# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email Catherine.Housecroft@unibas.ch _publ_contact_author_name 'Catherine E. Housecroft' loop_ _publ_author_name E.C.Constable G.Zhang 'Catherine E.Housecroft' J.A.Zampese data_gq143 _database_code_depnum_ccdc_archive 'CCDC 832650' #TrackingRef 'GQ143.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H90 Cl12 N18 Zn6, 14(H2 O)' _chemical_formula_sum 'C138 H118 Cl12 N18 O14 Zn6' _chemical_formula_weight 3070.31 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' 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' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.793(2) _cell_length_b 23.662(6) _cell_length_c 24.672(6) _cell_angle_alpha 68.897(19) _cell_angle_beta 87.31(2) _cell_angle_gamma 80.27(2) _cell_volume 4719(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 36.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7278 _exptl_absorpt_correction_T_max 0.9093 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; Crystals are unstable out of solvent and diffract poorly. Of many datasets on different crystals, this was the best. The non-merohedral twinning was dealt with using the TwinRotMat program in Platon. A HKLF 5 was generated from the original file (118787 measured reflections, R(int)=0.1520) using the twin law (-1,0,0/-0.5,0,1/-0.5,1,0) to give a modified file (16711 reflections, R(int)=0.0000) that was used in SHELXL97 with a basf of 0.2573. This structure contains large voids in which little solvent could be identified. Where possible, partial occupancy water molecules have been modelled on sites of electron density, but large voids still remain. It is probable the solvent within these voids is so disordered that the electron density is too smeared to create peaks in the difference map. ; _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 16711 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.05 _reflns_number_total 16711 _reflns_number_gt 14850 _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^)+(0.1603P)^2^+12.5366P] 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 16711 _refine_ls_number_parameters 875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.3034 _refine_ls_wR_factor_gt 0.2965 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.011 _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 0.01350(10) 0.50311(4) 0.68111(4) 0.0550(3) Uani 1 1 d . . . Cl1 Cl 0.0278(3) 0.40392(11) 0.69705(9) 0.0686(5) Uani 1 1 d . . . Cl2 Cl -0.2093(2) 0.56461(12) 0.64939(9) 0.0715(6) Uani 1 1 d . . . Zn2 Zn 0.32123(9) 0.62986(4) 0.15022(3) 0.0462(2) Uani 1 1 d . . . Cl3 Cl 0.1775(2) 0.55680(9) 0.17156(8) 0.0566(4) Uani 1 1 d . . . Cl4 Cl 0.4863(2) 0.64402(9) 0.07793(8) 0.0597(5) Uani 1 1 d . . . Zn3 Zn 0.37367(9) 1.19754(4) -0.01438(4) 0.0524(2) Uani 1 1 d . . . Cl5 Cl 0.4045(3) 1.20958(10) -0.10746(10) 0.0665(5) Uani 1 1 d . . . N1 N 0.1773(7) 0.5321(3) 0.6203(3) 0.0550(14) Uani 1 1 d . . . N2 N 0.4726(7) 0.5936(3) 0.4357(3) 0.0527(14) Uani 1 1 d . . . N3 N 0.4214(7) 0.6185(3) 0.2271(2) 0.0520(14) Uani 1 1 d . . . C1 C 0.2955(10) 0.5577(5) 0.6291(4) 0.071(2) Uani 1 1 d . . . H1A H 0.3018 0.5630 0.6653 0.085 Uiso 1 1 calc R . . C2 C 0.4068(9) 0.5766(4) 0.5889(3) 0.0605(19) Uani 1 1 d . . . H2A H 0.4875 0.5946 0.5972 0.073 Uiso 1 1 calc R . . C3 C 0.3993(9) 0.5689(4) 0.5354(3) 0.0538(17) Uani 1 1 d . . . C4 C 0.2792(9) 0.5432(4) 0.5262(3) 0.0564(17) Uani 1 1 d . . . H4A H 0.2701 0.5379 0.4902 0.068 Uiso 1 1 calc R . . C5 C 0.1723(9) 0.5250(4) 0.5684(3) 0.0569(17) Uani 1 1 d . . . H5A H 0.0914 0.5066 0.5609 0.068 Uiso 1 1 calc R . . Cl6 Cl 0.5776(2) 1.16787(10) 0.04470(10) 0.0697(5) Uani 1 1 d . . . C6 C 0.5130(9) 0.5917(4) 0.4885(3) 0.0535(17) Uani 1 1 d . . . C7 C 0.6452(9) 0.6102(4) 0.4985(3) 0.0569(18) Uani 1 1 d . . . H7A H 0.6714 0.6058 0.5369 0.068 Uiso 1 1 calc R . . C8 C 0.7420(9) 0.6357(4) 0.4523(3) 0.0546(17) Uani 1 1 d . . . C9 C 0.6978(8) 0.6387(4) 0.3972(3) 0.0541(17) Uani 1 1 d . . . H9A H 0.7578 0.6560 0.3641 0.065 Uiso 1 1 calc R . . C10 C 0.5649(8) 0.6161(4) 0.3913(3) 0.0521(16) Uani 1 1 d . . . C11 C 0.3744(9) 0.5802(4) 0.2776(3) 0.0573(18) Uani 1 1 d . . . H11A H 0.3086 0.5526 0.2766 0.069 Uiso 1 1 calc R . . C12 C 0.4186(9) 0.5796(4) 0.3308(3) 0.0571(18) Uani 1 1 d . . . H12A H 0.3786 0.5533 0.3655 0.069 Uiso 1 1 calc R . . C13 C 0.5187(8) 0.6162(4) 0.3342(3) 0.0528(16) Uani 1 1 d . . . C14 C 0.5695(10) 0.6554(4) 0.2819(3) 0.0593(19) Uani 1 1 d . . . H14A H 0.6385 0.6822 0.2821 0.071 Uiso 1 1 calc R . . C15 C 0.5190(9) 0.6550(4) 0.2298(3) 0.0538(17) Uani 1 1 d . . . H15A H 0.5551 0.6818 0.1946 0.065 Uiso 1 1 calc R . . C16 C 0.8812(9) 0.6583(4) 0.4600(3) 0.0586(18) Uani 1 1 d . . . C17 C 0.8934(11) 0.6798(5) 0.5053(4) 0.076(2) Uani 1 1 d . . . H17A H 0.8125 0.6776 0.5325 0.092 Uiso 1 1 calc R . . C18 C 1.0228(13) 0.7042(6) 0.5111(4) 0.086(3) Uani 1 1 d . . . H18A H 1.0281 0.7195 0.5416 0.103 Uiso 1 1 calc R . . C19 C 1.1430(11) 0.7062(5) 0.4729(4) 0.073(2) Uani 1 1 d . . . C20 C 1.1323(10) 0.6847(4) 0.4280(4) 0.066(2) Uani 1 1 d . . . H20A H 1.2142 0.6862 0.4013 0.079 Uiso 1 1 calc R . . C21 C 1.0034(9) 0.6609(4) 0.4220(4) 0.0614(19) Uani 1 1 d . . . H21A H 0.9985 0.6461 0.3912 0.074 Uiso 1 1 calc R . . C22 C 1.2779(13) 0.7297(5) 0.4806(5) 0.089(3) Uani 1 1 d . . . C23 C 1.3869(15) 0.7495(7) 0.4862(7) 0.110(4) Uani 1 1 d . . . H23 H 1.4755 0.7656 0.4907 0.132 Uiso 1 1 calc R . . N4 N 0.1832(7) 0.7133(3) 0.1343(3) 0.0485(13) Uani 1 1 d . . . N5 N 0.0130(7) 0.9370(3) 0.0901(3) 0.0514(13) Uani 1 1 d . . . N6 N 0.2306(7) 1.1326(3) 0.0174(3) 0.0551(14) Uani 1 1 d . . . C24 C 0.2217(9) 0.7641(3) 0.0945(4) 0.0560(17) Uani 1 1 d . . . H24A H 0.3059 0.7601 0.0698 0.067 Uiso 1 1 calc R . . C25 C 0.1448(8) 0.8219(3) 0.0876(3) 0.0557(17) Uani 1 1 d . . . H25A H 0.1775 0.8572 0.0596 0.067 Uiso 1 1 calc R . . C26 C 0.0183(8) 0.8281(3) 0.1224(3) 0.0490(15) Uani 1 1 d . . . C27 C -0.0242(9) 0.7750(3) 0.1628(4) 0.0565(17) Uani 1 1 d . . . H27A H -0.1113 0.7772 0.1867 0.068 Uiso 1 1 calc R . . C28 C 0.0621(9) 0.7189(3) 0.1677(3) 0.0557(17) Uani 1 1 d . . . H28A H 0.0342 0.6828 0.1960 0.067 Uiso 1 1 calc R . . C29 C -0.0653(8) 0.8906(3) 0.1154(3) 0.0509(16) Uani 1 1 d . . . C30 C -0.2148(8) 0.8989(3) 0.1345(3) 0.0537(16) Uani 1 1 d . . . H30A H -0.2655 0.8646 0.1530 0.064 Uiso 1 1 calc R . . C31 C -0.2906(9) 0.9586(3) 0.1262(3) 0.0537(17) Uani 1 1 d . . . C32 C -0.2098(9) 1.0059(3) 0.0994(4) 0.0565(17) Uani 1 1 d . . . H32A H -0.2586 1.0471 0.0914 0.068 Uiso 1 1 calc R . . C33 C -0.0571(8) 0.9939(3) 0.0837(3) 0.0515(16) Uani 1 1 d . . . C34 C 0.2775(9) 1.0753(3) 0.0177(3) 0.0565(17) Uani 1 1 d . . . H34A H 0.3772 1.0653 0.0038 0.068 Uiso 1 1 calc R . . C35 C 0.1839(9) 1.0302(3) 0.0379(3) 0.0537(17) Uani 1 1 d . . . H35A H 0.2199 0.9905 0.0368 0.064 Uiso 1 1 calc R . . C36 C 0.0412(8) 1.0424(3) 0.0591(3) 0.0517(16) Uani 1 1 d . . . C37 C -0.0088(8) 1.1044(3) 0.0606(4) 0.061(2) Uani 1 1 d . . . H37A H -0.1049 1.1154 0.0764 0.074 Uiso 1 1 calc R . . C38 C 0.0890(10) 1.1445(4) 0.0382(4) 0.069(2) Uani 1 1 d . . . H38A H 0.0552 1.1852 0.0369 0.083 Uiso 1 1 calc R . . C39 C -0.4494(9) 0.9689(3) 0.1462(4) 0.0574(18) Uani 1 1 d . . . C40 C -0.5484(8) 0.9263(4) 0.1526(4) 0.0574(18) Uani 1 1 d . . . H40A H -0.5141 0.8914 0.1422 0.069 Uiso 1 1 calc R . . C41 C -0.6966(9) 0.9347(4) 0.1741(4) 0.065(2) Uani 1 1 d . . . H41A H -0.7620 0.9052 0.1787 0.077 Uiso 1 1 calc R . . C42 C -0.7494(9) 0.9859(4) 0.1888(4) 0.066(2) Uani 1 1 d . . . C43 C -0.6545(10) 1.0287(4) 0.1805(4) 0.073(2) Uani 1 1 d . . . H43A H -0.6925 1.0649 0.1885 0.088 Uiso 1 1 calc R . . C44 C -0.5055(10) 1.0206(4) 0.1610(4) 0.069(2) Uani 1 1 d . . . H44A H -0.4409 1.0501 0.1576 0.083 Uiso 1 1 calc R . . C45 C -0.9045(11) 0.9948(5) 0.2108(5) 0.077(2) Uani 1 1 d . . . N7 N 0.2395(7) 1.2710(3) -0.0044(3) 0.0493(13) Uani 1 1 d . . . N8 N -0.0605(7) 1.4251(3) 0.0723(3) 0.0514(13) Uani 1 1 d . . . N9 N -0.0846(7) 1.4823(3) 0.2482(2) 0.0535(14) Uani 1 1 d . . . C46 C -1.0293(13) 1.0016(6) 0.2277(5) 0.100(4) Uani 1 1 d . . . H46 H -1.1313 1.0071 0.2415 0.120 Uiso 1 1 calc R . . C47 C 0.2452(11) 1.2856(4) 0.0428(4) 0.071(2) Uani 1 1 d . . . H47A H 0.3230 1.2625 0.0712 0.085 Uiso 1 1 calc R . . C48 C 0.1458(10) 1.3320(4) 0.0527(4) 0.071(2) Uani 1 1 d . . . H48A H 0.1506 1.3385 0.0884 0.085 Uiso 1 1 calc R . . C49 C 0.0381(8) 1.3693(3) 0.0102(3) 0.0514(16) Uani 1 1 d . . . C50 C 0.0375(11) 1.3578(4) -0.0403(4) 0.071(2) Uani 1 1 d . . . H50A H -0.0317 1.3833 -0.0712 0.085 Uiso 1 1 calc R . . C51 C 0.1392(10) 1.3084(4) -0.0459(4) 0.067(2) Uani 1 1 d . . . H51A H 0.1371 1.3010 -0.0812 0.080 Uiso 1 1 calc R . . C52 C -0.0705(9) 1.4217(3) 0.0189(3) 0.0510(16) Uani 1 1 d . . . C53 C -0.1731(9) 1.4611(3) -0.0233(3) 0.0532(16) Uani 1 1 d . . . H53A H -0.1770 1.4559 -0.0596 0.064 Uiso 1 1 calc R . . C54 C -0.2719(8) 1.5089(3) -0.0133(3) 0.0485(15) Uani 1 1 d . . . C55 C -0.2615(8) 1.5122(3) 0.0420(3) 0.0516(16) Uani 1 1 d . . . H55A H -0.3282 1.5432 0.0515 0.062 Uiso 1 1 calc R . . C56 C -0.1558(8) 1.4712(3) 0.0826(3) 0.0494(15) Uani 1 1 d . . . C57 C -0.0081(11) 1.4352(4) 0.2328(4) 0.066(2) Uani 1 1 d . . . H57A H 0.0633 1.4043 0.2597 0.079 Uiso 1 1 calc R . . C58 C -0.0301(10) 1.4307(4) 0.1807(4) 0.067(2) Uani 1 1 d . . . H58A H 0.0289 1.3981 0.1712 0.080 Uiso 1 1 calc R . . C59 C -0.1369(8) 1.4729(4) 0.1411(3) 0.0536(16) Uani 1 1 d . . . C60 C -0.2188(9) 1.5198(4) 0.1579(4) 0.064(2) Uani 1 1 d . . . H60A H -0.2955 1.5498 0.1328 0.077 Uiso 1 1 calc R . . C61 C -0.1874(9) 1.5221(4) 0.2113(3) 0.063(2) Uani 1 1 d . . . H61A H -0.2437 1.5545 0.2218 0.075 Uiso 1 1 calc R . . C62 C -0.3830(8) 1.5530(3) -0.0582(3) 0.0530(16) Uani 1 1 d . . . C63 C -0.3940(12) 1.5481(5) -0.1120(4) 0.078(3) Uani 1 1 d . . . H63A H -0.3290 1.5159 -0.1202 0.093 Uiso 1 1 calc R . . C64 C -0.4965(13) 1.5886(5) -0.1538(4) 0.087(3) Uani 1 1 d . . . H64A H -0.4992 1.5845 -0.1906 0.105 Uiso 1 1 calc R . . C65 C -0.5934(11) 1.6342(4) -0.1438(4) 0.072(2) Uani 1 1 d . . . C67 C -0.4868(11) 1.5980(4) -0.0479(4) 0.068(2) Uani 1 1 d . . . H67A H -0.4893 1.6009 -0.0105 0.081 Uiso 1 1 calc R . . C66 C -0.5870(11) 1.6388(4) -0.0902(4) 0.074(2) Uani 1 1 d . . . H66A H -0.6534 1.6708 -0.0822 0.088 Uiso 1 1 calc R . . C68 C -0.7065(14) 1.6767(6) -0.1874(6) 0.099(4) Uani 1 1 d . . . C69 C -0.792(2) 1.7092(7) -0.2223(8) 0.144(7) Uani 1 1 d . . . H69 H -0.8640 1.7364 -0.2515 0.173 Uiso 1 1 calc R . . O1 O -0.2770(13) 0.7965(3) 0.2890(3) 0.111(3) Uani 1 1 d . . . O2 O 0.2426(15) 0.7815(4) 0.2774(4) 0.136(4) Uani 1 1 d . . . O3 O 0.245(2) 1.2800(7) 0.2305(9) 0.268(12) Uani 1 1 d . . . O4 O -0.506(3) 1.2851(12) 0.3696(13) 0.275(16) Uani 0.75 1 d P . . O5 O -0.033(3) 0.8758(10) 0.3684(10) 0.160(10) Uani 0.50 1 d P . . O6 O -0.399(3) 1.1282(16) 0.2307(16) 0.32(2) Uani 0.75 1 d P . . O7 O -0.035(5) 1.2037(19) 0.1446(19) 0.30(3) Uani 0.50 1 d P . . O8 O 0.433(4) 0.9034(18) 0.3594(12) 0.237(19) Uani 0.50 1 d P . . O9 O -0.321(5) 0.825(2) 0.519(3) 0.39(4) Uani 0.50 1 d P . . O10 O -0.048(7) 1.226(4) 0.369(3) 0.52(7) Uani 0.50 1 d P . . 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 0.0504(5) 0.0723(6) 0.0443(4) -0.0223(4) -0.0033(3) -0.0110(4) Cl1 0.0722(13) 0.0776(13) 0.0676(12) -0.0388(10) 0.0128(10) -0.0171(10) Cl2 0.0572(11) 0.0915(15) 0.0572(11) -0.0168(10) -0.0130(9) -0.0074(10) Zn2 0.0465(4) 0.0469(4) 0.0446(4) -0.0189(3) -0.0066(3) 0.0017(3) Cl3 0.0659(11) 0.0572(10) 0.0507(9) -0.0221(8) -0.0037(8) -0.0131(8) Cl4 0.0646(11) 0.0563(10) 0.0536(10) -0.0207(8) 0.0063(8) 0.0031(8) Zn3 0.0441(4) 0.0428(4) 0.0683(5) -0.0200(4) 0.0008(4) -0.0014(3) Cl5 0.0715(12) 0.0654(12) 0.0741(12) -0.0369(10) 0.0089(10) -0.0174(10) N1 0.052(3) 0.070(4) 0.042(3) -0.019(3) -0.002(3) -0.009(3) N2 0.047(3) 0.063(4) 0.047(3) -0.020(3) -0.002(2) -0.006(3) N3 0.047(3) 0.062(4) 0.042(3) -0.017(3) -0.003(2) 0.003(3) C1 0.063(5) 0.114(7) 0.047(4) -0.037(4) 0.006(4) -0.030(5) C2 0.047(4) 0.086(6) 0.051(4) -0.024(4) 0.001(3) -0.019(4) C3 0.051(4) 0.063(4) 0.044(4) -0.016(3) -0.005(3) -0.005(3) C4 0.062(4) 0.067(5) 0.040(4) -0.019(3) 0.000(3) -0.010(4) C5 0.058(4) 0.066(5) 0.046(4) -0.020(3) -0.003(3) -0.010(4) Cl6 0.0492(10) 0.0602(11) 0.0828(14) -0.0094(10) -0.0080(9) 0.0028(8) C6 0.049(4) 0.065(4) 0.045(4) -0.020(3) -0.002(3) -0.003(3) C7 0.057(4) 0.076(5) 0.039(3) -0.022(3) -0.002(3) -0.011(4) C8 0.048(4) 0.069(5) 0.049(4) -0.024(3) -0.001(3) -0.009(3) C9 0.045(4) 0.072(5) 0.046(4) -0.022(3) 0.002(3) -0.009(3) C10 0.050(4) 0.065(4) 0.040(3) -0.020(3) -0.002(3) -0.003(3) C11 0.062(5) 0.063(4) 0.049(4) -0.020(3) -0.004(3) -0.016(4) C12 0.056(4) 0.067(5) 0.045(4) -0.014(3) -0.002(3) -0.013(4) C13 0.051(4) 0.063(4) 0.043(4) -0.019(3) -0.005(3) -0.002(3) C14 0.064(5) 0.075(5) 0.046(4) -0.024(4) 0.000(3) -0.024(4) C15 0.057(4) 0.063(4) 0.044(4) -0.021(3) -0.002(3) -0.013(3) C16 0.053(4) 0.066(5) 0.056(4) -0.021(4) -0.009(3) -0.006(4) C17 0.074(6) 0.103(7) 0.067(5) -0.040(5) 0.011(4) -0.034(5) C18 0.093(7) 0.116(8) 0.069(6) -0.044(6) 0.000(5) -0.045(6) C19 0.060(5) 0.077(6) 0.076(6) -0.016(5) -0.011(4) -0.017(4) C20 0.057(4) 0.064(5) 0.072(5) -0.018(4) -0.008(4) -0.006(4) C21 0.052(4) 0.075(5) 0.056(4) -0.022(4) -0.005(3) -0.009(4) C22 0.084(7) 0.082(7) 0.103(8) -0.029(6) -0.020(6) -0.025(5) C23 0.084(8) 0.116(10) 0.139(11) -0.047(8) -0.006(7) -0.037(7) N4 0.046(3) 0.047(3) 0.052(3) -0.020(3) -0.001(2) -0.001(2) N5 0.046(3) 0.045(3) 0.061(4) -0.019(3) -0.006(3) 0.000(2) N6 0.049(3) 0.043(3) 0.071(4) -0.018(3) -0.001(3) -0.005(3) C24 0.052(4) 0.042(4) 0.071(5) -0.020(3) 0.007(3) -0.002(3) C25 