# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Craig Rice' _publ_contact_author_email C.R.RICE@HUD.AC.UK _publ_section_title ; Isomeric Pyridyl-Thiazole Donor Units for Metal Ion Recognition in Bi- and Tri-metallic Helicates ; loop_ _publ_author_name 'Craig Rice' 'Sam Bullock' 'Lisa J Gillie' 'Lindsay P. Harding' 'Thomas Riis-Johannessen' ; M.Whitehead ; # Attachment 'HgZn_helicte.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 730541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Hg1.29Zn0.71(C28H20N6S2O)2][ClO4]4.2Et2O.1.42MeCN' _chemical_formula_sum 'C66.88 H64.32 Cl4 Hg1.29 N13.44 O20 S4 Zn0.71' _chemical_formula_weight 1951.57 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.571(3) _cell_length_b 16.707(2) _cell_length_c 22.669(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.375(3) _cell_angle_gamma 90.00 _cell_volume 7499.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3905 _exptl_absorpt_coefficient_mu 3.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67783 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'frames each covering 0.3\% in\w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35235 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8908 _reflns_number_gt 6780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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. Complex cation: Disorder present in the complex cation is caused by one of the metal sites being occupied by Zn in ca. 71 % of the crytsal and Hg in the remaining ca. 29 % of the crystal (these values correspond to refined population parameters). The two py-py units which constitute this site thus alternate between two positions; one in which metal-ligand bonds are relatively short (bonding to Zn) and one in which metal-ligand bonds are relatively long (bonding to Hg). The coordinates and ADPs of the metals were constrained to be equal (EXYZ and EADP) and their population parameters refined against a free variable which converged to ca. 0.71. The population parameters of the two py-py units were kept identical to those of their corresponding metal and their geometries were restrained using similartiy (SAME), coplanarity (FLAT) and distance (DFIX) restraints. The displacement parameters were refined anisotropically, but constrained (EADP) to be identical to those of the same atom in the other component. Counter anions: Of the two crystallographically independent perchlorate anions, one was sufficiently disordered to merit modelling as two components, the population parameters of which converged at 0.27:0.73. The geomteries of each component were introduced using a non-disordered ClO4 fragment from the CSD (FRAG/FEND) and further refined as rigid bodies (AFIX 9). Atoms were assigned ADPs, but they were constrained (EADP) to be identical to those of the same atom in the other component. Intstitial solvent 1: The site-occupancy of a partially resolved MeCN molecule was refined against a free variable which converged to 0.71. The molecule was refined isotropically and without positional or displacement parameters restraints. Intstitial solvent 2: A suspect molecule of Et2O was identified in the Fourier difference map, but owing to severe disorder, attempts at modelling were abandoned and the scattering contributions removed using the SQUEEZE routine in PLATON (A. L. Spek, Acta. Cryst., 1990, A46, C-34; PLATON -- A Multipurpose Crystallographic Tool; Utrecht University, Utrecht, The Netherlands, A. L. Spek, 2003). The additional Et2O solvates expressed in the complex formula [Hg1.29Zn0.71(L)2][ClO4]4.1.42MeCN.2Et2O are consistent with a residual electron density count of ca. 236 electrons per unit cell. ; _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^)+(0.0923P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8908 _refine_ls_number_parameters 486 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.921 _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 Hg1 Hg 1.0000 0.363302(16) 0.2500 0.03143(10) Uani 1 2 d S . . Zn1 Zn 1.0000 0.7890(9) 0.2500 0.0303(3) Uani 0.714(2) 2 d SP . 1 Hg2 Hg 1.0000 0.7854(8) 0.2500 0.0303(3) Uani 0.286(2) 2 d SP . 2 N11A N 1.0465(3) 0.8730(4) 0.2101(3) 0.0387(15) Uani 0.714(2) 1 d PDU . 1 C12A C 1.1145(4) 0.8833(4) 0.2436(4) 0.0435(18) Uani 0.714(2) 1 d PDU . 1 C13A C 1.1497(5) 0.9396(5) 0.2240(5) 0.068(3) Uani 0.714(2) 1 d PDU . 1 H13A H 1.1968 0.9466 0.2477 0.082 Uiso 0.714(2) 1 calc PR . 1 C14A C 1.1161(6) 0.9849(6) 0.1704(5) 0.088(4) Uani 0.714(2) 1 d PDU . 1 H14A H 1.1401 1.0229 0.1564 0.105 Uiso 0.714(2) 1 calc PR . 1 C15A C 1.0481(7) 0.9755(6) 0.1372(5) 0.081(3) Uani 0.714(2) 1 d PDU . 1 H15A H 1.0240 1.0077 0.1007 0.097 Uiso 0.714(2) 1 calc PR . 1 C16A C 1.0148(5) 0.9177(5) 0.1578(4) 0.053(2) Uani 0.714(2) 1 d PDU . 1 H16A H 0.9678 0.9096 0.1339 0.064 Uiso 0.714(2) 1 calc PR . 1 N21A N 1.1014(5) 0.7841(3) 0.3143(4) 0.0313(10) Uani 0.714(2) 1 d PDU . 1 C22A C 1.1454(4) 0.8309(4) 0.3006(3) 0.0373(14) Uani 0.714(2) 1 d PDU . 1 C23A C 1.2132(4) 0.8283(4) 0.3392(4) 0.0464(18) Uani 0.714(2) 1 d PDU . 1 H23A H 1.2447 0.8609 0.3306 0.056 Uiso 0.714(2) 1 calc PR . 1 C24A C 1.2337(5) 0.7772(5) 0.3904(4) 0.0517(19) Uani 0.714(2) 1 d PDU . 1 H24A H 1.2807 0.7750 0.4164 0.062 Uiso 0.714(2) 1 calc PR . 1 C25A C 1.1967(6) 0.7340(5) 0.4056(4) 0.0355(14) Uani 0.714(2) 1 d PDU . 1 H25A H 1.2141 0.7004 0.4424 0.043 Uiso 0.714(2) 1 calc PR . 1 C26A C 1.1240(6) 0.7364(4) 0.3648(4) 0.0332(10) Uani 0.714(2) 1 d PDU . 1 N11B N 1.0663(10) 0.8828(9) 0.2164(8) 0.0387(15) Uani 0.286(2) 1 d PDU . 2 C12B C 1.1341(10) 0.8826(8) 0.2531(8) 0.0435(18) Uani 0.286(2) 1 d PDU . 2 C13B C 1.1774(10) 0.9314(9) 0.2374(9) 0.068(3) Uani 0.286(2) 1 d PDU . 2 H13B H 1.2245 0.9310 0.2632 0.082 Uiso 0.286(2) 1 calc PR . 2 C14B C 1.1519(12) 0.9802(10) 0.1847(10) 0.088(4) Uani 0.286(2) 1 d PDU . 2 H14B H 1.1814 1.0136 0.1737 0.105 Uiso 0.286(2) 1 calc PR . 2 C15B C 1.0843(12) 0.9807(10) 0.1480(9) 0.081(3) Uani 0.286(2) 1 d PDU . 2 H15B H 1.0661 1.0144 0.1114 0.097 Uiso 0.286(2) 1 calc PR . 2 C16B C 1.0423(10) 0.9310(10) 0.1651(9) 0.053(2) Uani 0.286(2) 1 d PDU . 2 H16B H 0.9952 0.9313 0.1395 0.064 Uiso 0.286(2) 1 calc PR . 2 N21B N 1.1076(11) 0.7844(7) 0.3164(9) 0.0313(10) Uani 0.286(2) 1 d PDU . 2 C22B C 1.1572(10) 0.8275(7) 0.3087(8) 0.0373(14) Uani 0.286(2) 1 d PDU . 2 C23B C 1.2230(11) 0.8195(10) 0.3517(9) 0.0464(18) Uani 0.286(2) 1 d PDU . 2 H23B H 1.2582 0.8495 0.3470 0.056 Uiso 0.286(2) 1 calc PR . 2 C24B C 1.2362(13) 0.7670(12) 0.4012(9) 0.0517(19) Uani 0.286(2) 1 d PDU . 2 H24B H 1.2819 0.7615 0.4305 0.062 Uiso 0.286(2) 1 calc PR . 