# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Catherine E Housecroft' 'Edwin Constable' 'Jennifer A Zampese' 'Guoqi Zhang.' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Amalgamating metalloligands with coordination networks ; # Attachment 'GQ100.CIF' data_gq100 _database_code_depnum_ccdc_archive 'CCDC 755410' #TrackingRef 'GQ100.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H28 Hg N4 Ni O4' _chemical_formula_sum 'C26 H28 Hg N4 Ni O4' _chemical_formula_weight 719.80 _chemical_absolute_configuration ad 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.623(3) _cell_length_b 14.347(3) _cell_length_c 26.022(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5086.2(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 6.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1715 _exptl_absorpt_correction_T_max 0.7270 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; Due to the large atoms present, significant peaks of residual electron density remain in the difference map. These are Q1 3.50 and Q4 3.19 (0.837 and 0.844 from Hg1a) and Q2 3.50 and Q3 3.29 (0.849 and 0.844 from Hg1b) These peaks are the result of fourier truncation surrounding the heavy Hg atoms and therefore remain un-assigned. ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125195 _diffrn_reflns_av_R_equivalents 0.2027 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9989 _reflns_number_gt 9934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+3.3721P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(6) _refine_ls_number_reflns 9989 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1B Hg 0.102493(17) 0.051659(18) 0.628017(9) 0.02448(10) Uani 1 1 d . . . Ni1B Ni 0.11943(5) 0.01112(5) 0.76269(3) 0.01937(17) Uani 1 1 d . . . N1B N 0.1149(4) 0.0817(4) 0.82170(19) 0.0231(10) Uani 1 1 d . . . N2B N 0.1320(4) -0.0890(4) 0.80704(19) 0.0206(10) Uani 1 1 d . . . O1B O 0.1355(4) 0.2368(3) 0.64262(18) 0.0296(10) Uani 1 1 d . . . O2B O 0.1214(3) 0.1135(3) 0.71829(16) 0.0233(9) Uani 1 1 d . . . O3B O 0.1100(3) -0.0606(3) 0.70314(16) 0.0225(9) Uani 1 1 d . . . O4B O 0.0847(4) -0.1384(4) 0.61069(16) 0.0323(11) Uani 1 1 d . . . C1B C 0.1463(7) 0.2526(6) 0.5514(3) 0.047(2) Uani 1 1 d . . . H1B1 H 0.0848 0.2174 0.5498 0.071 Uiso 1 1 calc R . . H1B2 H 0.2019 0.2098 0.5479 0.071 Uiso 1 1 calc R . . H1B3 H 0.1480 0.2984 0.5235 0.071 Uiso 1 1 calc R . . C2B C 0.1528(5) 0.3020(5) 0.6021(3) 0.0299(14) Uani 1 1 d . . . H2BA H 0.2187 0.3302 0.6061 0.036 Uiso 1 1 calc R . . H2BB H 0.1034 0.3526 0.6035 0.036 Uiso 1 1 calc R . . C3B C 0.1376(5) 0.2705(5) 0.6917(3) 0.0250(13) Uani 1 1 d . . . C4B C 0.1299(4) 0.2019(5) 0.7313(3) 0.0235(13) Uani 1 1 d . . . C5B C 0.1321(4) 0.2330(5) 0.7823(3) 0.0262(13) Uani 1 1 d . . . C6B C 0.1381(5) 0.3297(5) 0.7938(3) 0.0295(14) Uani 1 1 d . . . H6BA H 0.1371 0.3501 0.8285 0.035 Uiso 1 1 calc R . . C7B C 0.1453(5) 0.3937(5) 0.7548(3) 0.0331(16) Uani 1 1 d . . . H7BA H 0.1500 0.4583 0.7626 0.040 Uiso 1 1 calc R . . C8B C 0.1457(5) 0.3635(5) 0.7032(3) 0.0326(15) Uani 1 1 d . . . H8BA H 0.1517 0.4078 0.6763 0.039 Uiso 1 1 calc R . . C9B C 0.1211(4) 0.1711(5) 0.8249(2) 0.0250(13) Uani 1 1 d . . . H9BA H 0.1181 0.1980 0.8582 0.030 Uiso 1 1 calc R . . C10B C 0.0968(4) 0.0255(5) 0.8682(2) 0.0241(12) Uani 1 1 d . . . H10A H 0.0259 0.0076 0.8679 0.029 Uiso 1 1 calc R . . C11B C 0.1183(5) 0.0691(5) 0.9212(2) 0.0318(15) Uani 1 1 d . . . H11A H 0.1874 0.0903 0.9227 0.038 Uiso 1 1 calc R . . H11B H 0.0752 0.1237 0.9268 0.038 Uiso 1 1 calc R . . C12B C 0.0998(6) -0.0039(7) 0.9629(3) 0.0445(19) Uani 1 1 d . . . H12A H 0.1169 0.0229 0.9968 0.053 Uiso 1 1 calc R . . H12B H 0.0291 -0.0198 0.9634 0.053 Uiso 1 1 calc R . . C13B C 0.1587(7) -0.0914(7) 0.9545(3) 0.045(2) Uani 1 1 d . . . H13A H 0.1422 -0.1372 0.9817 0.054 Uiso 1 1 calc R . . H13B H 0.2295 -0.0767 0.9574 0.054 Uiso 1 1 calc R . . C14B C 0.1385(5) -0.1342(5) 0.9022(2) 0.0325(15) Uani 1 1 d . . . H14A H 0.0699 -0.1568 0.9008 0.039 Uiso 1 1 calc R . . H14B H 0.1825 -0.1883 0.8968 0.039 Uiso 1 1 calc R . . C15B C 0.1552(4) -0.0624(5) 0.8595(2) 0.0245(12) Uani 1 1 d . . . H15A H 0.2263 -0.0448 0.8604 0.029 Uiso 1 1 calc R . . C16B C 0.1300(4) -0.1769(5) 0.7937(2) 0.0213(12) Uani 1 1 d . . . H16A H 0.1380 -0.2217 0.8202 0.026 Uiso 1 1 calc R . . C17B C 0.1169(4) -0.2116(4) 0.7427(2) 0.0207(12) Uani 1 1 d . . . C18B C 0.1077(4) -0.1524(4) 0.7004(3) 0.0218(12) Uani 1 1 d . . . C19B C 0.0992(4) -0.1961(4) 0.6507(2) 0.0240(12) Uani 1 1 d . . . C20B C 0.1051(4) -0.2921(4) 0.6466(2) 0.0232(12) Uani 1 1 d . . . H20A H 0.1025 -0.3202 0.6136 0.028 Uiso 1 1 calc R . . C21B C 0.1148(5) -0.3484(5) 0.6900(3) 0.0274(13) Uani 1 1 d . . . H21A H 0.1174 -0.4142 0.6864 0.033 Uiso 1 1 calc R . . C22B C 0.1207(5) -0.3096(5) 0.7375(2) 0.0244(13) Uani 1 1 d . . . H22A H 0.1272 -0.3480 0.7670 0.029 Uiso 1 1 calc R . . C23B C 0.0774(6) -0.1806(5) 0.5605(2) 0.0355(16) Uani 1 1 d . . . H23A H 0.0191 -0.2217 0.5589 0.043 Uiso 1 1 calc R . . H23B H 0.1365 -0.2185 0.5534 0.043 Uiso 1 1 calc R . . C24B C 0.0684(8) -0.1032(6) 0.5218(3) 0.057(2) Uani 1 1 d . . . H24A H 0.1292 -0.0667 0.5213 0.086 Uiso 1 1 calc R . . H24B H 0.0133 -0.0628 0.5311 0.086 Uiso 1 1 calc R . . H24C H 0.0569 -0.1299 0.4876 0.086 Uiso 1 1 calc R . . C50B C -0.0447(5) 0.0853(5) 0.6274(2) 0.0286(13) Uani 1 1 d . . . N50B N -0.1227(5) 0.1100(5) 0.6267(3) 0.0418(14) Uani 1 1 d . . . N60B N 0.3191(4) 0.0146(4) 0.5868(2) 0.0349(13) Uani 1 1 d . . . C60B C 0.2433(5) 0.0278(5) 0.6025(2) 0.0304(14) Uani 1 1 d . . . Hg1A Hg 0.403156(17) 0.541574(18) 0.626711(9) 0.02420(10) Uani 1 1 d . . . Ni1A Ni 0.38043(5) 0.50213(5) 0.76118(3) 0.01838(16) Uani 1 1 d . . . N1A N 0.3580(4) 0.5727(4) 0.81932(17) 0.0212(10) Uani 1 1 d . . . N2A N 0.3929(4) 0.4030(4) 0.80638(19) 0.0229(11) Uani 1 1 d . . . O1A O 0.3681(4) 0.7268(3) 0.64030(17) 0.0284(10) Uani 1 1 d . . . O2A O 0.3716(3) 0.6029(3) 0.71640(16) 0.0216(9) Uani 1 1 d . . . O3A O 0.3993(3) 0.4302(3) 0.70261(15) 0.0224(8) Uani 1 1 d . . . O4A O 0.4217(4) 0.3521(4) 0.61032(16) 0.0314(10) Uani 1 1 d . . . C1A C 0.3547(7) 0.7428(6) 0.5489(3) 0.0431(19) Uani 1 1 d . . . H1A1 H 0.3019 0.6966 0.5474 0.065 Uiso 1 1 calc R . . H1A2 H 0.4183 0.7114 0.5456 0.065 Uiso 1 1 calc R . . H1A3 H 0.3468 0.7876 0.5208 0.065 Uiso 1 1 calc R . . C2A C 0.3506(5) 0.7930(4) 0.5991(2) 0.0274(13) Uani 1 1 d . . . H2AA H 0.4010 0.8427 0.6000 0.033 Uiso 1 1 calc R . . H2AB H 0.2853 0.8224 0.6035 0.033 Uiso 1 1 calc R . . C3A C 0.3653(5) 0.7613(5) 0.6894(3) 0.0247(13) Uani 1 1 d . . . C4A C 0.3682(4) 0.6924(4) 0.7285(2) 0.0209(12) Uani 1 1 d . . . C5A C 0.3650(4) 0.7248(5) 0.7806(2) 0.0229(12) Uani 1 1 d . . . C6A C 0.3647(4) 0.8207(5) 0.7905(3) 0.0259(13) Uani 1 1 d . . . H6AA H 0.3659 0.8417 0.8251 0.031 Uiso 1 1 calc R . . C7A C 0.3626(5) 0.8852(5) 0.7516(2) 0.0278(15) Uani 1 1 d . . . H7AA H 0.3619 0.9499 0.7593 0.033 Uiso 1 1 calc R . . C8A C 0.3615(4) 0.8552(4) 0.7009(3) 0.0269(13) Uani 1 1 d . . . H8AA H 0.3581 0.8996 0.6738 0.032 Uiso 1 1 calc R . . C9A C 0.3574(4) 0.6620(5) 0.8219(2) 0.0249(13) Uani 1 1 d . . . H9AA H 0.3511 0.6885 0.8552 0.030 Uiso 1 1 calc R . . C10A C 0.3365(4) 0.5148(4) 0.8650(2) 0.0203(11) Uani 1 1 d . . . H10B H 0.2670 0.4930 0.8625 0.024 Uiso 1 1 calc R . . C11A C 0.3505(5) 0.5622(5) 0.9182(2) 0.0323(15) Uani 1 1 d . . . H11C H 0.4190 0.5841 0.9220 0.039 Uiso 1 1 calc R . . H11D H 0.3062 0.6166 0.9213 0.039 Uiso 1 1 calc R . . C12A C 0.3266(6) 0.4907(7) 0.9594(2) 0.0421(19) Uani 1 1 d . . . H12C H 0.3390 0.5185 0.9936 0.051 Uiso 1 1 calc R . . H12D H 0.2560 0.4748 0.9574 0.051 Uiso 1 1 calc R . . C13A C 0.3862(7) 0.4030(6) 0.9542(3) 0.0416(18) Uani 1 1 d . . . H13C H 0.3642 0.3575 0.9803 0.050 Uiso 1 1 calc R . . H13D H 0.4560 0.4176 0.9611 0.050 Uiso 1 1 calc R . . C14A C 0.3778(6) 0.3584(5) 0.9007(3) 0.0327(14) Uani 1 1 d . . . H14C H 0.4237 0.3051 0.8980 0.039 Uiso 1 1 calc R . . H14D H 0.3103 0.3349 0.8953 0.039 Uiso 1 1 calc R . . C15A C 0.4025(4) 0.4314(5) 0.8602(2) 0.0244(12) Uani 1 1 d . . . H15B H 0.4716 0.4524 0.8660 0.029 Uiso 1 1 calc R . . C16A C 0.3911(4) 0.3147(4) 0.7936(2) 0.0236(12) Uani 1 1 d . . . H16B H 0.3910 0.2703 0.8206 0.028 Uiso 1 1 calc R . . C17A C 0.3983(4) 0.3383(4) 0.6995(2) 0.0216(12) Uani 1 1 d . . . C18A C 0.3893(5) 0.2805(4) 0.7428(2) 0.0237(12) Uani 1 1 d . . . C19A C 0.4072(4) 0.2940(4) 0.6504(2) 0.0226(12) Uani 1 1 d . . . C20A C 0.4042(5) 0.1984(5) 0.6469(2) 0.0258(12) Uani 1 1 d . . . H20B H 0.4112 0.1698 0.6142 0.031 Uiso 1 1 calc R . . C21A C 0.3910(5) 0.1417(5) 0.6909(3) 0.0292(14) Uani 1 1 d . . . H21B H 0.3865 0.0759 0.6875 0.035 Uiso 1 1 calc R . . C22A C 0.3848(5) 0.1812(5) 0.7371(3) 0.0261(13) Uani 1 1 d . . . H22B H 0.3773 0.1431 0.7667 0.031 Uiso 1 1 calc R . . C23A C 0.4283(6) 0.3097(5) 0.5604(2) 0.0364(16) Uani 1 1 d . . . H23C H 0.3697 0.2707 0.5538 0.044 Uiso 1 1 calc R . . H23D H 0.4873 0.2695 0.5584 0.044 Uiso 1 1 calc R . . C24A C 0.4348(9) 0.3869(6) 0.5214(3) 0.059(3) Uani 1 1 d . . . H24D H 0.4890 0.4287 0.5304 0.088 Uiso 1 1 calc R . . H24E H 0.3731 0.4221 0.5212 0.088 Uiso 1 1 calc R . . H24F H 0.4464 0.3603 0.4873 0.088 Uiso 1 1 calc R . . C50A C 0.5513(5) 0.5657(5) 0.6275(3) 0.0333(14) Uani 1 1 d . . . N50A N 0.6327(5) 0.5845(6) 0.6273(3) 0.0497(17) Uani 1 1 d . . . N60A N 0.1821(4) 0.5226(4) 0.5874(2) 0.0306(12) Uani 1 1 d . . . C60A C 0.2593(5) 0.5275(4) 0.6028(2) 0.0275(13) 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 Hg1B 0.02610(15) 0.01656(15) 0.03077(15) 0.00088(9) -0.00024(10) -0.00187(8) Ni1B 0.0168(3) 0.0138(4) 0.0276(3) -0.0007(3) -0.0003(3) 0.0010(3) N1B 0.017(2) 0.023(3) 0.029(2) -0.002(2) 0.0007(19) 0.004(2) N2B 0.017(2) 0.021(3) 0.023(2) -0.003(2) -0.0022(17) 0.006(2) O1B 0.033(3) 0.012(2) 0.044(2) 0.0007(19) 0.0000(19) -0.0037(19) O2B 0.026(2) 0.012(2) 0.032(2) -0.0013(18) 0.0016(17) 0.0017(17) O3B 0.032(2) 0.011(2) 0.0248(19) 0.0003(16) -0.0024(17) -0.0036(19) O4B 0.049(3) 0.026(3) 0.022(2) -0.0040(18) -0.0032(19) -0.003(2) C1B 0.056(5) 0.028(4) 0.057(5) 0.008(4) -0.007(4) -0.013(4) C2B 0.022(3) 0.019(3) 0.048(4) 0.011(3) 0.003(3) -0.006(2) C3B 0.013(3) 0.021(3) 0.041(3) -0.002(3) -0.002(2) -0.002(2) C4B 0.017(3) 0.014(3) 0.040(3) -0.005(3) -0.005(2) -0.001(2) C5B 0.014(3) 0.017(3) 0.048(4) -0.004(3) -0.004(2) 0.001(2) C6B 0.030(3) 0.015(3) 0.044(4) -0.012(3) -0.002(3) -0.005(3) C7B 0.026(3) 0.016(3) 0.058(4) -0.009(3) -0.006(3) -0.001(2) C8B 0.020(3) 0.024(3) 0.054(4) 0.001(3) 0.004(3) 0.002(3) C9B 0.014(2) 0.023(3) 0.038(3) -0.006(3) 0.000(2) 0.004(2) C10B 0.026(3) 0.023(3) 0.023(3) 0.001(2) 0.001(2) 0.006(2) C11B 0.033(3) 0.032(4) 0.031(3) -0.009(3) -0.001(3) 0.006(3) C12B 0.052(4) 0.054(5) 0.027(3) 0.000(3) 0.002(3) 0.010(4) C13B 0.058(5) 0.042(5) 0.035(3) 0.002(3) -0.007(3) 0.014(4) C14B 0.032(3) 0.033(4) 0.032(3) 0.002(3) -0.001(3) 0.004(3) C15B 0.021(3) 0.019(3) 0.033(3) -0.001(3) 0.000(2) 0.005(2) C16B 0.015(3) 0.016(3) 0.033(3) 0.002(2) -0.001(2) 0.001(2) C17B 0.017(3) 0.014(3) 0.031(3) -0.003(2) 0.001(2) -0.001(2) C18B 0.012(3) 0.011(3) 0.043(3) -0.001(2) -0.001(2) -0.001(2) C19B 0.021(3) 0.013(3) 0.037(3) -0.005(2) -0.001(2) 0.004(3) C20B 0.019(3) 0.017(3) 0.034(3) -0.006(2) 0.001(2) -0.001(2) C21B 0.025(3) 0.013(3) 0.045(3) 0.002(3) 0.002(3) -0.001(3) C22B 0.020(3) 0.019(3) 0.034(3) 0.005(3) -0.003(3) 0.001(2) C23B 0.045(4) 0.027(4) 0.034(3) -0.001(3) -0.010(3) -0.008(3) C24B 0.092(7) 0.036(4) 0.044(4) 0.008(4) -0.016(4) -0.019(5) C50B 0.029(3) 0.026(3) 0.031(3) 0.001(3) -0.004(3) 0.000(3) N50B 0.032(3) 0.042(4) 0.051(3) -0.004(3) -0.001(3) -0.003(3) N60B 0.035(3) 0.022(3) 0.047(3) -0.008(3) 0.006(3) -0.002(3) C60B 0.044(4) 0.016(3) 0.031(3) -0.001(3) 0.003(3) 0.003(3) Hg1A 0.02688(15) 0.01664(15) 0.02907(15) 0.00041(9) 0.00043(10) 0.00144(8) Ni1A 0.0169(3) 0.0136(4) 0.0246(3) 0.0004(3) 0.0003(3) 0.0008(3) N1A 0.020(2) 0.026(3) 0.017(2) -0.002(2) 0.0003(17) -0.004(2) N2A 0.013(2) 0.024(3) 0.031(2) -0.003(2) 0.0017(19) 0.001(2) O1A 0.034(2) 0.015(2) 0.036(2) 0.0062(19) 0.0017(19) 0.003(2) O2A 0.022(2) 0.008(2) 0.035(2) 0.0008(17) -0.0001(16) 0.0009(16) O3A 0.026(2) 0.014(2) 0.0278(19) -0.0027(17) 0.0022(16) 0.0046(18) O4A 0.043(3) 0.023(2) 0.027(2) -0.0056(19) 0.0027(19) 0.006(2) C1A 0.060(5) 0.034(4) 0.035(3) 0.008(3) -0.002(3) 0.005(4) C2A 0.023(3) 0.014(3) 0.044(3) 0.012(3) 0.002(3) 0.002(2) C3A 0.017(3) 