0.047(4) 0.049(4) 0.063(4) -0.013(3) 0.003(3) -0.002(3) C26 0.046(4) 0.042(3) 0.060(4) -0.020(3) -0.003(3) -0.004(3) C27 0.051(4) 0.047(4) 0.068(5) -0.020(3) 0.003(3) -0.001(3) C28 0.056(4) 0.043(4) 0.061(4) -0.015(3) 0.006(3) -0.002(3) C29 0.046(4) 0.046(4) 0.058(4) -0.018(3) -0.005(3) 0.002(3) C30 0.046(4) 0.050(4) 0.061(4) -0.014(3) -0.008(3) -0.005(3) C31 0.052(4) 0.043(4) 0.065(4) -0.019(3) -0.004(3) -0.003(3) C32 0.056(4) 0.044(4) 0.067(5) -0.018(3) -0.004(3) -0.004(3) C33 0.049(4) 0.039(3) 0.064(4) -0.017(3) -0.005(3) -0.003(3) C34 0.055(4) 0.047(4) 0.066(5) -0.021(3) -0.001(3) -0.002(3) C35 0.054(4) 0.044(4) 0.063(4) -0.021(3) -0.001(3) -0.002(3) C36 0.048(4) 0.040(3) 0.067(4) -0.020(3) -0.010(3) 0.001(3) C37 0.032(3) 0.037(3) 0.097(6) -0.004(4) -0.001(3) -0.004(3) C38 0.053(4) 0.044(4) 0.104(7) -0.024(4) 0.009(4) 0.000(3) C39 0.055(4) 0.048(4) 0.064(4) -0.017(3) 0.000(3) -0.003(3) C40 0.041(4) 0.054(4) 0.073(5) -0.020(4) -0.007(3) 0.001(3) C41 0.046(4) 0.070(5) 0.070(5) -0.017(4) -0.004(3) -0.004(4) C42 0.049(4) 0.078(5) 0.062(5) -0.018(4) 0.005(4) -0.002(4) C43 0.065(5) 0.058(5) 0.089(6) -0.026(4) 0.011(4) 0.008(4) C44 0.062(5) 0.059(5) 0.091(6) -0.034(4) 0.013(4) -0.011(4) C45 0.056(5) 0.081(6) 0.088(6) -0.028(5) 0.013(4) -0.006(4) N7 0.044(3) 0.046(3) 0.054(3) -0.016(3) -0.003(2) -0.001(2) N8 0.045(3) 0.056(3) 0.053(3) -0.021(3) -0.002(2) -0.001(3) N9 0.053(3) 0.065(4) 0.043(3) -0.020(3) -0.002(3) -0.010(3) C46 0.069(6) 0.126(10) 0.100(8) -0.044(7) 0.014(6) 0.003(6) C47 0.072(5) 0.072(5) 0.069(5) -0.035(4) -0.032(4) 0.018(4) C48 0.066(5) 0.083(6) 0.067(5) -0.040(4) -0.021(4) 0.017(4) C49 0.046(4) 0.047(4) 0.058(4) -0.017(3) -0.005(3) -0.002(3) C50 0.082(6) 0.070(5) 0.060(5) -0.038(4) -0.018(4) 0.028(4) C51 0.076(5) 0.067(5) 0.058(4) -0.031(4) -0.014(4) 0.013(4) C52 0.054(4) 0.051(4) 0.049(4) -0.022(3) -0.003(3) -0.003(3) C53 0.055(4) 0.052(4) 0.054(4) -0.025(3) -0.004(3) 0.001(3) C54 0.044(3) 0.050(4) 0.053(4) -0.019(3) -0.004(3) -0.007(3) C55 0.045(4) 0.053(4) 0.060(4) -0.027(3) -0.002(3) -0.003(3) C56 0.043(3) 0.054(4) 0.054(4) -0.024(3) -0.001(3) -0.005(3) C57 0.078(5) 0.056(4) 0.058(4) -0.022(4) -0.021(4) 0.011(4) C58 0.071(5) 0.058(4) 0.070(5) -0.031(4) -0.015(4) 0.017(4) C59 0.049(4) 0.062(4) 0.050(4) -0.022(3) -0.006(3) -0.004(3) C60 0.057(4) 0.080(5) 0.057(4) -0.034(4) -0.015(3) 0.015(4) C61 0.054(4) 0.081(5) 0.058(4) -0.039(4) -0.013(3) 0.010(4) C62 0.044(4) 0.056(4) 0.054(4) -0.017(3) -0.010(3) 0.001(3) C63 0.080(6) 0.081(6) 0.067(5) -0.032(5) -0.021(4) 0.019(5) C64 0.101(7) 0.081(6) 0.072(6) -0.027(5) -0.037(5) 0.015(6) C65 0.063(5) 0.063(5) 0.080(6) -0.015(4) -0.025(4) 0.001(4) C67 0.073(5) 0.063(5) 0.064(5) -0.028(4) -0.014(4) 0.013(4) C66 0.070(5) 0.054(5) 0.085(6) -0.020(4) -0.014(5) 0.015(4) C68 0.089(7) 0.091(7) 0.107(8) -0.031(6) -0.047(7) 0.014(6) C69 0.152(14) 0.105(10) 0.154(14) -0.025(9) -0.095(12) 0.016(9) O1 0.210(9) 0.064(4) 0.059(4) -0.018(3) 0.043(5) -0.044(5) O2 0.219(11) 0.073(5) 0.076(5) 0.020(4) -0.004(6) -0.019(6) O3 0.209(16) 0.159(12) 0.35(2) 0.022(14) -0.193(17) -0.004(11) O4 0.30(3) 0.27(3) 0.32(3) -0.24(3) -0.13(3) 0.11(2) O5 0.16(2) 0.109(15) 0.143(18) 0.026(13) 0.023(15) -0.013(14) O6 0.31(3) 0.44(4) 0.45(4) -0.39(4) 0.19(3) -0.24(3) O7 0.38(5) 0.31(4) 0.38(5) -0.29(4) 0.30(5) -0.21(4) O8 0.22(3) 0.29(4) 0.122(19) -0.04(2) 0.03(2) 0.09(3) O9 0.22(4) 0.25(4) 0.80(12) -0.34(6) -0.28(6) 0.08(3) O10 0.41(7) 0.92(16) 0.35(6) -0.49(10) -0.21(6) 0.28(9) _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 N9 2.039(6) 2_576 ? Zn1 N1 2.046(6) . ? Zn1 Cl1 2.218(3) . ? Zn1 Cl2 2.220(2) . ? Zn2 N3 2.040(6) . ? Zn2 N4 2.049(6) . ? Zn2 Cl3 2.210(2) . ? Zn2 Cl4 2.211(2) . ? Zn3 N7 2.016(6) . ? Zn3 N6 2.061(6) . ? Zn3 Cl6 2.217(2) . ? Zn3 Cl5 2.219(2) . ? N1 C1 1.351(11) . ? N1 C5 1.354(10) . ? N2 C10 1.336(9) . ? N2 C6 1.347(9) . ? N3 C15 1.335(10) . ? N3 C11 1.345(10) . ? C1 C2 1.370(11) . ? C1 H1A 0.9500 . ? C2 C3 1.404(11) . ? C2 H2A 0.9500 . ? C3 C4 1.370(11) . ? C3 C6 1.501(11) . ? C4 C5 1.369(11) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.372(11) . ? C7 C8 1.404(11) . ? C7 H7A 0.9500 . ? C8 C9 1.407(10) . ? C8 C16 1.461(11) . ? C9 C10 1.398(11) . ? C9 H9A 0.9500 . ? C10 C13 1.485(10) . ? C11 C12 1.382(11) . ? C11 H11A 0.9500 . ? C12 C13 1.359(11) . ? C12 H12A 0.9500 . ? C13 C14 1.396(11) . ? C14 C15 1.383(10) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.387(12) . ? C16 C17 1.399(12) . ? C17 C18 1.395(13) . ? C17 H17A 0.9500 . ? C18 C19 1.379(14) . ? C18 H18A 0.9500 . ? C19 C20 1.388(14) . ? C19 C22 1.440(13) . ? C20 C21 1.383(12) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.169(15) . ? C23 H23 0.9500 . ? N4 C28 1.333(9) . ? N4 C24 1.335(10) . ? N5 C29 1.337(10) . ? N5 C33 1.339(9) . ? N6 C34 1.348(10) . ? N6 C38 1.348(10) . ? C24 C25 1.375(10) . ? C24 H24A 0.9500 . ? C25 C26 1.392(10) . ? C25 H25A 0.9500 . ? C26 C27 1.392(10) . ? C26 C29 1.489(9) . ? C27 C28 1.380(10) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.382(10) . ? C30 C31 1.405(10) . ? C30 H30A 0.9500 . ? C31 C32 1.373(11) . ? C31 C39 1.469(11) . ? C32 C33 1.391(11) . ? C32 H32A 0.9500 . ? C33 C36 1.491(10) . ? C34 C35 1.391(11) . ? C34 H34A 0.9500 . ? C35 C36 1.363(11) . ? C35 H35A 0.9500 . ? C36 C37 1.470(10) . ? C37 C38 1.341(11) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.402(11) . ? C39 C44 1.405(11) . ? C40 C41 1.394(11) . ? C40 H40A 0.9500 . ? C41 C42 1.388(13) . ? C41 H41A 0.9500 . ? C42 C43 1.371(13) . ? C42 C45 1.454(12) . ? C43 C44 1.381(12) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.161(14) . ? N7 C47 1.333(10) . ? N7 C51 1.334(10) . ? N8 C56 1.352(9) . ? N8 C52 1.356(9) . ? N9 C61 1.305(10) . ? N9 C57 1.368(10) . ? N9 Zn1 2.039(6) 2_576 ? C46 H46 0.9500 . ? C47 C48 1.371(12) . ? C47 H47A 0.9500 . ? C48 C49 1.386(11) . ? C48 H48A 0.9500 . ? C49 C50 1.368(11) . ? C49 C52 1.504(10) . ? C50 C51 1.391(11) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.367(10) . ? C53 C54 1.394(10) . ? C53 H53A 0.9500 . ? C54 C55 1.402(10) . ? C54 C62 1.482(10) . ? C55 C56 1.376(10) . ? C55 H55A 0.9500 . ? C56 C59 1.476(10) . ? C57 C58 1.353(12) . ? C57 H57A 0.9500 . ? C58 C59 1.378(11) . ? C58 H58A 0.9500 . ? C59 C60 1.398(11) . ? C60 C61 1.382(11) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 C67 1.369(11) . ? C62 C63 1.382(12) . ? C63 C64 1.371(12) . ? C63 H63A 0.9500 . ? C64 C65 1.345(14) . ? C64 H64A 0.9500 . ? C65 C66 1.371(14) . ? C65 C68 1.463(13) . ? C67 C66 1.367(12) . ? C67 H67A 0.9500 . ? C66 H66A 0.9500 . ? C68 C69 1.136(16) . ? C69 H69 0.9500 . ? 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 N9 Zn1 N1 103.9(3) 2_576 . ? N9 Zn1 Cl1 111.9(2) 2_576 . ? N1 Zn1 Cl1 105.2(2) . . ? N9 Zn1 Cl2 108.22(19) 2_576 . ? N1 Zn1 Cl2 108.14(19) . . ? Cl1 Zn1 Cl2 118.32(10) . . ? N3 Zn2 N4 100.1(2) . . ? N3 Zn2 Cl3 105.10(19) . . ? N4 Zn2 Cl3 109.89(18) . . ? N3 Zn2 Cl4 112.89(18) . . ? N4 Zn2 Cl4 105.70(18) . . ? Cl3 Zn2 Cl4 121.22(8) . . ? N7 Zn3 N6 100.5(2) . . ? N7 Zn3 Cl6 109.88(18) . . ? N6 Zn3 Cl6 107.51(19) . . ? N7 Zn3 Cl5 111.64(18) . . ? N6 Zn3 Cl5 105.4(2) . . ? Cl6 Zn3 Cl5 119.89(9) . . ? C1 N1 C5 116.5(7) . . ? C1 N1 Zn1 123.4(5) . . ? C5 N1 Zn1 120.1(5) . . ? C10 N2 C6 117.7(6) . . ? C15 N3 C11 117.7(6) . . ? C15 N3 Zn2 121.0(5) . . ? C11 N3 Zn2 120.6(5) . . ? N1 C1 C2 123.9(7) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 118.6(7) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? C4 C3 C2 117.6(7) . . ? C4 C3 C6 121.1(7) . . ? C2 C3 C6 121.1(7) . . ? C5 C4 C3 120.7(7) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? N1 C5 C4 122.6(7) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? N2 C6 C7 123.0(7) . . ? N2 C6 C3 114.4(6) . . ? C7 C6 C3 122.5(7) . . ? C6 C7 C8 120.4(7) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C7 C8 C9 116.3(7) . . ? C7 C8 C16 122.9(7) . . ? C9 C8 C16 120.8(7) . . ? C10 C9 C8 119.5(7) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? N2 C10 C9 122.9(6) . . ? N2 C10 C13 116.2(7) . . ? C9 C10 C13 120.9(7) . . ? N3 C11 C12 122.1(7) . . ? N3 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 120.7(7) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 117.2(7) . . ? C12 C13 C10 120.8(7) . . ? C14 C13 C10 122.0(7) . . ? C15 C14 C13 119.7(7) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? N3 C15 C14 122.5(7) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? C21 C16 C17 117.7(8) . . ? C21 C16 C8 121.5(7) . . ? C17 C16 C8 120.7(8) . . ? C18 C17 C16 120.9(9) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C19 C18 C17 120.3(9) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 119.1(8) . . ? C18 C19 C22 119.6(10) . . ? C20 C19 C22 121.3(10) . . ? C21 C20 C19 120.5(9) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C16 121.4(8) . . ? C20 C21 H21A 119.3 . . ? C16 C21 H21A 119.3 . . ? C23 C22 C19 179.1(16) . . ? C22 C23 H23 180.0 . . ? C28 N4 C24 118.4(6) . . ? C28 N4 Zn2 120.6(5) . . ? C24 N4 Zn2 120.7(5) . . ? C29 N5 C33 118.1(6) . . ? C34 N6 C38 117.0(7) . . ? C34 N6 Zn3 119.8(5) . . ? C38 N6 Zn3 123.2(5) . . ? N4 C24 C25 122.8(7) . . ? N4 C24 H24A 118.6 . . ? C25 C24 H24A 118.6 . . ? C24 C25 C26 119.0(7) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? C27 C26 C25 118.1(6) . . ? C27 C26 C29 122.6(7) . . ? C25 C26 C29 119.3(6) . . ? C28 C27 C26 119.0(7) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? N4 C28 C27 122.7(7) . . ? N4 C28 H28A 118.6 . . ? C27 C28 H28A 118.6 . . ? N5 C29 C30 123.1(6) . . ? N5 C29 C26 116.1(6) . . ? C30 C29 C26 120.8(7) . . ? C29 C30 C31 119.1(7) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C32 C31 C30 117.2(7) . . ? C32 C31 C39 122.4(7) . . ? C30 C31 C39 120.4(7) . . ? C31 C32 C33 120.5(7) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? N5 C33 C32 121.9(7) . . ? N5 C33 C36 114.9(6) . . ? C32 C33 C36 123.2(6) . . ? N6 C34 C35 121.8(7) . . ? N6 C34 H34A 119.1 . . ? C35 C34 H34A 119.1 . . ? C36 C35 C34 120.8(7) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C37 117.6(7) . . ? C35 C36 C33 121.5(6) . . ? C37 C36 C33 120.7(6) . . ? C38 C37 C36 116.1(7) . . ? C38 C37 H37A 121.9 . . ? C36 C37 H37A 121.9 . . ? C37 C38 N6 126.5(7) . . ? C37 C38 H38A 116.7 . . ? N6 C38 H38A 116.7 . . ? C40 C39 C44 117.9(7) . . ? C40 C39 C31 120.8(7) . . ? C44 C39 C31 121.2(7) . . ? C41 C40 C39 120.7(8) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C42 C41 C40 120.4(8) . . ? C42 C41 H41A 119.8 . . ? C40 C41 H41A 119.8 . . ? C43 C42 C41 118.8(8) . . ? C43 C42 C45 120.9(9) . . ? C41 C42 C45 120.3(9) . . ? C42 C43 C44 122.0(8) . . ? C42 C43 H43A 119.0 . . ? C44 C43 H43A 119.0 . . ? C43 C44 C39 120.0(8) . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? C46 C45 C42 178.9(13) . . ? C47 N7 C51 116.1(7) . . ? C47 N7 Zn3 123.2(5) . . ? C51 N7 Zn3 120.8(5) . . ? C56 N8 C52 116.9(6) . . ? C61 N9 C57 117.0(6) . . ? C61 N9 Zn1 121.8(5) . 2_576 ? C57 N9 Zn1 120.3(5) . 2_576 ? C45 C46 H46 180.0 . . ? N7 C47 C48 124.0(7) . . ? N7 C47 H47A 118.0 . . ? C48 C47 H47A 118.0 . . ? C47 C48 C49 119.3(8) . . ? C47 C48 H48A 120.4 . . ? C49 C48 H48A 120.4 . . ? C50 C49 C48 117.6(7) . . ? C50 C49 C52 121.5(7) . . ? C48 C49 C52 120.9(7) . . ? C49 C50 C51 119.3(7) . . ? C49 C50 H50A 120.4 . . ? C51 C50 H50A 120.4 . . ? N7 C51 C50 123.5(7) . . ? N7 C51 H51A 118.3 . . ? C50 C51 H51A 118.3 . . ? N8 C52 C53 123.3(7) . . ? N8 C52 C49 114.3(6) . . ? C53 C52 C49 122.4(6) . . ? C52 C53 C54 120.4(7) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C53 C54 C55 116.1(6) . . ? C53 C54 C62 121.9(7) . . ? C55 C54 C62 122.0(7) . . ? C56 C55 C54 120.8(7) . . ? C56 C55 H55A 119.6 . . ? C54 C55 H55A 119.6 . . ? N8 C56 C55 122.4(7) . . ? N8 C56 C59 114.1(6) . . ? C55 C56 C59 123.5(7) . . ? C58 C57 N9 122.5(7) . . ? C58 C57 H57A 118.7 . . ? N9 C57 H57A 118.7 . . ? C57 C58 C59 120.9(7) . . ? C57 C58 H58A 119.6 . . ? C59 C58 H58A 119.6 . . ? C58 C59 C60 116.4(7) . . ? C58 C59 C56 121.7(7) . . ? C60 C59 C56 121.7(7) . . ? C61 C60 C59 119.4(7) . . ? C61 C60 H60A 120.3 . . ? C59 C60 H60A 120.3 . . ? N9 C61 C60 123.7(7) . . ? N9 C61 H61A 118.2 . . ? C60 C61 H61A 118.2 . . ? C67 C62 C63 116.2(7) . . ? C67 C62 C54 122.5(7) . . ? C63 C62 C54 121.2(7) . . ? C64 C63 C62 121.6(9) . . ? C64 C63 H63A 119.2 . . ? C62 C63 H63A 119.2 . . ? C65 C64 C63 121.4(10) . . ? C65 C64 H64A 119.3 . . ? C63 C64 H64A 119.3 . . ? C64 C65 C66 117.9(8) . . ? C64 C65 C68 122.0(10) . . ? C66 C65 C68 120.1(9) . . ? C66 C67 C62 121.7(8) . . ? C66 C67 H67A 119.2 . . ? C62 C67 H67A 119.2 . . ? C67 C66 C65 121.1(8) . . ? C67 C66 H66A 119.4 . . ? C65 C66 H66A 119.4 . . ? C69 C68 C65 178.2(18) . . ? C68 C69 H69 180.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.135 _refine_diff_density_min -1.453 _refine_diff_density_rms 0.141 # start Validation Reply Form _vrf_PLAT306_I ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 RESPONSE: Data quality did not allow location of H's from difference map ; _vrf_PLAT602_I ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Residual electron density within this large void is too smeared to identify individual solvent molecules which must be heavily disordered. ; # Attachment 'GQ199.CIF' data_gq199 _database_code_depnum_ccdc_archive 'CCDC 832651' #TrackingRef 'GQ199.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C160 H112 I24 N32 Zn12, 1.5(C6 H4 Cl2), 12(H2 O)' _chemical_formula_sum 'C169 H142 Cl3 I24 N32 O12 Zn12' _chemical_formula_weight 6749.58 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall -R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 38.903(5) _cell_length_b 38.903(5) _cell_length_c 16.736(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21936(6) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9426 _cell_measurement_theta_min 4.92 _cell_measurement_theta_max 38.76 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9405 _exptl_absorpt_coefficient_mu 3.