Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bauer, Jeanette A Krause' 'Laavanya, P.' 'Panchanatheswaran, K.' 'Venkatasubramanian, U.' _publ_contact_author_name 'Prof K Panchanatheswaran' _publ_contact_author_address ; Department of Chemistry Bharathidasan University Tiruchirappalli 620 024 INDIA ; _publ_contact_author_email 'PAN@BDU.ERNET.IN' _publ_section_title ; Subtlety in the reactivity of a diketo phosphorus ylide towards mercuric halides: the unprecedented O-coordination of alpha-acetyl-alpha-benzoylmthylenetriphenylphosphorane to Hg(II) ; data_y2hgcl _database_code_CSD 167767 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H46 Cl2 Hg O4 P2' _chemical_formula_weight 1116.36 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.4399(2) _cell_length_b 10.0105(3) _cell_length_c 17.9576(4) _cell_angle_alpha 90.0000(11) _cell_angle_beta 100.525(2) _cell_angle_gamma 90.0000(11) _cell_volume 2375.37(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method ? _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 3.467 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25177 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.22 _reflns_number_total 11404 _reflns_number_observed 8726 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.8568P] 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 ? _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 0.00 _refine_ls_number_reflns 11403 _refine_ls_number_parameters 254 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_obs 0.0267 _refine_ls_wR_factor_all 0.0645 _refine_ls_wR_factor_obs 0.0587 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.24998(4) -0.2142(2) -0.00001(3) 0.02145(4) Uani 1 d . . Cl1 Cl 0.3066(2) -0.4199(3) 0.0436(2) 0.0286(7) Uani 1 d . . Cl2 Cl 0.1926(2) -0.0074(3) -0.0438(2) 0.0284(7) Uani 1 d . . P1 P 0.2098(2) -0.0833(3) 0.2353(2) 0.0159(6) Uani 1 d . . P2 P 0.2904(2) -0.3452(3) -0.23537(15) 0.0160(6) Uani 1 d . . O1 O 0.3404(5) -0.0946(8) 0.1321(4) 0.023(2) Uani 1 d . . O2 O 0.2709(6) -0.3444(9) 0.3249(4) 0.025(2) Uani 1 d . . O3 O 0.1573(6) -0.3312(7) -0.1302(4) 0.022(2) Uani 1 d . . O4 O 0.2282(6) -0.0771(8) -0.3275(4) 0.027(2) Uani 1 d . . C1 C 0.3233(6) -0.1806(9) 0.2496(5) 0.018(2) Uani 1 d . . C2 C 0.3784(7) -0.1689(10) 0.1877(5) 0.016(2) Uani 1 d . . C3 C 0.3384(6) -0.2775(10) 0.3055(6) 0.017(2) Uani 1 d . . C4 C 0.4747(7) -0.2396(12) 0.1881(5) 0.032(3) Uani 1 d . . H4A H 0.4638(8) -0.3361(12) 0.1914(18) 0.028(5) Uiso 1 calc R . H4B H 0.5247(9) -0.2105(25) 0.2318(11) 0.028(5) Uiso 1 calc R . H4C H 0.4996(14) -0.2193(28) 0.1414(9) 0.028(5) Uiso 1 calc R . C5 C 0.1792(7) -0.2537(9) -0.2486(5) 0.019(2) Uani 1 d . . C6 C 0.1235(7) -0.2677(11) -0.1894(6) 0.024(2) Uani 1 d . . C7 C 0.1575(8) -0.1418(10) -0.3085(5) 0.020(2) Uani 1 d . . C8 C 0.0228(6) -0.1907(10) -0.1869(5) 0.023(3) Uani 1 d . . H8A H -0.0344(7) -0.2407(18) -0.2154(15) 0.028(5) Uiso 1 calc R . H8B H 0.0257(11) -0.1021(15) -0.2095(17) 0.028(5) Uiso 1 calc R . H8C H 0.0140(14) -0.1810(29) -0.1342(5) 0.028(5) Uiso 1 calc R . C10 C 0.1534(4) -0.0926(7) 0.3206(2) 0.019(2) Uiso 1 d G . C11 C 0.2173(3) -0.0825(7) 0.3906(3) 0.018(2) Uiso 1 d G . C12 C 0.1772(3) -0.0839(7) 0.4567(2) 0.024(2) Uiso 1 d G . C13 C 0.0733(3) -0.0954(7) 0.4528(2) 0.025(2) Uiso 1 d G . C14 C 0.0095(3) -0.1055(7) 0.3828(3) 0.025(2) Uiso 1 d G . C15 C 0.0495(4) -0.1041(7) 0.3167(2) 0.023(2) Uiso 1 d G . H11 H 0.2882(3) -0.0746(10) 0.3933(4) 0.0311(15) Uiso 1 calc G . H12 H 0.2208(4) -0.0770(10) 0.5045(3) 0.0311(15) Uiso 1 d G . H13 H 0.0459(5) -0.0964(10) 0.4980(3) 0.0311(15) Uiso 1 d G . H14 H -0.0615(3) -0.1134(10) 0.3802(4) 0.0311(15) Uiso 1 d G . H15 H 0.0059(5) -0.1110(10) 0.2689(2) 0.0311(15) Uiso 1 d G . C20 C 0.2287(5) 0.0983(4) 0.2213(3) 0.024(3) Uiso 1 d G . C21 C 0.2398(5) 0.1861(5) 0.2822(2) 0.022(2) Uiso 1 d G . C22 C 0.2557(4) 0.3213(5) 0.2711(2) 0.021(2) Uiso 1 d G . C23 C 0.2605(4) 0.3686(4) 0.1990(3) 0.024(2) Uiso 1 d G . C24 C 0.2494(4) 0.2807(6) 0.1381(2) 0.023(2) Uiso 1 d G . C25 C 0.2335(5) 0.1456(5) 0.1493(3) 0.018(2) Uiso 1 d G . H21 H 0.2365(7) 0.1538(7) 0.3314(3) 0.0311(15) Uiso 1 calc G . H22 H 0.2633(6) 0.3814(6) 0.3127(3) 0.0311(15) Uiso 1 d G . H23 H 0.2714(7) 0.4609(4) 0.1914(4) 0.0311(15) Uiso 1 d G . H24 H 0.2527(6) 0.3130(8) 0.0889(2) 0.0311(15) Uiso 1 d G . H25 H 0.2259(7) 0.0855(7) 0.1077(3) 0.0311(15) Uiso 1 d G . C30 C 0.1151(3) -0.1372(4) 0.1563(2) 0.0075(15) Uiso 1 d G . C31 C 0.0394(3) -0.0492(3) 0.1240(2) 0.025(2) Uiso 1 d G . C32 C -0.0371(3) -0.0923(4) 0.0662(2) 0.0224(12) Uiso 1 d G . C33 