# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'de Namor,Angela F. Danil' 'Eduardo E. Castellano' 'Samir Chahine' 'H. Donald Brooke Jenkins' 'Oscar E. Piro' _publ_contact_author_name 'Prof Angela Danil de Namor' _publ_contact_author_address ; Department of Chemistry University of Surrey Guildford Surrey GU2 7XH UNITED KINGDOM ; _publ_contact_author_phone '(01483) 689581' _publ_contact_author_fax '(01483) 686851' _publ_contact_author_email A.Danil-De-Namor@surrey.ac.uk _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Preliminary Observation of Additive Thermodynamic Contribution of Pendant Arms to the Complexation of Calixarene Derivatives with Mercury (II) ; data_HgL(ClO4)2.2MeCN _database_code_depnum_ccdc_archive 'CCDC 270136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mercury(II) 5,11,17,23,tetra-tert-butyl[25,27-bis(hydroxy)-26,28- bis(ethylthioethoxy)]-calix(4)arene perchlorate diacetonitrile ; _chemical_name_common ? _chemical_formula_moiety HgL(ClO4)2.2MeCN _chemical_formula_sum 'C56 H76 Cl2 Hg N2 O12 S2' _chemical_formula_weight 1304.80 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 21.794(1) _cell_length_b 45.754(1) _cell_length_c 12.395(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12359.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 42375 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.061 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5344 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.120 -1 0 0 0.100 0 1 0 0.022 0 -1 0 0.083 0 0 1 0.042 0 0 -1 0.019 _exptl_absorpt_coefficient_mu 2.702 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; P. Coppens, L. Leiserowitz and D. Rabinovich, Acta Crystallogr. 1965, 18, 1035-1038. ; _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.852 _exptl_special_details ; Spek, A. L. Acta Crystallogr., Sect A 1990, 46, C34. ; _diffrn_ambient_temperature 100(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 'Enraf-Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 42375 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10851 _reflns_number_gt 7660 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+155.2410P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10851 _refine_ls_number_parameters 673 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 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 Hg Hg 0.405157(17) 0.037624(8) 0.76749(3) 0.03060(14) Uani 1 d . . . C11 C 0.5635(5) 0.0789(2) 0.7860(10) 0.038(3) Uani 1 d . . . C12 C 0.5939(5) 0.0777(2) 0.6872(10) 0.037(3) Uani 1 d . . . C13 C 0.6574(5) 0.0766(2) 0.6858(10) 0.036(3) Uani 1 d . . . H13 H 0.6778 0.0751 0.6183 0.043 