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2685 _exptl_absorpt_correction_T_max 0.6166 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; These crystals lose solvent rapidly and diffract very poorly due to the size of the molecule. This is the best dataset of many. It is assumed the position of N2 in the central ring is disordered, and modelled as such. The largest residual electron density peaks are close to the heavy iodide and zinc atoms. Most of the solvents filling the void space could not be identified. One partial solvent molecule has been modelled with heavy restraints, and the largest peaks remaining in the difference map have been modelled as partial occupancy water molecules, however it is possible these are the Cl atoms of disordered PhCl2 molecules. ; _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 96602 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8617 _reflns_number_gt 6624 _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^)+(0.1000P)^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 8617 _refine_ls_number_parameters 438 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1799 _refine_ls_R_factor_gt 0.1571 _refine_ls_wR_factor_ref 0.3959 _refine_ls_wR_factor_gt 0.3837 _refine_ls_goodness_of_fit_ref 2.582 _refine_ls_restrained_S_all 2.593 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 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 0.21792(4) 0.04799(4) -0.08794(12) 0.1022(5) Uani 1 1 d . . . I1 I 0.22004(3) -0.01555(3) -0.06089(8) 0.1177(3) Uani 1 1 d . . . I2 I 0.25523(3) 0.08942(3) -0.20760(8) 0.1201(4) Uani 1 1 d . . . Zn2 Zn 0.30114(5) 0.35877(4) 0.39849(11) 0.1091(5) Uani 1 1 d . . . I3 I 0.28479(5) 0.38402(3) 0.27254(8) 0.1566(5) Uani 1 1 d . . . I4 I 0.36469(4) 0.40025(3) 0.48253(9) 0.1350(4) Uani 1 1 d . . . N1 N 0.2381(3) 0.0821(3) 0.0122(9) 0.115(4) Uani 1 1 d . . . C1 C 0.2568(4) 0.1222(3) 0.0094(10) 0.099(4) Uani 1 1 d . . . H1A H 0.2610 0.1358 -0.0399 0.119 Uiso 1 1 calc R . . C2 C 0.2702(4) 0.1433(4) 0.0836(9) 0.102(4) Uani 1 1 d . . . H2A H 0.2829 0.1714 0.0823 0.122 Uiso 1 1 calc R . . C3 C 0.2661(4) 0.1265(4) 0.1508(9) 0.104(4) Uani 1 1 d . A . C4 C 0.2457(7) 0.0835(6) 0.1539(13) 0.157(7) Uani 1 1 d U . . H4A H 0.2445 0.0702 0.2023 0.189 Uiso 1 1 calc R . . C5 C 0.2282(8) 0.0623(6) 0.0852(15) 0.166(8) Uani 1 1 d U . . H5A H 0.2097 0.0346 0.0878 0.200 Uiso 1 1 calc R . . N2 N 0.2844(3) 0.1812(3) 0.2437(8) 0.093(3) Uani 0.33 1 d P A 1 C7' C 0.2844(3) 0.1812(3) 0.2437(8) 0.093(3) Uani 0.67 1 d P A 2 H7'A H 0.2772 0.1938 0.2040 0.112 Uiso 0.67 1 calc PR A 2 C6 C 0.2813(3) 0.1458(3) 0.2277(8) 0.090(3) Uani 1 1 d . . . C7 C 0.2930(3) 0.1292(3) 0.2884(8) 0.094(3) Uani 0.67 1 d P A 1 H7A H 0.2921 0.1047 0.2780 0.113 Uiso 0.67 1 calc PR A 1 N2' N 0.2930(3) 0.1292(3) 0.2884(8) 0.094(3) Uani 0.33 1 d P A 2 C8 C 0.3046(4) 0.1446(4) 0.3554(7) 0.094(3) Uani 1 1 d . . . C9 C 0.3079(3) 0.1820(3) 0.3711(8) 0.089(3) Uani 0.67 1 d P A 1 H9A H 0.3175 0.1944 0.4215 0.107 Uiso 0.67 1 calc PR A 1 N2" N 0.3079(3) 0.1820(3) 0.3711(8) 0.089(3) Uani 0.33 1 d P A 2 C10 C 0.2980(3) 0.1993(4) 0.3172(7) 0.082(3) Uani 1 1 d . . . N3 N 0.3012(3) 0.3078(3) 0.3697(6) 0.086(3) Uani 1 1 d . . . C11 C 0.2762(4) 0.2841(4) 0.3213(10) 0.103(4) Uani 1 1 d . A . H11A H 0.2577 0.2908 0.3001 0.123 Uiso 1 1 calc R . . C12 C 0.2732(4) 0.2464(4) 0.2943(11) 0.111(5) Uani 1 1 d . . . H12A H 0.2553 0.2296 0.2544 0.133 Uiso 1 1 calc R A . C13 C 0.3007(3) 0.2386(3) 0.3364(8) 0.090(3) Uani 1 1 d . A . C14 C 0.3274(4) 0.2652(4) 0.3908(9) 0.102(4) Uani 1 1 d . . . H14A H 0.3464 0.2604 0.4163 0.123 Uiso 1 1 calc R A . C15 C 0.3258(4) 0.2966(4) 0.4061(11) 0.115(5) Uani 1 1 d . A . H15A H 0.3432 0.3137 0.4462 0.138 Uiso 1 1 calc R . . N4 N 0.3392(3) 0.0860(3) 0.5256(7) 0.090(3) Uani 1 1 d . . . C16 C 0.3323(5) 0.0749(4) 0.4511(10) 0.117(5) Uani 1 1 d . A . H16A H 0.3350 0.0529 0.4351 0.141 Uiso 1 1 calc R . . C17 C 0.3212(5) 0.0938(4) 0.3927(9) 0.117(5) Uani 1 1 d . . . H17A H 0.3185 0.0861 0.3382 0.140 Uiso 1 1 calc R A . C18 C 0.3140(4) 0.1247(3) 0.4178(9) 0.095(4) Uani 1 1 d . A . C19 C 0.3216(4) 0.1358(4) 0.4929(9) 0.106(4) Uani 1 1 d . . . H19A H 0.3176 0.1564 0.5126 0.127 Uiso 1 1 calc R A . C20 C 0.3363(5) 0.1162(5) 0.5458(9) 0.109(5) Uani 1 1 d . A . H20A H 0.3443 0.1264 0.5982 0.131 Uiso 1 1 calc R . . N5 N 0.1589(3) 0.0339(3) -0.0929(8) 0.107(4) Uani 1 1 d . . . C21 C 0.1491(4) 0.0588(4) -0.1199(13) 0.128(7) Uani 1 1 d . . . H21A H 0.1698 0.0840 -0.1371 0.154 Uiso 1 1 calc R . . C22 C 0.1121(5) 0.0517(4) -0.1253(15) 0.138(7) Uani 1 1 d . . . H22A H 0.1074 0.0710 -0.1494 0.166 Uiso 1 1 calc R . . C23 C 0.0794(4) 0.0161(4) -0.0962(12) 0.108(5) Uani 1 1 d . . . C24 C 0.0894(4) -0.0094(4) -0.0680(12) 0.116(6) Uani 1 1 d . . . H24A H 0.0694 -0.0348 -0.0500 0.140 Uiso 1 1 calc R . . C25 C 0.1288(4) 0.0007(4) -0.0645(11) 0.113(5) Uani 1 1 d . . . H25A H 0.1348 -0.0176 -0.0397 0.135 Uiso 1 1 calc R . . C26 C 0.0399(4) 0.0094(3) -0.1059(11) 0.106(5) Uani 1 1 d . . . N6 N 0.0077(4) -0.0299(3) -0.1032(12) 0.122(5) Uani 0.33 1 d P . 1 C27 C 0.0077(4) -0.0299(3) -0.1032(12) 0.122(5) Uani 0.67 1 d P . 2 H27A H 0.0137 -0.0507 -0.0991 0.147 Uiso 0.67 1 calc PR . 2 Cl1 Cl 0.1721(3) 0.2043(3) 0.6295(7) 0.098(3) Uani 0.25 1 d PD B 2 Cl2 Cl 0.1870(3) 0.2241(3) 0.4350(7) 0.116(5) Uani 0.25 1 d PD B 2 C100 C 0.1425(3) 0.2111(6) 0.5719(7) 0.046(7) Uani 0.25 1 d PRDU B 2 C101 C 0.1412(3) 0.2151(3) 0.4896(7) 0.082(12) Uani 0.25 1 d PRDU B 2 C102 C 0.1085(3) 0.2144(6) 0.4544(7) 0.129(16) Uani 0.25 1 d PRU B 2 H10A H 0.1072 0.2161 0.3980 0.155 Uiso 0.25 1 calc PR B 2 C103 C 0.0777(4) 0.2112(6) 0.5016(7) 0.089(10) Uani 0.25 1 d PRU B 2 H10B H 0.0556 0.2111 0.4771 0.107 Uiso 0.25 1 calc PR B 2 C104 C 0.0787(3) 0.2082(4) 0.5820(9) 0.077(11) Uani 0.25 1 d PRU B 2 H10C H 0.0581 0.2074 0.6139 0.092 Uiso 0.25 1 calc PR B 2 C105 C 0.1110(3) 0.2062(6) 0.6192(7) 0.104(13) Uani 0.25 1 d PRU B 2 H10D H 0.1108 0.2017 0.6750 0.125 Uiso 0.25 1 calc PR B 2 O100 O 0.0923(3) 0.1386(3) -0.1960(13) 0.119(6) Uani 0.50 1 d P . . O101 O 0.1839(3) 0.1392(4) 0.2239(9) 0.069(4) Uani 0.50 1 d P . . O102 O 0.2150(7) 0.1664(7) -0.1869(15) 0.139(10) Uani 0.50 1 d P C 1 O103 O 0.1943(5) 0.1572(5) -0.1173(15) 0.111(7) Uani 0.50 1 d P D 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 0.0912(7) 0.0945(7) 0.1301(13) -0.0285(8) -0.0192(8) 0.0534(6) I1 0.1263(5) 0.1030(4) 0.1486(9) -0.0380(5) -0.0227(5) 0.0759(4) I2 0.1108(5) 0.1233(6) 0.1254(8) -0.0174(6) -0.0128(6) 0.0580(5) Zn2 0.1473(9) 0.0879(7) 0.1065(11) 0.0216(7) 0.0506(9) 0.0697(6) I3 0.2651(11) 0.1263(6) 0.1140(7) 0.0439(5) 0.0536(8) 0.1246(6) I4 0.1390(7) 0.1029(6) 0.1477(9) 0.0069(6) 0.0454(7) 0.0489(5) N1 0.140(6) 0.108(5) 0.129(9) -0.034(6) -0.033(7) 0.085(5) C1 0.113(7) 0.074(5) 0.126(11) -0.013(6) -0.006(7) 0.057(5) C2 0.125(7) 0.079(5) 0.115(10) -0.009(6) -0.029(8) 0.061(5) C3 0.143(7) 0.108(6) 0.105(10) -0.021(6) -0.019(7) 0.095(5) C4 0.236(14) 0.140(10) 0.119(12) -0.013(9) -0.028(11) 0.111(9) C5 0.214(15) 0.116(10) 0.156(15) 0.002(10) -0.031(13) 0.073(10) N2 0.109(5) 0.094(5) 0.113(9) 0.000(5) -0.008(6) 0.079(4) C7' 0.109(5) 0.094(5) 0.113(9) 0.000(5) -0.008(6) 0.079(4) C6 0.130(6) 0.094(5) 0.085(8) -0.010(5) -0.010(6) 0.084(4) C7 0.116(5) 0.085(4) 0.116(9) -0.001(5) -0.014(6) 0.077(4) N2' 0.116(5) 0.085(4) 0.116(9) -0.001(5) -0.014(6) 0.077(4) C8 0.122(6) 0.109(6) 0.072(7) -0.032(5) -0.037(6) 0.074(5) C9 0.103(6) 0.087(5) 0.088(7) -0.019(5) -0.010(6) 0.057(4) N2" 0.103(6) 0.087(5) 0.088(7) -0.019(5) -0.010(6) 0.057(4) C10 0.098(5) 0.117(6) 0.062(6) -0.001(5) -0.002(5) 0.077(4) N3 0.108(5) 0.082(4) 0.076(6) -0.008(4) 0.022(5) 0.054(4) C11 0.123(8) 0.074(6) 0.120(11) 0.002(6) -0.001(8) 0.056(5) C12 0.131(9) 0.072(6) 0.133(12) 0.002(7) 0.012(9) 0.053(6) C13 0.105(5) 0.093(5) 0.100(9) 0.000(5) 0.002(6) 0.072(4) C14 0.109(7) 0.117(8) 0.097(9) -0.012(7) 0.006(7) 0.069(6) C15 0.110(6) 0.130(8) 0.134(12) -0.041(8) -0.017(8) 0.083(6) N4 0.077(5) 0.074(5) 0.102(7) 0.013(5) -0.021(5) 0.024(4) C16 0.157(10) 0.078(6) 0.120(11) -0.015(7) -0.054(9) 0.060(6) C17 0.176(10) 0.094(6) 0.101(9) -0.024(6) -0.052(8) 0.082(6) C18 0.102(6) 0.058(5) 0.127(10) -0.020(6) -0.033(7) 0.042(4) C19 0.126(8) 0.096(7) 0.105(9) -0.039(7) -0.024(8) 0.062(6) C20 0.125(9) 0.108(9) 0.080(8) -0.026(7) -0.032(7) 0.047(7) N5 0.096(5) 0.080(5) 0.148(10) -0.026(6) -0.030(6) 0.045(4) C21 0.073(6) 0.082(7) 0.219(19) 0.019(9) -0.023(9) 0.031(6) C22 0.104(8) 0.087(7) 0.22(2) 0.014(10) -0.027(11) 0.047(6) C23 0.072(6) 0.068(6) 0.179(15) 0.005(8) 0.009(8) 0.030(5) C24 0.091(6) 0.091(7) 0.182(16) 0.014(8) -0.003(9) 0.057(5) C25 0.124(7) 0.108(7) 0.137(13) -0.003(7) -0.017(8) 0.081(5) C26 0.081(6) 0.061(5) 0.177(15) -0.009(7) -0.004(8) 0.036(4) N6 0.113(6) 0.082(5) 0.196(16) -0.011(7) -0.011(9) 0.066(5) C27 0.113(6) 0.082(5) 0.196(16) -0.011(7) -0.011(9) 0.066(5) Cl1 0.140(7) 0.107(6) 0.074(7) -0.006(5) -0.032(6) 0.082(5) Cl2 0.107(7) 0.067(6) 0.137(10) 0.001(6) 0.071(7) 0.017(6) C100 0.064(12) 0.030(10) 0.044(14) 0.010(10) 0.000(11) 0.023(9) C101 0.083(18) 0.041(14) 0.089(19) -0.008(14) -0.018(16) 0.006(12) C102 0.14(2) 0.10(2) 0.14(2) 0.004(19) 0.001(19) 0.058(15) C103 0.082(12) 0.078(13) 0.14(2) 0.013(14) -0.021(15) 0.066(10) C104 0.047(14) 0.062(15) 0.097(19) -0.003(15) 0.026(14) 0.009(11) C105 0.13(2) 0.057(15) 0.12(2) 0.009(16) -0.024(18) 0.044(13) O100 0.048(5) 0.062(5) 0.259(17) 0.099(7) 0.084(7) 0.036(4) O101 0.030(4) 0.068(6) 0.098(10) 0.020(6) -0.007(5) 0.017(4) O102 0.121(15) 0.106(14) 0.118(15) 0.017(12) -0.025(13) 0.003(12) O103 0.089(9) 0.057(7) 0.171(19) -0.007(10) 0.029(11) 0.023(7) _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 N1 2.036(13) . ? Zn1 N5 2.078(12) . ? Zn1 I2 2.525(2) . ? Zn1 I1 2.555(2) . ? Zn2 N3 2.042(10) . ? Zn2 N4 2.063(11) 12_556 ? Zn2 I3 2.537(2) . ? Zn2 I4 2.589(2) . ? N1 C1 1.352(16) . ? N1 C5 1.39(3) . ? C1 C2 1.44(2) . ? C1 H1A 0.9500 . ? C2 C3 1.27(2) . ? C2 H2A 0.9500 . ? C3 C4 1.45(2) . ? C3 C6 1.458(19) . ? C4 C5 1.38(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? N2 C6 1.348(16) . ? N2 C10 1.385(17) . ? C6 C7 1.398(18) . ? C7 C8 1.245(17) . ? C7 H7A 0.9500 . ? C8 C9 1.422(18) . ? C8 C18 1.45(2) . ? C9 C10 1.294(18) . ? C9 H9A 0.9500 . ? C10 C13 1.512(18) . ? N3 C11 1.245(17) . ? N3 C15 1.38(2) . ? C11 C12 1.48(2) . ? C11 H11A 0.9500 . ? C12 C13 1.44(2) . ? C12 H12A 0.9500 . ? C13 C14 1.379(18) . ? C14 C15 1.28(2) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? N4 C20 1.28(2) . ? N4 C16 1.30(2) . ? N4 Zn2 2.063(11) 11_556 ? C16 C17 1.42(2) . ? C16 H16A 0.9500 . ? C17 C18 1.43(2) . ? C17 H17A 0.9500 . ? C18 C19 1.31(2) . ? C19 C20 1.46(2) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? N5 C21 1.29(2) . ? N5 C25 1.325(17) . ? C21 C22 1.33(2) . ? C21 H21A 0.9500 . ? C22 C23 1.42(2) . ? C22 H22A 0.9500 . ? C23 C24 1.32(2) . ? C23 C26 1.435(19) . ? C24 C25 1.38(2) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.335(19) 2 ? C26 N6 1.335(19) 2 ? C26 N6 1.412(16) . ? N6 C26 1.335(19) 3 ? Cl1 C100 1.623(13) . ? Cl2 C101 1.8727 . ? C100 C105 1.3893 . ? C100 C101 1.3899 . ? C101 C102 1.3899 . ? C102 C103 1.3877 . ? C102 H10A 0.9500 . ? C103 C104 1.353(9) . ? C103 H10B 0.9500 . ? C104 C105 1.439(10) . ? C104 H10C 0.9500 . ? C105 H10D 0.9500 . ? 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 N1 Zn1 N5 102.7(5) . . ? N1 Zn1 I2 109.0(4) . . ? N5 Zn1 I2 110.1(4) . . ? N1 Zn1 I1 107.2(4) . . ? N5 Zn1 I1 108.5(3) . . ? I2 Zn1 I1 118.16(8) . . ? N3 Zn2 N4 103.1(4) . 12_556 ? N3 Zn2 I3 107.6(3) . . ? N4 Zn2 I3 107.4(3) 12_556 . ? N3 Zn2 I4 105.6(3) . . ? N4 Zn2 I4 107.5(4) 12_556 . ? I3 Zn2 I4 123.78(7) . . ? C1 N1 C5 120.6(15) . . ? C1 N1 Zn1 122.1(11) . . ? C5 N1 Zn1 116.9(11) . . ? N1 C1 C2 117.5(14) . . ? N1 C1 H1A 121.3 . . ? C2 C1 H1A 121.3 . . ? C3 C2 C1 123.8(12) . . ? C3 C2 H2A 118.1 . . ? C1 C2 H2A 118.1 . . ? C2 C3 C4 118.7(15) . . ? C2 C3 C6 127.1(12) . . ? C4 C3 C6 114.1(14) . . ? C5 C4 C3 118.8(19) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 N1 118.8(18) . . ? C4 C5 H5A 120.6 . . ? N1 C5 H5A 120.6 . . ? C6 N2 C10 121.0(12) . . ? N2 C6 C7 116.4(12) . . ? N2 C6 C3 120.5(12) . . ? C7 C6 C3 123.2(11) . . ? C8 C7 C6 123.8(12) . . ? C8 C7 H7A 118.1 . . ? C6 C7 H7A 118.1 . . ? C7 C8 C9 119.0(13) . . ? C7 C8 C18 121.3(12) . . ? C9 C8 C18 119.7(11) . . ? C10 C9 C8 120.5(11) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 N2 119.3(12) . . ? C9 C10 C13 119.3(11) . . ? N2 C10 C13 121.4(11) . . ? C11 N3 C15 117.5(12) . . ? C11 N3 Zn2 119.5(10) . . ? C15 N3 Zn2 122.8(9) . . ? N3 C11 C12 125.2(15) . . ? N3 C11 H11A 117.4 . . ? C12 C11 H11A 117.4 . . ? C13 C12 C11 111.1(13) . . ? C13 C12 H12A 124.4 . . ? C11 C12 H12A 124.4 . . ? C14 C13 C12 121.7(13) . . ? C14 C13 C10 123.1(12) . . ? C12 C13 C10 115.2(11) . . ? C15 C14 C13 118.1(15) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C14 C15 N3 126.0(14) . . ? C14 C15 H15A 117.0 . . ? N3 C15 H15A 117.0 . . ? C20 N4 C16 117.4(13) . . ? C20 N4 Zn2 123.6(10) . 11_556 ? C16 N4 Zn2 118.8(11) . 