Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'F. Gabbai' _publ_contact_author_email FRANCOIS@TAMU.EDU loop_ _publ_author_name F.Gabbai 'Ching-Wen Chiu' C.L.Dorsey J.D.Hoefelmeyer ; N.R.Honesty ; T.W.Hudnall P.Jewula M.Schulte T.J.Taylor data_f _database_code_depnum_ccdc_archive 'CCDC 675714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 1-{Mes2B}-(m2-F)-8-{Me2B}C10H6 _chemical_formula_sum 'C36 H52 B2 F N3 S' _chemical_formula_weight 599.49 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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.5814(15) _cell_length_b 17.441(2) _cell_length_c 20.6449(19) _cell_angle_alpha 90.00 _cell_angle_beta 114.742(5) _cell_angle_gamma 90.00 _cell_volume 3460.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 915 _cell_measurement_theta_min 4.238 _cell_measurement_theta_max 40.455 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15743 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5424 _reflns_number_gt 3526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1593P)^2^+0.1429P] 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 5424 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1346 _refine_ls_R_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.2574 _refine_ls_wR_factor_gt 0.2222 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _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 S1 S 0.13841(11) 0.29167(6) 0.36213(6) 0.0323(4) Uani 1 1 d . . . F1 F 0.6593(2) 0.04657(13) 0.27822(11) 0.0321(6) Uani 1 1 d . . . C1 C 0.4234(4) 0.0252(2) 0.2788(2) 0.0300(10) Uani 1 1 d . . . C2 C 0.3344(4) 0.0343(2) 0.3111(2) 0.0343(11) Uani 1 1 d . . . H2A H 0.3730 0.0421 0.3612 0.041 Uiso 1 1 calc R . . C3 C 0.1884(5) 0.0325(2) 0.2735(3) 0.0410(12) Uani 1 1 d . . . H3A H 0.1309 0.0381 0.2983 0.049 Uiso 1 1 calc R . . C4 C 0.1306(5) 0.0229(3) 0.2021(3) 0.0433(12) Uani 1 1 d . . . H4A H 0.0322 0.0209 0.1769 0.052 Uiso 1 1 calc R . . C5 C 0.1547(6) 0.0051(3) 0.0894(3) 0.0491(14) Uani 1 1 d . . . H5A H 0.0564 0.0037 0.0639 0.059 Uiso 1 1 calc R . . C6 C 0.2366(6) -0.0031(3) 0.0537(3) 0.0540(15) Uani 1 1 d . . . H6A H 0.1953 -0.0117 0.0037 0.065 Uiso 1 1 calc R . . C7 C 0.3800(6) 0.0012(3) 0.0902(2) 0.0473(13) Uani 1 1 d . . . H7A H 0.4346 -0.0035 0.0637 0.057 Uiso 1 1 calc R . . C8 C 0.4484(5) 0.0119(2) 0.1637(2) 0.0352(11) Uani 1 1 d . . . C9 C 0.3627(4) 0.0176(2) 0.2025(2) 0.0321(10) Uani 1 1 d . . . C10 C 0.2153(5) 0.0156(2) 0.1643(2) 0.0375(11) Uani 1 1 d . . . C11 C 0.6314(4) 0.0866(2) 0.3907(2) 0.0297(10) Uani 1 1 d . . . C12 C 0.6696(4) 0.0707(2) 0.4638(2) 0.0302(10) Uani 1 1 d . . . C13 C 0.7059(4) 0.1299(3) 0.5140(2) 0.0357(11) Uani 1 1 d . . . H13A H 0.7330 0.1174 0.5628 0.043 Uiso 1 1 calc R . . C14 C 0.7036(4) 0.2071(2) 0.4948(2) 0.0347(11) Uani 1 1 d . . . C15 C 0.6582(4) 0.2225(2) 0.4231(2) 0.0323(10) Uani 1 1 d . . . H15A H 0.6501 0.2745 0.4083 0.039 Uiso 1 1 calc R . . C16 C 0.6236(4) 0.1652(2) 0.3715(2) 0.0285(10) Uani 1 1 d . . . C17 C 0.6737(5) -0.0088(2) 0.4927(2) 0.0361(11) Uani 1 1 d . . . H17A H 0.7028 -0.0062 0.5444 0.054 Uiso 1 1 calc R . . H17B H 0.7401 -0.0401 0.4825 0.054 Uiso 1 1 calc R . . H17C H 0.5810 -0.0319 0.4701 0.054 Uiso 1 1 calc R . . C18 C 0.7407(5) 0.2698(3) 0.5501(3) 0.0478(13) Uani 1 1 d . . . H18A H 0.7332 0.3197 0.5270 0.072 Uiso 1 1 calc R . . H18B H 0.8362 0.2623 0.5859 0.072 Uiso 1 1 calc R . . H18C H 0.6767 0.2681 0.5733 0.072 Uiso 1 1 calc R . . C19 C 0.5772(4) 0.1921(2) 0.2953(2) 0.0310(10) Uani 1 1 d . . . H19A H 0.5797 0.2482 0.2943 0.047 Uiso 1 1 calc R . . H19B H 0.4821 0.1743 0.2667 0.047 Uiso 1 1 calc R . . H19C H 0.6398 0.1712 0.2757 0.047 Uiso 1 1 calc R . . C21 C 0.6572(4) -0.0658(2) 0.3534(2) 0.0295(10) Uani 1 1 d . . . C22 C 0.8044(4) -0.0737(2) 0.3827(2) 0.0323(10) Uani 1 1 d . . . C23 C 0.8675(5) -0.1452(3) 0.4026(2) 0.0365(11) Uani 1 1 d . . . H23A H 0.9662 -0.1482 0.4222 0.044 Uiso 1 1 calc R . . C24 C 0.7921(5) -0.2119(2) 0.3949(2) 0.0360(11) Uani 1 1 d . . . C25 C 0.6498(5) -0.2051(2) 0.3666(2) 0.0328(11) Uani 1 1 d . . . H25A H 0.5959 -0.2503 0.3606 0.039 Uiso 1 1 calc R . . C26 C 0.5801(4) -0.1348(2) 0.3461(2) 0.0313(10) Uani 1 1 d . . . C27 C 0.9011(4) -0.0067(3) 0.3942(2) 0.0382(11) Uani 1 1 d . . . H27A H 0.9976 -0.0248 0.4148 0.057 Uiso 1 1 calc R . . H27B H 0.8881 0.0300 0.4269 0.057 Uiso 1 1 calc R . . H27C H 0.8805 0.0185 0.3484 0.057 Uiso 1 1 calc R . . C28 C 0.8620(5) -0.2898(3) 0.4163(3) 0.0483(13) Uani 1 1 d . . . H28A H 0.7908 -0.3295 0.4067 0.072 Uiso 1 1 calc R . . H28B H 0.9241 -0.2895 0.4673 0.072 Uiso 1 1 calc R . . H28C H 0.9160 -0.3006 0.3887 0.072 Uiso 1 1 calc R . . C29 C 0.4238(4) -0.1388(2) 0.3187(2) 0.0367(11) Uani 1 1 d . . . H29A H 0.3953 -0.1922 0.3186 0.055 Uiso 1 1 calc R . . H29B H 0.3808 -0.1184 0.2700 0.055 Uiso 1 1 calc R . . H29C H 0.3938 -0.1083 0.3496 0.055 Uiso 1 1 calc R . . C31 C 0.6887(6) -0.0615(3) 0.2005(3) 0.0579(15) Uani 1 1 d . . . H31A H 0.7898 -0.0545 0.2215 0.087 Uiso 1 1 calc R . . H31B H 0.6577 -0.0820 0.1520 0.087 Uiso 1 1 calc R . . H31C H 0.6638 -0.0975 0.2297 0.087 Uiso 1 1 calc R . . C32 C 0.6707(5) 0.0865(3) 0.1639(2) 0.0491(13) Uani 1 1 d . . . H32A H 0.7727 0.0875 0.1867 0.074 Uiso 1 1 calc R . . H32B H 0.6344 0.1356 0.1718 0.074 Uiso 1 1 calc R . . H32C H 0.6390 0.0779 0.1125 0.074 Uiso 1 1 calc R . . C41 C 0.2550(5) 0.2299(3) 0.2829(2) 0.0397(11) Uani 1 1 d . . . H41A H 0.2457 0.1900 0.2477 0.060 Uiso 1 1 calc R . . H41B H 0.3414 0.2218 0.3257 0.060 Uiso 1 1 calc R . . H41C H 0.2575 0.2803 0.2626 0.060 Uiso 1 1 calc R . . C42 C 0.0029(5) 0.2291(3) 0.2365(2) 0.0478(13) Uani 1 1 d . . . H42A H 0.0046 0.1901 0.2027 0.072 Uiso 1 1 calc R . . H42B H -0.0075 0.2800 0.2147 0.072 Uiso 1 1 calc R . . H42C H -0.0755 0.2193 0.2489 0.072 Uiso 1 1 calc R . . C43 C -0.0883(5) 0.3224(3) 0.3783(3) 0.0479(13) Uani 1 1 d . . . H43A H -0.1637 0.2986 0.3870 0.072 Uiso 1 1 calc R . . H43B H -0.1275 0.3498 0.3327 0.072 Uiso 1 1 calc R . . H43C H -0.0377 0.3585 0.4168 0.072 Uiso 1 1 calc R . . C44 C -0.0163(5) 0.1845(3) 0.3921(3) 0.0422(12) Uani 1 1 d . . . H44A H -0.1030 0.1815 0.3984 0.063 Uiso 1 1 calc R . . H44B H 0.0617 0.1681 0.4361 0.063 Uiso 1 1 calc R . . H44C H -0.0227 0.1510 0.3527 0.063 Uiso 1 1 calc R . . C45 C 0.3319(5) 0.1919(2) 0.4508(2) 0.0382(11) Uani 1 1 d . . . H45A H 0.4261 0.1929 0.4892 0.057 Uiso 1 1 calc R . . H45B H 0.3311 0.1603 0.4114 0.057 Uiso 1 1 calc R . . H45C H 0.2675 0.1701 0.4689 0.057 Uiso 1 1 calc R . . C46 C 0.3575(5) 0.3323(3) 0.4760(2) 0.0439(12) Uani 1 1 d . . . H46A H 0.4468 0.3137 0.5118 0.066 Uiso 1 1 calc R . . H46B H 0.2985 0.3484 0.4996 0.066 Uiso 1 1 calc R . . H46C H 0.3735 0.3760 0.4506 0.066 Uiso 1 1 calc R . . B1 B 0.5877(5) 0.0204(3) 0.3292(3) 0.0296(11) Uani 1 1 d . . . B2 B 0.6153(6) 0.0184(3) 0.1976(3) 0.0367(13) Uani 1 1 d . . . N1 N 0.1349(4) 0.2260(2) 0.30202(18) 0.0356(9) Uani 1 1 d . . . N2 N 0.0062(4) 0.2635(2) 0.3759(2) 0.0418(10) Uani 1 1 d . . . N3 N 0.2881(4) 0.2708(2) 0.42520(18) 0.0347(9) Uani 1 1 d . . . 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 S1 0.0324(7) 0.0315(6) 0.0351(7) 0.0027(5) 0.0163(5) 0.0008(5) F1 0.0331(14) 0.0366(14) 0.0313(14) 0.0008(11) 0.0181(11) -0.0006(11) C1 0.035(3) 0.025(2) 0.029(2) 0.0002(18) 0.012(2) -0.0030(18) C2 0.033(3) 0.036(2) 0.033(2) -0.007(2) 0.013(2) -0.003(2) C3 0.034(3) 0.037(3) 0.053(3) -0.007(2) 0.020(2) -0.002(2) C4 0.027(3) 0.037(3) 0.052(3) 0.002(2) 0.004(2) -0.003(2) C5 0.047(3) 0.045(3) 0.037(3) 0.002(2) -0.001(3) -0.013(2) C6 0.066(4) 0.056(3) 0.028(3) -0.002(2) 0.008(3) -0.018(3) C7 0.060(4) 0.047(3) 0.034(3) 0.001(2) 0.019(3) -0.007(2) C8 0.048(3) 0.028(2) 0.031(3) -0.0004(19) 0.018(2) -0.006(2) C9 0.034(3) 0.023(2) 0.034(3) 0.0009(18) 0.008(2) -0.0052(18) C10 0.042(3) 0.030(2) 0.033(3) 0.0020(19) 0.008(2) -0.006(2) C11 0.023(2) 0.033(2) 0.033(2) -0.0008(19) 0.0121(18) 0.0004(18) C12 0.027(2) 0.036(2) 0.029(2) 0.0021(19) 0.0133(19) 0.0027(19) C13 0.027(2) 0.052(3) 0.029(2) -0.002(2) 0.0119(19) 0.003(2) C14 0.024(2) 0.042(3) 0.037(3) -0.009(2) 0.013(2) 0.0001(19) C15 0.026(2) 0.034(2) 0.039(3) -0.002(2) 0.015(2) -0.0014(18) C16 0.022(2) 0.033(2) 0.030(2) -0.0005(19) 0.0105(18) -0.0005(18) C17 0.038(3) 0.042(3) 0.029(2) 0.003(2) 0.015(2) 0.003(2) C18 0.039(3) 0.058(3) 0.042(3) -0.018(2) 0.013(2) 0.000(2) C19 0.029(2) 0.030(2) 0.037(3) -0.0021(19) 0.017(2) 0.0024(18) C21 0.035(3) 0.030(2) 0.024(2) -0.0005(18) 0.0122(19) -0.0006(19) C22 0.034(3) 0.034(2) 0.030(2) -0.0032(19) 0.0145(19) 0.000(2) C23 0.033(3) 0.044(3) 0.032(2) 0.005(2) 0.013(2) 0.006(2) C24 0.050(3) 0.034(3) 0.028(2) 0.0024(19) 0.020(2) 0.007(2) C25 0.046(3) 0.031(2) 0.023(2) -0.0009(18) 0.016(2) -0.002(2) C26 0.038(3) 0.034(2) 0.025(2) -0.0008(19) 0.0157(19) 0.000(2) C27 0.027(3) 0.043(3) 0.042(3) 0.001(2) 0.013(2) 0.001(2) C28 0.064(3) 0.038(3) 0.045(3) 0.009(2) 0.026(3) 0.008(2) C29 0.044(3) 0.029(2) 0.039(3) -0.004(2) 0.018(2) -0.007(2) C31 0.079(4) 0.062(3) 0.040(3) -0.001(3) 0.032(3) 0.021(3) C32 0.059(3) 0.057(3) 0.038(3) 0.001(2) 0.028(3) -0.006(3) C41 0.044(3) 0.044(3) 0.041(3) -0.001(2) 0.027(2) -0.001(2) C42 0.040(3) 0.056(3) 0.037(3) -0.004(2) 0.006(2) -0.002(2) C43 0.041(3) 0.049(3) 0.056(3) 0.004(2) 0.022(2) 0.010(2) C44 0.036(3) 0.037(3) 0.054(3) 0.005(2) 0.020(2) -0.002(2) C45 0.033(3) 0.044(3) 0.040(3) 0.005(2) 0.018(2) 0.010(2) C46 0.046(3) 0.046(3) 0.040(3) -0.004(2) 0.019(2) -0.009(2) B1 0.034(3) 0.033(3) 0.026(3) 0.004(2) 0.017(2) -0.002(2) B2 0.048(3) 0.037(3) 0.028(3) -0.001(2) 0.019(3) 0.001(2) N1 0.031(2) 0.039(2) 0.033(2) -0.0019(17) 0.0099(16) -0.0010(16) N2 0.040(2) 0.031(2) 0.062(3) 0.0073(19) 0.029(2) 0.0044(17) N3 0.035(2) 0.035(2) 0.029(2) -0.0011(16) 0.0090(16) -0.0035(16) _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 S1 N3 1.616(4) . ? S1 N2 1.616(4) . ? S1 N1 1.678(4) . ? F1 B1 1.600(5) . ? F1 B2 1.606(5) . ? C1 C2 1.372(6) . ? C1 C9 1.438(6) . ? C1 B1 1.611(6) . ? C2 C3 1.409(6) . ? C2 H2A 0.9500 . ? C3 C4 1.350(6) . ? C3 H3A 0.9500 . ? C4 C10 1.419(7) . ? C4 H4A 0.9500 . ? C5 C6 1.359(7) . ? C5 C10 1.417(6) . ? C5 H5A 0.9500 . ? C6 C7 1.386(7) . ? C6 H6A 0.9500 . ? C7 C8 1.394(6) . ? C7 H7A 0.9500 . ? C8 C9 1.444(6) . ? C8 B2 1.608(7) . ? C9 C10 1.423(6) . ? C11 C12 1.418(6) . ? C11 C16 1.419(6) . ? C11 B1 1.633(6) . ? C12 C13 1.397(6) . ? C12 C17 1.504(6) . ? C13 C14 1.401(6) . ? C13 H13A 0.9500 . ? C14 C15 1.377(6) . ? C14 C18 1.510(6) . ? C15 C16 1.395(6) . ? C15 H15A 0.9500 . ? C16 C19 