#------------------------------------------------------------------------------ #$Date: 2020-08-02 05:22:13 +0300 (Sun, 02 Aug 2020) $ #$Revision: 254738 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704984.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_7704984 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 'C30 H20 Cl2 Hg N4 O4' _chemical_formula_sum 'C30 H20 Cl2 Hg N4 O4' _chemical_formula_weight 771.99 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -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 106.966(11) _cell_angle_beta 92.424(10) _cell_angle_gamma 96.714(8) _cell_formula_units_Z 2 _cell_length_a 7.777(6) _cell_length_b 12.712(10) _cell_length_c 14.892(12) _cell_measurement_reflns_used 5064 _cell_measurement_temperature 140(2) _cell_measurement_theta_max 33.6 _cell_measurement_theta_min 2.5 _cell_volume 1394.0(19) _computing_data_collection 'CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 140(2) _diffrn_detector_area_resol_mean 13.6612 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Rigaku Mercury375R (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1422 _diffrn_reflns_av_unetI/netI 0.1277 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 15695 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.249 _diffrn_reflns_theta_min 1.690 _exptl_absorpt_coefficient_mu 5.757 _exptl_absorpt_correction_T_max 0.2168 _exptl_absorpt_correction_T_min 0.1871 _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 yellow _exptl_crystal_density_diffrn 1.839 _exptl_crystal_description prism _exptl_crystal_F_000 748 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad 0.2000 _refine_diff_density_max 1.698 _refine_diff_density_min -2.920 _refine_diff_density_rms 0.186 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 479 _refine_ls_number_reflns 6864 _refine_ls_number_restraints 204 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0593 _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^)+(0.0431P)^2^+0.8759P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1454 _refine_ls_wR_factor_ref 0.1520 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6011 _reflns_number_total 6864 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01541e2.cif _cod_data_source_block shelx7 _cod_original_cell_volume 1393.9(18) _cod_database_code 7704984 _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 0.392 _shelx_estimated_absorpt_t_max 0.392 _exptl_absorpt_correction_t_ave 0.2018 _shelx_res_file ; TITL AS15-2 in P-1 shelx.res created by SHELXL-2018/3 at 13:55:54 on 08-Jul-2020 CELL 0.71073 7.7768 12.7118 14.8917 106.966 92.424 96.714 ZERR 2.00 0.0056 0.0098 0.0115 0.011 0.010 0.008 LATT 1 SFAC C H N O CL HG UNIT 60 40 8 8 4 2 MERG 2 OMIT -2.00 56.50 OMIT 0 0 1 OMIT 0 -1 1 DELU 0.010 0.010 C20 C24A C25A C23A C22A C21A C19A C18A C17A DELU 0.010 0.010 C16A SIMU 0.040 0.080 1.700 C20 C24A C25A C23A C22A C21A C19A C18A SIMU 0.040 0.080 1.700 C17A C16A DELU 0.010 0.010 C20 C25B C24B C23B C22B C21B C19B C18B C17B DELU 0.010 0.010 C16B SIMU 0.040 0.080 1.700 C20 C25B