Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Francois Gabbai' 'Mason R. Haneline' 'Julie B. King' _publ_contact_author_name 'Dr Francois Gabbai' _publ_contact_author_address ; Chemistry TAMU 3255 Texas A&M University College Station Texas 77843-3255 UNITED STATES OF AMERICA ; _publ_contact_author_email FRANCOIS@TAMU.EDU _publ_section_title ; Methyl Substituted Benzene Adducts of Trimeric Perfluoro-o-phenylene Mercury ; data_compound_2 _database_code_CSD 208162 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (o-C6F4Hg)3-(CH3)(C6H5) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H8 F12 Hg3' _chemical_formula_weight 1138.08 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' F F 0.0171 0.0103 '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)/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 9.514(2) _cell_length_b 7.4205(19) _cell_length_c 35.267(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.550(4) _cell_angle_gamma 90.00 _cell_volume 2485.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 18.592 _exptl_absorpt_correction_type Emperical _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21172 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3906 _reflns_number_gt 3028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0700P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3906 _refine_ls_number_parameters 361 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 0.997 _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 -0.76004(5) -0.02106(7) 0.184356(14) 0.03491(18) Uani 1 1 d . . . Hg2 Hg -0.94449(6) 0.13532(8) 0.098726(14) 0.03856(19) Uani 1 1 d . . . Hg3 Hg -0.61543(6) -0.09703(7) 0.094788(14) 0.03737(19) Uani 1 1 d . . . F3 F -0.3163(10) -0.2784(14) 0.1118(2) 0.071(3) Uani 1 1 d . . . F4 F -0.1638(9) -0.3414(13) 0.1767(3) 0.064(3) Uani 1 1 d . . . F5 F -0.2644(9) -0.2533(12) 0.2448(2) 0.058(2) Uani 1 1 d . . . F6 F -0.5162(8) -0.1012(12) 0.2473(2) 0.052(2) Uani 1 1 d . . . F9 F -0.9744(9) 0.0099(11) 0.2492(2) 0.052(2) Uani 1 1 d . . . F10 F -1.2284(9) 0.1625(12) 0.2513(2) 0.056(2) Uani 1 1 d . . . F11 F -1.3610(9) 0.3006(14) 0.1874(2) 0.067(3) Uani 1 1 d . . . F12 F -1.2366(10) 0.2809(14) 0.1209(2) 0.071(3) Uani 1 1 d . . . F15 F -1.0186(9) 0.2876(13) 0.0156(3) 0.061(2) Uani 1 1 d . . . F16 F -0.9077(10) 0.2224(14) -0.0509(2) 0.072(3) Uani 1 1 d . . . F17 F -0.6915(12) -0.0128(15) -0.0550(3) 0.077(3) Uani 1 1 d . . . F18 F -0.5718(10) -0.1616(13) 0.0088(2) 0.062(3) Uani 1 1 d . . . C1 C -0.5558(14) -0.1107(17) 0.1801(4) 0.034(3) Uani 1 1 d U . . C2 C -0.5041(14) -0.1515(17) 0.1451(4) 0.034(3) Uani 1 1 d U . . C3 C -0.3702(14) -0.2308(17) 0.1454(4) 0.036(3) Uani 1 1 d U . . C4 C -0.2932(14) -0.2671(19) 0.1777(4) 0.039(3) Uani 1 1 d U . . C5 C -0.3441(13) -0.2227(19) 0.2120(4) 0.040(3) Uani 1 1 d U . . C6 C -0.4690(13) -0.1446(19) 0.2141(4) 0.034(3) Uani 1 1 d U . . C7 C -1.0351(14) 0.1406(18) 0.1498(4) 0.036(3) Uani 1 1 d U . . C8 C -0.9660(14) 0.0667(18) 0.1832(4) 0.034(3) Uani 1 1 d U . . C9 C -1.0328(14) 0.0798(19) 0.2169(4) 0.037(3) Uani 1 1 d U . . C10 C -1.1638(15) 0.1560(19) 0.2187(4) 0.039(3) Uani 1 1 d U . . C11 C -1.2303(15) 0.2226(19) 0.1855(4) 0.040(3) Uani 1 1 d U . . C12 C -1.1651(15) 0.214(2) 0.1529(4) 0.041(3) Uani 1 1 d U . . C13 C -0.7328(15) -0.0114(18) 0.0463(4) 0.037(3) Uani 1 1 d U . . C14 C -0.8481(15) 0.0997(19) 0.0483(4) 0.037(3) Uani 1 1 d U . . C15 C -0.9069(16) 0.180(2) 0.0156(4) 0.043(3) Uani 1 1 d U . . C16 C -0.8552(16) 0.146(2) -0.0191(4) 0.044(3) Uani 1 1 d U . . C17 C -0.7433(16) 0.030(2) -0.0210(4) 0.045(3) Uani 1 1 d U . . C18 C -0.6857(16) -0.047(2) 0.0115(4) 0.041(3) Uani 1 1 d U . . C01 C -0.6697(19) 0.461(2) 0.0911(5) 0.059(3) Uani 1 1 d U . . C02 C -0.6211(19) 0.407(2) 0.1255(5) 0.063(4) Uani 1 1 d U . . H02A H -0.5357 0.3461 0.1283 0.076 Uiso 1 1 calc R . . C03 C -0.6988(19) 0.443(2) 0.1581(6) 0.067(4) Uani 1 1 d U . . H03A H -0.6633 0.4095 0.1822 0.080 Uiso 1 1 calc R . . C04 C -0.826(2) 0.526(2) 0.1529(6) 0.067(4) Uani 1 1 d U . . H04A H -0.8782 0.5481 0.1738 0.080 Uiso 1 1 calc R . . C05 C -0.879(2) 0.578(2) 0.1179(5) 0.064(4) Uani 1 1 d U . . H05A H -0.9668 0.6337 0.1154 0.077 Uiso 1 1 calc R . . C06 C -0.8048(18) 0.549(2) 0.0860(5) 0.060(3) Uani 1 1 d U . . H06A H -0.8405 0.5854 0.0621 0.072 Uiso 1 1 calc R . . C07 C -0.583(2) 0.434(3) 0.0562(6) 0.081(5) Uani 1 1 d U . . H07A H -0.4959 0.3751 0.0638 0.122 Uiso 1 1 calc R . . H07B H -0.5633 0.5495 0.0453 0.122 Uiso 1 1 calc R . . H07C H -0.6351 0.3617 0.0377 0.122 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 0.0348(3) 0.0391(3) 0.0302(3) 0.0012(2) -0.0030(2) -0.0016(2) Hg2 0.0472(4) 0.0400(3) 0.0279(3) 0.0012(2) -0.0015(2) -0.0024(3) Hg3 0.0520(4) 0.0343(3) 0.0251(3) 0.0028(2) -0.0033(2) 0.0007(3) F3 0.079(7) 0.081(7) 0.055(6) 0.001(5) 0.024(5) 0.034(6) F4 0.049(6) 0.077(7) 0.067(6) 0.008(5) 0.008(5) 0.034(5) F5 0.050(5) 0.075(7) 0.047(5) 0.012(5) -0.014(4) 0.012(5) F6 0.041(5) 0.083(7) 0.034(5) 0.010(4) 0.009(4) 0.006(4) F9 0.052(5) 0.070(6) 0.032(4) 0.009(4) -0.009(4) 0.004(4) F10 0.066(6) 0.070(6) 0.032(5) -0.003(4) 0.010(4) 0.014(5) F11 0.049(6) 0.099(8) 0.052(5) -0.010(5) -0.003(4) 0.029(5) F12 0.069(6) 0.097(8) 0.047(5) 0.010(5) -0.007(5) 0.033(6) F15 0.047(5) 0.077(7) 0.059(6) 0.019(5) 0.001(4) 0.012(5) F16 0.085(7) 0.099(8) 0.031(5) 0.028(5) -0.013(5) -0.007(6) F17 0.101(8) 0.094(8) 0.038(5) 0.008(5) 0.023(5) 0.008(6) F18 0.080(7) 0.068(6) 0.039(5) -0.007(4) 0.013(5) 0.007(5) C1 0.035(6) 0.035(6) 0.031(5) 0.009(5) -0.007(5) -0.008(5) C2 0.041(6) 0.031(6) 0.030(5) 0.004(5) 0.004(5) -0.003(5) C3 0.045(6) 0.034(6) 0.030(5) 0.005(5) 0.006(5) 0.001(5) C4 0.035(6) 0.042(6) 0.039(6) 0.012(5) 0.000(5) 0.005(5) C5 0.027(6) 0.050(6) 0.041(6) 0.017(5) -0.002(5) 0.001(5) C6 0.024(5) 0.044(6) 0.036(6) 0.016(5) 0.007(5) -0.004(5) C7 0.033(6) 0.040(6) 0.035(6) -0.002(5) 0.006(5) 0.000(5) C8 0.030(6) 0.040(6) 0.033(5) 0.000(5) 0.002(5) -0.007(5) C9 0.031(6) 0.039(6) 0.039(6) 0.000(5) -0.007(5) -0.008(5) C10 0.043(6) 0.037(6) 0.038(6) -0.004(5) 0.002(5) 0.001(5) C11 0.046(6) 0.039(6) 0.034(6) -0.001(5) -0.012(5) 0.006(5) C12 0.042(6) 0.047(6) 0.032(6) -0.001(5) -0.012(5) 0.009(5) C13 0.041(6) 0.038(6) 0.031(5) 0.005(5) -0.002(5) -0.008(5) C14 0.040(6) 0.045(6) 0.026(5) 0.008(5) 0.003(5) -0.010(5) C15 0.043(6) 0.051(6) 0.035(6) 