11_556 ? N4 C16 C17 123.7(15) . . ? N4 C16 H16A 118.2 . . ? C17 C16 H16A 118.2 . . ? C16 C17 C18 118.3(14) . . ? C16 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? C19 C18 C17 116.8(14) . . ? C19 C18 C8 126.1(13) . . ? C17 C18 C8 116.4(13) . . ? C18 C19 C20 119.4(14) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? N4 C20 C19 123.8(13) . . ? N4 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? C21 N5 C25 114.2(13) . . ? C21 N5 Zn1 121.3(9) . . ? C25 N5 Zn1 124.4(11) . . ? N5 C21 C22 124.5(14) . . ? N5 C21 H21A 117.8 . . ? C22 C21 H21A 117.8 . . ? C21 C22 C23 122.0(16) . . ? C21 C22 H22A 119.0 . . ? C23 C22 H22A 119.0 . . ? C24 C23 C22 113.6(13) . . ? C24 C23 C26 126.6(12) . . ? C22 C23 C26 119.6(14) . . ? C23 C24 C25 120.2(13) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? N5 C25 C24 125.3(15) . . ? N5 C25 H25A 117.4 . . ? C24 C25 H25A 117.4 . . ? C27 C26 N6 0.0(18) 2 2 ? C27 C26 N6 115.1(14) 2 . ? N6 C26 N6 115.1(14) 2 . ? C27 C26 C23 125.1(11) 2 . ? N6 C26 C23 125.1(11) 2 . ? N6 C26 C23 118.7(12) . . ? C26 N6 C26 124.7(14) 3 . ? C105 C100 C101 120.1 . . ? C105 C100 Cl1 106.9(6) . . ? C101 C100 Cl1 132.4(7) . . ? C102 C101 C100 120.1 . . ? C102 C101 Cl2 125.0 . . ? C100 C101 Cl2 114.9 . . ? C103 C102 C101 120.1 . . ? C103 C102 H10A 120.0 . . ? C101 C102 H10A 120.0 . . ? C104 C103 C102 120.9(2) . . ? C104 C103 H10B 119.5 . . ? C102 C103 H10B 119.5 . . ? C103 C104 C105 119.81(7) . . ? C103 C104 H10C 120.1 . . ? C105 C104 H10C 120.1 . . ? C100 C105 C104 118.8(2) . . ? C100 C105 H10D 120.6 . . ? C104 C105 H10D 120.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.753 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.251 # Attachment 'GQ269.CIF' data_gq269 _database_code_depnum_ccdc_archive 'CCDC 832652' #TrackingRef 'GQ269.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H13 Cl I2 N4 Zn, 0.25(H2 O)' _chemical_formula_sum 'C20 H13.5 Cl I2 N4 O0.25 Zn' _chemical_formula_weight 668.46 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' 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8708(17) _cell_length_b 10.5239(11) _cell_length_c 20.888(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.277(13) _cell_angle_gamma 90.00 _cell_volume 2127.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7528 _cell_measurement_theta_min 5.53 _cell_measurement_theta_max 60.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 4.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5533 _exptl_absorpt_correction_T_max 0.9208 _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 27117 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4166 _reflns_number_gt 3840 _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^)+(0.0388P)^2^+4.9419P] 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 4166 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.98698(5) 0.37982(4) 0.18682(2) 0.02429(12) Uani 1 1 d . . . I1 I 0.94762(4) 0.14394(3) 0.202874(13) 0.03880(11) Uani 1 1 d . . . I2 I 1.19734(3) 0.44161(3) 0.141890(15) 0.03734(10) Uani 1 1 d . . . N1 N 0.9835(3) 0.4680(3) 0.27446(16) 0.0249(7) Uani 1 1 d . . . N2 N 1.0156(3) 0.7412(3) 0.47632(15) 0.0241(7) Uani 1 1 d . . . N3 N 1.3152(4) 1.0368(3) 0.62933(16) 0.0274(7) Uani 1 1 d . . . N4 N 0.3598(4) 0.6531(4) 0.5617(2) 0.0347(8) Uani 1 1 d . . . Cl1 Cl 0.73272(12) 0.68256(14) 0.66791(5) 0.0427(3) Uani 1 1 d . . . C1 C 0.9147(4) 0.4125(4) 0.31596(18) 0.0233(8) Uani 1 1 d . . . H1A H 0.8769 0.3303 0.3056 0.028 Uiso 1 1 calc R . . C2 C 0.8960(4) 0.4690(4) 0.37296(19) 0.0244(8) Uani 1 1 d . . . H2A H 0.8458 0.4266 0.4010 0.029 Uiso 1 1 calc R . . C3 C 0.9516(4) 0.5888(4) 0.38901(19) 0.0256(8) Uani 1 1 d . . . C4 C 1.0292(5) 0.6436(4) 0.3483(2) 0.0319(9) Uani 1 1 d . . . H4A H 1.0728 0.7234 0.3590 0.038 Uiso 1 1 calc R . . C5 C 1.0430(5) 0.5814(4) 0.2917(2) 0.0316(9) Uani 1 1 d . . . H5A H 1.0965 0.6200 0.2639 0.038 Uiso 1 1 calc R . . C6 C 0.9212(4) 0.6570(4) 0.44726(19) 0.0241(8) Uani 1 1 d . . . C7 C 0.7979(4) 0.6352(4) 0.46713(19) 0.0261(8) Uani 1 1 d . . . H7A H 0.7347 0.5740 0.4452 0.031 Uiso 1 1 calc R . . C8 C 0.7665(4) 0.7031(4) 0.51932(18) 0.0235(8) Uani 1 1 d . . . C9 C 0.8651(4) 0.7892(4) 0.55002(18) 0.0239(8) Uani 1 1 d . . . H9A H 0.8486 0.8373 0.5862 0.029 Uiso 1 1 calc R . . C10 C 0.9868(4) 0.8047(4) 0.52791(17) 0.0220(7) Uani 1 1 d . . . C11 C 1.3163(5) 0.9932(4) 0.56910(19) 0.0284(8) Uani 1 1 d . . . H11A H 1.3938 1.0112 0.5499 0.034 Uiso 1 1 calc R . . C12 C 1.2083(4) 0.9227(4) 0.53397(19) 0.0267(8) Uani 1 1 d . . . H12A H 1.2111 0.8958 0.4908 0.032 Uiso 1 1 calc R . . C13 C 1.0970(4) 0.8916(4) 0.56149(18) 0.0232(8) Uani 1 1 d . . . C14 C 1.0938(5) 0.9417(5) 0.6227(2) 0.0378(11) Uani 1 1 d . . . H14A H 1.0160 0.9278 0.6423 0.045 Uiso 1 1 calc R . . C15 C 1.2036(5) 1.0113(6) 0.6544(2) 0.0416(12) Uani 1 1 d . . . H15A H 1.2003 1.0433 0.6966 0.050 Uiso 1 1 calc R . . C16 C 0.3831(5) 0.6610(5) 0.5015(2) 0.0361(10) Uani 1 1 d . . . H16A H 0.3064 0.6548 0.4662 0.043 Uiso 1 1 calc R . . C17 C 0.5130(4) 0.6778(4) 0.4870(2) 0.0303(9) Uani 1 1 d . . . H17A H 0.5227 0.6831 0.4428 0.036 Uiso 1 1 calc R . . C18 C 0.6293(4) 0.6870(4) 0.53650(19) 0.0250(8) Uani 1 1 d . . . C19 C 0.6037(4) 0.6786(4) 0.5996(2) 0.0280(8) Uani 1 1 d . . . C20 C 0.4685(5) 0.6617(4) 0.6091(2) 0.0311(9) Uani 1 1 d . . . H20A H 0.4543 0.6559 0.6527 0.037 Uiso 1 1 calc R . . O1 O 1.000(5) 0.813(3) 0.3087(12) 0.148(16) Uani 0.25 1 d P . . 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 0.0297(2) 0.0236(2) 0.0194(2) 0.00181(17) 0.00441(17) 0.00471(18) I1 0.0645(2) 0.02459(16) 0.02528(15) -0.00185(10) 0.00386(13) -0.00504(13) I2 0.03965(17) 0.03993(19) 0.03643(17) -0.00070(12) 0.01725(13) -0.00234(12) N1 0.0282(17) 0.0215(16) 0.0248(16) 0.0004(13) 0.0043(13) 0.0036(13) N2 0.0270(16) 0.0227(16) 0.0209(15) -0.0014(13) 0.0005(13) 0.0002(13) N3 0.0311(17) 0.0281(18) 0.0225(16) -0.0044(13) 0.0040(13) -0.0049(14) N4 0.034(2) 0.032(2) 0.039(2) 0.0072(16) 0.0096(16) 0.0005(16) Cl1 0.0395(6) 0.0611(8) 0.0241(5) 0.0081(5) -0.0020(4) 0.0011(5) C1 0.0276(19) 0.0207(18) 0.0209(17) -0.0005(14) 0.0028(15) -0.0022(15) C2 0.0273(19) 0.0217(19) 0.0234(18) -0.0009(15) 0.0028(15) 0.0016(15) C3 0.0230(18) 0.028(2) 0.0242(19) -0.0050(16) 0.0017(15) 0.0016(16) C4 0.033(2) 0.030(2) 0.033(2) -0.0079(17) 0.0072(18) -0.0066(17) C5 0.037(2) 0.028(2) 0.032(2) -0.0014(17) 0.0112(18) -0.0045(18) C6 0.0256(19) 0.0222(19) 0.0225(18) -0.0041(15) -0.0001(15) 0.0009(15) C7 0.029(2) 0.025(2) 0.0220(18) -0.0030(15) -0.0007(15) -0.0009(16) C8 0.0255(18) 0.0227(19) 0.0204(17) 0.0027(15) -0.0004(14) 0.0049(15) C9 0.031(2) 0.0194(18) 0.0192(17) -0.0013(14) 0.0005(15) 0.0018(15) C10 0.0278(18) 0.0173(17) 0.0182(16) 0.0009(14) -0.0021(14) 0.0018(15) C11 0.035(2) 0.028(2) 0.0218(18) -0.0035(16) 0.0045(16) -0.0080(17) C12 0.035(2) 0.026(2) 0.0191(18) -0.0027(15) 0.0051(16) -0.0009(17) C13 0.0305(19) 0.0198(18) 0.0180(17) 0.0013(14) 0.0011(14) 0.0022(15) C14 0.033(2) 0.058(3) 0.024(2) -0.015(2) 0.0106(18) -0.014(2) C15 0.036(2) 0.062(3) 0.028(2) -0.020(2) 0.0090(18) -0.013(2) C16 0.031(2) 0.037(2) 0.038(2) 0.0030(19) 0.0014(18) -0.0010(19) C17 0.032(2) 0.030(2) 0.028(2) 0.0020(17) 0.0037(16) -0.0018(17) C18 0.032(2) 0.0163(18) 0.0266(19) 0.0007(15) 0.0068(16) 0.0022(15) C19 0.036(2) 0.0190(18) 0.0265(19) 0.0024(15) 0.0003(16) 0.0028(16) C20 0.042(2) 0.024(2) 0.031(2) 0.0037(16) 0.0147(18) 0.0019(17) O1 0.32(5) 0.075(16) 0.070(15) -0.025(13) 0.08(2) -0.08(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 Zn1 N1 2.059(3) . ? Zn1 N3 2.071(3) 4_575 ? Zn1 I2 2.5253(7) . ? Zn1 I1 2.5449(6) . ? N1 C1 1.336(5) . ? N1 C5 1.347(6) . ? N2 C6 1.342(5) . ? N2 C10 1.345(5) . ? N3 C15 1.337(6) . ? N3 C11 1.341(5) . ? N3 Zn1 2.071(3) 4_676 ? N4 C20 1.312(6) . ? N4 C16 1.325(6) . ? Cl1 C19 1.717(4) . ? C1 C2 1.375(6) . ? C1 H1A 0.9500 . ? C2 C3 1.390(6) . ? C2 H2A 0.9500 . ? C3 C4 1.377(6) . ? C3 C6 1.493(5) . ? C4 C5 1.381(6) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.380(6) . ? C7 C8 1.388(6) . ? C7 H7A 0.9500 . ? C8 C9 1.391(6) . ? C8 C18 1.478(6) . ? C9 C10 1.378(6) . ? C9 H9A 0.9500 . ? C10 C13 1.488(5) . ? C11 C12 1.386(6) . ? C11 H11A 0.9500 . ? C12 C13 1.375(6) . ? C12 H12A 0.9500 . ? C13 C14 1.389(6) . ? C14 C15 1.367(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.384(6) . ? C16 H16A 0.9500 . ? C17 C18 1.390(6) . ? C17 H17A 0.9500 . ? C18 C19 1.393(6) . ? C19 C20 1.399(6) . ? C20 H20A 0.9500 . ? 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 N1 Zn1 N3 99.83(13) . 4_575 ? N1 Zn1 I2 111.86(10) . . ? N3 Zn1 I2 108.34(10) 4_575 . ? N1 Zn1 I1 107.04(10) . . ? N3 Zn1 I1 111.15(10) 4_575 . ? I2 Zn1 I1 117.25(2) . . ? C1 N1 C5 117.6(4) . . ? C1 N1 Zn1 118.6(3) . . ? C5 N1 Zn1 123.7(3) . . ? C6 N2 C10 117.0(3) . . ? C15 N3 C11 117.2(4) . . ? C15 N3 Zn1 120.1(3) . 4_676 ? C11 N3 Zn1 122.2(3) . 4_676 ? C20 N4 C16 116.3(4) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 119.2(4) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 118.1(4) . . ? C4 C3 C6 121.8(4) . . ? C2 C3 C6 120.0(4) . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? N1 C5 C4 122.6(4) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? N2 C6 C7 123.3(4) . . ? N2 C6 C3 117.0(4) . . ? C7 C6 C3 119.7(3) . . ? C6 C7 C8 119.7(4) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C7 C8 C9 117.0(4) . . ? C7 C8 C18 119.2(4) . . ? C9 C8 C18 123.7(4) . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C10 C9 123.0(3) . . ? N2 C10 C13 115.7(3) . . ? C9 C10 C13 121.3(3) . . ? N3 C11 C12 122.2(4) . . ? N3 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 117.3(4) . . ? C12 C13 C10 121.3(3) . . ? C14 C13 C10 121.4(4) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N3 C15 C14 123.6(4) . . ? N3 C15 H15A 118.2 . . ? C14 C15 H15A 118.2 . . ? N4 C16 C17 123.7(4) . . ? N4 C16 H16A 118.1 . . ? C17 C16 H16A 118.1 . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C19 115.0(4) . . ? C17 C18 C8 119.4(4) . . ? C19 C18 C8 125.6(4) . . ? C18 C19 C20 119.8(4) . . ? C18 C19 Cl1 122.9(3) . . ? C20 C19 Cl1 117.3(3) . . ? N4 C20 C19 124.3(4) . . ? N4 C20 H20A 117.8 . . ? C19 C20 H20A 117.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.105 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.128 # Attachment 'GQ270.CIF' data_gq270 _database_code_depnum_ccdc_archive 'CCDC 832653' #TrackingRef 'GQ270.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H13 Cl3 N4 Zn' _chemical_formula_sum 'C20 H13 Cl3 N4 Zn' _chemical_formula_weight 481.08 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' 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 Orthorhombic _symmetry_space_group_name_H-M Pbca _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' '-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 17.353(3) _cell_length_b 10.3148(16) _cell_length_c 20.974(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3754.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1999 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 67.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_T_max 0.7211 _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 77342 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 29.25 _reflns_number_total 5068 _reflns_number_gt 4931 _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^)+(0.0286P)^2^+4.7705P] 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 5068 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.000 _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 0.086011(12) 0.36089(2) 0.328749(10) 0.01955(7) Uani 1 1 d . . . Cl1 Cl 0.10929(3) 0.15150(5) 0.31715(3) 0.03245(12) Uani 1 1 d . . . Cl2 Cl -0.03592(3) 0.42347(5) 0.33730(3) 0.02878(11) Uani 1 1 d . . . Cl3 Cl 0.49967(3) 0.82476(6) -0.02757(2) 0.03385(12) Uani 1 1 d . . . N1 N 0.13660(9) 0.44699(15) 0.25066(7) 0.0204(3) Uani 1 1 d . . . N2 N 0.22715(9) 0.75233(15) 0.07961(7) 0.0202(3) Uani 1 1 d . . . N3 N 0.14371(9) 1.04821(17) -0.09831(8) 0.0242(3) Uani 1 1 d . . . N4 N 0.63240(10) 0.81927(18) 0.12413(10) 0.0334(4) Uani 1 1 d . . . C1 C 0.21037(11) 0.41697(17) 0.23652(9) 0.0213(3) Uani 1 1 d . . . H1A H 0.2329 0.3434 0.2564 0.026 Uiso 1 1 calc R . . C2 C 0.25459(11) 0.48813(18) 0.19458(9) 0.0210(3) Uani 1 1 d . . . H2A H 0.3068 0.4653 0.1867 0.025 Uiso 1 1 calc R . . C3 C 0.22124(10) 0.59445(17) 0.16383(8) 0.0188(3) Uani 1 1 d . . . C4 C 0.14333(11) 0.61984(18) 0.17478(9) 0.0230(4) Uani 1 1 d . . . H4A H 0.1178 0.6872 0.1522 0.028 Uiso 1 1 calc R . . C5 C 0.10371(11) 0.54561(18) 0.21893(9) 0.0227(3) Uani 1 1 d . . . H5A H 0.0511 0.5652 0.2271 0.027 Uiso 1 1 calc R . . C6 C 0.26707(10) 0.68149(17) 0.12213(8) 0.0188(3) Uani 1 1 d . . . C7 C 0.34665(10) 0.69149(17) 0.12966(9) 0.0203(3) Uani 1 1 d . . . H7A H 0.3727 0.6385 0.1598 0.024 Uiso 1 1 calc R . . C8 C 0.38774(10) 0.78000(17) 0.09252(8) 0.0195(3) Uani 1 1 d . . . C9 C 0.34622(11) 0.85469(18) 0.04973(9) 0.0219(3) Uani 1 1 d . . . H9A H 0.3716 0.9180 0.0244 0.026 Uiso 1 1 calc R . . C10 C 0.26702(10) 0.83652(17) 0.04403(8) 0.0195(3) Uani 1 1 d . . . C11 C 0.10983(11) 1.01702(19) -0.04276(9) 0.0253(4) Uani 1 1 d . . . H11A H 0.0578 1.0426 -0.0361 0.030 Uiso 1 1 calc R . . C12 C 0.14694(11) 0.94967(19) 0.00510(9) 0.0235(4) Uani 1 1 d . . . H12A H 0.1209 0.9296 0.0437 0.028 Uiso 1 1 calc R . . C13 C 0.22324(10) 0.91152(18) -0.00416(8) 0.0203(3) Uani 1 1 d . . . C14 C 0.25792(11) 0.9422(2) -0.06166(9) 0.0283(4) Uani 1 1 d . . . H14A H 0.3096 0.9168 -0.0698 0.034 Uiso 1 1 calc R . . C15 C 0.21704(11) 1.0098(2) -0.10691(10) 0.0307(4) Uani 1 1 d . . . H15A H 0.2417 1.0304 -0.1461 0.037 Uiso 1 1 calc R . . C16 C 0.58241(12) 0.7999(2) 0.17140(11) 0.0311(4) Uani 1 1 d . . . H16A H 0.6016 0.7963 0.2138 0.037 Uiso 1 1 calc R . . C17 C 0.50387(11) 0.7847(2) 0.16205(10) 0.0257(4) Uani 1 1 d . . . H17A H 0.4713 0.7676 0.1975 0.031 Uiso 1 1 calc R . . C18 