0.019(3) 0.039(3) 0.003(3) 0.002(2) 0.005(2) C4A 0.017(3) 0.011(3) 0.035(3) -0.002(2) 0.001(2) 0.002(2) C5A 0.012(3) 0.024(3) 0.032(3) -0.003(3) -0.002(2) 0.000(2) C6A 0.020(3) 0.019(3) 0.039(3) -0.005(3) 0.001(2) 0.002(2) C7A 0.025(3) 0.010(3) 0.049(4) -0.005(3) -0.003(3) 0.004(2) C8A 0.021(3) 0.012(3) 0.047(4) 0.004(3) 0.001(2) -0.002(2) C9A 0.017(3) 0.022(3) 0.035(3) -0.006(3) -0.001(2) 0.002(2) C10A 0.020(3) 0.021(3) 0.020(2) 0.001(2) 0.003(2) 0.002(2) C11A 0.035(3) 0.032(4) 0.030(3) -0.011(3) -0.005(3) 0.009(3) C12A 0.052(4) 0.054(5) 0.021(3) 0.003(3) 0.006(3) 0.003(4) C13A 0.053(5) 0.040(5) 0.032(3) 0.001(3) -0.005(3) -0.003(4) C14A 0.039(3) 0.024(3) 0.035(3) 0.005(3) -0.005(3) -0.001(3) C15A 0.023(3) 0.021(3) 0.029(3) 0.002(2) -0.004(2) -0.002(3) C16A 0.018(3) 0.013(3) 0.039(3) 0.003(2) 0.000(2) 0.000(2) C17A 0.013(3) 0.015(3) 0.037(3) 0.001(2) 0.001(2) 0.000(2) C18A 0.020(3) 0.012(3) 0.038(3) 0.007(2) 0.000(2) 0.004(2) C19A 0.019(3) 0.013(3) 0.036(3) -0.003(2) -0.001(2) 0.006(2) C20A 0.025(3) 0.018(3) 0.035(3) -0.005(2) 0.000(2) -0.003(3) C21A 0.028(3) 0.015(3) 0.045(3) 0.003(3) -0.003(3) -0.003(3) C22A 0.025(3) 0.010(3) 0.044(3) 0.003(3) -0.004(3) -0.001(2) C23A 0.047(4) 0.028(4) 0.034(3) -0.003(3) 0.007(3) 0.012(3) C24A 0.100(8) 0.039(5) 0.037(4) 0.001(4) 0.015(4) 0.025(5) C50A 0.033(3) 0.030(4) 0.037(3) -0.001(3) 0.004(3) -0.001(3) N50A 0.034(3) 0.056(5) 0.059(4) -0.003(4) 0.000(3) 0.000(3) N60A 0.036(3) 0.024(3) 0.032(3) -0.004(2) -0.005(2) 0.001(2) C60A 0.033(3) 0.015(3) 0.034(3) -0.002(2) 0.000(2) -0.001(3) _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 Hg1B C60B 2.059(7) . ? Hg1B C50B 2.062(6) . ? Hg1B O2B 2.524(4) . ? Hg1B O3B 2.535(4) . ? Ni1B N1B 1.840(5) . ? Ni1B N2B 1.850(5) . ? Ni1B O3B 1.864(4) . ? Ni1B O2B 1.869(4) . ? N1B C9B 1.288(9) . ? N1B C10B 1.475(7) . ? N2B C16B 1.309(9) . ? N2B C15B 1.453(8) . ? O1B C3B 1.366(8) . ? O1B C2B 1.429(7) . ? O2B C4B 1.317(8) . ? O3B C18B 1.319(8) . ? O4B C19B 1.344(8) . ? O4B C23B 1.442(8) . ? C1B C2B 1.500(10) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C8B 1.371(10) . ? C3B C4B 1.430(10) . ? C4B C5B 1.401(10) . ? C5B C6B 1.421(9) . ? C5B C9B 1.428(10) . ? C6B C7B 1.371(11) . ? C6B H6BA 0.9500 . ? C7B C8B 1.412(10) . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B C15B 1.507(8) . ? C10B C11B 1.542(8) . ? C10B H10A 1.0000 . ? C11B C12B 1.529(11) . ? C11B H11A 0.9900 . ? C11B H11B 0.9900 . ? C12B C13B 1.506(12) . ? C12B H12A 0.9900 . ? C12B H12B 0.9900 . ? C13B C14B 1.520(10) . ? C13B H13A 0.9900 . ? C13B H13B 0.9900 . ? C14B C15B 1.532(9) . ? C14B H14A 0.9900 . ? C14B H14B 0.9900 . ? C15B H15A 1.0000 . ? C16B C17B 1.426(9) . ? C16B H16A 0.9500 . ? C17B C18B 1.396(9) . ? C17B C22B 1.414(9) . ? C18B C19B 1.443(9) . ? C19B C20B 1.384(8) . ? C20B C21B 1.396(9) . ? C20B H20A 0.9500 . ? C21B C22B 1.357(9) . ? C21B H21A 0.9500 . ? C22B H22A 0.9500 . ? C23B C24B 1.505(10) . ? C23B H23A 0.9900 . ? C23B H23B 0.9900 . ? C24B H24A 0.9800 . ? C24B H24B 0.9800 . ? C24B H24C 0.9800 . ? C50B N50B 1.121(9) . ? N60B C60B 1.126(9) . ? Hg1A C50A 2.047(7) . ? Hg1A C60A 2.066(7) . ? Hg1A O2A 2.531(4) . ? Hg1A O3A 2.541(4) . ? Ni1A N1A 1.846(5) . ? Ni1A N2A 1.853(5) . ? Ni1A O3A 1.859(4) . ? Ni1A O2A 1.861(4) . ? N1A C9A 1.283(9) . ? N1A C10A 1.480(7) . ? N2A C16A 1.310(8) . ? N2A C15A 1.465(8) . ? O1A C3A 1.371(8) . ? O1A C2A 1.452(7) . ? O2A C4A 1.322(8) . ? O3A C17A 1.321(8) . ? O4A C19A 1.350(8) . ? O4A C23A 1.437(7) . ? C1A C2A 1.493(10) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C8A 1.381(10) . ? C3A C4A 1.419(9) . ? C4A C5A 1.435(9) . ? C5A C6A 1.400(9) . ? C5A C9A 1.404(9) . ? C6A C7A 1.372(10) . ? C6A H6AA 0.9500 . ? C7A C8A 1.388(9) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A C15A 1.502(8) . ? C10A C11A 1.552(8) . ? C10A H10B 1.0000 . ? C11A C12A 1.520(11) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C12A C13A 1.504(12) . ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? C13A C14A 1.535(9) . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C14A C15A 1.524(9) . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C15A H15B 1.0000 . ? C16A C18A 1.411(9) . ? C16A H16B 0.9500 . ? C17A C18A 1.403(8) . ? C17A C19A 1.432(9) . ? C18A C22A 1.433(9) . ? C19A C20A 1.375(9) . ? C20A C21A 1.416(9) . ? C20A H20B 0.9500 . ? C21A C22A 1.332(10) . ? C21A H21B 0.9500 . ? C22A H22B 0.9500 . ? C23A C24A 1.505(10) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C50A N50A 1.142(10) . ? N60A C60A 1.128(9) . ? 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 C60B Hg1B C50B 160.4(2) . . ? C60B Hg1B O2B 105.3(2) . . ? C50B Hg1B O2B 91.4(2) . . ? C60B Hg1B O3B 96.1(2) . . ? C50B Hg1B O3B 101.2(2) . . ? O2B Hg1B O3B 60.11(14) . . ? N1B Ni1B N2B 84.8(2) . . ? N1B Ni1B O3B 174.1(2) . . ? N2B Ni1B O3B 95.5(2) . . ? N1B Ni1B O2B 94.8(2) . . ? N2B Ni1B O2B 173.8(2) . . ? O3B Ni1B O2B 85.48(19) . . ? C9B N1B C10B 120.2(5) . . ? C9B N1B Ni1B 126.8(5) . . ? C10B N1B Ni1B 112.9(4) . . ? C16B N2B C15B 120.5(6) . . ? C16B N2B Ni1B 125.5(5) . . ? C15B N2B Ni1B 113.7(4) . . ? C3B O1B C2B 117.0(5) . . ? C4B O2B Ni1B 126.8(4) . . ? C4B O2B Hg1B 125.9(4) . . ? Ni1B O2B Hg1B 107.29(19) . . ? C18B O3B Ni1B 126.6(4) . . ? C18B O3B Hg1B 126.3(4) . . ? Ni1B O3B Hg1B 107.04(19) . . ? C19B O4B C23B 116.9(5) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? O1B C2B C1B 109.2(6) . . ? O1B C2B H2BA 109.8 . . ? C1B C2B H2BA 109.8 . . ? O1B C2B H2BB 109.8 . . ? C1B C2B H2BB 109.8 . . ? H2BA C2B H2BB 108.3 . . ? O1B C3B C8B 123.4(7) . . ? O1B C3B C4B 115.4(6) . . ? C8B C3B C4B 121.2(7) . . ? O2B C4B C5B 123.6(6) . . ? O2B C4B C3B 119.0(6) . . ? C5B C4B C3B 117.5(6) . . ? C4B C5B C6B 120.7(7) . . ? C4B C5B C9B 122.3(6) . . ? C6B C5B C9B 116.8(6) . . ? C7B C6B C5B 120.3(7) . . ? C7B C6B H6BA 119.9 . . ? C5B C6B H6BA 119.9 . . ? C6B C7B C8B 119.8(7) . . ? C6B C7B H7BA 120.1 . . ? C8B C7B H7BA 120.1 . . ? C3B C8B C7B 120.5(7) . . ? C3B C8B H8BA 119.8 . . ? C7B C8B H8BA 119.8 . . ? N1B C9B C5B 125.2(6) . . ? N1B C9B H9BA 117.4 . . ? C5B C9B H9BA 117.4 . . ? N1B C10B C15B 104.2(5) . . ? N1B C10B C11B 118.7(5) . . ? C15B C10B C11B 111.9(5) . . ? N1B C10B H10A 107.1 . . ? C15B C10B H10A 107.1 . . ? C11B C10B H10A 107.1 . . ? C12B C11B C10B 109.0(6) . . ? C12B C11B H11A 109.9 . . ? C10B C11B H11A 109.9 . . ? C12B C11B H11B 109.9 . . ? C10B C11B H11B 109.9 . . ? H11A C11B H11B 108.3 . . ? C13B C12B C11B 112.4(6) . . ? C13B C12B H12A 109.1 . . ? C11B C12B H12A 109.1 . . ? C13B C12B H12B 109.1 . . ? C11B C12B H12B 109.1 . . ? H12A C12B H12B 107.9 . . ? C12B C13B C14B 111.7(6) . . ? C12B C13B H13A 109.3 . . ? C14B C13B H13A 109.3 . . ? C12B C13B H13B 109.3 . . ? C14B C13B H13B 109.3 . . ? H13A C13B H13B 107.9 . . ? C13B C14B C15B 110.5(7) . . ? C13B C14B H14A 109.5 . . ? C15B C14B H14A 109.5 . . ? C13B C14B H14B 109.5 . . ? C15B C14B H14B 109.5 . . ? H14A C14B H14B 108.1 . . ? N2B C15B C10B 104.2(5) . . ? N2B C15B C14B 118.1(6) . . ? C10B C15B C14B 112.1(5) . . ? N2B C15B H15A 107.3 . . ? C10B C15B H15A 107.3 . . ? C14B C15B H15A 107.3 . . ? N2B C16B C17B 125.8(6) . . ? N2B C16B H16A 117.1 . . ? C17B C16B H16A 117.1 . . ? C18B C17B C22B 122.2(6) . . ? C18B C17B C16B 122.1(6) . . ? C22B C17B C16B 115.6(6) . . ? O3B C18B C17B 124.3(6) . . ? O3B C18B C19B 118.9(6) . . ? C17B C18B C19B 116.8(6) . . ? O4B C19B C20B 124.1(6) . . ? O4B C19B C18B 116.1(5) . . ? C20B C19B C18B 119.8(6) . . ? C19B C20B C21B 121.3(6) . . ? C19B C20B H20A 119.4 . . ? C21B C20B H20A 119.4 . . ? C22B C21B C20B 120.4(6) . . ? C22B C21B H21A 119.8 . . ? C20B C21B H21A 119.8 . . ? C21B C22B C17B 119.6(6) . . ? C21B C22B H22A 120.2 . . ? C17B C22B H22A 120.2 . . ? O4B C23B C24B 107.7(6) . . ? O4B C23B H23A 110.2 . . ? C24B C23B H23A 110.2 . . ? O4B C23B H23B 110.2 . . ? C24B C23B H23B 110.2 . . ? H23A C23B H23B 108.5 . . ? C23B C24B H24A 109.5 . . ? C23B C24B H24B 109.5 . . ? H24A C24B H24B 109.5 . . ? C23B C24B H24C 109.5 . . ? H24A C24B H24C 109.5 . . ? H24B C24B H24C 109.5 . . ? N50B C50B Hg1B 175.1(6) . . ? N60B C60B Hg1B 177.6(6) . . ? C50A Hg1A C60A 162.6(3) . . ? C50A Hg1A O2A 95.7(2) . . ? C60A Hg1A O2A 98.7(2) . . ? C50A Hg1A O3A 96.8(2) . . ? C60A Hg1A O3A 98.8(2) . . ? O2A Hg1A O3A 59.91(14) . . ? N1A Ni1A N2A 85.2(2) . . ? N1A Ni1A O3A 178.4(2) . . ? N2A Ni1A O3A 94.7(2) . . ? N1A Ni1A O2A 94.4(2) . . ? N2A Ni1A O2A 178.3(2) . . ? O3A Ni1A O2A 85.8(2) . . ? C9A N1A C10A 121.1(5) . . ? C9A N1A Ni1A 126.3(5) . . ? C10A N1A Ni1A 112.6(4) . . ? C16A N2A C15A 120.9(6) . . ? C16A N2A Ni1A 125.4(5) . . ? C15A N2A Ni1A 113.7(4) . . ? C3A O1A C2A 116.6(5) . . ? C4A O2A Ni1A 127.4(4) . . ? C4A O2A Hg1A 124.3(4) . . ? Ni1A O2A Hg1A 107.24(19) . . ? C17A O3A Ni1A 127.1(4) . . ? C17A O3A Hg1A 125.5(4) . . ? Ni1A O3A Hg1A 106.9(2) . . ? C19A O4A C23A 116.5(5) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O1A C2A C1A 108.9(6) . . ? O1A C2A H2AA 109.9 . . ? C1A C2A H2AA 109.9 . . ? O1A C2A H2AB 109.9 . . ? C1A C2A H2AB 109.9 . . ? H2AA C2A H2AB 108.3 . . ? O1A C3A C8A 123.6(6) . . ? O1A C3A C4A 114.6(6) . . ? C8A C3A C4A 121.8(6) . . ? O2A C4A C3A 120.5(6) . . ? O2A C4A C5A 122.7(6) . . ? C3A C4A C5A 116.8(6) . . ? C6A C5A C9A 119.4(6) . . ? C6A C5A C4A 119.5(6) . . ? C9A C5A C4A 121.1(6) . . ? C7A C6A C5A 121.9(6) . . ? C7A C6A H6AA 119.1 . . ? C5A C6A H6AA 119.1 . . ? C6A C7A C8A 119.6(6) . . ? C6A C7A H7AA 120.2 . . ? C8A C7A H7AA 120.2 . . ? C3A C8A C7A 120.4(7) . . ? C3A C8A H8AA 119.8 . . ? C7A C8A H8AA 119.8 . . ? N1A C9A C5A 126.9(6) . . ? N1A C9A H9AA 116.6 . . ? C5A C9A H9AA 116.6 . . ? N1A C10A C15A 105.2(5) . . ? N1A C10A C11A 116.5(5) . . ? C15A C10A C11A 110.5(5) . . ? N1A C10A H10B 108.1 . . ? C15A C10A H10B 108.1 . . ? C11A C10A H10B 108.1 . . ? C12A C11A C10A 107.9(6) . . ? C12A C11A H11C 110.1 . . ? C10A C11A H11C 110.1 . . ? C12A C11A H11D 110.1 . . ? C10A C11A H11D 110.1 . . ? H11C C11A H11D 108.4 . . ? C13A C12A C11A 112.6(6) . . ? C13A C12A H12C 109.1 . . ? C11A C12A H12C 109.1 . . ? C13A C12A H12D 109.1 . . ? C11A C12A H12D 109.1 . . ? H12C C12A H12D 107.8 . . ? C12A C13A C14A 113.0(6) . . ? C12A C13A H13C 109.0 . . ? C14A C13A H13C 109.0 . . ? C12A C13A H13D 109.0 . . ? C14A C13A H13D 109.0 . . ? H13C C13A H13D 107.8 . . ? C15A C14A C13A 108.8(6) . . ? C15A C14A H14C 109.9 . . ? C13A C14A H14C 109.9 . . ? C15A C14A H14D 109.9 . . ? C13A C14A H14D 109.9 . . ? H14C C14A H14D 108.3 . . ? N2A C15A C10A 104.3(5) . . ? N2A C15A C14A 116.8(5) . . ? C10A C15A C14A 111.0(5) . . ? N2A C15A H15B 108.1 . . ? C10A C15A H15B 108.1 . . ? C14A C15A H15B 108.1 . . ? N2A C16A C18A 125.1(6) . . ? N2A C16A H16B 117.4 . . ? C18A C16A H16B 117.4 . . ? O3A C17A C18A 122.8(6) . . ? O3A C17A C19A 119.7(6) . . ? C18A C17A C19A 117.4(6) . . ? C17A C18A C16A 123.0(6) . . ? C17A C18A C22A 120.6(6) . . ? C16A C18A C22A 116.3(6) . . ? O4A C19A C20A 124.7(6) . . ? O4A C19A C17A 115.4(5) . . ? C20A C19A C17A 119.9(6) . . ? C19A C20A C21A 121.6(6) . . ? C19A C20A H20B 119.2 . . ? C21A C20A H20B 119.2 . . ? C22A C21A C20A 119.6(6) . . ? C22A C21A H21B 120.2 . . ? C20A C21A H21B 120.2 . . ? C21A C22A C18A 120.9(6) . . ? C21A C22A H22B 119.6 . . ? C18A C22A H22B 119.6 . . ? O4A C23A C24A 107.5(6) . . ? O4A C23A H23C 110.2 . . ? C24A C23A H23C 110.2 . . ? O4A C23A H23D 110.2 . . ? C24A C23A H23D 110.2 . . ? H23C C23A H23D 108.5 . . ? C23A C24A H24D 109.5 . . ? C23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N50A C50A Hg1A 176.0(8) . . ? N60A C60A Hg1A 176.1(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.499 _refine_diff_density_min -4.898 _refine_diff_density_rms 0.493 # Attachment 'GQ84.CIF' data_gq84 _database_code_depnum_ccdc_archive 'CCDC 755411' #TrackingRef 'GQ84.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H52 Cu2 Hg6 N12 O32' _chemical_formula_sum 'C48 H52 Cu2 Hg6 N12 O32' _chemical_formula_weight 2639.66 _chemical_absolute_configuration ad 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.070(3) _cell_length_b 9.5066(19) _cell_length_c 20.658(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.81(3) _cell_angle_gamma 90.00 _cell_volume 3133.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2436 _exptl_absorpt_coefficient_mu 15.