Uiso 1 calc R . . C14 C 0.6926(5) 0.0777(2) 0.7798(9) 0.036(2) Uani 1 d . . . C15 C 0.6604(5) 0.0801(2) 0.8763(10) 0.041(3) Uani 1 d . . . H15 H 0.6832 0.0815 0.9414 0.049 Uiso 1 calc R . . C16 C 0.5968(5) 0.0806(2) 0.8833(9) 0.035(2) Uani 1 d . . . C17 C 0.7630(5) 0.0764(2) 0.7714(8) 0.037(2) Uani 1 d . . . C18 C 0.7815(6) 0.0487(3) 0.7121(12) 0.064(4) Uani 1 d . . . H18A H 0.7649 0.0492 0.6387 0.096 Uiso 1 calc R . . H18B H 0.7653 0.0317 0.7504 0.096 Uiso 1 calc R . . H18C H 0.8264 0.0475 0.7091 0.096 Uiso 1 calc R . . C19 C 0.7929(5) 0.0752(3) 0.8856(10) 0.055(3) Uani 1 d . . . H19A H 0.8373 0.0725 0.8782 0.083 Uiso 1 calc R . . H19B H 0.7755 0.0588 0.9263 0.083 Uiso 1 calc R . . H19C H 0.7847 0.0935 0.9240 0.083 Uiso 1 calc R . . C110 C 0.7859(5) 0.1031(3) 0.7152(10) 0.050(3) Uani 1 d . . . H11A H 0.7713 0.1031 0.6404 0.076 Uiso 1 calc R . . H11B H 0.8308 0.1032 0.7159 0.076 Uiso 1 calc R . . H11C H 0.7705 0.1206 0.7523 0.076 Uiso 1 calc R . . O1 O 0.4997(3) 0.07883(15) 0.7855(6) 0.0407(18) Uani 1 d . . . C12' C 0.5569(5) 0.0791(2) 0.5828(9) 0.038(3) Uani 1 d . . . H12A H 0.5814 0.0713 0.5222 0.046 Uiso 1 calc R . . H12B H 0.5192 0.0672 0.5897 0.046 Uiso 1 calc R . . C21 C 0.4796(4) 0.1210(2) 0.5617(8) 0.032(2) Uani 1 d . . . C22 C 0.4652(5) 0.1506(2) 0.5500(7) 0.029(2) Uani 1 d . . . C23 C 0.5134(5) 0.1699(2) 0.5334(8) 0.038(3) Uani 1 d . . . H23 H 0.5046 0.1902 0.5266 0.045 Uiso 1 calc R . . C24 C 0.5743(5) 0.1608(2) 0.5263(9) 0.035(2) Uani 1 d . . . C25 C 0.5866(5) 0.1314(2) 0.5426(9) 0.035(2) Uani 1 d . . . H25 H 0.6280 0.1249 0.5410 0.042 Uiso 1 calc R . . C26 C 0.5401(4) 0.1107(2) 0.5614(8) 0.034(2) Uani 1 d . . . C27 C 0.6277(5) 0.1828(2) 0.5103(10) 0.045(3) Uani 1 d . . . C28 C 0.6824(6) 0.1681(3) 0.4564(15) 0.081(5) Uani 1 d . . . H28A H 0.7132 0.1828 0.4378 0.121 Uiso 1 calc R . . H28B H 0.6687 0.1581 0.3906 0.121 Uiso 1 calc R . . H28C H 0.7003 0.1537 0.5060 0.121 Uiso 1 calc R . . C29 C 0.6445(8) 0.1956(4) 0.6171(13) 0.098(6) Uani 1 d . . . H29A H 0.6783 0.2095 0.6077 0.147 Uiso 1 calc R . . H29B H 0.6575 0.1799 0.6660 0.147 Uiso 1 calc R . . H29C H 0.6089 0.2057 0.6477 0.147 Uiso 1 calc R . . C210 C 0.6053(7) 0.2074(3) 0.4347(13) 0.073(4) Uani 1 d . . . H21A H 0.6391 0.2210 0.4208 0.109 Uiso 1 calc R . . H21B H 0.5712 0.2179 0.4689 0.109 Uiso 1 calc R . . H21C H 0.5914 0.1989 0.3664 0.109 Uiso 1 calc R . . O2 O 0.4325(3) 0.10086(13) 0.5833(5) 0.0274(15) Uani 1 d . . . C211 C 0.4045(5) 0.0894(2) 0.4870(8) 0.033(2) Uani 1 d . . . H21D H 0.4364 0.0822 0.4367 0.039 Uiso 1 calc R . . H21E H 0.3804 0.1048 0.4503 0.039 Uiso 1 calc R . . C212 C 0.3629(5) 0.0644(2) 0.5210(8) 0.032(2) Uani 1 d . . . H21F H 0.3392 0.0573 0.4580 0.038 Uiso 1 calc R . . H21G H 0.3335 0.0712 0.5763 0.038 Uiso 1 calc R . . S2 S 0.40971(11) 0.03461(5) 0.57585(16) 0.0250(5) Uani 1 d . . . C213 C 0.3614(5) 0.0035(2) 0.5397(8) 0.031(2) Uani 1 d . . . H21H H 0.3698 -0.0131 0.5888 0.037 Uiso 1 calc R . . H21I H 0.3176 0.0088 0.5466 0.037 Uiso 1 calc R . . C214 C 0.3753(5) -0.0052(2) 0.4249(7) 0.036(3) Uani 1 d . . . H21J H 0.3699 0.0117 0.3774 0.055 Uiso 1 calc R . . H21K H 0.3474 -0.0209 0.4026 0.055 Uiso 1 calc R . . H21L H 0.4178 -0.0122 0.4200 0.055 Uiso 1 calc R . . C23' C 0.4004(5) 0.1620(2) 0.5633(8) 0.034(2) Uani 1 d . . . H23A H 0.3905 0.1753 0.5028 0.041 Uiso 1 calc R . . H23B H 0.3713 0.1454 0.5607 0.041 Uiso 1 calc R . . C31 C 0.3916(4) 0.1620(2) 0.7661(8) 0.030(2) Uani 1 d . . . C32 C 0.3876(4) 0.1770(2) 0.8656(8) 0.029(2) Uani 1 d . . . C33 C 0.3836(5) 0.2070(2) 0.8649(8) 0.031(2) Uani 1 d . . . H33 H 0.3802 0.2168 0.9321 0.037 Uiso 1 calc R . . C34 C 0.3843(5) 0.2235(2) 0.7709(9) 0.037(2) Uani 1 d . . . C35 C 0.3885(5) 0.2082(2) 0.6731(9) 0.034(2) Uani 1 d . . . H35 H 0.3885 0.2189 0.6075 0.041 Uiso 1 calc R . . C36 C 0.3926(4) 0.1780(2) 0.6683(7) 0.028(2) Uani 1 d . . . C37 C 0.3860(6) 0.2575(2) 0.7788(11) 0.050(3) Uani 1 d . . . C38 C 0.3353(7) 0.2684(2) 0.8490(11) 0.064(4) Uani 1 d . . . H38A H 0.3392 0.2896 0.8579 0.095 Uiso 1 calc R . . H38B H 0.3377 0.2589 0.9197 0.095 Uiso 1 calc R . . H38C H 0.2957 0.2639 0.8154 0.095 Uiso 1 calc R . . C39 C 0.3899(11) 0.2705(3) 0.6725(11) 0.121(9) Uani 1 d . . . H39A H 0.3527 0.2658 0.6315 0.182 Uiso 1 calc R . . H39B H 0.4258 0.2628 0.6346 0.182 Uiso 1 calc R . . H39C H 0.3937 0.2918 0.6794 0.182 Uiso 1 calc R . . C310 C 0.4464(7) 0.2665(3) 0.8405(12) 0.067(4) Uani 1 d . . . H31A H 0.4822 0.2595 0.8002 0.101 Uiso 1 calc R . . H31B H 0.4463 0.2577 0.9126 0.101 Uiso 1 calc R . . H31C H 0.4482 0.2878 0.8471 0.101 Uiso 1 calc R . . O3 O 0.3954(3) 0.13222(14) 0.7678(5) 0.0338(16) Uani 1 d . . . C34' C 0.3908(4) 0.1595(2) 0.9694(8) 0.031(2) Uani 1 d . . . H34A H 0.3658 0.1415 0.9623 0.037 Uiso 1 calc R . . H34B H 0.3742 0.1711 1.0300 0.037 Uiso 1 calc R . . C41 C 0.4783(5) 0.1228(2) 0.9871(8) 0.030(2) Uani 1 d . . . C42 C 0.5406(5) 0.1158(2) 1.0005(8) 0.033(2) Uani 1 d . . . C43 C 0.5811(4) 0.1386(2) 1.0171(8) 0.035(2) Uani 1 d . . . H43 H 0.6236 0.1344 1.0227 0.042 Uiso 1 calc R . . C44 C 0.5624(5) 0.1673(2) 1.0259(9) 0.037(2) Uani 1 d . . . C45 C 0.5001(5) 0.1731(2) 1.0112(8) 0.037(2) Uani 1 d . . . H45 H 0.4864 0.1928 1.0147 0.044 Uiso 1 calc R . . C46 C 0.4574(4) 0.1514(2) 0.9920(7) 0.028(2) Uani 1 d . . . C47 C 0.6096(5) 0.1925(3) 1.0434(10) 0.046(3) Uani 1 d . . . C48 C 0.6623(7) 0.1816(3) 1.1186(14) 0.082(5) Uani 1 d . . . H48A H 0.6448 0.1742 1.1860 0.124 Uiso 1 calc R . . H48B H 0.6902 0.1979 1.1344 0.124 Uiso 1 calc R . . H48C H 0.6850 0.1659 1.0825 0.124 Uiso 1 calc R . . C49 C 0.6353(8) 0.2005(4) 0.9340(13) 0.088(5) Uani 1 d . . . H49A H 0.6605 0.1843 0.9069 0.132 Uiso 1 calc R . . H49B H 0.6606 0.2181 0.9404 0.132 Uiso 1 calc R . . H49C H 0.6015 0.2041 0.8837 0.132 Uiso 1 calc R . . C410 C 0.5801(6) 0.2184(3) 1.0999(14) 0.072(5) Uani 1 d . . . H41C H 0.5502 0.2276 1.0516 0.108 Uiso 1 calc R . . H41D H 0.6119 0.2327 1.1190 0.108 Uiso 1 calc R . . H41E H 0.5594 0.2117 1.1655 0.108 Uiso 1 calc R . . O4 O 0.4370(3) 0.09993(13) 0.9624(5) 0.0296(15) Uani 1 d . . . C411 C 0.4059(5) 0.0884(2) 1.0552(7) 0.030(2) Uani 1 d . . . H41F H 0.3805 0.1037 1.0896 0.036 Uiso 1 calc R . . H41G H 0.4359 0.0811 1.1088 0.036 Uiso 1 calc R . . C412 C 0.3658(4) 0.0636(2) 1.0158(8) 0.029(2) Uani 1 d . . . H41H H 0.3372 0.0709 0.9598 0.035 Uiso 1 calc R . . H41I H 0.3412 0.0558 1.0764 0.035 Uiso 1 calc R . . S4 S 0.41427(11) 0.03445(5) 0.9591(2) 0.0292(5) Uani 1 d . . . C413 C 0.3707(5) 0.0017(2) 0.9990(9) 0.038(3) Uani 1 d . . . H41J H 0.3262 0.0051 0.9879 0.046 Uiso 1 calc R . . H41K H 0.3832 -0.0152 0.9542 0.046 Uiso 1 calc R . . C414 C 0.3834(6) -0.0047(2) 1.1182(10) 0.051(3) Uani 1 d . . . H41L H 0.4268 -0.0096 1.1276 0.077 Uiso 1 calc R . . H41M H 0.3580 -0.0212 1.1418 0.077 Uiso 1 calc R . . H41N H 0.3734 0.0126 1.1615 0.077 Uiso 1 calc R . . C41' C 0.5638(5) 0.0848(2) 0.9891(9) 0.037(3) Uani 1 d . . . H41A H 0.5922 0.0804 1.0493 0.044 Uiso 1 calc R . . H41B H 0.5288 0.0711 0.9934 0.044 Uiso 1 calc R . . Cl1 Cl 0.4788(2) -0.03644(12) 0.7244(4) 0.0299(9) Uani 0.687(12) d PG A 1 O11 O 0.4826(4) -0.0202(2) 0.6251(6) 0.067(4) Uiso 0.687(12) d PG A 1 O12 O 0.4591(4) -0.0174(2) 0.8100(6) 0.066(4) Uiso 0.687(12) d PG A 1 O13 O 0.4353(4) -0.05990(16) 0.7121(8) 0.066(4) Uiso 0.687(12) d PG A 1 O14 O 0.5382(3) -0.0483(2) 0.7502(7) 0.041(2) Uiso 0.687(12) d PG A 1 Cl1' Cl 0.4877(6) -0.0365(3) 0.7373(10) 0.0299(9) Uani 0.313(12) d PG A 2 O11' O 0.4865(10) -0.0052(3) 0.724(2) 0.078(10) Uiso 0.313(12) d PG A 2 O12' O 0.4645(11) -0.0439(5) 0.8426(11) 0.084(11) Uiso 0.313(12) d PG A 2 O13' O 0.4499(9) -0.0499(5) 0.6559(14) 0.060(8) Uiso 0.313(12) d PG A 2 O14' O 0.5498(7) -0.0468(5) 0.7268(18) 0.041(2) Uiso 0.313(12) d PG A 2 Cl2 Cl 0.24946(12) 0.04857(6) 0.7725(2) 0.0430(6) Uani 1 d . . . O21 O 0.3025(3) 0.06883(17) 0.7723(6) 0.0453(19) Uani 1 d . . . O22 O 0.2512(4) 0.03072(19) 0.6804(8) 0.065(3) Uani 1 d . . . O23 O 0.2540(4) 0.03062(19) 0.8679(7) 0.062(2) Uani 1 d . . . O24 O 