1.512(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.422(6) . ? C21 C26 1.424(6) . ? C21 B1 1.656(6) . ? C22 C23 1.392(6) . ? C22 C27 1.506(6) . ? C23 C24 1.382(6) . ? C23 H23A 0.9500 . ? C24 C25 1.373(6) . ? C24 C28 1.522(6) . ? C25 C26 1.403(6) . ? C25 H25A 0.9500 . ? C26 C29 1.509(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 B2 1.585(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 B2 1.606(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 N1 1.482(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 N1 1.483(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N2 1.449(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N2 1.460(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N3 1.478(5) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N3 1.465(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 N3 S1 N2 114.8(2) . . ? N3 S1 N1 98.80(18) . . ? N2 S1 N1 99.76(19) . . ? B1 F1 B2 125.7(3) . . ? C2 C1 C9 117.4(4) . . ? C2 C1 B1 117.8(4) . . ? C9 C1 B1 124.7(4) . . ? C1 C2 C3 123.2(4) . . ? C1 C2 H2A 118.4 . . ? C3 C2 H2A 118.4 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C10 120.7(4) . . ? C3 C4 H4A 119.7 . . ? C10 C4 H4A 119.7 . . ? C6 C5 C10 120.4(5) . . ? C6 C5 H5A 119.8 . . ? C10 C5 H5A 119.8 . . ? C5 C6 C7 120.1(5) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C8 123.4(5) . . ? C6 C7 H7A 118.3 . . ? C8 C7 H7A 118.3 . . ? C7 C8 C9 116.9(4) . . ? C7 C8 B2 117.3(4) . . ? C9 C8 B2 125.8(4) . . ? C10 C9 C1 119.5(4) . . ? C10 C9 C8 119.3(4) . . ? C1 C9 C8 121.2(4) . . ? C5 C10 C4 120.7(4) . . ? C5 C10 C9 119.8(5) . . ? C4 C10 C9 119.5(4) . . ? C12 C11 C16 116.3(4) . . ? C12 C11 B1 123.4(4) . . ? C16 C11 B1 120.1(4) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 C17 115.7(4) . . ? C11 C12 C17 123.4(4) . . ? C12 C13 C14 122.2(4) . . ? C12 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C15 C14 C13 116.7(4) . . ? C15 C14 C18 122.3(4) . . ? C13 C14 C18 120.9(4) . . ? C14 C15 C16 122.9(4) . . ? C14 C15 H15A 118.6 . . ? C16 C15 H15A 118.6 . . ? C15 C16 C11 120.9(4) . . ? C15 C16 C19 116.0(4) . . ? C11 C16 C19 123.1(4) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 116.1(4) . . ? C22 C21 B1 119.0(3) . . ? C26 C21 B1 124.9(4) . . ? C23 C22 C21 121.1(4) . . ? C23 C22 C27 116.0(4) . . ? C21 C22 C27 122.9(4) . . ? C24 C23 C22 122.5(4) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C25 C24 C23 117.0(4) . . ? C25 C24 C28 120.9(4) . . ? C23 C24 C28 122.1(4) . . ? C24 C25 C26 123.2(4) . . ? C24 C25 H25A 118.4 . . ? C26 C25 H25A 118.4 . . ? C25 C26 C21 120.1(4) . . ? C25 C26 C29 115.3(4) . . ? C21 C26 C29 124.6(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? B2 C31 H31A 109.5 . . ? B2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? B2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? B2 C32 H32A 109.5 . . ? B2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? B2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 C41 H41A 109.5 . . ? N1 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N1 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N1 C42 H42A 109.5 . . ? N1 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N1 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N2 C43 H43A 109.5 . . ? N2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N2 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 H45A 109.5 . . ? N3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C46 H46A 109.5 . . ? N3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N3 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F1 B1 C1 103.9(3) . . ? F1 B1 C11 104.5(3) . . ? C1 B1 C11 110.1(3) . . ? F1 B1 C21 100.7(3) . . ? C1 B1 C21 117.7(3) . . ? C11 B1 C21 117.5(3) . . ? C31 B2 C32 113.9(4) . . ? C31 B2 F1 107.7(4) . . ? C32 B2 F1 102.9(3) . . ? C31 B2 C8 112.7(4) . . ? C32 B2 C8 113.4(4) . . ? F1 B2 C8 105.2(3) . . ? C41 N1 C42 109.9(4) . . ? C41 N1 S1 114.2(3) . . ? C42 N1 S1 111.7(3) . . ? C43 N2 C44 118.6(4) . . ? C43 N2 S1 116.8(3) . . ? C44 N2 S1 124.3(3) . . ? C46 N3 C45 116.0(3) . . ? C46 N3 S1 116.1(3) . . ? C45 N3 S1 123.6(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 1.084 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.137 # Attachment '3-f.cif' data_sadn _database_code_depnum_ccdc_archive 'CCDC 675715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H74 B2 F Hg N3 S' _chemical_formula_weight 1134.51 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.9011(9) _cell_length_b 19.2576(14) _cell_length_c 23.5739(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.015(2) _cell_angle_gamma 90.00 _cell_volume 5382.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7846 _cell_measurement_theta_min 4.509 _cell_measurement_theta_max 44.749 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .014 _exptl_crystal_size_mid .01 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 2.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4838 _exptl_absorpt_correction_T_max 0.6939 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26547 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8402 _reflns_number_gt 7439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0605P)^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 0.608(7) _refine_ls_number_reflns 8402 _refine_ls_number_parameters 638 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _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 0.68294(2) 0.400426(12) 0.270532(17) 0.03260(9) Uani 1 1 d . . . B1 B 0.6946(8) 0.2987(5) 0.3828(4) 0.036(2) Uani 1 1 d . . . B2 B 0.6730(9) 0.3536(6) 0.1291(4) 0.040(2) Uani 1 1 d . . . F1 F 0.6521(4) 0.2853(2) 0.32258(17) 0.0370(10) Uani 1 1 d . . . N1 N 0.2683(7) 0.2324(5) 0.2468(4) 0.0674(14) Uani 1 1 d . . . N2 N 0.2646(8) 0.1259(6) 0.3015(5) 0.0674(14) Uani 1 1 d . . . N3 N 0.0757(7) 0.1640(5) 0.2535(4) 0.0674(14) Uani 1 1 d . . . S1 S 0.1885(2) 0.19587(13) 0.28814(9) 0.0562(7) Uani 1 1 d . . . C1 C 0.8463(12) 0.3982(5) 0.3097(6) 0.036(3) Uani 1 1 d . . . C2 C 0.9096(10) 0.4480(6) 0.2881(5) 0.037(3) Uani 1 1 d . . . H2 H 0.8747 0.4789 0.2605 0.045 Uiso 1 1 calc R . . C3 C 1.0268(10) 0.4563(6) 0.3050(5) 0.055(4) Uani 1 1 d . . . H3 H 1.0684 0.4934 0.2904 0.066 Uiso 1 1 calc R . . C4 C 1.0779(7) 0.4102(6) 0.3425(4) 0.050(2) Uani 1 1 d . . . H4 H 1.1570 0.4131 0.3520 0.060 Uiso 1 1 calc R . . C5 C 1.0706(8) 0.3130(6) 0.4068(4) 0.066(3) Uani 1 1 d . . . H5 H 1.1498 0.3167 0.4156 0.080 Uiso 1 1 calc R . . C6 C 1.0124(8) 0.2632(6) 0.4331(5) 0.069(3) Uani 1 1 d . . . H6 H 1.0511 0.2315 0.4588 0.083 Uiso 1 1 calc R . . C7 C 0.8952(7) 0.2591(5) 0.4219(4) 0.053(2) Uani 1 1 d . . . H7 H 0.8557 0.2246 0.4410 0.063 Uiso 1 1 calc R . . C8 C 0.8336(7) 0.3034(5) 0.3840(3) 0.043(2) Uani 1 1 d . . . C9 C 0.8965(6) 0.3522(5) 0.3537(3) 0.0328(17) Uani 1 1 d . . . C10 C 1.0164(7) 0.3586(5) 0.3673(4) 0.044(2) Uani 1 1 d . . . C11 C 0.6286(8) 0.3712(6) 0.4006(3) 0.0340(19) Uani 1 1 d . . . C12 C 0.6758(9) 0.4286(5) 0.4292(4) 0.040(2) Uani 1 1 d . . . C13 C 0.6151(11) 0.4856(6) 0.4410(5) 0.050(3) Uani 1 1 d . . . H13 H 0.6530 0.5235 0.4601 0.060 Uiso 1 1 calc R . . C14 C 0.5009(11) 0.4906(5) 0.4265(4) 0.055(3) Uani 1 1 d . . . C15 C 0.4466(9) 0.4332(6) 0.4003(4) 0.040(2) Uani 1 1 d . . . H15 H 0.3674 0.4339 0.3905 0.048 Uiso 1 1 calc R . . C16 C 0.5115(9) 0.3737(6) 0.3884(4) 0.037(2) Uani 1 1 d . . . C17 C 0.8022(7) 0.4333(6) 0.4516(4) 0.057(3) Uani 1 1 d . . . H17A H 0.8461 0.4502 0.4212 0.086 Uiso 1 1 calc R . . H17B H 0.8294 0.3871 0.4638 0.086 Uiso 1 1 calc R . . H17C H 0.8108 0.4653 0.4840 0.086 Uiso 1 1 calc R . . C18 C 0.4318(12) 0.5544(6) 0.4382(6) 0.079(4) Uani 1 1 d . . . H18A H 0.4620 0.5948 0.4192 0.119 Uiso 1 1 calc R . . H18B H 0.4356 0.5628 0.4793 0.119 Uiso 1 1 calc R . . H18C H 0.3531 0.5469 0.4235 0.119 Uiso 1 1 calc R . . C19 C 0.4451(9) 0.3144(5) 0.3628(5) 0.047(3) Uani 1 1 d . . . H19A H 0.4690 0.3044 0.3249 0.071 Uiso 1 1 calc R . . H19B H 0.3647 0.3262 0.3596 0.071 Uiso 1 1 calc R . . H19C H 0.4578 0.2733 0.3871 0.071 Uiso 1 1 calc R . . C21 C 0.6583(10) 0.2284(8) 0.4196(5) 0.049(4) Uani 1 1 d . . . C22 C 0.6541(8) 0.1614(5) 0.3948(4) 0.042(2) Uani 1 1 d . . . C23 C 0.6197(7) 0.1046(5) 0.4223(4) 0.041(2) Uani 1 1 d . . . H23 H 0.6202 0.0607 0.4040 0.050 Uiso 1 1 calc R . . C24 C 0.5839(8) 0.1089(6) 0.4763(4) 0.046(2) Uani 1 1 d . . . C25 C 0.5837(8) 0.1714(6) 0.5018(4) 0.038(2) Uani 1 1 d . . . H25 H 0.5573 0.1748 0.5386 0.045 Uiso 1 1 calc R . . C26 C 0.6207(7) 0.2309(5) 0.4761(4) 0.040(2) Uani 1 1 d . . . C27 C 0.6974(9) 0.1505(6) 0.3368(4) 0.060(3) Uani 1 1 d . . . H27A H 0.7355 0.1054 0.3360 0.091 Uiso 1 1 calc R . . H27B H 0.7507 0.1875 0.3295 0.091 Uiso 1 1 calc R . . H27C H 0.6338 0.1515 0.3074 0.091 Uiso 1 1 calc R . . C28 C 0.5464(8) 0.0439(6) 0.5048(4) 0.053(2) Uani 1 1 d . . . H28A H 0.5972 0.0346 0.5390 0.080 Uiso 1 1 calc R . . H28B H 0.5481 0.0047 0.4785 0.080 Uiso 1 1 calc R . . H28C H 0.4694 0.0503 0.5156 0.080 Uiso 1 1 calc R . . C29 C 0.6275(10) 0.2956(6) 0.5129(5) 0.058(3) Uani 1 1 d . . . H29A H 0.6982 0.3201 0.5082 0.087 Uiso 1 1 calc R . . H29B H 0.6250 0.2824 0.5529 0.087 Uiso 1 1 calc R . . H29C H 0.5636 0.3261 0.5014 0.087 Uiso 1 1 calc R . . C31 C 0.5235(10) 0.4229(6) 0.2272(5) 0.031(2) Uani 1 1 d . . . C32 C 0.4545(11) 0.4648(6) 0.2601(6) 0.047(3) Uani 1 1 d . . . H32 H 0.4842 0.4810 0.2965 0.057 Uiso 1 1 calc R . . C33 C 0.3451(10) 0.4824(6) 0.2401(5) 0.049(3) Uani 1 1 d . . . H33 H 0.3004 0.5101 0.2628 0.059 Uiso 1 1 calc R . . C34 C 0.3017(8) 0.4597(5) 0.1874(4) 0.046(2) Uani 1 1 d . . . H34 H 0.2282 0.4739 0.1731 0.056 Uiso 1 1 calc R . . C35 C 0.3128(7) 0.3870(5) 0.1036(4) 0.049(2) Uani 1 1 d . . . H35 H 0.2379 0.4005 0.0912 0.059 Uiso 1 1 calc R . . C36 C 0.3666(7) 0.3404(5) 0.0716(4) 0.050(2) Uani 1 1 d . . . H36 H 0.3288 0.3191 0.0389 0.060 Uiso 1 1 calc R . . C37 C 0.4805(7) 0.3252(5) 0.0888(3) 0.044(2) Uani 1 1 d . . . H37 H 0.5181 0.2919 0.0676 0.052 Uiso 1 1 calc R . . C38 C 0.5411(6) 0.3567(4) 0.1357(3) 0.0343(18) Uani 1 1 d . . . C39 C 0.4783(6) 0.3973(4) 0.1727(3) 0.0317(17) Uani 1 1 d . . . C40 C 0.3642(7) 0.4157(4) 0.1542(4) 0.040(2) Uani 1 1 d . . . C41 C 0.7199(7) 0.2837(5) 0.1066(3) 0.040(2) Uani 1 1 d . . . C42 C 0.7619(7) 0.2792(6) 0.0530(4) 0.040(3) Uani 1 1 d . . . C43 C 0.8004(7) 0.2158(6) 0.0327(4) 0.040(2) Uani 1 1 d . . . H43 H 0.8287 0.2140 -0.0037 0.048 Uiso 1 1 calc R . . C44 C 0.7976(9) 0.1558(7) 0.0651(5) 0.050(3) Uani 1 1 d . . . C45 C 0.7595(7) 0.1602(5) 0.1182(4) 0.046(2) Uani 1 1 d . . . H45 