#------------------------------------------------------------------------------ #$Date: 2020-08-02 05:22:13 +0300 (Sun, 02 Aug 2020) $ #$Revision: 254738 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704985.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7704985 loop_ _publ_author_name 'Samie, Ali' 'Salimi, Alireza' 'Garrison, Jered C.' _publ_section_title ; Coordination Chemistry of Mercury (II) Halide complexes: A Combined Experimental, Theoretical and (ICSD & CSD) Database study on the Relationship between Inorganic and Organic Units ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT01541E _journal_year 2020 _chemical_formula_moiety 'C32 H22 Hg I2 N2 O4' _chemical_formula_sum 'C32 H22 Hg I2 N2 O4' _chemical_formula_weight 952.90 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-07-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.4680(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.03860(10) _cell_length_b 12.9412(2) _cell_length_c 28.5482(4) _cell_measurement_reflns_used 17572 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 75.7430 _cell_measurement_theta_min 3.7290 _cell_volume 2968.87(7) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'ORTEP-3 for windows (Farrugia, 2012)' _computing_publication_material 'WinGx (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2005)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.2603 _diffrn_detector_type Onyx _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Onyx, Ultra' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 32603 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.060 _diffrn_reflns_theta_min 3.097 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 25.956 _exptl_absorpt_correction_T_max 0.1341 _exptl_absorpt_correction_T_min 0.0386 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_crystal_colour 'clear light brown' _exptl_crystal_density_diffrn 2.132 _exptl_crystal_description block _exptl_crystal_F_000 1784 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad 0.1000 _refine_diff_density_max 1.921 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.193 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 6097 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0397 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+4.2402P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.1115 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5724 _reflns_number_total 6097 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01541e2.cif _cod_data_source_block shelx3 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7704985 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.181 _shelx_estimated_absorpt_t_max 0.357 _exptl_absorpt_correction_t_ave 0.0871 _shelx_res_file ; TITL iran_as13 in P 21/c shelx.res created by SHELXL-2018/3 at 22:17:43 on 09-Jul-2020 CELL 1.54184 8.0386 12.9412 28.5482 