C -0.0381(3) -0.2234(4) 0.0407(2) 0.0278(12) Uiso 1 d G . C34 C 0.0376(3) -0.3115(3) 0.0730(2) 0.0307(15) Uiso 1 d G . C35 C 0.1141(3) -0.2684(4) 0.1308(2) 0.0261(15) Uiso 1 d G . H31 H 0.0400(5) 0.0405(4) 0.1414(3) 0.0311(15) Uiso 1 calc G . H32 H -0.0888(4) -0.0321(5) 0.0441(3) 0.0311(15) Uiso 1 d G . H33 H -0.0904(3) -0.2529(5) 0.0012(3) 0.0311(15) Uiso 1 d G . H34 H 0.0369(4) -0.4012(3) 0.0556(3) 0.0311(15) Uiso 1 d G . H35 H 0.1658(4) -0.3286(5) 0.1529(3) 0.0311(15) Uiso 1 d G . C40 C 0.4474(3) -0.3049(5) 0.3486(3) 0.019(2) Uiso 1 d G . C41 C 0.4862(4) -0.4337(5) 0.3583(3) 0.029(2) Uiso 1 d G . C42 C 0.5825(4) -0.4548(4) 0.4002(3) 0.0203(14) Uiso 1 d G . C43 C 0.6400(3) -0.3471(6) 0.4325(3) 0.030(3) Uiso 1 d G . C44 C 0.6012(3) -0.2183(5) 0.4228(3) 0.020(2) Uiso 1 d G . C45 C 0.5049(4) -0.1972(4) 0.3808(3) 0.033(2) Uiso 1 d G . H41 H 0.4469(5) -0.5073(6) 0.3362(4) 0.0311(15) Uiso 1 calc G . H42 H 0.6090(5) -0.5428(5) 0.4069(4) 0.0311(15) Uiso 1 d G . H43 H 0.7059(3) -0.3615(7) 0.4612(4) 0.0311(15) Uiso 1 d G . H44 H 0.6405(5) -0.1446(6) 0.4448(4) 0.0311(15) Uiso 1 d G . H45 H 0.4783(5) -0.1091(5) 0.3742(4) 0.0311(15) Uiso 1 d G . C50 C 0.3455(4) -0.3325(7) -0.3207(2) 0.015(2) Uiso 1 d G . C51 C 0.2872(3) -0.3434(7) -0.3928(3) 0.022(2) Uiso 1 d G . C52 C 0.3336(3) -0.3424(7) -0.4560(2) 0.020(2) Uiso 1 d G . C53 C 0.4381(3) -0.3305(6) -0.4470(2) 0.024(2) Uiso 1 d G . C54 C 0.4963(3) -0.3195(7) -0.3748(3) 0.025(2) Uiso 1 d G . C55 C 0.4500(4) -0.3205(7) -0.3117(2) 0.021(2) Uiso 1 d G . H51 H 0.2158(3) -0.3516(10) -0.3989(4) 0.0311(15) Uiso 1 calc G . H52 H 0.2938(4) -0.3499(10) -0.5053(2) 0.0311(15) Uiso 1 d G . H53 H 0.4698(4) -0.3298(10) -0.4902(3) 0.0311(15) Uiso 1 d G . H54 H 0.5678(3) -0.3114(10) -0.3687(4) 0.0311(15) Uiso 1 d G . H55 H 0.4898(5) -0.3130(10) -0.2624(2) 0.0311(15) Uiso 1 d G . C60 C 0.2696(5) -0.5225(4) -0.2222(3) 0.012(2) Uiso 1 d G . C61 C 0.2606(4) -0.6055(5) -0.2852(2) 0.020(2) Uiso 1 d G . C62 C 0.2452(4) -0.7418(5) -0.2776(2) 0.028(2) Uiso 1 d G . C63 C 0.2387(4) -0.7951(4) -0.2072(3) 0.024(2) Uiso 1 d G . C64 C 0.2477(4) -0.7121(6) -0.1443(2) 0.030(2) Uiso 1 d G . C65 C 0.2631(5) -0.5758(6) -0.1518(3) 0.028(2) Uiso 1 d G . H61 H 0.2650(7) -0.5691(7) -0.3333(3) 0.0311(15) Uiso 1 calc G . H62 H 0.2390(7) -0.7985(6) -0.3207(3) 0.0311(15) Uiso 1 d G . H63 H 0.2281(7) -0.8882(4) -0.2021(4) 0.0311(15) Uiso 1 d G . H64 H 0.2433(7) -0.7485(8) -0.0961(3) 0.0311(15) Uiso 1 d G . H65 H 0.2693(7) -0.5191(7) -0.1088(3) 0.0311(15) Uiso 1 d G . C70 C 0.3883(3) -0.2879(4) -0.1587(2) 0.029(2) Uiso 1 d G . C71 C 0.4632(3) -0.3687(3) -0.1180(3) 0.020(2) Uiso 1 d G . C72 C 0.5340(3) -0.3146(4) -0.0596(2) 0.0244(13) Uiso 1 d G . C73 C 0.5299(3) -0.1797(4) -0.0420(2) 0.0245(12) Uiso 1 d G . C74 C 0.4551(3) -0.0989(3) -0.0827(2) 0.0226(12) Uiso 1 d G . C75 C 0.3842(3) -0.1530(4) -0.1410(2) 0.0187(13) Uiso 1 d G . H71 H 0.4659(5) -0.4608(3) -0.1300(4) 0.0311(15) Uiso 1 calc G . H72 H 0.5852(4) -0.3698(5) -0.0318(3) 0.0311(15) Uiso 1 d G . H73 H 0.5784(4) -0.1428(5) -0.0021(3) 0.0311(15) Uiso 1 d G . H74 H 0.4523(4) -0.0068(3) -0.0707(3) 0.0311(15) Uiso 1 d G . H75 H 0.3330(4) -0.0978(5) -0.1688(3) 0.0311(15) Uiso 1 d G . C80 C 0.0531(3) -0.1219(5) -0.3481(3) 0.018(2) Uiso 1 d G . C81 C 0.0179(4) 0.0073(4) -0.3644(3) 0.018(2) Uiso 1 d G . C82 C -0.0772(4) 0.0279(5) -0.4084(3) 0.038(2) Uiso 1 d G . C83 C -0.1372(3) -0.0807(6) -0.4360(3) 0.030(3) Uiso 1 d G . C84 C -0.1020(3) -0.2099(5) -0.4196(3) 0.036(3) Uiso 1 d G . C85 C -0.0069(3) -0.2305(4) -0.3757(3) 0.0136(15) Uiso 1 d G . H81 H 0.0589(5) 0.0816(5) -0.3455(4) 0.0311(15) Uiso 1 calc G . H82 H -0.1013(5) 0.1162(5) -0.4195(4) 0.0311(15) Uiso 1 d G . H83 H -0.2023(4) -0.0667(8) -0.4660(4) 0.0311(15) Uiso 1 d G . H84 H -0.1430(5) -0.2842(6) -0.4385(4) 0.0311(15) Uiso 1 d G . H85 H 0.0172(5) -0.3188(4) -0.3645(4) 0.0311(15) Uiso 1 d G . 