C 0.47233(10) 0.79431(17) 0.10118(9) 0.0208(3) Uani 1 1 d . . . C19 C 0.52539(11) 0.81594(18) 0.05208(10) 0.0241(4) Uani 1 1 d . . . C20 C 0.60351(12) 0.8261(2) 0.06585(12) 0.0302(4) Uani 1 1 d . . . H20A H 0.6382 0.8387 0.0314 0.036 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 Zn1 0.01922(11) 0.01924(11) 0.02019(11) -0.00090(7) -0.00004(7) -0.00132(7) Cl1 0.0422(3) 0.0197(2) 0.0354(3) -0.00066(18) -0.0075(2) 0.00425(19) Cl2 0.0193(2) 0.0297(2) 0.0373(2) 0.00145(19) 0.00257(17) 0.00154(17) Cl3 0.0351(3) 0.0405(3) 0.0259(2) -0.0023(2) 0.00752(19) -0.0054(2) N1 0.0213(7) 0.0190(7) 0.0208(7) -0.0002(6) 0.0010(5) -0.0013(6) N2 0.0206(7) 0.0210(7) 0.0189(7) 0.0002(6) 0.0003(5) 0.0001(6) N3 0.0219(7) 0.0270(8) 0.0238(7) 0.0065(6) -0.0020(6) -0.0016(6) N4 0.0213(8) 0.0290(9) 0.0498(11) 0.0004(8) 0.0009(8) -0.0004(7) C1 0.0224(8) 0.0190(8) 0.0224(8) 0.0005(6) -0.0009(6) 0.0029(6) C2 0.0189(7) 0.0211(8) 0.0229(8) 0.0004(6) 0.0002(6) 0.0021(6) C3 0.0191(8) 0.0180(7) 0.0192(7) -0.0011(6) 0.0001(6) -0.0008(6) C4 0.0206(8) 0.0212(8) 0.0271(9) 0.0033(7) -0.0004(7) 0.0024(7) C5 0.0184(8) 0.0221(8) 0.0277(9) 0.0007(7) 0.0018(7) 0.0009(6) C6 0.0208(8) 0.0174(7) 0.0182(7) -0.0008(6) 0.0004(6) 0.0000(6) C7 0.0206(8) 0.0187(8) 0.0215(8) 0.0015(6) -0.0009(6) 0.0017(6) C8 0.0185(7) 0.0200(8) 0.0200(7) -0.0014(6) 0.0023(6) 0.0001(6) C9 0.0217(8) 0.0224(8) 0.0216(8) 0.0031(6) 0.0016(6) -0.0012(7) C10 0.0205(8) 0.0204(8) 0.0178(7) 0.0007(6) 0.0005(6) 0.0010(6) C11 0.0238(9) 0.0265(9) 0.0256(9) 0.0025(7) 0.0028(7) 0.0056(7) C12 0.0234(8) 0.0257(9) 0.0213(8) 0.0017(7) 0.0040(7) 0.0022(7) C13 0.0208(8) 0.0205(8) 0.0195(8) 0.0018(6) -0.0003(6) -0.0009(6) C14 0.0162(8) 0.0440(12) 0.0247(9) 0.0082(8) 0.0010(7) -0.0009(8) C15 0.0196(9) 0.0466(12) 0.0260(9) 0.0117(9) 0.0013(7) -0.0026(8) C16 0.0239(9) 0.0304(10) 0.0388(11) 0.0032(9) -0.0047(8) 0.0001(8) C17 0.0216(9) 0.0275(9) 0.0281(9) 0.0023(7) 0.0011(7) 0.0014(7) C18 0.0197(8) 0.0173(7) 0.0255(8) -0.0004(6) 0.0021(6) 0.0006(6) C19 0.0267(9) 0.0193(8) 0.0264(9) -0.0013(7) 0.0052(7) -0.0013(7) C20 0.0230(9) 0.0224(9) 0.0451(12) -0.0022(8) 0.0095(8) -0.0021(7) _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 N3 2.0547(16) 7_576 ? Zn1 N1 2.0596(16) . ? Zn1 Cl1 2.2107(6) . ? Zn1 Cl2 2.2193(6) . ? Cl3 C19 1.731(2) . ? N1 C5 1.343(2) . ? N1 C1 1.350(2) . ? N2 C10 1.338(2) . ? N2 C6 1.345(2) . ? N3 C11 1.344(2) . ? N3 C15 1.345(3) . ? N3 Zn1 2.0547(16) 7_575 ? N4 C20 1.323(3) . ? N4 C16 1.332(3) . ? C1 C2 1.379(3) . ? C1 H1A 0.9500 . ? C2 C3 1.398(2) . ? C2 H2A 0.9500 . ? C3 C4 1.396(3) . ? C3 C6 1.484(2) . ? C4 C5 1.384(3) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.394(2) . ? C7 C8 1.396(2) . ? C7 H7A 0.9500 . ? C8 C9 1.385(3) . ? C8 C18 1.486(2) . ? C9 C10 1.392(3) . ? C9 H9A 0.9500 . ? C10 C13 1.482(2) . ? C11 C12 1.380(3) . ? C11 H11A 0.9500 . ? C12 C13 1.395(3) . ? C12 H12A 0.9500 . ? C13 C14 1.384(3) . ? C14 C15 1.375(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.386(3) . ? C16 H16A 0.9500 . ? C17 C18 1.393(3) . ? C17 H17A 0.9500 . ? C18 C19 1.399(3) . ? C19 C20 1.390(3) . ? C20 H20A 0.9500 . ? 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 N3 Zn1 N1 100.82(7) 7_576 . ? N3 Zn1 Cl1 116.02(5) 7_576 . ? N1 Zn1 Cl1 104.83(5) . . ? N3 Zn1 Cl2 105.76(5) 7_576 . ? N1 Zn1 Cl2 110.19(5) . . ? Cl1 Zn1 Cl2 117.86(2) . . ? C5 N1 C1 117.89(16) . . ? C5 N1 Zn1 122.66(13) . . ? C1 N1 Zn1 118.68(12) . . ? C10 N2 C6 117.14(16) . . ? C11 N3 C15 117.37(17) . . ? C11 N3 Zn1 122.79(13) . 7_575 ? C15 N3 Zn1 119.70(13) . 7_575 ? C20 N4 C16 116.66(18) . . ? N1 C1 C2 123.07(17) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 118.80(17) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 118.18(16) . . ? C4 C3 C6 120.14(16) . . ? C2 C3 C6 121.65(16) . . ? C5 C4 C3 119.15(17) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? N1 C5 C4 122.65(17) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? N2 C6 C7 123.04(16) . . ? N2 C6 C3 116.32(15) . . ? C7 C6 C3 120.58(16) . . ? C6 C7 C8 119.42(16) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 117.37(17) . . ? C9 C8 C18 122.53(16) . . ? C7 C8 C18 120.07(16) . . ? C8 C9 C10 119.62(17) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? N2 C10 C9 123.37(17) . . ? N2 C10 C13 117.01(16) . . ? C9 C10 C13 119.61(16) . . ? N3 C11 C12 123.16(18) . . ? N3 C11 H11A 118.4 . . ? C12 C11 H11A 118.4 . . ? C11 C12 C13 118.92(17) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 117.99(17) . . ? C14 C13 C10 119.38(17) . . ? C12 C13 C10 122.60(16) . . ? C15 C14 C13 119.55(18) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? N3 C15 C14 123.01(18) . . ? N3 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? N4 C16 C17 123.5(2) . . ? N4 C16 H16A 118.3 . . ? C17 C16 H16A 118.3 . . ? C16 C17 C18 120.55(19) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C19 115.30(17) . . ? C17 C18 C8 119.55(16) . . ? C19 C18 C8 125.15(17) . . ? C20 C19 C18 120.06(19) . . ? C20 C19 Cl3 116.60(16) . . ? C18 C19 Cl3 123.29(15) . . ? N4 C20 C19 123.9(2) . . ? N4 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.906 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.068 # Attachment 'SQUEEZE143.CIF' data_squeeze _database_code_depnum_ccdc_archive 'CCDC 832654' #TrackingRef 'SQUEEZE143.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H90 Cl12 N18 Zn6' _chemical_formula_sum 'C138 H90 Cl12 N18 Zn6' _chemical_formula_weight 2818.03 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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.793(2) _cell_length_b 23.662(6) _cell_length_c 24.672(6) _cell_angle_alpha 68.897(19) _cell_angle_beta 87.31(2) _cell_angle_gamma 80.27(2) _cell_volume 4719(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 36.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7300 _exptl_absorpt_correction_T_max 0.9101 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; Crystals are unstable out of solvent and diffract poorly. Of many datasets on different crystals, this was the best. This structure contains large voids in which very little solvent could be identified. It is probable the solvent in these voids is so disordered that the electron density is too smeared to create peaks in the difference map, hence why SQUEEZE has been used. ; _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 16722 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.05 _reflns_number_total 16722 _reflns_number_gt 14711 _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^)+(0.1471P)^2^+4.8540P] 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 16722 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.2271 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _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 0.01360(7) 0.50307(3) 0.68114(2) 0.05455(18) Uani 1 1 d . . . Cl1 Cl 0.02823(18) 0.40388(7) 0.69715(6) 0.0681(4) Uani 1 1 d . . . Cl2 Cl -0.20947(16) 0.56465(8) 0.64934(6) 0.0712(4) Uani 1 1 d . . . Zn2 Zn 0.32103(6) 0.62991(2) 0.15015(2) 0.04608(16) Uani 1 1 d . . . Cl3 Cl 0.17733(16) 0.55675(6) 0.17149(5) 0.0571(3) Uani 1 1 d . . . Cl4 Cl 0.48659(16) 0.64414(6) 0.07796(5) 0.0596(3) Uani 1 1 d . . . Zn3 Zn 0.37368(6) 1.19749(2) -0.01431(3) 0.05230(17) Uani 1 1 d . . . Cl5 Cl 0.40431(17) 1.20958(7) -0.10743(6) 0.0658(3) Uani 1 1 d . . . N1 N 0.1785(5) 0.5320(2) 0.62029(17) 0.0564(10) Uani 1 1 d . . . N2 N 0.4723(5) 0.5936(2) 0.43584(17) 0.0528(9) Uani 1 1 d . . . N3 N 0.4213(5) 0.6190(2) 0.22727(17) 0.0527(9) Uani 1 1 d . . . C1 C 0.2953(7) 0.5575(3) 0.6292(2) 0.0694(16) Uani 1 1 d . . . H1A H 0.3012 0.5621 0.6658 0.083 Uiso 1 1 calc R . . C2 C 0.4066(6) 0.5775(3) 0.5898(2) 0.0557(12) Uani 1 1 d . . . H2A H 0.4857 0.5962 0.5980 0.067 Uiso 1 1 calc R . . C3 C 0.3983(6) 0.5690(2) 0.5355(2) 0.0522(11) Uani 1 1 d . . . C4 C 0.2791(6) 0.5429(2) 0.5264(2) 0.0562(12) Uani 1 1 d . . . H4A H 0.2711 0.5371 0.4906 0.067 Uiso 1 1 calc R . . C5 C 0.1715(6) 0.5252(3) 0.5681(2) 0.0581(12) Uani 1 1 d . . . H5A H 0.0893 0.5076 0.5604 0.070 Uiso 1 1 calc R . . Cl6 Cl 0.57778(16) 1.16788(7) 0.04456(7) 0.0695(4) Uani 1 1 d . . . C6 C 0.5130(6) 0.5916(2) 0.4886(2) 0.0543(11) Uani 1 1 d . . . C7 C 0.6457(6) 0.6106(3) 0.4983(2) 0.0580(12) Uani 1 1 d . . . H7A H 0.6714 0.6069 0.5366 0.070 Uiso 1 1 calc R . . C8 C 0.7420(6) 0.6352(3) 0.4525(2) 0.0554(11) Uani 1 1 d . . . C9 C 0.6972(6) 0.6384(3) 0.3972(2) 0.0541(11) Uani 1 1 d . . . H9A H 0.7569 0.6559 0.3641 0.065 Uiso 1 1 calc R . . C10 C 0.5651(6) 0.6160(2) 0.3915(2) 0.0517(11) Uani 1 1 d . . . C11 C 0.3740(6) 0.5805(3) 0.2776(2) 0.0571(12) Uani 1 1 d . . . H11A H 0.3080 0.5531 0.2764 0.069 Uiso 1 1 calc R . . C12 C 0.4179(6) 0.5795(3) 0.3310(2) 0.0571(12) Uani 1 1 d . . . H12A H 0.3782 0.5532 0.3657 0.068 Uiso 1 1 calc R . . C13 C 0.5189(6) 0.6166(2) 0.3340(2) 0.0533(11) Uani 1 1 d . . . C14 C 0.5705(7) 0.6554(3) 0.2815(2) 0.0611(13) Uani 1 1 d . . . H14A H 0.6411 0.6816 0.2817 0.073 Uiso 1 1 calc R . . C15 C 0.5190(6) 0.6556(2) 0.2296(2) 0.0542(11) Uani 1 1 d . . . H15A H 0.5540 0.6826 0.1943 0.065 Uiso 1 1 calc R . . C16 C 0.8821(6) 0.6582(3) 0.4600(2) 0.0604(12) Uani 1 1 d . . . C17 C 0.8937(8) 0.6799(3) 0.5051(3) 0.0757(16) Uani 1 1 d . . . H17A H 0.8125 0.6780 0.5322 0.091 Uiso 1 1 calc R . . C18 C 1.0237(9) 0.7042(4) 0.5109(3) 0.086(2) Uani 1 1 d . . . H18A H 1.0294 0.7193 0.5415 0.103 Uiso 1 1 calc R . . C19 C 1.1439(7) 0.7065(3) 0.4724(3) 0.0742(16) Uani 1 1 d . . . C20 C 1.1327(7) 0.6844(3) 0.4282(3) 0.0667(14) Uani 1 1 d . . . H20A H 1.2149 0.6857 0.4017 0.080 Uiso 1 1 calc R . . C21 C 1.0043(6) 0.6606(3) 0.4219(2) 0.0602(12) Uani 1 1 d . . . H21A H 0.9997 0.6457 0.3911 0.072 Uiso 1 1 calc R . . C22 C 1.2766(9) 0.7314(3) 0.4795(4) 0.089(2) Uani 1 1 d . . . C23 C 1.3866(10) 0.7503(5) 0.4847(4) 0.114(3) Uani 1 1 d . . . H23 H 1.4766 0.7657 0.4890 0.137 Uiso 1 1 calc R . . N4 N 0.1832(4) 0.71282(18) 0.13451(17) 0.0493(9) Uani 1 1 d . . . N5 N 0.0131(5) 0.93701(18) 0.09018(19) 0.0526(9) Uani 1 1 d . . . N6 N 0.2311(5) 1.13243(19) 0.0170(2) 0.0553(10) Uani 1 1 d . . . C24 C 0.2216(6) 0.7645(2) 0.0947(2) 0.0552(12) Uani 1 1 d . . . H24A H 0.3074 0.7609 0.0707 0.066 Uiso 1 1 calc R . . C25 C 0.1441(6) 0.8215(2) 0.0873(2) 0.0568(12) Uani 1 1 d . . . H25A H 0.1752 0.8566 0.0585 0.068 Uiso 1 1 calc R . . C26 C 0.0180(5) 0.8280(2) 0.1225(2) 0.0498(10) Uani 1 1 d . . . C27 C -0.0236(6) 0.7752(2) 0.1625(2) 0.0570(12) Uani 1 1 d . . . H27A H -0.1105 0.7775 0.1864 0.068 Uiso 1 1 calc R . . C28 C 0.0615(6) 0.7190(2) 0.1675(2) 0.0550(11) Uani 1 1 d . . . H28A H 0.0324 0.6831 0.1958 0.066 Uiso 1 1 calc R . . C29 C -0.0655(6) 0.8908(2) 0.1153(2) 0.0503(10) Uani 1 1 d . . . C30 C -0.2145(5) 0.8993(2) 0.1347(2) 0.0530(11) Uani 1 1 d . . . H30A H -0.2651 0.8651 0.1537 0.064 Uiso 1 1 calc R . . C31 C -0.2897(6) 0.9586(2) 0.1261(2) 0.0538(11) Uani 1 1 d . . . C32 C -0.2087(6) 1.0062(2) 0.0991(2) 0.0547(11) Uani 1 1 d . . . H32A H -0.2576 1.0474 0.0910 0.066 Uiso 1 1 calc R . . C33 C -0.0566(6) 0.9941(2) 0.0838(2) 0.0519(11) Uani 1 1 d . . . C34 C 0.2773(6) 1.0751(2) 0.0180(2) 0.0563(12) Uani 1 1 d . . . H34A H 0.3783 1.0647 0.0053 0.068 Uiso 1 1 calc R . . C35 C 0.1839(6) 1.0306(2) 0.0368(2) 0.0523(11) Uani 1 1 d . . . H35A H 0.2192 0.9912 0.0348 0.063 Uiso 1 1 calc R . . C36 C 0.0407(6) 1.0426(2) 0.0585(2) 0.0524(11) Uani 1 1 d . . . C37 C -0.0089(5) 1.1045(2) 0.0620(3) 0.0613(15) Uani 1 1 d . . . H37A H -0.1018 1.1149 0.0800 0.074 Uiso 1 1 calc R . . C38 C 0.0892(6) 1.1445(2) 0.0375(3) 0.0687(15) Uani 1 1 d . . . H38A H 0.0543 1.1858 0.0343 0.082 Uiso 1 1 calc R . . C39 C -0.4512(6) 0.9688(2) 0.1466(2) 0.0583(12) Uani 1 1 d . . . C40 C -0.5480(6) 0.9267(2) 0.1530(2) 0.0558(12) Uani 1 1 d . . . H40A H -0.5128 0.8916 0.1430 0.067 Uiso 1 1 calc R . . C41 C -0.6965(6) 0.9351(3) 0.1740(3) 0.0639(13) Uani 1 1 d . . . H41A H -0.7618 0.9057 0.1782 0.077 Uiso 1 1 calc R . . C42 C -0.7493(6) 0.9861(3) 0.1886(2) 0.0637(13) Uani 1 1 d . . . C43 C -0.6532(7) 1.0281(3) 0.1820(3) 0.0739(16) Uani 1 1 d . . . H43A H -0.6890 1.0634 0.1917 0.089 Uiso 1 1 calc R . . C44 C -0.5054(7) 1.0200(3) 0.1614(3) 0.0707(15) Uani 1 1 d . . . H44A H -0.4405 1.0496 0.1573 0.085 Uiso 1 1 calc R . . C45 C -0.9043(7) 0.9952(3) 0.2110(3) 0.0756(16) Uani 1 1 d . . . N7 N 0.2393(4) 1.27160(18) -0.00478(17) 0.0488(9) Uani 1 1 d . . . N8 N -0.0607(5) 1.42495(19) 0.07215(18) 0.0517(9) Uani 1 1 d . . . N9 N -0.0847(5) 1.4821(2) 0.24841(17) 0.0536(9) Uani 1 1 d . . . C46 C -1.0293(9) 1.0025(4) 0.2280(4) 0.104(3) Uani 1 1 d . . . H46 H -1.1313 1.0084 0.2418 0.125 Uiso 1 1 calc R . . C47 C 0.2461(8) 1.2859(3) 0.0428(3) 0.0724(17) Uani 1 1 d . . . H47A H 0.3243 1.2630 0.0712 0.087 Uiso 1 1 calc R . . C48 C 0.1448(7) 1.3321(3) 0.0523(3) 0.0725(16) Uani 1 1 d . . . H48A H 0.1483 1.3385 0.0880 0.087 Uiso 1 1 calc R . . C49 C 0.0382(6) 1.3692(2) 0.0101(2) 0.0517(11) Uani 1 1 d . . . C50 C 0.0399(8) 1.3579(3) -0.0403(3) 0.0728(17) Uani 1 1 d . . . H50A H -0.0277 1.3839 -0.0715 0.087 Uiso 1 1 calc R . . C51 C 0.1395(7) 1.3089(3) -0.0461(2) 0.0655(14) Uani 1 1 d . . . H51A H 0.1367 1.3014 -0.0814 0.079 Uiso 1 1 calc R . . C52 C -0.0707(6) 1.4212(2) 0.0191(2) 0.0513(11) Uani 1 1 d . . . C53 C -0.1729(6) 1.4611(2) -0.0233(2) 0.0525(11) Uani 1 1 d . . . H53A H -0.1758 1.4563 -0.0599 0.063 Uiso 1 1 calc R . . C54 C -0.2722(5) 1.5086(2) -0.0134(2) 0.0487(10) Uani 1 1 d . . . C55 C -0.2618(6) 1.5120(2) 0.0421(2) 0.0522(11) Uani 1 1 d . . . H55A H -0.3286 1.5429 0.0517 0.063 Uiso 1 1 calc R . . C56 C -0.1552(5) 1.4708(2) 0.0827(2) 0.0496(10) Uani 1 1 d . . . C57 C -0.0107(8) 