0.1940(3) 0.0650(2) 0.7741(7) 0.055(2) Uani 1 d . . . N5 N 0.2534(6) 0.1188(3) 0.5696(15) 0.093(5) Uani 1 d . . . C51 C 0.2478(7) 0.1274(3) 0.6630(18) 0.076(5) Uani 1 d . . . C52 C 0.2422(6) 0.1362(4) 0.7760(14) 0.086(5) Uani 1 d . . . H52A H 0.1993 0.1345 0.7987 0.129 Uiso 1 calc R . . H52B H 0.2559 0.1564 0.7841 0.129 Uiso 1 calc R . . H52C H 0.2678 0.1234 0.8209 0.129 Uiso 1 calc R . . N6 N 0.4065(5) 0.1534(3) 0.2744(8) 0.057(3) Uani 1 d . . . C61 C 0.4523(6) 0.1420(2) 0.2743(9) 0.042(3) Uani 1 d . . . C62 C 0.5124(6) 0.1281(3) 0.2769(9) 0.049(3) Uani 1 d . . . H62A H 0.5333 0.1331 0.3444 0.074 Uiso 1 calc R . . H62B H 0.5369 0.1349 0.2156 0.074 Uiso 1 calc R . . H62C H 0.5074 0.1068 0.2725 0.074 Uiso 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 Hg 0.0310(2) 0.0353(2) 0.0254(2) -0.00802(17) -0.00499(16) 0.00385(17) C11 0.030(6) 0.017(5) 0.068(8) -0.010(5) 0.000(5) 0.013(4) C12 0.030(6) 0.021(5) 0.061(7) -0.011(5) -0.018(6) 0.006(5) C13 0.031(6) 0.015(5) 0.061(7) -0.012(5) -0.012(5) 0.006(4) C14 0.029(5) 0.019(5) 0.058(7) -0.013(5) -0.007(5) 0.008(4) C15 0.046(7) 0.020(5) 0.057(7) -0.008(5) -0.014(6) 0.006(5) C16 0.027(5) 0.017(5) 0.061(7) -0.007(5) -0.014(5) 0.001(4) C17 0.034(6) 0.037(6) 0.038(6) -0.013(5) -0.010(5) 0.001(5) C18 0.052(8) 0.056(8) 0.084(10) -0.025(7) -0.025(7) 0.019(7) C19 0.035(7) 0.059(8) 0.071(9) -0.009(7) -0.017(6) 0.006(6) C110 0.039(6) 0.048(7) 0.063(8) -0.007(6) -0.009(6) -0.005(6) O1 0.029(4) 0.036(4) 0.057(5) -0.006(4) -0.009(4) 0.000(3) C12' 0.037(6) 0.030(6) 0.047(6) -0.010(5) -0.003(5) 0.001(5) C21 0.030(6) 0.032(6) 0.032(5) -0.010(4) -0.001(4) 0.000(4) C22 0.036(6) 0.028(5) 0.025(5) -0.005(4) 0.007(4) 0.006(5) C23 0.049(7) 0.024(5) 0.040(6) -0.006(5) 0.006(5) 0.006(5) C24 0.036(6) 0.031(6) 0.040(6) -0.010(5) 0.001(5) -0.008(5) C25 0.029(6) 0.027(5) 0.049(6) -0.015(5) 0.002(5) 0.000(4) C26 0.027(5) 0.031(6) 0.045(6) -0.015(5) -0.006(5) 0.003(5) C27 0.043(7) 0.024(6) 0.067(8) -0.010(5) -0.001(6) -0.009(5) C28 0.054(9) 0.050(9) 0.139(15) -0.006(9) 0.031(9) -0.008(7) C29 0.103(13) 0.103(14) 0.088(12) -0.030(10) 0.003(10) -0.063(11) C210 0.074(10) 0.049(8) 0.096(11) 0.003(8) 0.016(9) -0.024(8) O2 0.026(3) 0.025(4) 0.032(4) -0.005(3) -0.011(3) 0.003(3) C211 0.046(6) 0.018(5) 0.033(5) 0.001(4) -0.014(5) 0.000(5) C212 0.038(6) 0.024(5) 0.034(6) 0.000(4) -0.013(5) 0.003(4) S2 0.0364(13) 0.0258(12) 0.0128(10) -0.0011(9) -0.0068(9) 0.0017(11) C213 0.040(6) 0.021(5) 0.031(5) 0.002(4) 0.003(5) 0.001(4) C214 0.052(7) 0.038(6) 0.019(5) -0.005(4) -0.006(5) -0.002(5) C23' 0.045(6) 0.023(5) 0.035(6) 0.006(4) 0.002(5) 0.002(5) C31 0.032(5) 0.025(5) 0.032(5) -0.001(4) 0.006(4) 