0.008(5) -0.007(5) -0.013(6) C16 0.049(6) 0.050(6) 0.033(6) 0.017(5) -0.005(5) -0.009(5) C17 0.055(7) 0.053(7) 0.025(5) 0.003(5) -0.002(5) -0.008(6) C18 0.048(6) 0.043(6) 0.032(5) 0.002(5) 0.000(5) -0.006(5) C01 0.067(7) 0.033(6) 0.078(7) 0.003(6) -0.006(6) -0.010(6) C02 0.064(8) 0.043(7) 0.081(8) 0.004(7) -0.019(7) -0.005(6) C03 0.073(8) 0.049(7) 0.073(8) 0.009(7) -0.029(7) -0.016(6) C04 0.072(8) 0.051(7) 0.075(8) 0.002(7) -0.013(7) -0.017(6) C05 0.065(8) 0.047(7) 0.079(8) 0.013(7) -0.010(7) -0.005(6) C06 0.061(7) 0.039(6) 0.079(8) 0.010(6) -0.005(6) -0.006(6) C07 0.093(13) 0.057(10) 0.095(13) -0.011(10) 0.017(11) -0.017(10) _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 C8 2.063(13) . ? Hg1 C1 2.069(14) . ? Hg2 C7 2.046(13) . ? Hg2 C14 2.067(13) . ? Hg3 C2 2.049(13) . ? Hg3 C13 2.084(13) . ? Hg3 C01 4.173(16) . ? Hg3 C06 5.125(16) . ? F3 C3 1.364(15) . ? F4 C4 1.352(15) . ? F5 C5 1.361(14) . ? F6 C6 1.319(15) . ? F9 C9 1.341(15) . ? F10 C10 1.338(16) . ? F11 C11 1.377(16) . ? F12 C12 1.373(15) . ? F15 C15 1.327(17) . ? F16 C16 1.326(15) . ? F17 C17 1.360(17) . ? F18 C18 1.384(17) . ? C1 C2 1.389(18) . ? C1 C6 1.436(17) . ? C2 C3 1.403(18) . ? C3 C4 1.344(17) . ? C4 C5 1.371(19) . ? C5 C6 1.328(18) . ? C7 C12 1.363(19) . ? C7 C8 1.422(18) . ? C8 C9 1.385(19) . ? C9 C10 1.373(19) . ? C10 C11 1.385(18) . ? C11 C12 1.34(2) . ? C13 C18 1.36(2) . ? C13 C14 1.38(2) . ? C14 C15 1.387(18) . ? C15 C16 1.37(2) . ? C16 C17 1.38(2) . ? C17 C18 1.366(19) . ? C01 C02 1.33(2) . ? C01 C06 1.44(2) . ? C01 C07 1.54(3) . ? C02 C03 1.43(3) . ? C03 C04 1.36(2) . ? C04 C05 1.36(2) . ? C05 C06 1.38(2) . ? 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 C8 Hg1 C1 174.6(5) . . ? C7 Hg2 C14 173.5(6) . . ? C2 Hg3 C13 173.2(5) . . ? C2 Hg3 C01 106.2(4) . . ? C13 Hg3 C01 67.2(4) . . ? C2 Hg3 C06 113.4(4) . . ? C13 Hg3 C06 59.8(4) . . ? C01 Hg3 C06 13.5(3) . . ? C2 C1 C6 119.2(12) . . ? C2 C1 Hg1 121.4(9) . . ? C6 C1 Hg1 119.3(10) . . ? C1 C2 C3 117.1(11) . . ? C1 C2 Hg3 122.2(10) . . ? C3 C2 Hg3 120.6(9) . . ? C4 C3 F3 118.0(12) . . ? C4 C3 C2 122.5(12) . . ? F3 C3 C2 119.5(11) . . ? C3 C4 F4 120.6(13) . . ? C3 C4 C5 119.8(13) . . ? F4 C4 C5 119.6(11) . . ? C6 C5 F5 118.7(13) . . ? C6 C5 C4 121.3(12) . . ? F5 C5 C4 120.0(12) . . ? F6 C6 C5 120.7(12) . . ? F6 C6 C1 119.3(12) . . ? C5 C6 C1 120.0(13) . . ? C12 C7 C8 117.8(12) . . ? C12 C7 Hg2 120.7(10) . . ? C8 C7 Hg2 121.5(10) . . ? C9 C8 C7 117.9(12) . . ? C9 C8 Hg1 119.4(9) . . ? C7 C8 Hg1 121.9(10) . . ? F9 C9 C10 116.7(13) . . ? F9 C9 C8 120.9(12) . . ? C10 C9 C8 122.3(12) . . ? F10 C10 C9 121.4(12) . . ? F10 C10 C11 120.2(13) . . ? C9 C10 C11 118.4(13) . . ? C12 C11 F11 121.7(12) . . ? C12 C11 C10 119.8(13) . . ? F11 C11 C10 118.5(13) . . ? C11 C12 C7 123.7(12) . . ? C11 C12 F12 117.2(12) . . ? C7 C12 F12 119.0(13) . . ? C18 C13 C14 118.2(12) . . ? C18 C13 Hg3 119.5(11) . . ? C14 C13 Hg3 121.8(10) . . ? C13 C14 C15 119.8(13) . . ? C13 C14 Hg2 121.3(10) . . ? C15 C14 Hg2 118.8(11) . . ? F15 C15 C16 116.1(12) . . ? F15 C15 C14 122.9(14) . . ? C16 C15 C14 120.9(15) . . ? F16 C16 C15 122.6(14) . . ? F16 C16 C17 118.5(14) . . ? C15 C16 C17 118.9(13) . . ? F17 C17 C18 119.5(14) . . ? F17 C17 C16 121.0(13) . . ? C18 C17 C16 119.5(14) . . ? C13 C18 C17 122.6(14) . . ? C13 C18 F18 119.0(12) . . ? C17 C18 F18 118.4(13) . . ? C02 C01 C06 120.3(19) . . ? C02 C01 C07 121.1(18) . . ? C06 C01 C07 118.6(16) . . ? C02 C01 Hg3 68.9(10) . . ? C06 C01 Hg3 124.2(10) . . ? C07 C01 Hg3 80.0(10) . . ? C01 C02 C03 120.7(18) . . ? C04 C03 C02 118.4(17) . . ? C05 C04 C03 122(2) . . ? C04 C05 C06 120.9(19) . . ? C05 C06 C01 117.8(17) . . ? C05 C06 Hg3 107.0(10) . . ? C01 C06 Hg3 42.4(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.681 _refine_diff_density_min -2.237 _refine_diff_density_rms 0.297 #===END data_compound_3 _database_code_CSD 208163 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (o-C6F4Hg)3-1,2(CH3)2(C6H4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H10 F12 Hg3' _chemical_formula_weight 1152.11 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' F F 0.0171 0.0103 '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 20.050(4) _cell_length_b 6.8569(14) _cell_length_c 20.158(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.23(3) _cell_angle_gamma 90.00 _cell_volume 2507.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 18.432 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.4031 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16191 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4385 _reflns_number_gt 3807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0690P)^2^+70.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4385 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _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 0.57181(2) -0.16378(6) -0.03931(2) 0.01932(13) Uani 1 1 d . . . Hg3 Hg 0.75781(2) -0.02012(6) 0.07927(2) 0.01714(13) Uani 1 1 d . . . Hg2 Hg 0.69039(2) 0.00392(6) -0.11797(2) 0.01664(13) Uani 1 1 d . . . F3 F 0.7730(3) -0.0653(10) 0.2431(3) 0.0264(14) Uani 1 1 d . . . F4 F 0.6816(4) -0.1979(10) 0.2983(3) 0.0276(15) Uani 1 1 d . . . F5 F 0.5450(4) -0.3285(10) 0.2074(3) 0.0277(15) Uani 1 1 d . . . F6 F 0.4989(4) -0.3126(11) 0.0605(3) 0.0316(16) Uani 1 1 d . . . F15 F 0.8222(4) 0.1304(10) -0.1506(3) 0.0270(14) Uani 1 1 d . . . F16 F 0.9642(4) 0.2254(11) -0.0646(4) 0.0361(17) Uani 1 1 d . . . F17 F 1.0165(4) 0.2041(11) 0.0839(4) 0.0333(16) Uani 1 1 d . . . F18 F 0.9269(4) 0.0970(11) 0.1461(3) 0.0312(15) Uani 1 1 d . . . F9 F 0.4181(3) -0.2553(10) -0.1675(3) 0.0277(14) Uani 1 1 d . . . F10 F 0.3638(3) -0.2089(10) -0.3145(3) 0.0284(15) Uani 1 1 d . . . F11 F 0.4507(4) -0.0724(11) -0.3764(3) 0.0313(15) Uani 1 1 d . . . F12 F 0.5941(4) 0.0156(10) -0.2908(4) 0.0286(15) Uani 1 1 d . . . C1 C 0.6121(6) -0.1752(16) 0.0739(5) 0.019(2) Uani 1 1 d . . . C2 C 0.6830(6) -0.1105(17) 0.1198(5) 0.021(2) Uani 1 1 d . . . C3 C 0.7050(6) -0.1213(16) 0.1955(5) 0.019(2) Uani 1 1 d . . . C4 C 0.6584(6) -0.1879(17) 0.2254(6) 0.023(2) Uani 1 1 d . . . C5 C 0.5898(6) -0.2565(16) 0.1789(6) 0.020(2) Uani 1 1 d . . . C6 C 0.5679(6) -0.2461(17) 0.1040(6) 0.026(2) Uani 1 1 d . . . C13 C 0.8257(6) 0.0579(16) 0.0296(6) 0.019(2) Uani 1 1 d . . . C14 C 0.7984(5) 0.0609(17) -0.0469(5) 0.019(2) Uani 1 1 d . . . C15 C 