10 C9 C8 116.1(4) . . ? C7 C8 C9 121.2(4) . . ? C7 C8 Sb1 112.6(3) . . ? C9 C8 Sb1 125.9(3) . . ? C11 C19 C18 125.5(4) . . ? C11 C19 C20 118.6(4) . . ? C18 C19 C20 115.9(4) . . ? C28 C27 C32 120.5(4) . . ? C28 C27 Sb1 121.6(3) . . ? C32 C27 Sb1 117.9(3) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C26 C21 C22 120.2(4) . . ? C26 C21 Sb1 118.3(3) . . ? C22 C21 Sb1 121.5(3) . . ? C29 C30 C31 120.1(4) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C12 C11 C19 119.0(4) . . ? C12 C11 Hg1 119.8(4) . . ? C19 C11 Hg1 120.5(3) . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C4 C10 C5 120.1(4) . . ? C4 C10 C9 119.3(4) . . ? C5 C10 C9 120.6(4) . . ? C17 C18 C19 121.6(4) . . ? C17 C18 Sb1 113.3(3) . . ? C19 C18 Sb1 124.4(3) . . ? C3 C4 C10 121.2(4) . . ? C3 C4 H4A 119.4 . . ? C10 C4 H4A 119.4 . . ? C14 C20 C15 120.8(4) . . ? C14 C20 C19 119.2(4) . . ? C15 C20 C19 120.0(4) . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C16 C15 C20 121.6(4) . . ? C16 C15 H15A 119.2 . . ? C20 C15 H15A 119.2 . . ? C8 C7 C6 121.1(4) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C1 C2 C3 122.0(4) . . ? C1 C2 H2A 119.0 . . ? C3 C2 H2A 119.0 . . ? C25 C26 C21 119.4(4) . . ? C25 C26 H26A 120.3 . . ? C21 C26 H26A 120.3 . . ? C5 C6 C7 119.9(4) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C2 C1 C9 119.1(4) . . ? C2 C1 Hg1 120.8(3) . . ? C9 C1 Hg1 119.4(3) . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C18 C17 C16 121.0(5) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C11 C12 C13 122.5(5) . . ? C11 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C6 C5 C10 120.7(4) . . ? C6 C5 H5A 119.6 . . ? C10 C5 H5A 119.6 . . ? C15 C16 C17 119.8(5) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C32 C31 C30 120.2(4) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C13 C14 C20 121.0(4) . . ? C13 C14 H14A 119.5 . . ? C20 C14 H14A 119.5 . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? O1 C33 C34 106.4(4) . . ? O1 C33 H33A 110.4 . . ? C34 C33 H33A 110.4 . . ? O1 C33 H33B 110.4 . . ? C34 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? O1 C36 C35 106.6(5) . . ? O1 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? O1 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C35 C34 C33 105.5(5) . . ? C35 C34 H34A 110.6 . . ? C33 C34 H34A 110.6 . . ? C35 C34 H34B 110.6 . . ? C33 C34 H34B 110.6 . . ? H34A C34 H34B 108.8 . . ? C34 C35 C36 103.3(5) . . ? C34 C35 H35A 111.1 . . ? C36 C35 H35A 111.1 . . ? C34 C35 H35B 111.1 . . ? C36 C35 H35B 111.1 . . ? H35A C35 H35B 109.1 . . ? O2 C38 C37 131.7(8) . 3_465 ? O2 C38 H38A 104.3 . . ? C37 C38 H38A 104.3 3_465 . ? O2 C38 H38B 104.3 . . ? C37 C38 H38B 104.3 3_465 . ? H38A C38 H38B 105.6 . . ? C37 O2 C38 98.4(7) . . ? O2 C37 C38 118.6(9) . 