C24B C23B C22B C21B C19B C18B SIMU 0.040 0.080 1.700 C17B C16B DELU 0.010 0.010 O3A O3B C26A C26B SIMU 0.040 0.080 1.700 O3A O3B C26A C26B DELU 0.010 0.010 O4A O4B SIMU 0.040 0.080 1.700 O4A O4B FLAT 0.100 C20 C25B C24B C23B C22B C21B C19B C18B C17B C16B FLAT 0.100 C20 C24A C25A C23A C22A C21A C19A C18A C17A C16A FMAP 2 PLAN 20 SIZE 0.200 0.200 0.200 ACTA BOND L.S. 40 TEMP -133.00 WGHT 0.043100 0.875900 FVAR 0.21004 0.60052 N3 3 0.428042 0.773989 0.101211 11.00000 0.03926 0.03786 = 0.03614 0.01436 0.00907 0.00663 N1 3 0.561674 0.686275 -0.125818 11.00000 0.04380 0.04082 = 0.03806 0.02114 0.01058 0.00739 N4 3 0.109301 0.800838 0.179526 11.00000 0.04076 0.03885 = 0.06593 0.02547 0.01403 0.01269 N2 3 0.407969 0.613512 -0.310278 11.00000 0.05610 0.04031 = 0.05507 0.01255 -0.00841 0.00420 C14 1 0.462179 0.589075 -0.160287 11.00000 0.04540 0.04636 = 0.05497 0.03102 0.01354 0.01088 AFIX 43 H14 2 0.444104 0.542136 -0.121292 11.00000 -1.20000 AFIX 0 C15 1 0.383980 0.553882 -0.251059 11.00000 0.04698 0.03749 = 0.06110 0.01585 0.00532 -0.00428 AFIX 43 H15 2 0.310676 0.484729 -0.271677 11.00000 -1.20000 AFIX 0 C12 1 0.511353 0.712967 -0.277763 11.00000 0.04634 0.03833 = 0.05100 0.01837 0.00178 0.00368 C13 1 0.586299 0.748941 -0.185668 11.00000 0.04776 0.03666 = 0.04411 0.02171 -0.00258 -0.00397 AFIX 43 H13 2 0.656615 0.819137 -0.163850 11.00000 -1.20000 AFIX 0 O2A 4 0.639886 0.877515 -0.300347 11.00000 0.05424 0.04989 = 0.04988 0.03082 -0.00871 -0.00415 O1 4 0.471369 0.756087 -0.421639 11.00000 0.12121 0.05501 = 0.05061 0.02741 -0.03440 -0.00813 C11 1 0.536524 0.779386 -0.343990 11.00000 0.05238 0.04823 = 0.04105 0.02034 -0.00426 0.00328 C10 1 0.524773 1.025922 -0.341475 11.00000 0.03314 0.04139 = 0.02757 0.01162 -0.00292 0.00006 C1 1 0.658052 0.960299 -0.348166 11.00000 0.04571 0.03616 = 0.03051 0.01844 -0.00182 0.00563 C5 1 0.542882 1.111271 -0.383921 11.00000 0.04528 0.03512 = 0.03192 0.01290 0.00201 0.00965 C2 1 0.804074 0.975635 -0.390897 11.00000 0.05034 0.04580 = 0.04845 0.01690 0.00690 0.02529 AFIX 43 H2 2 0.893403 0.930375 -0.392076 11.00000 -1.20000 AFIX 0 C9 1 0.376287 1.011584 -0.291958 11.00000 0.04126 0.07091 = 0.03573 0.00625 -0.00040 -0.01681 AFIX 43 H9 2 0.363252 0.953339 -0.263750 11.00000 -1.20000 AFIX 0 C4 1 0.695822 1.128321 -0.430213 11.00000 0.05371 0.04461 = 0.03072 0.02085 0.00416 0.00495 AFIX 43 H4 2 0.710578 1.186552 -0.458383 11.00000 -1.20000 AFIX 0 C3 1 0.819728 1.061277 -0.433848 11.00000 0.04250 0.05583 = 0.04380 0.01904 0.01916 0.01691 AFIX 43 H3 2 0.919911 1.072096 -0.466146 11.00000 -1.20000 AFIX 0 C8 1 0.251471 1.080611 -0.284283 11.00000 0.03862 0.10744 = 0.04534 -0.00249 0.00109 0.00359 AFIX 43 H8 2 0.153990 1.071205 -0.249671 11.00000 -1.20000 AFIX 0 C7 1 0.266927 1.161457 -0.325637 11.00000 0.04508 0.08596 = 0.06537 -0.00929 -0.00228 0.03109 AFIX 43 H7 2 0.179182 1.208509 -0.320556 11.00000 -1.20000 AFIX 0 C6 1 0.407126 1.177333 -0.375087 11.00000 0.05445 0.05609 = 0.05411 0.00841 -0.00737 0.02550 AFIX 43 H6 2 0.413205 1.234645 -0.404382 11.00000 -1.20000 AFIX 0 C30 1 0.183327 