90.000 91.468 90.000 ZERR 4.00 0.0001 0.0002 0.0004 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H HG I O N UNIT 128 88 4 8 16 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.050 0.100 0.100 ACTA BOND BOND $H CONF L.S. 20 TEMP 20.00 WGHT 0.075700 4.240200 FVAR 1.12897 C1 1 0.729905 0.818591 0.405327 11.00000 0.03883 0.03319 = 0.03718 0.00190 0.00465 0.00134 C2 1 0.797875 0.807153 0.449059 11.00000 0.05054 0.03891 = 0.03765 -0.00130 -0.00056 -0.00492 AFIX 43 H2 2 0.856036 0.861317 0.463275 11.00000 -1.20000 AFIX 0 C3 1 0.779225 0.711499 0.472907 11.00000 0.04976 0.03966 = 0.03509 0.00328 -0.00321 -0.00107 AFIX 43 H3 2 0.823584 0.703473 0.503094 11.00000 -1.20000 AFIX 0 C4 1 0.696631 0.631598 0.451693 11.00000 0.04841 0.03570 = 0.04084 0.00753 0.00570 0.00331 AFIX 43 H4 2 0.686399 0.569141 0.467473 11.00000 -1.20000 AFIX 0 C5 1 0.626007 0.642229 0.405902 11.00000 0.04053 0.04020 = 0.04331 -0.00295 0.00157 0.00210 C6 1 0.542507 0.560283 0.382421 11.00000 0.04454 0.03639 = 0.05916 -0.00144 -0.00289 -0.00039 AFIX 43 H6 2 0.529867 0.497410 0.397701 11.00000 -1.20000 AFIX 0 C7 1 0.479704 0.571688 0.337503 11.00000 0.04805 0.04653 = 0.05780 -0.01269 -0.00635 -0.00145 AFIX 43 H7 2 0.427339 0.516372 0.322456 11.00000 -1.20000 AFIX 0 C8 1 0.494615 0.667452 0.314133 11.00000 0.04728 0.06024 = 0.04270 -0.00713 -0.00742 0.00474 AFIX 43 H8 2 0.451889 0.674962 0.283741 11.00000 -1.20000 AFIX 0 C9 1 0.571690 0.749147 0.336066 11.00000 0.04241 0.05043 = 0.03645 0.00127 -0.00059 0.00594 AFIX 43 H9 2 0.578091 0.812268 0.320644 11.00000 -1.20000 AFIX 0 C10 1 0.641702 0.739156 0.381758 11.00000 0.03736 0.03974 = 0.03527 0.00040 0.00506 0.00382 C11 1 0.644865 0.985629 0.381770 11.00000 0.04210 0.03728 = 0.03476 -0.00364 0.00010 -0.00600 C12 1 0.692450 1.074932 0.353390 11.00000 0.04309 0.03296 = 0.03565 -0.00033 -0.00385 -0.00256 C13 1 0.835691 1.077434 0.327172 11.00000 0.04441 0.03267 = 0.03327 -0.00272 -0.00127 0.00033 AFIX 43 H13 2 0.904123 1.019483 0.327374 11.00000 -1.20000 AFIX 0 C14 1 0.782461 1.242598 0.301773 11.00000 0.04161 0.03759 = 0.04230 0.00415 -0.00811 -0.00389 AFIX 43 H14 2 0.813661 1.299872 0.284390 11.00000 -1.20000 AFIX 0 C15 1 0.636702 1.247895 0.326627 11.00000 0.03863 0.04152 = 0.05565 0.00473 -0.00125 0.00511 AFIX 43 H15 2 0.570799 1.306961 0.325728 11.00000 -1.20000 AFIX 0 C16 1 0.592363 1.163048 0.352705 11.00000 0.04007 0.03623 = 0.05535 0.00317 0.00355 0.00132 AFIX 43 H16 2 0.495603 1.164537 0.369865 11.00000 -1.20000 AFIX 0 C17 1 0.979706 0.792424 0.093092 11.00000 0.05663 0.03596 = 0.03532 -0.00402 -0.00571 0.00728 C18 1 0.851842 0.729611 0.103925 11.00000 0.05328 0.04915 = 0.03481 -0.00260 0.00183 0.00639 AFIX 43 H18 2 0.767742 0.753385 0.122931 11.00000 -1.20000 AFIX 0 C19 1 0.846688 0.627247 0.086137 11.00000 0.04915 0.05524 = 0.04224 0.00355 -0.00354 -0.00826 AFIX 43 H19 2 0.757919 0.584133 