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0431 _exptl_absorpt_correction_T_max 0.7481 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ;Due to the large atoms present, significant peaks of residual electron density remain in the difference map. The largest are Q1 3.46 and Q2 3.43 (0.810 and 0.809 from Hg1a) and Q3 3.42 (0.871 from Hg1b) These peaks are the result of fourier truncation surrounding the heavy Hg atoms and therefore remain un-assigned. ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62656 _diffrn_reflns_av_R_equivalents 0.1877 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.40 _reflns_number_total 11174 _reflns_number_gt 10773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+24.0140P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(12) _refine_ls_number_reflns 11174 _refine_ls_number_parameters 906 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1A Hg 1.58725(3) 1.09479(7) 0.85280(3) 0.03461(16) Uani 1 1 d . . . Hg2A Hg 1.85884(4) 0.90413(8) 0.64061(3) 0.04033(19) Uani 1 1 d . . . Hg3A Hg 1.15008(4) 1.28621(7) 0.83619(4) 0.03926(17) Uani 1 1 d . . . Cu1A Cu 1.46510(10) 0.9007(2) 0.72299(9) 0.0270(4) Uani 1 1 d . . . N1A N 1.4790(7) 0.7923(14) 0.6496(6) 0.027(2) Uani 1 1 d . . . N2A N 1.3456(7) 0.8830(13) 0.6741(7) 0.027(3) Uani 1 1 d . . . O1A O 1.7260(8) 1.0603(19) 0.8273(7) 0.055(4) Uani 1 1 d . . . O2A O 1.5822(6) 0.9370(13) 0.7648(5) 0.035(3) Uani 1 1 d . . . O3A O 1.4551(6) 0.9919(14) 0.8010(5) 0.032(2) Uani 1 1 d . . . O4A O 1.4751(7) 1.1598(16) 0.9060(5) 0.040(3) Uani 1 1 d . . . C1A C 1.8258(18) 1.255(3) 0.8449(14) 0.075(7) Uani 1 1 d U . . H1A1 H 1.8220 1.2478 0.7965 0.113 Uiso 1 1 calc R . . H1A2 H 1.8821 1.2868 0.8735 0.113 Uiso 1 1 calc R . . H1A3 H 1.7842 1.3228 0.8483 0.113 Uiso 1 1 calc R . . C2A C 1.8093(13) 1.114(3) 0.8695(12) 0.060(6) Uani 1 1 d . . . H2AA H 1.8527 1.0472 0.8676 0.072 Uiso 1 1 calc R . . H2AB H 1.8132 1.1221 0.9184 0.072 Uiso 1 1 calc R . . C3A C 1.7162(9) 0.997(2) 0.7658(9) 0.034(4) Uani 1 1 d . . . C4A C 1.6363(8) 0.9358(17) 0.7317(8) 0.029(3) Uani 1 1 d . . . C5A C 1.6212(8) 0.8721(17) 0.6693(8) 0.029(3) Uani 1 1 d . . . C6A C 1.6850(9) 0.8640(19) 0.6394(9) 0.030(3) Uani 1 1 d . . . H6AA H 1.6735 0.8217 0.5953 0.037 Uiso 1 1 calc R . . C7A C 1.7594(10) 0.9155(17) 0.6736(9) 0.031(3) Uani 1 1 d . . . C8A C 1.7770(9) 0.990(2) 0.7351(8) 0.035(4) Uani 1 1 d . . . H8AA H 1.8296 1.0351 0.7559 0.042 Uiso 1 1 calc R . . C9A C 1.5433(8) 0.7932(16) 0.6329(7) 0.026(3) Uani 1 1 d . . . H9AA H 1.5415 0.7388 0.5938 0.031 Uiso 1 1 calc R . . C10A C 1.4021(8) 0.7137(16) 0.6146(8) 0.027(3) Uani 1 1 d . . . H10A H 1.4001 0.6355 0.6464 0.033 Uiso 1 1 calc R . . C11A C 1.3960(11) 0.648(2) 0.5472(9) 0.038(4) Uani 1 1 d . . . H11A H 1.4430 0.5813 0.5544 0.046 Uiso 1 1 calc R . . H11B H 1.3990 0.7211 0.5141 0.046 Uiso 1 1 calc R . . C12A C 1.3109(11) 0.568(2) 0.5179(9) 0.050(5) Uani 1 1 d . . . H12A H 1.3040 0.5298 0.4716 0.060 Uiso 1 1 calc R . . H12B H 1.3115 0.4881 0.5487 0.060 Uiso 1 1 calc R . . C13A C 1.2362(8) 0.6645(17) 0.5118(8) 0.032(3) Uani 1 1 d . . . H13A H 1.2326 0.7398 0.4777 0.038 Uiso 1 1 calc R . . H13B H 1.1838 0.6091 0.4944 0.038 Uiso 1 1 calc R . . C14A C 1.2446(9) 0.731(2) 0.5811(9) 0.040(4) Uani 1 1 d . . . H14A H 1.2437 0.6568 0.6146 0.048 Uiso 1 1 calc R . . H14B H 1.1972 0.7958 0.5752 0.048 Uiso 1 1 calc R . . C15A C 1.3286(8) 0.8123(15) 0.6084(6) 0.024(3) Uani 1 1 d . . . H15A H 1.3269 0.8857 0.5733 0.029 Uiso 1 1 calc R . . C16A C 1.2893(8) 0.9396(16) 0.6925(7) 0.026(3) Uani 1 1 d . . . H16A H 1.2326 0.9249 0.6636 0.031 Uiso 1 1 calc R . . C17A C 1.3044(9) 1.0239(15) 0.7533(8) 0.028(3) Uani 1 1 d . . . C18A C 1.3863(8) 1.0482(16) 0.8043(7) 0.025(3) Uani 1 1 d . . . C19A C 1.3946(9) 1.1418(18) 0.8586(8) 0.030(3) Uani 1 1 d . . . C20A C 1.3220(10) 1.2063(17) 0.8648(8) 0.032(3) Uani 1 1 d . . . H20A H 1.3278 1.2676 0.9026 0.038 Uiso 1 1 calc R . . C21A C 1.2470(9) 1.1816(19) 0.8188(9) 0.035(4) Uani 1 1 d . . . C22A C 1.2356(8) 1.094(2) 0.7651(8) 0.029(3) Uani 1 1 d U . . H22A H 1.1802 1.0783 0.7337 0.035 Uiso 1 1 calc R . . C23A C 1.4901(12) 1.243(2) 0.9620(9) 0.046(4) Uani 1 1 d . . . H23A H 1.5430 1.2133 0.9985 0.055 Uiso 1 1 calc R . . H23B H 1.4443 1.2314 0.9804 0.055 Uiso 1 1 calc R . . C24A C 1.4967(16) 1.395(2) 0.9457(13) 0.064(6) Uani 1 1 d . . . H24A H 1.5115 1.4032 0.9041 0.096 Uiso 1 1 calc R . . H24B H 1.5401 1.4406 0.9847 0.096 Uiso 1 1 calc R . . H24C H 1.4427 1.4418 0.9375 0.096 Uiso 1 1 calc R . . N10A N 1.5543(10) 1.3579(19) 0.7722(10) 0.054(4) Uani 1 1 d U . . O10A O 1.5054(12) 1.264(2) 0.7720(8) 0.086(7) Uani 1 1 d . . . O11A O 1.6183(13) 1.368(3) 0.8270(11) 0.094(6) Uani 1 1 d U . . O12A O 1.5345(11) 1.4476(18) 0.7263(12) 0.080(6) Uani 1 1 d . . . N20A N 1.6928(9) 1.003(2) 0.9870(9) 0.050(4) Uani 1 1 d . . . O20A O 1.6717(10) 1.1159(19) 0.9587(7) 0.060(4) Uani 1 1 d . . . O21A O 1.661(2) 0.897(2) 0.9583(13) 0.131(10) Uani 1 1 d U . . O22A O 1.7355(10) 0.997(2) 1.0504(8) 0.069(5) Uani 1 1 d . . . N30A N 2.0290(9) 0.896(2) 0.6501(8) 0.051(4) Uani 1 1 d . . . O30A O 1.9536(8) 0.885(3) 0.6024(7) 0.090(7) Uani 1 1 d . . . O31A O 2.0301(8) 0.916(2) 0.7082(8) 0.061(4) Uani 1 1 d . . . O32A O 2.0900(8) 0.878(3) 0.6336(9) 0.076(6) Uani 1 1 d . . . N40A N 1.0712(11) 1.3818(16) 0.9289(8) 0.043(4) Uani 1 1 d . . . O40A O 1.0669(8) 1.4147(16) 0.8671(8) 0.050(3) Uani 1 1 d . . . O41A O 1.1058(13) 1.2703(19) 0.9524(9) 0.076(5) Uani 1 1 d . . . O42A O 1.0337(12) 1.453(2) 0.9556(11) 0.081(6) Uani 1 1 d . . . Hg1B Hg 0.92376(4) 1.48506(8) 0.64470(3) 0.03788(18) Uani 1 1 d . . . Hg2B Hg 1.36027(4) 1.29190(8) 0.66588(4) 0.04351(19) Uani 1 1 d . . . Hg3B Hg 0.64753(3) 1.67721(8) 0.85604(3) 0.03654(17) Uani 1 1 d . . . Cu1B Cu 1.04396(10) 1.6754(2) 0.77626(9) 0.0298(4) Uani 1 1 d . . . N1B N 1.1608(7) 1.7225(14) 0.8139(6) 0.026(3) Uani 1 1 d . . . N2B N 1.0349(7) 1.7457(13) 0.8594(6) 0.027(3) Uani 1 1 d . . . O1B O 1.0362(8) 1.4276(15) 0.5929(6) 0.046(3) Uani 1 1 d . . . O2B O 1.0535(6) 1.5911(14) 0.6958(5) 0.033(2) Uani 1 1 d . . . O3B O 0.9290(6) 1.6265(14) 0.7354(6) 0.039(3) Uani 1 1 d . . . O4B O 0.7814(7) 1.5221(17) 0.6654(6) 0.046(3) Uani 1 1 d . . . C1B C 1.0130(17) 1.193(3) 0.5541(14) 0.076(7) Uani 1 1 d U . . H1B1 H 1.0498 1.1790 0.6024 0.114 Uiso 1 1 calc R . . H1B2 H 1.0295 1.1282 0.5243 0.114 Uiso 1 1 calc R . . H1B3 H 0.9548 1.1738 0.5496 0.114 Uiso 1 1 calc R . . C2B C 1.0197(14) 1.328(3) 0.5348(11) 0.059(6) Uani 1 1 d . . . H2BA H 0.9670 1.3550 0.4973 0.071 Uiso 1 1 calc R . . H2BB H 1.0657 1.3338 0.5163 0.071 Uiso 1 1 calc R . . C3B C 1.1174(11) 1.4397(17) 0.6382(9) 0.035(4) Uani 1 1 d . . . C4B C 1.1257(8) 1.5347(19) 0.6936(8) 0.031(3) Uani 1 1 d . . . C5B C 1.2054(9) 1.5641(17) 0.7412(8) 0.030(3) Uani 1 1 d . . . C6B C 1.2782(10) 1.5042(16) 0.7358(8) 0.032(3) Uani 1 1 d . . . H6BA H 1.3326 1.5273 0.7673 0.039 Uiso 1 1 calc R . . C7B C 1.2658(9) 1.4065(17) 0.6803(8) 0.030(3) Uani 1 1 d U . . C8B C 1.1854(12) 1.375(2) 0.6330(10) 0.048(5) Uani 1 1 d . . . H8BA H 1.1789 1.3085 0.5972 0.057 Uiso 1 1 calc R . . C9B C 1.2197(9) 1.6658(18) 0.7972(8) 0.031(3) Uani 1 1 d . . . H9BA H 1.2759 1.6919 0.8230 0.037 Uiso 1 1 calc R . . C10B C 1.1737(8) 1.8335(13) 0.8685(7) 0.022(3) Uani 1 1 d . . . H10B H 1.1502 1.9236 0.8445 0.027 Uiso 1 1 calc R . . C11B C 1.2624(9) 1.861(2) 0.9149(8) 0.037(4) Uani 1 1 d . . . H11C H 1.2956 1.8939 0.8871 0.045 Uiso 1 1 calc R . . H11D H 1.2881 1.7733 0.9390 0.045 Uiso 1 1 calc R . . C12B C 1.2622(10) 1.9737(19) 0.9680(9) 0.040(4) Uani 1 1 d . . . H12C H 1.3202 1.9887 1.0006 0.048 Uiso 1 1 calc R . . H12D H 1.2417 2.0637 0.9437 0.048 Uiso 1 1 calc R . . C13B C 1.2071(9) 1.9317(18) 1.0081(9) 0.037(4) Uani 1 1 d . . . H13C H 1.2309 1.8469 1.0360 0.045 Uiso 1 1 calc R . . H13D H 1.2068 2.0084 1.0404 0.045 Uiso 1 1 calc R . . C14B C 1.1211(9) 1.9022(19) 0.9626(7) 0.032(3) Uani 1 1 d . . . H14C H 1.0955 1.9892 0.9377 0.038 Uiso 1 1 calc R . . H14D H 1.0878 1.8721 0.9909 0.038 Uiso 1 1 calc R . . C15B C 1.1185(8) 1.7871(16) 0.9102(6) 0.025(3) Uani 1 1 d . . . H15B H 1.1446 1.7009 0.9369 0.030 Uiso 1 1 calc R . . C16B C 0.9697(8) 1.7444(13) 0.8760(6) 0.020(3) Uani 1 1 d . . . H16B H 0.9747 1.7804 0.9202 0.024 Uiso 1 1 calc R . . C17B C 0.8891(8) 1.6920(17) 0.8322(7) 0.028(3) Uani 1 1 d . . . C18B C 0.8734(8) 1.6326(16) 0.7670(7) 0.026(3) Uani 1 1 d . . . C19B C 0.7909(8) 1.5792(19) 0.7319(8) 0.030(3) Uani 1 1 d . . . C20B C 0.7291(9) 1.5892(17) 0.7599(8) 0.031(3) Uani 1 1 d . . . H20B H 0.6746 1.5546 0.7347 0.037 Uiso 1 1 calc R . . C21B C 0.7450(9) 1.6471(17) 0.8223(8) 0.033(4) Uani 1 1 d . . . C22B C 0.8239(10) 1.7025(19) 0.8590(8) 0.031(3) Uani 1 1 d . . . H22B H 0.8339 1.7475 0.9023 0.037 Uiso 1 1 calc R . . C23B C 0.6984(12) 1.466(2) 0.6241(10) 0.048(4) Uani 1 1 d . . . H23C H 0.6547 1.5306 0.6277 0.057 Uiso 1 1 calc R . . H23D H 0.6932 1.4617 0.5749 0.057 Uiso 1 1 calc R . . C24B C 0.6843(14) 1.329(3) 0.6460(11) 0.062(6) Uani 1 1 d . . . H24D H 0.7339 1.2704 0.6531 0.093 Uiso 1 1 calc R . . H24E H 0.6356 1.2865 0.6105 0.093 Uiso 1 1 calc R . . H24F H 0.6738 1.3365 0.6895 0.093 Uiso 1 1 calc R . . N10B N 0.9571(9) 1.220(2) 0.7246(10) 0.051(4) Uani 1 1 d . . . O10B O 1.0056(11) 1.320(2) 0.7261(9) 0.085(7) Uani 1 1 d U . . O11B O 0.8910(9) 1.217(2) 0.6781(11) 0.087(6) Uani 1 1 d . . . O12B O 0.9761(10) 1.1413(18) 0.7730(10) 0.074(5) Uani 1 1 d . . . N20B N 0.8123(9) 1.586(2) 0.5123(7) 0.046(4) Uani 1 1 d . . . O20B O 0.8409(9) 1.4727(18) 0.5354(7) 0.057(4) Uani 1 1 d . . . O21B O 0.837(2) 1.689(3) 0.5471(10) 0.138(12) Uani 1 1 d . . . O22B O 0.7714(9) 1.5944(19) 0.4493(7) 0.058(4) Uani 1 1 d . . . N30B N 1.4382(12) 1.165(2) 0.5776(11) 0.063(5) Uani 1 1 d . . . O30B O 1.4365(8) 1.1428(15) 0.6382(7) 0.047(3) Uani 1 1 d . . . O31B O 1.4060(17) 1.270(2) 0.5495(11) 0.101(8) Uani 1 1 d . . . O32B O 1.4746(15) 1.083(2) 0.5532(11) 0.097(7) Uani 1 1 d . . . N40B N 0.4776(9) 1.703(2) 0.8517(9) 0.058(5) Uani 1 1 d . . . O40B O 0.5529(7) 1.709(3) 0.8967(7) 0.075(6) Uani 1 1 d . . . O41B O 0.4210(8) 1.718(2) 0.8707(9) 0.070(5) Uani 1 1 d . . . O42B O 0.4733(8) 1.6681(18) 0.7910(6) 0.046(3) 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 Hg1A 0.0238(3) 0.0424(4) 0.0338(3) -0.0084(3) 0.0055(2) -0.0039(3) Hg2A 0.0254(3) 0.0554(5) 0.0414(4) -0.0044(3) 0.0134(2) -0.0016(3) Hg3A 0.0373(3) 0.0353(4) 0.0473(4) -0.0007(3) 0.0177(3) 0.0064(3) Cu1A 0.0182(7) 0.0296(10) 0.0310(9) -0.0066(8) 0.0058(7) -0.0014(7) N1A 0.020(5) 0.030(6) 0.032(6) -0.003(5) 0.009(4) 0.007(5) N2A 0.023(5) 0.012(5) 0.041(7) 0.003(5) 0.006(5) -0.001(4) O1A 0.034(6) 0.083(12) 0.049(7) -0.033(8) 0.017(5) -0.013(7) O2A 0.027(5) 0.045(7) 0.032(5) -0.002(5) 0.009(4) 0.002(5) O3A 0.026(5) 0.043(7) 0.029(5) -0.020(5) 0.012(4) -0.008(5) O4A 0.026(5) 0.060(8) 0.030(5) -0.011(5) 0.006(4) -0.005(5) C1A 0.077(10) 0.069(11) 0.076(10) -0.003(8) 0.022(8) 0.008(8) C2A 0.042(10) 0.071(16) 0.063(12) -0.029(12) 0.012(9) -0.017(11) C3A 0.018(6) 0.036(10) 0.044(8) -0.005(7) 0.007(6) 0.000(7) C4A 0.016(6) 0.034(8) 0.034(7) 0.000(6) 0.007(5) 0.002(6) C5A 0.021(6) 0.029(8) 0.036(7) -0.001(6) 0.011(6) 0.014(6) C6A 0.023(7) 0.037(9) 0.033(8) -0.001(6) 0.012(6) -0.005(6) C7A 0.034(7) 0.019(7) 0.044(8) -0.011(6) 0.017(7) -0.003(6) C8A 0.018(6) 0.051(11) 0.036(8) -0.001(8) 0.010(6) -0.002(7) C9A 0.017(6) 0.026(7) 0.032(7) 0.003(6) 0.005(5) 0.005(6) C10A 0.016(6) 0.026(7) 0.042(8) -0.008(6) 0.013(5) 0.001(6) C11A 0.039(8) 0.040(9) 0.041(9) -0.001(7) 0.021(7) 0.001(7) C12A 0.052(10) 0.043(10) 0.048(9) -0.015(8) 0.010(8) 0.020(9) C13A 0.017(6) 0.032(8) 0.038(8) -0.015(6) 0.000(5) -0.002(6) C14A 0.019(7) 0.049(10) 0.042(9) -0.018(8) 0.001(6) -0.010(7) C15A 0.022(6) 0.026(7) 0.022(6) 0.002(5) 0.005(5) 0.011(6) C16A 0.023(6) 0.031(8) 0.020(6) -0.013(5) 0.001(5) -0.002(6) C17A 0.025(6) 0.018(7) 0.050(9) 0.016(6) 0.023(6) 0.009(5) C18A 0.014(6) 0.031(8) 0.032(7) -0.012(6) 0.009(5) -0.010(5) C19A 0.029(7) 0.039(9) 0.029(7) -0.007(6) 0.019(6) 0.002(6) C20A 0.045(8) 0.025(8) 0.035(7) -0.008(6) 0.025(7) 0.008(7) C21A 0.028(7) 0.032(8) 0.054(9) 0.011(7) 0.024(7) 0.000(7) C22A 0.010(5) 0.041(7) 0.037(6) 0.005(6) 0.008(4) 0.000(5) C23A 0.041(9) 0.042(11) 0.044(9) 0.003(8) 0.002(8) 0.007(8) C24A 0.083(15) 0.011(8) 0.090(15) -0.008(9) 0.019(13) -0.009(8) N10A 0.043(8) 0.042(10) 0.080(11) 0.013(9) 0.028(7) 0.003(8) O10A 0.097(13) 0.073(12) 0.054(9) 0.011(8) -0.013(8) -0.053(11) O11A 0.093(6) 0.094(6) 0.094(6) 0.0001(10) 0.033(2) 0.0000(10) O12A 0.071(10) 0.040(10) 0.149(17) 0.018(10) 