2 C25B C 1.1943(15) 0.7266(10) 0.4112(9) 0.0355(14) Uani 0.286(2) 1 d PDU . 2 H25B H 1.2067 0.6911 0.4468 0.043 Uiso 0.286(2) 1 calc PR . 2 C26B C 1.1235(13) 0.7350(7) 0.3656(10) 0.0332(10) Uani 0.286(2) 1 d PDU . 2 N31 N 1.00692(19) 0.6968(2) 0.32903(19) 0.0328(8) Uani 1 1 d D . . C32 C 1.0696(2) 0.6896(3) 0.3720(2) 0.0348(10) Uani 1 1 d D . . S33 S 1.07846(7) 0.62542(8) 0.43270(6) 0.0440(3) Uani 1 1 d D . . C34 C 0.9932(3) 0.6058(3) 0.3996(2) 0.0394(11) Uani 1 1 d D . . H34 H 0.9704 0.5697 0.4164 0.047 Uiso 1 1 calc R . . C35 C 0.9637(2) 0.6504(3) 0.3452(2) 0.0335(10) Uani 1 1 d D . . C36 C 0.8900(2) 0.6505(3) 0.3024(2) 0.0347(11) Uani 1 1 d . . . H36A H 0.8650 0.6214 0.3241 0.042 Uiso 1 1 calc R . . H36B H 0.8736 0.7065 0.2958 0.042 Uiso 1 1 calc R . . O1 O 0.87527(16) 0.6147(2) 0.24133(16) 0.0343(7) Uani 1 1 d . . . N41 N 0.91257(18) 0.4498(2) 0.16986(17) 0.0287(8) Uani 1 1 d . . . C42 C 0.8965(2) 0.4198(3) 0.1093(2) 0.0354(11) Uani 1 1 d . . . C43 C 0.8361(2) 0.4391(3) 0.0592(2) 0.0365(11) Uani 1 1 d . . . H43 H 0.8253 0.4174 0.0175 0.044 Uiso 1 1 calc R . . C44 C 0.7932(2) 0.4887(3) 0.0702(2) 0.0372(11) Uani 1 1 d . . . H44 H 0.7518 0.5024 0.0359 0.045 Uiso 1 1 calc R . . C45 C 0.8079(2) 0.5196(3) 0.1294(2) 0.0371(11) Uani 1 1 d . . . H45 H 0.7769 0.5543 0.1370 0.045 Uiso 1 1 calc R . . C46 C 0.8695(2) 0.4996(3) 0.1793(2) 0.0339(10) Uani 1 1 d . . . C47 C 0.8900(3) 0.5317(3) 0.2464(2) 0.0377(11) Uani 1 1 d . . . H47A H 0.8648 0.5040 0.2685 0.045 Uiso 1 1 calc R . . H47B H 0.9389 0.5229 0.2713 0.045 Uiso 1 1 calc R . . N51 N 1.00179(19) 0.3405(2) 0.34506(18) 0.0292(8) Uani 1 1 d . . . C52 C 1.0510(2) 0.3673(3) 0.3955(2) 0.0350(10) Uani 1 1 d . . . S53 S 1.04470(8) 0.33976(10) 0.46571(7) 0.0498(4) Uani 1 1 d . . . C54 C 0.9720(3) 0.2895(4) 0.4225(3) 0.0486(14) Uani 1 1 d . . . H54 H 0.9464 0.2604 0.4410 0.058 Uiso 1 1 calc R . . C55 C 0.9551(2) 0.2963(3) 0.3577(2) 0.0335(10) Uani 1 1 d . . . N61 N 0.8875(2) 0.2925(3) 0.2464(2) 0.0439(11) Uani 1 1 d . . . C62 C 0.8954(2) 0.2668(3) 0.3047(2) 0.0371(11) Uani 1 1 d . . . C63 C 0.8487(3) 0.2164(4) 0.3134(3) 0.0514(14) Uani 1 1 d . . . H63 H 0.8553 0.1979 0.3551 0.062 Uiso 1 1 calc R . . C64 C 0.7926(3) 0.1936(4) 0.2606(3) 0.0592(17) Uani 1 1 d . . . H64 H 0.7602 0.1590 0.2658 0.071 Uiso 1 1 calc R . . C65 C 0.7836(3) 0.2196(4) 0.2024(3) 0.0600(17) Uani 1 1 d . . . H65 H 0.7451 0.2039 0.1657 0.072 Uiso 1 1 calc R . . C66 C 0.8319(3) 0.2704(4) 0.1965(3) 0.0569(16) Uani 1 1 d . . . H66 H 0.8250 0.2901 0.1551 0.068 Uiso 1 1 calc R . . Cl1A Cl 0.1227(4) 0.8896(6) 0.5079(5) 0.0382(4) Uani 0.272(6) 1 d PG A 1 O1AA O 0.1708(8) 0.8873(10) 0.4790(7) 0.074(2) Uani 0.272(6) 1 d PG A 1 O1BA O 0.0827(7) 0.9599(10) 0.4873(9) 0.090(2) Uani 0.272(6) 1 d PG A 1 O1CA O 0.0809(8) 0.8208(8) 0.4884(9) 0.062(2) Uani 0.272(6) 1 d PG A 1 O1DA O 0.1568(9) 0.8903(13) 0.5758(8) 0.0557(16) Uani 0.272(6) 1 d PG A 1 Cl1B Cl 0.11717(15) 0.8815(2) 0.51007(17) 0.0382(4) Uani 0.728(6) 1 d PG A 2 O1AB O 0.1323(3) 0.9180(3) 0.4599(2) 0.074(2) Uani 0.728(6) 1 d PG A 2 O1BB O 0.0532(3) 0.9101(4) 0.5065(3) 0.090(2) Uani 0.728(6) 1 d PG A 2 O1CB O 0.1147(3) 0.7967(3) 0.5016(3) 0.062(2) Uani 0.728(6) 1 d PG A 2 O1DB O 0.1684(3) 0.9015(4) 0.5713(3) 0.0557(16) Uani 0.728(6) 1 d PG A 2 Cl2 Cl 0.84003(8) 0.51102(10) 0.90979(7) 0.0551(4) Uani 1 1 d . . . O2A O 0.8256(3) 0.4278(3) 0.9049(3) 0.0785(16) Uani 1 1 d . . . O2B O 0.9105(2) 0.5190(3) 0.9554(3) 0.0892(18) Uani 1 1 d . . . O2C O 0.8353(4) 0.5463(5) 0.8530(3) 0.127(3) Uani 1 1 d . . . O2D O 0.7975(2) 0.5503(3) 0.93561(19) 0.0579(11) Uani 1 1 d . . . N1 N 0.8796(6) 0.7902(7) 0.3971(6) 0.098(4) Uiso 0.713(10) 1 d P . . C1A C 1.1087(6) 0.8328(8) 0.0650(6) 0.081(3) Uiso 0.713(10) 1 d P . . C1B C -0.0931(9) 0.8902(11) 0.4829(8) 0.130(6) Uiso 0.713(10) 1 d P . . H1A H -0.0449 0.8872 0.5106 0.155 Uiso 0.713(10) 1 calc PR . . H1B H -0.1198 0.8804 0.5085 0.155 Uiso 0.713(10) 1 calc PR . . H1C H -0.1037 0.9435 0.4633 0.155 Uiso 0.713(10) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.03070(14) 0.03921(16) 0.02444(14) 0.000 0.01100(10) 0.000 Zn1 0.0267(3) 0.0357(9) 0.0256(3) 0.000 0.00717(18) 0.000 Hg2 0.0267(3) 0.0357(9) 0.0256(3) 0.000 0.00717(18) 0.000 N11A 0.048(4) 0.032(3) 0.034(3) 0.001(2) 0.014(3) -0.004(3) C12A 0.050(5) 0.039(3) 0.040(4) -0.006(2) 0.017(4) -0.018(3) C13A 0.063(6) 0.073(6) 0.064(5) 0.005(4) 0.020(5) -0.033(5) C14A 0.100(7) 0.087(7) 0.060(6) 0.017(5) 0.013(6) -0.061(7) C15A 0.100(7) 0.068(6) 0.064(6) 0.029(5) 0.021(6) -0.024(7) C16A 0.069(6) 0.042(5) 0.041(4) 0.007(3) 0.013(4) -0.012(4) N21A 0.032(2) 0.034(2) 0.027(2) -0.0064(15) 0.0104(17) -0.0037(16) C22A 0.036(4) 0.039(3) 0.033(3) -0.010(2) 0.011(3) -0.010(2) C23A 0.036(3) 0.055(4) 0.041(4) -0.014(3) 0.008(3) -0.019(3) C24A 0.041(3) 0.063(5) 0.038(4) -0.015(3) 0.002(3) 0.008(3) C25A 0.049(3) 0.030(3) 0.020(3) -0.002(2) 0.006(2) 0.013(2) C26A 0.034(2) 0.032(3) 0.029(2) -0.0071(18) 0.0080(18) 0.0002(19) N11B 0.048(4) 0.032(3) 0.034(3) 0.001(2) 0.014(3) -0.004(3) C12B 0.050(5) 0.039(3) 0.040(4) -0.006(2) 0.017(4) -0.018(3) C13B 0.063(6) 0.073(6) 0.064(5) 0.005(4) 0.020(5) -0.033(5) C14B 0.100(7) 0.087(7) 0.060(6) 0.017(5) 0.013(6) -0.061(7) C15B 0.100(7) 0.068(6) 0.064(6) 0.029(5) 0.021(6) -0.024(7) C16B 0.069(6) 0.042(5) 0.041(4) 0.007(3) 0.013(4) -0.012(4) N21B 0.032(2) 0.034(2) 0.027(2) -0.0064(15) 0.0104(17) -0.0037(16) C22B 0.036(4) 0.039(3) 0.033(3) -0.010(2) 0.011(3) -0.010(2) C23B 0.036(3) 0.055(4) 0.041(4) -0.014(3) 0.008(3) -0.019(3) C24B 0.041(3) 0.063(5) 0.038(4) -0.015(3) 0.002(3) 0.008(3) C25B 0.049(3) 0.030(3) 0.020(3) -0.002(2) 0.006(2) 0.013(2) C26B 0.034(2) 0.032(3) 0.029(2) -0.0071(18) 0.0080(18) 0.0002(19) N31 0.036(2) 0.029(2) 0.039(2) -0.0040(17) 0.0204(17) -0.0002(16) C32 0.047(3) 0.028(3) 0.032(2) -0.0064(19) 0.018(2) 0.004(2) S33 0.0540(8) 0.0424(8) 0.0319(6) 0.0017(5) 0.0131(6) 0.0032(6) C34 0.048(3) 0.037(3) 0.036(3) 0.000(2) 0.021(2) 0.003(2) C35 0.041(3) 0.031(3) 0.033(2) -0.0005(18) 0.020(2) 0.0059(19) C36 0.037(2) 0.033(3) 0.039(3) 0.004(2) 0.020(2) 0.0056(19) O1 0.0379(17) 0.0324(19) 0.0346(18) 0.0061(14) 0.0164(14) 0.0070(14) N41 0.0287(18) 0.030(2) 0.0283(19) 0.0025(15) 0.0121(15) 0.0014(15) C42 0.037(2) 0.039(3) 0.030(2) 0.003(2) 0.014(2) -0.004(2) C43 0.037(2) 0.040(3) 0.026(2) 0.003(2) 0.0053(18) -0.004(2) C44 0.031(2) 0.041(3) 0.037(3) 0.006(2) 0.0107(19) -0.001(2) C45 0.029(2) 0.045(3) 0.036(3) 0.007(2) 0.0119(19) 0.005(2) C46 0.034(2) 0.034(3) 0.035(2) 0.007(2) 0.0137(19) -0.0009(19) C47 0.049(3) 0.035(3) 0.032(2) 0.003(2) 0.019(2) 0.009(2) N51 0.0321(19) 0.028(2) 0.0277(19) 0.0024(15) 0.0125(16) 0.0026(15) C52 0.040(2) 0.036(3) 0.032(2) 0.004(2) 