0.092906 11.00000 -1.20000 AFIX 0 C20 1 0.973896 0.591784 0.058733 11.00000 0.05194 0.03606 = 0.03909 -0.00460 -0.00735 0.00041 AFIX 43 H20 2 0.971779 0.524236 0.047615 11.00000 -1.20000 AFIX 0 C21 1 1.107162 0.657747 0.047538 11.00000 0.04635 0.03621 = 0.03446 0.00119 -0.00618 0.00263 C22 1 1.242237 0.626221 0.019313 11.00000 0.05217 0.04807 = 0.04787 -0.00945 0.00564 0.00115 AFIX 43 H22 2 1.243540 0.559390 0.007353 11.00000 -1.20000 AFIX 0 C23 1 1.367749 0.691074 0.009627 11.00000 0.05926 0.07370 = 0.05504 -0.00523 0.01151 0.00178 AFIX 43 H23 2 1.453267 0.668365 -0.009141 11.00000 -1.20000 AFIX 0 C24 1 1.371953 0.789995 0.026903 11.00000 0.05546 0.06573 = 0.06263 0.00149 0.00773 -0.01298 AFIX 43 H24 2 1.461009 0.833018 0.020301 11.00000 -1.20000 AFIX 0 C25 1 1.245766 0.825619 0.053787 11.00000 0.06565 0.03872 = 0.05820 -0.00082 -0.00400 -0.00586 AFIX 43 H25 2 1.249050 0.893151 0.064911 11.00000 -1.20000 AFIX 0 C26 1 1.110077 0.760980 0.064918 11.00000 0.05299 0.04043 = 0.03586 0.00155 -0.00596 0.00408 C27 1 0.902388 0.969207 0.091903 11.00000 0.04906 0.04611 = 0.04627 -0.00035 -0.00072 0.00208 C28 1 0.924029 1.068679 0.117593 11.00000 0.05216 0.03782 = 0.04148 -0.00471 -0.00216 -0.00144 C29 1 1.005402 1.074283 0.160784 11.00000 0.04023 0.03078 = 0.04244 0.00260 -0.00176 -0.00105 AFIX 43 H29 2 1.055672 1.015097 0.173028 11.00000 -1.20000 AFIX 0 C30 1 0.942704 1.246371 0.167140 11.00000 0.04292 0.03110 = 0.03670 -0.00156 -0.00101 -0.00064 AFIX 43 H30 2 0.948048 1.307538 0.184212 11.00000 -1.20000 AFIX 0 C31 1 0.861352 1.246705 0.123959 11.00000 0.04916 0.03683 = 0.04284 0.00487 -0.00142 0.00141 AFIX 43 H31 2 0.813777 1.307372 0.112409 11.00000 -1.20000 AFIX 0 C32 1 0.850746 1.157585 0.098125 11.00000 0.06023 0.04036 = 0.04257 0.00262 -0.00873 0.00010 AFIX 43 H32 2 0.797118 1.156180 0.068877 11.00000 -1.20000 AFIX 0 O1 5 0.518172 0.978322 0.403528 11.00000 0.04772 0.04360 = 0.05200 0.00637 0.01207 0.00217 O2A 5 0.761398 0.910203 0.380641 11.00000 0.04256 0.03395 = 0.04232 0.00679 0.00422 0.00085 O3 5 0.817691 0.957286 0.057032 11.00000 0.10006 0.04983 = 0.05419 -0.01104 -0.03129 0.01058 O4A 5 0.993245 0.892349 0.112823 11.00000 0.05335 0.03871 = 0.04361 -0.00438 -0.00204 -0.00033 N1 6 0.879915 1.159289 0.301630 11.00000 0.04444 0.03470 = 0.03566 0.00361 -0.00218 -0.00126 MOLE 1 HG1 3 1.144898 1.167105 0.261776 11.00000 0.04356 0.03110 = 0.03616 -0.00049 0.00050 -0.00147 I1 4 1.206843 1.369216 0.269210 11.00000 0.04315 0.03154 = 0.03927 -0.00272 -0.00059 -0.00345 I2 4 1.290042 0.987990 0.281167 11.00000 0.04474 0.03209 = 0.04604 -0.00031 -0.00449 0.00000 N2 6 1.014229 1.161540 0.185438 11.00000 0.04329 0.03278 = 0.03530 -0.00320 0.00328 -0.00500 HKLF 4 REM iran_as13 in P 21/c REM wR2 = 0.1115, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0397 for 5724 Fo > 4sig(Fo) and 0.0422 for all 6097 data REM 370 parameters