0.869443 0.135205 11.00000 0.03487 0.03888 = 0.04376 0.01882 -0.00526 0.00399 AFIX 43 H30 2 0.125320 0.929272 0.129654 11.00000 -1.20000 AFIX 0 C29 1 0.341917 0.856695 0.096896 11.00000 0.03940 0.03910 = 0.04087 0.01630 -0.00133 -0.00502 AFIX 43 H29 2 0.389991 0.908497 0.066831 11.00000 -1.20000 AFIX 0 C28 1 0.357207 0.704405 0.146674 11.00000 0.04629 0.04173 = 0.07160 0.03563 0.02558 0.01566 AFIX 43 H28 2 0.416033 0.644904 0.152234 11.00000 -1.20000 AFIX 0 C27 1 0.199384 0.718483 0.185513 11.00000 0.05242 0.04714 = 0.08037 0.04052 0.02885 0.02715 HG1 6 0.719239 0.754813 0.034567 11.00000 0.03890 0.04417 = 0.04424 0.02699 0.00666 0.00561 CL1 5 0.774718 0.937915 0.031504 11.00000 0.05202 0.04474 = 0.06339 0.02948 0.00463 0.00254 CL2 5 0.763969 0.583227 0.047663 11.00000 0.06016 0.05520 = 0.08518 0.04965 0.01023 0.01260 C20 1 0.044307 0.331542 0.318630 11.00000 0.05293 0.04512 = 0.06057 0.02139 0.01086 0.00780 PART 1 O4A 4 0.254356 0.588658 0.268158 21.00000 0.04163 0.04308 = 0.04989 0.02094 0.01141 0.01032 O3A 4 -0.006309 0.650979 0.285239 21.00000 0.04704 0.05705 = 0.04510 0.03679 0.02040 0.01933 C26A 1 0.136828 0.654191 0.256056 21.00000 0.04303 0.03788 = 0.04227 0.01486 0.00582 0.00321 C24A 1 0.033858 0.385469 0.172418 21.00000 0.05350 0.05004 = 0.03326 0.00064 0.01030 0.02161 AFIX 43 H24A 2 0.060478 0.432917 0.134610 21.00000 -1.20000 AFIX 0 C25A 1 0.095900 0.413117 0.272603 21.00000 0.02366 0.03035 = 0.04036 0.00254 -0.00886 0.00298 C23A 1 -0.070975 0.279206 0.138334 21.00000 0.05502 0.05958 = 0.03451 -0.01049 -0.00611 0.00495 AFIX 43 H23A 2 -0.120295 0.258882 0.075194 21.00000 -1.20000 AFIX 0 C22A 1 -0.104629 0.210632 0.182103 21.00000 0.08334 0.04538 = 0.08311 0.00439 -0.00746 0.00880 AFIX 43 H22A 2 -0.169587 0.140379 0.150650 21.00000 -1.20000 AFIX 0 C21A 1 -0.048093 0.235902 0.276449 21.00000 0.06389 0.03361 = 0.07909 0.02364 0.00345 0.00820 AFIX 43 H21A 2 -0.076404 0.184012 0.310078 21.00000 -1.20000 AFIX 0 C19A 1 0.111486 0.364104 0.415203 21.00000 0.05443 0.05014 = 0.06836 0.03409 0.00772 -0.00195 AFIX 43 H19A 2 0.084157 0.314314 0.450886 21.00000 -1.20000 AFIX 0 C18A 1 0.211768 0.461905 0.458440 21.00000 0.05636 0.06414 = 0.05808 0.03300 0.00805 -0.01270 AFIX 43 H18A 2 0.250839 0.477890 0.522915 21.00000 -1.20000 AFIX 0 C17A 1 0.260434 0.540957 0.411398 21.00000 0.04721 0.03977 = 0.03977 0.00724 -0.00939 -0.01259 AFIX 43 H17A 2 0.331642 0.609009 0.442594 21.00000 -1.20000 AFIX 0 C16A 1 0.200729 0.515367 0.319134 21.00000 0.02993 0.03365 = 0.04461 0.01007 -0.00199 0.00141 PART 2 O4B 4 0.161889 0.528036 0.183411 -21.00000 0.04075 0.02750 = 0.07268 0.01416 0.03353 0.01047 O3B 4 -0.027994 0.641261 0.252176 -21.00000 0.06813 0.06934 = 0.03625 0.04277 0.03350 0.03558 C26B 1 0.087168 0.624642 0.211265 -21.00000 0.03962 0.04051 = 0.04163 0.01049 0.01334 0.00251 C25B 1 0.119093 0.431267 0.298477 -21.00000 0.03753 0.04138 = 0.04501 0.00908 -0.00641 0.00120 C16B 1 0.072651 0.432593 0.202355 -21.00000 0.06865 0.01966 = 0.03301 0.00304 0.01441 0.01748 C17B 1 -0.015597 0.345135 0.129533 -21.00000 0.05405 