0.8467(6) 0.1213(15) -0.0758(6) 0.020(2) Uani 1 1 d . . . C16 C 0.9185(6) 0.1707(16) -0.0349(6) 0.024(2) Uani 1 1 d . . . C17 C 0.9460(6) 0.1629(15) 0.0405(7) 0.024(2) Uani 1 1 d . . . C18 C 0.8982(6) 0.1048(16) 0.0706(5) 0.020(2) Uani 1 1 d . . . C7 C 0.5811(6) -0.0653(16) -0.1820(6) 0.021(2) Uani 1 1 d . . . C8 C 0.5348(6) -0.1365(16) -0.1514(6) 0.020(2) Uani 1 1 d . . . C9 C 0.4640(6) -0.1872(16) -0.1964(6) 0.020(2) Uani 1 1 d . . . C10 C 0.4342(6) -0.1647(16) -0.2723(6) 0.020(2) Uani 1 1 d . . . C11 C 0.4789(6) -0.0939(17) -0.3032(5) 0.023(2) Uani 1 1 d . . . C12 C 0.5510(6) -0.0468(16) -0.2583(6) 0.020(2) Uani 1 1 d . . . C01 C 0.6748(7) -0.5143(15) -0.1362(7) 0.022(2) Uani 1 1 d . . . C02 C 0.7474(7) -0.4469(16) -0.1032(7) 0.030(3) Uani 1 1 d . . . C03 C 0.7816(7) -0.4430(18) -0.0271(7) 0.033(3) Uani 1 1 d . . . H03A H 0.8304 -0.4020 -0.0044 0.039 Uiso 1 1 calc R . . C04 C 0.7472(8) -0.4967(17) 0.0171(7) 0.034(3) Uani 1 1 d . . . H04A H 0.7721 -0.4906 0.0679 0.041 Uiso 1 1 calc R . . C05 C 0.6746(7) -0.5597(18) -0.0167(7) 0.032(3) Uani 1 1 d . . . H05A H 0.6499 -0.5953 0.0114 0.038 Uiso 1 1 calc R . . C06 C 0.6395(6) -0.5693(16) -0.0917(6) 0.023(2) Uani 1 1 d . . . H06A H 0.5910 -0.6134 -0.1138 0.028 Uiso 1 1 calc R . . C07 C 0.6348(8) -0.5321(18) -0.2177(7) 0.037(3) Uani 1 1 d . . . H07A H 0.6662 -0.4890 -0.2398 0.056 Uiso 1 1 calc R . . H07B H 0.5911 -0.4531 -0.2350 0.056 Uiso 1 1 calc R . . H07C H 0.6213 -0.6659 -0.2306 0.056 Uiso 1 1 calc R . . C08 C 0.7876(8) -0.393(2) -0.1484(9) 0.044(3) Uani 1 1 d . . . H08A H 0.8365 -0.3497 -0.1167 0.066 Uiso 1 1 calc R . . H08B H 0.7617 -0.2893 -0.1815 0.066 Uiso 1 1 calc R . . H08C H 0.7904 -0.5040 -0.1759 0.066 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 0.0221(2) 0.0259(2) 0.0119(2) 0.00124(15) 0.00899(16) 0.00060(16) Hg3 0.0199(2) 0.0224(2) 0.0116(2) 0.00052(14) 0.00910(17) 0.00011(15) Hg2 0.0191(2) 0.0205(2) 0.0114(2) 0.00031(14) 0.00749(17) 0.00096(15) F3 0.024(3) 0.039(4) 0.011(3) -0.001(3) 0.002(3) -0.010(3) F4 0.033(4) 0.038(4) 0.013(3) 0.002(3) 0.011(3) 0.003(3) F5 0.032(4) 0.039(4) 0.020(3) 0.002(3) 0.018(3) -0.006(3) F6 0.024(3) 0.055(5) 0.020(3) -0.002(3) 0.014(3) -0.010(3) F15 0.036(4) 0.032(4) 0.016(3) -0.001(3) 0.014(3) -0.003(3) F16 0.034(4) 0.045(4) 0.039(4) 0.003(3) 0.025(3) -0.004(3) F17 0.024(3) 0.041(4) 0.034(4) -0.006(3) 0.012(3) -0.002(3) F18 0.027(3) 0.046(4) 0.018(3) -0.006(3) 0.007(3) -0.006(3) F9 0.024(3) 0.034(4) 0.026(3) 0.001(3) 0.012(3) -0.001(3) F10 0.025(3) 0.042(4) 0.014(3) 0.001(3) 0.004(3) -0.005(3) F11 0.031(4) 0.046(4) 0.009(3) 0.002(3) 0.002(3) -0.003(3) F12 0.033(4) 0.040(4) 0.019(3) 0.001(3) 0.017(3) 0.000(3) C1 0.023(5) 0.025(6) 0.010(5) 0.001(4) 0.009(4) -0.002(4) C2 0.022(5) 0.034(6) 0.009(5) -0.003(4) 0.009(4) 0.005(5) C3 0.018(5) 0.020(5) 0.015(5) 0.001(4) 0.005(4) 0.004(4) C4 0.035(6) 0.030(6) 0.013(5) 0.004(4) 0.018(5) 0.007(5) C5 0.030(6) 0.021(6) 0.021(5) 0.000(4) 0.022(5) -0.006(5) C6 0.030(6) 0.027(6) 0.025(6) 0.004(5) 0.015(5) 0.006(5) C13 0.020(5) 0.019(5) 0.022(5) -0.003(4) 0.013(5) 0.002(4) C14 0.014(5) 0.031(6) 0.009(5) -0.002(4) 0.002(4) 0.014(5) C15 0.033(6) 0.014(5) 0.016(5) 0.002(4) 0.013(5) -0.003(4) C16 0.031(6) 0.022(6) 0.034(6) 0.002(5) 0.026(5) 0.000(5) C17 0.022(5) 0.015(6) 0.040(7) -0.007(5) 0.016(5) -0.002(4) C18 0.023(5) 0.027(6) 0.009(5) 0.003(4) 0.006(4) 0.000(5) C7 0.024(6) 0.016(5) 0.029(6) 0.012(4) 0.016(5) 0.010(4) C8 0.019(5) 0.022(6) 0.017(5) -0.007(4) 0.006(4) 0.001(4) C9 0.026(6) 0.024(6) 0.013(5) 0.001(4) 0.012(4) 0.002(4) C10 0.014(5) 0.027(6) 0.013(5) -0.004(4) -0.001(4) -0.001(4) C11 0.038(6) 0.026(6) 0.007(5) -0.002(4) 0.013(5) -0.003(5) C12 0.019(5) 0.019(5) 0.024(6) 0.001(4) 0.010(5) 0.002(4) C01 0.032(6) 0.012(5) 0.029(6) -0.001(4) 0.019(5) 0.007(4) C02 0.037(7) 0.009(5) 0.053(8) -0.001(5) 0.027(6) -0.004(5) C03 0.036(7) 0.019(6) 0.043(8) 0.005(5) 0.016(6) 0.008(5) C04 0.049(8) 0.024(7) 0.017(6) -0.003(4) 0.001(6) 0.008(5) C05 0.051(8) 0.027(6) 0.027(6) 0.005(5) 0.026(6) 0.012(6) C06 0.028(6) 0.020(6) 0.030(6) -0.003(5) 0.020(5) 0.000(5) C07 0.054(9) 0.023(6) 0.039(7) 0.000(5) 0.024(7) 0.006(6) C08 0.055(9) 0.027(7) 0.069(10) 0.003(7) 0.045(8) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C8 2.065(10) . ? Hg1 C1 2.072(10) . ? Hg1 C05 3.321(12) . ? Hg1 C06 3.451(11) . ? Hg3 C13 2.075(10) . ? Hg3 C2 2.086(10) . ? Hg3 C04 3.474(11) . ? Hg2 C14 2.062(10) . ? Hg2 C7 2.070(11) . ? Hg2 C02 3.265(11) . ? F3 C3 1.347(12) . ? F4 C4 1.341(12) . ? F5 C5 1.350(11) . ? F6 C6 1.362(14) . ? F15 C15 1.375(12) . ? F16 C16 1.343(12) . ? F17 C17 1.337(13) . ? F18 C18 1.379(11) . ? F9 C9 1.364(12) . ? F10 C10 1.336(12) . ? F11 C11 1.344(12) . ? F12 C12 1.358(12) . ? C1 C6 1.360(15) . ? C1 C2 1.397(15) . ? C2 C3 1.398(14) . ? C3 C4 1.386(15) . ? C4 C5 1.375(16) . ? C5 C6 1.383(15) . ? C13 C18 1.369(15) . ? C13 C14 1.400(14) . ? C14 C15 1.390(15) . ? C15 C16 1.362(16) . ? C16 C17 1.379(17) . ? C17 C18 1.394(15) . ? C7 C12 1.397(15) . ? C7 C8 1.401(15) . ? C8 C9 1.365(15) . ? C9 C10 1.394(14) . ? C10 C11 1.379(15) . ? C11 C12 1.377(16) . ? C01 C02 1.396(17) . ? C01 C06 1.411(16) . ? C01 C07 1.495(18) . ? C02 C03 1.388(19) . ? C02 C08 1.497(17) . ? C03 C04 1.390(19) . ? C04 C05 1.39(2) . ? C05 C06 1.370(17) . ? 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 C8 Hg1 C1 176.6(4) . . ? C8 Hg1 C05 97.8(4) . . ? C1 Hg1 C05 83.7(4) . . ? C8 Hg1 C06 75.1(3) . . ? C1 Hg1 C06 106.7(4) . . ? C05 Hg1 C06 23.2(3) . . ? C13 Hg3 C2 174.6(4) . . ? C13 Hg3 C04 91.2(4) . . ? C2 Hg3 C04 85.3(4) . . ? C14 Hg2 C7 175.1(4) . . ? C14 Hg2 C02 83.9(4) . . ? C7 Hg2 C02 94.4(4) . . ? C6 C1 C2 119.3(9) . . ? C6 C1 Hg1 118.9(8) . . ? C2 C1 Hg1 121.8(7) . . ? C1 C2 C3 117.7(9) . . ? C1 C2 Hg3 122.2(7) . . ? C3 C2 Hg3 119.9(8) . . ? F3 C3 C4 116.8(9) . . ? F3 C3 C2 121.0(9) . . ? C4 C3 C2 122.3(10) . . ? F4 C4 C5 120.5(9) . . ? F4 C4 C3 120.7(10) . . ? C5 C4 C3 118.7(9) . . ? F5 C5 C4 119.3(9) . . ? F5 C5 C6 121.6(10) . . ? C4 C5 C6 119.1(9) . . ? C1 C6 F6 120.5(10) . . ? C1 C6 C5 122.8(11) . . ? F6 C6 C5 116.7(10) . . ? C18 C13 C14 118.6(10) . . ? C18 C13 Hg3 121.0(8) . . ? C14 C13 Hg3 120.4(8) . . ? C15 C14 C13 116.8(10) . . ? C15 C14 Hg2 118.6(7) . . ? C13 C14 Hg2 124.4(8) . . ? C16 C15 F15 116.3(9) . . ? C16 C15 C14 124.5(10) . . ? F15 C15 C14 119.1(9) . . ? F16 C16 C15 