0.002(4) C32 0.027(5) 0.025(5) 0.034(6) 0.001(4) 0.005(4) 0.000(4) C33 0.038(6) 0.022(5) 0.032(6) -0.001(4) 0.005(4) 0.001(4) C34 0.046(6) 0.020(5) 0.046(6) 0.001(5) 0.016(5) 0.004(4) C35 0.038(6) 0.025(6) 0.040(6) 0.010(5) 0.008(5) 0.010(4) C36 0.028(5) 0.031(6) 0.027(5) 0.004(4) 0.000(4) 0.002(4) C37 0.054(7) 0.022(6) 0.073(9) 0.005(6) 0.013(6) 0.002(5) C38 0.101(11) 0.023(6) 0.067(9) -0.005(6) -0.007(8) 0.010(7) C39 0.31(3) 0.013(6) 0.043(8) 0.001(6) -0.004(12) -0.003(11) C310 0.076(10) 0.051(8) 0.074(10) 0.007(7) -0.015(8) -0.002(7) O3 0.049(4) 0.017(3) 0.035(4) 0.007(3) -0.002(3) 0.009(3) C34' 0.032(6) 0.029(6) 0.031(5) -0.001(4) 0.007(4) 0.005(4) C41 0.041(6) 0.018(5) 0.031(5) -0.004(4) -0.004(4) -0.004(4) C42 0.036(6) 0.027(5) 0.035(6) 0.001(4) -0.003(5) 0.003(5) C43 0.024(5) 0.039(6) 0.042(6) 0.000(5) 0.000(4) -0.005(5) C44 0.037(6) 0.027(6) 0.047(6) -0.006(5) 0.003(5) -0.007(5) C45 0.045(6) 0.024(6) 0.042(6) 0.000(5) 0.005(5) -0.002(5) C46 0.036(6) 0.022(5) 0.028(5) -0.005(4) 0.002(4) 0.001(4) C47 0.041(7) 0.038(7) 0.058(8) 0.006(6) -0.004(5) -0.012(5) C48 0.058(9) 0.072(10) 0.118(14) 0.009(9) -0.028(9) -0.030(8) C49 0.096(13) 0.085(12) 0.084(11) 0.009(9) 0.010(10) -0.054(10) C410 0.058(9) 0.036(7) 0.123(13) -0.025(8) -0.008(8) -0.018(6) O4 0.039(4) 0.018(3) 0.032(4) 0.000(3) 0.005(3) -0.006(3) C411 0.046(6) 0.018(5) 0.027(5) 0.001(4) -0.004(5) 0.003(5) C412 0.035(6) 0.025(5) 0.027(5) -0.003(4) 0.002(4) -0.007(4) S4 0.0361(14) 0.0193(12) 0.0323(13) -0.0021(10) -0.0026(10) -0.0010(11) C413 0.047(6) 0.022(6) 0.044(6) -0.004(5) -0.007(5) 0.000(5) C414 0.056(8) 0.025(6) 0.074(9) 0.013(6) 0.000(6) -0.005(5) C41' 0.038(6) 0.023(5) 0.050(7) -0.004(5) -0.001(5) 0.001(5) Cl1 0.027(2) 0.0292(12) 0.0338(17) 0.0010(13) 0.0034(15) 0.0018(13) Cl1' 0.027(2) 0.0292(12) 0.0338(17) 0.0010(13) 0.0034(15) 0.0018(13) Cl2 0.0327(13) 0.0558(16) 0.0405(14) 0.0035(13) 0.0003(12) 0.0060(12) O21 0.036(4) 0.051(5) 0.049(5) 0.001(4) -0.003(4) 0.002(4) O22 0.053(5) 0.067(6) 0.075(6) -0.042(5) 0.006(5) -0.011(5) O23 0.050(5) 0.069(6) 0.068(6) 0.025(5) -0.013(4) -0.003(5) O24 0.033(4) 0.076(6) 0.055(5) -0.001(4) 0.003(4) 0.009(4) N5 0.060(8) 0.085(11) 0.134(13) 0.020(10) 0.019(9) 0.004(8) C51 0.048(8) 0.050(9) 0.130(16) 0.011(10) 0.001(10) 0.004(7) C52 0.040(8) 0.098(12) 0.120(14) -0.045(11) 0.011(8) 0.011(8) N6 0.058(7) 0.057(7) 0.055(6) 0.002(5) -0.006(6) -0.005(6) C61 0.051(7) 0.031(6) 0.043(6) -0.001(5) 0.002(6) -0.007(5) C62 0.056(8) 0.049(7) 0.043(7) -0.005(6) 0.003(6) 0.001(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 Hg S2 2.381(2) . ? Hg S4 2.388(2) . ? Hg O21 2.655(7) . ? Hg O11' 2.697(19) . ? C11 O1 1.391(12) . ? C11 