0.05315 = 0.03990 0.02912 0.00545 0.01810 AFIX 43 H17B 2 -0.034656 0.349220 0.067275 -21.00000 -1.20000 AFIX 0 C18B 1 -0.074800 0.249242 0.156073 -21.00000 0.08981 0.04734 = 0.07240 0.03357 -0.03071 -0.00359 AFIX 43 H18B 2 -0.126877 0.185566 0.107271 -21.00000 -1.20000 AFIX 0 C19B 1 -0.064575 0.240731 0.238972 -21.00000 0.06123 0.03007 = 0.05611 0.02401 0.01643 0.00070 AFIX 43 H19B 2 -0.124730 0.177764 0.251591 -21.00000 -1.20000 AFIX 0 C21B 1 0.060392 0.317060 0.406317 -21.00000 0.07533 0.05112 = 0.06057 0.01828 0.00168 0.00259 AFIX 43 H21B 2 0.007152 0.251848 0.418279 -21.00000 -1.20000 AFIX 0 C22B 1 0.156770 0.401072 0.475581 -21.00000 0.07113 0.07755 = 0.06115 0.01311 0.00600 -0.00037 AFIX 43 H22B 2 0.162344 0.395273 0.537782 -21.00000 -1.20000 AFIX 0 C23B 1 0.246429 0.493831 0.460271 -21.00000 0.06637 0.05634 = 0.04531 -0.00530 -0.02747 -0.00313 AFIX 43 H23B 2 0.327487 0.543364 0.507688 -21.00000 -1.20000 AFIX 0 C24B 1 0.215513 0.513878 0.372699 -21.00000 0.05277 0.03385 = 0.06369 0.00914 -0.02708 0.00884 AFIX 43 H24B 2 0.259989 0.582999 0.364431 -21.00000 -1.20000 AFIX 0 HKLF 4 REM AS15-2 in P-1 REM wR2 = 0.1520, GooF = S = 1.077, Restrained GooF = 1.063 for all data REM R1 = 0.0593 for 6011 Fo > 4sig(Fo) and 0.0663 for all 6864 data REM 479 parameters refined using 204 restraints END WGHT 0.0431 0.8759 REM Highest difference peak 1.698, deepest hole -2.920, 1-sigma level 0.186 Q1 1 0.6583 0.6807 0.0142 11.00000 0.05 1.70 Q2 1 0.7829 0.7165 -0.0117 11.00000 0.05 1.56 Q3 1 0.7819 0.8306 0.0594 11.00000 0.05 1.54 Q4 1 0.8727 0.7468 0.0404 11.00000 0.05 1.51 Q5 1 0.4222 0.9006 -0.2556 11.00000 0.05 1.43 Q6 1 0.6306 0.8184 0.1019 11.00000 0.05 1.35 Q7 1 0.7760 0.7402 0.0075 11.00000 0.05 1.33 Q8 1 0.5797 0.7838 0.0401 11.00000 0.05 1.32 Q9 1 0.5607 0.7576 0.0207 11.00000 0.05 1.30 Q10 1 0.6221 0.6439 -0.0313 11.00000 0.05 0.90 Q11 1 0.3878 0.8005 -0.3191 11.00000 0.05 0.90 Q12 1 0.3142 0.7770 -0.3895 11.00000 0.05 0.85 Q13 1 0.8272 0.8706 0.1052 11.00000 0.05 0.80 Q14 1 0.4165 0.7105 -0.2557 11.00000 0.05 0.79 Q15 1 0.6752 0.7393 0.1179 11.00000 0.05 0.79 Q16 1 0.6157 0.6021 0.0407 11.00000 0.05 0.75 Q17 1 0.5471 0.6637 0.0242 11.00000 0.05 0.74 Q18 1 0.7785 0.7735 -0.0441 11.00000 0.05 0.71 Q19 1 0.8532 0.7035 0.1231 11.00000 0.05 0.69 Q20 1 0.7800 0.9790 0.0724 11.00000 0.05 0.66 ; _shelx_res_checksum 97306 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 N3 N 0.4280(8) 0.7740(5) 0.1012(4) 0.0367(12) Uani 1 1 d . . . . . N1 N 0.5617(8) 0.6863(5) -0.1258(4) 0.0385(12) Uani 1 1 d . . . . . N4 N 0.1093(9) 0.8008(5) 0.1795(5) 0.0455(14) Uani 1 1 d . . . . . N2 N 0.4080(10) 0.6135(6) -0.3103(5) 0.0514(16) Uani 1 1 d . . . . . C14 C 0.4622(10) 0.5891(6) -0.1603(5) 0.0448(16) Uani 1 1 d . . . . . H14 H 0.444104 0.542136 -0.121292 0.054 Uiso 1 1 calc R U . . . C15 C 0.3840(11) 0.5539(7) -0.2511(6) 0.0491(18) Uani 1 1 d . . . . . H15 H 0.310676 0.484729 -0.271677 0.059 Uiso 1 1 calc R U . . . C12 C 0.5114(11) 0.7130(6) -0.2778(5) 0.0444(16) Uani 1 1 d . . . . . C13 C 0.5863(10) 0.7489(6) -0.1857(5) 