refined using 0 restraints END WGHT 0.0773 3.6509 REM Highest difference peak 1.921, deepest hole -0.837, 1-sigma level 0.193 Q1 1 1.0968 1.2211 0.2590 11.00000 0.05 1.92 Q2 1 1.1977 1.2216 0.2682 11.00000 0.05 1.72 Q3 1 1.1101 1.1112 0.2560 11.00000 0.05 1.65 Q4 1 1.1744 1.1136 0.2532 11.00000 0.05 1.60 Q5 1 1.1934 1.1152 0.2656 11.00000 0.05 1.57 Q6 1 1.1850 1.3180 0.2611 11.00000 0.05 1.37 Q7 1 1.2749 1.0380 0.2873 11.00000 0.05 1.32 Q8 1 1.0934 1.1638 0.2970 11.00000 0.05 1.17 Q9 1 1.2346 0.9383 0.2792 11.00000 0.05 1.15 Q10 1 1.1467 0.9278 0.0917 11.00000 0.05 1.14 Q11 1 1.2579 1.4246 0.2703 11.00000 0.05 1.13 Q12 1 1.1894 1.1636 0.2300 11.00000 0.05 1.08 Q13 1 1.3510 0.9360 0.2745 11.00000 0.05 1.07 Q14 1 1.2666 1.3133 0.2803 11.00000 0.05 1.05 Q15 1 1.1833 1.4348 0.2761 11.00000 0.05 1.03 Q16 1 0.8462 0.6607 0.1081 11.00000 0.05 1.00 Q17 1 1.3368 0.9773 0.2521 11.00000 0.05 0.87 Q18 1 1.2177 1.0189 0.2534 11.00000 0.05 0.79 Q19 1 0.9498 0.9702 0.0388 11.00000 0.05 0.78 Q20 1 1.3808 1.0121 0.2649 11.00000 0.05 0.77 ; _shelx_res_checksum 27821 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7299(7) 0.8186(4) 0.4053(2) 0.0363(11) Uani 1 1 d . . . . . C2 C 0.7979(8) 0.8072(5) 0.4491(2) 0.0424(12) Uani 1 1 d . . . . . H2 H 0.856036 0.861317 0.463275 0.051 Uiso 1 1 calc R U . . . C3 C 0.7792(8) 0.7115(5) 0.4729(2) 0.0416(12) Uani 1 1 d . . . . . H3 H 0.823584 0.703473 0.503094 0.050 Uiso 1 1 calc R U . . . C4 C 0.6966(8) 0.6316(5) 0.4517(2) 0.0416(12) Uani 1 1 d . . . . . H4 H 0.686399 0.569141 0.467473 0.050 Uiso 1 1 calc R U . . . C5 C 0.6260(8) 0.6422(5) 0.4059(2) 0.0413(12) Uani 1 1 d . . . . . C6 C 0.5425(8) 0.5603(5) 0.3824(2) 0.0468(13) Uani 1 1 d . . . . . H6 H 0.529867 0.497410 0.397701 0.056 Uiso 1 1 calc R U . . . C7 C 0.4797(8) 0.5717(5) 0.3375(2) 0.0509(14) Uani 1 1 d . . . . . H7 H 0.427339 0.516372 0.322456 0.061 Uiso 1 1 calc R U . . . C8 C 0.4946(9) 0.6675(5) 0.3141(2) 0.0502(15) Uani 1 1 d . . . . . H8 H 0.451889 0.674962 0.283741 0.060 Uiso 1 1 calc R U . . . C9 C 0.5717(7) 0.7491(5) 0.3361(2) 0.0431(12) Uani 1 1 d . . . . . H9 H 0.578091 0.812268 0.320644 0.052 Uiso 1 1 calc R U . . . C10 C 0.6417(7) 0.7392(4) 0.38176(19) 0.0374(11) Uani 1 1 d . . . . . C11 C 0.6449(7) 0.9856(4) 0.38177(19) 0.0381(11) Uani 1 1 d . . . . . C12 C 0.6924(7) 1.0749(4) 0.35339(19) 0.0373(11) Uani 1 1 d . . . . . C13 C 0.8357(7) 1.0774(4) 0.32717(18) 0.0368(11) Uani 1 1 d . . . . . H13 H 0.904123 1.019483 0.327374 0.044 Uiso 1 1 calc R U . . . C14 C 0.7825(7) 1.2426(5) 0.3018(2) 0.0407(11) Uani 1 1 d . . . . . H14 H 0.813661 1.299872 0.284390 0.049 Uiso 1 1 calc R U . . . C15 C 0.6367(7) 1.2479(5) 0.3266(2) 0.0453(13) Uani 1 1 d . . . . . H15 H 0.570799 1.306961 0.325728 0.054 Uiso 1 1 calc R U . . . C16 C 0.5924(8) 1.1630(5) 0.3527(2) 0.0438(13) Uani 1 1 d . . . . . H16 H 0.495603 1.164537 0.369865 0.053 Uiso 1 