C12 1.394(16) . ? C11 C16 1.409(15) . ? C12 C13 1.386(14) . ? C12 C12' 1.526(15) . ? C13 C14 1.396(15) . ? C14 C15 1.392(16) . ? C14 C17 1.538(14) . ? C15 C16 1.390(14) . ? C16 C41' 1.507(15) . ? C17 C110 1.492(16) . ? C17 C18 1.519(15) . ? C17 C19 1.559(15) . ? C12' C26 1.513(14) . ? C21 C22 1.398(13) . ? C21 C26 1.400(13) . ? C21 O2 1.406(11) . ? C22 C23 1.388(14) . ? C22 C23' 1.513(14) . ? C23 C24 1.392(15) . ? C24 C25 1.389(14) . ? C24 C27 1.552(14) . ? C25 C26 1.406(14) . ? C27 C29 1.493(18) . ? C27 C28 1.523(17) . ? C27 C210 1.543(18) . ? O2 C211 1.439(11) . ? C211 C212 1.520(13) . ? C212 S2 1.832(9) . ? S2 C213 1.828(10) . ? C213 C214 1.509(13) . ? C23' C36 1.503(14) . ? C31 O3 1.366(11) . ? C31 C32 1.415(13) . ? C31 C36 1.416(13) . ? C32 C33 1.371(13) . ? C32 C34' 1.519(13) . ? C33 C34 1.390(14) . ? C34 C35 1.404(15) . ? C34 C37 1.559(14) . ? C35 C36 1.385(13) . ? C37 C39 1.448(18) . ? C37 C38 1.494(17) . ? C37 C310 1.576(18) . ? C34' C46 1.524(13) . ? C41 C46 1.386(13) . ? C41 C42 1.406(14) . ? C41 O4 1.415(11) . ? C42 C43 1.382(14) . ? C42 C41' 1.511(13) . ? C43 C44 1.379(14) . ? C44 C45 1.394(15) . ? C44 C47 1.560(14) . ? C45 C46 1.380(14) . ? C47 C49 1.512(18) . ? C47 C410 1.519(17) . ? C47 C48 1.561(18) . ? O4 C411 1.437(11) . ? C411 C412 1.512(13) . ? C412 S4 1.841(10) . ? S4 C413 1.842(10) . ? C413 C414 1.532(16) . ? Cl1 O13 1.4401 . ? Cl1 O12 1.4402 . ? Cl1 O14 1.4402 . ? Cl1 O11 1.4403 . ? Cl1' O14' 1.4402 . ? Cl1' O11' 1.4402 . ? Cl1' O13' 1.4403 . ? Cl1' O12' 1.4404 . ? Cl2 O22 1.403(8) . ? Cl2 O24 1.424(8) . ? Cl2 O23 1.443(9) . ? Cl2 O21 1.482(8) . ? N5 C51 1.23(2) . ? C51 C52 1.46(2) . ? N6 C61 1.125(15) . ? C61 C62 1.457(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 S2 Hg S4 170.12(8) . . ? S2 Hg O21 95.10(17) . . ? S4 Hg O21 94.60(17) . . ? S2 Hg O11' 74.4(5) . . ? S4 Hg O11' 95.7(5) . . ? O21 Hg O11' 161.7(5) . . ? O1 C11 C12 118.1(10) . . ? O1 C11 C16 121.2(10) . . ? C12 C11 C16 120.7(9) . . ? C13 C12 C11 119.1(10) . . ? C13 C12 C12' 121.4(11) . . ? C11 C12 C12' 119.5(9) . . ? C12 C13 C14 122.6(11) . . ? C15 C14 C13 116.3(10) . . ? C15 C14 C17 124.4(10) . . ? C13 C14 C17 119.4(10) . . ? C16 C15 C14 124.0(11) . . ? C15 C16 C11 117.3(11) . . ? C15 C16 C41' 122.1(10) . . ? C11 C16 C41' 120.5(9) . . ? C110 C17 C18 111.6(10) . . ? C110 C17 C14 109.4(9) . . ? C18 C17 C14 109.3(9) . . ? C110 C17 C19 108.3(9) . . ? C18 C17 C19 107.3(9) . . ? C14 C17 C19 110.9(9) . . ? C26 C12' C12 108.6(8) . . ? C22 C21 C26 122.6(9) . . ? C22 C21 O2 119.4(8) . . ? C26 C21 O2 117.8(9) . . ? C23 C22 C21 117.4(9) . . ? C23 C22 C23' 120.4(9) . . ? C21 C22 C23' 122.1(9) . . ? C22 C23 C24 