0.064(11) 0.009(8) N20A 0.030(7) 0.049(11) 0.063(10) -0.024(9) 0.008(7) -0.022(8) O20A 0.068(9) 0.055(10) 0.045(7) -0.007(7) 0.006(7) -0.004(8) O21A 0.21(2) 0.045(11) 0.112(15) -0.037(12) 0.020(15) -0.052(13) O22A 0.060(8) 0.081(12) 0.050(8) 0.015(9) -0.002(7) 0.018(9) N30A 0.036(7) 0.063(11) 0.051(9) -0.013(9) 0.012(7) -0.008(8) O30A 0.025(6) 0.20(2) 0.047(7) -0.004(12) 0.014(6) 0.002(11) O31A 0.031(6) 0.078(12) 0.066(10) -0.002(9) 0.007(6) 0.016(7) O32A 0.024(6) 0.127(17) 0.082(11) -0.009(11) 0.025(7) 0.009(9) N40A 0.068(10) 0.024(7) 0.057(9) 0.007(6) 0.045(8) 0.011(7) O40A 0.046(7) 0.045(8) 0.072(9) -0.011(7) 0.037(7) 0.006(6) O41A 0.112(14) 0.056(10) 0.081(10) 0.032(8) 0.061(10) 0.046(10) O42A 0.097(12) 0.064(11) 0.120(14) 0.022(10) 0.085(12) 0.022(10) Hg1B 0.0270(3) 0.0490(4) 0.0336(3) -0.0081(3) 0.0057(2) -0.0077(3) Hg2B 0.0439(4) 0.0354(4) 0.0547(4) 0.0040(3) 0.0219(3) 0.0055(3) Hg3B 0.0222(3) 0.0481(4) 0.0392(3) 0.0003(3) 0.0108(2) 0.0013(3) Cu1B 0.0174(7) 0.0385(11) 0.0320(9) -0.0071(9) 0.0068(7) -0.0047(8) N1B 0.024(5) 0.032(7) 0.021(5) -0.005(5) 0.007(4) -0.010(5) N2B 0.021(6) 0.031(7) 0.025(6) -0.004(5) 0.003(5) -0.007(5) O1B 0.045(7) 0.049(8) 0.045(7) -0.016(6) 0.017(5) -0.019(6) O2B 0.028(5) 0.036(6) 0.034(5) -0.014(5) 0.010(4) -0.005(5) O3B 0.024(5) 0.060(8) 0.035(5) -0.027(5) 0.012(4) -0.009(5) O4B 0.028(5) 0.071(10) 0.030(5) -0.019(6) -0.002(4) -0.013(6) C1B 0.075(10) 0.066(10) 0.080(10) -0.005(8) 0.020(8) 0.000(8) C2B 0.057(12) 0.067(16) 0.053(11) -0.032(11) 0.019(9) -0.010(10) C3B 0.044(9) 0.020(8) 0.048(9) -0.007(6) 0.024(7) -0.008(6) C4B 0.017(6) 0.044(9) 0.038(8) -0.001(7) 0.016(6) 0.000(6) C5B 0.025(7) 0.035(9) 0.035(7) -0.011(6) 0.017(6) 0.003(6) C6B 0.037(8) 0.021(7) 0.049(8) 0.005(6) 0.028(7) 0.008(6) C7B 0.028(6) 0.023(6) 0.047(7) 0.000(6) 0.025(5) 0.009(5) C8B 0.061(11) 0.037(10) 0.050(10) -0.010(8) 0.025(9) -0.022(9) C9B 0.026(7) 0.027(8) 0.044(8) 0.008(6) 0.017(6) 0.005(6) C10B 0.022(6) 0.015(6) 0.029(6) -0.010(5) 0.008(5) 0.003(5) C11B 0.019(6) 0.066(12) 0.026(7) -0.006(7) 0.007(6) -0.004(7) C12B 0.039(8) 0.030(8) 0.046(9) -0.002(7) 0.008(7) -0.013(7) C13B 0.028(7) 0.039(8) 0.047(8) -0.020(7) 0.015(7) -0.009(7) C14B 0.029(7) 0.038(9) 0.020(6) -0.014(6) -0.001(5) -0.001(7) C15B 0.025(6) 0.035(7) 0.018(5) -0.004(5) 0.009(5) 0.003(6) C16B 0.030(7) 0.020(6) 0.007(5) 0.000(4) 0.003(5) -0.002(5) C17B 0.017(6) 0.028(8) 0.035(7) 0.006(6) 0.006(5) -0.002(6) C18B 0.022(6) 0.031(8) 0.024(6) -0.006(6) 0.008(5) -0.002(6) C19B 0.018(6) 0.030(8) 0.040(8) -0.007(7) 0.009(6) -0.010(6) C20B 0.026(7) 0.019(7) 0.041(8) -0.002(7) 0.005(6) -0.009(6) C21B 0.023(7) 0.026(8) 0.040(8) 0.020(7) -0.001(6) 0.002(6) C22B 0.029(7) 0.035(9) 0.031(8) -0.007(7) 0.014(6) 0.006(7) C23B 0.041(9) 0.053(12) 0.047(10) -0.004(9) 0.014(8) -0.003(9) C24B 0.051(11) 0.081(17) 0.051(11) -0.014(11) 0.015(9) -0.018(11) N10B 0.028(7) 0.045(10) 0.076(11) -0.017(9) 0.016(7) -0.005(7) O10B 0.065(9) 0.112(15) 0.061(9) 0.029(10) 0.003(7) -0.048(10) O11B 0.032(7) 0.093(14) 0.111(14) 0.021(11) -0.004(8) 0.000(8) O12B 0.059(9) 0.048(10) 0.113(14) 0.039(10) 0.029(9) 0.009(7) N20B 0.037(7) 0.058(11) 0.034(7) 0.004(8) 0.000(6) -0.015(8) O20B 0.064(8) 0.055(9) 0.035(6) -0.023(6) -0.003(6) 0.025(8) O21B 0.27(4) 0.059(13) 0.061(11) 0.004(11) 0.025(16) 0.037(18) O22B 0.053(8) 0.058(9) 0.053(8) 0.015(8) 0.008(6) -0.015(8) N30B 0.066(11) 0.055(12) 0.081(12) -0.002(10) 0.040(10) 0.015(10) O30B 0.053(7) 0.040(7) 0.044(7) -0.002(5) 0.014(6) 0.007(6) O31B 0.17(2) 0.054(11) 0.113(15) 0.044(10) 0.097(15) 0.064(13) O32B 0.148(18) 0.065(11) 0.118(14) 0.025(11) 0.096(14) 0.068(12) N40B 0.028(7) 0.086(14) 0.054(9) 0.032(10) 0.009(7) 0.000(8) O40B 0.022(6) 0.158(19) 0.046(7) 0.002(10) 0.013(5) 0.024(9) O41B 0.029(6) 0.099(14) 0.085(11) 0.037(10) 0.024(7) 0.018(8) O42B 0.049(7) 0.055(9) 0.032(6) 0.001(6) 0.011(5) 0.002(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 Hg1A O20A 2.160(14) . ? Hg1A O2A 2.335(12) . ? Hg1A O3A 2.341(10) . ? Hg1A O10A 2.379(19) . ? Hg1A O4A 2.597(11) . ? Hg1A O1A 2.623(12) . ? Hg2A C7A 2.044(16) . ? Hg2A O30A 2.045(13) . ? Hg3A C21A 2.068(16) . ? Hg3A O40A 2.136(12) . ? Cu1A O3A 1.890(10) . ? Cu1A O2A 1.906(11) . ? Cu1A N1A 1.917(12) . ? Cu1A N2A 1.935(12) . ? N1A C9A 1.263(18) . ? N1A C10A 1.458(17) . ? N2A C16A 1.273(19) . ? N2A C15A 1.449(18) . ? O1A C3A 1.36(2) . ? O1A C2A 1.47(2) . ? O2A C4A 1.330(18) . ? O3A C18A 1.314(17) . ? O4A C23A 1.35(2) . ? O4A C19A 1.386(18) . ? C1A C2A 1.49(4) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C8A 1.40(2) . ? C3A C4A 1.42(2) . ? C4A C5A 1.36(2) . ? C5A C6A 1.43(2) . ? C5A C9A 1.48(2) . ? C6A C7A 1.31(2) . ? C6A H6AA 0.9500 . ? C7A C8A 1.39(2) . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A C11A 1.50(2) . ? C10A C15A 1.534(17) . ? C10A H10A 1.0000 . ? C11A C12A 1.56(3) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.54(2) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.52(2) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.55(2) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 1.0000 . ? C16A C17A 1.43(2) . ? C16A H16A 0.9500 . ? C17A C18A 1.438(19) . ? C17A C22A 1.45(2) . ? C18A C19A 1.40(2) . ? C19A C20A 1.43(2) . ? C20A C21A 1.32(2) . ? C20A H20A 0.9500 . ? C21A C22A 1.34(3) . ? C22A H22A 0.9500 . ? C23A C24A 1.50(3) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? N10A O10A 1.22(2) . ? N10A O12A 1.23(3) . ? N10A O11A 1.27(3) . ? N20A O21A 1.19(2) . ? N20A O20A 1.22(3) . ? N20A O22A 1.25(2) . ? N30A O31A 1.21(2) . ? N30A O32A 1.22(2) . ? N30A O30A 1.319(19) . ? N40A O42A 1.20(2) . ? N40A O41A 1.23(2) . ? N40A O40A 1.29(2) . ? Hg1B O20B 2.201(12) . ? Hg1B O3B 2.282(10) . ? Hg1B O2B 2.318(10) . ? Hg1B O10B 2.36(2) . ? Hg1B O1B 2.567(13) . ? Hg1B O4B 2.636(12) . ? Hg2B C7B 2.054(14) . ? Hg2B O30B 2.135(13) . ? Hg3B C21B 2.040(17) . ? Hg3B O40B 2.092(12) . ? Cu1B O3B 1.899(10) . ? Cu1B N2B 1.900(12) . ? Cu1B O2B 1.904(11) . ? Cu1B N1B 1.918(12) . ? N1B C9B 1.29(2) . ? N1B C10B 1.503(16) . ? N2B C16B 1.276(18) . ? N2B C15B 1.493(17) . ? O1B C3B 1.37(2) . ? O1B C2B 1.47(2) . ? O2B C4B 1.360(18) . ? O3B C18B 1.330(17) . ? O4B C19B 1.431(19) . ? O4B C23B 1.47(2) . ? C1B C2B 1.36(4) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C8B 1.35(3) . ? C3B C4B 1.42(2) . ? C4B C5B 1.40(2) . ? C5B C6B 1.41(2) . ? C5B C9B 1.46(2) . ? C6B C7B 1.43(2) . ? C6B H6BA 0.9500 . ? C7B C8B 1.41(2) . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B C11B 1.499(18) . ? C10B C15B 1.549(19) . ? C10B H10B 1.0000 . ? C11B C12B 1.53(2) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.51(2) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.462(19) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.530(19) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15B 1.0000 . ? C16B C17B 1.441(18) . ? C16B H16B 0.9500 . ? C17B C18B 1.40(2) . ? C17B C22B 1.41(2) . ? C18B C19B 1.429(19) . ? C19B C20B 1.37(2) . ? C20B C21B 1.34(2) . ? C20B H20B 0.9500 . ? C21B C22B 1.39(2) . ? C22B H22B 0.9500 . ? C23B C24B 1.42(3) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? N10B O11B 1.19(2) . ? N10B O12B 1.20(2) . ? N10B O10B 1.25(2) . ? N20B O21B 1.20(3) . ? N20B O20B 1.21(2) . ? N20B O22B 1.241(19) . ? N30B O31B 1.18(3) . ? N30B O32B 1.21(2) . ? N30B O30B 1.28(2) . ? N40B O41B 1.17(2) . ? N40B O42B 1.27(2) . ? N40B O40B 1.293(19) . ? 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 O20A Hg1A O2A 132.5(5) . . ? O20A Hg1A O3A 133.7(5) . . ? O2A Hg1A O3A 67.2(4) . . ? O20A Hg1A O10A 131.5(6) . . ? O2A Hg1A O10A 92.1(6) . . ? O3A Hg1A O10A 74.4(5) . . ? O20A Hg1A O4A 82.9(5) . . ? O2A Hg1A O4A 130.8(4) . . ? O3A Hg1A O4A 63.7(4) . . ? O10A Hg1A O4A 78.4(6) . . ? O20A Hg1A O1A 83.7(5) . . ? O2A Hg1A O1A 63.2(4) . . ? O3A Hg1A O1A 130.4(4) . . ? O10A Hg1A O1A 106.9(7) . . ? O4A Hg1A O1A 165.5(4) . . ? C7A Hg2A O30A 176.2(8) . . ? C21A Hg3A O40A 170.0(6) . . ? O3A Cu1A O2A 85.9(5) . . ? O3A Cu1A N1A 174.4(6) . . ? O2A Cu1A N1A 93.0(5) . . ? O3A Cu1A N2A 95.0(5) . . ? O2A Cu1A N2A 173.4(5) . . ? N1A Cu1A N2A 86.8(5) . . ? C9A N1A C10A 125.8(12) . . ? C9A N1A Cu1A 125.2(11) . . ? C10A N1A Cu1A 109.0(8) . . ? C16A N2A C15A 123.7(11) . . ? C16A N2A Cu1A 125.1(10) . . ? C15A N2A Cu1A 110.7(9) . . ? C3A O1A C2A 118.7(14) . . ? C3A O1A Hg1A 115.0(9) . . ? C2A O1A Hg1A 126.1(11) . . ? C4A O2A Cu1A 125.0(9) . . ? C4A O2A Hg1A 124.4(10) . . ? Cu1A O2A Hg1A 102.2(5) . . ? C18A O3A Cu1A 125.8(9) . . ? C18A O3A Hg1A 122.7(9) . . ? Cu1A O3A Hg1A 102.5(4) . . ? C23A O4A C19A 121.0(14) . . ? C23A O4A Hg1A 124.0(11) . . ? C19A O4A Hg1A 111.6(8) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O1A C2A C1A 112(2) . . ? O1A C2A H2AA 109.3 . . ? C1A C2A H2AA 109.3 . . ? O1A C2A H2AB 109.3 . . ? C1A C2A H2AB 109.3 . . ? H2AA C2A H2AB 107.9 . . ? O1A C3A C8A 125.5(15) . . ? O1A C3A C4A 115.0(14) . . ? C8A C3A C4A 119.5(16) . . ? O2A C4A C5A 123.9(13) . . ? O2A C4A C3A 117.5(14) . . ? C5A C4A C3A 118.5(14) . . ? C4A C5A C6A 121.0(14) . . ? C4A C5A C9A 122.6(13) . . ? C6A C5A C9A 116.0(13) . . ? C7A C6A C5A 119.2(15) . . ? C7A C6A H6AA 120.4 . . ? C5A C6A H6AA 120.4 . . ? C6A C7A C8A 122.5(15) . . ? C6A C7A Hg2A 124.1(12) . . ? C8A C7A Hg2A 113.3(11) . . ? C7A C8A C3A 119.0(15) . . ? C7A C8A H8AA 120.5 . . ? C3A C8A H8AA 120.5 . . ? N1A C9A C5A 125.2(13) . . ? N1A C9A H9AA 117.4 . . ? C5A C9A H9AA 117.4 . . ? N1A C10A C11A 115.3(12) . . ? N1A C10A C15A 107.1(11) . . ? C11A C10A C15A 113.2(12) . . ? N1A C10A H10A 106.9 . . ? C11A C10A H10A 106.9 . . ? C15A C10A H10A 106.9 . . ? C10A C11A C12A 108.2(13) . . ? C10A C11A H11A 110.1 . . ? C12A C11A H11A 110.1 . . ? C10A C11A H11B 110.1 . . ? C12A C11A H11B 110.1 . . ? H11A C11A H11B 108.4 . . ? C13A C12A C11A 112.0(14) . . ? C13A C12A H12A 109.2 . . ? C11A C12A H12A 109.2 . . ? C13A C12A H12B 109.2 . . ? C11A C12A H12B 109.2 . . ? H12A C12A H12B 107.9 . . ? C14A C13A C12A 111.7(13) . . ? C14A C13A H13A 109.3 . . ? C12A C13A H13A 109.3 . . ? C14A C13A H13B 109.3 . . ? C12A C13A H13B 109.3 . . ? H13A C13A H13B 107.9 . . ? C13A C14A C15A 108.3(13) . . ? C13A C14A H14A 110.0 . . ? C15A C14A H14A 110.0 . . ? C13A C14A H14B 110.0 . . ? C15A C14A H14B 110.0 . . ? H14A C14A H14B 108.4 . . ? N2A C15A C10A 108.6(10) . . ? N2A C15A C14A 115.1(12) . . ? C10A C15A C14A 110.4(12) . . ? N2A C15A H15A 107.5 . . ? C10A C15A H15A 107.5 . . ? C14A C15A H15A 107.5 . . ? N2A C16A C17A 125.3(12) . . ? N2A C16A H16A 117.3 . . ? C17A C16A H16A 117.3 . . ? C16A C17A C18A 123.8(13) . . ? C16A C17A C22A 120.1(13) . . ? C18A C17A C22A 116.0(14) . . ? O3A C18A C19A 117.6(12) . . ? O3A C18A C17A 123.3(13) . . ? C19A C18A C17A 119.0(13) . . ? O4A C19A C18A 115.9(13) . . ? O4A C19A C20A 124.0(14) . . ? C18A C19A C20A 120.0(14) . . ? C21A C20A C19A 120.7(14) . . ? C21A C20A H20A 119.6 . . ? C19A C20A H20A 119.6 . . ? C20A C21A C22A 121.7(15) . . ? C20A C21A Hg3A 114.9(13) . . ? C22A C21A Hg3A 123.4(11) . . ? C21A C22A C17A 122.5(13) . . ? C21A C22A H22A 118.7 . . ? C17A C22A H22A 118.7 . . ? O4A C23A C24A 112.4(18) . . ? O4A C23A H23A 109.1 . . ? C24A C23A H23A 109.1 . . ? O4A C23A H23B 109.1 . . ? C24A C23A H23B 109.1 . . ? H23A C23A H23B 107.9 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? O10A N10A O12A 120.3(19) . . ? O10A N10A O11A 115(2) . . ? O12A N10A O11A 123(2) . . ? N10A O10A Hg1A 105.2(13) . . ? O21A N20A O20A 120(2) . . ? O21A N20A O22A 118(2) . . ? O20A N20A O22A 120.5(18) . . ? N20A O20A Hg1A 112.5(12) . . ? O31A N30A O32A 125.9(16) . . ? O31A N30A O30A 115.0(15) . . ? O32A N30A O30A 118.9(16) . . ? N30A O30A Hg2A 113.6(12) . . ? O42A N40A O41A 124.8(17) . . ? O42A N40A O40A 117.8(17) . . ? O41A N40A O40A 116.8(15) . . ? N40A O40A Hg3A 110.3(11) . . ? O20B Hg1B O3B 134.2(5) . . ? O20B Hg1B O2B 130.7(6) . . ? O3B Hg1B O2B 67.5(4) . . ? O20B Hg1B O10B 134.2(7) . . ? O3B Hg1B O10B 88.1(7) . . ? O2B Hg1B O10B 74.8(5) . . ? O20B Hg1B O1B 82.2(5) . . ? O3B Hg1B O1B 130.6(4) . . ? O2B Hg1B O1B 63.1(4) . . ? O10B Hg1B O1B 79.3(6) . . ? O20B Hg1B O4B 83.1(5) . . ? O3B Hg1B O4B 63.7(4) . . ? O2B Hg1B O4B 130.9(4) . . ? O10B Hg1B O4B 108.6(6) . . ? O1B Hg1B O4B 164.8(4) . . ? C7B Hg2B O30B 167.4(6) . . ? C21B Hg3B O40B 176.6(6) . . ? O3B Cu1B N2B 94.9(5) . . ? O3B Cu1B O2B 84.5(4) . . ? N2B Cu1B O2B 175.7(6) . . ? O3B Cu1B N1B 177.5(5) . . ? N2B Cu1B N1B 87.6(5) . . ? O2B Cu1B N1B 93.0(5) . . ? C9B N1B C10B 