1.4349(3) 0.2335(2) 0.0676(15) Uani 1 1 d . . . H57A H 0.0574 1.4032 0.2611 0.081 Uiso 1 1 calc R . . C58 C -0.0299(7) 1.4309(3) 0.1804(3) 0.0695(15) Uani 1 1 d . . . H58A H 0.0309 1.3988 0.1706 0.083 Uiso 1 1 calc R . . C59 C -0.1369(6) 1.4733(2) 0.1408(2) 0.0551(11) Uani 1 1 d . . . C60 C -0.2191(6) 1.5199(3) 0.1579(2) 0.0644(14) Uani 1 1 d . . . H60A H -0.2965 1.5496 0.1329 0.077 Uiso 1 1 calc R . . C61 C -0.1875(6) 1.5228(3) 0.2110(2) 0.0618(13) Uani 1 1 d . . . H61A H -0.2425 1.5557 0.2211 0.074 Uiso 1 1 calc R . . C62 C -0.3830(6) 1.5527(2) -0.0584(2) 0.0522(11) Uani 1 1 d . . . C63 C -0.3929(8) 1.5479(3) -0.1120(3) 0.0779(18) Uani 1 1 d . . . H63A H -0.3265 1.5160 -0.1202 0.093 Uiso 1 1 calc R . . C64 C -0.4969(10) 1.5882(3) -0.1541(3) 0.090(2) Uani 1 1 d . . . H64A H -0.5011 1.5836 -0.1906 0.108 Uiso 1 1 calc R . . C65 C -0.5936(7) 1.6346(3) -0.1438(3) 0.0754(17) Uani 1 1 d . . . C67 C -0.4866(7) 1.5984(3) -0.0477(3) 0.0706(15) Uani 1 1 d . . . H67A H -0.4870 1.6018 -0.0105 0.085 Uiso 1 1 calc R . . C66 C -0.5893(8) 1.6390(3) -0.0901(3) 0.0762(17) Uani 1 1 d . . . H66A H -0.6580 1.6704 -0.0819 0.091 Uiso 1 1 calc R . . C68 C -0.7062(10) 1.6763(4) -0.1870(4) 0.101(3) Uani 1 1 d . . . C69 C -0.7987(15) 1.7094(5) -0.2217(6) 0.155(5) Uani 1 1 d . . . H69 H -0.8737 1.7362 -0.2497 0.186 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 Zn1 0.0500(3) 0.0717(4) 0.0435(3) -0.0216(3) -0.0031(2) -0.0110(3) Cl1 0.0718(8) 0.0765(9) 0.0665(8) -0.0375(7) 0.0132(6) -0.0166(7) Cl2 0.0569(7) 0.0907(10) 0.0568(7) -0.0163(7) -0.0123(6) -0.0066(7) Zn2 0.0468(3) 0.0466(3) 0.0441(3) -0.0186(2) -0.0068(2) 0.0016(2) Cl3 0.0675(8) 0.0569(7) 0.0509(6) -0.0220(5) -0.0043(5) -0.0135(6) Cl4 0.0655(8) 0.0558(7) 0.0531(6) -0.0204(5) 0.0069(5) 0.0023(6) Zn3 0.0442(3) 0.0427(3) 0.0680(4) -0.0199(3) 0.0008(2) -0.0016(2) Cl5 0.0708(8) 0.0655(8) 0.0723(8) -0.0359(7) 0.0089(6) -0.0179(6) N1 0.054(2) 0.074(3) 0.043(2) -0.0233(19) -0.0009(17) -0.008(2) N2 0.047(2) 0.065(2) 0.046(2) -0.0199(18) -0.0032(17) -0.0065(18) N3 0.049(2) 0.062(2) 0.042(2) -0.0182(18) -0.0036(16) 0.0054(19) C1 0.059(3) 0.112(5) 0.044(3) -0.031(3) 0.004(2) -0.027(3) C2 0.042(2) 0.082(4) 0.044(2) -0.021(2) -0.0018(19) -0.015(2) C3 0.048(3) 0.061(3) 0.043(2) -0.014(2) -0.0041(19) -0.005(2) C4 0.061(3) 0.065(3) 0.042(2) -0.019(2) 0.001(2) -0.009(2) C5 0.062(3) 0.067(3) 0.045(2) -0.020(2) -0.005(2) -0.009(2) Cl6 0.0489(7) 0.0608(7) 0.0823(9) -0.0097(6) -0.0089(6) 0.0026(6) C6 0.049(3) 0.067(3) 0.043(2) -0.019(2) -0.001(2) -0.002(2) C7 0.055(3) 0.077(3) 0.043(2) -0.021(2) -0.003(2) -0.011(2) C8 0.048(3) 0.071(3) 0.050(3) -0.026(2) -0.005(2) -0.007(2) C9 0.045(2) 0.071(3) 0.046(2) -0.022(2) 0.0014(19) -0.007(2) C10 0.052(3) 0.060(3) 0.041(2) -0.019(2) -0.003(2) -0.003(2) C11 0.063(3) 0.067(3) 0.043(2) -0.018(2) -0.003(2) -0.017(2) C12 0.055(3) 0.067(3) 0.051(3) -0.020(2) -0.003(2) -0.016(2) C13 0.051(3) 0.065(3) 0.042(2) -0.019(2) -0.0055(19) -0.002(2) C14 0.064(3) 0.078(4) 0.050(3) -0.027(2) 0.000(2) -0.026(3) C15 0.055(3) 0.064(3) 0.045(2) -0.021(2) -0.006(2) -0.010(2) C16 0.054(3) 0.072(3) 0.051(3) -0.017(2) -0.008(2) -0.008(2) C17 0.072(4) 0.100(5) 0.072(4) -0.043(3) 0.011(3) -0.033(3) C18 0.090(5) 0.113(5) 0.075(4) -0.048(4) -0.004(3) -0.038(4) C19 0.062(3) 0.077(4) 0.078(4) -0.015(3) -0.014(3) -0.020(3) C20 0.057(3) 0.065(3) 0.070(3) -0.017(3) -0.005(3) -0.005(3) C21 0.050(3) 0.073(3) 0.057(3) -0.023(2) -0.005(2) -0.009(2) C22 0.086(5) 0.079(4) 0.101(5) -0.025(4) -0.021(4) -0.019(4) C23 0.086(5) 0.123(7) 0.139(8) -0.038(6) -0.023(5) -0.043(5) N4 0.046(2) 0.049(2) 0.053(2) -0.0216(17) -0.0014(17) -0.0006(17) N5 0.046(2) 0.045(2) 0.065(2) -0.0191(18) -0.0050(18) 0.0010(17) N6 0.047(2) 0.046(2) 0.071(3) -0.0213(19) -0.0011(19) -0.0032(17) C24 0.053(3) 0.040(2) 0.069(3) -0.019(2) 0.009(2) -0.003(2) C25 0.045(2) 0.055(3) 0.065(3) -0.018(2) 0.004(2) -0.004(2) C26 0.046(2) 0.044(2) 0.061(3) -0.021(2) -0.003(2) -0.0045(19) C27 0.053(3) 0.049(3) 0.065(3) -0.019(2) 0.004(2) 0.001(2) C28 0.058(3) 0.044(2) 0.057(3) -0.015(2) 0.008(2) -0.005(2) C29 0.047(2) 0.043(2) 0.059(3) -0.019(2) -0.006(2) -0.001(2) C30 0.044(2) 0.047(2) 0.064(3) -0.014(2) -0.007(2) -0.007(2) C31 0.051(3) 0.046(2) 0.062(3) -0.018(2) -0.006(2) -0.004(2) C32 0.055(3) 0.042(2) 0.064(3) -0.017(2) -0.004(2) -0.002(2) C33 0.048(2) 0.038(2) 0.069(3) -0.019(2) -0.003(2) -0.0044(19) C34 0.055(3) 0.045(3) 0.065(3) -0.018(2) -0.001(2) -0.003(2) C35 0.054(3) 0.043(2) 0.057(3) -0.016(2) 0.000(2) -0.003(2) C36 0.048(2) 0.045(2) 0.063(3) -0.022(2) -0.011(2) 0.003(2) C37 0.029(2) 0.032(2) 0.102(4) 0.001(2) -0.003(2) -0.0057(17) C38 0.049(3) 0.045(3) 0.106(5) -0.024(3) 0.007(3) -0.001(2) C39 0.053(3) 0.049(3) 0.070(3) -0.020(2) 0.001(2) -0.001(2) C40 0.041(2) 0.051(3) 0.069(3) -0.018(2) -0.008(2) 0.000(2) C41 0.044(3) 0.075(4) 0.071(3) -0.025(3) -0.001(2) -0.007(2) C42 0.048(3) 0.072(3) 0.062(3) -0.019(3) 0.007(2) 0.000(2) C43 0.070(4) 0.056(3) 0.088(4) -0.026(3) 0.015(3) 0.008(3) C44 0.063(3) 0.057(3) 0.097(4) -0.036(3) 0.015(3) -0.008(3) C45 0.054(3) 0.084(4) 0.083(4) -0.027(3) 0.008(3) -0.003(3) N7 0.043(2) 0.049(2) 0.053(2) -0.0178(17) -0.0030(16) -0.0028(16) N8 0.046(2) 0.056(2) 0.054(2) -0.0220(18) -0.0019(17) -0.0049(18) N9 0.053(2) 0.064(2) 0.046(2) -0.0217(18) -0.0021(17) -0.0086(19) C46 0.072(5) 0.133(7) 0.098(5) -0.040(5) 0.014(4) 0.000(4) C47 0.079(4) 0.069(3) 0.071(3) -0.036(3) -0.033(3) 0.021(3) C48 0.073(4) 0.080(4) 0.064(3) -0.036(3) -0.022(3) 0.020(3) C49 0.047(2) 0.048(2) 0.059(3) -0.020(2) -0.005(2) -0.003(2) C50 0.086(4) 0.067(3) 0.062(3) -0.034(3) -0.023(3) 0.030(3) C51 0.073(3) 0.065(3) 0.059(3) -0.031(3) -0.014(3) 0.013(3) C52 0.056(3) 0.046(2) 0.053(3) -0.021(2) -0.002(2) -0.004(2) C53 0.055(3) 0.054(3) 0.050(2) -0.023(2) -0.002(2) -0.001(2) C54 0.043(2) 0.051(3) 0.054(3) -0.022(2) -0.0026(19) -0.007(2) C55 0.049(3) 0.053(3) 0.056(3) -0.024(2) -0.003(2) -0.002(2) C56 0.043(2) 0.054(3) 0.052(3) -0.021(2) -0.0004(19) -0.005(2) C57 0.087(4) 0.056(3) 0.058(3) -0.025(2) -0.022(3) 0.009(3) C58 0.075(4) 0.064(3) 0.068(3) -0.031(3) -0.017(3) 0.015(3) C59 0.051(3) 0.063(3) 0.052(3) -0.024(2) -0.006(2) -0.001(2) C60 0.056(3) 0.076(4) 0.060(3) -0.034(3) -0.016(2) 0.016(3) C61 0.057(3) 0.078(4) 0.055(3) -0.037(3) -0.012(2) 0.010(3) C62 0.049(3) 0.053(3) 0.053(3) -0.018(2) -0.010(2) -0.003(2) C63 0.078(4) 0.085(4) 0.067(3) -0.035(3) -0.020(3) 0.018(3) C64 0.108(5) 0.084(4) 0.068(4) -0.025(3) -0.035(4) 0.015(4) C65 0.066(4) 0.068(4) 0.079(4) -0.013(3) -0.027(3) 0.003(3) C67 0.074(4) 0.069(3) 0.064(3) -0.028(3) -0.015(3) 0.012(3) C66 0.075(4) 0.056(3) 0.087(4) -0.023(3) -0.014(3) 0.016(3) C68 0.092(5) 0.090(5) 0.106(6) -0.022(4) -0.048(5) 0.006(4) C69 0.151(10) 0.118(8) 0.167(10) -0.019(7) -0.098(9) 0.013(7) _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 N9 2.038(4) 2_576 ? Zn1 N1 2.053(4) . ? Zn1 Cl1 2.2172(17) . ? Zn1 Cl2 2.2228(17) . ? Zn2 N4 2.040(4) . ? Zn2 N3 2.047(4) . ? Zn2 Cl3 2.2114(15) . ? Zn2 Cl4 2.2125(15) . ? Zn3 N7 2.024(4) . ? Zn3 N6 2.060(4) . ? Zn3 Cl6 2.2156(16) . ? Zn3 Cl5 2.2196(16) . ? N1 C1 1.340(7) . ? N1 C5 1.360(6) . ? N2 C10 1.337(6) . ? N2 C6 1.349(6) . ? N3 C15 1.335(7) . ? N3 C11 1.345(6) . ? C1 C2 1.365(7) . ? C1 H1A 0.9500 . ? C2 C3 1.433(7) . ? C2 H2A 0.9500 . ? C3 C4 1.367(7) . ? C3 C6 1.505(7) . ? C4 C5 1.364(7) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.380(7) . ? C7 C8 1.391(7) . ? C7 H7A 0.9500 . ? C8 C9 1.410(7) . ? C8 C16 1.473(7) . ? C9 C10 1.389(7) . ? C9 H9A 0.9500 . ? C10 C13 1.489(6) . ? C11 C12 1.381(7) . ? C11 H11A 0.9500 . ? C12 C13 1.370(7) . ? C12 H12A 0.9500 . ? C13 C14 1.398(7) . ? C14 C15 1.378(7) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.388(8) . ? C16 C17 1.398(8) . ? C17 C18 1.399(9) . ? C17 H17A 0.9500 . ? C18 C19 1.383(10) . ? C18 H18A 0.9500 . ? C19 C20 1.381(9) . ? C19 C22 1.437(9) . ? C20 C21 1.383(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.162(10) . ? C23 H23 0.9500 . ? N4 C28 1.335(6) . ? N4 C24 1.349(6) . ? N5 C29 1.337(6) . ? N5 C33 1.342(6) . ? N6 C34 1.341(6) . ? N6 C38 1.349(7) . ? C24 C25 1.355(7) . ? C24 H24A 0.9500 . ? C25 C26 1.399(7) . ? C25 H25A 0.9500 . ? C26 C27 1.379(7) . ? C26 C29 1.494(6) . ? C27 C28 1.376(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.381(7) . ? C30 C31 1.391(7) . ? C30 H30A 0.9500 . ? C31 C32 1.380(7) . ? C31 C39 1.495(7) . ? C32 C33 1.384(7) . ? C32 H32A 0.9500 . ? C33 C36 1.484(7) . ? C34 C35 1.380(7) . ? C34 H34A 0.9500 . ? C35 C36 1.369(7) . ? C35 H35A 0.9500 . ? C36 C37 1.488(7) . ? C37 C38 1.349(7) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.380(8) . ? C39 C44 1.391(8) . ? C40 C41 1.391(7) . ? C40 H40A 0.9500 . ? C41 C42 1.384(9) . ? C41 H41A 0.9500 . ? C42 C43 1.372(9) . ? C42 C45 1.457(8) . ? C43 C44 1.381(8) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.165(10) . ? N7 C51 1.328(7) . ? N7 C47 1.341(7) . ? N8 C56 1.346(6) . ? N8 C52 1.351(6) . ? N9 C61 1.320(7) . ? N9 C57 1.354(7) . ? N9 Zn1 2.038(4) 2_576 ? C46 H46 0.9500 . ? C47 C48 1.370(8) . ? C47 H47A 0.9500 . ? C48 C49 1.374(7) . ? C48 H48A 0.9500 . ? C49 C50 1.362(7) . ? C49 C52 1.502(7) . ? C50 C51 1.378(7) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.374(7) . ? C53 C54 1.389(7) . ? C53 H53A 0.9500 . ? C54 C55 1.408(7) . ? C54 C62 1.482(7) . ? C55 C56 1.381(7) . ? C55 H55A 0.9500 . ? C56 C59 1.473(7) . ? C57 C58 1.368(8) . ? C57 H57A 0.9500 . ? C58 C59 1.381(7) . ? C58 H58A 0.9500 . ? C59 C60 1.398(7) . ? C60 C61 1.379(7) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 C63 1.374(8) . ? C62 C67 1.385(8) . ? C63 C64 1.382(9) . ? C63 H63A 0.9500 . ? C64 C65 1.362(10) . ? C64 H64A 0.9500 . ? C65 C66 1.369(9) . ? C65 C68 1.450(9) . ? C67 C66 1.380(8) . ? C67 H67A 0.9500 . ? C66 H66A 0.9500 . ? C68 C69 1.172(11) . ? C69 H69 0.9500 . ? 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 N9 Zn1 N1 103.70(17) 2_576 . ? N9 Zn1 Cl1 112.03(13) 2_576 . ? N1 Zn1 Cl1 105.16(14) . . ? N9 Zn1 Cl2 108.15(13) 2_576 . ? N1 Zn1 Cl2 108.31(13) . . ? Cl1 Zn1 Cl2 118.39(7) . . ? N4 Zn2 N3 99.78(16) . . ? N4 Zn2 Cl3 109.79(12) . . ? N3 Zn2 Cl3 105.27(13) . . ? N4 Zn2 Cl4 105.84(12) . . ? N3 Zn2 Cl4 112.78(13) . . ? Cl3 Zn2 Cl4 121.30(5) . . ? N7 Zn3 N6 101.06(16) . . ? N7 Zn3 Cl6 110.07(12) . . ? N6 Zn3 Cl6 107.70(13) . . ? N7 Zn3 Cl5 111.27(12) . . ? N6 Zn3 Cl5 105.03(13) . . ? Cl6 Zn3 Cl5 119.82(7) . . ? C1 N1 C5 117.3(5) . . ? C1 N1 Zn1 123.3(3) . . ? C5 N1 Zn1 119.5(4) . . ? C10 N2 C6 117.5(4) . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Zn2 120.8(3) . . ? C11 N3 Zn2 120.4(4) . . ? N1 C1 C2 124.9(5) . . ? N1 C1 H1A 117.5 . . ? C2 C1 H1A 117.5 . . ? C1 C2 C3 116.8(5) . . ? C1 C2 H2A 121.6 . . ? C3 C2 H2A 121.6 . . ? C4 C3 C2 118.2(5) . . ? C4 C3 C6 121.3(4) . . ? C2 C3 C6 120.5(5) . . ? C5 C4 C3 121.0(5) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? N1 C5 C4 121.8(5) . . ? N1 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? N2 C6 C7 122.8(5) . . ? N2 C6 C3 114.2(4) . . ? C7 C6 C3 122.9(4) . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C7 C8 C9 116.5(5) . . ? C7 C8 C16 122.9(5) . . ? C9 C8 C16 120.7(5) . . ? C10 C9 C8 119.4(5) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? N2 C10 C9 123.2(4) . . ? N2 C10 C13 116.3(4) . . ? C9 C10 C13 120.5(4) . . ? N3 C11 C12 122.4(5) . . ? N3 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 117.4(4) . . ? C12 C13 C10 120.0(5) . . ? C14 C13 C10 122.6(5) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C15 C14 122.0(5) . . ? N3 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C21 C16 C17 118.1(5) . . ? C21 C16 C8 121.5(5) . . ? C17 C16 C8 120.4(5) . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.3(6) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C20 C19 C18 118.7(6) . . ? C20 C19 C22 122.0(7) . . ? C18 C19 C22 119.3(7) . . ? C19 C20 C21 121.4(6) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C20 C21 C16 120.7(5) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C23 C22 C19 177.9(10) . . ? C22 C23 H23 180.0 . . ? C28 N4 C24 117.3(4) . . ? C28 N4 Zn2 121.3(3) . . ? C24 N4 Zn2 121.1(3) . . ? C29 N5 C33 118.1(4) . . ? C34 N6 C38 116.7(5) . . ? C34 N6 Zn3 120.5(4) . . ? C38 N6 Zn3 122.8(3) . . ? N4 C24 C25 123.4(5) . . ? N4 C24 H24A 118.3 . . ? C25 C24 H24A 118.3 . . ? C24 C25 C26 119.2(5) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C27 C26 C25 117.6(4) . . ? C27 C26 C29 123.1(4) . . ? C25 C26 C29 119.4(4) . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? N4 C28 C27 122.8(5) . . ? N4 C28 H28A 118.6 . . ? C27 C28 H28A 118.6 . . ? N5 C29 C30 122.9(4) . . ? N5 C29 C26 116.2(4) . . ? C30 C29 C26 120.9(4) . . ? C29 C30 C31 119.2(5) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C32 C31 C30 117.5(5) . . ? C32 C31 C39 122.5(4) . . ? C30 C31 C39 120.0(5) . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? N5 C33 C32 121.8(4) . . ? N5 C33 C36 115.1(4) . . ? C32 C33 C36 123.2(4) . . ? N6 C34 C35 122.5(5) . . ? N6 C34 H34A 118.7 . . ? C35 C34 H34A 118.7 . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C33 121.8(4) . . ? C35 C36 C37 117.9(5) . . ? C33 C36 C37 120.0(4) . . ? C38 C37 C36 114.4(5) . . ? C38 C37 H37A 122.8 . . ? C36 C37 H37A 122.8 . . ? N6 C38 C37 127.3(5) . . ? N6 C38 H38A 116.3 . . ? C37 C38 H38A 116.3 . . ? C40 C39 C44 118.6(5) . . ? C40 C39 C31 120.7(5) . . ? C44 C39 C31 120.7(5) . . ? C39 C40 C41 120.8(5) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C43 C42 C41 118.9(5) . . ? C43 C42 C45 120.3(6) . . ? C41 C42 C45 120.8(6) . . ? C42 C43 C44 121.3(5) . . ? C42 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? C43 C44 C39 120.2(6) . . ? C43 C44 H44A 119.9 . . ? C39 C44 H44A 119.9 . . ? C46 C45 C42 178.7(8) . . ? C51 N7 C47 116.6(4) . . ? C51 N7 Zn3 121.0(3) . . ? C47 N7 Zn3 122.4(3) . . ? C56 N8 C52 117.4(4) . . ? C61 N9 C57 117.2(4) . . ? C61 N9 Zn1 121.4(4) . 