1 calc R U . . . C17 C 0.9797(8) 0.7924(5) 0.0931(2) 0.0428(12) Uani 1 1 d . . . . . C18 C 0.8518(8) 0.7296(5) 0.1039(2) 0.0457(13) Uani 1 1 d . . . . . H18 H 0.767742 0.753385 0.122931 0.055 Uiso 1 1 calc R U . . . C19 C 0.8467(9) 0.6272(6) 0.0861(2) 0.0490(14) Uani 1 1 d . . . . . H19 H 0.757919 0.584133 0.092906 0.059 Uiso 1 1 calc R U . . . C20 C 0.9739(8) 0.5918(5) 0.0587(2) 0.0425(12) Uani 1 1 d . . . . . H20 H 0.971779 0.524236 0.047615 0.051 Uiso 1 1 calc R U . . . C21 C 1.1072(8) 0.6577(4) 0.0475(2) 0.0391(11) Uani 1 1 d . . . . . C22 C 1.2422(9) 0.6262(5) 0.0193(2) 0.0493(14) Uani 1 1 d . . . . . H22 H 1.243540 0.559390 0.007353 0.059 Uiso 1 1 calc R U . . . C23 C 1.3677(10) 0.6911(7) 0.0096(3) 0.0625(18) Uani 1 1 d . . . . . H23 H 1.453267 0.668365 -0.009141 0.075 Uiso 1 1 calc R U . . . C24 C 1.3720(10) 0.7900(7) 0.0269(3) 0.0612(18) Uani 1 1 d . . . . . H24 H 1.461009 0.833018 0.020301 0.073 Uiso 1 1 calc R U . . . C25 C 1.2458(10) 0.8256(5) 0.0538(3) 0.0543(16) Uani 1 1 d . . . . . H25 H 1.249050 0.893151 0.064911 0.065 Uiso 1 1 calc R U . . . C26 C 1.1101(8) 0.7610(5) 0.0649(2) 0.0432(12) Uani 1 1 d . . . . . C27 C 0.9024(8) 0.9692(5) 0.0919(2) 0.0472(13) Uani 1 1 d . . . . . C28 C 0.9240(8) 1.0687(5) 0.1176(2) 0.0439(12) Uani 1 1 d . . . . . C29 C 1.0054(7) 1.0743(4) 0.1608(2) 0.0379(11) Uani 1 1 d . . . . . H29 H 1.055672 1.015097 0.173028 0.045 Uiso 1 1 calc R U . . . C30 C 0.9427(7) 1.2464(4) 0.16714(19) 0.0369(10) Uani 1 1 d . . . . . H30 H 0.948048 1.307538 0.184212 0.044 Uiso 1 1 calc R U . . . C31 C 0.8614(8) 1.2467(5) 0.1240(2) 0.0430(12) Uani 1 1 d . . . . . H31 H 0.813777 1.307372 0.112409 0.052 Uiso 1 1 calc R U . . . C32 C 0.8507(9) 1.1576(5) 0.0981(2) 0.0479(14) Uani 1 1 d . . . . . H32 H 0.797118 1.156180 0.068877 0.057 Uiso 1 1 calc R U . . . O1 O 0.5182(6) 0.9783(3) 0.40353(16) 0.0476(10) Uani 1 1 d . . . . . O2A O 0.7614(5) 0.9102(3) 0.38064(14) 0.0396(8) Uani 1 1 d . . . . . O3 O 0.8177(8) 0.9573(4) 0.05703(18) 0.0686(15) Uani 1 1 d . . . . . O4A O 0.9932(6) 0.8923(3) 0.11282(15) 0.0453(9) Uani 1 1 d . . . . . N1 N 0.8799(6) 1.1593(4) 0.30163(16) 0.0383(10) Uani 1 1 d . . . . . Hg1 Hg 1.14490(3) 1.16711(2) 0.26178(2) 0.03695(10) Uani 1 1 d . . . . . I1 I 1.20684(4) 1.36922(3) 0.26921(2) 0.03802(11) Uani 1 1 d . . . . . I2 I 1.29004(5) 0.98799(3) 0.28117(2) 0.04105(11) Uani 1 1 d . . . . . N2 N 1.0142(6) 1.1615(3) 0.18544(16) 0.0371(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.033(3) 0.037(3) 0.002(2) 0.005(2) 0.001(2) C2 0.051(3) 0.039(3) 0.038(3) -0.001(2) -0.001(2) -0.005(2) C3 0.050(3) 0.040(3) 0.035(3) 0.003(2) -0.003(2) -0.001(2) C4 0.048(3) 0.036(3) 0.041(3) 0.008(2) 0.006(2) 0.003(2) C5 0.041(3) 0.040(3) 0.043(3) -0.003(2) 0.002(2) 0.002(2) C6 0.045(3) 0.036(3) 0.059(3) -0.001(3) -0.003(3) 0.000(2) C7 0.048(3) 0.047(3) 0.058(4) -0.013(3) -0.006(3) -0.001(3) C8 0.047(3) 