0.018(2) 0.005(2) S53 0.0660(9) 0.0527(9) 0.0335(7) 0.0006(6) 0.0226(6) -0.0138(7) C54 0.061(3) 0.047(3) 0.049(3) 0.002(3) 0.034(3) -0.011(3) C55 0.039(2) 0.031(3) 0.038(3) 0.003(2) 0.023(2) 0.0007(19) N61 0.046(2) 0.044(3) 0.045(3) 0.004(2) 0.021(2) -0.010(2) C62 0.041(3) 0.032(3) 0.045(3) 0.005(2) 0.023(2) 0.004(2) C63 0.049(3) 0.048(4) 0.060(4) 0.014(3) 0.025(3) -0.005(3) C64 0.041(3) 0.055(4) 0.079(5) 0.016(3) 0.021(3) -0.009(3) C65 0.044(3) 0.058(4) 0.072(4) -0.003(3) 0.015(3) -0.020(3) C66 0.049(3) 0.064(4) 0.050(3) 0.007(3) 0.011(3) -0.012(3) Cl1A 0.0409(8) 0.0377(10) 0.0378(7) -0.0011(6) 0.0174(6) -0.0033(7) O1AA 0.089(6) 0.085(6) 0.047(4) 0.025(3) 0.025(4) -0.023(4) O1BA 0.050(4) 0.122(7) 0.098(6) 0.000(5) 0.029(3) 0.026(4) O1CA 0.093(6) 0.033(4) 0.081(4) -0.016(3) 0.057(5) -0.015(3) O1DA 0.053(3) 0.066(4) 0.048(3) -0.009(2) 0.020(2) -0.029(3) Cl1B 0.0409(8) 0.0377(10) 0.0378(7) -0.0011(6) 0.0174(6) -0.0033(7) O1AB 0.089(6) 0.085(6) 0.047(4) 0.025(3) 0.025(4) -0.023(4) O1BB 0.050(4) 0.122(7) 0.098(6) 0.000(5) 0.029(3) 0.026(4) O1CB 0.093(6) 0.033(4) 0.081(4) -0.016(3) 0.057(5) -0.015(3) O1DB 0.053(3) 0.066(4) 0.048(3) -0.009(2) 0.020(2) -0.029(3) Cl2 0.0654(9) 0.0572(10) 0.0496(8) 0.0092(7) 0.0303(7) 0.0300(7) O2A 0.086(4) 0.080(4) 0.078(4) -0.038(3) 0.042(3) -0.011(3) O2B 0.054(3) 0.082(4) 0.113(4) -0.026(3) 0.013(3) 0.017(3) O2C 0.171(6) 0.152(6) 0.107(5) 0.059(5) 0.108(5) 0.105(5) O2D 0.068(3) 0.072(3) 0.040(2) 0.013(2) 0.028(2) 0.034(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N51 2.173(4) 2_755 ? Hg1 N51 2.173(4) . ? Hg1 N41 2.495(4) 2_755 ? Hg1 N41 2.495(4) . ? Hg1 N61 2.671(4) . ? Hg1 N61 2.671(4) 2_755 ? Zn1 N21A 2.095(10) 2_755 ? Zn1 N21A 2.095(10) . ? Zn1 N11A 2.124(12) . ? Zn1 N11A 2.124(12) 2_755 ? Zn1 N31 2.322(11) 2_755 ? Zn1 N31 2.322(11) . ? Hg2 N21B 2.21(2) 2_755 ? Hg2 N21B 2.21(2) . ? Hg2 N31 2.282(9) 2_755 ? Hg2 N31 2.282(9) . ? Hg2 N11B 2.478(19) . ? Hg2 N11B 2.478(19) 2_755 ? N11A C16A 1.337(8) . ? N11A C12A 1.369(9) . ? C12A C13A 1.387(9) . ? C12A C22A 1.482(8) . ? C13A C14A 1.370(13) . ? C13A H13A 0.9500 . ? C14A C15A 1.367(14) . ? C14A H14A 0.9500 . ? C15A C16A 1.391(13) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? N21A C26A 1.319(7) . ? N21A C22A 1.358(7) . ? C22A C23A 1.374(8) . ? C23A C24A 1.365(9) . ? C23A H23A 0.9500 . ? C24A C25A 1.224(9) . ? C24A H24A 0.9500 . ? C25A C26A 1.472(7) . ? C25A H25A 0.9500 . ? C26A C32 1.471(10) . ? N11B C16B 1.339(11) . ? N11B C12B 1.366(11) . ? C12B C13B 1.388(12) . ? C12B C22B 1.479(9) . ? C13B C14B 1.367(15) . ? C13B H13B 0.9500 . ? C14B C15B 1.363(17) . ? C14B H14B 0.9500 . ? C15B C16B 1.392(15) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? N21B C26B 1.319(9) . ? N21B C22B 1.357(9) . ? C22B C23B 1.373(10) . ? C23B C24B 1.363(12) . ? C23B H23B 0.9500 . ? C24B C25B 1.220(11) . ? C24B H24B 0.9500 . ? C25B C26B 1.471(9) . ? C25B H25B 0.9500 . ? C26B C32 1.444(18) . ? N31 C32 1.322(6) . ? N31 C35 1.371(6) . ? C32 S33 1.695(5) . ? S33 C34 1.720(5) . ? C34 C35 1.362(7) . ? C34 H34 0.9500 . ? C35 C36 1.498(7) . ? C36 O1 1.422(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O1 C47 1.419(6) . ? N41 C46 1.328(6) . ? N41 C42 1.370(6) . ? C42 C43 1.385(7) . ? C42 C52 1.471(7) 2_755 ? C43 C44 1.337(7) . ? C43 H43 0.9500 . ? C44 C45 1.354(7) . ? C44 H44 0.9500 . ? C45 C46 1.402(6) . ? C45 H45 0.9500 . ? C46 C47 1.502(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N51 C52 1.294(6) . ? N51 C55 1.367(6) . ? C52 C42 1.471(7) 2_755 ? C52 S53 1.712(5) . ? S53 C54 1.704(6) . ? C54 C55 1.370(7) . ? C54 H54 0.9500 . ? C55 C62 1.456(7) . ? N61 C66 1.333(7) . ? N61 C62 1.336(7) . ? C62 C63 1.387(7) . ? C63 C64 1.376(9) . ? C63 H63 0.9500 . ? C64 C65 1.327(9) . ? C64 H64 0.9500 . ? C65 C66 1.391(8) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? Cl1A O1CA 1.419(11) . ? Cl1A O1DA 1.420(11) . ? Cl1A O1BA 1.422(11) . ? Cl1A O1AA 1.428(12) . ? Cl1B O1CB 1.428(4) . ? Cl1B O1DB 1.429(4) . ? Cl1B O1BB 1.432(4) . ? Cl1B O1AB 1.438(4) . ? Cl2 O2C 1.383(6) . ? Cl2 O2A 1.419(5) . ? Cl2 O2D 1.429(4) . ? Cl2 O2B 1.466(5) . ? N1 C1A 1.066(15) 2_755 ? C1A N1 1.066(15) 2_755 ? C1A C1B 1.39(2) 2_655 ? C1B C1A 1.39(2) 2_655 ? C1B H1A 0.9800 . ? C1B H1B 0.9800 . ? C1B H1C 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 N51 Hg1 N51 159.8(2) 2_755 . ? N51 Hg1 N41 122.29(13) 2_755 2_755 ? N51 Hg1 N41 70.66(13) . 2_755 ? N51 Hg1 N41 70.66(13) 2_755 . ? N51 Hg1 N41 122.29(13) . . ? N41 Hg1 N41 109.22(18) 2_755 . ? N51 Hg1 N61 103.49(14) 2_755 . ? N51 Hg1 N61 67.15(14) . . ? N41 Hg1 N61 133.93(13) 2_755 . ? N41 Hg1 N61 79.56(13) . . ? N51 Hg1 N61 67.15(14) 2_755 2_755 ? N51 Hg1 N61 103.49(14) . 2_755 ? N41 Hg1 N61 79.56(13) 2_755 2_755 ? N41 Hg1 N61 133.93(13) . 2_755 ? N61 Hg1 N61 127.5(2) . 2_755 ? N21A Zn1 N21A 175.5(9) 2_755 . ? N21A Zn1 N11A 105.6(4) 2_755 . ? N21A Zn1 N11A 77.5(3) . . ? N21A Zn1 N11A 77.5(3) 2_755 2_755 ? N21A Zn1 N11A 105.6(4) . 2_755 ? N11A Zn1 N11A 97.3(7) . 2_755 ? N21A Zn1 N31 73.0(3) 2_755 2_755 ? N21A Zn1 N31 103.9(4) . 2_755 ? N11A Zn1 N31 90.4(2) . 2_755 ? N11A Zn1 N31 150.4(2) 2_755 2_755 ? N21A Zn1 N31 103.9(4) 2_755 . ? N21A Zn1 N31 73.0(3) . . ? N11A Zn1 N31 150.4(2) . . ? N11A Zn1 N31 90.4(2) 2_755 . ? N31 Zn1 N31 96.9(6) 2_755 . ? N21B Hg2 N21B 179.2(9) 2_755 . ? N21B Hg2 N31 74.8(5) 2_755 2_755 ? N21B Hg2 N31 104.7(3) . 2_755 ? N21B Hg2 N31 104.7(3) 2_755 . ? N21B Hg2 N31 74.8(5) . . ? N31 Hg2 N31 99.2(5) 2_755 . ? N21B Hg2 N11B 111.9(6) 2_755 . ? N21B Hg2 N11B 68.6(6) . . ? N31 Hg2 N11B 92.9(3) 2_755 . ? N31 Hg2 N11B 143.2(5) . . ? N21B Hg2 N11B 68.6(6) 2_755 2_755 ? N21B Hg2 N11B 111.9(6) . 2_755 ? N31 Hg2 N11B 143.2(5) 2_755 2_755 ? N31 Hg2 N11B 92.9(3) . 2_755 ? N11B Hg2 N11B 97.8(8) . 