2_576 ? C57 N9 Zn1 120.6(3) . 2_576 ? C45 C46 H46 180.0 . . ? N7 C47 C48 122.7(5) . . ? N7 C47 H47A 118.7 . . ? C48 C47 H47A 118.7 . . ? C47 C48 C49 120.2(5) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C50 C49 C48 117.0(5) . . ? C50 C49 C52 122.2(5) . . ? C48 C49 C52 120.7(5) . . ? C49 C50 C51 120.1(5) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? N7 C51 C50 123.0(5) . . ? N7 C51 H51A 118.5 . . ? C50 C51 H51A 118.5 . . ? N8 C52 C53 123.1(4) . . ? N8 C52 C49 114.8(4) . . ? C53 C52 C49 122.2(4) . . ? C52 C53 C54 120.6(5) . . ? C52 C53 H53A 119.7 . . ? C54 C53 H53A 119.7 . . ? C53 C54 C55 116.0(4) . . ? C53 C54 C62 121.9(4) . . ? C55 C54 C62 122.1(4) . . ? C56 C55 C54 120.5(4) . . ? C56 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? N8 C56 C55 122.4(4) . . ? N8 C56 C59 114.9(4) . . ? C55 C56 C59 122.7(4) . . ? N9 C57 C58 122.7(5) . . ? N9 C57 H57A 118.7 . . ? C58 C57 H57A 118.7 . . ? C57 C58 C59 120.4(5) . . ? C57 C58 H58A 119.8 . . ? C59 C58 H58A 119.8 . . ? C58 C59 C60 116.3(5) . . ? C58 C59 C56 121.0(5) . . ? C60 C59 C56 122.6(4) . . ? C61 C60 C59 119.9(5) . . ? C61 C60 H60A 120.0 . . ? C59 C60 H60A 120.0 . . ? N9 C61 C60 123.2(5) . . ? N9 C61 H61A 118.4 . . ? C60 C61 H61A 118.4 . . ? C63 C62 C67 116.9(5) . . ? C63 C62 C54 121.1(5) . . ? C67 C62 C54 121.9(5) . . ? C62 C63 C64 121.7(6) . . ? C62 C63 H63A 119.2 . . ? C64 C63 H63A 119.2 . . ? C65 C64 C63 120.8(6) . . ? C65 C64 H64A 119.6 . . ? C63 C64 H64A 119.6 . . ? C64 C65 C66 118.5(5) . . ? C64 C65 C68 121.4(7) . . ? C66 C65 C68 119.9(7) . . ? C66 C67 C62 121.2(6) . . ? C66 C67 H67A 119.4 . . ? C62 C67 H67A 119.4 . . ? C65 C66 C67 120.9(6) . . ? C65 C66 H66A 119.6 . . ? C67 C66 H66A 119.6 . . ? C69 C68 C65 179.0(12) . . ? C68 C69 H69 180.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.456 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.101 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.047 0.000 0.500 1835 405 ' ' 2 0.476 0.467 0.263 6 0 ' ' 3 0.524 0.533 0.737 5 1 ' ' _platon_squeeze_details ; ; # end Validation Reply Form # Attachment 'SQUEEZE143.CIF' data_squeeze _database_code_depnum_ccdc_archive 'CCDC 832655' #TrackingRef 'SQUEEZE143.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H90 Cl12 N18 Zn6' _chemical_formula_sum 'C138 H90 Cl12 N18 Zn6' _chemical_formula_weight 2818.03 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' 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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.793(2) _cell_length_b 23.662(6) _cell_length_c 24.672(6) _cell_angle_alpha 68.897(19) _cell_angle_beta 87.31(2) _cell_angle_gamma 80.27(2) _cell_volume 4719(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4401 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 36.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7300 _exptl_absorpt_correction_T_max 0.9101 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; Crystals are unstable out of solvent and diffract poorly. Of many datasets on different crystals, this was the best. This structure contains large voids in which very little solvent could be identified. It is probable the solvent in these voids is so disordered that the electron density is too smeared to create peaks in the difference map, hence why SQUEEZE has been used. The non-merohedral twinning was dealt with using the TwinRotMat program in Platon. A HKLF 5 was generated from the original file (118838 measured reflections, R(int)=0.1470) using the twin law (-1,0,0/-0.5,0,1/-0.5,1,0) to give a modified file (16722 reflections, R(int)=0.0000) that was used in SHELXL97 with a basf of 0.1649. ; _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 16722 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.05 _reflns_number_total 16722 _reflns_number_gt 14711 _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^)+(0.1471P)^2^+4.8540P] 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 16722 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.2271 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _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 0.01360(7) 0.50307(3) 0.68114(2) 0.05455(18) Uani 1 1 d . . . Cl1 Cl 0.02823(18) 0.40388(7) 0.69715(6) 0.0681(4) Uani 1 1 d . . . Cl2 Cl -0.20947(16) 0.56465(8) 0.64934(6) 0.0712(4) Uani 1 1 d . . . Zn2 Zn 0.32103(6) 0.62991(2) 0.15015(2) 0.04608(16) Uani 1 1 d . . . Cl3 Cl 0.17733(16) 0.55675(6) 0.17149(5) 0.0571(3) Uani 1 1 d . . . Cl4 Cl 0.48659(16) 0.64414(6) 0.07796(5) 0.0596(3) Uani 1 1 d . . . Zn3 Zn 0.37368(6) 1.19749(2) -0.01431(3) 0.05230(17) Uani 1 1 d . . . Cl5 Cl 0.40431(17) 1.20958(7) -0.10743(6) 0.0658(3) Uani 1 1 d . . . N1 N 0.1785(5) 0.5320(2) 0.62029(17) 0.0564(10) Uani 1 1 d . . . N2 N 0.4723(5) 0.5936(2) 0.43584(17) 0.0528(9) Uani 1 1 d . . . N3 N 0.4213(5) 0.6190(2) 0.22727(17) 0.0527(9) Uani 1 1 d . . . C1 C 0.2953(7) 0.5575(3) 0.6292(2) 0.0694(16) Uani 1 1 d . . . H1A H 0.3012 0.5621 0.6658 0.083 Uiso 1 1 calc R . . C2 C 0.4066(6) 0.5775(3) 0.5898(2) 0.0557(12) Uani 1 1 d . . . H2A H 0.4857 0.5962 0.5980 0.067 Uiso 1 1 calc R . . C3 C 0.3983(6) 0.5690(2) 0.5355(2) 0.0522(11) Uani 1 1 d . . . C4 C 0.2791(6) 0.5429(2) 0.5264(2) 0.0562(12) Uani 1 1 d . . . H4A H 0.2711 0.5371 0.4906 0.067 Uiso 1 1 calc R . . C5 C 0.1715(6) 0.5252(3) 0.5681(2) 0.0581(12) Uani 1 1 d . . . H5A H 0.0893 0.5076 0.5604 0.070 Uiso 1 1 calc R . . Cl6 Cl 0.57778(16) 1.16788(7) 0.04456(7) 0.0695(4) Uani 1 1 d . . . C6 C 0.5130(6) 0.5916(2) 0.4886(2) 0.0543(11) Uani 1 1 d . . . C7 C 0.6457(6) 0.6106(3) 0.4983(2) 0.0580(12) Uani 1 1 d . . . H7A H 0.6714 0.6069 0.5366 0.070 Uiso 1 1 calc R . . C8 C 0.7420(6) 0.6352(3) 0.4525(2) 0.0554(11) Uani 1 1 d . . . C9 C 0.6972(6) 0.6384(3) 0.3972(2) 0.0541(11) Uani 1 1 d . . . H9A H 0.7569 0.6559 0.3641 0.065 Uiso 1 1 calc R . . C10 C 0.5651(6) 0.6160(2) 0.3915(2) 0.0517(11) Uani 1 1 d . . . C11 C 0.3740(6) 0.5805(3) 0.2776(2) 0.0571(12) Uani 1 1 d . . . H11A H 0.3080 0.5531 0.2764 0.069 Uiso 1 1 calc R . . C12 C 0.4179(6) 0.5795(3) 0.3310(2) 0.0571(12) Uani 1 1 d . . . H12A H 0.3782 0.5532 0.3657 0.068 Uiso 1 1 calc R . . C13 C 0.5189(6) 0.6166(2) 0.3340(2) 0.0533(11) Uani 1 1 d . . . C14 C 0.5705(7) 0.6554(3) 0.2815(2) 0.0611(13) Uani 1 1 d . . . H14A H 0.6411 0.6816 0.2817 0.073 Uiso 1 1 calc R . . C15 C 0.5190(6) 0.6556(2) 0.2296(2) 0.0542(11) Uani 1 1 d . . . H15A H 0.5540 0.6826 0.1943 0.065 Uiso 1 1 calc R . . C16 C 0.8821(6) 0.6582(3) 0.4600(2) 0.0604(12) Uani 1 1 d . . . C17 C 0.8937(8) 0.6799(3) 0.5051(3) 0.0757(16) Uani 1 1 d . . . H17A H 0.8125 0.6780 0.5322 0.091 Uiso 1 1 calc R . . C18 C 1.0237(9) 0.7042(4) 0.5109(3) 0.086(2) Uani 1 1 d . . . H18A H 1.0294 0.7193 0.5415 0.103 Uiso 1 1 calc R . . C19 C 1.1439(7) 0.7065(3) 0.4724(3) 0.0742(16) Uani 1 1 d . . . C20 C 1.1327(7) 0.6844(3) 0.4282(3) 0.0667(14) Uani 1 1 d . . . H20A H 1.2149 0.6857 0.4017 0.080 Uiso 1 1 calc R . . C21 C 1.0043(6) 0.6606(3) 0.4219(2) 0.0602(12) Uani 1 1 d . . . H21A H 0.9997 0.6457 0.3911 0.072 Uiso 1 1 calc R . . C22 C 1.2766(9) 0.7314(3) 0.4795(4) 0.089(2) Uani 1 1 d . . . C23 C 1.3866(10) 0.7503(5) 0.4847(4) 0.114(3) Uani 1 1 d . . . H23 H 1.4766 0.7657 0.4890 0.137 Uiso 1 1 calc R . . N4 N 0.1832(4) 0.71282(18) 0.13451(17) 0.0493(9) Uani 1 1 d . . . N5 N 0.0131(5) 0.93701(18) 0.09018(19) 0.0526(9) Uani 1 1 d . . . N6 N 0.2311(5) 1.13243(19) 0.0170(2) 0.0553(10) Uani 1 1 d . . . C24 C 0.2216(6) 0.7645(2) 0.0947(2) 0.0552(12) Uani 1 1 d . . . H24A H 0.3074 0.7609 0.0707 0.066 Uiso 1 1 calc R . . C25 C 0.1441(6) 0.8215(2) 0.0873(2) 0.0568(12) Uani 1 1 d . . . H25A H 0.1752 0.8566 0.0585 0.068 Uiso 1 1 calc R . . C26 C 0.0180(5) 0.8280(2) 0.1225(2) 0.0498(10) Uani 1 1 d . . . C27 C -0.0236(6) 0.7752(2) 0.1625(2) 0.0570(12) Uani 1 1 d . . . H27A H -0.1105 0.7775 0.1864 0.068 Uiso 1 1 calc R . . C28 C 0.0615(6) 0.7190(2) 0.1675(2) 0.0550(11) Uani 1 1 d . . . H28A H 0.0324 0.6831 0.1958 0.066 Uiso 1 1 calc R . . C29 C -0.0655(6) 0.8908(2) 0.1153(2) 0.0503(10) Uani 1 1 d . . . C30 C -0.2145(5) 0.8993(2) 0.1347(2) 0.0530(11) Uani 1 1 d . . . H30A H -0.2651 0.8651 0.1537 0.064 Uiso 1 1 calc R . . C31 C -0.2897(6) 0.9586(2) 0.1261(2) 0.0538(11) Uani 1 1 d . . . C32 C -0.2087(6) 1.0062(2) 0.0991(2) 0.0547(11) Uani 1 1 d . . . H32A H -0.2576 1.0474 0.0910 0.066 Uiso 1 1 calc R . . C33 C -0.0566(6) 0.9941(2) 0.0838(2) 0.0519(11) Uani 1 1 d . . . C34 C 0.2773(6) 1.0751(2) 0.0180(2) 0.0563(12) Uani 1 1 d . . . H34A H 0.3783 1.0647 0.0053 0.068 Uiso 1 1 calc R . . C35 C 0.1839(6) 1.0306(2) 0.0368(2) 0.0523(11) Uani 1 1 d . . . H35A H 0.2192 0.9912 0.0348 0.063 Uiso 1 1 calc R . . C36 C 0.0407(6) 1.0426(2) 0.0585(2) 0.0524(11) Uani 1 1 d . . . C37 C -0.0089(5) 1.1045(2) 0.0620(3) 0.0613(15) Uani 1 1 d . . . H37A H -0.1018 1.1149 0.0800 0.074 Uiso 1 1 calc R . . C38 C 0.0892(6) 1.1445(2) 0.0375(3) 0.0687(15) Uani 1 1 d . . . H38A H 0.0543 1.1858 0.0343 0.082 Uiso 1 1 calc R . . C39 C -0.4512(6) 0.9688(2) 0.1466(2) 0.0583(12) Uani 1 1 d . . . C40 C -0.5480(6) 0.9267(2) 0.1530(2) 0.0558(12) Uani 1 1 d . . . H40A H -0.5128 0.8916 0.1430 0.067 Uiso 1 1 calc R . . C41 C -0.6965(6) 0.9351(3) 0.1740(3) 0.0639(13) Uani 1 1 d . . . H41A H -0.7618 0.9057 0.1782 0.077 Uiso 1 1 calc R . . C42 C -0.7493(6) 0.9861(3) 0.1886(2) 0.0637(13) Uani 1 1 d . . . C43 C -0.6532(7) 1.0281(3) 0.1820(3) 0.0739(16) Uani 1 1 d . . . H43A H -0.6890 1.0634 0.1917 0.089 Uiso 1 1 calc R . . C44 C -0.5054(7) 1.0200(3) 0.1614(3) 0.0707(15) Uani 1 1 d . . . H44A H -0.4405 1.0496 0.1573 0.085 Uiso 1 1 calc R . . C45 C -0.9043(7) 0.9952(3) 0.2110(3) 0.0756(16) Uani 1 1 d . . . N7 N 0.2393(4) 1.27160(18) -0.00478(17) 0.0488(9) Uani 1 1 d . . . N8 N -0.0607(5) 1.42495(19) 0.07215(18) 0.0517(9) Uani 1 1 d . . . N9 N -0.0847(5) 1.4821(2) 0.24841(17) 0.0536(9) Uani 1 1 d . . . C46 C -1.0293(9) 1.0025(4) 0.2280(4) 0.104(3) Uani 1 1 d . . . H46 H -1.1313 1.0084 0.2418 0.125 Uiso 1 1 calc R . . C47 C 0.2461(8) 1.2859(3) 0.0428(3) 0.0724(17) Uani 1 1 d . . . H47A H 0.3243 1.2630 0.0712 0.087 Uiso 1 1 calc R . . C48 C 0.1448(7) 1.3321(3) 0.0523(3) 0.0725(16) Uani 1 1 d . . . H48A H 0.1483 1.3385 0.0880 0.087 Uiso 1 1 calc R . . C49 C 0.0382(6) 1.3692(2) 0.0101(2) 0.0517(11) Uani 1 1 d . . . C50 C 0.0399(8) 1.3579(3) -0.0403(3) 0.0728(17) Uani 1 1 d . . . H50A H -0.0277 1.3839 -0.0715 0.087 Uiso 1 1 calc R . . C51 C 0.1395(7) 1.3089(3) -0.0461(2) 0.0655(14) Uani 1 1 d . . . H51A H 0.1367 1.3014 -0.0814 0.079 Uiso 1 1 calc R . . C52 C -0.0707(6) 1.4212(2) 0.0191(2) 0.0513(11) Uani 1 1 d . . . C53 C -0.1729(6) 1.4611(2) -0.0233(2) 0.0525(11) Uani 1 1 d . . . H53A H -0.1758 1.4563 -0.0599 0.063 Uiso 1 1 calc R . . C54 C -0.2722(5) 1.5086(2) -0.0134(2) 0.0487(10) Uani 1 1 d . . . C55 C -0.2618(6) 1.5120(2) 0.0421(2) 0.0522(11) Uani 1 1 d . . . H55A H -0.3286 1.5429 0.0517 0.063 Uiso 1 1 calc R . . C56 C -0.1552(5) 1.4708(2) 0.0827(2) 0.0496(10) Uani 1 1 d . . . C57 C -0.0107(8) 1.4349(3) 0.2335(2) 0.0676(15) Uani 1 1 d . . . H57A H 0.0574 1.4032 0.2611 0.081 Uiso 1 1 calc R . . C58 C -0.0299(7) 1.4309(3) 0.1804(3) 0.0695(15) Uani 1 1 d . . . H58A H 0.0309 1.3988 0.1706 0.083 Uiso 1 1 calc R . . C59 C -0.1369(6) 1.4733(2) 0.1408(2) 0.0551(11) Uani 1 1 d . . . C60 C -0.2191(6) 1.5199(3) 0.1579(2) 0.0644(14) Uani 1 1 d . . . H60A H -0.2965 1.5496 0.1329 0.077 Uiso 1 1 calc R . . C61 C -0.1875(6) 1.5228(3) 0.2110(2) 0.0618(13) Uani 1 1 d . . . H61A H -0.2425 1.5557 0.2211 0.074 Uiso 1 1 calc R . . C62 C -0.3830(6) 1.5527(2) -0.0584(2) 0.0522(11) Uani 1 1 d . . . C63 C -0.3929(8) 1.5479(3) -0.1120(3) 0.0779(18) Uani 1 1 d . . . H63A H -0.3265 1.5160 -0.1202 0.093 Uiso 1 1 calc R . . C64 C -0.4969(10) 1.5882(3) -0.1541(3) 0.090(2) Uani 1 1 d . . . H64A H -0.5011 1.5836 -0.1906 0.108 Uiso 1 1 calc R . . C65 C -0.5936(7) 1.6346(3) -0.1438(3) 0.0754(17) Uani 1 1 d . . . C67 C -0.4866(7) 1.5984(3) -0.0477(3) 0.0706(15) Uani 1 1 d . . . H67A H -0.4870 1.6018 -0.0105 0.085 Uiso 1 1 calc R . . C66 C -0.5893(8) 1.6390(3) -0.0901(3) 0.0762(17) Uani 1 1 d . . . H66A H -0.6580 1.6704 -0.0819 0.091 Uiso 1 1 calc R . . C68 C -0.7062(10) 1.6763(4) -0.1870(4) 0.101(3) Uani 1 1 d . . . C69 C -0.7987(15) 1.7094(5) -0.2217(6) 0.155(5) Uani 1 1 d . . . H69 H -0.8737 1.7362 -0.2497 0.186 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 Zn1 0.0500(3) 0.0717(4) 0.0435(3) -0.0216(3) -0.0031(2) -0.0110(3) Cl1 0.0718(8) 0.0765(9) 0.0665(8) -0.0375(7) 0.0132(6) -0.0166(7) Cl2 0.0569(7) 0.0907(10) 0.0568(7) -0.0163(7) -0.0123(6) -0.0066(7) Zn2 0.0468(3) 0.0466(3) 0.0441(3) -0.0186(2) -0.0068(2) 0.0016(2) Cl3 0.0675(8) 0.0569(7) 0.0509(6) -0.0220(5) -0.0043(5) -0.0135(6) Cl4 0.0655(8) 0.0558(7) 0.0531(6) -0.0204(5) 0.0069(5) 0.0023(6) Zn3 0.0442(3) 0.0427(3) 0.0680(4) -0.0199(3) 0.0008(2) -0.0016(2) Cl5 0.0708(8) 0.0655(8) 0.0723(8) -0.0359(7) 0.0089(6) -0.0179(6) N1 0.054(2) 0.074(3) 0.043(2) -0.0233(19) -0.0009(17) -0.008(2) N2 0.047(2) 0.065(2) 0.046(2) -0.0199(18) -0.0032(17) -0.0065(18) N3 0.049(2) 0.062(2) 0.042(2) -0.0182(18) -0.0036(16) 0.0054(19) C1 0.059(3) 0.112(5) 0.044(3) -0.031(3) 0.004(2) -0.027(3) C2 0.042(2) 0.082(4) 0.044(2) -0.021(2) -0.0018(19) -0.015(2) C3 0.048(3) 0.061(3) 0.043(2) -0.014(2) -0.0041(19) -0.005(2) C4 0.061(3) 0.065(3) 0.042(2) -0.019(2) 0.001(2) -0.009(2) C5 0.062(3) 0.067(3) 0.045(2) -0.020(2) -0.005(2) -0.009(2) Cl6 