H 0.7600 0.1203 0.1420 0.055 Uiso 1 1 calc R . . C46 C 0.7192(9) 0.2252(7) 0.1377(5) 0.040(3) Uani 1 1 d . . . C47 C 0.7653(7) 0.3404(5) 0.0147(4) 0.048(2) Uani 1 1 d . . . H47A H 0.6912 0.3629 0.0109 0.071 Uiso 1 1 calc R . . H47B H 0.7849 0.3252 -0.0229 0.071 Uiso 1 1 calc R . . H47C H 0.8221 0.3734 0.0307 0.071 Uiso 1 1 calc R . . C48 C 0.8324(10) 0.0875(5) 0.0413(6) 0.066(3) Uani 1 1 d . . . H48A H 0.7718 0.0699 0.0143 0.099 Uiso 1 1 calc R . . H48B H 0.8474 0.0541 0.0724 0.099 Uiso 1 1 calc R . . H48C H 0.9009 0.0940 0.0216 0.099 Uiso 1 1 calc R . . C49 C 0.6767(9) 0.2223(5) 0.1987(4) 0.061(3) Uani 1 1 d . . . H49A H 0.7247 0.2518 0.2245 0.091 Uiso 1 1 calc R . . H49B H 0.6803 0.1743 0.2125 0.091 Uiso 1 1 calc R . . H49C H 0.5987 0.2388 0.1971 0.091 Uiso 1 1 calc R . . C51 C 0.7507(9) 0.4200(7) 0.1332(4) 0.042(2) Uani 1 1 d . . . C52 C 0.7125(10) 0.4863(6) 0.1120(5) 0.046(3) Uani 1 1 d . . . C53 C 0.7896(8) 0.5400(6) 0.1076(4) 0.054(2) Uani 1 1 d . . . H53 H 0.7624 0.5835 0.0932 0.064 Uiso 1 1 calc R . . C54 C 0.9004(11) 0.5334(8) 0.1226(6) 0.071(4) Uani 1 1 d . . . C55 C 0.9385(10) 0.4716(8) 0.1450(5) 0.070(4) Uani 1 1 d . . . H61 H 1.0158 0.4680 0.1585 0.084 Uiso 1 1 calc R . . C56 C 0.8689(10) 0.4124(8) 0.1493(5) 0.049(3) Uani 1 1 d . . . C57 C 0.5903(7) 0.4996(5) 0.0890(4) 0.049(2) Uani 1 1 d . . . H57A H 0.5874 0.5393 0.0628 0.073 Uiso 1 1 calc R . . H57B H 0.5449 0.5098 0.1207 0.073 Uiso 1 1 calc R . . H57C H 0.5602 0.4583 0.0686 0.073 Uiso 1 1 calc R . . C58 C 0.9836(11) 0.5898(7) 0.1158(7) 0.099(5) Uani 1 1 d . . . H58A H 0.9458 0.6290 0.0956 0.149 Uiso 1 1 calc R . . H58B H 1.0439 0.5724 0.0938 0.149 Uiso 1 1 calc R . . H58C H 1.0159 0.6051 0.1534 0.149 Uiso 1 1 calc R . . C59 C 0.9207(10) 0.3479(7) 0.1729(6) 0.067(4) Uani 1 1 d . . . H59A H 0.9495 0.3207 0.1421 0.101 Uiso 1 1 calc R . . H59B H 0.8640 0.3207 0.1909 0.101 Uiso 1 1 calc R . . H59C H 0.9829 0.3594 0.2013 0.101 Uiso 1 1 calc R . . C61 C 0.3180(12) 0.2034(7) 0.2009(6) 0.099(4) Uani 1 1 d . . . H61A H 0.2639 0.2042 0.1670 0.149 Uiso 1 1 calc R . . H61B H 0.3398 0.1553 0.2098 0.149 Uiso 1 1 calc R . . H61C H 0.3850 0.2303 0.1935 0.149 Uiso 1 1 calc R . . C62 C 0.2438(9) 0.3062(6) 0.2413(5) 0.071(3) Uani 1 1 d . . . H62A H 0.3091 0.3303 0.2280 0.107 Uiso 1 1 calc R . . H62B H 0.2278 0.3250 0.2784 0.107 Uiso 1 1 calc R . . H62C H 0.1781 0.3131 0.2139 0.107 Uiso 1 1 calc R . . C63 C 0.3775(12) 0.1364(7) 0.3305(6) 0.088(4) Uani 1 1 d . . . H63A H 0.3734 0.1700 0.3614 0.131 Uiso 1 1 calc R . . H63B H 0.4282 0.1540 0.3032 0.131 Uiso 1 1 calc R . . H63C H 0.4065 0.0921 0.3462 0.131 Uiso 1 1 calc R . . C64 C 0.2028(11) 0.0783(6) 0.3398(5) 0.075(3) Uani 1 1 d . . . H64A H 0.2307 0.0307 0.3366 0.112 Uiso 1 1 calc R . . H64B H 0.1217 0.0796 0.3280 0.112 Uiso 1 1 calc R . . H64C H 0.2159 0.0940 0.3793 0.112 Uiso 1 1 calc R . . C65 C 0.0753(13) 0.1208(7) 0.2024(6) 0.085(4) Uani 1 1 d . . . H65A H 0.0603 0.0724 0.2123 0.128 Uiso 1 1 calc R . . H65B H 0.1489 0.1239 0.1869 0.128 Uiso 1 1 calc R . . H65C H 0.0164 0.1371 0.1739 0.128 Uiso 1 1 calc R . . C66 C -0.0272(11) 0.1834(7) 0.2728(7) 0.100(4) Uani 1 1 d . . . H66A H -0.0789 0.1981 0.2404 0.151 Uiso 1 1 calc R . . H66B H -0.0152 0.2220 0.2998 0.151 Uiso 1 1 calc R . . H66C H -0.0597 0.1439 0.2917 0.151 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 0.02862(13) 0.03589(14) 0.03260(13) 0.0012(2) -0.00119(9) 0.0017(3) B1 0.029(5) 0.044(5) 0.036(5) 0.000(4) 0.003(4) 0.003(4) B2 0.025(6) 0.059(7) 0.035(6) -0.004(5) 0.003(4) 0.000(5) F1 0.037(3) 0.041(3) 0.033(2) -0.0010(19) 0.0029(19) 0.0000(19) N1 0.047(3) 0.071(4) 0.087(4) -0.001(3) 0.022(3) -0.005(3) N2 0.047(3) 0.071(4) 0.087(4) -0.001(3) 0.022(3) -0.005(3) N3 0.047(3) 0.071(4) 0.087(4) -0.001(3) 0.022(3) -0.005(3) S1 0.0516(14) 0.0618(13) 0.0566(19) -0.0095(10) 0.0119(17) -0.0014(13) C1 0.033(6) 0.034(7) 0.040(6) -0.009(4) 0.006(4) -0.004(5) C2 0.045(7) 0.038(6) 0.030(5) 0.011(4) 0.008(5) -0.010(5) C3 0.035(6) 0.077(9) 0.054(7) 0.006(6) 0.001(5) -0.029(6) C4 0.022(4) 0.077(7) 0.051(6) -0.001(5) -0.004(4) -0.009(5) C5 0.025(5) 0.109(9) 0.064(7) 0.022(6) -0.002(4) -0.004(5) C6 0.046(6) 0.094(8) 0.067(7) 0.029(6) 0.003(5) 0.018(6) C7 0.032(5) 0.066(6) 0.060(6) 0.016(5) 0.001(4) 0.008(4) C8 0.030(5) 0.061(6) 0.038(5) 0.007(4) 0.001(4) 0.003(4) C9 0.021(4) 0.044(5) 0.033(4) 0.007(4) 0.004(3) 0.006(4) C10 0.027(5) 0.069(6) 0.036(5) -0.002(4) 0.004(4) 0.004(4) C11 0.031(6) 0.041(6) 0.030(5) 0.004(4) 0.007(4) -0.004(5) C12 0.048(6) 0.039(5) 0.032(5) 0.000(4) 0.007(4) 0.000(5) C13 0.063(8) 0.048(7) 0.040(6) -0.002(5) 0.016(5) -0.026(6) C14 0.090(9) 0.036(6) 0.040(6) 0.002(4) 0.010(6) 0.006(6) C15 0.027(6) 0.053(6) 0.039(5) 0.013(5) 0.002(5) 0.004(5) C16 0.034(7) 0.047(6) 0.030(5) -0.002(5) 0.006(4) 0.005(5) C17 0.040(5) 0.083(7) 0.050(6) -0.018(5) 0.013(4) -0.022(5) C18 0.090(11) 0.055(8) 0.093(10) -0.009(7) 0.009(8) 0.028(7) C19 0.023(5) 0.055(7) 0.064(7) 0.003(5) 0.000(4) 0.009(5) C21 0.033(6) 0.077(9) 0.038(7) 0.033(6) 0.003(5) 0.004(5) C22 0.032(5) 0.051(6) 0.042(5) -0.001(4) -0.001(4) 0.013(4) C23 0.041(5) 0.046(5) 0.037(5) 0.000(4) 0.000(4) 0.004(4) C24 0.020(5) 0.069(8) 0.046(6) 0.015(5) -0.006(4) -0.004(5) C25 0.023(5) 0.059(7) 0.033(6) 0.013(5) 0.013(4) 0.007(5) C26 0.021(4) 0.059(6) 0.040(5) -0.001(4) -0.003(4) 0.011(4) C27 0.068(7) 0.068(7) 0.046(6) -0.003(5) 0.012(5) 0.003(5) C28 0.040(6) 0.060(6) 0.059(6) 0.012(5) 0.004(5) -0.012(5) C29 0.060(8) 0.066(8) 0.051(7) 0.014(6) 0.019(6) 0.013(6) C31 0.031(5) 0.029(5) 0.033(6) 0.003(5) -0.001(4) 0.001(5) C32 0.042(7) 0.045(6) 0.055(7) -0.010(5) 0.005(5) 0.014(5) C33 0.037(6) 0.062(7) 0.050(6) -0.011(5) 0.007(5) 0.012(5) C34 0.034(5) 0.047(5) 0.058(6) -0.001(5) 0.002(4) 0.014(4) C35 0.019(4) 0.075(6) 0.051(6) 0.011(5) -0.005(4) 0.000(4) C36 0.026(5) 0.085(7) 0.039(5) -0.017(5) -0.003(4) 0.000(4) C37 0.028(4) 0.067(6) 0.036(5) -0.014(4) 0.003(4) -0.004(4) C38 0.035(5) 0.037(5) 0.031(4) 0.006(3) 0.006(3) 0.004(4) C39 0.025(4) 0.035(4) 0.036(4) 0.008(4) 0.005(3) -0.003(4) C40 0.038(5) 0.051(5) 0.033(5) 0.002(4) 0.010(4) 0.005(4) C41 0.030(5) 0.055(6) 0.036(5) 0.001(4) 0.005(4) 0.003(4) C42 0.019(5) 0.067(7) 0.033(6) -0.011(5) 0.005(4) 0.002(4) C43 0.021(5) 0.062(6) 0.036(5) -0.007(4) 0.011(4) -0.001(4) C44 0.036(6) 0.057(7) 0.057(8) -0.004(6) 0.009(5) 0.002(5) C45 0.030(5) 0.062(7) 0.046(6) 0.019(5) 0.004(4) 0.001(4) C46 0.019(5) 0.065(8) 0.036(6) -0.014(5) 0.002(4) -0.006(4) C47 0.035(5) 0.054(6) 0.053(6) -0.009(5) 0.001(4) -0.002(4) C48 0.054(7) 0.039(6) 0.104(10) -0.008(6) 0.009(7) -0.003(5) C49 0.067(7) 0.075(7) 0.043(5) 0.002(5) 0.018(5) 0.000(5) C51 0.042(7) 0.062(7) 0.024(5) -0.010(5) 0.006(4) -0.003(6) C52 0.048(7) 0.057(7) 0.034(6) -0.015(4) 0.012(5) 0.004(5) C53 0.049(6) 0.061(7) 0.054(6) -0.015(5) 0.023(5) -0.009(5) C54 0.072(9) 0.070(10) 0.078(9) -0.036(8) 0.044(7) -0.026(8) C55 0.050(7) 0.094(11) 0.068(8) -0.049(8) 0.026(6) -0.027(8) C56 0.013(6) 0.079(10) 0.053(7) -0.023(6) -0.003(5) 0.001(6) C57 0.049(6) 0.053(6) 0.045(5) 0.005(4) 0.014(4) 0.001(4) C58 0.061(8) 0.117(12) 0.128(12) -0.035(9) 0.053(8) -0.043(8) C59 0.029(6) 0.094(11) 0.077(9) -0.028(8) -0.012(6) -0.010(7) C61 0.105(11) 0.098(9) 0.099(10) -0.021(8) 0.039(8) -0.022(8) C62 0.062(7) 0.068(7) 0.088(8) 0.005(6) 0.030(6) 0.003(6) C63 0.084(10) 0.082(9) 0.094(10) 0.012(7) -0.011(8) -0.007(7) C64 0.083(9) 0.065(7) 0.077(8) 0.001(6) 0.009(6) -0.015(6) C65 0.089(11) 0.087(9) 0.085(10) -0.011(7) 0.032(8) -0.009(8) C66 0.072(8) 0.100(10) 0.132(12) -0.026(9) 0.026(8) 0.000(7) _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 2.079(14) . ? Hg1 C31 2.119(12) . ? Hg1 F1 2.576(4) . ? Hg1 B1 3.286(9) . ? Hg1 B2 3.445(10) . ? B1 F1 1.487(10) . ? B1 C11 1.672(14) . ? B1 C8 1.655(12) . ? B1 C21 1.685(16) . ? B2 C41 1.567(14) . ? B2 C38 1.592(13) . ? B2 C51 1.576(16) . ? N1 C61 1.395(14) . ? N1 C62 1.455(14) . ? N1 S1 1.583(9) . ? N2 C63 1.467(16) . ? N2 C64 1.520(16) . ? N2 S1 1.638(11) . ? N3 C66 1.394(15) . ? N3 C65 1.464(15) . ? N3 S1 1.629(9) . ? C1 C2 1.347(15) . ? C1 C9 1.451(15) . ? C2 C3 1.426(16) . ? C2 H2 0.9500 . ? C3 C4 1.359(15) . ? C3 H3 0.9500 . ? C4 C10 1.392(13) . ? C4 H4 0.9500 . ? C5 C6 1.363(15) . ? C5 C10 1.397(13) . ? C5 H5 0.9500 . ? C6 C7 1.399(13) . ? C6 H6 0.9500 . ? C7 C8 1.396(12) . ? C7 H7 0.9500 . ? C8 C9 1.432(11) . ? C9 C10 1.441(11) . ? C11 C16 1.399(15) . ? C11 C12 1.389(14) . ? C12 C13 1.356(16) . ? C12 C17 1.553(13) . ? C13 C14 1.376(17) . ? C13 H13 0.9500 . ? C14 C15 1.398(15) . ? C14 C18 1.517(15) . ? C15 C16 1.424(15) . ? C15 H15 0.9500 . ? C16 C19 1.486(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.415(17) . ? C21 C26 1.442(15) . ? C22 C23 1.352(13) . ? C22 C27 1.517(14) . ? C23 C24 1.380(13) . ? C23 H23 0.9500 . ? C24 C25 1.346(15) . ? C24 C28 1.506(14) . ? C25 C26 1.387(14) . ? C25 H25 0.9500 . ? C26 C29 1.516(14) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C32 1.427(17) . ? C31 C39 1.437(14) . ? C32 C33 1.388(17) . ? C32 H32 0.9500 . ? C33 C34 1.374(15) . ? C33 H33 0.9500 . ? C34 C40 1.409(12) . ? C34 H34 0.9500 . ? C35 C36 1.369(13) . ? C35 C40 1.405(13) . ? C35 H35 0.9500 . ? C36 C37 1.411(12) . ? C36 H36 0.9500 . ? C37 C38 1.403(11) . ? C37 H37 0.9500 . ? C38 C39 1.430(11) . ? C39 C40 1.433(12) . ? C41 C46 1.344(16) . ? C41 C42 1.401(13) . ? C42 C43 1.403(14) . ? C42 C47 1.489(14) . ? C43 C44 1.387(15) . ? C43 H43 0.9500 . ? C44 C45 1.371(15) . ? C44 C48 1.502(15) . ? C45 C46 1.431(17) . ? C45 H45 0.9500 . ? C46 C49 1.566(14) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.431(18) . ? C51 C56 1.431(16) . ? C52 C53 1.393(16) . ? C52 C57 1.529(14) . ? C53 C54 1.341(17) . ? C53 H53 0.9500 . ? C54 C55 1.36(2) . ? C54 C58 1.487(16) . ? C55 C56 1.419(18) . ? C55 H61 0.9500 . ? C56 C59 1.474(18) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? 