3_465 ? O2 C37 H37A 107.7 . . ? C38 C37 H37A 107.7 3_465 . ? O2 C37 H37B 107.7 . . ? C38 C37 H37B 107.7 3_465 . ? H37A C37 H37B 107.1 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Hg1 Sb1 C27 -92.34(17) . . . . ? C1 Hg1 Sb1 C27 97.21(17) . . . . ? O1 Hg1 Sb1 C27 3.85(15) . . . . ? F1 Hg1 Sb1 C27 -168.6(2) . . . . ? C11 Hg1 Sb1 C21 -137(4) . . . . ? C1 Hg1 Sb1 C21 53(4) . . . . ? O1 Hg1 Sb1 C21 -41(4) . . . . ? F1 Hg1 Sb1 C21 147(4) . . . . ? C11 Hg1 Sb1 C18 17.19(17) . . . . ? C1 Hg1 Sb1 C18 -153.26(17) . . . . ? O1 Hg1 Sb1 C18 113.38(15) . . . . ? F1 Hg1 Sb1 C18 -59.1(2) . . . . ? C11 Hg1 Sb1 C8 153.33(17) . . . . ? C1 Hg1 Sb1 C8 -17.12(17) . . . . ? O1 Hg1 Sb1 C8 -110.48(15) . . . . ? F1 Hg1 Sb1 C8 77.1(2) . . . . ? F5 P1 F1 Hg1 60.0(3) . . . . ? F4 P1 F1 Hg1 151.2(3) . . . . ? F3 P1 F1 Hg1 -31.9(3) . . . . ? F2 P1 F1 Hg1 160(11) . . . . ? F6 P1 F1 Hg1 -120.0(3) . . . . ? C11 Hg1 F1 P1 -69.2(3) . . . . ? C1 Hg1 F1 P1 99.3(3) . . . . ? O1 Hg1 F1 P1 -167.0(3) . . . . ? Sb1 Hg1 F1 P1 6.4(5) . . . . ? C11 Hg1 O1 C36 23.9(4) . . . . ? C1 Hg1 O1 C36 -154.6(4) . . . . ? F1 Hg1 O1 C36 111.9(4) . . . . ? Sb1 Hg1 O1 C36 -65.7(4) . . . . ? C11 Hg1 O1 C33 166.4(4) . . . . ? C1 Hg1 O1 C33 -12.1(4) . . . . ? F1 Hg1 O1 C33 -105.6(4) . . . . ? Sb1 Hg1 O1 C33 76.8(4) . . . . ? C1 C9 C8 C7 173.1(4) . . . . ? C10 C9 C8 C7 -5.7(6) . . . . ? C1 C9 C8 Sb1 -14.1(6) . . . . ? C10 C9 C8 Sb1 167.1(3) . . . . ? C27 Sb1 C8 C7 123.2(3) . . . . ? C21 Sb1 C8 C7 15.4(4) . . . . ? C18 Sb1 C8 C7 -103.7(4) . . . . ? Hg1 Sb1 C8 C7 -166.2(3) . . . . ? C27 Sb1 C8 C9 -50.1(4) . . . . ? C21 Sb1 C8 C9 -158.0(4) . . . . ? C18 Sb1 C8 C9 83.0(4) . . . . ? Hg1 Sb1 C8 C9 20.5(3) . . . . ? C29 C28 C27 C32 -0.4(7) . . . . ? C29 C28 C27 Sb1 -177.1(3) . . . . ? C31 C32 C27 C28 0.2(7) . . . . ? C31 C32 C27 Sb1 177.1(3) . . . . ? C21 Sb1 C27 C28 105.7(4) . . . . ? C18 Sb1 C27 C28 -146.7(4) . . . . ? C8 Sb1 C27 C28 -2.2(4) . . . . ? Hg1 Sb1 C27 C28 -73.2(3) . . . . ? C21 Sb1 C27 C32 -71.2(4) . . . . ? C18 Sb1 C27 C32 36.4(4) . . . . ? C8 Sb1 C27 C32 -179.0(3) . . . . ? Hg1 Sb1 C27 C32 110.0(3) . . . . ? C23 C22 C21 C26 -1.2(7) . . . . ? C23 C22 C21 Sb1 177.6(3) . . . . ? C27 Sb1 C21 C26 -4.1(4) . . . . ? C18 Sb1 C21 C26 -113.8(3) . . . . ? C8 Sb1 C21 C26 109.6(3) . . . . ? Hg1 Sb1 C21 C26 40(4) . . . . ? C27 Sb1 C21 C22 177.0(4) . . . . ? C18 Sb1 C21 C22 67.3(4) . . . . ? C8 Sb1 C21 C22 -69.3(4) . . . . ? Hg1 Sb1 C21 C22 -139(4) . . . . ? C18 C19 C11 C12 179.7(4) . . . . ? C20 C19 C11 C12 0.8(6) . . . . ? C18 C19 C11 Hg1 9.0(6) . . . . ? C20 C19 C11 Hg1 -169.8(3) . . . . ? C1 Hg1 C11 C12 -138.6(7) . . . . ? O1 Hg1 C11 C12 48.7(4) . . . . ? F1 Hg1 C11 C12 -26.2(4) . . . . ? Sb1 Hg1 C11 C12 171.1(4) . . . . ? C1 Hg1 C11 C19 