123.1(10) . . ? F16 C16 C17 118.2(10) . . ? C15 C16 C17 118.7(10) . . ? F17 C17 C16 121.8(10) . . ? F17 C17 C18 120.4(10) . . ? C16 C17 C18 117.8(10) . . ? C13 C18 F18 119.6(9) . . ? C13 C18 C17 123.6(10) . . ? F18 C18 C17 116.8(9) . . ? C12 C7 C8 117.3(10) . . ? C12 C7 Hg2 120.7(8) . . ? C8 C7 Hg2 121.9(8) . . ? C9 C8 C7 119.5(10) . . ? C9 C8 Hg1 119.4(8) . . ? C7 C8 Hg1 121.1(8) . . ? F9 C9 C8 120.2(9) . . ? F9 C9 C10 117.1(9) . . ? C8 C9 C10 122.6(10) . . ? F10 C10 C11 120.4(9) . . ? F10 C10 C9 121.1(10) . . ? C11 C10 C9 118.5(10) . . ? F11 C11 C12 121.9(10) . . ? F11 C11 C10 118.9(10) . . ? C12 C11 C10 119.2(9) . . ? F12 C12 C11 117.5(9) . . ? F12 C12 C7 119.7(9) . . ? C11 C12 C7 122.8(10) . . ? C02 C01 C06 119.3(11) . . ? C02 C01 C07 120.8(11) . . ? C06 C01 C07 119.8(11) . . ? C03 C02 C01 117.1(11) . . ? C03 C02 C08 121.7(12) . . ? C01 C02 C08 121.0(12) . . ? C03 C02 Hg2 94.1(7) . . ? C01 C02 Hg2 91.0(7) . . ? C08 C02 Hg2 88.1(7) . . ? C02 C03 C04 123.9(12) . . ? C05 C04 C03 118.1(11) . . ? C05 C04 Hg3 111.2(8) . . ? C03 C04 Hg3 90.6(7) . . ? C06 C05 C04 119.8(11) . . ? C06 C05 Hg1 83.7(7) . . ? C04 C05 Hg1 105.8(8) . . ? C05 C06 C01 121.8(11) . . ? C05 C06 Hg1 73.0(7) . . ? C01 C06 Hg1 110.4(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.019 _refine_diff_density_min -2.832 _refine_diff_density_rms 0.365 #===END data_compound_4 _database_code_CSD 208164 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (o-C6F4Hg)3-1,3(CH3)2(C6H4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H10 F12 Hg3' _chemical_formula_weight 1152.11 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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 15.923(3) _cell_length_b 21.678(4) _cell_length_c 7.2192(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2491.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.540 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 18.544 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.326298 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19871 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.29 _reflns_number_total 3573 _reflns_number_gt 3443 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0272P)^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 mixed _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 -0.001(9) _refine_ls_number_reflns 3573 _refine_ls_number_parameters 370 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0498 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.81751(2) 0.702789(17) 0.37655(5) 0.03005(10) Uani 1 1 d . . . Hg2 Hg 0.680606(19) 0.578159(16) 0.50978(5) 0.02849(10) Uani 1 1 d . . . Hg3 Hg 0.617691(19) 0.736901(14) 0.56447(6) 0.02744(10) Uani 1 1 d . . . F3 F 0.6047(3) 0.8819(2) 0.5930(9) 0.0427(14) Uani 1 1 d . . . F4 F 0.7055(4) 0.9730(2) 0.4756(10) 0.0546(18) Uani 1 1 d . . . F5 F 0.8503(4) 0.9476(3) 0.2973(10) 0.0559(18) Uani 1 1 d . . . F6 F 0.8990(4) 0.8288(3) 0.2486(9) 0.0584(18) Uani 1 1 d . . . F9 F 0.9910(3) 0.6466(2) 0.2880(9) 0.0478(15) Uani 1 1 d . . . F10 F 1.0531(3) 0.5301(3) 0.3056(8) 0.0480(15) Uani 1 1 d . . . F11 F 0.9548(3) 0.4370(2) 0.4132(9) 0.0489(16) Uani 1 1 d . . . F12 F 0.7915(3) 0.4564(3) 0.4972(9) 0.0509(16) Uani 1 1 d . . . F15 F 0.5191(3) 0.4978(2) 0.6016(9) 0.0417(15) Uani 1 1 d . . . F16 F 0.3706(3) 0.5251(3) 0.7505(9) 0.0436(15) Uani 1 1 d . . . F17 F 0.3321(3) 0.6445(3) 0.8329(9) 0.0451(16) Uani 1 1 d . . . F18 F 0.4395(3) 0.7354(2) 0.7416(9) 0.0468(16) Uani 1 1 d . . . C1 C 0.7765(5) 0.7924(4) 0.3964(14) 0.027(2) Uani 1 1 d . . . C2 C 0.6997(6) 0.8063(4) 0.4840(14) 0.032(2) Uani 1 1 d . . . C3 C 0.6771(5) 0.8674(4) 0.5086(15) 0.032(2) Uani 1 1 d . . . C4 C 0.7273(6) 0.9143(4) 0.4473(14) 0.037(3) Uani 1 1 d . . . C5 C 0.8008(6) 0.9014(4) 0.3579(16) 0.040(3) Uani 1 1 d . . . C6 C 0.8240(6) 0.8401(5) 0.3343(14) 0.037(3) Uani 1 1 d . . . C7 C 0.8048(5) 0.5634(4) 0.4349(13) 0.028(2) Uani 1 1 d . . . C8 C 0.8569(5) 0.6127(4) 0.3829(13) 0.030(2) Uani 1 1 d . . . C9 C 0.9390(6) 0.5992(5) 0.3388(13) 0.036(2) Uani 1 1 d . . . C10 C 0.9721(5) 0.5395(5) 0.3459(12) 0.033(2) Uani 1 1 d . . . C11 C 0.9216(6) 0.4938(4) 0.3990(14) 0.033(2) Uani 1 1 d . . . C12 C 0.8390(6) 0.5050(4) 0.4447(13) 0.031(2) Uani 1 1 d . . . C13 C 0.5394(5) 0.6640(4) 0.6293(11) 0.025(2) Uani 1 1 d . . . C14 C 0.5606(5) 0.6027(4) 0.5945(12) 0.029(2) Uani 1 1 d . . . C15 C 0.5021(5) 0.5580(4) 0.6368(13) 0.030(2) Uani 1 1 d . . . C16 C 0.4265(6) 0.5710(4) 0.7145(14) 0.031(2) Uani 1 1 d . . . C17 C 0.4064(5) 0.6309(5) 0.7547(13) 0.033(2) Uani 1 1 d . . . C18 C 0.4632(5) 0.6771(4) 0.7093(13) 0.030(2) Uani 1 1 d . . . C01 C 0.7532(6) 0.6536(4) -0.0451(12) 0.036(2) Uani 1 1 d . . . C02 C 0.7344(6) 0.7152(4) -0.0495(12) 0.028(2) Uani 1 1 d . . . H02A H 0.7745 0.7424 -0.0957 0.033 Uiso 1 1 calc R . . C03 C 0.6590(6) 0.7389(4) 0.0114(12) 0.028(2) Uani 1 1 d . . . C04 C 0.6001(6) 0.6982(4) 0.0842(15) 0.039(2) Uani 1 1 d . . . H04A H 0.5497 0.7130 0.1319 0.046 Uiso 1 1 calc R . . C05 C 0.6167(7) 0.6356(5) 0.0852(16) 0.049(3) Uani 1 1 d . . . H05A H 0.5764 0.6084 0.1297 0.059 Uiso 1 1 calc R . . C06 C 0.6921(7) 0.6130(4) 0.0212(16) 0.043(3) Uani 1 1 d . . . H06A H 0.7023 0.5708 0.0221 0.052 Uiso 1 1 calc R . . C07 C 0.8374(7) 0.6294(5) -0.1050(16) 0.048(3) Uani 1 1 d . . . H07A H 0.8716 0.6631 -0.1473 0.073 Uiso 1 1 calc R . . H07B H 0.8300 0.6003 -0.2037 0.073 Uiso 1 1 calc R . . H07C H 0.8644 0.6096 -0.0022 0.073 Uiso 1 1 calc R . . C08 C 0.6405(7) 0.8067(4) 0.0045(16) 0.044(3) Uani 1 1 d . . . H08A H 0.6873 0.8281 -0.0490 0.067 Uiso 1 1 calc R . . H08B H 0.6308 0.8217 0.1278 0.067 Uiso 1 1 calc R . . H08C H 0.5913 0.8137 -0.0696 0.067 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 0.0286(2) 0.0313(2) 0.0303(2) 0.00149(18) -0.00058(17) 0.00016(15) Hg2 0.02289(18) 0.0268(2) 0.0358(2) -0.00194(17) -0.00071(15) -0.00066(14) Hg3 0.02916(18) 0.02361(18) 0.02955(19) -0.00027(18) 0.00048(18) -0.00354(15) F3 0.047(3) 0.034(3) 0.047(4) -0.007(3) 0.007(3) 0.004(2) F4 0.054(3) 0.023(3) 0.087(5) 0.003(3) -0.017(4) -0.010(3) F5 0.043(3) 0.037(4) 0.087(5) 0.025(3) -0.005(3) -0.018(3) F6 0.037(3) 0.070(5) 0.069(5) 0.016(4) 0.014(3) -0.007(3) F9 0.029(3) 0.049(4) 0.066(4) 0.009(3) 0.009(3) 0.000(3) F10 0.027(3) 0.059(4) 0.058(4) -0.007(3) 0.006(3) 0.015(3) F11 0.045(3) 0.032(3) 0.069(4) -0.014(3) -0.009(3) 