0.060(4) 0.043(3) -0.007(3) -0.007(3) 0.005(3) C9 0.042(3) 0.050(3) 0.036(3) 0.001(2) -0.001(2) 0.006(2) C10 0.037(2) 0.040(3) 0.035(3) 0.000(2) 0.005(2) 0.004(2) C11 0.042(3) 0.037(3) 0.035(2) -0.004(2) 0.000(2) -0.006(2) C12 0.043(3) 0.033(3) 0.036(2) 0.000(2) -0.004(2) -0.003(2) C13 0.044(3) 0.033(3) 0.033(2) -0.003(2) -0.001(2) 0.000(2) C14 0.042(3) 0.038(3) 0.042(3) 0.004(2) -0.008(2) -0.004(2) C15 0.039(3) 0.042(3) 0.056(3) 0.005(3) -0.001(2) 0.005(2) C16 0.040(3) 0.036(3) 0.055(3) 0.003(2) 0.004(2) 0.001(2) C17 0.057(3) 0.036(3) 0.035(3) -0.004(2) -0.006(2) 0.007(2) C18 0.053(3) 0.049(3) 0.035(3) -0.003(2) 0.002(2) 0.006(3) C19 0.049(3) 0.055(4) 0.042(3) 0.004(3) -0.004(3) -0.008(3) C20 0.052(3) 0.036(3) 0.039(3) -0.005(2) -0.007(2) 0.000(2) C21 0.046(3) 0.036(3) 0.034(3) 0.001(2) -0.006(2) 0.003(2) C22 0.052(3) 0.048(4) 0.048(3) -0.009(3) 0.006(3) 0.001(3) C23 0.059(4) 0.074(5) 0.055(4) -0.005(4) 0.012(3) 0.002(4) C24 0.055(4) 0.066(5) 0.063(4) 0.001(4) 0.008(3) -0.013(3) C25 0.066(4) 0.039(3) 0.058(4) -0.001(3) -0.004(3) -0.006(3) C26 0.053(3) 0.040(3) 0.036(3) 0.002(2) -0.006(2) 0.004(3) C27 0.049(3) 0.046(3) 0.046(3) 0.000(3) -0.001(3) 0.002(3) C28 0.052(3) 0.038(3) 0.041(3) -0.005(2) -0.002(2) -0.001(2) C29 0.040(3) 0.031(3) 0.042(3) 0.003(2) -0.002(2) -0.001(2) C30 0.043(3) 0.031(2) 0.037(3) -0.002(2) -0.001(2) -0.001(2) C31 0.049(3) 0.037(3) 0.043(3) 0.005(2) -0.001(2) 0.001(2) C32 0.060(4) 0.040(3) 0.043(3) 0.003(2) -0.009(3) 0.000(3) O1 0.048(2) 0.044(2) 0.052(2) 0.0064(18) 0.0121(19) 0.0022(18) O2A 0.043(2) 0.034(2) 0.0423(19) 0.0068(16) 0.0042(16) 0.0009(16) O3 0.100(4) 0.050(3) 0.054(3) -0.011(2) -0.031(3) 0.011(3) O4A 0.053(2) 0.039(2) 0.044(2) -0.0044(17) -0.0020(18) -0.0003(18) N1 0.044(2) 0.035(2) 0.036(2) 0.0036(17) -0.0022(19) -0.0013(19) Hg1 0.04356(15) 0.03110(14) 0.03616(14) -0.00049(7) 0.00050(9) -0.00147(8) I1 0.0431(2) 0.03154(19) 0.03927(18) -0.00272(12) -0.00059(14) -0.00345(12) I2 0.0447(2) 0.03209(18) 0.0460(2) -0.00031(13) -0.00449(15) 0.00000(13) N2 0.043(2) 0.033(2) 0.035(2) -0.0032(17) 0.0033(18) -0.0050(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C1 O2A 118.7(5) . . ? C2 C1 C10 123.0(5) . . ? O2A C1 C10 118.1(5) . . ? C1 C2 C3 119.3(6) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 122.5(6) . . ? C6 C5 C10 118.2(6) . . ? C4 C5 C10 119.2(5) . . ? C7 C6 C5 121.3(6) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 120.1(6) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.1(6) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C1 C10 C9 123.9(6) . . ? C1 C10 C5 117.2(5) . . ? C9 C10 C5 119.0(6) . . ? O1 C11 O2A 123.2(5) . . ? O1 C11 C12 125.4(6) . . ? O2A C11 C12 111.4(5) . . ? C13 C12 C16 117.3(5) . . ? C13 C12 C11 123.2(5) . . ? C16 C12 C11 119.5(5) . . ? N1 C13 C12 123.2(5) . . ? N1 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? N1 C14 C15 