122.8(10) . . ? C25 C24 C23 117.7(9) . . ? C25 C24 C27 120.2(9) . . ? C23 C24 C27 122.0(10) . . ? C24 C25 C26 122.5(9) . . ? C21 C26 C25 116.9(9) . . ? C21 C26 C12' 123.3(9) . . ? C25 C26 C12' 119.8(9) . . ? C29 C27 C28 111.8(13) . . ? C29 C27 C210 109.3(12) . . ? C28 C27 C210 107.7(12) . . ? C29 C27 C24 108.9(11) . . ? C28 C27 C24 110.8(9) . . ? C210 C27 C24 108.2(10) . . ? C21 O2 C211 113.0(7) . . ? O2 C211 C212 107.4(8) . . ? C211 C212 S2 109.2(7) . . ? C213 S2 C212 99.6(5) . . ? C213 S2 Hg 105.4(3) . . ? C212 S2 Hg 107.7(3) . . ? C214 C213 S2 108.7(7) . . ? C36 C23' C22 111.6(8) . . ? O3 C31 C32 118.4(8) . . ? O3 C31 C36 121.8(9) . . ? C32 C31 C36 119.7(9) . . ? C33 C32 C31 118.9(9) . . ? C33 C32 C34' 122.5(9) . . ? C31 C32 C34' 118.5(9) . . ? C32 C33 C34 123.3(9) . . ? C33 C34 C35 116.9(9) . . ? C33 C34 C37 119.5(10) . . ? C35 C34 C37 123.5(10) . . ? C36 C35 C34 122.7(9) . . ? C35 C36 C31 118.5(9) . . ? C35 C36 C23' 122.1(9) . . ? C31 C36 C23' 119.4(9) . . ? C39 C37 C38 115.8(12) . . ? C39 C37 C34 110.8(10) . . ? C38 C37 C34 110.6(9) . . ? C39 C37 C310 106.7(12) . . ? C38 C37 C310 104.4(11) . . ? C34 C37 C310 108.0(10) . . ? C32 C34' C46 109.1(8) . . ? C46 C41 C42 121.9(9) . . ? C46 C41 O4 119.9(9) . . ? C42 C41 O4 118.1(8) . . ? C43 C42 C41 117.4(9) . . ? C43 C42 C41' 120.6(9) . . ? C41 C42 C41' 121.8(9) . . ? C44 C43 C42 122.9(9) . . ? C43 C44 C45 117.1(9) . . ? C43 C44 C47 121.3(10) . . ? C45 C44 C47 121.4(10) . . ? C46 C45 C44 122.9(10) . . ? C45 C46 C41 117.6(9) . . ? C45 C46 C34' 120.0(9) . . ? C41 C46 C34' 122.2(9) . . ? C49 C47 C410 112.5(12) . . ? C49 C47 C44 107.3(10) . . ? C410 C47 C44 111.2(10) . . ? C49 C47 C48 109.8(12) . . ? C410 C47 C48 106.5(12) . . ? C44 C47 C48 109.4(10) . . ? C41 O4 C411 113.5(7) . . ? O4 C411 C412 106.8(7) . . ? C411 C412 S4 109.5(7) . . ? C412 S4 C413 101.0(5) . . ? C412 S4 Hg 106.7(3) . . ? C413 S4 Hg 105.9(3) . . ? C414 C413 S4 108.8(7) . . ? C16 C41' C42 111.2(9) . . ? O13 Cl1 O12 109.5 . . ? O13 Cl1 O14 109.5 . . ? O12 Cl1 O14 109.5 . . ? O13 Cl1 O11 109.5 . . ? O12 Cl1 O11 109.5 . . ? O14 Cl1 O11 109.5 . . ? O14' Cl1' O11' 109.5 . . ? O14' Cl1' O13' 109.5 . . ? O11' Cl1' O13' 109.5 . . ? O14' Cl1' O12' 109.5 . . ? O11' Cl1' O12' 109.5 . . ? O13' Cl1' O12' 109.5 . . ? Cl1' O11' Hg 135.3(11) . . ? O22 Cl2 O24 110.0(6) . . ? O22 Cl2 O23 109.5(6) . . ? O24 Cl2 O23 110.3(5) . . ? O22 Cl2 O21 110.0(5) . . ? O24 Cl2 O21 109.4(5) . . ? O23 Cl2 O21 107.7(5) . . ? Cl2 O21 Hg 108.7(4) . . ? N5 C51 C52 177.1(17) . . ? N6 C61 C62 177.9(12) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 3.745 _refine_diff_density_min -2.598 _refine_diff_density_rms 0.163 #===END