125.0(12) . . ? C9B N1B Cu1B 126.2(11) . . ? C10B N1B Cu1B 108.8(9) . . ? C16B N2B C15B 121.4(11) . . ? C16B N2B Cu1B 126.8(9) . . ? C15B N2B Cu1B 111.3(9) . . ? C3B O1B C2B 117.6(15) . . ? C3B O1B Hg1B 114.8(10) . . ? C2B O1B Hg1B 121.3(11) . . ? C4B O2B Cu1B 123.7(9) . . ? C4B O2B Hg1B 123.0(10) . . ? Cu1B O2B Hg1B 102.5(5) . . ? C18B O3B Cu1B 125.2(9) . . ? C18B O3B Hg1B 127.0(9) . . ? Cu1B O3B Hg1B 104.0(5) . . ? C19B O4B C23B 116.8(13) . . ? C19B O4B Hg1B 114.2(8) . . ? C23B O4B Hg1B 127.6(11) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C1B C2B O1B 112(2) . . ? C1B C2B H2BA 109.1 . . ? O1B C2B H2BA 109.1 . . ? C1B C2B H2BB 109.1 . . ? O1B C2B H2BB 109.1 . . ? H2BA C2B H2BB 107.9 . . ? C8B C3B O1B 126.4(16) . . ? C8B C3B C4B 120.6(16) . . ? O1B C3B C4B 112.9(14) . . ? O2B C4B C5B 124.5(14) . . ? O2B C4B C3B 116.4(13) . . ? C5B C4B C3B 119.2(14) . . ? C4B C5B C6B 122.1(14) . . ? C4B C5B C9B 122.5(13) . . ? C6B C5B C9B 115.3(13) . . ? C5B C6B C7B 116.3(14) . . ? C5B C6B H6BA 121.9 . . ? C7B C6B H6BA 121.9 . . ? C8B C7B C6B 121.7(14) . . ? C8B C7B Hg2B 114.2(12) . . ? C6B C7B Hg2B 124.1(11) . . ? C3B C8B C7B 120.2(17) . . ? C3B C8B H8BA 119.9 . . ? C7B C8B H8BA 119.9 . . ? N1B C9B C5B 124.2(14) . . ? N1B C9B H9BA 117.9 . . ? C5B C9B H9BA 117.9 . . ? C11B C10B N1B 116.6(12) . . ? C11B C10B C15B 111.7(11) . . ? N1B C10B C15B 105.1(10) . . ? C11B C10B H10B 107.7 . . ? N1B C10B H10B 107.7 . . ? C15B C10B H10B 107.7 . . ? C10B C11B C12B 108.7(13) . . ? C10B C11B H11C 110.0 . . ? C12B C11B H11C 110.0 . . ? C10B C11B H11D 110.0 . . ? C12B C11B H11D 110.0 . . ? H11C C11B H11D 108.3 . . ? C13B C12B C11B 111.5(14) . . ? C13B C12B H12C 109.3 . . ? C11B C12B H12C 109.3 . . ? C13B C12B H12D 109.3 . . ? C11B C12B H12D 109.3 . . ? H12C C12B H12D 108.0 . . ? C14B C13B C12B 112.1(14) . . ? C14B C13B H13C 109.2 . . ? C12B C13B H13C 109.2 . . ? C14B C13B H13D 109.2 . . ? C12B C13B H13D 109.2 . . ? H13C C13B H13D 107.9 . . ? C13B C14B C15B 111.2(12) . . ? C13B C14B H14C 109.4 . . ? C15B C14B H14C 109.4 . . ? C13B C14B H14D 109.4 . . ? C15B C14B H14D 109.4 . . ? H14C C14B H14D 108.0 . . ? N2B C15B C14B 117.8(11) . . ? N2B C15B C10B 107.7(10) . . ? C14B C15B C10B 108.6(12) . . ? N2B C15B H15B 107.4 . . ? C14B C15B H15B 107.4 . . ? C10B C15B H15B 107.4 . . ? N2B C16B C17B 124.3(12) . . ? N2B C16B H16B 117.9 . . ? C17B C16B H16B 117.9 . . ? C18B C17B C22B 120.0(13) . . ? C18B C17B C16B 124.0(13) . . ? C22B C17B C16B 116.0(13) . . ? O3B C18B C17B 124.4(12) . . ? O3B C18B C19B 118.8(12) . . ? C17B C18B C19B 116.7(13) . . ? C20B C19B C18B 121.8(14) . . ? C20B C19B O4B 126.1(13) . . ? C18B C19B O4B 112.1(12) . . ? C21B C20B C19B 120.8(14) . . ? C21B C20B H20B 119.6 . . ? C19B C20B H20B 119.6 . . ? C20B C21B C22B 120.4(16) . . ? C20B C21B Hg3B 118.5(11) . . ? C22B C21B Hg3B 120.6(13) . . ? C21B C22B C17B 120.3(15) . . ? C21B C22B H22B 119.9 . . ? C17B C22B H22B 119.9 . . ? C24B C23B O4B 112.6(17) . . ? C24B C23B H23C 109.1 . . ? O4B C23B H23C 109.1 . . ? C24B C23B H23D 109.1 . . ? O4B C23B H23D 109.1 . . ? H23C C23B H23D 107.8 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? O11B N10B O12B 124(2) . . ? O11B N10B O10B 118(2) . . ? O12B N10B O10B 118.1(17) . . ? N10B O10B Hg1B 105.4(13) . . ? O21B N20B O20B 119.1(16) . . ? O21B N20B O22B 121(2) . . ? O20B N20B O22B 118.0(19) . . ? N20B O20B Hg1B 112.3(11) . . ? O31B N30B O32B 124(2) . . ? O31B N30B O30B 116.9(19) . . ? O32B N30B O30B 119(2) . . ? N30B O30B Hg2B 112.2(12) . . ? O41B N40B O42B 126.5(17) . . ? O41B N40B O40B 118.6(18) . . ? O42B N40B O40B 114.5(15) . . ? N40B O40B Hg3B 114.6(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.455 _refine_diff_density_min -3.408 _refine_diff_density_rms 0.317 # Attachment 'GQ99.CIF' data_gq99 _database_code_depnum_ccdc_archive 'CCDC 755412' #TrackingRef 'GQ99.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Br2 Hg N2 Ni O4' _chemical_formula_sum 'C24 H28 Br2 Hg N2 Ni O4' _chemical_formula_weight 827.56 _chemical_absolute_configuration ad 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' Ni Ni 0.3393 1.1124 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0776(12) _cell_length_b 17.2924(13) _cell_length_c 14.1961(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.220(8) _cell_angle_gamma 90.00 _cell_volume 2597.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 9.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2462 _exptl_absorpt_correction_T_max 0.3229 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; Due to the large atoms present, significant peaks of residual electron density remain in the difference map. These are Q1 3.42 and Q4 2.99 (0.839 and 0.823 from Hg1a) and Q2 3.41 and Q3 3.20 (0.870 and 0.847 from Hg1b) These peaks are the result of fourier truncation surrounding the heavy Hg atoms and therefore remain un-assigned. ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43549 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10176 _reflns_number_gt 10046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.7289P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(5) _refine_ls_number_reflns 10176 _refine_ls_number_parameters 618 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1A Hg -0.222599(17) 0.729406(9) -0.056440(14) 0.01893(6) Uani 1 1 d . . . Br1A Br -0.42291(6) 0.79984(4) -0.08665(4) 0.02775(12) Uani 1 1 d . . . Br2A Br -0.04085(6) 0.66930(4) -0.09349(6) 0.03927(16) Uani 1 1 d . . . Ni1A Ni -0.18729(6) 0.67622(4) 0.19029(5) 0.01568(13) Uani 1 1 d . . . N1A N -0.1613(4) 0.7267(3) 0.3090(3) 0.0172(8) Uani 1 1 d . . . N2A N -0.1860(4) 0.5862(2) 0.2607(3) 0.0168(8) Uani 1 1 d . . . O1A O -0.0923(4) 0.8634(2) 0.0052(3) 0.0255(9) Uani 1 1 d . . . O2A O -0.1591(4) 0.7627(2) 0.1227(3) 0.0219(8) Uani 1 1 d . . . O3A O -0.2388(4) 0.6286(2) 0.0684(3) 0.0197(7) Uani 1 1 d . . . O4A O -0.3199(4) 0.5849(2) -0.1194(3) 0.0240(8) Uani 1 1 d . . . C1A C -0.0909(9) 0.8822(4) -0.1590(5) 0.0435(18) Uani 1 1 d . . . H1A1 H -0.1811 0.8707 -0.1862 0.065 Uiso 1 1 calc R . . H1A2 H -0.0423 0.8341 -0.1521 0.065 Uiso 1 1 calc R . . H1A3 H -0.0647 0.9174 -0.2034 0.065 Uiso 1 1 calc R . . C2A C -0.0673(6) 0.9193(4) -0.0605(4) 0.0266(12) Uani 1 1 d . . . H2AA H 0.0216 0.9369 -0.0359 0.032 Uiso 1 1 calc R . . H2AB H -0.1232 0.9647 -0.0653 0.032 Uiso 1 1 calc R . . C3A C -0.0802(5) 0.8864(3) 0.0997(4) 0.0195(10) Uani 1 1 d . . . C4A C -0.1158(5) 0.8304(3) 0.1607(4) 0.0172(10) Uani 1 1 d . . . C5A C -0.1019(5) 0.8508(3) 0.2578(4) 0.0209(11) Uani 1 1 d . . . C6A C -0.0578(5) 0.9260(3) 0.2934(4) 0.0223(11) Uani 1 1 d . . . H6AA H -0.0515 0.9396 0.3595 0.027 Uiso 1 1 calc R . . C7A C -0.0247(5) 0.9783(3) 0.2345(4) 0.0220(11) Uani 1 1 d . . . H7AA H 0.0052 1.0279 0.2593 0.026 Uiso 1 1 calc R . . C8A C -0.0350(5) 0.9585(3) 0.1361(4) 0.0210(11) Uani 1 1 d . . . H8AA H -0.0108 0.9947 0.0947 0.025 Uiso 1 1 calc R . . C9A C -0.1299(5) 0.7990(3) 0.3262(4) 0.0178(10) Uani 1 1 d . . . H9AA H -0.1254 0.8187 0.3896 0.021 Uiso 1 1 calc R . . C10A C -0.1899(5) 0.6783(3) 0.3846(4) 0.0184(10) Uani 1 1 d . . . H10A H -0.2840 0.6747 0.3682 0.022 Uiso 1 1 calc R . . C11A C -0.1400(5) 0.7042(3) 0.4906(4) 0.0225(11) Uani 1 1 d . . . H11A H -0.1764 0.7551 0.4989 0.027 Uiso 1 1 calc R . . H11B H -0.0469 0.7095 0.5093 0.027 Uiso 1 1 calc R . . C12A C -0.1761(6) 0.6442(3) 0.5568(4) 0.0266(12) Uani 1 1 d . . . H12A H -0.2691 0.6441 0.5434 0.032 Uiso 1 1 calc R . . H12B H -0.1376 0.6587 0.6267 0.032 Uiso 1 1 calc R . . C13A C -0.1321(6) 0.5627(3) 0.5397(4) 0.0290(12) Uani 1 1 d . . . H13A H -0.1626 0.5252 0.5803 0.035 Uiso 1 1 calc R . . H13B H -0.0386 0.5610 0.5611 0.035 Uiso 1 1 calc R . . C14A C -0.1820(5) 0.5393(3) 0.4304(4) 0.0221(11) Uani 1 1 d . . . H14A H -0.1485 0.4878 0.4206 0.027 Uiso 1 1 calc R . . H14B H -0.2754 0.5362 0.4101 0.027 Uiso 1 1 calc R . . C15A C -0.1409(4) 0.5981(3) 0.3693(4) 0.0166(9) Uani 1 1 d . . . H15A H -0.0464 0.5997 0.3905 0.020 Uiso 1 1 calc R . . C16A C -0.2025(5) 0.5172(3) 0.2258(4) 0.0218(11) Uani 1 1 d . . . H16A H -0.1917 0.4758 0.2715 0.026 Uiso 1 1 calc R . . C17A C -0.2359(5) 0.4979(3) 0.1228(4) 0.0209(10) Uani 1 1 d . . . C18A C -0.2532(5) 0.5539(3) 0.0491(4) 0.0177(10) Uani 1 1 d . . . C19A C -0.2896(5) 0.5280(3) -0.0511(4) 0.0209(11) Uani 1 1 d . . . C20A C -0.2973(6) 0.4500(4) -0.0723(5) 0.0275(12) Uani 1 1 d . . . H20A H -0.3173 0.4337 -0.1391 0.033 Uiso 1 1 calc R . . C21A C -0.2764(7) 0.3948(4) 0.0022(5) 0.0357(15) Uani 1 1 d . . . H21A H -0.2809 0.3414 -0.0138 0.043 Uiso 1 1 calc R . . C22A C -0.2493(7) 0.4178(3) 0.0984(5) 0.0323(14) Uani 1 1 d . . . H22A H -0.2393 0.3803 0.1490 0.039 Uiso 1 1 calc R . . C23A C -0.3440(6) 0.5640(4) -0.2213(4) 0.0254(12) Uani 1 1 d . . . H23A H -0.4095 0.5232 -0.2395 0.030 Uiso 1 1 calc R . . H23B H -0.2659 0.5440 -0.2329 0.030 Uiso 1 1 calc R . . C24A C -0.3885(6) 0.6354(4) -0.2822(4) 0.0333(14) Uani 1 1 d . . . H24A H -0.3179 0.6717 -0.2726 0.050 Uiso 1 1 calc R . . H24B H -0.4564 0.6599 -0.2616 0.050 Uiso 1 1 calc R . . H24C H -0.4202 0.6211 -0.3520 0.050 Uiso 1 1 calc R . . Hg1B Hg 0.706205(17) 0.999758(9) 0.542764(14) 0.01805(6) Uani 1 1 d . . . Br1B Br 0.52609(6) 1.06670(4) 0.57342(5) 0.03285(14) Uani 1 1 d . . . Br2B Br 0.90095(5) 0.92248(3) 0.57643(4) 0.02464(12) Uani 1 1 d . . . Ni1B Ni 0.68667(6) 1.04816(4) 0.29788(5) 0.01635(13) Uani 1 1 d . . . N1B N 0.7270(4) 1.1323(3) 0.2316(3) 0.0192(9) Uani 1 1 d . . . N2B N 0.6270(4) 1.0019(3) 0.1757(3) 0.0198(8) Uani 1 1 d . . . O1B O 0.8212(4) 1.1387(2) 0.6099(3) 0.0203(8) Uani 1 1 d . . . O2B O 0.7508(4) 1.0935(2) 0.4215(3) 0.0196(7) Uani 1 1 d . . . O3B O 0.6368(4) 0.9682(2) 0.3634(3) 0.0215(8) Uani 1 1 d . . . O4B O 0.5677(4) 0.8693(2) 0.4820(3) 0.0236(8) Uani 1 1 d . . . C1B C 0.8698(6) 1.0921(4) 0.7734(4) 0.0266(12) Uani 1 1 d . . . H1B1 H 0.9294 1.0587 0.7536 0.040 Uiso 1 1 calc R . . H1B2 H 0.7904 1.0641 0.7653 0.040 Uiso 1 1 calc R . . H1B3 H 0.9059 1.1069 0.8427 0.040 Uiso 1 1 calc R . . C2B C 0.8445(5) 1.1638(4) 0.7097(4) 0.0236(11) Uani 1 1 d . . . H2BA H 0.7700 1.1918 0.7175 0.028 Uiso 1 1 calc R . . H2BB H 0.9184 1.1989 0.7287 0.028 Uiso 1 1 calc R . . C3B C 0.8024(5) 1.1949(3) 0.5392(4) 0.0188(11) Uani 1 1 d . . . C4B C 0.7707(5) 1.1681(4) 0.4398(4) 0.0210(11) Uani 1 1 d . . . C5B C 0.7663(5) 1.2233(4) 0.3665(4) 0.0256(11) Uani 1 1 d . . . C6B C 0.7836(8) 1.3027(4) 0.3899(5) 0.0409(17) Uani 1 1 d . . . H6BA H 0.7805 1.3394 0.3393 0.049 Uiso 1 1 calc R . . C7B C 0.8047(8) 1.3268(4) 0.4847(5) 0.0384(16) Uani 1 1 d . . . H7BA H 0.8111 1.3805 0.4994 0.046 Uiso 1 1 calc R . . C8B C 0.8170(6) 1.2730(3) 0.5610(5) 0.0255(12) Uani 1 1 d . . . H8BA H 0.8353 1.2901 0.6274 0.031 Uiso 1 1 calc R . . C9B C 0.7488(6) 1.2007(3) 0.2654(4) 0.0255(12) Uani 1 1 d . . . H9BA H 0.7540 1.2403 0.2203 0.031 Uiso 1 1 calc R . . C10B C 0.7221(5) 1.1129(3) 0.1287(4) 0.0203(10) Uani 1 1 d . . . H10B H 0.8016 1.0847 0.1305 0.024 Uiso 1 1 calc R . . C11B C 0.7081(5) 1.1811(4) 0.0575(4) 0.0228(11) Uani 1 1 d . . . H11C H 0.7816 1.2162 0.0800 0.027 Uiso 1 1 calc R . . H11D H 0.6306 1.2107 0.0544 0.027 Uiso 1 1 calc R . . C12B C 0.7002(6) 1.1480(4) -0.0443(4) 0.0312(13) Uani 1 1 d . . . H12C H 0.6884 1.1909 -0.0923 0.037 Uiso 1 1 calc R . . H12D H 0.7808 1.1219 -0.0411 0.037 Uiso 1 1 calc R . . C13B C 0.5920(6) 1.0907(4) -0.0801(4) 0.0303(13) Uani 1 1 d . . . H13C H 0.5925 1.0696 -0.1448 0.036 Uiso 1 1 calc R . . H13D H 0.5107 1.1179 -0.0892 0.036 Uiso 1 1 calc R . . C14B C 0.6028(6) 1.0240(4) -0.0070(4) 0.0262(12) Uani 1 1 d . . . H14C H 0.5274 0.9903 -0.0290 0.031 Uiso 1 1 calc R . . H14D H 0.6785 0.9925 -0.0038 0.031 Uiso 1 1 calc R . . C15B C 0.6129(5) 1.0571(3) 0.0935(4) 0.0198(10) Uani 1 1 d . . . H15B H 0.5337 1.0871 0.0870 0.024 Uiso 1 1 calc R . . C16B C 0.5977(5) 0.9302(3) 0.1573(4) 0.0209(10) Uani 1 1 d . . . H16B H 0.5852 0.9118 0.0920 0.025 Uiso 1 1 calc R . . C17B C 0.5829(5) 0.8764(3) 0.2305(4) 0.0197(10) Uani 1 1 d . . . C18B C 0.5955(5) 0.8986(3) 0.3274(4) 0.0174(10) Uani 1 1 d . . . C19B C 0.5604(5) 0.8441(3) 0.3900(4) 0.0202(11) Uani 1 1 d . . . C20B C 0.5191(5) 0.7717(3) 0.3565(4) 0.0234(11) Uani 1 1 d . . . H20B H 0.4961 0.7363 0.3994 0.028 Uiso 1 1 calc R . . C21B C 0.5102(5) 0.7490(3) 0.2598(4) 0.0232(11) Uani 1 1 d . . . H21B H 0.4830 0.6983 0.2378 0.028 Uiso 1 1 calc R . . C22B C 0.5412(5) 0.8009(3) 0.1967(4) 0.0230(11) Uani 