0.0418(15) Uani 1 1 d . . . . . H13 H 0.656615 0.819137 -0.163850 0.050 Uiso 1 1 calc R U . . . O2A O 0.6399(8) 0.8775(5) -0.3003(4) 0.0492(13) Uani 1 1 d . . . . . O1 O 0.4714(11) 0.7561(5) -0.4216(4) 0.076(2) Uani 1 1 d . . . . . C11 C 0.5365(11) 0.7794(7) -0.3440(5) 0.0462(17) Uani 1 1 d . . . . . C10 C 0.5248(9) 1.0259(6) -0.3415(4) 0.0343(13) Uani 1 1 d . . . . . C1 C 0.6581(10) 0.9603(6) -0.3482(4) 0.0358(13) Uani 1 1 d . . . . . C5 C 0.5429(10) 1.1113(6) -0.3839(4) 0.0365(14) Uani 1 1 d . . . . . C2 C 0.8041(11) 0.9756(6) -0.3909(5) 0.0459(17) Uani 1 1 d . . . . . H2 H 0.893403 0.930375 -0.392076 0.055 Uiso 1 1 calc R U . . . C9 C 0.3763(10) 1.0116(8) -0.2920(5) 0.054(2) Uani 1 1 d . . . . . H9 H 0.363252 0.953339 -0.263750 0.064 Uiso 1 1 calc R U . . . C4 C 0.6958(10) 1.1283(6) -0.4302(4) 0.0411(15) Uani 1 1 d . . . . . H4 H 0.710578 1.186552 -0.458383 0.049 Uiso 1 1 calc R U . . . C3 C 0.8197(10) 1.0613(7) -0.4338(5) 0.0452(17) Uani 1 1 d . . . . . H3 H 0.919911 1.072096 -0.466146 0.054 Uiso 1 1 calc R U . . . C8 C 0.2515(12) 1.0806(11) -0.2843(6) 0.070(3) Uani 1 1 d . . . . . H8 H 0.153990 1.071205 -0.249671 0.084 Uiso 1 1 calc R U . . . C7 C 0.2669(12) 1.1615(10) -0.3256(7) 0.071(3) Uani 1 1 d . . . . . H7 H 0.179182 1.208509 -0.320556 0.085 Uiso 1 1 calc R U . . . C6 C 0.4071(12) 1.1773(8) -0.3751(6) 0.055(2) Uani 1 1 d . . . . . H6 H 0.413205 1.234645 -0.404382 0.067 Uiso 1 1 calc R U . . . C30 C 0.1833(9) 0.8694(6) 0.1352(5) 0.0381(14) Uani 1 1 d . . . . . H30 H 0.125320 0.929272 0.129654 0.046 Uiso 1 1 calc R U . . . C29 C 0.3419(10) 0.8567(6) 0.0969(5) 0.0398(14) Uani 1 1 d . . . . . H29 H 0.389991 0.908497 0.066831 0.048 Uiso 1 1 calc R U . . . C28 C 0.3572(11) 0.7044(6) 0.1467(6) 0.0478(18) Uani 1 1 d . . . . . H28 H 0.416033 0.644904 0.152234 0.057 Uiso 1 1 calc R U . . . C27 C 0.1994(11) 0.7185(7) 0.1855(6) 0.053(2) Uani 1 1 d . . . . . Hg1 Hg 0.71924(3) 0.75481(2) 0.03457(2) 0.03937(11) Uani 1 1 d . . . . . Cl1 Cl 0.7747(3) 0.93792(16) 0.03150(14) 0.0509(4) Uani 1 1 d . . . . . Cl2 Cl 0.7640(3) 0.58323(18) 0.04766(17) 0.0601(5) Uani 1 1 d . . . . . C20 C 0.0443(11) 0.3315(7) 0.3186(6) 0.0514(17) Uani 1 1 d . U . . . O4A O 0.2544(11) 0.5887(7) 0.2682(6) 0.043(2) Uani 0.601(11) 1 d . U P A 1 O3A O -0.006(3) 0.6510(17) 0.2852(9) 0.044(3) Uani 0.601(11) 1 d . U P A 1 C26A C 0.1368(19) 0.6542(12) 0.2561(10) 0.041(3) Uani 0.601(11) 1 d . U P A 1 C24A C 0.034(2) 0.3855(16) 0.1724(11) 0.047(3) Uani 0.601(11) 1 d . U P A 1 H24A H 0.060478 0.432917 0.134610 0.056 Uiso 0.601(11) 1 calc R U P A 1 C25A C 0.0959(15) 0.4131(14) 0.2726(11) 0.034(3) Uani 0.601(11) 1 d . U P A 1 C23A C -0.071(3) 0.279(2) 0.1383(12) 0.056(5) Uani 0.601(11) 1 d . U P A 1 H23A H -0.120295 0.258882 0.075194 0.067 Uiso 0.601(11) 1 calc R U P A 1 C22A C -0.105(3) 0.2106(17) 0.1821(18) 0.074(5) Uani 0.601(11) 1 d . U P A 1 H22A H -0.169587 0.140379 0.150650 0.089 Uiso 0.601(11) 1 calc R U P A 1 C21A C -0.048(3) 0.2359(14) 0.2764(14) 0.057(4) Uani 0.601(11) 1 d . U P A 1 H21A H -0.076404 0.184012 0.310078 0.069 Uiso 0.601(11) 