2_755 ? C16A N11A C12A 118.7(7) . . ? C16A N11A Zn1 125.8(6) . . ? C12A N11A Zn1 115.5(4) . . ? N11A C12A C13A 120.7(7) . . ? N11A C12A C22A 115.0(5) . . ? C13A C12A C22A 124.4(7) . . ? C14A C13A C12A 119.7(9) . . ? C14A C13A H13A 120.2 . . ? C12A C13A H13A 120.2 . . ? C15A C14A C13A 119.9(8) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 118.6(8) . . ? C14A C15A H15A 120.7 . . ? C16A C15A H15A 120.7 . . ? N11A C16A C15A 122.4(9) . . ? N11A C16A H16A 118.8 . . ? C15A C16A H16A 118.8 . . ? C26A N21A C22A 119.7(5) . . ? C26A N21A Zn1 123.4(6) . . ? C22A N21A Zn1 116.8(6) . . ? N21A C22A C23A 119.9(6) . . ? N21A C22A C12A 115.2(5) . . ? C23A C22A C12A 124.9(6) . . ? C24A C23A C22A 117.8(6) . . ? C24A C23A H23A 121.1 . . ? C22A C23A H23A 121.1 . . ? C25A C24A C23A 125.5(7) . . ? C25A C24A H24A 117.3 . . ? C23A C24A H24A 117.3 . . ? C24A C25A C26A 117.3(6) . . ? C24A C25A H25A 121.3 . . ? C26A C25A H25A 121.3 . . ? N21A C26A C32 112.4(7) . . ? N21A C26A C25A 119.7(6) . . ? C32 C26A C25A 127.8(7) . . ? C16B N11B C12B 118.7(11) . . ? C16B N11B Hg2 126.3(12) . . ? C12B N11B Hg2 114.9(9) . . ? N11B C12B C13B 120.7(11) . . ? N11B C12B C22B 115.9(9) . . ? C13B C12B C22B 123.4(12) . . ? C14B C13B C12B 119.7(14) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C15B C14B C13B 119.9(13) . . ? C15B C14B H14B 120.1 . . ? C13B C14B H14B 120.1 . . ? C14B C15B C16B 118.9(13) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? N11B C16B C15B 122.1(14) . . ? N11B C16B H16B 119.0 . . ? C15B C16B H16B 119.0 . . ? C26B N21B C22B 119.1(9) . . ? C26B N21B Hg2 115.6(11) . . ? C22B N21B Hg2 125.3(9) . . ? N21B C22B C23B 120.2(9) . . ? N21B C22B C12B 115.1(9) . . ? C23B C22B C12B 124.7(11) . . ? C24B C23B C22B 117.9(11) . . ? C24B C23B H23B 121.1 . . ? C22B C23B H23B 121.1 . . ? C25B C24B C23B 125.5(12) . . ? C25B C24B H24B 117.3 . . ? C23B C24B H24B 117.3 . . ? C24B C25B C26B 117.1(11) . . ? C24B C25B H25B 121.4 . . ? C26B C25B H25B 121.4 . . ? N21B C26B C32 117.6(15) . . ? N21B C26B C25B 120.3(10) . . ? C32 C26B C25B 122.1(16) . . ? C32 N31 C35 110.9(4) . . ? C32 N31 Hg2 111.5(3) . . ? C35 N31 Hg2 137.5(3) . . ? C32 N31 Zn1 111.3(3) . . ? C35 N31 Zn1 137.7(3) . . ? Hg2 N31 Zn1 1.1(5) . . ? N31 C32 C26B 120.5(11) . . ? N31 C32 C26A 119.8(6) . . ? C26B C32 C26A 0.7(15) . . ? N31 C32 S33 114.1(4) . . ? C26B C32 S33 125.4(10) . . ? C26A C32 S33 126.0(5) . . ? C32 S33 C34 90.5(3) . . ? C35 C34 S33 109.1(4) . . ? C35 C34 H34 125.5 . . ? S33 C34 H34 125.5 . . ? C34 C35 N31 115.3(5) . . ? C34 C35 C36 125.7(5) . . ? N31 C35 C36 119.0(4) . . ? O1 C36 C35 113.6(4) . . ? O1 C36 H36A 108.8 . . ? C35 C36 H36A 108.8 . . ? O1 C36 H36B 108.8 . . ? C35 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C47 O1 C36 112.1(3) . . ? C46 N41 C42 118.4(4) . . ? C46 N41 Hg1 128.4(3) . . ? C42 N41 Hg1 109.6(3) . . ? N41 C42 C43 121.3(5) . . ? N41 C42 C52 113.4(4) . 2_755 ? C43 C42 C52 125.3(5) . 2_755 ? C44 C43 C42 119.1(5) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C44 C45 C46 119.0(5) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? N41 C46 C45 121.3(5) . . ? N41 C46 C47 116.2(4) . . ? C45 C46 C47 122.5(4) . . ? O1 C47 C46 107.5(4) . . ? O1 C47 H47A 110.2 . . ? C46 C47 H47A 110.2 . . ? O1 C47 H47B 110.2 . . ? C46 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? C52 N51 C55 114.5(4) . . ? C52 N51 Hg1 120.1(3) . . ? C55 N51 Hg1 125.3(3) . . ? N51 C52 C42 121.8(4) . 2_755 ? N51 C52 S53 112.9(4) . . ? C42 C52 S53 125.3(4) 2_755 . ? C54 S53 C52 89.5(3) . . ? C55 C54 S53 111.6(4) . . ? C55 C54 H54 124.2 . . ? S53 C54 H54 124.2 . . ? N51 C55 C54 111.4(4) . . ? N51 C55 C62 119.6(4) . . ? C54 C55 C62 129.0(4) . . ? C66 N61 C62 117.9(5) . . ? C66 N61 Hg1 130.5(4) . . ? C62 N61 Hg1 110.8(3) . . ? N61 C62 C63 121.5(5) . . ? N61 C62 C55 115.6(4) . . ? C63 C62 C55 122.9(5) . . ? C64 C63 C62 118.8(6) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C65 C64 C63 120.4(5) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 118.4(6) . . ? C64 C65 H65 120.8 . . ? C66 C65 H65 120.8 . . ? N61 C66 C65 122.9(6) . . ? N61 C66 H66 118.5 . . ? C65 C66 H66 118.5 . . ? O1CA Cl1A O1DA 109.6 . . ? O1CA Cl1A O1BA 109.8 . . ? O1DA Cl1A O1BA 109.5 . . ? O1CA Cl1A O1AA 108.9 . . ? O1DA Cl1A O1AA 109.8 . . ? O1BA Cl1A O1AA 109.3 . . ? O1CB Cl1B O1DB 109.6 . . ? O1CB Cl1B O1BB 109.8 . . ? O1DB Cl1B O1BB 109.5 . . ? O1CB Cl1B O1AB 108.9 . . ? O1DB Cl1B O1AB 109.8 . . ? O1BB Cl1B O1AB 109.2 . . ? O2C Cl2 O2A 114.4(4) . . ? O2C Cl2 O2D 111.3(3) . . ? O2A Cl2 O2D 109.0(3) . . ? O2C Cl2 O2B 106.9(5) . . ? O2A Cl2 O2B 106.1(3) . . ? O2D Cl2 O2B 108.9(3) . . ? N1 C1A C1B 178.0(17) 2_755 2_655 ? C1A C1B H1A 109.5 2_655 . ? C1A C1B H1B 109.5 2_655 . ? H1A C1B H1B 109.5 . . ? C1A C1B H1C 109.5 2_655 . ? H1A C1B H1C 109.5 . . ? H1B C1B H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.532 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.121 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.072 0.250 0.322 508.3 117.8 2 0.071 -0.250 0.821 508.3 117.8 _platon_squeeze_details ; ; # Attachment 'Zn2_helicate.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 730542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Zn2(C28H20N6S2O)2][ClO4]4.3MeCN.1Et2O' _chemical_formula_sum 'C66 H59 Cl4 N15 O19 S4 Zn2' _chemical_formula_weight 1767.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4711(7) _cell_length_b 14.3884(9) _cell_length_c 22.2744(13) _cell_angle_alpha 101.2690(10) _cell_angle_beta 97.5310(10) _cell_angle_gamma 99.0220(10) _cell_volume 3817.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88934 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'frames each covering 0.3\% in\w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67179 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 17470 _reflns_number_gt 10293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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. Complex cation: No major disorder present. Counter anions: Of the four crystallographically independent perchlorates, one was sufficiently disordered to merit modelling as two components, the population parameters of which converged at 0.58:0.42. Each component was refined with isotropic displacement parameters and no geometric restraints. Intstitial solvent: Three suspect MeCN and one Et2O molecules were located in the difference map, but owing to extensive disorder, attempts at modelling one MeCN were made. The latter was assigned two positions (population parameters refined to 0.67:0.33), which were introduced as rigid bodies. Scattering contributions from the remaining interstitial solvent was removed using the SQUEEZE routine in PLATON (A. L. Spek, Acta. Cryst., 1990, A46, C-34; PLATON -- A Multipurpose Crystallographic Tool; Utrecht University, Utrecht, The Netherlands, A. L. Spek, 2003). The additional solvates expressed in the complex formula [Zn2(L)2][ClO4]4.3MeCN.Et2O reflect the above estimates and are consistent with a residual electron density count of ca. 200 electrons per unit cell. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17470 _refine_ls_number_parameters 882 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1445 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _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 Zn1 Zn 0.84468(4) 0.82380(3) 0.62218(2) 0.03023(13) Uani 1 1 d . . . Zn2 Zn 0.61900(4) 0.59393(3) 0.84630(2) 0.02886(12) Uani 1 1 d . . . N11 N 1.0224(3) 0.8647(2) 0.62723(15) 0.0286(7) Uani 1 1 d . . . C12 C 1.0734(3) 0.7884(3) 0.61317(17) 0.0280(8) Uani 1 1 d . . . C13 C 1.1862(3) 0.8009(3) 0.6192(2) 0.0389(10) Uani 1 1 d . . . H13 H 1.2203 0.7468 0.6080 0.047 Uiso 1 1 calc R . . C14 C 1.2499(4) 0.8915(3) 0.6413(2) 0.0418(11) Uani 1 1 d . . . H14 H 1.3279 0.9007 0.6463 0.050 Uiso 1 1 calc R . . C15 C 1.1976(4) 0.9689(3) 0.6562(2) 0.0451(11) Uani 1 1 d . . . H15 H 1.2396 1.0323 0.6714 0.054 Uiso 1 1 calc R . . C16 C 1.0847(3) 0.9536(3) 0.6488(2) 0.0366(10) Uani 1 1 d . . . H16 H 1.0495 1.0071 0.6591 0.044 Uiso 1 1 calc R . . N21 N 0.8888(2) 0.6983(2) 0.59584(15) 0.0274(7) Uani 1 1 d . . . C22 C 0.8254(3) 0.6124(3) 0.58154(18) 0.0289(9) Uani 1 1 d . . . S23 S 0.89680(9) 0.52132(7) 0.56404(5) 0.0345(2) Uani 1 1 d . . . C24 C 1.0176(3) 0.6038(3) 0.57769(18) 0.0324(9) Uani 1 1 d . . . H24 H 1.0880 0.5879 0.5744 0.039 Uiso 1 1 calc R . . C25 C 0.9982(3) 0.6955(3) 0.59396(17) 0.0277(8) Uani 1 1 d . . . N31 N 0.6817(2) 0.6872(2) 0.61469(14) 0.0243(7) Uani 1 1 d . . . C32 C 0.7090(3) 0.6034(3) 0.58686(17) 0.0261(8) Uani 1 1 d . . . C33 C 0.6338(3) 0.5176(3) 0.56639(17) 0.0311(9) Uani 1 1 d . . . H33 H 0.6558 0.4607 0.5465 0.037 Uiso 1 1 calc R . . C34 C 0.5263(3) 0.5165(3) 0.57553(19) 0.0343(10) Uani 1 1 d . . . H34 H 0.4731 0.4584 0.5620 0.041 Uiso 1 1 calc R . . C35 C 0.4969(3) 0.5997(3) 0.60422(18) 0.0316(9) Uani 1 1 d . . . H35 H 0.4232 0.6001 0.6109 0.038 Uiso 1 1 calc R . . C36 C 0.5774(3) 0.6843(3) 0.62367(17) 0.0284(8) Uani 1 1 d . . . C37 C 0.5497(3) 0.7793(3) 0.65490(19) 0.0302(9) Uani 1 1 d . . . H37A H 0.6140 0.8164 0.6859 0.045 Uiso 1 1 calc R . . H37B H 0.5355 0.8177 0.6233 0.045 Uiso 1 1 calc R . . O1 O 0.4563(2) 0.76676(19) 0.68497(12) 0.0285(6) Uani 1 1 d . . . N41 N 0.6201(2) 0.7652(2) 0.83101(14) 0.0250(7) Uani 1 1 d . . . C42 C 0.6831(3) 0.8271(3) 0.88126(17) 0.0226(8) Uani 1 1 d . . . C43 C 0.6842(3) 0.9250(3) 0.89356(19) 0.0300(9) Uani 1 1 d . . . H43 H 0.7293 0.9664 0.9295 0.036 Uiso 1 1 calc R . . C44 C 0.6189(3) 0.9618(3) 0.85284(19) 0.0327(9) Uani 1 1 d . . . H44 H 0.6189 1.0291 0.8599 0.039 Uiso 1 1 calc R . . C45 C 0.5539(3) 0.8997(3) 0.80184(19) 0.0323(9) Uani 1 1 d . . . H45 H 0.5078 0.9238 0.7735 0.039 Uiso 1 1 calc R . . C46 C 0.5555(3) 0.8011(3) 0.79166(17) 0.0256(8) Uani 1 1 d . . . C47 C 0.4788(3) 0.7285(3) 0.73944(18) 0.0305(9) Uani 1 1 d . . . H47A H 0.5122 0.6707 0.7286 0.046 Uiso 1 1 calc R . . H47B H 0.4086 0.7082 0.7537 0.046 Uiso 1 1 calc R . . N51 N 0.7267(2) 0.6856(2) 0.91309(14) 0.0235(7) Uani 1 1 d . . . C52 C 0.7457(3) 0.7801(3) 0.92266(17) 0.0261(8) Uani 1 1 d . . . S53 S 0.84434(8) 0.83274(7) 0.98676(5) 0.0335(2) Uani 1 1 d . . . C54 C 0.8566(3) 0.7213(3) 0.99999(19) 0.0322(9) Uani 1 1 d . . . H54 H 0.9054 0.7101 1.0332 0.039 Uiso 1 1 calc R . . C55 C 0.7870(3) 0.6513(3) 0.95637(17) 0.0255(8) Uani 1 1 d . . . N61 N 0.6853(3) 0.4993(2) 0.89948(15) 0.0285(7) Uani 1 1 d . . . C62 C 0.7655(3) 0.5454(3) 0.94809(19) 0.0292(9) Uani 1 1 d . . . C63 C 0.8191(4) 0.4967(3) 0.9859(2) 0.0449(11) Uani 1 1 d . . . H63 H 0.8757 0.5305 1.0193 0.054 Uiso 1 1 calc R . . C64 C 0.7891(4) 0.3970(4) 0.9743(2) 0.0530(13) Uani 1 1 d . . . H64 H 0.8247 0.3616 1.0000 0.064 Uiso 1 1 calc R . . C65 C 0.7076(5) 0.3500(3) 0.9254(3) 0.0555(14) Uani 1 1 d . . . H65 H 0.6858 0.2818 0.9169 0.067 Uiso 1 1 calc R . . C66 C 0.6587(4) 0.4029(3) 0.8894(2) 0.0388(10) Uani 1 1 d . . . H66 H 0.6028 0.3698 0.8554 0.047 Uiso 1 1 calc R . . N71 N 0.7618(3) 0.8627(2) 0.54338(15) 0.0282(7) Uani 1 1 d . . . C72 C 0.7080(3) 0.9377(3) 0.55724(18) 0.0265(8) Uani 1 1 d . . . C73 C 0.6487(3) 0.9711(3) 0.51188(18) 0.0280(8) Uani 1 1 d . . . H73 H 0.6119 1.0235 0.5226 0.034 Uiso 1 1 calc R . . C74 C 0.6443(3) 0.9269(3) 0.4510(2) 0.0362(10) Uani 1 1 d . . . H74 H 0.6036 0.9484 0.4190 0.043 Uiso 1 1 calc R . . C75 C 0.6982(4) 0.8518(3) 0.4361(2) 0.0397(11) Uani 1 1 d . . . H75 H 0.6962 0.8215 0.3939 0.048 Uiso 1 1 calc R . . C76 C 0.7556(4) 0.8208(3) 0.48357(19) 0.0346(9) Uani 1 1 d . . . H76 H 0.7919 0.7679 0.4733 0.042 Uiso 1 1 calc R . . N81 N 0.7880(2) 0.9382(2) 0.66167(15) 0.0252(7) Uani 1 1 d . . . C82 C 0.8014(3) 0.9791(3) 0.72073(18) 0.0251(8) Uani 1 1 d . . . S83 S 0.72980(10) 1.07153(8) 0.73419(5) 0.0383(3) Uani 1 1 d . . . C84 C 0.6841(3) 1.0538(3) 0.65633(19) 0.0340(9) Uani 1 1 d . . . H84 H 0.6377 1.0908 0.6381 0.041 Uiso 1 1 calc R . . C85 C 0.7229(3) 0.9799(3) 0.62420(18) 0.0273(8) Uani 1 1 d . . . N91 N 0.8956(2) 0.8572(2) 0.74287(14) 0.0264(7) Uani 1 1 d . . . C92 C 0.8674(3) 0.9424(3) 0.76641(18) 0.0272(8) Uani 1 1 d . . . C93 C 0.8990(3) 0.9905(3) 0.82762(18) 0.0319(9) Uani 1 1 d . . . H93 H 0.8781 1.0506 0.8421 0.038 Uiso 1 1 calc R . . C94 C 0.9621(3) 0.9495(3) 0.86772(19) 0.0325(9) Uani 1 1 d . . . H94 H 0.9843 0.9805 0.9103 0.039 Uiso 1 1 calc R . . C95 C 0.9918(3) 0.8623(3) 0.84426(19) 0.0306(9) Uani 1 1 d . . . H95 H 1.0354 0.8329 0.8705 0.037 Uiso 1 1 calc R . . C96 C 0.9570(3) 0.8185(3) 0.78178(18) 0.0258(8) Uani 1 1 d . . . C97 C 0.9888(3) 0.7249(3) 0.75326(19) 0.0321(9) Uani 1 1 d . . . H97A H 0.9275 0.6867 0.7207 0.048 Uiso 1 1 calc R . . H97B H 1.0537 0.7392 0.7331 0.048 Uiso 1 1 calc R . . O2 O 1.0138(2) 0.66893(19) 0.79716(12) 0.0302(6) Uani 1 1 d . . . N101 N 0.7405(3) 0.5291(2) 0.76739(14) 0.0304(8) Uani 1 1 d . . . C102 C 0.6764(4) 0.4542(3) 0.72416(19) 0.0367(10) Uani 1 1 d . . . C103 C 0.7181(5) 0.3918(3) 0.6818(2) 0.0519(14) Uani 1 1 d . . . H103 H 0.6709 0.3393 0.6529 0.062 Uiso 1 1 calc R . . C104 C 0.8304(5) 0.4082(3) 0.6827(2) 0.0514(14) Uani 1 1 d . . . H104 H 0.8616 0.3674 0.6537 0.062 Uiso 1 1 calc R . . C105 C 0.8974(4) 0.4842(3) 0.7259(2) 0.0429(11) Uani 1 1 d . . . H105 H 0.9748 0.4962 0.7270 0.051 Uiso 1 1 calc R . . C106 C 0.8491(4) 0.5430(3) 0.76800(18) 0.0323(9) Uani 1 1 d . . . C107 C 0.9189(3) 0.6260(3) 0.81770(19) 0.0344(9) Uani 1 1 d . . . H07A H 0.8740 0.6755 0.8294 0.052 Uiso 1 1 calc R . . H07B H 0.9421 0.6018 0.8551 0.052 Uiso 1 1 calc R . . N111 N 0.5278(3) 0.5033(2) 0.77347(17) 0.0362(8) Uani 1 1 d . . . C112 C 0.5595(4) 0.4469(3) 0.7282(2) 0.0420(11) Uani 1 1 d . . . S113 S 0.45116(14) 0.37123(10) 0.67766(6) 0.0672(5) Uani 1 1 d . . . C114 C 0.3618(4) 0.4198(4) 0.7213(2) 0.0581(15) Uani 1 1 d . . . H114 H 0.2840 0.4002 0.7118 0.070 Uiso 1 1 calc R . . C115 C 0.4152(4) 0.4892(3) 0.7707(2) 0.0481(13) Uani 1 1 d . . . N121 N 0.4571(3) 0.6069(3) 0.86396(18) 0.0369(8) Uani 1 1 d . . . C122 C 0.3760(3) 0.5526(3) 0.8203(2) 0.0434(12) Uani 1 1 d . . . C123 C 0.2670(4) 0.5626(5) 0.8191(3) 0.0687(18) Uani 1 1 d . . . H123 H 0.2107 0.5238 0.7872 0.082 Uiso 1 1 calc R . . C124 C 0.2431(5) 0.6296(5) 0.8651(4) 0.0741(19) Uani 1 1 d . . . H124 H 0.1689 0.6369 0.8659 0.089 Uiso 1 1 calc R . . C125 C 0.3245(4) 