1 1 d . . . H22B H 0.5347 0.7861 0.1310 0.028 Uiso 1 1 calc R . . C23B C 0.5432(6) 0.8144(4) 0.5495(4) 0.0282(12) Uani 1 1 d . . . H23C H 0.6039 0.7710 0.5592 0.034 Uiso 1 1 calc R . . H23D H 0.4567 0.7933 0.5227 0.034 Uiso 1 1 calc R . . C24B C 0.5563(8) 0.8538(4) 0.6455(5) 0.0426(17) Uani 1 1 d . . . H24D H 0.4920 0.8943 0.6363 0.064 Uiso 1 1 calc R . . H24E H 0.6405 0.8770 0.6699 0.064 Uiso 1 1 calc R . . H24F H 0.5450 0.8159 0.6936 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1A 0.02299(9) 0.01564(10) 0.01626(9) 0.00040(7) 0.00289(7) -0.00109(7) Br1A 0.0281(3) 0.0292(3) 0.0261(3) 0.0031(2) 0.0082(2) 0.0060(2) Br2A 0.0262(3) 0.0293(3) 0.0635(5) -0.0041(3) 0.0152(3) 0.0031(2) Ni1A 0.0222(3) 0.0095(3) 0.0130(3) 0.0025(2) 0.0015(2) -0.0017(2) N1A 0.0214(18) 0.0127(19) 0.0162(19) 0.0064(18) 0.0035(15) 0.0030(17) N2A 0.0167(19) 0.0124(19) 0.018(2) 0.0038(16) 0.0007(16) -0.0007(15) O1A 0.043(2) 0.0172(19) 0.0144(18) 0.0004(15) 0.0063(17) -0.0093(16) O2A 0.037(2) 0.0119(17) 0.0134(17) -0.0018(14) 0.0023(15) -0.0084(15) O3A 0.0259(18) 0.0147(17) 0.0156(17) -0.0001(14) 0.0015(15) -0.0006(14) O4A 0.033(2) 0.0153(19) 0.0199(19) 0.0005(15) 0.0020(16) -0.0063(16) C1A 0.077(5) 0.034(4) 0.018(3) -0.001(3) 0.011(3) -0.020(4) C2A 0.041(3) 0.022(3) 0.018(3) 0.004(2) 0.010(2) -0.006(2) C3A 0.029(3) 0.014(2) 0.015(2) 0.0021(19) 0.005(2) 0.003(2) C4A 0.019(2) 0.009(2) 0.019(2) 0.0032(19) -0.0011(19) 0.0017(18) C5A 0.025(3) 0.014(2) 0.021(3) 0.003(2) 0.001(2) 0.000(2) C6A 0.030(3) 0.015(3) 0.016(2) 0.001(2) 0.000(2) 0.001(2) C7A 0.031(3) 0.010(2) 0.021(3) -0.0022(19) 0.001(2) -0.0017(19) C8A 0.026(3) 0.015(2) 0.018(2) 0.005(2) 0.001(2) -0.002(2) C9A 0.023(2) 0.015(2) 0.013(2) -0.0008(19) 0.0004(18) -0.0012(19) C10A 0.020(2) 0.016(2) 0.018(2) 0.008(2) 0.0054(19) 0.0018(19) C11A 0.030(3) 0.020(3) 0.016(2) 0.005(2) 0.004(2) 0.001(2) C12A 0.041(3) 0.025(3) 0.016(3) 0.006(2) 0.012(2) 0.000(2) C13A 0.040(3) 0.023(3) 0.023(3) 0.013(2) 0.008(2) 0.005(2) C14A 0.027(3) 0.018(2) 0.021(3) 0.007(2) 0.007(2) 0.006(2) C15A 0.018(2) 0.017(2) 0.012(2) 0.0025(18) 0.0010(18) -0.0011(18) C16A 0.033(3) 0.007(2) 0.023(3) 0.0049(19) 0.004(2) 0.0013(19) C17A 0.030(2) 0.009(2) 0.022(2) -0.004(2) 0.005(2) -0.005(2) C18A 0.021(2) 0.008(2) 0.021(3) -0.0020(19) 0.0022(19) -0.0045(19) C19A 0.022(2) 0.017(3) 0.022(3) 0.000(2) 0.002(2) -0.0025(19) C20A 0.032(3) 0.018(3) 0.028(3) -0.003(2) 0.002(2) -0.006(2) C21A 0.049(4) 0.011(3) 0.038(4) -0.003(2) -0.002(3) -0.005(2) C22A 0.054(4) 0.005(2) 0.033(3) -0.002(2) 0.006(3) -0.003(2) C23A 0.028(3) 0.028(3) 0.020(3) -0.005(2) 0.006(2) -0.007(2) C24A 0.035(3) 0.043(4) 0.017(3) 0.001(3) 0.001(2) -0.009(3) Hg1B 0.02226(9) 0.01387(10) 0.01705(9) 0.00032(7) 0.00431(7) -0.00027(7) Br1B 0.0277(3) 0.0259(3) 0.0465(4) -0.0013(3) 0.0134(3) 0.0052(2) Br2B 0.0266(3) 0.0229(3) 0.0233(3) 0.0001(2) 0.0056(2) 0.0056(2) Ni1B 0.0215(3) 0.0124(3) 0.0139(3) 0.0025(2) 0.0033(2) -0.0014(2) N1B 0.019(2) 0.017(2) 0.021(2) 0.0035(18) 0.0054(17) 0.0018(16) N2B 0.0210(19) 0.021(2) 0.0168(19) 0.003(2) 0.0054(16) 0.0005(19) O1B 0.0278(19) 0.0149(18) 0.0174(19) 0.0007(15) 0.0056(15) -0.0031(14) O2B 0.0285(18) 0.0111(16) 0.0180(18) -0.0003(14) 0.0049(15) -0.0028(14) O3B 0.0295(19) 0.0138(17) 0.0162(17) 0.0004(15) -0.0007(15) -0.0052(15) O4B 0.036(2) 0.0160(18) 0.0175(18) 0.0028(15) 0.0063(16) -0.0103(16) C1B 0.031(3) 0.032(3) 0.020(3) 0.002(2) 0.011(2) 0.001(2) C2B 0.022(2) 0.029(3) 0.021(3) -0.005(2) 0.007(2) -0.005(2) C3B 0.020(2) 0.014(2) 0.023(3) 0.000(2) 0.007(2) -0.0054(19) C4B 0.023(2) 0.017(3) 0.021(3) 0.001(2) 0.003(2) -0.0044(19) C5B 0.034(3) 0.016(3) 0.026(3) -0.001(2) 0.009(2) -0.007(2) C6B 0.074(5) 0.015(3) 0.031(3) 0.004(3) 0.010(3) -0.008(3) C7B 0.067(5) 0.013(3) 0.037(4) -0.002(3) 0.018(3) -0.009(3) C8B 0.034(3) 0.016(3) 0.025(3) -0.003(2) 0.007(2) -0.004(2) C9B 0.037(3) 0.015(2) 0.022(3) 0.007(2) 0.006(2) -0.002(2) C10B 0.023(2) 0.020(2) 0.017(2) 0.008(2) 0.006(2) 0.004(2) C11B 0.024(3) 0.024(3) 0.022(3) 0.010(2) 0.008(2) 0.001(2) C12B 0.037(3) 0.035(3) 0.023(3) 0.016(3) 0.010(2) 0.002(3) C13B 0.033(3) 0.038(3) 0.018(3) 0.010(2) 0.005(2) 0.003(3) C14B 0.030(3) 0.027(3) 0.021(3) 0.008(2) 0.006(2) 0.002(2) C15B 0.023(2) 0.020(2) 0.016(2) 0.008(2) 0.0068(19) 0.004(2) C16B 0.024(2) 0.021(3) 0.015(2) 0.002(2) 0.002(2) 0.000(2) C17B 0.023(2) 0.016(2) 0.017(2) 0.001(2) 0.002(2) 0.000(2) C18B 0.017(2) 0.010(2) 0.020(2) 0.0008(19) -0.0016(19) -0.0003(18) C19B 0.019(2) 0.020(3) 0.018(3) 0.005(2) -0.001(2) -0.0005(19) C20B 0.027(3) 0.014(2) 0.026(3) 0.006(2) 0.003(2) -0.001(2) C21B 0.023(2) 0.019(3) 0.022(3) 0.000(2) -0.001(2) -0.003(2) C22B 0.031(3) 0.015(3) 0.017(2) -0.001(2) -0.002(2) -0.001(2) C23B 0.039(3) 0.023(3) 0.022(3) 0.005(2) 0.008(2) -0.004(2) C24B 0.071(5) 0.038(4) 0.019(3) 0.008(3) 0.013(3) -0.015(3) _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 Hg1A Br1A 2.4551(6) . ? Hg1A Br2A 2.4571(7) . ? Hg1A O2A 2.497(4) . ? Hg1A O3A 2.530(4) . ? Ni1A N1A 1.843(4) . ? Ni1A O3A 1.848(4) . ? Ni1A N2A 1.848(4) . ? Ni1A O2A 1.852(4) . ? N1A C9A 1.301(7) . ? N1A C10A 1.468(6) . ? N2A C16A 1.284(7) . ? N2A C15A 1.488(6) . ? O1A C3A 1.368(7) . ? O1A C2A 1.426(7) . ? O2A C4A 1.319(6) . ? O3A C18A 1.320(6) . ? O4A C19A 1.352(7) . ? O4A C23A 1.437(7) . ? C1A C2A 1.489(9) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C8A 1.386(8) . ? C3A C4A 1.430(7) . ? C4A C5A 1.386(8) . ? C5A C9A 1.421(7) . ? C5A C6A 1.427(8) . ? C6A C7A 1.353(8) . ? C6A H6AA 0.9500 . ? C7A C8A 1.409(8) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A C11A 1.510(7) . ? C10A C15A 1.528(7) . ? C10A H10A 1.0000 . ? C11A C12A 1.530(7) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.533(8) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.540(8) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.492(7) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 1.0000 . ? C16A C17A 1.438(7) . ? C16A H16A 0.9500 . ? C17A C18A 1.397(8) . ? C17A C22A 1.424(7) . ? C18A C19A 1.431(8) . ? C19A C20A 1.378(8) . ? C20A C21A 1.392(9) . ? C20A H20A 0.9500 . ? C21A C22A 1.368(10) . ? C21A H21A 0.9500 . ? C22A H22A 0.9500 . ? C23A C24A 1.504(9) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? Hg1B Br1B 2.4545(6) . ? Hg1B Br2B 2.4612(6) . ? Hg1B O3B 2.493(4) . ? Hg1B O2B 2.517(4) . ? Ni1B O3B 1.840(4) . ? Ni1B N2B 1.846(5) . ? Ni1B N1B 1.858(4) . ? Ni1B O2B 1.860(4) . ? N1B C9B 1.272(8) . ? N1B C10B 1.484(7) . ? N2B C16B 1.289(8) . ? N2B C15B 1.480(6) . ? O1B C3B 1.368(7) . ? O1B C2B 1.431(7) . ? O2B C4B 1.321(7) . ? O3B C18B 1.334(6) . ? O4B C19B 1.356(7) . ? O4B C23B 1.431(7) . ? C1B C2B 1.512(8) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C8B 1.383(8) . ? C3B C4B 1.428(8) . ? C4B C5B 1.402(8) . ? C5B C6B 1.412(9) . ? C5B C9B 1.444(8) . ? C6B C7B 1.362(10) . ? C6B H6BA 0.9500 . ? C7B C8B 1.404(9) . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B C15B 1.513(7) . ? C10B C11B 1.530(7) . ? C10B H10B 1.0000 . ? C11B C12B 1.532(8) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.521(9) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.532(8) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.509(7) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15B 1.0000 . ? C16B C17B 1.440(7) . ? C16B H16B 0.9500 . ? C17B C18B 1.395(8) . ? C17B C22B 1.420(7) . ? C18B C19B 1.428(7) . ? C19B C20B 1.368(8) . ? C20B C21B 1.404(8) . ? C20B H20B 0.9500 . ? C21B C22B 1.380(8) . ? C21B H21B 0.9500 . ? C22B H22B 0.9500 . ? C23B C24B 1.492(9) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? 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 Br1A Hg1A Br2A 158.11(3) . . ? Br1A Hg1A O2A 91.78(10) . . ? Br2A Hg1A O2A 108.30(10) . . ? Br1A Hg1A O3A 102.49(9) . . ? Br2A Hg1A O3A 95.22(9) . . ? O2A Hg1A O3A 60.16(12) . . ? N1A Ni1A O3A 171.40(18) . . ? N1A Ni1A N2A 86.0(2) . . ? O3A Ni1A N2A 94.69(18) . . ? N1A Ni1A O2A 94.94(18) . . ? O3A Ni1A O2A 85.85(16) . . ? N2A Ni1A O2A 170.00(19) . . ? C9A N1A C10A 121.0(5) . . ? C9A N1A Ni1A 126.0(4) . . ? C10A N1A Ni1A 112.9(4) . . ? C16A N2A C15A 119.6(4) . . ? C16A N2A Ni1A 126.6(4) . . ? C15A N2A Ni1A 113.0(3) . . ? C3A O1A C2A 117.5(4) . . ? C4A O2A Ni1A 127.0(3) . . ? C4A O2A Hg1A 125.4(3) . . ? Ni1A O2A Hg1A 107.54(16) . . ? C18A O3A Ni1A 128.0(4) . . ? C18A O3A Hg1A 123.9(3) . . ? Ni1A O3A Hg1A 106.42(17) . . ? C19A O4A C23A 118.1(5) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O1A C2A C1A 107.9(5) . . ? O1A C2A H2AA 110.1 . . ? C1A C2A H2AA 110.1 . . ? O1A C2A H2AB 110.1 . . ? C1A C2A H2AB 110.1 . . ? H2AA C2A H2AB 108.4 . . ? O1A C3A C8A 123.2(5) . . ? O1A C3A C4A 115.6(5) . . ? C8A C3A C4A 121.1(5) . . ? O2A C4A C5A 123.5(5) . . ? O2A C4A C3A 119.1(5) . . ? C5A C4A C3A 117.4(5) . . ? C4A C5A C9A 122.4(5) . . ? C4A C5A C6A 120.6(5) . . ? C9A C5A C6A 117.0(5) . . ? C7A C6A C5A 121.1(5) . . ? C7A C6A H6AA 119.4 . . ? C5A C6A H6AA 119.4 . . ? C6A C7A C8A 119.5(5) . . ? C6A C7A H7AA 120.2 . . ? C8A C7A H7AA 120.2 . . ? C3A C8A C7A 120.1(5) . . ? C3A C8A H8AA 119.9 . . ? C7A C8A H8AA 119.9 . . ? N1A C9A C5A 125.3(5) . . ? N1A C9A H9AA 117.3 . . ? C5A C9A H9AA 117.3 . . ? N1A C10A C11A 117.7(4) . . ? N1A C10A C15A 104.5(4) . . ? C11A C10A C15A 111.7(4) . . ? N1A C10A H10A 107.5 . . ? C11A C10A H10A 107.5 . . ? C15A C10A H10A 107.5 . . ? C10A C11A C12A 109.0(5) . . ? C10A C11A H11A 109.9 . . ? C12A C11A H11A 109.9 . . ? C10A C11A H11B 109.9 . . ? C12A C11A H11B 109.9 . . ? H11A C11A H11B 108.3 . . ? C11A C12A C13A 111.9(5) . . ? C11A C12A H12A 109.2 . . ? C13A C12A H12A 109.2 . . ? C11A C12A H12B 109.2 . . ? C13A C12A H12B 109.2 . . ? H12A C12A H12B 107.9 . . ? C12A C13A C14A 111.4(5) . . ? C12A C13A H13A 109.4 . . ? C14A C13A H13A 109.4 . . ? C12A C13A H13B 109.4 . . ? C14A C13A H13B 109.4 . . ? H13A C13A H13B 108.0 . . ? C15A C14A C13A 109.1(5) . . ? C15A C14A H14A 109.9 . . ? C13A C14A H14A 109.9 . . ? C15A C14A H14B 109.9 . . ? C13A C14A H14B 109.9 . . ? H14A C14A H14B 108.3 . . ? N2A C15A C14A 116.2(4) . . ? N2A C15A C10A 104.4(4) . . ? C14A C15A C10A 110.7(4) . . ? N2A C15A H15A 108.5 . . ? C14A C15A H15A 108.5 . . ? C10A C15A H15A 108.5 . . ? N2A C16A C17A 124.9(5) . . ? N2A C16A H16A 117.5 . . ? C17A C16A H16A 117.5 . . ? C18A C17A C22A 120.7(5) . . ? C18A C17A C16A 122.5(5) . . ? C22A C17A C16A 116.8(5) . . ? O3A C18A C17A 122.8(5) . . ? O3A C18A C19A 119.6(5) . . ? C17A C18A C19A 117.5(5) . . ? O4A C19A C20A 124.7(6) . . ? O4A C19A C18A 114.9(5) . . ? C20A C19A C18A 120.3(5) . . ? C19A C20A C21A 121.2(6) . . ? C19A C20A H20A 119.4 . . ? C21A C20A H20A 119.4 . . ? C22A C21A C20A 119.8(6) . . ? C22A C21A H21A 120.1 . . ? C20A C21A H21A 120.1 . . ? C21A C22A C17A 120.1(6) . . ? C21A C22A H22A 119.9 . . ? C17A C22A H22A 119.9 . . ? O4A C23A C24A 107.7(5) . . ? O4A C23A H23A 110.2 . . ? C24A C23A H23A 110.2 . . ? O4A C23A H23B 110.2 . . ? C24A C23A H23B 110.2 . . ? H23A C23A H23B 108.5 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? Br1B Hg1B Br2B 158.98(2) . . ? Br1B Hg1B O3B 105.27(10) . . ? Br2B Hg1B O3B 93.85(9) . . ? Br1B Hg1B O2B 98.74(9) . . ? Br2B Hg1B O2B 98.29(9) . . ? O3B Hg1B O2B 60.39(12) . . ? O3B Ni1B N2B 94.10(19) . . ? O3B Ni1B N1B 176.15(19) . . ? N2B Ni1B N1B 86.4(2) . . ? O3B Ni1B O2B 85.85(16) . . ? N2B Ni1B O2B 178.50(19) . . ? N1B Ni1B O2B 93.78(19) . . ? C9B N1B C10B 121.9(5) . . ? C9B N1B Ni1B 125.8(4) . . ? C10B N1B Ni1B 112.2(3) . . ? C16B N2B C15B 120.0(5) . . ? C16B N2B Ni1B 127.3(4) . . ? C15B N2B Ni1B 112.7(4) . . ? C3B O1B C2B 117.0(4) . . ? C4B O2B Ni1B 126.3(4) . . ? C4B O2B Hg1B 123.3(3) . . ? Ni1B O2B Hg1B 106.05(16) . . ? C18B O3B Ni1B 127.2(3) . . ? C18B O3B Hg1B 123.8(3) . . ? Ni1B O3B Hg1B 107.70(16) . . ? C19B O4B C23B 117.5(4) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? O1B C2B C1B 106.9(5) . . ? O1B C2B H2BA 110.3 . . ? C1B C2B H2BA 110.3 . . ? O1B C2B H2BB 110.3 . . ? C1B C2B H2BB 110.3 . . ? H2BA C2B H2BB 108.6 . . ? O1B C3B C8B 123.2(5) . . ? O1B C3B C4B 115.6(5) . . ? C8B C3B C4B 121.1(5) . . ? O2B C4B C5B 123.5(5) . . ? O2B C4B C3B 119.3(5) . . ? C5B C4B C3B 117.2(5) . . ? C4B C5B C6B 121.0(6) . . ? C4B C5B C9B 121.2(5) . . ? C6B C5B C9B 117.7(6) . . ? C7B C6B C5B 120.1(6) . . ? C7B C6B H6BA 120.0 . . ? C5B C6B H6BA 120.0 . . ? C6B C7B C8B 120.6(6) . . ? C6B C7B H7BA 119.7 . . ? C8B C7B H7BA 119.7 . . ? C3B C8B C7B 119.7(6) . . ? C3B C8B H8BA 120.1 . . ? C7B C8B H8BA 