123.1(6) . . ? N1 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C16 C15 C14 118.1(6) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C12 120.1(6) . . ? C15 C16 H16 120.0 . . ? C12 C16 H16 120.0 . . ? C18 C17 C26 122.8(6) . . ? C18 C17 O4A 120.7(6) . . ? C26 C17 O4A 116.4(6) . . ? C17 C18 C19 119.6(6) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.8(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.3(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C26 119.6(6) . . ? C20 C21 C22 123.2(6) . . ? C26 C21 C22 117.3(6) . . ? C23 C22 C21 121.5(6) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 121.3(7) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 120.3(7) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C17 C26 C25 123.4(6) . . ? C17 C26 C21 117.9(6) . . ? C25 C26 C21 118.8(6) . . ? O3 C27 O4A 123.7(6) . . ? O3 C27 C28 125.1(6) . . ? O4A C27 C28 111.1(5) . . ? C29 C28 C32 119.7(6) . . ? C29 C28 C27 122.1(6) . . ? C32 C28 C27 118.1(6) . . ? N2 C29 C28 122.2(5) . . ? N2 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? N2 C30 C31 122.7(5) . . ? N2 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C32 C31 C30 120.0(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C28 117.3(6) . . ? C31 C32 H32 121.4 . . ? C28 C32 H32 121.4 . . ? C11 O2A C1 117.6(4) . . ? C27 O4A C17 117.3(5) . . ? C14 N1 C13 118.3(5) . . ? C14 N1 Hg1 119.2(4) . . ? C13 N1 Hg1 122.2(4) . . ? N2 Hg1 N1 93.16(16) . . ? N2 Hg1 I2 110.15(11) . . ? N1 Hg1 I2 104.55(11) . . ? N2 Hg1 I1 100.27(11) . . ? N1 Hg1 I1 99.59(11) . . ? I2 Hg1 I1 139.540(14) . . ? C29 N2 C30 118.2(5) . . ? C29 N2 Hg1 121.5(4) . . ? C30 N2 Hg1 120.3(3) . . ? 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 C1 C2 1.358(8) . ? C1 O2A 1.406(7) . ? C1 C10 1.410(8) . ? C2 C3 1.423(8) . ? C2 H2 0.9300 . ? C3 C4 1.362(9) . ? C3 H3 0.9300 . ? C4 C5 1.418(9) . ? C4 H4 0.9300 . ? C5 C6 1.415(9) . ? C5 C10 1.438(8) . ? C6 C7 1.374(10) . ? C6 H6 0.9300 . ? C7 C8 1.414(10) . ? C7 H7 0.9300 . ? C8 C9 1.369(9) . ? C8 H8 0.9300 . ? C9 C10 1.413(8) . ? C9 H9 0.9300 . ? C11 O1 1.210(7) . ? C11 O2A 1.354(7) . ? C11 C12 1.468(8) . ? C12 C13 1.390(8) . ? C12 C16 1.395(8) . ? C13 N1 1.339(7) . ? C13 H13 0.9300 . ? C14 N1 1.333(8) . ? C14 C15 1.387(9) . ? C14 H14 0.9300 . ? C15 C16 1.379(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.352(10) . ? C17 C26 1.398(9) . ? C17 O4A 1.414(7) . ? C18 C19 1.419(10) . ? C18 H18 0.9300 . ? C19 C20 1.382(9) . ? C19 H19 0.9300 . ? C20 C21 1.413(9) . ? C20 H20 0.9300 . ? C21 C26 1.425(8) . ? C21 C22 1.428(9) . ? C22 C23 1.347(11) . ? C22 H22 0.9300 . ? C23 C24 1.372(12) . ? C23 H23 0.9300 . ? C24 C25 1.368(11) . ? C24 H24 0.9300 . ? C25 C26 1.417(10) . ? C25 H25 0.9300 . ? C27 O3 1.202(8) . ? C27 O4A 1.363(8) . ? C27 C28 1.490(9) . ? C28 C29 1.383(8) . ? C28 C32 1.401(9) . ? C29 N2 1.332(7) . ? C29 H29 0.9300 . ? C30 N2 