0.6864(4) 0.9102(3) 0.0658(17) Uani 1 1 d . . . H125 H 0.3080 0.7339 0.9419 0.079 Uiso 1 1 calc R . . C126 C 0.4319(4) 0.6732(3) 0.9086(2) 0.0464(12) Uani 1 1 d . . . H126 H 0.4892 0.7121 0.9400 0.056 Uiso 1 1 calc R . . Cl1A Cl 0.14421(8) 0.84297(7) 0.00985(5) 0.0313(2) Uani 1 1 d . . . O1A O 0.1193(2) 0.93032(19) -0.00551(14) 0.0419(8) Uani 1 1 d . . . O2A O 0.0931(3) 0.8248(2) 0.06177(14) 0.0494(9) Uani 1 1 d . . . O3A O 0.2619(2) 0.8520(2) 0.02622(16) 0.0461(8) Uani 1 1 d . . . O4A O 0.1025(2) 0.76371(19) -0.04273(13) 0.0335(6) Uani 1 1 d . . . Cl1B Cl 0.39138(9) 0.76328(7) 0.48685(5) 0.0340(2) Uani 1 1 d . . . O1B O 0.3741(3) 0.7985(2) 0.43056(14) 0.0562(10) Uani 1 1 d . . . O2B O 0.4095(3) 0.8438(2) 0.53858(13) 0.0420(7) Uani 1 1 d . . . O3B O 0.4851(3) 0.7171(2) 0.48729(15) 0.0458(8) Uani 1 1 d . . . O4B O 0.2963(3) 0.6949(2) 0.48985(18) 0.0546(9) Uani 1 1 d . . . Cl1C Cl 0.13959(9) 0.40156(7) 0.60703(5) 0.0363(2) Uani 1 1 d . . . O1C O 0.2309(3) 0.4447(4) 0.5849(2) 0.0869(14) Uani 1 1 d . . . O2C O 0.1189(4) 0.4619(3) 0.66046(17) 0.0835(15) Uani 1 1 d . . . O3C O 0.1610(3) 0.3137(2) 0.62312(17) 0.0699(12) Uani 1 1 d . . . O4C O 0.0454(3) 0.3815(2) 0.55902(15) 0.0548(9) Uani 1 1 d . . . Cl1D Cl 0.4948(3) 0.1836(3) 0.76305(16) 0.0325(9) Uiso 0.419(7) 1 d P A 1 O1D O 0.4360(6) 0.2538(6) 0.7883(4) 0.048(2) Uiso 0.419(7) 1 d P A 1 O2D O 0.5912(8) 0.2259(7) 0.7541(5) 0.041(3) Uiso 0.419(7) 1 d P A 1 O3D O 0.4974(9) 0.1188(9) 0.8035(5) 0.072(3) Uiso 0.419(7) 1 d P A 1 O4D O 0.4234(9) 0.1340(8) 0.7039(6) 0.090(4) Uiso 0.419(7) 1 d P A 1 Cl1E Cl 0.4820(2) 0.1567(2) 0.75681(12) 0.0367(7) Uiso 0.581(7) 1 d P A 2 O1E O 0.3869(5) 0.2014(5) 0.7506(3) 0.059(2) Uiso 0.581(7) 1 d P A 2 O2E O 0.5770(6) 0.2139(5) 0.7356(4) 0.0408(19) Uiso 0.581(7) 1 d P A 2 O3E O 0.5227(6) 0.1553(5) 0.8226(3) 0.057(2) Uiso 0.581(7) 1 d P A 2 O4E O 0.4587(5) 0.0650(4) 0.7197(3) 0.0514(19) Uiso 0.581(7) 1 d P A 2 N1F N 0.9358(6) 0.1466(5) 0.6502(4) 0.079(3) Uiso 0.672(7) 1 d PG B 1 C1F C 0.9214(4) 0.1515(3) 0.5991(3) 0.056(2) Uiso 0.672(7) 1 d PG B 1 C2F C 0.9033(7) 0.1594(6) 0.5338(4) 0.056(2) Uiso 0.672(7) 1 d PG B 1 H1F H 0.9222 0.1037 0.5092 0.084 Uiso 0.672(7) 1 d PG B 1 H2F H 0.9460 0.2176 0.5286 0.084 Uiso 0.672(7) 1 d PG B 1 H3F H 0.8275 0.1614 0.5212 0.084 Uiso 0.672(7) 1 d PG B 1 N1G N 0.9799(12) 0.0370(10) 0.5166(6) 0.079(5) Uiso 0.328(7) 1 d PG . 2 C1G C 0.9385(8) 0.0968(7) 0.5330(4) 0.043(4) Uiso 0.328(7) 1 d PG B 2 C2G C 0.8857(16) 0.1738(13) 0.5533(9) 0.070(6) Uiso 0.328(7) 1 d PG B 2 H1G H 0.8378 0.1544 0.5783 0.104 Uiso 0.328(7) 1 d PG B 2 H2G H 0.8499 0.1921 0.5203 0.104 Uiso 0.328(7) 1 d PG B 2 H3G H 0.9371 0.2260 0.5753 0.104 Uiso 0.328(7) 1 d PG B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0320(3) 0.0271(2) 0.0336(3) 0.0074(2) 0.0043(2) 0.01160(19) Zn2 0.0240(2) 0.0301(2) 0.0303(3) 0.00610(19) -0.00074(18) 0.00376(18) N11 0.0297(17) 0.0295(17) 0.0293(18) 0.0105(14) 0.0059(14) 0.0074(14) C12 0.032(2) 0.033(2) 0.023(2) 0.0100(16) 0.0103(16) 0.0077(16) C13 0.030(2) 0.052(3) 0.041(3) 0.016(2) 0.0153(19) 0.011(2) C14 0.027(2) 0.056(3) 0.044(3) 0.017(2) 0.0115(19) 0.001(2) C15 0.040(3) 0.040(3) 0.052(3) 0.012(2) 0.005(2) -0.005(2) C16 0.039(2) 0.033(2) 0.038(2) 0.0117(19) 0.0091(19) 0.0018(18) N21 0.0254(17) 0.0315(17) 0.0262(18) 0.0069(14) 0.0068(13) 0.0054(13) C22 0.036(2) 0.0256(19) 0.024(2) 0.0034(16) 0.0023(17) 0.0072(16) S23 0.0461(6) 0.0295(5) 0.0313(6) 0.0069(4) 0.0098(5) 0.0142(5) C24 0.038(2) 0.039(2) 0.024(2) 0.0065(17) 0.0078(17) 0.0167(18) C25 0.032(2) 0.034(2) 0.021(2) 0.0084(16) 0.0109(16) 0.0102(17) N31 0.0247(16) 0.0243(16) 0.0254(17) 0.0084(13) 0.0033(13) 0.0066(13) C32 0.033(2) 0.0272(19) 0.0162(18) 0.0040(15) 0.0010(15) 0.0054(16) C33 0.042(2) 0.030(2) 0.018(2) 0.0031(16) 0.0006(17) 0.0026(17) C34 0.036(2) 0.032(2) 0.028(2) 0.0087(18) -0.0081(18) -0.0070(18) C35 0.027(2) 0.041(2) 0.026(2) 0.0132(18) 0.0004(16) 0.0000(17) C36 0.034(2) 0.035(2) 0.0195(19) 0.0130(16) 0.0025(16) 0.0071(17) C37 0.028(2) 0.034(2) 0.031(2) 0.0139(17) 0.0037(17) 0.0028(16) O1 0.0237(13) 0.0389(15) 0.0267(14) 0.0157(12) 0.0037(11) 0.0069(11) N41 0.0208(15) 0.0311(17) 0.0246(17) 0.0081(13) 0.0035(13) 0.0071(13) C42 0.0195(18) 0.0282(19) 0.0217(19) 0.0075(15) 0.0060(14) 0.0051(14) C43 0.034(2) 0.029(2) 0.028(2) 0.0067(17) 0.0052(17) 0.0081(17) C44 0.038(2) 0.029(2) 0.036(2) 0.0137(18) 0.0084(19) 0.0112(17) C45 0.033(2) 0.040(2) 0.032(2) 0.0157(19) 0.0114(18) 0.0159(18) C46 0.0243(19) 0.033(2) 0.0220(19) 0.0109(16) 0.0035(15) 0.0072(16) C47 0.034(2) 0.035(2) 0.024(2) 0.0157(17) 0.0014(17) 0.0012(17) N51 0.0219(16) 0.0243(16) 0.0262(17) 0.0079(13) 0.0036(13) 0.0072(12) C52 0.0250(19) 0.0277(19) 0.027(2) 0.0089(16) 0.0056(16) 0.0027(15) S53 0.0328(5) 0.0313(5) 0.0331(6) 0.0086(4) -0.0032(4) 0.0015(4) C54 0.030(2) 0.038(2) 0.031(2) 0.0134(18) 0.0001(17) 0.0103(17) C55 0.0202(18) 0.034(2) 0.026(2) 0.0137(17) 0.0045(15) 0.0082(15) N61 0.0243(17) 0.0261(16) 0.0370(19) 0.0168(14) -0.0012(14) 0.0032(13) C62 0.028(2) 0.033(2) 0.032(2) 0.0141(17) 0.0113(17) 0.0101(16) C63 0.052(3) 0.044(3) 0.041(3) 0.013(2) 0.000(2) 0.018(2) C64 0.065(3) 0.047(3) 0.055(3) 0.027(2) 0.002(3) 0.020(3) C65 0.069(4) 0.033(2) 0.068(4) 0.025(2) 0.002(3) 0.011(2) C66 0.041(2) 0.030(2) 0.047(3) 0.018(2) 0.005(2) 0.0024(18) N71 0.0310(18) 0.0277(17) 0.0259(18) 0.0082(14) 0.0003(14) 0.0058(14) C72 0.0227(19) 0.0251(19) 0.030(2) 0.0055(16) 0.0038(16) 0.0019(15) C73 0.028(2) 0.0245(19) 0.031(2) 0.0133(17) 0.0000(17) 0.0007(15) C74 0.037(2) 0.033(2) 0.036(2) 0.0167(19) -0.0035(19) -0.0030(18) C75 0.052(3) 0.028(2) 0.033(2) 0.0069(18) 0.001(2) -0.0062(19) C76 0.045(2) 0.029(2) 0.027(2) 0.0066(17) 0.0006(18) 0.0035(18) N81 0.0256(16) 0.0238(16) 0.0285(18) 0.0079(13) 0.0069(13) 0.0068(13) C82 0.0263(19) 0.0244(18) 0.028(2) 0.0095(16) 0.0083(16) 0.0080(15) S83 0.0514(7) 0.0404(6) 0.0314(6) 0.0115(5) 0.0122(5) 0.0249(5) C84 0.043(2) 0.039(2) 0.029(2) 0.0156(18) 0.0102(18) 0.0216(19) C85 0.028(2) 0.029(2) 0.028(2) 0.0126(16) 0.0066(16) 0.0068(16) N91 0.0262(17) 0.0297(17) 0.0252(17) 0.0077(14) 0.0051(13) 0.0085(13) C92 0.028(2) 0.0258(19) 0.028(2) 0.0091(16) 0.0046(16) 0.0032(15) C93 0.034(2) 0.034(2) 0.029(2) 0.0058(18) 0.0101(18) 0.0092(17) C94 0.031(2) 0.035(2) 0.029(2) 0.0043(18) 0.0030(17) 0.0035(17) C95 0.028(2) 0.038(2) 0.030(2) 0.0126(18) 0.0048(17) 0.0088(17) C96 0.0242(19) 0.0287(19) 0.028(2) 0.0106(16) 0.0085(16) 0.0076(15) C97 0.038(2) 0.034(2) 0.030(2) 0.0143(18) 0.0069(18) 0.0154(18) O2 0.0323(15) 0.0359(15) 0.0299(15) 0.0155(12) 0.0096(12) 0.0153(12) N101 0.045(2) 0.0268(17) 0.0190(17) 0.0063(13) 0.0005(14) 0.0074(15) C102 0.059(3) 