120.1 . . ? N1B C9B C5B 125.5(5) . . ? N1B C9B H9BA 117.3 . . ? C5B C9B H9BA 117.3 . . ? N1B C10B C15B 105.2(4) . . ? N1B C10B C11B 116.3(5) . . ? C15B C10B C11B 111.0(4) . . ? N1B C10B H10B 108.0 . . ? C15B C10B H10B 108.0 . . ? C11B C10B H10B 108.0 . . ? C10B C11B C12B 107.6(5) . . ? C10B C11B H11C 110.2 . . ? C12B C11B H11C 110.2 . . ? C10B C11B H11D 110.2 . . ? C12B C11B H11D 110.2 . . ? H11C C11B H11D 108.5 . . ? C13B C12B C11B 112.2(5) . . ? C13B C12B H12C 109.2 . . ? C11B C12B H12C 109.2 . . ? C13B C12B H12D 109.2 . . ? C11B C12B H12D 109.2 . . ? H12C C12B H12D 107.9 . . ? C12B C13B C14B 111.6(5) . . ? C12B C13B H13C 109.3 . . ? C14B C13B H13C 109.3 . . ? C12B C13B H13D 109.3 . . ? C14B C13B H13D 109.3 . . ? H13C C13B H13D 108.0 . . ? C15B C14B C13B 108.9(5) . . ? C15B C14B H14C 109.9 . . ? C13B C14B H14C 109.9 . . ? C15B C14B H14D 109.9 . . ? C13B C14B H14D 109.9 . . ? H14C C14B H14D 108.3 . . ? N2B C15B C14B 117.5(4) . . ? N2B C15B C10B 105.3(4) . . ? C14B C15B C10B 112.5(4) . . ? N2B C15B H15B 107.0 . . ? C14B C15B H15B 107.0 . . ? C10B C15B H15B 107.0 . . ? N2B C16B C17B 123.4(5) . . ? N2B C16B H16B 118.3 . . ? C17B C16B H16B 118.3 . . ? C18B C17B C22B 121.0(5) . . ? C18B C17B C16B 122.3(5) . . ? C22B C17B C16B 116.4(5) . . ? O3B C18B C17B 123.3(5) . . ? O3B C18B C19B 118.9(5) . . ? C17B C18B C19B 117.7(5) . . ? O4B C19B C20B 123.2(5) . . ? O4B C19B C18B 115.9(5) . . ? C20B C19B C18B 120.8(5) . . ? C19B C20B C21B 121.0(5) . . ? C19B C20B H20B 119.5 . . ? C21B C20B H20B 119.5 . . ? C22B C21B C20B 119.6(5) . . ? C22B C21B H21B 120.2 . . ? C20B C21B H21B 120.2 . . ? C21B C22B C17B 119.8(5) . . ? C21B C22B H22B 120.1 . . ? C17B C22B H22B 120.1 . . ? O4B C23B C24B 108.9(5) . . ? O4B C23B H23C 109.9 . . ? C24B C23B H23C 109.9 . . ? O4B C23B H23D 109.9 . . ? C24B C23B H23D 109.9 . . ? H23C C23B H23D 108.3 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.420 _refine_diff_density_min -2.306 _refine_diff_density_rms 0.180 # Attachment 'gq98.CIF' data_3t _database_code_depnum_ccdc_archive 'CCDC 755413' #TrackingRef 'gq98.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Br2 Cu Hg N2 O4' _chemical_formula_sum 'C24 H28 Br2 Cu Hg N2 O4' _chemical_formula_weight 832.42 _chemical_absolute_configuration ad 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' Cu Cu 0.3201 1.2651 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0988(9) _cell_length_b 17.2977(10) _cell_length_c 14.2186(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.704(6) _cell_angle_gamma 90.00 _cell_volume 2614.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 9.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2454 _exptl_absorpt_correction_T_max 0.3220 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120170 _diffrn_reflns_av_R_equivalents 0.1385 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.20 _reflns_number_total 12853 _reflns_number_gt 12799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+6.6495P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(5) _refine_ls_number_reflns 12853 _refine_ls_number_parameters 617 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1A Hg -0.228292(18) 0.731559(10) -0.057475(14) 0.01939(5) Uani 1 1 d . . . Br1A Br -0.42796(6) 0.80154(4) -0.08727(5) 0.02809(13) Uani 1 1 d . . . Br2A Br -0.04603(6) 0.67140(4) -0.09233(7) 0.04153(18) Uani 1 1 d . . . Cu1A Cu -0.19719(6) 0.67885(4) 0.18567(5) 0.01695(12) Uani 1 1 d . . . N1A N -0.1688(4) 0.7304(3) 0.3103(3) 0.0169(7) Uani 1 1 d . . . N2A N -0.1898(4) 0.5854(2) 0.2598(3) 0.0163(8) Uani 1 1 d . . . O1A O -0.0941(5) 0.8687(3) 0.0080(3) 0.0264(9) Uani 1 1 d . . . O2A O -0.1574(4) 0.7670(2) 0.1212(3) 0.0242(8) Uani 1 1 d . . . O3A O -0.2576(4) 0.6285(2) 0.0622(3) 0.0203(8) Uani 1 1 d . . . O4A O -0.3263(4) 0.5830(2) -0.1218(3) 0.0215(8) Uani 1 1 d . . . C1A C -0.0935(10) 0.8884(5) -0.1566(5) 0.047(2) Uani 1 1 d . . . H1A1 H -0.1827 0.8746 -0.1809 0.070 Uiso 1 1 calc R . . H1A2 H -0.0421 0.8416 -0.1516 0.070 Uiso 1 1 calc R . . H1A3 H -0.0723 0.9247 -0.2023 0.070 Uiso 1 1 calc R . . C2A C -0.0678(6) 0.9253(3) -0.0573(4) 0.0250(11) Uani 1 1 d . . . H2AA H 0.0211 0.9420 -0.0336 0.030 Uiso 1 1 calc R . . H2AB H -0.1222 0.9713 -0.0609 0.030 Uiso 1 1 calc R . . C3A C -0.0800(5) 0.8909(3) 0.1022(4) 0.0202(10) Uani 1 1 d . . . C4A C -0.1157(5) 0.8340(3) 0.1611(4) 0.0171(9) Uani 1 1 d . . . C5A C -0.1045(5) 0.8535(3) 0.2594(4) 0.0197(10) Uani 1 1 d . . . C6A C -0.0589(5) 0.9274(3) 0.2965(4) 0.0217(10) Uani 1 1 d . . . H6AA H -0.0521 0.9403 0.3628 0.026 Uiso 1 1 calc R . . C7A C -0.0247(6) 0.9799(3) 0.2374(4) 0.0233(11) Uani 1 1 d . . . H7AA H 0.0059 1.0292 0.2629 0.028 Uiso 1 1 calc R . . C8A C -0.0341(5) 0.9620(3) 0.1405(4) 0.0200(10) Uani 1 1 d . . . H8AA H -0.0089 0.9988 0.1002 0.024 Uiso 1 1 calc R . . C9A C -0.1329(5) 0.8011(3) 0.3283(4) 0.0197(10) Uani 1 1 d . . . H9AA H -0.1246 0.8201 0.3925 0.024 Uiso 1 1 calc R . . C10A C -0.1949(5) 0.6785(3) 0.3840(4) 0.0183(9) Uani 1 1 d . . . H10A H -0.2884 0.6746 0.3693 0.022 Uiso 1 1 calc R . . C11A C -0.1439(6) 0.7036(4) 0.4899(4) 0.0247(11) Uani 1 1 d . . . H11A H -0.1797 0.7545 0.4994 0.030 Uiso 1 1 calc R . . H11B H -0.0513 0.7087 0.5075 0.030 Uiso 1 1 calc R . . C12A C -0.1799(6) 0.6428(4) 0.5558(4) 0.0284(12) Uani 1 1 d . . . H12A H -0.1423 0.6572 0.6254 0.034 Uiso 1 1 calc R . . H12B H -0.2725 0.6423 0.5426 0.034 Uiso 1 1 calc R . . C13A C -0.1352(6) 0.5621(4) 0.5382(4) 0.0295(12) Uani 1 1 d . . . H13A H -0.0421 0.5610 0.5584 0.035 Uiso 1 1 calc R . . H13B H -0.1645 0.5243 0.5790 0.035 Uiso 1 1 calc R . . C14A C -0.1847(5) 0.5390(3) 0.4303(4) 0.0211(10) Uani 1 1 d . . . H14A H -0.1503 0.4878 0.4204 0.025 Uiso 1 1 calc R . . H14B H -0.2776 0.5349 0.4116 0.025 Uiso 1 1 calc R . . C15A C -0.1466(5) 0.5985(3) 0.3662(4) 0.0173(9) Uani 1 1 d . . . H15A H -0.0526 0.6007 0.3862 0.021 Uiso 1 1 calc R . . C16A C -0.2066(5) 0.5167(3) 0.2241(4) 0.0219(10) Uani 1 1 d . . . H16A H -0.1956 0.4749 0.2691 0.026 Uiso 1 1 calc R . . C17A C -0.2407(5) 0.4983(4) 0.1215(4) 0.0224(10) Uani 1 1 d . . . C18A C -0.2625(5) 0.5542(3) 0.0461(4) 0.0195(10) Uani 1 1 d . . . C19A C -0.2944(5) 0.5267(3) -0.0522(4) 0.0204(10) Uani 1 1 d . . . C20A C -0.2955(6) 0.4481(4) -0.0731(5) 0.0250(11) Uani 1 1 d . . . H20A H -0.3117 0.4312 -0.1392 0.030 Uiso 1 1 calc R . . C21A C -0.2729(7) 0.3942(4) 0.0030(5) 0.0343(14) Uani 1 1 d . . . H21A H -0.2749 0.3404 -0.0111 0.041 Uiso 1 1 calc R . . C22A C -0.2480(7) 0.4189(3) 0.0972(5) 0.0294(13) Uani 1 1 d . . . H22A H -0.2350 0.3817 0.1484 0.035 Uiso 1 1 calc R . . C23A C -0.3478(6) 0.5617(4) -0.2228(4) 0.0249(11) Uani 1 1 d . . . H23A H -0.4095 0.5189 -0.2402 0.030 Uiso 1 1 calc R . . H23B H -0.2683 0.5443 -0.2344 0.030 Uiso 1 1 calc R . . C24A C -0.3973(7) 0.6312(4) -0.2838(5) 0.0333(14) Uani 1 1 d . . . H24A H -0.3308 0.6703 -0.2735 0.050 Uiso 1 1 calc R . . H24B H -0.4686 0.6525 -0.2647 0.050 Uiso 1 1 calc R . . H24C H -0.4249 0.6166 -0.3533 0.050 Uiso 1 1 calc R . . Hg1B Hg 0.712077(18) 0.997878(10) 0.544984(14) 0.01842(5) Uani 1 1 d . . . Br1B Br 0.53033(6) 1.06410(4) 0.57296(6) 0.03458(15) Uani 1 1 d . . . Br2B Br 0.90686(5) 0.92196(4) 0.58019(4) 0.02484(12) Uani 1 1 d . . . Cu1B Cu 0.69528(6) 1.04564(4) 0.30235(5) 0.01767(12) Uani 1 1 d . . . N1B N 0.7347(4) 1.1335(3) 0.2320(3) 0.0192(8) Uani 1 1 d . . . N2B N 0.6280(4) 1.0001(3) 0.1744(3) 0.0200(8) Uani 1 1 d . . . O1B O 0.8267(4) 1.1419(2) 0.6108(3) 0.0228(8) Uani 1 1 d . . . O2B O 0.7629(4) 1.0937(2) 0.4272(3) 0.0209(8) Uani 1 1 d . . . O3B O 0.6415(4) 0.9624(2) 0.3668(3) 0.0217(8) Uani 1 1 d . . . O4B O 0.5737(4) 0.8635(2) 0.4827(3) 0.0234(8) Uani 1 1 d . . . C1B C 0.8760(7) 1.0971(4) 0.7755(4) 0.0285(12) Uani 1 1 d . . . H1B1 H 0.9359 1.0635 0.7562 0.043 Uiso 1 1 calc R . . H1B2 H 0.7975 1.0689 0.7689 0.043 Uiso 1 1 calc R . . H1B3 H 0.9119 1.1132 0.8439 0.043 Uiso 1 1 calc R . . C2B C 0.8495(6) 1.1676(4) 0.7100(4) 0.0245(11) Uani 1 1 d . . . H2BA H 0.7751 1.1955 0.7178 0.029 Uiso 1 1 calc R . . H2BB H 0.9225 1.2032 0.7278 0.029 Uiso 1 1 calc R . . C3B C 0.8075(5) 1.1970(3) 0.5406(4) 0.0199(10) Uani 1 1 d . . . C4B C 0.7785(5) 1.1691(4) 0.4420(4) 0.0201(11) Uani 1 1 d . . . C5B C 0.7699(6) 1.2235(4) 0.3673(4) 0.0255(11) Uani 1 1 d . . . C6B C 0.7833(8) 1.3032(4) 0.3883(5) 0.0378(16) Uani 1 1 d . . . H6BA H 0.7761 1.3396 0.3370 0.045 Uiso 1 1 calc R . . C7B C 0.8071(8) 1.3277(4) 0.4844(6) 0.0383(16) Uani 1 1 d . . . H7BA H 0.8163 1.3814 0.4989 0.046 Uiso 1 1 calc R . . C8B C 0.8178(6) 1.2753(4) 0.5600(5) 0.0265(12) Uani 1 1 d . . . H8BA H 0.8323 1.2933 0.6255 0.032 Uiso 1 1 calc R . . C9B C 0.7546(6) 1.2018(3) 0.2666(4) 0.0245(11) Uani 1 1 d . . . H9BA H 0.7597 1.2418 0.2222 0.029 Uiso 1 1 calc R . . C10B C 0.7261(5) 1.1135(3) 0.1297(4) 0.0182(9) Uani 1 1 d . . . H10B H 0.8050 1.0852 0.1303 0.022 Uiso 1 1 calc R . . C11B C 0.7124(5) 1.1807(4) 0.0580(4) 0.0228(11) Uani 1 1 d . . . H11C H 0.6347 1.2100 0.0546 0.027 Uiso 1 1 calc R . . H11D H 0.7850 1.2162 0.0804 0.027 Uiso 1 1 calc R . . C12B C 0.7066(5) 1.1484(4) -0.0429(4) 0.0268(11) Uani 1 1 d . . . H12C H 0.7872 1.1226 -0.0399 0.032 Uiso 1 1 calc R . . H12D H 0.6947 1.1914 -0.0906 0.032 Uiso 1 1 calc R . . C13B C 0.5991(6) 1.0908(4) -0.0778(5) 0.0300(12) Uani 1 1 d . . . H13C H 0.5181 1.1178 -0.0865 0.036 Uiso 1 1 calc R . . H13D H 0.5999 1.0697 -0.1424 0.036 Uiso 1 1 calc R . . C14B C 0.6093(6) 1.0244(4) -0.0056(4) 0.0244(11) Uani 1 1 d . . . H14C H 0.5347 0.9904 -0.0277 0.029 Uiso 1 1 calc R . . H14D H 0.6852 0.9932 -0.0023 0.029 Uiso 1 1 calc R . . C15B C 0.6174(5) 1.0568(3) 0.0942(4) 0.0201(10) Uani 1 1 d . . . H15B H 0.5382 1.0867 0.0875 0.024 Uiso 1 1 calc R . . C16B C 0.5957(5) 0.9299(3) 0.1575(4) 0.0192(10) Uani 1 1 d . . . H16B H 0.5796 0.9121 0.0919 0.023 Uiso 1 1 calc R . . C17B C 0.5816(5) 0.8754(3) 0.2292(4) 0.0178(9) Uani 1 1 d . . . C18B C 0.5973(5) 0.8954(3) 0.3285(4) 0.0175(9) Uani 1 1 d . . . C19B C 0.5613(5) 0.8398(3) 0.3900(4) 0.0183(9) Uani 1 1 d . . . C20B C 0.5151(5) 0.7689(3) 0.3535(4) 0.0231(11) Uani 1 1 d . . . H20B H 0.4905 0.7330 0.3951 0.028 Uiso 1 1 calc R . . C21B C 0.5037(5) 0.7484(3) 0.2556(4) 0.0247(11) Uani 1 1 d . . . H21B H 0.4743 0.6985 0.2318 0.030 Uiso 1 1 calc R . . C22B C 0.5353(5) 0.8012(3) 0.1951(4) 0.0227(11) Uani 1 1 d . . . H22B H 0.5261 0.7877 0.1286 0.027 Uiso 1 1 calc R . . C23B C 0.5424(6) 0.8092(4) 0.5481(4) 0.0264(12) Uani 1 1 d . . . H23C H 0.5950 0.7622 0.5538 0.032 Uiso 1 1 calc R . . H23D H 0.4530 0.7938 0.5226 0.032 Uiso 1 1 calc R . . C24B C 0.5652(10) 0.8466(5) 0.6459(5) 0.047(2) Uani 1 1 d . . . H24D H 0.5190 0.8956 0.6386 0.071 Uiso 1 1 calc R . . H24E H 0.6554 0.8566 0.6737 0.071 Uiso 1 1 calc R . . H24F H 0.5364 0.8123 0.6898 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1A 0.02150(9) 0.02017(10) 0.01580(8) 0.00075(7) 0.00425(6) -0.00072(7) Br1A 0.0270(3) 0.0328(3) 0.0264(3) 0.0025(2) 0.0108(2) 0.0055(2) Br2A 0.0246(3) 0.0338(3) 0.0689(5) -0.0039(3) 0.0176(3) 0.0035(2) Cu1A 0.0230(3) 0.0140(3) 0.0127(3) 0.0028(2) 0.0033(2) -0.0021(2) N1A 0.0224(18) 0.0159(18) 0.0134(18) 0.0046(17) 0.0065(15) 0.0011(17) N2A 0.0191(19) 0.0158(18) 0.016(2) 0.0044(15) 0.0075(16) 0.0010(15) O1A 0.042(2) 0.0216(19) 0.0137(18) 0.0012(15) 0.0046(17) -0.0098(17) O2A 0.037(2) 0.0181(18) 0.0159(18) 0.0026(15) 0.0046(16) -0.0083(16) O3A 0.0293(19) 0.0138(17) 0.0169(18) -0.0007(13) 0.0050(15) -0.0032(14) O4A 0.029(2) 0.0179(18) 0.0156(18) 0.0000(15) 0.0035(15) -0.0050(15) C1A 0.086(6) 0.039(4) 0.018(3) 0.001(3) 0.019(4) -0.021(4) C2A 0.037(3) 0.021(3) 0.018(3) 0.006(2) 0.010(2) -0.006(2) C3A 0.024(2) 0.020(2) 0.014(2) 0.0007(19) 0.0013(19) -0.0020(19) C4A 0.017(2) 0.017(2) 0.016(2) 0.0008(18) 0.0023(18) -0.0012(17) C5A 0.021(2) 0.020(2) 0.016(2) 0.0034(19) 0.0023(19) -0.0020(18) C6A 0.028(2) 0.019(2) 0.015(2) 0.0012(19) 0.0000(19) -0.002(2) C7A 0.032(3) 0.011(2) 0.022(3) -0.0016(18) 0.000(2) -0.0013(18) C8A 0.024(2) 0.016(2) 0.019(2) 0.0043(19) 0.0051(19) -0.0048(19) C9A 0.020(2) 0.022(2) 0.017(2) 0.0021(19) 0.0056(18) 0.0050(19) C10A 0.019(2) 0.021(2) 0.016(2) 0.0047(18) 0.0070(18) 0.0042(18) C11A 0.029(3) 0.027(3) 0.018(2) 0.003(2) 0.007(2) 0.002(2) C12A 0.034(3) 0.037(3) 0.017(3) 0.008(2) 0.012(2) 0.003(2) C13A 0.036(3) 0.033(3) 0.019(3) 0.013(2) 0.008(2) 0.007(2) C14A 0.024(2) 0.022(2) 0.021(2) 0.012(2) 0.013(2) 0.0074(19) C15A 0.020(2) 0.019(2) 0.014(2) 