1.339(7) . ? C30 C31 1.381(8) . ? C30 H30 0.9300 . ? C31 C32 1.370(9) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? N1 Hg1 2.443(5) . ? Hg1 N2 2.396(5) . ? Hg1 I2 2.6472(4) . ? Hg1 I1 2.6700(4) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2A C1 C2 C3 -174.6(5) . . . . ? C10 C1 C2 C3 -0.6(9) . . . . ? C1 C2 C3 C4 1.2(10) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C3 C4 C5 C6 178.6(6) . . . . ? C3 C4 C5 C10 -0.2(9) . . . . ? C4 C5 C6 C7 -178.0(6) . . . . ? C10 C5 C6 C7 0.9(9) . . . . ? C5 C6 C7 C8 -1.4(10) . . . . ? C6 C7 C8 C9 0.1(10) . . . . ? C7 C8 C9 C10 1.7(10) . . . . ? C2 C1 C10 C9 -179.3(6) . . . . ? O2A C1 C10 C9 -5.2(8) . . . . ? C2 C1 C10 C5 -0.4(8) . . . . ? O2A C1 C10 C5 173.6(5) . . . . ? C8 C9 C10 C1 176.7(6) . . . . ? C8 C9 C10 C5 -2.1(9) . . . . ? C6 C5 C10 C1 -178.1(5) . . . . ? C4 C5 C10 C1 0.8(8) . . . . ? C6 C5 C10 C9 0.8(8) . . . . ? C4 C5 C10 C9 179.7(5) . . . . ? O1 C11 C12 C13 -176.7(6) . . . . ? O2A C11 C12 C13 3.0(8) . . . . ? O1 C11 C12 C16 4.3(9) . . . . ? O2A C11 C12 C16 -176.0(5) . . . . ? C16 C12 C13 N1 -0.3(8) . . . . ? C11 C12 C13 N1 -179.3(5) . . . . ? N1 C14 C15 C16 0.7(9) . . . . ? C14 C15 C16 C12 -0.4(10) . . . . ? C13 C12 C16 C15 0.2(9) . . . . ? C11 C12 C16 C15 179.2(6) . . . . ? C26 C17 C18 C19 -0.3(9) . . . . ? O4A C17 C18 C19 -175.9(5) . . . . ? C17 C18 C19 C20 1.4(10) . . . . ? C18 C19 C20 C21 -1.4(9) . . . . ? C19 C20 C21 C26 0.4(9) . . . . ? C19 C20 C21 C22 -179.8(6) . . . . ? C20 C21 C22 C23 -179.6(7) . . . . ? C26 C21 C22 C23 0.3(10) . . . . ? C21 C22 C23 C24 0.7(12) . . . . ? C22 C23 C24 C25 -1.3(13) . . . . ? C23 C24 C25 C26 1.0(12) . . . . ? C18 C17 C26 C25 -179.2(6) . . . . ? O4A C17 C26 C25 -3.5(9) . . . . ? C18 C17 C26 C21 -0.7(9) . . . . ? O4A C17 C26 C21 175.1(5) . . . . ? C24 C25 C26 C17 178.5(7) . . . . ? C24 C25 C26 C21 0.0(10) . . . . ? C20 C21 C26 C17 0.6(8) . . . . ? C22 C21 C26 C17 -179.2(6) . . . . ? C20 C21 C26 C25 179.3(6) . . . . ? C22 C21 C26 C25 -0.6(9) . . . . ? O3 C27 C28 C29 171.3(7) . . . . ? O4A C27 C28 C29 -9.4(9) . . . . ? O3 C27 C28 C32 -5.1(11) . . . . ? O4A C27 C28 C32 174.3(6) . . . . ? C32 C28 C29 N2 1.4(10) . . . . ? C27 C28 C29 N2 -174.9(6) . . . . ? N2 C30 C31 C32 0.3(10) . . . . ? C30 C31 C32 C28 0.4(10) . . . . ? C29 C28 C32 C31 -1.2(10) . . . . ? C27 C28 C32 C31 175.2(6) . . . . ? O1 C11 O2A C1 1.4(8) . . . . ? C12 C11 O2A C1 -178.3(5) . . . . ? C2 C1 O2A C11 -97.2(6) . . . . ? C10 C1 O2A C11 88.5(6) . . . . ? O3 C27 O4A C17 -2.9(10) . . . . ? C28 C27 O4A C17 177.7(5) . . . . ? C18 C17 O4A C27 -82.7(7) . . . . ? C26 C17 O4A C27 101.4(6) . . . . ? C15 C14 N1 C13 -0.8(8) . . . . ? C15 C14 N1 Hg1 -174.6(5) . . . . ? C12 C13 N1 C14 0.6(8) . . . . ? C12 C13 N1 Hg1 174.3(4) . . . . ? C28 C29 N2 C30 -0.7(8) . . . . ? C28 C29 N2 Hg1 177.1(4) . . . . ? C31 C30 N2 C29 -0.2(8) . . . . ? C31 C30 N2 Hg1 -178.0(4) . . . . ?