1 calc R U P A 1 C19A C 0.111(2) 0.3641(15) 0.4152(13) 0.055(3) Uani 0.601(11) 1 d . U P A 1 H19A H 0.084157 0.314314 0.450886 0.066 Uiso 0.601(11) 1 calc R U P A 1 C18A C 0.212(3) 0.4619(19) 0.4584(16) 0.058(5) Uani 0.601(11) 1 d . U P A 1 H18A H 0.250839 0.477890 0.522915 0.070 Uiso 0.601(11) 1 calc R U P A 1 C17A C 0.260(2) 0.5410(12) 0.4114(11) 0.045(3) Uani 0.601(11) 1 d . U P A 1 H17A H 0.331642 0.609009 0.442594 0.054 Uiso 0.601(11) 1 calc R U P A 1 C16A C 0.2007(16) 0.5154(10) 0.3191(10) 0.037(3) Uani 0.601(11) 1 d . U P A 1 O4B O 0.1619(17) 0.5280(10) 0.1834(10) 0.046(4) Uani 0.399(11) 1 d . U P A 2 O3B O -0.028(5) 0.641(3) 0.2522(13) 0.049(6) Uani 0.399(11) 1 d . U P A 2 C26B C 0.087(3) 0.6246(18) 0.2113(15) 0.041(4) Uani 0.399(11) 1 d . U P A 2 C25B C 0.119(3) 0.431(3) 0.2985(19) 0.043(5) Uani 0.399(11) 1 d . U P A 2 C16B C 0.073(3) 0.4326(16) 0.2024(15) 0.040(5) Uani 0.399(11) 1 d . U P A 2 C17B C -0.016(3) 0.345(2) 0.1295(17) 0.045(5) Uani 0.399(11) 1 d . U P A 2 H17B H -0.034656 0.349220 0.067275 0.054 Uiso 0.399(11) 1 calc R U P A 2 C18B C -0.075(6) 0.249(3) 0.156(3) 0.069(9) Uani 0.399(11) 1 d . U P A 2 H18B H -0.126877 0.185566 0.107271 0.082 Uiso 0.399(11) 1 calc R U P A 2 C19B C -0.065(4) 0.241(2) 0.239(2) 0.047(5) Uani 0.399(11) 1 d . U P A 2 H19B H -0.124730 0.177764 0.251591 0.056 Uiso 0.399(11) 1 calc R U P A 2 C21B C 0.060(4) 0.317(2) 0.4063(18) 0.063(6) Uani 0.399(11) 1 d . U P A 2 H21B H 0.007152 0.251848 0.418279 0.075 Uiso 0.399(11) 1 calc R U P A 2 C22B C 0.157(4) 0.401(3) 0.476(2) 0.072(6) Uani 0.399(11) 1 d . U P A 2 H22B H 0.162344 0.395273 0.537782 0.087 Uiso 0.399(11) 1 calc R U P A 2 C23B C 0.246(5) 0.494(3) 0.460(2) 0.062(8) Uani 0.399(11) 1 d . U P A 2 H23B H 0.327487 0.543364 0.507688 0.075 Uiso 0.399(11) 1 calc R U P A 2 C24B C 0.216(3) 0.514(2) 0.373(2) 0.052(6) Uani 0.399(11) 1 d . U P A 2 H24B H 0.259989 0.582999 0.364431 0.062 Uiso 0.399(11) 1 calc R U P A 2 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 N3 0.039(3) 0.038(3) 0.036(3) 0.014(2) 0.009(2) 0.007(3) N1 0.044(3) 0.041(3) 0.038(3) 0.021(2) 0.011(2) 0.007(3) N4 0.041(3) 0.039(3) 0.066(4) 0.025(3) 0.014(3) 0.013(3) N2 0.056(4) 0.040(3) 0.055(4) 0.013(3) -0.008(3) 0.004(3) C14 0.045(4) 0.046(4) 0.055(4) 0.031(3) 0.014(3) 0.011(4) C15 0.047(4) 0.037(4) 0.061(4) 0.016(3) 0.005(4) -0.004(4) C12 0.046(4) 0.038(4) 0.051(4) 0.018(3) 0.002(3) 0.004(3) C13 0.048(4) 0.037(3) 0.044(3) 0.022(3) -0.003(3) -0.004(3) O2A 0.054(3) 0.050(3) 0.050(3) 0.031(2) -0.009(2) -0.004(3) O1 0.121(6) 0.055(4) 0.051(3) 0.027(3) -0.034(4) -0.008(4) C11 0.052(4) 0.048(4) 0.041(3) 0.020(3) -0.004(3) 0.003(4) C10 0.033(3) 0.041(3) 0.028(3) 0.012(2) -0.003(2) 0.000(3) C1 0.046(4) 0.036(3) 0.031(3) 0.018(2) -0.002(3) 0.006(3) C5 0.045(4) 0.035(3) 0.032(3) 0.013(2) 0.002(3) 0.010(3) C2 0.050(4) 0.046(4) 0.048(4) 0.017(3) 0.007(3) 0.025(4) C9 0.041(4) 0.071(6) 0.036(3) 0.006(3) 0.000(3) -0.017(4) C4 0.054(4) 0.045(4) 0.031(3) 0.021(3) 0.004(3) 0.005(3) C3 0.043(4) 0.056(4) 0.044(4) 0.019(3) 0.019(3) 0.017(4) C8 0.039(4) 0.107(9) 