32.0(10) . . . . ? O1 Hg1 C11 C19 -140.7(3) . . . . ? F1 Hg1 C11 C19 144.3(3) . . . . ? Sb1 Hg1 C11 C19 -18.3(3) . . . . ? C31 C30 C29 C28 1.1(7) . . . . ? C27 C28 C29 C30 -0.3(7) . . . . ? C1 C9 C10 C4 3.5(6) . . . . ? C8 C9 C10 C4 -177.5(4) . . . . ? C1 C9 C10 C5 -173.4(4) . . . . ? C8 C9 C10 C5 5.5(6) . . . . ? C11 C19 C18 C17 -175.6(4) . . . . ? C20 C19 C18 C17 3.3(6) . . . . ? C11 C19 C18 Sb1 15.4(6) . . . . ? C20 C19 C18 Sb1 -165.7(3) . . . . ? C27 Sb1 C18 C17 -118.3(3) . . . . ? C21 Sb1 C18 C17 -11.5(4) . . . . ? C8 Sb1 C18 C17 107.2(3) . . . . ? Hg1 Sb1 C18 C17 169.2(3) . . . . ? C27 Sb1 C18 C19 51.5(4) . . . . ? C21 Sb1 C18 C19 158.3(3) . . . . ? C8 Sb1 C18 C19 -83.0(4) . . . . ? Hg1 Sb1 C18 C19 -21.0(3) . . . . ? C5 C10 C4 C3 174.8(4) . . . . ? C9 C10 C4 C3 -2.2(7) . . . . ? C11 C19 C20 C14 -2.2(6) . . . . ? C18 C19 C20 C14 178.8(4) . . . . ? C11 C19 C20 C15 176.5(4) . . . . ? C18 C19 C20 C15 -2.4(6) . . . . ? C14 C20 C15 C16 178.7(4) . . . . ? C19 C20 C15 C16 0.0(7) . . . . ? C9 C8 C7 C6 1.1(7) . . . . ? Sb1 C8 C7 C6 -172.6(4) . . . . ? C24 C25 C26 C21 1.0(7) . . . . ? C22 C21 C26 C25 0.3(6) . . . . ? Sb1 C21 C26 C25 -178.6(3) . . . . ? C8 C7 C6 C5 4.2(7) . . . . ? C21 C22 C23 C24 0.9(7) . . . . ? C3 C2 C1 C9 -0.5(7) . . . . ? C3 C2 C1 Hg1 -171.1(4) . . . . ? C10 C9 C1 C2 -2.2(6) . . . . ? C8 C9 C1 C2 179.0(4) . . . . ? C10 C9 C1 Hg1 168.5(3) . . . . ? C8 C9 C1 Hg1 -10.3(6) . . . . ? C11 Hg1 C1 C2 139.1(7) . . . . ? O1 Hg1 C1 C2 -48.1(4) . . . . ? F1 Hg1 C1 C2 27.3(4) . . . . ? Sb1 Hg1 C1 C2 -170.6(4) . . . . ? C11 Hg1 C1 C9 -31.4(10) . . . . ? O1 Hg1 C1 C9 141.4(3) . . . . ? F1 Hg1 C1 C9 -143.3(3) . . . . ? Sb1 Hg1 C1 C9 18.9(3) . . . . ? C10 C4 C3 C2 -0.6(7) . . . . ? C1 C2 C3 C4 2.0(7) . . . . ? C19 C18 C17 C16 -1.7(7) . . . . ? Sb1 C18 C17 C16 168.4(3) . . . . ? C19 C11 C12 C13 1.2(7) . . . . ? Hg1 C11 C12 C13 172.0(4) . . . . ? C7 C6 C5 C10 -4.3(7) . . . . ? C4 C10 C5 C6 -177.6(4) . . . . ? C9 C10 C5 C6 -0.6(7) . . . . ? C20 C15 C16 C17 1.8(7) . . . . ? C18 C17 C16 C15 -0.9(7) . . . . ? C27 C32 C31 C30 0.6(7) . . . . ? C29 C30 C31 C32 -1.3(7) . . . . ? C15 C20 C14 C13 -177.1(4) . . . . ? C19 C20 C14 C13 1.6(7) . . . . ? C22 C23 C24 C25 0.4(7) . . . . ? C26 C25 C24 C23 -1.3(7) . . . . ? C20 C14 C13 C12 0.4(7) . . . . ? C11 C12 C13 C14 -1.9(7) . . . . ? C36 O1 C33 C34 -10.7(6) . . . . ? Hg1 O1 C33 C34 -155.7(3) . . . . ? C33 O1 C36 C35 26.2(6) . . . . ? Hg1 O1 C36 C35 174.1(4) . . . . ? O1 C33 C34 C35 -8.9(6) . . . . ? C33 C34 C35 C36 23.6(7) . . . . ? O1 C36 C35 C34 -30.8(7) . . . . ? C37 C38 O2 C37 -38.9(14) 3_465 . . . ? C38 O2 C37 C38 32.3(12) . . . 3_465 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.689 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.091