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 C31 169.0(4) . . ? C1 Hg1 F1 86.4(3) . . ? C31 Hg1 F1 104.3(3) . . ? C1 Hg1 B1 70.0(4) . . ? C31 Hg1 B1 118.8(3) . . ? F1 Hg1 B1 25.96(19) . . ? C1 Hg1 B2 112.1(4) . . ? C31 Hg1 B2 68.5(4) . . ? F1 Hg1 B2 104.0(2) . . ? B1 Hg1 B2 128.2(3) . . ? F1 B1 C11 104.8(6) . . ? F1 B1 C8 106.4(6) . . ? C11 B1 C8 116.1(7) . . ? F1 B1 C21 105.7(7) . . ? C11 B1 C21 113.2(8) . . ? C8 B1 C21 109.6(7) . . ? F1 B1 Hg1 49.3(3) . . ? C11 B1 Hg1 73.5(4) . . ? C8 B1 Hg1 87.3(4) . . ? C21 B1 Hg1 154.1(6) . . ? C41 B2 C38 116.6(9) . . ? C41 B2 C51 119.5(9) . . ? C38 B2 C51 122.9(8) . . ? C41 B2 Hg1 124.7(6) . . ? C38 B2 Hg1 81.2(5) . . ? C51 B2 Hg1 76.0(5) . . ? B1 F1 Hg1 104.7(4) . . ? C61 N1 C62 114.7(10) . . ? C61 N1 S1 128.1(8) . . ? C62 N1 S1 111.3(7) . . ? C63 N2 C64 106.2(11) . . ? C63 N2 S1 116.4(8) . . ? C64 N2 S1 108.8(8) . . ? C66 N3 C65 118.7(11) . . ? C66 N3 S1 116.4(9) . . ? C65 N3 S1 124.7(9) . . ? N1 S1 N3 111.8(5) . . ? N1 S1 N2 97.7(5) . . ? N3 S1 N2 101.8(5) . . ? C2 C1 C9 119.8(12) . . ? C2 C1 Hg1 110.4(10) . . ? C9 C1 Hg1 129.8(8) . . ? C1 C2 C3 122.6(12) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C4 C3 C2 118.7(10) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C10 121.2(9) . . ? C3 C4 H4 119.4 . . ? C10 C4 H4 119.4 . . ? C6 C5 C10 121.4(9) . . ? C6 C5 H5 119.3 . . ? C10 C5 H5 119.3 . . ? C5 C6 C7 119.5(9) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 123.1(9) . . ? C8 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C7 C8 C9 116.9(7) . . ? C7 C8 B1 116.5(7) . . ? C9 C8 B1 126.3(7) . . ? C8 C9 C1 123.9(8) . . ? C8 C9 C10 119.7(7) . . ? C1 C9 C10 116.4(8) . . ? C5 C10 C4 119.9(8) . . ? C5 C10 C9 119.1(8) . . ? C4 C10 C9 121.0(8) . . ? C16 C11 C12 115.2(10) . . ? C16 C11 B1 117.3(8) . . ? C12 C11 B1 127.4(9) . . ? C13 C12 C11 123.0(11) . . ? C13 C12 C17 113.6(9) . . ? C11 C12 C17 123.4(9) . . ? C12 C13 C14 122.6(11) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C15 117.6(10) . . ? C13 C14 C18 123.5(11) . . ? C15 C14 C18 118.9(12) . . ? C14 C15 C16 119.1(11) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C11 C16 C15 122.3(10) . . ? C11 C16 C19 122.8(9) . . ? C15 C16 C19 114.9(9) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C26 114.2(11) . . ? C22 C21 B1 121.4(10) . . ? C26 C21 B1 124.2(12) . . ? C23 C22 C21 122.7(10) . . ? C23 C22 C27 117.4(8) . . ? C21 C22 C27 119.7(9) . . ? C22 C23 C24 121.7(10) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 118.6(10) . . ? C25 C24 C28 122.1(10) . . ? C23 C24 C28 119.4(10) . . ? C24 C25 C26 122.1(10) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C21 120.7(11) . . ? C25 C26 C29 115.6(9) . . ? C21 C26 C29 123.5(10) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C39 119.5(11) . . ? C32 C31 Hg1 112.8(9) . . ? C39 C31 Hg1 127.6(8) . . ? C31 C32 C33 121.4(13) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.8(11) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C40 121.2(9) . . ? C33 C34 H34 119.4 . . ? C40 C34 H34 119.4 . . ? C36 C35 C40 122.5(8) . . ? C36 C35 H35 118.8 . . ? C40 C35 H35 118.8 . . ? C35 C36 C37 117.4(8) . . ? C35 C36 H36 121.3 . . ? C37 C36 H36 121.3 . . ? C38 C37 C36 123.6(8) . . ? C38 C37 H37 118.2 . . ? C36 C37 H37 118.2 . . ? C37 C38 C39 117.1(7) . . ? C37 C38 B2 110.5(7) . . ? C39 C38 B2 130.7(8) . . ? C38 C39 C40 118.8(7) . . ? C38 C39 C31 123.9(8) . . ? C40 C39 C31 117.2(8) . . ? C35 C40 C34 119.7(8) . . ? C35 C40 C39 119.4(7) . . ? C34 C40 C39 120.8(8) . . ? C46 C41 C42 117.3(9) . . ? C46 C41 B2 121.0(8) . . ? C42 C41 B2 121.7(9) . . ? C41 C42 C43 121.0(10) . . ? C41 C42 C47 122.0(9) . . ? C43 C42 C47 117.0(9) . . ? C44 C43 C42 120.8(9) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 118.5(10) . . ? C43 C44 C48 120.2(11) . . ? C45 C44 C48 121.3(11) . . ? C44 C45 C46 119.6(10) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C41 C46 C45 122.7(10) . . ? C41 C46 C49 123.3(10) . . ? C45 C46 C49 114.0(10) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 C56 117.3(11) . . ? C52 C51 B2 122.4(10) . . ? C56 C51 B2 119.4(11) . . ? C53 C52 C51 119.8(10) . . ? C53 C52 C57 117.5(10) . . ? C51 C52 C57 122.5(10) . . ? C54 C53 C52 123.3(12) . . ? C54 C53 H53 118.3 . . ? C52 C53 H53 118.3 . . ? C53 C54 C55 118.0(12) . . ? C53 C54 C58 123.4(15) . . ? C55 C54 C58 118.5(14) . . ? C54 C55 C56 123.6(13) . . ? C54 C55 H61 118.2 . . ? C56 C55 H61 118.2 . . ? C55 C56 C51 117.7(13) . . ? C55 C56 C59 118.5(12) . . ? C51 C56 C59 123.7(13) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N1 C61 H61A 109.5 . . ? N1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N1 C62 H62A 109.5 . . ? N1 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N1 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N2 C63 H63A 109.5 . . ? N2 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N2 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N2 C64 H64A 109.5 . . ? N2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N3 C65 H65A 109.5 . . ? N3 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N3 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N3 C66 H66A 109.5 . . ? N3 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N3 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.705 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.106 # Attachment '3.cif' data_sol _database_code_depnum_ccdc_archive 'CCDC 675716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56.50 H56.50 B2 Cl1.50 Hg' _chemical_formula_weight 1010.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 12.1981(19) _cell_length_b 27.747(4) _cell_length_c 14.241(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.204(7) _cell_angle_gamma 90.00 _cell_volume 4770.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 740 _cell_measurement_theta_min 7.983 _cell_measurement_theta_max 96.803 _exptl_crystal_description 'plate ' _exptl_crystal_colour 'colorless ' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 6.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5487 _exptl_absorpt_correction_T_max 0.9349 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MWPC area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31362 _diffrn_reflns_av_R_equivalents 0.1001 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 59.99 _reflns_number_total 6768 _reflns_number_gt 4409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. Half a disordered molecule of chloroform, disordered over four positions, was found in the asymmetric unit. Each of the four components was restrained to an idealized geometry and refined to convergence. ; _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^)+(0.1117P)^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 6768 _refine_ls_number_parameters 582 _refine_ls_number_restraints 628 _refine_ls_R_factor_all 0.1167 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.008 _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 -0.24061(4) 0.383929(17) -0.46008(3) 0.02493(18) Uani 1 1 d U . . B1 B -0.0145(12) 0.3264(5) -0.3339(10) 0.0274(14) Uani 1 1 d U . . C1 C -0.2281(10) 0.3950(5) -0.3077(8) 0.0287(17) Uani 1 1 d U . . C2 C -0.2991(10) 0.4312(5) -0.2972(9) 0.0330(18) Uani 1 1 d U . . H2 H -0.3399 0.4459 -0.3514 0.040 Uiso 1 1 calc R . . B2 B -0.4705(11) 0.3264(5) -0.5822(10) 0.0257(14) Uani 1 1 d U . . C3 C -0.3128(11) 0.4474(5) -0.2037(9) 0.0366(19) Uani 1 1 d U . . H3 H -0.3601 0.4736 -0.1941 0.044 Uiso 1 1 calc R . . C4 C -0.2522(10) 0.4224(5) -0.1268(9) 0.0341(18) Uani 1 1 d U . . H4 H -0.2632 0.4303 -0.0639 0.041 Uiso 1 1 calc R . . C5 C -0.1142(10) 0.3636(5) -0.0602(9) 0.0321(18) Uani 1 1 d U . . H5 H -0.1261 0.3730 0.0016 0.039 Uiso 1 1 calc R . . C6 C -0.0376(11) 0.3286(5) -0.0700(9) 0.0330(18) Uani 1 1 d U . . H6 H 0.0026 0.3134 -0.0160 0.040 Uiso 1 1 calc R . . C7 C -0.0200(11) 0.3157(5) -0.1629(9) 0.0309(17) Uani 1 1 d U . . H7 H 0.0323 0.2912 -0.1705 0.037 Uiso 1 1 calc R . . C8 C -0.0753(10) 0.3374(5) -0.2425(8) 0.0282(15) Uani 1 1 d U . . C9 C -0.1586(10) 0.3719(4) -0.2333(8) 0.0276(15) Uani 1 1 d U . . C10 C -0.1766(10) 0.3863(5) -0.1406(8) 0.0285(15) Uani 1 1 d U . . C11 C 0.0356(10) 0.2714(5) -0.3357(8) 0.0277(14) Uani 1 1 d U . . C12 C 0.1523(10) 0.2663(5) -0.3320(8) 0.0298(16) Uani 1 1 d U . . C13 C 0.1950(11) 0.2206(5) -0.3320(9) 0.0330(17) Uani 1 1 d U . . H13 H 0.2719 0.2165 -0.3342 0.040 Uiso 1 1 calc R . . C14 C 0.1276(11) 0.1794(5) -0.3287(9) 0.0343(17) Uani 1 1 d U . . C15 C 0.0172(11) 0.1852(5) -0.3256(8) 0.0315(17) Uani 1 1 d U . . H15 H -0.0284 0.1579 -0.3203 0.038 Uiso 1 1 calc R . . C16 C -0.0293(10) 0.2319(5) -0.3304(8) 0.0284(16) Uani 1 1 d U . . C17 C 0.2291(10) 0.3088(5) -0.3269(10) 0.036(3) Uani 1 1 d U . . H17A H 0.3060 0.2976 -0.3148 0.054 Uiso 1 1 calc R . . H17B H 0.2144 0.3302 -0.2753 0.054 Uiso 1 1 calc R . . H17C H 0.2169 0.3264 -0.3872 0.054 Uiso 1 1 calc R . . C18 C 0.1812(13) 0.1293(5) -0.3308(11) 0.046(3) Uani 1 1 d U . . H18A H 0.1981 0.1226 -0.3948 0.070 Uiso 1 1 calc R . . H18B H 0.1299 0.1048 -0.3133 0.070 Uiso 1 1 calc R . . H18C H 0.2498 0.1284 -0.2856 0.070 Uiso 1 1 calc R . . C19 C -0.1539(10) 0.2344(5) -0.3295(9) 0.033(2) Uani 1 1 d U . . H19A H -0.1879 0.2542 -0.3828 0.049 Uiso 1 1 calc R . . H19B H -0.1686 0.2488 -0.2698 0.049 Uiso 1 1 calc R . . H19C H -0.1851 0.2018 -0.3355 0.049 Uiso 1 1 calc R . . C21 C 0.0157(9) 0.3640(4) -0.4062(8) 0.0264(14) Uani 1 1 d U . . C22 C 0.0182(9) 0.3505(5) -0.5023(8) 0.0265(15) Uani 1 1 d U . . C23 C 0.0619(9) 0.3814(5) -0.5640(8) 0.0268(16) Uani 1 1 d U . . H23 H 0.0643 0.3715 -0.6275 0.032 Uiso 1 1 calc R . . C24 C 0.1024(9) 0.4271(5) -0.5345(9) 0.0282(16) Uani 1 1 d U . . C25 C 0.0969(9) 0.4404(5) -0.4427(9) 0.0276(16) Uani 1 1 d U . . H25 H 0.1224 0.4715 -0.4224 0.033 Uiso 1 1 calc R . . C26 C 0.0554(9) 0.4101(5) -0.3777(8) 0.0256(16) Uani 1 1 d U . . C27 C -0.0273(11) 0.3037(5) -0.5443(9) 0.031(2) Uani 1 1 d U . . H27A H 0.0220 0.2773 -0.5201 0.046 Uiso 1 1 calc R . . H27B H -0.0324 0.3052 -0.6136 0.046 Uiso 1 1 calc R . . H27C H -0.1011 0.2983 -0.5268 0.046 Uiso 1 1 calc R . . C28 C 0.1479(11) 0.4616(5) -0.6030(10) 0.037(3) Uani 1 1 d U . . H28A H 0.0866 0.4743 -0.6482 0.055 Uiso 1 1 calc R . . H28B H 0.1999 0.4444 -0.6374 0.055 Uiso 1 1 calc R . . H28C H 0.1863 0.4883 -0.5672 0.055 Uiso 1 1 calc R . . C29 C 0.0630(10) 0.4277(5) -0.2766(9) 0.030(2) Uani 1 1 d U . . H29A H -0.0093 0.4400 -0.2653 0.045 Uiso 1 1 calc R . . H29B H 0.1182 0.4535 -0.2658 0.045 Uiso 1 1 calc R . . H29C H 0.0851 0.4009 -0.2330 0.045 Uiso 1 1 calc R . . C31 C -0.2563(7) 0.3898(4) -0.6041(7) 0.0177(14) Uani 1 1 d DU . . C32 C -0.1803(9) 0.4220(4) -0.6283(9) 0.0258(16) Uani 1 1 d DU . . H32 H -0.1359 0.4371 -0.5762 0.031 Uiso 1 1 calc R . . C33 C -0.1570(10) 0.4364(4) -0.7198(9) 0.0300(17) Uani 1 1 d U . . H33 H -0.0992 0.4584 -0.7276 0.036 Uiso 1 1 calc R . . C34 C -0.2239(10) 0.4165(5) -0.7959(9) 0.0308(18) Uani 1 1 d U . . H34 H -0.2164 0.4258 -0.8588 0.037 Uiso 1 1 calc R . . C35 C -0.3740(11) 0.3612(5) -0.8568(9) 0.0331(18) Uani 1 1 d U . . H35 H -0.3643 0.3704 -0.9193 0.040 Uiso 1 1 calc R . . C36 C -0.4518(11) 