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 0.02764(6) 0.01706(5) 0.01967(6) 0.00234(5) 0.00440(4) 0.00329(5) Cl1 0.040(2) 0.020(2) 0.026(2) 0.0027(13) 0.0049(14) 0.0088(14) Cl2 0.041(2) 0.019(2) 0.024(2) 0.0047(13) 0.0028(14) 0.0050(14) P1 0.0156(14) 0.0124(14) 0.0189(15) 0.0002(13) 0.0009(11) 0.0018(13) P2 0.0165(14) 0.0175(15) 0.0138(14) -0.0003(13) 0.0021(11) -0.0009(13) O1 0.025(4) 0.028(4) 0.014(3) -0.004(3) 0.003(3) -0.002(3) O2 0.024(4) 0.022(4) 0.030(4) 0.007(3) 0.006(3) 0.004(3) O3 0.028(4) 0.013(3) 0.024(4) 0.007(3) 0.003(3) 0.005(3) O4 0.019(4) 0.017(3) 0.045(5) 0.005(3) 0.007(3) -0.007(3) C1 0.007(4) 0.014(4) 0.031(5) -0.011(3) -0.002(3) 0.009(3) C2 0.028(5) 0.015(4) 0.008(3) -0.001(3) 0.010(3) -0.002(3) C3 0.003(3) 0.017(4) 0.028(4) -0.004(4) -0.003(3) 0.002(3) C4 0.027(5) 0.052(8) 0.016(4) 0.003(5) 0.004(3) -0.011(5) C5 0.025(5) 0.022(5) 0.009(4) 0.010(3) 0.002(3) -0.005(3) C6 0.010(4) 0.017(4) 0.041(5) -0.007(3) -0.006(3) 0.000(3) C7 0.044(5) 0.007(3) 0.011(4) 0.003(3) 0.011(3) 0.003(3) C8 0.017(4) 0.024(6) 0.031(5) 0.002(4) 0.011(4) 0.014(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 Cl1 2.283(4) . ? Hg1 Cl2 2.297(3) . ? P1 C1 1.788(8) . ? P1 C30 1.807(4) . ? P1 C10 1.832(4) . ? P1 C20 1.859(5) . ? P2 C5 1.731(10) . ? P2 C70 1.815(4) . ? P2 C60 1.820(5) . ? P2 C50 1.823(4) . ? O1 C2 1.275(11) . ? O2 C3 1.227(11) . ? O3 C6 1.249(12) . ? O4 C7 1.247(11) . ? C1 C3 1.384(13) . ? C1 C2 1.450(11) . ? C2 C4 1.473(13) . ? C3 C40 1.551(9) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 C6 1.416(12) . ? C5 C7 1.543(12) . ? C6 C8 1.566(12) . ? C7 C80 1.466(10) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C10 C11 1.39 . ? C10 C15 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C12 H12 0.95 . ? C13 C14 1.39 . ? C13 H13 0.95 . ? C14 C15 1.39 . ? C14 H14 0.95 . ? C15 H11 3.26 . ? C15 H15 0.95 . ? C20 C21 1.39 . ? C20 C25 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C22 H22 0.95 . ? C23 C24 1.39 . ? C23 H23 0.95 . ? C24 C25 1.39 . ? C24 H24 0.95 . ? C25 H21 3.26 . ? C25 H25 0.95 . ? C30 C31 1.39 . ? C30 C35 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? C32 H32 0.95 . ? C33 C34 1.39 . ? C33 H33 0.95 . ? C34 C35 1.39 . ? C34 H34 0.95 . ? C35 H31 3.27 . ? C35 H35 0.95 . ? C40 C41 1.39 . ? C40 C45 1.39 . ? C41 C42 1.39 . ? C42 C43 1.39 . ? C42 H42 0.95 . ? C43 C44 1.39 . ? C43 H43 0.95 . ? C44 C45 1.39 . ? C44 H44 0.95 . ? C45 H41 3.27 . ? C45 H45 0.95 . ? C50 C51 1.39 . ? C50 C55 1.39 . ? C51 C52 1.39 . ? C52 C53 1.39 . ? C52 H52 0.95 . ? C53 C54 1.39 . ? C53 H53 0.95 . ? C54 C55 1.39 . ? C54 H54 0.95 . ? C55 H51 3.27 . ? C55 H55 0.95 . ? C60 C61 1.39 . ? C60 C65 1.39 . ? C61 C62 1.39 . ? C62 C63 1.39 . ? C62 H62 0.95 . ? C63 C64 1.39 . ? C63 H63 0.95 . ? C64 C65 1.39 . ? C64 H64 0.95 . ? C65 H61 3.27 . ? C65 H65 0.95 . ? C70 C71 1.39 . ? C70 C75 1.39 . ? C71 C72 1.39 . ? C72 C73 1.39 . ? C72 H72 0.95 . ? C73 C74 1.39 . ? C73 H73 0.95 . ? C74 C75 1.39 . ? C74 H74 0.95 . ? C75 H71 3.26 . ? C75 H75 0.95 . ? C80 C81 1.39 . ? C80 C85 1.39 . ? C81 C82 1.39 . ? C82 C83 1.39 . ? C82 H82 0.95 . ? C83 C84 1.39 . ? C83 H83 0.95 . ? C84 C85 1.39 . ? C84 H84 0.95 . ? C85 H81 3.26 . ? C85 H85 0.95 . ? 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 Cl1 Hg1 Cl2 179.8(2) . . ? C1 P1 C30 114.2(4) . . ? C1 P1 C10 108.9(4) . . ? C30 P1 C10 107.6(3) . . ? C1 P1 C20 114.7(4) . . ? C30 P1 C20 106.3(3) . . ? C10 P1 C20 104.5(3) . . ? C5 P2 C70 115.1(4) . . ? C5 P2 C60 112.6(4) . . ? C70 P2 C60 108.5(3) . . ? C5 P2 C50 108.7(3) . . ? C70 P2 C50 105.5(3) . . ? C60 P2 C50 105.8(3) . . ? C3 C1 C2 125.8(8) . . ? C3 C1 P1 119.6(6) . . ? C2 C1 P1 112.8(7) . . ? O1 C2 C1 117.4(9) . . ? O1 C2 C4 120.7(7) . . ? C1 C2 C4 121.9(8) . . ? O2 C3 C1 124.8(8) . . ? O2 C3 C40 116.2(9) . . ? C1 C3 C40 119.1(7) . . ? C2 C4 H4A 109.5(6) . . ? C2 C4 H4B 109.5(5) . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5(5) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 122.5(8) . . ? C6 C5 P2 114.0(7) . . ? C7 C5 P2 121.9(6) . . ? O3 C6 C5 121.9(9) . . ? O3 C6 C8 114.1(8) . . ? C5 C6 C8 123.5(9) . . ? O4 C7 C80 120.4(8) . . ? O4 C7 C5 120.7(9) . . ? C80 C7 C5 118.6(7) . . ? C6 C8 H8A 109.5(5) . . ? C6 C8 H8B 109.5(5) . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5(5) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C10 C15 120.0 . . ? C11 C10 P1 118.1(3) . . ? C15 C10 P1 121.8(3) . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H11 98.4 . . ? C10 C15 H11 21.6 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? H11 C15 H15 141.6 . . ? C21 C20 C25 120.0 . . ? C21 C20 P1 120.7(3) . . ? C25 C20 P1 119.3(3) . . ? C22 C21 C20 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.0 . . ? C24 C25 H21 98.4 . . ? C20 C25 H21 21.6 . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? H21 C25 H25 141.6 . . ? C31 C30 C35 120.0 . . ? C31 C30 P1 119.7(3) . . ? C35 C30 P1 120.2(2) . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 H31 98.4 . . ? C30 C35 H31 21.6 . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? H31 C35 H35 141.6 . . ? C41 C40 C45 120.0 . . ? C41 C40 C3 121.7(5) . . ? C45 C40 C3 118.2(5) . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H41 98.4 . . ? C40 C45 H41 21.6 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? H41 C45 H45 141.6 . . ? C51 C50 C55 120.0 . . ? C51 C50 P2 122.1(3) . . ? C55 C50 P2 117.7(3) . . ? C50 C51 C52 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 H51 98.4 . . ? C50 C55 H51 21.6 . . ? C54 C55 H55 120.0 . . ? C50 C55 H55 120.0 . . ? H51 C55 H55 141.6 . . ? C61 C60 C65 120.0 . . ? C61 C60 P2 118.1(3) . . ? C65 C60 P2 121.9(3) . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 H61 98.4 . . ? C60 C65 H61 21.6 . . ? C64 C65 H65 120.0 . . ? C60 C65 H65 120.0 . . ? H61 C65 H65 141.6 . . ? C71 C70 C75 120.0 . . ? C71 C70 P2 124.7(3) . . ? C75 C70 P2 115.3(3) . . ? C70 C71 C72 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.0 . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C70 120.0 . . ? C74 C75 H71 98.4 . . ? C70 C75 H71 21.6 . . ? C74 C75 H75 120.0 . . ? C70 C75 H75 120.0 . . ? H71 C75 H75 141.6 . . ? C81 C80 C85 120.0 . . ? C81 C80 C7 119.2(5) . . ? C85 C80 C7 120.5(5) . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82 120.0 . . ? C83 C82 H82 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C84 C85 C80 120.0 . . ? C84 C85 H81 98.4 . . ? C80 C85 H81 21.6 . . ? C84 C85 H85 120.0 . . ? C80 C85 H85 120.0 . . ? H81 C85 H85 141.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C30 P1 C1 C3 -100.6(7) . . . . ? C10 P1 C1 C3 19.7(8) . . . . ? C20 P1 C1 C3 136.3(7) . . . . ? C30 P1 C1 C2 65.3(8) . . . . ? C10 P1 C1 C2 -174.4(6) . . . . ? C20 P1 C1 C2 -57.7(8) . . . . ? C3 C1 C2 O1 164.1(9) . . . . ? P1 C1 C2 O1 -0.7(11) . . . . ? C3 C1 C2 C4 -15.7(15) . . . . ? P1 C1 C2 C4 179.4(8) . . . . ? C2 C1 C3 O2 -130.9(11) . . . . ? P1 C1 C3 O2 33.1(13) . . . . ? C2 C1 C3 C40 49.9(13) . . . . ? P1 C1 C3 C40 -146.1(7) . . . . ? C70 P2 C5 C6 -68.6(8) . . . . ? C60 P2 C5 C6 56.5(8) . . . . ? C50 P2 C5 C6 173.4(7) . . . . ? C70 P2 C5 C7 97.1(7) . . . . ? C60 P2 C5 C7 -137.9(7) . . . . ? C50 P2 C5 C7 -20.9(9) . . . . ? C7 C5 C6 O3 -159.5(9) . . . . ? P2 C5 C6 O3 6.1(13) . . . . ? C7 C5 C6 C8 11.9(15) . . . . ? P2 C5 C6 C8 177.5(8) . . . . ? C6 C5 C7 O4 135.4(10) . . . . ? P2 C5 C7 O4 -29.0(12) . . . . ? C6 C5 C7 C80 -50.5(12) . . . . ? P2 C5 C7 C80 145.0(7) . . . . ? C1 P1 C10 C11 42.7(5) . . . . ? C30 P1 C10 C11 167.0(3) . . . . ? C20 P1 C10 C11 -80.3(4) . . . . ? C1 P1 C10 C15 -139.8(5) . . . . ? C30 P1 C10 C15 -15.4(5) . . . . ? C20 P1 C10 C15 97.2(4) . . . . ? C15 C10 C11 C12 0.0 . . . . ? P1 C10 C11 C12 177.6(5) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? P1 C10 C15 C14 -177.5(5) . . . . ? C1 P1 C20 C21 -93.8(5) . . . . ? C30 P1 C20 C21 139.0(3) . . . . ? C10 P1 C20 C21 25.4(4) . . . . ? C1 P1 C20 C25 85.0(5) . . . . ? C30 P1 C20 C25 -42.2(4) . . . . ? C10 P1 C20 C25 -155.8(3) . . . . ? C25 C20 C21 C22 0.0 . . . . ? P1 C20 C21 C22 178.8(5) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C21 C20 C25 C24 0.0 . . . . ? P1 C20 C25 C24 -178.8(5) . . . . ? C1 P1 C30 C31 -159.4(4) . . . . ? C10 P1 C30 C31 79.5(4) . . . . ? C20 P1 C30 C31 -31.9(4) . . . . ? C1 P1 C30 C35 24.4(5) . . . . ? C10 P1 C30 C35 -96.7(4) . . . . ? C20 P1 C30 C35 151.9(3) . . . . ? C35 C30 C31 C32 0.0 . . . . ? P1 C30 C31 C32 -176.2(3) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C30 0.0 . . . . ? C31 C30 C35 C34 0.0 . . . . ? P1 C30 C35 C34 176.2(3) . . . . ? O2 C3 C40 C41 49.7(10) . . . . ? C1 C3 C40 C41 -131.0(7) . . . . ? O2 C3 C40 C45 -127.3(8) . . . . ? C1 C3 C40 C45 51.9(9) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C3 C40 C41 C42 -177.0(6) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C3 C40 C45 C44 177.1(6) . . . . ? C5 P2 C50 C51 -43.6(6) . . . . ? C70 P2 C50 C51 -167.5(4) . . . . ? C60 P2 C50 C51 77.6(4) . . . . ? C5 P2 C50 C55 140.8(5) . . . . ? C70 P2 C50 C55 16.9(4) . . . . ? C60 P2 C50 C55 -98.0(4) . . . . ? C55 C50 C51 C52 0.0 . . . . ? P2 C50 C51 C52 -175.5(5) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? P2 C50 C55 C54 175.7(5) . . . . ? C5 P2 C60 C61 95.6(5) . . . . ? C70 P2 C60 C61 -135.8(3) . . . . ? C50 P2 C60 C61 -23.0(4) . . . . ? C5 P2 C60 C65 -84.8(5) . . . . ? C70 P2 C60 C65 43.9(4) . . . . ? C50 P2 C60 C65 156.6(3) . . . . ? C65 C60 C61 C62 0.0 . . . . ? P2 C60 C61 C62 179.7(5) . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C60 0.0 . . . . ? C61 C60 C65 C64 0.0 . . . . ? P2 C60 C65 C64 -179.7(5) . . . . ? C5 P2 C70 C71 152.8(4) . . . . ? C60 P2 C70 C71 25.6(4) . . . . ? C50 P2 C70 C71 -87.4(4) . . . . ? C5 P2 C70 C75 -26.6(4) . . . . ? C60 P2 C70 C75 -153.8(3) . . . . ? C50 P2 C70 C75 93.2(4) . . . . ? C75 C70 C71 C72 0.0 . . . . ? P2 C70 C71 C72 -179.4(4) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C71 C70 C75 C74 0.0 . . . . ? P2 C70 C75 C74 179.4(4) . . . . ? O4 C7 C80 C81 -44.1(10) . . . . ? C5 C7 C80 C81 141.8(6) . . . . ? O4 C7 C80 C85 129.5(8) . . . . ? C5 C7 C80 C85 -44.6(9) . . . . ? C85 C80 C81 C82 0.0 . . . . ? C7 C80 C81 C82 173.6(6) . . . . ? C80 C81 C82 C83 0.0 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C80 0.0 . . . . ? C81 C80 C85 C84 0.0 . . . . ? C7 C80 C85 C84 -173.5(6) . . . . ? _refine_diff_density_max 0.555 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.084 data_y2hgbr _database_code_CSD 167768 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 Br2 Hg O2 P' _chemical_formula_weight 782.84 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5287(6) _cell_length_b 11.6425(8) _cell_length_c 12.3992(8) _cell_angle_alpha 94.835(2) _cell_angle_beta 98.281(2) _cell_angle_gamma 102.172(2) _cell_volume 1321.22(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 8.933 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _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 13906 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.21 _reflns_number_total 6329 _reflns_number_gt 5606 _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 w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+2.8380P] 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 6329 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.386735(19) 0.081692(14) 0.404547(13) 0.02670(6) Uani 1 d . . . Br1 Br 0.35109(5) -0.13258(4) 0.41816(3) 0.02616(9) Uani 1 d . . . Br2 Br 0.30608(5) 0.26691(4) 0.42397(4) 0.03676(11) Uani 1 d . . . O1 O 0.5507(3) 0.1056(2) 0.2743(2) 0.0237(6) Uani 1 d . . . O2 O 0.7710(3) 0.2014(3) -0.0174(2) 0.0244(6) Uani 1 d . . . C1 C 0.6499(4) 0.1966(3) 0.1360(3) 0.0192(7) Uani 1 d . . . C2 C 0.5296(4) 0.1342(3) 0.1777(3) 0.0200(7) Uani 1 d . . . C3 C 0.6607(4) 0.2120(3) 0.0210(3) 0.0182(7) Uani 1 d . . . C4 C 0.3768(5) 0.0953(4) 0.1118(4) 0.0291(9) Uani 1 d . . . H4A H 0.3821 0.0886 0.0333 0.045(9) Uiso 1 calc R . . H4B H 0.3203 0.1538 0.1287 0.045(9) Uiso 1 calc R . . H4C H 0.3293 0.0183 0.1310 0.045(9) Uiso 1 calc R . . P1 P 0.81698(11) 0.22413(8) 0.22777(8) 0.01676(18) Uani 1 d . . . C10 C 0.9508(2) 0.33759(19) 0.1812(2) 0.0191(7) Uiso 1 d G . . C11 C 1.0947(3) 0.3303(2) 0.1823(2) 0.0271(9) Uiso 1 d G . . C12 C 1.1961(2) 0.4267(2) 0.1609(3) 0.0346(10) Uiso 1 d G . . C13 C 1.1536(3) 0.5305(2) 0.1383(3) 0.0355(10) Uiso 1 d G . . C14 C 1.0097(3) 0.53777(19) 0.1371(3) 0.0324(10) Uiso 1 d G . . C15 C 0.9082(2) 0.4413(2) 0.1586(2) 0.0263(8) Uiso 1 d G . . H11 H 1.1238 0.2594 0.1978 0.041(3) Uiso 1 calc G . . H12 H 1.2945 0.4218 0.1616 0.041(3) Uiso 1 d G . . H13 H 1.2229 0.5964 0.1236 0.041(3) Uiso 1 d G . . H14 H 0.9806 0.6087 0.1217 0.041(3) Uiso 1 d G . . H15 H 0.8099 0.4463 0.1578 0.041(3) Uiso 1 d G . . C20 C 0.8078(3) 0.2983(2) 0.36068(16) 0.0193(7) Uiso 1 d G . . C21 C 0.6958(2) 0.3549(2) 0.37423(18) 0.0256(8) Uiso 1 d G . . C22 C 0.6994(3) 0.4221(2) 0.4731(2) 0.0328(10) Uiso 1 d G . . C23 C 0.8149(3) 0.4326(2) 0.55849(17) 0.0311(9) Uiso 1 d G . . C24 C 0.9268(3) 0.3759(3) 0.54493(18) 0.0290(9) Uiso 1 d G . . C25 C 0.9233(2) 0.3087(2) 0.4460(2) 0.0237(8) Uiso 1 d G . . H21 H 0.6169 0.3478 0.3159 0.041(3) Uiso 1 calc G . . H22 H 0.6228 0.4609 0.4824 0.041(3) Uiso 1 d G . . H23 H 0.8173 0.4785 0.6261 0.041(3) Uiso 1 d G . . H24 H 1.0058 0.3831 0.6033 0.041(3) Uiso 1 d G . . H25 H 0.9998 0.2700 0.4368 0.041(3) Uiso 1 d G . . C30 C 0.8859(3) 0.09205(19) 0.2448(2) 0.0196(7) Uiso 1 d G . . C31 C 0.9441(3) 0.0441(2) 0.15969(17) 0.0288(9) Uiso 1 d G . . C32 C 0.9961(3) -0.0580(2) 0.1700(2) 0.0333(10) Uiso 1 d G . . C33 C 0.9900(3) -0.1122(2) 0.2654(2) 0.0320(9) Uiso 1 d G . . C34 C 0.9318(3) -0.0643(2) 0.35055(18) 0.0318(9) Uiso 1 d G . . C35 C 0.8798(3) 0.0378(2) 0.34025(18) 0.0244(8) Uiso 1 d G . . H31 H 0.9482 0.0812 0.0945 0.041(3) Uiso 1 calc G . . H32 H 1.0359 -0.0907 0.1118 0.041(3) Uiso 1 d G . . H33 H 1.0256 -0.1820 0.2724 0.041(3) Uiso 1 d G . . H34 H 0.9277 -0.1013 0.4158 0.041(3) Uiso 1 d G . . H35 H 0.8401 0.0706 0.3984 0.041(3) Uiso 1 d G . . C40 C 0.5409(3) 0.2499(2) -0.05208(19) 0.0209(7) Uiso 1 d G . . C41 C 0.5171(3) 0.2136(2) -0.1642(2) 0.0279(9) Uiso 1 d G . . C42 C 0.4169(3) 0.2553(3) -0.23440(16) 0.0333(10) Uiso 1 d G . . C43 C 0.3406(3) 0.3334(3) -0.1925(2) 0.0355(10) Uiso 1 d G . . C44 C 0.3645(3) 0.3697(2) -0.0804(2) 0.0341(10) Uiso 1 d G . . C45 C 0.4646(3) 0.3279(2) -0.01018(16) 0.0267(9) Uiso 1 d G . . H41 H 0.5692 0.1602 -0.1928 0.041(3) Uiso 1 calc G . . H42 H 0.4006 0.2305 -0.3110 0.041(3) Uiso 1 d G . . H43 H 0.2722 0.3619 -0.2405 0.041(3) Uiso 1 d G . . H44 H 0.3123 0.4230 -0.0517 0.041(3) Uiso 1 d G . . H45 H 0.4809 0.3527 0.0664 0.041(3) Uiso 1 d G . . 