0.045(4) -0.002(5) 0.001(4) 0.004(5) C7 0.045(5) 0.086(7) 0.065(6) -0.009(5) -0.002(4) 0.031(5) C6 0.054(5) 0.056(5) 0.054(4) 0.008(4) -0.007(4) 0.026(4) C30 0.035(3) 0.039(3) 0.044(3) 0.019(3) -0.005(3) 0.004(3) C29 0.039(3) 0.039(3) 0.041(3) 0.016(3) -0.001(3) -0.005(3) C28 0.046(4) 0.042(4) 0.072(5) 0.036(4) 0.026(4) 0.016(4) C27 0.052(5) 0.047(4) 0.080(5) 0.041(4) 0.029(4) 0.027(4) Hg1 0.03890(17) 0.04417(17) 0.04424(17) 0.02699(12) 0.00666(12) 0.00561(14) Cl1 0.0520(10) 0.0447(9) 0.0634(11) 0.0295(8) 0.0046(9) 0.0025(9) Cl2 0.0602(12) 0.0552(11) 0.0852(14) 0.0496(11) 0.0102(11) 0.0126(11) C20 0.053(4) 0.045(4) 0.061(4) 0.021(3) 0.011(3) 0.008(4) O4A 0.042(4) 0.043(5) 0.050(5) 0.021(4) 0.011(4) 0.010(4) O3A 0.047(6) 0.057(6) 0.045(8) 0.037(8) 0.020(8) 0.019(5) C26A 0.043(6) 0.038(7) 0.042(7) 0.015(6) 0.006(6) 0.003(6) C24A 0.053(9) 0.050(9) 0.033(7) 0.001(6) 0.010(7) 0.022(7) C25A 0.024(5) 0.030(6) 0.040(7) 0.003(4) -0.009(5) 0.003(5) C23A 0.055(9) 0.060(11) 0.035(7) -0.010(6) -0.006(7) 0.005(9) C22A 0.083(13) 0.045(9) 0.083(11) 0.004(8) -0.007(10) 0.009(9) C21A 0.064(9) 0.034(6) 0.079(10) 0.024(7) 0.003(9) 0.008(6) C19A 0.054(9) 0.050(8) 0.068(7) 0.034(7) 0.008(7) -0.002(7) C18A 0.056(11) 0.064(11) 0.058(8) 0.033(8) 0.008(7) -0.013(9) C17A 0.047(8) 0.040(7) 0.040(7) 0.007(6) -0.009(6) -0.013(6) C16A 0.030(5) 0.034(6) 0.045(7) 0.010(5) -0.002(5) 0.001(5) O4B 0.041(7) 0.027(6) 0.073(9) 0.014(5) 0.034(6) 0.010(6) O3B 0.068(14) 0.069(12) 0.036(11) 0.043(11) 0.034(11) 0.036(10) C26B 0.040(10) 0.041(10) 0.042(10) 0.010(8) 0.013(8) 0.003(9) C25B 0.038(11) 0.041(10) 0.045(10) 0.009(8) -0.006(8) 0.001(8) C16B 0.069(14) 0.020(8) 0.033(10) 0.003(7) 0.014(9) 0.017(10) C17B 0.054(13) 0.053(14) 0.040(10) 0.029(10) 0.005(10) 0.018(11) C18B 0.09(2) 0.047(15) 0.072(11) 0.034(11) -0.031(15) -0.004(15) C19B 0.061(14) 0.030(9) 0.056(10) 0.024(8) 0.016(10) 0.001(8) C21B 0.075(17) 0.051(12) 0.061(9) 0.018(9) 0.002(10) 0.003(11) C22B 0.071(15) 0.078(15) 0.061(9) 0.013(10) 0.006(11) 0.000(13) C23B 0.066(17) 0.056(14) 0.045(11) -0.005(10) -0.027(12) -0.003(11) C24B 0.053(12) 0.034(8) 0.064(14) 0.009(9) -0.027(11) 0.009(7) 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' N N 0.0061 0.0033 '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' 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' 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 C29 N3 C28 117.1(6) . . ? C29 N3 Hg1 121.2(5) . . ? C28 N3 Hg1 121.7(5) . . ? C14 N1 C13 116.3(6) . . ? C14 N1 Hg1 124.9(4) . . ? C13 N1 Hg1 118.7(5) . . ? C30 N4 C27 115.6(6) . . ? C15 N2 C12 117.3(7) . . ? N1 C14 C15 122.2(7) . . ? N2 C15 C14 122.1(7) . . ? N2 C12 C13 120.2(7) . . ? N2 C12 C11 117.0(7) . . ? C13 C12 C11 122.8(7) . . ? N1 C13 C12 121.8(7) . . ? C11 O2A C1 118.2(6) . . ? O1 C11 O2A 123.6(7) . . ? O1 C11 C12 126.3(8) . . ? O2A C11 C12 109.9(6) . . ? C1 C10 C5 117.7(6) . . ? C1 C10 C9 122.8(7) . . ? C5 C10 C9 119.5(7) . . ? C2 C1 C10 123.9(6) . . ? C2 C1 O2A 119.5(6) . . ? C10 C1 O2A 116.4(6) . . ? C10 C5 C6 116.5(7) . . ? C10 C5 C4 119.3(6) . . ? C6 C5 C4 