0.0489(7) 0.0608(7) 0.0823(9) -0.0097(6) -0.0089(6) 0.0026(6) C6 0.049(3) 0.067(3) 0.043(2) -0.019(2) -0.001(2) -0.002(2) C7 0.055(3) 0.077(3) 0.043(2) -0.021(2) -0.003(2) -0.011(2) C8 0.048(3) 0.071(3) 0.050(3) -0.026(2) -0.005(2) -0.007(2) C9 0.045(2) 0.071(3) 0.046(2) -0.022(2) 0.0014(19) -0.007(2) C10 0.052(3) 0.060(3) 0.041(2) -0.019(2) -0.003(2) -0.003(2) C11 0.063(3) 0.067(3) 0.043(2) -0.018(2) -0.003(2) -0.017(2) C12 0.055(3) 0.067(3) 0.051(3) -0.020(2) -0.003(2) -0.016(2) C13 0.051(3) 0.065(3) 0.042(2) -0.019(2) -0.0055(19) -0.002(2) C14 0.064(3) 0.078(4) 0.050(3) -0.027(2) 0.000(2) -0.026(3) C15 0.055(3) 0.064(3) 0.045(2) -0.021(2) -0.006(2) -0.010(2) C16 0.054(3) 0.072(3) 0.051(3) -0.017(2) -0.008(2) -0.008(2) C17 0.072(4) 0.100(5) 0.072(4) -0.043(3) 0.011(3) -0.033(3) C18 0.090(5) 0.113(5) 0.075(4) -0.048(4) -0.004(3) -0.038(4) C19 0.062(3) 0.077(4) 0.078(4) -0.015(3) -0.014(3) -0.020(3) C20 0.057(3) 0.065(3) 0.070(3) -0.017(3) -0.005(3) -0.005(3) C21 0.050(3) 0.073(3) 0.057(3) -0.023(2) -0.005(2) -0.009(2) C22 0.086(5) 0.079(4) 0.101(5) -0.025(4) -0.021(4) -0.019(4) C23 0.086(5) 0.123(7) 0.139(8) -0.038(6) -0.023(5) -0.043(5) N4 0.046(2) 0.049(2) 0.053(2) -0.0216(17) -0.0014(17) -0.0006(17) N5 0.046(2) 0.045(2) 0.065(2) -0.0191(18) -0.0050(18) 0.0010(17) N6 0.047(2) 0.046(2) 0.071(3) -0.0213(19) -0.0011(19) -0.0032(17) C24 0.053(3) 0.040(2) 0.069(3) -0.019(2) 0.009(2) -0.003(2) C25 0.045(2) 0.055(3) 0.065(3) -0.018(2) 0.004(2) -0.004(2) C26 0.046(2) 0.044(2) 0.061(3) -0.021(2) -0.003(2) -0.0045(19) C27 0.053(3) 0.049(3) 0.065(3) -0.019(2) 0.004(2) 0.001(2) C28 0.058(3) 0.044(2) 0.057(3) -0.015(2) 0.008(2) -0.005(2) C29 0.047(2) 0.043(2) 0.059(3) -0.019(2) -0.006(2) -0.001(2) C30 0.044(2) 0.047(2) 0.064(3) -0.014(2) -0.007(2) -0.007(2) C31 0.051(3) 0.046(2) 0.062(3) -0.018(2) -0.006(2) -0.004(2) C32 0.055(3) 0.042(2) 0.064(3) -0.017(2) -0.004(2) -0.002(2) C33 0.048(2) 0.038(2) 0.069(3) -0.019(2) -0.003(2) -0.0044(19) C34 0.055(3) 0.045(3) 0.065(3) -0.018(2) -0.001(2) -0.003(2) C35 0.054(3) 0.043(2) 0.057(3) -0.016(2) 0.000(2) -0.003(2) C36 0.048(2) 0.045(2) 0.063(3) -0.022(2) -0.011(2) 0.003(2) C37 0.029(2) 0.032(2) 0.102(4) 0.001(2) -0.003(2) -0.0057(17) C38 0.049(3) 0.045(3) 0.106(5) -0.024(3) 0.007(3) -0.001(2) C39 0.053(3) 0.049(3) 0.070(3) -0.020(2) 0.001(2) -0.001(2) C40 0.041(2) 0.051(3) 0.069(3) -0.018(2) -0.008(2) 0.000(2) C41 0.044(3) 0.075(4) 0.071(3) -0.025(3) -0.001(2) -0.007(2) C42 0.048(3) 0.072(3) 0.062(3) -0.019(3) 0.007(2) 0.000(2) C43 0.070(4) 0.056(3) 0.088(4) -0.026(3) 0.015(3) 0.008(3) C44 0.063(3) 0.057(3) 0.097(4) -0.036(3) 0.015(3) -0.008(3) C45 0.054(3) 0.084(4) 0.083(4) -0.027(3) 0.008(3) -0.003(3) N7 0.043(2) 0.049(2) 0.053(2) -0.0178(17) -0.0030(16) -0.0028(16) N8 0.046(2) 0.056(2) 0.054(2) -0.0220(18) -0.0019(17) -0.0049(18) N9 0.053(2) 0.064(2) 0.046(2) -0.0217(18) -0.0021(17) -0.0086(19) C46 0.072(5) 0.133(7) 0.098(5) -0.040(5) 0.014(4) 0.000(4) C47 0.079(4) 0.069(3) 0.071(3) -0.036(3) -0.033(3) 0.021(3) C48 0.073(4) 0.080(4) 0.064(3) -0.036(3) -0.022(3) 0.020(3) C49 0.047(2) 0.048(2) 0.059(3) -0.020(2) -0.005(2) -0.003(2) C50 0.086(4) 0.067(3) 0.062(3) -0.034(3) -0.023(3) 0.030(3) C51 0.073(3) 0.065(3) 0.059(3) -0.031(3) -0.014(3) 0.013(3) C52 0.056(3) 0.046(2) 0.053(3) -0.021(2) -0.002(2) -0.004(2) C53 0.055(3) 0.054(3) 0.050(2) -0.023(2) -0.002(2) -0.001(2) C54 0.043(2) 0.051(3) 0.054(3) -0.022(2) -0.0026(19) -0.007(2) C55 0.049(3) 0.053(3) 0.056(3) -0.024(2) -0.003(2) -0.002(2) C56 0.043(2) 0.054(3) 0.052(3) -0.021(2) -0.0004(19) -0.005(2) C57 0.087(4) 0.056(3) 0.058(3) -0.025(2) -0.022(3) 0.009(3) C58 0.075(4) 0.064(3) 0.068(3) -0.031(3) -0.017(3) 0.015(3) C59 0.051(3) 0.063(3) 0.052(3) -0.024(2) -0.006(2) -0.001(2) C60 0.056(3) 0.076(4) 0.060(3) -0.034(3) -0.016(2) 0.016(3) C61 0.057(3) 0.078(4) 0.055(3) -0.037(3) -0.012(2) 0.010(3) C62 0.049(3) 0.053(3) 0.053(3) -0.018(2) -0.010(2) -0.003(2) C63 0.078(4) 0.085(4) 0.067(3) -0.035(3) -0.020(3) 0.018(3) C64 0.108(5) 0.084(4) 0.068(4) -0.025(3) -0.035(4) 0.015(4) C65 0.066(4) 0.068(4) 0.079(4) -0.013(3) -0.027(3) 0.003(3) C67 0.074(4) 0.069(3) 0.064(3) -0.028(3) -0.015(3) 0.012(3) C66 0.075(4) 0.056(3) 0.087(4) -0.023(3) -0.014(3) 0.016(3) C68 0.092(5) 0.090(5) 0.106(6) -0.022(4) -0.048(5) 0.006(4) C69 0.151(10) 0.118(8) 0.167(10) -0.019(7) -0.098(9) 0.013(7) _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 N9 2.038(4) 2_576 ? Zn1 N1 2.053(4) . ? Zn1 Cl1 2.2172(17) . ? Zn1 Cl2 2.2228(17) . ? Zn2 N4 2.040(4) . ? Zn2 N3 2.047(4) . ? Zn2 Cl3 2.2114(15) . ? Zn2 Cl4 2.2125(15) . ? Zn3 N7 2.024(4) . ? Zn3 N6 2.060(4) . ? Zn3 Cl6 2.2156(16) . ? Zn3 Cl5 2.2196(16) . ? N1 C1 1.340(7) . ? N1 C5 1.360(6) . ? N2 C10 1.337(6) . ? N2 C6 1.349(6) . ? N3 C15 1.335(7) . ? N3 C11 1.345(6) . ? C1 C2 1.365(7) . ? C1 H1A 0.9500 . ? C2 C3 1.433(7) . ? C2 H2A 0.9500 . ? C3 C4 1.367(7) . ? C3 C6 1.505(7) . ? C4 C5 1.364(7) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.380(7) . ? C7 C8 1.391(7) . ? C7 H7A 0.9500 . ? C8 C9 1.410(7) . ? C8 C16 1.473(7) . ? C9 C10 1.389(7) . ? C9 H9A 0.9500 . ? C10 C13 1.489(6) . ? C11 C12 1.381(7) . ? C11 H11A 0.9500 . ? C12 C13 1.370(7) . ? C12 H12A 0.9500 . ? C13 C14 1.398(7) . ? C14 C15 1.378(7) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C21 1.388(8) . ? C16 C17 1.398(8) . ? C17 C18 1.399(9) . ? C17 H17A 0.9500 . ? C18 C19 1.383(10) . ? C18 H18A 0.9500 . ? C19 C20 1.381(9) . ? C19 C22 1.437(9) . ? C20 C21 1.383(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.162(10) . ? C23 H23 0.9500 . ? N4 C28 1.335(6) . ? N4 C24 1.349(6) . ? N5 C29 1.337(6) . ? N5 C33 1.342(6) . ? N6 C34 1.341(6) . ? N6 C38 1.349(7) . ? C24 C25 1.355(7) . ? C24 H24A 0.9500 . ? C25 C26 1.399(7) . ? C25 H25A 0.9500 . ? C26 C27 1.379(7) . ? C26 C29 1.494(6) . ? C27 C28 1.376(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.381(7) . ? C30 C31 1.391(7) . ? C30 H30A 0.9500 . ? C31 C32 1.380(7) . ? C31 C39 1.495(7) . ? C32 C33 1.384(7) . ? C32 H32A 0.9500 . ? C33 C36 1.484(7) . ? C34 C35 1.380(7) . ? C34 H34A 0.9500 . ? C35 C36 1.369(7) . ? C35 H35A 0.9500 . ? C36 C37 1.488(7) . ? C37 C38 1.349(7) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.380(8) . ? C39 C44 1.391(8) . ? C40 C41 1.391(7) . ? C40 H40A 0.9500 . ? C41 C42 1.384(9) . ? C41 H41A 0.9500 . ? C42 C43 1.372(9) . ? C42 C45 1.457(8) . ? C43 C44 1.381(8) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.165(10) . ? N7 C51 1.328(7) . ? N7 C47 1.341(7) . ? N8 C56 1.346(6) . ? N8 C52 1.351(6) . ? N9 C61 1.320(7) . ? N9 C57 1.354(7) . ? N9 Zn1 2.038(4) 2_576 ? C46 H46 0.9500 . ? C47 C48 1.370(8) . ? C47 H47A 0.9500 . ? C48 C49 1.374(7) . ? C48 H48A 0.9500 . ? C49 C50 1.362(7) . ? C49 C52 1.502(7) . ? C50 C51 1.378(7) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C53 1.374(7) . ? C53 C54 1.389(7) . ? C53 H53A 0.9500 . ? C54 C55 1.408(7) . ? C54 C62 1.482(7) . ? C55 C56 1.381(7) . ? C55 H55A 0.9500 . ? C56 C59 1.473(7) . ? C57 C58 1.368(8) . ? C57 H57A 0.9500 . ? C58 C59 1.381(7) . ? C58 H58A 0.9500 . ? C59 C60 1.398(7) . ? C60 C61 1.379(7) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 C63 1.374(8) . ? C62 C67 1.385(8) . ? C63 C64 1.382(9) . ? C63 H63A 0.9500 . ? C64 C65 1.362(10) . ? C64 H64A 0.9500 . ? C65 C66 1.369(9) . ? C65 C68 1.450(9) . ? C67 C66 1.380(8) . ? C67 H67A 0.9500 . ? C66 H66A 0.9500 . ? C68 C69 1.172(11) . ? C69 H69 0.9500 . ? 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 N9 Zn1 N1 103.70(17) 2_576 . ? N9 Zn1 Cl1 112.03(13) 2_576 . ? N1 Zn1 Cl1 105.16(14) . . ? N9 Zn1 Cl2 108.15(13) 2_576 . ? N1 Zn1 Cl2 108.31(13) . . ? Cl1 Zn1 Cl2 118.39(7) . . ? N4 Zn2 N3 99.78(16) . . ? N4 Zn2 Cl3 109.79(12) . . ? N3 Zn2 Cl3 105.27(13) . . ? N4 Zn2 Cl4 105.84(12) . . ? N3 Zn2 Cl4 112.78(13) . . ? Cl3 Zn2 Cl4 121.30(5) . . ? N7 Zn3 N6 101.06(16) . . ? N7 Zn3 Cl6 110.07(12) . . ? N6 Zn3 Cl6 107.70(13) . . ? N7 Zn3 Cl5 111.27(12) . . ? N6 Zn3 Cl5 105.03(13) . . ? Cl6 Zn3 Cl5 119.82(7) . . ? C1 N1 C5 117.3(5) . . ? C1 N1 Zn1 123.3(3) . . ? C5 N1 Zn1 119.5(4) . . ? C10 N2 C6 117.5(4) . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Zn2 120.8(3) . . ? C11 N3 Zn2 120.4(4) . . ? N1 C1 C2 124.9(5) . . ? N1 C1 H1A 117.5 . . ? C2 C1 H1A 117.5 . . ? C1 C2 C3 116.8(5) . . ? C1 C2 H2A 121.6 . . ? C3 C2 H2A 121.6 . . ? C4 C3 C2 118.2(5) . . ? C4 C3 C6 121.3(4) . . ? C2 C3 C6 120.5(5) . . ? C5 C4 C3 121.0(5) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? N1 C5 C4 121.8(5) . . ? N1 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? N2 C6 C7 122.8(5) . . ? N2 C6 C3 114.2(4) . . ? C7 C6 C3 122.9(4) . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C7 C8 C9 116.5(5) . . ? C7 C8 C16 122.9(5) . . ? C9 C8 C16 120.7(5) . . ? C10 C9 C8 119.4(5) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? N2 C10 C9 123.2(4) . . ? N2 C10 C13 116.3(4) . . ? C9 C10 C13 120.5(4) . . ? N3 C11 C12 122.4(5) . . ? N3 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C13 C12 C11 119.9(5) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 117.4(4) . . ? C12 C13 C10 120.0(5) . . ? C14 C13 C10 122.6(5) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C15 C14 122.0(5) . . ? N3 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C21 C16 C17 118.1(5) . . ? C21 C16 C8 121.5(5) . . ? C17 C16 C8 120.4(5) . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.3(6) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C20 C19 C18 118.7(6) . . ? C20 C19 C22 122.0(7) . . ? C18 C19 C22 119.3(7) . . ? C19 C20 C21 121.4(6) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C20 C21 C16 120.7(5) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C23 C22 C19 177.9(10) . . ? C22 C23 H23 180.0 . . ? C28 N4 C24 117.3(4) . . ? C28 N4 Zn2 121.3(3) . . ? C24 N4 Zn2 121.1(3) . . ? C29 N5 C33 118.1(4) . . ? C34 N6 C38 116.7(5) . . ? C34 N6 Zn3 120.5(4) . . ? C38 N6 Zn3 122.8(3) . . ? N4 C24 C25 123.4(5) . . ? N4 C24 H24A 118.3 . . ? C25 C24 H24A 118.3 . . ? C24 C25 C26 119.2(5) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C27 C26 C25 117.6(4) . . ? C27 C26 C29 123.1(4) . . ? C25 C26 C29 119.4(4) . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? N4 C28 C27 122.8(5) . . ? N4 C28 H28A 118.6 . . ? C27 C28 H28A 118.6 . . ? N5 C29 C30 122.9(4) . . ? N5 C29 C26 116.2(4) . . ? C30 C29 C26 120.9(4) . . ? C29 C30 C31 119.2(5) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C32 C31 C30 117.5(5) . . ? C32 C31 C39 122.5(4) . . ? C30 C31 C39 120.0(5) . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? N5 C33 C32 121.8(4) . . ? N5 C33 C36 115.1(4) . . ? C32 C33 C36 123.2(4) . . ? N6 C34 C35 122.5(5) . . ? N6 C34 H34A 118.7 . . ? C35 C34 H34A 118.7 . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C33 121.8(4) . . ? C35 C36 C37 117.9(5) . . ? C33 C36 C37 120.0(4) . . ? C38 C37 C36 114.4(5) . . ? C38 C37 H37A 122.8 . . ? C36 C37 H37A 122.8 . . ? N6 C38 C37 127.3(5) . . ? N6 C38 H38A 116.3 . . ? C37 C38 H38A 116.3 . . ? C40 C39 C44 118.6(5) . . ? C40 C39 C31 120.7(5) . . ? C44 C39 C31 120.7(5) . . ? C39 C40 C41 120.8(5) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C43 C42 C41 118.9(5) . . ? C43 C42 C45 120.3(6) . . ? C41 C42 C45 120.8(6) . . ? C42 C43 C44 121.3(5) . . ? C42 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? C43 C44 C39 120.2(6) . . ? C43 C44 H44A 119.9 . . ? C39 C44 H44A 119.9 . . ? C46 C45 C42 178.7(8) . . ? C51 N7 C47 116.6(4) . . ? C51 N7 Zn3 121.0(3) . . ? C47 N7 Zn3 122.4(3) . . ? C56 N8 C52 117.4(4) . . ? C61 N9 C57 117.2(4) . . ? C61 N9 Zn1 121.4(4) . 2_576 ? C57 N9 Zn1 120.6(3) . 2_576 ? C45 C46 H46 180.0 . . ? N7 C47 C48 122.7(5) . . ? N7 C47 H47A 118.7 . . ? C48 C47 H47A 118.7 . . ? C47 C48 C49 120.2(5) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C50 C49 C48 117.0(5) . . ? C50 C49 C52 122.2(5) . . ? C48 C49 C52 120.7(5) . . ? C49 C50 C51 120.1(5) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? N7 C51 C50 123.0(5) . . ? N7 C51 H51A 118.5 . . ? C50 C51 H51A 118.5 . . ? N8 C52 C53 123.1(4) . . ? N8 C52 C49 114.8(4) . . ? C53 C52 C49 122.2(4) . . ? C52 C53 C54 120.6(5) . . ? C52 C53 H53A 119.7 . . ? C54 C53 H53A 119.7 . . ? C53 C54 C55 116.0(4) . . ? C53 C54 C62 121.9(4) . . ? C55 C54 C62 122.1(4) . . ? C56 C55 C54 120.5(4) . . ? C56 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? N8 C56 C55 122.4(4) . . ? N8 C56 C59 114.9(4) . . ? C55 C56 C59 122.7(4) . . ? N9 C57 C58 122.7(5) . . ? N9 C57 H57A 118.7 . . ? C58 C57 H57A 118.7 . . ? C57 C58 C59 120.4(5) . . ? C57 C58 H58A 119.8 . . ? C59 C58 H58A 119.8 . . ? C58 C59 C60 116.3(5) . . ? C58 C59 C56 121.0(5) . . ? C60 C59 C56 122.6(4) . . ? C61 C60 C59 119.9(5) . . ? C61 C60 H60A 120.0 . . ? C59 C60 H60A 120.0 . . ? N9 C61 C60 123.2(5) . . ? N9 C61 H61A 118.4 . . ? C60 C61 H61A 118.4 . . ? C63 C62 C67 116.9(5) . . ? C63 C62 C54 121.1(5) . . ? C67 C62 C54 121.9(5) . . ? C62 C63 C64 121.7(6) . . ? C62 C63 H63A 119.2 . . ? C64 C63 H63A 119.2 . . ? C65 C64 C63 120.8(6) . . ? C65 C64 H64A 119.6 . . ? C63 C64 H64A 119.6 . . ? C64 C65 C66 118.5(5) . . ? C64 C65 C68 121.4(7) . . ? C66 C65 C68 119.9(7) . . ? C66 C67 C62 121.2(6) . . ? C66 C67 H67A 119.4 . . ? C62 C67 H67A 119.4 . . ? C65 C66 C67 120.9(6) . . ? C65 C66 H66A 119.6 . . ? C67 C66 H66A 119.6 . . ? C69 C68 C65 179.0(12) . . ? C68 C69 H69 180.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.456 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.101 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.047 0.000 0.500 1835 405 ' ' 2 0.476 0.467 0.263 6 0 ' ' 3 0.524 0.533 0.737 5 1 ' ' _platon_squeeze_details ; ;