0.3298(5) -0.8443(9) 0.0329(18) Uani 1 1 d U . . H36 H -0.4929 0.3147 -0.8979 0.040 Uiso 1 1 calc R . . C37 C -0.4750(10) 0.3184(4) -0.7535(8) 0.0291(17) Uani 1 1 d U . . H37 H -0.5339 0.2968 -0.7471 0.035 Uiso 1 1 calc R . . C38 C -0.4134(9) 0.3381(4) -0.6718(8) 0.0247(14) Uani 1 1 d U . . C39 C -0.3223(9) 0.3716(4) -0.6803(8) 0.0237(14) Uani 1 1 d DU . . C40 C -0.3052(10) 0.3814(5) -0.7790(9) 0.0316(15) Uani 1 1 d U . . C41 C -0.4958(9) 0.3653(4) -0.5048(8) 0.0263(14) Uani 1 1 d U . . C42 C -0.4973(9) 0.3510(5) -0.4090(8) 0.0262(15) Uani 1 1 d U . . C43 C -0.5388(9) 0.3827(5) -0.3468(8) 0.0279(16) Uani 1 1 d U . . H43 H -0.5380 0.3734 -0.2825 0.034 Uiso 1 1 calc R . . C44 C -0.5810(10) 0.4270(5) -0.3759(9) 0.0291(16) Uani 1 1 d U . . C45 C -0.5770(10) 0.4408(5) -0.4671(9) 0.0294(17) Uani 1 1 d U . . H45 H -0.6039 0.4718 -0.4875 0.035 Uiso 1 1 calc R . . C46 C -0.5343(10) 0.4107(5) -0.5314(9) 0.0274(16) Uani 1 1 d U . . C47 C -0.4469(11) 0.3033(4) -0.3711(9) 0.031(2) Uani 1 1 d U . . H47A H -0.5039 0.2782 -0.3789 0.047 Uiso 1 1 calc R . . H47B H -0.4178 0.3067 -0.3037 0.047 Uiso 1 1 calc R . . H47C H -0.3866 0.2943 -0.4063 0.047 Uiso 1 1 calc R . . C48 C -0.6266(10) 0.4609(5) -0.3068(10) 0.038(3) Uani 1 1 d U . . H48A H -0.6528 0.4906 -0.3398 0.057 Uiso 1 1 calc R . . H48B H -0.5681 0.4686 -0.2544 0.057 Uiso 1 1 calc R . . H48C H -0.6884 0.4452 -0.2817 0.057 Uiso 1 1 calc R . . C49 C -0.5413(11) 0.4319(5) -0.6324(9) 0.032(2) Uani 1 1 d U . . H49A H -0.5695 0.4073 -0.6790 0.048 Uiso 1 1 calc R . . H49B H -0.4675 0.4421 -0.6437 0.048 Uiso 1 1 calc R . . H49C H -0.5915 0.4596 -0.6385 0.048 Uiso 1 1 calc R . . C51 C -0.5155(10) 0.2739(5) -0.5800(9) 0.0293(14) Uani 1 1 d U . . C52 C -0.6313(10) 0.2659(5) -0.5775(9) 0.0327(16) Uani 1 1 d U . . C53 C -0.6719(11) 0.2203(5) -0.5783(9) 0.0354(18) Uani 1 1 d U . . H53 H -0.7485 0.2158 -0.5753 0.042 Uiso 1 1 calc R . . C54 C -0.6048(11) 0.1796(5) -0.5835(9) 0.0377(18) Uani 1 1 d U . . C55 C -0.4922(11) 0.1877(5) -0.5894(9) 0.0347(17) Uani 1 1 d U . . H55 H -0.4468 0.1605 -0.5969 0.042 Uiso 1 1 calc R . . C56 C -0.4447(11) 0.2319(5) -0.5851(9) 0.0314(16) Uani 1 1 d U . . C57 C -0.7105(10) 0.3064(5) -0.5789(10) 0.039(3) Uani 1 1 d U . . H57A H -0.7859 0.2937 -0.5821 0.059 Uiso 1 1 calc R . . H57B H -0.7058 0.3267 -0.6345 0.059 Uiso 1 1 calc R . . H57C H -0.6924 0.3256 -0.5211 0.059 Uiso 1 1 calc R . . C58 C -0.6499(14) 0.1292(5) -0.5828(11) 0.052(3) Uani 1 1 d U . . H58A H -0.7272 0.1290 -0.6133 0.078 Uiso 1 1 calc R . . H58B H -0.6459 0.1180 -0.5171 0.078 Uiso 1 1 calc R . . H58C H -0.6059 0.1078 -0.6175 0.078 Uiso 1 1 calc R . . C59 C -0.3228(10) 0.2379(5) -0.5883(10) 0.037(3) Uani 1 1 d U . . H59A H -0.2882 0.2061 -0.5899 0.056 Uiso 1 1 calc R . . H59B H -0.2889 0.2555 -0.5318 0.056 Uiso 1 1 calc R . . H59C H -0.3119 0.2561 -0.6453 0.056 Uiso 1 1 calc R . . C1_1 C 0.0121(7) 0.4649(3) -0.0487(5) 0.0232(15) Uani 0.25 1 d PDU A -1 H1B_1 H -0.0228 0.4349 -0.0783 0.028 Uiso 0.25 1 calc PR A -1 Cl1_1 Cl -0.0210(8) 0.5226(4) -0.0992(5) 0.0232(15) Uani 0.25 1 d PDU A -1 Cl2_1 Cl 0.1581(6) 0.4736(4) -0.0336(6) 0.0232(15) Uani 0.25 1 d PDU A -1 Cl3_1 Cl -0.0039(7) 0.4819(4) 0.0691(5) 0.0232(15) Uani 0.25 1 d PDU A -1 C1_2 C 0.4735(9) 0.4765(4) -0.0599(7) 0.051(2) Uani 0.25 1 d PDU B -3 H1C_2 H 0.4879 0.4493 -0.1026 0.061 Uiso 0.25 1 calc PR B -3 Cl1_2 Cl 0.3375(7) 0.4896(5) -0.0355(10) 0.051(2) Uani 0.25 1 d PDU B -3 Cl2_2 Cl 0.5368(9) 0.4787(5) 0.0606(8) 0.051(2) Uani 0.25 1 d PDU B -3 Cl3_2 Cl 0.5061(11) 0.5371(4) -0.0863(9) 0.051(2) Uani 0.25 1 d PDU B -3 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 0.0226(3) 0.0317(3) 0.0199(3) 0.0004(3) 0.00074(16) 0.0008(3) B1 0.026(3) 0.035(3) 0.021(3) -0.001(3) 0.001(3) -0.002(3) C1 0.029(4) 0.038(4) 0.020(2) -0.005(3) 0.005(3) -0.007(3) C2 0.031(4) 0.043(4) 0.026(3) -0.005(3) 0.005(3) -0.003(3) B2 0.022(3) 0.034(3) 0.021(3) -0.001(3) 0.004(3) 0.000(3) C3 0.034(4) 0.049(4) 0.027(4) -0.007(3) 0.007(3) -0.003(3) C4 0.033(4) 0.048(4) 0.022(3) -0.008(3) 0.007(3) -0.006(3) C5 0.036(4) 0.044(4) 0.016(3) -0.004(3) 0.003(3) -0.009(3) C6 0.036(4) 0.044(4) 0.018(3) 0.000(3) -0.001(3) -0.007(3) C7 0.033(4) 0.040(4) 0.019(3) -0.002(3) 0.001(3) -0.006(3) C8 0.029(3) 0.036(3) 0.019(3) -0.002(3) 0.002(3) -0.006(3) C9 0.028(3) 0.037(4) 0.018(2) -0.003(3) 0.003(3) -0.009(3) C10 0.029(3) 0.041(4) 0.016(3) -0.004(3) 0.004(3) -0.010(3) C11 0.029(3) 0.036(3) 0.018(3) 0.001(3) 0.001(3) 0.000(2) C12 0.030(3) 0.038(3) 0.020(4) 0.003(3) -0.001(3) 0.003(3) C13 0.035(4) 0.039(3) 0.023(4) -0.001(4) -0.001(3) 0.006(3) C14 0.040(4) 0.037(3) 0.023(4) -0.004(3) -0.002(3) 0.005(3) C15 0.040(3) 0.035(3) 0.019(4) -0.002(3) 0.001(3) 0.001(3) C16 0.034(3) 0.034(3) 0.016(3) 0.000(3) 0.001(3) 0.000(3) C17 0.029(5) 0.045(5) 0.033(6) 0.012(5) -0.003(5) 0.000(4) C18 0.054(6) 0.039(4) 0.042(6) -0.009(5) -0.012(6) 0.011(4) C19 0.035(4) 0.035(6) 0.027(6) -0.003(5) 0.002(5) -0.006(4) C21 0.022(3) 0.034(3) 0.023(3) 0.001(2) 0.002(3) 0.001(3) C22 0.021(3) 0.034(3) 0.023(3) 0.002(3) 0.000(3) 0.001(3) C23 0.021(3) 0.034(3) 0.025(3) 0.004(3) 0.003(3) 0.006(3) C24 0.021(4) 0.035(3) 0.029(3) 0.006(3) 0.005(3) 0.004(3) C25 0.022(4) 0.032(4) 0.029(3) 0.003(3) 0.002(3) 0.003(3) C26 0.019(3) 0.033(3) 0.026(3) 0.001(3) 0.003(3) 0.003(3) C27 0.036(6) 0.036(5) 0.020(5) 0.001(4) 0.007(5) -0.003(4) C28 0.034(6) 0.040(6) 0.037(5) 0.010(5) 0.007(5) 0.000(5) C29 0.029(5) 0.033(6) 0.027(4) 0.002(4) 0.003(5) -0.004(5) C31 0.0176(17) 0.0169(17) 0.0187(16) 0.0007(10) 0.0030(10) 0.0024(10) C32 0.025(3) 0.027(3) 0.027(3) 0.003(3) 0.008(3) 0.005(3) C33 0.029(4) 0.034(4) 0.029(3) 0.003(3) 0.012(3) 0.004(3) C34 0.030(4) 0.039(4) 0.025(3) 0.003(3) 0.013(3) 0.004(3) C35 0.038(4) 0.040(4) 0.022(3) 0.002(3) 0.006(3) 0.003(3) C36 0.039(4) 0.037(4) 0.022(3) 0.000(3) 0.004(3) 0.001(3) C37 0.033(4) 0.033(4) 0.021(3) -0.002(3) 0.005(3) 0.002(3) C38 0.022(3) 0.031(3) 0.021(3) 0.000(3) 0.003(2) 0.002(2) C39 0.022(3) 0.028(3) 0.022(2) 0.006(3) 0.007(2) 0.006(2) C40 0.033(3) 0.039(3) 0.024(3) 0.004(3) 0.007(3) 0.003(3) C41 0.022(3) 0.034(3) 0.024(3) 0.000(2) 0.006(3) 0.002(3) C42 0.022(3) 0.034(3) 0.023(3) -0.002(3) 0.005(3) -0.001(3) C43 0.022(3) 0.035(3) 0.027(3) -0.004(3) 0.006(3) -0.001(3) C44 0.022(4) 0.036(4) 0.030(3) -0.006(3) 0.005(3) 0.001(3) C45 0.023(4) 0.034(4) 0.031(3) -0.002(3) 0.004(3) 0.002(3) C46 0.023(4) 0.033(3) 0.027(3) 0.001(3) 0.006(3) 0.002(3) C47 0.038(6) 0.029(5) 0.026(5) -0.001(4) 0.002(5) -0.001(4) C48 0.026(6) 0.045(6) 0.042(5) -0.016(5) 0.003(5) 0.006(5) C49 0.032(6) 0.036(6) 0.030(4) 0.003(4) 0.006(5) 0.007(5) C51 0.028(3) 0.038(3) 0.021(3) 0.000(3) 0.003(3) -0.003(2) C52 0.030(3) 0.047(3) 0.021(4) 0.000(3) 0.004(3) -0.009(3) C53 0.036(4) 0.050(4) 0.019(4) 0.002(4) 0.000(3) -0.012(3) C54 0.046(4) 0.046(4) 0.019(4) 0.003(4) -0.001(4) -0.011(3) C55 0.044(4) 0.039(3) 0.020(4) -0.001(4) 0.002(4) -0.004(3) C56 0.036(3) 0.037(3) 0.021(4) 0.000(3) 0.003(3) -0.001(3) C57 0.027(5) 0.057(5) 0.033(6) -0.011(6) 0.001(5) -0.005(4) C58 0.065(7) 0.049(5) 0.038(6) 0.004(6) -0.002(6) -0.018(5) C59 0.035(4) 0.040(6) 0.036(6) 0.001(5) 0.003(5) 0.005(4) C1_1 0.029(2) 0.030(2) 0.013(2) 0.0034(19) 0.011(2) -0.0038(18) Cl1_1 0.029(2) 0.030(2) 0.013(2) 0.0034(19) 0.011(2) -0.0038(18) Cl2_1 0.029(2) 0.030(2) 0.013(2) 0.0034(19) 0.011(2) -0.0038(18) Cl3_1 0.029(2) 0.030(2) 0.013(2) 0.0034(19) 0.011(2) -0.0038(18) C1_2 0.056(3) 0.050(3) 0.048(3) -0.005(2) 0.004(2) 0.007(2) Cl1_2 0.056(3) 0.050(3) 0.048(3) -0.005(2) 0.004(2) 0.007(2) Cl2_2 0.056(3) 0.050(3) 0.048(3) -0.005(2) 0.004(2) 0.007(2) Cl3_2 0.056(3) 0.050(3) 0.048(3) -0.005(2) 0.004(2) 0.007(2) _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 C31 2.039(10) . ? Hg1 C1 2.176(12) . ? B1 C21 1.546(18) . ? B1 C8 1.617(18) . ? B1 C11 1.646(19) . ? C1 C2 1.348(17) . ? C1 C9 1.411(18) . ? C2 C3 1.438(17) . ? C2 H2 0.9500 . ? B2 C51 1.560(19) . ? B2 C38 1.571(17) . ? B2 C41 1.603(18) . ? C3 C4 1.414(19) . ? C3 H3 0.9500 . ? C4 C10 1.393(18) . ? C4 H4 0.9500 . ? C5 C6 1.368(18) . ? C5 C10 1.428(18) . ? C5 H5 0.9500 . ? C6 C7 1.417(17) . ? C6 H6 0.9500 . ? C7 C8 1.371(18) . ? C7 H7 0.9500 . ? C8 C9 1.416(17) . ? C9 C10 1.426(16) . ? C11 C16 1.361(17) . ? C11 C12 1.423(17) . ? C12 C13 1.372(18) . ? C12 C17 1.501(18) . ? C13 C14 1.411(19) . ? C13 H13 0.9500 . ? C14 C15 1.364(18) . ? C14 C18 1.540(18) . ? C15 C16 1.411(18) . ? C15 H15 0.9500 . ? C16 C19 1.522(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C26 1.409(17) . ? C21 C22 1.424(17) . ? C22 C23 1.389(17) . ? C22 C27 1.500(17) . ? C23 C24 1.402(18) . ? C23 H23 0.9500 . ? C24 C25 1.368(18) . ? C24 C28 1.527(17) . ? C25 C26 1.397(17) . ? C25 H25 0.9500 . ? C26 C29 1.510(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 C39 1.354(11) . ? C31 C32 1.366(11) . ? C32 C33 1.431(16) . ? C32 H32 0.9500 . ? C33 C34 1.376(18) . ? C33 H33 0.9500 . ? C34 C40 1.435(18) . ? C34 H34 0.9500 . ? C35 C36 1.319(18) . ? C35 C40 1.407(18) . ? C35 H35 0.9500 . ? C36 C37 1.398(17) . ? C36 H36 0.9500 . ? C37 C38 1.403(17) . ? C37 H37 0.9500 . ? C38 C39 1.467(16) . ? C39 C40 1.475(16) . ? C41 C46 1.379(17) . ? C41 C42 1.424(17) . ? C42 C43 1.394(16) . ? C42 C47 1.525(18) . ? C43 C44 1.375(18) . ? C43 H43 0.9500 . ? C44 C45 1.362(18) . ? C44 C48 1.523(17) . ? C45 C46 1.395(17) . ? C45 H45 0.9500 . ? C46 C49 1.544(17) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.435(17) . ? C51 C56 1.456(18) . ? C52 C53 1.360(18) . ? C52 C57 1.480(19) . ? C53 C54 1.40(2) . ? C53 H53 0.9500 . ? C54 C55 1.406(19) . ? C54 C58 1.501(19) . ? C55 C56 1.356(18) . ? C55 H55 0.9500 . ? C56 C59 1.503(17) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C1_1 Cl3_1 1.7799(11) . ? C1_1 Cl2_1 1.7799(11) . ? C1_1 Cl1_1 1.7800(10) . ? C1_1 H1B_1 1.0000 . ? C1_2 Cl1_2 1.7799(10) . ? C1_2 Cl2_2 1.7800(11) . ? C1_2 Cl3_2 1.7800(10) . ? C1_2 H1C_2 1.0000 . ? 