0.013(3) F12 0.042(3) 0.033(3) 0.078(4) 0.004(3) -0.003(3) -0.002(3) F15 0.036(3) 0.018(3) 0.072(4) 0.004(3) 0.005(3) -0.001(2) F16 0.029(3) 0.041(3) 0.061(4) 0.010(3) 0.004(3) -0.011(3) F17 0.027(3) 0.050(4) 0.059(4) 0.000(3) 0.010(3) 0.004(3) F18 0.048(4) 0.028(3) 0.064(4) -0.006(3) 0.016(3) 0.004(3) C1 0.036(5) 0.021(5) 0.025(5) -0.001(4) -0.002(5) 0.004(4) C2 0.041(6) 0.024(5) 0.032(6) 0.006(4) -0.016(5) -0.011(4) C3 0.032(5) 0.028(5) 0.035(5) -0.001(5) -0.009(4) -0.004(4) C4 0.041(6) 0.021(5) 0.049(7) 0.001(4) -0.018(5) -0.005(4) C5 0.038(6) 0.035(6) 0.047(7) 0.017(5) -0.008(5) -0.007(5) C6 0.031(6) 0.042(7) 0.037(7) 0.009(5) 0.003(4) 0.002(5) C7 0.025(5) 0.027(5) 0.032(5) -0.009(4) 0.001(4) -0.003(4) C8 0.021(5) 0.047(6) 0.023(5) 0.002(5) -0.007(4) 0.017(4) C9 0.028(5) 0.050(6) 0.029(6) 0.004(5) -0.003(4) -0.009(5) C10 0.027(5) 0.053(6) 0.018(5) -0.014(4) 0.002(4) 0.012(5) C11 0.035(5) 0.028(6) 0.037(6) -0.007(5) -0.008(5) 0.005(4) C12 0.028(5) 0.022(5) 0.042(6) 0.001(4) -0.004(4) 0.001(4) C13 0.027(5) 0.028(5) 0.021(5) 0.007(4) -0.001(4) -0.004(4) C14 0.026(5) 0.039(6) 0.023(5) 0.012(4) -0.001(4) -0.005(4) C15 0.036(6) 0.020(5) 0.034(6) 0.004(4) -0.005(4) 0.001(4) C16 0.023(5) 0.033(6) 0.037(6) 0.011(5) -0.009(4) -0.010(4) C17 0.017(5) 0.049(7) 0.033(6) 0.000(5) 0.001(4) 0.003(5) C18 0.033(5) 0.029(6) 0.029(5) 0.005(4) -0.008(5) -0.004(4) C01 0.048(6) 0.036(6) 0.025(5) 0.003(4) -0.012(4) 0.005(5) C02 0.033(5) 0.023(5) 0.027(5) 0.002(4) -0.001(4) -0.009(4) C03 0.032(5) 0.033(6) 0.019(5) 0.000(4) -0.004(4) 0.001(4) C04 0.032(5) 0.050(7) 0.034(6) 0.007(6) 0.006(5) 0.006(4) C05 0.065(7) 0.052(7) 0.030(6) 0.014(6) -0.006(6) -0.023(6) C06 0.070(8) 0.024(5) 0.036(6) 0.003(5) -0.015(6) -0.009(5) C07 0.068(7) 0.041(6) 0.036(6) 0.000(5) -0.004(6) 0.017(6) C08 0.052(6) 0.036(6) 0.046(7) 0.002(5) 0.007(5) 0.002(5) _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 C8 2.051(9) . ? Hg1 C1 2.054(8) . ? Hg1 C02 3.359(9) . ? Hg2 C7 2.076(8) . ? Hg2 C14 2.076(9) . ? Hg2 C05 3.462(11) . ? Hg3 C13 2.066(8) . ? Hg3 C2 2.075(9) . ? F3 C3 1.341(11) . ? F4 C4 1.334(10) . ? F5 C5 1.346(11) . ? F6 C6 1.367(11) . ? F9 C9 1.369(10) . ? F10 C10 1.337(9) . ? F11 C11 1.343(10) . ? F12 C12 1.352(10) . ? F15 C15 1.358(10) . ? F16 C16 1.358(10) . ? F17 C17 1.343(10) . ? F18 C18 1.340(10) . ? C1 C6 1.357(13) . ? C1 C2 1.410(13) . ? C2 C3 1.384(13) . ? C3 C4 1.367(13) . ? C4 C5 1.366(14) . ? C5 C6 1.390(14) . ? C7 C12 1.378(12) . ? C7 C8 1.405(13) . ? C8 C9 1.376(13) . ? C9 C10 1.399(13) . ? C10 C11 1.332(13) . ? C11 C12 1.377(13) . ? C13 C18 1.374(12) . ? C13 C14 1.393(12) . ? C14 C15 1.378(12) . ? C15 C16 1.358(13) . ? C16 C17 1.369(13) . ? C17 C18 1.389(13) . ? C01 C02 1.370(12) . ? C01 C06 1.395(13) . ? C01 C07 1.503(13) . ? C02 C03 1.377(12) . ? C03 C04 1.392(13) . ? C03 C08 1.500(12) . ? C04 C05 1.382(14) . ? C05 C06 1.376(15) . ? 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 C8 Hg1 C1 174.7(4) . . ? C8 Hg1 C02 102.6(3) . . ? C1 Hg1 C02 82.1(3) . . ? C7 Hg2 C14 173.6(3) . . ? C7 Hg2 C05 96.0(3) . . ? C14 Hg2 C05 84.2(3) . . ? C13 Hg3 C2 175.9(4) . . ? C6 C1 C2 117.9(8) . . ? C6 C1 Hg1 121.4(7) . . ? C2 C1 Hg1 120.6(7) . . ? C3 C2 C1 119.2(9) . . ? C3 C2 Hg3 119.6(7) . . ? C1 C2 Hg3 121.1(7) . . ? F3 C3 C4 118.4(8) . . ? F3 C3 C2 120.4(8) . . ? C4 C3 C2 121.2(9) . . ? F4 C4 C5 119.3(9) . . ? F4 C4 C3 120.5(9) . . ? C5 C4 C3 120.1(9) . . ? F5 C5 C4 120.2(9) . . ? F5 C5 C6 121.1(9) . . ? C4 C5 C6 118.7(9) . . ? C1 C6 F6 119.9(9) . . ? C1 C6 C5 122.8(9) . . ? F6 C6 C5 117.3(9) . . ? C12 C7 C8 118.6(8) . . ? C12 C7 Hg2 120.3(7) . . ? C8 C7 Hg2 121.0(6) . . ? C9 C8 C7 117.4(8) . . ? C9 C8 Hg1 119.2(7) . . ? C7 C8 Hg1 123.4(6) . . ? F9 C9 C8 118.5(9) . . ? F9 C9 C10 118.4(8) . . ? C8 C9 C10 123.1(9) . . ? C11 C10 F10 122.1(9) . . ? C11 C10 C9 118.1(8) . . ? F10 C10 C9 119.8(9) . . ? C10 C11 F11 117.7(8) . . ? C10 C11 C12 120.9(8) . . ? F11 C11 C12 121.4(8) . . ? F12 C12 C11 117.6(8) . . ? F12 C12 C7 120.6(8) . . ? C11 C12 C7 121.8(9) . . ? C18 C13 C14 119.1(8) . . ? C18 C13 Hg3 118.0(6) . . ? C14 C13 Hg3 122.8(6) . . ? C15 C14 C13 117.8(8) . . ? C15 C14 Hg2 120.5(7) . . ? C13 C14 Hg2 121.4(6) . . ? F15 C15 C16 116.9(8) . . ? F15 C15 C14 120.0(8) . . ? C16 C15 C14 123.1(8) . . ? C15 C16 F16 120.6(8) . . ? C15 C16 C17 119.4(8) . . ? F16 C16 C17 120.0(8) . . ? F17 C17 C16 120.2(9) . . ? F17 C17 C18 121.0(9) . . ? C16 C17 C18 118.8(8) . . ? F18 C18 C13 121.1(8) . . ? F18 C18 C17 117.1(8) . . ? C13 C18 C17 121.7(8) . . ? C02 C01 C06 118.1(9) . . ? C02 C01 C07 121.8(9) . . ? C06 C01 C07 120.1(9) . . ? C01 C02 C03 123.1(8) . . ? C01 C02 Hg1 79.3(5) . . ? C03 C02 Hg1 94.7(5) . . ? C02 C03 C04 118.1(8) . . ? C02 C03 C08 121.8(8) . . ? C04 C03 C08 120.0(8) . . ? C05 C04 C03 119.7(9) . . ? C06 C05 C04 121.0(10) . . ? C06 C05 Hg2 85.0(7) . . ? C04 C05 Hg2 114.5(8) . . ? C05 C06 C01 119.9(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.249 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.144 #===END data_compound_5 _database_code_CSD 208165 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (o-C6F4Hg)3-1,4(CH3)2(C6H4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H10 F12 Hg3' _chemical_formula_weight 1152.11 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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 16.854(3) _cell_length_b 20.891(4) _cell_length_c 7.1384(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2513.