124.2(7) . . ? C1 C2 C3 117.7(6) . . ? C8 C9 C10 120.9(9) . . ? C3 C4 C5 119.7(7) . . ? C4 C3 C2 121.7(7) . . ? C7 C8 C9 120.0(9) . . ? C8 C7 C6 121.1(9) . . ? C7 C6 C5 122.1(9) . . ? N4 C30 C29 122.4(7) . . ? N3 C29 C30 121.6(7) . . ? N3 C28 C27 120.8(7) . . ? N4 C27 C28 122.4(7) . . ? N4 C27 C26B 112.7(10) . . ? C28 C27 C26B 122.5(9) . . ? N4 C27 C26A 116.1(8) . . ? C28 C27 C26A 120.4(8) . . ? Cl2 Hg1 Cl1 160.76(9) . . ? Cl2 Hg1 N1 96.90(15) . . ? Cl1 Hg1 N1 94.12(14) . . ? Cl2 Hg1 N3 100.81(15) . . ? Cl1 Hg1 N3 95.32(15) . . ? N1 Hg1 N3 87.81(19) . . ? C21A C20 C25A 123.8(12) . . ? C21A C20 C19A 123.4(13) . . ? C25A C20 C19A 112.7(11) . . ? C21B C20 C25B 123.1(17) . . ? C21B C20 C19B 118.8(17) . . ? C25B C20 C19B 117.9(14) . . ? C26A O4A C16A 115.0(10) . . ? O3A C26A O4A 123.9(14) . . ? O3A C26A C27 125.2(14) . . ? O4A C26A C27 110.1(10) . . ? C23A C24A C25A 112.6(16) . . ? C16A C25A C20 122.9(14) . . ? C16A C25A C24A 120.9(18) . . ? C20 C25A C24A 116.2(14) . . ? C22A C23A C24A 127.3(19) . . ? C23A C22A C21A 121(2) . . ? C20 C21A C22A 119.4(17) . . ? C18A C19A C20 123.6(16) . . ? C19A C18A C17A 122(2) . . ? C16A C17A C18A 117.0(16) . . ? C17A C16A O4A 118.9(12) . . ? C17A C16A C25A 121.3(14) . . ? O4A C16A C25A 119.7(14) . . ? C26B O4B C16B 116.6(14) . . ? O3B C26B O4B 129(2) . . ? O3B C26B C27 121(2) . . ? O4B C26B C27 109.8(13) . . ? C24B C25B C20 117(3) . . ? C24B C25B C16B 129(3) . . ? C20 C25B C16B 114(2) . . ? C17B C16B O4B 121(2) . . ? C17B C16B C25B 127(2) . . ? O4B C16B C25B 111(2) . . ? C16B C17B C18B 114(2) . . ? C19B C18B C17B 126(4) . . ? C18B C19B C20 120(3) . . ? C22B C21B C20 117(3) . . ? C21B C22B C23B 124(3) . . ? C22B C23B C24B 119(2) . . ? C25B C24B C23B 120(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 N3 C29 1.326(9) . ? N3 C28 1.346(9) . ? N3 Hg1 2.520(6) . ? N1 C14 1.327(10) . ? N1 C13 1.363(8) . ? N1 Hg1 2.501(6) . ? N4 C30 1.334(9) . ? N4 C27 1.347(9) . ? N2 C15 1.326(10) . ? N2 C12 1.361(10) . ? C14 C15 1.382(11) . ? C12 C13 1.391(10) . ? C12 C11 1.479(10) . ? O2A C11 1.368(10) . ? O2A C1 1.430(8) . ? O1 C11 1.182(9) . ? C10 C1 1.394(9) . ? C10 C5 1.403(9) . ? C10 C9 1.418(10) . ? C1 C2 1.347(10) . ? C5 C6 1.411(10) . ? C5 C4 1.426(10) . ? C2 C3 1.411(11) . ? C9 C8 1.369(14) . ? C4 C3 1.352(10) . ? C8 C7 1.340(16) . ? C7 C6 1.369(14) . ? C30 C29 1.387(10) . ? C28 C27 1.387(10) . ? C27 C26B 1.54(2) . ? C27 C26A 1.568(16) . ? Hg1 Cl2 2.310(3) . ? Hg1 Cl1 2.331(3) . ? C20 C21A 1.304(19) . ? C20 C21B 1.37(3) . ? C20 C25A 1.43(2) . ? C20 C19A 1.43(2) . ? C20 C25B 1.45(4) . ? C20 C19B 1.53(3) . ? O4A C26A 1.347(16) . ? O4A C16A 1.402(15) . ? O3A C26A 1.21(2) . ? C24A C23A 1.43(3) . ? C24A C25A 1.47(2) . ? C25A C16A 1.419(19) . ? C23A C22A 1.24(3) . ? C22A C21A 1.39(3) . ? C19A C18A 1.35(3) . ? C18A C17A 1.41(2) . ? C17A C16A 1.363(18) . ? O4B C26B 1.38(2) . ? O4B C16B 1.43(2) . ? O3B C26B 1.11(4) . ? C25B C24B 1.40(3) . ? C25B C16B 1.47(3) . ? C16B C17B 1.39(3) . ? C17B C18B 1.42(4) . ? C18B C19B 1.27(4) . ? C21B C22B 1.37(4) . ? C22B C23B 1.38(4) . ? C23B C24B 1.42(4) . ?