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 C31 Hg1 C1 167.2(4) . . ? C21 B1 C8 126.1(12) . . ? C21 B1 C11 119.4(11) . . ? C8 B1 C11 113.7(11) . . ? C2 C1 C9 125.5(12) . . ? C2 C1 Hg1 105.1(9) . . ? C9 C1 Hg1 129.3(9) . . ? C1 C2 C3 119.9(13) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C51 B2 C38 114.1(11) . . ? C51 B2 C41 120.8(11) . . ? C38 B2 C41 124.8(11) . . ? C4 C3 C2 116.5(12) . . ? C4 C3 H3 121.8 . . ? C2 C3 H3 121.8 . . ? C10 C4 C3 121.8(12) . . ? C10 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C10 121.7(11) . . ? C6 C5 H5 119.1 . . ? C10 C5 H5 119.1 . . ? C5 C6 C7 118.0(12) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C8 C7 C6 122.6(13) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C9 119.7(11) . . ? C7 C8 B1 110.7(11) . . ? C9 C8 B1 128.3(11) . . ? C1 C9 C8 126.8(11) . . ? C1 C9 C10 114.4(11) . . ? C8 C9 C10 118.8(11) . . ? C4 C10 C9 121.6(12) . . ? C4 C10 C5 119.4(11) . . ? C9 C10 C5 118.9(12) . . ? C16 C11 C12 120.4(12) . . ? C16 C11 B1 121.7(11) . . ? C12 C11 B1 117.6(11) . . ? C13 C12 C11 117.9(12) . . ? C13 C12 C17 119.6(11) . . ? C11 C12 C17 122.5(12) . . ? C12 C13 C14 121.8(12) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 119.2(12) . . ? C15 C14 C18 122.1(13) . . ? C13 C14 C18 118.7(12) . . ? C14 C15 C16 120.0(12) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.5(12) . . ? C11 C16 C19 123.6(12) . . ? C15 C16 C19 115.9(11) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 117.5(11) . . ? C26 C21 B1 121.8(11) . . ? C22 C21 B1 120.2(11) . . ? C23 C22 C21 120.6(12) . . ? C23 C22 C27 115.8(11) . . ? C21 C22 C27 123.6(11) . . ? C22 C23 C24 121.3(11) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 117.8(11) . . ? C25 C24 C28 120.8(12) . . ? C23 C24 C28 121.3(11) . . ? C24 C25 C26 122.9(12) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C21 119.8(11) . . ? C25 C26 C29 117.4(11) . . ? C21 C26 C29 122.6(11) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C39 C31 C32 112.9(10) . . ? C39 C31 Hg1 137.4(8) . . ? C32 C31 Hg1 109.7(7) . . ? C31 C32 C33 130.0(11) . . ? C31 C32 H32 115.0 . . ? C33 C32 H32 115.0 . . ? C34 C33 C32 115.6(11) . . ? C34 C33 H33 122.2 . . ? C32 C33 H33 122.2 . . ? C33 C34 C40 119.2(11) . . ? C33 C34 H34 120.4 . . ? C40 C34 H34 120.4 . . ? C36 C35 C40 121.0(12) . . ? C36 C35 H35 119.5 . . ? C40 C35 H35 119.5 . . ? C35 C36 C37 121.3(13) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C38 121.6(12) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C39 120.0(10) . . ? C37 C38 B2 110.3(10) . . ? C39 C38 B2 128.8(10) . . ? C31 C39 C38 122.8(10) . . ? C31 C39 C40 123.2(10) . . ? C38 C39 C40 114.0(10) . . ? C35 C40 C34 119.1(11) . . ? C35 C40 C39 121.9(11) . . ? C34 C40 C39 118.6(11) . . ? C46 C41 C42 117.9(11) . . ? C46 C41 B2 121.1(11) . . ? C42 C41 B2 120.1(11) . . ? C43 C42 C41 119.2(12) . . ? C43 C42 C47 119.2(11) . . ? C41 C42 C47 121.4(11) . . ? C44 C43 C42 121.9(11) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C45 C44 C43 118.4(11) . . ? C45 C44 C48 120.6(12) . . ? C43 C44 C48 120.9(12) . . ? C44 C45 C46 121.7(12) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C41 C46 C45 120.8(12) . . ? C41 C46 C49 125.1(11) . . ? C45 C46 C49 114.0(11) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 C56 118.1(12) . . ? C52 C51 B2 119.6(12) . . ? C56 C51 B2 122.2(11) . . ? C53 C52 C51 120.1(13) . . ? C53 C52 C57 118.1(12) . . ? C51 C52 C57 121.8(12) . . ? C52 C53 C54 122.4(13) . . ? C52 C53 H53 118.8 . . ? C54 C53 H53 118.8 . . ? C53 C54 C55 117.1(13) . . ? C53 C54 C58 122.1(13) . . ? C55 C54 C58 120.7(14) . . ? C56 C55 C54 123.9(13) . . ? C56 C55 H55 118.1 . . ? C54 C55 H55 118.1 . . ? C55 C56 C51 118.3(12) . . ? C55 C56 C59 121.1(12) . . ? C51 C56 C59 120.6(12) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? Cl3_1 C1_1 Cl2_1 95.30(7) . . ? Cl3_1 C1_1 Cl1_1 95.30(7) . . ? Cl2_1 C1_1 Cl1_1 95.28(7) . . ? Cl3_1 C1_1 H1B_1 121.4 . . ? Cl2_1 C1_1 H1B_1 121.4 . . ? Cl1_1 C1_1 H1B_1 121.4 . . ? Cl1_2 C1_2 Cl2_2 95.28(7) . . ? Cl1_2 C1_2 Cl3_2 95.27(7) . . ? Cl2_2 C1_2 Cl3_2 95.27(7) . . ? Cl1_2 C1_2 H1C_2 121.4 . . ? Cl2_2 C1_2 H1C_2 121.4 . . ? Cl3_2 C1_2 H1C_2 121.4 . . ? 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 C31 Hg1 C1 C2 36(2) . . . . ? C31 Hg1 C1 C9 -141.0(16) . . . . ? C9 C1 C2 C3 -4(2) . . . . ? Hg1 C1 C2 C3 179.1(10) . . . . ? C1 C2 C3 C4 -2.3(19) . . . . ? C2 C3 C4 C10 4.8(19) . . . . ? C10 C5 C6 C7 1.0(19) . . . . ? C5 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C9 -4.0(19) . . . . ? C6 C7 C8 B1 164.0(12) . . . . ? C21 B1 C8 C7 -131.5(13) . . . . ? C11 B1 C8 C7 38.0(14) . . . . ? C21 B1 C8 C9 35(2) . . . . ? C11 B1 C8 C9 -155.4(12) . . . . ? C2 C1 C9 C8 -173.1(13) . . . . ? Hg1 C1 C9 C8 3.6(19) . . . . ? C2 C1 C9 C10 6.6(19) . . . . ? Hg1 C1 C9 C10 -176.7(8) . . . . ? C7 C8 C9 C1 -175.4(12) . . . . ? B1 C8 C9 C1 19(2) . . . . ? C7 C8 C9 C10 5.0(18) . . . . ? B1 C8 C9 C10 -160.6(12) . . . . ? C3 C4 C10 C9 -1.6(19) . . . . ? C3 C4 C10 C5 177.4(12) . . . . ? C1 C9 C10 C4 -3.8(18) . . . . ? C8 C9 C10 C4 175.8(11) . . . . ? C1 C9 C10 C5 177.2(10) . . . . ? C8 C9 C10 C5 -3.2(18) . . . . ? C6 C5 C10 C4 -178.9(12) . . . . ? C6 C5 C10 C9 0.2(19) . . . . ? C21 B1 C11 C16 -134.4(12) . . . . ? C8 B1 C11 C16 55.5(15) . . . . ? C21 B1 C11 C12 52.8(16) . . . . ? C8 B1 C11 C12 -117.4(12) . . . . ? C16 C11 C12 C13 6.0(18) . . . . ? B1 C11 C12 C13 179.0(11) . . . . ? C16 C11 C12 C17 -173.2(11) . . . . ? B1 C11 C12 C17 -0.2(17) . . . . ? C11 C12 C13 C14 -4.6(18) . . . . ? C17 C12 C13 C14 174.6(12) . . . . ? C12 C13 C14 C15 0.1(19) . . . . ? C12 C13 C14 C18 178.9(12) . . . . ? C13 C14 C15 C16 3.1(18) . . . . ? C18 C14 C15 C16 -175.6(12) . . . . ? C12 C11 C16 C15 -3.0(18) . . . . ? B1 C11 C16 C15 -175.7(11) . . . . ? C12 C11 C16 C19 177.2(11) . . . . ? B1 C11 C16 C19 4.6(18) . . . . ? C14 C15 C16 C11 -1.6(18) . . . . ? C14 C15 C16 C19 178.1(11) . . . . ? C8 B1 C21 C26 38.8(18) . . . . ? C11 B1 C21 C26 -130.0(12) . . . . ? C8 B1 C21 C22 -149.7(12) . . . . ? C11 B1 C21 C22 41.4(16) . . . . ? C26 C21 C22 C23 2.1(17) . . . . ? B1 C21 C22 C23 -169.7(11) . . . . ? C26 C21 C22 C27 -176.3(11) . . . . ? B1 C21 C22 C27 11.9(18) . . . . ? C21 C22 C23 C24 -1.4(17) . . . . ? C27 C22 C23 C24 177.2(11) . . . . ? C22 C23 C24 C25 -0.5(17) . . . . ? C22 C23 C24 C28 -178.5(11) . . . . ? C23 C24 C25 C26 1.6(18) . . . . ? C28 C24 C25 C26 179.6(11) . . . . ? C24 C25 C26 C21 -0.8(18) . . . . ? C24 C25 C26 C29 174.9(11) . . . . ? C22 C21 C26 C25 -1.1(16) . . . . ? B1 C21 C26 C25 170.6(11) . . . . ? C22 C21 C26 C29 -176.5(11) . . . . ? B1 C21 C26 C29 -4.8(17) . . . . ? C1 Hg1 C31 C39 -124.0(18) . . . . ? C1 Hg1 C31 C32 54(2) . . . . ? C39 C31 C32 C33 -4.0(18) . . . . ? Hg1 C31 C32 C33 177.3(10) . . . . ? C31 C32 C33 C34 2.8(19) . . . . ? C32 C33 C34 C40 -3.8(17) . . . . ? C40 C35 C36 C37 5(2) . . . . ? C35 C36 C37 C38 -3(2) . . . . ? C36 C37 C38 C39 0.1(19) . . . . ? C36 C37 C38 B2 170.0(11) . . . . ? C51 B2 C38 C37 42.0(15) . . . . ? C41 B2 C38 C37 -130.6(12) . . . . ? C51 B2 C38 C39 -149.2(12) . . . . ? C41 B2 C38 C39 38.2(19) . . . . ? C32 C31 C39 C38 -177.1(10) . . . . ? Hg1 C31 C39 C38 1.0(19) . . . . ? C32 C31 C39 C40 6.4(17) . . . . ? Hg1 C31 C39 C40 -175.5(9) . . . . ? C37 C38 C39 C31 -176.5(11) . . . . ? B2 C38 C39 C31 15.6(19) . . . . ? C37 C38 C39 C40 0.2(16) . . . . ? B2 C38 C39 C40 -167.6(12) . . . . ? C36 C35 C40 C34 -178.1(12) . . . . ? C36 C35 C40 C39 -5(2) . . . . ? C33 C34 C40 C35 179.6(12) . . . . ? C33 C34 C40 C39 6.3(18) . . . . ? C31 C39 C40 C35 178.9(11) . . . . ? C38 C39 C40 C35 2.2(17) . . . . ? C31 C39 C40 C34 -8.0(19) . . . . ? C38 C39 C40 C34 175.2(11) . . . . ? C51 B2 C41 C46 -131.6(13) . . . . ? C38 B2 C41 C46 40.6(17) . . . . ? C51 B2 C41 C42 37.6(17) . . . . ? C38 B2 C41 C42 -150.3(12) . . . . ? C46 C41 C42 C43 1.1(17) . . . . ? B2 C41 C42 C43 -168.4(11) . . . . ? C46 C41 C42 C47 -174.4(11) . . . . ? B2 C41 C42 C47 16.0(17) . . . . ? C41 C42 C43 C44 1.6(17) . . . . ? C47 C42 C43 C44 177.2(11) . . . . ? C42 C43 C44 C45 -3.0(18) . . . . ? C42 C43 C44 C48 179.6(11) . . . . ? C43 C44 C45 C46 1.8(18) . . . . ? C48 C44 C45 C46 179.2(11) . . . . ? C42 C41 C46 C45 -2.3(17) . . . . ? B2 C41 C46 C45 167.1(11) . . . . ? C42 C41 C46 C49 -178.6(11) . . . . ? B2 C41 C46 C49 -9.2(18) . . . . ? C44 C45 C46 C41 0.9(19) . . . . ? C44 C45 C46 C49 177.6(11) . . . . ? C38 B2 C51 C52 -120.4(12) . . . . ? C41 B2 C51 C52 52.6(16) . . . . ? C38 B2 C51 C56 56.5(16) . . . . ? C41 B2 C51 C56 -130.5(12) . . . . ? C56 C51 C52 C53 1.1(18) . . . . ? B2 C51 C52 C53 178.1(11) . . . . ? C56 C51 C52 C57 -175.8(11) . . . . ? B2 C51 C52 C57 1.2(18) . . . . ? C51 C52 C53 C54 -1.3(19) . . . . ? C57 C52 C53 C54 175.7(12) . . . . ? C52 C53 C54 C55 -1.0(19) . . . . ? C52 C53 C54 C58 179.0(12) . . . . ? C53 C54 C55 C56 3.8(19) . . . . ? C58 C54 C55 C56 -176.2(12) . . . . ? C54 C55 C56 C51 -4.0(19) . . . . ? C54 C55 C56 C59 177.7(12) . . . . ? C52 C51 C56 C55 1.5(17) . . . . ? B2 C51 C56 C55 -175.4(12) . . . . ? C52 C51 C56 C59 179.8(11) . . . . ? B2 C51 C56 C59 2.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 3.103 _refine_diff_density_min -1.782 _refine_diff_density_rms 0.185 # Attachment '4.cif' data_jpsi _database_code_depnum_ccdc_archive 'CCDC 675717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 1-{Mes2B}-8-{HgCl}C10H6 _chemical_formula_sum 'C34 H34 B Cl Hg' _chemical_formula_weight 689.46 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' B B 0.0013 0.0007 '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' 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 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 13.9211(17) _cell_length_b 18.702(2) _cell_length_c 22.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.443(2) _cell_angle_gamma 90.00 _cell_volume 5801.