0.0044(17) 0.0058(18) -0.0014(17) C16A 0.028(2) 0.016(2) 0.024(3) 0.0076(19) 0.011(2) -0.0007(18) C17A 0.028(2) 0.017(2) 0.023(2) -0.001(2) 0.0076(19) -0.002(2) C18A 0.020(2) 0.019(2) 0.019(2) -0.0014(19) 0.0037(18) -0.0038(19) C19A 0.023(2) 0.015(2) 0.022(3) -0.001(2) 0.004(2) -0.0033(19) C20A 0.026(3) 0.023(3) 0.024(3) -0.005(2) 0.004(2) -0.002(2) C21A 0.045(4) 0.017(3) 0.036(4) -0.003(2) 0.002(3) -0.002(2) C22A 0.046(3) 0.013(2) 0.028(3) 0.008(2) 0.008(3) -0.001(2) C23A 0.028(3) 0.027(3) 0.020(3) -0.004(2) 0.008(2) -0.008(2) C24A 0.036(3) 0.043(4) 0.017(3) 0.000(3) 0.003(2) -0.009(3) Hg1B 0.02050(8) 0.01869(9) 0.01637(8) 0.00037(7) 0.00575(6) 0.00000(7) Br1B 0.0265(3) 0.0314(3) 0.0490(4) -0.0010(3) 0.0158(3) 0.0063(2) Br2B 0.0236(2) 0.0284(3) 0.0229(3) 0.0004(2) 0.0071(2) 0.0055(2) Cu1B 0.0221(3) 0.0167(3) 0.0138(3) 0.0028(2) 0.0046(2) -0.0023(2) N1B 0.022(2) 0.022(2) 0.015(2) 0.0035(16) 0.0084(17) -0.0011(17) N2B 0.0198(18) 0.025(2) 0.0150(18) 0.0063(19) 0.0054(15) 0.0028(19) O1B 0.029(2) 0.0210(19) 0.0182(19) -0.0018(15) 0.0066(16) -0.0012(15) O2B 0.030(2) 0.0164(18) 0.0145(17) -0.0007(14) 0.0032(15) -0.0020(15) O3B 0.031(2) 0.0168(17) 0.0159(17) 0.0012(14) 0.0053(15) -0.0084(15) O4B 0.036(2) 0.0201(18) 0.0141(18) 0.0010(15) 0.0078(16) -0.0120(16) C1B 0.038(3) 0.035(3) 0.014(2) 0.002(2) 0.010(2) -0.002(3) C2B 0.029(3) 0.027(3) 0.020(3) -0.001(2) 0.012(2) 0.000(2) C3B 0.020(2) 0.018(2) 0.022(3) -0.001(2) 0.0066(19) -0.0047(19) C4B 0.020(2) 0.019(3) 0.022(3) 0.0031(19) 0.007(2) -0.0038(17) C5B 0.035(3) 0.017(2) 0.026(3) 0.004(2) 0.011(2) -0.003(2) C6B 0.063(5) 0.022(3) 0.028(3) 0.002(2) 0.012(3) -0.010(3) C7B 0.065(5) 0.015(3) 0.035(4) -0.001(2) 0.014(3) -0.009(3) C8B 0.034(3) 0.021(3) 0.028(3) -0.007(2) 0.016(2) -0.008(2) C9B 0.032(3) 0.020(2) 0.024(3) 0.005(2) 0.013(2) -0.005(2) C10B 0.020(2) 0.021(2) 0.013(2) 0.0059(18) 0.0040(18) 0.0014(18) C11B 0.020(2) 0.030(3) 0.021(3) 0.011(2) 0.011(2) 0.0044(19) C12B 0.025(3) 0.037(3) 0.019(3) 0.012(2) 0.007(2) 0.000(2) C13B 0.032(3) 0.039(3) 0.020(3) 0.012(2) 0.008(2) 0.002(2) C14B 0.030(3) 0.029(3) 0.015(2) 0.006(2) 0.008(2) 0.003(2) C15B 0.020(2) 0.026(2) 0.014(2) 0.0075(19) 0.0044(18) -0.0008(19) C16B 0.022(2) 0.022(2) 0.013(2) 0.0021(18) 0.0051(18) 0.0012(19) C17B 0.019(2) 0.018(2) 0.014(2) 0.0013(18) 0.0005(17) 0.0007(18) C18B 0.017(2) 0.018(2) 0.014(2) 0.0019(18) -0.0004(17) -0.0032(18) C19B 0.018(2) 0.020(2) 0.017(2) 0.0032(19) 0.0048(18) -0.0012(18) C20B 0.023(2) 0.019(2) 0.025(3) 0.002(2) 0.003(2) -0.002(2) C21B 0.027(3) 0.023(3) 0.021(3) -0.002(2) 0.000(2) -0.002(2) C22B 0.025(2) 0.020(2) 0.018(2) -0.001(2) -0.002(2) 0.002(2) C23B 0.035(3) 0.025(3) 0.022(3) 0.004(2) 0.013(2) -0.006(2) C24B 0.079(6) 0.046(4) 0.018(3) 0.000(3) 0.016(3) -0.022(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 Hg1A Br2A 2.4489(7) . ? Hg1A Br1A 2.4527(7) . ? Hg1A O2A 2.509(4) . ? Hg1A O3A 2.548(4) . ? Cu1A O2A 1.895(4) . ? Cu1A O3A 1.901(4) . ? Cu1A N2A 1.919(4) . ? Cu1A N1A 1.927(4) . ? N1A C9A 1.289(7) . ? N1A C10A 1.471(6) . ? N2A C16A 1.284(7) . ? N2A C15A 1.468(7) . ? O1A C3A 1.359(7) . ? O1A C2A 1.436(7) . ? O2A C4A 1.315(6) . ? O3A C18A 1.305(7) . ? O4A C19A 1.362(7) . ? O4A C23A 1.436(7) . ? C1A C2A 1.501(9) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C8A 1.382(7) . ? C3A C4A 1.419(7) . ? C4A C5A 1.409(7) . ? C5A C6A 1.420(8) . ? C5A C9A 1.434(7) . ? C6A C7A 1.363(8) . ? C6A H6AA 0.9500 . ? C7A C8A 1.387(8) . ? C7A H7AA 0.9500 . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A C11A 1.513(8) . ? C10A C15A 1.531(7) . ? C10A H10A 1.0000 . ? C11A C12A 1.535(8) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C13A 1.526(9) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.526(8) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.513(7) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A H15A 1.0000 . ? C16A C17A 1.433(8) . ? C16A H16A 0.9500 . ? C17A C18A 1.411(8) . ? C17A C22A 1.414(8) . ? C18A C19A 1.421(8) . ? C19A C20A 1.391(8) . ? C20A C21A 1.396(10) . ? C20A H20A 0.9500 . ? C21A C22A 1.357(10) . ? C21A H21A 0.9500 . ? C22A H22A 0.9500 . ? C23A C24A 1.492(10) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? Hg1B Br1B 2.4496(7) . ? Hg1B Br2B 2.4549(6) . ? Hg1B O3B 2.504(4) . ? Hg1B O2B 2.533(4) . ? Cu1B O3B 1.893(4) . ? Cu1B O2B 1.908(4) . ? Cu1B N2B 1.926(5) . ? Cu1B N1B 1.937(4) . ? N1B C9B 1.274(8) . ? N1B C10B 1.472(7) . ? N2B C16B 1.269(8) . ? N2B C15B 1.483(6) . ? O1B C3B 1.352(7) . ? O1B C2B 1.431(7) . ? O2B C4B 1.323(7) . ? O3B C18B 1.314(6) . ? O4B C19B 1.348(7) . ? O4B C23B 1.433(7) . ? C1B C2B 1.511(9) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C8B 1.381(8) . ? C3B C4B 1.429(8) . ? C4B C5B 1.402(8) . ? C5B C6B 1.410(9) . ? C5B C9B 1.441(8) . ? C6B C7B 1.382(10) . ? C6B H6BA 0.9500 . ? C7B C8B 1.385(10) . ? C7B H7BA 0.9500 . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B C15B 1.523(7) . ? C10B C11B 1.525(7) . ? C10B H10B 1.0000 . ? C11B C12B 1.523(8) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.524(9) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.523(8) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.504(8) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B H15B 1.0000 . ? C16B C17B 1.429(7) . ? C16B H16B 0.9500 . ? C17B C22B 1.415(8) . ? C17B C18B 1.415(7) . ? C18B C19B 1.432(7) . ? C19B C20B 1.373(8) . ? C20B C21B 1.406(8) . ? C20B H20B 0.9500 . ? C21B C22B 1.368(9) . ? C21B H21B 0.9500 . ? C22B H22B 0.9500 . ? C23B C24B 1.488(9) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? 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 Br2A Hg1A Br1A 158.85(3) . . ? Br2A Hg1A O2A 105.75(11) . . ? Br1A Hg1A O2A 93.41(11) . . ? Br2A Hg1A O3A 96.28(10) . . ? Br1A Hg1A O3A 100.25(10) . . ? O2A Hg1A O3A 63.77(13) . . ? O2A Cu1A O3A 89.46(18) . . ? O2A Cu1A N2A 164.6(2) . . ? O3A Cu1A N2A 93.99(19) . . ? O2A Cu1A N1A 94.23(19) . . ? O3A Cu1A N1A 169.20(18) . . ? N2A Cu1A N1A 85.11(19) . . ? C9A N1A C10A 123.5(5) . . ? C9A N1A Cu1A 125.5(4) . . ? C10A N1A Cu1A 111.0(4) . . ? C16A N2A C15A 121.1(4) . . ? C16A N2A Cu1A 125.7(4) . . ? C15A N2A Cu1A 112.7(3) . . ? C3A O1A C2A 117.3(5) . . ? C4A O2A Cu1A 127.0(4) . . ? C4A O2A Hg1A 128.4(3) . . ? Cu1A O2A Hg1A 104.17(17) . . ? C18A O3A Cu1A 126.8(4) . . ? C18A O3A Hg1A 125.4(4) . . ? Cu1A O3A Hg1A 102.57(17) . . ? C19A O4A C23A 118.5(5) . . ? C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? O1A C2A C1A 107.4(5) . . ? O1A C2A H2AA 110.2 . . ? C1A C2A H2AA 110.2 . . ? O1A C2A H2AB 110.2 . . ? C1A C2A H2AB 110.2 . . ? H2AA C2A H2AB 108.5 . . ? O1A C3A C8A 124.3(5) . . ? O1A C3A C4A 114.4(5) . . ? C8A C3A C4A 121.2(5) . . ? O2A C4A C5A 124.0(5) . . ? O2A C4A C3A 118.7(5) . . ? C5A C4A C3A 117.3(5) . . ? C4A C5A C6A 120.3(5) . . ? C4A C5A C9A 123.5(5) . . ? C6A C5A C9A 116.1(5) . . ? C7A C6A C5A 120.3(5) . . ? C7A C6A H6AA 119.9 . . ? C5A C6A H6AA 119.9 . . ? C6A C7A C8A 120.6(5) . . ? C6A C7A H7AA 119.7 . . ? C8A C7A H7AA 119.7 . . ? C3A C8A C7A 120.3(5) . . ? C3A C8A H8AA 119.9 . . ? C7A C8A H8AA 119.9 . . ? N1A C9A C5A 125.4(5) . . ? N1A C9A H9AA 117.3 . . ? C5A C9A H9AA 117.3 . . ? N1A C10A C11A 116.1(5) . . ? N1A C10A C15A 106.5(4) . . ? C11A C10A C15A 112.1(4) . . ? N1A C10A H10A 107.3 . . ? C11A C10A H10A 107.3 . . ? C15A C10A H10A 107.3 . . ? C10A C11A C12A 108.8(5) . . ? C10A C11A H11A 109.9 . . ? C12A C11A H11A 109.9 . . ? C10A C11A H11B 109.9 . . ? C12A C11A H11B 109.9 . . ? H11A C11A H11B 108.3 . . ? C13A C12A C11A 111.9(5) . . ? C13A C12A H12A 109.2 . . ? C11A C12A H12A 109.2 . . ? C13A C12A H12B 109.2 . . ? C11A C12A H12B 109.2 . . ? H12A C12A H12B 107.9 . . ? C14A C13A C12A 111.4(5) . . ? C14A C13A H13A 109.4 . . ? C12A C13A H13A 109.4 . . ? C14A C13A H13B 109.4 . . ? C12A C13A H13B 109.4 . . ? H13A C13A H13B 108.0 . . ? C15A C14A C13A 110.1(5) . . ? C15A C14A H14A 109.6 . . ? C13A C14A H14A 109.6 . . ? C15A C14A H14B 109.6 . . ? C13A C14A H14B 109.6 . . ? H14A C14A H14B 108.1 . . ? N2A C15A C14A 116.8(4) . . ? N2A C15A C10A 106.4(4) . . ? C14A C15A C10A 110.1(4) . . ? N2A C15A H15A 107.7 . . ? C14A C15A H15A 107.7 . . ? C10A C15A H15A 107.7 . . ? N2A C16A C17A 125.0(5) . . ? N2A C16A H16A 117.5 . . ? C17A C16A H16A 117.5 . . ? C18A C17A C22A 119.6(5) . . ? C18A C17A C16A 124.0(5) . . ? C22A C17A C16A 116.3(5) . . ? O3A C18A C17A 123.5(5) . . ? O3A C18A C19A 119.2(5) . . ? C17A C18A C19A 117.3(5) . . ? O4A C19A C20A 124.0(5) . . ? O4A C19A C18A 114.5(5) . . ? C20A C19A C18A 121.5(6) . . ? C19A C20A C21A 119.9(6) . . ? C19A C20A H20A 120.1 . . ? C21A C20A H20A 120.1 . . ? C22A C21A C20A 119.7(6) . . ? C22A C21A H21A 120.1 . . ? C20A C21A H21A 120.1 . . ? C21A C22A C17A 121.9(6) . . ? C21A C22A H22A 119.1 . . ? C17A C22A H22A 119.1 . . ? O4A C23A C24A 107.5(5) . . ? O4A C23A H23A 110.2 . . ? C24A C23A H23A 110.2 . . ? O4A C23A H23B 110.2 . . ? C24A C23A H23B 110.2 . . ? H23A C23A H23B 108.5 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? Br1B Hg1B Br2B 159.23(3) . . ? Br1B Hg1B O3B 104.27(10) . . ? Br2B Hg1B O3B 94.36(10) . . ? Br1B Hg1B O2B 98.72(10) . . ? Br2B Hg1B O2B 97.73(10) . . ? O3B Hg1B O2B 63.63(13) . . ? O3B Cu1B O2B 88.61(17) . . ? O3B Cu1B N2B 93.18(19) . . ? O2B Cu1B N2B 178.2(2) . . ? O3B Cu1B N1B 174.90(19) . . ? O2B Cu1B N1B 92.96(19) . . ? N2B Cu1B N1B 85.2(2) . . ? C9B N1B C10B 123.6(5) . . ? C9B N1B Cu1B 124.6(4) . . ? C10B N1B Cu1B 111.5(3) . . ? C16B N2B C15B 122.2(5) . . ? C16B N2B Cu1B 125.6(4) . . ? C15B N2B Cu1B 112.2(4) . . ? C3B O1B C2B 117.0(5) . . ? C4B O2B Cu1B 125.1(4) . . ? C4B O2B Hg1B 125.7(3) . . ? Cu1B O2B Hg1B 103.11(17) . . ? C18B O3B Cu1B 127.0(4) . . ? C18B O3B Hg1B 127.4(3) . . ? Cu1B O3B Hg1B 104.65(17) . . ? C19B O4B C23B 117.4(5) . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? O1B C2B C1B 107.7(5) . . ? O1B C2B H2BA 110.2 . . ? C1B C2B H2BA 110.2 . . ? O1B C2B H2BB 110.2 . . ? C1B C2B H2BB 110.2 . . ? H2BA C2B H2BB 108.5 . . ? O1B C3B C8B 123.9(6) . . ? O1B C3B C4B 115.4(5) . . ? C8B C3B C4B 120.7(6) . . ? O2B C4B C5B 124.3(5) . . ? O2B C4B C3B 118.1(5) . . ? C5B C4B C3B 117.6(6) . . ? C4B C5B C6B 121.0(6) . . ? C4B C5B C9B 122.7(6) . . ? C6B C5B C9B 116.2(5) . . ? C7B C6B C5B 119.3(6) . . ? C7B C6B H6BA 120.3 . . ? C5B C6B H6BA 120.3 . . ? C6B C7B C8B 121.0(6) . . ? C6B C7B H7BA 119.5 . . ? C8B C7B H7BA 119.5 . . ? C3B C8B C7B 120.2(6) . . ? C3B C8B H8BA 119.9 . . ? C7B C8B H8BA 119.9 . . ? N1B C9B C5B 125.6(5) . . ? N1B C9B H9BA 117.2 . . ? C5B C9B H9BA 117.2 . . ? N1B C10B C15B 107.3(4) . . ? N1B C10B C11B 116.6(5) . . ? C15B C10B C11B 110.6(4) . . ? N1B C10B H10B 107.3 . . ? C15B C10B H10B 107.3 . . ? C11B C10B H10B 107.3 . . ? C12B C11B C10B 108.6(5) . . ? C12B C11B H11C 110.0 . . ? C10B C11B H11C 110.0 . . ? C12B C11B H11D 110.0 . . ? C10B C11B H11D 110.0 . . ? H11C C11B H11D 108.3 . . ? C11B C12B C13B 111.3(5) . . ? C11B C12B H12C 109.4 . . ? C13B C12B H12C 109.4 . . ? C11B C12B H12D 109.4 . . ? C13B C12B H12D 109.4 . . ? H12C C12B H12D 108.0 . . ? C14B C13B C12B 112.0(5) . . ? C14B C13B H13C 109.2 . . ? C12B C13B H13C 109.2 . . ? C14B C13B H13D 109.2 . . ? C12B C13B H13D 109.2 . . ? H13C C13B H13D 107.9 . . ? C15B C14B C13B 109.2(5) . . ? C15B C14B H14C 109.8 . . ? C13B C14B H14C 109.8 . . ? C15B C14B H14D 109.8 . . ? C13B C14B H14D 109.8 . . ? H14C C14B H14D 108.3 . . ? N2B C15B C14B 116.6(5) . . ? N2B C15B C10B 106.9(4) . . ? C14B C15B C10B 112.2(4) . . ? N2B C15B H15B 106.8 . . ? C14B C15B H15B 106.8 . . ? C10B C15B H15B 106.8 . . ? N2B C16B C17B 125.4(5) . . ? N2B C16B H16B 117.3 . . ? C17B C16B H16B 117.3 . . ? C22B C17B C18B 119.5(5) . . ? C22B C17B C16B 117.3(5) . . ? C18B C17B C16B 122.8(5) . . ? O3B C18B C17B 123.7(5) . . ? O3B C18B C19B 118.4(5) . . ? C17B C18B C19B 118.0(5) . . ? O4B C19B C20B 124.3(5) . . ? O4B C19B C18B 115.2(5) . . ? C20B C19B C18B 120.6(5) . . ? C19B C20B C21B 121.2(5) . . ? C19B C20B H20B 119.4 . . ? C21B C20B H20B 119.4 . . ? C22B C21B C20B 119.1(5) . . ? C22B C21B H21B 120.4 . . ? C20B C21B H21B 120.4 . . ? C21B C22B C17B 121.6(5) . . ? C21B C22B H22B 119.2 . . ? C17B C22B H22B 119.2 . . ? O4B C23B C24B 108.3(5) . . ? O4B C23B H23C 110.0 . . ? C24B C23B H23C 110.0 . . ? O4B C23B H23D 110.0 . . ? C24B C23B H23D 110.0 . . ? H23C C23B H23D 108.4 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.168 _refine_diff_density_min -3.052 _refine_diff_density_rms 0.168