0.023(2) 0.026(2) 0.0082(17) -0.002(2) 0.0031(19) C103 0.095(4) 0.036(2) 0.022(2) 0.0064(19) 0.008(2) 0.006(3) C104 0.098(4) 0.037(3) 0.027(2) 0.009(2) 0.023(3) 0.020(3) C105 0.061(3) 0.044(3) 0.031(2) 0.012(2) 0.017(2) 0.019(2) C106 0.051(3) 0.028(2) 0.024(2) 0.0100(17) 0.0114(18) 0.0125(18) C107 0.040(2) 0.036(2) 0.029(2) 0.0092(18) 0.0106(18) 0.0084(18) N111 0.036(2) 0.0260(17) 0.044(2) 0.0142(16) -0.0065(16) 0.0009(15) C112 0.060(3) 0.026(2) 0.033(2) 0.0139(19) -0.010(2) -0.007(2) S113 0.0909(11) 0.0515(8) 0.0374(7) 0.0157(6) -0.0256(7) -0.0293(7) C114 0.050(3) 0.070(3) 0.045(3) 0.030(3) -0.018(2) -0.017(3) C115 0.032(2) 0.046(3) 0.062(3) 0.034(2) -0.022(2) -0.010(2) N121 0.0248(18) 0.043(2) 0.050(2) 0.0265(18) 0.0047(16) 0.0095(15) C122 0.025(2) 0.047(3) 0.065(3) 0.037(2) -0.001(2) 0.0043(19) C123 0.024(3) 0.085(4) 0.104(5) 0.059(4) -0.010(3) 0.002(3) C124 0.035(3) 0.089(5) 0.122(6) 0.061(4) 0.019(3) 0.031(3) C125 0.041(3) 0.080(4) 0.103(5) 0.053(4) 0.033(3) 0.033(3) C126 0.038(3) 0.050(3) 0.064(3) 0.028(3) 0.021(2) 0.016(2) Cl1A 0.0310(5) 0.0274(5) 0.0348(5) 0.0089(4) -0.0025(4) 0.0078(4) O1A 0.0479(18) 0.0287(15) 0.0468(19) 0.0112(13) -0.0131(14) 0.0137(13) O2A 0.057(2) 0.0518(19) 0.0289(17) 0.0030(15) 0.0014(15) -0.0090(16) O3A 0.0306(16) 0.0373(17) 0.068(2) 0.0150(16) -0.0069(15) 0.0087(13) O4A 0.0393(16) 0.0277(14) 0.0319(16) 0.0035(12) 0.0011(13) 0.0097(12) Cl1B 0.0447(6) 0.0291(5) 0.0290(5) 0.0087(4) 0.0029(4) 0.0086(4) O1B 0.105(3) 0.0352(17) 0.0263(17) 0.0118(14) -0.0051(18) 0.0141(18) O2B 0.059(2) 0.0376(16) 0.0278(16) 0.0058(13) -0.0008(14) 0.0107(14) O3B 0.0484(19) 0.0377(17) 0.058(2) 0.0167(15) 0.0157(16) 0.0155(14) O4B 0.0413(19) 0.0376(18) 0.082(3) 0.0080(17) 0.0127(18) 0.0049(14) Cl1C 0.0388(6) 0.0400(6) 0.0311(5) 0.0057(4) 0.0009(4) 0.0175(4) O1C 0.046(2) 0.139(4) 0.077(3) 0.054(3) 0.007(2) -0.015(2) O2C 0.100(3) 0.111(3) 0.039(2) -0.017(2) -0.008(2) 0.076(3) O3C 0.101(3) 0.042(2) 0.056(2) 0.0127(17) -0.030(2) 0.015(2) O4C 0.053(2) 0.064(2) 0.0411(19) 0.0104(17) -0.0170(16) 0.0142(17) _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 Zn1 N21 1.972(3) . ? Zn1 N81 1.986(3) . ? Zn1 N71 2.134(3) . ? Zn1 N11 2.184(3) . ? Zn2 N111 1.962(3) . ? Zn2 N51 1.977(3) . ? Zn2 N121 2.136(3) . ? Zn2 N61 2.161(3) . ? N11 C16 1.350(5) . ? N11 C12 1.359(5) . ? C12 C13 1.376(5) . ? C12 C25 1.458(5) . ? C13 C14 1.377(6) . ? C13 H13 0.9500 . ? C14 C15 1.384(6) . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C22 1.315(5) . ? N21 C25 1.377(5) . ? C22 C32 1.459(5) . ? C22 S23 1.709(4) . ? S23 C24 1.717(4) . ? C24 C25 1.366(5) . ? C24 H24 0.9500 . ? N31 C36 1.337(5) . ? N31 C32 1.359(4) . ? C32 C33 1.384(5) . ? C33 C34 1.381(6) . ? C33 H33 0.9500 . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 C36 1.406(5) . ? C35 H35 0.9500 . ? C36 C37 1.520(5) . ? C37 O1 1.423(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O1 C47 1.440(5) . ? N41 C46 1.345(5) . ? N41 C42 1.351(5) . ? C42 C43 1.379(5) . ? C42 C52 1.462(5) . ? C43 C44 1.377(6) . ? C43 H43 0.9500 . ? C44 C45 1.371(6) . ? C44 H44 0.9500 . ? C45 C46 1.396(5) . ? C45 H45 0.9500 . ? C46 C47 1.510(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? N51 C52 1.313(5) . ? N51 C55 1.360(5) . ? C52 S53 1.718(4) . ? S53 C54 1.712(4) . ? C54 C55 1.355(5) . ? C54 H54 0.9500 . ? C55 C62 1.475(5) . ? N61 C66 1.341(5) . ? N61 C62 1.357(5) . ? C62 C63 1.370(6) . ? C63 C64 1.388(6) . ? C63 H63 0.9500 . ? C64 C65 1.372(7) . ? C64 H64 0.9500 . ? C65 C66 1.361(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? N71 C76 1.338(5) . ? N71 C72 1.364(5) . ? C72 C73 1.380(5) . ? C72 C85 1.471(5) . ? C73 C74 1.370(6) . ? C73 H73 0.9500 . ? C74 C75 1.371(6) . ? C74 H74 0.9500 . ? C75 C76 1.384(6) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? N81 C82 1.309(5) . ? N81 C85 1.374(5) . ? C82 C92 1.456(5) . ? C82 S83 1.715(4) . ? S83 C84 1.709(4) . ? C84 C85 1.354(5) . ? C84 H84 0.9500 . ? N91 C96 1.340(5) . ? N91 C92 1.354(5) . ? C92 C93 1.378(5) . ? C93 C94 1.390(6) . ? C93 H93 0.9500 . ? C94 C95 1.387(5) . ? C94 H94 0.9500 . ? C95 C96 1.391(5) . ? C95 H95 0.9500 . ? C96 C97 1.508(5) . ? C97 O2 1.417(5) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? O2 C107 1.419(5) . ? N101 C106 1.335(5) . ? N101 C102 1.360(5) . ? C102 C103 1.382(6) . ? C102 C112 1.461(7) . ? C103 C104 1.380(7) . ? C103 H103 0.9500 . ? C104 C105 1.382(7) . ? C104 H104 0.9500 . ? C105 C106 1.399(6) . ? C105 H105 0.9500 . ? C106 C107 1.521(6) . ? C107 H07A 0.9900 . ? C107 H07B 0.9900 . ? N111 C112 1.310(6) . ? N111 C115 1.379(6) . ? C112 S113 1.715(4) . ? S113 C114 1.713(6) . ? C114 C115 1.350(7) . ? C114 H114 0.9500 . ? C115 C122 1.476(7) . ? N121 C122 1.333(6) . ? N121 C126 1.343(6) . ? C122 C123 1.387(7) . ? C123 C124 1.361(9) . ? C123 H123 0.9500 . ? C124 C125 1.363(9) . ? C124 H124 0.9500 . ? C125 C126 1.385(6) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? Cl1A O1A 1.434(3) . ? Cl1A O4A 1.440(3) . ? Cl1A O2A 1.439(3) . ? Cl1A O3A 1.443(3) . ? Cl1B O2B 1.432(3) . ? Cl1B O3B 1.432(3) . ? Cl1B O4B 1.435(3) . ? Cl1B O1B 1.445(3) . ? Cl1C O1C 1.404(4) . ? Cl1C O2C 1.408(3) . ? Cl1C O4C 1.432(3) . ? Cl1C O3C 1.434(4) . ? Cl1D O2D 1.318(10) . ? Cl1D O1D 1.411(8) . ? Cl1D O4D 1.472(12) . ? Cl1D O3D 1.419(12) . ? Cl1E O4E 1.378(6) . ? Cl1E O1E 1.438(7) . ? Cl1E O2E 1.516(7) . ? Cl1E O3E 1.493(8) . ? N1F C1F 1.148(6) . ? C1F C2F 1.471(7) . ? C1F H1G 1.0938 . ? C1F H3G 1.2845 . ? C2F H1F 0.9584 . ? C2F H2F 0.9549 . ? C2F H3F 0.9576 . ? C2F H1G 1.3708 . ? C2F H2G 0.9258 . ? C2F H3G 1.1734 . ? N1G C1G 1.098(11) . ? N1G N1G 1.37(3) 2_756 ? N1G H1F 1.3095 . ? C1G C2G 1.407(14) . ? C1G H1F 0.5772 . ? C2G H1F 1.4370 . ? C2G H2F 1.1668 . ? C2G H3F 0.9188 . ? C2G H1G 0.9167 . ? C2G H2G 0.9133 . ? C2G H3G 0.9159 . ? 