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5087 _cell_measurement_theta_min 4.723 _cell_measurement_theta_max 56.075 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 5.419 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3713 _exptl_absorpt_correction_T_max 0.5092 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39001 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10220 _reflns_number_gt 7406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^2^+8.0000P] 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 rigid _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10220 _refine_ls_number_parameters 667 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _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 0.853948(19) 0.141643(16) 0.209904(13) 0.03021(10) Uani 1 1 d . . . Hg2 Hg 1.146386(19) 0.077839(16) 0.272686(13) 0.02995(10) Uani 1 1 d . . . Cl1 Cl 0.92872(12) 0.03110(10) 0.19916(8) 0.0344(4) Uani 1 1 d . . . Cl2 Cl 1.06760(13) 0.18746(10) 0.26584(9) 0.0362(5) Uani 1 1 d . . . B1 B 0.6490(6) 0.1489(5) 0.1281(3) 0.0276(19) Uani 1 1 d . . . B2 B 1.3443(6) 0.0774(5) 0.3702(3) 0.0258(18) Uani 1 1 d . . . C1 C 0.7951(5) 0.2397(4) 0.2270(3) 0.0284(17) Uani 1 1 d . . . C2 C 0.8544(5) 0.2843(4) 0.2642(3) 0.0360(19) Uani 1 1 d . . . H2A H 0.9170 0.2692 0.2781 0.043 Uiso 1 1 calc R . . C3 C 0.8236(5) 0.3517(4) 0.2819(4) 0.040(2) Uani 1 1 d . . . H3A H 0.8654 0.3811 0.3066 0.047 Uiso 1 1 calc R . . C4 C 0.7323(5) 0.3731(4) 0.2623(3) 0.0347(18) Uani 1 1 d . . . H4A H 0.7115 0.4176 0.2740 0.042 Uiso 1 1 calc R . . C5 C 0.5715(5) 0.3542(4) 0.2054(3) 0.0306(17) Uani 1 1 d . . . H5A H 0.5524 0.3992 0.2171 0.037 Uiso 1 1 calc R . . C6 C 0.5082(5) 0.3128(4) 0.1706(3) 0.0293(17) Uani 1 1 d . . . H6A H 0.4451 0.3287 0.1592 0.035 Uiso 1 1 calc R . . C7 C 0.5380(5) 0.2444(4) 0.1511(3) 0.0308(18) Uani 1 1 d . . . H7A H 0.4925 0.2156 0.1284 0.037 Uiso 1 1 calc R . . C8 C 0.6321(5) 0.2192(4) 0.1647(3) 0.0246(16) Uani 1 1 d . . . C9 C 0.6990(5) 0.2621(4) 0.2055(3) 0.0282(17) Uani 1 1 d . . . C10 C 0.6680(5) 0.3297(4) 0.2247(3) 0.0299(17) Uani 1 1 d . . . C11 C 0.7314(5) 0.1379(4) 0.0878(3) 0.0247(16) Uani 1 1 d . . . C12 C 0.7766(5) 0.1955(4) 0.0601(3) 0.0268(16) Uani 1 1 d . . . C13 C 0.8391(5) 0.1828(4) 0.0175(3) 0.0347(19) Uani 1 1 d . . . H13A H 0.8651 0.2215 -0.0009 0.042 Uiso 1 1 calc R . . C14 C 0.8636(5) 0.1141(4) 0.0016(3) 0.0346(18) Uani 1 1 d . . . C15 C 0.8231(5) 0.0576(4) 0.0289(3) 0.0347(18) Uani 1 1 d . . . H15A H 0.8393 0.0114 0.0185 0.042 Uiso 1 1 calc R . . C16 C 0.7590(5) 0.0663(4) 0.0711(3) 0.0292(17) Uani 1 1 d . . . C17 C 0.7585(5) 0.2732(4) 0.0718(3) 0.0348(18) Uani 1 1 d . . . H17A H 0.7963 0.3022 0.0482 0.052 Uiso 1 1 calc R . . H17B H 0.7768 0.2835 0.1136 0.052 Uiso 1 1 calc R . . H17C H 0.6910 0.2837 0.0609 0.052 Uiso 1 1 calc R . . C18 C 0.9311(6) 0.1014(5) -0.0450(4) 0.051(2) Uani 1 1 d . . . H18A H 0.9525 0.1465 -0.0589 0.077 Uiso 1 1 calc R . . H18B H 0.8975 0.0753 -0.0782 0.077 Uiso 1 1 calc R . . H18C H 0.9862 0.0743 -0.0275 0.077 Uiso 1 1 calc R . . C19 C 0.7232(5) -0.0009(4) 0.0973(3) 0.0326(18) Uani 1 1 d . . . H19A H 0.7508 -0.0416 0.0798 0.049 Uiso 1 1 calc R . . H19B H 0.6539 -0.0030 0.0889 0.049 Uiso 1 1 calc R . . H19C H 0.7420 -0.0011 0.1399 0.049 Uiso 1 1 calc R . . C21 C 0.5643(5) 0.0902(4) 0.1290(3) 0.0256(10) Uani 1 1 d U . . C22 C 0.5022(5) 0.0791(4) 0.0730(3) 0.0260(10) Uani 1 1 d U . . C23 C 0.4337(5) 0.0240(4) 0.0718(3) 0.0329(18) Uani 1 1 d . . . H23A H 0.3929 0.0156 0.0363 0.040 Uiso 1 1 calc R . . C24 C 0.4246(5) -0.0180(4) 0.1209(3) 0.0341(18) Uani 1 1 d . . . C25 C 0.4839(5) -0.0033(4) 0.1740(3) 0.0298(17) Uani 1 1 d . . . H25A H 0.4782 -0.0306 0.2080 0.036 Uiso 1 1 calc R . . C26 C 0.5535(5) 0.0533(4) 0.1774(3) 0.0260(10) Uani 1 1 d U . . C27 C 0.5034(6) 0.1254(4) 0.0176(3) 0.038(2) Uani 1 1 d . . . H27A H 0.4561 0.1080 -0.0140 0.057 Uiso 1 1 calc R . . H27B H 0.5665 0.1235 0.0048 0.057 Uiso 1 1 calc R . . H27C H 0.4883 0.1739 0.0269 0.057 Uiso 1 1 calc R . . C28 C 0.3542(6) -0.0801(5) 0.1182(4) 0.051(2) Uani 1 1 d . . . H28A H 0.3186 -0.0830 0.0787 0.076 Uiso 1 1 calc R . . H28B H 0.3100 -0.0729 0.1471 0.076 Uiso 1 1 calc R . . H28C H 0.3894 -0.1238 0.1271 0.076 Uiso 1 1 calc R . . C29 C 0.6160(5) 0.0632(4) 0.2358(3) 0.037(2) Uani 1 1 d . . . H29A H 0.6595 0.1024 0.2327 0.056 Uiso 1 1 calc R . . H29B H 0.6526 0.0204 0.2457 0.056 Uiso 1 1 calc R . . H29C H 0.5761 0.0731 0.2666 0.056 Uiso 1 1 calc R . . C31 C 1.2076(5) -0.0224(4) 0.2714(3) 0.0230(15) Uani 1 1 d . . . C32 C 1.1495(5) -0.0728(4) 0.2389(3) 0.0332(18) Uani 1 1 d . . . H32A H 1.0882 -0.0594 0.2209 0.040 Uiso 1 1 calc R . . C33 C 1.1798(5) -0.1424(4) 0.2322(3) 0.0335(18) Uani 1 1 d . . . H33A H 1.1386 -0.1758 0.2115 0.040 Uiso 1 1 calc R . . C34 C 1.2710(5) -0.1612(4) 0.2563(3) 0.0316(18) Uani 1 1 d . . . H34A H 1.2920 -0.2078 0.2516 0.038 Uiso 1 1 calc R . . C35 C 1.4310(5) -0.1330(4) 0.3090(3) 0.0322(18) Uani 1 1 d . . . H35A H 1.4512 -0.1793 0.3018 0.039 Uiso 1 1 calc R . . C36 C 1.4948(5) -0.0856(4) 0.3393(3) 0.0319(18) Uani 1 1 d . . . H36A H 1.5591 -0.0983 0.3509 0.038 Uiso 1 1 calc R . . C37 C 1.4607(5) -0.0169(4) 0.3525(3) 0.0298(17) Uani 1 1 d . . . H37A H 1.5047 0.0144 0.3735 0.036 Uiso 1 1 calc R . . C38 C 1.3664(5) 0.0072(4) 0.3365(3) 0.0246(16) Uani 1 1 d . . . C39 C 1.3013(5) -0.0409(4) 0.2996(3) 0.0264(16) Uani 1 1 d . . . C40 C 1.3342(5) -0.1118(4) 0.2884(3) 0.0277(16) Uani 1 1 d . . . C41 C 1.2492(5) 0.0910(4) 0.3999(3) 0.0279(17) Uani 1 1 d . . . C42 C 1.2113(5) 0.1616(4) 0.4042(3) 0.0275(17) Uani 1 1 d . . . C43 C 1.1324(5) 0.1745(5) 0.4344(3) 0.0355(19) Uani 1 1 d . . . H43A H 1.1076 0.2207 0.4347 0.043 Uiso 1 1 calc R . . C44 C 1.0892(5) 0.1207(5) 0.4645(3) 0.0357(19) Uani 1 1 d . . . C45 C 1.1270(5) 0.0522(5) 0.4625(3) 0.0355(19) Uani 1 1 d . . . H45A H 1.0992 0.0156 0.4826 0.043 Uiso 1 1 calc R . . C46 C 1.2055(5) 0.0358(4) 0.4316(3) 0.0312(18) Uani 1 1 d . . . C47 C 1.2530(5) 0.2264(4) 0.3749(3) 0.0318(18) Uani 1 1 d . . . H47A H 1.2175 0.2685 0.3831 0.048 Uiso 1 1 calc R . . H47B H 1.2479 0.2191 0.3323 0.048 Uiso 1 1 calc R . . H47C H 1.3199 0.2322 0.3909 0.048 Uiso 1 1 calc R . . C48 C 1.0073(6) 0.1368(5) 0.4989(4) 0.044(2) Uani 1 1 d . . . H48A H 0.9869 0.0936 0.5167 0.066 Uiso 1 1 calc R . . H48B H 0.9542 0.1563 0.4723 0.066 Uiso 1 1 calc R . . H48C H 1.0279 0.1708 0.5299 0.066 Uiso 1 1 calc R . . C49 C 1.2397(6) -0.0411(4) 0.4340(4) 0.041(2) Uani 1 1 d . . . H49A H 1.2009 -0.0687 0.4580 0.061 Uiso 1 1 calc R . . H49B H 1.3063 -0.0431 0.4515 0.061 Uiso 1 1 calc R . . H49C H 1.2335 -0.0604 0.3941 0.061 Uiso 1 1 calc R . . C51 C 1.4289(5) 0.1352(4) 0.3784(3) 0.0291(10) Uani 1 1 d U . . C52 C 1.4749(5) 0.1522(4) 0.4360(3) 0.0297(11) Uani 1 1 d U . . C53 C 1.5457(5) 0.2049(4) 0.4422(3) 0.038(2) Uani 1 1 d . . . H53A H 1.5771 0.2153 0.4803 0.046 Uiso 1 1 calc R . . C54 C 1.5714(5) 0.2428(4) 0.3934(4) 0.040(2) Uani 1 1 d . . . C55 C 1.5261(5) 0.2246(4) 0.3371(4) 0.039(2) Uani 1 1 d . . . H55A H 1.5418 0.2487 0.3035 0.046 Uiso 1 1 calc R . . C56 C 1.4544(5) 0.1684(4) 0.3301(3) 0.0292(11) Uani 1 1 d U . . C57 C 1.4538(6) 0.1108(4) 0.4908(3) 0.0370(19) Uani 1 1 d . . . H57A H 1.4033 0.0767 0.4792 0.056 Uiso 1 1 calc R . . H57B H 1.4335 0.1433 0.5198 0.056 Uiso 1 1 calc R . . H57C H 1.5113 0.0862 0.5080 0.056 Uiso 1 1 calc R . . C58 C 1.6457(6) 0.3029(5) 0.4027(4) 0.056(3) Uani 1 1 d . . . H58A H 1.6686 0.3074 0.4447 0.083 Uiso 1 1 calc R . . H58B H 1.6161 0.3470 0.3881 0.083 Uiso 1 1 calc R . . H58C H 1.6991 0.2922 0.3812 0.083 Uiso 1 1 calc R . . C59 C 1.4068(6) 0.1567(4) 0.2661(3) 0.0367(19) Uani 1 1 d . . . H59A H 1.3598 0.1191 0.2654 0.055 Uiso 1 1 calc R . . H59B H 1.4552 0.1437 0.2413 0.055 Uiso 1 1 calc R . . H59C H 1.3753 0.2000 0.2511 0.055 Uiso 1 1 calc R . . C61 C 0.8255(6) -0.0187(5) 0.3842(3) 0.046(2) Uani 1 1 d . . . H61A H 0.8386 -0.0673 0.3887 0.055 Uiso 1 1 calc R . . C62 C 0.7375(6) 0.0079(5) 0.3966(3) 0.045(2) Uani 1 1 d . . . H62A H 0.6926 -0.0223 0.4108 0.054 Uiso 1 1 calc R . . C63 C 0.7165(7) 0.0797(6) 0.3876(4) 0.062(3) Uani 1 1 d . . . H63A H 0.6563 0.0978 0.3937 0.075 Uiso 1 1 calc R . . C64 C 0.7868(7) 0.1244(5) 0.3694(4) 0.052(2) Uani 1 1 d . . . H64A H 0.7746 0.1731 0.3648 0.062 Uiso 1 1 calc R . . C65 C 0.8747(7) 0.0969(6) 0.3579(4) 0.053(3) Uani 1 1 d . . . H65A H 0.9213 0.1269 0.3451 0.063 Uiso 1 1 calc R . . C66 C 0.8927(6) 0.0255(5) 0.3656(4) 0.048(2) Uani 1 1 d . . . H66A H 0.9519 0.0070 0.3579 0.058 Uiso 1 1 calc R . . C71 C 1.2373(11) -0.3643(9) 0.3728(5) 0.104(5) Uani 1 1 d . . . H71A H 1.1764 -0.3838 0.3610 0.125 Uiso 1 1 calc R . . C72 C 1.2470(7) -0.2921(8) 0.3818(5) 0.078(4) Uani 1 1 d . . . H72A H 1.1920 -0.2633 0.3779 0.093 Uiso 1 1 calc R . . C73 C 1.3357(7) -0.2617(6) 0.3963(4) 0.055(3) Uani 1 1 d . . . H73A H 1.3421 -0.2125 0.4009 0.066 Uiso 1 1 calc R . . C74 C 1.4140(7) -0.3044(7) 0.4038(4) 0.062(3) Uani 1 1 d . . . H74A H 1.4747 -0.2841 0.4150 0.075 Uiso 1 1 calc R . . C75 C 1.4072(9) -0.3771(7) 0.3953(4) 0.078(4) Uani 1 1 d . . . H75A H 1.4625 -0.4055 0.3991 0.094 Uiso 1 1 calc R . . C76 C 1.3159(12) -0.4075(7) 0.3809(5) 0.094(5) Uani 1 1 d . . . H76A H 1.3090 -0.4568 0.3769 0.113 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 0.02579(16) 0.02546(18) 0.03826(17) -0.00008(13) -0.00008(12) 0.00084(12) Hg2 0.02601(16) 0.02478(18) 0.03835(18) 0.00097(13) 0.00146(12) 0.00120(12) Cl1 0.0265(9) 0.0265(11) 0.0486(11) 0.0020(9) -0.0018(8) 0.0005(7) Cl2 0.0268(10) 0.0263(11) 0.0536(12) 0.0025(9) -0.0019(8) -0.0002(8) B1 0.021(4) 0.036(6) 0.024(4) 0.009(4) -0.003(3) -0.003(4) B2 0.026(4) 0.025(5) 0.025(4) 0.004(4) 0.000(3) 0.004(3) C1 0.025(4) 0.028(4) 0.034(4) 0.000(3) 0.009(3) -0.001(3) C2 0.030(4) 0.034(5) 0.043(5) -0.006(4) 0.001(3) 0.002(3) C3 0.027(4) 0.042(6) 0.048(5) -0.015(4) 0.003(4) -0.011(4) C4 0.036(4) 0.025(5) 0.043(4) -0.010(4) 0.007(4) 0.002(3) C5 0.033(4) 0.023(4) 0.038(4) 0.006(3) 0.010(3) 0.003(3) C6 0.024(4) 0.030(5) 0.034(4) 0.003(3) 0.005(3) 0.005(3) C7 0.027(4) 0.039(5) 0.028(4) 0.011(3) 0.009(3) -0.007(3) C8 0.020(3) 0.024(4) 0.032(4) 0.006(3) 0.011(3) -0.002(3) C9 0.036(4) 0.027(4) 0.023(4) 0.001(3) 0.008(3) -0.002(3) C10 0.027(4) 0.030(5) 0.032(4) 0.001(3) 0.002(3) -0.002(3) C11 0.023(4) 0.027(4) 0.024(3) 0.002(3) 0.003(3) 0.001(3) C12 0.023(4) 0.032(5) 0.025(4) 0.004(3) 0.000(3) -0.001(3) C13 0.030(4) 0.043(6) 0.031(4) 0.007(4) 0.002(3) -0.007(4) C14 0.033(4) 0.038(5) 0.033(4) -0.006(4) 0.002(3) -0.002(4) C15 0.034(4) 0.033(5) 0.037(4) -0.005(4) 0.004(3) 0.002(3) C16 0.027(4) 0.038(5) 0.023(4) -0.001(3) 0.000(3) 0.000(3) C17 0.037(4) 0.034(5) 0.032(4) 0.003(3) 0.001(3) -0.005(4) C18 0.047(5) 0.058(7) 0.053(5) -0.014(5) 0.018(4) -0.005(5) C19 0.037(4) 0.028(5) 0.034(4) -0.007(3) 0.008(3) 0.007(3) C21 0.016(2) 0.026(3) 0.035(2) -0.0098(19) 0.0033(18) 0.0023(17) C22 0.017(2) 0.027(3) 0.034(2) -0.009(2) 0.0034(18) 0.0022(18) C23 0.036(4) 0.033(5) 0.030(4) -0.001(3) 0.003(3) -0.003(3) C24 0.033(4) 0.033(5) 0.036(4) -0.007(4) 0.003(3) 0.000(3) C25 0.030(4) 0.030(5) 0.029(4) 0.006(3) 0.003(3) -0.002(3) C26 0.016(2) 0.027(3) 0.035(2) -0.009(2) 0.0031(18) 0.0027(18) C27 0.043(5) 0.046(6) 0.027(4) 0.001(4) 0.005(3) -0.008(4) C28 0.052(5) 0.045(6) 0.054(5) 0.003(4) 0.002(4) -0.020(4) C29 0.038(4) 0.051(6) 0.018(4) 0.000(3) -0.015(3) -0.018(4) C31 0.021(4) 0.019(4) 0.031(4) 0.003(3) 0.009(3) 0.001(3) C32 0.029(4) 0.034(5) 0.037(4) -0.010(4) 0.008(3) 0.002(3) C33 0.032(4) 0.030(5) 0.038(4) -0.004(4) 0.004(3) -0.009(3) C34 0.029(4) 0.025(5) 0.043(4) -0.005(3) 0.009(3) 0.003(3) C35 0.035(4) 0.028(5) 0.034(4) 0.000(3) 0.007(3) 0.009(3) C36 0.031(4) 0.028(5) 0.036(4) -0.001(3) 0.003(3) 0.004(3) C37 0.027(4) 0.032(5) 0.033(4) -0.015(3) 