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 0.03223(10) 0.02762(9) 0.02511(9) 0.00945(6) 0.00884(6) 0.01230(6) Br1 0.0285(2) 0.02429(19) 0.0245(2) 0.00771(15) 0.00390(16) 0.00177(16) Br2 0.0314(2) 0.0315(2) 0.0508(3) 0.0055(2) 0.0044(2) 0.01602(18) O1 0.0265(15) 0.0236(14) 0.0218(14) 0.0052(11) 0.0069(11) 0.0041(11) O2 0.0241(14) 0.0302(15) 0.0203(13) 0.0026(11) 0.0061(11) 0.0077(12) C1 0.0179(18) 0.0210(18) 0.0182(18) 0.0032(14) 0.0007(14) 0.0042(14) C2 0.0241(19) 0.0153(16) 0.0216(18) 0.0027(14) 0.0056(15) 0.0057(14) C3 0.0222(19) 0.0150(16) 0.0163(17) -0.0005(13) 0.0024(14) 0.0034(14) C4 0.024(2) 0.025(2) 0.035(2) 0.0054(17) 0.0051(18) -0.0003(16) P1 0.0191(5) 0.0176(4) 0.0146(4) 0.0029(3) 0.0039(3) 0.0052(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 O1 2.397(3) . ? Hg1 Br2 2.4420(5) . ? Hg1 Br1 2.4693(5) . ? Hg1 Br1 2.9997(5) 2_656 ? Br1 Hg1 2.9997(5) 2_656 ? O1 C2 1.270(5) . ? O2 C3 1.239(5) . ? C1 C2 1.411(5) . ? C1 C3 1.468(5) . ? C1 P1 1.770(4) . ? C2 C4 1.520(6) . ? C3 C40 1.516(4) . ? P1 C30 1.811(2) . ? P1 C20 1.817(2) . ? P1 C10 1.826(2) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? 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 O1 Hg1 Br2 105.87(7) . . ? O1 Hg1 Br1 100.86(7) . . ? Br2 Hg1 Br1 151.064(18) . . ? O1 Hg1 Br1 87.67(7) . 2_656 ? Br2 Hg1 Br1 101.080(15) . 2_656 ? Br1 Hg1 Br1 90.761(13) . 2_656 ? Hg1 Br1 Hg1 89.239(13) . 2_656 ? C2 O1 Hg1 128.9(3) . . ? C2 C1 C3 127.6(3) . . ? C2 C1 P1 114.2(3) . . ? C3 C1 P1 115.9(3) . . ? O1 C2 C1 118.4(4) . . ? O1 C2 C4 118.0(4) . . ? C1 C2 C4 123.6(4) . . ? O2 C3 C1 121.2(3) . . ? O2 C3 C40 118.0(3) . . ? C1 C3 C40 120.6(3) . . ? C1 P1 C30 112.97(16) . . ? C1 P1 C20 112.61(15) . . ? C30 P1 C20 110.25(12) . . ? C1 P1 C10 109.49(16) . . ? C30 P1 C10 110.68(13) . . ? C20 P1 C10 100.12(13) . . ? C11 C10 C15 120.0 . . ? C11 C10 P1 122.79(15) . . ? C15 C10 P1 116.60(15) . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C10 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 P1 120.92(14) . . ? C25 C20 P1 118.71(14) . . ? C22 C21 C20 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 P1 118.77(14) . . ? C35 C30 P1 121.23(15) . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C34 C35 C30 120.0 . . ? C41 C40 C45 120.0 . . ? C41 C40 C3 118.7(2) . . ? C45 C40 C3 121.0(2) . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C40 120.0 . . ? 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 O1 Hg1 Br1 Hg1 87.78(7) . . . 2_656 ? Br2 Hg1 Br1 Hg1 -114.91(3) . . . 2_656 ? Br1 Hg1 Br1 Hg1 0.0 2_656 . . 2_656 ? Br2 Hg1 O1 C2 -54.5(3) . . . . ? Br1 Hg1 O1 C2 114.3(3) . . . . ? Br1 Hg1 O1 C2 -155.3(3) 2_656 . . . ? Hg1 O1 C2 C1 149.9(3) . . . . ? Hg1 O1 C2 C4 -32.2(5) . . . . ? C3 C1 C2 O1 162.9(4) . . . . ? P1 C1 C2 O1 0.8(5) . . . . ? C3 C1 C2 C4 -14.8(6) . . . . ? P1 C1 C2 C4 -176.9(3) . . . . ? C2 C1 C3 O2 -136.3(4) . . . . ? P1 C1 C3 O2 25.5(5) . . . . ? C2 C1 C3 C40 48.0(5) . . . . ? P1 C1 C3 C40 -150.2(3) . . . . ? C2 C1 P1 C30 71.6(3) . . . . ? C3 C1 P1 C30 -92.7(3) . . . . ? C2 C1 P1 C20 -54.1(3) . . . . ? C3 C1 P1 C20 141.6(3) . . . . ? C2 C1 P1 C10 -164.6(3) . . . . ? C3 C1 P1 C10 31.2(3) . . . . ? C1 P1 C10 C11 -137.77(19) . . . . ? C30 P1 C10 C11 -12.6(2) . . . . ? C20 P1 C10 C11 103.70(17) . . . . ? C1 P1 C10 C15 51.2(2) . . . . ? C30 P1 C10 C15 176.34(15) . . . . ? C20 P1 C10 C15 -67.36(17) . . . . ? C15 C10 C11 C12 0.0 . . . . ? P1 C10 C11 C12 -170.8(2) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? P1 C10 C15 C14 171.3(2) . . . . ? C1 P1 C20 C21 -17.0(2) . . . . ? C30 P1 C20 C21 -144.17(16) . . . . ? C10 P1 C20 C21 99.20(17) . . . . ? C1 P1 C20 C25 170.04(18) . . . . ? C30 P1 C20 C25 42.87(19) . . . . ? C10 P1 C20 C25 -73.76(17) . . . . ? C25 C20 C21 C22 0.0 . . . . ? P1 C20 C21 C22 -172.9(2) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C21 C20 C25 C24 0.0 . . . . ? P1 C20 C25 C24 173.0(2) . . . . ? C1 P1 C30 C31 73.1(2) . . . . ? C20 P1 C30 C31 -159.88(16) . . . . ? C10 P1 C30 C31 -50.04(19) . . . . ? C1 P1 C30 C35 -106.1(2) . . . . ? C20 P1 C30 C35 20.9(2) . . . . ? C10 P1 C30 C35 130.76(17) . . . . ? C35 C30 C31 C32 0.0 . . . . ? P1 C30 C31 C32 -179.2(2) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C30 0.0 . . . . ? C31 C30 C35 C34 0.0 . . . . ? P1 C30 C35 C34 179.2(2) . . . . ? O2 C3 C40 C41 33.2(4) . . . . ? C1 C3 C40 C41 -150.9(3) . . . . ? O2 C3 C40 C45 -141.1(3) . . . . ? C1 C3 C40 C45 34.8(4) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C3 C40 C41 C42 -174.4(3) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C3 C40 C45 C44 174.