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 18.385 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.624366 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _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 'smart ccd' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15314 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3779 _reflns_number_gt 3301 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0800P)^2^+40.0000P] 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 mixed _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 -0.06(2) _refine_ls_number_reflns 3779 _refine_ls_number_parameters 370 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 0.987 _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 0.87827(4) 0.73096(3) 0.18529(14) 0.0275(2) Uani 1 1 d . . . Hg2 Hg 0.81807(4) 0.56618(4) 0.23362(12) 0.0273(2) Uani 1 1 d . . . Hg3 Hg 0.68520(4) 0.69484(4) 0.35862(10) 0.0268(2) Uani 1 1 d . . . F3 F 0.6106(6) 0.8272(6) 0.496(2) 0.045(4) Uani 1 1 d . . . F4 F 0.6578(7) 0.9491(6) 0.458(2) 0.040(3) Uani 1 1 d . . . F5 F 0.7994(7) 0.9759(5) 0.277(2) 0.051(4) Uani 1 1 d . . . F6 F 0.8903(6) 0.8808(4) 0.159(2) 0.034(3) Uani 1 1 d . . . F9 F 1.0543(7) 0.7291(6) 0.0426(19) 0.038(3) Uani 1 1 d . . . F10 F 1.1582(6) 0.6361(6) -0.032(2) 0.043(3) Uani 1 1 d . . . F11 F 1.1205(6) 0.5102(6) 0.0435(18) 0.036(3) Uani 1 1 d . . . F12 F 0.9736(6) 0.4827(5) 0.167(2) 0.039(3) Uani 1 1 d . . . F15 F 0.7151(7) 0.4380(5) 0.248(2) 0.042(3) Uani 1 1 d . . . F16 F 0.5600(7) 0.4154(5) 0.3013(19) 0.041(3) Uani 1 1 d . . . F17 F 0.4625(6) 0.5141(6) 0.3944(18) 0.040(3) Uani 1 1 d . . . F18 F 0.5187(6) 0.6332(6) 0.426(2) 0.044(3) Uani 1 1 d . . . C1 C 0.8019(10) 0.8066(9) 0.256(3) 0.0274(19) Uani 1 1 d U . . C2 C 0.7257(10) 0.7882(9) 0.349(3) 0.0274(19) Uani 1 1 d U . . C3 C 0.6833(11) 0.8387(10) 0.399(3) 0.0273(19) Uani 1 1 d U . . C4 C 0.7011(11) 0.9048(9) 0.393(3) 0.0273(19) Uani 1 1 d U . . C5 C 0.7750(11) 0.9168(10) 0.303(3) 0.0274(19) Uani 1 1 d U . . C6 C 0.8216(10) 0.8676(9) 0.243(3) 0.0274(19) Uani 1 1 d U . . C7 C 0.9315(10) 0.5910(8) 0.173(3) 0.0295(18) Uani 1 1 d U . . C8 C 0.9563(11) 0.6560(9) 0.127(3) 0.0294(18) Uani 1 1 d U . . C9 C 1.0293(11) 0.6699(9) 0.071(3) 0.0295(18) Uani 1 1 d U . . C10 C 1.0881(11) 0.6215(10) 0.036(3) 0.0295(18) Uani 1 1 d U . . C11 C 1.0653(11) 0.5608(9) 0.080(3) 0.0294(18) Uani 1 1 d U . . C12 C 0.9920(11) 0.5454(9) 0.134(3) 0.0294(18) Uani 1 1 d U . . C13 C 0.6467(12) 0.5988(10) 0.354(3) 0.0314(19) Uani 1 1 d U . . C14 C 0.6998(12) 0.5497(10) 0.297(3) 0.0314(19) Uani 1 1 d U . . C15 C 0.6717(12) 0.4884(10) 0.288(3) 0.0315(19) Uani 1 1 d U . . C16 C 0.5897(12) 0.4758(9) 0.317(3) 0.0315(19) Uani 1 1 d U . . C17 C 0.5399(11) 0.5255(9) 0.368(3) 0.0315(19) Uani 1 1 d U . . C18 C 0.5704(12) 0.5856(10) 0.383(3) 0.0315(19) Uani 1 1 d U . . C01 C 0.8656(11) 0.7184(10) -0.292(3) 0.0348(18) Uani 1 1 d U . . C02 C 0.8031(12) 0.7551(11) -0.218(3) 0.0349(18) Uani 1 1 d U . . H02A H 0.8091 0.7989 -0.1994 0.042 Uiso 1 1 calc R . . C03 C 0.7305(12) 0.7240(10) -0.174(3) 0.0350(18) Uani 1 1 d U . . H03A H 0.6880 0.7477 -0.1279 0.042 Uiso 1 1 calc R . . C04 C 0.7227(12) 0.6586(11) -0.198(3) 0.0350(18) Uani 1 1 d U . . C05 C 0.7891(12) 0.6235(10) -0.262(3) 0.0349(18) Uani 1 1 d U . . H05A H 0.7854 0.5793 -0.2749 0.042 Uiso 1 1 calc R . . C06 C 0.8570(11) 0.6531(9) -0.305(4) 0.0348(18) Uani 1 1 d U . . H06A H 0.9000 0.6287 -0.3442 0.042 Uiso 1 1 calc R . . C07 C 0.9415(11) 0.7539(9) -0.343(3) 0.035(2) Uani 1 1 d U . . H07A H 0.9344 0.7989 -0.3215 0.053 Uiso 1 1 calc R . . H07B H 0.9536 0.7467 -0.4727 0.053 Uiso 1 1 calc R . . H07C H 0.9844 0.7384 -0.2669 0.053 Uiso 1 1 calc R . . C08 C 0.6430(12) 0.6260(10) -0.159(3) 0.035(2) Uani 1 1 d U . . H08A H 0.6476 0.5809 -0.1821 0.053 Uiso 1 1 calc R . . H08B H 0.6030 0.6438 -0.2391 0.053 Uiso 1 1 calc R . . H08C H 0.6285 0.6329 -0.0303 0.053 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 0.0249(3) 0.0279(4) 0.0297(5) -0.0006(4) -0.0007(4) 0.0027(3) Hg2 0.0236(4) 0.0268(4) 0.0314(5) 0.0001(3) -0.0004(3) 0.0011(3) Hg3 0.0257(4) 0.0291(4) 0.0257(5) -0.0018(3) -0.0006(3) -0.0001(3) F3 0.026(6) 0.048(8) 0.062(10) -0.028(7) 0.005(6) 0.007(5) F4 0.033(6) 0.037(7) 0.050(9) -0.016(6) -0.005(6) 0.008(5) F5 0.045(7) 0.023(6) 0.084(12) 0.014(7) -0.022(7) -0.001(5) F6 0.027(5) 0.017(5) 0.059(9) -0.003(6) 0.013(6) -0.003(4) F9 0.032(6) 0.035(7) 0.048(9) 0.004(6) 0.000(6) 0.001(5) F10 0.020(6) 0.050(7) 0.061(10) 0.015(7) -0.007(6) 0.004(5) F11 0.023(6) 0.055(8) 0.030(7) -0.011(6) 0.000(5) 0.014(5) F12 0.027(5) 0.024(6) 0.067(10) -0.012(6) 0.002(6) 0.007(4) F15 0.043(6) 0.028(6) 0.054(9) -0.006(6) -0.014(7) 0.002(5) F16 0.041(6) 0.024(6) 0.059(9) -0.010(6) -0.001(6) -0.012(5) F17 0.028(6) 0.054(7) 0.036(8) 0.000(6) 0.008(5) -0.010(5) F18 0.024(6) 0.050(7) 0.059(9) -0.022(7) 0.018(6) 0.011(5) C1 0.026(4) 0.037(4) 0.020(5) -0.009(4) -0.010(3) 0.012(3) C2 0.026(4) 0.036(4) 0.020(5) -0.009(4) -0.010(3) 0.012(3) C3 0.026(4) 0.036(4) 0.020(5) -0.010(4) -0.010(3) 0.011(3) C4 0.026(4) 0.036(4) 0.020(5) -0.010(4) -0.010(3) 0.011(3) C5 0.026(4) 0.036(4) 0.020(5) -0.010(4) -0.010(3) 0.011(3) C6 0.026(4) 0.037(4) 0.020(5) -0.009(4) -0.010(3) 0.011(3) C7 0.030(4) 0.027(4) 0.032(5) 0.000(3) 0.001(4) 0.005(3) C8 0.030(4) 0.027(4) 0.032(5) 0.000(3) 0.001(4) 0.005(3) C9 0.030(4) 0.027(4) 0.032(5) 0.000(3) 0.001(4) 0.005(3) C10 0.030(4) 0.027(4) 0.032(5) 0.000(3) 0.001(4) 0.005(3) C11 0.030(4) 0.026(4) 0.032(5) 0.000(3) 0.001(4) 0.006(3) C12 0.030(4) 0.026(4) 0.032(5) 0.000(3) 0.001(4) 0.005(3) C13 0.037(4) 0.033(4) 0.025(5) 0.006(4) -0.001(4) -0.010(3) C14 0.037(4) 0.033(4) 0.025(5) 0.006(4) 0.000(4) -0.010(3) C15 0.037(4) 0.033(4) 0.025(5) 0.006(4) 0.000(4) -0.010(3) C16 0.037(4) 0.033(4) 0.025(5) 0.006(4) 0.000(4) -0.010(3) C17 0.037(4) 0.033(4) 0.025(5) 0.006(4) -0.001(4) -0.010(3) C18 0.037(4) 0.033(4) 0.025(5) 0.006(4) -0.001(4) -0.010(3) C01 0.037(4) 0.041(4) 0.026(4) -0.005(4) -0.001(4) -0.004(3) C02 0.037(4) 0.041(4) 0.026(4) -0.005(4) -0.001(4) -0.004(3) C03 0.037(4) 0.041(4) 0.026(4) -0.005(4) -0.001(4) -0.003(3) C04 0.037(4) 0.041(4) 0.026(4) -0.004(4) -0.001(4) -0.003(3) C05 0.037(4) 0.041(4) 0.026(4) -0.005(4) 0.000(4) -0.003(3) C06 0.037(4) 0.041(4) 0.026(4) -0.005(4) -0.001(4) -0.004(3) C07 0.037(4) 0.042(4) 0.027(5) -0.004(4) 0.000(4) -0.004(4) C08 0.038(4) 0.042(4) 0.026(5) -0.005(4) 0.000(4) -0.003(4) _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 C8 2.086(18) . ? Hg1 C1 2.100(18) . ? Hg1 C02 3.19(2) . ? Hg1 C01 3.42(2) . ? Hg2 C7 2.028(18) . ? Hg2 C14 2.07(2) . ? Hg3 C2 2.07(2) . ? Hg3 C13 2.110(19) . ? F3 C3 1.43(2) . ? F4 C4 1.27(2) . ? F5 C5 1.31(2) . ? F6 C6 1.33(2) . ? F9 C9 1.32(2) . ? F10 C10 1.31(2) . ? F11 C11 1.43(2) . ? F12 C12 1.37(2) . ? F15 C15 1.31(2) . ? F16 C16 1.36(2) . ? F17 C17 1.34(2) . ? F18 C18 1.36(2) . ? C1 C6 1.32(3) . ? C1 C2 1.50(3) . ? C2 C3 1.32(3) . ? C3 C4 1.41(3) . ? C4 C5 1.42(3) . ? C5 C6 1.36(3) . ? C7 C12 1.42(2) . ? C7 C8 1.46(3) . ? C8 C9 1.33(3) . ? C9 C10 1.44(3) . ? C10 C11 1.36(3) . ? C11 C12 1.33(3) . ? C13 C18 1.33(3) . ? C13 C14 1.42(3) . ? C14 C15 1.37(3) . ? C15 C16 1.42(3) . ? C16 C17 1.38(3) . ? C17 C18 1.36(3) . ? C01 C06 1.38(3) . ? C01 C02 1.40(3) . ? C01 C07 1.52(3) . ? C02 C03 1.42(3) . ? C03 C04 1.38(3) . ? C04 C05 1.41(3) . ? C04 C08 1.53(3) . ? C05 C06 1.34(3) . ? 