0.014(3) -0.001(3) C38 0.020(4) 0.031(4) 0.025(4) 0.002(3) 0.008(3) 0.000(3) C39 0.022(4) 0.028(5) 0.030(4) 0.002(3) 0.006(3) -0.003(3) C40 0.027(4) 0.028(4) 0.029(4) -0.002(3) 0.008(3) 0.000(3) C41 0.029(4) 0.029(5) 0.027(4) 0.005(3) 0.008(3) -0.005(3) C42 0.030(4) 0.030(5) 0.022(4) 0.001(3) 0.002(3) -0.004(3) C43 0.035(4) 0.039(5) 0.032(4) -0.001(4) 0.001(3) 0.005(4) C44 0.035(4) 0.045(6) 0.027(4) -0.006(4) 0.002(3) -0.002(4) C45 0.035(4) 0.039(5) 0.033(4) -0.001(4) 0.009(3) -0.011(4) C46 0.035(4) 0.029(5) 0.030(4) -0.002(3) 0.007(3) -0.005(3) C47 0.033(4) 0.026(5) 0.036(4) -0.004(3) 0.003(3) -0.001(3) C48 0.044(5) 0.050(6) 0.040(5) 0.003(4) 0.014(4) 0.000(4) C49 0.055(5) 0.031(5) 0.041(5) 0.007(4) 0.023(4) 0.001(4) C51 0.021(2) 0.037(3) 0.029(2) -0.007(2) 0.0031(18) 0.0112(19) C52 0.022(2) 0.037(3) 0.030(2) -0.007(2) 0.0030(18) 0.010(2) C53 0.036(4) 0.041(5) 0.038(4) -0.014(4) 0.004(4) -0.002(4) C54 0.028(4) 0.036(5) 0.057(5) -0.012(4) 0.013(4) -0.007(4) C55 0.035(4) 0.029(5) 0.057(5) 0.005(4) 0.024(4) 0.004(4) C56 0.021(2) 0.038(3) 0.029(2) -0.008(2) 0.0036(19) 0.012(2) C57 0.045(5) 0.040(5) 0.025(4) -0.003(4) -0.001(3) 0.000(4) C58 0.046(5) 0.046(6) 0.077(7) -0.012(5) 0.016(5) -0.012(4) C59 0.042(5) 0.039(5) 0.029(4) 0.005(4) 0.008(3) 0.003(4) C61 0.047(5) 0.049(6) 0.041(5) -0.006(4) 0.000(4) 0.016(4) C62 0.047(5) 0.051(6) 0.036(4) -0.002(4) 0.003(4) -0.002(4) C63 0.046(6) 0.080(9) 0.056(6) -0.009(6) -0.012(5) 0.000(6) C64 0.049(6) 0.058(7) 0.045(5) -0.010(5) -0.004(4) 0.004(5) C65 0.050(6) 0.071(8) 0.036(5) -0.005(5) 0.002(4) -0.016(5) C66 0.041(5) 0.054(7) 0.053(5) -0.013(5) 0.018(4) 0.003(4) C71 0.117(12) 0.114(13) 0.072(8) 0.049(9) -0.028(8) -0.053(10) C72 0.036(6) 0.117(12) 0.078(7) 0.045(8) 0.000(5) -0.004(6) C73 0.058(6) 0.059(7) 0.049(5) 0.011(5) 0.003(5) -0.001(5) C74 0.048(6) 0.100(10) 0.040(5) 0.001(6) 0.013(4) -0.014(6) C75 0.090(9) 0.097(11) 0.047(6) -0.010(6) 0.006(6) 0.036(8) C76 0.153(14) 0.067(10) 0.053(7) 0.005(6) -0.018(8) -0.026(9) _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 2.065(7) . ? Hg1 Cl1 2.3411(19) . ? Hg1 C11 3.039(6) . ? Hg1 B1 3.190(7) . ? Hg1 Cl2 3.1925(18) . ? Hg2 C31 2.060(7) . ? Hg2 Cl2 2.3207(19) . ? Hg2 C41 3.037(7) . ? Hg2 B2 3.290(7) . ? Hg2 Cl1 3.3733(17) . ? B1 C11 1.565(11) . ? B1 C8 1.583(11) . ? B1 C21 1.613(10) . ? B2 C38 1.564(11) . ? B2 C41 1.579(11) . ? B2 C51 1.593(11) . ? C1 C2 1.376(10) . ? C1 C9 1.425(10) . ? C2 C3 1.405(11) . ? C2 H2A 0.9300 . ? C3 C4 1.351(10) . ? C3 H3A 0.9300 . ? C4 C10 1.407(10) . ? C4 H4A 0.9300 . ? C5 C6 1.346(10) . ? C5 C10 1.432(10) . ? C5 H5A 0.9300 . ? C6 C7 1.433(10) . ? C6 H6A 0.9300 . ? C7 C8 1.388(9) . ? C7 H7A 0.9300 . ? C8 C9 1.460(9) . ? C9 C10 1.422(10) . ? C11 C12 1.430(10) . ? C11 C16 1.455(10) . ? C12 C13 1.397(10) . ? C12 C17 1.505(10) . ? C13 C14 1.387(11) . ? C13 H13A 0.9300 . ? C14 C15 1.378(11) . ? C14 C18 1.514(11) . ? C15 C16 1.394(10) . ? C15 H15A 0.9300 . ? C16 C19 1.499(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 C26 1.315(10) . ? C21 C22 1.446(9) . ? C22 C23 1.402(10) . ? C22 C27 1.518(10) . ? C23 C24 1.374(10) . ? C23 H23A 0.9300 . ? C24 C25 1.389(9) . ? C24 C28 1.516(10) . ? C25 C26 1.430(10) . ? C25 H25A 0.9300 . ? C26 C29 1.488(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C32 1.388(10) . ? C31 C39 1.418(9) . ? C32 C33 1.382(10) . ? C32 H32A 0.9300 . ? C33 C34 1.360(10) . ? C33 H33A 0.9300 . ? C34 C40 1.408(10) . ? C34 H34A 0.9300 . ? C35 C36 1.372(10) . ? C35 C40 1.424(10) . ? C35 H35A 0.9300 . ? C36 C37 1.413(10) . ? C36 H36A 0.9300 . ? C37 C38 1.392(9) . ? C37 H37A 0.9300 . ? C38 C39 1.458(9) . ? C39 C40 1.435(10) . ? C41 C42 1.430(10) . ? C41 C46 1.432(10) . ? C42 C43 1.385(10) . ? C42 C47 1.530(10) . ? C43 C44 1.392(11) . ? C43 H43A 0.9300 . ? C44 C45 1.388(11) . ? C44 C48 1.489(10) . ? C45 C46 1.403(10) . ? C45 H45A 0.9300 . ? C46 C49 1.515(10) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C51 C56 1.337(10) . ? C51 C52 1.405(9) . ? C52 C53 1.388(10) . ? C52 C57 1.515(10) . ? C53 C54 1.390(11) . ? C53 H53A 0.9300 . ? C54 C55 1.382(11) . ? C54 C58 1.522(11) . ? C55 C56 1.444(11) . ? C55 H55A 0.9300 . ? C56 C59 1.521(9) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 C66 1.356(12) . ? C61 C62 1.384(11) . ? C61 H61A 0.9300 . ? C62 C63 1.383(13) . ? C62 H62A 0.9300 . ? C63 C64 1.388(13) . ? C63 H63A 0.9300 . ? C64 C65 1.382(12) . ? C64 H64A 0.9300 . ? C65 C66 1.366(13) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C71 C76 1.353(19) . ? C71 C72 1.370(17) . ? C71 H71A 0.9300 . ? C72 C73 1.360(13) . ? C72 H72A 0.9300 . ? C73 C74 1.344(13) . ? C73 H73A 0.9300 . ? C74 C75 1.376(15) . ? C74 H74A 0.9300 . ? C75 C76 1.391(17) . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? 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 Cl1 174.8(2) . . ? C1 Hg1 C11 89.9(2) . . ? Cl1 Hg1 C11 95.24(14) . . ? C1 Hg1 B1 73.9(3) . . ? Cl1 Hg1 B1 110.78(17) . . ? C11 Hg1 B1 28.98(19) . . ? C1 Hg1 Cl2 93.44(19) . . ? Cl1 Hg1 Cl2 82.74(6) . . ? C11 Hg1 Cl2 138.35(13) . . ? B1 Hg1 Cl2 158.97(16) . . ? C31 Hg2 Cl2 174.46(19) . . ? C31 Hg2 C41 86.6(2) . . ? Cl2 Hg2 C41 98.75(15) . . ? C31 Hg2 B2 72.2(2) . . ? Cl2 Hg2 B2 113.23(15) . . ? C41 Hg2 B2 28.54(19) . . ? C31 Hg2 Cl1 95.99(18) . . ? Cl2 Hg2 Cl1 79.02(5) . . ? C41 Hg2 Cl1 140.00(13) . . ? B2 Hg2 Cl1 161.26(15) . . ? Hg1 Cl1 Hg2 95.96(6) . . ? Hg2 Cl2 Hg1 101.37(6) . . ? C11 B1 C8 125.5(6) . . ? C11 B1 C21 120.5(7) . . ? C8 B1 C21 113.6(6) . . ? C11 B1 Hg1 70.2(3) . . ? C8 B1 Hg1 85.4(4) . . ? C21 B1 Hg1 124.4(5) . . ? C38 B2 C41 124.6(7) . . ? C38 B2 C51 115.9(6) . . ? C41 B2 C51 119.3(6) . . ? C38 B2 Hg2 83.1(4) . . ? C41 B2 Hg2 66.8(4) . . ? C51 B2 Hg2 128.2(5) . . ? C2 C1 C9 119.4(7) . . ? C2 C1 Hg1 115.4(5) . . ? C9 C1 Hg1 125.1(5) . . ? C1 C2 C3 122.2(7) . . ? C1 C2 H2A 118.9 . . ? C3 C2 H2A 118.9 . . ? C4 C3 C2 118.9(7) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C10 121.5(7) . . ? C3 C4 H4A 119.2 . . ? C10 C4 H4A 119.2 . . ? C6 C5 C10 120.7(7) . . ? C6 C5 H5A 119.7 . . ? C10 C5 H5A 119.7 . . ? C5 C6 C7 119.9(7) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C8 C7 C6 122.6(7) . . ? C8 C7 H7A 118.7 . . ? C6 C7 H7A 118.7 . . ? C7 C8 C9 117.3(7) . . ? C7 C8 B1 111.5(6) . . ? C9 C8 B1 131.0(6) . . ? C10 C9 C1 117.8(6) . . ? C10 C9 C8 119.1(6) . . ? C1 C9 C8 123.1(7) . . ? C4 C10 C9 120.1(7) . . ? C4 C10 C5 119.8(7) . . ? C9 C10 C5 120.2(7) . . ? C12 C11 C16 115.9(6) . . ? C12 C11 B1 123.3(7) . . ? C16 C11 B1 120.6(6) . . ? C12 C11 Hg1 98.5(4) . . ? C16 C11 Hg1 96.8(4) . . ? B1 C11 Hg1 80.9(4) . . ? C13 C12 C11 121.2(7) . . ? C13 C12 C17 114.6(7) . . ? C11 C12 C17 124.1(6) . . ? C14 C13 C12 121.9(7) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C15 C14 C13 117.9(7) . . ? C15 C14 C18 120.9(8) . . ? C13 C14 C18 121.2(7) . . ? C14 C15 C16 123.2(8) . . ? C14 C15 H15A 118.4 . . ? C16 C15 H15A 118.4 . . ? C15 C16 C11 119.8(7) . . ? C15 C16 C19 116.4(7) . . ? C11 C16 C19 123.9(6) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C26 C21 C22 121.7(6) . . ? C26 C21 B1 122.0(6) . . ? C22 C21 B1 116.3(6) . . ? C23 C22 C21 116.8(7) . . ? C23 C22 C27 118.8(6) . . ? C21 C22 C27 124.2(6) . . ? C24 C23 C22 122.6(7) . . ? C24 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? C23 C24 C25 118.1(7) . . ? C23 C24 C28 122.3(7) . . ? C25 C24 C28 119.7(7) . . ? C24 C25 C26 121.1(7) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C21 C26 C25 119.6(6) . . ? C21 C26 C29 123.2(7) . . ? C25 C26 C29 117.0(7) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C39 120.5(7) . . ? C32 C31 Hg2 114.4(5) . . ? C39 C31 Hg2 125.1(5) . . ? C33 C32 C31 122.2(7) . . ? C33 C32 H32A 118.9 . . ? C31 C32 H32A 118.9 . . ? C34 C33 C32 118.8(7) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C33 C34 C40 121.6(7) . . ? C33 C34 H34A 119.2 . . ? C40 C34 H34A 119.2 . . ? C36 C35 C40 120.3(7) . . ? C36 C35 H35A 119.8 . . ? C40 C35 H35A 119.8 . . ? C35 C36 C37 118.6(7) . . ? C35 C36 H36A 120.7 . . ? C37 C36 H36A 120.7 . . ? C38 C37 C36 124.9(7) . . ? C38 C37 H37A 117.6 . . ? C36 C37 H37A 117.6 . . ? C37 C38 C39 116.3(6) . . ? C37 C38 B2 112.7(6) . . ? C39 C38 B2 130.3(6) . . ? C31 C39 C40 116.3(6) . . ? C31 C39 C38 124.8(7) . . ? C40 C39 C38 118.8(6) . . ? C34 C40 C35 119.1(7) . . ? C34 C40 C39 120.2(6) . . ? C35 C40 C39 120.7(6) . . ? C42 C41 C46 116.6(6) . . ? C42 C41 B2 121.0(6) . . ? C46 C41 B2 121.8(7) . . ? C42 C41 Hg2 90.3(4) . . ? C46 C41 Hg2 103.4(4) . . ? B2 C41 Hg2 84.7(4) . . ? C43 C42 C41 121.2(7) . . ? C43 C42 C47 116.2(7) . . ? C41 C42 C47 122.6(6) . . ? C42 C43 C44 122.1(8) . . ? C42 C43 H43A 119.0 . . ? C44 C43 H43A 119.0 . . ? C45 C44 C43 117.6(7) . . ? C45 C44 C48 121.5(7) . . ? C43 C44 C48 120.9(8) . . ? C44 C45 C46 122.7(7) . . ? C44 C45 H45A 118.7 . . ? C46 C45 H45A 118.7 . . ? C45 C46 C41 119.8(7) . . ? C45 C46 C49 116.7(7) . . ? C41 C46 C49 123.4(7) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 120.4(7) . . ? C56 C51 B2 119.4(6) . . ? C52 C51 B2 120.2(7) . . ? C53 C52 C51 119.1(7) . . ? C53 C52 C57 119.5(6) . . ? C51 C52 C57 121.3(7) . . ? C52 C53 C54 122.4(7) . . ? C52 C53 H53A 118.8 . . ? C54 C53 H53A 118.8 . . ? C55 C54 C53 117.6(7) . . ? C55 C54 C58 121.9(8) . . ? C53 C54 C58 120.5(7) . . ? C54 C55 C56 120.4(7) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C51 C56 C55 120.2(7) . . ? C51 C56 C59 124.9(7) . . ? C55 C56 C59 114.7(7) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C66 C61 C62 120.5(9) . . ? C66 C61 H61A 119.8 . . ? C62 C61 H61A 119.8 . . ? C63 C62 C61 119.8(9) . . ? C63 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? C62 C63 C64 118.9(10) . . ? C62 C63 H63A 120.5 . . ? C64 C63 H63A 120.5 . . ? C65 C64 C63 120.5(10) . . ? C65 C64 H64A 119.8 . . ? C63 C64 H64A 119.8 . . ? C66 C65 C64 119.5(9) . . ? C66 C65 H65A 120.2 . . ? C64 C65 H65A 120.2 . . ? C61 C66 C65 120.8(9) . . ? C61 C66 H66A 119.6 . . ? C65 C66 H66A 119.6 . . ? C76 C71 C72 120.4(13) . . ? C76 C71 H71A 119.8 . . ? C72 C71 H71A 119.8 . . ? C73 C72 C71 121.0(12) . . ? C73 C72 H72A 119.5 . . ? C71 C72 H72A 119.5 . . ? C74 C73 C72 118.7(11) . . ? C74 C73 H73A 120.7 . . ? C72 C73 H73A 120.7 . . ? C73 C74 C75 121.9(10) . . ? C73 C74 H74A 119.0 . . ? C75 C74 H74A 119.0 . . ? C74 C75 C76 118.7(11) . . ? C74 C75 H75A 120.6 . . ? C76 C75 H75A 120.6 . . ? C71 C76 C75 119.1(13) . . ? C71 C76 H76A 120.5 . . ? C75 C76 H76A 120.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.597 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.249