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.239 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.135 data_y2hgi _database_code_CSD 167769 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 Hg I2 O2 P' _chemical_formula_weight 876.82 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9528(2) _cell_length_b 11.7157(3) _cell_length_c 13.8223(2) _cell_angle_alpha 107.6152(12) _cell_angle_beta 91.6914(4) _cell_angle_gamma 99.4180(4) _cell_volume 1358.37(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 8.020 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 14475 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6554 _reflns_number_gt 5663 _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 w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+5.4417P] 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 6554 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.09549(2) 0.176756(16) 0.059209(14) 0.02926(6) Uani 1 d . . . I1 I -0.22319(3) 0.02083(3) -0.03074(2) 0.02500(7) Uani 1 d . . . I2 I 0.12099(5) 0.39569(3) 0.04316(3) 0.04157(10) Uani 1 d . . . P1 P -0.25570(12) 0.19825(9) 0.33641(8) 0.0159(2) Uani 1 d . . . O1 O -0.0190(3) 0.1917(3) 0.2140(2) 0.0234(6) Uani 1 d . . . O2 O 0.0921(4) 0.3925(3) 0.5232(2) 0.0312(8) Uani 1 d . . . C1 C -0.0632(5) 0.2508(4) 0.3837(3) 0.0192(8) Uani 1 d . . . C2 C 0.0368(5) 0.2454(4) 0.3051(3) 0.0216(9) Uani 1 d . . . C3 C -0.0117(5) 0.3052(4) 0.4920(3) 0.0201(8) Uani 1 d . . . C4 C 0.2031(6) 0.2941(5) 0.3249(4) 0.0375(12) Uani 1 d . . . H4A H 0.2369 0.2983 0.3942 0.065(12) Uiso 1 calc R . . H4B H 0.2239 0.3758 0.3178 0.065(12) Uiso 1 calc R . . H4C H 0.2578 0.2403 0.2758 0.065(12) Uiso 1 calc R . . C10 C -0.3034(3) 0.2783(2) 0.24820(19) 0.0176(8) Uiso 1 d G . . C11 C -0.4134(3) 0.22400(19) 0.1670(2) 0.0246(9) Uiso 1 d G . . C12 C -0.4490(3) 0.2887(3) 0.10281(19) 0.0295(10) Uiso 1 d G . . C13 C -0.3746(3) 0.4077(2) 0.1198(2) 0.0288(10) Uiso 1 d G . . C14 C -0.2646(3) 0.46207(19) 0.2011(2) 0.0286(10) Uiso 1 d G . . C15 C -0.2290(3) 0.3974(2) 0.26523(19) 0.0241(9) Uiso 1 d G . . H11 H -0.4632 0.1444 0.1556 0.035(3) Uiso 1 calc G . . H12 H -0.5226 0.2523 0.0485 0.035(3) Uiso 1 d G . . H13 H -0.3984 0.4510 0.0769 0.035(3) Uiso 1 d G . . H14 H -0.2148 0.5417 0.2124 0.035(3) Uiso 1 d G . . H15 H -0.1554 0.4337 0.3196 0.035(3) Uiso 1 d G . . C20 C -0.3049(3) 0.03426(17) 0.2740(2) 0.0181(8) Uiso 1 d G . . C21 C -0.4530(3) -0.0232(2) 0.2372(2) 0.0215(9) Uiso 1 d G . . C22 C -0.4844(2) -0.1476(2) 0.1862(2) 0.0251(9) Uiso 1 d G . . C23 C -0.3677(3) -0.21452(17) 0.1720(2) 0.0251(9) Uiso 1 d G . . C24 C -0.2196(3) -0.1570(2) 0.2088(2) 0.0238(9) Uiso 1 d G . . C25 C -0.1881(2) -0.0326(2) 0.2598(2) 0.0223(9) Uiso 1 d G . . H21 H -0.5311 0.0216 0.2466 0.035(3) Uiso 1 calc G . . H22 H -0.5836 -0.1861 0.1615 0.035(3) Uiso 1 d G . . H23 H -0.3888 -0.2978 0.1379 0.035(3) Uiso 1 d G . . H24 H -0.1415 -0.2018 0.1994 0.035(3) Uiso 1 d G . . H25 H -0.0890 0.0058 0.2845 0.035(3) Uiso 1 d G . . C30 C -0.3770(3) 0.2392(2) 0.44037(19) 0.0183(8) Uiso 1 d G . . C31 C -0.3745(3) 0.3622(2) 0.4889(2) 0.0218(9) Uiso 1 d G . . C32 C -0.4654(3) 0.39805(18) 0.5685(2) 0.0253(9) Uiso 1 d G . . C33 C -0.5588(3) 0.3109(2) 0.5994(2) 0.0278(10) Uiso 1 d G . . C34 C -0.5612(3) 0.1878(2) 0.5509(2) 0.0279(10) Uiso 1 d G . . C35 C -0.4704(3) 0.15196(17) 0.4714(2) 0.0240(9) Uiso 1 d G . . H31 H -0.3121 0.4205 0.4682 0.035(3) Uiso 1 calc G . . H32 H -0.4638 0.4804 0.6009 0.035(3) Uiso 1 d G . . H33 H -0.6196 0.3348 0.6527 0.035(3) Uiso 1 d G . . H34 H -0.6237 0.1294 0.5716 0.035(3) Uiso 1 d G . . H35 H -0.4720 0.0696 0.4389 0.035(3) Uiso 1 d G . . C40 C -0.0803(3) 0.2457(2) 0.56780(19) 0.0211(8) Uiso 1 d G . . C41 C -0.0936(4) 0.31804(18) 0.6664(2) 0.0255(9) Uiso 1 d G . . C42 C -0.1378(4) 0.2643(2) 0.74036(17) 0.0313(10) Uiso 1 d G . . C43 C -0.1686(4) 0.1381(2) 0.71580(19) 0.0293(10) Uiso 1 d G . . C44 C -0.1553(4) 0.06580(18) 0.6172(2) 0.0266(10) Uiso 1 d G . . C45 C -0.1111(4) 0.1196(2) 0.54325(17) 0.0238(9) Uiso 1 d G . . H41 H -0.0730 0.4024 0.6828 0.035(3) Uiso 1 calc G . . H42 H -0.1467 0.3127 0.8063 0.035(3) Uiso 1 d G . . H43 H -0.1982 0.1022 0.7653 0.035(3) Uiso 1 d G . . H44 H -0.1760 -0.0186 0.6008 0.035(3) Uiso 1 d G . . H45 H -0.1022 0.0712 0.4773 0.035(3) Uiso 1 d G . . 