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 C8 Hg1 C1 177.4(8) . . ? C8 Hg1 C02 101.0(7) . . ? C1 Hg1 C02 81.6(7) . . ? C8 Hg1 C01 77.6(7) . . ? C1 Hg1 C01 105.0(7) . . ? C02 Hg1 C01 24.2(5) . . ? C7 Hg2 C14 174.8(8) . . ? C2 Hg3 C13 177.0(9) . . ? C6 C1 C2 119.7(17) . . ? C6 C1 Hg1 123.7(14) . . ? C2 C1 Hg1 116.0(13) . . ? C3 C2 C1 112.2(18) . . ? C3 C2 Hg3 124.4(15) . . ? C1 C2 Hg3 122.7(13) . . ? C2 C3 C4 131.0(19) . . ? C2 C3 F3 117.4(18) . . ? C4 C3 F3 111.2(15) . . ? F4 C4 C3 125.5(18) . . ? F4 C4 C5 122.7(18) . . ? C3 C4 C5 111.8(17) . . ? F5 C5 C6 118.9(18) . . ? F5 C5 C4 120.2(17) . . ? C6 C5 C4 120.9(19) . . ? C1 C6 F6 116.8(16) . . ? C1 C6 C5 124.1(19) . . ? F6 C6 C5 119.1(18) . . ? C12 C7 C8 112.1(16) . . ? C12 C7 Hg2 123.1(13) . . ? C8 C7 Hg2 123.8(12) . . ? C9 C8 C7 122.5(17) . . ? C9 C8 Hg1 118.7(14) . . ? C7 C8 Hg1 118.3(13) . . ? F9 C9 C8 123.2(17) . . ? F9 C9 C10 114.3(16) . . ? C8 C9 C10 122.5(18) . . ? F10 C10 C11 123.8(17) . . ? F10 C10 C9 121.4(18) . . ? C11 C10 C9 114.8(17) . . ? C12 C11 C10 123.6(18) . . ? C12 C11 F11 118.5(17) . . ? C10 C11 F11 117.4(16) . . ? C11 C12 F12 119.3(16) . . ? C11 C12 C7 124.0(18) . . ? F12 C12 C7 116.6(16) . . ? C18 C13 C14 120.2(19) . . ? C18 C13 Hg3 119.5(16) . . ? C14 C13 Hg3 119.7(14) . . ? C15 C14 C13 118.0(18) . . ? C15 C14 Hg2 118.7(16) . . ? C13 C14 Hg2 123.3(14) . . ? F15 C15 C14 124.6(18) . . ? F15 C15 C16 115.1(17) . . ? C14 C15 C16 120.3(19) . . ? F16 C16 C17 119.6(17) . . ? F16 C16 C15 121.1(18) . . ? C17 C16 C15 119.2(18) . . ? F17 C17 C18 121.5(19) . . ? F17 C17 C16 119.5(17) . . ? C18 C17 C16 118.9(18) . . ? C13 C18 F18 120.2(18) . . ? C13 C18 C17 123(2) . . ? F18 C18 C17 116.8(17) . . ? C06 C01 C02 119.2(18) . . ? C06 C01 C07 123.7(17) . . ? C02 C01 C07 117.0(18) . . ? C06 C01 Hg1 98.6(16) . . ? C02 C01 Hg1 68.5(13) . . ? C07 C01 Hg1 98.6(14) . . ? C01 C02 C03 119(2) . . ? C01 C02 Hg1 87.3(14) . . ? C03 C02 Hg1 93.9(14) . . ? C04 C03 C02 120(2) . . ? C03 C04 C05 118.6(19) . . ? C03 C04 C08 119.9(19) . . ? C05 C04 C08 121.5(19) . . ? C06 C05 C04 121(2) . . ? C05 C06 C01 122.3(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.524 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.340 #===END data_compound_6 _database_code_CSD 208166 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (o-C6F4Hg)3-1,3,5(CH3)3(C6H3) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H12 F12 Hg3' _chemical_formula_weight 1166.14 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' F F 0.0171 0.0103 '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)/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 16.453(3) _cell_length_b 7.3780(15) _cell_length_c 22.030(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.43(3) _cell_angle_gamma 90.00 _cell_volume 2657.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 17.391 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.252773 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29640 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.84 _reflns_number_total 6307 _reflns_number_gt 4633 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0747P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6307 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 0.31864(2) 0.52856(4) 0.477092(13) 0.04824(11) Uani 1 1 d . . . Hg2 Hg 0.187993(19) 0.39678(4) 0.339989(14) 0.04986(11) Uani 1 1 d . . . Hg3 Hg 0.11987(2) 0.34160(5) 0.487949(14) 0.05472(11) Uani 1 1 d . . . F3 F 0.0953(4) 0.3188(9) 0.6261(2) 0.0862(18) Uani 1 1 d . . . F4 F 0.1906(4) 0.4179(9) 0.7293(2) 0.0824(17) Uani 1 1 d . . . F5 F 0.3397(4) 0.5649(9) 0.7225(2) 0.0830(18) Uani 1 1 d . . . F6 F 0.3944(3) 0.6171(7) 0.6123(2) 0.0678(14) Uani 1 1 d . . . F9 F 0.4835(3) 0.6650(8) 0.4338(3) 0.0728(15) Uani 1 1 d . . . F10 F 0.5361(3) 0.6997(7) 0.3232(3) 0.0718(14) Uani 1 1 d . . . F11 F 0.4396(4) 0.5945(8) 0.2207(2) 0.0743(15) Uani 1 1 d . . . F12 F 0.2896(4) 0.4611(9) 0.2298(2) 0.0769(16) Uani 1 1 d . . . F15 F 0.0339(3) 0.3023(9) 0.2425(2) 0.0779(16) Uani 1 1 d . . . F16 F -0.1171(3) 0.1816(9) 0.2559(2) 0.0823(17) Uani 1 1 d . . . F17 F -0.1632(4) 0.1196(10) 0.3674(3) 0.093(2) Uani 1 1 d . . . F18 F -0.0567(4) 0.1906(11) 0.4682(3) 0.093(2) Uani 1 1 d . . . C1 C 0.2751(5) 0.4991(10) 0.5612(4) 0.0477(17) Uani 1 1 d . . . C2 C 0.1949(5) 0.4168(12) 0.5646(4) 0.0513(19) Uani 1 1 d . . . C3 C 0.1706(6) 0.3943(12) 0.6214(4) 0.057(2) Uani 1 1 d . . . C4 C 0.2176(6) 0.4407(13) 0.6746(4) 0.060(2) Uani 1 1 d . . . C5 C 0.2930(6) 0.5180(13) 0.6706(4) 0.060(2) Uani 1 1 d . . . C6 C 0.3202(5) 0.5453(11) 0.6139(4) 0.0519(19) Uani 1 1 d . . . C7 C 0.3054(5) 0.4981(11) 0.3375(4) 0.053(2) Uani 1 1 d . . . C8 C 0.3564(5) 0.5477(10) 0.3906(4) 0.0476(18) Uani 1 1 d . . . C9 C 0.4324(5) 0.6133(10) 0.3835(4) 0.0492(18) Uani 1 1 d . . . C10 C 0.4608(6) 0.6306(11) 0.3272(4) 0.057(2) Uani 1 1 d . . . C11 C 0.4127(5) 0.5768(11) 0.2759(4) 0.0513(19) Uani 1 1 d . . . C12 C 0.3358(6) 0.5123(12) 0.2823(4) 0.056(2) Uani 1 1 d . . . C13 C 0.0459(5) 0.2817(12) 0.4084(4) 0.0516(18) Uani 1 1 d . . . C14 C 0.0705(5) 0.3120(11) 0.3493(4) 0.0515(19) Uani 1 1 d . . . C15 C 0.0145(6) 0.2754(13) 0.3010(4) 0.058(2) Uani 1 1 d . . . C16 C -0.0644(6) 0.2115(13) 0.3055(4) 0.063(2) Uani 1 1 d . . . C17 C -0.0875(5) 0.1850(13) 0.3622(4) 0.063(2) Uani 1 1 d . . . C18 C -0.0314(6) 0.2187(14) 0.4118(4) 0.064(2) Uani 1 1 d . . . C01 C 0.2212(6) -0.0603(12) 0.4209(4) 0.057(2) Uani 1 1 d . . . C02 C 0.2384(6) -0.0419(10) 0.4837(4) 0.054(2) Uani 1 1 d . . . H02A H 0.1988 -0.0740 0.5088 0.065 Uiso 1 1 calc R . . C03 C 0.3135(6) 0.0236(11) 0.5102(4) 0.0523(19) Uani 1 1 d . . . C04 C 0.3717(6) 0.0692(11) 0.4710(4) 0.058(2) Uani 1 1 d . . . H04A H 0.4226 0.1118 0.4875 0.070 Uiso 1 1 calc R . . C05 C 0.3554(6) 0.0525(11) 0.4083(4) 0.056(2) Uani 1 1 d . . . C06 C 0.2789(7) -0.0104(12) 0.3838(4) 0.063(2) Uani 1 1 d . . . H06A H 0.2668 -0.0186 0.3416 0.076 Uiso 1 1 calc R . . C07 C 0.1381(6) -0.1412(14) 0.3930(5) 0.072(3) Uani 1 1 d . . . H07A H 0.1362 -0.1439 0.3493 0.107 Uiso 1 1 calc R . . H07B H 0.0942 -0.0675 0.4044 0.107 Uiso 1 1 calc R . . H07C H 0.1326 -0.2621 0.4081 0.107 Uiso 1 1 calc R . . C08 C 0.3337(7) 0.0397(13) 0.5780(4) 0.069(3) Uani 1 1 d . . . H08A H 0.2874 0.0025 0.5979 0.104 Uiso 1 1 calc R . . H08B H 0.3470 0.1633 0.5884 0.104 Uiso 1 1 calc R . . H08C H 0.3797 -0.0365 0.5911 0.104 Uiso 1 1 calc R . . C09 C 0.4194(7) 0.1001(14) 0.3673(5) 0.079(3) Uani 1 1 d . . . H09A H 0.4681 0.1408 0.3916 0.119 Uiso 1 1 calc R . . H09B H 0.3992 0.1948 0.3398 0.119 Uiso 1 1 calc R . . H09C H 0.4319 -0.0049 0.3443 0.119 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 0.0478(2) 0.05542(18) 0.04178(17) 0.00253(12) 0.00642(13) 0.00245(13) Hg2 0.04148(19) 0.0638(2) 0.04469(18) 0.00042(13) 0.00646(13) -0.00044(13) Hg3 0.0456(2) 0.0764(2) 0.04179(18) 0.00052(14) 0.00319(14) -0.00160(15) F3 0.076(4) 0.131(5) 0.054(3) 0.004(3) 0.014(3) -0.023(4) F4 0.094(5) 0.112(4) 0.044(3) -0.003(3) 0.020(3) -0.010(4) F5 0.099(5) 0.101(4) 0.045(3) -0.010(3) -0.009(3) -0.015(4) F6 0.066(4) 0.070(3) 0.066(3) 0.000(2) 0.000(3) -0.013(3) F9 0.064(4) 0.085(4) 0.068(3) -0.003(3) 0.001(3) -0.017(3) F10 0.049(3) 0.078(3) 0.092(4) 0.011(3) 0.023(3) -0.007(3) F11 0.071(4) 0.102(4) 0.055(3) 0.010(3) 0.028(3) 0.003(3) F12 0.069(4) 0.118(5) 0.044(3) -0.003(3) 0.009(3) -0.003(3) F15 0.064(4) 0.118(5) 0.052(3) -0.010(3) 0.007(3) -0.008(3) F16 0.063(4) 0.111(5) 0.068(4) -0.018(3) -0.015(3) -0.014(3) F17 0.049(3) 0.142(6) 0.083(4) 0.002(4) -0.006(3) -0.028(4) F18 0.056(4) 0.165(6) 0.060(3) 0.009(4) 0.014(3) -0.024(4) C1 0.040(4) 0.054(4) 0.049(4) 0.000(3) 0.005(3) 0.005(3) C2 0.049(5) 0.062(5) 0.043(4) 0.001(3) 0.007(4) 0.009(4) C3 0.056(6) 0.073(5) 0.044(5) 0.002(4) 0.014(4) 0.001(4) C4 0.063(6) 0.077(6) 0.041(4) 0.004(4) 0.012(4) 0.003(5) C5 0.068(6) 0.073(6) 0.037(4) -0.004(4) -0.007(4) 0.007(5) C6 0.049(5) 0.052(4) 0.053(5) 0.002(3) -0.001(4) 0.000(4) C7 0.048(5) 0.062(5) 0.050(4) 0.014(4) 0.013(4) 0.014(4) C8 0.046(5) 0.049(4) 0.048(4) 0.003(3) 0.006(4) 0.005(3) C9 0.042(4) 0.053(4) 0.054(5) 0.003(3) 0.012(4) -0.002(3) C10 0.057(6) 0.053(5) 0.065(5) 0.005(4) 0.022(5) 0.000(4) C11 0.048(5) 0.060(5) 0.049(4) 0.008(3) 0.017(4) 0.010(4) C12 0.056(6) 0.066(5) 0.046(4) 0.000(4) 0.011(4) 0.004(4) C13 0.037(4) 0.064(5) 0.053(5) 0.001(4) 0.005(4) 0.001(4) C14 0.043(5) 0.061(5) 0.051(5) 0.000(3) 0.005(4) 0.006(4) C15 0.050(5) 0.080(6) 0.043(4) -0.001(4) -0.001(4) -0.003(4) C16 0.058(6) 0.067(5) 0.059(5) -0.007(4) -0.012(4) -0.004(4) C17 0.034(5) 0.083(6) 0.069(6) 0.001(5) -0.001(4) -0.008(4) C18 0.053(6) 0.087(6) 0.053(5) 0.003(4) 0.008(4) -0.007(5) C01 0.059(6) 0.058(5) 0.056(5) -0.005(4) 0.009(4) 0.013(4) C02 0.058(6) 0.049(4) 0.056(5) 0.002(4) 0.012(4) 0.001(4) C03 0.059(6) 0.049(4) 0.049(4) 0.005(3) 0.002(4) 0.002(4) C04 0.048(5) 0.053(5) 0.073(6) 0.004(4) 0.005(4) 0.002(4) C05 0.062(6) 0.054(5) 0.056(5) 0.004(4) 0.019(4) 0.003(4) C06 0.088(8) 0.058(5) 0.046(5) 0.004(4) 0.014(5) 0.020(5) C07 0.060(6) 0.080(6) 0.071(6) -0.011(5) -0.008(5) -0.003(5) C08 0.079(7) 0.060(5) 0.063(6) 0.004(4) -0.012(5) 0.011(5) C09 0.088(8) 0.070(6) 0.085(7) 0.015(5) 0.036(6) 0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 C1 2.071(8) . ? Hg1 C8 2.074(8) . ? Hg1 C04 3.506(8) . ? Hg2 C14 2.065(8) . ? Hg2 C7 2.078(9) . ? Hg2 C06 3.445(8) . ? Hg3 C2 2.053(8) . ? Hg3 C13 2.066(8) . ? Hg3 C02 3.443(8) . ? F3 C3 1.372(10) . ? F4 C4 1.341(9) . ? F5 C5 1.351(9) . ? F6 C6 1.335(10) . ? F9 C9 1.368(10) . ? F10 C10 1.352(10) . ? F11 C11 1.346(9) . ? F12 C12 1.364(10) . ? F15 C15 1.377(9) . ? F16 C16 1.335(9) . ? F17 C17 1.353(10) . ? F18 C18 1.371(10) . ? C1 C6 1.350(11) . ? C1 C2 1.462(12) . ? C2 C3 1.366(11) . ? C3 C4 1.374(12) . ? C4 C5 1.377(13) . ? C5 C6 1.388(12) . ? C7 C12 1.369(11) . ? C7 C8 1.409(11) . ? C8 C9 1.366(11) . ? C9 C10 1.381(11) . ? C10 C11 1.366(12) . ? C11 C12 1.374(12) . ? C13 C18 1.364(12) . ? C13 C14 1.422(11) . ? C14 C15 1.355(11) . ? C15 C16 1.396(12) . ? C16 C17 1.361(12) . ? C17 C18 1.372(12) . ? C01 C06 1.372(13) . ? C01 C02 1.387(11) . ? C01 C07 1.553(13) . ? C02 C03 1.392(12) . ? C03 C04 1.401(12) . ? C03 C08 1.499(12) . ? C04 C05 1.382(12) . ? C05 C06 1.392(14) . ? C05 C09 1.505(12) . ? 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 C8 176.4(3) . . ? C1 Hg1 C04 92.6(3) . . ? C8 Hg1 C04 85.9(3) . . ? C14 Hg2 C7 174.6(3) . . ? C14 Hg2 C06 95.2(3) . . ? C7 Hg2 C06 86.9(3) . . ? C2 Hg3 C13 176.3(3) . . ? C2 Hg3 C02 87.4(3) . . ? C13 Hg3 C02 94.8(3) . . ? C6 C1 C2 118.2(7) . . ? C6 C1 Hg1 122.1(6) . . ? C2 C1 Hg1 119.6(6) . . ? C3 C2 C1 117.2(8) . . ? C3 C2 Hg3 120.6(7) . . ? C1 C2 Hg3 122.2(6) . . ? C2 C3 F3 118.6(8) . . ? C2 C3 C4 123.8(9) . . ? F3 C3 C4 117.6(7) . . ? F4 C4 C3 121.7(9) . . ? F4 C4 C5 120.0(8) . . ? C3 C4 C5 118.3(8) . . ? F5 C5 C4 118.9(8) . . ? F5 C5 C6 120.9(9) . . ? C4 C5 C6 120.1(8) . . ? F6 C6 C1 119.6(8) . . ? F6 C6 C5 118.0(8) . . ? C1 C6 C5 122.4(8) . . ? C12 C7 C8 118.3(8) . . ? C12 C7 Hg2 119.0(7) . . ? C8 C7 Hg2 122.7(6) . . ? C9 C8 C7 117.7(7) . . ? C9 C8 Hg1 120.0(6) . . ? C7 C8 Hg1 122.3(6) . . ? C8 C9 F9 119.7(7) . . ? C8 C9 C10 122.8(8) . . ? F9 C9 C10 117.5(8) . . ? F10 C10 C11 120.5(8) . . ? F10 C10 C9 119.9(8) . . ? C11 C10 C9 119.6(8) . . ? F11 C11 C10 120.1(8) . . ? F11 C11 C12 121.8(8) . . ? C10 C11 C12 118.1(7) . . ? F12 C12 C7 120.4(8) . . ? F12 C12 C11 116.2(7) . . ? C7 C12 C11 123.4(8) . . ? C18 C13 C14 117.7(8) . . ? C18 C13 Hg3 119.4(6) . . ? C14 C13 Hg3 122.8(6) . . ? C15 C14 C13 116.8(8) . . ? C15 C14 Hg2 122.9(6) . . ? C13 C14 Hg2 120.2(6) . . ? C14 C15 F15 119.9(8) . . ? C14 C15 C16 124.6(8) . . ? F15 C15 C16 115.5(7) . . ? F16 C16 C17 120.4(9) . . ? F16 C16 C15 121.5(8) . . ? C17 C16 C15 118.1(8) . . ? F17 C17 C16 118.9(8) . . ? F17 C17 C18 122.8(8) . . ? C16 C17 C18 118.3(8) . . ? C13 C18 F18 118.8(8) . . ? C13 C18 C17 124.5(8) . . ? F18 C18 C17 116.7(8) . . ? C06 C01 C02 119.4(9) . . ? C06 C01 C07 120.3(9) . . ? C02 C01 C07 120.3(8) . . ? C01 C02 C03 121.6(8) . . ? C01 C02 Hg3 93.1(5) . . ? C03 C02 Hg3 100.5(5) . . ? C02 C03 C04 117.4(8) . . ? C02 C03 C08 122.2(8) . . ? C04 C03 C08 120.3(9) . . ? C05 C04 C03 121.7(8) . . ? C05 C04 Hg1 95.9(5) . . ? C03 C04 Hg1 91.1(5) . . ? C04 C05 C06 118.9(8) . . ? C04 C05 C09 120.6(9) . . ? C06 C05 C09 120.5(9) . . ? C01 C06 C05 121.0(9) . . ? C01 C06 Hg2 95.3(6) . . ? C05 C06 Hg2 99.4(5) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 3.708 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.253