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 N21 Zn1 N81 168.48(13) . . ? N21 Zn1 N71 109.42(13) . . ? N81 Zn1 N71 78.26(13) . . ? N21 Zn1 N11 77.42(12) . . ? N81 Zn1 N11 108.67(12) . . ? N71 Zn1 N11 109.35(12) . . ? N111 Zn2 N51 172.44(14) . . ? N111 Zn2 N121 78.66(15) . . ? N51 Zn2 N121 108.41(13) . . ? N111 Zn2 N61 102.77(13) . . ? N51 Zn2 N61 77.64(12) . . ? N121 Zn2 N61 110.00(13) . . ? C16 N11 C12 118.7(3) . . ? C16 N11 Zn1 127.1(3) . . ? C12 N11 Zn1 113.7(2) . . ? N11 C12 C13 121.1(4) . . ? N11 C12 C25 113.8(3) . . ? C13 C12 C25 125.0(4) . . ? C12 C13 C14 120.1(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 118.5(4) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N11 C16 C15 121.9(4) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C22 N21 C25 113.3(3) . . ? C22 N21 Zn1 127.4(3) . . ? C25 N21 Zn1 119.3(2) . . ? N21 C22 C32 119.5(3) . . ? N21 C22 S23 112.8(3) . . ? C32 C22 S23 127.5(3) . . ? C22 S23 C24 90.40(19) . . ? C25 C24 S23 110.5(3) . . ? C25 C24 H24 124.8 . . ? S23 C24 H24 124.8 . . ? C24 C25 N21 113.0(4) . . ? C24 C25 C12 131.2(4) . . ? N21 C25 C12 115.7(3) . . ? C36 N31 C32 117.4(3) . . ? N31 C32 C33 123.1(4) . . ? N31 C32 C22 113.5(3) . . ? C33 C32 C22 123.4(3) . . ? C34 C33 C32 118.6(4) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C35 C34 C33 119.5(4) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 118.9(4) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? N31 C36 C35 122.5(4) . . ? N31 C36 C37 115.9(3) . . ? C35 C36 C37 121.6(4) . . ? O1 C37 C36 112.9(3) . . ? O1 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? O1 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 O1 C47 112.0(3) . . ? C46 N41 C42 118.2(3) . . ? N41 C42 C43 122.9(4) . . ? N41 C42 C52 113.7(3) . . ? C43 C42 C52 123.3(3) . . ? C44 C43 C42 118.9(4) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C45 C44 C43 118.9(4) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? N41 C46 C45 121.2(4) . . ? N41 C46 C47 116.4(3) . . ? C45 C46 C47 122.2(4) . . ? O1 C47 C46 112.2(3) . . ? O1 C47 H47A 109.2 . . ? C46 C47 H47A 109.2 . . ? O1 C47 H47B 109.2 . . ? C46 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C52 N51 C55 113.6(3) . . ? C52 N51 Zn2 126.9(3) . . ? C55 N51 Zn2 119.4(2) . . ? N51 C52 C42 119.6(3) . . ? N51 C52 S53 112.0(3) . . ? C42 C52 S53 128.4(3) . . ? C54 S53 C52 90.26(19) . . ? C55 C54 S53 110.4(3) . . ? C55 C54 H54 124.8 . . ? S53 C54 H54 124.8 . . ? C54 C55 N51 113.7(3) . . ? C54 C55 C62 131.2(4) . . ? N51 C55 C62 115.1(3) . . ? C66 N61 C62 117.7(4) . . ? C66 N61 Zn2 128.3(3) . . ? C62 N61 Zn2 114.0(2) . . ? N61 C62 C63 122.1(4) . . ? N61 C62 C55 113.7(3) . . ? C63 C62 C55 124.2(4) . . ? C62 C63 C64 118.7(5) . . ? C62 C63 H63 120.7 . . ? C64 C63 H63 120.7 . . ? C65 C64 C63 119.4(5) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C66 C65 C64 118.7(5) . . ? C66 C65 H65 120.6 . . ? C64 C65 H65 120.6 . . ? N61 C66 C65 123.4(4) . . ? N61 C66 H66 118.3 . . ? C65 C66 H66 118.3 . . ? C76 N71 C72 118.1(3) . . ? C76 N71 Zn1 127.3(3) . . ? C72 N71 Zn1 114.6(3) . . ? N71 C72 C73 122.2(4) . . ? N71 C72 C85 113.4(3) . . ? C73 C72 C85 124.4(3) . . ? C74 C73 C72 118.3(4) . . ? C74 C73 H73 120.8 . . ? C72 C73 H73 120.8 . . ? C73 C74 C75 120.4(4) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C74 C75 C76 118.7(4) . . ? C74 C75 H75 120.6 . . ? C76 C75 H75 120.6 . . ? N71 C76 C75 122.3(4) . . ? N71 C76 H76 118.9 . . ? C75 C76 H76 118.9 . . ? C82 N81 C85 113.7(3) . . ? C82 N81 Zn1 128.2(3) . . ? C85 N81 Zn1 118.1(2) . . ? N81 C82 C92 120.2(3) . . ? N81 C82 S83 112.1(3) . . ? C92 C82 S83 127.6(3) . . ? C84 S83 C82 90.36(19) . . ? C85 C84 S83 110.8(3) . . ? C85 C84 H84 124.6 . . ? S83 C84 H84 124.6 . . ? C84 C85 N81 113.0(3) . . ? C84 C85 C72 131.5(4) . . ? N81 C85 C72 115.4(3) . . ? C96 N91 C92 117.5(3) . . ? N91 C92 C93 123.4(4) . . ? N91 C92 C82 113.6(3) . . ? C93 C92 C82 123.0(3) . . ? C92 C93 C94 118.7(4) . . ? C92 C93 H93 120.7 . . ? C94 C93 H93 120.7 . . ? C95 C94 C93 118.6(4) . . ? C95 C94 H94 120.7 . . ? C93 C94 H94 120.7 . . ? C94 C95 C96 119.2(4) . . ? C94 C95 H95 120.4 . . ? C96 C95 H95 120.4 . . ? N91 C96 C95 122.6(3) . . ? N91 C96 C97 115.7(3) . . ? C95 C96 C97 121.6(4) . . ? O2 C97 C96 113.0(3) . . ? O2 C97 H97A 109.0 . . ? C96 C97 H97A 109.0 . . ? O2 C97 H97B 109.0 . . ? C96 C97 H97B 109.0 . . ? H97A C97 H97B 107.8 . . ? C97 O2 C107 112.8(3) . . ? C106 N101 C102 117.7(3) . . ? N101 C102 C103 123.4(5) . . ? N101 C102 C112 112.4(4) . . ? C103 C102 C112 124.2(4) . . ? C104 C103 C102 117.9(4) . . ? C104 C103 H103 121.0 . . ? C102 C103 H103 121.0 . . ? C103 C104 C105 119.9(4) . . ? C103 C104 H104 120.1 . . ? C105 C104 H104 120.1 . . ? C104 C105 C106 118.8(5) . . ? C104 C105 H105 120.6 . . ? C106 C105 H105 120.6 . . ? N101 C106 C105 122.3(4) . . ? N101 C106 C107 116.6(3) . . ? C105 C106 C107 121.1(4) . . ? O2 C107 C106 112.0(3) . . ? O2 C107 H07A 109.2 . . ? C106 C107 H07A 109.2 . . ? O2 C107 H07B 109.2 . . ? C106 C107 H07B 109.2 . . ? H07A C107 H07B 107.9 . . ? C112 N111 C115 113.7(4) . . ? C112 N111 Zn2 128.5(3) . . ? C115 N111 Zn2 117.6(3) . . ? N111 C112 C102 120.3(4) . . ? N111 C112 S113 112.7(4) . . ? C102 C112 S113 127.0(4) . . ? C114 S113 C112 89.6(2) . . ? C115 C114 S113 111.9(4) . . ? C115 C114 H114 124.1 . . ? S113 C114 H114 124.1 . . ? C114 C115 N111 112.1(5) . . ? C114 C115 C122 132.5(5) . . ? N111 C115 C122 115.4(4) . . ? C122 N121 C126 118.6(4) . . ? C122 N121 Zn2 114.6(3) . . ? C126 N121 Zn2 126.0(3) . . ? N121 C122 C123 122.4(5) . . ? N121 C122 C115 113.4(4) . . ? C123 C122 C115 123.9(5) . . ? C124 C123 C122 118.0(6) . . ? C124 C123 H123 121.0 . . ? C122 C123 H123 121.0 . . ? C123 C124 C125 120.8(5) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C124 C125 C126 118.4(6) . . ? C124 C125 H125 120.8 . . ? C126 C125 H125 120.8 . . ? N121 C126 C125 121.8(5) . . ? N121 C126 H126 119.1 . . ? C125 C126 H126 119.1 . . ? O1A Cl1A O4A 109.33(17) . . ? O1A Cl1A O2A 109.7(2) . . ? O4A Cl1A O2A 109.17(17) . . ? O1A Cl1A O3A 109.74(18) . . ? O4A Cl1A O3A 109.81(18) . . ? O2A Cl1A O3A 109.0(2) . . ? O2B Cl1B O3B 110.33(19) . . ? O2B Cl1B O4B 109.9(2) . . ? O3B Cl1B O4B 109.11(19) . . ? O2B Cl1B O1B 108.17(18) . . ? O3B Cl1B O1B 109.5(2) . . ? O4B Cl1B O1B 109.9(2) . . ? O1C Cl1C O2C 111.6(3) . . ? O1C Cl1C O4C 108.5(2) . . ? O2C Cl1C O4C 109.6(2) . . ? O1C Cl1C O3C 109.1(3) . . ? O2C Cl1C O3C 108.0(3) . . ? O4C Cl1C O3C 110.0(2) . . ? O2D Cl1D O1D 109.9(6) . . ? O2D Cl1D O4D 111.5(7) . . ? O1D Cl1D O4D 103.1(6) . . ? O2D Cl1D O3D 116.0(7) . . ? O1D Cl1D O3D 106.3(6) . . ? O4D Cl1D O3D 109.0(8) . . ? O4E Cl1E O1E 109.8(4) . . ? O4E Cl1E O2E 107.7(4) . . ? O1E Cl1E O2E 110.0(4) . . ? O4E Cl1E O3E 111.2(4) . . ? O1E Cl1E O3E 112.5(4) . . ? O2E Cl1E O3E 105.5(4) . . ? N1F C1F C2F 179.1 . . ? H1G C1F H3G 77.7 . . ? H1G C2F H2G 79.7 . . ? H1G C2F H3G 71.8 . . ? H2G C2F H3G 88.4 . . ? C1G N1G N1G 167.5(17) . 2_756 ? C1G N1G H1F 25.9 . . ? N1G N1G H1F 141.7 2_756 . ? N1G C1G C2G 179.1 . . ? N1G C1G H1F 98.0 . . ? C2G C1G H1F 81.2 . . ? C1G C2G H1F 23.4 . . ? C1G C2G H2F 85.1 . . ? C1G C2G H3F 99.7 . . ? C1G C2G H1G 107.9 . . ? C1G C2G H2G 110.9 . . ? H1G C2G H2G 111.4 . . ? C1G C2G H3G 109.4 . . ? H1G C2G H3G 109.8 . . ? H2G C2G H3G 107.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.611 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.085 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.307 1.000 728.9 220.0 2 0.211 0.652 0.704 9.2 0.3 3 0.789 0.348 0.296 9.9 0.4 _platon_squeeze_details ; ;