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 0.04346(12) 0.02241(9) 0.02398(10) 0.00896(7) 0.00887(8) 0.00744(8) I1 0.02220(14) 0.02524(14) 0.02690(16) 0.00646(12) -0.00284(11) 0.00655(11) I2 0.0624(2) 0.02412(16) 0.0455(2) 0.01621(15) 0.02015(18) 0.01548(16) P1 0.0158(5) 0.0165(5) 0.0152(5) 0.0047(4) 0.0009(4) 0.0026(4) O1 0.0220(16) 0.0301(16) 0.0165(15) 0.0046(13) 0.0027(12) 0.0046(13) O2 0.035(2) 0.0285(17) 0.0199(16) 0.0004(14) -0.0012(14) -0.0086(15) C1 0.018(2) 0.0197(19) 0.019(2) 0.0060(17) 0.0013(16) 0.0009(16) C2 0.022(2) 0.022(2) 0.020(2) 0.0056(18) 0.0010(17) 0.0021(17) C3 0.020(2) 0.020(2) 0.019(2) 0.0039(17) 0.0006(16) 0.0048(16) C4 0.020(2) 0.053(3) 0.030(3) 0.005(2) 0.001(2) -0.003(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 O1 2.370(3) . ? Hg1 I2 2.6146(4) . ? Hg1 I1 2.6761(3) 2 ? Hg1 I1 3.1198(4) . ? I1 Hg1 2.6761(3) 2 ? P1 C1 1.766(4) . ? P1 C30 1.822(2) . ? P1 C20 1.824(2) . ? P1 C10 1.828(2) . ? O1 C2 1.269(5) . ? O2 C3 1.223(5) . ? C1 C2 1.422(6) . ? C1 C3 1.465(6) . ? C2 C4 1.490(6) . ? C3 C40 1.517(5) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? 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 O1 Hg1 I2 104.05(8) . . ? O1 Hg1 I1 102.80(8) . 2 ? I2 Hg1 I1 146.317(13) . 2 ? O1 Hg1 I1 81.37(8) . . ? I2 Hg1 I1 111.303(13) . . ? I1 Hg1 I1 92.488(10) 2 . ? Hg1 I1 Hg1 87.512(10) 2 . ? C1 P1 C30 109.57(17) . . ? C1 P1 C20 114.29(17) . . ? C30 P1 C20 108.20(13) . . ? C1 P1 C10 109.28(16) . . ? C30 P1 C10 105.50(14) . . ? C20 P1 C10 109.62(13) . . ? C2 O1 Hg1 129.6(3) . . ? C2 C1 C3 122.9(4) . . ? C2 C1 P1 112.8(3) . . ? C3 C1 P1 124.1(3) . . ? O1 C2 C1 117.6(4) . . ? O1 C2 C4 119.0(4) . . ? C1 C2 C4 123.3(4) . . ? O2 C3 C1 122.4(4) . . ? O2 C3 C40 118.2(4) . . ? C1 C3 C40 119.2(3) . . ? C11 C10 C15 120.0 . . ? C11 C10 P1 121.63(15) . . ? C15 C10 P1 118.35(15) . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C10 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 P1 121.88(15) . . ? C25 C20 P1 118.06(15) . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 P1 117.82(15) . . ? C35 C30 P1 122.18(15) . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C30 120.0 . . ? C41 C40 C45 120.0 . . ? C41 C40 C3 119.2(2) . . ? C45 C40 C3 120.3(2) . . ? C40 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 C40 120.0 . . ? 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 O1 Hg1 I1 Hg1 -102.57(8) . . . 2 ? I2 Hg1 I1 Hg1 155.635(13) . . . 2 ? I1 Hg1 I1 Hg1 0.0 2 . . 2 ? I2 Hg1 O1 C2 -71.5(4) . . . . ? I1 Hg1 O1 C2 88.0(4) 2 . . . ? I1 Hg1 O1 C2 178.6(4) . . . . ? C30 P1 C1 C2 -167.6(3) . . . . ? C20 P1 C1 C2 70.8(3) . . . . ? C10 P1 C1 C2 -52.4(3) . . . . ? C30 P1 C1 C3 6.8(4) . . . . ? C20 P1 C1 C3 -114.8(3) . . . . ? C10 P1 C1 C3 122.0(3) . . . . ? Hg1 O1 C2 C1 173.4(3) . . . . ? Hg1 O1 C2 C4 -9.4(6) . . . . ? C3 C1 C2 O1 177.2(4) . . . . ? P1 C1 C2 O1 -8.3(5) . . . . ? C3 C1 C2 C4 0.1(7) . . . . ? P1 C1 C2 C4 174.6(4) . . . . ? C2 C1 C3 O2 33.6(7) . . . . ? P1 C1 C3 O2 -140.2(4) . . . . ? C2 C1 C3 C40 -141.3(4) . . . . ? P1 C1 C3 C40 44.8(5) . . . . ? C1 P1 C10 C11 149.9(2) . . . . ? C30 P1 C10 C11 -92.32(19) . . . . ? C20 P1 C10 C11 24.0(2) . . . . ? C1 P1 C10 C15 -31.4(2) . . . . ? C30 P1 C10 C15 86.30(18) . . . . ? C20 P1 C10 C15 -157.41(16) . . . . ? C15 C10 C11 C12 0.0 . . . . ? P1 C10 C11 C12 178.6(2) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? P1 C10 C15 C14 -178.6(2) . . . . ? C1 P1 C20 C21 176.6(2) . . . . ? C30 P1 C20 C21 54.2(2) . . . . ? C10 P1 C20 C21 -60.4(2) . . . . ? C1 P1 C20 C25 -6.2(2) . . . . ? C30 P1 C20 C25 -128.52(17) . . . . ? C10 P1 C20 C25 116.91(17) . . . . ? C25 C20 C21 C22 0.0 . . . . ? P1 C20 C21 C22 177.2(2) . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C21 C20 C25 C24 0.0 . . . . ? P1 C20 C25 C24 -177.3(2) . . . . ? C1 P1 C30 C31 64.1(2) . . . . ? C20 P1 C30 C31 -170.71(16) . . . . ? C10 P1 C30 C31 -53.45(19) . . . . ? C1 P1 C30 C35 -116.1(2) . . . . ? C20 P1 C30 C35 9.1(2) . . . . ? C10 P1 C30 C35 126.35(18) . . . . ? C35 C30 C31 C32 0.0 . . . . ? P1 C30 C31 C32 179.8(2) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C30 0.0 . . . . ? C31 C30 C35 C34 0.0 . . . . ? P1 C30 C35 C34 -179.8(2) . . . . ? O2 C3 C40 C41 35.9(5) . . . . ? C1 C3 C40 C41 -148.9(3) . . . . ? O2 C3 C40 C45 -135.8(4) . . . . ? C1 C3 C40 C45 39.3(4) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C3 C40 C41 C42 -171.8(3) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C3 C40 C45 C44 171.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 4.180 _refine_diff_density_min -2.055 _refine_diff_density_rms 0.140